#------------------------------------------------------------------------------ #$Date: 2024-02-05 13:04:56 +0100 (Mon, 05 Feb 2024) $ #$Revision: 289680 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/29/2022962.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2022962 loop_ _publ_author_name 'Kumagai, Hitoshi' 'Kawata, Satoshi' 'Ogihara, Nobuhiro' _publ_section_title ; Crystal structure of dilithium biphenyl-4,4'-di-sulfonate dihydrate. ; _journal_coeditor_code JP2001 _journal_issue 'Pt 1' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 22 _journal_page_last 24 _journal_paper_doi 10.1107/S2056989023010411 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac '[Li2 (C12 H8 O6 S2) (H2 O1)2]' _chemical_formula_moiety 'C12 H12 Li2 O8 S2' _chemical_formula_sum 'C12 H12 Li2 O8 S2' _chemical_formula_weight 362.22 _chemical_name_systematic ; \m-Biphenyl-4,4'-disulfonato-bis(aqualithium) ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.0000 _cell_angle_beta 99.994(7) _cell_angle_gamma 90.0000 _cell_formula_units_Z 2 _cell_length_a 15.8584(11) _cell_length_b 5.3693(4) _cell_length_c 8.8636(6) _cell_measurement_reflns_used 17604 _cell_measurement_temperature 286 _cell_measurement_theta_max 27.63 _cell_measurement_theta_min 3.19 _cell_volume 743.27(9) _computing_cell_refinement ; RAPID-AUTO (Rigaku, 1995) ; _computing_data_collection ; RAPID-AUTO (Rigaku, 1995) ; _computing_data_reduction ; RAPID-AUTO (Rigaku, 1995) ; _computing_molecular_graphics ; CrystalStructure 4.3 (Rigaku, 2019 ; _computing_publication_material ; CrystalStructure 4.3 (Rigaku, 2019) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014/5 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 286 _diffrn_detector_area_resol_mean 10.000 _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_unetI/netI 0.0520 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 9858 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.473 _diffrn_reflns_theta_min 3.914 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.396 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_correction_T_min 0.213 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (ABSCOR; Rigaku, 1995) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 372.00 _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.74 _refine_diff_density_min -0.28 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 133 _refine_ls_number_reflns 1666 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0606 _refine_ls_shift/su_max 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0948P)^2^+0.3642P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1551 _refine_ls_wR_factor_ref 0.1593 _reflns_number_gt 1490 _reflns_number_total 1666 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file jp2001sup1.cif _cod_data_source_block I _cod_depositor_comments 'Adding full bibliography for 2022962.cif.' _cod_database_code 2022962 _cod_database_fobs_code 2022962 _shelx_hkl_file ; -2 0 1 1.21 0.13 2 0 -1 0.56 0.28 2 0 -1 1.36 0.17 -2 0 1 1.82 0.24 -2 0 -1 0.60 0.40 -2 0 -1 0.38 0.09 0 -1 0 1.07 0.29 0 1 0 0.10 0.32 0 1 0 0.66 0.23 3 0 0 2641.10 335.51 1 -1 0 643.59 31.73 1 1 0 651.15 30.13 1 -1 0 597.44 29.18 -1 -1 0 680.34 32.09 -1 1 0 622.47 31.12 -1 1 0 604.13 29.44 -1 -1 0 649.26 30.58 1 1 0 630.48 30.23 -3 0 1 0.91 0.60 3 0 -1 0.16 0.15 -3 0 1 0.51 0.25 3 0 -1 0.35 0.32 0 1 1 8219.34 1383.34 0 1 -1 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11.70 2.57 -10 6 1 13.69 2.32 4 5 7 25.41 2.15 -4 -5 -7 24.55 2.96 -4 -5 -7 21.10 1.64 -4 5 -7 21.10 1.47 4 -5 7 19.79 1.57 -4 5 -7 24.93 1.74 4 -5 7 20.40 1.51 4 5 7 20.02 1.95 -7 3 10 30.38 2.03 7 -3 -10 27.98 1.94 7 3 -10 27.28 1.93 7 3 -10 25.07 1.90 -7 3 10 25.41 2.72 7 -3 -10 22.25 2.74 -11 3 -7 0.05 0.93 -11 -3 -7 -1.39 0.82 -11 3 -7 0.79 0.90 -11 -3 -7 -0.34 0.87 -6 -1 -10 1.10 0.89 -6 1 -10 1.28 1.41 7 -5 6 6.53 1.29 -7 -5 -6 7.43 1.16 7 -5 6 8.85 2.70 -7 -5 -6 7.55 1.42 -7 5 -6 6.19 1.26 7 5 6 6.71 0.87 -8 -2 -9 12.30 2.32 -8 2 -9 11.17 1.57 -8 2 -9 14.76 1.58 -8 -2 -9 11.09 1.54 6 -6 -5 3.27 1.90 6 -6 -5 6.18 1.38 -6 6 5 3.83 1.27 -6 -6 5 5.68 1.94 14 -5 -1 1.60 0.96 14 -5 -1 -0.10 0.91 14 5 -1 1.18 0.89 14 5 -1 -0.64 0.94 -14 5 1 2.32 0.97 -14 5 1 2.42 0.89 18 0 -7 -0.65 1.55 -16 4 4 -0.65 0.97 16 -4 -4 -1.27 1.25 -16 4 4 -0.52 1.23 16 4 -4 -0.28 1.62 16 -4 -4 -0.78 0.97 -3 6 -5 -0.70 0.64 -3 -6 -5 -0.58 0.79 3 -6 5 0.33 0.60 -3 6 -5 0.09 0.70 -3 -6 -5 -0.02 0.79 3 -6 5 0.01 0.75 3 6 5 0.24 0.74 3 6 5 -0.90 1.32 14 5 -2 6.20 1.37 -14 5 2 7.94 1.34 14 5 -2 7.80 2.07 14 -5 -2 8.32 1.30 14 -5 -2 6.71 1.37 -1 3 -10 10.46 1.04 -1 3 -10 7.79 1.03 1 3 10 11.70 1.57 -1 -3 -10 10.98 1.41 -1 1 -11 -0.40 0.63 -1 1 -11 1.28 0.93 -1 -1 -11 0.37 1.15 -1 -1 -11 -0.32 0.66 16 4 1 9.82 1.11 -16 4 -1 12.84 1.49 -16 4 -1 11.20 1.13 16 -4 1 9.00 1.13 16 -4 1 11.52 1.41 16 4 1 8.40 1.67 -16 -4 -1 8.56 0.95 -7 4 9 4.15 1.08 7 -4 -9 5.06 1.76 7 -4 -9 6.01 1.82 -7 4 9 6.88 1.15 7 4 -9 5.85 1.12 7 4 -9 5.77 1.65 -10 -6 0 11.83 1.57 -10 6 0 12.70 1.58 10 -6 0 10.99 1.51 10 6 0 10.06 2.36 10 -6 0 11.10 1.50 -10 -6 0 8.76 1.06 10 6 0 8.40 0.83 -10 6 0 12.92 1.43 -15 -1 -6 1.99 0.99 -15 1 -6 2.47 1.07 -15 -1 -6 4.58 2.97 -13 4 7 13.67 1.71 13 -4 -7 13.59 1.86 13 -4 -7 11.19 2.77 -13 4 7 14.19 1.36 13 4 -7 19.62 4.29 -6 3 -9 2.98 0.96 -6 3 -9 5.61 1.02 6 3 9 2.51 1.32 -6 -3 -9 4.33 1.13 10 6 -2 5.66 1.37 -10 -6 2 5.88 1.45 10 -6 -2 5.43 1.42 -10 6 2 7.02 1.33 10 -6 -2 5.26 1.25 -10 6 2 7.10 1.31 -2 0 -11 0.05 1.16 -2 0 -11 0.74 1.24 8 -1 -11 33.85 2.35 -8 1 11 29.88 2.08 8 1 -11 27.45 2.27 -8 1 11 35.31 1.98 8 -1 -11 30.81 2.45 8 1 -11 34.44 2.13 -19 0 6 12.08 1.48 19 0 -6 8.71 2.38 -17 2 7 7.27 1.43 17 -2 -7 6.32 0.75 17 2 -7 7.43 1.49 17 2 -7 5.62 2.52 17 -2 -7 6.80 1.59 -19 -1 -2 3.32 1.14 -19 1 -2 3.27 0.89 -19 1 -2 4.06 2.56 18 2 -6 12.09 2.47 18 -2 -6 8.11 0.86 18 -2 -6 9.52 1.75 -18 2 6 11.04 1.55 18 2 -6 12.21 1.61 -6 4 -8 0.50 0.81 -6 -4 -8 1.36 0.91 6 4 8 0.23 1.08 -6 4 -8 1.98 0.79 -11 4 8 -0.70 0.86 11 -4 -8 -0.11 0.67 11 4 -8 0.10 1.41 11 4 -8 0.32 1.45 11 -4 -8 0.48 0.91 11 2 -10 24.52 2.78 11 -2 -10 20.82 1.42 -11 2 10 20.46 1.84 11 2 -10 17.76 2.77 11 -2 -10 22.56 2.02 -18 3 4 57.03 3.76 -18 3 4 54.84 3.05 18 -3 -4 51.37 4.90 18 3 -4 58.79 3.76 18 -3 -4 52.63 2.97 -12 -5 -3 -0.50 1.06 -12 5 -3 0.74 0.89 12 5 3 0.31 0.97 -12 -5 -3 0.27 0.53 12 -5 3 0.95 0.92 -12 5 -3 -0.03 0.56 12 -5 3 0.20 0.86 12 5 3 -0.13 0.61 -6 -6 -4 7.07 1.22 -6 -6 -4 5.80 1.56 6 6 4 7.16 1.14 6 -6 4 6.10 1.06 -6 6 -4 8.58 1.18 6 6 4 6.68 1.11 6 -6 4 6.09 1.72 -6 6 -4 6.85 1.70 -9 3 -8 14.15 2.87 -9 -3 -8 8.88 1.33 11 -5 -6 1.97 0.89 -11 5 6 1.14 1.14 11 5 -6 0.94 1.13 11 5 -6 2.44 1.12 11 -5 -6 1.24 1.20 9 0 -11 0.10 0.35 9 0 -11 -1.27 0.71 9 0 -11 -0.60 1.06 9 0 -11 0.27 0.32 -14 3 8 7.57 1.51 -14 3 8 7.28 0.93 14 3 -8 13.40 3.51 14 -3 -8 9.15 1.56 14 -3 -8 8.01 1.37 14 5 0 0.80 0.88 -14 5 0 1.17 0.85 14 5 0 1.60 0.86 -14 5 0 1.51 1.03 14 -5 0 1.87 0.89 14 -5 0 1.47 1.00 13 0 -10 -0.62 0.90 -20 1 0 0.66 0.60 20 1 0 0.59 0.55 20 1 0 -0.01 0.89 -20 -1 0 -0.01 0.45 -20 1 0 0.43 0.53 -20 -1 0 -0.12 0.68 20 -1 0 0.40 0.58 -12 0 -8 26.10 2.34 -12 0 -8 32.53 3.61 -13 3 -6 8.95 1.42 -13 -3 -6 5.64 1.14 -13 -3 -6 6.26 1.12 15 1 -9 4.85 1.94 15 -1 -9 2.06 1.19 -15 1 9 3.08 1.13 15 1 -9 4.53 1.93 -17 0 8 17.22 1.83 13 -5 2 3.60 1.12 13 5 2 3.82 1.33 -13 -5 -2 2.77 0.63 -13 5 -2 4.11 0.82 13 5 2 2.43 0.84 -13 5 -2 4.45 1.18 9 6 2 0.80 0.84 -9 -6 -2 0.28 0.93 9 -6 2 -0.05 0.91 -9 6 -2 1.47 0.92 9 6 2 0.21 0.96 -9 6 -2 1.05 1.25 -9 -6 -2 0.33 0.89 3 -2 -11 0.17 0.72 -3 2 11 0.05 0.45 3 2 -11 8.90 1.28 3 -2 -11 0.70 0.73 2 4 9 23.72 3.03 -2 4 -9 20.40 1.42 -2 -4 -9 19.98 1.91 -2 4 -9 18.10 1.40 2 4 9 12.01 1.09 -2 4 -9 14.20 1.08 -2 4 -9 15.52 1.07 -19 2 -1 1.73 1.23 -19 -2 -1 0.66 0.47 -19 -2 -1 1.14 0.78 19 2 1 -0.01 0.84 -19 2 -1 0.82 0.79 19 -2 1 0.08 0.71 -4 2 11 22.22 1.77 4 -2 -11 20.25 1.64 4 2 -11 29.30 2.63 20 -1 -4 1.65 0.68 -20 1 4 1.73 1.47 -5 -2 -10 12.26 2.17 -5 2 -10 8.30 1.87 -5 -2 -10 9.08 2.20 14 -5 -3 3.28 1.98 14 5 -3 4.91 1.25 -9 5 7 -0.74 1.48 9 -5 -7 1.15 1.55 9 -5 -7 -0.45 0.80 -9 5 7 0.29 0.85 9 5 -7 0.44 0.91 2 -5 -8 24.66 2.80 -2 5 8 22.11 1.79 2 5 -8 23.82 2.22 3 5 -8 14.38 1.56 -3 5 8 7.94 1.37 -3 5 8 5.43 1.64 3 -5 -8 6.35 1.22 -8 3 10 3.13 0.85 8 3 -10 -0.63 1.38 -8 3 10 1.33 0.90 8 3 -10 -0.07 1.37 -14 2 9 25.12 2.10 14 2 -9 27.31 3.33 14 -2 -9 19.71 1.35 -14 2 9 19.75 1.35 11 -5 4 25.55 2.13 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 20241 _shelx_res_file ; TITL 180625kmgBphSO3Li-3RT shelxl.res created by SHELXL-2018/3 at 13:42:04 on 24-Nov-2023 CELL 0.71075 15.85840 5.36929 8.86361 90.00000 99.99380 90.00000 ZERR 2 0.00105 0.00041 0.00061 0.00000 0.00700 0.00000 LATT 1 SYMM -X, .50+Y, .50-Z SFAC C H LI O S UNIT 24 24 4 16 4 L.S. 20 FMAP 2 PLAN 52 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP 13.0 ACTA SIZE 0.500 0.400 0.200 DFIX 0.9000 0.0200 H1 O4 DFIX 0.9000 0.0200 H4 O4 DANG 1.4346 0.0400 H1 H4 WGHT 0.094800 0.364200 FVAR 0.67033 S1 5 0.678459 0.563702 0.594475 11.00000 0.03330 0.03448 = 0.03585 -0.00162 0.00929 0.00429 O1 4 0.666810 0.823757 0.629529 11.00000 0.06407 0.03592 = 0.07239 0.00000 0.03241 0.01162 O2 4 0.624157 0.488683 0.453225 11.00000 0.03767 0.09048 = 0.04128 -0.01149 0.00569 0.00076 O3 4 0.670410 0.401203 0.721470 11.00000 0.04808 0.04044 = 0.04847 0.00501 0.01311 -0.00007 O4 4 0.497483 1.092061 0.657892 11.00000 0.03960 0.06905 = 0.06663 0.01603 0.00725 0.00477 C1 1 0.785509 0.538379 0.564844 11.00000 0.03344 0.03161 = 0.03860 -0.00363 0.00600 0.00222 C2 1 0.817146 0.714309 0.475584 11.00000 0.03521 0.05807 = 0.07732 0.03216 0.01197 0.01117 C3 1 0.900752 0.696384 0.449945 11.00000 0.03556 0.06301 = 0.07905 0.03546 0.01373 0.00766 C4 1 0.954842 0.507528 0.513729 11.00000 0.03022 0.03367 = 0.04143 -0.00331 0.00418 0.00071 C5 1 0.922112 0.334919 0.604627 11.00000 0.04790 0.04653 = 0.10014 0.03006 0.02981 0.01863 C6 1 0.838141 0.348861 0.629671 11.00000 0.04888 0.04602 = 0.09501 0.03005 0.03332 0.01488 LI1 3 0.619452 1.077729 0.738834 11.00000 0.04071 0.04084 = 0.04340 0.00365 0.01062 0.00291 H1 2 0.464143 0.986367 0.695996 11.00000 0.13033 H2 2 0.777743 0.873618 0.441108 11.00000 0.08295 H3 2 0.915903 0.788945 0.374586 11.00000 0.09940 H4 2 0.462007 1.197024 0.599629 11.00000 0.12124 H5 2 0.954465 0.195852 0.643743 11.00000 0.07804 H6 2 0.822805 0.262277 0.695175 11.00000 0.09616 HKLF 4 REM 180625kmgBphSO3Li-3RT REM wR2 = 0.1593, GooF = S = 1.122, Restrained GooF = 1.121 for all data REM R1 = 0.0606 for 1490 Fo > 4sig(Fo) and 0.0683 for all 1666 data REM 133 parameters refined using 3 restraints END WGHT 0.0948 0.3642 REM Instructions for potential hydrogen bonds EQIV $6 -x+1, y+1/2, -z+3/2 HTAB O4 O3_$6 EQIV $7 -x+1, y-1/2, -z+3/2 HTAB O4 O4_$7 EQIV $5 x, -y+3/2, z-1/2 HTAB C2 O3_$5 EQIV $8 -x+1, -y+2, -z+1 HTAB O4 S1_$8 HTAB O4 O1_$8 HTAB O4 O2_$8 REM Highest difference peak 0.741, deepest hole -0.281, 1-sigma level 0.130 Q1 1 0.6440 0.5297 0.5138 11.00000 0.05 0.74 Q2 1 0.6815 0.4628 0.6552 11.00000 0.05 0.66 Q3 1 0.7236 0.5409 0.5592 11.00000 0.05 0.47 Q4 1 1.0000 0.5000 0.5000 10.50000 0.05 0.47 Q5 1 0.6570 0.6824 0.6299 11.00000 0.05 0.47 Q6 1 0.9488 0.4309 0.5974 11.00000 0.05 0.45 Q7 1 0.9431 0.4264 0.5479 11.00000 0.05 0.43 Q8 1 0.9146 0.5606 0.4497 11.00000 0.05 0.43 Q9 1 0.9344 0.6549 0.5270 11.00000 0.05 0.40 Q10 1 0.8001 0.4334 0.5685 11.00000 0.05 0.39 Q11 1 0.7846 0.5770 0.4875 11.00000 0.05 0.37 Q12 1 0.9083 0.3489 0.5263 11.00000 0.05 0.36 Q13 1 0.6949 0.7439 0.5911 11.00000 0.05 0.32 Q14 1 0.8647 0.7122 0.4797 11.00000 0.05 0.32 Q15 1 0.4990 0.9620 0.6486 11.00000 0.05 0.31 Q16 1 0.8239 0.6812 0.5509 11.00000 0.05 0.31 Q17 1 0.8836 0.3534 0.6312 11.00000 0.05 0.31 Q18 1 0.7011 0.3346 0.7355 11.00000 0.05 0.30 Q19 1 0.4856 1.0297 0.5569 11.00000 0.05 0.25 Q20 1 0.9745 0.2867 0.7158 11.00000 0.05 0.23 Q21 1 1.0000 0.0000 0.5000 10.50000 0.05 0.21 Q22 1 0.6204 0.8019 0.6856 11.00000 0.05 0.21 Q23 1 0.5562 1.0382 0.7434 11.00000 0.05 0.21 Q24 1 0.5980 0.7924 0.6462 11.00000 0.05 0.17 Q25 1 0.7644 0.7445 0.3911 11.00000 0.05 0.16 Q26 1 0.9202 0.8419 0.4198 11.00000 0.05 0.16 Q27 1 0.8161 0.2086 0.6461 11.00000 0.05 0.15 Q28 1 0.4618 1.0597 0.6862 11.00000 0.05 0.15 Q29 1 0.7219 0.1849 0.7808 11.00000 0.05 0.14 Q30 1 0.7593 0.5270 0.7636 11.00000 0.05 0.14 Q31 1 0.9772 0.7554 0.5813 11.00000 0.05 0.13 Q32 1 0.7394 1.1067 0.8563 11.00000 0.05 0.11 Q33 1 0.6803 0.5290 0.8218 11.00000 0.05 0.10 Q34 1 0.9056 0.3681 0.4283 11.00000 0.05 0.09 Q35 1 0.5971 0.9613 0.6038 11.00000 0.05 0.09 Q36 1 0.9406 0.1881 0.5808 11.00000 0.05 0.09 Q37 1 0.7583 0.9885 0.5624 11.00000 0.05 0.09 Q38 1 0.7570 0.4847 0.3674 11.00000 0.05 0.08 Q39 1 0.9666 0.5228 0.3264 11.00000 0.05 0.08 Q40 1 0.7239 0.9672 0.7162 11.00000 0.05 0.08 Q41 1 0.9750 0.1716 0.5515 11.00000 0.05 0.07 Q42 1 0.9256 0.5380 0.7011 11.00000 0.05 0.05 Q43 1 0.9450 0.7554 0.2392 11.00000 0.05 0.05 Q44 1 0.5766 1.1719 0.5609 11.00000 0.05 0.05 Q45 1 0.8560 0.2498 0.7604 11.00000 0.05 0.05 Q46 1 0.8741 0.8596 0.2489 11.00000 0.05 0.05 Q47 1 1.0125 0.0656 0.7004 11.00000 0.05 0.05 Q48 1 0.8646 0.5663 0.7334 11.00000 0.05 0.04 Q49 1 0.7526 0.9433 0.6463 11.00000 0.05 0.03 Q50 1 0.8660 0.5364 0.3359 11.00000 0.05 0.03 Q51 1 0.8665 0.1732 0.8165 11.00000 0.05 0.03 Q52 1 0.8786 0.4833 0.3518 11.00000 0.05 0.02 ; _shelx_res_checksum 18681 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-1/2-Y,-1/2+Z loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S S1 0.67846(4) 0.56370(10) 0.59448(6) 0.0341(3) Uani d 1 . . O O1 0.66681(15) 0.8238(3) 0.6295(3) 0.0550(6) Uani d 1 . . O O2 0.62416(15) 0.4887(5) 0.4532(2) 0.0566(6) Uani d 1 . . O O3 0.67041(13) 0.4012(4) 0.7215(2) 0.0451(5) Uani d 1 . . O O4 0.49748(14) 1.0921(5) 0.6579(3) 0.0587(6) Uani d 1 . . C C1 0.78551(17) 0.5384(4) 0.5648(3) 0.0346(5) Uani d 1 . . C C2 0.81715(19) 0.7143(6) 0.4756(4) 0.0566(8) Uani d 1 . . C C3 0.90075(19) 0.6964(6) 0.4499(4) 0.0588(9) Uani d 1 . . C C4 0.95484(15) 0.5075(4) 0.5137(3) 0.0354(5) Uani d 1 . . C C5 0.9221(2) 0.3349(6) 0.6046(5) 0.0628(9) Uani d 1 . . C C6 0.8381(2) 0.3489(6) 0.6297(5) 0.0608(9) Uani d 1 . . Li Li1 0.6195(3) 1.0777(8) 0.7388(5) 0.0413(9) Uani d 1 . . H H1 0.464(3) 0.986(9) 0.696(7) 0.13(2) Uiso d 1 . . H H2 0.778(3) 0.874(10) 0.441(5) 0.083(13) Uiso d 1 . . H H3 0.916(3) 0.789(10) 0.375(6) 0.099(16) Uiso d 1 . . H H4 0.462(3) 1.197(9) 0.600(6) 0.12(2) Uiso d 1 . . H H5 0.954(3) 0.196(9) 0.644(5) 0.078(13) Uiso d 1 . . H H6 0.823(3) 0.262(9) 0.695(6) 0.096(16) Uiso d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 0.0333(4) 0.0345(4) 0.0359(4) 0.0043(2) 0.0093(2) -0.0016(2) O1 0.0641(13) 0.0359(11) 0.0724(13) 0.0116(9) 0.0324(11) 0.0000(9) O2 0.0377(11) 0.0905(17) 0.0413(10) 0.0008(10) 0.0057(9) -0.0115(10) O3 0.0481(11) 0.0404(9) 0.0485(10) -0.0001(8) 0.0131(8) 0.0050(8) O4 0.0396(12) 0.0691(14) 0.0666(14) 0.0048(10) 0.0073(10) 0.0160(11) C1 0.0334(12) 0.0316(11) 0.0386(11) 0.0022(8) 0.0060(9) -0.0036(8) C2 0.0352(13) 0.0581(17) 0.077(2) 0.0112(12) 0.0120(13) 0.0322(15) C3 0.0356(14) 0.0630(19) 0.079(2) 0.0077(12) 0.0137(14) 0.0355(16) C4 0.0302(13) 0.0337(11) 0.0414(12) 0.0007(8) 0.0042(10) -0.0033(9) C5 0.0479(17) 0.0465(15) 0.100(3) 0.0186(13) 0.0298(17) 0.0301(17) C6 0.0489(16) 0.0460(15) 0.095(2) 0.0149(13) 0.0333(17) 0.0300(17) Li1 0.041(2) 0.041(2) 0.043(2) 0.0029(17) 0.0106(18) 0.0036(16) 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 for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; Li Li -0.0003 0.0001 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.1246 0.1234 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 S1 O2 . . 112.66(14) ? O3 S1 O1 . . 112.48(12) ? O2 S1 O1 . . 112.00(15) ? O3 S1 C1 . . 106.61(11) ? O2 S1 C1 . . 107.01(12) ? O1 S1 C1 . . 105.51(12) ? S1 O1 Li1 . . 151.24(19) ? S1 O2 Li1 . 4_575 145.2(2) ? S1 O3 Li1 . 1_545 134.28(19) ? Li1 O4 H1 . . 117(4) ? Li1 O4 H4 . . 136(4) ? H1 O4 H4 . . 106(4) ? C6 C1 C2 . . 119.4(3) ? C6 C1 S1 . . 121.5(2) ? C2 C1 S1 . . 119.09(19) ? C1 C2 C3 . . 119.9(3) ? C1 C2 H2 . . 117(2) ? C3 C2 H2 . . 122(2) ? C4 C3 C2 . . 121.8(3) ? C4 C3 H3 . . 119(3) ? C2 C3 H3 . . 118(3) ? C3 C4 C5 . . 117.3(2) ? C3 C4 C4 . 3_766 121.1(3) ? C5 C4 C4 . 3_766 121.6(3) ? C4 C5 C6 . . 121.5(3) ? C4 C5 H5 . . 121(3) ? C6 C5 H5 . . 118(3) ? C1 C6 C5 . . 120.1(3) ? C1 C6 H6 . . 119(4) ? C5 C6 H6 . . 120(4) ? O1 Li1 O2 . 4_576 114.8(2) ? O1 Li1 O3 . 1_565 113.3(2) ? O2 Li1 O3 4_576 1_565 107.5(2) ? O1 Li1 O4 . . 107.2(3) ? O2 Li1 O4 4_576 . 103.7(2) ? O3 Li1 O4 1_565 . 109.8(2) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 O3 . 1.4472(19) ? S1 O2 . 1.448(2) ? S1 O1 . 1.4492(19) ? S1 C1 . 1.768(3) ? O1 Li1 . 1.901(5) ? O2 Li1 4_575 1.922(5) ? O3 Li1 1_545 1.933(5) ? O4 Li1 . 1.944(5) ? O4 H1 . 0.88(2) ? O4 H4 . 0.89(2) ? C1 C6 . 1.377(4) ? C1 C2 . 1.381(4) ? C2 C3 . 1.387(4) ? C2 H2 . 1.07(5) ? C3 C4 . 1.384(4) ? C3 H3 . 0.90(5) ? C4 C5 . 1.387(4) ? C4 C4 3_766 1.496(5) ? C5 C6 . 1.390(4) ? C5 H5 . 0.94(5) ? C6 H6 . 0.81(5) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O4 H4 O2 . . 3_676 0.89(5) 2.17(5) 3.016(3) 157(5) y O4 H1 O3 . . 2_656 2.41(5) 3.205(3) 0.89(5) 149(4) y O4 H1 O4 . . 2_646 2.50(5) 3.136(4) 0.89(5) 129(4) y 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O3 S1 O1 Li1 . . . . -27.3(5) ? O2 S1 O1 Li1 . . . . 100.8(5) ? C1 S1 O1 Li1 . . . . -143.1(4) ? O3 S1 O2 Li1 . . . 4_575 -131.3(4) ? O1 S1 O2 Li1 . . . 4_575 100.7(4) ? C1 S1 O2 Li1 . . . 4_575 -14.4(4) ? O2 S1 O3 Li1 . . . 1_545 12.8(3) ? O1 S1 O3 Li1 . . . 1_545 140.6(3) ? C1 S1 O3 Li1 . . . 1_545 -104.2(3) ? O3 S1 C1 C6 . . . . 14.5(3) ? O2 S1 C1 C6 . . . . -106.3(3) ? O1 S1 C1 C6 . . . . 134.3(3) ? O3 S1 C1 C2 . . . . -165.0(2) ? O2 S1 C1 C2 . . . . 74.3(3) ? O1 S1 C1 C2 . . . . -45.2(3) ? C6 C1 C2 C3 . . . . 1.1(5) ? S1 C1 C2 C3 . . . . -179.5(3) ? C1 C2 C3 C4 . . . . -1.1(6) ? C2 C3 C4 C5 . . . . 0.2(5) ? C2 C3 C4 C4 . . . 3_766 -179.3(3) ? C3 C4 C5 C6 . . . . 0.6(6) ? C4 C4 C5 C6 3_766 . . . -179.8(4) ? C2 C1 C6 C5 . . . . -0.3(6) ? S1 C1 C6 C5 . . . . -179.7(3) ? C4 C5 C6 C1 . . . . -0.6(6) ?