# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Cousins, David' 'Davidson, Matthew' 'Garc\~Aa-Viv\~A^3^, Daniel' 'Mahon, Mary' _publ_contact_author_name 'Davidson, Matthew' _publ_contact_author_email m.g.davidson@bath.ac.uk _publ_section_title ; Structural Diversity in Polyamine Lewis Base Stabilized Lithium Aryloxides ; _publ_requested_category FM # Attachment '- LiOAr.cif' data_Compound_1b_k08mgd06 _database_code_depnum_ccdc_archive 'CCDC 778584' #TrackingRef '- LiOAr.cif' _audit_creation_date 2008-02-25T12:25:39-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H54 Li2 N4 O2' _chemical_formula_sum 'C30 H54 Li2 N4 O2' _chemical_formula_weight 516.65 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 25.1200(5) _cell_length_b 8.9500(2) _cell_length_c 18.7080(5) _cell_angle_alpha 90 _cell_angle_beta 127.9150(10) _cell_angle_gamma 90 _cell_volume 3318.21(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10799 _cell_measurement_theta_min 3.513 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.034 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.063 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_orient_matrix_ub_11 -0.0335303 _diffrn_orient_matrix_ub_12 -0.069 _diffrn_orient_matrix_ub_13 -0.0501592 _diffrn_orient_matrix_ub_21 0.0317868 _diffrn_orient_matrix_ub_22 -0.0855687 _diffrn_orient_matrix_ub_23 0.0331293 _diffrn_orient_matrix_ub_31 -0.0202855 _diffrn_orient_matrix_ub_32 -0.0200322 _diffrn_orient_matrix_ub_33 0.0312575 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_unetI/netI 0.0418 _diffrn_reflns_number 14427 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.83 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 3766 _reflns_number_gt 2727 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+1.3134P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 3765 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1383 _refine_ls_wR_factor_gt 0.1243 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.194 _refine_diff_density_min -0.199 _refine_diff_density_rms 0.039 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.38838(9) 0.57915(18) 0.57033(14) 0.0540(5) Uani 1 1 d . . . H17A H 0.3469 0.6354 0.5267 0.081 Uiso 1 1 calc R . . H17B H 0.4205 0.5957 0.5578 0.081 Uiso 1 1 calc R . . H17C H 0.4083 0.6131 0.6319 0.081 Uiso 1 1 calc R . . C2 C 0.32079(7) 0.39869(18) 0.57471(11) 0.0410(4) Uani 1 1 d . . . H12A H 0.3367 0.4409 0.6332 0.061 Uiso 1 1 calc R . . H12B H 0.3118 0.2918 0.5735 0.061 Uiso 1 1 calc R . . H12C H 0.2792 0.4495 0.5258 0.061 Uiso 1 1 calc R . . C3 C 0.34792(8) 0.36418(19) 0.47261(11) 0.0442(4) Uani 1 1 d . . . H16A H 0.3763 0.4063 0.4574 0.053 Uiso 1 1 calc R . . H16B H 0.3012 0.4 0.4266 0.053 Uiso 1 1 calc R . . C4 C 0.34890(8) 0.19618(19) 0.46828(10) 0.0443(4) Uani 1 1 d . . . H14A H 0.3176 0.1539 0.4784 0.053 Uiso 1 1 calc R . . H14B H 0.3329 0.1656 0.4071 0.053 Uiso 1 1 calc R . . C5 C 0.46101(8) 0.1720(2) 0.51234(11) 0.0471(4) Uani 1 1 d . . . H13A H 0.4408 0.1352 0.4512 0.071 Uiso 1 1 calc R . . H13B H 0.5051 0.1245 0.5557 0.071 Uiso 1 1 calc R . . H13C H 0.4668 0.2805 0.5142 0.071 Uiso 1 1 calc R . . C6 C 0.41355(11) -0.02847(19) 0.53902(13) 0.0613(5) Uani 1 1 d . . . H18A H 0.3984 -0.0703 0.4808 0.092 Uiso 1 1 calc R . . H18B H 0.3817 -0.0565 0.5506 0.092 Uiso 1 1 calc R . . H18C H 0.4584 -0.0677 0.5876 0.092 Uiso 1 1 calc R . . C10 C 0.59539(6) 0.23085(15) 0.72710(9) 0.0287(3) Uani 1 1 d . . . C11 C 0.62921(6) 0.09270(15) 0.74685(9) 0.0308(3) Uani 1 1 d . . . C12 C 0.67688(7) 0.07508(15) 0.73216(9) 0.0304(3) Uani 1 1 d . . . H5 H 0.6988 -0.0187 0.7454 0.036 Uiso 1 1 calc R . . C13 C 0.69356(6) 0.18914(15) 0.69897(9) 0.0296(3) Uani 1 1 d . . . C14 C 0.65966(6) 0.32429(15) 0.67920(9) 0.0309(3) Uani 1 1 d . . . H7 H 0.67 0.4041 0.6561 0.037 Uiso 1 1 calc R . . C15 C 0.61136(6) 0.34690(15) 0.69201(9) 0.0306(3) Uani 1 1 d . . . C16 C 0.61299(9) -0.03408(19) 0.78318(13) 0.0492(4) Uani 1 1 d . . . H15A H 0.5785 -0.002 0.789 0.074 Uiso 0.5 1 calc PR . . H15B H 0.6539 -0.0638 0.8427 0.074 Uiso 0.5 1 calc PR . . H15C H 0.596 -0.1191 0.7415 0.074 Uiso 0.5 1 calc PR . . H15D H 0.6404 -0.1213 0.7932 0.074 Uiso 0.5 1 calc PR . . H15E H 0.5651 -0.0595 0.7394 0.074 Uiso 0.5 1 calc PR . . H15F H 0.6229 -0.0042 0.8407 0.074 Uiso 0.5 1 calc PR . . C17 C 0.74631(7) 0.16807(17) 0.68521(11) 0.0402(4) Uani 1 1 d . . . H10A H 0.7903 0.2005 0.7397 0.06 Uiso 1 1 calc R . . H10B H 0.7343 0.2277 0.6333 0.06 Uiso 1 1 calc R . . H10C H 0.7486 0.0623 0.6738 0.06 Uiso 1 1 calc R . . C18 C 0.57474(8) 0.49397(17) 0.66791(11) 0.0411(4) Uani 1 1 d . . . H11A H 0.5428 0.4895 0.6815 0.062 Uiso 0.5 1 calc PR . . H11B H 0.5502 0.5139 0.6032 0.062 Uiso 0.5 1 calc PR . . H11C H 0.6074 0.5741 0.7034 0.062 Uiso 0.5 1 calc PR . . H11D H 0.5908 0.5622 0.6439 0.062 Uiso 0.5 1 calc PR . . H11E H 0.5834 0.5378 0.7222 0.062 Uiso 0.5 1 calc PR . . H11F H 0.5262 0.4775 0.622 0.062 Uiso 0.5 1 calc PR . . O1 O 0.54967(5) 0.25028(11) 0.74033(6) 0.0343(3) Uani 1 1 d . . . N1 N 0.37261(6) 0.41947(13) 0.56232(8) 0.0357(3) Uani 1 1 d . . . N2 N 0.41673(6) 0.13547(14) 0.53617(8) 0.0392(3) Uani 1 1 d . . . Li1 Li 0.45460(11) 0.2582(3) 0.66223(16) 0.0319(5) Uani 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 C1 0.0467(9) 0.0377(9) 0.0704(13) 0.0111(8) 0.0323(9) 0.0049(7) C2 0.0331(8) 0.0486(9) 0.0398(9) 0.0081(7) 0.0217(7) 0.0063(7) C3 0.0377(8) 0.0596(10) 0.0323(8) 0.0144(7) 0.0200(7) 0.0099(7) C4 0.0370(8) 0.0610(10) 0.0287(8) -0.0065(7) 0.0170(7) -0.0070(7) C5 0.0435(9) 0.0564(10) 0.0393(9) -0.0094(7) 0.0244(8) -0.0009(7) C6 0.0983(15) 0.0412(9) 0.0507(11) -0.0058(8) 0.0489(12) -0.0026(9) C10 0.0233(6) 0.0401(7) 0.0232(7) -0.0033(5) 0.0146(6) -0.0021(5) C11 0.0292(7) 0.0362(7) 0.0277(7) 0.0008(5) 0.0178(6) -0.0017(6) C12 0.0289(7) 0.0327(7) 0.0285(7) -0.0011(5) 0.0170(6) 0.0012(5) C13 0.0261(6) 0.0364(7) 0.0267(7) -0.0036(5) 0.0164(6) -0.0018(6) C14 0.0290(7) 0.0353(7) 0.0295(7) 0.0019(5) 0.0186(6) -0.0026(6) C15 0.0253(6) 0.0354(7) 0.0282(7) -0.0001(5) 0.0151(6) 0.0010(6) C16 0.0545(10) 0.0479(9) 0.0616(11) 0.0129(8) 0.0440(9) 0.0044(8) C17 0.0376(8) 0.0442(8) 0.0498(10) 0.0013(7) 0.0325(8) 0.0013(7) C18 0.0365(8) 0.0416(8) 0.0474(9) 0.0054(7) 0.0269(7) 0.0055(6) O1 0.0283(5) 0.0475(6) 0.0332(6) -0.0013(4) 0.0219(5) 0.0000(4) N1 0.0316(6) 0.0362(6) 0.0362(7) 0.0060(5) 0.0193(6) 0.0017(5) N2 0.0454(7) 0.0395(7) 0.0296(7) -0.0033(5) 0.0216(6) -0.0010(6) Li1 0.0303(11) 0.0361(12) 0.0301(12) 0.0013(9) 0.0189(10) -0.0010(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.4659(19) . ? C1 H17A 0.98 . ? C1 H17B 0.98 . ? C1 H17C 0.98 . ? C2 N1 1.4673(18) . ? C2 H12A 0.98 . ? C2 H12B 0.98 . ? C2 H12C 0.98 . ? C3 N1 1.472(2) . ? C3 C4 1.507(2) . ? C3 H16A 0.99 . ? C3 H16B 0.99 . ? C4 N2 1.467(2) . ? C4 H14A 0.99 . ? C4 H14B 0.99 . ? C5 N2 1.467(2) . ? C5 H13A 0.98 . ? C5 H13B 0.98 . ? C5 H13C 0.98 . ? C6 N2 1.472(2) . ? C6 H18A 0.98 . ? C6 H18B 0.98 . ? C6 H18C 0.98 . ? C10 O1 1.3267(15) . ? C10 C15 1.4122(19) . ? C10 C11 1.4146(19) . ? C11 C12 1.3925(18) . ? C11 C16 1.502(2) . ? C12 C13 1.3867(19) . ? C12 H5 0.95 . ? C13 C14 1.3921(19) . ? C13 C17 1.5089(18) . ? C14 C15 1.3884(18) . ? C14 H7 0.95 . ? C15 C18 1.5074(19) . ? C16 H15A 0.98 . ? C16 H15B 0.98 . ? C16 H15C 0.98 . ? C16 H15D 0.98 . ? C16 H15E 0.98 . ? C16 H15F 0.98 . ? C17 H10A 0.98 . ? C17 H10B 0.98 . ? C17 H10C 0.98 . ? C18 H11A 0.98 . ? C18 H11B 0.98 . ? C18 H11C 0.98 . ? C18 H11D 0.98 . ? C18 H11E 0.98 . ? C18 H11F 0.98 . ? O1 Li1 1.885(2) . ? O1 Li1 1.892(2) 2_656 ? N1 Li1 2.256(3) . ? N2 Li1 2.217(3) . ? Li1 O1 1.892(2) 2_656 ? Li1 Li1 2.604(5) 2_656 ? 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 C1 H17A 109.5 . . ? N1 C1 H17B 109.5 . . ? H17A C1 H17B 109.5 . . ? N1 C1 H17C 109.5 . . ? H17A C1 H17C 109.5 . . ? H17B C1 H17C 109.5 . . ? N1 C2 H12A 109.5 . . ? N1 C2 H12B 109.5 . . ? H12A C2 H12B 109.5 . . ? N1 C2 H12C 109.5 . . ? H12A C2 H12C 109.5 . . ? H12B C2 H12C 109.5 . . ? N1 C3 C4 112.79(12) . . ? N1 C3 H16A 109 . . ? C4 C3 H16A 109 . . ? N1 C3 H16B 109 . . ? C4 C3 H16B 109 . . ? H16A C3 H16B 107.8 . . ? N2 C4 C3 111.82(13) . . ? N2 C4 H14A 109.3 . . ? C3 C4 H14A 109.3 . . ? N2 C4 H14B 109.3 . . ? C3 C4 H14B 109.3 . . ? H14A C4 H14B 107.9 . . ? N2 C5 H13A 109.5 . . ? N2 C5 H13B 109.5 . . ? H13A C5 H13B 109.5 . . ? N2 C5 H13C 109.5 . . ? H13A C5 H13C 109.5 . . ? H13B C5 H13C 109.5 . . ? N2 C6 H18A 109.5 . . ? N2 C6 H18B 109.5 . . ? H18A C6 H18B 109.5 . . ? N2 C6 H18C 109.5 . . ? H18A C6 H18C 109.5 . . ? H18B C6 H18C 109.5 . . ? O1 C10 C15 121.07(12) . . ? O1 C10 C11 121.04(12) . . ? C15 C10 C11 117.89(11) . . ? C12 C11 C10 119.91(12) . . ? C12 C11 C16 120.60(13) . . ? C10 C11 C16 119.49(12) . . ? C13 C12 C11 122.56(12) . . ? C13 C12 H5 118.7 . . ? C11 C12 H5 118.7 . . ? C12 C13 C14 117.05(12) . . ? C12 C13 C17 121.54(12) . . ? C14 C13 C17 121.41(12) . . ? C15 C14 C13 122.52(12) . . ? C15 C14 H7 118.7 . . ? C13 C14 H7 118.7 . . ? C14 C15 C10 120.07(12) . . ? C14 C15 C18 120.86(12) . . ? C10 C15 C18 119.07(12) . . ? C11 C16 H15A 109.5 . . ? C11 C16 H15B 109.5 . . ? H15A C16 H15B 109.5 . . ? C11 C16 H15C 109.5 . . ? H15A C16 H15C 109.5 . . ? H15B C16 H15C 109.5 . . ? C11 C16 H15D 109.5 . . ? H15A C16 H15D 141.1 . . ? H15B C16 H15D 56.3 . . ? H15C C16 H15D 56.3 . . ? C11 C16 H15E 109.5 . . ? H15A C16 H15E 56.3 . . ? H15B C16 H15E 141.1 . . ? H15C C16 H15E 56.3 . . ? H15D C16 H15E 109.5 . . ? C11 C16 H15F 109.5 . . ? H15A C16 H15F 56.3 . . ? H15B C16 H15F 56.3 . . ? H15C C16 H15F 141.1 . . ? H15D C16 H15F 109.5 . . ? H15E C16 H15F 109.5 . . ? C13 C17 H10A 109.5 . . ? C13 C17 H10B 109.5 . . ? H10A C17 H10B 109.5 . . ? C13 C17 H10C 109.5 . . ? H10A C17 H10C 109.5 . . ? H10B C17 H10C 109.5 . . ? C15 C18 H11A 109.5 . . ? C15 C18 H11B 109.5 . . ? H11A C18 H11B 109.5 . . ? C15 C18 H11C 109.5 . . ? H11A C18 H11C 109.5 . . ? H11B C18 H11C 109.5 . . ? C15 C18 H11D 109.5 . . ? H11A C18 H11D 141.1 . . ? H11B C18 H11D 56.3 . . ? H11C C18 H11D 56.3 . . ? C15 C18 H11E 109.5 . . ? H11A C18 H11E 56.3 . . ? H11B C18 H11E 141.1 . . ? H11C C18 H11E 56.3 . . ? H11D C18 H11E 109.5 . . ? C15 C18 H11F 109.5 . . ? H11A C18 H11F 56.3 . . ? H11B C18 H11F 56.3 . . ? H11C C18 H11F 141.1 . . ? H11D C18 H11F 109.5 . . ? H11E C18 H11F 109.5 . . ? C10 O1 Li1 133.62(11) . . ? C10 O1 Li1 138.83(11) . 2_656 ? Li1 O1 Li1 87.17(11) . 2_656 ? C1 N1 C2 108.52(12) . . ? C1 N1 C3 110.02(13) . . ? C2 N1 C3 110.14(12) . . ? C1 N1 Li1 119.17(11) . . ? C2 N1 Li1 103.59(10) . . ? C3 N1 Li1 105.07(11) . . ? C4 N2 C5 110.40(12) . . ? C4 N2 C6 109.91(14) . . ? C5 N2 C6 107.52(13) . . ? C4 N2 Li1 104.38(11) . . ? C5 N2 Li1 107.65(11) . . ? C6 N2 Li1 116.90(12) . . ? O1 Li1 O1 92.67(11) . 2_656 ? O1 Li1 N2 108.48(11) . . ? O1 Li1 N2 139.91(12) 2_656 . ? O1 Li1 N1 137.98(12) . . ? O1 Li1 N1 105.00(11) 2_656 . ? N2 Li1 N1 81.90(9) . . ? O1 Li1 Li1 46.52(8) . 2_656 ? O1 Li1 Li1 46.31(8) 2_656 2_656 ? N2 Li1 Li1 144.31(10) . 2_656 ? N1 Li1 Li1 133.72(9) . 2_656 ? #===END data_Compound_1c_h08mgd11 _database_code_depnum_ccdc_archive 'CCDC 778585' #TrackingRef '- LiOAr.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H39 Li N2 O' _chemical_formula_weight 342.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 18.1130(11) _cell_length_b 13.6090(6) _cell_length_c 28.5820(17) _cell_angle_alpha 90.00 _cell_angle_beta 103.924(2) _cell_angle_gamma 90.00 _cell_volume 6838.4(7) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 172193 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 27.485 _exptl_crystal_description tabloid _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.998 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 0.060 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50422 _diffrn_reflns_av_R_equivalents 0.1350 _diffrn_reflns_av_sigmaI/netI 0.1715 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 25.03 _reflns_number_total 19936 _reflns_number_gt 8511 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _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^ > 2\s(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. The solution and refinement of this structure is a testimony to the engineering of modern diffractometers. Despite copious efforts on the part of the chemist, it proved impossible to improve the quality of these crystals and this is reflected in the esds associated with the unit cell parameters, atom positions and derived metric data. Nonetheless the structural characterization is unambiguous. With 6 molecules in the asymmetric unit, anisotropic refinement of all atoms was possible, despite truncation of data to a Bragg angle of 25\% in response to a combination of the crystal size, pseudosymmetry and diffraction fall-off in higher data shells. It is also highly likely that some disorder exists in several of the ethyl bridges of the bidentate amine ligands. Data quality was not of sufficient quality to resolve this unfortunately. To aid convergence, carbons in these ethyl groups were refined subject to some ADP restraints in the final least squares. ; _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^)+(0.1121P)^2^+5.4193P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 7(4) _refine_ls_number_reflns 19936 _refine_ls_number_parameters 1351 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.2313 _refine_ls_R_factor_gt 0.0929 _refine_ls_wR_factor_ref 0.2974 _refine_ls_wR_factor_gt 0.2135 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.038 _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 0.0298(5) 0.0522(6) 0.6232(3) 0.059(2) Uani 1 1 d . . . O2 O 0.0162(5) 0.0442(6) 0.2841(3) 0.053(2) Uani 1 1 d . . . O3 O 0.5324(5) 0.2493(6) 0.2945(3) 0.054(2) Uani 1 1 d . . . O4 O 0.4837(5) 0.7579(6) 0.3777(3) 0.055(2) Uani 1 1 d . . . O5 O 0.4786(4) 0.7855(5) 0.0493(2) 0.0409(19) Uani 1 1 d . . . O6 O 0.9744(5) 0.5793(5) 0.0391(2) 0.052(2) Uani 1 1 d . . . N1 N 0.0708(7) 0.0866(8) 0.7462(3) 0.059(3) Uani 1 1 d . . . N2 N 0.1300(7) 0.2378(8) 0.6977(4) 0.064(3) Uani 1 1 d . . . N3 N 0.0425(10) 0.0784(8) 0.4064(3) 0.088(4) Uani 1 1 d . . . N4 N 0.1218(7) 0.2220(7) 0.3636(4) 0.067(3) Uani 1 1 d . . . N5 N 0.6402(7) 0.0766(7) 0.3706(3) 0.056(3) Uani 1 1 d . . . N6 N 0.5701(6) 0.2232(9) 0.4188(3) 0.057(3) Uani 1 1 d . . . N7 N 0.3692(6) 0.5966(7) 0.2939(3) 0.055(3) Uani 1 1 d . . . N8 N 0.4539(8) 0.7361(7) 0.2527(3) 0.064(3) Uani 1 1 d . . . N9 N 0.3794(6) 0.5967(7) -0.0250(3) 0.047(3) Uani 1 1 d . . . N10 N 0.4362(6) 0.7510(6) -0.0759(3) 0.051(3) Uani 1 1 d . . . N11 N 0.8592(6) 0.7413(7) -0.0433(3) 0.044(2) Uani 1 1 d . . . N12 N 0.9425(7) 0.6029(7) -0.0872(3) 0.060(3) Uani 1 1 d . . . C1 C 0.0927(10) -0.0189(11) 0.7601(5) 0.089(5) Uani 1 1 d . . . H3 H 0.0888 -0.0308 0.7933 0.134 Uiso 1 1 calc R . . H4 H 0.1451 -0.0307 0.7579 0.134 Uiso 1 1 calc R . . H5 H 0.0584 -0.0636 0.7382 0.134 Uiso 1 1 calc R . . C2 C 0.0013(9) 0.1074(10) 0.7588(5) 0.076(4) Uani 1 1 d . . . H17G H 0.0072 0.0952 0.7933 0.114 Uiso 1 1 calc R . . H17H H -0.0389 0.0649 0.7402 0.114 Uiso 1 1 calc R . . H17I H -0.0124 0.1763 0.7516 0.114 Uiso 1 1 calc R . . C3 C 0.1340(10) 0.1443(11) 0.7708(5) 0.096(5) Uani 1 1 d U . . H82A H 0.1818 0.1109 0.7690 0.115 Uiso 1 1 calc R . . H82B H 0.1332 0.1498 0.8052 0.115 Uiso 1 1 calc R . . C4 C 0.1324(9) 0.2441(10) 0.7497(4) 0.074(4) Uani 1 1 d U . . H16N H 0.0870 0.2800 0.7542 0.088 Uiso 1 1 calc R . . H16O H 0.1782 0.2810 0.7665 0.088 Uiso 1 1 calc R . . C5 C 0.2023(9) 0.2192(13) 0.6857(6) 0.100(5) Uani 1 1 d . . . H6 H 0.2359 0.2760 0.6950 0.150 Uiso 1 1 calc R . . H7 H 0.1937 0.2082 0.6509 0.150 Uiso 1 1 calc R . . H8 H 0.2261 0.1608 0.7031 0.150 Uiso 1 1 calc R . . C6 C 0.1023(10) 0.3371(10) 0.6765(5) 0.094(5) Uani 1 1 d . . . H18D H 0.1345 0.3890 0.6946 0.142 Uiso 1 1 calc R . . H18E H 0.0496 0.3471 0.6785 0.142 Uiso 1 1 calc R . . H18F H 0.1049 0.3394 0.6427 0.142 Uiso 1 1 calc R . . C7 C -0.0026(6) 0.0050(9) 0.5841(4) 0.044(3) Uani 1 1 d . . . C8 C -0.0808(8) 0.0293(9) 0.5595(4) 0.055(3) Uani 1 1 d . . . C9 C -0.1120(7) -0.0309(10) 0.5187(4) 0.059(4) Uani 1 1 d . . . H91 H -0.1629 -0.0177 0.5018 0.071 Uiso 1 1 calc R . . C10 C -0.0743(7) -0.1079(9) 0.5013(4) 0.052(3) Uani 1 1 d . . . C11 C 0.0011(6) -0.1226(8) 0.5252(4) 0.046(3) Uani 1 1 d . . . H22 H 0.0289 -0.1728 0.5140 0.055 Uiso 1 1 calc R . . C12 C 0.0368(6) -0.0687(9) 0.5638(4) 0.043(3) Uani 1 1 d . . . C13 C 0.1214(7) -0.0881(10) 0.5873(4) 0.057(4) Uani 1 1 d . . . C14 C 0.1290(7) -0.1238(11) 0.6412(5) 0.066(4) Uani 1 1 d . . . H14D H 0.1022 -0.1864 0.6410 0.100 Uiso 1 1 calc R . . H14E H 0.1066 -0.0745 0.6586 0.100 Uiso 1 1 calc R . . H14F H 0.1829 -0.1325 0.6572 0.100 Uiso 1 1 calc R . . C15 C 0.1669(7) 0.0029(11) 0.5858(4) 0.067(4) Uani 1 1 d . . . H14A H 0.2211 -0.0116 0.5982 0.100 Uiso 1 1 calc R . . H14B H 0.1515 0.0538 0.6059 0.100 Uiso 1 1 calc R . . H14C H 0.1580 0.0264 0.5525 0.100 Uiso 1 1 calc R . . C16 C 0.1566(8) -0.1691(12) 0.5627(5) 0.078(4) Uani 1 1 d . . . H15A H 0.1276 -0.2300 0.5625 0.117 Uiso 1 1 calc R . . H15B H 0.2094 -0.1797 0.5805 0.117 Uiso 1 1 calc R . . H15C H 0.1553 -0.1495 0.5296 0.117 Uiso 1 1 calc R . . C17 C -0.1252(7) 0.1087(9) 0.5757(5) 0.063(4) Uani 1 1 d . . . C18 C -0.0822(7) 0.2083(9) 0.5770(5) 0.077(4) Uani 1 1 d . . . H99A H -0.0294 0.2003 0.5955 0.116 Uiso 1 1 calc R . . H99B H -0.1073 0.2584 0.5924 0.116 Uiso 1 1 calc R . . H99C H -0.0829 0.2288 0.5441 0.116 Uiso 1 1 calc R . . C19 C -0.1339(9) 0.0858(9) 0.6278(5) 0.087(5) Uani 1 1 d . . . H88A H -0.1653 0.0269 0.6270 0.131 Uiso 1 1 calc R . . H88B H -0.1583 0.1416 0.6397 0.131 Uiso 1 1 calc R . . H88C H -0.0836 0.0745 0.6492 0.131 Uiso 1 1 calc R . . C20 C -0.2042(7) 0.1268(12) 0.5427(6) 0.116(6) Uani 1 1 d . . . H98A H -0.1989 0.1590 0.5130 0.174 Uiso 1 1 calc R . . H98B H -0.2336 0.1690 0.5593 0.174 Uiso 1 1 calc R . . H98C H -0.2305 0.0639 0.5347 0.174 Uiso 1 1 calc R . . C21 C -0.1125(7) -0.1661(11) 0.4586(4) 0.083(5) Uani 1 1 d . . . H73A H -0.1420 -0.2191 0.4686 0.125 Uiso 1 1 calc R . . H73B H -0.0742 -0.1943 0.4435 0.125 Uiso 1 1 calc R . . H73C H -0.1467 -0.1234 0.4355 0.125 Uiso 1 1 calc R . . C30 C 0.0842(11) -0.0128(12) 0.4250(5) 0.100(6) Uani 1 1 d . . . H17A H 0.0866 -0.0195 0.4595 0.150 Uiso 1 1 calc R . . H17B H 0.1360 -0.0095 0.4202 0.150 Uiso 1 1 calc R . . H17C H 0.0577 -0.0696 0.4077 0.150 Uiso 1 1 calc R . . C31 C -0.0316(13) 0.0752(13) 0.4158(6) 0.130(8) Uani 1 1 d . . . H18A H -0.0270 0.0596 0.4498 0.195 Uiso 1 1 calc R . . H18B H -0.0621 0.0246 0.3956 0.195 Uiso 1 1 calc R . . H18C H -0.0563 0.1393 0.4083 0.195 Uiso 1 1 calc R . . C32 C 0.0741(9) 0.1708(10) 0.4329(4) 0.094(4) Uani 1 1 d U . . H20G H 0.0326 0.2194 0.4300 0.113 Uiso 1 1 calc R . . H20H H 0.0934 0.1554 0.4676 0.113 Uiso 1 1 calc R . . C33 C 0.1349(8) 0.2142(10) 0.4151(5) 0.081(4) Uani 1 1 d U . . H18G H 0.1449 0.2809 0.4290 0.097 Uiso 1 1 calc R . . H18H H 0.1815 0.1748 0.4272 0.097 Uiso 1 1 calc R . . C34 C 0.0789(10) 0.3120(10) 0.3470(7) 0.120(6) Uani 1 1 d . . . H17M H 0.1022 0.3674 0.3671 0.180 Uiso 1 1 calc R . . H17N H 0.0262 0.3039 0.3495 0.180 Uiso 1 1 calc R . . H17O H 0.0796 0.3247 0.3134 0.180 Uiso 1 1 calc R . . C35 C 0.1941(9) 0.2284(14) 0.3493(6) 0.102(6) Uani 1 1 d . . . H17J H 0.2197 0.2900 0.3612 0.153 Uiso 1 1 calc R . . H17K H 0.1843 0.2266 0.3140 0.153 Uiso 1 1 calc R . . H17L H 0.2265 0.1728 0.3629 0.153 Uiso 1 1 calc R . . C36 C -0.0093(7) -0.0065(8) 0.2428(4) 0.045(3) Uani 1 1 d . . . C37 C -0.0852(7) 0.0175(9) 0.2124(3) 0.047(3) Uani 1 1 d . . . C38 C -0.1109(7) -0.0429(10) 0.1716(3) 0.058(4) Uani 1 1 d . . . H100 H -0.1600 -0.0294 0.1518 0.070 Uiso 1 1 calc R . . C39 C -0.0711(7) -0.1199(10) 0.1581(4) 0.057(3) Uani 1 1 d . . . C40 C 0.0020(7) -0.1350(10) 0.1876(3) 0.051(3) Uani 1 1 d . . . H20 H 0.0319 -0.1861 0.1789 0.061 Uiso 1 1 calc R . . C41 C 0.0332(6) -0.0812(8) 0.2281(4) 0.037(3) Uani 1 1 d . . . C42 C 0.1153(7) -0.0972(9) 0.2588(4) 0.046(3) Uani 1 1 d . . . C43 C 0.1529(8) -0.1723(13) 0.2352(5) 0.088(5) Uani 1 1 d . . . H56A H 0.2010 -0.1919 0.2571 0.131 Uiso 1 1 calc R . . H56B H 0.1629 -0.1450 0.2056 0.131 Uiso 1 1 calc R . . H56C H 0.1197 -0.2298 0.2272 0.131 Uiso 1 1 calc R . . C44 C 0.1619(6) -0.0025(11) 0.2581(5) 0.075(4) Uani 1 1 d . . . H10D H 0.2133 -0.0114 0.2785 0.113 Uiso 1 1 calc R . . H10E H 0.1371 0.0525 0.2704 0.113 Uiso 1 1 calc R . . H10F H 0.1649 0.0116 0.2250 0.113 Uiso 1 1 calc R . . C45 C 0.1157(7) -0.1321(10) 0.3095(4) 0.064(4) Uani 1 1 d . . . H85A H 0.0913 -0.1967 0.3078 0.096 Uiso 1 1 calc R . . H85B H 0.0877 -0.0851 0.3247 0.096 Uiso 1 1 calc R . . H85C H 0.1683 -0.1369 0.3287 0.096 Uiso 1 1 calc R . . C46 C -0.1270(7) 0.1064(9) 0.2230(3) 0.052(3) Uani 1 1 d . . . C47 C -0.0809(8) 0.2020(9) 0.2281(4) 0.066(4) Uani 1 1 d . . . H62A H -0.0298 0.1902 0.2485 0.099 Uiso 1 1 calc R . . H62B H -0.1064 0.2525 0.2430 0.099 Uiso 1 1 calc R . . H62C H -0.0770 0.2243 0.1962 0.099 Uiso 1 1 calc R . . C48 C -0.1515(7) 0.0937(10) 0.2719(3) 0.055(3) Uani 1 1 d . . . H90A H -0.1897 0.0415 0.2684 0.082 Uiso 1 1 calc R . . H90B H -0.1732 0.1555 0.2801 0.082 Uiso 1 1 calc R . . H90C H -0.1070 0.0763 0.2975 0.082 Uiso 1 1 calc R . . C49 C -0.2021(7) 0.1226(11) 0.1847(4) 0.074(4) Uani 1 1 d . . . H11A H -0.1909 0.1350 0.1533 0.112 Uiso 1 1 calc R . . H11B H -0.2290 0.1793 0.1938 0.112 Uiso 1 1 calc R . . H11C H -0.2340 0.0639 0.1826 0.112 Uiso 1 1 calc R . . C50 C -0.1043(7) -0.1831(10) 0.1143(4) 0.071(4) Uani 1 1 d . . . H67A H -0.1496 -0.2172 0.1191 0.107 Uiso 1 1 calc R . . H67B H -0.0665 -0.2316 0.1101 0.107 Uiso 1 1 calc R . . H67C H -0.1183 -0.1414 0.0856 0.107 Uiso 1 1 calc R . . C60 C 0.5913(9) 0.3245(11) 0.4288(5) 0.089(5) Uani 1 1 d . . . H14 H 0.6107 0.3335 0.4636 0.134 Uiso 1 1 calc R . . H15 H 0.5467 0.3665 0.4172 0.134 Uiso 1 1 calc R . . H16 H 0.6309 0.3424 0.4123 0.134 Uiso 1 1 calc R . . C61 C 0.5000(8) 0.2092(12) 0.4344(4) 0.078(4) Uani 1 1 d . . . H19J H 0.4827 0.1412 0.4282 0.117 Uiso 1 1 calc R . . H19K H 0.4609 0.2540 0.4165 0.117 Uiso 1 1 calc R . . H19L H 0.5093 0.2232 0.4690 0.117 Uiso 1 1 calc R . . C62 C 0.6278(8) 0.1576(10) 0.4438(4) 0.093(4) Uani 1 1 d U . . H36A H 0.6738 0.1978 0.4564 0.112 Uiso 1 1 calc R . . H36B H 0.6110 0.1333 0.4722 0.112 Uiso 1 1 calc R . . C63 C 0.6499(9) 0.0796(11) 0.4229(4) 0.092(5) Uani 1 1 d U . . H20A H 0.6228 0.0220 0.4318 0.111 Uiso 1 1 calc R . . H20B H 0.7047 0.0697 0.4377 0.111 Uiso 1 1 calc R . . C64 C 0.6055(10) -0.0169(11) 0.3528(6) 0.111(6) Uani 1 1 d . . . H19D H 0.6427 -0.0698 0.3626 0.167 Uiso 1 1 calc R . . H19E H 0.5891 -0.0148 0.3176 0.167 Uiso 1 1 calc R . . H19F H 0.5614 -0.0290 0.3663 0.167 Uiso 1 1 calc R . . C65 C 0.7106(8) 0.0873(13) 0.3559(6) 0.094(5) Uani 1 1 d . . . H19M H 0.7313 0.1533 0.3643 0.142 Uiso 1 1 calc R . . H19N H 0.7011 0.0778 0.3209 0.142 Uiso 1 1 calc R . . H19O H 0.7472 0.0381 0.3724 0.142 Uiso 1 1 calc R . . C66 C 0.4978(7) 0.2959(8) 0.2550(3) 0.039(3) Uani 1 1 d . . . C67 C 0.4204(6) 0.2770(8) 0.2321(3) 0.036(3) Uani 1 1 d . . . C68 C 0.3870(6) 0.3299(8) 0.1923(3) 0.038(3) Uani 1 1 d . . . H28 H 0.3350 0.3174 0.1775 0.046 Uiso 1 1 calc R . . C69 C 0.4245(7) 0.4013(7) 0.1719(4) 0.041(3) Uani 1 1 d . . . C70 C 0.4992(7) 0.4184(7) 0.1946(4) 0.040(3) Uani 1 1 d . . . H24 H 0.5259 0.4666 0.1811 0.048 Uiso 1 1 calc R . . C71 C 0.5381(7) 0.3703(8) 0.2356(4) 0.040(3) Uani 1 1 d . . . C72 C 0.6227(7) 0.3943(8) 0.2580(4) 0.046(3) Uani 1 1 d . . . C73 C 0.6569(8) 0.4737(11) 0.2303(5) 0.071(4) Uani 1 1 d . . . H13A H 0.6483 0.4548 0.1964 0.106 Uiso 1 1 calc R . . H13B H 0.7117 0.4794 0.2445 0.106 Uiso 1 1 calc R . . H13C H 0.6324 0.5371 0.2327 0.106 Uiso 1 1 calc R . . C74 C 0.6327(8) 0.4286(11) 0.3100(4) 0.069(4) Uani 1 1 d . . . H59A H 0.6160 0.4970 0.3103 0.104 Uiso 1 1 calc R . . H59B H 0.6864 0.4236 0.3271 0.104 Uiso 1 1 calc R . . H59C H 0.6020 0.3871 0.3261 0.104 Uiso 1 1 calc R . . C75 C 0.6688(7) 0.2993(10) 0.2565(5) 0.064(4) Uani 1 1 d . . . H84A H 0.6475 0.2459 0.2722 0.097 Uiso 1 1 calc R . . H84B H 0.7220 0.3102 0.2736 0.097 Uiso 1 1 calc R . . H84C H 0.6663 0.2816 0.2230 0.097 Uiso 1 1 calc R . . C76 C 0.3750(7) 0.1964(7) 0.2518(3) 0.039(3) Uani 1 1 d . . . C77 C 0.3683(8) 0.2255(9) 0.3021(4) 0.065(4) Uani 1 1 d . . . H11D H 0.4190 0.2403 0.3223 0.098 Uiso 1 1 calc R . . H11E H 0.3458 0.1713 0.3165 0.098 Uiso 1 1 calc R . . H11F H 0.3359 0.2839 0.3000 0.098 Uiso 1 1 calc R . . C78 C 0.4135(8) 0.0980(8) 0.2536(4) 0.059(3) Uani 1 1 d . . . H48A H 0.4204 0.0815 0.2216 0.088 Uiso 1 1 calc R . . H48B H 0.3821 0.0477 0.2639 0.088 Uiso 1 1 calc R . . H48C H 0.4633 0.1008 0.2766 0.088 Uiso 1 1 calc R . . C79 C 0.2958(7) 0.1851(10) 0.2207(5) 0.069(4) Uani 1 1 d . . . H75A H 0.2661 0.2441 0.2234 0.104 Uiso 1 1 calc R . . H75B H 0.2715 0.1277 0.2314 0.104 Uiso 1 1 calc R . . H75C H 0.2981 0.1761 0.1871 0.104 Uiso 1 1 calc R . . C80 C 0.3857(8) 0.4577(9) 0.1274(4) 0.060(3) Uani 1 1 d . . . H94A H 0.3771 0.4140 0.0993 0.091 Uiso 1 1 calc R . . H94B H 0.4180 0.5128 0.1226 0.091 Uiso 1 1 calc R . . H94C H 0.3368 0.4828 0.1312 0.091 Uiso 1 1 calc R . . C90 C 0.2985(9) 0.5857(13) 0.3108(6) 0.094(5) Uani 1 1 d . . . H19S H 0.2662 0.5355 0.2915 0.142 Uiso 1 1 calc R . . H19T H 0.2713 0.6485 0.3073 0.142 Uiso 1 1 calc R . . H19U H 0.3113 0.5659 0.3448 0.142 Uiso 1 1 calc R . . C91 C 0.4122(9) 0.5067(10) 0.3042(5) 0.088(5) Uani 1 1 d . . . H19P H 0.3825 0.4523 0.2867 0.131 Uiso 1 1 calc R . . H19Q H 0.4234 0.4934 0.3389 0.131 Uiso 1 1 calc R . . H19R H 0.4600 0.5133 0.2941 0.131 Uiso 1 1 calc R . . C92 C 0.3503(8) 0.6190(11) 0.2408(4) 0.081(4) Uani 1 1 d U . . H15M H 0.3317 0.5581 0.2228 0.097 Uiso 1 1 calc R . . H15N H 0.3084 0.6675 0.2337 0.097 Uiso 1 1 calc R . . C93 C 0.4123(10) 0.6563(11) 0.2241(4) 0.092(4) Uani 1 1 d U . . H15D H 0.3930 0.6798 0.1906 0.111 Uiso 1 1 calc R . . H15E H 0.4482 0.6018 0.2233 0.111 Uiso 1 1 calc R . . C94 C 0.5355(11) 0.7424(11) 0.2464(6) 0.119(7) Uani 1 1 d . . . H19G H 0.5344 0.7482 0.2121 0.178 Uiso 1 1 calc R . . H19H H 0.5635 0.6829 0.2595 0.178 Uiso 1 1 calc R . . H19I H 0.5609 0.8000 0.2636 0.178 Uiso 1 1 calc R . . C95 C 0.4181(10) 0.8272(9) 0.2367(5) 0.087(5) Uani 1 1 d . . . H17 H 0.4171 0.8368 0.2026 0.130 Uiso 1 1 calc R . . H20E H 0.4465 0.8809 0.2557 0.130 Uiso 1 1 calc R . . H20F H 0.3659 0.8266 0.2408 0.130 Uiso 1 1 calc R . . C96 C 0.5112(7) 0.8009(8) 0.4188(3) 0.041(3) Uani 1 1 d . . . C97 C 0.5861(6) 0.7800(9) 0.4485(4) 0.044(3) Uani 1 1 d . . . C98 C 0.6135(7) 0.8350(10) 0.4899(4) 0.058(3) Uani 1 1 d . . . H209 H 0.6629 0.8196 0.5087 0.070 Uiso 1 1 calc R . . C99 C 0.5761(8) 0.9084(11) 0.5058(4) 0.061(4) Uani 1 1 d . . . C100 C 0.5010(7) 0.9269(9) 0.4780(4) 0.060(4) Uani 1 1 d . . . H140 H 0.4716 0.9764 0.4884 0.072 Uiso 1 1 calc R . . C101 C 0.4689(7) 0.8738(9) 0.4354(4) 0.046(3) Uani 1 1 d . . . C102 C 0.3840(7) 0.8950(10) 0.4081(4) 0.056(4) Uani 1 1 d . . . C103 C 0.3452(7) 0.9774(11) 0.4325(5) 0.072(4) Uani 1 1 d . . . H14G H 0.3508 0.9615 0.4666 0.108 Uiso 1 1 calc R . . H14H H 0.2910 0.9812 0.4164 0.108 Uiso 1 1 calc R . . H14I H 0.3695 1.0407 0.4297 0.108 Uiso 1 1 calc R . . C104 C 0.3385(8) 0.8033(11) 0.4032(5) 0.076(4) Uani 1 1 d . . . H14J H 0.3299 0.7852 0.4346 0.115 Uiso 1 1 calc R . . H14K H 0.3661 0.7504 0.3915 0.115 Uiso 1 1 calc R . . H14L H 0.2895 0.8139 0.3802 0.115 Uiso 1 1 calc R . . C105 C 0.3836(8) 0.9361(10) 0.3566(4) 0.067(4) Uani 1 1 d . . . H14M H 0.3311 0.9420 0.3376 0.101 Uiso 1 1 calc R . . H14N H 0.4116 0.8910 0.3404 0.101 Uiso 1 1 calc R . . H14O H 0.4080 1.0008 0.3598 0.101 Uiso 1 1 calc R . . C106 C 0.6289(7) 0.6957(9) 0.4344(5) 0.069(4) Uani 1 1 d . . . C107 C 0.5818(9) 0.6015(11) 0.4309(6) 0.114(6) Uani 1 1 d . . . H1 H 0.5655 0.5921 0.4609 0.171 Uiso 1 1 calc R . . H2 H 0.6128 0.5453 0.4258 0.171 Uiso 1 1 calc R . . H15F H 0.5371 0.6067 0.4038 0.171 Uiso 1 1 calc R . . C108 C 0.6496(9) 0.7169(10) 0.3876(5) 0.091(5) Uani 1 1 d . . . H15G H 0.6031 0.7264 0.3621 0.137 Uiso 1 1 calc R . . H15H H 0.6785 0.6616 0.3791 0.137 Uiso 1 1 calc R . . H15I H 0.6806 0.7767 0.3909 0.137 Uiso 1 1 calc R . . C109 C 0.7031(7) 0.6747(11) 0.4752(5) 0.100(5) Uani 1 1 d . . . H15J H 0.7351 0.7336 0.4806 0.150 Uiso 1 1 calc R . . H15K H 0.7313 0.6202 0.4654 0.150 Uiso 1 1 calc R . . H15L H 0.6888 0.6572 0.5052 0.150 Uiso 1 1 calc R . . C110 C 0.6080(8) 0.9643(11) 0.5518(4) 0.088(5) Uani 1 1 d . . . H14P H 0.6541 0.9314 0.5701 0.131 Uiso 1 1 calc R . . H14Q H 0.5702 0.9664 0.5711 0.131 Uiso 1 1 calc R . . H14R H 0.6206 1.0314 0.5440 0.131 Uiso 1 1 calc R . . C120 C 0.4116(10) 0.5048(9) -0.0025(4) 0.084(4) Uani 1 1 d . . . H9 H 0.3757 0.4510 -0.0135 0.126 Uiso 1 1 calc R . . H10 H 0.4212 0.5109 0.0327 0.126 Uiso 1 1 calc R . . H19C H 0.4595 0.4910 -0.0114 0.126 Uiso 1 1 calc R . . C121 C 0.3052(8) 0.6133(11) -0.0160(5) 0.080(5) Uani 1 1 d . . . H21A H 0.2852 0.6766 -0.0299 0.121 Uiso 1 1 calc R . . H21B H 0.3095 0.6142 0.0189 0.121 Uiso 1 1 calc R . . H21C H 0.2706 0.5605 -0.0308 0.121 Uiso 1 1 calc R . . C122 C 0.3738(8) 0.5896(9) -0.0768(4) 0.063(3) Uani 1 1 d U . . H19A H 0.4186 0.5536 -0.0820 0.076 Uiso 1 1 calc R . . H19B H 0.3279 0.5513 -0.0920 0.076 Uiso 1 1 calc R . . C123 C 0.3699(6) 0.6848(7) -0.0999(3) 0.055(3) Uani 1 1 d U . . H20C H 0.3215 0.7172 -0.0987 0.066 Uiso 1 1 calc R . . H20D H 0.3702 0.6756 -0.1342 0.066 Uiso 1 1 calc R . . C124 C 0.4171(8) 0.8514(9) -0.0916(4) 0.058(3) Uani 1 1 d . . . H18P H 0.4044 0.8541 -0.1269 0.087 Uiso 1 1 calc R . . H18Q H 0.4607 0.8943 -0.0787 0.087 Uiso 1 1 calc R . . H18R H 0.3734 0.8734 -0.0798 0.087 Uiso 1 1 calc R . . C125 C 0.5074(11) 0.7272(12) -0.0873(6) 0.113(6) Uani 1 1 d . . . H18J H 0.5017 0.7321 -0.1222 0.169 Uiso 1 1 calc R . . H18K H 0.5222 0.6600 -0.0766 0.169 Uiso 1 1 calc R . . H18L H 0.5467 0.7732 -0.0707 0.169 Uiso 1 1 calc R . . C126 C 0.5075(6) 0.8352(7) 0.0886(3) 0.032(3) Uani 1 1 d . . . C127 C 0.4643(7) 0.9130(8) 0.1032(4) 0.041(3) Uani 1 1 d . . . C128 C 0.4999(7) 0.9663(8) 0.1447(4) 0.043(3) Uani 1 1 d . . . H11 H 0.4714 1.0164 0.1555 0.052 Uiso 1 1 calc R . . C129 C 0.5728(8) 0.9505(8) 0.1705(3) 0.045(3) Uani 1 1 d . . . C130 C 0.6121(6) 0.8722(8) 0.1555(4) 0.042(3) Uani 1 1 d . . . H26 H 0.6624 0.8583 0.1733 0.050 Uiso 1 1 calc R . . C131 C 0.5807(6) 0.8151(7) 0.1163(3) 0.030(2) Uani 1 1 d . . . C132 C 0.6261(7) 0.7242(8) 0.1025(4) 0.057(3) Uani 1 1 d . . . C133 C 0.6994(7) 0.7078(9) 0.1408(5) 0.074(4) Uani 1 1 d . . . H69A H 0.7246 0.6484 0.1332 0.111 Uiso 1 1 calc R . . H69B H 0.6876 0.7001 0.1724 0.111 Uiso 1 1 calc R . . H69C H 0.7331 0.7645 0.1417 0.111 Uiso 1 1 calc R . . C134 C 0.5778(8) 0.6306(7) 0.1048(5) 0.072(4) Uani 1 1 d . . . H81A H 0.5281 0.6371 0.0820 0.108 Uiso 1 1 calc R . . H81B H 0.5707 0.6228 0.1375 0.108 Uiso 1 1 calc R . . H81C H 0.6042 0.5728 0.0963 0.108 Uiso 1 1 calc R . . C135 C 0.6438(8) 0.7410(9) 0.0538(5) 0.068(4) Uani 1 1 d . . . H40A H 0.6639 0.6803 0.0432 0.102 Uiso 1 1 calc R . . H40B H 0.6819 0.7933 0.0566 0.102 Uiso 1 1 calc R . . H40C H 0.5973 0.7603 0.0302 0.102 Uiso 1 1 calc R . . C136 C 0.3811(7) 0.9304(8) 0.0776(4) 0.039(3) Uani 1 1 d . . . C137 C 0.3347(7) 0.8342(8) 0.0771(4) 0.057(3) Uani 1 1 d . . . H17P H 0.3556 0.7828 0.0600 0.086 Uiso 1 1 calc R . . H17Q H 0.2814 0.8461 0.0607 0.086 Uiso 1 1 calc R . . H17R H 0.3378 0.8131 0.1103 0.086 Uiso 1 1 calc R . . C138 C 0.3753(8) 0.9634(9) 0.0260(4) 0.054(3) Uani 1 1 d . . . H18M H 0.3974 0.9130 0.0090 0.081 Uiso 1 1 calc R . . H18N H 0.4030 1.0253 0.0261 0.081 Uiso 1 1 calc R . . H18O H 0.3217 0.9731 0.0096 0.081 Uiso 1 1 calc R . . C139 C 0.3424(7) 1.0104(9) 0.1016(5) 0.058(3) Uani 1 1 d . . . H12 H 0.2898 1.0193 0.0830 0.087 Uiso 1 1 calc R . . H13 H 0.3702 1.0724 0.1024 0.087 Uiso 1 1 calc R . . H18I H 0.3426 0.9902 0.1345 0.087 Uiso 1 1 calc R . . C140 C 0.6092(8) 1.0124(11) 0.2130(4) 0.076(4) Uani 1 1 d . . . H10A H 0.6082 1.0814 0.2032 0.114 Uiso 1 1 calc R . . H10B H 0.6620 0.9913 0.2255 0.114 Uiso 1 1 calc R . . H10C H 0.5812 1.0049 0.2382 0.114 Uiso 1 1 calc R . . C150 C 0.7898(8) 0.7459(10) -0.0256(5) 0.074(4) Uani 1 1 d . . . H16D H 0.8033 0.7476 0.0097 0.112 Uiso 1 1 calc R . . H16E H 0.7584 0.6878 -0.0367 0.112 Uiso 1 1 calc R . . H16F H 0.7611 0.8053 -0.0381 0.112 Uiso 1 1 calc R . . C151 C 0.9007(10) 0.8313(10) -0.0325(5) 0.098(5) Uani 1 1 d . . . H16A H 0.8733 0.8840 -0.0528 0.147 Uiso 1 1 calc R . . H16B H 0.9512 0.8235 -0.0388 0.147 Uiso 1 1 calc R . . H16C H 0.9061 0.8480 0.0015 0.147 Uiso 1 1 calc R . . C152 C 0.8355(8) 0.7185(11) -0.0954(4) 0.079(4) Uani 1 1 d U . . H16J H 0.8111 0.7770 -0.1132 0.095 Uiso 1 1 calc R . . H16K H 0.7977 0.6645 -0.1007 0.095 Uiso 1 1 calc R . . C153 C 0.9033(8) 0.6884(8) -0.1143(4) 0.073(3) Uani 1 1 d U . . H16L H 0.8862 0.6713 -0.1489 0.087 Uiso 1 1 calc R . . H16M H 0.9392 0.7442 -0.1112 0.087 Uiso 1 1 calc R . . C154 C 1.0166(11) 0.5960(14) -0.0967(6) 0.122(7) Uani 1 1 d . . . H17D H 1.0480 0.5501 -0.0739 0.183 Uiso 1 1 calc R . . H17E H 1.0407 0.6610 -0.0931 0.183 Uiso 1 1 calc R . . H17F H 1.0118 0.5722 -0.1297 0.183 Uiso 1 1 calc R . . C155 C 0.9024(11) 0.5078(9) -0.0990(5) 0.100(6) Uani 1 1 d . . . H16G H 0.8990 0.4915 -0.1328 0.150 Uiso 1 1 calc R . . H16H H 0.8511 0.5130 -0.0936 0.150 Uiso 1 1 calc R . . H16I H 0.9307 0.4562 -0.0783 0.150 Uiso 1 1 calc R . . C156 C 1.0039(7) 0.5330(7) 0.0791(4) 0.038(3) Uani 1 1 d . . . C157 C 1.0803(7) 0.5560(7) 0.1047(4) 0.043(3) Uani 1 1 d . . . C158 C 1.1126(7) 0.5047(7) 0.1481(4) 0.048(3) Uani 1 1 d . . . H51 H 1.1624 0.5221 0.1657 0.058 Uiso 1 1 calc R . . C159 C 1.0747(7) 0.4302(7) 0.1660(4) 0.038(3) Uani 1 1 d . . . C160 C 1.0009(7) 0.4100(7) 0.1418(4) 0.039(3) Uani 1 1 d . . . H33 H 0.9738 0.3608 0.1544 0.047 Uiso 1 1 calc R . . C161 C 0.9635(7) 0.4591(8) 0.0992(4) 0.036(3) Uani 1 1 d . . . C162 C 0.8822(7) 0.4373(8) 0.0740(4) 0.045(3) Uani 1 1 d . . . C163 C 0.8734(8) 0.3972(8) 0.0238(4) 0.057(3) Uani 1 1 d . . . H35A H 0.8961 0.3315 0.0256 0.086 Uiso 1 1 calc R . . H35B H 0.8992 0.4409 0.0055 0.086 Uiso 1 1 calc R . . H35C H 0.8193 0.3932 0.0076 0.086 Uiso 1 1 calc R . . C164 C 0.8318(7) 0.5300(8) 0.0739(4) 0.051(3) Uani 1 1 d . . . H93A H 0.8506 0.5837 0.0570 0.077 Uiso 1 1 calc R . . H93B H 0.8341 0.5500 0.1071 0.077 Uiso 1 1 calc R . . H93C H 0.7791 0.5149 0.0574 0.077 Uiso 1 1 calc R . . C165 C 0.8466(7) 0.3596(8) 0.1008(4) 0.050(3) Uani 1 1 d . . . H25A H 0.7953 0.3438 0.0819 0.075 Uiso 1 1 calc R . . H25B H 0.8439 0.3854 0.1324 0.075 Uiso 1 1 calc R . . H25C H 0.8780 0.3002 0.1052 0.075 Uiso 1 1 calc R . . C166 C 1.1291(8) 0.6344(9) 0.0882(5) 0.060(4) Uani 1 1 d . . . C167 C 1.0854(7) 0.7345(7) 0.0844(4) 0.049(3) Uani 1 1 d . . . H60A H 1.0785 0.7530 0.1163 0.074 Uiso 1 1 calc R . . H60B H 1.0356 0.7277 0.0618 0.074 Uiso 1 1 calc R . . H60C H 1.1148 0.7856 0.0728 0.074 Uiso 1 1 calc R . . C168 C 1.1393(9) 0.6060(9) 0.0374(5) 0.087(5) Uani 1 1 d . . . H92A H 1.0896 0.5907 0.0161 0.131 Uiso 1 1 calc R . . H92B H 1.1725 0.5483 0.0401 0.131 Uiso 1 1 calc R . . H92C H 1.1623 0.6611 0.0239 0.131 Uiso 1 1 calc R . . C169 C 1.2053(8) 0.6507(9) 0.1213(6) 0.096(5) Uani 1 1 d . . . H43A H 1.2329 0.7007 0.1076 0.145 Uiso 1 1 calc R . . H43B H 1.2341 0.5890 0.1253 0.145 Uiso 1 1 calc R . . H43C H 1.1990 0.6729 0.1527 0.145 Uiso 1 1 calc R . . C170 C 1.1117(8) 0.3761(9) 0.2120(4) 0.065(4) Uani 1 1 d . . . H64A H 1.0912 0.4009 0.2385 0.097 Uiso 1 1 calc R . . H64B H 1.1668 0.3868 0.2196 0.097 Uiso 1 1 calc R . . H64C H 1.1010 0.3056 0.2077 0.097 Uiso 1 1 calc R . . Li1 Li 0.0607(13) 0.1171(18) 0.6747(8) 0.073(7) Uani 1 1 d . . . Li2 Li 0.0506(12) 0.1047(14) 0.3376(6) 0.052(5) Uani 1 1 d . . . Li3 Li 0.5661(12) 0.1916(12) 0.3481(5) 0.043(5) Uani 1 1 d . . . Li4 Li 0.4443(14) 0.7075(15) 0.3213(6) 0.060(6) Uani 1 1 d . . . Li5 Li 0.4455(11) 0.7230(12) -0.0041(6) 0.040(4) Uani 1 1 d . . . Li6 Li 0.9368(12) 0.6311(14) -0.0152(6) 0.051(5) Uani 1 1 d U . . 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 0.053(5) 0.083(5) 0.037(4) 0.003(4) 0.004(4) 0.012(4) O2 0.048(5) 0.062(5) 0.042(4) 0.002(4) -0.002(4) -0.007(4) O3 0.063(5) 0.061(5) 0.034(4) 0.003(3) 0.005(4) -0.005(4) O4 0.061(5) 0.067(5) 0.040(4) 0.002(3) 0.020(4) 0.014(4) O5 0.059(5) 0.033(4) 0.031(4) -0.008(3) 0.011(3) 0.000(3) O6 0.081(6) 0.044(4) 0.034(4) 0.009(3) 0.020(4) 0.009(4) N1 0.055(7) 0.086(8) 0.036(5) 0.017(5) 0.009(5) 0.001(6) N2 0.081(8) 0.056(6) 0.066(6) 0.016(5) 0.038(6) 0.022(6) N3 0.172(13) 0.043(6) 0.039(5) 0.008(4) 0.008(7) -0.030(7) N4 0.070(8) 0.046(6) 0.092(7) -0.018(5) 0.036(6) -0.011(5) N5 0.085(8) 0.058(6) 0.035(5) 0.002(4) 0.037(5) 0.010(5) N6 0.046(6) 0.081(7) 0.042(5) -0.013(5) 0.009(5) 0.009(6) N7 0.080(8) 0.045(5) 0.049(5) 0.016(4) 0.034(5) 0.032(5) N8 0.138(10) 0.027(5) 0.043(5) -0.006(4) 0.051(6) -0.005(6) N9 0.069(7) 0.055(6) 0.021(4) -0.003(4) 0.018(4) -0.001(5) N10 0.082(7) 0.029(5) 0.042(5) -0.007(4) 0.012(5) -0.015(5) N11 0.050(6) 0.043(5) 0.032(4) 0.008(4) -0.003(4) -0.007(4) N12 0.105(9) 0.045(6) 0.038(5) 0.007(4) 0.035(5) -0.002(6) C1 0.123(14) 0.079(10) 0.060(8) 0.010(7) 0.011(8) -0.001(9) C2 0.092(12) 0.065(8) 0.072(8) 0.028(6) 0.021(8) 0.007(8) C3 0.121(8) 0.095(7) 0.062(6) 0.018(5) 0.006(6) 0.008(6) C4 0.101(7) 0.069(6) 0.051(5) 0.001(5) 0.019(5) -0.006(5) C5 0.087(12) 0.088(10) 0.136(14) 0.002(9) 0.050(11) 0.008(9) C6 0.150(14) 0.071(9) 0.087(9) 0.033(7) 0.076(10) 0.006(9) C7 0.026(6) 0.081(8) 0.029(5) 0.019(5) 0.012(5) 0.016(6) C8 0.049(8) 0.075(8) 0.049(7) 0.024(6) 0.025(6) 0.005(6) C9 0.020(7) 0.108(10) 0.044(6) 0.037(7) -0.001(5) 0.005(6) C10 0.031(7) 0.092(9) 0.037(6) 0.011(5) 0.016(5) -0.014(6) C11 0.025(6) 0.079(8) 0.036(6) 0.009(5) 0.014(5) 0.012(5) C12 0.021(6) 0.086(8) 0.026(5) 0.005(5) 0.012(5) 0.008(5) C13 0.022(7) 0.103(10) 0.045(7) -0.002(6) 0.006(6) 0.012(7) C14 0.040(8) 0.086(9) 0.063(8) 0.013(6) -0.007(6) 0.009(7) C15 0.027(7) 0.122(11) 0.046(6) 0.002(7) -0.004(5) 0.018(7) C16 0.043(9) 0.115(11) 0.077(9) 0.002(8) 0.014(7) 0.011(8) C17 0.032(7) 0.061(8) 0.099(9) 0.020(7) 0.022(7) 0.009(6) C18 0.054(8) 0.081(9) 0.097(9) 0.031(7) 0.020(7) -0.002(6) C19 0.091(11) 0.040(7) 0.151(13) -0.004(7) 0.071(10) 0.025(7) C20 0.038(9) 0.099(11) 0.192(17) 0.025(10) -0.009(9) 0.021(8) C21 0.046(8) 0.149(13) 0.048(7) -0.007(7) -0.003(6) -0.034(8) C30 0.145(17) 0.098(12) 0.058(8) 0.019(8) 0.027(10) 0.006(11) C31 0.21(2) 0.099(12) 0.112(12) 0.057(9) 0.089(14) 0.058(12) C32 0.142(8) 0.082(6) 0.059(5) -0.007(5) 0.026(6) -0.014(6) C33 0.088(7) 0.084(7) 0.071(6) -0.029(5) 0.021(5) -0.026(5) C34 0.106(12) 0.051(8) 0.197(17) 0.001(9) 0.022(11) 0.023(8) C35 0.059(11) 0.125(14) 0.126(13) -0.016(11) 0.033(10) -0.009(9) C36 0.051(8) 0.046(6) 0.032(6) 0.000(5) 0.000(5) -0.007(6) C37 0.043(7) 0.078(8) 0.025(5) 0.006(5) 0.015(5) 0.008(6) C38 0.053(8) 0.105(10) 0.015(5) -0.002(5) 0.003(5) -0.009(7) C39 0.038(7) 0.105(9) 0.032(5) -0.020(6) 0.019(5) 0.000(6) C40 0.033(7) 0.089(8) 0.026(5) 0.009(5) -0.001(5) -0.001(6) C41 0.027(6) 0.054(6) 0.032(5) 0.001(4) 0.009(5) 0.000(5) C42 0.036(7) 0.068(7) 0.038(6) 0.002(5) 0.015(5) 0.001(6) C43 0.042(9) 0.135(13) 0.078(9) 0.011(9) -0.001(7) -0.011(8) C44 0.014(7) 0.128(12) 0.073(8) 0.027(8) -0.012(6) -0.011(7) C45 0.050(8) 0.083(9) 0.056(7) 0.016(6) 0.006(6) -0.004(7) C46 0.060(8) 0.074(7) 0.024(4) 0.012(5) 0.016(5) 0.008(6) C47 0.057(9) 0.080(8) 0.064(7) 0.035(6) 0.017(6) -0.014(7) C48 0.060(8) 0.073(7) 0.031(5) 0.005(5) 0.010(5) 0.000(6) C49 0.070(9) 0.119(10) 0.034(5) 0.015(6) 0.011(5) 0.033(8) C50 0.061(8) 0.107(10) 0.047(6) -0.033(6) 0.013(6) -0.034(7) C60 0.087(11) 0.117(12) 0.084(10) -0.056(8) 0.060(9) -0.061(9) C61 0.081(10) 0.123(11) 0.036(5) 0.012(6) 0.022(6) -0.026(8) C62 0.104(7) 0.111(7) 0.055(5) -0.022(5) 0.002(5) 0.046(6) C63 0.115(8) 0.097(7) 0.063(6) -0.003(5) 0.019(5) 0.035(6) C64 0.119(14) 0.069(9) 0.124(12) 0.035(8) -0.014(9) -0.036(9) C65 0.060(10) 0.137(14) 0.085(10) 0.027(9) 0.016(8) -0.012(9) C66 0.052(8) 0.042(6) 0.025(5) -0.001(5) 0.011(5) 0.015(5) C67 0.025(6) 0.058(6) 0.022(5) -0.007(4) -0.001(4) 0.001(5) C68 0.038(7) 0.055(6) 0.027(5) 0.001(4) 0.016(4) 0.005(5) C69 0.049(8) 0.043(6) 0.027(5) 0.003(4) 0.002(5) 0.003(5) C70 0.054(8) 0.039(6) 0.032(5) -0.007(4) 0.022(6) -0.013(5) C71 0.043(8) 0.049(6) 0.030(5) -0.009(5) 0.010(5) 0.004(6) C72 0.029(7) 0.053(7) 0.051(7) -0.006(5) -0.001(6) 0.007(6) C73 0.045(9) 0.087(10) 0.084(9) -0.022(8) 0.023(7) -0.022(7) C74 0.049(8) 0.102(10) 0.052(7) -0.034(7) 0.005(6) 0.016(7) C75 0.044(8) 0.085(9) 0.064(8) -0.014(7) 0.011(6) 0.014(7) C76 0.051(7) 0.037(6) 0.027(4) 0.006(4) 0.005(5) -0.005(5) C77 0.109(11) 0.047(7) 0.058(6) -0.008(5) 0.054(7) 0.013(7) C78 0.098(10) 0.046(6) 0.035(5) -0.012(4) 0.021(6) -0.003(6) C79 0.058(9) 0.069(8) 0.086(8) 0.001(6) 0.027(7) -0.016(7) C80 0.083(10) 0.071(7) 0.028(5) 0.004(5) 0.016(6) -0.008(6) C90 0.077(11) 0.120(13) 0.096(10) -0.010(9) 0.041(9) 0.013(10) C91 0.120(12) 0.056(8) 0.106(10) 0.024(7) 0.066(9) 0.013(8) C92 0.097(7) 0.088(7) 0.054(6) 0.007(5) 0.013(5) 0.015(6) C93 0.150(8) 0.078(7) 0.056(6) 0.012(5) 0.039(6) -0.008(6) C94 0.208(19) 0.056(8) 0.138(13) -0.017(8) 0.130(14) -0.022(10) C95 0.154(15) 0.050(8) 0.070(8) 0.012(6) 0.055(9) 0.036(9) C96 0.041(7) 0.058(7) 0.027(5) 0.003(5) 0.015(5) -0.006(5) C97 0.025(6) 0.071(8) 0.036(5) 0.016(5) 0.006(5) -0.008(5) C98 0.041(7) 0.091(9) 0.047(6) 0.012(6) 0.019(6) -0.013(6) C99 0.045(8) 0.120(11) 0.022(5) 0.003(6) 0.012(5) -0.026(7) C100 0.036(8) 0.095(9) 0.053(7) 0.014(6) 0.018(6) -0.008(6) C101 0.045(8) 0.064(7) 0.030(5) 0.002(5) 0.014(5) -0.004(6) C102 0.028(7) 0.091(9) 0.047(7) 0.017(6) 0.009(6) 0.012(7) C103 0.030(8) 0.116(11) 0.072(9) -0.001(8) 0.017(7) 0.017(7) C104 0.046(8) 0.118(11) 0.065(8) -0.004(7) 0.013(7) -0.015(8) C105 0.064(9) 0.092(9) 0.044(7) 0.019(6) 0.008(6) 0.023(7) C106 0.028(7) 0.070(8) 0.109(10) 0.037(7) 0.018(7) 0.002(6) C107 0.094(12) 0.096(11) 0.132(13) 0.056(9) -0.012(10) -0.010(9) C108 0.098(11) 0.052(7) 0.151(13) 0.018(7) 0.083(10) 0.015(7) C109 0.046(9) 0.103(10) 0.143(12) 0.034(9) 0.008(8) 0.002(7) C110 0.072(9) 0.152(13) 0.034(6) -0.011(7) 0.002(6) -0.033(8) C120 0.145(13) 0.058(8) 0.045(6) 0.003(5) 0.017(7) 0.018(8) C121 0.071(10) 0.080(9) 0.106(11) -0.037(8) 0.053(9) -0.015(8) C122 0.083(6) 0.064(6) 0.040(5) -0.010(4) 0.013(5) -0.012(5) C123 0.076(6) 0.046(5) 0.036(4) -0.009(4) -0.001(4) -0.004(4) C124 0.080(10) 0.043(7) 0.053(7) 0.011(5) 0.020(7) 0.002(6) C125 0.155(16) 0.093(11) 0.123(12) 0.032(9) 0.098(12) 0.054(11) C126 0.047(7) 0.030(5) 0.017(5) -0.001(4) 0.007(5) -0.012(5) C127 0.053(8) 0.042(6) 0.029(5) 0.007(5) 0.013(5) -0.005(5) C128 0.062(8) 0.035(6) 0.038(6) -0.020(5) 0.024(6) -0.011(5) C129 0.065(9) 0.045(6) 0.022(5) 0.008(4) 0.006(5) -0.014(6) C130 0.028(6) 0.048(7) 0.043(6) 0.019(5) -0.005(5) -0.017(5) C131 0.032(6) 0.030(5) 0.027(5) 0.011(4) 0.005(4) 0.000(4) C132 0.057(9) 0.037(6) 0.075(8) 0.004(5) 0.012(6) 0.004(6) C133 0.037(8) 0.062(8) 0.118(10) 0.024(7) 0.007(7) 0.013(6) C134 0.091(10) 0.017(5) 0.104(9) -0.003(5) 0.016(8) 0.014(6) C135 0.084(10) 0.049(7) 0.089(8) 0.002(6) 0.056(7) 0.005(6) C136 0.040(7) 0.038(6) 0.038(6) -0.004(4) 0.005(5) 0.001(5) C137 0.066(9) 0.043(6) 0.066(8) 0.008(5) 0.020(7) -0.010(6) C138 0.065(9) 0.052(7) 0.037(6) 0.000(5) -0.006(6) 0.005(6) C139 0.047(8) 0.053(7) 0.078(8) -0.020(6) 0.023(6) 0.011(6) C140 0.093(11) 0.101(10) 0.028(6) -0.002(6) 0.001(6) -0.021(8) C150 0.098(12) 0.064(8) 0.063(8) 0.010(6) 0.024(8) 0.022(8) C151 0.142(14) 0.068(9) 0.074(8) 0.003(6) 0.008(8) -0.054(9) C152 0.108(7) 0.085(6) 0.041(5) 0.013(5) 0.012(5) 0.017(5) C153 0.114(7) 0.064(6) 0.045(5) 0.021(4) 0.029(5) -0.015(5) C154 0.141(16) 0.123(13) 0.123(13) -0.055(10) 0.074(12) -0.033(11) C155 0.201(18) 0.046(8) 0.051(8) -0.019(6) 0.027(9) -0.018(9) C156 0.048(8) 0.031(6) 0.039(6) -0.007(5) 0.021(6) 0.000(5) C157 0.069(9) 0.018(5) 0.048(6) 0.012(4) 0.026(6) 0.006(5) C158 0.041(7) 0.030(6) 0.072(7) -0.014(5) 0.010(6) -0.002(5) C159 0.041(7) 0.025(5) 0.043(6) 0.002(4) 0.000(5) 0.013(5) C160 0.067(9) 0.017(5) 0.036(6) 0.008(4) 0.021(6) 0.012(5) C161 0.049(8) 0.026(5) 0.038(6) -0.006(5) 0.020(6) -0.002(5) C162 0.066(9) 0.034(6) 0.029(6) -0.011(5) -0.001(6) 0.005(6) C163 0.075(9) 0.049(7) 0.048(7) -0.014(5) 0.015(7) -0.014(6) C164 0.043(8) 0.049(7) 0.056(7) -0.022(5) 0.001(6) -0.005(6) C165 0.051(8) 0.043(7) 0.053(7) -0.004(5) 0.008(6) -0.013(6) C166 0.063(9) 0.041(6) 0.090(9) 0.006(6) 0.046(8) 0.003(6) C167 0.050(7) 0.020(5) 0.078(7) 0.013(5) 0.016(6) 0.004(5) C168 0.115(11) 0.048(7) 0.141(11) 0.031(7) 0.114(10) 0.015(7) C169 0.056(9) 0.048(7) 0.186(15) 0.037(8) 0.029(9) -0.019(6) C170 0.081(10) 0.046(6) 0.060(7) 0.011(5) 0.002(7) 0.024(6) Li1 0.050(13) 0.109(17) 0.059(12) 0.007(11) 0.013(10) -0.010(12) Li2 0.065(13) 0.050(10) 0.038(9) 0.019(8) 0.006(9) -0.005(10) Li3 0.071(12) 0.036(8) 0.017(6) -0.016(6) -0.003(7) -0.008(8) Li4 0.092(15) 0.059(11) 0.035(8) 0.003(8) 0.030(9) 0.009(10) Li5 0.057(12) 0.029(8) 0.033(9) -0.004(7) 0.011(8) 0.010(8) Li6 0.064(8) 0.051(8) 0.040(7) 0.007(6) 0.016(6) -0.010(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C7 1.299(13) . ? O1 Li1 1.69(2) . ? O2 C36 1.349(12) . ? O2 Li2 1.72(2) . ? O3 C66 1.314(12) . ? O3 Li3 1.700(18) . ? O4 C96 1.301(12) . ? O4 Li4 1.74(2) . ? O5 C126 1.308(11) . ? O5 Li5 1.724(17) . ? O6 C156 1.303(12) . ? O6 Li6 1.69(2) . ? N1 C2 1.419(16) . ? N1 C3 1.425(18) . ? N1 C1 1.517(18) . ? N1 Li1 2.05(2) . ? N2 C5 1.453(17) . ? N2 C4 1.478(14) . ? N2 C6 1.517(16) . ? N2 Li1 2.08(3) . ? N3 C31 1.43(2) . ? N3 C30 1.483(19) . ? N3 C32 1.507(15) . ? N3 Li2 2.04(2) . ? N4 C33 1.436(15) . ? N4 C35 1.466(16) . ? N4 C34 1.466(18) . ? N4 Li2 2.07(2) . ? N5 C65 1.444(16) . ? N5 C64 1.455(17) . ? N5 C63 1.463(14) . ? N5 Li3 2.06(2) . ? N6 C62 1.427(16) . ? N6 C60 1.441(17) . ? N6 C61 1.455(15) . ? N6 Li3 2.052(17) . ? N7 C91 1.443(16) . ? N7 C90 1.480(16) . ? N7 C92 1.504(14) . ? N7 Li4 2.06(2) . ? N8 C95 1.422(16) . ? N8 C93 1.456(17) . ? N8 C94 1.535(19) . ? N8 Li4 2.046(19) . ? N9 C121 1.446(15) . ? N9 C122 1.460(12) . ? N9 C120 1.463(15) . ? N9 Li5 2.10(2) . ? N10 C125 1.440(17) . ? N10 C124 1.453(14) . ? N10 C123 1.527(13) . ? N10 Li5 2.053(18) . ? N11 C151 1.430(15) . ? N11 C150 1.465(15) . ? N11 C152 1.481(14) . ? N11 Li6 2.08(2) . ? N12 C154 1.436(18) . ? N12 C153 1.481(15) . ? N12 C155 1.482(17) . ? N12 Li6 2.12(2) . ? C1 H3 0.9800 . ? C1 H4 0.9800 . ? C1 H5 0.9800 . ? C2 H17G 0.9800 . ? C2 H17H 0.9800 . ? C2 H17I 0.9800 . ? C3 C4 1.483(18) . ? C3 Li1 2.77(3) . ? C3 H82A 0.9900 . ? C3 H82B 0.9900 . ? C4 H16N 0.9900 . ? C4 H16O 0.9900 . ? C5 H6 0.9800 . ? C5 H7 0.9800 . ? C5 H8 0.9800 . ? C6 H18D 0.9800 . ? C6 H18E 0.9800 . ? C6 H18F 0.9800 . ? C7 C12 1.432(15) . ? C7 C8 1.460(16) . ? C8 C9 1.425(17) . ? C8 C17 1.486(17) . ? C9 C10 1.406(17) . ? C9 H91 0.9500 . ? C10 C11 1.386(15) . ? C10 C21 1.481(16) . ? C11 C12 1.351(15) . ? C11 H22 0.9500 . ? C12 C13 1.542(15) . ? C13 C15 1.493(18) . ? C13 C16 1.526(18) . ? C13 C14 1.590(16) . ? C14 H14D 0.9800 . ? C14 H14E 0.9800 . ? C14 H14F 0.9800 . ? C15 H14A 0.9800 . ? C15 H14B 0.9800 . ? C15 H14C 0.9800 . ? C16 H15A 0.9800 . ? C16 H15B 0.9800 . ? C16 H15C 0.9800 . ? C17 C20 1.533(17) . ? C17 C18 1.559(17) . ? C17 C19 1.565(17) . ? C18 H99A 0.9800 . ? C18 H99B 0.9800 . ? C18 H99C 0.9800 . ? C19 H88A 0.9800 . ? C19 H88B 0.9800 . ? C19 H88C 0.9800 . ? C20 H98A 0.9800 . ? C20 H98B 0.9800 . ? C20 H98C 0.9800 . ? C21 H73A 0.9800 . ? C21 H73B 0.9800 . ? C21 H73C 0.9800 . ? C30 H17A 0.9800 . ? C30 H17B 0.9800 . ? C30 H17C 0.9800 . ? C31 H18A 0.9800 . ? C31 H18B 0.9800 . ? C31 H18C 0.9800 . ? C32 C33 1.446(17) . ? C32 H20G 0.9900 . ? C32 H20H 0.9900 . ? C33 H18G 0.9900 . ? C33 H18H 0.9900 . ? C34 H17M 0.9800 . ? C34 H17N 0.9800 . ? C34 H17O 0.9800 . ? C35 H17J 0.9800 . ? C35 H17K 0.9800 . ? C35 H17L 0.9800 . ? C36 C41 1.400(15) . ? C36 C37 1.475(16) . ? C37 C38 1.412(15) . ? C37 C46 1.497(16) . ? C38 C39 1.379(17) . ? C38 H100 0.9500 . ? C39 C40 1.403(16) . ? C39 C50 1.518(15) . ? C40 C41 1.371(15) . ? C40 H20 0.9500 . ? C41 C42 1.549(16) . ? C42 C43 1.478(18) . ? C42 C45 1.525(16) . ? C42 C44 1.544(17) . ? C43 H56A 0.9800 . ? C43 H56B 0.9800 . ? C43 H56C 0.9800 . ? C44 H10D 0.9800 . ? C44 H10E 0.9800 . ? C44 H10F 0.9800 . ? C45 H85A 0.9800 . ? C45 H85B 0.9800 . ? C45 H85C 0.9800 . ? C46 C47 1.533(18) . ? C46 C49 1.543(16) . ? C46 C48 1.574(14) . ? C47 H62A 0.9800 . ? C47 H62B 0.9800 . ? C47 H62C 0.9800 . ? C48 H90A 0.9800 . ? C48 H90B 0.9800 . ? C48 H90C 0.9800 . ? C49 H11A 0.9800 . ? C49 H11B 0.9800 . ? C49 H11C 0.9800 . ? C50 H67A 0.9800 . ? C50 H67B 0.9800 . ? C50 H67C 0.9800 . ? C60 H14 0.9800 . ? C60 H15 0.9800 . ? C60 H16 0.9800 . ? C61 H19J 0.9800 . ? C61 H19K 0.9800 . ? C61 H19L 0.9800 . ? C62 C63 1.328(17) . ? C62 Li3 2.735(19) . ? C62 H36A 0.9900 . ? C62 H36B 0.9900 . ? C63 Li3 2.76(2) . ? C63 H20A 0.9900 . ? C63 H20B 0.9900 . ? C64 H19D 0.9800 . ? C64 H19E 0.9800 . ? C64 H19F 0.9800 . ? C65 H19M 0.9800 . ? C65 H19N 0.9800 . ? C65 H19O 0.9800 . ? C66 C67 1.422(15) . ? C66 C71 1.435(15) . ? C67 C68 1.359(14) . ? C67 C76 1.557(15) . ? C68 C69 1.390(15) . ? C68 H28 0.9500 . ? C69 C70 1.371(15) . ? C69 C80 1.508(15) . ? C70 C71 1.380(15) . ? C70 H24 0.9500 . ? C71 C72 1.546(16) . ? C72 C74 1.528(15) . ? C72 C75 1.545(16) . ? C72 C73 1.554(17) . ? C73 H13A 0.9800 . ? C73 H13B 0.9800 . ? C73 H13C 0.9800 . ? C74 H59A 0.9800 . ? C74 H59B 0.9800 . ? C74 H59C 0.9800 . ? C75 H84A 0.9800 . ? C75 H84B 0.9800 . ? C75 H84C 0.9800 . ? C76 C79 1.503(16) . ? C76 C78 1.505(16) . ? C76 C77 1.525(14) . ? C77 H11D 0.9800 . ? C77 H11E 0.9800 . ? C77 H11F 0.9800 . ? C78 H48A 0.9800 . ? C78 H48B 0.9800 . ? C78 H48C 0.9800 . ? C79 H75A 0.9800 . ? C79 H75B 0.9800 . ? C79 H75C 0.9800 . ? C80 H94A 0.9800 . ? C80 H94B 0.9800 . ? C80 H94C 0.9800 . ? C90 H19S 0.9800 . ? C90 H19T 0.9800 . ? C90 H19U 0.9800 . ? C91 H19P 0.9800 . ? C91 H19Q 0.9800 . ? C91 H19R 0.9800 . ? C92 C93 1.418(18) . ? C92 Li4 2.78(2) . ? C92 H15M 0.9900 . ? C92 H15N 0.9900 . ? C93 Li4 2.79(2) . ? C93 H15D 0.9900 . ? C93 H15E 0.9900 . ? C94 H19G 0.9800 . ? C94 H19H 0.9800 . ? C94 H19I 0.9800 . ? C95 H17 0.9800 . ? C95 H20E 0.9800 . ? C95 H20F 0.9800 . ? C96 C101 1.404(15) . ? C96 C97 1.445(15) . ? C97 C98 1.387(16) . ? C97 C106 1.493(17) . ? C98 C99 1.346(17) . ? C98 H209 0.9500 . ? C99 C100 1.421(17) . ? C99 C110 1.508(16) . ? C100 C101 1.417(16) . ? C100 H140 0.9500 . ? C101 C102 1.574(16) . ? C102 C104 1.483(18) . ? C102 C105 1.572(15) . ? C102 C103 1.574(17) . ? C103 H14G 0.9800 . ? C103 H14H 0.9800 . ? C103 H14I 0.9800 . ? C104 H14J 0.9800 . ? C104 H14K 0.9800 . ? C104 H14L 0.9800 . ? C105 H14M 0.9800 . ? C105 H14N 0.9800 . ? C105 H14O 0.9800 . ? C106 C108 1.503(17) . ? C106 C107 1.529(19) . ? C106 C109 1.579(17) . ? C107 H1 0.9800 . ? C107 H2 0.9800 . ? C107 H15F 0.9800 . ? C108 H15G 0.9800 . ? C108 H15H 0.9800 . ? C108 H15I 0.9800 . ? C109 H15J 0.9800 . ? C109 H15K 0.9800 . ? C109 H15L 0.9800 . ? C110 H14P 0.9800 . ? C110 H14Q 0.9800 . ? C110 H14R 0.9800 . ? C120 H9 0.9800 . ? C120 H10 0.9800 . ? C120 H19C 0.9800 . ? C121 H21A 0.9800 . ? C121 H21B 0.9800 . ? C121 H21C 0.9800 . ? C122 C123 1.449(15) . ? C122 H19A 0.9900 . ? C122 H19B 0.9900 . ? C123 H20C 0.9900 . ? C123 H20D 0.9900 . ? C124 H18P 0.9800 . ? C124 H18Q 0.9800 . ? C124 H18R 0.9800 . ? C125 H18J 0.9800 . ? C125 H18K 0.9800 . ? C125 H18L 0.9800 . ? C126 C131 1.397(14) . ? C126 C127 1.437(15) . ? C127 C128 1.407(14) . ? C127 C136 1.528(16) . ? C128 C129 1.365(16) . ? C128 H11 0.9500 . ? C129 C130 1.404(16) . ? C129 C140 1.495(15) . ? C130 C131 1.370(14) . ? C130 H26 0.9500 . ? C131 C132 1.587(16) . ? C132 C135 1.519(16) . ? C132 C133 1.521(16) . ? C132 C134 1.556(17) . ? C133 H69A 0.9800 . ? C133 H69B 0.9800 . ? C133 H69C 0.9800 . ? C134 H81A 0.9800 . ? C134 H81B 0.9800 . ? C134 H81C 0.9800 . ? C135 H40A 0.9800 . ? C135 H40B 0.9800 . ? C135 H40C 0.9800 . ? C136 C138 1.520(15) . ? C136 C139 1.541(15) . ? C136 C137 1.554(15) . ? C137 H17P 0.9800 . ? C137 H17Q 0.9800 . ? C137 H17R 0.9800 . ? C138 H18M 0.9800 . ? C138 H18N 0.9800 . ? C138 H18O 0.9800 . ? C139 H12 0.9800 . ? C139 H13 0.9800 . ? C139 H18I 0.9800 . ? C140 H10A 0.9800 . ? C140 H10B 0.9800 . ? C140 H10C 0.9800 . ? C150 H16D 0.9800 . ? C150 H16E 0.9800 . ? C150 H16F 0.9800 . ? C151 H16A 0.9800 . ? C151 H16B 0.9800 . ? C151 H16C 0.9800 . ? C152 C153 1.513(17) . ? C152 H16J 0.9900 . ? C152 H16K 0.9900 . ? C153 H16L 0.9900 . ? C153 H16M 0.9900 . ? C154 H17D 0.9800 . ? C154 H17E 0.9800 . ? C154 H17F 0.9800 . ? C155 H16G 0.9800 . ? C155 H16H 0.9800 . ? C155 H16I 0.9800 . ? C156 C157 1.436(16) . ? C156 C161 1.440(15) . ? C157 C158 1.421(15) . ? C157 C166 1.531(16) . ? C158 C159 1.389(15) . ? C158 H51 0.9500 . ? C159 C160 1.377(15) . ? C159 C170 1.517(14) . ? C160 C161 1.412(14) . ? C160 H33 0.9500 . ? C161 C162 1.505(16) . ? C162 C163 1.509(14) . ? C162 C165 1.534(16) . ? C162 C164 1.557(16) . ? C163 H35A 0.9800 . ? C163 H35B 0.9800 . ? C163 H35C 0.9800 . ? C164 H93A 0.9800 . ? C164 H93B 0.9800 . ? C164 H93C 0.9800 . ? C165 H25A 0.9800 . ? C165 H25B 0.9800 . ? C165 H25C 0.9800 . ? C166 C169 1.490(19) . ? C166 C168 1.558(17) . ? C166 C167 1.566(16) . ? C167 H60A 0.9800 . ? C167 H60B 0.9800 . ? C167 H60C 0.9800 . ? C168 H92A 0.9800 . ? C168 H92B 0.9800 . ? C168 H92C 0.9800 . ? C169 H43A 0.9800 . ? C169 H43B 0.9800 . ? C169 H43C 0.9800 . ? C170 H64A 0.9800 . ? C170 H64B 0.9800 . ? C170 H64C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 O1 Li1 172.7(11) . . ? C36 O2 Li2 177.7(11) . . ? C66 O3 Li3 172.2(10) . . ? C96 O4 Li4 176.4(11) . . ? C126 O5 Li5 176.1(10) . . ? C156 O6 Li6 175.5(10) . . ? C2 N1 C3 114.9(12) . . ? C2 N1 C1 108.3(11) . . ? C3 N1 C1 105.3(11) . . ? C2 N1 Li1 109.9(10) . . ? C3 N1 Li1 104.4(11) . . ? C1 N1 Li1 114.1(11) . . ? C5 N2 C4 116.0(12) . . ? C5 N2 C6 107.0(11) . . ? C4 N2 C6 106.1(10) . . ? C5 N2 Li1 107.3(11) . . ? C4 N2 Li1 103.5(10) . . ? C6 N2 Li1 117.4(11) . . ? C31 N3 C30 109.1(12) . . ? C31 N3 C32 101.1(14) . . ? C30 N3 C32 114.8(12) . . ? C31 N3 Li2 118.3(12) . . ? C30 N3 Li2 110.1(12) . . ? C32 N3 Li2 103.4(9) . . ? C33 N4 C35 110.7(12) . . ? C33 N4 C34 109.7(12) . . ? C35 N4 C34 107.4(13) . . ? C33 N4 Li2 104.2(9) . . ? C35 N4 Li2 117.7(11) . . ? C34 N4 Li2 106.9(11) . . ? C65 N5 C64 108.9(12) . . ? C65 N5 C63 113.5(12) . . ? C64 N5 C63 108.5(11) . . ? C65 N5 Li3 112.7(10) . . ? C64 N5 Li3 111.2(10) . . ? C63 N5 Li3 102.0(8) . . ? C62 N6 C60 111.8(12) . . ? C62 N6 C61 110.6(12) . . ? C60 N6 C61 105.9(11) . . ? C62 N6 Li3 102.1(9) . . ? C60 N6 Li3 109.9(10) . . ? C61 N6 Li3 116.6(10) . . ? C91 N7 C90 108.4(11) . . ? C91 N7 C92 111.0(10) . . ? C90 N7 C92 110.1(11) . . ? C91 N7 Li4 105.6(11) . . ? C90 N7 Li4 119.7(10) . . ? C92 N7 Li4 101.8(9) . . ? C95 N8 C93 109.6(12) . . ? C95 N8 C94 107.0(11) . . ? C93 N8 C94 110.9(11) . . ? C95 N8 Li4 109.7(10) . . ? C93 N8 Li4 104.2(10) . . ? C94 N8 Li4 115.4(12) . . ? C121 N9 C122 110.6(10) . . ? C121 N9 C120 110.1(11) . . ? C122 N9 C120 108.2(9) . . ? C121 N9 Li5 108.2(9) . . ? C122 N9 Li5 103.8(8) . . ? C120 N9 Li5 115.8(9) . . ? C125 N10 C124 107.5(11) . . ? C125 N10 C123 114.6(11) . . ? C124 N10 C123 108.2(10) . . ? C125 N10 Li5 108.8(10) . . ? C124 N10 Li5 116.1(9) . . ? C123 N10 Li5 101.9(8) . . ? C151 N11 C150 109.9(11) . . ? C151 N11 C152 114.0(10) . . ? C150 N11 C152 106.8(10) . . ? C151 N11 Li6 105.2(10) . . ? C150 N11 Li6 117.0(9) . . ? C152 N11 Li6 104.0(9) . . ? C154 N12 C153 107.7(11) . . ? C154 N12 C155 109.2(12) . . ? C153 N12 C155 114.8(11) . . ? C154 N12 Li6 117.5(11) . . ? C153 N12 Li6 103.7(9) . . ? C155 N12 Li6 104.1(9) . . ? N1 C1 H3 109.5 . . ? N1 C1 H4 109.5 . . ? H3 C1 H4 109.5 . . ? N1 C1 H5 109.5 . . ? H3 C1 H5 109.5 . . ? H4 C1 H5 109.5 . . ? N1 C2 H17G 109.5 . . ? N1 C2 H17H 109.5 . . ? H17G C2 H17H 109.5 . . ? N1 C2 H17I 109.5 . . ? H17G C2 H17I 109.5 . . ? H17H C2 H17I 109.5 . . ? N1 C3 C4 111.7(12) . . ? N1 C3 Li1 45.8(7) . . ? C4 C3 Li1 76.2(9) . . ? N1 C3 H82A 109.3 . . ? C4 C3 H82A 109.3 . . ? Li1 C3 H82A 96.0 . . ? N1 C3 H82B 109.3 . . ? C4 C3 H82B 109.3 . . ? Li1 C3 H82B 151.2 . . ? H82A C3 H82B 107.9 . . ? N2 C4 C3 110.4(11) . . ? N2 C4 H16N 109.6 . . ? C3 C4 H16N 109.6 . . ? N2 C4 H16O 109.6 . . ? C3 C4 H16O 109.6 . . ? H16N C4 H16O 108.1 . . ? N2 C5 H6 109.5 . . ? N2 C5 H7 109.5 . . ? H6 C5 H7 109.5 . . ? N2 C5 H8 109.5 . . ? H6 C5 H8 109.5 . . ? H7 C5 H8 109.5 . . ? N2 C6 H18D 109.5 . . ? N2 C6 H18E 109.5 . . ? H18D C6 H18E 109.5 . . ? N2 C6 H18F 109.5 . . ? H18D C6 H18F 109.5 . . ? H18E C6 H18F 109.5 . . ? O1 C7 C12 122.0(10) . . ? O1 C7 C8 119.2(11) . . ? C12 C7 C8 118.8(10) . . ? C9 C8 C7 114.3(11) . . ? C9 C8 C17 122.3(12) . . ? C7 C8 C17 123.3(11) . . ? C10 C9 C8 125.9(11) . . ? C10 C9 H91 117.0 . . ? C8 C9 H91 117.0 . . ? C11 C10 C9 116.0(11) . . ? C11 C10 C21 122.6(12) . . ? C9 C10 C21 121.4(11) . . ? C12 C11 C10 123.0(11) . . ? C12 C11 H22 118.5 . . ? C10 C11 H22 118.5 . . ? C11 C12 C7 121.6(10) . . ? C11 C12 C13 119.5(10) . . ? C7 C12 C13 118.8(10) . . ? C15 C13 C16 107.0(10) . . ? C15 C13 C12 110.1(11) . . ? C16 C13 C12 113.9(11) . . ? C15 C13 C14 111.1(11) . . ? C16 C13 C14 106.0(11) . . ? C12 C13 C14 108.7(9) . . ? C13 C14 H14D 109.5 . . ? C13 C14 H14E 109.5 . . ? H14D C14 H14E 109.5 . . ? C13 C14 H14F 109.5 . . ? H14D C14 H14F 109.5 . . ? H14E C14 H14F 109.5 . . ? C13 C15 H14A 109.5 . . ? C13 C15 H14B 109.5 . . ? H14A C15 H14B 109.5 . . ? C13 C15 H14C 109.5 . . ? H14A C15 H14C 109.5 . . ? H14B C15 H14C 109.5 . . ? C13 C16 H15A 109.5 . . ? C13 C16 H15B 109.5 . . ? H15A C16 H15B 109.5 . . ? C13 C16 H15C 109.5 . . ? H15A C16 H15C 109.5 . . ? H15B C16 H15C 109.5 . . ? C8 C17 C20 114.8(12) . . ? C8 C17 C18 109.6(10) . . ? C20 C17 C18 105.2(11) . . ? C8 C17 C19 109.7(10) . . ? C20 C17 C19 108.9(11) . . ? C18 C17 C19 108.3(11) . . ? C17 C18 H99A 109.5 . . ? C17 C18 H99B 109.5 . . ? H99A C18 H99B 109.5 . . ? C17 C18 H99C 109.5 . . ? H99A C18 H99C 109.5 . . ? H99B C18 H99C 109.5 . . ? C17 C19 H88A 109.5 . . ? C17 C19 H88B 109.5 . . ? H88A C19 H88B 109.5 . . ? C17 C19 H88C 109.5 . . ? H88A C19 H88C 109.5 . . ? H88B C19 H88C 109.5 . . ? C17 C20 H98A 109.5 . . ? C17 C20 H98B 109.5 . . ? H98A C20 H98B 109.5 . . ? C17 C20 H98C 109.5 . . ? H98A C20 H98C 109.5 . . ? H98B C20 H98C 109.5 . . ? C10 C21 H73A 109.5 . . ? C10 C21 H73B 109.5 . . ? H73A C21 H73B 109.5 . . ? C10 C21 H73C 109.5 . . ? H73A C21 H73C 109.5 . . ? H73B C21 H73C 109.5 . . ? N3 C30 H17A 109.5 . . ? N3 C30 H17B 109.5 . . ? H17A C30 H17B 109.5 . . ? N3 C30 H17C 109.5 . . ? H17A C30 H17C 109.5 . . ? H17B C30 H17C 109.5 . . ? N3 C31 H18A 109.5 . . ? N3 C31 H18B 109.5 . . ? H18A C31 H18B 109.5 . . ? N3 C31 H18C 109.5 . . ? H18A C31 H18C 109.5 . . ? H18B C31 H18C 109.5 . . ? C33 C32 N3 113.2(11) . . ? C33 C32 H20G 108.9 . . ? N3 C32 H20G 108.9 . . ? C33 C32 H20H 108.9 . . ? N3 C32 H20H 108.9 . . ? H20G C32 H20H 107.8 . . ? N4 C33 C32 116.0(11) . . ? N4 C33 H18G 108.3 . . ? C32 C33 H18G 108.3 . . ? N4 C33 H18H 108.3 . . ? C32 C33 H18H 108.3 . . ? H18G C33 H18H 107.4 . . ? N4 C34 H17M 109.5 . . ? N4 C34 H17N 109.5 . . ? H17M C34 H17N 109.5 . . ? N4 C34 H17O 109.5 . . ? H17M C34 H17O 109.5 . . ? H17N C34 H17O 109.5 . . ? N4 C35 H17J 109.5 . . ? N4 C35 H17K 109.5 . . ? H17J C35 H17K 109.5 . . ? N4 C35 H17L 109.5 . . ? H17J C35 H17L 109.5 . . ? H17K C35 H17L 109.5 . . ? O2 C36 C41 122.6(10) . . ? O2 C36 C37 118.4(10) . . ? C41 C36 C37 119.1(10) . . ? C38 C37 C36 115.7(11) . . ? C38 C37 C46 123.7(11) . . ? C36 C37 C46 120.4(10) . . ? C39 C38 C37 125.7(12) . . ? C39 C38 H100 117.2 . . ? C37 C38 H100 117.2 . . ? C38 C39 C40 115.1(11) . . ? C38 C39 C50 122.1(11) . . ? C40 C39 C50 122.8(11) . . ? C41 C40 C39 124.6(12) . . ? C41 C40 H20 117.7 . . ? C39 C40 H20 117.7 . . ? C40 C41 C36 119.8(11) . . ? C40 C41 C42 123.2(10) . . ? C36 C41 C42 117.0(10) . . ? C43 C42 C45 108.8(11) . . ? C43 C42 C44 105.0(10) . . ? C45 C42 C44 113.2(10) . . ? C43 C42 C41 108.9(10) . . ? C45 C42 C41 111.5(10) . . ? C44 C42 C41 109.2(9) . . ? C42 C43 H56A 109.5 . . ? C42 C43 H56B 109.5 . . ? H56A C43 H56B 109.5 . . ? C42 C43 H56C 109.5 . . ? H56A C43 H56C 109.5 . . ? H56B C43 H56C 109.5 . . ? C42 C44 H10D 109.5 . . ? C42 C44 H10E 109.5 . . ? H10D C44 H10E 109.5 . . ? C42 C44 H10F 109.5 . . ? H10D C44 H10F 109.5 . . ? H10E C44 H10F 109.5 . . ? C42 C45 H85A 109.5 . . ? C42 C45 H85B 109.5 . . ? H85A C45 H85B 109.5 . . ? C42 C45 H85C 109.5 . . ? H85A C45 H85C 109.5 . . ? H85B C45 H85C 109.5 . . ? C37 C46 C47 114.5(10) . . ? C37 C46 C49 112.0(10) . . ? C47 C46 C49 108.3(10) . . ? C37 C46 C48 110.8(9) . . ? C47 C46 C48 105.8(10) . . ? C49 C46 C48 104.9(9) . . ? C46 C47 H62A 109.5 . . ? C46 C47 H62B 109.5 . . ? H62A C47 H62B 109.5 . . ? C46 C47 H62C 109.5 . . ? H62A C47 H62C 109.5 . . ? H62B C47 H62C 109.5 . . ? C46 C48 H90A 109.5 . . ? C46 C48 H90B 109.5 . . ? H90A C48 H90B 109.5 . . ? C46 C48 H90C 109.5 . . ? H90A C48 H90C 109.5 . . ? H90B C48 H90C 109.5 . . ? C46 C49 H11A 109.5 . . ? C46 C49 H11B 109.5 . . ? H11A C49 H11B 109.5 . . ? C46 C49 H11C 109.5 . . ? H11A C49 H11C 109.5 . . ? H11B C49 H11C 109.5 . . ? C39 C50 H67A 109.5 . . ? C39 C50 H67B 109.5 . . ? H67A C50 H67B 109.5 . . ? C39 C50 H67C 109.5 . . ? H67A C50 H67C 109.5 . . ? H67B C50 H67C 109.5 . . ? N6 C60 H14 109.5 . . ? N6 C60 H15 109.5 . . ? H14 C60 H15 109.5 . . ? N6 C60 H16 109.5 . . ? H14 C60 H16 109.5 . . ? H15 C60 H16 109.5 . . ? N6 C61 H19J 109.5 . . ? N6 C61 H19K 109.5 . . ? H19J C61 H19K 109.5 . . ? N6 C61 H19L 109.5 . . ? H19J C61 H19L 109.5 . . ? H19K C61 H19L 109.5 . . ? C63 C62 N6 122.6(11) . . ? C63 C62 Li3 77.2(8) . . ? N6 C62 Li3 47.2(7) . . ? C63 C62 H36A 106.7 . . ? N6 C62 H36A 106.7 . . ? Li3 C62 H36A 112.1 . . ? C63 C62 H36B 106.7 . . ? N6 C62 H36B 106.7 . . ? Li3 C62 H36B 138.1 . . ? H36A C62 H36B 106.6 . . ? C62 C63 N5 120.5(12) . . ? C62 C63 Li3 74.8(9) . . ? N5 C63 Li3 46.9(7) . . ? C62 C63 H20A 107.2 . . ? N5 C63 H20A 107.2 . . ? Li3 C63 H20A 115.0 . . ? C62 C63 H20B 107.2 . . ? N5 C63 H20B 107.2 . . ? Li3 C63 H20B 135.5 . . ? H20A C63 H20B 106.8 . . ? N5 C64 H19D 109.5 . . ? N5 C64 H19E 109.5 . . ? H19D C64 H19E 109.5 . . ? N5 C64 H19F 109.5 . . ? H19D C64 H19F 109.5 . . ? H19E C64 H19F 109.5 . . ? N5 C65 H19M 109.5 . . ? N5 C65 H19N 109.5 . . ? H19M C65 H19N 109.5 . . ? N5 C65 H19O 109.5 . . ? H19M C65 H19O 109.5 . . ? H19N C65 H19O 109.5 . . ? O3 C66 C67 121.5(10) . . ? O3 C66 C71 119.3(11) . . ? C67 C66 C71 119.1(10) . . ? C68 C67 C66 118.7(10) . . ? C68 C67 C76 120.7(9) . . ? C66 C67 C76 120.6(9) . . ? C67 C68 C69 123.8(11) . . ? C67 C68 H28 118.1 . . ? C69 C68 H28 118.1 . . ? C70 C69 C68 116.6(9) . . ? C70 C69 C80 121.2(10) . . ? C68 C69 C80 122.2(11) . . ? C69 C70 C71 124.4(10) . . ? C69 C70 H24 117.8 . . ? C71 C70 H24 117.8 . . ? C70 C71 C66 117.4(10) . . ? C70 C71 C72 120.3(11) . . ? C66 C71 C72 122.3(10) . . ? C74 C72 C75 110.1(10) . . ? C74 C72 C71 109.9(10) . . ? C75 C72 C71 107.5(9) . . ? C74 C72 C73 108.4(10) . . ? C75 C72 C73 106.5(10) . . ? C71 C72 C73 114.4(10) . . ? C72 C73 H13A 109.5 . . ? C72 C73 H13B 109.5 . . ? H13A C73 H13B 109.5 . . ? C72 C73 H13C 109.5 . . ? H13A C73 H13C 109.5 . . ? H13B C73 H13C 109.5 . . ? C72 C74 H59A 109.5 . . ? C72 C74 H59B 109.5 . . ? H59A C74 H59B 109.5 . . ? C72 C74 H59C 109.5 . . ? H59A C74 H59C 109.5 . . ? H59B C74 H59C 109.5 . . ? C72 C75 H84A 109.5 . . ? C72 C75 H84B 109.5 . . ? H84A C75 H84B 109.5 . . ? C72 C75 H84C 109.5 . . ? H84A C75 H84C 109.5 . . ? H84B C75 H84C 109.5 . . ? C79 C76 C78 107.4(10) . . ? C79 C76 C77 107.7(10) . . ? C78 C76 C77 109.9(9) . . ? C79 C76 C67 111.7(8) . . ? C78 C76 C67 111.0(9) . . ? C77 C76 C67 109.1(9) . . ? C76 C77 H11D 109.5 . . ? C76 C77 H11E 109.5 . . ? H11D C77 H11E 109.5 . . ? C76 C77 H11F 109.5 . . ? H11D C77 H11F 109.5 . . ? H11E C77 H11F 109.5 . . ? C76 C78 H48A 109.5 . . ? C76 C78 H48B 109.5 . . ? H48A C78 H48B 109.5 . . ? C76 C78 H48C 109.5 . . ? H48A C78 H48C 109.5 . . ? H48B C78 H48C 109.5 . . ? C76 C79 H75A 109.5 . . ? C76 C79 H75B 109.5 . . ? H75A C79 H75B 109.5 . . ? C76 C79 H75C 109.5 . . ? H75A C79 H75C 109.5 . . ? H75B C79 H75C 109.5 . . ? C69 C80 H94A 109.5 . . ? C69 C80 H94B 109.5 . . ? H94A C80 H94B 109.5 . . ? C69 C80 H94C 109.5 . . ? H94A C80 H94C 109.5 . . ? H94B C80 H94C 109.5 . . ? N7 C90 H19S 109.5 . . ? N7 C90 H19T 109.5 . . ? H19S C90 H19T 109.5 . . ? N7 C90 H19U 109.5 . . ? H19S C90 H19U 109.5 . . ? H19T C90 H19U 109.5 . . ? N7 C91 H19P 109.5 . . ? N7 C91 H19Q 109.5 . . ? H19P C91 H19Q 109.5 . . ? N7 C91 H19R 109.5 . . ? H19P C91 H19R 109.5 . . ? H19Q C91 H19R 109.5 . . ? C93 C92 N7 114.0(12) . . ? C93 C92 Li4 75.3(9) . . ? N7 C92 Li4 46.3(7) . . ? C93 C92 H15M 108.8 . . ? N7 C92 H15M 108.8 . . ? Li4 C92 H15M 148.7 . . ? C93 C92 H15N 108.8 . . ? N7 C92 H15N 108.8 . . ? Li4 C92 H15N 99.7 . . ? H15M C92 H15N 107.6 . . ? C92 C93 N8 114.9(12) . . ? C92 C93 Li4 75.2(9) . . ? N8 C93 Li4 45.4(7) . . ? C92 C93 H15D 108.5 . . ? N8 C93 H15D 108.5 . . ? Li4 C93 H15D 145.5 . . ? C92 C93 H15E 108.5 . . ? N8 C93 H15E 108.5 . . ? Li4 C93 H15E 103.3 . . ? H15D C93 H15E 107.5 . . ? N8 C94 H19G 109.5 . . ? N8 C94 H19H 109.5 . . ? H19G C94 H19H 109.5 . . ? N8 C94 H19I 109.5 . . ? H19G C94 H19I 109.5 . . ? H19H C94 H19I 109.5 . . ? N8 C95 H17 109.5 . . ? N8 C95 H20E 109.5 . . ? H17 C95 H20E 109.5 . . ? N8 C95 H20F 109.5 . . ? H17 C95 H20F 109.5 . . ? H20E C95 H20F 109.5 . . ? O4 C96 C101 120.0(10) . . ? O4 C96 C97 123.0(11) . . ? C101 C96 C97 117.0(10) . . ? C98 C97 C96 119.1(11) . . ? C98 C97 C106 122.9(11) . . ? C96 C97 C106 117.9(10) . . ? C99 C98 C97 125.7(12) . . ? C99 C98 H209 117.2 . . ? C97 C98 H209 117.2 . . ? C98 C99 C100 115.8(11) . . ? C98 C99 C110 123.3(13) . . ? C100 C99 C110 120.8(13) . . ? C101 C100 C99 122.0(12) . . ? C101 C100 H140 119.0 . . ? C99 C100 H140 119.0 . . ? C96 C101 C100 120.4(11) . . ? C96 C101 C102 120.7(10) . . ? C100 C101 C102 118.9(11) . . ? C104 C102 C105 109.5(11) . . ? C104 C102 C101 110.3(11) . . ? C105 C102 C101 108.2(9) . . ? C104 C102 C103 110.1(11) . . ? C105 C102 C103 105.1(10) . . ? C101 C102 C103 113.5(10) . . ? C102 C103 H14G 109.5 . . ? C102 C103 H14H 109.5 . . ? H14G C103 H14H 109.5 . . ? C102 C103 H14I 109.5 . . ? H14G C103 H14I 109.5 . . ? H14H C103 H14I 109.5 . . ? C102 C104 H14J 109.5 . . ? C102 C104 H14K 109.5 . . ? H14J C104 H14K 109.5 . . ? C102 C104 H14L 109.5 . . ? H14J C104 H14L 109.5 . . ? H14K C104 H14L 109.5 . . ? C102 C105 H14M 109.5 . . ? C102 C105 H14N 109.5 . . ? H14M C105 H14N 109.5 . . ? C102 C105 H14O 109.5 . . ? H14M C105 H14O 109.5 . . ? H14N C105 H14O 109.5 . . ? C97 C106 C108 110.5(10) . . ? C97 C106 C107 110.1(11) . . ? C108 C106 C107 110.9(13) . . ? C97 C106 C109 110.1(12) . . ? C108 C106 C109 110.1(11) . . ? C107 C106 C109 105.0(11) . . ? C106 C107 H1 109.5 . . ? C106 C107 H2 109.5 . . ? H1 C107 H2 109.5 . . ? C106 C107 H15F 109.5 . . ? H1 C107 H15F 109.5 . . ? H2 C107 H15F 109.5 . . ? C106 C108 H15G 109.5 . . ? C106 C108 H15H 109.5 . . ? H15G C108 H15H 109.5 . . ? C106 C108 H15I 109.5 . . ? H15G C108 H15I 109.5 . . ? H15H C108 H15I 109.5 . . ? C106 C109 H15J 109.5 . . ? C106 C109 H15K 109.5 . . ? H15J C109 H15K 109.5 . . ? C106 C109 H15L 109.5 . . ? H15J C109 H15L 109.5 . . ? H15K C109 H15L 109.5 . . ? C99 C110 H14P 109.5 . . ? C99 C110 H14Q 109.5 . . ? H14P C110 H14Q 109.5 . . ? C99 C110 H14R 109.5 . . ? H14P C110 H14R 109.5 . . ? H14Q C110 H14R 109.5 . . ? N9 C120 H9 109.5 . . ? N9 C120 H10 109.5 . . ? H9 C120 H10 109.5 . . ? N9 C120 H19C 109.5 . . ? H9 C120 H19C 109.5 . . ? H10 C120 H19C 109.5 . . ? N9 C121 H21A 109.5 . . ? N9 C121 H21B 109.5 . . ? H21A C121 H21B 109.5 . . ? N9 C121 H21C 109.5 . . ? H21A C121 H21C 109.5 . . ? H21B C121 H21C 109.5 . . ? C123 C122 N9 112.8(9) . . ? C123 C122 H19A 109.0 . . ? N9 C122 H19A 109.0 . . ? C123 C122 H19B 109.0 . . ? N9 C122 H19B 109.0 . . ? H19A C122 H19B 107.8 . . ? C122 C123 N10 112.0(9) . . ? C122 C123 H20C 109.2 . . ? N10 C123 H20C 109.2 . . ? C122 C123 H20D 109.2 . . ? N10 C123 H20D 109.2 . . ? H20C C123 H20D 107.9 . . ? N10 C124 H18P 109.5 . . ? N10 C124 H18Q 109.5 . . ? H18P C124 H18Q 109.5 . . ? N10 C124 H18R 109.5 . . ? H18P C124 H18R 109.5 . . ? H18Q C124 H18R 109.5 . . ? N10 C125 H18J 109.5 . . ? N10 C125 H18K 109.5 . . ? H18J C125 H18K 109.5 . . ? N10 C125 H18L 109.5 . . ? H18J C125 H18L 109.5 . . ? H18K C125 H18L 109.5 . . ? O5 C126 C131 121.0(10) . . ? O5 C126 C127 119.8(10) . . ? C131 C126 C127 119.2(9) . . ? C128 C127 C126 117.0(11) . . ? C128 C127 C136 121.6(10) . . ? C126 C127 C136 121.2(10) . . ? C129 C128 C127 124.1(11) . . ? C129 C128 H11 117.9 . . ? C127 C128 H11 117.9 . . ? C128 C129 C130 116.8(10) . . ? C128 C129 C140 122.0(12) . . ? C130 C129 C140 121.2(12) . . ? C131 C130 C129 122.6(10) . . ? C131 C130 H26 118.7 . . ? C129 C130 H26 118.7 . . ? C130 C131 C126 120.2(10) . . ? C130 C131 C132 120.5(10) . . ? C126 C131 C132 119.3(9) . . ? C135 C132 C133 110.0(11) . . ? C135 C132 C134 114.0(11) . . ? C133 C132 C134 104.6(10) . . ? C135 C132 C131 110.3(9) . . ? C133 C132 C131 110.5(10) . . ? C134 C132 C131 107.3(9) . . ? C132 C133 H69A 109.5 . . ? C132 C133 H69B 109.5 . . ? H69A C133 H69B 109.5 . . ? C132 C133 H69C 109.5 . . ? H69A C133 H69C 109.5 . . ? H69B C133 H69C 109.5 . . ? C132 C134 H81A 109.5 . . ? C132 C134 H81B 109.5 . . ? H81A C134 H81B 109.5 . . ? C132 C134 H81C 109.5 . . ? H81A C134 H81C 109.5 . . ? H81B C134 H81C 109.5 . . ? C132 C135 H40A 109.5 . . ? C132 C135 H40B 109.5 . . ? H40A C135 H40B 109.5 . . ? C132 C135 H40C 109.5 . . ? H40A C135 H40C 109.5 . . ? H40B C135 H40C 109.5 . . ? C138 C136 C127 109.9(9) . . ? C138 C136 C139 106.9(10) . . ? C127 C136 C139 113.4(9) . . ? C138 C136 C137 109.2(9) . . ? C127 C136 C137 110.1(9) . . ? C139 C136 C137 107.2(9) . . ? C136 C137 H17P 109.5 . . ? C136 C137 H17Q 109.5 . . ? H17P C137 H17Q 109.5 . . ? C136 C137 H17R 109.5 . . ? H17P C137 H17R 109.5 . . ? H17Q C137 H17R 109.5 . . ? C136 C138 H18M 109.5 . . ? C136 C138 H18N 109.5 . . ? H18M C138 H18N 109.5 . . ? C136 C138 H18O 109.5 . . ? H18M C138 H18O 109.5 . . ? H18N C138 H18O 109.5 . . ? C136 C139 H12 109.5 . . ? C136 C139 H13 109.5 . . ? H12 C139 H13 109.5 . . ? C136 C139 H18I 109.5 . . ? H12 C139 H18I 109.5 . . ? H13 C139 H18I 109.5 . . ? C129 C140 H10A 109.5 . . ? C129 C140 H10B 109.5 . . ? H10A C140 H10B 109.5 . . ? C129 C140 H10C 109.5 . . ? H10A C140 H10C 109.5 . . ? H10B C140 H10C 109.5 . . ? N11 C150 H16D 109.5 . . ? N11 C150 H16E 109.5 . . ? H16D C150 H16E 109.5 . . ? N11 C150 H16F 109.5 . . ? H16D C150 H16F 109.5 . . ? H16E C150 H16F 109.5 . . ? N11 C151 H16A 109.5 . . ? N11 C151 H16B 109.5 . . ? H16A C151 H16B 109.5 . . ? N11 C151 H16C 109.5 . . ? H16A C151 H16C 109.5 . . ? H16B C151 H16C 109.5 . . ? N11 C152 C153 110.6(11) . . ? N11 C152 H16J 109.5 . . ? C153 C152 H16J 109.5 . . ? N11 C152 H16K 109.5 . . ? C153 C152 H16K 109.5 . . ? H16J C152 H16K 108.1 . . ? N12 C153 C152 110.7(9) . . ? N12 C153 H16L 109.5 . . ? C152 C153 H16L 109.5 . . ? N12 C153 H16M 109.5 . . ? C152 C153 H16M 109.5 . . ? H16L C153 H16M 108.1 . . ? N12 C154 H17D 109.5 . . ? N12 C154 H17E 109.5 . . ? H17D C154 H17E 109.5 . . ? N12 C154 H17F 109.5 . . ? H17D C154 H17F 109.5 . . ? H17E C154 H17F 109.5 . . ? N12 C155 H16G 109.5 . . ? N12 C155 H16H 109.5 . . ? H16G C155 H16H 109.5 . . ? N12 C155 H16I 109.5 . . ? H16G C155 H16I 109.5 . . ? H16H C155 H16I 109.5 . . ? O6 C156 C157 118.9(10) . . ? O6 C156 C161 123.1(11) . . ? C157 C156 C161 118.0(10) . . ? C158 C157 C156 118.8(10) . . ? C158 C157 C166 117.7(11) . . ? C156 C157 C166 123.5(10) . . ? C159 C158 C157 122.9(11) . . ? C159 C158 H51 118.6 . . ? C157 C158 H51 118.6 . . ? C160 C159 C158 117.9(10) . . ? C160 C159 C170 120.8(10) . . ? C158 C159 C170 121.3(11) . . ? C159 C160 C161 123.0(10) . . ? C159 C160 H33 118.5 . . ? C161 C160 H33 118.5 . . ? C160 C161 C156 119.4(11) . . ? C160 C161 C162 121.9(10) . . ? C156 C161 C162 118.7(10) . . ? C161 C162 C163 113.1(10) . . ? C161 C162 C165 112.2(9) . . ? C163 C162 C165 105.4(9) . . ? C161 C162 C164 110.3(9) . . ? C163 C162 C164 111.3(9) . . ? C165 C162 C164 104.1(9) . . ? C162 C163 H35A 109.5 . . ? C162 C163 H35B 109.5 . . ? H35A C163 H35B 109.5 . . ? C162 C163 H35C 109.5 . . ? H35A C163 H35C 109.5 . . ? H35B C163 H35C 109.5 . . ? C162 C164 H93A 109.5 . . ? C162 C164 H93B 109.5 . . ? H93A C164 H93B 109.5 . . ? C162 C164 H93C 109.5 . . ? H93A C164 H93C 109.5 . . ? H93B C164 H93C 109.5 . . ? C162 C165 H25A 109.5 . . ? C162 C165 H25B 109.5 . . ? H25A C165 H25B 109.5 . . ? C162 C165 H25C 109.5 . . ? H25A C165 H25C 109.5 . . ? H25B C165 H25C 109.5 . . ? C169 C166 C157 115.1(11) . . ? C169 C166 C168 109.2(12) . . ? C157 C166 C168 108.7(10) . . ? C169 C166 C167 106.9(10) . . ? C157 C166 C167 108.0(9) . . ? C168 C166 C167 108.8(10) . . ? C166 C167 H60A 109.5 . . ? C166 C167 H60B 109.5 . . ? H60A C167 H60B 109.5 . . ? C166 C167 H60C 109.5 . . ? H60A C167 H60C 109.5 . . ? H60B C167 H60C 109.5 . . ? C166 C168 H92A 109.5 . . ? C166 C168 H92B 109.5 . . ? H92A C168 H92B 109.5 . . ? C166 C168 H92C 109.5 . . ? H92A C168 H92C 109.5 . . ? H92B C168 H92C 109.5 . . ? C166 C169 H43A 109.5 . . ? C166 C169 H43B 109.5 . . ? H43A C169 H43B 109.5 . . ? C166 C169 H43C 109.5 . . ? H43A C169 H43C 109.5 . . ? H43B C169 H43C 109.5 . . ? C159 C170 H64A 109.5 . . ? C159 C170 H64B 109.5 . . ? H64A C170 H64B 109.5 . . ? C159 C170 H64C 109.5 . . ? H64A C170 H64C 109.5 . . ? H64B C170 H64C 109.5 . . ? O1 Li1 N1 133.9(14) . . ? O1 Li1 N2 137.4(13) . . ? N1 Li1 N2 86.7(10) . . ? O1 Li1 C3 155.6(14) . . ? N1 Li1 C3 29.9(5) . . ? N2 Li1 C3 58.1(7) . . ? O2 Li2 N3 132.8(12) . . ? O2 Li2 N4 138.6(11) . . ? N3 Li2 N4 88.4(9) . . ? O3 Li3 N6 135.4(11) . . ? O3 Li3 N5 134.3(10) . . ? N6 Li3 N5 89.2(7) . . ? O3 Li3 C62 162.2(9) . . ? N6 Li3 C62 30.7(5) . . ? N5 Li3 C62 58.7(5) . . ? O3 Li3 C63 164.6(11) . . ? N6 Li3 C63 58.0(6) . . ? N5 Li3 C63 31.2(4) . . ? C62 Li3 C63 27.9(4) . . ? O4 Li4 N8 134.6(13) . . ? O4 Li4 N7 136.7(11) . . ? N8 Li4 N7 88.6(9) . . ? O4 Li4 C92 165.6(12) . . ? N8 Li4 C92 57.8(6) . . ? N7 Li4 C92 31.9(5) . . ? O4 Li4 C93 164.4(12) . . ? N8 Li4 C93 30.4(5) . . ? N7 Li4 C93 58.5(6) . . ? C92 Li4 C93 29.5(4) . . ? O5 Li5 N10 136.1(11) . . ? O5 Li5 N9 135.2(10) . . ? N10 Li5 N9 87.9(7) . . ? O6 Li6 N11 137.7(12) . . ? O6 Li6 N12 135.4(13) . . ? N11 Li6 N12 86.7(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C3 C4 -78.6(14) . . . . ? C1 N1 C3 C4 162.3(12) . . . . ? Li1 N1 C3 C4 41.8(16) . . . . ? C2 N1 C3 Li1 -120.4(14) . . . . ? C1 N1 C3 Li1 120.5(13) . . . . ? C5 N2 C4 C3 -79.9(16) . . . . ? C6 N2 C4 C3 161.5(13) . . . . ? Li1 N2 C4 C3 37.3(15) . . . . ? N1 C3 C4 N2 -56.5(17) . . . . ? Li1 C3 C4 N2 -27.0(11) . . . . ? Li1 O1 C7 C12 -160(9) . . . . ? Li1 O1 C7 C8 22(9) . . . . ? O1 C7 C8 C9 -176.6(10) . . . . ? C12 C7 C8 C9 5.0(15) . . . . ? O1 C7 C8 C17 2.4(17) . . . . ? C12 C7 C8 C17 -176.0(10) . . . . ? C7 C8 C9 C10 -0.3(17) . . . . ? C17 C8 C9 C10 -179.4(11) . . . . ? C8 C9 C10 C11 -3.0(17) . . . . ? C8 C9 C10 C21 179.7(11) . . . . ? C9 C10 C11 C12 1.6(16) . . . . ? C21 C10 C11 C12 178.9(11) . . . . ? C10 C11 C12 C7 3.1(17) . . . . ? C10 C11 C12 C13 -178.3(10) . . . . ? O1 C7 C12 C11 175.0(10) . . . . ? C8 C7 C12 C11 -6.6(16) . . . . ? O1 C7 C12 C13 -3.6(16) . . . . ? C8 C7 C12 C13 174.8(10) . . . . ? C11 C12 C13 C15 120.7(12) . . . . ? C7 C12 C13 C15 -60.7(13) . . . . ? C11 C12 C13 C16 0.6(16) . . . . ? C7 C12 C13 C16 179.2(10) . . . . ? C11 C12 C13 C14 -117.4(12) . . . . ? C7 C12 C13 C14 61.2(14) . . . . ? C9 C8 C17 C20 -5.2(17) . . . . ? C7 C8 C17 C20 175.9(11) . . . . ? C9 C8 C17 C18 -123.3(12) . . . . ? C7 C8 C17 C18 57.8(15) . . . . ? C9 C8 C17 C19 117.9(13) . . . . ? C7 C8 C17 C19 -61.1(15) . . . . ? C31 N3 C32 C33 -157.0(13) . . . . ? C30 N3 C32 C33 85.8(15) . . . . ? Li2 N3 C32 C33 -34.2(16) . . . . ? C35 N4 C33 C32 -157.2(13) . . . . ? C34 N4 C33 C32 84.4(15) . . . . ? Li2 N4 C33 C32 -29.7(15) . . . . ? N3 C32 C33 N4 46.0(18) . . . . ? Li2 O2 C36 C41 -27(27) . . . . ? Li2 O2 C36 C37 152(26) . . . . ? O2 C36 C37 C38 -175.4(9) . . . . ? C41 C36 C37 C38 4.0(15) . . . . ? O2 C36 C37 C46 9.9(15) . . . . ? C41 C36 C37 C46 -170.6(10) . . . . ? C36 C37 C38 C39 -0.8(17) . . . . ? C46 C37 C38 C39 173.6(11) . . . . ? C37 C38 C39 C40 -2.1(18) . . . . ? C37 C38 C39 C50 178.1(11) . . . . ? C38 C39 C40 C41 1.9(18) . . . . ? C50 C39 C40 C41 -178.3(11) . . . . ? C39 C40 C41 C36 1.3(17) . . . . ? C39 C40 C41 C42 -177.6(11) . . . . ? O2 C36 C41 C40 175.1(10) . . . . ? C37 C36 C41 C40 -4.3(16) . . . . ? O2 C36 C41 C42 -6.0(15) . . . . ? C37 C36 C41 C42 174.6(10) . . . . ? C40 C41 C42 C43 4.0(15) . . . . ? C36 C41 C42 C43 -174.9(10) . . . . ? C40 C41 C42 C45 -116.1(13) . . . . ? C36 C41 C42 C45 65.0(13) . . . . ? C40 C41 C42 C44 118.0(12) . . . . ? C36 C41 C42 C44 -60.8(13) . . . . ? C38 C37 C46 C47 -122.6(12) . . . . ? C36 C37 C46 C47 51.6(13) . . . . ? C38 C37 C46 C49 1.2(15) . . . . ? C36 C37 C46 C49 175.4(10) . . . . ? C38 C37 C46 C48 118.0(12) . . . . ? C36 C37 C46 C48 -67.9(14) . . . . ? C60 N6 C62 C63 -135.7(16) . . . . ? C61 N6 C62 C63 106.5(17) . . . . ? Li3 N6 C62 C63 -18.3(19) . . . . ? C60 N6 C62 Li3 -117.4(13) . . . . ? C61 N6 C62 Li3 124.7(13) . . . . ? N6 C62 C63 N5 24(2) . . . . ? Li3 C62 C63 N5 10.8(14) . . . . ? N6 C62 C63 Li3 13.6(14) . . . . ? C65 N5 C63 C62 107.1(17) . . . . ? C64 N5 C63 C62 -131.8(16) . . . . ? Li3 N5 C63 C62 -14.4(19) . . . . ? C65 N5 C63 Li3 121.5(14) . . . . ? C64 N5 C63 Li3 -117.4(13) . . . . ? Li3 O3 C66 C67 -43(7) . . . . ? Li3 O3 C66 C71 135(7) . . . . ? O3 C66 C67 C68 177.8(9) . . . . ? C71 C66 C67 C68 0.4(14) . . . . ? O3 C66 C67 C76 -3.1(15) . . . . ? C71 C66 C67 C76 179.5(9) . . . . ? C66 C67 C68 C69 0.8(15) . . . . ? C76 C67 C68 C69 -178.4(9) . . . . ? C67 C68 C69 C70 -0.8(15) . . . . ? C67 C68 C69 C80 179.3(10) . . . . ? C68 C69 C70 C71 -0.4(16) . . . . ? C80 C69 C70 C71 179.5(10) . . . . ? C69 C70 C71 C66 1.5(16) . . . . ? C69 C70 C71 C72 179.3(10) . . . . ? O3 C66 C71 C70 -178.9(9) . . . . ? C67 C66 C71 C70 -1.5(14) . . . . ? O3 C66 C71 C72 3.3(15) . . . . ? C67 C66 C71 C72 -179.2(9) . . . . ? C70 C71 C72 C74 121.7(12) . . . . ? C66 C71 C72 C74 -60.5(13) . . . . ? C70 C71 C72 C75 -118.5(11) . . . . ? C66 C71 C72 C75 59.3(13) . . . . ? C70 C71 C72 C73 -0.4(15) . . . . ? C66 C71 C72 C73 177.3(10) . . . . ? C68 C67 C76 C79 2.3(14) . . . . ? C66 C67 C76 C79 -176.9(10) . . . . ? C68 C67 C76 C78 122.1(10) . . . . ? C66 C67 C76 C78 -57.1(12) . . . . ? C68 C67 C76 C77 -116.6(11) . . . . ? C66 C67 C76 C77 64.2(13) . . . . ? C91 N7 C92 C93 -76.0(16) . . . . ? C90 N7 C92 C93 163.9(13) . . . . ? Li4 N7 C92 C93 36.0(14) . . . . ? C91 N7 C92 Li4 -112.0(13) . . . . ? C90 N7 C92 Li4 128.0(12) . . . . ? N7 C92 C93 N8 -48.5(17) . . . . ? Li4 C92 C93 N8 -22.4(11) . . . . ? N7 C92 C93 Li4 -26.1(10) . . . . ? C95 N8 C93 C92 -86.1(14) . . . . ? C94 N8 C93 C92 156.0(13) . . . . ? Li4 N8 C93 C92 31.2(16) . . . . ? C95 N8 C93 Li4 -117.3(14) . . . . ? C94 N8 C93 Li4 124.8(14) . . . . ? Li4 O4 C96 C101 37(17) . . . . ? Li4 O4 C96 C97 -140(17) . . . . ? O4 C96 C97 C98 174.7(10) . . . . ? C101 C96 C97 C98 -3.1(15) . . . . ? O4 C96 C97 C106 -8.6(15) . . . . ? C101 C96 C97 C106 173.6(10) . . . . ? C96 C97 C98 C99 0.1(17) . . . . ? C106 C97 C98 C99 -176.5(11) . . . . ? C97 C98 C99 C100 2.6(18) . . . . ? C97 C98 C99 C110 178.6(11) . . . . ? C98 C99 C100 C101 -2.2(17) . . . . ? C110 C99 C100 C101 -178.3(11) . . . . ? O4 C96 C101 C100 -174.5(10) . . . . ? C97 C96 C101 C100 3.3(15) . . . . ? O4 C96 C101 C102 7.8(16) . . . . ? C97 C96 C101 C102 -174.3(9) . . . . ? C99 C100 C101 C96 -0.7(17) . . . . ? C99 C100 C101 C102 177.0(10) . . . . ? C96 C101 C102 C104 54.7(14) . . . . ? C100 C101 C102 C104 -123.0(12) . . . . ? C96 C101 C102 C105 -65.1(14) . . . . ? C100 C101 C102 C105 117.2(12) . . . . ? C96 C101 C102 C103 178.7(10) . . . . ? C100 C101 C102 C103 1.0(15) . . . . ? C98 C97 C106 C108 -116.6(13) . . . . ? C96 C97 C106 C108 66.9(14) . . . . ? C98 C97 C106 C107 120.6(12) . . . . ? C96 C97 C106 C107 -56.0(14) . . . . ? C98 C97 C106 C109 5.3(15) . . . . ? C96 C97 C106 C109 -171.3(10) . . . . ? C121 N9 C122 C123 80.7(14) . . . . ? C120 N9 C122 C123 -158.6(12) . . . . ? Li5 N9 C122 C123 -35.1(13) . . . . ? N9 C122 C123 N10 54.6(15) . . . . ? C125 N10 C123 C122 76.1(13) . . . . ? C124 N10 C123 C122 -163.9(10) . . . . ? Li5 N10 C123 C122 -41.1(12) . . . . ? Li5 O5 C126 C131 -62(14) . . . . ? Li5 O5 C126 C127 117(14) . . . . ? O5 C126 C127 C128 -177.4(9) . . . . ? C131 C126 C127 C128 1.3(14) . . . . ? O5 C126 C127 C136 8.3(14) . . . . ? C131 C126 C127 C136 -173.0(9) . . . . ? C126 C127 C128 C129 2.3(15) . . . . ? C136 C127 C128 C129 176.5(10) . . . . ? C127 C128 C129 C130 -3.7(16) . . . . ? C127 C128 C129 C140 177.0(10) . . . . ? C128 C129 C130 C131 1.7(15) . . . . ? C140 C129 C130 C131 -179.0(10) . . . . ? C129 C130 C131 C126 1.7(15) . . . . ? C129 C130 C131 C132 -176.9(9) . . . . ? O5 C126 C131 C130 175.5(9) . . . . ? C127 C126 C131 C130 -3.2(14) . . . . ? O5 C126 C131 C132 -5.8(14) . . . . ? C127 C126 C131 C132 175.5(9) . . . . ? C130 C131 C132 C135 -115.7(11) . . . . ? C126 C131 C132 C135 65.7(13) . . . . ? C130 C131 C132 C133 6.1(14) . . . . ? C126 C131 C132 C133 -172.5(10) . . . . ? C130 C131 C132 C134 119.5(11) . . . . ? C126 C131 C132 C134 -59.1(12) . . . . ? C128 C127 C136 C138 119.8(11) . . . . ? C126 C127 C136 C138 -66.2(13) . . . . ? C128 C127 C136 C139 0.2(14) . . . . ? C126 C127 C136 C139 174.3(9) . . . . ? C128 C127 C136 C137 -119.9(11) . . . . ? C126 C127 C136 C137 54.1(13) . . . . ? C151 N11 C152 C153 72.0(14) . . . . ? C150 N11 C152 C153 -166.5(10) . . . . ? Li6 N11 C152 C153 -42.1(12) . . . . ? C154 N12 C153 C152 -163.6(11) . . . . ? C155 N12 C153 C152 74.5(13) . . . . ? Li6 N12 C153 C152 -38.3(13) . . . . ? N11 C152 C153 N12 57.3(13) . . . . ? Li6 O6 C156 C157 107(14) . . . . ? Li6 O6 C156 C161 -73(14) . . . . ? O6 C156 C157 C158 -179.4(9) . . . . ? C161 C156 C157 C158 0.5(15) . . . . ? O6 C156 C157 C166 1.6(16) . . . . ? C161 C156 C157 C166 -178.5(9) . . . . ? C156 C157 C158 C159 2.7(16) . . . . ? C166 C157 C158 C159 -178.2(9) . . . . ? C157 C158 C159 C160 -4.1(15) . . . . ? C157 C158 C159 C170 179.0(10) . . . . ? C158 C159 C160 C161 2.2(15) . . . . ? C170 C159 C160 C161 179.2(10) . . . . ? C159 C160 C161 C156 0.9(15) . . . . ? C159 C160 C161 C162 -178.6(10) . . . . ? O6 C156 C161 C160 177.6(9) . . . . ? C157 C156 C161 C160 -2.2(14) . . . . ? O6 C156 C161 C162 -2.9(15) . . . . ? C157 C156 C161 C162 177.3(9) . . . . ? C160 C161 C162 C163 -117.6(11) . . . . ? C156 C161 C162 C163 62.9(13) . . . . ? C160 C161 C162 C165 1.4(14) . . . . ? C156 C161 C162 C165 -178.0(9) . . . . ? C160 C161 C162 C164 117.1(11) . . . . ? C156 C161 C162 C164 -62.4(12) . . . . ? C158 C157 C166 C169 -2.2(15) . . . . ? C156 C157 C166 C169 176.8(11) . . . . ? C158 C157 C166 C168 120.6(12) . . . . ? C156 C157 C166 C168 -60.4(14) . . . . ? C158 C157 C166 C167 -121.5(11) . . . . ? C156 C157 C166 C167 57.6(14) . . . . ? C7 O1 Li1 N1 79(9) . . . . ? C7 O1 Li1 N2 -123(8) . . . . ? C7 O1 Li1 C3 116(8) . . . . ? C2 N1 Li1 O1 -87(2) . . . . ? C3 N1 Li1 O1 149.5(18) . . . . ? C1 N1 Li1 O1 35(2) . . . . ? C2 N1 Li1 N2 107.9(11) . . . . ? C3 N1 Li1 N2 -15.9(12) . . . . ? C1 N1 Li1 N2 -130.3(12) . . . . ? C2 N1 Li1 C3 123.7(15) . . . . ? C1 N1 Li1 C3 -114.4(15) . . . . ? C5 N2 Li1 O1 -53(2) . . . . ? C4 N2 Li1 O1 -176.2(19) . . . . ? C6 N2 Li1 O1 67(2) . . . . ? C5 N2 Li1 N1 111.4(11) . . . . ? C4 N2 Li1 N1 -11.7(11) . . . . ? C6 N2 Li1 N1 -128.2(10) . . . . ? C5 N2 Li1 C3 102.2(10) . . . . ? C4 N2 Li1 C3 -21.0(9) . . . . ? C6 N2 Li1 C3 -137.4(10) . . . . ? N1 C3 Li1 O1 -62(3) . . . . ? C4 C3 Li1 O1 158(3) . . . . ? C4 C3 Li1 N1 -140.3(16) . . . . ? N1 C3 Li1 N2 161.3(15) . . . . ? C4 C3 Li1 N2 20.9(9) . . . . ? C36 O2 Li2 N3 -63(28) . . . . ? C36 O2 Li2 N4 111(26) . . . . ? C31 N3 Li2 O2 -60(2) . . . . ? C30 N3 Li2 O2 67(2) . . . . ? C32 N3 Li2 O2 -170.2(16) . . . . ? C31 N3 Li2 N4 124.6(13) . . . . ? C30 N3 Li2 N4 -109.0(12) . . . . ? C32 N3 Li2 N4 14.0(13) . . . . ? C33 N4 Li2 O2 -168.2(17) . . . . ? C35 N4 Li2 O2 -45(2) . . . . ? C34 N4 Li2 O2 76(2) . . . . ? C33 N4 Li2 N3 7.1(12) . . . . ? C35 N4 Li2 N3 130.1(13) . . . . ? C34 N4 Li2 N3 -109.0(12) . . . . ? C66 O3 Li3 N6 -49(8) . . . . ? C66 O3 Li3 N5 148(6) . . . . ? C66 O3 Li3 C62 -80(8) . . . . ? C66 O3 Li3 C63 165(5) . . . . ? C62 N6 Li3 O3 -161.5(16) . . . . ? C60 N6 Li3 O3 -43(2) . . . . ? C61 N6 Li3 O3 77.8(19) . . . . ? C62 N6 Li3 N5 6.8(11) . . . . ? C60 N6 Li3 N5 125.6(11) . . . . ? C61 N6 Li3 N5 -113.9(11) . . . . ? C60 N6 Li3 C62 118.8(14) . . . . ? C61 N6 Li3 C62 -120.7(15) . . . . ? C62 N6 Li3 C63 8.6(9) . . . . ? C60 N6 Li3 C63 127.4(11) . . . . ? C61 N6 Li3 C63 -112.1(12) . . . . ? C65 N5 Li3 O3 49.5(18) . . . . ? C64 N5 Li3 O3 -73.1(18) . . . . ? C63 N5 Li3 O3 171.5(15) . . . . ? C65 N5 Li3 N6 -119.0(11) . . . . ? C64 N5 Li3 N6 118.4(10) . . . . ? C63 N5 Li3 N6 2.9(11) . . . . ? C65 N5 Li3 C62 -115.0(11) . . . . ? C64 N5 Li3 C62 122.4(11) . . . . ? C63 N5 Li3 C62 7.0(9) . . . . ? C65 N5 Li3 C63 -122.0(15) . . . . ? C64 N5 Li3 C63 115.4(14) . . . . ? C63 C62 Li3 O3 -149(4) . . . . ? N6 C62 Li3 O3 47(4) . . . . ? C63 C62 Li3 N6 164.3(17) . . . . ? C63 C62 Li3 N5 -7.7(10) . . . . ? N6 C62 Li3 N5 -172.0(13) . . . . ? N6 C62 Li3 C63 -164.3(17) . . . . ? C62 C63 Li3 O3 144(4) . . . . ? N5 C63 Li3 O3 -24(4) . . . . ? C62 C63 Li3 N6 -9.4(10) . . . . ? N5 C63 Li3 N6 -176.5(13) . . . . ? C62 C63 Li3 N5 167.2(17) . . . . ? N5 C63 Li3 C62 -167.2(17) . . . . ? C96 O4 Li4 N8 58(18) . . . . ? C96 O4 Li4 N7 -121(16) . . . . ? C96 O4 Li4 C92 -89(17) . . . . ? C96 O4 Li4 C93 72(19) . . . . ? C95 N8 Li4 O4 -70(2) . . . . ? C93 N8 Li4 O4 172.8(17) . . . . ? C94 N8 Li4 O4 51(2) . . . . ? C95 N8 Li4 N7 109.6(12) . . . . ? C93 N8 Li4 N7 -7.6(12) . . . . ? C94 N8 Li4 N7 -129.5(10) . . . . ? C95 N8 Li4 C92 100.8(12) . . . . ? C93 N8 Li4 C92 -16.4(9) . . . . ? C94 N8 Li4 C92 -138.3(10) . . . . ? C95 N8 Li4 C93 117.2(16) . . . . ? C94 N8 Li4 C93 -121.9(14) . . . . ? C91 N7 Li4 O4 -79(2) . . . . ? C90 N7 Li4 O4 44(2) . . . . ? C92 N7 Li4 O4 165.4(17) . . . . ? C91 N7 Li4 N8 101.8(10) . . . . ? C90 N7 Li4 N8 -135.8(11) . . . . ? C92 N7 Li4 N8 -14.2(11) . . . . ? C91 N7 Li4 C92 116.0(11) . . . . ? C90 N7 Li4 C92 -121.6(13) . . . . ? C91 N7 Li4 C93 97.3(9) . . . . ? C90 N7 Li4 C93 -140.3(11) . . . . ? C92 N7 Li4 C93 -18.7(8) . . . . ? C93 C92 Li4 O4 170(5) . . . . ? N7 C92 Li4 O4 -44(4) . . . . ? C93 C92 Li4 N8 16.9(9) . . . . ? N7 C92 Li4 N8 163.2(13) . . . . ? C93 C92 Li4 N7 -146.3(14) . . . . ? N7 C92 Li4 C93 146.3(14) . . . . ? C92 C93 Li4 O4 -170(5) . . . . ? N8 C93 Li4 O4 -20(4) . . . . ? C92 C93 Li4 N8 -150.9(16) . . . . ? C92 C93 Li4 N7 20.1(8) . . . . ? N8 C93 Li4 N7 171.0(15) . . . . ? N8 C93 Li4 C92 150.9(16) . . . . ? C126 O5 Li5 N10 -39(15) . . . . ? C126 O5 Li5 N9 155(13) . . . . ? C125 N10 Li5 O5 84.8(17) . . . . ? C124 N10 Li5 O5 -37(2) . . . . ? C123 N10 Li5 O5 -153.9(14) . . . . ? C125 N10 Li5 N9 -104.9(11) . . . . ? C124 N10 Li5 N9 133.7(10) . . . . ? C123 N10 Li5 N9 16.4(9) . . . . ? C121 N9 Li5 O5 61.7(17) . . . . ? C122 N9 Li5 O5 179.2(14) . . . . ? C120 N9 Li5 O5 -62.4(17) . . . . ? C121 N9 Li5 N10 -108.8(10) . . . . ? C122 N9 Li5 N10 8.7(10) . . . . ? C120 N9 Li5 N10 127.1(9) . . . . ? C156 O6 Li6 N11 151(13) . . . . ? C156 O6 Li6 N12 -23(15) . . . . ? C151 N11 Li6 O6 80.3(19) . . . . ? C150 N11 Li6 O6 -42(2) . . . . ? C152 N11 Li6 O6 -159.5(17) . . . . ? C151 N11 Li6 N12 -104.0(10) . . . . ? C150 N11 Li6 N12 133.7(10) . . . . ? C152 N11 Li6 N12 16.1(10) . . . . ? C154 N12 Li6 O6 -54(2) . . . . ? C153 N12 Li6 O6 -172.2(16) . . . . ? C155 N12 Li6 O6 67(2) . . . . ? C154 N12 Li6 N11 130.6(12) . . . . ? C153 N12 Li6 N11 11.9(10) . . . . ? C155 N12 Li6 N11 -108.5(11) . . . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.339 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.057 #===END data_Compound_2a_k08mgd17 _database_code_depnum_ccdc_archive 'CCDC 778586' #TrackingRef '- LiOAr.cif' _audit_creation_date 2008-05-27T10:18:55-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C42 H66 Li4 N6 O4' _chemical_formula_weight 746.77 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5790(3) _cell_length_b 10.8690(3) _cell_length_c 12.0730(3) _cell_angle_alpha 114.8640(10) _cell_angle_beta 96.0450(10) _cell_angle_gamma 112.8760(10) _cell_volume 1098.84(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7165 _cell_measurement_theta_min 3.513 _cell_measurement_theta_max 27.485 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_orient_matrix_UB_11 -0.0378199 _diffrn_orient_matrix_UB_21 0.0206113 _diffrn_orient_matrix_UB_31 -0.0994240 _diffrn_orient_matrix_UB_12 0.0618780 _diffrn_orient_matrix_UB_22 -0.0348182 _diffrn_orient_matrix_UB_32 -0.0912106 _diffrn_orient_matrix_UB_13 -0.0203361 _diffrn_orient_matrix_UB_23 -0.0836598 _diffrn_orient_matrix_UB_33 -0.0433874 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_unetI/netI 0.0577 _diffrn_reflns_number 13042 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.8 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 5013 _reflns_number_gt 3402 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+0.2566P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.031(4) _refine_ls_number_reflns 5013 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1256 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.16 _refine_diff_density_min -0.234 _refine_diff_density_rms 0.034 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O2 O 0.36712(10) 0.88022(10) 0.40502(9) 0.0315(2) Uani 1 1 d . . . O1 O 0.58643(12) 0.89562(12) 0.27926(10) 0.0403(3) Uani 1 1 d . . . C21 C 0.26482(15) 0.74100(15) 0.37624(12) 0.0280(3) Uani 1 1 d . . . C26 C 0.27531(16) 0.60749(16) 0.30264(14) 0.0350(3) Uani 1 1 d . . . H26 H 0.3544 0.6156 0.2701 0.042 Uiso 1 1 calc R . . C22 C 0.14423(16) 0.72179(17) 0.41866(14) 0.0347(3) Uani 1 1 d . . . H22 H 0.1328 0.8096 0.4671 0.042 Uiso 1 1 calc R . . C12 C 0.63391(17) 0.73902(17) 0.09849(15) 0.0375(4) Uani 1 1 d . . . H12 H 0.5465 0.6501 0.0773 0.045 Uiso 1 1 calc R . . C11 C 0.67086(16) 0.88185(17) 0.20692(14) 0.0338(3) Uani 1 1 d . . . N1 N 0.24938(19) 0.77248(17) 0.07963(14) 0.0554(4) Uani 1 1 d . . . N3 N 0.31683(16) 1.20706(16) 0.51913(14) 0.0502(4) Uani 1 1 d . . . C14 C 0.85055(18) 0.85240(19) 0.04997(15) 0.0406(4) Uani 1 1 d . . . H14 H 0.9101 0.8428 -0.0034 0.049 Uiso 1 1 calc R . . C15 C 0.89015(17) 0.99295(18) 0.15668(15) 0.0375(3) Uani 1 1 d . . . H15 H 0.9786 1.0806 0.1776 0.045 Uiso 1 1 calc R . . C13 C 0.72216(18) 0.72554(18) 0.02229(15) 0.0412(4) Uani 1 1 d . . . H13 H 0.6943 0.6277 -0.0502 0.049 Uiso 1 1 calc R . . C23 C 0.04143(18) 0.57806(19) 0.39168(16) 0.0433(4) Uani 1 1 d . . . H23 H -0.0392 0.5686 0.422 0.052 Uiso 1 1 calc R . . C25 C 0.17183(19) 0.46400(17) 0.27683(15) 0.0439(4) Uani 1 1 d . . . H25 H 0.1818 0.3753 0.2279 0.053 Uiso 1 1 calc R . . C16 C 0.80290(17) 1.00806(17) 0.23370(15) 0.0370(3) Uani 1 1 d . . . H16 H 0.8329 1.1063 0.3066 0.044 Uiso 1 1 calc R . . C24 C 0.0544(2) 0.44765(19) 0.32099(16) 0.0480(4) Uani 1 1 d . . . H24 H -0.016 0.349 0.3032 0.058 Uiso 1 1 calc R . . Li2 Li 0.4208(3) 1.0763(3) 0.5564(2) 0.0352(5) Uani 1 1 d . . . Li1 Li 0.4106(3) 0.9023(3) 0.2612(2) 0.0400(6) Uani 1 1 d . . . N2 N 0.43521(15) 1.10839(15) 0.25588(13) 0.0416(3) Uani 1 1 d . . . C1 C 0.2598(2) 0.6422(2) -0.01457(19) 0.0571(5) Uani 1 1 d . . . H1A H 0.2447 0.5677 0.0148 0.086 Uiso 1 1 calc R . . H1B H 0.356 0.6786 -0.0246 0.086 Uiso 1 1 calc R . . H1C H 0.1856 0.5924 -0.0976 0.086 Uiso 1 1 calc R . . C9 C 0.3688(2) 1.3584(2) 0.6258(2) 0.0711(6) Uani 1 1 d . B . H9A H 0.308 1.402 0.6103 0.107 Uiso 1 1 calc R . . H9B H 0.469 1.4244 0.6359 0.107 Uiso 1 1 calc R . . H9C H 0.3652 1.3528 0.7044 0.107 Uiso 1 1 calc R . . C2 C 0.1044(3) 0.7168(3) 0.0899(2) 0.0718(6) Uani 1 1 d . . . H2A H 0.0329 0.6675 0.0055 0.108 Uiso 1 1 calc R . . H2B H 0.0954 0.804 0.1524 0.108 Uiso 1 1 calc R . . H2C H 0.0873 0.6415 0.1186 0.108 Uiso 1 1 calc R . . C5 C 0.5863(6) 1.1723(11) 0.2463(12) 0.0574(16) Uani 0.63(2) 1 d P A 1 H5A H 0.6065 1.2604 0.2333 0.086 Uiso 0.63(2) 1 calc PR A 1 H5B H 0.5929 1.0917 0.1734 0.086 Uiso 0.63(2) 1 calc PR A 1 H5C H 0.6571 1.2062 0.3262 0.086 Uiso 0.63(2) 1 calc PR A 1 C8 C 0.1647(3) 1.1255(4) 0.5350(4) 0.0524(11) Uani 0.668(8) 1 d P B 1 H8A H 0.1017 1.1638 0.5128 0.079 Uiso 0.668(8) 1 calc PR B 1 H8B H 0.1785 1.1487 0.6244 0.079 Uiso 0.668(8) 1 calc PR B 1 H8C H 0.1197 1.0134 0.4774 0.079 Uiso 0.668(8) 1 calc PR B 1 C6 C 0.4308(3) 1.2293(3) 0.3648(3) 0.0522(8) Uani 0.658(4) 1 d P A 1 H6A H 0.4429 1.314 0.3476 0.063 Uiso 0.658(4) 1 calc PR A 1 H6B H 0.5124 1.2717 0.4416 0.063 Uiso 0.658(4) 1 calc PR A 1 C4 C 0.3311(5) 1.0453(4) 0.1336(4) 0.0541(11) Uani 0.677(9) 1 d P A 1 H4A H 0.3667 1.1176 0.1008 0.065 Uiso 0.677(9) 1 calc PR A 1 H4B H 0.2388 1.0391 0.1478 0.065 Uiso 0.677(9) 1 calc PR A 1 C7 C 0.2884(3) 1.1711(4) 0.3927(3) 0.0520(8) Uani 0.658(4) 1 d P A 1 H7A H 0.2325 1.2197 0.3758 0.062 Uiso 0.658(4) 1 calc PR A 1 H7B H 0.2297 1.0578 0.3355 0.062 Uiso 0.658(4) 1 calc PR A 1 C3 C 0.3014(6) 0.8886(4) 0.0325(3) 0.0536(11) Uani 0.677(9) 1 d P A 1 H3A H 0.3907 0.8953 0.0111 0.064 Uiso 0.677(9) 1 calc PR A 1 H3B H 0.2264 0.8523 -0.0468 0.064 Uiso 0.677(9) 1 calc PR A 1 C7' C 0.3745(5) 1.2963(5) 0.4329(4) 0.0379(13) Uani 0.342(4) 1 d P A 2 H7'1 H 0.3292 1.3629 0.442 0.046 Uiso 0.342(4) 1 calc PR A 2 H7'2 H 0.4804 1.3653 0.4737 0.046 Uiso 0.342(4) 1 calc PR A 2 C6' C 0.3456(6) 1.1963(6) 0.2910(5) 0.0402(13) Uani 0.342(4) 1 d P A 2 H6'1 H 0.3649 1.2623 0.2514 0.048 Uiso 0.342(4) 1 calc PR A 2 H6'2 H 0.2414 1.1192 0.2513 0.048 Uiso 0.342(4) 1 calc PR A 2 C5' C 0.5848(10) 1.2186(13) 0.3026(13) 0.046(2) Uani 0.37(2) 1 d P A 2 H5'1 H 0.6408 1.165 0.2719 0.069 Uiso 0.37(2) 1 calc PR A 2 H5'2 H 0.618 1.2755 0.3971 0.069 Uiso 0.37(2) 1 calc PR A 2 H5'3 H 0.5985 1.291 0.2711 0.069 Uiso 0.37(2) 1 calc PR A 2 C8' C 0.1806(6) 1.1023(6) 0.4518(8) 0.046(2) Uani 0.332(8) 1 d P B 2 H8'1 H 0.1263 1.152 0.4364 0.068 Uiso 0.332(8) 1 calc PR B 2 H8'2 H 0.1385 1.0524 0.4999 0.068 Uiso 0.332(8) 1 calc PR B 2 H8'3 H 0.1757 1.0244 0.3691 0.068 Uiso 0.332(8) 1 calc PR B 2 C3' C 0.2327(9) 0.8845(6) 0.0511(6) 0.0349(16) Uani 0.323(9) 1 d P A 2 H3'1 H 0.1654 0.916 0.0911 0.042 Uiso 0.323(9) 1 calc PR A 2 H3'2 H 0.1961 0.8415 -0.0431 0.042 Uiso 0.323(9) 1 calc PR A 2 C4' C 0.3857(9) 1.0201(7) 0.1100(6) 0.0356(16) Uani 0.323(9) 1 d P A 2 H4'1 H 0.4534 0.9811 0.081 0.043 Uiso 0.323(9) 1 calc PR A 2 H4'2 H 0.3894 1.0915 0.0783 0.043 Uiso 0.323(9) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O2 0.0284(5) 0.0273(5) 0.0364(5) 0.0154(4) 0.0127(4) 0.0114(4) O1 0.0424(6) 0.0397(6) 0.0435(6) 0.0214(5) 0.0261(5) 0.0202(5) C21 0.0286(7) 0.0271(7) 0.0264(7) 0.0143(5) 0.0074(5) 0.0109(6) C26 0.0367(8) 0.0335(8) 0.0346(8) 0.0159(6) 0.0145(6) 0.0173(6) C22 0.0352(8) 0.0337(8) 0.0360(8) 0.0172(6) 0.0157(6) 0.0165(6) C12 0.0398(9) 0.0328(8) 0.0427(8) 0.0193(7) 0.0177(7) 0.0184(7) C11 0.0375(8) 0.0360(8) 0.0365(8) 0.0213(6) 0.0184(6) 0.0203(6) N1 0.0697(11) 0.0453(8) 0.0474(8) 0.0240(7) 0.0030(7) 0.0274(8) N3 0.0478(9) 0.0419(8) 0.0552(9) 0.0146(7) 0.0063(7) 0.0297(7) C14 0.0425(9) 0.0536(10) 0.0430(9) 0.0280(8) 0.0237(7) 0.0319(8) C15 0.0315(8) 0.0432(8) 0.0441(9) 0.0259(7) 0.0160(6) 0.0184(7) C13 0.0514(10) 0.0399(8) 0.0385(8) 0.0171(7) 0.0188(7) 0.0292(8) C23 0.0375(9) 0.0422(9) 0.0458(9) 0.0229(7) 0.0208(7) 0.0124(7) C25 0.0589(11) 0.0288(8) 0.0387(8) 0.0139(7) 0.0174(8) 0.0193(7) C16 0.0391(9) 0.0343(8) 0.0373(8) 0.0170(6) 0.0162(7) 0.0176(7) C24 0.0542(11) 0.0317(8) 0.0431(9) 0.0189(7) 0.0167(8) 0.0070(7) Li2 0.0336(13) 0.0315(12) 0.0413(13) 0.0175(11) 0.0143(10) 0.0166(10) Li1 0.0439(15) 0.0404(14) 0.0400(14) 0.0247(11) 0.0142(11) 0.0188(12) N2 0.0418(8) 0.0429(8) 0.0494(8) 0.0294(6) 0.0184(6) 0.0208(6) C1 0.0541(11) 0.0633(12) 0.0578(11) 0.0322(10) 0.0147(9) 0.0308(10) C9 0.0680(14) 0.0560(12) 0.0748(14) 0.0122(10) 0.0062(11) 0.0437(11) C2 0.0758(15) 0.0895(16) 0.0489(11) 0.0203(11) 0.0058(10) 0.0581(13) C5 0.051(2) 0.059(3) 0.087(5) 0.052(3) 0.036(3) 0.028(2) C8 0.0379(15) 0.0600(18) 0.080(3) 0.0442(18) 0.0267(15) 0.0301(13) C6 0.0453(17) 0.0500(16) 0.0597(19) 0.0281(14) 0.0195(15) 0.0202(13) C4 0.068(3) 0.059(2) 0.059(2) 0.0448(17) 0.0217(17) 0.0353(18) C7 0.0400(15) 0.0564(19) 0.0526(17) 0.0252(14) 0.0142(12) 0.0196(14) C3 0.067(3) 0.064(2) 0.0525(18) 0.0415(16) 0.0271(17) 0.0362(19) C7' 0.044(3) 0.037(3) 0.046(3) 0.026(2) 0.018(2) 0.025(2) C6' 0.046(3) 0.050(3) 0.046(3) 0.032(2) 0.023(2) 0.032(2) C5' 0.044(3) 0.042(4) 0.058(5) 0.032(4) 0.015(3) 0.018(3) C8' 0.036(3) 0.051(3) 0.063(5) 0.037(3) 0.023(3) 0.022(2) C3' 0.033(4) 0.039(3) 0.033(3) 0.020(2) 0.010(2) 0.014(3) C4' 0.044(4) 0.035(3) 0.036(3) 0.021(2) 0.018(2) 0.022(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O2 C21 1.3368(16) . ? O2 Li1 1.928(3) . ? O2 Li2 1.942(3) . ? O2 Li2 2.061(3) 2_676 ? O1 C11 1.3195(17) . ? O1 Li1 1.883(3) . ? O1 Li2 1.891(3) 2_676 ? C21 C22 1.3978(19) . ? C21 C26 1.4033(19) . ? C26 C25 1.386(2) . ? C26 H26 0.95 . ? C22 C23 1.381(2) . ? C22 H22 0.95 . ? C12 C13 1.383(2) . ? C12 C11 1.410(2) . ? C12 H12 0.95 . ? C11 C16 1.407(2) . ? N1 C1 1.450(2) . ? N1 C2 1.454(3) . ? N1 C3' 1.463(6) . ? N1 C3 1.533(4) . ? N1 Li1 2.109(3) . ? N3 C8' 1.316(5) . ? N3 C7 1.372(3) . ? N3 C9 1.425(2) . ? N3 C8 1.585(4) . ? N3 C7' 1.709(5) . ? N3 Li2 2.254(3) . ? C14 C15 1.379(2) . ? C14 C13 1.385(2) . ? C14 H14 0.95 . ? C15 C16 1.383(2) . ? C15 H15 0.95 . ? C13 H13 0.95 . ? C23 C24 1.384(2) . ? C23 H23 0.95 . ? C25 C24 1.381(2) . ? C25 H25 0.95 . ? C16 H16 0.95 . ? C24 H24 0.95 . ? Li2 O1 1.891(3) 2_676 ? Li2 O2 2.061(3) 2_676 ? Li2 Li1 2.550(4) 2_676 ? Li2 Li2 2.858(5) 2_676 ? Li1 N2 2.182(3) . ? Li1 Li2 2.550(4) 2_676 ? N2 C5' 1.424(9) . ? N2 C6 1.437(3) . ? N2 C4 1.443(4) . ? N2 C4' 1.513(6) . ? N2 C5 1.514(5) . ? N2 C6' 1.562(5) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C6 C7 1.526(4) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C4 C3 1.499(7) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C7' C6' 1.508(7) . ? C7' H7'1 0.99 . ? C7' H7'2 0.99 . ? C6' H6'1 0.99 . ? C6' H6'2 0.99 . ? C5' H5'1 0.98 . ? C5' H5'2 0.98 . ? C5' H5'3 0.98 . ? C8' H8'1 0.98 . ? C8' H8'2 0.98 . ? C8' H8'3 0.98 . ? C3' C4' 1.523(11) . ? C3' H3'1 0.99 . ? C3' H3'2 0.99 . ? C4' H4'1 0.99 . ? C4' H4'2 0.99 . ? 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 C21 O2 Li1 116.17(11) . . ? C21 O2 Li2 126.40(11) . . ? Li1 O2 Li2 112.77(12) . . ? C21 O2 Li2 117.82(11) . 2_676 ? Li1 O2 Li2 79.42(11) . 2_676 ? Li2 O2 Li2 91.05(11) . 2_676 ? C11 O1 Li1 134.88(13) . . ? C11 O1 Li2 140.06(13) . 2_676 ? Li1 O1 Li2 85.03(12) . 2_676 ? O2 C21 C22 121.90(12) . . ? O2 C21 C26 120.94(12) . . ? C22 C21 C26 117.15(12) . . ? C25 C26 C21 120.84(14) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? C23 C22 C21 121.44(14) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C13 C12 C11 121.45(14) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? O1 C11 C16 122.12(13) . . ? O1 C11 C12 121.69(13) . . ? C16 C11 C12 116.19(13) . . ? C1 N1 C2 108.58(16) . . ? C1 N1 C3' 122.5(3) . . ? C2 N1 C3' 90.8(4) . . ? C1 N1 C3 102.8(2) . . ? C2 N1 C3 119.7(3) . . ? C3' N1 C3 29.8(2) . . ? C1 N1 Li1 114.46(14) . . ? C2 N1 Li1 111.81(14) . . ? C3' N1 Li1 106.3(2) . . ? C3 N1 Li1 99.22(19) . . ? C8' N3 C7 69.1(4) . . ? C8' N3 C9 126.9(3) . . ? C7 N3 C9 124.3(2) . . ? C8' N3 C8 38.0(3) . . ? C7 N3 C8 106.0(2) . . ? C9 N3 C8 98.3(2) . . ? C8' N3 C7' 105.4(4) . . ? C7 N3 C7' 41.8(2) . . ? C9 N3 C7' 86.1(2) . . ? C8 N3 C7' 133.9(2) . . ? C8' N3 Li2 104.6(3) . . ? C7 N3 Li2 110.99(17) . . ? C9 N3 Li2 113.27(13) . . ? C8 N3 Li2 99.63(14) . . ? C7' N3 Li2 120.73(19) . . ? C15 C14 C13 118.59(14) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C14 C15 C16 120.95(14) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C12 C13 C14 121.05(14) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C22 C23 C24 120.84(15) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C24 C25 C26 121.13(15) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C15 C16 C11 121.76(14) . . ? C15 C16 H16 119.1 . . ? C11 C16 H16 119.1 . . ? C25 C24 C23 118.58(15) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? O1 Li2 O2 125.12(14) 2_676 . ? O1 Li2 O2 94.03(12) 2_676 2_676 ? O2 Li2 O2 88.95(10) . 2_676 ? O1 Li2 N3 105.04(12) 2_676 . ? O2 Li2 N3 113.28(13) . . ? O2 Li2 N3 131.41(13) 2_676 . ? O1 Li2 Li1 47.35(9) 2_676 2_676 ? O2 Li2 Li1 106.12(12) . 2_676 ? O2 Li2 Li1 47.99(9) 2_676 2_676 ? N3 Li2 Li1 140.59(13) . 2_676 ? O1 Li2 Li2 116.21(15) 2_676 2_676 ? O2 Li2 Li2 46.14(8) . 2_676 ? O2 Li2 Li2 42.81(7) 2_676 2_676 ? N3 Li2 Li2 138.21(16) . 2_676 ? Li1 Li2 Li2 72.91(12) 2_676 2_676 ? O1 Li1 O2 98.79(13) . . ? O1 Li1 N1 121.00(15) . . ? O2 Li1 N1 120.78(14) . . ? O1 Li1 N2 111.49(13) . . ? O2 Li1 N2 118.95(14) . . ? N1 Li1 N2 87.01(11) . . ? O1 Li1 Li2 47.62(9) . 2_676 ? O2 Li1 Li2 52.59(9) . 2_676 ? N1 Li1 Li2 151.75(14) . 2_676 ? N2 Li1 Li2 120.80(13) . 2_676 ? C5' N2 C6 82.6(7) . . ? C5' N2 C4 127.3(5) . . ? C6 N2 C4 115.7(3) . . ? C5' N2 C4' 108.9(7) . . ? C6 N2 C4' 142.9(4) . . ? C4 N2 C4' 29.8(2) . . ? C5' N2 C5 25.7(3) . . ? C6 N2 C5 107.6(5) . . ? C4 N2 C5 109.0(5) . . ? C4' N2 C5 85.1(6) . . ? C5' N2 C6' 108.8(6) . . ? C6 N2 C6' 39.6(2) . . ? C4 N2 C6' 76.2(3) . . ? C4' N2 C6' 104.7(4) . . ? C5 N2 C6' 126.2(4) . . ? C5' N2 Li1 109.8(4) . . ? C6 N2 Li1 118.90(16) . . ? C4 N2 Li1 102.96(17) . . ? C4' N2 Li1 91.0(3) . . ? C5 N2 Li1 101.5(2) . . ? C6' N2 Li1 130.3(2) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? N2 C6 C7 111.8(2) . . ? N2 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? N2 C6 H6B 109.3 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? N2 C4 C3 114.7(4) . . ? N2 C4 H4A 108.6 . . ? C3 C4 H4A 108.6 . . ? N2 C4 H4B 108.6 . . ? C3 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? N3 C7 C6 109.5(2) . . ? N3 C7 H7A 109.8 . . ? C6 C7 H7A 109.8 . . ? N3 C7 H7B 109.8 . . ? C6 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? C4 C3 N1 110.9(3) . . ? C4 C3 H3A 109.5 . . ? N1 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C6' C7' N3 118.1(3) . . ? C6' C7' H7'1 107.8 . . ? N3 C7' H7'1 107.8 . . ? C6' C7' H7'2 107.8 . . ? N3 C7' H7'2 107.8 . . ? H7'1 C7' H7'2 107.1 . . ? C7' C6' N2 116.1(4) . . ? C7' C6' H6'1 108.3 . . ? N2 C6' H6'1 108.3 . . ? C7' C6' H6'2 108.3 . . ? N2 C6' H6'2 108.3 . . ? H6'1 C6' H6'2 107.4 . . ? N2 C5' H5'1 109.5 . . ? N2 C5' H5'2 109.5 . . ? H5'1 C5' H5'2 109.5 . . ? N2 C5' H5'3 109.5 . . ? H5'1 C5' H5'3 109.5 . . ? H5'2 C5' H5'3 109.5 . . ? N3 C8' H8'1 109.5 . . ? N3 C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? N3 C8' H8'3 109.5 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? N1 C3' C4' 103.5(6) . . ? N1 C3' H3'1 111.1 . . ? C4' C3' H3'1 111.1 . . ? N1 C3' H3'2 111.1 . . ? C4' C3' H3'2 111.1 . . ? H3'1 C3' H3'2 109 . . ? N2 C4' C3' 112.8(6) . . ? N2 C4' H4'1 109 . . ? C3' C4' H4'1 109 . . ? N2 C4' H4'2 109 . . ? C3' C4' H4'2 109 . . ? H4'1 C4' H4'2 107.8 . . ? #===END data_Compound_2b_k08mgd07 _database_code_depnum_ccdc_archive 'CCDC 778587' #TrackingRef '- LiOAr.cif' _audit_creation_date 2008-03-03T22:57:37-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common k08mgd07 _chemical_formula_moiety 'C54 H90 Li4 N6 O4' _chemical_formula_sum 'C54 H90 Li4 N6 O4' _chemical_formula_weight 915.1068 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6420(3) _cell_length_b 11.7200(3) _cell_length_c 12.6870(5) _cell_angle_alpha 102.0700(10) _cell_angle_beta 92.7850(10) _cell_angle_gamma 110.697(2) _cell_volume 1434.49(8) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14116 _cell_measurement_theta_min 3.513 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.092168 _diffrn_orient_matrix_ub_12 -0.0287181 _diffrn_orient_matrix_ub_13 0.0233812 _diffrn_orient_matrix_ub_21 -0.0410425 _diffrn_orient_matrix_ub_22 -0.0408675 _diffrn_orient_matrix_ub_23 -0.077484 _diffrn_orient_matrix_ub_31 0.0097586 _diffrn_orient_matrix_ub_32 -0.0796373 _diffrn_orient_matrix_ub_33 0.0080791 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_unetI/netI 0.0693 _diffrn_reflns_number 20396 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.83 _diffrn_reflns_theta_max 27.42 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 6482 _reflns_number_gt 4284 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+0.2053P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 6482 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1285 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.155 _refine_diff_density_min -0.157 _refine_diff_density_rms 0.034 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O -0.02615(10) -0.12055(9) 0.43994(9) 0.0349(3) Uani 1 1 d . . . N1 N 0.02372(12) -0.23380(12) 0.71308(11) 0.0358(3) Uani 1 1 d . . . C1 C 0.12318(16) -0.11900(16) 0.69269(16) 0.0475(4) Uani 1 1 d . . . H1A H 0.2114 -0.1275 0.6896 0.071 Uiso 1 1 calc R . . H1B H 0.1315 -0.0467 0.7516 0.071 Uiso 1 1 calc R . . H1C H 0.0929 -0.1064 0.6233 0.071 Uiso 1 1 calc R . . Li1 Li -0.0980(3) -0.0451(2) 0.5533(2) 0.0359(6) Uani 1 1 d . . . O2 O -0.21054(10) -0.10991(9) 0.65216(8) 0.0324(2) Uani 1 1 d . . . N2 N -0.23893(12) -0.42851(12) 0.60904(11) 0.0347(3) Uani 1 1 d . . . C2 C 0.07269(19) -0.2526(2) 0.81543(15) 0.0532(5) Uani 1 1 d . . . H2A H 0.007 -0.3285 0.8305 0.08 Uiso 1 1 calc R . . H2B H 0.0838 -0.1798 0.8747 0.08 Uiso 1 1 calc R . . H2C H 0.1601 -0.2622 0.8097 0.08 Uiso 1 1 calc R . . Li2 Li -0.1825(2) -0.2392(2) 0.7012(2) 0.0345(6) Uani 1 1 d . . . N3 N -0.31158(13) -0.32238(12) 0.81489(11) 0.0384(3) Uani 1 1 d . . . C3 C 0.00919(16) -0.34024(15) 0.62168(14) 0.0412(4) Uani 1 1 d . . . H3A H 0.0911 -0.3614 0.6266 0.049 Uiso 1 1 calc R . . H3B H 0.0021 -0.3153 0.5524 0.049 Uiso 1 1 calc R . . C4 C -0.11376(16) -0.45455(15) 0.62114(14) 0.0405(4) Uani 1 1 d . . . H4A H -0.1177 -0.5248 0.5604 0.049 Uiso 1 1 calc R . . H4B H -0.1066 -0.4804 0.69 0.049 Uiso 1 1 calc R . . C5 C -0.28606(19) -0.44866(18) 0.49377(14) 0.0516(5) Uani 1 1 d . . . H5A H -0.3139 -0.538 0.4578 0.077 Uiso 1 1 calc R . . H5B H -0.2125 -0.399 0.4593 0.077 Uiso 1 1 calc R . . H5C H -0.3634 -0.4225 0.4871 0.077 Uiso 1 1 calc R . . C6 C -0.34662(17) -0.50616(15) 0.66207(14) 0.0417(4) Uani 1 1 d . . . H6A H -0.3488 -0.5933 0.6453 0.05 Uiso 1 1 calc R . . H6B H -0.4356 -0.5086 0.6324 0.05 Uiso 1 1 calc R . . C7 C -0.32364(17) -0.45479(15) 0.78382(14) 0.0407(4) Uani 1 1 d . . . H7A H -0.4001 -0.5064 0.8158 0.049 Uiso 1 1 calc R . . H7B H -0.2398 -0.4615 0.8143 0.049 Uiso 1 1 calc R . . C8 C -0.2657(2) -0.27154(18) 0.93189(15) 0.0542(5) Uani 1 1 d . . . H8A H -0.3325 -0.3194 0.9725 0.081 Uiso 1 1 calc R . . H8B H -0.2557 -0.1831 0.952 0.081 Uiso 1 1 calc R . . H8C H -0.1782 -0.2782 0.9494 0.081 Uiso 1 1 calc R . . C9 C -0.44381(18) -0.31326(17) 0.79093(17) 0.0518(5) Uani 1 1 d . . . H9A H -0.473 -0.3415 0.7123 0.078 Uiso 1 1 calc R . . H9B H -0.4359 -0.2258 0.8164 0.078 Uiso 1 1 calc R . . H9C H -0.5107 -0.3664 0.8282 0.078 Uiso 1 1 calc R . . C11 C -0.06171(15) -0.21530(13) 0.35147(12) 0.0307(3) Uani 1 1 d . . . C12 C 0.03219(15) -0.26805(13) 0.31106(12) 0.0328(3) Uani 1 1 d . . . C13 C -0.00735(18) -0.36362(15) 0.21631(13) 0.0397(4) Uani 1 1 d . . . H13 H 0.0574 -0.3968 0.189 0.048 Uiso 1 1 calc R . . C14 C -0.13771(18) -0.41280(15) 0.15964(14) 0.0431(4) Uani 1 1 d . . . C15 C -0.22942(17) -0.36144(15) 0.20167(14) 0.0404(4) Uani 1 1 d . . . H15 H -0.3193 -0.3937 0.1649 0.048 Uiso 1 1 calc R . . C16 C -0.19494(15) -0.26488(14) 0.29509(13) 0.0340(3) Uani 1 1 d . . . C17 C 0.17431(15) -0.21878(14) 0.36976(14) 0.0382(4) Uani 1 1 d . . . H17A H 0.174 -0.2519 0.4346 0.057 Uiso 1 1 calc R . . H17B H 0.2084 -0.1267 0.3915 0.057 Uiso 1 1 calc R . . H17C H 0.233 -0.2456 0.3214 0.057 Uiso 1 1 calc R . . C18 C -0.1793(2) -0.51700(19) 0.05711(17) 0.0656(6) Uani 1 1 d . . . H18A H -0.1021 -0.5412 0.0398 0.098 Uiso 0.5 1 calc PR . . H18B H -0.2087 -0.4877 -0.003 0.098 Uiso 0.5 1 calc PR . . H18C H -0.2542 -0.5897 0.068 0.098 Uiso 0.5 1 calc PR . . H18D H -0.2746 -0.5379 0.03 0.098 Uiso 0.5 1 calc PR . . H18E H -0.168 -0.5914 0.0729 0.098 Uiso 0.5 1 calc PR . . H18F H -0.1225 -0.4894 0.0018 0.098 Uiso 0.5 1 calc PR . . C19 C -0.29697(16) -0.21177(16) 0.33818(15) 0.0435(4) Uani 1 1 d . . . H19A H -0.384 -0.256 0.2911 0.065 Uiso 1 1 calc R . . H19B H -0.2649 -0.1221 0.3395 0.065 Uiso 1 1 calc R . . H19C H -0.3086 -0.2226 0.4121 0.065 Uiso 1 1 calc R . . C21 C -0.27634(14) -0.04944(13) 0.71549(12) 0.0300(3) Uani 1 1 d . . . C22 C -0.21593(15) 0.02500(14) 0.82057(13) 0.0345(3) Uani 1 1 d . . . C23 C -0.28715(17) 0.08549(16) 0.88453(14) 0.0428(4) Uani 1 1 d . . . H23 H -0.2456 0.1349 0.9554 0.051 Uiso 1 1 calc R . . C24 C -0.41687(17) 0.07654(16) 0.84883(15) 0.0447(4) Uani 1 1 d . . . C25 C -0.47360(15) 0.00415(15) 0.74496(14) 0.0404(4) Uani 1 1 d . . . H25 H -0.5616 -0.0026 0.7184 0.049 Uiso 1 1 calc R . . C26 C -0.40763(14) -0.05915(14) 0.67780(13) 0.0339(3) Uani 1 1 d . . . C27 C -0.07365(16) 0.04211(16) 0.86123(14) 0.0425(4) Uani 1 1 d . . . H27A H -0.049 0.0926 0.9365 0.064 Uiso 1 1 calc R . . H27B H -0.0109 0.0851 0.8154 0.064 Uiso 1 1 calc R . . H27C H -0.0684 -0.0403 0.8583 0.064 Uiso 1 1 calc R . . C28 C -0.4930(2) 0.1417(2) 0.92106(19) 0.0696(6) Uani 1 1 d . . . H28A H -0.4364 0.1881 0.991 0.104 Uiso 0.5 1 calc PR . . H28B H -0.5769 0.0789 0.9332 0.104 Uiso 0.5 1 calc PR . . H28C H -0.5149 0.2004 0.8857 0.104 Uiso 0.5 1 calc PR . . H28D H -0.5824 0.1235 0.8823 0.104 Uiso 0.5 1 calc PR . . H28E H -0.4419 0.2327 0.94 0.104 Uiso 0.5 1 calc PR . . H28F H -0.5039 0.1112 0.9876 0.104 Uiso 0.5 1 calc PR . . C29 C -0.47353(16) -0.13575(17) 0.56585(15) 0.0456(4) Uani 1 1 d . . . H29A H -0.5687 -0.1443 0.557 0.068 Uiso 1 1 calc R . . H29B H -0.4686 -0.2192 0.5553 0.068 Uiso 1 1 calc R . . H29C H -0.4265 -0.0938 0.5119 0.068 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 0.0376(6) 0.0275(5) 0.0358(6) 0.0030(5) 0.0071(4) 0.0100(4) N1 0.0324(7) 0.0398(7) 0.0365(7) 0.0103(6) 0.0038(5) 0.0144(5) C1 0.0310(8) 0.0478(10) 0.0596(12) 0.0143(9) 0.0073(8) 0.0089(7) Li1 0.0375(13) 0.0299(13) 0.0398(15) 0.0076(11) 0.0095(11) 0.0119(10) O2 0.0327(5) 0.0337(5) 0.0353(6) 0.0100(5) 0.0091(4) 0.0161(4) N2 0.0368(7) 0.0329(7) 0.0337(7) 0.0099(6) 0.0020(5) 0.0113(5) C2 0.0467(10) 0.0707(13) 0.0458(11) 0.0177(10) -0.0010(8) 0.0250(9) Li2 0.0340(13) 0.0314(13) 0.0392(15) 0.0097(11) 0.0072(11) 0.0125(10) N3 0.0406(7) 0.0380(7) 0.0393(8) 0.0123(6) 0.0117(6) 0.0154(6) C3 0.0405(9) 0.0464(9) 0.0426(10) 0.0108(8) 0.0116(7) 0.0224(7) C4 0.0475(9) 0.0377(9) 0.0427(10) 0.0092(7) 0.0096(7) 0.0231(7) C5 0.0550(11) 0.0492(10) 0.0392(10) 0.0125(8) -0.0039(8) 0.0061(8) C6 0.0427(9) 0.0322(8) 0.0472(10) 0.0120(7) 0.0054(7) 0.0093(7) C7 0.0432(9) 0.0370(8) 0.0448(10) 0.0171(7) 0.0112(7) 0.0137(7) C8 0.0679(12) 0.0535(11) 0.0413(11) 0.0116(9) 0.0155(9) 0.0215(9) C9 0.0431(9) 0.0505(10) 0.0717(13) 0.0275(10) 0.0206(9) 0.0204(8) C11 0.0376(8) 0.0245(7) 0.0302(8) 0.0088(6) 0.0083(6) 0.0099(6) C12 0.0396(8) 0.0282(7) 0.0349(8) 0.0126(7) 0.0095(6) 0.0144(6) C13 0.0582(10) 0.0370(8) 0.0333(9) 0.0111(7) 0.0108(7) 0.0267(8) C14 0.0632(11) 0.0348(9) 0.0323(9) 0.0073(7) 0.0022(8) 0.0205(8) C15 0.0444(9) 0.0346(8) 0.0387(9) 0.0123(7) 0.0000(7) 0.0093(7) C16 0.0374(8) 0.0299(7) 0.0353(9) 0.0125(7) 0.0077(6) 0.0104(6) C17 0.0401(8) 0.0333(8) 0.0471(10) 0.0156(7) 0.0114(7) 0.0165(7) C18 0.0956(16) 0.0560(12) 0.0427(11) -0.0046(9) -0.0068(10) 0.0367(11) C19 0.0380(9) 0.0416(9) 0.0513(11) 0.0135(8) 0.0102(7) 0.0135(7) C21 0.0310(7) 0.0269(7) 0.0341(8) 0.0100(6) 0.0096(6) 0.0112(6) C22 0.0336(8) 0.0345(8) 0.0358(9) 0.0097(7) 0.0066(6) 0.0123(6) C23 0.0446(9) 0.0439(9) 0.0355(9) 0.0010(7) 0.0061(7) 0.0160(7) C24 0.0406(9) 0.0467(10) 0.0473(11) 0.0034(8) 0.0136(8) 0.0202(7) C25 0.0290(8) 0.0410(9) 0.0522(11) 0.0092(8) 0.0083(7) 0.0150(7) C26 0.0292(7) 0.0318(8) 0.0395(9) 0.0078(7) 0.0070(6) 0.0102(6) C27 0.0405(9) 0.0472(9) 0.0380(9) 0.0071(8) 0.0004(7) 0.0167(7) C28 0.0599(12) 0.0788(15) 0.0713(15) -0.0039(12) 0.0194(11) 0.0383(11) C29 0.0353(8) 0.0511(10) 0.0467(10) 0.0022(8) -0.0005(7) 0.0179(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C11 1.3329(17) . ? O1 Li1 1.867(3) . ? O1 Li1 1.904(3) 2_556 ? N1 C2 1.463(2) . ? N1 C1 1.471(2) . ? N1 C3 1.472(2) . ? N1 Li2 2.171(3) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? Li1 O2 1.868(3) . ? Li1 O1 1.904(3) 2_556 ? O2 C21 1.3437(16) . ? O2 Li2 1.862(3) . ? N2 C5 1.465(2) . ? N2 C4 1.476(2) . ? N2 C6 1.4793(19) . ? N2 Li2 2.135(3) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? Li2 N3 2.180(3) . ? N3 C8 1.467(2) . ? N3 C9 1.471(2) . ? N3 C7 1.476(2) . ? C3 C4 1.504(2) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 C7 1.509(2) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C11 C12 1.413(2) . ? C11 C16 1.416(2) . ? C12 C13 1.390(2) . ? C12 C17 1.506(2) . ? C13 C14 1.392(2) . ? C13 H13 0.95 . ? C14 C15 1.390(2) . ? C14 C18 1.509(2) . ? C15 C16 1.387(2) . ? C15 H15 0.95 . ? C16 C19 1.503(2) . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C18 H18D 0.98 . ? C18 H18E 0.98 . ? C18 H18F 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C21 C22 1.409(2) . ? C21 C26 1.412(2) . ? C22 C23 1.391(2) . ? C22 C27 1.505(2) . ? C23 C24 1.392(2) . ? C23 H23 0.95 . ? C24 C25 1.383(2) . ? C24 C28 1.515(2) . ? C25 C26 1.390(2) . ? C25 H25 0.95 . ? C26 C29 1.497(2) . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C28 H28D 0.98 . ? C28 H28E 0.98 . ? C28 H28F 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 O1 Li1 142.04(12) . . ? C11 O1 Li1 124.15(12) . 2_556 ? Li1 O1 Li1 85.89(11) . 2_556 ? C2 N1 C1 108.53(13) . . ? C2 N1 C3 110.92(13) . . ? C1 N1 C3 108.46(13) . . ? C2 N1 Li2 114.81(12) . . ? C1 N1 Li2 113.69(11) . . ? C3 N1 Li2 100.07(11) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 Li1 O2 132.20(14) . . ? O1 Li1 O1 94.11(11) . 2_556 ? O2 Li1 O1 131.22(15) . 2_556 ? C21 O2 Li2 115.07(11) . . ? C21 O2 Li1 125.33(11) . . ? Li2 O2 Li1 116.08(12) . . ? C5 N2 C4 110.32(13) . . ? C5 N2 C6 110.56(12) . . ? C4 N2 C6 111.59(12) . . ? C5 N2 Li2 114.25(13) . . ? C4 N2 Li2 103.87(11) . . ? C6 N2 Li2 106.04(11) . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O2 Li2 N2 125.73(15) . . ? O2 Li2 N1 116.33(12) . . ? N2 Li2 N1 86.08(10) . . ? O2 Li2 N3 118.53(12) . . ? N2 Li2 N3 84.91(10) . . ? N1 Li2 N3 117.75(12) . . ? C8 N3 C9 108.48(14) . . ? C8 N3 C7 109.66(13) . . ? C9 N3 C7 110.25(13) . . ? C8 N3 Li2 118.68(12) . . ? C9 N3 Li2 107.06(12) . . ? C7 N3 Li2 102.46(11) . . ? N1 C3 C4 112.04(12) . . ? N1 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N1 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N2 C4 C3 110.92(12) . . ? N2 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 111.57(13) . . ? N2 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? N2 C6 H6B 109.3 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 108 . . ? N3 C7 C6 112.37(13) . . ? N3 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? N3 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C11 C12 121.14(13) . . ? O1 C11 C16 120.49(13) . . ? C12 C11 C16 118.37(14) . . ? C13 C12 C11 119.40(14) . . ? C13 C12 C17 120.76(14) . . ? C11 C12 C17 119.82(14) . . ? C12 C13 C14 122.86(15) . . ? C12 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C15 C14 C13 116.95(15) . . ? C15 C14 C18 120.80(17) . . ? C13 C14 C18 122.25(17) . . ? C16 C15 C14 122.61(16) . . ? C16 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? C15 C16 C11 119.79(14) . . ? C15 C16 C19 121.10(14) . . ? C11 C16 C19 119.11(14) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C18 H18D 109.5 . . ? H18A C18 H18D 141.1 . . ? H18B C18 H18D 56.3 . . ? H18C C18 H18D 56.3 . . ? C14 C18 H18E 109.5 . . ? H18A C18 H18E 56.3 . . ? H18B C18 H18E 141.1 . . ? H18C C18 H18E 56.3 . . ? H18D C18 H18E 109.5 . . ? C14 C18 H18F 109.5 . . ? H18A C18 H18F 56.3 . . ? H18B C18 H18F 56.3 . . ? H18C C18 H18F 141.1 . . ? H18D C18 H18F 109.5 . . ? H18E C18 H18F 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O2 C21 C22 120.83(13) . . ? O2 C21 C26 120.52(13) . . ? C22 C21 C26 118.65(13) . . ? C23 C22 C21 119.46(14) . . ? C23 C22 C27 120.54(15) . . ? C21 C22 C27 119.96(13) . . ? C22 C23 C24 122.65(16) . . ? C22 C23 H23 118.7 . . ? C24 C23 H23 118.7 . . ? C25 C24 C23 116.92(14) . . ? C25 C24 C28 121.60(16) . . ? C23 C24 C28 121.48(17) . . ? C24 C25 C26 122.93(15) . . ? C24 C25 H25 118.5 . . ? C26 C25 H25 118.5 . . ? C25 C26 C21 119.39(15) . . ? C25 C26 C29 120.70(14) . . ? C21 C26 C29 119.90(13) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C28 H28D 109.5 . . ? H28A C28 H28D 141.1 . . ? H28B C28 H28D 56.3 . . ? H28C C28 H28D 56.3 . . ? C24 C28 H28E 109.5 . . ? H28A C28 H28E 56.3 . . ? H28B C28 H28E 141.1 . . ? H28C C28 H28E 56.3 . . ? H28D C28 H28E 109.5 . . ? C24 C28 H28F 109.5 . . ? H28A C28 H28F 56.3 . . ? H28B C28 H28F 56.3 . . ? H28C C28 H28F 141.1 . . ? H28D C28 H28F 109.5 . . ? H28E C28 H28F 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? #===END data_Compound_2c_k08mgd10 _database_code_depnum_ccdc_archive 'CCDC 778588' #TrackingRef '- LiOAr.cif' _audit_creation_date 2008-04-21T12:45:26-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C24 H46 Li N3 O' _chemical_formula_weight 399.58 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' 'x+1/2, y+1/2, -z+1/2' '-x+1/2, y, z+1/2' _cell_length_a 8.90800(10) _cell_length_b 15.6050(3) _cell_length_c 36.6930(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5100.67(14) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 45286 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 25.350 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_measurement_device_type KappaCCD _diffrn_radiation_monochromator graphite _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _diffrn_measurement_method CCD # Orientation matrix from 'scale_all.out' _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_UB_11 0.0753273 _diffrn_orient_matrix_UB_21 0.0277771 _diffrn_orient_matrix_UB_31 0.0784635 _diffrn_orient_matrix_UB_12 -0.0475011 _diffrn_orient_matrix_UB_22 0.0157510 _diffrn_orient_matrix_UB_32 0.0400264 _diffrn_orient_matrix_UB_13 -0.0004700 _diffrn_orient_matrix_UB_23 -0.0255421 _diffrn_orient_matrix_UB_33 0.0094934 _diffrn_reflns_av_R_equivalents 0.0822 _diffrn_reflns_av_unetI/netI 0.0911 _diffrn_reflns_number 35008 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.32 _diffrn_reflns_theta_full 25.32 _diffrn_measured_fraction_theta_full 0.963 _diffrn_measured_fraction_theta_max 0.963 _reflns_number_total 8925 _reflns_number_gt 6806 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+0.4976P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 8925 _refine_ls_number_parameters 547 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(12) _refine_diff_density_max 0.192 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.05 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.61632(18) 0.92969(10) 0.03711(4) 0.0260(4) Uani 1 1 d . . . N1 N 0.5507(2) 0.89896(13) -0.05067(5) 0.0283(5) Uani 1 1 d . . . C1 C 0.8558(3) 1.08566(18) -0.04638(7) 0.0385(7) Uani 1 1 d . . . H1A H 0.9155 1.1392 -0.0464 0.046 Uiso 1 1 calc R . . H1B H 0.79 1.0866 -0.0681 0.046 Uiso 1 1 calc R . . Li1 Li 0.6850(5) 0.9543(3) -0.00789(11) 0.0247(10) Uani 1 1 d . . . O2 O -0.31959(18) 0.93159(10) 0.28878(4) 0.0248(4) Uani 1 1 d . . . N2 N 0.7623(2) 1.08322(14) -0.01351(5) 0.0304(6) Uani 1 1 d . . . C2 C 0.9614(3) 1.00969(18) -0.04906(7) 0.0375(7) Uani 1 1 d . . . H2A H 1.0148 1.0116 -0.0727 0.045 Uiso 1 1 calc R . . H2B H 1.0373 1.0134 -0.0294 0.045 Uiso 1 1 calc R . . Li2 Li -0.2498(5) 0.9658(3) 0.24537(11) 0.0273(10) Uani 1 1 d . . . N3 N 0.8798(2) 0.92764(14) -0.04596(5) 0.0293(5) Uani 1 1 d . . . C3 C 0.6632(3) 0.85257(18) -0.07298(7) 0.0353(7) Uani 1 1 d . . . H3A H 0.6172 0.8356 -0.0964 0.042 Uiso 1 1 calc R . . H3B H 0.6942 0.7997 -0.0601 0.042 Uiso 1 1 calc R . . N4 N -0.3767(2) 0.91834(13) 0.19929(5) 0.0259(5) Uani 1 1 d . . . C4 C 0.8002(3) 0.90744(18) -0.08029(7) 0.0345(7) Uani 1 1 d . . . H4A H 0.8689 0.8767 -0.097 0.041 Uiso 1 1 calc R . . H4B H 0.769 0.9614 -0.0923 0.041 Uiso 1 1 calc R . . N5 N -0.1653(2) 1.09481(13) 0.24803(5) 0.0263(5) Uani 1 1 d . . . C5 C 0.8539(4) 1.0975(2) 0.01928(7) 0.0520(9) Uani 1 1 d . . . H5A H 0.9274 1.0512 0.0217 0.078 Uiso 1 1 calc R . . H5B H 0.7888 1.0985 0.0408 0.078 Uiso 1 1 calc R . . H5C H 0.9065 1.1525 0.0172 0.078 Uiso 1 1 calc R . . N6 N -0.0492(2) 0.95242(14) 0.20613(5) 0.0310(6) Uani 1 1 d . . . C6 C 0.6473(4) 1.1503(2) -0.01603(9) 0.0557(9) Uani 1 1 d . . . H6A H 0.696 1.2064 -0.0183 0.084 Uiso 1 1 calc R . . H6B H 0.585 1.1494 0.006 0.084 Uiso 1 1 calc R . . H6C H 0.5842 1.14 -0.0375 0.084 Uiso 1 1 calc R . . C7 C 0.9891(3) 0.8594(2) -0.03815(8) 0.0430(8) Uani 1 1 d . . . H7A H 1.0681 0.86 -0.0567 0.064 Uiso 1 1 calc R . . H7B H 0.9382 0.8037 -0.0384 0.064 Uiso 1 1 calc R . . H7C H 1.0338 0.869 -0.0141 0.064 Uiso 1 1 calc R . . C8 C 0.4681(3) 0.9606(2) -0.07319(7) 0.0486(8) Uani 1 1 d . . . H8A H 0.4151 0.93 -0.0926 0.073 Uiso 1 1 calc R . . H8B H 0.5387 1.0015 -0.084 0.073 Uiso 1 1 calc R . . H8C H 0.3953 0.9913 -0.058 0.073 Uiso 1 1 calc R . . C9 C 0.4442(3) 0.83716(18) -0.03505(8) 0.0415(7) Uani 1 1 d . . . H9A H 0.3697 0.8677 -0.0203 0.062 Uiso 1 1 calc R . . H9B H 0.4985 0.7962 -0.0197 0.062 Uiso 1 1 calc R . . H9C H 0.3932 0.8063 -0.0548 0.062 Uiso 1 1 calc R . . C11 C 0.5426(3) 0.88802(15) 0.06220(6) 0.0211(6) Uani 1 1 d . . . C12 C 0.4016(3) 0.91985(15) 0.07621(6) 0.0223(6) Uani 1 1 d . . . C13 C 0.3162(3) 0.86760(16) 0.09881(6) 0.0253(6) Uani 1 1 d . . . H13 H 0.2214 0.8881 0.1068 0.03 Uiso 1 1 calc R . . C14 C 0.3624(3) 0.78680(16) 0.11033(6) 0.0242(6) Uani 1 1 d . . . C15 C 0.5049(3) 0.76105(16) 0.09978(6) 0.0261(6) Uani 1 1 d . . . H15 H 0.5416 0.7077 0.1085 0.031 Uiso 1 1 calc R . . C16 C 0.5969(3) 0.80947(16) 0.07700(6) 0.0230(6) Uani 1 1 d . . . C17 C 0.3484(3) 1.01064(17) 0.06667(6) 0.0288(6) Uani 1 1 d . . . C18 C 0.3128(3) 1.01814(18) 0.02583(7) 0.0396(7) Uani 1 1 d . . . H18A H 0.2797 1.0766 0.0203 0.059 Uiso 1 1 calc R . . H18B H 0.2328 0.9777 0.0195 0.059 Uiso 1 1 calc R . . H18C H 0.403 1.0049 0.0116 0.059 Uiso 1 1 calc R . . C19 C 0.4700(3) 1.07529(17) 0.07743(8) 0.0383(7) Uani 1 1 d . . . H19A H 0.4841 1.0741 0.1039 0.058 Uiso 1 1 calc R . . H19B H 0.4393 1.1329 0.0699 0.058 Uiso 1 1 calc R . . H19C H 0.5646 1.0602 0.0654 0.058 Uiso 1 1 calc R . . C20 C 0.2050(3) 1.03597(18) 0.08748(8) 0.0426(8) Uani 1 1 d . . . H20A H 0.221 1.0281 0.1137 0.064 Uiso 1 1 calc R . . H20B H 0.1214 0.9998 0.0795 0.064 Uiso 1 1 calc R . . H20C H 0.1812 1.0962 0.0825 0.064 Uiso 1 1 calc R . . C21 C 0.2625(3) 0.73024(18) 0.13352(7) 0.0357(7) Uani 1 1 d . . . H21A H 0.3004 0.6713 0.133 0.054 Uiso 1 1 calc R . . H21B H 0.1599 0.7315 0.1239 0.054 Uiso 1 1 calc R . . H21C H 0.2625 0.7513 0.1587 0.054 Uiso 1 1 calc R . . C22 C 0.7544(3) 0.77587(16) 0.06708(7) 0.0276(6) Uani 1 1 d . . . C23 C 0.8019(3) 0.70023(19) 0.09119(8) 0.0485(9) Uani 1 1 d . . . H23A H 0.7388 0.6504 0.0857 0.073 Uiso 1 1 calc R . . H23B H 0.7901 0.7159 0.1169 0.073 Uiso 1 1 calc R . . H23C H 0.9073 0.6861 0.0864 0.073 Uiso 1 1 calc R . . C24 C 0.7570(3) 0.74518(18) 0.02754(7) 0.0363(7) Uani 1 1 d . . . H24A H 0.8574 0.7236 0.0216 0.054 Uiso 1 1 calc R . . H24B H 0.7321 0.7931 0.0113 0.054 Uiso 1 1 calc R . . H24C H 0.6832 0.6992 0.0243 0.054 Uiso 1 1 calc R . . C25 C 0.8749(3) 0.8463(2) 0.07221(8) 0.0407(8) Uani 1 1 d . . . H25A H 0.9725 0.8247 0.0641 0.061 Uiso 1 1 calc R . . H25B H 0.8808 0.8621 0.098 0.061 Uiso 1 1 calc R . . H25C H 0.8476 0.8968 0.0578 0.061 Uiso 1 1 calc R . . C31 C -0.0732(3) 1.10980(17) 0.21550(7) 0.0335(7) Uani 1 1 d . . . H31A H -0.0128 1.1624 0.2191 0.04 Uiso 1 1 calc R . . H31B H -0.1398 1.1191 0.1943 0.04 Uiso 1 1 calc R . . C32 C 0.0311(3) 1.03491(18) 0.20762(7) 0.0358(7) Uani 1 1 d . . . H32A H 0.0822 1.0448 0.184 0.043 Uiso 1 1 calc R . . H32B H 0.1089 1.0321 0.2268 0.043 Uiso 1 1 calc R . . C33 C -0.2628(3) 0.88389(19) 0.17398(7) 0.0419(8) Uani 1 1 d . . . H33A H -0.3082 0.8762 0.1496 0.05 Uiso 1 1 calc R . . H33B H -0.2287 0.8271 0.1827 0.05 Uiso 1 1 calc R . . C34 C -0.1294(3) 0.9436(2) 0.17114(7) 0.0442(8) Uani 1 1 d . . . H34A H -0.0592 0.9214 0.1525 0.053 Uiso 1 1 calc R . . H34B H -0.1644 1.0008 0.1631 0.053 Uiso 1 1 calc R . . C35 C -0.2742(3) 1.16430(18) 0.25121(8) 0.0412(8) Uani 1 1 d . . . H35A H -0.2212 1.2192 0.2525 0.062 Uiso 1 1 calc R . . H35B H -0.3339 1.1564 0.2734 0.062 Uiso 1 1 calc R . . H35C H -0.3407 1.1639 0.2299 0.062 Uiso 1 1 calc R . . C36 C -0.0717(3) 1.09279(17) 0.28101(7) 0.0318(7) Uani 1 1 d . . . H36A H -0.0133 1.1459 0.2826 0.048 Uiso 1 1 calc R . . H36B H -0.0033 1.0437 0.2798 0.048 Uiso 1 1 calc R . . H36C H -0.1361 1.0875 0.3025 0.048 Uiso 1 1 calc R . . C37 C -0.4647(3) 0.98627(18) 0.18142(8) 0.0449(8) Uani 1 1 d . . . H37A H -0.5171 0.9624 0.1602 0.067 Uiso 1 1 calc R . . H37B H -0.3972 1.0322 0.1734 0.067 Uiso 1 1 calc R . . H37C H -0.5382 1.0094 0.1987 0.067 Uiso 1 1 calc R . . C38 C -0.4812(3) 0.84972(18) 0.20992(7) 0.0354(7) Uani 1 1 d . . . H38A H -0.5559 0.8726 0.2269 0.053 Uiso 1 1 calc R . . H38B H -0.4252 0.8033 0.2217 0.053 Uiso 1 1 calc R . . H38C H -0.532 0.8275 0.1882 0.053 Uiso 1 1 calc R . . C39 C 0.0596(3) 0.8824(2) 0.21004(8) 0.0480(8) Uani 1 1 d . . . H39A H 0.1383 0.8884 0.1915 0.072 Uiso 1 1 calc R . . H39B H 0.0084 0.8274 0.2068 0.072 Uiso 1 1 calc R . . H39C H 0.1049 0.8847 0.2344 0.072 Uiso 1 1 calc R . . C41 C -0.3890(3) 0.88333(15) 0.31281(6) 0.0209(6) Uani 1 1 d . . . C42 C -0.5307(3) 0.90855(15) 0.32804(6) 0.0206(6) Uani 1 1 d . . . C43 C -0.6079(3) 0.85095(16) 0.35012(6) 0.0244(6) Uani 1 1 d . . . H43 H -0.7038 0.8672 0.3591 0.029 Uiso 1 1 calc R . . C44 C -0.5522(3) 0.77119(16) 0.35970(6) 0.0242(6) Uani 1 1 d . . . C45 C -0.4087(3) 0.75091(15) 0.34754(6) 0.0238(6) Uani 1 1 d . . . H45 H -0.3656 0.6982 0.3551 0.029 Uiso 1 1 calc R . . C46 C -0.3250(3) 0.80422(15) 0.32473(6) 0.0215(6) Uani 1 1 d . . . C47 C -0.5940(3) 0.99895(16) 0.32095(6) 0.0237(6) Uani 1 1 d . . . C48 C -0.6255(3) 1.01283(17) 0.28020(6) 0.0324(7) Uani 1 1 d . . . H48A H -0.7004 0.9712 0.2719 0.049 Uiso 1 1 calc R . . H48B H -0.5324 1.0051 0.2663 0.049 Uiso 1 1 calc R . . H48C H -0.6636 1.071 0.2764 0.049 Uiso 1 1 calc R . . C49 C -0.4800(3) 1.06556(16) 0.33449(7) 0.0300(7) Uani 1 1 d . . . H49A H -0.5152 1.1232 0.3282 0.045 Uiso 1 1 calc R . . H49B H -0.3826 1.0552 0.3229 0.045 Uiso 1 1 calc R . . H49C H -0.4693 1.0607 0.361 0.045 Uiso 1 1 calc R . . C50 C -0.7412(3) 1.01591(17) 0.34140(7) 0.0297(6) Uani 1 1 d . . . H50A H -0.7246 1.0092 0.3677 0.045 Uiso 1 1 calc R . . H50B H -0.8177 0.9749 0.3333 0.045 Uiso 1 1 calc R . . H50C H -0.7755 1.0744 0.3363 0.045 Uiso 1 1 calc R . . C51 C -0.6426(3) 0.70925(17) 0.38290(7) 0.0356(7) Uani 1 1 d . . . H51A H -0.6312 0.7243 0.4087 0.053 Uiso 1 1 calc R . . H51B H -0.6061 0.6508 0.3789 0.053 Uiso 1 1 calc R . . H51C H -0.7488 0.7127 0.3761 0.053 Uiso 1 1 calc R . . C52 C -0.1677(3) 0.77646(15) 0.31198(6) 0.0226(6) Uani 1 1 d . . . C53 C -0.1106(3) 0.69703(17) 0.33218(7) 0.0353(7) Uani 1 1 d . . . H53A H -0.1774 0.6485 0.3272 0.053 Uiso 1 1 calc R . . H53B H -0.1088 0.7085 0.3584 0.053 Uiso 1 1 calc R . . H53C H -0.0089 0.6832 0.3238 0.053 Uiso 1 1 calc R . . C54 C -0.1750(3) 0.75415(17) 0.27123(7) 0.0310(7) Uani 1 1 d . . . H54A H -0.0755 0.7361 0.2628 0.046 Uiso 1 1 calc R . . H54B H -0.2072 0.8047 0.2574 0.046 Uiso 1 1 calc R . . H54C H -0.247 0.7075 0.2675 0.046 Uiso 1 1 calc R . . C55 C -0.0504(3) 0.84724(17) 0.31828(7) 0.0303(6) Uani 1 1 d . . . H55A H -0.0432 0.8596 0.3444 0.045 Uiso 1 1 calc R . . H55B H -0.0808 0.8992 0.3052 0.045 Uiso 1 1 calc R . . H55C H 0.0474 0.828 0.3092 0.045 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 0.0303(10) 0.0281(10) 0.0197(9) 0.0032(8) 0.0057(8) -0.0004(8) N1 0.0324(13) 0.0299(13) 0.0227(12) 0.0008(10) -0.0046(10) -0.0005(11) C1 0.0416(17) 0.0364(18) 0.0375(17) 0.0086(13) 0.0127(14) -0.0093(15) Li1 0.027(3) 0.023(2) 0.024(2) 0.0028(18) 0.0009(18) -0.0015(19) O2 0.0267(10) 0.0264(10) 0.0211(10) 0.0039(8) 0.0037(8) -0.0002(9) N2 0.0310(14) 0.0321(14) 0.0279(13) 0.0016(10) 0.0076(11) -0.0047(11) C2 0.0342(17) 0.0464(19) 0.0319(16) -0.0004(14) 0.0109(13) -0.0059(15) Li2 0.029(3) 0.028(2) 0.025(2) 0.0057(19) -0.0012(19) -0.006(2) N3 0.0264(12) 0.0381(13) 0.0232(12) 0.0014(10) 0.0004(10) 0.0013(11) C3 0.0400(18) 0.0408(17) 0.0252(15) -0.0087(13) -0.0052(13) 0.0039(15) N4 0.0297(13) 0.0257(12) 0.0224(12) 0.0002(9) -0.0005(10) -0.0046(11) C4 0.0412(18) 0.0402(17) 0.0219(15) -0.0015(13) 0.0063(13) 0.0088(14) N5 0.0276(12) 0.0280(12) 0.0233(12) 0.0052(10) -0.0007(10) 0.0008(11) C5 0.053(2) 0.065(2) 0.0371(18) -0.0138(16) 0.0055(16) -0.0266(18) N6 0.0282(13) 0.0397(14) 0.0251(13) -0.0048(11) 0.0035(10) -0.0042(11) C6 0.071(2) 0.0350(18) 0.061(2) 0.0147(16) 0.0226(19) 0.0138(18) C7 0.0355(17) 0.049(2) 0.0444(19) 0.0009(15) 0.0070(14) 0.0113(15) C8 0.053(2) 0.055(2) 0.0386(18) 0.0030(16) -0.0108(16) 0.0129(17) C9 0.0359(17) 0.0404(18) 0.0480(19) -0.0040(15) -0.0046(15) -0.0037(15) C11 0.0270(15) 0.0223(14) 0.0141(14) -0.0004(11) -0.0003(11) -0.0041(12) C12 0.0252(14) 0.0232(14) 0.0185(14) 0.0003(11) -0.0006(11) -0.0002(12) C13 0.0212(15) 0.0322(16) 0.0224(15) -0.0035(12) 0.0023(11) -0.0019(12) C14 0.0252(15) 0.0241(15) 0.0234(15) -0.0009(11) -0.0008(12) -0.0057(12) C15 0.0370(17) 0.0196(14) 0.0216(15) -0.0010(11) -0.0069(12) 0.0011(12) C16 0.0258(15) 0.0252(15) 0.0181(14) -0.0032(11) -0.0015(11) -0.0007(12) C17 0.0326(17) 0.0282(15) 0.0257(15) 0.0039(12) 0.0072(12) 0.0072(13) C18 0.0444(18) 0.0398(18) 0.0345(17) 0.0091(14) -0.0013(14) 0.0131(16) C19 0.054(2) 0.0248(16) 0.0365(18) -0.0006(13) 0.0114(15) 0.0026(15) C20 0.0421(18) 0.0399(18) 0.0458(18) 0.0046(15) 0.0114(15) 0.0116(15) C21 0.0406(18) 0.0358(17) 0.0307(17) 0.0017(13) 0.0067(13) -0.0089(14) C22 0.0331(17) 0.0294(16) 0.0204(15) 0.0013(12) 0.0022(12) 0.0066(14) C23 0.051(2) 0.054(2) 0.0399(19) 0.0118(16) 0.0114(15) 0.0284(17) C24 0.0365(18) 0.0394(18) 0.0329(17) -0.0058(13) 0.0038(13) 0.0085(14) C25 0.0253(17) 0.062(2) 0.0350(17) -0.0121(15) -0.0004(13) 0.0032(16) C31 0.0334(17) 0.0365(17) 0.0307(16) 0.0058(13) 0.0012(13) -0.0086(14) C32 0.0304(16) 0.0475(19) 0.0297(16) -0.0024(13) 0.0086(13) -0.0105(15) C33 0.048(2) 0.049(2) 0.0284(16) -0.0103(14) 0.0014(14) -0.0077(16) C34 0.0447(19) 0.062(2) 0.0261(17) -0.0054(15) 0.0046(14) -0.0114(16) C35 0.0325(17) 0.0378(19) 0.053(2) 0.0056(15) -0.0010(15) 0.0053(15) C36 0.0324(16) 0.0312(16) 0.0317(16) 0.0004(12) -0.0014(13) -0.0029(13) C37 0.052(2) 0.0420(19) 0.0413(18) 0.0100(14) -0.0170(15) -0.0010(16) C38 0.0336(17) 0.0348(17) 0.0378(17) -0.0019(14) -0.0072(13) -0.0045(14) C39 0.0387(19) 0.0478(19) 0.058(2) -0.0127(16) 0.0133(16) -0.0018(16) C41 0.0250(15) 0.0213(14) 0.0165(14) -0.0018(11) -0.0010(11) -0.0052(12) C42 0.0223(13) 0.0241(14) 0.0154(13) -0.0044(11) -0.0022(11) -0.0026(12) C43 0.0194(14) 0.0324(16) 0.0213(14) -0.0041(12) 0.0027(11) -0.0026(13) C44 0.0283(16) 0.0238(14) 0.0204(14) -0.0013(12) 0.0014(11) -0.0061(13) C45 0.0308(16) 0.0215(14) 0.0189(14) -0.0015(11) -0.0012(12) 0.0021(12) C46 0.0226(15) 0.0240(14) 0.0180(14) -0.0026(11) 0.0018(11) -0.0011(12) C47 0.0226(14) 0.0240(14) 0.0246(15) -0.0008(11) 0.0005(11) 0.0000(12) C48 0.0328(16) 0.0319(16) 0.0327(16) 0.0027(13) -0.0038(13) 0.0084(14) C49 0.0318(16) 0.0284(15) 0.0297(16) -0.0038(12) 0.0041(12) -0.0017(13) C50 0.0244(15) 0.0299(16) 0.0350(16) -0.0024(13) 0.0027(12) 0.0032(13) C51 0.0408(18) 0.0350(17) 0.0310(16) 0.0019(13) 0.0097(13) -0.0081(14) C52 0.0252(15) 0.0229(14) 0.0197(14) -0.0014(11) 0.0032(11) 0.0017(12) C53 0.0324(17) 0.0333(16) 0.0403(17) -0.0003(13) 0.0035(13) 0.0083(14) C54 0.0264(16) 0.0361(17) 0.0304(17) -0.0050(13) 0.0016(12) 0.0058(13) C55 0.0235(15) 0.0371(16) 0.0302(15) 0.0017(13) -0.0017(12) 0.0002(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C11 1.305(3) . ? O1 Li1 1.802(4) . ? N1 C8 1.465(3) . ? N1 C9 1.469(3) . ? N1 C3 1.483(3) . ? N1 Li1 2.154(4) . ? C1 N2 1.466(3) . ? C1 C2 1.516(4) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? Li1 N2 2.137(5) . ? Li1 N3 2.266(5) . ? O2 C41 1.314(3) . ? O2 Li2 1.791(4) . ? N2 C6 1.468(3) . ? N2 C5 1.471(3) . ? C2 N3 1.477(3) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? Li2 N5 2.152(5) . ? Li2 N4 2.165(4) . ? Li2 N6 2.305(5) . ? N3 C7 1.471(3) . ? N3 C4 1.479(3) . ? C3 C4 1.515(4) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? N4 C38 1.471(3) . ? N4 C37 1.472(3) . ? N4 C33 1.477(3) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? N5 C35 1.460(3) . ? N5 C31 1.467(3) . ? N5 C36 1.470(3) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? N6 C39 1.467(4) . ? N6 C32 1.473(3) . ? N6 C34 1.476(3) . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C11 C16 1.425(3) . ? C11 C12 1.445(3) . ? C12 C13 1.390(3) . ? C12 C17 1.534(3) . ? C13 C14 1.392(3) . ? C13 H13 0.95 . ? C14 C15 1.387(3) . ? C14 C21 1.515(3) . ? C15 C16 1.393(3) . ? C15 H15 0.95 . ? C16 C22 1.541(4) . ? C17 C19 1.532(4) . ? C17 C18 1.537(3) . ? C17 C20 1.540(3) . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 C24 1.528(4) . ? C22 C23 1.535(4) . ? C22 C25 1.548(4) . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C31 C32 1.521(4) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 C34 1.514(4) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C41 C46 1.428(3) . ? C41 C42 1.436(3) . ? C42 C43 1.392(3) . ? C42 C47 1.541(3) . ? C43 C44 1.385(3) . ? C43 H43 0.95 . ? C44 C45 1.390(3) . ? C44 C51 1.519(3) . ? C45 C46 1.397(3) . ? C45 H45 0.95 . ? C46 C52 1.539(3) . ? C47 C50 1.534(3) . ? C47 C49 1.536(3) . ? C47 C48 1.536(3) . ? C48 H48A 0.98 . ? C48 H48B 0.98 . ? C48 H48C 0.98 . ? C49 H49A 0.98 . ? C49 H49B 0.98 . ? C49 H49C 0.98 . ? C50 H50A 0.98 . ? C50 H50B 0.98 . ? C50 H50C 0.98 . ? C51 H51A 0.98 . ? C51 H51B 0.98 . ? C51 H51C 0.98 . ? C52 C53 1.531(3) . ? C52 C54 1.537(3) . ? C52 C55 1.538(3) . ? C53 H53A 0.98 . ? C53 H53B 0.98 . ? C53 H53C 0.98 . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C54 H54C 0.98 . ? C55 H55A 0.98 . ? C55 H55B 0.98 . ? C55 H55C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 O1 Li1 157.5(2) . . ? C8 N1 C9 109.0(2) . . ? C8 N1 C3 110.4(2) . . ? C9 N1 C3 109.3(2) . . ? C8 N1 Li1 115.3(2) . . ? C9 N1 Li1 109.73(19) . . ? C3 N1 Li1 102.85(18) . . ? N2 C1 C2 112.7(2) . . ? N2 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N2 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? O1 Li1 N2 113.5(2) . . ? O1 Li1 N1 113.2(2) . . ? N2 Li1 N1 119.1(2) . . ? O1 Li1 N3 141.8(2) . . ? N2 Li1 N3 82.34(16) . . ? N1 Li1 N3 84.41(16) . . ? C41 O2 Li2 158.5(2) . . ? C1 N2 C6 109.0(2) . . ? C1 N2 C5 110.7(2) . . ? C6 N2 C5 109.3(2) . . ? C1 N2 Li1 106.67(19) . . ? C6 N2 Li1 117.0(2) . . ? C5 N2 Li1 104.1(2) . . ? N3 C2 C1 111.6(2) . . ? N3 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N3 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108 . . ? O2 Li2 N5 111.1(2) . . ? O2 Li2 N4 114.3(2) . . ? N5 Li2 N4 122.6(2) . . ? O2 Li2 N6 142.9(2) . . ? N5 Li2 N6 80.89(16) . . ? N4 Li2 N6 83.46(16) . . ? C7 N3 C2 108.5(2) . . ? C7 N3 C4 109.2(2) . . ? C2 N3 C4 110.8(2) . . ? C7 N3 Li1 121.30(19) . . ? C2 N3 Li1 105.39(18) . . ? C4 N3 Li1 101.37(18) . . ? N1 C3 C4 111.5(2) . . ? N1 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? N1 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 108 . . ? C38 N4 C37 107.8(2) . . ? C38 N4 C33 109.7(2) . . ? C37 N4 C33 110.3(2) . . ? C38 N4 Li2 111.84(18) . . ? C37 N4 Li2 112.30(19) . . ? C33 N4 Li2 104.9(2) . . ? N3 C4 C3 110.8(2) . . ? N3 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C35 N5 C31 108.6(2) . . ? C35 N5 C36 109.1(2) . . ? C31 N5 C36 110.8(2) . . ? C35 N5 Li2 117.80(19) . . ? C31 N5 Li2 107.94(19) . . ? C36 N5 Li2 102.45(18) . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C39 N6 C32 109.0(2) . . ? C39 N6 C34 109.6(2) . . ? C32 N6 C34 110.4(2) . . ? C39 N6 Li2 121.22(19) . . ? C32 N6 Li2 105.90(18) . . ? C34 N6 Li2 100.14(19) . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C11 C16 121.8(2) . . ? O1 C11 C12 121.1(2) . . ? C16 C11 C12 117.1(2) . . ? C13 C12 C11 119.1(2) . . ? C13 C12 C17 120.6(2) . . ? C11 C12 C17 120.3(2) . . ? C12 C13 C14 123.5(2) . . ? C12 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C15 C14 C13 116.6(2) . . ? C15 C14 C21 121.7(2) . . ? C13 C14 C21 121.7(2) . . ? C14 C15 C16 123.3(2) . . ? C14 C15 H15 118.4 . . ? C16 C15 H15 118.4 . . ? C15 C16 C11 119.7(2) . . ? C15 C16 C22 119.5(2) . . ? C11 C16 C22 120.8(2) . . ? C19 C17 C12 109.3(2) . . ? C19 C17 C18 110.3(2) . . ? C12 C17 C18 110.9(2) . . ? C19 C17 C20 106.9(2) . . ? C12 C17 C20 112.4(2) . . ? C18 C17 C20 107.0(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14 C21 H21A 109.5 . . ? C14 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C14 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 C23 107.6(2) . . ? C24 C22 C16 110.2(2) . . ? C23 C22 C16 112.1(2) . . ? C24 C22 C25 109.1(2) . . ? C23 C22 C25 106.5(2) . . ? C16 C22 C25 111.1(2) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N5 C31 C32 111.9(2) . . ? N5 C31 H31A 109.2 . . ? C32 C31 H31A 109.2 . . ? N5 C31 H31B 109.2 . . ? C32 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? N6 C32 C31 112.5(2) . . ? N6 C32 H32A 109.1 . . ? C31 C32 H32A 109.1 . . ? N6 C32 H32B 109.1 . . ? C31 C32 H32B 109.1 . . ? H32A C32 H32B 107.8 . . ? N4 C33 C34 111.0(2) . . ? N4 C33 H33A 109.4 . . ? C34 C33 H33A 109.4 . . ? N4 C33 H33B 109.4 . . ? C34 C33 H33B 109.4 . . ? H33A C33 H33B 108 . . ? N6 C34 C33 112.2(2) . . ? N6 C34 H34A 109.2 . . ? C33 C34 H34A 109.2 . . ? N6 C34 H34B 109.2 . . ? C33 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? N5 C35 H35A 109.5 . . ? N5 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N5 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N5 C36 H36A 109.5 . . ? N5 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N5 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C37 H37A 109.5 . . ? N4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N4 C38 H38A 109.5 . . ? N4 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N4 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N6 C39 H39A 109.5 . . ? N6 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N6 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O2 C41 C46 120.9(2) . . ? O2 C41 C42 121.2(2) . . ? C46 C41 C42 118.0(2) . . ? C43 C42 C41 119.0(2) . . ? C43 C42 C47 120.6(2) . . ? C41 C42 C47 120.5(2) . . ? C44 C43 C42 123.4(2) . . ? C44 C43 H43 118.3 . . ? C42 C43 H43 118.3 . . ? C43 C44 C45 116.9(2) . . ? C43 C44 C51 121.6(2) . . ? C45 C44 C51 121.5(2) . . ? C44 C45 C46 123.2(2) . . ? C44 C45 H45 118.4 . . ? C46 C45 H45 118.4 . . ? C45 C46 C41 119.0(2) . . ? C45 C46 C52 120.1(2) . . ? C41 C46 C52 120.9(2) . . ? C50 C47 C49 106.9(2) . . ? C50 C47 C48 107.2(2) . . ? C49 C47 C48 109.9(2) . . ? C50 C47 C42 112.8(2) . . ? C49 C47 C42 108.8(2) . . ? C48 C47 C42 111.1(2) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C44 C51 H51A 109.5 . . ? C44 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C44 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C54 107.6(2) . . ? C53 C52 C55 106.4(2) . . ? C54 C52 C55 109.7(2) . . ? C53 C52 C46 112.5(2) . . ? C54 C52 C46 108.7(2) . . ? C55 C52 C46 111.74(19) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? #===END