Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Garth Giesbrecht' 'David L. Clark' 'John Gordon' 'Brian L. Scott' _publ_contact_author_name 'Dr Garth Giesbrecht' _publ_contact_author_address ; C-SIC Los Alamos National Laboratory Mail Stop J514 Los Alamos New Mexico 87545 UNITED STATES OF AMERICA ; _publ_contact_author_email GARTH@LANL.GOV _publ_section_title ; Synthesis, Structure and Solution Dynamics of Lithium Salts of Super-Bulky Cyclopentadienyl Ligands ; data_ccd576s _database_code_CSD 200149 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(lithium)bis(penta(3,5-dimethylphenyl)cyclopentadienide][lithium) bis(tetramethylethylenediamine)] ; _chemical_name_common ; ((lithium)bis(penta(3,5- dimethylphenyl)cyclopentadienide)(lithium) bis(tetramethylethylenediamine)) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C110 H138 Li3 N4 O4' _chemical_formula_weight 1594.12 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.216(4) _cell_length_b 20.023(5) _cell_length_c 22.771(6) _cell_angle_alpha 98.140(6) _cell_angle_beta 106.914(4) _cell_angle_gamma 109.938(5) _cell_volume 5617(3) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.943 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 0.056 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9705 _exptl_absorpt_correction_T_max 0.9819 _exptl_absorpt_process_details ? _exptl_crystal_preparation ; crystallized from THF/TMEDA ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28915 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0748 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 0.97 _diffrn_reflns_theta_max 22.46 _reflns_number_total 13878 _reflns_number_gt 8173 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The electron density of a disordered thf molecule was refined with the aid of PLATON/SQUEEZE (209 e/cell and 1728 \%A^3^). ; _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^)+(0.1776P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13878 _refine_ls_number_parameters 916 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1400 _refine_ls_R_factor_gt 0.0962 _refine_ls_wR_factor_ref 0.2954 _refine_ls_wR_factor_gt 0.2744 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.5340(3) 1.4673(2) 0.6013(2) 0.0389(11) Uani 1 1 d . . . C2 C 1.6125(3) 1.4588(2) 0.5765(2) 0.0370(11) Uani 1 1 d . . . C3 C 1.5569(3) 1.4022(2) 0.5184(2) 0.0393(11) Uani 1 1 d . . . C4 C 1.4439(3) 1.3761(2) 0.5070(2) 0.0390(11) Uani 1 1 d . . . C5 C 1.4314(3) 1.4169(2) 0.5584(2) 0.0386(11) Uani 1 1 d . . . C6 C 1.5585(4) 1.5147(3) 0.6643(2) 0.0465(12) Uani 1 1 d . . . C7 C 1.5077(4) 1.4868(3) 0.7048(2) 0.0543(13) Uani 1 1 d . . . H7 H 1.4581 1.4381 0.6918 0.065 Uiso 1 1 calc R . . C8 C 1.5303(5) 1.5311(4) 0.7647(3) 0.0659(16) Uani 1 1 d . . . C9 C 1.6091(5) 1.6013(4) 0.7849(3) 0.0775(19) Uani 1 1 d . . . H9 H 1.6283 1.6295 0.8259 0.093 Uiso 1 1 calc R . . C10 C 1.6606(4) 1.6311(3) 0.7462(3) 0.0630(15) Uani 1 1 d . . . C11 C 1.6342(4) 1.5879(3) 0.6868(2) 0.0495(13) Uani 1 1 d . . . H11 H 1.6679 1.6080 0.6602 0.059 Uiso 1 1 calc R . . C12 C 1.4671(7) 1.5007(4) 0.8064(3) 0.109(3) Uani 1 1 d . . . H12A H 1.4170 1.4506 0.7849 0.164 Uiso 1 1 calc R . . H12B H 1.4287 1.5302 0.8140 0.164 Uiso 1 1 calc R . . H12C H 1.5161 1.5022 0.8463 0.164 Uiso 1 1 calc R . . C13 C 1.7427(5) 1.7104(3) 0.7682(3) 0.097(2) Uani 1 1 d . . . H13A H 1.7494 1.7327 0.8103 0.145 Uiso 1 1 calc R . . H13B H 1.7195 1.7373 0.7395 0.145 Uiso 1 1 calc R . . H13C H 1.8110 1.7114 0.7689 0.145 Uiso 1 1 calc R . . C14 C 1.7306(4) 1.4976(2) 0.6081(2) 0.0442(12) Uani 1 1 d . . . C15 C 1.7820(4) 1.5050(3) 0.6727(2) 0.0499(12) Uani 1 1 d . . . H15 H 1.7405 1.4862 0.6962 0.060 Uiso 1 1 calc R . . C16 C 1.8921(4) 1.5392(3) 0.7028(2) 0.0545(13) Uani 1 1 d . . . C17 C 1.9547(4) 1.5655(3) 0.6670(3) 0.0593(14) Uani 1 1 d . . . H17 H 2.0291 1.5880 0.6866 0.071 Uiso 1 1 calc R . . C18 C 1.9071(4) 1.5585(3) 0.6023(3) 0.0561(13) Uani 1 1 d . . . C19 C 1.7962(3) 1.5244(2) 0.5743(2) 0.0453(12) Uani 1 1 d . . . H19 H 1.7641 1.5191 0.5311 0.054 Uiso 1 1 calc R . . C20 C 1.9436(5) 1.5495(4) 0.7737(3) 0.0868(19) Uani 1 1 d . . . H20A H 1.8891 1.5268 0.7901 0.130 Uiso 1 1 calc R . . H20B H 1.9800 1.6013 0.7951 0.130 Uiso 1 1 calc R . . H20C H 1.9943 1.5271 0.7810 0.130 Uiso 1 1 calc R . . C21 C 1.9749(4) 1.5890(3) 0.5645(3) 0.0787(18) Uani 1 1 d . . . H21A H 1.9293 1.5793 0.5211 0.118 Uiso 1 1 calc R . . H21B H 2.0243 1.5658 0.5658 0.118 Uiso 1 1 calc R . . H21C H 2.0144 1.6412 0.5825 0.118 Uiso 1 1 calc R . . C22 C 1.6031(3) 1.3671(2) 0.4790(2) 0.0394(11) Uani 1 1 d . . . C23 C 1.6907(4) 1.3508(3) 0.5070(2) 0.0482(12) Uani 1 1 d . . . H23 H 1.7214 1.3633 0.5512 0.058 Uiso 1 1 calc R . . C24 C 1.7334(4) 1.3168(3) 0.4715(3) 0.0526(13) Uani 1 1 d . . . C25 C 1.6858(4) 1.2971(3) 0.4056(3) 0.0589(14) Uani 1 1 d . . . H25 H 1.7133 1.2734 0.3812 0.071 Uiso 1 1 calc R . . C26 C 1.5978(4) 1.3121(3) 0.3749(2) 0.0521(13) Uani 1 1 d . . . C27 C 1.5581(4) 1.3467(2) 0.4124(2) 0.0463(12) Uani 1 1 d . . . H27 H 1.4993 1.3569 0.3926 0.056 Uiso 1 1 calc R . . C28 C 1.8300(4) 1.3020(3) 0.5040(3) 0.0800(18) Uani 1 1 d . . . H28A H 1.8515 1.3193 0.5494 0.120 Uiso 1 1 calc R . . H28B H 1.8879 1.3274 0.4911 0.120 Uiso 1 1 calc R . . H28C H 1.8120 1.2500 0.4924 0.120 Uiso 1 1 calc R . . C29 C 1.5485(5) 1.2927(4) 0.3039(3) 0.0833(19) Uani 1 1 d . . . H29A H 1.4889 1.3067 0.2919 0.125 Uiso 1 1 calc R . . H29B H 1.5239 1.2405 0.2869 0.125 Uiso 1 1 calc R . . H29C H 1.6012 1.3184 0.2874 0.125 Uiso 1 1 calc R . . C30 C 1.3590(3) 1.3098(2) 0.4579(2) 0.0411(11) Uani 1 1 d . . . C31 C 1.3659(4) 1.2415(3) 0.4509(2) 0.0487(12) Uani 1 1 d . . . H31 H 1.4298 1.2394 0.4747 0.058 Uiso 1 1 calc R . . C32 C 1.2840(4) 1.1775(3) 0.4111(2) 0.0543(13) Uani 1 1 d . . . C33 C 1.1915(4) 1.1809(3) 0.3751(2) 0.0631(15) Uani 1 1 d . . . H33 H 1.1354 1.1375 0.3476 0.076 Uiso 1 1 calc R . . C34 C 1.1774(4) 1.2465(3) 0.3777(2) 0.0602(14) Uani 1 1 d . . . C35 C 1.2614(4) 1.3108(3) 0.4188(2) 0.0484(12) Uani 1 1 d . . . H35 H 1.2539 1.3553 0.4208 0.058 Uiso 1 1 calc R . . C36 C 1.2944(5) 1.1042(3) 0.4094(3) 0.0785(18) Uani 1 1 d . . . H36A H 1.2288 1.0650 0.3799 0.118 Uiso 1 1 calc R . . H36B H 1.3081 1.0963 0.4511 0.118 Uiso 1 1 calc R . . H36C H 1.3528 1.1049 0.3960 0.118 Uiso 1 1 calc R . . C37 C 1.0767(4) 1.2525(4) 0.3383(3) 0.091(2) Uani 1 1 d . . . H37A H 1.0861 1.3031 0.3473 0.137 Uiso 1 1 calc R . . H37B H 1.0174 1.2237 0.3487 0.137 Uiso 1 1 calc R . . H37C H 1.0624 1.2344 0.2939 0.137 Uiso 1 1 calc R . . C38 C 1.3282(3) 1.4033(3) 0.5687(2) 0.0423(11) Uani 1 1 d . . . C39 C 1.2528(4) 1.3313(3) 0.5580(2) 0.0494(12) Uani 1 1 d . . . H39 H 1.2661 1.2912 0.5428 0.059 Uiso 1 1 calc R . . C40 C 1.1586(4) 1.3193(3) 0.5700(3) 0.0620(15) Uani 1 1 d . . . C41 C 1.1404(4) 1.3789(4) 0.5932(3) 0.0660(16) Uani 1 1 d . . . H41 H 1.0777 1.3709 0.6014 0.079 Uiso 1 1 calc R . . C42 C 1.2127(4) 1.4504(3) 0.6048(3) 0.0627(15) Uani 1 1 d . . . C43 C 1.3057(4) 1.4619(3) 0.5919(2) 0.0508(13) Uani 1 1 d . . . H43 H 1.3541 1.5099 0.5989 0.061 Uiso 1 1 calc R . . C44 C 1.0769(5) 1.2413(3) 0.5546(4) 0.096(2) Uani 1 1 d . . . H44A H 1.1038 1.2073 0.5391 0.144 Uiso 1 1 calc R . . H44B H 1.0110 1.2350 0.5225 0.144 Uiso 1 1 calc R . . H44C H 1.0639 1.2321 0.5923 0.144 Uiso 1 1 calc R . . C45 C 1.1936(5) 1.5171(4) 0.6316(4) 0.100(2) Uani 1 1 d . . . H45A H 1.2524 1.5616 0.6361 0.150 Uiso 1 1 calc R . . H45B H 1.1883 1.5154 0.6725 0.150 Uiso 1 1 calc R . . H45C H 1.1280 1.5160 0.6031 0.150 Uiso 1 1 calc R . . C46 C 0.4359(3) 0.9859(2) 0.08638(19) 0.0365(11) Uani 1 1 d . . . C47 C 0.5463(3) 0.9981(2) 0.11212(19) 0.0370(11) Uani 1 1 d . . . C48 C 0.5581(3) 0.9366(2) 0.0796(2) 0.0380(11) Uani 1 1 d . . . C49 C 0.4556(3) 0.8883(2) 0.0330(2) 0.0391(11) Uani 1 1 d . . . C50 C 0.3807(3) 0.9184(2) 0.0379(2) 0.0377(11) Uani 1 1 d . . . C51 C 0.3822(3) 1.0305(2) 0.1105(2) 0.0361(11) Uani 1 1 d . . . C52 C 0.3052(3) 1.0462(2) 0.0695(2) 0.0439(12) Uani 1 1 d . . . H52 H 0.2929 1.0342 0.0262 0.053 Uiso 1 1 calc R . . C53 C 0.2449(4) 1.0793(3) 0.0907(3) 0.0507(13) Uani 1 1 d . . . C54 C 0.2632(4) 1.0958(3) 0.1547(3) 0.0593(14) Uani 1 1 d . . . H54 H 0.2223 1.1168 0.1693 0.071 Uiso 1 1 calc R . . C55 C 0.3409(4) 1.0821(3) 0.1984(2) 0.0544(13) Uani 1 1 d . . . C56 C 0.3997(4) 1.0500(2) 0.1749(2) 0.0464(12) Uani 1 1 d . . . H56 H 0.4530 1.0412 0.2035 0.056 Uiso 1 1 calc R . . C57 C 0.1622(4) 1.0959(3) 0.0444(3) 0.0776(18) Uani 1 1 d . . . H57A H 0.1274 1.1175 0.0668 0.116 Uiso 1 1 calc R . . H57B H 0.1098 1.0511 0.0132 0.116 Uiso 1 1 calc R . . H57C H 0.1964 1.1298 0.0236 0.116 Uiso 1 1 calc R . . C58 C 0.3582(5) 1.0977(4) 0.2685(3) 0.0846(19) Uani 1 1 d . . . H58A H 0.4151 1.0847 0.2907 0.127 Uiso 1 1 calc R . . H58B H 0.2932 1.0692 0.2740 0.127 Uiso 1 1 calc R . . H58C H 0.3771 1.1493 0.2853 0.127 Uiso 1 1 calc R . . C59 C 0.6288(3) 1.0590(3) 0.1682(2) 0.0394(11) Uani 1 1 d . . . C60 C 0.6918(4) 1.0443(3) 0.2198(2) 0.0502(13) Uani 1 1 d . . . H60 H 0.6836 0.9958 0.2173 0.060 Uiso 1 1 calc R . . C61 C 0.7661(4) 1.0985(3) 0.2746(2) 0.0578(14) Uani 1 1 d . . . C62 C 0.7784(4) 1.1699(3) 0.2767(2) 0.0581(14) Uani 1 1 d . . . H62 H 0.8276 1.2071 0.3131 0.070 Uiso 1 1 calc R . . C63 C 0.7195(4) 1.1885(3) 0.2260(2) 0.0473(12) Uani 1 1 d . . . C64 C 0.6437(3) 1.1318(3) 0.1728(2) 0.0425(12) Uani 1 1 d . . . H64 H 0.6019 1.1433 0.1393 0.051 Uiso 1 1 calc R . . C65 C 0.8332(5) 1.0785(3) 0.3296(3) 0.088(2) Uani 1 1 d . . . H65A H 0.8158 1.0266 0.3181 0.133 Uiso 1 1 calc R . . H65B H 0.8177 1.0910 0.3670 0.133 Uiso 1 1 calc R . . H65C H 0.9082 1.1054 0.3382 0.133 Uiso 1 1 calc R . . C66 C 0.7383(4) 1.2674(3) 0.2277(3) 0.0683(16) Uani 1 1 d . . . H66A H 0.6904 1.2692 0.1889 0.102 Uiso 1 1 calc R . . H66B H 0.8113 1.2943 0.2319 0.102 Uiso 1 1 calc R . . H66C H 0.7253 1.2890 0.2633 0.102 Uiso 1 1 calc R . . C67 C 0.6575(3) 0.9230(3) 0.0958(2) 0.0406(11) Uani 1 1 d . . . C68 C 0.6537(4) 0.8529(3) 0.0976(2) 0.0510(13) Uani 1 1 d . . . H68 H 0.5879 0.8148 0.0895 0.061 Uiso 1 1 calc R . . C69 C 0.7448(4) 0.8382(3) 0.1109(2) 0.0599(14) Uani 1 1 d . . . C70 C 0.8415(5) 0.8952(4) 0.1252(3) 0.0669(16) Uani 1 1 d . . . H70 H 0.9032 0.8859 0.1351 0.080 Uiso 1 1 calc R . . C71 C 0.8513(4) 0.9670(3) 0.1255(2) 0.0614(15) Uani 1 1 d . . . C72 C 0.7572(4) 0.9787(3) 0.1094(2) 0.0481(12) Uani 1 1 d . . . H72 H 0.7613 1.0257 0.1076 0.058 Uiso 1 1 calc R . . C73 C 0.7368(5) 0.7590(3) 0.1087(3) 0.089(2) Uani 1 1 d . . . H73A H 0.6635 0.7266 0.0991 0.133 Uiso 1 1 calc R . . H73B H 0.7809 0.7582 0.1492 0.133 Uiso 1 1 calc R . . H73C H 0.7610 0.7430 0.0763 0.133 Uiso 1 1 calc R . . C74 C 0.9585(4) 1.0297(4) 0.1421(4) 0.096(2) Uani 1 1 d . . . H74A H 0.9489 1.0749 0.1422 0.145 Uiso 1 1 calc R . . H74B H 0.9895 1.0207 0.1112 0.145 Uiso 1 1 calc R . . H74C H 1.0055 1.0336 0.1836 0.145 Uiso 1 1 calc R . . C75 C 0.4300(3) 0.8152(2) -0.0084(2) 0.0400(11) Uani 1 1 d . . . C76 C 0.4945(4) 0.8066(3) -0.0426(2) 0.0492(12) Uani 1 1 d . . . H76 H 0.5528 0.8479 -0.0402 0.059 Uiso 1 1 calc R . . C77 C 0.4746(4) 0.7396(3) -0.0796(2) 0.0569(14) Uani 1 1 d . . . C78 C 0.3864(5) 0.6775(3) -0.0835(3) 0.0634(15) Uani 1 1 d . . . H78 H 0.3736 0.6315 -0.1076 0.076 Uiso 1 1 calc R . . C79 C 0.3179(4) 0.6833(3) -0.0521(2) 0.0570(14) Uani 1 1 d . . . C80 C 0.3420(4) 0.7521(3) -0.0144(2) 0.0481(12) Uani 1 1 d . . . H80 H 0.2979 0.7564 0.0077 0.058 Uiso 1 1 calc R . . C81 C 0.5457(5) 0.7322(3) -0.1154(3) 0.092(2) Uani 1 1 d . . . H81A H 0.5190 0.6818 -0.1393 0.138 Uiso 1 1 calc R . . H81B H 0.6175 0.7468 -0.0858 0.138 Uiso 1 1 calc R . . H81C H 0.5461 0.7632 -0.1439 0.138 Uiso 1 1 calc R . . C82 C 0.2205(5) 0.6165(3) -0.0588(3) 0.089(2) Uani 1 1 d . . . H82A H 0.1833 0.6305 -0.0336 0.134 Uiso 1 1 calc R . . H82B H 0.2430 0.5797 -0.0445 0.134 Uiso 1 1 calc R . . H82C H 0.1735 0.5970 -0.1027 0.134 Uiso 1 1 calc R . . C83 C 0.2618(3) 0.8814(2) 0.0052(2) 0.0400(11) Uani 1 1 d . . . C84 C 0.2145(3) 0.8494(3) -0.0602(2) 0.0450(12) Uani 1 1 d . . . H84 H 0.2583 0.8533 -0.0841 0.054 Uiso 1 1 calc R . . C85 C 0.1038(4) 0.8117(3) -0.0910(2) 0.0520(13) Uani 1 1 d . . . C86 C 0.0401(4) 0.8074(3) -0.0550(2) 0.0552(13) Uani 1 1 d . . . H86 H -0.0342 0.7840 -0.0752 0.066 Uiso 1 1 calc R . . C87 C 0.0836(4) 0.8371(3) 0.0107(2) 0.0500(13) Uani 1 1 d . . . C88 C 0.1949(3) 0.8740(2) 0.0397(2) 0.0425(11) Uani 1 1 d . . . H88 H 0.2252 0.8942 0.0836 0.051 Uiso 1 1 calc R . . C89 C 0.0559(4) 0.7800(4) -0.1621(3) 0.0850(19) Uani 1 1 d . . . H89A H 0.1125 0.7883 -0.1787 0.127 Uiso 1 1 calc R . . H89B H 0.0105 0.8034 -0.1809 0.127 Uiso 1 1 calc R . . H89C H 0.0142 0.7279 -0.1721 0.127 Uiso 1 1 calc R . . C90 C 0.0152(4) 0.8327(3) 0.0515(3) 0.0743(17) Uani 1 1 d . . . H90A H 0.0609 0.8565 0.0953 0.111 Uiso 1 1 calc R . . H90B H -0.0268 0.7820 0.0471 0.111 Uiso 1 1 calc R . . H90C H -0.0319 0.8570 0.0378 0.111 Uiso 1 1 calc R . . C91 C 1.6786(7) 1.1466(5) 0.7613(4) 0.128(3) Uiso 1 1 d . . . H91A H 1.7269 1.1815 0.7474 0.192 Uiso 1 1 calc R . . H91B H 1.6246 1.1075 0.7251 0.192 Uiso 1 1 calc R . . H91C H 1.7180 1.1266 0.7903 0.192 Uiso 1 1 calc R . . C92 C 1.5565(6) 1.1299(4) 0.8124(4) 0.107(2) Uiso 1 1 d . . . H92A H 1.5237 1.1541 0.8343 0.160 Uiso 1 1 calc R . . H92B H 1.5954 1.1089 0.8406 0.160 Uiso 1 1 calc R . . H92C H 1.5019 1.0915 0.7759 0.160 Uiso 1 1 calc R . . C93 C 1.7179(7) 1.2387(5) 0.8476(4) 0.123(3) Uiso 1 1 d . . . H93A H 1.7282 1.2171 0.8833 0.148 Uiso 1 1 calc R . . H93B H 1.7829 1.2512 0.8379 0.148 Uiso 1 1 calc R . . C94 C 1.7067(7) 1.3027(5) 0.8667(4) 0.136(3) Uiso 1 1 d . . . H94A H 1.7783 1.3401 0.8914 0.163 Uiso 1 1 calc R . . H94B H 1.6684 1.2947 0.8958 0.163 Uiso 1 1 calc R . . C95 C 1.7332(9) 1.3926(6) 0.8035(6) 0.192(5) Uiso 1 1 d . . . H95A H 1.7644 1.3695 0.7795 0.288 Uiso 1 1 calc R . . H95B H 1.7887 1.4275 0.8418 0.288 Uiso 1 1 calc R . . H95C H 1.6975 1.4177 0.7784 0.288 Uiso 1 1 calc R . . C96 C 1.6068(9) 1.3702(6) 0.8537(5) 0.181(4) Uiso 1 1 d . . . H96A H 1.5677 1.3917 0.8263 0.272 Uiso 1 1 calc R . . H96B H 1.6622 1.4081 0.8902 0.272 Uiso 1 1 calc R . . H96C H 1.5587 1.3348 0.8673 0.272 Uiso 1 1 calc R . . C97 C 1.3236(6) 1.1339(4) 0.7109(4) 0.116(2) Uiso 1 1 d . . . H97A H 1.3403 1.1312 0.7543 0.174 Uiso 1 1 calc R . . H97B H 1.3459 1.1016 0.6884 0.174 Uiso 1 1 calc R . . H97C H 1.2475 1.1192 0.6909 0.174 Uiso 1 1 calc R . . C98 C 1.3441(8) 1.2588(5) 0.7415(5) 0.151(3) Uiso 1 1 d . . . H98A H 1.3592 1.2566 0.7849 0.227 Uiso 1 1 calc R . . H98B H 1.2681 1.2429 0.7202 0.227 Uiso 1 1 calc R . . H98C H 1.3803 1.3086 0.7405 0.227 Uiso 1 1 calc R . . C99 C 1.3581(6) 1.2169(5) 0.6456(4) 0.116(2) Uiso 1 1 d . . . H99A H 1.2839 1.1840 0.6207 0.140 Uiso 1 1 calc R . . H99B H 1.3649 1.2668 0.6455 0.140 Uiso 1 1 calc R . . C100 C 1.4240(7) 1.2001(5) 0.6154(4) 0.128(3) Uiso 1 1 d . . . H10A H 1.4053 1.2097 0.5739 0.153 Uiso 1 1 calc R . . H10B H 1.4065 1.1477 0.6082 0.153 Uiso 1 1 calc R . . C101 C 1.5780(6) 1.3155(4) 0.6444(4) 0.109(2) Uiso 1 1 d . . . H10C H 1.5441 1.3409 0.6641 0.164 Uiso 1 1 calc R . . H10D H 1.5597 1.3158 0.6005 0.164 Uiso 1 1 calc R . . H10E H 1.6546 1.3397 0.6659 0.164 Uiso 1 1 calc R . . C102 C 1.5923(6) 1.2020(4) 0.6195(4) 0.122(3) Uiso 1 1 d . . . H10F H 1.5680 1.1519 0.6223 0.182 Uiso 1 1 calc R . . H10G H 1.6688 1.2262 0.6412 0.182 Uiso 1 1 calc R . . H10H H 1.5742 1.2024 0.5756 0.182 Uiso 1 1 calc R . . N1 N 1.6290(4) 1.1823(2) 0.7924(2) 0.0685(13) Uani 1 1 d . . . N2 N 1.6534(4) 1.3351(3) 0.8205(2) 0.0873(16) Uani 1 1 d . . . N3 N 1.3813(4) 1.2113(3) 0.7096(2) 0.0819(14) Uani 1 1 d . . . N4 N 1.5414(4) 1.2398(3) 0.6487(2) 0.0774(14) Uani 1 1 d . . . Li1 Li 1.5000 1.5000 0.5000 0.053(3) Uani 1 2 d S . . Li3 Li 0.5000 1.0000 0.0000 0.045(3) Uani 1 2 d S . . Li2 Li 1.5532(8) 1.2412(5) 0.7435(4) 0.063(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.040(3) 0.045(3) 0.037(3) 0.018(2) 0.014(2) 0.019(2) C2 0.032(2) 0.046(3) 0.036(3) 0.020(2) 0.012(2) 0.017(2) C3 0.039(3) 0.052(3) 0.039(3) 0.026(2) 0.018(2) 0.024(2) C4 0.033(3) 0.046(3) 0.039(3) 0.022(2) 0.013(2) 0.014(2) C5 0.036(3) 0.039(3) 0.043(3) 0.015(2) 0.015(2) 0.016(2) C6 0.040(3) 0.063(4) 0.043(3) 0.014(3) 0.013(2) 0.030(3) C7 0.071(3) 0.062(3) 0.055(3) 0.029(3) 0.033(3) 0.042(3) C8 0.088(4) 0.082(5) 0.056(4) 0.027(3) 0.034(3) 0.057(4) C9 0.086(4) 0.092(5) 0.051(4) -0.009(4) 0.012(4) 0.055(4) C10 0.054(3) 0.078(4) 0.059(4) 0.011(3) 0.016(3) 0.037(3) C11 0.045(3) 0.054(3) 0.046(3) 0.009(3) 0.012(2) 0.022(3) C12 0.169(7) 0.137(6) 0.091(5) 0.055(5) 0.090(5) 0.096(6) C13 0.070(4) 0.066(4) 0.112(6) -0.018(4) 0.006(4) 0.019(4) C14 0.042(3) 0.047(3) 0.047(3) 0.017(2) 0.015(2) 0.020(2) C15 0.042(3) 0.058(3) 0.047(3) 0.018(3) 0.014(2) 0.017(3) C16 0.048(3) 0.050(3) 0.050(3) 0.009(3) 0.002(3) 0.017(3) C17 0.036(3) 0.055(3) 0.074(4) 0.021(3) 0.009(3) 0.011(3) C18 0.043(3) 0.063(4) 0.063(4) 0.026(3) 0.016(3) 0.021(3) C19 0.040(3) 0.048(3) 0.051(3) 0.024(2) 0.016(2) 0.018(2) C20 0.063(4) 0.100(5) 0.068(4) 0.030(4) -0.004(3) 0.020(4) C21 0.042(3) 0.101(5) 0.094(5) 0.047(4) 0.029(3) 0.019(3) C22 0.037(3) 0.041(3) 0.041(3) 0.019(2) 0.015(2) 0.013(2) C23 0.046(3) 0.051(3) 0.051(3) 0.021(2) 0.015(2) 0.024(2) C24 0.053(3) 0.057(3) 0.065(4) 0.025(3) 0.032(3) 0.029(3) C25 0.072(4) 0.053(3) 0.075(4) 0.024(3) 0.049(3) 0.030(3) C26 0.054(3) 0.059(3) 0.054(3) 0.021(3) 0.026(3) 0.028(3) C27 0.042(3) 0.054(3) 0.050(3) 0.021(2) 0.021(2) 0.021(2) C28 0.062(4) 0.094(5) 0.106(5) 0.037(4) 0.036(3) 0.048(3) C29 0.094(5) 0.109(5) 0.058(4) 0.014(3) 0.036(4) 0.051(4) C30 0.038(3) 0.046(3) 0.042(3) 0.018(2) 0.019(2) 0.015(2) C31 0.049(3) 0.061(4) 0.040(3) 0.022(3) 0.018(2) 0.022(3) C32 0.058(3) 0.055(4) 0.046(3) 0.013(3) 0.020(3) 0.017(3) C33 0.061(4) 0.051(4) 0.050(3) 0.005(3) 0.011(3) 0.002(3) C34 0.041(3) 0.065(4) 0.052(3) 0.014(3) 0.005(3) 0.006(3) C35 0.050(3) 0.048(3) 0.048(3) 0.021(3) 0.016(3) 0.020(3) C36 0.114(5) 0.053(4) 0.074(4) 0.018(3) 0.038(4) 0.036(3) C37 0.056(4) 0.093(5) 0.089(5) 0.019(4) -0.006(3) 0.016(3) C38 0.042(3) 0.054(3) 0.043(3) 0.030(2) 0.019(2) 0.023(3) C39 0.044(3) 0.057(3) 0.055(3) 0.026(3) 0.020(2) 0.022(3) C40 0.052(3) 0.068(4) 0.074(4) 0.035(3) 0.026(3) 0.024(3) C41 0.044(3) 0.096(5) 0.078(4) 0.044(4) 0.033(3) 0.033(3) C42 0.052(3) 0.084(4) 0.079(4) 0.042(3) 0.039(3) 0.038(3) C43 0.051(3) 0.065(3) 0.052(3) 0.026(3) 0.025(3) 0.032(3) C44 0.055(4) 0.096(5) 0.145(6) 0.058(5) 0.047(4) 0.020(4) C45 0.100(5) 0.104(5) 0.157(7) 0.057(5) 0.089(5) 0.068(4) C46 0.035(3) 0.044(3) 0.036(3) 0.016(2) 0.016(2) 0.017(2) C47 0.040(3) 0.050(3) 0.026(2) 0.016(2) 0.012(2) 0.022(2) C48 0.040(3) 0.042(3) 0.038(3) 0.019(2) 0.017(2) 0.017(2) C49 0.038(3) 0.050(3) 0.035(3) 0.016(2) 0.016(2) 0.020(2) C50 0.037(3) 0.049(3) 0.035(3) 0.019(2) 0.017(2) 0.021(2) C51 0.036(2) 0.039(3) 0.034(3) 0.014(2) 0.014(2) 0.013(2) C52 0.045(3) 0.051(3) 0.042(3) 0.020(2) 0.019(2) 0.021(2) C53 0.048(3) 0.052(3) 0.066(4) 0.021(3) 0.031(3) 0.027(3) C54 0.061(3) 0.061(4) 0.079(4) 0.025(3) 0.044(3) 0.035(3) C55 0.063(3) 0.055(3) 0.055(3) 0.017(3) 0.036(3) 0.024(3) C56 0.047(3) 0.045(3) 0.050(3) 0.017(2) 0.021(2) 0.018(2) C57 0.069(4) 0.099(5) 0.094(5) 0.043(4) 0.036(3) 0.056(4) C58 0.114(5) 0.097(5) 0.063(4) 0.018(3) 0.050(4) 0.053(4) C59 0.036(3) 0.050(3) 0.041(3) 0.024(2) 0.016(2) 0.019(2) C60 0.043(3) 0.053(3) 0.047(3) 0.016(3) 0.015(3) 0.011(3) C61 0.043(3) 0.064(4) 0.043(3) 0.016(3) 0.000(3) 0.007(3) C62 0.044(3) 0.068(4) 0.043(3) 0.007(3) 0.010(3) 0.007(3) C63 0.044(3) 0.045(3) 0.052(3) 0.017(3) 0.020(3) 0.014(2) C64 0.035(3) 0.057(3) 0.036(3) 0.016(3) 0.012(2) 0.018(2) C65 0.073(4) 0.087(5) 0.064(4) 0.030(3) -0.010(3) 0.011(3) C66 0.063(4) 0.059(4) 0.072(4) 0.013(3) 0.027(3) 0.011(3) C67 0.033(3) 0.051(3) 0.035(3) 0.010(2) 0.012(2) 0.014(2) C68 0.050(3) 0.060(4) 0.052(3) 0.023(3) 0.021(2) 0.028(3) C69 0.060(4) 0.079(4) 0.061(4) 0.028(3) 0.028(3) 0.043(3) C70 0.056(4) 0.102(5) 0.072(4) 0.040(3) 0.030(3) 0.054(4) C71 0.037(3) 0.098(5) 0.060(4) 0.031(3) 0.024(3) 0.030(3) C72 0.047(3) 0.061(3) 0.048(3) 0.024(3) 0.021(2) 0.028(3) C73 0.102(5) 0.084(5) 0.120(6) 0.047(4) 0.048(4) 0.070(4) C74 0.045(4) 0.111(5) 0.145(6) 0.055(5) 0.039(4) 0.034(4) C75 0.040(3) 0.046(3) 0.037(3) 0.015(2) 0.013(2) 0.019(2) C76 0.054(3) 0.058(3) 0.044(3) 0.014(3) 0.022(3) 0.029(3) C77 0.072(4) 0.057(4) 0.057(3) 0.018(3) 0.034(3) 0.034(3) C78 0.082(4) 0.047(3) 0.060(4) 0.009(3) 0.025(3) 0.027(3) C79 0.063(3) 0.040(3) 0.056(3) 0.013(3) 0.018(3) 0.010(3) C80 0.048(3) 0.057(3) 0.047(3) 0.021(3) 0.019(2) 0.026(3) C81 0.114(5) 0.086(5) 0.105(5) 0.020(4) 0.070(5) 0.051(4) C82 0.089(5) 0.053(4) 0.092(5) 0.008(3) 0.026(4) -0.001(3) C83 0.032(2) 0.043(3) 0.043(3) 0.010(2) 0.012(2) 0.014(2) C84 0.038(3) 0.059(3) 0.042(3) 0.016(2) 0.016(2) 0.021(2) C85 0.044(3) 0.061(3) 0.047(3) 0.014(3) 0.012(3) 0.021(3) C86 0.032(3) 0.065(3) 0.060(4) 0.016(3) 0.011(3) 0.013(2) C87 0.040(3) 0.061(3) 0.061(4) 0.027(3) 0.026(3) 0.024(3) C88 0.039(3) 0.052(3) 0.039(3) 0.014(2) 0.014(2) 0.021(2) C89 0.056(3) 0.114(5) 0.053(4) 0.000(3) 0.003(3) 0.019(4) C90 0.052(3) 0.100(5) 0.085(4) 0.037(4) 0.039(3) 0.029(3) N1 0.083(3) 0.063(3) 0.074(3) 0.039(3) 0.039(3) 0.030(3) N2 0.111(4) 0.090(4) 0.068(3) 0.026(3) 0.028(3) 0.051(3) N3 0.091(4) 0.088(4) 0.076(4) 0.037(3) 0.035(3) 0.037(3) N4 0.110(4) 0.064(3) 0.074(3) 0.039(3) 0.044(3) 0.037(3) Li1 0.038(6) 0.069(8) 0.054(7) 0.024(6) 0.021(5) 0.019(6) Li3 0.045(6) 0.047(7) 0.044(6) 0.016(5) 0.014(5) 0.021(5) Li2 0.083(6) 0.052(5) 0.061(6) 0.030(4) 0.026(5) 0.030(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 C1 C5 1.411(6) . ? C1 C2 1.435(6) . ? C1 C6 1.475(6) . ? C1 Li1 2.445(4) . ? C2 C3 1.421(6) . ? C2 C14 1.480(6) . ? C2 Li1 2.441(4) . ? C3 C4 1.437(6) . ? C3 C22 1.487(6) . ? C3 Li1 2.405(4) . ? C4 C5 1.421(6) . ? C4 C30 1.474(6) . ? C4 Li1 2.377(4) . ? C5 C38 1.493(6) . ? C5 Li1 2.400(4) . ? C6 C7 1.393(7) . ? C6 C11 1.400(7) . ? C7 C8 1.401(7) . ? C8 C9 1.373(8) . ? C8 C12 1.538(8) . ? C9 C10 1.377(8) . ? C10 C11 1.366(7) . ? C10 C13 1.518(8) . ? C14 C19 1.393(6) . ? C14 C15 1.400(6) . ? C15 C16 1.378(6) . ? C16 C17 1.399(7) . ? C16 C20 1.518(7) . ? C17 C18 1.394(7) . ? C18 C19 1.384(6) . ? C18 C21 1.509(7) . ? C22 C23 1.391(6) . ? C22 C27 1.400(6) . ? C23 C24 1.377(6) . ? C24 C25 1.388(7) . ? C24 C28 1.506(7) . ? C25 C26 1.396(7) . ? C26 C27 1.381(6) . ? C26 C29 1.494(7) . ? C30 C31 1.395(6) . ? C30 C35 1.422(6) . ? C31 C32 1.363(7) . ? C32 C33 1.362(7) . ? C32 C36 1.522(7) . ? C33 C34 1.390(7) . ? C34 C35 1.385(7) . ? C34 C37 1.506(7) . ? C38 C43 1.390(6) . ? C38 C39 1.407(6) . ? C39 C40 1.390(7) . ? C40 C41 1.372(7) . ? C40 C44 1.510(8) . ? C41 C42 1.382(7) . ? C42 C43 1.387(6) . ? C42 C45 1.531(7) . ? C46 C50 1.418(6) . ? C46 C47 1.424(6) . ? C46 C51 1.501(6) . ? C46 Li3 2.409(4) . ? C47 C48 1.430(6) . ? C47 C59 1.485(6) . ? C47 Li3 2.453(4) . ? C48 C49 1.426(6) . ? C48 C67 1.483(6) . ? C48 Li3 2.463(4) . ? C49 C50 1.413(6) . ? C49 C75 1.486(6) . ? C49 Li3 2.399(4) . ? C50 C83 1.489(6) . ? C50 Li3 2.378(4) . ? C51 C52 1.376(6) . ? C51 C56 1.386(6) . ? C52 C53 1.395(6) . ? C53 C54 1.374(7) . ? C53 C57 1.499(7) . ? C54 C55 1.389(7) . ? C55 C56 1.388(6) . ? C55 C58 1.512(7) . ? C59 C64 1.384(6) . ? C59 C60 1.390(6) . ? C60 C61 1.386(7) . ? C61 C62 1.372(7) . ? C61 C65 1.532(7) . ? C62 C63 1.392(7) . ? C63 C64 1.391(6) . ? C63 C66 1.503(7) . ? C67 C72 1.385(6) . ? C67 C68 1.392(6) . ? C68 C69 1.382(6) . ? C69 C70 1.366(7) . ? C69 C73 1.542(7) . ? C70 C71 1.395(8) . ? C71 C72 1.389(6) . ? C71 C74 1.506(8) . ? C75 C80 1.398(6) . ? C75 C76 1.401(6) . ? C76 C77 1.368(6) . ? C77 C78 1.402(7) . ? C77 C81 1.502(7) . ? C78 C79 1.391(7) . ? C79 C80 1.387(6) . ? C79 C82 1.510(7) . ? C83 C88 1.383(6) . ? C83 C84 1.391(6) . ? C84 C85 1.392(6) . ? C85 C86 1.378(6) . ? C85 C89 1.505(7) . ? C86 C87 1.389(7) . ? C87 C88 1.394(6) . ? C87 C90 1.519(6) . ? C91 N1 1.415(8) . ? C92 N1 1.429(8) . ? C93 C94 1.370(10) . ? C93 N1 1.467(9) . ? C94 N2 1.472(9) . ? C94 Li2 2.788(13) . ? C95 N2 1.501(12) . ? C96 N2 1.402(11) . ? C97 N3 1.496(8) . ? C98 N3 1.442(9) . ? C99 C100 1.412(10) . ? C99 N3 1.427(8) . ? C100 N4 1.476(9) . ? C100 Li2 2.782(13) . ? C101 N4 1.452(8) . ? C102 N4 1.432(8) . ? N1 Li2 2.080(9) . ? N2 Li2 2.103(10) . ? N3 Li2 2.169(11) . ? N4 Li2 2.112(10) . ? Li1 C4 2.377(4) 2_886 ? Li1 C5 2.400(4) 2_886 ? Li1 C3 2.405(4) 2_886 ? Li1 C2 2.441(4) 2_886 ? Li1 C1 2.445(4) 2_886 ? Li3 C50 2.378(4) 2_675 ? Li3 C49 2.399(4) 2_675 ? Li3 C46 2.409(4) 2_675 ? Li3 C47 2.454(4) 2_675 ? Li3 C48 2.463(4) 2_675 ? 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 C5 C1 C2 108.2(4) . . ? C5 C1 C6 126.3(4) . . ? C2 C1 C6 125.2(4) . . ? C5 C1 Li1 71.3(2) . . ? C2 C1 Li1 72.8(2) . . ? C6 C1 Li1 126.9(3) . . ? C3 C2 C1 107.7(4) . . ? C3 C2 C14 125.7(4) . . ? C1 C2 C14 126.4(4) . . ? C3 C2 Li1 71.6(2) . . ? C1 C2 Li1 73.1(2) . . ? C14 C2 Li1 124.7(3) . . ? C2 C3 C4 107.9(4) . . ? C2 C3 C22 128.0(4) . . ? C4 C3 C22 123.7(4) . . ? C2 C3 Li1 74.3(2) . . ? C4 C3 Li1 71.4(2) . . ? C22 C3 Li1 125.7(3) . . ? C5 C4 C3 107.7(4) . . ? C5 C4 C30 125.6(4) . . ? C3 C4 C30 125.7(4) . . ? C5 C4 Li1 73.6(2) . . ? C3 C4 Li1 73.6(2) . . ? C30 C4 Li1 127.5(3) . . ? C1 C5 C4 108.5(4) . . ? C1 C5 C38 125.5(4) . . ? C4 C5 C38 125.7(4) . . ? C1 C5 Li1 74.8(2) . . ? C4 C5 Li1 71.8(2) . . ? C38 C5 Li1 124.3(3) . . ? C7 C6 C11 117.0(4) . . ? C7 C6 C1 120.4(5) . . ? C11 C6 C1 122.6(4) . . ? C6 C7 C8 121.0(5) . . ? C9 C8 C7 118.7(5) . . ? C9 C8 C12 121.5(6) . . ? C7 C8 C12 119.9(6) . . ? C8 C9 C10 122.0(5) . . ? C11 C10 C9 118.2(5) . . ? C11 C10 C13 120.9(6) . . ? C9 C10 C13 120.9(6) . . ? C10 C11 C6 122.9(5) . . ? C19 C14 C15 116.9(4) . . ? C19 C14 C2 121.8(4) . . ? C15 C14 C2 121.2(4) . . ? C16 C15 C14 122.3(5) . . ? C15 C16 C17 118.8(5) . . ? C15 C16 C20 120.3(5) . . ? C17 C16 C20 121.0(5) . . ? C18 C17 C16 121.0(4) . . ? C19 C18 C17 118.2(5) . . ? C19 C18 C21 121.2(5) . . ? C17 C18 C21 120.6(5) . . ? C18 C19 C14 122.9(5) . . ? C23 C22 C27 117.3(4) . . ? C23 C22 C3 121.2(4) . . ? C27 C22 C3 121.4(4) . . ? C24 C23 C22 122.3(5) . . ? C23 C24 C25 118.5(4) . . ? C23 C24 C28 120.3(5) . . ? C25 C24 C28 121.2(4) . . ? C24 C25 C26 121.6(4) . . ? C27 C26 C25 117.9(5) . . ? C27 C26 C29 120.5(4) . . ? C25 C26 C29 121.6(4) . . ? C26 C27 C22 122.3(4) . . ? C31 C30 C35 116.3(4) . . ? C31 C30 C4 121.9(4) . . ? C35 C30 C4 121.5(4) . . ? C32 C31 C30 123.5(5) . . ? C33 C32 C31 118.2(5) . . ? C33 C32 C36 121.2(5) . . ? C31 C32 C36 120.6(5) . . ? C32 C33 C34 122.7(5) . . ? C35 C34 C33 118.2(5) . . ? C35 C34 C37 117.6(5) . . ? C33 C34 C37 124.3(5) . . ? C34 C35 C30 121.1(5) . . ? C43 C38 C39 117.9(4) . . ? C43 C38 C5 120.7(4) . . ? C39 C38 C5 121.4(4) . . ? C40 C39 C38 121.0(5) . . ? C41 C40 C39 119.0(5) . . ? C41 C40 C44 121.5(5) . . ? C39 C40 C44 119.5(5) . . ? C40 C41 C42 121.9(5) . . ? C41 C42 C43 118.7(5) . . ? C41 C42 C45 122.1(5) . . ? C43 C42 C45 119.2(5) . . ? C42 C43 C38 121.6(5) . . ? C50 C46 C47 108.2(3) . . ? C50 C46 C51 124.4(4) . . ? C47 C46 C51 126.9(4) . . ? C50 C46 Li3 71.6(2) . . ? C47 C46 Li3 74.7(2) . . ? C51 C46 Li3 125.2(3) . . ? C46 C47 C48 107.4(4) . . ? C46 C47 C59 124.9(4) . . ? C48 C47 C59 127.3(4) . . ? C46 C47 Li3 71.3(2) . . ? C48 C47 Li3 73.5(2) . . ? C59 C47 Li3 126.7(3) . . ? C49 C48 C47 108.0(3) . . ? C49 C48 C67 126.3(4) . . ? C47 C48 C67 125.5(4) . . ? C49 C48 Li3 70.5(2) . . ? C47 C48 Li3 72.7(2) . . ? C67 C48 Li3 126.6(3) . . ? C50 C49 C48 107.9(4) . . ? C50 C49 C75 126.0(4) . . ? C48 C49 C75 125.8(4) . . ? C50 C49 Li3 72.0(3) . . ? C48 C49 Li3 75.4(3) . . ? C75 C49 Li3 123.5(3) . . ? C49 C50 C46 108.4(4) . . ? C49 C50 C83 126.4(4) . . ? C46 C50 C83 124.6(4) . . ? C49 C50 Li3 73.6(2) . . ? C46 C50 Li3 74.0(2) . . ? C83 C50 Li3 125.1(3) . . ? C52 C51 C56 117.5(4) . . ? C52 C51 C46 121.5(4) . . ? C56 C51 C46 120.6(4) . . ? C51 C52 C53 122.2(4) . . ? C54 C53 C52 118.2(4) . . ? C54 C53 C57 121.3(4) . . ? C52 C53 C57 120.5(5) . . ? C53 C54 C55 122.1(4) . . ? C56 C55 C54 117.4(5) . . ? C56 C55 C58 120.6(5) . . ? C54 C55 C58 121.9(5) . . ? C51 C56 C55 122.6(4) . . ? C64 C59 C60 117.1(4) . . ? C64 C59 C47 122.1(4) . . ? C60 C59 C47 120.7(4) . . ? C61 C60 C59 123.2(5) . . ? C62 C61 C60 117.4(5) . . ? C62 C61 C65 122.1(5) . . ? C60 C61 C65 120.5(5) . . ? C61 C62 C63 122.2(5) . . ? C64 C63 C62 118.1(4) . . ? C64 C63 C66 120.4(5) . . ? C62 C63 C66 121.5(5) . . ? C59 C64 C63 121.9(4) . . ? C72 C67 C68 117.4(4) . . ? C72 C67 C48 121.8(4) . . ? C68 C67 C48 120.8(4) . . ? C69 C68 C67 122.0(5) . . ? C70 C69 C68 118.3(5) . . ? C70 C69 C73 121.0(5) . . ? C68 C69 C73 120.7(5) . . ? C69 C70 C71 122.5(5) . . ? C72 C71 C70 117.1(5) . . ? C72 C71 C74 120.8(5) . . ? C70 C71 C74 122.1(5) . . ? C67 C72 C71 122.5(5) . . ? C80 C75 C76 117.1(4) . . ? C80 C75 C49 121.9(4) . . ? C76 C75 C49 121.0(4) . . ? C77 C76 C75 122.2(5) . . ? C76 C77 C78 118.9(4) . . ? C76 C77 C81 120.9(5) . . ? C78 C77 C81 120.3(5) . . ? C79 C78 C77 121.3(4) . . ? C80 C79 C78 117.8(5) . . ? C80 C79 C82 121.3(5) . . ? C78 C79 C82 120.9(5) . . ? C79 C80 C75 122.7(4) . . ? C88 C83 C84 117.7(4) . . ? C88 C83 C50 120.8(4) . . ? C84 C83 C50 121.4(4) . . ? C83 C84 C85 122.0(4) . . ? C86 C85 C84 118.2(4) . . ? C86 C85 C89 121.6(4) . . ? C84 C85 C89 120.2(4) . . ? C85 C86 C87 121.9(4) . . ? C86 C87 C88 118.0(4) . . ? C86 C87 C90 122.9(4) . . ? C88 C87 C90 119.1(5) . . ? C83 C88 C87 122.1(4) . . ? C94 C93 N1 116.6(7) . . ? C93 C94 N2 121.7(8) . . ? C93 C94 Li2 77.4(6) . . ? N2 C94 Li2 47.8(4) . . ? C100 C99 N3 115.1(7) . . ? C99 C100 N4 117.2(7) . . ? C99 C100 Li2 77.8(5) . . ? N4 C100 Li2 48.4(4) . . ? C91 N1 C92 109.2(5) . . ? C91 N1 C93 104.7(6) . . ? C92 N1 C93 110.7(5) . . ? C91 N1 Li2 117.3(5) . . ? C92 N1 Li2 110.5(5) . . ? C93 N1 Li2 104.3(5) . . ? C96 N2 C94 103.7(7) . . ? C96 N2 C95 108.1(7) . . ? C94 N2 C95 111.5(7) . . ? C96 N2 Li2 119.2(6) . . ? C94 N2 Li2 101.0(5) . . ? C95 N2 Li2 112.7(6) . . ? C99 N3 C98 107.5(6) . . ? C99 N3 C97 110.7(6) . . ? C98 N3 C97 108.9(6) . . ? C99 N3 Li2 102.5(5) . . ? C98 N3 Li2 116.8(5) . . ? C97 N3 Li2 110.2(5) . . ? C102 N4 C101 109.5(5) . . ? C102 N4 C100 108.1(6) . . ? C101 N4 C100 111.2(6) . . ? C102 N4 Li2 119.4(5) . . ? C101 N4 Li2 108.2(5) . . ? C100 N4 Li2 100.2(5) . . ? C4 Li1 C4 180.0(2) 2_886 . ? C4 Li1 C5 34.61(14) 2_886 2_886 ? C4 Li1 C5 145.39(14) . 2_886 ? C4 Li1 C5 145.39(14) 2_886 . ? C4 Li1 C5 34.61(14) . . ? C5 Li1 C5 180.000(1) 2_886 . ? C4 Li1 C3 34.98(14) 2_886 2_886 ? C4 Li1 C3 145.02(14) . 2_886 ? C5 Li1 C3 57.41(14) 2_886 2_886 ? C5 Li1 C3 122.59(14) . 2_886 ? C4 Li1 C3 145.02(14) 2_886 . ? C4 Li1 C3 34.98(14) . . ? C5 Li1 C3 122.59(14) 2_886 . ? C5 Li1 C3 57.41(14) . . ? C3 Li1 C3 180.000(2) 2_886 . ? C4 Li1 C2 122.70(14) 2_886 . ? C4 Li1 C2 57.30(14) . . ? C5 Li1 C2 123.13(14) 2_886 . ? C5 Li1 C2 56.87(14) . . ? C3 Li1 C2 145.91(14) 2_886 . ? C3 Li1 C2 34.09(14) . . ? C4 Li1 C2 57.30(14) 2_886 2_886 ? C4 Li1 C2 122.70(14) . 2_886 ? C5 Li1 C2 56.87(14) 2_886 2_886 ? C5 Li1 C2 123.13(14) . 2_886 ? C3 Li1 C2 34.09(14) 2_886 2_886 ? C3 Li1 C2 145.91(14) . 2_886 ? C2 Li1 C2 180.000(2) . 2_886 ? C4 Li1 C1 123.08(15) 2_886 . ? C4 Li1 C1 56.92(15) . . ? C5 Li1 C1 146.15(14) 2_886 . ? C5 Li1 C1 33.85(14) . . ? C3 Li1 C1 123.23(14) 2_886 . ? C3 Li1 C1 56.77(14) . . ? C2 Li1 C1 34.15(13) . . ? C2 Li1 C1 145.85(13) 2_886 . ? C4 Li1 C1 56.92(15) 2_886 2_886 ? C4 Li1 C1 123.08(15) . 2_886 ? C5 Li1 C1 33.85(14) 2_886 2_886 ? C5 Li1 C1 146.15(14) . 2_886 ? C3 Li1 C1 56.77(14) 2_886 2_886 ? C3 Li1 C1 123.23(14) . 2_886 ? C2 Li1 C1 145.85(13) . 2_886 ? C2 Li1 C1 34.15(13) 2_886 2_886 ? C1 Li1 C1 180.000(1) . 2_886 ? C50 Li3 C50 180.00(16) . 2_675 ? C50 Li3 C49 34.41(14) . . ? C50 Li3 C49 145.59(14) 2_675 . ? C50 Li3 C49 145.59(14) . 2_675 ? C50 Li3 C49 34.41(14) 2_675 2_675 ? C49 Li3 C49 180.000(1) . 2_675 ? C50 Li3 C46 34.46(14) . . ? C50 Li3 C46 145.54(14) 2_675 . ? C49 Li3 C46 57.07(14) . . ? C49 Li3 C46 122.93(14) 2_675 . ? C50 Li3 C46 145.54(14) . 2_675 ? C50 Li3 C46 34.46(14) 2_675 2_675 ? C49 Li3 C46 122.93(14) . 2_675 ? C49 Li3 C46 57.07(14) 2_675 2_675 ? C46 Li3 C46 180.0(2) . 2_675 ? C50 Li3 C47 56.91(14) . . ? C50 Li3 C47 123.09(14) 2_675 . ? C49 Li3 C47 56.86(14) . . ? C49 Li3 C47 123.14(14) 2_675 . ? C46 Li3 C47 34.05(13) . . ? C46 Li3 C47 145.95(13) 2_675 . ? C50 Li3 C47 123.09(14) . 2_675 ? C50 Li3 C47 56.91(14) 2_675 2_675 ? C49 Li3 C47 123.14(14) . 2_675 ? C49 Li3 C47 56.86(14) 2_675 2_675 ? C46 Li3 C47 145.95(13) . 2_675 ? C46 Li3 C47 34.05(13) 2_675 2_675 ? C47 Li3 C47 180.0(2) . 2_675 ? C50 Li3 C48 56.59(14) . . ? C50 Li3 C48 123.41(14) 2_675 . ? C49 Li3 C48 34.08(14) . . ? C49 Li3 C48 145.92(14) 2_675 . ? C46 Li3 C48 56.34(13) . . ? C46 Li3 C48 123.66(13) 2_675 . ? C47 Li3 C48 33.83(13) . . ? C47 Li3 C48 146.17(13) 2_675 . ? C50 Li3 C48 123.41(14) . 2_675 ? C50 Li3 C48 56.59(14) 2_675 2_675 ? C49 Li3 C48 145.92(14) . 2_675 ? C49 Li3 C48 34.08(14) 2_675 2_675 ? C46 Li3 C48 123.66(13) . 2_675 ? C46 Li3 C48 56.34(13) 2_675 2_675 ? C47 Li3 C48 146.17(13) . 2_675 ? C47 Li3 C48 33.83(13) 2_675 2_675 ? C48 Li3 C48 180.00(15) . 2_675 ? N1 Li2 N2 88.2(4) . . ? N1 Li2 N4 120.6(5) . . ? N2 Li2 N4 122.6(5) . . ? N1 Li2 N3 124.5(5) . . ? N2 Li2 N3 118.5(4) . . ? N4 Li2 N3 86.5(4) . . ? N1 Li2 C100 127.8(4) . . ? N2 Li2 C100 141.4(4) . . ? N4 Li2 C100 31.5(2) . . ? N3 Li2 C100 56.3(3) . . ? N1 Li2 C94 57.3(3) . . ? N2 Li2 C94 31.2(2) . . ? N4 Li2 C94 139.4(5) . . ? N3 Li2 C94 130.2(4) . . ? C100 Li2 C94 169.9(5) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 22.46 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.448 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.058 data_ccd582s _database_code_CSD 200150 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(lithium)bis(penta(3,5-dimethylphenyl)cyclopentadienide] [lithium(tetrahydrofuran)](tetrahydrofuran) ; _chemical_name_common ; ((lithium)bis(penta(3,5-dimethylphenyl)cyclopentadienide) (lithium(tetrahydrofuran))(tetrahydrofuran) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H106 Li2 O2' _chemical_formula_weight 1329.71 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.997(4) _cell_length_b 15.486(4) _cell_length_c 20.198(5) _cell_angle_alpha 97.393(4) _cell_angle_beta 102.993(5) _cell_angle_gamma 96.523(4) _cell_volume 4184.2(18) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.055 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.060 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9804 _exptl_absorpt_correction_T_max 0.9874 _exptl_absorpt_process_details ? _exptl_crystal_preparation ; crystallized from toluene ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20273 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0679 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 22.46 _reflns_number_total 10298 _reflns_number_gt 6519 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1284P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10298 _refine_ls_number_parameters 886 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1380 _refine_ls_R_factor_gt 0.0933 _refine_ls_wR_factor_ref 0.2726 _refine_ls_wR_factor_gt 0.2534 _refine_ls_goodness_of_fit_ref 1.305 _refine_ls_restrained_S_all 1.305 _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 O1 O 0.2692(6) 0.1544(6) 0.2599(4) 0.166(3) Uani 1 1 d . . . Li1 Li 0.0000 0.0000 0.0000 0.056(3) Uani 1 2 d S . . Li2 Li 0.5000 0.5000 0.5000 0.052(3) Uani 1 2 d S . . Li2 Li 0.1836(13) 0.1116(12) 0.1780(11) 0.065(5) Uani 0.50 1 d P . . Li2' Li 0.3170(12) 0.2953(12) 0.3730(9) 0.056(5) Uani 0.50 1 d P . . C1 C 0.1363(3) -0.0046(3) 0.0986(2) 0.0403(12) Uani 1 1 d . . . C2 C 0.0519(3) 0.0117(3) 0.1248(2) 0.0378(12) Uani 1 1 d . . . C3 C 0.0266(3) 0.0954(3) 0.1099(2) 0.0402(12) Uani 1 1 d . . . C4 C 0.0950(3) 0.1303(3) 0.0735(3) 0.0429(13) Uani 1 1 d . . . C5 C 0.1615(3) 0.0679(3) 0.0663(2) 0.0407(12) Uani 1 1 d . . . C6 C 0.1930(3) -0.0783(3) 0.1088(2) 0.0413(12) Uani 1 1 d . . . C7 C 0.1481(4) -0.1651(3) 0.0947(3) 0.0502(14) Uani 1 1 d . . . H7 H 0.0797 -0.1777 0.0776 0.060 Uiso 1 1 calc R . . C8 C 0.2022(4) -0.2339(3) 0.1052(3) 0.0565(15) Uani 1 1 d . . . C9 C 0.3059(4) -0.2139(4) 0.1305(3) 0.0567(15) Uani 1 1 d . . . H9 H 0.3432 -0.2594 0.1370 0.068 Uiso 1 1 calc R . . C10 C 0.3529(4) -0.1279(4) 0.1457(3) 0.0474(13) Uani 1 1 d . . . C11 C 0.2961(4) -0.0615(3) 0.1346(2) 0.0436(13) Uani 1 1 d . . . H11 H 0.3274 -0.0034 0.1445 0.052 Uiso 1 1 calc R . . C12 C 0.1519(5) -0.3277(4) 0.0919(4) 0.090(2) Uani 1 1 d . . . H12A H 0.0817 -0.3295 0.0752 0.135 Uiso 1 1 calc R . . H12B H 0.1649 -0.3520 0.1339 0.135 Uiso 1 1 calc R . . H12C H 0.1770 -0.3615 0.0581 0.135 Uiso 1 1 calc R . . C13 C 0.4629(4) -0.1085(4) 0.1755(3) 0.0722(18) Uani 1 1 d . . . H13A H 0.4837 -0.0461 0.1835 0.108 Uiso 1 1 calc R . . H13B H 0.4962 -0.1363 0.1438 0.108 Uiso 1 1 calc R . . H13C H 0.4790 -0.1309 0.2182 0.108 Uiso 1 1 calc R . . C14 C 0.0064(3) -0.0429(3) 0.1697(2) 0.0393(12) Uani 1 1 d . . . C15 C -0.0944(4) -0.0597(3) 0.1609(3) 0.0442(13) Uani 1 1 d . . . H15 H -0.1350 -0.0397 0.1247 0.053 Uiso 1 1 calc R . . C16 C -0.1383(4) -0.1053(4) 0.2037(3) 0.0581(15) Uani 1 1 d . . . C17 C -0.0752(4) -0.1351(4) 0.2572(3) 0.0640(16) Uani 1 1 d . . . H17 H -0.1026 -0.1662 0.2865 0.077 Uiso 1 1 calc R . . C18 C 0.0264(4) -0.1198(4) 0.2677(3) 0.0538(14) Uani 1 1 d . . . C19 C 0.0661(4) -0.0734(3) 0.2233(3) 0.0487(13) Uani 1 1 d . . . H19 H 0.1345 -0.0627 0.2298 0.058 Uiso 1 1 calc R . . C20 C -0.2497(4) -0.1241(5) 0.1928(4) 0.088(2) Uani 1 1 d . . . H20A H -0.2654 -0.1557 0.2278 0.132 Uiso 1 1 calc R . . H20B H -0.2782 -0.1590 0.1483 0.132 Uiso 1 1 calc R . . H20C H -0.2763 -0.0696 0.1953 0.132 Uiso 1 1 calc R . . C21 C 0.0927(5) -0.1518(5) 0.3266(3) 0.081(2) Uani 1 1 d . . . H21A H 0.0527 -0.1817 0.3520 0.122 Uiso 1 1 calc R . . H21B H 0.1354 -0.1024 0.3565 0.122 Uiso 1 1 calc R . . H21C H 0.1321 -0.1915 0.3088 0.122 Uiso 1 1 calc R . . C22 C -0.0449(4) 0.1439(3) 0.1375(3) 0.0454(13) Uani 1 1 d . . . C23 C -0.0479(4) 0.1491(3) 0.2060(3) 0.0576(15) Uani 1 1 d . . . H23 H -0.0081 0.1174 0.2341 0.069 Uiso 1 1 calc R . . C24 C -0.1084(5) 0.1998(4) 0.2332(3) 0.0758(19) Uani 1 1 d . . . C25 C -0.1660(5) 0.2481(4) 0.1928(4) 0.077(2) Uani 1 1 d . . . H25 H -0.2053 0.2837 0.2119 0.092 Uiso 1 1 calc R . . C26 C -0.1664(4) 0.2447(4) 0.1230(4) 0.0624(16) Uani 1 1 d . . . C27 C -0.1062(4) 0.1913(3) 0.0971(3) 0.0533(15) Uani 1 1 d . . . H27 H -0.1069 0.1869 0.0506 0.064 Uiso 1 1 calc R . . C28 C -0.1087(7) 0.2025(5) 0.3086(4) 0.117(3) Uani 1 1 d . . . H28A H -0.1550 0.2397 0.3200 0.176 Uiso 1 1 calc R . . H28B H -0.0435 0.2254 0.3367 0.176 Uiso 1 1 calc R . . H28C H -0.1278 0.1440 0.3168 0.176 Uiso 1 1 calc R . . C29 C -0.2289(5) 0.2978(5) 0.0788(4) 0.096(2) Uani 1 1 d . . . H29A H -0.2193 0.2879 0.0330 0.144 Uiso 1 1 calc R . . H29B H -0.2101 0.3592 0.0976 0.144 Uiso 1 1 calc R . . H29C H -0.2975 0.2804 0.0775 0.144 Uiso 1 1 calc R . . C30 C 0.1008(3) 0.2185(3) 0.0512(3) 0.0408(12) Uani 1 1 d . . . C31 C 0.0918(4) 0.2930(3) 0.0948(3) 0.0506(14) Uani 1 1 d . . . H31 H 0.0851 0.2872 0.1389 0.061 Uiso 1 1 calc R . . C32 C 0.0925(4) 0.3744(3) 0.0753(3) 0.0568(15) Uani 1 1 d . . . C33 C 0.1085(4) 0.3830(3) 0.0098(3) 0.0588(15) Uani 1 1 d . . . H33 H 0.1116 0.4380 -0.0039 0.071 Uiso 1 1 calc R . . C34 C 0.1195(4) 0.3120(3) -0.0335(3) 0.0532(14) Uani 1 1 d . . . C35 C 0.1167(3) 0.2293(3) -0.0128(3) 0.0432(13) Uani 1 1 d . . . H35 H 0.1255 0.1811 -0.0422 0.052 Uiso 1 1 calc R . . C36 C 0.0757(6) 0.4516(4) 0.1228(4) 0.092(2) Uani 1 1 d . . . H36A H 0.0786 0.5033 0.1013 0.139 Uiso 1 1 calc R . . H36B H 0.1260 0.4612 0.1651 0.139 Uiso 1 1 calc R . . H36C H 0.0117 0.4395 0.1322 0.139 Uiso 1 1 calc R . . C37 C 0.1317(6) 0.3201(4) -0.1058(3) 0.088(2) Uani 1 1 d . . . H37A H 0.1380 0.2636 -0.1288 0.131 Uiso 1 1 calc R . . H37B H 0.1901 0.3610 -0.1027 0.131 Uiso 1 1 calc R . . H37C H 0.0747 0.3409 -0.1313 0.131 Uiso 1 1 calc R . . C38 C 0.2493(3) 0.0794(3) 0.0368(2) 0.0406(12) Uani 1 1 d . . . C39 C 0.3220(3) 0.1537(3) 0.0598(3) 0.0443(13) Uani 1 1 d . . . H39 H 0.3123 0.1988 0.0916 0.053 Uiso 1 1 calc R . . C40 C 0.4070(4) 0.1618(3) 0.0368(3) 0.0507(14) Uani 1 1 d . . . C41 C 0.4174(4) 0.0948(4) -0.0135(3) 0.0546(15) Uani 1 1 d . . . H41 H 0.4736 0.1004 -0.0308 0.066 Uiso 1 1 calc R . . C42 C 0.3477(4) 0.0210(3) -0.0381(3) 0.0479(13) Uani 1 1 d . . . C43 C 0.2647(3) 0.0145(3) -0.0116(2) 0.0426(12) Uani 1 1 d . . . H43 H 0.2174 -0.0356 -0.0271 0.051 Uiso 1 1 calc R . . C44 C 0.4858(4) 0.2423(4) 0.0646(4) 0.080(2) Uani 1 1 d . . . H44A H 0.4648 0.2812 0.0977 0.120 Uiso 1 1 calc R . . H44B H 0.4953 0.2725 0.0273 0.120 Uiso 1 1 calc R . . H44C H 0.5471 0.2242 0.0861 0.120 Uiso 1 1 calc R . . C45 C 0.3588(4) -0.0507(4) -0.0931(3) 0.0679(17) Uani 1 1 d . . . H45A H 0.3034 -0.0969 -0.1025 0.102 Uiso 1 1 calc R . . H45B H 0.4190 -0.0740 -0.0774 0.102 Uiso 1 1 calc R . . H45C H 0.3609 -0.0267 -0.1344 0.102 Uiso 1 1 calc R . . C46 C 0.3545(3) 0.4446(3) 0.4068(3) 0.0442(13) Uani 1 1 d . . . C47 C 0.3405(3) 0.4068(3) 0.4658(3) 0.0440(13) Uani 1 1 d . . . C48 C 0.4123(4) 0.3491(3) 0.4808(2) 0.0441(13) Uani 1 1 d . . . C49 C 0.4708(3) 0.3521(3) 0.4313(2) 0.0414(12) Uani 1 1 d . . . C50 C 0.4352(4) 0.4111(3) 0.3856(2) 0.0444(13) Uani 1 1 d . . . C51 C 0.2898(4) 0.5020(3) 0.3702(2) 0.0460(13) Uani 1 1 d . . . C52 C 0.3297(4) 0.5793(4) 0.3524(3) 0.0509(14) Uani 1 1 d . . . H52 H 0.3978 0.5973 0.3661 0.061 Uiso 1 1 calc R . . C53 C 0.2694(5) 0.6308(4) 0.3142(3) 0.0582(15) Uani 1 1 d . . . C54 C 0.1674(5) 0.6025(5) 0.2958(3) 0.0700(18) Uani 1 1 d . . . H54 H 0.1263 0.6367 0.2713 0.084 Uiso 1 1 calc R . . C55 C 0.1244(4) 0.5246(5) 0.3126(3) 0.0630(16) Uani 1 1 d . . . C56 C 0.1868(4) 0.4765(4) 0.3498(3) 0.0548(15) Uani 1 1 d . . . H56 H 0.1597 0.4250 0.3620 0.066 Uiso 1 1 calc R . . C57 C 0.3156(5) 0.7133(5) 0.2959(4) 0.095(2) Uani 1 1 d . . . H57A H 0.2648 0.7416 0.2708 0.142 Uiso 1 1 calc R . . H57B H 0.3605 0.6991 0.2679 0.142 Uiso 1 1 calc R . . H57C H 0.3513 0.7521 0.3372 0.142 Uiso 1 1 calc R . . C58 C 0.0146(4) 0.4966(5) 0.2900(3) 0.098(2) Uani 1 1 d . . . H58A H -0.0155 0.5393 0.2650 0.147 Uiso 1 1 calc R . . H58B H -0.0117 0.4923 0.3296 0.147 Uiso 1 1 calc R . . H58C H 0.0006 0.4404 0.2608 0.147 Uiso 1 1 calc R . . C59 C 0.2580(3) 0.4202(3) 0.4994(2) 0.0432(13) Uani 1 1 d . . . C60 C 0.2354(3) 0.5048(3) 0.5157(2) 0.0429(13) Uani 1 1 d . . . H60 H 0.2740 0.5530 0.5070 0.051 Uiso 1 1 calc R . . C61 C 0.1564(4) 0.5179(4) 0.5445(3) 0.0522(14) Uani 1 1 d . . . C62 C 0.0999(4) 0.4460(4) 0.5565(3) 0.0639(16) Uani 1 1 d . . . H62 H 0.0454 0.4545 0.5744 0.077 Uiso 1 1 calc R . . C63 C 0.1208(4) 0.3612(4) 0.5430(3) 0.0591(15) Uani 1 1 d . . . C64 C 0.1994(4) 0.3500(4) 0.5139(3) 0.0569(15) Uani 1 1 d . . . H64 H 0.2138 0.2933 0.5035 0.068 Uiso 1 1 calc R . . C65 C 0.1365(4) 0.6098(4) 0.5630(3) 0.0778(19) Uani 1 1 d . . . H65A H 0.1835 0.6507 0.5504 0.117 Uiso 1 1 calc R . . H65B H 0.1426 0.6224 0.6117 0.117 Uiso 1 1 calc R . . H65C H 0.0706 0.6153 0.5389 0.117 Uiso 1 1 calc R . . C66 C 0.0609(5) 0.2843(4) 0.5583(4) 0.097(2) Uani 1 1 d . . . H66A H 0.0098 0.3039 0.5787 0.146 Uiso 1 1 calc R . . H66B H 0.1029 0.2550 0.5898 0.146 Uiso 1 1 calc R . . H66C H 0.0312 0.2442 0.5165 0.146 Uiso 1 1 calc R . . C67 C 0.4156(4) 0.2925(3) 0.5345(3) 0.0443(13) Uani 1 1 d . . . C68 C 0.4103(4) 0.3250(3) 0.6004(3) 0.0510(14) Uani 1 1 d . . . H68 H 0.4099 0.3851 0.6117 0.061 Uiso 1 1 calc R . . C69 C 0.4055(4) 0.2724(4) 0.6505(3) 0.0555(15) Uani 1 1 d . . . C70 C 0.4060(4) 0.1833(4) 0.6328(3) 0.0632(16) Uani 1 1 d . . . H70 H 0.4022 0.1468 0.6655 0.076 Uiso 1 1 calc R . . C71 C 0.4119(4) 0.1468(4) 0.5685(3) 0.0638(16) Uani 1 1 d . . . C72 C 0.4170(4) 0.2021(4) 0.5200(3) 0.0541(14) Uani 1 1 d . . . H72 H 0.4215 0.1781 0.4764 0.065 Uiso 1 1 calc R . . C73 C 0.3997(6) 0.3122(4) 0.7211(3) 0.087(2) Uani 1 1 d . . . H73A H 0.4017 0.3747 0.7235 0.130 Uiso 1 1 calc R . . H73B H 0.4548 0.3001 0.7548 0.130 Uiso 1 1 calc R . . H73C H 0.3389 0.2872 0.7302 0.130 Uiso 1 1 calc R . . C74 C 0.4157(6) 0.0501(4) 0.5514(4) 0.103(3) Uani 1 1 d . . . H74A H 0.4203 0.0365 0.5046 0.155 Uiso 1 1 calc R . . H74B H 0.3566 0.0169 0.5571 0.155 Uiso 1 1 calc R . . H74C H 0.4726 0.0349 0.5816 0.155 Uiso 1 1 calc R . . C75 C 0.5440(3) 0.2917(3) 0.4216(3) 0.0422(13) Uani 1 1 d . . . C76 C 0.6147(4) 0.2746(3) 0.4762(3) 0.0460(13) Uani 1 1 d . . . H76 H 0.6188 0.3036 0.5203 0.055 Uiso 1 1 calc R . . C77 C 0.6805(4) 0.2146(3) 0.4671(3) 0.0533(14) Uani 1 1 d . . . C78 C 0.6736(4) 0.1719(3) 0.4016(3) 0.0549(15) Uani 1 1 d . . . H78 H 0.7164 0.1316 0.3950 0.066 Uiso 1 1 calc R . . C79 C 0.6044(4) 0.1878(3) 0.3458(3) 0.0559(15) Uani 1 1 d . . . C80 C 0.5400(4) 0.2454(3) 0.3565(3) 0.0475(13) Uani 1 1 d . . . H80 H 0.4917 0.2541 0.3191 0.057 Uiso 1 1 calc R . . C81 C 0.7548(5) 0.1964(4) 0.5277(3) 0.0774(19) Uani 1 1 d . . . H81A H 0.7488 0.2319 0.5688 0.116 Uiso 1 1 calc R . . H81B H 0.8204 0.2103 0.5214 0.116 Uiso 1 1 calc R . . H81C H 0.7427 0.1353 0.5318 0.116 Uiso 1 1 calc R . . C82 C 0.5979(5) 0.1417(4) 0.2741(3) 0.091(2) Uani 1 1 d . . . H82A H 0.5452 0.1599 0.2421 0.136 Uiso 1 1 calc R . . H82B H 0.5851 0.0791 0.2726 0.136 Uiso 1 1 calc R . . H82C H 0.6595 0.1567 0.2618 0.136 Uiso 1 1 calc R . . C83 C 0.4706(4) 0.4262(3) 0.3235(2) 0.0403(12) Uani 1 1 d . . . C84 C 0.5706(4) 0.4412(3) 0.3246(3) 0.0450(13) Uani 1 1 d . . . H84 H 0.6173 0.4451 0.3661 0.054 Uiso 1 1 calc R . . C85 C 0.6027(4) 0.4503(3) 0.2658(3) 0.0510(14) Uani 1 1 d . . . C86 C 0.5321(4) 0.4457(3) 0.2040(3) 0.0561(15) Uani 1 1 d . . . H86 H 0.5530 0.4510 0.1639 0.067 Uiso 1 1 calc R . . C87 C 0.4320(4) 0.4334(3) 0.2010(3) 0.0492(14) Uani 1 1 d . . . C88 C 0.4034(4) 0.4227(3) 0.2608(3) 0.0492(14) Uani 1 1 d . . . H88 H 0.3360 0.4126 0.2590 0.059 Uiso 1 1 calc R . . C89 C 0.7126(4) 0.4662(4) 0.2688(3) 0.0726(18) Uani 1 1 d . . . H89A H 0.7217 0.4726 0.2239 0.109 Uiso 1 1 calc R . . H89B H 0.7426 0.4170 0.2838 0.109 Uiso 1 1 calc R . . H89C H 0.7431 0.5188 0.3006 0.109 Uiso 1 1 calc R . . C90 C 0.3562(5) 0.4306(4) 0.1350(3) 0.0799(19) Uani 1 1 d . . . H90A H 0.2910 0.4216 0.1429 0.120 Uiso 1 1 calc R . . H90B H 0.3631 0.3831 0.1016 0.120 Uiso 1 1 calc R . . H90C H 0.3661 0.4852 0.1180 0.120 Uiso 1 1 calc R . . C91 C 0.2979(7) 0.0973(7) 0.3150(4) 0.148(5) Uani 1 1 d . . . H91A H 0.3667 0.1131 0.3404 0.178 Uiso 1 1 calc R . . H91B H 0.2843 0.0350 0.2965 0.178 Uiso 1 1 calc R . . C92 C 0.2263(7) 0.1248(8) 0.3577(4) 0.154(5) Uani 1 1 d . . . H92A H 0.1686 0.0801 0.3487 0.185 Uiso 1 1 calc R . . H92B H 0.2583 0.1337 0.4065 0.185 Uiso 1 1 calc R . . C93 C 0.1992(15) 0.2030(8) 0.3381(10) 0.298(14) Uani 1 1 d . . . H93A H 0.2374 0.2491 0.3747 0.358 Uiso 1 1 calc R . . H93B H 0.1307 0.2016 0.3408 0.358 Uiso 1 1 calc R . . C94 C 0.2038(15) 0.2348(8) 0.2765(11) 0.313(14) Uani 1 1 d . . . H94A H 0.2405 0.2936 0.2832 0.375 Uiso 1 1 calc R . . H94B H 0.1400 0.2298 0.2441 0.375 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 O1 0.198(7) 0.164(7) 0.092(5) -0.049(5) 0.028(5) -0.064(6) Li1 0.050(8) 0.042(7) 0.077(10) 0.012(6) 0.018(7) -0.001(6) Li2 0.060(8) 0.068(8) 0.030(7) 0.014(6) 0.013(6) 0.006(6) Li2 0.054(11) 0.056(12) 0.077(14) 0.013(10) 0.005(10) -0.009(9) Li2' 0.049(11) 0.068(12) 0.040(11) 0.018(9) -0.010(8) -0.003(9) C1 0.041(3) 0.036(3) 0.041(3) 0.010(2) 0.005(2) -0.001(2) C2 0.045(3) 0.034(3) 0.033(3) 0.009(2) 0.007(2) 0.001(2) C3 0.038(3) 0.041(3) 0.042(3) 0.007(2) 0.012(2) 0.003(2) C4 0.044(3) 0.032(3) 0.049(3) 0.002(2) 0.008(3) 0.000(2) C5 0.037(3) 0.044(3) 0.040(3) 0.011(2) 0.007(2) 0.003(2) C6 0.039(3) 0.042(3) 0.044(3) 0.012(2) 0.012(2) 0.000(2) C7 0.043(3) 0.057(4) 0.051(4) 0.020(3) 0.008(3) 0.004(3) C8 0.063(4) 0.039(3) 0.069(4) 0.023(3) 0.013(3) 0.007(3) C9 0.061(4) 0.057(4) 0.061(4) 0.028(3) 0.017(3) 0.022(3) C10 0.045(3) 0.057(4) 0.042(3) 0.016(3) 0.007(3) 0.012(3) C11 0.048(3) 0.040(3) 0.040(3) 0.011(2) 0.005(3) 0.004(3) C12 0.091(5) 0.050(4) 0.126(6) 0.024(4) 0.013(4) 0.014(4) C13 0.044(4) 0.089(5) 0.088(5) 0.032(4) 0.011(3) 0.016(3) C14 0.036(3) 0.041(3) 0.040(3) 0.009(2) 0.007(2) 0.002(2) C15 0.048(3) 0.043(3) 0.042(3) 0.016(2) 0.005(3) 0.007(2) C16 0.061(4) 0.061(4) 0.056(4) 0.025(3) 0.018(3) 0.001(3) C17 0.073(4) 0.068(4) 0.066(4) 0.040(3) 0.031(4) 0.014(3) C18 0.059(4) 0.070(4) 0.038(3) 0.025(3) 0.009(3) 0.019(3) C19 0.040(3) 0.057(3) 0.052(4) 0.021(3) 0.010(3) 0.006(3) C20 0.051(4) 0.124(6) 0.100(5) 0.055(5) 0.026(4) 0.005(4) C21 0.077(4) 0.115(6) 0.064(4) 0.053(4) 0.015(4) 0.026(4) C22 0.051(3) 0.035(3) 0.051(4) 0.009(3) 0.013(3) 0.003(3) C23 0.080(4) 0.043(3) 0.054(4) 0.004(3) 0.027(3) 0.007(3) C24 0.102(5) 0.058(4) 0.078(5) -0.002(4) 0.051(4) 0.013(4) C25 0.079(5) 0.048(4) 0.114(6) 0.001(4) 0.050(5) 0.014(3) C26 0.053(4) 0.049(4) 0.087(5) 0.009(3) 0.023(4) 0.008(3) C27 0.055(3) 0.041(3) 0.063(4) 0.004(3) 0.021(3) -0.005(3) C28 0.171(8) 0.120(7) 0.077(5) 0.002(5) 0.061(6) 0.042(6) C29 0.063(4) 0.085(5) 0.153(7) 0.038(5) 0.031(5) 0.034(4) C30 0.038(3) 0.037(3) 0.046(3) 0.009(2) 0.008(3) 0.002(2) C31 0.057(3) 0.039(3) 0.052(4) 0.008(3) 0.010(3) -0.001(3) C32 0.063(4) 0.029(3) 0.072(4) 0.005(3) 0.009(3) -0.001(3) C33 0.068(4) 0.038(3) 0.068(4) 0.020(3) 0.007(3) 0.001(3) C34 0.055(3) 0.045(3) 0.058(4) 0.014(3) 0.010(3) 0.000(3) C35 0.044(3) 0.038(3) 0.046(3) 0.009(2) 0.007(3) 0.004(2) C36 0.142(7) 0.036(3) 0.101(5) 0.000(3) 0.045(5) 0.005(4) C37 0.133(6) 0.066(4) 0.072(5) 0.036(4) 0.031(4) 0.007(4) C38 0.037(3) 0.038(3) 0.043(3) 0.010(2) 0.003(2) 0.005(2) C39 0.044(3) 0.040(3) 0.047(3) 0.007(2) 0.010(3) 0.003(3) C40 0.037(3) 0.049(3) 0.064(4) 0.015(3) 0.006(3) -0.001(3) C41 0.046(3) 0.063(4) 0.062(4) 0.025(3) 0.020(3) 0.009(3) C42 0.044(3) 0.053(3) 0.048(3) 0.012(3) 0.011(3) 0.008(3) C43 0.042(3) 0.043(3) 0.041(3) 0.014(2) 0.002(3) 0.005(2) C44 0.054(4) 0.060(4) 0.121(6) 0.006(4) 0.027(4) -0.011(3) C45 0.066(4) 0.075(4) 0.065(4) 0.003(3) 0.026(3) 0.006(3) C46 0.043(3) 0.048(3) 0.043(3) 0.014(3) 0.009(3) 0.006(3) C47 0.038(3) 0.054(3) 0.043(3) 0.012(3) 0.015(3) 0.004(3) C48 0.047(3) 0.047(3) 0.038(3) 0.011(2) 0.010(3) 0.005(3) C49 0.038(3) 0.047(3) 0.038(3) 0.011(2) 0.008(2) 0.003(2) C50 0.045(3) 0.048(3) 0.039(3) 0.008(3) 0.008(3) 0.003(3) C51 0.050(3) 0.060(4) 0.033(3) 0.011(3) 0.012(3) 0.018(3) C52 0.053(3) 0.061(4) 0.041(3) 0.014(3) 0.012(3) 0.011(3) C53 0.073(4) 0.067(4) 0.045(4) 0.025(3) 0.017(3) 0.028(3) C54 0.071(5) 0.094(5) 0.055(4) 0.023(4) 0.011(4) 0.050(4) C55 0.055(4) 0.100(5) 0.035(3) 0.008(3) 0.007(3) 0.025(4) C56 0.047(4) 0.075(4) 0.044(3) 0.011(3) 0.012(3) 0.010(3) C57 0.113(6) 0.096(5) 0.093(5) 0.051(4) 0.033(5) 0.031(5) C58 0.050(4) 0.176(8) 0.072(5) 0.023(5) 0.008(4) 0.043(4) C59 0.042(3) 0.050(3) 0.038(3) 0.016(3) 0.008(3) 0.006(3) C60 0.046(3) 0.047(3) 0.034(3) 0.007(2) 0.010(3) 0.002(2) C61 0.047(3) 0.057(4) 0.050(3) 0.003(3) 0.011(3) 0.005(3) C62 0.049(3) 0.078(5) 0.074(4) 0.012(3) 0.033(3) 0.010(3) C63 0.050(3) 0.060(4) 0.071(4) 0.017(3) 0.022(3) -0.002(3) C64 0.057(4) 0.056(4) 0.062(4) 0.018(3) 0.019(3) 0.012(3) C65 0.064(4) 0.074(4) 0.092(5) -0.011(4) 0.025(4) 0.010(3) C66 0.072(5) 0.090(5) 0.148(7) 0.043(5) 0.053(5) 0.011(4) C67 0.048(3) 0.044(3) 0.047(3) 0.018(3) 0.017(3) 0.009(2) C68 0.059(4) 0.044(3) 0.051(4) 0.013(3) 0.014(3) 0.003(3) C69 0.071(4) 0.055(4) 0.042(3) 0.016(3) 0.013(3) 0.007(3) C70 0.085(4) 0.060(4) 0.060(4) 0.033(3) 0.032(4) 0.022(3) C71 0.075(4) 0.051(4) 0.078(5) 0.028(3) 0.032(4) 0.013(3) C72 0.054(3) 0.059(4) 0.052(4) 0.009(3) 0.016(3) 0.012(3) C73 0.144(6) 0.075(4) 0.051(4) 0.025(3) 0.038(4) 0.010(4) C74 0.155(7) 0.066(5) 0.116(6) 0.033(4) 0.071(6) 0.031(5) C75 0.040(3) 0.050(3) 0.038(3) 0.011(3) 0.013(3) 0.004(2) C76 0.047(3) 0.049(3) 0.041(3) 0.012(3) 0.007(3) 0.004(3) C77 0.052(3) 0.048(3) 0.064(4) 0.016(3) 0.017(3) 0.013(3) C78 0.066(4) 0.045(3) 0.063(4) 0.016(3) 0.023(3) 0.020(3) C79 0.073(4) 0.048(3) 0.051(4) 0.008(3) 0.022(3) 0.011(3) C80 0.054(3) 0.051(3) 0.031(3) 0.005(3) 0.001(3) 0.004(3) C81 0.075(4) 0.094(5) 0.071(5) 0.029(4) 0.012(4) 0.035(4) C82 0.104(5) 0.090(5) 0.067(5) -0.017(4) 0.009(4) 0.021(4) C83 0.049(3) 0.046(3) 0.027(3) 0.008(2) 0.008(3) 0.010(2) C84 0.052(3) 0.048(3) 0.037(3) 0.011(2) 0.013(3) 0.008(3) C85 0.057(3) 0.059(4) 0.040(4) 0.009(3) 0.018(3) 0.008(3) C86 0.074(4) 0.062(4) 0.038(4) 0.006(3) 0.029(3) 0.001(3) C87 0.058(4) 0.058(3) 0.028(3) 0.008(2) 0.006(3) 0.002(3) C88 0.046(3) 0.057(3) 0.043(4) 0.007(3) 0.012(3) 0.001(3) C89 0.059(4) 0.091(5) 0.070(4) 0.005(3) 0.028(3) 0.004(3) C90 0.094(5) 0.098(5) 0.046(4) 0.021(3) 0.012(4) 0.003(4) C91 0.156(8) 0.190(10) 0.047(5) 0.008(6) 0.001(6) -0.127(7) C92 0.114(7) 0.249(13) 0.053(5) 0.025(7) -0.012(5) -0.104(8) C93 0.46(3) 0.073(8) 0.25(2) -0.041(10) -0.13(2) 0.082(13) C94 0.36(2) 0.065(8) 0.38(3) 0.056(12) -0.15(2) -0.058(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. The electron density of a disordered thf molecule was refined with the aid of PLATON/SQUEEZE (74 e/cell and 838 \%A^3^). ; 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 O1 C91 1.521(12) . ? O1 C94 1.67(2) . ? O1 Li2 1.80(2) . ? Li1 C5 2.397(5) . ? Li1 C5 2.397(5) 2 ? Li1 C4 2.403(5) 2 ? Li1 C4 2.403(5) . ? Li1 C3 2.431(5) . ? Li1 C3 2.431(5) 2 ? Li1 C2 2.438(5) . ? Li1 C2 2.438(5) 2 ? Li1 C1 2.444(5) 2 ? Li1 C1 2.444(5) . ? Li2 C47 2.421(5) 2_666 ? Li2 C47 2.421(5) . ? Li2 C46 2.427(5) 2_666 ? Li2 C46 2.427(5) . ? Li2 C50 2.452(5) 2_666 ? Li2 C50 2.452(5) . ? Li2 C48 2.453(5) 2_666 ? Li2 C48 2.453(5) . ? Li2 C49 2.461(5) 2_666 ? Li2 C49 2.461(5) . ? Li2 C1 2.18(2) . ? Li2 C5 2.21(2) . ? Li2 C2 2.231(18) . ? Li2 C4 2.27(2) . ? Li2 C3 2.283(19) . ? Li2 C94 2.52(3) . ? Li2' C93 1.99(2) . ? Li2' C94 2.23(2) . ? Li2' C49 2.227(17) . ? Li2' C50 2.244(18) . ? Li2' C48 2.279(17) . ? Li2' C46 2.289(19) . ? Li2' C47 2.316(19) . ? Li2' C92 2.74(2) . ? C1 C5 1.419(6) . ? C1 C2 1.432(6) . ? C1 C6 1.472(6) . ? C2 C3 1.432(6) . ? C2 C14 1.509(6) . ? C3 C4 1.433(6) . ? C3 C22 1.480(7) . ? C4 C5 1.432(6) . ? C4 C30 1.491(6) . ? C5 C38 1.485(6) . ? C6 C7 1.384(7) . ? C6 C11 1.400(7) . ? C7 C8 1.386(7) . ? C8 C9 1.409(7) . ? C8 C12 1.504(8) . ? C9 C10 1.380(7) . ? C10 C11 1.380(6) . ? C10 C13 1.501(7) . ? C14 C15 1.372(6) . ? C14 C19 1.382(6) . ? C15 C16 1.386(7) . ? C16 C17 1.396(7) . ? C16 C20 1.514(7) . ? C17 C18 1.378(7) . ? C18 C19 1.389(7) . ? C18 C21 1.511(7) . ? C22 C27 1.386(7) . ? C22 C23 1.384(7) . ? C23 C24 1.374(8) . ? C24 C25 1.368(9) . ? C24 C28 1.519(9) . ? C25 C26 1.402(9) . ? C26 C27 1.384(7) . ? C26 C29 1.497(8) . ? C30 C35 1.388(7) . ? C30 C31 1.395(7) . ? C31 C32 1.368(7) . ? C32 C33 1.409(7) . ? C32 C36 1.509(7) . ? C33 C34 1.359(7) . ? C34 C35 1.396(7) . ? C34 C37 1.528(8) . ? C38 C43 1.380(6) . ? C38 C39 1.400(6) . ? C39 C40 1.370(6) . ? C40 C41 1.401(7) . ? C40 C44 1.521(7) . ? C41 C42 1.374(7) . ? C42 C43 1.384(7) . ? C42 C45 1.513(7) . ? C46 C50 1.423(6) . ? C46 C47 1.435(7) . ? C46 C51 1.485(7) . ? C47 C48 1.427(7) . ? C47 C59 1.485(6) . ? C48 C49 1.431(6) . ? C48 C67 1.476(7) . ? C49 C50 1.432(7) . ? C49 C75 1.491(6) . ? C50 C83 1.483(7) . ? C51 C52 1.386(7) . ? C51 C56 1.403(7) . ? C52 C53 1.401(7) . ? C53 C54 1.395(8) . ? C53 C57 1.493(8) . ? C54 C55 1.402(9) . ? C55 C56 1.370(7) . ? C55 C58 1.497(8) . ? C59 C64 1.389(7) . ? C59 C60 1.398(7) . ? C60 C61 1.382(7) . ? C61 C62 1.372(7) . ? C61 C65 1.498(7) . ? C62 C63 1.383(8) . ? C63 C64 1.377(7) . ? C63 C66 1.484(8) . ? C67 C68 1.382(7) . ? C67 C72 1.396(7) . ? C68 C69 1.387(7) . ? C69 C70 1.380(7) . ? C69 C73 1.502(7) . ? C70 C71 1.373(8) . ? C71 C72 1.389(7) . ? C71 C74 1.504(8) . ? C75 C76 1.381(6) . ? C75 C80 1.401(6) . ? C76 C77 1.405(7) . ? C77 C78 1.377(7) . ? C77 C81 1.498(7) . ? C78 C79 1.381(7) . ? C79 C80 1.369(7) . ? C79 C82 1.509(8) . ? C83 C84 1.388(6) . ? C83 C88 1.389(7) . ? C84 C85 1.378(7) . ? C85 C86 1.395(7) . ? C85 C89 1.517(7) . ? C86 C87 1.379(7) . ? C87 C88 1.377(7) . ? C87 C90 1.499(7) . ? C91 C92 1.523(13) . ? C92 C93 1.388(15) . ? C93 C94 1.41(3) . ? 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 C91 O1 C94 117.8(9) . . ? C91 O1 Li2 122.4(8) . . ? C94 O1 Li2 92.7(10) . . ? C5 Li1 C5 180.0(3) . 2 ? C5 Li1 C4 145.28(15) . 2 ? C5 Li1 C4 34.72(15) 2 2 ? C5 Li1 C4 34.72(15) . . ? C5 Li1 C4 145.28(15) 2 . ? C4 Li1 C4 180.0(3) 2 . ? C5 Li1 C3 57.28(15) . . ? C5 Li1 C3 122.72(15) 2 . ? C4 Li1 C3 145.53(15) 2 . ? C4 Li1 C3 34.47(15) . . ? C5 Li1 C3 122.72(15) . 2 ? C5 Li1 C3 57.28(15) 2 2 ? C4 Li1 C3 34.47(15) 2 2 ? C4 Li1 C3 145.53(15) . 2 ? C3 Li1 C3 180.0(3) . 2 ? C5 Li1 C2 56.72(15) . . ? C5 Li1 C2 123.28(15) 2 . ? C4 Li1 C2 123.07(16) 2 . ? C4 Li1 C2 56.93(16) . . ? C3 Li1 C2 34.20(15) . . ? C3 Li1 C2 145.80(15) 2 . ? C5 Li1 C2 123.28(15) . 2 ? C5 Li1 C2 56.72(15) 2 2 ? C4 Li1 C2 56.93(16) 2 2 ? C4 Li1 C2 123.07(16) . 2 ? C3 Li1 C2 145.80(15) . 2 ? C3 Li1 C2 34.20(15) 2 2 ? C2 Li1 C2 180.0(2) . 2 ? C5 Li1 C1 145.94(15) . 2 ? C5 Li1 C1 34.06(15) 2 2 ? C4 Li1 C1 57.13(16) 2 2 ? C4 Li1 C1 122.87(16) . 2 ? C3 Li1 C1 122.98(16) . 2 ? C3 Li1 C1 57.02(16) 2 2 ? C2 Li1 C1 145.88(15) . 2 ? C2 Li1 C1 34.12(15) 2 2 ? C5 Li1 C1 34.06(15) . . ? C5 Li1 C1 145.94(15) 2 . ? C4 Li1 C1 122.87(16) 2 . ? C4 Li1 C1 57.13(16) . . ? C3 Li1 C1 57.02(16) . . ? C3 Li1 C1 122.98(16) 2 . ? C2 Li1 C1 34.12(15) . . ? C2 Li1 C1 145.88(15) 2 . ? C1 Li1 C1 180.0(3) 2 . ? C47 Li2 C47 180.0(3) 2_666 . ? C47 Li2 C46 34.42(16) 2_666 2_666 ? C47 Li2 C46 145.58(16) . 2_666 ? C47 Li2 C46 145.58(16) 2_666 . ? C47 Li2 C46 34.42(16) . . ? C46 Li2 C46 180.000(1) 2_666 . ? C47 Li2 C50 56.72(16) 2_666 2_666 ? C47 Li2 C50 123.28(16) . 2_666 ? C46 Li2 C50 33.90(15) 2_666 2_666 ? C46 Li2 C50 146.11(15) . 2_666 ? C47 Li2 C50 123.28(16) 2_666 . ? C47 Li2 C50 56.72(16) . . ? C46 Li2 C50 146.10(15) 2_666 . ? C46 Li2 C50 33.89(15) . . ? C50 Li2 C50 180.000(1) 2_666 . ? C47 Li2 C48 34.04(16) 2_666 2_666 ? C47 Li2 C48 145.96(16) . 2_666 ? C46 Li2 C48 56.72(16) 2_666 2_666 ? C46 Li2 C48 123.28(16) . 2_666 ? C50 Li2 C48 56.61(16) 2_666 2_666 ? C50 Li2 C48 123.39(16) . 2_666 ? C47 Li2 C48 145.96(16) 2_666 . ? C47 Li2 C48 34.04(16) . . ? C46 Li2 C48 123.28(16) 2_666 . ? C46 Li2 C48 56.72(16) . . ? C50 Li2 C48 123.39(16) 2_666 . ? C50 Li2 C48 56.61(16) . . ? C48 Li2 C48 180.000(1) 2_666 . ? C47 Li2 C49 56.28(15) 2_666 2_666 ? C47 Li2 C49 123.72(15) . 2_666 ? C46 Li2 C49 56.19(16) 2_666 2_666 ? C46 Li2 C49 123.81(16) . 2_666 ? C50 Li2 C49 33.89(15) 2_666 2_666 ? C50 Li2 C49 146.11(15) . 2_666 ? C48 Li2 C49 33.86(15) 2_666 2_666 ? C48 Li2 C49 146.14(15) . 2_666 ? C47 Li2 C49 123.72(15) 2_666 . ? C47 Li2 C49 56.28(15) . . ? C46 Li2 C49 123.81(16) 2_666 . ? C46 Li2 C49 56.19(16) . . ? C50 Li2 C49 146.11(15) 2_666 . ? C50 Li2 C49 33.89(15) . . ? C48 Li2 C49 146.14(15) 2_666 . ? C48 Li2 C49 33.86(15) . . ? C49 Li2 C49 180.00(12) 2_666 . ? O1 Li2 C1 143.1(11) . . ? O1 Li2 C5 147.9(11) . . ? C1 Li2 C5 37.7(4) . . ? O1 Li2 C2 144.2(11) . . ? C1 Li2 C2 37.9(4) . . ? C5 Li2 C2 62.3(5) . . ? O1 Li2 C4 151.1(11) . . ? C1 Li2 C4 62.8(6) . . ? C5 Li2 C4 37.3(4) . . ? C2 Li2 C4 61.7(5) . . ? O1 Li2 C3 148.5(11) . . ? C1 Li2 C3 62.8(5) . . ? C5 Li2 C3 62.0(5) . . ? C2 Li2 C3 37.0(3) . . ? C4 Li2 C3 36.7(3) . . ? O1 Li2 C94 41.5(6) . . ? C1 Li2 C94 167.5(11) . . ? C5 Li2 C94 149.0(10) . . ? C2 Li2 C94 130.0(10) . . ? C4 Li2 C94 117.1(9) . . ? C3 Li2 C94 109.1(9) . . ? C93 Li2' C94 38.4(8) . . ? C93 Li2' C49 156.3(10) . . ? C94 Li2' C49 152.6(11) . . ? C93 Li2' C50 164.8(11) . . ? C94 Li2' C50 126.8(9) . . ? C49 Li2' C50 37.4(3) . . ? C93 Li2' C48 132.5(11) . . ? C94 Li2' C48 170.1(11) . . ? C49 Li2' C48 37.0(3) . . ? C50 Li2' C48 61.9(5) . . ? C93 Li2' C46 139.6(10) . . ? C94 Li2' C46 122.1(8) . . ? C49 Li2' C46 61.3(5) . . ? C50 Li2' C46 36.6(3) . . ? C48 Li2' C46 61.0(5) . . ? C93 Li2' C47 126.0(11) . . ? C94 Li2' C47 140.2(10) . . ? C49 Li2' C47 60.9(5) . . ? C50 Li2' C47 61.0(5) . . ? C48 Li2' C47 36.2(3) . . ? C46 Li2' C47 36.3(3) . . ? C93 Li2' C92 28.8(5) . . ? C94 Li2' C92 59.5(6) . . ? C49 Li2' C92 127.5(8) . . ? C50 Li2' C92 160.7(9) . . ? C48 Li2' C92 114.1(7) . . ? C46 Li2' C92 160.8(9) . . ? C47 Li2' C92 128.3(8) . . ? C5 C1 C2 107.4(4) . . ? C5 C1 C6 125.6(4) . . ? C2 C1 C6 126.8(4) . . ? C5 C1 Li2 72.3(6) . . ? C2 C1 Li2 73.0(5) . . ? C6 C1 Li2 115.9(6) . . ? C5 C1 Li1 71.2(3) . . ? C2 C1 Li1 72.7(3) . . ? C6 C1 Li1 125.9(3) . . ? Li2 C1 Li1 118.1(5) . . ? C3 C2 C1 108.7(4) . . ? C3 C2 C14 124.9(4) . . ? C1 C2 C14 125.9(4) . . ? C3 C2 Li2 73.5(6) . . ? C1 C2 Li2 69.2(6) . . ? C14 C2 Li2 116.6(6) . . ? C3 C2 Li1 72.6(3) . . ? C1 C2 Li1 73.2(3) . . ? C14 C2 Li1 127.0(3) . . ? Li2 C2 Li1 116.4(6) . . ? C2 C3 C4 107.4(4) . . ? C2 C3 C22 126.2(4) . . ? C4 C3 C22 125.6(4) . . ? C2 C3 Li2 69.5(5) . . ? C4 C3 Li2 71.0(6) . . ? C22 C3 Li2 116.8(6) . . ? C2 C3 Li1 73.2(3) . . ? C4 C3 Li1 71.7(3) . . ? C22 C3 Li1 128.6(3) . . ? Li2 C3 Li1 114.7(5) . . ? C5 C4 C3 107.8(4) . . ? C5 C4 C30 125.7(4) . . ? C3 C4 C30 126.4(4) . . ? C5 C4 Li2 69.2(6) . . ? C3 C4 Li2 72.3(5) . . ? C30 C4 Li2 120.9(6) . . ? C5 C4 Li1 72.4(3) . . ? C3 C4 Li1 73.8(3) . . ? C30 C4 Li1 122.7(3) . . ? Li2 C4 Li1 116.4(5) . . ? C1 C5 C4 108.8(4) . . ? C1 C5 C38 124.3(4) . . ? C4 C5 C38 126.6(4) . . ? C1 C5 Li2 70.0(6) . . ? C4 C5 Li2 73.5(6) . . ? C38 C5 Li2 117.7(6) . . ? C1 C5 Li1 74.8(3) . . ? C4 C5 Li1 72.9(3) . . ? C38 C5 Li1 123.3(3) . . ? Li2 C5 Li1 118.9(5) . . ? C7 C6 C11 117.7(4) . . ? C7 C6 C1 122.3(4) . . ? C11 C6 C1 119.9(4) . . ? C6 C7 C8 121.8(5) . . ? C7 C8 C9 118.5(5) . . ? C7 C8 C12 121.2(5) . . ? C9 C8 C12 120.3(5) . . ? C10 C9 C8 121.1(5) . . ? C11 C10 C9 118.4(5) . . ? C11 C10 C13 121.7(5) . . ? C9 C10 C13 119.8(5) . . ? C10 C11 C6 122.4(5) . . ? C15 C14 C19 118.2(5) . . ? C15 C14 C2 121.4(4) . . ? C19 C14 C2 120.3(4) . . ? C14 C15 C16 122.7(5) . . ? C15 C16 C17 117.2(5) . . ? C15 C16 C20 122.0(5) . . ? C17 C16 C20 120.8(5) . . ? C18 C17 C16 122.0(5) . . ? C17 C18 C19 118.3(5) . . ? C17 C18 C21 120.7(5) . . ? C19 C18 C21 121.0(5) . . ? C14 C19 C18 121.7(5) . . ? C27 C22 C23 117.5(5) . . ? C27 C22 C3 121.2(5) . . ? C23 C22 C3 121.2(5) . . ? C24 C23 C22 121.5(6) . . ? C25 C24 C23 120.0(6) . . ? C25 C24 C28 121.0(6) . . ? C23 C24 C28 119.0(7) . . ? C24 C25 C26 120.9(5) . . ? C27 C26 C25 117.4(6) . . ? C27 C26 C29 121.6(6) . . ? C25 C26 C29 121.0(6) . . ? C22 C27 C26 122.7(5) . . ? C35 C30 C31 117.9(4) . . ? C35 C30 C4 121.4(4) . . ? C31 C30 C4 120.7(4) . . ? C32 C31 C30 122.5(5) . . ? C31 C32 C33 117.9(5) . . ? C31 C32 C36 120.3(5) . . ? C33 C32 C36 121.8(5) . . ? C34 C33 C32 121.1(5) . . ? C33 C34 C35 119.9(5) . . ? C33 C34 C37 121.2(5) . . ? C35 C34 C37 118.9(5) . . ? C30 C35 C34 120.6(5) . . ? C43 C38 C39 117.6(4) . . ? C43 C38 C5 120.8(4) . . ? C39 C38 C5 121.5(4) . . ? C40 C39 C38 122.0(5) . . ? C39 C40 C41 117.7(5) . . ? C39 C40 C44 120.5(5) . . ? C41 C40 C44 121.8(5) . . ? C42 C41 C40 122.4(5) . . ? C41 C42 C43 117.6(5) . . ? C41 C42 C45 122.2(5) . . ? C43 C42 C45 120.2(5) . . ? C38 C43 C42 122.6(5) . . ? C50 C46 C47 108.2(4) . . ? C50 C46 C51 125.7(4) . . ? C47 C46 C51 125.8(4) . . ? C50 C46 Li2' 70.0(5) . . ? C47 C46 Li2' 72.8(5) . . ? C51 C46 Li2' 118.6(5) . . ? C50 C46 Li2 74.0(3) . . ? C47 C46 Li2 72.6(3) . . ? C51 C46 Li2 123.7(3) . . ? Li2' C46 Li2 117.7(5) . . ? C48 C47 C46 108.2(4) . . ? C48 C47 C59 127.3(4) . . ? C46 C47 C59 124.2(4) . . ? C48 C47 Li2' 70.5(5) . . ? C46 C47 Li2' 70.9(5) . . ? C59 C47 Li2' 119.7(5) . . ? C48 C47 Li2 74.2(3) . . ? C46 C47 Li2 73.0(3) . . ? C59 C47 Li2 123.4(3) . . ? Li2' C47 Li2 116.9(5) . . ? C49 C48 C47 107.4(4) . . ? C49 C48 C67 128.5(4) . . ? C47 C48 C67 123.9(4) . . ? C49 C48 Li2' 69.5(5) . . ? C47 C48 Li2' 73.3(5) . . ? C67 C48 Li2' 118.5(6) . . ? C49 C48 Li2 73.4(3) . . ? C47 C48 Li2 71.8(3) . . ? C67 C48 Li2 124.5(3) . . ? Li2' C48 Li2 117.1(5) . . ? C48 C49 C50 108.7(4) . . ? C48 C49 C75 124.9(4) . . ? C50 C49 C75 125.6(4) . . ? C48 C49 Li2' 73.5(5) . . ? C50 C49 Li2' 72.0(5) . . ? C75 C49 Li2' 112.5(6) . . ? C48 C49 Li2 72.8(3) . . ? C50 C49 Li2 72.7(3) . . ? C75 C49 Li2 128.7(3) . . ? Li2' C49 Li2 118.8(5) . . ? C46 C50 C49 107.5(4) . . ? C46 C50 C83 127.1(4) . . ? C49 C50 C83 125.1(4) . . ? C46 C50 Li2' 73.5(6) . . ? C49 C50 Li2' 70.7(5) . . ? C83 C50 Li2' 116.7(6) . . ? C46 C50 Li2 72.1(3) . . ? C49 C50 Li2 73.4(3) . . ? C83 C50 Li2 124.8(3) . . ? Li2' C50 Li2 118.5(5) . . ? C52 C51 C56 118.5(5) . . ? C52 C51 C46 121.2(5) . . ? C56 C51 C46 120.3(5) . . ? C51 C52 C53 121.3(5) . . ? C54 C53 C52 117.7(5) . . ? C54 C53 C57 122.9(5) . . ? C52 C53 C57 119.5(6) . . ? C53 C54 C55 122.6(5) . . ? C56 C55 C54 117.3(5) . . ? C56 C55 C58 122.5(6) . . ? C54 C55 C58 120.2(6) . . ? C55 C56 C51 122.6(6) . . ? C64 C59 C60 117.8(5) . . ? C64 C59 C47 121.7(4) . . ? C60 C59 C47 120.4(4) . . ? C61 C60 C59 121.1(5) . . ? C62 C61 C60 118.6(5) . . ? C62 C61 C65 122.0(5) . . ? C60 C61 C65 119.3(5) . . ? C61 C62 C63 122.5(5) . . ? C64 C63 C62 117.6(5) . . ? C64 C63 C66 120.4(5) . . ? C62 C63 C66 122.0(5) . . ? C63 C64 C59 122.3(5) . . ? C68 C67 C72 116.5(5) . . ? C68 C67 C48 121.7(4) . . ? C72 C67 C48 121.6(5) . . ? C67 C68 C69 123.2(5) . . ? C70 C69 C68 117.5(5) . . ? C70 C69 C73 122.1(5) . . ? C68 C69 C73 120.4(5) . . ? C71 C70 C69 122.3(5) . . ? C70 C71 C72 118.2(5) . . ? C70 C71 C74 121.0(5) . . ? C72 C71 C74 120.8(6) . . ? C71 C72 C67 122.3(5) . . ? C76 C75 C80 116.8(4) . . ? C76 C75 C49 122.2(4) . . ? C80 C75 C49 120.9(4) . . ? C75 C76 C77 121.9(5) . . ? C78 C77 C76 118.6(5) . . ? C78 C77 C81 121.1(5) . . ? C76 C77 C81 120.3(5) . . ? C77 C78 C79 121.2(5) . . ? C80 C79 C78 118.8(5) . . ? C80 C79 C82 120.1(5) . . ? C78 C79 C82 121.0(5) . . ? C79 C80 C75 122.7(5) . . ? C84 C83 C88 117.3(4) . . ? C84 C83 C50 122.3(4) . . ? C88 C83 C50 120.4(4) . . ? C85 C84 C83 121.8(5) . . ? C84 C85 C86 118.7(5) . . ? C84 C85 C89 120.4(5) . . ? C86 C85 C89 120.9(5) . . ? C87 C86 C85 121.4(5) . . ? C88 C87 C86 117.9(5) . . ? C88 C87 C90 120.7(5) . . ? C86 C87 C90 121.4(5) . . ? C87 C88 C83 123.0(5) . . ? O1 C91 C92 96.7(9) . . ? C93 C92 C91 106.0(12) . . ? C93 C92 Li2' 43.6(9) . . ? C91 C92 Li2' 88.2(6) . . ? C92 C93 C94 127.7(19) . . ? C92 C93 Li2' 107.5(12) . . ? C94 C93 Li2' 80.4(14) . . ? C93 C94 O1 87.6(11) . . ? C93 C94 Li2' 61.2(11) . . ? O1 C94 Li2' 92.7(9) . . ? C93 C94 Li2 111.8(10) . . ? O1 C94 Li2 45.8(7) . . ? Li2' C94 Li2 138.2(11) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 22.46 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.817 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.052 data_ccd5831 _database_code_CSD 200151 _audit_creation_method SHELXL-97 _chemical_name_systematic ; penta(3,5-dimethylphenyl)cyclopentadiene ; _chemical_name_common penta(3,5-dimethylphenyl)cyclopentadiene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H46' _chemical_formula_weight 586.82 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1689(19) _cell_length_b 12.805(3) _cell_length_c 17.290(4) _cell_angle_alpha 92.202(4) _cell_angle_beta 93.823(5) _cell_angle_gamma 104.869(5) _cell_volume 1741.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.119 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.063 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9845 _exptl_absorpt_correction_T_max 0.9925 _exptl_absorpt_process_details ? _exptl_crystal_preparation ; crystallized from toluene ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8242 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 23.34 _reflns_number_total 4694 _reflns_number_gt 3732 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1350P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4694 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.2286 _refine_ls_wR_factor_gt 0.2181 _refine_ls_goodness_of_fit_ref 1.323 _refine_ls_restrained_S_all 1.323 _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 H1 H 0.284(5) 0.650(3) 0.203(2) 0.080 Uiso 1 1 d . . . C1 C 0.4006(4) 0.6719(2) 0.19693(16) 0.0329(7) Uani 1 1 d . . . C2 C 0.4974(4) 0.6165(2) 0.25165(16) 0.0346(7) Uani 1 1 d . . . C3 C 0.6088(4) 0.6925(2) 0.29853(16) 0.0347(7) Uani 1 1 d . . . C4 C 0.5870(4) 0.8001(2) 0.28166(16) 0.0355(7) Uani 1 1 d . . . C5 C 0.4670(4) 0.7897(2) 0.22334(17) 0.0358(7) Uani 1 1 d . . . C6 C 0.4314(4) 0.6533(2) 0.11263(16) 0.0329(7) Uani 1 1 d . . . C7 C 0.2990(4) 0.6188(2) 0.05611(16) 0.0339(7) Uani 1 1 d . . . H7 H 0.1877 0.6054 0.0699 0.041 Uiso 1 1 calc R . . C8 C 0.3291(4) 0.6035(2) -0.02124(17) 0.0366(8) Uani 1 1 d . . . C9 C 0.4947(4) 0.6237(2) -0.04016(17) 0.0373(8) Uani 1 1 d . . . H9 H 0.5161 0.6127 -0.0916 0.045 Uiso 1 1 calc R . . C10 C 0.6312(4) 0.6600(2) 0.01509(17) 0.0356(7) Uani 1 1 d . . . C11 C 0.5956(4) 0.6737(2) 0.09128(17) 0.0354(7) Uani 1 1 d . . . H11 H 0.6851 0.6973 0.1293 0.043 Uiso 1 1 calc R . . C12 C 0.1844(4) 0.5665(3) -0.08193(18) 0.0507(9) Uani 1 1 d . . . H12A H 0.0790 0.5556 -0.0580 0.076 Uiso 1 1 calc R . . H12B H 0.1906 0.4998 -0.1073 0.076 Uiso 1 1 calc R . . H12C H 0.1906 0.6205 -0.1194 0.076 Uiso 1 1 calc R . . C13 C 0.8089(4) 0.6825(3) -0.0077(2) 0.0501(9) Uani 1 1 d . . . H13A H 0.8077 0.6677 -0.0626 0.075 Uiso 1 1 calc R . . H13B H 0.8675 0.6371 0.0195 0.075 Uiso 1 1 calc R . . H13C H 0.8661 0.7571 0.0053 0.075 Uiso 1 1 calc R . . C14 C 0.4692(4) 0.4982(2) 0.24950(16) 0.0356(7) Uani 1 1 d . . . C15 C 0.3094(4) 0.4297(2) 0.22846(17) 0.0378(8) Uani 1 1 d . . . H15 H 0.2198 0.4595 0.2147 0.045 Uiso 1 1 calc R . . C16 C 0.2800(4) 0.3182(2) 0.22737(17) 0.0398(8) Uani 1 1 d . . . C17 C 0.4165(4) 0.2756(3) 0.24545(18) 0.0456(9) Uani 1 1 d . . . H17 H 0.3989 0.2008 0.2442 0.055 Uiso 1 1 calc R . . C18 C 0.5779(4) 0.3407(3) 0.26524(18) 0.0438(8) Uani 1 1 d . . . C19 C 0.6004(4) 0.4511(3) 0.26669(17) 0.0411(8) Uani 1 1 d . . . H19 H 0.7086 0.4959 0.2798 0.049 Uiso 1 1 calc R . . C20 C 0.1067(4) 0.2457(3) 0.2094(2) 0.0554(10) Uani 1 1 d . . . H20A H 0.1111 0.1717 0.2120 0.083 Uiso 1 1 calc R . . H20B H 0.0646 0.2573 0.1581 0.083 Uiso 1 1 calc R . . H20C H 0.0325 0.2612 0.2465 0.083 Uiso 1 1 calc R . . C21 C 0.7245(5) 0.2936(3) 0.2839(2) 0.0651(11) Uani 1 1 d . . . H21A H 0.6859 0.2161 0.2798 0.098 Uiso 1 1 calc R . . H21B H 0.7724 0.3173 0.3358 0.098 Uiso 1 1 calc R . . H21C H 0.8094 0.3172 0.2479 0.098 Uiso 1 1 calc R . . C22 C 0.7283(4) 0.6747(2) 0.36186(17) 0.0372(8) Uani 1 1 d . . . C23 C 0.8933(4) 0.6730(2) 0.34789(18) 0.0412(8) Uani 1 1 d . . . H23 H 0.9294 0.6851 0.2984 0.049 Uiso 1 1 calc R . . C24 C 1.0041(4) 0.6538(3) 0.40533(19) 0.0450(8) Uani 1 1 d . . . C25 C 0.9494(5) 0.6368(3) 0.47839(19) 0.0480(9) Uani 1 1 d . . . H25 H 1.0233 0.6226 0.5175 0.058 Uiso 1 1 calc R . . C26 C 0.7879(4) 0.6401(3) 0.49549(18) 0.0458(8) Uani 1 1 d . . . C27 C 0.6791(4) 0.6595(2) 0.43573(17) 0.0406(8) Uani 1 1 d . . . H27 H 0.5700 0.6622 0.4461 0.049 Uiso 1 1 calc R . . C28 C 1.1825(5) 0.6510(4) 0.3877(2) 0.0715(12) Uani 1 1 d . . . H28A H 1.2430 0.6371 0.4340 0.107 Uiso 1 1 calc R . . H28B H 1.2407 0.7195 0.3695 0.107 Uiso 1 1 calc R . . H28C H 1.1765 0.5948 0.3485 0.107 Uiso 1 1 calc R . . C29 C 0.7294(6) 0.6245(4) 0.5753(2) 0.0753(12) Uani 1 1 d . . . H29A H 0.6140 0.6293 0.5752 0.113 Uiso 1 1 calc R . . H29B H 0.8006 0.6796 0.6109 0.113 Uiso 1 1 calc R . . H29C H 0.7360 0.5546 0.5912 0.113 Uiso 1 1 calc R . . C30 C 0.6835(4) 0.9010(2) 0.32631(17) 0.0388(8) Uani 1 1 d . . . C31 C 0.8580(4) 0.9286(3) 0.33491(19) 0.0464(9) Uani 1 1 d . . . H31 H 0.9159 0.8846 0.3104 0.056 Uiso 1 1 calc R . . C32 C 0.9503(4) 1.0200(3) 0.3790(2) 0.0529(9) Uani 1 1 d . . . C33 C 0.8606(5) 1.0837(3) 0.4138(2) 0.0546(10) Uani 1 1 d . . . H33 H 0.9204 1.1454 0.4435 0.066 Uiso 1 1 calc R . . C34 C 0.6856(4) 1.0597(3) 0.40638(19) 0.0486(9) Uani 1 1 d . . . C35 C 0.5990(4) 0.9677(3) 0.36202(18) 0.0426(8) Uani 1 1 d . . . H35 H 0.4810 0.9503 0.3560 0.051 Uiso 1 1 calc R . . C36 C 1.1406(5) 1.0470(3) 0.3892(3) 0.0778(13) Uani 1 1 d . . . H36A H 1.1826 1.1133 0.4205 0.117 Uiso 1 1 calc R . . H36B H 1.1858 1.0554 0.3393 0.117 Uiso 1 1 calc R . . H36C H 1.1751 0.9896 0.4142 0.117 Uiso 1 1 calc R . . C37 C 0.5927(5) 1.1299(3) 0.4466(2) 0.0695(12) Uani 1 1 d . . . H37A H 0.6731 1.1902 0.4738 0.104 Uiso 1 1 calc R . . H37B H 0.5220 1.0885 0.4827 0.104 Uiso 1 1 calc R . . H37C H 0.5232 1.1558 0.4088 0.104 Uiso 1 1 calc R . . C38 C 0.4107(4) 0.8750(2) 0.18293(17) 0.0372(8) Uani 1 1 d . . . C39 C 0.5295(4) 0.9599(2) 0.15479(18) 0.0420(8) Uani 1 1 d . . . H39 H 0.6443 0.9641 0.1648 0.050 Uiso 1 1 calc R . . C40 C 0.4830(4) 1.0376(2) 0.11272(19) 0.0458(9) Uani 1 1 d . . . C41 C 0.3118(5) 1.0317(3) 0.1010(2) 0.0522(9) Uani 1 1 d . . . H41 H 0.2786 1.0848 0.0735 0.063 Uiso 1 1 calc R . . C42 C 0.1880(4) 0.9499(3) 0.1288(2) 0.0478(9) Uani 1 1 d . . . C43 C 0.2409(4) 0.8716(2) 0.16926(18) 0.0418(8) Uani 1 1 d . . . H43 H 0.1597 0.8151 0.1878 0.050 Uiso 1 1 calc R . . C44 C 0.6133(5) 1.1268(3) 0.0807(3) 0.0671(11) Uani 1 1 d . . . H44A H 0.7248 1.1180 0.0942 0.101 Uiso 1 1 calc R . . H44B H 0.6053 1.1953 0.1022 0.101 Uiso 1 1 calc R . . H44C H 0.5935 1.1241 0.0252 0.101 Uiso 1 1 calc R . . C45 C 0.0037(5) 0.9461(3) 0.1166(3) 0.0676(11) Uani 1 1 d . . . H45A H -0.0090 1.0075 0.0890 0.101 Uiso 1 1 calc R . . H45B H -0.0430 0.9477 0.1660 0.101 Uiso 1 1 calc R . . H45C H -0.0552 0.8808 0.0870 0.101 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 C1 0.0362(18) 0.0335(17) 0.0288(15) -0.0009(12) 0.0060(13) 0.0081(14) C2 0.0394(18) 0.0360(17) 0.0283(15) -0.0024(13) 0.0086(13) 0.0089(14) C3 0.0380(18) 0.0375(17) 0.0294(16) 0.0003(13) 0.0069(13) 0.0104(14) C4 0.0381(18) 0.0369(17) 0.0308(16) -0.0037(13) 0.0054(14) 0.0088(14) C5 0.0378(18) 0.0327(17) 0.0370(17) -0.0029(13) 0.0070(14) 0.0090(14) C6 0.0374(19) 0.0249(15) 0.0359(17) 0.0010(12) 0.0059(14) 0.0066(13) C7 0.0322(17) 0.0312(16) 0.0368(17) 0.0030(13) 0.0049(13) 0.0050(13) C8 0.044(2) 0.0296(16) 0.0346(17) -0.0015(13) 0.0010(14) 0.0073(14) C9 0.050(2) 0.0315(16) 0.0316(16) 0.0017(13) 0.0105(15) 0.0114(15) C10 0.0383(19) 0.0302(16) 0.0389(17) 0.0027(13) 0.0061(14) 0.0091(14) C11 0.038(2) 0.0306(16) 0.0357(17) -0.0023(12) 0.0019(14) 0.0065(13) C12 0.052(2) 0.057(2) 0.0375(19) -0.0020(15) -0.0031(15) 0.0063(17) C13 0.046(2) 0.052(2) 0.054(2) 0.0003(16) 0.0158(16) 0.0122(17) C14 0.046(2) 0.0380(17) 0.0234(15) 0.0008(12) 0.0072(13) 0.0116(15) C15 0.046(2) 0.0371(18) 0.0318(16) -0.0016(13) 0.0087(14) 0.0129(15) C16 0.050(2) 0.0326(17) 0.0357(17) -0.0012(13) 0.0144(14) 0.0073(15) C17 0.066(2) 0.0317(17) 0.0404(18) 0.0008(14) 0.0151(16) 0.0122(17) C18 0.059(2) 0.0395(19) 0.0380(18) 0.0036(14) 0.0100(15) 0.0198(17) C19 0.049(2) 0.0409(19) 0.0338(17) 0.0000(14) 0.0062(14) 0.0119(15) C20 0.062(2) 0.041(2) 0.059(2) -0.0060(16) 0.0102(18) 0.0057(18) C21 0.075(3) 0.056(2) 0.074(3) 0.0105(19) 0.009(2) 0.031(2) C22 0.0435(19) 0.0309(16) 0.0367(17) -0.0031(13) 0.0050(14) 0.0091(14) C23 0.044(2) 0.0439(19) 0.0348(17) -0.0025(14) 0.0048(14) 0.0101(15) C24 0.044(2) 0.047(2) 0.043(2) -0.0101(15) -0.0054(15) 0.0142(16) C25 0.060(2) 0.0409(19) 0.0412(19) -0.0055(14) -0.0099(16) 0.0140(16) C26 0.060(2) 0.0398(19) 0.0364(18) 0.0012(14) 0.0034(16) 0.0112(16) C27 0.0452(19) 0.0417(18) 0.0352(18) -0.0004(14) 0.0059(14) 0.0113(15) C28 0.048(2) 0.096(3) 0.072(3) -0.012(2) -0.0013(19) 0.025(2) C29 0.102(3) 0.090(3) 0.039(2) 0.011(2) 0.014(2) 0.032(3) C30 0.044(2) 0.0350(17) 0.0343(17) -0.0013(13) 0.0005(14) 0.0059(15) C31 0.047(2) 0.0367(19) 0.054(2) 0.0018(15) 0.0018(16) 0.0078(16) C32 0.044(2) 0.041(2) 0.067(2) 0.0073(17) -0.0023(17) 0.0015(17) C33 0.060(3) 0.0378(19) 0.054(2) -0.0065(16) -0.0075(18) -0.0045(17) C34 0.057(2) 0.0369(19) 0.046(2) -0.0058(15) 0.0052(16) 0.0019(16) C35 0.0428(19) 0.0404(18) 0.0407(18) -0.0056(14) 0.0019(14) 0.0054(15) C36 0.054(3) 0.063(3) 0.105(4) 0.004(2) -0.010(2) -0.001(2) C37 0.075(3) 0.054(2) 0.074(3) -0.022(2) 0.014(2) 0.007(2) C38 0.043(2) 0.0328(17) 0.0360(17) -0.0064(13) 0.0019(14) 0.0108(14) C39 0.043(2) 0.0376(18) 0.0449(19) -0.0061(14) 0.0022(15) 0.0117(15) C40 0.058(2) 0.0323(18) 0.047(2) -0.0025(14) 0.0035(16) 0.0128(16) C41 0.069(3) 0.038(2) 0.052(2) -0.0058(16) -0.0094(18) 0.0225(19) C42 0.052(2) 0.0356(19) 0.054(2) -0.0118(16) -0.0092(17) 0.0150(17) C43 0.044(2) 0.0352(18) 0.0445(19) -0.0065(14) -0.0002(15) 0.0101(15) C44 0.077(3) 0.047(2) 0.078(3) 0.0143(19) 0.011(2) 0.014(2) C45 0.056(2) 0.061(2) 0.087(3) -0.005(2) -0.014(2) 0.023(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.504(4) . ? C1 C5 1.508(4) . ? C1 C6 1.516(4) . ? C2 C3 1.348(4) . ? C2 C14 1.472(4) . ? C3 C4 1.471(4) . ? C3 C22 1.481(4) . ? C4 C5 1.337(4) . ? C4 C30 1.485(4) . ? C5 C38 1.472(4) . ? C6 C11 1.377(4) . ? C6 C7 1.379(4) . ? C7 C8 1.391(4) . ? C8 C9 1.375(4) . ? C8 C12 1.494(4) . ? C9 C10 1.389(4) . ? C10 C11 1.382(4) . ? C10 C13 1.489(4) . ? C14 C19 1.379(4) . ? C14 C15 1.389(4) . ? C15 C16 1.384(4) . ? C16 C17 1.385(5) . ? C16 C20 1.486(5) . ? C17 C18 1.380(5) . ? C18 C19 1.377(4) . ? C18 C21 1.496(5) . ? C22 C27 1.370(4) . ? C22 C23 1.391(4) . ? C23 C24 1.370(5) . ? C24 C25 1.374(5) . ? C24 C28 1.517(5) . ? C25 C26 1.382(5) . ? C26 C27 1.389(5) . ? C26 C29 1.495(5) . ? C30 C31 1.374(4) . ? C30 C35 1.381(4) . ? C31 C32 1.386(5) . ? C32 C33 1.375(5) . ? C32 C36 1.500(5) . ? C33 C34 1.378(5) . ? C34 C35 1.381(4) . ? C34 C37 1.496(5) . ? C38 C43 1.381(4) . ? C38 C39 1.386(4) . ? C39 C40 1.370(4) . ? C40 C41 1.382(5) . ? C40 C44 1.499(5) . ? C41 C42 1.382(5) . ? C42 C43 1.384(5) . ? C42 C45 1.494(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 103.2(2) . . ? C2 C1 C6 112.9(2) . . ? C5 C1 C6 111.0(2) . . ? C3 C2 C14 128.6(3) . . ? C3 C2 C1 108.7(3) . . ? C14 C2 C1 122.6(3) . . ? C2 C3 C4 109.4(3) . . ? C2 C3 C22 127.3(3) . . ? C4 C3 C22 123.1(3) . . ? C5 C4 C3 109.2(3) . . ? C5 C4 C30 127.7(3) . . ? C3 C4 C30 123.1(3) . . ? C4 C5 C38 128.8(3) . . ? C4 C5 C1 109.3(3) . . ? C38 C5 C1 121.7(3) . . ? C11 C6 C7 118.9(3) . . ? C11 C6 C1 119.5(3) . . ? C7 C6 C1 121.7(3) . . ? C6 C7 C8 121.1(3) . . ? C9 C8 C7 118.4(3) . . ? C9 C8 C12 121.1(3) . . ? C7 C8 C12 120.5(3) . . ? C8 C9 C10 122.1(3) . . ? C9 C10 C11 117.7(3) . . ? C9 C10 C13 120.6(3) . . ? C11 C10 C13 121.7(3) . . ? C6 C11 C10 121.9(3) . . ? C19 C14 C15 117.5(3) . . ? C19 C14 C2 121.5(3) . . ? C15 C14 C2 121.0(3) . . ? C16 C15 C14 121.8(3) . . ? C17 C16 C15 118.1(3) . . ? C17 C16 C20 120.5(3) . . ? C15 C16 C20 121.4(3) . . ? C16 C17 C18 122.0(3) . . ? C19 C18 C17 117.8(3) . . ? C19 C18 C21 120.8(3) . . ? C17 C18 C21 121.4(3) . . ? C18 C19 C14 122.8(3) . . ? C27 C22 C23 118.3(3) . . ? C27 C22 C3 120.9(3) . . ? C23 C22 C3 120.9(3) . . ? C24 C23 C22 121.6(3) . . ? C23 C24 C25 118.5(3) . . ? C23 C24 C28 120.2(3) . . ? C25 C24 C28 121.3(3) . . ? C24 C25 C26 121.9(3) . . ? C25 C26 C27 117.9(3) . . ? C25 C26 C29 122.1(3) . . ? C27 C26 C29 120.0(3) . . ? C22 C27 C26 121.7(3) . . ? C31 C30 C35 118.5(3) . . ? C31 C30 C4 121.0(3) . . ? C35 C30 C4 120.5(3) . . ? C30 C31 C32 121.9(3) . . ? C33 C32 C31 117.5(3) . . ? C33 C32 C36 121.5(3) . . ? C31 C32 C36 121.0(3) . . ? C34 C33 C32 122.7(3) . . ? C33 C34 C35 117.8(3) . . ? C33 C34 C37 121.0(3) . . ? C35 C34 C37 121.1(3) . . ? C30 C35 C34 121.6(3) . . ? C43 C38 C39 118.1(3) . . ? C43 C38 C5 122.0(3) . . ? C39 C38 C5 119.9(3) . . ? C40 C39 C38 122.1(3) . . ? C41 C40 C39 117.9(3) . . ? C41 C40 C44 120.9(3) . . ? C39 C40 C44 121.3(3) . . ? C40 C41 C42 122.4(3) . . ? C43 C42 C41 117.6(3) . . ? C43 C42 C45 120.9(3) . . ? C41 C42 C45 121.5(3) . . ? C38 C43 C42 121.8(3) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 23.34 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 0.370 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.050