# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_2 _database_code_depnum_ccdc_archive 'CCDC 809471' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H16 Li4 N2 O10' _chemical_formula_sum 'C10 H16 Li4 N2 O10' _chemical_formula_weight 352.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.4358(5) _cell_length_b 8.4942(6) _cell_length_c 8.5389(6) _cell_angle_alpha 94.503(5) _cell_angle_beta 90.580(6) _cell_angle_gamma 104.865(5) _cell_volume 379.71(5) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max 28.33 _exptl_crystal_description columnar _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 182 _exptl_absorpt_coefficient_mu 0.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9679 _exptl_absorpt_correction_T_max 0.9806 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 4373 _diffrn_reflns_av_R_equivalents 0.0726 _diffrn_reflns_av_sigmaI/netI 0.0942 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 28.33 _reflns_number_total 1808 _reflns_number_gt 1085 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^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 1808 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0996 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1310 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 O1 O 0.1206(3) 0.43848(19) 0.62689(19) 0.0222(4) Uani 1 1 d . . . O2 O 0.5315(3) 0.4610(2) 0.6789(2) 0.0292(5) Uani 1 1 d . . . O3 O 0.1188(4) 1.0683(2) 0.7391(2) 0.0356(5) Uani 1 1 d . . . O4 O -0.0573(4) 0.8180(2) 0.62849(19) 0.0319(5) Uani 1 1 d . . . O5 O -0.3752(4) 0.1651(3) 0.5963(3) 0.0599(7) Uani 1 1 d . . . H5A H -0.4423 0.0965 0.6609 0.090 Uiso 1 1 d R . . H5B H -0.4402 0.1291 0.5054 0.090 Uiso 1 1 d R . . N1 N 0.0998(4) 0.6720(2) 0.8669(2) 0.0198(5) Uani 1 1 d . . . C1 C 0.3451(5) 0.6550(3) 0.8105(3) 0.0248(6) Uani 1 1 d . . . H1A H 0.4529 0.6507 0.9004 0.030 Uiso 1 1 calc R . . H1B H 0.4260 0.7517 0.7586 0.030 Uiso 1 1 calc R . . C2 C 0.1014(5) 0.8460(3) 0.8919(3) 0.0240(6) Uani 1 1 d . . . H2A H 0.2653 0.9075 0.9375 0.029 Uiso 1 1 calc R . . H2B H -0.0280 0.8577 0.9660 0.029 Uiso 1 1 calc R . . C3 C 0.0522(5) 0.9165(3) 0.7405(3) 0.0223(6) Uani 1 1 d . . . C4 C 0.0310(5) 0.5925(3) 1.0134(3) 0.0249(6) Uani 1 1 d . . . H4A H -0.1154 0.6240 1.0566 0.030 Uiso 1 1 calc R . . H4B H 0.1715 0.6302 1.0896 0.030 Uiso 1 1 calc R . . C5 C 0.3310(5) 0.5046(3) 0.6970(3) 0.0192(5) Uani 1 1 d . . . Li1 Li -0.1254(8) 0.5809(5) 0.6451(5) 0.0259(10) Uani 1 1 d . . . Li2 Li -0.0098(9) 0.1888(5) 0.5923(5) 0.0275(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0221(10) 0.0202(9) 0.0240(9) 0.0000(7) 0.0001(8) 0.0055(7) O2 0.0209(11) 0.0301(10) 0.0385(11) 0.0012(8) 0.0041(8) 0.0105(8) O3 0.0590(15) 0.0177(9) 0.0294(10) 0.0062(7) -0.0002(10) 0.0074(9) O4 0.0526(14) 0.0231(9) 0.0197(9) 0.0013(7) -0.0041(9) 0.0094(9) O5 0.0371(15) 0.0489(14) 0.0871(18) -0.0074(12) 0.0097(13) 0.0025(11) N1 0.0269(13) 0.0152(10) 0.0182(10) 0.0018(7) 0.0041(9) 0.0066(8) C1 0.0230(15) 0.0224(13) 0.0270(13) -0.0012(10) 0.0008(11) 0.0031(11) C2 0.0393(17) 0.0150(11) 0.0181(12) -0.0003(9) 0.0016(11) 0.0086(11) C3 0.0287(16) 0.0200(13) 0.0200(12) 0.0027(9) 0.0052(11) 0.0092(11) C4 0.0399(18) 0.0174(12) 0.0178(12) 0.0034(9) 0.0021(11) 0.0072(11) C5 0.0196(14) 0.0189(12) 0.0191(12) 0.0069(9) 0.0038(10) 0.0030(10) Li1 0.024(3) 0.024(2) 0.031(2) 0.0004(17) 0.0030(19) 0.0072(18) Li2 0.036(3) 0.024(2) 0.021(2) 0.0026(16) -0.0003(19) 0.0052(19) _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 C5 1.260(3) . ? O1 Li1 2.020(5) . ? O1 Li2 2.052(4) . ? O1 Li1 2.316(5) 2_566 ? O2 C5 1.245(3) . ? O2 Li1 1.919(5) 1_655 ? O3 C3 1.248(3) . ? O3 Li2 1.913(5) 1_565 ? O4 C3 1.256(3) . ? O4 Li2 1.923(5) 2_566 ? O4 Li1 1.968(4) . ? O5 Li2 1.945(5) . ? O5 H5A 0.8500 . ? O5 H5B 0.8500 . ? N1 C1 1.460(3) . ? N1 C2 1.474(3) . ? N1 C4 1.474(3) . ? N1 Li1 2.219(5) . ? C1 C5 1.527(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.516(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C4 C4 1.518(4) 2_567 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 Li1 2.760(5) . ? Li1 O2 1.919(5) 1_455 ? Li1 O1 2.316(5) 2_566 ? Li1 Li2 2.896(6) 2_566 ? Li1 Li1 3.222(9) 2_566 ? Li1 Li2 3.540(6) . ? Li2 O3 1.913(5) 1_545 ? Li2 O4 1.923(5) 2_566 ? Li2 Li1 2.896(6) 2_566 ? Li2 Li2 3.489(9) 2_556 ? 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 C5 O1 Li1 112.58(19) . . ? C5 O1 Li2 121.1(2) . . ? Li1 O1 Li2 120.8(2) . . ? C5 O1 Li1 115.83(18) . 2_566 ? Li1 O1 Li1 95.75(17) . 2_566 ? Li2 O1 Li1 82.83(16) . 2_566 ? C5 O2 Li1 132.1(2) . 1_655 ? C3 O3 Li2 124.5(2) . 1_565 ? C3 O4 Li2 130.5(2) . 2_566 ? C3 O4 Li1 120.1(2) . . ? Li2 O4 Li1 96.18(19) 2_566 . ? Li2 O5 H5A 110.1 . . ? Li2 O5 H5B 108.9 . . ? H5A O5 H5B 108.2 . . ? C1 N1 C2 110.51(19) . . ? C1 N1 C4 112.3(2) . . ? C2 N1 C4 109.47(19) . . ? C1 N1 Li1 97.45(18) . . ? C2 N1 Li1 105.17(17) . . ? C4 N1 Li1 121.15(18) . . ? N1 C1 C5 114.9(2) . . ? N1 C1 H1A 108.6 . . ? C5 C1 H1A 108.6 . . ? N1 C1 H1B 108.6 . . ? C5 C1 H1B 108.6 . . ? H1A C1 H1B 107.5 . . ? N1 C2 C3 112.33(19) . . ? N1 C2 H2A 109.1 . . ? C3 C2 H2A 109.1 . . ? N1 C2 H2B 109.1 . . ? C3 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? O3 C3 O4 125.5(2) . . ? O3 C3 C2 117.1(2) . . ? O4 C3 C2 117.4(2) . . ? N1 C4 C4 111.9(2) . 2_567 ? N1 C4 H4A 109.2 . . ? C4 C4 H4A 109.2 2_567 . ? N1 C4 H4B 109.2 . . ? C4 C4 H4B 109.2 2_567 . ? H4A C4 H4B 107.9 . . ? O2 C5 O1 125.8(2) . . ? O2 C5 C1 116.8(2) . . ? O1 C5 C1 117.4(2) . . ? O2 C5 Li1 163.6(2) . . ? O1 C5 Li1 42.50(14) . . ? C1 C5 Li1 75.88(17) . . ? O2 Li1 O4 118.2(2) 1_455 . ? O2 Li1 O1 113.2(2) 1_455 . ? O4 Li1 O1 128.6(2) . . ? O2 Li1 N1 113.1(2) 1_455 . ? O4 Li1 N1 80.24(16) . . ? O1 Li1 N1 81.19(17) . . ? O2 Li1 O1 101.03(19) 1_455 2_566 ? O4 Li1 O1 85.18(17) . 2_566 ? O1 Li1 O1 84.25(17) . 2_566 ? N1 Li1 O1 145.9(2) . 2_566 ? O2 Li1 C5 130.6(2) 1_455 . ? O4 Li1 C5 108.73(19) . . ? O1 Li1 C5 24.92(9) . . ? N1 Li1 C5 59.56(13) . . ? O1 Li1 C5 97.21(17) 2_566 . ? O2 Li1 Li2 123.5(2) 1_455 2_566 ? O4 Li1 Li2 41.31(13) . 2_566 ? O1 Li1 Li2 106.4(2) . 2_566 ? N1 Li1 Li2 111.39(18) . 2_566 ? O1 Li1 Li2 44.67(12) 2_566 2_566 ? C5 Li1 Li2 101.46(18) . 2_566 ? O2 Li1 Li1 112.6(2) 1_455 2_566 ? O4 Li1 Li1 109.3(2) . 2_566 ? O1 Li1 Li1 45.66(12) . 2_566 ? N1 Li1 Li1 119.9(2) . 2_566 ? O1 Li1 Li1 38.59(11) 2_566 2_566 ? C5 Li1 Li1 61.43(15) . 2_566 ? Li2 Li1 Li1 70.47(17) 2_566 2_566 ? O2 Li1 Li2 84.17(16) 1_455 . ? O4 Li1 Li2 156.3(2) . . ? O1 Li1 Li2 29.88(11) . . ? N1 Li1 Li2 98.96(17) . . ? O1 Li1 Li2 82.56(14) 2_566 . ? C5 Li1 Li2 53.28(11) . . ? Li2 Li1 Li2 120.93(16) 2_566 . ? Li1 Li1 Li2 50.46(14) 2_566 . ? O3 Li2 O4 124.4(3) 1_545 2_566 ? O3 Li2 O5 115.1(2) 1_545 . ? O4 Li2 O5 103.2(2) 2_566 . ? O3 Li2 O1 115.6(2) 1_545 . ? O4 Li2 O1 94.08(18) 2_566 . ? O5 Li2 O1 100.2(2) . . ? O3 Li2 Li1 145.0(3) 1_545 2_566 ? O4 Li2 Li1 42.51(12) 2_566 2_566 ? O5 Li2 Li1 99.9(2) . 2_566 ? O1 Li2 Li1 52.50(13) . 2_566 ? O3 Li2 Li2 70.89(17) 1_545 2_556 ? O4 Li2 Li2 63.21(15) 2_566 2_556 ? O5 Li2 Li2 101.0(2) . 2_556 ? O1 Li2 Li2 151.9(3) . 2_556 ? Li1 Li2 Li2 105.5(2) 2_566 2_556 ? O3 Li2 Li1 129.78(19) 1_545 . ? O4 Li2 Li1 99.39(17) 2_566 . ? O5 Li2 Li1 70.83(16) . . ? O1 Li2 Li1 29.36(12) . . ? Li1 Li2 Li1 59.07(16) 2_566 . ? Li2 Li2 Li1 159.3(2) 2_556 . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.458 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.078 data_3 _database_code_depnum_ccdc_archive 'CCDC 809472' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H7 Li2 O6' _chemical_formula_weight 164.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.13440(10) _cell_length_b 7.7339(2) _cell_length_c 9.3901(2) _cell_angle_alpha 107.1380(10) _cell_angle_beta 98.0990(10) _cell_angle_gamma 93.3740(10) _cell_volume 350.770(14) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4159 _cell_measurement_theta_min 2.3016 _cell_measurement_theta_max 28.2855 _exptl_crystal_description lamellar _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 170 _exptl_absorpt_coefficient_mu 0.143 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9721 _exptl_absorpt_correction_T_max 0.9831 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 6283 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 28.32 _reflns_number_total 1743 _reflns_number_gt 1506 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+0.1770P] 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 1743 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 0.823 _refine_ls_restrained_S_all 0.823 _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 C1 C 0.2510(2) -0.09234(14) 0.69041(12) 0.0170(2) Uani 1 1 d . . . C2 C 0.0614(2) -0.26326(15) 0.65119(12) 0.0216(2) Uani 1 1 d . . . H2A H -0.1173 -0.2286 0.6477 0.026 Uiso 1 1 calc R . . H2B H 0.0941 -0.3169 0.7324 0.026 Uiso 1 1 calc R . . C3 C 0.0750(2) -0.40936(13) 0.50237(11) 0.0153(2) Uani 1 1 d . . . H3A H 0.2607 -0.4274 0.4953 0.018 Uiso 1 1 calc R . . C4 C -0.0474(2) -0.34905(13) 0.36828(11) 0.0162(2) Uani 1 1 d . . . O1 O -0.23853(18) 0.16504(14) 0.96603(10) 0.0339(2) Uani 1 1 d . . . H1A H -0.3951 0.1199 0.9111 0.051 Uiso 1 1 d . . . H1B H -0.2191 0.1085 1.0304 0.051 Uiso 1 1 d . . . O2 O 0.3010(2) 0.39258(15) 1.06206(12) 0.0430(3) Uani 1 1 d . . . H2C H 0.2697 0.4739 1.1344 0.065 Uiso 1 1 d . . . H2D H 0.4606 0.3890 1.0674 0.065 Uiso 1 1 d . . . O3 O 0.10635(15) -0.31078(11) 0.28412(9) 0.02180(19) Uani 1 1 d . . . O4 O 0.39249(18) -0.06840(11) 0.59865(9) 0.0273(2) Uani 1 1 d . . . O5 O -0.28974(16) -0.34124(12) 0.34727(10) 0.0279(2) Uani 1 1 d . . . O6 O 0.25756(16) 0.02025(10) 0.81978(8) 0.02124(19) Uani 1 1 d . . . Li2 Li 0.4520(4) -0.1786(3) 0.3909(2) 0.0220(4) Uani 1 1 d . . . Li1 Li 0.0650(4) 0.2323(3) 0.8859(2) 0.0242(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0209(5) 0.0146(4) 0.0146(5) 0.0044(4) 0.0015(4) -0.0002(4) C2 0.0286(6) 0.0189(5) 0.0151(5) 0.0022(4) 0.0066(4) -0.0064(4) C3 0.0165(5) 0.0152(5) 0.0136(5) 0.0047(4) 0.0022(4) -0.0027(4) C4 0.0192(5) 0.0129(4) 0.0155(5) 0.0035(4) 0.0022(4) -0.0001(4) O1 0.0266(5) 0.0501(6) 0.0284(5) 0.0214(4) 0.0004(4) -0.0070(4) O2 0.0319(5) 0.0449(6) 0.0360(6) -0.0098(5) 0.0030(4) -0.0027(4) O3 0.0210(4) 0.0290(4) 0.0178(4) 0.0114(3) 0.0036(3) -0.0013(3) O4 0.0366(5) 0.0220(4) 0.0215(4) 0.0028(3) 0.0119(4) -0.0090(3) O5 0.0181(4) 0.0347(5) 0.0358(5) 0.0173(4) 0.0049(3) 0.0059(3) O6 0.0280(4) 0.0177(4) 0.0151(4) 0.0014(3) 0.0031(3) -0.0005(3) Li2 0.0211(9) 0.0216(9) 0.0218(9) 0.0046(7) 0.0046(7) -0.0015(7) Li1 0.0244(10) 0.0265(10) 0.0213(9) 0.0077(8) 0.0023(7) 0.0017(8) _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 O4 1.2486(13) . ? C1 O6 1.2636(13) . ? C1 C2 1.5136(14) . ? C2 C3 1.5299(14) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.5347(14) . ? C3 C3 1.5450(19) 2_546 ? C3 H3A 0.9800 . ? C4 O5 1.2402(13) . ? C4 O3 1.2732(13) . ? C4 Li2 2.764(2) . ? C4 Li1 2.782(2) 2_556 ? O1 Li1 1.931(2) . ? O1 H1A 0.8823 . ? O1 H1B 0.8431 . ? O2 Li1 1.947(2) . ? O2 H2C 0.8207 . ? O2 H2D 0.8165 . ? O3 Li2 1.970(2) . ? O3 Li1 1.983(2) 2_556 ? O4 Li2 1.961(2) . ? O4 Li2 1.996(2) 2_656 ? O5 Li2 1.885(2) 1_455 ? O6 Li1 1.953(2) . ? Li2 O5 1.885(2) 1_655 ? Li2 O4 1.996(2) 2_656 ? Li2 Li2 2.880(4) 2_656 ? Li2 Li1 3.357(3) 2_556 ? Li1 O3 1.983(2) 2_556 ? Li1 C4 2.782(2) 2_556 ? Li1 Li2 3.357(3) 2_556 ? 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 O4 C1 O6 123.21(10) . . ? O4 C1 C2 120.65(9) . . ? O6 C1 C2 116.14(9) . . ? C1 C2 C3 116.30(9) . . ? C1 C2 H2A 108.2 . . ? C3 C2 H2A 108.2 . . ? C1 C2 H2B 108.2 . . ? C3 C2 H2B 108.2 . . ? H2A C2 H2B 107.4 . . ? C2 C3 C4 110.09(8) . . ? C2 C3 C3 109.88(10) . 2_546 ? C4 C3 C3 109.70(10) . 2_546 ? C2 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? C3 C3 H3A 109.0 2_546 . ? O5 C4 O3 123.64(10) . . ? O5 C4 C3 118.43(9) . . ? O3 C4 C3 117.93(9) . . ? O5 C4 Li2 147.29(8) . . ? O3 C4 Li2 40.14(6) . . ? C3 C4 Li2 85.25(7) . . ? O5 C4 Li1 83.69(8) . 2_556 ? O3 C4 Li1 39.95(6) . 2_556 ? C3 C4 Li1 157.88(8) . 2_556 ? Li2 C4 Li1 74.48(6) . 2_556 ? Li1 O1 H1A 124.3 . . ? Li1 O1 H1B 119.5 . . ? H1A O1 H1B 104.6 . . ? Li1 O2 H2C 130.7 . . ? Li1 O2 H2D 119.4 . . ? H2C O2 H2D 109.8 . . ? C4 O3 Li2 115.23(9) . . ? C4 O3 Li1 115.70(9) . 2_556 ? Li2 O3 Li1 116.25(9) . 2_556 ? C1 O4 Li2 141.09(9) . . ? C1 O4 Li2 122.12(9) . 2_656 ? Li2 O4 Li2 93.41(8) . 2_656 ? C4 O5 Li2 142.03(10) . 1_455 ? C1 O6 Li1 130.91(9) . . ? O5 Li2 O4 121.33(11) 1_655 . ? O5 Li2 O3 107.54(10) 1_655 . ? O4 Li2 O3 103.93(9) . . ? O5 Li2 O4 108.27(10) 1_655 2_656 ? O4 Li2 O4 86.59(8) . 2_656 ? O3 Li2 O4 129.26(11) . 2_656 ? O5 Li2 C4 113.63(9) 1_655 . ? O4 Li2 C4 80.90(7) . . ? O3 Li2 C4 24.63(4) . . ? O4 Li2 C4 136.74(9) 2_656 . ? O5 Li2 Li2 124.84(12) 1_655 2_656 ? O4 Li2 Li2 43.78(6) . 2_656 ? O3 Li2 Li2 127.06(12) . 2_656 ? O4 Li2 Li2 42.81(6) 2_656 2_656 ? C4 Li2 Li2 113.40(10) . 2_656 ? O5 Li2 Li1 116.06(9) 1_655 2_556 ? O4 Li2 Li1 116.90(9) . 2_556 ? O3 Li2 Li1 31.99(5) . 2_556 ? O4 Li2 Li1 98.97(8) 2_656 2_556 ? C4 Li2 Li1 53.01(5) . 2_556 ? Li2 Li2 Li1 114.59(10) 2_656 2_556 ? O2 Li1 O1 104.24(10) . . ? O2 Li1 O6 103.94(10) . . ? O1 Li1 O6 109.32(10) . . ? O2 Li1 O3 124.17(11) . 2_556 ? O1 Li1 O3 101.34(10) . 2_556 ? O6 Li1 O3 112.93(10) . 2_556 ? O2 Li1 C4 113.21(9) . 2_556 ? O1 Li1 C4 125.54(10) . 2_556 ? O6 Li1 C4 98.60(8) . 2_556 ? O3 Li1 C4 24.35(4) 2_556 2_556 ? O2 Li1 Li2 148.84(10) . 2_556 ? O1 Li1 Li2 74.95(7) . 2_556 ? O6 Li1 Li2 105.61(9) . 2_556 ? O3 Li1 Li2 31.76(5) 2_556 2_556 ? C4 Li1 Li2 52.51(5) 2_556 2_556 ? 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 O1 H1A O6 0.88 1.88 2.7542(12) 171.8 1_455 O1 H1B O6 0.84 1.97 2.8010(11) 167.4 2_557 O2 H2C O3 0.82 2.14 2.9407(13) 166.0 1_566 O2 H2D O1 0.82 2.46 3.1072(15) 137.0 1_655 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.368 _refine_diff_density_min -0.184 _refine_diff_density_rms 0.043 data_4 _database_code_depnum_ccdc_archive 'CCDC 809473' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H13 Li N O5' _chemical_formula_weight 186.11 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' 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 5.4998(2) _cell_length_b 10.6053(4) _cell_length_c 15.2719(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.942(2) _cell_angle_gamma 90.00 _cell_volume 877.39(6) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 6276 _cell_measurement_theta_min 2.3497 _cell_measurement_theta_max 28.3403 _exptl_crystal_description columnar _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 0.119 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6740 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 13945 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 28.35 _reflns_number_total 2183 _reflns_number_gt 1717 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+0.2190P] 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 2183 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1167 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 O1 O -0.00605(17) 0.69185(10) 0.40065(7) 0.0325(3) Uani 1 1 d . . . O3 O -0.28086(19) 0.93004(10) 0.32473(7) 0.0346(3) Uani 1 1 d . . . O2 O 0.39460(18) 0.70151(11) 0.39881(8) 0.0352(3) Uani 1 1 d . . . C3 C -0.0189(2) 0.94353(12) 0.46775(8) 0.0200(3) Uani 1 1 d . . . H3A H -0.1449 0.8876 0.4847 0.024 Uiso 1 1 calc R . . N1S N 0.0996(2) 0.45128(12) 0.34075(8) 0.0314(3) Uani 1 1 d . . . H1SA H 0.0654 0.5319 0.3524 0.038 Uiso 1 1 calc R . . H1SE H 0.1741 0.4508 0.2927 0.038 Uiso 1 1 calc R . . C1 C 0.2010(2) 0.74583(13) 0.41869(9) 0.0217(3) Uani 1 1 d . . . C4 C -0.1046(2) 0.98847(13) 0.37198(9) 0.0229(3) Uani 1 1 d . . . O1W O -0.4021(2) 0.66386(12) 0.22779(8) 0.0448(3) Uani 1 1 d . . . H1WA H -0.4918 0.5993 0.2308 0.067 Uiso 1 1 d R . . H1WB H -0.2666 0.6419 0.2127 0.067 Uiso 1 1 d R . . O4 O 0.0041(2) 1.07828(11) 0.34376(8) 0.0431(3) Uani 1 1 d . . . C2 C 0.2216(2) 0.86872(14) 0.47059(9) 0.0262(3) Uani 1 1 d . . . H2A H 0.3398 0.9224 0.4481 0.031 Uiso 1 1 calc R . . H2B H 0.2885 0.8501 0.5322 0.031 Uiso 1 1 calc R . . C2S C 0.2709(4) 0.39917(19) 0.41739(11) 0.0461(4) Uani 1 1 d . . . H2SA H 0.4187 0.4490 0.4280 0.069 Uiso 1 1 calc R . . H2SB H 0.3116 0.3138 0.4048 0.069 Uiso 1 1 calc R . . H2SC H 0.1937 0.4008 0.4692 0.069 Uiso 1 1 calc R . . C1S C -0.1333(3) 0.38007(19) 0.32025(14) 0.0511(5) Uani 1 1 d . . . H1SB H -0.2372 0.4176 0.2700 0.077 Uiso 1 1 calc R . . H1SC H -0.2159 0.3820 0.3707 0.077 Uiso 1 1 calc R . . H1SD H -0.0984 0.2943 0.3066 0.077 Uiso 1 1 calc R . . Li1 Li -0.3342(4) 0.7487(2) 0.34509(17) 0.0302(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0214(5) 0.0274(6) 0.0477(7) -0.0097(5) 0.0034(4) -0.0005(4) O3 0.0361(5) 0.0393(7) 0.0250(5) 0.0013(5) -0.0048(4) -0.0058(5) O2 0.0268(5) 0.0316(6) 0.0507(7) -0.0062(5) 0.0167(5) 0.0021(4) C3 0.0218(6) 0.0186(6) 0.0193(6) -0.0012(5) 0.0028(5) 0.0008(5) N1S 0.0432(7) 0.0259(7) 0.0256(6) -0.0004(5) 0.0071(5) -0.0017(5) C1 0.0222(6) 0.0216(7) 0.0212(6) 0.0020(5) 0.0038(5) 0.0023(5) C4 0.0286(6) 0.0205(7) 0.0201(6) -0.0010(5) 0.0052(5) 0.0043(5) O1W 0.0393(6) 0.0512(8) 0.0447(7) -0.0142(6) 0.0095(5) -0.0098(5) O4 0.0676(8) 0.0333(6) 0.0295(6) 0.0036(5) 0.0112(5) -0.0161(6) C2 0.0211(6) 0.0255(7) 0.0308(7) -0.0045(6) 0.0014(5) 0.0021(5) C2S 0.0563(10) 0.0441(10) 0.0346(9) 0.0017(8) -0.0015(8) 0.0069(8) C1S 0.0419(9) 0.0426(11) 0.0667(13) 0.0073(9) 0.0036(9) -0.0053(8) Li1 0.0233(11) 0.0339(14) 0.0336(13) -0.0017(11) 0.0054(10) 0.0003(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.2617(16) . ? O1 Li1 1.953(3) . ? O3 C4 1.2661(17) . ? O3 Li1 1.978(3) . ? O2 C1 1.2485(15) . ? O2 Li1 1.890(3) 1_655 ? C3 C4 1.5330(18) . ? C3 C2 1.5367(17) . ? C3 C3 1.542(2) 3_576 ? C3 H3A 0.9800 . ? N1S C1S 1.473(2) . ? N1S C2S 1.477(2) . ? N1S H1SA 0.9000 . ? N1S H1SE 0.9000 . ? C1 C2 1.5194(19) . ? C4 O4 1.2406(18) . ? O1W Li1 1.982(3) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2S H2SA 0.9600 . ? C2S H2SB 0.9600 . ? C2S H2SC 0.9600 . ? C1S H1SB 0.9600 . ? C1S H1SC 0.9600 . ? C1S H1SD 0.9600 . ? Li1 O2 1.890(3) 1_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 Li1 133.35(12) . . ? C4 O3 Li1 120.40(12) . . ? C1 O2 Li1 140.90(13) . 1_655 ? C4 C3 C2 107.99(10) . . ? C4 C3 C3 110.69(13) . 3_576 ? C2 C3 C3 111.26(13) . 3_576 ? C4 C3 H3A 108.9 . . ? C2 C3 H3A 108.9 . . ? C3 C3 H3A 108.9 3_576 . ? C1S N1S C2S 112.88(14) . . ? C1S N1S H1SA 109.0 . . ? C2S N1S H1SA 109.0 . . ? C1S N1S H1SE 109.0 . . ? C2S N1S H1SE 109.0 . . ? H1SA N1S H1SE 107.8 . . ? O2 C1 O1 123.47(13) . . ? O2 C1 C2 117.37(11) . . ? O1 C1 C2 119.11(11) . . ? O4 C4 O3 123.03(13) . . ? O4 C4 C3 118.87(12) . . ? O3 C4 C3 118.08(12) . . ? Li1 O1W H1WA 109.7 . . ? Li1 O1W H1WB 109.4 . . ? H1WA O1W H1WB 109.8 . . ? C1 C2 C3 116.21(11) . . ? C1 C2 H2A 108.2 . . ? C3 C2 H2A 108.2 . . ? C1 C2 H2B 108.2 . . ? C3 C2 H2B 108.2 . . ? H2A C2 H2B 107.4 . . ? N1S C2S H2SA 109.5 . . ? N1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? N1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? N1S C1S H1SB 109.5 . . ? N1S C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? N1S C1S H1SD 109.5 . . ? H1SB C1S H1SD 109.5 . . ? H1SC C1S H1SD 109.5 . . ? O2 Li1 O1 117.98(14) 1_455 . ? O2 Li1 O3 118.40(13) 1_455 . ? O1 Li1 O3 102.56(12) . . ? O2 Li1 O1W 103.43(12) 1_455 . ? O1 Li1 O1W 105.56(12) . . ? O3 Li1 O1W 108.02(13) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.286 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.043