Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_name 'FS Mair, RG Pritchard, UMIST, Manchester' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0186 loop_ _publ_author_name 'Francis Mair' 'David T. Carey' 'Elaine K. Cope-Eatough' 'Robin G. Pritchard' ; E.Vilapana-Mafe ; 'John E. Warren' 'Rebecca J. Woods' _publ_contact_author 'FS Mair, RG Pritchard, UMIST, Manchester' _publ_contact_author_email frank.mair@umist.ac.uk _publ_section_title ;Structures and reactions of monomeric and dimeric lithium diazapentadienyl complexes with electrophiles... ; #==END # CIF produced by WinGX routine CIF_UPDATE # Created on 2002-10-09 at 00:05:13 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : c:\wingx\files\archive.dat # CIF files read : u absorb dreduc sortav struct data_4 _database_code_CSD 199213 _audit_creation_date 2002-10-09T00:05:13-00:00 _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_moiety 'C66 H86 Li2 N4 O2' _chemical_formula_sum 'C66 H86 Li2 N4 O2' _chemical_formula_weight 981.27 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.6269(3) _cell_length_b 22.2662(3) _cell_length_c 23.8287(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5638.36(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 40910 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9899 _exptl_absorpt_correction_T_max 0.9952 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _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 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_UB_11 0.365857E-1 _diffrn_orient_matrix_UB_12 0.222348E-1 _diffrn_orient_matrix_UB_13 0.326078E-1 _diffrn_orient_matrix_UB_21 -0.776783E-1 _diffrn_orient_matrix_UB_22 -0.84144E-2 _diffrn_orient_matrix_UB_23 0.22344E-1 _diffrn_orient_matrix_UB_31 0.385036E-1 _diffrn_orient_matrix_UB_32 -0.381028E-1 _diffrn_orient_matrix_UB_33 0.140938E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_unetI/netI 0.0556 _diffrn_reflns_number 37520 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 25.75 _diffrn_reflns_theta_full 25.75 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _reflns_number_total 10524 _reflns_number_gt 8360 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0214P)^2^+1.2608P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 10524 _refine_ls_number_parameters 1011 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.001 _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 0.1(11) _refine_diff_density_max 0.166 _refine_diff_density_min -0.17 _refine_diff_density_rms 0.037 #----------------------------------------------------------------------------# # 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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 0.4577(3) 0.30122(10) 0.37114(11) 0.0337(5) Uani 1 1 d . . . C2 C 0.4435(2) 0.23748(9) 0.35083(8) 0.0254(5) Uani 1 1 d . . . C3 C 0.5642(2) 0.20771(9) 0.33087(9) 0.0251(5) Uani 1 1 d . . . C4 C 0.59290(19) 0.14762(9) 0.35775(8) 0.0241(5) Uani 1 1 d . . . C5 C 0.7198(2) 0.14167(11) 0.38493(11) 0.0348(6) Uani 1 1 d . . . C6 C 0.2222(2) 0.24043(9) 0.35533(9) 0.0262(5) Uani 1 1 d . . . C7 C 0.1390(2) 0.22725(9) 0.39936(9) 0.0273(5) Uani 1 1 d . . . C8 C 0.0230(2) 0.25695(10) 0.39934(10) 0.0333(5) Uani 1 1 d . . . C9 C -0.0103(2) 0.29760(10) 0.35796(10) 0.0358(6) Uani 1 1 d . . . C10 C 0.0726(2) 0.30962(10) 0.31476(10) 0.0355(6) Uani 1 1 d . . . C11 C 0.1880(2) 0.28110(10) 0.31337(10) 0.0311(5) Uani 1 1 d . . . C12 C 0.1754(2) 0.18381(10) 0.44568(9) 0.0328(5) Uani 1 1 d . . . C13 C 0.2580(3) 0.21546(14) 0.48881(12) 0.0493(7) Uani 1 1 d . . . C14 C 0.0627(3) 0.15388(12) 0.47370(11) 0.0413(6) Uani 1 1 d . . . C15 C 0.54245(19) 0.04664(9) 0.37549(8) 0.0250(5) Uani 1 1 d . . . C16 C 0.5153(2) 0.02843(9) 0.43042(9) 0.0276(5) Uani 1 1 d . . . C17 C 0.5431(2) -0.03041(10) 0.44537(10) 0.0354(5) Uani 1 1 d . . . C18 C 0.5937(2) -0.07111(11) 0.40766(10) 0.0390(6) Uani 1 1 d . . . C19 C 0.6186(2) -0.05280(10) 0.35308(11) 0.0382(6) Uani 1 1 d . . . C20 C 0.5931(2) 0.00601(10) 0.33710(10) 0.0312(5) Uani 1 1 d . . . C21 C 0.4542(2) 0.07065(10) 0.47199(9) 0.0347(5) Uani 1 1 d . . . C22 C 0.3311(3) 0.04418(14) 0.49369(12) 0.0482(7) Uani 1 1 d . . . C23 C 0.5405(3) 0.08577(16) 0.52123(13) 0.0574(8) Uani 1 1 d . . . C24 C 0.5597(2) 0.20046(8) 0.26232(8) 0.0237(5) Uani 1 1 d . . . C25 C 0.5481(2) 0.26353(9) 0.23440(9) 0.0281(5) Uani 1 1 d . . . C26 C 0.5357(2) 0.25423(10) 0.17075(9) 0.0316(5) Uani 1 1 d . . . C27 C 0.6551(2) 0.22443(10) 0.14795(10) 0.0353(5) Uani 1 1 d . . . C28 C 0.6747(2) 0.16387(10) 0.17759(9) 0.0338(5) Uani 1 1 d . . . C29 C 0.6866(2) 0.17323(10) 0.24124(9) 0.0280(5) Uani 1 1 d . . . C30 C 0.7689(3) 0.26461(12) 0.15897(11) 0.0415(6) Uani 1 1 d . . . C31 C 0.7814(2) 0.27429(11) 0.22260(10) 0.0375(6) Uani 1 1 d . . . C32 C 0.6625(2) 0.30433(10) 0.24535(11) 0.0356(5) Uani 1 1 d . . . C33 C 0.8004(2) 0.21396(10) 0.25188(11) 0.0341(5) Uani 1 1 d . . . C41 C 0.2812(2) -0.06300(10) 0.14449(10) 0.0290(5) Uani 1 1 d . . . C42 C 0.2923(2) 0.00237(9) 0.16155(8) 0.0235(5) Uani 1 1 d . . . C43 C 0.1708(2) 0.03228(9) 0.17917(8) 0.0225(4) Uani 1 1 d . . . C44 C 0.14237(19) 0.09160(9) 0.15036(8) 0.0233(4) Uani 1 1 d . . . C45 C 0.0126(2) 0.09791(11) 0.12574(11) 0.0323(5) Uani 1 1 d . . . C46 C 0.5134(2) 0.00044(9) 0.15550(8) 0.0246(5) Uani 1 1 d . . . C47 C 0.5919(2) 0.01468(9) 0.11020(9) 0.0268(5) Uani 1 1 d . . . C48 C 0.7079(2) -0.01448(10) 0.10716(10) 0.0344(5) Uani 1 1 d . . . C49 C 0.7464(2) -0.05578(10) 0.14727(11) 0.0373(6) Uani 1 1 d . . . C50 C 0.6688(2) -0.06802(10) 0.19239(10) 0.0330(5) Uani 1 1 d . . . C51 C 0.5525(2) -0.04012(9) 0.19649(9) 0.0283(5) Uani 1 1 d . . . C52 C 0.5501(2) 0.05828(10) 0.06495(9) 0.0299(5) Uani 1 1 d . . . C53 C 0.4667(3) 0.02580(13) 0.02255(11) 0.0443(6) Uani 1 1 d . . . C54 C 0.6589(3) 0.08957(13) 0.03530(12) 0.0432(6) Uani 1 1 d . . . C55 C 0.1960(2) 0.19262(9) 0.13121(9) 0.0252(5) Uani 1 1 d . . . C56 C 0.2228(2) 0.21264(9) 0.07679(9) 0.0297(5) Uani 1 1 d . . . C57 C 0.2003(2) 0.27328(10) 0.06496(10) 0.0370(6) Uani 1 1 d . . . C58 C 0.1544(2) 0.31222(10) 0.10489(10) 0.0370(6) Uani 1 1 d . . . C59 C 0.1291(2) 0.29176(10) 0.15841(10) 0.0376(6) Uani 1 1 d . . . C60 C 0.1505(2) 0.23207(9) 0.17129(10) 0.0323(5) Uani 1 1 d . . . C61 C 0.2720(3) 0.17082(11) 0.03140(10) 0.0417(6) Uani 1 1 d . . . C62 C 0.3865(3) 0.19648(15) 0.00159(14) 0.0565(8) Uani 1 1 d . . . C63 C 0.1698(4) 0.15648(15) -0.01119(13) 0.0607(8) Uani 1 1 d . . . C64 C 0.17308(19) 0.04285(8) 0.24751(8) 0.0225(4) Uani 1 1 d . . . C65 C 0.1923(2) -0.01820(9) 0.27804(9) 0.0262(5) Uani 1 1 d . . . C66 C 0.2029(2) -0.00526(11) 0.34150(9) 0.0309(5) Uani 1 1 d . . . C67 C 0.0809(2) 0.02321(10) 0.36259(10) 0.0322(5) Uani 1 1 d . . . C68 C 0.0554(2) 0.08125(10) 0.33064(9) 0.0311(5) Uani 1 1 d . . . C69 C 0.0440(2) 0.06809(9) 0.26729(9) 0.0258(5) Uani 1 1 d . . . C70 C -0.0285(2) -0.02065(11) 0.35371(10) 0.0383(6) Uani 1 1 d . . . C71 C -0.0405(2) -0.03408(11) 0.29068(10) 0.0357(5) Uani 1 1 d . . . C72 C 0.0819(2) -0.06174(10) 0.26907(10) 0.0329(5) Uani 1 1 d . . . C73 C -0.0654(2) 0.02435(10) 0.25873(10) 0.0321(5) Uani 1 1 d . . . N1 N 0.33856(16) 0.20902(7) 0.34866(7) 0.0256(4) Uani 1 1 d . . . N2 N 0.51142(16) 0.10547(7) 0.35564(7) 0.0248(4) Uani 1 1 d . . . N41 N 0.39662(16) 0.03135(7) 0.16312(7) 0.0239(4) Uani 1 1 d . . . N42 N 0.22629(16) 0.13276(7) 0.14956(7) 0.0240(4) Uani 1 1 d . . . O1 O 0.46133(13) 0.16469(6) 0.24882(6) 0.0258(3) Uani 1 1 d . . . O2 O 0.26815(13) 0.08166(6) 0.25939(6) 0.0245(3) Uani 1 1 d . . . Li1 Li 0.3612(3) 0.12883(15) 0.30419(14) 0.0262(8) Uani 1 1 d . . . Li2 Li 0.3733(3) 0.11416(15) 0.20399(14) 0.0256(8) Uani 1 1 d . . . H1A H 0.381(3) 0.3171(11) 0.3906(11) 0.048(7) Uiso 1 1 d . . . H1B H 0.529(3) 0.3016(11) 0.3993(11) 0.052(7) Uiso 1 1 d . . . H1C H 0.484(2) 0.3303(12) 0.3404(11) 0.053(8) Uiso 1 1 d . . . H3 H 0.6323(19) 0.2338(9) 0.3406(8) 0.020(5) Uiso 1 1 d . . . H5A H 0.733(2) 0.1004(12) 0.3989(10) 0.046(7) Uiso 1 1 d . . . H5B H 0.727(3) 0.1718(15) 0.4149(14) 0.085(11) Uiso 1 1 d . . . H5C H 0.788(3) 0.1506(12) 0.3584(11) 0.055(8) Uiso 1 1 d . . . H8 H -0.038(2) 0.2481(10) 0.4310(9) 0.035(6) Uiso 1 1 d . . . H9 H -0.095(2) 0.3174(10) 0.3597(10) 0.038(6) Uiso 1 1 d . . . H10 H 0.056(3) 0.3393(12) 0.2827(11) 0.051(7) Uiso 1 1 d . . . H11 H 0.245(2) 0.2855(10) 0.2810(10) 0.039(7) Uiso 1 1 d . . . H12 H 0.231(2) 0.1514(11) 0.4270(10) 0.044(7) Uiso 1 1 d . . . H13A H 0.278(3) 0.1873(13) 0.5211(12) 0.067(9) Uiso 1 1 d . . . H13B H 0.208(2) 0.2457(11) 0.5066(9) 0.032(6) Uiso 1 1 d . . . H13C H 0.335(3) 0.2375(12) 0.4695(12) 0.064(8) Uiso 1 1 d . . . H14A H 0.093(2) 0.1218(12) 0.5019(11) 0.054(8) Uiso 1 1 d . . . H14B H 0.005(2) 0.1343(9) 0.4458(10) 0.032(6) Uiso 1 1 d . . . H14C H 0.021(3) 0.1859(12) 0.4972(11) 0.056(8) Uiso 1 1 d . . . H17 H 0.525(2) -0.0441(11) 0.4846(11) 0.049(7) Uiso 1 1 d . . . H18 H 0.602(2) -0.1141(11) 0.4202(10) 0.046(7) Uiso 1 1 d . . . H19 H 0.654(2) -0.0827(11) 0.3266(10) 0.045(7) Uiso 1 1 d . . . H20 H 0.610(2) 0.0203(11) 0.2977(11) 0.049(7) Uiso 1 1 d . . . H21 H 0.434(2) 0.1090(10) 0.4512(9) 0.038(6) Uiso 1 1 d . . . H22A H 0.352(3) 0.0052(13) 0.5162(11) 0.059(8) Uiso 1 1 d . . . H22B H 0.272(3) 0.0301(13) 0.4613(14) 0.075(10) Uiso 1 1 d . . . H22C H 0.285(3) 0.0731(12) 0.5168(11) 0.051(8) Uiso 1 1 d . . . H23A H 0.619(3) 0.1040(13) 0.5068(12) 0.060(9) Uiso 1 1 d . . . H23B H 0.557(3) 0.0454(15) 0.5446(13) 0.082(10) Uiso 1 1 d . . . H23C H 0.496(3) 0.1179(14) 0.5483(13) 0.079(10) Uiso 1 1 d . . . H25 H 0.473(2) 0.2819(9) 0.2485(8) 0.021(5) Uiso 1 1 d . . . H26A H 0.458(2) 0.2291(10) 0.1625(9) 0.032(6) Uiso 1 1 d . . . H26B H 0.524(2) 0.2948(10) 0.1521(9) 0.034(6) Uiso 1 1 d . . . H27 H 0.644(2) 0.2186(11) 0.1057(11) 0.050(7) Uiso 1 1 d . . . H28A H 0.753(3) 0.1456(10) 0.1630(10) 0.041(7) Uiso 1 1 d . . . H28B H 0.600(2) 0.1343(9) 0.1697(9) 0.031(6) Uiso 1 1 d . . . H29 H 0.702(2) 0.1327(10) 0.2597(9) 0.034(6) Uiso 1 1 d . . . H30A H 0.851(3) 0.2459(12) 0.1422(11) 0.059(8) Uiso 1 1 d . . . H30B H 0.753(3) 0.3052(13) 0.1408(12) 0.063(8) Uiso 1 1 d . . . H31 H 0.855(3) 0.3013(11) 0.2297(10) 0.050(7) Uiso 1 1 d . . . H32A H 0.670(2) 0.3115(10) 0.2855(11) 0.041(7) Uiso 1 1 d . . . H32B H 0.653(2) 0.3443(12) 0.2242(11) 0.051(7) Uiso 1 1 d . . . H33A H 0.883(2) 0.1917(10) 0.2357(10) 0.042(7) Uiso 1 1 d . . . H33B H 0.812(2) 0.2224(10) 0.2917(10) 0.040(7) Uiso 1 1 d . . . H41A H 0.358(3) -0.0784(11) 0.1246(10) 0.045(7) Uiso 1 1 d . . . H41B H 0.201(2) -0.0704(10) 0.1208(10) 0.040(6) Uiso 1 1 d . . . H41C H 0.270(3) -0.0898(12) 0.1796(12) 0.058(8) Uiso 1 1 d . . . H43 H 0.1002(19) 0.0044(8) 0.1706(8) 0.016(5) Uiso 1 1 d . . . H45A H -0.002(3) 0.0669(14) 0.0944(14) 0.084(10) Uiso 1 1 d . . . H45B H -0.005(2) 0.1402(12) 0.1119(10) 0.053(8) Uiso 1 1 d . . . H45C H -0.057(3) 0.0872(12) 0.1526(12) 0.059(8) Uiso 1 1 d . . . H48 H 0.763(2) -0.0055(10) 0.0731(10) 0.042(7) Uiso 1 1 d . . . H49 H 0.829(3) -0.0753(11) 0.1421(11) 0.053(7) Uiso 1 1 d . . . H50 H 0.693(2) -0.0982(11) 0.2215(11) 0.048(7) Uiso 1 1 d . . . H51 H 0.498(2) -0.0483(9) 0.2283(9) 0.031(6) Uiso 1 1 d . . . H52 H 0.497(2) 0.0915(9) 0.0837(8) 0.026(5) Uiso 1 1 d . . . H53A H 0.393(3) 0.0071(12) 0.0416(11) 0.053(8) Uiso 1 1 d . . . H53B H 0.522(3) -0.0064(12) 0.0031(11) 0.058(8) Uiso 1 1 d . . . H53C H 0.433(3) 0.0543(12) -0.0057(11) 0.053(7) Uiso 1 1 d . . . H54A H 0.706(2) 0.0619(11) 0.0110(11) 0.044(7) Uiso 1 1 d . . . H54B H 0.722(3) 0.1080(13) 0.0640(13) 0.075(10) Uiso 1 1 d . . . H54C H 0.624(3) 0.1245(12) 0.0104(11) 0.058(8) Uiso 1 1 d . . . H57 H 0.216(2) 0.2868(10) 0.0263(10) 0.034(6) Uiso 1 1 d . . . H58 H 0.145(2) 0.3543(11) 0.0953(10) 0.043(7) Uiso 1 1 d . . . H59 H 0.100(3) 0.3184(12) 0.1882(11) 0.057(8) Uiso 1 1 d . . . H60 H 0.137(2) 0.2159(11) 0.2100(11) 0.048(7) Uiso 1 1 d . . . H61 H 0.297(2) 0.1321(11) 0.0494(10) 0.044(7) Uiso 1 1 d . . . H62A H 0.454(3) 0.2067(13) 0.0311(12) 0.068(9) Uiso 1 1 d . . . H62B H 0.366(3) 0.2366(14) -0.0185(12) 0.073(9) Uiso 1 1 d . . . H62C H 0.422(3) 0.1664(13) -0.0247(12) 0.066(9) Uiso 1 1 d . . . H63A H 0.088(3) 0.1395(14) 0.0079(14) 0.087(11) Uiso 1 1 d . . . H63B H 0.201(3) 0.1251(14) -0.0377(14) 0.086(11) Uiso 1 1 d . . . H63C H 0.138(3) 0.1969(15) -0.0314(14) 0.083(10) Uiso 1 1 d . . . H65 H 0.278(2) -0.0372(9) 0.2648(8) 0.029(6) Uiso 1 1 d . . . H66A H 0.220(2) -0.0448(11) 0.3617(10) 0.039(6) Uiso 1 1 d . . . H66B H 0.277(2) 0.0214(9) 0.3497(9) 0.027(6) Uiso 1 1 d . . . H67 H 0.090(2) 0.0325(9) 0.4038(9) 0.030(6) Uiso 1 1 d . . . H68A H 0.123(2) 0.1105(10) 0.3375(9) 0.035(6) Uiso 1 1 d . . . H68B H -0.024(2) 0.0993(9) 0.3419(9) 0.029(6) Uiso 1 1 d . . . H69 H 0.0276(19) 0.1052(9) 0.2482(8) 0.022(5) Uiso 1 1 d . . . H70A H -0.008(2) -0.0583(10) 0.3738(9) 0.034(6) Uiso 1 1 d . . . H70B H -0.111(2) -0.0013(10) 0.3680(10) 0.040(7) Uiso 1 1 d . . . H71 H -0.113(3) -0.0620(11) 0.2845(10) 0.052(7) Uiso 1 1 d . . . H72A H 0.100(2) -0.1012(10) 0.2898(9) 0.035(6) Uiso 1 1 d . . . H72B H 0.069(2) -0.0737(9) 0.2286(10) 0.031(6) Uiso 1 1 d . . . H73A H -0.078(2) 0.0141(9) 0.2166(10) 0.033(6) Uiso 1 1 d . . . H73B H -0.145(2) 0.0422(10) 0.2737(10) 0.039(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0357(14) 0.0272(12) 0.0382(13) -0.0079(10) -0.0070(12) -0.0010(11) C2 0.0289(12) 0.0242(10) 0.0231(11) 0.0007(9) -0.0060(9) -0.0004(10) C3 0.0222(11) 0.0218(10) 0.0314(11) -0.0015(9) -0.0039(9) -0.0025(9) C4 0.0223(11) 0.0268(11) 0.0233(11) -0.0017(9) -0.0003(9) 0.0001(9) C5 0.0274(13) 0.0329(13) 0.0442(15) 0.0024(12) -0.0079(12) -0.0009(11) C6 0.0244(11) 0.0238(10) 0.0305(11) -0.0072(9) -0.0051(10) 0.0008(9) C7 0.0265(12) 0.0272(11) 0.0283(11) -0.0075(9) -0.0037(9) 0.0021(10) C8 0.0290(13) 0.0349(12) 0.0361(13) -0.0098(10) 0.0000(11) 0.0039(11) C9 0.0284(13) 0.0331(12) 0.0460(14) -0.0119(11) -0.0088(12) 0.0076(10) C10 0.0386(14) 0.0265(11) 0.0413(14) -0.0050(10) -0.0132(12) 0.0046(11) C11 0.0320(13) 0.0287(11) 0.0325(12) -0.0027(10) -0.0051(11) 0.0005(10) C12 0.0302(13) 0.0389(13) 0.0295(12) -0.0031(10) 0.0003(10) 0.0038(11) C13 0.0575(19) 0.0520(17) 0.0383(15) 0.0000(14) -0.0139(14) -0.0017(16) C14 0.0419(15) 0.0460(15) 0.0359(14) -0.0008(13) 0.0040(13) 0.0011(13) C15 0.0204(11) 0.0269(11) 0.0276(11) 0.0002(9) -0.0025(9) -0.0014(9) C16 0.0223(11) 0.0303(11) 0.0303(11) 0.0019(9) -0.0022(9) 0.0034(10) C17 0.0370(14) 0.0333(12) 0.0358(13) 0.0083(10) 0.0027(11) 0.0048(11) C18 0.0409(14) 0.0269(12) 0.0491(15) 0.0072(11) 0.0031(12) 0.0043(11) C19 0.0403(14) 0.0289(12) 0.0454(14) -0.0058(11) 0.0081(12) 0.0026(11) C20 0.0319(13) 0.0299(12) 0.0318(13) -0.0015(10) 0.0017(10) -0.0008(10) C21 0.0394(14) 0.0354(12) 0.0291(12) 0.0018(10) 0.0011(11) 0.0108(11) C22 0.0425(16) 0.0642(19) 0.0379(15) 0.0009(14) 0.0109(13) 0.0125(15) C23 0.057(2) 0.066(2) 0.0495(17) -0.0198(16) -0.0068(16) 0.0049(17) C24 0.0244(11) 0.0219(10) 0.0248(10) -0.0021(8) -0.0029(9) -0.0035(9) C25 0.0279(12) 0.0252(11) 0.0313(12) 0.0012(9) -0.0021(10) -0.0005(10) C26 0.0308(13) 0.0315(12) 0.0324(12) 0.0070(10) -0.0039(10) -0.0070(11) C27 0.0358(13) 0.0424(13) 0.0276(13) 0.0020(11) 0.0029(11) -0.0125(11) C28 0.0298(13) 0.0375(13) 0.0341(13) -0.0050(10) 0.0040(11) -0.0026(12) C29 0.0234(12) 0.0285(11) 0.0321(12) -0.0003(10) 0.0000(10) -0.0035(9) C30 0.0364(14) 0.0473(15) 0.0407(15) 0.0080(12) 0.0040(12) -0.0119(13) C31 0.0305(13) 0.0372(13) 0.0447(14) 0.0033(11) -0.0032(11) -0.0139(12) C32 0.0450(15) 0.0259(11) 0.0359(14) 0.0021(11) -0.0063(12) -0.0116(11) C33 0.0247(12) 0.0385(13) 0.0390(14) -0.0001(11) -0.0033(11) -0.0063(10) C41 0.0345(13) 0.0232(11) 0.0294(12) -0.0045(10) -0.0024(11) -0.0002(10) C42 0.0285(12) 0.0226(10) 0.0195(10) 0.0003(8) -0.0028(9) 0.0014(9) C43 0.0214(10) 0.0207(10) 0.0255(11) -0.0008(8) 0.0000(9) -0.0022(9) C44 0.0234(11) 0.0237(10) 0.0228(11) -0.0007(8) -0.0023(9) 0.0010(9) C45 0.0272(13) 0.0298(12) 0.0400(14) 0.0053(11) -0.0076(11) -0.0022(10) C46 0.0243(11) 0.0222(10) 0.0274(11) -0.0045(9) -0.0021(9) 0.0002(9) C47 0.0266(12) 0.0240(11) 0.0297(12) -0.0040(9) -0.0015(9) 0.0003(9) C48 0.0304(13) 0.0341(12) 0.0388(13) -0.0027(10) 0.0037(11) 0.0034(10) C49 0.0286(13) 0.0356(13) 0.0477(15) -0.0052(11) -0.0028(12) 0.0048(11) C50 0.0342(13) 0.0272(12) 0.0378(13) -0.0006(10) -0.0072(11) 0.0034(11) C51 0.0306(12) 0.0256(11) 0.0286(12) -0.0023(9) -0.0028(10) 0.0012(10) C52 0.0313(13) 0.0297(11) 0.0287(11) 0.0002(9) 0.0039(10) 0.0025(10) C53 0.0527(17) 0.0443(15) 0.0359(14) 0.0016(12) -0.0109(14) 0.0007(14) C54 0.0432(16) 0.0465(15) 0.0399(15) 0.0089(13) 0.0120(13) -0.0005(14) C55 0.0245(11) 0.0209(10) 0.0303(12) 0.0012(9) -0.0036(9) -0.0023(9) C56 0.0344(13) 0.0262(11) 0.0286(11) 0.0026(9) -0.0026(10) 0.0024(10) C57 0.0438(15) 0.0303(12) 0.0370(14) 0.0095(11) -0.0011(12) 0.0073(11) C58 0.0430(14) 0.0234(12) 0.0445(14) 0.0051(10) -0.0002(12) 0.0039(11) C59 0.0443(15) 0.0261(12) 0.0425(14) -0.0071(11) 0.0017(12) 0.0022(11) C60 0.0395(13) 0.0272(12) 0.0302(13) -0.0017(10) 0.0026(11) 0.0008(11) C61 0.0595(17) 0.0329(13) 0.0326(13) 0.0044(11) 0.0082(13) 0.0126(12) C62 0.058(2) 0.0608(19) 0.0504(17) 0.0014(16) 0.0171(16) 0.0125(16) C63 0.083(2) 0.0573(19) 0.0415(17) -0.0145(15) 0.0066(17) -0.0101(19) C64 0.0212(10) 0.0206(9) 0.0259(11) 0.0004(8) -0.0010(9) -0.0026(9) C65 0.0274(12) 0.0245(11) 0.0267(11) 0.0021(9) 0.0004(9) -0.0006(10) C66 0.0321(13) 0.0334(12) 0.0272(12) 0.0065(10) -0.0023(10) -0.0055(11) C67 0.0308(13) 0.0385(13) 0.0272(12) -0.0002(10) 0.0033(10) -0.0069(11) C68 0.0265(12) 0.0336(12) 0.0332(12) -0.0046(10) 0.0066(10) -0.0004(11) C69 0.0223(11) 0.0242(10) 0.0308(12) 0.0011(9) 0.0014(9) -0.0003(9) C70 0.0365(14) 0.0413(14) 0.0370(13) 0.0049(11) 0.0079(12) -0.0068(12) C71 0.0312(13) 0.0372(13) 0.0386(13) 0.0017(10) 0.0020(11) -0.0148(11) C72 0.0370(14) 0.0251(11) 0.0367(14) 0.0029(10) -0.0017(10) -0.0090(10) C73 0.0225(12) 0.0366(12) 0.0371(14) -0.0014(10) 0.0020(10) -0.0031(10) N1 0.0235(9) 0.0250(9) 0.0283(9) -0.0025(7) -0.0020(8) 0.0026(8) N2 0.0256(9) 0.0253(9) 0.0235(9) 0.0002(7) -0.0005(8) 0.0002(8) N41 0.0242(10) 0.0223(8) 0.0252(9) -0.0002(7) 0.0017(8) 0.0001(8) N42 0.0274(10) 0.0207(8) 0.0240(9) 0.0022(7) -0.0014(8) 0.0009(8) O1 0.0229(7) 0.0265(7) 0.0279(7) -0.0017(6) -0.0027(7) -0.0072(6) O2 0.0227(7) 0.0250(7) 0.0258(8) -0.0013(6) -0.0003(6) -0.0075(6) Li1 0.0244(19) 0.0267(17) 0.0276(18) -0.0002(14) -0.0006(15) -0.0015(15) Li2 0.0254(19) 0.0246(17) 0.0269(18) 0.0018(15) -0.0013(15) -0.0027(15) #----------------------------------------------------------------------------# # 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 C2 1.507(3) . ? C2 N1 1.284(3) . ? C2 C3 1.520(3) . ? C3 C4 1.514(3) . ? C3 C24 1.642(3) . ? C4 N2 1.278(3) . ? C4 C5 1.502(3) . ? C6 C11 1.397(3) . ? C6 C7 1.403(3) . ? C6 N1 1.429(3) . ? C7 C8 1.399(3) . ? C7 C12 1.518(3) . ? C8 C9 1.384(3) . ? C9 C10 1.381(3) . ? C10 C11 1.381(3) . ? C12 C14 1.524(3) . ? C12 C13 1.525(3) . ? C15 C20 1.395(3) . ? C15 C16 1.400(3) . ? C15 N2 1.431(3) . ? C16 C17 1.390(3) . ? C16 C21 1.512(3) . ? C17 C18 1.385(3) . ? C18 C19 1.388(3) . ? C19 C20 1.390(3) . ? C21 C22 1.525(4) . ? C21 C23 1.527(4) . ? C24 O1 1.353(2) . ? C24 C25 1.559(3) . ? C24 C29 1.562(3) . ? C25 C26 1.536(3) . ? C25 C32 1.540(3) . ? C26 C27 1.531(3) . ? C27 C30 1.527(3) . ? C27 C28 1.537(3) . ? C28 C29 1.536(3) . ? C29 C33 1.533(3) . ? C30 C31 1.537(4) . ? C31 C33 1.527(3) . ? C31 C32 1.529(3) . ? C41 C42 1.516(3) . ? C42 N41 1.283(3) . ? C42 C43 1.512(3) . ? C43 C44 1.519(3) . ? C43 C64 1.646(3) . ? C44 N42 1.279(3) . ? C44 C45 1.505(3) . ? C46 C51 1.394(3) . ? C46 C47 1.400(3) . ? C46 N41 1.431(3) . ? C47 C48 1.396(3) . ? C47 C52 1.517(3) . ? C48 C49 1.388(3) . ? C49 C50 1.382(3) . ? C50 C51 1.386(3) . ? C52 C54 1.524(3) . ? C52 C53 1.526(3) . ? C55 C60 1.385(3) . ? C55 C56 1.401(3) . ? C55 N42 1.439(2) . ? C56 C57 1.400(3) . ? C56 C61 1.520(3) . ? C57 C58 1.377(3) . ? C58 C59 1.381(3) . ? C59 C60 1.383(3) . ? C61 C62 1.520(4) . ? C61 C63 1.520(4) . ? C64 O2 1.359(2) . ? C64 C65 1.555(3) . ? C64 C69 1.555(3) . ? C65 C72 1.537(3) . ? C65 C66 1.543(3) . ? C66 C67 1.529(3) . ? C67 C68 1.524(3) . ? C67 C70 1.533(3) . ? C68 C69 1.543(3) . ? C69 C73 1.530(3) . ? C70 C71 1.537(3) . ? C71 C72 1.528(3) . ? C71 C73 1.530(3) . ? N1 Li1 2.090(4) . ? N2 Li1 2.079(4) . ? N41 Li2 2.100(4) . ? N42 Li2 2.072(4) . ? O1 Li2 1.812(4) . ? O1 Li1 1.874(4) . ? O2 Li1 1.795(4) . ? O2 Li2 1.875(4) . ? Li1 Li2 2.413(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C2 C1 124.4(2) . . ? N1 C2 C3 120.33(17) . . ? C1 C2 C3 115.30(19) . . ? C4 C3 C2 115.02(17) . . ? C4 C3 C24 109.87(16) . . ? C2 C3 C24 109.25(16) . . ? N2 C4 C5 124.09(19) . . ? N2 C4 C3 119.71(18) . . ? C5 C4 C3 116.19(19) . . ? C11 C6 C7 120.4(2) . . ? C11 C6 N1 117.58(19) . . ? C7 C6 N1 121.74(18) . . ? C8 C7 C6 117.2(2) . . ? C8 C7 C12 121.7(2) . . ? C6 C7 C12 121.09(19) . . ? C9 C8 C7 122.3(2) . . ? C10 C9 C8 119.7(2) . . ? C9 C10 C11 119.7(2) . . ? C10 C11 C6 120.8(2) . . ? C7 C12 C14 113.4(2) . . ? C7 C12 C13 110.03(19) . . ? C14 C12 C13 111.1(2) . . ? C20 C15 C16 120.31(19) . . ? C20 C15 N2 117.77(18) . . ? C16 C15 N2 121.76(18) . . ? C17 C16 C15 118.0(2) . . ? C17 C16 C21 120.6(2) . . ? C15 C16 C21 121.39(19) . . ? C18 C17 C16 122.2(2) . . ? C17 C18 C19 119.3(2) . . ? C18 C19 C20 119.7(2) . . ? C19 C20 C15 120.4(2) . . ? C16 C21 C22 110.5(2) . . ? C16 C21 C23 112.5(2) . . ? C22 C21 C23 109.9(2) . . ? O1 C24 C25 111.58(17) . . ? O1 C24 C29 111.23(15) . . ? C25 C24 C29 106.29(17) . . ? O1 C24 C3 108.48(16) . . ? C25 C24 C3 109.78(15) . . ? C29 C24 C3 109.45(16) . . ? C26 C25 C32 108.31(19) . . ? C26 C25 C24 107.87(17) . . ? C32 C25 C24 113.37(18) . . ? C27 C26 C25 109.75(19) . . ? C30 C27 C26 109.9(2) . . ? C30 C27 C28 109.1(2) . . ? C26 C27 C28 109.26(19) . . ? C29 C28 C27 110.24(19) . . ? C33 C29 C28 107.98(19) . . ? C33 C29 C24 113.49(17) . . ? C28 C29 C24 107.41(18) . . ? C27 C30 C31 108.7(2) . . ? C33 C31 C32 109.40(19) . . ? C33 C31 C30 109.8(2) . . ? C32 C31 C30 109.8(2) . . ? C31 C32 C25 109.53(18) . . ? C31 C33 C29 109.90(19) . . ? N41 C42 C43 120.52(17) . . ? N41 C42 C41 123.9(2) . . ? C43 C42 C41 115.55(19) . . ? C42 C43 C44 115.31(17) . . ? C42 C43 C64 109.00(16) . . ? C44 C43 C64 109.01(15) . . ? N42 C44 C45 124.48(18) . . ? N42 C44 C43 119.41(18) . . ? C45 C44 C43 116.09(18) . . ? C51 C46 C47 120.63(19) . . ? C51 C46 N41 118.78(19) . . ? C47 C46 N41 120.36(18) . . ? C48 C47 C46 117.4(2) . . ? C48 C47 C52 121.3(2) . . ? C46 C47 C52 121.22(18) . . ? C49 C48 C47 122.2(2) . . ? C50 C49 C48 119.4(2) . . ? C49 C50 C51 119.9(2) . . ? C50 C51 C46 120.4(2) . . ? C47 C52 C54 113.6(2) . . ? C47 C52 C53 109.71(18) . . ? C54 C52 C53 110.5(2) . . ? C60 C55 C56 120.52(19) . . ? C60 C55 N42 117.13(18) . . ? C56 C55 N42 122.04(19) . . ? C57 C56 C55 117.3(2) . . ? C57 C56 C61 120.4(2) . . ? C55 C56 C61 122.26(19) . . ? C58 C57 C56 121.9(2) . . ? C57 C58 C59 120.0(2) . . ? C58 C59 C60 119.4(2) . . ? C59 C60 C55 120.9(2) . . ? C56 C61 C62 112.2(2) . . ? C56 C61 C63 111.0(2) . . ? C62 C61 C63 109.8(2) . . ? O2 C64 C65 111.16(16) . . ? O2 C64 C69 111.27(15) . . ? C65 C64 C69 106.84(16) . . ? O2 C64 C43 107.92(15) . . ? C65 C64 C43 109.86(15) . . ? C69 C64 C43 109.80(16) . . ? C72 C65 C66 108.07(18) . . ? C72 C65 C64 112.72(17) . . ? C66 C65 C64 107.74(17) . . ? C67 C66 C65 109.70(18) . . ? C68 C67 C66 109.77(18) . . ? C68 C67 C70 109.7(2) . . ? C66 C67 C70 109.51(19) . . ? C67 C68 C69 109.97(18) . . ? C73 C69 C68 108.11(18) . . ? C73 C69 C64 113.56(17) . . ? C68 C69 C64 107.22(17) . . ? C67 C70 C71 108.77(19) . . ? C72 C71 C73 108.80(19) . . ? C72 C71 C70 109.7(2) . . ? C73 C71 C70 109.6(2) . . ? C71 C72 C65 110.38(18) . . ? C69 C73 C71 110.06(19) . . ? C2 N1 C6 120.35(16) . . ? C2 N1 Li1 110.02(17) . . ? C6 N1 Li1 125.02(16) . . ? C4 N2 C15 120.21(17) . . ? C4 N2 Li1 111.09(16) . . ? C15 N2 Li1 126.92(16) . . ? C42 N41 C46 120.25(16) . . ? C42 N41 Li2 110.68(16) . . ? C46 N41 Li2 125.70(16) . . ? C44 N42 C55 120.79(17) . . ? C44 N42 Li2 111.91(16) . . ? C55 N42 Li2 122.96(16) . . ? C24 O1 Li2 154.79(17) . . ? C24 O1 Li1 121.48(16) . . ? Li2 O1 Li1 81.80(15) . . ? C64 O2 Li1 154.88(17) . . ? C64 O2 Li2 122.82(16) . . ? Li1 O2 Li2 82.22(16) . . ? O2 Li1 O1 98.24(17) . . ? O2 Li1 N2 128.86(19) . . ? O1 Li1 N2 94.91(16) . . ? O2 Li1 N1 137.6(2) . . ? O1 Li1 N1 93.34(15) . . ? N2 Li1 N1 90.18(15) . . ? O2 Li1 Li2 50.33(12) . . ? O1 Li1 Li2 47.99(12) . . ? N2 Li1 Li2 120.56(17) . . ? N1 Li1 Li2 128.56(17) . . ? O1 Li2 O2 97.61(17) . . ? O1 Li2 N42 129.36(19) . . ? O2 Li2 N42 93.92(16) . . ? O1 Li2 N41 139.3(2) . . ? O2 Li2 N41 93.32(15) . . ? N42 Li2 N41 88.52(14) . . ? O1 Li2 Li1 50.22(12) . . ? O2 Li2 Li1 47.46(12) . . ? N42 Li2 Li1 123.49(18) . . ? N41 Li2 Li1 125.73(16) . . ? #==END # CIF produced by WinGX routine CIF_UPDATE # Created on 1999-12-11 at 13:51:14 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.1beta5 # Request file : C:\chem\wingx\files\archive.dat # CIF files read : f struct data_1f _database_code_CSD 199312 _audit_creation_date 1999-12-11T13:51:14-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C29 H36 F6 N2' _chemical_formula_structural 'C29 H36 F6 N2' _chemical_formula_sum 'C29 H36 F6 N2' _chemical_formula_weight 526.6 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 11.5857(10) _cell_length_b 9.3714(10) _cell_length_c 26.8363(10) _cell_angle_alpha 90.000 _cell_angle_beta 92.389(10) _cell_angle_gamma 90.000 _cell_volume 2911.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71069 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour clear _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.097 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_number 5173 _diffrn_reflns_av_R_equivalents 0.0139 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.962 _diffrn_measured_fraction_theta_max 0.962 _reflns_number_total 4916 _reflns_number_gt 3227 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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^)+(0.0531P)^2^+2.2951P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4916 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0984 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1482 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.04 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.347 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.038 #----------------------------------------------------------------------------# # 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' F F 0.0171 0.0103 '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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group F1A F 0.71038(18) 0.8275(3) 0.00149(7) 0.1014(9) Uani 1 d . . . F1B F 0.8163(2) 0.6537(3) -0.01555(7) 0.1042(8) Uani 1 d . . . F1C F 0.88551(19) 0.8645(3) -0.01715(6) 0.1053(9) Uani 1 d . . . F5C F 1.15793(16) 0.9263(2) 0.17988(6) 0.0762(6) Uani 1 d . . . F5B F 1.10344(18) 1.0517(2) 0.11721(7) 0.0812(6) Uani 1 d . . . F5A F 1.19616(17) 0.8566(3) 0.10757(9) 0.0970(8) Uani 1 d . . . N6 N 0.79454(18) 0.6779(2) 0.09087(8) 0.0408(5) Uani 1 d . . . N19 N 0.95174(17) 0.7651(2) 0.16252(7) 0.0344(5) Uani 1 d . . . C1 C 0.8175(3) 0.7796(4) 0.00798(11) 0.0642(9) Uani 1 d . . . C2 C 0.8562(2) 0.7656(3) 0.06179(9) 0.0431(7) Uani 1 d . . . C3 C 0.9528(2) 0.8377(3) 0.07793(9) 0.0443(7) Uani 1 d . . . C4 C 1.0011(2) 0.8343(3) 0.12778(9) 0.0364(6) Uani 1 d . . . C5 C 1.1144(3) 0.9178(3) 0.13431(10) 0.0501(7) Uani 1 d . . . C7 C 0.6864(2) 0.6061(3) 0.07976(8) 0.0373(6) Uani 1 d . . . C8 C 0.6879(3) 0.4611(3) 0.06468(9) 0.0484(7) Uani 1 d . . . C9 C 0.5797(3) 0.3930(4) 0.05782(11) 0.0603(9) Uani 1 d . . . C10 C 0.4780(3) 0.4640(4) 0.06530(11) 0.0611(9) Uani 1 d . . . C11 C 0.4797(3) 0.6053(4) 0.07987(11) 0.0539(8) Uani 1 d . . . C12 C 0.5835(2) 0.6798(3) 0.08731(9) 0.0430(7) Uani 1 d . . . C13 C 0.5811(3) 0.8355(3) 0.10507(11) 0.0528(7) Uani 1 d . . . C14 C 0.4957(4) 0.9303(5) 0.07436(19) 0.0834(12) Uani 1 d . . . C15 C 0.5551(5) 0.8418(6) 0.15951(15) 0.0810(12) Uani 1 d . . . C16 C 0.7995(4) 0.3792(4) 0.05762(12) 0.0702(10) Uani 1 d . . . C17 C 0.8198(8) 0.2727(9) 0.1002(2) 0.129(2) Uani 1 d . . . C18 C 0.7978(7) 0.2991(10) 0.0081(2) 0.125(3) Uani 1 d . . . C20 C 0.9928(2) 0.7542(3) 0.21351(8) 0.0338(6) Uani 1 d . . . C21 C 0.9376(2) 0.8393(3) 0.24869(9) 0.0415(6) Uani 1 d . . . C22 C 0.9721(3) 0.8230(3) 0.29832(10) 0.0528(8) Uani 1 d . . . C23 C 1.0558(3) 0.7252(4) 0.31247(11) 0.0603(9) Uani 1 d . . . C24 C 1.1064(3) 0.6402(4) 0.27807(12) 0.0578(8) Uani 1 d . . . C25 C 1.0760(2) 0.6517(3) 0.22718(10) 0.0433(6) Uani 1 d . . . C26 C 1.1322(3) 0.5544(3) 0.19007(13) 0.0594(8) Uani 1 d . . . C27 C 1.0957(6) 0.3971(5) 0.1983(3) 0.1053(18) Uani 1 d . . . C28 C 1.2653(4) 0.5634(6) 0.1939(2) 0.0923(13) Uani 1 d . . . C29 C 0.8476(3) 0.9501(3) 0.23265(12) 0.0605(9) Uani 1 d . . . C30 C 0.9053(6) 1.0911(5) 0.2198(2) 0.1003(17) Uani 1 d . . . C31 C 0.7540(4) 0.9785(5) 0.27034(17) 0.0740(10) Uani 1 d . . . H3 H 0.991(2) 0.893(3) 0.0566(10) 0.040(7) Uiso 1 d . . . H6 H 0.825(2) 0.680(3) 0.1216(11) 0.048(8) Uiso 1 d . . . H9 H 0.582(3) 0.297(4) 0.0484(12) 0.072(10) Uiso 1 d . . . H10 H 0.407(3) 0.414(3) 0.0592(11) 0.068(10) Uiso 1 d . . . H11 H 0.407(3) 0.653(3) 0.0852(10) 0.049(8) Uiso 1 d . . . H13 H 0.653(3) 0.873(3) 0.1010(10) 0.047(8) Uiso 1 d . . . H14A H 0.508(4) 0.922(4) 0.0410(17) 0.100(15) Uiso 1 d . . . H14B H 0.403(6) 0.892(6) 0.077(2) 0.17(2) Uiso 1 d . . . H14C H 0.507(4) 1.036(6) 0.0888(17) 0.128(17) Uiso 1 d . . . H15A H 0.473(4) 0.797(4) 0.1645(15) 0.099(14) Uiso 1 d . . . H15B H 0.559(3) 0.932(5) 0.1689(15) 0.093(14) Uiso 1 d . . . H15C H 0.611(4) 0.779(5) 0.1794(16) 0.105(14) Uiso 1 d . . . H16 H 0.868(3) 0.449(4) 0.0542(12) 0.077(11) Uiso 1 d . . . H17A H 0.837(5) 0.339(6) 0.129(2) 0.14(2) Uiso 1 d . . . H17B H 0.781(10) 0.195(13) 0.101(5) 0.33(8) Uiso 1 d . . . H17C H 0.903(5) 0.242(6) 0.0936(18) 0.131(18) Uiso 1 d . . . H18A H 0.740(6) 0.232(7) 0.003(3) 0.18(3) Uiso 1 d . . . H18B H 0.790(5) 0.370(6) -0.021(2) 0.16(3) Uiso 1 d . . . H18C H 0.872(4) 0.251(5) 0.0068(16) 0.108(14) Uiso 1 d . . . H22 H 0.933(3) 0.888(4) 0.3245(12) 0.073(10) Uiso 1 d . . . H23 H 1.080(3) 0.719(3) 0.3471(13) 0.071(9) Uiso 1 d . . . H24 H 1.158(3) 0.574(4) 0.2873(12) 0.066(10) Uiso 1 d . . . H26 H 1.113(3) 0.573(3) 0.1577(13) 0.068(10) Uiso 1 d . . . H27A H 1.017(6) 0.402(7) 0.184(2) 0.17(3) Uiso 1 d . . . H27B H 1.122(4) 0.341(5) 0.1676(17) 0.109(14) Uiso 1 d . . . H27C H 1.105(9) 0.368(11) 0.230(4) 0.30(6) Uiso 1 d . . . H28A H 1.304(5) 0.672(7) 0.194(2) 0.18(2) Uiso 1 d . . . H28B H 1.295(5) 0.513(7) 0.231(2) 0.17(2) Uiso 1 d . . . H28C H 1.292(4) 0.507(5) 0.1652(17) 0.104(14) Uiso 1 d . . . H29 H 0.807(3) 0.918(4) 0.2040(13) 0.073(10) Uiso 1 d . . . H30A H 0.959(4) 1.077(5) 0.1905(18) 0.121(15) Uiso 1 d . . . H30B H 0.846(5) 1.156(6) 0.209(2) 0.15(2) Uiso 1 d . . . H30C H 0.949(4) 1.122(5) 0.2540(19) 0.120(17) Uiso 1 d . . . H31A H 0.699(4) 1.043(5) 0.2576(17) 0.114(17) Uiso 1 d . . . H31B H 0.791(3) 1.022(4) 0.3009(14) 0.084(12) Uiso 1 d . . . H32C H 0.721(4) 0.889(6) 0.2810(17) 0.123(17) Uiso 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 F1A 0.0629(14) 0.186(3) 0.0544(11) 0.0454(14) -0.0125(9) 0.0017(15) F1B 0.129(2) 0.144(2) 0.0391(10) -0.0177(12) -0.0063(11) -0.0205(17) F1C 0.0891(16) 0.186(2) 0.0397(10) 0.0381(12) -0.0088(9) -0.0617(16) F5C 0.0778(13) 0.0990(15) 0.0501(10) 0.0179(9) -0.0189(9) -0.0514(11) F5B 0.0967(15) 0.0728(13) 0.0726(12) 0.0292(10) -0.0147(10) -0.0400(11) F5A 0.0463(12) 0.137(2) 0.1090(17) -0.0341(15) 0.0194(11) -0.0265(12) N6 0.0292(13) 0.0633(15) 0.0297(11) 0.0019(10) -0.0028(9) -0.0045(11) N19 0.0345(12) 0.0350(11) 0.0333(10) -0.0003(9) -0.0019(9) 0.0006(9) C1 0.053(2) 0.104(3) 0.0354(15) 0.0078(17) -0.0026(14) -0.0163(19) C2 0.0330(15) 0.0635(18) 0.0328(13) 0.0044(12) 0.0008(11) -0.0036(13) C3 0.0402(17) 0.0593(18) 0.0337(13) 0.0083(13) 0.0039(11) -0.0088(14) C4 0.0325(15) 0.0413(14) 0.0355(13) 0.0006(11) 0.0026(10) 0.0002(11) C5 0.0509(19) 0.0606(19) 0.0389(14) 0.0040(13) 0.0021(13) -0.0154(15) C7 0.0264(15) 0.0557(17) 0.0295(12) 0.0024(11) -0.0021(10) -0.0047(12) C8 0.0533(19) 0.0581(18) 0.0329(13) -0.0034(12) -0.0071(12) 0.0018(15) C9 0.082(3) 0.052(2) 0.0455(17) -0.0020(14) -0.0126(16) -0.0132(19) C10 0.055(2) 0.076(2) 0.0513(18) 0.0070(16) -0.0095(15) -0.025(2) C11 0.0326(18) 0.081(2) 0.0480(16) 0.0078(15) 0.0010(13) -0.0041(17) C12 0.0327(16) 0.0600(18) 0.0362(13) 0.0070(12) -0.0024(11) -0.0066(13) C13 0.0396(19) 0.0608(19) 0.0585(18) -0.0007(15) 0.0059(14) 0.0028(15) C14 0.092(3) 0.075(3) 0.082(3) 0.011(2) -0.008(2) 0.022(2) C15 0.106(4) 0.073(3) 0.065(2) -0.009(2) 0.005(2) 0.016(3) C16 0.075(3) 0.075(2) 0.0590(19) -0.0196(17) -0.0123(17) 0.024(2) C17 0.148(6) 0.135(5) 0.102(4) 0.001(4) -0.025(4) 0.083(5) C18 0.112(5) 0.168(6) 0.094(4) -0.069(4) -0.015(3) 0.059(5) C20 0.0326(14) 0.0341(13) 0.0342(12) 0.0035(10) -0.0036(10) -0.0086(11) C21 0.0518(17) 0.0349(14) 0.0376(13) 0.0012(11) 0.0006(11) -0.0097(12) C22 0.070(2) 0.0514(17) 0.0370(14) -0.0008(13) 0.0015(14) -0.0116(16) C23 0.074(2) 0.069(2) 0.0374(16) 0.0104(15) -0.0109(15) -0.0131(18) C24 0.052(2) 0.059(2) 0.061(2) 0.0247(16) -0.0121(15) 0.0003(16) C25 0.0382(16) 0.0429(15) 0.0487(15) 0.0090(12) -0.0007(12) -0.0034(12) C26 0.055(2) 0.059(2) 0.064(2) 0.0065(16) 0.0028(16) 0.0179(16) C27 0.094(4) 0.068(3) 0.156(5) -0.033(3) 0.041(4) -0.003(3) C28 0.060(3) 0.109(4) 0.110(4) 0.005(3) 0.021(2) 0.015(3) C29 0.082(2) 0.0531(19) 0.0459(17) -0.0087(14) 0.0019(16) 0.0163(17) C30 0.148(5) 0.059(2) 0.099(3) 0.026(2) 0.061(4) 0.031(3) C31 0.077(3) 0.066(3) 0.081(3) -0.009(2) 0.018(2) 0.008(2) #----------------------------------------------------------------------------# # 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 F1A C1 1.324(4) . ? F1B C1 1.338(4) . ? F1C C1 1.324(4) . ? F5C C5 1.306(3) . ? F5B C5 1.340(3) . ? F5A C5 1.341(4) . ? N6 C2 1.357(3) . ? N6 C7 1.442(3) . ? N19 C4 1.289(3) . ? N19 C20 1.434(3) . ? C1 C2 1.500(4) . ? C2 C3 1.363(4) . ? C3 C4 1.429(3) . ? C4 C5 1.531(4) . ? C7 C12 1.400(4) . ? C7 C8 1.418(4) . ? C8 C9 1.412(4) . ? C8 C16 1.522(4) . ? C9 C10 1.375(5) . ? C10 C11 1.381(5) . ? C11 C12 1.398(4) . ? C12 C13 1.535(4) . ? C13 C15 1.505(5) . ? C13 C14 1.543(5) . ? C16 C18 1.525(5) . ? C16 C17 1.528(7) . ? C20 C25 1.399(4) . ? C20 C21 1.409(4) . ? C21 C22 1.383(4) . ? C21 C29 1.521(4) . ? C22 C23 1.376(5) . ? C23 C24 1.369(5) . ? C24 C25 1.400(4) . ? C25 C26 1.517(4) . ? C26 C28 1.544(5) . ? C26 C27 1.551(6) . ? C29 C30 1.527(6) . ? C29 C31 1.537(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N6 C7 129.6(2) . . ? C4 N19 C20 125.9(2) . . ? F1C C1 F1A 107.7(3) . . ? F1C C1 F1B 106.5(3) . . ? F1A C1 F1B 104.2(3) . . ? F1C C1 C2 112.5(3) . . ? F1A C1 C2 113.4(3) . . ? F1B C1 C2 112.0(3) . . ? N6 C2 C3 124.2(2) . . ? N6 C2 C1 117.6(2) . . ? C3 C2 C1 118.1(2) . . ? C2 C3 C4 124.8(2) . . ? N19 C4 C3 121.3(2) . . ? N19 C4 C5 125.3(2) . . ? C3 C4 C5 113.3(2) . . ? F5C C5 F5B 106.9(2) . . ? F5C C5 F5A 105.9(3) . . ? F5B C5 F5A 106.0(2) . . ? F5C C5 C4 115.8(2) . . ? F5B C5 C4 111.8(2) . . ? F5A C5 C4 110.0(2) . . ? C12 C7 C8 122.3(2) . . ? C12 C7 N6 118.5(2) . . ? C8 C7 N6 119.1(2) . . ? C9 C8 C7 116.7(3) . . ? C9 C8 C16 120.7(3) . . ? C7 C8 C16 122.6(3) . . ? C10 C9 C8 121.6(3) . . ? C9 C10 C11 120.2(3) . . ? C10 C11 C12 121.4(3) . . ? C11 C12 C7 117.8(3) . . ? C11 C12 C13 119.5(3) . . ? C7 C12 C13 122.7(2) . . ? C15 C13 C12 110.2(3) . . ? C15 C13 C14 110.2(3) . . ? C12 C13 C14 113.6(3) . . ? C8 C16 C18 112.1(3) . . ? C8 C16 C17 110.0(4) . . ? C18 C16 C17 109.0(5) . . ? C25 C20 C21 122.7(2) . . ? C25 C20 N19 119.8(2) . . ? C21 C20 N19 117.2(2) . . ? C22 C21 C20 117.5(3) . . ? C22 C21 C29 121.0(3) . . ? C20 C21 C29 121.4(2) . . ? C23 C22 C21 120.7(3) . . ? C24 C23 C22 121.2(3) . . ? C23 C24 C25 121.1(3) . . ? C20 C25 C24 116.8(3) . . ? C20 C25 C26 123.4(2) . . ? C24 C25 C26 119.8(3) . . ? C25 C26 C28 112.2(3) . . ? C25 C26 C27 110.6(3) . . ? C28 C26 C27 108.6(4) . . ? C21 C29 C30 110.7(4) . . ? C21 C29 C31 115.2(3) . . ? C30 C29 C31 109.0(3) . . ? #==END # CIF produced by WinGX routine CIF_UPDATE # Created on 2002-09-16 at 16:50:47 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : c:\wingx\files\archive.dat # CIF files read : fm98t psi_scan struct data_2c _database_code_CSD 199313 _audit_creation_date 2002-09-16T16:50:47-00:00 _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_moiety 'C35 H53 Li1 N2 O3' _chemical_formula_sum 'C35 H53 Li N2 O3' _chemical_formula_weight 556.73 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 m' _symmetry_space_group_name_Hall 'R 3 -2"' _symmetry_Int_Tables_number 160 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x+y, y, z' 'x, x-y, z' '-y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' '-y+1/3, -x+2/3, z+2/3' _cell_length_a 32.123(9) _cell_length_b 32.123(9) _cell_length_c 9.273(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 8287(4) _cell_formula_units_Z 9 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.6 _cell_measurement_theta_max 14 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.004 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 3 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.9815 _exptl_absorpt_correction_T_max 0.9876 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_unetI/netI 0.0746 _diffrn_reflns_number 5339 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.2 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 1817 _reflns_number_gt 1022 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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. Solvent in channels along the C axis was unmodellable. SQUEEZE was used to deal with this density. ; _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^)+(0.0740P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00069(5) _refine_ls_number_reflns 1817 _refine_ls_number_parameters 216 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1434 _refine_ls_wR_factor_gt 0.1257 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.916 _refine_ls_shift/su_max 0.055 _refine_ls_shift/su_mean 0.007 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(4) _refine_diff_density_max 0.15 _refine_diff_density_min -0.125 _refine_diff_density_rms 0.03 #----------------------------------------------------------------------------# # 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 C1 C 0.71013(3) 0.21139(4) 0.24345(13) 0.0430(4) Uani 1 1 d . . . C2 C 0.73936(3) 0.26064(3) 0.2687(2) 0.0488(5) Uani 1 2 d S . . H2 H 0.7238 0.2762 0.3079 0.059 Uiso 1 2 calc SR . . C3 C 0.65842(4) 0.18920(4) 0.29164(17) 0.0635(5) Uani 1 1 d . . . H3A H 0.6375 0.1675 0.2176 0.095 Uiso 1 1 calc R . . H3B H 0.6506 0.2144 0.3079 0.095 Uiso 1 1 calc R . . H3C H 0.6539 0.1715 0.3804 0.095 Uiso 1 1 calc R . . C4 C 0.69474(3) 0.13492(4) 0.16118(14) 0.0466(4) Uani 1 1 d . . . C5 C 0.68689(4) 0.10232(4) 0.27144(16) 0.0509(4) Uani 1 1 d . . . C6 C 0.65993(4) 0.05331(4) 0.2412(2) 0.0718(6) Uani 1 1 d . . . H6 H 0.6544 0.031 0.3149 0.086 Uiso 1 1 calc R . . C7 C 0.64137(4) 0.03690(5) 0.10657(19) 0.0735(6) Uani 1 1 d . . . H7 H 0.623 0.0037 0.0881 0.088 Uiso 1 1 calc R . . C8 C 0.64998(5) 0.06931(5) 0.00011(19) 0.0762(6) Uani 1 1 d . . . H8 H 0.6382 0.0584 -0.0933 0.091 Uiso 1 1 calc R . . C9 C 0.67564(4) 0.11763(4) 0.02724(15) 0.0594(5) Uani 1 1 d . . . H9 H 0.6803 0.1394 -0.0472 0.071 Uiso 1 1 calc R . . C10 C 0.70803(4) 0.11859(4) 0.41866(15) 0.0615(5) Uani 1 1 d . . . H10 H 0.7159 0.1524 0.429 0.074 Uiso 1 1 calc R . . C11 C 0.75554(5) 0.11826(5) 0.4296(2) 0.0889(7) Uani 1 1 d . . . H11A H 0.7492 0.0855 0.4212 0.133 Uiso 1 1 calc R . . H11B H 0.7705 0.1315 0.5219 0.133 Uiso 1 1 calc R . . H11C H 0.7769 0.1376 0.3525 0.133 Uiso 1 1 calc R . . C12 C 0.67571(6) 0.09120(6) 0.54138(19) 0.0947(7) Uani 1 1 d . . . H12A H 0.6668 0.0576 0.5341 0.142 Uiso 1 1 calc R . . H12B H 0.647 0.0939 0.5378 0.142 Uiso 1 1 calc R . . H12C H 0.6923 0.1043 0.6318 0.142 Uiso 1 1 calc R . . C13 C 0.74816(5) 0.25184(5) -0.1323(3) 0.1093(9) Uani 1 2 d S . . H13A H 0.76 0.2785 -0.0634 0.131 Uiso 0.5 1 calc PR . . H13B H 0.7136 0.2305 -0.1173 0.131 Uiso 0.5 1 calc PR . . C14 C 0.75891(14) 0.27010(10) -0.2865(3) 0.1642(17) Uani 0.5 1 d P . . H14A H 0.7325 0.2732 -0.3275 0.197 Uiso 0.5 1 calc PR . . H14B H 0.7887 0.3012 -0.2923 0.197 Uiso 0.5 1 calc PR . . C15 C 0.76339(7) 0.23661(7) -0.3514(4) 0.2178(17) Uani 1 2 d S . . H15A H 0.7845 0.2501 -0.4353 0.261 Uiso 0.5 1 calc PR . . H15B H 0.7319 0.2113 -0.3852 0.261 Uiso 0.5 1 calc PR . . C16 C 0.78263(6) 0.21737(6) -0.2562(3) 0.1363(13) Uani 1 2 d S . . H16A H 0.7679 0.1826 -0.2716 0.164 Uiso 0.5 1 calc PR . . H16B H 0.8174 0.2321 -0.2716 0.164 Uiso 0.5 1 calc PR . . C17 C 0.79879(5) 0.12870(4) 0.0110(2) 0.1042(7) Uani 1 1 d . . . H17A H 0.7725 0.1204 -0.0572 0.125 Uiso 1 1 calc R . . H17B H 0.7856 0.1086 0.0972 0.125 Uiso 1 1 calc R . . C18 C 0.83511(5) 0.12094(6) -0.0539(3) 0.1284(9) Uani 1 1 d . . . H18A H 0.8385 0.0967 0.0008 0.154 Uiso 1 1 calc R . . H18B H 0.8259 0.1093 -0.153 0.154 Uiso 1 1 calc R . . N1 N 0.72504(3) 0.18461(3) 0.18055(11) 0.0451(3) Uani 1 1 d . . . O1 O 0.77360(3) 0.22640(3) -0.11940(14) 0.0795(5) Uani 1 2 d S . . O2 O 0.82142(2) 0.17858(2) 0.04875(17) 0.0750(5) Uani 1 2 d S . . Li1 Li 0.78683(5) 0.21317(5) 0.0804(3) 0.0527(9) Uani 1 2 d S . . O41 O 0.55994(17) 0.10402(13) 0.8450(5) 0.348(3) Uani 0.5 1 d PD . . C42 C 0.55164(7) 0.10327(15) 0.7072(5) 0.330(5) Uani 1 2 d SD . . H42A H 0.5171 0.0885 0.6883 0.396 Uiso 0.5 1 calc PR . . H42B H 0.5641 0.0853 0.6549 0.396 Uiso 0.5 1 calc PR . . C43 C 0.57405(8) 0.14810(15) 0.6688(4) 0.275(3) Uani 1 2 d SD . . H43A H 0.5528 0.1551 0.6105 0.33 Uiso 0.5 1 calc PR . . H43B H 0.6023 0.1551 0.6105 0.33 Uiso 0.5 1 calc PR . . C44 C 0.58753(7) 0.17505(14) 0.7857(5) 0.296(4) Uani 1 2 d SD . . H44A H 0.6226 0.1958 0.7846 0.356 Uiso 0.5 1 calc PR . . H44B H 0.5733 0.1958 0.7846 0.356 Uiso 0.5 1 calc PR . . C45 C 0.57505(11) 0.1501(2) 0.9032(5) 0.350(4) Uani 1 2 d SD . . H45A H 0.5488 0.1515 0.9525 0.42 Uiso 0.5 1 calc PR . . H45B H 0.6022 0.1603 0.9694 0.42 Uiso 0.5 1 calc PR . . 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 0.0375(5) 0.0492(5) 0.0448(7) 0.0031(6) 0.0000(5) 0.0235(4) C2 0.0435(4) 0.0435(4) 0.0707(12) -0.0024(5) 0.0024(5) 0.0302(5) C3 0.0471(5) 0.0615(6) 0.0857(10) 0.0007(7) 0.0068(6) 0.0298(4) C4 0.0370(5) 0.0431(5) 0.0620(8) -0.0069(6) 0.0018(6) 0.0218(3) C5 0.0402(5) 0.0446(5) 0.0681(8) 0.0037(6) 0.0067(6) 0.0213(4) C6 0.0545(6) 0.0515(6) 0.1048(12) 0.0044(8) 0.0108(8) 0.0232(5) C7 0.0474(6) 0.0466(6) 0.1098(11) -0.0175(7) 0.0092(8) 0.0111(5) C8 0.0601(8) 0.0625(7) 0.0860(10) -0.0330(7) -0.0091(8) 0.0157(6) C9 0.0482(6) 0.0567(6) 0.0619(9) -0.0108(7) -0.0059(7) 0.0176(5) C10 0.0636(6) 0.0549(6) 0.0624(9) 0.0106(7) 0.0057(7) 0.0269(5) C11 0.0742(7) 0.0994(9) 0.0908(12) 0.0065(9) -0.0169(8) 0.0418(6) C12 0.0940(10) 0.0890(9) 0.0879(12) 0.0249(9) 0.0146(9) 0.0359(7) C13 0.1516(8) 0.1516(8) 0.0719(16) 0.0003(7) -0.0003(7) 0.1111(9) C14 0.346(3) 0.0900(15) 0.084(2) -0.0241(16) -0.087(2) 0.1293(15) C15 0.3593(16) 0.3593(16) 0.0554(17) 0.0066(12) -0.0066(12) 0.2701(19) C16 0.1823(11) 0.1823(11) 0.0623(16) -0.0107(10) 0.0107(10) 0.1047(14) C17 0.0821(7) 0.0531(6) 0.1806(17) -0.0087(9) 0.0472(9) 0.0362(5) C18 0.0700(8) 0.0764(8) 0.227(2) -0.0403(11) 0.0318(11) 0.0278(6) N1 0.0344(4) 0.0443(4) 0.0530(6) 0.0037(5) 0.0013(5) 0.0171(3) O1 0.1078(4) 0.1078(4) 0.0449(7) -0.0071(4) 0.0071(4) 0.0706(5) O2 0.0510(3) 0.0510(3) 0.1146(11) -0.0146(4) 0.0146(4) 0.0193(4) Li1 0.0570(7) 0.0570(7) 0.0532(18) 0.0029(8) -0.0029(8) 0.0353(8) O41 0.181(3) 0.375(3) 0.480(5) 0.277(3) 0.076(5) 0.135(3) C42 0.556(10) 0.126(3) 0.164(4) -0.028(4) -0.0138(18) 0.0629(17) C43 0.367(6) 0.280(5) 0.149(4) 0.102(4) 0.0511(18) 0.140(3) C44 0.422(8) 0.111(3) 0.252(6) -0.033(4) -0.0164(19) 0.0553(16) C45 0.410(6) 0.576(12) 0.120(3) -0.123(5) -0.062(3) 0.288(6) #----------------------------------------------------------------------------# # 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 1.3121(17) . ? C1 C2 1.3979(13) . ? C1 C3 1.5110(16) . ? C2 C1 1.3979(13) 6_665 ? C4 C9 1.3736(18) . ? C4 C5 1.3936(19) . ? C4 N1 1.4049(13) . ? C5 C6 1.3940(16) . ? C5 C10 1.4977(19) . ? C6 C7 1.370(2) . ? C7 C8 1.359(2) . ? C8 C9 1.3683(18) . ? C10 C12 1.495(2) . ? C10 C11 1.535(2) . ? C13 O1 1.421(3) . ? C13 C14 1.518(4) . ? C14 C15 1.302(5) . ? C15 C16 1.388(5) . ? C16 O1 1.364(3) . ? C17 O2 1.4332(16) . ? C17 C18 1.441(3) . ? C18 C18 1.412(3) 6_665 ? N1 Li1 1.955(2) . ? O1 Li1 1.994(3) . ? O2 C17 1.4333(16) 6_665 ? O2 Li1 1.947(3) . ? Li1 N1 1.955(2) 6_665 ? O41 O41 0.509(12) 4_655 ? O41 C42 1.304(6) . ? O41 C45 1.413(7) . ? C42 C43 1.297(6) . ? C43 C44 1.318(6) . ? C44 C45 1.292(6) . ? 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 C2 123.88(10) . . ? N1 C1 C3 119.86(9) . . ? C2 C1 C3 116.26(12) . . ? C1 C2 C1 128.80(16) . 6_665 ? C9 C4 C5 118.89(10) . . ? C9 C4 N1 119.39(11) . . ? C5 C4 N1 121.48(11) . . ? C4 C5 C6 118.55(13) . . ? C4 C5 C10 121.76(10) . . ? C6 C5 C10 119.65(13) . . ? C7 C6 C5 121.52(15) . . ? C8 C7 C6 118.96(12) . . ? C7 C8 C9 120.79(15) . . ? C8 C9 C4 121.26(13) . . ? C12 C10 C5 115.36(10) . . ? C12 C10 C11 110.23(14) . . ? C5 C10 C11 109.67(13) . . ? O1 C13 C14 102.5(2) . . ? C15 C14 C13 102.4(3) . . ? C14 C15 C16 109.4(3) . . ? O1 C16 C15 107.9(3) . . ? O2 C17 C18 107.07(11) . . ? C18 C18 C17 108.57(7) 6_665 . ? C1 N1 C4 121.93(9) . . ? C1 N1 Li1 121.42(9) . . ? C4 N1 Li1 115.88(11) . . ? C16 O1 C13 106.8(2) . . ? C16 O1 Li1 136.75(19) . . ? C13 O1 Li1 116.49(16) . . ? C17 O2 C17 108.71(16) . 6_665 ? C17 O2 Li1 124.05(8) . . ? C17 O2 Li1 124.05(8) 6_665 . ? O2 Li1 N1 122.61(10) . 6_665 ? O2 Li1 N1 122.61(10) . . ? N1 Li1 N1 95.84(14) 6_665 . ? O2 Li1 O1 102.98(15) . . ? N1 Li1 O1 105.49(12) 6_665 . ? N1 Li1 O1 105.49(12) . . ? O41 O41 C42 78.7(3) 4_655 . ? O41 O41 C45 79.6(2) 4_655 . ? C42 O41 C45 110.7(4) . . ? O41 C42 C43 104.7(4) . . ? C42 C43 C44 108.7(4) . . ? C45 C44 C43 112.8(4) . . ? C44 C45 O41 99.5(4) . . ? #==END # CIF produced by WinGX routine CIF_UPDATE # Created on 2002-08-01 at 11:48:00 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : c:\chem\wingx\files\archive.dat # CIF files read : a dreduc struct sortav data_2g _database_code_CSD 199314 _audit_creation_date 2002-08-01T11:48:00-00:00 _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_moiety 'C38 H42 Li2 N4 O4' _chemical_formula_sum 'C38 H42 Li2 N4 O4' _chemical_formula_weight 632.64 _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 10.6917(4) _cell_length_b 11.8407(5) _cell_length_c 15.3648(9) _cell_angle_alpha 77.010(2) _cell_angle_beta 85.387(2) _cell_angle_gamma 66.242(2) _cell_volume 1734.63(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 73598 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 28.283 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.9732 _exptl_absorpt_correction_T_max 0.977 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _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 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_UB_11 0.991479E-1 _diffrn_orient_matrix_UB_12 -0.307285E-1 _diffrn_orient_matrix_UB_13 -0.154435E-1 _diffrn_orient_matrix_UB_21 -0.246849E-1 _diffrn_orient_matrix_UB_22 0.239624E-1 _diffrn_orient_matrix_UB_23 -0.649233E-1 _diffrn_orient_matrix_UB_31 -0.21379E-2 _diffrn_orient_matrix_UB_32 0.859786E-1 _diffrn_orient_matrix_UB_33 -0.28905E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0748 _diffrn_reflns_av_unetI/netI 0.0854 _diffrn_reflns_number 21314 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.903 _diffrn_measured_fraction_theta_max 0.903 _reflns_number_total 7179 _reflns_number_gt 4221 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _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^)+(0.0779P)^2^+0.1646P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7179 _refine_ls_number_parameters 601 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1183 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1619 _refine_ls_wR_factor_gt 0.135 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.195 _refine_diff_density_min -0.182 _refine_diff_density_rms 0.038 #----------------------------------------------------------------------------# # 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.49857(13) 0.61145(13) 0.33474(10) 0.0499(4) Uani 1 d . . . O2 O 0.92514(15) 0.20664(14) 0.03125(11) 0.0611(5) Uani 1 d . . . N1 N 0.57359(16) 0.48214(15) 0.19958(12) 0.0422(4) Uani 1 d . . . N2 N 0.77111(16) 0.22356(15) 0.18265(12) 0.0455(4) Uani 1 d . . . Li1 Li 0.7548(3) 0.3480(3) 0.2471(3) 0.0508(9) Uani 1 d . . . C1 C 0.3664(2) 0.5524(2) 0.10547(18) 0.0471(5) Uani 1 d . . . C2 C 0.49970(18) 0.45174(19) 0.14806(14) 0.0419(5) Uani 1 d . . . C3 C 0.5365(2) 0.33283(19) 0.13193(14) 0.0429(5) Uani 1 d . . . C4 C 0.6653(2) 0.22840(19) 0.14122(14) 0.0440(5) Uani 1 d . . . C5 C 0.6765(3) 0.1228(2) 0.0981(2) 0.0570(6) Uani 1 d . . . C6 C 0.55891(19) 0.60973(19) 0.18378(15) 0.0444(5) Uani 1 d . . . C7 C 0.53009(19) 0.67350(19) 0.25367(16) 0.0477(6) Uani 1 d . . . C8 C 0.5323(2) 0.7922(2) 0.2424(2) 0.0596(7) Uani 1 d . . . C9 C 0.5598(3) 0.8511(3) 0.1594(2) 0.0688(8) Uani 1 d . . . C10 C 0.5841(3) 0.7925(3) 0.0887(2) 0.0689(8) Uani 1 d . . . C11 C 0.5842(2) 0.6718(2) 0.10077(19) 0.0567(6) Uani 1 d . . . C12 C 0.4486(3) 0.6801(3) 0.4046(2) 0.0627(7) Uani 1 d . . . C13 C 0.9008(2) 0.12201(19) 0.18158(16) 0.0482(5) Uani 1 d . . . C14 C 0.9831(2) 0.1160(2) 0.10618(16) 0.0527(6) Uani 1 d . . . C15 C 1.1148(2) 0.0236(2) 0.1097(2) 0.0622(7) Uani 1 d . . . C16 C 1.1644(3) -0.0654(2) 0.1874(2) 0.0689(8) Uani 1 d . . . C17 C 1.0852(3) -0.0605(2) 0.2625(2) 0.0700(8) Uani 1 d . . . C18 C 0.9549(2) 0.0339(2) 0.25960(19) 0.0584(6) Uani 1 d . . . C19 C 1.0020(3) 0.2031(3) -0.0482(2) 0.0727(8) Uani 1 d . . . H1A H 0.299(2) 0.514(2) 0.1069(16) 0.065(7) Uiso 1 d . . . H1B H 0.324(2) 0.624(2) 0.1372(14) 0.047(6) Uiso 1 d . . . H1C H 0.378(2) 0.586(2) 0.0441(18) 0.063(7) Uiso 1 d . . . H3 H 0.465(2) 0.319(2) 0.1034(15) 0.057(6) Uiso 1 d . . . H5A H 0.588(3) 0.124(2) 0.0909(16) 0.067(7) Uiso 1 d . . . H5B H 0.713(3) 0.138(3) 0.039(2) 0.095(10) Uiso 1 d . . . H5C H 0.730(3) 0.040(2) 0.1369(17) 0.070(7) Uiso 1 d . . . H8 H 0.511(2) 0.836(2) 0.2910(16) 0.051(7) Uiso 1 d . . . H9 H 0.560(3) 0.939(3) 0.1540(18) 0.080(8) Uiso 1 d . . . H10 H 0.603(2) 0.826(2) 0.0321(19) 0.069(8) Uiso 1 d . . . H11 H 0.609(2) 0.6275(19) 0.0547(15) 0.038(6) Uiso 1 d . . . H12A H 0.518(3) 0.704(2) 0.4248(17) 0.074(8) Uiso 1 d . . . H12B H 0.368(3) 0.758(3) 0.3835(18) 0.079(8) Uiso 1 d . . . H12C H 0.423(3) 0.619(3) 0.453(2) 0.091(9) Uiso 1 d . . . H15 H 1.167(2) 0.0289(19) 0.0541(16) 0.051(6) Uiso 1 d . . . H16 H 1.258(3) -0.131(3) 0.1891(19) 0.086(8) Uiso 1 d . . . H17 H 1.118(3) -0.119(3) 0.321(2) 0.095(9) Uiso 1 d . . . H18 H 0.904(2) 0.037(2) 0.3129(18) 0.066(7) Uiso 1 d . . . H19A H 1.082(3) 0.215(2) -0.0346(18) 0.079(8) Uiso 1 d . . . H19B H 1.032(3) 0.115(3) -0.062(2) 0.107(11) Uiso 1 d . . . H19C H 0.936(3) 0.284(3) -0.100(2) 0.099(9) Uiso 1 d . . . O3 O 0.89050(14) 0.42740(14) 0.22040(10) 0.0521(4) Uani 1 d . . . O4 O 0.35241(12) 0.43605(13) 0.36353(10) 0.0492(4) Uani 1 d . . . N3 N 0.76921(15) 0.37530(15) 0.37473(12) 0.0433(4) Uani 1 d . . . N4 N 0.59010(15) 0.24425(15) 0.37810(12) 0.0433(4) Uani 1 d . . . Li2 Li 0.5591(3) 0.4262(3) 0.3420(3) 0.0479(9) Uani 1 d . . . C20 C 0.9712(2) 0.2534(3) 0.4744(2) 0.0525(6) Uani 1 d . . . C21 C 0.83985(18) 0.26892(19) 0.43343(14) 0.0423(5) Uani 1 d . . . C22 C 0.80024(19) 0.1681(2) 0.45900(15) 0.0445(5) Uani 1 d . . . C23 C 0.68365(19) 0.15378(19) 0.43435(14) 0.0436(5) Uani 1 d . . . C24 C 0.6713(3) 0.0322(3) 0.4798(2) 0.0615(7) Uani 1 d . . . C25 C 0.81321(19) 0.47718(19) 0.35937(15) 0.0451(5) Uani 1 d . . . C26 C 0.86809(19) 0.5095(2) 0.27662(16) 0.0473(6) Uani 1 d . . . C27 C 0.8975(2) 0.6165(2) 0.2551(2) 0.0580(7) Uani 1 d . . . C28 C 0.8725(2) 0.6920(2) 0.3165(2) 0.0649(8) Uani 1 d . . . C29 C 0.8200(2) 0.6613(2) 0.3986(2) 0.0636(7) Uani 1 d . . . C30 C 0.7903(2) 0.5548(2) 0.41921(19) 0.0546(6) Uani 1 d . . . C31 C 0.9378(3) 0.4577(3) 0.1322(2) 0.0666(7) Uani 1 d . . . C32 C 0.47919(19) 0.22634(19) 0.34793(14) 0.0434(5) Uani 1 d . . . C33 C 0.35242(19) 0.33086(19) 0.33890(15) 0.0452(5) Uani 1 d . . . C34 C 0.2381(2) 0.3263(2) 0.30468(16) 0.0526(6) Uani 1 d . . . C35 C 0.2483(2) 0.2203(2) 0.27726(18) 0.0582(7) Uani 1 d . . . C36 C 0.3722(2) 0.1191(2) 0.28185(18) 0.0562(6) Uani 1 d . . . C37 C 0.4863(2) 0.1227(2) 0.31694(16) 0.0504(6) Uani 1 d . . . C38 C 0.2307(2) 0.5496(2) 0.3423(2) 0.0573(7) Uani 1 d . . . H20A H 1.012(2) 0.170(2) 0.5099(16) 0.062(7) Uiso 1 d . . . H20B H 0.957(3) 0.319(3) 0.5080(19) 0.081(9) Uiso 1 d . . . H20C H 1.027(3) 0.268(2) 0.4305(18) 0.062(7) Uiso 1 d . . . H22 H 0.861(2) 0.0957(19) 0.5015(14) 0.043(5) Uiso 1 d . . . H24A H 0.716(2) 0.000(2) 0.5347(17) 0.060(7) Uiso 1 d . . . H24B H 0.714(3) -0.034(3) 0.4410(18) 0.074(8) Uiso 1 d . . . H24C H 0.579(3) 0.043(2) 0.4870(18) 0.079(8) Uiso 1 d . . . H27 H 0.934(2) 0.635(2) 0.1978(17) 0.063(7) Uiso 1 d . . . H28 H 0.893(2) 0.764(2) 0.2993(17) 0.069(8) Uiso 1 d . . . H29 H 0.800(2) 0.716(2) 0.4428(17) 0.062(7) Uiso 1 d . . . H30 H 0.750(2) 0.534(2) 0.4797(17) 0.060(7) Uiso 1 d . . . H31A H 0.946(2) 0.391(2) 0.1019(17) 0.065(8) Uiso 1 d . . . H31B H 0.872(2) 0.549(2) 0.0991(16) 0.062(7) Uiso 1 d . . . H31C H 1.031(3) 0.454(3) 0.1329(19) 0.089(9) Uiso 1 d . . . H34 H 0.158(2) 0.3962(19) 0.3029(13) 0.042(5) Uiso 1 d . . . H35 H 0.170(2) 0.220(2) 0.2540(16) 0.062(7) Uiso 1 d . . . H36 H 0.3812(19) 0.044(2) 0.2612(14) 0.042(5) Uiso 1 d . . . H37 H 0.568(2) 0.051(2) 0.3166(14) 0.049(6) Uiso 1 d . . . H38A H 0.251(2) 0.617(2) 0.3618(16) 0.062(7) Uiso 1 d . . . H38B H 0.158(3) 0.537(2) 0.3750(16) 0.058(7) Uiso 1 d . . . H38C H 0.217(2) 0.568(2) 0.2730(19) 0.069(7) Uiso 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 O1 0.0411(8) 0.0479(8) 0.0579(10) -0.0150(8) 0.0006(7) -0.0129(6) O2 0.0482(9) 0.0608(10) 0.0602(11) -0.0047(8) 0.0071(8) -0.0128(7) N1 0.0367(9) 0.0406(9) 0.0460(10) -0.0049(8) -0.0073(7) -0.0128(7) N2 0.0359(9) 0.0426(9) 0.0548(11) -0.0101(8) -0.0002(8) -0.0123(7) Li1 0.0390(18) 0.048(2) 0.060(2) -0.0104(18) -0.0069(16) -0.0110(15) C1 0.0375(11) 0.0456(13) 0.0522(16) -0.0043(12) -0.0072(10) -0.0122(10) C2 0.0336(10) 0.0449(12) 0.0426(12) -0.0016(10) -0.0005(9) -0.0148(9) C3 0.0374(11) 0.0475(13) 0.0439(13) -0.0064(10) -0.0022(9) -0.0182(9) C4 0.0416(11) 0.0424(11) 0.0472(13) -0.0082(10) 0.0023(9) -0.0168(9) C5 0.0512(14) 0.0520(15) 0.0713(19) -0.0150(14) 0.0000(13) -0.0227(12) C6 0.0324(10) 0.0426(12) 0.0526(14) -0.0017(11) -0.0087(9) -0.0119(8) C7 0.0324(10) 0.0407(12) 0.0627(16) -0.0040(11) -0.0105(10) -0.0088(8) C8 0.0453(13) 0.0439(14) 0.086(2) -0.0111(15) -0.0110(13) -0.0132(10) C9 0.0569(15) 0.0493(15) 0.101(2) -0.0034(17) -0.0172(15) -0.0247(12) C10 0.0574(15) 0.0650(18) 0.077(2) 0.0168(17) -0.0173(14) -0.0307(13) C11 0.0516(13) 0.0555(15) 0.0615(17) 0.0002(14) -0.0118(12) -0.0242(11) C12 0.0509(15) 0.0641(17) 0.0722(19) -0.0279(15) -0.0008(13) -0.0145(13) C13 0.0396(11) 0.0423(12) 0.0598(15) -0.0124(11) -0.0004(10) -0.0124(9) C14 0.0458(12) 0.0500(13) 0.0596(16) -0.0111(12) 0.0003(11) -0.0164(10) C15 0.0440(13) 0.0594(15) 0.0753(19) -0.0181(14) 0.0053(13) -0.0115(11) C16 0.0416(14) 0.0627(16) 0.090(2) -0.0215(15) -0.0090(14) -0.0037(12) C17 0.0534(15) 0.0607(16) 0.077(2) -0.0069(15) -0.0138(14) -0.0043(12) C18 0.0476(13) 0.0598(15) 0.0562(16) -0.0087(13) -0.0033(12) -0.0108(11) C19 0.0572(16) 0.089(2) 0.0660(19) -0.0089(17) 0.0152(14) -0.0293(16) O3 0.0405(8) 0.0579(9) 0.0560(10) -0.0078(8) 0.0023(7) -0.0202(7) O4 0.0311(7) 0.0454(8) 0.0635(10) -0.0107(7) -0.0030(6) -0.0073(6) N3 0.0355(9) 0.0446(10) 0.0480(11) -0.0044(8) -0.0066(8) -0.0157(7) N4 0.0299(8) 0.0437(9) 0.0512(11) -0.0041(8) -0.0018(7) -0.0120(7) Li2 0.0336(17) 0.048(2) 0.055(2) -0.0066(17) -0.0052(15) -0.0110(14) C20 0.0369(12) 0.0537(15) 0.0600(17) -0.0027(14) -0.0093(11) -0.0139(11) C21 0.0288(10) 0.0480(12) 0.0450(12) -0.0086(10) -0.0015(9) -0.0103(8) C22 0.0334(10) 0.0423(12) 0.0472(13) -0.0007(10) -0.0039(9) -0.0078(9) C23 0.0331(10) 0.0411(11) 0.0478(13) -0.0024(10) 0.0032(9) -0.0100(8) C24 0.0450(14) 0.0572(16) 0.0720(19) 0.0128(15) -0.0145(13) -0.0208(12) C25 0.0321(10) 0.0435(12) 0.0544(14) -0.0035(11) -0.0102(10) -0.0113(9) C26 0.0301(10) 0.0475(12) 0.0604(15) -0.0075(12) -0.0085(10) -0.0120(9) C27 0.0384(12) 0.0569(15) 0.0750(19) 0.0045(14) -0.0113(12) -0.0225(11) C28 0.0459(13) 0.0474(14) 0.104(2) -0.0052(16) -0.0243(14) -0.0220(11) C29 0.0472(13) 0.0583(16) 0.087(2) -0.0196(16) -0.0184(14) -0.0164(12) C30 0.0428(12) 0.0547(14) 0.0648(17) -0.0102(13) -0.0124(12) -0.0165(10) C31 0.0572(16) 0.077(2) 0.0632(19) -0.0095(16) 0.0062(13) -0.0275(14) C32 0.0343(10) 0.0461(12) 0.0460(13) -0.0013(10) 0.0003(9) -0.0163(9) C33 0.0363(11) 0.0469(12) 0.0484(13) -0.0044(10) 0.0003(9) -0.0152(9) C34 0.0314(11) 0.0555(14) 0.0627(16) -0.0048(12) -0.0027(10) -0.0125(10) C35 0.0445(13) 0.0599(15) 0.0711(17) -0.0045(13) -0.0108(12) -0.0244(11) C36 0.0531(14) 0.0506(14) 0.0676(17) -0.0090(13) -0.0057(12) -0.0240(11) C37 0.0418(12) 0.0428(12) 0.0606(15) -0.0033(11) -0.0018(10) -0.0142(10) C38 0.0343(12) 0.0525(15) 0.072(2) -0.0118(13) -0.0031(12) -0.0041(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C7 1.388(3) . ? O1 C12 1.431(3) . ? O1 Li2 2.000(4) . ? O2 C14 1.373(3) . ? O2 C19 1.415(3) . ? N1 C2 1.356(3) . ? N1 C6 1.420(3) . ? N1 Li1 2.009(4) . ? N1 Li2 2.151(4) . ? N2 C4 1.317(3) . ? N2 C13 1.425(3) . ? N2 Li1 1.898(4) . ? Li1 O3 1.997(4) . ? Li1 N3 2.085(4) . ? Li1 Li2 2.432(5) . ? Li1 C26 2.771(4) . ? C1 C2 1.520(3) . ? C1 H1A 0.99(2) . ? C1 H1B 1.00(2) . ? C1 H1C 0.95(3) . ? C2 C3 1.376(3) . ? C3 C4 1.423(3) . ? C3 H3 1.00(2) . ? C4 C5 1.502(3) . ? C5 H5A 0.96(3) . ? C5 H5B 0.97(3) . ? C5 H5C 0.99(3) . ? C6 C11 1.387(3) . ? C6 C7 1.394(3) . ? C7 C8 1.386(3) . ? C8 C9 1.379(4) . ? C8 H8 0.96(2) . ? C9 C10 1.370(4) . ? C9 H9 1.02(3) . ? C10 C11 1.399(4) . ? C10 H10 0.91(3) . ? C11 H11 0.93(2) . ? C12 H12A 0.98(3) . ? C12 H12B 0.99(3) . ? C12 H12C 1.02(3) . ? C13 C18 1.387(3) . ? C13 C14 1.394(3) . ? C14 C15 1.388(3) . ? C15 C16 1.380(4) . ? C15 H15 0.99(2) . ? C16 C17 1.373(4) . ? C16 H16 0.99(3) . ? C17 C18 1.387(3) . ? C17 H17 0.99(3) . ? C18 H18 0.95(3) . ? C19 H19A 0.97(3) . ? C19 H19B 1.03(3) . ? C19 H19C 1.12(3) . ? O3 C26 1.380(3) . ? O3 C31 1.428(3) . ? O4 C33 1.381(3) . ? O4 C38 1.438(2) . ? O4 Li2 2.168(3) . ? N3 C21 1.343(2) . ? N3 C25 1.430(3) . ? N3 Li2 2.148(3) . ? N4 C23 1.325(2) . ? N4 C32 1.415(2) . ? N4 Li2 1.995(4) . ? C20 C21 1.512(3) . ? C20 H20A 0.95(2) . ? C20 H20B 0.98(3) . ? C20 H20C 0.90(3) . ? C21 C22 1.389(3) . ? C22 C23 1.415(3) . ? C22 H22 0.98(2) . ? C23 C24 1.505(3) . ? C24 H24A 0.93(3) . ? C24 H24B 1.03(3) . ? C24 H24C 0.95(3) . ? C25 C30 1.383(3) . ? C25 C26 1.396(3) . ? C26 C27 1.389(3) . ? C27 C28 1.381(4) . ? C27 H27 0.95(3) . ? C28 C29 1.373(4) . ? C28 H28 0.93(3) . ? C29 C30 1.385(3) . ? C29 H29 0.99(3) . ? C30 H30 1.02(2) . ? C31 H31A 0.97(3) . ? C31 H31B 1.06(2) . ? C31 H31C 0.99(3) . ? C32 C37 1.386(3) . ? C32 C33 1.410(3) . ? C33 C34 1.394(3) . ? C34 C35 1.372(3) . ? C34 H34 0.92(2) . ? C35 C36 1.376(3) . ? C35 H35 0.94(2) . ? C36 C37 1.392(3) . ? C36 H36 0.98(2) . ? C37 H37 0.95(2) . ? C38 H38A 1.01(3) . ? C38 H38B 0.93(2) . ? C38 H38C 1.05(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 O1 C12 118.11(19) . . ? C7 O1 Li2 112.63(17) . . ? C12 O1 Li2 128.5(2) . . ? C14 O2 C19 118.22(19) . . ? C2 N1 C6 118.19(16) . . ? C2 N1 Li1 117.51(17) . . ? C6 N1 Li1 117.43(15) . . ? C2 N1 Li2 117.07(15) . . ? C6 N1 Li2 105.27(17) . . ? Li1 N1 Li2 71.45(15) . . ? C4 N2 C13 120.20(18) . . ? C4 N2 Li1 121.42(17) . . ? C13 N2 Li1 118.36(17) . . ? N2 Li1 O3 116.9(2) . . ? N2 Li1 N1 99.98(17) . . ? O3 Li1 N1 106.57(17) . . ? N2 Li1 N3 143.2(2) . . ? O3 Li1 N3 82.01(15) . . ? N1 Li1 N3 104.36(18) . . ? N2 Li1 Li2 120.89(19) . . ? O3 Li1 Li2 121.69(19) . . ? N1 Li1 Li2 56.99(13) . . ? N3 Li1 Li2 56.17(13) . . ? N2 Li1 C26 144.95(19) . . ? O3 Li1 C26 28.13(8) . . ? N1 Li1 C26 96.71(14) . . ? N3 Li1 C26 58.20(11) . . ? Li2 Li1 C26 94.03(16) . . ? C2 C1 H1A 109.1(13) . . ? C2 C1 H1B 113.6(12) . . ? H1A C1 H1B 106.5(18) . . ? C2 C1 H1C 111.8(14) . . ? H1A C1 H1C 107(2) . . ? H1B C1 H1C 108.9(19) . . ? N1 C2 C3 124.03(17) . . ? N1 C2 C1 119.52(19) . . ? C3 C2 C1 116.44(19) . . ? C2 C3 C4 130.49(19) . . ? C2 C3 H3 115.9(12) . . ? C4 C3 H3 113.3(13) . . ? N2 C4 C3 123.27(19) . . ? N2 C4 C5 120.75(19) . . ? C3 C4 C5 115.96(19) . . ? C4 C5 H5A 110.6(15) . . ? C4 C5 H5B 107.4(18) . . ? H5A C5 H5B 107(2) . . ? C4 C5 H5C 110.6(15) . . ? H5A C5 H5C 106(2) . . ? H5B C5 H5C 115(2) . . ? C11 C6 C7 117.5(2) . . ? C11 C6 N1 121.6(2) . . ? C7 C6 N1 120.65(19) . . ? C8 C7 O1 122.2(2) . . ? C8 C7 C6 121.7(2) . . ? O1 C7 C6 116.06(18) . . ? C9 C8 C7 119.6(3) . . ? C9 C8 H8 119.5(13) . . ? C7 C8 H8 120.9(13) . . ? C10 C9 C8 120.0(3) . . ? C10 C9 H9 123.0(15) . . ? C8 C9 H9 117.0(15) . . ? C9 C10 C11 120.2(3) . . ? C9 C10 H10 124.7(17) . . ? C11 C10 H10 115.1(17) . . ? C6 C11 C10 120.9(3) . . ? C6 C11 H11 117.8(12) . . ? C10 C11 H11 121.1(13) . . ? O1 C12 H12A 111.9(16) . . ? O1 C12 H12B 110.2(16) . . ? H12A C12 H12B 108(2) . . ? O1 C12 H12C 103.1(17) . . ? H12A C12 H12C 113(2) . . ? H12B C12 H12C 111(2) . . ? C18 C13 C14 118.0(2) . . ? C18 C13 N2 120.0(2) . . ? C14 C13 N2 121.61(19) . . ? O2 C14 C15 123.9(2) . . ? O2 C14 C13 115.55(18) . . ? C15 C14 C13 120.5(2) . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 124.7(12) . . ? C14 C15 H15 115.1(13) . . ? C17 C16 C15 120.0(2) . . ? C17 C16 H16 120.3(16) . . ? C15 C16 H16 119.7(16) . . ? C16 C17 C18 119.7(3) . . ? C16 C17 H17 123.3(17) . . ? C18 C17 H17 116.9(18) . . ? C13 C18 C17 121.5(3) . . ? C13 C18 H18 120.8(15) . . ? C17 C18 H18 117.7(15) . . ? O2 C19 H19A 105.4(17) . . ? O2 C19 H19B 108.7(18) . . ? H19A C19 H19B 109(2) . . ? O2 C19 H19C 106.0(15) . . ? H19A C19 H19C 111(2) . . ? H19B C19 H19C 116(2) . . ? C26 O3 C31 118.7(2) . . ? C26 O3 Li1 108.86(16) . . ? C31 O3 Li1 122.5(2) . . ? C33 O4 C38 116.37(17) . . ? C33 O4 Li2 105.58(15) . . ? C38 O4 Li2 124.83(17) . . ? C21 N3 C25 118.56(16) . . ? C21 N3 Li1 113.99(17) . . ? C25 N3 Li1 104.03(16) . . ? C21 N3 Li2 121.69(15) . . ? C25 N3 Li2 115.71(14) . . ? Li1 N3 Li2 70.11(15) . . ? C23 N4 C32 121.62(17) . . ? C23 N4 Li2 127.90(17) . . ? C32 N4 Li2 109.49(15) . . ? N4 Li2 O1 165.0(2) . . ? N4 Li2 N3 88.84(14) . . ? O1 Li2 N3 96.35(15) . . ? N4 Li2 N1 111.08(19) . . ? O1 Li2 N1 82.29(14) . . ? N3 Li2 N1 97.56(15) . . ? N4 Li2 O4 77.99(13) . . ? O1 Li2 O4 92.27(14) . . ? N3 Li2 O4 157.0(2) . . ? N1 Li2 O4 104.72(15) . . ? N4 Li2 Li1 83.05(16) . . ? O1 Li2 Li1 111.38(18) . . ? N3 Li2 Li1 53.72(12) . . ? N1 Li2 Li1 51.56(12) . . ? O4 Li2 Li1 140.7(2) . . ? C21 C20 H20A 109.0(14) . . ? C21 C20 H20B 112.0(15) . . ? H20A C20 H20B 113(2) . . ? C21 C20 H20C 109.1(15) . . ? H20A C20 H20C 111(2) . . ? H20B C20 H20C 103(2) . . ? N3 C21 C22 123.52(17) . . ? N3 C21 C20 120.04(19) . . ? C22 C21 C20 116.43(18) . . ? C21 C22 C23 130.27(18) . . ? C21 C22 H22 115.4(11) . . ? C23 C22 H22 114.3(11) . . ? N4 C23 C22 121.60(18) . . ? N4 C23 C24 123.16(18) . . ? C22 C23 C24 115.18(18) . . ? C23 C24 H24A 110.9(14) . . ? C23 C24 H24B 110.0(14) . . ? H24A C24 H24B 108(2) . . ? C23 C24 H24C 111.5(15) . . ? H24A C24 H24C 110(2) . . ? H24B C24 H24C 106(2) . . ? C30 C25 C26 117.7(2) . . ? C30 C25 N3 122.8(2) . . ? C26 C25 N3 119.1(2) . . ? O3 C26 C27 124.0(2) . . ? O3 C26 C25 114.91(18) . . ? C27 C26 C25 121.1(2) . . ? O3 C26 Li1 43.01(11) . . ? C27 C26 Li1 154.75(19) . . ? C25 C26 Li1 76.61(15) . . ? C28 C27 C26 119.5(3) . . ? C28 C27 H27 122.5(15) . . ? C26 C27 H27 117.9(15) . . ? C29 C28 C27 120.5(3) . . ? C29 C28 H28 122.5(16) . . ? C27 C28 H28 117.1(16) . . ? C28 C29 C30 119.5(3) . . ? C28 C29 H29 121.0(14) . . ? C30 C29 H29 119.4(14) . . ? C25 C30 C29 121.8(3) . . ? C25 C30 H30 119.2(13) . . ? C29 C30 H30 119.0(13) . . ? O3 C31 H31A 107.7(15) . . ? O3 C31 H31B 110.5(13) . . ? H31A C31 H31B 114(2) . . ? O3 C31 H31C 111.6(17) . . ? H31A C31 H31C 104(2) . . ? H31B C31 H31C 109(2) . . ? C37 C32 C33 117.13(18) . . ? C37 C32 N4 126.41(18) . . ? C33 C32 N4 116.01(19) . . ? O4 C33 C34 123.71(19) . . ? O4 C33 C32 115.36(17) . . ? C34 C33 C32 120.9(2) . . ? C35 C34 C33 120.1(2) . . ? C35 C34 H34 123.5(13) . . ? C33 C34 H34 116.4(13) . . ? C34 C35 C36 120.1(2) . . ? C34 C35 H35 118.5(15) . . ? C36 C35 H35 121.4(15) . . ? C35 C36 C37 119.9(2) . . ? C35 C36 H36 120.8(11) . . ? C37 C36 H36 119.3(11) . . ? C32 C37 C36 121.7(2) . . ? C32 C37 H37 123.0(13) . . ? C36 C37 H37 115.3(13) . . ? O4 C38 H38A 105.6(13) . . ? O4 C38 H38B 108.8(14) . . ? H38A C38 H38B 110(2) . . ? O4 C38 H38C 106.0(14) . . ? H38A C38 H38C 112.6(19) . . ? H38B C38 H38C 113(2) . . ? 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 C4 N2 Li1 O3 -129.6(2) . . . . ? C13 N2 Li1 O3 51.8(3) . . . . ? C4 N2 Li1 N1 -15.2(3) . . . . ? C13 N2 Li1 N1 166.24(16) . . . . ? C4 N2 Li1 N3 115.7(3) . . . . ? C13 N2 Li1 N3 -62.9(4) . . . . ? C4 N2 Li1 Li2 42.2(3) . . . . ? C13 N2 Li1 Li2 -136.4(2) . . . . ? C4 N2 Li1 C26 -132.4(3) . . . . ? C13 N2 Li1 C26 49.0(4) . . . . ? C2 N1 Li1 N2 9.0(2) . . . . ? C6 N1 Li1 N2 -141.53(18) . . . . ? Li2 N1 Li1 N2 120.49(19) . . . . ? C2 N1 Li1 O3 131.10(18) . . . . ? C6 N1 Li1 O3 -19.4(3) . . . . ? Li2 N1 Li1 O3 -117.4(2) . . . . ? C2 N1 Li1 N3 -143.12(17) . . . . ? C6 N1 Li1 N3 66.4(2) . . . . ? Li2 N1 Li1 N3 -31.62(15) . . . . ? C2 N1 Li1 Li2 -111.50(18) . . . . ? C6 N1 Li1 Li2 98.0(2) . . . . ? C2 N1 Li1 C26 158.05(15) . . . . ? C6 N1 Li1 C26 7.5(2) . . . . ? Li2 N1 Li1 C26 -90.46(15) . . . . ? C6 N1 C2 C3 155.18(19) . . . . ? Li1 N1 C2 C3 4.9(3) . . . . ? Li2 N1 C2 C3 -77.3(2) . . . . ? C6 N1 C2 C1 -25.7(3) . . . . ? Li1 N1 C2 C1 -175.99(19) . . . . ? Li2 N1 C2 C1 101.9(2) . . . . ? N1 C2 C3 C4 -18.8(4) . . . . ? C1 C2 C3 C4 162.1(2) . . . . ? C13 N2 C4 C3 -173.58(19) . . . . ? Li1 N2 C4 C3 7.9(3) . . . . ? C13 N2 C4 C5 4.6(3) . . . . ? Li1 N2 C4 C5 -174.0(2) . . . . ? C2 C3 C4 N2 11.7(4) . . . . ? C2 C3 C4 C5 -166.6(2) . . . . ? C2 N1 C6 C11 -57.4(3) . . . . ? Li1 N1 C6 C11 92.9(2) . . . . ? Li2 N1 C6 C11 169.64(18) . . . . ? C2 N1 C6 C7 128.3(2) . . . . ? Li1 N1 C6 C7 -81.3(2) . . . . ? Li2 N1 C6 C7 -4.6(2) . . . . ? C12 O1 C7 C8 8.9(3) . . . . ? Li2 O1 C7 C8 -162.03(18) . . . . ? C12 O1 C7 C6 -170.85(18) . . . . ? Li2 O1 C7 C6 18.2(2) . . . . ? C11 C6 C7 C8 -2.8(3) . . . . ? N1 C6 C7 C8 171.69(17) . . . . ? C11 C6 C7 O1 176.92(17) . . . . ? N1 C6 C7 O1 -8.6(2) . . . . ? O1 C7 C8 C9 -177.75(19) . . . . ? C6 C7 C8 C9 2.0(3) . . . . ? C7 C8 C9 C10 0.2(3) . . . . ? C8 C9 C10 C11 -1.4(4) . . . . ? C7 C6 C11 C10 1.6(3) . . . . ? N1 C6 C11 C10 -172.85(19) . . . . ? C9 C10 C11 C6 0.5(3) . . . . ? C4 N2 C13 C18 -111.6(2) . . . . ? Li1 N2 C13 C18 66.9(3) . . . . ? C4 N2 C13 C14 75.8(3) . . . . ? Li1 N2 C13 C14 -105.6(3) . . . . ? C19 O2 C14 C15 2.4(4) . . . . ? C19 O2 C14 C13 -178.0(2) . . . . ? C18 C13 C14 O2 -179.0(2) . . . . ? N2 C13 C14 O2 -6.4(3) . . . . ? C18 C13 C14 C15 0.6(3) . . . . ? N2 C13 C14 C15 173.2(2) . . . . ? O2 C14 C15 C16 -178.9(2) . . . . ? C13 C14 C15 C16 1.5(4) . . . . ? C14 C15 C16 C17 -2.0(4) . . . . ? C15 C16 C17 C18 0.3(4) . . . . ? C14 C13 C18 C17 -2.3(4) . . . . ? N2 C13 C18 C17 -175.1(2) . . . . ? C16 C17 C18 C13 1.9(4) . . . . ? N2 Li1 O3 C26 -176.63(17) . . . . ? N1 Li1 O3 C26 72.7(2) . . . . ? N3 Li1 O3 C26 -30.01(16) . . . . ? Li2 Li1 O3 C26 11.6(3) . . . . ? N2 Li1 O3 C31 38.4(3) . . . . ? N1 Li1 O3 C31 -72.3(3) . . . . ? N3 Li1 O3 C31 -175.02(19) . . . . ? Li2 Li1 O3 C31 -133.4(2) . . . . ? C26 Li1 O3 C31 -145.0(3) . . . . ? N2 Li1 N3 C21 18.9(4) . . . . ? O3 Li1 N3 C21 -106.12(16) . . . . ? N1 Li1 N3 C21 148.73(16) . . . . ? Li2 Li1 N3 C21 116.77(17) . . . . ? C26 Li1 N3 C21 -122.23(15) . . . . ? N2 Li1 N3 C25 149.5(3) . . . . ? O3 Li1 N3 C25 24.46(15) . . . . ? N1 Li1 N3 C25 -80.69(18) . . . . ? Li2 Li1 N3 C25 -112.65(16) . . . . ? C26 Li1 N3 C25 8.35(11) . . . . ? N2 Li1 N3 Li2 -97.8(3) . . . . ? O3 Li1 N3 Li2 137.11(16) . . . . ? N1 Li1 N3 Li2 31.96(15) . . . . ? C26 Li1 N3 Li2 121.00(13) . . . . ? C23 N4 Li2 O1 -85.7(8) . . . . ? C32 N4 Li2 O1 82.9(8) . . . . ? C23 N4 Li2 N3 24.8(3) . . . . ? C32 N4 Li2 N3 -166.54(15) . . . . ? C23 N4 Li2 N1 122.5(2) . . . . ? C32 N4 Li2 N1 -68.9(2) . . . . ? C23 N4 Li2 O4 -136.21(19) . . . . ? C32 N4 Li2 O4 32.45(17) . . . . ? C23 N4 Li2 Li1 78.4(2) . . . . ? C32 N4 Li2 Li1 -112.97(17) . . . . ? C7 O1 Li2 N4 -169.6(7) . . . . ? C12 O1 Li2 N4 20.7(8) . . . . ? C7 O1 Li2 N3 80.79(18) . . . . ? C12 O1 Li2 N3 -88.9(2) . . . . ? C7 O1 Li2 N1 -16.02(16) . . . . ? C12 O1 Li2 N1 174.24(18) . . . . ? C7 O1 Li2 O4 -120.58(15) . . . . ? C12 O1 Li2 O4 69.7(2) . . . . ? C7 O1 Li2 Li1 27.4(2) . . . . ? C12 O1 Li2 Li1 -142.4(2) . . . . ? C21 N3 Li2 N4 -24.3(2) . . . . ? C25 N3 Li2 N4 178.65(17) . . . . ? Li1 N3 Li2 N4 82.22(16) . . . . ? C21 N3 Li2 O1 141.54(19) . . . . ? C25 N3 Li2 O1 -15.5(2) . . . . ? Li1 N3 Li2 O1 -111.92(18) . . . . ? C21 N3 Li2 N1 -135.43(18) . . . . ? C25 N3 Li2 N1 67.5(2) . . . . ? Li1 N3 Li2 N1 -28.89(14) . . . . ? C21 N3 Li2 O4 30.2(6) . . . . ? C25 N3 Li2 O4 -126.8(5) . . . . ? Li1 N3 Li2 O4 136.7(5) . . . . ? C21 N3 Li2 Li1 -106.5(2) . . . . ? C25 N3 Li2 Li1 96.42(19) . . . . ? C2 N1 Li2 N4 50.2(2) . . . . ? C6 N1 Li2 N4 -176.20(15) . . . . ? Li1 N1 Li2 N4 -61.86(17) . . . . ? C2 N1 Li2 O1 -122.69(16) . . . . ? C6 N1 Li2 O1 10.91(15) . . . . ? Li1 N1 Li2 O1 125.24(16) . . . . ? C2 N1 Li2 N3 141.89(16) . . . . ? C6 N1 Li2 N3 -84.52(16) . . . . ? Li1 N1 Li2 N3 29.82(15) . . . . ? C2 N1 Li2 O4 -32.4(2) . . . . ? C6 N1 Li2 O4 101.24(16) . . . . ? Li1 N1 Li2 O4 -144.43(19) . . . . ? C2 N1 Li2 Li1 112.07(19) . . . . ? C6 N1 Li2 Li1 -114.34(16) . . . . ? C33 O4 Li2 N4 -33.16(17) . . . . ? C38 O4 Li2 N4 -172.3(2) . . . . ? C33 O4 Li2 O1 158.38(15) . . . . ? C38 O4 Li2 O1 19.3(3) . . . . ? C33 O4 Li2 N3 -89.5(5) . . . . ? C38 O4 Li2 N3 131.4(5) . . . . ? C33 O4 Li2 N1 75.76(18) . . . . ? C38 O4 Li2 N1 -63.3(3) . . . . ? C33 O4 Li2 Li1 29.7(3) . . . . ? C38 O4 Li2 Li1 -109.4(3) . . . . ? N2 Li1 Li2 N4 42.5(2) . . . . ? O3 Li1 Li2 N4 -146.1(2) . . . . ? N1 Li1 Li2 N4 124.02(17) . . . . ? N3 Li1 Li2 N4 -93.68(14) . . . . ? C26 Li1 Li2 N4 -140.60(14) . . . . ? N2 Li1 Li2 O1 -141.9(2) . . . . ? O3 Li1 Li2 O1 29.6(3) . . . . ? N1 Li1 Li2 O1 -60.36(16) . . . . ? N3 Li1 Li2 O1 81.95(17) . . . . ? C26 Li1 Li2 O1 35.03(19) . . . . ? N2 Li1 Li2 N3 136.2(2) . . . . ? O3 Li1 Li2 N3 -52.38(18) . . . . ? N1 Li1 Li2 N3 -142.30(18) . . . . ? C26 Li1 Li2 N3 -46.92(11) . . . . ? N2 Li1 Li2 N1 -81.5(2) . . . . ? O3 Li1 Li2 N1 89.9(2) . . . . ? N3 Li1 Li2 N1 142.30(18) . . . . ? C26 Li1 Li2 N1 95.39(14) . . . . ? N2 Li1 Li2 O4 -18.8(4) . . . . ? O3 Li1 Li2 O4 152.7(2) . . . . ? N1 Li1 Li2 O4 62.7(3) . . . . ? N3 Li1 Li2 O4 -155.0(3) . . . . ? C26 Li1 Li2 O4 158.1(2) . . . . ? C25 N3 C21 C22 174.6(2) . . . . ? Li1 N3 C21 C22 -62.4(3) . . . . ? Li2 N3 C21 C22 18.2(3) . . . . ? C25 N3 C21 C20 -6.4(3) . . . . ? Li1 N3 C21 C20 116.6(2) . . . . ? Li2 N3 C21 C20 -162.8(2) . . . . ? N3 C21 C22 C23 -2.0(4) . . . . ? C20 C21 C22 C23 178.9(2) . . . . ? C32 N4 C23 C22 174.92(19) . . . . ? Li2 N4 C23 C22 -17.6(3) . . . . ? C32 N4 C23 C24 -8.1(3) . . . . ? Li2 N4 C23 C24 159.4(2) . . . . ? C21 C22 C23 N4 0.3(4) . . . . ? C21 C22 C23 C24 -177.0(3) . . . . ? C21 N3 C25 C30 -75.8(2) . . . . ? Li1 N3 C25 C30 156.35(19) . . . . ? Li2 N3 C25 C30 81.9(2) . . . . ? C21 N3 C25 C26 111.5(2) . . . . ? Li1 N3 C25 C26 -16.3(2) . . . . ? Li2 N3 C25 C26 -90.7(2) . . . . ? C31 O3 C26 C27 -4.6(3) . . . . ? Li1 O3 C26 C27 -151.17(19) . . . . ? C31 O3 C26 C25 175.83(19) . . . . ? Li1 O3 C26 C25 29.3(2) . . . . ? C31 O3 C26 Li1 146.6(2) . . . . ? C30 C25 C26 O3 179.08(16) . . . . ? N3 C25 C26 O3 -7.9(2) . . . . ? C30 C25 C26 C27 -0.5(3) . . . . ? N3 C25 C26 C27 172.52(17) . . . . ? C30 C25 C26 Li1 -160.86(18) . . . . ? N3 C25 C26 Li1 12.14(16) . . . . ? N2 Li1 C26 O3 5.2(3) . . . . ? N1 Li1 C26 O3 -112.9(2) . . . . ? N3 Li1 C26 O3 144.35(19) . . . . ? Li2 Li1 C26 O3 -170.1(2) . . . . ? N2 Li1 C26 C27 74.8(5) . . . . ? O3 Li1 C26 C27 69.5(5) . . . . ? N1 Li1 C26 C27 -43.4(5) . . . . ? N3 Li1 C26 C27 -146.1(4) . . . . ? Li2 Li1 C26 C27 -100.6(5) . . . . ? N2 Li1 C26 C25 -147.6(3) . . . . ? O3 Li1 C26 C25 -152.9(2) . . . . ? N1 Li1 C26 C25 94.23(17) . . . . ? N3 Li1 C26 C25 -8.52(11) . . . . ? Li2 Li1 C26 C25 37.02(15) . . . . ? O3 C26 C27 C28 -179.35(18) . . . . ? C25 C26 C27 C28 0.2(3) . . . . ? Li1 C26 C27 C28 130.2(4) . . . . ? C26 C27 C28 C29 0.6(3) . . . . ? C27 C28 C29 C30 -1.0(3) . . . . ? C26 C25 C30 C29 0.1(3) . . . . ? N3 C25 C30 C29 -172.65(18) . . . . ? C28 C29 C30 C25 0.6(3) . . . . ? C23 N4 C32 C37 -46.5(3) . . . . ? Li2 N4 C32 C37 144.0(2) . . . . ? C23 N4 C32 C33 141.5(2) . . . . ? Li2 N4 C32 C33 -28.0(2) . . . . ? C38 O4 C33 C34 -7.3(3) . . . . ? Li2 O4 C33 C34 -150.4(2) . . . . ? C38 O4 C33 C32 170.8(2) . . . . ? Li2 O4 C33 C32 27.7(2) . . . . ? C37 C32 C33 O4 -174.74(18) . . . . ? N4 C32 C33 O4 -2.0(3) . . . . ? C37 C32 C33 C34 3.4(3) . . . . ? N4 C32 C33 C34 176.17(19) . . . . ? O4 C33 C34 C35 176.5(2) . . . . ? C32 C33 C34 C35 -1.5(3) . . . . ? C33 C34 C35 C36 -1.3(4) . . . . ? C34 C35 C36 C37 2.0(4) . . . . ? C33 C32 C37 C36 -2.7(3) . . . . ? N4 C32 C37 C36 -174.6(2) . . . . ? C35 C36 C37 C32 0.1(4) . . . . ?