# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email shangao67@yahoo.com _publ_contact_author_name 'Shan Gao' loop_ _publ_author_name 'Wang Wan' 'Zhi-Biao Zhu' 'Li-Hua Huo' 'Zhao-Peng Deng' 'Hui Zhao' 'Shan Gao' data_d _database_code_depnum_ccdc_archive 'CCDC 852885' #TrackingRef 'complex 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C3 H6 Li O6 S' _chemical_formula_sum 'C3 H6 Li O6 S' _chemical_formula_weight 177.08 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' S S 0.1246 0.1234 '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 6.3752(13) _cell_length_b 7.1912(14) _cell_length_c 8.2477(16) _cell_angle_alpha 73.61(3) _cell_angle_beta 68.38(3) _cell_angle_gamma 66.73(3) _cell_volume 318.76(14) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2607 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 27.44 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.845 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 182 _exptl_absorpt_coefficient_mu 0.482 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9183 _exptl_absorpt_correction_T_max 0.9489 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3159 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.45 _reflns_number_total 1447 _reflns_number_gt 1172 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0273P)^2^+0.6099P] 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 1447 _refine_ls_number_parameters 115 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0927 _refine_ls_wR_factor_gt 0.0697 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.8027(8) 0.1840(7) 0.9030(6) 0.0300(9) Uani 1 1 d . . . S1 S 0.86824(10) 0.22724(9) 1.25495(7) 0.01823(16) Uani 1 1 d . . . O1 O 0.7985(3) 0.3235(3) 1.0925(2) 0.0232(4) Uani 1 1 d . . . O1W O 0.8137(4) 0.4153(4) 0.7049(3) 0.0379(5) Uani 1 1 d D . . H1W1 H 0.832(6) 0.398(6) 0.602(2) 0.057 Uiso 1 1 d D . . H1W2 H 0.901(6) 0.483(5) 0.698(4) 0.057 Uiso 1 1 d D . . O2 O 1.0998(3) 0.0674(3) 1.2211(2) 0.0245(4) Uani 1 1 d . . . O2W O 0.4355(3) 0.2589(3) 0.9635(2) 0.0256(4) Uani 1 1 d D . . H2W1 H 0.377(5) 0.3881(16) 0.940(4) 0.038 Uiso 1 1 d D . . H2W2 H 0.365(5) 0.216(4) 1.068(2) 0.038 Uiso 1 1 d D . . O3 O 0.8526(3) 0.3772(3) 1.3492(2) 0.0284(4) Uani 1 1 d . . . O4 O 0.2268(3) 0.0886(3) 1.8351(2) 0.0249(4) Uani 1 1 d D . . H4O H 0.283(5) 0.158(4) 1.866(4) 0.037 Uiso 1 1 d D . . C1 C 0.6585(4) 0.1028(3) 1.3936(3) 0.0178(4) Uani 1 1 d . . . C2 C 0.5238(4) 0.1509(3) 1.5603(3) 0.0190(5) Uani 1 1 d . . . H2 H 0.5399 0.2521 1.5999 0.023 Uiso 1 1 calc R . . C3 C 0.3641(4) 0.0480(4) 1.6688(3) 0.0178(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 Li1 0.030(2) 0.029(2) 0.032(2) -0.0082(18) -0.0090(19) -0.0077(18) S1 0.0194(3) 0.0219(3) 0.0152(3) -0.0043(2) -0.0011(2) -0.0111(2) O1 0.0280(9) 0.0232(8) 0.0181(8) -0.0036(6) -0.0057(7) -0.0087(7) O1W 0.0441(12) 0.0491(13) 0.0275(10) 0.0018(9) -0.0101(9) -0.0280(10) O2 0.0169(8) 0.0279(9) 0.0260(9) -0.0032(7) -0.0038(7) -0.0075(7) O2W 0.0270(9) 0.0225(9) 0.0261(9) -0.0028(7) -0.0046(7) -0.0103(7) O3 0.0373(10) 0.0339(10) 0.0221(9) -0.0091(7) -0.0013(8) -0.0236(8) O4 0.0282(9) 0.0332(10) 0.0178(8) -0.0132(7) 0.0030(7) -0.0171(8) C1 0.0168(10) 0.0216(11) 0.0153(10) -0.0026(8) -0.0027(8) -0.0086(9) C2 0.0209(11) 0.0187(11) 0.0209(11) -0.0065(9) -0.0040(9) -0.0096(9) C3 0.0179(11) 0.0236(11) 0.0123(10) -0.0066(8) -0.0015(8) -0.0072(9) _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 O1W 1.979(5) . ? Li1 O1 2.070(5) . ? Li1 O2W 2.077(5) . ? Li1 O2 2.095(5) 2_757 ? Li1 O4 2.394(5) 1_654 ? Li1 O4 2.479(5) 2_658 ? Li1 Li1 3.348(9) 2_757 ? S1 O3 1.4518(18) . ? S1 O2 1.4545(19) . ? S1 O1 1.4640(18) . ? S1 C1 1.771(2) . ? O1W H1W1 0.85(3) . ? O1W H1W2 0.85(3) . ? O2 Li1 2.095(5) 2_757 ? O2W H2W1 0.85(3) . ? O2W H2W2 0.84(3) . ? O4 C3 1.369(3) . ? O4 Li1 2.394(5) 1_456 ? O4 Li1 2.479(5) 2_658 ? O4 H4O 0.85(3) . ? C1 C2 1.382(3) . ? C1 C3 1.398(3) 2_658 ? C2 C3 1.391(3) . ? C2 H2 0.9300 . ? C3 C1 1.398(3) 2_658 ? 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 O1W Li1 O1 97.7(2) . . ? O1W Li1 O2W 92.8(2) . . ? O1 Li1 O2W 97.0(2) . . ? O1W Li1 O2 103.7(2) . 2_757 ? O1 Li1 O2 153.6(3) . 2_757 ? O2W Li1 O2 97.2(2) . 2_757 ? O1W Li1 O4 88.39(19) . 1_654 ? O1 Li1 O4 83.69(17) . 1_654 ? O2W Li1 O4 178.5(2) . 1_654 ? O2 Li1 O4 81.63(17) 2_757 1_654 ? O1W Li1 O4 176.1(2) . 2_658 ? O1 Li1 O4 78.99(16) . 2_658 ? O2W Li1 O4 85.66(18) . 2_658 ? O2 Li1 O4 80.04(16) 2_757 2_658 ? O4 Li1 O4 93.22(17) 1_654 2_658 ? O1W Li1 Li1 135.9(3) . 2_757 ? O1 Li1 Li1 77.30(19) . 2_757 ? O2W Li1 Li1 131.2(3) . 2_757 ? O2 Li1 Li1 76.58(18) 2_757 2_757 ? O4 Li1 Li1 47.67(13) 1_654 2_757 ? O4 Li1 Li1 45.55(12) 2_658 2_757 ? O3 S1 O2 113.24(11) . . ? O3 S1 O1 112.15(11) . . ? O2 S1 O1 111.35(11) . . ? O3 S1 C1 106.97(11) . . ? O2 S1 C1 106.25(11) . . ? O1 S1 C1 106.36(11) . . ? S1 O1 Li1 128.54(16) . . ? Li1 O1W H1W1 119(2) . . ? Li1 O1W H1W2 116(2) . . ? H1W1 O1W H1W2 109.6(16) . . ? S1 O2 Li1 126.17(17) . 2_757 ? Li1 O2W H2W1 108(2) . . ? Li1 O2W H2W2 116(2) . . ? H2W1 O2W H2W2 110.6(16) . . ? C3 O4 Li1 118.27(18) . 1_456 ? C3 O4 Li1 122.83(18) . 2_658 ? Li1 O4 Li1 86.78(17) 1_456 2_658 ? C3 O4 H4O 108(2) . . ? Li1 O4 H4O 119(2) 1_456 . ? Li1 O4 H4O 101(2) 2_658 . ? C2 C1 C3 120.8(2) . 2_658 ? C2 C1 S1 120.90(17) . . ? C3 C1 S1 118.25(17) 2_658 . ? C1 C2 C3 120.0(2) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? O4 C3 C2 122.6(2) . . ? O4 C3 C1 118.3(2) . 2_658 ? C2 C3 C1 119.1(2) . 2_658 ? 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 O3 S1 O1 Li1 176.8(2) . . . . ? O2 S1 O1 Li1 48.7(2) . . . . ? C1 S1 O1 Li1 -66.6(2) . . . . ? O1W Li1 O1 S1 -157.77(15) . . . . ? O2W Li1 O1 S1 108.4(2) . . . . ? O2 Li1 O1 S1 -13.8(7) 2_757 . . . ? O4 Li1 O1 S1 -70.3(2) 1_654 . . . ? O4 Li1 O1 S1 24.3(2) 2_658 . . . ? Li1 Li1 O1 S1 -22.3(3) 2_757 . . . ? O3 S1 O2 Li1 177.87(19) . . . 2_757 ? O1 S1 O2 Li1 -54.7(2) . . . 2_757 ? C1 S1 O2 Li1 60.7(2) . . . 2_757 ? O3 S1 C1 C2 -2.1(2) . . . . ? O2 S1 C1 C2 119.1(2) . . . . ? O1 S1 C1 C2 -122.16(19) . . . . ? O3 S1 C1 C3 179.02(18) . . . 2_658 ? O2 S1 C1 C3 -59.7(2) . . . 2_658 ? O1 S1 C1 C3 59.0(2) . . . 2_658 ? C3 C1 C2 C3 0.4(4) 2_658 . . . ? S1 C1 C2 C3 -178.46(18) . . . . ? Li1 O4 C3 C2 123.6(2) 1_456 . . . ? Li1 O4 C3 C2 -130.7(2) 2_658 . . . ? Li1 O4 C3 C1 -56.3(3) 1_456 . . 2_658 ? Li1 O4 C3 C1 49.4(3) 2_658 . . 2_658 ? C1 C2 C3 O4 179.8(2) . . . . ? C1 C2 C3 C1 -0.4(4) . . . 2_658 ? 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 O1W H1W1 O3 0.85(3) 2.09(3) 2.934(3) 175(4) 1_554 O1W H1W2 O3 0.85(3) 2.05(3) 2.895(3) 172(3) 2_767 O2W H2W1 O1 0.85(3) 1.92(3) 2.764(3) 172(3) 2_667 O2W H2W2 O2 0.84(3) 2.16(2) 2.883(3) 143(3) 1_455 O4 H4O O2W 0.85(3) 1.89(3) 2.730(3) 168(3) 1_556 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.509 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.097 # Attachment 'complex 2.cif' data_z _database_code_depnum_ccdc_archive 'CCDC 852886' #TrackingRef 'complex 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C3 H4 Li O5 S' _chemical_formula_sum 'C3 H4 Li O5 S' _chemical_formula_weight 159.06 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' S S 0.1246 0.1234 '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 4.8192(10) _cell_length_b 7.1534(14) _cell_length_c 8.3947(17) _cell_angle_alpha 92.21(3) _cell_angle_beta 93.66(3) _cell_angle_gamma 101.87(3) _cell_volume 282.23(10) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2050 _cell_measurement_theta_min 3.70 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.872 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 162 _exptl_absorpt_coefficient_mu 0.520 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9077 _exptl_absorpt_correction_T_max 0.9402 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2781 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1281 _reflns_number_gt 1133 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0658P)^2^+0.3403P] 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 1281 _refine_ls_number_parameters 100 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1252 _refine_ls_wR_factor_gt 0.1095 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.1807(10) 0.3528(7) 0.9772(6) 0.0296(10) Uani 1 1 d . . . S1 S 0.31793(12) 0.73023(8) 0.78786(7) 0.0193(2) Uani 1 1 d . . . O1 O 0.1033(4) 0.5958(3) 0.8643(2) 0.0248(4) Uani 1 1 d . . . O1W O -0.0926(4) 0.1421(3) 0.8468(2) 0.0266(4) Uani 1 1 d D . . H1W1 H -0.213(5) 0.048(3) 0.877(4) 0.040 Uiso 1 1 d D . . H1W2 H 0.017(6) 0.101(4) 0.785(3) 0.040 Uiso 1 1 d D . . O2 O 0.5738(4) 0.7904(3) 0.8963(2) 0.0245(4) Uani 1 1 d . . . O3 O 0.2173(4) 0.8884(3) 0.7211(2) 0.0293(5) Uani 1 1 d . . . O4 O 0.5091(4) 0.3671(3) 0.8046(2) 0.0252(4) Uani 1 1 d D . . H4O H 0.621(6) 0.290(4) 0.805(4) 0.038 Uiso 1 1 d D . . C1 C 0.5074(5) 0.4302(4) 0.6528(3) 0.0195(5) Uani 1 1 d . . . C2 C 0.4159(5) 0.5996(4) 0.6251(3) 0.0195(5) Uani 1 1 d . . . C3 C 0.4077(5) 0.6693(4) 0.4740(3) 0.0219(5) Uani 1 1 d . . . H3 H 0.3456 0.7823 0.4574 0.026 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 Li1 0.029(2) 0.028(2) 0.032(2) 0.0013(19) 0.005(2) 0.0069(19) S1 0.0237(4) 0.0175(3) 0.0178(3) -0.0006(2) 0.0054(2) 0.0060(2) O1 0.0249(9) 0.0247(9) 0.0251(9) -0.0003(7) 0.0090(7) 0.0037(7) O1W 0.0271(10) 0.0197(9) 0.0336(11) 0.0001(8) 0.0071(8) 0.0052(8) O2 0.0270(10) 0.0217(9) 0.0231(9) -0.0005(7) 0.0000(8) 0.0019(7) O3 0.0415(11) 0.0261(10) 0.0258(10) 0.0031(8) 0.0090(8) 0.0177(9) O4 0.0333(10) 0.0282(10) 0.0186(9) 0.0064(7) 0.0082(8) 0.0143(8) C1 0.0212(11) 0.0212(12) 0.0178(11) 0.0038(9) 0.0037(9) 0.0071(9) C2 0.0217(11) 0.0198(12) 0.0178(11) -0.0013(9) 0.0055(9) 0.0054(9) C3 0.0257(12) 0.0216(12) 0.0214(12) 0.0029(9) 0.0056(10) 0.0106(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 Li1 O2 2.000(5) 2_667 ? Li1 O1W 2.019(5) . ? Li1 O1 2.045(5) 2_567 ? Li1 O1 2.099(5) . ? Li1 O4 2.203(5) . ? Li1 Li1 3.024(9) 2_567 ? Li1 Li1 3.343(10) 2_667 ? S1 O3 1.4383(19) . ? S1 O1 1.4593(19) . ? S1 O2 1.464(2) . ? S1 C2 1.769(2) . ? O1 Li1 2.045(5) 2_567 ? O1W H1W1 0.85(3) . ? O1W H1W2 0.85(3) . ? O2 Li1 2.000(5) 2_667 ? O4 C1 1.368(3) . ? O4 H4O 0.85(3) . ? C1 C3 1.387(3) 2_666 ? C1 C2 1.394(3) . ? C2 C3 1.382(3) . ? C3 C1 1.387(3) 2_666 ? C3 H3 0.9300 . ? 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 O2 Li1 O1W 102.8(2) 2_667 . ? O2 Li1 O1 103.2(2) 2_667 2_567 ? O1W Li1 O1 95.9(2) . 2_567 ? O2 Li1 O1 153.0(3) 2_667 . ? O1W Li1 O1 101.2(2) . . ? O1 Li1 O1 86.27(19) 2_567 . ? O2 Li1 O4 83.76(18) 2_667 . ? O1W Li1 O4 92.9(2) . . ? O1 Li1 O4 167.3(3) 2_567 . ? O1 Li1 O4 82.99(19) . . ? O2 Li1 Li1 140.6(3) 2_667 2_567 ? O1W Li1 Li1 101.8(3) . 2_567 ? O1 Li1 Li1 43.84(14) 2_567 2_567 ? O1 Li1 Li1 42.44(13) . 2_567 ? O4 Li1 Li1 125.1(3) . 2_567 ? O2 Li1 Li1 75.1(2) 2_667 2_667 ? O1W Li1 Li1 148.6(3) . 2_667 ? O1 Li1 Li1 115.2(3) 2_567 2_667 ? O1 Li1 Li1 78.0(2) . 2_667 ? O4 Li1 Li1 55.76(15) . 2_667 ? Li1 Li1 Li1 98.3(3) 2_567 2_667 ? O3 S1 O1 114.41(12) . . ? O3 S1 O2 113.03(12) . . ? O1 S1 O2 110.17(11) . . ? O3 S1 C2 106.20(11) . . ? O1 S1 C2 105.94(12) . . ? O2 S1 C2 106.44(12) . . ? S1 O1 Li1 129.74(18) . 2_567 ? S1 O1 Li1 124.24(17) . . ? Li1 O1 Li1 93.73(19) 2_567 . ? Li1 O1W H1W1 130(2) . . ? Li1 O1W H1W2 102(2) . . ? H1W1 O1W H1W2 109.2(17) . . ? S1 O2 Li1 133.27(19) . 2_667 ? C1 O4 Li1 128.8(2) . . ? C1 O4 H4O 105(2) . . ? Li1 O4 H4O 122(2) . . ? O4 C1 C3 122.1(2) . 2_666 ? O4 C1 C2 118.7(2) . . ? C3 C1 C2 119.2(2) 2_666 . ? C3 C2 C1 121.2(2) . . ? C3 C2 S1 119.60(19) . . ? C1 C2 S1 119.18(19) . . ? C2 C3 C1 119.6(2) . 2_666 ? C2 C3 H3 120.2 . . ? C1 C3 H3 120.2 2_666 . ? 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 O3 S1 O1 Li1 -46.9(3) . . . 2_567 ? O2 S1 O1 Li1 81.8(2) . . . 2_567 ? C2 S1 O1 Li1 -163.5(2) . . . 2_567 ? O3 S1 O1 Li1 -178.8(2) . . . . ? O2 S1 O1 Li1 -50.2(2) . . . . ? C2 S1 O1 Li1 64.6(2) . . . . ? O2 Li1 O1 S1 33.0(7) 2_667 . . . ? O1W Li1 O1 S1 -119.71(19) . . . . ? O1 Li1 O1 S1 145.01(19) 2_567 . . . ? O4 Li1 O1 S1 -28.1(2) . . . . ? Li1 Li1 O1 S1 145.01(19) 2_567 . . . ? Li1 Li1 O1 S1 28.3(3) 2_667 . . . ? O2 Li1 O1 Li1 -112.0(6) 2_667 . . 2_567 ? O1W Li1 O1 Li1 95.3(2) . . . 2_567 ? O1 Li1 O1 Li1 0.0 2_567 . . 2_567 ? O4 Li1 O1 Li1 -173.1(3) . . . 2_567 ? Li1 Li1 O1 Li1 -116.7(2) 2_667 . . 2_567 ? O3 S1 O2 Li1 -178.9(2) . . . 2_667 ? O1 S1 O2 Li1 51.8(3) . . . 2_667 ? C2 S1 O2 Li1 -62.7(3) . . . 2_667 ? O2 Li1 O4 C1 171.6(2) 2_667 . . . ? O1W Li1 O4 C1 69.0(3) . . . . ? O1 Li1 O4 C1 -64.7(13) 2_567 . . . ? O1 Li1 O4 C1 -32.0(3) . . . . ? Li1 Li1 O4 C1 -37.6(5) 2_567 . . . ? Li1 Li1 O4 C1 -112.2(2) 2_667 . . . ? Li1 O4 C1 C3 -135.2(3) . . . 2_666 ? Li1 O4 C1 C2 44.5(4) . . . . ? O4 C1 C2 C3 -179.5(2) . . . . ? C3 C1 C2 C3 0.2(4) 2_666 . . . ? O4 C1 C2 S1 2.2(3) . . . . ? C3 C1 C2 S1 -178.1(2) 2_666 . . . ? O3 S1 C2 C3 5.3(2) . . . . ? O1 S1 C2 C3 127.3(2) . . . . ? O2 S1 C2 C3 -115.4(2) . . . . ? O3 S1 C2 C1 -176.4(2) . . . . ? O1 S1 C2 C1 -54.4(2) . . . . ? O2 S1 C2 C1 62.9(2) . . . . ? C1 C2 C3 C1 -0.2(4) . . . 2_666 ? S1 C2 C3 C1 178.1(2) . . . 2_666 ? 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 O1W H1W1 O2 0.85(3) 1.94(3) 2.755(3) 161(3) 1_445 O1W H1W2 O3 0.85(3) 2.03(2) 2.794(3) 149(3) 1_545 O4 H4O O1W 0.85(3) 1.93(3) 2.762(3) 168(4) 1_655 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.734 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.109 # Attachment 'complex 3.cif' data_w _database_code_depnum_ccdc_archive 'CCDC 852887' #TrackingRef 'complex 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H38 Li12 O49 S6' _chemical_formula_sum 'C18 H38 Li12 O49 S6' _chemical_formula_weight 1314.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C mc21 ' _symmetry_space_group_name_Hall 'C 2c -2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' '-x, y, z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' _cell_length_a 36.593(7) _cell_length_b 12.589(3) _cell_length_c 10.619(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4891.8(17) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 16699 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.41 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 0.412 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9148 _exptl_absorpt_correction_T_max 0.9445 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21176 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.42 _reflns_number_total 5599 _reflns_number_gt 5386 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0685P)^2^+7.0622P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.42(11) _refine_ls_number_reflns 5599 _refine_ls_number_parameters 445 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1290 _refine_ls_wR_factor_gt 0.1239 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.2535(3) 0.1179(9) 0.6037(11) 0.069(3) Uani 1 1 d . . . Li2 Li 0.1772(3) 0.0056(7) 0.6172(8) 0.0493(19) Uani 1 1 d . . . Li3 Li 0.08524(19) 0.0970(4) 0.6113(8) 0.0291(11) Uani 1 1 d . . . Li4 Li 0.0000 0.0044(9) 0.6263(13) 0.046(3) Uani 1 2 d S . . Li5 Li 0.0000 0.4737(9) 1.1150(14) 0.049(3) Uani 1 2 d S . . Li6 Li 0.07890(15) 0.3737(5) 1.1266(10) 0.0408(17) Uani 1 1 d . . . Li7 Li 0.1600(2) 0.4722(5) 0.1105(8) 0.0357(15) Uani 1 1 d . . . S1 S 0.25413(2) 0.26647(7) 0.35840(11) 0.0329(3) Uani 1 1 d . . . S2 S 0.07850(2) 0.23778(7) 0.38341(8) 0.0229(2) Uani 1 1 d . . . S3 S 0.08794(2) 0.25245(7) 0.85563(9) 0.0246(2) Uani 1 1 d . . . O1 O 0.27007(9) 0.2185(5) 0.4642(5) 0.0959(18) Uani 1 1 d . . . O1W O 0.23919(17) -0.0265(5) 0.6540(10) 0.0718(12) Uani 1 1 d D . . H1W1 H 0.2170(10) -0.046(10) 0.651(18) 0.275 Uiso 1 1 d D . . H1W2 H 0.253(3) -0.075(9) 0.624(16) 0.275 Uiso 1 1 d D . . O2W O 0.16566(7) 0.0313(3) 0.7882(3) 0.0413(7) Uani 1 1 d D . . H2W1 H 0.1860(5) 0.035(4) 0.825(4) 0.062 Uiso 1 1 d D . . H2W2 H 0.1489(8) 0.054(4) 0.836(3) 0.062 Uiso 1 1 d D . . O2 O 0.26127(10) 0.3799(3) 0.3573(10) 0.151(3) Uani 1 1 d . . . O3 O 0.26588(9) 0.2286(4) 0.2385(4) 0.0708(12) Uani 1 1 d . . . O3W O 0.16866(8) -0.1353(3) 0.5561(4) 0.0464(8) Uani 1 1 d D . . H3W1 H 0.1859(8) -0.181(3) 0.554(6) 0.070 Uiso 1 1 d D . . H3W2 H 0.1484(6) -0.168(3) 0.566(6) 0.070 Uiso 1 1 d D . . O4 O 0.20563(8) 0.1146(2) 0.5167(4) 0.0465(8) Uani 1 1 d . . . O4W O 0.08382(13) -0.0536(2) 0.6228(6) 0.0750(12) Uani 1 1 d D . . H4W1 H 0.0799(15) -0.112(3) 0.661(7) 0.113 Uiso 1 1 d D . . H4W2 H 0.1064(5) -0.040(5) 0.622(8) 0.113 Uiso 1 1 d D . . O5 O 0.13598(7) 0.1112(2) 0.5375(3) 0.0339(6) Uani 1 1 d . . . O5W O 0.0000 0.0153(3) 0.4433(5) 0.0430(10) Uani 1 2 d SD . . H5W H 0.01892(14) 0.0552(12) 0.440(6) 0.064 Uiso 1 1 d D . . O6 O 0.06743(8) 0.1385(3) 0.4353(3) 0.0501(9) Uani 1 1 d . . . O6W O 0.0000 -0.1446(3) 0.6839(5) 0.0401(10) Uani 1 2 d S . . H6W H -0.0189 -0.1788 0.7073 0.060 Uiso 1 1 d R . . O7 O 0.06720(8) 0.3312(3) 0.4559(4) 0.0648(11) Uani 1 1 d . . . O7W O 0.04425(8) 0.4840(2) 1.2381(3) 0.0432(7) Uani 1 1 d D . . H7W1 H 0.0522(14) 0.5474(16) 1.245(4) 0.065 Uiso 1 1 d D . . H7W2 H 0.0421(14) 0.458(3) 1.3123(19) 0.065 Uiso 1 1 d D . . O8 O 0.06500(7) 0.2504(2) 0.2560(4) 0.0397(8) Uani 1 1 d . . . O8W O 0.0000 0.5997(4) 1.0292(10) 0.103(3) Uani 1 2 d SD . . H8W H -0.01899(14) 0.631(5) 1.057(7) 0.155 Uiso 1 1 d D . . O9 O 0.12712(6) 0.3782(2) 0.2270(3) 0.0298(6) Uani 1 1 d . . . O9W O 0.10804(10) 0.4947(3) 1.0186(4) 0.0618(10) Uani 1 1 d D . . H9W1 H 0.0987(17) 0.556(2) 1.025(5) 0.093 Uiso 1 1 d D . . H9W2 H 0.1071(17) 0.474(4) 0.943(2) 0.093 Uiso 1 1 d D . . O10 O 0.19712(6) 0.3733(2) 0.1983(3) 0.0300(6) Uani 1 1 d . . . O10W O 0.16483(9) 0.6207(4) 0.1834(7) 0.0876(19) Uani 1 1 d D . . HAW2 H 0.1828(13) 0.616(7) 0.234(5) 0.131 Uiso 1 1 d D . . HAW1 H 0.1466(12) 0.647(6) 0.222(6) 0.131 Uiso 1 1 d D . . O11 O 0.03518(6) 0.1117(2) 0.6946(3) 0.0278(5) Uani 1 1 d . . . O11W O 0.1928(3) 0.4779(4) -0.0414(6) 0.164(4) Uani 1 1 d D . . HBW2 H 0.1733(19) 0.441(9) -0.05(2) 0.246 Uiso 1 1 d D . . HBW1 H 0.211(2) 0.436(9) -0.043(17) 0.246 Uiso 1 1 d D . . O12 O 0.10279(7) 0.1651(3) 0.7820(3) 0.0474(8) Uani 1 1 d . . . O13 O 0.10084(7) 0.24638(19) 0.9866(3) 0.0297(6) Uani 1 1 d . . . O14 O 0.09603(6) 0.3565(2) 0.8039(3) 0.0421(7) Uani 1 1 d . . . O15 O 0.03510(6) 0.3686(2) 1.0179(3) 0.0304(6) Uani 1 1 d . . . C1 C 0.20636(10) 0.2513(3) 0.3674(5) 0.0288(8) Uani 1 1 d . . . C2 C 0.18978(10) 0.1780(3) 0.4473(4) 0.0258(7) Uani 1 1 d . . . C3 C 0.14783(9) 0.1744(3) 0.4570(4) 0.0239(7) Uani 1 1 d . . . C4 C 0.12664(8) 0.2402(2) 0.3780(4) 0.0176(6) Uani 1 1 d . . . C5 C 0.14304(8) 0.3114(3) 0.2939(4) 0.0222(7) Uani 1 1 d . . . C6 C 0.18588(8) 0.3150(3) 0.2822(4) 0.0256(7) Uani 1 1 d . . . C7 C 0.02123(7) 0.1717(3) 0.7759(4) 0.0207(7) Uani 1 1 d . . . C8 C 0.04050(9) 0.2393(2) 0.8585(5) 0.0248(7) Uani 1 1 d . . . C9 C 0.02066(8) 0.3058(2) 0.9406(4) 0.0210(7) 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 Li1 0.064(5) 0.080(6) 0.064(6) 0.006(5) -0.036(5) -0.009(5) Li2 0.086(5) 0.039(3) 0.022(3) 0.005(3) 0.014(4) 0.016(4) Li3 0.030(3) 0.025(2) 0.033(3) -0.009(3) 0.009(2) -0.002(3) Li4 0.056(6) 0.023(4) 0.058(7) -0.006(4) 0.000 0.000 Li5 0.042(5) 0.048(7) 0.056(7) -0.025(5) 0.000 0.000 Li6 0.014(2) 0.045(3) 0.064(4) 0.019(4) -0.020(3) -0.016(3) Li7 0.054(4) 0.026(3) 0.028(3) -0.004(3) 0.006(3) -0.010(3) S1 0.0133(4) 0.0371(4) 0.0481(6) -0.0063(5) -0.0024(4) 0.0019(3) S2 0.0156(4) 0.0284(4) 0.0246(5) -0.0024(4) 0.0026(3) -0.0047(3) S3 0.0149(4) 0.0325(4) 0.0265(5) -0.0041(3) -0.0010(3) -0.0007(3) O1 0.0325(17) 0.191(5) 0.064(3) 0.048(3) -0.0177(17) -0.003(2) O1W 0.0286(15) 0.128(4) 0.062(2) -0.013(2) 0.0065(15) -0.00101(19) O2W 0.0353(14) 0.0611(19) 0.0273(14) -0.0025(13) -0.0067(10) -0.0085(12) O2 0.0324(17) 0.0392(18) 0.380(11) 0.009(4) -0.051(4) -0.0082(15) O3 0.0284(15) 0.125(4) 0.059(2) -0.009(2) 0.0060(15) -0.0095(19) O3W 0.0321(14) 0.0585(19) 0.049(2) -0.0060(16) -0.0016(12) 0.0042(14) O4 0.0383(14) 0.0338(14) 0.067(2) 0.0130(15) -0.0243(16) -0.0007(12) O4W 0.103(3) 0.0236(13) 0.098(3) 0.006(2) 0.052(2) 0.008(2) O5 0.0301(12) 0.0391(14) 0.0325(13) 0.0115(11) 0.0049(11) 0.0073(11) O5W 0.060(3) 0.0262(17) 0.043(2) -0.0115(17) 0.000 0.000 O6 0.0387(14) 0.0637(19) 0.0478(18) 0.0388(15) -0.0130(12) -0.0266(14) O6W 0.0236(16) 0.0278(17) 0.069(3) 0.0134(19) 0.000 0.000 O7 0.0257(13) 0.077(2) 0.092(3) -0.045(2) 0.0202(15) -0.0059(15) O7W 0.0538(16) 0.0320(13) 0.0439(16) -0.0040(11) -0.0223(14) -0.0117(12) O8 0.0196(13) 0.0444(15) 0.055(2) 0.0197(13) -0.0090(13) -0.0164(11) O8W 0.034(2) 0.063(3) 0.213(9) 0.084(5) 0.000 0.000 O9 0.0181(10) 0.0392(13) 0.0321(14) 0.0160(11) -0.0011(10) -0.0035(10) O9W 0.073(2) 0.0469(16) 0.066(2) 0.0200(16) -0.0424(18) -0.0198(17) O10 0.0234(11) 0.0376(13) 0.0289(13) 0.0070(10) 0.0049(10) -0.0046(11) O10W 0.0342(17) 0.078(3) 0.150(5) -0.057(3) 0.031(2) -0.0150(18) O11 0.0160(10) 0.0404(13) 0.0270(12) -0.0154(10) -0.0002(9) 0.0035(9) O11W 0.329(10) 0.093(4) 0.070(4) 0.030(3) 0.102(5) 0.087(5) O12 0.0177(10) 0.070(2) 0.0549(18) -0.0274(16) -0.0063(11) 0.0107(12) O13 0.0243(13) 0.0364(13) 0.0284(15) 0.0024(10) -0.0063(11) -0.0004(10) O14 0.0203(11) 0.0499(15) 0.0560(18) 0.0271(14) -0.0048(12) -0.0094(11) O15 0.0195(10) 0.0344(12) 0.0372(15) -0.0143(11) -0.0078(10) 0.0007(10) C1 0.0153(15) 0.0383(17) 0.033(2) -0.0025(14) -0.0049(18) 0.0031(13) C2 0.0270(16) 0.0198(14) 0.0305(18) -0.0033(13) -0.0095(14) 0.0001(13) C3 0.0318(17) 0.0207(14) 0.0193(16) -0.0017(12) -0.0015(14) 0.0059(13) C4 0.0123(13) 0.0207(12) 0.0197(17) 0.0057(12) 0.0028(15) -0.0023(11) C5 0.0119(12) 0.0310(15) 0.0238(17) 0.0059(14) 0.0061(13) -0.0015(12) C6 0.0134(13) 0.0373(17) 0.0261(17) -0.0001(14) -0.0011(14) -0.0011(13) C7 0.0131(14) 0.0263(15) 0.0227(17) -0.0003(13) 0.0016(12) 0.0055(11) C8 0.0173(15) 0.0274(14) 0.0295(19) 0.0015(14) -0.0056(18) 0.0002(12) C9 0.0246(16) 0.0176(13) 0.0208(16) 0.0023(12) -0.0065(13) -0.0024(12) _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 O1W 1.965(12) . ? Li1 O4 1.981(9) . ? Li1 O1 2.041(13) . ? Li1 O10 2.070(9) 6 ? Li1 O3 2.508(13) 6 ? Li1 Li2 3.133(14) . ? Li1 Li7 3.364(13) 6 ? Li2 O2W 1.892(9) . ? Li2 O3W 1.914(10) . ? Li2 O4 2.026(9) . ? Li2 O5 2.181(9) . ? Li2 O1W 2.337(11) . ? Li2 H1W1 1.63(10) . ? Li2 H2W1 2.26(4) . ? Li3 O4W 1.902(6) . ? Li3 O5 2.023(7) . ? Li3 O11 2.043(7) . ? Li3 O6 2.047(9) . ? Li3 O12 2.105(8) . ? Li3 S2 3.009(8) . ? Li3 Li4 3.334(8) . ? Li3 H4W2 1.90(6) . ? Li4 O5W 1.948(15) . ? Li4 O6W 1.973(13) . ? Li4 O11 2.002(9) . ? Li4 O11 2.002(9) 4 ? Li4 C7 2.750(12) 4 ? Li4 C7 2.750(12) . ? Li4 Li3 3.334(8) 4 ? Li4 H5W 2.19(6) . ? Li5 O8W 1.829(15) . ? Li5 O7W 2.085(10) . ? Li5 O7W 2.085(10) 4 ? Li5 O15 2.113(9) 4 ? Li5 O15 2.113(9) . ? Li5 Li6 3.152(8) 4 ? Li5 Li6 3.152(8) . ? Li5 H8W 2.18(8) . ? Li6 O15 1.976(7) . ? Li6 O9 2.063(7) 1_556 ? Li6 O8 2.134(8) 1_556 ? Li6 O9W 2.185(8) . ? Li6 O7W 2.223(9) . ? Li6 O13 2.328(10) . ? Li6 Li7 3.220(9) 1_556 ? Li7 O11W 2.012(10) . ? Li7 O10W 2.030(8) . ? Li7 O10 2.067(8) . ? Li7 O9 2.092(8) . ? Li7 O9W 2.154(9) 1_554 ? Li7 Li6 3.220(9) 1_554 ? Li7 Li1 3.364(13) 6_554 ? Li7 HBW2 1.8(2) . ? S1 O1 1.403(4) . ? S1 O3 1.426(4) . ? S1 O2 1.451(3) . ? S1 C1 1.761(4) . ? S2 O6 1.425(3) . ? S2 O8 1.449(4) . ? S2 O7 1.466(3) . ? S2 C4 1.763(3) . ? S3 O14 1.451(3) . ? S3 O12 1.455(3) . ? S3 O13 1.471(3) . ? S3 C8 1.744(3) . ? O1W H1W1 0.85(6) . ? O1W H1W2 0.85(6) . ? O2W H2W1 0.84(5) . ? O2W H2W2 0.85(6) . ? O3 Li1 2.508(13) 6_554 ? O3W H3W1 0.85(6) . ? O3W H3W2 0.85(6) . ? O4 C2 1.232(4) . ? O4W H4W1 0.85(6) . ? O4W H4W2 0.85(6) . ? O5 C3 1.246(5) . ? O5W H5W 0.86(6) . ? O6W H6W 0.8500 . ? O7W H7W1 0.85(6) . ? O7W H7W2 0.85(6) . ? O8 Li6 2.134(8) 1_554 ? O8W H8W 0.85(6) . ? O9 C5 1.246(4) . ? O9 Li6 2.063(7) 1_554 ? O9W Li7 2.154(9) 1_556 ? O9W H9W1 0.85(6) . ? O9W H9W2 0.85(6) . ? O10 C6 1.225(5) . ? O10 Li1 2.070(9) 6_554 ? O10W HAW2 0.85(6) . ? O10W HAW1 0.85(6) . ? O11 C7 1.255(4) . ? O11W HBW2 0.85(6) . ? O11W HBW1 0.85(6) . ? O15 C9 1.257(4) . ? C1 C2 1.393(6) . ? C1 C6 1.422(6) . ? C2 C3 1.539(5) . ? C3 C4 1.411(5) . ? C4 C5 1.400(5) . ? C5 C6 1.573(4) . ? C7 C8 1.411(5) . ? C7 C7 1.553(5) 4 ? C8 C9 1.409(5) . ? C9 C9 1.512(6) 4 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Li1 O4 82.6(4) . . ? O1W Li1 O1 148.3(8) . . ? O4 Li1 O1 86.4(4) . . ? O1W Li1 O10 98.7(5) . 6 ? O4 Li1 O10 177.7(7) . 6 ? O1 Li1 O10 93.4(4) . 6 ? O1W Li1 O3 118.8(7) . 6 ? O4 Li1 O3 91.8(4) . 6 ? O1 Li1 O3 91.1(5) . 6 ? O10 Li1 O3 85.9(4) 6 6 ? O1W Li1 Li2 48.1(3) . . ? O4 Li1 Li2 39.1(3) . . ? O1 Li1 Li2 125.3(4) . . ? O10 Li1 Li2 141.2(5) 6 . ? O3 Li1 Li2 94.0(4) 6 . ? O1W Li1 Li7 86.2(4) . 6 ? O4 Li1 Li7 146.6(6) . 6 ? O1 Li1 Li7 86.9(4) . 6 ? O10 Li1 Li7 35.6(2) 6 6 ? O3 Li1 Li7 120.9(4) 6 6 ? Li2 Li1 Li7 133.3(4) . 6 ? O2W Li2 O3W 116.6(5) . . ? O2W Li2 O4 120.3(5) . . ? O3W Li2 O4 122.2(4) . . ? O2W Li2 O5 96.5(4) . . ? O3W Li2 O5 108.6(5) . . ? O4 Li2 O5 74.8(3) . . ? O2W Li2 O1W 94.9(5) . . ? O3W Li2 O1W 93.2(4) . . ? O4 Li2 O1W 72.9(3) . . ? O5 Li2 O1W 147.3(5) . . ? O2W Li2 Li1 99.5(5) . . ? O3W Li2 Li1 123.2(4) . . ? O4 Li2 Li1 38.1(3) . . ? O5 Li2 Li1 108.9(4) . . ? O1W Li2 Li1 38.8(3) . . ? O2W Li2 H1W1 93(6) . . ? O3W Li2 H1W1 82(4) . . ? O4 Li2 H1W1 86(5) . . ? O5 Li2 H1W1 161(5) . . ? O1W Li2 H1W1 14(4) . . ? Li1 Li2 H1W1 53(4) . . ? O2W Li2 H2W1 21.1(6) . . ? O3W Li2 H2W1 120.2(14) . . ? O4 Li2 H2W1 109.4(12) . . ? O5 Li2 H2W1 112.3(10) . . ? O1W Li2 H2W1 74.1(8) . . ? Li1 Li2 H2W1 81.1(9) . . ? H1W1 Li2 H2W1 74(6) . . ? O4W Li3 O5 97.9(3) . . ? O4W Li3 O11 92.2(3) . . ? O5 Li3 O11 169.4(3) . . ? O4W Li3 O6 107.7(4) . . ? O5 Li3 O6 85.2(3) . . ? O11 Li3 O6 95.0(3) . . ? O4W Li3 O12 111.0(4) . . ? O5 Li3 O12 91.0(3) . . ? O11 Li3 O12 82.2(3) . . ? O6 Li3 O12 141.2(3) . . ? O4W Li3 S2 129.5(4) . . ? O5 Li3 S2 73.3(2) . . ? O11 Li3 S2 102.8(3) . . ? O6 Li3 S2 24.44(12) . . ? O12 Li3 S2 118.6(2) . . ? O4W Li3 Li4 67.8(3) . . ? O5 Li3 Li4 155.2(4) . . ? O11 Li3 Li4 34.1(2) . . ? O6 Li3 Li4 80.5(3) . . ? O12 Li3 Li4 112.8(4) . . ? S2 Li3 Li4 99.7(3) . . ? O4W Li3 H4W2 25.7(5) . . ? O5 Li3 H4W2 74.2(11) . . ? O11 Li3 H4W2 115.1(13) . . ? O6 Li3 H4W2 115(3) . . ? O12 Li3 H4W2 101(2) . . ? S2 Li3 H4W2 128(3) . . ? Li4 Li3 H4W2 93.5(6) . . ? O5W Li4 O6W 112.1(6) . . ? O5W Li4 O11 108.3(5) . . ? O6W Li4 O11 121.9(6) . . ? O5W Li4 O11 108.3(5) . 4 ? O6W Li4 O11 121.9(6) . 4 ? O11 Li4 O11 80.0(5) . 4 ? O5W Li4 C7 121.5(6) . 4 ? O6W Li4 C7 123.3(6) . 4 ? O11 Li4 C7 57.0(3) . 4 ? O11 Li4 C7 24.81(18) 4 4 ? O5W Li4 C7 121.5(6) . . ? O6W Li4 C7 123.3(6) . . ? O11 Li4 C7 24.81(18) . . ? O11 Li4 C7 57.0(3) 4 . ? C7 Li4 C7 32.81(18) 4 . ? O5W Li4 Li3 85.9(3) . . ? O6W Li4 Li3 110.3(2) . . ? O11 Li4 Li3 34.89(15) . . ? O11 Li4 Li3 112.5(4) 4 . ? C7 Li4 Li3 91.4(3) 4 . ? C7 Li4 Li3 59.69(18) . . ? O5W Li4 Li3 85.9(3) . 4 ? O6W Li4 Li3 110.3(2) . 4 ? O11 Li4 Li3 112.5(4) . 4 ? O11 Li4 Li3 34.89(15) 4 4 ? C7 Li4 Li3 59.69(18) 4 4 ? C7 Li4 Li3 91.4(3) . 4 ? Li3 Li4 Li3 138.6(4) . 4 ? O5W Li4 H5W 22.9(8) . . ? O6W Li4 H5W 123.9(9) . . ? O11 Li4 H5W 85.9(9) . . ? O11 Li4 H5W 109.5(7) 4 . ? C7 Li4 H5W 112.8(8) 4 . ? C7 Li4 H5W 102.1(9) . . ? Li3 Li4 H5W 63.9(7) . . ? Li3 Li4 H5W 98.6(5) 4 . ? O8W Li5 O7W 105.0(4) . . ? O8W Li5 O7W 105.0(4) . 4 ? O7W Li5 O7W 101.9(7) . 4 ? O8W Li5 O15 107.4(7) . 4 ? O7W Li5 O15 144.8(6) . 4 ? O7W Li5 O15 82.7(2) 4 4 ? O8W Li5 O15 107.4(7) . . ? O7W Li5 O15 82.7(2) . . ? O7W Li5 O15 144.8(6) 4 . ? O15 Li5 O15 74.9(4) 4 . ? O8W Li5 Li6 111.5(3) . 4 ? O7W Li5 Li6 135.4(7) . 4 ? O7W Li5 Li6 44.7(2) 4 4 ? O15 Li5 Li6 38.0(2) 4 4 ? O15 Li5 Li6 109.0(4) . 4 ? O8W Li5 Li6 111.5(3) . . ? O7W Li5 Li6 44.7(2) . . ? O7W Li5 Li6 135.4(7) 4 . ? O15 Li5 Li6 109.0(4) 4 . ? O15 Li5 Li6 38.0(2) . . ? Li6 Li5 Li6 132.7(4) 4 . ? O8W Li5 H8W 22.2(14) . . ? O7W Li5 H8W 111.6(7) . . ? O7W Li5 H8W 82.8(14) 4 . ? O15 Li5 H8W 103.6(8) 4 . ? O15 Li5 H8W 128.4(18) . . ? Li6 Li5 H8W 94.6(6) 4 . ? Li6 Li5 H8W 131.6(9) . . ? O15 Li6 O9 175.4(5) . 1_556 ? O15 Li6 O8 99.2(3) . 1_556 ? O9 Li6 O8 83.7(3) 1_556 1_556 ? O15 Li6 O9W 96.4(4) . . ? O9 Li6 O9W 80.5(2) 1_556 . ? O8 Li6 O9W 164.0(3) 1_556 . ? O15 Li6 O7W 82.4(2) . . ? O9 Li6 O7W 101.2(4) 1_556 . ? O8 Li6 O7W 88.6(4) 1_556 . ? O9W Li6 O7W 97.0(3) . . ? O15 Li6 O13 83.4(4) . . ? O9 Li6 O13 93.1(3) 1_556 . ? O8 Li6 O13 89.6(3) 1_556 . ? O9W Li6 O13 88.7(4) . . ? O7W Li6 O13 165.2(3) . . ? O15 Li6 Li5 41.2(3) . . ? O9 Li6 Li5 142.4(5) 1_556 . ? O8 Li6 Li5 95.6(3) 1_556 . ? O9W Li6 Li5 98.5(3) . . ? O7W Li6 Li5 41.3(3) . . ? O13 Li6 Li5 124.5(4) . . ? O15 Li6 Li7 136.8(4) . 1_556 ? O9 Li6 Li7 39.53(19) 1_556 1_556 ? O8 Li6 Li7 122.3(3) 1_556 1_556 ? O9W Li6 Li7 41.73(19) . 1_556 ? O7W Li6 Li7 108.2(3) . 1_556 ? O13 Li6 Li7 85.0(2) . 1_556 ? Li5 Li6 Li7 133.5(3) . 1_556 ? O11W Li7 O10W 102.8(4) . . ? O11W Li7 O10 89.5(4) . . ? O10W Li7 O10 108.9(4) . . ? O11W Li7 O9 146.8(4) . . ? O10W Li7 O9 110.2(4) . . ? O10 Li7 O9 76.7(3) . . ? O11W Li7 O9W 99.1(5) . 1_554 ? O10W Li7 O9W 97.4(4) . 1_554 ? O10 Li7 O9W 149.7(3) . 1_554 ? O9 Li7 O9W 80.5(3) . 1_554 ? O11W Li7 Li6 127.3(5) . 1_554 ? O10W Li7 Li6 114.5(4) . 1_554 ? O10 Li7 Li6 110.5(3) . 1_554 ? O9 Li7 Li6 38.9(2) . 1_554 ? O9W Li7 Li6 42.5(2) 1_554 1_554 ? O11W Li7 Li1 55.5(4) . 6_554 ? O10W Li7 Li1 103.6(3) . 6_554 ? O10 Li7 Li1 35.6(2) . 6_554 ? O9 Li7 Li1 111.3(4) . 6_554 ? O9W Li7 Li1 149.8(4) 1_554 6_554 ? Li6 Li7 Li1 137.6(3) 1_554 6_554 ? O11W Li7 HBW2 25(3) . . ? O10W Li7 HBW2 123(3) . . ? O10 Li7 HBW2 96(5) . . ? O9 Li7 HBW2 126(2) . . ? O9W Li7 HBW2 81(3) 1_554 . ? Li6 Li7 HBW2 102.4(9) 1_554 . ? Li1 Li7 HBW2 69(4) 6_554 . ? O1 S1 O3 116.5(3) . . ? O1 S1 O2 110.8(4) . . ? O3 S1 O2 105.5(4) . . ? O1 S1 C1 108.8(2) . . ? O3 S1 C1 108.1(2) . . ? O2 S1 C1 106.60(19) . . ? O6 S2 O8 111.16(17) . . ? O6 S2 O7 114.9(2) . . ? O8 S2 O7 107.8(2) . . ? O6 S2 C4 108.19(16) . . ? O8 S2 C4 107.95(18) . . ? O7 S2 C4 106.56(16) . . ? O8 S2 Li3 147.52(17) . . ? O7 S2 Li3 94.2(2) . . ? C4 S2 Li3 87.41(17) . . ? O14 S3 O12 113.8(2) . . ? O14 S3 O13 109.84(17) . . ? O12 S3 O13 110.44(18) . . ? O14 S3 C8 107.19(15) . . ? O12 S3 C8 108.02(17) . . ? O13 S3 C8 107.3(2) . . ? S1 O1 Li1 136.5(3) . . ? Li1 O1W Li2 93.1(4) . . ? Li1 O1W H1W1 121(10) . . ? Li1 O1W H1W2 114(10) . . ? Li2 O1W H1W2 129(10) . . ? H1W1 O1W H1W2 110(12) . . ? Li2 O2W H2W1 105(3) . . ? Li2 O2W H2W2 143(3) . . ? H2W1 O2W H2W2 110(3) . . ? S1 O3 Li1 99.6(3) . 6_554 ? Li2 O3W H3W1 121(3) . . ? Li2 O3W H3W2 123(3) . . ? H3W1 O3W H3W2 109(3) . . ? C2 O4 Li1 133.0(4) . . ? C2 O4 Li2 120.8(4) . . ? Li1 O4 Li2 102.9(5) . . ? Li3 O4W H4W1 153(5) . . ? Li3 O4W H4W2 77(4) . . ? H4W1 O4W H4W2 110(6) . . ? C3 O5 Li3 129.9(3) . . ? C3 O5 Li2 114.5(3) . . ? Li3 O5 Li2 115.5(3) . . ? Li4 O5W H5W 95(4) . . ? S2 O6 Li3 119.1(2) . . ? Li4 O6W H6W 124.9 . . ? Li5 O7W Li6 94.0(4) . . ? Li5 O7W H7W1 112(3) . . ? Li6 O7W H7W1 116(3) . . ? Li5 O7W H7W2 119(3) . . ? Li6 O7W H7W2 108(3) . . ? H7W1 O7W H7W2 108(4) . . ? S2 O8 Li6 126.9(3) . 1_554 ? Li5 O8W H8W 103(6) . . ? C5 O9 Li6 132.5(3) . 1_554 ? C5 O9 Li7 116.8(3) . . ? Li6 O9 Li7 101.6(3) 1_554 . ? Li7 O9W Li6 95.8(3) 1_556 . ? Li7 O9W H9W1 116(4) 1_556 . ? Li6 O9W H9W1 113(5) . . ? Li7 O9W H9W2 115(4) 1_556 . ? Li6 O9W H9W2 106(4) . . ? H9W1 O9W H9W2 110(5) . . ? C6 O10 Li7 117.9(3) . . ? C6 O10 Li1 132.7(4) . 6_554 ? Li7 O10 Li1 108.8(4) . 6_554 ? Li7 O10W HAW2 104(6) . . ? Li7 O10W HAW1 118(6) . . ? HAW2 O10W HAW1 109(6) . . ? C7 O11 Li4 113.2(3) . . ? C7 O11 Li3 135.8(3) . . ? Li4 O11 Li3 111.0(3) . . ? Li7 O11W HBW2 63(10) . . ? Li7 O11W HBW1 118(10) . . ? HBW2 O11W HBW1 108(10) . . ? S3 O12 Li3 131.0(2) . . ? S3 O13 Li6 117.2(2) . . ? C9 O15 Li6 138.0(3) . . ? C9 O15 Li5 117.2(3) . . ? Li6 O15 Li5 100.8(4) . . ? C2 C1 C6 122.1(3) . . ? C2 C1 S1 122.5(3) . . ? C6 C1 S1 115.3(3) . . ? O4 C2 C1 126.1(3) . . ? O4 C2 C3 114.3(3) . . ? C1 C2 C3 119.6(3) . . ? O5 C3 C4 126.3(3) . . ? O5 C3 C2 114.3(3) . . ? C4 C3 C2 119.4(3) . . ? C5 C4 C3 121.3(3) . . ? C5 C4 S2 117.4(2) . . ? C3 C4 S2 121.3(2) . . ? O9 C5 C4 126.6(3) . . ? O9 C5 C6 113.7(3) . . ? C4 C5 C6 119.7(3) . . ? O10 C6 C1 128.6(3) . . ? O10 C6 C5 114.2(3) . . ? C1 C6 C5 117.3(3) . . ? O11 C7 C8 125.9(3) . . ? O11 C7 C7 114.00(17) . 4 ? C8 C7 C7 119.99(19) . 4 ? C8 C7 Li4 164.2(3) . . ? C7 C7 Li4 73.60(9) 4 . ? C9 C8 C7 119.0(3) . . ? C9 C8 S3 117.8(3) . . ? C7 C8 S3 122.9(3) . . ? O15 C9 C8 124.1(3) . . ? O15 C9 C9 114.86(18) . 4 ? C8 C9 C9 120.99(19) . 4 ? 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 O1W Li1 Li2 O2W 86.0(6) . . . . ? O4 Li1 Li2 O2W -127.9(5) . . . . ? O1 Li1 Li2 O2W -134.1(7) . . . . ? O10 Li1 Li2 O2W 48.5(10) 6 . . . ? O3 Li1 Li2 O2W -39.9(4) 6 . . . ? Li7 Li1 Li2 O2W 100.7(6) 6 . . . ? O1W Li1 Li2 O3W -44.8(7) . . . . ? O4 Li1 Li2 O3W 101.3(6) . . . . ? O1 Li1 Li2 O3W 95.1(8) . . . . ? O10 Li1 Li2 O3W -82.3(10) 6 . . . ? O3 Li1 Li2 O3W -170.7(5) 6 . . . ? Li7 Li1 Li2 O3W -30.0(9) 6 . . . ? O1W Li1 Li2 O4 -146.1(8) . . . . ? O1 Li1 Li2 O4 -6.2(5) . . . . ? O10 Li1 Li2 O4 176.4(12) 6 . . . ? O3 Li1 Li2 O4 88.0(5) 6 . . . ? Li7 Li1 Li2 O4 -131.3(8) 6 . . . ? O1W Li1 Li2 O5 -173.7(7) . . . . ? O4 Li1 Li2 O5 -27.6(4) . . . . ? O1 Li1 Li2 O5 -33.8(8) . . . . ? O10 Li1 Li2 O5 148.8(8) 6 . . . ? O3 Li1 Li2 O5 60.4(5) 6 . . . ? Li7 Li1 Li2 O5 -158.9(5) 6 . . . ? O4 Li1 Li2 O1W 146.1(8) . . . . ? O1 Li1 Li2 O1W 139.9(10) . . . . ? O10 Li1 Li2 O1W -37.5(8) 6 . . . ? O3 Li1 Li2 O1W -125.9(7) 6 . . . ? Li7 Li1 Li2 O1W 14.8(6) 6 . . . ? O4W Li3 Li4 O5W -96.7(5) . . . . ? O5 Li3 Li4 O5W -38.6(11) . . . . ? O11 Li3 Li4 O5W 130.9(6) . . . . ? O6 Li3 Li4 O5W 17.0(3) . . . . ? O12 Li3 Li4 O5W 158.9(4) . . . . ? S2 Li3 Li4 O5W 32.2(4) . . . . ? O4W Li3 Li4 O6W 15.4(5) . . . . ? O5 Li3 Li4 O6W 73.5(12) . . . . ? O11 Li3 Li4 O6W -117.1(8) . . . . ? O6 Li3 Li4 O6W 129.1(6) . . . . ? O12 Li3 Li4 O6W -89.0(6) . . . . ? S2 Li3 Li4 O6W 144.3(5) . . . . ? O4W Li3 Li4 O11 132.5(6) . . . . ? O5 Li3 Li4 O11 -169.4(10) . . . . ? O6 Li3 Li4 O11 -113.9(5) . . . . ? O12 Li3 Li4 O11 28.0(5) . . . . ? S2 Li3 Li4 O11 -98.6(4) . . . . ? O4W Li3 Li4 O11 155.2(7) . . . 4 ? O5 Li3 Li4 O11 -146.7(7) . . . 4 ? O11 Li3 Li4 O11 22.8(4) . . . 4 ? O6 Li3 Li4 O11 -91.1(6) . . . 4 ? O12 Li3 Li4 O11 50.8(7) . . . 4 ? S2 Li3 Li4 O11 -75.9(6) . . . 4 ? O4W Li3 Li4 C7 141.9(5) . . . 4 ? O5 Li3 Li4 C7 -160.0(8) . . . 4 ? O11 Li3 Li4 C7 9.4(3) . . . 4 ? O6 Li3 Li4 C7 -104.5(4) . . . 4 ? O12 Li3 Li4 C7 37.4(5) . . . 4 ? S2 Li3 Li4 C7 -89.2(3) . . . 4 ? O4W Li3 Li4 C7 132.9(4) . . . . ? O5 Li3 Li4 C7 -169.0(9) . . . . ? O11 Li3 Li4 C7 0.4(2) . . . . ? O6 Li3 Li4 C7 -113.5(3) . . . . ? O12 Li3 Li4 C7 28.5(3) . . . . ? S2 Li3 Li4 C7 -98.2(3) . . . . ? O4W Li3 Li4 Li3 -175.6(8) . . . 4 ? O5 Li3 Li4 Li3 -117.5(7) . . . 4 ? O11 Li3 Li4 Li3 51.9(7) . . . 4 ? O6 Li3 Li4 Li3 -61.9(8) . . . 4 ? O12 Li3 Li4 Li3 80.0(9) . . . 4 ? S2 Li3 Li4 Li3 -46.7(8) . . . 4 ? O8W Li5 Li6 O15 -91.1(8) . . . . ? O7W Li5 Li6 O15 179.0(6) . . . . ? O7W Li5 Li6 O15 126.3(7) 4 . . . ? O15 Li5 Li6 O15 27.3(4) 4 . . . ? Li6 Li5 Li6 O15 62.6(7) 4 . . . ? O8W Li5 Li6 O9 84.3(10) . . . 1_556 ? O7W Li5 Li6 O9 -5.5(7) . . . 1_556 ? O7W Li5 Li6 O9 -58.2(9) 4 . . 1_556 ? O15 Li5 Li6 O9 -157.3(5) 4 . . 1_556 ? O15 Li5 Li6 O9 175.5(7) . . . 1_556 ? Li6 Li5 Li6 O9 -122.0(6) 4 . . 1_556 ? O8W Li5 Li6 O8 171.3(7) . . . 1_556 ? O7W Li5 Li6 O8 81.4(4) . . . 1_556 ? O7W Li5 Li6 O8 28.8(7) 4 . . 1_556 ? O15 Li5 Li6 O8 -70.3(7) 4 . . 1_556 ? O15 Li5 Li6 O8 -97.6(4) . . . 1_556 ? Li6 Li5 Li6 O8 -35.0(10) 4 . . 1_556 ? O8W Li5 Li6 O9W -1.1(8) . . . . ? O7W Li5 Li6 O9W -91.0(4) . . . . ? O7W Li5 Li6 O9W -143.6(6) 4 . . . ? O15 Li5 Li6 O9W 117.3(6) 4 . . . ? O15 Li5 Li6 O9W 90.1(5) . . . . ? Li6 Li5 Li6 O9W 152.6(6) 4 . . . ? O8W Li5 Li6 O7W 89.9(6) . . . . ? O7W Li5 Li6 O7W -52.7(6) 4 . . . ? O15 Li5 Li6 O7W -151.7(8) 4 . . . ? O15 Li5 Li6 O7W -179.0(6) . . . . ? Li6 Li5 Li6 O7W -116.4(9) 4 . . . ? O8W Li5 Li6 O13 -95.4(7) . . . . ? O7W Li5 Li6 O13 174.8(5) . . . . ? O7W Li5 Li6 O13 122.1(6) 4 . . . ? O15 Li5 Li6 O13 23.1(8) 4 . . . ? O15 Li5 Li6 O13 -4.2(5) . . . . ? Li6 Li5 Li6 O13 58.4(10) 4 . . . ? O8W Li5 Li6 Li7 25.1(11) . . . 1_556 ? O7W Li5 Li6 Li7 -64.8(7) . . . 1_556 ? O7W Li5 Li6 Li7 -117.5(7) 4 . . 1_556 ? O15 Li5 Li6 Li7 143.5(5) 4 . . 1_556 ? O15 Li5 Li6 Li7 116.2(6) . . . 1_556 ? Li6 Li5 Li6 Li7 178.8(3) 4 . . 1_556 ? O4W Li3 S2 O6 30.3(4) . . . . ? O5 Li3 S2 O6 116.7(4) . . . . ? O11 Li3 S2 O6 -73.5(3) . . . . ? O12 Li3 S2 O6 -161.4(5) . . . . ? Li4 Li3 S2 O6 -38.8(3) . . . . ? O4W Li3 S2 O8 24.6(7) . . . . ? O5 Li3 S2 O8 111.0(3) . . . . ? O11 Li3 S2 O8 -79.2(4) . . . . ? O6 Li3 S2 O8 -5.7(5) . . . . ? O12 Li3 S2 O8 -167.2(3) . . . . ? Li4 Li3 S2 O8 -44.5(4) . . . . ? O4W Li3 S2 O7 157.9(4) . . . . ? O5 Li3 S2 O7 -115.6(2) . . . . ? O11 Li3 S2 O7 54.2(3) . . . . ? O6 Li3 S2 O7 127.6(3) . . . . ? O12 Li3 S2 O7 -33.8(3) . . . . ? Li4 Li3 S2 O7 88.8(3) . . . . ? O4W Li3 S2 C4 -95.6(4) . . . . ? O5 Li3 S2 C4 -9.2(2) . . . . ? O11 Li3 S2 C4 160.6(2) . . . . ? O6 Li3 S2 C4 -125.9(3) . . . . ? O12 Li3 S2 C4 72.6(3) . . . . ? Li4 Li3 S2 C4 -164.8(3) . . . . ? O3 S1 O1 Li1 -109.6(7) . . . . ? O2 S1 O1 Li1 129.8(7) . . . . ? C1 S1 O1 Li1 12.9(8) . . . . ? O1W Li1 O1 S1 72.0(13) . . . . ? O4 Li1 O1 S1 2.3(9) . . . . ? O10 Li1 O1 S1 -175.4(6) 6 . . . ? O3 Li1 O1 S1 -89.5(7) 6 . . . ? Li2 Li1 O1 S1 6.2(11) . . . . ? Li7 Li1 O1 S1 149.6(6) 6 . . . ? O4 Li1 O1W Li2 -20.8(5) . . . . ? O1 Li1 O1W Li2 -91.5(11) . . . . ? O10 Li1 O1W Li2 157.3(5) 6 . . . ? O3 Li1 O1W Li2 67.3(6) 6 . . . ? Li7 Li1 O1W Li2 -169.3(5) 6 . . . ? O2W Li2 O1W Li1 -99.1(6) . . . . ? O3W Li2 O1W Li1 143.9(6) . . . . ? O4 Li2 O1W Li1 21.1(5) . . . . ? O5 Li2 O1W Li1 11.1(12) . . . . ? O1 S1 O3 Li1 -160.6(3) . . . 6_554 ? O2 S1 O3 Li1 -37.2(3) . . . 6_554 ? C1 S1 O3 Li1 76.5(3) . . . 6_554 ? O1W Li1 O4 C2 -176.6(6) . . . . ? O1 Li1 O4 C2 -26.4(8) . . . . ? O3 Li1 O4 C2 64.6(7) 6 . . . ? Li2 Li1 O4 C2 158.6(7) . . . . ? Li7 Li1 O4 C2 -105.2(9) 6 . . . ? O1W Li1 O4 Li2 24.8(6) . . . . ? O1 Li1 O4 Li2 174.9(4) . . . . ? O3 Li1 O4 Li2 -94.0(4) 6 . . . ? Li7 Li1 O4 Li2 96.2(9) 6 . . . ? O2W Li2 O4 C2 -97.7(6) . . . . ? O3W Li2 O4 C2 93.8(6) . . . . ? O5 Li2 O4 C2 -9.0(5) . . . . ? O1W Li2 O4 C2 176.6(4) . . . . ? Li1 Li2 O4 C2 -161.9(6) . . . . ? O2W Li2 O4 Li1 64.2(6) . . . . ? O3W Li2 O4 Li1 -104.3(7) . . . . ? O5 Li2 O4 Li1 153.0(4) . . . . ? O1W Li2 O4 Li1 -21.5(5) . . . . ? O4W Li3 O5 C3 142.4(4) . . . . ? O11 Li3 O5 C3 -56(3) . . . . ? O6 Li3 O5 C3 35.2(4) . . . . ? O12 Li3 O5 C3 -106.1(4) . . . . ? S2 Li3 O5 C3 13.4(4) . . . . ? Li4 Li3 O5 C3 89.9(9) . . . . ? O4W Li3 O5 Li2 -41.2(5) . . . . ? O11 Li3 O5 Li2 120(2) . . . . ? O6 Li3 O5 Li2 -148.4(3) . . . . ? O12 Li3 O5 Li2 70.2(4) . . . . ? S2 Li3 O5 Li2 -170.2(3) . . . . ? Li4 Li3 O5 Li2 -93.7(9) . . . . ? O2W Li2 O5 C3 129.9(4) . . . . ? O3W Li2 O5 C3 -109.2(4) . . . . ? O4 Li2 O5 C3 10.2(4) . . . . ? O1W Li2 O5 C3 20.1(11) . . . . ? Li1 Li2 O5 C3 27.4(5) . . . . ? O2W Li2 O5 Li3 -47.1(5) . . . . ? O3W Li2 O5 Li3 73.9(5) . . . . ? O4 Li2 O5 Li3 -166.7(3) . . . . ? O1W Li2 O5 Li3 -156.8(8) . . . . ? Li1 Li2 O5 Li3 -149.5(4) . . . . ? O8 S2 O6 Li3 176.7(3) . . . . ? O7 S2 O6 Li3 -60.5(3) . . . . ? C4 S2 O6 Li3 58.4(3) . . . . ? O4W Li3 O6 S2 -155.9(3) . . . . ? O5 Li3 O6 S2 -59.1(3) . . . . ? O11 Li3 O6 S2 110.2(3) . . . . ? O12 Li3 O6 S2 26.5(7) . . . . ? Li4 Li3 O6 S2 141.2(3) . . . . ? O8W Li5 O7W Li6 -105.5(5) . . . . ? O7W Li5 O7W Li6 145.2(4) 4 . . . ? O15 Li5 O7W Li6 51.0(11) 4 . . . ? O15 Li5 O7W Li6 0.6(4) . . . . ? Li6 Li5 O7W Li6 110.4(6) 4 . . . ? O15 Li6 O7W Li5 -0.7(4) . . . . ? O9 Li6 O7W Li5 176.6(4) 1_556 . . . ? O8 Li6 O7W Li5 -100.1(4) 1_556 . . . ? O9W Li6 O7W Li5 94.9(4) . . . . ? O13 Li6 O7W Li5 -17.1(16) . . . . ? Li7 Li6 O7W Li5 136.2(5) 1_556 . . . ? O6 S2 O8 Li6 -171.6(3) . . . 1_554 ? O7 S2 O8 Li6 61.6(3) . . . 1_554 ? C4 S2 O8 Li6 -53.1(4) . . . 1_554 ? Li3 S2 O8 Li6 -168.0(3) . . . 1_554 ? O11W Li7 O9 C5 68.9(10) . . . . ? O10W Li7 O9 C5 -104.3(4) . . . . ? O10 Li7 O9 C5 1.2(4) . . . . ? O9W Li7 O9 C5 161.2(3) 1_554 . . . ? Li6 Li7 O9 C5 151.3(4) 1_554 . . . ? Li1 Li7 O9 C5 10.0(5) 6_554 . . . ? O11W Li7 O9 Li6 -82.4(10) . . . 1_554 ? O10W Li7 O9 Li6 104.4(4) . . . 1_554 ? O10 Li7 O9 Li6 -150.0(3) . . . 1_554 ? O9W Li7 O9 Li6 9.9(3) 1_554 . . 1_554 ? Li1 Li7 O9 Li6 -141.2(4) 6_554 . . 1_554 ? O15 Li6 O9W Li7 -167.2(4) . . . 1_556 ? O9 Li6 O9W Li7 9.3(3) 1_556 . . 1_556 ? O8 Li6 O9W Li7 -0.2(19) 1_556 . . 1_556 ? O7W Li6 O9W Li7 109.6(3) . . . 1_556 ? O13 Li6 O9W Li7 -84.0(3) . . . 1_556 ? Li5 Li6 O9W Li7 151.3(4) . . . 1_556 ? O11W Li7 O10 C6 -156.3(4) . . . . ? O10W Li7 O10 C6 100.4(4) . . . . ? O9 Li7 O10 C6 -6.7(4) . . . . ? O9W Li7 O10 C6 -48.9(10) 1_554 . . . ? Li6 Li7 O10 C6 -26.2(5) 1_554 . . . ? Li1 Li7 O10 C6 -172.5(5) 6_554 . . . ? O11W Li7 O10 Li1 16.2(5) . . . 6_554 ? O10W Li7 O10 Li1 -87.1(5) . . . 6_554 ? O9 Li7 O10 Li1 165.8(4) . . . 6_554 ? O9W Li7 O10 Li1 123.6(9) 1_554 . . 6_554 ? Li6 Li7 O10 Li1 146.3(5) 1_554 . . 6_554 ? O5W Li4 O11 C7 126.6(4) . . . . ? O6W Li4 O11 C7 -101.1(5) . . . . ? O11 Li4 O11 C7 20.4(6) 4 . . . ? C7 Li4 O11 C7 10.4(3) 4 . . . ? Li3 Li4 O11 C7 179.2(5) . . . . ? Li3 Li4 O11 C7 33.4(7) 4 . . . ? O5W Li4 O11 Li3 -52.6(5) . . . . ? O6W Li4 O11 Li3 79.7(7) . . . . ? O11 Li4 O11 Li3 -158.7(3) 4 . . . ? C7 Li4 O11 Li3 -168.8(3) 4 . . . ? C7 Li4 O11 Li3 -179.2(5) . . . . ? Li3 Li4 O11 Li3 -145.7(5) 4 . . . ? O4W Li3 O11 C7 138.0(4) . . . . ? O5 Li3 O11 C7 -24(3) . . . . ? O6 Li3 O11 C7 -114.0(4) . . . . ? O12 Li3 O11 C7 27.1(5) . . . . ? S2 Li3 O11 C7 -90.6(5) . . . . ? Li4 Li3 O11 C7 -178.9(7) . . . . ? O4W Li3 O11 Li4 -43.1(6) . . . . ? O5 Li3 O11 Li4 155(3) . . . . ? O6 Li3 O11 Li4 64.9(5) . . . . ? O12 Li3 O11 Li4 -154.0(5) . . . . ? S2 Li3 O11 Li4 88.3(5) . . . . ? O14 S3 O12 Li3 -76.5(3) . . . . ? O13 S3 O12 Li3 159.4(3) . . . . ? C8 S3 O12 Li3 42.3(4) . . . . ? O4W Li3 O12 S3 -132.3(4) . . . . ? O5 Li3 O12 S3 128.8(3) . . . . ? O11 Li3 O12 S3 -43.0(4) . . . . ? O6 Li3 O12 S3 45.3(7) . . . . ? S2 Li3 O12 S3 57.4(4) . . . . ? Li4 Li3 O12 S3 -58.4(5) . . . . ? O14 S3 O13 Li6 56.3(3) . . . . ? O12 S3 O13 Li6 -177.5(2) . . . . ? C8 S3 O13 Li6 -59.9(2) . . . . ? O15 Li6 O13 S3 30.9(3) . . . . ? O9 Li6 O13 S3 -146.1(2) 1_556 . . . ? O8 Li6 O13 S3 130.2(2) 1_556 . . . ? O9W Li6 O13 S3 -65.8(3) . . . . ? O7W Li6 O13 S3 47.3(17) . . . . ? Li5 Li6 O13 S3 33.7(5) . . . . ? Li7 Li6 O13 S3 -107.4(2) 1_556 . . . ? O8 Li6 O15 C9 -67.3(6) 1_556 . . . ? O9W Li6 O15 C9 109.1(4) . . . . ? O7W Li6 O15 C9 -154.6(4) . . . . ? O13 Li6 O15 C9 21.2(6) . . . . ? Li5 Li6 O15 C9 -155.3(6) . . . . ? Li7 Li6 O15 C9 96.7(6) 1_556 . . . ? O8 Li6 O15 Li5 88.0(5) 1_556 . . . ? O9W Li6 O15 Li5 -95.6(5) . . . . ? O7W Li6 O15 Li5 0.7(4) . . . . ? O13 Li6 O15 Li5 176.5(4) . . . . ? Li7 Li6 O15 Li5 -108.0(6) 1_556 . . . ? O8W Li5 O15 C9 -95.6(4) . . . . ? O7W Li5 O15 C9 160.9(3) . . . . ? O7W Li5 O15 C9 60.6(13) 4 . . . ? O15 Li5 O15 C9 8.3(6) 4 . . . ? Li6 Li5 O15 C9 25.3(7) 4 . . . ? Li6 Li5 O15 C9 161.7(5) . . . . ? O8W Li5 O15 Li6 102.7(5) . . . . ? O7W Li5 O15 Li6 -0.7(4) . . . . ? O7W Li5 O15 Li6 -101.0(10) 4 . . . ? O15 Li5 O15 Li6 -153.3(3) 4 . . . ? Li6 Li5 O15 Li6 -136.4(5) 4 . . . ? O1 S1 C1 C2 -16.5(5) . . . . ? O3 S1 C1 C2 110.9(4) . . . . ? O2 S1 C1 C2 -136.0(5) . . . . ? O1 S1 C1 C6 166.9(4) . . . . ? O3 S1 C1 C6 -65.7(4) . . . . ? O2 S1 C1 C6 47.3(5) . . . . ? Li1 O4 C2 C1 29.1(8) . . . . ? Li2 O4 C2 C1 -175.3(5) . . . . ? Li1 O4 C2 C3 -149.0(6) . . . . ? Li2 O4 C2 C3 6.6(5) . . . . ? C6 C1 C2 O4 174.2(4) . . . . ? S1 C1 C2 O4 -2.1(6) . . . . ? C6 C1 C2 C3 -7.8(6) . . . . ? S1 C1 C2 C3 175.8(3) . . . . ? Li3 O5 C3 C4 -13.3(6) . . . . ? Li2 O5 C3 C4 170.3(4) . . . . ? Li3 O5 C3 C2 166.4(3) . . . . ? Li2 O5 C3 C2 -10.0(5) . . . . ? O4 C2 C3 O5 3.0(4) . . . . ? C1 C2 C3 O5 -175.2(4) . . . . ? O4 C2 C3 C4 -177.3(4) . . . . ? C1 C2 C3 C4 4.6(4) . . . . ? O5 C3 C4 C5 177.6(4) . . . . ? C2 C3 C4 C5 -2.2(5) . . . . ? O5 C3 C4 S2 -1.3(5) . . . . ? C2 C3 C4 S2 179.0(2) . . . . ? O6 S2 C4 C5 158.8(3) . . . . ? O8 S2 C4 C5 38.4(3) . . . . ? O7 S2 C4 C5 -77.2(4) . . . . ? Li3 S2 C4 C5 -170.8(3) . . . . ? O6 S2 C4 C3 -22.3(4) . . . . ? O8 S2 C4 C3 -142.7(3) . . . . ? O7 S2 C4 C3 101.7(4) . . . . ? Li3 S2 C4 C3 8.1(3) . . . . ? Li6 O9 C5 C4 -39.4(7) 1_554 . . . ? Li7 O9 C5 C4 -179.7(4) . . . . ? Li6 O9 C5 C6 143.3(4) 1_554 . . . ? Li7 O9 C5 C6 3.0(4) . . . . ? C3 C4 C5 O9 -174.3(4) . . . . ? S2 C4 C5 O9 4.5(6) . . . . ? C3 C4 C5 C6 2.7(5) . . . . ? S2 C4 C5 C6 -178.4(2) . . . . ? Li7 O10 C6 C1 -170.6(4) . . . . ? Li1 O10 C6 C1 19.1(8) 6_554 . . . ? Li7 O10 C6 C5 9.9(4) . . . . ? Li1 O10 C6 C5 -160.4(5) 6_554 . . . ? C2 C1 C6 O10 -171.3(4) . . . . ? S1 C1 C6 O10 5.4(6) . . . . ? C2 C1 C6 C5 8.2(5) . . . . ? S1 C1 C6 C5 -175.2(3) . . . . ? O9 C5 C6 O10 -8.6(4) . . . . ? C4 C5 C6 O10 174.0(4) . . . . ? O9 C5 C6 C1 171.9(4) . . . . ? C4 C5 C6 C1 -5.6(4) . . . . ? Li4 O11 C7 C8 166.1(5) . . . . ? Li3 O11 C7 C8 -15.0(7) . . . . ? Li4 O11 C7 C7 -17.0(5) . . . 4 ? Li3 O11 C7 C7 161.9(4) . . . 4 ? Li3 O11 C7 Li4 178.9(7) . . . . ? O5W Li4 C7 O11 -63.4(4) . . . . ? O6W Li4 C7 O11 95.1(4) . . . . ? O11 Li4 C7 O11 -155.8(7) 4 . . . ? C7 Li4 C7 O11 -163.8(5) 4 . . . ? Li3 Li4 C7 O11 -0.6(3) . . . . ? Li3 Li4 C7 O11 -149.4(6) 4 . . . ? O5W Li4 C7 C8 -108.9(15) . . . . ? O6W Li4 C7 C8 49.6(15) . . . . ? O11 Li4 C7 C8 -45.4(16) . . . . ? O11 Li4 C7 C8 158.8(13) 4 . . . ? C7 Li4 C7 C8 150.7(13) 4 . . . ? Li3 Li4 C7 C8 -46.0(15) . . . . ? Li3 Li4 C7 C8 165.2(13) 4 . . . ? O5W Li4 C7 C7 100.4(3) . . . 4 ? O6W Li4 C7 C7 -101.1(3) . . . 4 ? O11 Li4 C7 C7 163.8(5) . . . 4 ? O11 Li4 C7 C7 8.0(2) 4 . . 4 ? Li3 Li4 C7 C7 163.3(2) . . . 4 ? Li3 Li4 C7 C7 14.4(2) 4 . . 4 ? O11 C7 C8 C9 176.9(3) . . . . ? C7 C7 C8 C9 0.3(4) 4 . . . ? Li4 C7 C8 C9 -147.0(13) . . . . ? O11 C7 C8 S3 2.2(6) . . . . ? C7 C7 C8 S3 -174.50(17) 4 . . . ? Li4 C7 C8 S3 38.3(16) . . . . ? O14 S3 C8 C9 -66.6(4) . . . . ? O12 S3 C8 C9 170.4(3) . . . . ? O13 S3 C8 C9 51.3(3) . . . . ? O14 S3 C8 C7 108.2(3) . . . . ? O12 S3 C8 C7 -14.8(4) . . . . ? O13 S3 C8 C7 -133.8(3) . . . . ? Li6 O15 C9 C8 -34.8(7) . . . . ? Li5 O15 C9 C8 172.7(5) . . . . ? Li6 O15 C9 C9 145.2(4) . . . 4 ? Li5 O15 C9 C9 -7.3(5) . . . 4 ? C7 C8 C9 O15 179.8(3) . . . . ? S3 C8 C9 O15 -5.2(5) . . . . ? C7 C8 C9 C9 -0.3(4) . . . 4 ? S3 C8 C9 C9 174.77(15) . . . 4 ? 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 O1W H1W1 O3W 0.85(6) 2.33(8) 3.101(6) 152(15) . O1W H1W1 O2W 0.85(6) 2.57(12) 3.130(10) 125(12) . O1W H1W2 O3 0.85(6) 2.34(16) 2.869(7) 121(15) 3 O2W H2W1 O2 0.84(5) 2.24(3) 2.990(5) 149(5) 6 O2W H2W2 O12 0.85(6) 2.27(4) 2.852(4) 126(4) . O2W H2W2 O3W 0.85(6) 2.65(4) 3.134(5) 118(3) 3 O3W H3W1 O1 0.85(6) 2.26(3) 3.061(6) 156(5) 8_545 O3W H3W2 O13 0.85(6) 2.17(3) 2.942(4) 150(6) 3_554 O4W H4W1 O8 0.85(6) 2.089(12) 2.935(5) 175(6) 3 O4W H4W2 O5 0.85(6) 2.37(5) 2.961(5) 128(5) . O5W H5W O6 0.86(6) 2.062(7) 2.916(3) 174.5(17) . O6W H6W O8 0.85 1.98 2.832(3) 175.9 2 O7W H7W1 O14 0.85(6) 2.11(3) 2.847(4) 145(5) 3_565 O7W H7W2 O7 0.85(6) 2.39(3) 3.123(6) 144(4) 1_556 O8W H8W O7 0.85(6) 2.12(5) 2.722(4) 128(6) 2_565 O9W H9W1 O7 0.85(6) 1.97(3) 2.734(5) 150(5) 3_565 O9W H9W2 O14 0.85(6) 2.13(3) 2.902(5) 151(6) . O10W HAW2 O3 0.85(6) 2.36(7) 2.935(5) 125(7) 8 O10W HAW1 O14 0.85(6) 2.04(4) 2.839(4) 155(8) 3_564 O11W HBW2 O9W 0.85(6) 2.58(11) 3.172(11) 127(12) 1_554 O11W HBW1 O1 0.85(6) 2.06(8) 2.822(8) 147(12) 6_554 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.454 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.073 # Attachment 'complex 4.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 852888' #TrackingRef 'complex 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H4 Li O8 S2, H4 N' _chemical_formula_sum 'C6 H8 Li N O8 S2' _chemical_formula_weight 293.19 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C mca ' _symmetry_space_group_name_Hall '-C 2bc 2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 18.130(4) _cell_length_b 9.0962(18) _cell_length_c 13.786(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2273.5(8) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 8982 _cell_measurement_theta_min 3.72 _cell_measurement_theta_max 27.41 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.500 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9154 _exptl_absorpt_correction_T_max 0.9379 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10568 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0128 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 27.42 _reflns_number_total 1337 _reflns_number_gt 1236 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0611P)^2^+1.2832P] 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 1337 _refine_ls_number_parameters 95 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0922 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.083 _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 0.2500 0.4347(3) 0.7500 0.0259(7) Uani 1 2 d S . . S1 S 0.148679(17) 0.68790(3) 0.69272(2) 0.02040(15) Uani 1 1 d . . . O1 O 0.18796(5) 0.55350(11) 0.66681(7) 0.0301(3) Uani 1 1 d . . . O2 O 0.19025(6) 0.81787(10) 0.66362(8) 0.0314(3) Uani 1 1 d . . . O3 O 0.12672(7) 0.69008(11) 0.79374(8) 0.0320(3) Uani 1 1 d . . . O4 O 0.13282(6) 0.70543(13) 0.47722(8) 0.0334(3) Uani 1 1 d D . . H4O H 0.1289(14) 0.723(2) 0.4176(8) 0.050 Uiso 1 1 d D . . N1 N 0.27526(11) 0.5000 0.5000 0.0355(4) Uani 1 2 d SD . . H1N1 H 0.2448(9) 0.5334(19) 0.5430(13) 0.053 Uiso 1 1 d D . . H1N2 H 0.2994(10) 0.5735(16) 0.4781(14) 0.053 Uiso 1 1 d D . . C1 C 0.06656(7) 0.68891(13) 0.62456(10) 0.0213(3) Uani 1 1 d . . . C2 C 0.06657(7) 0.69925(14) 0.52261(10) 0.0237(3) Uani 1 1 d . . . C3 C 0.0000 0.7030(2) 0.47254(14) 0.0266(4) Uani 1 2 d S . . H3 H 0.0000 0.7080 0.4052 0.032 Uiso 1 2 calc SR . . C4 C 0.0000 0.68289(19) 0.67355(14) 0.0227(4) Uani 1 2 d S . . H4 H 0.0000 0.6746 0.7408 0.027 Uiso 1 2 calc SR . . 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 0.0268(15) 0.0295(16) 0.0213(15) 0.000 -0.0006(11) 0.000 S1 0.0178(2) 0.0284(2) 0.0150(2) 0.00017(10) -0.00154(10) -0.00050(10) O1 0.0302(5) 0.0343(5) 0.0257(5) -0.0007(4) -0.0052(4) 0.0093(4) O2 0.0315(6) 0.0353(6) 0.0273(6) 0.0039(4) -0.0056(4) -0.0104(4) O3 0.0278(5) 0.0522(7) 0.0159(5) -0.0020(4) -0.0005(4) -0.0017(4) O4 0.0204(5) 0.0638(7) 0.0162(5) 0.0032(4) 0.0028(4) 0.0010(4) N1 0.0366(10) 0.0422(10) 0.0276(9) 0.0108(8) 0.000 0.000 C1 0.0176(6) 0.0301(6) 0.0162(6) 0.0001(4) -0.0014(4) 0.0002(4) C2 0.0208(6) 0.0334(7) 0.0168(7) 0.0008(4) 0.0019(5) 0.0006(5) C3 0.0250(9) 0.0412(10) 0.0135(8) 0.0017(7) 0.000 0.000 C4 0.0211(9) 0.0324(9) 0.0145(8) 0.0004(6) 0.000 0.000 _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 O2 1.9291(19) 16_545 ? Li1 O2 1.9291(19) 10_557 ? Li1 O1 1.9359(19) 7_546 ? Li1 O1 1.9359(19) . ? Li1 S1 3.006(2) 10_557 ? Li1 S1 3.006(2) 16_545 ? Li1 S1 3.050(2) 7_546 ? Li1 S1 3.050(2) . ? S1 O3 1.4486(11) . ? S1 O2 1.4583(10) . ? S1 O1 1.4593(10) . ? S1 C1 1.7606(13) . ? S1 Li1 3.006(2) 10_567 ? O2 Li1 1.9291(19) 10_567 ? O4 C2 1.3555(17) . ? O4 H4O 0.84(2) . ? N1 H1N1 0.86(2) . ? N1 H1N2 0.85(2) . ? C1 C4 1.3839(16) . ? C1 C2 1.4087(18) . ? C2 C3 1.3907(16) . ? C3 C2 1.3907(16) 12 ? C3 H3 0.9300 . ? C4 C1 1.3839(16) 12 ? C4 H4 0.9300 . ? 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 O2 Li1 O2 113.12(16) 16_545 10_557 ? O2 Li1 O1 110.30(5) 16_545 7_546 ? O2 Li1 O1 105.55(5) 10_557 7_546 ? O2 Li1 O1 105.55(5) 16_545 . ? O2 Li1 O1 110.30(5) 10_557 . ? O1 Li1 O1 112.15(15) 7_546 . ? O2 Li1 S1 95.38(11) 16_545 10_557 ? O2 Li1 S1 23.55(5) 10_557 10_557 ? O1 Li1 S1 128.04(5) 7_546 10_557 ? O1 Li1 S1 102.55(5) . 10_557 ? O2 Li1 S1 23.55(5) 16_545 16_545 ? O2 Li1 S1 95.38(11) 10_557 16_545 ? O1 Li1 S1 102.55(5) 7_546 16_545 ? O1 Li1 S1 128.04(5) . 16_545 ? S1 Li1 S1 83.37(8) 10_557 16_545 ? O2 Li1 S1 103.75(5) 16_545 7_546 ? O2 Li1 S1 126.47(5) 10_557 7_546 ? O1 Li1 S1 22.37(5) 7_546 7_546 ? O1 Li1 S1 94.70(11) . 7_546 ? S1 Li1 S1 149.759(14) 10_557 7_546 ? S1 Li1 S1 105.302(18) 16_545 7_546 ? O2 Li1 S1 126.47(5) 16_545 . ? O2 Li1 S1 103.75(5) 10_557 . ? O1 Li1 S1 94.70(11) 7_546 . ? O1 Li1 S1 22.37(5) . . ? S1 Li1 S1 105.302(17) 10_557 . ? S1 Li1 S1 149.759(14) 16_545 . ? S1 Li1 S1 81.93(7) 7_546 . ? O3 S1 O2 113.30(6) . . ? O3 S1 O1 112.39(6) . . ? O2 S1 O1 111.07(7) . . ? O3 S1 C1 106.29(7) . . ? O2 S1 C1 106.62(6) . . ? O1 S1 C1 106.64(6) . . ? O3 S1 Li1 84.56(5) . 10_567 ? O1 S1 Li1 113.06(6) . 10_567 ? C1 S1 Li1 130.77(5) . 10_567 ? O3 S1 Li1 85.81(5) . . ? O2 S1 Li1 111.84(6) . . ? C1 S1 Li1 130.65(5) . . ? Li1 S1 Li1 97.348(17) 10_567 . ? S1 O1 Li1 127.31(8) . . ? S1 O2 Li1 124.55(9) . 10_567 ? C2 O4 H4O 112.6(17) . . ? H1N1 N1 H1N2 107.1(12) . . ? C4 C1 C2 119.32(13) . . ? C4 C1 S1 118.47(11) . . ? C2 C1 S1 122.19(10) . . ? O4 C2 C3 122.61(12) . . ? O4 C2 C1 117.61(12) . . ? C3 C2 C1 119.78(13) . . ? C2 C3 C2 120.40(17) 12 . ? C2 C3 H3 119.8 12 . ? C2 C3 H3 119.8 . . ? C1 C4 C1 121.37(17) 12 . ? C1 C4 H4 119.3 12 . ? C1 C4 H4 119.3 . . ? 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 O2 Li1 S1 O3 174.87(11) 16_545 . . . ? O2 Li1 S1 O3 41.73(8) 10_557 . . . ? O1 Li1 S1 O3 -65.55(6) 7_546 . . . ? O1 Li1 S1 O3 151.85(11) . . . . ? S1 Li1 S1 O3 66.02(5) 10_557 . . . ? S1 Li1 S1 O3 169.42(14) 16_545 . . . ? S1 Li1 S1 O3 -83.96(5) 7_546 . . . ? O2 Li1 S1 O2 -71.69(11) 16_545 . . . ? O2 Li1 S1 O2 155.18(6) 10_557 . . . ? O1 Li1 S1 O2 47.90(6) 7_546 . . . ? O1 Li1 S1 O2 -94.70(11) . . . . ? S1 Li1 S1 O2 179.46(6) 10_557 . . . ? S1 Li1 S1 O2 -77.13(14) 16_545 . . . ? S1 Li1 S1 O2 29.49(5) 7_546 . . . ? O2 Li1 S1 O1 23.02(10) 16_545 . . . ? O2 Li1 S1 O1 -110.12(14) 10_557 . . . ? O1 Li1 S1 O1 142.60(10) 7_546 . . . ? S1 Li1 S1 O1 -85.83(11) 10_557 . . . ? S1 Li1 S1 O1 17.57(11) 16_545 . . . ? S1 Li1 S1 O1 124.19(10) 7_546 . . . ? O2 Li1 S1 C1 66.93(13) 16_545 . . . ? O2 Li1 S1 C1 -66.20(8) 10_557 . . . ? O1 Li1 S1 C1 -173.48(7) 7_546 . . . ? O1 Li1 S1 C1 43.92(11) . . . . ? S1 Li1 S1 C1 -41.92(6) 10_557 . . . ? S1 Li1 S1 C1 61.49(15) 16_545 . . . ? S1 Li1 S1 C1 168.11(6) 7_546 . . . ? O2 Li1 S1 Li1 -101.17(10) 16_545 . . 10_567 ? O2 Li1 S1 Li1 125.69(6) 10_557 . . 10_567 ? O1 Li1 S1 Li1 18.41(4) 7_546 . . 10_567 ? O1 Li1 S1 Li1 -124.19(10) . . . 10_567 ? S1 Li1 S1 Li1 149.98(3) 10_557 . . 10_567 ? S1 Li1 S1 Li1 -106.62(13) 16_545 . . 10_567 ? S1 Li1 S1 Li1 0.0 7_546 . . 10_567 ? O3 S1 O1 Li1 -30.59(12) . . . . ? O2 S1 O1 Li1 97.52(11) . . . . ? C1 S1 O1 Li1 -146.68(9) . . . . ? Li1 S1 O1 Li1 63.08(9) 10_567 . . . ? O2 Li1 O1 S1 -160.95(9) 16_545 . . . ? O2 Li1 O1 S1 76.53(15) 10_557 . . . ? O1 Li1 O1 S1 -40.81(7) 7_546 . . . ? S1 Li1 O1 S1 99.75(11) 10_557 . . . ? S1 Li1 O1 S1 -168.87(8) 16_545 . . . ? S1 Li1 O1 S1 -55.26(8) 7_546 . . . ? O3 S1 O2 Li1 27.52(12) . . . 10_567 ? O1 S1 O2 Li1 -100.10(10) . . . 10_567 ? C1 S1 O2 Li1 144.09(10) . . . 10_567 ? Li1 S1 O2 Li1 -67.47(9) . . . 10_567 ? O3 S1 C1 C4 -3.65(13) . . . . ? O2 S1 C1 C4 -124.80(12) . . . . ? O1 S1 C1 C4 116.46(12) . . . . ? Li1 S1 C1 C4 -100.63(11) 10_567 . . . ? Li1 S1 C1 C4 95.02(12) . . . . ? O3 S1 C1 C2 174.76(10) . . . . ? O2 S1 C1 C2 53.61(12) . . . . ? O1 S1 C1 C2 -65.14(11) . . . . ? Li1 S1 C1 C2 77.77(11) 10_567 . . . ? Li1 S1 C1 C2 -86.57(11) . . . . ? C4 C1 C2 O4 179.77(13) . . . . ? S1 C1 C2 O4 1.38(16) . . . . ? C4 C1 C2 C3 -0.1(2) . . . . ? S1 C1 C2 C3 -178.52(12) . . . . ? O4 C2 C3 C2 -178.72(10) . . . 12 ? C1 C2 C3 C2 1.2(3) . . . 12 ? C2 C1 C4 C1 -0.9(2) . . . 12 ? S1 C1 C4 C1 177.52(9) . . . 12 ? 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 O4 H4O O3 0.84(2) 1.88(2) 2.704(2) 166(2) 11_575 N1 H1N1 O1 0.86(2) 2.00(2) 2.834(2) 160.8(19) . N1 H1N2 O2 0.85(2) 2.20(2) 2.868(2) 135.3(18) 13_566 N1 H1N2 O4 0.85(2) 2.44(2) 3.171(2) 144.6(17) 13_566 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.470 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.084 # Attachment 'complex 5.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 852889' #TrackingRef 'complex 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H6 Li2 O9 S2, H2 O' _chemical_formula_sum 'C6 H8 Li2 O10 S2' _chemical_formula_weight 318.12 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' S S 0.1246 0.1234 '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 7.7858(16) _cell_length_b 8.8783(18) _cell_length_c 9.1955(18) _cell_angle_alpha 83.00(3) _cell_angle_beta 66.68(3) _cell_angle_gamma 75.45(3) _cell_volume 564.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4823 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.44 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 324 _exptl_absorpt_coefficient_mu 0.520 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8987 _exptl_absorpt_correction_T_max 0.9403 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5578 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2557 _reflns_number_gt 2222 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0559P)^2^+0.5686P] 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 2557 _refine_ls_number_parameters 199 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.1018 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.2809(6) -0.1334(5) 0.9439(5) 0.0296(8) Uani 1 1 d . . . Li2 Li 0.2229(6) 0.5351(4) 0.9911(4) 0.0230(7) Uani 1 1 d . . . S1 S 0.14097(7) 0.22874(5) 0.88711(5) 0.01515(14) Uani 1 1 d . . . S2 S 0.36810(7) 0.42698(5) 0.26867(5) 0.01683(14) Uani 1 1 d . . . O1 O 0.2348(2) 0.09903(18) 0.96069(18) 0.0246(3) Uani 1 1 d . . . O1W O 0.3856(2) -0.17662(17) 1.12430(19) 0.0242(3) Uani 1 1 d D . . H1W2 H 0.353(3) -0.248(3) 1.192(3) 0.036 Uiso 1 1 d D . . H1W1 H 0.5075(15) -0.194(3) 1.081(3) 0.036 Uiso 1 1 d D . . O2 O 0.1951(3) 0.37323(19) 0.89004(19) 0.0307(4) Uani 1 1 d . . . O2W O 0.0980(3) -0.2952(2) 0.6516(2) 0.0415(5) Uani 1 1 d D . . H2W2 H 0.162(4) -0.338(4) 0.563(2) 0.062 Uiso 1 1 d D . . H2W1 H 0.005(4) -0.338(4) 0.704(3) 0.062 Uiso 1 1 d D . . O3 O -0.0672(2) 0.24952(18) 0.95322(18) 0.0235(3) Uani 1 1 d . . . O4 O 0.1790(3) -0.07032(18) 0.75355(18) 0.0265(4) Uani 1 1 d D . . H4O H 0.149(4) -0.141(3) 0.720(4) 0.040 Uiso 1 1 d D . . O5 O 0.3446(3) 0.56601(17) 0.34987(19) 0.0297(4) Uani 1 1 d . . . O6 O 0.2279(2) 0.44502(19) 0.19534(19) 0.0285(4) Uani 1 1 d . . . O7 O 0.5632(2) 0.37470(18) 0.15529(18) 0.0252(3) Uani 1 1 d . . . O8 O 0.3869(3) 0.10635(18) 0.21132(18) 0.0284(4) Uani 1 1 d D . . H8O H 0.373(5) 0.019(2) 0.196(4) 0.043 Uiso 1 1 d D . . C1 C 0.2204(3) 0.1881(2) 0.6853(2) 0.0154(4) Uani 1 1 d . . . C2 C 0.2233(3) 0.0417(2) 0.6403(2) 0.0178(4) Uani 1 1 d . . . C3 C 0.2779(3) 0.0131(2) 0.4809(2) 0.0199(4) Uani 1 1 d . . . H3 H 0.2813 -0.0840 0.4504 0.024 Uiso 1 1 calc R . . C4 C 0.3273(3) 0.1298(2) 0.3673(2) 0.0178(4) Uani 1 1 d . . . C5 C 0.3213(3) 0.2770(2) 0.4131(2) 0.0169(4) Uani 1 1 d . . . C6 C 0.2711(3) 0.3037(2) 0.5716(2) 0.0166(4) Uani 1 1 d . . . H6 H 0.2714 0.3999 0.6018 0.020 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 Li1 0.036(2) 0.029(2) 0.026(2) 0.0042(16) -0.0115(17) -0.0160(17) Li2 0.0264(18) 0.0210(17) 0.0224(18) -0.0027(14) -0.0081(15) -0.0078(15) S1 0.0193(3) 0.0146(2) 0.0109(2) -0.00032(16) -0.00427(18) -0.00509(18) S2 0.0223(3) 0.0144(2) 0.0120(2) 0.00191(17) -0.00401(19) -0.00630(19) O1 0.0289(8) 0.0260(8) 0.0198(7) 0.0001(6) -0.0136(7) -0.0007(7) O1W 0.0305(8) 0.0193(7) 0.0248(8) 0.0026(6) -0.0121(7) -0.0078(7) O2 0.0506(11) 0.0271(8) 0.0182(8) -0.0029(6) -0.0081(7) -0.0225(8) O2W 0.0439(11) 0.0374(10) 0.0413(11) -0.0128(8) -0.0032(9) -0.0218(9) O3 0.0189(7) 0.0248(8) 0.0202(7) 0.0011(6) -0.0029(6) -0.0019(6) O4 0.0480(10) 0.0196(7) 0.0173(7) 0.0053(6) -0.0124(7) -0.0197(7) O5 0.0489(10) 0.0168(7) 0.0204(8) -0.0006(6) -0.0065(7) -0.0133(7) O6 0.0321(9) 0.0320(9) 0.0251(8) 0.0110(7) -0.0159(7) -0.0110(7) O7 0.0233(8) 0.0258(8) 0.0201(8) 0.0010(6) 0.0007(6) -0.0102(6) O8 0.0542(11) 0.0194(7) 0.0132(7) -0.0007(6) -0.0100(7) -0.0155(7) C1 0.0198(9) 0.0163(9) 0.0104(8) 0.0008(7) -0.0046(7) -0.0069(7) C2 0.0220(10) 0.0156(9) 0.0165(9) 0.0020(7) -0.0074(8) -0.0064(8) C3 0.0305(11) 0.0139(9) 0.0152(9) -0.0004(7) -0.0068(8) -0.0078(8) C4 0.0217(10) 0.0184(9) 0.0124(9) 0.0004(7) -0.0050(7) -0.0058(8) C5 0.0223(10) 0.0142(9) 0.0131(9) 0.0028(7) -0.0060(7) -0.0047(8) C6 0.0207(10) 0.0131(8) 0.0151(9) -0.0007(7) -0.0042(7) -0.0061(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 Li1 O1 2.018(4) . ? Li1 O3 2.026(4) 2_557 ? Li1 O1W 2.079(4) . ? Li1 O4 2.155(4) . ? Li1 O7 2.278(5) 2_656 ? Li1 O8 2.468(5) 2_656 ? Li1 Li2 3.043(5) 1_545 ? Li2 O2 1.902(4) . ? Li2 O6 1.961(4) 1_556 ? Li2 O7 1.964(4) 2_666 ? Li2 O3 1.993(4) 2_567 ? Li2 S1 2.958(4) 2_567 ? Li2 Li1 3.043(5) 1_565 ? S1 O1 1.4477(16) . ? S1 O2 1.4536(16) . ? S1 O3 1.4589(16) . ? S1 C1 1.761(2) . ? S1 Li2 2.958(4) 2_567 ? S2 O5 1.4552(16) . ? S2 O7 1.4561(17) . ? S2 O6 1.4627(17) . ? S2 C5 1.760(2) . ? O1W H1W2 0.84(4) . ? O1W H1W1 0.85(4) . ? O2W H2W2 0.85(4) . ? O2W H2W1 0.85(4) . ? O3 Li2 1.993(4) 2_567 ? O3 Li1 2.026(4) 2_557 ? O4 C2 1.352(2) . ? O4 H4O 0.85(4) . ? O6 Li2 1.961(4) 1_554 ? O7 Li2 1.964(4) 2_666 ? O7 Li1 2.278(5) 2_656 ? O8 C4 1.347(2) . ? O8 Li1 2.468(5) 2_656 ? O8 H8O 0.85(4) . ? C1 C6 1.385(3) . ? C1 C2 1.404(3) . ? C2 C3 1.391(3) . ? C3 C4 1.389(3) . ? C3 H3 0.9300 . ? C4 C5 1.406(3) . ? C5 C6 1.386(3) . ? C6 H6 0.9300 . ? 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 O1 Li1 O3 122.1(2) . 2_557 ? O1 Li1 O1W 92.01(18) . . ? O3 Li1 O1W 96.55(18) 2_557 . ? O1 Li1 O4 83.68(16) . . ? O3 Li1 O4 87.41(17) 2_557 . ? O1W Li1 O4 175.3(2) . . ? O1 Li1 O7 157.3(2) . 2_656 ? O3 Li1 O7 79.62(15) 2_557 2_656 ? O1W Li1 O7 91.75(17) . 2_656 ? O4 Li1 O7 91.50(17) . 2_656 ? O1 Li1 O8 82.25(15) . 2_656 ? O3 Li1 O8 155.7(2) 2_557 2_656 ? O1W Li1 O8 81.01(15) . 2_656 ? O4 Li1 O8 96.44(16) . 2_656 ? O7 Li1 O8 76.28(14) 2_656 2_656 ? O1 Li1 Li2 162.3(2) . 1_545 ? O3 Li1 Li2 40.37(12) 2_557 1_545 ? O1W Li1 Li2 88.63(16) . 1_545 ? O4 Li1 Li2 96.06(16) . 1_545 ? O7 Li1 Li2 40.20(10) 2_656 1_545 ? O8 Li1 Li2 115.31(18) 2_656 1_545 ? O2 Li2 O6 105.38(19) . 1_556 ? O2 Li2 O7 109.7(2) . 2_666 ? O6 Li2 O7 119.5(2) 1_556 2_666 ? O2 Li2 O3 131.9(2) . 2_567 ? O6 Li2 O3 102.68(18) 1_556 2_567 ? O7 Li2 O3 88.53(16) 2_666 2_567 ? O2 Li2 S1 111.04(17) . 2_567 ? O6 Li2 S1 98.05(15) 1_556 2_567 ? O7 Li2 S1 112.52(16) 2_666 2_567 ? O3 Li2 S1 26.03(7) 2_567 2_567 ? O2 Li2 Li1 143.2(2) . 1_565 ? O6 Li2 Li1 111.30(17) 1_556 1_565 ? O7 Li2 Li1 48.45(13) 2_666 1_565 ? O3 Li2 Li1 41.19(12) 2_567 1_565 ? S1 Li2 Li1 66.93(12) 2_567 1_565 ? O1 S1 O2 112.79(10) . . ? O1 S1 O3 112.56(10) . . ? O2 S1 O3 110.81(11) . . ? O1 S1 C1 107.68(10) . . ? O2 S1 C1 105.53(10) . . ? O3 S1 C1 106.99(10) . . ? O1 S1 Li2 133.35(10) . 2_567 ? O2 S1 Li2 74.16(11) . 2_567 ? C1 S1 Li2 114.65(10) . 2_567 ? O5 S2 O7 112.52(11) . . ? O5 S2 O6 112.43(11) . . ? O7 S2 O6 111.43(10) . . ? O5 S2 C5 107.31(9) . . ? O7 S2 C5 106.84(10) . . ? O6 S2 C5 105.83(10) . . ? S1 O1 Li1 131.99(15) . . ? Li1 O1W H1W2 119(2) . . ? Li1 O1W H1W1 107(2) . . ? H1W2 O1W H1W1 109.3(15) . . ? S1 O2 Li2 154.21(16) . . ? H2W2 O2W H2W1 110.1(17) . . ? S1 O3 Li2 117.15(15) . 2_567 ? S1 O3 Li1 143.05(16) . 2_557 ? Li2 O3 Li1 98.43(18) 2_567 2_557 ? C2 O4 Li1 127.19(17) . . ? C2 O4 H4O 110(2) . . ? Li1 O4 H4O 117(2) . . ? S2 O6 Li2 132.46(16) . 1_554 ? S2 O7 Li2 138.75(15) . 2_666 ? S2 O7 Li1 129.37(14) . 2_656 ? Li2 O7 Li1 91.35(16) 2_666 2_656 ? C4 O8 Li1 114.03(17) . 2_656 ? C4 O8 H8O 111(2) . . ? Li1 O8 H8O 110(2) 2_656 . ? C6 C1 C2 120.17(18) . . ? C6 C1 S1 119.65(15) . . ? C2 C1 S1 120.11(15) . . ? O4 C2 C3 121.57(18) . . ? O4 C2 C1 118.74(18) . . ? C3 C2 C1 119.65(18) . . ? C4 C3 C2 120.02(18) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? O8 C4 C3 122.21(18) . . ? O8 C4 C5 117.63(18) . . ? C3 C4 C5 120.14(18) . . ? C6 C5 C4 119.62(18) . . ? C6 C5 S2 121.04(15) . . ? C4 C5 S2 119.29(15) . . ? C1 C6 C5 120.38(18) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 S1 O1 Li1 -160.5(2) . . . . ? O3 S1 O1 Li1 73.2(2) . . . . ? C1 S1 O1 Li1 -44.5(2) . . . . ? Li2 S1 O1 Li1 110.1(2) 2_567 . . . ? O3 Li1 O1 S1 -73.4(3) 2_557 . . . ? O1W Li1 O1 S1 -172.45(14) . . . . ? O4 Li1 O1 S1 9.5(2) . . . . ? O7 Li1 O1 S1 88.1(6) 2_656 . . . ? O8 Li1 O1 S1 106.90(18) 2_656 . . . ? Li2 Li1 O1 S1 -80.7(7) 1_545 . . . ? O1 S1 O2 Li2 -56.6(4) . . . . ? O3 S1 O2 Li2 70.6(4) . . . . ? C1 S1 O2 Li2 -173.9(4) . . . . ? Li2 S1 O2 Li2 74.3(4) 2_567 . . . ? O6 Li2 O2 S1 22.3(5) 1_556 . . . ? O7 Li2 O2 S1 152.2(3) 2_666 . . . ? O3 Li2 O2 S1 -101.3(4) 2_567 . . . ? S1 Li2 O2 S1 -82.9(4) 2_567 . . . ? Li1 Li2 O2 S1 -162.1(3) 1_565 . . . ? O1 S1 O3 Li2 133.27(16) . . . 2_567 ? O2 S1 O3 Li2 5.91(18) . . . 2_567 ? C1 S1 O3 Li2 -108.64(16) . . . 2_567 ? O1 S1 O3 Li1 -29.6(3) . . . 2_557 ? O2 S1 O3 Li1 -157.0(2) . . . 2_557 ? C1 S1 O3 Li1 88.5(3) . . . 2_557 ? Li2 S1 O3 Li1 -162.9(3) 2_567 . . 2_557 ? O1 Li1 O4 C2 42.2(3) . . . . ? O3 Li1 O4 C2 164.87(18) 2_557 . . . ? O7 Li1 O4 C2 -115.6(2) 2_656 . . . ? O8 Li1 O4 C2 -39.2(3) 2_656 . . . ? Li2 Li1 O4 C2 -155.64(18) 1_545 . . . ? O5 S2 O6 Li2 84.3(2) . . . 1_554 ? O7 S2 O6 Li2 -43.1(2) . . . 1_554 ? C5 S2 O6 Li2 -158.8(2) . . . 1_554 ? O5 S2 O7 Li2 -34.1(3) . . . 2_666 ? O6 S2 O7 Li2 93.2(2) . . . 2_666 ? C5 S2 O7 Li2 -151.6(2) . . . 2_666 ? O5 S2 O7 Li1 156.77(17) . . . 2_656 ? O6 S2 O7 Li1 -75.90(19) . . . 2_656 ? C5 S2 O7 Li1 39.2(2) . . . 2_656 ? O1 S1 C1 C6 -135.84(17) . . . . ? O2 S1 C1 C6 -15.1(2) . . . . ? O3 S1 C1 C6 102.92(18) . . . . ? Li2 S1 C1 C6 64.25(19) 2_567 . . . ? O1 S1 C1 C2 47.28(19) . . . . ? O2 S1 C1 C2 167.98(17) . . . . ? O3 S1 C1 C2 -73.96(18) . . . . ? Li2 S1 C1 C2 -112.63(18) 2_567 . . . ? Li1 O4 C2 C3 132.2(2) . . . . ? Li1 O4 C2 C1 -45.5(3) . . . . ? C6 C1 C2 O4 177.90(19) . . . . ? S1 C1 C2 O4 -5.2(3) . . . . ? C6 C1 C2 C3 0.2(3) . . . . ? S1 C1 C2 C3 177.05(16) . . . . ? O4 C2 C3 C4 -178.3(2) . . . . ? C1 C2 C3 C4 -0.7(3) . . . . ? Li1 O8 C4 C3 -116.7(2) 2_656 . . . ? Li1 O8 C4 C5 61.6(2) 2_656 . . . ? C2 C3 C4 O8 177.8(2) . . . . ? C2 C3 C4 C5 -0.3(3) . . . . ? O8 C4 C5 C6 -176.46(19) . . . . ? C3 C4 C5 C6 1.8(3) . . . . ? O8 C4 C5 S2 6.2(3) . . . . ? C3 C4 C5 S2 -175.54(16) . . . . ? O5 S2 C5 C6 0.5(2) . . . . ? O7 S2 C5 C6 121.36(18) . . . . ? O6 S2 C5 C6 -119.79(18) . . . . ? O5 S2 C5 C4 177.75(17) . . . . ? O7 S2 C5 C4 -61.35(19) . . . . ? O6 S2 C5 C4 57.51(19) . . . . ? C2 C1 C6 C5 1.3(3) . . . . ? S1 C1 C6 C5 -175.58(15) . . . . ? C4 C5 C6 C1 -2.3(3) . . . . ? S2 C5 C6 C1 175.01(16) . . . . ? 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 O1W H1W2 O5 0.84(4) 2.06(2) 2.883(2) 166(2) 1_546 O1W H1W1 O1 0.85(4) 2.25(2) 2.981(2) 144(3) 2_657 O2W H2W2 O5 0.85(4) 2.05(3) 2.886(3) 173(3) 1_545 O2W H2W1 O6 0.85(4) 2.09(2) 2.933(3) 172(3) 2_556 O4 H4O O2W 0.85(4) 1.76(2) 2.611(2) 177(3) . O8 H8O O1W 0.85(4) 1.90(2) 2.732(2) 169(3) 1_554 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.543 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.095 # Attachment 'complex 6.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 852890' #TrackingRef 'complex 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C3 H5 Li2 O6 S, H2 O' _chemical_formula_sum 'C3 H7 Li2 O7 S' _chemical_formula_weight 201.03 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P nma ' _symmetry_space_group_name_Hall '-P 2ac 2n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 13.552(3) _cell_length_b 15.623(3) _cell_length_c 7.5203(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1592.2(6) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 12024 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.43 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.403 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9059 _exptl_absorpt_correction_T_max 0.9309 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14697 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.44 _reflns_number_total 1883 _reflns_number_gt 1718 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0469P)^2^+1.7384P] 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 1883 _refine_ls_number_parameters 121 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.3245(2) -0.08893(19) -0.4779(4) 0.0225(6) Uani 1 1 d . . . Li2 Li 0.4818(3) 0.0171(2) -0.3372(5) 0.0312(7) Uani 1 1 d . . . S1 S 0.32970(3) 0.07763(2) -0.66800(5) 0.01450(13) Uani 1 1 d . . . O1 O 0.31830(10) 0.03564(8) -0.49572(17) 0.0239(3) Uani 1 1 d . . . O1W O 0.25795(11) -0.15664(9) -0.66821(19) 0.0311(3) Uani 1 1 d . . . H1W1 H 0.2055 -0.1309 -0.6780 0.047 Uiso 1 1 d R . . H1W2 H 0.2882 -0.1529 -0.7623 0.047 Uiso 1 1 d R . . O2 O 0.23446(9) 0.10070(8) -0.74536(18) 0.0229(3) Uani 1 1 d . . . O2W O 0.42831(11) 0.07818(10) -0.1337(2) 0.0368(4) Uani 1 1 d . . . H2W1 H 0.4136 0.0646 -0.0318 0.055 Uiso 1 1 d R . . H2W2 H 0.4781 0.0517 -0.1622 0.055 Uiso 1 1 d R . . O3 O 0.38948(9) 0.02440(7) -0.78709(17) 0.0224(3) Uani 1 1 d . . . O3W O 0.39170(12) -0.16272(10) 0.0376(2) 0.0427(4) Uani 1 1 d . . . H3W1 H 0.3608 -0.1406 -0.0441 0.064 Uiso 1 1 d R . . H3W2 H 0.4417 -0.1345 0.0557 0.064 Uiso 1 1 d R . . O4 O 0.53376(8) 0.09667(7) -0.52835(17) 0.0189(3) Uani 1 1 d . . . C1 C 0.34511(17) 0.2500 -0.6657(3) 0.0162(4) Uani 1 2 d S . . H1 H 0.2815 0.2500 -0.7120 0.019 Uiso 1 2 d SR . . C2 C 0.39201(11) 0.17312(9) -0.6313(2) 0.0153(3) Uani 1 1 d . . . C3 C 0.48969(12) 0.17076(10) -0.5619(2) 0.0159(3) Uani 1 1 d . . . C4 C 0.53560(17) 0.2500 -0.5303(4) 0.0204(5) Uani 1 2 d S . . H4 H 0.5997 0.2500 -0.4862 0.025 Uiso 1 2 d SR . . 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 0.0200(14) 0.0200(13) 0.0276(16) 0.0026(12) 0.0009(11) 0.0001(11) Li2 0.0433(19) 0.0217(15) 0.0287(17) -0.0008(13) 0.0073(14) 0.0015(14) S1 0.0161(2) 0.0099(2) 0.0175(2) -0.00095(13) -0.00124(14) -0.00038(13) O1 0.0320(7) 0.0167(6) 0.0230(7) 0.0041(5) 0.0036(5) -0.0013(5) O1W 0.0281(7) 0.0316(7) 0.0334(8) -0.0014(6) -0.0051(6) 0.0040(6) O2 0.0187(6) 0.0183(6) 0.0317(7) -0.0047(5) -0.0085(5) -0.0002(5) O2W 0.0343(8) 0.0500(9) 0.0261(7) 0.0010(6) 0.0080(6) 0.0160(7) O3 0.0251(6) 0.0183(6) 0.0238(6) -0.0052(5) 0.0011(5) 0.0042(5) O3W 0.0417(9) 0.0354(8) 0.0510(10) 0.0024(7) -0.0125(8) -0.0015(7) O4 0.0157(5) 0.0127(5) 0.0282(6) 0.0030(5) -0.0016(5) 0.0029(4) C1 0.0141(10) 0.0136(10) 0.0211(11) 0.000 -0.0036(8) 0.000 C2 0.0145(7) 0.0106(7) 0.0210(8) -0.0004(6) -0.0018(6) -0.0019(6) C3 0.0150(7) 0.0132(7) 0.0195(8) 0.0014(6) -0.0004(6) 0.0019(6) C4 0.0138(10) 0.0173(11) 0.0303(13) 0.000 -0.0063(9) 0.000 _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 O4 1.926(3) 5_654 ? Li1 O2 1.931(4) 2 ? Li1 O1 1.953(3) . ? Li1 O1W 1.995(4) . ? Li1 Li2 2.900(5) . ? Li1 S1 2.970(3) . ? Li1 Li2 3.176(5) 5_654 ? Li1 H1W1 2.3007 . ? Li2 O2W 1.944(4) . ? Li2 O4 2.027(4) . ? Li2 O4 2.056(4) 5_654 ? Li2 O3 2.083(4) 5_654 ? Li2 O1 2.532(4) . ? Li2 Li2 2.554(7) 5_654 ? Li2 S1 2.953(4) 5_654 ? Li2 Li1 3.176(5) 5_654 ? Li2 H2W2 1.4240 . ? S1 O1 1.4604(13) . ? S1 O2 1.4609(12) . ? S1 O3 1.4663(12) . ? S1 C2 1.7364(15) . ? S1 Li2 2.953(4) 5_654 ? O1W H1W1 0.8200 . ? O1W H1W2 0.8200 . ? O2 Li1 1.931(4) 2_554 ? O2W H2W1 0.8200 . ? O2W H2W2 0.8200 . ? O3 Li2 2.083(4) 5_654 ? O3W H3W1 0.8200 . ? O3W H3W2 0.8200 . ? O4 C3 1.3267(19) . ? O4 Li1 1.926(3) 5_654 ? O4 Li2 2.056(4) 5_654 ? C1 C2 1.3833(19) 8_565 ? C1 C2 1.3833(19) . ? C1 H1 0.9300 . ? C2 C3 1.423(2) . ? C3 C4 1.4058(19) . ? C4 C3 1.4058(19) 8_565 ? C4 H4 0.9300 . ? 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 Li1 O2 112.61(17) 5_654 2 ? O4 Li1 O1 96.13(14) 5_654 . ? O2 Li1 O1 98.01(15) 2 . ? O4 Li1 O1W 115.79(17) 5_654 . ? O2 Li1 O1W 114.35(16) 2 . ? O1 Li1 O1W 117.38(17) . . ? O4 Li1 Li2 45.04(10) 5_654 . ? O2 Li1 Li2 91.61(14) 2 . ? O1 Li1 Li2 59.14(11) . . ? O1W Li1 Li2 153.74(17) . . ? O4 Li1 S1 92.46(11) 5_654 . ? O2 Li1 S1 121.95(14) 2 . ? O1 Li1 S1 25.13(6) . . ? O1W Li1 S1 97.47(13) . . ? Li2 Li1 S1 69.97(10) . . ? O4 Li1 Li2 37.62(10) 5_654 5_654 ? O2 Li1 Li2 140.53(16) 2 5_654 ? O1 Li1 Li2 69.70(11) . 5_654 ? O1W Li1 Li2 104.29(14) . 5_654 ? Li2 Li1 Li2 49.46(13) . 5_654 ? S1 Li1 Li2 57.31(8) . 5_654 ? O4 Li1 H1W1 134.2 5_654 . ? O2 Li1 H1W1 106.0 2 . ? O1 Li1 H1W1 102.1 . . ? O1W Li1 H1W1 20.5 . . ? Li2 Li1 H1W1 156.4 . . ? S1 Li1 H1W1 87.2 . . ? Li2 Li1 H1W1 113.2 5_654 . ? O2W Li2 O4 112.76(17) . . ? O2W Li2 O4 140.7(2) . 5_654 ? O4 Li2 O4 102.54(15) . 5_654 ? O2W Li2 O3 96.42(16) . 5_654 ? O4 Li2 O3 102.61(17) . 5_654 ? O4 Li2 O3 92.14(14) 5_654 5_654 ? O2W Li2 O1 89.32(14) . . ? O4 Li2 O1 84.27(13) . . ? O4 Li2 O1 77.16(13) 5_654 . ? O3 Li2 O1 168.42(17) 5_654 . ? O2W Li2 Li2 158.4(3) . 5_654 ? O4 Li2 Li2 51.78(12) . 5_654 ? O4 Li2 Li2 50.76(12) 5_654 5_654 ? O3 Li2 Li2 101.7(2) 5_654 5_654 ? O1 Li2 Li2 75.04(17) . 5_654 ? O2W Li2 Li1 107.07(17) . . ? O4 Li2 Li1 110.31(16) . . ? O4 Li2 Li1 41.52(10) 5_654 . ? O3 Li2 Li1 126.99(15) 5_654 . ? O1 Li2 Li1 41.44(9) . . ? Li2 Li2 Li1 70.90(17) 5_654 . ? O2W Li2 S1 123.93(17) . 5_654 ? O4 Li2 S1 90.93(13) . 5_654 ? O4 Li2 S1 70.23(10) 5_654 5_654 ? O3 Li2 S1 27.53(6) 5_654 5_654 ? O1 Li2 S1 145.14(14) . 5_654 ? Li2 Li2 S1 74.97(16) 5_654 5_654 ? Li1 Li2 S1 110.77(12) . 5_654 ? O2W Li2 Li1 118.65(16) . 5_654 ? O4 Li2 Li1 35.46(9) . 5_654 ? O4 Li2 Li1 100.08(14) 5_654 5_654 ? O3 Li2 Li1 67.30(12) 5_654 5_654 ? O1 Li2 Li1 118.48(14) . 5_654 ? Li2 Li2 Li1 59.64(15) 5_654 5_654 ? Li1 Li2 Li1 130.54(13) . 5_654 ? S1 Li2 Li1 57.83(9) 5_654 5_654 ? O2W Li2 H2W2 22.0 . . ? O4 Li2 H2W2 115.8 . . ? O4 Li2 H2W2 141.2 5_654 . ? O3 Li2 H2W2 74.5 5_654 . ? O1 Li2 H2W2 111.2 . . ? Li2 Li2 H2W2 166.5 5_654 . ? Li1 Li2 H2W2 121.9 . . ? S1 Li2 H2W2 102.0 5_654 . ? Li1 Li2 H2W2 107.4 5_654 . ? O1 S1 O2 111.76(8) . . ? O1 S1 O3 110.22(7) . . ? O2 S1 O3 112.64(8) . . ? O1 S1 C2 107.23(8) . . ? O2 S1 C2 106.32(7) . . ? O3 S1 C2 108.40(8) . . ? O1 S1 Li2 81.64(8) . 5_654 ? O2 S1 Li2 153.30(9) . 5_654 ? C2 S1 Li2 90.45(9) . 5_654 ? O2 S1 Li1 112.76(8) . . ? O3 S1 Li1 79.07(8) . . ? C2 S1 Li1 133.46(8) . . ? Li2 S1 Li1 64.86(9) 5_654 . ? S1 O1 Li1 120.27(13) . . ? S1 O1 Li2 112.11(10) . . ? Li1 O1 Li2 79.42(12) . . ? Li1 O1W H1W1 101.3 . . ? Li1 O1W H1W2 110.8 . . ? H1W1 O1W H1W2 108.7 . . ? S1 O2 Li1 134.62(12) . 2_554 ? Li2 O2W H2W1 134.4 . . ? H2W1 O2W H2W2 108.2 . . ? S1 O3 Li2 111.42(12) . 5_654 ? H3W1 O3W H3W2 108.6 . . ? C3 O4 Li1 120.57(13) . 5_654 ? C3 O4 Li2 120.90(14) . . ? Li1 O4 Li2 106.91(15) 5_654 . ? C3 O4 Li2 127.93(15) . 5_654 ? Li1 O4 Li2 93.44(15) 5_654 5_654 ? Li2 O4 Li2 77.46(15) . 5_654 ? C2 C1 C2 120.5(2) 8_565 . ? C2 C1 H1 119.7 8_565 . ? C2 C1 H1 119.7 . . ? C1 C2 C3 121.23(15) . . ? C1 C2 S1 119.53(13) . . ? C3 C2 S1 119.23(12) . . ? O4 C3 C4 122.47(15) . . ? O4 C3 C2 120.73(14) . . ? C4 C3 C2 116.79(15) . . ? C3 C4 C3 123.4(2) . 8_565 ? C3 C4 H4 118.3 . . ? C3 C4 H4 118.3 8_565 . ? 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 O4 Li1 Li2 O2W -150.9(2) 5_654 . . . ? O2 Li1 Li2 O2W -29.87(18) 2 . . . ? O1 Li1 Li2 O2W 68.51(16) . . . . ? O1W Li1 Li2 O2W 158.5(3) . . . . ? S1 Li1 Li2 O2W 93.72(15) . . . . ? Li2 Li1 Li2 O2W 157.3(3) 5_654 . . . ? O4 Li1 Li2 O4 86.06(17) 5_654 . . . ? O2 Li1 Li2 O4 -152.91(15) 2 . . . ? O1 Li1 Li2 O4 -54.53(15) . . . . ? O1W Li1 Li2 O4 35.5(4) . . . . ? S1 Li1 Li2 O4 -29.32(13) . . . . ? Li2 Li1 Li2 O4 34.28(9) 5_654 . . . ? O2 Li1 Li2 O4 121.03(17) 2 . . 5_654 ? O1 Li1 Li2 O4 -140.59(18) . . . 5_654 ? O1W Li1 Li2 O4 -50.6(3) . . . 5_654 ? S1 Li1 Li2 O4 -115.38(14) . . . 5_654 ? Li2 Li1 Li2 O4 -51.77(14) 5_654 . . 5_654 ? O4 Li1 Li2 O3 -38.71(18) 5_654 . . 5_654 ? O2 Li1 Li2 O3 82.3(2) 2 . . 5_654 ? O1 Li1 Li2 O3 -179.3(2) . . . 5_654 ? O1W Li1 Li2 O3 -89.3(4) . . . 5_654 ? S1 Li1 Li2 O3 -154.1(2) . . . 5_654 ? Li2 Li1 Li2 O3 -90.5(2) 5_654 . . 5_654 ? O4 Li1 Li2 O1 140.59(18) 5_654 . . . ? O2 Li1 Li2 O1 -98.38(14) 2 . . . ? O1W Li1 Li2 O1 90.0(4) . . . . ? S1 Li1 Li2 O1 25.22(6) . . . . ? Li2 Li1 Li2 O1 88.82(17) 5_654 . . . ? O4 Li1 Li2 Li2 51.77(14) 5_654 . . 5_654 ? O2 Li1 Li2 Li2 172.81(18) 2 . . 5_654 ? O1 Li1 Li2 Li2 -88.82(17) . . . 5_654 ? O1W Li1 Li2 Li2 1.2(4) . . . 5_654 ? S1 Li1 Li2 Li2 -63.60(14) . . . 5_654 ? O4 Li1 Li2 S1 -13.08(12) 5_654 . . 5_654 ? O2 Li1 Li2 S1 107.95(13) 2 . . 5_654 ? O1 Li1 Li2 S1 -153.68(15) . . . 5_654 ? O1W Li1 Li2 S1 -63.7(4) . . . 5_654 ? S1 Li1 Li2 S1 -128.46(12) . . . 5_654 ? Li2 Li1 Li2 S1 -64.86(14) 5_654 . . 5_654 ? O4 Li1 Li2 Li1 51.77(14) 5_654 . . 5_654 ? O2 Li1 Li2 Li1 172.81(18) 2 . . 5_654 ? O1 Li1 Li2 Li1 -88.82(17) . . . 5_654 ? O1W Li1 Li2 Li1 1.2(4) . . . 5_654 ? S1 Li1 Li2 Li1 -63.60(14) . . . 5_654 ? Li2 Li1 Li2 Li1 0.0 5_654 . . 5_654 ? O4 Li1 S1 O1 -99.23(18) 5_654 . . . ? O2 Li1 S1 O1 19.48(12) 2 . . . ? O1W Li1 S1 O1 144.4(2) . . . . ? Li2 Li1 S1 O1 -59.44(14) . . . . ? Li2 Li1 S1 O1 -113.42(16) 5_654 . . . ? O4 Li1 S1 O2 165.04(10) 5_654 . . . ? O2 Li1 S1 O2 -76.26(16) 2 . . . ? O1 Li1 S1 O2 -95.74(14) . . . . ? O1W Li1 S1 O2 48.63(13) . . . . ? Li2 Li1 S1 O2 -155.18(10) . . . . ? Li2 Li1 S1 O2 150.84(10) 5_654 . . . ? O4 Li1 S1 O3 54.91(12) 5_654 . . . ? O2 Li1 S1 O3 173.62(16) 2 . . . ? O1 Li1 S1 O3 154.14(15) . . . . ? O1W Li1 S1 O3 -61.50(11) . . . . ? Li2 Li1 S1 O3 94.70(10) . . . . ? Li2 Li1 S1 O3 40.72(9) 5_654 . . . ? O4 Li1 S1 C2 -50.16(17) 5_654 . . . ? O2 Li1 S1 C2 68.55(19) 2 . . . ? O1 Li1 S1 C2 49.07(17) . . . . ? O1W Li1 S1 C2 -166.56(10) . . . . ? Li2 Li1 S1 C2 -10.37(14) . . . . ? Li2 Li1 S1 C2 -64.35(13) 5_654 . . . ? O4 Li1 S1 Li2 14.19(11) 5_654 . . 5_654 ? O2 Li1 S1 Li2 132.90(18) 2 . . 5_654 ? O1 Li1 S1 Li2 113.42(16) . . . 5_654 ? O1W Li1 S1 Li2 -102.22(14) . . . 5_654 ? Li2 Li1 S1 Li2 53.98(13) . . . 5_654 ? O2 S1 O1 Li1 98.91(14) . . . . ? O3 S1 O1 Li1 -27.15(15) . . . . ? C2 S1 O1 Li1 -144.96(13) . . . . ? Li2 S1 O1 Li1 -57.10(14) 5_654 . . . ? O2 S1 O1 Li2 -170.66(10) . . . . ? O3 S1 O1 Li2 63.28(12) . . . . ? C2 S1 O1 Li2 -54.52(11) . . . . ? Li2 S1 O1 Li2 33.34(15) 5_654 . . . ? Li1 S1 O1 Li2 90.44(16) . . . . ? O4 Li1 O1 S1 82.67(16) 5_654 . . . ? O2 Li1 O1 S1 -163.40(10) 2 . . . ? O1W Li1 O1 S1 -40.6(2) . . . . ? Li2 Li1 O1 S1 109.53(13) . . . . ? Li2 Li1 O1 S1 55.43(13) 5_654 . . . ? O4 Li1 O1 Li2 -26.86(13) 5_654 . . . ? O2 Li1 O1 Li2 87.07(14) 2 . . . ? O1W Li1 O1 Li2 -150.12(18) . . . . ? S1 Li1 O1 Li2 -109.53(13) . . . . ? Li2 Li1 O1 Li2 -54.10(13) 5_654 . . . ? O2W Li2 O1 S1 124.29(12) . . . . ? O4 Li2 O1 S1 11.33(13) . . . . ? O4 Li2 O1 S1 -92.96(11) 5_654 . . . ? O3 Li2 O1 S1 -115.8(9) 5_654 . . . ? Li2 Li2 O1 S1 -40.59(17) 5_654 . . . ? Li1 Li2 O1 S1 -118.53(13) . . . . ? S1 Li2 O1 S1 -72.0(2) 5_654 . . . ? Li1 Li2 O1 S1 1.66(17) 5_654 . . . ? O2W Li2 O1 Li1 -117.18(15) . . . . ? O4 Li2 O1 Li1 129.86(15) . . . . ? O4 Li2 O1 Li1 25.57(13) 5_654 . . . ? O3 Li2 O1 Li1 2.8(9) 5_654 . . . ? Li2 Li2 O1 Li1 77.94(17) 5_654 . . . ? S1 Li2 O1 Li1 46.5(2) 5_654 . . . ? Li1 Li2 O1 Li1 120.19(15) 5_654 . . . ? O1 S1 O2 Li1 -133.67(17) . . . 2_554 ? O3 S1 O2 Li1 -8.94(19) . . . 2_554 ? C2 S1 O2 Li1 109.64(17) . . . 2_554 ? Li2 S1 O2 Li1 -17.2(3) 5_654 . . 2_554 ? Li1 S1 O2 Li1 -96.20(15) . . . 2_554 ? O1 S1 O3 Li2 -48.77(14) . . . 5_654 ? O2 S1 O3 Li2 -174.34(12) . . . 5_654 ? C2 S1 O3 Li2 68.31(13) . . . 5_654 ? Li1 S1 O3 Li2 -64.07(13) . . . 5_654 ? O2W Li2 O4 C3 -35.4(3) . . . . ? O4 Li2 O4 C3 126.93(16) 5_654 . . . ? O3 Li2 O4 C3 -137.97(14) 5_654 . . . ? O1 Li2 O4 C3 51.47(16) . . . . ? Li2 Li2 O4 C3 126.93(16) 5_654 . . . ? Li1 Li2 O4 C3 84.28(18) . . . . ? S1 Li2 O4 C3 -163.13(11) 5_654 . . . ? Li1 Li2 O4 C3 -143.3(2) 5_654 . . . ? O2W Li2 O4 Li1 107.9(2) . . . 5_654 ? O4 Li2 O4 Li1 -89.80(18) 5_654 . . 5_654 ? O3 Li2 O4 Li1 5.30(19) 5_654 . . 5_654 ? O1 Li2 O4 Li1 -165.26(12) . . . 5_654 ? Li2 Li2 O4 Li1 -89.80(18) 5_654 . . 5_654 ? Li1 Li2 O4 Li1 -132.45(12) . . . 5_654 ? S1 Li2 O4 Li1 -19.86(15) 5_654 . . 5_654 ? O2W Li2 O4 Li2 -162.3(3) . . . 5_654 ? O4 Li2 O4 Li2 0.0 5_654 . . 5_654 ? O3 Li2 O4 Li2 95.11(18) 5_654 . . 5_654 ? O1 Li2 O4 Li2 -75.45(14) . . . 5_654 ? Li1 Li2 O4 Li2 -42.65(11) . . . 5_654 ? S1 Li2 O4 Li2 69.95(12) 5_654 . . 5_654 ? Li1 Li2 O4 Li2 89.80(18) 5_654 . . 5_654 ? C2 C1 C2 C3 -0.8(3) 8_565 . . . ? C2 C1 C2 S1 177.62(12) 8_565 . . . ? O1 S1 C2 C1 -115.79(17) . . . . ? O2 S1 C2 C1 3.90(18) . . . . ? O3 S1 C2 C1 125.23(16) . . . . ? Li2 S1 C2 C1 162.83(17) 5_654 . . . ? Li1 S1 C2 C1 -142.48(16) . . . . ? O1 S1 C2 C3 62.64(15) . . . . ? O2 S1 C2 C3 -177.67(13) . . . . ? O3 S1 C2 C3 -56.34(15) . . . . ? Li2 S1 C2 C3 -18.74(15) 5_654 . . . ? Li1 S1 C2 C3 35.95(19) . . . . ? Li1 O4 C3 C4 -24.0(3) 5_654 . . . ? Li2 O4 C3 C4 114.3(2) . . . . ? Li2 O4 C3 C4 -147.3(2) 5_654 . . . ? Li1 O4 C3 C2 156.48(17) 5_654 . . . ? Li2 O4 C3 C2 -65.2(2) . . . . ? Li2 O4 C3 C2 33.2(3) 5_654 . . . ? C1 C2 C3 O4 179.59(18) . . . . ? S1 C2 C3 O4 1.2(2) . . . . ? C1 C2 C3 C4 0.1(3) . . . . ? S1 C2 C3 C4 -178.33(16) . . . . ? O4 C3 C4 C3 -178.85(15) . . . 8_565 ? C2 C3 C4 C3 0.7(4) . . . 8_565 ? 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 O1W H1W1 O2W 0.82 2.02 2.818(2) 164.5 2_554 O1W H1W2 O3W 0.82 2.06 2.861(2) 164.6 1_554 O2W H2W1 O3 0.82 1.97 2.789(2) 174.4 1_556 O2W H2W2 O3 0.82 2.19 3.0033(19) 174.6 5_654 O3W H3W1 O2 0.82 2.08 2.897(2) 170.5 2 O3W H3W2 O2W 0.82 2.05 2.866(2) 170.5 5_655 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.425 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.065