#------------------------------------------------------------------------------ #$Date: 2024-05-06 07:20:18 +0300 (Mon, 06 May 2024) $ #$Revision: 291720 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/30/2023067.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_2023067 loop_ _publ_author_name 'Bieler, Irén' 'Wagner, Christoph' 'Merzweiler, Kurt' _publ_section_title ; Lithium and sodium 3-(3,4-di-hydroxy-phen-yl)propenoate hydrate. ; _journal_issue 'Pt 4' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 401 _journal_page_last 407 _journal_paper_doi 10.1107/S2056989024002494 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac '[Li (C9 H7 O4) (H2 O)]' _chemical_formula_moiety 'C9 H9 Li O5' _chemical_formula_sum 'C9 H9 Li O5' _chemical_formula_weight 204.10 _chemical_name_systematic ; Poly[aqua[\m-3-(3,4-dihydroxyphenyl)propenoato]lithium] ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _cell_angle_alpha 90 _cell_angle_beta 98.572(18) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.3083(12) _cell_length_b 4.8511(5) _cell_length_c 22.587(4) _cell_measurement_reflns_used 3964 _cell_measurement_temperature 220 _cell_measurement_theta_max 25.95 _cell_measurement_theta_min 2.45 _cell_volume 900.2(2) _computing_cell_refinement ; X-AREA (Stoe & Cie, 2016) ; _computing_data_collection ; X-AREA (Stoe & Cie, 2016) ; _computing_data_reduction ; X-AREA (Stoe & Cie, 2016) ; _computing_molecular_graphics ; DIAMOND (Brandenburg & Putz, 2019) ; _computing_publication_material ; Olex2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 220 _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_area_resol_mean 6.67 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_device '2-circle diffractometer' _diffrn_measurement_device_type 'Stoe IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_unetI/netI 0.0292 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 4973 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.109 _diffrn_reflns_theta_min 2.511 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _exptl_absorpt_coefficient_mu 0.122 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 424 _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.188 _refine_diff_density_min -0.146 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 152 _refine_ls_number_reflns 1735 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.007 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0317 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.0259P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.0791 _reflns_number_gt 1314 _reflns_number_total 1735 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5710.cif _cod_data_source_block 1 _cod_depositor_comments 'Adding full bibliography for 2023067--2023068.cif.' _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2023067 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.946 _shelx_estimated_absorpt_t_max 0.982 _shelx_hkl_file ; -4 -1 -12 146.73 8.86 2 0.47906-0.88146-0.33792 0.18969-0.73358 0.30112 -4 0 -23 4.07 10.16 2 0.47906-0.93766-0.33792 0.33702-0.73358-0.04906 -4 0 -22 88.50 10.99 2 0.47906-0.93337-0.33792 0.33934-0.73358-0.01716 -4 0 -21 -1.11 9.16 2 0.47906-0.92952-0.33792 0.33721-0.73358 0.01518 -4 0 -20 20.72 9.29 2 0.47906-0.92344-0.33792 0.33840-0.73358 0.04725 -4 0 -19 0.14 9.57 2 0.47906-0.91722-0.33792 0.33756-0.73358 0.07833 -4 0 -18 42.77 8.30 2 0.47906-0.90965-0.33792 0.33713-0.73358 0.11013 -4 0 -17 -0.77 8.09 2 0.47906-0.90142-0.33792 0.33513-0.73358 0.14237 -3 0 -9 525.60 10.98 2 0.47906-0.78041-0.33792 0.33714-0.73358 0.40949 -3 1 -16 97.65 9.38 2 0.47906-0.81769-0.33792 0.48632-0.73358 0.18870 -3 1 -15 104.12 7.90 2 0.47906-0.80799-0.33792 0.48319-0.73358 0.21888 -2 0 -5 2.03 9.55 2 0.47906-0.67711-0.33792 0.33783-0.73358 0.55022 -2 1 -9 986.33 13.29 2 0.47906-0.69604-0.33792 0.48577-0.73358 0.42447 -2 2 -24 20.77 11.79 2 0.47906-0.77072-0.33792 0.63511-0.73358-0.05499 -2 2 -23 -1.02 10.72 2 0.47906-0.76666-0.33792 0.63642-0.73358-0.02247 -2 2 -22 18.56 11.02 2 0.47906-0.76225-0.33792 0.63656-0.73358 0.00968 -2 2 -21 16.59 9.37 2 0.47906-0.75754-0.33792 0.63545-0.73358 0.04182 -2 2 -20 309.89 11.02 2 0.47906-0.75066-0.33792 0.63499-0.73358 0.07527 -2 2 -19 7.96 8.17 2 0.47906-0.74452-0.33792 0.63290-0.73358 0.10567 -2 2 -18 4.54 8.17 2 0.47906-0.73686-0.33792 0.63093-0.73358 0.13670 -2 2 -17 18.98 8.31 2 0.47906-0.72836-0.33792 0.62830-0.73358 0.16808 -1 2 -11 174.21 9.43 2 0.47906-0.61882-0.33792 0.63262-0.73358 0.37392 0 -5 -1 34.31 9.74 2 0.47906-0.48366-0.33792-0.39657-0.73358 0.70031 0 3 -17 29.83 8.34 2 0.47906-0.56116-0.33792 0.78061-0.73358 0.19471 0 3 -16 38.70 8.47 2 0.47906-0.55208-0.33792 0.77598-0.73358 0.22545 1 -1 3 5991.79 36.70 2 0.47906-0.37731-0.33792 0.19042-0.73358 0.84285 1 2 -5 225.96 10.21 2 0.47906-0.41606-0.33792 0.63143-0.73358 0.58981 1 3 -12 1015.91 13.33 2 0.47906-0.45207-0.33792 0.77906-0.73358 0.36768 2 -5 2 246.73 11.08 2 0.47906-0.29703-0.33792-0.39573-0.73358 0.81521 2 -1 4 8.39 8.66 2 0.47906-0.28711-0.33792 0.19204-0.73358 0.88773 2 3 -9 561.54 11.96 2 0.47906-0.34815-0.33792 0.77585-0.73358 0.47340 3 4 -19 19.80 10.30 2 0.47906-0.30866-0.33792 0.92727-0.73358 0.16910 3 4 -18 135.09 11.59 2 0.47906-0.30231-0.33792 0.92177-0.73358 0.20047 4 -5 3 7.87 10.62 2 0.47906-0.11963-0.33792-0.39782-0.73358 0.88112 4 -4 5 2.75 8.02 2 0.47906-0.10929-0.33792-0.24814-0.73358 0.93557 4 -2 6 446.54 10.29 2 0.47906-0.10268-0.33792 0.04377-0.73358 0.96856 4 0 4 12.59 7.27 2 0.47906-0.11411-0.33792 0.33874-0.73358 0.90889 5 -4 5 -11.60 9.50 2 0.47906-0.02294-0.33792-0.24878-0.73358 0.95377 5 -3 6 18.42 8.51 2 0.47906-0.01923-0.33792-0.10143-0.73358 0.98097 5 -2 6 228.08 8.95 2 0.47906-0.01801-0.33792 0.04470-0.73358 0.98586 5 1 2 935.18 17.13 2 0.47906-0.03694-0.33792 0.48328-0.73358 0.86200 5 4 -14 8.12 10.82 2 0.47906-0.11118-0.33792 0.92271-0.73358 0.35282 6 -4 5 -10.68 10.69 2 0.47906 0.06358-0.33792-0.24794-0.73358 0.96473 6 -3 6 32.18 9.75 2 0.47906 0.06820-0.33792-0.10086-0.73358 0.99157 6 -2 6 550.62 11.60 2 0.47906 0.06896-0.33792 0.04461-0.73358 0.99626 6 0 4 132.76 8.74 2 0.47906 0.05817-0.33792 0.33881-0.73358 0.93889 6 1 2 59.66 8.32 2 0.47906 0.04926-0.33792 0.48500-0.73358 0.87293 7 -4 5 31.54 11.40 2 0.47906 0.14878-0.33792-0.24646-0.73358 0.96816 7 -1 5 537.61 11.75 2 0.47906 0.14933-0.33792 0.19100-0.73358 0.98229 8 -3 5 30.72 10.50 2 0.47906 0.23578-0.33792-0.10155-0.73358 0.99005 8 -2 5 15.50 9.58 2 0.47906 0.23684-0.33792 0.04447-0.73358 0.99476 -4 -2 -10 462.32 14.98 3 0.46900-0.86229-0.32830 0.03338-0.74413 0.37424 -4 -1 -11 649.74 14.83 3 0.46900-0.86330-0.32830 0.18045-0.74413 0.34117 -4 0 -16 436.19 13.76 3 0.46900-0.89034-0.32830 0.32788-0.74413 0.18428 -3 -1 -6 952.10 18.46 3 0.46900-0.75562-0.32830 0.18016-0.74413 0.51357 -3 1 -14 8.52 10.60 3 0.46900-0.79451-0.32830 0.47394-0.74413 0.26195 -2 2 -16 45.02 12.31 3 0.46900-0.71744-0.32830 0.62079-0.74413 0.21107 -1 -4 -1 12.36 10.30 3 0.46900-0.55929-0.32830-0.25845-0.74413 0.69646 -1 0 -2 -3.60 14.76 3 0.46900-0.56475-0.32830 0.32859-0.74413 0.66796 -1 1 -5 131.97 14.99 3 0.46900-0.57947-0.32830 0.47466-0.74413 0.57299 -1 2 -10 96.55 10.34 3 0.46900-0.60111-0.32830 0.62017-0.74413 0.41376 0 -4 1 2.46 10.27 3 0.46900-0.46248-0.32830-0.25748-0.74413 0.77072 0 -3 2 1984.39 20.36 3 0.46900-0.45887-0.32830-0.11277-0.74413 0.80442 0 2 -7 951.62 15.81 3 0.46900-0.50191-0.32830 0.62251-0.74413 0.52358 0 3 -15 7.34 11.98 3 0.46900-0.53940-0.32830 0.76708-0.74413 0.26849 1 3 -11 483.91 13.54 3 0.46900-0.43494-0.32830 0.76622-0.74413 0.40792 3 -4 4 721.35 15.09 3 0.46900-0.19109-0.32830-0.25874-0.74413 0.90773 3 -3 5 22.55 11.12 3 0.46900-0.18565-0.32830-0.11125-0.74413 0.93827 3 3 -7 11.82 11.27 3 0.46900-0.24127-0.32830 0.76463-0.74413 0.55931 3 4 -17 72.11 15.77 3 0.46900-0.28943-0.32830 0.91383-0.74413 0.24370 4 -1 5 507.72 12.34 3 0.46900-0.09874-0.32830 0.18205-0.74413 0.95420 4 4 -15 175.60 16.58 3 0.46900-0.19467-0.32830 0.91665-0.74413 0.32095 5 0 4 3.11 10.66 3 0.46900-0.01764-0.32830 0.32797-0.74413 0.93321 6 -1 5 15.36 10.64 3 0.46900 0.07345-0.32830 0.18274-0.74413 0.98139 6 4 -13 13.14 15.37 3 0.46900-0.01097-0.32830 0.91199-0.74413 0.40793 8 0 3 4.05 11.50 3 0.46900 0.23642-0.32830 0.32875-0.74413 0.94041 8 1 1 237.31 13.87 3 0.46900 0.22670-0.32830 0.47285-0.74413 0.87739 8 2 -2 7.99 13.39 3 0.46900 0.21316-0.32830 0.61970-0.74413 0.78091 9 1 0 46.72 13.66 3 0.46900 0.31047-0.32830 0.47626-0.74413 0.86111 9 2 -3 329.86 18.86 3 0.46900 0.29402-0.32830 0.62032-0.74413 0.76481 -4 0 -15 -3.28 8.69 3 0.45886-0.87817-0.31865 0.31700-0.75448 0.22713 -4 0 -14 402.10 9.93 3 0.45886-0.86765-0.31865 0.31439-0.75448 0.25525 -3 0 -8 -1.11 7.05 3 0.45886-0.75450-0.31865 0.31669-0.75448 0.45935 -3 1 -13 11.13 7.76 3 0.45886-0.77954-0.31865 0.46424-0.75448 0.30389 -2 1 -8 3105.48 21.31 3 0.45886-0.67021-0.31865 0.46583-0.75448 0.47538 -2 2 -15 386.30 9.68 3 0.45886-0.70517-0.31865 0.61238-0.75448 0.25324 -2 2 -14 11.89 7.38 3 0.45886-0.69388-0.31865 0.60792-0.75448 0.28310 -1 -3 0 0.62 6.56 3 0.45886-0.54592-0.31865-0.12112-0.75448 0.73923 -1 3 -23 73.09 12.27 3 0.45886-0.65017-0.31865 0.75308-0.75448 0.01007 -1 3 -22 1.94 10.77 3 0.45886-0.64566-0.31865 0.75181-0.75448 0.04274 -1 3 -21 -16.26 11.03 3 0.45886-0.63954-0.31865 0.75075-0.75448 0.07455 0 -2 2 1495.92 19.09 3 0.45886-0.44874-0.31865 0.02422-0.75448 0.81781 0 3 -14 109.93 9.27 3 0.45886-0.52561-0.31865 0.75730-0.75448 0.31006 1 -5 0 6.42 9.34 3 0.45886-0.37174-0.31865-0.41499-0.75448 0.76482 1 -4 2 -5.90 7.34 3 0.45886-0.36242-0.31865-0.26819-0.75448 0.82839 1 -3 3 6.52 6.49 3 0.45886-0.35970-0.31865-0.12164-0.75448 0.86163 2 -5 1 56.20 9.77 3 0.45886-0.28131-0.31865-0.41608-0.75448 0.81206 2 -4 3 43.44 8.72 3 0.45886-0.27120-0.31865-0.26772-0.75448 0.87341 2 -3 4 213.19 9.45 3 0.45886-0.26680-0.31865-0.12146-0.75448 0.90592 2 4 -20 59.02 12.47 3 0.45886-0.37974-0.31865 0.90353-0.75448 0.14557 2 4 -19 175.70 11.89 3 0.45886-0.37264-0.31865 0.89958-0.75448 0.17538 3 -5 2 189.96 10.36 3 0.45886-0.19042-0.31865-0.41484-0.75448 0.85020 3 -2 5 28.91 6.63 3 0.45886-0.17593-0.31865 0.02558-0.75448 0.94764 3 4 -16 92.99 10.00 3 0.45886-0.27556-0.31865 0.90438-0.75448 0.28624 4 -4 4 23.66 8.04 3 0.45886-0.09510-0.31865-0.26875-0.75448 0.93290 4 -3 5 76.75 8.21 3 0.45886-0.08950-0.31865-0.12123-0.75448 0.96414 4 4 -14 41.64 10.00 3 0.45886-0.17949-0.31865 0.90386-0.75448 0.36201 5 -3 5 553.87 11.34 3 0.45886-0.00394-0.31865-0.12043-0.75448 0.98081 5 -1 5 265.33 9.93 3 0.45886-0.00265-0.31865 0.17157-0.75448 0.97484 5 4 -13 56.19 11.81 3 0.45886-0.08735-0.31865 0.90320-0.75448 0.40696 6 -4 4 -1.94 10.73 3 0.45886 0.07886-0.31865-0.26979-0.75448 0.95965 6 -3 5 8.21 8.05 3 0.45886 0.08355-0.31865-0.12110-0.75448 0.99011 7 -4 4 108.03 12.19 3 0.45886 0.16443-0.31865-0.26683-0.75448 0.96229 7 -2 5 5.68 8.06 3 0.45886 0.16965-0.31865 0.02528-0.75448 0.99952 8 -3 4 38.45 10.36 3 0.45886 0.25262-0.31865-0.12187-0.75448 0.98603 8 -1 4 -2.80 9.47 3 0.45886 0.25070-0.31865 0.17183-0.75448 0.97992 9 -1 3 11.76 11.12 3 0.45886 0.33412-0.31865 0.17236-0.75448 0.96640 9 0 2 2.68 9.14 3 0.45886 0.32745-0.31865 0.31840-0.75448 0.92941 -4 -4 -13 45.88 18.66 3 0.45880-0.86628-0.31823-0.27034-0.75474 0.28753 -3 -2 -5 25.14 12.25 3 0.45880-0.74105-0.31823 0.02394-0.75474 0.55530 -5 -2 -19 176.13 16.23 4 0.44854-0.97057-0.30833 0.01400-0.76502 0.09492 -5 -2 -18 567.40 18.80 4 0.44854-0.96245-0.30833 0.01368-0.76502 0.12647 -4 -3 -10 16.42 11.61 4 0.44854-0.84132-0.30833-0.13296-0.76502 0.39370 -3 1 -12 166.24 12.10 4 0.44854-0.76319-0.30833 0.45317-0.76502 0.34526 -1 -5 -4 95.43 14.20 4 0.44854-0.55543-0.30833-0.42673-0.76502 0.62226 -1 2 -9 2517.49 20.02 4 0.44854-0.57578-0.30833 0.60060-0.76502 0.46656 -1 3 -20 14.22 13.86 4 0.44854-0.63037-0.30833 0.74773-0.76502 0.11712 -1 3 -19 655.88 16.22 4 0.44854-0.62344-0.30833 0.74398-0.76502 0.14954 0 -5 -2 218.23 14.87 4 0.44854-0.46023-0.30833-0.42730-0.76502 0.70007 0 3 -13 -16.81 10.51 4 0.44854-0.50866-0.30833 0.74619-0.76502 0.35321 1 3 -10 284.03 12.91 4 0.44854-0.40968-0.30833 0.74684-0.76502 0.46105 2 -2 4 1703.20 17.94 4 0.44854-0.25691-0.30833 0.01464-0.76502 0.91800 2 2 -3 510.68 17.51 4 0.44854-0.28978-0.30833 0.60103-0.76502 0.69662 2 3 -8 20.96 11.60 4 0.44854-0.31323-0.30833 0.74688-0.76502 0.53727 2 4 -18 2.63 15.80 4 0.44854-0.36037-0.30833 0.89252-0.76502 0.21915 3 0 3 306.41 14.04 4 0.44854-0.17436-0.30833 0.30936-0.76502 0.90026 3 1 1 578.05 20.47 4 0.44854-0.18374-0.30833 0.45544-0.76502 0.83648 3 4 -15 8.05 13.64 4 0.44854-0.26011-0.30833 0.89340-0.76502 0.32789 4 -2 5 0.05 11.31 4 0.44854-0.07921-0.30833 0.01537-0.76502 0.97426 4 3 -6 140.18 12.59 4 0.44854-0.13221-0.30833 0.74768-0.76502 0.62738 4 4 -13 66.18 13.75 4 0.44854-0.16381-0.30833 0.88899-0.76502 0.40265 5 -2 5 88.54 11.15 4 0.44854 0.00757-0.30833 0.01524-0.76502 0.99012 6 -2 5 720.22 15.61 4 0.44854 0.09362-0.30833 0.01547-0.76502 0.99848 7 0 3 316.65 14.05 4 0.44854 0.17162-0.30833 0.30943-0.76502 0.95167 8 -2 4 19.27 13.33 4 0.44854 0.26181-0.30833 0.01504-0.76502 0.99309 -5 -2 -17 47.54 9.68 4 0.43814-0.95001-0.29796 0.00215-0.77534 0.16860 -5 -1 -21 0.63 11.52 4 0.43814-0.97113-0.29796 0.14833-0.77534 0.04219 -5 -1 -20 23.88 10.59 4 0.43814-0.96470-0.29796 0.14883-0.77534 0.07321 -5 -1 -19 28.93 11.03 4 0.43814-0.95717-0.29796 0.14858-0.77534 0.10518 -4 -1 -10 75.83 8.36 4 0.43814-0.83184-0.29796 0.15026-0.77534 0.40631 -4 0 -13 6.73 7.58 4 0.43814-0.84785-0.29796 0.29704-0.77534 0.31055 -4 1 -23 4.36 11.71 4 0.43814-0.88948-0.29796 0.44023-0.77534-0.00784 -4 1 -22 26.31 10.70 4 0.43814-0.88431-0.29796 0.44087-0.77534 0.02365 -4 1 -21 53.65 11.36 4 0.43814-0.87853-0.29796 0.44047-0.77534 0.05525 -4 1 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107.35 12.64 11 0.28764-0.34745-0.15446 0.74419-0.88894 0.50936 1 -5 -5 493.54 16.20 11 0.28764-0.22594-0.15446-0.57716-0.88894 0.73990 2 3 -5 1.21 12.17 11 0.28764-0.13909-0.15446 0.59671-0.88894 0.75923 3 4 -9 208.33 13.69 11 0.28764-0.07311-0.15446 0.74360-0.88894 0.64543 5 -3 0 376.74 12.99 11 0.28764 0.14488-0.15446-0.28612-0.88894 0.95799 5 -2 1 87.71 11.75 11 0.28764 0.14948-0.15446-0.13904-0.88894 0.99018 5 0 1 69.75 10.31 11 0.28764 0.14985-0.15446 0.15531-0.88894 0.98796 5 1 0 17.15 9.97 11 0.28764 0.14423-0.15446 0.30076-0.88894 0.95390 5 4 -9 34.21 13.92 11 0.28764 0.10021-0.15446 0.74213-0.88894 0.67075 7 -1 0 131.67 13.23 11 0.28764 0.31778-0.15446 0.00888-0.88894 0.98604 8 -1 -1 292.08 13.27 11 0.28764 0.40062-0.15446 0.00895-0.88894 0.96740 10 0 -4 -4.99 14.35 11 0.28764 0.55473-0.15446 0.15499-0.88894 0.89404 -6 0 -15 5.07 9.44 11 0.27545-0.86604-0.14298 0.14200-0.89645 0.33917 -6 1 -19 56.09 11.74 11 0.27545-0.88869-0.14298 0.28945-0.89645 0.21318 -6 1 -18 6.68 10.56 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0.40087 0.20202-0.64061-0.97766 0.70696 5 -3 -12 106.58 8.82 26-0.10494 0.47959 0.20202-0.64295-0.97766 0.66209 5 -1 -6 56.73 8.63 26-0.10494 0.50866 0.20202-0.35057-0.97766 0.85420 6 -3 -14 64.10 10.05 26-0.10494 0.55340 0.20202-0.64121-0.97766 0.60878 6 -2 -10 2.46 8.77 26-0.10494 0.57105 0.20202-0.49381-0.97766 0.73447 7 -3 -17 -8.94 11.86 26-0.10494 0.62669 0.20202-0.64352-0.97766 0.52923 7 -2 -13 -3.54 9.69 26-0.10494 0.65205 0.20202-0.49966-0.97766 0.66248 7 -1 -10 69.10 9.18 26-0.10494 0.66316 0.20202-0.35034-0.97766 0.75459 8 -2 -16 3.44 10.58 26-0.10494 0.72394 0.20202-0.50053-0.97766 0.57934 8 1 -10 50.56 9.99 26-0.10494 0.74862 0.20202-0.05733-0.97766 0.76751 9 0 -14 3.83 10.94 26-0.10494 0.81854 0.20202-0.20516-0.97766 0.65550 9 1 -13 17.16 10.82 26-0.10494 0.82159 0.20202-0.05752-0.97766 0.68650 -6 -3 -12 10.61 23.18 25-0.07926-0.49871 0.17937-0.62069-0.98055 0.51920 4 4 -5 35.17 15.15 26-0.10509 0.42687 0.20213 0.38426-0.97768 0.87562 -7 -1 -6 100.08 12.62 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204.42 10.30 78-0.69414 0.46912 0.57787-0.43161 0.31752-0.69148 -1 -1 5 216.57 13.61 78-0.69414 0.63071 0.57787-0.72549 0.31752-0.17110 -1 -1 16 176.32 11.98 78-0.69414 0.68118 0.57787-0.72464 0.31752 0.17878 -1 0 25 71.56 13.45 78-0.69414 0.72634 0.57787-0.57968 0.31752 0.46726 0 0 20 186.74 12.88 78-0.69414 0.78736 0.57787-0.57779 0.31752 0.31878 1 1 20 -7.68 11.67 78-0.69414 0.87606 0.57787-0.43205 0.31752 0.33253 1 2 -5 241.44 12.54 78-0.69414 0.75975 0.57787-0.28505 0.31752-0.46432 1 2 24 42.83 15.14 78-0.69414 0.89721 0.57787-0.28652 0.31752 0.46094 1 3 -7 50.44 12.05 78-0.69414 0.75056 0.57787-0.13974 0.31752-0.52757 1 5 -7 53.90 13.89 78-0.69414 0.75036 0.57787 0.15276 0.31752-0.52679 2 2 17 3.61 11.97 78-0.69414 0.95064 0.57787-0.28545 0.31752 0.24938 2 3 -2 802.41 19.39 78-0.69414 0.86028 0.57787-0.13856 0.31752-0.35753 2 3 20 65.24 15.75 78-0.69414 0.96798 0.57787-0.13908 0.31752 0.34606 2 4 -3 3.42 10.16 78-0.69414 0.85518 0.57787 0.00758 0.31752-0.38696 2 5 -2 165.06 14.84 78-0.69414 0.86027 0.57787 0.15281 0.31752-0.35601 -8 -1 -8 293.63 12.43 78-0.68939-0.04188 0.57151-0.72086 0.33357-0.68974 -8 0 -12 10.67 10.37 78-0.68939-0.05929 0.57151-0.57392 0.33357-0.81606 -7 -1 -8 30.41 8.26 78-0.68939 0.04575 0.57151-0.71959 0.33357-0.67743 -7 0 -12 7.13 9.30 78-0.68939 0.02684 0.57151-0.57417 0.33357-0.80458 -5 -2 24 19.68 10.84 78-0.68939 0.37040 0.57151-0.87148 0.33357 0.36881 -5 0 -11 167.14 8.58 78-0.68939 0.20706 0.57151-0.57504 0.33357-0.75085 -5 1 -14 5.96 8.02 78-0.68939 0.19218 0.57151-0.42814 0.33357-0.84405 -5 2 -16 193.10 10.53 78-0.68939 0.18194 0.57151-0.27917 0.33357-0.90509 -5 3 -17 98.88 11.57 78-0.68939 0.17856 0.57151-0.13470 0.33357-0.93737 -4 -2 21 71.35 9.83 78-0.68939 0.44213 0.57151-0.86714 0.33357 0.28498 -4 2 -15 0.05 8.18 78-0.68939 0.27593 0.57151-0.28291 0.33357-0.86708 -4 3 -16 56.64 9.47 78-0.68939 0.27284 0.57151-0.13638 0.33357-0.90131 -3 -2 9 -0.60 6.50 78-0.68939 0.47140 0.57151-0.86560 0.33357-0.08445 -3 -2 13 109.61 8.64 78-0.68939 0.49205 0.57151-0.86763 0.33357 0.04265 -3 -2 14 77.96 8.14 78-0.68939 0.49467 0.57151-0.86670 0.33357 0.07411 -3 -2 15 4.28 7.44 78-0.68939 0.49814 0.57151-0.86411 0.33357 0.10626 -3 -1 27 98.12 11.69 78-0.68939 0.55654 0.57151-0.72002 0.33357 0.48834 -3 0 -9 541.50 10.93 78-0.68939 0.38602 0.57151-0.57140 0.33357-0.65718 -3 1 -12 178.16 8.91 78-0.68939 0.37565 0.57151-0.42838 0.33357-0.75594 -3 2 -14 71.00 9.16 78-0.68939 0.36717 0.57151-0.28175 0.33357-0.82168 -2 -1 23 13.61 9.38 78-0.68939 0.62660 0.57151-0.72247 0.33357 0.37490 -2 -1 24 17.43 9.35 78-0.68939 0.62383 0.57151-0.71327 0.33357 0.40222 -2 0 -7 -1.71 8.14 78-0.68939 0.48388 0.57151-0.57185 0.33357-0.58111 -2 2 -13 359.48 9.48 78-0.68939 0.45378 0.57151-0.27699 0.33357-0.76970 -2 3 -14 4.18 8.14 78-0.68939 0.45297 0.57151-0.13379 0.33357-0.80445 -1 -1 17 1030.29 12.73 78-0.68939 0.68374 0.57151-0.72029 0.33357 0.19528 -1 -1 18 913.23 12.15 78-0.68939 0.68318 0.57151-0.71587 0.33357 0.22709 -1 0 26 7.26 10.56 78-0.68939 0.72511 0.57151-0.57183 0.33357 0.48200 -1 2 -11 184.70 9.25 78-0.68939 0.55104 0.57151-0.27841 0.33357-0.69548 -1 3 -12 62.23 7.80 78-0.68939 0.55178 0.57151-0.13433 0.33357-0.73209 -1 5 -12 43.37 11.12 78-0.68939 0.55076 0.57151 0.15888 0.33357-0.72987 0 0 21 -1.39 8.41 78-0.68939 0.78783 0.57151-0.57155 0.33357 0.33433 0 1 26 71.10 11.31 78-0.68939 0.81775 0.57151-0.42884 0.33357 0.49650 0 1 27 185.97 13.16 78-0.68939 0.80842 0.57151-0.42030 0.33357 0.52339 0 3 -10 620.04 11.41 78-0.68939 0.64358 0.57151-0.13134 0.33357-0.65012 1 1 21 14.24 8.09 78-0.68939 0.87546 0.57151-0.42563 0.33357 0.34819 1 2 25 92.79 12.03 78-0.68939 0.89409 0.57151-0.27958 0.33357 0.47491 2 2 18 9.47 8.09 78-0.68939 0.95041 0.57151-0.27948 0.33357 0.26582 2 3 21 9.30 10.56 78-0.68939 0.96553 0.57151-0.13319 0.33357 0.36101 -6 -2 -1 138.44 18.13 78-0.69386 0.16825 0.57751-0.87261 0.31749-0.42587 -4 -2 3 12.57 11.63 78-0.68928 0.35642 0.57182-0.86602 0.33373-0.28921 -4 -2 22 31.43 13.21 79-0.68436 0.44206 0.56554-0.86316 0.34976 0.30114 -4 0 -10 12.07 11.17 79-0.68436 0.29105 0.56554-0.56560 0.34976-0.71843 -4 1 -13 90.35 10.83 79-0.68436 0.27766 0.56554-0.41970 0.34976-0.81250 -3 -2 7 476.64 13.56 79-0.68436 0.45535 0.56554-0.85654 0.34976-0.16475 -3 -2 8 190.00 10.95 79-0.68436 0.46142 0.56554-0.86115 0.34976-0.13348 -3 -2 16 56.06 10.63 79-0.68436 0.50005 0.56554-0.86256 0.34976 0.12189 -3 -2 17 484.67 14.19 79-0.68436 0.50347 0.56554-0.85826 0.34976 0.15334 -1 -1 4 1433.68 23.91 79-0.68436 0.61559 0.56554-0.71262 0.34976-0.23527 -1 -1 19 2334.33 19.27 79-0.68436 0.68529 0.56554-0.71146 0.34976 0.24213 -1 0 27 5.95 14.87 79-0.68436 0.72306 0.56554-0.56534 0.34976 0.49577 0 0 22 215.72 12.52 79-0.68436 0.78724 0.56554-0.56641 0.34976 0.35022 0 2 -8 1359.00 16.73 79-0.68436 0.64968 0.56554-0.27159 0.34976-0.60493 0 5 -9 108.26 14.05 79-0.68436 0.64849 0.56554 0.16610 0.34976-0.63995 1 1 22 5.81 13.43 79-0.68436 0.87464 0.56554-0.41979 0.34976 0.36296 1 5 -6 18.56 13.97 79-0.68436 0.74617 0.56554 0.16528 0.34976-0.52883 2 2 19 -6.18 11.41 79-0.68436 0.94991 0.56554-0.27425 0.34976 0.28115 2 3 22 -0.22 16.55 79-0.68436 0.96277 0.56554-0.12729 0.34976 0.37587 2 4 -2 -0.30 10.26 79-0.68436 0.85327 0.56554 0.01981 0.34976-0.38966 2 5 -1 56.37 13.98 79-0.68436 0.85705 0.56554 0.16595 0.34976-0.35746 -9 -1 -7 22.77 10.81 79-0.67920-0.13273 0.55949-0.70885 0.36584-0.70386 -7 1 -14 11.65 10.44 79-0.67920 0.00831 0.55949-0.41308 0.36584-0.89867 -6 -1 -7 3.40 7.12 79-0.67920 0.12682 0.55949-0.70879 0.36584-0.66583 -6 0 -11 -3.15 8.21 79-0.67920 0.10815 0.55949-0.56193 0.36584-0.79384 -5 2 -15 0.76 9.56 79-0.67920 0.17794 0.55949-0.26893 0.36584-0.90930 -5 3 -16 33.13 10.72 79-0.67920 0.17334 0.55949-0.12266 0.36584-0.94064 -4 -2 23 82.51 11.06 79-0.67920 0.44339 0.55949-0.85835 0.36584 0.31726 -4 -2 24 50.96 10.72 79-0.67920 0.44173 0.55949-0.85017 0.36584 0.34560 -3 -2 18 1414.36 15.02 79-0.67920 0.50549 0.55949-0.85594 0.36584 0.16920 -3 -2 19 325.24 10.19 79-0.67920 0.50577 0.55949-0.85166 0.36584 0.20083 -2 -1 25 58.25 11.12 79-0.67920 0.62584 0.55949-0.71104 0.36584 0.40589 -2 1 -10 29.43 6.82 79-0.67920 0.45838 0.55949-0.41293 0.36584-0.70919 -2 2 -12 35.65 7.87 79-0.67920 0.45119 0.55949-0.26718 0.36584-0.77465 -2 3 -13 268.09 9.69 79-0.67920 0.44949 0.55949-0.12214 0.36584-0.80849 -2 5 -13 43.23 11.68 79-0.67920 0.44643 0.55949 0.17066 0.36584-0.80358 -1 -1 20 29.37 8.94 79-0.67920 0.68645 0.55949-0.70755 0.36584 0.25832 -1 0 -4 1.72 9.67 79-0.67920 0.57266 0.55949-0.55927 0.36584-0.50548 -1 1 -8 5524.60 28.24 79-0.67920 0.55339 0.55949-0.41191 0.36584-0.63255 -1 2 -10 107.93 7.42 79-0.67920 0.54912 0.55949-0.26924 0.36584-0.70040 -1 5 -11 264.04 12.16 79-0.67920 0.54498 0.55949 0.17140 0.36584-0.73212 0 0 23 -0.21 9.62 79-0.67920 0.78692 0.55949-0.56051 0.36584 0.36638 0 1 -5 2.34 8.44 79-0.67920 0.65672 0.55949-0.41248 0.36584-0.52532 0 3 -9 702.27 12.22 79-0.67920 0.64123 0.55949-0.12153 0.36584-0.65423 1 0 9 4282.19 26.25 79-0.67920 0.80607 0.55949-0.55843 0.36584-0.06584 1 0 10 0.69 8.06 79-0.67920 0.81183 0.55949-0.55909 0.36584-0.03621 1 0 11 542.56 11.10 79-0.67920 0.81733 0.55949-0.55945 0.36584-0.00273 1 0 12 -3.48 6.93 79-0.67920 0.82137 0.55949-0.55973 0.36584 0.02914 1 0 13 584.23 10.76 79-0.67920 0.82528 0.55949-0.55839 0.36584 0.06094 1 0 14 -3.68 6.69 79-0.67920 0.82831 0.55949-0.55653 0.36584 0.09245 1 1 23 1.80 9.22 79-0.67920 0.87364 0.55949-0.41369 0.36584 0.37808 1 3 -6 573.93 12.49 79-0.67920 0.73959 0.55949-0.12088 0.36584-0.54512 2 2 20 293.28 11.33 79-0.67920 0.94899 0.55949-0.26964 0.36584 0.29660 ; _shelx_hkl_checksum 63391 _shelx_res_file ; TITL TEST STRUCTURE G:\ACDATEN\Z\IPDS4110 ipds4110.res created by SHELXL-2018/3 at 13:17:11 on 10-Oct-2022 CELL 0.71073 8.3083 4.8511 22.5866 90 98.572 90 ZERR 4 0.0012 0.0005 0.0036 0 0.018 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Li O UNIT 36 36 4 20 L.S. 11 PLAN 15 SIZE 0.15 0.15 0.46 TEMP -53.15 CONF MPLA C1 > C9 O1 > O4 FREE C1 Li HTAB BOND MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.047000 0.025900 FVAR 1.34642 C1 1 0.715753 0.187365 0.656532 11.00000 0.02690 0.02188 = 0.02114 0.00028 0.00435 -0.00267 C2 1 0.740350 0.057288 0.599015 11.00000 0.04121 0.02323 = 0.02583 -0.00271 0.00893 -0.00061 AFIX 43 H2 2 0.787147 -0.119367 0.599929 11.00000 -1.20000 AFIX 0 C3 1 0.699066 0.179841 0.546342 11.00000 0.02811 0.03009 = 0.02453 -0.00284 0.00558 -0.00189 AFIX 43 H3A 2 0.647720 0.352195 0.547117 11.00000 -1.20000 AFIX 0 C4 1 0.723809 0.079068 0.487055 11.00000 0.02716 0.02978 = 0.02317 -0.00209 0.00556 -0.00486 C5 1 0.649582 0.221003 0.436184 11.00000 0.02647 0.03266 = 0.02552 -0.00306 0.00681 0.00037 AFIX 43 H5 2 0.579486 0.369071 0.440744 11.00000 -1.20000 AFIX 0 C6 1 0.677399 0.147547 0.379289 11.00000 0.02682 0.03266 = 0.02170 -0.00087 0.00256 -0.00331 C7 1 0.784737 -0.065812 0.372463 11.00000 0.02756 0.03234 = 0.02221 -0.00524 0.00627 -0.00475 C8 1 0.856572 -0.212993 0.422052 11.00000 0.03289 0.02833 = 0.03136 -0.00392 0.00612 0.00298 AFIX 43 H8 2 0.926536 -0.360889 0.417203 11.00000 -1.20000 AFIX 0 C9 1 0.825547 -0.142732 0.478854 11.00000 0.03769 0.03147 = 0.02493 0.00052 0.00335 -0.00217 AFIX 43 H9 2 0.873489 -0.245454 0.512161 11.00000 -1.20000 AFIX 0 LI 3 0.795648 0.663233 0.717987 11.00000 0.03885 0.02290 = 0.02388 -0.00093 0.00755 0.00253 O1 4 0.750139 0.045014 0.703748 11.00000 0.04684 0.02261 = 0.02081 0.00149 0.00875 0.00368 O2 4 0.666706 0.433568 0.656939 11.00000 0.04055 0.02269 = 0.02423 -0.00113 0.00194 0.00469 O3 4 0.607833 0.280558 0.328008 11.00000 0.04204 0.04860 = 0.02198 0.00161 0.00377 0.01316 H3 2 0.524831 0.395258 0.335471 11.00000 0.06020 O4 4 0.816096 -0.114001 0.315142 11.00000 0.04550 0.04186 = 0.02293 -0.00459 0.01060 0.00656 H4 2 0.868596 -0.271168 0.313353 11.00000 0.06793 O5 4 1.033680 0.591463 0.718940 11.00000 0.03779 0.04438 = 0.02608 0.00048 0.00486 0.00600 H5A 2 1.081855 0.739586 0.712191 11.00000 0.09186 H5B 2 1.069628 0.547660 0.752168 11.00000 0.07023 HKLF 4 REM TEST STRUCTURE G:\ACDATEN\Z\IPDS4110 REM wR2 = 0.0791, GooF = S = 1.007, Restrained GooF = 1.007 for all data REM R1 = 0.0317 for 1314 Fo > 4sig(Fo) and 0.0491 for all 1735 data REM 152 parameters refined using 0 restraints END WGHT 0.0470 0.0259 REM Instructions for potential hydrogen bonds EQIV $5 -x+1, -y+1, -z+1 HTAB O3 O2_$5 EQIV $6 -x+2, -y, -z+1 HTAB O4 O5_$6 EQIV $7 -x+2, -y+1, -z+1 HTAB O5 O4_$7 EQIV $8 x+1/2, -y+1/2, z+1/2 HTAB O5 O3_$8 HTAB O5 O4_$8 REM Highest difference peak 0.188, deepest hole -0.146, 1-sigma level 0.038 Q1 1 0.8144 0.0278 0.4892 11.00000 0.05 0.19 Q2 1 0.6673 0.0742 0.5739 11.00000 0.05 0.16 Q3 1 0.7288 0.1368 0.6227 11.00000 0.05 0.16 Q4 1 0.7462 0.0793 0.7345 11.00000 0.05 0.15 Q5 1 0.7713 0.1724 0.5788 11.00000 0.05 0.15 Q6 1 0.7187 0.1679 0.4682 11.00000 0.05 0.14 Q7 1 0.7150 0.2350 0.4126 11.00000 0.05 0.14 Q8 1 0.7387 -0.1129 0.4863 11.00000 0.05 0.14 Q9 1 0.7840 -0.1559 0.3973 11.00000 0.05 0.13 Q10 1 0.6517 0.1068 0.4115 11.00000 0.05 0.13 Q11 1 0.7060 0.0970 0.5106 11.00000 0.05 0.13 Q12 1 0.6422 0.0976 0.4611 11.00000 0.05 0.13 Q13 1 0.9405 -0.2649 0.5183 11.00000 0.05 0.13 Q14 1 0.8003 -0.1415 0.6967 11.00000 0.05 0.13 Q15 1 0.8589 0.0095 0.7055 11.00000 0.05 0.12 ; _shelx_res_checksum 21765 loop_ _space_group_symop_operation_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' 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 C C1 0.71575(16) 0.1874(3) 0.65653(5) 0.0232(3) Uani d 1 . . C C2 0.74035(18) 0.0573(3) 0.59901(6) 0.0297(3) Uani d 1 . . H H2 0.787147 -0.119367 0.599929 0.036 Uiso calc 1 . . C C3 0.69907(16) 0.1798(3) 0.54634(6) 0.0274(3) Uani d 1 . . H H3A 0.647720 0.352195 0.547117 0.033 Uiso calc 1 . . C C4 0.72381(16) 0.0791(3) 0.48705(6) 0.0265(3) Uani d 1 . . C C5 0.64958(16) 0.2210(3) 0.43618(6) 0.0279(3) Uani d 1 . . H H5 0.579486 0.369071 0.440744 0.034 Uiso calc 1 . . C C6 0.67740(16) 0.1475(3) 0.37929(6) 0.0272(3) Uani d 1 . . C C7 0.78474(16) -0.0658(3) 0.37246(6) 0.0271(3) Uani d 1 . . C C8 0.85657(17) -0.2130(3) 0.42205(6) 0.0307(3) Uani d 1 . . H H8 0.926536 -0.360889 0.417203 0.037 Uiso calc 1 . . C C9 0.82555(18) -0.1427(3) 0.47885(6) 0.0315(3) Uani d 1 . . H H9 0.873489 -0.245454 0.512161 0.038 Uiso calc 1 . . Li Li 0.7956(3) 0.6632(5) 0.71799(10) 0.0283(5) Uani d 1 . . O O1 0.75014(12) 0.0450(2) 0.70375(4) 0.0297(3) Uani d 1 . . O O2 0.66671(12) 0.43357(19) 0.65694(4) 0.0294(3) Uani d 1 . . O O3 0.60783(14) 0.2806(2) 0.32801(4) 0.0376(3) Uani d 1 . . H H3 0.525(3) 0.395(4) 0.3355(9) 0.060(6) Uiso d 1 . . O O4 0.81610(14) -0.1140(3) 0.31514(4) 0.0362(3) Uani d 1 . . H H4 0.869(3) -0.271(5) 0.3134(9) 0.068(7) Uiso d 1 . . O O5 1.03368(14) 0.5915(3) 0.71894(5) 0.0361(3) Uani d 1 . . H H5A 1.082(3) 0.740(6) 0.7122(11) 0.092(9) Uiso d 1 . . H H5B 1.070(3) 0.548(5) 0.7522(11) 0.070(7) 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 C1 0.0269(7) 0.0219(7) 0.0211(7) -0.0027(6) 0.0043(5) 0.0003(5) C2 0.0412(8) 0.0232(7) 0.0258(7) -0.0006(6) 0.0089(6) -0.0027(6) C3 0.0281(7) 0.0301(8) 0.0245(7) -0.0019(6) 0.0056(5) -0.0028(6) C4 0.0272(7) 0.0298(8) 0.0232(7) -0.0049(6) 0.0056(5) -0.0021(6) C5 0.0265(7) 0.0327(8) 0.0255(7) 0.0004(6) 0.0068(5) -0.0031(6) C6 0.0268(7) 0.0327(8) 0.0217(7) -0.0033(6) 0.0026(5) -0.0009(5) C7 0.0276(7) 0.0323(8) 0.0222(7) -0.0048(6) 0.0063(5) -0.0052(6) C8 0.0329(8) 0.0283(8) 0.0314(7) 0.0030(7) 0.0061(6) -0.0039(6) C9 0.0377(8) 0.0315(8) 0.0249(7) -0.0022(7) 0.0034(6) 0.0005(6) Li 0.0389(13) 0.0229(11) 0.0239(11) 0.0025(10) 0.0075(9) -0.0009(9) O1 0.0468(6) 0.0226(5) 0.0208(5) 0.0037(4) 0.0087(4) 0.0015(4) O2 0.0406(6) 0.0227(5) 0.0242(5) 0.0047(5) 0.0019(4) -0.0011(4) O3 0.0420(6) 0.0486(7) 0.0220(5) 0.0132(6) 0.0038(4) 0.0016(5) O4 0.0455(6) 0.0419(7) 0.0229(5) 0.0066(6) 0.0106(4) -0.0046(5) O5 0.0378(6) 0.0444(7) 0.0261(6) 0.0060(6) 0.0049(5) 0.0005(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O1 C1 C2 . . 117.48(12) y O2 C1 C2 . . 119.66(12) ? O2 C1 O1 . . 122.83(12) ? C1 C2 H2 . . 118.6 ? C3 C2 C1 . . 122.84(13) ? C3 C2 H2 . . 118.6 ? C2 C3 H3A . . 116.0 ? C2 C3 C4 . . 127.96(14) ? C4 C3 H3A . . 116.0 ? C5 C4 C3 . . 118.68(13) ? C9 C4 C3 . . 123.15(12) ? C9 C4 C5 . . 118.07(12) ? C4 C5 H5 . . 119.3 ? C6 C5 C4 . . 121.35(14) ? C6 C5 H5 . . 119.3 ? C5 C6 C7 . . 119.53(12) ? O3 C6 C5 . . 123.57(13) ? O3 C6 C7 . . 116.87(11) ? C8 C7 C6 . . 120.01(12) ? O4 C7 C6 . . 116.41(12) ? O4 C7 C8 . . 123.56(13) ? C7 C8 H8 . . 119.9 ? C7 C8 C9 . . 120.23(13) ? C9 C8 H8 . . 119.9 ? C4 C9 H9 . . 119.6 ? C8 C9 C4 . . 120.72(13) ? C8 C9 H9 . . 119.6 ? Li Li Li 2_646 2_656 109.00(13) ? O1 Li Li 1_565 2_656 39.93(3) ? O1 Li Li 1_565 2_646 144.46(14) ? O1 Li Li 2_656 2_646 38.92(9) ? O1 Li Li 2_656 2_656 72.61(11) ? O1 Li O1 1_565 2_656 112.20(11) y O1 Li O2 2_656 . 108.08(12) y O1 Li O2 1_565 . 111.04(12) y O1 Li O5 2_656 . 105.35(12) y O1 Li O5 1_565 . 109.92(12) y O2 Li Li . 2_646 74.16(8) ? O2 Li Li . 2_656 130.66(15) ? O2 Li O5 . . 110.08(11) y O5 Li Li . 2_646 100.11(11) ? O5 Li Li . 2_656 117.27(13) ? C1 O1 Li . 1_545 133.25(11) ? C1 O1 Li . 2_646 123.58(11) ? Li O1 Li 1_545 2_646 101.15(8) y C1 O2 Li . . 113.53(11) ? C6 O3 H3 . . 111.2(12) ? C7 O4 H4 . . 110.7(14) ? Li O5 H5A . . 110.0(18) ? Li O5 H5B . . 106.7(16) ? H5A O5 H5B . . 106(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 C1 C2 . 1.4855(18) y C1 O1 . 1.2669(16) y C1 O2 . 1.2624(16) y C2 H2 . 0.9400 ? C2 C3 . 1.3285(19) y C3 H3A . 0.9400 ? C3 C4 . 1.4685(18) yes C4 C5 . 1.401(2) ? C4 C9 . 1.398(2) ? C5 H5 . 0.9400 ? C5 C6 . 1.3857(18) ? C6 C7 . 1.390(2) ? C6 O3 . 1.3757(17) y C7 C8 . 1.386(2) ? C7 O4 . 1.3781(16) y C8 H8 . 0.9400 ? C8 C9 . 1.388(2) ? C9 H9 . 0.9400 ? Li Li 2_646 2.979(3) ? Li Li 2_646 2.979(3) ? Li O1 2_656 1.949(2) y Li O1 1_565 1.908(2) y Li O2 . 1.962(2) y Li O5 . 2.005(3) y O3 H3 . 0.92(2) ? O4 H4 . 0.88(3) ? O5 H5A . 0.85(3) ? O5 H5B . 0.79(3) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O3 H3 O2 3_666 0.92(2) 1.83(2) 2.734(2) 168(2) O4 H4 O5 3_756 0.88(2) 1.94(2) 2.793(2) 160.7(2) O5 H5A O4 3_766 0.85(3) 2.13(2) 2.977(2) 173(2) O5 H5B O3 4_666 0.80(2) 2.33(2) 3.042(2) 150(2) O5 H5B O4 4_666 0.80(2) 2.33(2) 2.953(2) 136(2) 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 C1 C2 C3 C4 . . . . 176.94(13) ? C2 C1 O1 Li . . . 1_545 -12.6(2) ? C2 C1 O1 Li . . . 2_646 -173.12(12) ? C2 C1 O2 Li . . . . -131.35(13) ? C2 C3 C4 C5 . . . . 170.59(14) ? C2 C3 C4 C9 . . . . -13.2(2) ? C3 C4 C5 C6 . . . . 175.49(13) ? C3 C4 C9 C8 . . . . -173.87(13) ? C4 C5 C6 C7 . . . . -1.9(2) ? C4 C5 C6 O3 . . . . -179.85(13) ? C5 C4 C9 C8 . . . . 2.4(2) ? C5 C6 C7 C8 . . . . 3.4(2) ? C5 C6 C7 O4 . . . . -175.22(12) ? C6 C7 C8 C9 . . . . -2.0(2) ? C7 C8 C9 C4 . . . . -1.0(2) ? C9 C4 C5 C6 . . . . -0.9(2) ? O1 C1 C2 C3 . . . . 175.69(13) ? O1 C1 O2 Li . . . . 46.58(17) ? O2 C1 C2 C3 . . . . -6.3(2) ? O2 C1 O1 Li . . . 1_545 169.48(14) ? O2 C1 O1 Li . . . 2_646 8.9(2) ? O3 C6 C7 C8 . . . . -178.57(13) ? O3 C6 C7 O4 . . . . 2.84(18) ? O4 C7 C8 C9 . . . . 176.53(13) ?