Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Kenneth Henderson' _publ_contact_author_address ; Dept. of Chemistry and Biochemistry The University of Notre Dame Notre Dame IN46556 USA ; _publ_contact_author_email khenders@nd.edu _publ_contact_author_phone '(574) 631 8025' _publ_contact_author_fax '(574) 631 6652' loop_ _publ_author_name _publ_author_address K.Henderson ;Dept. of Chemistry and Biochemistry The University of Notre Dame Notre Dame IN46556 USA ; D.MacDougall ;Dept. of Chemistry and Biochemistry The University of Notre Dame Notre Dame IN46556 USA ; B.Noll ;Dept. of Chemistry and Biochemistry The University of Notre Dame Notre Dame IN46556 USA ; A.Kennedy ;Dept. of Pure and Applied Chemistry The University of Strathclyde Glasgow G1 1XL UKA ; _publ_section_title ; Synthesis of mono- and geminal dimetallated carbanions of bis(phenylsulfonyl)methane using alkali metal bases and structural comparisons with lithiated bis(phenylsulfonyl)imides ; data_kwh0603m _database_code_depnum_ccdc_archive 'CCDC 267871' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common 'Lithium bis(phenylsulfonyl)imide THF solvate' _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 Li2 N2 O10 S4' _chemical_formula_sum 'C32 H36 Li2 N2 O10 S4' _chemical_formula_weight 750.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.8793(7) _cell_length_b 9.3620(6) _cell_length_c 34.239(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.697(1) _cell_angle_gamma 90.00 _cell_volume 3475.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7610 _cell_measurement_theta_min 2.387 _cell_measurement_theta_max 28.283 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.332 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9306 _exptl_absorpt_correction_T_max 0.9504 _exptl_absorpt_process_details 'Blessing, R.H. (1995) Acta Cryst. A51, 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Siemens KFFMO2K-90' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36012 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.30 _reflns_number_total 8630 _reflns_number_gt 7668 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART/SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2001; Sheldrick, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _refine_special_details ; Hydrogen atoms on THF were placed at calculated positions and allowed to ride on the position of the parent atom. Thermal parameters for these hydrogens were set to 1.2\\times the equivalent isotropic U of the parent atom. All other hydrogens were located by difference map and freely refined All non-hydrogen atoms were refined with parameters for anisotropic thermal motion. Disorder was observed in the positions of THF ring O29, C29-C32. An alternate position was modelled for C32. Site occupancy for the major component was fixed at 0.63.The largest peak in the final difference map, 1.097e/\%A^3^, was located near C31 and represents disorder of this group. There is no free solvent and no additional disorder was modelled. 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^)+(0.0602P)^2^+2.8021P] 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 8630 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.1175 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.2288(3) 0.6187(3) 0.08716(9) 0.0211(6) Uani 1 1 d . . . Li2 Li 0.7290(3) 0.9115(3) 0.08406(10) 0.0240(6) Uani 1 1 d . . . O1 O 0.09542(11) 0.74827(14) 0.07098(3) 0.0199(2) Uani 1 1 d . . . O2 O -0.10747(11) 0.85161(14) 0.07713(4) 0.0212(3) Uani 1 1 d . . . O3 O 0.19866(11) 0.61044(13) 0.14165(3) 0.0196(2) Uani 1 1 d . . . O4 O 0.03078(12) 0.52714(13) 0.17986(4) 0.0222(3) Uani 1 1 d . . . O5 O 0.59222(11) 0.78315(14) 0.07002(4) 0.0216(3) Uani 1 1 d . . . O6 O 0.38964(11) 0.68207(14) 0.07784(4) 0.0220(3) Uani 1 1 d . B . O7 O 0.69828(11) 0.92823(13) 0.13890(4) 0.0214(3) Uani 1 1 d . . . O8 O 0.53250(12) 1.01664(13) 0.17739(4) 0.0240(3) Uani 1 1 d . B . O9 O 0.20523(11) 0.44704(14) 0.05798(4) 0.0235(3) Uani 1 1 d . . . O10 O 0.70038(13) 1.06982(17) 0.04960(5) 0.0424(4) Uani 1 1 d . . . N1 N -0.01636(12) 0.71899(15) 0.13279(4) 0.0167(3) Uani 1 1 d . . . N2 N 0.48341(12) 0.81998(15) 0.13213(4) 0.0175(3) Uani 1 1 d . B . S1 S 0.01155(3) 0.81433(4) 0.096647(11) 0.01574(10) Uani 1 1 d . . . S2 S 0.08838(4) 0.64432(4) 0.161401(11) 0.01550(10) Uani 1 1 d . . . S3 S 0.50972(3) 0.72059(4) 0.096618(11) 0.01630(10) Uani 1 1 d . . . S4 S 0.58930(4) 0.89715(4) 0.159580(12) 0.01673(10) Uani 1 1 d . . . C1 C 0.08216(15) 0.97531(17) 0.11356(5) 0.0176(3) Uani 1 1 d . . . C2 C 0.20566(16) 1.0001(2) 0.10816(5) 0.0220(3) Uani 1 1 d . . . C3 C 0.26127(18) 1.1246(2) 0.12311(6) 0.0272(4) Uani 1 1 d . . . C4 C 0.1935(2) 1.2228(2) 0.14263(6) 0.0296(4) Uani 1 1 d . . . C5 C 0.06990(19) 1.1976(2) 0.14791(6) 0.0278(4) Uani 1 1 d . . . C6 C 0.01318(17) 1.07268(19) 0.13367(6) 0.0228(4) Uani 1 1 d . . . C7 C 0.13306(15) 0.77065(17) 0.19810(5) 0.0171(3) Uani 1 1 d . . . C8 C 0.05976(17) 0.7858(2) 0.22941(5) 0.0246(4) Uani 1 1 d . . . C9 C 0.09046(18) 0.8892(2) 0.25746(6) 0.0317(4) Uani 1 1 d . . . C10 C 0.19261(18) 0.9763(2) 0.25439(6) 0.0306(4) Uani 1 1 d . . . C11 C 0.26551(17) 0.9595(2) 0.22344(6) 0.0247(4) Uani 1 1 d . . . C12 C 0.23738(15) 0.85501(18) 0.19515(5) 0.0191(3) Uani 1 1 d . . . C13 C 0.58023(15) 0.56100(18) 0.11444(5) 0.0183(3) Uani 1 1 d . B . C14 C 0.51197(17) 0.46585(19) 0.13537(6) 0.0238(4) Uani 1 1 d . . . C15 C 0.5682(2) 0.3415(2) 0.14983(6) 0.0303(4) Uani 1 1 d . B . C16 C 0.6913(2) 0.3147(2) 0.14427(7) 0.0318(4) Uani 1 1 d . . . C17 C 0.75908(18) 0.4107(2) 0.12414(6) 0.0280(4) Uani 1 1 d . B . C18 C 0.70367(16) 0.5350(2) 0.10871(5) 0.0225(3) Uani 1 1 d . . . C19 C 0.63512(15) 0.77548(18) 0.19747(5) 0.0180(3) Uani 1 1 d . B . C20 C 0.56323(17) 0.7661(2) 0.22915(5) 0.0245(4) Uani 1 1 d . . . C21 C 0.59424(19) 0.6667(2) 0.25830(6) 0.0316(4) Uani 1 1 d . B . C22 C 0.69503(18) 0.5771(2) 0.25549(6) 0.0308(4) Uani 1 1 d . . . C23 C 0.76651(17) 0.5877(2) 0.22401(6) 0.0255(4) Uani 1 1 d . B . C24 C 0.73822(15) 0.68872(19) 0.19470(5) 0.0198(3) Uani 1 1 d . . . C25 C 0.29870(17) 0.3712(2) 0.03872(6) 0.0245(4) Uani 1 1 d . . . H25A H 0.3424 0.3020 0.0568 0.029 Uiso 1 1 calc R . . H25B H 0.3596 0.4383 0.0290 0.029 Uiso 1 1 calc R . . C26 C 0.2283(2) 0.2950(3) 0.00508(7) 0.0428(6) Uani 1 1 d . . . H26A H 0.2168 0.3577 -0.0182 0.051 Uiso 1 1 calc R . . H26B H 0.2717 0.2070 -0.0020 0.051 Uiso 1 1 calc R . . C27 C 0.1066(2) 0.2601(2) 0.02067(7) 0.0351(5) Uani 1 1 d . . . H27A H 0.1111 0.1694 0.0355 0.042 Uiso 1 1 calc R . . H27B H 0.0402 0.2530 -0.0008 0.042 Uiso 1 1 calc R . . C28 C 0.08559(17) 0.3850(2) 0.04706(6) 0.0272(4) Uani 1 1 d . . . H28A H 0.0308 0.4561 0.0331 0.033 Uiso 1 1 calc R . . H28B H 0.0467 0.3526 0.0707 0.033 Uiso 1 1 calc R . . C29 C 0.58735(19) 1.1495(3) 0.04558(8) 0.0402(5) Uani 1 1 d . B . H29A H 0.5592 1.1716 0.0717 0.048 Uiso 1 1 calc R . . H29B H 0.5222 1.0938 0.0305 0.048 Uiso 1 1 calc R . . C30 C 0.61378(19) 1.2857(2) 0.02411(6) 0.0321(4) Uani 1 1 d . . . H30A H 0.5942 1.3704 0.0398 0.038 Uiso 1 1 calc R B . H30B H 0.5646 1.2899 -0.0015 0.038 Uiso 1 1 calc R . . C31 C 0.7510(2) 1.2796(3) 0.01853(7) 0.0408(5) Uani 1 1 d . B . H31A H 0.7697 1.3244 -0.0065 0.049 Uiso 1 1 calc R A 1 H31B H 0.8005 1.3266 0.0404 0.049 Uiso 1 1 calc R A 1 C32 C 0.7735(4) 1.1225(4) 0.01819(12) 0.0306(8) Uani 0.63 1 d P B 1 H32A H 0.7445 1.0802 -0.0074 0.037 Uiso 0.63 1 calc PR B 1 H32B H 0.8621 1.1005 0.0239 0.037 Uiso 0.63 1 calc PR B 1 C32A C 0.8015(6) 1.1493(9) 0.0362(3) 0.0376(17) Uani 0.37 1 d P B 2 H32C H 0.8434 1.0929 0.0167 0.045 Uiso 0.37 1 calc PR B 2 H32D H 0.8623 1.1720 0.0585 0.045 Uiso 0.37 1 calc PR B 2 H2 H 0.252(2) 0.930(3) 0.0946(7) 0.027(6) Uiso 1 1 d . . . H3 H 0.346(2) 1.140(3) 0.1201(7) 0.031(6) Uiso 1 1 d . . . H4 H 0.231(2) 1.307(3) 0.1528(7) 0.037(7) Uiso 1 1 d . . . H5 H 0.022(2) 1.261(3) 0.1613(7) 0.034(6) Uiso 1 1 d . . . H6 H -0.068(2) 1.050(2) 0.1381(6) 0.026(6) Uiso 1 1 d . . . H8 H -0.009(2) 0.733(3) 0.2315(7) 0.026(6) Uiso 1 1 d . . . H9 H 0.042(2) 0.901(3) 0.2789(8) 0.046(8) Uiso 1 1 d . . . H10 H 0.210(2) 1.050(3) 0.2733(7) 0.035(6) Uiso 1 1 d . . . H11 H 0.333(2) 1.019(3) 0.2218(7) 0.032(6) Uiso 1 1 d . . . H12 H 0.290(2) 0.838(2) 0.1755(6) 0.021(5) Uiso 1 1 d . . . H14 H 0.432(2) 0.488(2) 0.1401(6) 0.022(5) Uiso 1 1 d . . . H15 H 0.519(2) 0.275(3) 0.1638(7) 0.038(7) Uiso 1 1 d . . . H16 H 0.728(2) 0.231(3) 0.1547(7) 0.037(7) Uiso 1 1 d . . . H17 H 0.842(2) 0.396(3) 0.1200(7) 0.030(6) Uiso 1 1 d . . . H18 H 0.756(2) 0.602(3) 0.0951(7) 0.040(7) Uiso 1 1 d . . . H20 H 0.495(2) 0.823(3) 0.2306(7) 0.037(7) Uiso 1 1 d . . . H21 H 0.548(2) 0.663(3) 0.2799(7) 0.037(7) Uiso 1 1 d . . . H22 H 0.712(2) 0.507(3) 0.2739(8) 0.044(7) Uiso 1 1 d . . . H23 H 0.834(2) 0.526(3) 0.2214(7) 0.036(7) Uiso 1 1 d . . . H24 H 0.788(2) 0.700(2) 0.1742(6) 0.020(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.0161(13) 0.0232(15) 0.0242(14) -0.0038(11) 0.0019(11) 0.0008(11) Li2 0.0157(14) 0.0252(16) 0.0314(16) 0.0067(12) 0.0034(12) 0.0002(11) O1 0.0151(5) 0.0254(6) 0.0192(6) -0.0029(5) 0.0018(4) 0.0045(5) O2 0.0133(5) 0.0275(7) 0.0222(6) -0.0001(5) -0.0026(4) 0.0039(5) O3 0.0159(6) 0.0213(6) 0.0217(6) -0.0019(5) 0.0018(4) 0.0046(5) O4 0.0242(6) 0.0156(6) 0.0268(6) 0.0014(5) 0.0031(5) -0.0026(5) O5 0.0161(6) 0.0281(7) 0.0209(6) 0.0037(5) 0.0032(5) -0.0040(5) O6 0.0140(6) 0.0291(7) 0.0224(6) -0.0010(5) -0.0008(5) -0.0029(5) O7 0.0157(6) 0.0204(6) 0.0281(6) 0.0015(5) 0.0021(5) -0.0046(5) O8 0.0245(6) 0.0162(6) 0.0315(7) -0.0031(5) 0.0030(5) 0.0029(5) O9 0.0156(6) 0.0256(6) 0.0297(7) -0.0092(5) 0.0041(5) -0.0026(5) O10 0.0226(7) 0.0376(9) 0.0697(11) 0.0315(8) 0.0209(7) 0.0112(6) N1 0.0133(6) 0.0178(7) 0.0191(6) 0.0003(5) 0.0014(5) -0.0005(5) N2 0.0127(6) 0.0178(7) 0.0217(7) 0.0000(5) 0.0008(5) -0.0003(5) S1 0.01148(18) 0.0177(2) 0.01778(19) -0.00114(14) -0.00009(14) 0.00168(14) S2 0.01467(19) 0.01332(19) 0.01847(19) -0.00120(14) 0.00108(14) 0.00060(13) S3 0.01172(18) 0.0186(2) 0.01857(19) 0.00093(14) 0.00113(14) -0.00151(14) S4 0.01438(19) 0.01335(19) 0.0224(2) 0.00027(14) 0.00088(14) -0.00087(13) C1 0.0159(7) 0.0155(7) 0.0210(8) 0.0031(6) -0.0011(6) -0.0003(6) C2 0.0181(8) 0.0222(8) 0.0258(9) 0.0047(7) 0.0018(6) 0.0000(6) C3 0.0220(9) 0.0243(9) 0.0346(10) 0.0080(8) -0.0020(7) -0.0068(7) C4 0.0347(11) 0.0172(9) 0.0356(10) 0.0041(7) -0.0047(8) -0.0057(7) C5 0.0320(10) 0.0168(8) 0.0345(10) -0.0016(7) 0.0016(8) 0.0027(7) C6 0.0203(8) 0.0186(8) 0.0295(9) 0.0003(7) 0.0018(7) 0.0022(7) C7 0.0155(7) 0.0165(8) 0.0190(7) -0.0012(6) -0.0003(6) 0.0016(6) C8 0.0185(8) 0.0297(10) 0.0259(9) -0.0044(7) 0.0039(7) -0.0019(7) C9 0.0245(9) 0.0441(12) 0.0269(9) -0.0138(9) 0.0047(7) -0.0002(8) C10 0.0251(9) 0.0321(10) 0.0337(10) -0.0157(8) -0.0031(8) 0.0001(8) C11 0.0182(8) 0.0211(8) 0.0339(10) -0.0042(7) -0.0025(7) -0.0014(7) C12 0.0148(7) 0.0182(8) 0.0239(8) 0.0011(6) -0.0002(6) 0.0004(6) C13 0.0175(8) 0.0161(7) 0.0210(8) -0.0022(6) 0.0005(6) 0.0003(6) C14 0.0207(8) 0.0173(8) 0.0336(9) 0.0005(7) 0.0032(7) -0.0016(7) C15 0.0343(10) 0.0157(8) 0.0408(11) 0.0025(8) 0.0016(8) -0.0026(7) C16 0.0371(11) 0.0174(9) 0.0399(11) -0.0032(8) -0.0026(9) 0.0059(8) C17 0.0232(9) 0.0265(10) 0.0340(10) -0.0065(8) -0.0005(7) 0.0076(7) C18 0.0168(8) 0.0241(9) 0.0266(9) -0.0029(7) 0.0013(6) 0.0012(7) C19 0.0155(7) 0.0162(8) 0.0218(8) -0.0002(6) -0.0017(6) -0.0017(6) C20 0.0172(8) 0.0308(10) 0.0255(9) 0.0014(7) 0.0029(7) 0.0027(7) C21 0.0248(10) 0.0422(12) 0.0282(10) 0.0087(9) 0.0045(8) 0.0021(8) C22 0.0243(9) 0.0342(11) 0.0329(10) 0.0129(8) -0.0031(8) 0.0008(8) C23 0.0179(8) 0.0229(9) 0.0347(10) 0.0030(7) -0.0038(7) 0.0012(7) C24 0.0152(7) 0.0189(8) 0.0250(8) -0.0016(6) 0.0002(6) -0.0007(6) C25 0.0212(8) 0.0230(9) 0.0302(9) -0.0058(7) 0.0074(7) 0.0012(7) C26 0.0432(13) 0.0469(14) 0.0402(12) -0.0194(10) 0.0147(10) -0.0104(11) C27 0.0321(11) 0.0336(11) 0.0384(11) -0.0085(9) -0.0037(9) -0.0063(9) C28 0.0176(8) 0.0364(10) 0.0273(9) -0.0036(8) 0.0008(7) -0.0065(7) C29 0.0213(10) 0.0459(13) 0.0540(14) 0.0209(11) 0.0074(9) 0.0095(9) C30 0.0269(10) 0.0357(11) 0.0332(10) 0.0086(8) 0.0004(8) 0.0080(8) C31 0.0366(12) 0.0396(13) 0.0481(13) 0.0185(10) 0.0150(10) 0.0074(10) C32 0.029(2) 0.0276(19) 0.038(2) 0.0125(17) 0.0188(17) 0.0072(15) C32A 0.022(3) 0.037(4) 0.055(5) 0.023(4) 0.007(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O9 1.898(3) . ? Li1 O6 1.899(3) . ? Li1 O3 1.922(3) . ? Li1 O1 1.937(3) . ? Li1 S1 3.029(3) . ? Li2 O2 1.899(3) 1_655 ? Li2 O10 1.904(3) . ? Li2 O7 1.940(3) . ? Li2 O5 1.942(3) . ? Li2 S3 3.039(3) . ? O1 S1 1.4556(12) . ? O2 S1 1.4502(12) . ? O2 Li2 1.899(3) 1_455 ? O3 S2 1.4596(12) . ? O4 S2 1.4354(12) . ? O5 S3 1.4532(12) . ? O6 S3 1.4534(12) . ? O7 S4 1.4591(12) . ? O8 S4 1.4375(13) . ? O9 C25 1.444(2) . ? O9 C28 1.446(2) . ? O10 C32A 1.434(7) . ? O10 C29 1.435(2) . ? O10 C32 1.474(4) . ? N1 S1 1.5752(14) . ? N1 S2 1.6014(14) . ? N2 S3 1.5759(15) . ? N2 S4 1.5985(14) . ? S1 C1 1.7675(17) . ? S2 C7 1.7647(17) . ? S3 C13 1.7654(17) . ? S4 C19 1.7673(17) . ? C1 C2 1.391(2) . ? C1 C6 1.397(2) . ? C2 C3 1.392(3) . ? C2 H2 0.97(2) . ? C3 C4 1.384(3) . ? C3 H3 0.94(2) . ? C4 C5 1.392(3) . ? C4 H4 0.94(3) . ? C5 C6 1.392(3) . ? C5 H5 0.94(3) . ? C6 H6 0.93(2) . ? C7 C12 1.393(2) . ? C7 C8 1.394(2) . ? C8 C9 1.386(3) . ? C8 H8 0.91(2) . ? C9 C10 1.389(3) . ? C9 H9 0.94(3) . ? C10 C11 1.383(3) . ? C10 H10 0.95(3) . ? C11 C12 1.393(2) . ? C11 H11 0.93(2) . ? C12 H12 0.93(2) . ? C13 C18 1.394(2) . ? C13 C14 1.395(2) . ? C14 C15 1.387(3) . ? C14 H14 0.93(2) . ? C15 C16 1.391(3) . ? C15 H15 0.97(3) . ? C16 C17 1.382(3) . ? C16 H16 0.93(3) . ? C17 C18 1.395(3) . ? C17 H17 0.93(2) . ? C18 H18 0.98(3) . ? C19 C20 1.391(2) . ? C19 C24 1.394(2) . ? C20 C21 1.386(3) . ? C20 H20 0.92(3) . ? C21 C22 1.390(3) . ? C21 H21 0.93(3) . ? C22 C23 1.383(3) . ? C22 H22 0.92(3) . ? C23 C24 1.395(3) . ? C23 H23 0.94(3) . ? C24 H24 0.93(2) . ? C25 C26 1.509(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.504(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.506(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.511(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.522(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32A 1.450(8) . ? C31 C32 1.491(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32A H32C 0.9900 . ? C32A H32D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Li1 O6 105.24(15) . . ? O9 Li1 O3 116.77(17) . . ? O6 Li1 O3 114.11(16) . . ? O9 Li1 O1 108.29(15) . . ? O6 Li1 O1 115.78(17) . . ? O3 Li1 O1 96.85(14) . . ? O9 Li1 S1 119.69(13) . . ? O6 Li1 S1 124.52(14) . . ? O3 Li1 S1 73.94(10) . . ? O2 Li2 O10 105.05(15) 1_655 . ? O2 Li2 O7 112.46(16) 1_655 . ? O10 Li2 O7 120.29(18) . . ? O2 Li2 O5 119.56(18) 1_655 . ? O10 Li2 O5 104.20(16) . . ? O7 Li2 O5 95.76(14) . . ? O2 Li2 S3 126.76(15) 1_655 . ? O10 Li2 S3 117.07(14) . . ? O7 Li2 S3 73.22(10) . . ? S1 O1 Li1 125.83(12) . . ? S1 O2 Li2 145.48(13) . 1_455 ? S2 O3 Li1 130.78(12) . . ? S3 O5 Li2 126.46(12) . . ? S3 O6 Li1 144.12(12) . . ? S4 O7 Li2 131.65(12) . . ? C25 O9 C28 109.68(14) . . ? C25 O9 Li1 125.96(14) . . ? C28 O9 Li1 123.79(14) . . ? C32A O10 C29 111.9(3) . . ? C29 O10 C32 105.4(2) . . ? C32A O10 Li2 120.7(3) . . ? C29 O10 Li2 124.00(15) . . ? C32 O10 Li2 129.9(2) . . ? S1 N1 S2 123.69(9) . . ? S3 N2 S4 123.56(9) . . ? O2 S1 O1 113.84(7) . . ? O2 S1 N1 106.03(7) . . ? O1 S1 N1 113.84(8) . . ? O2 S1 C1 107.06(8) . . ? O1 S1 C1 106.44(8) . . ? N1 S1 C1 109.41(8) . . ? O2 S1 Li1 140.47(8) . . ? N1 S1 Li1 86.78(8) . . ? C1 S1 Li1 103.23(8) . . ? O4 S2 O3 116.29(8) . . ? O4 S2 N1 106.78(8) . . ? O3 S2 N1 112.46(7) . . ? O4 S2 C7 107.66(8) . . ? O3 S2 C7 106.66(8) . . ? N1 S2 C7 106.49(8) . . ? O5 S3 O6 113.68(7) . . ? O5 S3 N2 113.96(8) . . ? O6 S3 N2 105.92(7) . . ? O5 S3 C13 106.53(8) . . ? O6 S3 C13 107.00(8) . . ? N2 S3 C13 109.53(8) . . ? O6 S3 Li2 140.42(8) . . ? N2 S3 Li2 87.49(8) . . ? C13 S3 Li2 102.87(8) . . ? O8 S4 O7 116.43(8) . . ? O8 S4 N2 106.68(8) . . ? O7 S4 N2 112.33(7) . . ? O8 S4 C19 107.18(8) . . ? O7 S4 C19 107.05(8) . . ? N2 S4 C19 106.66(8) . . ? C2 C1 C6 121.36(16) . . ? C2 C1 S1 119.82(13) . . ? C6 C1 S1 118.76(13) . . ? C1 C2 C3 119.11(18) . . ? C1 C2 H2 119.8(14) . . ? C3 C2 H2 121.1(14) . . ? C4 C3 C2 120.09(18) . . ? C4 C3 H3 120.9(15) . . ? C2 C3 H3 119.0(15) . . ? C3 C4 C5 120.58(18) . . ? C3 C4 H4 120.5(16) . . ? C5 C4 H4 118.9(16) . . ? C4 C5 C6 120.15(18) . . ? C4 C5 H5 122.6(16) . . ? C6 C5 H5 117.2(16) . . ? C5 C6 C1 118.70(17) . . ? C5 C6 H6 122.2(14) . . ? C1 C6 H6 119.0(14) . . ? C12 C7 C8 121.25(16) . . ? C12 C7 S2 120.44(13) . . ? C8 C7 S2 118.28(13) . . ? C9 C8 C7 118.90(18) . . ? C9 C8 H8 118.8(14) . . ? C7 C8 H8 122.2(14) . . ? C8 C9 C10 120.43(18) . . ? C8 C9 H9 120.3(17) . . ? C10 C9 H9 119.3(17) . . ? C11 C10 C9 120.24(18) . . ? C11 C10 H10 120.4(15) . . ? C9 C10 H10 119.3(15) . . ? C10 C11 C12 120.37(18) . . ? C10 C11 H11 118.9(15) . . ? C12 C11 H11 120.7(15) . . ? C11 C12 C7 118.78(16) . . ? C11 C12 H12 120.8(14) . . ? C7 C12 H12 120.3(14) . . ? C18 C13 C14 121.35(17) . . ? C18 C13 S3 119.69(14) . . ? C14 C13 S3 118.91(13) . . ? C15 C14 C13 118.79(17) . . ? C15 C14 H14 121.5(14) . . ? C13 C14 H14 119.7(14) . . ? C14 C15 C16 120.25(19) . . ? C14 C15 H15 117.9(16) . . ? C16 C15 H15 121.8(16) . . ? C17 C16 C15 120.67(19) . . ? C17 C16 H16 120.5(16) . . ? C15 C16 H16 118.8(16) . . ? C16 C17 C18 119.99(18) . . ? C16 C17 H17 122.6(15) . . ? C18 C17 H17 117.4(15) . . ? C13 C18 C17 118.92(18) . . ? C13 C18 H18 123.6(15) . . ? C17 C18 H18 117.4(15) . . ? C20 C19 C24 121.54(16) . . ? C20 C19 S4 118.06(13) . . ? C24 C19 S4 120.36(13) . . ? C21 C20 C19 119.00(18) . . ? C21 C20 H20 119.9(16) . . ? C19 C20 H20 121.1(16) . . ? C20 C21 C22 120.14(19) . . ? C20 C21 H21 118.8(16) . . ? C22 C21 H21 121.0(16) . . ? C23 C22 C21 120.50(18) . . ? C23 C22 H22 119.4(17) . . ? C21 C22 H22 120.0(17) . . ? C22 C23 C24 120.29(18) . . ? C22 C23 H23 121.4(15) . . ? C24 C23 H23 118.3(15) . . ? C19 C24 C23 118.50(17) . . ? C19 C24 H24 120.9(13) . . ? C23 C24 H24 120.6(13) . . ? O9 C25 C26 104.40(15) . . ? O9 C25 H25A 110.9 . . ? C26 C25 H25A 110.9 . . ? O9 C25 H25B 110.9 . . ? C26 C25 H25B 110.9 . . ? H25A C25 H25B 108.9 . . ? C27 C26 C25 103.80(17) . . ? C27 C26 H26A 111.0 . . ? C25 C26 H26A 111.0 . . ? C27 C26 H26B 111.0 . . ? C25 C26 H26B 111.0 . . ? H26A C26 H26B 109.0 . . ? C26 C27 C28 103.02(17) . . ? C26 C27 H27A 111.2 . . ? C28 C27 H27A 111.2 . . ? C26 C27 H27B 111.2 . . ? C28 C27 H27B 111.2 . . ? H27A C27 H27B 109.1 . . ? O9 C28 C27 106.84(15) . . ? O9 C28 H28A 110.4 . . ? C27 C28 H28A 110.4 . . ? O9 C28 H28B 110.4 . . ? C27 C28 H28B 110.4 . . ? H28A C28 H28B 108.6 . . ? O10 C29 C30 106.83(16) . . ? O10 C29 H29A 110.4 . . ? C30 C29 H29A 110.4 . . ? O10 C29 H29B 110.4 . . ? C30 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? C29 C30 C31 104.91(17) . . ? C29 C30 H30A 110.8 . . ? C31 C30 H30A 110.8 . . ? C29 C30 H30B 110.8 . . ? C31 C30 H30B 110.8 . . ? H30A C30 H30B 108.8 . . ? C32A C31 C30 108.7(3) . . ? C32 C31 C30 101.6(2) . . ? C32A C31 H31A 128.3 . . ? C32 C31 H31A 111.5 . . ? C30 C31 H31A 111.5 . . ? C32A C31 H31B 83.9 . . ? C32 C31 H31B 111.5 . . ? C30 C31 H31B 111.5 . . ? H31A C31 H31B 109.3 . . ? O10 C32 C31 103.1(3) . . ? O10 C32 H32A 111.2 . . ? C31 C32 H32A 111.2 . . ? O10 C32 H32B 111.2 . . ? C31 C32 H32B 111.2 . . ? H32A C32 H32B 109.1 . . ? O10 C32A C31 107.2(5) . . ? O10 C32A H32C 110.3 . . ? C31 C32A H32C 110.3 . . ? O10 C32A H32D 110.3 . . ? C31 C32A H32D 110.3 . . ? H32C C32A H32D 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 Li1 O1 S1 123.89(14) . . . . ? O6 Li1 O1 S1 -118.27(16) . . . . ? O3 Li1 O1 S1 2.7(2) . . . . ? O9 Li1 O3 S2 -94.48(19) . . . . ? O6 Li1 O3 S2 142.28(13) . . . . ? O1 Li1 O3 S2 20.0(2) . . . . ? S1 Li1 O3 S2 21.12(14) . . . . ? O2 Li2 O5 S3 115.33(18) 1_655 . . . ? O10 Li2 O5 S3 -127.84(14) . . . . ? O7 Li2 O5 S3 -4.6(2) . . . . ? O9 Li1 O6 S3 -122.97(19) . . . . ? O3 Li1 O6 S3 6.3(3) . . . . ? O1 Li1 O6 S3 117.5(2) . . . . ? S1 Li1 O6 S3 92.9(2) . . . . ? O2 Li2 O7 S4 -143.46(13) 1_655 . . . ? O10 Li2 O7 S4 92.0(2) . . . . ? O5 Li2 O7 S4 -18.1(2) . . . . ? S3 Li2 O7 S4 -19.97(15) . . . . ? O6 Li1 O9 C25 9.5(2) . . . . ? O3 Li1 O9 C25 -118.24(19) . . . . ? O1 Li1 O9 C25 133.85(16) . . . . ? S1 Li1 O9 C25 155.71(14) . . . . ? O6 Li1 O9 C28 -160.93(15) . . . . ? O3 Li1 O9 C28 71.4(2) . . . . ? O1 Li1 O9 C28 -36.5(2) . . . . ? S1 Li1 O9 C28 -14.7(2) . . . . ? O2 Li2 O10 C32A -21.8(5) 1_655 . . . ? O7 Li2 O10 C32A 106.2(5) . . . . ? O5 Li2 O10 C32A -148.3(5) . . . . ? S3 Li2 O10 C32A -168.2(5) . . . . ? O2 Li2 O10 C29 -179.5(2) 1_655 . . . ? O7 Li2 O10 C29 -51.5(3) . . . . ? O5 Li2 O10 C29 54.0(3) . . . . ? S3 Li2 O10 C29 34.1(3) . . . . ? O2 Li2 O10 C32 11.2(4) 1_655 . . . ? O7 Li2 O10 C32 139.2(3) . . . . ? O5 Li2 O10 C32 -115.3(3) . . . . ? S3 Li2 O10 C32 -135.2(3) . . . . ? Li2 O2 S1 O1 168.5(2) 1_455 . . . ? Li2 O2 S1 N1 42.6(2) 1_455 . . . ? Li2 O2 S1 C1 -74.2(2) 1_455 . . . ? Li2 O2 S1 Li1 147.4(2) 1_455 . . . ? Li1 O1 S1 O2 -153.81(14) . . . . ? Li1 O1 S1 N1 -32.12(16) . . . . ? Li1 O1 S1 C1 88.48(15) . . . . ? S2 N1 S1 O2 175.83(10) . . . . ? S2 N1 S1 O1 49.91(13) . . . . ? S2 N1 S1 C1 -69.02(12) . . . . ? S2 N1 S1 Li1 33.87(11) . . . . ? O9 Li1 S1 O2 -25.8(2) . . . . ? O6 Li1 S1 O2 113.64(17) . . . . ? O3 Li1 S1 O2 -137.83(11) . . . . ? O1 Li1 S1 O2 39.4(2) . . . . ? O9 Li1 S1 O1 -65.13(17) . . . . ? O6 Li1 S1 O1 74.28(19) . . . . ? O3 Li1 S1 O1 -177.2(2) . . . . ? O9 Li1 S1 N1 85.71(16) . . . . ? O6 Li1 S1 N1 -134.87(17) . . . . ? O3 Li1 S1 N1 -26.34(10) . . . . ? O1 Li1 S1 N1 150.85(15) . . . . ? O9 Li1 S1 C1 -165.10(15) . . . . ? O6 Li1 S1 C1 -25.69(18) . . . . ? O3 Li1 S1 C1 82.85(11) . . . . ? O1 Li1 S1 C1 -99.97(15) . . . . ? Li1 O3 S2 O4 114.73(16) . . . . ? Li1 O3 S2 N1 -8.82(18) . . . . ? Li1 O3 S2 C7 -125.20(16) . . . . ? S1 N1 S2 O4 -157.87(10) . . . . ? S1 N1 S2 O3 -29.17(13) . . . . ? S1 N1 S2 C7 87.32(11) . . . . ? Li2 O5 S3 O6 154.90(14) . . . . ? Li2 O5 S3 N2 33.39(17) . . . . ? Li2 O5 S3 C13 -87.51(16) . . . . ? Li1 O6 S3 O5 -171.3(2) . . . . ? Li1 O6 S3 N2 -45.4(2) . . . . ? Li1 O6 S3 C13 71.3(2) . . . . ? Li1 O6 S3 Li2 -151.3(2) . . . . ? S4 N2 S3 O5 -49.89(13) . . . . ? S4 N2 S3 O6 -175.61(10) . . . . ? S4 N2 S3 C13 69.32(12) . . . . ? S4 N2 S3 Li2 -33.45(11) . . . . ? O2 Li2 S3 O5 -78.9(2) 1_655 . . . ? O10 Li2 S3 O5 59.29(17) . . . . ? O7 Li2 S3 O5 175.2(2) . . . . ? O2 Li2 S3 O6 -116.50(18) 1_655 . . . ? O10 Li2 S3 O6 21.7(2) . . . . ? O7 Li2 S3 O6 137.67(11) . . . . ? O5 Li2 S3 O6 -37.6(2) . . . . ? O2 Li2 S3 N2 131.29(19) 1_655 . . . ? O10 Li2 S3 N2 -90.48(17) . . . . ? O7 Li2 S3 N2 25.46(10) . . . . ? O5 Li2 S3 N2 -149.78(15) . . . . ? O2 Li2 S3 C13 21.8(2) 1_655 . . . ? O10 Li2 S3 C13 160.05(16) . . . . ? O7 Li2 S3 C13 -84.01(11) . . . . ? O5 Li2 S3 C13 100.76(15) . . . . ? Li2 O7 S4 O8 -115.83(17) . . . . ? Li2 O7 S4 N2 7.58(18) . . . . ? Li2 O7 S4 C19 124.33(16) . . . . ? S3 N2 S4 O8 157.91(10) . . . . ? S3 N2 S4 O7 29.20(13) . . . . ? S3 N2 S4 C19 -87.79(12) . . . . ? O2 S1 C1 C2 -135.21(14) . . . . ? O1 S1 C1 C2 -13.11(16) . . . . ? N1 S1 C1 C2 110.32(14) . . . . ? Li1 S1 C1 C2 19.07(16) . . . . ? O2 S1 C1 C6 47.47(16) . . . . ? O1 S1 C1 C6 169.58(13) . . . . ? N1 S1 C1 C6 -67.00(15) . . . . ? Li1 S1 C1 C6 -158.24(14) . . . . ? C6 C1 C2 C3 -0.1(3) . . . . ? S1 C1 C2 C3 -177.31(14) . . . . ? C1 C2 C3 C4 -0.8(3) . . . . ? C2 C3 C4 C5 0.7(3) . . . . ? C3 C4 C5 C6 0.2(3) . . . . ? C4 C5 C6 C1 -1.1(3) . . . . ? C2 C1 C6 C5 1.0(3) . . . . ? S1 C1 C6 C5 178.26(14) . . . . ? O4 S2 C7 C12 148.32(14) . . . . ? O3 S2 C7 C12 22.83(16) . . . . ? N1 S2 C7 C12 -97.46(14) . . . . ? O4 S2 C7 C8 -33.18(16) . . . . ? O3 S2 C7 C8 -158.67(14) . . . . ? N1 S2 C7 C8 81.04(15) . . . . ? C12 C7 C8 C9 1.5(3) . . . . ? S2 C7 C8 C9 -176.98(16) . . . . ? C7 C8 C9 C10 0.0(3) . . . . ? C8 C9 C10 C11 -0.7(3) . . . . ? C9 C10 C11 C12 -0.1(3) . . . . ? C10 C11 C12 C7 1.6(3) . . . . ? C8 C7 C12 C11 -2.3(3) . . . . ? S2 C7 C12 C11 176.16(13) . . . . ? O5 S3 C13 C18 13.40(16) . . . . ? O6 S3 C13 C18 135.33(14) . . . . ? N2 S3 C13 C18 -110.29(15) . . . . ? Li2 S3 C13 C18 -18.37(16) . . . . ? O5 S3 C13 C14 -169.05(14) . . . . ? O6 S3 C13 C14 -47.12(16) . . . . ? N2 S3 C13 C14 67.26(16) . . . . ? Li2 S3 C13 C14 159.17(15) . . . . ? C18 C13 C14 C15 -1.6(3) . . . . ? S3 C13 C14 C15 -179.06(15) . . . . ? C13 C14 C15 C16 1.6(3) . . . . ? C14 C15 C16 C17 -0.4(3) . . . . ? C15 C16 C17 C18 -0.9(3) . . . . ? C14 C13 C18 C17 0.3(3) . . . . ? S3 C13 C18 C17 177.84(14) . . . . ? C16 C17 C18 C13 0.9(3) . . . . ? O8 S4 C19 C20 32.75(16) . . . . ? O7 S4 C19 C20 158.35(14) . . . . ? N2 S4 C19 C20 -81.21(15) . . . . ? O8 S4 C19 C24 -149.33(14) . . . . ? O7 S4 C19 C24 -23.72(16) . . . . ? N2 S4 C19 C24 96.72(15) . . . . ? C24 C19 C20 C21 -0.9(3) . . . . ? S4 C19 C20 C21 177.05(16) . . . . ? C19 C20 C21 C22 -0.7(3) . . . . ? C20 C21 C22 C23 1.1(3) . . . . ? C21 C22 C23 C24 0.0(3) . . . . ? C20 C19 C24 C23 2.0(3) . . . . ? S4 C19 C24 C23 -175.90(13) . . . . ? C22 C23 C24 C19 -1.5(3) . . . . ? C28 O9 C25 C26 19.3(2) . . . . ? Li1 O9 C25 C26 -152.23(19) . . . . ? O9 C25 C26 C27 -33.1(2) . . . . ? C25 C26 C27 C28 33.8(2) . . . . ? C25 O9 C28 C27 2.1(2) . . . . ? Li1 O9 C28 C27 173.87(17) . . . . ? C26 C27 C28 O9 -22.6(2) . . . . ? C32A O10 C29 C30 6.1(5) . . . . ? C32 O10 C29 C30 -23.0(3) . . . . ? Li2 O10 C29 C30 165.6(2) . . . . ? O10 C29 C30 C31 -3.0(3) . . . . ? C29 C30 C31 C32A -0.9(5) . . . . ? C29 C30 C31 C32 27.2(3) . . . . ? C32A O10 C32 C31 -67.1(8) . . . . ? C29 O10 C32 C31 40.8(3) . . . . ? Li2 O10 C32 C31 -148.5(2) . . . . ? C32A C31 C32 O10 67.0(7) . . . . ? C30 C31 C32 O10 -41.2(3) . . . . ? C29 O10 C32A C31 -6.7(7) . . . . ? C32 O10 C32A C31 75.0(8) . . . . ? Li2 O10 C32A C31 -166.9(3) . . . . ? C32 C31 C32A O10 -74.8(7) . . . . ? C30 C31 C32A O10 4.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.097 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.076 _chemical_compound_source Synthesized _exptl_crystal_recrystallization_method 'Slow cooling of a hot THF solution' data_kwh1203m _database_code_depnum_ccdc_archive 'CCDC 267872' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common 'Lithium bis(phenylsulfonyl)imide pyridine solvate' _chemical_melting_point ? _chemical_formula_moiety 'C22 H20 Li N3 O4 S2' _chemical_formula_sum 'C22 H20 Li N3 O4 S2' _chemical_formula_weight 461.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7604(6) _cell_length_b 12.8589(7) _cell_length_c 16.3444(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.549(1) _cell_angle_gamma 90.00 _cell_volume 2178.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8399 _cell_measurement_theta_min 2.524 _cell_measurement_theta_max 28.312 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.279 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.97 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details 'Blessing, R. H. (1995) Acta Cryst. A51, 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Siemens KFFMO2K-90' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23105 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.31 _reflns_number_total 5418 _reflns_number_gt 5025 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART/SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2001; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _refine_special_details ; All hydrogen atoms were placed at calculated positions and allowed to ride on the position of the parent atom. Thermal parameters for these hydrogens were set to 1.2\\times the equivalent isotropic U of the parent atom. All non-hydrogen atoms were refined with parameters for anisotropic thermal motion. No disorder was found in the final solution. No free molecules of solvent are found in the lattice. The largest peak in the final difference map, 0.726e/\%A^3^, was located near C1. 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^)+(0.0548P)^2^+0.9823P] 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 5418 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0975 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 0.9533(2) 0.60938(17) 0.26515(14) 0.0201(4) Uani 1 1 d . . . N1 N 0.84692(10) 0.91310(9) 0.25430(7) 0.0179(2) Uani 1 1 d . . . N2 N 0.82206(10) 0.48994(9) 0.24548(7) 0.0205(2) Uani 1 1 d . . . N3 N 1.03653(10) 0.63513(9) 0.39160(7) 0.0216(2) Uani 1 1 d . . . O1 O 0.90558(9) 1.09268(7) 0.28596(6) 0.02154(19) Uani 1 1 d . . . O2 O 0.68250(9) 1.05730(7) 0.20305(6) 0.0219(2) Uani 1 1 d . . . O3 O 0.84643(9) 0.72894(7) 0.22948(6) 0.0230(2) Uani 1 1 d . . . O4 O 0.65418(9) 0.80280(8) 0.26090(6) 0.0225(2) Uani 1 1 d . . . S1 S 0.79360(3) 1.02441(2) 0.269179(18) 0.01587(8) Uani 1 1 d . . . S2 S 0.75735(3) 0.81514(2) 0.220963(18) 0.01617(8) Uani 1 1 d . . . C1 C 0.74730(12) 1.02324(10) 0.36524(8) 0.0185(2) Uani 1 1 d . . . C2 C 0.64303(13) 1.08351(11) 0.37119(9) 0.0249(3) Uani 1 1 d . . . H2 H 0.5951 1.1223 0.3237 0.030 Uiso 1 1 calc R . . C3 C 0.60972(14) 1.08628(14) 0.44778(10) 0.0336(3) Uani 1 1 d . . . H3 H 0.5384 1.1270 0.4527 0.040 Uiso 1 1 calc R . . C4 C 0.67986(17) 1.03005(13) 0.51652(10) 0.0352(4) Uani 1 1 d . . . H4 H 0.6554 1.0311 0.5682 0.042 Uiso 1 1 calc R . . C5 C 0.78577(19) 0.97199(13) 0.51080(10) 0.0371(4) Uani 1 1 d . . . H5 H 0.8348 0.9347 0.5588 0.045 Uiso 1 1 calc R . . C6 C 0.81997(16) 0.96847(12) 0.43471(9) 0.0292(3) Uani 1 1 d . . . H6 H 0.8925 0.9289 0.4303 0.035 Uiso 1 1 calc R . . C7 C 0.68702(12) 0.82818(9) 0.11047(8) 0.0178(2) Uani 1 1 d . . . C8 C 0.76065(14) 0.80428(11) 0.05491(9) 0.0261(3) Uani 1 1 d . . . H8 H 0.8477 0.7823 0.0761 0.031 Uiso 1 1 calc R . . C9 C 0.70544(17) 0.81286(13) -0.03196(10) 0.0334(3) Uani 1 1 d . . . H9 H 0.7547 0.7963 -0.0705 0.040 Uiso 1 1 calc R . . C10 C 0.57908(16) 0.84549(12) -0.06247(9) 0.0303(3) Uani 1 1 d . . . H10 H 0.5422 0.8521 -0.1219 0.036 Uiso 1 1 calc R . . C11 C 0.50621(15) 0.86857(12) -0.00707(10) 0.0313(3) Uani 1 1 d . . . H11 H 0.4193 0.8906 -0.0285 0.038 Uiso 1 1 calc R . . C12 C 0.55985(13) 0.85970(12) 0.08016(9) 0.0267(3) Uani 1 1 d . . . H12 H 0.5098 0.8751 0.1185 0.032 Uiso 1 1 calc R . . C13 C 0.70516(12) 0.51193(11) 0.25613(9) 0.0215(3) Uani 1 1 d . . . H13 H 0.6899 0.5801 0.2736 0.026 Uiso 1 1 calc R . . C14 C 0.60586(12) 0.43990(11) 0.24286(9) 0.0224(3) Uani 1 1 d . . . H14 H 0.5252 0.4581 0.2522 0.027 Uiso 1 1 calc R . . C15 C 0.62633(12) 0.34098(11) 0.21579(9) 0.0226(3) Uani 1 1 d . . . H15 H 0.5597 0.2903 0.2058 0.027 Uiso 1 1 calc R . . C16 C 0.74573(13) 0.31709(10) 0.20355(9) 0.0223(3) Uani 1 1 d . . . H16 H 0.7622 0.2501 0.1843 0.027 Uiso 1 1 calc R . . C17 C 0.84065(12) 0.39327(10) 0.22007(8) 0.0212(3) Uani 1 1 d . . . H17 H 0.9230 0.3761 0.2130 0.025 Uiso 1 1 calc R . . C18 C 1.02909(14) 0.72724(11) 0.42726(9) 0.0265(3) Uani 1 1 d . . . H18 H 0.9798 0.7804 0.3931 0.032 Uiso 1 1 calc R . . C19 C 1.08916(16) 0.74975(13) 0.51139(10) 0.0328(3) Uani 1 1 d . . . H19 H 1.0805 0.8164 0.5343 0.039 Uiso 1 1 calc R . . C20 C 1.16164(16) 0.67341(15) 0.56109(10) 0.0365(4) Uani 1 1 d . . . H20 H 1.2041 0.6862 0.6191 0.044 Uiso 1 1 calc R . . C21 C 1.17127(19) 0.57814(16) 0.52501(11) 0.0459(5) Uani 1 1 d . . . H21 H 1.2212 0.5241 0.5577 0.055 Uiso 1 1 calc R . . C22 C 1.10732(17) 0.56215(13) 0.44059(10) 0.0364(4) Uani 1 1 d . . . H22 H 1.1142 0.4960 0.4163 0.044 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 0.0164(10) 0.0212(10) 0.0219(10) -0.0002(8) 0.0037(8) 0.0012(8) N1 0.0114(4) 0.0220(5) 0.0193(5) -0.0028(4) 0.0026(4) 0.0014(4) N2 0.0144(5) 0.0233(5) 0.0236(5) 0.0000(4) 0.0048(4) -0.0011(4) N3 0.0186(5) 0.0258(6) 0.0200(5) 0.0012(4) 0.0044(4) 0.0022(4) O1 0.0174(4) 0.0243(5) 0.0236(4) -0.0018(4) 0.0067(3) -0.0060(4) O2 0.0173(4) 0.0236(5) 0.0217(4) 0.0030(4) -0.0002(3) 0.0026(3) O3 0.0212(4) 0.0215(5) 0.0245(5) 0.0015(4) 0.0029(4) 0.0074(4) O4 0.0175(4) 0.0274(5) 0.0246(5) 0.0017(4) 0.0089(4) -0.0015(4) S1 0.01210(14) 0.01853(15) 0.01663(15) 0.00010(10) 0.00323(11) -0.00047(10) S2 0.01273(14) 0.01819(15) 0.01693(15) 0.00066(10) 0.00284(11) 0.00204(10) C1 0.0187(6) 0.0194(6) 0.0188(6) -0.0034(4) 0.0073(5) -0.0042(4) C2 0.0162(6) 0.0296(7) 0.0291(7) -0.0072(5) 0.0062(5) -0.0035(5) C3 0.0230(7) 0.0443(9) 0.0382(8) -0.0188(7) 0.0162(6) -0.0097(6) C4 0.0452(9) 0.0386(9) 0.0289(7) -0.0140(6) 0.0220(7) -0.0185(7) C5 0.0609(11) 0.0301(8) 0.0219(7) 0.0002(6) 0.0136(7) -0.0011(7) C6 0.0397(8) 0.0265(7) 0.0219(7) 0.0002(5) 0.0094(6) 0.0072(6) C7 0.0174(6) 0.0169(5) 0.0171(5) -0.0013(4) 0.0010(4) -0.0005(4) C8 0.0240(7) 0.0311(7) 0.0227(6) -0.0026(5) 0.0054(5) 0.0052(5) C9 0.0399(9) 0.0394(9) 0.0206(7) -0.0044(6) 0.0073(6) 0.0065(7) C10 0.0382(8) 0.0266(7) 0.0199(6) -0.0029(5) -0.0028(6) -0.0014(6) C11 0.0230(7) 0.0354(8) 0.0281(7) 0.0009(6) -0.0057(5) 0.0026(6) C12 0.0177(6) 0.0348(8) 0.0253(7) -0.0008(6) 0.0018(5) 0.0037(5) C13 0.0186(6) 0.0220(6) 0.0250(6) 0.0011(5) 0.0079(5) 0.0016(5) C14 0.0139(5) 0.0284(7) 0.0253(6) 0.0060(5) 0.0060(5) 0.0016(5) C15 0.0155(6) 0.0266(6) 0.0241(6) 0.0043(5) 0.0026(5) -0.0048(5) C16 0.0208(6) 0.0199(6) 0.0253(6) 0.0007(5) 0.0046(5) 0.0002(5) C17 0.0143(5) 0.0239(6) 0.0252(6) 0.0009(5) 0.0049(5) 0.0016(5) C18 0.0279(7) 0.0244(7) 0.0234(6) 0.0008(5) 0.0006(5) -0.0023(5) C19 0.0379(8) 0.0309(8) 0.0253(7) -0.0052(6) 0.0010(6) -0.0085(6) C20 0.0306(8) 0.0541(10) 0.0199(7) 0.0011(7) -0.0016(6) -0.0039(7) C21 0.0484(10) 0.0571(11) 0.0262(8) 0.0086(8) -0.0001(7) 0.0239(9) C22 0.0436(9) 0.0375(9) 0.0258(7) 0.0020(6) 0.0053(6) 0.0188(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 O3 1.915(2) . ? Li1 O1 1.931(2) 2_745 ? Li1 N3 2.047(2) . ? Li1 N2 2.052(2) . ? N1 S1 1.5849(11) . ? N1 S2 1.5908(11) . ? N2 C17 1.3425(17) . ? N2 C13 1.3453(16) . ? N3 C18 1.3318(18) . ? N3 C22 1.3323(18) . ? O1 S1 1.4562(9) . ? O1 Li1 1.931(2) 2_755 ? O2 S1 1.4434(9) . ? O3 S2 1.4474(9) . ? O4 S2 1.4396(9) . ? S1 C1 1.7700(13) . ? S2 C7 1.7690(12) . ? C1 C6 1.3859(19) . ? C1 C2 1.3884(18) . ? C2 C3 1.392(2) . ? C2 H2 0.9500 . ? C3 C4 1.378(3) . ? C3 H3 0.9500 . ? C4 C5 1.386(3) . ? C4 H4 0.9500 . ? C5 C6 1.389(2) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.3851(18) . ? C7 C8 1.3903(18) . ? C8 C9 1.389(2) . ? C8 H8 0.9500 . ? C9 C10 1.382(2) . ? C9 H9 0.9500 . ? C10 C11 1.380(2) . ? C10 H10 0.9500 . ? C11 C12 1.392(2) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.3865(18) . ? C13 H13 0.9500 . ? C14 C15 1.384(2) . ? C14 H14 0.9500 . ? C15 C16 1.3867(18) . ? C15 H15 0.9500 . ? C16 C17 1.3885(18) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.3842(19) . ? C18 H18 0.9500 . ? C19 C20 1.376(2) . ? C19 H19 0.9500 . ? C20 C21 1.375(3) . ? C20 H20 0.9500 . ? C21 C22 1.382(2) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? 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 O3 Li1 O1 115.80(12) . 2_745 ? O3 Li1 N3 104.01(11) . . ? O1 Li1 N3 105.83(11) 2_745 . ? O3 Li1 N2 102.78(11) . . ? O1 Li1 N2 115.90(12) 2_745 . ? N3 Li1 N2 112.07(11) . . ? S1 N1 S2 123.82(6) . . ? C17 N2 C13 117.17(11) . . ? C17 N2 Li1 126.02(11) . . ? C13 N2 Li1 116.77(11) . . ? C18 N3 C22 117.08(12) . . ? C18 N3 Li1 121.62(11) . . ? C22 N3 Li1 121.17(12) . . ? S1 O1 Li1 133.82(9) . 2_755 ? S2 O3 Li1 166.47(9) . . ? O2 S1 O1 116.22(6) . . ? O2 S1 N1 114.26(6) . . ? O1 S1 N1 104.95(6) . . ? O2 S1 C1 107.05(6) . . ? O1 S1 C1 104.69(6) . . ? N1 S1 C1 109.15(6) . . ? O4 S2 O3 116.32(6) . . ? O4 S2 N1 113.71(6) . . ? O3 S2 N1 104.40(6) . . ? O4 S2 C7 107.60(6) . . ? O3 S2 C7 105.18(6) . . ? N1 S2 C7 109.19(6) . . ? C6 C1 C2 121.02(13) . . ? C6 C1 S1 120.00(10) . . ? C2 C1 S1 118.84(10) . . ? C1 C2 C3 119.02(14) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 120.19(14) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.53(14) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C4 C5 C6 119.85(15) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C1 C6 C5 119.36(15) . . ? C1 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C12 C7 C8 120.82(12) . . ? C12 C7 S2 120.28(10) . . ? C8 C7 S2 118.89(10) . . ? C9 C8 C7 119.19(13) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C10 C9 C8 120.19(14) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 120.38(13) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 120.13(14) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C7 C12 C11 119.27(13) . . ? C7 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? N2 C13 C14 123.19(12) . . ? N2 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C15 C14 C13 118.82(12) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C14 C15 C16 118.87(12) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? C15 C16 C17 118.51(12) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? N2 C17 C16 123.41(12) . . ? N2 C17 H17 118.3 . . ? C16 C17 H17 118.3 . . ? N3 C18 C19 123.63(14) . . ? N3 C18 H18 118.2 . . ? C19 C18 H18 118.2 . . ? C20 C19 C18 118.51(15) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? C21 C20 C19 118.58(14) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? C20 C21 C22 119.07(15) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? N3 C22 C21 123.13(16) . . ? N3 C22 H22 118.4 . . ? C21 C22 H22 118.4 . . ? 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 O3 Li1 N2 C17 145.02(12) . . . . ? O1 Li1 N2 C17 17.70(19) 2_745 . . . ? N3 Li1 N2 C17 -103.90(14) . . . . ? O3 Li1 N2 C13 -32.43(15) . . . . ? O1 Li1 N2 C13 -159.74(12) 2_745 . . . ? N3 Li1 N2 C13 78.66(15) . . . . ? O3 Li1 N3 C18 -11.62(17) . . . . ? O1 Li1 N3 C18 110.85(14) 2_745 . . . ? N2 Li1 N3 C18 -121.93(13) . . . . ? O3 Li1 N3 C22 172.59(13) . . . . ? O1 Li1 N3 C22 -64.94(17) 2_745 . . . ? N2 Li1 N3 C22 62.28(17) . . . . ? O1 Li1 O3 S2 -159.8(3) 2_745 . . . ? N3 Li1 O3 S2 -44.1(4) . . . . ? N2 Li1 O3 S2 72.8(4) . . . . ? Li1 O1 S1 O2 -83.52(13) 2_755 . . . ? Li1 O1 S1 N1 43.75(13) 2_755 . . . ? Li1 O1 S1 C1 158.64(12) 2_755 . . . ? S2 N1 S1 O2 -42.63(10) . . . . ? S2 N1 S1 O1 -171.08(7) . . . . ? S2 N1 S1 C1 77.17(9) . . . . ? Li1 O3 S2 O4 -28.4(4) . . . . ? Li1 O3 S2 N1 97.7(4) . . . . ? Li1 O3 S2 C7 -147.4(4) . . . . ? S1 N1 S2 O4 -43.83(10) . . . . ? S1 N1 S2 O3 -171.61(8) . . . . ? S1 N1 S2 C7 76.34(9) . . . . ? O2 S1 C1 C6 162.11(11) . . . . ? O1 S1 C1 C6 -73.97(12) . . . . ? N1 S1 C1 C6 37.95(13) . . . . ? O2 S1 C1 C2 -22.25(12) . . . . ? O1 S1 C1 C2 101.67(11) . . . . ? N1 S1 C1 C2 -146.41(10) . . . . ? C6 C1 C2 C3 -1.7(2) . . . . ? S1 C1 C2 C3 -177.29(11) . . . . ? C1 C2 C3 C4 0.2(2) . . . . ? C2 C3 C4 C5 1.4(2) . . . . ? C3 C4 C5 C6 -1.4(2) . . . . ? C2 C1 C6 C5 1.6(2) . . . . ? S1 C1 C6 C5 177.17(12) . . . . ? C4 C5 C6 C1 -0.1(2) . . . . ? O4 S2 C7 C12 21.47(13) . . . . ? O3 S2 C7 C12 146.08(11) . . . . ? N1 S2 C7 C12 -102.38(12) . . . . ? O4 S2 C7 C8 -157.24(11) . . . . ? O3 S2 C7 C8 -32.63(12) . . . . ? N1 S2 C7 C8 78.91(12) . . . . ? C12 C7 C8 C9 0.3(2) . . . . ? S2 C7 C8 C9 179.05(12) . . . . ? C7 C8 C9 C10 0.4(2) . . . . ? C8 C9 C10 C11 -0.8(2) . . . . ? C9 C10 C11 C12 0.4(2) . . . . ? C8 C7 C12 C11 -0.8(2) . . . . ? S2 C7 C12 C11 -179.46(11) . . . . ? C10 C11 C12 C7 0.4(2) . . . . ? C17 N2 C13 C14 0.6(2) . . . . ? Li1 N2 C13 C14 178.23(12) . . . . ? N2 C13 C14 C15 -1.3(2) . . . . ? C13 C14 C15 C16 0.5(2) . . . . ? C14 C15 C16 C17 0.8(2) . . . . ? C13 N2 C17 C16 0.9(2) . . . . ? Li1 N2 C17 C16 -176.52(13) . . . . ? C15 C16 C17 N2 -1.6(2) . . . . ? C22 N3 C18 C19 -0.7(2) . . . . ? Li1 N3 C18 C19 -176.67(14) . . . . ? N3 C18 C19 C20 0.6(2) . . . . ? C18 C19 C20 C21 0.0(3) . . . . ? C19 C20 C21 C22 -0.5(3) . . . . ? C18 N3 C22 C21 0.2(3) . . . . ? Li1 N3 C22 C21 176.21(17) . . . . ? C20 C21 C22 N3 0.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.726 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.063 _exptl_crystal_recrystallization_method 'Slow cooling of a hot pyridine solution' data_sodiate _database_code_depnum_ccdc_archive 'CCDC 267873' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H19 Na O5 S2' _chemical_formula_weight 390.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Na Na 0.0362 0.0249 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.9292(1) _cell_length_b 27.1577(5) _cell_length_c 11.2618(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.258(1) _cell_angle_gamma 90.00 _cell_volume 1802.61(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'clear colourless' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.344 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3669 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 26.36 _reflns_number_total 3669 _reflns_number_gt 2862 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Denzo & Collect' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0395P)^2^+1.1429P] 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 3669 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0916 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Na1 Na 1.20749(13) 0.04342(3) 0.06694(7) 0.0224(2) Uani 1 1 d . . . S1 S 0.66781(8) 0.077395(18) -0.05928(4) 0.01844(13) Uani 1 1 d . . . S2 S 0.88935(8) 0.151221(18) 0.10598(4) 0.01966(13) Uani 1 1 d . . . O1 O 0.4405(2) 0.05703(5) -0.08155(13) 0.0241(3) Uani 1 1 d . . . O2 O 0.8508(2) 0.04163(5) -0.03908(13) 0.0230(3) Uani 1 1 d . . . O3 O 1.0988(2) 0.12409(5) 0.10043(13) 0.0247(3) Uani 1 1 d . . . O4 O 0.8466(3) 0.17203(5) 0.21939(13) 0.0278(4) Uani 1 1 d . . . O5 O 1.3506(3) 0.03055(7) 0.26084(15) 0.0437(5) Uani 1 1 d . . . C1 C 0.6659(4) 0.11589(7) 0.05699(18) 0.0199(4) Uani 1 1 d . . . C2 C 0.7221(3) 0.10933(7) -0.19109(18) 0.0195(4) Uani 1 1 d . . . C3 C 0.9173(4) 0.10032(9) -0.2443(2) 0.0287(5) Uani 1 1 d . . . H3 H 1.0224 0.0759 -0.2132 0.034 Uiso 1 1 calc R . . C4 C 0.9570(4) 0.12773(10) -0.3447(2) 0.0376(6) Uani 1 1 d . . . H4 H 1.0895 0.1217 -0.3829 0.045 Uiso 1 1 calc R . . C5 C 0.8066(5) 0.16323(9) -0.3887(2) 0.0382(6) Uani 1 1 d . . . H5 H 0.8356 0.1817 -0.4571 0.046 Uiso 1 1 calc R . . C6 C 0.6130(5) 0.17235(9) -0.3344(2) 0.0371(6) Uani 1 1 d . . . H6 H 0.5092 0.1971 -0.3651 0.045 Uiso 1 1 calc R . . C7 C 0.5708(4) 0.14533(8) -0.23502(19) 0.0285(5) Uani 1 1 d . . . H7 H 0.4381 0.1515 -0.1971 0.034 Uiso 1 1 calc R . . C8 C 0.9028(3) 0.20192(7) 0.00634(18) 0.0207(4) Uani 1 1 d . . . C9 C 1.0841(4) 0.20630(8) -0.0611(2) 0.0275(5) Uani 1 1 d . . . H9 H 1.2057 0.1834 -0.0514 0.033 Uiso 1 1 calc R . . C10 C 1.0866(4) 0.24443(8) -0.1429(2) 0.0326(5) Uani 1 1 d . . . H10 H 1.2109 0.2479 -0.1888 0.039 Uiso 1 1 calc R . . C11 C 0.9089(4) 0.27735(8) -0.1576(2) 0.0319(5) Uani 1 1 d . . . H11 H 0.9107 0.3033 -0.2142 0.038 Uiso 1 1 calc R . . C12 C 0.7271(4) 0.27286(8) -0.0904(2) 0.0293(5) Uani 1 1 d . . . H12 H 0.6048 0.2956 -0.1011 0.035 Uiso 1 1 calc R . . C13 C 0.7245(4) 0.23524(7) -0.00770(19) 0.0245(5) Uani 1 1 d . . . H13 H 0.6014 0.2322 0.0392 0.029 Uiso 1 1 calc R . . C14 C 1.2355(10) 0.0450(7) 0.3554(7) 0.050(2) Uani 0.80(4) 1 d P . . H14A H 1.1990 0.0162 0.4036 0.060 Uiso 0.80(4) 1 calc PR . . H14B H 1.0927 0.0621 0.3263 0.060 Uiso 0.80(4) 1 calc PR . . C14A C 1.241(4) 0.0625(14) 0.364(2) 0.035(6) Uiso 0.20(4) 1 d P . . H14C H 1.1254 0.0862 0.3291 0.042 Uiso 0.20(4) 1 d PR . . H14D H 1.1657 0.0382 0.4120 0.042 Uiso 0.20(4) 1 d PR . . C15 C 1.4023(5) 0.08090(11) 0.4313(3) 0.0565(8) Uani 1 1 d . . . H15A H 1.3601 0.1157 0.4149 0.068 Uiso 1 1 calc R . . H15B H 1.4026 0.0745 0.5179 0.068 Uiso 1 1 calc R . . C16 C 1.6298(5) 0.06935(11) 0.3905(2) 0.0470(7) Uani 1 1 d . . . H16A H 1.7402 0.0598 0.4589 0.056 Uiso 1 1 calc R . . H16B H 1.6900 0.0981 0.3502 0.056 Uiso 1 1 calc R . . C17 C 1.5847(4) 0.02709(10) 0.3047(2) 0.0419(6) Uani 1 1 d . . . H17A H 1.6806 0.0298 0.2384 0.050 Uiso 1 1 calc R . . H17B H 1.6170 -0.0047 0.3460 0.050 Uiso 1 1 calc R . . H1 H 0.528(4) 0.1284(8) 0.067(2) 0.024(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0213(4) 0.0218(4) 0.0238(4) 0.0001(3) 0.0011(3) 0.0014(3) S1 0.0170(3) 0.0185(2) 0.0198(3) 0.0001(2) 0.00194(19) -0.0001(2) S2 0.0203(3) 0.0204(3) 0.0182(3) -0.0019(2) 0.0017(2) 0.0014(2) O1 0.0189(7) 0.0260(8) 0.0274(8) -0.0007(6) 0.0022(6) -0.0050(6) O2 0.0231(8) 0.0191(7) 0.0262(8) -0.0001(6) 0.0000(6) 0.0049(6) O3 0.0205(8) 0.0240(7) 0.0290(8) -0.0025(6) -0.0003(6) 0.0020(6) O4 0.0352(9) 0.0300(8) 0.0183(8) -0.0059(6) 0.0036(7) 0.0007(7) O5 0.0412(10) 0.0605(12) 0.0276(10) 0.0028(8) -0.0049(8) -0.0014(9) C1 0.0188(11) 0.0222(10) 0.0196(11) -0.0006(8) 0.0057(8) 0.0006(9) C2 0.0215(10) 0.0209(10) 0.0161(10) -0.0014(8) 0.0018(8) -0.0025(8) C3 0.0232(11) 0.0386(13) 0.0246(12) -0.0018(10) 0.0046(9) 0.0015(10) C4 0.0311(13) 0.0587(16) 0.0245(12) -0.0020(12) 0.0099(10) -0.0056(12) C5 0.0478(16) 0.0461(15) 0.0208(12) 0.0047(11) 0.0041(11) -0.0106(13) C6 0.0495(16) 0.0357(13) 0.0251(13) 0.0072(10) -0.0003(11) 0.0061(12) C7 0.0291(12) 0.0322(12) 0.0242(12) 0.0019(9) 0.0034(9) 0.0053(10) C8 0.0218(11) 0.0208(10) 0.0192(11) -0.0026(8) 0.0005(8) -0.0032(9) C9 0.0236(11) 0.0289(11) 0.0305(12) -0.0025(9) 0.0053(9) -0.0008(9) C10 0.0316(13) 0.0347(13) 0.0332(13) 0.0025(10) 0.0111(10) -0.0056(11) C11 0.0424(14) 0.0246(11) 0.0282(13) 0.0040(9) 0.0010(11) -0.0065(10) C12 0.0307(12) 0.0247(11) 0.0317(13) 0.0004(9) -0.0010(10) 0.0028(10) C13 0.0229(11) 0.0242(11) 0.0266(12) -0.0031(9) 0.0031(9) -0.0003(9) C14 0.046(2) 0.069(6) 0.038(3) 0.010(3) 0.0127(18) -0.007(3) C15 0.073(2) 0.0461(16) 0.0547(19) -0.0029(14) 0.0264(17) 0.0025(16) C16 0.0507(17) 0.0577(17) 0.0331(15) -0.0082(13) 0.0061(13) -0.0099(14) C17 0.0442(15) 0.0462(15) 0.0320(14) -0.0005(12) -0.0103(12) 0.0092(13) _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 Na1 O5 2.2818(18) . ? Na1 O1 2.3122(17) 1_655 ? Na1 O2 2.3130(16) . ? Na1 O3 2.3262(16) . ? Na1 O2 2.3513(15) 3_755 ? Na1 S1 3.3417(9) 1_655 ? Na1 S1 3.3664(9) 3_755 ? Na1 Na1 3.6165(15) 3_755 ? S1 O1 1.4529(14) . ? S1 O2 1.4555(14) . ? S1 C1 1.677(2) . ? S1 C2 1.779(2) . ? S1 Na1 3.3417(9) 1_455 ? S1 Na1 3.3664(9) 3_755 ? S2 O4 1.4440(15) . ? S2 O3 1.4512(15) . ? S2 C1 1.680(2) . ? S2 C8 1.784(2) . ? O1 Na1 2.3122(17) 1_455 ? O2 Na1 2.3513(15) 3_755 ? O5 C14 1.383(11) . ? O5 C17 1.424(3) . ? O5 C14A 1.64(3) . ? C1 H1 0.90(2) . ? C2 C7 1.381(3) . ? C2 C3 1.382(3) . ? C3 C4 1.395(3) . ? C3 H3 0.9500 . ? C4 C5 1.369(4) . ? C4 H4 0.9500 . ? C5 C6 1.381(4) . ? C5 H5 0.9500 . ? C6 C7 1.384(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.387(3) . ? C8 C9 1.387(3) . ? C9 C10 1.387(3) . ? C9 H9 0.9500 . ? C10 C11 1.378(3) . ? C10 H10 0.9500 . ? C11 C12 1.388(3) . ? C11 H11 0.9500 . ? C12 C13 1.383(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.573(15) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 H14C 1.3127 . ? C14 H14D 0.8180 . ? C14A H14C 0.9900 . ? C14A H14D 0.9900 . ? C15 C16 1.505(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.505(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Na1 O1 121.83(7) . 1_655 ? O5 Na1 O2 135.60(7) . . ? O1 Na1 O2 102.41(6) 1_655 . ? O5 Na1 O3 94.00(6) . . ? O1 Na1 O3 99.48(6) 1_655 . ? O2 Na1 O3 81.35(5) . . ? O5 Na1 O2 90.64(6) . 3_755 ? O1 Na1 O2 98.70(6) 1_655 3_755 ? O2 Na1 O2 78.33(5) . 3_755 ? O3 Na1 O2 155.17(6) . 3_755 ? O5 Na1 S1 102.33(5) . 1_655 ? O1 Na1 S1 21.25(4) 1_655 1_655 ? O2 Na1 S1 121.97(5) . 1_655 ? O3 Na1 S1 93.58(4) . 1_655 ? O2 Na1 S1 109.24(5) 3_755 1_655 ? O5 Na1 S1 79.36(5) . 3_755 ? O1 Na1 S1 89.26(4) 1_655 3_755 ? O2 Na1 S1 99.05(4) . 3_755 ? O3 Na1 S1 170.98(5) . 3_755 ? O2 Na1 S1 21.37(4) 3_755 3_755 ? S1 Na1 S1 93.81(2) 1_655 3_755 ? O5 Na1 Na1 117.66(6) . 3_755 ? O1 Na1 Na1 103.64(5) 1_655 3_755 ? O2 Na1 Na1 39.55(4) . 3_755 ? O3 Na1 Na1 119.59(5) . 3_755 ? O2 Na1 Na1 38.78(4) 3_755 3_755 ? S1 Na1 Na1 123.56(4) 1_655 3_755 ? S1 Na1 Na1 59.68(2) 3_755 3_755 ? O1 S1 O2 115.75(8) . . ? O1 S1 C1 106.68(10) . . ? O2 S1 C1 111.25(10) . . ? O1 S1 C2 106.88(9) . . ? O2 S1 C2 104.85(9) . . ? C1 S1 C2 111.41(10) . . ? O1 S1 Na1 35.23(6) . 1_455 ? O2 S1 Na1 112.25(6) . 1_455 ? C1 S1 Na1 76.38(7) . 1_455 ? C2 S1 Na1 136.06(7) . 1_455 ? O1 S1 Na1 80.02(6) . 3_755 ? O2 S1 Na1 36.06(6) . 3_755 ? C1 S1 Na1 130.39(7) . 3_755 ? C2 S1 Na1 113.19(7) . 3_755 ? Na1 S1 Na1 86.19(2) 1_455 3_755 ? O4 S2 O3 118.05(9) . . ? O4 S2 C1 107.82(10) . . ? O3 S2 C1 110.12(9) . . ? O4 S2 C8 106.17(9) . . ? O3 S2 C8 105.52(9) . . ? C1 S2 C8 108.80(10) . . ? S1 O1 Na1 123.52(9) . 1_455 ? S1 O2 Na1 133.69(8) . . ? S1 O2 Na1 122.57(8) . 3_755 ? Na1 O2 Na1 101.67(5) . 3_755 ? S2 O3 Na1 137.62(9) . . ? C14 O5 C17 107.2(3) . . ? C14 O5 C14A 15.7(8) . . ? C17 O5 C14A 103.6(9) . . ? C14 O5 Na1 122.0(3) . . ? C17 O5 Na1 126.06(16) . . ? C14A O5 Na1 117.5(9) . . ? S1 C1 S2 122.72(13) . . ? S1 C1 H1 114.5(14) . . ? S2 C1 H1 115.8(14) . . ? C7 C2 C3 120.8(2) . . ? C7 C2 S1 118.33(16) . . ? C3 C2 S1 120.79(16) . . ? C2 C3 C4 118.7(2) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 120.6(2) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.4(2) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C7 119.7(2) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C2 C7 C6 119.8(2) . . ? C2 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C13 C8 C9 120.5(2) . . ? C13 C8 S2 119.31(16) . . ? C9 C8 S2 120.08(16) . . ? C10 C9 C8 119.5(2) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C11 C10 C9 120.1(2) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.4(2) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 119.9(2) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C8 119.6(2) . . ? C12 C13 H13 120.2 . . ? C8 C13 H13 120.2 . . ? O5 C14 C15 105.1(4) . . ? O5 C14 H14A 110.7 . . ? C15 C14 H14A 110.7 . . ? O5 C14 H14B 110.7 . . ? C15 C14 H14B 110.7 . . ? H14A C14 H14B 108.8 . . ? O5 C14 H14C 110.1 . . ? C15 C14 H14C 82.1 . . ? H14A C14 H14C 131.6 . . ? H14B C14 H14C 30.5 . . ? O5 C14 H14D 150.4 . . ? C15 C14 H14D 93.4 . . ? H14A C14 H14D 40.0 . . ? H14B C14 H14D 83.0 . . ? H14C C14 H14D 95.0 . . ? O5 C14A H14C 111.9 . . ? O5 C14A H14D 105.7 . . ? H14C C14A H14D 108.4 . . ? C16 C15 C14 103.7(4) . . ? C16 C15 H15A 111.0 . . ? C14 C15 H15A 111.0 . . ? C16 C15 H15B 111.0 . . ? C14 C15 H15B 111.0 . . ? H15A C15 H15B 109.0 . . ? C15 C16 C17 104.6(2) . . ? C15 C16 H16A 110.8 . . ? C17 C16 H16A 110.8 . . ? C15 C16 H16B 110.8 . . ? C17 C16 H16B 110.8 . . ? H16A C16 H16B 108.9 . . ? O5 C17 C16 105.7(2) . . ? O5 C17 H17A 110.6 . . ? C16 C17 H17A 110.6 . . ? O5 C17 H17B 110.6 . . ? C16 C17 H17B 110.6 . . ? H17A C17 H17B 108.7 . . ? 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 Na1 92.63(11) . . . 1_455 ? C1 S1 O1 Na1 -31.74(12) . . . 1_455 ? C2 S1 O1 Na1 -151.03(10) . . . 1_455 ? Na1 S1 O1 Na1 97.61(8) 3_755 . . 1_455 ? O1 S1 O2 Na1 -152.10(11) . . . . ? C1 S1 O2 Na1 -30.13(15) . . . . ? C2 S1 O2 Na1 90.42(13) . . . . ? Na1 S1 O2 Na1 -113.59(11) 1_455 . . . ? Na1 S1 O2 Na1 -160.44(19) 3_755 . . . ? O1 S1 O2 Na1 8.34(13) . . . 3_755 ? C1 S1 O2 Na1 130.32(10) . . . 3_755 ? C2 S1 O2 Na1 -109.13(10) . . . 3_755 ? Na1 S1 O2 Na1 46.85(11) 1_455 . . 3_755 ? O5 Na1 O2 S1 84.49(15) . . . . ? O1 Na1 O2 S1 -100.27(13) 1_655 . . . ? O3 Na1 O2 S1 -2.39(12) . . . . ? O2 Na1 O2 S1 163.26(16) 3_755 . . . ? S1 Na1 O2 S1 -91.21(13) 1_655 . . . ? S1 Na1 O2 S1 168.49(11) 3_755 . . . ? Na1 Na1 O2 S1 163.26(16) 3_755 . . . ? O5 Na1 O2 Na1 -78.77(10) . . . 3_755 ? O1 Na1 O2 Na1 96.47(6) 1_655 . . 3_755 ? O3 Na1 O2 Na1 -165.65(7) . . . 3_755 ? O2 Na1 O2 Na1 0.0 3_755 . . 3_755 ? S1 Na1 O2 Na1 105.53(6) 1_655 . . 3_755 ? S1 Na1 O2 Na1 5.23(5) 3_755 . . 3_755 ? O4 S2 O3 Na1 114.12(13) . . . . ? C1 S2 O3 Na1 -10.24(17) . . . . ? C8 S2 O3 Na1 -127.49(13) . . . . ? O5 Na1 O3 S2 -108.71(14) . . . . ? O1 Na1 O3 S2 128.08(13) 1_655 . . . ? O2 Na1 O3 S2 26.84(14) . . . . ? O2 Na1 O3 S2 -8.5(2) 3_755 . . . ? S1 Na1 O3 S2 148.64(13) 1_655 . . . ? S1 Na1 O3 S2 -66.4(4) 3_755 . . . ? Na1 Na1 O3 S2 16.38(16) 3_755 . . . ? O1 Na1 O5 C14 148.8(9) 1_655 . . . ? O2 Na1 O5 C14 -36.7(9) . . . . ? O3 Na1 O5 C14 45.0(9) . . . . ? O2 Na1 O5 C14 -110.6(9) 3_755 . . . ? S1 Na1 O5 C14 139.6(9) 1_655 . . . ? S1 Na1 O5 C14 -128.8(9) 3_755 . . . ? Na1 Na1 O5 C14 -81.5(9) 3_755 . . . ? O1 Na1 O5 C17 -3.7(2) 1_655 . . . ? O2 Na1 O5 C17 170.86(16) . . . . ? O3 Na1 O5 C17 -107.42(19) . . . . ? O2 Na1 O5 C17 96.99(19) 3_755 . . . ? S1 Na1 O5 C17 -12.87(19) 1_655 . . . ? S1 Na1 O5 C17 78.74(18) 3_755 . . . ? Na1 Na1 O5 C17 126.02(18) 3_755 . . . ? O1 Na1 O5 C14A 131.4(14) 1_655 . . . ? O2 Na1 O5 C14A -54.1(14) . . . . ? O3 Na1 O5 C14A 27.6(14) . . . . ? O2 Na1 O5 C14A -128.0(14) 3_755 . . . ? S1 Na1 O5 C14A 122.2(14) 1_655 . . . ? S1 Na1 O5 C14A -146.2(14) 3_755 . . . ? Na1 Na1 O5 C14A -98.9(14) 3_755 . . . ? O1 S1 C1 S2 -174.77(12) . . . . ? O2 S1 C1 S2 58.14(16) . . . . ? C2 S1 C1 S2 -58.47(16) . . . . ? Na1 S1 C1 S2 167.04(15) 1_455 . . . ? Na1 S1 C1 S2 94.24(14) 3_755 . . . ? O4 S2 C1 S1 -168.97(12) . . . . ? O3 S2 C1 S1 -38.90(17) . . . . ? C8 S2 C1 S1 76.30(16) . . . . ? O1 S1 C2 C7 54.93(18) . . . . ? O2 S1 C2 C7 178.31(16) . . . . ? C1 S1 C2 C7 -61.24(19) . . . . ? Na1 S1 C2 C7 31.2(2) 1_455 . . . ? Na1 S1 C2 C7 141.09(15) 3_755 . . . ? O1 S1 C2 C3 -128.69(17) . . . . ? O2 S1 C2 C3 -5.31(19) . . . . ? C1 S1 C2 C3 115.14(18) . . . . ? Na1 S1 C2 C3 -152.43(14) 1_455 . . . ? Na1 S1 C2 C3 -42.53(19) 3_755 . . . ? C7 C2 C3 C4 -1.1(3) . . . . ? S1 C2 C3 C4 -177.36(17) . . . . ? C2 C3 C4 C5 0.7(3) . . . . ? C3 C4 C5 C6 -0.1(4) . . . . ? C4 C5 C6 C7 -0.1(4) . . . . ? C3 C2 C7 C6 0.8(3) . . . . ? S1 C2 C7 C6 177.21(18) . . . . ? C5 C6 C7 C2 -0.2(4) . . . . ? O4 S2 C8 C13 -53.72(18) . . . . ? O3 S2 C8 C13 -179.78(16) . . . . ? C1 S2 C8 C13 62.08(19) . . . . ? O4 S2 C8 C9 129.82(17) . . . . ? O3 S2 C8 C9 3.76(19) . . . . ? C1 S2 C8 C9 -114.38(18) . . . . ? C13 C8 C9 C10 0.2(3) . . . . ? S2 C8 C9 C10 176.58(17) . . . . ? C8 C9 C10 C11 -0.7(3) . . . . ? C9 C10 C11 C12 0.4(3) . . . . ? C10 C11 C12 C13 0.2(3) . . . . ? C11 C12 C13 C8 -0.7(3) . . . . ? C9 C8 C13 C12 0.5(3) . . . . ? S2 C8 C13 C12 -175.92(16) . . . . ? C17 O5 C14 C15 35.0(9) . . . . ? C14A O5 C14 C15 -44(4) . . . . ? Na1 O5 C14 C15 -121.9(3) . . . . ? O5 C14 C15 C16 -18.4(8) . . . . ? C14 C15 C16 C17 -3.9(5) . . . . ? C14 O5 C17 C16 -38.2(8) . . . . ? C14A O5 C17 C16 -22.4(13) . . . . ? Na1 O5 C17 C16 117.5(2) . . . . ? C15 C16 C17 O5 24.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.289 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.055 data_lithiate _database_code_depnum_ccdc_archive 'CCDC 267874' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H19 Li O5 S2' _chemical_formula_weight 374.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.7976(4) _cell_length_b 34.489(3) _cell_length_c 9.0798(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.882(2) _cell_angle_gamma 90.00 _cell_volume 1762.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'clear colorless' _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.326 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9751 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.0897 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 24.72 _reflns_number_total 2947 _reflns_number_gt 1784 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Denzo & Collect' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0536P)^2^+1.4060P] 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 2947 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1131 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1339 _refine_ls_wR_factor_gt 0.1149 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 -0.3902(12) 0.0731(2) 0.5954(7) 0.0359(18) Uani 1 1 d . . . S1 S 0.14530(19) 0.08701(3) 0.70861(11) 0.0288(3) Uani 1 1 d . . . S2 S -0.13517(19) 0.14898(3) 0.53198(11) 0.0296(3) Uani 1 1 d . . . O1 O 0.3748(5) 0.06914(7) 0.7146(3) 0.0323(7) Uani 1 1 d . . . O2 O -0.0562(5) 0.06086(7) 0.6922(3) 0.0316(7) Uani 1 1 d . . . O3 O -0.1644(5) 0.16561(8) 0.3826(3) 0.0392(8) Uani 1 1 d . . . O4 O -0.3381(5) 0.12868(7) 0.5648(3) 0.0355(7) Uani 1 1 d . . . O5 O -0.4754(5) 0.04495(8) 0.4117(3) 0.0437(8) Uani 1 1 d . . . C1 C 0.0997(8) 0.11946(12) 0.5667(4) 0.0282(10) Uani 1 1 d . . . C2 C -0.0828(7) 0.18907(11) 0.6582(4) 0.0265(10) Uani 1 1 d . . . C3 C -0.2295(8) 0.19594(13) 0.7551(5) 0.0432(12) Uani 1 1 d . . . H3 H -0.3612 0.1795 0.7539 0.052 Uiso 1 1 calc R . . C4 C -0.1821(10) 0.22702(14) 0.8535(5) 0.0562(14) Uani 1 1 d . . . H4 H -0.2798 0.2315 0.9221 0.067 Uiso 1 1 calc R . . C5 C 0.0038(10) 0.25134(14) 0.8532(6) 0.0537(14) Uani 1 1 d . . . H5 H 0.0343 0.2726 0.9215 0.064 Uiso 1 1 calc R . . C6 C 0.1467(8) 0.24520(13) 0.7550(5) 0.0453(12) Uani 1 1 d . . . H6 H 0.2736 0.2625 0.7532 0.054 Uiso 1 1 calc R . . C7 C 0.1041(8) 0.21356(12) 0.6586(5) 0.0392(11) Uani 1 1 d . . . H7 H 0.2049 0.2087 0.5921 0.047 Uiso 1 1 calc R . . C8 C 0.1665(7) 0.11049(11) 0.8852(4) 0.0274(10) Uani 1 1 d . . . C9 C -0.0080(8) 0.10592(12) 0.9640(5) 0.0366(11) Uani 1 1 d . . . H9 H -0.1387 0.0891 0.9266 0.044 Uiso 1 1 calc R . . C10 C 0.0097(8) 0.12620(13) 1.0987(5) 0.0444(12) Uani 1 1 d . . . H10 H -0.1089 0.1231 1.1540 0.053 Uiso 1 1 calc R . . C11 C 0.1981(9) 0.15059(14) 1.1517(5) 0.0470(12) Uani 1 1 d . . . H11 H 0.2079 0.1645 1.2434 0.056 Uiso 1 1 calc R . . C12 C 0.3737(8) 0.15524(13) 1.0739(5) 0.0466(13) Uani 1 1 d . . . H12 H 0.5045 0.1720 1.1118 0.056 Uiso 1 1 calc R . . C13 C 0.3563(8) 0.13506(12) 0.9394(5) 0.0386(11) Uani 1 1 d . . . H13 H 0.4753 0.1382 0.8844 0.046 Uiso 1 1 calc R . . C14 C -0.7092(8) 0.03505(13) 0.3277(5) 0.0444(12) Uani 1 1 d . B . H14A H -0.8138 0.0581 0.3135 0.053 Uiso 1 1 calc R . . H14B H -0.7786 0.0149 0.3815 0.053 Uiso 1 1 calc R . . C15 C -0.6826(8) 0.02002(13) 0.1761(5) 0.0455(12) Uani 1 1 d . . . H15A H -0.6744 -0.0087 0.1759 0.055 Uiso 1 1 calc R B . H15B H -0.8165 0.0286 0.0929 0.055 Uiso 1 1 calc R . . C16 C -0.4511(9) 0.03775(15) 0.1609(5) 0.0580(14) Uani 1 1 d . B . H16A H -0.3729 0.0214 0.0976 0.070 Uiso 1 1 calc R A 1 H16B H -0.4761 0.0641 0.1163 0.070 Uiso 1 1 calc R A 1 C17 C -0.3088(11) 0.0391(3) 0.3218(7) 0.043(3) Uani 0.768(16) 1 d P B 1 H17A H -0.2214 0.0145 0.3496 0.052 Uiso 0.768(16) 1 calc PR B 1 H17B H -0.1929 0.0607 0.3362 0.052 Uiso 0.768(16) 1 calc PR B 1 C17A C -0.376(4) 0.0647(9) 0.277(2) 0.039(7) Uiso 0.232(16) 1 d P B 2 H17C H -0.4471 0.0906 0.2494 0.047 Uiso 0.232(16) 1 calc PR B 2 H17D H -0.2003 0.0671 0.3058 0.047 Uiso 0.232(16) 1 calc PR B 2 H1 H 0.236(7) 0.1290(11) 0.546(4) 0.046(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.035(4) 0.044(5) 0.030(4) -0.003(3) 0.010(3) 0.001(3) S1 0.0298(6) 0.0320(6) 0.0257(6) 0.0014(5) 0.0089(4) 0.0019(5) S2 0.0313(6) 0.0325(6) 0.0245(6) -0.0012(5) 0.0056(4) 0.0011(5) O1 0.0307(17) 0.0360(17) 0.0314(16) 0.0030(13) 0.0097(13) 0.0083(13) O2 0.0298(17) 0.0344(16) 0.0318(16) -0.0006(13) 0.0096(13) -0.0042(13) O3 0.051(2) 0.0423(18) 0.0220(15) 0.0073(13) 0.0049(14) 0.0087(15) O4 0.0255(16) 0.0336(17) 0.0476(18) -0.0050(14) 0.0095(14) -0.0032(13) O5 0.0332(19) 0.059(2) 0.0406(18) -0.0201(16) 0.0126(15) -0.0092(16) C1 0.029(3) 0.030(2) 0.027(2) -0.0033(19) 0.010(2) 0.000(2) C2 0.029(2) 0.031(2) 0.021(2) 0.0013(18) 0.0075(18) 0.001(2) C3 0.049(3) 0.039(3) 0.046(3) -0.006(2) 0.021(2) -0.010(2) C4 0.072(4) 0.058(4) 0.048(3) -0.020(3) 0.034(3) -0.009(3) C5 0.076(4) 0.039(3) 0.045(3) -0.013(2) 0.012(3) -0.008(3) C6 0.042(3) 0.039(3) 0.054(3) -0.004(2) 0.010(3) -0.011(2) C7 0.045(3) 0.037(3) 0.040(3) -0.006(2) 0.019(2) -0.004(2) C8 0.026(2) 0.033(2) 0.023(2) 0.0011(19) 0.0038(18) 0.003(2) C9 0.031(3) 0.044(3) 0.035(3) 0.000(2) 0.009(2) -0.001(2) C10 0.047(3) 0.062(3) 0.029(2) -0.001(2) 0.017(2) 0.003(3) C11 0.054(3) 0.057(3) 0.028(2) -0.005(2) 0.007(2) 0.002(3) C12 0.050(3) 0.054(3) 0.031(3) -0.006(2) 0.000(2) -0.012(2) C13 0.036(3) 0.049(3) 0.032(3) 0.002(2) 0.010(2) -0.006(2) C14 0.035(3) 0.047(3) 0.048(3) -0.007(2) 0.004(2) -0.005(2) C15 0.050(3) 0.048(3) 0.033(3) -0.004(2) -0.001(2) -0.007(2) C16 0.072(4) 0.067(4) 0.037(3) -0.001(3) 0.017(3) -0.014(3) C17 0.037(4) 0.057(6) 0.039(4) -0.011(4) 0.017(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O5 1.890(7) . ? Li1 O1 1.937(7) 1_455 ? Li1 O2 1.970(7) . ? Li1 O4 1.972(7) . ? S1 O2 1.455(3) . ? S1 O1 1.455(3) . ? S1 C1 1.679(4) . ? S1 C8 1.774(4) . ? S2 O3 1.445(3) . ? S2 O4 1.460(3) . ? S2 C1 1.669(4) . ? S2 C2 1.775(4) . ? O1 Li1 1.937(7) 1_655 ? O5 C17 1.420(6) . ? O5 C14 1.428(5) . ? O5 C17A 1.62(2) . ? C1 H1 0.92(4) . ? C2 C7 1.373(5) . ? C2 C3 1.383(5) . ? C3 C4 1.380(6) . ? C3 H3 0.9500 . ? C4 C5 1.366(6) . ? C4 H4 0.9500 . ? C5 C6 1.372(6) . ? C5 H5 0.9500 . ? C6 C7 1.384(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.381(5) . ? C8 C13 1.383(5) . ? C9 C10 1.391(6) . ? C9 H9 0.9500 . ? C10 C11 1.371(6) . ? C10 H10 0.9500 . ? C11 C12 1.381(6) . ? C11 H11 0.9500 . ? C12 C13 1.388(6) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.513(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.511(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17A 1.40(2) . ? C16 C17 1.496(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17A H17C 0.9900 . ? C17A H17D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Li1 O1 112.8(4) . 1_455 ? O5 Li1 O2 107.8(3) . . ? O1 Li1 O2 118.9(4) 1_455 . ? O5 Li1 O4 113.0(4) . . ? O1 Li1 O4 107.4(3) 1_455 . ? O2 Li1 O4 95.9(3) . . ? O2 S1 O1 116.47(16) . . ? O2 S1 C1 111.10(19) . . ? O1 S1 C1 106.56(19) . . ? O2 S1 C8 104.79(17) . . ? O1 S1 C8 107.16(17) . . ? C1 S1 C8 110.70(18) . . ? O3 S2 O4 117.60(18) . . ? O3 S2 C1 109.03(19) . . ? O4 S2 C1 109.3(2) . . ? O3 S2 C2 105.10(17) . . ? O4 S2 C2 105.24(17) . . ? C1 S2 C2 110.36(19) . . ? S1 O1 Li1 135.1(3) . 1_655 ? S1 O2 Li1 126.3(3) . . ? S2 O4 Li1 130.8(3) . . ? C17 O5 C14 110.4(4) . . ? C17 O5 C17A 38.0(9) . . ? C14 O5 C17A 99.4(8) . . ? C17 O5 Li1 120.7(4) . . ? C14 O5 Li1 127.4(3) . . ? C17A O5 Li1 112.6(8) . . ? S2 C1 S1 121.5(3) . . ? S2 C1 H1 117(3) . . ? S1 C1 H1 114(3) . . ? C7 C2 C3 119.9(4) . . ? C7 C2 S2 119.5(3) . . ? C3 C2 S2 120.6(3) . . ? C4 C3 C2 119.2(4) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C5 C4 C3 120.7(5) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.4(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C7 119.3(4) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? C2 C7 C6 120.5(4) . . ? C2 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C9 C8 C13 120.3(4) . . ? C9 C8 S1 121.0(3) . . ? C13 C8 S1 118.6(3) . . ? C8 C9 C10 119.3(4) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C11 C10 C9 120.1(4) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.9(4) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C13 119.0(4) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C8 C13 C12 120.3(4) . . ? C8 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? O5 C14 C15 106.1(4) . . ? O5 C14 H14A 110.5 . . ? C15 C14 H14A 110.5 . . ? O5 C14 H14B 110.5 . . ? C15 C14 H14B 110.5 . . ? H14A C14 H14B 108.7 . . ? C16 C15 C14 103.4(4) . . ? C16 C15 H15A 111.1 . . ? C14 C15 H15A 111.1 . . ? C16 C15 H15B 111.1 . . ? C14 C15 H15B 111.1 . . ? H15A C15 H15B 109.1 . . ? C17A C16 C17 40.6(11) . . ? C17A C16 C15 108.9(9) . . ? C17 C16 C15 102.6(4) . . ? C17A C16 H16A 135.6 . . ? C17 C16 H16A 111.3 . . ? C15 C16 H16A 111.3 . . ? C17A C16 H16B 71.8 . . ? C17 C16 H16B 111.3 . . ? C15 C16 H16B 111.3 . . ? H16A C16 H16B 109.2 . . ? O5 C17 C16 105.9(5) . . ? O5 C17 H17A 110.6 . . ? C16 C17 H17A 110.6 . . ? O5 C17 H17B 110.6 . . ? C16 C17 H17B 110.6 . . ? H17A C17 H17B 108.7 . . ? C16 C17A O5 100.7(14) . . ? C16 C17A H17C 111.6 . . ? O5 C17A H17C 111.6 . . ? C16 C17A H17D 111.6 . . ? O5 C17A H17D 111.6 . . ? H17C C17A H17D 109.4 . . ? 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 O2 S1 O1 Li1 121.0(4) . . . 1_655 ? C1 S1 O1 Li1 -3.6(4) . . . 1_655 ? C8 S1 O1 Li1 -122.1(4) . . . 1_655 ? O1 S1 O2 Li1 -151.7(3) . . . . ? C1 S1 O2 Li1 -29.4(3) . . . . ? C8 S1 O2 Li1 90.2(3) . . . . ? O5 Li1 O2 S1 109.9(3) . . . . ? O1 Li1 O2 S1 -120.2(4) 1_455 . . . ? O4 Li1 O2 S1 -6.6(4) . . . . ? O3 S2 O4 Li1 109.9(3) . . . . ? C1 S2 O4 Li1 -15.0(4) . . . . ? C2 S2 O4 Li1 -133.5(3) . . . . ? O5 Li1 O4 S2 -78.6(5) . . . . ? O1 Li1 O4 S2 156.3(3) 1_455 . . . ? O2 Li1 O4 S2 33.5(4) . . . . ? O1 Li1 O5 C17 -169.5(6) 1_455 . . . ? O2 Li1 O5 C17 -36.3(6) . . . . ? O4 Li1 O5 C17 68.4(6) . . . . ? O1 Li1 O5 C14 25.9(6) 1_455 . . . ? O2 Li1 O5 C14 159.2(4) . . . . ? O4 Li1 O5 C14 -96.1(5) . . . . ? O1 Li1 O5 C17A 148.7(12) 1_455 . . . ? O2 Li1 O5 C17A -78.1(12) . . . . ? O4 Li1 O5 C17A 26.6(12) . . . . ? O3 S2 C1 S1 -164.4(2) . . . . ? O4 S2 C1 S1 -34.6(3) . . . . ? C2 S2 C1 S1 80.7(3) . . . . ? O2 S1 C1 S2 57.4(3) . . . . ? O1 S1 C1 S2 -174.7(2) . . . . ? C8 S1 C1 S2 -58.6(3) . . . . ? O3 S2 C2 C7 -57.1(4) . . . . ? O4 S2 C2 C7 178.0(3) . . . . ? C1 S2 C2 C7 60.3(4) . . . . ? O3 S2 C2 C3 122.4(4) . . . . ? O4 S2 C2 C3 -2.4(4) . . . . ? C1 S2 C2 C3 -120.2(4) . . . . ? C7 C2 C3 C4 -1.4(7) . . . . ? S2 C2 C3 C4 179.1(4) . . . . ? C2 C3 C4 C5 1.6(8) . . . . ? C3 C4 C5 C6 -0.1(8) . . . . ? C4 C5 C6 C7 -1.5(8) . . . . ? C3 C2 C7 C6 -0.2(7) . . . . ? S2 C2 C7 C6 179.4(3) . . . . ? C5 C6 C7 C2 1.6(7) . . . . ? O2 S1 C8 C9 -8.5(4) . . . . ? O1 S1 C8 C9 -132.9(3) . . . . ? C1 S1 C8 C9 111.3(4) . . . . ? O2 S1 C8 C13 174.5(3) . . . . ? O1 S1 C8 C13 50.2(4) . . . . ? C1 S1 C8 C13 -65.6(4) . . . . ? C13 C8 C9 C10 -0.2(6) . . . . ? S1 C8 C9 C10 -177.1(3) . . . . ? C8 C9 C10 C11 0.4(6) . . . . ? C9 C10 C11 C12 -0.6(7) . . . . ? C10 C11 C12 C13 0.6(7) . . . . ? C9 C8 C13 C12 0.3(6) . . . . ? S1 C8 C13 C12 177.3(3) . . . . ? C11 C12 C13 C8 -0.5(7) . . . . ? C17 O5 C14 C15 2.9(6) . . . . ? C17A O5 C14 C15 40.7(11) . . . . ? Li1 O5 C14 C15 168.8(4) . . . . ? O5 C14 C15 C16 -22.8(5) . . . . ? C14 C15 C16 C17A -8.8(15) . . . . ? C14 C15 C16 C17 33.0(6) . . . . ? C14 O5 C17 C16 18.5(7) . . . . ? C17A O5 C17 C16 -60.4(12) . . . . ? Li1 O5 C17 C16 -148.4(4) . . . . ? C17A C16 C17 O5 72.5(13) . . . . ? C15 C16 C17 O5 -32.0(7) . . . . ? C17 C16 C17A O5 -54.9(12) . . . . ? C15 C16 C17A O5 32.4(18) . . . . ? C17 O5 C17A C16 65.6(15) . . . . ? C14 O5 C17A C16 -45.6(16) . . . . ? Li1 O5 C17A C16 177.1(11) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 24.72 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.399 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.067