#------------------------------------------------------------------------------ #$Date: 2026-05-19 23:57:05 +0100 (Tue, 19 May 2026) $ #$Revision: 305999 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721038.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7721038 loop_ _publ_author_name 'Zhao, Yunze' 'Zhang, Jianfeng' 'Li, Sai' 'Schwedtmann, Kevin' 'Wenzel, Marco' 'Doert, Thomas' 'Xing, Huifang' 'Yang, Liangrong' 'Weigand, Jan J.' _publ_section_title ; Spacer-Tuned Diphosphine Dioxides as Preorganised Co-Ligands for Synergistic Lithium Extraction with \b-Diketonates † ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00738D _journal_year 2026 _chemical_formula_moiety 'C35 H30 F3 Li O5 P2' _chemical_formula_sum 'C35 H30 F3 Li O5 P2' _chemical_formula_weight 656.47 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2026-03-12 _audit_creation_method ; Olex2 1.3 (compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938) ; _audit_update_record ; 2026-03-17 deposited with the CCDC. 2026-05-18 downloaded from the CCDC. ; _cell_angle_alpha 94.060(3) _cell_angle_beta 102.209(3) _cell_angle_gamma 112.235(3) _cell_formula_units_Z 2 _cell_length_a 10.1389(4) _cell_length_b 11.9692(4) _cell_length_c 14.6521(5) _cell_measurement_reflns_used 15945 _cell_measurement_temperature 170.00(10) _cell_measurement_theta_max 33.4610 _cell_measurement_theta_min 2.1910 _cell_volume 1586.14(11) _computing_cell_refinement 'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro system (CCD 43.127a 64-bit (release 16-06-2024))' _computing_data_reduction 'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 170.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 13.3333 _diffrn_detector_type 'Eiger2 1M' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.852 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -42.00 -12.90 0.30 3.00 -- -14.86 112.00 -21.00 97 2 \w 12.00 75.00 0.30 3.00 -- 14.70 57.00 0.00 210 3 \w -50.00 28.00 0.30 3.00 -- 14.70 -57.00 120.00 260 4 \w 8.00 33.80 0.30 3.00 -- 14.70 -99.00 -90.00 86 5 \w 11.00 82.10 0.30 3.00 -- 14.70 38.00 -60.00 237 6 \w 5.00 31.10 0.30 3.00 -- 14.70 -99.00 0.00 87 7 \w -69.00 3.00 0.30 3.00 -- -14.86 -77.00 90.00 240 8 \w -79.00 -1.00 0.30 3.00 -- -14.86 -57.00 -30.00 260 9 \w -74.00 -48.20 0.30 3.00 -- -14.86 178.00 -60.00 86 10 \w -88.00 -46.00 0.30 3.00 -- -14.86 178.00 90.00 140 11 \w -75.00 -41.10 0.30 3.00 -- -14.86 178.00 60.00 113 12 \w -64.00 8.00 0.30 3.00 -- -14.86 -77.00-150.00 240 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, Eiger2 1M' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0424785000 _diffrn_orient_matrix_UB_12 0.0630045000 _diffrn_orient_matrix_UB_13 0.0183846000 _diffrn_orient_matrix_UB_21 0.0085043000 _diffrn_orient_matrix_UB_22 0.0111180000 _diffrn_orient_matrix_UB_23 -0.0457608000 _diffrn_orient_matrix_UB_31 -0.0651372000 _diffrn_orient_matrix_UB_32 0.0110758000 _diffrn_orient_matrix_UB_33 -0.0095532000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_unetI/netI 0.0626 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.852 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 32586 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.852 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 34.085 _diffrn_reflns_theta_min 2.159 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.197 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_correction_T_min 0.961 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.375 _exptl_crystal_description plate _exptl_crystal_F_000 680 _exptl_crystal_size_max 0.235 _exptl_crystal_size_mid 0.214 _exptl_crystal_size_min 0.122 _refine_diff_density_max 0.500 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.063 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 423 _refine_ls_number_reflns 11086 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0452 _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^)+(0.0588P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1112 _refine_ls_wR_factor_ref 0.1219 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7773 _reflns_number_total 11086 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00738d2.cif _cod_data_source_block jjw1837 _cod_original_cell_volume 1586.14(10) _cod_database_code 7721038 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C35H30F3LiO5P2 _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_max 0.976 _shelx_estimated_absorpt_t_min 0.955 _reflns_odcompleteness_completeness 99.93 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 30.44 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Secondary CH2 refined with riding coordinates: C23(H23A,H23B) 2.b Aromatic/amide H refined with riding coordinates: C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35) ; _shelx_res_file ; TITL jjw1837_a.res in P-1 jjw1837.res created by SHELXL-2018/3 at 09:14:19 on 12-Mar-2026 REM Old TITL jjw1837 in P-1 REM SHELXT solution in P-1: R1 0.113, Rweak 0.006, Alpha 0.042 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C35 Li O4 F4 P2 CELL 0.71073 10.1389 11.9692 14.6521 94.06 102.209 112.235 ZERR 2 0.0004 0.0004 0.0005 0.003 0.003 0.003 LATT 1 SFAC C H F Li O P UNIT 70 60 6 2 10 4 L.S. 4 PLAN 2 SIZE 0.122 0.214 0.235 TEMP -103 CONF FREE Li1 H5a list 4 MORE -1 BOND $H fmap 2 53 acta OMIT 10 -10 7 REM REM REM WGHT 0.058800 FVAR 0.60066 P1 6 0.158624 0.685355 0.469795 11.00000 0.01987 0.02015 = 0.02066 0.00388 0.00655 0.00841 P2 6 0.183782 0.503947 0.323337 11.00000 0.02073 0.02192 = 0.02198 0.00211 0.00586 0.00991 F1 3 0.733867 0.937588 0.912633 11.00000 0.02945 0.04789 = 0.04463 -0.00419 0.01423 0.00272 F2 3 0.537604 0.967924 0.904474 11.00000 0.05240 0.03265 = 0.05807 -0.00853 0.00230 0.02145 F3 3 0.604665 0.872813 1.010751 11.00000 0.05099 0.04274 = 0.02525 -0.00364 0.01033 0.00254 O1 5 0.495073 0.783451 0.764259 11.00000 0.04969 0.02738 = 0.02384 0.00420 0.00843 0.01171 O2 5 0.310424 0.534124 0.736343 11.00000 0.04584 0.02755 = 0.02237 0.00271 0.00255 0.01215 O3 5 0.232403 0.653811 0.556984 11.00000 0.02598 0.03021 = 0.02324 0.00690 0.00626 0.01377 O4 5 0.319707 0.514918 0.393640 11.00000 0.02664 0.02995 = 0.02518 0.00159 0.00339 0.01467 O5 5 0.492075 0.606026 0.581811 11.00000 0.03393 0.04738 = 0.02722 -0.00220 0.00174 0.02656 H5A 2 0.440953 0.580241 0.527276 11.00000 0.05709 H5B 2 0.550204 0.571122 0.593297 11.00000 0.05047 C1 1 0.595082 0.885028 0.920118 11.00000 0.02792 0.03180 = 0.02733 0.00061 0.00862 0.00971 C2 1 0.504422 0.766259 0.848623 11.00000 0.02769 0.02657 = 0.02376 0.00084 0.00602 0.01167 C3 1 0.443292 0.659724 0.883941 11.00000 0.03154 0.02941 = 0.02140 0.00318 0.00425 0.01167 AFIX 43 H3 2 0.466852 0.662332 0.950570 11.00000 -1.20000 AFIX 0 C4 1 0.346683 0.546443 0.824800 11.00000 0.02887 0.02844 = 0.02353 0.00505 0.00403 0.01571 C5 1 0.279709 0.435750 0.868546 11.00000 0.02953 0.02731 = 0.02881 0.00655 0.00451 0.01450 C6 1 0.205145 0.321727 0.808833 11.00000 0.05278 0.02966 = 0.03246 0.00725 0.00394 0.01695 AFIX 43 H6 2 0.204074 0.315947 0.743659 11.00000 -1.20000 AFIX 0 C7 1 0.133349 0.217910 0.844072 11.00000 0.06020 0.02730 = 0.04966 0.01030 0.00241 0.01495 AFIX 43 H7 2 0.084162 0.141082 0.803127 11.00000 -1.20000 AFIX 0 C8 1 0.132519 0.224940 0.938386 11.00000 0.04923 0.03741 = 0.05659 0.02494 0.01383 0.01745 AFIX 43 H8 2 0.081348 0.153561 0.962091 11.00000 -1.20000 AFIX 0 C9 1 0.205982 0.335538 0.997582 11.00000 0.05140 0.04575 = 0.03968 0.01876 0.01761 0.02074 AFIX 43 H9 2 0.206649 0.340394 1.062686 11.00000 -1.20000 AFIX 0 C10 1 0.279273 0.440311 0.963340 11.00000 0.04358 0.03504 = 0.03094 0.00799 0.01096 0.01639 AFIX 43 H10 2 0.329898 0.516278 1.005311 11.00000 -1.20000 AFIX 0 C11 1 0.022702 0.739175 0.491645 11.00000 0.02266 0.02220 = 0.02321 0.00560 0.00907 0.01016 C12 1 0.076397 0.846991 0.557668 11.00000 0.02782 0.02494 = 0.03561 -0.00005 0.00990 0.00888 AFIX 43 H12 2 0.179192 0.888365 0.586298 11.00000 -1.20000 AFIX 0 C13 1 -0.020561 0.892931 0.581001 11.00000 0.04302 0.02799 = 0.03799 0.00097 0.01618 0.01736 AFIX 43 H13 2 0.016012 0.966712 0.624937 11.00000 -1.20000 AFIX 0 C14 1 -0.169964 0.832287 0.540875 11.00000 0.03891 0.04176 = 0.03605 0.01065 0.01816 0.02659 AFIX 43 H14 2 -0.236084 0.864143 0.557404 11.00000 -1.20000 AFIX 0 C15 1 -0.223770 0.725271 0.476668 11.00000 0.02586 0.04318 = 0.03524 0.00540 0.00836 0.01746 AFIX 43 H15 2 -0.326904 0.683537 0.449351 11.00000 -1.20000 AFIX 0 C16 1 -0.127561 0.678292 0.451803 11.00000 0.02618 0.02832 = 0.02711 0.00197 0.00702 0.01145 AFIX 43 H16 2 -0.164904 0.604648 0.407611 11.00000 -1.20000 AFIX 0 C17 1 0.283160 0.802589 0.422416 11.00000 0.02371 0.01981 = 0.02369 0.00266 0.00840 0.00725 C18 1 0.432934 0.827757 0.447290 11.00000 0.02357 0.02331 = 0.03022 0.00529 0.00729 0.00809 AFIX 43 H18 2 0.470022 0.786635 0.492453 11.00000 -1.20000 AFIX 0 C19 1 0.527908 0.912739 0.406213 11.00000 0.02411 0.02951 = 0.04104 0.00722 0.01187 0.00658 AFIX 43 H19 2 0.629933 0.928811 0.422656 11.00000 -1.20000 AFIX 0 C20 1 0.475567 0.974404 0.341484 11.00000 0.03597 0.02882 = 0.03876 0.01128 0.01809 0.00822 AFIX 43 H20 2 0.541585 1.033132 0.313989 11.00000 -1.20000 AFIX 0 C21 1 0.326838 0.950502 0.316758 11.00000 0.03974 0.03597 = 0.03711 0.01820 0.01232 0.01584 AFIX 43 H21 2 0.290625 0.992731 0.272190 11.00000 -1.20000 AFIX 0 C22 1 0.231016 0.865168 0.356934 11.00000 0.02482 0.03420 = 0.03518 0.01272 0.00758 0.01241 AFIX 43 H22 2 0.128975 0.848992 0.339869 11.00000 -1.20000 AFIX 0 C23 1 0.062861 0.554826 0.374429 11.00000 0.02101 0.02173 = 0.02332 0.00296 0.00767 0.00844 AFIX 23 H23A 2 -0.000120 0.576442 0.323623 11.00000 -1.20000 H23B 2 -0.002786 0.485776 0.398832 11.00000 -1.20000 AFIX 0 C24 1 0.228480 0.591076 0.230552 11.00000 0.02882 0.02582 = 0.02525 0.00326 0.01106 0.01286 C25 1 0.119480 0.595604 0.156993 11.00000 0.03732 0.05659 = 0.03623 0.01693 0.01598 0.02672 AFIX 43 H25 2 0.018409 0.552114 0.154860 11.00000 -1.20000 AFIX 0 C26 1 0.158251 0.663405 0.086987 11.00000 0.06251 0.06730 = 0.03726 0.02470 0.02177 0.04409 AFIX 43 H26 2 0.083626 0.665692 0.036485 11.00000 -1.20000 AFIX 0 C27 1 0.304765 0.727714 0.090159 11.00000 0.07216 0.03974 = 0.03899 0.01564 0.03224 0.02645 AFIX 43 H27 2 0.330742 0.776139 0.042932 11.00000 -1.20000 AFIX 0 C28 1 0.412494 0.721977 0.160931 11.00000 0.04568 0.04200 = 0.03985 0.00377 0.02266 0.00163 AFIX 43 H28 2 0.513255 0.765085 0.162118 11.00000 -1.20000 AFIX 0 C29 1 0.375212 0.653084 0.231493 11.00000 0.02968 0.03904 = 0.02900 0.00209 0.01022 0.00650 AFIX 43 H29 2 0.450526 0.648641 0.280302 11.00000 -1.20000 AFIX 0 C30 1 0.071236 0.349442 0.263944 11.00000 0.02618 0.02411 = 0.02341 0.00098 0.00620 0.01086 C31 1 0.143549 0.276147 0.242037 11.00000 0.02879 0.02762 = 0.03384 0.00226 0.01129 0.01322 AFIX 43 H31 2 0.248063 0.306781 0.261969 11.00000 -1.20000 AFIX 0 C32 1 0.062670 0.158818 0.191241 11.00000 0.04520 0.03061 = 0.03805 0.00014 0.01269 0.02084 AFIX 43 H32 2 0.112030 0.109086 0.176734 11.00000 -1.20000 AFIX 0 C33 1 -0.088273 0.114059 0.161780 11.00000 0.04879 0.02760 = 0.04260 -0.00701 0.00056 0.01462 AFIX 43 H33 2 -0.142809 0.034397 0.125488 11.00000 -1.20000 AFIX 0 C34 1 -0.161043 0.184541 0.184766 11.00000 0.02985 0.03356 = 0.06746 -0.01044 -0.00595 0.01019 AFIX 43 H34 2 -0.265709 0.152460 0.165917 11.00000 -1.20000 AFIX 0 C35 1 -0.081230 0.302361 0.235452 11.00000 0.02894 0.02904 = 0.05484 -0.00537 0.00336 0.01343 AFIX 43 H35 2 -0.131580 0.350927 0.250658 11.00000 -1.20000 AFIX 0 LI1 4 0.385772 0.653197 0.659092 11.00000 0.03390 0.03048 = 0.02416 0.00375 0.00651 0.01450 HKLF 4 REM jjw1837_a.res in P-1 REM wR2 = 0.1219, GooF = S = 1.045, Restrained GooF = 1.045 for all data REM R1 = 0.0452 for 7773 Fo > 4sig(Fo) and 0.0707 for all 11086 data REM 423 parameters refined using 0 restraints END WGHT 0.0588 0.0000 REM Highest difference peak 0.500, deepest hole -0.403, 1-sigma level 0.063 Q1 1 0.1985 0.5587 0.2764 11.00000 0.05 0.50 Q2 1 0.1789 0.6772 0.5219 11.00000 0.05 0.39 ; _shelx_res_checksum 79076 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.734 _oxdiff_exptl_absorpt_empirical_full_min 0.627 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.15862(4) 0.68536(3) 0.46979(2) 0.01988(8) Uani 1 1 d . . . . . P2 P 0.18378(4) 0.50395(3) 0.32334(2) 0.02117(8) Uani 1 1 d . . . . . F1 F 0.73387(10) 0.93759(9) 0.91263(6) 0.0445(2) Uani 1 1 d . . . . . F2 F 0.53760(11) 0.96792(8) 0.90447(7) 0.0492(3) Uani 1 1 d . . . . . F3 F 0.60466(11) 0.87281(8) 1.01075(6) 0.0451(2) Uani 1 1 d . . . . . O1 O 0.49507(12) 0.78345(9) 0.76426(7) 0.0350(2) Uani 1 1 d . . . . . O2 O 0.31042(12) 0.53412(9) 0.73634(6) 0.0338(2) Uani 1 1 d . . . . . O3 O 0.23240(10) 0.65381(8) 0.55698(6) 0.02561(19) Uani 1 1 d . . . . . O4 O 0.31971(10) 0.51492(8) 0.39364(6) 0.0270(2) Uani 1 1 d . . . . . O5 O 0.49208(13) 0.60603(10) 0.58181(8) 0.0345(2) Uani 1 1 d . . . . . H5A H 0.441(2) 0.5802(18) 0.5273(16) 0.057(6) Uiso 1 1 d . . . . . H5B H 0.550(2) 0.5711(17) 0.5933(13) 0.050(5) Uiso 1 1 d . . . . . C1 C 0.59508(16) 0.88503(13) 0.92012(9) 0.0297(3) Uani 1 1 d . . . . . C2 C 0.50442(15) 0.76626(12) 0.84862(9) 0.0261(3) Uani 1 1 d . . . . . C3 C 0.44329(16) 0.65972(12) 0.88394(9) 0.0281(3) Uani 1 1 d . . . . . H3 H 0.466852 0.662332 0.950570 0.034 Uiso 1 1 calc R U . . . C4 C 0.34668(15) 0.54644(12) 0.82480(9) 0.0261(3) Uani 1 1 d . . . . . C5 C 0.27971(16) 0.43575(12) 0.86855(9) 0.0280(3) Uani 1 1 d . . . . . C6 C 0.20515(19) 0.32173(13) 0.80883(11) 0.0392(4) Uani 1 1 d . . . . . H6 H 0.204074 0.315947 0.743659 0.047 Uiso 1 1 calc R U . . . C7 C 0.1333(2) 0.21791(15) 0.84407(13) 0.0483(4) Uani 1 1 d . . . . . H7 H 0.084162 0.141082 0.803127 0.058 Uiso 1 1 calc R U . . . C8 C 0.1325(2) 0.22494(16) 0.93839(13) 0.0468(4) Uani 1 1 d . . . . . H8 H 0.081348 0.153561 0.962091 0.056 Uiso 1 1 calc R U . . . C9 C 0.2060(2) 0.33554(15) 0.99758(12) 0.0437(4) Uani 1 1 d . . . . . H9 H 0.206649 0.340394 1.062686 0.052 Uiso 1 1 calc R U . . . C10 C 0.27927(18) 0.44031(14) 0.96334(10) 0.0360(3) Uani 1 1 d . . . . . H10 H 0.329898 0.516278 1.005311 0.043 Uiso 1 1 calc R U . . . C11 C 0.02270(14) 0.73917(11) 0.49164(8) 0.0217(2) Uani 1 1 d . . . . . C12 C 0.07640(16) 0.84699(12) 0.55767(10) 0.0300(3) Uani 1 1 d . . . . . H12 H 0.179192 0.888365 0.586298 0.036 Uiso 1 1 calc R U . . . C13 C -0.02056(18) 0.89293(13) 0.58100(10) 0.0347(3) Uani 1 1 d . . . . . H13 H 0.016012 0.966712 0.624937 0.042 Uiso 1 1 calc R U . . . C14 C -0.16996(17) 0.83229(14) 0.54087(10) 0.0341(3) Uani 1 1 d . . . . . H14 H -0.236084 0.864143 0.557404 0.041 Uiso 1 1 calc R U . . . C15 C -0.22377(16) 0.72527(14) 0.47667(10) 0.0337(3) Uani 1 1 d . . . . . H15 H -0.326904 0.683537 0.449351 0.040 Uiso 1 1 calc R U . . . C16 C -0.12756(15) 0.67829(12) 0.45180(9) 0.0272(3) Uani 1 1 d . . . . . H16 H -0.164904 0.604648 0.407611 0.033 Uiso 1 1 calc R U . . . C17 C 0.28316(14) 0.80259(11) 0.42242(8) 0.0226(2) Uani 1 1 d . . . . . C18 C 0.43293(15) 0.82776(11) 0.44729(9) 0.0260(3) Uani 1 1 d . . . . . H18 H 0.470022 0.786635 0.492453 0.031 Uiso 1 1 calc R U . . . C19 C 0.52791(16) 0.91274(13) 0.40621(10) 0.0322(3) Uani 1 1 d . . . . . H19 H 0.629933 0.928811 0.422656 0.039 Uiso 1 1 calc R U . . . C20 C 0.47557(17) 0.97440(13) 0.34148(10) 0.0343(3) Uani 1 1 d . . . . . H20 H 0.541585 1.033132 0.313989 0.041 Uiso 1 1 calc R U . . . C21 C 0.32684(18) 0.95050(14) 0.31676(11) 0.0364(3) Uani 1 1 d . . . . . H21 H 0.290625 0.992731 0.272190 0.044 Uiso 1 1 calc R U . . . C22 C 0.23102(16) 0.86517(13) 0.35693(10) 0.0309(3) Uani 1 1 d . . . . . H22 H 0.128975 0.848992 0.339869 0.037 Uiso 1 1 calc R U . . . C23 C 0.06286(14) 0.55483(11) 0.37443(8) 0.0218(2) Uani 1 1 d . . . . . H23A H -0.000120 0.576442 0.323623 0.026 Uiso 1 1 calc R U . . . H23B H -0.002786 0.485776 0.398832 0.026 Uiso 1 1 calc R U . . . C24 C 0.22848(15) 0.59108(12) 0.23055(9) 0.0254(3) Uani 1 1 d . . . . . C25 C 0.11948(19) 0.59560(16) 0.15699(11) 0.0394(4) Uani 1 1 d . . . . . H25 H 0.018409 0.552114 0.154860 0.047 Uiso 1 1 calc R U . . . C26 C 0.1583(2) 0.66340(18) 0.08699(12) 0.0478(4) Uani 1 1 d . . . . . H26 H 0.083626 0.665692 0.036485 0.057 Uiso 1 1 calc R U . . . C27 C 0.3048(2) 0.72771(15) 0.09016(11) 0.0457(4) Uani 1 1 d . . . . . H27 H 0.330742 0.776139 0.042932 0.055 Uiso 1 1 calc R U . . . C28 C 0.4125(2) 0.72198(16) 0.16093(11) 0.0457(4) Uani 1 1 d . . . . . H28 H 0.513255 0.765085 0.162118 0.055 Uiso 1 1 calc R U . . . C29 C 0.37521(17) 0.65308(14) 0.23149(10) 0.0346(3) Uani 1 1 d . . . . . H29 H 0.450526 0.648641 0.280302 0.042 Uiso 1 1 calc R U . . . C30 C 0.07124(15) 0.34944(11) 0.26394(8) 0.0245(3) Uani 1 1 d . . . . . C31 C 0.14355(16) 0.27615(12) 0.24204(10) 0.0291(3) Uani 1 1 d . . . . . H31 H 0.248063 0.306781 0.261969 0.035 Uiso 1 1 calc R U . . . C32 C 0.06267(18) 0.15882(13) 0.19124(10) 0.0362(3) Uani 1 1 d . . . . . H32 H 0.112030 0.109086 0.176734 0.043 Uiso 1 1 calc R U . . . C33 C -0.0883(2) 0.11406(14) 0.16178(11) 0.0424(4) Uani 1 1 d . . . . . H33 H -0.142809 0.034397 0.125488 0.051 Uiso 1 1 calc R U . . . C34 C -0.16104(19) 0.18454(15) 0.18477(14) 0.0485(4) Uani 1 1 d . . . . . H34 H -0.265709 0.152460 0.165917 0.058 Uiso 1 1 calc R U . . . C35 C -0.08123(17) 0.30236(13) 0.23545(12) 0.0389(4) Uani 1 1 d . . . . . H35 H -0.131580 0.350927 0.250658 0.047 Uiso 1 1 calc R U . . . Li1 Li 0.3858(3) 0.6532(2) 0.65909(15) 0.0293(5) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.01987(16) 0.02015(15) 0.02066(14) 0.00388(11) 0.00655(12) 0.00841(13) P2 0.02073(17) 0.02192(15) 0.02198(15) 0.00211(11) 0.00586(12) 0.00991(13) F1 0.0294(5) 0.0479(5) 0.0446(5) -0.0042(4) 0.0142(4) 0.0027(4) F2 0.0524(6) 0.0326(5) 0.0581(6) -0.0085(4) 0.0023(5) 0.0215(5) F3 0.0510(6) 0.0427(5) 0.0253(4) -0.0036(4) 0.0103(4) 0.0025(4) O1 0.0497(7) 0.0274(5) 0.0238(4) 0.0042(4) 0.0084(4) 0.0117(5) O2 0.0458(6) 0.0275(5) 0.0224(4) 0.0027(4) 0.0025(4) 0.0121(5) O3 0.0260(5) 0.0302(5) 0.0232(4) 0.0069(3) 0.0063(4) 0.0138(4) O4 0.0266(5) 0.0299(5) 0.0252(4) 0.0016(3) 0.0034(4) 0.0147(4) O5 0.0339(6) 0.0474(6) 0.0272(5) -0.0022(4) 0.0017(4) 0.0266(5) C1 0.0279(7) 0.0318(7) 0.0273(6) 0.0006(5) 0.0086(5) 0.0097(6) C2 0.0277(7) 0.0266(6) 0.0238(6) 0.0008(5) 0.0060(5) 0.0117(6) C3 0.0315(7) 0.0294(7) 0.0214(6) 0.0032(5) 0.0043(5) 0.0117(6) C4 0.0289(7) 0.0284(6) 0.0235(6) 0.0051(5) 0.0040(5) 0.0157(6) C5 0.0295(7) 0.0273(6) 0.0288(6) 0.0065(5) 0.0045(5) 0.0145(6) C6 0.0528(10) 0.0297(7) 0.0325(7) 0.0073(6) 0.0039(7) 0.0169(7) C7 0.0602(12) 0.0273(8) 0.0497(9) 0.0103(7) 0.0024(8) 0.0150(8) C8 0.0492(11) 0.0374(9) 0.0566(10) 0.0249(7) 0.0138(8) 0.0175(8) C9 0.0514(11) 0.0458(9) 0.0397(8) 0.0188(7) 0.0176(8) 0.0207(8) C10 0.0436(9) 0.0350(8) 0.0309(7) 0.0080(6) 0.0110(6) 0.0164(7) C11 0.0227(6) 0.0222(6) 0.0232(5) 0.0056(4) 0.0091(5) 0.0102(5) C12 0.0278(7) 0.0249(6) 0.0356(7) 0.0000(5) 0.0099(6) 0.0089(6) C13 0.0430(9) 0.0280(7) 0.0380(7) 0.0010(6) 0.0162(7) 0.0174(7) C14 0.0389(9) 0.0418(8) 0.0361(7) 0.0106(6) 0.0182(6) 0.0266(7) C15 0.0259(7) 0.0432(8) 0.0352(7) 0.0054(6) 0.0084(6) 0.0175(7) C16 0.0262(7) 0.0283(6) 0.0271(6) 0.0020(5) 0.0070(5) 0.0115(6) C17 0.0237(6) 0.0198(5) 0.0237(5) 0.0027(4) 0.0084(5) 0.0073(5) C18 0.0236(7) 0.0233(6) 0.0302(6) 0.0053(5) 0.0073(5) 0.0081(5) C19 0.0241(7) 0.0295(7) 0.0410(8) 0.0072(6) 0.0119(6) 0.0066(6) C20 0.0360(8) 0.0288(7) 0.0388(7) 0.0113(6) 0.0181(6) 0.0082(6) C21 0.0397(9) 0.0360(8) 0.0371(7) 0.0182(6) 0.0123(7) 0.0158(7) C22 0.0248(7) 0.0342(7) 0.0352(7) 0.0127(6) 0.0076(6) 0.0124(6) C23 0.0210(6) 0.0217(6) 0.0233(5) 0.0030(4) 0.0077(5) 0.0084(5) C24 0.0288(7) 0.0258(6) 0.0253(6) 0.0033(5) 0.0111(5) 0.0129(6) C25 0.0373(9) 0.0566(10) 0.0362(8) 0.0169(7) 0.0160(7) 0.0267(8) C26 0.0625(12) 0.0673(12) 0.0373(8) 0.0247(8) 0.0218(8) 0.0441(10) C27 0.0722(13) 0.0397(9) 0.0390(8) 0.0156(7) 0.0322(8) 0.0265(9) C28 0.0457(10) 0.0420(9) 0.0398(8) 0.0038(7) 0.0227(8) 0.0016(8) C29 0.0297(8) 0.0390(8) 0.0290(7) 0.0021(6) 0.0102(6) 0.0065(6) C30 0.0262(7) 0.0241(6) 0.0234(6) 0.0010(4) 0.0062(5) 0.0109(5) C31 0.0288(7) 0.0276(6) 0.0338(7) 0.0023(5) 0.0113(6) 0.0132(6) C32 0.0452(9) 0.0306(7) 0.0381(7) 0.0001(6) 0.0127(7) 0.0208(7) C33 0.0488(10) 0.0276(7) 0.0426(8) -0.0070(6) 0.0006(7) 0.0146(7) C34 0.0299(9) 0.0336(8) 0.0675(11) -0.0104(7) -0.0059(8) 0.0102(7) C35 0.0289(8) 0.0290(7) 0.0548(9) -0.0054(6) 0.0034(7) 0.0134(6) Li1 0.0339(13) 0.0305(12) 0.0242(10) 0.0038(8) 0.0065(9) 0.0145(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -2 5 0.0610 0 2 -5 0.0610 -5 2 2 0.1119 5 -2 -2 0.1119 0 -5 -1 0.0934 0 5 1 0.0934 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 P1 C11 111.28(5) . . ? O3 P1 C17 113.56(6) . . ? O3 P1 C23 112.41(5) . . ? C11 P1 C23 106.61(6) . . ? C17 P1 C11 106.60(6) . . ? C17 P1 C23 105.92(6) . . ? O4 P2 C23 113.83(5) . . ? O4 P2 C24 111.21(6) . . ? O4 P2 C30 112.96(6) . . ? C24 P2 C23 107.36(6) . . ? C30 P2 C23 105.63(6) . . ? C30 P2 C24 105.28(6) . . ? C2 O1 Li1 122.27(12) . . ? C4 O2 Li1 127.44(12) . . ? P1 O3 Li1 160.20(10) . . ? H5A O5 H5B 109.2(18) . . ? Li1 O5 H5A 110.1(14) . . ? Li1 O5 H5B 131.0(13) . . ? F1 C1 C2 112.03(10) . . ? F2 C1 F1 105.80(12) . . ? F2 C1 C2 110.71(11) . . ? F3 C1 F1 106.24(11) . . ? F3 C1 F2 106.35(11) . . ? F3 C1 C2 115.11(12) . . ? O1 C2 C1 112.54(12) . . ? O1 C2 C3 129.79(12) . . ? C3 C2 C1 117.65(11) . . ? C2 C3 H3 118.6 . . ? C2 C3 C4 122.76(12) . . ? C4 C3 H3 118.6 . . ? O2 C4 C3 123.07(12) . . ? O2 C4 C5 117.22(12) . . ? C3 C4 C5 119.68(11) . . ? C6 C5 C4 117.97(12) . . ? C10 C5 C4 123.90(12) . . ? C10 C5 C6 118.01(14) . . ? C5 C6 H6 119.7 . . ? C7 C6 C5 120.51(15) . . ? C7 C6 H6 119.7 . . ? C6 C7 H7 119.8 . . ? C6 C7 C8 120.47(15) . . ? C8 C7 H7 119.8 . . ? C7 C8 H8 120.2 . . ? C9 C8 C7 119.57(16) . . ? C9 C8 H8 120.2 . . ? C8 C9 H9 119.7 . . ? C8 C9 C10 120.58(15) . . ? C10 C9 H9 119.7 . . ? C5 C10 H10 119.6 . . ? C9 C10 C5 120.85(14) . . ? C9 C10 H10 119.6 . . ? C12 C11 P1 115.88(10) . . ? C16 C11 P1 124.45(9) . . ? C16 C11 C12 119.58(11) . . ? C11 C12 H12 120.1 . . ? C13 C12 C11 119.85(13) . . ? C13 C12 H12 120.1 . . ? C12 C13 H13 119.8 . . ? C14 C13 C12 120.34(13) . . ? C14 C13 H13 119.8 . . ? C13 C14 H14 119.9 . . ? C13 C14 C15 120.11(12) . . ? C15 C14 H14 119.9 . . ? C14 C15 H15 119.9 . . ? C14 C15 C16 120.28(14) . . ? C16 C15 H15 119.9 . . ? C11 C16 C15 119.81(12) . . ? C11 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C18 C17 P1 119.86(9) . . ? C18 C17 C22 119.21(12) . . ? C22 C17 P1 120.85(10) . . ? C17 C18 H18 120.0 . . ? C19 C18 C17 119.95(12) . . ? C19 C18 H18 120.0 . . ? C18 C19 H19 119.7 . . ? C20 C19 C18 120.54(13) . . ? C20 C19 H19 119.7 . . ? C19 C20 H20 120.0 . . ? C19 C20 C21 119.90(13) . . ? C21 C20 H20 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 C20 119.96(13) . . ? C22 C21 H21 120.0 . . ? C17 C22 H22 119.8 . . ? C21 C22 C17 120.44(13) . . ? C21 C22 H22 119.8 . . ? P1 C23 P2 114.49(7) . . ? P1 C23 H23A 108.6 . . ? P1 C23 H23B 108.6 . . ? P2 C23 H23A 108.6 . . ? P2 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? C25 C24 P2 121.73(11) . . ? C29 C24 P2 119.06(11) . . ? C29 C24 C25 119.19(13) . . ? C24 C25 H25 120.0 . . ? C26 C25 C24 120.01(16) . . ? C26 C25 H25 120.0 . . ? C25 C26 H26 119.9 . . ? C27 C26 C25 120.29(16) . . ? C27 C26 H26 119.9 . . ? C26 C27 H27 119.9 . . ? C28 C27 C26 120.18(15) . . ? C28 C27 H27 119.9 . . ? C27 C28 H28 119.9 . . ? C27 C28 C29 120.21(17) . . ? C29 C28 H28 119.9 . . ? C24 C29 C28 120.08(15) . . ? C24 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C31 C30 P2 117.48(10) . . ? C35 C30 P2 123.38(9) . . ? C35 C30 C31 119.07(12) . . ? C30 C31 H31 120.0 . . ? C32 C31 C30 119.98(13) . . ? C32 C31 H31 120.0 . . ? C31 C32 H32 119.8 . . ? C33 C32 C31 120.39(13) . . ? C33 C32 H32 119.8 . . ? C32 C33 H33 119.9 . . ? C32 C33 C34 120.14(14) . . ? C34 C33 H33 119.9 . . ? C33 C34 H34 120.0 . . ? C33 C34 C35 119.99(16) . . ? C35 C34 H34 120.0 . . ? C30 C35 C34 120.39(13) . . ? C30 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? O1 Li1 O2 94.10(10) . . ? O1 Li1 O3 124.52(12) . . ? O1 Li1 H5A 134.3(5) . . ? O2 Li1 O3 111.95(13) . . ? O2 Li1 H5A 115.2(5) . . ? O3 Li1 H5A 77.7(5) . . ? O5 Li1 O1 118.22(14) . . ? O5 Li1 O2 112.38(12) . . ? O5 Li1 O3 96.45(11) . . ? O5 Li1 H5A 19.4(5) . . ? 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 P1 O3 1.4873(9) . ? P1 C11 1.8016(12) . ? P1 C17 1.7925(13) . ? P1 C23 1.8180(12) . ? P2 O4 1.4903(9) . ? P2 C23 1.8229(12) . ? P2 C24 1.8013(13) . ? P2 C30 1.7984(13) . ? F1 C1 1.3390(17) . ? F2 C1 1.3379(16) . ? F3 C1 1.3334(16) . ? O1 C2 1.2572(15) . ? O1 Li1 1.914(2) . ? O2 C4 1.2518(15) . ? O2 Li1 1.915(3) . ? O3 Li1 1.919(2) . ? O5 H5A 0.82(2) . ? O5 H5B 0.84(2) . ? O5 Li1 1.910(2) . ? C1 C2 1.5350(19) . ? C2 C3 1.3816(19) . ? C3 H3 0.9500 . ? C3 C4 1.4207(19) . ? C4 C5 1.5003(19) . ? C5 C6 1.404(2) . ? C5 C10 1.3871(19) . ? C6 H6 0.9500 . ? C6 C7 1.381(2) . ? C7 H7 0.9500 . ? C7 C8 1.380(2) . ? C8 H8 0.9500 . ? C8 C9 1.370(2) . ? C9 H9 0.9500 . ? C9 C10 1.385(2) . ? C10 H10 0.9500 . ? C11 C12 1.4023(17) . ? C11 C16 1.3843(19) . ? C12 H12 0.9500 . ? C12 C13 1.3821(19) . ? C13 H13 0.9500 . ? C13 C14 1.378(2) . ? C14 H14 0.9500 . ? C14 C15 1.381(2) . ? C15 H15 0.9500 . ? C15 C16 1.3917(18) . ? C16 H16 0.9500 . ? C17 C18 1.3906(18) . ? C17 C22 1.3957(18) . ? C18 H18 0.9500 . ? C18 C19 1.3837(19) . ? C19 H19 0.9500 . ? C19 C20 1.381(2) . ? C20 H20 0.9500 . ? C20 C21 1.384(2) . ? C21 H21 0.9500 . ? C21 C22 1.382(2) . ? C22 H22 0.9500 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.391(2) . ? C24 C29 1.385(2) . ? C25 H25 0.9500 . ? C25 C26 1.383(2) . ? C26 H26 0.9500 . ? C26 C27 1.379(3) . ? C27 H27 0.9500 . ? C27 C28 1.364(3) . ? C28 H28 0.9500 . ? C28 C29 1.394(2) . ? C29 H29 0.9500 . ? C30 C31 1.3988(17) . ? C30 C35 1.384(2) . ? C31 H31 0.9500 . ? C31 C32 1.3859(19) . ? C32 H32 0.9500 . ? C32 C33 1.372(2) . ? C33 H33 0.9500 . ? C33 C34 1.380(2) . ? C34 H34 0.9500 . ? C34 C35 1.389(2) . ? C35 H35 0.9500 . ? Li1 H5A 2.32(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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 C11 C12 C13 -178.02(11) . . . . ? P1 C11 C16 C15 177.20(10) . . . . ? P1 C17 C18 C19 175.91(10) . . . . ? P1 C17 C22 C21 -176.32(11) . . . . ? P2 C24 C25 C26 -179.91(12) . . . . ? P2 C24 C29 C28 -179.42(11) . . . . ? P2 C30 C31 C32 -176.10(11) . . . . ? P2 C30 C35 C34 176.05(14) . . . . ? F1 C1 C2 O1 -60.53(16) . . . . ? F1 C1 C2 C3 121.06(14) . . . . ? F2 C1 C2 O1 57.30(16) . . . . ? F2 C1 C2 C3 -121.10(14) . . . . ? F3 C1 C2 O1 177.94(12) . . . . ? F3 C1 C2 C3 -0.47(18) . . . . ? O1 C2 C3 C4 -3.8(2) . . . . ? O2 C4 C5 C6 12.23(19) . . . . ? O2 C4 C5 C10 -163.66(13) . . . . ? O3 P1 C11 C12 62.49(11) . . . . ? O3 P1 C11 C16 -114.05(11) . . . . ? O3 P1 C17 C18 19.92(11) . . . . ? O3 P1 C17 C22 -163.32(10) . . . . ? O3 P1 C23 P2 -69.77(8) . . . . ? O4 P2 C23 P1 35.87(9) . . . . ? O4 P2 C24 C25 -179.54(11) . . . . ? O4 P2 C24 C29 1.82(12) . . . . ? O4 P2 C30 C31 -36.91(12) . . . . ? O4 P2 C30 C35 146.17(12) . . . . ? C1 C2 C3 C4 174.26(12) . . . . ? C2 C3 C4 O2 0.6(2) . . . . ? C2 C3 C4 C5 -177.49(12) . . . . ? C3 C4 C5 C6 -169.59(13) . . . . ? C3 C4 C5 C10 14.5(2) . . . . ? C4 C5 C6 C7 -175.86(14) . . . . ? C4 C5 C10 C9 175.20(14) . . . . ? C5 C6 C7 C8 0.7(3) . . . . ? C6 C5 C10 C9 -0.7(2) . . . . ? C6 C7 C8 C9 -1.2(3) . . . . ? C7 C8 C9 C10 0.8(3) . . . . ? C8 C9 C10 C5 0.1(3) . . . . ? C10 C5 C6 C7 0.3(2) . . . . ? C11 P1 O3 Li1 -123.9(3) . . . . ? C11 P1 C17 C18 142.81(10) . . . . ? C11 P1 C17 C22 -40.43(12) . . . . ? C11 P1 C23 P2 168.05(6) . . . . ? C11 C12 C13 C14 1.0(2) . . . . ? C12 C11 C16 C15 0.8(2) . . . . ? C12 C13 C14 C15 -0.3(2) . . . . ? C13 C14 C15 C16 -0.3(2) . . . . ? C14 C15 C16 C11 0.0(2) . . . . ? C16 C11 C12 C13 -1.3(2) . . . . ? C17 P1 O3 Li1 -3.6(3) . . . . ? C17 P1 C11 C12 -61.83(11) . . . . ? C17 P1 C11 C16 121.63(11) . . . . ? C17 P1 C23 P2 54.79(8) . . . . ? C17 C18 C19 C20 0.9(2) . . . . ? C18 C17 C22 C21 0.5(2) . . . . ? C18 C19 C20 C21 -0.5(2) . . . . ? C19 C20 C21 C22 0.1(2) . . . . ? C20 C21 C22 C17 -0.1(2) . . . . ? C22 C17 C18 C19 -0.90(18) . . . . ? C23 P1 O3 Li1 116.6(3) . . . . ? C23 P1 C11 C12 -174.62(10) . . . . ? C23 P1 C11 C16 8.84(13) . . . . ? C23 P1 C17 C18 -103.91(10) . . . . ? C23 P1 C17 C22 72.84(11) . . . . ? C23 P2 C24 C25 -54.42(12) . . . . ? C23 P2 C24 C29 126.94(11) . . . . ? C23 P2 C30 C31 -161.95(10) . . . . ? C23 P2 C30 C35 21.13(14) . . . . ? C24 P2 C23 P1 -87.66(8) . . . . ? C24 P2 C30 C31 84.63(11) . . . . ? C24 P2 C30 C35 -92.29(13) . . . . ? C24 C25 C26 C27 -0.6(2) . . . . ? C25 C24 C29 C28 1.9(2) . . . . ? C25 C26 C27 C28 1.9(3) . . . . ? C26 C27 C28 C29 -1.3(2) . . . . ? C27 C28 C29 C24 -0.6(2) . . . . ? C29 C24 C25 C26 -1.3(2) . . . . ? C30 P2 C23 P1 160.37(7) . . . . ? C30 P2 C24 C25 57.79(12) . . . . ? C30 P2 C24 C29 -120.85(11) . . . . ? C30 C31 C32 C33 0.3(2) . . . . ? C31 C30 C35 C34 -0.8(2) . . . . ? C31 C32 C33 C34 -1.7(3) . . . . ? C32 C33 C34 C35 1.9(3) . . . . ? C33 C34 C35 C30 -0.6(3) . . . . ? C35 C30 C31 C32 1.0(2) . . . . ? Li1 O1 C2 C1 -178.75(11) . . . . ? Li1 O1 C2 C3 -0.6(2) . . . . ? Li1 O2 C4 C3 6.6(2) . . . . ? Li1 O2 C4 C5 -175.33(12) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.0002 -1.9994 4.9984 -0.0341 -0.2510 -0.0699 0.0002 1.9994 -4.9984 0.0341 0.2510 0.0699 -5.0000 1.9989 1.9986 -0.0497 -0.1118 0.3287 5.0000 -1.9989 -1.9986 0.0497 0.1118 -0.3287 -0.0078 -5.0005 -0.9997 -0.3338 -0.0099 -0.0453 0.0078 5.0005 0.9997 0.3338 0.0099 0.0453