# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Zofia Janas' _publ_contact_author_email zj@wchuwr.pl _publ_section_title ; Lithium complexes supported by tripodal diaminebis(aryloxide) ligands: S ynthesis and structure. ; _publ_author_name Z.Janas data_1b(C48H68Li4N2O6) _database_code_depnum_ccdc_archive 'CCDC 832240' #TrackingRef '- MS_Janas.cif' # CCDC 832240 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H68 Li4 N4 O6' _chemical_formula_sum 'C48 H68 Li4 N4 O6' _chemical_formula_weight 824.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_space_group_name_H-M 'P b c n' _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2-y,1/2+z 3 1/2+x,1/2-y,-z 4 -x,y,1/2-z 5 -x,-y,-z 6 1/2+x,1/2+y,1/2-z 7 1/2-x,1/2+y,z 8 x,-y,1/2+z _cell_length_a 11.397(3) _cell_length_b 17.772(4) _cell_length_c 22.892(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4636.7(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3443 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.163 _exptl_crystal_size_mid 0.152 _exptl_crystal_size_min 0.063 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kuma KM-4 CCD kappa-axis diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33997 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5567 _reflns_number_gt 4256 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD. Version 1.171.33 (Oxford Diffraction, 2009) ; _computing_cell_refinement ; CrysAlis RED. Version 1.171.33 Oxford Diffraction, 2009) ; _computing_data_reduction ; CrysAlis RED. Version 1.171.33 (Oxford Diffraction, 2009) ; _computing_structure_solution 'SHELXTL. Version 6.14 (Bruker, 2003)' _computing_structure_refinement 'SHELXTL. Version 6.14 (Bruker, 2003)' _computing_molecular_graphics ' DIAMOND. Version 3.1f. (Brandenburg, K. 2007)' _computing_publication_material ; SHELXTL. Version 6.14 (Bruker, 2003) publCIF Version 1.0_c (Westrip, S. P. 2007) ; _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^)+(0.0616P)^2^+0.4283P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5567 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.59138(17) 0.39515(11) 0.70801(8) 0.0223(4) Uani 1 1 d . . . Li2 Li 0.43047(17) 0.28149(11) 0.70757(8) 0.0220(4) Uani 1 1 d . . . O11 O 0.41899(7) 0.39700(4) 0.70374(3) 0.02066(18) Uani 1 1 d . . . O21 O 0.59980(7) 0.28086(4) 0.70967(3) 0.01920(17) Uani 1 1 d . . . N1 N 0.59562(8) 0.40041(5) 0.60953(4) 0.0204(2) Uani 1 1 d . . . N2 N 0.75473(9) 0.47128(6) 0.69355(4) 0.0254(2) Uani 1 1 d . . . C1 C 0.49262(10) 0.44308(7) 0.58795(5) 0.0244(3) Uani 1 1 d . B . H1A H 0.4992 0.4473 0.5458 0.029 Uiso 1 1 calc R . . H1B H 0.4968 0.4936 0.6038 0.029 Uiso 1 1 calc R . . C2 C 0.59622(10) 0.32179(6) 0.58779(5) 0.0214(2) Uani 1 1 d . B . H2A H 0.6070 0.3220 0.5458 0.026 Uiso 1 1 calc R . . H2B H 0.5210 0.2986 0.5961 0.026 Uiso 1 1 calc R . . C3 C 0.70300(11) 0.44082(7) 0.59206(5) 0.0249(3) Uani 1 1 d . B . H3A H 0.6922 0.4623 0.5535 0.030 Uiso 1 1 calc R . . H3B H 0.7681 0.4058 0.5902 0.030 Uiso 1 1 calc R . . C4 C 0.73114(11) 0.50293(6) 0.63532(5) 0.0254(3) Uani 1 1 d . B . H4A H 0.7993 0.5308 0.6220 0.031 Uiso 1 1 calc R . . H4B H 0.6655 0.5376 0.6376 0.031 Uiso 1 1 calc R . . C5 C 0.75043(14) 0.53093(7) 0.73779(6) 0.0372(3) Uani 1 1 d . B . H5A H 0.8077 0.5688 0.7287 0.056 Uiso 1 1 calc R . . H5B H 0.7671 0.5099 0.7755 0.056 Uiso 1 1 calc R . . H5C H 0.6737 0.5532 0.7381 0.056 Uiso 1 1 calc R . . C6 C 0.87110(11) 0.43525(8) 0.69396(7) 0.0371(3) Uani 1 1 d . B . H6A H 0.9286 0.4699 0.6792 0.056 Uiso 1 1 calc R . . H6B H 0.8694 0.3912 0.6697 0.056 Uiso 1 1 calc R . . H6C H 0.8912 0.4212 0.7332 0.056 Uiso 1 1 calc R . . C11 C 0.34280(10) 0.39217(6) 0.66022(5) 0.0194(2) Uani 1 1 d . B . C12 C 0.37344(10) 0.41153(6) 0.60193(5) 0.0207(2) Uani 1 1 d . . . C13 C 0.28920(11) 0.40595(6) 0.55790(5) 0.0245(3) Uani 1 1 d . B . H13A H 0.3107 0.4189 0.5200 0.029 Uiso 1 1 calc R . . C14 C 0.17442(11) 0.38195(6) 0.56784(5) 0.0261(3) Uani 1 1 d . . . C15 C 0.14603(10) 0.36032(6) 0.62441(6) 0.0256(3) Uani 1 1 d . B . H15A H 0.0708 0.3428 0.6324 0.031 Uiso 1 1 calc R . . C16 C 0.22818(10) 0.36442(6) 0.66933(5) 0.0225(2) Uani 1 1 d . . . H16A H 0.2069 0.3484 0.7065 0.027 Uiso 1 1 calc R B . C17 C 0.08475(12) 0.38063(8) 0.51916(6) 0.0370(3) Uani 1 1 d . B . H17A H 0.1138 0.3506 0.4874 0.056 Uiso 1 1 calc R . . H17B H 0.0708 0.4310 0.5057 0.056 Uiso 1 1 calc R . . H17C H 0.0127 0.3595 0.5334 0.056 Uiso 1 1 calc R . . C21 C 0.68971(10) 0.25990(6) 0.67641(5) 0.0180(2) Uani 1 1 d . . . C22 C 0.69251(10) 0.27583(6) 0.61572(5) 0.0192(2) Uani 1 1 d . B . C23 C 0.78671(10) 0.25001(6) 0.58229(5) 0.0224(2) Uani 1 1 d . . . H23A H 0.7863 0.2595 0.5423 0.027 Uiso 1 1 calc R B . C24 C 0.88131(10) 0.21077(6) 0.60585(5) 0.0236(2) Uani 1 1 d . B . C25 C 0.88053(10) 0.19869(6) 0.66596(5) 0.0242(3) Uani 1 1 d . . . H25A H 0.9438 0.1745 0.6834 0.029 Uiso 1 1 calc R B . C26 C 0.78711(10) 0.22206(6) 0.70037(5) 0.0217(2) Uani 1 1 d . B . H26A H 0.7888 0.2125 0.7403 0.026 Uiso 1 1 calc R . . C27 C 0.98040(11) 0.18282(8) 0.56765(6) 0.0318(3) Uani 1 1 d . . . H27A H 0.9543 0.1802 0.5278 0.048 Uiso 1 1 calc R B . H27B H 1.0042 0.1337 0.5804 0.048 Uiso 1 1 calc R . . H27C H 1.0456 0.2168 0.5704 0.048 Uiso 1 1 calc R . . C31 C 0.46082(11) 0.13119(7) 0.65304(6) 0.0293(3) Uani 1 1 d . . . H31A H 0.4732 0.1102 0.6917 0.035 Uiso 1 1 calc R A 1 H31B H 0.5363 0.1453 0.6368 0.035 Uiso 1 1 calc R A 1 C32 C 0.40034(11) 0.07392(7) 0.61371(6) 0.0272(3) Uani 0.688(9) 1 d P B 1 H32A H 0.3581 0.0368 0.6366 0.033 Uiso 0.688(9) 1 calc PR B 1 H32B H 0.4566 0.0484 0.5888 0.033 Uiso 0.688(9) 1 calc PR B 1 C33 C 0.3158(4) 0.1222(2) 0.57766(17) 0.0326(7) Uani 0.688(9) 1 d P B 1 H33A H 0.3545 0.1438 0.5438 0.039 Uiso 0.688(9) 1 calc PR B 1 H33B H 0.2482 0.0934 0.5650 0.039 Uiso 0.688(9) 1 calc PR B 1 C34 C 0.2812(3) 0.18292(19) 0.62165(19) 0.0357(8) Uani 0.688(9) 1 d P B 1 H34A H 0.2576 0.2286 0.6017 0.043 Uiso 0.688(9) 1 calc PR B 1 H34B H 0.2169 0.1658 0.6460 0.043 Uiso 0.688(9) 1 calc PR B 1 O31 O 0.38465(7) 0.19579(5) 0.65620(4) 0.0269(2) Uani 0.688(9) 1 d P B 1 C321 C 0.40034(11) 0.07392(7) 0.61371(6) 0.0272(3) Uani 0.312(9) 1 d P B 2 H32C H 0.4469 0.0638 0.5791 0.033 Uiso 0.312(9) 1 calc PR B 2 H32D H 0.3867 0.0270 0.6343 0.033 Uiso 0.312(9) 1 calc PR B 2 C341 C 0.3240(9) 0.1938(3) 0.5992(3) 0.0353(18) Uani 0.312(9) 1 d P B 2 H34C H 0.3768 0.2056 0.5673 0.042 Uiso 0.312(9) 1 calc PR B 2 H34D H 0.2575 0.2278 0.5983 0.042 Uiso 0.312(9) 1 calc PR B 2 C331 C 0.2855(9) 0.1116(5) 0.5978(5) 0.040(2) Uani 0.312(9) 1 d P B 2 H33C H 0.2248 0.1014 0.6264 0.048 Uiso 0.312(9) 1 calc PR B 2 H33D H 0.2584 0.0967 0.5594 0.048 Uiso 0.312(9) 1 calc PR B 2 O311 O 0.38465(7) 0.19579(5) 0.65620(4) 0.0269(2) Uani 0.312(9) 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.0252(10) 0.0225(9) 0.0193(10) 0.0020(7) -0.0006(8) 0.0000(8) Li2 0.0226(10) 0.0240(9) 0.0196(10) -0.0010(7) 0.0013(8) 0.0010(8) O11 0.0222(4) 0.0254(4) 0.0143(4) 0.0006(3) -0.0025(3) 0.0037(3) O21 0.0198(4) 0.0216(4) 0.0162(4) -0.0003(3) 0.0025(3) 0.0016(3) N1 0.0208(5) 0.0214(5) 0.0189(5) 0.0031(4) 0.0004(4) -0.0007(4) N2 0.0269(5) 0.0257(5) 0.0235(5) 0.0057(4) -0.0046(4) -0.0062(4) C1 0.0292(6) 0.0252(6) 0.0187(6) 0.0071(4) -0.0033(5) 0.0018(5) C2 0.0243(6) 0.0247(5) 0.0151(5) 0.0000(4) -0.0005(4) -0.0011(5) C3 0.0266(6) 0.0266(6) 0.0215(6) 0.0066(4) 0.0035(5) -0.0040(5) C4 0.0282(6) 0.0238(5) 0.0243(6) 0.0072(5) -0.0010(5) -0.0050(5) C5 0.0548(9) 0.0291(6) 0.0275(7) 0.0033(5) -0.0097(6) -0.0155(6) C6 0.0237(6) 0.0422(8) 0.0452(8) 0.0189(6) -0.0048(6) -0.0072(6) C11 0.0234(6) 0.0171(5) 0.0176(5) -0.0014(4) -0.0026(4) 0.0054(4) C12 0.0251(6) 0.0188(5) 0.0182(6) 0.0013(4) -0.0025(4) 0.0046(4) C13 0.0317(6) 0.0232(5) 0.0186(6) 0.0003(4) -0.0049(5) 0.0071(5) C14 0.0276(6) 0.0222(5) 0.0284(7) -0.0052(5) -0.0092(5) 0.0078(5) C15 0.0215(6) 0.0207(5) 0.0346(7) -0.0040(5) -0.0026(5) 0.0039(5) C16 0.0243(6) 0.0209(5) 0.0224(6) -0.0008(4) 0.0008(5) 0.0048(4) C17 0.0351(7) 0.0388(7) 0.0372(8) -0.0058(6) -0.0161(6) 0.0080(6) C21 0.0193(5) 0.0162(5) 0.0183(5) -0.0021(4) 0.0014(4) -0.0020(4) C22 0.0207(5) 0.0193(5) 0.0175(5) -0.0023(4) -0.0006(4) -0.0020(4) C23 0.0256(6) 0.0238(5) 0.0178(6) -0.0028(4) 0.0030(4) -0.0043(5) C24 0.0220(6) 0.0225(5) 0.0263(6) -0.0055(4) 0.0053(5) -0.0027(4) C25 0.0200(6) 0.0234(6) 0.0290(6) -0.0011(5) -0.0012(5) 0.0031(4) C26 0.0241(6) 0.0218(5) 0.0192(6) 0.0005(4) -0.0010(4) 0.0005(5) C27 0.0265(7) 0.0336(7) 0.0354(7) -0.0074(5) 0.0090(6) 0.0013(5) C31 0.0283(6) 0.0226(6) 0.0371(7) -0.0029(5) -0.0063(5) 0.0058(5) C32 0.0329(7) 0.0215(5) 0.0271(7) -0.0035(5) 0.0035(5) -0.0001(5) C33 0.0329(17) 0.0374(15) 0.0277(18) -0.0111(12) -0.0050(11) 0.0070(12) C34 0.0274(13) 0.0403(14) 0.0395(18) -0.0198(12) -0.0116(11) 0.0091(11) O31 0.0262(4) 0.0248(4) 0.0296(5) -0.0092(3) -0.0096(4) 0.0066(3) C321 0.0329(7) 0.0215(5) 0.0271(7) -0.0035(5) 0.0035(5) -0.0001(5) C341 0.045(4) 0.029(2) 0.031(3) -0.003(2) -0.020(3) 0.008(2) C331 0.045(5) 0.031(3) 0.044(5) -0.016(3) -0.021(3) 0.006(3) O311 0.0262(4) 0.0248(4) 0.0296(5) -0.0092(3) -0.0096(4) 0.0066(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O11 C11 1.324(2) . yes O11 Li1 1.967(2) . yes O11 Li2 2.059(2) . yes O11 Li1 2.024(2) 4_656 yes O21 C21 1.330(2) . yes O21 Li1 2.034(2) . yes O21 Li2 1.931(2) . yes O21 Li2 1.926(2) 4_656 yes O31 C31 1.441(2) . yes O31 C34 1.438(4) . yes O31 Li2 1.994(2) . yes O311 Li2 1.994(2) . yes O311 C341 1.477(8) . yes O311 C31 1.441(2) . yes N1 Li1 2.257(2) . yes N1 C2 1.483(2) . yes N1 C3 1.474(2) . yes N1 C1 1.482(2) . yes N2 C4 1.472(2) . yes N2 C5 1.467(2) . yes N2 C6 1.473(2) . yes N2 Li1 2.325(2) . yes C1 C12 1.504(2) . no C2 C22 1.510(2) . no C3 C4 1.517(2) . no C11 C12 1.422(2) . no C11 C16 1.412(2) . no C11 Li2 2.458(2) . yes C12 C13 1.395(2) . no C13 C14 1.395(2) . no C14 C17 1.512(2) . no C14 C15 1.389(2) . no C15 C16 1.393(2) . no C21 C22 1.418(2) . no C21 C26 1.409(2) . no C22 C23 1.396(2) . no C23 C24 1.393(2) . no C24 C25 1.393(2) . no C24 C27 1.512(2) . no C25 C26 1.388(2) . no C31 C32 1.524(2) . no C31 C321 1.524(2) . no C32 C33 1.532(4) . no C33 C34 1.528(5) . no C1 H1B 0.9700 . no C1 H1A 0.9700 . no C2 H2A 0.9700 . no C2 H2B 0.9700 . no C3 H3B 0.9700 . no C3 H3A 0.9700 . no C4 H4A 0.9700 . no C4 H4B 0.9700 . no C5 H5A 0.9600 . no C5 H5B 0.9600 . no C5 H5C 0.9600 . no C6 H6C 0.9600 . no C6 H6B 0.9600 . no C6 H6A 0.9600 . no C13 H13A 0.9300 . no C15 H15A 0.9300 . no C16 H16A 0.9300 . no C17 H17A 0.9600 . no C17 H17C 0.9600 . no C17 H17B 0.9600 . no C23 H23A 0.9300 . no C25 H25A 0.9300 . no C26 H26A 0.9300 . no C27 H27A 0.9600 . no C27 H27B 0.9600 . no C27 H27C 0.9600 . no C31 H31B 0.9700 . no C31 H31A 0.9700 . no C32 H32A 0.9700 . no C32 H32B 0.9700 . no C33 H33A 0.9700 . no C33 H33B 0.9700 . no C34 H34A 0.9700 . no C34 H34B 0.9700 . no C321 C331 1.515(10) . no C331 C341 1.526(11) . no C321 H32C 0.9700 . no C321 H32D 0.9700 . no C331 H33C 0.9700 . no C331 H33D 0.9700 . no C341 H34C 0.9700 . no C341 H34D 0.9700 . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 O11 Li1 133.71(9) . . yes C11 O11 Li2 90.52(8) . . yes C11 O11 Li1 135.36(9) . 4_656 yes Li1 O11 Li2 85.28(8) . . yes Li1 O11 Li1 90.48(8) . 4_656 yes Li1 O11 Li2 86.85(8) 4_656 . yes C21 O21 Li1 107.78(8) . . yes C21 O21 Li2 139.26(9) . . yes C21 O21 Li2 134.66(9) . 4_656 yes Li1 O21 Li2 86.94(9) . . yes Li1 O21 Li2 90.24(8) . 4_656 yes Li2 O21 Li2 81.11(8) . 4_656 yes C31 O31 C34 109.85(16) . . yes C31 O31 Li2 118.71(9) . . yes C34 O31 Li2 131.35(16) . . yes C31 O311 C341 102.6(3) . . yes C341 O311 Li2 131.5(2) . . yes C31 O311 Li2 118.71(9) . . yes C1 N1 C2 111.95(9) . . yes C1 N1 C3 108.53(9) . . yes C3 N1 Li1 108.00(8) . . yes C1 N1 Li1 109.70(8) . . yes C2 N1 C3 111.35(9) . . yes C2 N1 Li1 107.23(8) . . yes C4 N2 C5 110.06(10) . . yes C4 N2 C6 109.66(10) . . yes C4 N2 Li1 101.84(8) . . yes C6 N2 Li1 117.85(9) . . yes C5 N2 Li1 107.19(9) . . yes C5 N2 C6 109.87(11) . . yes N1 C1 C12 116.98(10) . . yes N1 C2 C22 111.77(9) . . yes N1 C3 C4 110.66(9) . . yes N2 C4 C3 110.60(9) . . yes O11 C11 C12 121.96(10) . . yes O11 C11 C16 121.21(10) . . yes O11 C11 Li2 56.88(7) . . yes C16 C11 Li2 91.80(8) . . yes C12 C11 C16 116.78(10) . . no C12 C11 Li2 120.51(9) . . yes C1 C12 C11 120.79(10) . . no C1 C12 C13 119.61(10) . . no C11 C12 C13 119.46(10) . . no C12 C13 C14 123.31(11) . . no C15 C14 C17 121.69(11) . . no C13 C14 C15 117.08(11) . . no C13 C14 C17 121.23(11) . . no C14 C15 C16 121.15(11) . . no C11 C16 C15 122.09(11) . . no O21 C21 C22 121.49(10) . . yes O21 C21 C26 121.19(10) . . yes C22 C21 C26 117.32(10) . . no C21 C22 C23 119.26(10) . . no C2 C22 C21 120.42(10) . . no C2 C22 C23 120.30(10) . . no C22 C23 C24 123.21(11) . . no C23 C24 C25 117.06(10) . . no C23 C24 C27 121.24(11) . . no C25 C24 C27 121.70(10) . . no C24 C25 C26 121.30(10) . . no C21 C26 C25 121.75(10) . . no O31 C31 C32 106.82(10) . . yes O311 C31 C321 106.82(10) . . yes C31 C32 C33 103.22(17) . . no C32 C33 C34 101.7(3) . . no O31 C34 C33 105.3(3) . . yes N1 C1 H1B 108.00 . . no C12 C1 H1A 108.00 . . no N1 C1 H1A 108.00 . . no C12 C1 H1B 108.00 . . no H1A C1 H1B 107.00 . . no N1 C2 H2B 109.00 . . no C22 C2 H2A 109.00 . . no C22 C2 H2B 109.00 . . no N1 C2 H2A 109.00 . . no H2A C2 H2B 108.00 . . no H3A C3 H3B 108.00 . . no N1 C3 H3A 109.00 . . no C4 C3 H3B 110.00 . . no C4 C3 H3A 110.00 . . no N1 C3 H3B 110.00 . . no N2 C4 H4A 109.00 . . no C3 C4 H4A 110.00 . . no N2 C4 H4B 110.00 . . no C3 C4 H4B 110.00 . . no H4A C4 H4B 108.00 . . no N2 C5 H5B 109.00 . . no N2 C5 H5C 109.00 . . no H5A C5 H5B 109.00 . . no N2 C5 H5A 110.00 . . no H5A C5 H5C 109.00 . . no H5B C5 H5C 110.00 . . no H6A C6 H6B 109.00 . . no H6A C6 H6C 109.00 . . no H6B C6 H6C 110.00 . . no N2 C6 H6B 109.00 . . no N2 C6 H6C 110.00 . . no N2 C6 H6A 109.00 . . no C12 C13 H13A 118.00 . . no C14 C13 H13A 118.00 . . no C16 C15 H15A 119.00 . . no C14 C15 H15A 119.00 . . no C15 C16 H16A 119.00 . . no C11 C16 H16A 119.00 . . no C14 C17 H17B 110.00 . . no C14 C17 H17A 109.00 . . no H17A C17 H17B 109.00 . . no C14 C17 H17C 110.00 . . no H17A C17 H17C 110.00 . . no H17B C17 H17C 109.00 . . no C22 C23 H23A 118.00 . . no C24 C23 H23A 118.00 . . no C26 C25 H25A 119.00 . . no C24 C25 H25A 119.00 . . no C21 C26 H26A 119.00 . . no C25 C26 H26A 119.00 . . no H27B C27 H27C 109.00 . . no H27A C27 H27B 109.00 . . no H27A C27 H27C 109.00 . . no C24 C27 H27B 110.00 . . no C24 C27 H27C 109.00 . . no C24 C27 H27A 110.00 . . no H31A C31 H31B 109.00 . . no C321 C31 H31A 110.00 . . no O31 C31 H31A 110.00 . . no O311 C31 H31A 110.00 . . no C321 C31 H31B 110.00 . . no O311 C31 H31B 110.00 . . no O31 C31 H31B 110.00 . . no C32 C31 H31A 110.00 . . no C32 C31 H31B 110.00 . . no H32A C32 H32B 109.00 . . no C31 C32 H32B 111.00 . . no C33 C32 H32A 111.00 . . no C31 C32 H32A 111.00 . . no C33 C32 H32B 111.00 . . no C32 C33 H33A 111.00 . . no C32 C33 H33B 111.00 . . no C34 C33 H33A 111.00 . . no C34 C33 H33B 111.00 . . no H33A C33 H33B 109.00 . . no C33 C34 H34A 111.00 . . no H34A C34 H34B 109.00 . . no C33 C34 H34B 111.00 . . no O31 C34 H34B 111.00 . . no O31 C34 H34A 111.00 . . no C31 C321 C331 103.8(4) . . no C321 C331 C341 99.8(7) . . no O311 C341 C331 100.1(6) . . yes C31 C321 H32C 111.00 . . no C31 C321 H32D 111.00 . . no C331 C321 H32C 111.00 . . no C331 C321 H32D 111.00 . . no H32C C321 H32D 109.00 . . no C321 C331 H33C 112.00 . . no C321 C331 H33D 112.00 . . no C341 C331 H33C 112.00 . . no H33C C331 H33D 110.00 . . no C341 C331 H33D 112.00 . . no O311 C341 H34C 112.00 . . no H34C C341 H34D 110.00 . . no C331 C341 H34D 112.00 . . no O311 C341 H34D 112.00 . . no C331 C341 H34C 112.00 . . no O11 Li1 N1 88.34(8) . . yes O11 Li1 N1 176.07(11) 4_656 . yes O11 Li1 N2 141.52(10) . . yes O11 Li1 O11 89.49(8) . 4_656 yes O21 Li1 N1 93.38(8) . . yes O21 Li1 N2 123.10(10) . . yes O11 Li1 O21 90.02(8) 4_656 . yes N1 Li1 N2 79.43(7) . . yes O11 Li1 O21 93.71(9) . . yes O11 Li1 N2 100.34(8) 4_656 . yes O21 Li2 C11 114.96(9) . . yes O21 Li2 O21 98.89(9) . 4_656 yes O31 Li2 C11 104.17(8) . . yes O21 Li2 O31 121.93(10) 4_656 . yes O311 Li2 C11 104.17(8) . . yes O21 Li2 C11 111.45(9) 4_656 . yes O21 Li2 O311 121.93(10) 4_656 . yes O21 Li2 O311 105.79(9) . . yes O11 Li2 O21 94.04(9) . . yes O11 Li2 O31 136.05(10) . . yes O11 Li2 C11 32.60(4) . . yes O11 Li2 O311 136.05(10) . . yes O11 Li2 O21 92.08(8) . 4_656 yes O21 Li2 O31 105.79(9) . . yes 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 Li1 O11 C11 C12 -23.94(17) . . . . no Li1 O11 C11 C16 153.40(11) . . . . no Li1 O11 C11 Li2 83.97(12) . . . . no Li2 O11 C11 C12 -107.91(11) . . . . no Li2 O11 C11 C16 69.43(11) . . . . no Li1 O11 C11 C12 166.05(11) 4_656 . . . no Li1 O11 C11 C16 -16.61(17) 4_656 . . . no Li1 O11 C11 Li2 -86.04(12) 4_656 . . . no Li2 O11 Li1 N1 94.61(8) . . . . no Li1 O11 Li1 N1 -178.59(8) 4_656 . . . no C11 O11 Li1 N2 79.06(19) . . . . no Li2 O11 Li1 N2 165.26(16) . . . . no Li1 O11 Li1 N2 -107.94(16) 4_656 . . . no C11 O11 Li1 O11 -174.86(9) . . . 4_656 no Li2 O11 Li1 O11 -88.66(8) . . . 4_656 no Li1 O11 Li1 O11 -1.86(8) 4_656 . . 4_656 no Li1 O11 Li2 O31 -119.18(15) . . . . no Li1 O11 Li2 O31 150.07(15) 4_656 . . . no C11 O11 Li1 O11 174.71(9) 4_656 4_656 . . no Li1 O11 Li1 O11 1.92(9) 4_656 4_656 . . no Li2 O11 Li1 O11 87.16(8) 4_656 4_656 . . no C11 O11 Li1 O21 81.00(13) 4_656 4_656 . . no Li1 O11 Li1 O21 -91.80(8) 4_656 4_656 . . no Li2 O11 Li1 O21 -6.55(8) 4_656 4_656 . . no C11 O11 Li1 N2 -42.72(14) 4_656 4_656 . . no Li1 O11 Li1 N2 144.49(9) 4_656 4_656 . . no Li2 O11 Li1 N2 -130.27(9) 4_656 4_656 . . no C11 O11 Li2 O21 132.44(8) . . . . no Li1 O11 Li2 O21 -1.40(8) . . . . no Li1 O11 Li2 O21 -92.15(9) 4_656 . . . no C11 O11 Li2 O31 14.66(16) . . . . no Li1 O11 Li1 O21 88.12(8) 4_656 . . . no C11 O11 Li1 N1 8.41(14) . . . . no Li1 O11 Li2 C11 -133.84(9) . . . . no Li1 O11 Li2 C11 135.41(9) 4_656 . . . no C11 O11 Li2 O21 -128.49(9) . . . 4_656 no C11 O11 Li1 O21 -84.87(12) . . . . no Li2 O11 Li1 O21 1.33(8) . . . . no Li1 O11 Li2 O21 97.67(9) . . . 4_656 no Li1 O11 Li2 O21 6.92(9) 4_656 . . 4_656 no Li2 O21 Li2 O21 -0.68(9) 4_656 . . 4_656 no Li2 O21 Li2 O21 0.67(9) 4_656 4_656 . . no C21 O21 Li2 O31 -41.82(18) 4_656 4_656 . . no Li1 O21 Li2 O31 -157.50(12) 4_656 4_656 . . no Li2 O21 Li2 O31 115.63(13) 4_656 4_656 . . no C21 O21 Li2 C11 81.87(14) 4_656 4_656 . . no Li2 O21 Li1 O11 -1.41(8) . . . . no Li1 O21 Li2 O21 87.54(9) 4_656 4_656 . . no C21 O21 Li1 O11 139.82(8) . . . . no Li2 O21 Li1 O11 -82.49(9) 4_656 . . . no C21 O21 Li1 N1 51.26(10) . . . . no Li2 O21 Li1 N1 -89.97(8) . . . . no Li2 O21 Li1 N1 -171.05(8) 4_656 . . . no Li1 O21 Li2 C11 -33.82(10) 4_656 4_656 . . no Li2 O21 Li2 C11 -120.68(10) 4_656 4_656 . . no Li2 O21 Li1 N2 109.37(11) 4_656 . . . no C21 O21 Li1 O11 -130.70(8) . . . 4_656 no Li2 O21 Li1 O11 88.07(8) . . . 4_656 no Li2 O21 Li1 O11 6.99(9) 4_656 . . 4_656 no Li2 O21 C21 C26 -136.90(13) . . . . no Li2 O21 C21 C22 -171.26(11) 4_656 . . . no Li2 O21 C21 C26 7.61(18) 4_656 . . . no C21 O21 Li2 O21 154.62(10) . . . 4_656 no Li1 O21 Li2 O21 -91.39(9) . . . 4_656 no Li2 O21 Li2 C11 118.08(10) 4_656 . . . no Li1 O21 C21 C26 116.46(11) . . . . no Li2 O21 C21 C22 44.23(18) . . . . no C21 O21 Li2 O11 108.81(12) 4_656 4_656 . . no C21 O21 Li1 N2 -28.32(13) . . . . no Li2 O21 Li1 N2 -169.55(11) . . . . no C21 O21 Li2 O21 -156.78(10) 4_656 4_656 . . no Li1 O21 C21 C22 -62.41(12) . . . . no C21 O21 Li2 O11 -112.64(12) . . . . no Li1 O21 Li2 O11 1.35(8) . . . . no C21 O21 Li2 O31 27.71(17) . . . . no Li1 O21 Li2 O31 141.70(10) . . . . no Li2 O21 Li2 O31 -127.58(10) 4_656 . . . no C21 O21 Li2 C11 -86.63(15) . . . . no Li1 O21 Li2 C11 27.36(10) . . . . no Li2 O21 Li2 O11 -93.74(9) 4_656 4_656 . . no Li2 O21 Li2 O11 92.07(9) 4_656 . . . no Li1 O21 Li2 O11 -6.88(8) 4_656 4_656 . . no C34 O31 Li2 O11 -41.1(3) . . . . no Li2 O31 C34 C33 161.50(19) . . . . no C34 O31 Li2 O21 -154.6(2) . . . . no C31 O31 Li2 O21 29.27(13) . . . . no C34 O31 C31 C32 -0.1(2) . . . . no C31 O31 Li2 O21 -82.17(14) . . . 4_656 no Li2 O31 C31 C32 176.85(10) . . . . no C31 O31 Li2 C11 150.84(9) . . . . no C31 O31 C34 C33 -22.1(3) . . . . no C31 O31 Li2 O11 142.76(14) . . . . no C34 O31 Li2 O21 94.0(3) . . . 4_656 no C34 O31 Li2 C11 -33.0(2) . . . . no C1 N1 Li1 N2 -112.28(8) . . . . no C1 N1 Li1 O11 31.05(10) . . . . no C2 N1 Li1 N2 125.94(8) . . . . no C2 N1 Li1 O11 -90.74(9) . . . . no C3 N1 Li1 O11 149.17(8) . . . . no C1 N1 Li1 O21 124.67(9) . . . . no C2 N1 Li1 O21 2.89(10) . . . . no C3 N1 Li1 O21 -117.21(9) . . . . no Li1 N1 C1 C12 -61.51(12) . . . . no C2 N1 C3 C4 -152.77(9) . . . . no Li1 N1 C3 C4 -35.30(12) . . . . no C1 N1 C3 C4 83.57(11) . . . . no C3 N1 Li1 N2 5.84(9) . . . . no C2 N1 C1 C12 57.41(12) . . . . no C3 N1 C1 C12 -179.29(9) . . . . no Li1 N1 C2 C22 -52.53(11) . . . . no C1 N1 C2 C22 -172.90(9) . . . . no C3 N1 C2 C22 65.41(12) . . . . no C6 N2 C4 C3 74.19(13) . . . . no C5 N2 C4 C3 -164.83(11) . . . . no Li1 N2 C4 C3 -51.38(11) . . . . no C5 N2 Li1 N1 139.55(9) . . . . no C6 N2 Li1 O11 87.99(11) . . . 4_656 no C4 N2 Li1 O11 -152.04(9) . . . 4_656 no C5 N2 Li1 O11 -36.47(11) . . . 4_656 no C6 N2 Li1 O11 -169.61(14) . . . . no C4 N2 Li1 O21 111.11(11) . . . . no C6 N2 Li1 O21 -8.86(15) . . . . no C4 N2 Li1 N1 23.97(8) . . . . no C6 N2 Li1 N1 -96.00(10) . . . . no C4 N2 Li1 O11 -49.64(17) . . . . no C5 N2 Li1 O11 65.93(17) . . . . no C5 N2 Li1 O21 -133.32(11) . . . . no N1 C1 C12 C11 51.72(14) . . . . no N1 C1 C12 C13 -132.66(11) . . . . no N1 C2 C22 C23 -112.75(11) . . . . no N1 C2 C22 C21 65.78(13) . . . . no N1 C3 C4 N2 62.51(13) . . . . no O11 C11 Li2 O21 57.19(9) . . . 4_656 no O11 C11 C12 C1 -3.82(16) . . . . no C12 C11 Li2 O31 -59.13(13) . . . . no C16 C11 Li2 O31 63.68(10) . . . . no C12 C11 Li2 O11 110.44(12) . . . . no C16 C11 Li2 O11 -126.76(10) . . . . no O11 C11 Li2 O21 -54.29(10) . . . . no C12 C11 Li2 O21 56.15(14) . . . . no C16 C11 Li2 O21 178.95(10) . . . . no O11 C11 Li2 O31 -169.56(11) . . . . no C16 C11 C12 C1 178.73(10) . . . . no C16 C11 C12 C13 3.10(15) . . . . no Li2 C11 C12 C1 -71.50(13) . . . . no Li2 C11 C12 C13 112.87(11) . . . . no C12 C11 Li2 O21 167.62(10) . . . 4_656 no C16 C11 Li2 O21 -69.58(11) . . . 4_656 no O11 C11 C12 C13 -179.45(10) . . . . no Li2 C11 C16 C15 -129.65(11) . . . . no O11 C11 C16 C15 178.67(10) . . . . no C12 C11 C16 C15 -3.86(16) . . . . no C11 C12 C13 C14 -0.07(17) . . . . no C1 C12 C13 C14 -175.75(10) . . . . no C12 C13 C14 C17 176.88(11) . . . . no C12 C13 C14 C15 -2.34(16) . . . . no C17 C14 C15 C16 -177.60(11) . . . . no C13 C14 C15 C16 1.62(16) . . . . no C14 C15 C16 C11 1.51(17) . . . . no O21 C21 C22 C2 3.98(16) . . . . no C26 C21 C22 C23 3.61(16) . . . . no O21 C21 C22 C23 -177.48(10) . . . . no C26 C21 C22 C2 -174.93(10) . . . . no O21 C21 C26 C25 178.82(10) . . . . no C22 C21 C26 C25 -2.27(16) . . . . no C21 C22 C23 C24 -1.98(17) . . . . no C2 C22 C23 C24 176.56(10) . . . . no C22 C23 C24 C25 -1.17(16) . . . . no C22 C23 C24 C27 178.98(11) . . . . no C23 C24 C25 C26 2.60(16) . . . . no C27 C24 C25 C26 -177.55(11) . . . . no C24 C25 C26 C21 -0.90(17) . . . . no O31 C31 C32 C33 21.9(2) . . . . no C31 C32 C33 C34 -33.9(3) . . . . no C32 C33 C34 O31 34.7(3) . . . . no _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.299 _refine_diff_density_min -0.203 _refine_diff_density_rms 0.039 data_2b(C56H84Cl2Li6N4O8,C4H8O) _database_code_depnum_ccdc_archive 'CCDC 832241' #TrackingRef '- MS_Janas.cif' # CCDC 832241 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H84 Cl2 Li6 N4 O8, C4 H8 O ' _chemical_formula_sum 'C60 H92 Cl2 Li6 N4 O9 ' _chemical_formula_weight 1125.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.417(8) _cell_length_b 12.217(4) _cell_length_c 23.689(8) _cell_angle_alpha 90.00 _cell_angle_beta 109.91(5) _cell_angle_gamma 90.00 _cell_volume 6372(4) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 14556 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 0.156 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; 'Oxford Xcalibur PX \k-geometry diffractometer with CCD area detector' ; _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29932 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 29.95 _reflns_number_total 8667 _reflns_number_gt 5427 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisCCD (Oxford Diffraction, 2009)' _computing_cell_refinement 'CrysAlisRED (Oxford Diffraction, 2009)' _computing_data_reduction CrysAlisRED _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0780P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8667 _refine_ls_number_parameters 410 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0865 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1435 _refine_ls_wR_factor_gt 0.1333 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.73095(13) 0.7280(2) 0.39887(14) 0.0280(6) Uani 1 1 d . . . Li2 Li 0.80702(13) 0.6127(2) 0.48470(13) 0.0267(6) Uani 1 1 d . . . Li3 Li 0.66586(13) 0.6533(2) 0.47922(14) 0.0267(6) Uani 1 1 d . . . Cl1 Cl 0.840476(19) 0.65597(4) 0.58513(2) 0.02903(12) Uani 1 1 d . . . O11 O 0.72127(5) 0.59405(9) 0.43856(5) 0.0237(3) Uani 1 1 d . A . O21 O 0.68333(5) 0.74980(9) 0.55218(5) 0.0240(3) Uani 1 1 d . . . N1 N 0.66422(6) 0.50558(11) 0.52858(6) 0.0229(3) Uani 1 1 d . . . N2 N 0.57126(6) 0.60521(12) 0.42790(7) 0.0276(3) Uani 1 1 d . . . C1 C 0.70877(8) 0.42812(14) 0.51815(8) 0.0245(4) Uani 1 1 d . A . H1A H 0.7069 0.3579 0.5383 0.029 Uiso 1 1 calc R . . H1B H 0.7502 0.4583 0.5370 0.029 Uiso 1 1 calc R . . C2 C 0.68382(8) 0.53072(14) 0.59343(8) 0.0254(4) Uani 1 1 d . A . H2A H 0.7271 0.5528 0.6074 0.030 Uiso 1 1 calc R . . H2B H 0.6805 0.4636 0.6155 0.030 Uiso 1 1 calc R . . C3 C 0.60126(8) 0.46165(14) 0.50680(8) 0.0273(4) Uani 1 1 d . A . H3A H 0.5787 0.4922 0.5317 0.033 Uiso 1 1 calc R . . H3B H 0.6028 0.3812 0.5120 0.033 Uiso 1 1 calc R . . C4 C 0.56703(8) 0.48837(15) 0.44134(8) 0.0289(4) Uani 1 1 d . A . H4A H 0.5838 0.4440 0.4156 0.035 Uiso 1 1 calc R . . H4B H 0.5238 0.4683 0.4315 0.035 Uiso 1 1 calc R . . C5 C 0.53192(8) 0.67191(16) 0.45099(10) 0.0361(5) Uani 1 1 d . A . H5A H 0.5360 0.7492 0.4420 0.054 Uiso 1 1 calc R . . H5B H 0.5439 0.6621 0.4945 0.054 Uiso 1 1 calc R . . H5C H 0.4896 0.6490 0.4319 0.054 Uiso 1 1 calc R . . C6 C 0.55320(9) 0.62181(17) 0.36283(9) 0.0373(5) Uani 1 1 d . A . H6A H 0.5106 0.6005 0.3437 0.056 Uiso 1 1 calc R . . H6B H 0.5788 0.5768 0.3468 0.056 Uiso 1 1 calc R . . H6C H 0.5581 0.6991 0.3545 0.056 Uiso 1 1 calc R . . C11 C 0.70424(7) 0.49385(14) 0.41595(8) 0.0233(4) Uani 1 1 d . . . C12 C 0.69841(7) 0.40604(14) 0.45288(8) 0.0237(4) Uani 1 1 d . A . C13 C 0.68273(7) 0.30206(14) 0.42836(8) 0.0266(4) Uani 1 1 d . . . H13 H 0.6797 0.2442 0.4540 0.032 Uiso 1 1 calc R A . C14 C 0.67127(8) 0.27906(15) 0.36762(9) 0.0302(4) Uani 1 1 d . A . C15 C 0.67543(8) 0.36651(16) 0.33141(8) 0.0306(4) Uani 1 1 d . . . H15 H 0.6669 0.3544 0.2897 0.037 Uiso 1 1 calc R A . C16 C 0.69171(8) 0.47126(15) 0.35473(8) 0.0272(4) Uani 1 1 d . A . H16 H 0.6944 0.5286 0.3287 0.033 Uiso 1 1 calc R . . C17 C 0.65413(11) 0.16582(17) 0.34200(10) 0.0437(5) Uani 1 1 d . . . H17A H 0.6559 0.1630 0.3013 0.066 Uiso 1 1 calc R A . H17B H 0.6128 0.1487 0.3407 0.066 Uiso 1 1 calc R . . H17C H 0.6825 0.1123 0.3674 0.066 Uiso 1 1 calc R . . C21 C 0.64945(7) 0.72737(14) 0.58638(8) 0.0236(4) Uani 1 1 d . . . C22 C 0.64699(8) 0.62073(14) 0.60848(8) 0.0239(4) Uani 1 1 d . . . C23 C 0.61150(8) 0.60072(15) 0.64471(8) 0.0279(4) Uani 1 1 d . A . H23 H 0.6105 0.5287 0.6594 0.034 Uiso 1 1 calc R . . C24 C 0.57772(8) 0.68227(16) 0.65993(8) 0.0297(4) Uani 1 1 d . . . C25 C 0.58032(8) 0.78720(16) 0.63777(9) 0.0323(4) Uani 1 1 d . A . H25 H 0.5578 0.8445 0.6473 0.039 Uiso 1 1 calc R . . C26 C 0.61518(8) 0.80978(15) 0.60196(8) 0.0290(4) Uani 1 1 d . . . H26 H 0.6160 0.8822 0.5877 0.035 Uiso 1 1 calc R A . C27 C 0.53878(9) 0.65832(18) 0.69849(9) 0.0384(5) Uani 1 1 d . A . H27A H 0.4957 0.6633 0.6738 0.058 Uiso 1 1 calc R . . H27B H 0.5478 0.7118 0.7312 0.058 Uiso 1 1 calc R . . H27C H 0.5477 0.5845 0.7153 0.058 Uiso 1 1 calc R . . O31 O 0.85545(5) 0.47857(10) 0.48521(6) 0.0294(3) Uani 1 1 d D . . C31 C 0.84672(8) 0.40292(15) 0.43619(8) 0.0290(4) Uani 1 1 d D A . H31A H 0.8280 0.4403 0.3972 0.035 Uiso 1 1 calc R . . H31B H 0.8201 0.3416 0.4389 0.035 Uiso 1 1 calc R . . C32 C 0.90990(8) 0.36120(16) 0.44244(9) 0.0341(4) Uani 1 1 d D . . H32A H 0.9303 0.4102 0.4219 0.041 Uiso 1 1 calc R A . H32B H 0.9083 0.2862 0.4262 0.041 Uiso 1 1 calc R . . C33 C 0.94180(8) 0.36314(16) 0.51040(9) 0.0345(4) Uani 1 1 d D A . H33A H 0.9319 0.2972 0.5295 0.041 Uiso 1 1 calc R . . H33B H 0.9864 0.3683 0.5210 0.041 Uiso 1 1 calc R . . C34 C 0.91613(8) 0.46538(16) 0.52876(9) 0.0323(4) Uani 1 1 d D A . H34A H 0.9144 0.4572 0.5697 0.039 Uiso 1 1 calc R . . H34B H 0.9416 0.5297 0.5282 0.039 Uiso 1 1 calc R . . O41 O 0.7185(2) 0.7530(6) 0.3115(2) 0.0365(11) Uani 0.754(5) 1 d PD A 1 C41 C 0.7460(2) 0.7072(4) 0.2711(2) 0.0406(11) Uani 0.754(5) 1 d PD A 1 H41A H 0.7494 0.6267 0.2753 0.049 Uiso 0.754(5) 1 calc PR A 1 H41B H 0.7869 0.7385 0.2784 0.049 Uiso 0.754(5) 1 calc PR A 1 C42 C 0.70221(17) 0.7398(5) 0.20926(15) 0.0578(12) Uani 0.754(5) 1 d PD A 1 H42A H 0.7244 0.7515 0.1809 0.069 Uiso 0.754(5) 1 calc PR A 1 H42B H 0.6711 0.6824 0.1929 0.069 Uiso 0.754(5) 1 calc PR A 1 C43 C 0.6749(2) 0.8385(5) 0.21867(16) 0.0893(18) Uani 0.754(5) 1 d PD A 1 H43A H 0.6943 0.9023 0.2067 0.107 Uiso 0.754(5) 1 calc PR A 1 H43B H 0.6310 0.8389 0.1947 0.107 Uiso 0.754(5) 1 calc PR A 1 C44 C 0.6835(3) 0.8430(4) 0.28070(16) 0.098(2) Uani 0.754(5) 1 d PD A 1 H44A H 0.6435 0.8424 0.2863 0.117 Uiso 0.754(5) 1 calc PR A 1 H44B H 0.7044 0.9121 0.2978 0.117 Uiso 0.754(5) 1 calc PR A 1 O411 O 0.7106(7) 0.730(2) 0.3124(7) 0.050(6) Uani 0.246(5) 1 d PD A 2 C411 C 0.7534(8) 0.717(2) 0.2811(9) 0.101(10) Uani 0.246(5) 1 d PD A 2 H41C H 0.7823 0.6562 0.2980 0.122 Uiso 0.246(5) 1 calc PR A 2 H41D H 0.7761 0.7850 0.2813 0.122 Uiso 0.246(5) 1 calc PR A 2 C421 C 0.7107(7) 0.6899(13) 0.2199(7) 0.069(5) Uiso 0.246(5) 1 d PD A 2 H42C H 0.7036 0.6099 0.2157 0.083 Uiso 0.246(5) 1 calc PR A 2 H42D H 0.7275 0.7145 0.1889 0.083 Uiso 0.246(5) 1 calc PR A 2 C431 C 0.6498(6) 0.7516(14) 0.2126(5) 0.084(4) Uiso 0.246(5) 1 d PD A 2 H43C H 0.6505 0.8275 0.1982 0.101 Uiso 0.246(5) 1 calc PR A 2 H43D H 0.6143 0.7125 0.1847 0.101 Uiso 0.246(5) 1 calc PR A 2 C441 C 0.6492(5) 0.7496(10) 0.2735(4) 0.056(3) Uiso 0.246(5) 1 d PD A 2 H44C H 0.6346 0.8205 0.2835 0.067 Uiso 0.246(5) 1 calc PR A 2 H44D H 0.6220 0.6909 0.2781 0.067 Uiso 0.246(5) 1 calc PR A 2 O51 O 0.5051(12) 1.1544(6) 0.7513(9) 0.201(4) Uani 0.50 1 d P B -3 C51 C 0.4997(3) 1.0752(4) 0.69980(18) 0.1203(16) Uani 1 1 d . B -3 H51A H 0.4660 1.0994 0.6635 0.144 Uiso 0.256(16) 1 d PR C -3 H51B H 0.5376 1.0767 0.6899 0.144 Uiso 0.256(16) 1 d PR C -3 H51C H 0.4573 1.0748 0.6707 0.144 Uiso 0.744(16) 1 d PR C -3 H51D H 0.5274 1.0959 0.6782 0.144 Uiso 0.744(16) 1 d PR C -3 C53 C 0.4808(10) 0.9817(13) 0.7090(7) 0.066(5) Uiso 0.256(16) 1 d P B -3 H53A H 0.5021 0.9963 0.6801 0.079 Uiso 0.256(16) 1 d PR C -3 H53B H 0.4412 1.0122 0.6835 0.079 Uiso 0.256(16) 1 d PR C -3 C52 C 0.5158(4) 0.9740(4) 0.7275(3) 0.096(2) Uani 0.744(16) 1 d P B -3 H52A H 0.5604 0.9647 0.7452 0.115 Uiso 0.744(16) 1 d PR C -3 H52B H 0.4989 0.9148 0.6980 0.115 Uiso 0.744(16) 1 d PR C -3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.0242(14) 0.0325(16) 0.0313(17) 0.0018(13) 0.0146(13) 0.0014(12) Li2 0.0229(14) 0.0300(15) 0.0303(17) -0.0007(13) 0.0129(13) 0.0007(12) Li3 0.0202(13) 0.0315(16) 0.0310(16) 0.0006(13) 0.0123(12) -0.0002(12) Cl1 0.0262(2) 0.0321(2) 0.0314(3) -0.00096(19) 0.01315(18) 0.00336(17) O11 0.0185(5) 0.0265(6) 0.0293(7) -0.0011(5) 0.0122(5) -0.0005(4) O21 0.0211(5) 0.0273(6) 0.0291(7) 0.0005(5) 0.0155(5) -0.0007(5) N1 0.0194(6) 0.0250(7) 0.0287(8) -0.0019(6) 0.0139(6) 0.0001(5) N2 0.0188(7) 0.0299(8) 0.0358(9) 0.0005(7) 0.0114(6) 0.0012(6) C1 0.0230(8) 0.0238(8) 0.0305(10) 0.0019(7) 0.0144(7) 0.0033(6) C2 0.0253(8) 0.0263(9) 0.0285(10) 0.0034(7) 0.0143(8) 0.0019(7) C3 0.0232(8) 0.0262(9) 0.0383(11) -0.0025(8) 0.0180(8) -0.0041(7) C4 0.0186(8) 0.0320(10) 0.0389(11) -0.0064(8) 0.0135(8) -0.0024(7) C5 0.0222(8) 0.0332(10) 0.0544(13) -0.0028(9) 0.0149(9) 0.0039(7) C6 0.0270(9) 0.0417(11) 0.0407(12) 0.0031(9) 0.0084(9) 0.0001(8) C11 0.0143(7) 0.0285(9) 0.0304(10) -0.0011(7) 0.0118(7) 0.0025(6) C12 0.0157(7) 0.0279(9) 0.0306(10) -0.0013(7) 0.0119(7) 0.0029(6) C13 0.0204(8) 0.0273(9) 0.0351(11) 0.0021(8) 0.0132(8) 0.0030(7) C14 0.0244(8) 0.0305(10) 0.0359(11) -0.0048(8) 0.0107(8) 0.0010(7) C15 0.0255(8) 0.0408(11) 0.0274(10) -0.0049(8) 0.0116(8) 0.0014(8) C16 0.0228(8) 0.0331(10) 0.0288(10) 0.0027(8) 0.0128(7) 0.0015(7) C17 0.0528(13) 0.0347(11) 0.0418(13) -0.0076(9) 0.0140(11) -0.0030(10) C21 0.0186(7) 0.0295(9) 0.0258(9) -0.0030(7) 0.0117(7) -0.0019(6) C22 0.0225(8) 0.0280(9) 0.0248(9) -0.0015(7) 0.0126(7) -0.0015(7) C23 0.0269(8) 0.0318(10) 0.0298(10) -0.0022(8) 0.0157(8) -0.0067(7) C24 0.0213(8) 0.0440(11) 0.0288(10) -0.0053(8) 0.0149(8) -0.0056(7) C25 0.0257(9) 0.0405(11) 0.0370(11) -0.0057(9) 0.0188(8) 0.0027(8) C26 0.0269(8) 0.0290(9) 0.0361(11) 0.0010(8) 0.0172(8) 0.0036(7) C27 0.0305(9) 0.0551(13) 0.0393(12) -0.0085(10) 0.0247(9) -0.0090(9) O31 0.0214(6) 0.0330(7) 0.0331(7) -0.0054(5) 0.0084(5) 0.0056(5) C31 0.0241(8) 0.0316(10) 0.0322(11) -0.0051(8) 0.0109(8) 0.0028(7) C32 0.0272(9) 0.0393(11) 0.0386(11) -0.0029(9) 0.0151(8) 0.0088(8) C33 0.0255(9) 0.0373(11) 0.0393(12) 0.0000(8) 0.0091(8) 0.0080(8) C34 0.0221(8) 0.0360(10) 0.0359(11) -0.0024(8) 0.0061(8) 0.0028(7) O41 0.0438(19) 0.045(2) 0.0270(17) 0.0054(13) 0.0207(14) 0.0003(15) C41 0.051(2) 0.047(2) 0.036(3) -0.0082(19) 0.0303(19) -0.0118(18) C42 0.045(2) 0.104(4) 0.0281(18) -0.012(2) 0.0181(15) -0.019(2) C43 0.096(3) 0.133(5) 0.038(2) 0.018(2) 0.022(2) 0.032(3) C44 0.165(5) 0.085(3) 0.032(2) 0.019(2) 0.020(3) 0.056(3) O411 0.038(5) 0.070(13) 0.057(7) 0.027(6) 0.036(5) 0.012(7) C411 0.077(13) 0.19(2) 0.060(12) -0.077(12) 0.048(10) -0.066(13) O51 0.343(13) 0.129(5) 0.123(5) -0.059(8) 0.068(6) 0.065(12) C51 0.168(5) 0.107(3) 0.071(3) -0.032(3) 0.021(3) -0.012(3) C52 0.088(5) 0.087(3) 0.106(5) 0.001(3) 0.026(4) 0.059(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O11 1.938(3) . ? Li1 O411 1.939(16) . ? Li1 O21 1.965(3) 7_666 ? Li1 O41 2.013(5) . ? Li1 Cl1 2.320(3) 7_666 ? Li1 Li2 2.612(5) . ? Li1 C21 2.756(3) 7_666 ? Li1 Li3 2.959(4) . ? Li1 Li3 3.396(5) 7_666 ? Li2 O21 1.942(3) 7_666 ? Li2 O11 1.945(3) . ? Li2 O31 1.991(3) . ? Li2 Cl1 2.299(3) . ? Li2 Li3 2.989(4) 7_666 ? Li2 Li3 3.301(4) . ? Li3 O11 1.997(3) . ? Li3 O21 2.016(3) . ? Li3 N1 2.158(3) . ? Li3 N2 2.213(3) . ? Li3 Cl1 2.761(3) 7_666 ? Li3 C11 2.787(3) . ? Li3 Li2 2.990(4) 7_666 ? Li3 Li1 3.396(5) 7_666 ? Cl1 Li1 2.320(3) 7_666 ? Cl1 Li3 2.761(3) 7_666 ? O11 C11 1.341(2) . ? O21 C21 1.3412(19) . ? O21 Li2 1.942(3) 7_666 ? O21 Li1 1.965(3) 7_666 ? N1 C2 1.478(2) . ? N1 C3 1.486(2) . ? N1 C1 1.490(2) . ? N2 C6 1.467(3) . ? N2 C5 1.468(2) . ? N2 C4 1.473(2) . ? C1 C12 1.506(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C22 1.513(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.519(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 C16 1.405(3) . ? C11 C12 1.420(2) . ? C12 C13 1.393(2) . ? C13 C14 1.399(3) . ? C13 H13 0.9500 . ? C14 C15 1.394(3) . ? C14 C17 1.509(3) . ? C15 C16 1.395(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C21 C22 1.413(2) . ? C21 C26 1.413(2) . ? C21 Li1 2.756(3) 7_666 ? C22 C23 1.405(2) . ? C23 C24 1.394(2) . ? C23 H23 0.9500 . ? C24 C25 1.394(3) . ? C24 C27 1.523(2) . ? C25 C26 1.390(2) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? O31 C31 1.443(2) . ? O31 C34 1.453(2) . ? C31 C32 1.524(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.527(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.513(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? O41 C44 1.417(7) . ? O41 C41 1.435(5) . ? C41 C42 1.528(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.418(6) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.415(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? O411 C441 1.441(14) . ? O411 C411 1.443(14) . ? C411 C421 1.490(14) . ? C411 H41C 0.9900 . ? C411 H41D 0.9900 . ? C421 C431 1.569(13) . ? C421 H42C 0.9900 . ? C421 H42D 0.9900 . ? C431 C441 1.447(12) . ? C431 H43C 0.9900 . ? C431 H43D 0.9900 . ? C441 H44C 0.9900 . ? C441 H44D 0.9900 . ? O51 C51 1.528(13) . ? C51 C53 1.271(13) . ? C51 C52 1.390(6) . ? C51 H51A 0.9947 . ? C51 H51B 0.9922 . ? C51 H51C 0.9969 . ? C51 H51D 0.9856 . ? C53 H53A 0.9889 . ? C53 H53B 0.9911 . ? C53 H52B 0.9936 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Li1 O411 119.6(7) . . ? O11 Li1 O21 95.46(14) . 7_666 ? O411 Li1 O21 117.1(5) . 7_666 ? O11 Li1 O41 128.8(3) . . ? O411 Li1 O41 9.8(9) . . ? O21 Li1 O41 110.3(2) 7_666 . ? O11 Li1 Cl1 103.10(12) . 7_666 ? O411 Li1 Cl1 103.6(6) . 7_666 ? O21 Li1 Cl1 117.87(15) 7_666 7_666 ? O41 Li1 Cl1 102.4(2) . 7_666 ? O11 Li1 Li2 47.84(10) . . ? O411 Li1 Li2 133.2(6) . . ? O21 Li1 Li2 47.66(10) 7_666 . ? O41 Li1 Li2 134.7(2) . . ? Cl1 Li1 Li2 122.73(14) 7_666 . ? O11 Li1 C21 112.78(14) . 7_666 ? O411 Li1 C21 90.3(5) . 7_666 ? O21 Li1 C21 26.91(6) 7_666 7_666 ? O41 Li1 C21 83.41(19) . 7_666 ? Cl1 Li1 C21 128.04(13) 7_666 7_666 ? Li2 Li1 C21 67.29(11) . 7_666 ? O11 Li1 Li3 41.99(8) . . ? O411 Li1 Li3 133.5(6) . . ? O21 Li1 Li3 108.03(14) 7_666 . ? O41 Li1 Li3 141.5(2) . . ? Cl1 Li1 Li3 61.67(9) 7_666 . ? Li2 Li1 Li3 72.37(11) . . ? C21 Li1 Li3 134.69(14) 7_666 . ? O11 Li1 Li3 96.60(13) . 7_666 ? O411 Li1 Li3 137.9(6) . 7_666 ? O21 Li1 Li3 31.91(8) 7_666 7_666 ? O41 Li1 Li3 128.4(2) . 7_666 ? Cl1 Li1 Li3 86.78(11) 7_666 7_666 ? Li2 Li1 Li3 57.94(11) . 7_666 ? C21 Li1 Li3 53.81(8) 7_666 7_666 ? Li3 Li1 Li3 87.59(11) . 7_666 ? O21 Li2 O11 96.00(14) 7_666 . ? O21 Li2 O31 124.16(15) 7_666 . ? O11 Li2 O31 112.58(16) . . ? O21 Li2 Cl1 102.47(13) 7_666 . ? O11 Li2 Cl1 122.09(14) . . ? O31 Li2 Cl1 100.97(14) . . ? O21 Li2 Li1 48.43(10) 7_666 . ? O11 Li2 Li1 47.62(10) . . ? O31 Li2 Li1 133.20(16) . . ? Cl1 Li2 Li1 125.69(14) . . ? O21 Li2 Li3 41.88(9) 7_666 7_666 ? O11 Li2 Li3 110.54(13) . 7_666 ? O31 Li2 Li3 136.09(15) . 7_666 ? Cl1 Li2 Li3 61.31(9) . 7_666 ? Li1 Li2 Li3 74.29(12) . 7_666 ? O21 Li2 Li3 96.94(12) 7_666 . ? O11 Li2 Li3 33.62(8) . . ? O31 Li2 Li3 133.21(14) . . ? Cl1 Li2 Li3 89.42(11) . . ? Li1 Li2 Li3 58.68(10) . . ? Li3 Li2 Li3 88.86(10) 7_666 . ? O11 Li3 O21 130.55(16) . . ? O11 Li3 N1 95.32(13) . . ? O21 Li3 N1 93.47(13) . . ? O11 Li3 N2 109.41(15) . . ? O21 Li3 N2 119.95(14) . . ? N1 Li3 N2 82.90(12) . . ? O11 Li3 Cl1 87.77(11) . 7_666 ? O21 Li3 Cl1 86.37(11) . 7_666 ? N1 Li3 Cl1 176.04(13) . 7_666 ? N2 Li3 Cl1 93.74(12) . 7_666 ? O11 Li3 C11 26.56(6) . . ? O21 Li3 C11 149.49(15) . . ? N1 Li3 C11 77.02(10) . . ? N2 Li3 C11 87.99(11) . . ? Cl1 Li3 C11 105.04(10) 7_666 . ? O11 Li3 Li1 40.50(9) . . ? O21 Li3 Li1 111.88(13) . . ? N1 Li3 Li1 135.61(14) . . ? N2 Li3 Li1 111.54(14) . . ? Cl1 Li3 Li1 47.71(7) 7_666 . ? C11 Li3 Li1 62.51(9) . . ? O11 Li3 Li2 112.01(13) . 7_666 ? O21 Li3 Li2 40.02(9) . 7_666 ? N1 Li3 Li2 133.33(14) . 7_666 ? N2 Li3 Li2 119.10(13) . 7_666 ? Cl1 Li3 Li2 46.91(8) 7_666 7_666 ? C11 Li3 Li2 138.25(12) . 7_666 ? Li1 Li3 Li2 77.48(10) . 7_666 ? O11 Li3 Li2 32.64(8) . . ? O21 Li3 Li2 98.39(13) . . ? N1 Li3 Li2 93.18(12) . . ? N2 Li3 Li2 141.58(14) . . ? Cl1 Li3 Li2 90.76(9) 7_666 . ? C11 Li3 Li2 54.14(8) . . ? Li1 Li3 Li2 48.95(9) . . ? Li2 Li3 Li2 91.14(11) 7_666 . ? O11 Li3 Li1 100.02(12) . 7_666 ? O21 Li3 Li1 31.02(8) . 7_666 ? N1 Li3 Li1 92.02(12) . 7_666 ? N2 Li3 Li1 150.46(13) . 7_666 ? Cl1 Li3 Li1 89.88(10) 7_666 7_666 ? C11 Li3 Li1 119.31(11) . 7_666 ? Li1 Li3 Li1 92.41(11) . 7_666 ? Li2 Li3 Li1 47.78(9) 7_666 7_666 ? Li2 Li3 Li1 67.52(10) . 7_666 ? Li2 Cl1 Li1 107.40(11) . 7_666 ? Li2 Cl1 Li3 71.78(10) . 7_666 ? Li1 Cl1 Li3 70.62(10) 7_666 7_666 ? C11 O11 Li1 130.13(14) . . ? C11 O11 Li2 116.16(13) . . ? Li1 O11 Li2 84.54(14) . . ? C11 O11 Li3 111.70(12) . . ? Li1 O11 Li3 97.51(13) . . ? Li2 O11 Li3 113.74(14) . . ? C21 O21 Li2 129.20(13) . 7_666 ? C21 O21 Li1 111.55(14) . 7_666 ? Li2 O21 Li1 83.91(13) 7_666 7_666 ? C21 O21 Li3 114.16(13) . . ? Li2 O21 Li3 98.10(13) 7_666 . ? Li1 O21 Li3 117.06(13) 7_666 . ? C2 N1 C3 110.85(13) . . ? C2 N1 C1 108.49(14) . . ? C3 N1 C1 112.39(13) . . ? C2 N1 Li3 109.44(13) . . ? C3 N1 Li3 108.21(13) . . ? C1 N1 Li3 107.37(12) . . ? C6 N2 C5 108.78(15) . . ? C6 N2 C4 110.14(15) . . ? C5 N2 C4 111.14(14) . . ? C6 N2 Li3 114.64(14) . . ? C5 N2 Li3 106.61(14) . . ? C4 N2 Li3 105.47(13) . . ? N1 C1 C12 114.01(14) . . ? N1 C1 H1A 108.8 . . ? C12 C1 H1A 108.8 . . ? N1 C1 H1B 108.8 . . ? C12 C1 H1B 108.8 . . ? H1A C1 H1B 107.6 . . ? N1 C2 C22 113.32(14) . . ? N1 C2 H2A 108.9 . . ? C22 C2 H2A 108.9 . . ? N1 C2 H2B 108.9 . . ? C22 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? N1 C3 C4 113.13(14) . . ? N1 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? N1 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? N2 C4 C3 112.20(15) . . ? N2 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? N2 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O11 C11 C16 121.37(15) . . ? O11 C11 C12 121.42(15) . . ? C16 C11 C12 117.21(16) . . ? O11 C11 Li3 41.73(9) . . ? C16 C11 Li3 134.42(14) . . ? C12 C11 Li3 94.61(12) . . ? C13 C12 C11 119.94(16) . . ? C13 C12 C1 121.26(15) . . ? C11 C12 C1 118.79(15) . . ? C12 C13 C14 122.88(17) . . ? C12 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C15 C14 C13 116.71(17) . . ? C15 C14 C17 121.32(18) . . ? C13 C14 C17 121.95(17) . . ? C14 C15 C16 121.77(17) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C15 C16 C11 121.45(17) . . ? C15 C16 H16 119.3 . . ? C11 C16 H16 119.3 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O21 C21 C22 121.29(14) . . ? O21 C21 C26 121.18(15) . . ? C22 C21 C26 117.52(15) . . ? O21 C21 Li1 41.54(10) . 7_666 ? C22 C21 Li1 107.66(12) . 7_666 ? C26 C21 Li1 117.97(13) . 7_666 ? C23 C22 C21 119.61(15) . . ? C23 C22 C2 121.39(15) . . ? C21 C22 C2 118.99(14) . . ? C24 C23 C22 122.66(17) . . ? C24 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C23 C24 C25 117.28(15) . . ? C23 C24 C27 121.76(17) . . ? C25 C24 C27 120.95(16) . . ? C26 C25 C24 121.47(16) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C25 C26 C21 121.44(17) . . ? C25 C26 H26 119.3 . . ? C21 C26 H26 119.3 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C31 O31 C34 109.68(13) . . ? C31 O31 Li2 126.73(14) . . ? C34 O31 Li2 120.86(14) . . ? O31 C31 C32 105.62(15) . . ? O31 C31 H31A 110.6 . . ? C32 C31 H31A 110.6 . . ? O31 C31 H31B 110.6 . . ? C32 C31 H31B 110.6 . . ? H31A C31 H31B 108.7 . . ? C31 C32 C33 101.97(15) . . ? C31 C32 H32A 111.4 . . ? C33 C32 H32A 111.4 . . ? C31 C32 H32B 111.4 . . ? C33 C32 H32B 111.4 . . ? H32A C32 H32B 109.2 . . ? C34 C33 C32 102.49(15) . . ? C34 C33 H33A 111.3 . . ? C32 C33 H33A 111.3 . . ? C34 C33 H33B 111.3 . . ? C32 C33 H33B 111.3 . . ? H33A C33 H33B 109.2 . . ? O31 C34 C33 106.00(15) . . ? O31 C34 H34A 110.5 . . ? C33 C34 H34A 110.5 . . ? O31 C34 H34B 110.5 . . ? C33 C34 H34B 110.5 . . ? H34A C34 H34B 108.7 . . ? C44 O41 C41 105.8(4) . . ? C44 O41 Li1 120.2(4) . . ? C41 O41 Li1 133.2(4) . . ? O41 C41 C42 103.3(3) . . ? O41 C41 H41A 111.1 . . ? C42 C41 H41A 111.1 . . ? O41 C41 H41B 111.1 . . ? C42 C41 H41B 111.1 . . ? H41A C41 H41B 109.1 . . ? C43 C42 C41 105.2(3) . . ? C43 C42 H42A 110.7 . . ? C41 C42 H42A 110.7 . . ? C43 C42 H42B 110.7 . . ? C41 C42 H42B 110.7 . . ? H42A C42 H42B 108.8 . . ? C44 C43 C42 106.5(4) . . ? C44 C43 H43A 110.4 . . ? C42 C43 H43A 110.4 . . ? C44 C43 H43B 110.4 . . ? C42 C43 H43B 110.4 . . ? H43A C43 H43B 108.6 . . ? C43 C44 O41 110.9(4) . . ? C43 C44 H44A 109.5 . . ? O41 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? O41 C44 H44B 109.5 . . ? H44A C44 H44B 108.0 . . ? C441 O411 C411 113.9(12) . . ? C441 O411 Li1 120.7(11) . . ? C411 O411 Li1 125.4(12) . . ? O411 C411 C421 99.8(13) . . ? O411 C411 H41C 111.8 . . ? C421 C411 H41C 111.8 . . ? O411 C411 H41D 111.8 . . ? C421 C411 H41D 111.8 . . ? H41C C411 H41D 109.5 . . ? C411 C421 C431 106.6(11) . . ? C411 C421 H42C 110.4 . . ? C431 C421 H42C 110.4 . . ? C411 C421 H42D 110.4 . . ? C431 C421 H42D 110.4 . . ? H42C C421 H42D 108.6 . . ? C441 C431 C421 101.4(9) . . ? C441 C431 H43C 111.5 . . ? C421 C431 H43C 111.5 . . ? C441 C431 H43D 111.5 . . ? C421 C431 H43D 111.5 . . ? H43C C431 H43D 109.3 . . ? O411 C441 C431 107.1(10) . . ? O411 C441 H44C 110.3 . . ? C431 C441 H44C 110.3 . . ? O411 C441 H44D 110.3 . . ? C431 C441 H44D 110.3 . . ? H44C C441 H44D 108.5 . . ? C53 C51 O51 111.8(9) . . ? C52 C51 O51 104.5(8) . . ? C53 C51 H51D 130.4 . . ? C52 C51 H51D 110.6 . . ? O51 C51 H51D 111.2 . . ? H51A C51 H51D 86.8 . . ? H51B C51 H51D 22.1 . . ? H51C C51 H51D 108.6 . . ? C53 C51 H53A 48.9 . . ? C52 C51 H53A 50.5 . . ? O51 C51 H53A 155.0 . . ? H51A C51 H53A 91.9 . . ? H51B C51 H53A 74.5 . . ? H51C C51 H53A 83.2 . . ? H51D C51 H53A 82.3 . . ? C53 C51 H53B 40.8 . . ? C52 C51 H53B 75.1 . . ? O51 C51 H53B 110.4 . . ? H51A C51 H53B 62.9 . . ? H51B C51 H53B 139.4 . . ? H51C C51 H53B 38.2 . . ? H51D C51 H53B 134.6 . . ? H53A C51 H53B 67.0 . . ? C52 C53 C51 81.1(12) . . ? C52 C53 H51C 122.8 . . ? C51 C53 H51C 42.6 . . ? C52 C53 H53A 74.7 . . ? C51 C53 H53A 55.5 . . ? H51C C53 H53A 66.3 . . ? C52 C53 H53B 163.4 . . ? C51 C53 H53B 82.3 . . ? H51C C53 H53B 40.8 . . ? H53A C53 H53B 95.7 . . ? C52 C53 H52B 66.2 . . ? C51 C53 H52B 119.4 . . ? H51C C53 H52B 126.1 . . ? H53A C53 H52B 67.0 . . ? H53B C53 H52B 123.0 . . ? C53 C52 C51 64.6(11) . . ? C53 C52 H53A 60.9 . . ? C51 C52 H53A 49.9 . . ? C53 C52 H52A 172.0 . . ? C51 C52 H52A 112.3 . . ? H53A C52 H52A 111.2 . . ? C53 C52 H52B 66.7 . . ? C51 C52 H52B 109.8 . . ? H53A C52 H52B 63.2 . . ? H52A C52 H52B 109.0 . . ? 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 O11 Li1 Li2 O21 -176.94(17) . . . 7_666 ? O411 Li1 Li2 O21 89.4(9) . . . 7_666 ? O41 Li1 Li2 O21 76.0(4) . . . 7_666 ? Cl1 Li1 Li2 O21 -99.56(17) 7_666 . . 7_666 ? C21 Li1 Li2 O21 22.12(7) 7_666 . . 7_666 ? Li3 Li1 Li2 O21 -136.79(14) . . . 7_666 ? Li3 Li1 Li2 O21 -38.34(9) 7_666 . . 7_666 ? O411 Li1 Li2 O11 -93.7(9) . . . . ? O21 Li1 Li2 O11 176.94(17) 7_666 . . . ? O41 Li1 Li2 O11 -107.1(4) . . . . ? Cl1 Li1 Li2 O11 77.38(16) 7_666 . . . ? C21 Li1 Li2 O11 -160.94(14) 7_666 . . . ? Li3 Li1 Li2 O11 40.15(9) . . . . ? Li3 Li1 Li2 O11 138.60(13) 7_666 . . . ? O11 Li1 Li2 O31 81.7(2) . . . . ? O411 Li1 Li2 O31 -11.9(9) . . . . ? O21 Li1 Li2 O31 -101.3(2) 7_666 . . . ? O41 Li1 Li2 O31 -25.4(4) . . . . ? Cl1 Li1 Li2 O31 159.10(16) 7_666 . . . ? C21 Li1 Li2 O31 -79.22(19) 7_666 . . . ? Li3 Li1 Li2 O31 121.9(2) . . . . ? Li3 Li1 Li2 O31 -139.7(2) 7_666 . . . ? O11 Li1 Li2 Cl1 -103.30(17) . . . . ? O411 Li1 Li2 Cl1 163.0(9) . . . . ? O21 Li1 Li2 Cl1 73.64(16) 7_666 . . . ? O41 Li1 Li2 Cl1 149.6(3) . . . . ? Cl1 Li1 Li2 Cl1 -25.9(2) 7_666 . . . ? C21 Li1 Li2 Cl1 95.76(16) 7_666 . . . ? Li3 Li1 Li2 Cl1 -63.15(16) . . . . ? Li3 Li1 Li2 Cl1 35.30(13) 7_666 . . . ? O11 Li1 Li2 Li3 -138.60(13) . . . 7_666 ? O411 Li1 Li2 Li3 127.7(9) . . . 7_666 ? O21 Li1 Li2 Li3 38.34(9) 7_666 . . 7_666 ? O41 Li1 Li2 Li3 114.3(4) . . . 7_666 ? Cl1 Li1 Li2 Li3 -61.22(15) 7_666 . . 7_666 ? C21 Li1 Li2 Li3 60.46(8) 7_666 . . 7_666 ? Li3 Li1 Li2 Li3 -98.45(10) . . . 7_666 ? O11 Li1 Li2 Li3 -40.15(9) . . . . ? O411 Li1 Li2 Li3 -133.8(9) . . . . ? O21 Li1 Li2 Li3 136.79(14) 7_666 . . . ? O41 Li1 Li2 Li3 -147.2(4) . . . . ? Cl1 Li1 Li2 Li3 37.23(13) 7_666 . . . ? C21 Li1 Li2 Li3 158.91(12) 7_666 . . . ? Li3 Li1 Li2 Li3 98.45(10) 7_666 . . . ? O411 Li1 Li3 O11 87.9(9) . . . . ? O21 Li1 Li3 O11 -77.75(15) 7_666 . . . ? O41 Li1 Li3 O11 96.3(4) . . . . ? Cl1 Li1 Li3 O11 169.73(17) 7_666 . . . ? Li2 Li1 Li3 O11 -45.60(11) . . . . ? C21 Li1 Li3 O11 -73.44(19) 7_666 . . . ? Li3 Li1 Li3 O11 -102.64(14) 7_666 . . . ? O11 Li1 Li3 O21 127.49(19) . . . . ? O411 Li1 Li3 O21 -144.6(9) . . . . ? O21 Li1 Li3 O21 49.74(19) 7_666 . . . ? O41 Li1 Li3 O21 -136.2(4) . . . . ? Cl1 Li1 Li3 O21 -62.78(13) 7_666 . . . ? Li2 Li1 Li3 O21 81.89(15) . . . . ? C21 Li1 Li3 O21 54.1(2) 7_666 . . . ? Li3 Li1 Li3 O21 24.86(11) 7_666 . . . ? O11 Li1 Li3 N1 7.27(19) . . . . ? O411 Li1 Li3 N1 95.2(9) . . . . ? O21 Li1 Li3 N1 -70.5(2) 7_666 . . . ? O41 Li1 Li3 N1 103.5(4) . . . . ? Cl1 Li1 Li3 N1 177.0(2) 7_666 . . . ? Li2 Li1 Li3 N1 -38.3(2) . . . . ? C21 Li1 Li3 N1 -66.2(3) 7_666 . . . ? Li3 Li1 Li3 N1 -95.4(2) 7_666 . . . ? O11 Li1 Li3 N2 -95.05(16) . . . . ? O411 Li1 Li3 N2 -7.1(9) . . . . ? O21 Li1 Li3 N2 -172.80(13) 7_666 . . . ? O41 Li1 Li3 N2 1.2(4) . . . . ? Cl1 Li1 Li3 N2 74.68(13) 7_666 . . . ? Li2 Li1 Li3 N2 -140.65(15) . . . . ? C21 Li1 Li3 N2 -168.49(15) 7_666 . . . ? Li3 Li1 Li3 N2 162.32(16) 7_666 . . . ? O11 Li1 Li3 Cl1 -169.73(17) . . . 7_666 ? O411 Li1 Li3 Cl1 -81.8(9) . . . 7_666 ? O21 Li1 Li3 Cl1 112.52(15) 7_666 . . 7_666 ? O41 Li1 Li3 Cl1 -73.5(4) . . . 7_666 ? Li2 Li1 Li3 Cl1 144.67(13) . . . 7_666 ? C21 Li1 Li3 Cl1 116.83(19) 7_666 . . 7_666 ? Li3 Li1 Li3 Cl1 87.64(10) 7_666 . . 7_666 ? O11 Li1 Li3 C11 -19.40(8) . . . . ? O411 Li1 Li3 C11 68.5(9) . . . . ? O21 Li1 Li3 C11 -97.15(14) 7_666 . . . ? O41 Li1 Li3 C11 76.9(4) . . . . ? Cl1 Li1 Li3 C11 150.33(12) 7_666 . . . ? Li2 Li1 Li3 C11 -65.00(10) . . . . ? C21 Li1 Li3 C11 -92.84(18) 7_666 . . . ? Li3 Li1 Li3 C11 -122.04(11) 7_666 . . . ? O11 Li1 Li3 Li2 148.34(16) . . . 7_666 ? O411 Li1 Li3 Li2 -123.7(9) . . . 7_666 ? O21 Li1 Li3 Li2 70.59(14) 7_666 . . 7_666 ? O41 Li1 Li3 Li2 -115.4(4) . . . 7_666 ? Cl1 Li1 Li3 Li2 -41.93(9) 7_666 . . 7_666 ? Li2 Li1 Li3 Li2 102.74(11) . . . 7_666 ? C21 Li1 Li3 Li2 74.90(18) 7_666 . . 7_666 ? Li3 Li1 Li3 Li2 45.70(8) 7_666 . . 7_666 ? O11 Li1 Li3 Li2 45.60(12) . . . . ? O411 Li1 Li3 Li2 133.5(9) . . . . ? O21 Li1 Li3 Li2 -32.15(11) 7_666 . . . ? O41 Li1 Li3 Li2 141.9(4) . . . . ? Cl1 Li1 Li3 Li2 -144.67(13) 7_666 . . . ? C21 Li1 Li3 Li2 -27.84(15) 7_666 . . . ? Li3 Li1 Li3 Li2 -57.04(10) 7_666 . . . ? O11 Li1 Li3 Li1 102.63(14) . . . 7_666 ? O411 Li1 Li3 Li1 -169.4(9) . . . 7_666 ? O21 Li1 Li3 Li1 24.88(11) 7_666 . . 7_666 ? O41 Li1 Li3 Li1 -161.1(4) . . . 7_666 ? Cl1 Li1 Li3 Li1 -87.64(10) 7_666 . . 7_666 ? Li2 Li1 Li3 Li1 57.03(10) . . . 7_666 ? C21 Li1 Li3 Li1 29.20(16) 7_666 . . 7_666 ? Li3 Li1 Li3 Li1 0.0 7_666 . . 7_666 ? O21 Li2 Li3 O11 90.41(16) 7_666 . . . ? O31 Li2 Li3 O11 -62.5(2) . . . . ? Cl1 Li2 Li3 O11 -167.09(18) . . . . ? Li1 Li2 Li3 O11 59.35(14) . . . . ? Li3 Li2 Li3 O11 131.59(18) 7_666 . . . ? O21 Li2 Li3 O21 -80.71(15) 7_666 . . . ? O11 Li2 Li3 O21 -171.1(2) . . . . ? O31 Li2 Li3 O21 126.37(19) . . . . ? Cl1 Li2 Li3 O21 21.79(13) . . . . ? Li1 Li2 Li3 O21 -111.77(15) . . . . ? Li3 Li2 Li3 O21 -39.53(9) 7_666 . . . ? O21 Li2 Li3 N1 -174.69(13) 7_666 . . . ? O11 Li2 Li3 N1 94.90(16) . . . . ? O31 Li2 Li3 N1 32.4(2) . . . . ? Cl1 Li2 Li3 N1 -72.19(12) . . . . ? Li1 Li2 Li3 N1 154.25(15) . . . . ? Li3 Li2 Li3 N1 -133.51(15) 7_666 . . . ? O21 Li2 Li3 N2 102.7(2) 7_666 . . . ? O11 Li2 Li3 N2 12.3(2) . . . . ? O31 Li2 Li3 N2 -50.2(3) . . . . ? Cl1 Li2 Li3 N2 -154.8(2) . . . . ? Li1 Li2 Li3 N2 71.7(2) . . . . ? Li3 Li2 Li3 N2 143.9(3) 7_666 . . . ? O21 Li2 Li3 Cl1 5.74(12) 7_666 . . 7_666 ? O11 Li2 Li3 Cl1 -84.67(14) . . . 7_666 ? O31 Li2 Li3 Cl1 -147.19(18) . . . 7_666 ? Cl1 Li2 Li3 Cl1 108.23(10) . . . 7_666 ? Li1 Li2 Li3 Cl1 -25.33(10) . . . 7_666 ? Li3 Li2 Li3 Cl1 46.92(8) 7_666 . . 7_666 ? O21 Li2 Li3 C11 113.84(13) 7_666 . . . ? O11 Li2 Li3 C11 23.42(10) . . . . ? O31 Li2 Li3 C11 -39.09(18) . . . . ? Cl1 Li2 Li3 C11 -143.67(12) . . . . ? Li1 Li2 Li3 C11 82.77(12) . . . . ? Li3 Li2 Li3 C11 155.02(14) 7_666 . . . ? O21 Li2 Li3 Li1 31.06(11) 7_666 . . . ? O11 Li2 Li3 Li1 -59.35(14) . . . . ? O31 Li2 Li3 Li1 -121.9(2) . . . . ? Cl1 Li2 Li3 Li1 133.56(14) . . . . ? Li3 Li2 Li3 Li1 72.25(12) 7_666 . . . ? O21 Li2 Li3 Li2 -41.18(10) 7_666 . . 7_666 ? O11 Li2 Li3 Li2 -131.59(18) . . . 7_666 ? O31 Li2 Li3 Li2 165.9(2) . . . 7_666 ? Cl1 Li2 Li3 Li2 61.31(9) . . . 7_666 ? Li1 Li2 Li3 Li2 -72.25(12) . . . 7_666 ? Li3 Li2 Li3 Li2 0.0 7_666 . . 7_666 ? O21 Li2 Li3 Li1 -83.82(12) 7_666 . . 7_666 ? O11 Li2 Li3 Li1 -174.23(17) . . . 7_666 ? O31 Li2 Li3 Li1 123.3(2) . . . 7_666 ? Cl1 Li2 Li3 Li1 18.68(8) . . . 7_666 ? Li1 Li2 Li3 Li1 -114.88(11) . . . 7_666 ? Li3 Li2 Li3 Li1 -42.63(8) 7_666 . . 7_666 ? O21 Li2 Cl1 Li1 69.99(14) 7_666 . . 7_666 ? O11 Li2 Cl1 Li1 -35.39(19) . . . 7_666 ? O31 Li2 Cl1 Li1 -161.06(11) . . . 7_666 ? Li1 Li2 Cl1 Li1 22.7(2) . . . 7_666 ? Li3 Li2 Cl1 Li1 62.02(11) 7_666 . . 7_666 ? O11 Li2 Cl1 Li3 -97.40(17) . . . 7_666 ? O31 Li2 Cl1 Li3 136.92(13) . . . 7_666 ? Li1 Li2 Cl1 Li3 -39.35(15) . . . 7_666 ? Li3 Li2 Cl1 Li3 -89.01(10) . . . 7_666 ? O411 Li1 O11 C11 3.3(6) . . . . ? O21 Li1 O11 C11 -122.19(16) 7_666 . . . ? O41 Li1 O11 C11 -0.6(3) . . . . ? Cl1 Li1 O11 C11 117.52(15) 7_666 . . . ? Li2 Li1 O11 C11 -119.92(17) . . . . ? C21 Li1 O11 C11 -100.85(18) 7_666 . . . ? Li3 Li1 O11 C11 126.80(19) . . . . ? Li3 Li1 O11 C11 -154.26(13) 7_666 . . . ? O411 Li1 O11 Li2 123.2(6) . . . . ? O21 Li1 O11 Li2 -2.27(13) 7_666 . . . ? O41 Li1 O11 Li2 119.3(3) . . . . ? Cl1 Li1 O11 Li2 -122.56(14) 7_666 . . . ? C21 Li1 O11 Li2 19.06(14) 7_666 . . . ? Li3 Li1 O11 Li2 -113.29(14) . . . . ? Li3 Li1 O11 Li2 -34.35(12) 7_666 . . . ? O411 Li1 O11 Li3 -123.5(6) . . . . ? O21 Li1 O11 Li3 111.01(14) 7_666 . . . ? O41 Li1 O11 Li3 -127.4(3) . . . . ? Cl1 Li1 O11 Li3 -9.27(15) 7_666 . . . ? Li2 Li1 O11 Li3 113.29(14) . . . . ? C21 Li1 O11 Li3 132.35(14) 7_666 . . . ? Li3 Li1 O11 Li3 78.94(13) 7_666 . . . ? O21 Li2 O11 C11 134.71(13) 7_666 . . . ? O31 Li2 O11 C11 3.8(2) . . . . ? Cl1 Li2 O11 C11 -116.49(17) . . . . ? Li1 Li2 O11 C11 132.41(15) . . . . ? Li3 Li2 O11 C11 175.24(12) 7_666 . . . ? Li3 Li2 O11 C11 -131.77(18) . . . . ? O21 Li2 O11 Li1 2.30(13) 7_666 . . . ? O31 Li2 O11 Li1 -128.63(16) . . . . ? Cl1 Li2 O11 Li1 111.10(17) . . . . ? Li3 Li2 O11 Li1 42.83(14) 7_666 . . . ? Li3 Li2 O11 Li1 95.82(15) . . . . ? O21 Li2 O11 Li3 -93.52(15) 7_666 . . . ? O31 Li2 O11 Li3 135.56(15) . . . . ? Cl1 Li2 O11 Li3 15.3(2) . . . . ? Li1 Li2 O11 Li3 -95.82(15) . . . . ? Li3 Li2 O11 Li3 -52.98(19) 7_666 . . . ? O21 Li3 O11 C11 145.50(19) . . . . ? N1 Li3 O11 C11 46.32(17) . . . . ? N2 Li3 O11 C11 -38.01(18) . . . . ? Cl1 Li3 O11 C11 -131.19(12) 7_666 . . . ? Li1 Li3 O11 C11 -138.78(17) . . . . ? Li2 Li3 O11 C11 -172.33(13) 7_666 . . . ? Li2 Li3 O11 C11 133.91(18) . . . . ? Li1 Li3 O11 C11 139.33(12) 7_666 . . . ? O21 Li3 O11 Li1 -75.7(2) . . . . ? N1 Li3 O11 Li1 -174.90(13) . . . . ? N2 Li3 O11 Li1 100.77(16) . . . . ? Cl1 Li3 O11 Li1 7.59(13) 7_666 . . . ? C11 Li3 O11 Li1 138.78(17) . . . . ? Li2 Li3 O11 Li1 -33.55(17) 7_666 . . . ? Li2 Li3 O11 Li1 -87.31(15) . . . . ? Li1 Li3 O11 Li1 -81.89(14) 7_666 . . . ? O21 Li3 O11 Li2 11.6(3) . . . . ? N1 Li3 O11 Li2 -87.59(15) . . . . ? N2 Li3 O11 Li2 -171.92(14) . . . . ? Cl1 Li3 O11 Li2 94.90(13) 7_666 . . . ? C11 Li3 O11 Li2 -133.91(18) . . . . ? Li1 Li3 O11 Li2 87.31(15) . . . . ? Li2 Li3 O11 Li2 53.8(2) 7_666 . . . ? Li1 Li3 O11 Li2 5.42(16) 7_666 . . . ? O11 Li3 O21 C21 -144.82(19) . . . . ? N1 Li3 O21 C21 -44.79(16) . . . . ? N2 Li3 O21 C21 39.0(2) . . . . ? Cl1 Li3 O21 C21 131.24(12) 7_666 . . . ? C11 Li3 O21 C21 -114.9(3) . . . . ? Li1 Li3 O21 C21 172.48(13) . . . . ? Li2 Li3 O21 C21 139.78(16) 7_666 . . . ? Li2 Li3 O21 C21 -138.52(12) . . . . ? Li1 Li3 O21 C21 -132.95(19) 7_666 . . . ? O11 Li3 O21 Li2 75.4(2) . . . 7_666 ? N1 Li3 O21 Li2 175.43(12) . . . 7_666 ? N2 Li3 O21 Li2 -100.76(17) . . . 7_666 ? Cl1 Li3 O21 Li2 -8.53(11) 7_666 . . 7_666 ? C11 Li3 O21 Li2 105.3(3) . . . 7_666 ? Li1 Li3 O21 Li2 32.70(16) . . . 7_666 ? Li2 Li3 O21 Li2 81.70(14) . . . 7_666 ? Li1 Li3 O21 Li2 87.27(15) 7_666 . . 7_666 ? O11 Li3 O21 Li1 -11.9(3) . . . 7_666 ? N1 Li3 O21 Li1 88.16(15) . . . 7_666 ? N2 Li3 O21 Li1 171.96(15) . . . 7_666 ? Cl1 Li3 O21 Li1 -95.81(13) 7_666 . . 7_666 ? C11 Li3 O21 Li1 18.1(3) . . . 7_666 ? Li1 Li3 O21 Li1 -54.6(2) . . . 7_666 ? Li2 Li3 O21 Li1 -87.27(15) 7_666 . . 7_666 ? Li2 Li3 O21 Li1 -5.57(17) . . . 7_666 ? O11 Li3 N1 C2 123.86(13) . . . . ? O21 Li3 N1 C2 -7.43(15) . . . . ? N2 Li3 N1 C2 -127.19(12) . . . . ? Cl1 Li3 N1 C2 -95(2) 7_666 . . . ? C11 Li3 N1 C2 143.24(11) . . . . ? Li1 Li3 N1 C2 119.1(2) . . . . ? Li2 Li3 N1 C2 -3.4(2) 7_666 . . . ? Li2 Li3 N1 C2 91.19(13) . . . . ? Li1 Li3 N1 C2 23.60(13) 7_666 . . . ? O11 Li3 N1 C3 -115.25(13) . . . . ? O21 Li3 N1 C3 113.47(13) . . . . ? Li1 Li3 N1 C3 -120.0(2) . . . . ? Li2 Li3 N1 C3 117.50(18) 7_666 . . . ? Li2 Li3 N1 C3 -147.92(12) . . . . ? Li1 Li3 N1 C3 144.49(11) 7_666 . . . ? O11 Li3 N1 C1 6.29(16) . . . . ? O21 Li3 N1 C1 -125.00(13) . . . . ? N2 Li3 N1 C1 115.24(13) . . . . ? Li1 Li3 N1 C1 1.6(2) . . . . ? Li2 Li3 N1 C1 -120.96(18) 7_666 . . . ? Li2 Li3 N1 C1 -26.38(14) . . . . ? Li1 Li3 N1 C1 -93.97(13) 7_666 . . . ? O11 Li3 N2 C6 -46.2(2) . . . . ? O21 Li3 N2 C6 130.71(17) . . . . ? N1 Li3 N2 C6 -139.37(14) . . . . ? Li1 Li3 N2 C6 -2.90(19) . . . . ? Li2 Li3 N2 C6 84.41(18) 7_666 . . . ? Li2 Li3 N2 C6 -53.2(3) . . . . ? Li1 Li3 N2 C6 139.1(3) 7_666 . . . ? O11 Li3 N2 C5 -166.63(14) . . . . ? O21 Li3 N2 C5 10.3(2) . . . . ? N1 Li3 N2 C5 100.20(14) . . . . ? Cl1 Li3 N2 C5 -77.68(14) 7_666 . . . ? C11 Li3 N2 C5 177.37(12) . . . . ? Li1 Li3 N2 C5 -123.32(15) . . . . ? Li2 Li3 N2 C5 -36.02(19) 7_666 . . . ? Li2 Li3 N2 C5 -173.6(2) . . . . ? Li1 Li3 N2 C5 18.7(3) 7_666 . . . ? O11 Li3 N2 C4 75.13(17) . . . . ? O21 Li3 N2 C4 -107.95(17) . . . . ? N1 Li3 N2 C4 -18.03(13) . . . . ? Cl1 Li3 N2 C4 164.08(11) 7_666 . . . ? C11 Li3 N2 C4 59.14(13) . . . . ? Li1 Li3 N2 C4 118.44(14) . . . . ? Li2 Li3 N2 C4 -154.26(13) 7_666 . . . ? Li2 Li3 N2 C4 68.1(2) . . . . ? Li1 Li3 N2 C4 -99.5(3) 7_666 . . . ? C2 N1 C1 C12 -173.05(13) . . . . ? C3 N1 C1 C12 64.02(18) . . . . ? Li3 N1 C1 C12 -54.86(17) . . . . ? C3 N1 C2 C22 -64.15(18) . . . . ? C1 N1 C2 C22 171.99(13) . . . . ? Li3 N1 C2 C22 55.12(17) . . . . ? C2 N1 C3 C4 150.20(14) . . . . ? C1 N1 C3 C4 -88.21(17) . . . . ? Li3 N1 C3 C4 30.18(18) . . . . ? C6 N2 C4 C3 163.96(14) . . . . ? C5 N2 C4 C3 -75.41(18) . . . . ? Li3 N2 C4 C3 39.74(17) . . . . ? N1 C3 C4 N2 -49.32(18) . . . . ? Li1 O11 C11 C16 1.9(2) . . . . ? Li2 O11 C11 C16 -104.05(18) . . . . ? Li3 O11 C11 C16 123.24(17) . . . . ? Li1 O11 C11 C12 -178.39(15) . . . . ? Li2 O11 C11 C12 75.63(18) . . . . ? Li3 O11 C11 C12 -57.09(19) . . . . ? Li1 O11 C11 Li3 -121.3(2) . . . . ? Li2 O11 C11 Li3 132.71(18) . . . . ? O21 Li3 C11 O11 -58.0(3) . . . . ? N1 Li3 C11 O11 -132.36(17) . . . . ? N2 Li3 C11 O11 144.46(18) . . . . ? Cl1 Li3 C11 O11 51.13(13) 7_666 . . . ? Li1 Li3 C11 O11 28.85(13) . . . . ? Li2 Li3 C11 O11 10.70(18) 7_666 . . . ? Li2 Li3 C11 O11 -28.65(12) . . . . ? Li1 Li3 C11 O11 -47.40(14) 7_666 . . . ? O11 Li3 C11 C16 -89.8(2) . . . . ? O21 Li3 C11 C16 -147.7(3) . . . . ? N1 Li3 C11 C16 137.87(17) . . . . ? N2 Li3 C11 C16 54.7(2) . . . . ? Cl1 Li3 C11 C16 -38.6(2) 7_666 . . . ? Li1 Li3 C11 C16 -60.93(18) . . . . ? Li2 Li3 C11 C16 -79.1(3) 7_666 . . . ? Li2 Li3 C11 C16 -118.43(19) . . . . ? Li1 Li3 C11 C16 -137.17(17) 7_666 . . . ? O11 Li3 C11 C12 134.05(18) . . . . ? O21 Li3 C11 C12 76.1(3) . . . . ? N1 Li3 C11 C12 1.70(12) . . . . ? N2 Li3 C11 C12 -81.48(13) . . . . ? Cl1 Li3 C11 C12 -174.82(12) 7_666 . . . ? Li1 Li3 C11 C12 162.90(14) . . . . ? Li2 Li3 C11 C12 144.8(2) 7_666 . . . ? Li2 Li3 C11 C12 105.40(13) . . . . ? Li1 Li3 C11 C12 86.66(15) 7_666 . . . ? O11 C11 C12 C13 -177.71(14) . . . . ? C16 C11 C12 C13 2.0(2) . . . . ? Li3 C11 C12 C13 148.19(14) . . . . ? O11 C11 C12 C1 3.0(2) . . . . ? C16 C11 C12 C1 -177.36(14) . . . . ? Li3 C11 C12 C1 -31.15(16) . . . . ? N1 C1 C12 C13 -115.57(17) . . . . ? N1 C1 C12 C11 63.75(19) . . . . ? C11 C12 C13 C14 -1.0(2) . . . . ? C1 C12 C13 C14 178.36(15) . . . . ? C12 C13 C14 C15 -0.8(2) . . . . ? C12 C13 C14 C17 -179.78(17) . . . . ? C13 C14 C15 C16 1.6(3) . . . . ? C17 C14 C15 C16 -179.46(18) . . . . ? C14 C15 C16 C11 -0.5(3) . . . . ? O11 C11 C16 C15 178.43(15) . . . . ? C12 C11 C16 C15 -1.3(2) . . . . ? Li3 C11 C16 C15 -130.35(18) . . . . ? Li2 O21 C21 C22 178.59(17) 7_666 . . . ? Li1 O21 C21 C22 -81.3(2) 7_666 . . . ? Li3 O21 C21 C22 54.2(2) . . . . ? Li2 O21 C21 C26 -1.8(3) 7_666 . . . ? Li1 O21 C21 C26 98.25(19) 7_666 . . . ? Li3 O21 C21 C26 -126.24(18) . . . . ? Li2 O21 C21 Li1 -100.1(2) 7_666 . . 7_666 ? Li3 O21 C21 Li1 135.51(18) . . . 7_666 ? O21 C21 C22 C23 179.30(16) . . . . ? C26 C21 C22 C23 -0.3(3) . . . . ? Li1 C21 C22 C23 135.83(16) 7_666 . . . ? O21 C21 C22 C2 0.5(3) . . . . ? C26 C21 C22 C2 -179.15(16) . . . . ? Li1 C21 C22 C2 -43.02(19) 7_666 . . . ? N1 C2 C22 C23 116.84(18) . . . . ? N1 C2 C22 C21 -64.3(2) . . . . ? C21 C22 C23 C24 0.4(3) . . . . ? C2 C22 C23 C24 179.19(17) . . . . ? C22 C23 C24 C25 -0.2(3) . . . . ? C22 C23 C24 C27 179.04(17) . . . . ? C23 C24 C25 C26 0.0(3) . . . . ? C27 C24 C25 C26 -179.28(18) . . . . ? C24 C25 C26 C21 0.1(3) . . . . ? O21 C21 C26 C25 -179.52(17) . . . . ? C22 C21 C26 C25 0.1(3) . . . . ? Li1 C21 C26 C25 -131.53(18) 7_666 . . . ? O21 Li2 O31 C31 -78.0(2) 7_666 . . . ? O11 Li2 O31 C31 36.7(2) . . . . ? Cl1 Li2 O31 C31 168.55(12) . . . . ? Li1 Li2 O31 C31 -15.6(3) . . . . ? Li3 Li2 O31 C31 -131.7(2) 7_666 . . . ? Li3 Li2 O31 C31 68.9(2) . . . . ? O21 Li2 O31 C34 81.2(2) 7_666 . . . ? O11 Li2 O31 C34 -163.99(14) . . . . ? Cl1 Li2 O31 C34 -32.17(18) . . . . ? Li1 Li2 O31 C34 143.67(19) . . . . ? Li3 Li2 O31 C34 27.6(3) 7_666 . . . ? Li3 Li2 O31 C34 -131.85(19) . . . . ? C34 O31 C31 C32 -14.18(19) . . . . ? Li2 O31 C31 C32 147.00(16) . . . . ? O31 C31 C32 C33 32.05(19) . . . . ? C31 C32 C33 C34 -37.19(19) . . . . ? C31 O31 C34 C33 -9.93(19) . . . . ? Li2 O31 C34 C33 -172.40(15) . . . . ? C32 C33 C34 O31 29.65(19) . . . . ? O11 Li1 O41 C44 131.6(5) . . . . ? O411 Li1 O41 C44 111(4) . . . . ? O21 Li1 O41 C44 -113.1(5) 7_666 . . . ? Cl1 Li1 O41 C44 13.2(6) 7_666 . . . ? Li2 Li1 O41 C44 -163.0(4) . . . . ? C21 Li1 O41 C44 -114.4(5) 7_666 . . . ? Li3 Li1 O41 C44 73.0(7) . . . . ? Li3 Li1 O41 C44 -82.6(5) 7_666 . . . ? O11 Li1 O41 C41 -60.2(7) . . . . ? O411 Li1 O41 C41 -81(4) . . . . ? O21 Li1 O41 C41 55.1(7) 7_666 . . . ? Cl1 Li1 O41 C41 -178.6(6) 7_666 . . . ? Li2 Li1 O41 C41 5.3(9) . . . . ? C21 Li1 O41 C41 53.8(6) 7_666 . . . ? Li3 Li1 O41 C41 -118.8(5) . . . . ? Li3 Li1 O41 C41 85.6(7) 7_666 . . . ? C44 O41 C41 C42 -26.1(6) . . . . ? Li1 O41 C41 C42 164.4(5) . . . . ? O41 C41 C42 C43 28.5(5) . . . . ? C41 C42 C43 C44 -19.5(6) . . . . ? C42 C43 C44 O41 3.3(7) . . . . ? C41 O41 C44 C43 15.4(7) . . . . ? Li1 O41 C44 C43 -173.5(5) . . . . ? O11 Li1 O411 C441 85.8(17) . . . . ? O21 Li1 O411 C441 -159.7(13) 7_666 . . . ? O41 Li1 O411 C441 -112(5) . . . . ? Cl1 Li1 O411 C441 -28.1(18) 7_666 . . . ? Li2 Li1 O411 C441 144.1(12) . . . . ? C21 Li1 O411 C441 -157.6(17) 7_666 . . . ? Li3 Li1 O411 C441 36(2) . . . . ? Li3 Li1 O411 C441 -128.6(13) 7_666 . . . ? O11 Li1 O411 C411 -97(2) . . . . ? O21 Li1 O411 C411 17(2) 7_666 . . . ? O41 Li1 O411 C411 65(3) . . . . ? Cl1 Li1 O411 C411 149(2) 7_666 . . . ? Li2 Li1 O411 C411 -39(3) . . . . ? C21 Li1 O411 C411 20(2) 7_666 . . . ? Li3 Li1 O411 C411 -147.3(18) . . . . ? Li3 Li1 O411 C411 49(3) 7_666 . . . ? C441 O411 C411 C421 -20(3) . . . . ? Li1 O411 C411 C421 163.0(16) . . . . ? O411 C411 C421 C431 31(2) . . . . ? C411 C421 C431 C441 -32.6(18) . . . . ? C411 O411 C441 C431 -1(2) . . . . ? Li1 O411 C441 C431 176.9(13) . . . . ? C421 C431 C441 O411 19.7(17) . . . . ? O51 C51 C53 C52 -83.8(17) . . . . ? O51 C51 C52 C53 107.6(16) . . . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.468 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.058 # Attachment '- MS_Janas.cif' data_H2L2(C20H28N2O2) _database_code_depnum_ccdc_archive 'CCDC 832242' #TrackingRef '- MS_Janas.cif' # CCDC 832242 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H28 N2 O2' _chemical_formula_sum 'C20 H28 N2 O2' _chemical_formula_weight 328.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.820(3) _cell_length_b 6.049(3) _cell_length_c 21.294(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.48(3) _cell_angle_gamma 90.00 _cell_volume 1820.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2727 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _exptl_crystal_description PLATE _exptl_crystal_colour WHITE _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kuma KM-4 CCD kappa-axis diffractometer' _diffrn_measurement_method \OMEGA _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12298 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4128 _reflns_number_gt 2768 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma KM4 software 1996' _computing_cell_refinement 'Kuma KM4 software 1996' _computing_data_reduction 'Kuma KM4 software 1996' _computing_structure_solution 'SHELXTL-NT V5.1, Bruker AXS 1999' _computing_structure_refinement 'SHELXTL-NT V5.1, Bruker AXS 1999' _computing_molecular_graphics 'SHELXTL-NT V5.1, Bruker AXS 1999' _computing_publication_material 'SHELXTL-NT V5.1, Bruker AXS 1999' _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^)+(0.0479P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4128 _refine_ls_number_parameters 229 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O11 O 0.34465(7) 0.33713(16) 0.14314(5) 0.0235(2) Uani 1 1 d D . . H11A H 0.3124(11) 0.231(2) 0.1141(7) 0.060(6) Uiso 1 1 d D . . O21 O 0.10982(7) 0.38063(16) 0.13690(5) 0.0224(2) Uani 1 1 d D . . H21A H 0.1540(10) 0.272(2) 0.1392(9) 0.057(6) Uiso 1 1 d D . . N1 N 0.18822(7) -0.02259(18) 0.14628(5) 0.0173(3) Uani 1 1 d . . . N2 N 0.24672(8) 0.10373(19) 0.03156(5) 0.0201(3) Uani 1 1 d . . . C1 C 0.28707(9) -0.0978(2) 0.17755(7) 0.0185(3) Uani 1 1 d . . . H1A H 0.3185 -0.1196 0.1430 0.022 Uiso 1 1 calc R . . H1B H 0.2861 -0.2419 0.1994 0.022 Uiso 1 1 calc R . . C2 C 0.13230(9) -0.0627(2) 0.19226(7) 0.0183(3) Uani 1 1 d . . . H2A H 0.1702 -0.0179 0.2372 0.022 Uiso 1 1 calc R . . H2B H 0.1191 -0.2229 0.1932 0.022 Uiso 1 1 calc R . . C3 C 0.14580(10) -0.1288(2) 0.08144(7) 0.0205(3) Uani 1 1 d . . . H3A H 0.0790 -0.1663 0.0764 0.025 Uiso 1 1 calc R . . H3B H 0.1800 -0.2679 0.0793 0.025 Uiso 1 1 calc R . . C4 C 0.15036(10) 0.0231(2) 0.02515(7) 0.0226(3) Uani 1 1 d . . . H4A H 0.1262 -0.0579 -0.0170 0.027 Uiso 1 1 calc R . . H4B H 0.1084 0.1516 0.0235 0.027 Uiso 1 1 calc R . . C5 C 0.24171(11) 0.2988(3) -0.01050(7) 0.0303(4) Uani 1 1 d . . . H5A H 0.2127 0.2574 -0.0567 0.046 Uiso 1 1 calc R . . H5B H 0.3057 0.3554 -0.0047 0.046 Uiso 1 1 calc R . . H5C H 0.2035 0.4135 0.0018 0.046 Uiso 1 1 calc R . . C6 C 0.30452(11) -0.0666(3) 0.01304(7) 0.0289(4) Uani 1 1 d . . . H6A H 0.3067 -0.1987 0.0401 0.043 Uiso 1 1 calc R . . H6B H 0.3688 -0.0103 0.0202 0.043 Uiso 1 1 calc R . . H6C H 0.2766 -0.1045 -0.0335 0.043 Uiso 1 1 calc R . . C11 C 0.36914(9) 0.2702(2) 0.20774(7) 0.0186(3) Uani 1 1 d . . . C12 C 0.34316(9) 0.0651(2) 0.22746(7) 0.0174(3) Uani 1 1 d . . . C13 C 0.37418(9) 0.0121(2) 0.29454(7) 0.0206(3) Uani 1 1 d . . . H13 H 0.3570 -0.1270 0.3082 0.025 Uiso 1 1 calc R . . C14 C 0.42919(9) 0.1548(2) 0.34203(7) 0.0226(3) Uani 1 1 d . . . C15 C 0.45319(9) 0.3578(2) 0.32064(7) 0.0221(3) Uani 1 1 d . . . H15 H 0.4905 0.4588 0.3520 0.027 Uiso 1 1 calc R . . C16 C 0.42390(9) 0.4163(2) 0.25445(7) 0.0204(3) Uani 1 1 d . . . H16 H 0.4412 0.5557 0.2410 0.024 Uiso 1 1 calc R . . C17 C 0.46442(11) 0.0860(3) 0.41366(7) 0.0331(4) Uani 1 1 d . . . H17A H 0.4219 -0.0260 0.4223 0.050 Uiso 1 1 calc R . . H17B H 0.4659 0.2151 0.4417 0.050 Uiso 1 1 calc R . . H17C H 0.5283 0.0243 0.4232 0.050 Uiso 1 1 calc R . . C21 C 0.03307(9) 0.2771(2) 0.14734(6) 0.0178(3) Uani 1 1 d . . . C22 C 0.03971(9) 0.0624(2) 0.17331(6) 0.0169(3) Uani 1 1 d . . . C23 C -0.04021(9) -0.0295(2) 0.18463(6) 0.0178(3) Uani 1 1 d . . . H23 H -0.0361 -0.1748 0.2023 0.021 Uiso 1 1 calc R . . C24 C -0.12584(10) 0.0828(2) 0.17117(6) 0.0190(3) Uani 1 1 d . . . C25 C -0.13028(10) 0.2951(2) 0.14448(7) 0.0205(3) Uani 1 1 d . . . H25 H -0.1880 0.3752 0.1343 0.025 Uiso 1 1 calc R . . C26 C -0.05203(10) 0.3909(2) 0.13250(7) 0.0204(3) Uani 1 1 d . . . H26 H -0.0567 0.5350 0.1141 0.024 Uiso 1 1 calc R . . C27 C -0.21054(10) -0.0233(2) 0.18476(7) 0.0248(3) Uani 1 1 d . . . H27A H -0.2130 -0.1805 0.1731 0.037 Uiso 1 1 calc R . . H27B H -0.2685 0.0498 0.1583 0.037 Uiso 1 1 calc R . . H27C H -0.2049 -0.0081 0.2316 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O11 0.0248(5) 0.0234(6) 0.0198(5) 0.0017(4) 0.0031(5) -0.0038(5) O21 0.0212(5) 0.0180(5) 0.0293(6) 0.0019(4) 0.0098(5) -0.0021(4) N1 0.0154(6) 0.0211(6) 0.0151(6) 0.0006(5) 0.0043(5) 0.0001(5) N2 0.0217(6) 0.0204(6) 0.0182(6) 0.0013(5) 0.0060(5) 0.0000(5) C1 0.0173(7) 0.0188(7) 0.0198(7) 0.0013(6) 0.0062(6) 0.0004(6) C2 0.0189(7) 0.0178(7) 0.0191(7) 0.0022(6) 0.0070(6) -0.0002(6) C3 0.0194(7) 0.0213(7) 0.0205(7) -0.0032(6) 0.0059(6) -0.0025(6) C4 0.0219(7) 0.0259(8) 0.0189(7) -0.0020(6) 0.0046(6) -0.0008(6) C5 0.0377(9) 0.0287(8) 0.0231(8) 0.0026(7) 0.0068(7) -0.0028(7) C6 0.0269(8) 0.0364(9) 0.0245(8) -0.0010(7) 0.0092(7) 0.0033(7) C11 0.0134(6) 0.0234(8) 0.0188(7) 0.0004(6) 0.0043(6) 0.0026(6) C12 0.0129(6) 0.0192(7) 0.0204(7) -0.0014(6) 0.0052(6) 0.0020(6) C13 0.0167(7) 0.0229(7) 0.0232(7) 0.0042(6) 0.0076(6) 0.0019(6) C14 0.0165(7) 0.0336(9) 0.0178(7) 0.0004(6) 0.0053(6) 0.0031(6) C15 0.0148(7) 0.0269(8) 0.0229(8) -0.0063(6) 0.0030(6) 0.0010(6) C16 0.0149(7) 0.0199(7) 0.0263(8) 0.0001(6) 0.0062(6) 0.0018(6) C17 0.0290(8) 0.0474(10) 0.0209(8) 0.0015(7) 0.0045(7) -0.0025(8) C21 0.0187(7) 0.0190(7) 0.0159(7) -0.0029(6) 0.0057(6) -0.0035(6) C22 0.0183(7) 0.0183(7) 0.0136(7) -0.0024(5) 0.0043(6) -0.0007(6) C23 0.0222(7) 0.0159(7) 0.0147(7) 0.0002(5) 0.0046(6) -0.0015(6) C24 0.0195(7) 0.0227(7) 0.0153(7) -0.0047(6) 0.0061(6) -0.0027(6) C25 0.0193(7) 0.0220(7) 0.0192(7) -0.0034(6) 0.0042(6) 0.0030(6) C26 0.0260(7) 0.0156(7) 0.0181(7) 0.0010(6) 0.0046(6) 0.0009(6) C27 0.0217(7) 0.0277(8) 0.0260(8) -0.0031(7) 0.0089(6) -0.0012(7) _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 O11 C11 1.374(2) . ? O11 H11A 0.920(3) . ? O21 C21 1.374(2) . ? O21 H21A 0.920(3) . ? N1 C2 1.481(2) . ? N1 C3 1.481(2) . ? N1 C1 1.487(2) . ? N2 C6 1.468(2) . ? N2 C5 1.469(2) . ? N2 C4 1.476(2) . ? C1 C12 1.504(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C22 1.512(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.528(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 C16 1.394(2) . ? C11 C12 1.400(2) . ? C12 C13 1.400(2) . ? C13 C14 1.392(2) . ? C13 H13 0.9500 . ? C14 C15 1.393(2) . ? C14 C17 1.515(2) . ? C15 C16 1.390(2) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C21 C26 1.387(2) . ? C21 C22 1.403(2) . ? C22 C23 1.393(2) . ? C23 C24 1.391(2) . ? C23 H23 0.9500 . ? C24 C25 1.398(2) . ? C24 C27 1.513(2) . ? C25 C26 1.387(2) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 O11 H11A 113.2(12) . . ? C21 O21 H21A 106.0(12) . . ? C2 N1 C3 112.36(10) . . ? C2 N1 C1 109.01(10) . . ? C3 N1 C1 111.72(10) . . ? C6 N2 C5 109.05(11) . . ? C6 N2 C4 111.69(12) . . ? C5 N2 C4 109.79(11) . . ? N1 C1 C12 112.16(11) . . ? N1 C1 H1A 109.2 . . ? C12 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C12 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? N1 C2 C22 112.65(11) . . ? N1 C2 H2A 109.1 . . ? C22 C2 H2A 109.1 . . ? N1 C2 H2B 109.1 . . ? C22 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? N1 C3 C4 111.36(11) . . ? N1 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? N1 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? N2 C4 C3 113.31(11) . . ? N2 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? N2 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O11 C11 C16 116.71(13) . . ? O11 C11 C12 123.20(12) . . ? C16 C11 C12 120.08(13) . . ? C13 C12 C11 118.24(12) . . ? C13 C12 C1 120.90(13) . . ? C11 C12 C1 120.80(12) . . ? C14 C13 C12 122.71(14) . . ? C14 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? C13 C14 C15 117.43(13) . . ? C13 C14 C17 120.70(14) . . ? C15 C14 C17 121.82(13) . . ? C16 C15 C14 121.55(13) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C15 C16 C11 119.99(14) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O21 C21 C26 118.48(12) . . ? O21 C21 C22 121.49(12) . . ? C26 C21 C22 120.02(13) . . ? C23 C22 C21 118.35(12) . . ? C23 C22 C2 120.32(12) . . ? C21 C22 C2 121.25(12) . . ? C24 C23 C22 122.66(13) . . ? C24 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C23 C24 C25 117.46(13) . . ? C23 C24 C27 120.73(13) . . ? C25 C24 C27 121.81(13) . . ? C26 C25 C24 121.26(13) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C21 120.24(13) . . ? C25 C26 H26 119.9 . . ? C21 C26 H26 119.9 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 C12 -77.96(13) . . . . ? C3 N1 C1 C12 157.26(11) . . . . ? C3 N1 C2 C22 -71.16(14) . . . . ? C1 N1 C2 C22 164.43(10) . . . . ? C2 N1 C3 C4 138.42(11) . . . . ? C1 N1 C3 C4 -98.69(13) . . . . ? C6 N2 C4 C3 77.09(14) . . . . ? C5 N2 C4 C3 -161.81(12) . . . . ? N1 C3 C4 N2 54.08(15) . . . . ? O11 C11 C12 C13 178.38(12) . . . . ? C16 C11 C12 C13 -0.48(19) . . . . ? O11 C11 C12 C1 1.04(19) . . . . ? C16 C11 C12 C1 -177.81(12) . . . . ? N1 C1 C12 C13 113.02(14) . . . . ? N1 C1 C12 C11 -69.71(16) . . . . ? C11 C12 C13 C14 0.22(19) . . . . ? C1 C12 C13 C14 177.56(12) . . . . ? C12 C13 C14 C15 0.1(2) . . . . ? C12 C13 C14 C17 -177.43(13) . . . . ? C13 C14 C15 C16 -0.27(19) . . . . ? C17 C14 C15 C16 177.28(13) . . . . ? C14 C15 C16 C11 0.0(2) . . . . ? O11 C11 C16 C15 -178.56(11) . . . . ? C12 C11 C16 C15 0.4(2) . . . . ? O21 C21 C22 C23 177.90(12) . . . . ? C26 C21 C22 C23 -1.14(19) . . . . ? O21 C21 C22 C2 1.28(19) . . . . ? C26 C21 C22 C2 -177.76(12) . . . . ? N1 C2 C22 C23 145.83(12) . . . . ? N1 C2 C22 C21 -37.62(17) . . . . ? C21 C22 C23 C24 0.08(19) . . . . ? C2 C22 C23 C24 176.72(12) . . . . ? C22 C23 C24 C25 0.80(19) . . . . ? C22 C23 C24 C27 -179.56(12) . . . . ? C23 C24 C25 C26 -0.64(19) . . . . ? C27 C24 C25 C26 179.73(12) . . . . ? C24 C25 C26 C21 -0.4(2) . . . . ? O21 C21 C26 C25 -177.76(12) . . . . ? C22 C21 C26 C25 1.31(19) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H11A N2 0.920(3) 1.898(8) 2.770(2) 157(2) . O21 H21A N1 0.920(3) 1.844(10) 2.683(2) 150(2) . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.260 _refine_diff_density_min -0.201 _refine_diff_density_rms 0.040