# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Daniel Stern' _publ_contact_author_email dstern@chemie.uni-goettingen.de loop_ _publ_author_name D.Stalke N.Finkelmeier D.Stern data_1_[BrAnLi_2THF]2 _database_code_depnum_ccdc_archive 'CCDC 766244' #TrackingRef '1_[BrAnLi_2THF]2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H48 Br2 Li2 O4' _chemical_formula_sum 'C44 H48 Br2 Li2 O4' _chemical_formula_weight 814.52 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' Br Br -0.2901 2.4595 '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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.477(2) _cell_length_b 17.529(3) _cell_length_c 19.792(3) _cell_angle_alpha 64.145(2) _cell_angle_beta 78.978(2) _cell_angle_gamma 89.269(2) _cell_volume 3811.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9810 _cell_measurement_theta_min 2.193 _cell_measurement_theta_max 26.763 _exptl_crystal_description Platte _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 2.169 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6708 _exptl_absorpt_correction_T_max 0.8993 _exptl_absorpt_process_details SADABS-2007/4 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Mo rotating anode' _diffrn_radiation_monochromator 'multilayer mirror optics' _diffrn_measurement_device_type 'BRUKER TXS rotating anode' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 77094 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.68 _reflns_number_total 14441 _reflns_number_gt 11881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2.2-0' _computing_cell_refinement 'SAINT V7.46A' _computing_data_reduction 'SAINT V7.46A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL v6.10' _computing_publication_material 'XP in SHELXTL v6.10' _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^)+(0.0563P)^2^+2.0145P] 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 14441 _refine_ls_number_parameters 937 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.082 _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 Br1 Br 0.24127(2) 1.229883(16) 0.382546(15) 0.02595(8) Uani 1 1 d . . . Br2 Br -0.22765(2) 0.761768(19) 0.120431(17) 0.03416(8) Uani 1 1 d . . . Br3 Br 0.75276(2) 0.729279(17) -0.113133(14) 0.02676(8) Uani 1 1 d . . . Br4 Br 0.29574(2) 0.250118(16) 0.619071(14) 0.02414(7) Uani 1 1 d . . . C1 C 0.09792(19) 1.07161(15) 0.26836(13) 0.0167(5) Uani 1 1 d . . . C2 C 0.04550(19) 1.14041(14) 0.27748(13) 0.0153(5) Uani 1 1 d . . . C3 C -0.05528(19) 1.16452(15) 0.25151(14) 0.0195(5) Uani 1 1 d . . . H3 H -0.0840 1.1345 0.2281 0.023 Uiso 1 1 calc R . . C4 C -0.1115(2) 1.22851(16) 0.25898(15) 0.0234(6) Uani 1 1 d . . . H4 H -0.1768 1.2434 0.2398 0.028 Uiso 1 1 calc R . . C5 C -0.0715(2) 1.27276(16) 0.29576(15) 0.0230(6) Uani 1 1 d . . . H5 H -0.1116 1.3162 0.3025 0.028 Uiso 1 1 calc R . . C6 C 0.0232(2) 1.25362(15) 0.32129(14) 0.0200(5) Uani 1 1 d . . . H6 H 0.0483 1.2839 0.3458 0.024 Uiso 1 1 calc R . . C7 C 0.08652(18) 1.18847(14) 0.31202(13) 0.0148(5) Uani 1 1 d . . . C8 C 0.18572(19) 1.16825(14) 0.33571(13) 0.0159(5) Uani 1 1 d . . . C9 C 0.24600(19) 1.10435(14) 0.32582(13) 0.0164(5) Uani 1 1 d . . . C10 C 0.3503(2) 1.08448(15) 0.34724(14) 0.0213(5) Uani 1 1 d . . . H10 H 0.3812 1.1160 0.3685 0.026 Uiso 1 1 calc R . . C11 C 0.4056(2) 1.02142(17) 0.33767(16) 0.0276(6) Uani 1 1 d . . . H11 H 0.4744 1.0094 0.3522 0.033 Uiso 1 1 calc R . . C12 C 0.3610(2) 0.97355(17) 0.30607(16) 0.0276(6) Uani 1 1 d . . . H12 H 0.3999 0.9295 0.2996 0.033 Uiso 1 1 calc R . . C13 C 0.2623(2) 0.99062(16) 0.28492(15) 0.0241(6) Uani 1 1 d . . . H13 H 0.2337 0.9576 0.2641 0.029 Uiso 1 1 calc R . . C14 C 0.19980(19) 1.05676(15) 0.29294(14) 0.0169(5) Uani 1 1 d . . . C15 C -0.05903(19) 0.90995(15) 0.23327(13) 0.0176(5) Uani 1 1 d . . . C16 C -0.01336(19) 0.83966(15) 0.22307(13) 0.0173(5) Uani 1 1 d . . . C17 C 0.0890(2) 0.81282(16) 0.24532(14) 0.0221(5) Uani 1 1 d . . . H17 H 0.1240 0.8427 0.2664 0.027 Uiso 1 1 calc R . . C18 C 0.1382(2) 0.74625(17) 0.23754(15) 0.0265(6) Uani 1 1 d . . . H18 H 0.2059 0.7305 0.2531 0.032 Uiso 1 1 calc R . . C19 C 0.0875(2) 0.70065(17) 0.20600(16) 0.0289(6) Uani 1 1 d . . . H19 H 0.1213 0.6541 0.2008 0.035 Uiso 1 1 calc R . . C20 C -0.0089(2) 0.72312(16) 0.18325(15) 0.0261(6) Uani 1 1 d . . . H20 H -0.0411 0.6923 0.1619 0.031 Uiso 1 1 calc R . . C21 C -0.0631(2) 0.79269(15) 0.19087(14) 0.0191(5) Uani 1 1 d . . . C22 C -0.1625(2) 0.81822(16) 0.16814(14) 0.0207(5) Uani 1 1 d . . . C23 C -0.2157(2) 0.88395(15) 0.17886(13) 0.0197(5) Uani 1 1 d . . . C24 C -0.3199(2) 0.90924(17) 0.15913(15) 0.0267(6) Uani 1 1 d . . . H24 H -0.3547 0.8814 0.1364 0.032 Uiso 1 1 calc R . . C25 C -0.3696(2) 0.97231(18) 0.17242(16) 0.0308(6) Uani 1 1 d . . . H25 H -0.4389 0.9873 0.1595 0.037 Uiso 1 1 calc R . . C26 C -0.3194(2) 1.01576(17) 0.20520(16) 0.0286(6) Uani 1 1 d . . . H26 H -0.3551 1.0592 0.2149 0.034 Uiso 1 1 calc R . . C27 C -0.2192(2) 0.99479(15) 0.22280(15) 0.0227(5) Uani 1 1 d . . . H27 H -0.1854 1.0257 0.2434 0.027 Uiso 1 1 calc R . . C28 C -0.16255(19) 0.92825(15) 0.21158(13) 0.0182(5) Uani 1 1 d . . . C29 C -0.0400(2) 1.09721(18) 0.03882(16) 0.0326(6) Uani 1 1 d U . . H29A H -0.0685 1.0367 0.0634 0.039 Uiso 1 1 calc R . . H29B H 0.0163 1.1080 -0.0077 0.039 Uiso 1 1 calc R . . C30 C -0.1314(3) 1.1545(3) 0.01853(19) 0.0520(9) Uani 1 1 d U . . H30A H -0.2033 1.1242 0.0496 0.062 Uiso 1 1 calc R . . H30B H -0.1330 1.1764 -0.0366 0.062 Uiso 1 1 calc R . . C31 C -0.1031(4) 1.2256(3) 0.0375(2) 0.0721(12) Uani 1 1 d U . . H31A H -0.1594 1.2259 0.0800 0.087 Uiso 1 1 calc R . . H31B H -0.0981 1.2814 -0.0078 0.087 Uiso 1 1 calc R . . C32 C 0.0073(3) 1.20771(17) 0.06087(16) 0.0328(6) Uani 1 1 d U . . H32A H 0.0685 1.2358 0.0161 0.039 Uiso 1 1 calc R . . H32B H 0.0138 1.2269 0.1003 0.039 Uiso 1 1 calc R . . C33 C 0.2910(2) 1.07199(17) 0.08684(16) 0.0282(6) Uani 1 1 d . . . H33A H 0.3156 1.0802 0.1281 0.034 Uiso 1 1 calc R . . H33B H 0.2739 1.1276 0.0487 0.034 Uiso 1 1 calc R . . C34 C 0.3791(2) 1.0340(2) 0.0489(2) 0.0427(8) Uani 1 1 d . . . H34A H 0.4104 1.0757 -0.0046 0.051 Uiso 1 1 calc R . . H34B H 0.4389 1.0164 0.0777 0.051 Uiso 1 1 calc R . . C35 C 0.3206(2) 0.95751(19) 0.05063(17) 0.0342(7) Uani 1 1 d . . . H35A H 0.3412 0.9552 0.0008 0.041 Uiso 1 1 calc R . . H35B H 0.3370 0.9038 0.0917 0.041 Uiso 1 1 calc R . . C36 C 0.2012(2) 0.97370(18) 0.06699(16) 0.0280(6) Uani 1 1 d . . . H36A H 0.1779 1.0126 0.0192 0.034 Uiso 1 1 calc R . . H36B H 0.1539 0.9198 0.0915 0.034 Uiso 1 1 calc R . . C37 C 0.0910(2) 0.85368(16) 0.45764(15) 0.0238(6) Uani 1 1 d . . . H37A H 0.0385 0.8611 0.4983 0.029 Uiso 1 1 calc R . . H37B H 0.1499 0.9004 0.4344 0.029 Uiso 1 1 calc R . . C38 C 0.1376(2) 0.76847(17) 0.48953(16) 0.0276(6) Uani 1 1 d . . . H38A H 0.1427 0.7500 0.5437 0.033 Uiso 1 1 calc R . . H38B H 0.2113 0.7704 0.4591 0.033 Uiso 1 1 calc R . . C39 C 0.0555(2) 0.70897(18) 0.48293(18) 0.0338(7) Uani 1 1 d . . . H39A H 0.0934 0.6763 0.4567 0.041 Uiso 1 1 calc R . . H39B H 0.0141 0.6687 0.5342 0.041 Uiso 1 1 calc R . . C40 C -0.0206(2) 0.76861(16) 0.43543(15) 0.0237(6) Uani 1 1 d . . . H40A H -0.0344 0.7522 0.3957 0.028 Uiso 1 1 calc R . . H40B H -0.0915 0.7672 0.4686 0.028 Uiso 1 1 calc R . . C41 C -0.1244(2) 0.99568(16) 0.44544(14) 0.0213(5) Uani 1 1 d . . . H41A H -0.0540 1.0311 0.4245 0.026 Uiso 1 1 calc R . . H41B H -0.1209 0.9484 0.4959 0.026 Uiso 1 1 calc R . . C42 C -0.2192(2) 1.04880(16) 0.45328(15) 0.0242(6) Uani 1 1 d . . . H42A H -0.1974 1.1102 0.4216 0.029 Uiso 1 1 calc R . . H42B H -0.2450 1.0379 0.5074 0.029 Uiso 1 1 calc R . . C43 C -0.3083(2) 1.0188(2) 0.42397(19) 0.0355(7) Uani 1 1 d . . . H43A H -0.3784 1.0017 0.4620 0.043 Uiso 1 1 calc R . . H43B H -0.3203 1.0643 0.3748 0.043 Uiso 1 1 calc R . . C44 C -0.2626(2) 0.94351(17) 0.41329(15) 0.0243(6) Uani 1 1 d . . . H44A H -0.2837 0.8902 0.4612 0.029 Uiso 1 1 calc R . . H44B H -0.2890 0.9376 0.3716 0.029 Uiso 1 1 calc R . . C45 C 0.42376(19) 0.41042(14) 0.34646(13) 0.0157(5) Uani 1 1 d . . . C46 C 0.47458(18) 0.33797(14) 0.39232(13) 0.0147(5) Uani 1 1 d . . . C47 C 0.56964(19) 0.31133(15) 0.35661(14) 0.0184(5) Uani 1 1 d . . . H47 H 0.5980 0.3439 0.3033 0.022 Uiso 1 1 calc R . . C48 C 0.62048(19) 0.24131(16) 0.39626(14) 0.0206(5) Uani 1 1 d . . . H48 H 0.6825 0.2257 0.3703 0.025 Uiso 1 1 calc R . . C49 C 0.5811(2) 0.19171(15) 0.47604(14) 0.0209(5) Uani 1 1 d . . . H49 H 0.6167 0.1428 0.5035 0.025 Uiso 1 1 calc R . . C50 C 0.4923(2) 0.21403(15) 0.51356(14) 0.0190(5) Uani 1 1 d . . . H50 H 0.4670 0.1805 0.5671 0.023 Uiso 1 1 calc R . . C51 C 0.43649(18) 0.28705(14) 0.47381(13) 0.0152(5) Uani 1 1 d . . . C52 C 0.34610(19) 0.31269(14) 0.51063(13) 0.0152(5) Uani 1 1 d . . . C53 C 0.29039(18) 0.38289(14) 0.47010(14) 0.0163(5) Uani 1 1 d . . . C54 C 0.19906(19) 0.41153(16) 0.50606(15) 0.0217(5) Uani 1 1 d . . . H54 H 0.1748 0.3828 0.5602 0.026 Uiso 1 1 calc R . . C55 C 0.1464(2) 0.47866(17) 0.46463(16) 0.0258(6) Uani 1 1 d . . . H55 H 0.0869 0.4970 0.4901 0.031 Uiso 1 1 calc R . . C56 C 0.1792(2) 0.52184(16) 0.38358(16) 0.0254(6) Uani 1 1 d . . . H56 H 0.1401 0.5675 0.3547 0.030 Uiso 1 1 calc R . . C57 C 0.26690(19) 0.49734(15) 0.34765(15) 0.0204(5) Uani 1 1 d . . . H57 H 0.2881 0.5270 0.2934 0.024 Uiso 1 1 calc R . . C58 C 0.32909(19) 0.42876(14) 0.38785(14) 0.0167(5) Uani 1 1 d . . . C59 C 0.57551(19) 0.57991(15) 0.15279(13) 0.0161(5) Uani 1 1 d . . . C60 C 0.52860(19) 0.64773(14) 0.09817(13) 0.0152(5) Uani 1 1 d . . . C61 C 0.42341(19) 0.67299(15) 0.12192(14) 0.0191(5) Uani 1 1 d . . . H61 H 0.3874 0.6440 0.1743 0.023 Uiso 1 1 calc R . . C62 C 0.3733(2) 0.73651(15) 0.07263(15) 0.0219(5) Uani 1 1 d . . . H62 H 0.3041 0.7515 0.0909 0.026 Uiso 1 1 calc R . . C63 C 0.4243(2) 0.78029(16) -0.00593(15) 0.0229(5) Uani 1 1 d . . . H63 H 0.3887 0.8241 -0.0404 0.028 Uiso 1 1 calc R . . C64 C 0.5238(2) 0.75990(15) -0.03232(14) 0.0204(5) Uani 1 1 d . . . H64 H 0.5568 0.7899 -0.0852 0.024 Uiso 1 1 calc R . . C65 C 0.58021(19) 0.69409(14) 0.01783(13) 0.0155(5) Uani 1 1 d . . . C66 C 0.68319(19) 0.67170(15) -0.00696(13) 0.0163(5) Uani 1 1 d . . . C67 C 0.73747(19) 0.60839(14) 0.04353(13) 0.0150(5) Uani 1 1 d . . . C68 C 0.8453(2) 0.58676(16) 0.02073(14) 0.0205(5) Uani 1 1 d . . . H68 H 0.8829 0.6164 -0.0312 0.025 Uiso 1 1 calc R . . C69 C 0.8944(2) 0.52498(16) 0.07168(15) 0.0234(6) Uani 1 1 d . . . H69 H 0.9661 0.5122 0.0552 0.028 Uiso 1 1 calc R . . C70 C 0.8398(2) 0.47900(16) 0.14958(14) 0.0221(5) Uani 1 1 d . . . H70 H 0.8744 0.4353 0.1849 0.027 Uiso 1 1 calc R . . C71 C 0.7377(2) 0.49792(15) 0.17326(14) 0.0188(5) Uani 1 1 d . . . H71 H 0.7022 0.4664 0.2255 0.023 Uiso 1 1 calc R . . C72 C 0.68118(19) 0.56336(14) 0.12290(13) 0.0148(5) Uani 1 1 d . . . C73 C 0.2160(2) 0.42817(16) 0.21333(15) 0.0235(6) Uani 1 1 d . . . H73A H 0.1895 0.4245 0.2652 0.028 Uiso 1 1 calc R . . H73B H 0.2261 0.3701 0.2181 0.028 Uiso 1 1 calc R . . C74 C 0.1349(2) 0.47114(18) 0.16164(16) 0.0298(6) Uani 1 1 d . . . H74A H 0.0808 0.4990 0.1851 0.036 Uiso 1 1 calc R . . H74B H 0.0954 0.4292 0.1523 0.036 Uiso 1 1 calc R . . C75 C 0.2062(2) 0.53705(17) 0.08686(16) 0.0281(6) Uani 1 1 d . . . H75A H 0.1878 0.5337 0.0417 0.034 Uiso 1 1 calc R . . H75B H 0.1975 0.5954 0.0817 0.034 Uiso 1 1 calc R . . C76 C 0.3209(2) 0.51169(16) 0.09566(14) 0.0230(5) Uani 1 1 d . . . H76A H 0.3397 0.4665 0.0792 0.028 Uiso 1 1 calc R . . H76B H 0.3755 0.5611 0.0652 0.028 Uiso 1 1 calc R . . C77 C 0.5733(2) 0.39227(17) 0.10363(15) 0.0264(6) Uani 1 1 d . . . H77A H 0.6148 0.4487 0.0783 0.032 Uiso 1 1 calc R . . H77B H 0.5252 0.3896 0.0702 0.032 Uiso 1 1 calc R . . C78 C 0.6503(2) 0.32178(19) 0.12013(17) 0.0319(7) Uani 1 1 d . . . H78A H 0.7189 0.3386 0.1300 0.038 Uiso 1 1 calc R . . H78B H 0.6684 0.3067 0.0768 0.038 Uiso 1 1 calc R . . C79 C 0.5846(2) 0.24719(18) 0.19245(17) 0.0314(6) Uani 1 1 d . . . H79A H 0.5644 0.2005 0.1807 0.038 Uiso 1 1 calc R . . H79B H 0.6272 0.2248 0.2335 0.038 Uiso 1 1 calc R . . C80 C 0.4829(2) 0.28647(15) 0.21597(15) 0.0232(5) Uani 1 1 d . . . H80A H 0.4192 0.2717 0.1996 0.028 Uiso 1 1 calc R . . H80B H 0.4647 0.2659 0.2723 0.028 Uiso 1 1 calc R . . C81 C 0.5095(2) 0.71807(15) 0.25883(15) 0.0242(6) Uani 1 1 d . . . H81A H 0.5062 0.7385 0.2041 0.029 Uiso 1 1 calc R . . H81B H 0.5869 0.7225 0.2627 0.029 Uiso 1 1 calc R . . C82 C 0.4401(2) 0.76971(17) 0.29358(18) 0.0315(7) Uani 1 1 d . . . H82A H 0.3887 0.8017 0.2608 0.038 Uiso 1 1 calc R . . H82B H 0.4871 0.8103 0.2997 0.038 Uiso 1 1 calc R . . C83 C 0.3777(2) 0.70344(18) 0.37162(17) 0.0309(6) Uani 1 1 d . . . H83A H 0.3860 0.7187 0.4131 0.037 Uiso 1 1 calc R . . H83B H 0.2989 0.6974 0.3719 0.037 Uiso 1 1 calc R . . C84 C 0.4318(2) 0.62265(17) 0.38048(15) 0.0262(6) Uani 1 1 d . . . H84A H 0.4971 0.6177 0.4033 0.031 Uiso 1 1 calc R . . H84B H 0.3801 0.5719 0.4133 0.031 Uiso 1 1 calc R . . C85 C 0.6458(2) 0.47824(17) 0.41494(15) 0.0308(6) Uani 1 1 d . . . H85A H 0.5798 0.4377 0.4374 0.037 Uiso 1 1 calc R . . H85B H 0.6422 0.5148 0.4417 0.037 Uiso 1 1 calc R . . C86 C 0.7484(3) 0.43186(19) 0.4210(2) 0.0474(9) Uani 1 1 d . . . H86A H 0.7371 0.3770 0.4193 0.057 Uiso 1 1 calc R . . H86B H 0.7722 0.4211 0.4691 0.057 Uiso 1 1 calc R . . C87 C 0.8324(3) 0.4928(2) 0.3507(2) 0.0477(9) Uani 1 1 d . . . H87A H 0.8662 0.4639 0.3196 0.057 Uiso 1 1 calc R . . H87B H 0.8908 0.5153 0.3662 0.057 Uiso 1 1 calc R . . C88 C 0.7649(2) 0.56446(18) 0.30558(16) 0.0280(6) Uani 1 1 d . . . H88A H 0.7746 0.6148 0.3149 0.034 Uiso 1 1 calc R . . H88B H 0.7870 0.5817 0.2498 0.034 Uiso 1 1 calc R . . Li1 Li 0.0637(3) 1.0321(3) 0.1790(2) 0.0205(9) Uani 1 1 d . . . Li2 Li -0.0221(3) 0.9468(3) 0.3221(2) 0.0198(9) Uani 1 1 d . . . Li3 Li 0.4535(3) 0.4574(3) 0.2184(2) 0.0189(8) Uani 1 1 d . . . Li4 Li 0.5323(3) 0.5410(3) 0.2796(2) 0.0211(9) Uani 1 1 d . . . O1 O 0.00529(15) 1.11727(11) 0.09120(10) 0.0263(4) Uani 1 1 d . . . O2 O 0.19655(14) 1.01193(11) 0.11802(10) 0.0257(4) Uani 1 1 d . . . O3 O 0.03662(15) 0.85208(11) 0.40048(10) 0.0237(4) Uani 1 1 d . . . O4 O -0.14603(14) 0.96330(11) 0.39361(10) 0.0252(4) Uani 1 1 d . . . O5 O 0.31685(13) 0.48106(11) 0.17640(9) 0.0209(4) Uani 1 1 d . . . O6 O 0.51060(15) 0.37682(11) 0.17776(10) 0.0235(4) Uani 1 1 d . . . O7 O 0.46226(14) 0.63166(10) 0.30329(10) 0.0214(4) Uani 1 1 d . . . O8 O 0.65385(14) 0.52860(11) 0.33416(10) 0.0238(4) 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 Br1 0.03288(15) 0.02288(14) 0.02534(15) -0.01245(12) -0.00846(11) -0.00342(11) Br2 0.03347(16) 0.04481(18) 0.03134(17) -0.02524(14) -0.00073(12) -0.01306(13) Br3 0.02900(14) 0.02803(15) 0.01647(14) -0.00560(11) 0.00015(10) 0.00147(11) Br4 0.02672(14) 0.02527(14) 0.01711(14) -0.00819(11) 0.00026(10) -0.00135(11) C1 0.0172(11) 0.0160(12) 0.0153(12) -0.0064(10) -0.0011(9) -0.0025(9) C2 0.0171(11) 0.0126(11) 0.0114(11) -0.0019(9) -0.0003(9) -0.0021(9) C3 0.0196(12) 0.0204(13) 0.0169(13) -0.0068(10) -0.0034(10) -0.0024(10) C4 0.0174(12) 0.0232(13) 0.0255(14) -0.0076(11) -0.0034(10) 0.0031(10) C5 0.0225(13) 0.0159(12) 0.0255(14) -0.0074(11) 0.0019(11) 0.0032(10) C6 0.0255(13) 0.0137(12) 0.0176(13) -0.0065(10) 0.0020(10) -0.0016(10) C7 0.0170(11) 0.0125(11) 0.0102(11) -0.0024(9) 0.0023(9) -0.0042(9) C8 0.0218(12) 0.0131(11) 0.0111(12) -0.0040(9) -0.0028(9) -0.0035(9) C9 0.0187(12) 0.0127(11) 0.0130(12) -0.0021(10) -0.0013(9) -0.0017(9) C10 0.0215(12) 0.0189(13) 0.0210(13) -0.0052(11) -0.0073(10) -0.0032(10) C11 0.0190(13) 0.0265(14) 0.0319(16) -0.0073(12) -0.0072(11) 0.0036(11) C12 0.0246(14) 0.0205(13) 0.0391(17) -0.0146(12) -0.0066(12) 0.0084(11) C13 0.0239(13) 0.0202(13) 0.0305(15) -0.0147(12) -0.0021(11) 0.0020(10) C14 0.0179(12) 0.0139(12) 0.0165(12) -0.0054(10) -0.0012(10) 0.0006(9) C15 0.0222(12) 0.0164(12) 0.0134(12) -0.0063(10) -0.0024(10) -0.0011(10) C16 0.0188(12) 0.0180(12) 0.0135(12) -0.0069(10) 0.0002(9) -0.0038(10) C17 0.0238(13) 0.0213(13) 0.0201(13) -0.0082(11) -0.0042(10) -0.0027(10) C18 0.0236(13) 0.0259(14) 0.0271(15) -0.0101(12) -0.0030(11) 0.0033(11) C19 0.0328(15) 0.0201(13) 0.0306(16) -0.0129(12) 0.0051(12) 0.0002(11) C20 0.0309(14) 0.0251(14) 0.0238(14) -0.0162(12) 0.0050(11) -0.0073(11) C21 0.0213(12) 0.0199(12) 0.0129(12) -0.0071(10) 0.0042(10) -0.0072(10) C22 0.0236(13) 0.0242(13) 0.0122(12) -0.0083(11) 0.0026(10) -0.0121(10) C23 0.0225(12) 0.0195(12) 0.0104(12) -0.0011(10) -0.0009(10) -0.0077(10) C24 0.0249(13) 0.0303(15) 0.0194(14) -0.0044(12) -0.0074(11) -0.0083(11) C25 0.0248(14) 0.0290(15) 0.0289(16) -0.0022(13) -0.0102(12) 0.0002(12) C26 0.0269(14) 0.0200(13) 0.0321(16) -0.0052(12) -0.0063(12) 0.0042(11) C27 0.0260(13) 0.0168(12) 0.0217(14) -0.0058(11) -0.0032(11) -0.0028(10) C28 0.0192(12) 0.0173(12) 0.0120(12) -0.0018(10) -0.0007(9) -0.0043(10) C29 0.0416(16) 0.0337(15) 0.0188(14) -0.0067(12) -0.0093(12) -0.0136(12) C30 0.0276(15) 0.092(3) 0.0289(17) -0.0179(17) -0.0106(13) 0.0041(16) C31 0.091(3) 0.090(3) 0.056(2) -0.042(2) -0.041(2) 0.067(2) C32 0.0496(17) 0.0199(14) 0.0242(15) -0.0079(12) -0.0018(13) 0.0016(12) C33 0.0254(14) 0.0285(15) 0.0300(15) -0.0152(13) 0.0021(11) -0.0040(11) C34 0.0210(14) 0.070(2) 0.056(2) -0.0444(19) -0.0075(14) 0.0064(15) C35 0.0400(17) 0.0337(16) 0.0319(16) -0.0186(14) -0.0042(13) 0.0140(13) C36 0.0288(14) 0.0328(15) 0.0248(15) -0.0172(13) 0.0003(11) -0.0027(12) C37 0.0289(14) 0.0267(14) 0.0196(13) -0.0120(11) -0.0093(11) 0.0035(11) C38 0.0278(14) 0.0336(15) 0.0304(15) -0.0198(13) -0.0129(12) 0.0131(12) C39 0.0400(17) 0.0265(15) 0.0374(17) -0.0128(13) -0.0171(14) 0.0080(13) C40 0.0201(12) 0.0224(13) 0.0245(14) -0.0069(11) -0.0037(11) -0.0027(10) C41 0.0217(12) 0.0225(13) 0.0179(13) -0.0082(11) -0.0017(10) -0.0012(10) C42 0.0281(14) 0.0238(13) 0.0243(14) -0.0134(12) -0.0071(11) 0.0040(11) C43 0.0316(15) 0.0420(18) 0.0453(19) -0.0276(15) -0.0158(14) 0.0112(13) C44 0.0218(13) 0.0260(14) 0.0237(14) -0.0110(12) -0.0010(11) -0.0061(11) C45 0.0179(11) 0.0145(11) 0.0155(12) -0.0074(10) -0.0032(9) -0.0019(9) C46 0.0156(11) 0.0141(11) 0.0150(12) -0.0071(10) -0.0030(9) -0.0026(9) C47 0.0195(12) 0.0193(12) 0.0149(12) -0.0074(10) -0.0005(10) -0.0013(10) C48 0.0174(12) 0.0223(13) 0.0230(14) -0.0118(11) -0.0022(10) 0.0046(10) C49 0.0231(13) 0.0170(12) 0.0227(13) -0.0074(11) -0.0090(10) 0.0070(10) C50 0.0229(12) 0.0160(12) 0.0161(12) -0.0051(10) -0.0043(10) -0.0006(10) C51 0.0151(11) 0.0144(11) 0.0177(12) -0.0086(10) -0.0028(9) -0.0029(9) C52 0.0178(11) 0.0152(11) 0.0123(12) -0.0066(10) -0.0007(9) -0.0056(9) C53 0.0141(11) 0.0145(12) 0.0223(13) -0.0105(10) -0.0019(10) -0.0027(9) C54 0.0170(12) 0.0253(13) 0.0247(14) -0.0149(11) 0.0009(10) -0.0024(10) C55 0.0150(12) 0.0272(14) 0.0377(16) -0.0182(13) -0.0016(11) 0.0021(10) C56 0.0202(13) 0.0198(13) 0.0350(16) -0.0099(12) -0.0089(11) 0.0047(10) C57 0.0195(12) 0.0168(12) 0.0235(14) -0.0067(11) -0.0068(10) -0.0004(10) C58 0.0169(11) 0.0137(11) 0.0208(13) -0.0081(10) -0.0057(10) -0.0018(9) C59 0.0173(11) 0.0163(12) 0.0156(12) -0.0086(10) -0.0010(9) -0.0020(9) C60 0.0184(12) 0.0135(11) 0.0151(12) -0.0082(10) -0.0020(9) -0.0015(9) C61 0.0187(12) 0.0164(12) 0.0214(13) -0.0097(11) 0.0011(10) -0.0021(10) C62 0.0204(12) 0.0187(12) 0.0267(14) -0.0111(11) -0.0028(11) 0.0021(10) C63 0.0239(13) 0.0181(12) 0.0262(14) -0.0072(11) -0.0101(11) 0.0037(10) C64 0.0245(13) 0.0174(12) 0.0167(13) -0.0051(10) -0.0045(10) -0.0007(10) C65 0.0177(11) 0.0122(11) 0.0180(12) -0.0076(10) -0.0044(9) -0.0020(9) C66 0.0204(12) 0.0161(12) 0.0108(12) -0.0056(10) 0.0000(9) -0.0049(9) C67 0.0175(11) 0.0139(11) 0.0151(12) -0.0084(10) -0.0015(9) -0.0026(9) C68 0.0214(12) 0.0223(13) 0.0172(13) -0.0104(11) 0.0020(10) -0.0016(10) C69 0.0185(12) 0.0268(14) 0.0259(14) -0.0141(12) -0.0005(10) 0.0031(10) C70 0.0236(13) 0.0202(13) 0.0206(13) -0.0059(11) -0.0081(10) 0.0060(10) C71 0.0230(12) 0.0192(12) 0.0137(12) -0.0071(10) -0.0025(10) -0.0017(10) C72 0.0181(11) 0.0129(11) 0.0161(12) -0.0088(10) -0.0035(9) -0.0006(9) C73 0.0221(13) 0.0225(13) 0.0222(14) -0.0062(11) -0.0046(11) -0.0047(10) C74 0.0220(13) 0.0348(16) 0.0304(16) -0.0113(13) -0.0081(12) 0.0014(12) C75 0.0325(15) 0.0241(14) 0.0267(15) -0.0062(12) -0.0163(12) 0.0020(11) C76 0.0265(13) 0.0240(13) 0.0160(13) -0.0066(11) -0.0041(10) -0.0027(11) C77 0.0355(15) 0.0246(14) 0.0181(14) -0.0114(11) 0.0022(11) -0.0062(12) C78 0.0228(14) 0.0439(17) 0.0382(17) -0.0279(15) -0.0023(12) 0.0011(12) C79 0.0357(16) 0.0289(15) 0.0356(17) -0.0165(13) -0.0157(13) 0.0113(12) C80 0.0256(13) 0.0189(13) 0.0255(14) -0.0101(11) -0.0052(11) -0.0014(10) C81 0.0278(14) 0.0171(13) 0.0261(14) -0.0086(11) -0.0034(11) -0.0040(11) C82 0.0309(15) 0.0218(14) 0.0479(19) -0.0197(14) -0.0117(13) 0.0051(12) C83 0.0237(14) 0.0380(16) 0.0438(18) -0.0313(15) -0.0028(12) 0.0020(12) C84 0.0297(14) 0.0300(15) 0.0202(14) -0.0152(12) 0.0023(11) -0.0033(11) C85 0.0419(17) 0.0255(14) 0.0197(14) -0.0025(12) -0.0124(12) -0.0088(12) C86 0.076(2) 0.0271(16) 0.056(2) -0.0214(16) -0.045(2) 0.0194(16) C87 0.0396(18) 0.077(3) 0.054(2) -0.049(2) -0.0237(16) 0.0314(18) C88 0.0242(14) 0.0334(15) 0.0313(16) -0.0196(13) -0.0034(11) -0.0039(12) Li1 0.022(2) 0.024(2) 0.017(2) -0.0114(18) -0.0017(17) 0.0013(17) Li2 0.024(2) 0.019(2) 0.017(2) -0.0076(17) -0.0060(17) 0.0002(17) Li3 0.023(2) 0.018(2) 0.017(2) -0.0084(17) -0.0037(17) 0.0007(16) Li4 0.024(2) 0.020(2) 0.019(2) -0.0096(18) -0.0021(17) -0.0006(17) O1 0.0350(10) 0.0203(9) 0.0239(10) -0.0061(8) -0.0157(8) -0.0008(8) O2 0.0239(9) 0.0295(10) 0.0264(10) -0.0184(9) 0.0044(8) -0.0058(8) O3 0.0299(10) 0.0220(9) 0.0184(9) -0.0056(8) -0.0115(8) -0.0009(8) O4 0.0219(9) 0.0292(10) 0.0287(10) -0.0204(9) 0.0043(8) -0.0048(8) O5 0.0192(9) 0.0255(9) 0.0150(9) -0.0055(8) -0.0048(7) -0.0026(7) O6 0.0333(10) 0.0188(9) 0.0177(9) -0.0098(8) 0.0005(8) 0.0004(8) O7 0.0271(9) 0.0166(9) 0.0196(9) -0.0100(8) 0.0023(7) -0.0027(7) O8 0.0245(9) 0.0257(10) 0.0172(9) -0.0050(8) -0.0068(7) -0.0023(8) _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 Br1 C8 1.909(2) . ? Br2 C22 1.913(2) . ? Br3 C66 1.914(2) . ? Br4 C52 1.911(2) . ? C1 C14 1.428(3) . ? C1 C2 1.428(3) . ? C1 Li1 2.271(5) . ? C1 Li2 2.368(5) . ? C2 C3 1.438(3) . ? C2 C7 1.444(3) . ? C3 C4 1.363(3) . ? C3 H3 0.9500 . ? C4 C5 1.422(4) . ? C4 H4 0.9500 . ? C5 C6 1.354(4) . ? C5 H5 0.9500 . ? C6 C7 1.437(3) . ? C6 H6 0.9500 . ? C7 C8 1.394(3) . ? C8 C9 1.404(3) . ? C9 C10 1.437(3) . ? C9 C14 1.443(3) . ? C10 C11 1.359(4) . ? C10 H10 0.9500 . ? C11 C12 1.417(4) . ? C11 H11 0.9500 . ? C12 C13 1.364(4) . ? C12 H12 0.9500 . ? C13 C14 1.438(3) . ? C13 H13 0.9500 . ? C15 C28 1.427(3) . ? C15 C16 1.428(3) . ? C15 Li2 2.242(5) . ? C15 Li1 2.352(5) . ? C16 C17 1.437(3) . ? C16 C21 1.446(3) . ? C17 C18 1.366(4) . ? C17 H17 0.9500 . ? C18 C19 1.425(4) . ? C18 H18 0.9500 . ? C19 C20 1.358(4) . ? C19 H19 0.9500 . ? C20 C21 1.438(4) . ? C20 H20 0.9500 . ? C21 C22 1.402(4) . ? C22 C23 1.397(4) . ? C23 C24 1.438(4) . ? C23 C28 1.442(3) . ? C24 C25 1.360(4) . ? C24 H24 0.9500 . ? C25 C26 1.411(4) . ? C25 H25 0.9500 . ? C26 C27 1.365(4) . ? C26 H26 0.9500 . ? C27 C28 1.433(3) . ? C27 H27 0.9500 . ? C29 O1 1.437(3) . ? C29 C30 1.504(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.513(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.522(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 O1 1.428(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O2 1.437(3) . ? C33 C34 1.522(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.519(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.513(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 O2 1.428(3) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 O3 1.436(3) . ? C37 C38 1.505(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.534(4) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.529(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 O3 1.444(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 O4 1.437(3) . ? C41 C42 1.522(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.542(4) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.514(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 O4 1.438(3) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C58 1.421(3) . ? C45 C46 1.426(3) . ? C45 Li3 2.250(5) . ? C45 Li4 2.362(5) . ? C46 C47 1.441(3) . ? C46 C51 1.444(3) . ? C47 C48 1.362(3) . ? C47 H47 0.9500 . ? C48 C49 1.417(3) . ? C48 H48 0.9500 . ? C49 C50 1.364(3) . ? C49 H49 0.9500 . ? C50 C51 1.432(3) . ? C50 H50 0.9500 . ? C51 C52 1.401(3) . ? C52 C53 1.404(3) . ? C53 C54 1.430(3) . ? C53 C58 1.448(3) . ? C54 C55 1.354(4) . ? C54 H54 0.9500 . ? C55 C56 1.418(4) . ? C55 H55 0.9500 . ? C56 C57 1.358(4) . ? C56 H56 0.9500 . ? C57 C58 1.435(3) . ? C57 H57 0.9500 . ? C59 C72 1.419(3) . ? C59 C60 1.424(3) . ? C59 Li4 2.248(5) . ? C59 Li3 2.347(5) . ? C60 C61 1.439(3) . ? C60 C65 1.449(3) . ? C61 C62 1.360(4) . ? C61 H61 0.9500 . ? C62 C63 1.416(4) . ? C62 H62 0.9500 . ? C63 C64 1.358(4) . ? C63 H63 0.9500 . ? C64 C65 1.435(3) . ? C64 H64 0.9500 . ? C65 C66 1.400(3) . ? C66 C67 1.401(3) . ? C67 C68 1.435(3) . ? C67 C72 1.447(3) . ? C68 C69 1.354(4) . ? C68 H68 0.9500 . ? C69 C70 1.421(4) . ? C69 H69 0.9500 . ? C70 C71 1.360(3) . ? C70 H70 0.9500 . ? C71 C72 1.434(3) . ? C71 H71 0.9500 . ? C73 O5 1.437(3) . ? C73 C74 1.530(4) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.532(4) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.513(4) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 O5 1.437(3) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 O6 1.434(3) . ? C77 C78 1.514(4) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C79 1.541(4) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C80 1.528(4) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 O6 1.438(3) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 O7 1.441(3) . ? C81 C82 1.529(4) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C83 1.529(4) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.515(4) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 O7 1.440(3) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 O8 1.434(3) . ? C85 C86 1.504(4) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 C87 1.534(5) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 C88 1.538(4) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 O8 1.431(3) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? Li1 O2 1.981(4) . ? Li1 O1 1.993(5) . ? Li2 O3 1.964(4) . ? Li2 O4 1.997(4) . ? Li3 O6 1.975(4) . ? Li3 O5 1.999(4) . ? Li4 O8 1.981(5) . ? Li4 O7 1.991(4) . ? 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 C14 C1 C2 113.6(2) . . ? C14 C1 Li1 120.58(19) . . ? C2 C1 Li1 120.7(2) . . ? C14 C1 Li2 112.87(19) . . ? C2 C1 Li2 112.06(18) . . ? Li1 C1 Li2 67.17(16) . . ? C1 C2 C3 119.1(2) . . ? C1 C2 C7 124.3(2) . . ? C3 C2 C7 116.5(2) . . ? C4 C3 C2 123.0(2) . . ? C4 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? C3 C4 C5 119.4(2) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C6 C5 C4 120.7(2) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 121.4(2) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C8 C7 C6 123.2(2) . . ? C8 C7 C2 117.9(2) . . ? C6 C7 C2 118.9(2) . . ? C7 C8 C9 122.0(2) . . ? C7 C8 Br1 118.82(17) . . ? C9 C8 Br1 119.19(18) . . ? C8 C9 C10 123.0(2) . . ? C8 C9 C14 117.8(2) . . ? C10 C9 C14 119.2(2) . . ? C11 C10 C9 121.3(2) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 120.3(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 120.1(2) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 122.5(2) . . ? C12 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? C1 C14 C13 119.2(2) . . ? C1 C14 C9 124.2(2) . . ? C13 C14 C9 116.6(2) . . ? C28 C15 C16 113.6(2) . . ? C28 C15 Li2 117.9(2) . . ? C16 C15 Li2 122.5(2) . . ? C28 C15 Li1 112.22(19) . . ? C16 C15 Li1 113.61(19) . . ? Li2 C15 Li1 67.89(16) . . ? C15 C16 C17 119.1(2) . . ? C15 C16 C21 124.3(2) . . ? C17 C16 C21 116.6(2) . . ? C18 C17 C16 122.8(2) . . ? C18 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? C17 C18 C19 119.6(3) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 120.6(2) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 121.3(2) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C22 C21 C20 123.3(2) . . ? C22 C21 C16 117.6(2) . . ? C20 C21 C16 119.1(2) . . ? C23 C22 C21 122.2(2) . . ? C23 C22 Br2 118.71(19) . . ? C21 C22 Br2 119.10(18) . . ? C22 C23 C24 123.5(2) . . ? C22 C23 C28 117.7(2) . . ? C24 C23 C28 118.8(2) . . ? C25 C24 C23 121.3(2) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C26 120.8(3) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C27 C26 C25 119.4(3) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C26 C27 C28 123.0(2) . . ? C26 C27 H27 118.5 . . ? C28 C27 H27 118.5 . . ? C15 C28 C27 118.8(2) . . ? C15 C28 C23 124.5(2) . . ? C27 C28 C23 116.7(2) . . ? O1 C29 C30 105.6(2) . . ? O1 C29 H29A 110.6 . . ? C30 C29 H29A 110.6 . . ? O1 C29 H29B 110.6 . . ? C30 C29 H29B 110.6 . . ? H29A C29 H29B 108.7 . . ? C29 C30 C31 103.3(3) . . ? C29 C30 H30A 111.1 . . ? C31 C30 H30A 111.1 . . ? C29 C30 H30B 111.1 . . ? C31 C30 H30B 111.1 . . ? H30A C30 H30B 109.1 . . ? C30 C31 C32 105.6(3) . . ? C30 C31 H31A 110.6 . . ? C32 C31 H31A 110.6 . . ? C30 C31 H31B 110.6 . . ? C32 C31 H31B 110.6 . . ? H31A C31 H31B 108.8 . . ? O1 C32 C31 102.4(3) . . ? O1 C32 H32A 111.3 . . ? C31 C32 H32A 111.3 . . ? O1 C32 H32B 111.3 . . ? C31 C32 H32B 111.3 . . ? H32A C32 H32B 109.2 . . ? O2 C33 C34 105.9(2) . . ? O2 C33 H33A 110.6 . . ? C34 C33 H33A 110.6 . . ? O2 C33 H33B 110.6 . . ? C34 C33 H33B 110.6 . . ? H33A C33 H33B 108.7 . . ? C35 C34 C33 104.9(2) . . ? C35 C34 H34A 110.8 . . ? C33 C34 H34A 110.8 . . ? C35 C34 H34B 110.8 . . ? C33 C34 H34B 110.8 . . ? H34A C34 H34B 108.9 . . ? C36 C35 C34 102.6(2) . . ? C36 C35 H35A 111.2 . . ? C34 C35 H35A 111.2 . . ? C36 C35 H35B 111.2 . . ? C34 C35 H35B 111.2 . . ? H35A C35 H35B 109.2 . . ? O2 C36 C35 103.9(2) . . ? O2 C36 H36A 111.0 . . ? C35 C36 H36A 111.0 . . ? O2 C36 H36B 111.0 . . ? C35 C36 H36B 111.0 . . ? H36A C36 H36B 109.0 . . ? O3 C37 C38 104.3(2) . . ? O3 C37 H37A 110.9 . . ? C38 C37 H37A 110.9 . . ? O3 C37 H37B 110.9 . . ? C38 C37 H37B 110.9 . . ? H37A C37 H37B 108.9 . . ? C37 C38 C39 103.8(2) . . ? C37 C38 H38A 111.0 . . ? C39 C38 H38A 111.0 . . ? C37 C38 H38B 111.0 . . ? C39 C38 H38B 111.0 . . ? H38A C38 H38B 109.0 . . ? C40 C39 C38 104.3(2) . . ? C40 C39 H39A 110.9 . . ? C38 C39 H39A 110.9 . . ? C40 C39 H39B 110.9 . . ? C38 C39 H39B 110.9 . . ? H39A C39 H39B 108.9 . . ? O3 C40 C39 105.1(2) . . ? O3 C40 H40A 110.7 . . ? C39 C40 H40A 110.7 . . ? O3 C40 H40B 110.7 . . ? C39 C40 H40B 110.7 . . ? H40A C40 H40B 108.8 . . ? O4 C41 C42 105.8(2) . . ? O4 C41 H41A 110.6 . . ? C42 C41 H41A 110.6 . . ? O4 C41 H41B 110.6 . . ? C42 C41 H41B 110.6 . . ? H41A C41 H41B 108.7 . . ? C41 C42 C43 103.7(2) . . ? C41 C42 H42A 111.0 . . ? C43 C42 H42A 111.0 . . ? C41 C42 H42B 111.0 . . ? C43 C42 H42B 111.0 . . ? H42A C42 H42B 109.0 . . ? C44 C43 C42 103.9(2) . . ? C44 C43 H43A 111.0 . . ? C42 C43 H43A 111.0 . . ? C44 C43 H43B 111.0 . . ? C42 C43 H43B 111.0 . . ? H43A C43 H43B 109.0 . . ? O4 C44 C43 103.9(2) . . ? O4 C44 H44A 111.0 . . ? C43 C44 H44A 111.0 . . ? O4 C44 H44B 111.0 . . ? C43 C44 H44B 111.0 . . ? H44A C44 H44B 109.0 . . ? C58 C45 C46 114.0(2) . . ? C58 C45 Li3 121.9(2) . . ? C46 C45 Li3 120.40(19) . . ? C58 C45 Li4 104.38(18) . . ? C46 C45 Li4 117.20(19) . . ? Li3 C45 Li4 67.76(16) . . ? C45 C46 C47 119.4(2) . . ? C45 C46 C51 124.4(2) . . ? C47 C46 C51 116.2(2) . . ? C48 C47 C46 122.7(2) . . ? C48 C47 H47 118.7 . . ? C46 C47 H47 118.7 . . ? C47 C48 C49 120.2(2) . . ? C47 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? C50 C49 C48 120.1(2) . . ? C50 C49 H49 119.9 . . ? C48 C49 H49 119.9 . . ? C49 C50 C51 121.3(2) . . ? C49 C50 H50 119.3 . . ? C51 C50 H50 119.3 . . ? C52 C51 C50 122.9(2) . . ? C52 C51 C46 117.6(2) . . ? C50 C51 C46 119.5(2) . . ? C51 C52 C53 121.9(2) . . ? C51 C52 Br4 119.37(18) . . ? C53 C52 Br4 118.69(17) . . ? C52 C53 C54 123.3(2) . . ? C52 C53 C58 117.8(2) . . ? C54 C53 C58 118.9(2) . . ? C55 C54 C53 121.4(2) . . ? C55 C54 H54 119.3 . . ? C53 C54 H54 119.3 . . ? C54 C55 C56 120.7(2) . . ? C54 C55 H55 119.6 . . ? C56 C55 H55 119.6 . . ? C57 C56 C55 119.4(2) . . ? C57 C56 H56 120.3 . . ? C55 C56 H56 120.3 . . ? C56 C57 C58 123.1(2) . . ? C56 C57 H57 118.5 . . ? C58 C57 H57 118.5 . . ? C45 C58 C57 119.6(2) . . ? C45 C58 C53 124.1(2) . . ? C57 C58 C53 116.3(2) . . ? C72 C59 C60 114.3(2) . . ? C72 C59 Li4 117.1(2) . . ? C60 C59 Li4 123.30(19) . . ? C72 C59 Li3 112.87(18) . . ? C60 C59 Li3 111.36(18) . . ? Li4 C59 Li3 68.06(16) . . ? C59 C60 C61 119.8(2) . . ? C59 C60 C65 123.9(2) . . ? C61 C60 C65 116.4(2) . . ? C62 C61 C60 122.8(2) . . ? C62 C61 H61 118.6 . . ? C60 C61 H61 118.6 . . ? C61 C62 C63 120.0(2) . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C64 C63 C62 120.3(2) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C63 C64 C65 121.5(2) . . ? C63 C64 H64 119.2 . . ? C65 C64 H64 119.2 . . ? C66 C65 C64 123.3(2) . . ? C66 C65 C60 117.8(2) . . ? C64 C65 C60 118.9(2) . . ? C65 C66 C67 122.1(2) . . ? C65 C66 Br3 119.23(18) . . ? C67 C66 Br3 118.64(17) . . ? C66 C67 C68 123.5(2) . . ? C66 C67 C72 117.6(2) . . ? C68 C67 C72 118.9(2) . . ? C69 C68 C67 121.4(2) . . ? C69 C68 H68 119.3 . . ? C67 C68 H68 119.3 . . ? C68 C69 C70 120.6(2) . . ? C68 C69 H69 119.7 . . ? C70 C69 H69 119.7 . . ? C71 C70 C69 119.6(2) . . ? C71 C70 H70 120.2 . . ? C69 C70 H70 120.2 . . ? C70 C71 C72 122.9(2) . . ? C70 C71 H71 118.5 . . ? C72 C71 H71 118.5 . . ? C59 C72 C71 119.2(2) . . ? C59 C72 C67 124.3(2) . . ? C71 C72 C67 116.6(2) . . ? O5 C73 C74 105.4(2) . . ? O5 C73 H73A 110.7 . . ? C74 C73 H73A 110.7 . . ? O5 C73 H73B 110.7 . . ? C74 C73 H73B 110.7 . . ? H73A C73 H73B 108.8 . . ? C73 C74 C75 104.6(2) . . ? C73 C74 H74A 110.8 . . ? C75 C74 H74A 110.8 . . ? C73 C74 H74B 110.8 . . ? C75 C74 H74B 110.8 . . ? H74A C74 H74B 108.9 . . ? C76 C75 C74 102.9(2) . . ? C76 C75 H75A 111.2 . . ? C74 C75 H75A 111.2 . . ? C76 C75 H75B 111.2 . . ? C74 C75 H75B 111.2 . . ? H75A C75 H75B 109.1 . . ? O5 C76 C75 103.8(2) . . ? O5 C76 H76A 111.0 . . ? C75 C76 H76A 111.0 . . ? O5 C76 H76B 111.0 . . ? C75 C76 H76B 111.0 . . ? H76A C76 H76B 109.0 . . ? O6 C77 C78 104.3(2) . . ? O6 C77 H77A 110.9 . . ? C78 C77 H77A 110.9 . . ? O6 C77 H77B 110.9 . . ? C78 C77 H77B 110.9 . . ? H77A C77 H77B 108.9 . . ? C77 C78 C79 103.6(2) . . ? C77 C78 H78A 111.0 . . ? C79 C78 H78A 111.0 . . ? C77 C78 H78B 111.0 . . ? C79 C78 H78B 111.0 . . ? H78A C78 H78B 109.0 . . ? C80 C79 C78 103.9(2) . . ? C80 C79 H79A 111.0 . . ? C78 C79 H79A 111.0 . . ? C80 C79 H79B 111.0 . . ? C78 C79 H79B 111.0 . . ? H79A C79 H79B 109.0 . . ? O6 C80 C79 105.4(2) . . ? O6 C80 H80A 110.7 . . ? C79 C80 H80A 110.7 . . ? O6 C80 H80B 110.7 . . ? C79 C80 H80B 110.7 . . ? H80A C80 H80B 108.8 . . ? O7 C81 C82 105.2(2) . . ? O7 C81 H81A 110.7 . . ? C82 C81 H81A 110.7 . . ? O7 C81 H81B 110.7 . . ? C82 C81 H81B 110.7 . . ? H81A C81 H81B 108.8 . . ? C81 C82 C83 104.7(2) . . ? C81 C82 H82A 110.8 . . ? C83 C82 H82A 110.8 . . ? C81 C82 H82B 110.8 . . ? C83 C82 H82B 110.8 . . ? H82A C82 H82B 108.9 . . ? C84 C83 C82 103.1(2) . . ? C84 C83 H83A 111.1 . . ? C82 C83 H83A 111.1 . . ? C84 C83 H83B 111.1 . . ? C82 C83 H83B 111.1 . . ? H83A C83 H83B 109.1 . . ? O7 C84 C83 104.1(2) . . ? O7 C84 H84A 110.9 . . ? C83 C84 H84A 110.9 . . ? O7 C84 H84B 110.9 . . ? C83 C84 H84B 110.9 . . ? H84A C84 H84B 109.0 . . ? O8 C85 C86 104.6(2) . . ? O8 C85 H85A 110.8 . . ? C86 C85 H85A 110.8 . . ? O8 C85 H85B 110.8 . . ? C86 C85 H85B 110.8 . . ? H85A C85 H85B 108.9 . . ? C85 C86 C87 103.7(2) . . ? C85 C86 H86A 111.0 . . ? C87 C86 H86A 111.0 . . ? C85 C86 H86B 111.0 . . ? C87 C86 H86B 111.0 . . ? H86A C86 H86B 109.0 . . ? C86 C87 C88 104.1(2) . . ? C86 C87 H87A 110.9 . . ? C88 C87 H87A 110.9 . . ? C86 C87 H87B 110.9 . . ? C88 C87 H87B 110.9 . . ? H87A C87 H87B 109.0 . . ? O8 C88 C87 104.6(2) . . ? O8 C88 H88A 110.8 . . ? C87 C88 H88A 110.8 . . ? O8 C88 H88B 110.8 . . ? C87 C88 H88B 110.8 . . ? H88A C88 H88B 108.9 . . ? O2 Li1 O1 97.35(19) . . ? O2 Li1 C1 114.1(2) . . ? O1 Li1 C1 117.8(2) . . ? O2 Li1 C15 108.26(19) . . ? O1 Li1 C15 105.80(19) . . ? C1 Li1 C15 112.21(19) . . ? O3 Li2 O4 96.88(19) . . ? O3 Li2 C15 110.4(2) . . ? O4 Li2 C15 119.1(2) . . ? O3 Li2 C1 110.79(19) . . ? O4 Li2 C1 105.82(18) . . ? C15 Li2 C1 112.70(19) . . ? O6 Li3 O5 98.44(19) . . ? O6 Li3 C45 116.9(2) . . ? O5 Li3 C45 113.7(2) . . ? O6 Li3 C59 105.97(19) . . ? O5 Li3 C59 108.61(19) . . ? C45 Li3 C59 112.06(18) . . ? O8 Li4 O7 96.90(19) . . ? O8 Li4 C59 117.9(2) . . ? O7 Li4 C59 112.2(2) . . ? O8 Li4 C45 105.70(19) . . ? O7 Li4 C45 111.56(19) . . ? C59 Li4 C45 111.58(18) . . ? C32 O1 C29 104.8(2) . . ? C32 O1 Li1 130.8(2) . . ? C29 O1 Li1 124.1(2) . . ? C36 O2 C33 105.29(19) . . ? C36 O2 Li1 127.26(19) . . ? C33 O2 Li1 119.85(19) . . ? C37 O3 C40 104.92(18) . . ? C37 O3 Li2 128.38(19) . . ? C40 O3 Li2 119.02(19) . . ? C41 O4 C44 104.74(18) . . ? C41 O4 Li2 120.09(18) . . ? C44 O4 Li2 134.95(19) . . ? C73 O5 C76 104.86(18) . . ? C73 O5 Li3 123.81(18) . . ? C76 O5 Li3 121.09(18) . . ? C77 O6 C80 104.41(18) . . ? C77 O6 Li3 130.31(19) . . ? C80 O6 Li3 124.79(19) . . ? C84 O7 C81 104.23(18) . . ? C84 O7 Li4 122.22(19) . . ? C81 O7 Li4 118.60(19) . . ? C88 O8 C85 104.82(19) . . ? C88 O8 Li4 130.3(2) . . ? C85 O8 Li4 124.89(19) . . ? 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 C14 C1 C2 C3 177.1(2) . . . . ? Li1 C1 C2 C3 22.2(3) . . . . ? Li2 C1 C2 C3 -53.5(3) . . . . ? C14 C1 C2 C7 -3.3(3) . . . . ? Li1 C1 C2 C7 -158.2(2) . . . . ? Li2 C1 C2 C7 126.1(2) . . . . ? C1 C2 C3 C4 179.0(2) . . . . ? C7 C2 C3 C4 -0.6(3) . . . . ? C2 C3 C4 C5 -1.7(4) . . . . ? C3 C4 C5 C6 1.9(4) . . . . ? C4 C5 C6 C7 0.2(4) . . . . ? C5 C6 C7 C8 178.3(2) . . . . ? C5 C6 C7 C2 -2.5(3) . . . . ? C1 C2 C7 C8 2.2(3) . . . . ? C3 C2 C7 C8 -178.1(2) . . . . ? C1 C2 C7 C6 -177.0(2) . . . . ? C3 C2 C7 C6 2.7(3) . . . . ? C6 C7 C8 C9 -179.9(2) . . . . ? C2 C7 C8 C9 0.9(3) . . . . ? C6 C7 C8 Br1 -0.2(3) . . . . ? C2 C7 C8 Br1 -179.36(16) . . . . ? C7 C8 C9 C10 177.7(2) . . . . ? Br1 C8 C9 C10 -2.0(3) . . . . ? C7 C8 C9 C14 -2.6(3) . . . . ? Br1 C8 C9 C14 177.68(16) . . . . ? C8 C9 C10 C11 179.2(2) . . . . ? C14 C9 C10 C11 -0.5(4) . . . . ? C9 C10 C11 C12 0.0(4) . . . . ? C10 C11 C12 C13 0.1(4) . . . . ? C11 C12 C13 C14 0.3(4) . . . . ? C2 C1 C14 C13 -178.4(2) . . . . ? Li1 C1 C14 C13 -23.5(3) . . . . ? Li2 C1 C14 C13 52.6(3) . . . . ? C2 C1 C14 C9 1.5(3) . . . . ? Li1 C1 C14 C9 156.3(2) . . . . ? Li2 C1 C14 C9 -127.5(2) . . . . ? C12 C13 C14 C1 179.0(2) . . . . ? C12 C13 C14 C9 -0.8(4) . . . . ? C8 C9 C14 C1 1.4(3) . . . . ? C10 C9 C14 C1 -178.9(2) . . . . ? C8 C9 C14 C13 -178.8(2) . . . . ? C10 C9 C14 C13 0.9(3) . . . . ? C28 C15 C16 C17 -177.9(2) . . . . ? Li2 C15 C16 C17 -25.7(3) . . . . ? Li1 C15 C16 C17 52.2(3) . . . . ? C28 C15 C16 C21 2.6(3) . . . . ? Li2 C15 C16 C21 154.7(2) . . . . ? Li1 C15 C16 C21 -127.4(2) . . . . ? C15 C16 C17 C18 180.0(2) . . . . ? C21 C16 C17 C18 -0.4(4) . . . . ? C16 C17 C18 C19 0.1(4) . . . . ? C17 C18 C19 C20 0.4(4) . . . . ? C18 C19 C20 C21 -0.6(4) . . . . ? C19 C20 C21 C22 179.9(2) . . . . ? C19 C20 C21 C16 0.3(4) . . . . ? C15 C16 C21 C22 0.1(3) . . . . ? C17 C16 C21 C22 -179.5(2) . . . . ? C15 C16 C21 C20 179.8(2) . . . . ? C17 C16 C21 C20 0.2(3) . . . . ? C20 C21 C22 C23 177.5(2) . . . . ? C16 C21 C22 C23 -2.9(3) . . . . ? C20 C21 C22 Br2 -2.8(3) . . . . ? C16 C21 C22 Br2 176.84(17) . . . . ? C21 C22 C23 C24 -177.3(2) . . . . ? Br2 C22 C23 C24 3.0(3) . . . . ? C21 C22 C23 C28 2.6(3) . . . . ? Br2 C22 C23 C28 -177.11(16) . . . . ? C22 C23 C24 C25 178.4(2) . . . . ? C28 C23 C24 C25 -1.5(4) . . . . ? C23 C24 C25 C26 0.8(4) . . . . ? C24 C25 C26 C27 0.8(4) . . . . ? C25 C26 C27 C28 -1.8(4) . . . . ? C16 C15 C28 C27 176.9(2) . . . . ? Li2 C15 C28 C27 23.4(3) . . . . ? Li1 C15 C28 C27 -52.5(3) . . . . ? C16 C15 C28 C23 -2.9(3) . . . . ? Li2 C15 C28 C23 -156.4(2) . . . . ? Li1 C15 C28 C23 127.7(2) . . . . ? C26 C27 C28 C15 -178.7(2) . . . . ? C26 C27 C28 C23 1.1(4) . . . . ? C22 C23 C28 C15 0.5(3) . . . . ? C24 C23 C28 C15 -179.6(2) . . . . ? C22 C23 C28 C27 -179.3(2) . . . . ? C24 C23 C28 C27 0.6(3) . . . . ? O1 C29 C30 C31 21.0(3) . . . . ? C29 C30 C31 C32 4.6(4) . . . . ? C30 C31 C32 O1 -28.5(3) . . . . ? O2 C33 C34 C35 8.7(3) . . . . ? C33 C34 C35 C36 16.2(3) . . . . ? C34 C35 C36 O2 -36.0(3) . . . . ? O3 C37 C38 C39 -31.6(3) . . . . ? C37 C38 C39 C40 9.2(3) . . . . ? C38 C39 C40 O3 16.1(3) . . . . ? O4 C41 C42 C43 17.7(3) . . . . ? C41 C42 C43 C44 7.9(3) . . . . ? C42 C43 C44 O4 -30.8(3) . . . . ? C58 C45 C46 C47 178.3(2) . . . . ? Li3 C45 C46 C47 19.5(3) . . . . ? Li4 C45 C46 C47 -59.4(3) . . . . ? C58 C45 C46 C51 -0.8(3) . . . . ? Li3 C45 C46 C51 -159.6(2) . . . . ? Li4 C45 C46 C51 121.5(2) . . . . ? C45 C46 C47 C48 -177.9(2) . . . . ? C51 C46 C47 C48 1.3(3) . . . . ? C46 C47 C48 C49 -0.7(4) . . . . ? C47 C48 C49 C50 -0.2(4) . . . . ? C48 C49 C50 C51 0.4(4) . . . . ? C49 C50 C51 C52 -179.0(2) . . . . ? C49 C50 C51 C46 0.2(3) . . . . ? C45 C46 C51 C52 -2.6(3) . . . . ? C47 C46 C51 C52 178.2(2) . . . . ? C45 C46 C51 C50 178.1(2) . . . . ? C47 C46 C51 C50 -1.0(3) . . . . ? C50 C51 C52 C53 -177.9(2) . . . . ? C46 C51 C52 C53 2.9(3) . . . . ? C50 C51 C52 Br4 1.6(3) . . . . ? C46 C51 C52 Br4 -177.64(16) . . . . ? C51 C52 C53 C54 -179.0(2) . . . . ? Br4 C52 C53 C54 1.6(3) . . . . ? C51 C52 C53 C58 0.2(3) . . . . ? Br4 C52 C53 C58 -179.25(16) . . . . ? C52 C53 C54 C55 -178.8(2) . . . . ? C58 C53 C54 C55 2.0(3) . . . . ? C53 C54 C55 C56 1.3(4) . . . . ? C54 C55 C56 C57 -2.4(4) . . . . ? C55 C56 C57 C58 0.2(4) . . . . ? C46 C45 C58 C57 -176.7(2) . . . . ? Li3 C45 C58 C57 -18.3(3) . . . . ? Li4 C45 C58 C57 54.2(3) . . . . ? C46 C45 C58 C53 4.3(3) . . . . ? Li3 C45 C58 C53 162.7(2) . . . . ? Li4 C45 C58 C53 -124.8(2) . . . . ? C56 C57 C58 C45 -176.2(2) . . . . ? C56 C57 C58 C53 2.9(3) . . . . ? C52 C53 C58 C45 -4.1(3) . . . . ? C54 C53 C58 C45 175.1(2) . . . . ? C52 C53 C58 C57 176.8(2) . . . . ? C54 C53 C58 C57 -4.0(3) . . . . ? C72 C59 C60 C61 -177.7(2) . . . . ? Li4 C59 C60 C61 -24.1(3) . . . . ? Li3 C59 C60 C61 53.0(3) . . . . ? C72 C59 C60 C65 2.9(3) . . . . ? Li4 C59 C60 C65 156.4(2) . . . . ? Li3 C59 C60 C65 -126.5(2) . . . . ? C59 C60 C61 C62 -179.2(2) . . . . ? C65 C60 C61 C62 0.3(3) . . . . ? C60 C61 C62 C63 0.7(4) . . . . ? C61 C62 C63 C64 -0.8(4) . . . . ? C62 C63 C64 C65 0.0(4) . . . . ? C63 C64 C65 C66 -179.4(2) . . . . ? C63 C64 C65 C60 1.0(3) . . . . ? C59 C60 C65 C66 -1.3(3) . . . . ? C61 C60 C65 C66 179.3(2) . . . . ? C59 C60 C65 C64 178.4(2) . . . . ? C61 C60 C65 C64 -1.0(3) . . . . ? C64 C65 C66 C67 178.7(2) . . . . ? C60 C65 C66 C67 -1.7(3) . . . . ? C64 C65 C66 Br3 -1.2(3) . . . . ? C60 C65 C66 Br3 178.40(16) . . . . ? C65 C66 C67 C68 -176.9(2) . . . . ? Br3 C66 C67 C68 3.0(3) . . . . ? C65 C66 C67 C72 2.6(3) . . . . ? Br3 C66 C67 C72 -177.48(16) . . . . ? C66 C67 C68 C69 -180.0(2) . . . . ? C72 C67 C68 C69 0.5(4) . . . . ? C67 C68 C69 C70 0.6(4) . . . . ? C68 C69 C70 C71 -0.7(4) . . . . ? C69 C70 C71 C72 -0.3(4) . . . . ? C60 C59 C72 C71 178.3(2) . . . . ? Li4 C59 C72 C71 23.1(3) . . . . ? Li3 C59 C72 C71 -53.1(3) . . . . ? C60 C59 C72 C67 -1.9(3) . . . . ? Li4 C59 C72 C67 -157.1(2) . . . . ? Li3 C59 C72 C67 126.7(2) . . . . ? C70 C71 C72 C59 -178.9(2) . . . . ? C70 C71 C72 C67 1.3(3) . . . . ? C66 C67 C72 C59 -0.7(3) . . . . ? C68 C67 C72 C59 178.8(2) . . . . ? C66 C67 C72 C71 179.1(2) . . . . ? C68 C67 C72 C71 -1.4(3) . . . . ? O5 C73 C74 C75 13.0(3) . . . . ? C73 C74 C75 C76 12.9(3) . . . . ? C74 C75 C76 O5 -34.5(3) . . . . ? O6 C77 C78 C79 30.8(3) . . . . ? C77 C78 C79 C80 -7.3(3) . . . . ? C78 C79 C80 O6 -18.5(3) . . . . ? O7 C81 C82 C83 16.3(3) . . . . ? C81 C82 C83 C84 9.8(3) . . . . ? C82 C83 C84 O7 -32.8(3) . . . . ? O8 C85 C86 C87 30.0(3) . . . . ? C85 C86 C87 C88 -6.5(3) . . . . ? C86 C87 C88 O8 -19.1(3) . . . . ? C14 C1 Li1 O2 -18.2(3) . . . . ? C2 C1 Li1 O2 134.9(2) . . . . ? Li2 C1 Li1 O2 -122.2(2) . . . . ? C14 C1 Li1 O1 -131.4(2) . . . . ? C2 C1 Li1 O1 21.7(3) . . . . ? Li2 C1 Li1 O1 124.6(2) . . . . ? C14 C1 Li1 C15 105.3(2) . . . . ? C2 C1 Li1 C15 -101.6(2) . . . . ? Li2 C1 Li1 C15 1.38(17) . . . . ? C28 C15 Li1 O2 -122.4(2) . . . . ? C16 C15 Li1 O2 8.2(3) . . . . ? Li2 C15 Li1 O2 125.3(2) . . . . ? C28 C15 Li1 O1 -18.9(3) . . . . ? C16 C15 Li1 O1 111.7(2) . . . . ? Li2 C15 Li1 O1 -131.2(2) . . . . ? C28 C15 Li1 C1 110.9(2) . . . . ? C16 C15 Li1 C1 -118.5(2) . . . . ? Li2 C15 Li1 C1 -1.45(18) . . . . ? C28 C15 Li2 O3 132.6(2) . . . . ? C16 C15 Li2 O3 -18.4(3) . . . . ? Li1 C15 Li2 O3 -123.1(2) . . . . ? C28 C15 Li2 O4 21.9(3) . . . . ? C16 C15 Li2 O4 -129.1(2) . . . . ? Li1 C15 Li2 O4 126.2(3) . . . . ? C28 C15 Li2 C1 -102.9(2) . . . . ? C16 C15 Li2 C1 106.1(2) . . . . ? Li1 C15 Li2 C1 1.40(17) . . . . ? C14 C1 Li2 O3 7.9(3) . . . . ? C2 C1 Li2 O3 -121.9(2) . . . . ? Li1 C1 Li2 O3 122.8(2) . . . . ? C14 C1 Li2 O4 111.8(2) . . . . ? C2 C1 Li2 O4 -18.0(3) . . . . ? Li1 C1 Li2 O4 -133.2(2) . . . . ? C14 C1 Li2 C15 -116.4(2) . . . . ? C2 C1 Li2 C15 113.8(2) . . . . ? Li1 C1 Li2 C15 -1.46(18) . . . . ? C58 C45 Li3 O6 -138.2(2) . . . . ? C46 C45 Li3 O6 18.8(3) . . . . ? Li4 C45 Li3 O6 128.3(2) . . . . ? C58 C45 Li3 O5 -24.5(3) . . . . ? C46 C45 Li3 O5 132.6(2) . . . . ? Li4 C45 Li3 O5 -118.0(2) . . . . ? C58 C45 Li3 C59 99.2(2) . . . . ? C46 C45 Li3 C59 -103.7(2) . . . . ? Li4 C45 Li3 C59 5.69(17) . . . . ? C72 C59 Li3 O6 -23.2(3) . . . . ? C60 C59 Li3 O6 106.9(2) . . . . ? Li4 C59 Li3 O6 -134.5(2) . . . . ? C72 C59 Li3 O5 -128.1(2) . . . . ? C60 C59 Li3 O5 2.0(3) . . . . ? Li4 C59 Li3 O5 120.5(2) . . . . ? C72 C59 Li3 C45 105.4(2) . . . . ? C60 C59 Li3 C45 -124.5(2) . . . . ? Li4 C59 Li3 C45 -5.96(18) . . . . ? C72 C59 Li4 O8 23.0(3) . . . . ? C60 C59 Li4 O8 -129.9(2) . . . . ? Li3 C59 Li4 O8 128.3(3) . . . . ? C72 C59 Li4 O7 134.3(2) . . . . ? C60 C59 Li4 O7 -18.5(3) . . . . ? Li3 C59 Li4 O7 -120.4(2) . . . . ? C72 C59 Li4 C45 -99.7(2) . . . . ? C60 C59 Li4 C45 107.5(2) . . . . ? Li3 C59 Li4 C45 5.66(17) . . . . ? C58 C45 Li4 O8 105.7(2) . . . . ? C46 C45 Li4 O8 -21.4(3) . . . . ? Li3 C45 Li4 O8 -135.3(2) . . . . ? C58 C45 Li4 O7 1.5(3) . . . . ? C46 C45 Li4 O7 -125.6(2) . . . . ? Li3 C45 Li4 O7 120.5(2) . . . . ? C58 C45 Li4 C59 -124.9(2) . . . . ? C46 C45 Li4 C59 107.9(2) . . . . ? Li3 C45 Li4 C59 -5.92(18) . . . . ? C31 C32 O1 C29 42.4(3) . . . . ? C31 C32 O1 Li1 -143.6(3) . . . . ? C30 C29 O1 C32 -40.6(3) . . . . ? C30 C29 O1 Li1 144.9(2) . . . . ? O2 Li1 O1 C32 -102.6(3) . . . . ? C1 Li1 O1 C32 19.6(4) . . . . ? C15 Li1 O1 C32 146.0(2) . . . . ? O2 Li1 O1 C29 70.4(3) . . . . ? C1 Li1 O1 C29 -167.4(2) . . . . ? C15 Li1 O1 C29 -41.0(3) . . . . ? C35 C36 O2 C33 43.0(3) . . . . ? C35 C36 O2 Li1 -168.1(2) . . . . ? C34 C33 O2 C36 -32.2(3) . . . . ? C34 C33 O2 Li1 176.1(2) . . . . ? O1 Li1 O2 C36 -66.1(3) . . . . ? C1 Li1 O2 C36 169.0(2) . . . . ? C15 Li1 O2 C36 43.3(3) . . . . ? O1 Li1 O2 C33 78.9(2) . . . . ? C1 Li1 O2 C33 -46.1(3) . . . . ? C15 Li1 O2 C33 -171.7(2) . . . . ? C38 C37 O3 C40 43.1(2) . . . . ? C38 C37 O3 Li2 -168.5(2) . . . . ? C39 C40 O3 C37 -36.8(3) . . . . ? C39 C40 O3 Li2 171.2(2) . . . . ? O4 Li2 O3 C37 -69.4(3) . . . . ? C15 Li2 O3 C37 166.0(2) . . . . ? C1 Li2 O3 C37 40.4(3) . . . . ? O4 Li2 O3 C40 75.2(2) . . . . ? C15 Li2 O3 C40 -49.4(3) . . . . ? C1 Li2 O3 C40 -174.97(18) . . . . ? C42 C41 O4 C44 -38.2(2) . . . . ? C42 C41 O4 Li2 146.4(2) . . . . ? C43 C44 O4 C41 43.2(3) . . . . ? C43 C44 O4 Li2 -142.5(3) . . . . ? O3 Li2 O4 C41 68.7(2) . . . . ? C15 Li2 O4 C41 -173.3(2) . . . . ? C1 Li2 O4 C41 -45.3(3) . . . . ? O3 Li2 O4 C44 -105.0(3) . . . . ? C15 Li2 O4 C44 13.0(4) . . . . ? C1 Li2 O4 C44 141.1(2) . . . . ? C74 C73 O5 C76 -35.6(3) . . . . ? C74 C73 O5 Li3 179.3(2) . . . . ? C75 C76 O5 C73 44.3(2) . . . . ? C75 C76 O5 Li3 -169.3(2) . . . . ? O6 Li3 O5 C73 84.1(2) . . . . ? C45 Li3 O5 C73 -40.3(3) . . . . ? C59 Li3 O5 C73 -165.80(19) . . . . ? O6 Li3 O5 C76 -55.7(3) . . . . ? C45 Li3 O5 C76 179.87(19) . . . . ? C59 Li3 O5 C76 54.4(3) . . . . ? C78 C77 O6 C80 -43.8(2) . . . . ? C78 C77 O6 Li3 144.1(2) . . . . ? C79 C80 O6 C77 38.9(3) . . . . ? C79 C80 O6 Li3 -148.4(2) . . . . ? O5 Li3 O6 C77 83.1(3) . . . . ? C45 Li3 O6 C77 -154.8(2) . . . . ? C59 Li3 O6 C77 -29.1(3) . . . . ? O5 Li3 O6 C80 -87.6(2) . . . . ? C45 Li3 O6 C80 34.5(3) . . . . ? C59 Li3 O6 C80 160.20(19) . . . . ? C83 C84 O7 C81 44.5(2) . . . . ? C83 C84 O7 Li4 -177.5(2) . . . . ? C82 C81 O7 C84 -37.7(3) . . . . ? C82 C81 O7 Li4 -177.6(2) . . . . ? O8 Li4 O7 C84 -53.2(3) . . . . ? C59 Li4 O7 C84 -177.25(19) . . . . ? C45 Li4 O7 C84 56.7(3) . . . . ? O8 Li4 O7 C81 79.2(2) . . . . ? C59 Li4 O7 C81 -44.8(3) . . . . ? C45 Li4 O7 C81 -170.91(19) . . . . ? C87 C88 O8 C85 38.9(3) . . . . ? C87 C88 O8 Li4 -140.9(2) . . . . ? C86 C85 O8 C88 -43.7(3) . . . . ? C86 C85 O8 Li4 136.1(2) . . . . ? O7 Li4 O8 C88 -97.5(3) . . . . ? C59 Li4 O8 C88 22.2(4) . . . . ? C45 Li4 O8 C88 147.8(2) . . . . ? O7 Li4 O8 C85 82.8(3) . . . . ? C59 Li4 O8 C85 -157.5(2) . . . . ? C45 Li4 O8 C85 -31.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.697 _refine_diff_density_min -0.766 _refine_diff_density_rms 0.075 # Attachment '2_[BrAnLi_DME]2.cif' data_2_[BrAnLi_DME]2 _database_code_depnum_ccdc_archive 'CCDC 766245' #TrackingRef '2_[BrAnLi_DME]2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H36 Br2 Li2 O4' _chemical_formula_sum 'C36 H36 Br2 Li2 O4' _chemical_formula_weight 706.35 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.578(2) _cell_length_b 9.1589(19) _cell_length_c 15.943(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.795(3) _cell_angle_gamma 90.00 _cell_volume 1544.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5403 _cell_measurement_theta_min 2.296 _cell_measurement_theta_max 25.412 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 2.664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4586 _exptl_absorpt_correction_T_max 0.5870 _exptl_absorpt_process_details SADABS-2007/4 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Mo rotating anode' _diffrn_radiation_monochromator 'INCOATEC Helios mirror optics' _diffrn_measurement_device_type 'BRUKER TXS with D8-Goniometer' _diffrn_measurement_method 'omega sceans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15536 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.45 _reflns_number_total 2840 _reflns_number_gt 2417 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2.2-0' _computing_cell_refinement 'SAINT V7.46A' _computing_data_reduction 'SAINT V7.46A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL v6.10' _computing_publication_material 'XP in SHELXTL v6.10' _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^)+(0.0843P)^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 2840 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Br1 Br 0.11742(3) 0.07609(3) 0.166844(19) 0.02790(16) Uani 1 1 d . . . O1 O 0.24364(19) 0.6790(2) 0.53254(14) 0.0264(5) Uani 1 1 d . . . O2 O 0.0537(2) 0.7964(2) 0.43655(13) 0.0263(5) Uani 1 1 d . . . Li1 Li 0.0787(5) 0.5973(5) 0.4851(3) 0.0254(12) Uani 1 1 d . . . C1 C 0.0949(3) 0.2111(3) 0.25735(18) 0.0217(6) Uani 1 1 d . . . C2 C 0.1824(3) 0.2092(3) 0.32328(18) 0.0215(6) Uani 1 1 d . . . C3 C 0.2932(3) 0.1199(3) 0.32371(19) 0.0255(7) Uani 1 1 d . . . H3 H 0.3109 0.0608 0.2763 0.031 Uiso 1 1 calc R . . C4 C 0.3732(3) 0.1183(4) 0.3907(2) 0.0265(7) Uani 1 1 d . . . H4 H 0.4477 0.0604 0.3891 0.032 Uiso 1 1 calc R . . C5 C 0.3476(3) 0.2012(4) 0.4626(2) 0.0275(7) Uani 1 1 d . . . H5 H 0.4025 0.1963 0.5102 0.033 Uiso 1 1 calc R . . C6 C 0.2433(3) 0.2887(3) 0.4638(2) 0.0261(7) Uani 1 1 d . . . H6 H 0.2271 0.3431 0.5132 0.031 Uiso 1 1 calc R . . C7 C 0.1577(3) 0.3028(3) 0.39487(19) 0.0220(6) Uani 1 1 d . . . C8 C 0.0560(3) 0.4044(3) 0.3980(2) 0.0220(7) Uani 1 1 d . . . C9 C -0.0215(3) 0.4066(3) 0.3246(2) 0.0224(7) Uani 1 1 d . . . C10 C -0.1222(3) 0.5106(4) 0.31673(19) 0.0263(7) Uani 1 1 d . . . H10 H -0.1319 0.5811 0.3599 0.032 Uiso 1 1 calc R . . C11 C -0.2041(3) 0.5132(4) 0.2509(2) 0.0301(7) Uani 1 1 d . . . H11 H -0.2683 0.5856 0.2481 0.036 Uiso 1 1 calc R . . C12 C -0.1943(3) 0.4076(3) 0.1858(2) 0.0291(8) Uani 1 1 d . . . H12 H -0.2541 0.4067 0.1408 0.035 Uiso 1 1 calc R . . C13 C -0.0995(3) 0.3089(3) 0.18840(19) 0.0257(7) Uani 1 1 d . . . H13 H -0.0937 0.2389 0.1447 0.031 Uiso 1 1 calc R . . C14 C -0.0078(3) 0.3068(3) 0.25489(19) 0.0226(6) Uani 1 1 d . . . C15 C 0.3592(3) 0.6215(4) 0.5663(2) 0.0293(7) Uani 1 1 d . . . H15A H 0.4240 0.6228 0.5230 0.044 Uiso 1 1 calc R . . H15B H 0.3456 0.5209 0.5850 0.044 Uiso 1 1 calc R . . H15C H 0.3871 0.6814 0.6140 0.044 Uiso 1 1 calc R . . C16 C 0.2584(3) 0.8258(3) 0.5045(2) 0.0280(7) Uani 1 1 d . . . H16A H 0.3044 0.8283 0.4509 0.034 Uiso 1 1 calc R . . H16B H 0.3063 0.8838 0.5466 0.034 Uiso 1 1 calc R . . C17 C 0.1265(3) 0.8864(4) 0.4929(2) 0.0281(7) Uani 1 1 d . . . H17A H 0.0844 0.8910 0.5479 0.034 Uiso 1 1 calc R . . H17B H 0.1313 0.9868 0.4702 0.034 Uiso 1 1 calc R . . C18 C 0.0711(3) 0.8311(4) 0.3501(2) 0.0311(7) Uani 1 1 d . . . H18A H 0.0424 0.9312 0.3393 0.047 Uiso 1 1 calc R . . H18B H 0.0219 0.7632 0.3151 0.047 Uiso 1 1 calc R . . H18C H 0.1609 0.8227 0.3365 0.047 Uiso 1 1 calc R . . 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 Br1 0.0383(2) 0.0224(2) 0.0229(2) -0.00616(12) -0.00263(14) 0.00184(12) O1 0.0267(11) 0.0185(11) 0.0339(12) 0.0032(9) -0.0070(9) -0.0033(9) O2 0.0322(12) 0.0175(12) 0.0292(12) 0.0006(9) -0.0019(9) -0.0044(9) Li1 0.032(3) 0.020(3) 0.024(3) 0.002(2) -0.005(2) -0.005(2) C1 0.0322(16) 0.0145(15) 0.0184(15) -0.0038(11) 0.0018(12) -0.0042(12) C2 0.0279(15) 0.0156(15) 0.0211(15) 0.0011(11) 0.0007(12) -0.0037(12) C3 0.0297(16) 0.0205(16) 0.0264(17) -0.0031(13) 0.0014(13) -0.0048(13) C4 0.0251(16) 0.0216(16) 0.0328(18) 0.0038(14) 0.0007(14) -0.0014(13) C5 0.0294(17) 0.0271(18) 0.0259(17) 0.0034(13) -0.0043(13) -0.0040(13) C6 0.0328(17) 0.0231(17) 0.0225(16) -0.0031(13) 0.0003(13) -0.0075(13) C7 0.0285(16) 0.0150(15) 0.0224(16) 0.0003(12) -0.0013(12) -0.0057(12) C8 0.0279(16) 0.0162(16) 0.0218(16) -0.0013(12) 0.0002(13) -0.0053(12) C9 0.0299(16) 0.0151(16) 0.0224(16) 0.0008(11) 0.0020(13) -0.0033(12) C10 0.0343(17) 0.0199(17) 0.0247(16) 0.0000(13) 0.0027(13) 0.0012(13) C11 0.0336(17) 0.0251(18) 0.0316(18) 0.0021(14) 0.0012(14) 0.0041(14) C12 0.0351(18) 0.0278(19) 0.0241(18) 0.0049(13) -0.0054(14) 0.0002(14) C13 0.0345(17) 0.0192(16) 0.0235(16) 0.0007(12) -0.0018(13) -0.0030(13) C14 0.0289(16) 0.0166(15) 0.0221(16) 0.0014(12) -0.0007(12) -0.0048(12) C15 0.0268(16) 0.0295(18) 0.0314(18) -0.0003(14) -0.0084(14) -0.0035(14) C16 0.0323(17) 0.0185(16) 0.0330(18) -0.0021(13) -0.0028(14) -0.0027(13) C17 0.0306(17) 0.0165(16) 0.0370(19) -0.0055(14) -0.0042(14) -0.0013(13) C18 0.0374(18) 0.0233(18) 0.0326(18) 0.0052(14) -0.0002(14) -0.0044(14) _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 Br1 C1 1.918(3) . ? O1 C16 1.426(4) . ? O1 C15 1.429(4) . ? O1 Li1 2.035(6) . ? O2 C18 1.430(4) . ? O2 C17 1.436(4) . ? O2 Li1 1.997(6) . ? Li1 C8 2.257(6) . ? Li1 C8 2.361(6) 3_566 ? Li1 Li1 2.489(10) 3_566 ? C1 C2 1.391(4) . ? C1 C14 1.396(4) . ? C2 C3 1.429(4) . ? C2 C7 1.454(4) . ? C3 C4 1.354(4) . ? C3 H3 0.9500 . ? C4 C5 1.405(5) . ? C4 H4 0.9500 . ? C5 C6 1.365(5) . ? C5 H5 0.9500 . ? C6 C7 1.419(4) . ? C6 H6 0.9500 . ? C7 C8 1.424(4) . ? C8 C9 1.419(4) . ? C8 Li1 2.361(6) 3_566 ? C9 C10 1.433(4) . ? C9 C14 1.448(4) . ? C10 C11 1.351(4) . ? C10 H10 0.9500 . ? C11 C12 1.424(5) . ? C11 H11 0.9500 . ? C12 C13 1.350(5) . ? C12 H12 0.9500 . ? C13 C14 1.427(4) . ? C13 H13 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.510(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 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 C16 O1 C15 111.6(2) . . ? C16 O1 Li1 109.1(2) . . ? C15 O1 Li1 136.8(2) . . ? C18 O2 C17 113.6(2) . . ? C18 O2 Li1 124.0(2) . . ? C17 O2 Li1 102.4(2) . . ? O2 Li1 O1 85.2(2) . . ? O2 Li1 C8 117.6(3) . . ? O1 Li1 C8 126.9(3) . . ? O2 Li1 C8 103.5(2) . 3_566 ? O1 Li1 C8 103.4(2) . 3_566 ? C8 Li1 C8 114.8(2) . 3_566 ? O2 Li1 Li1 130.0(4) . 3_566 ? O1 Li1 Li1 139.9(4) . 3_566 ? C8 Li1 Li1 59.4(2) . 3_566 ? C8 Li1 Li1 55.4(2) 3_566 3_566 ? C2 C1 C14 122.6(3) . . ? C2 C1 Br1 118.2(2) . . ? C14 C1 Br1 119.3(2) . . ? C1 C2 C3 123.2(3) . . ? C1 C2 C7 117.5(3) . . ? C3 C2 C7 119.3(3) . . ? C4 C3 C2 120.9(3) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 120.8(3) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 119.6(3) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 123.4(3) . . ? C5 C6 H6 118.3 . . ? C7 C6 H6 118.3 . . ? C6 C7 C8 120.4(3) . . ? C6 C7 C2 115.8(3) . . ? C8 C7 C2 123.8(3) . . ? C9 C8 C7 114.1(3) . . ? C9 C8 Li1 123.5(3) . . ? C7 C8 Li1 117.3(3) . . ? C9 C8 Li1 107.6(2) . 3_566 ? C7 C8 Li1 119.2(2) . 3_566 ? Li1 C8 Li1 65.2(2) . 3_566 ? C8 C9 C10 120.1(3) . . ? C8 C9 C14 124.2(3) . . ? C10 C9 C14 115.7(3) . . ? C11 C10 C9 123.2(3) . . ? C11 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? C10 C11 C12 120.1(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 119.6(3) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C14 121.9(3) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C1 C14 C13 123.4(3) . . ? C1 C14 C9 117.4(3) . . ? C13 C14 C9 119.2(3) . . ? O1 C15 H15A 109.5 . . ? O1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O1 C16 C17 106.2(3) . . ? O1 C16 H16A 110.5 . . ? C17 C16 H16A 110.5 . . ? O1 C16 H16B 110.5 . . ? C17 C16 H16B 110.5 . . ? H16A C16 H16B 108.7 . . ? O2 C17 C16 110.7(3) . . ? O2 C17 H17A 109.5 . . ? C16 C17 H17A 109.5 . . ? O2 C17 H17B 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? O2 C18 H18A 109.5 . . ? O2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 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 C18 O2 Li1 O1 104.2(3) . . . . ? C17 O2 Li1 O1 -25.8(3) . . . . ? C18 O2 Li1 C8 -25.3(4) . . . . ? C17 O2 Li1 C8 -155.3(3) . . . . ? C18 O2 Li1 C8 -153.1(2) . . . 3_566 ? C17 O2 Li1 C8 76.9(3) . . . 3_566 ? C18 O2 Li1 Li1 -97.2(5) . . . 3_566 ? C17 O2 Li1 Li1 132.8(5) . . . 3_566 ? C16 O1 Li1 O2 -2.8(3) . . . . ? C15 O1 Li1 O2 -162.7(3) . . . . ? C16 O1 Li1 C8 118.4(3) . . . . ? C15 O1 Li1 C8 -41.4(5) . . . . ? C16 O1 Li1 C8 -105.6(2) . . . 3_566 ? C15 O1 Li1 C8 94.6(4) . . . 3_566 ? C16 O1 Li1 Li1 -157.1(5) . . . 3_566 ? C15 O1 Li1 Li1 43.1(8) . . . 3_566 ? C14 C1 C2 C3 -175.0(3) . . . . ? Br1 C1 C2 C3 5.0(4) . . . . ? C14 C1 C2 C7 5.4(4) . . . . ? Br1 C1 C2 C7 -174.5(2) . . . . ? C1 C2 C3 C4 -177.7(3) . . . . ? C7 C2 C3 C4 1.8(5) . . . . ? C2 C3 C4 C5 1.9(5) . . . . ? C3 C4 C5 C6 -2.5(5) . . . . ? C4 C5 C6 C7 -0.7(5) . . . . ? C5 C6 C7 C8 -175.3(3) . . . . ? C5 C6 C7 C2 4.2(4) . . . . ? C1 C2 C7 C6 174.9(3) . . . . ? C3 C2 C7 C6 -4.7(4) . . . . ? C1 C2 C7 C8 -5.7(4) . . . . ? C3 C2 C7 C8 174.8(3) . . . . ? C6 C7 C8 C9 179.9(3) . . . . ? C2 C7 C8 C9 0.4(4) . . . . ? C6 C7 C8 Li1 24.3(4) . . . . ? C2 C7 C8 Li1 -155.1(3) . . . . ? C6 C7 C8 Li1 -51.0(4) . . . 3_566 ? C2 C7 C8 Li1 129.5(3) . . . 3_566 ? O2 Li1 C8 C9 -26.8(4) . . . . ? O1 Li1 C8 C9 -132.7(3) . . . . ? C8 Li1 C8 C9 95.4(3) 3_566 . . . ? Li1 Li1 C8 C9 95.4(3) 3_566 . . . ? O2 Li1 C8 C7 126.3(3) . . . . ? O1 Li1 C8 C7 20.4(4) . . . . ? C8 Li1 C8 C7 -111.5(3) 3_566 . . . ? Li1 Li1 C8 C7 -111.5(3) 3_566 . . . ? O2 Li1 C8 Li1 -122.2(4) . . . 3_566 ? O1 Li1 C8 Li1 131.8(5) . . . 3_566 ? C8 Li1 C8 Li1 0.0 3_566 . . 3_566 ? C7 C8 C9 C10 -175.7(3) . . . . ? Li1 C8 C9 C10 -21.8(4) . . . . ? Li1 C8 C9 C10 49.6(3) 3_566 . . . ? C7 C8 C9 C14 5.3(4) . . . . ? Li1 C8 C9 C14 159.2(3) . . . . ? Li1 C8 C9 C14 -129.3(3) 3_566 . . . ? C8 C9 C10 C11 -176.0(3) . . . . ? C14 C9 C10 C11 3.0(4) . . . . ? C9 C10 C11 C12 1.2(5) . . . . ? C10 C11 C12 C13 -2.8(5) . . . . ? C11 C12 C13 C14 0.0(5) . . . . ? C2 C1 C14 C13 -179.1(3) . . . . ? Br1 C1 C14 C13 0.9(4) . . . . ? C2 C1 C14 C9 -0.2(4) . . . . ? Br1 C1 C14 C9 179.8(2) . . . . ? C12 C13 C14 C1 -176.7(3) . . . . ? C12 C13 C14 C9 4.4(5) . . . . ? C8 C9 C14 C1 -5.7(4) . . . . ? C10 C9 C14 C1 175.3(3) . . . . ? C8 C9 C14 C13 173.3(3) . . . . ? C10 C9 C14 C13 -5.7(4) . . . . ? C15 O1 C16 C17 -165.0(3) . . . . ? Li1 O1 C16 C17 29.7(3) . . . . ? C18 O2 C17 C16 -85.1(3) . . . . ? Li1 O2 C17 C16 51.0(3) . . . . ? O1 C16 C17 O2 -55.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.45 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.833 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.101 # Attachment '3_BrAnLi_LiBr_4THF.cif' data_3_BrAnLi_LiBr_4THF _database_code_depnum_ccdc_archive 'CCDC 766246' #TrackingRef '3_BrAnLi_LiBr_4THF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H104 Br5 Li5 O10' _chemical_formula_weight 1683.90 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' Br Br -0.2901 2.4595 '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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3818(18) _cell_length_b 14.470(3) _cell_length_c 28.554(5) _cell_angle_alpha 88.542(3) _cell_angle_beta 85.980(2) _cell_angle_gamma 89.426(3) _cell_volume 3865.5(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9891 _cell_measurement_theta_min 2.243 _cell_measurement_theta_max 25.095 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1732 _exptl_absorpt_coefficient_mu 2.657 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3301 _exptl_absorpt_correction_T_max 0.4286 _exptl_absorpt_process_details SADABS-2007/4 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'TXS Mo rotating anode' _diffrn_radiation_monochromator 'INCOATEC Helios mirror optics' _diffrn_measurement_device_type 'BRUKER TXS APEX2 with D8-Goniometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 57729 _diffrn_reflns_av_R_equivalents 0.0596 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.14 _reflns_number_total 13688 _reflns_number_gt 10759 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 2.2-0' _computing_cell_refinement 'SAINT V7.46A' _computing_data_reduction 'SAINT V7.46A' _computing_structure_solution 'SHELXS in SHELXTL v6.10' _computing_structure_refinement 'SHELXL in SHELXTL v6.10' _computing_molecular_graphics 'XP in SHELXTL v6.10' _computing_publication_material 'XP in SHELXTL v6.10' _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^)+(0.1116P)^2^+14.3246P] 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 13688 _refine_ls_number_parameters 1215 _refine_ls_number_restraints 1021 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.1937 _refine_ls_wR_factor_gt 0.1843 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.006 _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 Br1 Br 0.08664(6) 0.73957(6) 0.21256(2) 0.0378(2) Uani 1 1 d DU . . Br2 Br 0.60635(6) 0.74037(4) 0.452994(18) 0.02325(16) Uani 1 1 d U . . Br3 Br -0.10690(6) 0.75801(6) 0.83842(2) 0.0388(2) Uani 1 1 d U A . Br4 Br 0.37202(6) 0.76249(4) 0.554547(19) 0.02628(16) Uani 1 1 d U . . Li1 Li 0.4965(10) 0.6412(7) 0.3944(3) 0.024(2) Uani 1 1 d U . . Li2 Li 0.4876(10) 0.8305(7) 0.3906(3) 0.024(2) Uani 1 1 d U . . Li3 Li -0.1371(11) 0.7643(7) 0.7437(4) 0.029(2) Uani 1 1 d U . . Li4 Li -0.0033(13) 0.8471(8) 0.9012(3) 0.036(3) Uani 1 1 d U . . Li5 Li -0.0048(12) 0.6615(9) 0.9015(4) 0.038(3) Uani 1 1 d U . . O1 O 0.3719(5) 0.5535(3) 0.42990(16) 0.0423(12) Uani 1 1 d DU . . O2 O 0.6375(4) 0.5595(3) 0.36348(14) 0.0274(9) Uani 1 1 d U . . O3 O 0.3493(4) 0.9165(3) 0.42017(16) 0.0321(10) Uani 1 1 d U . . O4 O 0.6372(4) 0.9134(3) 0.36166(14) 0.0317(10) Uani 1 1 d U . . O5 O -0.2524(4) 0.8776(3) 0.74521(14) 0.0293(9) Uani 1 1 d U . . O6 O -0.2474(4) 0.6489(3) 0.74439(14) 0.0285(9) Uani 1 1 d U . . C1 C 0.2068(5) 0.7365(4) 0.26398(17) 0.0187(11) Uani 1 1 d DU . . C2 C 0.1428(5) 0.7344(4) 0.30962(18) 0.0177(11) Uani 1 1 d DU . . C3 C -0.0091(6) 0.7337(4) 0.3208(2) 0.0252(13) Uani 1 1 d DU . . H3 H -0.0713 0.7351 0.2959 0.030 Uiso 1 1 calc R . . C4 C -0.0654(6) 0.7311(4) 0.3654(2) 0.0268(13) Uani 1 1 d DU . . H4 H -0.1662 0.7315 0.3715 0.032 Uiso 1 1 calc R . . C5 C 0.0242(6) 0.7276(4) 0.4032(2) 0.0241(13) Uani 1 1 d DU . . H5 H -0.0164 0.7242 0.4346 0.029 Uiso 1 1 calc R . . C6 C 0.1692(6) 0.7292(4) 0.39453(18) 0.0222(12) Uani 1 1 d DU . . H6 H 0.2278 0.7280 0.4204 0.027 Uiso 1 1 calc R . . C7 C 0.2361(5) 0.7325(4) 0.34787(17) 0.0173(11) Uani 1 1 d DU . . C8 C 0.3852(5) 0.7338(3) 0.34072(16) 0.0083(9) Uani 1 1 d DU . . C9 C 0.4431(5) 0.7364(4) 0.29363(18) 0.0170(11) Uani 1 1 d DU . . C10 C 0.5946(5) 0.7372(4) 0.28344(19) 0.0225(12) Uani 1 1 d DU . . H10 H 0.6549 0.7362 0.3088 0.027 Uiso 1 1 calc R . . C11 C 0.6558(6) 0.7395(4) 0.23874(19) 0.0237(12) Uani 1 1 d DU . . H11 H 0.7568 0.7410 0.2333 0.028 Uiso 1 1 calc R . . C12 C 0.5675(6) 0.7396(4) 0.20050(19) 0.0242(12) Uani 1 1 d DU . . H12 H 0.6096 0.7403 0.1693 0.029 Uiso 1 1 calc R . . C13 C 0.4225(6) 0.7386(4) 0.20820(18) 0.0210(12) Uani 1 1 d DU . . H13 H 0.3653 0.7396 0.1820 0.025 Uiso 1 1 calc R . . C14 C 0.3545(5) 0.7362(4) 0.25416(18) 0.0170(11) Uani 1 1 d DU . . C15 C 0.2833(11) 0.4936(6) 0.4053(3) 0.067(3) Uani 1 1 d DU . . H15A H 0.3329 0.4340 0.3990 0.080 Uiso 1 1 calc R . . H15B H 0.2598 0.5226 0.3750 0.080 Uiso 1 1 calc R . . C16 C 0.1510(9) 0.4788(6) 0.4366(3) 0.058(2) Uani 1 1 d DU . . H16A H 0.1090 0.4174 0.4321 0.069 Uiso 1 1 calc R . . H16B H 0.0785 0.5275 0.4314 0.069 Uiso 1 1 calc R . . C17 C 0.2078(9) 0.4850(6) 0.4842(3) 0.055(2) Uani 1 1 d DU . . H17A H 0.1315 0.5044 0.5078 0.066 Uiso 1 1 calc R . . H17B H 0.2471 0.4246 0.4944 0.066 Uiso 1 1 calc R . . C18 C 0.3201(9) 0.5543(6) 0.4786(2) 0.055(2) Uani 1 1 d DU . . H18A H 0.2814 0.6161 0.4869 0.066 Uiso 1 1 calc R . . H18B H 0.3982 0.5387 0.4990 0.066 Uiso 1 1 calc R . . C19 C 0.7443(7) 0.5140(5) 0.3897(2) 0.0341(15) Uani 1 1 d U . . H19A H 0.7033 0.4597 0.4074 0.041 Uiso 1 1 calc R . . H19B H 0.7821 0.5568 0.4123 0.041 Uiso 1 1 calc R . . C20 C 0.8620(7) 0.4841(4) 0.3540(2) 0.0311(14) Uani 1 1 d U . . H20A H 0.8925 0.4196 0.3604 0.037 Uiso 1 1 calc R . . H20B H 0.9458 0.5251 0.3543 0.037 Uiso 1 1 calc R . . C21 C 0.7936(7) 0.4925(5) 0.3072(2) 0.0337(15) Uani 1 1 d U . . H21A H 0.8342 0.5452 0.2880 0.040 Uiso 1 1 calc R . . H21B H 0.8086 0.4352 0.2892 0.040 Uiso 1 1 calc R . . C22 C 0.6374(7) 0.5082(5) 0.3203(2) 0.0326(15) Uani 1 1 d U . . H22A H 0.5918 0.5446 0.2956 0.039 Uiso 1 1 calc R . . H22B H 0.5867 0.4488 0.3257 0.039 Uiso 1 1 calc R . . C23 C 0.2206(7) 0.9588(4) 0.4055(2) 0.0304(14) Uani 1 1 d U . . H23A H 0.1735 0.9183 0.3839 0.036 Uiso 1 1 calc R . . H23B H 0.2413 1.0189 0.3893 0.036 Uiso 1 1 calc R . . C24 C 0.1283(7) 0.9719(5) 0.4494(2) 0.0351(15) Uani 1 1 d U . . H24A H 0.0697 0.9165 0.4574 0.042 Uiso 1 1 calc R . . H24B H 0.0643 1.0263 0.4463 0.042 Uiso 1 1 calc R . . C25 C 0.2362(8) 0.9874(5) 0.4863(2) 0.0394(17) Uani 1 1 d U . . H25A H 0.2329 1.0522 0.4966 0.047 Uiso 1 1 calc R . . H25B H 0.2172 0.9456 0.5140 0.047 Uiso 1 1 calc R . . C26 C 0.3795(8) 0.9648(5) 0.4606(3) 0.0439(18) Uani 1 1 d U . . H26A H 0.4320 1.0223 0.4517 0.053 Uiso 1 1 calc R . . H26B H 0.4385 0.9261 0.4810 0.053 Uiso 1 1 calc R . . C27 C 0.7426(8) 0.9546(5) 0.3885(2) 0.0400(17) Uani 1 1 d U . . H27A H 0.7763 0.9096 0.4120 0.048 Uiso 1 1 calc R . . H27B H 0.7019 1.0091 0.4051 0.048 Uiso 1 1 calc R . . C28 C 0.8641(7) 0.9830(5) 0.3540(2) 0.0348(15) Uani 1 1 d U . . H28A H 0.9459 0.9396 0.3557 0.042 Uiso 1 1 calc R . . H28B H 0.8965 1.0462 0.3602 0.042 Uiso 1 1 calc R . . C29 C 0.7997(7) 0.9795(5) 0.3058(2) 0.0366(16) Uani 1 1 d U . . H29A H 0.8164 1.0380 0.2876 0.044 Uiso 1 1 calc R . . H29B H 0.8407 0.9275 0.2873 0.044 Uiso 1 1 calc R . . C30 C 0.6415(7) 0.9654(5) 0.3187(2) 0.0324(14) Uani 1 1 d U . . H30A H 0.5913 1.0254 0.3228 0.039 Uiso 1 1 calc R . . H30B H 0.5968 0.9309 0.2941 0.039 Uiso 1 1 calc R . . Br5 Br 0.39739(14) 0.80043(10) 1.07762(4) 0.0370(4) Uani 0.505(2) 1 d PDU A 1 C31 C 0.2794(10) 0.7815(10) 1.0271(3) 0.025(3) Uani 0.505(2) 1 d PDU A 1 C32 C 0.3437(9) 0.7852(9) 0.9811(3) 0.018(2) Uani 0.505(2) 1 d PDU A 1 C33 C 0.4923(10) 0.8041(8) 0.9693(3) 0.023(2) Uani 0.505(2) 1 d PDU A 1 H33 H 0.5531 0.8169 0.9935 0.028 Uiso 0.505(2) 1 calc PR A 1 C34 C 0.5462(12) 0.8039(9) 0.9244(4) 0.036(3) Uani 0.505(2) 1 d PDU A 1 H34 H 0.6444 0.8174 0.9175 0.043 Uiso 0.505(2) 1 calc PR A 1 C35 C 0.4615(12) 0.7842(12) 0.8878(4) 0.030(3) Uani 0.505(2) 1 d PDU A 1 H35 H 0.5022 0.7840 0.8563 0.036 Uiso 0.505(2) 1 calc PR A 1 C36 C 0.3195(13) 0.765(4) 0.8972(5) 0.025(8) Uani 0.505(2) 1 d PDU A 1 H36 H 0.2635 0.7510 0.8719 0.030 Uiso 0.505(2) 1 calc PR A 1 C37 C 0.2529(11) 0.7658(18) 0.9435(4) 0.023(7) Uani 0.505(2) 1 d PDU A 1 C38 C 0.1034(6) 0.7520(4) 0.95017(18) 0.0232(12) Uani 0.505(2) 1 d PDU A 1 C39 C 0.0491(14) 0.745(5) 0.9980(4) 0.019(3) Uani 0.505(2) 1 d PDU A 1 C40 C -0.1010(15) 0.7295(12) 1.0086(6) 0.025(5) Uani 0.505(2) 1 d PDU A 1 H40 H -0.1603 0.7198 0.9835 0.030 Uiso 0.505(2) 1 calc PR A 1 C41 C -0.1607(19) 0.7283(15) 1.0535(6) 0.028(6) Uani 0.505(2) 1 d PDU A 1 H41 H -0.2604 0.7185 1.0594 0.034 Uiso 0.505(2) 1 calc PR A 1 C42 C -0.074(2) 0.742(6) 1.0913(7) 0.032(4) Uani 0.505(2) 1 d PDU A 1 H42 H -0.1155 0.7382 1.1226 0.039 Uiso 0.505(2) 1 calc PR A 1 C43 C 0.068(2) 0.759(3) 1.0832(6) 0.037(10) Uani 0.505(2) 1 d PDU A 1 H43 H 0.1235 0.7686 1.1091 0.044 Uiso 0.505(2) 1 calc PR A 1 C44 C 0.1342(13) 0.764(3) 1.0369(5) 0.034(10) Uani 0.505(2) 1 d PDU A 1 Br5' Br 0.39885(14) 0.69273(10) 1.07780(4) 0.0364(4) Uani 0.495(2) 1 d PDU A 2 C31' C 0.2789(10) 0.7149(9) 1.0271(3) 0.019(2) Uani 0.495(2) 1 d PDU A 2 C32' C 0.3447(10) 0.7163(9) 0.9815(3) 0.019(2) Uani 0.495(2) 1 d PDU A 2 C33' C 0.4927(10) 0.6998(8) 0.9695(4) 0.024(3) Uani 0.495(2) 1 d PDU A 2 H33' H 0.5543 0.6852 0.9937 0.028 Uiso 0.495(2) 1 calc PR A 2 C34' C 0.5470(11) 0.7044(9) 0.9246(4) 0.030(3) Uani 0.495(2) 1 d PDU A 2 H34' H 0.6464 0.6938 0.9179 0.036 Uiso 0.495(2) 1 calc PR A 2 C35' C 0.4611(12) 0.7242(12) 0.8878(4) 0.029(3) Uani 0.495(2) 1 d PDU A 2 H35' H 0.5014 0.7260 0.8563 0.034 Uiso 0.495(2) 1 calc PR A 2 C36' C 0.3181(15) 0.741(4) 0.8972(5) 0.036(12) Uani 0.495(2) 1 d PDU A 2 H36' H 0.2612 0.7568 0.8718 0.043 Uiso 0.495(2) 1 calc PR A 2 C37' C 0.2521(11) 0.7360(18) 0.9436(4) 0.016(5) Uani 0.495(2) 1 d PDU A 2 C38' C 0.1034(6) 0.7520(4) 0.95017(18) 0.0232(12) Uani 0.495(2) 1 d PDU A 2 C39' C 0.0480(14) 0.754(5) 0.9980(4) 0.019(3) Uani 0.495(2) 1 d PDU A 2 C40' C -0.1027(14) 0.7665(12) 1.0087(6) 0.020(4) Uani 0.495(2) 1 d PDU A 2 H40' H -0.1630 0.7764 0.9836 0.024 Uiso 0.495(2) 1 calc PR A 2 C41' C -0.162(2) 0.7650(16) 1.0538(7) 0.035(7) Uani 0.495(2) 1 d PDU A 2 H41' H -0.2622 0.7741 1.0597 0.042 Uiso 0.495(2) 1 calc PR A 2 C42' C -0.075(2) 0.750(6) 1.0916(7) 0.032(4) Uani 0.495(2) 1 d PDU A 2 H42' H -0.1156 0.7512 1.1229 0.039 Uiso 0.495(2) 1 calc PR A 2 C43' C 0.068(2) 0.733(3) 1.0835(5) 0.032(9) Uani 0.495(2) 1 d PDU A 2 H43' H 0.1239 0.7197 1.1094 0.038 Uiso 0.495(2) 1 calc PR A 2 C44' C 0.1346(13) 0.736(3) 1.0372(5) 0.027(8) Uani 0.495(2) 1 d PDU A 2 C45 C 0.2295(6) 0.7653(4) 0.60583(18) 0.0190(11) Uani 1 1 d U . . C46 C 0.2725(6) 0.7649(4) 0.65155(19) 0.0197(11) Uani 1 1 d U . . C47 C 0.4186(6) 0.7633(4) 0.6625(2) 0.0228(12) Uani 1 1 d U . . H47 H 0.4913 0.7629 0.6376 0.027 Uiso 1 1 calc R . . C48 C 0.4567(6) 0.7623(4) 0.7076(2) 0.0274(13) Uani 1 1 d U . . H48 H 0.5549 0.7619 0.7138 0.033 Uiso 1 1 calc R . . C49 C 0.3499(6) 0.7619(4) 0.7456(2) 0.0286(14) Uani 1 1 d U . . H49 H 0.3760 0.7600 0.7771 0.034 Uiso 1 1 calc R . . C50 C 0.2103(6) 0.7644(4) 0.73593(19) 0.0225(12) Uani 1 1 d U . . H50 H 0.1405 0.7654 0.7617 0.027 Uiso 1 1 calc R . . C51 C 0.1613(6) 0.7656(4) 0.6895(2) 0.0200(12) Uani 1 1 d U . . C52 C 0.0134(6) 0.7671(4) 0.68344(19) 0.0197(11) Uani 1 1 d U . . C53 C -0.0201(6) 0.7689(4) 0.63580(19) 0.0189(11) Uani 1 1 d U . . C54 C -0.1665(6) 0.7707(4) 0.6245(2) 0.0218(12) Uani 1 1 d U . . H54 H -0.2390 0.7707 0.6495 0.026 Uiso 1 1 calc R . . C55 C -0.2059(7) 0.7723(4) 0.5801(2) 0.0263(13) Uani 1 1 d U . . H55 H -0.3045 0.7746 0.5746 0.032 Uiso 1 1 calc R . . C56 C -0.1032(6) 0.7707(4) 0.5417(2) 0.0234(12) Uani 1 1 d U . . H56 H -0.1324 0.7707 0.5105 0.028 Uiso 1 1 calc R . . C57 C 0.0377(6) 0.7692(4) 0.54965(19) 0.0208(12) Uani 1 1 d U . . H57 H 0.1066 0.7691 0.5236 0.025 Uiso 1 1 calc R . . C58 C 0.0852(5) 0.7678(4) 0.59596(19) 0.0177(11) Uani 1 1 d U . . C59 C -0.2390(8) 0.9416(5) 0.7064(2) 0.0382(16) Uani 1 1 d U . . H59A H -0.3203 0.9359 0.6864 0.046 Uiso 1 1 calc R . . H59B H -0.1490 0.9304 0.6871 0.046 Uiso 1 1 calc R . . C60 C -0.2384(9) 1.0358(5) 0.7275(3) 0.050(2) Uani 1 1 d U . . H60A H -0.2878 1.0818 0.7079 0.060 Uiso 1 1 calc R . . H60B H -0.1396 1.0566 0.7309 0.060 Uiso 1 1 calc R . . C61 C -0.3186(10) 1.0214(6) 0.7751(3) 0.060(2) Uani 1 1 d U . . H61A H -0.2592 1.0399 0.8005 0.072 Uiso 1 1 calc R . . H61B H -0.4082 1.0583 0.7770 0.072 Uiso 1 1 calc R . . C62 C -0.3505(7) 0.9202(5) 0.7790(2) 0.0329(15) Uani 1 1 d U . . H62A H -0.3359 0.8959 0.8111 0.039 Uiso 1 1 calc R . . H62B H -0.4504 0.9085 0.7719 0.039 Uiso 1 1 calc R . . C71 C -0.3431(7) 0.6025(5) 0.7784(2) 0.0350(15) Uani 1 1 d U . . H71A H -0.4437 0.6154 0.7718 0.042 Uiso 1 1 calc R . . H71B H -0.3278 0.6232 0.8105 0.042 Uiso 1 1 calc R . . C72 C -0.3102(11) 0.5012(5) 0.7744(3) 0.058(2) Uani 1 1 d U . . H72A H -0.3992 0.4647 0.7761 0.070 Uiso 1 1 calc R . . H72B H -0.2503 0.4794 0.7997 0.070 Uiso 1 1 calc R . . C73 C -0.2302(8) 0.4925(5) 0.7268(3) 0.0454(19) Uani 1 1 d U . . H73A H -0.1307 0.4713 0.7300 0.054 Uiso 1 1 calc R . . H73B H -0.2782 0.4484 0.7072 0.054 Uiso 1 1 calc R . . C74 C -0.2338(8) 0.5891(5) 0.7056(2) 0.0385(16) Uani 1 1 d U . . H74A H -0.1447 0.6020 0.6859 0.046 Uiso 1 1 calc R . . H74B H -0.3160 0.5970 0.6859 0.046 Uiso 1 1 calc R . . O7 O 0.1494(15) 0.5738(14) 0.8681(6) 0.034(4) Uani 0.505(2) 1 d PDU A 1 C80 C 0.2488(17) 0.5188(14) 0.8933(6) 0.038(5) Uani 0.505(2) 1 d PDU A 1 H80A H 0.2027 0.4620 0.9070 0.046 Uiso 0.505(2) 1 calc PR A 1 H80B H 0.2863 0.5543 0.9189 0.046 Uiso 0.505(2) 1 calc PR A 1 C81 C 0.366(2) 0.495(2) 0.8570(7) 0.073(8) Uani 0.505(2) 1 d PDU A 1 H81A H 0.4401 0.5439 0.8542 0.087 Uiso 0.505(2) 1 calc PR A 1 H81B H 0.4114 0.4351 0.8643 0.087 Uiso 0.505(2) 1 calc PR A 1 C82 C 0.287(3) 0.491(3) 0.8134(8) 0.080(12) Uani 0.505(2) 1 d PDU A 1 H82A H 0.3453 0.5182 0.7864 0.096 Uiso 0.505(2) 1 calc PR A 1 H82B H 0.2659 0.4263 0.8066 0.096 Uiso 0.505(2) 1 calc PR A 1 C83 C 0.154(3) 0.543(2) 0.8205(7) 0.052(9) Uani 0.505(2) 1 d PDU A 1 H83A H 0.1528 0.5966 0.7982 0.062 Uiso 0.505(2) 1 calc PR A 1 H83B H 0.0714 0.5034 0.8159 0.062 Uiso 0.505(2) 1 calc PR A 1 O7' O 0.0928(17) 0.5734(14) 0.8711(6) 0.040(5) Uani 0.495(2) 1 d PDU A 2 C80' C 0.173(2) 0.5094(13) 0.8988(5) 0.048(5) Uani 0.495(2) 1 d PDU A 2 H80C H 0.1113 0.4579 0.9111 0.058 Uiso 0.495(2) 1 calc PR A 2 H80D H 0.2101 0.5410 0.9257 0.058 Uiso 0.495(2) 1 calc PR A 2 C81' C 0.294(2) 0.4736(14) 0.8673(7) 0.050(5) Uani 0.495(2) 1 d PDU A 2 H81C H 0.3164 0.4082 0.8750 0.060 Uiso 0.495(2) 1 calc PR A 2 H81D H 0.3806 0.5113 0.8687 0.060 Uiso 0.495(2) 1 calc PR A 2 C82' C 0.231(3) 0.484(2) 0.8202(6) 0.068(9) Uani 0.495(2) 1 d PDU A 2 H82C H 0.3078 0.4875 0.7945 0.082 Uiso 0.495(2) 1 calc PR A 2 H82D H 0.1688 0.4309 0.8147 0.082 Uiso 0.495(2) 1 calc PR A 2 C83' C 0.149(4) 0.570(2) 0.8228(7) 0.060(10) Uani 0.495(2) 1 d PDU A 2 H83C H 0.2105 0.6236 0.8144 0.072 Uiso 0.495(2) 1 calc PR A 2 H83D H 0.0702 0.5691 0.8014 0.072 Uiso 0.495(2) 1 calc PR A 2 O8 O -0.1234(12) 0.5560(8) 0.9249(4) 0.037(2) Uani 0.505(2) 1 d PU A 1 C84 C -0.1741(19) 0.5014(12) 0.8886(6) 0.061(4) Uani 0.505(2) 1 d PU A 1 H84A H -0.1054 0.4510 0.8804 0.073 Uiso 0.505(2) 1 calc PR A 1 H84B H -0.1869 0.5400 0.8601 0.073 Uiso 0.505(2) 1 calc PR A 1 C85 C -0.3097(19) 0.4636(14) 0.9070(8) 0.075(5) Uani 0.505(2) 1 d PU A 1 H85A H -0.3201 0.3991 0.8972 0.091 Uiso 0.505(2) 1 calc PR A 1 H85B H -0.3904 0.5011 0.8962 0.091 Uiso 0.505(2) 1 calc PR A 1 C86 C -0.3042(19) 0.4678(13) 0.9585(8) 0.077(5) Uani 0.505(2) 1 d PU A 1 H86A H -0.3194 0.4058 0.9733 0.092 Uiso 0.505(2) 1 calc PR A 1 H86B H -0.3789 0.5104 0.9718 0.092 Uiso 0.505(2) 1 calc PR A 1 C87 C -0.154(2) 0.5036(13) 0.9670(7) 0.052(5) Uani 0.505(2) 1 d PU A 1 H87A H -0.1557 0.5427 0.9950 0.063 Uiso 0.505(2) 1 calc PR A 1 H87B H -0.0847 0.4522 0.9704 0.063 Uiso 0.505(2) 1 calc PR A 1 O8' O -0.1738(10) 0.6021(8) 0.9349(3) 0.032(2) Uani 0.495(2) 1 d PU A 2 C84' C -0.2993(13) 0.5754(10) 0.9120(5) 0.032(3) Uani 0.495(2) 1 d PU A 2 H84C H -0.2804 0.5181 0.8943 0.039 Uiso 0.495(2) 1 calc PR A 2 H84D H -0.3283 0.6250 0.8901 0.039 Uiso 0.495(2) 1 calc PR A 2 C85' C -0.4142(15) 0.5596(10) 0.9511(4) 0.035(3) Uani 0.495(2) 1 d PU A 2 H85C H -0.4683 0.5028 0.9459 0.042 Uiso 0.495(2) 1 calc PR A 2 H85D H -0.4817 0.6126 0.9530 0.042 Uiso 0.495(2) 1 calc PR A 2 C86' C -0.3323(13) 0.5495(11) 0.9969(4) 0.036(3) Uani 0.495(2) 1 d PU A 2 H86C H -0.3518 0.6027 1.0176 0.043 Uiso 0.495(2) 1 calc PR A 2 H86D H -0.3581 0.4916 1.0145 0.043 Uiso 0.495(2) 1 calc PR A 2 C87' C -0.1772(15) 0.5476(12) 0.9773(5) 0.029(3) Uani 0.495(2) 1 d PU A 2 H87C H -0.1143 0.5743 0.9998 0.035 Uiso 0.495(2) 1 calc PR A 2 H87D H -0.1454 0.4835 0.9709 0.035 Uiso 0.495(2) 1 calc PR A 2 O9 O -0.1746(10) 0.9055(8) 0.9353(3) 0.031(2) Uani 0.505(2) 1 d PU A 1 C88 C -0.3029(14) 0.9331(11) 0.9133(5) 0.041(3) Uani 0.505(2) 1 d PU A 1 H88A H -0.3319 0.8848 0.8921 0.049 Uiso 0.505(2) 1 calc PR A 1 H88B H -0.2876 0.9915 0.8949 0.049 Uiso 0.505(2) 1 calc PR A 1 C89 C -0.4145(14) 0.9460(10) 0.9528(4) 0.035(3) Uani 0.505(2) 1 d PU A 1 H89A H -0.4805 0.8928 0.9557 0.043 Uiso 0.505(2) 1 calc PR A 1 H89B H -0.4706 1.0033 0.9479 0.043 Uiso 0.505(2) 1 calc PR A 1 C90 C -0.3288(14) 0.9523(10) 0.9966(4) 0.037(3) Uani 0.505(2) 1 d PU A 1 H90A H -0.3542 1.0091 1.0140 0.045 Uiso 0.505(2) 1 calc PR A 1 H90B H -0.3463 0.8979 1.0179 0.045 Uiso 0.505(2) 1 calc PR A 1 C91 C -0.1773(17) 0.9545(12) 0.9771(6) 0.037(4) Uani 0.505(2) 1 d PU A 1 H91A H -0.1459 1.0190 0.9707 0.044 Uiso 0.505(2) 1 calc PR A 1 H91B H -0.1137 0.9247 0.9993 0.044 Uiso 0.505(2) 1 calc PR A 1 O9' O -0.1216(11) 0.9521(9) 0.9246(4) 0.037(2) Uani 0.495(2) 1 d PU A 2 C88' C -0.173(2) 1.0113(13) 0.8879(7) 0.067(5) Uani 0.495(2) 1 d PU A 2 H88C H -0.1838 0.9760 0.8592 0.080 Uiso 0.495(2) 1 calc PR A 2 H88D H -0.1060 1.0628 0.8803 0.080 Uiso 0.495(2) 1 calc PR A 2 C89' C -0.313(2) 1.0471(14) 0.9069(9) 0.080(6) Uani 0.495(2) 1 d PU A 2 H89C H -0.3921 1.0104 0.8958 0.096 Uiso 0.495(2) 1 calc PR A 2 H89D H -0.3263 1.1126 0.8971 0.096 Uiso 0.495(2) 1 calc PR A 2 C90' C -0.309(2) 1.0381(12) 0.9578(9) 0.081(6) Uani 0.495(2) 1 d PU A 2 H90C H -0.3820 0.9937 0.9709 0.097 Uiso 0.495(2) 1 calc PR A 2 H90D H -0.3273 1.0986 0.9726 0.097 Uiso 0.495(2) 1 calc PR A 2 C91' C -0.157(2) 1.0023(15) 0.9659(7) 0.056(5) Uani 0.495(2) 1 d PU A 2 H91C H -0.0900 1.0540 0.9689 0.067 Uiso 0.495(2) 1 calc PR A 2 H91D H -0.1564 0.9617 0.9944 0.067 Uiso 0.495(2) 1 calc PR A 2 O10 O 0.0915(13) 0.9394(10) 0.8707(5) 0.032(3) Uani 0.505(2) 1 d PDU A 1 C92 C 0.173(3) 0.9967(15) 0.8988(6) 0.054(6) Uani 0.505(2) 1 d PDU A 1 H92A H 0.2153 0.9593 0.9240 0.065 Uiso 0.505(2) 1 calc PR A 1 H92B H 0.1122 1.0457 0.9134 0.065 Uiso 0.505(2) 1 calc PR A 1 C93 C 0.289(2) 1.0383(14) 0.8663(8) 0.052(6) Uani 0.505(2) 1 d PDU A 1 H93A H 0.3758 0.9991 0.8650 0.063 Uiso 0.505(2) 1 calc PR A 1 H93B H 0.3130 1.1010 0.8762 0.063 Uiso 0.505(2) 1 calc PR A 1 C94 C 0.223(3) 1.0417(18) 0.8204(7) 0.056(7) Uani 0.505(2) 1 d PDU A 1 H94A H 0.1731 1.1015 0.8156 0.067 Uiso 0.505(2) 1 calc PR A 1 H94B H 0.2963 1.0333 0.7942 0.067 Uiso 0.505(2) 1 calc PR A 1 C95 C 0.125(2) 0.9682(18) 0.8232(6) 0.058(9) Uani 0.505(2) 1 d PDU A 1 H95A H 0.1668 0.9154 0.8054 0.070 Uiso 0.505(2) 1 calc PR A 1 H95B H 0.0366 0.9880 0.8088 0.070 Uiso 0.505(2) 1 calc PR A 1 O10' O 0.1522(12) 0.9341(10) 0.8700(5) 0.027(3) Uani 0.495(2) 1 d PDU A 2 C92' C 0.2427(18) 0.9887(15) 0.8963(6) 0.036(5) Uani 0.495(2) 1 d PDU A 2 H92C H 0.2901 0.9497 0.9197 0.043 Uiso 0.495(2) 1 calc PR A 2 H92D H 0.1867 1.0377 0.9130 0.043 Uiso 0.495(2) 1 calc PR A 2 C93' C 0.351(2) 1.030(2) 0.8612(8) 0.075(10) Uani 0.495(2) 1 d PDU A 2 H93C H 0.4387 0.9919 0.8584 0.090 Uiso 0.495(2) 1 calc PR A 2 H93D H 0.3754 1.0936 0.8698 0.090 Uiso 0.495(2) 1 calc PR A 2 C94' C 0.275(3) 1.031(2) 0.8168(9) 0.079(14) Uani 0.495(2) 1 d PDU A 2 H94C H 0.2238 1.0901 0.8125 0.095 Uiso 0.495(2) 1 calc PR A 2 H94D H 0.3444 1.0221 0.7894 0.095 Uiso 0.495(2) 1 calc PR A 2 C95' C 0.179(2) 0.9569(15) 0.8215(5) 0.037(6) Uani 0.495(2) 1 d PDU A 2 H95C H 0.2192 0.9026 0.8047 0.045 Uiso 0.495(2) 1 calc PR A 2 H95D H 0.0880 0.9748 0.8078 0.045 Uiso 0.495(2) 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 Br1 0.0189(3) 0.0767(5) 0.0183(3) 0.0004(3) -0.0052(2) 0.0009(3) Br2 0.0157(3) 0.0400(4) 0.0142(3) -0.0019(2) -0.0015(2) 0.0009(2) Br3 0.0207(3) 0.0836(6) 0.0123(3) -0.0003(3) -0.0026(2) 0.0007(3) Br4 0.0153(3) 0.0446(4) 0.0180(3) 0.0004(2) 0.0044(2) 0.0007(2) Li1 0.017(5) 0.032(5) 0.023(5) 0.001(4) -0.001(4) -0.003(4) Li2 0.017(5) 0.024(5) 0.031(5) -0.003(4) -0.002(4) -0.003(4) Li3 0.023(5) 0.035(6) 0.030(5) -0.001(4) -0.006(4) -0.001(4) Li4 0.049(7) 0.044(7) 0.014(5) 0.000(4) -0.003(4) 0.023(5) Li5 0.039(6) 0.058(8) 0.018(5) 0.002(5) -0.003(4) -0.022(5) O1 0.050(3) 0.037(3) 0.038(3) -0.009(2) 0.018(2) -0.019(2) O2 0.028(2) 0.037(2) 0.017(2) -0.0051(17) 0.0011(17) 0.0085(18) O3 0.023(2) 0.037(3) 0.036(2) -0.016(2) -0.0013(18) 0.0072(18) O4 0.027(2) 0.047(3) 0.022(2) -0.0014(19) -0.0009(17) -0.0151(19) O5 0.031(2) 0.034(2) 0.022(2) 0.0033(18) 0.0038(17) 0.0042(18) O6 0.031(2) 0.036(2) 0.017(2) -0.0011(17) 0.0037(17) -0.0010(19) C1 0.012(3) 0.031(3) 0.013(3) 0.001(2) -0.003(2) 0.001(2) C2 0.011(3) 0.024(3) 0.018(3) -0.005(2) 0.004(2) 0.001(2) C3 0.013(3) 0.039(4) 0.023(3) -0.002(3) 0.000(2) 0.000(2) C4 0.013(3) 0.037(4) 0.029(3) -0.002(3) 0.008(2) -0.002(2) C5 0.021(3) 0.026(3) 0.023(3) -0.002(2) 0.009(2) 0.002(2) C6 0.016(3) 0.035(3) 0.014(3) -0.005(2) 0.002(2) -0.001(2) C7 0.015(3) 0.021(3) 0.015(3) -0.004(2) 0.004(2) 0.000(2) C8 0.006(2) 0.008(2) 0.010(2) -0.0022(18) 0.0044(18) -0.0013(17) C9 0.009(2) 0.023(3) 0.018(3) -0.001(2) 0.002(2) 0.000(2) C10 0.011(3) 0.036(3) 0.021(3) -0.001(2) -0.002(2) 0.000(2) C11 0.013(3) 0.035(3) 0.023(3) -0.006(2) 0.002(2) -0.002(2) C12 0.024(3) 0.033(3) 0.015(3) 0.001(2) 0.005(2) 0.003(2) C13 0.018(3) 0.030(3) 0.015(3) 0.001(2) -0.002(2) 0.000(2) C14 0.014(3) 0.019(3) 0.018(3) -0.004(2) 0.001(2) 0.001(2) C15 0.118(8) 0.046(5) 0.035(4) -0.013(4) 0.016(5) -0.044(5) C16 0.055(5) 0.040(4) 0.082(6) 0.023(4) -0.031(5) -0.020(4) C17 0.051(5) 0.072(6) 0.040(4) 0.007(4) 0.008(4) -0.007(4) C18 0.060(5) 0.074(6) 0.031(4) 0.002(4) -0.005(4) -0.011(4) C19 0.044(4) 0.039(4) 0.020(3) 0.001(3) -0.004(3) 0.012(3) C20 0.034(4) 0.028(3) 0.031(3) 0.000(3) -0.004(3) 0.011(3) C21 0.044(4) 0.030(4) 0.026(3) -0.008(3) 0.002(3) 0.007(3) C22 0.044(4) 0.032(4) 0.023(3) -0.006(3) -0.007(3) 0.002(3) C23 0.040(4) 0.026(3) 0.025(3) 0.001(3) -0.004(3) 0.009(3) C24 0.035(4) 0.033(4) 0.038(4) -0.007(3) -0.004(3) 0.007(3) C25 0.065(5) 0.033(4) 0.021(3) -0.002(3) -0.008(3) 0.015(3) C26 0.047(4) 0.036(4) 0.051(5) -0.016(3) -0.023(4) 0.007(3) C27 0.048(4) 0.051(4) 0.023(3) -0.001(3) -0.007(3) -0.023(3) C28 0.031(4) 0.037(4) 0.038(4) 0.004(3) -0.007(3) -0.009(3) C29 0.042(4) 0.040(4) 0.027(3) 0.000(3) 0.007(3) -0.011(3) C30 0.037(4) 0.031(4) 0.031(3) 0.005(3) -0.010(3) 0.006(3) Br5 0.0288(7) 0.0593(10) 0.0238(7) -0.0012(6) -0.0079(5) -0.0069(6) C31 0.021(6) 0.036(8) 0.020(6) 0.000(5) -0.011(5) -0.003(5) C32 0.016(5) 0.034(8) 0.005(5) 0.000(5) -0.007(4) 0.000(5) C33 0.024(6) 0.032(7) 0.015(5) -0.005(5) -0.006(4) 0.000(5) C34 0.028(7) 0.043(8) 0.035(7) 0.006(6) 0.005(6) -0.018(6) C35 0.029(7) 0.048(9) 0.012(6) 0.009(6) -0.001(5) 0.000(7) C36 0.013(10) 0.05(2) 0.013(10) 0.010(8) -0.001(7) -0.005(6) C37 0.018(8) 0.023(16) 0.028(9) 0.008(6) -0.002(6) -0.007(5) C38 0.016(3) 0.034(3) 0.019(3) 0.004(2) -0.003(2) 0.002(2) C39 0.018(3) 0.023(10) 0.017(3) 0.001(2) 0.000(2) 0.001(2) C40 0.025(7) 0.019(11) 0.032(8) 0.005(7) -0.007(6) -0.001(6) C41 0.016(7) 0.046(16) 0.021(8) 0.012(8) 0.003(5) -0.005(8) C42 0.031(4) 0.048(11) 0.017(3) 0.000(3) 0.007(3) -0.002(3) C43 0.033(12) 0.05(2) 0.025(11) 0.004(7) -0.007(9) -0.001(8) C44 0.023(10) 0.07(3) 0.012(9) 0.006(7) 0.003(7) -0.005(7) Br5' 0.0301(7) 0.0557(10) 0.0241(7) 0.0018(6) -0.0092(5) 0.0085(6) C31' 0.012(5) 0.024(7) 0.021(6) 0.002(5) -0.005(4) -0.001(5) C32' 0.015(6) 0.019(7) 0.025(6) 0.001(5) -0.008(4) 0.004(5) C33' 0.015(5) 0.032(7) 0.025(6) -0.002(5) -0.009(5) 0.012(5) C34' 0.007(5) 0.034(7) 0.050(8) -0.005(6) 0.002(5) -0.007(5) C35' 0.021(7) 0.049(9) 0.016(6) 0.000(7) 0.004(5) -0.001(7) C36' 0.030(13) 0.06(3) 0.020(11) -0.010(10) 0.006(8) -0.005(8) C37' 0.016(7) 0.024(16) 0.007(7) 0.003(5) 0.002(5) -0.001(5) C38' 0.016(3) 0.034(3) 0.019(3) 0.004(2) -0.003(2) 0.002(2) C39' 0.018(3) 0.023(10) 0.017(3) 0.001(2) 0.000(2) 0.001(2) C40' 0.019(7) 0.026(12) 0.015(7) -0.001(7) 0.006(5) 0.002(6) C41' 0.025(9) 0.046(17) 0.031(9) -0.001(9) 0.008(6) -0.002(9) C42' 0.031(4) 0.048(11) 0.017(3) 0.000(3) 0.007(3) -0.002(3) C43' 0.023(10) 0.06(3) 0.011(10) 0.006(7) 0.009(7) 0.005(8) C44' 0.023(10) 0.05(2) 0.013(9) -0.004(7) 0.004(6) -0.003(6) C45 0.016(3) 0.026(3) 0.014(3) 0.001(2) 0.006(2) -0.001(2) C46 0.015(3) 0.024(3) 0.019(3) 0.000(2) 0.000(2) 0.001(2) C47 0.015(3) 0.034(3) 0.019(3) 0.002(2) 0.004(2) 0.004(2) C48 0.013(3) 0.041(4) 0.028(3) -0.001(3) 0.000(2) 0.000(2) C49 0.025(3) 0.041(4) 0.021(3) 0.000(3) -0.008(2) 0.001(3) C50 0.018(3) 0.032(3) 0.017(3) 0.003(2) 0.003(2) -0.001(2) C51 0.014(3) 0.022(3) 0.023(3) 0.001(2) -0.001(2) 0.003(2) C52 0.017(3) 0.022(3) 0.019(3) 0.000(2) 0.003(2) -0.001(2) C53 0.018(3) 0.021(3) 0.018(3) 0.001(2) 0.004(2) 0.002(2) C54 0.016(3) 0.026(3) 0.022(3) -0.001(2) 0.004(2) 0.002(2) C55 0.027(3) 0.025(3) 0.026(3) 0.001(2) 0.003(2) 0.003(2) C56 0.019(3) 0.029(3) 0.022(3) 0.003(2) -0.005(2) 0.001(2) C57 0.020(3) 0.027(3) 0.015(3) 0.002(2) 0.001(2) 0.001(2) C58 0.010(2) 0.023(3) 0.020(3) -0.001(2) 0.005(2) 0.000(2) C59 0.041(4) 0.038(4) 0.033(4) 0.009(3) 0.010(3) 0.006(3) C60 0.059(5) 0.032(4) 0.054(5) -0.005(3) 0.026(4) -0.001(3) C61 0.078(6) 0.045(5) 0.053(5) -0.017(4) 0.031(4) -0.016(4) C62 0.038(4) 0.040(4) 0.019(3) -0.004(3) 0.008(3) 0.000(3) C71 0.038(4) 0.037(4) 0.028(3) 0.002(3) 0.012(3) 0.000(3) C72 0.086(6) 0.042(5) 0.042(5) 0.012(4) 0.023(4) 0.013(4) C73 0.045(4) 0.032(4) 0.055(5) 0.001(3) 0.016(4) 0.007(3) C74 0.046(4) 0.038(4) 0.030(4) -0.006(3) 0.009(3) 0.000(3) O7 0.036(9) 0.050(7) 0.015(6) -0.005(5) 0.003(6) 0.018(7) C80 0.030(9) 0.045(10) 0.037(10) 0.021(8) 0.010(8) 0.013(9) C81 0.048(13) 0.13(2) 0.039(11) -0.037(12) -0.012(10) 0.051(13) C82 0.053(18) 0.13(3) 0.062(16) -0.037(15) -0.017(12) 0.069(17) C83 0.081(17) 0.06(2) 0.015(10) -0.021(9) -0.010(9) 0.041(13) O7' 0.051(12) 0.047(8) 0.019(6) 0.005(5) 0.013(8) 0.018(9) C80' 0.084(16) 0.036(10) 0.023(8) 0.002(7) 0.003(10) 0.035(11) C81' 0.054(13) 0.049(11) 0.046(12) 0.001(9) -0.009(11) 0.024(11) C82' 0.058(19) 0.12(2) 0.026(10) -0.025(11) -0.004(10) 0.056(17) C83' 0.12(2) 0.043(17) 0.018(11) -0.002(9) 0.005(11) 0.048(12) O8 0.036(6) 0.049(7) 0.026(5) 0.009(5) -0.003(4) -0.014(5) C84 0.067(10) 0.055(9) 0.064(10) 0.021(8) -0.033(8) -0.030(8) C85 0.042(8) 0.064(9) 0.120(12) 0.012(10) -0.011(9) -0.004(7) C86 0.055(9) 0.049(9) 0.117(12) 0.026(9) 0.046(9) 0.012(7) C87 0.058(10) 0.040(10) 0.055(11) 0.014(8) 0.017(8) 0.013(8) O8' 0.024(5) 0.043(7) 0.028(5) -0.005(5) 0.004(4) -0.003(4) C84' 0.024(6) 0.044(8) 0.030(7) 0.000(6) -0.010(5) -0.011(6) C85' 0.036(7) 0.041(8) 0.028(7) 0.003(6) -0.005(6) -0.010(6) C86' 0.026(7) 0.063(10) 0.018(6) 0.003(6) -0.002(5) -0.007(6) C87' 0.023(7) 0.039(10) 0.025(8) 0.014(7) -0.003(6) 0.007(7) O9 0.025(5) 0.044(6) 0.022(5) -0.006(4) 0.005(4) 0.001(4) C88 0.032(7) 0.050(9) 0.040(8) -0.003(7) 0.002(6) 0.006(6) C89 0.038(7) 0.036(8) 0.032(7) -0.007(6) -0.001(6) 0.005(6) C90 0.035(7) 0.056(9) 0.021(6) -0.012(6) 0.003(5) 0.014(6) C91 0.028(8) 0.038(10) 0.044(9) -0.016(8) 0.002(6) -0.001(7) O9' 0.030(6) 0.055(7) 0.028(6) -0.009(5) -0.005(4) 0.010(5) C88' 0.081(12) 0.064(11) 0.061(11) -0.029(9) -0.040(10) 0.034(9) C89' 0.065(12) 0.047(10) 0.129(17) -0.012(11) -0.016(12) 0.012(9) C90' 0.068(11) 0.039(9) 0.125(16) -0.017(10) 0.068(11) -0.007(8) C91' 0.069(12) 0.050(12) 0.046(11) -0.023(9) 0.024(9) -0.014(10) O10 0.027(8) 0.047(7) 0.025(5) 0.003(4) -0.008(6) -0.007(7) C92 0.088(18) 0.047(11) 0.029(9) -0.006(8) -0.006(11) -0.022(13) C93 0.070(17) 0.039(10) 0.051(13) -0.007(9) -0.016(12) -0.018(11) C94 0.07(2) 0.059(14) 0.034(11) 0.023(9) -0.003(11) -0.005(13) C95 0.044(14) 0.094(19) 0.034(11) 0.035(11) 0.000(9) -0.003(12) O10' 0.016(7) 0.047(7) 0.020(5) 0.006(4) -0.008(6) -0.011(6) C92' 0.027(9) 0.047(11) 0.034(9) 0.002(8) 0.003(8) -0.017(9) C93' 0.044(14) 0.15(3) 0.031(11) 0.038(12) -0.013(10) -0.046(14) C94' 0.042(16) 0.14(3) 0.057(16) 0.017(15) -0.020(12) -0.031(17) C95' 0.048(14) 0.048(11) 0.017(8) -0.010(7) -0.002(7) 0.007(10) _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 Br1 C1 1.912(5) . ? Br2 Li2 2.500(10) . ? Br2 Li1 2.512(10) . ? Br3 Li4 2.492(11) . ? Br3 Li5 2.490(12) . ? Br3 Li3 2.738(10) . ? Br4 C45 1.914(5) . ? Li1 O2 1.946(10) . ? Li1 O1 1.949(10) . ? Li1 C8 2.309(11) . ? Li2 O3 1.953(10) . ? Li2 O4 1.978(10) . ? Li2 C8 2.287(10) . ? Li3 O5 1.954(11) . ? Li3 O6 1.972(11) . ? Li3 C52 2.148(12) . ? Li4 O10 1.785(19) . ? Li4 O9' 1.974(14) . ? Li4 O9 2.009(14) . ? Li4 O10' 2.075(18) . ? Li4 C38 2.219(11) . ? Li5 O7' 1.77(2) . ? Li5 O8 1.973(15) . ? Li5 O8' 1.984(14) . ? Li5 O7 2.109(19) . ? Li5 C38 2.234(12) . ? O1 C15 1.436(8) . ? O1 C18 1.440(8) . ? O2 C19 1.438(7) . ? O2 C22 1.454(7) . ? O3 C26 1.413(8) . ? O3 C23 1.432(7) . ? O4 C30 1.421(7) . ? O4 C27 1.436(7) . ? O5 C59 1.425(8) . ? O5 C62 1.433(7) . ? O6 C74 1.421(8) . ? O6 C71 1.436(7) . ? C1 C2 1.396(7) . ? C1 C14 1.395(7) . ? C2 C3 1.437(7) . ? C2 C7 1.446(7) . ? C3 C4 1.344(8) . ? C3 H3 0.9500 . ? C4 C5 1.415(8) . ? C4 H4 0.9500 . ? C5 C6 1.365(7) . ? C5 H5 0.9500 . ? C6 C7 1.432(7) . ? C6 H6 0.9500 . ? C7 C8 1.400(6) . ? C8 C9 1.414(6) . ? C9 C10 1.431(7) . ? C9 C14 1.446(7) . ? C10 C11 1.362(7) . ? C10 H10 0.9500 . ? C11 C12 1.416(8) . ? C11 H11 0.9500 . ? C12 C13 1.363(8) . ? C12 H12 0.9500 . ? C13 C14 1.418(7) . ? C13 H13 0.9500 . ? C15 C16 1.492(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.500(10) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.460(10) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.518(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.524(9) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.504(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.487(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.534(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.522(10) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.506(9) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.543(9) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.518(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? Br5 C31 1.905(9) . ? C31 C44 1.396(13) . ? C31 C32 1.407(11) . ? C32 C33 1.439(11) . ? C32 C37 1.452(12) . ? C33 C34 1.344(12) . ? C33 H33 0.9500 . ? C34 C35 1.394(13) . ? C34 H34 0.9500 . ? C35 C36 1.370(15) . ? C35 H35 0.9500 . ? C36 C37 1.422(12) . ? C36 H36 0.9500 . ? C37 C38 1.417(11) . ? C38 C39 1.424(11) . ? C39 C40 1.439(15) . ? C39 C44 1.446(17) . ? C40 C41 1.363(13) . ? C40 H40 0.9500 . ? C41 C42 1.412(16) . ? C41 H41 0.9500 . ? C42 C43 1.359(18) . ? C42 H42 0.9500 . ? C43 C44 1.421(13) . ? C43 H43 0.9500 . ? Br5' C31' 1.914(9) . ? C31' C44' 1.395(14) . ? C31' C32' 1.401(11) . ? C32' C33' 1.426(11) . ? C32' C37' 1.455(12) . ? C33' C34' 1.346(13) . ? C33' H33' 0.9500 . ? C34' C35' 1.391(13) . ? C34' H34' 0.9500 . ? C35' C36' 1.371(15) . ? C35' H35' 0.9500 . ? C36' C37' 1.426(13) . ? C36' H36' 0.9500 . ? C39' C40' 1.437(15) . ? C39' C44' 1.446(16) . ? C40' C41' 1.368(13) . ? C40' H40' 0.9500 . ? C41' C42' 1.413(16) . ? C41' H41' 0.9500 . ? C42' C43' 1.360(18) . ? C42' H42' 0.9500 . ? C43' C44' 1.423(12) . ? C43' H43' 0.9500 . ? C45 C46 1.393(7) . ? C45 C58 1.402(7) . ? C46 C47 1.427(8) . ? C46 C51 1.451(7) . ? C47 C48 1.362(8) . ? C47 H47 0.9500 . ? C48 C49 1.422(8) . ? C48 H48 0.9500 . ? C49 C50 1.357(8) . ? C49 H49 0.9500 . ? C50 C51 1.433(8) . ? C50 H50 0.9500 . ? C51 C52 1.410(7) . ? C52 C53 1.417(8) . ? C53 C54 1.432(8) . ? C53 C58 1.454(7) . ? C54 C55 1.345(8) . ? C54 H54 0.9500 . ? C55 C56 1.410(8) . ? C55 H55 0.9500 . ? C56 C57 1.358(8) . ? C56 H56 0.9500 . ? C57 C58 1.424(8) . ? C57 H57 0.9500 . ? C59 C60 1.503(10) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.518(10) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.498(10) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C71 C72 1.500(10) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.513(10) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.510(10) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? O7 C83 1.437(15) . ? O7 C80 1.440(13) . ? C80 C81 1.501(16) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 C82 1.499(16) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C83 1.448(16) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? O7' C80' 1.442(14) . ? O7' C83' 1.444(15) . ? C80' C81' 1.493(17) . ? C80' H80C 0.9900 . ? C80' H80D 0.9900 . ? C81' C82' 1.508(15) . ? C81' H81C 0.9900 . ? C81' H81D 0.9900 . ? C82' C83' 1.460(18) . ? C82' H82C 0.9900 . ? C82' H82D 0.9900 . ? C83' H83C 0.9900 . ? C83' H83D 0.9900 . ? O8 C87 1.42(2) . ? O8 C84 1.43(2) . ? C84 C85 1.45(2) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 C86 1.48(3) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 C87 1.54(3) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? O8' C87' 1.426(17) . ? O8' C84' 1.446(15) . ? C84' C85' 1.510(18) . ? C84' H84C 0.9900 . ? C84' H84D 0.9900 . ? C85' C86' 1.566(17) . ? C85' H85C 0.9900 . ? C85' H85D 0.9900 . ? C86' C87' 1.523(19) . ? C86' H86C 0.9900 . ? C86' H86D 0.9900 . ? C87' H87C 0.9900 . ? C87' H87D 0.9900 . ? O9 C91 1.403(18) . ? O9 C88 1.444(17) . ? C88 C89 1.497(18) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 C90 1.539(18) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 C91 1.49(2) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? O9' C91' 1.42(2) . ? O9' C88' 1.44(2) . ? C88' C89' 1.48(3) . ? C88' H88C 0.9900 . ? C88' H88D 0.9900 . ? C89' C90' 1.46(3) . ? C89' H89C 0.9900 . ? C89' H89D 0.9900 . ? C90' C91' 1.55(3) . ? C90' H90C 0.9900 . ? C90' H90D 0.9900 . ? C91' H91C 0.9900 . ? C91' H91D 0.9900 . ? O10 C95 1.424(14) . ? O10 C92 1.432(16) . ? C92 C93 1.49(2) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 C94 1.488(17) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 C95 1.408(19) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? O10' C95' 1.420(14) . ? O10' C92' 1.428(16) . ? C92' C93' 1.49(2) . ? C92' H92C 0.9900 . ? C92' H92D 0.9900 . ? C93' C94' 1.493(18) . ? C93' H93C 0.9900 . ? C93' H93D 0.9900 . ? C94' C95' 1.41(2) . ? C94' H94C 0.9900 . ? C94' H94D 0.9900 . ? C95' H95C 0.9900 . ? C95' H95D 0.9900 . ? 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 Li2 Br2 Li1 66.3(3) . . ? Li4 Br3 Li5 65.2(4) . . ? Li4 Br3 Li3 141.2(4) . . ? Li5 Br3 Li3 142.2(4) . . ? O2 Li1 O1 101.9(5) . . ? O2 Li1 C8 111.4(5) . . ? O1 Li1 C8 115.0(5) . . ? O2 Li1 Br2 111.5(4) . . ? O1 Li1 Br2 107.2(4) . . ? C8 Li1 Br2 109.7(4) . . ? O3 Li2 O4 103.0(5) . . ? O3 Li2 C8 112.3(4) . . ? O4 Li2 C8 116.0(5) . . ? O3 Li2 Br2 109.1(4) . . ? O4 Li2 Br2 105.0(4) . . ? C8 Li2 Br2 110.8(4) . . ? O5 Li3 O6 114.9(5) . . ? O5 Li3 C52 110.2(5) . . ? O6 Li3 C52 109.1(5) . . ? O5 Li3 Br3 94.6(4) . . ? O6 Li3 Br3 94.3(4) . . ? C52 Li3 Br3 133.1(5) . . ? O10 Li4 O9' 80.9(7) . . ? O10 Li4 O9 106.0(8) . . ? O9' Li4 O9 25.4(4) . . ? O10 Li4 O10' 14.8(6) . . ? O9' Li4 O10' 92.4(7) . . ? O9 Li4 O10' 117.8(8) . . ? O10 Li4 C38 121.3(7) . . ? O9' Li4 C38 121.2(6) . . ? O9 Li4 C38 109.3(6) . . ? O10' Li4 C38 107.3(6) . . ? O10 Li4 Br3 104.8(6) . . ? O9' Li4 Br3 115.0(6) . . ? O9 Li4 Br3 103.8(6) . . ? O10' Li4 Br3 108.3(6) . . ? C38 Li4 Br3 110.2(5) . . ? O7' Li5 O8 82.3(9) . . ? O7' Li5 O8' 106.9(9) . . ? O8 Li5 O8' 25.0(4) . . ? O7' Li5 O7 12.2(11) . . ? O8 Li5 O7 92.2(9) . . ? O8' Li5 O7 117.2(9) . . ? O7' Li5 C38 120.2(9) . . ? O8 Li5 C38 121.8(6) . . ? O8' Li5 C38 110.1(6) . . ? O7 Li5 C38 108.8(7) . . ? O7' Li5 Br3 104.4(7) . . ? O8 Li5 Br3 115.0(6) . . ? O8' Li5 Br3 104.1(6) . . ? O7 Li5 Br3 106.6(6) . . ? C38 Li5 Br3 109.7(5) . . ? C15 O1 C18 108.8(5) . . ? C15 O1 Li1 119.5(5) . . ? C18 O1 Li1 129.2(5) . . ? C19 O2 C22 104.5(4) . . ? C19 O2 Li1 120.5(4) . . ? C22 O2 Li1 132.1(5) . . ? C26 O3 C23 104.3(5) . . ? C26 O3 Li2 121.4(5) . . ? C23 O3 Li2 133.3(5) . . ? C30 O4 C27 105.1(5) . . ? C30 O4 Li2 130.0(5) . . ? C27 O4 Li2 122.4(5) . . ? C59 O5 C62 105.2(5) . . ? C59 O5 Li3 119.4(5) . . ? C62 O5 Li3 135.3(5) . . ? C74 O6 C71 105.0(5) . . ? C74 O6 Li3 120.6(5) . . ? C71 O6 Li3 134.3(5) . . ? C2 C1 C14 123.0(5) . . ? C2 C1 Br1 118.6(4) . . ? C14 C1 Br1 118.5(4) . . ? C1 C2 C3 124.2(5) . . ? C1 C2 C7 117.4(4) . . ? C3 C2 C7 118.4(4) . . ? C4 C3 C2 121.8(5) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 120.6(5) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 119.9(5) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 122.4(5) . . ? C5 C6 H6 118.8 . . ? C7 C6 H6 118.8 . . ? C8 C7 C6 120.3(5) . . ? C8 C7 C2 122.8(4) . . ? C6 C7 C2 116.9(4) . . ? C7 C8 C9 116.9(4) . . ? C7 C8 Li2 112.3(4) . . ? C9 C8 Li2 115.9(4) . . ? C7 C8 Li1 112.7(4) . . ? C9 C8 Li1 118.3(4) . . ? Li2 C8 Li1 73.2(4) . . ? C8 C9 C10 120.2(5) . . ? C8 C9 C14 122.5(4) . . ? C10 C9 C14 117.3(4) . . ? C11 C10 C9 122.5(5) . . ? C11 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? C10 C11 C12 119.4(5) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C13 C12 C11 120.5(5) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 121.9(5) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C1 C14 C13 124.2(5) . . ? C1 C14 C9 117.4(4) . . ? C13 C14 C9 118.4(4) . . ? O1 C15 C16 106.1(6) . . ? O1 C15 H15A 110.5 . . ? C16 C15 H15A 110.5 . . ? O1 C15 H15B 110.5 . . ? C16 C15 H15B 110.5 . . ? H15A C15 H15B 108.7 . . ? C15 C16 C17 101.4(6) . . ? C15 C16 H16A 111.5 . . ? C17 C16 H16A 111.5 . . ? C15 C16 H16B 111.5 . . ? C17 C16 H16B 111.5 . . ? H16A C16 H16B 109.3 . . ? C18 C17 C16 105.0(6) . . ? C18 C17 H17A 110.7 . . ? C16 C17 H17A 110.7 . . ? C18 C17 H17B 110.7 . . ? C16 C17 H17B 110.7 . . ? H17A C17 H17B 108.8 . . ? O1 C18 C17 106.2(6) . . ? O1 C18 H18A 110.5 . . ? C17 C18 H18A 110.5 . . ? O1 C18 H18B 110.5 . . ? C17 C18 H18B 110.5 . . ? H18A C18 H18B 108.7 . . ? O2 C19 C20 106.2(5) . . ? O2 C19 H19A 110.5 . . ? C20 C19 H19A 110.5 . . ? O2 C19 H19B 110.5 . . ? C20 C19 H19B 110.5 . . ? H19A C19 H19B 108.7 . . ? C19 C20 C21 104.1(5) . . ? C19 C20 H20A 110.9 . . ? C21 C20 H20A 110.9 . . ? C19 C20 H20B 110.9 . . ? C21 C20 H20B 110.9 . . ? H20A C20 H20B 109.0 . . ? C22 C21 C20 104.6(5) . . ? C22 C21 H21A 110.8 . . ? C20 C21 H21A 110.8 . . ? C22 C21 H21B 110.8 . . ? C20 C21 H21B 110.8 . . ? H21A C21 H21B 108.9 . . ? O2 C22 C21 103.4(5) . . ? O2 C22 H22A 111.1 . . ? C21 C22 H22A 111.1 . . ? O2 C22 H22B 111.1 . . ? C21 C22 H22B 111.1 . . ? H22A C22 H22B 109.0 . . ? O3 C23 C24 105.5(5) . . ? O3 C23 H23A 110.6 . . ? C24 C23 H23A 110.6 . . ? O3 C23 H23B 110.6 . . ? C24 C23 H23B 110.6 . . ? H23A C23 H23B 108.8 . . ? C23 C24 C25 103.3(6) . . ? C23 C24 H24A 111.1 . . ? C25 C24 H24A 111.1 . . ? C23 C24 H24B 111.1 . . ? C25 C24 H24B 111.1 . . ? H24A C24 H24B 109.1 . . ? C26 C25 C24 103.6(5) . . ? C26 C25 H25A 111.0 . . ? C24 C25 H25A 111.0 . . ? C26 C25 H25B 111.0 . . ? C24 C25 H25B 111.0 . . ? H25A C25 H25B 109.0 . . ? O3 C26 C25 106.6(5) . . ? O3 C26 H26A 110.4 . . ? C25 C26 H26A 110.4 . . ? O3 C26 H26B 110.4 . . ? C25 C26 H26B 110.4 . . ? H26A C26 H26B 108.6 . . ? O4 C27 C28 106.5(5) . . ? O4 C27 H27A 110.4 . . ? C28 C27 H27A 110.4 . . ? O4 C27 H27B 110.4 . . ? C28 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? C27 C28 C29 103.9(5) . . ? C27 C28 H28A 111.0 . . ? C29 C28 H28A 111.0 . . ? C27 C28 H28B 111.0 . . ? C29 C28 H28B 111.0 . . ? H28A C28 H28B 109.0 . . ? C30 C29 C28 103.3(5) . . ? C30 C29 H29A 111.1 . . ? C28 C29 H29A 111.1 . . ? C30 C29 H29B 111.1 . . ? C28 C29 H29B 111.1 . . ? H29A C29 H29B 109.1 . . ? O4 C30 C29 104.3(5) . . ? O4 C30 H30A 110.9 . . ? C29 C30 H30A 110.9 . . ? O4 C30 H30B 110.9 . . ? C29 C30 H30B 110.9 . . ? H30A C30 H30B 108.9 . . ? C44 C31 C32 122.6(9) . . ? C44 C31 Br5 119.4(8) . . ? C32 C31 Br5 118.0(7) . . ? C31 C32 C33 124.6(8) . . ? C31 C32 C37 116.8(8) . . ? C33 C32 C37 118.5(8) . . ? C34 C33 C32 120.9(9) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 121.7(10) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C36 C35 C34 119.8(11) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 122.4(14) . . ? C35 C36 H36 118.8 . . ? C37 C36 H36 118.8 . . ? C38 C37 C36 119.2(10) . . ? C38 C37 C32 123.9(9) . . ? C36 C37 C32 116.8(10) . . ? C37 C38 C39 114.9(9) . . ? C37 C38 Li4 108.2(9) . . ? C39 C38 Li4 119(2) . . ? C37 C38 Li5 119.6(8) . . ? C39 C38 Li5 115(2) . . ? Li4 C38 Li5 74.2(5) . . ? C38 C39 C40 119.3(12) . . ? C38 C39 C44 123.1(16) . . ? C40 C39 C44 117.2(10) . . ? C41 C40 C39 121.9(13) . . ? C41 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? C40 C41 C42 120.0(13) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C43 C42 C41 120.6(14) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C42 C43 C44 121.6(15) . . ? C42 C43 H43 119.2 . . ? C44 C43 H43 119.2 . . ? C31 C44 C43 123.4(13) . . ? C31 C44 C39 118.0(11) . . ? C43 C44 C39 118.6(13) . . ? C44' C31' C32' 123.5(9) . . ? C44' C31' Br5' 119.1(8) . . ? C32' C31' Br5' 117.2(7) . . ? C31' C32' C33' 125.7(8) . . ? C31' C32' C37' 116.2(8) . . ? C33' C32' C37' 118.1(8) . . ? C34' C33' C32' 121.5(9) . . ? C34' C33' H33' 119.3 . . ? C32' C33' H33' 119.3 . . ? C33' C34' C35' 121.6(10) . . ? C33' C34' H34' 119.2 . . ? C35' C34' H34' 119.2 . . ? C36' C35' C34' 119.7(11) . . ? C36' C35' H35' 120.1 . . ? C34' C35' H35' 120.1 . . ? C35' C36' C37' 122.1(15) . . ? C35' C36' H36' 118.9 . . ? C37' C36' H36' 118.9 . . ? C36' C37' C32' 117.0(10) . . ? C40' C39' C44' 116.9(10) . . ? C41' C40' C39' 122.1(13) . . ? C41' C40' H40' 118.9 . . ? C39' C40' H40' 118.9 . . ? C40' C41' C42' 119.8(14) . . ? C40' C41' H41' 120.1 . . ? C42' C41' H41' 120.1 . . ? C43' C42' C41' 120.7(14) . . ? C43' C42' H42' 119.6 . . ? C41' C42' H42' 119.6 . . ? C42' C43' C44' 121.3(15) . . ? C42' C43' H43' 119.4 . . ? C44' C43' H43' 119.4 . . ? C31' C44' C43' 123.3(14) . . ? C31' C44' C39' 117.5(11) . . ? C43' C44' C39' 119.1(12) . . ? C46 C45 C58 122.4(5) . . ? C46 C45 Br4 119.0(4) . . ? C58 C45 Br4 118.6(4) . . ? C45 C46 C47 123.4(5) . . ? C45 C46 C51 117.3(5) . . ? C47 C46 C51 119.2(5) . . ? C48 C47 C46 121.8(5) . . ? C48 C47 H47 119.1 . . ? C46 C47 H47 119.1 . . ? C47 C48 C49 120.2(5) . . ? C47 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? C50 C49 C48 119.0(5) . . ? C50 C49 H49 120.5 . . ? C48 C49 H49 120.5 . . ? C49 C50 C51 124.3(5) . . ? C49 C50 H50 117.8 . . ? C51 C50 H50 117.8 . . ? C52 C51 C50 119.7(5) . . ? C52 C51 C46 124.8(5) . . ? C50 C51 C46 115.5(5) . . ? C51 C52 C53 113.8(5) . . ? C51 C52 Li3 119.9(5) . . ? C53 C52 Li3 126.2(5) . . ? C52 C53 C54 119.8(5) . . ? C52 C53 C58 124.5(5) . . ? C54 C53 C58 115.7(5) . . ? C55 C54 C53 122.8(5) . . ? C55 C54 H54 118.6 . . ? C53 C54 H54 118.6 . . ? C54 C55 C56 121.1(6) . . ? C54 C55 H55 119.4 . . ? C56 C55 H55 119.4 . . ? C57 C56 C55 119.3(5) . . ? C57 C56 H56 120.3 . . ? C55 C56 H56 120.3 . . ? C56 C57 C58 121.8(5) . . ? C56 C57 H57 119.1 . . ? C58 C57 H57 119.1 . . ? C45 C58 C57 123.8(5) . . ? C45 C58 C53 117.1(5) . . ? C57 C58 C53 119.1(5) . . ? O5 C59 C60 105.7(6) . . ? O5 C59 H59A 110.6 . . ? C60 C59 H59A 110.6 . . ? O5 C59 H59B 110.6 . . ? C60 C59 H59B 110.6 . . ? H59A C59 H59B 108.7 . . ? C59 C60 C61 103.5(6) . . ? C59 C60 H60A 111.1 . . ? C61 C60 H60A 111.1 . . ? C59 C60 H60B 111.1 . . ? C61 C60 H60B 111.1 . . ? H60A C60 H60B 109.0 . . ? C62 C61 C60 105.5(6) . . ? C62 C61 H61A 110.6 . . ? C60 C61 H61A 110.6 . . ? C62 C61 H61B 110.6 . . ? C60 C61 H61B 110.6 . . ? H61A C61 H61B 108.8 . . ? O5 C62 C61 105.4(5) . . ? O5 C62 H62A 110.7 . . ? C61 C62 H62A 110.7 . . ? O5 C62 H62B 110.7 . . ? C61 C62 H62B 110.7 . . ? H62A C62 H62B 108.8 . . ? O6 C71 C72 106.1(5) . . ? O6 C71 H71A 110.5 . . ? C72 C71 H71A 110.5 . . ? O6 C71 H71B 110.5 . . ? C72 C71 H71B 110.5 . . ? H71A C71 H71B 108.7 . . ? C71 C72 C73 104.8(6) . . ? C71 C72 H72A 110.8 . . ? C73 C72 H72A 110.8 . . ? C71 C72 H72B 110.8 . . ? C73 C72 H72B 110.8 . . ? H72A C72 H72B 108.9 . . ? C74 C73 C72 104.1(6) . . ? C74 C73 H73A 110.9 . . ? C72 C73 H73A 110.9 . . ? C74 C73 H73B 110.9 . . ? C72 C73 H73B 110.9 . . ? H73A C73 H73B 109.0 . . ? O6 C74 C73 105.4(6) . . ? O6 C74 H74A 110.7 . . ? C73 C74 H74A 110.7 . . ? O6 C74 H74B 110.7 . . ? C73 C74 H74B 110.7 . . ? H74A C74 H74B 108.8 . . ? C83 O7 C80 108.5(13) . . ? C83 O7 Li5 127.2(13) . . ? C80 O7 Li5 123.0(12) . . ? O7 C80 C81 104.4(11) . . ? O7 C80 H80A 110.9 . . ? C81 C80 H80A 110.9 . . ? O7 C80 H80B 110.9 . . ? C81 C80 H80B 110.9 . . ? H80A C80 H80B 108.9 . . ? C82 C81 C80 101.9(13) . . ? C82 C81 H81A 111.4 . . ? C80 C81 H81A 111.4 . . ? C82 C81 H81B 111.4 . . ? C80 C81 H81B 111.4 . . ? H81A C81 H81B 109.3 . . ? C83 C82 C81 108.8(13) . . ? C83 C82 H82A 109.9 . . ? C81 C82 H82A 109.9 . . ? C83 C82 H82B 109.9 . . ? C81 C82 H82B 109.9 . . ? H82A C82 H82B 108.3 . . ? O7 C83 C82 105.9(13) . . ? O7 C83 H83A 110.6 . . ? C82 C83 H83A 110.6 . . ? O7 C83 H83B 110.6 . . ? C82 C83 H83B 110.6 . . ? H83A C83 H83B 108.7 . . ? C80' O7' C83' 108.6(12) . . ? C80' O7' Li5 117.2(13) . . ? C83' O7' Li5 130.5(15) . . ? O7' C80' C81' 107.1(11) . . ? O7' C80' H80C 110.3 . . ? C81' C80' H80C 110.3 . . ? O7' C80' H80D 110.3 . . ? C81' C80' H80D 110.3 . . ? H80C C80' H80D 108.6 . . ? C80' C81' C82' 100.7(13) . . ? C80' C81' H81C 111.6 . . ? C82' C81' H81C 111.6 . . ? C80' C81' H81D 111.6 . . ? C82' C81' H81D 111.6 . . ? H81C C81' H81D 109.4 . . ? C83' C82' C81' 104.6(14) . . ? C83' C82' H82C 110.8 . . ? C81' C82' H82C 110.8 . . ? C83' C82' H82D 110.8 . . ? C81' C82' H82D 110.8 . . ? H82C C82' H82D 108.9 . . ? O7' C83' C82' 104.7(15) . . ? O7' C83' H83C 110.8 . . ? C82' C83' H83C 110.8 . . ? O7' C83' H83D 110.8 . . ? C82' C83' H83D 110.8 . . ? H83C C83' H83D 108.9 . . ? C87 O8 C84 105.0(13) . . ? C87 O8 Li5 139.4(12) . . ? C84 O8 Li5 114.0(9) . . ? O8 C84 C85 106.3(17) . . ? O8 C84 H84A 110.5 . . ? C85 C84 H84A 110.5 . . ? O8 C84 H84B 110.5 . . ? C85 C84 H84B 110.5 . . ? H84A C84 H84B 108.7 . . ? C84 C85 C86 104.2(16) . . ? C84 C85 H85A 110.9 . . ? C86 C85 H85A 110.9 . . ? C84 C85 H85B 110.9 . . ? C86 C85 H85B 110.9 . . ? H85A C85 H85B 108.9 . . ? C85 C86 C87 106.0(15) . . ? C85 C86 H86A 110.5 . . ? C87 C86 H86A 110.5 . . ? C85 C86 H86B 110.5 . . ? C87 C86 H86B 110.5 . . ? H86A C86 H86B 108.7 . . ? O8 C87 C86 100.3(16) . . ? O8 C87 H87A 111.7 . . ? C86 C87 H87A 111.7 . . ? O8 C87 H87B 111.7 . . ? C86 C87 H87B 111.7 . . ? H87A C87 H87B 109.5 . . ? C87' O8' C84' 105.1(10) . . ? C87' O8' Li5 127.3(9) . . ? C84' O8' Li5 123.7(9) . . ? O8' C84' C85' 105.6(10) . . ? O8' C84' H84C 110.6 . . ? C85' C84' H84C 110.6 . . ? O8' C84' H84D 110.6 . . ? C85' C84' H84D 110.6 . . ? H84C C84' H84D 108.7 . . ? C84' C85' C86' 105.0(10) . . ? C84' C85' H85C 110.7 . . ? C86' C85' H85C 110.7 . . ? C84' C85' H85D 110.7 . . ? C86' C85' H85D 110.7 . . ? H85C C85' H85D 108.8 . . ? C87' C86' C85' 101.9(10) . . ? C87' C86' H86C 111.4 . . ? C85' C86' H86C 111.4 . . ? C87' C86' H86D 111.4 . . ? C85' C86' H86D 111.4 . . ? H86C C86' H86D 109.3 . . ? O8' C87' C86' 105.5(11) . . ? O8' C87' H87C 110.6 . . ? C86' C87' H87C 110.6 . . ? O8' C87' H87D 110.6 . . ? C86' C87' H87D 110.6 . . ? H87C C87' H87D 108.8 . . ? C91 O9 C88 105.5(11) . . ? C91 O9 Li4 127.0(10) . . ? C88 O9 Li4 124.2(8) . . ? O9 C88 C89 105.6(11) . . ? O9 C88 H88A 110.6 . . ? C89 C88 H88A 110.6 . . ? O9 C88 H88B 110.6 . . ? C89 C88 H88B 110.6 . . ? H88A C88 H88B 108.7 . . ? C88 C89 C90 104.2(11) . . ? C88 C89 H89A 110.9 . . ? C90 C89 H89A 110.9 . . ? C88 C89 H89B 110.9 . . ? C90 C89 H89B 110.9 . . ? H89A C89 H89B 108.9 . . ? C91 C90 C89 103.7(11) . . ? C91 C90 H90A 111.0 . . ? C89 C90 H90A 111.0 . . ? C91 C90 H90B 111.0 . . ? C89 C90 H90B 111.0 . . ? H90A C90 H90B 109.0 . . ? O9 C91 C90 105.5(12) . . ? O9 C91 H91A 110.6 . . ? C90 C91 H91A 110.6 . . ? O9 C91 H91B 110.6 . . ? C90 C91 H91B 110.6 . . ? H91A C91 H91B 108.8 . . ? C91' O9' C88' 103.2(14) . . ? C91' O9' Li4 141.6(12) . . ? C88' O9' Li4 113.9(9) . . ? O9' C88' C89' 105.6(18) . . ? O9' C88' H88C 110.6 . . ? C89' C88' H88C 110.6 . . ? O9' C88' H88D 110.6 . . ? C89' C88' H88D 110.6 . . ? H88C C88' H88D 108.7 . . ? C88' C89' C90' 105.0(17) . . ? C88' C89' H89C 110.8 . . ? C90' C89' H89C 110.8 . . ? C88' C89' H89D 110.8 . . ? C90' C89' H89D 110.8 . . ? H89C C89' H89D 108.8 . . ? C89' C90' C91' 105.0(15) . . ? C89' C90' H90C 110.8 . . ? C91' C90' H90C 110.8 . . ? C89' C90' H90D 110.8 . . ? C91' C90' H90D 110.8 . . ? H90C C90' H90D 108.8 . . ? O9' C91' C90' 102.1(17) . . ? O9' C91' H91C 111.4 . . ? C90' C91' H91C 111.4 . . ? O9' C91' H91D 111.4 . . ? C90' C91' H91D 111.4 . . ? H91C C91' H91D 109.2 . . ? C95 O10 C92 106.1(12) . . ? C95 O10 Li4 137.3(13) . . ? C92 O10 Li4 116.1(12) . . ? O10 C92 C93 106.5(11) . . ? O10 C92 H92A 110.4 . . ? C93 C92 H92A 110.4 . . ? O10 C92 H92B 110.4 . . ? C93 C92 H92B 110.4 . . ? H92A C92 H92B 108.6 . . ? C92 C93 C94 102.8(15) . . ? C92 C93 H93A 111.2 . . ? C94 C93 H93A 111.2 . . ? C92 C93 H93B 111.2 . . ? C94 C93 H93B 111.2 . . ? H93A C93 H93B 109.1 . . ? C95 C94 C93 104.6(12) . . ? C95 C94 H94A 110.8 . . ? C93 C94 H94A 110.8 . . ? C95 C94 H94B 110.8 . . ? C93 C94 H94B 110.8 . . ? H94A C94 H94B 108.9 . . ? C94 C95 O10 111.2(14) . . ? C94 C95 H95A 109.4 . . ? O10 C95 H95A 109.4 . . ? C94 C95 H95B 109.4 . . ? O10 C95 H95B 109.4 . . ? H95A C95 H95B 108.0 . . ? C95' O10' C92' 108.8(11) . . ? C95' O10' Li4 127.9(11) . . ? C92' O10' Li4 123.1(11) . . ? O10' C92' C93' 105.8(12) . . ? O10' C92' H92C 110.6 . . ? C93' C92' H92C 110.6 . . ? O10' C92' H92D 110.6 . . ? C93' C92' H92D 110.6 . . ? H92C C92' H92D 108.7 . . ? C92' C93' C94' 102.9(15) . . ? C92' C93' H93C 111.2 . . ? C94' C93' H93C 111.2 . . ? C92' C93' H93D 111.2 . . ? C94' C93' H93D 111.2 . . ? H93C C93' H93D 109.1 . . ? C95' C94' C93' 105.9(15) . . ? C95' C94' H94C 110.6 . . ? C93' C94' H94C 110.6 . . ? C95' C94' H94D 110.6 . . ? C93' C94' H94D 110.6 . . ? H94C C94' H94D 108.7 . . ? C94' C95' O10' 108.7(12) . . ? C94' C95' H95C 110.0 . . ? O10' C95' H95C 110.0 . . ? C94' C95' H95D 110.0 . . ? O10' C95' H95D 110.0 . . ? H95C C95' H95D 108.3 . . ? 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 Li2 Br2 Li1 O2 122.1(5) . . . . ? Li2 Br2 Li1 O1 -127.2(5) . . . . ? Li2 Br2 Li1 C8 -1.8(3) . . . . ? Li1 Br2 Li2 O3 126.0(5) . . . . ? Li1 Br2 Li2 O4 -124.2(5) . . . . ? Li1 Br2 Li2 C8 1.8(3) . . . . ? Li4 Br3 Li3 O5 -62.9(6) . . . . ? Li5 Br3 Li3 O5 176.4(4) . . . . ? Li4 Br3 Li3 O6 -178.3(4) . . . . ? Li5 Br3 Li3 O6 61.0(6) . . . . ? Li4 Br3 Li3 C52 60.4(9) . . . . ? Li5 Br3 Li3 C52 -60.3(9) . . . . ? Li5 Br3 Li4 O10 138.2(7) . . . . ? Li3 Br3 Li4 O10 -6.3(9) . . . . ? Li5 Br3 Li4 O9' -135.1(8) . . . . ? Li3 Br3 Li4 O9' 80.4(8) . . . . ? Li5 Br3 Li4 O9 -110.8(6) . . . . ? Li3 Br3 Li4 O9 104.7(7) . . . . ? Li5 Br3 Li4 O10' 123.2(7) . . . . ? Li3 Br3 Li4 O10' -21.3(8) . . . . ? Li5 Br3 Li4 C38 6.1(4) . . . . ? Li3 Br3 Li4 C38 -138.3(5) . . . . ? Li4 Br3 Li5 O7' -136.2(9) . . . . ? Li3 Br3 Li5 O7' 7.4(11) . . . . ? Li4 Br3 Li5 O8 135.7(8) . . . . ? Li3 Br3 Li5 O8 -80.7(8) . . . . ? Li4 Br3 Li5 O8' 111.8(7) . . . . ? Li3 Br3 Li5 O8' -104.6(7) . . . . ? Li4 Br3 Li5 O7 -123.7(8) . . . . ? Li3 Br3 Li5 O7 19.9(10) . . . . ? Li4 Br3 Li5 C38 -6.1(4) . . . . ? Li3 Br3 Li5 C38 137.5(5) . . . . ? O2 Li1 O1 C15 -68.9(8) . . . . ? C8 Li1 O1 C15 51.7(8) . . . . ? Br2 Li1 O1 C15 173.8(6) . . . . ? O2 Li1 O1 C18 131.1(7) . . . . ? C8 Li1 O1 C18 -108.3(8) . . . . ? Br2 Li1 O1 C18 13.9(9) . . . . ? O1 Li1 O2 C19 -73.3(6) . . . . ? C8 Li1 O2 C19 163.7(5) . . . . ? Br2 Li1 O2 C19 40.7(7) . . . . ? O1 Li1 O2 C22 84.0(7) . . . . ? C8 Li1 O2 C22 -39.1(8) . . . . ? Br2 Li1 O2 C22 -162.0(5) . . . . ? O4 Li2 O3 C26 -71.4(7) . . . . ? C8 Li2 O3 C26 163.1(5) . . . . ? Br2 Li2 O3 C26 39.8(7) . . . . ? O4 Li2 O3 C23 95.2(7) . . . . ? C8 Li2 O3 C23 -30.3(9) . . . . ? Br2 Li2 O3 C23 -153.6(5) . . . . ? O3 Li2 O4 C30 -80.9(7) . . . . ? C8 Li2 O4 C30 42.2(8) . . . . ? Br2 Li2 O4 C30 164.9(5) . . . . ? O3 Li2 O4 C27 78.1(7) . . . . ? C8 Li2 O4 C27 -158.8(5) . . . . ? Br2 Li2 O4 C27 -36.0(7) . . . . ? O6 Li3 O5 C59 -116.8(6) . . . . ? C52 Li3 O5 C59 6.9(8) . . . . ? Br3 Li3 O5 C59 146.3(5) . . . . ? O6 Li3 O5 C62 67.8(9) . . . . ? C52 Li3 O5 C62 -168.6(6) . . . . ? Br3 Li3 O5 C62 -29.1(8) . . . . ? O5 Li3 O6 C74 116.3(6) . . . . ? C52 Li3 O6 C74 -8.0(7) . . . . ? Br3 Li3 O6 C74 -146.7(5) . . . . ? O5 Li3 O6 C71 -67.6(8) . . . . ? C52 Li3 O6 C71 168.1(5) . . . . ? Br3 Li3 O6 C71 29.5(7) . . . . ? C14 C1 C2 C3 -179.3(6) . . . . ? Br1 C1 C2 C3 0.5(8) . . . . ? C14 C1 C2 C7 0.4(8) . . . . ? Br1 C1 C2 C7 -179.7(4) . . . . ? C1 C2 C3 C4 179.6(6) . . . . ? C7 C2 C3 C4 -0.2(9) . . . . ? C2 C3 C4 C5 -0.9(10) . . . . ? C3 C4 C5 C6 1.5(9) . . . . ? C4 C5 C6 C7 -1.2(9) . . . . ? C5 C6 C7 C8 -179.8(5) . . . . ? C5 C6 C7 C2 0.1(8) . . . . ? C1 C2 C7 C8 0.7(8) . . . . ? C3 C2 C7 C8 -179.5(5) . . . . ? C1 C2 C7 C6 -179.2(5) . . . . ? C3 C2 C7 C6 0.6(8) . . . . ? C6 C7 C8 C9 179.6(5) . . . . ? C2 C7 C8 C9 -0.4(8) . . . . ? C6 C7 C8 Li2 -42.9(7) . . . . ? C2 C7 C8 Li2 137.2(5) . . . . ? C6 C7 C8 Li1 37.5(7) . . . . ? C2 C7 C8 Li1 -142.4(5) . . . . ? O3 Li2 C8 C7 -16.1(7) . . . . ? O4 Li2 C8 C7 -134.1(5) . . . . ? Br2 Li2 C8 C7 106.3(5) . . . . ? O3 Li2 C8 C9 121.9(5) . . . . ? O4 Li2 C8 C9 3.9(7) . . . . ? Br2 Li2 C8 C9 -115.7(5) . . . . ? O3 Li2 C8 Li1 -124.3(5) . . . . ? O4 Li2 C8 Li1 117.7(5) . . . . ? Br2 Li2 C8 Li1 -1.9(4) . . . . ? O2 Li1 C8 C7 130.2(5) . . . . ? O1 Li1 C8 C7 15.0(7) . . . . ? Br2 Li1 C8 C7 -105.8(4) . . . . ? O2 Li1 C8 C9 -11.2(7) . . . . ? O1 Li1 C8 C9 -126.5(5) . . . . ? Br2 Li1 C8 C9 112.7(5) . . . . ? O2 Li1 C8 Li2 -122.1(5) . . . . ? O1 Li1 C8 Li2 122.7(6) . . . . ? Br2 Li1 C8 Li2 1.9(4) . . . . ? C7 C8 C9 C10 -179.6(5) . . . . ? Li2 C8 C9 C10 44.3(7) . . . . ? Li1 C8 C9 C10 -39.7(7) . . . . ? C7 C8 C9 C14 -1.1(7) . . . . ? Li2 C8 C9 C14 -137.2(5) . . . . ? Li1 C8 C9 C14 138.8(5) . . . . ? C8 C9 C10 C11 179.8(5) . . . . ? C14 C9 C10 C11 1.2(9) . . . . ? C9 C10 C11 C12 -1.0(9) . . . . ? C10 C11 C12 C13 0.8(9) . . . . ? C11 C12 C13 C14 -0.9(9) . . . . ? C2 C1 C14 C13 -179.8(5) . . . . ? Br1 C1 C14 C13 0.4(8) . . . . ? C2 C1 C14 C9 -1.8(8) . . . . ? Br1 C1 C14 C9 178.4(4) . . . . ? C12 C13 C14 C1 179.1(6) . . . . ? C12 C13 C14 C9 1.1(8) . . . . ? C8 C9 C14 C1 2.2(8) . . . . ? C10 C9 C14 C1 -179.3(5) . . . . ? C8 C9 C14 C13 -179.7(5) . . . . ? C10 C9 C14 C13 -1.2(8) . . . . ? C18 O1 C15 C16 16.1(10) . . . . ? Li1 O1 C15 C16 -147.6(6) . . . . ? O1 C15 C16 C17 -31.2(9) . . . . ? C15 C16 C17 C18 35.0(9) . . . . ? C15 O1 C18 C17 6.4(10) . . . . ? Li1 O1 C18 C17 168.1(6) . . . . ? C16 C17 C18 O1 -26.3(9) . . . . ? C22 O2 C19 C20 36.0(7) . . . . ? Li1 O2 C19 C20 -161.3(5) . . . . ? O2 C19 C20 C21 -15.1(7) . . . . ? C19 C20 C21 C22 -10.5(7) . . . . ? C19 O2 C22 C21 -42.4(6) . . . . ? Li1 O2 C22 C21 157.7(6) . . . . ? C20 C21 C22 O2 32.1(6) . . . . ? C26 O3 C23 C24 -42.3(7) . . . . ? Li2 O3 C23 C24 149.4(6) . . . . ? O3 C23 C24 C25 31.2(7) . . . . ? C23 C24 C25 C26 -9.3(7) . . . . ? C23 O3 C26 C25 35.7(7) . . . . ? Li2 O3 C26 C25 -154.3(5) . . . . ? C24 C25 C26 O3 -15.7(7) . . . . ? C30 O4 C27 C28 -36.3(7) . . . . ? Li2 O4 C27 C28 160.2(5) . . . . ? O4 C27 C28 C29 15.4(8) . . . . ? C27 C28 C29 C30 9.3(7) . . . . ? C27 O4 C30 C29 42.1(6) . . . . ? Li2 O4 C30 C29 -156.1(6) . . . . ? C28 C29 C30 O4 -31.2(7) . . . . ? C44 C31 C32 C33 179(2) . . . . ? Br5 C31 C32 C33 -1.2(19) . . . . ? C44 C31 C32 C37 -2(3) . . . . ? Br5 C31 C32 C37 176.9(14) . . . . ? C31 C32 C33 C34 178.1(14) . . . . ? C37 C32 C33 C34 0(2) . . . . ? C32 C33 C34 C35 -1(2) . . . . ? C33 C34 C35 C36 0(3) . . . . ? C34 C35 C36 C37 1(6) . . . . ? C35 C36 C37 C38 176(3) . . . . ? C35 C36 C37 C32 -2(6) . . . . ? C31 C32 C37 C38 6(3) . . . . ? C33 C32 C37 C38 -175.8(16) . . . . ? C31 C32 C37 C36 -177(3) . . . . ? C33 C32 C37 C36 1(4) . . . . ? C36 C37 C38 C39 174(4) . . . . ? C32 C37 C38 C39 -9(4) . . . . ? C36 C37 C38 Li4 -50(3) . . . . ? C32 C37 C38 Li4 127.1(18) . . . . ? C36 C37 C38 Li5 32(3) . . . . ? C32 C37 C38 Li5 -151.2(16) . . . . ? O10 Li4 C38 C37 -12.7(13) . . . . ? O9' Li4 C38 C37 -111.4(12) . . . . ? O9 Li4 C38 C37 -136.4(10) . . . . ? O10' Li4 C38 C37 -7.6(11) . . . . ? Br3 Li4 C38 C37 110.1(10) . . . . ? O10 Li4 C38 C39 121(3) . . . . ? O9' Li4 C38 C39 22(3) . . . . ? O9 Li4 C38 C39 -3(3) . . . . ? O10' Li4 C38 C39 126(3) . . . . ? Br3 Li4 C38 C39 -116(3) . . . . ? O10 Li4 C38 Li5 -129.2(9) . . . . ? O9' Li4 C38 Li5 132.0(9) . . . . ? O9 Li4 C38 Li5 107.0(7) . . . . ? O10' Li4 C38 Li5 -124.2(7) . . . . ? Br3 Li4 C38 Li5 -6.5(5) . . . . ? O7' Li5 C38 C37 25.2(15) . . . . ? O8 Li5 C38 C37 125.4(13) . . . . ? O8' Li5 C38 C37 150.1(12) . . . . ? O7 Li5 C38 C37 20.4(13) . . . . ? Br3 Li5 C38 C37 -95.8(12) . . . . ? O7' Li5 C38 C39 -117(3) . . . . ? O8 Li5 C38 C39 -17(3) . . . . ? O8' Li5 C38 C39 8(3) . . . . ? O7 Li5 C38 C39 -122(3) . . . . ? Br3 Li5 C38 C39 122(3) . . . . ? O7' Li5 C38 Li4 127.5(9) . . . . ? O8 Li5 C38 Li4 -132.3(9) . . . . ? O8' Li5 C38 Li4 -107.6(7) . . . . ? O7 Li5 C38 Li4 122.7(7) . . . . ? Br3 Li5 C38 Li4 6.4(5) . . . . ? C37 C38 C39 C40 -179(4) . . . . ? Li4 C38 C39 C40 50(6) . . . . ? Li5 C38 C39 C40 -35(6) . . . . ? C37 C38 C39 C44 9(7) . . . . ? Li4 C38 C39 C44 -122(4) . . . . ? Li5 C38 C39 C44 153(4) . . . . ? C38 C39 C40 C41 -176(4) . . . . ? C44 C39 C40 C41 -3(7) . . . . ? C39 C40 C41 C42 -1(6) . . . . ? C40 C41 C42 C43 3(8) . . . . ? C41 C42 C43 C44 -1(9) . . . . ? C32 C31 C44 C43 180(3) . . . . ? Br5 C31 C44 C43 0(5) . . . . ? C32 C31 C44 C39 2(5) . . . . ? Br5 C31 C44 C39 -177(4) . . . . ? C42 C43 C44 C31 -180(5) . . . . ? C42 C43 C44 C39 -3(7) . . . . ? C38 C39 C44 C31 -6(7) . . . . ? C40 C39 C44 C31 -178(4) . . . . ? C38 C39 C44 C43 177(5) . . . . ? C40 C39 C44 C43 4(7) . . . . ? C44' C31' C32' C33' 177(2) . . . . ? Br5' C31' C32' C33' 2.0(19) . . . . ? C44' C31' C32' C37' -3(3) . . . . ? Br5' C31' C32' C37' -178.2(14) . . . . ? C31' C32' C33' C34' -178.6(13) . . . . ? C37' C32' C33' C34' 2(2) . . . . ? C32' C33' C34' C35' -1(2) . . . . ? C33' C34' C35' C36' 1(4) . . . . ? C34' C35' C36' C37' -2(6) . . . . ? C35' C36' C37' C32' 3(6) . . . . ? C31' C32' C37' C36' 178(3) . . . . ? C33' C32' C37' C36' -3(4) . . . . ? C44' C39' C40' C41' 2(7) . . . . ? C39' C40' C41' C42' 0(6) . . . . ? C40' C41' C42' C43' -2(8) . . . . ? C41' C42' C43' C44' 4(9) . . . . ? C32' C31' C44' C43' 179(3) . . . . ? Br5' C31' C44' C43' -6(5) . . . . ? C32' C31' C44' C39' 4(5) . . . . ? Br5' C31' C44' C39' 179(4) . . . . ? C42' C43' C44' C31' -177(5) . . . . ? C42' C43' C44' C39' -2(7) . . . . ? C40' C39' C44' C31' 175(4) . . . . ? C40' C39' C44' C43' -1(7) . . . . ? C58 C45 C46 C47 -179.4(5) . . . . ? Br4 C45 C46 C47 0.6(8) . . . . ? C58 C45 C46 C51 1.0(8) . . . . ? Br4 C45 C46 C51 -179.0(4) . . . . ? C45 C46 C47 C48 -179.6(6) . . . . ? C51 C46 C47 C48 0.0(9) . . . . ? C46 C47 C48 C49 0.6(9) . . . . ? C47 C48 C49 C50 -1.3(9) . . . . ? C48 C49 C50 C51 1.3(10) . . . . ? C49 C50 C51 C52 179.3(6) . . . . ? C49 C50 C51 C46 -0.6(9) . . . . ? C45 C46 C51 C52 -0.4(8) . . . . ? C47 C46 C51 C52 -180.0(5) . . . . ? C45 C46 C51 C50 179.5(5) . . . . ? C47 C46 C51 C50 -0.1(8) . . . . ? C50 C51 C52 C53 179.5(5) . . . . ? C46 C51 C52 C53 -0.6(8) . . . . ? C50 C51 C52 Li3 -1.5(8) . . . . ? C46 C51 C52 Li3 178.4(5) . . . . ? O5 Li3 C52 C51 117.5(6) . . . . ? O6 Li3 C52 C51 -115.5(6) . . . . ? Br3 Li3 C52 C51 0.0(9) . . . . ? O5 Li3 C52 C53 -63.7(7) . . . . ? O6 Li3 C52 C53 63.3(7) . . . . ? Br3 Li3 C52 C53 178.9(5) . . . . ? C51 C52 C53 C54 -179.9(5) . . . . ? Li3 C52 C53 C54 1.1(8) . . . . ? C51 C52 C53 C58 0.9(8) . . . . ? Li3 C52 C53 C58 -178.0(5) . . . . ? C52 C53 C54 C55 -179.9(5) . . . . ? C58 C53 C54 C55 -0.7(8) . . . . ? C53 C54 C55 C56 1.1(9) . . . . ? C54 C55 C56 C57 -1.2(9) . . . . ? C55 C56 C57 C58 0.9(9) . . . . ? C46 C45 C58 C57 179.4(5) . . . . ? Br4 C45 C58 C57 -0.6(8) . . . . ? C46 C45 C58 C53 -0.7(8) . . . . ? Br4 C45 C58 C53 179.3(4) . . . . ? C56 C57 C58 C45 179.4(6) . . . . ? C56 C57 C58 C53 -0.6(8) . . . . ? C52 C53 C58 C45 -0.4(8) . . . . ? C54 C53 C58 C45 -179.5(5) . . . . ? C52 C53 C58 C57 179.6(5) . . . . ? C54 C53 C58 C57 0.4(8) . . . . ? C62 O5 C59 C60 38.8(7) . . . . ? Li3 O5 C59 C60 -137.9(6) . . . . ? O5 C59 C60 C61 -25.4(8) . . . . ? C59 C60 C61 C62 3.5(9) . . . . ? C59 O5 C62 C61 -36.1(7) . . . . ? Li3 O5 C62 C61 139.8(7) . . . . ? C60 C61 C62 O5 19.3(9) . . . . ? C74 O6 C71 C72 35.8(7) . . . . ? Li3 O6 C71 C72 -140.7(7) . . . . ? O6 C71 C72 C73 -18.6(9) . . . . ? C71 C72 C73 C74 -4.3(9) . . . . ? C71 O6 C74 C73 -38.6(7) . . . . ? Li3 O6 C74 C73 138.6(6) . . . . ? C72 C73 C74 O6 26.1(8) . . . . ? O7' Li5 O7 C83 56(5) . . . . ? O8 Li5 O7 C83 91(2) . . . . ? O8' Li5 O7 C83 90(3) . . . . ? C38 Li5 O7 C83 -144(2) . . . . ? Br3 Li5 O7 C83 -26(3) . . . . ? O7' Li5 O7 C80 -109(5) . . . . ? O8 Li5 O7 C80 -73.9(16) . . . . ? O8' Li5 O7 C80 -74.8(18) . . . . ? C38 Li5 O7 C80 50.9(18) . . . . ? Br3 Li5 O7 C80 169.1(14) . . . . ? C83 O7 C80 C81 32(3) . . . . ? Li5 O7 C80 C81 -160.8(16) . . . . ? O7 C80 C81 C82 -31(3) . . . . ? C80 C81 C82 C83 21(4) . . . . ? C80 O7 C83 C82 -18(3) . . . . ? Li5 O7 C83 C82 175(2) . . . . ? C81 C82 C83 O7 -3(4) . . . . ? O8 Li5 O7' C80' -70.1(17) . . . . ? O8' Li5 O7' C80' -74.1(18) . . . . ? O7 Li5 O7' C80' 74(4) . . . . ? C38 Li5 O7' C80' 52(2) . . . . ? Br3 Li5 O7' C80' 176.0(16) . . . . ? O8 Li5 O7' C83' 134(3) . . . . ? O8' Li5 O7' C83' 130(3) . . . . ? O7 Li5 O7' C83' -81(5) . . . . ? C38 Li5 O7' C83' -103(3) . . . . ? Br3 Li5 O7' C83' 20(3) . . . . ? C83' O7' C80' C81' 7(3) . . . . ? Li5 O7' C80' C81' -153.8(15) . . . . ? O7' C80' C81' C82' -27(2) . . . . ? C80' C81' C82' C83' 37(3) . . . . ? C80' O7' C83' C82' 17(4) . . . . ? Li5 O7' C83' C82' 174(2) . . . . ? C81' C82' C83' O7' -34(4) . . . . ? O7' Li5 O8 C87 108.9(19) . . . . ? O8' Li5 O8 C87 -80(2) . . . . ? O7 Li5 O8 C87 101.8(19) . . . . ? C38 Li5 O8 C87 -12(2) . . . . ? Br3 Li5 O8 C87 -148.7(17) . . . . ? O7' Li5 O8 C84 -54.1(14) . . . . ? O8' Li5 O8 C84 116.9(17) . . . . ? O7 Li5 O8 C84 -61.2(13) . . . . ? C38 Li5 O8 C84 -175.0(11) . . . . ? Br3 Li5 O8 C84 48.3(14) . . . . ? C87 O8 C84 C85 41.4(18) . . . . ? Li5 O8 C84 C85 -150.0(12) . . . . ? O8 C84 C85 C86 -21.6(19) . . . . ? C84 C85 C86 C87 -4(2) . . . . ? C84 O8 C87 C86 -41.2(17) . . . . ? Li5 O8 C87 C86 154.8(15) . . . . ? C85 C86 C87 O8 27.6(19) . . . . ? O7' Li5 O8' C87' 77.3(15) . . . . ? O8 Li5 O8' C87' 67.9(15) . . . . ? O7 Li5 O8' C87' 70.1(15) . . . . ? C38 Li5 O8' C87' -54.9(15) . . . . ? Br3 Li5 O8' C87' -172.4(12) . . . . ? O7' Li5 O8' C84' -76.8(14) . . . . ? O8 Li5 O8' C84' -86.2(14) . . . . ? O7 Li5 O8' C84' -84.0(13) . . . . ? C38 Li5 O8' C84' 151.0(10) . . . . ? Br3 Li5 O8' C84' 33.4(13) . . . . ? C87' O8' C84' C85' 37.0(14) . . . . ? Li5 O8' C84' C85' -164.0(10) . . . . ? O8' C84' C85' C86' -17.0(15) . . . . ? C84' C85' C86' C87' -7.5(15) . . . . ? C84' O8' C87' C86' -42.5(15) . . . . ? Li5 O8' C87' C86' 159.5(11) . . . . ? C85' C86' C87' O8' 30.1(16) . . . . ? O10 Li4 O9 C91 -77.7(15) . . . . ? O9' Li4 O9 C91 -68.1(15) . . . . ? O10' Li4 O9 C91 -68.1(15) . . . . ? C38 Li4 O9 C91 54.6(15) . . . . ? Br3 Li4 O9 C91 172.2(13) . . . . ? O10 Li4 O9 C88 78.7(13) . . . . ? O9' Li4 O9 C88 88.3(15) . . . . ? O10' Li4 O9 C88 88.3(13) . . . . ? C38 Li4 O9 C88 -148.9(11) . . . . ? Br3 Li4 O9 C88 -31.3(13) . . . . ? C91 O9 C88 C89 -35.7(15) . . . . ? Li4 O9 C88 C89 163.6(10) . . . . ? O9 C88 C89 C90 16.5(15) . . . . ? C88 C89 C90 C91 7.0(15) . . . . ? C88 O9 C91 C90 40.6(16) . . . . ? Li4 O9 C91 C90 -159.5(11) . . . . ? C89 C90 C91 O9 -28.9(16) . . . . ? O10 Li4 O9' C91' -111(2) . . . . ? O9 Li4 O9' C91' 79(2) . . . . ? O10' Li4 O9' C91' -101(2) . . . . ? C38 Li4 O9' C91' 11(2) . . . . ? Br3 Li4 O9' C91' 147.3(19) . . . . ? O10 Li4 O9' C88' 53.8(13) . . . . ? O9 Li4 O9' C88' -116.8(16) . . . . ? O10' Li4 O9' C88' 63.2(13) . . . . ? C38 Li4 O9' C88' 175.0(12) . . . . ? Br3 Li4 O9' C88' -48.3(14) . . . . ? C91' O9' C88' C89' -41.6(19) . . . . ? Li4 O9' C88' C89' 148.3(13) . . . . ? O9' C88' C89' C90' 22(2) . . . . ? C88' C89' C90' C91' 4(2) . . . . ? C88' O9' C91' C90' 42.5(18) . . . . ? Li4 O9' C91' C90' -152.1(16) . . . . ? C89' C90' C91' O9' -29(2) . . . . ? O9' Li4 O10 C95 -118(2) . . . . ? O9 Li4 O10 C95 -114(2) . . . . ? O10' Li4 O10 C95 102(4) . . . . ? C38 Li4 O10 C95 121(2) . . . . ? Br3 Li4 O10 C95 -4(2) . . . . ? O9' Li4 O10 C92 72.2(15) . . . . ? O9 Li4 O10 C92 76.4(15) . . . . ? O10' Li4 O10 C92 -68(3) . . . . ? C38 Li4 O10 C92 -48.9(17) . . . . ? Br3 Li4 O10 C92 -174.2(14) . . . . ? C95 O10 C92 C93 -18(2) . . . . ? Li4 O10 C92 C93 155.5(15) . . . . ? O10 C92 C93 C94 28(2) . . . . ? C92 C93 C94 C95 -28(3) . . . . ? C93 C94 C95 O10 19(3) . . . . ? C92 O10 C95 C94 -1(3) . . . . ? Li4 O10 C95 C94 -171.6(18) . . . . ? O10 Li4 O10' C95' -66(3) . . . . ? O9' Li4 O10' C95' -104.5(16) . . . . ? O9 Li4 O10' C95' -104.5(16) . . . . ? C38 Li4 O10' C95' 131.7(15) . . . . ? Br3 Li4 O10' C95' 12.8(17) . . . . ? O10 Li4 O10' C92' 108(3) . . . . ? O9' Li4 O10' C92' 68.9(14) . . . . ? O9 Li4 O10' C92' 68.9(15) . . . . ? C38 Li4 O10' C92' -54.9(14) . . . . ? Br3 Li4 O10' C92' -173.8(12) . . . . ? C95' O10' C92' C93' -13(2) . . . . ? Li4 O10' C92' C93' 172.4(15) . . . . ? O10' C92' C93' C94' 25(3) . . . . ? C92' C93' C94' C95' -28(3) . . . . ? C93' C94' C95' O10' 21(3) . . . . ? C92' O10' C95' C94' -5(3) . . . . ? Li4 O10' C95' C94' 169.1(19) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.14 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 3.952 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.139 # Attachment '4_BrAnLi_LiBr_2DME.cif' data_4_BrAnLi_LiBr_2DME _database_code_depnum_ccdc_archive 'CCDC 766247' #TrackingRef '4_BrAnLi_LiBr_2DME.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H28.25 Br1.75 Li2 O4' _chemical_formula_weight 510.22 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.891(3) _cell_length_b 8.2807(13) _cell_length_c 32.847(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.332(2) _cell_angle_gamma 90.00 _cell_volume 5304.7(14) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6314 _cell_measurement_theta_min 2.219 _cell_measurement_theta_max 24.297 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2075 _exptl_absorpt_coefficient_mu 2.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6425 _exptl_absorpt_correction_T_max 0.8132 _exptl_absorpt_process_details SADABS-2008/2 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'micro-focus sealed tube' _diffrn_radiation_monochromator 'multilayer mirror optics' _diffrn_measurement_device_type 'Bruker Smart APEXII Quazar' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30017 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.39 _reflns_number_total 4837 _reflns_number_gt 3802 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2.2-0' _computing_cell_refinement 'SAINT V7.46A' _computing_data_reduction 'SAINT V7.46A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL v6.10' _computing_publication_material 'XP in SHELXTL v6.10' _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^)+(0.0546P)^2^+21.9085P] 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 4837 _refine_ls_number_parameters 330 _refine_ls_number_restraints 610 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1355 _refine_ls_wR_factor_gt 0.1287 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.174 0.250 152 26 ' ' 2 0.500 -0.174 0.750 152 26 ' ' 3 0.000 0.326 0.750 152 26 ' ' 4 0.000 0.674 0.250 152 26 ' ' _platon_squeeze_details ; The structure contain one pentane molecule on special position wich could not be resolved propably. Therefore the SQUEEZE algorithm of PLATON was used to take this diffuse electron denity into account. ; 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 Br1 Br 0.06976(3) -0.16365(10) 0.80726(2) 0.0654(3) Uani 0.737(3) 1 d PU A 1 Br2 Br 0.42472(2) 0.32270(5) 0.946358(14) 0.04403(16) Uani 1 1 d U B . Li1 Li 0.3204(3) 0.3475(8) 0.8925(2) 0.0418(12) Uani 1 1 d U . . Li2 Li 0.3735(4) 0.0581(8) 0.9203(2) 0.0424(12) Uani 1 1 d U . . O1 O 0.34378(15) 0.4871(4) 0.84678(9) 0.0484(7) Uani 1 1 d U . . O2 O 0.25768(16) 0.5275(4) 0.89872(10) 0.0555(8) Uani 1 1 d U . . C1 C 0.1490(2) -0.0445(6) 0.83587(15) 0.0532(10) Uani 1 1 d U . . H1 H 0.1084 -0.0954 0.8215 0.064 Uiso 0.263(3) 1 calc PR A 1 C2 C 0.2018(2) -0.0198(6) 0.81472(14) 0.0513(10) Uani 1 1 d U A . C3 C 0.2009(3) -0.0706(7) 0.77286(16) 0.0713(14) Uani 1 1 d U . . H3 H 0.1611 -0.1217 0.7575 0.086 Uiso 1 1 calc R A . C4 C 0.2554(4) -0.0472(8) 0.75492(17) 0.0808(16) Uani 1 1 d U A . H4 H 0.2536 -0.0837 0.7273 0.097 Uiso 1 1 calc R . . C5 C 0.3148(4) 0.0297(7) 0.77601(17) 0.0746(15) Uani 1 1 d U . . H5 H 0.3525 0.0463 0.7627 0.090 Uiso 1 1 calc R A . C6 C 0.3181(3) 0.0802(6) 0.81562(15) 0.0571(11) Uani 1 1 d U A . H6 H 0.3584 0.1339 0.8294 0.069 Uiso 1 1 calc R . . C7 C 0.2636(2) 0.0563(5) 0.83739(13) 0.0446(9) Uani 1 1 d U . . C8 C 0.2722(2) 0.1061(5) 0.87903(13) 0.0407(8) Uani 1 1 d U A . C9 C 0.2151(2) 0.0760(5) 0.89796(13) 0.0391(8) Uani 1 1 d U . . C10 C 0.2186(2) 0.1215(6) 0.94060(15) 0.0493(10) Uani 1 1 d U A . H10 H 0.2593 0.1712 0.9552 0.059 Uiso 1 1 calc R . . C11 C 0.1659(3) 0.0962(6) 0.96091(16) 0.0555(11) Uani 1 1 d U . . H11 H 0.1701 0.1294 0.9890 0.067 Uiso 1 1 calc R A . C12 C 0.1061(2) 0.0216(6) 0.94036(17) 0.0546(11) Uani 1 1 d U A . H12 H 0.0696 0.0033 0.9546 0.066 Uiso 1 1 calc R . . C13 C 0.0994(2) -0.0251(6) 0.90024(17) 0.0539(10) Uani 1 1 d U . . H13 H 0.0582 -0.0771 0.8871 0.065 Uiso 1 1 calc R A . C14 C 0.1519(2) 0.0010(5) 0.87689(14) 0.0440(9) Uani 1 1 d U A . C15 C 0.4089(2) 0.4931(7) 0.83550(17) 0.0646(14) Uani 1 1 d U . . H15A H 0.4047 0.5453 0.8083 0.097 Uiso 1 1 calc R . . H15B H 0.4265 0.3831 0.8340 0.097 Uiso 1 1 calc R . . H15C H 0.4407 0.5551 0.8563 0.097 Uiso 1 1 calc R . . C16 C 0.3177(3) 0.6439(5) 0.85079(17) 0.0600(12) Uani 1 1 d U . . H16A H 0.3123 0.7023 0.8240 0.072 Uiso 1 1 calc R . . H16B H 0.3497 0.7058 0.8720 0.072 Uiso 1 1 calc R . . C17 C 0.2502(3) 0.6277(7) 0.86331(17) 0.0674(13) Uani 1 1 d U . . H17A H 0.2334 0.7354 0.8697 0.081 Uiso 1 1 calc R . . H17B H 0.2164 0.5800 0.8403 0.081 Uiso 1 1 calc R . . C18 C 0.1963(3) 0.5190(9) 0.9150(2) 0.095(2) Uani 1 1 d U . . H18A H 0.1827 0.6280 0.9217 0.143 Uiso 1 1 calc R . . H18B H 0.2044 0.4527 0.9402 0.143 Uiso 1 1 calc R . . H18C H 0.1597 0.4704 0.8943 0.143 Uiso 1 1 calc R . . O3 O 0.447(2) -0.098(7) 0.9064(14) 0.067(4) Uani 0.104(11) 1 d PDU B 1 O4 O 0.379(3) -0.080(5) 0.9679(19) 0.061(4) Uani 0.104(11) 1 d PDU B 1 C19 C 0.336(3) -0.093(7) 0.9979(16) 0.076(8) Uani 0.104(11) 1 d PDU B 1 H19A H 0.3107 -0.1962 0.9940 0.115 Uiso 0.104(11) 1 calc PR B 1 H19B H 0.3026 -0.0039 0.9944 0.115 Uiso 0.104(11) 1 calc PR B 1 H19C H 0.3638 -0.0896 1.0259 0.115 Uiso 0.104(11) 1 calc PR B 1 C20 C 0.411(3) -0.230(4) 0.9617(16) 0.071(4) Uani 0.104(11) 1 d PDU B 1 H20A H 0.3770 -0.3020 0.9444 0.085 Uiso 0.104(11) 1 calc PR B 1 H20B H 0.4270 -0.2831 0.9888 0.085 Uiso 0.104(11) 1 calc PR B 1 C21 C 0.468(3) -0.202(7) 0.9412(17) 0.076(4) Uani 0.104(11) 1 d PDU B 1 H21A H 0.5065 -0.1513 0.9610 0.092 Uiso 0.104(11) 1 calc PR B 1 H21B H 0.4845 -0.3057 0.9319 0.092 Uiso 0.104(11) 1 calc PR B 1 C22 C 0.503(3) -0.056(9) 0.887(2) 0.085(9) Uani 0.104(11) 1 d PDU B 1 H22A H 0.5299 0.0293 0.9038 0.127 Uiso 0.104(11) 1 calc PR B 1 H22B H 0.4851 -0.0164 0.8593 0.127 Uiso 0.104(11) 1 calc PR B 1 H22C H 0.5317 -0.1507 0.8863 0.127 Uiso 0.104(11) 1 calc PR B 1 O3' O 0.4543(3) -0.0548(7) 0.90407(19) 0.0727(14) Uani 0.896(11) 1 d PDU B 2 O4' O 0.3813(4) -0.1185(6) 0.9618(2) 0.0653(13) Uani 0.896(11) 1 d PDU B 2 C19' C 0.3312(4) -0.2010(9) 0.9798(2) 0.087(2) Uani 0.896(11) 1 d PDU B 2 H19D H 0.3236 -0.3092 0.9677 0.131 Uiso 0.896(11) 1 calc PR B 2 H19E H 0.2880 -0.1403 0.9743 0.131 Uiso 0.896(11) 1 calc PR B 2 H19F H 0.3475 -0.2101 1.0099 0.131 Uiso 0.896(11) 1 calc PR B 2 C20' C 0.4402(4) -0.2158(8) 0.9605(3) 0.0834(18) Uani 0.896(11) 1 d PDU B 2 H20C H 0.4266 -0.3130 0.9433 0.100 Uiso 0.896(11) 1 calc PR B 2 H20D H 0.4616 -0.2514 0.9888 0.100 Uiso 0.896(11) 1 calc PR B 2 C21' C 0.4890(4) -0.1201(10) 0.9427(2) 0.0855(18) Uani 0.896(11) 1 d PDU B 2 H21C H 0.5077 -0.0317 0.9619 0.103 Uiso 0.896(11) 1 calc PR B 2 H21D H 0.5276 -0.1889 0.9382 0.103 Uiso 0.896(11) 1 calc PR B 2 C22' C 0.4992(4) 0.0292(14) 0.8832(3) 0.113(3) Uani 0.896(11) 1 d PDU B 2 H22D H 0.5209 0.1181 0.9007 0.169 Uiso 0.896(11) 1 calc PR B 2 H22E H 0.4733 0.0726 0.8570 0.169 Uiso 0.896(11) 1 calc PR B 2 H22F H 0.5346 -0.0449 0.8774 0.169 Uiso 0.896(11) 1 calc PR B 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 Br1 0.0440(4) 0.0718(5) 0.0713(5) -0.0141(4) -0.0108(3) -0.0109(3) Br2 0.0388(2) 0.0343(2) 0.0551(3) 0.0021(2) -0.00013(18) -0.00391(19) Li1 0.037(3) 0.034(2) 0.053(4) 0.006(2) 0.005(2) -0.0001(19) Li2 0.041(3) 0.031(2) 0.053(3) 0.003(2) 0.005(2) 0.001(2) O1 0.0435(16) 0.0438(16) 0.0559(17) 0.0103(14) 0.0051(13) -0.0033(13) O2 0.0533(18) 0.0456(17) 0.067(2) 0.0086(15) 0.0106(15) 0.0148(15) C1 0.038(2) 0.050(3) 0.063(2) 0.006(2) -0.0111(17) 0.0006(19) C2 0.054(2) 0.044(2) 0.049(2) 0.0062(19) -0.0046(17) 0.0049(19) C3 0.086(3) 0.070(4) 0.048(2) 0.002(2) -0.010(2) -0.002(3) C4 0.126(5) 0.075(4) 0.042(3) 0.000(3) 0.017(3) -0.005(3) C5 0.113(4) 0.062(3) 0.058(3) 0.004(3) 0.040(3) -0.011(3) C6 0.077(3) 0.043(3) 0.055(2) 0.005(2) 0.021(2) -0.008(2) C7 0.056(2) 0.034(2) 0.0424(19) 0.0086(17) 0.0056(16) -0.0012(18) C8 0.0411(18) 0.0330(18) 0.0471(19) 0.0032(16) 0.0067(14) -0.0024(15) C9 0.0378(19) 0.0241(19) 0.053(2) 0.0017(17) 0.0046(16) 0.0010(15) C10 0.050(2) 0.044(2) 0.055(2) 0.001(2) 0.0131(19) -0.007(2) C11 0.059(3) 0.045(3) 0.068(3) 0.006(2) 0.025(2) 0.001(2) C12 0.044(2) 0.043(3) 0.083(3) 0.015(2) 0.027(2) 0.0060(19) C13 0.032(2) 0.042(2) 0.085(3) 0.012(2) 0.006(2) 0.0014(19) C14 0.0342(19) 0.034(2) 0.060(2) 0.0082(18) -0.0006(16) 0.0022(16) C15 0.049(3) 0.072(3) 0.073(3) 0.019(3) 0.013(2) -0.008(2) C16 0.074(3) 0.035(2) 0.068(3) 0.012(2) 0.006(2) 0.003(2) C17 0.068(3) 0.061(3) 0.069(3) 0.014(2) 0.001(2) 0.027(2) C18 0.084(4) 0.087(5) 0.128(5) 0.015(4) 0.054(4) 0.036(4) O3 0.056(7) 0.046(7) 0.095(8) -0.008(6) 0.005(6) 0.017(6) O4 0.071(9) 0.035(6) 0.068(9) 0.016(7) -0.003(6) 0.000(7) C19 0.103(18) 0.062(18) 0.060(15) 0.025(13) 0.006(12) -0.006(15) C20 0.073(9) 0.035(4) 0.091(9) 0.009(6) -0.021(7) 0.003(6) C21 0.064(8) 0.044(8) 0.108(9) -0.003(7) -0.016(7) 0.015(6) C22 0.061(15) 0.08(2) 0.118(17) -0.012(15) 0.024(13) 0.028(13) O3' 0.055(2) 0.057(3) 0.104(3) -0.014(2) 0.009(2) 0.019(2) O4' 0.079(2) 0.033(2) 0.073(3) 0.011(2) -0.0146(19) -0.004(2) C19' 0.141(5) 0.056(4) 0.064(4) 0.024(3) 0.020(4) -0.009(4) C20' 0.081(4) 0.037(3) 0.108(5) 0.003(3) -0.040(3) 0.009(3) C21' 0.061(3) 0.051(4) 0.127(5) -0.015(3) -0.022(3) 0.022(3) C22' 0.066(5) 0.130(8) 0.157(7) 0.000(6) 0.056(5) 0.036(5) _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 Br1 C1 1.938(5) . ? Br2 Li1 2.457(7) . ? Br2 Li2 2.496(7) . ? Li1 O2 1.980(7) . ? Li1 O1 2.019(7) . ? Li1 C8 2.224(8) . ? Li2 O4 1.92(4) . ? Li2 O4' 1.985(9) . ? Li2 O3' 2.019(9) . ? Li2 O3 2.07(4) . ? Li2 C8 2.232(8) . ? Li2 C20 2.77(4) . ? O1 C16 1.414(6) . ? O1 C15 1.417(5) . ? O2 C17 1.413(6) . ? O2 C18 1.427(6) . ? C1 C2 1.385(7) . ? C1 C14 1.389(7) . ? C1 H1 0.9500 . ? C2 C3 1.435(7) . ? C2 C7 1.450(6) . ? C3 C4 1.346(9) . ? C3 H3 0.9500 . ? C4 C5 1.399(9) . ? C4 H4 0.9500 . ? C5 C6 1.356(7) . ? C5 H5 0.9500 . ? C6 C7 1.424(7) . ? C6 H6 0.9500 . ? C7 C8 1.407(6) . ? C8 C9 1.419(6) . ? C9 C10 1.439(6) . ? C9 C14 1.450(6) . ? C10 C11 1.365(6) . ? C10 H10 0.9500 . ? C11 C12 1.393(7) . ? C11 H11 0.9500 . ? C12 C13 1.354(7) . ? C12 H12 0.9500 . ? C13 C14 1.429(6) . ? C13 H13 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.485(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O3 C22 1.411(13) . ? O3 C21 1.424(12) . ? O4 C19 1.432(12) . ? O4 C20 1.431(13) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.455(14) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? O3' C22' 1.411(9) . ? O3' C21' 1.426(8) . ? O4' C19' 1.429(8) . ? O4' C20' 1.431(9) . ? C19' H19D 0.9800 . ? C19' H19E 0.9800 . ? C19' H19F 0.9800 . ? C20' C21' 1.461(10) . ? C20' H20C 0.9900 . ? C20' H20D 0.9900 . ? C21' H21C 0.9900 . ? C21' H21D 0.9900 . ? C22' H22D 0.9800 . ? C22' H22E 0.9800 . ? C22' H22F 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 Li1 Br2 Li2 66.2(2) . . ? O2 Li1 O1 83.6(3) . . ? O2 Li1 C8 116.2(4) . . ? O1 Li1 C8 121.4(4) . . ? O2 Li1 Br2 116.6(3) . . ? O1 Li1 Br2 107.4(3) . . ? C8 Li1 Br2 109.8(3) . . ? O4 Li2 O4' 11.3(14) . . ? O4 Li2 O3' 91.3(12) . . ? O4' Li2 O3' 83.2(3) . . ? O4 Li2 O3 83.3(13) . . ? O4' Li2 O3 74.3(12) . . ? O3' Li2 O3 11.0(14) . . ? O4 Li2 C8 119.8(19) . . ? O4' Li2 C8 119.2(4) . . ? O3' Li2 C8 126.4(4) . . ? O3 Li2 C8 124.9(15) . . ? O4 Li2 Br2 107(2) . . ? O4' Li2 Br2 116.0(4) . . ? O3' Li2 Br2 101.8(3) . . ? O3 Li2 Br2 111.3(17) . . ? C8 Li2 Br2 108.1(3) . . ? O4 Li2 C20 28.9(8) . . ? O4' Li2 C20 18.6(10) . . ? O3' Li2 C20 65.3(10) . . ? O3 Li2 C20 55.9(9) . . ? C8 Li2 C20 125.0(13) . . ? Br2 Li2 C20 122.3(12) . . ? C16 O1 C15 111.3(4) . . ? C16 O1 Li1 108.3(3) . . ? C15 O1 Li1 124.8(3) . . ? C17 O2 C18 112.2(4) . . ? C17 O2 Li1 108.8(4) . . ? C18 O2 Li1 127.2(4) . . ? C2 C1 C14 123.7(4) . . ? C2 C1 Br1 117.2(4) . . ? C14 C1 Br1 119.0(4) . . ? C2 C1 H1 118.2 . . ? C14 C1 H1 118.2 . . ? Br1 C1 H1 4.3 . . ? C1 C2 C3 124.7(5) . . ? C1 C2 C7 117.2(4) . . ? C3 C2 C7 118.0(5) . . ? C4 C3 C2 121.2(6) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 121.5(5) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 119.5(6) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C7 122.8(5) . . ? C5 C6 H6 118.6 . . ? C7 C6 H6 118.6 . . ? C8 C7 C6 119.3(4) . . ? C8 C7 C2 123.7(4) . . ? C6 C7 C2 117.0(4) . . ? C7 C8 C9 114.9(4) . . ? C7 C8 Li1 114.9(3) . . ? C9 C8 Li1 115.0(3) . . ? C7 C8 Li2 117.4(4) . . ? C9 C8 Li2 114.0(3) . . ? Li1 C8 Li2 74.7(3) . . ? C8 C9 C10 119.4(4) . . ? C8 C9 C14 124.0(4) . . ? C10 C9 C14 116.6(4) . . ? C11 C10 C9 122.7(4) . . ? C11 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? C10 C11 C12 119.8(5) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 120.6(4) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 122.5(4) . . ? C12 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C1 C14 C13 125.7(4) . . ? C1 C14 C9 116.5(4) . . ? C13 C14 C9 117.7(4) . . ? O1 C15 H15A 109.5 . . ? O1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O1 C16 C17 108.1(4) . . ? O1 C16 H16A 110.1 . . ? C17 C16 H16A 110.1 . . ? O1 C16 H16B 110.1 . . ? C17 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? O2 C17 C16 109.1(4) . . ? O2 C17 H17A 109.9 . . ? C16 C17 H17A 109.9 . . ? O2 C17 H17B 109.9 . . ? C16 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? O2 C18 H18A 109.5 . . ? O2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22 O3 C21 111.9(16) . . ? C22 O3 Li2 126(4) . . ? C21 O3 Li2 107.8(19) . . ? C19 O4 C20 111.9(16) . . ? C19 O4 Li2 132(3) . . ? C20 O4 Li2 111(2) . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O4 C20 C21 109.9(16) . . ? O4 C20 Li2 40.5(16) . . ? C21 C20 Li2 78.1(14) . . ? O4 C20 H20A 109.7 . . ? C21 C20 H20A 109.7 . . ? Li2 C20 H20A 98.8 . . ? O4 C20 H20B 109.7 . . ? C21 C20 H20B 109.7 . . ? Li2 C20 H20B 146.5 . . ? H20A C20 H20B 108.2 . . ? O3 C21 C20 109.6(15) . . ? O3 C21 H21A 109.7 . . ? C20 C21 H21A 109.7 . . ? O3 C21 H21B 109.7 . . ? C20 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? O3 C22 H22A 109.5 . . ? O3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C22' O3' C21' 112.1(6) . . ? C22' O3' Li2 120.8(5) . . ? C21' O3' Li2 102.3(5) . . ? C19' O4' C20' 112.7(5) . . ? C19' O4' Li2 132.1(6) . . ? C20' O4' Li2 110.3(5) . . ? O4' C19' H19D 109.5 . . ? O4' C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? O4' C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? O4' C20' C21' 108.6(5) . . ? O4' C20' H20C 110.0 . . ? C21' C20' H20C 110.0 . . ? O4' C20' H20D 110.0 . . ? C21' C20' H20D 110.0 . . ? H20C C20' H20D 108.3 . . ? O3' C21' C20' 108.5(6) . . ? O3' C21' H21C 110.0 . . ? C20' C21' H21C 110.0 . . ? O3' C21' H21D 110.0 . . ? C20' C21' H21D 110.0 . . ? H21C C21' H21D 108.4 . . ? O3' C22' H22D 109.5 . . ? O3' C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? O3' C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 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 Li2 Br2 Li1 O2 143.1(4) . . . . ? Li2 Br2 Li1 O1 -125.4(4) . . . . ? Li2 Br2 Li1 C8 8.4(3) . . . . ? Li1 Br2 Li2 O4 -138.3(14) . . . . ? Li1 Br2 Li2 O4' -145.2(5) . . . . ? Li1 Br2 Li2 O3' 126.6(4) . . . . ? Li1 Br2 Li2 O3 132.4(12) . . . . ? Li1 Br2 Li2 C8 -8.3(3) . . . . ? Li1 Br2 Li2 C20 -165.3(12) . . . . ? O2 Li1 O1 C16 13.9(4) . . . . ? C8 Li1 O1 C16 130.7(4) . . . . ? Br2 Li1 O1 C16 -102.1(4) . . . . ? O2 Li1 O1 C15 148.0(4) . . . . ? C8 Li1 O1 C15 -95.3(5) . . . . ? Br2 Li1 O1 C15 32.0(5) . . . . ? O1 Li1 O2 C17 14.7(4) . . . . ? C8 Li1 O2 C17 -107.2(5) . . . . ? Br2 Li1 O2 C17 120.9(4) . . . . ? O1 Li1 O2 C18 154.2(5) . . . . ? C8 Li1 O2 C18 32.3(7) . . . . ? Br2 Li1 O2 C18 -99.5(6) . . . . ? C14 C1 C2 C3 177.8(5) . . . . ? Br1 C1 C2 C3 2.5(7) . . . . ? C14 C1 C2 C7 0.7(7) . . . . ? Br1 C1 C2 C7 -174.6(3) . . . . ? C1 C2 C3 C4 -177.6(5) . . . . ? C7 C2 C3 C4 -0.6(8) . . . . ? C2 C3 C4 C5 -1.0(9) . . . . ? C3 C4 C5 C6 0.8(10) . . . . ? C4 C5 C6 C7 1.1(9) . . . . ? C5 C6 C7 C8 177.2(5) . . . . ? C5 C6 C7 C2 -2.5(7) . . . . ? C1 C2 C7 C8 -0.3(7) . . . . ? C3 C2 C7 C8 -177.5(4) . . . . ? C1 C2 C7 C6 179.5(4) . . . . ? C3 C2 C7 C6 2.3(6) . . . . ? C6 C7 C8 C9 -179.6(4) . . . . ? C2 C7 C8 C9 0.1(6) . . . . ? C6 C7 C8 Li1 43.6(5) . . . . ? C2 C7 C8 Li1 -136.6(4) . . . . ? C6 C7 C8 Li2 -41.4(5) . . . . ? C2 C7 C8 Li2 138.3(4) . . . . ? O2 Li1 C8 C7 102.6(5) . . . . ? O1 Li1 C8 C7 3.8(6) . . . . ? Br2 Li1 C8 C7 -122.4(4) . . . . ? O2 Li1 C8 C9 -34.1(5) . . . . ? O1 Li1 C8 C9 -132.9(4) . . . . ? Br2 Li1 C8 C9 100.9(4) . . . . ? O2 Li1 C8 Li2 -143.9(4) . . . . ? O1 Li1 C8 Li2 117.3(4) . . . . ? Br2 Li1 C8 Li2 -8.9(3) . . . . ? O4 Li2 C8 C7 -118.4(17) . . . . ? O4' Li2 C8 C7 -105.5(5) . . . . ? O3' Li2 C8 C7 -1.4(6) . . . . ? O3 Li2 C8 C7 -14.8(17) . . . . ? Br2 Li2 C8 C7 119.2(4) . . . . ? C20 Li2 C8 C7 -84.6(12) . . . . ? O4 Li2 C8 C9 20.2(17) . . . . ? O4' Li2 C8 C9 33.1(6) . . . . ? O3' Li2 C8 C9 137.2(5) . . . . ? O3 Li2 C8 C9 123.7(16) . . . . ? Br2 Li2 C8 C9 -102.3(4) . . . . ? C20 Li2 C8 C9 54.0(13) . . . . ? O4 Li2 C8 Li1 131.1(17) . . . . ? O4' Li2 C8 Li1 144.0(5) . . . . ? O3' Li2 C8 Li1 -111.9(5) . . . . ? O3 Li2 C8 Li1 -125.4(16) . . . . ? Br2 Li2 C8 Li1 8.6(3) . . . . ? C20 Li2 C8 Li1 164.9(12) . . . . ? C7 C8 C9 C10 179.7(4) . . . . ? Li1 C8 C9 C10 -43.6(5) . . . . ? Li2 C8 C9 C10 40.1(5) . . . . ? C7 C8 C9 C14 -0.4(6) . . . . ? Li1 C8 C9 C14 136.3(4) . . . . ? Li2 C8 C9 C14 -140.0(4) . . . . ? C8 C9 C10 C11 -179.9(4) . . . . ? C14 C9 C10 C11 0.2(6) . . . . ? C9 C10 C11 C12 0.9(7) . . . . ? C10 C11 C12 C13 -0.5(7) . . . . ? C11 C12 C13 C14 -0.9(7) . . . . ? C2 C1 C14 C13 -178.6(4) . . . . ? Br1 C1 C14 C13 -3.3(6) . . . . ? C2 C1 C14 C9 -1.0(7) . . . . ? Br1 C1 C14 C9 174.3(3) . . . . ? C12 C13 C14 C1 179.5(5) . . . . ? C12 C13 C14 C9 1.9(6) . . . . ? C8 C9 C14 C1 0.8(6) . . . . ? C10 C9 C14 C1 -179.3(4) . . . . ? C8 C9 C14 C13 178.6(4) . . . . ? C10 C9 C14 C13 -1.5(6) . . . . ? C15 O1 C16 C17 -179.0(4) . . . . ? Li1 O1 C16 C17 -38.4(5) . . . . ? C18 O2 C17 C16 174.3(5) . . . . ? Li1 O2 C17 C16 -39.7(6) . . . . ? O1 C16 C17 O2 52.6(6) . . . . ? O4 Li2 O3 C22 -145(4) . . . . ? O4' Li2 O3 C22 -152(4) . . . . ? O3' Li2 O3 C22 -8(7) . . . . ? C8 Li2 O3 C22 94(4) . . . . ? Br2 Li2 O3 C22 -39(4) . . . . ? C20 Li2 O3 C22 -155(5) . . . . ? O4 Li2 O3 C21 -9(5) . . . . ? O4' Li2 O3 C21 -15(4) . . . . ? O3' Li2 O3 C21 128(10) . . . . ? C8 Li2 O3 C21 -130(4) . . . . ? Br2 Li2 O3 C21 97(4) . . . . ? C20 Li2 O3 C21 -19(3) . . . . ? O4' Li2 O4 C19 -131(16) . . . . ? O3' Li2 O4 C19 -175(6) . . . . ? O3 Li2 O4 C19 -168(6) . . . . ? C8 Li2 O4 C19 -41(7) . . . . ? Br2 Li2 O4 C19 82(6) . . . . ? C20 Li2 O4 C19 -150(10) . . . . ? O4' Li2 O4 C20 19(7) . . . . ? O3' Li2 O4 C20 -25(4) . . . . ? O3 Li2 O4 C20 -17(5) . . . . ? C8 Li2 O4 C20 109(4) . . . . ? Br2 Li2 O4 C20 -128(4) . . . . ? C19 O4 C20 C21 -163(5) . . . . ? Li2 O4 C20 C21 40(5) . . . . ? C19 O4 C20 Li2 157(8) . . . . ? O4' Li2 C20 O4 -12(5) . . . . ? O3' Li2 C20 O4 152(5) . . . . ? O3 Li2 C20 O4 159(6) . . . . ? C8 Li2 C20 O4 -89(5) . . . . ? Br2 Li2 C20 O4 64(5) . . . . ? O4 Li2 C20 C21 -142(5) . . . . ? O4' Li2 C20 C21 -153(5) . . . . ? O3' Li2 C20 C21 11(3) . . . . ? O3 Li2 C20 C21 18(3) . . . . ? C8 Li2 C20 C21 129(3) . . . . ? Br2 Li2 C20 C21 -78(3) . . . . ? C22 O3 C21 C20 175(5) . . . . ? Li2 O3 C21 C20 32(5) . . . . ? O4 C20 C21 O3 -48(4) . . . . ? Li2 C20 C21 O3 -23(4) . . . . ? O4 Li2 O3' C22' -149(2) . . . . ? O4' Li2 O3' C22' -157.2(6) . . . . ? O3 Li2 O3' C22' 167(8) . . . . ? C8 Li2 O3' C22' 81.3(7) . . . . ? Br2 Li2 O3' C22' -42.0(7) . . . . ? C20 Li2 O3' C22' -162.3(15) . . . . ? O4 Li2 O3' C21' -24(2) . . . . ? O4' Li2 O3' C21' -31.8(5) . . . . ? O3 Li2 O3' C21' -67(8) . . . . ? C8 Li2 O3' C21' -153.3(5) . . . . ? Br2 Li2 O3' C21' 83.4(5) . . . . ? C20 Li2 O3' C21' -36.9(13) . . . . ? O4 Li2 O4' C19' 76(10) . . . . ? O3' Li2 O4' C19' -147.8(6) . . . . ? O3 Li2 O4' C19' -141.2(19) . . . . ? C8 Li2 O4' C19' -19.6(8) . . . . ? Br2 Li2 O4' C19' 112.4(7) . . . . ? C20 Li2 O4' C19' -133(4) . . . . ? O4 Li2 O4' C20' -131(11) . . . . ? O3' Li2 O4' C20' 5.0(6) . . . . ? O3 Li2 O4' C20' 11.6(17) . . . . ? C8 Li2 O4' C20' 133.2(6) . . . . ? Br2 Li2 O4' C20' -94.8(6) . . . . ? C20 Li2 O4' C20' 20(4) . . . . ? C19' O4' C20' C21' -178.5(6) . . . . ? Li2 O4' C20' C21' 23.1(8) . . . . ? C22' O3' C21' C20' -175.3(6) . . . . ? Li2 O3' C21' C20' 53.8(7) . . . . ? O4' C20' C21' O3' -52.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.634 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.078