#------------------------------------------------------------------------------ #$Date: 2026-05-19 23:57:05 +0100 (Tue, 19 May 2026) $ #$Revision: 305999 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721039.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_7721039 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 'C36 H30 F3 Li O4 P2, 0.75(H2 O), 0.087(C1 H2 Cl2)' _chemical_formula_sum 'C36.08 H31.67 Cl0.18 F3 Li O4.75 P2' _chemical_formula_weight 673.39 _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 64.326(5) _cell_angle_beta 89.184(4) _cell_angle_gamma 65.971(5) _cell_formula_units_Z 2 _cell_length_a 12.5215(7) _cell_length_b 12.7280(6) _cell_length_c 13.3509(6) _cell_measurement_reflns_used 9173 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 76.2560 _cell_measurement_theta_min 3.7400 _cell_volume 1717.19(19) _computing_cell_refinement 'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro system (CCD 43.132a 64-bit (release 05-08-2024))' _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 n/a (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.5700 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.984 _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 -98.00 -62.00 0.50 5.00 -- -38.50 -19.00 -19.00 72 2 \w -75.00 40.00 0.50 5.00 -- -38.50 19.00 148.00 230 3 \w 88.00 121.00 0.50 5.00 -- 42.50 19.00 148.00 66 4 \w -4.00 22.00 0.50 5.00 -- 42.50 -19.00 -19.00 52 5 \w 33.00 87.00 0.50 20.00 -- 111.00 -19.00 -19.00 108 6 \w 76.00 129.00 0.50 20.00 -- 111.00 19.00 148.00 106 7 \w -86.00 -8.00 0.50 5.00 -- -38.50 125.00 150.00 156 8 \w 27.00 95.00 0.50 5.00 -- 42.50-125.00 60.00 136 9 \w 35.00 62.00 0.50 5.00 -- 42.50 38.00-180.00 54 10 \w 6.00 78.00 0.50 5.00 -- 42.50 -99.00 -90.00 144 11 \w 71.00 114.00 0.50 5.00 -- 42.50 38.00-180.00 86 12 \w 59.00 103.00 0.50 20.00 -- 111.00-125.00 30.00 88 13 \w 77.00 104.00 0.50 20.00 -- 111.00 -61.00 60.00 54 14 \w 72.00 107.00 0.50 20.00 -- 111.00 -94.00 30.00 70 15 \w 71.00 106.00 0.50 20.00 -- 111.00 -94.00 90.00 70 16 \w 49.00 76.00 0.50 20.00 -- 111.00 -15.00 90.00 54 17 \w 38.00 91.00 0.50 20.00 -- 111.00 -30.00 90.00 106 18 \w 112.00 139.00 0.50 20.00 -- 111.00 -77.00 -30.00 54 19 \w 32.00 107.00 0.50 20.00 -- 111.00 -94.00 150.00 150 20 \w 103.00 135.00 0.50 20.00 -- 111.00 -45.00-180.00 64 21 \w 43.00 122.00 0.50 20.00 -- 111.00 -45.00 0.00 158 22 \w 56.00 83.00 0.50 20.00 -- 111.00-125.00 0.00 54 23 \w 31.00 107.00 0.50 20.00 -- 111.00 -94.00 -90.00 152 24 \w 56.00 106.00 0.50 20.00 -- 111.00 -94.00-180.00 100 25 \w 31.00 156.00 0.50 20.00 -- 111.00 -15.00-150.00 250 26 \w 78.00 154.00 0.50 20.00 -- 111.00 -15.00 90.00 152 27 \w 105.00 132.00 0.50 20.00 -- 111.00 30.00 30.00 54 28 \w 40.00 71.00 0.50 20.00 -- 111.00 -45.00-180.00 62 29 \w 61.00 107.00 0.50 20.00 -- 111.00 -94.00 -60.00 92 30 \w 40.00 69.00 0.50 20.00 -- 111.00 -77.00 -30.00 58 31 \w 30.00 64.00 0.50 20.00 -- 111.00 -94.00 30.00 68 32 \w 78.00 106.00 0.50 20.00 -- 111.00 -94.00 0.00 56 33 \w 125.00 150.00 0.50 20.00 -- 111.00 45.00 -90.00 50 34 \w 31.00 107.00 0.50 20.00 -- 111.00 -94.00-150.00 152 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.1221580000 _diffrn_orient_matrix_UB_12 0.0852181000 _diffrn_orient_matrix_UB_13 0.0143463000 _diffrn_orient_matrix_UB_21 0.0559849000 _diffrn_orient_matrix_UB_22 0.0730818000 _diffrn_orient_matrix_UB_23 0.0297401000 _diffrn_orient_matrix_UB_31 -0.0286728000 _diffrn_orient_matrix_UB_32 0.0994264000 _diffrn_orient_matrix_UB_33 -0.1263454000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_unetI/netI 0.0416 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 17731 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.631 _diffrn_reflns_theta_min 3.747 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.754 _exptl_absorpt_correction_T_max 0.929 _exptl_absorpt_correction_T_min 0.736 _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 1.302 _exptl_crystal_description needle _exptl_crystal_F_000 698 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.973 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.064 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 455 _refine_ls_number_reflns 7105 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0498 _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^)+(0.0799P)^2^+0.6330P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1317 _refine_ls_wR_factor_ref 0.1378 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6306 _reflns_number_total 7105 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00738d2.cif _cod_data_source_block jjw1835 _cod_original_cell_volume 1717.20(17) _cod_database_code 7721039 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C36.1Cl0.2F3H31.7LiO4.8P2 _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 0.917 _shelx_estimated_absorpt_t_min 0.710 _reflns_odcompleteness_completeness 99.59 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 74.33 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All O(H,H) groups 2. Others Sof(Cl1)=Sof(Cl2)=Sof(C37)=Sof(H37A)=Sof(H37B)=FVAR(1) Fixed Sof: O5(0.75) H5A(0.75) H5B(0.75) 3.a Free rotating group: O5(H5A,H5B) 3.b Secondary CH2 refined with riding coordinates: C23(H23A,H23B), C36(H36A,H36B), C37(H37A,H37B) 3.c 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 jjw1835_a.res in P-1 jjw1835.res created by SHELXL-2018/3 at 09:19:03 on 12-Mar-2026 REM Old TITL jjw1835 in P-1 REM SHELXT solution in P-1: R1 0.133, Rweak 0.008, Alpha 0.050 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C36 Li3 O F7 P2 CELL 1.54184 12.5215 12.728 13.3509 64.326 89.184 65.971 ZERR 2 0.0007 0.0006 0.0006 0.005 0.004 0.005 LATT 1 SFAC C H Cl F Li O P UNIT 72.17 63.35 0.35 6 2 9.5 4 EQIV $1 1-X,1-Y,-Z L.S. 4 0 0 PLAN 6 SIZE 0.05 0.07 0.21 TEMP -173 CONF FREE Cl1 F1 FREE Cl2 Cl1_$1 FREE P2 Li1 FREE C2 Li1 BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.079900 0.633000 FVAR 6.05630 0.08691 P1 7 0.170209 0.400716 0.618131 11.00000 0.02233 0.02374 = 0.01923 -0.00928 0.00507 -0.01171 P2 7 0.562049 0.292486 0.552717 11.00000 0.02068 0.02175 = 0.02294 -0.01181 0.00533 -0.01013 F1 4 0.313907 0.707419 0.066592 11.00000 0.07911 0.06599 = 0.03723 -0.01455 0.01355 -0.05507 F2 4 0.159925 0.726042 -0.020201 11.00000 0.12232 0.06489 = 0.02461 0.00366 -0.01531 -0.07238 F3 4 0.143760 0.807907 0.092027 11.00000 0.09173 0.02904 = 0.06339 -0.00764 0.00589 -0.02002 O1 6 0.269476 0.563449 0.272021 11.00000 0.03638 0.02982 = 0.02249 -0.01221 0.00513 -0.01866 O2 6 0.243976 0.331245 0.347408 11.00000 0.04015 0.03260 = 0.02135 -0.00865 0.00188 -0.02237 O3 6 0.251146 0.415318 0.535297 11.00000 0.02796 0.03240 = 0.02408 -0.01459 0.00889 -0.01691 O4 6 0.483650 0.299013 0.464239 11.00000 0.02571 0.02937 = 0.02796 -0.01683 0.00532 -0.01267 C1 1 0.207826 0.705297 0.079268 11.00000 0.07012 0.03822 = 0.02845 -0.00725 -0.00275 -0.03524 C2 1 0.222759 0.578540 0.181803 11.00000 0.03854 0.02783 = 0.02132 -0.00806 0.00304 -0.01764 C3 1 0.186389 0.499384 0.160640 11.00000 0.05332 0.03440 = 0.02074 -0.01013 0.00299 -0.02723 AFIX 43 H3 2 0.149217 0.529479 0.085606 11.00000 -1.20000 AFIX 0 C4 1 0.202056 0.375815 0.245614 11.00000 0.02536 0.02729 = 0.02207 -0.01259 0.00782 -0.01350 C5 1 0.166893 0.292570 0.214101 11.00000 0.02963 0.02777 = 0.02475 -0.01414 0.00958 -0.01519 C6 1 0.169103 0.179579 0.301334 11.00000 0.02749 0.02686 = 0.02767 -0.01243 0.00826 -0.01282 AFIX 43 H6 2 0.193114 0.157347 0.377828 11.00000 -1.20000 AFIX 0 C7 1 0.136826 0.099172 0.278230 11.00000 0.03260 0.02546 = 0.03600 -0.01273 0.00900 -0.01487 AFIX 43 H7 2 0.136909 0.023651 0.338697 11.00000 -1.20000 AFIX 0 C8 1 0.104354 0.128941 0.166711 11.00000 0.04183 0.03607 = 0.04457 -0.02663 0.01422 -0.02260 AFIX 43 H8 2 0.082898 0.073587 0.150560 11.00000 -1.20000 AFIX 0 C9 1 0.103482 0.240013 0.079146 11.00000 0.06208 0.05021 = 0.03335 -0.02710 0.01706 -0.03641 AFIX 43 H9 2 0.082264 0.260141 0.002746 11.00000 -1.20000 AFIX 0 C10 1 0.133496 0.322360 0.102349 11.00000 0.05519 0.04082 = 0.02565 -0.01807 0.01429 -0.03209 AFIX 43 H10 2 0.131191 0.399118 0.041767 11.00000 -1.20000 AFIX 0 C11 1 0.182672 0.237901 0.685546 11.00000 0.02803 0.02603 = 0.02294 -0.00711 0.00048 -0.01327 C12 1 0.134512 0.195396 0.782375 11.00000 0.06159 0.04548 = 0.02426 -0.01445 0.01115 -0.03577 AFIX 43 H12 2 0.095725 0.251905 0.813908 11.00000 -1.20000 AFIX 0 C13 1 0.143854 0.070151 0.831927 11.00000 0.07726 0.05352 = 0.02627 -0.00714 0.00505 -0.04731 AFIX 43 H13 2 0.111188 0.040888 0.897431 11.00000 -1.20000 AFIX 0 C14 1 0.200525 -0.011801 0.786113 11.00000 0.05762 0.03156 = 0.04396 0.00002 -0.00983 -0.02577 AFIX 43 H14 2 0.207035 -0.097528 0.820669 11.00000 -1.20000 AFIX 0 C15 1 0.248098 0.029670 0.690117 11.00000 0.03726 0.02813 = 0.06343 -0.01863 0.00088 -0.01173 AFIX 43 H15 2 0.287262 -0.027386 0.659184 11.00000 -1.20000 AFIX 0 C16 1 0.238043 0.155416 0.639472 11.00000 0.02720 0.03061 = 0.04263 -0.01519 0.00682 -0.01358 AFIX 43 H16 2 0.269305 0.184796 0.572996 11.00000 -1.20000 AFIX 0 C17 1 0.204719 0.432139 0.729222 11.00000 0.02921 0.03136 = 0.02058 -0.01195 0.00830 -0.01794 C18 1 0.320572 0.354006 0.794501 11.00000 0.03275 0.04672 = 0.03013 -0.02141 0.00559 -0.01613 AFIX 43 H18 2 0.373459 0.282299 0.784336 11.00000 -1.20000 AFIX 0 C19 1 0.358349 0.380725 0.873669 11.00000 0.04087 0.05780 = 0.03256 -0.02283 0.00335 -0.02291 AFIX 43 H19 2 0.436976 0.327655 0.917765 11.00000 -1.20000 AFIX 0 C20 1 0.280394 0.485972 0.888392 11.00000 0.05641 0.05179 = 0.02674 -0.02123 0.01007 -0.03401 AFIX 43 H20 2 0.306582 0.505449 0.941757 11.00000 -1.20000 AFIX 0 C21 1 0.165226 0.562173 0.825825 11.00000 0.05279 0.03717 = 0.02876 -0.01875 0.01259 -0.02283 AFIX 43 H21 2 0.112098 0.632641 0.837426 11.00000 -1.20000 AFIX 0 C22 1 0.126931 0.535763 0.745730 11.00000 0.03649 0.03296 = 0.02500 -0.01419 0.00892 -0.01720 AFIX 43 H22 2 0.047895 0.588401 0.702514 11.00000 -1.20000 AFIX 0 C23 1 0.014899 0.508452 0.550933 11.00000 0.02300 0.02754 = 0.02503 -0.01245 0.00350 -0.00975 AFIX 23 H23A 2 -0.036452 0.487947 0.606068 11.00000 -1.20000 H23B 2 -0.000530 0.599831 0.525043 11.00000 -1.20000 AFIX 0 C24 1 0.575818 0.169356 0.693076 11.00000 0.02212 0.02315 = 0.02649 -0.01055 0.00671 -0.01024 C25 1 0.618862 0.168472 0.789349 11.00000 0.03043 0.03024 = 0.02926 -0.01148 0.00458 -0.01457 AFIX 43 H25 2 0.640317 0.234651 0.781896 11.00000 -1.20000 AFIX 0 C26 1 0.630258 0.070451 0.896212 11.00000 0.03785 0.03929 = 0.02666 -0.00879 0.00261 -0.01656 AFIX 43 H26 2 0.659384 0.069461 0.962090 11.00000 -1.20000 AFIX 0 C27 1 0.598842 -0.026253 0.906359 11.00000 0.04246 0.03539 = 0.03394 -0.00634 0.01094 -0.01881 AFIX 43 H27 2 0.606905 -0.093392 0.979440 11.00000 -1.20000 AFIX 0 C28 1 0.556264 -0.025536 0.811655 11.00000 0.04406 0.03251 = 0.04445 -0.01416 0.01603 -0.02390 AFIX 43 H28 2 0.535009 -0.091986 0.819557 11.00000 -1.20000 AFIX 0 C29 1 0.544217 0.072187 0.704315 11.00000 0.03102 0.03112 = 0.03453 -0.01642 0.01031 -0.01729 AFIX 43 H29 2 0.514573 0.072774 0.638873 11.00000 -1.20000 AFIX 0 C30 1 0.711495 0.252062 0.525455 11.00000 0.02192 0.01973 = 0.02478 -0.00957 0.00693 -0.00938 C31 1 0.741312 0.212981 0.441826 11.00000 0.02814 0.02920 = 0.02396 -0.01203 0.00640 -0.01359 AFIX 43 H31 2 0.681756 0.216084 0.395848 11.00000 -1.20000 AFIX 0 C32 1 0.858231 0.169619 0.426176 11.00000 0.03568 0.03588 = 0.02923 -0.01772 0.01526 -0.01714 AFIX 43 H32 2 0.878679 0.142947 0.369381 11.00000 -1.20000 AFIX 0 C33 1 0.945178 0.165056 0.492930 11.00000 0.02637 0.03057 = 0.03676 -0.01359 0.01373 -0.01394 AFIX 43 H33 2 1.025307 0.133866 0.482589 11.00000 -1.20000 AFIX 0 C34 1 0.915996 0.205794 0.574937 11.00000 0.02498 0.02860 = 0.03573 -0.01383 0.00625 -0.01493 AFIX 43 H34 2 0.975792 0.203487 0.619966 11.00000 -1.20000 AFIX 0 C35 1 0.798588 0.250127 0.591012 11.00000 0.02711 0.02540 = 0.03150 -0.01508 0.00795 -0.01282 AFIX 43 H35 2 0.778049 0.278927 0.646504 11.00000 -1.20000 AFIX 0 C36 1 0.508109 0.444178 0.558546 11.00000 0.02308 0.02222 = 0.02322 -0.01204 0.00614 -0.00962 AFIX 23 H36A 2 0.430926 0.462727 0.584044 11.00000 -1.20000 H36B 2 0.565631 0.437113 0.614019 11.00000 -1.20000 AFIX 0 LI1 5 0.313030 0.403133 0.410050 11.00000 0.02709 0.03003 = 0.02404 -0.01259 0.00578 -0.01562 AFIX 6 O5 6 0.505732 0.106544 0.402089 10.75000 0.09000 0.04240 = 0.07824 -0.03761 -0.01532 -0.02054 H5A 2 0.492609 0.168283 0.420061 10.75000 -1.50000 H5B 2 0.570583 0.041475 0.449267 10.75000 -1.50000 AFIX 0 CL1 3 0.434223 0.579221 0.038274 21.00000 0.05710 0.06084 = 0.05967 -0.00297 -0.01549 -0.03658 CL2 3 0.556169 0.299035 0.157541 21.00000 0.10109 0.05103 = 0.07543 -0.03787 -0.01896 -0.00733 C37 1 0.495706 0.438386 0.168014 21.00000 0.03234 0.04463 = 0.05214 -0.01820 0.01258 -0.01246 AFIX 23 H37A 2 0.558185 0.441815 0.209391 21.00000 -1.20000 H37B 2 0.432744 0.436611 0.213517 21.00000 -1.20000 AFIX 0 HKLF 4 REM jjw1835_a.res in P-1 REM wR2 = 0.1378, GooF = S = 1.036, Restrained GooF = 1.036 for all data REM R1 = 0.0498 for 6306 Fo > 4sig(Fo) and 0.0559 for all 7105 data REM 455 parameters refined using 0 restraints END WGHT 0.0799 0.6330 REM Highest difference peak 0.973, deepest hole -0.360, 1-sigma level 0.064 Q1 1 0.0355 0.8171 0.0848 11.00000 0.05 0.97 Q2 1 0.2305 0.7772 0.0826 11.00000 0.05 0.64 Q3 1 0.2175 0.3983 0.5704 11.00000 0.05 0.42 Q4 1 0.1724 0.4161 0.6756 11.00000 0.05 0.41 Q5 1 0.5567 0.0765 0.4162 11.00000 0.05 0.38 Q6 1 0.7204 0.2217 0.4999 11.00000 0.05 0.37 ; _shelx_res_checksum 17568 _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 2.049 _oxdiff_exptl_absorpt_empirical_full_min 0.425 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 0.17021(4) 0.40072(4) 0.61813(3) 0.02154(12) Uani 1 1 d . . . . . P2 P 0.56205(4) 0.29249(4) 0.55272(4) 0.02100(12) Uani 1 1 d . . . . . F1 F 0.31391(16) 0.70742(17) 0.06659(12) 0.0561(4) Uani 1 1 d . . . . . F2 F 0.15993(19) 0.72604(17) -0.02020(11) 0.0687(6) Uani 1 1 d . . . . . F3 F 0.14376(19) 0.80791(15) 0.09203(15) 0.0695(5) Uani 1 1 d . . . . . O1 O 0.26948(13) 0.56345(13) 0.27202(11) 0.0281(3) Uani 1 1 d . . . . . O2 O 0.24398(13) 0.33124(14) 0.34741(11) 0.0306(3) Uani 1 1 d . . . . . O3 O 0.25115(12) 0.41532(13) 0.53530(11) 0.0263(3) Uani 1 1 d . . . . . O4 O 0.48365(11) 0.29901(13) 0.46424(11) 0.0261(3) Uani 1 1 d . . . . . C1 C 0.2078(3) 0.7053(2) 0.07927(19) 0.0446(6) Uani 1 1 d . . . . . C2 C 0.22276(19) 0.57854(19) 0.18180(15) 0.0295(4) Uani 1 1 d . . . . . C3 C 0.1864(2) 0.4994(2) 0.16064(16) 0.0343(4) Uani 1 1 d . . . . . H3 H 0.149217 0.529479 0.085606 0.041 Uiso 1 1 calc R U . . . C4 C 0.20206(16) 0.37582(18) 0.24561(15) 0.0239(3) Uani 1 1 d . . . . . C5 C 0.16689(17) 0.29257(18) 0.21410(15) 0.0258(4) Uani 1 1 d . . . . . C6 C 0.16910(17) 0.17958(19) 0.30133(16) 0.0272(4) Uani 1 1 d . . . . . H6 H 0.193114 0.157347 0.377828 0.033 Uiso 1 1 calc R U . . . C7 C 0.13683(18) 0.09917(19) 0.27823(17) 0.0313(4) Uani 1 1 d . . . . . H7 H 0.136909 0.023651 0.338697 0.038 Uiso 1 1 calc R U . . . C8 C 0.1044(2) 0.1289(2) 0.16671(19) 0.0358(4) Uani 1 1 d . . . . . H8 H 0.082898 0.073587 0.150560 0.043 Uiso 1 1 calc R U . . . C9 C 0.1035(2) 0.2400(2) 0.07915(19) 0.0413(5) Uani 1 1 d . . . . . H9 H 0.082264 0.260141 0.002746 0.050 Uiso 1 1 calc R U . . . C10 C 0.1335(2) 0.3224(2) 0.10235(17) 0.0356(5) Uani 1 1 d . . . . . H10 H 0.131191 0.399118 0.041767 0.043 Uiso 1 1 calc R U . . . C11 C 0.18267(17) 0.23790(18) 0.68555(15) 0.0269(4) Uani 1 1 d . . . . . C12 C 0.1345(2) 0.1954(2) 0.78237(17) 0.0401(5) Uani 1 1 d . . . . . H12 H 0.095725 0.251905 0.813908 0.048 Uiso 1 1 calc R U . . . C13 C 0.1439(3) 0.0702(3) 0.83193(19) 0.0501(6) Uani 1 1 d . . . . . H13 H 0.111188 0.040888 0.897431 0.060 Uiso 1 1 calc R U . . . C14 C 0.2005(2) -0.0118(2) 0.7861(2) 0.0491(6) Uani 1 1 d . . . . . H14 H 0.207035 -0.097528 0.820669 0.059 Uiso 1 1 calc R U . . . C15 C 0.2481(2) 0.0297(2) 0.6901(2) 0.0450(5) Uani 1 1 d . . . . . H15 H 0.287262 -0.027386 0.659184 0.054 Uiso 1 1 calc R U . . . C16 C 0.23804(18) 0.1554(2) 0.63947(19) 0.0340(4) Uani 1 1 d . . . . . H16 H 0.269305 0.184796 0.572996 0.041 Uiso 1 1 calc R U . . . C17 C 0.20472(17) 0.43214(19) 0.72922(15) 0.0255(4) Uani 1 1 d . . . . . C18 C 0.32057(19) 0.3540(2) 0.79450(17) 0.0357(4) Uani 1 1 d . . . . . H18 H 0.373459 0.282299 0.784336 0.043 Uiso 1 1 calc R U . . . C19 C 0.3583(2) 0.3807(3) 0.87367(19) 0.0427(5) Uani 1 1 d . . . . . H19 H 0.436976 0.327655 0.917765 0.051 Uiso 1 1 calc R U . . . C20 C 0.2804(2) 0.4860(2) 0.88839(18) 0.0401(5) Uani 1 1 d . . . . . H20 H 0.306582 0.505449 0.941757 0.048 Uiso 1 1 calc R U . . . C21 C 0.1652(2) 0.5622(2) 0.82582(17) 0.0372(5) Uani 1 1 d . . . . . H21 H 0.112098 0.632641 0.837426 0.045 Uiso 1 1 calc R U . . . C22 C 0.12693(19) 0.5358(2) 0.74573(16) 0.0306(4) Uani 1 1 d . . . . . H22 H 0.047895 0.588401 0.702514 0.037 Uiso 1 1 calc R U . . . C23 C 0.01490(16) 0.50845(18) 0.55093(15) 0.0257(4) Uani 1 1 d . . . . . H23A H -0.036452 0.487947 0.606068 0.031 Uiso 1 1 calc R U . . . H23B H -0.000530 0.599831 0.525043 0.031 Uiso 1 1 calc R U . . . C24 C 0.57582(16) 0.16936(17) 0.69308(15) 0.0243(3) Uani 1 1 d . . . . . C25 C 0.61886(18) 0.1685(2) 0.78935(16) 0.0305(4) Uani 1 1 d . . . . . H25 H 0.640317 0.234651 0.781896 0.037 Uiso 1 1 calc R U . . . C26 C 0.6303(2) 0.0705(2) 0.89621(18) 0.0375(5) Uani 1 1 d . . . . . H26 H 0.659384 0.069461 0.962090 0.045 Uiso 1 1 calc R U . . . C27 C 0.5988(2) -0.0263(2) 0.90636(19) 0.0408(5) Uani 1 1 d . . . . . H27 H 0.606905 -0.093392 0.979440 0.049 Uiso 1 1 calc R U . . . C28 C 0.5563(2) -0.0255(2) 0.8117(2) 0.0394(5) Uani 1 1 d . . . . . H28 H 0.535009 -0.091986 0.819557 0.047 Uiso 1 1 calc R U . . . C29 C 0.54422(18) 0.0722(2) 0.70431(17) 0.0305(4) Uani 1 1 d . . . . . H29 H 0.514573 0.072774 0.638873 0.037 Uiso 1 1 calc R U . . . C30 C 0.71149(15) 0.25206(17) 0.52545(15) 0.0225(3) Uani 1 1 d . . . . . C31 C 0.74131(17) 0.21298(19) 0.44183(15) 0.0270(4) Uani 1 1 d . . . . . H31 H 0.681756 0.216084 0.395848 0.032 Uiso 1 1 calc R U . . . C32 C 0.85823(19) 0.1696(2) 0.42618(17) 0.0322(4) Uani 1 1 d . . . . . H32 H 0.878679 0.142947 0.369381 0.039 Uiso 1 1 calc R U . . . C33 C 0.94518(18) 0.1651(2) 0.49293(17) 0.0317(4) Uani 1 1 d . . . . . H33 H 1.025307 0.133866 0.482589 0.038 Uiso 1 1 calc R U . . . C34 C 0.91600(17) 0.20579(19) 0.57494(17) 0.0291(4) Uani 1 1 d . . . . . H34 H 0.975792 0.203487 0.619966 0.035 Uiso 1 1 calc R U . . . C35 C 0.79859(17) 0.25013(18) 0.59101(16) 0.0269(4) Uani 1 1 d . . . . . H35 H 0.778049 0.278927 0.646504 0.032 Uiso 1 1 calc R U . . . C36 C 0.50811(16) 0.44418(16) 0.55855(14) 0.0225(3) Uani 1 1 d . . . . . H36A H 0.430926 0.462727 0.584044 0.027 Uiso 1 1 calc R U . . . H36B H 0.565631 0.437113 0.614019 0.027 Uiso 1 1 calc R U . . . Li1 Li 0.3130(3) 0.4031(3) 0.4100(3) 0.0260(6) Uani 1 1 d . . . . . O5 O 0.5057(3) 0.1065(3) 0.4021(3) 0.0694(8) Uani 0.75 1 d G . P . . H5A H 0.492609 0.168283 0.420061 0.104 Uiso 0.75 1 d G U P . . H5B H 0.570583 0.041475 0.449267 0.104 Uiso 0.75 1 d G U P . . Cl1 Cl 0.4342(8) 0.5792(9) 0.0383(7) 0.065(3) Uani 0.087(2) 1 d . . P . . Cl2 Cl 0.5562(11) 0.2990(9) 0.1575(9) 0.082(4) Uani 0.087(2) 1 d . . P . . C37 C 0.496(2) 0.438(3) 0.168(3) 0.047(7) Uani 0.087(2) 1 d . . P . . H37A H 0.558185 0.441815 0.209391 0.056 Uiso 0.087(2) 1 calc R U P . . H37B H 0.432744 0.436611 0.213517 0.056 Uiso 0.087(2) 1 calc R U P . . 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 0.0223(2) 0.0237(2) 0.0192(2) -0.00928(17) 0.00507(16) -0.01171(17) P2 0.0207(2) 0.0218(2) 0.0229(2) -0.01181(17) 0.00533(16) -0.01013(17) F1 0.0791(11) 0.0660(10) 0.0372(7) -0.0145(7) 0.0136(7) -0.0551(9) F2 0.1223(15) 0.0649(10) 0.0246(6) 0.0037(6) -0.0153(7) -0.0724(11) F3 0.0917(14) 0.0290(8) 0.0634(10) -0.0076(7) 0.0059(9) -0.0200(8) O1 0.0364(7) 0.0298(7) 0.0225(6) -0.0122(5) 0.0051(5) -0.0187(6) O2 0.0402(8) 0.0326(7) 0.0214(6) -0.0087(5) 0.0019(5) -0.0224(6) O3 0.0280(6) 0.0324(7) 0.0241(6) -0.0146(5) 0.0089(5) -0.0169(6) O4 0.0257(6) 0.0294(7) 0.0280(6) -0.0168(5) 0.0053(5) -0.0127(5) C1 0.0701(16) 0.0382(12) 0.0285(10) -0.0073(9) -0.0028(10) -0.0352(12) C2 0.0385(10) 0.0278(9) 0.0213(8) -0.0081(7) 0.0030(7) -0.0176(8) C3 0.0533(13) 0.0344(10) 0.0207(8) -0.0101(8) 0.0030(8) -0.0272(10) C4 0.0254(8) 0.0273(9) 0.0221(8) -0.0126(7) 0.0078(6) -0.0135(7) C5 0.0296(9) 0.0278(9) 0.0247(8) -0.0141(7) 0.0096(7) -0.0152(7) C6 0.0275(9) 0.0269(9) 0.0277(9) -0.0124(7) 0.0083(7) -0.0128(7) C7 0.0326(10) 0.0255(9) 0.0360(10) -0.0127(8) 0.0090(8) -0.0149(8) C8 0.0418(11) 0.0361(11) 0.0446(11) -0.0266(9) 0.0142(9) -0.0226(9) C9 0.0621(15) 0.0502(13) 0.0333(10) -0.0271(10) 0.0171(10) -0.0364(12) C10 0.0552(13) 0.0408(11) 0.0256(9) -0.0181(8) 0.0143(9) -0.0321(10) C11 0.0280(9) 0.0260(9) 0.0229(8) -0.0071(7) 0.0005(7) -0.0133(7) C12 0.0616(14) 0.0455(12) 0.0243(9) -0.0145(9) 0.0111(9) -0.0358(11) C13 0.0773(18) 0.0535(15) 0.0263(10) -0.0071(10) 0.0051(10) -0.0473(14) C14 0.0576(15) 0.0316(11) 0.0440(12) 0.0000(9) -0.0098(11) -0.0258(11) C15 0.0373(12) 0.0281(11) 0.0634(15) -0.0186(10) 0.0009(10) -0.0117(9) C16 0.0272(10) 0.0306(10) 0.0426(11) -0.0152(8) 0.0068(8) -0.0136(8) C17 0.0292(9) 0.0314(9) 0.0206(8) -0.0120(7) 0.0083(7) -0.0179(8) C18 0.0327(10) 0.0467(12) 0.0301(9) -0.0214(9) 0.0056(8) -0.0161(9) C19 0.0409(12) 0.0578(14) 0.0326(10) -0.0228(10) 0.0033(9) -0.0229(11) C20 0.0564(14) 0.0518(13) 0.0267(9) -0.0212(9) 0.0101(9) -0.0340(12) C21 0.0528(13) 0.0372(11) 0.0288(9) -0.0188(8) 0.0126(9) -0.0228(10) C22 0.0365(10) 0.0330(10) 0.0250(8) -0.0142(8) 0.0089(7) -0.0172(8) C23 0.0230(8) 0.0275(9) 0.0250(8) -0.0124(7) 0.0035(7) -0.0097(7) C24 0.0221(8) 0.0232(8) 0.0265(8) -0.0105(7) 0.0067(6) -0.0102(7) C25 0.0304(10) 0.0302(10) 0.0293(9) -0.0115(8) 0.0046(7) -0.0146(8) C26 0.0379(11) 0.0393(11) 0.0267(9) -0.0088(8) 0.0026(8) -0.0166(9) C27 0.0425(12) 0.0354(11) 0.0339(10) -0.0063(9) 0.0109(9) -0.0188(10) C28 0.0441(12) 0.0325(11) 0.0444(12) -0.0142(9) 0.0160(10) -0.0239(10) C29 0.0310(10) 0.0311(10) 0.0345(10) -0.0164(8) 0.0103(8) -0.0173(8) C30 0.0219(8) 0.0197(8) 0.0248(8) -0.0096(6) 0.0069(6) -0.0094(7) C31 0.0281(9) 0.0292(9) 0.0240(8) -0.0120(7) 0.0064(7) -0.0136(8) C32 0.0357(11) 0.0359(10) 0.0292(9) -0.0177(8) 0.0153(8) -0.0171(9) C33 0.0264(9) 0.0306(10) 0.0368(10) -0.0136(8) 0.0137(8) -0.0139(8) C34 0.0250(9) 0.0286(9) 0.0357(9) -0.0138(8) 0.0062(7) -0.0149(8) C35 0.0271(9) 0.0254(9) 0.0315(9) -0.0151(7) 0.0079(7) -0.0128(7) C36 0.0231(8) 0.0222(8) 0.0232(8) -0.0120(7) 0.0061(6) -0.0096(7) Li1 0.0271(15) 0.0300(16) 0.0240(14) -0.0126(12) 0.0058(11) -0.0156(13) O5 0.090(2) 0.0424(14) 0.0782(19) -0.0376(14) -0.0153(16) -0.0205(14) Cl1 0.057(5) 0.061(5) 0.060(5) -0.003(4) -0.015(3) -0.037(4) Cl2 0.101(8) 0.051(5) 0.075(6) -0.038(4) -0.019(5) -0.007(5) C37 0.032(13) 0.045(15) 0.052(15) -0.018(12) 0.013(11) -0.012(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 0.0243 0 2 -5 0.0243 -5 -2 -1 0.0963 5 2 1 0.0963 0 -5 -3 0.0258 0 5 3 0.0258 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 111.57(8) . . ? O3 P1 C17 111.64(8) . . ? O3 P1 C23 112.10(8) . . ? C11 P1 C23 106.20(9) . . ? C17 P1 C11 106.75(9) . . ? C17 P1 C23 108.28(9) . . ? O4 P2 C24 112.67(8) . . ? O4 P2 C30 110.71(8) . . ? O4 P2 C36 112.57(8) . . ? C24 P2 C30 106.17(8) . . ? C24 P2 C36 106.69(8) . . ? C36 P2 C30 107.68(8) . . ? C2 O1 Li1 120.13(15) . . ? C4 O2 Li1 126.92(16) . . ? P1 O3 Li1 153.54(13) . . ? P2 O4 Li1 128.35(12) . . ? F1 C1 C2 110.9(2) . . ? F2 C1 F1 105.7(2) . . ? F2 C1 C2 115.17(18) . . ? F3 C1 F1 104.8(2) . . ? F3 C1 F2 107.4(2) . . ? F3 C1 C2 112.1(2) . . ? O1 C2 C1 112.31(17) . . ? O1 C2 C3 130.71(18) . . ? C3 C2 C1 116.95(17) . . ? C2 C3 H3 118.4 . . ? C2 C3 C4 123.13(18) . . ? C4 C3 H3 118.4 . . ? O2 C4 C3 123.03(17) . . ? O2 C4 C5 117.24(16) . . ? C3 C4 C5 119.73(16) . . ? C6 C5 C4 118.09(16) . . ? C6 C5 C10 118.66(18) . . ? C10 C5 C4 123.25(17) . . ? C5 C6 H6 119.5 . . ? C7 C6 C5 121.03(18) . . ? C7 C6 H6 119.5 . . ? C6 C7 H7 120.0 . . ? C6 C7 C8 120.02(18) . . ? C8 C7 H7 120.0 . . ? C7 C8 H8 120.2 . . ? C9 C8 C7 119.51(19) . . ? C9 C8 H8 120.2 . . ? C8 C9 H9 119.8 . . ? C8 C9 C10 120.5(2) . . ? C10 C9 H9 119.8 . . ? C5 C10 H10 119.9 . . ? C9 C10 C5 120.27(19) . . ? C9 C10 H10 119.9 . . ? C12 C11 P1 120.64(16) . . ? C16 C11 P1 119.49(14) . . ? C16 C11 C12 119.86(19) . . ? C11 C12 H12 120.2 . . ? C13 C12 C11 119.6(2) . . ? C13 C12 H12 120.2 . . ? C12 C13 H13 120.0 . . ? C14 C13 C12 120.1(2) . . ? C14 C13 H13 120.0 . . ? C13 C14 H14 119.7 . . ? C13 C14 C15 120.7(2) . . ? C15 C14 H14 119.7 . . ? C14 C15 H15 120.2 . . ? C14 C15 C16 119.5(2) . . ? C16 C15 H15 120.2 . . ? C11 C16 C15 120.3(2) . . ? C11 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 P1 116.74(15) . . ? C22 C17 P1 123.37(15) . . ? C22 C17 C18 119.62(18) . . ? C17 C18 H18 119.8 . . ? C19 C18 C17 120.3(2) . . ? C19 C18 H18 119.8 . . ? C18 C19 H19 120.2 . . ? C18 C19 C20 119.6(2) . . ? C20 C19 H19 120.2 . . ? C19 C20 H20 119.8 . . ? C21 C20 C19 120.4(2) . . ? C21 C20 H20 119.8 . . ? C20 C21 H21 119.9 . . ? C20 C21 C22 120.1(2) . . ? C22 C21 H21 119.9 . . ? C17 C22 C21 119.9(2) . . ? C17 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? P1 C23 H23A 109.8 . . ? P1 C23 H23B 109.8 . . ? C23 C23 P1 109.51(16) 2_566 . ? C23 C23 H23A 109.8 2_566 . ? C23 C23 H23B 109.8 2_566 . ? H23A C23 H23B 108.2 . . ? C25 C24 P2 121.45(14) . . ? C25 C24 C29 119.97(17) . . ? C29 C24 P2 118.57(15) . . ? C24 C25 H25 120.1 . . ? C26 C25 C24 119.77(19) . . ? C26 C25 H25 120.1 . . ? C25 C26 H26 120.1 . . ? C25 C26 C27 119.7(2) . . ? C27 C26 H26 120.1 . . ? C26 C27 H27 119.7 . . ? C28 C27 C26 120.61(19) . . ? C28 C27 H27 119.7 . . ? C27 C28 H28 119.9 . . ? C27 C28 C29 120.2(2) . . ? C29 C28 H28 119.9 . . ? C24 C29 H29 120.1 . . ? C28 C29 C24 119.7(2) . . ? C28 C29 H29 120.1 . . ? C31 C30 P2 118.40(14) . . ? C35 C30 P2 121.49(13) . . ? C35 C30 C31 119.94(16) . . ? C30 C31 H31 120.1 . . ? C32 C31 C30 119.74(18) . . ? C32 C31 H31 120.1 . . ? C31 C32 H32 119.9 . . ? C33 C32 C31 120.28(18) . . ? C33 C32 H32 119.9 . . ? C32 C33 H33 119.8 . . ? C32 C33 C34 120.38(18) . . ? C34 C33 H33 119.8 . . ? C33 C34 H34 120.1 . . ? C33 C34 C35 119.79(18) . . ? C35 C34 H34 120.1 . . ? C30 C35 C34 119.83(17) . . ? C30 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? P2 C36 H36A 109.6 . . ? P2 C36 H36B 109.6 . . ? C36 C36 P2 110.37(15) 2_666 . ? C36 C36 H36A 109.6 2_666 . ? C36 C36 H36B 109.6 2_666 . ? H36A C36 H36B 108.1 . . ? O1 Li1 O4 113.62(16) . . ? O2 Li1 O1 95.46(15) . . ? O2 Li1 O4 112.52(17) . . ? O3 Li1 O1 117.32(18) . . ? O3 Li1 O2 112.57(16) . . ? O3 Li1 O4 105.45(16) . . ? H5A O5 H5B 104.4 . . ? C37 Cl1 Cl2 149.8(11) . 2_665 ? Cl1 C37 H37A 108.7 . . ? Cl1 C37 H37B 108.7 . . ? Cl2 C37 Cl1 114.2(18) . . ? Cl2 C37 H37A 108.7 . . ? Cl2 C37 H37B 108.7 . . ? H37A C37 H37B 107.6 . . ? 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 1.4927(12) . ? P1 C11 1.8037(19) . ? P1 C17 1.7943(19) . ? P1 C23 1.8108(18) . ? P2 O4 1.4992(13) . ? P2 C24 1.8005(18) . ? P2 C30 1.8049(17) . ? P2 C36 1.8046(17) . ? F1 C1 1.346(3) . ? F2 C1 1.335(3) . ? F3 C1 1.309(3) . ? O1 C2 1.248(2) . ? O1 Li1 1.929(3) . ? O2 C4 1.247(2) . ? O2 Li1 1.901(3) . ? O3 Li1 1.874(3) . ? O4 Li1 1.937(3) . ? C1 C2 1.536(3) . ? C2 C3 1.388(3) . ? C3 H3 0.9500 . ? C3 C4 1.417(3) . ? C4 C5 1.505(2) . ? C5 C6 1.394(3) . ? C5 C10 1.394(3) . ? C6 H6 0.9500 . ? C6 C7 1.386(3) . ? C7 H7 0.9500 . ? C7 C8 1.389(3) . ? C8 H8 0.9500 . ? C8 C9 1.386(3) . ? C9 H9 0.9500 . ? C9 C10 1.393(3) . ? C10 H10 0.9500 . ? C11 C12 1.402(3) . ? C11 C16 1.384(3) . ? C12 H12 0.9500 . ? C12 C13 1.389(3) . ? C13 H13 0.9500 . ? C13 C14 1.380(4) . ? C14 H14 0.9500 . ? C14 C15 1.387(4) . ? C15 H15 0.9500 . ? C15 C16 1.391(3) . ? C16 H16 0.9500 . ? C17 C18 1.401(3) . ? C17 C22 1.392(3) . ? C18 H18 0.9500 . ? C18 C19 1.383(3) . ? C19 H19 0.9500 . ? C19 C20 1.394(4) . ? C20 H20 0.9500 . ? C20 C21 1.382(4) . ? C21 H21 0.9500 . ? C21 C22 1.394(3) . ? C22 H22 0.9500 . ? C23 C23 1.539(3) 2_566 ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.395(3) . ? C24 C29 1.395(3) . ? C25 H25 0.9500 . ? C25 C26 1.390(3) . ? C26 H26 0.9500 . ? C26 C27 1.392(3) . ? C27 H27 0.9500 . ? C27 C28 1.374(3) . ? C28 H28 0.9500 . ? C28 C29 1.390(3) . ? C29 H29 0.9500 . ? C30 C31 1.397(3) . ? C30 C35 1.394(3) . ? C31 H31 0.9500 . ? C31 C32 1.387(3) . ? C32 H32 0.9500 . ? C32 C33 1.384(3) . ? C33 H33 0.9500 . ? C33 C34 1.388(3) . ? C34 H34 0.9500 . ? C34 C35 1.395(3) . ? C35 H35 0.9500 . ? C36 C36 1.534(3) 2_666 ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? O5 H5A 0.8713 . ? O5 H5B 0.8700 . ? Cl1 Cl2 2.425(15) 2_665 ? Cl1 C37 1.74(3) . ? Cl2 C37 1.69(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? 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 O3 Li1 O1 107.3(3) . . . . ? P1 O3 Li1 O2 -2.1(4) . . . . ? P1 O3 Li1 O4 -125.1(3) . . . . ? P1 C11 C12 C13 179.16(19) . . . . ? P1 C11 C16 C15 -179.78(17) . . . . ? P1 C17 C18 C19 173.10(17) . . . . ? P1 C17 C22 C21 -172.88(15) . . . . ? P2 C24 C25 C26 -178.82(16) . . . . ? P2 C24 C29 C28 178.71(16) . . . . ? P2 C30 C31 C32 -173.97(15) . . . . ? P2 C30 C35 C34 173.53(14) . . . . ? F1 C1 C2 O1 59.0(3) . . . . ? F1 C1 C2 C3 -119.5(2) . . . . ? F2 C1 C2 O1 179.0(2) . . . . ? F2 C1 C2 C3 0.5(3) . . . . ? F3 C1 C2 O1 -57.7(3) . . . . ? F3 C1 C2 C3 123.8(2) . . . . ? O1 C2 C3 C4 -2.5(4) . . . . ? O2 C4 C5 C6 7.9(3) . . . . ? O2 C4 C5 C10 -171.47(19) . . . . ? O3 P1 C11 C12 166.33(16) . . . . ? O3 P1 C11 C16 -15.13(19) . . . . ? O3 P1 C17 C18 -58.61(17) . . . . ? O3 P1 C17 C22 115.32(16) . . . . ? O3 P1 C23 C23 51.92(19) . . . 2_566 ? O4 P2 C24 C25 -163.76(15) . . . . ? O4 P2 C24 C29 17.29(17) . . . . ? O4 P2 C30 C31 -9.69(17) . . . . ? O4 P2 C30 C35 174.97(14) . . . . ? O4 P2 C36 C36 -55.14(18) . . . 2_666 ? C1 C2 C3 C4 175.7(2) . . . . ? C2 C3 C4 O2 4.0(3) . . . . ? C2 C3 C4 C5 -176.25(19) . . . . ? C3 C4 C5 C6 -171.90(18) . . . . ? C3 C4 C5 C10 8.7(3) . . . . ? C4 C5 C6 C7 179.45(17) . . . . ? C4 C5 C10 C9 179.1(2) . . . . ? C5 C6 C7 C8 1.6(3) . . . . ? C6 C5 C10 C9 -0.2(3) . . . . ? C6 C7 C8 C9 -0.6(3) . . . . ? C7 C8 C9 C10 -0.8(4) . . . . ? C8 C9 C10 C5 1.2(4) . . . . ? C10 C5 C6 C7 -1.1(3) . . . . ? C11 P1 O3 Li1 53.5(3) . . . . ? C11 P1 C17 C18 63.56(17) . . . . ? C11 P1 C17 C22 -122.51(16) . . . . ? C11 P1 C23 C23 -70.16(18) . . . 2_566 ? C11 C12 C13 C14 0.2(4) . . . . ? C12 C11 C16 C15 -1.2(3) . . . . ? C12 C13 C14 C15 -0.4(4) . . . . ? C13 C14 C15 C16 -0.2(4) . . . . ? C14 C15 C16 C11 1.0(3) . . . . ? C16 C11 C12 C13 0.6(3) . . . . ? C17 P1 O3 Li1 172.9(3) . . . . ? C17 P1 C11 C12 44.11(19) . . . . ? C17 P1 C11 C16 -137.35(16) . . . . ? C17 P1 C23 C23 175.51(16) . . . 2_566 ? C17 C18 C19 C20 0.1(3) . . . . ? C18 C17 C22 C21 0.9(3) . . . . ? C18 C19 C20 C21 1.1(3) . . . . ? C19 C20 C21 C22 -1.3(3) . . . . ? C20 C21 C22 C17 0.3(3) . . . . ? C22 C17 C18 C19 -1.1(3) . . . . ? C23 P1 O3 Li1 -65.5(3) . . . . ? C23 P1 C11 C12 -71.26(18) . . . . ? C23 P1 C11 C16 107.29(16) . . . . ? C23 P1 C17 C18 177.53(15) . . . . ? C23 P1 C17 C22 -8.55(18) . . . . ? C24 P2 O4 Li1 90.05(16) . . . . ? C24 P2 C30 C31 112.90(15) . . . . ? C24 P2 C30 C35 -62.44(17) . . . . ? C24 P2 C36 C36 -179.21(16) . . . 2_666 ? C24 C25 C26 C27 0.1(3) . . . . ? C25 C24 C29 C28 -0.3(3) . . . . ? C25 C26 C27 C28 -0.2(3) . . . . ? C26 C27 C28 C29 0.1(3) . . . . ? C27 C28 C29 C24 0.2(3) . . . . ? C29 C24 C25 C26 0.1(3) . . . . ? C30 P2 O4 Li1 -151.23(15) . . . . ? C30 P2 C24 C25 74.89(17) . . . . ? C30 P2 C24 C29 -104.05(16) . . . . ? C30 P2 C36 C36 67.17(18) . . . 2_666 ? C30 C31 C32 C33 0.0(3) . . . . ? C31 C30 C35 C34 -1.7(3) . . . . ? C31 C32 C33 C34 -1.1(3) . . . . ? C32 C33 C34 C35 0.8(3) . . . . ? C33 C34 C35 C30 0.6(3) . . . . ? C35 C30 C31 C32 1.4(3) . . . . ? C36 P2 O4 Li1 -30.65(17) . . . . ? C36 P2 C24 C25 -39.75(17) . . . . ? C36 P2 C24 C29 141.30(15) . . . . ? C36 P2 C30 C31 -133.13(14) . . . . ? C36 P2 C30 C35 51.53(17) . . . . ? Li1 O1 C2 C1 -173.46(18) . . . . ? Li1 O1 C2 C3 4.8(3) . . . . ? Li1 O2 C4 C3 -8.1(3) . . . . ? Li1 O2 C4 C5 172.09(17) . . . . ? Cl2 Cl1 C37 Cl2 -40(3) 2_665 . . . ? 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 0.0000 -2.0000 4.9999 -0.0987 0.0025 -0.8306 -0.0000 2.0000 -4.9999 0.0987 -0.0025 0.8306 -5.0000 -2.0000 -0.9998 0.4260 -0.4558 0.0708 5.0000 2.0000 0.9998 -0.4260 0.4558 -0.0708 -0.0000 -5.0000 -3.0002 -0.4691 -0.4546 -0.1181 0.0000 5.0000 3.0002 0.4691 0.4546 0.1181