Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Eichler, Barrett E.' 'Olmstead, Marylin' 'Power, Philip P.' 'Prust, Jorg' 'Roesky, H. W.' 'Stender, Matthias' 'Wright, Robert J.' _publ_contact_author_name 'Dr Philip P Power' _publ_contact_author_address ; Dr Philip P Power Department of Chemistry University of California Davis One Shields Avenue Davis California 95616 UNITED STATES OF AMERICA ; _publ_contact_author_email 'pppower@ucdavis.edu' _publ_section_title ; The synthesis and structure of lithium derivatives of the sterically encumbered beta-diketiminate ligand [{(2,6-i-Pr2H3C6)N(CH3)C}2CH]-, and a modified synthesis of the aminoimine precursor ; data_be45 _database_code_CSD 162354 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'NacNacLi.THF' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H49 Li N2 O' _chemical_formula_weight 496.68 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' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.936(5) _cell_length_b 14.757(5) _cell_length_c 15.720(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.499(6) _cell_angle_gamma 90.00 _cell_volume 3099.7(19) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 415 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 23.39 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.064 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9779 _exptl_absorpt_correction_T_max 0.9858 _exptl_absorpt_process_details ; SADABS: an empirical absorption program by G. M. Sheldrick using the method described by Blessing, R. H.; Acta Cryst. A51, 1995, 33. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 frames remeasured' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% '<0.01' _diffrn_reflns_number 20948 _diffrn_reflns_av_R_equivalents 0.0872 _diffrn_reflns_av_sigmaI/netI 0.0739 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 30.00 _reflns_number_total 4513 _reflns_number_gt 2707 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL v. 5.10' _computing_structure_solution 'XS, Bruker SHELXTL v. 5.10' _computing_structure_refinement 'XL, Bruker SHELXTL v. 5.10' _computing_molecular_graphics 'XP, Bruker SHELXTL v. 5.10' _computing_publication_material 'XCIF, Bruker SHELXTL v. 5.10' _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^)+(0.0894P)^2^+6.0603P] 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 4513 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1356 _refine_ls_R_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.2159 _refine_ls_wR_factor_gt 0.1772 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 N1 N 0.90141(12) 0.06499(11) 0.26351(11) 0.0143(4) Uani 1 1 d . . . O1 O 1.0000 0.27552(15) 0.2500 0.0292(6) Uani 1 2 d S . . C1 C 0.91552(15) -0.02385(14) 0.26575(14) 0.0149(4) Uani 1 1 d . . . Li1 Li 1.0000 0.1542(5) 0.2500 0.0274(14) Uani 1 2 d S . . C2 C 1.0000 -0.0653(2) 0.2500 0.0158(6) Uani 1 2 d S . . H2A H 1.0000 -0.1297 0.2500 0.019 Uiso 1 2 calc SR . . C3 C 0.83840(17) -0.08646(15) 0.28563(17) 0.0221(5) Uani 1 1 d . . . H3A H 0.7834 -0.0504 0.2953 0.033 Uiso 1 1 calc R . . H3B H 0.8697 -0.1219 0.3390 0.033 Uiso 1 1 calc R . . H3C H 0.8123 -0.1275 0.2354 0.033 Uiso 1 1 calc R . . C4 C 0.81209(15) 0.10118(14) 0.27643(14) 0.0146(4) Uani 1 1 d . . . C5 C 0.72444(15) 0.10687(14) 0.20421(14) 0.0168(4) Uani 1 1 d . . . C6 C 0.64019(16) 0.14923(15) 0.21764(16) 0.0222(5) Uani 1 1 d . . . H6A H 0.5808 0.1535 0.1697 0.027 Uiso 1 1 calc R . . C7 C 0.64167(17) 0.18515(16) 0.29953(17) 0.0242(5) Uani 1 1 d . . . H7A H 0.5836 0.2135 0.3075 0.029 Uiso 1 1 calc R . . C8 C 0.72766(17) 0.17949(16) 0.36927(16) 0.0232(5) Uani 1 1 d . . . H8A H 0.7282 0.2044 0.4251 0.028 Uiso 1 1 calc R . . C9 C 0.81436(16) 0.13774(14) 0.35960(15) 0.0178(4) Uani 1 1 d . . . C10 C 0.90663(18) 0.13059(17) 0.43818(15) 0.0248(5) Uani 1 1 d . . . H10A H 0.9586 0.0966 0.4185 0.030 Uiso 1 1 calc R . . C11 C 0.8846(2) 0.0771(2) 0.51385(18) 0.0412(7) Uani 1 1 d . . . H11A H 0.8574 0.0175 0.4920 0.062 Uiso 1 1 calc R . . H11B H 0.8356 0.1102 0.5360 0.062 Uiso 1 1 calc R . . H11C H 0.9465 0.0693 0.5620 0.062 Uiso 1 1 calc R . . C12 C 0.9501(2) 0.2236(2) 0.47171(19) 0.0380(7) Uani 1 1 d . . . H12A H 0.9644 0.2572 0.4229 0.057 Uiso 1 1 calc R . . H12B H 1.0121 0.2156 0.5198 0.057 Uiso 1 1 calc R . . H12C H 0.9016 0.2574 0.4939 0.057 Uiso 1 1 calc R . . C13 C 0.72364(17) 0.07069(15) 0.11358(15) 0.0204(5) Uani 1 1 d . . . H13A H 0.7787 0.0251 0.1228 0.024 Uiso 1 1 calc R . . C14 C 0.6260(2) 0.0230(2) 0.06482(19) 0.0388(7) Uani 1 1 d . . . H14A H 0.6305 0.0012 0.0072 0.058 Uiso 1 1 calc R . . H14B H 0.5702 0.0657 0.0558 0.058 Uiso 1 1 calc R . . H14C H 0.6149 -0.0284 0.1003 0.058 Uiso 1 1 calc R . . C15 C 0.7462(2) 0.14636(18) 0.05580(18) 0.0340(6) Uani 1 1 d . . . H15A H 0.8088 0.1766 0.0876 0.051 Uiso 1 1 calc R . . H15B H 0.6914 0.1905 0.0424 0.051 Uiso 1 1 calc R . . H15C H 0.7530 0.1206 0.0003 0.051 Uiso 1 1 calc R . . C16 C 1.08874(19) 0.33236(17) 0.2727(2) 0.0322(6) Uani 1 1 d . . . H16A H 1.1221 0.3310 0.2249 0.039 Uiso 1 1 calc R . . H16B H 1.1368 0.3116 0.3286 0.039 Uiso 1 1 calc R . . C17 C 1.05173(19) 0.42641(16) 0.28338(18) 0.0296(6) Uani 1 1 d . . . H17A H 1.0954 0.4732 0.2687 0.036 Uiso 1 1 calc R . . H17B H 1.0476 0.4366 0.3445 0.036 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 N1 0.0135(8) 0.0150(8) 0.0146(8) 0.0006(7) 0.0042(7) -0.0004(6) O1 0.0195(12) 0.0153(11) 0.0537(17) 0.000 0.0118(11) 0.000 C1 0.0142(9) 0.0170(9) 0.0125(9) 0.0004(8) 0.0021(7) -0.0019(8) Li1 0.004(2) 0.064(4) 0.016(3) 0.000 0.006(2) 0.000 C2 0.0157(13) 0.0142(13) 0.0177(14) 0.000 0.0051(11) 0.000 C3 0.0187(11) 0.0168(10) 0.0326(13) 0.0032(9) 0.0103(9) -0.0021(8) C4 0.0135(9) 0.0142(9) 0.0184(10) 0.0019(8) 0.0079(8) -0.0014(7) C5 0.0158(10) 0.0157(9) 0.0190(11) 0.0029(8) 0.0050(8) -0.0016(8) C6 0.0139(10) 0.0222(11) 0.0281(13) 0.0059(9) 0.0020(9) 0.0009(8) C7 0.0195(11) 0.0218(11) 0.0351(14) 0.0037(10) 0.0137(10) 0.0046(9) C8 0.0266(12) 0.0230(11) 0.0248(12) -0.0004(9) 0.0149(10) 0.0027(9) C9 0.0184(10) 0.0187(10) 0.0172(10) 0.0009(8) 0.0065(8) 0.0000(8) C10 0.0248(12) 0.0333(13) 0.0158(11) -0.0030(9) 0.0048(9) 0.0052(10) C11 0.0477(17) 0.0479(17) 0.0229(14) 0.0086(12) 0.0018(12) 0.0006(14) C12 0.0308(14) 0.0471(17) 0.0333(15) -0.0091(13) 0.0045(12) -0.0081(12) C13 0.0193(10) 0.0221(11) 0.0181(11) 0.0017(9) 0.0025(8) -0.0021(8) C14 0.0311(14) 0.0540(18) 0.0282(14) -0.0097(13) 0.0038(11) -0.0162(13) C15 0.0488(17) 0.0317(14) 0.0248(13) 0.0051(11) 0.0157(12) -0.0011(12) C16 0.0214(12) 0.0222(12) 0.0510(17) 0.0017(11) 0.0069(12) -0.0054(9) C17 0.0349(14) 0.0200(11) 0.0359(14) -0.0054(10) 0.0133(11) -0.0056(10) _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 N1 C1 1.325(3) . ? N1 C4 1.421(3) . ? N1 Li1 1.958(5) . ? O1 C16 1.452(3) . ? O1 C16 1.452(3) 2_755 ? O1 Li1 1.790(7) . ? C1 C2 1.410(2) . ? C1 C3 1.516(3) . ? Li1 N1 1.958(5) 2_755 ? C2 C1 1.410(2) 2_755 ? C4 C9 1.406(3) . ? C4 C5 1.414(3) . ? C5 C6 1.398(3) . ? C5 C13 1.519(3) . ? C6 C7 1.387(4) . ? C7 C8 1.378(3) . ? C8 C9 1.402(3) . ? C9 C10 1.513(3) . ? C10 C12 1.532(4) . ? C10 C11 1.530(4) . ? C13 C15 1.527(3) . ? C13 C14 1.530(3) . ? C16 C17 1.507(4) . ? C17 C17 1.523(5) 2_755 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C4 119.84(17) . . ? C1 N1 Li1 124.4(2) . . ? C4 N1 Li1 115.7(2) . . ? C16 O1 C16 109.5(3) . 2_755 ? C16 O1 Li1 125.27(13) . . ? C16 O1 Li1 125.27(13) 2_755 . ? N1 C1 C2 123.4(2) . . ? N1 C1 C3 120.01(18) . . ? C2 C1 C3 116.6(2) . . ? O1 Li1 N1 132.27(16) . . ? O1 Li1 N1 132.27(16) . 2_755 ? N1 Li1 N1 95.5(3) . 2_755 ? C1 C2 C1 128.6(3) 2_755 . ? C9 C4 C5 120.64(19) . . ? C9 C4 N1 119.19(18) . . ? C5 C4 N1 119.97(19) . . ? C6 C5 C4 118.4(2) . . ? C6 C5 C13 121.07(19) . . ? C4 C5 C13 120.45(19) . . ? C7 C6 C5 121.3(2) . . ? C8 C7 C6 119.7(2) . . ? C7 C8 C9 121.5(2) . . ? C8 C9 C4 118.5(2) . . ? C8 C9 C10 120.1(2) . . ? C4 C9 C10 121.46(19) . . ? C9 C10 C12 112.3(2) . . ? C9 C10 C11 111.0(2) . . ? C12 C10 C11 110.0(2) . . ? C5 C13 C15 110.67(19) . . ? C5 C13 C14 113.6(2) . . ? C15 C13 C14 110.0(2) . . ? O1 C16 C17 105.4(2) . . ? C16 C17 C17 102.13(16) . 2_755 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.889 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.066 data_be46 _database_code_CSD 162355 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(NacNacLi)2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H39.50 Li N2' _chemical_formula_weight 423.07 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' _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 12.4708(14) _cell_length_b 14.0455(16) _cell_length_c 15.1235(17) _cell_angle_alpha 90.765(3) _cell_angle_beta 91.189(3) _cell_angle_gamma 102.979(3) _cell_volume 2580.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 2313 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 30.19 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 922 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9865 _exptl_absorpt_correction_T_max 0.9895 _exptl_absorpt_process_details ; SADABS: an empirical absorption program by G. M. Sheldrick using the method described by Blessing, R. H.; Acta Cryst. A51, 1995, 33. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 frames remeasured' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% '<0.01' _diffrn_reflns_number 9315 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0872 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.25 _reflns_number_total 9315 _reflns_number_gt 4630 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL v. 5.10' _computing_structure_solution 'XS, Bruker SHELXTL v. 5.10' _computing_structure_refinement 'XL, Bruker SHELXTL v. 5.10' _computing_molecular_graphics 'XP, Bruker SHELXTL v. 5.10' _computing_publication_material 'XCIF, Bruker SHELXTL v. 5.10' _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^)+(0.1223P)^2^+0.1214P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0118(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9315 _refine_ls_number_parameters 591 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1546 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.2406 _refine_ls_wR_factor_gt 0.1956 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.5954(5) 0.8972(5) 0.3971(4) 0.0463(16) Uani 1 1 d . . . N1 N 0.6451(2) 0.81020(19) 0.31946(17) 0.0328(7) Uani 1 1 d . . . N2 N 0.5921(2) 1.0060(2) 0.3225(2) 0.0378(7) Uani 1 1 d . . . C1 C 0.6609(3) 0.8331(2) 0.2354(2) 0.0423(9) Uani 1 1 d . . . C2 C 0.6334(3) 0.9159(2) 0.1968(2) 0.0416(9) Uani 1 1 d . . . H2A H 0.6386 0.9184 0.1343 0.050 Uiso 1 1 calc R . . C3 C 0.6001(3) 0.9940(3) 0.2361(2) 0.0385(9) Uani 1 1 d . . . C4 C 0.7121(5) 0.7706(3) 0.1749(2) 0.0809(17) Uani 1 1 d . . . H4A H 0.6702 0.7027 0.1766 0.121 Uiso 1 1 calc R . . H4B H 0.7883 0.7741 0.1945 0.121 Uiso 1 1 calc R . . H4C H 0.7111 0.7943 0.1143 0.121 Uiso 1 1 calc R . . C5 C 0.5709(3) 1.0688(3) 0.1734(3) 0.0513(10) Uani 1 1 d . . . H5A H 0.6182 1.1333 0.1871 0.077 Uiso 1 1 calc R . . H5B H 0.4937 1.0715 0.1806 0.077 Uiso 1 1 calc R . . H5C H 0.5820 1.0499 0.1123 0.077 Uiso 1 1 calc R . . C6 C 0.6784(3) 0.7249(2) 0.3519(2) 0.0315(8) Uani 1 1 d . . . C7 C 0.7864(3) 0.7332(2) 0.3842(2) 0.0313(8) Uani 1 1 d . . . C8 C 0.8132(3) 0.6538(2) 0.4260(2) 0.0383(9) Uani 1 1 d . . . H8A H 0.8859 0.6588 0.4488 0.046 Uiso 1 1 calc R . . C9 C 0.7355(3) 0.5676(2) 0.4348(2) 0.0428(9) Uani 1 1 d . . . H9A H 0.7542 0.5143 0.4647 0.051 Uiso 1 1 calc R . . C10 C 0.6309(3) 0.5589(2) 0.4001(2) 0.0394(9) Uani 1 1 d . . . H10A H 0.5787 0.4986 0.4050 0.047 Uiso 1 1 calc R . . C11 C 0.5994(3) 0.6361(2) 0.3580(2) 0.0326(8) Uani 1 1 d . A . C12 C 0.4840(3) 0.6254(2) 0.3190(2) 0.0325(8) Uani 1 1 d . . . C13A C 0.4860(5) 0.6070(5) 0.2204(4) 0.0318(15) Uiso 0.50 1 d P A 1 H13A H 0.5622 0.6131 0.2024 0.048 Uiso 0.50 1 calc PR A 1 H13B H 0.4540 0.6551 0.1892 0.048 Uiso 0.50 1 calc PR A 1 H13C H 0.4431 0.5411 0.2058 0.048 Uiso 0.50 1 calc PR A 1 C14A C 0.4080(6) 0.5406(5) 0.3641(5) 0.0396(17) Uiso 0.50 1 d P A 1 H14A H 0.4251 0.4789 0.3449 0.059 Uiso 0.50 1 calc PR A 1 H14B H 0.3313 0.5400 0.3480 0.059 Uiso 0.50 1 calc PR A 1 H14C H 0.4186 0.5483 0.4284 0.059 Uiso 0.50 1 calc PR A 1 C13B C 0.4473(6) 0.5351(5) 0.2599(5) 0.0417(18) Uiso 0.50 1 d P A 2 H13D H 0.5045 0.5323 0.2170 0.062 Uiso 0.50 1 calc PR A 2 H13E H 0.3788 0.5381 0.2283 0.062 Uiso 0.50 1 calc PR A 2 H13F H 0.4350 0.4765 0.2961 0.062 Uiso 0.50 1 calc PR A 2 C14B C 0.3892(6) 0.6267(5) 0.3852(5) 0.0393(17) Uiso 0.50 1 d P A 2 H14D H 0.4104 0.6839 0.4248 0.059 Uiso 0.50 1 calc PR A 2 H14E H 0.3760 0.5671 0.4201 0.059 Uiso 0.50 1 calc PR A 2 H14F H 0.3218 0.6299 0.3519 0.059 Uiso 0.50 1 calc PR A 2 C15 C 0.8737(3) 0.8274(2) 0.3742(2) 0.0341(8) Uani 1 1 d . . . H15A H 0.8468 0.8658 0.3268 0.041 Uiso 1 1 calc R . . C16 C 0.9837(3) 0.8090(3) 0.3453(3) 0.0544(11) Uani 1 1 d . . . H16A H 0.9726 0.7686 0.2911 0.082 Uiso 1 1 calc R . . H16B H 1.0149 0.7752 0.3922 0.082 Uiso 1 1 calc R . . H16C H 1.0345 0.8716 0.3339 0.082 Uiso 1 1 calc R . . C17 C 0.8880(4) 0.8893(3) 0.4585(3) 0.0583(12) Uani 1 1 d . . . H17A H 0.8166 0.9010 0.4755 0.087 Uiso 1 1 calc R . . H17B H 0.9393 0.9519 0.4485 0.087 Uiso 1 1 calc R . . H17C H 0.9175 0.8549 0.5060 0.087 Uiso 1 1 calc R . . C18 C 0.5606(3) 1.0909(3) 0.3565(3) 0.0456(10) Uani 1 1 d . . . C19 C 0.6385(3) 1.1783(3) 0.3734(3) 0.0445(10) Uani 1 1 d . . . C20 C 0.6064(4) 1.2547(3) 0.4182(3) 0.0597(12) Uani 1 1 d . . . H20A H 0.6591 1.3139 0.4304 0.072 Uiso 1 1 calc R . . C21 C 0.4989(4) 1.2454(3) 0.4449(3) 0.0655(14) Uani 1 1 d . . . H21A H 0.4784 1.2968 0.4771 0.079 Uiso 1 1 calc R . . C22 C 0.4227(4) 1.1614(3) 0.4242(3) 0.0624(13) Uani 1 1 d . . . H22A H 0.3489 1.1555 0.4421 0.075 Uiso 1 1 calc R . . C23 C 0.4499(3) 1.0836(3) 0.3776(3) 0.0516(11) Uani 1 1 d . . . C24 C 0.3623(3) 0.9942(3) 0.3499(3) 0.0577(12) Uani 1 1 d . . . H24A H 0.3958 0.9579 0.3047 0.069 Uiso 1 1 calc R . . C25 C 0.3341(4) 0.9277(4) 0.4268(3) 0.0738(14) Uani 1 1 d . . . H25A H 0.4014 0.9120 0.4512 0.111 Uiso 1 1 calc R . . H25B H 0.2827 0.8674 0.4069 0.111 Uiso 1 1 calc R . . H25C H 0.2999 0.9603 0.4724 0.111 Uiso 1 1 calc R . . C26 C 0.2605(3) 1.0185(4) 0.3059(3) 0.0788(16) Uani 1 1 d . . . H26A H 0.2139 0.9590 0.2795 0.118 Uiso 1 1 calc R . . H26B H 0.2833 1.0667 0.2598 0.118 Uiso 1 1 calc R . . H26C H 0.2190 1.0455 0.3504 0.118 Uiso 1 1 calc R . . C27 C 0.7576(3) 1.1939(3) 0.3425(3) 0.0439(9) Uani 1 1 d . . . H27A H 0.7624 1.1357 0.3054 0.053 Uiso 1 1 calc R . . C28 C 0.7885(3) 1.2832(3) 0.2848(3) 0.0576(12) Uani 1 1 d . . . H28A H 0.7345 1.2782 0.2360 0.086 Uiso 1 1 calc R . . H28B H 0.8617 1.2868 0.2608 0.086 Uiso 1 1 calc R . . H28C H 0.7894 1.3423 0.3203 0.086 Uiso 1 1 calc R . . C29 C 0.8417(4) 1.2025(3) 0.4166(3) 0.0654(12) Uani 1 1 d . . . H29A H 0.8298 1.1408 0.4484 0.098 Uiso 1 1 calc R . . H29B H 0.8344 1.2553 0.4575 0.098 Uiso 1 1 calc R . . H29C H 0.9157 1.2171 0.3923 0.098 Uiso 1 1 calc R . . Li2 Li 0.1009(5) 0.4028(4) 0.0992(3) 0.0328(13) Uani 1 1 d . . . N3 N 0.1483(2) 0.31632(18) 0.17986(16) 0.0269(6) Uani 1 1 d . . . N4 N 0.0817(3) 0.5063(2) 0.17676(18) 0.0400(8) Uani 1 1 d . B . C30 C 0.1546(3) 0.3366(2) 0.2654(2) 0.0301(8) Uani 1 1 d . . . C31 C 0.1221(3) 0.4167(2) 0.3037(2) 0.0398(9) Uani 1 1 d . B . H31A H 0.1263 0.4199 0.3664 0.048 Uiso 1 1 calc R . . C32 C 0.0845(3) 0.4924(2) 0.2641(2) 0.0465(10) Uani 1 1 d . . . C33 C 0.1991(3) 0.2716(3) 0.3288(2) 0.0457(10) Uani 1 1 d . . . H33A H 0.2741 0.2690 0.3126 0.069 Uiso 1 1 calc R . . H33B H 0.1520 0.2055 0.3258 0.069 Uiso 1 1 calc R . . H33C H 0.2001 0.2981 0.3892 0.069 Uiso 1 1 calc R . . C34A C 0.0706(6) 0.5662(4) 0.3296(4) 0.0273(15) Uiso 0.50 1 d P B 1 H34A H 0.1424 0.5980 0.3557 0.041 Uiso 0.50 1 calc PR B 1 H34B H 0.0222 0.5348 0.3761 0.041 Uiso 0.50 1 calc PR B 1 H34C H 0.0377 0.6152 0.3007 0.041 Uiso 0.50 1 calc PR B 1 C34B C 0.0103(6) 0.5532(5) 0.3207(5) 0.0349(17) Uiso 0.50 1 d P B 2 H34D H -0.0674 0.5306 0.3029 0.052 Uiso 0.50 1 calc PR B 2 H34E H 0.0345 0.6231 0.3089 0.052 Uiso 0.50 1 calc PR B 2 H34F H 0.0194 0.5422 0.3840 0.052 Uiso 0.50 1 calc PR B 2 C35 C 0.1784(3) 0.2296(2) 0.1481(2) 0.0296(8) Uani 1 1 d . . . C36 C 0.2854(3) 0.2358(3) 0.1156(2) 0.0336(8) Uani 1 1 d . . . C37 C 0.3067(3) 0.1537(3) 0.0727(2) 0.0413(9) Uani 1 1 d . . . H37A H 0.3777 0.1571 0.0496 0.050 Uiso 1 1 calc R . . C38 C 0.2279(3) 0.0682(3) 0.0629(2) 0.0436(10) Uani 1 1 d . . . H38A H 0.2438 0.0140 0.0318 0.052 Uiso 1 1 calc R . . C39 C 0.1252(3) 0.0614(3) 0.0988(2) 0.0396(9) Uani 1 1 d . . . H39A H 0.0715 0.0016 0.0933 0.048 Uiso 1 1 calc R . . C40 C 0.0996(3) 0.1407(2) 0.1427(2) 0.0300(8) Uani 1 1 d . . . C41 C -0.0123(3) 0.1294(2) 0.1849(2) 0.0314(8) Uani 1 1 d . . . H41A H -0.0084 0.1885 0.2236 0.038 Uiso 1 1 calc R . . C42 C -0.0386(3) 0.0411(3) 0.2441(3) 0.0517(11) Uani 1 1 d . . . H42A H 0.0213 0.0447 0.2878 0.078 Uiso 1 1 calc R . . H42B H -0.0468 -0.0187 0.2080 0.078 Uiso 1 1 calc R . . H42C H -0.1074 0.0403 0.2746 0.078 Uiso 1 1 calc R . . C43 C -0.1051(3) 0.1262(3) 0.1182(3) 0.0562(11) Uani 1 1 d . . . H43A H -0.0924 0.1879 0.0864 0.084 Uiso 1 1 calc R . . H43B H -0.1750 0.1165 0.1488 0.084 Uiso 1 1 calc R . . H43C H -0.1078 0.0721 0.0760 0.084 Uiso 1 1 calc R . . C44 C 0.3756(3) 0.3269(3) 0.1299(2) 0.0370(9) Uani 1 1 d . . . H44A H 0.3447 0.3746 0.1655 0.044 Uiso 1 1 calc R . . C45 C 0.4176(4) 0.3757(3) 0.0449(3) 0.0575(11) Uani 1 1 d . . . H45A H 0.3579 0.3980 0.0142 0.086 Uiso 1 1 calc R . . H45B H 0.4436 0.3290 0.0069 0.086 Uiso 1 1 calc R . . H45C H 0.4784 0.4319 0.0585 0.086 Uiso 1 1 calc R . . C46 C 0.4722(3) 0.3037(4) 0.1835(4) 0.0832(18) Uani 1 1 d . . . H46A H 0.4443 0.2669 0.2360 0.125 Uiso 1 1 calc R . . H46B H 0.5233 0.3648 0.2018 0.125 Uiso 1 1 calc R . . H46C H 0.5107 0.2646 0.1469 0.125 Uiso 1 1 calc R . . C47 C 0.0438(4) 0.5885(2) 0.1435(2) 0.0433(10) Uani 1 1 d . . . C48 C 0.1192(4) 0.6782(3) 0.1305(2) 0.0465(10) Uani 1 1 d . B . C49 C 0.0814(4) 0.7534(3) 0.0896(3) 0.0531(11) Uani 1 1 d . . . H49A H 0.1310 0.8145 0.0816 0.064 Uiso 1 1 calc R B . C50 C -0.0267(4) 0.7407(3) 0.0603(2) 0.0516(11) Uani 1 1 d . B . H50A H -0.0503 0.7918 0.0306 0.062 Uiso 1 1 calc R . . C51 C -0.1000(4) 0.6534(3) 0.0746(2) 0.0496(10) Uani 1 1 d . . . H51A H -0.1743 0.6450 0.0545 0.060 Uiso 1 1 calc R B . C52 C -0.0674(4) 0.5767(3) 0.1180(2) 0.0470(10) Uani 1 1 d . B . C53 C -0.1513(4) 0.4850(3) 0.1423(3) 0.0557(11) Uani 1 1 d . . . C54A C -0.1577(7) 0.4191(6) 0.0694(5) 0.049(2) Uiso 0.50 1 d P B 1 H54A H -0.0904 0.3942 0.0679 0.073 Uiso 0.50 1 calc PR B 1 H54B H -0.1658 0.4531 0.0144 0.073 Uiso 0.50 1 calc PR B 1 H54C H -0.2214 0.3644 0.0757 0.073 Uiso 0.50 1 calc PR B 1 C54B C -0.2188(7) 0.4276(6) 0.0545(5) 0.049(2) Uiso 0.50 1 d P B 2 H54D H -0.1670 0.4053 0.0157 0.073 Uiso 0.50 1 calc PR B 2 H54E H -0.2548 0.4723 0.0222 0.073 Uiso 0.50 1 calc PR B 2 H54F H -0.2745 0.3712 0.0735 0.073 Uiso 0.50 1 calc PR B 2 C55 C -0.2507(3) 0.5103(3) 0.1873(3) 0.0534(11) Uani 1 1 d . B . H55A H -0.2250 0.5587 0.2349 0.080 Uiso 1 1 calc R . . H55B H -0.2962 0.4511 0.2122 0.080 Uiso 1 1 calc R . . H55C H -0.2945 0.5373 0.1437 0.080 Uiso 1 1 calc R . . C56 C 0.2390(4) 0.6943(3) 0.1616(3) 0.0536(11) Uani 1 1 d . . . C57A C 0.3006(7) 0.7743(6) 0.1025(5) 0.055(2) Uiso 0.50 1 d P B 1 H57A H 0.2983 0.7491 0.0416 0.083 Uiso 0.50 1 calc PR B 1 H57B H 0.3773 0.7950 0.1235 0.083 Uiso 0.50 1 calc PR B 1 H57C H 0.2657 0.8302 0.1044 0.083 Uiso 0.50 1 calc PR B 1 C58A C 0.2425(7) 0.7165(6) 0.2528(5) 0.052(2) Uiso 0.50 1 d P B 1 H58A H 0.2081 0.6578 0.2850 0.078 Uiso 0.50 1 calc PR B 1 H58B H 0.2026 0.7680 0.2637 0.078 Uiso 0.50 1 calc PR B 1 H58C H 0.3193 0.7391 0.2731 0.078 Uiso 0.50 1 calc PR B 1 C57B C 0.3382(7) 0.7072(7) 0.0960(6) 0.060(2) Uiso 0.50 1 d P B 2 H57D H 0.3228 0.6544 0.0513 0.090 Uiso 0.50 1 calc PR B 2 H57E H 0.4058 0.7048 0.1293 0.090 Uiso 0.50 1 calc PR B 2 H57F H 0.3475 0.7703 0.0669 0.090 Uiso 0.50 1 calc PR B 2 C58B C 0.2853(7) 0.7908(6) 0.2270(6) 0.055(2) Uiso 0.50 1 d P B 2 H58D H 0.2316 0.7933 0.2728 0.083 Uiso 0.50 1 calc PR B 2 H58E H 0.2962 0.8503 0.1920 0.083 Uiso 0.50 1 calc PR B 2 H58F H 0.3554 0.7858 0.2548 0.083 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.052(4) 0.043(4) 0.048(4) 0.011(3) 0.006(3) 0.019(3) N1 0.0385(17) 0.0287(15) 0.0278(16) 0.0041(12) -0.0085(13) 0.0009(13) N2 0.0353(17) 0.0363(17) 0.0456(19) 0.0108(14) 0.0031(14) 0.0154(13) C1 0.062(3) 0.0265(19) 0.030(2) -0.0026(15) -0.0089(18) -0.0054(17) C2 0.060(3) 0.029(2) 0.0284(19) 0.0047(15) -0.0117(17) -0.0054(17) C3 0.035(2) 0.036(2) 0.040(2) 0.0133(17) -0.0072(17) 0.0004(16) C4 0.190(6) 0.030(2) 0.024(2) -0.0056(17) 0.000(3) 0.028(3) C5 0.048(2) 0.050(2) 0.055(3) 0.022(2) -0.0117(19) 0.0090(19) C6 0.047(2) 0.0226(17) 0.0206(17) -0.0017(13) -0.0039(15) 0.0004(15) C7 0.044(2) 0.0214(17) 0.0251(18) -0.0014(14) -0.0054(15) 0.0015(15) C8 0.048(2) 0.0296(19) 0.0321(19) 0.0006(15) -0.0106(17) -0.0020(17) C9 0.062(3) 0.0281(19) 0.033(2) 0.0066(15) -0.0133(18) 0.0003(18) C10 0.054(2) 0.0269(19) 0.0305(19) 0.0020(15) -0.0085(17) -0.0038(17) C11 0.046(2) 0.0266(18) 0.0211(17) -0.0051(14) -0.0004(15) -0.0006(16) C12 0.037(2) 0.0284(18) 0.0286(18) -0.0077(14) 0.0029(15) 0.0002(15) C15 0.045(2) 0.0235(18) 0.0291(19) -0.0008(14) -0.0020(16) -0.0010(15) C16 0.048(2) 0.034(2) 0.081(3) 0.011(2) 0.009(2) 0.0062(18) C17 0.069(3) 0.046(2) 0.044(2) -0.0073(19) -0.002(2) -0.020(2) C18 0.045(2) 0.044(2) 0.056(2) 0.0213(19) 0.0121(19) 0.0237(19) C19 0.047(2) 0.036(2) 0.056(2) 0.0172(18) 0.0116(19) 0.0200(19) C20 0.061(3) 0.042(2) 0.087(3) 0.024(2) 0.035(2) 0.030(2) C21 0.071(3) 0.053(3) 0.089(3) 0.029(2) 0.038(3) 0.043(3) C22 0.052(3) 0.063(3) 0.086(3) 0.042(3) 0.031(2) 0.036(2) C23 0.041(2) 0.055(3) 0.068(3) 0.030(2) 0.010(2) 0.026(2) C24 0.042(2) 0.065(3) 0.073(3) 0.034(2) 0.007(2) 0.024(2) C25 0.070(3) 0.075(3) 0.075(3) 0.036(3) 0.003(3) 0.011(3) C26 0.042(3) 0.103(4) 0.097(4) 0.053(3) 0.004(2) 0.025(3) C27 0.044(2) 0.037(2) 0.057(2) 0.0024(18) 0.0093(19) 0.0201(18) C28 0.059(3) 0.042(2) 0.075(3) 0.013(2) 0.026(2) 0.016(2) C29 0.057(3) 0.074(3) 0.067(3) 0.008(2) 0.014(2) 0.018(2) Li2 0.040(3) 0.032(3) 0.030(3) -0.003(2) -0.001(2) 0.015(3) N3 0.0283(15) 0.0271(15) 0.0246(15) -0.0009(11) 0.0005(12) 0.0052(12) N4 0.064(2) 0.0264(16) 0.0313(17) 0.0016(13) 0.0105(15) 0.0124(14) C30 0.0309(19) 0.0265(18) 0.0290(19) 0.0020(14) -0.0023(14) -0.0015(14) C31 0.068(3) 0.0236(18) 0.0248(18) -0.0051(15) 0.0025(17) 0.0030(17) C32 0.084(3) 0.0227(19) 0.031(2) -0.0040(15) 0.010(2) 0.0088(19) C33 0.060(3) 0.043(2) 0.032(2) 0.0093(17) -0.0057(18) 0.0070(19) C35 0.0362(19) 0.0311(19) 0.0254(17) 0.0077(14) 0.0058(15) 0.0149(15) C36 0.0334(19) 0.043(2) 0.0294(18) 0.0133(16) 0.0059(15) 0.0174(17) C37 0.045(2) 0.048(2) 0.040(2) 0.0157(17) 0.0174(18) 0.0269(19) C38 0.060(3) 0.036(2) 0.043(2) 0.0072(17) 0.0226(19) 0.024(2) C39 0.048(2) 0.032(2) 0.041(2) 0.0067(16) 0.0149(18) 0.0125(17) C40 0.0351(19) 0.0282(18) 0.0305(18) 0.0059(14) 0.0040(15) 0.0144(15) C41 0.038(2) 0.0277(18) 0.0310(18) -0.0007(14) 0.0052(15) 0.0111(15) C42 0.055(3) 0.048(2) 0.058(3) 0.019(2) 0.019(2) 0.020(2) C43 0.042(2) 0.086(3) 0.042(2) 0.002(2) 0.0084(19) 0.016(2) C44 0.0268(19) 0.045(2) 0.041(2) 0.0143(17) 0.0044(16) 0.0106(16) C45 0.075(3) 0.045(2) 0.050(3) 0.017(2) 0.008(2) 0.006(2) C46 0.034(2) 0.092(4) 0.119(4) 0.068(3) -0.016(3) 0.001(2) C47 0.079(3) 0.0261(19) 0.029(2) -0.0030(15) 0.0143(19) 0.0187(19) C48 0.078(3) 0.028(2) 0.037(2) -0.0011(16) 0.019(2) 0.016(2) C49 0.090(4) 0.029(2) 0.042(2) 0.0015(17) 0.014(2) 0.014(2) C50 0.090(3) 0.029(2) 0.038(2) 0.0036(17) 0.011(2) 0.018(2) C51 0.081(3) 0.040(2) 0.032(2) -0.0011(17) 0.009(2) 0.023(2) C52 0.073(3) 0.031(2) 0.040(2) -0.0008(17) 0.014(2) 0.017(2) C53 0.083(3) 0.036(2) 0.048(2) -0.0086(18) 0.022(2) 0.012(2) C55 0.054(3) 0.042(2) 0.062(3) -0.002(2) -0.004(2) 0.007(2) C56 0.070(3) 0.042(2) 0.053(3) 0.0053(19) 0.024(2) 0.018(2) _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 N1 1.894(7) . ? Li1 N2 1.919(7) . ? N1 C1 1.323(4) . ? N1 C6 1.442(4) . ? N2 C3 1.325(4) . ? N2 C18 1.429(4) . ? C1 C2 1.413(5) . ? C1 C4 1.507(5) . ? C2 C3 1.388(5) . ? C3 C5 1.523(4) . ? C6 C7 1.403(5) . ? C6 C11 1.411(4) . ? C7 C8 1.391(4) . ? C7 C15 1.524(4) . ? C8 C9 1.380(5) . ? C9 C10 1.374(5) . ? C10 C11 1.390(5) . ? C11 C12 1.518(5) . ? C12 C13A 1.511(7) . ? C12 C13B 1.520(8) . ? C12 C14A 1.525(7) . ? C12 C14B 1.568(7) . ? C15 C17 1.518(5) . ? C15 C16 1.524(5) . ? C18 C19 1.400(5) . ? C18 C23 1.405(5) . ? C19 C20 1.398(5) . ? C19 C27 1.535(5) . ? C20 C21 1.387(5) . ? C21 C22 1.366(6) . ? C22 C23 1.401(6) . ? C23 C24 1.516(6) . ? C24 C25 1.498(6) . ? C24 C26 1.529(5) . ? C27 C29 1.505(6) . ? C27 C28 1.520(5) . ? Li2 N3 1.909(6) . ? Li2 N4 1.916(6) . ? Li2 C51 2.732(6) 2_565 ? N3 C30 1.318(4) . ? N3 C35 1.433(4) . ? N4 C32 1.339(4) . ? N4 C47 1.435(4) . ? C30 C31 1.402(4) . ? C30 C33 1.514(4) . ? C31 C32 1.390(5) . ? C32 C34A 1.466(7) . ? C32 C34B 1.639(7) . ? C35 C40 1.405(4) . ? C35 C36 1.416(4) . ? C36 C37 1.394(5) . ? C36 C44 1.512(5) . ? C37 C38 1.376(5) . ? C38 C39 1.385(5) . ? C39 C40 1.391(4) . ? C40 C41 1.523(4) . ? C41 C43 1.512(5) . ? C41 C42 1.519(5) . ? C44 C45 1.513(5) . ? C44 C46 1.535(5) . ? C47 C52 1.404(5) . ? C47 C48 1.412(5) . ? C48 C49 1.396(5) . ? C48 C56 1.524(6) . ? C49 C50 1.382(6) . ? C50 C51 1.377(5) . ? C51 C52 1.400(5) . ? C51 Li2 2.732(6) 2_565 ? C52 C53 1.521(5) . ? C53 C54A 1.420(8) . ? C53 C55 1.534(5) . ? C53 C54B 1.657(9) . ? C56 C58A 1.407(8) . ? C56 C57A 1.522(9) . ? C56 C57B 1.581(9) . ? C56 C58B 1.654(9) . ? 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 N1 Li1 N2 102.3(3) . . ? C1 N1 C6 118.8(3) . . ? C1 N1 Li1 119.5(3) . . ? C6 N1 Li1 121.3(3) . . ? C3 N2 C18 119.9(3) . . ? C3 N2 Li1 118.2(3) . . ? C18 N2 Li1 120.8(3) . . ? N1 C1 C2 123.7(3) . . ? N1 C1 C4 120.3(3) . . ? C2 C1 C4 115.9(3) . . ? C3 C2 C1 130.0(3) . . ? N2 C3 C2 124.3(3) . . ? N2 C3 C5 119.6(3) . . ? C2 C3 C5 116.1(3) . . ? C7 C6 C11 120.7(3) . . ? C7 C6 N1 119.6(3) . . ? C11 C6 N1 119.4(3) . . ? C8 C7 C6 118.9(3) . . ? C8 C7 C15 120.0(3) . . ? C6 C7 C15 121.1(3) . . ? C9 C8 C7 120.8(3) . . ? C10 C9 C8 119.9(3) . . ? C9 C10 C11 121.7(3) . . ? C10 C11 C6 117.9(3) . . ? C10 C11 C12 121.3(3) . . ? C6 C11 C12 120.8(3) . . ? C13A C12 C11 109.1(3) . . ? C13A C12 C13B 46.3(4) . . ? C11 C12 C13B 113.1(4) . . ? C13A C12 C14A 111.2(4) . . ? C11 C12 C14A 108.3(4) . . ? C13B C12 C14A 66.4(4) . . ? C13A C12 C14B 133.4(4) . . ? C11 C12 C14B 117.3(4) . . ? C13B C12 C14B 107.3(4) . . ? C14A C12 C14B 50.5(4) . . ? C17 C15 C16 110.8(3) . . ? C17 C15 C7 111.2(3) . . ? C16 C15 C7 112.7(3) . . ? C19 C18 C23 120.1(4) . . ? C19 C18 N2 121.4(3) . . ? C23 C18 N2 118.5(4) . . ? C20 C19 C18 119.1(4) . . ? C20 C19 C27 118.8(4) . . ? C18 C19 C27 122.1(3) . . ? C21 C20 C19 121.0(4) . . ? C22 C21 C20 119.2(4) . . ? C21 C22 C23 122.0(4) . . ? C22 C23 C18 118.3(4) . . ? C22 C23 C24 121.0(4) . . ? C18 C23 C24 120.7(4) . . ? C25 C24 C23 110.1(4) . . ? C25 C24 C26 112.4(4) . . ? C23 C24 C26 113.6(4) . . ? C29 C27 C28 108.8(4) . . ? C29 C27 C19 114.1(3) . . ? C28 C27 C19 111.6(3) . . ? N3 Li2 N4 101.8(3) . . ? N3 Li2 C51 114.3(2) . 2_565 ? N4 Li2 C51 143.6(3) . 2_565 ? C30 N3 C35 119.5(3) . . ? C30 N3 Li2 120.1(3) . . ? C35 N3 Li2 120.5(2) . . ? C32 N4 C47 119.5(3) . . ? C32 N4 Li2 118.3(3) . . ? C47 N4 Li2 121.0(3) . . ? N3 C30 C31 124.0(3) . . ? N3 C30 C33 120.1(3) . . ? C31 C30 C33 115.9(3) . . ? C32 C31 C30 130.1(3) . . ? N4 C32 C31 124.4(3) . . ? N4 C32 C34A 123.1(4) . . ? C31 C32 C34A 111.4(4) . . ? N4 C32 C34B 114.0(4) . . ? C31 C32 C34B 119.7(4) . . ? C34A C32 C34B 26.9(3) . . ? C40 C35 C36 120.3(3) . . ? C40 C35 N3 120.1(3) . . ? C36 C35 N3 119.5(3) . . ? C37 C36 C35 118.0(3) . . ? C37 C36 C44 120.6(3) . . ? C35 C36 C44 121.3(3) . . ? C38 C37 C36 121.8(3) . . ? C37 C38 C39 119.6(3) . . ? C38 C39 C40 121.0(3) . . ? C39 C40 C35 119.1(3) . . ? C39 C40 C41 119.6(3) . . ? C35 C40 C41 121.3(3) . . ? C43 C41 C42 110.3(3) . . ? C43 C41 C40 113.2(3) . . ? C42 C41 C40 112.0(3) . . ? C36 C44 C45 113.5(3) . . ? C36 C44 C46 110.5(3) . . ? C45 C44 C46 109.4(3) . . ? C52 C47 C48 120.3(3) . . ? C52 C47 N4 119.4(3) . . ? C48 C47 N4 120.1(4) . . ? C49 C48 C47 118.6(4) . . ? C49 C48 C56 120.1(4) . . ? C47 C48 C56 121.3(3) . . ? C50 C49 C48 121.4(4) . . ? C51 C50 C49 119.6(4) . . ? C50 C51 C52 121.4(4) . . ? C50 C51 Li2 92.4(3) . 2_565 ? C52 C51 Li2 102.4(3) . 2_565 ? C51 C52 C47 118.6(4) . . ? C51 C52 C53 120.9(4) . . ? C47 C52 C53 120.3(3) . . ? C54A C53 C52 105.9(4) . . ? C54A C53 C55 124.9(5) . . ? C52 C53 C55 111.4(3) . . ? C54A C53 C54B 29.8(4) . . ? C52 C53 C54B 112.3(4) . . ? C55 C53 C54B 97.1(4) . . ? C58A C56 C57A 116.4(6) . . ? C58A C56 C48 107.0(4) . . ? C57A C56 C48 104.5(4) . . ? C58A C56 C57B 128.3(6) . . ? C57A C56 C57B 43.3(4) . . ? C48 C56 C57B 123.2(4) . . ? C58A C56 C58B 42.7(4) . . ? C57A C56 C58B 73.9(5) . . ? C48 C56 C58B 115.9(4) . . ? C57B C56 C58B 99.2(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.387 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.063 data_be49 _database_code_CSD 162356 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'NacNacH' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H42 N2' _chemical_formula_weight 418.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.053(5) _cell_length_b 17.944(6) _cell_length_c 20.034(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.40(2) _cell_angle_gamma 90.00 _cell_volume 5366(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 4.91 _cell_measurement_theta_max 27.89 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.036 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 0.444 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8932 _exptl_absorpt_correction_T_max 0.9653 _exptl_absorpt_process_details ; XABS2: an empirical absorption correction program. Parkin, S.; Moezzi, B.; Hope, H. J. Appl. Cryst. 1995, 28, 53-56. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Siemens Cu rotating anode' _diffrn_radiation_monochromator 'nickel filter' _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method 2\q-\w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% '<0.01' _diffrn_reflns_number 7786 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 56.44 _reflns_number_total 7091 _reflns_number_gt 5195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens XDISK' _computing_structure_solution 'XS, Bruker SHELXTL v. 5.10' _computing_structure_refinement 'XL, Bruker SHELXTL v. 5.10' _computing_molecular_graphics 'XP, Bruker SHELXTL v. 5.10' _computing_publication_material 'XCIF, Bruker SHELXTL v. 5.10' _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^)+(0.0653P)^2^+4.6853P] 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 7091 _refine_ls_number_parameters 587 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1659 _refine_ls_wR_factor_gt 0.1489 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.49703(15) 0.78985(12) 0.01102(11) 0.0235(5) Uani 1 1 d . . . C1 C 0.54909(18) 0.80252(15) -0.03584(13) 0.0241(6) Uani 1 1 d . . . N2 N 0.64817(16) 0.78325(13) 0.09804(11) 0.0249(6) Uani 1 1 d . . . C2 C 0.64341(18) 0.80602(16) -0.01911(13) 0.0265(7) Uani 1 1 d . . . H2B H 0.6768 0.8160 -0.0541 0.032 Uiso 1 1 calc R . . N3 N 0.75058(17) 0.74303(15) 0.76262(12) 0.0355(7) Uani 1 1 d . . . C3 C 0.69073(18) 0.79601(15) 0.04435(14) 0.0242(6) Uani 1 1 d . . . N4 N 0.90038(15) 0.76186(14) 0.84704(11) 0.0297(6) Uani 1 1 d . . . C4 C 0.5116(2) 0.81524(18) -0.10807(14) 0.0359(8) Uani 1 1 d . . . H4B H 0.4638 0.7806 -0.1208 0.054 Uiso 1 1 calc R . . H4C H 0.5579 0.8080 -0.1362 0.054 Uiso 1 1 calc R . . H4D H 0.4891 0.8652 -0.1134 0.054 Uiso 1 1 calc R . . C5 C 0.79051(19) 0.80042(19) 0.05380(15) 0.0383(8) Uani 1 1 d . . . H5A H 0.8149 0.7558 0.0753 0.058 Uiso 1 1 calc R . . H5B H 0.8094 0.8427 0.0814 0.058 Uiso 1 1 calc R . . H5C H 0.8115 0.8056 0.0108 0.058 Uiso 1 1 calc R . . C6 C 0.40173(18) 0.78634(15) -0.00516(13) 0.0227(6) Uani 1 1 d . . . C7 C 0.35969(19) 0.71627(16) -0.01248(14) 0.0301(7) Uani 1 1 d . . . C8 C 0.2670(2) 0.71405(18) -0.02739(15) 0.0362(8) Uani 1 1 d . . . H8A H 0.2385 0.6681 -0.0337 0.043 Uiso 1 1 calc R . . C9 C 0.2161(2) 0.77812(18) -0.03302(13) 0.0319(7) Uani 1 1 d . . . H9A H 0.1541 0.7754 -0.0429 0.038 Uiso 1 1 calc R . . C10 C 0.25812(19) 0.84622(17) -0.02380(14) 0.0319(7) Uani 1 1 d . . . H10A H 0.2236 0.8894 -0.0271 0.038 Uiso 1 1 calc R . . C11 C 0.35083(18) 0.85214(16) -0.00964(13) 0.0263(7) Uani 1 1 d . . . C12 C 0.3953(2) 0.92759(16) 0.00378(16) 0.0369(8) Uani 1 1 d . . . H12A H 0.4570 0.9231 -0.0066 0.044 Uiso 1 1 calc R . . C13 C 0.3510(3) 0.9895(2) -0.0397(3) 0.0831(15) Uani 1 1 d . . . H13A H 0.3482 0.9758 -0.0863 0.125 Uiso 1 1 calc R . . H13B H 0.3851 1.0345 -0.0316 0.125 Uiso 1 1 calc R . . H13C H 0.2914 0.9973 -0.0288 0.125 Uiso 1 1 calc R . . C14 C 0.4005(3) 0.9471(2) 0.0780(2) 0.0833(15) Uani 1 1 d . . . H14A H 0.4341 0.9095 0.1043 0.125 Uiso 1 1 calc R . . H14B H 0.3410 0.9496 0.0904 0.125 Uiso 1 1 calc R . . H14C H 0.4294 0.9945 0.0861 0.125 Uiso 1 1 calc R . . C15 C 0.4142(2) 0.64470(17) -0.00520(18) 0.0455(9) Uani 1 1 d . . . H15A H 0.4746 0.6577 0.0159 0.055 Uiso 1 1 calc R . . C16 C 0.3758(3) 0.5877(2) 0.0408(2) 0.0719(13) Uani 1 1 d . . . H16A H 0.3711 0.6102 0.0837 0.108 Uiso 1 1 calc R . . H16B H 0.4149 0.5452 0.0470 0.108 Uiso 1 1 calc R . . H16C H 0.3176 0.5720 0.0205 0.108 Uiso 1 1 calc R . . C17 C 0.4232(3) 0.6106(2) -0.0733(2) 0.0758(13) Uani 1 1 d . . . H17A H 0.4476 0.6469 -0.1011 0.114 Uiso 1 1 calc R . . H17B H 0.3654 0.5951 -0.0945 0.114 Uiso 1 1 calc R . . H17C H 0.4625 0.5683 -0.0675 0.114 Uiso 1 1 calc R . . C18 C 0.69303(18) 0.76500(16) 0.16324(14) 0.0267(7) Uani 1 1 d . . . C19 C 0.71453(19) 0.82165(18) 0.21077(14) 0.0330(7) Uani 1 1 d . . . C20 C 0.7526(2) 0.8003(2) 0.27559(15) 0.0425(9) Uani 1 1 d . . . H20A H 0.7666 0.8368 0.3082 0.051 Uiso 1 1 calc R . . C21 C 0.7696(2) 0.7269(2) 0.29207(17) 0.0462(9) Uani 1 1 d . . . H21A H 0.7942 0.7140 0.3355 0.055 Uiso 1 1 calc R . . C22 C 0.7505(2) 0.6733(2) 0.24457(17) 0.0486(9) Uani 1 1 d . . . H22A H 0.7635 0.6239 0.2559 0.058 Uiso 1 1 calc R . . C23 C 0.7121(2) 0.69022(18) 0.17948(16) 0.0400(8) Uani 1 1 d . . . C24 C 0.6874(3) 0.62896(19) 0.1286(2) 0.0608(11) Uani 1 1 d . . . H24A H 0.6776 0.6523 0.0840 0.073 Uiso 1 1 calc R . . C25 C 0.5998(3) 0.5935(3) 0.1411(3) 0.1014(19) Uani 1 1 d . . . H25A H 0.5541 0.6310 0.1390 0.152 Uiso 1 1 calc R . . H25B H 0.6069 0.5707 0.1848 0.152 Uiso 1 1 calc R . . H25C H 0.5830 0.5563 0.1074 0.152 Uiso 1 1 calc R . . C26 C 0.7617(3) 0.5703(2) 0.1271(2) 0.0722(12) Uani 1 1 d . . . H26A H 0.7441 0.5351 0.0919 0.108 Uiso 1 1 calc R . . H26B H 0.7712 0.5449 0.1696 0.108 Uiso 1 1 calc R . . H26C H 0.8161 0.5945 0.1189 0.108 Uiso 1 1 calc R . . C27 C 0.6968(2) 0.90237(18) 0.19357(17) 0.0433(8) Uani 1 1 d . . . H27A H 0.6760 0.9051 0.1452 0.052 Uiso 1 1 calc R . . C28 C 0.6223(3) 0.9335(2) 0.2304(2) 0.0628(11) Uani 1 1 d . . . H28A H 0.5694 0.9037 0.2201 0.094 Uiso 1 1 calc R . . H28B H 0.6096 0.9839 0.2164 0.094 Uiso 1 1 calc R . . H28C H 0.6411 0.9324 0.2781 0.094 Uiso 1 1 calc R . . C29 C 0.7822(3) 0.9490(2) 0.2069(2) 0.0617(11) Uani 1 1 d . . . H29A H 0.7700 0.9990 0.1912 0.093 Uiso 1 1 calc R . . H29B H 0.8277 0.9275 0.1835 0.093 Uiso 1 1 calc R . . H29C H 0.8024 0.9498 0.2543 0.093 Uiso 1 1 calc R . . C30 C 0.8058(2) 0.73608(19) 0.71445(14) 0.0361(8) Uani 1 1 d . . . C31 C 0.8962(2) 0.74421(19) 0.72913(15) 0.0406(8) Uani 1 1 d . . . H31A H 0.9299 0.7398 0.6936 0.049 Uiso 1 1 calc R . . C32 C 0.9440(2) 0.75900(18) 0.79440(15) 0.0359(8) Uani 1 1 d . . . C33 C 0.7629(2) 0.7187(2) 0.64414(15) 0.0526(10) Uani 1 1 d . . . H33A H 0.7225 0.7581 0.6283 0.079 Uiso 1 1 calc R . . H33B H 0.7303 0.6727 0.6443 0.079 Uiso 1 1 calc R . . H33C H 0.8084 0.7141 0.6150 0.079 Uiso 1 1 calc R . . C34 C 1.0429(2) 0.7718(2) 0.79886(16) 0.0523(10) Uani 1 1 d . . . H34A H 1.0707 0.7603 0.8435 0.078 Uiso 1 1 calc R . . H34B H 1.0540 0.8231 0.7889 0.078 Uiso 1 1 calc R . . H34C H 1.0674 0.7403 0.7670 0.078 Uiso 1 1 calc R . . C35 C 0.6555(2) 0.74321(19) 0.74939(14) 0.0343(8) Uani 1 1 d . . . C36 C 0.6113(2) 0.8079(2) 0.72325(14) 0.0392(8) Uani 1 1 d . . . C37 C 0.5181(2) 0.8048(2) 0.70871(15) 0.0463(9) Uani 1 1 d . . . H37A H 0.4870 0.8466 0.6910 0.056 Uiso 1 1 calc R . . C38 C 0.4714(2) 0.7407(2) 0.72010(15) 0.0490(10) Uani 1 1 d . . . H38A H 0.4096 0.7393 0.7088 0.059 Uiso 1 1 calc R . . C39 C 0.5160(2) 0.6791(2) 0.74818(15) 0.0466(9) Uani 1 1 d . . . H39A H 0.4834 0.6370 0.7570 0.056 Uiso 1 1 calc R . . C40 C 0.6087(2) 0.6782(2) 0.76368(14) 0.0379(8) Uani 1 1 d . . . C41 C 0.6586(2) 0.6123(2) 0.79784(17) 0.0468(9) Uani 1 1 d . . . H41A H 0.7159 0.6084 0.7798 0.056 Uiso 1 1 calc R . . C42 C 0.6112(3) 0.5375(2) 0.7863(2) 0.0734(13) Uani 1 1 d . . . H42A H 0.5973 0.5287 0.7388 0.110 Uiso 1 1 calc R . . H42B H 0.5568 0.5381 0.8066 0.110 Uiso 1 1 calc R . . H42C H 0.6496 0.4985 0.8061 0.110 Uiso 1 1 calc R . . C43 C 0.6797(3) 0.6267(2) 0.87379(17) 0.0573(10) Uani 1 1 d . . . H43A H 0.7120 0.5850 0.8949 0.086 Uiso 1 1 calc R . . H43B H 0.6248 0.6331 0.8927 0.086 Uiso 1 1 calc R . . H43C H 0.7155 0.6709 0.8812 0.086 Uiso 1 1 calc R . . C44 C 0.6619(2) 0.8799(2) 0.71433(16) 0.0467(9) Uani 1 1 d . . . H44A H 0.7255 0.8672 0.7167 0.056 Uiso 1 1 calc R . . C45 C 0.6525(4) 0.9331(3) 0.7719(2) 0.0907(16) Uani 1 1 d . . . H45A H 0.6836 0.9786 0.7652 0.136 Uiso 1 1 calc R . . H45B H 0.6776 0.9107 0.8136 0.136 Uiso 1 1 calc R . . H45C H 0.5902 0.9436 0.7734 0.136 Uiso 1 1 calc R . . C46 C 0.6355(3) 0.9195(3) 0.6483(2) 0.0904(16) Uani 1 1 d . . . H46A H 0.6397 0.8855 0.6118 0.136 Uiso 1 1 calc R . . H46B H 0.6750 0.9609 0.6448 0.136 Uiso 1 1 calc R . . H46C H 0.5751 0.9372 0.6463 0.136 Uiso 1 1 calc R . . C47 C 0.94533(18) 0.77644(16) 0.91259(14) 0.0278(7) Uani 1 1 d . . . C48 C 0.96311(19) 0.71642(16) 0.95770(14) 0.0291(7) Uani 1 1 d . . . C49 C 0.99988(19) 0.73122(18) 1.02340(14) 0.0342(8) Uani 1 1 d . . . H49A H 1.0119 0.6918 1.0534 0.041 Uiso 1 1 calc R . . C50 C 1.01906(19) 0.80296(17) 1.04539(15) 0.0334(7) Uani 1 1 d . . . H50A H 1.0434 0.8119 1.0897 0.040 Uiso 1 1 calc R . . C51 C 1.00164(19) 0.86114(18) 1.00079(15) 0.0336(7) Uani 1 1 d . . . H51A H 1.0147 0.9095 1.0156 0.040 Uiso 1 1 calc R . . C52 C 0.96500(18) 0.84946(17) 0.93408(14) 0.0301(7) Uani 1 1 d . . . C53 C 0.9445(2) 0.91654(17) 0.88748(16) 0.0380(8) Uani 1 1 d . . . H53A H 0.9249 0.8974 0.8422 0.046 Uiso 1 1 calc R . . C54 C 0.8672(2) 0.9620(2) 0.90927(19) 0.0512(9) Uani 1 1 d . . . H54A H 0.8139 0.9320 0.9051 0.077 Uiso 1 1 calc R . . H54B H 0.8570 1.0052 0.8811 0.077 Uiso 1 1 calc R . . H54C H 0.8821 0.9772 0.9553 0.077 Uiso 1 1 calc R . . C55 C 1.0282(2) 0.9642(2) 0.88378(18) 0.0531(10) Uani 1 1 d . . . H55A H 1.0138 1.0044 0.8526 0.080 Uiso 1 1 calc R . . H55B H 1.0744 0.9339 0.8688 0.080 Uiso 1 1 calc R . . H55C H 1.0487 0.9841 0.9275 0.080 Uiso 1 1 calc R . . C56 C 0.9449(2) 0.63674(18) 0.93408(16) 0.0409(8) Uani 1 1 d . . . H56A H 0.9031 0.6386 0.8924 0.049 Uiso 1 1 calc R . . C57 C 1.0324(3) 0.5997(2) 0.9176(2) 0.0737(13) Uani 1 1 d . . . H57A H 1.0570 0.6286 0.8840 0.111 Uiso 1 1 calc R . . H57B H 1.0196 0.5502 0.9009 0.111 Uiso 1 1 calc R . . H57C H 1.0749 0.5974 0.9576 0.111 Uiso 1 1 calc R . . C58 C 0.9016(3) 0.5903(2) 0.98451(18) 0.0622(11) Uani 1 1 d . . . H58A H 0.8474 0.6141 0.9938 0.093 Uiso 1 1 calc R . . H58B H 0.9421 0.5859 1.0254 0.093 Uiso 1 1 calc R . . H58C H 0.8879 0.5416 0.9661 0.093 Uiso 1 1 calc R . . H2 H 0.584(3) 0.780(2) 0.085(2) 0.086(14) Uiso 1 1 d . . . H3 H 0.782(3) 0.749(2) 0.8048(19) 0.072(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0265(13) 0.0155(13) 0.0290(13) -0.0003(10) 0.0051(10) -0.0015(10) C1 0.0297(16) 0.0137(15) 0.0294(15) -0.0031(12) 0.0056(12) 0.0026(12) N2 0.0258(13) 0.0224(14) 0.0268(13) 0.0011(10) 0.0047(11) -0.0008(11) C2 0.0304(16) 0.0252(17) 0.0255(15) 0.0009(12) 0.0100(12) 0.0005(13) N3 0.0293(14) 0.0509(19) 0.0263(14) -0.0059(12) 0.0037(12) -0.0003(12) C3 0.0260(15) 0.0129(15) 0.0343(16) -0.0014(12) 0.0059(13) 0.0001(12) N4 0.0291(13) 0.0355(16) 0.0246(13) -0.0023(11) 0.0042(11) 0.0022(11) C4 0.0349(17) 0.043(2) 0.0302(16) 0.0008(15) 0.0037(13) 0.0004(15) C5 0.0328(18) 0.049(2) 0.0334(17) 0.0021(15) 0.0066(14) 0.0023(15) C6 0.0260(15) 0.0194(16) 0.0223(14) 0.0010(12) 0.0015(11) 0.0005(12) C7 0.0335(17) 0.0195(17) 0.0367(17) -0.0001(13) 0.0018(13) -0.0026(13) C8 0.0350(18) 0.0295(19) 0.0431(18) -0.0013(15) 0.0012(14) -0.0094(15) C9 0.0263(16) 0.043(2) 0.0264(15) -0.0024(14) 0.0019(12) -0.0038(15) C10 0.0320(17) 0.0318(19) 0.0319(16) 0.0038(14) 0.0043(13) 0.0083(14) C11 0.0299(17) 0.0220(17) 0.0274(15) 0.0008(12) 0.0049(12) 0.0029(13) C12 0.0390(18) 0.0181(17) 0.054(2) -0.0025(15) 0.0090(15) 0.0007(14) C13 0.076(3) 0.030(2) 0.136(4) 0.023(2) -0.012(3) -0.002(2) C14 0.114(4) 0.062(3) 0.079(3) -0.039(2) 0.031(3) -0.043(3) C15 0.042(2) 0.0161(17) 0.076(2) 0.0022(17) -0.0040(17) -0.0042(14) C16 0.079(3) 0.039(2) 0.095(3) 0.026(2) 0.002(2) 0.000(2) C17 0.096(3) 0.038(2) 0.097(3) -0.006(2) 0.029(3) 0.016(2) C18 0.0253(15) 0.0257(17) 0.0289(16) 0.0042(13) 0.0032(12) -0.0041(13) C19 0.0310(17) 0.036(2) 0.0325(17) -0.0026(14) 0.0072(13) -0.0062(14) C20 0.0329(18) 0.063(3) 0.0320(18) -0.0084(17) 0.0046(14) -0.0093(17) C21 0.0340(19) 0.068(3) 0.0360(19) 0.0197(19) 0.0018(15) -0.0007(18) C22 0.049(2) 0.049(2) 0.046(2) 0.0199(19) -0.0027(17) 0.0022(18) C23 0.046(2) 0.031(2) 0.0412(19) 0.0088(15) -0.0004(15) -0.0015(15) C24 0.089(3) 0.023(2) 0.064(2) 0.0094(17) -0.017(2) 0.002(2) C25 0.073(3) 0.046(3) 0.174(6) -0.030(3) -0.025(3) 0.000(2) C26 0.100(3) 0.045(3) 0.074(3) 0.010(2) 0.021(2) 0.011(2) C27 0.053(2) 0.032(2) 0.0443(19) -0.0107(16) 0.0062(16) -0.0078(16) C28 0.062(3) 0.045(2) 0.083(3) -0.014(2) 0.014(2) 0.002(2) C29 0.072(3) 0.039(2) 0.078(3) -0.017(2) 0.022(2) -0.015(2) C30 0.0337(18) 0.047(2) 0.0279(16) -0.0044(15) 0.0053(13) -0.0003(15) C31 0.0321(18) 0.062(2) 0.0284(16) -0.0078(16) 0.0086(14) 0.0028(16) C32 0.0313(17) 0.044(2) 0.0331(17) -0.0034(15) 0.0081(14) 0.0030(15) C33 0.041(2) 0.089(3) 0.0275(17) -0.0147(18) 0.0036(15) 0.0008(19) C34 0.0334(19) 0.085(3) 0.0392(19) -0.0146(19) 0.0087(15) -0.0018(19) C35 0.0291(17) 0.051(2) 0.0223(15) -0.0078(14) 0.0023(12) 0.0032(16) C36 0.0386(19) 0.057(2) 0.0218(15) -0.0059(15) 0.0053(13) -0.0025(17) C37 0.038(2) 0.072(3) 0.0292(17) -0.0028(17) 0.0024(14) 0.0103(19) C38 0.0291(18) 0.088(3) 0.0299(17) -0.0121(19) 0.0052(14) -0.007(2) C39 0.040(2) 0.066(3) 0.0339(18) -0.0077(18) 0.0059(15) -0.0066(19) C40 0.0328(18) 0.053(2) 0.0279(16) -0.0117(15) 0.0045(13) -0.0047(16) C41 0.048(2) 0.046(2) 0.047(2) -0.0064(17) 0.0076(16) -0.0043(17) C42 0.090(3) 0.057(3) 0.073(3) -0.009(2) 0.006(2) -0.013(2) C43 0.068(3) 0.054(3) 0.049(2) 0.0053(19) 0.0010(18) -0.002(2) C44 0.046(2) 0.055(2) 0.0385(19) 0.0038(17) 0.0036(16) 0.0044(18) C45 0.127(4) 0.069(3) 0.082(3) -0.025(3) 0.037(3) -0.038(3) C46 0.103(4) 0.087(4) 0.072(3) 0.030(3) -0.022(3) -0.025(3) C47 0.0243(15) 0.0307(18) 0.0287(16) -0.0026(14) 0.0050(12) 0.0005(13) C48 0.0286(16) 0.0267(18) 0.0324(16) -0.0019(14) 0.0050(13) -0.0006(13) C49 0.0330(17) 0.038(2) 0.0324(17) 0.0059(15) 0.0061(13) 0.0067(15) C50 0.0324(17) 0.038(2) 0.0300(16) -0.0053(15) 0.0046(13) -0.0005(15) C51 0.0310(16) 0.0306(18) 0.0398(18) -0.0108(15) 0.0066(13) -0.0015(14) C52 0.0269(16) 0.0288(18) 0.0354(17) -0.0017(14) 0.0074(13) 0.0011(13) C53 0.0430(19) 0.0300(19) 0.0403(18) 0.0024(15) 0.0027(15) -0.0005(15) C54 0.049(2) 0.036(2) 0.066(2) 0.0061(18) 0.0014(18) 0.0058(17) C55 0.059(2) 0.044(2) 0.057(2) 0.0102(18) 0.0126(18) -0.0047(19) C56 0.050(2) 0.0304(19) 0.0414(19) 0.0000(15) 0.0040(15) -0.0036(16) C57 0.076(3) 0.038(2) 0.111(4) -0.022(2) 0.025(3) 0.004(2) C58 0.085(3) 0.044(2) 0.055(2) 0.0061(19) 0.001(2) -0.015(2) _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 N1 C1 1.318(3) . ? N1 C6 1.431(3) . ? C1 C2 1.418(4) . ? C1 C4 1.501(4) . ? N2 C3 1.341(3) . ? N2 C18 1.429(4) . ? C2 C3 1.386(4) . ? N3 C30 1.358(4) . ? N3 C35 1.421(4) . ? C3 C5 1.492(4) . ? N4 C32 1.313(4) . ? N4 C47 1.422(3) . ? C6 C7 1.407(4) . ? C6 C11 1.404(4) . ? C7 C8 1.390(4) . ? C7 C15 1.521(4) . ? C8 C9 1.378(4) . ? C9 C10 1.378(4) . ? C10 C11 1.392(4) . ? C11 C12 1.519(4) . ? C12 C13 1.513(5) . ? C12 C14 1.519(5) . ? C15 C17 1.518(5) . ? C15 C16 1.539(5) . ? C18 C23 1.402(4) . ? C18 C19 1.402(4) . ? C19 C20 1.403(4) . ? C19 C27 1.505(4) . ? C20 C21 1.374(5) . ? C21 C22 1.358(5) . ? C22 C23 1.391(4) . ? C23 C24 1.512(5) . ? C24 C25 1.513(6) . ? C24 C26 1.538(5) . ? C27 C28 1.525(5) . ? C27 C29 1.528(5) . ? C30 C31 1.362(4) . ? C30 C33 1.505(4) . ? C31 C32 1.434(4) . ? C32 C34 1.498(4) . ? C35 C36 1.406(5) . ? C35 C40 1.411(5) . ? C36 C37 1.396(4) . ? C36 C44 1.522(5) . ? C37 C38 1.382(5) . ? C38 C39 1.376(5) . ? C39 C40 1.389(4) . ? C40 C41 1.517(5) . ? C41 C42 1.524(5) . ? C41 C43 1.536(5) . ? C44 C46 1.508(5) . ? C44 C45 1.518(5) . ? C47 C52 1.399(4) . ? C47 C48 1.409(4) . ? C48 C49 1.386(4) . ? C48 C56 1.520(4) . ? C49 C50 1.379(4) . ? C50 C51 1.377(4) . ? C51 C52 1.395(4) . ? C52 C53 1.530(4) . ? C53 C54 1.530(4) . ? C53 C55 1.532(4) . ? C56 C58 1.520(5) . ? C56 C57 1.549(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C6 121.1(2) . . ? N1 C1 C2 120.6(2) . . ? N1 C1 C4 121.9(2) . . ? C2 C1 C4 117.5(2) . . ? C3 N2 C18 123.7(2) . . ? C3 C2 C1 126.3(3) . . ? C30 N3 C35 124.1(3) . . ? N2 C3 C2 121.0(3) . . ? N2 C3 C5 119.0(2) . . ? C2 C3 C5 120.0(3) . . ? C32 N4 C47 121.4(2) . . ? C7 C6 C11 120.7(3) . . ? C7 C6 N1 119.2(2) . . ? C11 C6 N1 120.0(2) . . ? C8 C7 C6 118.3(3) . . ? C8 C7 C15 120.7(3) . . ? C6 C7 C15 121.0(3) . . ? C9 C8 C7 121.7(3) . . ? C8 C9 C10 119.2(3) . . ? C9 C10 C11 121.8(3) . . ? C10 C11 C6 118.3(3) . . ? C10 C11 C12 120.8(3) . . ? C6 C11 C12 120.9(2) . . ? C13 C12 C11 113.6(3) . . ? C13 C12 C14 111.0(3) . . ? C11 C12 C14 110.1(3) . . ? C7 C15 C17 111.3(3) . . ? C7 C15 C16 112.3(3) . . ? C17 C15 C16 110.8(3) . . ? C23 C18 C19 120.9(3) . . ? C23 C18 N2 119.3(3) . . ? C19 C18 N2 119.7(3) . . ? C20 C19 C18 117.5(3) . . ? C20 C19 C27 120.9(3) . . ? C18 C19 C27 121.6(3) . . ? C21 C20 C19 121.7(3) . . ? C22 C21 C20 119.7(3) . . ? C21 C22 C23 121.8(3) . . ? C22 C23 C18 118.3(3) . . ? C22 C23 C24 120.6(3) . . ? C18 C23 C24 121.0(3) . . ? C25 C24 C23 109.7(4) . . ? C25 C24 C26 111.5(3) . . ? C23 C24 C26 113.2(3) . . ? C19 C27 C28 111.2(3) . . ? C19 C27 C29 111.5(3) . . ? C28 C27 C29 111.7(3) . . ? N3 C30 C31 121.5(3) . . ? N3 C30 C33 117.1(3) . . ? C31 C30 C33 121.4(3) . . ? C30 C31 C32 125.9(3) . . ? N4 C32 C31 119.7(3) . . ? N4 C32 C34 122.8(3) . . ? C31 C32 C34 117.5(3) . . ? C36 C35 C40 122.2(3) . . ? C36 C35 N3 119.3(3) . . ? C40 C35 N3 118.6(3) . . ? C37 C36 C35 117.4(3) . . ? C37 C36 C44 120.9(3) . . ? C35 C36 C44 121.7(3) . . ? C38 C37 C36 121.2(3) . . ? C39 C38 C37 120.3(3) . . ? C38 C39 C40 121.5(4) . . ? C39 C40 C35 117.4(3) . . ? C39 C40 C41 122.3(3) . . ? C35 C40 C41 120.3(3) . . ? C40 C41 C42 115.0(3) . . ? C40 C41 C43 110.0(3) . . ? C42 C41 C43 109.4(3) . . ? C46 C44 C45 109.3(4) . . ? C46 C44 C36 115.1(3) . . ? C45 C44 C36 110.3(3) . . ? C52 C47 C48 120.2(3) . . ? C52 C47 N4 120.9(3) . . ? C48 C47 N4 118.7(3) . . ? C49 C48 C47 118.8(3) . . ? C49 C48 C56 120.6(3) . . ? C47 C48 C56 120.5(3) . . ? C50 C49 C48 121.6(3) . . ? C51 C50 C49 119.1(3) . . ? C50 C51 C52 121.8(3) . . ? C51 C52 C47 118.5(3) . . ? C51 C52 C53 119.4(3) . . ? C47 C52 C53 122.1(3) . . ? C52 C53 C54 110.2(3) . . ? C52 C53 C55 111.5(3) . . ? C54 C53 C55 112.1(3) . . ? C58 C56 C48 112.6(3) . . ? C58 C56 C57 110.9(3) . . ? C48 C56 C57 110.3(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 56.44 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.215 _refine_diff_density_min -0.200 _refine_diff_density_rms 0.039 data_mas03n _database_code_CSD 162357 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[NacNacLi]12*hexane' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C354 H492 Li12 N24' _chemical_formula_weight 5166.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 32.8393(11) _cell_length_b 16.7836(6) _cell_length_c 33.3750(11) _cell_angle_alpha 90.00 _cell_angle_beta 112.2750(10) _cell_angle_gamma 90.00 _cell_volume 17022.3(10) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 5959 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 31.34 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.008 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5636 _exptl_absorpt_coefficient_mu 0.057 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9725 _exptl_absorpt_correction_T_max 0.9864 _exptl_absorpt_process_details ; SADABS: an empirical absorption program by G. M. Sheldrick using the method described by Blessing, R. H.; Acta Cryst. A51, 1995, 33. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 frames remeasured' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% '<0.01' _diffrn_reflns_number 31158 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1053 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.35 _reflns_number_total 31158 _reflns_number_gt 15015 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL v. 5.10' _computing_structure_solution 'XS, Bruker SHELXTL v. 5.10' _computing_structure_refinement 'XL, Bruker SHELXTL v. 5.10' _computing_molecular_graphics 'XP, Bruker SHELXTL v. 5.10' _computing_publication_material 'XCIF, Bruker SHELXTL v. 5.10' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1780P)^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 SHELXL _refine_ls_extinction_coef 0.00166(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 31158 _refine_ls_number_parameters 1775 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.1708 _refine_ls_R_factor_gt 0.0898 _refine_ls_wR_factor_ref 0.2932 _refine_ls_wR_factor_gt 0.2448 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.948 _refine_ls_shift/su_max 4.494 _refine_ls_shift/su_mean 0.091 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 0.6389(2) 0.2978(4) 0.5867(2) 0.0423(17) Uani 1 1 d . . . N1 N 0.65760(10) 0.40164(17) 0.57963(9) 0.0317(7) Uani 1 1 d . . . N2 N 0.67531(10) 0.23625(17) 0.56572(9) 0.0310(7) Uani 1 1 d . . . C1 C 0.69158(13) 0.4136(2) 0.56834(11) 0.0315(9) Uani 1 1 d . . . C2 C 0.71438(12) 0.3516(2) 0.55721(11) 0.0308(8) Uani 1 1 d . . . H2 H 0.7380 0.3683 0.5494 0.037 Uiso 1 1 calc R . . C3 C 0.70743(12) 0.2694(2) 0.55596(11) 0.0293(8) Uani 1 1 d . . . C4 C 0.70768(15) 0.4977(2) 0.56693(14) 0.0433(10) Uani 1 1 d . . . H4A H 0.6832 0.5305 0.5481 0.065 Uiso 1 1 calc R . . H4B H 0.7311 0.4968 0.5555 0.065 Uiso 1 1 calc R . . H4C H 0.7191 0.5201 0.5962 0.065 Uiso 1 1 calc R . . C5 C 0.73833(14) 0.2183(2) 0.54360(14) 0.0409(10) Uani 1 1 d . . . H5A H 0.7663 0.2131 0.5684 0.061 Uiso 1 1 calc R . . H5B H 0.7435 0.2429 0.5193 0.061 Uiso 1 1 calc R . . H5C H 0.7253 0.1654 0.5350 0.061 Uiso 1 1 calc R . . C6 C 0.63531(13) 0.4692(2) 0.58798(12) 0.0359(9) Uani 1 1 d D . . C7 C 0.60064(15) 0.5033(2) 0.55369(13) 0.0445(11) Uani 1 1 d D . . C8 C 0.57745(17) 0.5666(3) 0.56261(16) 0.0581(13) Uani 1 1 d D . . H8 H 0.5539 0.5909 0.5396 0.070 Uiso 1 1 calc R . . C9 C 0.58838(19) 0.5938(3) 0.60398(17) 0.0638(15) Uani 1 1 d D . . H9 H 0.5722 0.6365 0.6094 0.077 Uiso 1 1 calc R . . C10 C 0.62264(17) 0.5602(3) 0.63814(16) 0.0587(13) Uani 1 1 d D . . H10 H 0.6299 0.5797 0.6667 0.070 Uiso 1 1 calc R . . C11 C 0.64661(15) 0.4969(2) 0.63019(14) 0.0476(11) Uani 1 1 d D . . C12 C 0.68361(16) 0.4561(3) 0.66824(14) 0.0614(14) Uani 1 1 d D . . H12 H 0.7022 0.4252 0.6559 0.074 Uiso 1 1 calc R . . C13 C 0.7136(2) 0.5165(4) 0.70066(19) 0.104(2) Uani 1 1 d D . . H13A H 0.6970 0.5434 0.7157 0.156 Uiso 1 1 calc R . . H13B H 0.7240 0.5560 0.6851 0.156 Uiso 1 1 calc R . . H13C H 0.7388 0.4887 0.7218 0.156 Uiso 1 1 calc R . . C14 C 0.6645(2) 0.3980(3) 0.69067(17) 0.0787(18) Uani 1 1 d D . . H14A H 0.6884 0.3715 0.7141 0.118 Uiso 1 1 calc R . . H14B H 0.6470 0.3581 0.6698 0.118 Uiso 1 1 calc R . . H14C H 0.6457 0.4266 0.7027 0.118 Uiso 1 1 calc R . . C15 C 0.58850(15) 0.4738(3) 0.50741(13) 0.0468(11) Uani 1 1 d D . . H15 H 0.6146 0.4447 0.5062 0.056 Uiso 1 1 calc R . . C16 C 0.5776(2) 0.5401(3) 0.47441(16) 0.0737(16) Uani 1 1 d D . . H16A H 0.5750 0.5183 0.4463 0.111 Uiso 1 1 calc R . . H16B H 0.6010 0.5803 0.4838 0.111 Uiso 1 1 calc R . . H16C H 0.5496 0.5648 0.4717 0.111 Uiso 1 1 calc R . . C17 C 0.5508(2) 0.4159(3) 0.49488(17) 0.0817(18) Uani 1 1 d D . . H17A H 0.5263 0.4397 0.5006 0.123 Uiso 1 1 calc R . . H17B H 0.5603 0.3670 0.5119 0.123 Uiso 1 1 calc R . . H17C H 0.5412 0.4033 0.4640 0.123 Uiso 1 1 calc R . . C18 C 0.67104(12) 0.1526(2) 0.56679(12) 0.0304(9) Uani 1 1 d . . . C19 C 0.64125(13) 0.1126(2) 0.53004(12) 0.0335(9) Uani 1 1 d . . . C20 C 0.63330(14) 0.0316(2) 0.53400(14) 0.0411(10) Uani 1 1 d . . . H20 H 0.6141 0.0032 0.5095 0.049 Uiso 1 1 calc R . . C21 C 0.65309(15) -0.0077(2) 0.57308(14) 0.0418(10) Uani 1 1 d . . . H21 H 0.6465 -0.0621 0.5755 0.050 Uiso 1 1 calc R . . C22 C 0.68214(15) 0.0317(2) 0.60820(14) 0.0428(10) Uani 1 1 d . . . H22 H 0.6961 0.0037 0.6347 0.051 Uiso 1 1 calc R . . C23 C 0.69166(14) 0.1119(2) 0.60588(13) 0.0379(10) Uani 1 1 d . B . C24 C 0.72261(15) 0.1550(3) 0.64567(14) 0.0493(11) Uani 1 1 d . . . H24 H 0.7252 0.2038 0.6296 0.059 Uiso 1 1 calc R A 1 C25 C 0.69827(18) 0.1961(3) 0.67025(16) 0.0688(15) Uani 1 1 d . B . H25A H 0.6875 0.1561 0.6852 0.103 Uiso 1 1 calc R . . H25B H 0.6733 0.2259 0.6499 0.103 Uiso 1 1 calc R . . H25C H 0.7182 0.2328 0.6915 0.103 Uiso 1 1 calc R . . C26A C 0.7694(9) 0.1360(15) 0.6622(9) 0.206(12) Uiso 0.50 1 d P B 1 H26A H 0.7770 0.1134 0.6388 0.309 Uiso 0.50 1 calc PR B 1 H26B H 0.7762 0.0973 0.6858 0.309 Uiso 0.50 1 calc PR B 1 H26C H 0.7866 0.1847 0.6730 0.309 Uiso 0.50 1 calc PR B 1 C26B C 0.7612(3) 0.1072(5) 0.6740(3) 0.0338(19) Uiso 0.50 1 d P B 2 H26D H 0.7756 0.0824 0.6562 0.051 Uiso 0.50 1 calc PR B 2 H26E H 0.7512 0.0656 0.6887 0.051 Uiso 0.50 1 calc PR B 2 H26F H 0.7821 0.1421 0.6955 0.051 Uiso 0.50 1 calc PR B 2 C27 C 0.61741(15) 0.1549(2) 0.48735(13) 0.0429(10) Uani 1 1 d . . . H27 H 0.6223 0.2135 0.4927 0.051 Uiso 1 1 calc R . . C28 C 0.56799(15) 0.1404(3) 0.46901(15) 0.0572(13) Uani 1 1 d . . . H28A H 0.5621 0.0843 0.4606 0.086 Uiso 1 1 calc R . . H28B H 0.5540 0.1743 0.4436 0.086 Uiso 1 1 calc R . . H28C H 0.5560 0.1530 0.4910 0.086 Uiso 1 1 calc R . . C29 C 0.63587(16) 0.1315(3) 0.45329(14) 0.0582(13) Uani 1 1 d . . . H29A H 0.6670 0.1467 0.4634 0.087 Uiso 1 1 calc R . . H29B H 0.6194 0.1590 0.4260 0.087 Uiso 1 1 calc R . . H29C H 0.6331 0.0738 0.4486 0.087 Uiso 1 1 calc R . . Li2 Li 0.4756(2) 0.1491(4) 0.66762(19) 0.0363(15) Uani 1 1 d . . . N3 N 0.48100(9) 0.11607(18) 0.72397(9) 0.0286(7) Uani 1 1 d . . . N4 N 0.53395(9) 0.18746(17) 0.68096(9) 0.0269(7) Uani 1 1 d . . . C30 C 0.51346(12) 0.1410(2) 0.75883(11) 0.0289(8) Uani 1 1 d . . . C31 C 0.54999(12) 0.1840(2) 0.75759(11) 0.0283(8) Uani 1 1 d . . . H31 H 0.5702 0.2029 0.7847 0.034 Uiso 1 1 calc R . . C32 C 0.56023(12) 0.2024(2) 0.72162(11) 0.0264(8) Uani 1 1 d . . . C33 C 0.51390(13) 0.1237(3) 0.80334(12) 0.0384(10) Uani 1 1 d . . . H33A H 0.5071 0.1725 0.8156 0.058 Uiso 1 1 calc R . . H33B H 0.5431 0.1044 0.8221 0.058 Uiso 1 1 calc R . . H33C H 0.4918 0.0829 0.8012 0.058 Uiso 1 1 calc R . . C34 C 0.60455(12) 0.2420(2) 0.73120(12) 0.0318(9) Uani 1 1 d . . . H34A H 0.6198 0.2154 0.7147 0.048 Uiso 1 1 calc R . . H34B H 0.6224 0.2380 0.7622 0.048 Uiso 1 1 calc R . . H34C H 0.6001 0.2983 0.7228 0.048 Uiso 1 1 calc R . . C35 C 0.44638(12) 0.0685(2) 0.72691(11) 0.0313(9) Uani 1 1 d . . . C36 C 0.44661(12) -0.0149(2) 0.71849(11) 0.0341(9) Uani 1 1 d . . . C37 C 0.41022(14) -0.0599(3) 0.71639(13) 0.0431(10) Uani 1 1 d . . . H37 H 0.4099 -0.1155 0.7109 0.052 Uiso 1 1 calc R . . C38 C 0.37496(14) -0.0255(3) 0.72205(14) 0.0499(12) Uani 1 1 d . . . H38 H 0.3504 -0.0572 0.7202 0.060 Uiso 1 1 calc R . . C39 C 0.37499(13) 0.0552(3) 0.73046(13) 0.0472(11) Uani 1 1 d . . . H39 H 0.3505 0.0781 0.7347 0.057 Uiso 1 1 calc R . . C40 C 0.41077(12) 0.1039(2) 0.73288(12) 0.0356(9) Uani 1 1 d . . . C41 C 0.41018(13) 0.1928(3) 0.74109(13) 0.0426(10) Uani 1 1 d . . . H41 H 0.4409 0.2129 0.7491 0.051 Uiso 1 1 calc R . . C42 C 0.39583(19) 0.2124(3) 0.77900(18) 0.0720(16) Uani 1 1 d . . . H42A H 0.3979 0.2699 0.7842 0.108 Uiso 1 1 calc R . . H42B H 0.4151 0.1846 0.8051 0.108 Uiso 1 1 calc R . . H42C H 0.3654 0.1950 0.7717 0.108 Uiso 1 1 calc R . . C43 C 0.38099(16) 0.2372(3) 0.70000(16) 0.0652(14) Uani 1 1 d . . . H43A H 0.3920 0.2280 0.6769 0.098 Uiso 1 1 calc R . . H43B H 0.3816 0.2944 0.7061 0.098 Uiso 1 1 calc R . . H43C H 0.3507 0.2176 0.6908 0.098 Uiso 1 1 calc R . . C44 C 0.48594(14) -0.0541(2) 0.71301(13) 0.0409(10) Uani 1 1 d . . . H44 H 0.5010 -0.0121 0.7023 0.049 Uiso 1 1 calc R . . C45 C 0.51881(15) -0.0834(3) 0.75595(14) 0.0557(12) Uani 1 1 d . . . H45A H 0.5263 -0.0399 0.7771 0.084 Uiso 1 1 calc R . . H45B H 0.5455 -0.1018 0.7522 0.084 Uiso 1 1 calc R . . H45C H 0.5059 -0.1276 0.7664 0.084 Uiso 1 1 calc R . . C46 C 0.47348(17) -0.1217(3) 0.67971(16) 0.0574(13) Uani 1 1 d . . . H46A H 0.4624 -0.1671 0.6910 0.086 Uiso 1 1 calc R . . H46B H 0.4995 -0.1380 0.6741 0.086 Uiso 1 1 calc R . . H46C H 0.4506 -0.1032 0.6527 0.086 Uiso 1 1 calc R . . C47 C 0.54720(11) 0.2060(2) 0.64632(11) 0.0275(8) Uani 1 1 d . . . C48 C 0.56114(11) 0.1430(2) 0.62646(11) 0.0281(8) Uani 1 1 d . . . C49 C 0.57239(12) 0.1604(2) 0.59132(12) 0.0346(9) Uani 1 1 d . . . H49 H 0.5827 0.1190 0.5781 0.042 Uiso 1 1 calc R . . C50 C 0.56884(13) 0.2376(2) 0.57519(12) 0.0372(10) Uani 1 1 d . . . H50 H 0.5766 0.2486 0.5510 0.045 Uiso 1 1 calc R . . C51 C 0.55414(14) 0.2985(2) 0.59419(13) 0.0400(10) Uani 1 1 d . . . H51 H 0.5520 0.3510 0.5830 0.048 Uiso 1 1 calc R . . C52 C 0.54243(13) 0.2841(2) 0.62964(12) 0.0327(9) Uani 1 1 d . . . C53 C 0.52152(14) 0.3480(2) 0.64783(13) 0.0400(10) Uani 1 1 d . . . H53 H 0.5317 0.3391 0.6798 0.048 Uiso 1 1 calc R . . C54 C 0.47099(15) 0.3388(3) 0.62854(13) 0.0469(11) Uani 1 1 d . . . H54A H 0.4577 0.3795 0.6408 0.070 Uiso 1 1 calc R . . H54B H 0.4630 0.2858 0.6355 0.070 Uiso 1 1 calc R . . H54C H 0.4601 0.3453 0.5970 0.070 Uiso 1 1 calc R . . C55 C 0.5341(2) 0.4323(3) 0.64091(19) 0.0697(15) Uani 1 1 d . . . H55A H 0.5663 0.4374 0.6529 0.105 Uiso 1 1 calc R . . H55B H 0.5215 0.4699 0.6555 0.105 Uiso 1 1 calc R . . H55C H 0.5228 0.4441 0.6098 0.105 Uiso 1 1 calc R . . C56 C 0.56220(13) 0.0572(2) 0.64277(12) 0.0350(9) Uani 1 1 d . . . H56 H 0.5377 0.0520 0.6535 0.042 Uiso 1 1 calc R . . C57 C 0.55493(14) -0.0066(2) 0.60799(13) 0.0430(10) Uani 1 1 d . . . H57A H 0.5805 -0.0083 0.5996 0.065 Uiso 1 1 calc R . . H57B H 0.5285 0.0063 0.5826 0.065 Uiso 1 1 calc R . . H57C H 0.5512 -0.0586 0.6195 0.065 Uiso 1 1 calc R . . C58 C 0.60491(15) 0.0402(3) 0.68084(13) 0.0475(11) Uani 1 1 d . . . H58A H 0.6040 -0.0138 0.6916 0.071 Uiso 1 1 calc R . . H58B H 0.6086 0.0788 0.7040 0.071 Uiso 1 1 calc R . . H58C H 0.6297 0.0447 0.6715 0.071 Uiso 1 1 calc R . . Li3 Li 0.3072(2) 0.1031(4) 0.4493(2) 0.0433(17) Uani 1 1 d . . . N5 N 0.26629(10) 0.17369(18) 0.40911(10) 0.0318(7) Uani 1 1 d . . . N6 N 0.33483(10) 0.17114(17) 0.49797(9) 0.0295(7) Uani 1 1 d . . . C59 C 0.26111(12) 0.2467(2) 0.42133(12) 0.0338(9) Uani 1 1 d . . . C60 C 0.28729(13) 0.2800(2) 0.46203(12) 0.0347(9) Uani 1 1 d . . . H60 H 0.2812 0.3342 0.4658 0.042 Uiso 1 1 calc R . . C61 C 0.32062(13) 0.2457(2) 0.49739(12) 0.0326(9) Uani 1 1 d . . . C62 C 0.22462(15) 0.2991(3) 0.39238(16) 0.0593(13) Uani 1 1 d . . . H62A H 0.2289 0.3090 0.3653 0.089 Uiso 1 1 calc R . . H62B H 0.2249 0.3498 0.4070 0.089 Uiso 1 1 calc R . . H62C H 0.1963 0.2725 0.3860 0.089 Uiso 1 1 calc R . . C63 C 0.33939(14) 0.2975(2) 0.53765(13) 0.0384(10) Uani 1 1 d . . . H63A H 0.3263 0.2820 0.5584 0.058 Uiso 1 1 calc R . . H63B H 0.3326 0.3535 0.5296 0.058 Uiso 1 1 calc R . . H63C H 0.3714 0.2904 0.5508 0.058 Uiso 1 1 calc R . . C64 C 0.23667(13) 0.1429(2) 0.36915(13) 0.0382(10) Uani 1 1 d . . . C65 C 0.24172(19) 0.1576(3) 0.33044(15) 0.0609(14) Uani 1 1 d . . . C66 C 0.2113(3) 0.1207(3) 0.29244(16) 0.094(2) Uani 1 1 d . . . H66 H 0.2131 0.1301 0.2651 0.112 Uiso 1 1 calc R . . C67 C 0.1783(2) 0.0699(3) 0.2958(3) 0.104(3) Uani 1 1 d . . . H67 H 0.1576 0.0462 0.2704 0.125 Uiso 1 1 calc R . . C68 C 0.1757(2) 0.0552(4) 0.3336(3) 0.096(2) Uani 1 1 d . . . H68 H 0.1540 0.0193 0.3351 0.115 Uiso 1 1 calc R . . C69 C 0.20372(15) 0.0903(3) 0.37059(18) 0.0618(14) Uani 1 1 d . D . C70 C 0.2002(3) 0.0674(5) 0.4140(3) 0.115(3) Uani 1 1 d . . . H70 H 0.2253 0.1027 0.4313 0.137 Uiso 1 1 calc R C 1 C71A C 0.1653(5) 0.1288(10) 0.4140(5) 0.113(5) Uiso 0.50 1 d P D 1 H71A H 0.1625 0.1700 0.3923 0.169 Uiso 0.50 1 calc PR D 1 H71B H 0.1743 0.1534 0.4427 0.169 Uiso 0.50 1 calc PR D 1 H71C H 0.1369 0.1020 0.4070 0.169 Uiso 0.50 1 calc PR D 1 C71B C 0.1594(4) 0.0666(8) 0.4231(4) 0.087(4) Uiso 0.50 1 d P D 2 H71D H 0.1420 0.1144 0.4107 0.131 Uiso 0.50 1 calc PR D 2 H71E H 0.1670 0.0659 0.4545 0.131 Uiso 0.50 1 calc PR D 2 H71F H 0.1421 0.0190 0.4101 0.131 Uiso 0.50 1 calc PR D 2 C72 C 0.2236(3) -0.0033(6) 0.4326(2) 0.138(3) Uani 1 1 d . D . H72A H 0.2328 -0.0010 0.4642 0.207 Uiso 1 1 calc R . . H72B H 0.2495 -0.0081 0.4251 0.207 Uiso 1 1 calc R . . H72C H 0.2044 -0.0496 0.4215 0.207 Uiso 1 1 calc R . . C73 C 0.2781(2) 0.2107(3) 0.32858(18) 0.0754(17) Uani 1 1 d . . . H73 H 0.2870 0.2477 0.3539 0.090 Uiso 1 1 calc R . . C74 C 0.2647(3) 0.2605(4) 0.2876(2) 0.119(3) Uani 1 1 d . . . H74A H 0.2865 0.3025 0.2913 0.179 Uiso 1 1 calc R . . H74B H 0.2358 0.2846 0.2818 0.179 Uiso 1 1 calc R . . H74C H 0.2630 0.2264 0.2631 0.179 Uiso 1 1 calc R . . C75 C 0.3175(3) 0.1627(4) 0.3316(3) 0.132(3) Uani 1 1 d . . . H75A H 0.3264 0.1289 0.3574 0.198 Uiso 1 1 calc R . . H75B H 0.3417 0.1985 0.3335 0.198 Uiso 1 1 calc R . . H75C H 0.3102 0.1291 0.3058 0.198 Uiso 1 1 calc R . . C76 C 0.36667(12) 0.1399(2) 0.53704(11) 0.0302(8) Uani 1 1 d . . . C77 C 0.41060(12) 0.1310(2) 0.54066(12) 0.0324(9) Uani 1 1 d . . . C78 C 0.44027(13) 0.0950(2) 0.57783(12) 0.0352(9) Uani 1 1 d . . . H78 H 0.4701 0.0889 0.5809 0.042 Uiso 1 1 calc R . . C79 C 0.42752(13) 0.0679(2) 0.61050(12) 0.0360(9) Uani 1 1 d . . . H79 H 0.4485 0.0437 0.6356 0.043 Uiso 1 1 calc R . . C80 C 0.38412(13) 0.0761(2) 0.60658(12) 0.0355(9) Uani 1 1 d . . . H80 H 0.3755 0.0572 0.6291 0.043 Uiso 1 1 calc R . . C81 C 0.35280(12) 0.1118(2) 0.56983(12) 0.0318(9) Uani 1 1 d . . . C82 C 0.30460(13) 0.1139(2) 0.56442(13) 0.0379(9) Uani 1 1 d . . . H82 H 0.2885 0.1484 0.5389 0.045 Uiso 1 1 calc R . . C83 C 0.28493(15) 0.0303(3) 0.55470(18) 0.0600(13) Uani 1 1 d . . . H83A H 0.2891 0.0090 0.5292 0.090 Uiso 1 1 calc R . . H83B H 0.2534 0.0328 0.5491 0.090 Uiso 1 1 calc R . . H83C H 0.2997 -0.0044 0.5796 0.090 Uiso 1 1 calc R . . C84 C 0.29766(14) 0.1489(3) 0.60368(14) 0.0477(11) Uani 1 1 d . . . H84A H 0.3115 0.1141 0.6288 0.071 Uiso 1 1 calc R . . H84B H 0.2661 0.1529 0.5974 0.071 Uiso 1 1 calc R . . H84C H 0.3110 0.2020 0.6100 0.071 Uiso 1 1 calc R . . C85 C 0.42471(14) 0.1575(3) 0.50455(13) 0.0426(10) Uani 1 1 d . . . H85 H 0.3987 0.1508 0.4768 0.051 Uiso 1 1 calc R . . C86 C 0.43653(18) 0.2449(3) 0.50853(16) 0.0601(13) Uani 1 1 d . . . H86A H 0.4107 0.2765 0.5063 0.090 Uiso 1 1 calc R . . H86B H 0.4463 0.2601 0.4852 0.090 Uiso 1 1 calc R . . H86C H 0.4603 0.2548 0.5366 0.090 Uiso 1 1 calc R . . C87 C 0.46251(14) 0.1090(3) 0.50031(14) 0.0478(11) Uani 1 1 d . . . H87A H 0.4666 0.1247 0.4738 0.072 Uiso 1 1 calc R . . H87B H 0.4554 0.0521 0.4990 0.072 Uiso 1 1 calc R . . H87C H 0.4897 0.1193 0.5254 0.072 Uiso 1 1 calc R . . Li4 Li 0.0951(2) 0.1089(5) 0.2897(2) 0.0528(19) Uani 1 1 d . H . N7 N 0.06791(11) 0.1382(2) 0.23033(11) 0.0420(8) Uani 1 1 d . . . N8 N 0.04503(14) 0.0872(3) 0.30374(13) 0.0744(14) Uani 1 1 d . . . C88 C 0.02513(15) 0.1478(3) 0.21244(15) 0.0501(11) Uani 1 1 d . H . C89 C -0.00390(14) 0.1301(3) 0.23324(17) 0.0601(14) Uani 1 1 d . . . H89 H -0.0341 0.1392 0.2164 0.072 Uiso 1 1 calc R H . C90 C 0.00522(17) 0.1009(4) 0.27518(18) 0.0760(17) Uani 1 1 d . E . C91 C 0.00406(16) 0.1818(4) 0.16699(16) 0.0707(15) Uani 1 1 d . . . H91A H 0.0159 0.2351 0.1662 0.106 Uiso 1 1 calc R H . H91B H -0.0279 0.1853 0.1589 0.106 Uiso 1 1 calc R . . H91C H 0.0105 0.1469 0.1466 0.106 Uiso 1 1 calc R . . C92A C -0.0353(4) 0.1087(9) 0.2884(4) 0.088(4) Uiso 0.50 1 d P E 1 H92A H -0.0278 0.0880 0.3177 0.132 Uiso 0.50 1 calc PR E 1 H92B H -0.0600 0.0782 0.2681 0.132 Uiso 0.50 1 calc PR E 1 H92C H -0.0437 0.1649 0.2875 0.132 Uiso 0.50 1 calc PR E 1 C92B C -0.0351(3) 0.0667(7) 0.2842(3) 0.053(3) Uiso 0.50 1 d P E 2 H92D H -0.0252 0.0483 0.3143 0.079 Uiso 0.50 1 calc PR E 2 H92E H -0.0480 0.0219 0.2647 0.079 Uiso 0.50 1 calc PR E 2 H92F H -0.0573 0.1085 0.2794 0.079 Uiso 0.50 1 calc PR E 2 C93 C 0.09509(13) 0.1575(3) 0.20699(13) 0.0439(11) Uani 1 1 d . . . C94 C 0.10483(16) 0.0993(3) 0.18124(15) 0.0587(13) Uani 1 1 d . G . C95 C 0.13635(19) 0.1200(4) 0.16374(17) 0.0757(18) Uani 1 1 d . . . H95 H 0.1437 0.0826 0.1462 0.091 Uiso 1 1 calc R . . C96 C 0.15659(19) 0.1930(5) 0.17167(17) 0.0756(18) Uani 1 1 d . . . H96 H 0.1786 0.2045 0.1605 0.091 Uiso 1 1 calc R . . C97 C 0.14584(16) 0.2493(4) 0.19528(16) 0.0697(16) Uani 1 1 d . . . H97 H 0.1594 0.3003 0.1994 0.084 Uiso 1 1 calc R . . C98 C 0.11494(15) 0.2326(3) 0.21351(14) 0.0518(12) Uani 1 1 d . . . C99 C 0.10454(19) 0.2939(3) 0.24150(15) 0.0656(14) Uani 1 1 d . . . H99 H 0.0746 0.2800 0.2405 0.079 Uiso 1 1 calc R . . C100 C 0.1015(3) 0.3793(4) 0.2266(2) 0.108(2) Uani 1 1 d . . . H10A H 0.1305 0.3975 0.2285 0.162 Uiso 1 1 calc R . . H10B H 0.0913 0.4127 0.2449 0.162 Uiso 1 1 calc R . . H10C H 0.0806 0.3830 0.1965 0.162 Uiso 1 1 calc R . . C101 C 0.1353(2) 0.2884(4) 0.28928(19) 0.101(2) Uani 1 1 d . . . H10D H 0.1367 0.2331 0.2991 0.151 Uiso 1 1 calc R . . H10E H 0.1240 0.3223 0.3067 0.151 Uiso 1 1 calc R . . H10F H 0.1648 0.3064 0.2927 0.151 Uiso 1 1 calc R . . C102 C 0.0839(2) 0.0189(3) 0.17367(18) 0.0773(17) Uani 1 1 d . . . H102 H 0.0674 0.0081 0.1929 0.093 Uiso 1 1 calc R F 1 C103 C 0.0556(2) 0.0045(4) 0.1254(2) 0.105(2) Uani 1 1 d . G . H10G H 0.0328 0.0458 0.1151 0.158 Uiso 1 1 calc R . . H10H H 0.0416 -0.0480 0.1220 0.158 Uiso 1 1 calc R . . H10I H 0.0743 0.0066 0.1085 0.158 Uiso 1 1 calc R . . C204 C 0.1253(4) -0.0411(7) 0.1832(4) 0.071(3) Uiso 0.50 1 d P G 1 H20A H 0.1149 -0.0963 0.1793 0.106 Uiso 0.50 1 calc PR G 1 H20B H 0.1464 -0.0335 0.2129 0.106 Uiso 0.50 1 calc PR G 1 H20C H 0.1398 -0.0297 0.1629 0.106 Uiso 0.50 1 calc PR G 1 C304 C 0.1099(5) -0.0552(8) 0.1917(5) 0.089(4) Uiso 0.50 1 d P G 2 H30A H 0.0902 -0.1015 0.1838 0.134 Uiso 0.50 1 calc PR G 2 H30B H 0.1236 -0.0511 0.2233 0.134 Uiso 0.50 1 calc PR G 2 H30C H 0.1327 -0.0616 0.1798 0.134 Uiso 0.50 1 calc PR G 2 C205 C 0.0517(3) 0.0386(6) 0.3441(3) 0.075(3) Uiso 0.60 1 d PD H 1 C206 C 0.0643(3) -0.0409(5) 0.3474(3) 0.062(2) Uiso 0.60 1 d PD H 1 C207 C 0.0742(4) -0.0828(8) 0.3863(4) 0.122(4) Uiso 0.60 1 d PD H 1 H207 H 0.0849 -0.1360 0.3907 0.147 Uiso 0.60 1 calc PR H 1 C208 C 0.0668(5) -0.0389(8) 0.4168(5) 0.116(5) Uiso 0.60 1 d PD H 1 H208 H 0.0664 -0.0692 0.4406 0.140 Uiso 0.60 1 calc PR H 1 C209 C 0.0594(6) 0.0453(9) 0.4201(4) 0.108(5) Uiso 0.60 1 d PD H 1 H209 H 0.0605 0.0727 0.4453 0.130 Uiso 0.60 1 calc PR H 1 C210 C 0.0506(3) 0.0792(6) 0.3794(3) 0.082(3) Uiso 0.60 1 d PD H 1 C211 C 0.0406(3) 0.1752(7) 0.3747(4) 0.081(3) Uiso 0.60 1 d PD H 1 H211 H 0.0284 0.1916 0.3436 0.098 Uiso 0.60 1 calc PR H 1 C212 C 0.0063(5) 0.1925(9) 0.3970(5) 0.146(5) Uiso 0.60 1 d PD H 1 H21A H -0.0207 0.1622 0.3821 0.219 Uiso 0.60 1 calc PR H 1 H21B H -0.0005 0.2496 0.3951 0.219 Uiso 0.60 1 calc PR H 1 H21C H 0.0191 0.1765 0.4275 0.219 Uiso 0.60 1 calc PR H 1 C213 C 0.0800(4) 0.2223(9) 0.3996(5) 0.133(5) Uiso 0.60 1 d PD H 1 H21D H 0.1026 0.2144 0.3875 0.200 Uiso 0.60 1 calc PR H 1 H21E H 0.0914 0.2049 0.4299 0.200 Uiso 0.60 1 calc PR H 1 H21F H 0.0722 0.2789 0.3981 0.200 Uiso 0.60 1 calc PR H 1 C214 C 0.0687(3) -0.0861(6) 0.3090(4) 0.096(4) Uiso 0.60 1 d PD H 1 H214 H 0.0796 -0.0461 0.2932 0.116 Uiso 0.60 1 calc PR H 1 C215 C 0.1025(4) -0.1523(7) 0.3220(4) 0.119(4) Uiso 0.60 1 d PD H 1 H21G H 0.1036 -0.1775 0.2959 0.178 Uiso 0.60 1 calc PR H 1 H21H H 0.0943 -0.1921 0.3390 0.178 Uiso 0.60 1 calc PR H 1 H21I H 0.1314 -0.1302 0.3394 0.178 Uiso 0.60 1 calc PR H 1 C216 C 0.0245(3) -0.1154(5) 0.2762(3) 0.134(5) Uiso 0.60 1 d PD H 1 H21J H 0.0033 -0.0714 0.2684 0.201 Uiso 0.60 1 calc PR H 1 H21K H 0.0135 -0.1587 0.2890 0.201 Uiso 0.60 1 calc PR H 1 H21L H 0.0285 -0.1349 0.2502 0.201 Uiso 0.60 1 calc PR H 1 C305 C 0.0460(3) 0.0739(5) 0.3462(3) 0.087(5) Uiso 0.40 1 d PRD H 2 C306 C 0.0573(3) -0.0046(5) 0.3587(3) 0.088(5) Uiso 0.40 1 d PRD H 2 C307 C 0.0653(3) -0.0282(5) 0.4009(3) 0.227(13) Uiso 0.40 1 d PRD H 2 H307 H 0.0763 -0.0797 0.4113 0.272 Uiso 0.40 1 calc PR H 2 C308 C 0.0571(10) 0.0239(11) 0.4250(7) 0.120(10) Uiso 0.40 1 d PD H 2 H308 H 0.0548 0.0032 0.4506 0.144 Uiso 0.40 1 calc PR H 2 C309 C 0.0507(7) 0.1081(11) 0.4196(5) 0.125(7) Uiso 0.40 1 d PD H 2 H309 H 0.0527 0.1442 0.4422 0.150 Uiso 0.40 1 calc PR H 2 C310 C 0.0410(5) 0.1309(9) 0.3753(4) 0.080(5) Uiso 0.40 1 d PD H 2 C311 C 0.0343(7) 0.2210(10) 0.3583(7) 0.136(8) Uiso 0.40 1 d PD H 2 H311 H 0.0230 0.2164 0.3260 0.163 Uiso 0.40 1 calc PR H 2 C312 C -0.0039(8) 0.2641(16) 0.3677(10) 0.206(13) Uiso 0.40 1 d PD H 2 H31A H -0.0286 0.2273 0.3619 0.309 Uiso 0.40 1 calc PR H 2 H31B H -0.0136 0.3110 0.3490 0.309 Uiso 0.40 1 calc PR H 2 H31C H 0.0070 0.2807 0.3981 0.309 Uiso 0.40 1 calc PR H 2 C313 C 0.0701(8) 0.2779(15) 0.3690(10) 0.199(12) Uiso 0.40 1 d PD H 2 H31D H 0.0953 0.2531 0.3649 0.299 Uiso 0.40 1 calc PR H 2 H31E H 0.0788 0.2944 0.3993 0.299 Uiso 0.40 1 calc PR H 2 H31F H 0.0605 0.3247 0.3502 0.299 Uiso 0.40 1 calc PR H 2 C314 C 0.0606(5) -0.0724(8) 0.3293(5) 0.085(5) Uiso 0.40 1 d PD H 2 H314 H 0.0694 -0.0497 0.3060 0.102 Uiso 0.40 1 calc PR H 2 C315 C 0.0938(6) -0.1352(11) 0.3537(7) 0.142(8) Uiso 0.40 1 d PD H 2 H31G H 0.0945 -0.1775 0.3337 0.214 Uiso 0.40 1 calc PR H 2 H31H H 0.0854 -0.1580 0.3766 0.214 Uiso 0.40 1 calc PR H 2 H31I H 0.1231 -0.1109 0.3668 0.214 Uiso 0.40 1 calc PR H 2 C316 C 0.0149(6) -0.1077(15) 0.3088(9) 0.187(11) Uiso 0.40 1 d PD H 2 H31J H 0.0153 -0.1512 0.2893 0.281 Uiso 0.40 1 calc PR H 2 H31K H -0.0057 -0.0664 0.2923 0.281 Uiso 0.40 1 calc PR H 2 H31L H 0.0057 -0.1284 0.3314 0.281 Uiso 0.40 1 calc PR H 2 Li5 Li 0.1424(3) 0.2569(4) 0.1040(2) 0.0451(17) Uani 1 1 d . . . N9 N 0.14753(10) 0.36362(18) 0.08931(10) 0.0344(8) Uani 1 1 d . . . N10 N 0.16517(11) 0.20390(18) 0.06662(10) 0.0353(8) Uani 1 1 d . . . C117 C 0.15703(13) 0.3819(2) 0.05528(12) 0.0336(9) Uani 1 1 d . . . C118 C 0.17030(13) 0.3255(2) 0.03130(12) 0.0365(9) Uani 1 1 d . . . H118 H 0.1776 0.3468 0.0085 0.044 Uiso 1 1 calc R . . C119 C 0.17432(13) 0.2425(2) 0.03634(12) 0.0334(9) Uani 1 1 d . . . C120 C 0.15344(14) 0.4675(2) 0.03988(13) 0.0403(10) Uani 1 1 d . . . H12A H 0.1243 0.4885 0.0359 0.060 Uiso 1 1 calc R . . H12B H 0.1575 0.4697 0.0123 0.060 Uiso 1 1 calc R . . H12C H 0.1761 0.4997 0.0615 0.060 Uiso 1 1 calc R . . C121 C 0.19033(14) 0.1983(2) 0.00580(13) 0.0414(10) Uani 1 1 d . . . H12D H 0.1989 0.1441 0.0166 0.062 Uiso 1 1 calc R . . H12E H 0.2158 0.2261 0.0039 0.062 Uiso 1 1 calc R . . H12F H 0.1667 0.1960 -0.0230 0.062 Uiso 1 1 calc R . . C122 C 0.13656(13) 0.4255(2) 0.11315(12) 0.0323(9) Uani 1 1 d . . . C123 C 0.09314(13) 0.4359(2) 0.10853(13) 0.0393(10) Uani 1 1 d . J . C124 C 0.08316(14) 0.4941(2) 0.13330(15) 0.0462(11) Uani 1 1 d . . . H124 H 0.0534 0.5024 0.1299 0.055 Uiso 1 1 calc R . . C125 C 0.11598(15) 0.5398(3) 0.16280(15) 0.0488(11) Uani 1 1 d . . . H125 H 0.1088 0.5789 0.1797 0.059 Uiso 1 1 calc R . . C126 C 0.15918(14) 0.5283(2) 0.16749(13) 0.0428(10) Uani 1 1 d . . . H126 H 0.1816 0.5599 0.1877 0.051 Uiso 1 1 calc R . . C127 C 0.17060(13) 0.4713(2) 0.14332(12) 0.0340(9) Uani 1 1 d . . . C128 C 0.21850(13) 0.4570(2) 0.15020(13) 0.0390(10) Uani 1 1 d . . . H128 H 0.2189 0.4364 0.1223 0.047 Uiso 1 1 calc R . . C129 C 0.24685(15) 0.5319(3) 0.16151(16) 0.0537(12) Uani 1 1 d . . . H12G H 0.2328 0.5736 0.1402 0.081 Uiso 1 1 calc R . . H12H H 0.2759 0.5198 0.1613 0.081 Uiso 1 1 calc R . . H12I H 0.2500 0.5504 0.1904 0.081 Uiso 1 1 calc R . . C130 C 0.23809(14) 0.3921(3) 0.18413(14) 0.0493(11) Uani 1 1 d . . . H13D H 0.2350 0.4074 0.2111 0.074 Uiso 1 1 calc R . . H13E H 0.2694 0.3854 0.1894 0.074 Uiso 1 1 calc R . . H13F H 0.2225 0.3418 0.1736 0.074 Uiso 1 1 calc R . . C131 C 0.05571(15) 0.3870(3) 0.07672(16) 0.0556(12) Uani 1 1 d . . . H131 H 0.0733 0.3699 0.0594 0.067 Uiso 1 1 calc R I 1 C232 C 0.0249(3) 0.4384(6) 0.0409(3) 0.045(2) Uiso 0.50 1 d P J 1 H23A H 0.0391 0.4895 0.0404 0.068 Uiso 0.50 1 calc PR J 1 H23B H -0.0022 0.4477 0.0460 0.068 Uiso 0.50 1 calc PR J 1 H23C H 0.0178 0.4113 0.0130 0.068 Uiso 0.50 1 calc PR J 1 C233 C 0.0514(4) 0.3050(7) 0.0911(4) 0.081(4) Uiso 0.50 1 d P J 1 H23D H 0.0785 0.2904 0.1154 0.121 Uiso 0.50 1 calc PR J 1 H23E H 0.0466 0.2677 0.0671 0.121 Uiso 0.50 1 calc PR J 1 H23F H 0.0264 0.3025 0.1003 0.121 Uiso 0.50 1 calc PR J 1 C332 C 0.0382(5) 0.4133(9) 0.0344(4) 0.087(4) Uiso 0.50 1 d P J 2 H33D H 0.0593 0.4485 0.0289 0.131 Uiso 0.50 1 calc PR J 2 H33E H 0.0109 0.4425 0.0294 0.131 Uiso 0.50 1 calc PR J 2 H33F H 0.0319 0.3675 0.0147 0.131 Uiso 0.50 1 calc PR J 2 C333 C 0.0344(3) 0.3342(5) 0.0957(3) 0.039(2) Uiso 0.50 1 d P J 2 H33G H 0.0534 0.3249 0.1260 0.059 Uiso 0.50 1 calc PR J 2 H33H H 0.0286 0.2835 0.0800 0.059 Uiso 0.50 1 calc PR J 2 H33I H 0.0066 0.3577 0.0941 0.059 Uiso 0.50 1 calc PR J 2 C134 C 0.16760(12) 0.1191(2) 0.06987(12) 0.0311(9) Uani 1 1 d . . . C135 C 0.13120(13) 0.0732(2) 0.04612(13) 0.0369(9) Uani 1 1 d . L . C136 C 0.13189(13) -0.0083(2) 0.05460(14) 0.0399(10) Uani 1 1 d . . . H136 H 0.1072 -0.0404 0.0386 0.048 Uiso 1 1 calc R . . C137 C 0.16824(12) -0.0428(2) 0.08611(13) 0.0352(9) Uani 1 1 d . . . H137 H 0.1679 -0.0979 0.0925 0.042 Uiso 1 1 calc R . . C138 C 0.20478(13) 0.0023(2) 0.10813(12) 0.0331(9) Uani 1 1 d . . . H138 H 0.2300 -0.0225 0.1289 0.040 Uiso 1 1 calc R . . C139 C 0.20560(12) 0.0840(2) 0.10062(12) 0.0303(8) Uani 1 1 d . . . C140 C 0.24618(13) 0.1333(2) 0.12567(14) 0.0414(10) Uani 1 1 d . . . C141 C 0.26368(15) 0.1184(3) 0.17485(14) 0.0531(12) Uani 1 1 d . . . H14D H 0.2394 0.1230 0.1850 0.080 Uiso 1 1 calc R . . H14E H 0.2864 0.1580 0.1897 0.080 Uiso 1 1 calc R . . H14F H 0.2764 0.0648 0.1811 0.080 Uiso 1 1 calc R . . C142 C 0.28341(14) 0.1144(3) 0.11003(15) 0.0538(12) Uani 1 1 d . . . H14G H 0.2914 0.0580 0.1153 0.081 Uiso 1 1 calc R . . H14H H 0.3091 0.1475 0.1259 0.081 Uiso 1 1 calc R . . H14I H 0.2735 0.1257 0.0790 0.081 Uiso 1 1 calc R . . C143 C 0.09048(15) 0.1128(3) 0.01269(16) 0.0553(13) Uani 1 1 d . . . H143 H 0.1035 0.1613 0.0048 0.066 Uiso 1 1 calc R K 1 C244 C 0.0623(3) 0.1482(6) 0.0335(3) 0.057(3) Uiso 0.50 1 d P L 1 H24A H 0.0808 0.1737 0.0608 0.086 Uiso 0.50 1 calc PR L 1 H24B H 0.0446 0.1064 0.0394 0.086 Uiso 0.50 1 calc PR L 1 H24C H 0.0428 0.1881 0.0142 0.086 Uiso 0.50 1 calc PR L 1 C344 C 0.0510(6) 0.0936(12) 0.0245(6) 0.142(6) Uiso 0.50 1 d P L 2 H34D H 0.0555 0.1169 0.0528 0.212 Uiso 0.50 1 calc PR L 2 H34E H 0.0479 0.0357 0.0258 0.212 Uiso 0.50 1 calc PR L 2 H34F H 0.0243 0.1159 0.0026 0.212 Uiso 0.50 1 calc PR L 2 C145 C 0.0718(2) 0.0715(4) -0.0289(2) 0.111(3) Uani 1 1 d . L . H14J H 0.0602 0.0197 -0.0247 0.167 Uiso 1 1 calc R . . H14K H 0.0947 0.0637 -0.0406 0.167 Uiso 1 1 calc R . . H14L H 0.0479 0.1036 -0.0491 0.167 Uiso 1 1 calc R . . Li6 Li 0.2146(2) -0.1324(4) 0.0673(2) 0.0359(15) Uani 1 1 d . . . N11 N 0.26578(10) -0.18775(18) 0.10294(9) 0.0301(7) Uani 1 1 d . . . N12 N 0.18121(10) -0.21786(17) 0.03416(10) 0.0314(7) Uani 1 1 d . . . C146 C 0.27231(12) -0.2635(2) 0.09528(11) 0.0307(9) Uani 1 1 d . . . C147 C 0.24210(13) -0.3090(2) 0.06222(12) 0.0333(9) Uani 1 1 d . . . H147 H 0.2515 -0.3612 0.0589 0.040 Uiso 1 1 calc R . . C148 C 0.20000(13) -0.2881(2) 0.03348(12) 0.0334(9) Uani 1 1 d . . . C149 C 0.31506(14) -0.3043(2) 0.12320(13) 0.0413(10) Uani 1 1 d . . . H14M H 0.3389 -0.2862 0.1145 0.062 Uiso 1 1 calc R . . H14N H 0.3117 -0.3622 0.1194 0.062 Uiso 1 1 calc R . . H14O H 0.3222 -0.2909 0.1537 0.062 Uiso 1 1 calc R . . C150 C 0.17478(14) -0.3485(2) -0.00057(13) 0.0408(10) Uani 1 1 d . . . H15A H 0.1470 -0.3613 0.0025 0.061 Uiso 1 1 calc R . . H15B H 0.1924 -0.3971 0.0031 0.061 Uiso 1 1 calc R . . H15C H 0.1686 -0.3263 -0.0294 0.061 Uiso 1 1 calc R . . C151 C 0.29920(12) -0.1439(2) 0.13561(11) 0.0299(8) Uani 1 1 d . . . C152 C 0.33354(12) -0.1097(2) 0.12637(11) 0.0308(9) Uani 1 1 d . . . C153 C 0.36365(13) -0.0611(2) 0.15780(12) 0.0352(9) Uani 1 1 d . . . H153 H 0.3872 -0.0376 0.1521 0.042 Uiso 1 1 calc R . . C154 C 0.35969(13) -0.0469(2) 0.19672(13) 0.0394(10) Uani 1 1 d . . . H154 H 0.3808 -0.0146 0.2179 0.047 Uiso 1 1 calc R . . C155 C 0.32497(13) -0.0794(2) 0.20499(12) 0.0390(10) Uani 1 1 d . . . H155 H 0.3222 -0.0684 0.2317 0.047 Uiso 1 1 calc R . . C156 C 0.29420(12) -0.1278(2) 0.17487(12) 0.0339(9) Uani 1 1 d . . . C157 C 0.25557(13) -0.1626(3) 0.18387(13) 0.0398(10) Uani 1 1 d . . . H157 H 0.2303 -0.1667 0.1554 0.048 Uiso 1 1 calc R . . C158 C 0.24024(16) -0.1105(3) 0.21319(15) 0.0562(13) Uani 1 1 d . . . H15D H 0.2624 -0.1117 0.2428 0.084 Uiso 1 1 calc R . . H15E H 0.2122 -0.1309 0.2131 0.084 Uiso 1 1 calc R . . H15F H 0.2363 -0.0556 0.2024 0.084 Uiso 1 1 calc R . . C159 C 0.26534(15) -0.2470(3) 0.20234(15) 0.0496(11) Uani 1 1 d . . . H15G H 0.2709 -0.2819 0.1814 0.074 Uiso 1 1 calc R . . H15H H 0.2400 -0.2672 0.2080 0.074 Uiso 1 1 calc R . . H15I H 0.2913 -0.2461 0.2294 0.074 Uiso 1 1 calc R . . C160 C 0.33717(13) -0.1221(2) 0.08281(12) 0.0364(9) Uani 1 1 d . . . H160 H 0.3180 -0.1683 0.0683 0.044 Uiso 1 1 calc R . . C161 C 0.38410(14) -0.1406(3) 0.08609(14) 0.0489(11) Uani 1 1 d . . . H16D H 0.4027 -0.0934 0.0966 0.073 Uiso 1 1 calc R . . H16E H 0.3835 -0.1555 0.0575 0.073 Uiso 1 1 calc R . . H16F H 0.3961 -0.1848 0.1063 0.073 Uiso 1 1 calc R . . C162 C 0.31984(16) -0.0483(3) 0.05405(13) 0.0517(12) Uani 1 1 d . . . H16G H 0.2893 -0.0384 0.0505 0.078 Uiso 1 1 calc R . . H16H H 0.3213 -0.0576 0.0256 0.078 Uiso 1 1 calc R . . H16I H 0.3379 -0.0020 0.0677 0.078 Uiso 1 1 calc R . . C163 C 0.13674(12) -0.2039(2) 0.00721(12) 0.0319(9) Uani 1 1 d . . . C164 C 0.12652(13) -0.1607(2) -0.03165(13) 0.0362(9) Uani 1 1 d . . . C165 C 0.08326(14) -0.1395(3) -0.05533(14) 0.0445(10) Uani 1 1 d . . . H165 H 0.0764 -0.1103 -0.0815 0.053 Uiso 1 1 calc R . . C166 C 0.05018(14) -0.1601(3) -0.04162(15) 0.0463(11) Uani 1 1 d . . . H166 H 0.0207 -0.1445 -0.0579 0.056 Uiso 1 1 calc R . . C167 C 0.06006(13) -0.2034(2) -0.00410(15) 0.0444(11) Uani 1 1 d . . . H167 H 0.0369 -0.2183 0.0049 0.053 Uiso 1 1 calc R . . C168 C 0.10262(13) -0.2259(2) 0.02082(13) 0.0365(9) Uani 1 1 d . . . C169 C 0.11209(14) -0.2740(3) 0.06179(14) 0.0509(12) Uani 1 1 d . . . H169 H 0.1441 -0.2879 0.0736 0.061 Uiso 1 1 calc R . . C170 C 0.1025(2) -0.2283(3) 0.09708(18) 0.088(2) Uani 1 1 d . . . H17D H 0.1192 -0.1783 0.1034 0.131 Uiso 1 1 calc R . . H17E H 0.1112 -0.2609 0.1234 0.131 Uiso 1 1 calc R . . H17F H 0.0710 -0.2165 0.0869 0.131 Uiso 1 1 calc R . . C171 C 0.08599(17) -0.3518(3) 0.05239(16) 0.0573(13) Uani 1 1 d . . . H17G H 0.0546 -0.3400 0.0442 0.086 Uiso 1 1 calc R . . H17H H 0.0962 -0.3854 0.0783 0.086 Uiso 1 1 calc R . . H17I H 0.0904 -0.3798 0.0286 0.086 Uiso 1 1 calc R . . C172 C 0.16287(14) -0.1362(3) -0.04714(14) 0.0443(10) Uani 1 1 d . . . H172 H 0.1904 -0.1641 -0.0283 0.053 Uiso 1 1 calc R . . C173 C 0.17185(17) -0.0468(3) -0.0414(2) 0.0678(15) Uani 1 1 d . . . H17J H 0.1971 -0.0336 -0.0489 0.102 Uiso 1 1 calc R . . H17K H 0.1783 -0.0321 -0.0112 0.102 Uiso 1 1 calc R . . H17L H 0.1459 -0.0175 -0.0604 0.102 Uiso 1 1 calc R . . C174 C 0.15286(18) -0.1631(4) -0.09357(16) 0.0753(16) Uani 1 1 d . . . H17M H 0.1453 -0.2199 -0.0963 0.113 Uiso 1 1 calc R . . H17N H 0.1788 -0.1544 -0.1008 0.113 Uiso 1 1 calc R . . H17O H 0.1280 -0.1323 -0.1134 0.113 Uiso 1 1 calc R . . C175 C 0.1303(10) -0.2616(17) 0.2548(9) 0.217(11) Uiso 0.50 1 d P . . C176 C 0.1738(8) -0.3087(15) 0.2614(8) 0.170(8) Uiso 0.50 1 d P . . C177 C 0.1937(8) -0.3539(14) 0.2913(8) 0.169(8) Uiso 0.50 1 d P . . C178 C 0.1959(5) -0.4290(9) 0.3214(5) 0.100(4) Uiso 0.50 1 d P . . C179 C 0.1619(10) -0.4426(16) 0.3122(8) 0.198(10) Uiso 0.50 1 d P . . C180 C 0.1469(6) -0.5042(11) 0.3369(6) 0.136(6) Uiso 0.50 1 d P . . 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 0.053(4) 0.028(3) 0.056(4) -0.001(3) 0.032(4) -0.003(3) N1 0.044(2) 0.0253(16) 0.0288(17) -0.0022(13) 0.0167(15) -0.0013(14) N2 0.0393(19) 0.0250(16) 0.0335(17) -0.0025(14) 0.0193(15) -0.0052(14) C1 0.042(2) 0.025(2) 0.027(2) 0.0004(16) 0.0114(18) -0.0042(17) C2 0.031(2) 0.031(2) 0.031(2) -0.0003(17) 0.0128(17) -0.0055(17) C3 0.030(2) 0.034(2) 0.0234(19) -0.0002(16) 0.0103(16) -0.0003(17) C4 0.056(3) 0.028(2) 0.052(3) -0.0031(19) 0.027(2) -0.007(2) C5 0.045(3) 0.036(2) 0.049(3) -0.0029(19) 0.027(2) -0.0020(19) C6 0.051(3) 0.022(2) 0.042(2) -0.0007(18) 0.027(2) -0.0005(18) C7 0.062(3) 0.033(2) 0.050(3) 0.009(2) 0.035(2) 0.011(2) C8 0.086(4) 0.045(3) 0.058(3) 0.014(2) 0.043(3) 0.027(3) C9 0.097(4) 0.036(3) 0.077(4) 0.006(3) 0.055(3) 0.019(3) C10 0.084(4) 0.042(3) 0.062(3) -0.016(2) 0.040(3) -0.001(3) C11 0.066(3) 0.031(2) 0.054(3) -0.012(2) 0.032(2) -0.004(2) C12 0.073(4) 0.066(3) 0.043(3) -0.023(2) 0.019(3) -0.001(3) C13 0.097(5) 0.122(6) 0.069(4) -0.051(4) 0.006(4) 0.000(4) C14 0.114(5) 0.075(4) 0.055(3) 0.015(3) 0.041(3) 0.040(4) C15 0.057(3) 0.046(3) 0.043(3) 0.011(2) 0.024(2) 0.017(2) C16 0.110(5) 0.063(3) 0.056(3) 0.020(3) 0.040(3) 0.001(3) C17 0.138(6) 0.064(3) 0.056(3) -0.010(3) 0.050(4) -0.028(4) C18 0.036(2) 0.027(2) 0.037(2) -0.0027(17) 0.0232(18) 0.0003(17) C19 0.047(2) 0.025(2) 0.040(2) -0.0025(17) 0.029(2) -0.0002(18) C20 0.054(3) 0.033(2) 0.049(3) -0.012(2) 0.033(2) -0.008(2) C21 0.063(3) 0.025(2) 0.055(3) 0.004(2) 0.041(2) 0.002(2) C22 0.058(3) 0.038(2) 0.040(2) 0.007(2) 0.027(2) 0.008(2) C23 0.052(3) 0.031(2) 0.039(2) 0.0023(18) 0.027(2) 0.0056(19) C24 0.055(3) 0.046(3) 0.043(3) 0.001(2) 0.015(2) 0.007(2) C25 0.080(4) 0.079(4) 0.044(3) -0.014(3) 0.019(3) 0.015(3) C27 0.063(3) 0.032(2) 0.035(2) -0.0097(18) 0.021(2) -0.008(2) C28 0.054(3) 0.075(3) 0.049(3) 0.001(2) 0.028(2) 0.008(3) C29 0.055(3) 0.091(4) 0.036(2) -0.001(2) 0.025(2) -0.014(3) Li2 0.035(4) 0.049(4) 0.027(3) 0.002(3) 0.013(3) -0.006(3) N3 0.0242(17) 0.0360(18) 0.0277(17) 0.0017(14) 0.0124(14) -0.0011(14) N4 0.0320(18) 0.0310(17) 0.0202(15) 0.0000(13) 0.0128(13) 0.0021(14) C30 0.025(2) 0.033(2) 0.029(2) 0.0025(17) 0.0092(16) 0.0061(17) C31 0.026(2) 0.034(2) 0.0226(18) -0.0028(16) 0.0063(16) 0.0014(16) C32 0.028(2) 0.0236(19) 0.028(2) 0.0012(15) 0.0112(16) 0.0062(16) C33 0.034(2) 0.054(3) 0.028(2) 0.0041(19) 0.0121(18) -0.0006(19) C34 0.027(2) 0.035(2) 0.033(2) -0.0034(17) 0.0114(17) -0.0016(17) C35 0.026(2) 0.045(2) 0.0222(19) 0.0042(17) 0.0085(16) -0.0041(17) C36 0.034(2) 0.045(2) 0.0233(19) 0.0076(17) 0.0104(17) -0.0060(19) C37 0.041(3) 0.049(3) 0.036(2) 0.005(2) 0.0105(19) -0.009(2) C38 0.036(3) 0.067(3) 0.043(3) 0.008(2) 0.011(2) -0.016(2) C39 0.027(2) 0.075(3) 0.042(2) 0.009(2) 0.0151(19) -0.002(2) C40 0.024(2) 0.052(3) 0.029(2) 0.0040(18) 0.0094(17) -0.0016(19) C41 0.029(2) 0.060(3) 0.042(2) 0.001(2) 0.0173(19) 0.004(2) C42 0.081(4) 0.077(4) 0.081(4) -0.006(3) 0.058(3) 0.002(3) C43 0.051(3) 0.062(3) 0.068(3) -0.001(3) 0.006(3) 0.005(3) C44 0.048(3) 0.040(2) 0.039(2) 0.0039(19) 0.020(2) 0.000(2) C45 0.052(3) 0.067(3) 0.047(3) 0.018(2) 0.017(2) 0.013(2) C46 0.076(4) 0.039(3) 0.061(3) 0.002(2) 0.030(3) 0.005(2) C47 0.026(2) 0.035(2) 0.0231(18) -0.0040(16) 0.0107(16) -0.0004(16) C48 0.024(2) 0.037(2) 0.0240(19) -0.0048(16) 0.0099(16) 0.0000(16) C49 0.030(2) 0.046(2) 0.031(2) -0.0033(18) 0.0147(17) 0.0014(18) C50 0.040(2) 0.049(3) 0.029(2) 0.0046(19) 0.0208(18) 0.001(2) C51 0.049(3) 0.036(2) 0.039(2) 0.0070(19) 0.020(2) 0.003(2) C52 0.038(2) 0.033(2) 0.030(2) 0.0019(17) 0.0156(18) 0.0041(18) C53 0.060(3) 0.029(2) 0.037(2) 0.0021(18) 0.026(2) 0.008(2) C54 0.059(3) 0.047(3) 0.040(2) 0.004(2) 0.024(2) 0.020(2) C55 0.095(4) 0.035(3) 0.093(4) -0.002(3) 0.051(3) 0.001(3) C56 0.044(2) 0.034(2) 0.033(2) 0.0014(17) 0.0216(19) 0.0030(18) C57 0.045(3) 0.040(2) 0.044(2) -0.005(2) 0.016(2) 0.005(2) C58 0.058(3) 0.038(2) 0.039(2) 0.0004(19) 0.010(2) 0.005(2) Li3 0.057(5) 0.036(4) 0.035(4) -0.008(3) 0.016(3) 0.006(3) N5 0.0304(18) 0.0340(18) 0.0307(17) 0.0040(14) 0.0114(14) 0.0020(14) N6 0.0324(18) 0.0274(17) 0.0273(16) 0.0025(13) 0.0098(14) 0.0023(14) C59 0.025(2) 0.034(2) 0.041(2) 0.0069(18) 0.0113(18) 0.0034(17) C60 0.042(2) 0.025(2) 0.042(2) 0.0054(18) 0.022(2) 0.0047(18) C61 0.038(2) 0.029(2) 0.037(2) -0.0002(17) 0.0204(19) -0.0024(18) C62 0.048(3) 0.041(3) 0.071(3) -0.001(2) 0.002(2) 0.007(2) C63 0.046(3) 0.031(2) 0.042(2) -0.0039(18) 0.021(2) -0.0010(19) C64 0.035(2) 0.035(2) 0.035(2) 0.0082(18) 0.0036(18) 0.0083(19) C65 0.105(4) 0.034(3) 0.038(3) 0.010(2) 0.021(3) 0.010(3) C66 0.174(7) 0.049(3) 0.030(3) 0.012(2) 0.006(3) 0.030(4) C67 0.121(6) 0.028(3) 0.093(5) -0.007(3) -0.040(4) 0.006(3) C68 0.061(4) 0.061(4) 0.116(6) 0.003(4) -0.025(4) -0.002(3) C69 0.032(3) 0.048(3) 0.089(4) -0.006(3) 0.004(3) -0.003(2) C70 0.121(6) 0.099(5) 0.176(8) -0.010(5) 0.116(6) -0.046(5) C72 0.175(9) 0.182(9) 0.081(5) 0.043(6) 0.076(6) 0.003(7) C73 0.136(6) 0.050(3) 0.061(3) 0.012(3) 0.061(4) 0.008(3) C74 0.178(8) 0.089(5) 0.127(6) 0.062(5) 0.098(6) 0.050(5) C75 0.127(7) 0.094(5) 0.182(8) 0.091(6) 0.068(6) 0.025(5) C76 0.038(2) 0.0244(19) 0.027(2) -0.0058(16) 0.0113(17) -0.0037(17) C77 0.034(2) 0.033(2) 0.030(2) -0.0058(17) 0.0116(17) -0.0031(17) C78 0.031(2) 0.040(2) 0.033(2) -0.0090(18) 0.0104(18) 0.0001(18) C79 0.041(2) 0.033(2) 0.027(2) -0.0006(17) 0.0050(18) 0.0030(18) C80 0.039(2) 0.033(2) 0.032(2) 0.0030(17) 0.0107(18) -0.0042(18) C81 0.035(2) 0.028(2) 0.030(2) -0.0015(17) 0.0105(17) -0.0036(17) C82 0.034(2) 0.041(2) 0.039(2) 0.0068(19) 0.0129(18) -0.0019(18) C83 0.042(3) 0.050(3) 0.087(4) -0.007(3) 0.023(3) -0.010(2) C84 0.040(3) 0.060(3) 0.048(3) 0.005(2) 0.023(2) 0.002(2) C85 0.043(3) 0.053(3) 0.032(2) -0.0032(19) 0.0142(19) -0.002(2) C86 0.082(4) 0.053(3) 0.067(3) -0.001(2) 0.053(3) 0.000(3) C87 0.042(3) 0.064(3) 0.044(3) -0.016(2) 0.023(2) -0.008(2) Li4 0.040(4) 0.075(5) 0.044(4) 0.005(4) 0.016(3) 0.002(4) N7 0.033(2) 0.051(2) 0.045(2) 0.0024(17) 0.0187(17) 0.0003(16) N8 0.046(3) 0.137(4) 0.048(2) 0.009(3) 0.027(2) -0.006(3) C88 0.040(3) 0.059(3) 0.049(3) -0.001(2) 0.014(2) -0.001(2) C89 0.024(2) 0.089(4) 0.068(3) 0.005(3) 0.018(2) 0.002(2) C90 0.042(3) 0.133(5) 0.062(4) -0.001(3) 0.030(3) -0.009(3) C91 0.041(3) 0.115(5) 0.050(3) 0.003(3) 0.010(2) 0.009(3) C93 0.033(2) 0.062(3) 0.035(2) 0.006(2) 0.0111(19) 0.004(2) C94 0.055(3) 0.079(4) 0.045(3) 0.013(3) 0.022(2) 0.027(3) C95 0.070(4) 0.117(5) 0.051(3) 0.026(3) 0.036(3) 0.047(4) C96 0.057(4) 0.128(6) 0.048(3) 0.030(4) 0.027(3) 0.014(4) C97 0.043(3) 0.116(5) 0.043(3) 0.027(3) 0.008(2) -0.015(3) C98 0.041(3) 0.075(3) 0.036(2) 0.017(2) 0.011(2) -0.002(2) C99 0.083(4) 0.060(3) 0.048(3) 0.003(3) 0.017(3) -0.021(3) C100 0.144(7) 0.096(5) 0.078(5) 0.020(4) 0.034(4) 0.006(5) C101 0.104(5) 0.116(6) 0.067(4) 0.004(4) 0.016(4) 0.012(4) C102 0.107(5) 0.064(4) 0.064(4) -0.001(3) 0.036(3) 0.022(3) C103 0.088(5) 0.120(6) 0.092(5) -0.006(4) 0.016(4) 0.004(4) Li5 0.063(5) 0.031(4) 0.044(4) 0.000(3) 0.023(4) 0.006(3) N9 0.042(2) 0.0282(17) 0.0269(17) -0.0050(14) 0.0062(15) 0.0030(15) N10 0.045(2) 0.0262(17) 0.0338(18) 0.0002(14) 0.0140(15) 0.0078(15) C117 0.040(2) 0.029(2) 0.023(2) 0.0007(16) 0.0026(17) 0.0027(18) C118 0.048(3) 0.028(2) 0.031(2) 0.0027(17) 0.0122(19) 0.0071(18) C119 0.037(2) 0.034(2) 0.025(2) -0.0004(17) 0.0077(17) 0.0034(18) C120 0.054(3) 0.029(2) 0.039(2) 0.0040(18) 0.019(2) 0.0065(19) C121 0.054(3) 0.035(2) 0.042(2) -0.0014(19) 0.025(2) 0.004(2) C122 0.042(2) 0.026(2) 0.029(2) -0.0010(16) 0.0125(18) 0.0023(17) C123 0.039(3) 0.029(2) 0.046(2) -0.0006(19) 0.012(2) 0.0003(18) C124 0.035(2) 0.043(3) 0.065(3) -0.003(2) 0.025(2) 0.001(2) C125 0.058(3) 0.041(3) 0.061(3) -0.011(2) 0.038(3) -0.002(2) C126 0.049(3) 0.042(2) 0.044(2) -0.018(2) 0.025(2) -0.014(2) C127 0.036(2) 0.037(2) 0.031(2) -0.0040(18) 0.0150(18) -0.0032(18) C128 0.037(2) 0.047(2) 0.032(2) -0.0081(19) 0.0124(18) -0.006(2) C129 0.045(3) 0.059(3) 0.060(3) -0.005(2) 0.023(2) -0.010(2) C130 0.037(3) 0.063(3) 0.045(3) 0.001(2) 0.011(2) 0.001(2) C131 0.043(3) 0.049(3) 0.057(3) 0.004(2) 0.000(2) -0.007(2) C134 0.035(2) 0.025(2) 0.035(2) -0.0019(16) 0.0159(18) 0.0065(17) C135 0.031(2) 0.036(2) 0.039(2) -0.0065(18) 0.0084(18) 0.0078(18) C136 0.028(2) 0.036(2) 0.055(3) -0.016(2) 0.016(2) -0.0033(18) C137 0.035(2) 0.026(2) 0.047(2) -0.0060(18) 0.018(2) 0.0011(18) C138 0.034(2) 0.026(2) 0.038(2) 0.0017(17) 0.0133(18) 0.0048(17) C139 0.029(2) 0.029(2) 0.037(2) -0.0016(17) 0.0171(18) 0.0014(17) C140 0.035(2) 0.035(2) 0.052(3) -0.001(2) 0.015(2) 0.0001(19) C141 0.044(3) 0.061(3) 0.050(3) -0.017(2) 0.013(2) -0.006(2) C142 0.038(3) 0.066(3) 0.059(3) 0.003(2) 0.019(2) -0.010(2) C143 0.043(3) 0.043(3) 0.065(3) -0.011(2) 0.004(2) 0.012(2) C145 0.088(5) 0.122(6) 0.077(4) -0.006(4) -0.023(4) 0.042(4) Li6 0.027(3) 0.036(4) 0.040(4) -0.003(3) 0.008(3) 0.003(3) N11 0.0307(18) 0.0302(18) 0.0293(17) 0.0011(14) 0.0114(14) 0.0017(14) N12 0.0300(18) 0.0284(17) 0.0366(18) -0.0037(14) 0.0137(15) 0.0003(14) C146 0.033(2) 0.031(2) 0.030(2) 0.0047(17) 0.0150(17) 0.0070(17) C147 0.040(2) 0.028(2) 0.037(2) 0.0014(17) 0.0199(19) 0.0065(18) C148 0.043(2) 0.029(2) 0.038(2) -0.0049(17) 0.027(2) -0.0047(18) C149 0.047(3) 0.039(2) 0.040(2) 0.0035(19) 0.019(2) 0.011(2) C150 0.042(3) 0.035(2) 0.047(2) -0.0091(19) 0.018(2) -0.0062(19) C151 0.026(2) 0.033(2) 0.0257(19) 0.0047(16) 0.0038(16) 0.0107(17) C152 0.029(2) 0.033(2) 0.027(2) 0.0032(17) 0.0074(17) 0.0066(17) C153 0.030(2) 0.038(2) 0.031(2) 0.0027(18) 0.0045(17) 0.0051(18) C154 0.035(2) 0.041(2) 0.033(2) -0.0011(18) 0.0027(18) 0.0070(19) C155 0.036(2) 0.052(3) 0.022(2) 0.0013(18) 0.0039(18) 0.014(2) C156 0.030(2) 0.040(2) 0.028(2) 0.0077(17) 0.0063(17) 0.0129(18) C157 0.037(2) 0.055(3) 0.029(2) 0.0038(19) 0.0133(18) 0.007(2) C158 0.062(3) 0.067(3) 0.052(3) 0.011(2) 0.036(3) 0.018(3) C159 0.057(3) 0.052(3) 0.052(3) -0.002(2) 0.035(2) -0.003(2) C160 0.034(2) 0.044(2) 0.030(2) -0.0041(18) 0.0113(18) -0.0030(19) C161 0.049(3) 0.055(3) 0.049(3) -0.007(2) 0.026(2) -0.004(2) C162 0.064(3) 0.061(3) 0.034(2) 0.005(2) 0.022(2) 0.004(2) C163 0.028(2) 0.030(2) 0.036(2) -0.0105(17) 0.0102(17) -0.0031(17) C164 0.035(2) 0.036(2) 0.038(2) -0.0093(18) 0.0136(19) -0.0029(18) C165 0.038(3) 0.043(3) 0.047(3) -0.002(2) 0.010(2) -0.006(2) C166 0.026(2) 0.043(3) 0.061(3) -0.001(2) 0.006(2) -0.0001(19) C167 0.031(2) 0.045(3) 0.060(3) -0.009(2) 0.020(2) -0.010(2) C168 0.030(2) 0.036(2) 0.044(2) -0.0089(19) 0.0148(19) -0.0078(18) C169 0.035(3) 0.075(3) 0.046(3) 0.003(2) 0.018(2) -0.012(2) C170 0.142(6) 0.076(4) 0.065(4) -0.027(3) 0.062(4) -0.061(4) C171 0.074(4) 0.038(3) 0.064(3) 0.007(2) 0.031(3) 0.006(2) C172 0.034(2) 0.056(3) 0.045(3) 0.004(2) 0.017(2) 0.001(2) C173 0.055(3) 0.056(3) 0.110(4) 0.008(3) 0.051(3) -0.005(3) C174 0.065(4) 0.119(5) 0.050(3) 0.004(3) 0.030(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 N1 1.892(7) . ? Li1 N2 1.903(7) . ? Li1 C50 2.406(8) . ? N1 C1 1.321(5) . ? N1 C6 1.433(5) . ? N2 C3 1.337(5) . ? N2 C18 1.413(5) . ? C1 C2 1.411(5) . ? C1 C4 1.515(5) . ? C2 C3 1.396(5) . ? C3 C5 1.501(5) . ? C6 C11 1.394(5) . ? C6 C7 1.395(6) . ? C7 C8 1.403(5) . ? C7 C15 1.524(6) . ? C8 C9 1.367(6) . ? C9 C10 1.382(7) . ? C10 C11 1.406(6) . ? C11 C12 1.546(6) . ? C12 C14 1.503(7) . ? C12 C13 1.536(7) . ? C15 C17 1.503(7) . ? C15 C16 1.510(6) . ? C18 C23 1.399(5) . ? C18 C19 1.415(5) . ? C19 C20 1.399(5) . ? C19 C27 1.518(6) . ? C20 C21 1.384(6) . ? C21 C22 1.369(6) . ? C21 Li3 2.357(7) 3_656 ? C22 C23 1.390(6) . ? C23 C24 1.515(6) . ? C24 C26A 1.46(3) . ? C24 C26B 1.494(14) . ? C24 C25 1.511(6) . ? C27 C28 1.522(6) . ? C27 C29 1.529(6) . ? Li2 N3 1.903(7) . ? Li2 N4 1.907(7) . ? Li2 C79 2.388(7) . ? N3 C30 1.313(5) . ? N3 C35 1.423(5) . ? N4 C32 1.327(5) . ? N4 C47 1.416(4) . ? C30 C31 1.414(5) . ? C30 C33 1.508(5) . ? C31 C32 1.399(5) . ? C32 C34 1.520(5) . ? C35 C40 1.392(5) . ? C35 C36 1.427(6) . ? C36 C37 1.393(5) . ? C36 C44 1.521(6) . ? C37 C38 1.370(6) . ? C38 C39 1.383(7) . ? C39 C40 1.408(6) . ? C40 C41 1.518(6) . ? C41 C43 1.536(6) . ? C41 C42 1.543(6) . ? C44 C45 1.513(6) . ? C44 C46 1.532(6) . ? C47 C52 1.409(5) . ? C47 C48 1.414(5) . ? C48 C49 1.388(5) . ? C48 C56 1.534(5) . ? C49 C50 1.391(6) . ? C50 C51 1.382(6) . ? C51 C52 1.397(5) . ? C52 C53 1.519(5) . ? C53 C55 1.515(6) . ? C53 C54 1.544(6) . ? C56 C58 1.521(6) . ? C56 C57 1.530(5) . ? Li3 N5 1.908(8) . ? Li3 N6 1.911(7) . ? Li3 C21 2.357(7) 3_656 ? N5 C59 1.322(5) . ? N5 C64 1.417(5) . ? N6 C61 1.333(5) . ? N6 C76 1.426(5) . ? C59 C60 1.418(6) . ? C59 C62 1.505(6) . ? C60 C61 1.394(5) . ? C61 C63 1.521(5) . ? C64 C65 1.386(6) . ? C64 C69 1.411(6) . ? C65 C66 1.424(8) . ? C65 C73 1.511(8) . ? C66 C67 1.417(10) . ? C67 C68 1.319(10) . ? C67 Li4 2.740(11) . ? C68 C69 1.363(8) . ? C68 Li4 2.652(10) . ? C69 C70 1.546(9) . ? C70 C72 1.420(11) . ? C70 C71B 1.482(13) . ? C70 C71A 1.543(16) . ? C73 C75 1.494(9) . ? C73 C74 1.519(8) . ? C76 C77 1.410(5) . ? C76 C81 1.416(5) . ? C77 C78 1.392(5) . ? C77 C85 1.513(5) . ? C78 C79 1.385(5) . ? C79 C80 1.388(6) . ? C80 C81 1.402(5) . ? C81 C82 1.524(5) . ? C82 C83 1.527(6) . ? C82 C84 1.530(6) . ? C85 C86 1.510(6) . ? C85 C87 1.535(6) . ? Li4 N7 1.903(8) . ? Li4 N8 1.908(8) . ? N7 C88 1.311(5) . ? N7 C93 1.427(5) . ? N8 C90 1.314(7) . ? N8 C305 1.423(10) . ? N8 C205 1.518(10) . ? C88 C89 1.408(6) . ? C88 C91 1.520(7) . ? C89 C90 1.404(7) . ? C90 C92A 1.559(14) . ? C90 C92B 1.575(11) . ? C93 C98 1.397(7) . ? C93 C94 1.416(7) . ? C94 C95 1.411(7) . ? C94 C102 1.492(8) . ? C95 C96 1.371(9) . ? C96 C97 1.361(8) . ? C96 Li5 2.383(7) . ? C97 C98 1.395(6) . ? C98 C99 1.514(7) . ? C99 C100 1.507(8) . ? C99 C101 1.533(8) . ? C102 C304 1.498(15) . ? C102 C103 1.543(8) . ? C102 C204 1.623(13) . ? C205 C210 1.375(11) . ? C205 C206 1.387(11) . ? C206 C207 1.403(11) . ? C206 C214 1.543(12) . ? C207 C208 1.350(14) . ? C208 C209 1.445(15) . ? C209 C210 1.395(13) . ? C210 C211 1.640(12) . ? C211 C213 1.476(12) . ? C211 C212 1.594(12) . ? C214 C215 1.514(12) . ? C214 C216 1.529(11) . ? C305 C306 1.3900 . ? C305 C310 1.414(13) . ? C306 C307 1.3900 . ? C306 C314 1.532(13) . ? C307 C308 1.285(15) . ? C308 C309 1.430(16) . ? C309 C310 1.442(14) . ? C310 C311 1.601(15) . ? C311 C313 1.451(15) . ? C311 C312 1.578(16) . ? C314 C316 1.515(15) . ? C314 C315 1.514(14) . ? Li5 N9 1.880(7) . ? Li5 N10 1.899(7) . ? N9 C117 1.323(5) . ? N9 C122 1.435(5) . ? N10 C119 1.327(5) . ? N10 C134 1.428(5) . ? C117 C118 1.410(5) . ? C117 C120 1.516(5) . ? C118 C119 1.403(5) . ? C119 C121 1.507(5) . ? C122 C123 1.386(6) . ? C122 C127 1.414(5) . ? C123 C124 1.397(6) . ? C123 C131 1.524(6) . ? C124 C125 1.384(6) . ? C125 C126 1.381(6) . ? C126 C127 1.391(5) . ? C127 C128 1.520(5) . ? C128 C129 1.524(6) . ? C128 C130 1.527(6) . ? C131 C332 1.381(14) . ? C131 C333 1.417(9) . ? C131 C233 1.482(12) . ? C131 C232 1.510(10) . ? C134 C135 1.390(5) . ? C134 C139 1.409(5) . ? C135 C136 1.395(6) . ? C135 C143 1.532(6) . ? C136 C137 1.383(6) . ? C137 C138 1.373(5) . ? C137 Li6 2.385(7) . ? C138 C139 1.396(5) . ? C138 Li6 2.720(7) . ? C139 C140 1.521(5) . ? C140 C142 1.534(6) . ? C140 C141 1.540(6) . ? C143 C145 1.461(7) . ? C143 C244 1.476(11) . ? C143 C344 1.526(18) . ? Li6 N12 1.888(7) . ? Li6 N11 1.895(7) . ? N11 C146 1.331(5) . ? N11 C151 1.424(5) . ? N12 C148 1.335(5) . ? N12 C163 1.414(5) . ? C146 C147 1.398(5) . ? C146 C149 1.522(5) . ? C147 C148 1.396(5) . ? C148 C150 1.514(5) . ? C151 C152 1.400(5) . ? C151 C156 1.407(5) . ? C152 C153 1.399(5) . ? C152 C160 1.517(5) . ? C153 C154 1.375(5) . ? C154 C155 1.383(6) . ? C155 C156 1.386(6) . ? C156 C157 1.527(5) . ? C157 C158 1.533(6) . ? C157 C159 1.530(6) . ? C160 C161 1.535(6) . ? C160 C162 1.537(6) . ? C163 C168 1.408(5) . ? C163 C164 1.411(5) . ? C164 C165 1.385(6) . ? C164 C172 1.526(5) . ? C165 C166 1.373(6) . ? C166 C167 1.376(6) . ? C167 C168 1.381(6) . ? C168 C169 1.515(6) . ? C169 C171 1.528(6) . ? C169 C170 1.535(7) . ? C172 C174 1.526(6) . ? C172 C173 1.526(6) . ? C175 C176 1.58(3) . ? C176 C177 1.22(3) . ? C177 C178 1.60(3) . ? C178 C179 1.06(3) . ? C179 C180 1.52(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 N1 Li1 N2 100.1(3) . . ? N1 Li1 C50 134.6(4) . . ? N2 Li1 C50 114.2(3) . . ? C1 N1 C6 119.0(3) . . ? C1 N1 Li1 121.6(3) . . ? C6 N1 Li1 119.4(3) . . ? C3 N2 C18 121.0(3) . . ? C3 N2 Li1 121.8(3) . . ? C18 N2 Li1 116.6(3) . . ? N1 C1 C2 123.6(3) . . ? N1 C1 C4 119.5(3) . . ? C2 C1 C4 116.9(3) . . ? C3 C2 C1 129.7(4) . . ? N2 C3 C2 122.6(3) . . ? N2 C3 C5 120.5(3) . . ? C2 C3 C5 116.9(3) . . ? C11 C6 C7 120.9(4) . . ? C11 C6 N1 120.1(4) . . ? C7 C6 N1 118.9(3) . . ? C6 C7 C8 118.5(4) . . ? C6 C7 C15 121.1(3) . . ? C8 C7 C15 120.4(4) . . ? C9 C8 C7 120.7(5) . . ? C8 C9 C10 121.2(4) . . ? C9 C10 C11 119.4(4) . . ? C6 C11 C10 119.3(4) . . ? C6 C11 C12 120.5(4) . . ? C10 C11 C12 120.1(4) . . ? C14 C12 C13 110.7(5) . . ? C14 C12 C11 110.5(4) . . ? C13 C12 C11 112.3(4) . . ? C17 C15 C16 109.3(4) . . ? C17 C15 C7 111.3(4) . . ? C16 C15 C7 113.5(4) . . ? C23 C18 N2 119.4(3) . . ? C23 C18 C19 120.5(3) . . ? N2 C18 C19 119.5(3) . . ? C20 C19 C18 118.1(4) . . ? C20 C19 C27 119.7(4) . . ? C18 C19 C27 122.2(3) . . ? C21 C20 C19 120.9(4) . . ? C22 C21 C20 120.2(4) . . ? C22 C21 Li3 108.0(3) . 3_656 ? C20 C21 Li3 98.3(3) . 3_656 ? C21 C22 C23 121.2(4) . . ? C22 C23 C18 119.0(4) . . ? C22 C23 C24 120.2(4) . . ? C18 C23 C24 120.7(4) . . ? C26A C24 C26B 28.9(11) . . ? C26A C24 C25 126.4(11) . . ? C26B C24 C25 113.5(6) . . ? C26A C24 C23 119.2(11) . . ? C26B C24 C23 115.1(6) . . ? C25 C24 C23 112.1(4) . . ? C19 C27 C28 113.2(4) . . ? C19 C27 C29 111.6(4) . . ? C28 C27 C29 108.8(4) . . ? N3 Li2 N4 99.1(3) . . ? N3 Li2 C79 114.1(3) . . ? N4 Li2 C79 132.9(3) . . ? C30 N3 C35 121.3(3) . . ? C30 N3 Li2 121.6(3) . . ? C35 N3 Li2 117.0(3) . . ? C32 N4 C47 120.7(3) . . ? C32 N4 Li2 120.6(3) . . ? C47 N4 Li2 118.4(3) . . ? N3 C30 C31 123.3(3) . . ? N3 C30 C33 120.9(3) . . ? C31 C30 C33 115.8(3) . . ? C32 C31 C30 128.4(3) . . ? N4 C32 C31 124.1(3) . . ? N4 C32 C34 119.8(3) . . ? C31 C32 C34 116.0(3) . . ? C40 C35 N3 120.4(4) . . ? C40 C35 C36 120.9(4) . . ? N3 C35 C36 118.2(3) . . ? C37 C36 C35 118.3(4) . . ? C37 C36 C44 120.7(4) . . ? C35 C36 C44 121.0(3) . . ? C38 C37 C36 121.2(4) . . ? C37 C38 C39 120.4(4) . . ? C38 C39 C40 121.1(4) . . ? C35 C40 C39 118.2(4) . . ? C35 C40 C41 121.0(4) . . ? C39 C40 C41 120.9(4) . . ? C40 C41 C43 111.2(4) . . ? C40 C41 C42 112.7(4) . . ? C43 C41 C42 110.3(4) . . ? C45 C44 C36 111.1(3) . . ? C45 C44 C46 110.1(4) . . ? C36 C44 C46 113.7(4) . . ? C52 C47 N4 120.3(3) . . ? C52 C47 C48 121.2(3) . . ? N4 C47 C48 118.2(3) . . ? C49 C48 C47 118.4(3) . . ? C49 C48 C56 121.3(3) . . ? C47 C48 C56 120.2(3) . . ? C48 C49 C50 120.9(4) . . ? C51 C50 C49 120.2(3) . . ? C51 C50 Li1 95.5(3) . . ? C49 C50 Li1 113.2(3) . . ? C50 C51 C52 121.1(4) . . ? C51 C52 C47 118.1(3) . . ? C51 C52 C53 121.8(3) . . ? C47 C52 C53 119.9(3) . . ? C55 C53 C52 114.0(4) . . ? C55 C53 C54 110.0(4) . . ? C52 C53 C54 109.9(3) . . ? C58 C56 C57 109.4(3) . . ? C58 C56 C48 111.2(3) . . ? C57 C56 C48 114.3(3) . . ? N5 Li3 N6 102.0(3) . . ? N5 Li3 C21 121.8(3) . 3_656 ? N6 Li3 C21 122.3(4) . 3_656 ? C59 N5 C64 120.4(3) . . ? C59 N5 Li3 119.8(3) . . ? C64 N5 Li3 119.0(3) . . ? C61 N6 C76 119.3(3) . . ? C61 N6 Li3 119.9(3) . . ? C76 N6 Li3 120.4(3) . . ? N5 C59 C60 124.0(3) . . ? N5 C59 C62 120.5(4) . . ? C60 C59 C62 115.5(4) . . ? C61 C60 C59 130.1(4) . . ? N6 C61 C60 123.9(4) . . ? N6 C61 C63 120.1(3) . . ? C60 C61 C63 115.9(3) . . ? C65 C64 C69 120.5(4) . . ? C65 C64 N5 122.0(4) . . ? C69 C64 N5 117.2(4) . . ? C64 C65 C66 117.5(5) . . ? C64 C65 C73 121.3(4) . . ? C66 C65 C73 121.2(5) . . ? C67 C66 C65 119.4(6) . . ? C68 C67 C66 121.1(6) . . ? C68 C67 Li4 72.2(5) . . ? C66 C67 Li4 128.5(4) . . ? C67 C68 C69 121.3(7) . . ? C67 C68 Li4 79.6(5) . . ? C69 C68 Li4 122.9(5) . . ? C68 C69 C64 120.2(6) . . ? C68 C69 C70 118.5(6) . . ? C64 C69 C70 121.2(5) . . ? C72 C70 C71B 106.5(8) . . ? C72 C70 C71A 146.7(9) . . ? C71B C70 C71A 43.5(7) . . ? C72 C70 C69 113.5(6) . . ? C71B C70 C69 126.0(9) . . ? C71A C70 C69 98.8(9) . . ? C75 C73 C65 110.9(5) . . ? C75 C73 C74 107.8(5) . . ? C65 C73 C74 113.4(6) . . ? C77 C76 C81 121.1(3) . . ? C77 C76 N6 119.3(3) . . ? C81 C76 N6 119.3(3) . . ? C78 C77 C76 118.1(3) . . ? C78 C77 C85 121.0(4) . . ? C76 C77 C85 120.9(3) . . ? C79 C78 C77 121.8(4) . . ? C78 C79 C80 120.0(4) . . ? C78 C79 Li2 97.8(3) . . ? C80 C79 Li2 111.3(3) . . ? C79 C80 C81 120.8(4) . . ? C80 C81 C76 118.3(4) . . ? C80 C81 C82 119.9(3) . . ? C76 C81 C82 121.7(3) . . ? C81 C82 C83 109.9(3) . . ? C81 C82 C84 113.1(3) . . ? C83 C82 C84 110.2(4) . . ? C86 C85 C77 111.2(3) . . ? C86 C85 C87 109.5(4) . . ? C77 C85 C87 114.8(4) . . ? N7 Li4 N8 101.4(4) . . ? N7 Li4 C68 129.7(4) . . ? N8 Li4 C68 124.9(4) . . ? N7 Li4 C67 101.6(4) . . ? N8 Li4 C67 149.7(5) . . ? C68 Li4 C67 28.3(2) . . ? C88 N7 C93 120.5(4) . . ? C88 N7 Li4 120.3(4) . . ? C93 N7 Li4 118.9(4) . . ? C90 N8 C305 113.0(5) . . ? C90 N8 C205 120.5(5) . . ? C305 N8 C205 24.6(5) . . ? C90 N8 Li4 120.1(4) . . ? C305 N8 Li4 125.4(5) . . ? C205 N8 Li4 118.2(5) . . ? N7 C88 C89 123.9(4) . . ? N7 C88 C91 120.3(4) . . ? C89 C88 C91 115.7(4) . . ? C90 C89 C88 129.6(4) . . ? N8 C90 C89 124.2(4) . . ? N8 C90 C92A 122.1(7) . . ? C89 C90 C92A 111.7(7) . . ? N8 C90 C92B 118.4(6) . . ? C89 C90 C92B 116.2(6) . . ? C92A C90 C92B 26.6(6) . . ? C98 C93 C94 121.1(4) . . ? C98 C93 N7 118.2(4) . . ? C94 C93 N7 120.4(4) . . ? C95 C94 C93 116.9(5) . . ? C95 C94 C102 121.0(5) . . ? C93 C94 C102 122.2(4) . . ? C96 C95 C94 121.2(6) . . ? C97 C96 C95 121.3(5) . . ? C97 C96 Li5 103.6(4) . . ? C95 C96 Li5 108.3(4) . . ? C96 C97 C98 120.2(6) . . ? C97 C98 C93 119.2(5) . . ? C97 C98 C99 120.2(5) . . ? C93 C98 C99 120.5(4) . . ? C100 C99 C98 116.4(5) . . ? C100 C99 C101 109.7(5) . . ? C98 C99 C101 112.8(5) . . ? C94 C102 C304 121.9(8) . . ? C94 C102 C103 112.0(5) . . ? C304 C102 C103 108.4(7) . . ? C94 C102 C204 103.3(6) . . ? C304 C102 C204 25.9(6) . . ? C103 C102 C204 103.7(6) . . ? C210 C205 C206 120.8(9) . . ? C210 C205 N8 116.9(8) . . ? C206 C205 N8 121.7(7) . . ? C205 C206 C207 120.9(9) . . ? C205 C206 C214 121.7(8) . . ? C207 C206 C214 117.4(9) . . ? C208 C207 C206 112.2(12) . . ? C207 C208 C209 132.4(15) . . ? C210 C209 C208 107.7(12) . . ? C205 C210 C209 124.6(10) . . ? C205 C210 C211 118.2(9) . . ? C209 C210 C211 117.0(9) . . ? C213 C211 C212 105.2(10) . . ? C213 C211 C210 111.8(10) . . ? C212 C211 C210 106.5(9) . . ? C215 C214 C216 111.2(9) . . ? C215 C214 C206 114.4(9) . . ? C216 C214 C206 113.0(8) . . ? C306 C305 C310 121.5(7) . . ? C306 C305 N8 110.4(4) . . ? C310 C305 N8 127.8(9) . . ? C307 C306 C305 120.0 . . ? C307 C306 C314 113.9(7) . . ? C305 C306 C314 126.1(7) . . ? C308 C307 C306 115.9(10) . . ? C307 C308 C309 130.4(18) . . ? C310 C309 C308 110.9(15) . . ? C305 C310 C309 119.1(12) . . ? C305 C310 C311 115.6(11) . . ? C309 C310 C311 124.1(13) . . ? C313 C311 C312 106.2(16) . . ? C313 C311 C310 123.0(18) . . ? C312 C311 C310 112.1(16) . . ? C316 C314 C315 111.0(15) . . ? C316 C314 C306 106.3(14) . . ? C315 C314 C306 112.6(14) . . ? N9 Li5 N10 100.4(4) . . ? N9 Li5 C96 132.1(4) . . ? N10 Li5 C96 115.3(3) . . ? C117 N9 C122 119.9(3) . . ? C117 N9 Li5 121.1(3) . . ? C122 N9 Li5 118.7(3) . . ? C119 N10 C134 121.5(3) . . ? C119 N10 Li5 122.0(3) . . ? C134 N10 Li5 116.2(3) . . ? N9 C117 C118 123.8(3) . . ? N9 C117 C120 119.8(3) . . ? C118 C117 C120 116.4(3) . . ? C119 C118 C117 129.3(4) . . ? N10 C119 C118 122.5(3) . . ? N10 C119 C121 120.8(3) . . ? C118 C119 C121 116.7(3) . . ? C123 C122 C127 120.9(3) . . ? C123 C122 N9 119.5(3) . . ? C127 C122 N9 119.4(3) . . ? C122 C123 C124 118.9(4) . . ? C122 C123 C131 122.3(4) . . ? C124 C123 C131 118.7(4) . . ? C125 C124 C123 121.0(4) . . ? C126 C125 C124 119.5(4) . . ? C125 C126 C127 121.5(4) . . ? C126 C127 C122 118.2(4) . . ? C126 C127 C128 120.8(3) . . ? C122 C127 C128 121.0(3) . . ? C127 C128 C129 114.1(4) . . ? C127 C128 C130 110.2(3) . . ? C129 C128 C130 111.0(4) . . ? C332 C131 C333 124.9(8) . . ? C332 C131 C233 125.1(9) . . ? C333 C131 C233 32.0(5) . . ? C332 C131 C232 27.5(6) . . ? C333 C131 C232 114.5(6) . . ? C233 C131 C232 132.1(7) . . ? C332 C131 C123 117.0(7) . . ? C333 C131 C123 115.4(5) . . ? C233 C131 C123 115.2(6) . . ? C232 C131 C123 111.4(5) . . ? C135 C134 C139 121.1(3) . . ? C135 C134 N10 119.9(3) . . ? C139 C134 N10 118.7(3) . . ? C134 C135 C136 118.9(4) . . ? C134 C135 C143 119.9(4) . . ? C136 C135 C143 121.1(4) . . ? C137 C136 C135 120.4(4) . . ? C138 C137 C136 120.2(4) . . ? C138 C137 Li6 88.5(3) . . ? C136 C137 Li6 121.1(3) . . ? C137 C138 C139 121.2(4) . . ? C137 C138 Li6 61.2(2) . . ? C139 C138 Li6 135.4(3) . . ? C138 C139 C134 117.9(3) . . ? C138 C139 C140 120.5(3) . . ? C134 C139 C140 121.5(3) . . ? C139 C140 C142 110.2(3) . . ? C139 C140 C141 113.1(3) . . ? C142 C140 C141 107.8(3) . . ? C145 C143 C244 121.6(6) . . ? C145 C143 C344 93.0(8) . . ? C244 C143 C344 38.5(7) . . ? C145 C143 C135 115.0(4) . . ? C244 C143 C135 111.2(5) . . ? C344 C143 C135 108.2(8) . . ? N12 Li6 N11 100.1(3) . . ? N12 Li6 C137 110.3(3) . . ? N11 Li6 C137 130.4(3) . . ? N12 Li6 C138 140.6(3) . . ? N11 Li6 C138 109.8(3) . . ? C137 Li6 C138 30.30(14) . . ? C146 N11 C151 120.5(3) . . ? C146 N11 Li6 121.2(3) . . ? C151 N11 Li6 118.1(3) . . ? C148 N12 C163 120.5(3) . . ? C148 N12 Li6 120.8(3) . . ? C163 N12 Li6 118.4(3) . . ? N11 C146 C147 123.8(3) . . ? N11 C146 C149 119.4(3) . . ? C147 C146 C149 116.9(3) . . ? C148 C147 C146 128.8(4) . . ? N12 C148 C147 123.6(3) . . ? N12 C148 C150 118.6(4) . . ? C147 C148 C150 117.7(3) . . ? C152 C151 C156 120.9(3) . . ? C152 C151 N11 119.6(3) . . ? C156 C151 N11 119.0(3) . . ? C151 C152 C153 118.3(3) . . ? C151 C152 C160 121.2(3) . . ? C153 C152 C160 120.5(3) . . ? C154 C153 C152 121.1(4) . . ? C153 C154 C155 120.0(4) . . ? C154 C155 C156 121.1(4) . . ? C155 C156 C151 118.6(4) . . ? C155 C156 C157 120.9(3) . . ? C151 C156 C157 120.6(3) . . ? C156 C157 C158 113.9(4) . . ? C156 C157 C159 111.8(3) . . ? C158 C157 C159 109.9(3) . . ? C152 C160 C161 113.6(3) . . ? C152 C160 C162 110.1(3) . . ? C161 C160 C162 109.4(3) . . ? C168 C163 C164 119.3(4) . . ? C168 C163 N12 120.5(3) . . ? C164 C163 N12 119.9(3) . . ? C165 C164 C163 119.4(4) . . ? C165 C164 C172 120.2(4) . . ? C163 C164 C172 120.4(4) . . ? C166 C165 C164 121.0(4) . . ? C165 C166 C167 119.5(4) . . ? C166 C167 C168 121.9(4) . . ? C167 C168 C163 118.8(4) . . ? C167 C168 C169 120.2(4) . . ? C163 C168 C169 121.0(4) . . ? C168 C169 C171 111.3(4) . . ? C168 C169 C170 113.2(4) . . ? C171 C169 C170 108.8(4) . . ? C164 C172 C174 111.7(4) . . ? C164 C172 C173 111.2(4) . . ? C174 C172 C173 112.1(4) . . ? C177 C176 C175 127(3) . . ? C176 C177 C178 152(2) . . ? C179 C178 C177 101(2) . . ? C178 C179 C180 121(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.951 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.081 data_mn1074 _database_code_CSD 162358 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'NacNacLi(Et2O)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H51 Li N2 O' _chemical_formula_weight 498.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 47.323(6) _cell_length_b 10.1697(9) _cell_length_c 19.9329(12) _cell_angle_alpha 90.00 _cell_angle_beta 94.366(7) _cell_angle_gamma 90.00 _cell_volume 9565.1(15) _cell_formula_units_Z 12 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 4.95 _cell_measurement_theta_max 29.73 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.039 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3288 _exptl_absorpt_coefficient_mu 0.459 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8099 _exptl_absorpt_correction_T_max 0.9058 _exptl_absorpt_process_details ; XABS2: an empirical absorption correction program. Parkin, S.; Moezzi, B.; Hope, H. J. Appl. Cryst. 1995, 28, 53-56. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Siemens Cu rotating anode' _diffrn_radiation_monochromator 'nickel filter' _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method 2\q-\w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% '<0.01' _diffrn_reflns_number 6883 _diffrn_reflns_av_R_equivalents 0.0123 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.45 _diffrn_reflns_theta_max 56.38 _reflns_number_total 6292 _reflns_number_gt 5149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens XDISK' _computing_structure_solution 'XS, Bruker SHELXTL v. 5.10' _computing_structure_refinement 'XL, Bruker SHELXTL v. 5.10' _computing_molecular_graphics 'XP, Bruker SHELXTL v. 5.10' _computing_publication_material 'XCIF, Bruker SHELXTL v. 5.10' _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^)+(0.0717P)^2^+9.3260P] 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 6292 _refine_ls_number_parameters 520 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1313 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 O1 O 0.16680(3) 0.51926(14) 0.17583(7) 0.0337(4) Uani 1 1 d . . . O2 O 0.0000 0.4417(2) 0.2500 0.0434(6) Uani 1 2 d S . . N1 N 0.17131(3) 0.62683(16) 0.01004(8) 0.0281(4) Uani 1 1 d . . . N2 N 0.15781(3) 0.82788(16) 0.10794(8) 0.0288(4) Uani 1 1 d . . . N3 N 0.00746(3) 0.13241(17) 0.32252(8) 0.0305(4) Uani 1 1 d . . . Li1 Li 0.16552(8) 0.6437(4) 0.10380(17) 0.0348(8) Uani 1 1 d . . . Li2 Li 0.0000 0.2526(5) 0.2500 0.0379(12) Uani 1 2 d S . . C1 C 0.17018(4) 0.7309(2) -0.02998(10) 0.0296(5) Uani 1 1 d . . . C2 C 0.16294(4) 0.8578(2) -0.00990(10) 0.0312(5) Uani 1 1 d . . . H2A H 0.1619 0.9208 -0.0438 0.037 Uiso 1 1 calc R . . C3 C 0.15697(4) 0.9038(2) 0.05380(10) 0.0299(5) Uani 1 1 d . . . C4 C 0.17752(5) 0.7160(2) -0.10221(11) 0.0419(6) Uani 1 1 d . . . H4A H 0.1658 0.6491 -0.1239 0.063 Uiso 1 1 calc R . . H4B H 0.1971 0.6915 -0.1030 0.063 Uiso 1 1 calc R . . H4C H 0.1743 0.7979 -0.1255 0.063 Uiso 1 1 calc R . . C5 C 0.14953(5) 1.0480(2) 0.05899(11) 0.0414(6) Uani 1 1 d . . . H5A H 0.1325 1.0570 0.0818 0.062 Uiso 1 1 calc R . . H5B H 0.1467 1.0849 0.0147 0.062 Uiso 1 1 calc R . . H5C H 0.1647 1.0935 0.0838 0.062 Uiso 1 1 calc R . . C6 C 0.17868(4) 0.5028(2) -0.01733(10) 0.0279(5) Uani 1 1 d . . . C7 C 0.20693(4) 0.4596(2) -0.01019(10) 0.0327(5) Uani 1 1 d . . . C8 C 0.21320(5) 0.3359(2) -0.03508(12) 0.0416(6) Uani 1 1 d . . . H8A H 0.2318 0.3061 -0.0306 0.050 Uiso 1 1 calc R . . C9 C 0.19262(5) 0.2566(2) -0.06607(12) 0.0460(6) Uani 1 1 d . . . H9A H 0.1974 0.1747 -0.0826 0.055 Uiso 1 1 calc R . . C10 C 0.16489(5) 0.2995(2) -0.07251(12) 0.0429(6) Uani 1 1 d . . . H10A H 0.1510 0.2456 -0.0936 0.051 Uiso 1 1 calc R . . C11 C 0.15722(4) 0.4217(2) -0.04816(10) 0.0327(5) Uani 1 1 d . . . C12 C 0.12658(5) 0.4672(2) -0.05336(11) 0.0399(6) Uani 1 1 d . . . H12A H 0.1266 0.5623 -0.0613 0.048 Uiso 1 1 calc R . . C13 C 0.10830(6) 0.4041(3) -0.11102(14) 0.0643(8) Uani 1 1 d . . . H13A H 0.1170 0.4171 -0.1524 0.096 Uiso 1 1 calc R . . H13B H 0.0899 0.4438 -0.1142 0.096 Uiso 1 1 calc R . . H13C H 0.1065 0.3116 -0.1027 0.096 Uiso 1 1 calc R . . C14 C 0.11302(5) 0.4435(3) 0.01285(14) 0.0592(7) Uani 1 1 d . . . H14A H 0.1233 0.4912 0.0483 0.089 Uiso 1 1 calc R . . H14B H 0.1135 0.3512 0.0232 0.089 Uiso 1 1 calc R . . H14C H 0.0937 0.4731 0.0086 0.089 Uiso 1 1 calc R . . C15 C 0.23025(4) 0.5437(2) 0.02415(11) 0.0395(5) Uani 1 1 d . . . H15A H 0.2224 0.6319 0.0297 0.047 Uiso 1 1 calc R . . C16 C 0.25590(5) 0.5576(3) -0.01692(14) 0.0559(7) Uani 1 1 d . . . H16A H 0.2694 0.6158 0.0058 0.084 Uiso 1 1 calc R . . H16B H 0.2500 0.5928 -0.0604 0.084 Uiso 1 1 calc R . . H16C H 0.2644 0.4728 -0.0221 0.084 Uiso 1 1 calc R . . C17 C 0.23918(5) 0.4909(3) 0.09415(12) 0.0535(7) Uani 1 1 d . . . H17A H 0.2230 0.4871 0.1203 0.080 Uiso 1 1 calc R . . H17B H 0.2532 0.5482 0.1159 0.080 Uiso 1 1 calc R . . H17C H 0.2470 0.4044 0.0904 0.080 Uiso 1 1 calc R . . C18 C 0.15429(4) 0.88558(19) 0.17185(10) 0.0280(5) Uani 1 1 d . . . C19 C 0.17811(4) 0.9374(2) 0.20987(10) 0.0312(5) Uani 1 1 d . . . C20 C 0.17492(5) 0.9774(2) 0.27513(11) 0.0384(5) Uani 1 1 d . . . H20A H 0.1905 1.0113 0.3008 0.046 Uiso 1 1 calc R . . C21 C 0.14925(5) 0.9683(2) 0.30290(11) 0.0416(6) Uani 1 1 d . . . H21A H 0.1477 0.9942 0.3472 0.050 Uiso 1 1 calc R . . C22 C 0.12586(5) 0.9207(2) 0.26508(11) 0.0374(5) Uani 1 1 d . . . H22A H 0.1085 0.9165 0.2840 0.045 Uiso 1 1 calc R . . C23 C 0.12769(4) 0.8788(2) 0.19922(10) 0.0314(5) Uani 1 1 d . . . C24 C 0.10179(4) 0.8258(2) 0.15853(11) 0.0376(5) Uani 1 1 d . . . H24A H 0.1052 0.8340 0.1108 0.045 Uiso 1 1 calc R . . C25 C 0.09734(5) 0.6813(3) 0.17298(15) 0.0572(7) Uani 1 1 d . . . H25A H 0.1141 0.6330 0.1643 0.086 Uiso 1 1 calc R . . H25B H 0.0816 0.6490 0.1446 0.086 Uiso 1 1 calc R . . H25C H 0.0935 0.6705 0.2193 0.086 Uiso 1 1 calc R . . C26 C 0.07487(5) 0.9018(3) 0.16969(16) 0.0666(8) Uani 1 1 d . . . H26A H 0.0783 0.9943 0.1649 0.100 Uiso 1 1 calc R . . H26B H 0.0693 0.8843 0.2141 0.100 Uiso 1 1 calc R . . H26C H 0.0600 0.8749 0.1371 0.100 Uiso 1 1 calc R . . C27 C 0.20681(4) 0.9466(2) 0.18048(11) 0.0357(5) Uani 1 1 d . . . H27A H 0.2036 0.9345 0.1317 0.043 Uiso 1 1 calc R . . C28 C 0.22629(5) 0.8368(3) 0.20700(15) 0.0586(7) Uani 1 1 d . . . H28A H 0.2442 0.8446 0.1879 0.088 Uiso 1 1 calc R . . H28B H 0.2179 0.7534 0.1948 0.088 Uiso 1 1 calc R . . H28C H 0.2291 0.8430 0.2551 0.088 Uiso 1 1 calc R . . C29 C 0.22103(5) 1.0788(3) 0.19219(16) 0.0567(7) Uani 1 1 d . . . H29A H 0.2086 1.1472 0.1747 0.085 Uiso 1 1 calc R . . H29B H 0.2383 1.0811 0.1697 0.085 Uiso 1 1 calc R . . H29C H 0.2253 1.0920 0.2396 0.085 Uiso 1 1 calc R . . C30 C 0.17122(5) 0.5605(2) 0.24516(10) 0.0369(5) Uani 1 1 d . . . H30A H 0.1563 0.5242 0.2703 0.044 Uiso 1 1 calc R . . H30B H 0.1699 0.6555 0.2473 0.044 Uiso 1 1 calc R . . C31 C 0.19952(5) 0.5177(3) 0.27784(12) 0.0473(6) Uani 1 1 d . . . H31A H 0.2023 0.5559 0.3219 0.071 Uiso 1 1 calc R . . H31B H 0.2143 0.5466 0.2510 0.071 Uiso 1 1 calc R . . H31C H 0.2000 0.4236 0.2815 0.071 Uiso 1 1 calc R . . C32 C 0.16515(5) 0.3788(2) 0.16610(12) 0.0419(6) Uani 1 1 d . . . H32A H 0.1824 0.3391 0.1861 0.050 Uiso 1 1 calc R . . H32B H 0.1641 0.3604 0.1182 0.050 Uiso 1 1 calc R . . C33 C 0.14032(6) 0.3161(3) 0.19576(13) 0.0593(7) Uani 1 1 d . . . H33A H 0.1395 0.2247 0.1839 0.089 Uiso 1 1 calc R . . H33B H 0.1232 0.3589 0.1786 0.089 Uiso 1 1 calc R . . H33C H 0.1424 0.3247 0.2438 0.089 Uiso 1 1 calc R . . C34 C 0.00531(4) 0.0039(2) 0.31345(10) 0.0314(5) Uani 1 1 d . . . C35 C 0.0000 -0.0548(3) 0.2500 0.0335(7) Uani 1 2 d S . . H35A H 0.0000 -0.1462 0.2500 0.040 Uiso 1 2 calc SR . . C36 C 0.00860(5) -0.0875(2) 0.37345(11) 0.0418(6) Uani 1 1 d . . . H36A H -0.0036 -0.0588 0.4070 0.063 Uiso 1 1 calc R . . H36B H 0.0279 -0.0863 0.3919 0.063 Uiso 1 1 calc R . . H36C H 0.0035 -0.1752 0.3595 0.063 Uiso 1 1 calc R . . C37 C 0.01470(4) 0.1854(2) 0.38789(10) 0.0311(5) Uani 1 1 d . . . C38 C -0.00676(5) 0.2375(2) 0.42511(11) 0.0362(5) Uani 1 1 d . . . C39 C 0.00102(5) 0.3063(3) 0.48399(12) 0.0469(6) Uani 1 1 d . . . H39A H -0.0130 0.3430 0.5085 0.056 Uiso 1 1 calc R . . C40 C 0.02901(6) 0.3212(3) 0.50660(12) 0.0520(7) Uani 1 1 d . . . H40A H 0.0338 0.3684 0.5458 0.062 Uiso 1 1 calc R . . C41 C 0.04992(5) 0.2659(3) 0.47108(12) 0.0470(6) Uani 1 1 d . . . H41A H 0.0688 0.2749 0.4872 0.056 Uiso 1 1 calc R . . C42 C 0.04336(5) 0.1970(2) 0.41154(11) 0.0365(5) Uani 1 1 d . . . C43 C 0.06681(5) 0.1381(2) 0.37286(11) 0.0403(6) Uani 1 1 d . . . H43A H 0.0582 0.0684 0.3441 0.048 Uiso 1 1 calc R . . C44 C 0.07894(8) 0.2382(3) 0.32714(17) 0.0818(10) Uani 1 1 d . . . H44A H 0.0641 0.2720 0.2964 0.123 Uiso 1 1 calc R . . H44B H 0.0931 0.1973 0.3023 0.123 Uiso 1 1 calc R . . H44C H 0.0873 0.3090 0.3536 0.123 Uiso 1 1 calc R . . C45 C 0.08985(6) 0.0748(4) 0.41888(15) 0.0808(11) Uani 1 1 d . . . H45A H 0.1023 0.0254 0.3925 0.121 Uiso 1 1 calc R . . H45B H 0.0814 0.0170 0.4498 0.121 Uiso 1 1 calc R . . H45C H 0.1005 0.1418 0.4436 0.121 Uiso 1 1 calc R . . C46 C -0.03788(5) 0.2192(2) 0.40212(12) 0.0426(6) Uani 1 1 d . . . H46A H -0.0389 0.1574 0.3643 0.051 Uiso 1 1 calc R . . C47 C -0.05149(5) 0.3476(3) 0.37669(15) 0.0601(7) Uani 1 1 d . . . H47A H -0.0412 0.3818 0.3408 0.090 Uiso 1 1 calc R . . H47B H -0.0510 0.4102 0.4128 0.090 Uiso 1 1 calc R . . H47C H -0.0708 0.3315 0.3605 0.090 Uiso 1 1 calc R . . C48 C -0.05448(5) 0.1596(3) 0.45686(14) 0.0609(7) Uani 1 1 d . . . H48A H -0.0460 0.0776 0.4712 0.091 Uiso 1 1 calc R . . H48B H -0.0737 0.1448 0.4396 0.091 Uiso 1 1 calc R . . H48C H -0.0542 0.2188 0.4944 0.091 Uiso 1 1 calc R . . C49 C 0.01268(7) 0.5176(3) 0.30581(17) 0.0711(9) Uani 1 1 d . . . H49A H 0.0178 0.4585 0.3429 0.085 Uiso 1 1 calc R . . H49B H -0.0014 0.5786 0.3206 0.085 Uiso 1 1 calc R . . C50 C 0.03766(7) 0.5915(3) 0.2904(2) 0.0841(10) Uani 1 1 d . . . H50A H 0.0459 0.6325 0.3306 0.126 Uiso 1 1 calc R . . H50B H 0.0324 0.6577 0.2575 0.126 Uiso 1 1 calc R . . H50C H 0.0512 0.5329 0.2728 0.126 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 O1 0.0401(8) 0.0326(8) 0.0284(8) 0.0028(6) 0.0023(6) 0.0055(7) O2 0.0512(14) 0.0285(12) 0.0484(13) 0.000 -0.0104(11) 0.000 N1 0.0288(9) 0.0298(10) 0.0256(9) 0.0000(8) 0.0020(7) 0.0017(7) N2 0.0301(9) 0.0309(10) 0.0255(9) -0.0012(8) 0.0017(7) 0.0021(7) N3 0.0284(9) 0.0298(10) 0.0327(10) -0.0007(8) -0.0010(7) -0.0021(7) Li1 0.040(2) 0.035(2) 0.0303(18) 0.0022(16) 0.0062(15) 0.0038(16) Li2 0.046(3) 0.030(3) 0.038(3) 0.000 0.001(2) 0.000 C1 0.0280(11) 0.0335(12) 0.0273(11) 0.0022(9) 0.0015(9) 0.0028(9) C2 0.0369(12) 0.0301(12) 0.0265(11) 0.0061(9) 0.0026(9) 0.0046(9) C3 0.0277(11) 0.0301(11) 0.0318(12) -0.0003(10) 0.0009(9) 0.0020(9) C4 0.0608(16) 0.0364(13) 0.0292(12) 0.0029(10) 0.0074(11) 0.0056(11) C5 0.0551(15) 0.0342(13) 0.0346(12) 0.0022(10) 0.0016(11) 0.0090(11) C6 0.0337(12) 0.0280(11) 0.0225(10) 0.0027(9) 0.0055(9) 0.0026(9) C7 0.0356(12) 0.0336(12) 0.0290(11) 0.0019(9) 0.0039(9) 0.0030(10) C8 0.0432(14) 0.0373(14) 0.0439(13) 0.0000(11) 0.0006(11) 0.0117(11) C9 0.0548(16) 0.0314(13) 0.0510(15) -0.0064(11) -0.0005(12) 0.0075(12) C10 0.0513(15) 0.0339(13) 0.0424(13) -0.0022(11) -0.0032(11) -0.0048(11) C11 0.0369(12) 0.0331(12) 0.0280(11) 0.0017(9) 0.0011(9) -0.0019(10) C12 0.0361(13) 0.0404(13) 0.0425(13) 0.0023(11) -0.0020(10) -0.0030(10) C13 0.0430(15) 0.082(2) 0.0651(18) -0.0088(16) -0.0127(13) -0.0069(14) C14 0.0420(15) 0.075(2) 0.0615(17) 0.0052(15) 0.0107(13) 0.0024(14) C15 0.0311(12) 0.0395(13) 0.0475(14) -0.0053(11) 0.0004(10) 0.0051(10) C16 0.0435(15) 0.0658(18) 0.0594(17) 0.0011(14) 0.0099(12) -0.0057(13) C17 0.0425(14) 0.0741(19) 0.0431(14) -0.0098(13) -0.0020(11) 0.0017(13) C18 0.0320(12) 0.0254(11) 0.0264(11) -0.0006(9) 0.0012(9) 0.0058(9) C19 0.0312(11) 0.0298(12) 0.0322(12) -0.0026(9) 0.0000(9) 0.0023(9) C20 0.0376(13) 0.0416(13) 0.0352(13) -0.0052(10) -0.0036(10) -0.0007(10) C21 0.0489(15) 0.0486(15) 0.0275(12) -0.0095(11) 0.0039(11) 0.0006(11) C22 0.0346(13) 0.0434(14) 0.0353(12) -0.0026(10) 0.0090(10) 0.0043(10) C23 0.0318(12) 0.0323(12) 0.0301(11) 0.0000(9) 0.0024(9) 0.0045(9) C24 0.0282(12) 0.0492(14) 0.0354(12) -0.0034(11) 0.0015(9) 0.0011(10) C25 0.0416(14) 0.0506(16) 0.0771(19) -0.0068(14) -0.0111(13) -0.0059(12) C26 0.0381(15) 0.069(2) 0.090(2) -0.0107(17) -0.0116(14) 0.0149(13) C27 0.0312(12) 0.0371(13) 0.0383(12) -0.0035(10) 0.0006(9) -0.0002(10) C28 0.0421(14) 0.0508(16) 0.085(2) 0.0128(15) 0.0176(14) 0.0088(12) C29 0.0388(14) 0.0438(15) 0.088(2) -0.0027(14) 0.0105(13) -0.0029(12) C30 0.0416(13) 0.0388(13) 0.0309(12) 0.0003(10) 0.0056(10) 0.0013(10) C31 0.0439(14) 0.0593(16) 0.0381(13) 0.0115(12) -0.0011(11) -0.0017(12) C32 0.0557(15) 0.0321(13) 0.0382(13) -0.0002(10) 0.0040(11) 0.0083(11) C33 0.083(2) 0.0451(16) 0.0503(15) -0.0013(13) 0.0102(14) -0.0170(14) C34 0.0269(11) 0.0321(13) 0.0346(12) 0.0033(10) -0.0015(9) -0.0005(9) C35 0.0388(18) 0.0236(16) 0.0367(18) 0.000 -0.0057(14) 0.000 C36 0.0495(14) 0.0358(13) 0.0388(13) 0.0058(10) -0.0055(11) -0.0048(11) C37 0.0328(12) 0.0310(12) 0.0287(11) 0.0018(9) -0.0018(9) -0.0035(9) C38 0.0376(13) 0.0386(13) 0.0321(12) -0.0011(10) 0.0012(10) -0.0016(10) C39 0.0491(15) 0.0519(15) 0.0400(14) -0.0082(12) 0.0050(11) 0.0012(12) C40 0.0576(17) 0.0584(17) 0.0385(13) -0.0148(12) -0.0064(12) -0.0048(13) C41 0.0393(14) 0.0565(16) 0.0436(14) -0.0080(12) -0.0073(11) -0.0061(12) C42 0.0339(12) 0.0386(13) 0.0362(12) 0.0007(10) -0.0027(10) -0.0038(10) C43 0.0317(12) 0.0492(14) 0.0394(13) -0.0017(11) -0.0013(10) -0.0043(11) C44 0.100(3) 0.065(2) 0.087(2) 0.0010(18) 0.050(2) -0.0058(18) C45 0.0423(16) 0.144(3) 0.0564(18) 0.0028(19) 0.0034(13) 0.0331(18) C46 0.0350(13) 0.0526(15) 0.0403(13) -0.0033(11) 0.0033(10) 0.0010(11) C47 0.0410(15) 0.0714(19) 0.0673(18) 0.0101(15) 0.0002(13) 0.0062(14) C48 0.0425(15) 0.078(2) 0.0623(17) 0.0078(15) 0.0071(13) -0.0048(14) C49 0.070(2) 0.0397(16) 0.100(2) -0.0030(16) -0.0176(17) -0.0004(14) C50 0.062(2) 0.064(2) 0.123(3) 0.003(2) -0.0081(19) 0.0050(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 O1 C32 1.443(3) . ? O1 C30 1.444(2) . ? O1 Li1 1.911(4) . ? O2 C49 1.446(3) . ? O2 C49 1.446(3) 2 ? O2 Li2 1.924(5) . ? N1 C1 1.324(3) . ? N1 C6 1.428(3) . ? N1 Li1 1.917(4) . ? N2 C3 1.325(3) . ? N2 C18 1.424(3) . ? N2 Li1 1.912(4) . ? N3 C34 1.322(3) . ? N3 C37 1.428(3) . ? N3 Li2 1.905(4) . ? Li2 N3 1.905(4) 2 ? C1 C2 1.402(3) . ? C1 C4 1.514(3) . ? C2 C3 1.402(3) . ? C3 C5 1.513(3) . ? C6 C7 1.404(3) . ? C6 C11 1.412(3) . ? C7 C8 1.393(3) . ? C7 C15 1.517(3) . ? C8 C9 1.374(3) . ? C9 C10 1.379(3) . ? C10 C11 1.392(3) . ? C11 C12 1.518(3) . ? C12 C13 1.526(3) . ? C12 C14 1.530(3) . ? C15 C16 1.521(3) . ? C15 C17 1.524(3) . ? C18 C19 1.411(3) . ? C18 C23 1.411(3) . ? C19 C20 1.382(3) . ? C19 C27 1.522(3) . ? C20 C21 1.376(3) . ? C21 C22 1.379(3) . ? C22 C23 1.389(3) . ? C23 C24 1.516(3) . ? C24 C25 1.515(3) . ? C24 C26 1.521(3) . ? C27 C29 1.514(3) . ? C27 C28 1.517(3) . ? C30 C31 1.508(3) . ? C32 C33 1.498(4) . ? C34 C35 1.404(2) . ? C34 C36 1.513(3) . ? C35 C34 1.404(2) 2 ? C37 C42 1.406(3) . ? C37 C38 1.406(3) . ? C38 C39 1.392(3) . ? C38 C46 1.520(3) . ? C39 C40 1.374(3) . ? C40 C41 1.380(4) . ? C41 C42 1.393(3) . ? C42 C43 1.522(3) . ? C43 C45 1.514(4) . ? C43 C44 1.509(4) . ? C46 C48 1.519(3) . ? C46 C47 1.525(4) . ? C49 C50 1.453(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C32 O1 C30 114.73(16) . . ? C32 O1 Li1 123.78(16) . . ? C30 O1 Li1 121.40(17) . . ? C49 O2 C49 115.5(3) . 2 ? C49 O2 Li2 122.26(14) . . ? C49 O2 Li2 122.26(14) 2 . ? C1 N1 C6 118.41(16) . . ? C1 N1 Li1 120.91(17) . . ? C6 N1 Li1 120.57(16) . . ? C3 N2 C18 119.35(17) . . ? C3 N2 Li1 122.00(17) . . ? C18 N2 Li1 118.58(16) . . ? C34 N3 C37 120.56(17) . . ? C34 N3 Li2 121.49(18) . . ? C37 N3 Li2 117.92(17) . . ? O1 Li1 N2 127.70(19) . . ? O1 Li1 N1 132.4(2) . . ? N2 Li1 N1 99.88(17) . . ? N3 Li2 N3 100.2(3) 2 . ? N3 Li2 O2 129.89(13) 2 . ? N3 Li2 O2 129.89(13) . . ? N1 C1 C2 124.31(18) . . ? N1 C1 C4 119.41(18) . . ? C2 C1 C4 116.28(18) . . ? C3 C2 C1 129.52(19) . . ? N2 C3 C2 123.20(19) . . ? N2 C3 C5 120.12(18) . . ? C2 C3 C5 116.68(18) . . ? C7 C6 C11 120.58(19) . . ? C7 C6 N1 119.74(18) . . ? C11 C6 N1 119.59(18) . . ? C8 C7 C6 118.3(2) . . ? C8 C7 C15 120.18(19) . . ? C6 C7 C15 121.55(19) . . ? C9 C8 C7 121.8(2) . . ? C8 C9 C10 119.6(2) . . ? C9 C10 C11 121.4(2) . . ? C10 C11 C6 118.4(2) . . ? C10 C11 C12 121.4(2) . . ? C6 C11 C12 120.22(19) . . ? C11 C12 C13 114.0(2) . . ? C11 C12 C14 110.75(19) . . ? C13 C12 C14 109.4(2) . . ? C16 C15 C7 113.08(19) . . ? C16 C15 C17 110.4(2) . . ? C7 C15 C17 110.85(19) . . ? C19 C18 C23 120.67(18) . . ? C19 C18 N2 119.43(17) . . ? C23 C18 N2 119.61(18) . . ? C20 C19 C18 118.37(19) . . ? C20 C19 C27 120.57(19) . . ? C18 C19 C27 121.06(18) . . ? C21 C20 C19 121.5(2) . . ? C22 C21 C20 120.0(2) . . ? C21 C22 C23 121.3(2) . . ? C22 C23 C18 118.16(19) . . ? C22 C23 C24 120.57(19) . . ? C18 C23 C24 121.27(18) . . ? C23 C24 C25 111.17(19) . . ? C23 C24 C26 113.2(2) . . ? C25 C24 C26 109.6(2) . . ? C29 C27 C28 110.4(2) . . ? C29 C27 C19 113.25(19) . . ? C28 C27 C19 110.90(19) . . ? O1 C30 C31 112.90(18) . . ? O1 C32 C33 113.85(19) . . ? N3 C34 C35 123.4(2) . . ? N3 C34 C36 119.78(19) . . ? C35 C34 C36 116.9(2) . . ? C34 C35 C34 129.7(3) 2 . ? C42 C37 C38 120.56(19) . . ? C42 C37 N3 119.74(18) . . ? C38 C37 N3 119.39(18) . . ? C39 C38 C37 118.6(2) . . ? C39 C38 C46 120.2(2) . . ? C37 C38 C46 121.15(19) . . ? C40 C39 C38 121.2(2) . . ? C39 C40 C41 119.8(2) . . ? C40 C41 C42 121.4(2) . . ? C41 C42 C37 118.3(2) . . ? C41 C42 C43 120.4(2) . . ? C37 C42 C43 121.26(19) . . ? C45 C43 C44 111.3(2) . . ? C45 C43 C42 112.3(2) . . ? C44 C43 C42 111.5(2) . . ? C38 C46 C48 112.00(19) . . ? C38 C46 C47 111.8(2) . . ? C48 C46 C47 110.6(2) . . ? O2 C49 C50 114.2(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 56.38 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.659 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.041