Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_'([OPO]Li2)2(THF)4' _database_code_depnum_ccdc_archive 'CCDC 653592' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C102 H140 Li4 O8 P2' _chemical_formula_sum 'C102 H140 Li4 O8 P2' _chemical_formula_weight 1583.84 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' 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4016(13) _cell_length_b 13.8466(17) _cell_length_c 27.718(3) _cell_angle_alpha 77.004(5) _cell_angle_beta 80.257(4) _cell_angle_gamma 76.333(4) _cell_volume 4833.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7623 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 28.03 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.088 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8956 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details Semi-empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/ADSC CCD' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 72152 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 28.03 _reflns_number_total 23119 _reflns_number_gt 17228 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'd*TREK (MSC, 1997)' _computing_cell_refinement 'd*TREK (MSC, 1997)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2004)' _computing_structure_solution 'SIR97 (Altomere et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+2.2777P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23119 _refine_ls_number_parameters 1057 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1462 _refine_ls_wR_factor_gt 0.1329 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.26152(11) 0.52107(11) 0.40356(6) 0.0196(3) Uani 1 1 d . . . C2 C 0.31732(12) 0.56203(12) 0.35740(6) 0.0218(3) Uani 1 1 d . . . C3 C 0.41860(12) 0.51276(12) 0.34521(6) 0.0234(3) Uani 1 1 d . . . H3 H 0.4540 0.5380 0.3139 0.028 Uiso 1 1 calc R . . C4 C 0.47217(11) 0.42829(12) 0.37589(6) 0.0217(3) Uani 1 1 d . . . C5 C 0.42123(11) 0.39708(12) 0.42265(6) 0.0207(3) Uani 1 1 d . . . H5 H 0.4563 0.3431 0.4455 0.025 Uiso 1 1 calc R . . C6 C 0.31903(11) 0.44349(11) 0.43683(6) 0.0193(3) Uani 1 1 d . . . C7 C 0.09388(11) 0.31554(11) 0.47733(6) 0.0192(3) Uani 1 1 d . . . C8 C 0.05756(12) 0.23412(12) 0.46695(6) 0.0215(3) Uani 1 1 d . . . C9 C 0.12975(13) 0.14613(12) 0.45979(6) 0.0251(3) Uani 1 1 d . . . H9 H 0.1054 0.0928 0.4523 0.030 Uiso 1 1 calc R . . C10 C 0.23589(12) 0.13109(12) 0.46294(6) 0.0241(3) Uani 1 1 d . . . C11 C 0.26793(12) 0.20820(12) 0.47634(6) 0.0226(3) Uani 1 1 d . . . H11 H 0.3387 0.1998 0.4803 0.027 Uiso 1 1 calc R . . C12 C 0.19961(11) 0.29822(11) 0.48427(6) 0.0194(3) Uani 1 1 d . . . C13 C 0.34765(12) 0.34209(12) 0.53715(6) 0.0217(3) Uani 1 1 d . . . C14 C 0.42027(13) 0.39743(14) 0.54054(7) 0.0296(4) Uani 1 1 d . . . H14 H 0.4192 0.4623 0.5198 0.035 Uiso 1 1 calc R . . C15 C 0.49373(15) 0.35965(16) 0.57351(8) 0.0392(4) Uani 1 1 d . . . H15 H 0.5431 0.3980 0.5748 0.047 Uiso 1 1 calc R . . C16 C 0.49493(15) 0.26611(17) 0.60444(8) 0.0414(5) Uani 1 1 d . . . H16 H 0.5451 0.2400 0.6271 0.050 Uiso 1 1 calc R . . C17 C 0.42316(15) 0.21056(15) 0.60237(7) 0.0369(4) Uani 1 1 d . . . H17 H 0.4236 0.1465 0.6239 0.044 Uiso 1 1 calc R . . C18 C 0.35015(13) 0.24804(13) 0.56888(6) 0.0281(4) Uani 1 1 d . . . H18 H 0.3014 0.2090 0.5676 0.034 Uiso 1 1 calc R . . C19 C 0.26617(13) 0.65683(13) 0.32229(6) 0.0275(4) Uani 1 1 d . . . C20 C 0.18092(15) 0.63342(16) 0.29864(7) 0.0378(4) Uani 1 1 d . . . H20A H 0.2115 0.5815 0.2785 0.057 Uiso 1 1 calc R . . H20B H 0.1477 0.6952 0.2773 0.057 Uiso 1 1 calc R . . H20C H 0.1292 0.6086 0.3250 0.057 Uiso 1 1 calc R . . C21 C 0.21984(15) 0.74253(13) 0.35136(7) 0.0352(4) Uani 1 1 d . . . H21A H 0.1701 0.7197 0.3793 0.053 Uiso 1 1 calc R . . H21B H 0.1846 0.8017 0.3292 0.053 Uiso 1 1 calc R . . H21C H 0.2753 0.7609 0.3641 0.053 Uiso 1 1 calc R . . C22 C 0.34383(15) 0.69659(16) 0.27944(7) 0.0421(5) Uani 1 1 d . . . H22A H 0.4008 0.7101 0.2932 0.063 Uiso 1 1 calc R . . H22B H 0.3090 0.7593 0.2594 0.063 Uiso 1 1 calc R . . H22C H 0.3712 0.6458 0.2584 0.063 Uiso 1 1 calc R . . C23 C 0.58120(12) 0.37432(13) 0.35739(6) 0.0259(3) Uani 1 1 d . . . C24 C 0.65453(14) 0.44936(16) 0.34217(8) 0.0381(4) Uani 1 1 d . . . H24A H 0.6268 0.5057 0.3164 0.057 Uiso 1 1 calc R . . H24B H 0.7229 0.4146 0.3291 0.057 Uiso 1 1 calc R . . H24C H 0.6606 0.4755 0.3713 0.057 Uiso 1 1 calc R . . C25 C 0.57493(15) 0.33085(16) 0.31205(8) 0.0401(5) Uani 1 1 d . . . H25A H 0.5456 0.3857 0.2860 0.060 Uiso 1 1 calc R . . H25B H 0.5307 0.2808 0.3220 0.060 Uiso 1 1 calc R . . H25C H 0.6445 0.2983 0.2992 0.060 Uiso 1 1 calc R . . C26 C 0.62707(14) 0.28751(15) 0.39756(7) 0.0387(4) Uani 1 1 d . . . H26A H 0.6964 0.2550 0.3844 0.058 Uiso 1 1 calc R . . H26B H 0.5826 0.2377 0.4072 0.058 Uiso 1 1 calc R . . H26C H 0.6316 0.3143 0.4268 0.058 Uiso 1 1 calc R . . C27 C -0.05802(12) 0.24185(12) 0.46365(7) 0.0261(3) Uani 1 1 d . . . C28 C -0.09999(15) 0.33329(15) 0.42435(8) 0.0409(5) Uani 1 1 d . . . H28A H -0.0594 0.3278 0.3918 0.061 Uiso 1 1 calc R . . H28B H -0.0947 0.3958 0.4338 0.061 Uiso 1 1 calc R . . H28C H -0.1726 0.3346 0.4224 0.061 Uiso 1 1 calc R . . C29 C -0.12039(14) 0.25151(16) 0.51488(8) 0.0391(4) Uani 1 1 d . . . H29A H -0.1944 0.2631 0.5122 0.059 Uiso 1 1 calc R . . H29B H -0.1062 0.3086 0.5261 0.059 Uiso 1 1 calc R . . H29C H -0.1003 0.1890 0.5390 0.059 Uiso 1 1 calc R . . C30 C -0.07810(15) 0.14765(14) 0.44958(8) 0.0379(4) Uani 1 1 d . . . H30A H -0.1522 0.1563 0.4478 0.057 Uiso 1 1 calc R . . H30B H -0.0558 0.0878 0.4749 0.057 Uiso 1 1 calc R . . H30C H -0.0392 0.1387 0.4171 0.057 Uiso 1 1 calc R . . C31 C 0.31483(13) 0.03552(13) 0.45231(7) 0.0310(4) Uani 1 1 d . . . C32 C 0.41000(15) 0.06541(15) 0.41837(9) 0.0441(5) Uani 1 1 d . . . H32A H 0.4404 0.1063 0.4342 0.066 Uiso 1 1 calc R . . H32B H 0.3893 0.1049 0.3863 0.066 Uiso 1 1 calc R . . H32C H 0.4612 0.0042 0.4129 0.066 Uiso 1 1 calc R . . C33 C 0.34984(18) -0.02883(16) 0.50161(9) 0.0502(6) Uani 1 1 d . . . H33A H 0.2899 -0.0488 0.5237 0.075 Uiso 1 1 calc R . . H33B H 0.3815 0.0108 0.5176 0.075 Uiso 1 1 calc R . . H33C H 0.4005 -0.0896 0.4950 0.075 Uiso 1 1 calc R . . C34 C 0.26983(17) -0.02834(16) 0.42671(11) 0.0529(6) Uani 1 1 d . . . H34A H 0.2089 -0.0484 0.4479 0.079 Uiso 1 1 calc R . . H34B H 0.3219 -0.0890 0.4213 0.079 Uiso 1 1 calc R . . H34C H 0.2498 0.0114 0.3945 0.079 Uiso 1 1 calc R . . C35 C 0.75723(11) -0.18762(11) 0.05090(5) 0.0195(3) Uani 1 1 d . . . C36 C 0.82534(12) -0.28485(12) 0.06192(6) 0.0218(3) Uani 1 1 d . . . C37 C 0.90163(12) -0.29495(12) 0.09213(6) 0.0246(3) Uani 1 1 d . . . H37 H 0.9445 -0.3600 0.1004 0.029 Uiso 1 1 calc R . . C38 C 0.91965(12) -0.21601(13) 0.11119(6) 0.0250(3) Uani 1 1 d . . . C39 C 0.86055(12) -0.12057(12) 0.09605(6) 0.0239(3) Uani 1 1 d . . . H39 H 0.8732 -0.0640 0.1063 0.029 Uiso 1 1 calc R . . C40 C 0.78269(12) -0.10612(11) 0.06591(6) 0.0207(3) Uani 1 1 d . . . C41 C 0.50193(12) 0.00598(11) 0.09820(6) 0.0192(3) Uani 1 1 d . . . C42 C 0.42567(12) 0.01079(12) 0.14119(6) 0.0231(3) Uani 1 1 d . . . C43 C 0.45683(14) 0.01939(13) 0.18529(6) 0.0285(4) Uani 1 1 d . . . H43 H 0.4064 0.0214 0.2138 0.034 Uiso 1 1 calc R . . C44 C 0.55709(14) 0.02521(13) 0.19049(6) 0.0289(4) Uani 1 1 d . . . C45 C 0.62768(13) 0.02734(12) 0.14782(6) 0.0257(3) Uani 1 1 d . . . H45 H 0.6959 0.0338 0.1496 0.031 Uiso 1 1 calc R . . C46 C 0.60144(12) 0.02029(11) 0.10229(6) 0.0207(3) Uani 1 1 d . . . C47 C 0.77699(12) 0.10675(12) 0.04907(6) 0.0232(3) Uani 1 1 d . . . C48 C 0.87528(14) 0.09682(13) 0.02140(7) 0.0305(4) Uani 1 1 d . . . H48 H 0.9015 0.0398 0.0059 0.037 Uiso 1 1 calc R . . C49 C 0.93521(15) 0.16892(15) 0.01617(8) 0.0401(5) Uani 1 1 d . . . H49 H 1.0023 0.1603 -0.0022 0.048 Uiso 1 1 calc R . . C50 C 0.89678(16) 0.25266(15) 0.03766(9) 0.0458(5) Uani 1 1 d . . . H50 H 0.9372 0.3023 0.0340 0.055 Uiso 1 1 calc R . . C51 C 0.79951(16) 0.26483(15) 0.06462(9) 0.0430(5) Uani 1 1 d . . . H51 H 0.7731 0.3232 0.0791 0.052 Uiso 1 1 calc R . . C52 C 0.73999(14) 0.19197(13) 0.07068(7) 0.0306(4) Uani 1 1 d . . . H52 H 0.6736 0.2005 0.0897 0.037 Uiso 1 1 calc R . . C53 C 0.81543(12) -0.37550(12) 0.04064(6) 0.0245(3) Uani 1 1 d . . . C54 C 0.71285(14) -0.40919(13) 0.06187(7) 0.0324(4) Uani 1 1 d . . . H54A H 0.6551 -0.3512 0.0560 0.049 Uiso 1 1 calc R . . H54B H 0.7122 -0.4354 0.0978 0.049 Uiso 1 1 calc R . . H54C H 0.7058 -0.4624 0.0454 0.049 Uiso 1 1 calc R . . C55 C 0.82160(14) -0.34543(14) -0.01652(7) 0.0316(4) Uani 1 1 d . . . H55A H 0.8887 -0.3276 -0.0302 0.047 Uiso 1 1 calc R . . H55B H 0.7659 -0.2871 -0.0256 0.047 Uiso 1 1 calc R . . H55C H 0.8141 -0.4025 -0.0301 0.047 Uiso 1 1 calc R . . C56 C 0.90242(15) -0.46829(13) 0.05333(8) 0.0348(4) Uani 1 1 d . . . H56A H 0.8959 -0.5225 0.0374 0.052 Uiso 1 1 calc R . . H56B H 0.8972 -0.4919 0.0896 0.052 Uiso 1 1 calc R . . H56C H 0.9696 -0.4496 0.0411 0.052 Uiso 1 1 calc R . . C57 C 0.31233(13) 0.00714(13) 0.13947(6) 0.0282(4) Uani 1 1 d . . . C58 C 0.30515(15) -0.09054(15) 0.12405(8) 0.0396(5) Uani 1 1 d . . . H58A H 0.2323 -0.0924 0.1247 0.059 Uiso 1 1 calc R . . H58B H 0.3376 -0.1493 0.1474 0.059 Uiso 1 1 calc R . . H58C H 0.3410 -0.0923 0.0903 0.059 Uiso 1 1 calc R . . C59 C 0.26356(14) 0.09973(15) 0.10284(7) 0.0363(4) Uani 1 1 d . . . H59A H 0.2600 0.1613 0.1154 0.054 Uiso 1 1 calc R . . H59B H 0.1936 0.0942 0.0994 0.054 Uiso 1 1 calc R . . H59C H 0.3059 0.1029 0.0702 0.054 Uiso 1 1 calc R . . C60 C 0.24570(15) 0.01066(17) 0.19056(7) 0.0424(5) Uani 1 1 d . . . H60A H 0.2476 0.0727 0.2015 0.064 Uiso 1 1 calc R . . H60B H 0.2731 -0.0485 0.2151 0.064 Uiso 1 1 calc R . . H60C H 0.1741 0.0100 0.1875 0.064 Uiso 1 1 calc R . . C61 C 1.00335(14) -0.23544(14) 0.14590(7) 0.0331(4) Uani 1 1 d . . . C62 C 1.11012(16) -0.2658(2) 0.11726(10) 0.0567(6) Uani 1 1 d . . . H62A H 1.1633 -0.2780 0.1395 0.085 Uiso 1 1 calc R . . H62B H 1.1220 -0.2111 0.0890 0.085 Uiso 1 1 calc R . . H62C H 1.1136 -0.3277 0.1050 0.085 Uiso 1 1 calc R . . C63 C 0.9850(2) -0.3206(2) 0.18971(10) 0.0730(9) Uani 1 1 d . . . H63A H 1.0383 -0.3330 0.2119 0.110 Uiso 1 1 calc R . . H63B H 0.9884 -0.3823 0.1773 0.110 Uiso 1 1 calc R . . H63C H 0.9166 -0.3012 0.2081 0.110 Uiso 1 1 calc R . . C64 C 1.0037(2) -0.1417(2) 0.16616(11) 0.0620(7) Uani 1 1 d . . . H64A H 1.0581 -0.1577 0.1880 0.093 Uiso 1 1 calc R . . H64B H 0.9364 -0.1206 0.1851 0.093 Uiso 1 1 calc R . . H64C H 1.0169 -0.0867 0.1383 0.093 Uiso 1 1 calc R . . C65 C 0.59201(17) 0.02543(16) 0.24072(7) 0.0408(5) Uani 1 1 d . . . C66 C 0.6614(2) -0.0767(2) 0.25813(9) 0.0660(8) Uani 1 1 d . . . H66A H 0.7202 -0.0895 0.2324 0.099 Uiso 1 1 calc R . . H66B H 0.6218 -0.1303 0.2640 0.099 Uiso 1 1 calc R . . H66C H 0.6869 -0.0760 0.2892 0.099 Uiso 1 1 calc R . . C67 C 0.6570(3) 0.1076(2) 0.23371(11) 0.0776(9) Uani 1 1 d . . . H67A H 0.7163 0.0951 0.2082 0.116 Uiso 1 1 calc R . . H67B H 0.6820 0.1050 0.2653 0.116 Uiso 1 1 calc R . . H67C H 0.6140 0.1746 0.2232 0.116 Uiso 1 1 calc R . . C68 C 0.5016(2) 0.0453(3) 0.28052(9) 0.0911(12) Uani 1 1 d . . . H68A H 0.4569 0.1110 0.2694 0.137 Uiso 1 1 calc R . . H68B H 0.5274 0.0459 0.3115 0.137 Uiso 1 1 calc R . . H68C H 0.4619 -0.0083 0.2865 0.137 Uiso 1 1 calc R . . C69 C -0.1392(2) 0.5703(2) 0.35603(13) 0.0736(9) Uani 1 1 d . . . H69A H -0.1941 0.5539 0.3834 0.088 Uiso 1 1 calc R . . H69B H -0.1206 0.5158 0.3363 0.088 Uiso 1 1 calc R . . C70 C -0.17713(18) 0.66801(18) 0.32389(8) 0.0481(5) Uani 1 1 d . . . H70A H -0.2529 0.6904 0.3317 0.058 Uiso 1 1 calc R . . H70B H -0.1609 0.6629 0.2882 0.058 Uiso 1 1 calc R . . C71 C -0.11982(17) 0.74129(16) 0.33579(8) 0.0455(5) Uani 1 1 d . . . H71A H -0.0681 0.7609 0.3075 0.055 Uiso 1 1 calc R . . H71B H -0.1686 0.8031 0.3437 0.055 Uiso 1 1 calc R . . C72 C -0.06769(14) 0.68110(14) 0.38100(7) 0.0348(4) Uani 1 1 d . . . H72A H -0.0011 0.7004 0.3810 0.042 Uiso 1 1 calc R . . H72B H -0.1127 0.6926 0.4123 0.042 Uiso 1 1 calc R . . C73 C 0.23040(17) 0.33078(17) 0.34884(8) 0.0467(5) Uani 1 1 d . . . H73A H 0.2444 0.2982 0.3833 0.056 Uiso 1 1 calc R . . H73B H 0.2834 0.3713 0.3334 0.056 Uiso 1 1 calc R . . C74 C 0.2310(3) 0.2534(3) 0.31917(12) 0.0899(11) Uani 1 1 d . . . H74A H 0.3007 0.2333 0.3012 0.108 Uiso 1 1 calc R . . H74B H 0.2108 0.1923 0.3411 0.108 Uiso 1 1 calc R . . C75 C 0.1563(3) 0.3013(3) 0.28415(13) 0.0937(11) Uani 1 1 d . . . H75A H 0.1134 0.2536 0.2820 0.112 Uiso 1 1 calc R . . H75B H 0.1922 0.3228 0.2505 0.112 Uiso 1 1 calc R . . C76 C 0.0906(2) 0.3909(2) 0.30341(8) 0.0533(6) Uani 1 1 d . . . H76A H 0.0957 0.4538 0.2786 0.064 Uiso 1 1 calc R . . H76B H 0.0173 0.3845 0.3103 0.064 Uiso 1 1 calc R . . C77 C 0.37345(14) -0.27935(14) 0.05270(7) 0.0330(4) Uani 1 1 d . . . H77A H 0.3143 -0.2309 0.0380 0.040 Uiso 1 1 calc R . . H77B H 0.3571 -0.2926 0.0895 0.040 Uiso 1 1 calc R . . C78 C 0.39651(19) -0.37734(16) 0.03298(9) 0.0490(5) Uani 1 1 d . . . H78A H 0.3338 -0.3883 0.0224 0.059 Uiso 1 1 calc R . . H78B H 0.4223 -0.4360 0.0588 0.059 Uiso 1 1 calc R . . C79 C 0.47999(16) -0.36267(14) -0.01165(8) 0.0394(4) Uani 1 1 d . . . H79A H 0.5427 -0.4169 -0.0073 0.047 Uiso 1 1 calc R . . H79B H 0.4542 -0.3626 -0.0431 0.047 Uiso 1 1 calc R . . C80 C 0.50292(14) -0.25967(13) -0.01188(7) 0.0308(4) Uani 1 1 d . . . H80A H 0.5781 -0.2613 -0.0199 0.037 Uiso 1 1 calc R . . H80B H 0.4661 -0.2064 -0.0368 0.037 Uiso 1 1 calc R . . C81 C 0.6121(2) -0.23513(17) 0.17243(8) 0.0514(6) Uani 1 1 d . . . H81A H 0.5649 -0.1954 0.1958 0.062 Uiso 1 1 calc R . . H81B H 0.6664 -0.1973 0.1553 0.062 Uiso 1 1 calc R . . C82 C 0.6586(3) -0.3358(2) 0.19916(13) 0.0800(10) Uani 1 1 d . . . H82A H 0.6615 -0.3337 0.2344 0.096 Uiso 1 1 calc R . . H82B H 0.7299 -0.3584 0.1834 0.096 Uiso 1 1 calc R . . C83 C 0.59206(17) -0.40618(16) 0.19639(8) 0.0440(5) Uani 1 1 d . . . H83A H 0.5523 -0.4259 0.2292 0.053 Uiso 1 1 calc R . . H83B H 0.6343 -0.4681 0.1853 0.053 Uiso 1 1 calc R . . C84 C 0.51977(15) -0.34573(14) 0.15816(7) 0.0367(4) Uani 1 1 d . . . H84A H 0.5218 -0.3846 0.1320 0.044 Uiso 1 1 calc R . . H84B H 0.4477 -0.3304 0.1745 0.044 Uiso 1 1 calc R . . C201 C 0.4154(3) 0.3094(2) 0.15475(14) 0.0877(10) Uani 1 1 d . . . H201 H 0.4569 0.2469 0.1481 0.105 Uiso 1 1 calc R . . C202 C 0.3337(2) 0.3575(2) 0.12893(10) 0.0666(7) Uani 1 1 d . . . H202 H 0.3164 0.3279 0.1045 0.080 Uiso 1 1 calc R . . C203 C 0.2766(2) 0.4491(2) 0.13848(10) 0.0649(7) Uani 1 1 d . . . H203 H 0.2208 0.4837 0.1199 0.078 Uiso 1 1 calc R . . C204 C 0.2992(2) 0.4907(2) 0.17423(11) 0.0702(8) Uani 1 1 d . . . H204 H 0.2587 0.5538 0.1806 0.084 Uiso 1 1 calc R . . C205 C 0.3775(3) 0.4440(2) 0.20036(15) 0.0863(10) Uani 1 1 d . . . H205 H 0.3923 0.4735 0.2255 0.104 Uiso 1 1 calc R . . C206 C 0.4365(3) 0.3539(3) 0.19105(17) 0.1065(14) Uani 1 1 d . . . H206 H 0.4927 0.3212 0.2096 0.128 Uiso 1 1 calc R . . C301 C 0.0295(3) 0.3150(3) 0.16408(12) 0.0822(9) Uani 1 1 d . . . H301 H 0.0993 0.3024 0.1490 0.099 Uiso 1 1 calc R . . C302 C -0.0303(4) 0.2556(3) 0.16078(14) 0.0968(11) Uani 1 1 d . . . H302 H -0.0042 0.2012 0.1435 0.116 Uiso 1 1 calc R . . C303 C -0.1332(4) 0.2724(4) 0.18287(19) 0.1240(19) Uani 1 1 d . . . H303 H -0.1787 0.2305 0.1810 0.149 Uiso 1 1 calc R . . C304 C -0.1668(3) 0.3565(4) 0.20854(14) 0.1087(16) Uani 1 1 d . . . H304 H -0.2356 0.3716 0.2246 0.130 Uiso 1 1 calc R . . C305 C -0.0977(3) 0.4130(3) 0.20913(13) 0.0913(11) Uani 1 1 d . . . H305 H -0.1182 0.4692 0.2256 0.110 Uiso 1 1 calc R . . C306 C -0.0029(3) 0.3915(3) 0.18739(13) 0.0811(9) Uani 1 1 d . . . H306 H 0.0440 0.4325 0.1885 0.097 Uiso 1 1 calc R . . C401 C 0.9593(4) 0.0875(3) 0.30367(17) 0.1102(13) Uani 1 1 d . . . H401 H 0.9829 0.1309 0.2744 0.132 Uiso 1 1 calc R . . C402 C 1.0272(4) 0.0140(4) 0.32869(17) 0.1139(15) Uani 1 1 d . . . H402 H 1.0989 0.0060 0.3169 0.137 Uiso 1 1 calc R . . C403 C 0.9956(4) -0.0483(3) 0.37012(16) 0.1047(15) Uani 1 1 d . . . H403 H 1.0456 -0.0992 0.3872 0.126 Uiso 1 1 calc R . . C404 C 0.8914(4) -0.0400(3) 0.38854(15) 0.1069(14) Uani 1 1 d . . . H404 H 0.8685 -0.0840 0.4177 0.128 Uiso 1 1 calc R . . C405 C 0.8202(3) 0.0389(4) 0.36093(19) 0.1018(13) Uani 1 1 d . . . H405 H 0.7478 0.0485 0.3711 0.122 Uiso 1 1 calc R . . C406 C 0.8596(3) 0.0992(3) 0.31984(16) 0.0972(12) Uani 1 1 d . . . H406 H 0.8130 0.1525 0.3019 0.117 Uiso 1 1 calc R . . O1 O 0.16032(8) 0.55064(8) 0.41539(4) 0.0224(2) Uani 1 1 d . . . O2 O 0.03324(8) 0.40736(8) 0.47857(4) 0.0210(2) Uani 1 1 d . . . O3 O -0.05115(10) 0.57718(10) 0.37611(5) 0.0371(3) Uani 1 1 d . . . O4 O 0.12860(11) 0.39348(11) 0.34867(5) 0.0391(3) Uani 1 1 d . . . O5 O 0.67301(8) -0.17171(8) 0.02856(4) 0.0212(2) Uani 1 1 d . . . O6 O 0.48449(8) -0.01534(8) 0.05584(4) 0.0204(2) Uani 1 1 d . . . O7 O 0.46671(9) -0.24046(9) 0.03773(5) 0.0303(3) Uani 1 1 d . . . O8 O 0.55597(11) -0.25389(9) 0.13693(5) 0.0355(3) Uani 1 1 d . . . P1 P 0.24617(3) 0.40295(3) 0.496970(14) 0.01802(9) Uani 1 1 d . . . P2 P 0.69839(3) 0.01633(3) 0.047177(15) 0.01946(9) Uani 1 1 d . . . Li1 Li 0.0835(2) 0.5317(2) 0.48188(11) 0.0253(6) Uani 1 1 d . . . Li2 Li 0.0680(2) 0.4745(2) 0.40156(11) 0.0300(6) Uani 1 1 d . . . Li3 Li 0.5967(2) -0.0413(2) -0.00346(10) 0.0248(6) Uani 1 1 d . . . Li4 Li 0.5423(2) -0.1730(2) 0.07022(10) 0.0269(6) 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 C1 0.0162(7) 0.0210(7) 0.0230(7) -0.0065(6) -0.0026(6) -0.0041(6) C2 0.0187(7) 0.0244(8) 0.0216(7) -0.0029(6) -0.0034(6) -0.0039(6) C3 0.0194(7) 0.0287(8) 0.0210(7) -0.0038(6) 0.0001(6) -0.0056(6) C4 0.0145(7) 0.0250(8) 0.0263(8) -0.0072(6) -0.0016(6) -0.0036(6) C5 0.0169(7) 0.0221(7) 0.0232(7) -0.0039(6) -0.0042(6) -0.0034(6) C6 0.0171(7) 0.0217(7) 0.0197(7) -0.0045(6) -0.0004(6) -0.0061(6) C7 0.0178(7) 0.0191(7) 0.0200(7) -0.0044(6) 0.0003(6) -0.0037(6) C8 0.0184(7) 0.0221(7) 0.0250(8) -0.0046(6) -0.0025(6) -0.0060(6) C9 0.0252(8) 0.0215(8) 0.0306(8) -0.0074(7) -0.0030(7) -0.0070(6) C10 0.0205(8) 0.0212(7) 0.0285(8) -0.0061(6) 0.0000(6) -0.0011(6) C11 0.0160(7) 0.0238(8) 0.0269(8) -0.0048(6) -0.0012(6) -0.0028(6) C12 0.0175(7) 0.0200(7) 0.0214(7) -0.0044(6) -0.0010(6) -0.0054(6) C13 0.0182(7) 0.0258(8) 0.0210(7) -0.0077(6) -0.0017(6) -0.0016(6) C14 0.0291(9) 0.0327(9) 0.0305(9) -0.0081(7) -0.0069(7) -0.0092(7) C15 0.0309(10) 0.0523(12) 0.0420(11) -0.0184(9) -0.0138(8) -0.0082(9) C16 0.0338(10) 0.0534(12) 0.0372(10) -0.0148(9) -0.0187(8) 0.0063(9) C17 0.0392(11) 0.0343(10) 0.0312(9) -0.0021(8) -0.0107(8) 0.0047(8) C18 0.0272(9) 0.0292(9) 0.0264(8) -0.0038(7) -0.0039(7) -0.0041(7) C19 0.0224(8) 0.0289(8) 0.0248(8) 0.0011(7) -0.0011(6) -0.0002(7) C20 0.0323(10) 0.0466(11) 0.0296(9) -0.0015(8) -0.0103(8) 0.0005(8) C21 0.0332(10) 0.0260(9) 0.0395(10) -0.0009(8) -0.0006(8) -0.0008(7) C22 0.0347(10) 0.0411(11) 0.0345(10) 0.0104(8) 0.0042(8) 0.0008(8) C23 0.0162(7) 0.0316(9) 0.0272(8) -0.0059(7) -0.0002(6) -0.0015(6) C24 0.0187(8) 0.0460(11) 0.0475(11) -0.0073(9) 0.0028(8) -0.0090(8) C25 0.0313(10) 0.0484(12) 0.0407(11) -0.0215(9) -0.0009(8) 0.0017(8) C26 0.0219(9) 0.0435(11) 0.0402(10) -0.0021(9) -0.0011(8) 0.0061(8) C27 0.0194(8) 0.0250(8) 0.0367(9) -0.0084(7) -0.0059(7) -0.0064(6) C28 0.0311(10) 0.0411(11) 0.0531(12) -0.0002(9) -0.0189(9) -0.0110(8) C29 0.0256(9) 0.0453(11) 0.0505(12) -0.0163(9) 0.0055(8) -0.0161(8) C30 0.0282(9) 0.0345(10) 0.0587(13) -0.0180(9) -0.0086(9) -0.0104(8) C31 0.0253(9) 0.0220(8) 0.0446(10) -0.0112(7) -0.0014(7) -0.0002(7) C32 0.0329(10) 0.0345(10) 0.0591(13) -0.0172(10) 0.0114(9) 0.0002(8) C33 0.0484(13) 0.0316(10) 0.0586(14) -0.0009(10) -0.0078(11) 0.0084(9) C34 0.0410(12) 0.0368(11) 0.0883(18) -0.0371(12) -0.0093(12) 0.0023(9) C35 0.0177(7) 0.0198(7) 0.0189(7) -0.0029(6) 0.0009(6) -0.0027(6) C36 0.0199(7) 0.0207(7) 0.0228(7) -0.0047(6) 0.0012(6) -0.0025(6) C37 0.0203(8) 0.0222(8) 0.0266(8) -0.0018(6) -0.0020(6) 0.0010(6) C38 0.0189(8) 0.0285(8) 0.0261(8) -0.0035(7) -0.0040(6) -0.0028(6) C39 0.0220(8) 0.0253(8) 0.0258(8) -0.0079(6) -0.0022(6) -0.0052(6) C40 0.0184(7) 0.0198(7) 0.0226(7) -0.0039(6) -0.0009(6) -0.0025(6) C41 0.0212(7) 0.0145(7) 0.0202(7) -0.0029(6) -0.0021(6) -0.0010(5) C42 0.0237(8) 0.0189(7) 0.0233(8) -0.0035(6) 0.0017(6) -0.0015(6) C43 0.0315(9) 0.0276(8) 0.0219(8) -0.0072(7) 0.0029(7) 0.0007(7) C44 0.0359(10) 0.0275(8) 0.0219(8) -0.0084(7) -0.0066(7) 0.0016(7) C45 0.0262(8) 0.0251(8) 0.0268(8) -0.0080(7) -0.0061(7) -0.0021(6) C46 0.0211(7) 0.0181(7) 0.0212(7) -0.0041(6) -0.0012(6) -0.0014(6) C47 0.0235(8) 0.0199(7) 0.0268(8) -0.0019(6) -0.0058(6) -0.0059(6) C48 0.0293(9) 0.0251(8) 0.0362(9) -0.0063(7) 0.0015(7) -0.0073(7) C49 0.0315(10) 0.0362(10) 0.0514(12) -0.0041(9) 0.0033(9) -0.0148(8) C50 0.0405(11) 0.0313(10) 0.0703(15) -0.0085(10) -0.0045(10) -0.0193(9) C51 0.0441(12) 0.0266(9) 0.0635(14) -0.0170(9) -0.0071(10) -0.0093(8) C52 0.0284(9) 0.0254(8) 0.0397(10) -0.0110(7) -0.0041(7) -0.0045(7) C53 0.0238(8) 0.0195(7) 0.0286(8) -0.0070(6) -0.0018(6) 0.0000(6) C54 0.0320(9) 0.0228(8) 0.0416(10) -0.0067(7) -0.0002(8) -0.0068(7) C55 0.0345(10) 0.0296(9) 0.0303(9) -0.0108(7) -0.0018(7) -0.0028(7) C56 0.0349(10) 0.0233(8) 0.0437(11) -0.0117(8) -0.0067(8) 0.0052(7) C57 0.0218(8) 0.0299(9) 0.0284(8) -0.0049(7) 0.0044(7) -0.0029(7) C58 0.0288(10) 0.0373(10) 0.0545(12) -0.0131(9) 0.0050(9) -0.0131(8) C59 0.0237(9) 0.0397(10) 0.0384(10) -0.0054(8) 0.0008(7) 0.0018(8) C60 0.0308(10) 0.0545(13) 0.0354(10) -0.0070(9) 0.0109(8) -0.0081(9) C61 0.0269(9) 0.0356(10) 0.0377(10) -0.0040(8) -0.0130(8) -0.0047(7) C62 0.0262(10) 0.0776(17) 0.0642(15) -0.0151(13) -0.0181(10) 0.0034(10) C63 0.085(2) 0.095(2) 0.0475(14) 0.0259(14) -0.0396(14) -0.0514(17) C64 0.0529(14) 0.0624(15) 0.0840(19) -0.0321(14) -0.0426(14) 0.0031(12) C65 0.0465(12) 0.0496(12) 0.0254(9) -0.0156(8) -0.0096(8) 0.0031(9) C66 0.0845(19) 0.0689(17) 0.0382(12) -0.0119(12) -0.0305(13) 0.0144(14) C67 0.112(3) 0.087(2) 0.0557(16) -0.0252(15) -0.0352(16) -0.0335(19) C68 0.0633(18) 0.172(4) 0.0349(13) -0.0526(18) -0.0057(12) 0.012(2) C69 0.0629(17) 0.0495(14) 0.121(3) -0.0097(15) -0.0622(18) -0.0064(12) C70 0.0489(13) 0.0573(14) 0.0367(11) -0.0082(10) -0.0172(9) -0.0006(10) C71 0.0479(12) 0.0381(11) 0.0441(12) 0.0003(9) -0.0102(10) -0.0012(9) C72 0.0262(9) 0.0370(10) 0.0400(10) -0.0095(8) -0.0042(8) -0.0018(7) C73 0.0466(12) 0.0478(12) 0.0439(12) -0.0175(10) -0.0119(10) 0.0068(10) C74 0.117(3) 0.073(2) 0.075(2) -0.0395(17) -0.0348(19) 0.0296(19) C75 0.112(3) 0.099(3) 0.084(2) -0.056(2) -0.042(2) 0.009(2) C76 0.0588(15) 0.0656(15) 0.0397(12) -0.0158(11) -0.0157(10) -0.0090(12) C77 0.0271(9) 0.0325(9) 0.0406(10) -0.0073(8) -0.0024(8) -0.0095(7) C78 0.0631(14) 0.0363(11) 0.0528(13) -0.0115(10) 0.0036(11) -0.0253(10) C79 0.0437(11) 0.0287(9) 0.0480(11) -0.0144(8) -0.0045(9) -0.0063(8) C80 0.0317(9) 0.0294(9) 0.0326(9) -0.0086(7) -0.0030(7) -0.0068(7) C81 0.0829(17) 0.0395(12) 0.0349(11) -0.0052(9) -0.0188(11) -0.0124(11) C82 0.094(2) 0.0619(17) 0.089(2) 0.0274(15) -0.0574(18) -0.0324(16) C83 0.0440(12) 0.0371(11) 0.0380(11) 0.0089(9) -0.0002(9) -0.0022(9) C84 0.0367(10) 0.0340(10) 0.0318(9) 0.0033(8) 0.0033(8) -0.0068(8) C201 0.101(3) 0.0502(16) 0.101(3) -0.0184(17) -0.016(2) 0.0106(16) C202 0.088(2) 0.0655(17) 0.0534(15) -0.0101(13) -0.0090(14) -0.0303(16) C203 0.0566(16) 0.0722(18) 0.0582(16) 0.0019(14) -0.0113(12) -0.0088(13) C204 0.081(2) 0.0488(15) 0.0719(18) -0.0056(13) -0.0112(16) -0.0017(14) C205 0.096(2) 0.0577(17) 0.120(3) -0.0318(18) -0.048(2) -0.0076(16) C206 0.100(3) 0.087(2) 0.143(4) -0.040(2) -0.074(3) 0.019(2) C301 0.0659(19) 0.098(3) 0.072(2) -0.0142(19) -0.0154(16) 0.0053(18) C302 0.121(3) 0.094(3) 0.082(2) -0.028(2) -0.026(2) -0.015(2) C303 0.136(4) 0.130(4) 0.124(4) 0.037(3) -0.069(3) -0.084(3) C304 0.057(2) 0.143(4) 0.075(2) 0.040(2) 0.0087(17) 0.008(2) C305 0.110(3) 0.082(2) 0.063(2) -0.0086(17) -0.010(2) 0.011(2) C306 0.073(2) 0.086(2) 0.083(2) -0.0078(19) -0.0281(18) -0.0090(18) C401 0.114(3) 0.112(3) 0.099(3) -0.023(2) -0.033(3) 0.005(3) C402 0.109(3) 0.116(3) 0.102(3) -0.040(3) -0.025(3) 0.033(3) C403 0.143(4) 0.070(2) 0.090(3) -0.039(2) -0.051(3) 0.051(2) C404 0.182(5) 0.067(2) 0.088(3) -0.050(2) -0.013(3) -0.026(3) C405 0.082(2) 0.111(3) 0.136(4) -0.082(3) -0.017(3) -0.009(2) C406 0.086(3) 0.110(3) 0.095(3) -0.023(2) -0.046(2) 0.008(2) O1 0.0132(5) 0.0288(6) 0.0241(5) -0.0049(5) -0.0013(4) -0.0033(4) O2 0.0155(5) 0.0189(5) 0.0290(6) -0.0078(4) -0.0013(4) -0.0021(4) O3 0.0249(6) 0.0338(7) 0.0527(8) -0.0025(6) -0.0151(6) -0.0046(5) O4 0.0420(8) 0.0432(8) 0.0327(7) -0.0119(6) -0.0089(6) -0.0026(6) O5 0.0178(5) 0.0200(5) 0.0254(5) -0.0050(4) -0.0036(4) -0.0023(4) O6 0.0198(5) 0.0217(5) 0.0196(5) -0.0056(4) -0.0020(4) -0.0029(4) O7 0.0259(6) 0.0308(6) 0.0370(7) -0.0122(5) 0.0004(5) -0.0091(5) O8 0.0468(8) 0.0285(6) 0.0280(6) 0.0011(5) -0.0046(6) -0.0074(6) P1 0.01457(18) 0.01941(18) 0.02017(18) -0.00419(15) -0.00120(14) -0.00399(14) P2 0.01869(19) 0.01811(18) 0.02166(19) -0.00473(15) -0.00196(15) -0.00346(14) Li1 0.0202(13) 0.0252(14) 0.0299(14) -0.0085(11) 0.0009(11) -0.0038(11) Li2 0.0250(14) 0.0325(15) 0.0334(15) -0.0075(12) -0.0071(12) -0.0039(12) Li3 0.0231(13) 0.0248(13) 0.0251(13) -0.0043(11) -0.0037(11) -0.0021(11) Li4 0.0264(14) 0.0254(14) 0.0267(14) -0.0028(11) -0.0015(11) -0.0044(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.3274(18) . ? C1 C6 1.415(2) . ? C1 C2 1.438(2) . ? C2 C3 1.390(2) . ? C2 C19 1.538(2) . ? C3 C4 1.403(2) . ? C3 H3 0.9500 . ? C4 C5 1.386(2) . ? C4 C23 1.536(2) . ? C5 C6 1.400(2) . ? C5 H5 0.9500 . ? C6 P1 1.8260(15) . ? C7 O2 1.3416(18) . ? C7 C12 1.419(2) . ? C7 C8 1.430(2) . ? C7 Li2 2.680(3) . ? C8 C9 1.395(2) . ? C8 C27 1.544(2) . ? C9 C10 1.403(2) . ? C9 H9 0.9500 . ? C10 C11 1.383(2) . ? C10 C31 1.538(2) . ? C11 C12 1.399(2) . ? C11 H11 0.9500 . ? C12 P1 1.8296(15) . ? C13 C18 1.395(2) . ? C13 C14 1.400(2) . ? C13 P1 1.8301(16) . ? C14 C15 1.387(3) . ? C14 H14 0.9500 . ? C15 C16 1.381(3) . ? C15 H15 0.9500 . ? C16 C17 1.381(3) . ? C16 H16 0.9500 . ? C17 C18 1.392(2) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C22 1.535(2) . ? C19 C21 1.535(3) . ? C19 C20 1.538(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C26 1.531(2) . ? C23 C25 1.533(3) . ? C23 C24 1.539(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C30 1.535(2) . ? C27 C28 1.535(3) . ? C27 C29 1.537(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C34 1.526(3) . ? C31 C32 1.533(3) . ? C31 C33 1.534(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 O5 1.3281(18) . ? C35 C40 1.416(2) . ? C35 C36 1.438(2) . ? C36 C37 1.391(2) . ? C36 C53 1.542(2) . ? C37 C38 1.400(2) . ? C37 H37 0.9500 . ? C38 C39 1.385(2) . ? C38 C61 1.537(2) . ? C39 C40 1.396(2) . ? C39 H39 0.9500 . ? C40 P2 1.8216(16) . ? C41 O6 1.3425(18) . ? C41 C46 1.420(2) . ? C41 C42 1.435(2) . ? C41 Li4 2.670(3) . ? C42 C43 1.394(2) . ? C42 C57 1.541(2) . ? C43 C44 1.398(3) . ? C43 H43 0.9500 . ? C44 C45 1.383(2) . ? C44 C65 1.543(2) . ? C45 C46 1.396(2) . ? C45 H45 0.9500 . ? C46 P2 1.8321(16) . ? C47 C52 1.392(2) . ? C47 C48 1.401(2) . ? C47 P2 1.8307(16) . ? C48 C49 1.392(2) . ? C48 H48 0.9500 . ? C49 C50 1.375(3) . ? C49 H49 0.9500 . ? C50 C51 1.382(3) . ? C50 H50 0.9500 . ? C51 C52 1.393(3) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.536(2) . ? C53 C56 1.537(2) . ? C53 C55 1.538(2) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C59 1.531(2) . ? C57 C58 1.535(3) . ? C57 C60 1.545(2) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C63 1.522(3) . ? C61 C64 1.527(3) . ? C61 C62 1.528(3) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C68 1.512(3) . ? C65 C66 1.524(3) . ? C65 C67 1.550(4) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 O3 1.418(3) . ? C69 C70 1.472(3) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.527(3) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.518(3) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 O3 1.437(2) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 O4 1.434(2) . ? C73 C74 1.488(4) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.452(4) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.491(4) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 O4 1.442(2) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 O7 1.437(2) . ? C77 C78 1.521(3) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C79 1.533(3) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C80 1.527(2) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 O7 1.441(2) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 O8 1.435(3) . ? C81 C82 1.470(3) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C83 1.490(3) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.525(3) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 O8 1.434(2) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C201 C202 1.364(4) . ? C201 C206 1.389(5) . ? C201 H201 0.9500 . ? C202 C203 1.374(4) . ? C202 H202 0.9500 . ? C203 C204 1.358(4) . ? C203 H203 0.9500 . ? C204 C205 1.330(4) . ? C204 H204 0.9500 . ? C205 C206 1.363(5) . ? C205 H205 0.9500 . ? C206 H206 0.9500 . ? C301 C302 1.303(5) . ? C301 C306 1.313(5) . ? C301 H301 0.9500 . ? C302 C303 1.399(7) . ? C302 H302 0.9500 . ? C303 C304 1.442(7) . ? C303 H303 0.9500 . ? C304 C305 1.351(6) . ? C304 H304 0.9500 . ? C305 C306 1.307(5) . ? C305 H305 0.9500 . ? C306 H306 0.9500 . ? C401 C406 1.319(6) . ? C401 C402 1.343(5) . ? C401 H401 0.9500 . ? C402 C403 1.344(6) . ? C402 H402 0.9500 . ? C403 C404 1.391(6) . ? C403 H403 0.9500 . ? C404 C405 1.438(6) . ? C404 H404 0.9500 . ? C405 C406 1.361(6) . ? C405 H405 0.9500 . ? C406 H406 0.9500 . ? O1 Li2 1.936(3) . ? O1 Li1 1.948(3) . ? O2 Li1 1.890(3) 2_566 ? O2 Li1 2.016(3) . ? O2 Li2 2.148(3) . ? O3 Li2 1.981(3) . ? O4 Li2 1.994(3) . ? O5 Li4 1.930(3) . ? O5 Li3 1.951(3) . ? O6 Li3 1.878(3) 2_655 ? O6 Li3 2.065(3) . ? O6 Li4 2.107(3) . ? O7 Li4 1.960(3) . ? O8 Li4 1.948(3) . ? P1 Li1 2.499(3) . ? P2 Li3 2.476(3) . ? Li1 O2 1.890(3) 2_566 ? Li1 Li1 2.560(5) 2_566 ? Li1 Li2 2.579(4) . ? Li1 Li2 3.507(4) 2_566 ? Li2 Li1 3.507(4) 2_566 ? Li3 O6 1.878(3) 2_655 ? Li3 Li4 2.545(4) . ? Li3 Li3 2.567(5) 2_655 ? Li3 Li4 3.433(4) 2_655 ? Li4 Li3 3.433(4) 2_655 ? 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 O1 C1 C6 119.57(13) . . ? O1 C1 C2 123.44(14) . . ? C6 C1 C2 116.97(13) . . ? C3 C2 C1 118.00(14) . . ? C3 C2 C19 120.96(14) . . ? C1 C2 C19 121.03(13) . . ? C2 C3 C4 124.56(14) . . ? C2 C3 H3 117.7 . . ? C4 C3 H3 117.7 . . ? C5 C4 C3 116.53(14) . . ? C5 C4 C23 122.89(14) . . ? C3 C4 C23 120.58(14) . . ? C4 C5 C6 121.26(14) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 121.77(14) . . ? C5 C6 P1 123.36(12) . . ? C1 C6 P1 114.69(11) . . ? O2 C7 C12 119.71(13) . . ? O2 C7 C8 122.53(13) . . ? C12 C7 C8 117.70(13) . . ? O2 C7 Li2 52.57(10) . . ? C12 C7 Li2 104.83(11) . . ? C8 C7 Li2 109.66(12) . . ? C9 C8 C7 118.14(14) . . ? C9 C8 C27 120.18(14) . . ? C7 C8 C27 121.68(14) . . ? C8 C9 C10 124.46(15) . . ? C8 C9 H9 117.8 . . ? C10 C9 H9 117.8 . . ? C11 C10 C9 116.25(14) . . ? C11 C10 C31 120.27(14) . . ? C9 C10 C31 123.48(15) . . ? C10 C11 C12 122.20(14) . . ? C10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C11 C12 C7 120.92(14) . . ? C11 C12 P1 121.13(11) . . ? C7 C12 P1 117.59(11) . . ? C18 C13 C14 117.68(15) . . ? C18 C13 P1 123.62(12) . . ? C14 C13 P1 118.29(12) . . ? C15 C14 C13 121.47(17) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C16 C15 C14 119.79(18) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 119.91(17) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C18 120.28(18) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C13 120.86(17) . . ? C17 C18 H18 119.6 . . ? C13 C18 H18 119.6 . . ? C22 C19 C21 107.02(15) . . ? C22 C19 C20 107.19(15) . . ? C21 C19 C20 109.73(15) . . ? C22 C19 C2 112.26(14) . . ? C21 C19 C2 109.84(14) . . ? C20 C19 C2 110.69(14) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C26 C23 C25 108.61(16) . . ? C26 C23 C4 111.87(14) . . ? C25 C23 C4 108.72(14) . . ? C26 C23 C24 107.98(15) . . ? C25 C23 C24 109.25(15) . . ? C4 C23 C24 110.36(14) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C30 C27 C28 106.96(15) . . ? C30 C27 C29 107.05(15) . . ? C28 C27 C29 109.42(16) . . ? C30 C27 C8 112.51(14) . . ? C28 C27 C8 111.55(14) . . ? C29 C27 C8 109.21(14) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C34 C31 C32 108.16(17) . . ? C34 C31 C33 108.98(17) . . ? C32 C31 C33 108.40(17) . . ? C34 C31 C10 112.07(15) . . ? C32 C31 C10 109.93(14) . . ? C33 C31 C10 109.23(16) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O5 C35 C40 119.62(13) . . ? O5 C35 C36 123.74(14) . . ? C40 C35 C36 116.63(14) . . ? C37 C36 C35 118.05(14) . . ? C37 C36 C53 120.58(14) . . ? C35 C36 C53 121.36(14) . . ? C36 C37 C38 124.65(15) . . ? C36 C37 H37 117.7 . . ? C38 C37 H37 117.7 . . ? C39 C38 C37 116.61(15) . . ? C39 C38 C61 122.52(15) . . ? C37 C38 C61 120.85(15) . . ? C38 C39 C40 121.05(15) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C39 C40 C35 122.27(14) . . ? C39 C40 P2 123.15(12) . . ? C35 C40 P2 114.38(11) . . ? O6 C41 C46 119.42(13) . . ? O6 C41 C42 123.13(14) . . ? C46 C41 C42 117.39(14) . . ? O6 C41 Li4 51.22(9) . . ? C46 C41 Li4 103.37(11) . . ? C42 C41 Li4 112.52(12) . . ? C43 C42 C41 117.96(15) . . ? C43 C42 C57 120.15(14) . . ? C41 C42 C57 121.89(14) . . ? C42 C43 C44 124.60(15) . . ? C42 C43 H43 117.7 . . ? C44 C43 H43 117.7 . . ? C45 C44 C43 116.54(15) . . ? C45 C44 C65 119.84(16) . . ? C43 C44 C65 123.58(16) . . ? C44 C45 C46 121.85(16) . . ? C44 C45 H45 119.1 . . ? C46 C45 H45 119.1 . . ? C45 C46 C41 121.27(14) . . ? C45 C46 P2 120.91(12) . . ? C41 C46 P2 117.54(11) . . ? C52 C47 C48 118.01(15) . . ? C52 C47 P2 123.82(13) . . ? C48 C47 P2 117.60(13) . . ? C49 C48 C47 121.28(17) . . ? C49 C48 H48 119.4 . . ? C47 C48 H48 119.4 . . ? C50 C49 C48 119.62(18) . . ? C50 C49 H49 120.2 . . ? C48 C49 H49 120.2 . . ? C49 C50 C51 120.19(18) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C50 C51 C52 120.37(18) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C47 C52 C51 120.51(17) . . ? C47 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? C54 C53 C56 106.75(14) . . ? C54 C53 C55 109.44(15) . . ? C56 C53 C55 107.82(14) . . ? C54 C53 C36 111.36(13) . . ? C56 C53 C36 112.10(14) . . ? C55 C53 C36 109.27(13) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C59 C57 C58 110.09(16) . . ? C59 C57 C42 109.51(14) . . ? C58 C57 C42 111.10(14) . . ? C59 C57 C60 106.60(15) . . ? C58 C57 C60 107.03(15) . . ? C42 C57 C60 112.37(15) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C63 C61 C64 108.6(2) . . ? C63 C61 C62 109.4(2) . . ? C64 C61 C62 107.33(18) . . ? C63 C61 C38 109.35(16) . . ? C64 C61 C38 112.41(15) . . ? C62 C61 C38 109.68(16) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C68 C65 C66 109.4(2) . . ? C68 C65 C44 112.37(18) . . ? C66 C65 C44 108.92(16) . . ? C68 C65 C67 108.8(2) . . ? C66 C65 C67 107.4(2) . . ? C44 C65 C67 109.88(18) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O3 C69 C70 108.9(2) . . ? O3 C69 H69A 109.9 . . ? C70 C69 H69A 109.9 . . ? O3 C69 H69B 109.9 . . ? C70 C69 H69B 109.9 . . ? H69A C69 H69B 108.3 . . ? C69 C70 C71 104.54(17) . . ? C69 C70 H70A 110.8 . . ? C71 C70 H70A 110.8 . . ? C69 C70 H70B 110.8 . . ? C71 C70 H70B 110.8 . . ? H70A C70 H70B 108.9 . . ? C72 C71 C70 103.64(16) . . ? C72 C71 H71A 111.0 . . ? C70 C71 H71A 111.0 . . ? C72 C71 H71B 111.0 . . ? C70 C71 H71B 111.0 . . ? H71A C71 H71B 109.0 . . ? O3 C72 C71 104.72(16) . . ? O3 C72 H72A 110.8 . . ? C71 C72 H72A 110.8 . . ? O3 C72 H72B 110.8 . . ? C71 C72 H72B 110.8 . . ? H72A C72 H72B 108.9 . . ? O4 C73 C74 105.2(2) . . ? O4 C73 H73A 110.7 . . ? C74 C73 H73A 110.7 . . ? O4 C73 H73B 110.7 . . ? C74 C73 H73B 110.7 . . ? H73A C73 H73B 108.8 . . ? C75 C74 C73 105.6(2) . . ? C75 C74 H74A 110.6 . . ? C73 C74 H74A 110.6 . . ? C75 C74 H74B 110.6 . . ? C73 C74 H74B 110.6 . . ? H74A C74 H74B 108.7 . . ? C74 C75 C76 106.6(2) . . ? C74 C75 H75A 110.4 . . ? C76 C75 H75A 110.4 . . ? C74 C75 H75B 110.4 . . ? C76 C75 H75B 110.4 . . ? H75A C75 H75B 108.6 . . ? O4 C76 C75 106.8(2) . . ? O4 C76 H76A 110.4 . . ? C75 C76 H76A 110.4 . . ? O4 C76 H76B 110.4 . . ? C75 C76 H76B 110.4 . . ? H76A C76 H76B 108.6 . . ? O7 C77 C78 104.73(15) . . ? O7 C77 H77A 110.8 . . ? C78 C77 H77A 110.8 . . ? O7 C77 H77B 110.8 . . ? C78 C77 H77B 110.8 . . ? H77A C77 H77B 108.9 . . ? C77 C78 C79 104.58(15) . . ? C77 C78 H78A 110.8 . . ? C79 C78 H78A 110.8 . . ? C77 C78 H78B 110.8 . . ? C79 C78 H78B 110.8 . . ? H78A C78 H78B 108.9 . . ? C80 C79 C78 104.12(15) . . ? C80 C79 H79A 110.9 . . ? C78 C79 H79A 110.9 . . ? C80 C79 H79B 110.9 . . ? C78 C79 H79B 110.9 . . ? H79A C79 H79B 109.0 . . ? O7 C80 C79 105.56(14) . . ? O7 C80 H80A 110.6 . . ? C79 C80 H80A 110.6 . . ? O7 C80 H80B 110.6 . . ? C79 C80 H80B 110.6 . . ? H80A C80 H80B 108.8 . . ? O8 C81 C82 105.40(19) . . ? O8 C81 H81A 110.7 . . ? C82 C81 H81A 110.7 . . ? O8 C81 H81B 110.7 . . ? C82 C81 H81B 110.7 . . ? H81A C81 H81B 108.8 . . ? C81 C82 C83 106.9(2) . . ? C81 C82 H82A 110.3 . . ? C83 C82 H82A 110.3 . . ? C81 C82 H82B 110.3 . . ? C83 C82 H82B 110.3 . . ? H82A C82 H82B 108.6 . . ? C82 C83 C84 104.44(17) . . ? C82 C83 H83A 110.9 . . ? C84 C83 H83A 110.9 . . ? C82 C83 H83B 110.9 . . ? C84 C83 H83B 110.9 . . ? H83A C83 H83B 108.9 . . ? O8 C84 C83 106.42(16) . . ? O8 C84 H84A 110.4 . . ? C83 C84 H84A 110.4 . . ? O8 C84 H84B 110.4 . . ? C83 C84 H84B 110.4 . . ? H84A C84 H84B 108.6 . . ? C202 C201 C206 118.4(3) . . ? C202 C201 H201 120.8 . . ? C206 C201 H201 120.8 . . ? C201 C202 C203 119.5(3) . . ? C201 C202 H202 120.2 . . ? C203 C202 H202 120.2 . . ? C204 C203 C202 120.6(3) . . ? C204 C203 H203 119.7 . . ? C202 C203 H203 119.7 . . ? C205 C204 C203 120.7(3) . . ? C205 C204 H204 119.6 . . ? C203 C204 H204 119.6 . . ? C204 C205 C206 119.9(3) . . ? C204 C205 H205 120.1 . . ? C206 C205 H205 120.1 . . ? C205 C206 C201 120.8(3) . . ? C205 C206 H206 119.6 . . ? C201 C206 H206 119.6 . . ? C302 C301 C306 122.5(4) . . ? C302 C301 H301 118.7 . . ? C306 C301 H301 118.7 . . ? C301 C302 C303 119.7(4) . . ? C301 C302 H302 120.2 . . ? C303 C302 H302 120.2 . . ? C302 C303 C304 116.8(4) . . ? C302 C303 H303 121.6 . . ? C304 C303 H303 121.6 . . ? C305 C304 C303 118.1(4) . . ? C305 C304 H304 121.0 . . ? C303 C304 H304 121.0 . . ? C306 C305 C304 120.8(4) . . ? C306 C305 H305 119.6 . . ? C304 C305 H305 119.6 . . ? C305 C306 C301 122.1(4) . . ? C305 C306 H306 118.9 . . ? C301 C306 H306 118.9 . . ? C406 C401 C402 119.8(5) . . ? C406 C401 H401 120.1 . . ? C402 C401 H401 120.1 . . ? C401 C402 C403 121.2(5) . . ? C401 C402 H402 119.4 . . ? C403 C402 H402 119.4 . . ? C402 C403 C404 121.4(4) . . ? C402 C403 H403 119.3 . . ? C404 C403 H403 119.3 . . ? C403 C404 C405 116.3(4) . . ? C403 C404 H404 121.9 . . ? C405 C404 H404 121.9 . . ? C406 C405 C404 118.1(4) . . ? C406 C405 H405 121.0 . . ? C404 C405 H405 121.0 . . ? C401 C406 C405 123.2(4) . . ? C401 C406 H406 118.4 . . ? C405 C406 H406 118.4 . . ? C1 O1 Li2 118.99(13) . . ? C1 O1 Li1 126.80(13) . . ? Li2 O1 Li1 83.23(13) . . ? C7 O2 Li1 138.85(13) . 2_566 ? C7 O2 Li1 124.89(12) . . ? Li1 O2 Li1 81.83(12) 2_566 . ? C7 O2 Li2 97.69(12) . . ? Li1 O2 Li2 120.48(13) 2_566 . ? Li1 O2 Li2 76.48(12) . . ? C69 O3 C72 105.24(15) . . ? C69 O3 Li2 132.84(16) . . ? C72 O3 Li2 121.60(14) . . ? C73 O4 C76 107.49(16) . . ? C73 O4 Li2 121.53(14) . . ? C76 O4 Li2 130.74(16) . . ? C35 O5 Li4 117.79(13) . . ? C35 O5 Li3 126.70(12) . . ? Li4 O5 Li3 81.95(12) . . ? C41 O6 Li3 139.71(13) . 2_655 ? C41 O6 Li3 124.50(12) . . ? Li3 O6 Li3 81.10(13) 2_655 . ? C41 O6 Li4 99.00(11) . . ? Li3 O6 Li4 118.87(13) 2_655 . ? Li3 O6 Li4 75.17(11) . . ? C77 O7 C80 105.42(13) . . ? C77 O7 Li4 133.54(14) . . ? C80 O7 Li4 121.05(13) . . ? C84 O8 C81 107.68(15) . . ? C84 O8 Li4 127.11(15) . . ? C81 O8 Li4 125.06(15) . . ? C6 P1 C12 100.99(7) . . ? C6 P1 C13 103.12(7) . . ? C12 P1 C13 104.80(7) . . ? C6 P1 Li1 96.10(8) . . ? C12 P1 Li1 95.32(8) . . ? C13 P1 Li1 148.71(8) . . ? C40 P2 C47 103.25(7) . . ? C40 P2 C46 100.89(7) . . ? C47 P2 C46 105.55(7) . . ? C40 P2 Li3 96.73(8) . . ? C47 P2 Li3 146.45(8) . . ? C46 P2 Li3 96.64(8) . . ? O2 Li1 O1 142.19(16) 2_566 . ? O2 Li1 O2 98.17(12) 2_566 . ? O1 Li1 O2 97.80(13) . . ? O2 Li1 P1 136.55(15) 2_566 . ? O1 Li1 P1 79.75(10) . . ? O2 Li1 P1 81.40(10) . . ? O2 Li1 Li1 51.23(10) 2_566 2_566 ? O1 Li1 Li1 133.6(2) . 2_566 ? O2 Li1 Li1 46.94(10) . 2_566 ? P1 Li1 Li1 114.71(16) . 2_566 ? O2 Li1 Li2 122.23(15) 2_566 . ? O1 Li1 Li2 48.18(10) . . ? O2 Li1 Li2 54.05(10) . . ? P1 Li1 Li2 92.76(11) . . ? Li1 Li1 Li2 86.06(15) 2_566 . ? O2 Li1 Li2 31.85(8) 2_566 2_566 ? O1 Li1 Li2 173.78(14) . 2_566 ? O2 Li1 Li2 86.18(10) . 2_566 ? P1 Li1 Li2 105.65(10) . 2_566 ? Li1 Li1 Li2 47.20(11) 2_566 2_566 ? Li2 Li1 Li2 133.26(11) . 2_566 ? O1 Li2 O3 105.51(15) . . ? O1 Li2 O4 113.89(15) . . ? O3 Li2 O4 106.98(15) . . ? O1 Li2 O2 93.91(13) . . ? O3 Li2 O2 111.82(15) . . ? O4 Li2 O2 123.16(15) . . ? O1 Li2 Li1 48.58(10) . . ? O3 Li2 Li1 101.80(14) . . ? O4 Li2 Li1 150.04(16) . . ? O2 Li2 Li1 49.47(9) . . ? O1 Li2 C7 99.68(12) . . ? O3 Li2 C7 135.80(15) . . ? O4 Li2 C7 94.75(12) . . ? O2 Li2 C7 29.74(6) . . ? Li1 Li2 C7 69.35(10) . . ? O1 Li2 Li1 95.00(12) . 2_566 ? O3 Li2 Li1 85.01(11) . 2_566 ? O4 Li2 Li1 143.29(14) . 2_566 ? O2 Li2 Li1 27.67(7) . 2_566 ? Li1 Li2 Li1 46.74(11) . 2_566 ? C7 Li2 Li1 56.80(8) . 2_566 ? O6 Li3 O5 140.65(16) 2_655 . ? O6 Li3 O6 98.90(13) 2_655 . ? O5 Li3 O6 97.67(12) . . ? O6 Li3 P2 137.95(14) 2_655 . ? O5 Li3 P2 79.90(10) . . ? O6 Li3 P2 80.91(10) . . ? O6 Li3 Li4 121.69(15) 2_655 . ? O5 Li3 Li4 48.67(9) . . ? O6 Li3 Li4 53.16(9) . . ? P2 Li3 Li4 92.00(11) . . ? O6 Li3 Li3 52.63(10) 2_655 2_655 ? O5 Li3 Li3 132.29(19) . 2_655 ? O6 Li3 Li3 46.27(9) . 2_655 ? P2 Li3 Li3 114.58(16) . 2_655 ? Li4 Li3 Li3 84.37(15) . 2_655 ? O6 Li3 Li4 32.51(8) 2_655 2_655 ? O5 Li3 Li4 173.12(14) . 2_655 ? O6 Li3 Li4 85.84(10) . 2_655 ? P2 Li3 Li4 106.57(10) . 2_655 ? Li4 Li3 Li4 131.91(11) . 2_655 ? Li3 Li3 Li4 47.54(11) 2_655 2_655 ? O5 Li4 O8 113.29(15) . . ? O5 Li4 O7 104.90(14) . . ? O8 Li4 O7 106.51(14) . . ? O5 Li4 O6 96.94(12) . . ? O8 Li4 O6 123.59(15) . . ? O7 Li4 O6 110.11(14) . . ? O5 Li4 Li3 49.38(9) . . ? O8 Li4 Li3 151.61(16) . . ? O7 Li4 Li3 100.41(13) . . ? O6 Li4 Li3 51.67(9) . . ? O5 Li4 C41 102.08(12) . . ? O8 Li4 C41 95.51(12) . . ? O7 Li4 C41 134.31(14) . . ? O6 Li4 C41 29.78(6) . . ? Li3 Li4 C41 71.12(10) . . ? O5 Li4 Li3 97.06(11) . 2_655 ? O8 Li4 Li3 143.95(14) . 2_655 ? O7 Li4 Li3 82.58(11) . 2_655 ? O6 Li4 Li3 28.62(7) . 2_655 ? Li3 Li4 Li3 48.09(11) . 2_655 ? C41 Li4 Li3 57.90(8) . 2_655 ? 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 O1 C1 C2 C3 -168.46(14) . . . . ? C6 C1 C2 C3 9.9(2) . . . . ? O1 C1 C2 C19 10.9(2) . . . . ? C6 C1 C2 C19 -170.74(14) . . . . ? C1 C2 C3 C4 -3.1(2) . . . . ? C19 C2 C3 C4 177.53(15) . . . . ? C2 C3 C4 C5 -4.1(2) . . . . ? C2 C3 C4 C23 175.39(15) . . . . ? C3 C4 C5 C6 4.3(2) . . . . ? C23 C4 C5 C6 -175.24(15) . . . . ? C4 C5 C6 C1 2.9(2) . . . . ? C4 C5 C6 P1 177.73(12) . . . . ? O1 C1 C6 C5 168.41(14) . . . . ? C2 C1 C6 C5 -10.0(2) . . . . ? O1 C1 C6 P1 -6.88(19) . . . . ? C2 C1 C6 P1 174.70(11) . . . . ? O2 C7 C8 C9 171.42(14) . . . . ? C12 C7 C8 C9 -5.7(2) . . . . ? Li2 C7 C8 C9 113.94(15) . . . . ? O2 C7 C8 C27 -8.7(2) . . . . ? C12 C7 C8 C27 174.23(14) . . . . ? Li2 C7 C8 C27 -66.13(17) . . . . ? C7 C8 C9 C10 1.2(2) . . . . ? C27 C8 C9 C10 -178.76(15) . . . . ? C8 C9 C10 C11 3.1(2) . . . . ? C8 C9 C10 C31 -176.81(16) . . . . ? C9 C10 C11 C12 -2.7(2) . . . . ? C31 C10 C11 C12 177.22(15) . . . . ? C10 C11 C12 C7 -1.9(2) . . . . ? C10 C11 C12 P1 -174.96(12) . . . . ? O2 C7 C12 C11 -171.02(14) . . . . ? C8 C7 C12 C11 6.2(2) . . . . ? Li2 C7 C12 C11 -115.96(15) . . . . ? O2 C7 C12 P1 2.23(19) . . . . ? C8 C7 C12 P1 179.43(11) . . . . ? Li2 C7 C12 P1 57.29(14) . . . . ? C18 C13 C14 C15 1.3(3) . . . . ? P1 C13 C14 C15 174.27(14) . . . . ? C13 C14 C15 C16 -1.1(3) . . . . ? C14 C15 C16 C17 0.1(3) . . . . ? C15 C16 C17 C18 0.6(3) . . . . ? C16 C17 C18 C13 -0.4(3) . . . . ? C14 C13 C18 C17 -0.6(3) . . . . ? P1 C13 C18 C17 -173.15(14) . . . . ? C3 C2 C19 C22 -9.3(2) . . . . ? C1 C2 C19 C22 171.38(16) . . . . ? C3 C2 C19 C21 -128.21(17) . . . . ? C1 C2 C19 C21 52.4(2) . . . . ? C3 C2 C19 C20 110.46(18) . . . . ? C1 C2 C19 C20 -68.9(2) . . . . ? C5 C4 C23 C26 -3.1(2) . . . . ? C3 C4 C23 C26 177.37(16) . . . . ? C5 C4 C23 C25 116.81(18) . . . . ? C3 C4 C23 C25 -62.7(2) . . . . ? C5 C4 C23 C24 -123.39(17) . . . . ? C3 C4 C23 C24 57.1(2) . . . . ? C9 C8 C27 C30 -2.9(2) . . . . ? C7 C8 C27 C30 177.14(15) . . . . ? C9 C8 C27 C28 -123.14(18) . . . . ? C7 C8 C27 C28 56.9(2) . . . . ? C9 C8 C27 C29 115.78(17) . . . . ? C7 C8 C27 C29 -64.1(2) . . . . ? C11 C10 C31 C34 -166.63(18) . . . . ? C9 C10 C31 C34 13.2(3) . . . . ? C11 C10 C31 C32 -46.3(2) . . . . ? C9 C10 C31 C32 133.56(18) . . . . ? C11 C10 C31 C33 72.5(2) . . . . ? C9 C10 C31 C33 -107.6(2) . . . . ? O5 C35 C36 C37 -170.26(14) . . . . ? C40 C35 C36 C37 8.7(2) . . . . ? O5 C35 C36 C53 10.3(2) . . . . ? C40 C35 C36 C53 -170.69(14) . . . . ? C35 C36 C37 C38 -2.5(2) . . . . ? C53 C36 C37 C38 176.86(15) . . . . ? C36 C37 C38 C39 -4.0(2) . . . . ? C36 C37 C38 C61 177.73(16) . . . . ? C37 C38 C39 C40 4.0(2) . . . . ? C61 C38 C39 C40 -177.73(15) . . . . ? C38 C39 C40 C35 2.5(2) . . . . ? C38 C39 C40 P2 177.03(12) . . . . ? O5 C35 C40 C39 170.08(14) . . . . ? C36 C35 C40 C39 -8.9(2) . . . . ? O5 C35 C40 P2 -4.88(18) . . . . ? C36 C35 C40 P2 176.11(11) . . . . ? O6 C41 C42 C43 171.13(14) . . . . ? C46 C41 C42 C43 -6.0(2) . . . . ? Li4 C41 C42 C43 113.76(15) . . . . ? O6 C41 C42 C57 -9.1(2) . . . . ? C46 C41 C42 C57 173.74(14) . . . . ? Li4 C41 C42 C57 -66.49(18) . . . . ? C41 C42 C43 C44 1.0(2) . . . . ? C57 C42 C43 C44 -178.75(16) . . . . ? C42 C43 C44 C45 3.2(3) . . . . ? C42 C43 C44 C65 -174.54(17) . . . . ? C43 C44 C45 C46 -2.3(2) . . . . ? C65 C44 C45 C46 175.57(16) . . . . ? C44 C45 C46 C41 -2.9(2) . . . . ? C44 C45 C46 P2 -176.63(13) . . . . ? O6 C41 C46 C45 -170.21(14) . . . . ? C42 C41 C46 C45 7.0(2) . . . . ? Li4 C41 C46 C45 -117.45(15) . . . . ? O6 C41 C46 P2 3.74(19) . . . . ? C42 C41 C46 P2 -179.00(11) . . . . ? Li4 C41 C46 P2 56.50(13) . . . . ? C52 C47 C48 C49 1.0(3) . . . . ? P2 C47 C48 C49 172.60(15) . . . . ? C47 C48 C49 C50 -1.3(3) . . . . ? C48 C49 C50 C51 0.5(3) . . . . ? C49 C50 C51 C52 0.6(3) . . . . ? C48 C47 C52 C51 0.2(3) . . . . ? P2 C47 C52 C51 -170.92(15) . . . . ? C50 C51 C52 C47 -1.0(3) . . . . ? C37 C36 C53 C54 114.78(17) . . . . ? C35 C36 C53 C54 -65.84(19) . . . . ? C37 C36 C53 C56 -4.7(2) . . . . ? C35 C36 C53 C56 174.65(15) . . . . ? C37 C36 C53 C55 -124.20(16) . . . . ? C35 C36 C53 C55 55.18(19) . . . . ? C43 C42 C57 C59 116.52(17) . . . . ? C41 C42 C57 C59 -63.2(2) . . . . ? C43 C42 C57 C58 -121.65(17) . . . . ? C41 C42 C57 C58 58.6(2) . . . . ? C43 C42 C57 C60 -1.8(2) . . . . ? C41 C42 C57 C60 178.50(15) . . . . ? C39 C38 C61 C63 127.7(2) . . . . ? C37 C38 C61 C63 -54.0(2) . . . . ? C39 C38 C61 C64 7.0(3) . . . . ? C37 C38 C61 C64 -174.80(19) . . . . ? C39 C38 C61 C62 -112.3(2) . . . . ? C37 C38 C61 C62 65.9(2) . . . . ? C45 C44 C65 C68 167.9(2) . . . . ? C43 C44 C65 C68 -14.5(3) . . . . ? C45 C44 C65 C66 -70.8(2) . . . . ? C43 C44 C65 C66 106.9(2) . . . . ? C45 C44 C65 C67 46.6(3) . . . . ? C43 C44 C65 C67 -135.7(2) . . . . ? O3 C69 C70 C71 -12.6(3) . . . . ? C69 C70 C71 C72 -9.7(3) . . . . ? C70 C71 C72 O3 28.3(2) . . . . ? O4 C73 C74 C75 28.0(4) . . . . ? C73 C74 C75 C76 -17.2(4) . . . . ? C74 C75 C76 O4 0.3(4) . . . . ? O7 C77 C78 C79 -25.9(2) . . . . ? C77 C78 C79 C80 3.4(2) . . . . ? C78 C79 C80 O7 20.1(2) . . . . ? O8 C81 C82 C83 -26.1(3) . . . . ? C81 C82 C83 C84 11.3(3) . . . . ? C82 C83 C84 O8 7.5(3) . . . . ? C206 C201 C202 C203 1.7(5) . . . . ? C201 C202 C203 C204 -1.7(5) . . . . ? C202 C203 C204 C205 0.6(5) . . . . ? C203 C204 C205 C206 0.5(6) . . . . ? C204 C205 C206 C201 -0.5(7) . . . . ? C202 C201 C206 C205 -0.6(6) . . . . ? C306 C301 C302 C303 -0.3(6) . . . . ? C301 C302 C303 C304 -0.1(6) . . . . ? C302 C303 C304 C305 0.5(5) . . . . ? C303 C304 C305 C306 -0.6(5) . . . . ? C304 C305 C306 C301 0.2(5) . . . . ? C302 C301 C306 C305 0.3(6) . . . . ? C406 C401 C402 C403 0.1(7) . . . . ? C401 C402 C403 C404 0.6(6) . . . . ? C402 C403 C404 C405 -0.2(5) . . . . ? C403 C404 C405 C406 -0.7(5) . . . . ? C402 C401 C406 C405 -1.1(7) . . . . ? C404 C405 C406 C401 1.5(6) . . . . ? C6 C1 O1 Li2 -83.58(18) . . . . ? C2 C1 O1 Li2 94.73(18) . . . . ? C6 C1 O1 Li1 20.7(2) . . . . ? C2 C1 O1 Li1 -161.01(15) . . . . ? C12 C7 O2 Li1 -114.9(2) . . . 2_566 ? C8 C7 O2 Li1 68.0(2) . . . 2_566 ? Li2 C7 O2 Li1 158.8(2) . . . 2_566 ? C12 C7 O2 Li1 7.4(2) . . . . ? C8 C7 O2 Li1 -169.66(15) . . . . ? Li2 C7 O2 Li1 -78.85(15) . . . . ? C12 C7 O2 Li2 86.24(16) . . . . ? C8 C7 O2 Li2 -90.81(16) . . . . ? C70 C69 O3 C72 31.3(3) . . . . ? C70 C69 O3 Li2 -155.4(2) . . . . ? C71 C72 O3 C69 -36.8(2) . . . . ? C71 C72 O3 Li2 149.01(17) . . . . ? C74 C73 O4 C76 -28.1(3) . . . . ? C74 C73 O4 Li2 156.9(2) . . . . ? C75 C76 O4 C73 17.5(3) . . . . ? C75 C76 O4 Li2 -168.2(2) . . . . ? C40 C35 O5 Li4 -82.96(17) . . . . ? C36 C35 O5 Li4 95.98(18) . . . . ? C40 C35 O5 Li3 18.3(2) . . . . ? C36 C35 O5 Li3 -162.76(15) . . . . ? C46 C41 O6 Li3 -116.0(2) . . . 2_655 ? C42 C41 O6 Li3 67.0(2) . . . 2_655 ? Li4 C41 O6 Li3 160.5(2) . . . 2_655 ? C46 C41 O6 Li3 5.4(2) . . . . ? C42 C41 O6 Li3 -171.70(14) . . . . ? Li4 C41 O6 Li3 -78.13(14) . . . . ? C46 C41 O6 Li4 83.53(15) . . . . ? C42 C41 O6 Li4 -93.57(16) . . . . ? C78 C77 O7 C80 39.72(18) . . . . ? C78 C77 O7 Li4 -140.67(18) . . . . ? C79 C80 O7 C77 -37.60(18) . . . . ? C79 C80 O7 Li4 142.73(15) . . . . ? C83 C84 O8 C81 -24.2(2) . . . . ? C83 C84 O8 Li4 151.44(17) . . . . ? C82 C81 O8 C84 31.4(3) . . . . ? C82 C81 O8 Li4 -144.3(2) . . . . ? C5 C6 P1 C12 -83.19(14) . . . . ? C1 C6 P1 C12 92.02(12) . . . . ? C5 C6 P1 C13 25.02(15) . . . . ? C1 C6 P1 C13 -159.78(11) . . . . ? C5 C6 P1 Li1 -179.84(14) . . . . ? C1 C6 P1 Li1 -4.63(13) . . . . ? C11 C12 P1 C6 68.36(14) . . . . ? C7 C12 P1 C6 -104.87(12) . . . . ? C11 C12 P1 C13 -38.53(14) . . . . ? C7 C12 P1 C13 148.24(12) . . . . ? C11 C12 P1 Li1 165.64(14) . . . . ? C7 C12 P1 Li1 -7.59(13) . . . . ? C18 C13 P1 C6 -132.88(14) . . . . ? C14 C13 P1 C6 54.58(14) . . . . ? C18 C13 P1 C12 -27.57(16) . . . . ? C14 C13 P1 C12 159.89(13) . . . . ? C18 C13 P1 Li1 100.7(2) . . . . ? C14 C13 P1 Li1 -71.8(2) . . . . ? C39 C40 P2 C47 26.56(15) . . . . ? C35 C40 P2 C47 -158.53(11) . . . . ? C39 C40 P2 C46 -82.45(14) . . . . ? C35 C40 P2 C46 92.46(12) . . . . ? C39 C40 P2 Li3 179.42(14) . . . . ? C35 C40 P2 Li3 -5.66(13) . . . . ? C52 C47 P2 C40 -134.30(15) . . . . ? C48 C47 P2 C40 54.59(15) . . . . ? C52 C47 P2 C46 -28.81(16) . . . . ? C48 C47 P2 C46 160.08(13) . . . . ? C52 C47 P2 Li3 100.7(2) . . . . ? C48 C47 P2 Li3 -70.4(2) . . . . ? C45 C46 P2 C40 67.44(14) . . . . ? C41 C46 P2 C40 -106.53(12) . . . . ? C45 C46 P2 C47 -39.77(14) . . . . ? C41 C46 P2 C47 146.26(12) . . . . ? C45 C46 P2 Li3 165.64(14) . . . . ? C41 C46 P2 Li3 -8.34(13) . . . . ? C1 O1 Li1 O2 147.8(2) . . . 2_566 ? Li2 O1 Li1 O2 -90.8(3) . . . 2_566 ? C1 O1 Li1 O2 -97.98(16) . . . . ? Li2 O1 Li1 O2 23.41(13) . . . . ? C1 O1 Li1 P1 -18.25(16) . . . . ? Li2 O1 Li1 P1 103.14(11) . . . . ? C1 O1 Li1 Li1 -132.7(2) . . . 2_566 ? Li2 O1 Li1 Li1 -11.4(3) . . . 2_566 ? C1 O1 Li1 Li2 -121.39(17) . . . . ? C1 O1 Li1 Li2 132.4(12) . . . 2_566 ? Li2 O1 Li1 Li2 -106.2(13) . . . 2_566 ? C7 O2 Li1 O2 -145.83(14) . . . 2_566 ? Li1 O2 Li1 O2 0.0 2_566 . . 2_566 ? Li2 O2 Li1 O2 124.16(14) . . . 2_566 ? C7 O2 Li1 O1 68.56(17) . . . . ? Li1 O2 Li1 O1 -145.61(19) 2_566 . . . ? Li2 O2 Li1 O1 -21.45(12) . . . . ? C7 O2 Li1 P1 -9.77(15) . . . . ? Li1 O2 Li1 P1 136.06(15) 2_566 . . . ? Li2 O2 Li1 P1 -99.78(10) . . . . ? C7 O2 Li1 Li1 -145.83(14) . . . 2_566 ? Li2 O2 Li1 Li1 124.16(14) . . . 2_566 ? C7 O2 Li1 Li2 90.01(15) . . . . ? Li1 O2 Li1 Li2 -124.16(14) 2_566 . . . ? C7 O2 Li1 Li2 -116.25(13) . . . 2_566 ? Li1 O2 Li1 Li2 29.59(9) 2_566 . . 2_566 ? Li2 O2 Li1 Li2 153.75(8) . . . 2_566 ? C6 P1 Li1 O2 -157.71(19) . . . 2_566 ? C12 P1 Li1 O2 100.6(2) . . . 2_566 ? C13 P1 Li1 O2 -29.7(3) . . . 2_566 ? C6 P1 Li1 O1 9.87(10) . . . . ? C12 P1 Li1 O1 -91.82(9) . . . . ? C13 P1 Li1 O1 137.84(13) . . . . ? C6 P1 Li1 O2 109.48(9) . . . . ? C12 P1 Li1 O2 7.79(10) . . . . ? C13 P1 Li1 O2 -122.55(14) . . . . ? C6 P1 Li1 Li1 143.40(17) . . . 2_566 ? C12 P1 Li1 Li1 41.71(18) . . . 2_566 ? C13 P1 Li1 Li1 -88.6(2) . . . 2_566 ? C6 P1 Li1 Li2 56.47(11) . . . . ? C12 P1 Li1 Li2 -45.21(11) . . . . ? C13 P1 Li1 Li2 -175.55(13) . . . . ? C6 P1 Li1 Li2 -166.98(9) . . . 2_566 ? C12 P1 Li1 Li2 91.34(10) . . . 2_566 ? C13 P1 Li1 Li2 -39.00(19) . . . 2_566 ? C1 O1 Li2 O3 -139.21(14) . . . . ? Li1 O1 Li2 O3 92.19(15) . . . . ? C1 O1 Li2 O4 -22.2(2) . . . . ? Li1 O1 Li2 O4 -150.78(17) . . . . ? C1 O1 Li2 O2 106.86(14) . . . . ? Li1 O1 Li2 O2 -21.74(12) . . . . ? C1 O1 Li2 Li1 128.60(15) . . . . ? C1 O1 Li2 C7 77.46(15) . . . . ? Li1 O1 Li2 C7 -51.14(12) . . . . ? C1 O1 Li2 Li1 134.60(12) . . . 2_566 ? Li1 O1 Li2 Li1 5.99(14) . . . 2_566 ? C69 O3 Li2 O1 174.1(2) . . . . ? C72 O3 Li2 O1 -13.5(2) . . . . ? C69 O3 Li2 O4 52.5(3) . . . . ? C72 O3 Li2 O4 -135.16(16) . . . . ? C69 O3 Li2 O2 -85.1(3) . . . . ? C72 O3 Li2 O2 87.26(19) . . . . ? C69 O3 Li2 Li1 -135.9(3) . . . . ? C72 O3 Li2 Li1 36.4(2) . . . . ? C69 O3 Li2 C7 -63.5(3) . . . . ? C72 O3 Li2 C7 108.8(2) . . . . ? C69 O3 Li2 Li1 -92.1(3) . . . 2_566 ? C72 O3 Li2 Li1 80.27(15) . . . 2_566 ? C73 O4 Li2 O1 47.4(2) . . . . ? C76 O4 Li2 O1 -126.3(2) . . . . ? C73 O4 Li2 O3 163.56(16) . . . . ? C76 O4 Li2 O3 -10.1(3) . . . . ? C73 O4 Li2 O2 -64.9(2) . . . . ? C76 O4 Li2 O2 121.5(2) . . . . ? C73 O4 Li2 Li1 0.2(4) . . . . ? C76 O4 Li2 Li1 -173.4(3) . . . . ? C73 O4 Li2 C7 -55.41(19) . . . . ? C76 O4 Li2 C7 130.96(19) . . . . ? C73 O4 Li2 Li1 -91.5(3) . . . 2_566 ? C76 O4 Li2 Li1 94.8(3) . . . 2_566 ? C7 O2 Li2 O1 -102.71(13) . . . . ? Li1 O2 Li2 O1 93.31(15) 2_566 . . . ? Li1 O2 Li2 O1 21.43(12) . . . . ? C7 O2 Li2 O3 148.86(14) . . . . ? Li1 O2 Li2 O3 -15.1(2) 2_566 . . . ? Li1 O2 Li2 O3 -87.00(16) . . . . ? C7 O2 Li2 O4 19.27(19) . . . . ? Li1 O2 Li2 O4 -144.71(16) 2_566 . . . ? Li1 O2 Li2 O4 143.41(19) . . . . ? C7 O2 Li2 Li1 -124.14(12) . . . . ? Li1 O2 Li2 Li1 71.88(16) 2_566 . . . ? Li1 O2 Li2 C7 -163.98(16) 2_566 . . . ? Li1 O2 Li2 C7 124.14(12) . . . . ? C7 O2 Li2 Li1 163.98(16) . . . 2_566 ? Li1 O2 Li2 Li1 -71.88(16) . . . 2_566 ? O2 Li1 Li2 O1 133.56(19) 2_566 . . . ? O2 Li1 Li2 O1 -150.91(15) . . . . ? P1 Li1 Li2 O1 -73.62(10) . . . . ? Li1 Li1 Li2 O1 171.79(19) 2_566 . . . ? Li2 Li1 Li2 O1 171.79(19) 2_566 . . . ? O2 Li1 Li2 O3 33.2(2) 2_566 . . . ? O1 Li1 Li2 O3 -100.37(15) . . . . ? O2 Li1 Li2 O3 108.71(14) . . . . ? P1 Li1 Li2 O3 -173.99(12) . . . . ? Li1 Li1 Li2 O3 71.41(16) 2_566 . . . ? Li2 Li1 Li2 O3 71.41(16) 2_566 . . . ? O2 Li1 Li2 O4 -163.1(3) 2_566 . . . ? O1 Li1 Li2 O4 63.3(3) . . . . ? O2 Li1 Li2 O4 -87.6(3) . . . . ? P1 Li1 Li2 O4 -10.3(3) . . . . ? Li1 Li1 Li2 O4 -124.9(3) 2_566 . . . ? Li2 Li1 Li2 O4 -124.9(3) 2_566 . . . ? O2 Li1 Li2 O2 -75.53(16) 2_566 . . . ? O1 Li1 Li2 O2 150.91(15) . . . . ? P1 Li1 Li2 O2 77.30(10) . . . . ? Li1 Li1 Li2 O2 -37.30(10) 2_566 . . . ? Li2 Li1 Li2 O2 -37.30(10) 2_566 . . . ? O2 Li1 Li2 C7 -101.56(16) 2_566 . . . ? O1 Li1 Li2 C7 124.89(12) . . . . ? O2 Li1 Li2 C7 -26.02(6) . . . . ? P1 Li1 Li2 C7 51.27(8) . . . . ? Li1 Li1 Li2 C7 -63.33(12) 2_566 . . . ? Li2 Li1 Li2 C7 -63.33(12) 2_566 . . . ? O2 Li1 Li2 Li1 -38.23(10) 2_566 . . 2_566 ? O1 Li1 Li2 Li1 -171.79(19) . . . 2_566 ? O2 Li1 Li2 Li1 37.30(10) . . . 2_566 ? P1 Li1 Li2 Li1 114.60(16) . . . 2_566 ? Li2 Li1 Li2 Li1 0.0 2_566 . . 2_566 ? O2 C7 Li2 O1 80.85(14) . . . . ? C12 C7 Li2 O1 -35.44(16) . . . . ? C8 C7 Li2 O1 -162.68(13) . . . . ? O2 C7 Li2 O3 -43.5(2) . . . . ? C12 C7 Li2 O3 -159.8(2) . . . . ? C8 C7 Li2 O3 73.0(2) . . . . ? O2 C7 Li2 O4 -163.90(16) . . . . ? C12 C7 Li2 O4 79.80(14) . . . . ? C8 C7 Li2 O4 -47.43(15) . . . . ? C12 C7 Li2 O2 -116.29(15) . . . . ? C8 C7 Li2 O2 116.47(15) . . . . ? O2 C7 Li2 Li1 42.24(10) . . . . ? C12 C7 Li2 Li1 -74.05(13) . . . . ? C8 C7 Li2 Li1 158.71(13) . . . . ? O2 C7 Li2 Li1 -8.81(9) . . . 2_566 ? C12 C7 Li2 Li1 -125.10(12) . . . 2_566 ? C8 C7 Li2 Li1 107.66(12) . . . 2_566 ? C35 O5 Li3 O6 149.4(2) . . . 2_655 ? Li4 O5 Li3 O6 -91.8(3) . . . 2_655 ? C35 O5 Li3 O6 -96.33(15) . . . . ? Li4 O5 Li3 O6 22.47(13) . . . . ? C35 O5 Li3 P2 -17.04(15) . . . . ? Li4 O5 Li3 P2 101.76(11) . . . . ? C35 O5 Li3 Li4 -118.81(16) . . . . ? C35 O5 Li3 Li3 -131.2(2) . . . 2_655 ? Li4 O5 Li3 Li3 -12.4(3) . . . 2_655 ? C35 O5 Li3 Li4 143.3(11) . . . 2_655 ? Li4 O5 Li3 Li4 -97.9(12) . . . 2_655 ? C41 O6 Li3 O6 -146.01(14) . . . 2_655 ? Li3 O6 Li3 O6 0.0 2_655 . . 2_655 ? Li4 O6 Li3 O6 123.16(14) . . . 2_655 ? C41 O6 Li3 O5 69.81(16) . . . . ? Li3 O6 Li3 O5 -144.18(19) 2_655 . . . ? Li4 O6 Li3 O5 -21.02(12) . . . . ? C41 O6 Li3 P2 -8.61(14) . . . . ? Li3 O6 Li3 P2 137.40(14) 2_655 . . . ? Li4 O6 Li3 P2 -99.44(10) . . . . ? C41 O6 Li3 Li4 90.83(15) . . . . ? Li3 O6 Li3 Li4 -123.16(14) 2_655 . . . ? C41 O6 Li3 Li3 -146.01(14) . . . 2_655 ? Li4 O6 Li3 Li3 123.16(14) . . . 2_655 ? C41 O6 Li3 Li4 -116.15(13) . . . 2_655 ? Li3 O6 Li3 Li4 29.87(9) 2_655 . . 2_655 ? Li4 O6 Li3 Li4 153.03(8) . . . 2_655 ? C40 P2 Li3 O6 -157.3(2) . . . 2_655 ? C47 P2 Li3 O6 -30.7(3) . . . 2_655 ? C46 P2 Li3 O6 100.9(2) . . . 2_655 ? C40 P2 Li3 O5 9.92(10) . . . . ? C47 P2 Li3 O5 136.47(12) . . . . ? C46 P2 Li3 O5 -91.93(9) . . . . ? C40 P2 Li3 O6 109.46(9) . . . . ? C47 P2 Li3 O6 -123.99(13) . . . . ? C46 P2 Li3 O6 7.62(9) . . . . ? C40 P2 Li3 Li4 57.28(11) . . . . ? C47 P2 Li3 Li4 -176.17(12) . . . . ? C46 P2 Li3 Li4 -44.57(11) . . . . ? C40 P2 Li3 Li3 142.00(16) . . . 2_655 ? C47 P2 Li3 Li3 -91.4(2) . . . 2_655 ? C46 P2 Li3 Li3 40.15(17) . . . 2_655 ? C40 P2 Li3 Li4 -167.67(9) . . . 2_655 ? C47 P2 Li3 Li4 -41.12(19) . . . 2_655 ? C46 P2 Li3 Li4 90.48(10) . . . 2_655 ? C35 O5 Li4 O8 -25.8(2) . . . . ? Li3 O5 Li4 O8 -153.20(17) . . . . ? C35 O5 Li4 O7 -141.55(13) . . . . ? Li3 O5 Li4 O7 91.03(14) . . . . ? C35 O5 Li4 O6 105.45(14) . . . . ? Li3 O5 Li4 O6 -21.97(12) . . . . ? C35 O5 Li4 Li3 127.42(15) . . . . ? C35 O5 Li4 C41 75.69(14) . . . . ? Li3 O5 Li4 C41 -51.73(12) . . . . ? C35 O5 Li4 Li3 134.29(12) . . . 2_655 ? Li3 O5 Li4 Li3 6.87(14) . . . 2_655 ? C84 O8 Li4 O5 -113.83(18) . . . . ? C81 O8 Li4 O5 61.1(2) . . . . ? C84 O8 Li4 O7 1.0(2) . . . . ? C81 O8 Li4 O7 175.86(17) . . . . ? C84 O8 Li4 O6 129.83(18) . . . . ? C81 O8 Li4 O6 -55.3(3) . . . . ? C84 O8 Li4 Li3 -159.9(3) . . . . ? C81 O8 Li4 Li3 15.0(4) . . . . ? C84 O8 Li4 C41 140.48(15) . . . . ? C81 O8 Li4 C41 -44.6(2) . . . . ? C84 O8 Li4 Li3 101.2(3) . . . 2_655 ? C81 O8 Li4 Li3 -83.9(3) . . . 2_655 ? C77 O7 Li4 O5 168.88(15) . . . . ? C80 O7 Li4 O5 -11.6(2) . . . . ? C77 O7 Li4 O8 48.5(2) . . . . ? C80 O7 Li4 O8 -131.93(15) . . . . ? C77 O7 Li4 O6 -87.8(2) . . . . ? C80 O7 Li4 O6 91.76(17) . . . . ? C77 O7 Li4 Li3 -140.62(16) . . . . ? C80 O7 Li4 Li3 38.94(18) . . . . ? C77 O7 Li4 C41 -66.9(3) . . . . ? C80 O7 Li4 C41 112.66(19) . . . . ? C77 O7 Li4 Li3 -95.76(17) . . . 2_655 ? C80 O7 Li4 Li3 83.80(14) . . . 2_655 ? C41 O6 Li4 O5 -102.23(13) . . . . ? Li3 O6 Li4 O5 92.02(15) 2_655 . . . ? Li3 O6 Li4 O5 21.22(12) . . . . ? C41 O6 Li4 O8 21.75(19) . . . . ? Li3 O6 Li4 O8 -144.00(17) 2_655 . . . ? Li3 O6 Li4 O8 145.20(19) . . . . ? C41 O6 Li4 O7 149.08(13) . . . . ? Li3 O6 Li4 O7 -16.66(19) 2_655 . . . ? Li3 O6 Li4 O7 -87.47(15) . . . . ? C41 O6 Li4 Li3 -123.45(12) . . . . ? Li3 O6 Li4 Li3 70.80(16) 2_655 . . . ? Li3 O6 Li4 C41 -165.74(16) 2_655 . . . ? Li3 O6 Li4 C41 123.45(12) . . . . ? C41 O6 Li4 Li3 165.74(16) . . . 2_655 ? Li3 O6 Li4 Li3 -70.80(16) . . . 2_655 ? O6 Li3 Li4 O5 131.86(19) 2_655 . . . ? O6 Li3 Li4 O5 -151.75(15) . . . . ? P2 Li3 Li4 O5 -74.67(10) . . . . ? Li3 Li3 Li4 O5 170.82(19) 2_655 . . . ? Li4 Li3 Li4 O5 170.82(19) 2_655 . . . ? O6 Li3 Li4 O8 -167.6(3) 2_655 . . . ? O5 Li3 Li4 O8 60.6(3) . . . . ? O6 Li3 Li4 O8 -91.2(3) . . . . ? P2 Li3 Li4 O8 -14.1(4) . . . . ? Li3 Li3 Li4 O8 -128.6(3) 2_655 . . . ? Li4 Li3 Li4 O8 -128.6(3) 2_655 . . . ? O6 Li3 Li4 O7 31.1(2) 2_655 . . . ? O5 Li3 Li4 O7 -100.77(14) . . . . ? O6 Li3 Li4 O7 107.48(14) . . . . ? P2 Li3 Li4 O7 -175.45(11) . . . . ? Li3 Li3 Li4 O7 70.05(16) 2_655 . . . ? Li4 Li3 Li4 O7 70.05(16) 2_655 . . . ? O6 Li3 Li4 O6 -76.40(16) 2_655 . . . ? O5 Li3 Li4 O6 151.75(15) . . . . ? P2 Li3 Li4 O6 77.08(10) . . . . ? Li3 Li3 Li4 O6 -37.43(10) 2_655 . . . ? Li4 Li3 Li4 O6 -37.43(10) 2_655 . . . ? O6 Li3 Li4 C41 -102.37(16) 2_655 . . . ? O5 Li3 Li4 C41 125.78(13) . . . . ? O6 Li3 Li4 C41 -25.97(6) . . . . ? P2 Li3 Li4 C41 51.10(8) . . . . ? Li3 Li3 Li4 C41 -63.41(12) 2_655 . . . ? Li4 Li3 Li4 C41 -63.41(12) 2_655 . . . ? O6 Li3 Li4 Li3 -38.96(10) 2_655 . . 2_655 ? O5 Li3 Li4 Li3 -170.82(19) . . . 2_655 ? O6 Li3 Li4 Li3 37.43(10) . . . 2_655 ? P2 Li3 Li4 Li3 114.51(16) . . . 2_655 ? Li4 Li3 Li4 Li3 0.0 2_655 . . 2_655 ? O6 C41 Li4 O5 82.80(13) . . . . ? C46 C41 Li4 O5 -34.38(15) . . . . ? C42 C41 Li4 O5 -161.99(13) . . . . ? O6 C41 Li4 O8 -161.94(16) . . . . ? C46 C41 Li4 O8 80.88(14) . . . . ? C42 C41 Li4 O8 -46.73(16) . . . . ? O6 C41 Li4 O7 -42.40(18) . . . . ? C46 C41 Li4 O7 -159.58(18) . . . . ? C42 C41 Li4 O7 72.8(2) . . . . ? C46 C41 Li4 O6 -117.18(14) . . . . ? C42 C41 Li4 O6 115.21(15) . . . . ? O6 C41 Li4 Li3 43.77(10) . . . . ? C46 C41 Li4 Li3 -73.41(12) . . . . ? C42 C41 Li4 Li3 158.97(13) . . . . ? O6 C41 Li4 Li3 -8.00(9) . . . 2_655 ? C46 C41 Li4 Li3 -125.18(12) . . . 2_655 ? C42 C41 Li4 Li3 107.20(13) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.947 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.049 data_'[[OPO]Li2(H2O)]2' _database_code_depnum_ccdc_archive 'CCDC 653593' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H118 Li4 O8 P2' _chemical_formula_sum 'C86 H118 Li4 O8 P2' _chemical_formula_weight 1369.50 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.2530(11) _cell_length_b 19.8120(16) _cell_length_c 20.8950(19) _cell_angle_alpha 90.00 _cell_angle_beta 102.419(3) _cell_angle_gamma 90.00 _cell_volume 4145.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12229 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 26.73 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.104 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8924 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details Semi-empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/ADSC CCD' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23709 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 26.73 _reflns_number_total 8047 _reflns_number_gt 6000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'd*TREK (MSC, 1997)' _computing_cell_refinement 'd*TREK (MSC, 1997)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2004)' _computing_structure_solution 'SIR97 (Altomere et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1197P)^2^+2.4260P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8047 _refine_ls_number_parameters 475 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.2212 _refine_ls_wR_factor_gt 0.1980 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6521(2) 0.11502(12) 0.61067(11) 0.0229(5) Uani 1 1 d . . . C2 C 0.7214(3) 0.17600(12) 0.63443(12) 0.0256(5) Uani 1 1 d . . . C3 C 0.7222(3) 0.19629(12) 0.69828(12) 0.0274(6) Uani 1 1 d . . . H3 H 0.7691 0.2353 0.7136 0.033 Uiso 1 1 calc R . . C4 C 0.6571(3) 0.16196(12) 0.74117(12) 0.0274(6) Uani 1 1 d . . . C5 C 0.5844(3) 0.10521(12) 0.71613(11) 0.0254(5) Uani 1 1 d . . . H5 H 0.5381 0.0816 0.7427 0.031 Uiso 1 1 calc R . . C6 C 0.5786(2) 0.08234(11) 0.65221(11) 0.0218(5) Uani 1 1 d . . . C7 C 0.3487(2) 0.09987(12) 0.37549(11) 0.0228(5) Uani 1 1 d . . . C8 C 0.2816(3) 0.15945(13) 0.34648(12) 0.0278(6) Uani 1 1 d . . . C9 C 0.2889(3) 0.17530(13) 0.28271(13) 0.0300(6) Uani 1 1 d . . . H9 H 0.2428 0.2133 0.2638 0.036 Uiso 1 1 calc R . . C10 C 0.3611(3) 0.13797(13) 0.24455(12) 0.0294(6) Uani 1 1 d . . . C11 C 0.4325(3) 0.08344(12) 0.27485(12) 0.0260(5) Uani 1 1 d . . . H11 H 0.4841 0.0585 0.2519 0.031 Uiso 1 1 calc R . . C12 C 0.5705(2) -0.06450(11) 0.66073(11) 0.0228(5) Uani 1 1 d . . . C13 C 0.3296(3) 0.01506(13) 0.66036(12) 0.0267(6) Uani 1 1 d . . . H13 H 0.3566 0.0186 0.7082 0.032 Uiso 1 1 calc R . . C14 C 0.2524(3) 0.07898(14) 0.63325(15) 0.0372(7) Uani 1 1 d . . . H14A H 0.2296 0.0768 0.5863 0.056 Uiso 1 1 calc R . . H14B H 0.3070 0.1180 0.6467 0.056 Uiso 1 1 calc R . . H14C H 0.1722 0.0821 0.6498 0.056 Uiso 1 1 calc R . . C15 C 0.2428(3) -0.04819(14) 0.64272(14) 0.0360(6) Uani 1 1 d . . . H15A H 0.1629 -0.0437 0.6593 0.054 Uiso 1 1 calc R . . H15B H 0.2916 -0.0872 0.6619 0.054 Uiso 1 1 calc R . . H15C H 0.2196 -0.0532 0.5960 0.054 Uiso 1 1 calc R . . C16 C 0.7913(3) 0.21787(13) 0.58978(13) 0.0331(6) Uani 1 1 d . . . C17 C 0.8544(4) 0.28246(15) 0.62383(16) 0.0460(8) Uani 1 1 d . . . H17A H 0.7865 0.3094 0.6366 0.069 Uiso 1 1 calc R . . H17B H 0.8953 0.3077 0.5942 0.069 Uiso 1 1 calc R . . H17C H 0.9209 0.2706 0.6620 0.069 Uiso 1 1 calc R . . C18 C 0.6889(3) 0.23980(15) 0.52883(15) 0.0458(8) Uani 1 1 d . . . H18A H 0.6523 0.2006 0.5044 0.069 Uiso 1 1 calc R . . H18B H 0.7316 0.2679 0.5020 0.069 Uiso 1 1 calc R . . H18C H 0.6184 0.2646 0.5418 0.069 Uiso 1 1 calc R . . C19 C 0.9045(3) 0.17713(16) 0.56994(18) 0.0498(9) Uani 1 1 d . . . H19A H 0.9658 0.1618 0.6086 0.075 Uiso 1 1 calc R . . H19B H 0.9508 0.2053 0.5447 0.075 Uiso 1 1 calc R . . H19C H 0.8673 0.1389 0.5441 0.075 Uiso 1 1 calc R . . C20 C 0.6676(3) 0.18433(14) 0.81239(13) 0.0340(6) Uani 1 1 d . . . C21 C 0.7056(5) 0.25849(17) 0.82279(17) 0.0662(12) Uani 1 1 d . . . H21A H 0.6400 0.2859 0.7947 0.099 Uiso 1 1 calc R . . H21B H 0.7914 0.2659 0.8125 0.099 Uiso 1 1 calc R . . H21C H 0.7095 0.2705 0.8677 0.099 Uiso 1 1 calc R . . C22 C 0.5348(4) 0.1749(2) 0.83296(17) 0.0643(11) Uani 1 1 d . . . H22A H 0.4652 0.1969 0.8019 0.096 Uiso 1 1 calc R . . H22B H 0.5405 0.1942 0.8756 0.096 Uiso 1 1 calc R . . H22C H 0.5152 0.1276 0.8343 0.096 Uiso 1 1 calc R . . C23 C 0.7734(4) 0.1408(2) 0.85640(15) 0.0578(10) Uani 1 1 d . . . H23A H 0.7843 0.1554 0.9010 0.087 Uiso 1 1 calc R . . H23B H 0.8567 0.1452 0.8429 0.087 Uiso 1 1 calc R . . H23C H 0.7456 0.0944 0.8529 0.087 Uiso 1 1 calc R . . C24 C 0.2036(3) 0.20391(13) 0.38560(14) 0.0351(6) Uani 1 1 d . . . C25 C 0.0856(3) 0.16455(16) 0.40225(17) 0.0472(8) Uani 1 1 d . . . H25A H 0.0348 0.1939 0.4241 0.071 Uiso 1 1 calc R . . H25B H 0.1191 0.1273 0.4304 0.071 Uiso 1 1 calc R . . H25C H 0.0295 0.1479 0.3626 0.071 Uiso 1 1 calc R . . C26 C 0.2970(4) 0.22805(16) 0.44888(16) 0.0484(8) Uani 1 1 d . . . H26A H 0.3709 0.2521 0.4383 0.073 Uiso 1 1 calc R . . H26B H 0.3297 0.1898 0.4758 0.073 Uiso 1 1 calc R . . H26C H 0.2490 0.2574 0.4722 0.073 Uiso 1 1 calc R . . C27 C 0.1463(4) 0.26695(15) 0.34694(17) 0.0506(9) Uani 1 1 d . . . H27A H 0.2172 0.2915 0.3341 0.076 Uiso 1 1 calc R . . H27B H 0.1042 0.2951 0.3740 0.076 Uiso 1 1 calc R . . H27C H 0.0818 0.2537 0.3086 0.076 Uiso 1 1 calc R . . C28 C 0.3557(3) 0.15514(15) 0.17228(13) 0.0395(7) Uani 1 1 d . . . C29 C 0.3397(6) 0.2317(2) 0.1592(2) 0.0876(16) Uani 1 1 d . . . H29A H 0.2533 0.2459 0.1647 0.131 Uiso 1 1 calc R . . H29B H 0.3483 0.2412 0.1153 0.131 Uiso 1 1 calc R . . H29C H 0.4076 0.2556 0.1896 0.131 Uiso 1 1 calc R . . C30 C 0.4841(4) 0.1360(3) 0.15212(18) 0.0801(14) Uani 1 1 d . . . H30A H 0.4783 0.1485 0.1072 0.120 Uiso 1 1 calc R . . H30B H 0.4978 0.0882 0.1570 0.120 Uiso 1 1 calc R . . H30C H 0.5577 0.1593 0.1794 0.120 Uiso 1 1 calc R . . C31 C 0.2393(5) 0.1192(3) 0.13055(17) 0.0817(14) Uani 1 1 d . . . H31A H 0.1587 0.1321 0.1437 0.123 Uiso 1 1 calc R . . H31B H 0.2518 0.0713 0.1357 0.123 Uiso 1 1 calc R . . H31C H 0.2327 0.1311 0.0854 0.123 Uiso 1 1 calc R . . C51 C 0.9438(3) 0.04261(16) 0.73546(15) 0.0444(7) Uani 1 1 d . . . H51 H 0.8695 0.0658 0.7125 0.053 Uiso 1 1 calc R . . C52 C 0.9382(3) -0.02581(17) 0.74305(15) 0.0447(7) Uani 1 1 d . . . H52 H 0.8600 -0.0492 0.7254 0.054 Uiso 1 1 calc R . . C53 C 1.0485(4) -0.06003(18) 0.77693(17) 0.0556(9) Uani 1 1 d . . . H53 H 1.0457 -0.1067 0.7814 0.067 Uiso 1 1 calc R . . C54 C 1.1626(4) -0.0251(2) 0.80412(17) 0.0612(10) Uani 1 1 d . . . H54 H 1.2366 -0.0479 0.8280 0.073 Uiso 1 1 calc R . . C55 C 1.1669(4) 0.0434(2) 0.79596(17) 0.0597(10) Uani 1 1 d . . . H55 H 1.2444 0.0670 0.8140 0.072 Uiso 1 1 calc R . . C56 C 1.0584(4) 0.07704(17) 0.76157(16) 0.0524(9) Uani 1 1 d . . . H56 H 1.0623 0.1235 0.7559 0.063 Uiso 1 1 calc R . . C101 C 0.0161(7) 0.0298(3) 0.9425(3) 0.1068(19) Uani 1 1 d . . . H101 H 0.0266 0.0498 0.9037 0.128 Uiso 1 1 calc R . . C100 C 0.0282(6) -0.0392(3) 0.9510(3) 0.1059(19) Uani 1 1 d . . . H100 H 0.0478 -0.0659 0.9177 0.127 Uiso 1 1 calc R . . C102 C -0.0119(5) 0.0685(4) 0.9927(3) 0.1044(19) Uani 1 1 d . . . H102 H -0.0196 0.1151 0.9879 0.125 Uiso 1 1 calc R . . C200 C 0.3962(13) -0.0398(7) 1.0051(5) 0.149(4) Uani 1 1 d . . . H200 H 0.3250 -0.0677 1.0085 0.179 Uiso 1 1 calc R . . C201 C 0.3747(11) 0.0235(8) 0.9816(4) 0.148(3) Uani 1 1 d . . . H201 H 0.2879 0.0399 0.9691 0.177 Uiso 1 1 calc R . . C202 C 0.5243(18) -0.0622(4) 1.0238(4) 0.147(4) Uani 1 1 d . . . H202 H 0.5405 -0.1055 1.0407 0.176 Uiso 1 1 calc R . . Li1 Li 0.4974(4) 0.0680(2) 0.49534(19) 0.0251(9) Uani 1 1 d . . . Li2 Li 0.7164(5) 0.0030(2) 0.5307(2) 0.0274(9) Uani 1 1 d . . . O1 O 0.65616(17) 0.08972(8) 0.55286(8) 0.0250(4) Uani 1 1 d . A . O2 O 0.33695(17) 0.07816(8) 0.43362(8) 0.0258(4) Uani 1 1 d . . . O3 O 0.42739(17) 0.00421(7) 0.55239(8) 0.0214(4) Uani 1 1 d . . . P1 P 0.47825(6) 0.00865(3) 0.62621(3) 0.01983(19) Uani 1 1 d . . . O5 O 0.9135(6) 0.0055(3) 0.5625(16) 0.050(4) Uani 0.56(5) 1 d P A 1 O4 O 0.9142(8) 0.0034(4) 0.5296(15) 0.042(4) Uani 0.44(5) 1 d P A 2 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 C1 0.0212(13) 0.0224(11) 0.0248(12) -0.0011(9) 0.0045(10) 0.0007(10) C2 0.0258(14) 0.0228(11) 0.0294(13) -0.0024(10) 0.0085(10) -0.0006(10) C3 0.0277(14) 0.0207(11) 0.0336(13) -0.0067(10) 0.0062(11) -0.0015(10) C4 0.0281(14) 0.0265(12) 0.0276(13) -0.0054(10) 0.0061(10) 0.0017(11) C5 0.0273(14) 0.0269(12) 0.0231(12) -0.0011(10) 0.0075(10) 0.0010(10) C6 0.0235(13) 0.0197(11) 0.0228(12) -0.0003(9) 0.0063(10) 0.0031(9) C7 0.0211(13) 0.0227(11) 0.0241(12) 0.0026(9) 0.0038(10) -0.0028(10) C8 0.0252(14) 0.0273(12) 0.0311(13) 0.0042(10) 0.0069(11) 0.0015(10) C9 0.0297(15) 0.0249(12) 0.0344(14) 0.0089(10) 0.0045(11) 0.0012(11) C10 0.0326(15) 0.0289(12) 0.0266(13) 0.0062(10) 0.0060(11) -0.0023(11) C11 0.0316(15) 0.0237(11) 0.0238(12) 0.0014(9) 0.0085(10) -0.0023(10) C12 0.0230(13) 0.0209(11) 0.0248(12) 0.0011(9) 0.0060(10) -0.0032(9) C13 0.0244(14) 0.0324(13) 0.0258(13) 0.0005(10) 0.0109(11) -0.0001(11) C14 0.0283(16) 0.0384(15) 0.0475(17) -0.0033(13) 0.0135(13) 0.0080(12) C15 0.0295(16) 0.0414(15) 0.0389(15) 0.0051(12) 0.0116(12) -0.0070(12) C16 0.0378(16) 0.0270(13) 0.0370(15) -0.0047(11) 0.0135(12) -0.0095(12) C17 0.059(2) 0.0349(15) 0.0486(18) -0.0076(13) 0.0210(16) -0.0211(15) C18 0.063(2) 0.0371(15) 0.0381(16) 0.0074(13) 0.0118(15) -0.0126(15) C19 0.047(2) 0.0444(17) 0.069(2) -0.0140(16) 0.0364(17) -0.0149(15) C20 0.0409(17) 0.0349(14) 0.0269(13) -0.0107(11) 0.0088(12) -0.0019(12) C21 0.119(4) 0.0442(19) 0.0379(18) -0.0186(15) 0.021(2) -0.013(2) C22 0.057(2) 0.098(3) 0.0444(19) -0.0304(19) 0.0261(17) -0.007(2) C23 0.070(3) 0.070(2) 0.0291(16) -0.0070(15) 0.0014(16) 0.0165(19) C24 0.0375(17) 0.0287(13) 0.0413(15) 0.0073(11) 0.0130(13) 0.0109(12) C25 0.0369(18) 0.0485(18) 0.062(2) 0.0173(15) 0.0235(15) 0.0145(15) C26 0.060(2) 0.0376(16) 0.0489(18) -0.0066(14) 0.0136(16) 0.0136(15) C27 0.060(2) 0.0365(16) 0.061(2) 0.0158(15) 0.0268(17) 0.0231(15) C28 0.0476(19) 0.0436(16) 0.0277(14) 0.0118(12) 0.0088(13) 0.0006(14) C29 0.159(5) 0.060(2) 0.051(2) 0.0275(19) 0.038(3) 0.014(3) C30 0.069(3) 0.135(4) 0.042(2) 0.037(2) 0.0244(19) 0.013(3) C31 0.091(3) 0.113(4) 0.0332(18) 0.008(2) -0.0028(19) -0.035(3) C51 0.0419(19) 0.0496(18) 0.0400(16) -0.0027(14) 0.0050(14) 0.0113(15) C52 0.0364(18) 0.0543(18) 0.0426(17) -0.0007(14) 0.0068(14) -0.0107(15) C53 0.073(3) 0.0425(18) 0.054(2) 0.0117(15) 0.0198(19) 0.0066(17) C54 0.044(2) 0.096(3) 0.0429(19) 0.007(2) 0.0061(16) 0.022(2) C55 0.037(2) 0.097(3) 0.0462(19) -0.023(2) 0.0121(16) -0.022(2) C56 0.075(3) 0.0388(16) 0.0487(19) -0.0120(14) 0.0244(18) -0.0113(17) C101 0.123(5) 0.128(5) 0.073(3) 0.016(3) 0.027(3) 0.035(4) C100 0.125(5) 0.124(5) 0.068(3) 0.009(3) 0.018(3) 0.039(4) C102 0.108(5) 0.126(5) 0.079(4) 0.008(3) 0.020(3) 0.026(4) C200 0.164(10) 0.166(10) 0.130(7) 0.007(6) 0.059(7) -0.064(7) C201 0.149(8) 0.201(10) 0.094(5) -0.020(6) 0.028(5) -0.008(8) C202 0.271(14) 0.095(5) 0.082(4) 0.004(4) 0.053(7) -0.029(8) Li1 0.027(2) 0.0242(19) 0.026(2) 0.0009(16) 0.0082(17) -0.0006(17) Li2 0.027(2) 0.030(2) 0.027(2) 0.0005(17) 0.0082(18) 0.0002(17) O1 0.0278(10) 0.0258(8) 0.0240(8) -0.0057(7) 0.0115(7) -0.0061(7) O2 0.0249(10) 0.0295(9) 0.0249(9) 0.0062(7) 0.0095(7) 0.0060(7) O3 0.0218(9) 0.0218(8) 0.0217(9) -0.0011(6) 0.0070(7) -0.0004(6) P1 0.0203(4) 0.0198(3) 0.0206(3) -0.0002(2) 0.0071(3) -0.0006(2) O5 0.024(2) 0.054(3) 0.069(12) 0.002(3) 0.007(3) 0.0005(18) O4 0.025(3) 0.057(4) 0.043(10) 0.005(4) 0.003(3) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.317(3) . ? C1 C6 1.422(3) . ? C1 C2 1.435(3) . ? C2 C3 1.392(3) . ? C2 C16 1.536(3) . ? C3 C4 1.403(4) . ? C3 H3 0.9300 . ? C4 C5 1.388(3) . ? C4 C20 1.534(3) . ? C5 C6 1.399(3) . ? C5 H5 0.9300 . ? C6 P1 1.801(2) . ? C7 O2 1.318(3) . ? C7 C12 1.421(3) 3_656 ? C7 C8 1.433(3) . ? C8 C9 1.386(4) . ? C8 C24 1.538(4) . ? C9 C10 1.409(4) . ? C9 H9 0.9300 . ? C10 C11 1.380(4) . ? C10 C28 1.537(3) . ? C11 C12 1.404(3) 3_656 ? C11 H11 0.9300 . ? C12 C11 1.404(3) 3_656 ? C12 C7 1.421(3) 3_656 ? C12 P1 1.795(2) . ? C13 C15 1.535(4) . ? C13 C14 1.536(4) . ? C13 P1 1.821(3) . ? C13 H13 0.9800 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C18 1.529(4) . ? C16 C17 1.538(4) . ? C16 C19 1.542(4) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.524(4) . ? C20 C22 1.524(4) . ? C20 C23 1.529(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C26 1.533(4) . ? C24 C27 1.534(4) . ? C24 C25 1.540(4) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C31 1.498(5) . ? C28 C30 1.514(5) . ? C28 C29 1.544(5) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C51 C56 1.366(5) . ? C51 C52 1.368(5) . ? C51 H51 0.9300 . ? C52 C53 1.377(5) . ? C52 H52 0.9300 . ? C53 C54 1.372(6) . ? C53 H53 0.9300 . ? C54 C55 1.370(6) . ? C54 H54 0.9300 . ? C55 C56 1.362(5) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C101 C102 1.378(8) . ? C101 C100 1.382(9) . ? C101 H101 0.9300 . ? C100 C102 1.353(7) 3_557 ? C100 H100 0.9300 . ? C102 C100 1.353(7) 3_557 ? C102 H102 0.9300 . ? C200 C201 1.349(13) . ? C200 C202 1.361(13) . ? C200 H200 0.9300 . ? C201 C202 1.312(11) 3_657 ? C201 H201 0.9300 . ? C202 C201 1.312(11) 3_657 ? C202 H202 0.9300 . ? Li1 O1 1.854(4) . ? Li1 O2 1.870(4) . ? Li1 O3 1.975(4) . ? Li1 O3 1.991(4) 3_656 ? Li1 Li2 2.561(6) 3_656 ? Li1 Li1 2.699(8) 3_656 ? Li1 P1 3.015(4) 3_656 ? Li2 O2 1.901(4) 3_656 ? Li2 O1 1.916(4) . ? Li2 O5 1.988(9) . ? Li2 O3 2.026(5) 3_656 ? Li2 O4 2.033(13) . ? Li2 Li1 2.561(6) 3_656 ? O2 Li2 1.901(4) 3_656 ? O3 P1 1.5209(17) . ? O3 Li1 1.991(4) 3_656 ? O3 Li2 2.026(5) 3_656 ? P1 Li1 3.015(4) 3_656 ? 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 O1 C1 C6 120.8(2) . . ? O1 C1 C2 121.8(2) . . ? C6 C1 C2 117.4(2) . . ? C3 C2 C1 118.4(2) . . ? C3 C2 C16 121.3(2) . . ? C1 C2 C16 120.4(2) . . ? C2 C3 C4 124.5(2) . . ? C2 C3 H3 117.7 . . ? C4 C3 H3 117.7 . . ? C5 C4 C3 116.3(2) . . ? C5 C4 C20 121.3(2) . . ? C3 C4 C20 122.4(2) . . ? C4 C5 C6 122.1(2) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 121.0(2) . . ? C5 C6 P1 117.05(18) . . ? C1 C6 P1 121.88(17) . . ? O2 C7 C12 120.6(2) . 3_656 ? O2 C7 C8 121.9(2) . . ? C12 C7 C8 117.5(2) 3_656 . ? C9 C8 C7 118.2(2) . . ? C9 C8 C24 121.5(2) . . ? C7 C8 C24 120.3(2) . . ? C8 C9 C10 124.6(2) . . ? C8 C9 H9 117.7 . . ? C10 C9 H9 117.7 . . ? C11 C10 C9 116.3(2) . . ? C11 C10 C28 121.8(2) . . ? C9 C10 C28 121.9(2) . . ? C10 C11 C12 122.0(2) . 3_656 ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 3_656 . ? C11 C12 C7 120.9(2) 3_656 3_656 ? C11 C12 P1 118.88(18) 3_656 . ? C7 C12 P1 120.08(17) 3_656 . ? C15 C13 C14 111.0(2) . . ? C15 C13 P1 109.86(18) . . ? C14 C13 P1 108.74(18) . . ? C15 C13 H13 109.1 . . ? C14 C13 H13 109.1 . . ? P1 C13 H13 109.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C2 109.4(2) . . ? C18 C16 C17 107.1(2) . . ? C2 C16 C17 111.9(2) . . ? C18 C16 C19 110.3(3) . . ? C2 C16 C19 110.9(2) . . ? C17 C16 C19 107.1(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 107.2(3) . . ? C21 C20 C23 109.3(3) . . ? C22 C20 C23 108.8(3) . . ? C21 C20 C4 112.3(2) . . ? C22 C20 C4 110.9(2) . . ? C23 C20 C4 108.2(2) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 C27 107.3(3) . . ? C26 C24 C8 109.7(2) . . ? C27 C24 C8 111.7(2) . . ? C26 C24 C25 109.8(3) . . ? C27 C24 C25 107.5(2) . . ? C8 C24 C25 110.7(2) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C31 C28 C30 110.6(3) . . ? C31 C28 C10 108.8(3) . . ? C30 C28 C10 111.6(3) . . ? C31 C28 C29 108.8(3) . . ? C30 C28 C29 105.2(3) . . ? C10 C28 C29 111.8(3) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C56 C51 C52 120.2(3) . . ? C56 C51 H51 119.9 . . ? C52 C51 H51 119.9 . . ? C51 C52 C53 119.8(3) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? C54 C53 C52 119.8(3) . . ? C54 C53 H53 120.1 . . ? C52 C53 H53 120.1 . . ? C55 C54 C53 119.7(3) . . ? C55 C54 H54 120.2 . . ? C53 C54 H54 120.2 . . ? C56 C55 C54 120.4(3) . . ? C56 C55 H55 119.8 . . ? C54 C55 H55 119.8 . . ? C55 C56 C51 120.0(3) . . ? C55 C56 H56 120.0 . . ? C51 C56 H56 120.0 . . ? C102 C101 C100 118.7(5) . . ? C102 C101 H101 120.6 . . ? C100 C101 H101 120.6 . . ? C102 C100 C101 120.7(6) 3_557 . ? C102 C100 H100 119.6 3_557 . ? C101 C100 H100 119.6 . . ? C100 C102 C101 120.5(6) 3_557 . ? C100 C102 H102 119.7 3_557 . ? C101 C102 H102 119.7 . . ? C201 C200 C202 118.6(9) . . ? C201 C200 H200 120.7 . . ? C202 C200 H200 120.7 . . ? C202 C201 C200 120.3(9) 3_657 . ? C202 C201 H201 119.9 3_657 . ? C200 C201 H201 119.9 . . ? C201 C202 C200 121.1(9) 3_657 . ? C201 C202 H202 119.4 3_657 . ? C200 C202 H202 119.4 . . ? O1 Li1 O2 160.2(3) . . ? O1 Li1 O3 98.04(19) . . ? O2 Li1 O3 96.05(19) . . ? O1 Li1 O3 96.37(19) . 3_656 ? O2 Li1 O3 96.33(19) . 3_656 ? O3 Li1 O3 94.21(18) . 3_656 ? O1 Li1 Li2 149.0(2) . 3_656 ? O2 Li1 Li2 47.72(14) . 3_656 ? O3 Li1 Li2 51.09(14) . 3_656 ? O3 Li1 Li2 84.58(17) 3_656 3_656 ? O1 Li1 Li1 100.6(2) . 3_656 ? O2 Li1 Li1 99.1(2) . 3_656 ? O3 Li1 Li1 47.36(13) . 3_656 ? O3 Li1 Li1 46.85(13) 3_656 3_656 ? Li2 Li1 Li1 58.06(17) 3_656 3_656 ? O1 Li1 P1 116.28(18) . 3_656 ? O2 Li1 P1 72.14(13) . 3_656 ? O3 Li1 P1 107.06(16) . 3_656 ? O3 Li1 P1 26.54(7) 3_656 3_656 ? Li2 Li1 P1 76.53(14) 3_656 3_656 ? Li1 Li1 P1 63.56(15) 3_656 3_656 ? O2 Li2 O1 121.9(2) 3_656 . ? O2 Li2 O5 104.3(5) 3_656 . ? O1 Li2 O5 104.7(5) . . ? O2 Li2 O3 93.4(2) 3_656 3_656 ? O1 Li2 O3 93.3(2) . 3_656 ? O5 Li2 O3 142.0(10) . 3_656 ? O2 Li2 O4 112.3(4) 3_656 . ? O1 Li2 O4 111.9(4) . . ? O5 Li2 O4 19.7(2) . . ? O3 Li2 O4 122.3(9) 3_656 . ? O2 Li2 Li1 46.72(14) 3_656 3_656 ? O1 Li2 Li1 103.8(2) . 3_656 ? O5 Li2 Li1 147.9(3) . 3_656 ? O3 Li2 Li1 49.31(14) 3_656 3_656 ? O4 Li2 Li1 144.1(5) . 3_656 ? C1 O1 Li1 119.10(19) . . ? C1 O1 Li2 129.7(2) . . ? Li1 O1 Li2 85.3(2) . . ? C7 O2 Li1 115.44(19) . . ? C7 O2 Li2 136.7(2) . 3_656 ? Li1 O2 Li2 85.56(19) . 3_656 ? P1 O3 Li1 119.04(15) . . ? P1 O3 Li1 117.66(15) . 3_656 ? Li1 O3 Li1 85.79(18) . 3_656 ? P1 O3 Li2 154.24(17) . 3_656 ? Li1 O3 Li2 79.60(17) . 3_656 ? Li1 O3 Li2 79.00(17) 3_656 3_656 ? O3 P1 C12 113.39(10) . . ? O3 P1 C6 113.68(10) . . ? C12 P1 C6 108.43(12) . . ? O3 P1 C13 105.54(11) . . ? C12 P1 C13 108.18(11) . . ? C6 P1 C13 107.28(11) . . ? O3 P1 Li1 35.80(10) . 3_656 ? C12 P1 Li1 78.47(11) . 3_656 ? C6 P1 Li1 121.11(11) . 3_656 ? C13 P1 Li1 126.38(12) . 3_656 ? 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 O1 C1 C2 C3 -174.3(2) . . . . ? C6 C1 C2 C3 5.4(4) . . . . ? O1 C1 C2 C16 6.4(4) . . . . ? C6 C1 C2 C16 -173.9(2) . . . . ? C1 C2 C3 C4 -1.5(4) . . . . ? C16 C2 C3 C4 177.9(2) . . . . ? C2 C3 C4 C5 -2.1(4) . . . . ? C2 C3 C4 C20 176.5(3) . . . . ? C3 C4 C5 C6 1.5(4) . . . . ? C20 C4 C5 C6 -177.1(2) . . . . ? C4 C5 C6 C1 2.6(4) . . . . ? C4 C5 C6 P1 -179.2(2) . . . . ? O1 C1 C6 C5 173.7(2) . . . . ? C2 C1 C6 C5 -6.1(4) . . . . ? O1 C1 C6 P1 -4.4(3) . . . . ? C2 C1 C6 P1 175.82(18) . . . . ? O2 C7 C8 C9 -174.0(2) . . . . ? C12 C7 C8 C9 6.1(4) 3_656 . . . ? O2 C7 C8 C24 5.8(4) . . . . ? C12 C7 C8 C24 -174.1(2) 3_656 . . . ? C7 C8 C9 C10 -1.9(4) . . . . ? C24 C8 C9 C10 178.3(3) . . . . ? C8 C9 C10 C11 -2.4(4) . . . . ? C8 C9 C10 C28 175.0(3) . . . . ? C9 C10 C11 C12 2.3(4) . . . 3_656 ? C28 C10 C11 C12 -175.1(2) . . . 3_656 ? C3 C2 C16 C18 -120.2(3) . . . . ? C1 C2 C16 C18 59.1(3) . . . . ? C3 C2 C16 C17 -1.6(4) . . . . ? C1 C2 C16 C17 177.7(3) . . . . ? C3 C2 C16 C19 117.9(3) . . . . ? C1 C2 C16 C19 -62.8(3) . . . . ? C5 C4 C20 C21 -159.0(3) . . . . ? C3 C4 C20 C21 22.4(4) . . . . ? C5 C4 C20 C22 -39.2(4) . . . . ? C3 C4 C20 C22 142.3(3) . . . . ? C5 C4 C20 C23 80.2(3) . . . . ? C3 C4 C20 C23 -98.4(3) . . . . ? C9 C8 C24 C26 -122.3(3) . . . . ? C7 C8 C24 C26 57.9(3) . . . . ? C9 C8 C24 C27 -3.5(4) . . . . ? C7 C8 C24 C27 176.8(3) . . . . ? C9 C8 C24 C25 116.3(3) . . . . ? C7 C8 C24 C25 -63.4(3) . . . . ? C11 C10 C28 C31 90.2(4) . . . . ? C9 C10 C28 C31 -87.1(4) . . . . ? C11 C10 C28 C30 -32.1(4) . . . . ? C9 C10 C28 C30 150.7(3) . . . . ? C11 C10 C28 C29 -149.6(3) . . . . ? C9 C10 C28 C29 33.1(4) . . . . ? C56 C51 C52 C53 -0.2(5) . . . . ? C51 C52 C53 C54 1.4(5) . . . . ? C52 C53 C54 C55 -1.6(5) . . . . ? C53 C54 C55 C56 0.6(5) . . . . ? C54 C55 C56 C51 0.6(5) . . . . ? C52 C51 C56 C55 -0.8(5) . . . . ? C102 C101 C100 C102 0.5(10) . . . 3_557 ? C100 C101 C102 C100 -0.5(10) . . . 3_557 ? C202 C200 C201 C202 0.9(15) . . . 3_657 ? C201 C200 C202 C201 -0.9(15) . . . 3_657 ? C6 C1 O1 Li1 51.6(3) . . . . ? C2 C1 O1 Li1 -128.7(3) . . . . ? C6 C1 O1 Li2 -58.3(4) . . . . ? C2 C1 O1 Li2 121.4(3) . . . . ? O2 Li1 O1 C1 77.7(7) . . . . ? O3 Li1 O1 C1 -57.4(2) . . . . ? O3 Li1 O1 C1 -152.61(18) 3_656 . . . ? Li2 Li1 O1 C1 -62.5(5) 3_656 . . . ? Li1 Li1 O1 C1 -105.4(2) 3_656 . . . ? P1 Li1 O1 C1 -171.02(16) 3_656 . . . ? O2 Li1 O1 Li2 -148.9(7) . . . . ? O3 Li1 O1 Li2 76.01(19) . . . . ? O3 Li1 O1 Li2 -19.17(18) 3_656 . . . ? Li2 Li1 O1 Li2 70.9(5) 3_656 . . . ? Li1 Li1 O1 Li2 28.0(2) 3_656 . . . ? P1 Li1 O1 Li2 -37.6(2) 3_656 . . . ? O2 Li2 O1 C1 47.1(4) 3_656 . . . ? O5 Li2 O1 C1 -70.6(10) . . . . ? O3 Li2 O1 C1 143.2(2) 3_656 . . . ? O4 Li2 O1 C1 -89.9(9) . . . . ? Li1 Li2 O1 C1 94.4(3) 3_656 . . . ? O2 Li2 O1 Li1 -77.3(3) 3_656 . . . ? O5 Li2 O1 Li1 165.0(9) . . . . ? O3 Li2 O1 Li1 18.74(18) 3_656 . . . ? O4 Li2 O1 Li1 145.6(9) . . . . ? Li1 Li2 O1 Li1 -30.1(2) 3_656 . . . ? C12 C7 O2 Li1 56.3(3) 3_656 . . . ? C8 C7 O2 Li1 -123.6(3) . . . . ? C12 C7 O2 Li2 -56.1(4) 3_656 . . 3_656 ? C8 C7 O2 Li2 124.0(3) . . . 3_656 ? O1 Li1 O2 C7 65.9(7) . . . . ? O3 Li1 O2 C7 -158.71(17) . . . . ? O3 Li1 O2 C7 -63.8(2) 3_656 . . . ? Li2 Li1 O2 C7 -140.5(2) 3_656 . . . ? Li1 Li1 O2 C7 -111.0(2) 3_656 . . . ? P1 Li1 O2 C7 -52.71(17) 3_656 . . . ? O1 Li1 O2 Li2 -153.5(7) . . . 3_656 ? O3 Li1 O2 Li2 -18.18(19) . . . 3_656 ? O3 Li1 O2 Li2 76.75(19) 3_656 . . 3_656 ? Li1 Li1 O2 Li2 29.5(2) 3_656 . . 3_656 ? P1 Li1 O2 Li2 87.83(14) 3_656 . . 3_656 ? O1 Li1 O3 P1 22.4(2) . . . . ? O2 Li1 O3 P1 -143.72(14) . . . . ? O3 Li1 O3 P1 119.45(17) 3_656 . . . ? Li2 Li1 O3 P1 -160.98(18) 3_656 . . . ? Li1 Li1 O3 P1 119.45(17) 3_656 . . . ? P1 Li1 O3 P1 143.13(11) 3_656 . . . ? O1 Li1 O3 Li1 -97.1(2) . . . 3_656 ? O2 Li1 O3 Li1 96.8(2) . . . 3_656 ? O3 Li1 O3 Li1 0.0 3_656 . . 3_656 ? Li2 Li1 O3 Li1 79.57(18) 3_656 . . 3_656 ? P1 Li1 O3 Li1 23.69(8) 3_656 . . 3_656 ? O1 Li1 O3 Li2 -176.6(2) . . . 3_656 ? O2 Li1 O3 Li2 17.26(18) . . . 3_656 ? O3 Li1 O3 Li2 -79.57(18) 3_656 . . 3_656 ? Li1 Li1 O3 Li2 -79.57(18) 3_656 . . 3_656 ? P1 Li1 O3 Li2 -55.89(17) 3_656 . . 3_656 ? Li1 O3 P1 C12 -114.90(18) . . . . ? Li1 O3 P1 C12 -13.57(19) 3_656 . . . ? Li2 O3 P1 C12 112.6(3) 3_656 . . . ? Li1 O3 P1 C6 9.6(2) . . . . ? Li1 O3 P1 C6 110.88(17) 3_656 . . . ? Li2 O3 P1 C6 -122.9(3) 3_656 . . . ? Li1 O3 P1 C13 126.87(18) . . . . ? Li1 O3 P1 C13 -131.81(17) 3_656 . . . ? Li2 O3 P1 C13 -5.6(4) 3_656 . . . ? Li1 O3 P1 Li1 -101.3(2) . . . 3_656 ? Li2 O3 P1 Li1 126.2(4) 3_656 . . 3_656 ? C11 C12 P1 O3 -149.42(19) 3_656 . . . ? C7 C12 P1 O3 34.4(2) 3_656 . . . ? C11 C12 P1 C6 83.3(2) 3_656 . . . ? C7 C12 P1 C6 -92.9(2) 3_656 . . . ? C11 C12 P1 C13 -32.7(2) 3_656 . . . ? C7 C12 P1 C13 151.07(19) 3_656 . . . ? C11 C12 P1 Li1 -157.5(2) 3_656 . . 3_656 ? C7 C12 P1 Li1 26.3(2) 3_656 . . 3_656 ? C5 C6 P1 O3 154.97(18) . . . . ? C1 C6 P1 O3 -26.8(2) . . . . ? C5 C6 P1 C12 -77.9(2) . . . . ? C1 C6 P1 C12 100.2(2) . . . . ? C5 C6 P1 C13 38.7(2) . . . . ? C1 C6 P1 C13 -143.1(2) . . . . ? C5 C6 P1 Li1 -165.36(18) . . . 3_656 ? C1 C6 P1 Li1 12.8(3) . . . 3_656 ? C15 C13 P1 O3 61.2(2) . . . . ? C14 C13 P1 O3 -60.5(2) . . . . ? C15 C13 P1 C12 -60.5(2) . . . . ? C14 C13 P1 C12 177.86(18) . . . . ? C15 C13 P1 C6 -177.24(18) . . . . ? C14 C13 P1 C6 61.1(2) . . . . ? C15 C13 P1 Li1 28.4(2) . . . 3_656 ? C14 C13 P1 Li1 -93.3(2) . . . 3_656 ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 0.645 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.073 data_'[[OPO]Li2]2(ArOLi)2' _database_code_depnum_ccdc_archive 'CCDC 653594' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C116 H154 Li6 O6 P2' _chemical_formula_sum 'C116 H154 Li6 O6 P2' _chemical_formula_weight 1747.97 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' 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9823(14) _cell_length_b 15.5897(17) _cell_length_c 16.1226(16) _cell_angle_alpha 103.686(2) _cell_angle_beta 101.950(1) _cell_angle_gamma 111.550(2) _cell_volume 2788.4(8) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3198 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.88 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 946 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8895 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details Semi-empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/ADSC CCD' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25238 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0729 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 27.88 _reflns_number_total 11576 _reflns_number_gt 8470 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'd*TREK (MSC, 1997)' _computing_cell_refinement 'd*TREK (MSC, 1997)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2004)' _computing_structure_solution 'SIR97 (Altomere et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1249P)^2^+2.3000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11576 _refine_ls_number_parameters 653 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_gt 0.0811 _refine_ls_wR_factor_ref 0.2363 _refine_ls_wR_factor_gt 0.2072 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2077(2) 0.19422(17) 0.63682(16) 0.0250(5) Uani 1 1 d . . . C2 C 0.2146(2) 0.10753(16) 0.59156(16) 0.0235(5) Uani 1 1 d . . . C3 C 0.3118(2) 0.09174(17) 0.63158(17) 0.0264(5) Uani 1 1 d . . . C4 C 0.3901(2) 0.15927(19) 0.71563(18) 0.0305(5) Uani 1 1 d . . . H4 H 0.4543 0.1481 0.7423 0.037 Uiso 1 1 calc R . . C5 C 0.3812(2) 0.24199(18) 0.76351(17) 0.0303(5) Uani 1 1 d . A . C6 C 0.2888(2) 0.25840(18) 0.72139(17) 0.0282(5) Uani 1 1 d . . . H6 H 0.2805 0.3148 0.7509 0.034 Uiso 1 1 calc R . . C7 C 0.0651(2) 0.29067(18) 0.67155(17) 0.0280(5) Uani 1 1 d . . . C8 C 0.0044(2) 0.23289(18) 0.71654(17) 0.0286(5) Uani 1 1 d . . . C9 C -0.0263(2) 0.2792(2) 0.78868(18) 0.0337(6) Uani 1 1 d . . . C10 C 0.0083(3) 0.3798(2) 0.81143(18) 0.0397(7) Uani 1 1 d . . . H10 H -0.0112 0.4110 0.8598 0.048 Uiso 1 1 calc R . . C11 C 0.0696(3) 0.4378(2) 0.76824(19) 0.0400(7) Uani 1 1 d . B . C12 C 0.0967(2) 0.39159(19) 0.69708(18) 0.0335(6) Uani 1 1 d . . . H12 H 0.1371 0.4288 0.6653 0.040 Uiso 1 1 calc R . . C13 C 0.1738(2) 0.31450(18) 0.53436(18) 0.0307(5) Uani 1 1 d . . . C14 C 0.1086(3) 0.3200(2) 0.4572(2) 0.0427(7) Uani 1 1 d . . . H14 H 0.0267 0.2792 0.4328 0.051 Uiso 1 1 calc R . . C15 C 0.1609(4) 0.3838(3) 0.4154(3) 0.0571(9) Uani 1 1 d . . . H15 H 0.1147 0.3864 0.3629 0.068 Uiso 1 1 calc R . . C16 C 0.2791(3) 0.4434(2) 0.4497(3) 0.0548(9) Uani 1 1 d . . . H16 H 0.3152 0.4878 0.4216 0.066 Uiso 1 1 calc R . . C17 C 0.3446(3) 0.4378(3) 0.5252(3) 0.0577(9) Uani 1 1 d . . . H17 H 0.4267 0.4783 0.5489 0.069 Uiso 1 1 calc R . . C18 C 0.2927(3) 0.3740(2) 0.5674(2) 0.0476(8) Uani 1 1 d . . . H18 H 0.3396 0.3713 0.6196 0.057 Uiso 1 1 calc R . . C19 C 0.3358(2) 0.0075(2) 0.58159(19) 0.0342(6) Uani 1 1 d . . . C20 C 0.2298(3) -0.0933(2) 0.5477(2) 0.0459(8) Uani 1 1 d . . . H20A H 0.1988 -0.1027 0.5971 0.069 Uiso 1 1 calc R . . H20B H 0.2539 -0.1449 0.5267 0.069 Uiso 1 1 calc R . . H20C H 0.1690 -0.0966 0.4978 0.069 Uiso 1 1 calc R . . C21 C 0.3693(3) 0.0280(2) 0.5001(2) 0.0450(7) Uani 1 1 d . . . H21A H 0.3097 0.0409 0.4639 0.067 Uiso 1 1 calc R . . H21B H 0.3742 -0.0291 0.4631 0.067 Uiso 1 1 calc R . . H21C H 0.4454 0.0855 0.5212 0.067 Uiso 1 1 calc R . . C22 C 0.4370(3) -0.0013(3) 0.6419(2) 0.0503(8) Uani 1 1 d . . . H22A H 0.5085 0.0601 0.6619 0.075 Uiso 1 1 calc R . . H22B H 0.4495 -0.0554 0.6076 0.075 Uiso 1 1 calc R . . H22C H 0.4175 -0.0144 0.6946 0.075 Uiso 1 1 calc R . . C23 C 0.4697(3) 0.3153(2) 0.8554(2) 0.0426(7) Uani 1 1 d . . . C27 C -0.0963(3) 0.2189(3) 0.8380(2) 0.0477(8) Uani 1 1 d . . . C28 C -0.0301(4) 0.1680(3) 0.8807(3) 0.0655(11) Uani 1 1 d . . . H28A H 0.0506 0.2162 0.9164 0.098 Uiso 1 1 calc R . . H28B H -0.0295 0.1161 0.8330 0.098 Uiso 1 1 calc R . . H28C H -0.0692 0.1393 0.9200 0.098 Uiso 1 1 calc R . . C29 C -0.2160(3) 0.1422(3) 0.7715(3) 0.0653(10) Uani 1 1 d . . . H29A H -0.2593 0.1021 0.8024 0.098 Uiso 1 1 calc R . . H29B H -0.2055 0.1000 0.7215 0.098 Uiso 1 1 calc R . . H29C H -0.2602 0.1753 0.7477 0.098 Uiso 1 1 calc R . . C30 C -0.1170(4) 0.2837(3) 0.9145(3) 0.0723(12) Uani 1 1 d . . . H30A H -0.1603 0.3168 0.8895 0.108 Uiso 1 1 calc R . . H30B H -0.0415 0.3330 0.9590 0.108 Uiso 1 1 calc R . . H30C H -0.1625 0.2427 0.9438 0.108 Uiso 1 1 calc R . . C31 C 0.1071(4) 0.5487(2) 0.8003(2) 0.0598(10) Uani 1 1 d . . . C35 C 0.0519(2) 0.09015(18) 0.29938(17) 0.0285(5) Uani 1 1 d . . . C36 C 0.1730(2) 0.1407(2) 0.34331(19) 0.0358(6) Uani 1 1 d . . . H36 H 0.2043 0.1357 0.3997 0.043 Uiso 1 1 calc R . . C37 C 0.2486(3) 0.1975(2) 0.3081(2) 0.0442(7) Uani 1 1 d . . . H37 H 0.3303 0.2294 0.3399 0.053 Uiso 1 1 calc R . . C38 C 0.2068(3) 0.2085(2) 0.2269(2) 0.0470(8) Uani 1 1 d . C . C39 C 0.0857(3) 0.1588(2) 0.18418(19) 0.0396(7) Uani 1 1 d . . . H39 H 0.0553 0.1650 0.1281 0.047 Uiso 1 1 calc R . . C40 C 0.0065(2) 0.10138(18) 0.21722(17) 0.0307(6) Uani 1 1 d . . . C41 C -0.1258(3) 0.0597(2) 0.1681(2) 0.0391(7) Uani 1 1 d . . . C42 C -0.1521(3) 0.0650(3) 0.0723(3) 0.0697(12) Uani 1 1 d . . . H42A H -0.1221 0.0261 0.0361 0.105 Uiso 1 1 calc R . . H42B H -0.1141 0.1335 0.0758 0.105 Uiso 1 1 calc R . . H42C H -0.2370 0.0387 0.0441 0.105 Uiso 1 1 calc R . . C43 C -0.1728(4) 0.1223(3) 0.2230(3) 0.0713(12) Uani 1 1 d . . . H43A H -0.2579 0.0949 0.1954 0.107 Uiso 1 1 calc R . . H43B H -0.1361 0.1898 0.2237 0.107 Uiso 1 1 calc R . . H43C H -0.1544 0.1220 0.2850 0.107 Uiso 1 1 calc R . . C44 C -0.1951(3) -0.0475(2) 0.1578(2) 0.0495(8) Uani 1 1 d . . . H44A H -0.2078 -0.0511 0.2150 0.074 Uiso 1 1 calc R . . H44B H -0.1511 -0.0845 0.1416 0.074 Uiso 1 1 calc R . . H44C H -0.2709 -0.0756 0.1102 0.074 Uiso 1 1 calc R . . C45 C 0.2853(4) 0.2708(3) 0.1842(3) 0.0729(13) Uani 1 1 d . . . C99 C 0.8229(7) 0.3486(5) 0.4703(6) 0.134(3) Uani 1 1 d . . . H99A H 0.8575 0.4183 0.4768 0.201 Uiso 1 1 calc R . . H99B H 0.7869 0.3085 0.4061 0.201 Uiso 1 1 calc R . . H99C H 0.8842 0.3320 0.4982 0.201 Uiso 1 1 calc R . . C100 C 0.7321(4) 0.3289(3) 0.5156(3) 0.0659(11) Uani 1 1 d . . . C101 C 0.6162(5) 0.3061(3) 0.4730(3) 0.0791(13) Uani 1 1 d . . . H101 H 0.5914 0.2981 0.4108 0.095 Uiso 1 1 calc R . . C102 C 0.5369(4) 0.2948(3) 0.5187(4) 0.0799(13) Uani 1 1 d . . . H102 H 0.4582 0.2799 0.4881 0.096 Uiso 1 1 calc R . . C103 C 0.5691(4) 0.3045(3) 0.6056(4) 0.0778(13) Uani 1 1 d . . . H103 H 0.5144 0.2981 0.6375 0.093 Uiso 1 1 calc R . . C104 C 0.6810(5) 0.3237(4) 0.6480(3) 0.0871(15) Uani 1 1 d . . . H104 H 0.7040 0.3294 0.7097 0.105 Uiso 1 1 calc R . . C105 C 0.7615(4) 0.3350(3) 0.6035(3) 0.0774(13) Uani 1 1 d . . . H105 H 0.8390 0.3473 0.6344 0.093 Uiso 1 1 calc R . . C201 C 0.5006(10) 0.0683(12) 0.0969(13) 0.305(11) Uani 1 1 d . . . H201 H 0.5066 0.1163 0.1489 0.366 Uiso 1 1 calc R . . C202 C 0.5406(7) 0.0869(9) 0.0149(10) 0.184(6) Uani 1 1 d . . . H202 H 0.5735 0.1555 0.0254 0.221 Uiso 1 1 calc R . . C203 C 0.4544(8) -0.0328(13) 0.0780(13) 0.241(9) Uani 1 1 d . . . H203 H 0.4237 -0.0648 0.1167 0.289 Uiso 1 1 calc R . . O1 O 0.12970(14) 0.04354(11) 0.51425(11) 0.0243(4) Uani 1 1 d . . . O2 O 0.01805(16) -0.13857(12) 0.30784(12) 0.0314(4) Uani 1 1 d . . . O3 O 0.01485(16) -0.03359(12) 0.66197(12) 0.0293(4) Uani 1 1 d . . . P1 P 0.09394(6) 0.22221(4) 0.57870(4) 0.02552(17) Uani 1 1 d . . . Li1 Li 0.0180(4) -0.0606(3) 0.5426(3) 0.0299(9) Uani 1 1 d . . . Li2 Li -0.1014(4) -0.1020(3) 0.2792(3) 0.0357(10) Uani 1 1 d . . . Li3 Li 0.1035(4) -0.0141(3) 0.3896(3) 0.0338(10) Uani 1 1 d . . . C24 C 0.4066(5) 0.3241(4) 0.9241(3) 0.084(2) Uani 0.868(7) 1 d P A 1 H24A H 0.3644 0.2592 0.9276 0.126 Uiso 0.868(7) 1 calc PR A 1 H24B H 0.3509 0.3501 0.9056 0.126 Uiso 0.868(7) 1 calc PR A 1 H24C H 0.4638 0.3687 0.9834 0.126 Uiso 0.868(7) 1 calc PR A 1 C25 C 0.5641(7) 0.2845(5) 0.8868(4) 0.138(4) Uani 0.868(7) 1 d P A 1 H25A H 0.6219 0.3343 0.9438 0.207 Uiso 0.868(7) 1 calc PR A 1 H25B H 0.6028 0.2777 0.8411 0.207 Uiso 0.868(7) 1 calc PR A 1 H25C H 0.5290 0.2214 0.8958 0.207 Uiso 0.868(7) 1 calc PR A 1 C26 C 0.5283(4) 0.4159(3) 0.8476(3) 0.0737(17) Uani 0.868(7) 1 d P A 1 H26A H 0.4696 0.4400 0.8322 0.111 Uiso 0.868(7) 1 calc PR A 1 H26B H 0.5648 0.4109 0.8003 0.111 Uiso 0.868(7) 1 calc PR A 1 H26C H 0.5884 0.4617 0.9053 0.111 Uiso 0.868(7) 1 calc PR A 1 C32 C -0.0008(5) 0.5691(3) 0.8123(3) 0.0654(15) Uani 0.835(7) 1 d P B 1 H32A H 0.0215 0.6396 0.8281 0.098 Uiso 0.835(7) 1 calc PR B 1 H32B H -0.0241 0.5471 0.8605 0.098 Uiso 0.835(7) 1 calc PR B 1 H32C H -0.0666 0.5332 0.7557 0.098 Uiso 0.835(7) 1 calc PR B 1 C33 C 0.1490(7) 0.5949(3) 0.7349(4) 0.079(2) Uani 0.835(7) 1 d P B 1 H33A H 0.1671 0.6647 0.7566 0.119 Uiso 0.835(7) 1 calc PR B 1 H33B H 0.0877 0.5623 0.6757 0.119 Uiso 0.835(7) 1 calc PR B 1 H33C H 0.2196 0.5880 0.7295 0.119 Uiso 0.835(7) 1 calc PR B 1 C34 C 0.1993(5) 0.5945(3) 0.8933(4) 0.0801(19) Uani 0.835(7) 1 d P B 1 H34A H 0.2682 0.5839 0.8890 0.120 Uiso 0.835(7) 1 calc PR B 1 H34B H 0.1672 0.5640 0.9345 0.120 Uiso 0.835(7) 1 calc PR B 1 H34C H 0.2221 0.6652 0.9163 0.120 Uiso 0.835(7) 1 calc PR B 1 C46 C 0.2398(6) 0.3502(5) 0.1697(5) 0.101(3) Uani 0.831(8) 1 d P C 1 H46A H 0.2881 0.3912 0.1419 0.152 Uiso 0.831(8) 1 calc PR C 1 H46B H 0.2452 0.3916 0.2281 0.152 Uiso 0.831(8) 1 calc PR C 1 H46C H 0.1580 0.3165 0.1301 0.152 Uiso 0.831(8) 1 calc PR C 1 C47 C 0.2715(5) 0.2082(5) 0.0928(4) 0.095(3) Uani 0.831(8) 1 d P C 1 H47A H 0.3280 0.2469 0.0685 0.142 Uiso 0.831(8) 1 calc PR C 1 H47B H 0.1918 0.1849 0.0523 0.142 Uiso 0.831(8) 1 calc PR C 1 H47C H 0.2858 0.1518 0.0977 0.142 Uiso 0.831(8) 1 calc PR C 1 C48 C 0.4088(6) 0.3298(7) 0.2457(5) 0.116(4) Uani 0.831(8) 1 d P C 1 H48A H 0.4404 0.2857 0.2624 0.174 Uiso 0.831(8) 1 calc PR C 1 H48B H 0.4110 0.3756 0.3002 0.174 Uiso 0.831(8) 1 calc PR C 1 H48C H 0.4562 0.3668 0.2148 0.174 Uiso 0.831(8) 1 calc PR C 1 C24A C 0.469(4) 0.260(3) 0.924(3) 0.078(10) Uiso 0.132(7) 1 d P A 2 H24D H 0.3987 0.2480 0.9418 0.117 Uiso 0.132(7) 1 calc PR A 2 H24E H 0.5388 0.2990 0.9772 0.117 Uiso 0.132(7) 1 calc PR A 2 H24F H 0.4686 0.1964 0.8954 0.117 Uiso 0.132(7) 1 calc PR A 2 C25A C 0.589(3) 0.358(2) 0.847(2) 0.059(8) Uiso 0.132(7) 1 d P A 2 H25D H 0.5937 0.4045 0.8148 0.089 Uiso 0.132(7) 1 calc PR A 2 H25E H 0.6046 0.3053 0.8138 0.089 Uiso 0.132(7) 1 calc PR A 2 H25F H 0.6479 0.3925 0.9076 0.089 Uiso 0.132(7) 1 calc PR A 2 C26A C 0.454(3) 0.408(3) 0.894(3) 0.085(12) Uiso 0.132(7) 1 d P A 2 H26D H 0.5180 0.4515 0.9501 0.127 Uiso 0.132(7) 1 calc PR A 2 H26E H 0.3790 0.3891 0.9058 0.127 Uiso 0.132(7) 1 calc PR A 2 H26F H 0.4539 0.4419 0.8499 0.127 Uiso 0.132(7) 1 calc PR A 2 C32A C 0.064(4) 0.577(3) 0.724(3) 0.116(14) Uiso 0.165(7) 1 d P B 2 H32D H -0.0211 0.5406 0.6984 0.173 Uiso 0.165(7) 1 calc PR B 2 H32E H 0.0990 0.5608 0.6770 0.173 Uiso 0.165(7) 1 calc PR B 2 H32F H 0.0870 0.6474 0.7445 0.173 Uiso 0.165(7) 1 calc PR B 2 C33A C 0.268(3) 0.600(2) 0.813(2) 0.086(9) Uiso 0.165(7) 1 d P B 2 H33D H 0.3049 0.6713 0.8423 0.128 Uiso 0.165(7) 1 calc PR B 2 H33E H 0.2774 0.5835 0.7533 0.128 Uiso 0.165(7) 1 calc PR B 2 H33F H 0.3058 0.5711 0.8500 0.128 Uiso 0.165(7) 1 calc PR B 2 C34A C 0.119(3) 0.600(3) 0.890(2) 0.095(11) Uiso 0.165(7) 1 d P B 2 H34D H 0.1692 0.6702 0.9053 0.142 Uiso 0.165(7) 1 calc PR B 2 H34E H 0.1550 0.5746 0.9316 0.142 Uiso 0.165(7) 1 calc PR B 2 H34F H 0.0419 0.5908 0.8940 0.142 Uiso 0.165(7) 1 calc PR B 2 C46A C 0.241(2) 0.274(2) 0.1003(18) 0.065(7) Uiso 0.169(8) 1 d P C 2 H46D H 0.1925 0.3101 0.1042 0.097 Uiso 0.169(8) 1 calc PR C 2 H46E H 0.1924 0.2074 0.0573 0.097 Uiso 0.169(8) 1 calc PR C 2 H46F H 0.3052 0.3081 0.0799 0.097 Uiso 0.169(8) 1 calc PR C 2 C47A C 0.376(2) 0.2095(19) 0.1600(19) 0.069(8) Uiso 0.169(8) 1 d P C 2 H47D H 0.3262 0.1403 0.1230 0.104 Uiso 0.169(8) 1 calc PR C 2 H47E H 0.4266 0.2137 0.2167 0.104 Uiso 0.169(8) 1 calc PR C 2 H47F H 0.4250 0.2413 0.1271 0.104 Uiso 0.169(8) 1 calc PR C 2 C48A C 0.389(8) 0.357(7) 0.229(7) 0.25(5) Uiso 0.169(8) 1 d P C 2 H48D H 0.4108 0.3890 0.1852 0.375 Uiso 0.169(8) 1 calc PR C 2 H48E H 0.4513 0.3418 0.2561 0.375 Uiso 0.169(8) 1 calc PR C 2 H48F H 0.3766 0.4017 0.2757 0.375 Uiso 0.169(8) 1 calc PR C 2 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 C1 0.0257(12) 0.0244(12) 0.0230(12) 0.0069(9) 0.0086(10) 0.0095(9) C2 0.0224(11) 0.0226(11) 0.0217(12) 0.0060(9) 0.0084(9) 0.0062(8) C3 0.0230(12) 0.0273(12) 0.0286(13) 0.0086(9) 0.0105(10) 0.0102(9) C4 0.0243(12) 0.0347(14) 0.0309(14) 0.0128(10) 0.0060(10) 0.0119(10) C5 0.0297(13) 0.0293(13) 0.0236(13) 0.0075(10) 0.0051(10) 0.0069(10) C6 0.0321(13) 0.0240(12) 0.0234(13) 0.0060(9) 0.0082(10) 0.0086(9) C7 0.0332(13) 0.0255(12) 0.0235(13) 0.0058(9) 0.0059(10) 0.0143(10) C8 0.0298(13) 0.0290(13) 0.0265(13) 0.0063(10) 0.0058(10) 0.0162(10) C9 0.0370(14) 0.0431(15) 0.0239(13) 0.0084(11) 0.0078(11) 0.0237(12) C10 0.0556(18) 0.0475(17) 0.0210(13) 0.0025(11) 0.0091(12) 0.0353(14) C11 0.0571(18) 0.0357(15) 0.0257(14) 0.0027(11) 0.0061(13) 0.0275(13) C12 0.0433(15) 0.0263(13) 0.0286(14) 0.0063(10) 0.0060(11) 0.0177(11) C13 0.0398(14) 0.0250(13) 0.0282(14) 0.0073(10) 0.0134(11) 0.0150(10) C14 0.0482(17) 0.0462(17) 0.0422(17) 0.0236(13) 0.0153(14) 0.0242(14) C15 0.078(3) 0.062(2) 0.052(2) 0.0390(18) 0.0249(19) 0.0385(19) C16 0.078(2) 0.0404(18) 0.060(2) 0.0315(16) 0.038(2) 0.0234(17) C17 0.052(2) 0.0458(19) 0.060(2) 0.0230(16) 0.0203(17) 0.0021(15) C18 0.0423(17) 0.0469(18) 0.0400(17) 0.0183(14) 0.0081(14) 0.0060(13) C19 0.0292(13) 0.0366(15) 0.0374(15) 0.0078(11) 0.0102(11) 0.0184(11) C20 0.0405(16) 0.0338(16) 0.063(2) 0.0111(14) 0.0160(15) 0.0204(12) C21 0.0420(17) 0.0582(19) 0.0421(18) 0.0140(14) 0.0193(14) 0.0285(14) C22 0.0463(18) 0.058(2) 0.051(2) 0.0119(15) 0.0107(15) 0.0354(16) C23 0.0444(17) 0.0358(16) 0.0298(15) 0.0012(11) -0.0012(13) 0.0124(12) C27 0.056(2) 0.058(2) 0.0376(17) 0.0148(14) 0.0255(15) 0.0300(16) C28 0.093(3) 0.085(3) 0.051(2) 0.044(2) 0.038(2) 0.053(2) C29 0.054(2) 0.076(3) 0.065(3) 0.019(2) 0.037(2) 0.0207(19) C30 0.093(3) 0.085(3) 0.056(2) 0.021(2) 0.050(2) 0.044(2) C31 0.097(3) 0.0350(18) 0.0407(19) -0.0011(13) 0.0118(19) 0.0366(18) C35 0.0383(14) 0.0248(12) 0.0249(13) 0.0102(9) 0.0118(11) 0.0146(10) C36 0.0371(15) 0.0359(15) 0.0295(14) 0.0112(11) 0.0065(12) 0.0133(11) C37 0.0344(15) 0.0456(17) 0.0372(17) 0.0111(13) 0.0081(13) 0.0054(12) C38 0.0437(17) 0.0483(18) 0.0357(17) 0.0149(13) 0.0156(14) 0.0045(13) C39 0.0452(16) 0.0388(15) 0.0266(14) 0.0159(11) 0.0100(12) 0.0080(12) C40 0.0362(14) 0.0272(13) 0.0259(13) 0.0100(10) 0.0083(11) 0.0114(10) C41 0.0371(15) 0.0425(16) 0.0383(16) 0.0229(13) 0.0080(12) 0.0148(12) C42 0.048(2) 0.090(3) 0.056(2) 0.049(2) -0.0019(17) 0.0096(18) C43 0.056(2) 0.073(3) 0.093(3) 0.025(2) 0.021(2) 0.040(2) C44 0.0383(16) 0.0474(18) 0.051(2) 0.0245(15) 0.0022(14) 0.0081(13) C45 0.061(2) 0.078(3) 0.043(2) 0.0229(19) 0.0186(18) -0.009(2) C99 0.182(7) 0.101(4) 0.203(8) 0.080(5) 0.145(7) 0.088(5) C100 0.091(3) 0.043(2) 0.084(3) 0.0290(19) 0.048(3) 0.037(2) C101 0.114(4) 0.073(3) 0.049(2) 0.024(2) 0.012(3) 0.045(3) C102 0.058(3) 0.071(3) 0.078(3) 0.014(2) 0.005(2) 0.012(2) C103 0.077(3) 0.071(3) 0.084(3) 0.037(2) 0.037(3) 0.018(2) C104 0.115(4) 0.113(4) 0.058(3) 0.045(3) 0.027(3) 0.067(3) C105 0.072(3) 0.083(3) 0.076(3) 0.022(2) 0.006(2) 0.046(2) C201 0.100(7) 0.314(17) 0.52(3) 0.274(19) -0.023(12) 0.093(9) C202 0.073(4) 0.260(13) 0.262(13) 0.217(12) 0.027(7) 0.053(6) C203 0.083(5) 0.321(18) 0.340(19) 0.265(17) 0.001(9) 0.054(8) O1 0.0227(8) 0.0245(8) 0.0222(9) 0.0042(6) 0.0066(7) 0.0095(6) O2 0.0383(10) 0.0269(9) 0.0316(10) 0.0096(7) 0.0144(8) 0.0156(7) O3 0.0386(10) 0.0264(9) 0.0242(9) 0.0127(7) 0.0114(8) 0.0124(7) P1 0.0291(3) 0.0219(3) 0.0234(3) 0.0057(2) 0.0075(2) 0.0107(2) Li1 0.033(2) 0.025(2) 0.027(2) 0.0074(16) 0.0077(18) 0.0108(17) Li2 0.041(3) 0.031(2) 0.030(2) 0.0097(18) 0.007(2) 0.0143(19) Li3 0.038(2) 0.038(2) 0.029(2) 0.0114(18) 0.0131(19) 0.0201(19) C24 0.096(4) 0.072(3) 0.024(2) -0.0063(19) 0.017(2) -0.010(3) C25 0.138(6) 0.117(5) 0.081(4) -0.050(4) -0.083(5) 0.088(5) C26 0.069(3) 0.047(2) 0.047(3) 0.0043(18) 0.000(2) -0.017(2) C32 0.092(4) 0.051(3) 0.065(3) 0.011(2) 0.022(3) 0.052(3) C33 0.138(6) 0.028(2) 0.089(4) 0.021(2) 0.057(4) 0.042(3) C34 0.083(4) 0.043(3) 0.072(4) -0.018(2) -0.004(3) 0.022(2) C46 0.102(5) 0.080(4) 0.107(5) 0.065(4) 0.037(4) 0.002(3) C47 0.074(4) 0.130(6) 0.055(3) 0.032(3) 0.041(3) 0.007(3) C48 0.051(3) 0.149(7) 0.070(4) 0.058(4) 0.004(3) -0.042(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.398(3) . ? C1 C2 1.420(3) . ? C1 P1 1.829(2) . ? C2 O1 1.341(3) . ? C2 C3 1.427(3) . ? C3 C4 1.395(4) . ? C3 C19 1.541(3) . ? C4 C5 1.396(4) . ? C4 H4 0.9500 . ? C5 C6 1.392(4) . ? C5 C23 1.534(4) . ? C6 H6 0.9500 . ? C7 C12 1.401(4) . ? C7 C8 1.408(4) . ? C7 P1 1.814(3) . ? C8 O2 1.329(3) . ? C8 C9 1.428(4) . ? C9 C10 1.392(4) . ? C9 C27 1.538(4) . ? C10 C11 1.390(4) . ? C10 H10 0.9500 . ? C11 C12 1.386(4) . ? C11 C31 1.533(4) . ? C12 H12 0.9500 . ? C13 C18 1.379(4) . ? C13 C14 1.393(4) . ? C13 P1 1.832(3) . ? C14 C15 1.383(4) . ? C14 H14 0.9500 . ? C15 C16 1.372(5) . ? C15 H15 0.9500 . ? C16 C17 1.374(5) . ? C16 H16 0.9500 . ? C17 C18 1.387(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.535(4) . ? C19 C22 1.535(4) . ? C19 C21 1.533(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C25A 1.50(3) . ? C23 C26 1.520(5) . ? C23 C24 1.517(6) . ? C23 C25 1.511(6) . ? C23 C26A 1.53(4) . ? C23 C24A 1.56(4) . ? C27 C29 1.528(5) . ? C27 C28 1.535(5) . ? C27 C30 1.537(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C34A 1.42(4) . ? C31 C33 1.495(7) . ? C31 C32A 1.48(4) . ? C31 C34 1.521(6) . ? C31 C32 1.584(6) . ? C31 C33A 1.89(3) . ? C35 O3 1.356(3) 2_556 ? C35 C36 1.399(4) . ? C35 C40 1.413(4) . ? C36 C37 1.378(4) . ? C36 H36 0.9500 . ? C37 C38 1.384(4) . ? C37 H37 0.9500 . ? C38 C39 1.397(4) . ? C38 C45 1.529(4) . ? C39 C40 1.386(4) . ? C39 H39 0.9500 . ? C40 C41 1.540(4) . ? C41 C44 1.527(4) . ? C41 C43 1.536(5) . ? C41 C42 1.539(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C48A 1.40(9) . ? C45 C46A 1.38(3) . ? C45 C48 1.493(7) . ? C45 C47 1.495(7) . ? C45 C46 1.598(8) . ? C45 C47A 1.82(3) . ? C99 C100 1.489(7) . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? C100 C105 1.358(6) . ? C100 C101 1.387(7) . ? C101 C102 1.371(7) . ? C101 H101 0.9500 . ? C102 C103 1.330(7) . ? C102 H102 0.9500 . ? C103 C104 1.357(7) . ? C103 H103 0.9500 . ? C104 C105 1.369(7) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C201 C203 1.393(17) . ? C201 C202 1.567(19) . ? C201 H201 0.9500 . ? C202 C203 1.56(2) 2_655 ? C202 H202 0.9500 . ? C203 C202 1.56(2) 2_655 ? C203 H203 0.9500 . ? O1 Li3 1.897(5) . ? O1 Li1 1.960(5) . ? O1 Li1 2.085(5) 2_556 ? O2 C8 1.329(3) 2_556 ? O2 Li3 1.826(5) . ? O2 Li2 1.849(5) . ? O3 C35 1.356(3) 2_556 ? O3 Li2 1.869(5) 2_556 ? O3 Li1 1.883(5) . ? O3 Li3 2.051(5) 2_556 ? P1 Li1 2.467(4) 2_556 ? Li1 O1 2.085(5) 2_556 ? Li1 P1 2.467(4) 2_556 ? Li1 Li3 2.549(6) 2_556 ? Li1 Li1 2.699(8) 2_556 ? Li2 O3 1.869(5) 2_556 ? Li2 Li3 2.515(7) . ? Li2 Li1 3.017(6) 2_556 ? Li3 O3 2.051(5) 2_556 ? Li3 Li1 2.549(6) 2_556 ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C25A H25D 0.9800 . ? C25A H25E 0.9800 . ? C25A H25F 0.9800 . ? C26A H26D 0.9800 . ? C26A H26E 0.9800 . ? C26A H26F 0.9800 . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 0.9800 . ? C33A H33D 0.9800 . ? C33A H33E 0.9800 . ? C33A H33F 0.9800 . ? C34A H34D 0.9800 . ? C34A H34E 0.9800 . ? C34A H34F 0.9800 . ? C46A H46D 0.9800 . ? C46A H46E 0.9800 . ? C46A H46F 0.9800 . ? C47A H47D 0.9800 . ? C47A H47E 0.9800 . ? C47A H47F 0.9800 . ? C48A H48D 0.9800 . ? C48A H48E 0.9800 . ? C48A H48F 0.9800 . ? 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 C6 C1 C2 121.0(2) . . ? C6 C1 P1 121.03(19) . . ? C2 C1 P1 117.91(18) . . ? C6 C1 Li2 85.72(18) . 2_556 ? C2 C1 Li2 87.63(18) . 2_556 ? P1 C1 Li2 99.31(15) . 2_556 ? O1 C2 C1 119.2(2) . . ? O1 C2 C3 122.7(2) . . ? C1 C2 C3 118.0(2) . . ? O1 C2 Li2 103.95(17) . 2_556 ? C1 C2 Li2 61.79(16) . 2_556 ? C3 C2 Li2 101.54(18) . 2_556 ? C4 C3 C2 117.8(2) . . ? C4 C3 C19 120.3(2) . . ? C2 C3 C19 121.7(2) . . ? C5 C4 C3 124.9(2) . . ? C5 C4 H4 117.5 . . ? C3 C4 H4 117.5 . . ? C6 C5 C4 116.3(2) . . ? C6 C5 C23 120.2(2) . . ? C4 C5 C23 123.5(2) . . ? C5 C6 C1 121.8(2) . . ? C5 C6 Li2 100.89(19) . 2_556 ? C1 C6 Li2 63.65(16) . 2_556 ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? Li2 C6 H6 105.2 2_556 . ? C12 C7 C8 121.4(2) . . ? C12 C7 P1 124.6(2) . . ? C8 C7 P1 114.05(18) . . ? O2 C8 C7 118.6(2) 2_556 . ? O2 C8 C9 122.9(2) 2_556 . ? C7 C8 C9 118.5(2) . . ? O2 C8 Li2 35.15(14) 2_556 2_556 ? C7 C8 Li2 103.48(19) . 2_556 ? C9 C8 Li2 125.1(2) . 2_556 ? C10 C9 C8 117.5(3) . . ? C10 C9 C27 121.9(2) . . ? C8 C9 C27 120.7(2) . . ? C11 C10 C9 124.5(3) . . ? C11 C10 H10 117.7 . . ? C9 C10 H10 117.7 . . ? C12 C11 C10 117.4(3) . . ? C12 C11 C31 122.0(3) . . ? C10 C11 C31 120.6(3) . . ? C11 C12 C7 120.7(3) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? C18 C13 C14 117.8(3) . . ? C18 C13 P1 125.8(2) . . ? C14 C13 P1 116.3(2) . . ? C15 C14 C13 121.3(3) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 119.1(3) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C16 C17 C18 121.0(3) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C13 C18 C17 120.6(3) . . ? C13 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 C22 106.4(2) . . ? C20 C19 C21 108.4(3) . . ? C22 C19 C21 108.0(2) . . ? C20 C19 C3 113.1(2) . . ? C22 C19 C3 112.0(2) . . ? C21 C19 C3 108.7(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25A C23 C26 55.3(12) . . ? C25A C23 C24 140.6(12) . . ? C26 C23 C24 108.1(4) . . ? C25A C23 C25 55.9(12) . . ? C26 C23 C25 107.9(5) . . ? C24 C23 C25 110.5(5) . . ? C25A C23 C26A 102(2) . . ? C26 C23 C26A 51.5(15) . . ? C24 C23 C26A 57.5(15) . . ? C25 C23 C26A 132.3(15) . . ? C25A C23 C5 109.7(12) . . ? C26 C23 C5 109.6(3) . . ? C24 C23 C5 109.7(3) . . ? C25 C23 C5 111.0(3) . . ? C26A C23 C5 116.5(15) . . ? C25A C23 C24A 110.1(19) . . ? C26 C23 C24A 142.2(15) . . ? C24 C23 C24A 58.6(15) . . ? C25 C23 C24A 56.3(15) . . ? C26A C23 C24A 110(2) . . ? C5 C23 C24A 108.2(15) . . ? C29 C27 C28 109.8(3) . . ? C29 C27 C30 107.6(3) . . ? C28 C27 C30 107.1(3) . . ? C29 C27 C9 109.6(3) . . ? C28 C27 C9 110.7(3) . . ? C30 C27 C9 111.9(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C34A C31 C33 125.6(15) . . ? C34A C31 C32A 121(2) . . ? C33 C31 C32A 39.0(19) . . ? C34A C31 C34 42.3(16) . . ? C33 C31 C34 112.2(5) . . ? C32A C31 C34 140.0(19) . . ? C34A C31 C11 120.8(15) . . ? C33 C31 C11 112.7(3) . . ? C32A C31 C11 109.6(18) . . ? C34 C31 C11 108.1(3) . . ? C34A C31 C32 64.3(16) . . ? C33 C31 C32 107.5(4) . . ? C32A C31 C32 73(2) . . ? C34 C31 C32 106.7(4) . . ? C11 C31 C32 109.5(3) . . ? C34A C31 C33A 97.3(19) . . ? C33 C31 C33A 60.8(11) . . ? C32A C31 C33A 100(2) . . ? C34 C31 C33A 59.4(11) . . ? C11 C31 C33A 102.1(10) . . ? C32 C31 C33A 148.3(10) . . ? O3 C35 C36 118.3(2) 2_556 . ? O3 C35 C40 123.9(2) 2_556 . ? C36 C35 C40 117.8(2) . . ? C37 C36 C35 122.7(3) . . ? C37 C36 H36 118.7 . . ? C35 C36 H36 118.7 . . ? C36 C37 C38 120.8(3) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C37 C38 C39 116.1(3) . . ? C37 C38 C45 123.7(3) . . ? C39 C38 C45 120.2(3) . . ? C40 C39 C38 125.0(3) . . ? C40 C39 H39 117.5 . . ? C38 C39 H39 117.5 . . ? C39 C40 C35 117.5(2) . . ? C39 C40 C41 119.5(2) . . ? C35 C40 C41 122.8(2) . . ? C44 C41 C43 108.6(3) . . ? C44 C41 C40 113.8(2) . . ? C43 C41 C40 107.6(3) . . ? C44 C41 C42 106.4(3) . . ? C43 C41 C42 108.0(3) . . ? C40 C41 C42 112.3(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C48A C45 C46A 106(4) . . ? C48A C45 C48 26(4) . . ? C46A C45 C48 125.9(11) . . ? C48A C45 C47 118(4) . . ? C46A C45 C47 50.3(11) . . ? C48 C45 C47 114.7(5) . . ? C48A C45 C38 127(4) . . ? C46A C45 C38 121.6(11) . . ? C48 C45 C38 112.4(4) . . ? C47 C45 C38 110.0(4) . . ? C48A C45 C46 79(4) . . ? C46A C45 C46 56.7(12) . . ? C48 C45 C46 104.8(6) . . ? C47 C45 C46 107.0(5) . . ? C38 C45 C46 107.4(4) . . ? C48A C45 C47A 87(5) . . ? C46A C45 C47A 100.5(15) . . ? C48 C45 C47A 68.6(10) . . ? C47 C45 C47A 54.5(9) . . ? C38 C45 C47A 103.8(9) . . ? C46 C45 C47A 148.0(9) . . ? C100 C99 H99A 109.5 . . ? C100 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C100 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? C105 C100 C101 116.8(4) . . ? C105 C100 C99 120.1(5) . . ? C101 C100 C99 123.1(5) . . ? C100 C101 C102 121.4(4) . . ? C100 C101 H101 119.3 . . ? C102 C101 H101 119.3 . . ? C103 C102 C101 120.5(5) . . ? C103 C102 H102 119.7 . . ? C101 C102 H102 119.7 . . ? C102 C103 C104 119.2(5) . . ? C102 C103 H103 120.4 . . ? C104 C103 H103 120.4 . . ? C103 C104 C105 121.2(4) . . ? C103 C104 H104 119.4 . . ? C105 C104 H104 119.4 . . ? C100 C105 C104 120.9(4) . . ? C100 C105 H105 119.5 . . ? C104 C105 H105 119.5 . . ? C203 C201 C202 106.1(17) . . ? C203 C201 H201 127.0 . . ? C202 C201 H201 127.0 . . ? C201 C202 C203 142.4(11) . 2_655 ? C201 C202 H202 108.8 . . ? C203 C202 H202 108.8 2_655 . ? C201 C203 C202 111.5(14) . 2_655 ? C201 C203 H203 124.2 . . ? C202 C203 H203 124.2 2_655 . ? C2 O1 Li3 141.9(2) . . ? C2 O1 Li1 108.16(19) . . ? Li3 O1 Li1 103.9(2) . . ? C2 O1 Li1 123.75(18) . 2_556 ? Li3 O1 Li1 79.46(19) . 2_556 ? Li1 O1 Li1 83.62(19) . 2_556 ? C8 O2 Li3 148.9(2) 2_556 . ? C8 O2 Li2 120.4(2) 2_556 . ? Li3 O2 Li2 86.4(2) . . ? C35 O3 Li2 120.8(2) 2_556 2_556 ? C35 O3 Li1 131.0(2) 2_556 . ? Li2 O3 Li1 107.0(2) 2_556 . ? C35 O3 Li3 96.98(19) 2_556 2_556 ? Li2 O3 Li3 79.7(2) 2_556 2_556 ? Li1 O3 Li3 80.65(19) . 2_556 ? C7 P1 C1 102.60(11) . . ? C7 P1 C13 104.60(12) . . ? C1 P1 C13 103.03(12) . . ? C7 P1 Li1 135.00(14) . 2_556 ? C1 P1 Li1 96.46(13) . 2_556 ? C13 P1 Li1 110.23(13) . 2_556 ? O3 Li1 O1 117.9(2) . . ? O3 Li1 O1 98.0(2) . 2_556 ? O1 Li1 O1 96.38(19) . 2_556 ? O3 Li1 P1 125.1(2) . 2_556 ? O1 Li1 P1 116.6(2) . 2_556 ? O1 Li1 P1 81.06(15) 2_556 2_556 ? O3 Li1 Li3 52.56(16) . 2_556 ? O1 Li1 Li3 105.6(2) . 2_556 ? O1 Li1 Li3 47.02(14) 2_556 2_556 ? P1 Li1 Li3 115.8(2) 2_556 2_556 ? O3 Li1 Li1 116.6(3) . 2_556 ? O1 Li1 Li1 50.16(15) . 2_556 ? O1 Li1 Li1 46.22(14) 2_556 2_556 ? P1 Li1 Li1 101.9(2) 2_556 2_556 ? Li3 Li1 Li1 70.7(2) 2_556 2_556 ? O3 Li1 Li2 36.33(13) . 2_556 ? O1 Li1 Li2 82.35(17) . 2_556 ? O1 Li1 Li2 95.84(18) 2_556 2_556 ? P1 Li1 Li2 160.9(2) 2_556 2_556 ? Li3 Li1 Li2 52.92(16) 2_556 2_556 ? Li1 Li1 Li2 89.0(2) 2_556 2_556 ? O2 Li2 O3 98.5(2) . 2_556 ? O2 Li2 C1 91.63(19) . 2_556 ? O3 Li2 C1 116.3(2) 2_556 2_556 ? O2 Li2 Li3 46.44(16) . . ? O3 Li2 Li3 53.35(16) 2_556 . ? C1 Li2 Li3 101.2(2) 2_556 . ? O2 Li2 C6 101.5(2) . 2_556 ? O3 Li2 C6 140.9(3) 2_556 2_556 ? C1 Li2 C6 30.63(9) 2_556 2_556 ? Li3 Li2 C6 128.5(2) . 2_556 ? O2 Li2 C8 24.44(10) . 2_556 ? O3 Li2 C8 122.9(2) 2_556 2_556 ? C1 Li2 C8 79.32(15) 2_556 2_556 ? Li3 Li2 C8 70.11(16) . 2_556 ? C6 Li2 C8 80.21(14) 2_556 2_556 ? O2 Li2 C2 110.0(2) . 2_556 ? O3 Li2 C2 88.90(19) 2_556 2_556 ? C1 Li2 C2 30.59(9) 2_556 2_556 ? Li3 Li2 C2 96.05(19) . 2_556 ? C6 Li2 C2 52.70(11) 2_556 2_556 ? C8 Li2 C2 105.85(17) 2_556 2_556 ? O2 Li2 Li1 95.9(2) . 2_556 ? O3 Li2 Li1 36.64(13) 2_556 2_556 ? C1 Li2 Li1 79.97(16) 2_556 2_556 ? Li3 Li2 Li1 53.96(16) . 2_556 ? C6 Li2 Li1 107.59(18) 2_556 2_556 ? C8 Li2 Li1 113.94(18) 2_556 2_556 ? C2 Li2 Li1 55.23(13) 2_556 2_556 ? O2 Li3 O1 134.0(3) . . ? O2 Li3 O3 93.0(2) . 2_556 ? O1 Li3 O3 98.7(2) . 2_556 ? O2 Li3 Li2 47.20(16) . . ? O1 Li3 Li2 120.2(2) . . ? O3 Li3 Li2 46.98(15) 2_556 . ? O2 Li3 Li1 114.3(2) . 2_556 ? O1 Li3 Li1 53.52(15) . 2_556 ? O3 Li3 Li1 46.79(14) 2_556 2_556 ? Li2 Li3 Li1 73.12(19) . 2_556 ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? C23 C24A H24D 109.5 . . ? C23 C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C23 C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? C23 C25A H25D 109.5 . . ? C23 C25A H25E 109.5 . . ? H25D C25A H25E 109.5 . . ? C23 C25A H25F 109.5 . . ? H25D C25A H25F 109.5 . . ? H25E C25A H25F 109.5 . . ? C23 C26A H26D 109.5 . . ? C23 C26A H26E 109.5 . . ? H26D C26A H26E 109.5 . . ? C23 C26A H26F 109.5 . . ? H26D C26A H26F 109.5 . . ? H26E C26A H26F 109.5 . . ? C31 C32A H32D 109.5 . . ? C31 C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? C31 C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? C31 C33A H33D 109.5 . . ? C31 C33A H33E 109.5 . . ? H33D C33A H33E 109.5 . . ? C31 C33A H33F 109.5 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? C31 C34A H34D 109.5 . . ? C31 C34A H34E 109.5 . . ? H34D C34A H34E 109.5 . . ? C31 C34A H34F 109.5 . . ? H34D C34A H34F 109.5 . . ? H34E C34A H34F 109.5 . . ? C45 C46A H46D 109.5 . . ? C45 C46A H46E 109.5 . . ? H46D C46A H46E 109.5 . . ? C45 C46A H46F 109.5 . . ? H46D C46A H46F 109.5 . . ? H46E C46A H46F 109.5 . . ? C45 C47A H47D 109.5 . . ? C45 C47A H47E 109.5 . . ? H47D C47A H47E 109.5 . . ? C45 C47A H47F 109.5 . . ? H47D C47A H47F 109.5 . . ? H47E C47A H47F 109.5 . . ? C45 C48A H48D 109.5 . . ? C45 C48A H48E 109.5 . . ? H48D C48A H48E 109.5 . . ? C45 C48A H48F 109.5 . . ? H48D C48A H48F 109.5 . . ? H48E C48A H48F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 O1 174.3(2) . . . . ? P1 C1 C2 O1 -8.5(3) . . . . ? Li2 C1 C2 O1 90.7(2) 2_556 . . . ? C6 C1 C2 C3 -4.8(3) . . . . ? P1 C1 C2 C3 172.35(17) . . . . ? Li2 C1 C2 C3 -88.4(2) 2_556 . . . ? C6 C1 C2 Li2 83.6(2) . . . 2_556 ? P1 C1 C2 Li2 -99.28(19) . . . 2_556 ? O1 C2 C3 C4 -175.0(2) . . . . ? C1 C2 C3 C4 4.1(3) . . . . ? Li2 C2 C3 C4 -60.0(2) 2_556 . . . ? O1 C2 C3 C19 9.3(4) . . . . ? C1 C2 C3 C19 -171.6(2) . . . . ? Li2 C2 C3 C19 124.3(2) 2_556 . . . ? C2 C3 C4 C5 -0.6(4) . . . . ? C19 C3 C4 C5 175.2(2) . . . . ? C3 C4 C5 C6 -2.3(4) . . . . ? C3 C4 C5 C23 -179.3(3) . . . . ? C4 C5 C6 C1 1.5(4) . . . . ? C23 C5 C6 C1 178.7(2) . . . . ? C4 C5 C6 Li2 67.2(3) . . . 2_556 ? C23 C5 C6 Li2 -115.7(2) . . . 2_556 ? C2 C1 C6 C5 2.0(4) . . . . ? P1 C1 C6 C5 -175.08(19) . . . . ? Li2 C1 C6 C5 86.6(3) 2_556 . . . ? C2 C1 C6 Li2 -84.6(2) . . . 2_556 ? P1 C1 C6 Li2 98.3(2) . . . 2_556 ? C12 C7 C8 O2 -176.7(2) . . . 2_556 ? P1 C7 C8 O2 4.6(3) . . . 2_556 ? C12 C7 C8 C9 0.9(4) . . . . ? P1 C7 C8 C9 -177.82(19) . . . . ? C12 C7 C8 Li2 -142.5(2) . . . 2_556 ? P1 C7 C8 Li2 38.8(2) . . . 2_556 ? O2 C8 C9 C10 176.1(2) 2_556 . . . ? C7 C8 C9 C10 -1.4(4) . . . . ? Li2 C8 C9 C10 133.4(2) 2_556 . . . ? O2 C8 C9 C27 -4.6(4) 2_556 . . . ? C7 C8 C9 C27 177.9(2) . . . . ? Li2 C8 C9 C27 -47.2(4) 2_556 . . . ? C8 C9 C10 C11 0.6(4) . . . . ? C27 C9 C10 C11 -178.7(3) . . . . ? C9 C10 C11 C12 0.7(4) . . . . ? C9 C10 C11 C31 -178.1(3) . . . . ? C10 C11 C12 C7 -1.3(4) . . . . ? C31 C11 C12 C7 177.5(3) . . . . ? C8 C7 C12 C11 0.5(4) . . . . ? P1 C7 C12 C11 179.1(2) . . . . ? C18 C13 C14 C15 -0.7(5) . . . . ? P1 C13 C14 C15 -177.0(3) . . . . ? C13 C14 C15 C16 0.0(5) . . . . ? C14 C15 C16 C17 0.7(6) . . . . ? C15 C16 C17 C18 -0.7(6) . . . . ? C14 C13 C18 C17 0.7(5) . . . . ? P1 C13 C18 C17 176.5(3) . . . . ? C16 C17 C18 C13 0.0(6) . . . . ? C4 C3 C19 C20 130.7(3) . . . . ? C2 C3 C19 C20 -53.7(3) . . . . ? C4 C3 C19 C22 10.5(4) . . . . ? C2 C3 C19 C22 -173.9(2) . . . . ? C4 C3 C19 C21 -108.8(3) . . . . ? C2 C3 C19 C21 66.8(3) . . . . ? C6 C5 C23 C25A -118.2(13) . . . . ? C4 C5 C23 C25A 58.8(14) . . . . ? C6 C5 C23 C26 -59.1(4) . . . . ? C4 C5 C23 C26 117.8(4) . . . . ? C6 C5 C23 C24 59.4(4) . . . . ? C4 C5 C23 C24 -123.7(4) . . . . ? C6 C5 C23 C25 -178.2(5) . . . . ? C4 C5 C23 C25 -1.3(6) . . . . ? C6 C5 C23 C26A -3.3(18) . . . . ? C4 C5 C23 C26A 173.7(17) . . . . ? C6 C5 C23 C24A 121.7(17) . . . . ? C4 C5 C23 C24A -61.3(17) . . . . ? C10 C9 C27 C29 117.3(3) . . . . ? C8 C9 C27 C29 -62.1(4) . . . . ? C10 C9 C27 C28 -121.5(3) . . . . ? C8 C9 C27 C28 59.2(4) . . . . ? C10 C9 C27 C30 -2.0(4) . . . . ? C8 C9 C27 C30 178.7(3) . . . . ? C12 C11 C31 C34A -156.0(19) . . . . ? C10 C11 C31 C34A 23(2) . . . . ? C12 C11 C31 C33 13.3(6) . . . . ? C10 C11 C31 C33 -168.0(4) . . . . ? C12 C11 C31 C32A 55(2) . . . . ? C10 C11 C31 C32A -126(2) . . . . ? C12 C11 C31 C34 -111.3(4) . . . . ? C10 C11 C31 C34 67.4(5) . . . . ? C12 C11 C31 C32 132.8(3) . . . . ? C10 C11 C31 C32 -48.4(4) . . . . ? C12 C11 C31 C33A -49.8(11) . . . . ? C10 C11 C31 C33A 128.9(11) . . . . ? O3 C35 C36 C37 177.9(3) 2_556 . . . ? C40 C35 C36 C37 -2.3(4) . . . . ? C35 C36 C37 C38 1.2(5) . . . . ? C36 C37 C38 C39 -0.3(5) . . . . ? C36 C37 C38 C45 179.6(3) . . . . ? C37 C38 C39 C40 0.5(5) . . . . ? C45 C38 C39 C40 -179.3(3) . . . . ? C38 C39 C40 C35 -1.6(5) . . . . ? C38 C39 C40 C41 173.6(3) . . . . ? O3 C35 C40 C39 -177.8(2) 2_556 . . . ? C36 C35 C40 C39 2.4(4) . . . . ? O3 C35 C40 C41 7.2(4) 2_556 . . . ? C36 C35 C40 C41 -172.7(2) . . . . ? C39 C40 C41 C44 136.7(3) . . . . ? C35 C40 C41 C44 -48.4(4) . . . . ? C39 C40 C41 C43 -103.0(3) . . . . ? C35 C40 C41 C43 71.9(3) . . . . ? C39 C40 C41 C42 15.8(4) . . . . ? C35 C40 C41 C42 -169.3(3) . . . . ? C37 C38 C45 C48A -33(6) . . . . ? C39 C38 C45 C48A 146(6) . . . . ? C37 C38 C45 C46A 175.6(15) . . . . ? C39 C38 C45 C46A -4.6(15) . . . . ? C37 C38 C45 C48 -8.4(8) . . . . ? C39 C38 C45 C48 171.4(6) . . . . ? C37 C38 C45 C47 120.7(5) . . . . ? C39 C38 C45 C47 -59.5(6) . . . . ? C37 C38 C45 C46 -123.2(4) . . . . ? C39 C38 C45 C46 56.6(5) . . . . ? C37 C38 C45 C47A 63.8(10) . . . . ? C39 C38 C45 C47A -116.3(10) . . . . ? C105 C100 C101 C102 2.9(6) . . . . ? C99 C100 C101 C102 -175.7(4) . . . . ? C100 C101 C102 C103 -0.7(7) . . . . ? C101 C102 C103 C104 -1.4(7) . . . . ? C102 C103 C104 C105 1.2(8) . . . . ? C101 C100 C105 C104 -3.1(7) . . . . ? C99 C100 C105 C104 175.6(5) . . . . ? C103 C104 C105 C100 1.1(8) . . . . ? C203 C201 C202 C203 0.5(16) . . . 2_655 ? C202 C201 C203 C202 -0.3(11) . . . 2_655 ? C1 C2 O1 Li3 117.2(3) . . . . ? C3 C2 O1 Li3 -63.7(4) . . . . ? Li2 C2 O1 Li3 -177.5(3) 2_556 . . . ? C1 C2 O1 Li1 -96.9(2) . . . . ? C3 C2 O1 Li1 82.1(3) . . . . ? Li2 C2 O1 Li1 -31.7(2) 2_556 . . . ? C1 C2 O1 Li1 -2.4(3) . . . 2_556 ? C3 C2 O1 Li1 176.6(2) . . . 2_556 ? Li2 C2 O1 Li1 62.8(2) 2_556 . . 2_556 ? C12 C7 P1 C1 109.2(2) . . . . ? C8 C7 P1 C1 -72.1(2) . . . . ? C12 C7 P1 C13 1.9(3) . . . . ? C8 C7 P1 C13 -179.37(19) . . . . ? C12 C7 P1 Li1 -138.0(2) . . . 2_556 ? C8 C7 P1 Li1 40.6(3) . . . 2_556 ? C6 C1 P1 C7 -31.6(2) . . . . ? C2 C1 P1 C7 151.28(19) . . . . ? Li2 C1 P1 C7 59.03(16) 2_556 . . . ? C6 C1 P1 C13 76.9(2) . . . . ? C2 C1 P1 C13 -100.2(2) . . . . ? Li2 C1 P1 C13 167.50(14) 2_556 . . . ? C6 C1 P1 Li1 -170.5(2) . . . 2_556 ? C2 C1 P1 Li1 12.3(2) . . . 2_556 ? Li2 C1 P1 Li1 -79.95(16) 2_556 . . 2_556 ? C18 C13 P1 C7 84.1(3) . . . . ? C14 C13 P1 C7 -99.9(2) . . . . ? C18 C13 P1 C1 -22.8(3) . . . . ? C14 C13 P1 C1 153.1(2) . . . . ? C18 C13 P1 Li1 -124.8(3) . . . 2_556 ? C14 C13 P1 Li1 51.1(3) . . . 2_556 ? C35 O3 Li1 O1 179.9(2) 2_556 . . . ? Li2 O3 Li1 O1 12.7(3) 2_556 . . . ? Li3 O3 Li1 O1 88.7(3) 2_556 . . . ? C35 O3 Li1 O1 78.2(3) 2_556 . . 2_556 ? Li2 O3 Li1 O1 -89.0(2) 2_556 . . 2_556 ? Li3 O3 Li1 O1 -12.90(18) 2_556 . . 2_556 ? C35 O3 Li1 P1 -6.4(4) 2_556 . . 2_556 ? Li2 O3 Li1 P1 -173.7(2) 2_556 . . 2_556 ? Li3 O3 Li1 P1 -97.6(3) 2_556 . . 2_556 ? C35 O3 Li1 Li3 91.1(3) 2_556 . . 2_556 ? Li2 O3 Li1 Li3 -76.1(2) 2_556 . . 2_556 ? C35 O3 Li1 Li1 122.9(3) 2_556 . . 2_556 ? Li2 O3 Li1 Li1 -44.3(3) 2_556 . . 2_556 ? Li3 O3 Li1 Li1 31.8(3) 2_556 . . 2_556 ? C35 O3 Li1 Li2 167.2(3) 2_556 . . 2_556 ? Li3 O3 Li1 Li2 76.1(2) 2_556 . . 2_556 ? C2 O1 Li1 O3 20.9(3) . . . . ? Li3 O1 Li1 O3 180.0(2) . . . . ? Li1 O1 Li1 O3 -102.6(3) 2_556 . . . ? C2 O1 Li1 O1 123.48(19) . . . 2_556 ? Li3 O1 Li1 O1 -77.5(2) . . . 2_556 ? Li1 O1 Li1 O1 0.0 2_556 . . 2_556 ? C2 O1 Li1 P1 -153.34(19) . . . 2_556 ? Li3 O1 Li1 P1 5.7(3) . . . 2_556 ? Li1 O1 Li1 P1 83.2(2) 2_556 . . 2_556 ? C2 O1 Li1 Li3 76.4(2) . . . 2_556 ? Li3 O1 Li1 Li3 -124.53(17) . . . 2_556 ? Li1 O1 Li1 Li3 -47.07(16) 2_556 . . 2_556 ? C2 O1 Li1 Li1 123.48(19) . . . 2_556 ? Li3 O1 Li1 Li1 -77.5(2) . . . 2_556 ? C2 O1 Li1 Li2 28.41(19) . . . 2_556 ? Li3 O1 Li1 Li2 -172.52(18) . . . 2_556 ? Li1 O1 Li1 Li2 -95.06(18) 2_556 . . 2_556 ? C8 O2 Li2 O3 176.2(2) 2_556 . . 2_556 ? Li3 O2 Li2 O3 13.0(2) . . . 2_556 ? C8 O2 Li2 C1 59.3(3) 2_556 . . 2_556 ? Li3 O2 Li2 C1 -104.0(2) . . . 2_556 ? C8 O2 Li2 Li3 163.3(3) 2_556 . . . ? C8 O2 Li2 C6 30.0(3) 2_556 . . 2_556 ? Li3 O2 Li2 C6 -133.2(2) . . . 2_556 ? Li3 O2 Li2 C8 -163.3(3) . . . 2_556 ? C8 O2 Li2 C2 84.3(3) 2_556 . . 2_556 ? Li3 O2 Li2 C2 -79.0(2) . . . 2_556 ? C8 O2 Li2 Li1 139.4(2) 2_556 . . 2_556 ? Li3 O2 Li2 Li1 -23.9(2) . . . 2_556 ? C8 O2 Li3 O1 -57.8(6) 2_556 . . . ? Li2 O2 Li3 O1 93.4(4) . . . . ? C8 O2 Li3 O3 -162.9(3) 2_556 . . 2_556 ? Li2 O2 Li3 O3 -11.7(2) . . . 2_556 ? C8 O2 Li3 Li2 -151.2(5) 2_556 . . . ? C8 O2 Li3 Li1 -119.7(4) 2_556 . . 2_556 ? Li2 O2 Li3 Li1 31.5(3) . . . 2_556 ? C2 O1 Li3 O2 137.4(3) . . . . ? Li1 O1 Li3 O2 -9.2(4) . . . . ? Li1 O1 Li3 O2 -89.9(4) 2_556 . . . ? C2 O1 Li3 O3 -119.8(3) . . . 2_556 ? Li1 O1 Li3 O3 93.5(2) . . . 2_556 ? Li1 O1 Li3 O3 12.87(18) 2_556 . . 2_556 ? C2 O1 Li3 Li2 -164.6(3) . . . . ? Li1 O1 Li3 Li2 48.7(3) . . . . ? Li1 O1 Li3 Li2 -31.9(2) 2_556 . . . ? C2 O1 Li3 Li1 -132.7(3) . . . 2_556 ? Li1 O1 Li3 Li1 80.7(2) . . . 2_556 ? O3 Li2 Li3 O2 -163.9(3) 2_556 . . . ? C1 Li2 Li3 O2 81.5(2) 2_556 . . . ? C6 Li2 Li3 O2 66.0(3) 2_556 . . . ? C8 Li2 Li3 O2 7.28(12) 2_556 . . . ? C2 Li2 Li3 O2 112.0(2) 2_556 . . . ? Li1 Li2 Li3 O2 150.1(2) 2_556 . . . ? O2 Li2 Li3 O1 -123.7(3) . . . . ? O3 Li2 Li3 O1 72.3(3) 2_556 . . . ? C1 Li2 Li3 O1 -42.3(3) 2_556 . . . ? C6 Li2 Li3 O1 -57.8(4) 2_556 . . . ? C8 Li2 Li3 O1 -116.5(3) 2_556 . . . ? C2 Li2 Li3 O1 -11.8(3) 2_556 . . . ? Li1 Li2 Li3 O1 26.4(2) 2_556 . . . ? O2 Li2 Li3 O3 163.9(3) . . . 2_556 ? C1 Li2 Li3 O3 -114.6(2) 2_556 . . 2_556 ? C6 Li2 Li3 O3 -130.1(3) 2_556 . . 2_556 ? C8 Li2 Li3 O3 171.2(2) 2_556 . . 2_556 ? C2 Li2 Li3 O3 -84.09(18) 2_556 . . 2_556 ? Li1 Li2 Li3 O3 -45.94(16) 2_556 . . 2_556 ? O2 Li2 Li3 Li1 -150.1(2) . . . 2_556 ? O3 Li2 Li3 Li1 45.94(16) 2_556 . . 2_556 ? C1 Li2 Li3 Li1 -68.67(19) 2_556 . . 2_556 ? C6 Li2 Li3 Li1 -84.2(3) 2_556 . . 2_556 ? C8 Li2 Li3 Li1 -142.85(18) 2_556 . . 2_556 ? C2 Li2 Li3 Li1 -38.15(16) 2_556 . . 2_556 ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.869 _refine_diff_density_max 1.926 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.059 data_'[[OPO]Li3Cl(ArOLi)](THF)3' _database_code_depnum_ccdc_archive 'CCDC 653595' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C57 H92 Cl Li4 O6 P' _chemical_formula_sum 'C57 H92 Cl Li4 O6 P' _chemical_formula_weight 968.55 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' 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 17.7457(3) _cell_length_b 18.2033(4) _cell_length_c 18.3850(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5938.91(19) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1546 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 24.63 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.082 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 0.135 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9013 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 130426 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.05 _reflns_number_total 6708 _reflns_number_gt 5011 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+4.0986P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6708 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1658 _refine_ls_wR_factor_gt 0.1482 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.25985(10) 0.17198(10) 0.57582(10) 0.0243(4) Uani 1 1 d . . . C2 C 0.28356(10) 0.13881(10) 0.50971(10) 0.0253(4) Uani 1 1 d . . . C3 C 0.24081(11) 0.07656(11) 0.48404(11) 0.0296(4) Uani 1 1 d . . . C4 C 0.17556(12) 0.05738(11) 0.52182(12) 0.0340(5) Uani 1 1 d . . . H4 H 0.1475 0.0182 0.5041 0.041 Uiso 1 1 calc R . . C5 C 0.14920(11) 0.09283(11) 0.58452(12) 0.0326(5) Uani 1 1 d . A . C6 C 0.19401(11) 0.14935(11) 0.61114(11) 0.0288(4) Uani 1 1 d . . . H6 H 0.1798 0.1729 0.6539 0.035 Uiso 1 1 calc R . . C7 C 0.07307(14) 0.07367(13) 0.61903(15) 0.0475(6) Uani 1 1 d . . . C11 C 0.26541(12) 0.03141(12) 0.41700(12) 0.0349(5) Uani 1 1 d . . . C12 C 0.21301(17) -0.03443(15) 0.40228(16) 0.0571(7) Uani 1 1 d . . . H12A H 0.2317 -0.0619 0.3615 0.086 Uiso 1 1 calc R . . H12B H 0.1632 -0.0169 0.3918 0.086 Uiso 1 1 calc R . . H12C H 0.2115 -0.0655 0.4444 0.086 Uiso 1 1 calc R . . C13 C 0.34460(15) 0.00041(14) 0.42970(15) 0.0504(6) Uani 1 1 d . . . H13A H 0.3641 -0.0188 0.3848 0.076 Uiso 1 1 calc R . . H13B H 0.3422 -0.0382 0.4652 0.076 Uiso 1 1 calc R . . H13C H 0.3771 0.0388 0.4470 0.076 Uiso 1 1 calc R . . C14 C 0.26471(15) 0.07846(14) 0.34737(12) 0.0445(6) Uani 1 1 d . . . H14A H 0.2990 0.1189 0.3529 0.067 Uiso 1 1 calc R . . H14B H 0.2148 0.0969 0.3391 0.067 Uiso 1 1 calc R . . H14C H 0.2800 0.0489 0.3067 0.067 Uiso 1 1 calc R . . C15 C 0.29826(16) 0.2500 0.71044(15) 0.0286(6) Uani 1 2 d S . . H15 H 0.2439 0.2500 0.7198 0.034 Uiso 1 2 calc SR . . C16 C 0.33299(14) 0.18057(14) 0.74348(12) 0.0438(6) Uani 1 1 d . . . H16A H 0.3859 0.1791 0.7325 0.066 Uiso 1 1 calc R . . H16B H 0.3088 0.1380 0.7234 0.066 Uiso 1 1 calc R . . H16C H 0.3261 0.1811 0.7953 0.066 Uiso 1 1 calc R . . C17 C 0.56242(15) 0.2500 0.45735(16) 0.0287(6) Uani 1 2 d S . . C18 C 0.59792(17) 0.2500 0.38901(16) 0.0376(7) Uani 1 2 d S . . H18 H 0.5684 0.2500 0.3472 0.045 Uiso 1 2 calc SR . . C19 C 0.67582(17) 0.2500 0.38218(17) 0.0383(7) Uani 1 2 d S . . H19 H 0.6973 0.2500 0.3361 0.046 Uiso 1 2 calc SR . . C20 C 0.72206(15) 0.2500 0.44279(17) 0.0317(6) Uani 1 2 d S . . C21 C 0.68648(15) 0.2500 0.51053(16) 0.0310(6) Uani 1 2 d S . . H21 H 0.7167 0.2500 0.5519 0.037 Uiso 1 2 calc SR . . C22 C 0.60776(15) 0.2500 0.52018(15) 0.0278(6) Uani 1 2 d S . . C23 C 0.57399(15) 0.2500 0.59711(15) 0.0310(6) Uani 1 2 d S . . C24 C 0.52685(12) 0.17995(12) 0.60881(12) 0.0355(5) Uani 1 1 d . . . H24A H 0.4897 0.1761 0.5711 0.053 Uiso 1 1 calc R . . H24B H 0.5022 0.1824 0.6552 0.053 Uiso 1 1 calc R . . H24C H 0.5593 0.1377 0.6074 0.053 Uiso 1 1 calc R . . C25 C 0.63486(19) 0.2500 0.65722(18) 0.0495(9) Uani 1 2 d S . . H25A H 0.6110 0.2500 0.7041 0.074 Uiso 1 2 calc SR . . H25B H 0.6657 0.2931 0.6525 0.074 Uiso 0.50 1 calc PR . . H25C H 0.6657 0.2069 0.6525 0.074 Uiso 0.50 1 calc PR . . C26 C 0.80854(16) 0.2500 0.43444(19) 0.0377(7) Uani 1 2 d S . . C27 C 0.84870(17) 0.2500 0.5080(2) 0.0548(10) Uani 1 2 d S . . H27A H 0.8341 0.2928 0.5351 0.082 Uiso 0.50 1 calc PR . . H27B H 0.9022 0.2506 0.5005 0.082 Uiso 1 2 calc SR . . H27C H 0.8350 0.2067 0.5347 0.082 Uiso 0.50 1 calc PR . . C28 C 0.83273(14) 0.31884(15) 0.39218(16) 0.0535(7) Uani 1 1 d . . . H28A H 0.8179 0.3619 0.4187 0.080 Uiso 1 1 calc R . . H28B H 0.8090 0.3189 0.3453 0.080 Uiso 1 1 calc R . . H28C H 0.8865 0.3187 0.3862 0.080 Uiso 1 1 calc R . . C29 C 0.55506(17) 0.05951(17) 0.41733(15) 0.0587(7) Uani 1 1 d . . . H29A H 0.5313 0.0222 0.4472 0.070 Uiso 1 1 calc R . . H29B H 0.5796 0.0947 0.4491 0.070 Uiso 1 1 calc R . . C30 C 0.6100(3) 0.0260(3) 0.3681(2) 0.1154(18) Uani 1 1 d . . . H30A H 0.6593 0.0476 0.3757 0.138 Uiso 1 1 calc R . . H30B H 0.6134 -0.0264 0.3773 0.138 Uiso 1 1 calc R . . C31 C 0.5856(2) 0.0388(3) 0.29537(19) 0.0896(13) Uani 1 1 d . . . H31A H 0.5802 -0.0075 0.2697 0.107 Uiso 1 1 calc R . . H31B H 0.6222 0.0687 0.2697 0.107 Uiso 1 1 calc R . . C32 C 0.5130(2) 0.0769(3) 0.29851(17) 0.0939(14) Uani 1 1 d . . . H32A H 0.5143 0.1208 0.2686 0.113 Uiso 1 1 calc R . . H32B H 0.4731 0.0452 0.2807 0.113 Uiso 1 1 calc R . . C33 C 0.13049(17) 0.2500 0.44569(18) 0.0427(8) Uani 1 2 d S . . H33A H 0.1297 0.2963 0.4718 0.051 Uiso 0.50 1 calc PR . . H33B H 0.1383 0.2105 0.4803 0.051 Uiso 0.50 1 calc PR . . C34 C 0.0591(3) 0.239(2) 0.4046(3) 0.089(7) Uani 0.50 1 d P . . H34A H 0.0302 0.1996 0.4265 0.106 Uiso 0.50 1 calc PR . . H34B H 0.0291 0.2836 0.4065 0.106 Uiso 0.50 1 calc PR . . C35 C 0.0751(3) 0.2222(3) 0.3340(3) 0.0631(17) Uani 0.50 1 d P . . H35A H 0.0395 0.2459 0.3015 0.076 Uiso 0.50 1 calc PR . . H35B H 0.0724 0.1695 0.3264 0.076 Uiso 0.50 1 calc PR . . C36 C 0.1545(2) 0.2500 0.31994(18) 0.0456(8) Uani 1 2 d S . . H36A H 0.1813 0.2176 0.2870 0.055 Uiso 0.50 1 calc PR . . H36B H 0.1537 0.2991 0.2995 0.055 Uiso 0.50 1 calc PR . . O1 O 0.34181(7) 0.16790(7) 0.47262(7) 0.0273(3) Uani 1 1 d . . . O2 O 0.48609(10) 0.2500 0.45932(11) 0.0318(5) Uani 1 2 d S . . O3 O 0.49960(9) 0.09586(10) 0.37238(9) 0.0484(4) Uani 1 1 d . . . O4 O 0.18890(11) 0.2500 0.39083(11) 0.0367(5) Uani 1 2 d S . . P1 P 0.31455(4) 0.2500 0.61039(4) 0.02216(17) Uani 1 2 d S . . Cl1 Cl 0.38205(3) 0.2500 0.30983(3) 0.02725(17) Uani 1 2 d S . . Li1 Li 0.2954(3) 0.2500 0.4132(3) 0.0338(11) Uani 1 2 d S . . Li2 Li 0.4310(2) 0.1706(2) 0.4062(2) 0.0368(8) Uani 1 1 d . . . Li3 Li 0.4022(3) 0.2500 0.5152(3) 0.0298(10) Uani 1 2 d S . . C8 C 0.0604(6) -0.0086(6) 0.6223(5) 0.053(2) Uani 0.696(10) 1 d P A 1 H8A H 0.0965 -0.0303 0.6548 0.080 Uiso 0.696(10) 1 calc PR A 1 H8B H 0.0664 -0.0292 0.5746 0.080 Uiso 0.696(10) 1 calc PR A 1 H8C H 0.0104 -0.0184 0.6398 0.080 Uiso 0.696(10) 1 calc PR A 1 C9 C 0.0603(3) 0.1079(3) 0.6908(3) 0.0575(18) Uani 0.696(10) 1 d P A 1 H9A H 0.0128 0.0916 0.7100 0.086 Uiso 0.696(10) 1 calc PR A 1 H9B H 0.0597 0.1603 0.6857 0.086 Uiso 0.696(10) 1 calc PR A 1 H9C H 0.1000 0.0938 0.7234 0.086 Uiso 0.696(10) 1 calc PR A 1 C10 C 0.0101(2) 0.1059(4) 0.5643(3) 0.0679(18) Uani 0.696(10) 1 d P A 1 H10A H -0.0392 0.0950 0.5829 0.102 Uiso 0.696(10) 1 calc PR A 1 H10B H 0.0160 0.0837 0.5172 0.102 Uiso 0.696(10) 1 calc PR A 1 H10C H 0.0160 0.1582 0.5601 0.102 Uiso 0.696(10) 1 calc PR A 1 C100 C 0.0434(14) 0.0019(15) 0.5990(11) 0.057(5) Uani 0.304(10) 1 d P A 2 H10D H 0.0034 -0.0112 0.6316 0.085 Uiso 0.304(10) 1 calc PR A 2 H10E H 0.0829 -0.0340 0.6019 0.085 Uiso 0.304(10) 1 calc PR A 2 H10F H 0.0244 0.0038 0.5501 0.085 Uiso 0.304(10) 1 calc PR A 2 C101 C 0.0253(7) 0.1336(7) 0.6278(13) 0.111(10) Uani 0.304(10) 1 d P A 2 H10G H 0.0141 0.1545 0.5811 0.166 Uiso 0.304(10) 1 calc PR A 2 H10H H 0.0494 0.1698 0.6577 0.166 Uiso 0.304(10) 1 calc PR A 2 H10I H -0.0206 0.1178 0.6505 0.166 Uiso 0.304(10) 1 calc PR A 2 C102 C 0.1016(10) 0.0536(10) 0.7120(6) 0.094(7) Uani 0.304(10) 1 d P A 2 H10J H 0.1368 0.0900 0.7282 0.141 Uiso 0.304(10) 1 calc PR A 2 H10K H 0.1248 0.0060 0.7137 0.141 Uiso 0.304(10) 1 calc PR A 2 H10L H 0.0581 0.0540 0.7430 0.141 Uiso 0.304(10) 1 calc PR A 2 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 C1 0.0236(9) 0.0241(9) 0.0253(9) -0.0003(7) -0.0027(7) 0.0016(7) C2 0.0225(9) 0.0268(9) 0.0264(10) 0.0007(8) -0.0017(7) 0.0027(7) C3 0.0312(10) 0.0280(10) 0.0296(10) -0.0042(8) -0.0009(8) 0.0000(8) C4 0.0345(11) 0.0283(10) 0.0392(12) -0.0072(9) 0.0000(9) -0.0066(8) C5 0.0309(10) 0.0303(10) 0.0366(11) -0.0029(9) 0.0049(9) -0.0046(8) C6 0.0296(10) 0.0290(10) 0.0277(10) -0.0031(8) 0.0039(8) -0.0002(8) C7 0.0415(13) 0.0388(13) 0.0621(16) -0.0103(11) 0.0183(12) -0.0139(10) C11 0.0375(11) 0.0330(11) 0.0342(11) -0.0091(9) 0.0017(9) -0.0001(9) C12 0.0717(18) 0.0456(14) 0.0541(16) -0.0245(12) 0.0132(14) -0.0149(13) C13 0.0523(15) 0.0463(14) 0.0526(15) -0.0136(12) 0.0009(12) 0.0173(12) C14 0.0551(14) 0.0476(14) 0.0309(12) -0.0108(10) -0.0038(10) 0.0009(11) C15 0.0281(14) 0.0354(15) 0.0222(13) 0.000 0.0005(11) 0.000 C16 0.0464(13) 0.0553(14) 0.0297(11) 0.0120(10) -0.0002(10) 0.0098(11) C17 0.0199(12) 0.0366(15) 0.0296(15) 0.000 -0.0005(11) 0.000 C18 0.0300(15) 0.059(2) 0.0235(15) 0.000 -0.0012(12) 0.000 C19 0.0302(15) 0.0550(19) 0.0298(16) 0.000 0.0085(13) 0.000 C20 0.0219(13) 0.0356(15) 0.0377(16) 0.000 0.0043(12) 0.000 C21 0.0229(13) 0.0402(16) 0.0297(15) 0.000 -0.0020(11) 0.000 C22 0.0220(13) 0.0341(14) 0.0272(14) 0.000 0.0001(11) 0.000 C23 0.0214(13) 0.0462(17) 0.0255(14) 0.000 -0.0002(11) 0.000 C24 0.0306(10) 0.0414(12) 0.0346(11) 0.0082(9) 0.0040(9) 0.0057(9) C25 0.0343(17) 0.088(3) 0.0265(16) 0.000 -0.0025(13) 0.000 C26 0.0226(14) 0.0437(17) 0.0469(19) 0.000 0.0103(13) 0.000 C27 0.0194(15) 0.082(3) 0.063(2) 0.000 -0.0010(15) 0.000 C28 0.0349(12) 0.0521(15) 0.0736(19) 0.0070(13) 0.0175(12) -0.0055(11) C29 0.0615(17) 0.0674(18) 0.0471(15) 0.0017(13) 0.0033(13) 0.0241(14) C30 0.103(3) 0.168(4) 0.075(3) -0.016(3) 0.005(2) 0.087(3) C31 0.069(2) 0.140(4) 0.059(2) -0.028(2) 0.0144(17) 0.031(2) C32 0.106(3) 0.134(3) 0.0421(16) -0.0310(19) -0.0048(17) 0.058(3) C33 0.0265(15) 0.067(2) 0.0347(17) 0.000 0.0026(13) 0.000 C34 0.031(2) 0.17(2) 0.061(3) 0.002(7) -0.005(2) -0.033(9) C35 0.051(3) 0.087(5) 0.051(3) -0.004(3) -0.019(2) -0.011(3) C36 0.048(2) 0.060(2) 0.0295(17) 0.000 -0.0087(15) 0.000 O1 0.0237(7) 0.0321(7) 0.0260(7) -0.0023(6) 0.0019(5) -0.0008(5) O2 0.0181(9) 0.0486(12) 0.0287(10) 0.000 -0.0005(8) 0.000 O3 0.0443(9) 0.0625(11) 0.0384(9) -0.0102(8) 0.0023(7) 0.0153(8) O4 0.0260(10) 0.0544(13) 0.0296(11) 0.000 -0.0022(8) 0.000 P1 0.0209(3) 0.0253(3) 0.0202(3) 0.000 -0.0007(3) 0.000 Cl1 0.0209(3) 0.0414(4) 0.0194(3) 0.000 -0.0024(2) 0.000 Li1 0.026(2) 0.045(3) 0.031(3) 0.000 -0.002(2) 0.000 Li2 0.0332(18) 0.047(2) 0.0305(18) -0.0061(16) -0.0007(15) 0.0037(16) Li3 0.021(2) 0.040(3) 0.029(2) 0.000 0.0004(18) 0.000 C8 0.066(6) 0.042(3) 0.052(5) -0.006(3) 0.028(3) -0.019(3) C9 0.049(2) 0.060(3) 0.064(3) -0.024(3) 0.031(2) -0.025(2) C10 0.0253(18) 0.092(4) 0.086(4) 0.022(3) 0.002(2) -0.008(2) C100 0.046(8) 0.063(11) 0.061(12) -0.007(9) 0.007(7) -0.017(7) C101 0.056(8) 0.070(8) 0.21(3) 0.011(11) 0.071(13) 0.003(6) C102 0.121(12) 0.117(13) 0.045(6) 0.006(6) 0.004(6) -0.083(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.399(3) . ? C1 C2 1.421(3) . ? C1 P1 1.8339(19) . ? C2 O1 1.347(2) . ? C2 C3 1.443(3) . ? C3 C4 1.395(3) . ? C3 C11 1.544(3) . ? C4 C5 1.401(3) . ? C4 H4 0.9300 . ? C5 C6 1.389(3) . ? C5 C7 1.533(3) . ? C6 H6 0.9300 . ? C7 C101 1.391(12) . ? C7 C100 1.46(3) . ? C7 C9 1.476(5) . ? C7 C8 1.515(11) . ? C7 C10 1.615(5) . ? C7 C102 1.819(13) . ? C11 C13 1.532(3) . ? C11 C14 1.540(3) . ? C11 C12 1.541(3) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.532(3) 8_565 ? C15 C16 1.532(3) . ? C15 P1 1.862(3) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O2 1.355(3) . ? C17 C18 1.405(4) . ? C17 C22 1.408(4) . ? C18 C19 1.388(4) . ? C18 H18 0.9300 . ? C19 C20 1.384(4) . ? C19 H19 0.9300 . ? C20 C21 1.396(4) . ? C20 C26 1.542(4) . ? C21 C22 1.408(4) . ? C21 H21 0.9300 . ? C22 C23 1.536(4) . ? C23 C24 1.540(3) . ? C23 C24 1.540(3) 8_565 ? C23 C25 1.545(4) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.529(5) . ? C26 C28 1.536(3) 8_565 ? C26 C28 1.536(3) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 O3 1.445(3) . ? C29 C30 1.463(4) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.426(5) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.464(5) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 O3 1.421(3) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 O4 1.446(4) . ? C33 C34 1.489(7) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.363(11) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.521(6) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 O4 1.439(4) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? O1 Li3 1.999(3) . ? O1 Li2 2.000(4) . ? O1 Li1 2.027(4) . ? O2 Li3 1.810(5) . ? O2 Li2 2.000(4) . ? O2 Li2 2.000(4) 8_565 ? O3 Li2 1.929(4) . ? O4 Li1 1.933(5) . ? P1 C1 1.8339(19) 8_565 ? P1 Li3 2.340(5) . ? Cl1 Li1 2.445(5) . ? Cl1 Li2 2.445(4) 8_565 ? Cl1 Li2 2.445(4) . ? Li1 O1 2.027(4) 8_565 ? Li1 C2 2.700(4) 8_565 ? Li1 Li2 2.810(5) 8_565 ? Li2 Li2 2.889(8) 8_565 ? Li3 O1 1.999(3) 8_565 ? Li3 Li2 2.524(5) 8_565 ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C100 H10D 0.9600 . ? C100 H10E 0.9600 . ? C100 H10F 0.9600 . ? C101 H10G 0.9600 . ? C101 H10H 0.9600 . ? C101 H10I 0.9600 . ? C102 H10J 0.9600 . ? C102 H10K 0.9600 . ? C102 H10L 0.9600 . ? 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 C6 C1 C2 121.29(17) . . ? C6 C1 P1 120.62(15) . . ? C2 C1 P1 117.96(14) . . ? O1 C2 C1 119.56(17) . . ? O1 C2 C3 123.14(17) . . ? C1 C2 C3 117.24(17) . . ? C4 C3 C2 118.04(18) . . ? C4 C3 C11 119.93(18) . . ? C2 C3 C11 122.03(17) . . ? C3 C4 C5 124.86(19) . . ? C3 C4 H4 117.6 . . ? C5 C4 H4 117.6 . . ? C6 C5 C4 116.08(18) . . ? C6 C5 C7 121.81(19) . . ? C4 C5 C7 122.01(19) . . ? C5 C6 C1 122.19(18) . . ? C5 C6 H6 118.9 . . ? C1 C6 H6 118.9 . . ? C101 C7 C100 120.8(12) . . ? C101 C7 C9 58.2(9) . . ? C100 C7 C9 123.3(10) . . ? C101 C7 C8 132.9(7) . . ? C100 C7 C8 21.6(7) . . ? C9 C7 C8 111.0(4) . . ? C101 C7 C5 114.0(5) . . ? C100 C7 C5 114.7(11) . . ? C9 C7 C5 114.2(2) . . ? C8 C7 C5 111.8(4) . . ? C101 C7 C10 50.6(9) . . ? C100 C7 C10 85.3(8) . . ? C9 C7 C10 107.3(4) . . ? C8 C7 C10 106.4(4) . . ? C5 C7 C10 105.6(2) . . ? C101 C7 C102 102.7(11) . . ? C100 C7 C102 99.1(8) . . ? C9 C7 C102 44.6(6) . . ? C8 C7 C102 78.7(5) . . ? C5 C7 C102 100.9(5) . . ? C10 C7 C102 148.4(6) . . ? C13 C11 C14 109.8(2) . . ? C13 C11 C12 107.1(2) . . ? C14 C11 C12 106.4(2) . . ? C13 C11 C3 109.48(18) . . ? C14 C11 C3 111.42(17) . . ? C12 C11 C3 112.55(18) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C16 111.2(3) 8_565 . ? C16 C15 P1 109.23(15) 8_565 . ? C16 C15 P1 109.23(15) . . ? C16 C15 H15 109.1 8_565 . ? C16 C15 H15 109.1 . . ? P1 C15 H15 109.1 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O2 C17 C18 118.2(3) . . ? O2 C17 C22 123.3(3) . . ? C18 C17 C22 118.5(2) . . ? C19 C18 C17 121.8(3) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C20 C19 C18 121.2(3) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 116.7(3) . . ? C19 C20 C26 120.7(3) . . ? C21 C20 C26 122.6(3) . . ? C20 C21 C22 124.1(3) . . ? C20 C21 H21 117.9 . . ? C22 C21 H21 117.9 . . ? C17 C22 C21 117.6(3) . . ? C17 C22 C23 122.2(2) . . ? C21 C22 C23 120.2(2) . . ? C22 C23 C24 109.90(15) . . ? C22 C23 C24 109.90(15) . 8_565 ? C24 C23 C24 111.8(2) . 8_565 ? C22 C23 C25 112.7(2) . . ? C24 C23 C25 106.25(16) . . ? C24 C23 C25 106.25(16) 8_565 . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C28 108.51(19) . 8_565 ? C27 C26 C28 108.51(19) . . ? C28 C26 C28 109.4(3) 8_565 . ? C27 C26 C20 112.1(3) . . ? C28 C26 C20 109.17(18) 8_565 . ? C28 C26 C20 109.17(18) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C29 C30 106.9(3) . . ? O3 C29 H29A 110.3 . . ? C30 C29 H29A 110.3 . . ? O3 C29 H29B 110.3 . . ? C30 C29 H29B 110.3 . . ? H29A C29 H29B 108.6 . . ? C31 C30 C29 108.0(3) . . ? C31 C30 H30A 110.1 . . ? C29 C30 H30A 110.1 . . ? C31 C30 H30B 110.1 . . ? C29 C30 H30B 110.1 . . ? H30A C30 H30B 108.4 . . ? C30 C31 C32 107.9(3) . . ? C30 C31 H31A 110.1 . . ? C32 C31 H31A 110.1 . . ? C30 C31 H31B 110.1 . . ? C32 C31 H31B 110.1 . . ? H31A C31 H31B 108.4 . . ? O3 C32 C31 107.4(3) . . ? O3 C32 H32A 110.2 . . ? C31 C32 H32A 110.2 . . ? O3 C32 H32B 110.2 . . ? C31 C32 H32B 110.2 . . ? H32A C32 H32B 108.5 . . ? O4 C33 C34 104.8(3) . . ? O4 C33 H33A 110.8 . . ? C34 C33 H33A 110.8 . . ? O4 C33 H33B 110.8 . . ? C34 C33 H33B 110.8 . . ? H33A C33 H33B 108.9 . . ? C35 C34 C33 109.7(5) . . ? C35 C34 H34A 109.7 . . ? C33 C34 H34A 109.7 . . ? C35 C34 H34B 109.7 . . ? C33 C34 H34B 109.7 . . ? H34A C34 H34B 108.2 . . ? C34 C35 C36 106.2(8) . . ? C34 C35 H35A 110.5 . . ? C36 C35 H35A 110.5 . . ? C34 C35 H35B 110.5 . . ? C36 C35 H35B 110.5 . . ? H35A C35 H35B 108.7 . . ? O4 C36 C35 103.8(3) . . ? O4 C36 H36A 111.0 . . ? C35 C36 H36A 111.0 . . ? O4 C36 H36B 111.0 . . ? C35 C36 H36B 111.0 . . ? H36A C36 H36B 109.0 . . ? C2 O1 Li3 120.44(18) . . ? C2 O1 Li2 157.89(17) . . ? Li3 O1 Li2 78.28(18) . . ? C2 O1 Li1 104.52(17) . . ? Li3 O1 Li1 82.99(15) . . ? Li2 O1 Li1 88.51(19) . . ? C17 O2 Li3 146.9(2) . . ? C17 O2 Li2 118.41(15) . . ? Li3 O2 Li2 82.83(16) . . ? C17 O2 Li2 118.41(15) . 8_565 ? Li3 O2 Li2 82.83(16) . 8_565 ? Li2 O2 Li2 92.5(2) . 8_565 ? C32 O3 C29 108.8(2) . . ? C32 O3 Li2 125.7(2) . . ? C29 O3 Li2 124.66(18) . . ? C36 O4 C33 109.1(2) . . ? C36 O4 Li1 127.3(2) . . ? C33 O4 Li1 123.5(2) . . ? C1 P1 C1 101.51(12) . 8_565 ? C1 P1 C15 105.08(8) . . ? C1 P1 C15 105.08(8) 8_565 . ? C1 P1 Li3 95.31(9) . . ? C1 P1 Li3 95.31(10) 8_565 . ? C15 P1 Li3 147.30(15) . . ? Li1 Cl1 Li2 70.16(12) . 8_565 ? Li1 Cl1 Li2 70.16(12) . . ? Li2 Cl1 Li2 72.44(18) 8_565 . ? O4 Li1 O1 120.80(17) . 8_565 ? O4 Li1 O1 120.80(17) . . ? O1 Li1 O1 95.0(2) 8_565 . ? O4 Li1 Cl1 116.7(2) . . ? O1 Li1 Cl1 99.39(17) 8_565 . ? O1 Li1 Cl1 99.39(17) . . ? O4 Li1 C2 93.66(16) . 8_565 ? O1 Li1 C2 28.87(7) 8_565 8_565 ? O1 Li1 C2 103.3(2) . 8_565 ? Cl1 Li1 C2 124.03(12) . 8_565 ? O4 Li1 Li2 145.81(14) . 8_565 ? O1 Li1 Li2 45.36(12) 8_565 8_565 ? O1 Li1 Li2 93.18(19) . 8_565 ? Cl1 Li1 Li2 54.92(12) . 8_565 ? C2 Li1 Li2 73.22(12) 8_565 8_565 ? O3 Li2 O2 111.01(19) . . ? O3 Li2 O1 132.7(2) . . ? O2 Li2 O1 96.11(16) . . ? O3 Li2 Cl1 114.07(17) . . ? O2 Li2 Cl1 95.79(16) . . ? O1 Li2 Cl1 100.15(15) . . ? O3 Li2 Li2 134.88(13) . 8_565 ? O2 Li2 Li2 43.74(11) . 8_565 ? O1 Li2 Li2 91.43(12) . 8_565 ? Cl1 Li2 Li2 53.78(9) . 8_565 ? O2 Li3 O1 102.61(18) . . ? O2 Li3 O1 102.61(18) . 8_565 ? O1 Li3 O1 96.8(2) . 8_565 ? O2 Li3 P1 166.2(3) . . ? O1 Li3 P1 86.40(15) . . ? O1 Li3 P1 86.40(15) 8_565 . ? O2 Li3 Li2 51.82(14) . 8_565 ? O1 Li3 Li2 103.0(2) . 8_565 ? O1 Li3 Li2 50.88(12) 8_565 8_565 ? P1 Li3 Li2 136.77(15) . 8_565 ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? C7 C100 H10D 109.5 . . ? C7 C100 H10E 109.5 . . ? H10D C100 H10E 109.5 . . ? C7 C100 H10F 109.5 . . ? H10D C100 H10F 109.5 . . ? H10E C100 H10F 109.5 . . ? C7 C101 H10G 109.5 . . ? C7 C101 H10H 109.5 . . ? H10G C101 H10H 109.5 . . ? C7 C101 H10I 109.5 . . ? H10G C101 H10I 109.5 . . ? H10H C101 H10I 109.5 . . ? C7 C102 H10J 109.5 . . ? C7 C102 H10K 109.5 . . ? H10J C102 H10K 109.5 . . ? C7 C102 H10L 109.5 . . ? H10J C102 H10L 109.5 . . ? H10K C102 H10L 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 O1 171.80(17) . . . . ? P1 C1 C2 O1 -3.9(2) . . . . ? C6 C1 C2 C3 -5.5(3) . . . . ? P1 C1 C2 C3 178.78(14) . . . . ? O1 C2 C3 C4 -171.43(18) . . . . ? C1 C2 C3 C4 5.7(3) . . . . ? O1 C2 C3 C11 8.7(3) . . . . ? C1 C2 C3 C11 -174.09(18) . . . . ? C2 C3 C4 C5 -1.9(3) . . . . ? C11 C3 C4 C5 177.9(2) . . . . ? C3 C4 C5 C6 -2.4(3) . . . . ? C3 C4 C5 C7 174.0(2) . . . . ? C4 C5 C6 C1 2.8(3) . . . . ? C7 C5 C6 C1 -173.6(2) . . . . ? C2 C1 C6 C5 1.2(3) . . . . ? P1 C1 C6 C5 176.79(16) . . . . ? C6 C5 C7 C101 51.2(12) . . . . ? C4 C5 C7 C101 -125.0(12) . . . . ? C6 C5 C7 C100 -163.5(8) . . . . ? C4 C5 C7 C100 20.3(8) . . . . ? C6 C5 C7 C9 -13.2(4) . . . . ? C4 C5 C7 C9 170.7(3) . . . . ? C6 C5 C7 C8 -140.2(4) . . . . ? C4 C5 C7 C8 43.7(5) . . . . ? C6 C5 C7 C10 104.5(4) . . . . ? C4 C5 C7 C10 -71.6(4) . . . . ? C6 C5 C7 C102 -58.1(7) . . . . ? C4 C5 C7 C102 125.8(7) . . . . ? C4 C3 C11 C13 -121.5(2) . . . . ? C2 C3 C11 C13 58.3(3) . . . . ? C4 C3 C11 C14 116.8(2) . . . . ? C2 C3 C11 C14 -63.3(3) . . . . ? C4 C3 C11 C12 -2.5(3) . . . . ? C2 C3 C11 C12 177.3(2) . . . . ? O2 C17 C18 C19 180.0 . . . . ? C22 C17 C18 C19 0.0 . . . . ? C17 C18 C19 C20 0.0 . . . . ? C18 C19 C20 C21 0.0 . . . . ? C18 C19 C20 C26 180.0 . . . . ? C19 C20 C21 C22 0.0 . . . . ? C26 C20 C21 C22 180.0 . . . . ? O2 C17 C22 C21 180.0 . . . . ? C18 C17 C22 C21 0.0 . . . . ? O2 C17 C22 C23 0.0 . . . . ? C18 C17 C22 C23 180.0 . . . . ? C20 C21 C22 C17 0.0 . . . . ? C20 C21 C22 C23 180.0 . . . . ? C17 C22 C23 C24 61.70(16) . . . . ? C21 C22 C23 C24 -118.30(16) . . . . ? C17 C22 C23 C24 -61.70(16) . . . 8_565 ? C21 C22 C23 C24 118.30(16) . . . 8_565 ? C17 C22 C23 C25 180.0 . . . . ? C21 C22 C23 C25 0.0 . . . . ? C19 C20 C26 C27 180.0 . . . . ? C21 C20 C26 C27 0.0 . . . . ? C19 C20 C26 C28 -59.8(2) . . . 8_565 ? C21 C20 C26 C28 120.2(2) . . . 8_565 ? C19 C20 C26 C28 59.8(2) . . . . ? C21 C20 C26 C28 -120.2(2) . . . . ? O3 C29 C30 C31 -3.0(5) . . . . ? C29 C30 C31 C32 -3.1(6) . . . . ? C30 C31 C32 O3 8.1(6) . . . . ? O4 C33 C34 C35 9(3) . . . . ? C33 C34 C35 C36 -21(3) . . . . ? C34 C35 C36 O4 25.6(16) . . . . ? C1 C2 O1 Li3 6.9(3) . . . . ? C3 C2 O1 Li3 -175.99(18) . . . . ? C1 C2 O1 Li2 152.1(4) . . . . ? C3 C2 O1 Li2 -30.8(5) . . . . ? C1 C2 O1 Li1 -83.4(2) . . . . ? C3 C2 O1 Li1 93.7(2) . . . . ? C18 C17 O2 Li3 180.0 . . . . ? C22 C17 O2 Li3 0.0 . . . . ? C18 C17 O2 Li2 55.22(16) . . . . ? C22 C17 O2 Li2 -124.78(16) . . . . ? C18 C17 O2 Li2 -55.22(16) . . . 8_565 ? C22 C17 O2 Li2 124.78(16) . . . 8_565 ? C31 C32 O3 C29 -10.0(5) . . . . ? C31 C32 O3 Li2 159.9(3) . . . . ? C30 C29 O3 C32 8.1(4) . . . . ? C30 C29 O3 Li2 -162.0(3) . . . . ? C35 C36 O4 C33 -20.1(3) . . . . ? C35 C36 O4 Li1 159.9(3) . . . . ? C34 C33 O4 C36 7.9(16) . . . . ? C34 C33 O4 Li1 -172.1(16) . . . . ? C6 C1 P1 C1 -79.42(18) . . . 8_565 ? C2 C1 P1 C1 96.35(15) . . . 8_565 ? C6 C1 P1 C15 29.84(18) . . . . ? C2 C1 P1 C15 -154.38(15) . . . . ? C6 C1 P1 Li3 -175.95(17) . . . . ? C2 C1 P1 Li3 -0.18(17) . . . . ? C16 C15 P1 C1 -172.42(16) 8_565 . . . ? C16 C15 P1 C1 65.76(19) . . . . ? C16 C15 P1 C1 -65.76(19) 8_565 . . 8_565 ? C16 C15 P1 C1 172.42(16) . . . 8_565 ? C16 C15 P1 Li3 60.91(16) 8_565 . . . ? C16 C15 P1 Li3 -60.91(16) . . . . ? C36 O4 Li1 O1 120.9(2) . . . 8_565 ? C33 O4 Li1 O1 -59.1(2) . . . 8_565 ? C36 O4 Li1 O1 -120.9(2) . . . . ? C33 O4 Li1 O1 59.1(2) . . . . ? C36 O4 Li1 Cl1 0.0 . . . . ? C33 O4 Li1 Cl1 180.0 . . . . ? C36 O4 Li1 C2 131.31(10) . . . 8_565 ? C33 O4 Li1 C2 -48.69(10) . . . 8_565 ? C36 O4 Li1 Li2 66.2(4) . . . 8_565 ? C33 O4 Li1 Li2 -113.8(4) . . . 8_565 ? C2 O1 Li1 O4 -22.0(3) . . . . ? Li3 O1 Li1 O4 -141.7(3) . . . . ? Li2 O1 Li1 O4 139.9(3) . . . . ? C2 O1 Li1 O1 108.57(18) . . . 8_565 ? Li3 O1 Li1 O1 -11.1(2) . . . 8_565 ? Li2 O1 Li1 O1 -89.51(19) . . . 8_565 ? C2 O1 Li1 Cl1 -151.03(13) . . . . ? Li3 O1 Li1 Cl1 89.27(17) . . . . ? Li2 O1 Li1 Cl1 10.89(15) . . . . ? C2 O1 Li1 C2 80.51(18) . . . 8_565 ? Li3 O1 Li1 C2 -39.19(19) . . . 8_565 ? Li2 O1 Li1 C2 -117.57(18) . . . 8_565 ? C2 O1 Li1 Li2 154.01(15) . . . 8_565 ? Li3 O1 Li1 Li2 34.31(18) . . . 8_565 ? Li2 O1 Li1 Li2 -44.07(17) . . . 8_565 ? Li2 Cl1 Li1 O4 141.09(10) 8_565 . . . ? Li2 Cl1 Li1 O4 -141.09(10) . . . . ? Li2 Cl1 Li1 O1 9.46(14) 8_565 . . 8_565 ? Li2 Cl1 Li1 O1 87.28(18) . . . 8_565 ? Li2 Cl1 Li1 O1 -87.28(18) 8_565 . . . ? Li2 Cl1 Li1 O1 -9.46(14) . . . . ? Li2 Cl1 Li1 C2 25.85(19) 8_565 . . 8_565 ? Li2 Cl1 Li1 C2 103.7(2) . . . 8_565 ? Li2 Cl1 Li1 Li2 77.8(2) . . . 8_565 ? C32 O3 Li2 O2 -117.6(3) . . . . ? C29 O3 Li2 O2 50.8(3) . . . . ? C32 O3 Li2 O1 121.7(4) . . . . ? C29 O3 Li2 O1 -69.9(4) . . . . ? C32 O3 Li2 Cl1 -10.8(4) . . . . ? C29 O3 Li2 Cl1 157.6(2) . . . . ? C32 O3 Li2 Li2 -72.8(3) . . . 8_565 ? C29 O3 Li2 Li2 95.6(2) . . . 8_565 ? C17 O2 Li2 O3 9.4(3) . . . . ? Li3 O2 Li2 O3 -143.8(2) . . . . ? Li2 O2 Li2 O3 133.79(14) 8_565 . . . ? C17 O2 Li2 O1 149.91(18) . . . . ? Li3 O2 Li2 O1 -3.23(16) . . . . ? Li2 O2 Li2 O1 -85.67(18) 8_565 . . . ? C17 O2 Li2 Cl1 -109.19(18) . . . . ? Li3 O2 Li2 Cl1 97.67(15) . . . . ? Li2 O2 Li2 Cl1 15.2(2) 8_565 . . . ? C17 O2 Li2 Li2 -124.4(2) . . . 8_565 ? Li3 O2 Li2 Li2 82.44(17) . . . 8_565 ? C2 O1 Li2 O3 -20.7(6) . . . . ? Li3 O1 Li2 O3 129.1(3) . . . . ? Li1 O1 Li2 O3 -147.8(3) . . . . ? C2 O1 Li2 O2 -146.9(4) . . . . ? Li3 O1 Li2 O2 2.96(15) . . . . ? Li1 O1 Li2 O2 86.11(17) . . . . ? C2 O1 Li2 Cl1 116.1(4) . . . . ? Li3 O1 Li2 Cl1 -94.06(16) . . . . ? Li1 O1 Li2 Cl1 -10.92(15) . . . . ? C2 O1 Li2 Li2 169.5(4) . . . 8_565 ? Li3 O1 Li2 Li2 -40.64(11) . . . 8_565 ? Li1 O1 Li2 Li2 42.50(11) . . . 8_565 ? Li1 Cl1 Li2 O3 156.2(2) . . . . ? Li2 Cl1 Li2 O3 -129.11(15) 8_565 . . . ? Li1 Cl1 Li2 O2 -87.68(15) . . . . ? Li2 Cl1 Li2 O2 -13.01(18) 8_565 . . . ? Li1 Cl1 Li2 O1 9.61(13) . . . . ? Li2 Cl1 Li2 O1 84.28(15) 8_565 . . . ? Li1 Cl1 Li2 Li2 -74.67(11) . . . 8_565 ? C17 O2 Li3 O1 -129.98(14) . . . . ? Li2 O2 Li3 O1 3.29(17) . . . . ? Li2 O2 Li3 O1 96.75(19) 8_565 . . . ? C17 O2 Li3 O1 129.98(14) . . . 8_565 ? Li2 O2 Li3 O1 -96.75(19) . . . 8_565 ? Li2 O2 Li3 O1 -3.29(17) 8_565 . . 8_565 ? C17 O2 Li3 P1 0.000(2) . . . . ? Li2 O2 Li3 P1 133.27(12) . . . . ? Li2 O2 Li3 P1 -133.27(12) 8_565 . . . ? C17 O2 Li3 Li2 133.27(12) . . . 8_565 ? Li2 O2 Li3 Li2 -93.5(2) . . . 8_565 ? C2 O1 Li3 O2 163.99(16) . . . . ? Li2 O1 Li3 O2 -3.33(17) . . . . ? Li1 O1 Li3 O2 -93.3(2) . . . . ? C2 O1 Li3 O1 -91.4(2) . . . 8_565 ? Li2 O1 Li3 O1 101.3(2) . . . 8_565 ? Li1 O1 Li3 O1 11.3(2) . . . 8_565 ? C2 O1 Li3 P1 -5.49(18) . . . . ? Li2 O1 Li3 P1 -172.81(15) . . . . ? Li1 O1 Li3 P1 97.26(17) . . . . ? C2 O1 Li3 Li2 -142.77(17) . . . 8_565 ? Li2 O1 Li3 Li2 49.91(19) . . . 8_565 ? Li1 O1 Li3 Li2 -40.0(2) . . . 8_565 ? C1 P1 Li3 O2 -128.94(6) . . . . ? C1 P1 Li3 O2 128.94(6) 8_565 . . . ? C15 P1 Li3 O2 0.000(2) . . . . ? C1 P1 Li3 O1 2.53(12) . . . . ? C1 P1 Li3 O1 -99.59(11) 8_565 . . . ? C15 P1 Li3 O1 131.47(10) . . . . ? C1 P1 Li3 O1 99.59(11) . . . 8_565 ? C1 P1 Li3 O1 -2.53(12) 8_565 . . 8_565 ? C15 P1 Li3 O1 -131.47(10) . . . 8_565 ? C1 P1 Li3 Li2 107.7(3) . . . 8_565 ? C1 P1 Li3 Li2 5.6(3) 8_565 . . 8_565 ? C15 P1 Li3 Li2 -123.3(3) . . . 8_565 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.083 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.058