# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Guofu Zi' _publ_contact_author_email gzi@bnu.edu.cn loop_ _publ_author_name 'Wenshan Ren' 'Xuebin Deng' 'Guofu Zi' 'De-Cat Fang' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 829579' #TrackingRef 'Compound 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H50 O2 P4 S4 Th' _chemical_formula_sum 'C54 H50 O2 P4 S4 Th' _chemical_formula_weight 1215.10 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 '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 10.8832(12) _cell_length_b 14.6759(17) _cell_length_c 17.335(2) _cell_angle_alpha 69.998(2) _cell_angle_beta 88.651(2) _cell_angle_gamma 75.203(2) _cell_volume 2509.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 1437 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 20.93 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 3.307 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4920 _exptl_absorpt_correction_T_max 0.7778 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12837 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.1099 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.25 _reflns_number_total 8998 _reflns_number_gt 7149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0341P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8998 _refine_ls_number_parameters 588 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.975 _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 0.6673(7) 0.7796(6) 0.5577(5) 0.0181(17) Uani 1 1 d . . . C2 C 0.6013(7) 0.7125(6) 0.6031(5) 0.0215(18) Uani 1 1 d . . . H2 H 0.6415 0.6593 0.6517 0.026 Uiso 1 1 calc R . . C3 C 0.4768(8) 0.7221(7) 0.5785(6) 0.034(2) Uani 1 1 d . . . H3 H 0.4328 0.6748 0.6095 0.041 Uiso 1 1 calc R . . C4 C 0.4164(8) 0.8013(8) 0.5085(6) 0.039(3) Uani 1 1 d . . . H4 H 0.3308 0.8086 0.4921 0.047 Uiso 1 1 calc R . . C5 C 0.4812(8) 0.8692(8) 0.4630(5) 0.043(3) Uani 1 1 d . . . H5 H 0.4397 0.9233 0.4154 0.051 Uiso 1 1 calc R . . C6 C 0.6078(8) 0.8589(7) 0.4865(5) 0.035(2) Uani 1 1 d . . . H6 H 0.6527 0.9051 0.4546 0.042 Uiso 1 1 calc R . . C7 C 0.9129(7) 0.8106(6) 0.5038(5) 0.0186(18) Uani 1 1 d . . . C8 C 0.9304(8) 0.9054(6) 0.4697(5) 0.0251(19) Uani 1 1 d . . . H8 H 0.8901 0.9561 0.4913 0.030 Uiso 1 1 calc R . . C9 C 1.0065(8) 0.9279(6) 0.4039(5) 0.026(2) Uani 1 1 d . . . H9 H 1.0182 0.9936 0.3817 0.031 Uiso 1 1 calc R . . C10 C 1.0654(7) 0.8568(6) 0.3699(5) 0.0219(19) Uani 1 1 d . . . H10 H 1.1165 0.8725 0.3246 0.026 Uiso 1 1 calc R . . C11 C 1.0467(7) 0.7609(6) 0.4051(5) 0.027(2) Uani 1 1 d . . . H11 H 1.0862 0.7102 0.3833 0.033 Uiso 1 1 calc R . . C12 C 0.9727(7) 0.7384(6) 0.4701(5) 0.0229(19) Uani 1 1 d . . . H12 H 0.9619 0.6724 0.4928 0.027 Uiso 1 1 calc R . . C13 C 0.9052(7) 0.6682(5) 0.6688(5) 0.0154(17) Uani 1 1 d . . . C14 C 1.1006(7) 0.4916(6) 0.6558(5) 0.0189(18) Uani 1 1 d . . . C15 C 1.1939(7) 0.5421(6) 0.6312(5) 0.0244(19) Uani 1 1 d . . . H15 H 1.1801 0.6081 0.6324 0.029 Uiso 1 1 calc R . . C16 C 1.3062(7) 0.4983(6) 0.6049(5) 0.028(2) Uani 1 1 d . . . H16 H 1.3691 0.5342 0.5880 0.034 Uiso 1 1 calc R . . C17 C 1.3275(8) 0.4029(7) 0.6032(5) 0.030(2) Uani 1 1 d . . . H17 H 1.4061 0.3726 0.5860 0.036 Uiso 1 1 calc R . . C18 C 1.2378(8) 0.3513(6) 0.6257(5) 0.027(2) Uani 1 1 d . . . H18 H 1.2518 0.2863 0.6222 0.033 Uiso 1 1 calc R . . C19 C 1.1229(8) 0.3953(6) 0.6544(5) 0.026(2) Uani 1 1 d . . . H19 H 1.0612 0.3585 0.6728 0.031 Uiso 1 1 calc R . . C20 C 0.8484(6) 0.4716(5) 0.6974(4) 0.0131(16) Uani 1 1 d U . . C21 C 0.7861(7) 0.4918(6) 0.6206(5) 0.0252(19) Uani 1 1 d . . . H21 H 0.8049 0.5401 0.5724 0.030 Uiso 1 1 calc R . . C22 C 0.6979(8) 0.4410(6) 0.6161(5) 0.028(2) Uani 1 1 d . . . H22 H 0.6542 0.4560 0.5646 0.034 Uiso 1 1 calc R . . C23 C 0.6716(7) 0.3687(6) 0.6850(5) 0.0242(19) Uani 1 1 d . . . H23 H 0.6126 0.3325 0.6808 0.029 Uiso 1 1 calc R . . C24 C 0.7325(8) 0.3497(6) 0.7602(5) 0.029(2) Uani 1 1 d . . . H24 H 0.7128 0.3018 0.8084 0.035 Uiso 1 1 calc R . . C25 C 0.8213(7) 0.3997(6) 0.7659(5) 0.0247(19) Uani 1 1 d . . . H25 H 0.8643 0.3844 0.8176 0.030 Uiso 1 1 calc R . . C26 C 0.8741(7) 0.8698(5) 0.9934(5) 0.0184(17) Uani 1 1 d . . . C27 C 0.9938(8) 0.8760(6) 1.0098(5) 0.026(2) Uani 1 1 d . . . H27 H 1.0478 0.8920 0.9661 0.031 Uiso 1 1 calc R . . C28 C 1.0368(9) 0.8592(7) 1.0890(6) 0.042(3) Uani 1 1 d . . . H28 H 1.1200 0.8642 1.0987 0.050 Uiso 1 1 calc R . . C29 C 0.9629(8) 0.8358(6) 1.1536(6) 0.031(2) Uani 1 1 d . . . H29 H 0.9944 0.8238 1.2078 0.038 Uiso 1 1 calc R . . C30 C 0.8423(9) 0.8297(6) 1.1393(5) 0.030(2) Uani 1 1 d . . . H30 H 0.7891 0.8138 1.1835 0.036 Uiso 1 1 calc R . . C31 C 0.7983(8) 0.8473(6) 1.0587(5) 0.0237(19) Uani 1 1 d . . . H31 H 0.7145 0.8437 1.0488 0.028 Uiso 1 1 calc R . . C32 C 0.6882(7) 1.0006(5) 0.8586(4) 0.0136(16) Uani 1 1 d . . . C33 C 0.6533(7) 1.0596(6) 0.9066(5) 0.0229(19) Uani 1 1 d . . . H33 H 0.6955 1.0390 0.9595 0.027 Uiso 1 1 calc R . . C34 C 0.5576(7) 1.1488(6) 0.8788(5) 0.0243(19) Uani 1 1 d . . . H34 H 0.5348 1.1894 0.9120 0.029 Uiso 1 1 calc R . . C35 C 0.4957(7) 1.1778(6) 0.8018(5) 0.0217(19) Uani 1 1 d . . . H35 H 0.4297 1.2386 0.7822 0.026 Uiso 1 1 calc R . . C36 C 0.5297(8) 1.1189(6) 0.7538(5) 0.028(2) Uani 1 1 d . . . H36 H 0.4875 1.1395 0.7009 0.034 Uiso 1 1 calc R . . C37 C 0.6245(7) 1.0302(6) 0.7817(5) 0.0191(18) Uani 1 1 d . . . H37 H 0.6463 0.9894 0.7486 0.023 Uiso 1 1 calc R . . C38 C 0.7751(7) 0.7804(5) 0.8900(4) 0.0147(17) Uani 1 1 d . . . C39 C 0.6065(7) 0.6676(5) 0.9955(5) 0.0153(17) Uani 1 1 d . . . C40 C 0.6796(7) 0.6527(6) 1.0652(5) 0.0212(18) Uani 1 1 d . . . H40 H 0.7532 0.6774 1.0599 0.025 Uiso 1 1 calc R . . C41 C 0.6464(8) 0.6024(6) 1.1424(5) 0.030(2) Uani 1 1 d . . . H41 H 0.6967 0.5932 1.1899 0.036 Uiso 1 1 calc R . . C42 C 0.5396(8) 0.5649(6) 1.1511(5) 0.026(2) Uani 1 1 d . . . H42 H 0.5156 0.5317 1.2043 0.031 Uiso 1 1 calc R . . C43 C 0.4701(8) 0.5762(6) 1.0828(5) 0.032(2) Uani 1 1 d . . . H43 H 0.3990 0.5485 1.0882 0.038 Uiso 1 1 calc R . . C44 C 0.5022(8) 0.6275(6) 1.0058(5) 0.032(2) Uani 1 1 d . . . H44 H 0.4519 0.6356 0.9587 0.039 Uiso 1 1 calc R . . C45 C 0.4997(7) 0.8268(5) 0.8434(5) 0.0166(17) Uani 1 1 d . . . C46 C 0.4128(7) 0.8710(5) 0.8885(5) 0.0201(18) Uani 1 1 d . . . H46 H 0.4284 0.8522 0.9463 0.024 Uiso 1 1 calc R . . C47 C 0.3028(8) 0.9430(6) 0.8481(5) 0.029(2) Uani 1 1 d . . . H47 H 0.2423 0.9726 0.8789 0.035 Uiso 1 1 calc R . . C48 C 0.2798(8) 0.9724(6) 0.7641(5) 0.030(2) Uani 1 1 d . . . H48 H 0.2035 1.0209 0.7372 0.036 Uiso 1 1 calc R . . C49 C 0.3688(8) 0.9306(6) 0.7196(5) 0.028(2) Uani 1 1 d . . . H49 H 0.3556 0.9527 0.6614 0.034 Uiso 1 1 calc R . . C50 C 0.4777(7) 0.8563(6) 0.7591(5) 0.0215(18) Uani 1 1 d . . . H50 H 0.5370 0.8259 0.7282 0.026 Uiso 1 1 calc R . . C51 C 1.0627(10) 0.6095(8) 0.9936(6) 0.063(3) Uani 1 1 d U . . H51A H 1.0970 0.5363 1.0125 0.094 Uiso 1 1 calc R . . H51B H 0.9712 0.6260 1.0012 0.094 Uiso 1 1 calc R . . H51C H 1.1060 0.6373 1.0256 0.094 Uiso 1 1 calc R . . C52 C 1.2142(8) 0.6256(8) 0.8939(5) 0.039(2) Uani 1 1 d . . . H52A H 1.2366 0.5609 0.8841 0.046 Uiso 1 1 calc R . . H52B H 1.2691 0.6186 0.9415 0.046 Uiso 1 1 calc R . . C53 C 1.2349(8) 0.7068(7) 0.8200(5) 0.033(2) Uani 1 1 d . . . H53A H 1.2246 0.7692 0.8324 0.040 Uiso 1 1 calc R . . H53B H 1.3224 0.6874 0.8030 0.040 Uiso 1 1 calc R . . C54 C 1.1634(8) 0.7941(6) 0.6779(5) 0.030(2) Uani 1 1 d . . . H54A H 1.1512 0.8602 0.6831 0.045 Uiso 1 1 calc R . . H54B H 1.1020 0.7988 0.6354 0.045 Uiso 1 1 calc R . . H54C H 1.2502 0.7715 0.6627 0.045 Uiso 1 1 calc R . . O1 O 1.0823(5) 0.6503(4) 0.9113(3) 0.0234(13) Uani 1 1 d . . . O2 O 1.1440(5) 0.7232(4) 0.7554(3) 0.0224(13) Uani 1 1 d . . . P1 P 0.82534(18) 0.77349(14) 0.59544(12) 0.0148(4) Uani 1 1 d . . . P2 P 0.96060(18) 0.54326(14) 0.70369(12) 0.0139(4) Uani 1 1 d . . . P3 P 0.81541(18) 0.88338(14) 0.89088(12) 0.0136(4) Uani 1 1 d . . . P4 P 0.64889(18) 0.73396(14) 0.89278(12) 0.0139(4) Uani 1 1 d . . . S1 S 0.79685(19) 0.88300(14) 0.64648(12) 0.0193(4) Uani 1 1 d . . . S2 S 1.02146(18) 0.50308(14) 0.82327(11) 0.0170(4) Uani 1 1 d . . . S3 S 0.95562(18) 0.90271(15) 0.81325(13) 0.0211(5) Uani 1 1 d . . . S4 S 0.69453(18) 0.63370(14) 0.83369(12) 0.0183(4) Uani 1 1 d . . . Th1 Th 0.91239(3) 0.71776(2) 0.792569(17) 0.01306(9) 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 0.016(4) 0.025(5) 0.017(4) -0.015(4) 0.003(3) -0.001(3) C2 0.017(4) 0.020(4) 0.028(5) -0.012(4) 0.003(4) 0.000(4) C3 0.019(5) 0.048(6) 0.047(6) -0.030(5) 0.015(4) -0.013(4) C4 0.015(5) 0.075(8) 0.032(6) -0.031(6) -0.001(4) -0.001(5) C5 0.028(5) 0.060(7) 0.019(5) -0.009(5) -0.015(4) 0.017(5) C6 0.026(5) 0.049(6) 0.024(5) -0.009(5) -0.001(4) -0.004(4) C7 0.025(4) 0.019(4) 0.016(4) -0.008(4) 0.002(3) -0.012(4) C8 0.037(5) 0.012(4) 0.026(5) -0.005(4) 0.006(4) -0.010(4) C9 0.041(5) 0.018(4) 0.021(5) -0.001(4) 0.006(4) -0.018(4) C10 0.025(5) 0.027(5) 0.010(4) -0.003(4) 0.004(3) -0.007(4) C11 0.026(5) 0.030(5) 0.028(5) -0.017(4) 0.010(4) -0.002(4) C12 0.029(5) 0.019(4) 0.025(5) -0.010(4) 0.006(4) -0.012(4) C13 0.013(4) 0.014(4) 0.019(4) -0.006(3) 0.007(3) -0.003(3) C14 0.020(4) 0.020(4) 0.013(4) -0.007(4) -0.003(3) 0.002(4) C15 0.026(5) 0.028(5) 0.026(5) -0.013(4) 0.011(4) -0.014(4) C16 0.017(4) 0.037(5) 0.038(5) -0.018(5) 0.021(4) -0.014(4) C17 0.016(4) 0.049(6) 0.015(4) -0.012(4) 0.000(4) 0.006(4) C18 0.027(5) 0.019(5) 0.037(5) -0.016(4) 0.005(4) -0.001(4) C19 0.026(5) 0.018(5) 0.033(5) -0.008(4) 0.002(4) -0.007(4) C20 0.012(4) 0.010(4) 0.020(4) -0.012(3) 0.001(3) 0.002(3) C21 0.028(5) 0.028(5) 0.018(4) -0.006(4) 0.000(4) -0.008(4) C22 0.026(5) 0.033(5) 0.025(5) -0.009(4) -0.004(4) -0.007(4) C23 0.024(5) 0.027(5) 0.032(5) -0.017(4) 0.006(4) -0.015(4) C24 0.028(5) 0.030(5) 0.030(5) -0.009(4) 0.017(4) -0.013(4) C25 0.018(4) 0.025(5) 0.024(5) 0.001(4) -0.001(4) -0.007(4) C26 0.025(4) 0.008(4) 0.024(4) -0.007(3) 0.003(4) -0.005(3) C27 0.030(5) 0.027(5) 0.017(4) 0.005(4) -0.006(4) -0.016(4) C28 0.037(6) 0.046(6) 0.038(6) -0.002(5) -0.017(5) -0.017(5) C29 0.043(6) 0.017(5) 0.030(5) -0.002(4) -0.016(4) -0.007(4) C30 0.049(6) 0.016(4) 0.022(5) -0.010(4) 0.011(4) -0.001(4) C31 0.024(5) 0.023(5) 0.026(5) -0.011(4) -0.004(4) -0.004(4) C32 0.011(4) 0.014(4) 0.018(4) -0.007(3) 0.004(3) -0.006(3) C33 0.022(4) 0.019(4) 0.023(5) -0.006(4) 0.002(4) 0.000(4) C34 0.023(5) 0.027(5) 0.022(5) -0.013(4) 0.008(4) 0.001(4) C35 0.016(4) 0.019(4) 0.023(5) -0.004(4) -0.006(4) 0.003(3) C36 0.037(5) 0.029(5) 0.018(5) -0.005(4) -0.007(4) -0.010(4) C37 0.023(4) 0.016(4) 0.017(4) -0.006(4) 0.004(3) -0.003(3) C38 0.014(4) 0.020(4) 0.009(4) -0.006(3) 0.003(3) 0.000(3) C39 0.016(4) 0.008(4) 0.019(4) -0.003(3) 0.006(3) -0.003(3) C40 0.018(4) 0.022(4) 0.016(4) -0.004(4) 0.006(3) 0.001(4) C41 0.031(5) 0.030(5) 0.019(5) -0.006(4) 0.004(4) 0.004(4) C42 0.028(5) 0.018(4) 0.020(5) -0.001(4) 0.010(4) 0.007(4) C43 0.033(5) 0.037(5) 0.026(5) -0.001(4) 0.013(4) -0.026(4) C44 0.031(5) 0.037(5) 0.027(5) -0.007(4) 0.000(4) -0.011(4) C45 0.015(4) 0.016(4) 0.022(4) -0.007(4) -0.002(3) -0.007(3) C46 0.018(4) 0.019(4) 0.023(5) -0.015(4) -0.009(3) 0.008(3) C47 0.027(5) 0.022(5) 0.038(6) -0.015(4) 0.002(4) 0.000(4) C48 0.024(5) 0.029(5) 0.034(5) -0.007(4) -0.002(4) -0.005(4) C49 0.034(5) 0.031(5) 0.017(4) 0.003(4) -0.002(4) -0.018(4) C50 0.024(4) 0.021(4) 0.018(4) -0.002(4) 0.004(4) -0.009(4) C51 0.057(5) 0.069(5) 0.046(5) -0.014(4) 0.009(4) 0.004(4) C52 0.020(5) 0.065(7) 0.027(5) -0.015(5) -0.001(4) -0.007(5) C53 0.027(5) 0.044(6) 0.029(5) -0.008(5) -0.004(4) -0.013(4) C54 0.026(5) 0.034(5) 0.033(5) -0.011(4) 0.008(4) -0.015(4) O1 0.019(3) 0.035(3) 0.017(3) -0.010(3) 0.006(2) -0.008(3) O2 0.019(3) 0.029(3) 0.020(3) -0.010(3) 0.001(2) -0.004(3) P1 0.0176(10) 0.0138(10) 0.0109(10) -0.0032(8) 0.0005(8) -0.0024(8) P2 0.0143(10) 0.0128(10) 0.0135(10) -0.0038(8) 0.0016(8) -0.0027(8) P3 0.0144(10) 0.0132(10) 0.0145(10) -0.0066(9) 0.0030(8) -0.0036(8) P4 0.0128(10) 0.0142(10) 0.0139(10) -0.0043(9) 0.0021(8) -0.0034(8) S1 0.0249(11) 0.0138(10) 0.0179(10) -0.0059(9) 0.0025(9) -0.0022(9) S2 0.0189(10) 0.0143(10) 0.0138(10) -0.0035(8) -0.0001(8) 0.0004(8) S3 0.0197(11) 0.0212(11) 0.0286(12) -0.0133(10) 0.0110(9) -0.0105(9) S4 0.0192(10) 0.0191(11) 0.0216(11) -0.0113(9) 0.0065(9) -0.0082(9) Th1 0.01282(15) 0.01419(15) 0.01286(15) -0.00577(11) 0.00223(11) -0.00335(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 C2 1.382(11) . ? C1 C6 1.403(11) . ? C1 P1 1.825(8) . ? C2 C3 1.388(11) . ? C2 H2 0.9500 . ? C3 C4 1.392(12) . ? C3 H3 0.9500 . ? C4 C5 1.382(13) . ? C4 H4 0.9500 . ? C5 C6 1.401(12) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.374(10) . ? C7 C12 1.392(10) . ? C7 P1 1.825(8) . ? C8 C9 1.391(11) . ? C8 H8 0.9500 . ? C9 C10 1.380(10) . ? C9 H9 0.9500 . ? C10 C11 1.395(11) . ? C10 H10 0.9500 . ? C11 C12 1.366(11) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 P1 1.668(7) . ? C13 P2 1.669(7) . ? C13 Th1 2.498(7) . ? C14 C19 1.380(10) . ? C14 C15 1.381(11) . ? C14 P2 1.835(8) . ? C15 C16 1.373(10) . ? C15 H15 0.9500 . ? C16 C17 1.371(11) . ? C16 H16 0.9500 . ? C17 C18 1.355(11) . ? C17 H17 0.9500 . ? C18 C19 1.417(10) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.377(10) . ? C20 C21 1.411(10) . ? C20 P2 1.831(7) . ? C21 C22 1.376(11) . ? C21 H21 0.9500 . ? C22 C23 1.380(11) . ? C22 H22 0.9500 . ? C23 C24 1.384(11) . ? C23 H23 0.9500 . ? C24 C25 1.377(11) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.372(10) . ? C26 C31 1.382(11) . ? C26 P3 1.831(8) . ? C27 C28 1.380(11) . ? C27 H27 0.9500 . ? C28 C29 1.362(13) . ? C28 H28 0.9500 . ? C29 C30 1.373(12) . ? C29 H29 0.9500 . ? C30 C31 1.403(11) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.378(10) . ? C32 C37 1.392(10) . ? C32 P3 1.831(7) . ? C33 C34 1.387(10) . ? C33 H33 0.9500 . ? C34 C35 1.387(10) . ? C34 H34 0.9500 . ? C35 C36 1.375(10) . ? C35 H35 0.9500 . ? C36 C37 1.377(10) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 P4 1.675(7) . ? C38 P3 1.682(8) . ? C38 Th1 2.485(7) . ? C39 C40 1.385(10) . ? C39 C44 1.388(11) . ? C39 P4 1.827(7) . ? C40 C41 1.380(10) . ? C40 H40 0.9500 . ? C41 C42 1.393(11) . ? C41 H41 0.9500 . ? C42 C43 1.359(11) . ? C42 H42 0.9500 . ? C43 C44 1.377(11) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C50 1.381(10) . ? C45 C46 1.388(10) . ? C45 P4 1.834(7) . ? C46 C47 1.389(10) . ? C46 H46 0.9500 . ? C47 C48 1.379(11) . ? C47 H47 0.9500 . ? C48 C49 1.376(11) . ? C48 H48 0.9500 . ? C49 C50 1.389(11) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 O1 1.381(11) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 O1 1.439(9) . ? C52 C53 1.480(12) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 O2 1.428(9) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 O2 1.440(9) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? O1 Th1 2.547(5) . ? O2 Th1 2.601(5) . ? P1 S1 2.041(3) . ? P1 Th1 3.330(2) . ? P2 S2 2.028(3) . ? P2 Th1 3.3439(19) . ? P3 S3 2.021(3) . ? P3 Th1 3.3711(19) . ? P4 S4 2.024(3) . ? P4 Th1 3.3163(19) . ? S1 Th1 2.8751(19) . ? S2 Th1 2.9310(19) . ? S3 Th1 3.007(2) . ? S4 Th1 2.9094(19) . ? 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 C2 C1 C6 119.9(7) . . ? C2 C1 P1 120.3(6) . . ? C6 C1 P1 119.5(6) . . ? C1 C2 C3 120.6(8) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C2 C3 C4 119.9(9) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 119.9(8) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.6(8) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 119.1(9) . . ? C5 C6 H6 120.5 . . ? C1 C6 H6 120.5 . . ? C8 C7 C12 118.1(7) . . ? C8 C7 P1 122.8(6) . . ? C12 C7 P1 119.0(6) . . ? C7 C8 C9 120.7(8) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 121.5(7) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C11 117.2(7) . . ? C9 C10 H10 121.4 . . ? C11 C10 H10 121.4 . . ? C12 C11 C10 121.4(8) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C7 121.1(8) . . ? C11 C12 H12 119.4 . . ? C7 C12 H12 119.4 . . ? P1 C13 P2 149.3(5) . . ? P1 C13 Th1 104.3(3) . . ? P2 C13 Th1 105.0(3) . . ? C19 C14 C15 118.6(7) . . ? C19 C14 P2 120.0(6) . . ? C15 C14 P2 120.8(6) . . ? C16 C15 C14 121.1(8) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C17 C16 C15 120.1(8) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C18 C17 C16 120.8(8) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 119.3(8) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C14 C19 C18 120.1(8) . . ? C14 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C25 C20 C21 119.0(7) . . ? C25 C20 P2 121.8(6) . . ? C21 C20 P2 119.2(6) . . ? C22 C21 C20 119.4(8) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 C23 121.2(8) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C24 119.1(7) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C25 C24 C23 120.5(8) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C20 C25 C24 120.8(8) . . ? C20 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C27 C26 C31 117.6(7) . . ? C27 C26 P3 122.9(6) . . ? C31 C26 P3 119.5(6) . . ? C26 C27 C28 120.9(8) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C29 C28 C27 121.6(8) . . ? C29 C28 H28 119.2 . . ? C27 C28 H28 119.2 . . ? C28 C29 C30 119.0(8) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? C29 C30 C31 119.4(8) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C26 C31 C30 121.6(8) . . ? C26 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? C33 C32 C37 119.3(7) . . ? C33 C32 P3 123.1(6) . . ? C37 C32 P3 117.6(5) . . ? C32 C33 C34 120.9(8) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? C35 C34 C33 119.2(7) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C36 C35 C34 120.0(7) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 120.7(7) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C36 C37 C32 119.9(7) . . ? C36 C37 H37 120.1 . . ? C32 C37 H37 120.1 . . ? P4 C38 P3 141.9(4) . . ? P4 C38 Th1 104.0(3) . . ? P3 C38 Th1 106.4(3) . . ? C40 C39 C44 117.9(7) . . ? C40 C39 P4 121.2(6) . . ? C44 C39 P4 120.8(6) . . ? C41 C40 C39 120.6(8) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C40 C41 C42 120.3(8) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C43 C42 C41 119.4(8) . . ? C43 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? C42 C43 C44 120.3(8) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C39 121.4(8) . . ? C43 C44 H44 119.3 . . ? C39 C44 H44 119.3 . . ? C50 C45 C46 120.0(7) . . ? C50 C45 P4 118.8(6) . . ? C46 C45 P4 121.1(6) . . ? C45 C46 C47 119.1(7) . . ? C45 C46 H46 120.5 . . ? C47 C46 H46 120.5 . . ? C48 C47 C46 121.2(8) . . ? C48 C47 H47 119.4 . . ? C46 C47 H47 119.4 . . ? C49 C48 C47 119.1(8) . . ? C49 C48 H48 120.4 . . ? C47 C48 H48 120.4 . . ? C48 C49 C50 120.6(8) . . ? C48 C49 H49 119.7 . . ? C50 C49 H49 119.7 . . ? C45 C50 C49 119.9(8) . . ? C45 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? O1 C51 H51A 109.5 . . ? O1 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O1 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O1 C52 C53 108.7(7) . . ? O1 C52 H52A 109.9 . . ? C53 C52 H52A 109.9 . . ? O1 C52 H52B 109.9 . . ? C53 C52 H52B 109.9 . . ? H52A C52 H52B 108.3 . . ? O2 C53 C52 108.6(7) . . ? O2 C53 H53A 110.0 . . ? C52 C53 H53A 110.0 . . ? O2 C53 H53B 110.0 . . ? C52 C53 H53B 110.0 . . ? H53A C53 H53B 108.4 . . ? O2 C54 H54A 109.5 . . ? O2 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O2 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C51 O1 C52 113.2(7) . . ? C51 O1 Th1 125.7(6) . . ? C52 O1 Th1 118.8(4) . . ? C53 O2 C54 113.3(6) . . ? C53 O2 Th1 118.2(5) . . ? C54 O2 Th1 118.8(4) . . ? C13 P1 C1 118.4(4) . . ? C13 P1 C7 113.6(4) . . ? C1 P1 C7 105.5(3) . . ? C13 P1 S1 105.5(3) . . ? C1 P1 S1 105.2(2) . . ? C7 P1 S1 108.1(3) . . ? C13 P1 Th1 46.6(3) . . ? C1 P1 Th1 124.3(3) . . ? C7 P1 Th1 130.1(2) . . ? S1 P1 Th1 59.06(7) . . ? C13 P2 C20 116.6(3) . . ? C13 P2 C14 116.2(4) . . ? C20 P2 C14 103.8(3) . . ? C13 P2 S2 106.3(3) . . ? C20 P2 S2 108.8(3) . . ? C14 P2 S2 104.5(2) . . ? C13 P2 Th1 46.2(3) . . ? C20 P2 Th1 125.7(2) . . ? C14 P2 Th1 130.5(3) . . ? S2 P2 Th1 60.38(7) . . ? C38 P3 C32 116.1(3) . . ? C38 P3 C26 112.2(3) . . ? C32 P3 C26 104.7(3) . . ? C38 P3 S3 107.0(3) . . ? C32 P3 S3 107.7(2) . . ? C26 P3 S3 108.9(3) . . ? C38 P3 Th1 45.0(2) . . ? C32 P3 Th1 128.7(2) . . ? C26 P3 Th1 126.4(2) . . ? S3 P3 Th1 61.96(7) . . ? C38 P4 C39 115.5(4) . . ? C38 P4 C45 115.3(3) . . ? C39 P4 C45 103.9(3) . . ? C38 P4 S4 106.3(3) . . ? C39 P4 S4 107.2(2) . . ? C45 P4 S4 108.3(3) . . ? C38 P4 Th1 46.6(2) . . ? C39 P4 Th1 135.2(2) . . ? C45 P4 Th1 120.9(3) . . ? S4 P4 Th1 60.41(7) . . ? P1 S1 Th1 83.42(8) . . ? P2 S2 Th1 82.65(8) . . ? P3 S3 Th1 81.67(8) . . ? P4 S4 Th1 82.38(8) . . ? C38 Th1 C13 142.7(2) . . ? C38 Th1 O1 83.7(2) . . ? C13 Th1 O1 129.5(2) . . ? C38 Th1 O2 131.2(2) . . ? C13 Th1 O2 84.4(2) . . ? O1 Th1 O2 62.84(16) . . ? C38 Th1 S1 95.99(17) . . ? C13 Th1 S1 66.45(17) . . ? O1 Th1 S1 146.16(13) . . ? O2 Th1 S1 94.16(12) . . ? C38 Th1 S4 66.20(18) . . ? C13 Th1 S4 83.17(17) . . ? O1 Th1 S4 112.81(13) . . ? O2 Th1 S4 157.80(12) . . ? S1 Th1 S4 97.61(6) . . ? C38 Th1 S2 122.53(17) . . ? C13 Th1 S2 65.65(17) . . ? O1 Th1 S2 72.01(12) . . ? O2 Th1 S2 81.58(12) . . ? S1 Th1 S2 132.10(5) . . ? S4 Th1 S2 76.55(5) . . ? C38 Th1 S3 64.97(18) . . ? C13 Th1 S3 132.00(17) . . ? O1 Th1 S3 75.56(13) . . ? O2 Th1 S3 72.49(12) . . ? S1 Th1 S3 73.82(6) . . ? S4 Th1 S3 128.97(5) . . ? S2 Th1 S3 145.16(5) . . ? C38 Th1 P4 29.35(17) . . ? C13 Th1 P4 115.85(17) . . ? O1 Th1 P4 100.99(12) . . ? O2 Th1 P4 159.75(12) . . ? S1 Th1 P4 94.30(5) . . ? S4 Th1 P4 37.21(5) . . ? S2 Th1 P4 105.91(5) . . ? S3 Th1 P4 92.32(5) . . ? C38 Th1 P1 124.27(16) . . ? C13 Th1 P1 29.04(16) . . ? O1 Th1 P1 151.18(12) . . ? O2 Th1 P1 90.49(12) . . ? S1 Th1 P1 37.52(5) . . ? S4 Th1 P1 87.51(5) . . ? S2 Th1 P1 94.62(5) . . ? S3 Th1 P1 108.20(5) . . ? P4 Th1 P1 107.29(5) . . ? C38 Th1 P2 141.81(18) . . ? C13 Th1 P2 28.82(17) . . ? O1 Th1 P2 105.87(12) . . ? O2 Th1 P2 84.08(12) . . ? S1 Th1 P2 95.17(5) . . ? S4 Th1 P2 76.19(5) . . ? S2 Th1 P2 36.97(5) . . ? S3 Th1 P2 152.97(5) . . ? P4 Th1 P2 113.40(5) . . ? P1 Th1 P2 57.66(5) . . ? C38 Th1 P3 28.60(18) . . ? C13 Th1 P3 150.80(16) . . ? O1 Th1 P3 78.44(12) . . ? O2 Th1 P3 105.85(12) . . ? S1 Th1 P3 85.31(5) . . ? S4 Th1 P3 93.86(5) . . ? S2 Th1 P3 141.92(5) . . ? S3 Th1 P3 36.37(5) . . ? P4 Th1 P3 56.66(5) . . ? P1 Th1 P3 122.08(5) . . ? P2 Th1 P3 170.02(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.144 _refine_diff_density_min -0.955 _refine_diff_density_rms 0.189 # Attachment 'Compund 3.cif' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 829580' #TrackingRef 'Compund 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C87 H90 Li2 O6 P6 S6 Th' _chemical_formula_sum 'C87 H90 Li2 O6 P6 S6 Th' _chemical_formula_weight 1855.69 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 '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' 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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 21.0477(11) _cell_length_b 23.5378(12) _cell_length_c 35.0309(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17354.9(15) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5918 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 22.97 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7536 _exptl_absorpt_coefficient_mu 2.024 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6110 _exptl_absorpt_correction_T_max 0.6876 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 100950 _diffrn_reflns_av_R_equivalents 0.1101 _diffrn_reflns_av_sigmaI/netI 0.0881 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.61 _reflns_number_total 20035 _reflns_number_gt 12897 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0336P)^2^+0.0824P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20035 _refine_ls_number_parameters 980 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0879 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.002 _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 0.7017(2) 0.15516(19) 0.03658(12) 0.0188(10) Uani 1 1 d . . . C2 C 0.5936(2) 0.2295(2) 0.01527(14) 0.0245(11) Uani 1 1 d . . . C3 C 0.5386(2) 0.2417(2) 0.03506(16) 0.0325(13) Uani 1 1 d . . . H3 H 0.5399 0.2458 0.0620 0.039 Uiso 1 1 calc R . . C4 C 0.4809(3) 0.2480(2) 0.01582(19) 0.0444(16) Uani 1 1 d . . . H4 H 0.4435 0.2575 0.0296 0.053 Uiso 1 1 calc R . . C5 C 0.4783(3) 0.2406(2) -0.02292(18) 0.0455(16) Uani 1 1 d . . . H5 H 0.4389 0.2447 -0.0359 0.055 Uiso 1 1 calc R . . C6 C 0.5326(3) 0.2273(2) -0.04319(17) 0.0450(16) Uani 1 1 d . . . H6 H 0.5303 0.2213 -0.0700 0.054 Uiso 1 1 calc R . . C7 C 0.5902(3) 0.2226(2) -0.02441(15) 0.0382(14) Uani 1 1 d . . . H7 H 0.6277 0.2147 -0.0385 0.046 Uiso 1 1 calc R . . C8 C 0.7171(2) 0.27810(19) 0.01752(13) 0.0220(10) Uani 1 1 d . . . C9 C 0.6902(2) 0.3325(2) 0.01595(14) 0.0296(12) Uani 1 1 d . . . H9 H 0.6477 0.3382 0.0242 0.036 Uiso 1 1 calc R . . C10 C 0.7254(3) 0.3781(2) 0.00245(15) 0.0370(13) Uani 1 1 d . . . H10 H 0.7075 0.4152 0.0019 0.044 Uiso 1 1 calc R . . C11 C 0.7869(3) 0.3693(2) -0.01025(16) 0.0395(14) Uani 1 1 d . . . H11 H 0.8111 0.4001 -0.0200 0.047 Uiso 1 1 calc R . . C12 C 0.8130(3) 0.3154(2) -0.00871(14) 0.0334(13) Uani 1 1 d . . . H12 H 0.8551 0.3094 -0.0176 0.040 Uiso 1 1 calc R . . C13 C 0.7786(2) 0.2702(2) 0.00551(12) 0.0237(11) Uani 1 1 d . . . H13 H 0.7975 0.2337 0.0070 0.028 Uiso 1 1 calc R . . C14 C 0.6621(2) 0.0673(2) -0.01939(12) 0.0238(11) Uani 1 1 d . . . C15 C 0.5993(2) 0.0769(2) -0.01061(14) 0.0321(13) Uani 1 1 d . . . H15 H 0.5880 0.1060 0.0069 0.038 Uiso 1 1 calc R . . C16 C 0.5526(3) 0.0438(3) -0.02765(16) 0.0435(16) Uani 1 1 d . . . H16 H 0.5093 0.0492 -0.0208 0.052 Uiso 1 1 calc R . . C17 C 0.5687(3) 0.0032(3) -0.05438(17) 0.0529(19) Uani 1 1 d . . . H17 H 0.5364 -0.0188 -0.0663 0.064 Uiso 1 1 calc R . . C18 C 0.6307(3) -0.0053(2) -0.06375(17) 0.0482(17) Uani 1 1 d . . . H18 H 0.6415 -0.0334 -0.0821 0.058 Uiso 1 1 calc R . . C19 C 0.6780(3) 0.0262(2) -0.04685(14) 0.0344(13) Uani 1 1 d . . . H19 H 0.7212 0.0203 -0.0537 0.041 Uiso 1 1 calc R . . C20 C 0.7836(2) 0.1202(2) -0.02860(12) 0.0244(11) Uani 1 1 d . . . C21 C 0.7679(3) 0.1598(2) -0.05631(14) 0.0344(13) Uani 1 1 d . . . H21 H 0.7267 0.1762 -0.0565 0.041 Uiso 1 1 calc R . . C22 C 0.8121(3) 0.1758(2) -0.08384(15) 0.0426(15) Uani 1 1 d . . . H22 H 0.8013 0.2037 -0.1023 0.051 Uiso 1 1 calc R . . C23 C 0.8706(3) 0.1517(3) -0.08434(17) 0.0576(19) Uani 1 1 d . . . H23 H 0.9007 0.1628 -0.1031 0.069 Uiso 1 1 calc R . . C24 C 0.8863(3) 0.1112(3) -0.05765(18) 0.066(2) Uani 1 1 d . . . H24 H 0.9269 0.0937 -0.0585 0.079 Uiso 1 1 calc R . . C25 C 0.8431(3) 0.0958(3) -0.02954(15) 0.0457(16) Uani 1 1 d . . . H25 H 0.8547 0.0684 -0.0109 0.055 Uiso 1 1 calc R . . C26 C 0.8286(2) 0.09346(18) 0.12841(12) 0.0152(9) Uani 1 1 d . . . C27 C 0.9486(2) 0.1269(2) 0.09182(13) 0.0225(10) Uani 1 1 d . . . C28 C 0.9463(3) 0.1287(2) 0.05237(13) 0.0314(12) Uani 1 1 d . . . H28 H 0.9100 0.1441 0.0400 0.038 Uiso 1 1 calc R . . C29 C 0.9964(3) 0.1084(2) 0.03063(15) 0.0404(15) Uani 1 1 d . . . H29 H 0.9946 0.1109 0.0036 0.048 Uiso 1 1 calc R . . C30 C 1.0484(3) 0.0848(2) 0.04781(16) 0.0411(15) Uani 1 1 d . . . H30 H 1.0823 0.0702 0.0328 0.049 Uiso 1 1 calc R . . C31 C 1.0511(3) 0.0824(3) 0.08689(17) 0.0509(18) Uani 1 1 d . . . H31 H 1.0872 0.0662 0.0990 0.061 Uiso 1 1 calc R . . C32 C 1.0022(2) 0.1033(3) 0.10880(15) 0.0405(15) Uani 1 1 d . . . H32 H 1.0050 0.1016 0.1358 0.049 Uiso 1 1 calc R . . C33 C 0.9133(2) 0.1798(2) 0.16211(13) 0.0213(11) Uani 1 1 d . . . C34 C 0.9552(2) 0.2255(2) 0.15821(14) 0.0278(12) Uani 1 1 d . . . H34 H 0.9668 0.2380 0.1334 0.033 Uiso 1 1 calc R . . C35 C 0.9800(3) 0.2527(2) 0.18991(16) 0.0391(15) Uani 1 1 d . . . H35 H 1.0083 0.2838 0.1869 0.047 Uiso 1 1 calc R . . C36 C 0.9633(3) 0.2344(2) 0.22581(16) 0.0379(14) Uani 1 1 d . . . H36 H 0.9800 0.2531 0.2476 0.046 Uiso 1 1 calc R . . C37 C 0.9221(2) 0.1889(2) 0.23044(14) 0.0321(13) Uani 1 1 d . . . H37 H 0.9107 0.1765 0.2553 0.039 Uiso 1 1 calc R . . C38 C 0.8977(2) 0.1613(2) 0.19851(12) 0.0228(11) Uani 1 1 d . . . H38 H 0.8701 0.1297 0.2017 0.027 Uiso 1 1 calc R . . C39 C 0.8696(2) -0.02629(19) 0.11696(13) 0.0198(10) Uani 1 1 d . . . C40 C 0.8990(2) -0.0115(2) 0.08279(13) 0.0247(11) Uani 1 1 d . . . H40 H 0.8955 0.0262 0.0733 0.030 Uiso 1 1 calc R . . C41 C 0.9335(2) -0.0517(2) 0.06251(14) 0.0307(13) Uani 1 1 d . . . H41 H 0.9545 -0.0410 0.0396 0.037 Uiso 1 1 calc R . . C42 C 0.9375(2) -0.1064(2) 0.07526(15) 0.0314(13) Uani 1 1 d . . . H42 H 0.9606 -0.1339 0.0610 0.038 Uiso 1 1 calc R . . C43 C 0.9078(2) -0.1219(2) 0.10897(15) 0.0316(12) Uani 1 1 d . . . H43 H 0.9106 -0.1600 0.1179 0.038 Uiso 1 1 calc R . . C44 C 0.8742(2) -0.0819(2) 0.12971(14) 0.0282(12) Uani 1 1 d . . . H44 H 0.8541 -0.0926 0.1529 0.034 Uiso 1 1 calc R . . C45 C 0.8487(2) 0.01151(19) 0.19236(12) 0.0204(11) Uani 1 1 d . . . C46 C 0.9126(3) 0.0101(2) 0.20095(15) 0.0334(13) Uani 1 1 d . . . H46 H 0.9430 0.0159 0.1813 0.040 Uiso 1 1 calc R . . C47 C 0.9332(3) 0.0001(2) 0.23840(17) 0.0455(16) Uani 1 1 d . . . H47 H 0.9773 0.0002 0.2442 0.055 Uiso 1 1 calc R . . C48 C 0.8898(3) -0.0097(2) 0.26652(17) 0.0476(17) Uani 1 1 d . . . H48 H 0.9036 -0.0178 0.2918 0.057 Uiso 1 1 calc R . . C49 C 0.8269(3) -0.0081(3) 0.25846(15) 0.0513(17) Uani 1 1 d . . . H49 H 0.7969 -0.0145 0.2783 0.062 Uiso 1 1 calc R . . C50 C 0.8056(3) 0.0029(2) 0.22149(14) 0.0364(14) Uani 1 1 d . . . H50 H 0.7613 0.0044 0.2163 0.044 Uiso 1 1 calc R . . C51 C 0.6293(2) 0.12291(19) 0.15369(12) 0.0187(10) Uani 1 1 d . . . C52 C 0.6434(2) 0.13909(19) 0.23705(13) 0.0233(11) Uani 1 1 d . . . C53 C 0.6958(3) 0.1192(2) 0.25679(15) 0.0358(13) Uani 1 1 d . . . H53 H 0.7370 0.1220 0.2459 0.043 Uiso 1 1 calc R . . C54 C 0.6876(3) 0.0950(3) 0.29254(17) 0.0576(19) Uani 1 1 d . . . H54 H 0.7236 0.0810 0.3059 0.069 Uiso 1 1 calc R . . C55 C 0.6293(4) 0.0908(3) 0.30889(17) 0.060(2) Uani 1 1 d . . . H55 H 0.6248 0.0750 0.3337 0.072 Uiso 1 1 calc R . . C56 C 0.5763(3) 0.1100(3) 0.28917(16) 0.0484(17) Uani 1 1 d . . . H56 H 0.5352 0.1063 0.3001 0.058 Uiso 1 1 calc R . . C57 C 0.5835(3) 0.1342(2) 0.25373(14) 0.0351(13) Uani 1 1 d . . . H57 H 0.5472 0.1477 0.2404 0.042 Uiso 1 1 calc R . . C58 C 0.6011(2) 0.2325(2) 0.19317(13) 0.0234(11) Uani 1 1 d . . . C59 C 0.6201(3) 0.2748(2) 0.21814(14) 0.0315(13) Uani 1 1 d . . . H59 H 0.6574 0.2696 0.2330 0.038 Uiso 1 1 calc R . . C60 C 0.5854(3) 0.3248(2) 0.22177(16) 0.0399(15) Uani 1 1 d . . . H60 H 0.5997 0.3539 0.2385 0.048 Uiso 1 1 calc R . . C61 C 0.5303(3) 0.3324(2) 0.20110(15) 0.0367(14) Uani 1 1 d . . . H61 H 0.5062 0.3662 0.2037 0.044 Uiso 1 1 calc R . . C62 C 0.5106(3) 0.2899(2) 0.17641(14) 0.0335(13) Uani 1 1 d . . . H62 H 0.4727 0.2947 0.1620 0.040 Uiso 1 1 calc R . . C63 C 0.5457(2) 0.2402(2) 0.17244(13) 0.0265(12) Uani 1 1 d . . . H63 H 0.5316 0.2114 0.1554 0.032 Uiso 1 1 calc R . . C64 C 0.5657(2) 0.01196(19) 0.16637(13) 0.0192(10) Uani 1 1 d . . . C65 C 0.6000(2) 0.0051(2) 0.19944(13) 0.0253(12) Uani 1 1 d . . . H65 H 0.6285 0.0338 0.2077 0.030 Uiso 1 1 calc R . . C66 C 0.5926(3) -0.0447(2) 0.22097(14) 0.0323(13) Uani 1 1 d . . . H66 H 0.6157 -0.0492 0.2441 0.039 Uiso 1 1 calc R . . C67 C 0.5521(3) -0.0870(2) 0.20901(15) 0.0363(14) Uani 1 1 d . . . H67 H 0.5472 -0.1206 0.2237 0.044 Uiso 1 1 calc R . . C68 C 0.5188(2) -0.0801(2) 0.17548(16) 0.0345(13) Uani 1 1 d . . . H68 H 0.4914 -0.1095 0.1669 0.041 Uiso 1 1 calc R . . C69 C 0.5250(2) -0.0307(2) 0.15407(15) 0.0310(12) Uani 1 1 d . . . H69 H 0.5014 -0.0261 0.1311 0.037 Uiso 1 1 calc R . . C70 C 0.4929(2) 0.10413(19) 0.13610(13) 0.0201(10) Uani 1 1 d . . . C71 C 0.4517(2) 0.0978(2) 0.16704(15) 0.0318(13) Uani 1 1 d . . . H71 H 0.4649 0.0766 0.1887 0.038 Uiso 1 1 calc R . . C72 C 0.3921(3) 0.1220(2) 0.16633(17) 0.0419(14) Uani 1 1 d . . . H72 H 0.3645 0.1176 0.1876 0.050 Uiso 1 1 calc R . . C73 C 0.3724(3) 0.1524(3) 0.13539(18) 0.0514(18) Uani 1 1 d . . . H73 H 0.3308 0.1682 0.1350 0.062 Uiso 1 1 calc R . . C74 C 0.4120(3) 0.1601(3) 0.10503(17) 0.0450(16) Uani 1 1 d . . . H74 H 0.3984 0.1822 0.0839 0.054 Uiso 1 1 calc R . . C75 C 0.4722(2) 0.1356(2) 0.10483(14) 0.0302(12) Uani 1 1 d . . . H75 H 0.4993 0.1404 0.0834 0.036 Uiso 1 1 calc R . . C76 C 0.3103(4) 0.6878(3) 0.0917(2) 0.087(3) Uani 1 1 d . . . H76A H 0.3526 0.6779 0.0820 0.131 Uiso 1 1 calc R . . H76B H 0.2807 0.6910 0.0703 0.131 Uiso 1 1 calc R . . H76C H 0.2957 0.6580 0.1092 0.131 Uiso 1 1 calc R . . C77 C 0.3519(4) 0.7374(3) 0.1445(2) 0.073(2) Uani 1 1 d . . . H77A H 0.3946 0.7228 0.1379 0.087 Uiso 1 1 calc R . . H77B H 0.3325 0.7115 0.1635 0.087 Uiso 1 1 calc R . . C78 C 0.3571(4) 0.7963(4) 0.1607(2) 0.087(3) Uani 1 1 d . . . H78A H 0.3145 0.8143 0.1612 0.105 Uiso 1 1 calc R . . H78B H 0.3731 0.7943 0.1872 0.105 Uiso 1 1 calc R . . C79 C 0.3738(5) 0.8758(5) 0.1222(3) 0.129(4) Uani 1 1 d . . . H79A H 0.3415 0.8648 0.1035 0.194 Uiso 1 1 calc R . . H79B H 0.4079 0.8968 0.1094 0.194 Uiso 1 1 calc R . . H79C H 0.3545 0.9000 0.1418 0.194 Uiso 1 1 calc R . . C80 C 0.7895(6) 0.2350(6) 0.7908(2) 0.159(6) Uani 1 1 d . . . H80A H 0.8217 0.2478 0.7726 0.239 Uiso 1 1 calc R . . H80B H 0.7764 0.2670 0.8069 0.239 Uiso 1 1 calc R . . H80C H 0.7525 0.2204 0.7769 0.239 Uiso 1 1 calc R . . C81 C 0.8166(6) 0.1373(5) 0.7959(3) 0.124(4) Uani 1 1 d . . . H81A H 0.8474 0.1387 0.7746 0.149 Uiso 1 1 calc R . . H81B H 0.7740 0.1295 0.7851 0.149 Uiso 1 1 calc R . . C82 C 0.8344(5) 0.0907(6) 0.8224(3) 0.134(4) Uani 1 1 d . . . H82A H 0.8127 0.0947 0.8473 0.161 Uiso 1 1 calc R . . H82B H 0.8245 0.0530 0.8114 0.161 Uiso 1 1 calc R . . C83 C 0.9277(6) 0.0496(4) 0.8485(3) 0.158(5) Uani 1 1 d . . . H83A H 0.8976 0.0395 0.8688 0.237 Uiso 1 1 calc R . . H83B H 0.9685 0.0602 0.8599 0.237 Uiso 1 1 calc R . . H83C H 0.9338 0.0170 0.8315 0.237 Uiso 1 1 calc R . . O1 O 0.3133(3) 0.7403(2) 0.11137(15) 0.0896(18) Uani 1 1 d . . . O2 O 0.3980(4) 0.8289(3) 0.1387(2) 0.133(3) Uani 1 1 d . . . O3 O 0.8157(4) 0.1904(3) 0.81466(19) 0.126(2) Uani 1 1 d . . . O4 O 0.9018(3) 0.0992(3) 0.82595(18) 0.109(2) Uani 1 1 d . . . P1 P 0.67074(6) 0.21993(5) 0.03838(3) 0.0192(3) Uani 1 1 d . . . P2 P 0.72458(6) 0.10271(5) 0.00787(3) 0.0179(3) Uani 1 1 d . . . P3 P 0.87916(6) 0.14591(5) 0.12031(3) 0.0169(3) Uani 1 1 d . . . P4 P 0.82361(6) 0.02597(5) 0.14325(3) 0.0171(3) Uani 1 1 d . . . P5 P 0.64833(6) 0.16770(5) 0.18870(3) 0.0189(3) Uani 1 1 d . . . P6 P 0.57460(6) 0.07767(5) 0.13839(3) 0.0178(3) Uani 1 1 d . . . S1 S 0.65872(6) 0.23857(5) 0.09473(3) 0.0236(3) Uani 1 1 d . . . S2 S 0.76350(6) 0.04189(5) 0.04193(3) 0.0208(3) Uani 1 1 d . . . S3 S 0.83062(6) 0.20666(5) 0.09081(3) 0.0214(3) Uani 1 1 d . . . S4 S 0.73028(6) 0.00455(5) 0.14034(3) 0.0198(3) Uani 1 1 d . . . S5 S 0.74029(6) 0.19005(5) 0.18041(3) 0.0227(3) Uani 1 1 d . . . S6 S 0.59893(6) 0.05633(5) 0.08402(3) 0.0208(3) Uani 1 1 d . . . Th1 Th 0.719806(7) 0.123281(7) 0.105341(4) 0.01417(5) Uani 1 1 d . . . O6 O 0.84152(18) 0.41084(14) 0.07338(10) 0.0371(9) Uani 1 1 d . . . O5 O 0.78574(18) 0.32938(14) 0.15342(10) 0.0375(9) Uani 1 1 d . . . C86 C 0.8065(3) 0.3692(2) 0.09310(15) 0.0340(13) Uani 1 1 d . . . H86A H 0.8088 0.3328 0.0791 0.041 Uiso 1 1 calc R . . H86B H 0.7614 0.3808 0.0945 0.041 Uiso 1 1 calc R . . C85 C 0.8324(3) 0.3612(2) 0.13311(15) 0.0372(14) Uani 1 1 d . . . H85A H 0.8732 0.3404 0.1324 0.045 Uiso 1 1 calc R . . H85B H 0.8394 0.3985 0.1455 0.045 Uiso 1 1 calc R . . C87 C 0.9040(3) 0.3929(3) 0.0620(2) 0.0585(19) Uani 1 1 d . . . H87A H 0.9324 0.3937 0.0841 0.088 Uiso 1 1 calc R . . H87B H 0.9202 0.4187 0.0423 0.088 Uiso 1 1 calc R . . H87C H 0.9019 0.3542 0.0518 0.088 Uiso 1 1 calc R . . C84 C 0.7943(4) 0.3338(3) 0.19363(16) 0.067(2) Uani 1 1 d . . . H84A H 0.8370 0.3207 0.2004 0.100 Uiso 1 1 calc R . . H84B H 0.7626 0.3102 0.2067 0.100 Uiso 1 1 calc R . . H84C H 0.7891 0.3735 0.2015 0.100 Uiso 1 1 calc R . . Li2 Li 0.8155(4) 0.4878(3) 0.0767(2) 0.029(2) Uani 1 1 d . . . Li1 Li 0.7543(5) 0.2606(4) 0.1309(3) 0.036(2) 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 0.021(2) 0.017(2) 0.018(2) 0.0024(19) 0.002(2) -0.001(2) C2 0.022(3) 0.019(3) 0.033(3) 0.012(2) -0.008(2) -0.001(2) C3 0.028(3) 0.028(3) 0.042(3) 0.004(2) 0.001(3) 0.000(2) C4 0.020(3) 0.041(4) 0.073(5) -0.005(3) -0.004(3) 0.002(3) C5 0.032(3) 0.038(4) 0.067(4) 0.010(3) -0.024(3) -0.002(3) C6 0.049(4) 0.044(4) 0.042(4) 0.010(3) -0.025(3) -0.001(3) C7 0.029(3) 0.050(4) 0.035(3) 0.012(3) -0.005(3) 0.000(3) C8 0.021(2) 0.023(3) 0.022(2) 0.0058(19) 0.000(2) 0.000(2) C9 0.028(3) 0.026(3) 0.035(3) 0.001(2) 0.005(2) 0.001(2) C10 0.044(3) 0.020(3) 0.046(3) 0.009(2) -0.006(3) 0.000(3) C11 0.037(3) 0.035(3) 0.046(3) 0.019(3) 0.004(3) -0.007(3) C12 0.029(3) 0.036(3) 0.035(3) 0.008(2) 0.007(3) -0.001(3) C13 0.024(3) 0.026(3) 0.021(3) 0.005(2) -0.001(2) 0.008(2) C14 0.030(3) 0.023(3) 0.018(2) 0.003(2) -0.010(2) -0.004(2) C15 0.027(3) 0.038(3) 0.031(3) 0.012(2) -0.007(3) -0.006(3) C16 0.032(3) 0.054(4) 0.045(4) 0.020(3) -0.012(3) -0.014(3) C17 0.056(4) 0.055(4) 0.047(4) 0.010(3) -0.029(4) -0.034(4) C18 0.065(5) 0.032(4) 0.048(4) -0.005(3) -0.020(4) -0.011(3) C19 0.039(3) 0.029(3) 0.036(3) -0.005(2) -0.010(3) -0.006(3) C20 0.027(3) 0.030(3) 0.016(2) -0.001(2) 0.002(2) -0.005(3) C21 0.039(3) 0.036(3) 0.028(3) 0.006(2) 0.005(3) 0.002(3) C22 0.066(5) 0.039(4) 0.023(3) 0.006(3) 0.006(3) -0.011(3) C23 0.042(4) 0.099(6) 0.032(4) 0.010(4) 0.012(3) -0.020(4) C24 0.032(4) 0.120(7) 0.046(4) 0.016(4) 0.008(3) 0.005(4) C25 0.030(3) 0.077(5) 0.031(3) 0.015(3) 0.002(3) 0.001(3) C26 0.014(2) 0.017(2) 0.014(2) -0.0046(18) -0.0002(19) 0.0004(19) C27 0.020(2) 0.022(3) 0.025(3) -0.002(2) 0.001(2) -0.006(2) C28 0.034(3) 0.036(3) 0.024(3) -0.002(2) 0.005(2) 0.005(3) C29 0.055(4) 0.043(4) 0.023(3) -0.001(2) 0.016(3) 0.008(3) C30 0.029(3) 0.056(4) 0.039(3) -0.007(3) 0.015(3) 0.005(3) C31 0.024(3) 0.091(5) 0.039(4) -0.013(3) -0.002(3) 0.023(3) C32 0.024(3) 0.077(4) 0.021(3) -0.004(3) -0.001(2) 0.015(3) C33 0.015(2) 0.024(3) 0.025(3) -0.005(2) -0.001(2) -0.002(2) C34 0.030(3) 0.027(3) 0.027(3) 0.002(2) -0.002(2) -0.001(2) C35 0.042(4) 0.024(3) 0.051(4) -0.007(3) -0.015(3) -0.016(3) C36 0.045(4) 0.034(3) 0.035(3) -0.013(3) -0.016(3) 0.004(3) C37 0.031(3) 0.045(4) 0.020(3) -0.009(2) -0.002(2) 0.003(3) C38 0.024(3) 0.024(3) 0.020(3) -0.001(2) 0.000(2) -0.003(2) C39 0.018(2) 0.017(2) 0.025(3) -0.0035(19) -0.005(2) 0.003(2) C40 0.028(3) 0.016(3) 0.030(3) -0.003(2) -0.003(2) 0.000(2) C41 0.030(3) 0.027(3) 0.035(3) -0.009(2) 0.010(2) -0.004(2) C42 0.028(3) 0.026(3) 0.040(3) -0.013(2) -0.005(3) 0.006(2) C43 0.034(3) 0.016(3) 0.045(3) -0.005(2) -0.012(3) 0.002(2) C44 0.033(3) 0.020(3) 0.031(3) 0.001(2) -0.003(2) 0.000(2) C45 0.026(3) 0.017(2) 0.018(2) 0.0009(19) -0.006(2) 0.003(2) C46 0.030(3) 0.040(3) 0.030(3) 0.006(2) -0.008(3) 0.002(3) C47 0.048(4) 0.043(4) 0.046(4) 0.002(3) -0.028(3) 0.005(3) C48 0.069(5) 0.043(4) 0.031(3) 0.004(3) -0.022(3) -0.003(3) C49 0.061(5) 0.072(5) 0.020(3) 0.004(3) 0.001(3) 0.003(4) C50 0.034(3) 0.052(4) 0.023(3) -0.001(3) -0.004(3) -0.001(3) C51 0.017(2) 0.021(2) 0.019(2) 0.005(2) 0.0044(19) -0.002(2) C52 0.032(3) 0.019(3) 0.018(2) -0.0039(19) 0.007(2) -0.001(2) C53 0.035(3) 0.042(3) 0.031(3) 0.007(3) -0.001(3) 0.007(3) C54 0.065(5) 0.072(5) 0.036(4) 0.026(3) -0.003(4) 0.012(4) C55 0.091(6) 0.068(5) 0.022(3) 0.015(3) 0.017(4) 0.002(4) C56 0.058(4) 0.053(4) 0.034(3) 0.009(3) 0.024(3) 0.004(3) C57 0.043(3) 0.036(3) 0.026(3) 0.004(2) 0.008(3) 0.008(3) C58 0.026(3) 0.018(3) 0.026(3) 0.002(2) 0.006(2) -0.001(2) C59 0.030(3) 0.028(3) 0.037(3) -0.009(2) 0.002(3) -0.002(3) C60 0.052(4) 0.019(3) 0.049(4) -0.012(3) 0.007(3) -0.003(3) C61 0.049(4) 0.024(3) 0.037(3) 0.006(2) 0.022(3) 0.018(3) C62 0.032(3) 0.038(3) 0.030(3) 0.011(2) 0.004(3) 0.012(3) C63 0.029(3) 0.024(3) 0.026(3) 0.005(2) 0.000(2) 0.000(2) C64 0.018(2) 0.021(3) 0.019(2) 0.0031(19) 0.007(2) 0.002(2) C65 0.026(3) 0.024(3) 0.026(3) -0.003(2) 0.009(2) 0.003(2) C66 0.042(3) 0.030(3) 0.025(3) 0.008(2) 0.010(3) 0.012(3) C67 0.043(4) 0.023(3) 0.042(3) 0.017(2) 0.014(3) 0.006(3) C68 0.028(3) 0.020(3) 0.055(4) 0.010(3) -0.004(3) -0.003(2) C69 0.026(3) 0.031(3) 0.036(3) 0.002(2) -0.006(2) 0.000(2) C70 0.016(2) 0.015(2) 0.030(3) 0.000(2) 0.001(2) -0.0034(19) C71 0.025(3) 0.034(3) 0.036(3) 0.003(2) 0.004(3) 0.004(2) C72 0.025(3) 0.050(4) 0.050(4) -0.007(3) 0.010(3) 0.002(3) C73 0.027(3) 0.068(5) 0.060(4) -0.020(4) -0.011(3) 0.022(3) C74 0.042(4) 0.053(4) 0.040(3) -0.003(3) -0.015(3) 0.024(3) C75 0.026(3) 0.034(3) 0.031(3) 0.000(2) -0.002(2) 0.008(2) C76 0.086(6) 0.087(7) 0.089(6) -0.017(5) 0.002(5) 0.001(5) C77 0.070(5) 0.076(6) 0.072(5) 0.007(4) -0.030(4) -0.003(4) C78 0.090(7) 0.102(7) 0.071(6) -0.010(5) 0.010(5) -0.026(6) C79 0.135(10) 0.157(11) 0.096(7) 0.059(7) -0.054(7) -0.052(8) C80 0.196(14) 0.235(15) 0.047(6) 0.029(8) 0.019(7) 0.019(11) C81 0.159(11) 0.133(11) 0.082(7) -0.037(7) 0.016(7) 0.002(9) C82 0.086(8) 0.203(14) 0.114(9) -0.065(9) -0.011(8) -0.009(9) C83 0.236(16) 0.060(7) 0.178(11) 0.004(7) 0.012(10) 0.028(8) O1 0.096(4) 0.090(4) 0.082(4) -0.016(3) -0.030(3) 0.030(4) O2 0.138(6) 0.087(5) 0.173(7) 0.035(5) 0.064(6) -0.017(5) O3 0.155(7) 0.125(6) 0.099(5) -0.037(5) -0.006(5) -0.018(5) O4 0.095(5) 0.125(6) 0.108(5) -0.008(4) 0.025(4) -0.017(4) P1 0.0190(6) 0.0176(6) 0.0211(6) 0.0033(5) 0.0008(5) 0.0020(5) P2 0.0198(6) 0.0180(6) 0.0160(6) 0.0004(5) -0.0015(5) -0.0007(5) P3 0.0166(6) 0.0192(6) 0.0151(6) -0.0001(5) -0.0016(5) -0.0018(5) P4 0.0169(6) 0.0176(6) 0.0169(6) 0.0008(5) -0.0010(5) 0.0017(5) P5 0.0199(6) 0.0180(6) 0.0188(6) -0.0009(5) 0.0027(5) -0.0001(5) P6 0.0170(6) 0.0171(6) 0.0191(6) 0.0020(5) 0.0012(5) -0.0007(5) S1 0.0264(7) 0.0211(7) 0.0233(7) 0.0002(5) 0.0027(5) 0.0053(5) S2 0.0246(6) 0.0183(6) 0.0194(6) 0.0000(5) -0.0021(5) 0.0046(5) S3 0.0195(6) 0.0203(6) 0.0242(6) 0.0052(5) -0.0006(5) -0.0020(5) S4 0.0189(6) 0.0191(6) 0.0214(6) 0.0029(5) -0.0013(5) -0.0018(5) S5 0.0198(6) 0.0246(7) 0.0236(7) -0.0038(5) 0.0010(5) -0.0035(5) S6 0.0202(6) 0.0238(7) 0.0183(6) -0.0021(5) 0.0003(5) -0.0028(5) Th1 0.01426(8) 0.01337(8) 0.01489(8) 0.00017(7) 0.00021(7) -0.00016(7) O6 0.040(2) 0.022(2) 0.049(2) -0.0011(17) 0.016(2) -0.0021(18) O5 0.049(3) 0.026(2) 0.037(2) -0.0047(16) -0.0044(19) -0.0096(19) C86 0.038(3) 0.019(3) 0.045(3) 0.000(2) 0.002(3) -0.010(3) C85 0.038(3) 0.020(3) 0.053(4) 0.000(2) -0.007(3) -0.001(3) C87 0.035(4) 0.058(5) 0.082(5) -0.012(4) 0.019(4) 0.004(3) C84 0.107(6) 0.060(5) 0.034(4) -0.012(3) 0.004(4) -0.039(4) Li2 0.046(6) 0.019(4) 0.021(4) -0.002(3) 0.003(4) 0.004(4) Li1 0.049(6) 0.020(5) 0.038(5) -0.008(4) 0.003(5) -0.008(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 P1 1.660(5) . ? C1 P2 1.663(5) . ? C1 Th1 2.552(4) . ? C2 C3 1.381(7) . ? C2 C7 1.401(7) . ? C2 P1 1.827(5) . ? C3 C4 1.396(7) . ? C3 H3 0.9500 . ? C4 C5 1.370(8) . ? C4 H4 0.9500 . ? C5 C6 1.381(8) . ? C5 H5 0.9500 . ? C6 C7 1.384(7) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.375(6) . ? C8 C9 1.401(6) . ? C8 P1 1.833(5) . ? C9 C10 1.387(7) . ? C9 H9 0.9500 . ? C10 C11 1.385(7) . ? C10 H10 0.9500 . ? C11 C12 1.383(7) . ? C11 H11 0.9500 . ? C12 C13 1.378(6) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.376(7) . ? C14 C19 1.403(7) . ? C14 P2 1.826(5) . ? C15 C16 1.389(7) . ? C15 H15 0.9500 . ? C16 C17 1.380(8) . ? C16 H16 0.9500 . ? C17 C18 1.362(9) . ? C17 H17 0.9500 . ? C18 C19 1.376(7) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.379(7) . ? C20 C21 1.386(7) . ? C20 P2 1.828(5) . ? C21 C22 1.392(7) . ? C21 H21 0.9500 . ? C22 C23 1.354(8) . ? C22 H22 0.9500 . ? C23 C24 1.375(9) . ? C23 H23 0.9500 . ? C24 C25 1.388(8) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 P3 1.655(4) . ? C26 P4 1.675(4) . ? C26 Th1 2.527(4) . ? C27 C28 1.383(6) . ? C27 C32 1.390(7) . ? C27 P3 1.826(5) . ? C28 C29 1.386(7) . ? C28 H28 0.9500 . ? C29 C30 1.367(7) . ? C29 H29 0.9500 . ? C30 C31 1.371(7) . ? C30 H30 0.9500 . ? C31 C32 1.375(7) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.387(6) . ? C33 C34 1.396(6) . ? C33 P3 1.816(5) . ? C34 C35 1.385(6) . ? C34 H34 0.9500 . ? C35 C36 1.375(7) . ? C35 H35 0.9500 . ? C36 C37 1.388(7) . ? C36 H36 0.9500 . ? C37 C38 1.392(6) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.386(6) . ? C39 C40 1.392(6) . ? C39 P4 1.816(5) . ? C40 C41 1.387(6) . ? C40 H40 0.9500 . ? C41 C42 1.367(7) . ? C41 H41 0.9500 . ? C42 C43 1.384(7) . ? C42 H42 0.9500 . ? C43 C44 1.384(7) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.379(7) . ? C45 C50 1.380(7) . ? C45 P4 1.832(4) . ? C46 C47 1.402(7) . ? C46 H46 0.9500 . ? C47 C48 1.364(8) . ? C47 H47 0.9500 . ? C48 C49 1.353(8) . ? C48 H48 0.9500 . ? C49 C50 1.395(7) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 P6 1.657(5) . ? C51 P5 1.666(5) . ? C51 Th1 2.549(4) . ? C52 C53 1.384(7) . ? C52 C57 1.395(7) . ? C52 P5 1.826(5) . ? C53 C54 1.386(7) . ? C53 H53 0.9500 . ? C54 C55 1.358(9) . ? C54 H54 0.9500 . ? C55 C56 1.386(9) . ? C55 H55 0.9500 . ? C56 C57 1.374(7) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 C59 1.385(6) . ? C58 C63 1.386(6) . ? C58 P5 1.827(5) . ? C59 C60 1.392(7) . ? C59 H59 0.9500 . ? C60 C61 1.379(7) . ? C60 H60 0.9500 . ? C61 C62 1.386(7) . ? C61 H61 0.9500 . ? C62 C63 1.390(6) . ? C62 H62 0.9500 . ? C63 H63 0.9500 . ? C64 C65 1.374(6) . ? C64 C69 1.388(6) . ? C64 P6 1.841(5) . ? C65 C66 1.401(6) . ? C65 H65 0.9500 . ? C66 C67 1.376(7) . ? C66 H66 0.9500 . ? C67 C68 1.377(7) . ? C67 H67 0.9500 . ? C68 C69 1.391(6) . ? C68 H68 0.9500 . ? C69 H69 0.9500 . ? C70 C75 1.392(6) . ? C70 C71 1.395(6) . ? C70 P6 1.832(5) . ? C71 C72 1.380(7) . ? C71 H71 0.9500 . ? C72 C73 1.362(8) . ? C72 H72 0.9500 . ? C73 C74 1.364(8) . ? C73 H73 0.9500 . ? C74 C75 1.393(7) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 O1 1.417(8) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 O1 1.418(7) . ? C77 C78 1.502(10) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 O2 1.387(9) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 O2 1.347(10) . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 O3 1.451(11) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 O3 1.411(10) . ? C81 C82 1.484(14) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 O4 1.438(11) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 O4 1.512(10) . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? P1 S1 2.0378(17) . ? P1 Th1 3.4270(12) . ? P2 S2 2.0357(16) . ? P3 S3 2.0387(17) . ? P3 Th1 3.4362(12) . ? P4 S4 2.0306(17) . ? P4 Th1 3.4327(12) . ? P5 S5 2.0268(17) . ? P5 Th1 3.4472(12) . ? P6 S6 2.0352(17) . ? P6 Th1 3.4399(12) . ? S1 Li1 2.433(10) . ? S1 Th1 3.0257(12) . ? S2 Li2 2.423(9) 8_755 ? S2 Th1 3.0741(12) . ? S3 Li1 2.482(9) . ? S3 Th1 3.0904(12) . ? S4 Li2 2.460(8) 8_755 ? S4 Th1 3.0597(11) . ? S5 Li1 2.419(9) . ? S5 Th1 3.0937(12) . ? S6 Li2 2.430(9) 8_755 ? S6 Th1 3.0845(12) . ? Th1 Li2 3.424(8) 8_755 ? Th1 Li1 3.431(8) . ? O6 C86 1.407(6) . ? O6 C87 1.438(6) . ? O6 Li2 1.896(9) . ? O5 C84 1.424(6) . ? O5 C85 1.426(6) . ? O5 Li1 1.919(9) . ? C86 C85 1.515(7) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? Li2 S2 2.423(9) 8_765 ? Li2 S6 2.430(9) 8_765 ? Li2 S4 2.460(8) 8_765 ? Li2 Th1 3.424(8) 8_765 ? 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 P1 C1 P2 144.9(3) . . ? P1 C1 Th1 107.0(2) . . ? P2 C1 Th1 108.0(2) . . ? C3 C2 C7 118.6(5) . . ? C3 C2 P1 123.3(4) . . ? C7 C2 P1 118.1(4) . . ? C2 C3 C4 120.6(5) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 120.0(6) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.3(5) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C7 119.9(6) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 120.5(5) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? C13 C8 C9 119.4(4) . . ? C13 C8 P1 121.5(4) . . ? C9 C8 P1 118.9(4) . . ? C10 C9 C8 120.4(5) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 119.5(5) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C12 C11 C10 119.7(5) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C13 C12 C11 120.9(5) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C8 C13 C12 120.1(5) . . ? C8 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C19 119.7(5) . . ? C15 C14 P2 119.9(4) . . ? C19 C14 P2 120.1(4) . . ? C14 C15 C16 119.4(5) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C17 C16 C15 120.5(6) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 120.0(6) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 120.7(6) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C18 C19 C14 119.6(6) . . ? C18 C19 H19 120.2 . . ? C14 C19 H19 120.2 . . ? C25 C20 C21 118.7(5) . . ? C25 C20 P2 122.7(4) . . ? C21 C20 P2 118.6(4) . . ? C20 C21 C22 120.5(5) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 120.2(6) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 119.9(6) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C25 120.5(6) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C20 C25 C24 120.2(5) . . ? C20 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? P3 C26 P4 143.2(3) . . ? P3 C26 Th1 108.7(2) . . ? P4 C26 Th1 107.8(2) . . ? C28 C27 C32 117.9(5) . . ? C28 C27 P3 120.7(4) . . ? C32 C27 P3 120.9(4) . . ? C27 C28 C29 120.8(5) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C30 C29 C28 120.5(5) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 119.2(5) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C30 C31 C32 120.8(5) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? C31 C32 C27 120.7(5) . . ? C31 C32 H32 119.6 . . ? C27 C32 H32 119.6 . . ? C38 C33 C34 118.8(4) . . ? C38 C33 P3 120.6(4) . . ? C34 C33 P3 120.6(4) . . ? C35 C34 C33 121.1(5) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C36 C35 C34 119.4(5) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 C37 120.6(5) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C36 C37 C38 119.8(5) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C33 C38 C37 120.3(5) . . ? C33 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C44 C39 C40 118.8(4) . . ? C44 C39 P4 120.9(4) . . ? C40 C39 P4 120.3(3) . . ? C41 C40 C39 120.2(4) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C42 C41 C40 120.5(5) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C43 120.0(5) . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 119.9(5) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C39 120.6(5) . . ? C43 C44 H44 119.7 . . ? C39 C44 H44 119.7 . . ? C46 C45 C50 118.4(4) . . ? C46 C45 P4 119.4(4) . . ? C50 C45 P4 122.1(4) . . ? C45 C46 C47 120.7(5) . . ? C45 C46 H46 119.7 . . ? C47 C46 H46 119.7 . . ? C48 C47 C46 119.8(6) . . ? C48 C47 H47 120.1 . . ? C46 C47 H47 120.1 . . ? C49 C48 C47 120.0(5) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C48 C49 C50 120.9(6) . . ? C48 C49 H49 119.5 . . ? C50 C49 H49 119.5 . . ? C45 C50 C49 120.1(5) . . ? C45 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? P6 C51 P5 144.2(3) . . ? P6 C51 Th1 107.8(2) . . ? P5 C51 Th1 107.9(2) . . ? C53 C52 C57 118.9(5) . . ? C53 C52 P5 122.9(4) . . ? C57 C52 P5 118.1(4) . . ? C52 C53 C54 119.5(5) . . ? C52 C53 H53 120.3 . . ? C54 C53 H53 120.3 . . ? C55 C54 C53 121.5(6) . . ? C55 C54 H54 119.3 . . ? C53 C54 H54 119.3 . . ? C54 C55 C56 119.5(6) . . ? C54 C55 H55 120.2 . . ? C56 C55 H55 120.2 . . ? C57 C56 C55 119.8(6) . . ? C57 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? C56 C57 C52 120.8(6) . . ? C56 C57 H57 119.6 . . ? C52 C57 H57 119.6 . . ? C59 C58 C63 118.7(5) . . ? C59 C58 P5 119.8(4) . . ? C63 C58 P5 121.5(4) . . ? C58 C59 C60 120.9(5) . . ? C58 C59 H59 119.5 . . ? C60 C59 H59 119.5 . . ? C61 C60 C59 120.2(5) . . ? C61 C60 H60 119.9 . . ? C59 C60 H60 119.9 . . ? C60 C61 C62 119.2(5) . . ? C60 C61 H61 120.4 . . ? C62 C61 H61 120.4 . . ? C61 C62 C63 120.7(5) . . ? C61 C62 H62 119.7 . . ? C63 C62 H62 119.7 . . ? C58 C63 C62 120.3(5) . . ? C58 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C65 C64 C69 120.0(4) . . ? C65 C64 P6 119.7(4) . . ? C69 C64 P6 120.3(4) . . ? C64 C65 C66 119.6(5) . . ? C64 C65 H65 120.2 . . ? C66 C65 H65 120.2 . . ? C67 C66 C65 120.7(5) . . ? C67 C66 H66 119.7 . . ? C65 C66 H66 119.7 . . ? C66 C67 C68 119.3(5) . . ? C66 C67 H67 120.3 . . ? C68 C67 H67 120.3 . . ? C67 C68 C69 120.7(5) . . ? C67 C68 H68 119.6 . . ? C69 C68 H68 119.6 . . ? C64 C69 C68 119.6(5) . . ? C64 C69 H69 120.2 . . ? C68 C69 H69 120.2 . . ? C75 C70 C71 118.4(4) . . ? C75 C70 P6 120.6(4) . . ? C71 C70 P6 120.8(4) . . ? C72 C71 C70 120.4(5) . . ? C72 C71 H71 119.8 . . ? C70 C71 H71 119.8 . . ? C73 C72 C71 120.6(5) . . ? C73 C72 H72 119.7 . . ? C71 C72 H72 119.7 . . ? C72 C73 C74 120.2(5) . . ? C72 C73 H73 119.9 . . ? C74 C73 H73 119.9 . . ? C73 C74 C75 120.4(5) . . ? C73 C74 H74 119.8 . . ? C75 C74 H74 119.8 . . ? C70 C75 C74 120.0(5) . . ? C70 C75 H75 120.0 . . ? C74 C75 H75 120.0 . . ? O1 C76 H76A 109.5 . . ? O1 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? O1 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? O1 C77 C78 107.9(6) . . ? O1 C77 H77A 110.1 . . ? C78 C77 H77A 110.1 . . ? O1 C77 H77B 110.1 . . ? C78 C77 H77B 110.1 . . ? H77A C77 H77B 108.4 . . ? O2 C78 C77 110.2(7) . . ? O2 C78 H78A 109.6 . . ? C77 C78 H78A 109.6 . . ? O2 C78 H78B 109.6 . . ? C77 C78 H78B 109.6 . . ? H78A C78 H78B 108.1 . . ? O2 C79 H79A 109.5 . . ? O2 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? O2 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? O3 C80 H80A 109.5 . . ? O3 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? O3 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? O3 C81 C82 111.4(9) . . ? O3 C81 H81A 109.3 . . ? C82 C81 H81A 109.3 . . ? O3 C81 H81B 109.3 . . ? C82 C81 H81B 109.3 . . ? H81A C81 H81B 108.0 . . ? O4 C82 C81 101.5(11) . . ? O4 C82 H82A 111.5 . . ? C81 C82 H82A 111.5 . . ? O4 C82 H82B 111.5 . . ? C81 C82 H82B 111.5 . . ? H82A C82 H82B 109.3 . . ? O4 C83 H83A 109.5 . . ? O4 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? O4 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C76 O1 C77 112.5(6) . . ? C79 O2 C78 117.2(8) . . ? C81 O3 C80 112.2(9) . . ? C82 O4 C83 107.1(9) . . ? C1 P1 C2 116.4(2) . . ? C1 P1 C8 117.5(2) . . ? C2 P1 C8 101.8(2) . . ? C1 P1 S1 106.46(16) . . ? C2 P1 S1 107.01(17) . . ? C8 P1 S1 106.95(16) . . ? C1 P1 Th1 45.39(15) . . ? C2 P1 Th1 130.73(15) . . ? C8 P1 Th1 127.47(15) . . ? S1 P1 Th1 61.14(4) . . ? C1 P2 C14 116.6(2) . . ? C1 P2 C20 116.9(2) . . ? C14 P2 C20 103.1(2) . . ? C1 P2 S2 106.50(16) . . ? C14 P2 S2 105.94(16) . . ? C20 P2 S2 107.11(17) . . ? C26 P3 C33 116.4(2) . . ? C26 P3 C27 115.2(2) . . ? C33 P3 C27 103.4(2) . . ? C26 P3 S3 106.73(16) . . ? C33 P3 S3 107.37(16) . . ? C27 P3 S3 107.24(16) . . ? C26 P3 Th1 44.15(15) . . ? C33 P3 Th1 125.24(15) . . ? C27 P3 Th1 131.30(15) . . ? S3 P3 Th1 62.76(4) . . ? C26 P4 C39 116.8(2) . . ? C26 P4 C45 116.7(2) . . ? C39 P4 C45 101.3(2) . . ? C26 P4 S4 106.28(16) . . ? C39 P4 S4 108.81(16) . . ? C45 P4 S4 106.27(17) . . ? C26 P4 Th1 44.50(15) . . ? C39 P4 Th1 126.53(15) . . ? C45 P4 Th1 132.14(15) . . ? S4 P4 Th1 62.00(4) . . ? C51 P5 C52 115.8(2) . . ? C51 P5 C58 117.4(2) . . ? C52 P5 C58 101.4(2) . . ? C51 P5 S5 106.75(16) . . ? C52 P5 S5 106.45(17) . . ? C58 P5 S5 108.38(16) . . ? C51 P5 Th1 44.72(15) . . ? C52 P5 Th1 134.34(16) . . ? C58 P5 Th1 124.28(15) . . ? S5 P5 Th1 62.65(4) . . ? C51 P6 C70 116.6(2) . . ? C51 P6 C64 116.0(2) . . ? C70 P6 C64 102.3(2) . . ? C51 P6 S6 106.64(16) . . ? C70 P6 S6 106.22(16) . . ? C64 P6 S6 108.46(15) . . ? C51 P6 Th1 44.85(15) . . ? C70 P6 Th1 135.54(15) . . ? C64 P6 Th1 122.13(15) . . ? S6 P6 Th1 62.52(4) . . ? P1 S1 Li1 116.6(2) . . ? P1 S1 Th1 82.72(5) . . ? Li1 S1 Th1 77.0(2) . . ? P2 S2 Li2 112.8(2) . 8_755 ? P2 S2 Th1 82.23(5) . . ? Li2 S2 Th1 76.03(19) 8_755 . ? P3 S3 Li1 113.3(2) . . ? P3 S3 Th1 81.33(5) . . ? Li1 S3 Th1 75.1(2) . . ? P4 S4 Li2 117.7(2) . 8_755 ? P4 S4 Th1 82.13(5) . . ? Li2 S4 Th1 75.82(19) 8_755 . ? P5 S5 Li1 113.4(2) . . ? P5 S5 Th1 81.76(5) . . ? Li1 S5 Th1 75.9(2) . . ? P6 S6 Li2 116.65(19) . 8_755 ? P6 S6 Th1 81.65(5) . . ? Li2 S6 Th1 75.7(2) 8_755 . ? C26 Th1 C51 117.62(13) . . ? C26 Th1 C1 121.24(14) . . ? C51 Th1 C1 121.12(14) . . ? C26 Th1 S1 132.32(10) . . ? C51 Th1 S1 76.53(10) . . ? C1 Th1 S1 63.70(10) . . ? C26 Th1 S4 63.45(10) . . ? C51 Th1 S4 77.55(10) . . ? C1 Th1 S4 131.12(10) . . ? S1 Th1 S4 154.03(3) . . ? C26 Th1 S2 77.70(9) . . ? C51 Th1 S2 134.56(10) . . ? C1 Th1 S2 62.98(10) . . ? S1 Th1 S2 126.67(3) . . ? S4 Th1 S2 72.47(3) . . ? C26 Th1 S6 133.06(10) . . ? C51 Th1 S6 62.79(10) . . ? C1 Th1 S6 78.38(10) . . ? S1 Th1 S6 94.47(3) . . ? S4 Th1 S6 71.93(3) . . ? S2 Th1 S6 75.72(3) . . ? C26 Th1 S3 62.96(10) . . ? C51 Th1 S3 132.50(10) . . ? C1 Th1 S3 76.72(10) . . ? S1 Th1 S3 74.39(3) . . ? S4 Th1 S3 126.28(3) . . ? S2 Th1 S3 92.92(3) . . ? S6 Th1 S3 155.10(3) . . ? C26 Th1 S5 75.11(9) . . ? C51 Th1 S5 62.68(10) . . ? C1 Th1 S5 132.37(10) . . ? S1 Th1 S5 73.03(3) . . ? S4 Th1 S5 96.51(3) . . ? S2 Th1 S5 152.76(3) . . ? S6 Th1 S5 125.47(3) . . ? S3 Th1 S5 73.27(3) . . ? C26 Th1 Li2 91.82(18) . 8_755 ? C51 Th1 Li2 91.66(18) . 8_755 ? C1 Th1 Li2 87.99(16) . 8_755 ? S1 Th1 Li2 134.98(15) . 8_755 ? S4 Th1 Li2 44.15(14) . 8_755 ? S2 Th1 Li2 43.38(14) . 8_755 ? S6 Th1 Li2 43.46(16) . 8_755 ? S3 Th1 Li2 135.00(15) . 8_755 ? S5 Th1 Li2 138.78(13) . 8_755 ? C26 Th1 P1 132.55(10) . . ? C51 Th1 P1 103.41(10) . . ? C1 Th1 P1 27.58(10) . . ? S1 Th1 P1 36.15(3) . . ? S4 Th1 P1 154.46(3) . . ? S2 Th1 P1 90.53(3) . . ? S6 Th1 P1 85.69(3) . . ? S3 Th1 P1 72.13(3) . . ? S5 Th1 P1 106.65(3) . . ? Li2 Th1 P1 110.62(14) 8_755 . ? C26 Th1 Li1 89.22(19) . . ? C51 Th1 Li1 89.32(19) . . ? C1 Th1 Li1 90.05(19) . . ? S1 Th1 Li1 43.72(17) . . ? S4 Th1 Li1 137.78(16) . . ? S2 Th1 Li1 135.40(16) . . ? S6 Th1 Li1 135.97(17) . . ? S3 Th1 Li1 44.36(16) . . ? S5 Th1 Li1 43.14(16) . . ? Li2 Th1 Li1 178.0(2) 8_755 . ? P1 Th1 Li1 67.48(16) . . ? C86 O6 C87 114.3(4) . . ? C86 O6 Li2 118.9(4) . . ? C87 O6 Li2 124.1(4) . . ? C84 O5 C85 111.6(4) . . ? C84 O5 Li1 120.8(4) . . ? C85 O5 Li1 118.4(4) . . ? O6 C86 C85 110.6(4) . . ? O6 C86 H86A 109.5 . . ? C85 C86 H86A 109.5 . . ? O6 C86 H86B 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 108.1 . . ? O5 C85 C86 106.2(4) . . ? O5 C85 H85A 110.5 . . ? C86 C85 H85A 110.5 . . ? O5 C85 H85B 110.5 . . ? C86 C85 H85B 110.5 . . ? H85A C85 H85B 108.7 . . ? O6 C87 H87A 109.5 . . ? O6 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? O6 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? O5 C84 H84A 109.5 . . ? O5 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? O5 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? O6 Li2 S2 132.0(4) . 8_765 ? O6 Li2 S6 115.3(4) . 8_765 ? S2 Li2 S6 102.3(3) 8_765 8_765 ? O6 Li2 S4 108.8(4) . 8_765 ? S2 Li2 S4 95.9(3) 8_765 8_765 ? S6 Li2 S4 95.1(3) 8_765 8_765 ? O6 Li2 Th1 166.0(4) . 8_765 ? S2 Li2 Th1 60.60(17) 8_765 8_765 ? S6 Li2 Th1 60.81(17) 8_765 8_765 ? S4 Li2 Th1 60.03(16) 8_765 8_765 ? O5 Li1 S5 109.0(4) . . ? O5 Li1 S1 132.7(5) . . ? S5 Li1 S1 97.3(3) . . ? O5 Li1 S3 116.2(4) . . ? S5 Li1 S3 97.7(3) . . ? S1 Li1 S3 97.6(3) . . ? O5 Li1 Th1 167.2(5) . . ? S5 Li1 Th1 60.98(18) . . ? S1 Li1 Th1 59.25(18) . . ? S3 Li1 Th1 60.52(18) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.346 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.131