Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Chi-Tien Chen' _publ_contact_author_address ; Department of Chemistry National Chung Hsing University 250 Kuo Kuang Rd. Taichung 402 TAIWAN ; _publ_contact_author_email CTCHEN@DRAGON.NCHU.EDU.TW _publ_section_title ; Structural and Catalytic Studies of Lithium Complexes Bearing Pendant Amino-Phenolate Ligands ; loop_ _publ_author_name 'Chi-Tien Chen' 'Chia-Lin Ho' 'Chi-An Huang' data_HONMePhSMe _database_code_depnum_ccdc_archive 'CCDC 646484' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H35 N O S' _chemical_formula_weight 385.59 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.4226(12) _cell_length_b 9.8356(9) _cell_length_c 17.4956(15) _cell_angle_alpha 90.00 _cell_angle_beta 108.763(2) _cell_angle_gamma 90.00 _cell_volume 2349.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3996 _cell_measurement_theta_min 2.408 _cell_measurement_theta_max 25.969 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.090 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.150 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.678 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12881 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 26.06 _reflns_number_total 4594 _reflns_number_gt 2967 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4594 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1658 _refine_ls_wR_factor_gt 0.1483 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 S S 0.40986(5) 0.52096(6) 0.09504(4) 0.0808(3) Uani 1 1 d . . . O O 0.28304(10) 0.23192(14) -0.03183(8) 0.0643(4) Uani 1 1 d . . . H0A H 0.3157 0.2590 0.0131 0.096 Uiso 1 1 calc R . . N N 0.40471(11) 0.18228(15) 0.12072(9) 0.0496(4) Uani 1 1 d . . . C1 C 0.23761(13) 0.11244(18) -0.02457(11) 0.0486(4) Uani 1 1 d . . . C2 C 0.17792(13) 0.04731(19) -0.09403(11) 0.0483(4) Uani 1 1 d . . . C3 C 0.13312(14) -0.07281(19) -0.08277(11) 0.0509(5) Uani 1 1 d . . . H3A H 0.0930 -0.1173 -0.1283 0.061 Uiso 1 1 calc R . . C4 C 0.14436(13) -0.13056(19) -0.00801(11) 0.0507(5) Uani 1 1 d . . . C5 C 0.20528(13) -0.0631(2) 0.05883(11) 0.0514(5) Uani 1 1 d . . . H5A H 0.2157 -0.1000 0.1099 0.062 Uiso 1 1 calc R . . C6 C 0.25096(14) 0.05724(19) 0.05183(11) 0.0498(4) Uani 1 1 d . . . C7 C 0.31116(15) 0.1326(2) 0.12658(12) 0.0587(5) Uani 1 1 d . . . H7A H 0.2736 0.2092 0.1356 0.070 Uiso 1 1 calc R . . H7B H 0.3241 0.0725 0.1728 0.070 Uiso 1 1 calc R . . C8 C 0.46593(17) 0.0699(2) 0.11042(15) 0.0715(6) Uani 1 1 d . . . H8A H 0.4315 0.0195 0.0627 0.107 Uiso 1 1 calc R . . H8B H 0.4809 0.0111 0.1566 0.107 Uiso 1 1 calc R . . H8C H 0.5256 0.1053 0.1052 0.107 Uiso 1 1 calc R . . C9 C 0.45611(15) 0.2630(2) 0.19321(12) 0.0572(5) Uani 1 1 d . . . H9A H 0.4782 0.2030 0.2395 0.069 Uiso 1 1 calc R . . H9B H 0.4108 0.3280 0.2034 0.069 Uiso 1 1 calc R . . C10 C 0.54230(14) 0.3377(2) 0.18369(11) 0.0537(5) Uani 1 1 d . . . C11 C 0.53009(15) 0.4576(2) 0.13851(12) 0.0570(5) Uani 1 1 d . . . C12 C 0.6112(2) 0.5200(2) 0.12804(15) 0.0761(7) Uani 1 1 d . . . H12A H 0.6036 0.5990 0.0974 0.091 Uiso 1 1 calc R . . C13 C 0.7030(2) 0.4658(3) 0.1628(2) 0.0913(9) Uani 1 1 d . . . H13A H 0.7569 0.5086 0.1553 0.110 Uiso 1 1 calc R . . C14 C 0.71632(19) 0.3507(3) 0.2081(2) 0.0914(9) Uani 1 1 d . . . H14A H 0.7787 0.3147 0.2312 0.110 Uiso 1 1 calc R . . C15 C 0.63609(17) 0.2878(2) 0.21942(14) 0.0708(6) Uani 1 1 d . . . H15A H 0.6452 0.2105 0.2516 0.085 Uiso 1 1 calc R . . C16 C 0.09042(14) -0.2620(2) -0.00232(12) 0.0592(5) Uani 1 1 d . . . C17 C 0.1157(3) -0.3138(3) 0.08325(17) 0.1124(11) Uani 1 1 d . . . H17A H 0.1848 -0.3305 0.1047 0.169 Uiso 1 1 calc R . . H17B H 0.0808 -0.3968 0.0836 0.169 Uiso 1 1 calc R . . H17C H 0.0974 -0.2471 0.1159 0.169 Uiso 1 1 calc R . . C18 C 0.1158(2) -0.3737(3) -0.05330(18) 0.0905(8) Uani 1 1 d . . . H18A H 0.1849 -0.3914 -0.0333 0.136 Uiso 1 1 calc R . . H18B H 0.0978 -0.3444 -0.1085 0.136 Uiso 1 1 calc R . . H18C H 0.0806 -0.4551 -0.0500 0.136 Uiso 1 1 calc R . . C19 C -0.02095(18) -0.2361(3) -0.0365(2) 0.0938(8) Uani 1 1 d . . . H19A H -0.0389 -0.1668 -0.0052 0.141 Uiso 1 1 calc R . . H19B H -0.0555 -0.3185 -0.0338 0.141 Uiso 1 1 calc R . . H19C H -0.0378 -0.2070 -0.0917 0.141 Uiso 1 1 calc R . . C20 C 0.16186(15) 0.1055(2) -0.17861(11) 0.0576(5) Uani 1 1 d . . . C21 C 0.11302(19) 0.2450(2) -0.18567(15) 0.0793(7) Uani 1 1 d . . . H21A H 0.1535 0.3046 -0.1451 0.119 Uiso 1 1 calc R . . H21B H 0.0502 0.2357 -0.1782 0.119 Uiso 1 1 calc R . . H21C H 0.1046 0.2824 -0.2382 0.119 Uiso 1 1 calc R . . C22 C 0.25957(19) 0.1164(3) -0.19469(14) 0.0825(7) Uani 1 1 d . . . H22A H 0.3035 0.1727 -0.1542 0.124 Uiso 1 1 calc R . . H22B H 0.2492 0.1558 -0.2470 0.124 Uiso 1 1 calc R . . H22C H 0.2875 0.0274 -0.1930 0.124 Uiso 1 1 calc R . . C23 C 0.0943(2) 0.0147(3) -0.24490(13) 0.0873(8) Uani 1 1 d . . . H23A H 0.1228 -0.0741 -0.2422 0.131 Uiso 1 1 calc R . . H23B H 0.0862 0.0541 -0.2968 0.131 Uiso 1 1 calc R . . H23C H 0.0316 0.0074 -0.2370 0.131 Uiso 1 1 calc R . . C24 C 0.4268(3) 0.6847(3) 0.0555(2) 0.1073(10) Uani 1 1 d . . . H24A H 0.3642 0.7266 0.0306 0.161 Uiso 1 1 calc R . . H24B H 0.4597 0.6735 0.0161 0.161 Uiso 1 1 calc R . . H24C H 0.4656 0.7413 0.0986 0.161 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 S 0.0884(5) 0.0580(4) 0.0834(5) 0.0043(3) 0.0102(3) -0.0039(3) O 0.0856(10) 0.0505(8) 0.0530(8) 0.0031(6) 0.0171(7) -0.0276(7) N 0.0605(9) 0.0415(8) 0.0460(8) -0.0053(6) 0.0159(7) -0.0127(7) C1 0.0575(11) 0.0392(9) 0.0505(10) 0.0010(8) 0.0193(8) -0.0107(8) C2 0.0543(10) 0.0453(10) 0.0441(10) 0.0018(8) 0.0141(8) -0.0057(8) C3 0.0580(11) 0.0463(10) 0.0456(10) -0.0026(8) 0.0129(8) -0.0143(8) C4 0.0551(10) 0.0445(10) 0.0521(10) 0.0026(8) 0.0167(8) -0.0102(8) C5 0.0591(11) 0.0509(11) 0.0439(10) 0.0049(8) 0.0163(8) -0.0128(9) C6 0.0565(10) 0.0487(10) 0.0454(10) -0.0023(8) 0.0180(8) -0.0121(8) C7 0.0694(12) 0.0609(12) 0.0463(10) -0.0053(9) 0.0197(9) -0.0247(10) C8 0.0734(14) 0.0534(12) 0.0817(15) -0.0131(11) 0.0165(12) -0.0047(11) C9 0.0737(12) 0.0538(11) 0.0424(10) -0.0069(8) 0.0162(9) -0.0199(10) C10 0.0642(12) 0.0495(11) 0.0448(10) -0.0109(8) 0.0142(9) -0.0142(9) C11 0.0756(13) 0.0464(11) 0.0508(11) -0.0119(8) 0.0227(10) -0.0176(9) C12 0.1017(19) 0.0598(14) 0.0751(15) -0.0146(11) 0.0399(15) -0.0304(14) C13 0.089(2) 0.085(2) 0.116(2) -0.0356(18) 0.0558(18) -0.0391(16) C14 0.0635(14) 0.091(2) 0.117(2) -0.0367(18) 0.0248(14) -0.0152(14) C15 0.0755(15) 0.0620(13) 0.0667(14) -0.0111(11) 0.0114(11) -0.0105(11) C16 0.0624(12) 0.0513(12) 0.0619(12) 0.0041(9) 0.0172(10) -0.0211(9) C17 0.152(3) 0.097(2) 0.0780(18) 0.0203(15) 0.0219(17) -0.069(2) C18 0.1085(19) 0.0560(14) 0.108(2) -0.0077(14) 0.0360(16) -0.0228(14) C19 0.0728(15) 0.0876(18) 0.119(2) 0.0072(17) 0.0288(15) -0.0256(14) C20 0.0754(13) 0.0515(11) 0.0435(10) 0.0052(8) 0.0158(9) -0.0110(10) C21 0.0965(17) 0.0598(14) 0.0733(15) 0.0195(11) 0.0159(13) 0.0022(12) C22 0.1036(19) 0.0920(18) 0.0640(14) 0.0069(13) 0.0440(13) -0.0084(15) C23 0.126(2) 0.0759(16) 0.0446(11) 0.0052(11) 0.0060(13) -0.0259(15) C24 0.155(3) 0.0519(15) 0.096(2) 0.0048(14) 0.0154(19) 0.0010(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 S C11 1.768(2) . ? S C24 1.801(3) . ? O C1 1.371(2) . ? N C8 1.462(3) . ? N C7 1.469(2) . ? N C9 1.478(2) . ? C1 C6 1.397(2) . ? C1 C2 1.398(2) . ? C2 C3 1.391(3) . ? C2 C20 1.533(2) . ? C3 C4 1.387(3) . ? C4 C5 1.385(3) . ? C4 C16 1.528(2) . ? C5 C6 1.379(3) . ? C6 C7 1.511(3) . ? C9 C10 1.499(3) . ? C10 C15 1.385(3) . ? C10 C11 1.399(3) . ? C11 C12 1.385(3) . ? C12 C13 1.374(4) . ? C13 C14 1.360(4) . ? C14 C15 1.381(3) . ? C16 C17 1.511(3) . ? C16 C18 1.532(3) . ? C16 C19 1.544(3) . ? C20 C22 1.527(3) . ? C20 C21 1.529(3) . ? C20 C23 1.538(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 S C24 104.17(13) . . ? C8 N C7 111.22(16) . . ? C8 N C9 110.86(16) . . ? C7 N C9 109.72(14) . . ? O C1 C6 119.91(16) . . ? O C1 C2 119.41(15) . . ? C6 C1 C2 120.68(16) . . ? C3 C2 C1 116.76(16) . . ? C3 C2 C20 121.42(16) . . ? C1 C2 C20 121.82(16) . . ? C4 C3 C2 124.26(17) . . ? C5 C4 C3 116.75(17) . . ? C5 C4 C16 123.23(17) . . ? C3 C4 C16 120.02(16) . . ? C6 C5 C4 121.83(17) . . ? C5 C6 C1 119.71(16) . . ? C5 C6 C7 120.14(16) . . ? C1 C6 C7 120.09(16) . . ? N C7 C6 112.81(15) . . ? N C9 C10 111.91(15) . . ? C15 C10 C11 118.76(19) . . ? C15 C10 C9 120.05(19) . . ? C11 C10 C9 121.19(18) . . ? C12 C11 C10 119.4(2) . . ? C12 C11 S 122.72(18) . . ? C10 C11 S 117.90(15) . . ? C13 C12 C11 120.3(2) . . ? C14 C13 C12 121.1(2) . . ? C13 C14 C15 119.3(3) . . ? C14 C15 C10 121.2(2) . . ? C17 C16 C4 112.61(17) . . ? C17 C16 C18 108.0(2) . . ? C4 C16 C18 110.27(16) . . ? C17 C16 C19 109.2(2) . . ? C4 C16 C19 108.87(17) . . ? C18 C16 C19 107.8(2) . . ? C22 C20 C21 110.55(19) . . ? C22 C20 C2 110.00(17) . . ? C21 C20 C2 109.62(17) . . ? C22 C20 C23 107.5(2) . . ? C21 C20 C23 107.25(19) . . ? C2 C20 C23 111.91(16) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.375 _refine_diff_density_min -0.223 _refine_diff_density_rms 0.051 #==END data_compound3 _database_code_depnum_ccdc_archive 'CCDC 646485' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H34 Li N O2' _chemical_formula_weight 375.46 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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6656(8) _cell_length_b 10.6883(9) _cell_length_c 10.9810(9) _cell_angle_alpha 96.694(2) _cell_angle_beta 90.990(2) _cell_angle_gamma 92.233(2) _cell_volume 1125.57(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2929 _cell_measurement_theta_min 2.794 _cell_measurement_theta_max 25.995 _exptl_crystal_description parallelpiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.324 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6425 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 26.02 _reflns_number_total 4358 _reflns_number_gt 3229 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4358 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0892 _refine_ls_R_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.2336 _refine_ls_wR_factor_gt 0.2144 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 Li Li -0.0203(3) 0.0894(3) 0.5825(3) 0.0446(7) Uani 1 1 d . . . O1 O 0.10641(13) 0.07463(11) 0.45620(11) 0.0420(4) Uani 1 1 d . . . O2 O 0.13495(15) -0.24636(13) 0.42682(12) 0.0498(4) Uani 1 1 d . . . N N 0.03459(16) -0.10740(14) 0.22561(13) 0.0413(4) Uani 1 1 d . . . C1 C 0.20222(18) 0.11596(16) 0.38454(16) 0.0378(4) Uani 1 1 d . . . C2 C 0.32852(19) 0.18241(17) 0.42982(16) 0.0410(4) Uani 1 1 d . . . C3 C 0.4208(2) 0.22231(18) 0.34639(17) 0.0463(5) Uani 1 1 d . . . H3A H 0.5013 0.2659 0.3773 0.056 Uiso 1 1 calc R . . C4 C 0.4024(2) 0.20221(18) 0.21915(17) 0.0454(5) Uani 1 1 d . . . C5 C 0.2820(2) 0.13517(17) 0.17660(17) 0.0438(4) Uani 1 1 d . . . H5A H 0.2665 0.1173 0.0924 0.053 Uiso 1 1 calc R . . C6 C 0.18369(19) 0.09375(16) 0.25545(16) 0.0399(4) Uani 1 1 d . . . C7 C 0.0527(2) 0.02584(17) 0.20117(17) 0.0446(5) Uani 1 1 d . . . H7A H -0.0261 0.0715 0.2333 0.053 Uiso 1 1 calc R . . H7B H 0.0521 0.0281 0.1131 0.053 Uiso 1 1 calc R . . C8 C -0.0796(3) -0.1653(3) 0.1430(2) 0.0722(7) Uani 1 1 d . . . H8A H -0.0947 -0.2521 0.1559 0.108 Uiso 1 1 calc R . . H8B H -0.0552 -0.1605 0.0592 0.108 Uiso 1 1 calc R . . H8C H -0.1627 -0.1209 0.1603 0.108 Uiso 1 1 calc R . . C9 C 0.1595(2) -0.17741(18) 0.19249(18) 0.0492(5) Uani 1 1 d . . . H9A H 0.2383 -0.1367 0.2391 0.059 Uiso 1 1 calc R . . H9B H 0.1770 -0.1742 0.1062 0.059 Uiso 1 1 calc R . . C10 C 0.1463(2) -0.31308(18) 0.2167(2) 0.0498(5) Uani 1 1 d . . . C11 C 0.13738(19) -0.34602(18) 0.33484(19) 0.0467(5) Uani 1 1 d . . . C12 C 0.1326(3) -0.4709(2) 0.3568(3) 0.0638(6) Uani 1 1 d . . . H12A H 0.1271 -0.4913 0.4367 0.077 Uiso 1 1 calc R . . C13 C 0.1359(3) -0.5648(2) 0.2603(3) 0.0802(8) Uani 1 1 d . . . H13A H 0.1353 -0.6486 0.2753 0.096 Uiso 1 1 calc R . . C14 C 0.1401(4) -0.5359(2) 0.1428(3) 0.0874(9) Uani 1 1 d . . . H14A H 0.1392 -0.5998 0.0776 0.105 Uiso 1 1 calc R . . C15 C 0.1458(3) -0.4107(2) 0.1211(2) 0.0698(7) Uani 1 1 d . . . H15A H 0.1493 -0.3914 0.0407 0.084 Uiso 1 1 calc R . . C16 C 0.5132(2) 0.2500(2) 0.13452(19) 0.0568(6) Uani 1 1 d . . . C17 C 0.6441(3) 0.1752(3) 0.1451(3) 0.0863(9) Uani 1 1 d . . . H17A H 0.6227 0.0874 0.1203 0.129 Uiso 1 1 calc R . . H17B H 0.6778 0.1864 0.2286 0.129 Uiso 1 1 calc R . . H17C H 0.7138 0.2050 0.0931 0.129 Uiso 1 1 calc R . . C18 C 0.5489(4) 0.3901(3) 0.1740(3) 0.0930(10) Uani 1 1 d . . . H18A H 0.5807 0.4013 0.2580 0.139 Uiso 1 1 calc R . . H18B H 0.4679 0.4379 0.1656 0.139 Uiso 1 1 calc R . . H18C H 0.6204 0.4188 0.1230 0.139 Uiso 1 1 calc R . . C19 C 0.4651(3) 0.2357(3) 0.0004(2) 0.0863(9) Uani 1 1 d . . . H19A H 0.4427 0.1484 -0.0266 0.129 Uiso 1 1 calc R . . H19B H 0.5377 0.2655 -0.0488 0.129 Uiso 1 1 calc R . . H19C H 0.3846 0.2841 -0.0079 0.129 Uiso 1 1 calc R . . C20 C 0.3579(2) 0.2121(2) 0.56886(17) 0.0489(5) Uani 1 1 d . . . C21 C 0.3517(3) 0.0909(2) 0.6307(2) 0.0631(6) Uani 1 1 d . . . H21A H 0.4188 0.0344 0.5951 0.095 Uiso 1 1 calc R . . H21B H 0.2608 0.0514 0.6189 0.095 Uiso 1 1 calc R . . H21C H 0.3717 0.1108 0.7169 0.095 Uiso 1 1 calc R . . C22 C 0.5027(3) 0.2750(3) 0.5979(2) 0.0751(8) Uani 1 1 d . . . H22A H 0.5720 0.2193 0.5652 0.113 Uiso 1 1 calc R . . H22B H 0.5161 0.2926 0.6851 0.113 Uiso 1 1 calc R . . H22C H 0.5103 0.3523 0.5614 0.113 Uiso 1 1 calc R . . C23 C 0.2524(2) 0.3054(2) 0.6236(2) 0.0587(6) Uani 1 1 d . . . H23A H 0.1603 0.2695 0.6076 0.088 Uiso 1 1 calc R . . H23B H 0.2622 0.3824 0.5868 0.088 Uiso 1 1 calc R . . H23C H 0.2685 0.3227 0.7105 0.088 Uiso 1 1 calc R . . C24 C 0.1485(3) -0.2740(3) 0.5504(2) 0.0686(7) Uani 1 1 d . . . H24A H 0.1452 -0.1974 0.6052 0.103 Uiso 1 1 calc R . . H24B H 0.2353 -0.3123 0.5614 0.103 Uiso 1 1 calc R . . H24C H 0.0740 -0.3309 0.5676 0.103 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 Li 0.0508(17) 0.0449(16) 0.0383(15) 0.0082(13) 0.0064(13) -0.0063(13) O1 0.0441(7) 0.0453(7) 0.0360(7) 0.0059(5) 0.0051(5) -0.0104(5) O2 0.0578(9) 0.0503(8) 0.0415(8) 0.0069(6) -0.0018(6) 0.0012(6) N 0.0432(8) 0.0427(8) 0.0377(8) 0.0071(6) 0.0000(6) -0.0081(6) C1 0.0431(10) 0.0355(9) 0.0350(9) 0.0072(7) 0.0011(7) -0.0045(7) C2 0.0441(10) 0.0443(9) 0.0337(9) 0.0038(7) -0.0008(7) -0.0066(7) C3 0.0456(10) 0.0507(11) 0.0409(10) 0.0038(8) 0.0001(8) -0.0134(8) C4 0.0531(11) 0.0472(10) 0.0356(9) 0.0081(8) 0.0051(8) -0.0109(8) C5 0.0564(11) 0.0422(10) 0.0327(9) 0.0071(7) -0.0001(8) -0.0078(8) C6 0.0493(10) 0.0358(9) 0.0342(9) 0.0065(7) -0.0027(7) -0.0078(7) C7 0.0515(11) 0.0448(10) 0.0378(9) 0.0114(8) -0.0083(8) -0.0091(8) C8 0.0743(16) 0.0835(17) 0.0566(14) 0.0081(12) -0.0062(12) -0.0203(13) C9 0.0555(12) 0.0485(11) 0.0433(10) 0.0049(8) 0.0135(8) -0.0060(8) C10 0.0526(11) 0.0427(10) 0.0531(11) 0.0017(8) 0.0099(9) -0.0036(8) C11 0.0410(10) 0.0430(10) 0.0562(12) 0.0063(8) 0.0060(8) -0.0006(7) C12 0.0681(15) 0.0488(12) 0.0780(16) 0.0197(11) 0.0128(12) 0.0047(10) C13 0.098(2) 0.0401(12) 0.103(2) 0.0084(13) 0.0196(16) 0.0055(12) C14 0.113(2) 0.0480(14) 0.096(2) -0.0172(13) 0.0197(18) 0.0006(14) C15 0.0937(18) 0.0537(13) 0.0594(14) -0.0056(10) 0.0148(12) 0.0022(12) C16 0.0625(13) 0.0652(13) 0.0423(11) 0.0100(9) 0.0100(9) -0.0173(10) C17 0.0680(17) 0.127(3) 0.0653(16) 0.0183(16) 0.0210(13) -0.0021(16) C18 0.118(3) 0.0763(18) 0.0829(19) 0.0108(14) 0.0337(17) -0.0428(17) C19 0.088(2) 0.125(2) 0.0466(13) 0.0271(14) 0.0082(12) -0.0353(17) C20 0.0480(11) 0.0636(12) 0.0335(9) 0.0030(8) -0.0026(8) -0.0086(9) C21 0.0725(15) 0.0768(15) 0.0415(11) 0.0131(10) -0.0047(10) 0.0067(12) C22 0.0556(14) 0.119(2) 0.0456(12) -0.0031(13) -0.0072(10) -0.0246(13) C23 0.0688(14) 0.0598(13) 0.0443(11) -0.0044(9) 0.0029(10) -0.0081(10) C24 0.0824(17) 0.0798(16) 0.0458(12) 0.0172(11) -0.0026(11) 0.0059(13) _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 Li O1 1.863(3) . ? Li O1 1.910(3) 2_556 ? Li O2 2.058(4) 2_556 ? Li N 2.101(3) 2_556 ? Li Li 2.522(6) 2_556 ? O1 C1 1.321(2) . ? O1 Li 1.910(3) 2_556 ? O2 C11 1.381(2) . ? O2 C24 1.427(3) . ? O2 Li 2.058(4) 2_556 ? N C9 1.474(3) . ? N C7 1.484(2) . ? N C8 1.486(3) . ? N Li 2.101(3) 2_556 ? C1 C6 1.417(2) . ? C1 C2 1.439(2) . ? C2 C3 1.380(3) . ? C2 C20 1.542(2) . ? C3 C4 1.396(3) . ? C4 C5 1.387(3) . ? C4 C16 1.541(3) . ? C5 C6 1.391(3) . ? C6 C7 1.512(2) . ? C9 C10 1.505(3) . ? C10 C11 1.387(3) . ? C10 C15 1.391(3) . ? C11 C12 1.383(3) . ? C12 C13 1.373(4) . ? C13 C14 1.362(4) . ? C14 C15 1.386(4) . ? C16 C19 1.526(3) . ? C16 C17 1.532(4) . ? C16 C18 1.534(4) . ? C20 C21 1.530(3) . ? C20 C23 1.536(3) . ? C20 C22 1.541(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Li O1 96.09(15) . 2_556 ? O1 Li O2 110.16(15) . 2_556 ? O1 Li O2 119.64(18) 2_556 2_556 ? O1 Li N 142.63(19) . 2_556 ? O1 Li N 99.35(14) 2_556 2_556 ? O2 Li N 91.21(13) 2_556 2_556 ? O1 Li Li 48.83(11) . 2_556 ? O1 Li Li 47.26(11) 2_556 2_556 ? O2 Li Li 129.0(2) 2_556 2_556 ? N Li Li 135.2(2) 2_556 2_556 ? C1 O1 Li 155.28(15) . . ? C1 O1 Li 120.40(14) . 2_556 ? Li O1 Li 83.91(15) . 2_556 ? C11 O2 C24 117.55(17) . . ? C11 O2 Li 124.07(15) . 2_556 ? C24 O2 Li 110.82(16) . 2_556 ? C9 N C7 110.75(15) . . ? C9 N C8 106.88(17) . . ? C7 N C8 106.81(16) . . ? C9 N Li 107.74(14) . 2_556 ? C7 N Li 102.22(13) . 2_556 ? C8 N Li 122.20(16) . 2_556 ? O1 C1 C6 119.71(15) . . ? O1 C1 C2 123.68(15) . . ? C6 C1 C2 116.61(16) . . ? C3 C2 C1 118.69(16) . . ? C3 C2 C20 120.72(16) . . ? C1 C2 C20 120.57(16) . . ? C2 C3 C4 125.01(17) . . ? C5 C4 C3 115.75(17) . . ? C5 C4 C16 123.67(17) . . ? C3 C4 C16 120.56(17) . . ? C4 C5 C6 122.26(17) . . ? C5 C6 C1 121.65(16) . . ? C5 C6 C7 118.74(16) . . ? C1 C6 C7 119.60(16) . . ? N C7 C6 115.00(15) . . ? N C9 C10 112.63(16) . . ? C11 C10 C15 117.3(2) . . ? C11 C10 C9 121.59(18) . . ? C15 C10 C9 121.1(2) . . ? O2 C11 C12 123.3(2) . . ? O2 C11 C10 115.45(17) . . ? C12 C11 C10 121.2(2) . . ? C13 C12 C11 119.8(2) . . ? C14 C13 C12 120.5(2) . . ? C13 C14 C15 119.6(2) . . ? C14 C15 C10 121.5(3) . . ? C19 C16 C17 108.6(2) . . ? C19 C16 C18 107.9(2) . . ? C17 C16 C18 109.0(2) . . ? C19 C16 C4 112.47(19) . . ? C17 C16 C4 109.08(19) . . ? C18 C16 C4 109.68(19) . . ? C21 C20 C23 111.15(17) . . ? C21 C20 C22 106.95(19) . . ? C23 C20 C22 106.87(19) . . ? C21 C20 C2 110.55(16) . . ? C23 C20 C2 108.97(16) . . ? C22 C20 C2 112.31(16) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.322 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.067 #==END data_compound4 _database_code_depnum_ccdc_archive 'CCDC 646486' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H68 Li2 N2 O2 S2' _chemical_formula_weight 783.04 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' Li Li -0.0003 0.0001 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.726(2) _cell_length_b 13.834(2) _cell_length_c 18.762(3) _cell_angle_alpha 72.370(3) _cell_angle_beta 72.813(4) _cell_angle_gamma 65.937(3) _cell_volume 2817.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5836 _cell_measurement_theta_min 2.324 _cell_measurement_theta_max 25.825 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.923 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.125 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.694 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15649 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.04 _reflns_number_total 10729 _reflns_number_gt 6770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10729 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1893 _refine_ls_wR_factor_gt 0.1710 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.3305(3) 0.9417(3) 0.3526(2) 0.0650(9) Uani 1 1 d . . . Li2 Li 0.3962(3) 0.8708(3) 0.2364(2) 0.0632(9) Uani 1 1 d . . . S1 S 0.44115(5) 0.94750(5) 0.44476(4) 0.0760(2) Uani 1 1 d . . . S2 S 0.53281(6) 0.68161(4) 0.21713(4) 0.0733(2) Uani 1 1 d . . . O1 O 0.42000(13) 0.98025(11) 0.25542(9) 0.0637(4) Uani 1 1 d . . . O2 O 0.29689(13) 0.83930(11) 0.32992(8) 0.0623(4) Uani 1 1 d . . . N1 N 0.20675(15) 1.08830(14) 0.37275(11) 0.0645(5) Uani 1 1 d . . . N2 N 0.30877(16) 0.87775(12) 0.15758(10) 0.0598(4) Uani 1 1 d . . . C1 C 0.43794(19) 1.07216(15) 0.24329(12) 0.0579(5) Uani 1 1 d . . . C2 C 0.54997(19) 1.08255(15) 0.21001(12) 0.0596(5) Uani 1 1 d . . . C3 C 0.5599(2) 1.18227(17) 0.20151(14) 0.0703(6) Uani 1 1 d . . . H3A H 0.6333 1.1886 0.1803 0.084 Uiso 1 1 calc R . . C4 C 0.4681(2) 1.27252(17) 0.22245(17) 0.0794(7) Uani 1 1 d . A . C5 C 0.3597(2) 1.26074(18) 0.25350(17) 0.0791(7) Uani 1 1 d . . . H5A H 0.2957 1.3199 0.2679 0.095 Uiso 1 1 calc R . . C6 C 0.3431(2) 1.16391(17) 0.26390(14) 0.0654(6) Uani 1 1 d . . . C7 C 0.2223(2) 1.15607(18) 0.29600(15) 0.0720(6) Uani 1 1 d . . . H7A H 0.1656 1.2286 0.2971 0.086 Uiso 1 1 calc R . . H7B H 0.2044 1.1278 0.2614 0.086 Uiso 1 1 calc R . . C8 C 0.0920(2) 1.0760(2) 0.39228(17) 0.0851(7) Uani 1 1 d . . . H8A H 0.0314 1.1430 0.4019 0.128 Uiso 1 1 calc R . . H8B H 0.0887 1.0199 0.4371 0.128 Uiso 1 1 calc R . . H8C H 0.0806 1.0571 0.3506 0.128 Uiso 1 1 calc R . . C9 C 0.2165(2) 1.1373(2) 0.42957(16) 0.0783(7) Uani 1 1 d . . . H9A H 0.1500 1.2040 0.4337 0.094 Uiso 1 1 calc R . . H9B H 0.2871 1.1557 0.4114 0.094 Uiso 1 1 calc R . . C10 C 0.2206(2) 1.0643(2) 0.50785(15) 0.0719(6) Uani 1 1 d . . . C11 C 0.3197(2) 0.9742(2) 0.52180(15) 0.0724(6) Uani 1 1 d . . . C12 C 0.3219(3) 0.9096(3) 0.59487(16) 0.0882(8) Uani 1 1 d . . . H12A H 0.3890 0.8507 0.6049 0.106 Uiso 1 1 calc R . . C13 C 0.2238(3) 0.9333(3) 0.65265(19) 0.1018(9) Uani 1 1 d . . . H13A H 0.2244 0.8884 0.7009 0.122 Uiso 1 1 calc R . . C14 C 0.1275(3) 1.0208(4) 0.6394(2) 0.1035(10) Uani 1 1 d . . . H14A H 0.0628 1.0368 0.6788 0.124 Uiso 1 1 calc R . . C15 C 0.1244(3) 1.0862(3) 0.5681(2) 0.0906(8) Uani 1 1 d . . . H15A H 0.0572 1.1461 0.5597 0.109 Uiso 1 1 calc R . . C16 C 0.4839(3) 1.3811(2) 0.2119(2) 0.1097(11) Uani 1 1 d . . . C17 C 0.3896(13) 1.4682(7) 0.1629(10) 0.218(6) Uani 0.70 1 d P A 1 H17A H 0.3512 1.4322 0.1483 0.327 Uiso 0.70 1 calc PR A 1 H17B H 0.4283 1.5058 0.1180 0.327 Uiso 0.70 1 calc PR A 1 H17C H 0.3324 1.5191 0.1928 0.327 Uiso 0.70 1 calc PR A 1 C18 C 0.4349(16) 1.4192(11) 0.2866(7) 0.255(7) Uani 0.70 1 d P A 1 H18A H 0.4838 1.3723 0.3227 0.382 Uiso 0.70 1 calc PR A 1 H18B H 0.3567 1.4176 0.3061 0.382 Uiso 0.70 1 calc PR A 1 H18C H 0.4330 1.4917 0.2783 0.382 Uiso 0.70 1 calc PR A 1 C19 C 0.5991(8) 1.3805(8) 0.1780(14) 0.304(11) Uani 0.70 1 d P A 1 H19A H 0.6530 1.3251 0.2084 0.457 Uiso 0.70 1 calc PR A 1 H19B H 0.6028 1.4496 0.1748 0.457 Uiso 0.70 1 calc PR A 1 H19C H 0.6198 1.3664 0.1276 0.457 Uiso 0.70 1 calc PR A 1 C17' C 0.3760(11) 1.4698(8) 0.2267(16) 0.117(6) Uani 0.30 1 d P A 2 H17D H 0.3596 1.4753 0.2790 0.175 Uiso 0.30 1 calc PR A 2 H17E H 0.3129 1.4573 0.2173 0.175 Uiso 0.30 1 calc PR A 2 H17F H 0.3835 1.5359 0.1939 0.175 Uiso 0.30 1 calc PR A 2 C18' C 0.5682(14) 1.3623(9) 0.2639(11) 0.111(4) Uani 0.30 1 d P A 2 H18D H 0.6026 1.2862 0.2835 0.166 Uiso 0.30 1 calc PR A 2 H18E H 0.5250 1.3985 0.3056 0.166 Uiso 0.30 1 calc PR A 2 H18F H 0.6291 1.3908 0.2349 0.166 Uiso 0.30 1 calc PR A 2 C19' C 0.5299(17) 1.4157(10) 0.1253(8) 0.119(5) Uani 0.30 1 d P A 2 H19D H 0.6131 1.3785 0.1133 0.179 Uiso 0.30 1 calc PR A 2 H19E H 0.5135 1.4924 0.1122 0.179 Uiso 0.30 1 calc PR A 2 H19F H 0.4917 1.3976 0.0967 0.179 Uiso 0.30 1 calc PR A 2 C20 C 0.6564(2) 0.98529(17) 0.18676(14) 0.0666(6) Uani 1 1 d . . . C21 C 0.7677(2) 1.0142(2) 0.15062(19) 0.0923(8) Uani 1 1 d . . . H21A H 0.7854 1.0398 0.1863 0.139 Uiso 1 1 calc R . . H21B H 0.7552 1.0697 0.1054 0.139 Uiso 1 1 calc R . . H21C H 0.8321 0.9510 0.1376 0.139 Uiso 1 1 calc R . . C22 C 0.6330(3) 0.9440(2) 0.12758(15) 0.0818(7) Uani 1 1 d . . . H22A H 0.6181 1.0010 0.0833 0.123 Uiso 1 1 calc R . . H22B H 0.5660 0.9217 0.1492 0.123 Uiso 1 1 calc R . . H22C H 0.7004 0.8836 0.1132 0.123 Uiso 1 1 calc R . . C23 C 0.6806(2) 0.8954(2) 0.25765(16) 0.0855(7) Uani 1 1 d . . . H23A H 0.6962 0.9216 0.2939 0.128 Uiso 1 1 calc R . . H23B H 0.7474 0.8345 0.2435 0.128 Uiso 1 1 calc R . . H23C H 0.6133 0.8736 0.2801 0.128 Uiso 1 1 calc R . . C24 C 0.5479(3) 0.8250(3) 0.48384(19) 0.0979(9) Uani 1 1 d . . . H24A H 0.5817 0.8401 0.5169 0.147 Uiso 1 1 calc R . . H24B H 0.6085 0.7962 0.4432 0.147 Uiso 1 1 calc R . . H24C H 0.5107 0.7731 0.5124 0.147 Uiso 1 1 calc R . . C25 C 0.23363(17) 0.78166(15) 0.33274(12) 0.0554(5) Uani 1 1 d . . . C26 C 0.22076(18) 0.69526(16) 0.39526(12) 0.0575(5) Uani 1 1 d . . . C27 C 0.15117(18) 0.64072(16) 0.39282(13) 0.0609(5) Uani 1 1 d . . . H27A H 0.1422 0.5847 0.4338 0.073 Uiso 1 1 calc R . . C28 C 0.09427(18) 0.66408(16) 0.33352(13) 0.0612(5) Uani 1 1 d . . . C29 C 0.10998(18) 0.74687(17) 0.27350(13) 0.0623(5) Uani 1 1 d . . . H29A H 0.0741 0.7644 0.2324 0.075 Uiso 1 1 calc R . . C30 C 0.17734(18) 0.80520(15) 0.27202(12) 0.0585(5) Uani 1 1 d . . . C31 C 0.1898(2) 0.89695(17) 0.20540(13) 0.0659(6) Uani 1 1 d . . . H31A H 0.1355 0.9110 0.1734 0.079 Uiso 1 1 calc R . . H31B H 0.1669 0.9616 0.2249 0.079 Uiso 1 1 calc R . . C32 C 0.3094(3) 0.97543(19) 0.09792(15) 0.0836(7) Uani 1 1 d . . . H32A H 0.2695 0.9812 0.0598 0.125 Uiso 1 1 calc R . . H32B H 0.3890 0.9706 0.0748 0.125 Uiso 1 1 calc R . . H32C H 0.2701 1.0382 0.1202 0.125 Uiso 1 1 calc R . . C33 C 0.3446(2) 0.78338(18) 0.12310(14) 0.0682(6) Uani 1 1 d . . . H33A H 0.2924 0.7998 0.0890 0.082 Uiso 1 1 calc R . . H33B H 0.3349 0.7224 0.1633 0.082 Uiso 1 1 calc R . . C34 C 0.4686(2) 0.75082(17) 0.07945(14) 0.0695(6) Uani 1 1 d . . . C35 C 0.5642(2) 0.70349(17) 0.11632(14) 0.0700(6) Uani 1 1 d . . . C36 C 0.6769(3) 0.6750(2) 0.0734(2) 0.0980(9) Uani 1 1 d . . . H36A H 0.7408 0.6439 0.0975 0.118 Uiso 1 1 calc R . . C37 C 0.6954(4) 0.6926(3) -0.0059(3) 0.1238(12) Uani 1 1 d . . . H37A H 0.7715 0.6742 -0.0346 0.149 Uiso 1 1 calc R . . C38 C 0.6020(4) 0.7369(3) -0.0415(2) 0.1181(11) Uani 1 1 d . . . H38A H 0.6140 0.7474 -0.0942 0.142 Uiso 1 1 calc R . . C39 C 0.4914(3) 0.7655(2) 0.00071(16) 0.0919(8) Uani 1 1 d . . . H39A H 0.4284 0.7960 -0.0242 0.110 Uiso 1 1 calc R . . C40 C 0.0124(2) 0.60428(19) 0.33828(15) 0.0718(6) Uani 1 1 d . . . C41 C 0.0624(3) 0.4838(2) 0.3759(2) 0.1015(10) Uani 1 1 d . . . H41A H 0.0104 0.4482 0.3779 0.152 Uiso 1 1 calc R . . H41B H 0.0698 0.4774 0.4267 0.152 Uiso 1 1 calc R . . H41C H 0.1382 0.4507 0.3466 0.152 Uiso 1 1 calc R . . C42 C -0.1069(2) 0.6555(2) 0.3854(2) 0.0954(9) Uani 1 1 d . . . H42A H -0.1390 0.7307 0.3623 0.143 Uiso 1 1 calc R . . H42B H -0.0987 0.6490 0.4361 0.143 Uiso 1 1 calc R . . H42C H -0.1585 0.6194 0.3877 0.143 Uiso 1 1 calc R . . C43 C -0.0042(3) 0.6124(3) 0.2590(2) 0.1160(11) Uani 1 1 d . . . H43A H -0.0348 0.6872 0.2346 0.174 Uiso 1 1 calc R . . H43B H -0.0583 0.5777 0.2636 0.174 Uiso 1 1 calc R . . H43C H 0.0699 0.5775 0.2289 0.174 Uiso 1 1 calc R . . C44 C 0.2829(2) 0.66309(19) 0.46184(13) 0.0688(6) Uani 1 1 d . . . C45 C 0.2635(3) 0.5639(3) 0.52051(17) 0.1021(10) Uani 1 1 d . . . H45A H 0.1810 0.5793 0.5404 0.153 Uiso 1 1 calc R . . H45B H 0.3030 0.5473 0.5615 0.153 Uiso 1 1 calc R . . H45C H 0.2945 0.5031 0.4964 0.153 Uiso 1 1 calc R . . C46 C 0.2359(3) 0.7567(3) 0.50323(16) 0.0981(9) Uani 1 1 d . . . H46A H 0.1528 0.7747 0.5214 0.147 Uiso 1 1 calc R . . H46B H 0.2517 0.8187 0.4686 0.147 Uiso 1 1 calc R . . H46C H 0.2739 0.7356 0.5456 0.147 Uiso 1 1 calc R . . C47 C 0.4155(2) 0.6339(2) 0.43290(16) 0.0845(7) Uani 1 1 d . . . H47A H 0.4447 0.5748 0.4072 0.127 Uiso 1 1 calc R . . H47B H 0.4534 0.6130 0.4753 0.127 Uiso 1 1 calc R . . H47C H 0.4316 0.6955 0.3980 0.127 Uiso 1 1 calc R . . C48 C 0.6726(3) 0.6217(3) 0.2435(2) 0.1127(10) Uani 1 1 d . . . H48A H 0.7114 0.5510 0.2318 0.169 Uiso 1 1 calc R . . H48B H 0.6626 0.6157 0.2973 0.169 Uiso 1 1 calc R . . H48C H 0.7192 0.6661 0.2157 0.169 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 Li1 0.076(2) 0.0573(19) 0.074(2) -0.0181(17) -0.0106(18) -0.0349(17) Li2 0.075(2) 0.0497(18) 0.075(2) -0.0160(16) -0.0087(18) -0.0341(16) S1 0.0629(4) 0.0887(4) 0.0853(4) -0.0371(3) -0.0075(3) -0.0268(3) S2 0.0866(4) 0.0510(3) 0.0882(4) -0.0137(3) -0.0263(3) -0.0241(3) O1 0.0761(10) 0.0479(7) 0.0787(10) -0.0169(7) -0.0067(7) -0.0365(7) O2 0.0732(9) 0.0521(8) 0.0744(9) -0.0124(6) -0.0104(7) -0.0379(7) N1 0.0568(10) 0.0627(10) 0.0851(13) -0.0241(9) -0.0079(9) -0.0298(8) N2 0.0724(12) 0.0422(8) 0.0651(11) -0.0035(7) -0.0139(9) -0.0257(8) C1 0.0676(13) 0.0438(10) 0.0706(13) -0.0108(9) -0.0112(10) -0.0300(9) C2 0.0665(13) 0.0440(10) 0.0737(14) -0.0129(9) -0.0108(10) -0.0263(9) C3 0.0658(14) 0.0537(12) 0.0986(17) -0.0193(11) -0.0053(12) -0.0331(11) C4 0.0776(16) 0.0443(11) 0.119(2) -0.0231(12) -0.0033(14) -0.0311(11) C5 0.0677(15) 0.0463(11) 0.120(2) -0.0257(12) -0.0036(13) -0.0216(10) C6 0.0652(13) 0.0496(11) 0.0861(16) -0.0155(10) -0.0102(11) -0.0272(10) C7 0.0626(14) 0.0575(12) 0.0997(18) -0.0171(12) -0.0164(12) -0.0240(10) C8 0.0657(15) 0.0956(18) 0.108(2) -0.0293(15) -0.0056(13) -0.0442(14) C9 0.0683(15) 0.0652(14) 0.113(2) -0.0442(14) -0.0084(13) -0.0231(11) C10 0.0674(15) 0.0765(15) 0.0901(17) -0.0426(14) -0.0049(12) -0.0325(12) C11 0.0688(15) 0.0867(16) 0.0823(17) -0.0404(14) -0.0079(12) -0.0362(13) C12 0.0926(19) 0.104(2) 0.0813(19) -0.0361(16) -0.0159(15) -0.0368(16) C13 0.106(3) 0.131(3) 0.085(2) -0.0454(19) -0.0032(18) -0.053(2) C14 0.095(2) 0.148(3) 0.092(2) -0.067(2) 0.0157(17) -0.061(2) C15 0.0779(18) 0.105(2) 0.108(2) -0.0599(19) 0.0010(16) -0.0372(15) C16 0.098(2) 0.0537(15) 0.180(3) -0.0366(19) 0.005(2) -0.0425(15) C17 0.290(16) 0.072(4) 0.325(15) 0.013(7) -0.130(13) -0.086(6) C18 0.373(19) 0.234(12) 0.264(12) -0.174(11) 0.109(12) -0.243(14) C19 0.133(7) 0.117(6) 0.67(3) -0.184(13) 0.102(12) -0.099(6) C17' 0.087(7) 0.033(5) 0.24(2) -0.043(9) -0.045(11) -0.016(4) C18' 0.101(9) 0.073(6) 0.198(13) -0.054(8) -0.026(9) -0.053(6) C19' 0.134(12) 0.072(7) 0.158(11) 0.011(7) -0.006(9) -0.084(9) C20 0.0697(14) 0.0511(11) 0.0817(15) -0.0198(10) -0.0071(11) -0.0249(10) C21 0.0704(16) 0.0799(17) 0.123(2) -0.0400(16) 0.0087(15) -0.0288(13) C22 0.1004(19) 0.0667(14) 0.0834(17) -0.0280(12) -0.0012(14) -0.0370(13) C23 0.0850(18) 0.0604(14) 0.104(2) -0.0151(13) -0.0261(15) -0.0147(12) C24 0.0747(18) 0.104(2) 0.116(2) -0.0381(18) -0.0218(16) -0.0193(15) C25 0.0548(11) 0.0424(10) 0.0720(13) -0.0121(9) -0.0090(10) -0.0224(9) C26 0.0543(11) 0.0496(11) 0.0701(13) -0.0088(9) -0.0091(10) -0.0245(9) C27 0.0575(12) 0.0516(11) 0.0736(14) -0.0038(9) -0.0097(10) -0.0279(9) C28 0.0520(12) 0.0534(11) 0.0830(15) -0.0145(10) -0.0110(10) -0.0247(9) C29 0.0551(12) 0.0576(12) 0.0777(14) -0.0107(10) -0.0181(10) -0.0221(10) C30 0.0561(12) 0.0457(10) 0.0720(13) -0.0069(9) -0.0131(10) -0.0196(9) C31 0.0701(14) 0.0485(11) 0.0776(15) -0.0033(10) -0.0227(12) -0.0206(10) C32 0.104(2) 0.0552(13) 0.0827(17) 0.0031(11) -0.0167(14) -0.0333(13) C33 0.0819(16) 0.0569(12) 0.0759(15) -0.0127(10) -0.0211(12) -0.0311(11) C34 0.0877(17) 0.0535(12) 0.0755(16) -0.0164(11) -0.0132(13) -0.0325(12) C35 0.0795(16) 0.0471(11) 0.0873(16) -0.0192(11) -0.0118(13) -0.0255(11) C36 0.085(2) 0.0862(19) 0.122(3) -0.0354(18) -0.0103(18) -0.0261(15) C37 0.114(3) 0.129(3) 0.116(3) -0.049(2) 0.025(2) -0.047(2) C38 0.128(3) 0.123(3) 0.092(2) -0.026(2) -0.001(2) -0.044(2) C39 0.109(2) 0.0866(18) 0.0766(19) -0.0208(14) -0.0101(16) -0.0339(16) C40 0.0607(13) 0.0689(14) 0.0989(18) -0.0167(12) -0.0149(12) -0.0366(11) C41 0.0899(19) 0.0624(15) 0.168(3) -0.0234(16) -0.0291(19) -0.0404(14) C42 0.0641(16) 0.0836(17) 0.140(3) -0.0206(17) -0.0067(15) -0.0386(13) C43 0.127(3) 0.151(3) 0.119(3) -0.029(2) -0.026(2) -0.095(2) C44 0.0731(15) 0.0713(14) 0.0692(14) -0.0017(11) -0.0160(11) -0.0404(12) C45 0.119(2) 0.115(2) 0.0883(19) 0.0291(16) -0.0407(17) -0.078(2) C46 0.116(2) 0.118(2) 0.0760(17) -0.0253(16) -0.0103(16) -0.0584(19) C47 0.0757(17) 0.0866(17) 0.0930(18) 0.0041(14) -0.0296(14) -0.0374(14) C48 0.103(2) 0.097(2) 0.136(3) -0.0196(19) -0.049(2) -0.0186(18) _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 Li1 O2 1.828(3) . ? Li1 O1 1.894(4) . ? Li1 N1 2.059(4) . ? Li1 S1 2.567(4) . ? Li2 O1 1.809(3) . ? Li2 O2 1.882(4) . ? Li2 N2 2.058(4) . ? Li2 S2 2.549(3) . ? S1 C11 1.775(3) . ? S1 C24 1.793(3) . ? S2 C35 1.770(3) . ? S2 C48 1.780(3) . ? O1 C1 1.323(2) . ? O2 C25 1.326(2) . ? N1 C8 1.464(3) . ? N1 C7 1.469(3) . ? N1 C9 1.482(3) . ? N2 C32 1.472(3) . ? N2 C31 1.477(3) . ? N2 C33 1.477(3) . ? C1 C6 1.410(3) . ? C1 C2 1.425(3) . ? C2 C3 1.393(3) . ? C2 C20 1.535(3) . ? C3 C4 1.384(3) . ? C3 H3A 0.9300 . ? C4 C5 1.386(3) . ? C4 C16 1.542(3) . ? C5 C6 1.387(3) . ? C5 H5A 0.9300 . ? C6 C7 1.512(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.511(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.389(4) . ? C10 C15 1.399(4) . ? C11 C12 1.392(4) . ? C12 C13 1.387(4) . ? C12 H12A 0.9300 . ? C13 C14 1.348(5) . ? C13 H13A 0.9300 . ? C14 C15 1.370(5) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C19 1.413(8) . ? C16 C17' 1.441(13) . ? C16 C18 1.514(9) . ? C16 C19' 1.552(14) . ? C16 C18' 1.552(13) . ? C16 C17 1.594(11) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C17' H17D 0.9600 . ? C17' H17E 0.9600 . ? C17' H17F 0.9600 . ? C18' H18D 0.9600 . ? C18' H18E 0.9600 . ? C18' H18F 0.9600 . ? C19' H19D 0.9600 . ? C19' H19E 0.9600 . ? C19' H19F 0.9600 . ? C20 C23 1.529(4) . ? C20 C21 1.535(3) . ? C20 C22 1.538(3) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C30 1.409(3) . ? C25 C26 1.424(3) . ? C26 C27 1.395(3) . ? C26 C44 1.531(3) . ? C27 C28 1.391(3) . ? C27 H27A 0.9300 . ? C28 C29 1.376(3) . ? C28 C40 1.543(3) . ? C29 C30 1.387(3) . ? C29 H29A 0.9300 . ? C30 C31 1.511(3) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.499(3) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C39 1.386(4) . ? C34 C35 1.400(3) . ? C35 C36 1.382(4) . ? C36 C37 1.396(5) . ? C36 H36A 0.9300 . ? C37 C38 1.363(5) . ? C37 H37A 0.9300 . ? C38 C39 1.357(5) . ? C38 H38A 0.9300 . ? C39 H39A 0.9300 . ? C40 C42 1.516(4) . ? C40 C43 1.528(4) . ? C40 C41 1.539(4) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C47 1.530(4) . ? C44 C46 1.531(4) . ? C44 C45 1.535(3) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? 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 O2 Li1 O1 96.88(17) . . ? O2 Li1 N1 123.5(2) . . ? O1 Li1 N1 103.13(17) . . ? O2 Li1 S1 136.92(19) . . ? O1 Li1 S1 103.13(15) . . ? N1 Li1 S1 88.56(13) . . ? O1 Li2 O2 97.96(18) . . ? O1 Li2 N2 128.4(2) . . ? O2 Li2 N2 102.83(17) . . ? O1 Li2 S2 132.44(19) . . ? O2 Li2 S2 101.50(14) . . ? N2 Li2 S2 88.60(13) . . ? C11 S1 C24 104.69(14) . . ? C11 S1 Li1 96.98(12) . . ? C24 S1 Li1 119.21(13) . . ? C35 S2 C48 104.87(16) . . ? C35 S2 Li2 100.56(11) . . ? C48 S2 Li2 121.34(14) . . ? C1 O1 Li2 159.78(18) . . ? C1 O1 Li1 114.87(16) . . ? Li2 O1 Li1 82.48(16) . . ? C25 O2 Li1 156.94(18) . . ? C25 O2 Li2 117.30(16) . . ? Li1 O2 Li2 82.34(16) . . ? C8 N1 C7 109.77(19) . . ? C8 N1 C9 110.08(19) . . ? C7 N1 C9 110.32(18) . . ? C8 N1 Li1 106.71(17) . . ? C7 N1 Li1 99.94(17) . . ? C9 N1 Li1 119.40(18) . . ? C32 N2 C31 109.09(17) . . ? C32 N2 C33 110.58(18) . . ? C31 N2 C33 110.33(16) . . ? C32 N2 Li2 107.09(17) . . ? C31 N2 Li2 99.02(17) . . ? C33 N2 Li2 119.88(16) . . ? O1 C1 C6 119.24(19) . . ? O1 C1 C2 122.55(19) . . ? C6 C1 C2 118.21(17) . . ? C3 C2 C1 117.90(19) . . ? C3 C2 C20 121.6(2) . . ? C1 C2 C20 120.48(17) . . ? C4 C3 C2 124.5(2) . . ? C4 C3 H3A 117.7 . . ? C2 C3 H3A 117.7 . . ? C3 C4 C5 116.39(19) . . ? C3 C4 C16 122.5(2) . . ? C5 C4 C16 121.2(2) . . ? C4 C5 C6 122.3(2) . . ? C4 C5 H5A 118.8 . . ? C6 C5 H5A 118.8 . . ? C5 C6 C1 120.6(2) . . ? C5 C6 C7 120.3(2) . . ? C1 C6 C7 119.07(18) . . ? N1 C7 C6 115.69(19) . . ? N1 C7 H7A 108.4 . . ? C6 C7 H7A 108.4 . . ? N1 C7 H7B 108.4 . . ? C6 C7 H7B 108.4 . . ? H7A C7 H7B 107.4 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C10 113.59(19) . . ? N1 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? N1 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C11 C10 C15 118.4(3) . . ? C11 C10 C9 121.0(2) . . ? C15 C10 C9 120.6(3) . . ? C10 C11 C12 119.7(2) . . ? C10 C11 S1 117.9(2) . . ? C12 C11 S1 122.4(2) . . ? C13 C12 C11 120.0(3) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C14 C13 C12 120.5(3) . . ? C14 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? C13 C14 C15 120.4(3) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C14 C15 C10 121.0(3) . . ? C14 C15 H15A 119.5 . . ? C10 C15 H15A 119.5 . . ? C19 C16 C17' 130.4(7) . . ? C19 C16 C18 114.1(10) . . ? C17' C16 C18 55.6(9) . . ? C19 C16 C4 114.2(3) . . ? C17' C16 C4 114.5(5) . . ? C18 C16 C4 109.4(4) . . ? C19 C16 C19' 54.6(9) . . ? C17' C16 C19' 102.9(12) . . ? C18 C16 C19' 144.0(6) . . ? C4 C16 C19' 106.0(5) . . ? C19 C16 C18' 61.0(9) . . ? C17' C16 C18' 111.1(10) . . ? C18 C16 C18' 60.2(8) . . ? C4 C16 C18' 107.6(5) . . ? C19' C16 C18' 114.8(8) . . ? C19 C16 C17 112.5(10) . . ? C17' C16 C17 44.8(9) . . ? C18 C16 C17 100.3(8) . . ? C4 C16 C17 105.1(4) . . ? C19' C16 C17 63.3(8) . . ? C18' C16 C17 146.1(5) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C17' H17D 109.5 . . ? C16 C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? C16 C17' H17F 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? C16 C18' H18D 109.5 . . ? C16 C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C16 C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? C16 C19' H19D 109.5 . . ? C16 C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? C16 C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? C23 C20 C2 109.14(19) . . ? C23 C20 C21 107.9(2) . . ? C2 C20 C21 112.20(18) . . ? C23 C20 C22 110.12(19) . . ? C2 C20 C22 110.3(2) . . ? C21 C20 C22 107.2(2) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? S1 C24 H24A 109.5 . . ? S1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? S1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O2 C25 C30 119.60(18) . . ? O2 C25 C26 122.27(18) . . ? C30 C25 C26 118.13(17) . . ? C27 C26 C25 117.56(19) . . ? C27 C26 C44 121.67(18) . . ? C25 C26 C44 120.76(17) . . ? C28 C27 C26 124.74(19) . . ? C28 C27 H27A 117.6 . . ? C26 C27 H27A 117.6 . . ? C29 C28 C27 116.22(18) . . ? C29 C28 C40 122.7(2) . . ? C27 C28 C40 121.01(19) . . ? C28 C29 C30 122.4(2) . . ? C28 C29 H29A 118.8 . . ? C30 C29 H29A 118.8 . . ? C29 C30 C25 120.97(19) . . ? C29 C30 C31 120.28(19) . . ? C25 C30 C31 118.74(18) . . ? N2 C31 C30 115.06(17) . . ? N2 C31 H31A 108.5 . . ? C30 C31 H31A 108.5 . . ? N2 C31 H31B 108.5 . . ? C30 C31 H31B 108.5 . . ? H31A C31 H31B 107.5 . . ? N2 C32 H32A 109.5 . . ? N2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N2 C33 C34 114.35(17) . . ? N2 C33 H33A 108.7 . . ? C34 C33 H33A 108.7 . . ? N2 C33 H33B 108.7 . . ? C34 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? C39 C34 C35 118.2(3) . . ? C39 C34 C33 120.2(2) . . ? C35 C34 C33 121.6(2) . . ? C36 C35 C34 119.3(3) . . ? C36 C35 S2 123.4(2) . . ? C34 C35 S2 117.32(19) . . ? C35 C36 C37 120.4(3) . . ? C35 C36 H36A 119.8 . . ? C37 C36 H36A 119.8 . . ? C38 C37 C36 120.0(3) . . ? C38 C37 H37A 120.0 . . ? C36 C37 H37A 120.0 . . ? C39 C38 C37 119.5(4) . . ? C39 C38 H38A 120.2 . . ? C37 C38 H38A 120.2 . . ? C38 C39 C34 122.5(3) . . ? C38 C39 H39A 118.7 . . ? C34 C39 H39A 118.7 . . ? C42 C40 C43 108.2(3) . . ? C42 C40 C41 108.8(2) . . ? C43 C40 C41 108.6(3) . . ? C42 C40 C28 109.22(19) . . ? C43 C40 C28 111.0(2) . . ? C41 C40 C28 110.95(19) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C47 C44 C46 109.7(2) . . ? C47 C44 C26 110.4(2) . . ? C46 C44 C26 109.8(2) . . ? C47 C44 C45 106.9(2) . . ? C46 C44 C45 107.7(2) . . ? C26 C44 C45 112.30(19) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? S2 C48 H48A 109.5 . . ? S2 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? S2 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.411 _refine_diff_density_min -0.212 _refine_diff_density_rms 0.053 #==END data_compound5 _database_code_depnum_ccdc_archive 'CCDC 646487' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H64 Li2 N2 O4' _chemical_formula_weight 626.79 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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.434(3) _cell_length_b 17.666(3) _cell_length_c 12.896(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.790(4) _cell_angle_gamma 90.00 _cell_volume 4041.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3605 _cell_measurement_theta_min 2.305 _cell_measurement_theta_max 21.209 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.030 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.9885 _exptl_absorpt_correction_T_max 0.9936 _exptl_absorpt_process_details EMPIRICAL _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45212 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.99 _reflns_number_total 7913 _reflns_number_gt 4031 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7913 _refine_ls_number_parameters 455 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1381 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.2160 _refine_ls_wR_factor_gt 0.1773 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.154 _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 Li1 Li 0.2882(2) 0.4077(3) 0.9265(4) 0.0634(12) Uani 1 1 d . B . Li2 Li 0.2052(3) 0.3475(3) 1.0254(4) 0.0630(12) Uani 1 1 d . B . O1 O 0.30409(9) 0.38096(10) 1.07546(14) 0.0555(5) Uani 1 1 d . . . O2 O 0.35146(15) 0.49640(16) 0.8930(3) 0.1155(10) Uani 1 1 d . . . O3 O 0.18830(9) 0.38433(10) 0.87898(14) 0.0541(5) Uani 1 1 d . . . O4 O 0.11994(12) 0.37321(15) 1.09010(17) 0.0812(7) Uani 1 1 d . . . N1 N 0.37097(13) 0.34028(14) 0.89425(18) 0.0620(6) Uani 1 1 d . . . N2 N 0.14859(13) 0.24241(14) 0.99271(17) 0.0622(7) Uani 1 1 d . . . C1 C 0.37372(14) 0.36704(14) 1.1336(2) 0.0475(6) Uani 1 1 d . B . C2 C 0.40470(15) 0.39917(16) 1.2381(2) 0.0579(7) Uani 1 1 d . . . C3 C 0.47760(16) 0.37882(17) 1.2944(2) 0.0618(8) Uani 1 1 d . . . H3A H 0.4975 0.4002 1.3621 0.074 Uiso 1 1 calc R . . C4 C 0.52309(14) 0.32883(16) 1.2569(2) 0.0541(7) Uani 1 1 d . . . C5 C 0.49290(14) 0.30061(14) 1.1550(2) 0.0520(7) Uani 1 1 d . B . H5A H 0.5220 0.2680 1.1262 0.062 Uiso 1 1 calc R . . C6 C 0.42083(14) 0.31866(14) 1.0931(2) 0.0484(6) Uani 1 1 d . . . C7 C 0.39064(16) 0.28487(16) 0.9833(2) 0.0571(7) Uani 1 1 d . B . H7A H 0.4280 0.2502 0.9701 0.069 Uiso 1 1 calc R . . H7B H 0.3460 0.2555 0.9826 0.069 Uiso 1 1 calc R . . C8 C 0.3437(2) 0.3006(2) 0.7908(3) 0.1006(13) Uani 1 1 d . B . H8A H 0.3834 0.2699 0.7783 0.151 Uiso 1 1 calc R . . H8B H 0.3281 0.3370 0.7338 0.151 Uiso 1 1 calc R . . H8C H 0.3017 0.2690 0.7927 0.151 Uiso 1 1 calc R . . C9 C 0.43354(18) 0.3911(2) 0.8926(3) 0.0846(10) Uani 1 1 d . B . H9A H 0.4651 0.3985 0.9654 0.102 Uiso 1 1 calc R A 1 H9B H 0.4642 0.3684 0.8505 0.102 Uiso 1 1 calc R A 1 C10 C 0.4057(7) 0.4628(10) 0.8468(14) 0.214(9) Uani 0.65 1 d P B 1 H10A H 0.4479 0.4973 0.8556 0.256 Uiso 0.65 1 calc PR B 1 H10B H 0.3831 0.4562 0.7701 0.256 Uiso 0.65 1 calc PR B 1 C10' C 0.4010(10) 0.4659(8) 0.8380(8) 0.067(5) Uani 0.35 1 d P B 2 H10C H 0.4416 0.5014 0.8400 0.080 Uiso 0.35 1 calc PR B 2 H10D H 0.3742 0.4567 0.7632 0.080 Uiso 0.35 1 calc PR B 2 C11 C 0.3698(4) 0.5583(4) 0.9557(4) 0.189(3) Uani 1 1 d . B . H11A H 0.3994 0.5919 0.9251 0.284 Uiso 1 1 calc R . . H11B H 0.3985 0.5435 1.0267 0.284 Uiso 1 1 calc R . . H11C H 0.3247 0.5837 0.9600 0.284 Uiso 1 1 calc R . . C12 C 0.60246(15) 0.30766(18) 1.3274(2) 0.0670(8) Uani 1 1 d . . . C13 C 0.6392(3) 0.2508(4) 1.2769(5) 0.217(4) Uani 1 1 d . . . H13A H 0.6403 0.2681 1.2067 0.326 Uiso 1 1 calc R . . H13B H 0.6117 0.2041 1.2702 0.326 Uiso 1 1 calc R . . H13C H 0.6898 0.2429 1.3206 0.326 Uiso 1 1 calc R . . C14 C 0.5985(2) 0.2806(3) 1.4380(4) 0.152(2) Uani 1 1 d . . . H14A H 0.5921 0.2267 1.4368 0.229 Uiso 1 1 calc R . . H14B H 0.5565 0.3043 1.4557 0.229 Uiso 1 1 calc R . . H14C H 0.6443 0.2939 1.4910 0.229 Uiso 1 1 calc R . . C15 C 0.6513(2) 0.3784(3) 1.3518(5) 0.156(2) Uani 1 1 d . . . H15A H 0.6584 0.3983 1.2860 0.234 Uiso 1 1 calc R . . H15B H 0.6994 0.3657 1.4000 0.234 Uiso 1 1 calc R . . H15C H 0.6269 0.4157 1.3848 0.234 Uiso 1 1 calc R . . C16 C 0.35773(18) 0.4523(2) 1.2890(3) 0.0775(10) Uani 1 1 d . . . C17 C 0.3294(2) 0.5194(2) 1.2147(3) 0.1036(13) Uani 1 1 d . . . H17A H 0.3717 0.5468 1.2035 0.155 Uiso 1 1 calc R . . H17B H 0.3002 0.5522 1.2469 0.155 Uiso 1 1 calc R . . H17C H 0.2986 0.5014 1.1467 0.155 Uiso 1 1 calc R . . C18 C 0.2899(2) 0.4092(2) 1.3074(3) 0.0952(12) Uani 1 1 d . . . H18A H 0.3075 0.3673 1.3551 0.143 Uiso 1 1 calc R . . H18B H 0.2591 0.3906 1.2397 0.143 Uiso 1 1 calc R . . H18C H 0.2607 0.4426 1.3388 0.143 Uiso 1 1 calc R . . C19 C 0.4039(3) 0.4841(3) 1.3979(3) 0.153(2) Uani 1 1 d . . . H19A H 0.4217 0.4431 1.4471 0.229 Uiso 1 1 calc R . . H19B H 0.3727 0.5169 1.4268 0.229 Uiso 1 1 calc R . . H19C H 0.4461 0.5121 1.3880 0.229 Uiso 1 1 calc R . . C20 C 0.11723(13) 0.37780(14) 0.82106(19) 0.0436(6) Uani 1 1 d . B . C21 C 0.07489(14) 0.43840(13) 0.76091(19) 0.0450(6) Uani 1 1 d . . . C22 C -0.00127(14) 0.42513(15) 0.7091(2) 0.0513(7) Uani 1 1 d . B . H22A H -0.0289 0.4652 0.6709 0.062 Uiso 1 1 calc R . . C23 C -0.03882(13) 0.35741(14) 0.7099(2) 0.0476(6) Uani 1 1 d . . . C24 C 0.00481(14) 0.29822(14) 0.76512(19) 0.0459(6) Uani 1 1 d . B . H24A H -0.0175 0.2511 0.7659 0.055 Uiso 1 1 calc R . . C25 C 0.08046(13) 0.30696(13) 0.81899(18) 0.0424(6) Uani 1 1 d . . . C26 C 0.12481(15) 0.23966(15) 0.8739(2) 0.0520(7) Uani 1 1 d . B . H26A H 0.0945 0.1946 0.8519 0.062 Uiso 1 1 calc R . . H26B H 0.1695 0.2346 0.8484 0.062 Uiso 1 1 calc R . . C27 C 0.1932(2) 0.1727(2) 1.0298(3) 0.1023(13) Uani 1 1 d . B . H27A H 0.1613 0.1291 1.0097 0.154 Uiso 1 1 calc R . . H27B H 0.2131 0.1741 1.1067 0.154 Uiso 1 1 calc R . . H27C H 0.2340 0.1697 0.9969 0.154 Uiso 1 1 calc R . . C28 C 0.0848(2) 0.2466(3) 1.0401(3) 0.0891(12) Uani 1 1 d . B . H28A H 0.0996 0.2251 1.1120 0.107 Uiso 1 1 calc R C 1 H28B H 0.0434 0.2165 0.9970 0.107 Uiso 1 1 calc R C 1 C29 C 0.0572(9) 0.3296(11) 1.0466(17) 0.122(7) Uani 0.60 1 d P B 1 H29A H 0.0311 0.3479 0.9752 0.146 Uiso 0.60 1 calc PR B 1 H29B H 0.0228 0.3319 1.0916 0.146 Uiso 0.60 1 calc PR B 1 C29' C 0.0566(12) 0.3205(9) 1.0501(19) 0.058(4) Uiso 0.40 1 d P B 2 H29C H 0.0254 0.3194 1.0997 0.069 Uiso 0.40 1 calc PR B 2 H29D H 0.0257 0.3375 0.9805 0.069 Uiso 0.40 1 calc PR B 2 C30 C 0.0986(3) 0.4478(3) 1.1041(4) 0.1143(14) Uani 1 1 d . B . H30A H 0.0570 0.4474 1.1356 0.171 Uiso 1 1 calc R . . H30B H 0.0837 0.4728 1.0354 0.171 Uiso 1 1 calc R . . H30C H 0.1403 0.4743 1.1507 0.171 Uiso 1 1 calc R . . C31 C -0.12231(15) 0.34572(18) 0.6540(2) 0.0628(8) Uani 1 1 d . B . C32 C -0.1669(9) 0.3181(8) 0.7331(12) 0.086(3) Uani 0.53 1 d P B 1 H32A H -0.1582 0.3521 0.7934 0.129 Uiso 0.53 1 calc PR B 1 H32B H -0.1503 0.2682 0.7582 0.129 Uiso 0.53 1 calc PR B 1 H32C H -0.2197 0.3169 0.6967 0.129 Uiso 0.53 1 calc PR B 1 C33 C -0.1560(13) 0.4206(13) 0.6050(18) 0.140(8) Uani 0.53 1 d P B 1 H33A H -0.1541 0.4566 0.6615 0.211 Uiso 0.53 1 calc PR B 1 H33B H -0.2074 0.4129 0.5645 0.211 Uiso 0.53 1 calc PR B 1 H33C H -0.1276 0.4396 0.5582 0.211 Uiso 0.53 1 calc PR B 1 C34 C -0.1290(10) 0.2941(11) 0.5706(17) 0.158(10) Uani 0.53 1 d P B 1 H34A H -0.1010 0.2492 0.5978 0.238 Uiso 0.53 1 calc PR B 1 H34B H -0.1095 0.3161 0.5156 0.238 Uiso 0.53 1 calc PR B 1 H34C H -0.1811 0.2814 0.5406 0.238 Uiso 0.53 1 calc PR B 1 C32' C -0.1561(13) 0.3142(18) 0.742(3) 0.218(15) Uani 0.47 1 d P B 2 H32D H -0.1313 0.2676 0.7692 0.328 Uiso 0.47 1 calc PR B 2 H32E H -0.2089 0.3050 0.7117 0.328 Uiso 0.47 1 calc PR B 2 H32F H -0.1490 0.3502 0.7994 0.328 Uiso 0.47 1 calc PR B 2 C33' C -0.1658(11) 0.4176(7) 0.6072(11) 0.057(3) Uani 0.47 1 d P B 2 H33D H -0.1443 0.4389 0.5537 0.085 Uiso 0.47 1 calc PR B 2 H33E H -0.1625 0.4538 0.6638 0.085 Uiso 0.47 1 calc PR B 2 H33F H -0.2177 0.4052 0.5747 0.085 Uiso 0.47 1 calc PR B 2 C34' C -0.1347(11) 0.2847(10) 0.5559(14) 0.079(4) Uani 0.47 1 d P B 2 H34D H -0.1109 0.2377 0.5833 0.118 Uiso 0.47 1 calc PR B 2 H34E H -0.1127 0.3039 0.5017 0.118 Uiso 0.47 1 calc PR B 2 H34F H -0.1877 0.2765 0.5250 0.118 Uiso 0.47 1 calc PR B 2 C35 C 0.11196(15) 0.51458(14) 0.7518(2) 0.0564(7) Uani 1 1 d . B . C36 C 0.05676(19) 0.57138(16) 0.6808(3) 0.0873(11) Uani 1 1 d . . . H36A H 0.0371 0.5505 0.6099 0.131 Uiso 1 1 calc R B . H36B H 0.0828 0.6178 0.6760 0.131 Uiso 1 1 calc R . . H36C H 0.0161 0.5812 0.7121 0.131 Uiso 1 1 calc R . . C37 C 0.17619(18) 0.50278(17) 0.6989(3) 0.0744(9) Uani 1 1 d . . . H37A H 0.1566 0.4800 0.6292 0.112 Uiso 1 1 calc R B . H37B H 0.2137 0.4702 0.7433 0.112 Uiso 1 1 calc R . . H37C H 0.1986 0.5507 0.6909 0.112 Uiso 1 1 calc R . . C38 C 0.1425(2) 0.55091(18) 0.8640(3) 0.0847(10) Uani 1 1 d . . . H38A H 0.1655 0.5987 0.8568 0.127 Uiso 1 1 calc R B . H38B H 0.1793 0.5180 0.9091 0.127 Uiso 1 1 calc R . . H38C H 0.1017 0.5587 0.8959 0.127 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 Li1 0.036(2) 0.071(3) 0.076(3) 0.010(2) 0.002(2) -0.004(2) Li2 0.044(3) 0.088(3) 0.053(3) 0.001(2) 0.006(2) -0.007(2) O1 0.0343(9) 0.0700(12) 0.0537(11) -0.0061(9) -0.0023(8) 0.0020(8) O2 0.0662(17) 0.0845(18) 0.196(3) 0.035(2) 0.036(2) -0.0116(14) O3 0.0348(9) 0.0663(12) 0.0547(10) 0.0056(9) 0.0008(8) -0.0068(8) O4 0.0540(13) 0.1131(19) 0.0767(15) -0.0125(13) 0.0183(11) -0.0068(13) N1 0.0471(14) 0.0879(17) 0.0469(13) -0.0023(12) 0.0055(11) -0.0046(12) N2 0.0508(14) 0.0798(17) 0.0498(13) 0.0178(12) 0.0032(12) -0.0063(12) C1 0.0353(13) 0.0526(15) 0.0485(15) 0.0007(12) 0.0009(12) -0.0010(11) C2 0.0458(15) 0.0669(18) 0.0542(16) -0.0140(14) 0.0020(13) 0.0060(13) C3 0.0477(16) 0.079(2) 0.0495(16) -0.0125(14) -0.0032(13) 0.0013(15) C4 0.0382(14) 0.0664(17) 0.0522(16) 0.0010(13) 0.0031(13) 0.0020(13) C5 0.0396(14) 0.0599(16) 0.0543(16) -0.0002(13) 0.0089(13) 0.0063(12) C6 0.0414(14) 0.0538(15) 0.0473(15) -0.0005(12) 0.0075(12) -0.0005(12) C7 0.0509(16) 0.0665(18) 0.0504(16) -0.0077(13) 0.0077(13) 0.0028(13) C8 0.100(3) 0.140(3) 0.0497(18) -0.014(2) 0.0006(19) 0.014(2) C9 0.0505(19) 0.119(3) 0.085(2) 0.021(2) 0.0203(18) -0.003(2) C10 0.068(8) 0.239(16) 0.36(2) 0.130(14) 0.101(10) 0.005(8) C10' 0.077(12) 0.070(8) 0.037(5) 0.036(5) -0.012(6) -0.008(7) C11 0.224(7) 0.200(6) 0.137(4) -0.029(4) 0.039(5) -0.152(6) C12 0.0365(15) 0.092(2) 0.0662(19) 0.0111(16) 0.0024(14) 0.0037(15) C13 0.114(4) 0.331(9) 0.152(5) -0.094(5) -0.055(4) 0.147(5) C14 0.072(3) 0.259(6) 0.113(3) 0.090(4) 0.001(3) 0.031(3) C15 0.063(3) 0.174(5) 0.191(5) 0.048(4) -0.034(3) -0.026(3) C16 0.061(2) 0.090(2) 0.071(2) -0.0311(18) -0.0002(17) 0.0177(18) C17 0.098(3) 0.072(2) 0.141(3) -0.028(2) 0.031(3) 0.014(2) C18 0.085(3) 0.127(3) 0.079(2) 0.001(2) 0.031(2) 0.038(2) C19 0.110(4) 0.201(5) 0.119(3) -0.103(4) -0.016(3) 0.055(3) C20 0.0354(13) 0.0552(15) 0.0394(13) -0.0007(11) 0.0087(11) -0.0019(11) C21 0.0393(14) 0.0465(14) 0.0475(14) 0.0019(11) 0.0091(12) 0.0006(11) C22 0.0421(15) 0.0552(16) 0.0531(15) 0.0086(12) 0.0069(13) 0.0088(12) C23 0.0333(13) 0.0599(16) 0.0470(14) 0.0004(12) 0.0063(11) -0.0023(12) C24 0.0395(14) 0.0494(14) 0.0457(14) 0.0029(11) 0.0061(12) -0.0052(11) C25 0.0375(13) 0.0491(14) 0.0388(13) 0.0022(11) 0.0075(11) 0.0006(11) C26 0.0445(15) 0.0559(16) 0.0506(15) 0.0081(12) 0.0042(12) -0.0013(12) C27 0.092(3) 0.097(3) 0.095(3) 0.046(2) -0.013(2) 0.004(2) C28 0.085(3) 0.125(3) 0.061(2) 0.002(2) 0.027(2) -0.034(2) C29 0.058(5) 0.230(17) 0.089(7) -0.033(8) 0.040(4) -0.058(7) C30 0.101(3) 0.121(4) 0.131(4) -0.019(3) 0.048(3) 0.000(3) C31 0.0351(15) 0.076(2) 0.0695(19) 0.0041(16) 0.0013(14) 0.0030(14) C32 0.041(6) 0.120(8) 0.098(7) 0.032(6) 0.020(5) 0.003(5) C33 0.038(7) 0.159(15) 0.192(17) -0.005(12) -0.024(8) 0.008(7) C34 0.050(6) 0.174(14) 0.196(16) -0.122(11) -0.061(7) 0.025(7) C32' 0.027(7) 0.35(3) 0.27(3) 0.12(2) 0.031(10) -0.030(11) C33' 0.038(6) 0.056(6) 0.066(6) -0.003(5) -0.004(5) 0.012(4) C34' 0.073(9) 0.071(6) 0.076(6) -0.020(6) -0.009(6) -0.016(5) C35 0.0510(16) 0.0471(15) 0.0700(18) 0.0034(13) 0.0148(15) -0.0022(13) C36 0.075(2) 0.0537(19) 0.128(3) 0.0280(19) 0.019(2) 0.0022(16) C37 0.070(2) 0.069(2) 0.087(2) 0.0158(17) 0.0251(19) -0.0096(16) C38 0.094(3) 0.062(2) 0.096(2) -0.0169(18) 0.022(2) -0.0168(18) _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 Li1 O3 1.823(5) . ? Li1 O1 1.922(5) . ? Li1 N1 2.064(6) . ? Li1 O2 2.068(5) . ? Li2 O1 1.856(5) . ? Li2 O3 1.941(5) . ? Li2 O4 2.022(5) . ? Li2 N2 2.116(5) . ? O1 C1 1.322(3) . ? O2 C11 1.348(6) . ? O2 C10' 1.408(18) . ? O2 C10 1.425(17) . ? O3 C20 1.325(3) . ? O4 C29 1.376(17) . ? O4 C30 1.401(4) . ? O4 C29' 1.47(2) . ? N1 C9 1.467(4) . ? N1 C8 1.469(4) . ? N1 C7 1.477(3) . ? N2 C28 1.468(4) . ? N2 C26 1.475(3) . ? N2 C27 1.486(4) . ? C1 C6 1.416(4) . ? C1 C2 1.429(3) . ? C2 C3 1.390(4) . ? C2 C16 1.540(4) . ? C3 C4 1.392(4) . ? C3 H3A 0.9300 . ? C4 C5 1.373(4) . ? C4 C12 1.544(4) . ? C5 C6 1.388(3) . ? C5 H5A 0.9300 . ? C6 C7 1.498(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.432(15) . ? C9 C10' 1.540(14) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10' H10C 0.9700 . ? C10' H10D 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.459(5) . ? C12 C15 1.522(5) . ? C12 C14 1.525(5) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.524(5) . ? C16 C19 1.537(4) . ? C16 C18 1.537(5) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C25 1.420(3) . ? C20 C21 1.424(3) . ? C21 C22 1.401(3) . ? C21 C35 1.528(3) . ? C22 C23 1.384(3) . ? C22 H22A 0.9300 . ? C23 C24 1.391(3) . ? C23 C31 1.526(3) . ? C24 C25 1.387(3) . ? C24 H24A 0.9300 . ? C25 C26 1.506(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29' 1.424(18) . ? C28 C29 1.563(18) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29' H29C 0.9700 . ? C29' H29D 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C34 1.39(2) . ? C31 C33 1.52(2) . ? C31 C33' 1.535(14) . ? C31 C32' 1.54(3) . ? C31 C32 1.552(15) . ? C31 C34' 1.63(2) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C32' H32D 0.9600 . ? C32' H32E 0.9600 . ? C32' H32F 0.9600 . ? C33' H33D 0.9600 . ? C33' H33E 0.9600 . ? C33' H33F 0.9600 . ? C34' H34D 0.9600 . ? C34' H34E 0.9600 . ? C34' H34F 0.9600 . ? C35 C37 1.533(4) . ? C35 C36 1.541(4) . ? C35 C38 1.542(4) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? 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 O3 Li1 O1 98.4(2) . . ? O3 Li1 N1 122.4(3) . . ? O1 Li1 N1 98.1(2) . . ? O3 Li1 O2 132.6(3) . . ? O1 Li1 O2 117.0(3) . . ? N1 Li1 O2 84.6(2) . . ? O1 Li2 O3 96.6(2) . . ? O1 Li2 O4 125.8(3) . . ? O3 Li2 O4 112.9(2) . . ? O1 Li2 N2 137.1(3) . . ? O3 Li2 N2 99.2(2) . . ? O4 Li2 N2 83.2(2) . . ? C1 O1 Li2 148.0(2) . . ? C1 O1 Li1 118.2(2) . . ? Li2 O1 Li1 82.1(2) . . ? C11 O2 C10' 121.4(7) . . ? C11 O2 C10 119.9(7) . . ? C10' O2 C10 5.4(9) . . ? C11 O2 Li1 123.7(4) . . ? C10' O2 Li1 107.2(6) . . ? C10 O2 Li1 105.7(6) . . ? C20 O3 Li1 164.3(2) . . ? C20 O3 Li2 113.1(2) . . ? Li1 O3 Li2 82.4(2) . . ? C29 O4 C30 110.1(8) . . ? C29 O4 C29' 5.6(14) . . ? C30 O4 C29' 114.6(7) . . ? C29 O4 Li2 111.6(8) . . ? C30 O4 Li2 122.8(3) . . ? C29' O4 Li2 110.2(8) . . ? C9 N1 C8 110.8(3) . . ? C9 N1 C7 112.9(2) . . ? C8 N1 C7 109.9(2) . . ? C9 N1 Li1 106.1(2) . . ? C8 N1 Li1 111.6(2) . . ? C7 N1 Li1 105.3(2) . . ? C28 N2 C26 112.9(2) . . ? C28 N2 C27 110.1(3) . . ? C26 N2 C27 106.8(3) . . ? C28 N2 Li2 106.3(3) . . ? C26 N2 Li2 103.1(2) . . ? C27 N2 Li2 117.6(2) . . ? O1 C1 C6 120.1(2) . . ? O1 C1 C2 122.6(2) . . ? C6 C1 C2 117.4(2) . . ? C3 C2 C1 118.1(2) . . ? C3 C2 C16 120.7(2) . . ? C1 C2 C16 121.1(2) . . ? C2 C3 C4 124.8(2) . . ? C2 C3 H3A 117.6 . . ? C4 C3 H3A 117.6 . . ? C5 C4 C3 115.9(2) . . ? C5 C4 C12 123.2(3) . . ? C3 C4 C12 120.9(2) . . ? C4 C5 C6 122.8(2) . . ? C4 C5 H5A 118.6 . . ? C6 C5 H5A 118.6 . . ? C5 C6 C1 120.9(2) . . ? C5 C6 C7 120.2(2) . . ? C1 C6 C7 118.8(2) . . ? N1 C7 C6 114.9(2) . . ? N1 C7 H7A 108.6 . . ? C6 C7 H7A 108.6 . . ? N1 C7 H7B 108.6 . . ? C6 C7 H7B 108.6 . . ? H7A C7 H7B 107.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 N1 110.6(5) . . ? C10 C9 C10' 3.1(11) . . ? N1 C9 C10' 108.8(7) . . ? C10 C9 H9A 109.5 . . ? N1 C9 H9A 109.5 . . ? C10' C9 H9A 112.6 . . ? C10 C9 H9B 109.5 . . ? N1 C9 H9B 109.5 . . ? C10' C9 H9B 108.3 . . ? H9A C9 H9B 108.1 . . ? O2 C10 C9 114.2(10) . . ? O2 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? O2 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? O2 C10' C9 108.9(8) . . ? O2 C10' H10C 109.9 . . ? C9 C10' H10C 109.9 . . ? O2 C10' H10D 109.9 . . ? C9 C10' H10D 109.9 . . ? H10C C10' H10D 108.3 . . ? O2 C11 H11A 109.5 . . ? O2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C15 109.7(5) . . ? C13 C12 C14 110.4(4) . . ? C15 C12 C14 103.9(4) . . ? C13 C12 C4 112.6(3) . . ? C15 C12 C4 109.6(3) . . ? C14 C12 C4 110.3(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 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C19 107.5(3) . . ? C17 C16 C18 109.2(3) . . ? C19 C16 C18 108.1(3) . . ? C17 C16 C2 110.0(3) . . ? C19 C16 C2 112.1(3) . . ? C18 C16 C2 109.8(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O3 C20 C25 118.8(2) . . ? O3 C20 C21 123.6(2) . . ? C25 C20 C21 117.7(2) . . ? C22 C21 C20 117.6(2) . . ? C22 C21 C35 121.5(2) . . ? C20 C21 C35 120.9(2) . . ? C23 C22 C21 125.4(2) . . ? C23 C22 H22A 117.3 . . ? C21 C22 H22A 117.3 . . ? C22 C23 C24 115.7(2) . . ? C22 C23 C31 123.8(2) . . ? C24 C23 C31 120.6(2) . . ? C25 C24 C23 122.4(2) . . ? C25 C24 H24A 118.8 . . ? C23 C24 H24A 118.8 . . ? C24 C25 C20 121.1(2) . . ? C24 C25 C26 119.4(2) . . ? C20 C25 C26 119.4(2) . . ? N2 C26 C25 115.6(2) . . ? N2 C26 H26A 108.4 . . ? C25 C26 H26A 108.4 . . ? N2 C26 H26B 108.4 . . ? C25 C26 H26B 108.4 . . ? H26A C26 H26B 107.4 . . ? N2 C27 H27A 109.5 . . ? N2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29' C28 N2 115.9(9) . . ? C29' C28 C29 3.7(16) . . ? N2 C28 C29 112.3(7) . . ? C29' C28 H28A 106.7 . . ? N2 C28 H28A 109.2 . . ? C29 C28 H28A 109.2 . . ? C29' C28 H28B 107.7 . . ? N2 C28 H28B 109.2 . . ? C29 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? O4 C29 C28 107.3(11) . . ? O4 C29 H29A 110.3 . . ? C28 C29 H29A 110.3 . . ? O4 C29 H29B 110.3 . . ? C28 C29 H29B 110.3 . . ? H29A C29 H29B 108.5 . . ? C28 C29' O4 109.7(13) . . ? C28 C29' H29C 109.7 . . ? O4 C29' H29C 109.7 . . ? C28 C29' H29D 109.7 . . ? O4 C29' H29D 109.7 . . ? H29C C29' H29D 108.2 . . ? O4 C30 H30A 109.5 . . ? O4 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O4 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C34 C31 C33 108.0(12) . . ? C34 C31 C23 108.7(8) . . ? C33 C31 C23 108.9(9) . . ? C34 C31 C33' 108.1(10) . . ? C33 C31 C33' 7.4(16) . . ? C23 C31 C33' 115.2(7) . . ? C34 C31 C32' 111.4(15) . . ? C33 C31 C32' 114.8(14) . . ? C23 C31 C32' 105.0(10) . . ? C33' C31 C32' 108.5(13) . . ? C34 C31 C32 110.6(12) . . ? C33 C31 C32 108.5(11) . . ? C23 C31 C32 112.2(6) . . ? C33' C31 C32 101.9(9) . . ? C32' C31 C32 7.8(15) . . ? C34 C31 C34' 2.9(14) . . ? C33 C31 C34' 107.3(10) . . ? C23 C31 C34' 111.5(7) . . ? C33' C31 C34' 107.1(8) . . ? C32' C31 C34' 109.4(14) . . ? C32 C31 C34' 108.3(8) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C32' H32D 109.5 . . ? C31 C32' H32E 109.5 . . ? H32D C32' H32E 109.5 . . ? C31 C32' H32F 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? C31 C33' H33D 109.5 . . ? C31 C33' H33E 109.5 . . ? H33D C33' H33E 109.5 . . ? C31 C33' H33F 109.5 . . ? H33D C33' H33F 109.5 . . ? H33E C33' H33F 109.5 . . ? C31 C34' H34D 109.5 . . ? C31 C34' H34E 109.5 . . ? H34D C34' H34E 109.5 . . ? C31 C34' H34F 109.5 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? C21 C35 C37 109.3(2) . . ? C21 C35 C36 112.5(2) . . ? C37 C35 C36 106.8(2) . . ? C21 C35 C38 110.5(2) . . ? C37 C35 C38 110.2(3) . . ? C36 C35 C38 107.5(3) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.441 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.041 #==END data_compound7 _database_code_depnum_ccdc_archive 'CCDC 670604' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H40 Li N O3' _chemical_formula_weight 421.53 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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3335(10) _cell_length_b 10.6740(11) _cell_length_c 12.8376(13) _cell_angle_alpha 99.290(2) _cell_angle_beta 90.890(2) _cell_angle_gamma 112.650(2) _cell_volume 1284.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2526 _cell_measurement_theta_min 2.407 _cell_measurement_theta_max 25.858 _exptl_crystal_description parallelpied _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.475 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7371 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 26.01 _reflns_number_total 4984 _reflns_number_gt 3086 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4984 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.2149 _refine_ls_wR_factor_gt 0.1918 _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_restrained_S_all 1.199 _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 Li Li 0.3667(4) 0.5588(4) 0.1088(3) 0.0572(9) Uani 1 1 d . . . O1 O 0.55897(15) 0.63844(15) 0.14712(11) 0.0503(4) Uani 1 1 d . . . O2 O 0.2116(2) 0.5663(2) 0.20278(16) 0.0801(6) Uani 1 1 d . . . O3 O 0.3023(2) 0.39017(18) 0.01009(15) 0.0757(6) Uani 1 1 d . . . H1 H 0.349(4) 0.372(4) -0.049(3) 0.107(11) Uiso 1 1 d . . . N N 0.3510(2) 0.7360(2) 0.06436(15) 0.0584(5) Uani 1 1 d . . . C1 C 0.5976(2) 0.7573(2) 0.21543(16) 0.0417(5) Uani 1 1 d . . . C2 C 0.6641(2) 0.7782(2) 0.31744(16) 0.0409(5) Uani 1 1 d . . . C3 C 0.7025(2) 0.9066(2) 0.38284(17) 0.0451(5) Uani 1 1 d . . . H3A H 0.7479 0.9198 0.4492 0.054 Uiso 1 1 calc R . . C4 C 0.6770(2) 1.0169(2) 0.35507(17) 0.0467(5) Uani 1 1 d . . . C5 C 0.6082(2) 0.9920(2) 0.25639(18) 0.0500(5) Uani 1 1 d . . . H5A H 0.5876 1.0621 0.2354 0.060 Uiso 1 1 calc R . . C6 C 0.5681(2) 0.8666(2) 0.18661(16) 0.0468(5) Uani 1 1 d . . . C7 C 0.4941(3) 0.8453(2) 0.07973(18) 0.0575(6) Uani 1 1 d . . . H7A H 0.4884 0.9314 0.0700 0.069 Uiso 1 1 calc R . . H7B H 0.5499 0.8222 0.0257 0.069 Uiso 1 1 calc R . . C8 C 0.2957(3) 0.7091(4) -0.0467(2) 0.0903(10) Uani 1 1 d . . . H8A H 0.2899 0.7912 -0.0638 0.135 Uiso 1 1 calc R . . H8B H 0.2036 0.6361 -0.0569 0.135 Uiso 1 1 calc R . . H8C H 0.3572 0.6824 -0.0919 0.135 Uiso 1 1 calc R . . C9 C 0.2571(3) 0.7699(3) 0.1373(2) 0.0741(8) Uani 1 1 d . . . H9A H 0.2137 0.8221 0.1053 0.089 Uiso 1 1 calc R . . H9B H 0.3120 0.8280 0.2018 0.089 Uiso 1 1 calc R . . C10 C 0.1454(3) 0.6457(4) 0.1644(3) 0.0912(10) Uani 1 1 d . . . H10A H 0.0914 0.6724 0.2182 0.109 Uiso 1 1 calc R . . H10B H 0.0821 0.5924 0.1022 0.109 Uiso 1 1 calc R . . C11 C 0.1284(4) 0.4733(4) 0.2643(3) 0.1116(13) Uani 1 1 d . . . H11A H 0.0650 0.5091 0.2990 0.167 Uiso 1 1 calc R . . H11B H 0.1878 0.4609 0.3164 0.167 Uiso 1 1 calc R . . H11C H 0.0753 0.3861 0.2194 0.167 Uiso 1 1 calc R . . C12 C 0.7249(3) 1.1573(2) 0.42866(19) 0.0569(6) Uani 1 1 d . . . C13 C 0.8437(5) 1.2611(4) 0.3847(4) 0.162(2) Uani 1 1 d . . . H13A H 0.9197 1.2307 0.3768 0.243 Uiso 1 1 calc R . . H13B H 0.8755 1.3484 0.4322 0.243 Uiso 1 1 calc R . . H13C H 0.8123 1.2711 0.3170 0.243 Uiso 1 1 calc R . . C14 C 0.6064(4) 1.2038(4) 0.4429(4) 0.1357(17) Uani 1 1 d . . . H14A H 0.5312 1.1368 0.4719 0.203 Uiso 1 1 calc R . . H14B H 0.5733 1.2135 0.3756 0.203 Uiso 1 1 calc R . . H14C H 0.6386 1.2911 0.4904 0.203 Uiso 1 1 calc R . . C15 C 0.7693(7) 1.1510(4) 0.5392(3) 0.179(3) Uani 1 1 d . . . H15A H 0.6943 1.0807 0.5657 0.269 Uiso 1 1 calc R . . H15B H 0.7903 1.2386 0.5843 0.269 Uiso 1 1 calc R . . H15C H 0.8514 1.1296 0.5382 0.269 Uiso 1 1 calc R . . C16 C 0.6918(2) 0.6598(2) 0.35527(18) 0.0526(6) Uani 1 1 d . . . C17 C 0.7962(3) 0.6234(3) 0.2860(2) 0.0766(8) Uani 1 1 d . . . H17A H 0.8137 0.5499 0.3093 0.115 Uiso 1 1 calc R . . H17B H 0.8829 0.7030 0.2917 0.115 Uiso 1 1 calc R . . H17C H 0.7574 0.5944 0.2135 0.115 Uiso 1 1 calc R . . C18 C 0.5531(3) 0.5334(3) 0.3494(2) 0.0727(8) Uani 1 1 d . . . H18A H 0.5712 0.4604 0.3731 0.109 Uiso 1 1 calc R . . H18B H 0.5119 0.5030 0.2776 0.109 Uiso 1 1 calc R . . H18C H 0.4894 0.5577 0.3939 0.109 Uiso 1 1 calc R . . C19 C 0.7531(3) 0.6992(3) 0.4709(2) 0.0779(8) Uani 1 1 d . . . H19A H 0.7686 0.6230 0.4912 0.117 Uiso 1 1 calc R . . H19B H 0.6883 0.7212 0.5155 0.117 Uiso 1 1 calc R . . H19C H 0.8408 0.7779 0.4785 0.117 Uiso 1 1 calc R . . C20 C 0.1727(3) 0.2766(3) 0.0003(2) 0.0765(8) Uani 1 1 d . . . H20A H 0.1661 0.2137 -0.0651 0.092 Uiso 1 1 calc R . . H20B H 0.0974 0.3088 -0.0049 0.092 Uiso 1 1 calc R . . C21 C 0.1512(2) 0.1989(2) 0.09029(18) 0.0572(6) Uani 1 1 d . . . C22 C 0.0172(3) 0.1200(3) 0.1126(2) 0.0669(7) Uani 1 1 d . . . H22A H -0.0595 0.1153 0.0709 0.080 Uiso 1 1 calc R . . C23 C -0.0062(4) 0.0477(3) 0.1953(2) 0.0802(8) Uani 1 1 d . . . H23A H -0.0976 -0.0050 0.2086 0.096 Uiso 1 1 calc R . . C24 C 0.1036(5) 0.0536(4) 0.2566(3) 0.0948(10) Uani 1 1 d . . . H24A H 0.0875 0.0052 0.3124 0.114 Uiso 1 1 calc R . . C25 C 0.2382(4) 0.1299(4) 0.2376(3) 0.0949(10) Uani 1 1 d . . . H25A H 0.3136 0.1326 0.2798 0.114 Uiso 1 1 calc R . . C26 C 0.2624(3) 0.2040(3) 0.1543(2) 0.0747(8) Uani 1 1 d . . . H26A H 0.3542 0.2571 0.1421 0.090 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 Li 0.056(2) 0.050(2) 0.057(2) 0.0038(17) 0.0097(18) 0.0134(17) O1 0.0529(9) 0.0446(8) 0.0504(9) 0.0012(7) 0.0055(7) 0.0189(7) O2 0.0709(12) 0.0787(13) 0.0904(14) 0.0194(11) 0.0342(10) 0.0267(10) O3 0.0736(12) 0.0545(11) 0.0704(12) -0.0075(8) 0.0270(10) 0.0009(9) N 0.0581(12) 0.0643(13) 0.0513(11) 0.0044(9) -0.0060(9) 0.0250(10) C1 0.0371(11) 0.0392(11) 0.0467(12) 0.0081(9) 0.0106(9) 0.0123(9) C2 0.0371(11) 0.0401(11) 0.0480(12) 0.0101(9) 0.0079(9) 0.0169(8) C3 0.0421(12) 0.0464(12) 0.0468(12) 0.0093(9) 0.0051(9) 0.0170(9) C4 0.0439(12) 0.0407(11) 0.0525(13) 0.0073(9) 0.0073(10) 0.0138(9) C5 0.0507(13) 0.0413(12) 0.0609(14) 0.0156(10) 0.0051(11) 0.0187(10) C6 0.0471(12) 0.0425(12) 0.0492(12) 0.0111(9) 0.0052(10) 0.0147(9) C7 0.0639(15) 0.0529(14) 0.0542(13) 0.0170(11) 0.0034(11) 0.0187(11) C8 0.088(2) 0.103(2) 0.0688(18) 0.0082(17) -0.0227(16) 0.0293(18) C9 0.0639(17) 0.0782(19) 0.086(2) 0.0035(15) 0.0021(14) 0.0390(15) C10 0.0636(19) 0.103(3) 0.106(2) 0.0043(19) 0.0146(17) 0.0366(18) C11 0.132(3) 0.077(2) 0.108(3) 0.0094(19) 0.070(2) 0.023(2) C12 0.0599(15) 0.0392(12) 0.0651(15) 0.0025(10) 0.0042(11) 0.0154(11) C13 0.158(4) 0.058(2) 0.194(5) -0.029(2) 0.083(4) -0.023(2) C14 0.105(3) 0.091(3) 0.191(4) -0.052(3) 0.009(3) 0.047(2) C15 0.351(8) 0.071(2) 0.093(3) -0.029(2) -0.078(4) 0.079(4) C16 0.0596(14) 0.0507(13) 0.0560(13) 0.0129(10) 0.0055(11) 0.0297(11) C17 0.084(2) 0.084(2) 0.0862(19) 0.0159(15) 0.0155(15) 0.0585(17) C18 0.083(2) 0.0545(15) 0.0805(18) 0.0273(13) 0.0076(15) 0.0212(14) C19 0.107(2) 0.0716(18) 0.0667(17) 0.0145(14) -0.0092(16) 0.0477(17) C20 0.0651(18) 0.0713(18) 0.0671(17) 0.0090(13) 0.0024(13) 0.0002(13) C21 0.0514(14) 0.0518(13) 0.0541(13) -0.0079(10) 0.0082(11) 0.0113(10) C22 0.0575(15) 0.0578(15) 0.0702(16) -0.0016(12) 0.0101(12) 0.0113(12) C23 0.086(2) 0.0587(17) 0.0780(19) 0.0040(14) 0.0269(17) 0.0115(14) C24 0.119(3) 0.084(2) 0.078(2) 0.0182(17) 0.020(2) 0.035(2) C25 0.109(3) 0.111(3) 0.076(2) 0.0036(19) -0.0084(19) 0.060(2) C26 0.0581(16) 0.085(2) 0.0720(18) -0.0049(15) 0.0063(14) 0.0254(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li O1 1.856(4) . ? Li O3 1.898(4) . ? Li O2 2.039(4) . ? Li N 2.124(4) . ? Li C1 2.669(4) . ? O1 C1 1.334(2) . ? O2 C11 1.402(3) . ? O2 C10 1.414(4) . ? O3 C20 1.405(3) . ? O3 H1 0.94(4) . ? N C9 1.463(3) . ? N C8 1.469(3) . ? N C7 1.474(3) . ? C1 C2 1.413(3) . ? C1 C6 1.414(3) . ? C2 C3 1.393(3) . ? C2 C16 1.545(3) . ? C3 C4 1.397(3) . ? C3 H3A 0.9300 . ? C4 C5 1.378(3) . ? C4 C12 1.530(3) . ? C5 C6 1.393(3) . ? C5 H5A 0.9300 . ? C6 C7 1.501(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.481(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C14 1.491(4) . ? C12 C13 1.493(4) . ? C12 C15 1.505(4) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C19 1.532(3) . ? C16 C17 1.532(3) . ? C16 C18 1.534(3) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.499(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.379(3) . ? C21 C26 1.381(4) . ? C22 C23 1.382(4) . ? C22 H22A 0.9300 . ? C23 C24 1.345(5) . ? C23 H23A 0.9300 . ? C24 C25 1.364(5) . ? C24 H24A 0.9300 . ? C25 C26 1.400(4) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Li O3 115.6(2) . . ? O1 Li O2 126.6(2) . . ? O3 Li O2 110.4(2) . . ? O1 Li N 96.41(18) . . ? O3 Li N 119.5(2) . . ? O2 Li N 83.05(16) . . ? O1 Li C1 27.47(8) . . ? O3 Li C1 143.0(2) . . ? O2 Li C1 102.85(16) . . ? N Li C1 79.45(14) . . ? C1 O1 Li 112.59(16) . . ? C11 O2 C10 114.0(2) . . ? C11 O2 Li 131.2(2) . . ? C10 O2 Li 109.4(2) . . ? C20 O3 Li 129.1(2) . . ? C20 O3 H1 106(2) . . ? Li O3 H1 125(2) . . ? C9 N C8 111.8(2) . . ? C9 N C7 111.9(2) . . ? C8 N C7 109.7(2) . . ? C9 N Li 104.51(18) . . ? C8 N Li 111.9(2) . . ? C7 N Li 106.94(17) . . ? O1 C1 C2 122.69(17) . . ? O1 C1 C6 119.21(18) . . ? C2 C1 C6 118.07(18) . . ? O1 C1 Li 39.94(12) . . ? C2 C1 Li 133.08(16) . . ? C6 C1 Li 94.61(16) . . ? C3 C2 C1 118.62(17) . . ? C3 C2 C16 121.12(18) . . ? C1 C2 C16 120.26(18) . . ? C2 C3 C4 124.2(2) . . ? C2 C3 H3A 117.9 . . ? C4 C3 H3A 117.9 . . ? C5 C4 C3 115.8(2) . . ? C5 C4 C12 122.04(19) . . ? C3 C4 C12 122.2(2) . . ? C4 C5 C6 123.03(19) . . ? C4 C5 H5A 118.5 . . ? C6 C5 H5A 118.5 . . ? C5 C6 C1 120.23(19) . . ? C5 C6 C7 120.83(18) . . ? C1 C6 C7 118.93(19) . . ? N C7 C6 113.82(18) . . ? N C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? N C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N C8 H8A 109.5 . . ? N C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N C9 C10 112.6(2) . . ? N C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? N C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? O2 C10 C9 107.7(2) . . ? O2 C10 H10A 110.2 . . ? C9 C10 H10A 110.2 . . ? O2 C10 H10B 110.2 . . ? C9 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? O2 C11 H11A 109.5 . . ? O2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C13 110.2(3) . . ? C14 C12 C15 103.9(4) . . ? C13 C12 C15 109.8(4) . . ? C14 C12 C4 111.1(2) . . ? C13 C12 C4 109.7(2) . . ? C15 C12 C4 112.0(2) . . ? 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 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C19 C16 C17 108.5(2) . . ? C19 C16 C18 106.4(2) . . ? C17 C16 C18 110.6(2) . . ? C19 C16 C2 112.13(19) . . ? C17 C16 C2 109.26(18) . . ? C18 C16 C2 109.98(18) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O3 C20 C21 114.1(2) . . ? O3 C20 H20A 108.7 . . ? C21 C20 H20A 108.7 . . ? O3 C20 H20B 108.7 . . ? C21 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? C22 C21 C26 117.4(3) . . ? C22 C21 C20 120.4(2) . . ? C26 C21 C20 122.2(2) . . ? C21 C22 C23 121.8(3) . . ? C21 C22 H22A 119.1 . . ? C23 C22 H22A 119.1 . . ? C24 C23 C22 119.9(3) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C25 120.6(3) . . ? C23 C24 H24A 119.7 . . ? C25 C24 H24A 119.7 . . ? C24 C25 C26 119.7(3) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C21 C26 C25 120.6(3) . . ? C21 C26 H26A 119.7 . . ? C25 C26 H26A 119.7 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.536 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.044 #==END