# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl #TrackingRef 'C52H74Li N2O6Y.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H74 Li N2 O6 Y' _chemical_formula_sum 'C52 H74 Li N2 O6 Y' _chemical_formula_weight 918.98 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' Y Y -2.7962 3.5667 '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 monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 27.718(3) _cell_length_b 9.8144(10) _cell_length_c 20.410(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.217(2) _cell_angle_gamma 90.00 _cell_volume 5063.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10151 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 1.199 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.503 _exptl_absorpt_correction_T_max 0.698 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12693 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4689 _reflns_number_gt 3899 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^)+(0.1053P)^2^+5.0040P] 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 SHELXL _refine_ls_extinction_coef 0.0037(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4689 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1789 _refine_ls_wR_factor_gt 0.1688 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 Y1 Y 0.5000 0.39173(5) 0.7500 0.0446(2) Uani 1 2 d S . . O1 O 0.54596(10) 0.5629(3) 0.81525(13) 0.0499(6) Uani 1 1 d . . . O2 O 0.42723(10) 0.2345(3) 0.72340(14) 0.0497(6) Uani 1 1 d . . . O3 O 0.48200(14) 0.8320(4) 0.8092(2) 0.0859(11) Uani 1 1 d . . . N1 N 0.47912(12) 0.3565(3) 0.84589(16) 0.0480(7) Uani 1 1 d . . . C1 C 0.58176(14) 0.5255(4) 0.88184(18) 0.0457(8) Uani 1 1 d . . . C2 C 0.63731(14) 0.5456(4) 0.90439(19) 0.0462(8) Uani 1 1 d . . . C3 C 0.67083(14) 0.4946(4) 0.9713(2) 0.0482(9) Uani 1 1 d . . . H3 H 0.7074 0.5071 0.9861 0.058 Uiso 1 1 calc R . . C4 C 0.65390(15) 0.4261(4) 1.0179(2) 0.0485(9) Uani 1 1 d . . . C5 C 0.59976(15) 0.4116(4) 0.9950(2) 0.0493(9) Uani 1 1 d . . . H5 H 0.5868 0.3667 1.0252 0.059 Uiso 1 1 calc R . . C6 C 0.56364(14) 0.4610(4) 0.92885(19) 0.0478(9) Uani 1 1 d . . . C7 C 0.50536(15) 0.4385(5) 0.9102(2) 0.0574(10) Uani 1 1 d . . . H7A H 0.5016 0.3935 0.9506 0.069 Uiso 1 1 calc R . . H7B H 0.4877 0.5272 0.9031 0.069 Uiso 1 1 calc R . . C8 C 0.43478(14) 0.2865(4) 0.8403(2) 0.0483(9) Uani 1 1 d . . . C9 C 0.40649(14) 0.2151(4) 0.7756(2) 0.0474(8) Uani 1 1 d . . . C10 C 0.36289(16) 0.1353(4) 0.7641(3) 0.0601(11) Uani 1 1 d . . . H10 H 0.3459 0.0884 0.7204 0.072 Uiso 1 1 calc R . . C11 C 0.34412(19) 0.1245(5) 0.8177(3) 0.0712(13) Uani 1 1 d . . . H11 H 0.3148 0.0692 0.8111 0.085 Uiso 1 1 calc R . . C12 C 0.36943(17) 0.1968(5) 0.8806(3) 0.0710(13) Uani 1 1 d . . . H12 H 0.3566 0.1912 0.9166 0.085 Uiso 1 1 calc R . . C13 C 0.41320(16) 0.2773(5) 0.8922(2) 0.0620(11) Uani 1 1 d . . . H13 H 0.4289 0.3267 0.9353 0.074 Uiso 1 1 calc R . . C14 C 0.39480(17) 0.1891(4) 0.6514(2) 0.0613(11) Uani 1 1 d . . . H14A H 0.3890 0.0917 0.6517 0.092 Uiso 1 1 calc R . . H14B H 0.4126 0.2091 0.6203 0.092 Uiso 1 1 calc R . . H14C H 0.3610 0.2360 0.6338 0.092 Uiso 1 1 calc R . . C15 C 0.66005(17) 0.6192(4) 0.8567(2) 0.0543(10) Uani 1 1 d . . . C16 C 0.72157(18) 0.6282(5) 0.8935(3) 0.0680(12) Uani 1 1 d . . . H16A H 0.7364 0.5370 0.9021 0.102 Uiso 1 1 calc R . . H16B H 0.7323 0.6762 0.9388 0.102 Uiso 1 1 calc R . . H16C H 0.7343 0.6770 0.8624 0.102 Uiso 1 1 calc R . . C17 C 0.6398(2) 0.7661(5) 0.8437(3) 0.0810(15) Uani 1 1 d . . . H17A H 0.6560 0.8141 0.8164 0.121 Uiso 1 1 calc R . . H17B H 0.6488 0.8113 0.8895 0.121 Uiso 1 1 calc R . . H17C H 0.6017 0.7659 0.8170 0.121 Uiso 1 1 calc R . . C18 C 0.6463(2) 0.5435(5) 0.7866(2) 0.0708(13) Uani 1 1 d . . . H18A H 0.6082 0.5358 0.7615 0.106 Uiso 1 1 calc R . . H18B H 0.6619 0.4531 0.7965 0.106 Uiso 1 1 calc R . . H18C H 0.6601 0.5931 0.7569 0.106 Uiso 1 1 calc R . . C19 C 0.69386(15) 0.3729(4) 1.0908(2) 0.0525(10) Uani 1 1 d . . . C20 C 0.7383(2) 0.2942(7) 1.0827(3) 0.0933(19) Uani 1 1 d . . . H20A H 0.7235 0.2193 1.0494 0.140 Uiso 1 1 calc R . . H20B H 0.7621 0.2586 1.1290 0.140 Uiso 1 1 calc R . . H20C H 0.7576 0.3544 1.0643 0.140 Uiso 1 1 calc R . . C21 C 0.6676(2) 0.2817(7) 1.1273(3) 0.0954(19) Uani 1 1 d . . . H21A H 0.6408 0.3332 1.1357 0.143 Uiso 1 1 calc R . . H21B H 0.6941 0.2495 1.1727 0.143 Uiso 1 1 calc R . . H21C H 0.6513 0.2044 1.0965 0.143 Uiso 1 1 calc R . . C22 C 0.7178(3) 0.4940(7) 1.1407(3) 0.0985(11) Uani 1 1 d . . . H22A H 0.7364 0.5521 1.1203 0.148 Uiso 1 1 calc R . . H22B H 0.7424 0.4611 1.1873 0.148 Uiso 1 1 calc R . . H22C H 0.6898 0.5455 1.1462 0.148 Uiso 1 1 calc R . . C23 C 0.4479(3) 0.8167(7) 0.8439(3) 0.0985(11) Uani 1 1 d . . . H23A H 0.4415 0.7199 0.8491 0.118 Uiso 1 1 calc R . . H23B H 0.4139 0.8610 0.8161 0.118 Uiso 1 1 calc R . . C24 C 0.4744(3) 0.8820(7) 0.9163(3) 0.0985(11) Uani 1 1 d . . . H24A H 0.4510 0.9492 0.9239 0.118 Uiso 1 1 calc R . . H24B H 0.4844 0.8135 0.9546 0.118 Uiso 1 1 calc R . . C25 C 0.5220(3) 0.9488(11) 0.9147(4) 0.140(3) Uani 1 1 d . . . H25A H 0.5540 0.8963 0.9425 0.168 Uiso 1 1 calc R . . H25B H 0.5262 1.0413 0.9343 0.168 Uiso 1 1 calc R . . C26 C 0.5116(3) 0.9516(8) 0.8356(4) 0.116(2) Uani 1 1 d . . . H26A H 0.4914 1.0327 0.8118 0.139 Uiso 1 1 calc R . . H26B H 0.5448 0.9495 0.8292 0.139 Uiso 1 1 calc R . . Li1 Li 0.5000 0.7027(9) 0.7500 0.050(2) Uani 1 2 d S . . 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 Y1 0.0446(3) 0.0449(3) 0.0401(3) 0.000 0.0130(2) 0.000 O1 0.0495(14) 0.0515(14) 0.0360(13) 0.0011(11) 0.0046(11) -0.0024(12) O2 0.0470(13) 0.0502(14) 0.0474(15) -0.0052(12) 0.0148(12) -0.0043(11) O3 0.086(2) 0.082(2) 0.116(3) -0.048(2) 0.068(2) -0.030(2) N1 0.0388(15) 0.0606(19) 0.0404(17) -0.0005(14) 0.0122(13) -0.0023(14) C1 0.0478(19) 0.0447(19) 0.0347(18) -0.0048(15) 0.0069(16) -0.0030(16) C2 0.049(2) 0.0431(19) 0.041(2) -0.0021(15) 0.0128(16) -0.0057(16) C3 0.0430(18) 0.053(2) 0.043(2) -0.0007(17) 0.0112(16) -0.0034(16) C4 0.0469(19) 0.055(2) 0.039(2) -0.0005(16) 0.0128(16) 0.0030(17) C5 0.050(2) 0.061(2) 0.0352(19) -0.0007(16) 0.0161(16) -0.0006(17) C6 0.0436(19) 0.055(2) 0.041(2) -0.0082(17) 0.0136(16) -0.0033(17) C7 0.046(2) 0.077(3) 0.046(2) -0.005(2) 0.0162(18) 0.002(2) C8 0.0430(18) 0.050(2) 0.049(2) 0.0073(17) 0.0159(16) 0.0067(16) C9 0.0427(18) 0.0459(19) 0.050(2) 0.0059(16) 0.0155(16) 0.0035(16) C10 0.049(2) 0.057(2) 0.068(3) 0.003(2) 0.017(2) -0.0047(19) C11 0.055(2) 0.083(3) 0.076(3) 0.013(3) 0.027(2) -0.011(2) C12 0.051(2) 0.096(4) 0.071(3) 0.018(3) 0.030(2) 0.004(2) C13 0.052(2) 0.078(3) 0.054(2) 0.008(2) 0.0199(19) 0.003(2) C14 0.064(2) 0.058(2) 0.058(3) -0.012(2) 0.021(2) -0.012(2) C15 0.057(2) 0.050(2) 0.048(2) 0.0052(17) 0.0141(19) -0.0116(18) C16 0.056(2) 0.076(3) 0.066(3) 0.012(2) 0.019(2) -0.013(2) C17 0.077(3) 0.057(3) 0.089(4) 0.016(3) 0.013(3) -0.009(2) C18 0.083(3) 0.084(3) 0.051(3) 0.002(2) 0.032(2) -0.025(3) C19 0.046(2) 0.069(3) 0.038(2) 0.0082(17) 0.0134(16) 0.0094(18) C20 0.093(4) 0.128(5) 0.062(3) 0.027(3) 0.034(3) 0.051(4) C21 0.082(3) 0.133(5) 0.056(3) 0.034(3) 0.014(3) -0.004(3) C22 0.109(3) 0.108(3) 0.066(2) -0.0121(18) 0.0238(19) -0.013(2) C23 0.109(3) 0.108(3) 0.066(2) -0.0121(18) 0.0238(19) -0.013(2) C24 0.109(3) 0.108(3) 0.066(2) -0.0121(18) 0.0238(19) -0.013(2) C25 0.122(6) 0.187(8) 0.081(5) -0.024(5) 0.011(4) -0.046(6) C26 0.103(4) 0.127(6) 0.138(6) -0.052(5) 0.069(5) -0.038(4) Li1 0.049(5) 0.052(5) 0.048(5) 0.000 0.017(4) 0.000 _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 Y1 O1 2.197(3) . ? Y1 O1 2.197(3) 2_656 ? Y1 N1 2.283(3) 2_656 ? Y1 N1 2.283(3) . ? Y1 O2 2.418(2) . ? Y1 O2 2.418(2) 2_656 ? Y1 C1 3.016(3) . ? Y1 C1 3.016(3) 2_656 ? Y1 Li1 3.052(9) . ? O1 C1 1.364(4) . ? O1 Li1 1.972(7) . ? O2 C9 1.416(5) . ? O2 C14 1.443(5) . ? O3 C23 1.403(7) . ? O3 C26 1.408(7) . ? O3 Li1 1.952(7) . ? N1 C8 1.372(5) . ? N1 C7 1.454(5) . ? C1 C6 1.403(5) . ? C1 C2 1.428(5) . ? C2 C3 1.393(5) . ? C2 C15 1.539(5) . ? C3 C4 1.393(5) . ? C3 H3 0.9400 . ? C4 C5 1.384(5) . ? C4 C19 1.537(5) . ? C5 C6 1.397(5) . ? C5 H5 0.9400 . ? C6 C7 1.516(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.414(5) . ? C8 C13 1.416(6) . ? C9 C10 1.377(6) . ? C10 C11 1.395(7) . ? C10 H10 0.9400 . ? C11 C12 1.380(7) . ? C11 H11 0.9400 . ? C12 C13 1.384(6) . ? C12 H12 0.9400 . ? C13 H13 0.9400 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 C18 1.516(6) . ? C15 C17 1.530(6) . ? C15 C16 1.558(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C20 1.520(6) . ? C19 C21 1.525(6) . ? C19 C22 1.528(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 C24 1.497(8) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.487(10) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.520(10) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? Li1 O3 1.952(7) 2_656 ? Li1 O1 1.972(7) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Y1 O1 80.25(13) . 2_656 ? O1 Y1 N1 110.33(11) . 2_656 ? O1 Y1 N1 83.33(11) 2_656 2_656 ? O1 Y1 N1 83.33(11) . . ? O1 Y1 N1 110.33(11) 2_656 . ? N1 Y1 N1 162.60(17) 2_656 . ? O1 Y1 O2 147.88(9) . . ? O1 Y1 O2 97.41(9) 2_656 . ? N1 Y1 O2 101.09(10) 2_656 . ? N1 Y1 O2 67.32(10) . . ? O1 Y1 O2 97.41(9) . 2_656 ? O1 Y1 O2 147.88(9) 2_656 2_656 ? N1 Y1 O2 67.32(10) 2_656 2_656 ? N1 Y1 O2 101.09(10) . 2_656 ? O2 Y1 O2 100.69(12) . 2_656 ? O1 Y1 C1 24.46(10) . . ? O1 Y1 C1 104.16(10) 2_656 . ? N1 Y1 C1 117.95(11) 2_656 . ? N1 Y1 C1 70.31(11) . . ? O2 Y1 C1 136.92(9) . . ? O2 Y1 C1 79.93(9) 2_656 . ? O1 Y1 C1 104.16(10) . 2_656 ? O1 Y1 C1 24.46(10) 2_656 2_656 ? N1 Y1 C1 70.31(11) 2_656 2_656 ? N1 Y1 C1 117.95(11) . 2_656 ? O2 Y1 C1 79.93(9) . 2_656 ? O2 Y1 C1 136.92(9) 2_656 2_656 ? C1 Y1 C1 128.40(14) . 2_656 ? O1 Y1 Li1 40.12(7) . . ? O1 Y1 Li1 40.12(7) 2_656 . ? N1 Y1 Li1 98.70(9) 2_656 . ? N1 Y1 Li1 98.70(9) . . ? O2 Y1 Li1 129.66(6) . . ? O2 Y1 Li1 129.66(6) 2_656 . ? C1 Y1 Li1 64.20(7) . . ? C1 Y1 Li1 64.20(7) 2_656 . ? C1 O1 Li1 149.9(3) . . ? C1 O1 Y1 113.7(2) . . ? Li1 O1 Y1 94.0(2) . . ? C9 O2 C14 116.7(3) . . ? C9 O2 Y1 118.4(2) . . ? C14 O2 Y1 122.7(2) . . ? C23 O3 C26 107.7(4) . . ? C23 O3 Li1 129.8(4) . . ? C26 O3 Li1 121.5(4) . . ? C8 N1 C7 116.8(3) . . ? C8 N1 Y1 122.6(2) . . ? C7 N1 Y1 118.7(2) . . ? O1 C1 C6 119.0(3) . . ? O1 C1 C2 122.1(3) . . ? C6 C1 C2 118.9(3) . . ? O1 C1 Y1 41.83(15) . . ? C6 C1 Y1 93.7(2) . . ? C2 C1 Y1 131.6(2) . . ? C3 C2 C1 117.6(3) . . ? C3 C2 C15 120.5(3) . . ? C1 C2 C15 121.9(3) . . ? C2 C3 C4 124.5(3) . . ? C2 C3 H3 117.7 . . ? C4 C3 H3 117.7 . . ? C5 C4 C3 116.2(3) . . ? C5 C4 C19 122.9(3) . . ? C3 C4 C19 120.9(3) . . ? C4 C5 C6 122.6(4) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 120.1(3) . . ? C5 C6 C7 117.4(3) . . ? C1 C6 C7 122.5(3) . . ? N1 C7 C6 113.2(3) . . ? N1 C7 H7A 108.9 . . ? C6 C7 H7A 108.9 . . ? N1 C7 H7B 108.9 . . ? C6 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N1 C8 C9 117.4(3) . . ? N1 C8 C13 127.5(4) . . ? C9 C8 C13 115.1(4) . . ? C10 C9 C8 123.6(4) . . ? C10 C9 O2 123.1(4) . . ? C8 C9 O2 113.3(3) . . ? C9 C10 C11 119.5(4) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 118.7(4) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C11 C12 C13 121.9(4) . . ? C11 C12 H12 119.1 . . ? C13 C12 H12 119.1 . . ? C12 C13 C8 121.2(4) . . ? C12 C13 H13 119.4 . . ? C8 C13 H13 119.4 . . ? O2 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C18 C15 C17 111.4(4) . . ? C18 C15 C2 111.0(3) . . ? C17 C15 C2 109.6(4) . . ? C18 C15 C16 106.5(4) . . ? C17 C15 C16 106.3(3) . . ? C2 C15 C16 111.9(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C21 109.0(4) . . ? C20 C19 C22 108.6(5) . . ? C21 C19 C22 107.1(4) . . ? C20 C19 C4 111.2(3) . . ? C21 C19 C4 111.9(3) . . ? C22 C19 C4 108.9(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O3 C23 C24 107.1(5) . . ? O3 C23 H23A 110.3 . . ? C24 C23 H23A 110.3 . . ? O3 C23 H23B 110.3 . . ? C24 C23 H23B 110.3 . . ? H23A C23 H23B 108.5 . . ? C25 C24 C23 104.3(6) . . ? C25 C24 H24A 110.9 . . ? C23 C24 H24A 110.9 . . ? C25 C24 H24B 110.9 . . ? C23 C24 H24B 110.9 . . ? H24A C24 H24B 108.9 . . ? C24 C25 C26 104.4(5) . . ? C24 C25 H25A 110.9 . . ? C26 C25 H25A 110.9 . . ? C24 C25 H25B 110.9 . . ? C26 C25 H25B 110.9 . . ? H25A C25 H25B 108.9 . . ? O3 C26 C25 102.6(6) . . ? O3 C26 H26A 111.2 . . ? C25 C26 H26A 111.2 . . ? O3 C26 H26B 111.2 . . ? C25 C26 H26B 111.2 . . ? H26A C26 H26B 109.2 . . ? O3 Li1 O3 99.0(5) . 2_656 ? O3 Li1 O1 127.72(13) . 2_656 ? O3 Li1 O1 107.01(16) 2_656 2_656 ? O3 Li1 O1 107.01(16) . . ? O3 Li1 O1 127.72(13) 2_656 . ? O1 Li1 O1 91.8(4) 2_656 . ? O3 Li1 Y1 130.5(2) . . ? O3 Li1 Y1 130.5(2) 2_656 . ? O1 Li1 Y1 45.9(2) 2_656 . ? O1 Li1 Y1 45.9(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Y1 O1 C1 167.8(3) 2_656 . . . ? N1 Y1 O1 C1 -113.1(2) 2_656 . . . ? N1 Y1 O1 C1 55.8(2) . . . . ? O2 Y1 O1 C1 79.4(3) . . . . ? O2 Y1 O1 C1 -44.6(2) 2_656 . . . ? C1 Y1 O1 C1 172.98(17) 2_656 . . . ? Li1 Y1 O1 C1 167.8(3) . . . . ? O1 Y1 O1 Li1 0.000(2) 2_656 . . . ? N1 Y1 O1 Li1 79.09(12) 2_656 . . . ? N1 Y1 O1 Li1 -112.03(12) . . . . ? O2 Y1 O1 Li1 -88.42(18) . . . . ? O2 Y1 O1 Li1 147.59(10) 2_656 . . . ? C1 Y1 O1 Li1 -167.8(3) . . . . ? C1 Y1 O1 Li1 5.18(12) 2_656 . . . ? O1 Y1 O2 C9 -18.7(3) . . . . ? O1 Y1 O2 C9 -102.2(2) 2_656 . . . ? N1 Y1 O2 C9 173.2(2) 2_656 . . . ? N1 Y1 O2 C9 6.8(2) . . . . ? O2 Y1 O2 C9 104.5(2) 2_656 . . . ? C1 Y1 O2 C9 17.8(3) . . . . ? C1 Y1 O2 C9 -119.4(2) 2_656 . . . ? Li1 Y1 O2 C9 -75.5(2) . . . . ? O1 Y1 O2 C14 143.7(3) . . . . ? O1 Y1 O2 C14 60.2(3) 2_656 . . . ? N1 Y1 O2 C14 -24.4(3) 2_656 . . . ? N1 Y1 O2 C14 169.2(3) . . . . ? O2 Y1 O2 C14 -93.1(3) 2_656 . . . ? C1 Y1 O2 C14 -179.8(3) . . . . ? C1 Y1 O2 C14 43.0(3) 2_656 . . . ? Li1 Y1 O2 C14 86.9(3) . . . . ? O1 Y1 N1 C8 157.4(3) . . . . ? O1 Y1 N1 C8 80.4(3) 2_656 . . . ? N1 Y1 N1 C8 -59.8(3) 2_656 . . . ? O2 Y1 N1 C8 -9.2(3) . . . . ? O2 Y1 N1 C8 -106.3(3) 2_656 . . . ? C1 Y1 N1 C8 178.7(3) . . . . ? C1 Y1 N1 C8 54.9(3) 2_656 . . . ? Li1 Y1 N1 C8 120.2(3) . . . . ? O1 Y1 N1 C7 -6.6(3) . . . . ? O1 Y1 N1 C7 -83.6(3) 2_656 . . . ? N1 Y1 N1 C7 136.2(3) 2_656 . . . ? O2 Y1 N1 C7 -173.2(3) . . . . ? O2 Y1 N1 C7 89.7(3) 2_656 . . . ? C1 Y1 N1 C7 14.7(3) . . . . ? C1 Y1 N1 C7 -109.1(3) 2_656 . . . ? Li1 Y1 N1 C7 -43.8(3) . . . . ? Li1 O1 C1 C6 95.7(5) . . . . ? Y1 O1 C1 C6 -59.5(4) . . . . ? Li1 O1 C1 C2 -86.5(6) . . . . ? Y1 O1 C1 C2 118.3(3) . . . . ? Li1 O1 C1 Y1 155.2(6) . . . . ? O1 Y1 C1 O1 -12.4(3) 2_656 . . . ? N1 Y1 C1 O1 77.5(3) 2_656 . . . ? N1 Y1 C1 O1 -119.3(3) . . . . ? O2 Y1 C1 O1 -130.1(2) . . . . ? O2 Y1 C1 O1 135.0(2) 2_656 . . . ? C1 Y1 C1 O1 -8.7(2) 2_656 . . . ? Li1 Y1 C1 O1 -8.7(2) . . . . ? O1 Y1 C1 C6 130.9(4) . . . . ? O1 Y1 C1 C6 118.5(2) 2_656 . . . ? N1 Y1 C1 C6 -151.5(2) 2_656 . . . ? N1 Y1 C1 C6 11.7(2) . . . . ? O2 Y1 C1 C6 0.9(3) . . . . ? O2 Y1 C1 C6 -94.1(2) 2_656 . . . ? C1 Y1 C1 C6 122.3(2) 2_656 . . . ? Li1 Y1 C1 C6 122.3(2) . . . . ? O1 Y1 C1 C2 -94.2(4) . . . . ? O1 Y1 C1 C2 -106.6(3) 2_656 . . . ? N1 Y1 C1 C2 -16.7(4) 2_656 . . . ? N1 Y1 C1 C2 146.5(4) . . . . ? O2 Y1 C1 C2 135.7(3) . . . . ? O2 Y1 C1 C2 40.8(3) 2_656 . . . ? C1 Y1 C1 C2 -102.9(3) 2_656 . . . ? Li1 Y1 C1 C2 -102.9(3) . . . . ? O1 C1 C2 C3 -175.2(3) . . . . ? C6 C1 C2 C3 2.6(5) . . . . ? Y1 C1 C2 C3 -123.5(3) . . . . ? O1 C1 C2 C15 3.9(5) . . . . ? C6 C1 C2 C15 -178.2(3) . . . . ? Y1 C1 C2 C15 55.7(5) . . . . ? C1 C2 C3 C4 -0.5(6) . . . . ? C15 C2 C3 C4 -179.6(4) . . . . ? C2 C3 C4 C5 -1.1(6) . . . . ? C2 C3 C4 C19 179.8(4) . . . . ? C3 C4 C5 C6 0.6(6) . . . . ? C19 C4 C5 C6 179.6(4) . . . . ? C4 C5 C6 C1 1.6(6) . . . . ? C4 C5 C6 C7 -180.0(4) . . . . ? O1 C1 C6 C5 174.7(3) . . . . ? C2 C1 C6 C5 -3.2(5) . . . . ? Y1 C1 C6 C5 139.6(3) . . . . ? O1 C1 C6 C7 -3.7(6) . . . . ? C2 C1 C6 C7 178.4(4) . . . . ? Y1 C1 C6 C7 -38.8(4) . . . . ? C8 N1 C7 C6 154.8(4) . . . . ? Y1 N1 C7 C6 -40.3(5) . . . . ? C5 C6 C7 N1 -118.8(4) . . . . ? C1 C6 C7 N1 59.6(5) . . . . ? C7 N1 C8 C9 175.1(3) . . . . ? Y1 N1 C8 C9 10.8(5) . . . . ? C7 N1 C8 C13 -4.5(6) . . . . ? Y1 N1 C8 C13 -168.8(3) . . . . ? N1 C8 C9 C10 176.7(4) . . . . ? C13 C8 C9 C10 -3.7(6) . . . . ? N1 C8 C9 O2 -3.7(5) . . . . ? C13 C8 C9 O2 175.9(3) . . . . ? C14 O2 C9 C10 12.0(5) . . . . ? Y1 O2 C9 C10 175.5(3) . . . . ? C14 O2 C9 C8 -167.6(3) . . . . ? Y1 O2 C9 C8 -4.1(4) . . . . ? C8 C9 C10 C11 1.3(6) . . . . ? O2 C9 C10 C11 -178.3(4) . . . . ? C9 C10 C11 C12 1.2(7) . . . . ? C10 C11 C12 C13 -1.1(7) . . . . ? C11 C12 C13 C8 -1.5(7) . . . . ? N1 C8 C13 C12 -176.7(4) . . . . ? C9 C8 C13 C12 3.7(6) . . . . ? C3 C2 C15 C18 117.9(4) . . . . ? C1 C2 C15 C18 -61.3(5) . . . . ? C3 C2 C15 C17 -118.6(4) . . . . ? C1 C2 C15 C17 62.2(5) . . . . ? C3 C2 C15 C16 -0.9(5) . . . . ? C1 C2 C15 C16 179.9(4) . . . . ? C5 C4 C19 C20 132.5(5) . . . . ? C3 C4 C19 C20 -48.5(6) . . . . ? C5 C4 C19 C21 10.4(6) . . . . ? C3 C4 C19 C21 -170.6(4) . . . . ? C5 C4 C19 C22 -107.9(5) . . . . ? C3 C4 C19 C22 71.1(5) . . . . ? C26 O3 C23 C24 -28.9(8) . . . . ? Li1 O3 C23 C24 139.0(5) . . . . ? O3 C23 C24 C25 6.9(8) . . . . ? C23 C24 C25 C26 15.5(9) . . . . ? C23 O3 C26 C25 38.1(8) . . . . ? Li1 O3 C26 C25 -131.0(6) . . . . ? C24 C25 C26 O3 -32.4(9) . . . . ? C23 O3 Li1 O3 153.4(6) . . . 2_656 ? C26 O3 Li1 O3 -40.2(5) . . . 2_656 ? C23 O3 Li1 O1 33.6(7) . . . 2_656 ? C26 O3 Li1 O1 -160.0(6) . . . 2_656 ? C23 O3 Li1 O1 -72.5(5) . . . . ? C26 O3 Li1 O1 93.9(6) . . . . ? C23 O3 Li1 Y1 -26.6(6) . . . . ? C26 O3 Li1 Y1 139.8(5) . . . . ? C1 O1 Li1 O3 -26.8(6) . . . . ? Y1 O1 Li1 O3 130.5(2) . . . . ? C1 O1 Li1 O3 89.4(5) . . . 2_656 ? Y1 O1 Li1 O3 -113.2(4) . . . 2_656 ? C1 O1 Li1 O1 -157.3(5) . . . 2_656 ? Y1 O1 Li1 O1 0.0 . . . 2_656 ? C1 O1 Li1 Y1 -157.3(5) . . . . ? O1 Y1 Li1 O3 -73.00(19) . . . . ? O1 Y1 Li1 O3 107.00(19) 2_656 . . . ? N1 Y1 Li1 O3 175.67(17) 2_656 . . . ? N1 Y1 Li1 O3 -4.33(17) . . . . ? O2 Y1 Li1 O3 63.35(17) . . . . ? O2 Y1 Li1 O3 -116.65(17) 2_656 . . . ? C1 Y1 Li1 O3 -67.42(17) . . . . ? C1 Y1 Li1 O3 112.58(17) 2_656 . . . ? O1 Y1 Li1 O3 107.00(19) . . . 2_656 ? O1 Y1 Li1 O3 -73.00(19) 2_656 . . 2_656 ? N1 Y1 Li1 O3 -4.33(17) 2_656 . . 2_656 ? N1 Y1 Li1 O3 175.67(17) . . . 2_656 ? O2 Y1 Li1 O3 -116.65(17) . . . 2_656 ? O2 Y1 Li1 O3 63.35(17) 2_656 . . 2_656 ? C1 Y1 Li1 O3 112.58(17) . . . 2_656 ? C1 Y1 Li1 O3 -67.42(17) 2_656 . . 2_656 ? O1 Y1 Li1 O1 180.0 . . . 2_656 ? N1 Y1 Li1 O1 68.66(13) 2_656 . . 2_656 ? N1 Y1 Li1 O1 -111.34(13) . . . 2_656 ? O2 Y1 Li1 O1 -43.65(14) . . . 2_656 ? O2 Y1 Li1 O1 136.35(14) 2_656 . . 2_656 ? C1 Y1 Li1 O1 -174.42(13) . . . 2_656 ? C1 Y1 Li1 O1 5.58(13) 2_656 . . 2_656 ? O1 Y1 Li1 O1 180.0 2_656 . . . ? N1 Y1 Li1 O1 -111.34(13) 2_656 . . . ? N1 Y1 Li1 O1 68.66(13) . . . . ? O2 Y1 Li1 O1 136.35(14) . . . . ? O2 Y1 Li1 O1 -43.65(14) 2_656 . . . ? C1 Y1 Li1 O1 5.58(13) . . . . ? C1 Y1 Li1 O1 -174.42(13) 2_656 . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.960 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.081 _database_code_depnum_ccdc_archive 'CCDC 932399' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H74 Li N2 O6 Yb' _chemical_formula_sum 'C52 H74 Li N2 O6 Yb' _chemical_formula_weight 1003.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 27.682(2) _cell_length_b 9.8350(5) _cell_length_c 20.3641(16) _cell_angle_alpha 90.00 _cell_angle_beta 114.208(2) _cell_angle_gamma 90.00 _cell_volume 5056.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10816 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2084 _exptl_absorpt_coefficient_mu 1.897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.570 _exptl_absorpt_correction_T_max 0.759 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12695 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_unetI/netI 0.0448 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4693 _reflns_number_gt 4222 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Their C24-C25 and C25-C26 distances were constrained. ; _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^)+(0.0706P)^2^+6.0723P] 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 4693 _refine_ls_number_parameters 271 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1285 _refine_ls_wR_factor_gt 0.1240 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.105 _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 Yb1 Yb 0.5000 0.39005(3) 0.7500 0.04623(15) Uani 1 2 d S . . O1 O 0.54676(15) 0.5572(4) 0.81353(18) 0.0512(9) Uani 1 1 d . . . O2 O 0.42883(14) 0.2330(4) 0.7232(2) 0.0509(9) Uani 1 1 d . . . O3 O 0.4838(2) 0.8221(6) 0.8116(4) 0.110(2) Uani 1 1 d . . . N1 N 0.48011(18) 0.3552(5) 0.8454(2) 0.0510(11) Uani 1 1 d . . . C1 C 0.5830(2) 0.5223(5) 0.8809(3) 0.0479(12) Uani 1 1 d . . . C2 C 0.6383(2) 0.5426(5) 0.9030(3) 0.0468(12) Uani 1 1 d . . . C3 C 0.6720(2) 0.4946(5) 0.9712(3) 0.0487(12) Uani 1 1 d . . . H3 H 0.7086 0.5094 0.9865 0.058 Uiso 1 1 calc R . . C4 C 0.6552(2) 0.4263(6) 1.0181(3) 0.0498(13) Uani 1 1 d . . . C5 C 0.6011(2) 0.4124(6) 0.9955(3) 0.0503(13) Uani 1 1 d . . . H5 H 0.5880 0.3690 1.0260 0.060 Uiso 1 1 calc R . . C6 C 0.5651(2) 0.4611(6) 0.9284(3) 0.0494(12) Uani 1 1 d . . . C7 C 0.5062(2) 0.4379(7) 0.9095(3) 0.0608(15) Uani 1 1 d . . . H7A H 0.5025 0.3935 0.9503 0.073 Uiso 1 1 calc R . . H7B H 0.4883 0.5263 0.9021 0.073 Uiso 1 1 calc R . . C8 C 0.4361(2) 0.2862(5) 0.8401(3) 0.0490(12) Uani 1 1 d . . . C9 C 0.4079(2) 0.2131(5) 0.7749(3) 0.0504(13) Uani 1 1 d . . . C10 C 0.3647(3) 0.1340(6) 0.7632(4) 0.0602(15) Uani 1 1 d . . . H10 H 0.3477 0.0881 0.7192 0.072 Uiso 1 1 calc R . . C11 C 0.3460(3) 0.1214(7) 0.8170(4) 0.0717(19) Uani 1 1 d . . . H11 H 0.3173 0.0638 0.8107 0.086 Uiso 1 1 calc R . . C12 C 0.3706(3) 0.1960(8) 0.8799(4) 0.0731(19) Uani 1 1 d . . . H12 H 0.3572 0.1913 0.9156 0.088 Uiso 1 1 calc R . . C13 C 0.4143(2) 0.2772(7) 0.8915(3) 0.0625(15) Uani 1 1 d . . . H13 H 0.4297 0.3271 0.9345 0.075 Uiso 1 1 calc R . . C14 C 0.3972(3) 0.1865(6) 0.6509(3) 0.0640(15) Uani 1 1 d . . . H14A H 0.3910 0.0895 0.6515 0.096 Uiso 1 1 calc R . . H14B H 0.4159 0.2047 0.6205 0.096 Uiso 1 1 calc R . . H14C H 0.3636 0.2341 0.6320 0.096 Uiso 1 1 calc R . . C15 C 0.6613(3) 0.6150(5) 0.8553(3) 0.0550(14) Uani 1 1 d . . . C16 C 0.7223(3) 0.6246(6) 0.8917(4) 0.0657(17) Uani 1 1 d . . . H16A H 0.7373 0.5339 0.8988 0.099 Uiso 1 1 calc R . . H16B H 0.7331 0.6696 0.9379 0.099 Uiso 1 1 calc R . . H16C H 0.7349 0.6763 0.8612 0.099 Uiso 1 1 calc R . . C17 C 0.6403(3) 0.7621(7) 0.8401(4) 0.082(2) Uani 1 1 d . . . H17A H 0.6493 0.8097 0.8853 0.122 Uiso 1 1 calc R . . H17B H 0.6022 0.7608 0.8134 0.122 Uiso 1 1 calc R . . H17C H 0.6564 0.8085 0.8120 0.122 Uiso 1 1 calc R . . C18 C 0.6473(3) 0.5375(7) 0.7856(3) 0.0689(17) Uani 1 1 d . . . H18A H 0.6638 0.5812 0.7573 0.103 Uiso 1 1 calc R . . H18B H 0.6092 0.5369 0.7586 0.103 Uiso 1 1 calc R . . H18C H 0.6601 0.4448 0.7963 0.103 Uiso 1 1 calc R . . C19 C 0.6953(2) 0.3760(6) 1.0915(3) 0.0548(14) Uani 1 1 d . . . C20 C 0.7397(3) 0.2976(10) 1.0834(4) 0.098(3) Uani 1 1 d . . . H20A H 0.7592 0.3579 1.0654 0.147 Uiso 1 1 calc R . . H20B H 0.7250 0.2232 1.0498 0.147 Uiso 1 1 calc R . . H20C H 0.7634 0.2616 1.1298 0.147 Uiso 1 1 calc R . . C21 C 0.6691(3) 0.2808(10) 1.1269(4) 0.095(3) Uani 1 1 d . . . H21A H 0.6958 0.2454 1.1715 0.143 Uiso 1 1 calc R . . H21B H 0.6522 0.2060 1.0945 0.143 Uiso 1 1 calc R . . H21C H 0.6427 0.3307 1.1370 0.143 Uiso 1 1 calc R . . C22 C 0.7175(3) 0.4956(8) 1.1410(4) 0.087(2) Uani 1 1 d . . . H22A H 0.7419 0.4634 1.1880 0.131 Uiso 1 1 calc R . . H22B H 0.6889 0.5455 1.1457 0.131 Uiso 1 1 calc R . . H22C H 0.7362 0.5549 1.1212 0.131 Uiso 1 1 calc R . . C23 C 0.4486(4) 0.8138(13) 0.8440(6) 0.1312(19) Uani 1 1 d . . . H23A H 0.4396 0.7187 0.8480 0.157 Uiso 1 1 calc R . . H23B H 0.4159 0.8632 0.8155 0.157 Uiso 1 1 calc R . . C24 C 0.4756(4) 0.8767(12) 0.9175(6) 0.1312(19) Uani 1 1 d D . . H24A H 0.4528 0.9437 0.9263 0.157 Uiso 1 1 calc R . . H24B H 0.4861 0.8074 0.9554 0.157 Uiso 1 1 calc R . . C25 C 0.5221(4) 0.9418(13) 0.9135(5) 0.1312(19) Uani 1 1 d D . . H25A H 0.5543 0.8898 0.9414 0.157 Uiso 1 1 calc R . . H25B H 0.5265 1.0344 0.9328 0.157 Uiso 1 1 calc R . . C26 C 0.5121(5) 0.9445(13) 0.8331(5) 0.1312(19) Uani 1 1 d D . . H26A H 0.4909 1.0232 0.8080 0.157 Uiso 1 1 calc R . . H26B H 0.5452 0.9426 0.8264 0.157 Uiso 1 1 calc R . . Li1 Li 0.5000 0.6983(13) 0.7500 0.054(3) Uani 1 2 d S . . 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 Yb1 0.0578(2) 0.0399(2) 0.0448(2) 0.000 0.02492(17) 0.000 O1 0.060(2) 0.048(2) 0.0421(19) 0.0033(17) 0.0173(18) -0.0012(18) O2 0.059(2) 0.0434(19) 0.058(2) -0.0040(17) 0.0317(19) -0.0034(17) O3 0.094(4) 0.087(4) 0.190(6) -0.074(4) 0.099(4) -0.041(3) N1 0.050(3) 0.062(3) 0.048(2) 0.000(2) 0.028(2) 0.001(2) C1 0.066(3) 0.035(3) 0.043(3) -0.002(2) 0.023(3) -0.001(2) C2 0.062(3) 0.033(3) 0.043(3) -0.002(2) 0.020(3) -0.005(2) C3 0.052(3) 0.047(3) 0.047(3) -0.001(2) 0.020(3) -0.001(2) C4 0.062(3) 0.048(3) 0.042(3) -0.002(2) 0.024(3) 0.005(3) C5 0.062(3) 0.055(3) 0.039(3) 0.001(2) 0.026(3) 0.003(3) C6 0.055(3) 0.053(3) 0.044(3) -0.008(2) 0.024(3) 0.000(3) C7 0.059(3) 0.083(4) 0.045(3) 0.001(3) 0.025(3) 0.006(3) C8 0.053(3) 0.047(3) 0.052(3) 0.012(2) 0.027(3) 0.012(2) C9 0.050(3) 0.046(3) 0.063(3) 0.012(3) 0.030(3) 0.007(2) C10 0.058(4) 0.054(3) 0.068(4) 0.011(3) 0.026(3) 0.001(3) C11 0.060(4) 0.078(5) 0.083(5) 0.020(4) 0.036(4) -0.004(3) C12 0.061(4) 0.098(5) 0.073(4) 0.027(4) 0.041(4) 0.010(4) C13 0.062(4) 0.076(4) 0.057(3) 0.009(3) 0.031(3) 0.011(3) C14 0.075(4) 0.057(4) 0.062(4) -0.008(3) 0.031(3) -0.010(3) C15 0.069(4) 0.043(3) 0.052(3) 0.006(2) 0.023(3) -0.009(3) C16 0.072(4) 0.060(4) 0.069(4) 0.007(3) 0.033(4) -0.013(3) C17 0.095(5) 0.050(4) 0.087(5) 0.013(3) 0.024(4) -0.012(4) C18 0.086(5) 0.077(4) 0.057(3) 0.001(3) 0.043(3) -0.022(4) C19 0.059(3) 0.068(4) 0.040(3) 0.006(2) 0.024(3) 0.010(3) C20 0.109(6) 0.127(7) 0.072(4) 0.039(5) 0.051(5) 0.063(6) C21 0.090(5) 0.125(7) 0.058(4) 0.032(4) 0.016(4) -0.008(5) C22 0.089(5) 0.085(5) 0.059(4) -0.010(4) 0.002(4) 0.007(4) C23 0.122(4) 0.154(5) 0.108(4) -0.015(4) 0.037(3) -0.047(4) C24 0.122(4) 0.154(5) 0.108(4) -0.015(4) 0.037(3) -0.047(4) C25 0.122(4) 0.154(5) 0.108(4) -0.015(4) 0.037(3) -0.047(4) C26 0.122(4) 0.154(5) 0.108(4) -0.015(4) 0.037(3) -0.047(4) Li1 0.043(7) 0.054(8) 0.073(8) 0.000 0.033(6) 0.000 _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 Yb1 O1 2.163(4) . ? Yb1 O1 2.163(4) 2_656 ? Yb1 N1 2.253(4) 2_656 ? Yb1 N1 2.253(4) . ? Yb1 O2 2.384(4) . ? Yb1 O2 2.384(4) 2_656 ? Yb1 C1 3.009(5) . ? Yb1 C1 3.009(5) 2_656 ? Yb1 Li1 3.031(13) . ? Yb1 C8 3.193(5) 2_656 ? Yb1 C8 3.193(5) . ? O1 C1 1.371(6) . ? O1 Li1 1.975(10) . ? O2 C9 1.408(6) . ? O2 C14 1.445(7) . ? O3 C23 1.384(11) . ? O3 C26 1.405(12) . ? O3 Li1 1.930(10) . ? N1 C8 1.359(7) . ? N1 C7 1.454(8) . ? C1 C6 1.392(7) . ? C1 C2 1.421(8) . ? C2 C3 1.401(7) . ? C2 C15 1.537(8) . ? C3 C4 1.394(8) . ? C3 H3 0.9400 . ? C4 C5 1.380(8) . ? C4 C19 1.533(8) . ? C5 C6 1.405(8) . ? C5 H5 0.9400 . ? C6 C7 1.530(8) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C13 1.410(7) . ? C8 C9 1.429(8) . ? C9 C10 1.362(8) . ? C10 C11 1.396(10) . ? C10 H10 0.9400 . ? C11 C12 1.389(10) . ? C11 H11 0.9400 . ? C12 C13 1.388(9) . ? C12 H12 0.9400 . ? C13 H13 0.9400 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 C18 1.514(9) . ? C15 C17 1.542(9) . ? C15 C16 1.545(9) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C22 1.507(9) . ? C19 C20 1.518(9) . ? C19 C21 1.532(9) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 C24 1.505(14) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.470(12) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.545(12) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? Li1 O3 1.930(10) 2_656 ? Li1 O1 1.975(10) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Yb1 O1 81.08(19) . 2_656 ? O1 Yb1 N1 109.49(16) . 2_656 ? O1 Yb1 N1 84.12(16) 2_656 2_656 ? O1 Yb1 N1 84.12(16) . . ? O1 Yb1 N1 109.49(16) 2_656 . ? N1 Yb1 N1 162.5(3) 2_656 . ? O1 Yb1 O2 149.90(13) . . ? O1 Yb1 O2 96.88(14) 2_656 . ? N1 Yb1 O2 100.09(15) 2_656 . ? N1 Yb1 O2 68.14(15) . . ? O1 Yb1 O2 96.88(14) . 2_656 ? O1 Yb1 O2 149.90(13) 2_656 2_656 ? N1 Yb1 O2 68.14(15) 2_656 2_656 ? N1 Yb1 O2 100.09(15) . 2_656 ? O2 Yb1 O2 99.22(17) . 2_656 ? O1 Yb1 C1 24.40(14) . . ? O1 Yb1 C1 104.71(14) 2_656 . ? N1 Yb1 C1 117.53(16) 2_656 . ? N1 Yb1 C1 70.69(16) . . ? O2 Yb1 C1 137.90(13) . . ? O2 Yb1 C1 79.52(14) 2_656 . ? O1 Yb1 C1 104.71(14) . 2_656 ? O1 Yb1 C1 24.40(14) 2_656 2_656 ? N1 Yb1 C1 70.69(16) 2_656 2_656 ? N1 Yb1 C1 117.53(16) . 2_656 ? O2 Yb1 C1 79.52(14) . 2_656 ? O2 Yb1 C1 137.90(13) 2_656 2_656 ? C1 Yb1 C1 128.8(2) . 2_656 ? O1 Yb1 Li1 40.54(10) . . ? O1 Yb1 Li1 40.54(10) 2_656 . ? N1 Yb1 Li1 98.75(13) 2_656 . ? N1 Yb1 Li1 98.75(13) . . ? O2 Yb1 Li1 130.39(9) . . ? O2 Yb1 Li1 130.39(9) 2_656 . ? C1 Yb1 Li1 64.40(10) . . ? C1 Yb1 Li1 64.40(10) 2_656 . ? O1 Yb1 C8 104.48(14) . 2_656 ? O1 Yb1 C8 103.64(14) 2_656 2_656 ? N1 Yb1 C8 21.06(16) 2_656 2_656 ? N1 Yb1 C8 146.71(16) . 2_656 ? O2 Yb1 C8 105.16(12) . 2_656 ? O2 Yb1 C8 47.48(13) 2_656 2_656 ? C1 Yb1 C8 104.23(14) . 2_656 ? C1 Yb1 C8 91.75(14) 2_656 2_656 ? Li1 Yb1 C8 108.64(10) . 2_656 ? O1 Yb1 C8 103.64(14) . . ? O1 Yb1 C8 104.48(13) 2_656 . ? N1 Yb1 C8 146.71(16) 2_656 . ? N1 Yb1 C8 21.06(16) . . ? O2 Yb1 C8 47.48(13) . . ? O2 Yb1 C8 105.16(12) 2_656 . ? C1 Yb1 C8 91.75(14) . . ? C1 Yb1 C8 104.23(14) 2_656 . ? Li1 Yb1 C8 108.64(10) . . ? C8 Yb1 C8 142.71(19) 2_656 . ? C1 O1 Li1 147.8(4) . . ? C1 O1 Yb1 114.9(3) . . ? Li1 O1 Yb1 94.1(3) . . ? C9 O2 C14 117.1(4) . . ? C9 O2 Yb1 118.3(3) . . ? C14 O2 Yb1 122.4(3) . . ? C23 O3 C26 108.4(8) . . ? C23 O3 Li1 132.0(7) . . ? C26 O3 Li1 119.6(6) . . ? C8 N1 C7 116.7(4) . . ? C8 N1 Yb1 122.4(4) . . ? C7 N1 Yb1 118.8(4) . . ? O1 C1 C6 118.7(5) . . ? O1 C1 C2 122.1(5) . . ? C6 C1 C2 119.1(5) . . ? O1 C1 Yb1 40.7(2) . . ? C6 C1 Yb1 93.9(3) . . ? C2 C1 Yb1 132.3(3) . . ? C3 C2 C1 117.3(5) . . ? C3 C2 C15 120.2(5) . . ? C1 C2 C15 122.5(5) . . ? C4 C3 C2 124.6(5) . . ? C4 C3 H3 117.7 . . ? C2 C3 H3 117.7 . . ? C5 C4 C3 116.1(5) . . ? C5 C4 C19 123.0(5) . . ? C3 C4 C19 120.8(5) . . ? C4 C5 C6 122.1(5) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C1 C6 C5 120.6(5) . . ? C1 C6 C7 122.4(5) . . ? C5 C6 C7 116.9(5) . . ? N1 C7 C6 113.2(4) . . ? N1 C7 H7A 108.9 . . ? C6 C7 H7A 108.9 . . ? N1 C7 H7B 108.9 . . ? C6 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N1 C8 C13 128.0(5) . . ? N1 C8 C9 117.1(4) . . ? C13 C8 C9 114.9(5) . . ? N1 C8 Yb1 36.6(2) . . ? C13 C8 Yb1 162.5(4) . . ? C9 C8 Yb1 81.2(3) . . ? C10 C9 O2 123.3(5) . . ? C10 C9 C8 123.8(5) . . ? O2 C9 C8 112.9(4) . . ? C9 C10 C11 119.7(6) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 118.6(6) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C13 C12 C11 121.6(6) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C8 121.3(6) . . ? C12 C13 H13 119.3 . . ? C8 C13 H13 119.3 . . ? O2 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C18 C15 C2 110.3(4) . . ? C18 C15 C17 110.7(6) . . ? C2 C15 C17 110.0(5) . . ? C18 C15 C16 106.8(6) . . ? C2 C15 C16 112.3(5) . . ? C17 C15 C16 106.6(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22 C19 C20 110.0(6) . . ? C22 C19 C21 107.8(6) . . ? C20 C19 C21 107.6(6) . . ? C22 C19 C4 109.5(5) . . ? C20 C19 C4 110.6(5) . . ? C21 C19 C4 111.3(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O3 C23 C24 106.8(8) . . ? O3 C23 H23A 110.4 . . ? C24 C23 H23A 110.4 . . ? O3 C23 H23B 110.4 . . ? C24 C23 H23B 110.4 . . ? H23A C23 H23B 108.6 . . ? C25 C24 C23 102.3(9) . . ? C25 C24 H24A 111.3 . . ? C23 C24 H24A 111.3 . . ? C25 C24 H24B 111.3 . . ? C23 C24 H24B 111.3 . . ? H24A C24 H24B 109.2 . . ? C24 C25 C26 106.6(9) . . ? C24 C25 H25A 110.4 . . ? C26 C25 H25A 110.4 . . ? C24 C25 H25B 110.4 . . ? C26 C25 H25B 110.4 . . ? H25A C25 H25B 108.6 . . ? O3 C26 C25 98.6(8) . . ? O3 C26 H26A 112.1 . . ? C25 C26 H26A 112.1 . . ? O3 C26 H26B 112.1 . . ? C25 C26 H26B 112.1 . . ? H26A C26 H26B 109.7 . . ? O3 Li1 O3 101.7(7) 2_656 . ? O3 Li1 O1 106.4(3) 2_656 2_656 ? O3 Li1 O1 127.20(19) . 2_656 ? O3 Li1 O1 127.20(19) 2_656 . ? O3 Li1 O1 106.4(3) . . ? O1 Li1 O1 90.7(6) 2_656 . ? O3 Li1 Yb1 129.1(4) 2_656 . ? O3 Li1 Yb1 129.1(4) . . ? O1 Li1 Yb1 45.4(3) 2_656 . ? O1 Li1 Yb1 45.4(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 O1 Yb1 O1 C1 165.5(4) 2_656 . . . ? N1 Yb1 O1 C1 -114.0(3) 2_656 . . . ? N1 Yb1 O1 C1 54.7(3) . . . . ? O2 Yb1 O1 C1 77.2(4) . . . . ? O2 Yb1 O1 C1 -44.8(3) 2_656 . . . ? C1 Yb1 O1 C1 171.7(2) 2_656 . . . ? Li1 Yb1 O1 C1 165.5(4) . . . . ? C8 Yb1 O1 C1 -92.6(3) 2_656 . . . ? C8 Yb1 O1 C1 62.7(4) . . . . ? O1 Yb1 O1 Li1 0.000(2) 2_656 . . . ? N1 Yb1 O1 Li1 80.47(18) 2_656 . . . ? N1 Yb1 O1 Li1 -110.83(17) . . . . ? O2 Yb1 O1 Li1 -88.3(3) . . . . ? O2 Yb1 O1 Li1 149.67(14) 2_656 . . . ? C1 Yb1 O1 Li1 -165.5(4) . . . . ? C1 Yb1 O1 Li1 6.13(17) 2_656 . . . ? C8 Yb1 O1 Li1 101.89(16) 2_656 . . . ? C8 Yb1 O1 Li1 -102.85(14) . . . . ? O1 Yb1 O2 C9 -16.9(5) . . . . ? O1 Yb1 O2 C9 -101.0(3) 2_656 . . . ? N1 Yb1 O2 C9 173.8(3) 2_656 . . . ? N1 Yb1 O2 C9 7.3(3) . . . . ? O2 Yb1 O2 C9 104.5(3) 2_656 . . . ? C1 Yb1 O2 C9 20.0(4) . . . . ? C1 Yb1 O2 C9 -118.2(3) 2_656 . . . ? Li1 Yb1 O2 C9 -75.5(3) . . . . ? C8 Yb1 O2 C9 152.8(3) 2_656 . . . ? C8 Yb1 O2 C9 2.4(3) . . . . ? O1 Yb1 O2 C14 145.8(4) . . . . ? O1 Yb1 O2 C14 61.7(4) 2_656 . . . ? N1 Yb1 O2 C14 -23.5(4) 2_656 . . . ? N1 Yb1 O2 C14 170.0(4) . . . . ? O2 Yb1 O2 C14 -92.8(4) 2_656 . . . ? C1 Yb1 O2 C14 -177.3(4) . . . . ? C1 Yb1 O2 C14 44.5(4) 2_656 . . . ? Li1 Yb1 O2 C14 87.2(4) . . . . ? C8 Yb1 O2 C14 -44.5(4) 2_656 . . . ? C8 Yb1 O2 C14 165.1(5) . . . . ? O1 Yb1 N1 C8 157.9(4) . . . . ? O1 Yb1 N1 C8 79.6(4) 2_656 . . . ? N1 Yb1 N1 C8 -60.0(4) 2_656 . . . ? O2 Yb1 N1 C8 -10.1(4) . . . . ? O2 Yb1 N1 C8 -106.1(4) 2_656 . . . ? C1 Yb1 N1 C8 178.9(4) . . . . ? C1 Yb1 N1 C8 54.4(5) 2_656 . . . ? Li1 Yb1 N1 C8 120.0(4) . . . . ? C8 Yb1 N1 C8 -94.5(5) 2_656 . . . ? O1 Yb1 N1 C7 -5.1(4) . . . . ? O1 Yb1 N1 C7 -83.5(4) 2_656 . . . ? N1 Yb1 N1 C7 137.0(4) 2_656 . . . ? O2 Yb1 N1 C7 -173.2(5) . . . . ? O2 Yb1 N1 C7 90.9(4) 2_656 . . . ? C1 Yb1 N1 C7 15.8(4) . . . . ? C1 Yb1 N1 C7 -108.6(4) 2_656 . . . ? Li1 Yb1 N1 C7 -43.0(4) . . . . ? C8 Yb1 N1 C7 102.4(5) 2_656 . . . ? C8 Yb1 N1 C7 -163.0(7) . . . . ? Li1 O1 C1 C6 93.4(8) . . . . ? Yb1 O1 C1 C6 -58.8(5) . . . . ? Li1 O1 C1 C2 -88.7(8) . . . . ? Yb1 O1 C1 C2 119.2(4) . . . . ? Li1 O1 C1 Yb1 152.1(8) . . . . ? O1 Yb1 C1 O1 -14.8(4) 2_656 . . . ? N1 Yb1 C1 O1 76.2(4) 2_656 . . . ? N1 Yb1 C1 O1 -120.7(4) . . . . ? O2 Yb1 C1 O1 -133.2(3) . . . . ? O2 Yb1 C1 O1 134.6(3) 2_656 . . . ? C1 Yb1 C1 O1 -10.4(3) 2_656 . . . ? Li1 Yb1 C1 O1 -10.4(3) . . . . ? C8 Yb1 C1 O1 93.8(3) 2_656 . . . ? C8 Yb1 C1 O1 -120.3(3) . . . . ? O1 Yb1 C1 C6 131.3(5) . . . . ? O1 Yb1 C1 C6 116.5(3) 2_656 . . . ? N1 Yb1 C1 C6 -152.5(3) 2_656 . . . ? N1 Yb1 C1 C6 10.6(3) . . . . ? O2 Yb1 C1 C6 -1.9(4) . . . . ? O2 Yb1 C1 C6 -94.1(3) 2_656 . . . ? C1 Yb1 C1 C6 120.9(3) 2_656 . . . ? Li1 Yb1 C1 C6 120.9(3) . . . . ? C8 Yb1 C1 C6 -135.0(3) 2_656 . . . ? C8 Yb1 C1 C6 11.0(3) . . . . ? O1 Yb1 C1 C2 -92.6(6) . . . . ? O1 Yb1 C1 C2 -107.4(5) 2_656 . . . ? N1 Yb1 C1 C2 -16.4(5) 2_656 . . . ? N1 Yb1 C1 C2 146.7(5) . . . . ? O2 Yb1 C1 C2 134.2(4) . . . . ? O2 Yb1 C1 C2 42.0(5) 2_656 . . . ? C1 Yb1 C1 C2 -103.0(5) 2_656 . . . ? Li1 Yb1 C1 C2 -103.0(5) . . . . ? C8 Yb1 C1 C2 1.1(5) 2_656 . . . ? C8 Yb1 C1 C2 147.1(5) . . . . ? O1 C1 C2 C3 -175.7(5) . . . . ? C6 C1 C2 C3 2.3(7) . . . . ? Yb1 C1 C2 C3 -125.4(5) . . . . ? O1 C1 C2 C15 4.9(8) . . . . ? C6 C1 C2 C15 -177.2(5) . . . . ? Yb1 C1 C2 C15 55.1(7) . . . . ? C1 C2 C3 C4 1.3(8) . . . . ? C15 C2 C3 C4 -179.2(5) . . . . ? C2 C3 C4 C5 -3.2(8) . . . . ? C2 C3 C4 C19 179.2(5) . . . . ? C3 C4 C5 C6 1.6(8) . . . . ? C19 C4 C5 C6 179.0(5) . . . . ? O1 C1 C6 C5 174.1(5) . . . . ? C2 C1 C6 C5 -3.9(8) . . . . ? Yb1 C1 C6 C5 140.2(5) . . . . ? O1 C1 C6 C7 -3.2(8) . . . . ? C2 C1 C6 C7 178.8(5) . . . . ? Yb1 C1 C6 C7 -37.2(6) . . . . ? C4 C5 C6 C1 1.9(8) . . . . ? C4 C5 C6 C7 179.4(5) . . . . ? C8 N1 C7 C6 155.0(5) . . . . ? Yb1 N1 C7 C6 -41.0(7) . . . . ? C1 C6 C7 N1 58.4(8) . . . . ? C5 C6 C7 N1 -119.0(6) . . . . ? C7 N1 C8 C13 -4.8(8) . . . . ? Yb1 N1 C8 C13 -168.2(4) . . . . ? C7 N1 C8 C9 175.3(5) . . . . ? Yb1 N1 C8 C9 11.9(6) . . . . ? C7 N1 C8 Yb1 163.4(7) . . . . ? O1 Yb1 C8 N1 -22.6(4) . . . . ? O1 Yb1 C8 N1 -106.7(4) 2_656 . . . ? N1 Yb1 C8 N1 151.7(5) 2_656 . . . ? O2 Yb1 C8 N1 167.2(5) . . . . ? O2 Yb1 C8 N1 78.6(4) 2_656 . . . ? C1 Yb1 C8 N1 -1.1(4) . . . . ? C1 Yb1 C8 N1 -131.9(4) 2_656 . . . ? Li1 Yb1 C8 N1 -64.6(4) . . . . ? C8 Yb1 C8 N1 115.4(4) 2_656 . . . ? O1 Yb1 C8 C13 10.0(13) . . . . ? O1 Yb1 C8 C13 -74.1(13) 2_656 . . . ? N1 Yb1 C8 C13 -175.7(12) 2_656 . . . ? N1 Yb1 C8 C13 32.6(12) . . . . ? O2 Yb1 C8 C13 -160.2(13) . . . . ? O2 Yb1 C8 C13 111.1(13) 2_656 . . . ? C1 Yb1 C8 C13 31.5(13) . . . . ? C1 Yb1 C8 C13 -99.3(13) 2_656 . . . ? Li1 Yb1 C8 C13 -32.0(13) . . . . ? C8 Yb1 C8 C13 148.0(13) 2_656 . . . ? O1 Yb1 C8 C9 168.1(3) . . . . ? O1 Yb1 C8 C9 84.0(3) 2_656 . . . ? N1 Yb1 C8 C9 -17.6(4) 2_656 . . . ? N1 Yb1 C8 C9 -169.3(6) . . . . ? O2 Yb1 C8 C9 -2.1(3) . . . . ? O2 Yb1 C8 C9 -90.7(3) 2_656 . . . ? C1 Yb1 C8 C9 -170.4(3) . . . . ? C1 Yb1 C8 C9 58.8(3) 2_656 . . . ? Li1 Yb1 C8 C9 126.1(3) . . . . ? C8 Yb1 C8 C9 -53.9(3) 2_656 . . . ? C14 O2 C9 C10 11.2(7) . . . . ? Yb1 O2 C9 C10 174.9(4) . . . . ? C14 O2 C9 C8 -167.8(5) . . . . ? Yb1 O2 C9 C8 -4.2(5) . . . . ? N1 C8 C9 C10 176.6(5) . . . . ? C13 C8 C9 C10 -3.4(8) . . . . ? Yb1 C8 C9 C10 -176.3(5) . . . . ? N1 C8 C9 O2 -4.3(7) . . . . ? C13 C8 C9 O2 175.7(4) . . . . ? Yb1 C8 C9 O2 2.8(4) . . . . ? O2 C9 C10 C11 -179.0(5) . . . . ? C8 C9 C10 C11 0.0(9) . . . . ? C9 C10 C11 C12 3.1(9) . . . . ? C10 C11 C12 C13 -2.8(10) . . . . ? C11 C12 C13 C8 -0.7(10) . . . . ? N1 C8 C13 C12 -176.3(6) . . . . ? C9 C8 C13 C12 3.7(8) . . . . ? Yb1 C8 C13 C12 159.7(10) . . . . ? C3 C2 C15 C18 119.2(6) . . . . ? C1 C2 C15 C18 -61.3(7) . . . . ? C3 C2 C15 C17 -118.3(6) . . . . ? C1 C2 C15 C17 61.1(7) . . . . ? C3 C2 C15 C16 0.3(7) . . . . ? C1 C2 C15 C16 179.7(5) . . . . ? C5 C4 C19 C22 -105.3(7) . . . . ? C3 C4 C19 C22 72.1(7) . . . . ? C5 C4 C19 C20 133.3(7) . . . . ? C3 C4 C19 C20 -49.3(8) . . . . ? C5 C4 C19 C21 13.8(8) . . . . ? C3 C4 C19 C21 -168.9(6) . . . . ? C26 O3 C23 C24 -35.6(13) . . . . ? Li1 O3 C23 C24 141.9(9) . . . . ? O3 C23 C24 C25 11.2(14) . . . . ? C23 C24 C25 C26 14.1(15) . . . . ? C23 O3 C26 C25 42.0(12) . . . . ? Li1 O3 C26 C25 -135.8(8) . . . . ? C24 C25 C26 O3 -33.7(14) . . . . ? C23 O3 Li1 O3 146.7(11) . . . 2_656 ? C26 O3 Li1 O3 -36.1(7) . . . 2_656 ? C23 O3 Li1 O1 25.4(13) . . . 2_656 ? C26 O3 Li1 O1 -157.4(8) . . . 2_656 ? C23 O3 Li1 O1 -78.5(10) . . . . ? C26 O3 Li1 O1 98.7(9) . . . . ? C23 O3 Li1 Yb1 -33.3(11) . . . . ? C26 O3 Li1 Yb1 143.9(7) . . . . ? C1 O1 Li1 O3 93.8(8) . . . 2_656 ? Yb1 O1 Li1 O3 -111.4(6) . . . 2_656 ? C1 O1 Li1 O3 -25.5(8) . . . . ? Yb1 O1 Li1 O3 129.4(3) . . . . ? C1 O1 Li1 O1 -154.9(7) . . . 2_656 ? Yb1 O1 Li1 O1 0.0 . . . 2_656 ? C1 O1 Li1 Yb1 -154.9(7) . . . . ? O1 Yb1 Li1 O3 107.0(3) . . . 2_656 ? O1 Yb1 Li1 O3 -73.0(3) 2_656 . . 2_656 ? N1 Yb1 Li1 O3 -2.9(3) 2_656 . . 2_656 ? N1 Yb1 Li1 O3 177.1(3) . . . 2_656 ? O2 Yb1 Li1 O3 -114.2(3) . . . 2_656 ? O2 Yb1 Li1 O3 65.8(3) 2_656 . . 2_656 ? C1 Yb1 Li1 O3 113.6(3) . . . 2_656 ? C1 Yb1 Li1 O3 -66.4(3) 2_656 . . 2_656 ? C8 Yb1 Li1 O3 16.3(3) 2_656 . . 2_656 ? C8 Yb1 Li1 O3 -163.7(3) . . . 2_656 ? O1 Yb1 Li1 O3 -73.0(3) . . . . ? O1 Yb1 Li1 O3 107.0(3) 2_656 . . . ? N1 Yb1 Li1 O3 177.1(3) 2_656 . . . ? N1 Yb1 Li1 O3 -2.9(3) . . . . ? O2 Yb1 Li1 O3 65.8(3) . . . . ? O2 Yb1 Li1 O3 -114.2(3) 2_656 . . . ? C1 Yb1 Li1 O3 -66.4(3) . . . . ? C1 Yb1 Li1 O3 113.6(3) 2_656 . . . ? C8 Yb1 Li1 O3 -163.7(3) 2_656 . . . ? C8 Yb1 Li1 O3 16.3(3) . . . . ? O1 Yb1 Li1 O1 180.000(1) . . . 2_656 ? N1 Yb1 Li1 O1 70.16(19) 2_656 . . 2_656 ? N1 Yb1 Li1 O1 -109.84(19) . . . 2_656 ? O2 Yb1 Li1 O1 -41.17(19) . . . 2_656 ? O2 Yb1 Li1 O1 138.83(19) 2_656 . . 2_656 ? C1 Yb1 Li1 O1 -173.42(19) . . . 2_656 ? C1 Yb1 Li1 O1 6.58(19) 2_656 . . 2_656 ? C8 Yb1 Li1 O1 89.34(18) 2_656 . . 2_656 ? C8 Yb1 Li1 O1 -90.66(18) . . . 2_656 ? O1 Yb1 Li1 O1 180.000(1) 2_656 . . . ? N1 Yb1 Li1 O1 -109.84(19) 2_656 . . . ? N1 Yb1 Li1 O1 70.16(19) . . . . ? O2 Yb1 Li1 O1 138.83(19) . . . . ? O2 Yb1 Li1 O1 -41.17(19) 2_656 . . . ? C1 Yb1 Li1 O1 6.58(19) . . . . ? C1 Yb1 Li1 O1 -173.42(19) 2_656 . . . ? C8 Yb1 Li1 O1 -90.66(18) 2_656 . . . ? C8 Yb1 Li1 O1 89.34(18) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.462 _refine_diff_density_min -1.247 _refine_diff_density_rms 0.126 _database_code_depnum_ccdc_archive 'CCDC 932400' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H86 Cl2 Li2 N3 O4 Si2 Y' _chemical_formula_sum 'C56 H86 Cl2 Li2 N3 O4 Si2 Y' _chemical_formula_weight 1095.15 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41 c d' _symmetry_space_group_name_Hall 'I 4bw -2c' _symmetry_Int_Tables_number 110 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/2, z+1/4' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x, z+3/4' '-x, y, z+1/2' 'y, x+1/2, z+3/4' 'x+1/2, -y+1/2, z' '-y+1/2, -x, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1, z+3/4' '-x+1, -y+1, z+1' 'y+1, -x+1/2, z+5/4' '-x+1/2, y+1/2, z+1' 'y+1/2, x+1, z+5/4' 'x+1, -y+1, z+1/2' '-y+1, -x+1/2, z+3/4' _cell_length_a 21.534(2) _cell_length_b 21.534(2) _cell_length_c 26.604(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12337.0(19) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 18280 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4656 _exptl_absorpt_coefficient_mu 1.113 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.571 _exptl_absorpt_correction_T_max 0.811 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22948 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_unetI/netI 0.0528 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5746 _reflns_number_gt 4553 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Their O2-C25,O2-C25', O2-C28,O2-C28',C26-C27,C25-C26,C27-C28,C27'-C28',C25'-C26', C26'-C27' and C27'-C28' distances were constrained. ; _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^)+(0.0907P)^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 SHELXL _refine_ls_extinction_coef 0.0036(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.030(13) _refine_ls_number_reflns 5746 _refine_ls_number_parameters 316 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1693 _refine_ls_wR_factor_gt 0.1572 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.100 _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 Y1 Y 0.5000 0.5000 0.12502(6) 0.04106(19) Uani 1 2 d S . . Cl1 Cl 0.60508(10) 0.83133(8) 0.10539(8) 0.1023(7) Uani 1 1 d . B . Si1 Si 0.51727(8) 0.43263(8) 0.00893(6) 0.0654(4) Uani 1 1 d . B . O1 O 0.40084(15) 0.50582(13) 0.14888(13) 0.0474(7) Uani 1 1 d . . . O2 O 0.6343(2) 0.5745(2) 0.25515(16) 0.0889(14) Uani 1 1 d D . . N1 N 0.50807(17) 0.5888(2) 0.17619(16) 0.0484(9) Uani 1 1 d . . . N2 N 0.5000 0.5000 0.0403(3) 0.0512(17) Uani 1 2 d S . . C1 C 0.3666(2) 0.5562(2) 0.16263(15) 0.0454(10) Uani 1 1 d . . . C2 C 0.3051(2) 0.5668(2) 0.14421(17) 0.0456(10) Uani 1 1 d . . . C3 C 0.2759(2) 0.6213(2) 0.15960(18) 0.0542(12) Uani 1 1 d . . . H3 H 0.2359 0.6296 0.1472 0.065 Uiso 1 1 calc R . . C4 C 0.3026(2) 0.6646(2) 0.19250(19) 0.0544(11) Uani 1 1 d . A . C5 C 0.3607(2) 0.6521(2) 0.20963(19) 0.0522(12) Uani 1 1 d . A . H5 H 0.3794 0.6804 0.2318 0.063 Uiso 1 1 calc R . . C6 C 0.3938(2) 0.5993(2) 0.19594(18) 0.0463(11) Uani 1 1 d . . . C7 C 0.2733(2) 0.5200(2) 0.11029(19) 0.0539(12) Uani 1 1 d . . . C8 C 0.3085(3) 0.5093(3) 0.0613(2) 0.0666(15) Uani 1 1 d . . . H8A H 0.3050 0.5459 0.0402 0.100 Uiso 1 1 calc R . . H8B H 0.2909 0.4738 0.0439 0.100 Uiso 1 1 calc R . . H8C H 0.3519 0.5014 0.0686 0.100 Uiso 1 1 calc R . . C9 C 0.2659(3) 0.4561(3) 0.1366(3) 0.0776(18) Uani 1 1 d . . . H9A H 0.3065 0.4402 0.1456 0.116 Uiso 1 1 calc R . . H9B H 0.2456 0.4273 0.1140 0.116 Uiso 1 1 calc R . . H9C H 0.2410 0.4611 0.1667 0.116 Uiso 1 1 calc R . . C10 C 0.2078(3) 0.5402(3) 0.0949(2) 0.0661(15) Uani 1 1 d . . . H10A H 0.1825 0.5457 0.1248 0.099 Uiso 1 1 calc R . . H10B H 0.1894 0.5086 0.0737 0.099 Uiso 1 1 calc R . . H10C H 0.2101 0.5791 0.0766 0.099 Uiso 1 1 calc R . . C11 C 0.2677(3) 0.7249(3) 0.2057(3) 0.0688(16) Uani 1 1 d . . . C12 C 0.3087(6) 0.7736(7) 0.2311(5) 0.069(3) Uiso 0.50 1 d P A 1 C12' C 0.2975(7) 0.7557(7) 0.2531(6) 0.080(3) Uiso 0.50 1 d P A 2 C13 C 0.2558(4) 0.7603(4) 0.1560(5) 0.102(3) Uani 1 1 d . A . H13A H 0.2336 0.7985 0.1630 0.154 Uiso 1 1 calc R . . H13B H 0.2312 0.7346 0.1336 0.154 Uiso 1 1 calc R . . H13C H 0.2952 0.7699 0.1401 0.154 Uiso 1 1 calc R . . C14 C 0.2042(4) 0.7097(4) 0.2286(3) 0.100(3) Uani 1 1 d . A . H14A H 0.2100 0.6873 0.2599 0.149 Uiso 1 1 calc R . . H14B H 0.1806 0.6843 0.2054 0.149 Uiso 1 1 calc R . . H14C H 0.1818 0.7480 0.2351 0.149 Uiso 1 1 calc R . . C15 C 0.4582(2) 0.5870(2) 0.21536(17) 0.0510(11) Uani 1 1 d . B . H15A H 0.4679 0.6179 0.2412 0.061 Uiso 1 1 calc R . . H15B H 0.4588 0.5461 0.2314 0.061 Uiso 1 1 calc R . . C16 C 0.5297(2) 0.6473(2) 0.16246(18) 0.0506(11) Uani 1 1 d . B . C17 C 0.5113(3) 0.7039(3) 0.1836(2) 0.0617(14) Uani 1 1 d . . . H17 H 0.4821 0.7037 0.2099 0.074 Uiso 1 1 calc R B . C18 C 0.5348(3) 0.7599(3) 0.1670(2) 0.0674(14) Uani 1 1 d . B . H18 H 0.5218 0.7973 0.1820 0.081 Uiso 1 1 calc R . . C19 C 0.5775(3) 0.7607(3) 0.1284(2) 0.0702(15) Uani 1 1 d . . . C20 C 0.5976(3) 0.7052(3) 0.1071(2) 0.0775(17) Uani 1 1 d . B . H20 H 0.6271 0.7055 0.0810 0.093 Uiso 1 1 calc R . . C21 C 0.5742(2) 0.6502(3) 0.1246(2) 0.0648(14) Uani 1 1 d . . . H21 H 0.5887 0.6129 0.1104 0.078 Uiso 1 1 calc R B . C22 C 0.4462(3) 0.3933(3) -0.0152(2) 0.089(2) Uani 1 1 d . . . H22A H 0.4157 0.3903 0.0115 0.134 Uiso 1 1 calc R B . H22B H 0.4568 0.3520 -0.0269 0.134 Uiso 1 1 calc R . . H22C H 0.4290 0.4172 -0.0428 0.134 Uiso 1 1 calc R . . C23 C 0.5599(3) 0.3764(3) 0.0508(2) 0.0687(14) Uani 1 1 d . . . H23A H 0.5995 0.3942 0.0606 0.103 Uiso 1 1 calc R B . H23B H 0.5670 0.3379 0.0328 0.103 Uiso 1 1 calc R . . H23C H 0.5352 0.3682 0.0806 0.103 Uiso 1 1 calc R . . C24 C 0.5696(4) 0.4437(4) -0.0471(2) 0.097(2) Uani 1 1 d . . . H24A H 0.5503 0.4723 -0.0705 0.145 Uiso 1 1 calc R B . H24B H 0.5763 0.4040 -0.0635 0.145 Uiso 1 1 calc R . . H24C H 0.6091 0.4604 -0.0360 0.145 Uiso 1 1 calc R . . C25 C 0.6100(6) 0.6245(6) 0.2848(5) 0.078(2) Uiso 0.50 1 d PD B 1 C26 C 0.6521(6) 0.6361(6) 0.3274(5) 0.078(2) Uiso 0.50 1 d PD B 1 C27 C 0.6873(7) 0.5748(6) 0.3290(4) 0.078(2) Uiso 0.50 1 d PD B 1 C28 C 0.6955(4) 0.5599(7) 0.2737(4) 0.078(2) Uiso 0.50 1 d PD B 1 C25' C 0.5990(8) 0.5981(9) 0.2965(5) 0.114(3) Uiso 0.50 1 d PD B 2 C26' C 0.6456(8) 0.6080(10) 0.3374(7) 0.114(3) Uiso 0.50 1 d PD B 2 C27' C 0.7086(8) 0.5885(8) 0.3157(7) 0.114(3) Uiso 0.50 1 d PD B 2 C28' C 0.6816(7) 0.5409(7) 0.2805(6) 0.114(3) Uiso 0.50 1 d PD B 2 Li1 Li 0.5972(4) 0.5610(5) 0.1932(4) 0.068(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 Y1 0.0423(3) 0.0378(3) 0.0431(3) 0.000 0.000 0.0006(2) Cl1 0.0998(14) 0.0767(11) 0.1304(16) 0.0133(10) -0.0042(11) -0.0337(10) Si1 0.0764(10) 0.0694(10) 0.0504(7) -0.0115(7) 0.0073(8) -0.0126(8) O1 0.0422(17) 0.0436(17) 0.0564(18) -0.0017(14) 0.0036(15) 0.0058(13) O2 0.080(3) 0.113(3) 0.074(2) -0.031(2) -0.023(2) 0.034(3) N1 0.041(2) 0.049(2) 0.056(2) -0.0112(19) 0.0005(17) 0.0014(17) N2 0.059(4) 0.055(4) 0.039(3) 0.000 0.000 -0.011(3) C1 0.047(3) 0.045(2) 0.044(2) 0.0019(19) 0.003(2) 0.004(2) C2 0.043(2) 0.043(2) 0.051(2) 0.004(2) 0.0010(19) 0.002(2) C3 0.046(3) 0.058(3) 0.059(3) -0.002(2) -0.005(2) 0.000(2) C4 0.044(3) 0.057(3) 0.062(3) -0.008(2) 0.005(2) 0.011(2) C5 0.051(3) 0.053(3) 0.053(3) -0.010(2) -0.003(2) 0.001(2) C6 0.040(2) 0.053(3) 0.046(2) -0.002(2) -0.001(2) 0.005(2) C7 0.044(3) 0.054(3) 0.064(3) 0.001(2) -0.008(2) 0.000(2) C8 0.066(4) 0.069(4) 0.065(3) -0.010(3) -0.005(3) 0.002(3) C9 0.068(4) 0.060(3) 0.105(5) 0.013(3) -0.024(3) -0.012(3) C10 0.058(3) 0.063(3) 0.078(3) -0.011(3) -0.019(3) 0.000(3) C11 0.059(3) 0.056(3) 0.091(4) -0.008(3) -0.003(3) 0.006(3) C13 0.106(6) 0.069(4) 0.133(8) 0.025(5) 0.023(5) 0.019(4) C14 0.097(5) 0.085(5) 0.117(6) -0.005(4) 0.041(5) 0.033(5) C15 0.050(3) 0.055(3) 0.049(2) -0.011(2) -0.005(2) 0.004(2) C16 0.038(2) 0.049(3) 0.065(3) -0.013(2) -0.012(2) -0.005(2) C17 0.059(3) 0.061(3) 0.065(3) -0.016(3) 0.000(3) 0.001(3) C18 0.073(4) 0.054(3) 0.075(3) -0.008(3) -0.002(3) -0.002(3) C19 0.065(3) 0.059(3) 0.086(4) 0.008(3) -0.015(3) -0.017(3) C20 0.069(4) 0.079(4) 0.084(4) -0.023(3) 0.012(3) -0.023(3) C21 0.053(3) 0.061(3) 0.080(3) -0.021(3) 0.008(3) -0.009(2) C22 0.106(5) 0.088(5) 0.073(3) -0.024(3) -0.004(4) -0.030(4) C23 0.075(4) 0.053(3) 0.079(3) -0.008(3) 0.013(3) -0.003(3) C24 0.112(6) 0.114(6) 0.064(4) 0.000(4) 0.029(4) -0.005(5) Li1 0.052(5) 0.068(6) 0.084(6) -0.029(5) -0.004(4) 0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O1 2.231(3) . ? Y1 O1 2.231(3) 11_554 ? Y1 N2 2.254(7) . ? Y1 N1 2.354(4) . ? Y1 N1 2.354(4) 11_554 ? Y1 Li1 3.066(9) . ? Y1 Li1 3.066(9) 11_554 ? Y1 Si1 3.433(2) 11_554 ? Cl1 C19 1.744(6) . ? Si1 N2 1.715(4) . ? Si1 C22 1.864(7) . ? Si1 C23 1.884(6) . ? Si1 C24 1.883(6) . ? O1 C1 1.362(5) . ? O1 Li1 1.861(9) 11_554 ? O2 C28' 1.420(9) . ? O2 C25' 1.431(9) . ? O2 C25 1.433(8) . ? O2 C28 1.441(8) . ? O2 Li1 1.853(10) . ? N1 C16 1.392(7) . ? N1 C15 1.497(6) . ? N1 Li1 2.061(10) . ? N2 Si1 1.715(4) 11_554 ? C1 C6 1.409(6) . ? C1 C2 1.431(6) . ? C1 Li1 2.765(10) 11_554 ? C2 C3 1.393(7) . ? C2 C7 1.517(7) . ? C3 C4 1.402(7) . ? C3 H3 0.9400 . ? C4 C5 1.357(7) . ? C4 C11 1.541(8) . ? C5 C6 1.391(7) . ? C5 H5 0.9400 . ? C6 C15 1.504(7) . ? C7 C8 1.525(8) . ? C7 C10 1.532(7) . ? C7 C9 1.551(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.527(14) . ? C11 C14 1.532(10) . ? C11 C13 1.549(12) . ? C11 C12' 1.562(15) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C21 1.393(7) . ? C16 C17 1.400(7) . ? C16 Li1 2.498(11) . ? C17 C18 1.381(8) . ? C17 H17 0.9400 . ? C18 C19 1.378(8) . ? C18 H18 0.9400 . ? C19 C20 1.393(8) . ? C20 C21 1.368(8) . ? C20 H20 0.9400 . ? C21 Li1 2.697(13) . ? C21 H21 0.9400 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C26 1.473(14) . ? C26 C27 1.521(9) . ? C27 C28 1.516(9) . ? C25' C26' 1.495(17) . ? C26' C27' 1.533(16) . ? C27' C28' 1.504(9) . ? Li1 O1 1.861(9) 11_554 ? Li1 C1 2.765(10) 11_554 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Y1 O1 146.9(2) . 11_554 ? O1 Y1 N2 106.53(10) . . ? O1 Y1 N2 106.53(10) 11_554 . ? O1 Y1 N1 81.98(13) . . ? O1 Y1 N1 79.07(12) 11_554 . ? N2 Y1 N1 125.33(12) . . ? O1 Y1 N1 79.07(12) . 11_554 ? O1 Y1 N1 81.98(13) 11_554 11_554 ? N2 Y1 N1 125.33(12) . 11_554 ? N1 Y1 N1 109.3(2) . 11_554 ? O1 Y1 Li1 117.4(2) . . ? O1 Y1 Li1 37.09(19) 11_554 . ? N2 Y1 Li1 126.3(2) . . ? N1 Y1 Li1 42.2(2) . . ? N1 Y1 Li1 93.2(2) 11_554 . ? O1 Y1 Li1 37.09(19) . 11_554 ? O1 Y1 Li1 117.4(2) 11_554 11_554 ? N2 Y1 Li1 126.3(2) . 11_554 ? N1 Y1 Li1 93.2(2) . 11_554 ? N1 Y1 Li1 42.2(2) 11_554 11_554 ? Li1 Y1 Li1 107.4(4) . 11_554 ? O1 Y1 Si1 97.39(10) . 11_554 ? O1 Y1 Si1 112.54(10) 11_554 11_554 ? N2 Y1 Si1 25.87(3) . 11_554 ? N1 Y1 Si1 100.66(12) . 11_554 ? N1 Y1 Si1 148.84(12) 11_554 11_554 ? Li1 Y1 Si1 115.2(2) . 11_554 ? Li1 Y1 Si1 129.78(18) 11_554 11_554 ? N2 Si1 C22 112.0(3) . . ? N2 Si1 C23 111.2(3) . . ? C22 Si1 C23 108.2(3) . . ? N2 Si1 C24 114.1(3) . . ? C22 Si1 C24 106.1(3) . . ? C23 Si1 C24 104.9(4) . . ? C1 O1 Li1 117.3(4) . 11_554 ? C1 O1 Y1 129.7(3) . . ? Li1 O1 Y1 96.6(3) 11_554 . ? C28' O2 C25' 101.4(11) . . ? C28' O2 C25 112.6(9) . . ? C25' O2 C25 27.9(9) . . ? C28' O2 C28 21.7(9) . . ? C25' O2 C28 107.4(9) . . ? C25 O2 C28 108.0(8) . . ? C28' O2 Li1 130.6(8) . . ? C25' O2 Li1 120.7(8) . . ? C25 O2 Li1 116.7(6) . . ? C28 O2 Li1 131.6(6) . . ? C16 N1 C15 116.5(4) . . ? C16 N1 Li1 90.5(4) . . ? C15 N1 Li1 120.5(4) . . ? C16 N1 Y1 127.5(3) . . ? C15 N1 Y1 109.2(3) . . ? Li1 N1 Y1 87.7(3) . . ? Si1 N2 Si1 121.7(4) . 11_554 ? Si1 N2 Y1 119.1(2) . . ? Si1 N2 Y1 119.1(2) 11_554 . ? O1 C1 C6 117.9(4) . . ? O1 C1 C2 122.4(4) . . ? C6 C1 C2 119.7(4) . . ? O1 C1 Li1 36.8(3) . 11_554 ? C6 C1 Li1 107.3(4) . 11_554 ? C2 C1 Li1 120.5(4) . 11_554 ? C3 C2 C1 116.8(4) . . ? C3 C2 C7 122.2(4) . . ? C1 C2 C7 121.0(4) . . ? C2 C3 C4 124.0(5) . . ? C2 C3 H3 118.0 . . ? C4 C3 H3 118.0 . . ? C5 C4 C3 117.0(5) . . ? C5 C4 C11 122.8(5) . . ? C3 C4 C11 120.2(4) . . ? C4 C5 C6 123.2(5) . . ? C4 C5 H5 118.4 . . ? C6 C5 H5 118.4 . . ? C5 C6 C1 119.3(4) . . ? C5 C6 C15 121.8(4) . . ? C1 C6 C15 118.9(4) . . ? C2 C7 C8 112.6(4) . . ? C2 C7 C10 112.6(4) . . ? C8 C7 C10 105.8(4) . . ? C2 C7 C9 111.5(4) . . ? C8 C7 C9 107.7(5) . . ? C10 C7 C9 106.1(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C14 119.1(8) . . ? C12 C11 C4 113.4(7) . . ? C14 C11 C4 110.3(5) . . ? C12 C11 C13 97.8(7) . . ? C14 C11 C13 107.3(6) . . ? C4 C11 C13 107.5(6) . . ? C12 C11 C12' 27.7(6) . . ? C14 C11 C12' 97.9(8) . . ? C4 C11 C12' 109.9(7) . . ? C13 C11 C12' 123.3(8) . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C6 114.7(4) . . ? N1 C15 H15A 108.6 . . ? C6 C15 H15A 108.6 . . ? N1 C15 H15B 108.6 . . ? C6 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? N1 C16 C21 117.4(4) . . ? N1 C16 C17 126.0(5) . . ? C21 C16 C17 116.6(5) . . ? N1 C16 Li1 55.6(3) . . ? C21 C16 Li1 82.5(4) . . ? C17 C16 Li1 132.9(4) . . ? C18 C17 C16 121.8(5) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C19 C18 C17 119.6(5) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 120.0(5) . . ? C18 C19 Cl1 120.0(5) . . ? C20 C19 Cl1 120.0(5) . . ? C21 C20 C19 119.4(6) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C20 C21 C16 122.5(5) . . ? C20 C21 Li1 141.1(5) . . ? C16 C21 Li1 66.7(4) . . ? C20 C21 H21 118.7 . . ? C16 C21 H21 118.7 . . ? Li1 C21 H21 66.6 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O2 C25 C26 109.0(9) . . ? C25 C26 C27 100.4(10) . . ? C28 C27 C26 102.4(10) . . ? O2 C28 C27 100.3(9) . . ? O2 C25' C26' 104.7(12) . . ? C25' C26' C27' 106.3(14) . . ? C28' C27' C26' 94.6(14) . . ? O2 C28' C27' 103.1(12) . . ? O2 Li1 O1 132.4(6) . 11_554 ? O2 Li1 N1 123.5(5) . . ? O1 Li1 N1 96.1(4) 11_554 . ? O2 Li1 C16 115.2(5) . . ? O1 Li1 C16 112.4(5) 11_554 . ? N1 Li1 C16 33.9(2) . . ? O2 Li1 C21 124.7(5) . . ? O1 Li1 C21 97.2(4) 11_554 . ? N1 Li1 C21 58.2(3) . . ? C16 Li1 C21 30.8(2) . . ? O2 Li1 C1 106.5(5) . 11_554 ? O1 Li1 C1 26.0(2) 11_554 11_554 ? N1 Li1 C1 117.6(4) . 11_554 ? C16 Li1 C1 138.3(4) . 11_554 ? C21 Li1 C1 120.2(4) . 11_554 ? O2 Li1 Y1 152.6(5) . . ? O1 Li1 Y1 46.3(2) 11_554 . ? N1 Li1 Y1 50.1(2) . . ? C16 Li1 Y1 74.2(3) . . ? C21 Li1 Y1 77.2(3) . . ? C1 Li1 Y1 68.1(2) 11_554 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Y1 O1 C1 83.2(4) 11_554 . . . ? N2 Y1 O1 C1 -96.8(4) . . . . ? N1 Y1 O1 C1 27.8(4) . . . . ? N1 Y1 O1 C1 139.4(4) 11_554 . . . ? Li1 Y1 O1 C1 51.4(4) . . . . ? Li1 Y1 O1 C1 134.1(5) 11_554 . . . ? Si1 Y1 O1 C1 -72.0(4) 11_554 . . . ? O1 Y1 O1 Li1 -50.8(4) 11_554 . . 11_554 ? N2 Y1 O1 Li1 129.2(4) . . . 11_554 ? N1 Y1 O1 Li1 -106.3(4) . . . 11_554 ? N1 Y1 O1 Li1 5.3(4) 11_554 . . 11_554 ? Li1 Y1 O1 Li1 -82.6(6) . . . 11_554 ? Si1 Y1 O1 Li1 153.9(4) 11_554 . . 11_554 ? O1 Y1 N1 C16 -123.1(4) . . . . ? O1 Y1 N1 C16 84.1(4) 11_554 . . . ? N2 Y1 N1 C16 -18.5(4) . . . . ? N1 Y1 N1 C16 161.5(4) 11_554 . . . ? Li1 Y1 N1 C16 88.9(5) . . . . ? Li1 Y1 N1 C16 -158.5(4) 11_554 . . . ? Si1 Y1 N1 C16 -27.0(4) 11_554 . . . ? O1 Y1 N1 C15 26.5(3) . . . . ? O1 Y1 N1 C15 -126.3(3) 11_554 . . . ? N2 Y1 N1 C15 131.1(3) . . . . ? N1 Y1 N1 C15 -48.9(3) 11_554 . . . ? Li1 Y1 N1 C15 -121.6(5) . . . . ? Li1 Y1 N1 C15 -9.0(3) 11_554 . . . ? Si1 Y1 N1 C15 122.5(3) 11_554 . . . ? O1 Y1 N1 Li1 148.0(3) . . . . ? O1 Y1 N1 Li1 -4.8(3) 11_554 . . . ? N2 Y1 N1 Li1 -107.4(3) . . . . ? N1 Y1 N1 Li1 72.6(3) 11_554 . . . ? Li1 Y1 N1 Li1 112.6(4) 11_554 . . . ? Si1 Y1 N1 Li1 -115.9(3) 11_554 . . . ? C22 Si1 N2 Si1 -78.4(3) . . . 11_554 ? C23 Si1 N2 Si1 160.4(2) . . . 11_554 ? C24 Si1 N2 Si1 42.0(3) . . . 11_554 ? C22 Si1 N2 Y1 101.6(3) . . . . ? C23 Si1 N2 Y1 -19.6(2) . . . . ? C24 Si1 N2 Y1 -138.0(3) . . . . ? O1 Y1 N2 Si1 -107.73(10) . . . . ? O1 Y1 N2 Si1 72.27(10) 11_554 . . . ? N1 Y1 N2 Si1 160.44(13) . . . . ? N1 Y1 N2 Si1 -19.56(13) 11_554 . . . ? Li1 Y1 N2 Si1 107.7(2) . . . . ? Li1 Y1 N2 Si1 -72.3(2) 11_554 . . . ? Si1 Y1 N2 Si1 180.0 11_554 . . . ? O1 Y1 N2 Si1 72.27(10) . . . 11_554 ? O1 Y1 N2 Si1 -107.73(10) 11_554 . . 11_554 ? N1 Y1 N2 Si1 -19.56(13) . . . 11_554 ? N1 Y1 N2 Si1 160.44(13) 11_554 . . 11_554 ? Li1 Y1 N2 Si1 -72.3(2) . . . 11_554 ? Li1 Y1 N2 Si1 107.7(2) 11_554 . . 11_554 ? Li1 O1 C1 C6 81.6(6) 11_554 . . . ? Y1 O1 C1 C6 -45.0(5) . . . . ? Li1 O1 C1 C2 -98.9(5) 11_554 . . . ? Y1 O1 C1 C2 134.5(4) . . . . ? Y1 O1 C1 Li1 -126.6(6) . . . 11_554 ? O1 C1 C2 C3 -177.6(4) . . . . ? C6 C1 C2 C3 1.9(6) . . . . ? Li1 C1 C2 C3 139.1(4) 11_554 . . . ? O1 C1 C2 C7 3.4(6) . . . . ? C6 C1 C2 C7 -177.1(4) . . . . ? Li1 C1 C2 C7 -39.9(6) 11_554 . . . ? C1 C2 C3 C4 -1.6(7) . . . . ? C7 C2 C3 C4 177.3(5) . . . . ? C2 C3 C4 C5 0.6(8) . . . . ? C2 C3 C4 C11 177.6(5) . . . . ? C3 C4 C5 C6 0.2(8) . . . . ? C11 C4 C5 C6 -176.7(5) . . . . ? C4 C5 C6 C1 0.1(8) . . . . ? C4 C5 C6 C15 179.6(5) . . . . ? O1 C1 C6 C5 178.3(4) . . . . ? C2 C1 C6 C5 -1.2(7) . . . . ? Li1 C1 C6 C5 -143.4(4) 11_554 . . . ? O1 C1 C6 C15 -1.1(6) . . . . ? C2 C1 C6 C15 179.3(4) . . . . ? Li1 C1 C6 C15 37.2(5) 11_554 . . . ? C3 C2 C7 C8 120.6(5) . . . . ? C1 C2 C7 C8 -60.5(6) . . . . ? C3 C2 C7 C10 1.0(6) . . . . ? C1 C2 C7 C10 179.9(4) . . . . ? C3 C2 C7 C9 -118.2(5) . . . . ? C1 C2 C7 C9 60.7(6) . . . . ? C5 C4 C11 C12 11.0(10) . . . . ? C3 C4 C11 C12 -165.9(7) . . . . ? C5 C4 C11 C14 -125.4(6) . . . . ? C3 C4 C11 C14 57.7(8) . . . . ? C5 C4 C11 C13 117.9(6) . . . . ? C3 C4 C11 C13 -59.0(7) . . . . ? C5 C4 C11 C12' -18.6(10) . . . . ? C3 C4 C11 C12' 164.5(8) . . . . ? C16 N1 C15 C6 81.0(5) . . . . ? Li1 N1 C15 C6 -171.2(4) . . . . ? Y1 N1 C15 C6 -72.3(4) . . . . ? C5 C6 C15 N1 -113.6(5) . . . . ? C1 C6 C15 N1 65.9(6) . . . . ? C15 N1 C16 C21 -177.4(4) . . . . ? Li1 N1 C16 C21 57.8(5) . . . . ? Y1 N1 C16 C21 -29.7(6) . . . . ? C15 N1 C16 C17 3.3(7) . . . . ? Li1 N1 C16 C17 -121.5(5) . . . . ? Y1 N1 C16 C17 151.0(4) . . . . ? C15 N1 C16 Li1 124.8(5) . . . . ? Y1 N1 C16 Li1 -87.5(4) . . . . ? N1 C16 C17 C18 -179.1(5) . . . . ? C21 C16 C17 C18 1.6(8) . . . . ? Li1 C16 C17 C18 107.0(7) . . . . ? C16 C17 C18 C19 0.3(9) . . . . ? C17 C18 C19 C20 -1.4(9) . . . . ? C17 C18 C19 Cl1 177.3(5) . . . . ? C18 C19 C20 C21 0.7(9) . . . . ? Cl1 C19 C20 C21 -178.0(5) . . . . ? C19 C20 C21 C16 1.2(9) . . . . ? C19 C20 C21 Li1 -91.2(9) . . . . ? N1 C16 C21 C20 178.3(5) . . . . ? C17 C16 C21 C20 -2.3(8) . . . . ? Li1 C16 C21 C20 -136.9(6) . . . . ? N1 C16 C21 Li1 -44.8(4) . . . . ? C17 C16 C21 Li1 134.6(5) . . . . ? C28' O2 C25 C26 14.3(16) . . . . ? C25' O2 C25 C26 85(2) . . . . ? C28 O2 C25 C26 -8.3(14) . . . . ? Li1 O2 C25 C26 -169.1(9) . . . . ? O2 C25 C26 C27 -19.5(14) . . . . ? C25 C26 C27 C28 38.7(15) . . . . ? C28' O2 C28 C27 -74(3) . . . . ? C25' O2 C28 C27 3.1(15) . . . . ? C25 O2 C28 C27 32.4(13) . . . . ? Li1 O2 C28 C27 -170.8(8) . . . . ? C26 C27 C28 O2 -44.0(15) . . . . ? C28' O2 C25' C26' 32.0(17) . . . . ? C25 O2 C25' C26' -85(2) . . . . ? C28 O2 C25' C26' 10.5(17) . . . . ? Li1 O2 C25' C26' -174.9(11) . . . . ? O2 C25' C26' C27' 0(2) . . . . ? C25' C26' C27' C28' -30(2) . . . . ? C25' O2 C28' C27' -54.0(17) . . . . ? C25 O2 C28' C27' -27.2(18) . . . . ? C28 O2 C28' C27' 55(2) . . . . ? Li1 O2 C28' C27' 156.8(10) . . . . ? C26' C27' C28' O2 50.7(18) . . . . ? C28' O2 Li1 O1 11.6(15) . . . 11_554 ? C25' O2 Li1 O1 -132.7(12) . . . 11_554 ? C25 O2 Li1 O1 -164.2(9) . . . 11_554 ? C28 O2 Li1 O1 40.5(14) . . . 11_554 ? C28' O2 Li1 N1 152.6(12) . . . . ? C25' O2 Li1 N1 8.3(14) . . . . ? C25 O2 Li1 N1 -23.2(11) . . . . ? C28 O2 Li1 N1 -178.5(9) . . . . ? C28' O2 Li1 C16 -169.5(11) . . . . ? C25' O2 Li1 C16 46.2(13) . . . . ? C25 O2 Li1 C16 14.7(10) . . . . ? C28 O2 Li1 C16 -140.6(9) . . . . ? C28' O2 Li1 C21 -135.5(11) . . . . ? C25' O2 Li1 C21 80.2(12) . . . . ? C25 O2 Li1 C21 48.7(10) . . . . ? C28 O2 Li1 C21 -106.6(10) . . . . ? C28' O2 Li1 C1 11.9(13) . . . 11_554 ? C25' O2 Li1 C1 -132.4(11) . . . 11_554 ? C25 O2 Li1 C1 -164.0(8) . . . 11_554 ? C28 O2 Li1 C1 40.7(11) . . . 11_554 ? C28' O2 Li1 Y1 85.9(15) . . . . ? C25' O2 Li1 Y1 -58.4(16) . . . . ? C25 O2 Li1 Y1 -90.0(13) . . . . ? C28 O2 Li1 Y1 114.8(12) . . . . ? C16 N1 Li1 O2 86.0(7) . . . . ? C15 N1 Li1 O2 -35.6(8) . . . . ? Y1 N1 Li1 O2 -146.5(6) . . . . ? C16 N1 Li1 O1 -121.8(5) . . . 11_554 ? C15 N1 Li1 O1 116.6(5) . . . 11_554 ? Y1 N1 Li1 O1 5.6(4) . . . 11_554 ? C15 N1 Li1 C16 -121.6(5) . . . . ? Y1 N1 Li1 C16 127.5(3) . . . . ? C16 N1 Li1 C21 -27.2(3) . . . . ? C15 N1 Li1 C21 -148.7(4) . . . . ? Y1 N1 Li1 C21 100.3(2) . . . . ? C16 N1 Li1 C1 -137.2(5) . . . 11_554 ? C15 N1 Li1 C1 101.2(5) . . . 11_554 ? Y1 N1 Li1 C1 -9.7(4) . . . 11_554 ? C16 N1 Li1 Y1 -127.5(3) . . . . ? C15 N1 Li1 Y1 111.0(4) . . . . ? N1 C16 Li1 O2 -113.1(6) . . . . ? C21 C16 Li1 O2 116.1(6) . . . . ? C17 C16 Li1 O2 -3.6(9) . . . . ? N1 C16 Li1 O1 66.0(5) . . . 11_554 ? C21 C16 Li1 O1 -64.8(5) . . . 11_554 ? C17 C16 Li1 O1 175.6(5) . . . 11_554 ? C21 C16 Li1 N1 -130.7(4) . . . . ? C17 C16 Li1 N1 109.6(6) . . . . ? N1 C16 Li1 C21 130.7(4) . . . . ? C17 C16 Li1 C21 -119.7(6) . . . . ? N1 C16 Li1 C1 64.9(6) . . . 11_554 ? C21 C16 Li1 C1 -65.9(7) . . . 11_554 ? C17 C16 Li1 C1 174.5(6) . . . 11_554 ? N1 C16 Li1 Y1 39.3(3) . . . . ? C21 C16 Li1 Y1 -91.5(3) . . . . ? C17 C16 Li1 Y1 148.8(5) . . . . ? C20 C21 Li1 O2 32.1(10) . . . . ? C16 C21 Li1 O2 -81.3(6) . . . . ? C20 C21 Li1 O1 -124.0(7) . . . 11_554 ? C16 C21 Li1 O1 122.5(5) . . . 11_554 ? C20 C21 Li1 N1 143.2(7) . . . . ? C16 C21 Li1 N1 29.8(3) . . . . ? C20 C21 Li1 C16 113.4(8) . . . . ? C20 C21 Li1 C1 -111.1(7) . . . 11_554 ? C16 C21 Li1 C1 135.4(5) . . . 11_554 ? C20 C21 Li1 Y1 -166.1(7) . . . . ? C16 C21 Li1 Y1 80.5(3) . . . . ? O1 Y1 Li1 O2 50.9(11) . . . . ? O1 Y1 Li1 O2 -100.6(11) 11_554 . . . ? N2 Y1 Li1 O2 -167.9(9) . . . . ? N1 Y1 Li1 O2 87.1(10) . . . . ? N1 Y1 Li1 O2 -28.5(10) 11_554 . . . ? Li1 Y1 Li1 O2 12.1(9) 11_554 . . . ? Si1 Y1 Li1 O2 164.7(10) 11_554 . . . ? O1 Y1 Li1 O1 151.5(2) . . . 11_554 ? N2 Y1 Li1 O1 -67.3(4) . . . 11_554 ? N1 Y1 Li1 O1 -172.2(5) . . . 11_554 ? N1 Y1 Li1 O1 72.2(3) 11_554 . . 11_554 ? Li1 Y1 Li1 O1 112.7(4) 11_554 . . 11_554 ? Si1 Y1 Li1 O1 -94.6(3) 11_554 . . 11_554 ? O1 Y1 Li1 N1 -36.2(4) . . . . ? O1 Y1 Li1 N1 172.2(5) 11_554 . . . ? N2 Y1 Li1 N1 105.0(3) . . . . ? N1 Y1 Li1 N1 -115.6(3) 11_554 . . . ? Li1 Y1 Li1 N1 -75.0(3) 11_554 . . . ? Si1 Y1 Li1 N1 77.6(3) 11_554 . . . ? O1 Y1 Li1 C16 -63.6(3) . . . . ? O1 Y1 Li1 C16 144.9(5) 11_554 . . . ? N2 Y1 Li1 C16 77.6(3) . . . . ? N1 Y1 Li1 C16 -27.4(2) . . . . ? N1 Y1 Li1 C16 -142.9(2) 11_554 . . . ? Li1 Y1 Li1 C16 -102.4(3) 11_554 . . . ? Si1 Y1 Li1 C16 50.3(3) 11_554 . . . ? O1 Y1 Li1 C21 -95.3(2) . . . . ? O1 Y1 Li1 C21 113.2(4) 11_554 . . . ? N2 Y1 Li1 C21 45.9(3) . . . . ? N1 Y1 Li1 C21 -59.0(3) . . . . ? N1 Y1 Li1 C21 -174.6(2) 11_554 . . . ? Li1 Y1 Li1 C21 -134.1(3) 11_554 . . . ? Si1 Y1 Li1 C21 18.6(3) 11_554 . . . ? O1 Y1 Li1 C1 134.46(17) . . . 11_554 ? O1 Y1 Li1 C1 -17.1(2) 11_554 . . 11_554 ? N2 Y1 Li1 C1 -84.3(3) . . . 11_554 ? N1 Y1 Li1 C1 170.7(4) . . . 11_554 ? N1 Y1 Li1 C1 55.1(2) 11_554 . . 11_554 ? Li1 Y1 Li1 C1 95.7(3) 11_554 . . 11_554 ? Si1 Y1 Li1 C1 -111.69(19) 11_554 . . 11_554 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.090 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.089 _database_code_depnum_ccdc_archive 'CCDC 932401' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H86 Cl2 Li2 N3 O4 Si2 Yb' _chemical_formula_sum 'C56 H86 Cl2 Li2 N3 O4 Si2 Yb' _chemical_formula_weight 1179.28 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41 c d' _symmetry_space_group_name_Hall 'I 4bw -2c' _symmetry_Int_Tables_number 110 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/2, z+1/4' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x, z+3/4' '-x, y, z+1/2' 'y, x+1/2, z+3/4' 'x+1/2, -y+1/2, z' '-y+1/2, -x, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1, z+3/4' '-x+1, -y+1, z+1' 'y+1, -x+1/2, z+5/4' '-x+1/2, y+1/2, z+1' 'y+1/2, x+1, z+5/4' 'x+1, -y+1, z+1/2' '-y+1, -x+1/2, z+3/4' _cell_length_a 21.4729(17) _cell_length_b 21.4729(17) _cell_length_c 26.555(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12244.3(17) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10892 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4904 _exptl_absorpt_coefficient_mu 1.697 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.314 _exptl_absorpt_correction_T_max 0.525 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17999 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_unetI/netI 0.0389 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5943 _reflns_number_gt 4447 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Their C25'-C26',C26'- C27', C27'-C28',C27-C28,C25-C26,C26-C27,O2-C25,O2-C25',O2-C28 and O2-C28' distances were constrained. ; _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^)+(0.0828P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(4) _refine_ls_number_reflns 5943 _refine_ls_number_parameters 315 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1398 _refine_ls_wR_factor_gt 0.1266 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.012 _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 Yb1 Yb 0.5000 0.0000 0.87450(12) 0.03290(12) Uani 1 2 d S . . Cl1 Cl 0.39497(10) -0.33099(9) 0.89520(8) 0.0916(6) Uani 1 1 d . B . Si1 Si 0.48277(9) 0.06730(8) 0.99000(6) 0.0569(4) Uani 1 1 d . B . O1 O 0.59828(17) -0.00617(14) 0.85266(16) 0.0391(8) Uani 1 1 d . . . O2 O 0.3649(2) -0.0738(2) 0.74596(16) 0.0815(14) Uani 1 1 d D . . N1 N 0.49159(19) -0.0879(2) 0.82457(18) 0.0435(11) Uani 1 1 d . . . N2 N 0.5000 0.0000 0.9577(4) 0.039(2) Uani 1 2 d S . . C1 C 0.6329(2) -0.0564(2) 0.83871(17) 0.0375(11) Uani 1 1 d . . . C2 C 0.6948(2) -0.0666(2) 0.85677(18) 0.0398(11) Uani 1 1 d . . . C3 C 0.7245(3) -0.1211(3) 0.84116(19) 0.0483(12) Uani 1 1 d . . . H3 H 0.7647 -0.1293 0.8536 0.058 Uiso 1 1 calc R . . C4 C 0.6979(2) -0.1641(3) 0.8080(2) 0.0461(12) Uani 1 1 d . A . C5 C 0.6389(3) -0.1510(3) 0.7905(2) 0.0468(13) Uani 1 1 d . A . H5 H 0.6201 -0.1788 0.7678 0.056 Uiso 1 1 calc R . . C6 C 0.6065(2) -0.0989(2) 0.8050(2) 0.0399(12) Uani 1 1 d . . . C7 C 0.7267(2) -0.0199(3) 0.8916(2) 0.0455(12) Uani 1 1 d . . . C8 C 0.6918(3) -0.0092(3) 0.9402(2) 0.0610(17) Uani 1 1 d . . . H8A H 0.6943 -0.0463 0.9609 0.092 Uiso 1 1 calc R . . H8B H 0.6484 -0.0002 0.9328 0.092 Uiso 1 1 calc R . . H8C H 0.7101 0.0256 0.9580 0.092 Uiso 1 1 calc R . . C9 C 0.7334(3) 0.0445(3) 0.8645(3) 0.0683(18) Uani 1 1 d . . . H9A H 0.6925 0.0596 0.8549 0.102 Uiso 1 1 calc R . . H9B H 0.7590 0.0397 0.8347 0.102 Uiso 1 1 calc R . . H9C H 0.7528 0.0741 0.8872 0.102 Uiso 1 1 calc R . . C10 C 0.7931(3) -0.0400(3) 0.9060(2) 0.0568(14) Uani 1 1 d . . . H10A H 0.8176 -0.0462 0.8758 0.085 Uiso 1 1 calc R . . H10B H 0.7914 -0.0786 0.9250 0.085 Uiso 1 1 calc R . . H10C H 0.8123 -0.0078 0.9265 0.085 Uiso 1 1 calc R . . C11 C 0.7326(3) -0.2246(3) 0.7948(3) 0.0611(17) Uani 1 1 d . . . C12 C 0.6907(7) -0.2743(7) 0.7693(6) 0.060(3) Uiso 0.50 1 d P A 1 C12' C 0.7005(7) -0.2566(7) 0.7494(6) 0.069(4) Uiso 0.50 1 d P A 2 C13 C 0.7438(5) -0.2619(5) 0.8431(6) 0.095(4) Uani 1 1 d . A . H13A H 0.7669 -0.2994 0.8352 0.143 Uiso 1 1 calc R . . H13B H 0.7041 -0.2730 0.8580 0.143 Uiso 1 1 calc R . . H13C H 0.7674 -0.2368 0.8667 0.143 Uiso 1 1 calc R . . C14 C 0.7972(4) -0.2091(4) 0.7723(3) 0.086(3) Uani 1 1 d . A . H14A H 0.7920 -0.1844 0.7420 0.129 Uiso 1 1 calc R . . H14B H 0.8189 -0.2474 0.7641 0.129 Uiso 1 1 calc R . . H14C H 0.8214 -0.1857 0.7967 0.129 Uiso 1 1 calc R . . C15 C 0.5418(2) -0.0860(3) 0.78455(18) 0.0432(12) Uani 1 1 d . B . H15A H 0.5416 -0.0449 0.7686 0.052 Uiso 1 1 calc R . . H15B H 0.5321 -0.1170 0.7586 0.052 Uiso 1 1 calc R . . C16 C 0.4705(2) -0.1456(2) 0.83818(18) 0.0430(12) Uani 1 1 d . B . C17 C 0.4885(3) -0.2026(3) 0.8163(2) 0.0510(13) Uani 1 1 d . . . H17 H 0.5175 -0.2029 0.7898 0.061 Uiso 1 1 calc R B . C18 C 0.4636(3) -0.2588(3) 0.8338(2) 0.0600(15) Uani 1 1 d . B . H18 H 0.4757 -0.2963 0.8183 0.072 Uiso 1 1 calc R . . C19 C 0.4229(3) -0.2605(3) 0.8722(2) 0.0609(16) Uani 1 1 d . . . C20 C 0.4030(3) -0.2053(3) 0.8935(2) 0.0656(17) Uani 1 1 d . B . H20 H 0.3738 -0.2060 0.9198 0.079 Uiso 1 1 calc R . . C21 C 0.4256(3) -0.1497(3) 0.8765(2) 0.0564(14) Uani 1 1 d . . . H21 H 0.4105 -0.1127 0.8910 0.068 Uiso 1 1 calc R B . C22 C 0.5539(4) 0.1072(3) 1.0144(2) 0.077(2) Uani 1 1 d . . . H22A H 0.5851 0.1091 0.9880 0.116 Uiso 1 1 calc R B . H22B H 0.5704 0.0842 1.0428 0.116 Uiso 1 1 calc R . . H22C H 0.5433 0.1491 1.0249 0.116 Uiso 1 1 calc R . . C23 C 0.4400(3) 0.1243(3) 0.9494(2) 0.0605(15) Uani 1 1 d . . . H23A H 0.3998 0.1072 0.9403 0.091 Uiso 1 1 calc R B . H23B H 0.4640 0.1322 0.9191 0.091 Uiso 1 1 calc R . . H23C H 0.4342 0.1629 0.9677 0.091 Uiso 1 1 calc R . . C24 C 0.4308(4) 0.0555(4) 1.0465(3) 0.078(2) Uani 1 1 d . . . H24A H 0.4511 0.0279 1.0703 0.118 Uiso 1 1 calc R B . H24B H 0.3917 0.0373 1.0358 0.118 Uiso 1 1 calc R . . H24C H 0.4229 0.0954 1.0625 0.118 Uiso 1 1 calc R . . C25 C 0.3896(7) -0.1254(6) 0.7178(5) 0.076(2) Uiso 0.50 1 d PD B 1 C26 C 0.3471(7) -0.1357(7) 0.6745(6) 0.076(2) Uiso 0.50 1 d PD B 1 C27 C 0.3156(8) -0.0698(7) 0.6715(4) 0.076(2) Uiso 0.50 1 d PD B 1 C28 C 0.3037(5) -0.0594(7) 0.7271(4) 0.076(2) Uiso 0.50 1 d PD B 1 C25' C 0.4001(8) -0.0999(9) 0.7049(5) 0.093(3) Uiso 0.50 1 d PD B 2 C26' C 0.3569(8) -0.1094(10) 0.6627(6) 0.093(3) Uiso 0.50 1 d PD B 2 C27' C 0.2935(8) -0.0899(8) 0.6827(6) 0.093(3) Uiso 0.50 1 d PD B 2 C28' C 0.3166(7) -0.0415(7) 0.7196(6) 0.093(3) Uiso 0.50 1 d PD B 2 Li1 Li 0.4025(4) -0.0612(5) 0.8085(4) 0.052(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 Yb1 0.03385(17) 0.03075(17) 0.0341(2) 0.000 0.000 0.00071(9) Cl1 0.0913(14) 0.0661(11) 0.1174(15) 0.0113(11) -0.0029(11) -0.0322(10) Si1 0.0676(10) 0.0580(10) 0.0451(7) -0.0104(7) 0.0079(8) -0.0109(9) O1 0.0250(17) 0.0386(19) 0.054(2) -0.0007(14) -0.0020(17) 0.0043(12) O2 0.071(3) 0.106(4) 0.068(2) -0.031(3) -0.023(2) 0.033(3) N1 0.041(2) 0.045(3) 0.044(3) -0.009(2) -0.0032(19) 0.0004(18) N2 0.047(4) 0.045(4) 0.023(4) 0.000 0.000 -0.005(2) C1 0.036(3) 0.036(3) 0.041(2) 0.002(2) 0.003(2) 0.0030(19) C2 0.034(3) 0.042(3) 0.043(3) -0.001(2) -0.001(2) 0.0044(19) C3 0.038(3) 0.053(3) 0.054(3) 0.006(2) -0.006(2) 0.004(2) C4 0.035(3) 0.054(3) 0.050(3) -0.005(3) -0.001(2) 0.009(2) C5 0.043(3) 0.052(3) 0.046(3) -0.011(2) -0.001(2) -0.001(2) C6 0.034(3) 0.041(3) 0.044(3) 0.003(2) -0.007(2) 0.007(2) C7 0.039(3) 0.040(3) 0.057(3) 0.000(3) -0.005(2) 0.002(2) C8 0.060(4) 0.068(4) 0.056(4) -0.015(3) -0.007(3) 0.011(3) C9 0.059(4) 0.051(3) 0.095(5) 0.010(3) -0.007(4) -0.013(3) C10 0.049(3) 0.053(3) 0.069(3) -0.009(3) -0.020(3) 0.006(3) C11 0.047(3) 0.049(3) 0.088(5) -0.010(3) -0.001(3) 0.005(3) C13 0.104(7) 0.079(5) 0.103(9) 0.024(6) 0.014(6) 0.023(5) C14 0.080(5) 0.089(6) 0.089(6) -0.001(4) 0.031(4) 0.030(5) C15 0.037(3) 0.048(3) 0.044(3) -0.004(2) 0.004(2) 0.006(2) C16 0.037(3) 0.041(3) 0.051(3) -0.012(2) -0.012(2) 0.002(2) C17 0.047(3) 0.050(3) 0.056(3) -0.008(3) 0.002(3) -0.003(2) C18 0.057(4) 0.051(4) 0.072(4) -0.008(3) -0.003(3) 0.001(3) C19 0.061(4) 0.048(3) 0.074(4) 0.011(3) -0.016(3) -0.017(3) C20 0.063(4) 0.060(4) 0.074(4) -0.017(3) 0.020(3) -0.026(3) C21 0.046(3) 0.059(3) 0.064(3) -0.022(3) 0.008(3) -0.004(3) C22 0.091(5) 0.079(5) 0.061(3) -0.026(4) -0.003(4) -0.023(4) C23 0.066(4) 0.051(3) 0.065(3) -0.008(3) 0.014(3) -0.001(3) C24 0.082(5) 0.091(6) 0.062(4) 0.001(4) 0.015(4) -0.011(4) Li1 0.049(5) 0.047(5) 0.060(5) -0.029(5) -0.012(4) -0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O1 2.193(4) 11_544 ? Yb1 O1 2.193(4) . ? Yb1 N2 2.209(10) . ? Yb1 N1 2.314(5) . ? Yb1 N1 2.314(5) 11_544 ? Yb1 Li1 3.031(9) . ? Yb1 Li1 3.031(9) 11_544 ? Yb1 C15 3.151(5) 11_544 ? Yb1 Si1 3.411(3) 11_544 ? Cl1 C19 1.739(6) . ? Si1 N2 1.721(5) . ? Si1 C22 1.868(7) . ? Si1 C23 1.871(7) . ? Si1 C24 1.888(7) . ? O1 C1 1.361(6) . ? O1 Li1 1.863(9) 11_544 ? O2 C28' 1.431(9) . ? O2 C25 1.438(9) . ? O2 C25' 1.440(9) . ? O2 C28 1.441(9) . ? O2 Li1 1.866(9) . ? N1 C16 1.368(7) . ? N1 C15 1.515(7) . ? N1 Li1 2.042(11) . ? N2 Si1 1.721(5) 11_544 ? C1 C6 1.397(7) . ? C1 C2 1.431(7) . ? C1 Li1 2.758(11) 11_544 ? C2 C3 1.396(7) . ? C2 C7 1.525(7) . ? C3 C4 1.398(8) . ? C3 H3 0.9400 . ? C4 C5 1.379(8) . ? C4 C11 1.539(8) . ? C5 C6 1.373(8) . ? C5 H5 0.9400 . ? C6 C15 1.516(7) . ? C7 C8 1.511(8) . ? C7 C10 1.539(7) . ? C7 C9 1.565(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C13 1.530(15) . ? C11 C14 1.546(11) . ? C11 C12 1.551(15) . ? C11 C12' 1.549(16) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C21 1.405(8) . ? C16 C17 1.409(8) . ? C17 C18 1.398(9) . ? C17 H17 0.9400 . ? C18 C19 1.345(9) . ? C18 H18 0.9400 . ? C19 C20 1.381(9) . ? C20 C21 1.365(8) . ? C20 H20 0.9400 . ? C21 H21 0.9400 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C26 1.487(15) . ? C26 C27 1.571(15) . ? C27 C28 1.517(9) . ? C25' C26' 1.469(16) . ? C26' C27' 1.520(16) . ? C27' C28' 1.510(9) . ? Li1 O1 1.863(9) 11_544 ? Li1 C1 2.758(11) 11_544 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Yb1 O1 149.3(3) 11_544 . ? O1 Yb1 N2 105.34(13) 11_544 . ? O1 Yb1 N2 105.34(13) . . ? O1 Yb1 N1 79.78(14) 11_544 . ? O1 Yb1 N1 82.78(15) . . ? N2 Yb1 N1 124.96(15) . . ? O1 Yb1 N1 82.78(15) 11_544 11_544 ? O1 Yb1 N1 79.78(14) . 11_544 ? N2 Yb1 N1 124.96(15) . 11_544 ? N1 Yb1 N1 110.1(3) . 11_544 ? O1 Yb1 Li1 37.7(2) 11_544 . ? O1 Yb1 Li1 119.1(2) . . ? N2 Yb1 Li1 125.3(2) . . ? N1 Yb1 Li1 42.3(2) . . ? N1 Yb1 Li1 94.4(3) 11_544 . ? O1 Yb1 Li1 119.1(2) 11_544 11_544 ? O1 Yb1 Li1 37.7(2) . 11_544 ? N2 Yb1 Li1 125.3(2) . 11_544 ? N1 Yb1 Li1 94.4(3) . 11_544 ? N1 Yb1 Li1 42.3(2) 11_544 11_544 ? Li1 Yb1 Li1 109.3(4) . 11_544 ? O1 Yb1 C15 59.31(14) 11_544 11_544 ? O1 Yb1 C15 96.28(16) . 11_544 ? N2 Yb1 C15 139.30(10) . 11_544 ? N1 Yb1 C15 91.25(18) . 11_544 ? N1 Yb1 C15 27.06(15) 11_544 11_544 ? Li1 Yb1 C15 67.6(2) . 11_544 ? Li1 Yb1 C15 60.3(2) 11_544 11_544 ? O1 Yb1 Si1 111.58(13) 11_544 11_544 ? O1 Yb1 Si1 96.19(13) . 11_544 ? N2 Yb1 Si1 25.94(4) . 11_544 ? N1 Yb1 Si1 100.25(14) . 11_544 ? N1 Yb1 Si1 148.48(15) 11_544 11_544 ? Li1 Yb1 Si1 114.3(2) . 11_544 ? Li1 Yb1 Si1 128.97(19) 11_544 11_544 ? C15 Yb1 Si1 163.99(11) 11_544 11_544 ? N2 Si1 C22 112.5(3) . . ? N2 Si1 C23 111.5(3) . . ? C22 Si1 C23 107.5(3) . . ? N2 Si1 C24 114.3(4) . . ? C22 Si1 C24 105.7(3) . . ? C23 Si1 C24 104.8(4) . . ? C1 O1 Li1 116.7(5) . 11_544 ? C1 O1 Yb1 130.2(3) . . ? Li1 O1 Yb1 96.4(3) 11_544 . ? C28' O2 C25 112.7(9) . . ? C28' O2 C25' 101.4(10) . . ? C25 O2 C25' 27.5(9) . . ? C28' O2 C28 20.6(9) . . ? C25 O2 C28 108.8(9) . . ? C25' O2 C28 107.5(9) . . ? C28' O2 Li1 132.8(7) . . ? C25 O2 Li1 114.5(7) . . ? C25' O2 Li1 120.2(8) . . ? C28 O2 Li1 132.3(6) . . ? C16 N1 C15 116.5(4) . . ? C16 N1 Li1 89.9(4) . . ? C15 N1 Li1 120.9(4) . . ? C16 N1 Yb1 127.8(4) . . ? C15 N1 Yb1 108.9(3) . . ? Li1 N1 Yb1 87.9(3) . . ? Si1 N2 Si1 120.2(6) 11_544 . ? Si1 N2 Yb1 119.9(3) 11_544 . ? Si1 N2 Yb1 119.9(3) . . ? O1 C1 C6 118.1(4) . . ? O1 C1 C2 122.5(4) . . ? C6 C1 C2 119.5(4) . . ? O1 C1 Li1 37.1(3) . 11_544 ? C6 C1 Li1 107.5(4) . 11_544 ? C2 C1 Li1 119.6(4) . 11_544 ? C3 C2 C1 116.9(4) . . ? C3 C2 C7 121.7(4) . . ? C1 C2 C7 121.3(4) . . ? C4 C3 C2 123.7(5) . . ? C4 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? C5 C4 C3 116.9(5) . . ? C5 C4 C11 122.7(5) . . ? C3 C4 C11 120.2(5) . . ? C6 C5 C4 122.5(5) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 C1 120.4(5) . . ? C5 C6 C15 120.7(5) . . ? C1 C6 C15 118.8(5) . . ? C8 C7 C2 113.2(4) . . ? C8 C7 C10 106.8(5) . . ? C2 C7 C10 112.5(4) . . ? C8 C7 C9 107.7(5) . . ? C2 C7 C9 110.1(5) . . ? C10 C7 C9 106.1(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C4 109.0(7) . . ? C13 C11 C14 107.2(7) . . ? C4 C11 C14 109.9(5) . . ? C13 C11 C12 95.6(9) . . ? C4 C11 C12 113.5(7) . . ? C14 C11 C12 120.1(9) . . ? C13 C11 C12' 119.4(9) . . ? C4 C11 C12' 109.6(7) . . ? C14 C11 C12' 101.3(9) . . ? C12 C11 C12' 25.5(6) . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C6 113.3(4) . . ? N1 C15 H15A 108.9 . . ? C6 C15 H15A 108.9 . . ? N1 C15 H15B 108.9 . . ? C6 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? N1 C16 C21 118.3(5) . . ? N1 C16 C17 126.0(5) . . ? C21 C16 C17 115.7(5) . . ? C18 C17 C16 120.6(6) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C17 121.5(6) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C20 119.3(6) . . ? C18 C19 Cl1 120.9(5) . . ? C20 C19 Cl1 119.8(5) . . ? C21 C20 C19 120.4(6) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C16 122.5(5) . . ? C20 C21 H21 118.8 . . ? C16 C21 H21 118.8 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O2 C25 C26 106.9(10) . . ? C25 C26 C27 99.8(11) . . ? C28 C27 C26 99.0(12) . . ? O2 C28 C27 98.8(9) . . ? O2 C25' C26' 107.5(12) . . ? C25' C26' C27' 105.1(13) . . ? C28' C27' C26' 97.0(14) . . ? O2 C28' C27' 102.9(11) . . ? O1 Li1 O2 132.0(6) 11_544 . ? O1 Li1 N1 95.4(4) 11_544 . ? O2 Li1 N1 123.4(5) . . ? O1 Li1 C1 26.2(2) 11_544 11_544 ? O2 Li1 C1 105.8(5) . 11_544 ? N1 Li1 C1 117.0(4) . 11_544 ? O1 Li1 Yb1 46.0(2) 11_544 . ? O2 Li1 Yb1 151.2(5) . . ? N1 Li1 Yb1 49.7(2) . . ? C1 Li1 Yb1 67.9(2) 11_544 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Yb1 O1 C1 -82.1(4) 11_544 . . . ? N2 Yb1 O1 C1 97.9(4) . . . . ? N1 Yb1 O1 C1 -26.4(4) . . . . ? N1 Yb1 O1 C1 -138.4(5) 11_544 . . . ? Li1 Yb1 O1 C1 -49.1(5) . . . . ? Li1 Yb1 O1 C1 -133.3(6) 11_544 . . . ? C15 Yb1 O1 C1 -116.9(4) 11_544 . . . ? Si1 Yb1 O1 C1 73.2(4) 11_544 . . . ? O1 Yb1 O1 Li1 51.2(3) 11_544 . . 11_544 ? N2 Yb1 O1 Li1 -128.8(3) . . . 11_544 ? N1 Yb1 O1 Li1 106.9(4) . . . 11_544 ? N1 Yb1 O1 Li1 -5.1(4) 11_544 . . 11_544 ? Li1 Yb1 O1 Li1 84.3(6) . . . 11_544 ? C15 Yb1 O1 Li1 16.4(4) 11_544 . . 11_544 ? Si1 Yb1 O1 Li1 -153.5(3) 11_544 . . 11_544 ? O1 Yb1 N1 C16 -83.7(4) 11_544 . . . ? O1 Yb1 N1 C16 121.7(4) . . . . ? N2 Yb1 N1 C16 18.0(5) . . . . ? N1 Yb1 N1 C16 -162.0(5) 11_544 . . . ? Li1 Yb1 N1 C16 -88.3(5) . . . . ? Li1 Yb1 N1 C16 157.6(4) 11_544 . . . ? C15 Yb1 N1 C16 -142.2(4) 11_544 . . . ? Si1 Yb1 N1 C16 26.7(4) 11_544 . . . ? O1 Yb1 N1 C15 126.7(4) 11_544 . . . ? O1 Yb1 N1 C15 -28.0(3) . . . . ? N2 Yb1 N1 C15 -131.7(3) . . . . ? N1 Yb1 N1 C15 48.3(3) 11_544 . . . ? Li1 Yb1 N1 C15 122.0(5) . . . . ? Li1 Yb1 N1 C15 7.9(4) 11_544 . . . ? C15 Yb1 N1 C15 68.2(4) 11_544 . . . ? Si1 Yb1 N1 C15 -123.0(3) 11_544 . . . ? O1 Yb1 N1 Li1 4.6(3) 11_544 . . . ? O1 Yb1 N1 Li1 -150.0(4) . . . . ? N2 Yb1 N1 Li1 106.3(3) . . . . ? N1 Yb1 N1 Li1 -73.7(3) 11_544 . . . ? Li1 Yb1 N1 Li1 -114.1(4) 11_544 . . . ? C15 Yb1 N1 Li1 -53.9(3) 11_544 . . . ? Si1 Yb1 N1 Li1 114.9(3) 11_544 . . . ? C22 Si1 N2 Si1 78.8(3) . . . 11_544 ? C23 Si1 N2 Si1 -160.3(2) . . . 11_544 ? C24 Si1 N2 Si1 -41.7(3) . . . 11_544 ? C22 Si1 N2 Yb1 -101.2(3) . . . . ? C23 Si1 N2 Yb1 19.7(2) . . . . ? C24 Si1 N2 Yb1 138.3(3) . . . . ? O1 Yb1 N2 Si1 107.95(11) 11_544 . . 11_544 ? O1 Yb1 N2 Si1 -72.05(11) . . . 11_544 ? N1 Yb1 N2 Si1 19.83(14) . . . 11_544 ? N1 Yb1 N2 Si1 -160.17(14) 11_544 . . 11_544 ? Li1 Yb1 N2 Si1 72.2(2) . . . 11_544 ? Li1 Yb1 N2 Si1 -107.8(2) 11_544 . . 11_544 ? C15 Yb1 N2 Si1 168.42(16) 11_544 . . 11_544 ? O1 Yb1 N2 Si1 -72.05(11) 11_544 . . . ? O1 Yb1 N2 Si1 107.95(11) . . . . ? N1 Yb1 N2 Si1 -160.17(14) . . . . ? N1 Yb1 N2 Si1 19.83(14) 11_544 . . . ? Li1 Yb1 N2 Si1 -107.8(2) . . . . ? Li1 Yb1 N2 Si1 72.2(2) 11_544 . . . ? C15 Yb1 N2 Si1 -11.58(16) 11_544 . . . ? Si1 Yb1 N2 Si1 180.000(3) 11_544 . . . ? Li1 O1 C1 C6 -81.9(6) 11_544 . . . ? Yb1 O1 C1 C6 44.1(6) . . . . ? Li1 O1 C1 C2 97.4(6) 11_544 . . . ? Yb1 O1 C1 C2 -136.7(4) . . . . ? Yb1 O1 C1 Li1 126.0(6) . . . 11_544 ? O1 C1 C2 C3 177.6(5) . . . . ? C6 C1 C2 C3 -3.1(7) . . . . ? Li1 C1 C2 C3 -138.9(5) 11_544 . . . ? O1 C1 C2 C7 -2.3(7) . . . . ? C6 C1 C2 C7 177.0(5) . . . . ? Li1 C1 C2 C7 41.2(6) 11_544 . . . ? C1 C2 C3 C4 2.3(8) . . . . ? C7 C2 C3 C4 -177.8(5) . . . . ? C2 C3 C4 C5 -0.4(8) . . . . ? C2 C3 C4 C11 -177.0(5) . . . . ? C3 C4 C5 C6 -0.9(8) . . . . ? C11 C4 C5 C6 175.6(6) . . . . ? C4 C5 C6 C1 0.0(8) . . . . ? C4 C5 C6 C15 179.6(5) . . . . ? O1 C1 C6 C5 -178.7(5) . . . . ? C2 C1 C6 C5 2.0(7) . . . . ? Li1 C1 C6 C5 142.5(5) 11_544 . . . ? O1 C1 C6 C15 1.8(7) . . . . ? C2 C1 C6 C15 -177.5(4) . . . . ? Li1 C1 C6 C15 -37.0(6) 11_544 . . . ? C3 C2 C7 C8 -120.8(5) . . . . ? C1 C2 C7 C8 59.1(6) . . . . ? C3 C2 C7 C10 0.4(7) . . . . ? C1 C2 C7 C10 -179.7(5) . . . . ? C3 C2 C7 C9 118.6(6) . . . . ? C1 C2 C7 C9 -61.5(6) . . . . ? C5 C4 C11 C13 -116.6(7) . . . . ? C3 C4 C11 C13 59.8(8) . . . . ? C5 C4 C11 C14 126.2(7) . . . . ? C3 C4 C11 C14 -57.4(8) . . . . ? C5 C4 C11 C12 -11.4(11) . . . . ? C3 C4 C11 C12 165.0(8) . . . . ? C5 C4 C11 C12' 15.7(10) . . . . ? C3 C4 C11 C12' -167.9(8) . . . . ? C16 N1 C15 C6 -80.7(6) . . . . ? Li1 N1 C15 C6 172.0(4) . . . . ? Yb1 N1 C15 C6 72.8(5) . . . . ? C5 C6 C15 N1 115.0(6) . . . . ? C1 C6 C15 N1 -65.5(6) . . . . ? C15 N1 C16 C21 177.6(4) . . . . ? Li1 N1 C16 C21 -57.5(5) . . . . ? Yb1 N1 C16 C21 29.9(6) . . . . ? C15 N1 C16 C17 -4.0(7) . . . . ? Li1 N1 C16 C17 120.9(6) . . . . ? Yb1 N1 C16 C17 -151.7(4) . . . . ? N1 C16 C17 C18 179.8(5) . . . . ? C21 C16 C17 C18 -1.8(8) . . . . ? C16 C17 C18 C19 -1.2(9) . . . . ? C17 C18 C19 C20 2.9(9) . . . . ? C17 C18 C19 Cl1 -177.2(5) . . . . ? C18 C19 C20 C21 -1.5(9) . . . . ? Cl1 C19 C20 C21 178.6(5) . . . . ? C19 C20 C21 C16 -1.7(9) . . . . ? N1 C16 C21 C20 -178.2(5) . . . . ? C17 C16 C21 C20 3.2(8) . . . . ? C28' O2 C25 C26 -11.4(17) . . . . ? C25' O2 C25 C26 -82(2) . . . . ? C28 O2 C25 C26 10.3(16) . . . . ? Li1 O2 C25 C26 169.5(10) . . . . ? O2 C25 C26 C27 21.6(16) . . . . ? C25 C26 C27 C28 -44.0(15) . . . . ? C28' O2 C28 C27 66(3) . . . . ? C25 O2 C28 C27 -38.7(15) . . . . ? C25' O2 C28 C27 -9.7(15) . . . . ? Li1 O2 C28 C27 167.2(9) . . . . ? C26 C27 C28 O2 50.0(15) . . . . ? C28' O2 C25' C26' -28.1(17) . . . . ? C25 O2 C25' C26' 90(3) . . . . ? C28 O2 C25' C26' -7.7(18) . . . . ? Li1 O2 C25' C26' 174.9(12) . . . . ? O2 C25' C26' C27' -3(2) . . . . ? C25' C26' C27' C28' 30.1(19) . . . . ? C25 O2 C28' C27' 22.4(18) . . . . ? C25' O2 C28' C27' 48.7(16) . . . . ? C28 O2 C28' C27' -61(2) . . . . ? Li1 O2 C28' C27' -158.7(10) . . . . ? C26' C27' C28' O2 -48.6(18) . . . . ? C28' O2 Li1 O1 -14.4(15) . . . 11_544 ? C25 O2 Li1 O1 164.5(10) . . . 11_544 ? C25' O2 Li1 O1 134.2(12) . . . 11_544 ? C28 O2 Li1 O1 -42.5(14) . . . 11_544 ? C28' O2 Li1 N1 -152.6(11) . . . . ? C25 O2 Li1 N1 26.3(12) . . . . ? C25' O2 Li1 N1 -4.0(13) . . . . ? C28 O2 Li1 N1 179.3(10) . . . . ? C28' O2 Li1 C1 -13.8(13) . . . 11_544 ? C25 O2 Li1 C1 165.1(9) . . . 11_544 ? C25' O2 Li1 C1 134.7(11) . . . 11_544 ? C28 O2 Li1 C1 -41.9(11) . . . 11_544 ? C28' O2 Li1 Yb1 -86.6(15) . . . . ? C25 O2 Li1 Yb1 92.3(14) . . . . ? C25' O2 Li1 Yb1 61.9(15) . . . . ? C28 O2 Li1 Yb1 -114.7(13) . . . . ? C16 N1 Li1 O1 122.5(5) . . . 11_544 ? C15 N1 Li1 O1 -116.3(5) . . . 11_544 ? Yb1 N1 Li1 O1 -5.4(4) . . . 11_544 ? C16 N1 Li1 O2 -87.4(7) . . . . ? C15 N1 Li1 O2 33.8(9) . . . . ? Yb1 N1 Li1 O2 144.7(6) . . . . ? C16 N1 Li1 C1 138.0(5) . . . 11_544 ? C15 N1 Li1 C1 -100.7(5) . . . 11_544 ? Yb1 N1 Li1 C1 10.2(4) . . . 11_544 ? C16 N1 Li1 Yb1 127.9(4) . . . . ? C15 N1 Li1 Yb1 -110.9(5) . . . . ? O1 Yb1 Li1 O1 -152.9(3) . . . 11_544 ? N2 Yb1 Li1 O1 67.2(4) . . . 11_544 ? N1 Yb1 Li1 O1 172.5(5) . . . 11_544 ? N1 Yb1 Li1 O1 -72.2(3) 11_544 . . 11_544 ? Li1 Yb1 Li1 O1 -112.8(4) 11_544 . . 11_544 ? C15 Yb1 Li1 O1 -68.3(3) 11_544 . . 11_544 ? Si1 Yb1 Li1 O1 94.4(3) 11_544 . . 11_544 ? O1 Yb1 Li1 O2 99.9(11) 11_544 . . . ? O1 Yb1 Li1 O2 -53.0(11) . . . . ? N2 Yb1 Li1 O2 167.1(9) . . . . ? N1 Yb1 Li1 O2 -87.6(10) . . . . ? N1 Yb1 Li1 O2 27.7(10) 11_544 . . . ? Li1 Yb1 Li1 O2 -12.9(9) 11_544 . . . ? C15 Yb1 Li1 O2 31.6(10) 11_544 . . . ? Si1 Yb1 Li1 O2 -165.7(9) 11_544 . . . ? O1 Yb1 Li1 N1 -172.5(5) 11_544 . . . ? O1 Yb1 Li1 N1 34.5(4) . . . . ? N2 Yb1 Li1 N1 -105.4(3) . . . . ? N1 Yb1 Li1 N1 115.3(4) 11_544 . . . ? Li1 Yb1 Li1 N1 74.6(3) 11_544 . . . ? C15 Yb1 Li1 N1 119.2(4) 11_544 . . . ? Si1 Yb1 Li1 N1 -78.2(3) 11_544 . . . ? O1 Yb1 Li1 C1 17.2(2) 11_544 . . 11_544 ? O1 Yb1 Li1 C1 -135.7(2) . . . 11_544 ? N2 Yb1 Li1 C1 84.4(2) . . . 11_544 ? N1 Yb1 Li1 C1 -170.2(4) . . . 11_544 ? N1 Yb1 Li1 C1 -55.0(2) 11_544 . . 11_544 ? Li1 Yb1 Li1 C1 -95.6(2) 11_544 . . 11_544 ? C15 Yb1 Li1 C1 -51.08(18) 11_544 . . 11_544 ? Si1 Yb1 Li1 C1 111.59(19) 11_544 . . 11_544 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.632 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.093 _database_code_depnum_ccdc_archive 'CCDC 932402' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H86 Br2 Li2 N3 O4 Si2 Y' _chemical_formula_sum 'C56 H86 Br2 Li2 N3 O4 Si2 Y' _chemical_formula_weight 1184.07 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41 c d' _symmetry_space_group_name_Hall 'I 4bw -2c' _symmetry_Int_Tables_number 110 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/2, z+1/4' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x, z+3/4' '-x, y, z+1/2' 'y, x+1/2, z+3/4' 'x+1/2, -y+1/2, z' '-y+1/2, -x, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1, z+3/4' '-x+1, -y+1, z+1' 'y+1, -x+1/2, z+5/4' '-x+1/2, y+1/2, z+1' 'y+1/2, x+1, z+5/4' 'x+1, -y+1, z+1/2' '-y+1, -x+1/2, z+3/4' _cell_length_a 21.645(2) _cell_length_b 21.645(2) _cell_length_c 26.471(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12402(2) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 12815 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 1.00 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4944 _exptl_absorpt_coefficient_mu 2.310 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.164 _exptl_absorpt_correction_T_max 0.372 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18106 _diffrn_reflns_av_R_equivalents 0.0734 _diffrn_reflns_av_unetI/netI 0.2505 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5973 _reflns_number_gt 3699 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Their C25'-C26',C26'- C27', C27'-C28',C25-C26,C26-C27,C27-C28,O2-C25,O2-C25',O2-C28 and O2-C28' distances were constrained. ; _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^)+(0.1108P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.050(13) _refine_ls_number_reflns 5973 _refine_ls_number_parameters 322 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1149 _refine_ls_R_factor_gt 0.0754 _refine_ls_wR_factor_ref 0.2201 _refine_ls_wR_factor_gt 0.1904 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 Y1 Y 0.5000 0.5000 0.49843(7) 0.0452(2) Uani 1 2 d S . . Br1 Br 0.83631(6) 0.39880(6) 0.52341(6) 0.1042(5) Uani 1 1 d . B . Si1 Si 0.43331(14) 0.48273(14) 0.61495(9) 0.0707(7) Uani 1 1 d . B . O1 O 0.5047(2) 0.5989(2) 0.4741(2) 0.0536(12) Uani 1 1 d . . . O2 O 0.5781(4) 0.3651(3) 0.3694(2) 0.091(2) Uani 1 1 d D . . N1 N 0.5880(3) 0.4928(3) 0.4468(3) 0.0566(17) Uani 1 1 d . . . N2 N 0.5000 0.5000 0.5835(3) 0.052(2) Uani 1 2 d S . . C1 C 0.5557(4) 0.6336(4) 0.4616(3) 0.056(2) Uani 1 1 d . B . C2 C 0.5647(4) 0.6947(4) 0.4795(3) 0.057(2) Uani 1 1 d . . . C3 C 0.6187(4) 0.7228(4) 0.4655(3) 0.059(2) Uani 1 1 d . . . H3 H 0.6262 0.7626 0.4784 0.071 Uiso 1 1 calc R . . C4 C 0.6634(4) 0.6977(4) 0.4339(3) 0.062(2) Uani 1 1 d . A . C5 C 0.6516(4) 0.6396(4) 0.4155(3) 0.055(2) Uani 1 1 d . A . H5 H 0.6802 0.6214 0.3933 0.067 Uiso 1 1 calc R . . C6 C 0.5981(4) 0.6064(4) 0.4287(3) 0.0516(18) Uani 1 1 d . . . C7 C 0.5168(4) 0.7243(4) 0.5146(3) 0.059(2) Uani 1 1 d . . . C8 C 0.5071(5) 0.6896(5) 0.5637(3) 0.076(3) Uani 1 1 d . . . H8A H 0.5039 0.6457 0.5568 0.114 Uiso 1 1 calc R . . H8B H 0.4694 0.7039 0.5797 0.114 Uiso 1 1 calc R . . H8C H 0.5418 0.6971 0.5860 0.114 Uiso 1 1 calc R . . C9 C 0.4549(5) 0.7315(4) 0.4874(5) 0.084(3) Uani 1 1 d . . . H9A H 0.4615 0.7504 0.4546 0.126 Uiso 1 1 calc R . . H9B H 0.4277 0.7574 0.5074 0.126 Uiso 1 1 calc R . . H9C H 0.4361 0.6912 0.4830 0.126 Uiso 1 1 calc R . . C10 C 0.5376(4) 0.7904(5) 0.5298(4) 0.073(2) Uani 1 1 d . . . H10A H 0.5801 0.7892 0.5415 0.109 Uiso 1 1 calc R . . H10B H 0.5112 0.8058 0.5565 0.109 Uiso 1 1 calc R . . H10C H 0.5347 0.8175 0.5007 0.109 Uiso 1 1 calc R . . C11 C 0.7229(4) 0.7323(4) 0.4210(4) 0.064(2) Uani 1 1 d . . . C12 C 0.7584(11) 0.7012(12) 0.3769(12) 0.081(7) Uani 0.50 1 d P A 1 H12A H 0.7921 0.7278 0.3663 0.122 Uiso 0.50 1 calc PR A 1 H12B H 0.7305 0.6946 0.3487 0.122 Uiso 0.50 1 calc PR A 1 H12C H 0.7748 0.6619 0.3881 0.122 Uiso 0.50 1 calc PR A 1 C12' C 0.7704(18) 0.694(2) 0.4005(12) 0.109(14) Uiso 0.50 1 d P A 2 H12D H 0.7670 0.6527 0.4146 0.163 Uiso 0.50 1 calc PR A 2 H12E H 0.8105 0.7111 0.4089 0.163 Uiso 0.50 1 calc PR A 2 H12F H 0.7661 0.6919 0.3641 0.163 Uiso 0.50 1 calc PR A 2 C13 C 0.7570(5) 0.7465(5) 0.4695(5) 0.089(4) Uani 1 1 d . A . H13A H 0.7652 0.7083 0.4875 0.133 Uiso 1 1 calc R . . H13B H 0.7320 0.7734 0.4904 0.133 Uiso 1 1 calc R . . H13C H 0.7958 0.7668 0.4616 0.133 Uiso 1 1 calc R . . C14 C 0.7076(5) 0.7940(6) 0.3967(5) 0.099(4) Uani 1 1 d . A . H14A H 0.7455 0.8160 0.3891 0.148 Uiso 1 1 calc R . . H14B H 0.6826 0.8184 0.4197 0.148 Uiso 1 1 calc R . . H14C H 0.6847 0.7870 0.3656 0.148 Uiso 1 1 calc R . . C15 C 0.5875(4) 0.5424(4) 0.4073(3) 0.0523(18) Uani 1 1 d . B . H15A H 0.5476 0.5417 0.3898 0.063 Uiso 1 1 calc R . . H15B H 0.6197 0.5335 0.3823 0.063 Uiso 1 1 calc R . . C16 C 0.6460(4) 0.4713(4) 0.4607(3) 0.056(2) Uani 1 1 d . B . C17 C 0.7022(4) 0.4909(4) 0.4404(4) 0.064(2) Uani 1 1 d . . . H17 H 0.7021 0.5201 0.4142 0.076 Uiso 1 1 calc R B . C18 C 0.7576(5) 0.4686(4) 0.4579(4) 0.073(3) Uani 1 1 d . B . H18 H 0.7946 0.4817 0.4427 0.087 Uiso 1 1 calc R . . C19 C 0.7599(4) 0.4266(4) 0.4981(4) 0.070(2) Uani 1 1 d . . . C20 C 0.7049(5) 0.4063(5) 0.5171(4) 0.079(3) Uani 1 1 d . B . H20 H 0.7053 0.3768 0.5431 0.095 Uiso 1 1 calc R . . C21 C 0.6492(4) 0.4273(4) 0.4995(4) 0.068(2) Uani 1 1 d . . . H21 H 0.6125 0.4119 0.5138 0.082 Uiso 1 1 calc R B . C22 C 0.4438(6) 0.4291(7) 0.6705(4) 0.106(4) Uani 1 1 d . . . H22A H 0.4748 0.3983 0.6625 0.159 Uiso 1 1 calc R B . H22B H 0.4049 0.4087 0.6780 0.159 Uiso 1 1 calc R . . H22C H 0.4570 0.4527 0.6998 0.159 Uiso 1 1 calc R . . C23 C 0.3776(5) 0.4401(5) 0.5724(4) 0.075(3) Uani 1 1 d . . . H23A H 0.3889 0.4471 0.5374 0.113 Uiso 1 1 calc R B . H23B H 0.3360 0.4552 0.5782 0.113 Uiso 1 1 calc R . . H23C H 0.3794 0.3963 0.5797 0.113 Uiso 1 1 calc R . . C24 C 0.3931(5) 0.5537(6) 0.6393(4) 0.089(3) Uani 1 1 d . . . H24A H 0.4175 0.5721 0.6660 0.133 Uiso 1 1 calc R B . H24B H 0.3528 0.5424 0.6524 0.133 Uiso 1 1 calc R . . H24C H 0.3881 0.5832 0.6120 0.133 Uiso 1 1 calc R . . C25 C 0.5979(14) 0.3974(10) 0.3250(6) 0.100(4) Uiso 0.50 1 d PD B 1 H25A H 0.6380 0.4171 0.3310 0.120 Uiso 0.50 1 calc PR B 1 H25B H 0.5679 0.4295 0.3161 0.120 Uiso 0.50 1 calc PR B 1 C26 C 0.6031(14) 0.3510(10) 0.2829(9) 0.100(4) Uiso 0.50 1 d PD B 1 H26A H 0.5705 0.3580 0.2578 0.120 Uiso 0.50 1 calc PR B 1 H26B H 0.6433 0.3548 0.2661 0.120 Uiso 0.50 1 calc PR B 1 C27 C 0.5965(13) 0.2891(11) 0.3056(8) 0.100(4) Uiso 0.50 1 d PD B 1 H27A H 0.5679 0.2636 0.2859 0.120 Uiso 0.50 1 calc PR B 1 H27B H 0.6366 0.2682 0.3076 0.120 Uiso 0.50 1 calc PR B 1 C28 C 0.5719(13) 0.3011(6) 0.3561(8) 0.100(4) Uiso 0.50 1 d PD B 1 H28A H 0.5282 0.2895 0.3571 0.120 Uiso 0.50 1 calc PR B 1 H28B H 0.5941 0.2757 0.3808 0.120 Uiso 0.50 1 calc PR B 1 C25' C 0.6270(8) 0.3898(9) 0.3398(7) 0.075(3) Uiso 0.50 1 d PD B 2 H25C H 0.6640 0.3948 0.3607 0.090 Uiso 0.50 1 calc PR B 2 H25D H 0.6152 0.4305 0.3267 0.090 Uiso 0.50 1 calc PR B 2 C26' C 0.6403(9) 0.3481(9) 0.2978(7) 0.075(3) Uiso 0.50 1 d PD B 2 H26C H 0.6759 0.3217 0.3053 0.090 Uiso 0.50 1 calc PR B 2 H26D H 0.6482 0.3711 0.2666 0.090 Uiso 0.50 1 calc PR B 2 C27' C 0.5813(9) 0.3107(11) 0.2940(7) 0.075(3) Uiso 0.50 1 d PD B 2 H27C H 0.5540 0.3282 0.2682 0.090 Uiso 0.50 1 calc PR B 2 H27D H 0.5907 0.2679 0.2848 0.090 Uiso 0.50 1 calc PR B 2 C28' C 0.5518(9) 0.3132(7) 0.3438(6) 0.075(3) Uiso 0.50 1 d PD B 2 H28C H 0.5071 0.3184 0.3403 0.090 Uiso 0.50 1 calc PR B 2 H28D H 0.5599 0.2751 0.3627 0.090 Uiso 0.50 1 calc PR B 2 Li1 Li 0.5603(8) 0.4047(6) 0.4279(6) 0.073(5) 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 Y1 0.0445(5) 0.0467(5) 0.0444(4) 0.000 0.000 0.0000(4) Br1 0.0831(8) 0.1037(9) 0.1257(9) 0.0015(8) -0.0152(7) 0.0307(6) Si1 0.0729(17) 0.0847(19) 0.0544(12) 0.0073(13) 0.0103(12) 0.0092(14) O1 0.050(3) 0.045(3) 0.066(3) 0.000(3) 0.005(2) -0.005(2) O2 0.119(6) 0.072(4) 0.082(4) -0.025(3) 0.038(4) -0.022(4) N1 0.052(4) 0.050(4) 0.068(4) -0.001(3) 0.023(3) -0.002(3) N2 0.055(5) 0.060(6) 0.039(5) 0.000 0.000 0.004(4) C1 0.069(6) 0.053(5) 0.047(4) 0.001(4) 0.001(4) -0.001(4) C2 0.077(6) 0.050(4) 0.045(4) 0.003(3) -0.005(4) -0.008(4) C3 0.057(5) 0.056(5) 0.065(5) -0.007(4) 0.001(4) -0.007(4) C4 0.064(5) 0.060(5) 0.061(5) 0.003(4) 0.002(4) -0.007(4) C5 0.058(5) 0.047(4) 0.061(5) 0.004(4) 0.021(4) -0.001(4) C6 0.054(4) 0.048(4) 0.053(4) 0.000(3) -0.004(4) -0.008(3) C7 0.049(4) 0.054(5) 0.074(5) -0.003(4) -0.001(4) 0.004(3) C8 0.099(8) 0.072(7) 0.057(5) -0.014(5) 0.016(5) -0.005(5) C9 0.070(6) 0.055(5) 0.126(9) -0.019(5) -0.033(6) 0.011(4) C10 0.067(5) 0.071(6) 0.079(6) -0.015(5) 0.000(5) -0.001(4) C11 0.057(5) 0.055(5) 0.079(6) -0.006(4) -0.002(4) -0.018(4) C12 0.056(12) 0.079(14) 0.11(2) -0.007(15) 0.031(14) -0.036(11) C13 0.055(6) 0.095(8) 0.117(9) 0.027(7) -0.024(6) -0.015(5) C14 0.074(7) 0.115(10) 0.107(9) 0.028(8) -0.011(6) -0.027(7) C15 0.060(5) 0.046(4) 0.051(4) 0.002(3) 0.008(4) -0.004(3) C16 0.057(5) 0.046(4) 0.066(5) -0.013(4) 0.016(4) 0.012(4) C17 0.054(5) 0.062(5) 0.075(6) 0.007(4) 0.015(5) 0.005(4) C18 0.070(6) 0.060(6) 0.088(7) 0.004(5) 0.016(5) -0.004(4) C19 0.053(5) 0.057(5) 0.100(6) -0.007(5) -0.011(5) 0.014(4) C20 0.095(8) 0.074(6) 0.069(5) 0.011(5) 0.012(6) 0.021(5) C21 0.070(5) 0.051(5) 0.083(6) 0.009(5) 0.013(5) 0.018(4) C22 0.109(9) 0.155(12) 0.055(6) 0.023(7) -0.004(6) 0.000(9) C23 0.067(6) 0.073(6) 0.085(6) 0.002(5) 0.000(5) -0.001(5) C24 0.078(7) 0.108(9) 0.081(6) -0.012(6) 0.025(6) 0.028(6) Li1 0.090(11) 0.038(7) 0.091(10) -0.006(7) 0.045(9) -0.013(7) _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 Y1 O1 2.239(5) 11_554 ? Y1 O1 2.239(5) . ? Y1 N2 2.253(9) . ? Y1 N1 2.349(6) 11_554 ? Y1 N1 2.349(6) . ? Y1 Li1 3.073(14) 11_554 ? Y1 Li1 3.073(14) . ? Y1 Si1 3.426(3) 11_554 ? Br1 C19 1.884(8) . ? Si1 N2 1.707(5) . ? Si1 C24 1.879(11) . ? Si1 C22 1.888(11) . ? Si1 C23 1.890(10) . ? O1 C1 1.375(10) . ? O1 Li1 1.867(15) 11_554 ? O2 C25' 1.422(9) . ? O2 C28' 1.429(9) . ? O2 C25 1.433(10) . ? O2 C28 1.435(10) . ? O2 Li1 1.811(16) . ? N1 C16 1.387(11) . ? N1 C15 1.500(11) . ? N1 Li1 2.060(15) . ? N2 Si1 1.707(5) 11_554 ? C1 C6 1.396(11) . ? C1 C2 1.418(11) . ? C2 C3 1.369(12) . ? C2 C7 1.532(12) . ? C3 C4 1.391(12) . ? C3 H3 0.9400 . ? C4 C5 1.371(12) . ? C4 C11 1.528(12) . ? C5 C6 1.406(11) . ? C5 H5 0.9400 . ? C6 C15 1.515(11) . ? C7 C8 1.515(14) . ? C7 C9 1.529(12) . ? C7 C10 1.553(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12' 1.43(4) . ? C11 C13 1.512(15) . ? C11 C14 1.518(15) . ? C11 C12 1.55(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C12' H12D 0.9700 . ? C12' H12E 0.9700 . ? C12' H12F 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C17 1.396(12) . ? C16 C21 1.403(12) . ? C17 C18 1.374(14) . ? C17 H17 0.9400 . ? C18 C19 1.399(14) . ? C18 H18 0.9400 . ? C19 C20 1.365(13) . ? C20 C21 1.369(13) . ? C20 H20 0.9400 . ? C21 H21 0.9400 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C26 1.505(18) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 C27 1.475(18) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.460(17) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C25' C26' 1.458(17) . ? C25' H25C 0.9800 . ? C25' H25D 0.9800 . ? C26' C27' 1.515(17) . ? C26' H26C 0.9800 . ? C26' H26D 0.9800 . ? C27' C28' 1.466(17) . ? C27' H27C 0.9800 . ? C27' H27D 0.9800 . ? C28' H28C 0.9800 . ? C28' H28D 0.9800 . ? Li1 O1 1.867(15) 11_554 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Y1 O1 146.5(3) 11_554 . ? O1 Y1 N2 106.73(15) 11_554 . ? O1 Y1 N2 106.73(15) . . ? O1 Y1 N1 81.9(2) 11_554 11_554 ? O1 Y1 N1 78.8(2) . 11_554 ? N2 Y1 N1 125.5(2) . 11_554 ? O1 Y1 N1 78.8(2) 11_554 . ? O1 Y1 N1 81.9(2) . . ? N2 Y1 N1 125.5(2) . . ? N1 Y1 N1 108.9(4) 11_554 . ? O1 Y1 Li1 116.6(3) 11_554 11_554 ? O1 Y1 Li1 37.1(3) . 11_554 ? N2 Y1 Li1 127.4(3) . 11_554 ? N1 Y1 Li1 42.1(3) 11_554 11_554 ? N1 Y1 Li1 92.1(4) . 11_554 ? O1 Y1 Li1 37.1(3) 11_554 . ? O1 Y1 Li1 116.6(3) . . ? N2 Y1 Li1 127.4(3) . . ? N1 Y1 Li1 92.1(4) 11_554 . ? N1 Y1 Li1 42.1(3) . . ? Li1 Y1 Li1 105.2(7) 11_554 . ? O1 Y1 Si1 112.51(16) 11_554 11_554 ? O1 Y1 Si1 97.79(16) . 11_554 ? N2 Y1 Si1 25.80(5) . 11_554 ? N1 Y1 Si1 149.1(2) 11_554 11_554 ? N1 Y1 Si1 100.9(2) . 11_554 ? Li1 Y1 Si1 130.8(3) 11_554 11_554 ? Li1 Y1 Si1 116.2(4) . 11_554 ? N2 Si1 C24 112.3(4) . . ? N2 Si1 C22 114.4(5) . . ? C24 Si1 C22 106.9(6) . . ? N2 Si1 C23 110.8(4) . . ? C24 Si1 C23 107.9(5) . . ? C22 Si1 C23 104.0(6) . . ? C1 O1 Li1 118.1(7) . 11_554 ? C1 O1 Y1 128.9(5) . . ? Li1 O1 Y1 96.5(5) 11_554 . ? C25' O2 C28' 109.2(11) . . ? C25' O2 C25 30.8(12) . . ? C28' O2 C25 96.5(12) . . ? C25' O2 C28 107.2(13) . . ? C28' O2 C28 24.3(13) . . ? C25 O2 C28 107.3(13) . . ? C25' O2 Li1 116.8(9) . . ? C28' O2 Li1 133.9(9) . . ? C25 O2 Li1 122.2(11) . . ? C28 O2 Li1 130.4(11) . . ? C16 N1 C15 115.6(6) . . ? C16 N1 Li1 91.0(7) . . ? C15 N1 Li1 119.4(7) . . ? C16 N1 Y1 127.0(6) . . ? C15 N1 Y1 110.6(5) . . ? Li1 N1 Y1 88.1(5) . . ? Si1 N2 Si1 121.7(6) . 11_554 ? Si1 N2 Y1 119.2(3) . . ? Si1 N2 Y1 119.2(3) 11_554 . ? O1 C1 C6 116.6(7) . . ? O1 C1 C2 122.6(7) . . ? C6 C1 C2 120.8(8) . . ? C3 C2 C1 116.2(8) . . ? C3 C2 C7 123.8(7) . . ? C1 C2 C7 120.0(8) . . ? C2 C3 C4 125.7(8) . . ? C2 C3 H3 117.2 . . ? C4 C3 H3 117.2 . . ? C5 C4 C3 116.2(8) . . ? C5 C4 C11 121.9(8) . . ? C3 C4 C11 121.9(8) . . ? C4 C5 C6 122.3(7) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C1 C6 C5 118.7(7) . . ? C1 C6 C15 121.3(7) . . ? C5 C6 C15 120.0(7) . . ? C8 C7 C9 109.4(8) . . ? C8 C7 C2 114.1(7) . . ? C9 C7 C2 110.4(7) . . ? C8 C7 C10 106.0(7) . . ? C9 C7 C10 106.4(7) . . ? C2 C7 C10 110.2(7) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12' C11 C13 95.0(16) . . ? C12' C11 C14 120.4(17) . . ? C13 C11 C14 106.8(8) . . ? C12' C11 C4 113.9(18) . . ? C13 C11 C4 108.8(8) . . ? C14 C11 C4 110.0(8) . . ? C12' C11 C12 26.5(16) . . ? C13 C11 C12 118.9(14) . . ? C14 C11 C12 99.8(14) . . ? C4 C11 C12 111.9(10) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? C11 C12' H12D 109.5 . . ? C11 C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C11 C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C6 113.2(6) . . ? N1 C15 H15A 108.9 . . ? C6 C15 H15A 108.9 . . ? N1 C15 H15B 108.9 . . ? C6 C15 H15B 108.9 . . ? H15A C15 H15B 107.8 . . ? N1 C16 C17 125.7(8) . . ? N1 C16 C21 117.9(7) . . ? C17 C16 C21 116.4(8) . . ? C18 C17 C16 121.7(9) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C17 C18 C19 121.0(9) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C18 117.3(8) . . ? C20 C19 Br1 122.1(8) . . ? C18 C19 Br1 120.6(7) . . ? C19 C20 C21 122.4(9) . . ? C19 C20 H20 118.8 . . ? C21 C20 H20 118.8 . . ? C20 C21 C16 121.2(9) . . ? C20 C21 H21 119.4 . . ? C16 C21 H21 119.4 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O2 C25 C26 107.7(16) . . ? O2 C25 H25A 110.2 . . ? C26 C25 H25A 110.2 . . ? O2 C25 H25B 110.2 . . ? C26 C25 H25B 110.2 . . ? H25A C25 H25B 108.5 . . ? C27 C26 C25 107.2(19) . . ? C27 C26 H26A 110.3 . . ? C25 C26 H26A 110.3 . . ? C27 C26 H26B 110.3 . . ? C25 C26 H26B 110.3 . . ? H26A C26 H26B 108.5 . . ? C28 C27 C26 104.3(19) . . ? C28 C27 H27A 110.9 . . ? C26 C27 H27A 110.9 . . ? C28 C27 H27B 110.9 . . ? C26 C27 H27B 110.9 . . ? H27A C27 H27B 108.9 . . ? O2 C28 C27 111.3(17) . . ? O2 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? O2 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? O2 C25' C26' 109.5(13) . . ? O2 C25' H25C 109.8 . . ? C26' C25' H25C 109.8 . . ? O2 C25' H25D 109.8 . . ? C26' C25' H25D 109.8 . . ? H25C C25' H25D 108.2 . . ? C25' C26' C27' 102.5(15) . . ? C25' C26' H26C 111.3 . . ? C27' C26' H26C 111.3 . . ? C25' C26' H26D 111.3 . . ? C27' C26' H26D 111.3 . . ? H26C C26' H26D 109.2 . . ? C28' C27' C26' 106.6(14) . . ? C28' C27' H27C 110.4 . . ? C26' C27' H27C 110.4 . . ? C28' C27' H27D 110.4 . . ? C26' C27' H27D 110.4 . . ? H27C C27' H27D 108.6 . . ? O2 C28' C27' 106.4(13) . . ? O2 C28' H28C 110.4 . . ? C27' C28' H28C 110.4 . . ? O2 C28' H28D 110.4 . . ? C27' C28' H28D 110.4 . . ? H28C C28' H28D 108.6 . . ? O2 Li1 O1 134.4(10) . 11_554 ? O2 Li1 N1 125.8(8) . . ? O1 Li1 N1 95.7(6) 11_554 . ? O2 Li1 Y1 158.0(10) . . ? O1 Li1 Y1 46.4(3) 11_554 . ? N1 Li1 Y1 49.8(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 O1 Y1 O1 C1 -85.5(6) 11_554 . . . ? N2 Y1 O1 C1 94.5(6) . . . . ? N1 Y1 O1 C1 -141.5(7) 11_554 . . . ? N1 Y1 O1 C1 -30.2(6) . . . . ? Li1 Y1 O1 C1 -134.6(9) 11_554 . . . ? Li1 Y1 O1 C1 -54.8(8) . . . . ? Si1 Y1 O1 C1 69.7(6) 11_554 . . . ? O1 Y1 O1 Li1 49.1(6) 11_554 . . 11_554 ? N2 Y1 O1 Li1 -130.9(6) . . . 11_554 ? N1 Y1 O1 Li1 -6.9(7) 11_554 . . 11_554 ? N1 Y1 O1 Li1 104.4(7) . . . 11_554 ? Li1 Y1 O1 Li1 79.8(10) . . . 11_554 ? Si1 Y1 O1 Li1 -155.7(6) 11_554 . . 11_554 ? O1 Y1 N1 C16 -83.7(6) 11_554 . . . ? O1 Y1 N1 C16 123.8(7) . . . . ? N2 Y1 N1 C16 19.0(7) . . . . ? N1 Y1 N1 C16 -161.0(7) 11_554 . . . ? Li1 Y1 N1 C16 159.6(7) 11_554 . . . ? Li1 Y1 N1 C16 -89.8(8) . . . . ? Si1 Y1 N1 C16 27.4(6) 11_554 . . . ? O1 Y1 N1 C15 127.0(5) 11_554 . . . ? O1 Y1 N1 C15 -25.5(5) . . . . ? N2 Y1 N1 C15 -130.4(5) . . . . ? N1 Y1 N1 C15 49.6(5) 11_554 . . . ? Li1 Y1 N1 C15 10.3(6) 11_554 . . . ? Li1 Y1 N1 C15 120.8(8) . . . . ? Si1 Y1 N1 C15 -122.0(5) 11_554 . . . ? O1 Y1 N1 Li1 6.2(6) 11_554 . . . ? O1 Y1 N1 Li1 -146.3(6) . . . . ? N2 Y1 N1 Li1 108.8(6) . . . . ? N1 Y1 N1 Li1 -71.2(6) 11_554 . . . ? Li1 Y1 N1 Li1 -110.5(7) 11_554 . . . ? Si1 Y1 N1 Li1 117.2(6) 11_554 . . . ? C24 Si1 N2 Si1 78.8(4) . . . 11_554 ? C22 Si1 N2 Si1 -43.4(5) . . . 11_554 ? C23 Si1 N2 Si1 -160.5(4) . . . 11_554 ? C24 Si1 N2 Y1 -101.2(4) . . . . ? C22 Si1 N2 Y1 136.6(5) . . . . ? C23 Si1 N2 Y1 19.5(4) . . . . ? O1 Y1 N2 Si1 -72.75(18) 11_554 . . . ? O1 Y1 N2 Si1 107.25(18) . . . . ? N1 Y1 N2 Si1 19.2(2) 11_554 . . . ? N1 Y1 N2 Si1 -160.8(2) . . . . ? Li1 Y1 N2 Si1 72.2(4) 11_554 . . . ? Li1 Y1 N2 Si1 -107.8(4) . . . . ? Si1 Y1 N2 Si1 180.0 11_554 . . . ? O1 Y1 N2 Si1 107.25(18) 11_554 . . 11_554 ? O1 Y1 N2 Si1 -72.75(18) . . . 11_554 ? N1 Y1 N2 Si1 -160.8(2) 11_554 . . 11_554 ? N1 Y1 N2 Si1 19.2(2) . . . 11_554 ? Li1 Y1 N2 Si1 -107.8(4) 11_554 . . 11_554 ? Li1 Y1 N2 Si1 72.2(4) . . . 11_554 ? Li1 O1 C1 C6 -79.7(10) 11_554 . . . ? Y1 O1 C1 C6 47.0(10) . . . . ? Li1 O1 C1 C2 98.2(9) 11_554 . . . ? Y1 O1 C1 C2 -135.1(7) . . . . ? O1 C1 C2 C3 177.6(8) . . . . ? C6 C1 C2 C3 -4.6(11) . . . . ? O1 C1 C2 C7 0.8(11) . . . . ? C6 C1 C2 C7 178.6(7) . . . . ? C1 C2 C3 C4 3.1(13) . . . . ? C7 C2 C3 C4 179.8(8) . . . . ? C2 C3 C4 C5 -0.1(13) . . . . ? C2 C3 C4 C11 -179.2(8) . . . . ? C3 C4 C5 C6 -1.6(13) . . . . ? C11 C4 C5 C6 177.5(8) . . . . ? O1 C1 C6 C5 -178.9(7) . . . . ? C2 C1 C6 C5 3.2(11) . . . . ? O1 C1 C6 C15 1.0(11) . . . . ? C2 C1 C6 C15 -176.9(7) . . . . ? C4 C5 C6 C1 0.0(12) . . . . ? C4 C5 C6 C15 -179.9(8) . . . . ? C3 C2 C7 C8 -116.9(9) . . . . ? C1 C2 C7 C8 59.7(10) . . . . ? C3 C2 C7 C9 119.4(9) . . . . ? C1 C2 C7 C9 -64.0(10) . . . . ? C3 C2 C7 C10 2.1(11) . . . . ? C1 C2 C7 C10 178.7(8) . . . . ? C5 C4 C11 C12' -15.9(19) . . . . ? C3 C4 C11 C12' 163.2(16) . . . . ? C5 C4 C11 C13 -120.5(10) . . . . ? C3 C4 C11 C13 58.5(12) . . . . ? C5 C4 C11 C14 122.9(10) . . . . ? C3 C4 C11 C14 -58.1(12) . . . . ? C5 C4 C11 C12 12.9(19) . . . . ? C3 C4 C11 C12 -168.1(16) . . . . ? C16 N1 C15 C6 -83.1(8) . . . . ? Li1 N1 C15 C6 169.9(7) . . . . ? Y1 N1 C15 C6 70.0(7) . . . . ? C1 C6 C15 N1 -64.9(10) . . . . ? C5 C6 C15 N1 115.0(8) . . . . ? C15 N1 C16 C17 -1.5(11) . . . . ? Li1 N1 C16 C17 122.1(9) . . . . ? Y1 N1 C16 C17 -149.5(7) . . . . ? C15 N1 C16 C21 176.6(7) . . . . ? Li1 N1 C16 C21 -59.9(9) . . . . ? Y1 N1 C16 C21 28.5(10) . . . . ? N1 C16 C17 C18 177.5(9) . . . . ? C21 C16 C17 C18 -0.5(13) . . . . ? C16 C17 C18 C19 -2.1(14) . . . . ? C17 C18 C19 C20 3.6(14) . . . . ? C17 C18 C19 Br1 -177.5(7) . . . . ? C18 C19 C20 C21 -2.5(15) . . . . ? Br1 C19 C20 C21 178.6(8) . . . . ? C19 C20 C21 C16 0.0(15) . . . . ? N1 C16 C21 C20 -176.6(9) . . . . ? C17 C16 C21 C20 1.6(13) . . . . ? C25' O2 C25 C26 96(3) . . . . ? C28' O2 C25 C26 -22(2) . . . . ? C28 O2 C25 C26 1(3) . . . . ? Li1 O2 C25 C26 -175.2(17) . . . . ? O2 C25 C26 C27 -10(3) . . . . ? C25 C26 C27 C28 14(3) . . . . ? C25' O2 C28 C27 -24(3) . . . . ? C28' O2 C28 C27 75(3) . . . . ? C25 O2 C28 C27 9(3) . . . . ? Li1 O2 C28 C27 -175.6(17) . . . . ? C26 C27 C28 O2 -15(3) . . . . ? C28' O2 C25' C26' -9(2) . . . . ? C25 O2 C25' C26' -79(3) . . . . ? C28 O2 C25' C26' 16(2) . . . . ? Li1 O2 C25' C26' 172.7(14) . . . . ? O2 C25' C26' C27' 20(2) . . . . ? C25' C26' C27' C28' -24(2) . . . . ? C25' O2 C28' C27' -7(2) . . . . ? C25 O2 C28' C27' 22(2) . . . . ? C28 O2 C28' C27' -96(4) . . . . ? Li1 O2 C28' C27' 171.0(14) . . . . ? C26' C27' C28' O2 19(2) . . . . ? C25' O2 Li1 O1 167.9(15) . . . 11_554 ? C28' O2 Li1 O1 -10(2) . . . 11_554 ? C25 O2 Li1 O1 132.8(18) . . . 11_554 ? C28 O2 Li1 O1 -42(2) . . . 11_554 ? C25' O2 Li1 N1 16(2) . . . . ? C28' O2 Li1 N1 -160.9(16) . . . . ? C25 O2 Li1 N1 -19(2) . . . . ? C28 O2 Li1 N1 166.5(18) . . . . ? C25' O2 Li1 Y1 87(2) . . . . ? C28' O2 Li1 Y1 -91(2) . . . . ? C25 O2 Li1 Y1 52(3) . . . . ? C28 O2 Li1 Y1 -123(2) . . . . ? C16 N1 Li1 O2 -80.5(13) . . . . ? C15 N1 Li1 O2 39.9(15) . . . . ? Y1 N1 Li1 O2 152.6(12) . . . . ? C16 N1 Li1 O1 119.7(8) . . . 11_554 ? C15 N1 Li1 O1 -120.0(8) . . . 11_554 ? Y1 N1 Li1 O1 -7.3(7) . . . 11_554 ? C16 N1 Li1 Y1 127.0(6) . . . . ? C15 N1 Li1 Y1 -112.7(7) . . . . ? O1 Y1 Li1 O2 103(2) 11_554 . . . ? O1 Y1 Li1 O2 -49(2) . . . . ? N2 Y1 Li1 O2 168.6(18) . . . . ? N1 Y1 Li1 O2 29(2) 11_554 . . . ? N1 Y1 Li1 O2 -87.3(19) . . . . ? Li1 Y1 Li1 O2 -11.4(18) 11_554 . . . ? Si1 Y1 Li1 O2 -163.9(19) 11_554 . . . ? O1 Y1 Li1 O1 -152.2(4) . . . 11_554 ? N2 Y1 Li1 O1 65.8(7) . . . 11_554 ? N1 Y1 Li1 O1 -73.7(6) 11_554 . . 11_554 ? N1 Y1 Li1 O1 169.9(9) . . . 11_554 ? Li1 Y1 Li1 O1 -114.2(7) 11_554 . . 11_554 ? Si1 Y1 Li1 O1 93.3(6) 11_554 . . 11_554 ? O1 Y1 Li1 N1 -169.9(9) 11_554 . . . ? O1 Y1 Li1 N1 37.9(7) . . . . ? N2 Y1 Li1 N1 -104.2(4) . . . . ? N1 Y1 Li1 N1 116.4(6) 11_554 . . . ? Li1 Y1 Li1 N1 75.8(4) 11_554 . . . ? Si1 Y1 Li1 N1 -76.7(5) 11_554 . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.697 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.086 _database_code_depnum_ccdc_archive 'CCDC 932403' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H86 Br2 Li2 N3 O4 Si2 Yb' _chemical_formula_sum 'C56 H86 Br2 Li2 N3 O4 Si2 Yb' _chemical_formula_weight 1268.20 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' Si Si 0.0817 0.0704 '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' Yb Yb -0.3850 5.5486 '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 tetragonal _symmetry_space_group_name_H-M 'I 41 c d' _symmetry_space_group_name_Hall 'I 4bw -2c' _symmetry_Int_Tables_number 110 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/2, z+1/4' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x, z+3/4' '-x, y, z+1/2' 'y, x+1/2, z+3/4' 'x+1/2, -y+1/2, z' '-y+1/2, -x, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1, z+3/4' '-x+1, -y+1, z+1' 'y+1, -x+1/2, z+5/4' '-x+1/2, y+1/2, z+1' 'y+1/2, x+1, z+5/4' 'x+1, -y+1, z+1/2' '-y+1, -x+1/2, z+3/4' _cell_length_a 21.5857(11) _cell_length_b 21.5857(11) _cell_length_c 26.4362(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12317.7(11) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 20631 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5192 _exptl_absorpt_coefficient_mu 2.897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.304 _exptl_absorpt_correction_T_max 0.419 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33898 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_unetI/netI 0.0348 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6887 _reflns_number_gt 5733 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Their C25'-C26',C26'-C27', C27'-C28',C25-C26,C26-C27,C27-C28,O2-C25,O2-C25',O2-C28, O2-C28' and C11-C12 distances were constrained. ; _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^)+(0.0777P)^2^+51.3191P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.024(15) _refine_ls_number_reflns 6887 _refine_ls_number_parameters 317 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1246 _refine_ls_goodness_of_fit_ref 0.895 _refine_ls_restrained_S_all 0.896 _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 Yb1 Yb 0.5000 0.0000 0.87537(7) 0.03247(11) Uani 1 2 d S . . Br1 Br 0.39896(4) -0.33623(4) 0.90097(4) 0.0835(3) Uani 1 1 d . B . Si1 Si 0.48261(10) 0.06686(10) 0.99138(7) 0.0523(4) Uani 1 1 d . B . O1 O 0.59800(18) -0.00484(16) 0.85359(17) 0.0347(8) Uani 1 1 d . . . O2 O 0.3639(2) -0.0771(3) 0.7478(2) 0.0736(16) Uani 1 1 d D . . N1 N 0.4932(2) -0.0870(2) 0.8250(2) 0.0366(11) Uani 1 1 d . . . N2 N 0.5000 0.0000 0.9591(3) 0.040(2) Uani 1 2 d S . . C1 C 0.6324(3) -0.0554(3) 0.8399(2) 0.0369(12) Uani 1 1 d . . . C2 C 0.6933(3) -0.0648(3) 0.8586(2) 0.0363(12) Uani 1 1 d . . . C3 C 0.7238(3) -0.1190(3) 0.8442(2) 0.0434(14) Uani 1 1 d . . . H3 H 0.7637 -0.1263 0.8571 0.052 Uiso 1 1 calc R . . C4 C 0.6979(3) -0.1633(3) 0.8117(3) 0.0451(14) Uani 1 1 d . A . C5 C 0.6397(3) -0.1505(3) 0.7926(3) 0.0433(14) Uani 1 1 d . A . H5 H 0.6217 -0.1784 0.7696 0.052 Uiso 1 1 calc R . . C6 C 0.6070(3) -0.0983(3) 0.8063(2) 0.0381(13) Uani 1 1 d . . . C7 C 0.7241(3) -0.0166(3) 0.8935(3) 0.0436(14) Uani 1 1 d . . . C8 C 0.6884(4) -0.0081(4) 0.9426(3) 0.060(2) Uani 1 1 d . . . H8A H 0.6463 0.0048 0.9350 0.090 Uiso 1 1 calc R . . H8B H 0.7085 0.0234 0.9630 0.090 Uiso 1 1 calc R . . H8C H 0.6875 -0.0469 0.9610 0.090 Uiso 1 1 calc R . . C9 C 0.7317(3) 0.0448(3) 0.8661(3) 0.064(2) Uani 1 1 d . . . H9A H 0.7535 0.0737 0.8878 0.096 Uiso 1 1 calc R . . H9B H 0.6912 0.0613 0.8577 0.096 Uiso 1 1 calc R . . H9C H 0.7553 0.0384 0.8353 0.096 Uiso 1 1 calc R . . C10 C 0.7911(3) -0.0375(3) 0.9083(3) 0.0541(16) Uani 1 1 d . . . H10A H 0.7889 -0.0755 0.9278 0.081 Uiso 1 1 calc R . . H10B H 0.8107 -0.0054 0.9284 0.081 Uiso 1 1 calc R . . H10C H 0.8151 -0.0446 0.8778 0.081 Uiso 1 1 calc R . . C11 C 0.7332(3) -0.2228(3) 0.7981(3) 0.0552(19) Uani 1 1 d D . . C12 C 0.7034(7) -0.2578(7) 0.7554(6) 0.056(4) Uiso 0.50 1 d PD A 1 H12A H 0.7117 -0.2366 0.7238 0.085 Uiso 0.50 1 calc PR A 1 H12B H 0.6590 -0.2599 0.7609 0.085 Uiso 0.50 1 calc PR A 1 H12C H 0.7202 -0.2994 0.7540 0.085 Uiso 0.50 1 calc PR A 1 C12' C 0.6893(9) -0.2730(8) 0.7754(7) 0.062(4) Uiso 0.50 1 d P A 2 H12D H 0.7101 -0.3128 0.7755 0.093 Uiso 0.50 1 calc PR A 2 H12E H 0.6786 -0.2618 0.7409 0.093 Uiso 0.50 1 calc PR A 2 H12F H 0.6519 -0.2755 0.7956 0.093 Uiso 0.50 1 calc PR A 2 C13 C 0.7470(4) -0.2573(4) 0.8483(6) 0.081(4) Uani 1 1 d . A . H13A H 0.7666 -0.2967 0.8410 0.121 Uiso 1 1 calc R . . H13B H 0.7086 -0.2643 0.8665 0.121 Uiso 1 1 calc R . . H13C H 0.7745 -0.2323 0.8690 0.121 Uiso 1 1 calc R . . C14 C 0.7953(5) -0.2069(4) 0.7734(4) 0.076(3) Uani 1 1 d . A . H14A H 0.7880 -0.1841 0.7423 0.114 Uiso 1 1 calc R . . H14B H 0.8177 -0.2447 0.7658 0.114 Uiso 1 1 calc R . . H14C H 0.8197 -0.1816 0.7963 0.114 Uiso 1 1 calc R . . C15 C 0.5428(3) -0.0858(3) 0.7858(2) 0.0360(12) Uani 1 1 d . B . H15 H 0.5349 -0.0780 0.7514 0.043 Uiso 1 1 calc R . . C16 C 0.4720(2) -0.1452(3) 0.8387(2) 0.0398(13) Uani 1 1 d . B . C17 C 0.4913(3) -0.2020(3) 0.8176(3) 0.0446(15) Uani 1 1 d . . . H17 H 0.5204 -0.2021 0.7912 0.054 Uiso 1 1 calc R B . C18 C 0.4679(3) -0.2580(3) 0.8354(3) 0.0518(16) Uani 1 1 d . B . H18 H 0.4802 -0.2953 0.8200 0.062 Uiso 1 1 calc R . . C19 C 0.4269(3) -0.2594(3) 0.8753(3) 0.0532(16) Uani 1 1 d . . . C20 C 0.4056(3) -0.2043(3) 0.8953(3) 0.0597(18) Uani 1 1 d . B . H20 H 0.3762 -0.2049 0.9215 0.072 Uiso 1 1 calc R . . C21 C 0.4270(3) -0.1486(3) 0.8773(3) 0.0515(16) Uani 1 1 d . . . H21 H 0.4113 -0.1117 0.8912 0.062 Uiso 1 1 calc R B . C22 C 0.5529(4) 0.1071(4) 1.0154(3) 0.073(2) Uani 1 1 d . . . H22A H 0.5860 0.1031 0.9908 0.110 Uiso 1 1 calc R B . H22B H 0.5656 0.0885 1.0471 0.110 Uiso 1 1 calc R . . H22C H 0.5436 0.1505 1.0207 0.110 Uiso 1 1 calc R . . C23 C 0.4400(4) 0.1238(3) 0.9503(3) 0.0606(19) Uani 1 1 d . . . H23A H 0.4090 0.1021 0.9306 0.091 Uiso 1 1 calc R B . H23B H 0.4691 0.1440 0.9277 0.091 Uiso 1 1 calc R . . H23C H 0.4201 0.1546 0.9714 0.091 Uiso 1 1 calc R . . C24 C 0.4304(4) 0.0538(5) 1.0471(3) 0.077(3) Uani 1 1 d . . . H24A H 0.4528 0.0316 1.0732 0.115 Uiso 1 1 calc R B . H24B H 0.3948 0.0296 1.0366 0.115 Uiso 1 1 calc R . . H24C H 0.4166 0.0934 1.0602 0.115 Uiso 1 1 calc R . . C25 C 0.3911(7) -0.1240(7) 0.7169(6) 0.060(2) Uiso 0.50 1 d PD B 1 H25A H 0.4000 -0.1610 0.7371 0.072 Uiso 0.50 1 calc PR B 1 H25B H 0.4299 -0.1090 0.7021 0.072 Uiso 0.50 1 calc PR B 1 C26 C 0.3474(7) -0.1385(8) 0.6775(6) 0.060(2) Uiso 0.50 1 d PD B 1 H26A H 0.3326 -0.1811 0.6815 0.072 Uiso 0.50 1 calc PR B 1 H26B H 0.3674 -0.1349 0.6444 0.072 Uiso 0.50 1 calc PR B 1 C27 C 0.2950(7) -0.0952(7) 0.6807(6) 0.060(2) Uiso 0.50 1 d PD B 1 H27A H 0.2555 -0.1174 0.6787 0.072 Uiso 0.50 1 calc PR B 1 H27B H 0.2968 -0.0647 0.6533 0.072 Uiso 0.50 1 calc PR B 1 C28 C 0.3021(5) -0.0646(8) 0.7306(6) 0.060(2) Uiso 0.50 1 d PD B 1 H28A H 0.2956 -0.0199 0.7274 0.072 Uiso 0.50 1 calc PR B 1 H28B H 0.2718 -0.0811 0.7547 0.072 Uiso 0.50 1 calc PR B 1 C25' C 0.3998(9) -0.0976(12) 0.7056(6) 0.096(4) Uiso 0.50 1 d PD B 2 H25C H 0.4246 -0.1337 0.7153 0.116 Uiso 0.50 1 calc PR B 2 H25D H 0.4282 -0.0646 0.6950 0.116 Uiso 0.50 1 calc PR B 2 C26' C 0.3584(10) -0.1140(11) 0.6636(9) 0.096(4) Uiso 0.50 1 d PD B 2 H26C H 0.3784 -0.1083 0.6307 0.116 Uiso 0.50 1 calc PR B 2 H26D H 0.3430 -0.1565 0.6665 0.116 Uiso 0.50 1 calc PR B 2 C27' C 0.3121(11) -0.0709(11) 0.6718(8) 0.096(4) Uiso 0.50 1 d PD B 2 H27C H 0.2718 -0.0899 0.6647 0.116 Uiso 0.50 1 calc PR B 2 H27D H 0.3176 -0.0361 0.6484 0.116 Uiso 0.50 1 calc PR B 2 C28' C 0.3127(8) -0.0474(10) 0.7244(8) 0.096(4) Uiso 0.50 1 d PD B 2 H28C H 0.3178 -0.0023 0.7249 0.116 Uiso 0.50 1 calc PR B 2 H28D H 0.2740 -0.0579 0.7418 0.116 Uiso 0.50 1 calc PR B 2 Li1 Li 0.4034(5) -0.0612(6) 0.8072(5) 0.055(3) 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 Yb1 0.03400(17) 0.03011(16) 0.03330(18) 0.000 0.000 0.00039(11) Br1 0.0831(6) 0.0641(5) 0.1032(7) 0.0150(5) 0.0009(5) -0.0287(4) Si1 0.0629(11) 0.0565(11) 0.0376(9) -0.0090(8) 0.0062(9) -0.0092(9) O1 0.0274(19) 0.033(2) 0.043(2) 0.0013(15) 0.0021(17) 0.0041(13) O2 0.060(3) 0.097(4) 0.063(3) -0.033(3) -0.017(3) 0.025(3) N1 0.033(2) 0.036(3) 0.040(3) -0.011(2) -0.0059(19) 0.0008(18) N2 0.061(5) 0.041(4) 0.019(4) 0.000 0.000 -0.004(3) C1 0.040(3) 0.036(3) 0.035(3) 0.005(2) 0.005(2) -0.001(2) C2 0.035(3) 0.039(3) 0.035(3) -0.002(2) 0.002(2) 0.000(2) C3 0.034(3) 0.048(3) 0.048(4) -0.002(3) -0.005(3) 0.004(2) C4 0.038(3) 0.043(3) 0.054(4) -0.003(3) -0.002(3) 0.003(3) C5 0.043(3) 0.045(3) 0.042(3) -0.009(3) 0.002(3) 0.000(3) C6 0.030(3) 0.045(3) 0.039(3) 0.006(3) -0.001(2) 0.001(2) C7 0.034(3) 0.042(3) 0.055(4) 0.001(3) -0.011(3) -0.002(2) C8 0.062(5) 0.069(5) 0.049(4) -0.014(3) -0.010(4) 0.007(3) C9 0.052(4) 0.053(4) 0.086(6) 0.016(4) -0.014(4) -0.009(3) C10 0.044(4) 0.054(4) 0.064(4) -0.008(3) -0.015(3) -0.001(3) C11 0.048(4) 0.046(4) 0.071(5) -0.011(3) -0.004(3) 0.006(3) C13 0.075(6) 0.053(5) 0.114(9) 0.020(5) 0.019(5) 0.023(5) C14 0.083(6) 0.065(5) 0.080(7) 0.002(4) 0.028(5) 0.022(5) C15 0.035(3) 0.044(3) 0.029(3) -0.007(2) -0.001(2) 0.006(2) C16 0.028(3) 0.045(3) 0.046(3) -0.007(3) -0.008(2) -0.002(2) C17 0.043(3) 0.040(3) 0.050(4) -0.008(3) 0.001(3) 0.004(2) C18 0.051(4) 0.045(4) 0.060(4) -0.010(3) -0.002(3) 0.002(3) C19 0.048(4) 0.039(3) 0.073(4) 0.004(3) -0.006(4) -0.016(3) C20 0.053(4) 0.068(4) 0.058(4) -0.010(4) 0.012(3) -0.020(3) C21 0.048(3) 0.044(3) 0.063(4) -0.019(3) 0.003(3) -0.007(3) C22 0.087(6) 0.068(5) 0.065(5) -0.028(4) -0.005(4) -0.020(4) C23 0.061(4) 0.051(4) 0.070(5) -0.005(3) 0.003(4) 0.003(3) C24 0.084(6) 0.095(7) 0.051(5) -0.002(4) 0.026(4) 0.000(5) Li1 0.039(6) 0.064(7) 0.062(7) -0.034(6) -0.019(5) 0.001(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 Yb1 O1 2.195(4) . ? Yb1 O1 2.195(4) 11_544 ? Yb1 N2 2.213(9) . ? Yb1 N1 2.307(5) . ? Yb1 N1 2.307(5) 11_544 ? Yb1 Li1 3.056(10) . ? Yb1 Li1 3.056(10) 11_544 ? Yb1 C15 3.145(6) 11_544 ? Yb1 Si1 3.410(2) 11_544 ? Br1 C19 1.891(6) . ? Si1 N2 1.719(5) . ? Si1 C22 1.859(8) . ? Si1 C24 1.875(8) . ? Si1 C23 1.880(8) . ? O1 C1 1.368(7) . ? O1 Li1 1.881(11) 11_544 ? O2 C28' 1.422(9) . ? O2 C25 1.426(9) . ? O2 C25' 1.429(9) . ? O2 C28 1.436(9) . ? O2 Li1 1.819(12) . ? N1 C16 1.386(8) . ? N1 C15 1.490(8) . ? N1 Li1 2.070(12) . ? N2 Si1 1.719(5) 11_544 ? C1 C6 1.395(8) . ? C1 C2 1.420(8) . ? C1 Li1 2.770(13) 11_544 ? C2 C3 1.396(8) . ? C2 C7 1.541(8) . ? C3 C4 1.401(9) . ? C3 H3 0.9400 . ? C4 C5 1.383(9) . ? C4 C11 1.536(9) . ? C5 C6 1.377(9) . ? C5 H5 0.9400 . ? C6 C15 1.513(8) . ? C7 C8 1.521(11) . ? C7 C9 1.518(10) . ? C7 C10 1.564(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.503(13) . ? C11 C14 1.532(12) . ? C11 C12' 1.559(18) . ? C11 C13 1.550(16) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C12' H12D 0.9700 . ? C12' H12E 0.9700 . ? C12' H12F 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15 0.9400 . ? C16 C21 1.412(9) . ? C16 C17 1.410(9) . ? C17 C18 1.391(10) . ? C17 H17 0.9400 . ? C18 C19 1.377(10) . ? C18 H18 0.9400 . ? C19 C20 1.381(10) . ? C20 C21 1.373(9) . ? C20 H20 0.9400 . ? C21 H21 0.9400 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C26 1.439(15) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 C27 1.469(15) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.483(15) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C25' C26' 1.468(17) . ? C25' H25C 0.9800 . ? C25' H25D 0.9800 . ? C26' C27' 1.382(17) . ? C26' H26C 0.9800 . ? C26' H26D 0.9800 . ? C27' C28' 1.481(17) . ? C27' H27C 0.9800 . ? C27' H27D 0.9800 . ? C28' H28C 0.9800 . ? C28' H28D 0.9800 . ? Li1 O1 1.881(11) 11_544 ? Li1 C1 2.770(13) 11_544 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Yb1 O1 149.6(2) . 11_544 ? O1 Yb1 N2 105.21(12) . . ? O1 Yb1 N2 105.21(12) 11_544 . ? O1 Yb1 N1 82.60(15) . . ? O1 Yb1 N1 79.96(15) 11_544 . ? N2 Yb1 N1 125.29(15) . . ? O1 Yb1 N1 79.96(15) . 11_544 ? O1 Yb1 N1 82.60(15) 11_544 11_544 ? N2 Yb1 N1 125.29(15) . 11_544 ? N1 Yb1 N1 109.4(3) . 11_544 ? O1 Yb1 Li1 118.8(3) . . ? O1 Yb1 Li1 37.7(2) 11_544 . ? N2 Yb1 Li1 126.1(3) . . ? N1 Yb1 Li1 42.6(3) . . ? N1 Yb1 Li1 93.1(3) 11_544 . ? O1 Yb1 Li1 37.7(2) . 11_544 ? O1 Yb1 Li1 118.8(3) 11_544 11_544 ? N2 Yb1 Li1 126.1(3) . 11_544 ? N1 Yb1 Li1 93.1(3) . 11_544 ? N1 Yb1 Li1 42.6(3) 11_544 11_544 ? Li1 Yb1 Li1 107.7(5) . 11_544 ? O1 Yb1 C15 96.52(16) . 11_544 ? O1 Yb1 C15 59.43(15) 11_544 11_544 ? N2 Yb1 C15 138.86(11) . 11_544 ? N1 Yb1 C15 91.45(18) . 11_544 ? N1 Yb1 C15 26.44(17) 11_544 11_544 ? Li1 Yb1 C15 67.1(3) . 11_544 ? Li1 Yb1 C15 60.1(2) 11_544 11_544 ? O1 Yb1 Si1 96.29(12) . 11_544 ? O1 Yb1 Si1 111.23(13) 11_544 11_544 ? N2 Yb1 Si1 25.93(4) . 11_544 ? N1 Yb1 Si1 100.50(15) . 11_544 ? N1 Yb1 Si1 148.97(15) 11_544 11_544 ? Li1 Yb1 Si1 115.0(3) . 11_544 ? Li1 Yb1 Si1 129.6(2) 11_544 11_544 ? C15 Yb1 Si1 163.49(12) 11_544 11_544 ? N2 Si1 C22 112.5(3) . . ? N2 Si1 C24 113.3(4) . . ? C22 Si1 C24 107.0(4) . . ? N2 Si1 C23 111.6(4) . . ? C22 Si1 C23 106.9(4) . . ? C24 Si1 C23 104.9(4) . . ? C1 O1 Li1 116.1(5) . 11_544 ? C1 O1 Yb1 129.1(3) . . ? Li1 O1 Yb1 96.9(4) 11_544 . ? C28' O2 C25 112.9(11) . . ? C28' O2 C25' 102.8(13) . . ? C25 O2 C25' 27.1(11) . . ? C28' O2 C28 18.8(12) . . ? C25 O2 C28 109.4(9) . . ? C25' O2 C28 108.3(11) . . ? C28' O2 Li1 130.9(10) . . ? C25 O2 Li1 115.9(8) . . ? C25' O2 Li1 118.6(10) . . ? C28 O2 Li1 132.4(8) . . ? C16 N1 C15 115.7(5) . . ? C16 N1 Li1 89.7(5) . . ? C15 N1 Li1 120.7(5) . . ? C16 N1 Yb1 127.5(4) . . ? C15 N1 Yb1 110.0(4) . . ? Li1 N1 Yb1 88.4(3) . . ? Si1 N2 Si1 120.4(5) 11_544 . ? Si1 N2 Yb1 119.8(3) 11_544 . ? Si1 N2 Yb1 119.8(3) . . ? O1 C1 C6 119.0(5) . . ? O1 C1 C2 121.6(5) . . ? C6 C1 C2 119.3(5) . . ? O1 C1 Li1 37.6(3) . 11_544 ? C6 C1 Li1 107.2(5) . 11_544 ? C2 C1 Li1 119.8(5) . 11_544 ? C3 C2 C1 117.5(5) . . ? C3 C2 C7 121.8(5) . . ? C1 C2 C7 120.8(5) . . ? C2 C3 C4 123.5(5) . . ? C2 C3 H3 118.2 . . ? C4 C3 H3 118.2 . . ? C5 C4 C3 116.7(6) . . ? C5 C4 C11 122.2(6) . . ? C3 C4 C11 121.1(5) . . ? C4 C5 C6 122.2(6) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 120.7(6) . . ? C5 C6 C15 121.4(5) . . ? C1 C6 C15 118.0(5) . . ? C8 C7 C9 110.9(6) . . ? C8 C7 C2 112.0(5) . . ? C9 C7 C2 110.5(6) . . ? C8 C7 C10 106.9(6) . . ? C9 C7 C10 105.8(5) . . ? C2 C7 C10 110.7(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C4 112.5(8) . . ? C12 C11 C14 99.6(10) . . ? C4 C11 C14 110.1(6) . . ? C12 C11 C12' 26.1(8) . . ? C4 C11 C12' 111.7(8) . . ? C14 C11 C12' 121.6(10) . . ? C12 C11 C13 119.0(9) . . ? C4 C11 C13 107.3(7) . . ? C14 C11 C13 107.8(7) . . ? C12' C11 C13 96.6(9) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? C11 C12' H12D 109.5 . . ? C11 C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C11 C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C6 114.0(5) . . ? N1 C15 H15 123.0 . . ? C6 C15 H15 123.0 . . ? N1 C16 C21 117.6(5) . . ? N1 C16 C17 126.1(6) . . ? C21 C16 C17 116.3(6) . . ? C18 C17 C16 121.0(6) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C19 C18 C17 120.8(6) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 119.2(6) . . ? C18 C19 Br1 120.0(5) . . ? C20 C19 Br1 120.8(6) . . ? C21 C20 C19 120.6(7) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C16 121.9(6) . . ? C20 C21 H21 119.1 . . ? C16 C21 H21 119.1 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O2 C25 C26 107.5(11) . . ? O2 C25 H25A 110.2 . . ? C26 C25 H25A 110.2 . . ? O2 C25 H25B 110.2 . . ? C26 C25 H25B 110.2 . . ? H25A C25 H25B 108.5 . . ? C25 C26 C27 108.9(12) . . ? C25 C26 H26A 109.9 . . ? C27 C26 H26A 109.9 . . ? C25 C26 H26B 109.9 . . ? C27 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? C26 C27 C28 104.7(12) . . ? C26 C27 H27A 110.8 . . ? C28 C27 H27A 110.8 . . ? C26 C27 H27B 110.8 . . ? C28 C27 H27B 110.8 . . ? H27A C27 H27B 108.9 . . ? O2 C28 C27 107.1(11) . . ? O2 C28 H28A 110.3 . . ? C27 C28 H28A 110.3 . . ? O2 C28 H28B 110.3 . . ? C27 C28 H28B 110.3 . . ? H28A C28 H28B 108.5 . . ? O2 C25' C26' 109.5(15) . . ? O2 C25' H25C 109.8 . . ? C26' C25' H25C 109.8 . . ? O2 C25' H25D 109.8 . . ? C26' C25' H25D 109.8 . . ? H25C C25' H25D 108.2 . . ? C27' C26' C25' 99.3(18) . . ? C27' C26' H26C 111.9 . . ? C25' C26' H26C 111.9 . . ? C27' C26' H26D 111.9 . . ? C25' C26' H26D 111.9 . . ? H26C C26' H26D 109.6 . . ? C26' C27' C28' 111.8(18) . . ? C26' C27' H27C 109.3 . . ? C28' C27' H27C 109.3 . . ? C26' C27' H27D 109.3 . . ? C28' C27' H27D 109.3 . . ? H27C C27' H27D 107.9 . . ? O2 C28' C27' 105.1(15) . . ? O2 C28' H28C 110.7 . . ? C27' C28' H28C 110.7 . . ? O2 C28' H28D 110.7 . . ? C27' C28' H28D 110.7 . . ? H28C C28' H28D 108.8 . . ? O2 Li1 O1 134.3(7) . 11_544 ? O2 Li1 N1 125.7(6) . . ? O1 Li1 N1 94.1(5) 11_544 . ? O2 Li1 C1 108.1(6) . 11_544 ? O1 Li1 C1 26.3(3) 11_544 11_544 ? N1 Li1 C1 115.7(4) . 11_544 ? O2 Li1 Yb1 155.5(7) . . ? O1 Li1 Yb1 45.5(2) 11_544 . ? N1 Li1 Yb1 49.0(2) . . ? C1 Li1 Yb1 67.3(3) 11_544 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Yb1 O1 C1 -82.3(5) 11_544 . . . ? N2 Yb1 O1 C1 97.7(5) . . . . ? N1 Yb1 O1 C1 -27.0(5) . . . . ? N1 Yb1 O1 C1 -138.3(5) 11_544 . . . ? Li1 Yb1 O1 C1 -50.3(6) . . . . ? Li1 Yb1 O1 C1 -132.0(7) 11_544 . . . ? C15 Yb1 O1 C1 -117.6(5) 11_544 . . . ? Si1 Yb1 O1 C1 72.8(5) 11_544 . . . ? O1 Yb1 O1 Li1 49.6(5) 11_544 . . 11_544 ? N2 Yb1 O1 Li1 -130.4(5) . . . 11_544 ? N1 Yb1 O1 Li1 105.0(5) . . . 11_544 ? N1 Yb1 O1 Li1 -6.3(5) 11_544 . . 11_544 ? Li1 Yb1 O1 Li1 81.7(8) . . . 11_544 ? C15 Yb1 O1 Li1 14.4(5) 11_544 . . 11_544 ? Si1 Yb1 O1 Li1 -155.2(5) 11_544 . . 11_544 ? O1 Yb1 N1 C16 122.4(5) . . . . ? O1 Yb1 N1 C16 -82.6(4) 11_544 . . . ? N2 Yb1 N1 C16 19.0(5) . . . . ? N1 Yb1 N1 C16 -161.0(5) 11_544 . . . ? Li1 Yb1 N1 C16 -88.3(6) . . . . ? Li1 Yb1 N1 C16 158.6(5) 11_544 . . . ? C15 Yb1 N1 C16 -141.2(4) 11_544 . . . ? Si1 Yb1 N1 C16 27.3(4) 11_544 . . . ? O1 Yb1 N1 C15 -27.0(3) . . . . ? O1 Yb1 N1 C15 127.9(4) 11_544 . . . ? N2 Yb1 N1 C15 -130.5(3) . . . . ? N1 Yb1 N1 C15 49.5(3) 11_544 . . . ? Li1 Yb1 N1 C15 122.2(6) . . . . ? Li1 Yb1 N1 C15 9.2(4) 11_544 . . . ? C15 Yb1 N1 C15 69.4(4) 11_544 . . . ? Si1 Yb1 N1 C15 -122.1(3) 11_544 . . . ? O1 Yb1 N1 Li1 -149.3(5) . . . . ? O1 Yb1 N1 Li1 5.7(4) 11_544 . . . ? N2 Yb1 N1 Li1 107.3(4) . . . . ? N1 Yb1 N1 Li1 -72.7(4) 11_544 . . . ? Li1 Yb1 N1 Li1 -113.0(6) 11_544 . . . ? C15 Yb1 N1 Li1 -52.9(4) 11_544 . . . ? Si1 Yb1 N1 Li1 115.7(4) 11_544 . . . ? C22 Si1 N2 Si1 79.2(3) . . . 11_544 ? C24 Si1 N2 Si1 -42.4(4) . . . 11_544 ? C23 Si1 N2 Si1 -160.6(3) . . . 11_544 ? C22 Si1 N2 Yb1 -100.8(3) . . . . ? C24 Si1 N2 Yb1 137.6(4) . . . . ? C23 Si1 N2 Yb1 19.4(3) . . . . ? O1 Yb1 N2 Si1 -72.59(12) . . . 11_544 ? O1 Yb1 N2 Si1 107.41(12) 11_544 . . 11_544 ? N1 Yb1 N2 Si1 19.06(16) . . . 11_544 ? N1 Yb1 N2 Si1 -160.94(16) 11_544 . . 11_544 ? Li1 Yb1 N2 Si1 72.2(3) . . . 11_544 ? Li1 Yb1 N2 Si1 -107.8(3) 11_544 . . 11_544 ? C15 Yb1 N2 Si1 168.07(18) 11_544 . . 11_544 ? O1 Yb1 N2 Si1 107.41(13) . . . . ? O1 Yb1 N2 Si1 -72.59(13) 11_544 . . . ? N1 Yb1 N2 Si1 -160.94(16) . . . . ? N1 Yb1 N2 Si1 19.06(16) 11_544 . . . ? Li1 Yb1 N2 Si1 -107.8(3) . . . . ? Li1 Yb1 N2 Si1 72.2(3) 11_544 . . . ? C15 Yb1 N2 Si1 -11.93(18) 11_544 . . . ? Si1 Yb1 N2 Si1 180.000(2) 11_544 . . . ? Li1 O1 C1 C6 -80.3(7) 11_544 . . . ? Yb1 O1 C1 C6 44.4(7) . . . . ? Li1 O1 C1 C2 99.0(7) 11_544 . . . ? Yb1 O1 C1 C2 -136.3(5) . . . . ? Yb1 O1 C1 Li1 124.7(7) . . . 11_544 ? O1 C1 C2 C3 177.3(5) . . . . ? C6 C1 C2 C3 -3.4(8) . . . . ? Li1 C1 C2 C3 -138.8(5) 11_544 . . . ? O1 C1 C2 C7 -2.6(8) . . . . ? C6 C1 C2 C7 176.7(5) . . . . ? Li1 C1 C2 C7 41.3(7) 11_544 . . . ? C1 C2 C3 C4 1.7(9) . . . . ? C7 C2 C3 C4 -178.5(6) . . . . ? C2 C3 C4 C5 1.3(10) . . . . ? C2 C3 C4 C11 -178.6(6) . . . . ? C3 C4 C5 C6 -2.6(10) . . . . ? C11 C4 C5 C6 177.4(6) . . . . ? C4 C5 C6 C1 0.8(10) . . . . ? C4 C5 C6 C15 -178.8(6) . . . . ? O1 C1 C6 C5 -178.4(6) . . . . ? C2 C1 C6 C5 2.3(9) . . . . ? Li1 C1 C6 C5 142.7(6) 11_544 . . . ? O1 C1 C6 C15 1.3(8) . . . . ? C2 C1 C6 C15 -178.0(5) . . . . ? Li1 C1 C6 C15 -37.7(6) 11_544 . . . ? C3 C2 C7 C8 -118.4(7) . . . . ? C1 C2 C7 C8 61.4(7) . . . . ? C3 C2 C7 C9 117.5(7) . . . . ? C1 C2 C7 C9 -62.7(7) . . . . ? C3 C2 C7 C10 0.7(8) . . . . ? C1 C2 C7 C10 -179.5(6) . . . . ? C5 C4 C11 C12 11.2(12) . . . . ? C3 C4 C11 C12 -168.9(9) . . . . ? C5 C4 C11 C14 121.3(8) . . . . ? C3 C4 C11 C14 -58.8(10) . . . . ? C5 C4 C11 C12' -17.0(12) . . . . ? C3 C4 C11 C12' 163.0(10) . . . . ? C5 C4 C11 C13 -121.6(8) . . . . ? C3 C4 C11 C13 58.3(9) . . . . ? C16 N1 C15 C6 -80.9(6) . . . . ? Li1 N1 C15 C6 172.9(5) . . . . ? Yb1 N1 C15 C6 72.4(5) . . . . ? C5 C6 C15 N1 114.6(7) . . . . ? C1 C6 C15 N1 -65.1(7) . . . . ? C15 N1 C16 C21 177.2(5) . . . . ? Li1 N1 C16 C21 -58.5(6) . . . . ? Yb1 N1 C16 C21 29.2(7) . . . . ? C15 N1 C16 C17 -2.7(8) . . . . ? Li1 N1 C16 C17 121.7(7) . . . . ? Yb1 N1 C16 C17 -150.6(5) . . . . ? N1 C16 C17 C18 178.3(6) . . . . ? C21 C16 C17 C18 -1.5(9) . . . . ? C16 C17 C18 C19 -2.4(10) . . . . ? C17 C18 C19 C20 4.6(10) . . . . ? C17 C18 C19 Br1 -176.8(5) . . . . ? C18 C19 C20 C21 -2.9(11) . . . . ? Br1 C19 C20 C21 178.5(6) . . . . ? C19 C20 C21 C16 -1.1(11) . . . . ? N1 C16 C21 C20 -176.6(6) . . . . ? C17 C16 C21 C20 3.3(10) . . . . ? C28' O2 C25 C26 -16(2) . . . . ? C25' O2 C25 C26 -89(3) . . . . ? C28 O2 C25 C26 3.7(17) . . . . ? Li1 O2 C25 C26 168.6(11) . . . . ? O2 C25 C26 C27 6.3(19) . . . . ? C25 C26 C27 C28 -13.2(19) . . . . ? C28' O2 C28 C27 92(4) . . . . ? C25 O2 C28 C27 -12.0(16) . . . . ? C25' O2 C28 C27 16.7(18) . . . . ? Li1 O2 C28 C27 -173.6(10) . . . . ? C26 C27 C28 O2 15.2(17) . . . . ? C28' O2 C25' C26' -33(2) . . . . ? C25 O2 C25' C26' 82(3) . . . . ? C28 O2 C25' C26' -15(2) . . . . ? Li1 O2 C25' C26' 174.0(15) . . . . ? O2 C25' C26' C27' 34(3) . . . . ? C25' C26' C27' C28' -21(3) . . . . ? C25 O2 C28' C27' -8(2) . . . . ? C25' O2 C28' C27' 18(2) . . . . ? C28 O2 C28' C27' -91(4) . . . . ? Li1 O2 C28' C27' 166.2(13) . . . . ? C26' C27' C28' O2 2(3) . . . . ? C28' O2 Li1 O1 -12(2) . . . 11_544 ? C25 O2 Li1 O1 162.2(12) . . . 11_544 ? C25' O2 Li1 O1 131.7(15) . . . 11_544 ? C28 O2 Li1 O1 -37.2(18) . . . 11_544 ? C28' O2 Li1 N1 -157.5(15) . . . . ? C25 O2 Li1 N1 16.7(14) . . . . ? C25' O2 Li1 N1 -13.7(17) . . . . ? C28 O2 Li1 N1 177.4(11) . . . . ? C28' O2 Li1 C1 -14.6(16) . . . 11_544 ? C25 O2 Li1 C1 159.6(10) . . . 11_544 ? C25' O2 Li1 C1 129.1(13) . . . 11_544 ? C28 O2 Li1 C1 -39.7(14) . . . 11_544 ? C28' O2 Li1 Yb1 -89(2) . . . . ? C25 O2 Li1 Yb1 84.9(18) . . . . ? C25' O2 Li1 Yb1 54(2) . . . . ? C28 O2 Li1 Yb1 -114.4(16) . . . . ? C16 N1 Li1 O2 -83.1(9) . . . . ? C15 N1 Li1 O2 37.0(11) . . . . ? Yb1 N1 Li1 O2 149.4(9) . . . . ? C16 N1 Li1 O1 120.9(6) . . . 11_544 ? C15 N1 Li1 O1 -119.0(6) . . . 11_544 ? Yb1 N1 Li1 O1 -6.6(5) . . . 11_544 ? C16 N1 Li1 C1 136.5(6) . . . 11_544 ? C15 N1 Li1 C1 -103.4(6) . . . 11_544 ? Yb1 N1 Li1 C1 9.0(6) . . . 11_544 ? C16 N1 Li1 Yb1 127.5(4) . . . . ? C15 N1 Li1 Yb1 -112.4(5) . . . . ? O1 Yb1 Li1 O2 -52.1(15) . . . . ? O1 Yb1 Li1 O2 101.8(16) 11_544 . . . ? N2 Yb1 Li1 O2 167.3(13) . . . . ? N1 Yb1 Li1 O2 -87.4(14) . . . . ? N1 Yb1 Li1 O2 28.2(15) 11_544 . . . ? Li1 Yb1 Li1 O2 -12.7(13) 11_544 . . . ? C15 Yb1 Li1 O2 32.6(14) 11_544 . . . ? Si1 Yb1 Li1 O2 -165.3(14) 11_544 . . . ? O1 Yb1 Li1 O1 -153.9(3) . . . 11_544 ? N2 Yb1 Li1 O1 65.5(5) . . . 11_544 ? N1 Yb1 Li1 O1 170.8(7) . . . 11_544 ? N1 Yb1 Li1 O1 -73.6(4) 11_544 . . 11_544 ? Li1 Yb1 Li1 O1 -114.5(5) 11_544 . . 11_544 ? C15 Yb1 Li1 O1 -69.2(4) 11_544 . . 11_544 ? Si1 Yb1 Li1 O1 92.9(4) 11_544 . . 11_544 ? O1 Yb1 Li1 N1 35.3(5) . . . . ? O1 Yb1 Li1 N1 -170.8(7) 11_544 . . . ? N2 Yb1 Li1 N1 -105.2(3) . . . . ? N1 Yb1 Li1 N1 115.6(4) 11_544 . . . ? Li1 Yb1 Li1 N1 74.8(3) 11_544 . . . ? C15 Yb1 Li1 N1 120.0(4) 11_544 . . . ? Si1 Yb1 Li1 N1 -77.9(4) 11_544 . . . ? O1 Yb1 Li1 C1 -135.9(2) . . . 11_544 ? O1 Yb1 Li1 C1 18.0(3) 11_544 . . 11_544 ? N2 Yb1 Li1 C1 83.5(3) . . . 11_544 ? N1 Yb1 Li1 C1 -171.2(6) . . . 11_544 ? N1 Yb1 Li1 C1 -55.6(3) 11_544 . . 11_544 ? Li1 Yb1 Li1 C1 -96.5(3) 11_544 . . 11_544 ? C15 Yb1 Li1 C1 -51.2(2) 11_544 . . 11_544 ? Si1 Yb1 Li1 C1 110.9(3) 11_544 . . 11_544 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.702 _refine_diff_density_min -0.884 _refine_diff_density_rms 0.081 _database_code_depnum_ccdc_archive 'CCDC 932404' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H86 Cl2 Li2 N3 O4 Si2 Y' _chemical_formula_sum 'C56 H86 Cl2 Li2 N3 O4 Si2 Y' _chemical_formula_weight 1095.15 _chemical_absolute_configuration ad 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.8454(4) _cell_length_b 21.7412(8) _cell_length_c 23.3527(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6014.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4405 _cell_measurement_theta_min 3.3019 _cell_measurement_theta_max 26.3108 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.80 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 1.142 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.74543 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4692 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20523 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_unetI/netI 0.1255 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 26.37 _reflns_number_total 12098 _reflns_number_gt 7733 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.027(5) _refine_ls_number_reflns 12098 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1082 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.0911 _refine_ls_wR_factor_gt 0.0808 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _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 Y1 Y 0.49728(3) 0.520395(16) 0.214404(15) 0.02171(9) Uani 1 1 d . . . O1 O 0.57943(19) 0.50299(11) 0.29846(10) 0.0250(7) Uani 1 1 d . . . O2 O 0.41459(18) 0.46283(11) 0.14642(10) 0.0234(6) Uani 1 1 d . . . O3 O 0.4380(2) 0.40472(13) 0.38470(13) 0.0426(8) Uani 1 1 d . . . O4 O 0.5625(2) 0.33946(14) 0.10616(14) 0.0480(9) Uani 1 1 d . . . N1 N 0.6532(2) 0.45572(14) 0.18647(13) 0.0249(8) Uani 1 1 d . . . N2 N 0.3409(2) 0.47676(15) 0.26784(12) 0.0243(8) Uani 1 1 d . . . N3 N 0.5091(3) 0.62024(13) 0.19053(13) 0.0370(8) Uani 1 1 d . . . Si1 Si 0.63301(13) 0.66075(6) 0.19628(6) 0.0526(4) Uani 1 1 d . . . Si2 Si 0.38753(13) 0.65443(6) 0.16549(6) 0.0495(4) Uani 1 1 d . . . Cl1 Cl 0.61891(8) 0.52979(6) 0.08213(4) 0.0400(3) Uani 1 1 d . . . Cl2 Cl 0.37558(9) 0.59625(5) 0.32254(5) 0.0430(3) Uani 1 1 d . . . Li1 Li 0.4494(5) 0.4737(4) 0.3355(3) 0.0350(17) Uani 1 1 d . . . Li2 Li 0.5460(5) 0.4234(4) 0.1237(3) 0.0363(19) Uani 1 1 d . . . C1 C 0.6731(3) 0.47402(19) 0.31908(16) 0.0221(9) Uani 1 1 d . . . C2 C 0.7240(3) 0.49102(18) 0.37195(16) 0.0223(9) Uani 1 1 d . . . C3 C 0.8054(3) 0.45130(19) 0.39398(17) 0.0267(10) Uani 1 1 d . . . H3 H 0.8364 0.4608 0.4295 0.032 Uiso 1 1 calc R . . C4 C 0.8436(3) 0.39823(19) 0.36663(18) 0.0303(11) Uani 1 1 d . . . C5 C 0.7991(3) 0.38641(18) 0.31265(18) 0.0276(10) Uani 1 1 d . . . H5 H 0.8252 0.3525 0.2922 0.033 Uiso 1 1 calc R . . C6 C 0.7163(3) 0.42406(17) 0.28812(18) 0.0237(9) Uani 1 1 d . . . C7 C 0.6903(3) 0.54903(19) 0.40545(17) 0.0288(10) Uani 1 1 d . . . C8 C 0.7753(4) 0.5641(2) 0.45350(19) 0.0444(13) Uani 1 1 d . . . H8A H 0.7749 0.5316 0.4814 0.067 Uiso 1 1 calc R . . H8B H 0.7544 0.6021 0.4716 0.067 Uiso 1 1 calc R . . H8C H 0.8496 0.5679 0.4375 0.067 Uiso 1 1 calc R . . C9 C 0.6838(3) 0.60498(19) 0.36641(18) 0.0363(11) Uani 1 1 d . . . H9A H 0.7549 0.6105 0.3474 0.054 Uiso 1 1 calc R . . H9B H 0.6669 0.6408 0.3888 0.054 Uiso 1 1 calc R . . H9C H 0.6255 0.5989 0.3384 0.054 Uiso 1 1 calc R . . C10 C 0.5746(3) 0.5397(2) 0.43535(18) 0.0391(12) Uani 1 1 d . . . H10A H 0.5166 0.5357 0.4069 0.059 Uiso 1 1 calc R . . H10B H 0.5586 0.5746 0.4592 0.059 Uiso 1 1 calc R . . H10C H 0.5771 0.5032 0.4584 0.059 Uiso 1 1 calc R . . C11 C 0.9276(3) 0.3540(2) 0.3959(2) 0.0392(12) Uani 1 1 d . . . C12 C 0.8622(5) 0.3158(3) 0.4390(3) 0.091(2) Uani 1 1 d . . . H12A H 0.9121 0.2866 0.4566 0.136 Uiso 1 1 calc R . . H12B H 0.8024 0.2943 0.4198 0.136 Uiso 1 1 calc R . . H12C H 0.8309 0.3422 0.4678 0.136 Uiso 1 1 calc R . . C13 C 0.9854(5) 0.3130(3) 0.3536(2) 0.087(2) Uani 1 1 d . . . H13A H 1.0214 0.3376 0.3248 0.131 Uiso 1 1 calc R . . H13B H 0.9308 0.2864 0.3360 0.131 Uiso 1 1 calc R . . H13C H 1.0411 0.2886 0.3730 0.131 Uiso 1 1 calc R . . C14 C 1.0168(4) 0.3897(2) 0.4281(2) 0.0608(15) Uani 1 1 d . . . H14A H 1.0567 0.4160 0.4020 0.091 Uiso 1 1 calc R . . H14B H 1.0689 0.3616 0.4456 0.091 Uiso 1 1 calc R . . H14C H 0.9815 0.4142 0.4573 0.091 Uiso 1 1 calc R . . C15 C 0.6655(3) 0.40706(19) 0.23017(18) 0.0285(11) Uani 1 1 d . . . H15A H 0.7116 0.3746 0.2138 0.034 Uiso 1 1 calc R . . H15B H 0.5913 0.3897 0.2371 0.034 Uiso 1 1 calc R . . C16 C 0.7540(3) 0.47181(19) 0.15897(16) 0.0265(10) Uani 1 1 d . . . C17 C 0.7520(3) 0.5083(2) 0.10923(18) 0.0323(11) Uani 1 1 d . . . C18 C 0.8459(3) 0.5291(2) 0.08073(17) 0.0367(11) Uani 1 1 d . . . H18 H 0.8387 0.5537 0.0484 0.044 Uiso 1 1 calc R . . C19 C 0.9506(3) 0.5129(2) 0.1009(2) 0.0499(13) Uani 1 1 d . . . H19 H 1.0153 0.5272 0.0828 0.060 Uiso 1 1 calc R . . C20 C 0.9588(3) 0.4755(2) 0.1478(2) 0.0456(12) Uani 1 1 d . . . H20 H 1.0297 0.4631 0.1605 0.055 Uiso 1 1 calc R . . C21 C 0.8638(3) 0.45577(19) 0.17656(18) 0.0341(11) Uani 1 1 d . . . H21 H 0.8726 0.4310 0.2087 0.041 Uiso 1 1 calc R . . C22 C 0.3204(3) 0.42770(18) 0.14070(18) 0.0256(10) Uani 1 1 d . . . C23 C 0.2689(3) 0.41634(19) 0.08696(18) 0.0285(10) Uani 1 1 d . . . C24 C 0.1831(3) 0.3718(2) 0.08594(19) 0.0349(11) Uani 1 1 d . . . H24 H 0.1511 0.3625 0.0506 0.042 Uiso 1 1 calc R . . C25 C 0.1422(3) 0.34051(19) 0.13303(19) 0.0299(10) Uani 1 1 d . . . C26 C 0.1906(3) 0.35598(18) 0.18554(19) 0.0288(10) Uani 1 1 d . . . H26 H 0.1649 0.3366 0.2186 0.035 Uiso 1 1 calc R . . C27 C 0.2763(3) 0.39957(18) 0.19005(17) 0.0234(10) Uani 1 1 d . . . C28 C 0.3033(3) 0.4482(2) 0.03082(18) 0.0318(11) Uani 1 1 d . . . C29 C 0.3150(4) 0.5177(2) 0.03955(18) 0.0422(11) Uani 1 1 d . . . H29A H 0.2445 0.5343 0.0526 0.063 Uiso 1 1 calc R . . H29B H 0.3355 0.5368 0.0039 0.063 Uiso 1 1 calc R . . H29C H 0.3725 0.5257 0.0676 0.063 Uiso 1 1 calc R . . C30 C 0.4152(4) 0.4224(2) 0.00734(19) 0.0497(14) Uani 1 1 d . . . H30A H 0.4749 0.4310 0.0339 0.075 Uiso 1 1 calc R . . H30B H 0.4319 0.4415 -0.0288 0.075 Uiso 1 1 calc R . . H30C H 0.4086 0.3788 0.0022 0.075 Uiso 1 1 calc R . . C31 C 0.2149(4) 0.4390(2) -0.01729(19) 0.0552(15) Uani 1 1 d . . . H31A H 0.2139 0.3966 -0.0287 0.083 Uiso 1 1 calc R . . H31B H 0.2344 0.4642 -0.0495 0.083 Uiso 1 1 calc R . . H31C H 0.1416 0.4505 -0.0034 0.083 Uiso 1 1 calc R . . C32 C 0.0546(4) 0.2906(3) 0.1268(3) 0.0775(10) Uani 1 1 d . . . C33 C 0.1096(4) 0.2319(2) 0.1074(3) 0.0775(10) Uani 1 1 d . . . H33A H 0.1507 0.2393 0.0727 0.116 Uiso 1 1 calc R . . H33B H 0.0526 0.2013 0.1007 0.116 Uiso 1 1 calc R . . H33C H 0.1604 0.2177 0.1366 0.116 Uiso 1 1 calc R . . C34 C -0.0355(4) 0.3081(3) 0.0821(3) 0.0775(10) Uani 1 1 d . . . H34A H -0.0711 0.3459 0.0931 0.116 Uiso 1 1 calc R . . H34B H -0.0912 0.2761 0.0800 0.116 Uiso 1 1 calc R . . H34C H -0.0004 0.3130 0.0453 0.116 Uiso 1 1 calc R . . C35 C -0.0095(5) 0.2773(2) 0.1819(2) 0.0775(10) Uani 1 1 d . . . H35A H 0.0416 0.2610 0.2100 0.116 Uiso 1 1 calc R . . H35B H -0.0680 0.2478 0.1744 0.116 Uiso 1 1 calc R . . H35C H -0.0425 0.3146 0.1961 0.116 Uiso 1 1 calc R . . C36 C 0.3295(3) 0.41218(19) 0.24814(18) 0.0280(11) Uani 1 1 d . . . H36A H 0.2857 0.3902 0.2767 0.034 Uiso 1 1 calc R . . H36B H 0.4044 0.3941 0.2479 0.034 Uiso 1 1 calc R . . C37 C 0.2418(3) 0.50351(17) 0.28696(17) 0.0250(9) Uani 1 1 d . . . C38 C 0.2434(3) 0.56091(19) 0.31431(17) 0.0292(10) Uani 1 1 d . . . C39 C 0.1506(3) 0.5914(2) 0.33414(19) 0.0402(12) Uani 1 1 d . . . H39 H 0.1584 0.6294 0.3519 0.048 Uiso 1 1 calc R . . C40 C 0.0444(4) 0.5652(2) 0.3277(2) 0.0475(13) Uani 1 1 d . . . H40 H -0.0202 0.5857 0.3400 0.057 Uiso 1 1 calc R . . C41 C 0.0376(3) 0.5086(2) 0.30289(19) 0.0450(13) Uani 1 1 d . . . H41 H -0.0325 0.4897 0.2994 0.054 Uiso 1 1 calc R . . C42 C 0.1326(3) 0.4785(2) 0.28276(17) 0.0349(10) Uani 1 1 d . . . H42 H 0.1238 0.4402 0.2657 0.042 Uiso 1 1 calc R . . C43 C 0.7537(4) 0.6114(2) 0.2192(2) 0.0501(13) Uani 1 1 d . . . H43A H 0.7258 0.5774 0.2413 0.075 Uiso 1 1 calc R . . H43B H 0.8049 0.6352 0.2420 0.075 Uiso 1 1 calc R . . H43C H 0.7924 0.5961 0.1860 0.075 Uiso 1 1 calc R . . C44 C 0.6791(5) 0.6978(3) 0.1277(3) 0.096(2) Uani 1 1 d . . . H44A H 0.6819 0.6674 0.0979 0.144 Uiso 1 1 calc R . . H44B H 0.7526 0.7156 0.1327 0.144 Uiso 1 1 calc R . . H44C H 0.6263 0.7294 0.1173 0.144 Uiso 1 1 calc R . . C45 C 0.6244(5) 0.7252(2) 0.2499(3) 0.090(2) Uani 1 1 d . . . H45A H 0.5901 0.7605 0.2323 0.135 Uiso 1 1 calc R . . H45B H 0.6990 0.7356 0.2627 0.135 Uiso 1 1 calc R . . H45C H 0.5798 0.7123 0.2820 0.135 Uiso 1 1 calc R . . C46 C 0.2631(4) 0.6010(2) 0.1708(2) 0.0556(14) Uani 1 1 d . . . H46A H 0.2864 0.5600 0.1613 0.083 Uiso 1 1 calc R . . H46B H 0.2053 0.6141 0.1447 0.083 Uiso 1 1 calc R . . H46C H 0.2340 0.6017 0.2092 0.083 Uiso 1 1 calc R . . C47 C 0.3443(5) 0.7262(2) 0.2056(3) 0.086(2) Uani 1 1 d . . . H47A H 0.3448 0.7180 0.2460 0.129 Uiso 1 1 calc R . . H47B H 0.2697 0.7382 0.1940 0.129 Uiso 1 1 calc R . . H47C H 0.3964 0.7588 0.1972 0.129 Uiso 1 1 calc R . . C48 C 0.3970(5) 0.6774(2) 0.0878(2) 0.0766(19) Uani 1 1 d . . . H48A H 0.4553 0.7077 0.0831 0.115 Uiso 1 1 calc R . . H48B H 0.3261 0.6943 0.0756 0.115 Uiso 1 1 calc R . . H48C H 0.4144 0.6419 0.0650 0.115 Uiso 1 1 calc R . . C49 C 0.5253(4) 0.3649(2) 0.4065(2) 0.0565(15) Uani 1 1 d . . . H49A H 0.5976 0.3858 0.4066 0.068 Uiso 1 1 calc R . . H49B H 0.5316 0.3281 0.3832 0.068 Uiso 1 1 calc R . . C50 C 0.4912(6) 0.3487(3) 0.4656(2) 0.0720(16) Uani 1 1 d . . . H50A H 0.5228 0.3775 0.4930 0.086 Uiso 1 1 calc R . . H50B H 0.5160 0.3075 0.4754 0.086 Uiso 1 1 calc R . . C51 C 0.3653(5) 0.3526(3) 0.4648(2) 0.0798(19) Uani 1 1 d . . . H51A H 0.3323 0.3118 0.4653 0.096 Uiso 1 1 calc R . . H51B H 0.3380 0.3752 0.4978 0.096 Uiso 1 1 calc R . . C52 C 0.3352(4) 0.3851(3) 0.4112(3) 0.0703(18) Uani 1 1 d . . . H52A H 0.2942 0.3577 0.3859 0.084 Uiso 1 1 calc R . . H52B H 0.2878 0.4203 0.4196 0.084 Uiso 1 1 calc R . . C53 C 0.4833(6) 0.2917(2) 0.1120(3) 0.102(2) Uani 1 1 d . . . H53A H 0.4165 0.3007 0.0895 0.123 Uiso 1 1 calc R . . H53B H 0.4610 0.2876 0.1518 0.123 Uiso 1 1 calc R . . C54 C 0.5343(5) 0.2356(3) 0.0925(3) 0.103(3) Uani 1 1 d . . . H54A H 0.5030 0.2235 0.0558 0.124 Uiso 1 1 calc R . . H54B H 0.5215 0.2028 0.1198 0.124 Uiso 1 1 calc R . . C55 C 0.6558(5) 0.2487(3) 0.0871(4) 0.105(3) Uani 1 1 d . . . H55A H 0.6971 0.2315 0.1192 0.126 Uiso 1 1 calc R . . H55B H 0.6856 0.2314 0.0519 0.126 Uiso 1 1 calc R . . C56 C 0.6647(5) 0.3144(3) 0.0866(3) 0.103(3) Uani 1 1 d . . . H56A H 0.7262 0.3275 0.1112 0.123 Uiso 1 1 calc R . . H56B H 0.6802 0.3287 0.0480 0.123 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 Y1 0.02142(17) 0.02438(17) 0.01932(19) 0.0009(2) -0.0025(2) 0.0001(2) O1 0.0227(13) 0.0364(17) 0.0158(16) 0.0029(12) -0.0037(11) 0.0020(12) O2 0.0170(13) 0.0334(17) 0.0199(16) -0.0019(13) -0.0040(11) -0.0055(12) O3 0.0368(17) 0.047(2) 0.044(2) 0.0137(17) -0.0009(15) -0.0014(15) O4 0.0447(19) 0.0388(19) 0.060(2) -0.0141(18) -0.0045(17) 0.0027(17) N1 0.0235(18) 0.032(2) 0.019(2) 0.0007(16) -0.0024(15) 0.0022(15) N2 0.0230(17) 0.0285(18) 0.021(2) 0.0031(17) -0.0039(13) 0.0012(17) N3 0.060(2) 0.0237(17) 0.027(2) 0.0029(15) 0.004(2) -0.001(2) Si1 0.0798(10) 0.0325(8) 0.0455(10) 0.0039(7) 0.0078(8) -0.0144(8) Si2 0.0833(11) 0.0332(8) 0.0322(9) 0.0031(7) -0.0027(8) 0.0148(7) Cl1 0.0302(5) 0.0592(8) 0.0305(7) 0.0102(6) -0.0004(5) 0.0044(6) Cl2 0.0332(6) 0.0423(7) 0.0536(9) -0.0144(6) -0.0017(6) -0.0030(5) Li1 0.034(3) 0.046(4) 0.025(4) 0.002(4) -0.002(3) -0.005(4) Li2 0.027(4) 0.057(5) 0.025(5) -0.008(4) -0.006(3) 0.006(3) C1 0.0160(19) 0.030(2) 0.020(2) 0.005(2) -0.0001(17) -0.006(2) C2 0.0166(19) 0.031(2) 0.020(2) 0.001(2) 0.0026(17) -0.0032(18) C3 0.024(2) 0.036(3) 0.020(3) -0.002(2) -0.0028(19) -0.006(2) C4 0.026(2) 0.038(3) 0.027(3) 0.007(2) -0.0087(19) 0.000(2) C5 0.029(2) 0.026(2) 0.028(3) -0.002(2) 0.000(2) 0.0006(19) C6 0.018(2) 0.035(2) 0.019(2) 0.005(2) -0.0028(19) -0.0059(18) C7 0.027(2) 0.040(3) 0.020(3) -0.005(2) -0.0037(19) -0.002(2) C8 0.042(3) 0.057(3) 0.034(3) -0.017(3) -0.010(2) 0.001(2) C9 0.040(3) 0.037(3) 0.032(3) -0.007(2) 0.000(2) -0.001(2) C10 0.033(2) 0.051(3) 0.033(3) -0.006(2) 0.003(2) -0.005(2) C11 0.035(3) 0.045(3) 0.037(3) 0.007(3) -0.012(2) 0.007(2) C12 0.069(4) 0.098(5) 0.106(5) 0.071(4) -0.025(4) 0.008(4) C13 0.103(4) 0.097(4) 0.062(4) -0.021(3) -0.042(4) 0.065(4) C14 0.039(3) 0.071(4) 0.073(4) 0.008(3) -0.029(3) 0.009(3) C15 0.028(2) 0.026(2) 0.032(3) -0.004(2) -0.003(2) 0.0017(19) C16 0.030(2) 0.030(2) 0.019(2) -0.009(2) -0.0030(18) 0.002(2) C17 0.028(2) 0.044(3) 0.025(3) -0.009(2) -0.0009(19) -0.002(2) C18 0.035(3) 0.053(3) 0.021(2) 0.003(2) 0.0030(19) -0.007(2) C19 0.033(2) 0.079(4) 0.038(3) 0.001(3) 0.009(2) -0.012(3) C20 0.024(2) 0.074(3) 0.039(3) -0.004(3) 0.001(2) 0.010(2) C21 0.029(2) 0.045(3) 0.028(3) 0.000(2) -0.005(2) 0.005(2) C22 0.021(2) 0.029(2) 0.026(3) 0.000(2) -0.005(2) 0.006(2) C23 0.021(2) 0.036(3) 0.029(3) -0.006(2) -0.0052(19) 0.005(2) C24 0.029(2) 0.049(3) 0.027(3) -0.010(2) -0.006(2) -0.001(2) C25 0.022(2) 0.032(2) 0.036(3) -0.006(2) -0.003(2) -0.006(2) C26 0.024(2) 0.027(2) 0.035(3) 0.000(2) 0.001(2) 0.0001(19) C27 0.023(2) 0.026(2) 0.021(3) 0.002(2) -0.0092(19) 0.0042(19) C28 0.024(2) 0.052(3) 0.019(3) 0.004(2) -0.0069(19) 0.003(2) C29 0.050(3) 0.049(3) 0.027(3) 0.011(3) -0.005(2) 0.000(3) C30 0.045(3) 0.078(4) 0.026(3) 0.002(3) -0.001(2) 0.010(3) C31 0.059(3) 0.076(4) 0.031(3) 0.008(3) -0.013(2) -0.007(3) C32 0.0636(19) 0.0661(19) 0.103(3) -0.014(2) -0.0062(17) -0.0269(16) C33 0.0636(19) 0.0661(19) 0.103(3) -0.014(2) -0.0062(17) -0.0269(16) C34 0.0636(19) 0.0661(19) 0.103(3) -0.014(2) -0.0062(17) -0.0269(16) C35 0.0636(19) 0.0661(19) 0.103(3) -0.014(2) -0.0062(17) -0.0269(16) C36 0.023(2) 0.031(3) 0.030(3) 0.009(2) 0.0012(19) 0.003(2) C37 0.021(2) 0.040(3) 0.014(2) 0.004(2) 0.0010(19) -0.0039(18) C38 0.023(2) 0.041(3) 0.024(3) 0.001(2) -0.0004(19) 0.002(2) C39 0.041(3) 0.048(3) 0.032(3) -0.013(2) 0.002(2) 0.006(2) C40 0.033(3) 0.063(3) 0.047(4) -0.012(3) 0.009(2) 0.005(2) C41 0.024(2) 0.061(3) 0.050(3) -0.002(3) 0.0065(19) -0.006(2) C42 0.026(2) 0.042(2) 0.036(3) -0.004(3) -0.001(2) 0.000(2) C43 0.065(3) 0.049(3) 0.037(3) -0.013(3) 0.012(3) -0.013(3) C44 0.107(5) 0.102(5) 0.077(5) 0.054(4) 0.001(4) -0.039(4) C45 0.108(5) 0.047(4) 0.116(6) -0.032(4) -0.014(4) -0.013(4) C46 0.065(3) 0.064(4) 0.037(3) 0.006(3) 0.002(3) 0.028(3) C47 0.122(5) 0.065(4) 0.071(5) -0.006(4) -0.008(4) 0.050(4) C48 0.128(5) 0.058(4) 0.044(4) 0.018(3) -0.021(4) -0.006(4) C49 0.043(3) 0.059(3) 0.068(4) 0.014(3) 0.005(3) 0.001(3) C50 0.095(4) 0.068(4) 0.053(4) 0.016(3) -0.010(4) -0.008(4) C51 0.109(5) 0.077(4) 0.053(4) 0.013(4) 0.038(4) 0.023(4) C52 0.047(3) 0.078(4) 0.085(5) 0.029(4) 0.021(3) -0.006(3) C53 0.091(5) 0.044(3) 0.172(8) 0.019(4) 0.035(5) -0.003(4) C54 0.077(5) 0.044(4) 0.189(8) -0.027(4) 0.013(4) -0.008(3) C55 0.076(5) 0.050(4) 0.188(8) 0.006(5) 0.033(5) 0.016(4) C56 0.061(4) 0.056(4) 0.192(8) -0.024(5) 0.032(4) 0.004(3) _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 Y1 O1 2.223(2) . ? Y1 N3 2.245(3) . ? Y1 O2 2.246(2) . ? Y1 N1 2.411(3) . ? Y1 N2 2.427(3) . ? O1 C1 1.364(4) . ? O1 Li1 1.878(7) . ? O2 C22 1.359(4) . ? O2 Li2 1.855(7) . ? O3 C52 1.432(5) . ? O3 C49 1.442(5) . ? O3 Li1 1.894(8) . ? O4 C56 1.404(6) . ? O4 C53 1.406(6) . ? O4 Li2 1.880(8) . ? N1 C16 1.400(5) . ? N1 C15 1.477(5) . ? N1 Li2 2.063(7) . ? N2 C37 1.384(4) . ? N2 C36 1.484(5) . ? N2 Li1 2.037(7) . ? N3 Si2 1.723(4) . ? N3 Si1 1.717(4) . ? Si1 C43 1.866(5) . ? Si1 C44 1.875(5) . ? Si1 C45 1.882(5) . ? Si2 C46 1.881(5) . ? Si2 C48 1.886(5) . ? Si2 C47 1.890(5) . ? Cl1 C17 1.762(4) . ? Cl2 C38 1.754(4) . ? C1 C6 1.402(5) . ? C1 C2 1.423(5) . ? C2 C3 1.392(5) . ? C2 C7 1.537(5) . ? C3 C4 1.394(5) . ? C3 H3 0.9300 . ? C4 C5 1.390(5) . ? C4 C11 1.543(5) . ? C5 C6 1.401(5) . ? C5 H5 0.9300 . ? C6 C15 1.526(5) . ? C7 C9 1.522(5) . ? C7 C8 1.543(5) . ? C7 C10 1.551(5) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C13 1.496(6) . ? C11 C12 1.518(7) . ? C11 C14 1.512(6) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.407(5) . ? C16 C21 1.408(5) . ? C17 C18 1.372(5) . ? C18 C19 1.372(5) . ? C18 H18 0.9300 . ? C19 C20 1.368(6) . ? C19 H19 0.9300 . ? C20 C21 1.379(5) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.405(5) . ? C22 C23 1.417(5) . ? C23 C24 1.404(6) . ? C23 C28 1.537(6) . ? C24 C25 1.380(6) . ? C24 H24 0.9300 . ? C25 C26 1.395(5) . ? C25 C32 1.508(6) . ? C26 C27 1.393(5) . ? C26 H26 0.9300 . ? C27 C36 1.521(5) . ? C28 C29 1.532(6) . ? C28 C30 1.540(6) . ? C28 C31 1.549(6) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.502(7) . ? C32 C35 1.522(7) . ? C32 C34 1.540(7) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.402(5) . ? C37 C42 1.407(5) . ? C38 C39 1.365(5) . ? C39 C40 1.388(6) . ? C39 H39 0.9300 . ? C40 C41 1.364(6) . ? C40 H40 0.9300 . ? C41 C42 1.383(5) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.479(6) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.495(8) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.479(7) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.434(7) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.472(8) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.434(7) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Y1 N3 110.88(10) . . ? O1 Y1 O2 136.06(9) . . ? N3 Y1 O2 112.96(10) . . ? O1 Y1 N1 78.72(9) . . ? N3 Y1 N1 116.67(12) . . ? O2 Y1 N1 79.51(9) . . ? O1 Y1 N2 79.26(9) . . ? N3 Y1 N2 123.58(12) . . ? O2 Y1 N2 79.21(9) . . ? N1 Y1 N2 119.73(11) . . ? C1 O1 Li1 110.4(3) . . ? C1 O1 Y1 138.3(2) . . ? Li1 O1 Y1 96.0(2) . . ? C22 O2 Li2 113.7(3) . . ? C22 O2 Y1 137.8(2) . . ? Li2 O2 Y1 95.4(2) . . ? C52 O3 C49 106.1(3) . . ? C52 O3 Li1 124.0(3) . . ? C49 O3 Li1 129.8(3) . . ? C56 O4 C53 108.7(4) . . ? C56 O4 Li2 122.4(4) . . ? C53 O4 Li2 128.8(4) . . ? C16 N1 C15 114.3(3) . . ? C16 N1 Li2 106.5(3) . . ? C15 N1 Li2 107.9(3) . . ? C16 N1 Y1 129.2(2) . . ? C15 N1 Y1 107.8(2) . . ? Li2 N1 Y1 85.4(2) . . ? C37 N2 C36 114.9(3) . . ? C37 N2 Li1 107.4(3) . . ? C36 N2 Li1 105.5(3) . . ? C37 N2 Y1 130.5(2) . . ? C36 N2 Y1 106.2(2) . . ? Li1 N2 Y1 86.0(2) . . ? Si2 N3 Si1 121.31(18) . . ? Si2 N3 Y1 116.71(19) . . ? Si1 N3 Y1 121.98(19) . . ? N3 Si1 C43 112.46(18) . . ? N3 Si1 C44 113.7(2) . . ? C43 Si1 C44 105.6(3) . . ? N3 Si1 C45 112.8(2) . . ? C43 Si1 C45 106.2(2) . . ? C44 Si1 C45 105.3(3) . . ? N3 Si2 C46 111.48(18) . . ? N3 Si2 C48 113.0(2) . . ? C46 Si2 C48 105.9(2) . . ? N3 Si2 C47 114.5(2) . . ? C46 Si2 C47 105.3(3) . . ? C48 Si2 C47 105.9(3) . . ? O1 Li1 O3 127.3(4) . . ? O1 Li1 N2 98.6(3) . . ? O3 Li1 N2 116.9(4) . . ? O2 Li2 O4 126.7(4) . . ? O2 Li2 N1 99.0(3) . . ? O4 Li2 N1 115.0(4) . . ? O1 C1 C6 118.2(3) . . ? O1 C1 C2 122.1(3) . . ? C6 C1 C2 119.6(3) . . ? C3 C2 C1 116.9(4) . . ? C3 C2 C7 120.1(3) . . ? C1 C2 C7 123.0(3) . . ? C2 C3 C4 124.7(4) . . ? C2 C3 H3 117.7 . . ? C4 C3 H3 117.7 . . ? C5 C4 C3 116.5(4) . . ? C5 C4 C11 122.0(4) . . ? C3 C4 C11 121.5(4) . . ? C4 C5 C6 121.9(4) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C1 C6 C5 119.8(4) . . ? C1 C6 C15 120.1(3) . . ? C5 C6 C15 119.8(4) . . ? C9 C7 C2 111.3(3) . . ? C9 C7 C8 107.4(3) . . ? C2 C7 C8 112.0(3) . . ? C9 C7 C10 109.2(3) . . ? C2 C7 C10 110.6(3) . . ? C8 C7 C10 106.1(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C12 110.1(5) . . ? C13 C11 C14 108.3(4) . . ? C12 C11 C14 107.9(4) . . ? C13 C11 C4 112.0(4) . . ? C12 C11 C4 107.8(4) . . ? C14 C11 C4 110.6(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C6 118.6(3) . . ? N1 C15 H15A 107.7 . . ? C6 C15 H15A 107.7 . . ? N1 C15 H15B 107.7 . . ? C6 C15 H15B 107.7 . . ? H15A C15 H15B 107.1 . . ? N1 C16 C17 120.4(3) . . ? N1 C16 C21 126.3(4) . . ? C17 C16 C21 113.3(4) . . ? C18 C17 C16 124.9(4) . . ? C18 C17 Cl1 117.6(3) . . ? C16 C17 Cl1 117.4(3) . . ? C19 C18 C17 118.8(4) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C20 C19 C18 119.5(4) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 121.1(4) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C20 C21 C16 122.4(4) . . ? C20 C21 H21 118.8 . . ? C16 C21 H21 118.8 . . ? O2 C22 C27 118.0(4) . . ? O2 C22 C23 122.6(4) . . ? C27 C22 C23 119.4(4) . . ? C24 C23 C22 116.5(4) . . ? C24 C23 C28 119.2(4) . . ? C22 C23 C28 124.2(4) . . ? C25 C24 C23 125.4(4) . . ? C25 C24 H24 117.3 . . ? C23 C24 H24 117.3 . . ? C24 C25 C26 115.9(4) . . ? C24 C25 C32 121.2(4) . . ? C26 C25 C32 122.8(5) . . ? C27 C26 C25 122.0(4) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C26 C27 C22 120.3(4) . . ? C26 C27 C36 119.5(4) . . ? C22 C27 C36 119.9(3) . . ? C29 C28 C23 110.8(4) . . ? C29 C28 C30 109.1(4) . . ? C23 C28 C30 111.6(3) . . ? C29 C28 C31 106.5(4) . . ? C23 C28 C31 112.4(4) . . ? C30 C28 C31 106.1(4) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C35 108.0(5) . . ? C33 C32 C25 110.0(4) . . ? C35 C32 C25 113.5(5) . . ? C33 C32 C34 107.8(5) . . ? C35 C32 C34 105.9(4) . . ? C25 C32 C34 111.4(5) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N2 C36 C27 119.0(3) . . ? N2 C36 H36A 107.6 . . ? C27 C36 H36A 107.6 . . ? N2 C36 H36B 107.6 . . ? C27 C36 H36B 107.6 . . ? H36A C36 H36B 107.0 . . ? N2 C37 C38 120.6(3) . . ? N2 C37 C42 126.5(4) . . ? C38 C37 C42 112.8(3) . . ? C39 C38 C37 125.1(4) . . ? C39 C38 Cl2 118.0(3) . . ? C37 C38 Cl2 116.9(3) . . ? C38 C39 C40 119.7(4) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C41 C40 C39 117.9(4) . . ? C41 C40 H40 121.0 . . ? C39 C40 H40 121.0 . . ? C40 C41 C42 121.5(4) . . ? C40 C41 H41 119.2 . . ? C42 C41 H41 119.2 . . ? C41 C42 C37 122.9(4) . . ? C41 C42 H42 118.6 . . ? C37 C42 H42 118.6 . . ? Si1 C43 H43A 109.5 . . ? Si1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si1 C44 H44A 109.5 . . ? Si1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si1 C45 H45A 109.5 . . ? Si1 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si1 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si2 C46 H46A 109.5 . . ? Si2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? Si2 C47 H47A 109.5 . . ? Si2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Si2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? Si2 C48 H48A 109.5 . . ? Si2 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si2 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O3 C49 C50 106.0(4) . . ? O3 C49 H49A 110.5 . . ? C50 C49 H49A 110.5 . . ? O3 C49 H49B 110.5 . . ? C50 C49 H49B 110.5 . . ? H49A C49 H49B 108.7 . . ? C49 C50 C51 104.3(4) . . ? C49 C50 H50A 110.9 . . ? C51 C50 H50A 110.9 . . ? C49 C50 H50B 110.9 . . ? C51 C50 H50B 110.9 . . ? H50A C50 H50B 108.9 . . ? C52 C51 C50 106.1(4) . . ? C52 C51 H51A 110.5 . . ? C50 C51 H51A 110.5 . . ? C52 C51 H51B 110.5 . . ? C50 C51 H51B 110.5 . . ? H51A C51 H51B 108.7 . . ? O3 C52 C51 107.7(4) . . ? O3 C52 H52A 110.2 . . ? C51 C52 H52A 110.2 . . ? O3 C52 H52B 110.2 . . ? C51 C52 H52B 110.2 . . ? H52A C52 H52B 108.5 . . ? O4 C53 C54 108.4(5) . . ? O4 C53 H53A 110.0 . . ? C54 C53 H53A 110.0 . . ? O4 C53 H53B 110.0 . . ? C54 C53 H53B 110.0 . . ? H53A C53 H53B 108.4 . . ? C53 C54 C55 106.0(5) . . ? C53 C54 H54A 110.5 . . ? C55 C54 H54A 110.5 . . ? C53 C54 H54B 110.5 . . ? C55 C54 H54B 110.5 . . ? H54A C54 H54B 108.7 . . ? C56 C55 C54 105.3(5) . . ? C56 C55 H55A 110.7 . . ? C54 C55 H55A 110.7 . . ? C56 C55 H55B 110.7 . . ? C54 C55 H55B 110.7 . . ? H55A C55 H55B 108.8 . . ? O4 C56 C55 108.7(5) . . ? O4 C56 H56A 110.0 . . ? C55 C56 H56A 110.0 . . ? O4 C56 H56B 110.0 . . ? C55 C56 H56B 110.0 . . ? H56A C56 H56B 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 N3 Y1 O1 C1 -110.5(3) . . . . ? O2 Y1 O1 C1 65.6(4) . . . . ? N1 Y1 O1 C1 4.0(3) . . . . ? N2 Y1 O1 C1 127.5(3) . . . . ? N3 Y1 O1 Li1 119.4(3) . . . . ? O2 Y1 O1 Li1 -64.5(3) . . . . ? N1 Y1 O1 Li1 -126.2(3) . . . . ? N2 Y1 O1 Li1 -2.6(3) . . . . ? O1 Y1 O2 C22 66.9(4) . . . . ? N3 Y1 O2 C22 -117.0(3) . . . . ? N1 Y1 O2 C22 128.3(3) . . . . ? N2 Y1 O2 C22 5.0(3) . . . . ? O1 Y1 O2 Li2 -67.8(3) . . . . ? N3 Y1 O2 Li2 108.3(3) . . . . ? N1 Y1 O2 Li2 -6.4(3) . . . . ? N2 Y1 O2 Li2 -129.7(3) . . . . ? O1 Y1 N1 C16 -105.1(3) . . . . ? N3 Y1 N1 C16 2.8(3) . . . . ? O2 Y1 N1 C16 113.3(3) . . . . ? N2 Y1 N1 C16 -175.6(3) . . . . ? O1 Y1 N1 C15 40.0(2) . . . . ? N3 Y1 N1 C15 147.9(2) . . . . ? O2 Y1 N1 C15 -101.6(2) . . . . ? N2 Y1 N1 C15 -30.6(3) . . . . ? O1 Y1 N1 Li2 147.3(2) . . . . ? N3 Y1 N1 Li2 -104.8(2) . . . . ? O2 Y1 N1 Li2 5.8(2) . . . . ? N2 Y1 N1 Li2 76.8(2) . . . . ? O1 Y1 N2 C37 111.9(3) . . . . ? N3 Y1 N2 C37 3.9(4) . . . . ? O2 Y1 N2 C37 -106.6(3) . . . . ? N1 Y1 N2 C37 -177.8(3) . . . . ? O1 Y1 N2 C36 -102.5(2) . . . . ? N3 Y1 N2 C36 149.4(2) . . . . ? O2 Y1 N2 C36 38.9(2) . . . . ? N1 Y1 N2 C36 -32.3(2) . . . . ? O1 Y1 N2 Li1 2.4(2) . . . . ? N3 Y1 N2 Li1 -105.6(3) . . . . ? O2 Y1 N2 Li1 143.9(2) . . . . ? N1 Y1 N2 Li1 72.7(3) . . . . ? O1 Y1 N3 Si2 -133.89(16) . . . . ? O2 Y1 N3 Si2 49.0(2) . . . . ? N1 Y1 N3 Si2 138.55(16) . . . . ? N2 Y1 N3 Si2 -43.1(2) . . . . ? O1 Y1 N3 Si1 46.6(2) . . . . ? O2 Y1 N3 Si1 -130.49(17) . . . . ? N1 Y1 N3 Si1 -41.0(2) . . . . ? N2 Y1 N3 Si1 137.37(18) . . . . ? Si2 N3 Si1 C43 -175.7(2) . . . . ? Y1 N3 Si1 C43 3.8(3) . . . . ? Si2 N3 Si1 C44 -55.6(3) . . . . ? Y1 N3 Si1 C44 123.9(3) . . . . ? Si2 N3 Si1 C45 64.2(3) . . . . ? Y1 N3 Si1 C45 -116.2(3) . . . . ? Si1 N3 Si2 C46 -174.5(2) . . . . ? Y1 N3 Si2 C46 6.0(3) . . . . ? Si1 N3 Si2 C48 66.4(3) . . . . ? Y1 N3 Si2 C48 -113.1(2) . . . . ? Si1 N3 Si2 C47 -55.0(3) . . . . ? Y1 N3 Si2 C47 125.4(3) . . . . ? C1 O1 Li1 O3 -10.5(6) . . . . ? Y1 O1 Li1 O3 136.7(4) . . . . ? C1 O1 Li1 N2 -144.0(3) . . . . ? Y1 O1 Li1 N2 3.1(3) . . . . ? C52 O3 Li1 O1 -179.7(5) . . . . ? C49 O3 Li1 O1 5.2(8) . . . . ? C52 O3 Li1 N2 -53.1(6) . . . . ? C49 O3 Li1 N2 131.8(4) . . . . ? C37 N2 Li1 O1 -134.1(3) . . . . ? C36 N2 Li1 O1 102.9(4) . . . . ? Y1 N2 Li1 O1 -2.9(3) . . . . ? C37 N2 Li1 O3 86.1(4) . . . . ? C36 N2 Li1 O3 -36.9(4) . . . . ? Y1 N2 Li1 O3 -142.6(4) . . . . ? C22 O2 Li2 O4 -10.5(6) . . . . ? Y1 O2 Li2 O4 138.0(5) . . . . ? C22 O2 Li2 N1 -141.1(3) . . . . ? Y1 O2 Li2 N1 7.5(3) . . . . ? C56 O4 Li2 O2 176.8(5) . . . . ? C53 O4 Li2 O2 -6.5(8) . . . . ? C56 O4 Li2 N1 -59.0(6) . . . . ? C53 O4 Li2 N1 117.7(5) . . . . ? C16 N1 Li2 O2 -136.5(3) . . . . ? C15 N1 Li2 O2 100.3(4) . . . . ? Y1 N1 Li2 O2 -6.9(3) . . . . ? C16 N1 Li2 O4 85.7(4) . . . . ? C15 N1 Li2 O4 -37.5(5) . . . . ? Y1 N1 Li2 O4 -144.8(4) . . . . ? Li1 O1 C1 C6 97.6(4) . . . . ? Y1 O1 C1 C6 -28.2(5) . . . . ? Li1 O1 C1 C2 -79.2(4) . . . . ? Y1 O1 C1 C2 155.0(3) . . . . ? O1 C1 C2 C3 168.2(3) . . . . ? C6 C1 C2 C3 -8.6(5) . . . . ? O1 C1 C2 C7 -9.8(5) . . . . ? C6 C1 C2 C7 173.4(3) . . . . ? C1 C2 C3 C4 3.2(6) . . . . ? C7 C2 C3 C4 -178.7(3) . . . . ? C2 C3 C4 C5 2.5(6) . . . . ? C2 C3 C4 C11 -175.4(4) . . . . ? C3 C4 C5 C6 -3.0(6) . . . . ? C11 C4 C5 C6 174.9(4) . . . . ? O1 C1 C6 C5 -168.6(3) . . . . ? C2 C1 C6 C5 8.3(5) . . . . ? O1 C1 C6 C15 5.7(5) . . . . ? C2 C1 C6 C15 -177.4(3) . . . . ? C4 C5 C6 C1 -2.3(6) . . . . ? C4 C5 C6 C15 -176.6(4) . . . . ? C3 C2 C7 C9 135.0(4) . . . . ? C1 C2 C7 C9 -47.1(5) . . . . ? C3 C2 C7 C8 14.7(5) . . . . ? C1 C2 C7 C8 -167.4(4) . . . . ? C3 C2 C7 C10 -103.4(4) . . . . ? C1 C2 C7 C10 74.5(4) . . . . ? C5 C4 C11 C13 21.0(6) . . . . ? C3 C4 C11 C13 -161.2(4) . . . . ? C5 C4 C11 C12 -100.3(5) . . . . ? C3 C4 C11 C12 77.5(5) . . . . ? C5 C4 C11 C14 141.9(4) . . . . ? C3 C4 C11 C14 -40.2(6) . . . . ? C16 N1 C15 C6 76.5(4) . . . . ? Li2 N1 C15 C6 -165.2(3) . . . . ? Y1 N1 C15 C6 -74.3(3) . . . . ? C1 C6 C15 N1 51.4(5) . . . . ? C5 C6 C15 N1 -134.3(4) . . . . ? C15 N1 C16 C17 167.5(4) . . . . ? Li2 N1 C16 C17 48.5(5) . . . . ? Y1 N1 C16 C17 -49.2(5) . . . . ? C15 N1 C16 C21 -13.6(5) . . . . ? Li2 N1 C16 C21 -132.6(4) . . . . ? Y1 N1 C16 C21 129.7(4) . . . . ? N1 C16 C17 C18 176.6(4) . . . . ? C21 C16 C17 C18 -2.4(6) . . . . ? N1 C16 C17 Cl1 -2.4(5) . . . . ? C21 C16 C17 Cl1 178.6(3) . . . . ? C16 C17 C18 C19 1.1(7) . . . . ? Cl1 C17 C18 C19 -179.9(4) . . . . ? C17 C18 C19 C20 1.5(7) . . . . ? C18 C19 C20 C21 -2.6(8) . . . . ? C19 C20 C21 C16 1.2(7) . . . . ? N1 C16 C21 C20 -177.8(4) . . . . ? C17 C16 C21 C20 1.2(6) . . . . ? Li2 O2 C22 C27 101.2(4) . . . . ? Y1 O2 C22 C27 -28.3(5) . . . . ? Li2 O2 C22 C23 -75.9(5) . . . . ? Y1 O2 C22 C23 154.7(3) . . . . ? O2 C22 C23 C24 170.3(3) . . . . ? C27 C22 C23 C24 -6.7(5) . . . . ? O2 C22 C23 C28 -7.9(6) . . . . ? C27 C22 C23 C28 175.1(4) . . . . ? C22 C23 C24 C25 3.0(6) . . . . ? C28 C23 C24 C25 -178.7(4) . . . . ? C23 C24 C25 C26 0.9(6) . . . . ? C23 C24 C25 C32 -176.2(4) . . . . ? C24 C25 C26 C27 -1.0(6) . . . . ? C32 C25 C26 C27 176.0(4) . . . . ? C25 C26 C27 C22 -2.8(6) . . . . ? C25 C26 C27 C36 -177.1(4) . . . . ? O2 C22 C27 C26 -170.4(3) . . . . ? C23 C22 C27 C26 6.8(5) . . . . ? O2 C22 C27 C36 3.9(5) . . . . ? C23 C22 C27 C36 -179.0(4) . . . . ? C24 C23 C28 C29 134.9(4) . . . . ? C22 C23 C28 C29 -46.9(5) . . . . ? C24 C23 C28 C30 -103.3(4) . . . . ? C22 C23 C28 C30 75.0(5) . . . . ? C24 C23 C28 C31 15.8(5) . . . . ? C22 C23 C28 C31 -165.9(4) . . . . ? C24 C25 C32 C33 79.2(6) . . . . ? C26 C25 C32 C33 -97.7(6) . . . . ? C24 C25 C32 C35 -159.8(5) . . . . ? C26 C25 C32 C35 23.3(7) . . . . ? C24 C25 C32 C34 -40.3(6) . . . . ? C26 C25 C32 C34 142.8(5) . . . . ? C37 N2 C36 C27 76.0(5) . . . . ? Li1 N2 C36 C27 -166.0(3) . . . . ? Y1 N2 C36 C27 -75.7(3) . . . . ? C26 C27 C36 N2 -130.5(4) . . . . ? C22 C27 C36 N2 55.1(5) . . . . ? C36 N2 C37 C38 170.8(3) . . . . ? Li1 N2 C37 C38 53.8(5) . . . . ? Y1 N2 C37 C38 -46.0(5) . . . . ? C36 N2 C37 C42 -8.4(6) . . . . ? Li1 N2 C37 C42 -125.4(4) . . . . ? Y1 N2 C37 C42 134.8(3) . . . . ? N2 C37 C38 C39 179.3(4) . . . . ? C42 C37 C38 C39 -1.4(6) . . . . ? N2 C37 C38 Cl2 0.2(5) . . . . ? C42 C37 C38 Cl2 179.5(3) . . . . ? C37 C38 C39 C40 0.1(7) . . . . ? Cl2 C38 C39 C40 179.2(4) . . . . ? C38 C39 C40 C41 1.8(7) . . . . ? C39 C40 C41 C42 -2.2(7) . . . . ? C40 C41 C42 C37 0.8(7) . . . . ? N2 C37 C42 C41 -179.8(4) . . . . ? C38 C37 C42 C41 1.0(6) . . . . ? C52 O3 C49 C50 -32.0(5) . . . . ? Li1 O3 C49 C50 143.8(4) . . . . ? O3 C49 C50 C51 28.0(5) . . . . ? C49 C50 C51 C52 -13.7(6) . . . . ? C49 O3 C52 C51 23.1(6) . . . . ? Li1 O3 C52 C51 -153.0(4) . . . . ? C50 C51 C52 O3 -5.4(7) . . . . ? C56 O4 C53 C54 -3.5(8) . . . . ? Li2 O4 C53 C54 179.4(5) . . . . ? O4 C53 C54 C55 12.8(8) . . . . ? C53 C54 C55 C56 -17.1(9) . . . . ? C53 O4 C56 C55 -7.7(8) . . . . ? Li2 O4 C56 C55 169.7(5) . . . . ? C54 C55 C56 O4 15.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.793 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.067 _database_code_depnum_ccdc_archive 'CCDC 932405' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl8 #TrackingRef 'C56H86Cl2 Li2N3O4Si2 Yb.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H86 Cl2 Li2 N3 O4 Si2 Yb' _chemical_formula_sum 'C56 H86 Cl2 Li2 N3 O4 Si2 Yb' _chemical_formula_weight 1179.28 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 11.752(3) _cell_length_b 21.587(5) _cell_length_c 23.405(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5937(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 27887 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2452 _exptl_absorpt_coefficient_mu 1.749 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3739 _exptl_absorpt_correction_T_max 0.7211 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33774 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.1161 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.55 _reflns_number_total 13539 _reflns_number_gt 9883 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^)+(0.0788P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_number_reflns 13539 _refine_ls_number_parameters 626 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0970 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.1903 _refine_ls_wR_factor_gt 0.1576 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 Yb1 Yb 0.99764(3) -0.018606(16) 0.284407(13) 0.03243(11) Uani 1 1 d . . . O1 O 1.0786(5) -0.0031(3) 0.2013(2) 0.0380(15) Uani 1 1 d . . . O2 O 0.9171(5) 0.0361(3) 0.3516(3) 0.0395(16) Uani 1 1 d . . . O3 O 0.9394(6) 0.0950(4) 0.1150(3) 0.0518(19) Uani 1 1 d . . . O4 O 1.0637(8) 0.1602(4) 0.3932(6) 0.093(2) Uani 1 1 d . . . N1 N 1.1536(7) 0.0435(4) 0.3133(3) 0.0373(18) Uani 1 1 d . . . N2 N 0.8436(6) 0.0246(4) 0.2310(3) 0.0357(18) Uani 1 1 d . . . N3 N 1.0097(9) -0.1172(3) 0.3081(3) 0.0433(19) Uani 1 1 d . . . Si1 Si 1.1312(4) -0.15850(16) 0.30245(16) 0.0644(10) Uani 1 1 d . . . Si2 Si 0.8863(4) -0.15204(16) 0.33339(15) 0.0656(10) Uani 1 1 d . . . Cl1 Cl 1.1203(2) -0.02867(15) 0.41825(11) 0.0562(7) Uani 1 1 d . . . Cl2 Cl 0.8759(2) -0.09656(14) 0.17552(13) 0.0563(7) Uani 1 1 d . . . Li1 Li 0.9491(14) 0.0255(9) 0.1642(7) 0.046(4) Uani 1 1 d . . . Li2 Li 1.0513(17) 0.0767(10) 0.3745(8) 0.057(5) Uani 1 1 d . . . C1 C 1.1747(8) 0.0263(5) 0.1804(4) 0.040(2) Uani 1 1 d . . . C2 C 1.2220(8) 0.0084(4) 0.1277(4) 0.035(2) Uani 1 1 d . . . C3 C 1.3010(8) 0.0484(5) 0.1061(4) 0.037(2) Uani 1 1 d . . . H3 H 1.3314 0.0391 0.0699 0.045 Uiso 1 1 calc R . . C4 C 1.3397(9) 0.1010(5) 0.1324(4) 0.048(3) Uani 1 1 d . . . C5 C 1.2983(9) 0.1142(5) 0.1878(4) 0.045(3) Uani 1 1 d . . . H5 H 1.3267 0.1484 0.2081 0.054 Uiso 1 1 calc R . . C6 C 1.2154(9) 0.0765(5) 0.2122(4) 0.040(2) Uani 1 1 d . . . C7 C 1.1900(9) -0.0493(5) 0.0940(4) 0.041(2) Uani 1 1 d . . . C8 C 1.2749(9) -0.0637(6) 0.0471(5) 0.058(3) Uani 1 1 d . . . H8A H 1.2592 -0.1044 0.0314 0.087 Uiso 1 1 calc R . . H8B H 1.3514 -0.0629 0.0627 0.087 Uiso 1 1 calc R . . H8C H 1.2686 -0.0329 0.0171 0.087 Uiso 1 1 calc R . . C9 C 1.1856(9) -0.1054(5) 0.1330(4) 0.045(3) Uani 1 1 d . . . H9A H 1.1679 -0.1420 0.1107 0.067 Uiso 1 1 calc R . . H9B H 1.1271 -0.0992 0.1618 0.067 Uiso 1 1 calc R . . H9C H 1.2587 -0.1107 0.1516 0.067 Uiso 1 1 calc R . . C10 C 1.0774(8) -0.0395(6) 0.0633(4) 0.048(3) Uani 1 1 d . . . H10A H 1.0169 -0.0351 0.0913 0.072 Uiso 1 1 calc R . . H10B H 1.0616 -0.0748 0.0390 0.072 Uiso 1 1 calc R . . H10C H 1.0817 -0.0023 0.0402 0.072 Uiso 1 1 calc R . . C11 C 1.4298(9) 0.1445(6) 0.1039(5) 0.055(3) Uani 1 1 d . . . C12 C 1.4816(16) 0.1880(7) 0.1462(6) 0.100(6) Uani 1 1 d . . . H12A H 1.5354 0.2149 0.1269 0.150 Uiso 1 1 calc R . . H12B H 1.5208 0.1645 0.1755 0.150 Uiso 1 1 calc R . . H12C H 1.4222 0.2129 0.1636 0.150 Uiso 1 1 calc R . . C13 C 1.3605(14) 0.1832(9) 0.0597(10) 0.133(9) Uani 1 1 d . . . H13A H 1.3251 0.1555 0.0323 0.199 Uiso 1 1 calc R . . H13B H 1.4112 0.2114 0.0399 0.199 Uiso 1 1 calc R . . H13C H 1.3022 0.2067 0.0795 0.199 Uiso 1 1 calc R . . C14 C 1.5128(11) 0.1109(7) 0.0706(6) 0.079(4) Uani 1 1 d . . . H14A H 1.4740 0.0827 0.0448 0.119 Uiso 1 1 calc R . . H14B H 1.5619 0.0875 0.0960 0.119 Uiso 1 1 calc R . . H14C H 1.5582 0.1399 0.0486 0.119 Uiso 1 1 calc R . . C15 C 1.1657(9) 0.0930(5) 0.2698(4) 0.042(3) Uani 1 1 d . . . H15A H 1.2131 0.1258 0.2864 0.050 Uiso 1 1 calc R . . H15B H 1.0901 0.1108 0.2633 0.050 Uiso 1 1 calc R . . C16 C 1.2540(7) 0.0273(5) 0.3412(4) 0.035(2) Uani 1 1 d . . . C17 C 1.2531(8) -0.0079(6) 0.3897(4) 0.049(3) Uani 1 1 d . . . C18 C 1.3494(9) -0.0289(6) 0.4182(5) 0.057(3) Uani 1 1 d . . . H18 H 1.3421 -0.0541 0.4508 0.069 Uiso 1 1 calc R . . C19 C 1.4529(8) -0.0130(7) 0.3988(5) 0.069(4) Uani 1 1 d . . . H19 H 1.5197 -0.0263 0.4172 0.083 Uiso 1 1 calc R . . C20 C 1.4565(9) 0.0234(6) 0.3512(5) 0.057(3) Uani 1 1 d . . . H20 H 1.5287 0.0354 0.3379 0.069 Uiso 1 1 calc R . . C21 C 1.3654(8) 0.0435(5) 0.3215(4) 0.047(3) Uani 1 1 d . . . H21 H 1.3749 0.0677 0.2885 0.056 Uiso 1 1 calc R . . C22 C 0.8223(7) 0.0722(4) 0.3572(4) 0.035(2) Uani 1 1 d . . . C23 C 0.7704(8) 0.0831(4) 0.4121(4) 0.040(2) Uani 1 1 d . . . C24 C 0.6828(9) 0.1276(5) 0.4125(4) 0.047(3) Uani 1 1 d . . . H24 H 0.6478 0.1362 0.4477 0.056 Uiso 1 1 calc R . . C25 C 0.6450(9) 0.1590(5) 0.3662(5) 0.049(3) Uani 1 1 d . . . C26 C 0.6887(10) 0.1441(5) 0.3139(5) 0.049(3) Uani 1 1 d . . . H26 H 0.6597 0.1634 0.2810 0.059 Uiso 1 1 calc R . . C27 C 0.7767(8) 0.1000(5) 0.3086(4) 0.038(2) Uani 1 1 d . . . C28 C 0.8066(9) 0.0508(6) 0.4672(4) 0.052(3) Uani 1 1 d . . . C29 C 0.7144(11) 0.0615(7) 0.5152(5) 0.068(4) Uani 1 1 d . . . H29A H 0.6404 0.0488 0.5012 0.102 Uiso 1 1 calc R . . H29B H 0.7122 0.1050 0.5253 0.102 Uiso 1 1 calc R . . H29C H 0.7340 0.0372 0.5487 0.102 Uiso 1 1 calc R . . C30 C 0.9135(11) 0.0772(8) 0.4917(5) 0.076(4) Uani 1 1 d . . . H30A H 0.9033 0.1211 0.4987 0.114 Uiso 1 1 calc R . . H30B H 0.9756 0.0711 0.4650 0.114 Uiso 1 1 calc R . . H30C H 0.9310 0.0564 0.5274 0.114 Uiso 1 1 calc R . . C31 C 0.8150(13) -0.0179(7) 0.4586(5) 0.070(4) Uani 1 1 d . . . H31A H 0.8793 -0.0271 0.4340 0.105 Uiso 1 1 calc R . . H31B H 0.7457 -0.0329 0.4408 0.105 Uiso 1 1 calc R . . H31C H 0.8253 -0.0381 0.4952 0.105 Uiso 1 1 calc R . . C32 C 0.5539(10) 0.2104(5) 0.3734(6) 0.058(3) Uani 1 1 d . . . C33 C 0.6088(16) 0.2685(7) 0.3929(10) 0.125(8) Uani 1 1 d . . . H33A H 0.6577 0.2598 0.4253 0.187 Uiso 1 1 calc R . . H33B H 0.5508 0.2981 0.4041 0.187 Uiso 1 1 calc R . . H33C H 0.6539 0.2857 0.3620 0.187 Uiso 1 1 calc R . . C34 C 0.4657(12) 0.1916(9) 0.4167(8) 0.100(6) Uani 1 1 d . . . H34A H 0.4117 0.2251 0.4219 0.151 Uiso 1 1 calc R . . H34B H 0.5026 0.1825 0.4528 0.151 Uiso 1 1 calc R . . H34C H 0.4260 0.1550 0.4032 0.151 Uiso 1 1 calc R . . C35 C 0.4925(16) 0.2217(8) 0.3166(7) 0.118(7) Uani 1 1 d . . . H35A H 0.5471 0.2352 0.2881 0.176 Uiso 1 1 calc R . . H35B H 0.4350 0.2534 0.3216 0.176 Uiso 1 1 calc R . . H35C H 0.4567 0.1836 0.3040 0.176 Uiso 1 1 calc R . . C36 C 0.8344(9) 0.0893(5) 0.2520(4) 0.040(3) Uani 1 1 d . . . H36A H 0.7935 0.1134 0.2230 0.048 Uiso 1 1 calc R . . H36B H 0.9115 0.1064 0.2545 0.048 Uiso 1 1 calc R . . C37 C 0.7437(7) -0.0033(5) 0.2126(4) 0.034(2) Uani 1 1 d . . . C38 C 0.7447(9) -0.0600(5) 0.1840(4) 0.043(2) Uani 1 1 d . . . C39 C 0.6483(9) -0.0918(6) 0.1649(4) 0.053(3) Uani 1 1 d . . . H39 H 0.6537 -0.1313 0.1482 0.063 Uiso 1 1 calc R . . C40 C 0.5480(9) -0.0634(7) 0.1715(5) 0.064(3) Uani 1 1 d . . . H40 H 0.4824 -0.0828 0.1571 0.077 Uiso 1 1 calc R . . C41 C 0.5369(9) -0.0091(6) 0.1975(5) 0.061(3) Uani 1 1 d . . . H41 H 0.4647 0.0087 0.2031 0.073 Uiso 1 1 calc R . . C42 C 0.6357(9) 0.0213(6) 0.2164(4) 0.057(3) Uani 1 1 d . . . H42 H 0.6277 0.0609 0.2326 0.068 Uiso 1 1 calc R . . C43 C 1.2521(11) -0.1098(6) 0.2788(5) 0.065(3) Uani 1 1 d . . . H43A H 1.2929 -0.0945 0.3119 0.098 Uiso 1 1 calc R . . H43B H 1.2237 -0.0752 0.2566 0.098 Uiso 1 1 calc R . . H43C H 1.3032 -0.1344 0.2554 0.098 Uiso 1 1 calc R . . C44 C 1.1804(15) -0.1961(7) 0.3715(7) 0.104(6) Uani 1 1 d . . . H44A H 1.1180 -0.2193 0.3882 0.156 Uiso 1 1 calc R . . H44B H 1.2049 -0.1642 0.3981 0.156 Uiso 1 1 calc R . . H44C H 1.2433 -0.2238 0.3636 0.156 Uiso 1 1 calc R . . C45 C 1.1202(17) -0.2236(6) 0.2490(7) 0.104(7) Uani 1 1 d . . . H45A H 1.0847 -0.2085 0.2143 0.156 Uiso 1 1 calc R . . H45B H 1.0745 -0.2568 0.2650 0.156 Uiso 1 1 calc R . . H45C H 1.1957 -0.2391 0.2403 0.156 Uiso 1 1 calc R . . C46 C 0.7602(10) -0.0990(6) 0.3279(5) 0.066(4) Uani 1 1 d . . . H46A H 0.7302 -0.1003 0.2893 0.099 Uiso 1 1 calc R . . H46B H 0.7834 -0.0570 0.3369 0.099 Uiso 1 1 calc R . . H46C H 0.7019 -0.1122 0.3545 0.099 Uiso 1 1 calc R . . C47 C 0.8465(15) -0.2235(7) 0.2933(7) 0.099(6) Uani 1 1 d . . . H47A H 0.9014 -0.2559 0.3013 0.149 Uiso 1 1 calc R . . H47B H 0.8461 -0.2148 0.2527 0.149 Uiso 1 1 calc R . . H47C H 0.7714 -0.2370 0.3051 0.149 Uiso 1 1 calc R . . C48 C 0.8958(15) -0.1741(7) 0.4111(5) 0.085(5) Uani 1 1 d . . . H48A H 0.9047 -0.1370 0.4340 0.127 Uiso 1 1 calc R . . H48B H 0.9608 -0.2011 0.4169 0.127 Uiso 1 1 calc R . . H48C H 0.8268 -0.1955 0.4223 0.127 Uiso 1 1 calc R . . C49 C 1.0204(10) 0.1354(6) 0.0940(6) 0.072(4) Uani 1 1 d . . . H49A H 1.0955 0.1158 0.0933 0.086 Uiso 1 1 calc R . . H49B H 1.0244 0.1728 0.1177 0.086 Uiso 1 1 calc R . . C50 C 0.9825(18) 0.1514(7) 0.0343(6) 0.097(6) Uani 1 1 d . . . H50A H 1.0069 0.1933 0.0239 0.116 Uiso 1 1 calc R . . H50B H 1.0138 0.1220 0.0066 0.116 Uiso 1 1 calc R . . C51 C 0.8596(12) 0.1473(9) 0.0363(7) 0.092(5) Uani 1 1 d . . . H51A H 0.8302 0.1259 0.0025 0.110 Uiso 1 1 calc R . . H51B H 0.8254 0.1887 0.0383 0.110 Uiso 1 1 calc R . . C52 C 0.8355(12) 0.1122(8) 0.0878(6) 0.082(4) Uani 1 1 d . . . H52A H 0.7897 0.1374 0.1140 0.098 Uiso 1 1 calc R . . H52B H 0.7918 0.0750 0.0781 0.098 Uiso 1 1 calc R . . C53 C 0.9907(14) 0.2075(5) 0.3864(8) 0.093(2) Uani 1 1 d . . . H53A H 0.9176 0.1969 0.4041 0.111 Uiso 1 1 calc R . . H53B H 0.9776 0.2145 0.3456 0.111 Uiso 1 1 calc R . . C54 C 1.0336(11) 0.2629(6) 0.4118(8) 0.093(2) Uani 1 1 d . . . H54A H 0.9991 0.2706 0.4492 0.111 Uiso 1 1 calc R . . H54B H 1.0213 0.2989 0.3871 0.111 Uiso 1 1 calc R . . C55 C 1.1516(12) 0.2481(6) 0.4166(9) 0.093(2) Uani 1 1 d . . . H55A H 1.1945 0.2680 0.3857 0.111 Uiso 1 1 calc R . . H55B H 1.1814 0.2632 0.4532 0.111 Uiso 1 1 calc R . . C56 C 1.1629(12) 0.1845(6) 0.4134(9) 0.093(2) Uani 1 1 d . . . H56A H 1.2258 0.1738 0.3877 0.111 Uiso 1 1 calc R . . H56B H 1.1797 0.1675 0.4513 0.111 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 Yb1 0.03144(19) 0.03514(19) 0.03071(18) 0.00066(14) 0.0027(2) 0.0003(2) O1 0.027(3) 0.057(4) 0.030(3) 0.005(3) 0.003(3) -0.005(3) O2 0.035(3) 0.047(4) 0.036(3) -0.011(3) 0.005(3) 0.017(3) O3 0.033(4) 0.066(5) 0.057(4) 0.011(4) -0.001(3) -0.001(4) O4 0.068(4) 0.051(3) 0.160(6) -0.014(4) 0.000(4) -0.003(3) N1 0.042(5) 0.033(4) 0.037(4) 0.004(3) 0.008(4) -0.002(4) N2 0.024(4) 0.050(5) 0.033(4) -0.001(4) -0.011(3) -0.008(4) N3 0.052(5) 0.036(4) 0.042(4) 0.006(3) 0.012(5) -0.013(5) Si1 0.083(3) 0.0467(19) 0.064(2) 0.0049(17) 0.001(2) 0.0148(19) Si2 0.101(3) 0.0438(18) 0.0520(19) 0.0037(15) 0.004(2) -0.018(2) Cl1 0.0433(13) 0.079(2) 0.0466(13) 0.0140(14) 0.0030(12) -0.0036(14) Cl2 0.0405(14) 0.0546(16) 0.0737(18) -0.0178(15) 0.0031(14) -0.0048(13) Li1 0.044(9) 0.055(10) 0.039(8) -0.012(8) 0.005(7) 0.025(8) Li2 0.067(12) 0.065(12) 0.040(9) -0.005(9) -0.017(9) -0.008(10) C1 0.043(5) 0.052(6) 0.025(4) 0.002(4) -0.003(4) -0.003(5) C2 0.035(5) 0.040(5) 0.029(4) 0.013(4) 0.007(4) -0.010(4) C3 0.032(5) 0.044(6) 0.036(5) -0.013(4) 0.000(4) 0.026(4) C4 0.038(5) 0.055(7) 0.050(6) 0.014(5) 0.000(5) 0.010(5) C5 0.044(6) 0.045(6) 0.045(6) 0.009(5) -0.006(5) 0.031(5) C6 0.052(6) 0.039(5) 0.029(4) 0.000(4) 0.011(4) -0.005(5) C7 0.044(5) 0.039(6) 0.038(5) -0.004(4) 0.016(4) 0.008(5) C8 0.045(6) 0.076(8) 0.054(6) -0.025(6) 0.010(5) 0.001(6) C9 0.044(6) 0.035(5) 0.055(6) -0.004(5) 0.026(5) -0.011(5) C10 0.028(5) 0.075(8) 0.042(5) -0.013(5) -0.001(4) 0.004(5) C11 0.034(5) 0.076(8) 0.055(6) 0.007(6) 0.017(5) 0.012(6) C12 0.113(14) 0.108(11) 0.079(9) -0.012(8) 0.033(10) -0.078(12) C13 0.066(10) 0.133(16) 0.20(2) 0.106(16) -0.002(12) -0.030(11) C14 0.050(7) 0.101(10) 0.086(9) -0.005(7) 0.038(8) -0.014(8) C15 0.041(6) 0.033(5) 0.051(7) 0.005(5) -0.005(5) 0.003(5) C16 0.022(4) 0.051(6) 0.033(4) -0.005(4) -0.013(3) 0.013(4) C17 0.030(5) 0.082(8) 0.036(5) -0.008(5) 0.003(4) -0.040(5) C18 0.046(6) 0.078(8) 0.048(6) -0.004(6) -0.030(5) 0.010(6) C19 0.016(4) 0.119(11) 0.072(8) 0.007(8) -0.006(5) -0.006(6) C20 0.044(6) 0.080(8) 0.048(6) -0.003(6) 0.000(5) -0.009(6) C21 0.036(5) 0.060(7) 0.044(5) 0.007(5) 0.012(5) 0.004(5) C22 0.020(4) 0.045(6) 0.039(5) -0.014(4) -0.002(4) -0.015(4) C23 0.033(5) 0.037(5) 0.049(6) -0.010(4) 0.016(4) -0.001(4) C24 0.046(6) 0.052(7) 0.043(6) -0.017(5) 0.011(5) -0.005(5) C25 0.050(6) 0.044(6) 0.054(7) -0.007(5) -0.009(5) -0.013(5) C26 0.062(7) 0.035(5) 0.051(6) -0.007(5) -0.017(5) 0.017(5) C27 0.033(5) 0.043(5) 0.038(5) 0.007(4) -0.003(4) -0.015(5) C28 0.037(5) 0.086(9) 0.032(5) -0.010(6) 0.010(4) -0.020(6) C29 0.067(8) 0.085(10) 0.053(7) 0.013(7) 0.013(6) 0.000(8) C30 0.067(8) 0.124(13) 0.037(6) -0.007(7) -0.017(6) -0.007(9) C31 0.096(10) 0.076(9) 0.039(6) 0.002(6) 0.016(6) 0.005(9) C32 0.046(6) 0.047(7) 0.079(8) -0.012(6) 0.013(6) 0.029(5) C33 0.110(14) 0.056(9) 0.21(2) -0.020(12) 0.035(15) 0.007(10) C34 0.056(9) 0.121(14) 0.124(13) 0.004(12) 0.019(9) 0.008(9) C35 0.115(13) 0.123(13) 0.115(12) -0.024(10) -0.060(12) 0.093(13) C36 0.036(5) 0.047(6) 0.037(5) 0.002(5) 0.014(4) 0.010(5) C37 0.016(3) 0.059(6) 0.026(4) 0.006(4) 0.005(3) 0.023(4) C38 0.042(6) 0.044(6) 0.044(5) 0.001(5) 0.007(5) 0.011(5) C39 0.046(6) 0.062(7) 0.050(6) -0.017(6) 0.008(5) -0.016(6) C40 0.034(6) 0.091(10) 0.067(7) -0.009(7) -0.008(5) 0.000(6) C41 0.030(5) 0.082(9) 0.069(7) -0.008(7) 0.012(5) 0.004(6) C42 0.053(6) 0.069(7) 0.047(6) -0.010(6) -0.005(5) -0.013(6) C43 0.075(8) 0.079(9) 0.042(6) -0.018(6) 0.000(6) 0.025(7) C44 0.120(14) 0.074(10) 0.119(13) 0.047(10) 0.029(11) 0.052(10) C45 0.129(17) 0.050(8) 0.134(16) -0.026(9) 0.038(12) 0.019(9) C46 0.065(8) 0.062(8) 0.071(8) 0.007(7) 0.011(7) -0.045(7) C47 0.121(14) 0.089(11) 0.088(11) -0.035(9) 0.035(11) -0.065(10) C48 0.134(14) 0.062(8) 0.058(8) 0.015(7) 0.027(9) -0.002(9) C49 0.040(7) 0.057(7) 0.119(11) 0.023(7) -0.022(7) -0.017(6) C50 0.154(17) 0.072(9) 0.065(8) 0.021(7) 0.032(11) 0.047(12) C51 0.053(8) 0.132(15) 0.090(11) 0.003(11) -0.020(8) -0.014(9) C52 0.072(9) 0.090(11) 0.084(10) 0.042(9) 0.003(8) -0.013(8) C53 0.068(4) 0.051(3) 0.160(6) -0.014(4) 0.000(4) -0.003(3) C54 0.068(4) 0.051(3) 0.160(6) -0.014(4) 0.000(4) -0.003(3) C55 0.068(4) 0.051(3) 0.160(6) -0.014(4) 0.000(4) -0.003(3) C56 0.068(4) 0.051(3) 0.160(6) -0.014(4) 0.000(4) -0.003(3) _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 Yb1 O2 2.183(6) . ? Yb1 O1 2.191(6) . ? Yb1 N3 2.204(7) . ? Yb1 N1 2.369(8) . ? Yb1 N2 2.389(7) . ? O1 C1 1.384(11) . ? O1 Li1 1.857(17) . ? O2 C22 1.365(10) . ? O2 Li2 1.88(2) . ? O3 C49 1.382(12) . ? O3 C52 1.427(15) . ? O3 Li1 1.90(2) . ? O4 C53 1.343(16) . ? O4 C56 1.364(16) . ? O4 Li2 1.86(2) . ? N1 C16 1.394(11) . ? N1 C15 1.482(12) . ? N1 Li2 2.00(2) . ? N2 C37 1.388(11) . ? N2 C36 1.483(13) . ? N2 Li1 1.995(18) . ? N3 Si1 1.689(10) . ? N3 Si2 1.738(10) . ? Si1 C43 1.852(14) . ? Si1 C45 1.885(15) . ? Si1 C44 1.899(15) . ? Si2 C47 1.865(13) . ? Si2 C46 1.877(14) . ? Si2 C48 1.883(13) . ? Cl1 C17 1.757(9) . ? Cl2 C38 1.744(10) . ? C1 C6 1.400(13) . ? C1 C2 1.407(12) . ? C2 C3 1.365(13) . ? C2 C7 1.523(14) . ? C3 C4 1.368(15) . ? C3 H3 0.9400 . ? C4 C5 1.414(14) . ? C4 C11 1.564(15) . ? C5 C6 1.391(14) . ? C5 H5 0.9400 . ? C6 C15 1.512(13) . ? C7 C8 1.515(13) . ? C7 C9 1.517(14) . ? C7 C10 1.520(13) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C14 1.444(15) . ? C11 C12 1.494(17) . ? C11 C13 1.56(2) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C17 1.366(14) . ? C16 C21 1.431(13) . ? C17 C18 1.390(14) . ? C18 C19 1.344(15) . ? C18 H18 0.9400 . ? C19 C20 1.365(17) . ? C19 H19 0.9400 . ? C20 C21 1.347(15) . ? C20 H20 0.9400 . ? C21 H21 0.9400 . ? C22 C27 1.395(13) . ? C22 C23 1.440(12) . ? C23 C24 1.409(14) . ? C23 C28 1.527(15) . ? C24 C25 1.352(15) . ? C24 H24 0.9400 . ? C25 C26 1.366(15) . ? C25 C32 1.551(15) . ? C26 C27 1.410(14) . ? C26 H26 0.9400 . ? C27 C36 1.506(13) . ? C28 C30 1.494(16) . ? C28 C31 1.500(18) . ? C28 C29 1.578(15) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 C33 1.48(2) . ? C32 C34 1.505(18) . ? C32 C35 1.534(18) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 C42 1.379(13) . ? C37 C38 1.395(14) . ? C38 C39 1.399(15) . ? C39 C40 1.337(15) . ? C39 H39 0.9400 . ? C40 C41 1.328(17) . ? C40 H40 0.9400 . ? C41 C42 1.405(15) . ? C41 H41 0.9400 . ? C42 H42 0.9400 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 H45C 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C46 H46C 0.9700 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C49 C50 1.505(18) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.45(2) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.452(19) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.426(18) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.427(19) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.381(18) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 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 O2 Yb1 O1 138.2(2) . . ? O2 Yb1 N3 111.7(3) . . ? O1 Yb1 N3 110.0(3) . . ? O2 Yb1 N1 79.8(3) . . ? O1 Yb1 N1 80.3(2) . . ? N3 Yb1 N1 115.2(3) . . ? O2 Yb1 N2 80.6(2) . . ? O1 Yb1 N2 78.8(2) . . ? N3 Yb1 N2 123.9(3) . . ? N1 Yb1 N2 120.9(3) . . ? C1 O1 Li1 110.6(8) . . ? C1 O1 Yb1 137.5(5) . . ? Li1 O1 Yb1 96.3(6) . . ? C22 O2 Li2 113.0(8) . . ? C22 O2 Yb1 137.0(6) . . ? Li2 O2 Yb1 95.4(7) . . ? C49 O3 C52 105.4(8) . . ? C49 O3 Li1 132.5(8) . . ? C52 O3 Li1 121.9(9) . . ? C53 O4 C56 107.1(11) . . ? C53 O4 Li2 131.2(11) . . ? C56 O4 Li2 121.5(11) . . ? C16 N1 C15 114.9(8) . . ? C16 N1 Li2 105.2(8) . . ? C15 N1 Li2 106.9(8) . . ? C16 N1 Yb1 130.3(6) . . ? C15 N1 Yb1 106.7(6) . . ? Li2 N1 Yb1 86.7(6) . . ? C37 N2 C36 116.7(8) . . ? C37 N2 Li1 106.6(7) . . ? C36 N2 Li1 107.2(8) . . ? C37 N2 Yb1 129.3(6) . . ? C36 N2 Yb1 104.5(6) . . ? Li1 N2 Yb1 86.7(5) . . ? Si1 N3 Si2 120.2(4) . . ? Si1 N3 Yb1 123.0(5) . . ? Si2 N3 Yb1 116.7(5) . . ? N3 Si1 C43 111.9(5) . . ? N3 Si1 C45 112.8(7) . . ? C43 Si1 C45 106.1(7) . . ? N3 Si1 C44 114.6(6) . . ? C43 Si1 C44 105.3(7) . . ? C45 Si1 C44 105.5(8) . . ? N3 Si2 C47 113.3(6) . . ? N3 Si2 C46 111.8(5) . . ? C47 Si2 C46 105.8(7) . . ? N3 Si2 C48 112.9(6) . . ? C47 Si2 C48 107.0(7) . . ? C46 Si2 C48 105.5(7) . . ? O1 Li1 O3 126.6(11) . . ? O1 Li1 N2 98.0(8) . . ? O3 Li1 N2 116.6(8) . . ? O4 Li2 O2 125.7(12) . . ? O4 Li2 N1 117.9(12) . . ? O2 Li2 N1 97.6(8) . . ? O1 C1 C6 116.5(8) . . ? O1 C1 C2 120.5(9) . . ? C6 C1 C2 122.9(9) . . ? C3 C2 C1 114.9(9) . . ? C3 C2 C7 119.6(8) . . ? C1 C2 C7 125.5(8) . . ? C2 C3 C4 125.7(9) . . ? C2 C3 H3 117.1 . . ? C4 C3 H3 117.1 . . ? C3 C4 C5 117.7(10) . . ? C3 C4 C11 122.1(10) . . ? C5 C4 C11 120.1(11) . . ? C6 C5 C4 120.0(11) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 118.3(9) . . ? C5 C6 C15 120.0(9) . . ? C1 C6 C15 121.6(9) . . ? C8 C7 C9 107.2(9) . . ? C8 C7 C10 105.1(8) . . ? C9 C7 C10 111.4(9) . . ? C8 C7 C2 112.3(9) . . ? C9 C7 C2 110.4(8) . . ? C10 C7 C2 110.2(8) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C12 113.5(11) . . ? C14 C11 C13 105.3(13) . . ? C12 C11 C13 108.4(14) . . ? C14 C11 C4 112.6(11) . . ? C12 C11 C4 111.8(10) . . ? C13 C11 C4 104.5(9) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C6 118.7(8) . . ? N1 C15 H15A 107.6 . . ? C6 C15 H15A 107.6 . . ? N1 C15 H15B 107.6 . . ? C6 C15 H15B 107.6 . . ? H15A C15 H15B 107.1 . . ? C17 C16 N1 121.5(8) . . ? C17 C16 C21 114.2(8) . . ? N1 C16 C21 124.2(8) . . ? C16 C17 C18 125.1(9) . . ? C16 C17 Cl1 117.7(8) . . ? C18 C17 Cl1 117.2(9) . . ? C19 C18 C17 119.4(11) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 116.9(11) . . ? C18 C19 H19 121.5 . . ? C20 C19 H19 121.5 . . ? C21 C20 C19 125.5(11) . . ? C21 C20 H20 117.2 . . ? C19 C20 H20 117.2 . . ? C20 C21 C16 118.8(9) . . ? C20 C21 H21 120.6 . . ? C16 C21 H21 120.6 . . ? O2 C22 C27 118.8(8) . . ? O2 C22 C23 121.6(9) . . ? C27 C22 C23 119.6(9) . . ? C24 C23 C22 115.3(9) . . ? C24 C23 C28 120.6(9) . . ? C22 C23 C28 124.1(9) . . ? C25 C24 C23 125.2(10) . . ? C25 C24 H24 117.4 . . ? C23 C24 H24 117.4 . . ? C24 C25 C26 118.4(10) . . ? C24 C25 C32 119.9(10) . . ? C26 C25 C32 121.7(10) . . ? C25 C26 C27 120.9(10) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C22 C27 C26 120.0(9) . . ? C22 C27 C36 118.6(9) . . ? C26 C27 C36 120.8(9) . . ? C30 C28 C31 111.9(12) . . ? C30 C28 C23 112.7(10) . . ? C31 C28 C23 110.8(9) . . ? C30 C28 C29 104.4(9) . . ? C31 C28 C29 106.6(10) . . ? C23 C28 C29 110.1(10) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C34 108.8(13) . . ? C33 C32 C35 109.7(14) . . ? C34 C32 C35 107.6(13) . . ? C33 C32 C25 109.8(11) . . ? C34 C32 C25 110.8(11) . . ? C35 C32 C25 110.1(10) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N2 C36 C27 117.9(9) . . ? N2 C36 H36A 107.8 . . ? C27 C36 H36A 107.8 . . ? N2 C36 H36B 107.8 . . ? C27 C36 H36B 107.8 . . ? H36A C36 H36B 107.2 . . ? C42 C37 N2 126.3(9) . . ? C42 C37 C38 112.1(9) . . ? N2 C37 C38 121.5(8) . . ? C37 C38 C39 125.3(9) . . ? C37 C38 Cl2 117.3(8) . . ? C39 C38 Cl2 117.2(8) . . ? C40 C39 C38 116.8(11) . . ? C40 C39 H39 121.6 . . ? C38 C39 H39 121.6 . . ? C41 C40 C39 123.1(11) . . ? C41 C40 H40 118.5 . . ? C39 C40 H40 118.5 . . ? C40 C41 C42 118.4(11) . . ? C40 C41 H41 120.8 . . ? C42 C41 H41 120.8 . . ? C37 C42 C41 124.1(11) . . ? C37 C42 H42 117.9 . . ? C41 C42 H42 117.9 . . ? Si1 C43 H43A 109.5 . . ? Si1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si1 C44 H44A 109.5 . . ? Si1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si1 C45 H45A 109.5 . . ? Si1 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si1 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si2 C46 H46A 109.5 . . ? Si2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? Si2 C47 H47A 109.5 . . ? Si2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Si2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? Si2 C48 H48A 109.5 . . ? Si2 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si2 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O3 C49 C50 105.7(11) . . ? O3 C49 H49A 110.6 . . ? C50 C49 H49A 110.6 . . ? O3 C49 H49B 110.6 . . ? C50 C49 H49B 110.6 . . ? H49A C49 H49B 108.7 . . ? C51 C50 C49 104.6(12) . . ? C51 C50 H50A 110.8 . . ? C49 C50 H50A 110.8 . . ? C51 C50 H50B 110.8 . . ? C49 C50 H50B 110.8 . . ? H50A C50 H50B 108.9 . . ? C50 C51 C52 104.7(12) . . ? C50 C51 H51A 110.8 . . ? C52 C51 H51A 110.8 . . ? C50 C51 H51B 110.8 . . ? C52 C51 H51B 110.8 . . ? H51A C51 H51B 108.9 . . ? O3 C52 C51 109.8(11) . . ? O3 C52 H52A 109.7 . . ? C51 C52 H52A 109.7 . . ? O3 C52 H52B 109.7 . . ? C51 C52 H52B 109.7 . . ? H52A C52 H52B 108.2 . . ? O4 C53 C54 111.3(14) . . ? O4 C53 H53A 109.4 . . ? C54 C53 H53A 109.4 . . ? O4 C53 H53B 109.4 . . ? C54 C53 H53B 109.4 . . ? H53A C53 H53B 108.0 . . ? C53 C54 C55 100.9(13) . . ? C53 C54 H54A 111.6 . . ? C55 C54 H54A 111.6 . . ? C53 C54 H54B 111.6 . . ? C55 C54 H54B 111.6 . . ? H54A C54 H54B 109.4 . . ? C56 C55 C54 108.1(13) . . ? C56 C55 H55A 110.1 . . ? C54 C55 H55A 110.1 . . ? C56 C55 H55B 110.1 . . ? C54 C55 H55B 110.1 . . ? H55A C55 H55B 108.4 . . ? O4 C56 C55 108.6(13) . . ? O4 C56 H56A 110.0 . . ? C55 C56 H56A 110.0 . . ? O4 C56 H56B 110.0 . . ? C55 C56 H56B 110.0 . . ? H56A C56 H56B 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 O2 Yb1 O1 C1 65.1(10) . . . . ? N3 Yb1 O1 C1 -110.8(9) . . . . ? N1 Yb1 O1 C1 2.5(9) . . . . ? N2 Yb1 O1 C1 127.0(9) . . . . ? O2 Yb1 O1 Li1 -65.0(7) . . . . ? N3 Yb1 O1 Li1 119.1(7) . . . . ? N1 Yb1 O1 Li1 -127.6(7) . . . . ? N2 Yb1 O1 Li1 -3.1(6) . . . . ? O1 Yb1 O2 C22 64.9(9) . . . . ? N3 Yb1 O2 C22 -119.2(8) . . . . ? N1 Yb1 O2 C22 127.6(8) . . . . ? N2 Yb1 O2 C22 3.6(8) . . . . ? O1 Yb1 O2 Li2 -67.6(7) . . . . ? N3 Yb1 O2 Li2 108.3(7) . . . . ? N1 Yb1 O2 Li2 -4.9(7) . . . . ? N2 Yb1 O2 Li2 -128.9(7) . . . . ? O2 Yb1 N1 C16 111.8(8) . . . . ? O1 Yb1 N1 C16 -105.2(8) . . . . ? N3 Yb1 N1 C16 2.5(8) . . . . ? N2 Yb1 N1 C16 -175.7(7) . . . . ? O2 Yb1 N1 C15 -102.1(6) . . . . ? O1 Yb1 N1 C15 41.0(6) . . . . ? N3 Yb1 N1 C15 148.6(6) . . . . ? N2 Yb1 N1 C15 -29.5(7) . . . . ? O2 Yb1 N1 Li2 4.6(6) . . . . ? O1 Yb1 N1 Li2 147.6(6) . . . . ? N3 Yb1 N1 Li2 -104.7(6) . . . . ? N2 Yb1 N1 Li2 77.1(7) . . . . ? O2 Yb1 N2 C37 -104.8(7) . . . . ? O1 Yb1 N2 C37 111.7(7) . . . . ? N3 Yb1 N2 C37 5.0(8) . . . . ? N1 Yb1 N2 C37 -177.0(7) . . . . ? O2 Yb1 N2 C36 39.4(5) . . . . ? O1 Yb1 N2 C36 -104.0(6) . . . . ? N3 Yb1 N2 C36 149.3(5) . . . . ? N1 Yb1 N2 C36 -32.7(6) . . . . ? O2 Yb1 N2 Li1 146.3(6) . . . . ? O1 Yb1 N2 Li1 2.9(6) . . . . ? N3 Yb1 N2 Li1 -103.8(6) . . . . ? N1 Yb1 N2 Li1 74.2(7) . . . . ? O2 Yb1 N3 Si1 -130.6(5) . . . . ? O1 Yb1 N3 Si1 46.5(6) . . . . ? N1 Yb1 N3 Si1 -41.9(6) . . . . ? N2 Yb1 N3 Si1 136.2(5) . . . . ? O2 Yb1 N3 Si2 49.4(5) . . . . ? O1 Yb1 N3 Si2 -133.5(4) . . . . ? N1 Yb1 N3 Si2 138.1(4) . . . . ? N2 Yb1 N3 Si2 -43.8(5) . . . . ? Si2 N3 Si1 C43 -176.4(5) . . . . ? Yb1 N3 Si1 C43 3.6(7) . . . . ? Si2 N3 Si1 C45 64.0(8) . . . . ? Yb1 N3 Si1 C45 -115.9(7) . . . . ? Si2 N3 Si1 C44 -56.7(9) . . . . ? Yb1 N3 Si1 C44 123.3(7) . . . . ? Si1 N3 Si2 C47 -54.3(9) . . . . ? Yb1 N3 Si2 C47 125.7(8) . . . . ? Si1 N3 Si2 C46 -173.7(6) . . . . ? Yb1 N3 Si2 C46 6.3(7) . . . . ? Si1 N3 Si2 C48 67.5(7) . . . . ? Yb1 N3 Si2 C48 -112.5(6) . . . . ? C1 O1 Li1 O3 -11.0(13) . . . . ? Yb1 O1 Li1 O3 135.6(9) . . . . ? C1 O1 Li1 N2 -142.8(8) . . . . ? Yb1 O1 Li1 N2 3.7(8) . . . . ? C49 O3 Li1 O1 4.0(18) . . . . ? C52 O3 Li1 O1 178.9(11) . . . . ? C49 O3 Li1 N2 128.4(13) . . . . ? C52 O3 Li1 N2 -56.7(15) . . . . ? C37 N2 Li1 O1 -133.6(8) . . . . ? C36 N2 Li1 O1 100.8(9) . . . . ? Yb1 N2 Li1 O1 -3.4(7) . . . . ? C37 N2 Li1 O3 88.4(11) . . . . ? C36 N2 Li1 O3 -37.3(12) . . . . ? Yb1 N2 Li1 O3 -141.4(9) . . . . ? C53 O4 Li2 O2 -11(2) . . . . ? C56 O4 Li2 O2 175.0(14) . . . . ? C53 O4 Li2 N1 113.3(17) . . . . ? C56 O4 Li2 N1 -60.5(18) . . . . ? C22 O2 Li2 O4 -8.5(16) . . . . ? Yb1 O2 Li2 O4 138.4(12) . . . . ? C22 O2 Li2 N1 -141.1(8) . . . . ? Yb1 O2 Li2 N1 5.8(8) . . . . ? C16 N1 Li2 O4 86.2(12) . . . . ? C15 N1 Li2 O4 -36.4(13) . . . . ? Yb1 N1 Li2 O4 -142.8(10) . . . . ? C16 N1 Li2 O2 -136.3(8) . . . . ? C15 N1 Li2 O2 101.1(9) . . . . ? Yb1 N1 Li2 O2 -5.3(7) . . . . ? Li1 O1 C1 C6 97.8(10) . . . . ? Yb1 O1 C1 C6 -27.9(14) . . . . ? Li1 O1 C1 C2 -77.6(11) . . . . ? Yb1 O1 C1 C2 156.6(7) . . . . ? O1 C1 C2 C3 167.0(8) . . . . ? C6 C1 C2 C3 -8.1(14) . . . . ? O1 C1 C2 C7 -11.4(14) . . . . ? C6 C1 C2 C7 173.5(9) . . . . ? C1 C2 C3 C4 3.3(14) . . . . ? C7 C2 C3 C4 -178.2(9) . . . . ? C2 C3 C4 C5 2.6(14) . . . . ? C2 C3 C4 C11 -179.4(9) . . . . ? C3 C4 C5 C6 -4.1(13) . . . . ? C11 C4 C5 C6 177.9(9) . . . . ? C4 C5 C6 C1 -0.4(14) . . . . ? C4 C5 C6 C15 -176.1(9) . . . . ? O1 C1 C6 C5 -168.5(8) . . . . ? C2 C1 C6 C5 6.9(15) . . . . ? O1 C1 C6 C15 7.1(14) . . . . ? C2 C1 C6 C15 -177.5(9) . . . . ? C3 C2 C7 C8 15.7(13) . . . . ? C1 C2 C7 C8 -166.0(10) . . . . ? C3 C2 C7 C9 135.3(9) . . . . ? C1 C2 C7 C9 -46.4(12) . . . . ? C3 C2 C7 C10 -101.2(10) . . . . ? C1 C2 C7 C10 77.2(11) . . . . ? C3 C4 C11 C14 -35.1(14) . . . . ? C5 C4 C11 C14 142.8(11) . . . . ? C3 C4 C11 C12 -164.3(12) . . . . ? C5 C4 C11 C12 13.6(15) . . . . ? C3 C4 C11 C13 78.6(15) . . . . ? C5 C4 C11 C13 -103.4(14) . . . . ? C16 N1 C15 C6 77.7(11) . . . . ? Li2 N1 C15 C6 -166.0(9) . . . . ? Yb1 N1 C15 C6 -74.4(9) . . . . ? C5 C6 C15 N1 -134.3(10) . . . . ? C1 C6 C15 N1 50.2(14) . . . . ? C15 N1 C16 C17 166.6(9) . . . . ? Li2 N1 C16 C17 49.3(12) . . . . ? Yb1 N1 C16 C17 -49.4(12) . . . . ? C15 N1 C16 C21 -15.8(13) . . . . ? Li2 N1 C16 C21 -133.1(11) . . . . ? Yb1 N1 C16 C21 128.2(9) . . . . ? N1 C16 C17 C18 176.2(10) . . . . ? C21 C16 C17 C18 -1.7(16) . . . . ? N1 C16 C17 Cl1 -3.6(13) . . . . ? C21 C16 C17 Cl1 178.5(8) . . . . ? C16 C17 C18 C19 1.9(19) . . . . ? Cl1 C17 C18 C19 -178.4(10) . . . . ? C17 C18 C19 C20 -0.3(19) . . . . ? C18 C19 C20 C21 -1(2) . . . . ? C19 C20 C21 C16 1.5(19) . . . . ? C17 C16 C21 C20 0.1(15) . . . . ? N1 C16 C21 C20 -177.7(10) . . . . ? Li2 O2 C22 C27 101.8(10) . . . . ? Yb1 O2 C22 C27 -25.3(13) . . . . ? Li2 O2 C22 C23 -76.8(11) . . . . ? Yb1 O2 C22 C23 156.1(7) . . . . ? O2 C22 C23 C24 171.9(8) . . . . ? C27 C22 C23 C24 -6.7(13) . . . . ? O2 C22 C23 C28 -6.9(14) . . . . ? C27 C22 C23 C28 174.5(9) . . . . ? C22 C23 C24 C25 0.8(15) . . . . ? C28 C23 C24 C25 179.5(10) . . . . ? C23 C24 C25 C26 4.8(17) . . . . ? C23 C24 C25 C32 -175.4(10) . . . . ? C24 C25 C26 C27 -4.3(17) . . . . ? C32 C25 C26 C27 175.8(9) . . . . ? O2 C22 C27 C26 -171.4(8) . . . . ? C23 C22 C27 C26 7.2(14) . . . . ? O2 C22 C27 C36 -0.3(13) . . . . ? C23 C22 C27 C36 178.4(9) . . . . ? C25 C26 C27 C22 -1.6(16) . . . . ? C25 C26 C27 C36 -172.5(10) . . . . ? C24 C23 C28 C30 -101.3(12) . . . . ? C22 C23 C28 C30 77.3(14) . . . . ? C24 C23 C28 C31 132.4(11) . . . . ? C22 C23 C28 C31 -48.9(14) . . . . ? C24 C23 C28 C29 14.7(14) . . . . ? C22 C23 C28 C29 -166.6(10) . . . . ? C24 C25 C32 C33 80.6(16) . . . . ? C26 C25 C32 C33 -99.6(15) . . . . ? C24 C25 C32 C34 -39.6(16) . . . . ? C26 C25 C32 C34 140.2(13) . . . . ? C24 C25 C32 C35 -158.5(13) . . . . ? C26 C25 C32 C35 21.3(17) . . . . ? C37 N2 C36 C27 71.5(11) . . . . ? Li1 N2 C36 C27 -169.2(9) . . . . ? Yb1 N2 C36 C27 -78.1(9) . . . . ? C22 C27 C36 N2 60.0(13) . . . . ? C26 C27 C36 N2 -129.0(10) . . . . ? C36 N2 C37 C42 -5.9(13) . . . . ? Li1 N2 C37 C42 -125.6(11) . . . . ? Yb1 N2 C37 C42 134.8(9) . . . . ? C36 N2 C37 C38 170.0(8) . . . . ? Li1 N2 C37 C38 50.3(11) . . . . ? Yb1 N2 C37 C38 -49.3(11) . . . . ? C42 C37 C38 C39 -4.8(15) . . . . ? N2 C37 C38 C39 178.8(10) . . . . ? C42 C37 C38 Cl2 179.6(8) . . . . ? N2 C37 C38 Cl2 3.2(12) . . . . ? C37 C38 C39 C40 4.5(17) . . . . ? Cl2 C38 C39 C40 -179.9(9) . . . . ? C38 C39 C40 C41 -3.4(19) . . . . ? C39 C40 C41 C42 3(2) . . . . ? N2 C37 C42 C41 -179.4(10) . . . . ? C38 C37 C42 C41 4.4(15) . . . . ? C40 C41 C42 C37 -3.8(18) . . . . ? C52 O3 C49 C50 -30.7(14) . . . . ? Li1 O3 C49 C50 144.9(11) . . . . ? O3 C49 C50 C51 30.2(16) . . . . ? C49 C50 C51 C52 -16.9(18) . . . . ? C49 O3 C52 C51 20.5(17) . . . . ? Li1 O3 C52 C51 -155.6(12) . . . . ? C50 C51 C52 O3 -1.1(19) . . . . ? C56 O4 C53 C54 -10(2) . . . . ? Li2 O4 C53 C54 175.0(15) . . . . ? O4 C53 C54 C55 18(2) . . . . ? C53 C54 C55 C56 -19(2) . . . . ? C53 O4 C56 C55 -3(2) . . . . ? Li2 O4 C56 C55 172.6(14) . . . . ? C54 C55 C56 O4 14(2) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.439 _refine_diff_density_min -1.972 _refine_diff_density_rms 0.150 _database_code_depnum_ccdc_archive 'CCDC 932406' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H111 Li3 N3 O9 Y, 1.5(C6 H14)' _chemical_formula_sum 'C87 H132 Li3 N3 O9 Y' _chemical_formula_weight 1473.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Y Y -2.7962 3.5667 '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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.5789(8) _cell_length_b 16.5947(8) _cell_length_c 17.4085(13) _cell_angle_alpha 81.215(7) _cell_angle_beta 76.870(7) _cell_angle_gamma 68.303(6) _cell_volume 4321.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 18715 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description chip _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1590 _exptl_absorpt_coefficient_mu 0.729 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.507 _exptl_absorpt_correction_T_max 0.760 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35555 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_unetI/netI 0.0992 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.50 _reflns_number_total 15957 _reflns_number_gt 11649 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Their C73-C74,C68'- C69', C63-C66,C63-C65',C67'-C68',C69'-C70',C67-C68,C68-C69,C69-C70, O7-C67', O7-C70',O7-C67,07-C70,C79'-C80',C80'-C81',C81'-C82',C82'-C83',C83'-C84' C79-C80,C80-C81,C81-C82,C82-C83,C83-C84,C85-C86,C86-C87,C87-C88,C88-C89, C89-C90, C19-C20',C19-C21',C19-C20,C19-C21,C19-C22'and C19-C22 distances were constrained. ; _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^)+(0.0952P)^2^+4.4888P] 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 15957 _refine_ls_number_parameters 880 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1280 _refine_ls_R_factor_gt 0.0947 _refine_ls_wR_factor_ref 0.2318 _refine_ls_wR_factor_gt 0.2094 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.53773(3) 0.19740(3) 0.19406(3) 0.03514(16) Uani 1 1 d . C . O1 O 0.6758(2) 0.1992(2) 0.1487(2) 0.0397(8) Uani 1 1 d . . . O2 O 0.1649(3) 0.5525(3) 0.1191(3) 0.0706(12) Uani 1 1 d . . . O3 O 0.5679(2) 0.0559(2) 0.24450(19) 0.0409(8) Uani 1 1 d . C . O4 O 0.4000(3) 0.3001(2) -0.1725(2) 0.0652(12) Uani 1 1 d . C . O5 O 0.4093(2) 0.1778(2) 0.21508(19) 0.0382(8) Uani 1 1 d . C . O6 O 0.7122(3) 0.2602(3) 0.5066(3) 0.0820(14) Uani 1 1 d . C . O7 O 0.7578(3) 0.1633(3) -0.0451(2) 0.0715(12) Uani 1 1 d D . . O8 O 0.3844(3) -0.0087(3) 0.3065(2) 0.0657(11) Uani 1 1 d . C . O9 O 0.4721(3) 0.4793(3) 0.3065(3) 0.0805(14) Uani 1 1 d . . . N1 N 0.5117(2) 0.3504(2) 0.1608(2) 0.0365(9) Uani 1 1 d . C . N2 N 0.5824(3) 0.1224(2) 0.0727(2) 0.0385(9) Uani 1 1 d . . . N3 N 0.4756(3) 0.2454(2) 0.3269(2) 0.0376(9) Uani 1 1 d . . . C1 C 0.7171(3) 0.2563(3) 0.1487(3) 0.0386(11) Uani 1 1 d . . . C2 C 0.8042(3) 0.2291(3) 0.1618(3) 0.0430(12) Uani 1 1 d . . . C3 C 0.8413(4) 0.2927(3) 0.1585(3) 0.0510(14) Uani 1 1 d . . . H3 H 0.8998 0.2747 0.1665 0.061 Uiso 1 1 calc R . . C4 C 0.7971(4) 0.3811(3) 0.1440(4) 0.0529(14) Uani 1 1 d . A . C5 C 0.7108(4) 0.4056(3) 0.1323(3) 0.0474(13) Uani 1 1 d . . . H5 H 0.6785 0.4649 0.1232 0.057 Uiso 1 1 calc R . . C6 C 0.6708(3) 0.3447(3) 0.1335(3) 0.0390(11) Uani 1 1 d . . . C7 C 0.5808(3) 0.3781(3) 0.1094(3) 0.0409(11) Uani 1 1 d . . . H7A H 0.5599 0.4419 0.1056 0.049 Uiso 1 1 calc R . . H7B H 0.5886 0.3602 0.0564 0.049 Uiso 1 1 calc R . . C8 C 0.4262(3) 0.4020(3) 0.1481(3) 0.0368(11) Uani 1 1 d . . . C9 C 0.4058(3) 0.4615(3) 0.0819(3) 0.0441(12) Uani 1 1 d . C . H9 H 0.4519 0.4685 0.0418 0.053 Uiso 1 1 calc R . . C10 C 0.3195(4) 0.5094(4) 0.0748(3) 0.0534(14) Uani 1 1 d . . . H10 H 0.3081 0.5484 0.0301 0.064 Uiso 1 1 calc R C . C11 C 0.2493(4) 0.5013(3) 0.1320(4) 0.0514(14) Uani 1 1 d . C . C12 C 0.2669(3) 0.4448(3) 0.1974(3) 0.0492(13) Uani 1 1 d . . . H12 H 0.2202 0.4384 0.2372 0.059 Uiso 1 1 calc R C . C13 C 0.3539(3) 0.3970(3) 0.2047(3) 0.0444(12) Uani 1 1 d . C . H13 H 0.3643 0.3594 0.2504 0.053 Uiso 1 1 calc R . . C14 C 0.0955(4) 0.5256(5) 0.1628(6) 0.099(3) Uani 1 1 d . . . H14A H 0.1098 0.4643 0.1572 0.149 Uiso 1 1 calc R . . H14B H 0.0415 0.5591 0.1431 0.149 Uiso 1 1 calc R . . H14C H 0.0873 0.5347 0.2182 0.149 Uiso 1 1 calc R . . C15 C 0.8599(3) 0.1324(3) 0.1795(3) 0.0475(13) Uani 1 1 d . . . C16 C 0.9533(4) 0.1204(4) 0.1907(4) 0.0714(18) Uani 1 1 d . . . H16A H 0.9854 0.1396 0.1421 0.107 Uiso 1 1 calc R . . H16B H 0.9844 0.0594 0.2042 0.107 Uiso 1 1 calc R . . H16C H 0.9489 0.1545 0.2330 0.107 Uiso 1 1 calc R . . C17 C 0.8702(4) 0.0777(4) 0.1115(4) 0.0716(19) Uani 1 1 d . . . H17A H 0.8141 0.0717 0.1119 0.107 Uiso 1 1 calc R . . H17B H 0.9144 0.0206 0.1185 0.107 Uiso 1 1 calc R . . H17C H 0.8887 0.1065 0.0614 0.107 Uiso 1 1 calc R . . C18 C 0.8140(4) 0.0957(4) 0.2556(4) 0.0658(17) Uani 1 1 d . . . H18A H 0.8072 0.1293 0.2991 0.099 Uiso 1 1 calc R . . H18B H 0.8494 0.0355 0.2670 0.099 Uiso 1 1 calc R . . H18C H 0.7563 0.0991 0.2490 0.099 Uiso 1 1 calc R . . C19 C 0.8432(4) 0.4474(4) 0.1372(4) 0.074(2) Uani 1 1 d D . . C20 C 0.8860(12) 0.4334(11) 0.2091(9) 0.097(2) Uiso 0.50 1 d PD A 1 H20A H 0.9310 0.3759 0.2101 0.145 Uiso 0.50 1 calc PR A 1 H20B H 0.8415 0.4383 0.2569 0.145 Uiso 0.50 1 calc PR A 1 H20C H 0.9129 0.4770 0.2061 0.145 Uiso 0.50 1 calc PR A 1 C20' C 0.8070(11) 0.4929(11) 0.2162(9) 0.097(2) Uiso 0.50 1 d PD A 2 H20D H 0.8157 0.4492 0.2605 0.145 Uiso 0.50 1 calc PR A 2 H20E H 0.7445 0.5261 0.2199 0.145 Uiso 0.50 1 calc PR A 2 H20F H 0.8384 0.5316 0.2176 0.145 Uiso 0.50 1 calc PR A 2 C21 C 0.7886(12) 0.5397(9) 0.1130(11) 0.097(2) Uiso 0.50 1 d PD A 1 H21A H 0.8253 0.5756 0.1015 0.145 Uiso 0.50 1 calc PR A 1 H21B H 0.7397 0.5626 0.1557 0.145 Uiso 0.50 1 calc PR A 1 H21C H 0.7660 0.5401 0.0662 0.145 Uiso 0.50 1 calc PR A 1 C21' C 0.8140(12) 0.5215(10) 0.0751(9) 0.097(2) Uiso 0.50 1 d PD A 2 H21D H 0.8434 0.5627 0.0739 0.145 Uiso 0.50 1 calc PR A 2 H21E H 0.7505 0.5507 0.0880 0.145 Uiso 0.50 1 calc PR A 2 H21F H 0.8294 0.4986 0.0236 0.145 Uiso 0.50 1 calc PR A 2 C22 C 0.9237(10) 0.4204(11) 0.0724(10) 0.097(2) Uiso 0.50 1 d PD A 1 H22A H 0.9564 0.4594 0.0676 0.145 Uiso 0.50 1 calc PR A 1 H22B H 0.9054 0.4231 0.0227 0.145 Uiso 0.50 1 calc PR A 1 H22C H 0.9611 0.3614 0.0854 0.145 Uiso 0.50 1 calc PR A 1 C22' C 0.9411(9) 0.4126(11) 0.1299(11) 0.097(2) Uiso 0.50 1 d PD A 2 H22D H 0.9683 0.3939 0.0770 0.145 Uiso 0.50 1 calc PR A 2 H22E H 0.9578 0.3635 0.1684 0.145 Uiso 0.50 1 calc PR A 2 H22F H 0.9609 0.4577 0.1394 0.145 Uiso 0.50 1 calc PR A 2 C23 C 0.6457(3) -0.0079(3) 0.2186(3) 0.0365(11) Uani 1 1 d . C . C24 C 0.7011(3) -0.0632(3) 0.2705(3) 0.0404(12) Uani 1 1 d . . . C25 C 0.7818(3) -0.1217(3) 0.2359(3) 0.0452(13) Uani 1 1 d . . . H25 H 0.8203 -0.1573 0.2695 0.054 Uiso 1 1 calc R . . C26 C 0.8092(3) -0.1307(3) 0.1553(3) 0.0439(12) Uani 1 1 d . . . C27 C 0.7503(3) -0.0801(3) 0.1072(3) 0.0446(12) Uani 1 1 d . C . H27 H 0.7655 -0.0866 0.0525 0.053 Uiso 1 1 calc R . . C28 C 0.6691(3) -0.0196(3) 0.1377(3) 0.0387(11) Uani 1 1 d . . . C29 C 0.6024(3) 0.0278(3) 0.0843(3) 0.0412(12) Uani 1 1 d . C . H29A H 0.6251 0.0035 0.0326 0.049 Uiso 1 1 calc R . . H29B H 0.5474 0.0167 0.1069 0.049 Uiso 1 1 calc R . . C30 C 0.5364(3) 0.1613(3) 0.0107(3) 0.0362(11) Uani 1 1 d . C . C31 C 0.5154(4) 0.2516(3) -0.0084(3) 0.0453(12) Uani 1 1 d . . . H31 H 0.5329 0.2833 0.0210 0.054 Uiso 1 1 calc R C . C32 C 0.4704(4) 0.2951(3) -0.0681(3) 0.0530(14) Uani 1 1 d . C . H32 H 0.4570 0.3555 -0.0782 0.064 Uiso 1 1 calc R . . C33 C 0.4449(4) 0.2508(3) -0.1134(3) 0.0483(13) Uani 1 1 d . . . C34 C 0.4636(4) 0.1628(3) -0.0973(3) 0.0504(14) Uani 1 1 d . C . H34 H 0.4459 0.1321 -0.1274 0.060 Uiso 1 1 calc R . . C35 C 0.5088(3) 0.1192(3) -0.0364(3) 0.0431(12) Uani 1 1 d . . . H35 H 0.5213 0.0590 -0.0265 0.052 Uiso 1 1 calc R C . C36 C 0.3660(5) 0.2569(4) -0.2143(4) 0.079(2) Uani 1 1 d . . . H36A H 0.4145 0.2118 -0.2428 0.119 Uiso 1 1 calc R C . H36B H 0.3329 0.2985 -0.2515 0.119 Uiso 1 1 calc R . . H36C H 0.3274 0.2311 -0.1773 0.119 Uiso 1 1 calc R . . C37 C 0.6724(4) -0.0636(3) 0.3614(3) 0.0488(13) Uani 1 1 d . . . C38 C 0.7434(5) -0.1283(4) 0.4045(4) 0.082(2) Uani 1 1 d . . . H38A H 0.7945 -0.1102 0.3941 0.123 Uiso 1 1 calc R . . H38B H 0.7606 -0.1856 0.3860 0.123 Uiso 1 1 calc R . . H38C H 0.7204 -0.1302 0.4610 0.123 Uiso 1 1 calc R . . C39 C 0.5908(5) -0.0905(5) 0.3849(4) 0.077(2) Uani 1 1 d . . . H39A H 0.5701 -0.0885 0.4416 0.116 Uiso 1 1 calc R . . H39B H 0.6058 -0.1491 0.3703 0.116 Uiso 1 1 calc R . . H39C H 0.5445 -0.0507 0.3578 0.116 Uiso 1 1 calc R . . C40 C 0.6499(5) 0.0259(4) 0.3911(3) 0.0633(17) Uani 1 1 d . . . H40A H 0.7032 0.0400 0.3826 0.095 Uiso 1 1 calc R . . H40B H 0.6247 0.0249 0.4471 0.095 Uiso 1 1 calc R . . H40C H 0.6075 0.0695 0.3623 0.095 Uiso 1 1 calc R . . C41 C 0.8981(4) -0.1990(3) 0.1203(3) 0.0526(14) Uani 1 1 d . . . C42 C 0.8800(4) -0.2778(4) 0.1037(4) 0.0731(19) Uani 1 1 d . . . H42A H 0.8374 -0.2595 0.0687 0.110 Uiso 1 1 calc R . . H42B H 0.8564 -0.3042 0.1531 0.110 Uiso 1 1 calc R . . H42C H 0.9345 -0.3199 0.0788 0.110 Uiso 1 1 calc R . . C43 C 0.9409(4) -0.1617(4) 0.0428(4) 0.077(2) Uani 1 1 d . . . H43A H 0.9967 -0.2052 0.0220 0.116 Uiso 1 1 calc R . . H43B H 0.9513 -0.1107 0.0526 0.116 Uiso 1 1 calc R . . H43C H 0.9019 -0.1457 0.0048 0.116 Uiso 1 1 calc R . . C44 C 0.9638(4) -0.2282(5) 0.1768(4) 0.082(2) Uani 1 1 d . . . H44A H 0.9390 -0.2537 0.2260 0.124 Uiso 1 1 calc R . . H44B H 0.9758 -0.1784 0.1874 0.124 Uiso 1 1 calc R . . H44C H 1.0184 -0.2709 0.1528 0.124 Uiso 1 1 calc R . . C45 C 0.3284(3) 0.2131(3) 0.2593(3) 0.0383(11) Uani 1 1 d . C . C46 C 0.2507(3) 0.2267(4) 0.2314(3) 0.0474(13) Uani 1 1 d . . . C47 C 0.1694(4) 0.2634(4) 0.2821(3) 0.0542(14) Uani 1 1 d . . . H47 H 0.1172 0.2733 0.2636 0.065 Uiso 1 1 calc R . . C48 C 0.1620(3) 0.2858(4) 0.3577(3) 0.0498(13) Uani 1 1 d . B . C49 C 0.2398(3) 0.2717(3) 0.3825(3) 0.0473(13) Uani 1 1 d . B . H49 H 0.2367 0.2870 0.4332 0.057 Uiso 1 1 calc R . . C50 C 0.3228(3) 0.2358(3) 0.3358(3) 0.0412(12) Uani 1 1 d . . . C51 C 0.4038(3) 0.2157(3) 0.3722(3) 0.0418(12) Uani 1 1 d . C . H51A H 0.3840 0.2413 0.4234 0.050 Uiso 1 1 calc R . . H51B H 0.4286 0.1525 0.3830 0.050 Uiso 1 1 calc R . . C52 C 0.5331(3) 0.2472(3) 0.3737(3) 0.0379(11) Uani 1 1 d . C . C53 C 0.5229(4) 0.2320(3) 0.4572(3) 0.0448(12) Uani 1 1 d . . . H53 H 0.4740 0.2178 0.4859 0.054 Uiso 1 1 calc R C . C54 C 0.5831(4) 0.2375(4) 0.4970(3) 0.0557(15) Uani 1 1 d . C . H54 H 0.5743 0.2264 0.5523 0.067 Uiso 1 1 calc R . . C55 C 0.6554(4) 0.2585(4) 0.4592(4) 0.0554(15) Uani 1 1 d . . . C56 C 0.6680(4) 0.2746(4) 0.3777(3) 0.0544(14) Uani 1 1 d . C . H56 H 0.7172 0.2889 0.3502 0.065 Uiso 1 1 calc R . . C57 C 0.6076(4) 0.2695(3) 0.3374(3) 0.0475(13) Uani 1 1 d . . . H57 H 0.6168 0.2817 0.2822 0.057 Uiso 1 1 calc R C . C58 C 0.7967(5) 0.2583(6) 0.4670(6) 0.109(3) Uani 1 1 d . . . H58A H 0.8238 0.2091 0.4346 0.164 Uiso 1 1 calc R C . H58B H 0.8329 0.2527 0.5055 0.164 Uiso 1 1 calc R . . H58C H 0.7917 0.3117 0.4336 0.164 Uiso 1 1 calc R . . C59 C 0.2525(4) 0.2061(4) 0.1483(3) 0.0556(15) Uani 1 1 d . . . C60 C 0.1592(5) 0.2186(7) 0.1344(5) 0.100(3) Uani 1 1 d . . . H60A H 0.1369 0.1768 0.1690 0.150 Uiso 1 1 calc R . . H60B H 0.1628 0.2097 0.0797 0.150 Uiso 1 1 calc R . . H60C H 0.1195 0.2771 0.1458 0.150 Uiso 1 1 calc R . . C61 C 0.3095(5) 0.1106(4) 0.1335(4) 0.0753(19) Uani 1 1 d . . . H61A H 0.3707 0.1014 0.1340 0.113 Uiso 1 1 calc R . . H61B H 0.3048 0.0979 0.0824 0.113 Uiso 1 1 calc R . . H61C H 0.2889 0.0725 0.1747 0.113 Uiso 1 1 calc R . . C62 C 0.2908(4) 0.2651(4) 0.0857(3) 0.0684(18) Uani 1 1 d . . . H62A H 0.2508 0.3248 0.0889 0.103 Uiso 1 1 calc R . . H62B H 0.2981 0.2468 0.0334 0.103 Uiso 1 1 calc R . . H62C H 0.3477 0.2607 0.0953 0.103 Uiso 1 1 calc R . . C63 C 0.0710(4) 0.3238(4) 0.4102(4) 0.0665(17) Uani 1 1 d D . . C64 C 0.0326(13) 0.2526(12) 0.4367(12) 0.107(2) Uiso 0.50 1 d P B 1 H64A H 0.0707 0.2067 0.4676 0.160 Uiso 0.50 1 calc PR B 1 H64B H 0.0281 0.2291 0.3908 0.160 Uiso 0.50 1 calc PR B 1 H64C H -0.0257 0.2760 0.4689 0.160 Uiso 0.50 1 calc PR B 1 C64' C 0.0049(13) 0.2882(12) 0.3940(12) 0.107(2) Uiso 0.50 1 d P B 2 H64D H 0.0293 0.2251 0.3975 0.160 Uiso 0.50 1 calc PR B 2 H64E H -0.0077 0.3094 0.3413 0.160 Uiso 0.50 1 calc PR B 2 H64F H -0.0493 0.3072 0.4327 0.160 Uiso 0.50 1 calc PR B 2 C65 C 0.0115(13) 0.4008(12) 0.3652(12) 0.107(2) Uiso 0.50 1 d P B 1 H65A H -0.0428 0.4293 0.4009 0.160 Uiso 0.50 1 calc PR B 1 H65B H -0.0023 0.3801 0.3223 0.160 Uiso 0.50 1 calc PR B 1 H65C H 0.0417 0.4417 0.3439 0.160 Uiso 0.50 1 calc PR B 1 C65' C 0.0352(13) 0.4222(9) 0.3889(12) 0.107(2) Uiso 0.50 1 d PD B 2 H65D H -0.0227 0.4475 0.4212 0.160 Uiso 0.50 1 calc PR B 2 H65E H 0.0306 0.4330 0.3335 0.160 Uiso 0.50 1 calc PR B 2 H65F H 0.0751 0.4483 0.3987 0.160 Uiso 0.50 1 calc PR B 2 C66 C 0.0760(13) 0.3585(12) 0.4848(10) 0.107(2) Uiso 0.50 1 d PD B 1 H66A H 0.1098 0.3109 0.5175 0.160 Uiso 0.50 1 calc PR B 1 H66B H 0.0168 0.3850 0.5143 0.160 Uiso 0.50 1 calc PR B 1 H66C H 0.1046 0.4016 0.4701 0.160 Uiso 0.50 1 calc PR B 1 C66' C 0.0762(13) 0.3089(13) 0.4973(11) 0.107(2) Uiso 0.50 1 d P B 2 H66D H 0.1068 0.3439 0.5092 0.160 Uiso 0.50 1 calc PR B 2 H66E H 0.1082 0.2479 0.5098 0.160 Uiso 0.50 1 calc PR B 2 H66F H 0.0170 0.3252 0.5287 0.160 Uiso 0.50 1 calc PR B 2 C67 C 0.7927(13) 0.2303(11) -0.0753(12) 0.102(2) Uiso 0.50 1 d PD C 1 H67A H 0.8548 0.2073 -0.1011 0.123 Uiso 0.50 1 calc PR C 1 H67B H 0.7861 0.2678 -0.0343 0.123 Uiso 0.50 1 calc PR C 1 C67' C 0.7721(15) 0.2453(11) -0.0671(11) 0.102(2) Uiso 0.50 1 d PD C 2 H67C H 0.8235 0.2436 -0.0472 0.123 Uiso 0.50 1 calc PR C 2 H67D H 0.7204 0.2923 -0.0430 0.123 Uiso 0.50 1 calc PR C 2 C68 C 0.7317(13) 0.2776(11) -0.1354(11) 0.102(2) Uiso 0.50 1 d PD C 1 H68A H 0.6766 0.3197 -0.1096 0.123 Uiso 0.50 1 calc PR C 1 H68B H 0.7609 0.3083 -0.1786 0.123 Uiso 0.50 1 calc PR C 1 C68' C 0.7869(13) 0.2626(12) -0.1537(10) 0.102(2) Uiso 0.50 1 d PD C 2 H68C H 0.8496 0.2519 -0.1757 0.123 Uiso 0.50 1 calc PR C 2 H68D H 0.7522 0.3226 -0.1693 0.123 Uiso 0.50 1 calc PR C 2 C69 C 0.7136(12) 0.2075(10) -0.1660(11) 0.102(2) Uiso 0.50 1 d PD C 1 H69A H 0.7371 0.2030 -0.2227 0.123 Uiso 0.50 1 calc PR C 1 H69B H 0.6502 0.2174 -0.1559 0.123 Uiso 0.50 1 calc PR C 1 C69' C 0.7564(12) 0.1998(11) -0.1793(11) 0.102(2) Uiso 0.50 1 d PD C 2 H69C H 0.8009 0.1690 -0.2226 0.123 Uiso 0.50 1 calc PR C 2 H69D H 0.7016 0.2315 -0.1995 0.123 Uiso 0.50 1 calc PR C 2 C70 C 0.7635(15) 0.1263(12) -0.1169(10) 0.102(2) Uiso 0.50 1 d PD C 1 H70A H 0.7345 0.0829 -0.1066 0.123 Uiso 0.50 1 calc PR C 1 H70B H 0.8250 0.0997 -0.1432 0.123 Uiso 0.50 1 calc PR C 1 C70' C 0.7405(15) 0.1356(13) -0.1143(10) 0.102(2) Uiso 0.50 1 d PD C 2 H70C H 0.6794 0.1372 -0.1056 0.123 Uiso 0.50 1 calc PR C 2 H70D H 0.7807 0.0766 -0.1259 0.123 Uiso 0.50 1 calc PR C 2 C71 C 0.3739(6) -0.0847(5) 0.2888(5) 0.0909(17) Uani 1 1 d . . . H71A H 0.4195 -0.1371 0.3065 0.109 Uiso 1 1 calc R . . H71B H 0.3780 -0.0848 0.2318 0.109 Uiso 1 1 calc R . . C72 C 0.2844(6) -0.0817(5) 0.3324(5) 0.0909(17) Uani 1 1 d . . . H72A H 0.2845 -0.1403 0.3518 0.109 Uiso 1 1 calc R . . H72B H 0.2406 -0.0554 0.2980 0.109 Uiso 1 1 calc R . . C73 C 0.2644(6) -0.0269(7) 0.4002(6) 0.124(4) Uani 1 1 d D . . H73A H 0.2033 0.0139 0.4069 0.149 Uiso 1 1 calc R . . H73B H 0.2732 -0.0634 0.4496 0.149 Uiso 1 1 calc R . . C74 C 0.3256(8) 0.0188(6) 0.3785(5) 0.125(4) Uani 1 1 d D . . H74A H 0.2931 0.0814 0.3725 0.150 Uiso 1 1 calc R . . H74B H 0.3596 0.0081 0.4206 0.150 Uiso 1 1 calc R . . C75 C 0.5150(7) 0.4930(5) 0.3632(6) 0.1235(18) Uani 1 1 d . . . H75A H 0.5792 0.4644 0.3493 0.148 Uiso 1 1 calc R . . H75B H 0.4942 0.4700 0.4162 0.148 Uiso 1 1 calc R . . C76 C 0.4914(8) 0.5890(5) 0.3607(6) 0.1235(18) Uani 1 1 d . . . H76A H 0.4600 0.6095 0.4128 0.148 Uiso 1 1 calc R . . H76B H 0.5452 0.6038 0.3468 0.148 Uiso 1 1 calc R . . C77 C 0.4370(8) 0.6300(6) 0.3037(6) 0.1235(18) Uani 1 1 d . . . H77A H 0.4566 0.6749 0.2703 0.148 Uiso 1 1 calc R . . H77B H 0.3752 0.6566 0.3293 0.148 Uiso 1 1 calc R . . C78 C 0.4477(8) 0.5582(5) 0.2568(6) 0.1235(18) Uani 1 1 d . . . H78A H 0.3923 0.5673 0.2399 0.148 Uiso 1 1 calc R . . H78B H 0.4938 0.5554 0.2096 0.148 Uiso 1 1 calc R . . C79 C 0.151(3) 0.633(3) 0.340(3) 0.214(4) Uiso 0.50 1 d PD D 1 C79' C 0.171(3) 0.607(3) 0.365(3) 0.214(4) Uiso 0.50 1 d PD E 2 C80 C 0.194(3) 0.561(3) 0.399(2) 0.214(4) Uiso 0.50 1 d PD D 1 C80' C 0.248(2) 0.546(2) 0.401(2) 0.214(4) Uiso 0.50 1 d PD E 2 C81 C 0.263(2) 0.488(2) 0.438(2) 0.214(4) Uiso 0.50 1 d PD D 1 C81' C 0.225(2) 0.512(2) 0.4821(17) 0.214(4) Uiso 0.50 1 d PD E 2 C82 C 0.283(3) 0.451(2) 0.516(2) 0.214(4) Uiso 0.50 1 d PD D 1 C82' C 0.229(2) 0.495(2) 0.5761(16) 0.214(4) Uiso 0.50 1 d PD E 2 C83 C 0.275(2) 0.383(2) 0.584(2) 0.214(4) Uiso 0.50 1 d PD D 1 C83' C 0.311(2) 0.408(2) 0.5755(18) 0.214(4) Uiso 0.50 1 d PD E 2 C84 C 0.194(2) 0.382(2) 0.637(2) 0.214(4) Uiso 0.50 1 d PD D 1 C84' C 0.3479(19) 0.4169(19) 0.4798(17) 0.214(4) Uiso 0.50 1 d PD E 2 C85 C 1.0054(19) 0.8931(18) 0.3623(17) 0.142(3) Uiso 0.50 1 d PD . . C86 C 0.9631(16) 0.9659(17) 0.4174(14) 0.142(3) Uiso 0.50 1 d PD . . C87 C 1.025(2) 0.962(4) 0.4697(18) 0.142(3) Uiso 0.50 1 d PD . . C88 C 0.992(3) 1.036(3) 0.5191(17) 0.142(3) Uiso 0.50 1 d PD . . C89 C 0.9962(17) 1.0253(16) 0.6059(14) 0.142(3) Uiso 0.50 1 d PD . . C90 C 0.9656(18) 1.1002(18) 0.6554(17) 0.142(3) Uiso 0.50 1 d PD . . Li1 Li 0.6978(6) 0.1433(6) 0.0562(6) 0.055(2) Uani 1 1 d . C . Li2 Li 0.4543(6) 0.0579(5) 0.2499(6) 0.051(2) Uani 1 1 d . . . Li3 Li 0.4775(7) 0.3710(6) 0.2794(6) 0.057(2) Uani 1 1 d . C . 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 Y1 0.0334(3) 0.0358(3) 0.0367(3) 0.00066(18) -0.00628(19) -0.01398(19) O1 0.0322(18) 0.0396(18) 0.050(2) -0.0011(15) -0.0073(15) -0.0173(14) O2 0.039(2) 0.068(3) 0.094(3) 0.018(2) -0.023(2) -0.0089(19) O3 0.0370(19) 0.0379(18) 0.0416(19) 0.0033(14) -0.0054(15) -0.0095(14) O4 0.085(3) 0.055(2) 0.063(3) 0.0124(19) -0.043(2) -0.023(2) O5 0.0309(18) 0.0423(18) 0.0411(19) -0.0047(14) -0.0031(15) -0.0141(14) O6 0.082(3) 0.116(4) 0.076(3) 0.000(3) -0.041(3) -0.053(3) O7 0.073(3) 0.093(3) 0.058(3) -0.011(2) 0.004(2) -0.049(3) O8 0.081(3) 0.071(3) 0.060(3) 0.005(2) -0.007(2) -0.050(2) O9 0.116(4) 0.048(2) 0.087(3) -0.012(2) -0.041(3) -0.022(2) N1 0.032(2) 0.038(2) 0.039(2) 0.0024(17) -0.0076(18) -0.0144(17) N2 0.047(2) 0.034(2) 0.037(2) 0.0027(16) -0.0132(19) -0.0158(18) N3 0.038(2) 0.043(2) 0.035(2) 0.0008(17) -0.0078(18) -0.0186(18) C1 0.035(3) 0.042(3) 0.041(3) -0.001(2) -0.006(2) -0.018(2) C2 0.037(3) 0.046(3) 0.048(3) 0.001(2) -0.010(2) -0.017(2) C3 0.039(3) 0.056(3) 0.062(4) -0.006(3) -0.016(3) -0.018(3) C4 0.042(3) 0.051(3) 0.072(4) -0.002(3) -0.016(3) -0.020(3) C5 0.047(3) 0.041(3) 0.056(3) 0.002(2) -0.013(3) -0.017(2) C6 0.043(3) 0.040(3) 0.037(3) 0.002(2) -0.008(2) -0.020(2) C7 0.042(3) 0.041(3) 0.044(3) 0.006(2) -0.010(2) -0.021(2) C8 0.040(3) 0.033(2) 0.040(3) -0.001(2) -0.007(2) -0.017(2) C9 0.041(3) 0.044(3) 0.045(3) 0.009(2) -0.009(2) -0.016(2) C10 0.054(4) 0.051(3) 0.053(3) 0.013(3) -0.022(3) -0.016(3) C11 0.038(3) 0.041(3) 0.069(4) 0.006(3) -0.017(3) -0.007(2) C12 0.038(3) 0.048(3) 0.056(3) 0.005(2) -0.006(3) -0.013(2) C13 0.042(3) 0.040(3) 0.047(3) 0.010(2) -0.012(2) -0.012(2) C14 0.041(4) 0.089(5) 0.151(8) 0.026(5) -0.019(5) -0.016(4) C15 0.037(3) 0.049(3) 0.056(3) 0.005(2) -0.009(3) -0.018(2) C16 0.046(4) 0.071(4) 0.094(5) 0.009(4) -0.024(3) -0.017(3) C17 0.057(4) 0.055(4) 0.093(5) -0.016(3) -0.020(4) -0.001(3) C18 0.054(4) 0.058(4) 0.080(4) 0.017(3) -0.021(3) -0.017(3) C19 0.061(4) 0.057(4) 0.117(6) -0.001(4) -0.036(4) -0.028(3) C23 0.032(3) 0.035(2) 0.042(3) 0.004(2) -0.006(2) -0.015(2) C24 0.048(3) 0.031(2) 0.042(3) 0.004(2) -0.015(2) -0.011(2) C25 0.044(3) 0.035(3) 0.056(3) 0.004(2) -0.020(3) -0.009(2) C26 0.042(3) 0.040(3) 0.048(3) -0.003(2) -0.009(2) -0.013(2) C27 0.047(3) 0.042(3) 0.042(3) 0.001(2) -0.008(2) -0.015(2) C28 0.041(3) 0.033(2) 0.044(3) 0.001(2) -0.013(2) -0.013(2) C29 0.044(3) 0.037(3) 0.042(3) -0.001(2) -0.009(2) -0.013(2) C30 0.032(3) 0.041(3) 0.036(3) 0.001(2) -0.007(2) -0.013(2) C31 0.059(3) 0.042(3) 0.043(3) 0.005(2) -0.017(3) -0.026(2) C32 0.067(4) 0.040(3) 0.056(3) 0.002(2) -0.026(3) -0.017(3) C33 0.050(3) 0.049(3) 0.046(3) 0.008(2) -0.016(3) -0.019(3) C34 0.067(4) 0.045(3) 0.045(3) -0.002(2) -0.023(3) -0.021(3) C35 0.053(3) 0.039(3) 0.042(3) 0.003(2) -0.021(2) -0.016(2) C36 0.092(5) 0.074(4) 0.080(5) 0.006(4) -0.055(4) -0.019(4) C37 0.059(4) 0.044(3) 0.040(3) 0.004(2) -0.011(3) -0.015(3) C38 0.101(6) 0.074(4) 0.051(4) 0.007(3) -0.032(4) -0.003(4) C39 0.108(6) 0.087(5) 0.044(4) 0.020(3) -0.012(4) -0.055(4) C40 0.089(5) 0.058(4) 0.037(3) -0.002(3) -0.007(3) -0.024(3) C41 0.043(3) 0.044(3) 0.063(4) -0.010(3) -0.013(3) -0.003(2) C42 0.060(4) 0.050(4) 0.099(5) -0.017(3) -0.011(4) -0.005(3) C43 0.061(4) 0.076(4) 0.082(5) -0.017(4) 0.006(4) -0.016(3) C44 0.045(4) 0.100(5) 0.085(5) -0.022(4) -0.019(4) 0.004(3) C45 0.035(3) 0.040(3) 0.039(3) -0.002(2) -0.006(2) -0.013(2) C46 0.040(3) 0.060(3) 0.046(3) 0.001(2) -0.009(2) -0.022(3) C47 0.034(3) 0.069(4) 0.059(4) 0.002(3) -0.010(3) -0.018(3) C48 0.039(3) 0.058(3) 0.047(3) -0.004(3) -0.003(2) -0.013(2) C49 0.045(3) 0.052(3) 0.039(3) -0.004(2) -0.002(2) -0.015(2) C50 0.035(3) 0.042(3) 0.044(3) 0.001(2) -0.002(2) -0.015(2) C51 0.038(3) 0.051(3) 0.036(3) 0.002(2) -0.004(2) -0.019(2) C52 0.042(3) 0.034(2) 0.038(3) -0.002(2) -0.011(2) -0.011(2) C53 0.047(3) 0.054(3) 0.038(3) 0.000(2) -0.009(2) -0.023(2) C54 0.069(4) 0.067(4) 0.041(3) -0.001(3) -0.023(3) -0.029(3) C55 0.048(3) 0.066(4) 0.060(4) -0.010(3) -0.020(3) -0.022(3) C56 0.053(4) 0.067(4) 0.055(4) -0.001(3) -0.009(3) -0.036(3) C57 0.051(3) 0.058(3) 0.038(3) -0.003(2) -0.009(2) -0.023(3) C58 0.071(6) 0.147(8) 0.131(8) -0.028(6) -0.045(6) -0.041(5) C59 0.042(3) 0.079(4) 0.051(3) -0.012(3) -0.015(3) -0.021(3) C60 0.059(4) 0.181(9) 0.075(5) -0.030(5) -0.020(4) -0.047(5) C61 0.095(5) 0.084(5) 0.062(4) -0.018(3) -0.022(4) -0.040(4) C62 0.075(5) 0.080(4) 0.046(3) 0.001(3) -0.015(3) -0.022(4) C63 0.042(3) 0.085(5) 0.068(4) -0.006(3) -0.003(3) -0.022(3) C71 0.108(5) 0.095(4) 0.088(4) -0.012(3) 0.001(3) -0.067(4) C72 0.108(5) 0.095(4) 0.088(4) -0.012(3) 0.001(3) -0.067(4) C73 0.097(7) 0.156(9) 0.132(8) -0.055(7) 0.035(6) -0.074(7) C74 0.215(11) 0.144(8) 0.057(5) -0.025(5) 0.032(6) -0.135(8) C75 0.168(5) 0.078(3) 0.143(5) -0.027(3) -0.053(4) -0.044(3) C76 0.168(5) 0.078(3) 0.143(5) -0.027(3) -0.053(4) -0.044(3) C77 0.168(5) 0.078(3) 0.143(5) -0.027(3) -0.053(4) -0.044(3) C78 0.168(5) 0.078(3) 0.143(5) -0.027(3) -0.053(4) -0.044(3) Li1 0.044(5) 0.057(6) 0.065(6) -0.012(5) -0.004(5) -0.021(4) Li2 0.048(5) 0.041(5) 0.064(6) 0.000(4) -0.006(5) -0.019(4) Li3 0.082(7) 0.048(5) 0.051(5) 0.003(4) -0.016(5) -0.035(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 Y1 O5 2.213(3) . ? Y1 O1 2.255(3) . ? Y1 O3 2.289(3) . ? Y1 N1 2.412(4) . ? Y1 N3 2.432(4) . ? Y1 N2 2.443(4) . ? Y1 Li2 3.047(9) . ? Y1 Li1 3.101(10) . ? Y1 Li3 3.163(9) . ? O1 C1 1.360(6) . ? O1 Li1 1.878(10) . ? O2 C11 1.391(6) . ? O2 C14 1.407(8) . ? O3 C23 1.364(5) . ? O3 Li2 1.851(10) . ? O4 C33 1.387(6) . ? O4 C36 1.416(7) . ? O5 C45 1.350(6) . ? O5 Li2 1.903(9) . ? O6 C55 1.394(6) . ? O6 C58 1.405(9) . ? O7 C67 1.416(15) . ? O7 C70 1.445(15) . ? O7 C67' 1.446(15) . ? O7 C70' 1.474(15) . ? O7 Li1 1.865(11) . ? O8 C71 1.420(8) . ? O8 C74 1.422(9) . ? O8 Li2 1.906(10) . ? O9 C75 1.428(9) . ? O9 C78 1.431(10) . ? O9 Li3 1.893(10) . ? N1 C8 1.406(6) . ? N1 C7 1.458(6) . ? N1 Li3 2.058(10) . ? N2 C30 1.401(6) . ? N2 C29 1.471(6) . ? N2 Li1 2.018(10) . ? N3 C52 1.398(6) . ? N3 C51 1.475(6) . ? N3 Li3 2.129(10) . ? C1 C6 1.397(7) . ? C1 C2 1.406(7) . ? C2 C3 1.393(7) . ? C2 C15 1.552(7) . ? C3 C4 1.388(7) . ? C3 H3 0.9400 . ? C4 C5 1.390(7) . ? C4 C19 1.533(8) . ? C5 C6 1.394(7) . ? C5 H5 0.9400 . ? C6 C7 1.520(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C13 1.388(7) . ? C8 C9 1.415(6) . ? C8 Li3 2.531(10) . ? C9 C10 1.380(7) . ? C9 H9 0.9400 . ? C10 C11 1.383(8) . ? C10 H10 0.9400 . ? C11 C12 1.372(7) . ? C12 C13 1.390(7) . ? C12 H12 0.9400 . ? C13 Li3 2.541(11) . ? C13 H13 0.9400 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 C18 1.531(8) . ? C15 C16 1.540(8) . ? C15 C17 1.540(8) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C22' 1.490(13) . ? C19 C22 1.512(14) . ? C19 C21 1.514(14) . ? C19 C21' 1.519(14) . ? C19 C20 1.523(13) . ? C19 C20' 1.559(13) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C20' H20D 0.9700 . ? C20' H20E 0.9700 . ? C20' H20F 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C21' H21D 0.9700 . ? C21' H21E 0.9700 . ? C21' H21F 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C22' H22D 0.9700 . ? C22' H22E 0.9700 . ? C22' H22F 0.9700 . ? C23 C28 1.396(7) . ? C23 C24 1.415(6) . ? C24 C25 1.396(7) . ? C24 C37 1.546(7) . ? C25 C26 1.387(7) . ? C25 H25 0.9400 . ? C26 C27 1.382(7) . ? C26 C41 1.548(7) . ? C27 C28 1.394(7) . ? C27 H27 0.9400 . ? C28 C29 1.518(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 C35 1.397(7) . ? C30 C31 1.412(7) . ? C31 C32 1.371(7) . ? C31 H31 0.9400 . ? C32 C33 1.379(7) . ? C32 H32 0.9400 . ? C33 C34 1.373(7) . ? C34 C35 1.390(6) . ? C34 H34 0.9400 . ? C35 H35 0.9400 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C37 C38 1.524(7) . ? C37 C39 1.529(9) . ? C37 C40 1.533(8) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? C41 C42 1.527(8) . ? C41 C44 1.529(8) . ? C41 C43 1.530(9) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? C45 C46 1.408(7) . ? C45 C50 1.412(7) . ? C45 Li2 2.649(10) . ? C46 C47 1.408(7) . ? C46 C59 1.528(7) . ? C47 C48 1.390(8) . ? C47 H47 0.9400 . ? C48 C49 1.380(7) . ? C48 C63 1.535(8) . ? C49 C50 1.394(7) . ? C49 H49 0.9400 . ? C50 C51 1.519(7) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 C57 1.404(7) . ? C52 C53 1.419(7) . ? C52 Li3 2.455(10) . ? C53 C54 1.373(7) . ? C53 H53 0.9400 . ? C54 C55 1.368(8) . ? C54 H54 0.9400 . ? C55 C56 1.385(8) . ? C56 C57 1.380(7) . ? C56 H56 0.9400 . ? C57 H57 0.9400 . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C58 H58C 0.9700 . ? C59 C62 1.540(9) . ? C59 C61 1.541(9) . ? C59 C60 1.552(8) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C60 H60C 0.9700 . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C61 H61C 0.9700 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C62 H62C 0.9700 . ? C63 C64 1.508(19) . ? C63 C66' 1.515(19) . ? C63 C64' 1.518(19) . ? C63 C65 1.527(18) . ? C63 C66 1.529(14) . ? C63 C65' 1.534(14) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C64 H64C 0.9700 . ? C64' H64D 0.9700 . ? C64' H64E 0.9700 . ? C64' H64F 0.9700 . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C65 H65C 0.9700 . ? C65' H65D 0.9700 . ? C65' H65E 0.9700 . ? C65' H65F 0.9700 . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C66 H66C 0.9700 . ? C66' H66D 0.9700 . ? C66' H66E 0.9700 . ? C66' H66F 0.9700 . ? C67 C68 1.540(17) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67' C68' 1.472(17) . ? C67' H67C 0.9800 . ? C67' H67D 0.9800 . ? C68 C69 1.498(16) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68' C69' 1.474(16) . ? C68' H68C 0.9800 . ? C68' H68D 0.9800 . ? C69 C70 1.542(17) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69' C70' 1.479(17) . ? C69' H69C 0.9800 . ? C69' H69D 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70' H70C 0.9800 . ? C70' H70D 0.9800 . ? C71 C72 1.491(10) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C72 C73 1.503(11) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C73 C74 1.434(10) . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C75 C76 1.488(11) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C76 C77 1.416(12) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C77 C78 1.481(11) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C79 C80 1.520(19) . ? C79' C80' 1.507(19) . ? C80 C81 1.515(19) . ? C80' C81' 1.460(19) . ? C81 C82 1.463(19) . ? C81' C82' 1.630(18) . ? C82 C83 1.521(19) . ? C82' C83' 1.578(18) . ? C83 C84 1.459(19) . ? C83' C84' 1.642(19) . ? C85 C90 0.55(4) 2_776 ? C85 C86 1.514(18) . ? C85 C89 1.53(4) 2_776 ? C86 C89 0.76(3) 2_776 ? C86 C88 1.46(4) 2_776 ? C86 C87 1.495(19) . ? C86 C90 1.73(4) 2_776 ? C87 C88 0.29(7) 2_776 ? C87 C89 1.40(4) 2_776 ? C87 C88 1.466(15) . ? C87 C87 1.62(9) 2_776 ? C88 C87 0.29(7) 2_776 ? C88 C88 1.35(9) 2_776 ? C88 C86 1.46(4) 2_776 ? C88 C89 1.509(19) . ? C89 C86 0.76(3) 2_776 ? C89 C87 1.40(4) 2_776 ? C89 C90 1.485(18) . ? C89 C85 1.53(4) 2_776 ? C90 C85 0.55(4) 2_776 ? C90 C86 1.73(4) 2_776 ? 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 O5 Y1 O1 166.79(12) . . ? O5 Y1 O3 75.68(12) . . ? O1 Y1 O3 100.57(11) . . ? O5 Y1 N1 108.00(12) . . ? O1 Y1 N1 77.76(12) . . ? O3 Y1 N1 170.50(12) . . ? O5 Y1 N3 79.28(12) . . ? O1 Y1 N3 113.60(13) . . ? O3 Y1 N3 89.80(12) . . ? N1 Y1 N3 82.44(13) . . ? O5 Y1 N2 89.33(13) . . ? O1 Y1 N2 77.49(13) . . ? O3 Y1 N2 79.02(12) . . ? N1 Y1 N2 109.47(13) . . ? N3 Y1 N2 165.75(13) . . ? O5 Y1 Li2 38.47(18) . . ? O1 Y1 Li2 135.93(18) . . ? O3 Y1 Li2 37.29(19) . . ? N1 Y1 Li2 146.11(19) . . ? N3 Y1 Li2 85.0(2) . . ? N2 Y1 Li2 80.8(2) . . ? O5 Y1 Li1 129.88(19) . . ? O1 Y1 Li1 36.96(19) . . ? O3 Y1 Li1 91.2(2) . . ? N1 Y1 Li1 92.8(2) . . ? N3 Y1 Li1 150.0(2) . . ? N2 Y1 Li1 40.6(2) . . ? Li2 Y1 Li1 112.9(2) . . ? O5 Y1 Li3 99.3(2) . . ? O1 Y1 Li3 92.7(2) . . ? O3 Y1 Li3 130.87(18) . . ? N1 Y1 Li3 40.60(19) . . ? N3 Y1 Li3 42.26(19) . . ? N2 Y1 Li3 150.05(19) . . ? Li2 Y1 Li3 123.0(3) . . ? Li1 Y1 Li3 123.9(3) . . ? C1 O1 Li1 118.6(4) . . ? C1 O1 Y1 135.0(3) . . ? Li1 O1 Y1 96.8(3) . . ? C11 O2 C14 116.1(5) . . ? C23 O3 Li2 127.9(4) . . ? C23 O3 Y1 121.8(3) . . ? Li2 O3 Y1 94.2(3) . . ? C33 O4 C36 116.9(4) . . ? C45 O5 Li2 107.8(4) . . ? C45 O5 Y1 136.2(3) . . ? Li2 O5 Y1 95.2(3) . . ? C55 O6 C58 116.1(5) . . ? C67 O7 C70 101.3(13) . . ? C67 O7 C67' 14.1(15) . . ? C70 O7 C67' 107.9(12) . . ? C67 O7 C70' 105.3(12) . . ? C70 O7 C70' 13.7(15) . . ? C67' O7 C70' 108.6(11) . . ? C67 O7 Li1 129.4(10) . . ? C70 O7 Li1 128.0(11) . . ? C67' O7 Li1 119.4(9) . . ? C70' O7 Li1 120.3(9) . . ? C71 O8 C74 107.6(5) . . ? C71 O8 Li2 132.0(5) . . ? C74 O8 Li2 120.4(5) . . ? C75 O9 C78 107.0(6) . . ? C75 O9 Li3 126.9(5) . . ? C78 O9 Li3 123.6(5) . . ? C8 N1 C7 113.3(4) . . ? C8 N1 Li3 91.9(4) . . ? C7 N1 Li3 120.9(4) . . ? C8 N1 Y1 116.2(3) . . ? C7 N1 Y1 119.7(3) . . ? Li3 N1 Y1 89.7(3) . . ? C30 N2 C29 112.9(4) . . ? C30 N2 Li1 112.3(4) . . ? C29 N2 Li1 107.5(4) . . ? C30 N2 Y1 118.2(3) . . ? C29 N2 Y1 115.3(3) . . ? Li1 N2 Y1 87.5(3) . . ? C52 N3 C51 112.8(4) . . ? C52 N3 Li3 85.5(4) . . ? C51 N3 Li3 131.9(4) . . ? C52 N3 Y1 118.4(3) . . ? C51 N3 Y1 116.7(3) . . ? Li3 N3 Y1 87.6(3) . . ? O1 C1 C6 117.9(4) . . ? O1 C1 C2 122.3(4) . . ? C6 C1 C2 119.8(5) . . ? C3 C2 C1 117.8(5) . . ? C3 C2 C15 119.1(4) . . ? C1 C2 C15 123.0(5) . . ? C4 C3 C2 123.9(5) . . ? C4 C3 H3 118.1 . . ? C2 C3 H3 118.1 . . ? C3 C4 C5 116.6(5) . . ? C3 C4 C19 121.4(5) . . ? C5 C4 C19 121.9(5) . . ? C4 C5 C6 122.0(5) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 119.8(5) . . ? C5 C6 C7 117.1(4) . . ? C1 C6 C7 122.8(4) . . ? N1 C7 C6 117.1(4) . . ? N1 C7 H7A 108.0 . . ? C6 C7 H7A 108.0 . . ? N1 C7 H7B 108.0 . . ? C6 C7 H7B 108.0 . . ? H7A C7 H7B 107.3 . . ? C13 C8 N1 119.1(4) . . ? C13 C8 C9 115.2(4) . . ? N1 C8 C9 125.7(4) . . ? C13 C8 Li3 74.5(4) . . ? N1 C8 Li3 54.4(3) . . ? C9 C8 Li3 147.5(4) . . ? C10 C9 C8 121.4(5) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 121.5(5) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C12 C11 C10 118.6(5) . . ? C12 C11 O2 124.5(5) . . ? C10 C11 O2 116.9(5) . . ? C11 C12 C13 119.8(5) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C8 C13 C12 123.5(5) . . ? C8 C13 Li3 73.7(4) . . ? C12 C13 Li3 146.7(5) . . ? C8 C13 H13 118.2 . . ? C12 C13 H13 118.2 . . ? Li3 C13 H13 54.1 . . ? O2 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C18 C15 C16 107.7(5) . . ? C18 C15 C17 108.4(5) . . ? C16 C15 C17 107.6(5) . . ? C18 C15 C2 109.6(4) . . ? C16 C15 C2 112.5(5) . . ? C17 C15 C2 110.8(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22' C19 C22 42.1(8) . . ? C22' C19 C21 125.4(11) . . ? C22 C19 C21 106.4(11) . . ? C22' C19 C21' 111.5(11) . . ? C22 C19 C21' 80.8(10) . . ? C21 C19 C21' 28.1(9) . . ? C22' C19 C20 58.9(9) . . ? C22 C19 C20 101.0(10) . . ? C21 C19 C20 117.5(10) . . ? C21' C19 C20 135.8(11) . . ? C22' C19 C4 117.1(8) . . ? C22 C19 C4 106.6(8) . . ? C21 C19 C4 114.5(9) . . ? C21' C19 C4 112.3(9) . . ? C20 C19 C4 109.3(8) . . ? C22' C19 C20' 105.4(10) . . ? C22 C19 C20' 142.6(11) . . ? C21 C19 C20' 76.0(9) . . ? C21' C19 C20' 103.4(10) . . ? C20 C19 C20' 50.3(8) . . ? C4 C19 C20' 105.8(8) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? C19 C20' H20D 109.5 . . ? C19 C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? C19 C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? C19 C21' H21D 109.5 . . ? C19 C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? C19 C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? C19 C22' H22D 109.5 . . ? C19 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C19 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? O3 C23 C28 117.7(4) . . ? O3 C23 C24 122.6(4) . . ? C28 C23 C24 119.7(4) . . ? C25 C24 C23 116.9(5) . . ? C25 C24 C37 120.7(4) . . ? C23 C24 C37 122.3(4) . . ? C26 C25 C24 124.4(4) . . ? C26 C25 H25 117.8 . . ? C24 C25 H25 117.8 . . ? C27 C26 C25 116.9(5) . . ? C27 C26 C41 120.7(5) . . ? C25 C26 C41 122.2(4) . . ? C26 C27 C28 121.6(5) . . ? C26 C27 H27 119.2 . . ? C28 C27 H27 119.2 . . ? C27 C28 C23 120.3(4) . . ? C27 C28 C29 119.8(4) . . ? C23 C28 C29 119.7(4) . . ? N2 C29 C28 114.4(4) . . ? N2 C29 H29A 108.6 . . ? C28 C29 H29A 108.6 . . ? N2 C29 H29B 108.6 . . ? C28 C29 H29B 108.6 . . ? H29A C29 H29B 107.6 . . ? C35 C30 N2 126.4(4) . . ? C35 C30 C31 114.9(4) . . ? N2 C30 C31 118.8(4) . . ? C32 C31 C30 122.7(5) . . ? C32 C31 H31 118.6 . . ? C30 C31 H31 118.6 . . ? C31 C32 C33 120.4(5) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C34 C33 C32 119.3(5) . . ? C34 C33 O4 124.3(5) . . ? C32 C33 O4 116.3(5) . . ? C33 C34 C35 120.0(5) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C30 122.7(5) . . ? C34 C35 H35 118.6 . . ? C30 C35 H35 118.6 . . ? O4 C36 H36A 109.5 . . ? O4 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O4 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C39 107.6(5) . . ? C38 C37 C40 107.2(5) . . ? C39 C37 C40 109.0(5) . . ? C38 C37 C24 112.6(5) . . ? C39 C37 C24 108.2(4) . . ? C40 C37 C24 112.1(4) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C44 109.1(5) . . ? C42 C41 C43 108.9(5) . . ? C44 C41 C43 107.7(6) . . ? C42 C41 C26 108.4(5) . . ? C44 C41 C26 112.1(5) . . ? C43 C41 C26 110.6(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O5 C45 C46 121.7(4) . . ? O5 C45 C50 118.4(4) . . ? C46 C45 C50 119.9(5) . . ? O5 C45 Li2 43.1(3) . . ? C46 C45 Li2 118.6(4) . . ? C50 C45 Li2 103.9(4) . . ? C47 C46 C45 117.6(5) . . ? C47 C46 C59 120.0(5) . . ? C45 C46 C59 122.3(5) . . ? C48 C47 C46 123.6(5) . . ? C48 C47 H47 118.2 . . ? C46 C47 H47 118.2 . . ? C49 C48 C47 116.7(5) . . ? C49 C48 C63 122.6(5) . . ? C47 C48 C63 120.7(5) . . ? C48 C49 C50 123.0(5) . . ? C48 C49 H49 118.5 . . ? C50 C49 H49 118.5 . . ? C49 C50 C45 119.1(5) . . ? C49 C50 C51 118.1(5) . . ? C45 C50 C51 122.6(4) . . ? N3 C51 C50 118.0(4) . . ? N3 C51 H51A 107.8 . . ? C50 C51 H51A 107.8 . . ? N3 C51 H51B 107.8 . . ? C50 C51 H51B 107.8 . . ? H51A C51 H51B 107.2 . . ? N3 C52 C57 118.9(4) . . ? N3 C52 C53 126.7(5) . . ? C57 C52 C53 114.4(4) . . ? N3 C52 Li3 59.9(3) . . ? C57 C52 Li3 75.7(4) . . ? C53 C52 Li3 136.2(4) . . ? C54 C53 C52 121.3(5) . . ? C54 C53 H53 119.3 . . ? C52 C53 H53 119.3 . . ? C55 C54 C53 122.5(5) . . ? C55 C54 H54 118.7 . . ? C53 C54 H54 118.7 . . ? C54 C55 C56 118.3(5) . . ? C54 C55 O6 116.6(5) . . ? C56 C55 O6 125.0(6) . . ? C57 C56 C55 119.5(5) . . ? C57 C56 H56 120.3 . . ? C55 C56 H56 120.3 . . ? C56 C57 C52 124.0(5) . . ? C56 C57 H57 118.0 . . ? C52 C57 H57 118.0 . . ? O6 C58 H58A 109.5 . . ? O6 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? O6 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C46 C59 C62 110.3(5) . . ? C46 C59 C61 111.3(5) . . ? C62 C59 C61 108.3(5) . . ? C46 C59 C60 112.4(5) . . ? C62 C59 C60 108.3(5) . . ? C61 C59 C60 106.0(6) . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C59 C62 H62A 109.5 . . ? C59 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C59 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 C66' 78.4(11) . . ? C64 C63 C64' 37.3(8) . . ? C66' C63 C64' 110.5(12) . . ? C64 C63 C65 112.2(11) . . ? C66' C63 C65 130.0(11) . . ? C64' C63 C65 77.0(11) . . ? C64 C63 C66 107.1(11) . . ? C66' C63 C66 31.2(9) . . ? C64' C63 C66 131.0(12) . . ? C65 C63 C66 106.4(11) . . ? C64 C63 C65' 136.4(11) . . ? C66' C63 C65' 108.3(11) . . ? C64' C63 C65' 106.2(11) . . ? C65 C63 C65' 31.1(9) . . ? C66 C63 C65' 79.1(11) . . ? C64 C63 C48 108.5(9) . . ? C66' C63 C48 111.9(9) . . ? C64' C63 C48 111.5(9) . . ? C65 C63 C48 110.0(9) . . ? C66 C63 C48 112.6(9) . . ? C65' C63 C48 108.1(9) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? C63 C64' H64D 109.5 . . ? C63 C64' H64E 109.5 . . ? H64D C64' H64E 109.5 . . ? C63 C64' H64F 109.5 . . ? H64D C64' H64F 109.5 . . ? H64E C64' H64F 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? C63 C65' H65D 109.5 . . ? C63 C65' H65E 109.5 . . ? H65D C65' H65E 109.5 . . ? C63 C65' H65F 109.5 . . ? H65D C65' H65F 109.5 . . ? H65E C65' H65F 109.5 . . ? C63 C66 H66A 109.5 . . ? C63 C66 H66B 109.5 . . ? C63 C66 H66C 109.5 . . ? C63 C66' H66D 109.5 . . ? C63 C66' H66E 109.5 . . ? H66D C66' H66E 109.5 . . ? C63 C66' H66F 109.5 . . ? H66D C66' H66F 109.5 . . ? H66E C66' H66F 109.5 . . ? O7 C67 C68 98.8(13) . . ? O7 C67 H67A 112.0 . . ? C68 C67 H67A 112.0 . . ? O7 C67 H67B 112.0 . . ? C68 C67 H67B 112.0 . . ? H67A C67 H67B 109.7 . . ? O7 C67' C68' 110.4(14) . . ? O7 C67' H67C 109.6 . . ? C68' C67' H67C 109.6 . . ? O7 C67' H67D 109.6 . . ? C68' C67' H67D 109.6 . . ? H67C C67' H67D 108.1 . . ? C69 C68 C67 105.4(14) . . ? C69 C68 H68A 110.7 . . ? C67 C68 H68A 110.7 . . ? C69 C68 H68B 110.7 . . ? C67 C68 H68B 110.7 . . ? H68A C68 H68B 108.8 . . ? C67' C68' C69' 102.4(15) . . ? C67' C68' H68C 111.3 . . ? C69' C68' H68C 111.3 . . ? C67' C68' H68D 111.3 . . ? C69' C68' H68D 111.3 . . ? H68C C68' H68D 109.2 . . ? C68 C69 C70 101.4(14) . . ? C68 C69 H69A 111.5 . . ? C70 C69 H69A 111.5 . . ? C68 C69 H69B 111.5 . . ? C70 C69 H69B 111.5 . . ? H69A C69 H69B 109.3 . . ? C68' C69' C70' 112.4(15) . . ? C68' C69' H69C 109.1 . . ? C70' C69' H69C 109.1 . . ? C68' C69' H69D 109.1 . . ? C70' C69' H69D 109.1 . . ? H69C C69' H69D 107.9 . . ? O7 C70 C69 101.3(13) . . ? O7 C70 H70A 111.5 . . ? C69 C70 H70A 111.5 . . ? O7 C70 H70B 111.5 . . ? C69 C70 H70B 111.5 . . ? H70A C70 H70B 109.3 . . ? O7 C70' C69' 103.9(14) . . ? O7 C70' H70C 111.0 . . ? C69' C70' H70C 111.0 . . ? O7 C70' H70D 111.0 . . ? C69' C70' H70D 111.0 . . ? H70C C70' H70D 109.0 . . ? O8 C71 C72 105.8(6) . . ? O8 C71 H71A 110.6 . . ? C72 C71 H71A 110.6 . . ? O8 C71 H71B 110.6 . . ? C72 C71 H71B 110.6 . . ? H71A C71 H71B 108.7 . . ? C71 C72 C73 105.2(6) . . ? C71 C72 H72A 110.7 . . ? C73 C72 H72A 110.7 . . ? C71 C72 H72B 110.7 . . ? C73 C72 H72B 110.7 . . ? H72A C72 H72B 108.8 . . ? C74 C73 C72 104.5(7) . . ? C74 C73 H73A 110.9 . . ? C72 C73 H73A 110.9 . . ? C74 C73 H73B 110.9 . . ? C72 C73 H73B 110.9 . . ? H73A C73 H73B 108.9 . . ? O8 C74 C73 110.9(7) . . ? O8 C74 H74A 109.5 . . ? C73 C74 H74A 109.5 . . ? O8 C74 H74B 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 108.0 . . ? O9 C75 C76 105.5(7) . . ? O9 C75 H75A 110.6 . . ? C76 C75 H75A 110.6 . . ? O9 C75 H75B 110.6 . . ? C76 C75 H75B 110.6 . . ? H75A C75 H75B 108.8 . . ? C77 C76 C75 109.5(8) . . ? C77 C76 H76A 109.8 . . ? C75 C76 H76A 109.8 . . ? C77 C76 H76B 109.8 . . ? C75 C76 H76B 109.8 . . ? H76A C76 H76B 108.2 . . ? C76 C77 C78 103.9(8) . . ? C76 C77 H77A 111.0 . . ? C78 C77 H77A 111.0 . . ? C76 C77 H77B 111.0 . . ? C78 C77 H77B 111.0 . . ? H77A C77 H77B 109.0 . . ? O9 C78 C77 107.2(8) . . ? O9 C78 H78A 110.3 . . ? C77 C78 H78A 110.3 . . ? O9 C78 H78B 110.3 . . ? C77 C78 H78B 110.3 . . ? H78A C78 H78B 108.5 . . ? C81 C80 C79 162(4) . . ? C81' C80' C79' 115(3) . . ? C82 C81 C80 141(4) . . ? C80' C81' C82' 154(4) . . ? C81 C82 C83 146(4) . . ? C83' C82' C81' 100.1(13) . . ? C84 C83 C82 126(4) . . ? C82' C83' C84' 95.1(12) . . ? C90 C85 C86 104(5) 2_776 . ? C90 C85 C89 75(4) 2_776 2_776 ? C86 C85 C89 28.8(14) . 2_776 ? C89 C86 C88 79(3) 2_776 2_776 ? C89 C86 C87 68(3) 2_776 . ? C88 C86 C87 11(3) 2_776 . ? C89 C86 C85 77(3) 2_776 . ? C88 C86 C85 118(3) 2_776 . ? C87 C86 C85 110(3) . . ? C89 C86 C90 59(3) 2_776 2_776 ? C88 C86 C90 111(2) 2_776 2_776 ? C87 C86 C90 101(2) . 2_776 ? C85 C86 C90 17.9(16) . 2_776 ? C88 C87 C89 106(10) 2_776 2_776 ? C88 C87 C88 62(10) 2_776 . ? C89 C87 C88 119(3) 2_776 . ? C88 C87 C86 78(10) 2_776 . ? C89 C87 C86 30.0(14) 2_776 . ? C88 C87 C86 113(2) . . ? C88 C87 C87 53(10) 2_776 2_776 ? C89 C87 C87 119(4) 2_776 2_776 ? C88 C87 C87 9(3) . 2_776 ? C86 C87 C87 109(4) . 2_776 ? C87 C88 C88 108(10) 2_776 2_776 ? C87 C88 C86 91(10) 2_776 2_776 ? C88 C88 C86 123(5) 2_776 2_776 ? C87 C88 C87 118(10) 2_776 . ? C88 C88 C87 11(3) 2_776 . ? C86 C88 C87 120(3) 2_776 . ? C87 C88 C89 63(9) 2_776 . ? C88 C88 C89 120(5) 2_776 . ? C86 C88 C89 29.4(14) 2_776 . ? C87 C88 C89 123(2) . . ? C86 C89 C87 82(3) 2_776 2_776 ? C86 C89 C90 95(3) 2_776 . ? C87 C89 C90 120(3) 2_776 . ? C86 C89 C88 72(3) 2_776 . ? C87 C89 C88 11(3) 2_776 . ? C90 C89 C88 123(3) . . ? C86 C89 C85 75(3) 2_776 2_776 ? C87 C89 C85 115(3) 2_776 2_776 ? C90 C89 C85 20.9(17) . 2_776 ? C88 C89 C85 114(3) . 2_776 ? C85 C90 C89 84(5) 2_776 . ? C85 C90 C86 58(4) 2_776 2_776 ? C89 C90 C86 25.8(13) . 2_776 ? O7 Li1 O1 130.1(6) . . ? O7 Li1 N2 121.2(5) . . ? O1 Li1 N2 98.1(5) . . ? O7 Li1 Y1 151.6(5) . . ? O1 Li1 Y1 46.2(2) . . ? N2 Li1 Y1 51.9(2) . . ? O3 Li2 O5 94.7(4) . . ? O3 Li2 O8 136.0(5) . . ? O5 Li2 O8 125.1(5) . . ? O3 Li2 C45 115.8(4) . . ? O5 Li2 C45 29.01(19) . . ? O8 Li2 C45 97.6(4) . . ? O3 Li2 Y1 48.5(2) . . ? O5 Li2 Y1 46.3(2) . . ? O8 Li2 Y1 164.6(5) . . ? C45 Li2 Y1 70.9(2) . . ? O9 Li3 N1 116.5(5) . . ? O9 Li3 N3 143.7(5) . . ? N1 Li3 N3 99.3(4) . . ? O9 Li3 C52 114.8(5) . . ? N1 Li3 C52 118.0(5) . . ? N3 Li3 C52 34.6(2) . . ? O9 Li3 C8 105.7(4) . . ? N1 Li3 C8 33.7(2) . . ? N3 Li3 C8 107.7(4) . . ? C52 Li3 C8 139.5(4) . . ? O9 Li3 C13 108.8(5) . . ? N1 Li3 C13 62.1(3) . . ? N3 Li3 C13 92.6(4) . . ? C52 Li3 C13 126.7(4) . . ? C8 Li3 C13 31.8(2) . . ? O9 Li3 Y1 161.8(5) . . ? N1 Li3 Y1 49.7(2) . . ? N3 Li3 Y1 50.2(2) . . ? C52 Li3 Y1 71.5(2) . . ? C8 Li3 Y1 69.4(2) . . ? C13 Li3 Y1 76.7(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 O5 Y1 O1 C1 148.6(5) . . . . ? O3 Y1 O1 C1 -139.2(4) . . . . ? N1 Y1 O1 C1 31.3(4) . . . . ? N3 Y1 O1 C1 -44.8(4) . . . . ? N2 Y1 O1 C1 144.7(4) . . . . ? Li2 Y1 O1 C1 -153.1(4) . . . . ? Li1 Y1 O1 C1 143.1(6) . . . . ? Li3 Y1 O1 C1 -6.7(4) . . . . ? O5 Y1 O1 Li1 5.5(6) . . . . ? O3 Y1 O1 Li1 77.7(3) . . . . ? N1 Y1 O1 Li1 -111.9(3) . . . . ? N3 Y1 O1 Li1 172.1(3) . . . . ? N2 Y1 O1 Li1 1.6(3) . . . . ? Li2 Y1 O1 Li1 63.8(4) . . . . ? Li3 Y1 O1 Li1 -149.8(4) . . . . ? O5 Y1 O3 C23 143.4(3) . . . . ? O1 Y1 O3 C23 -23.6(3) . . . . ? N1 Y1 O3 C23 -102.6(8) . . . . ? N3 Y1 O3 C23 -137.6(3) . . . . ? N2 Y1 O3 C23 51.2(3) . . . . ? Li2 Y1 O3 C23 140.4(5) . . . . ? Li1 Y1 O3 C23 12.3(4) . . . . ? Li3 Y1 O3 C23 -126.7(4) . . . . ? O5 Y1 O3 Li2 3.0(3) . . . . ? O1 Y1 O3 Li2 -164.0(3) . . . . ? N1 Y1 O3 Li2 117.0(8) . . . . ? N3 Y1 O3 Li2 82.0(3) . . . . ? N2 Y1 O3 Li2 -89.1(3) . . . . ? Li1 Y1 O3 Li2 -128.1(4) . . . . ? Li3 Y1 O3 Li2 92.9(4) . . . . ? O1 Y1 O5 C45 -165.3(5) . . . . ? O3 Y1 O5 C45 119.7(4) . . . . ? N1 Y1 O5 C45 -51.1(4) . . . . ? N3 Y1 O5 C45 27.2(4) . . . . ? N2 Y1 O5 C45 -161.4(4) . . . . ? Li2 Y1 O5 C45 122.6(5) . . . . ? Li1 Y1 O5 C45 -161.0(4) . . . . ? Li3 Y1 O5 C45 -10.3(4) . . . . ? O1 Y1 O5 Li2 72.1(6) . . . . ? O3 Y1 O5 Li2 -2.9(3) . . . . ? N1 Y1 O5 Li2 -173.8(3) . . . . ? N3 Y1 O5 Li2 -95.5(3) . . . . ? N2 Y1 O5 Li2 75.9(3) . . . . ? Li1 Y1 O5 Li2 76.4(4) . . . . ? Li3 Y1 O5 Li2 -132.9(3) . . . . ? O5 Y1 N1 C8 -8.8(3) . . . . ? O1 Y1 N1 C8 158.9(3) . . . . ? O3 Y1 N1 C8 -120.3(7) . . . . ? N3 Y1 N1 C8 -84.9(3) . . . . ? N2 Y1 N1 C8 87.0(3) . . . . ? Li2 Y1 N1 C8 -15.7(5) . . . . ? Li1 Y1 N1 C8 124.9(4) . . . . ? Li3 Y1 N1 C8 -92.0(4) . . . . ? O5 Y1 N1 C7 -150.8(3) . . . . ? O1 Y1 N1 C7 16.9(3) . . . . ? O3 Y1 N1 C7 97.7(8) . . . . ? N3 Y1 N1 C7 133.1(3) . . . . ? N2 Y1 N1 C7 -55.0(3) . . . . ? Li2 Y1 N1 C7 -157.7(4) . . . . ? Li1 Y1 N1 C7 -17.1(4) . . . . ? Li3 Y1 N1 C7 126.0(5) . . . . ? O5 Y1 N1 Li3 83.2(3) . . . . ? O1 Y1 N1 Li3 -109.1(3) . . . . ? O3 Y1 N1 Li3 -28.3(9) . . . . ? N3 Y1 N1 Li3 7.1(3) . . . . ? N2 Y1 N1 Li3 179.0(3) . . . . ? Li2 Y1 N1 Li3 76.2(5) . . . . ? Li1 Y1 N1 Li3 -143.1(4) . . . . ? O5 Y1 N2 C30 65.4(3) . . . . ? O1 Y1 N2 C30 -115.5(3) . . . . ? O3 Y1 N2 C30 141.0(3) . . . . ? N1 Y1 N2 C30 -43.5(4) . . . . ? N3 Y1 N2 C30 102.1(6) . . . . ? Li2 Y1 N2 C30 103.1(4) . . . . ? Li1 Y1 N2 C30 -114.0(5) . . . . ? Li3 Y1 N2 C30 -42.2(6) . . . . ? O5 Y1 N2 C29 -72.4(3) . . . . ? O1 Y1 N2 C29 106.7(3) . . . . ? O3 Y1 N2 C29 3.2(3) . . . . ? N1 Y1 N2 C29 178.7(3) . . . . ? N3 Y1 N2 C29 -35.7(7) . . . . ? Li2 Y1 N2 C29 -34.7(3) . . . . ? Li1 Y1 N2 C29 108.2(4) . . . . ? Li3 Y1 N2 C29 -180.0(4) . . . . ? O5 Y1 N2 Li1 179.4(3) . . . . ? O1 Y1 N2 Li1 -1.4(3) . . . . ? O3 Y1 N2 Li1 -105.0(3) . . . . ? N1 Y1 N2 Li1 70.6(3) . . . . ? N3 Y1 N2 Li1 -143.9(5) . . . . ? Li2 Y1 N2 Li1 -142.9(3) . . . . ? Li3 Y1 N2 Li1 71.8(5) . . . . ? O5 Y1 N3 C52 159.5(3) . . . . ? O1 Y1 N3 C52 -17.4(3) . . . . ? O3 Y1 N3 C52 84.1(3) . . . . ? N1 Y1 N3 C52 -90.4(3) . . . . ? N2 Y1 N3 C52 122.1(5) . . . . ? Li2 Y1 N3 C52 121.1(4) . . . . ? Li1 Y1 N3 C52 -7.9(6) . . . . ? Li3 Y1 N3 C52 -83.6(4) . . . . ? O5 Y1 N3 C51 19.7(3) . . . . ? O1 Y1 N3 C51 -157.2(3) . . . . ? O3 Y1 N3 C51 -55.8(3) . . . . ? N1 Y1 N3 C51 129.7(3) . . . . ? N2 Y1 N3 C51 -17.8(7) . . . . ? Li2 Y1 N3 C51 -18.8(3) . . . . ? Li1 Y1 N3 C51 -147.8(4) . . . . ? Li3 Y1 N3 C51 136.6(5) . . . . ? O5 Y1 N3 Li3 -116.9(3) . . . . ? O1 Y1 N3 Li3 66.2(3) . . . . ? O3 Y1 N3 Li3 167.7(3) . . . . ? N1 Y1 N3 Li3 -6.9(3) . . . . ? N2 Y1 N3 Li3 -154.3(5) . . . . ? Li2 Y1 N3 Li3 -155.3(4) . . . . ? Li1 Y1 N3 Li3 75.7(5) . . . . ? Li1 O1 C1 C6 96.5(6) . . . . ? Y1 O1 C1 C6 -40.8(6) . . . . ? Li1 O1 C1 C2 -82.2(6) . . . . ? Y1 O1 C1 C2 140.5(4) . . . . ? O1 C1 C2 C3 178.3(5) . . . . ? C6 C1 C2 C3 -0.4(7) . . . . ? O1 C1 C2 C15 -1.6(8) . . . . ? C6 C1 C2 C15 179.7(5) . . . . ? C1 C2 C3 C4 0.9(8) . . . . ? C15 C2 C3 C4 -179.2(5) . . . . ? C2 C3 C4 C5 -0.2(9) . . . . ? C2 C3 C4 C19 -177.1(6) . . . . ? C3 C4 C5 C6 -1.0(8) . . . . ? C19 C4 C5 C6 175.9(6) . . . . ? C4 C5 C6 C1 1.5(8) . . . . ? C4 C5 C6 C7 -172.3(5) . . . . ? O1 C1 C6 C5 -179.5(4) . . . . ? C2 C1 C6 C5 -0.7(7) . . . . ? O1 C1 C6 C7 -6.0(7) . . . . ? C2 C1 C6 C7 172.7(5) . . . . ? C8 N1 C7 C6 162.9(4) . . . . ? Li3 N1 C7 C6 55.4(6) . . . . ? Y1 N1 C7 C6 -54.1(5) . . . . ? C5 C6 C7 N1 -132.3(5) . . . . ? C1 C6 C7 N1 54.1(7) . . . . ? C7 N1 C8 C13 -164.2(4) . . . . ? Li3 N1 C8 C13 -39.2(5) . . . . ? Y1 N1 C8 C13 51.4(5) . . . . ? C7 N1 C8 C9 14.7(7) . . . . ? Li3 N1 C8 C9 139.7(5) . . . . ? Y1 N1 C8 C9 -129.7(4) . . . . ? C7 N1 C8 Li3 -125.0(5) . . . . ? Y1 N1 C8 Li3 90.6(3) . . . . ? C13 C8 C9 C10 -1.0(7) . . . . ? N1 C8 C9 C10 -180.0(5) . . . . ? Li3 C8 C9 C10 -101.9(9) . . . . ? C8 C9 C10 C11 -0.1(9) . . . . ? C9 C10 C11 C12 0.8(9) . . . . ? C9 C10 C11 O2 -180.0(5) . . . . ? C14 O2 C11 C12 -19.8(9) . . . . ? C14 O2 C11 C10 161.0(6) . . . . ? C10 C11 C12 C13 -0.3(8) . . . . ? O2 C11 C12 C13 -179.5(5) . . . . ? N1 C8 C13 C12 -179.5(5) . . . . ? C9 C8 C13 C12 1.5(8) . . . . ? Li3 C8 C13 C12 148.3(6) . . . . ? N1 C8 C13 Li3 32.2(4) . . . . ? C9 C8 C13 Li3 -146.8(5) . . . . ? C11 C12 C13 C8 -0.9(8) . . . . ? C11 C12 C13 Li3 112.4(8) . . . . ? C3 C2 C15 C18 119.4(6) . . . . ? C1 C2 C15 C18 -60.7(7) . . . . ? C3 C2 C15 C16 -0.4(7) . . . . ? C1 C2 C15 C16 179.5(5) . . . . ? C3 C2 C15 C17 -121.0(6) . . . . ? C1 C2 C15 C17 58.9(7) . . . . ? C3 C4 C19 C22' 12.4(12) . . . . ? C5 C4 C19 C22' -164.4(10) . . . . ? C3 C4 C19 C22 56.6(10) . . . . ? C5 C4 C19 C22 -120.2(9) . . . . ? C3 C4 C19 C21 173.9(9) . . . . ? C5 C4 C19 C21 -2.8(12) . . . . ? C3 C4 C19 C21' 143.3(9) . . . . ? C5 C4 C19 C21' -33.5(11) . . . . ? C3 C4 C19 C20 -51.8(11) . . . . ? C5 C4 C19 C20 131.5(9) . . . . ? C3 C4 C19 C20' -104.6(9) . . . . ? C5 C4 C19 C20' 78.7(9) . . . . ? Li2 O3 C23 C28 70.2(6) . . . . ? Y1 O3 C23 C28 -56.0(5) . . . . ? Li2 O3 C23 C24 -107.8(6) . . . . ? Y1 O3 C23 C24 125.9(4) . . . . ? O3 C23 C24 C25 -175.6(4) . . . . ? C28 C23 C24 C25 6.4(7) . . . . ? O3 C23 C24 C37 8.0(7) . . . . ? C28 C23 C24 C37 -170.0(5) . . . . ? C23 C24 C25 C26 -2.3(8) . . . . ? C37 C24 C25 C26 174.2(5) . . . . ? C24 C25 C26 C27 -2.4(8) . . . . ? C24 C25 C26 C41 -177.8(5) . . . . ? C25 C26 C27 C28 3.1(8) . . . . ? C41 C26 C27 C28 178.6(5) . . . . ? C26 C27 C28 C23 0.9(8) . . . . ? C26 C27 C28 C29 -173.5(5) . . . . ? O3 C23 C28 C27 176.1(4) . . . . ? C24 C23 C28 C27 -5.9(7) . . . . ? O3 C23 C28 C29 -9.5(7) . . . . ? C24 C23 C28 C29 168.6(4) . . . . ? C30 N2 C29 C28 167.0(4) . . . . ? Li1 N2 C29 C28 42.7(6) . . . . ? Y1 N2 C29 C28 -52.9(5) . . . . ? C27 C28 C29 N2 -115.9(5) . . . . ? C23 C28 C29 N2 69.6(6) . . . . ? C29 N2 C30 C35 1.2(7) . . . . ? Li1 N2 C30 C35 122.8(5) . . . . ? Y1 N2 C30 C35 -137.6(4) . . . . ? C29 N2 C30 C31 -178.0(4) . . . . ? Li1 N2 C30 C31 -56.4(6) . . . . ? Y1 N2 C30 C31 43.2(6) . . . . ? C35 C30 C31 C32 0.7(8) . . . . ? N2 C30 C31 C32 -180.0(5) . . . . ? C30 C31 C32 C33 -1.1(9) . . . . ? C31 C32 C33 C34 1.1(9) . . . . ? C31 C32 C33 O4 -179.9(5) . . . . ? C36 O4 C33 C34 4.9(9) . . . . ? C36 O4 C33 C32 -174.1(6) . . . . ? C32 C33 C34 C35 -0.7(9) . . . . ? O4 C33 C34 C35 -179.7(5) . . . . ? C33 C34 C35 C30 0.4(9) . . . . ? N2 C30 C35 C34 -179.6(5) . . . . ? C31 C30 C35 C34 -0.4(8) . . . . ? C25 C24 C37 C38 4.0(7) . . . . ? C23 C24 C37 C38 -179.7(5) . . . . ? C25 C24 C37 C39 -114.8(6) . . . . ? C23 C24 C37 C39 61.5(6) . . . . ? C25 C24 C37 C40 125.0(5) . . . . ? C23 C24 C37 C40 -58.7(7) . . . . ? C27 C26 C41 C42 -76.4(7) . . . . ? C25 C26 C41 C42 98.8(6) . . . . ? C27 C26 C41 C44 163.2(6) . . . . ? C25 C26 C41 C44 -21.6(8) . . . . ? C27 C26 C41 C43 42.9(7) . . . . ? C25 C26 C41 C43 -141.9(6) . . . . ? Li2 O5 C45 C46 -99.4(6) . . . . ? Y1 O5 C45 C46 142.4(4) . . . . ? Li2 O5 C45 C50 79.9(5) . . . . ? Y1 O5 C45 C50 -38.4(6) . . . . ? Y1 O5 C45 Li2 -118.2(5) . . . . ? O5 C45 C46 C47 179.6(5) . . . . ? C50 C45 C46 C47 0.3(7) . . . . ? Li2 C45 C46 C47 129.4(5) . . . . ? O5 C45 C46 C59 -2.7(8) . . . . ? C50 C45 C46 C59 178.0(5) . . . . ? Li2 C45 C46 C59 -52.9(7) . . . . ? C45 C46 C47 C48 -0.8(8) . . . . ? C59 C46 C47 C48 -178.5(5) . . . . ? C46 C47 C48 C49 1.0(9) . . . . ? C46 C47 C48 C63 -178.7(5) . . . . ? C47 C48 C49 C50 -0.8(8) . . . . ? C63 C48 C49 C50 178.9(5) . . . . ? C48 C49 C50 C45 0.4(8) . . . . ? C48 C49 C50 C51 -174.5(5) . . . . ? O5 C45 C50 C49 -179.4(4) . . . . ? C46 C45 C50 C49 -0.2(7) . . . . ? Li2 C45 C50 C49 -135.5(5) . . . . ? O5 C45 C50 C51 -4.8(7) . . . . ? C46 C45 C50 C51 174.5(5) . . . . ? Li2 C45 C50 C51 39.1(6) . . . . ? C52 N3 C51 C50 162.1(4) . . . . ? Li3 N3 C51 C50 56.8(7) . . . . ? Y1 N3 C51 C50 -55.9(5) . . . . ? C49 C50 C51 N3 -131.8(5) . . . . ? C45 C50 C51 N3 53.5(7) . . . . ? C51 N3 C52 C57 176.5(4) . . . . ? Li3 N3 C52 C57 -49.6(5) . . . . ? Y1 N3 C52 C57 35.2(5) . . . . ? C51 N3 C52 C53 -6.4(7) . . . . ? Li3 N3 C52 C53 127.5(5) . . . . ? Y1 N3 C52 C53 -147.8(4) . . . . ? C51 N3 C52 Li3 -133.9(5) . . . . ? Y1 N3 C52 Li3 84.8(4) . . . . ? N3 C52 C53 C54 -178.4(5) . . . . ? C57 C52 C53 C54 -1.3(7) . . . . ? Li3 C52 C53 C54 -95.8(7) . . . . ? C52 C53 C54 C55 0.6(9) . . . . ? C53 C54 C55 C56 -0.1(9) . . . . ? C53 C54 C55 O6 -178.8(5) . . . . ? C58 O6 C55 C54 163.4(6) . . . . ? C58 O6 C55 C56 -15.2(9) . . . . ? C54 C55 C56 C57 0.3(9) . . . . ? O6 C55 C56 C57 178.9(5) . . . . ? C55 C56 C57 C52 -1.2(9) . . . . ? N3 C52 C57 C56 179.0(5) . . . . ? C53 C52 C57 C56 1.6(7) . . . . ? Li3 C52 C57 C56 136.1(6) . . . . ? C47 C46 C59 C62 113.4(6) . . . . ? C45 C46 C59 C62 -64.3(7) . . . . ? C47 C46 C59 C61 -126.4(6) . . . . ? C45 C46 C59 C61 55.9(7) . . . . ? C47 C46 C59 C60 -7.6(8) . . . . ? C45 C46 C59 C60 174.8(6) . . . . ? C49 C48 C63 C64 -108.2(10) . . . . ? C47 C48 C63 C64 71.4(10) . . . . ? C49 C48 C63 C66' -23.6(11) . . . . ? C47 C48 C63 C66' 156.1(9) . . . . ? C49 C48 C63 C64' -147.9(9) . . . . ? C47 C48 C63 C64' 31.8(11) . . . . ? C49 C48 C63 C65 128.6(10) . . . . ? C47 C48 C63 C65 -51.7(11) . . . . ? C49 C48 C63 C66 10.2(11) . . . . ? C47 C48 C63 C66 -170.1(9) . . . . ? C49 C48 C63 C65' 95.7(10) . . . . ? C47 C48 C63 C65' -84.6(10) . . . . ? C70 O7 C67 C68 54.0(16) . . . . ? C67' O7 C67 C68 -65(5) . . . . ? C70' O7 C67 C68 40.5(16) . . . . ? Li1 O7 C67 C68 -113.9(13) . . . . ? C67 O7 C67' C68' 64(5) . . . . ? C70 O7 C67' C68' 0(2) . . . . ? C70' O7 C67' C68' -14(2) . . . . ? Li1 O7 C67' C68' -157.5(13) . . . . ? O7 C67 C68 C69 -34.1(19) . . . . ? O7 C67' C68' C69' 15(2) . . . . ? C67 C68 C69 C70 2(2) . . . . ? C67' C68' C69' C70' -11(2) . . . . ? C67 O7 C70 C69 -53.9(18) . . . . ? C67' O7 C70 C69 -41.0(18) . . . . ? C70' O7 C70 C69 54(5) . . . . ? Li1 O7 C70 C69 114.2(13) . . . . ? C68 C69 C70 O7 29.6(19) . . . . ? C67 O7 C70' C69' -7.6(18) . . . . ? C70 O7 C70' C69' -82(6) . . . . ? C67' O7 C70' C69' 7(2) . . . . ? Li1 O7 C70' C69' 149.7(12) . . . . ? C68' C69' C70' O7 3(2) . . . . ? C74 O8 C71 C72 22.5(9) . . . . ? Li2 O8 C71 C72 -153.9(6) . . . . ? O8 C71 C72 C73 -24.7(9) . . . . ? C71 C72 C73 C74 17.5(11) . . . . ? C71 O8 C74 C73 -11.7(11) . . . . ? Li2 O8 C74 C73 165.3(8) . . . . ? C72 C73 C74 O8 -4.1(12) . . . . ? C78 O9 C75 C76 16.5(11) . . . . ? Li3 O9 C75 C76 178.7(7) . . . . ? O9 C75 C76 C77 -0.5(13) . . . . ? C75 C76 C77 C78 -14.9(13) . . . . ? C75 O9 C78 C77 -26.3(11) . . . . ? Li3 O9 C78 C77 170.8(7) . . . . ? C76 C77 C78 O9 25.3(12) . . . . ? C79 C80 C81 C82 146(10) . . . . ? C79' C80' C81' C82' -123(6) . . . . ? C80 C81 C82 C83 94(8) . . . . ? C80' C81' C82' C83' -88(6) . . . . ? C81 C82 C83 C84 -68(8) . . . . ? C81' C82' C83' C84' 16(3) . . . . ? C90 C85 C86 C89 -2(8) 2_776 . . 2_776 ? C90 C85 C86 C88 -71(8) 2_776 . . 2_776 ? C89 C85 C86 C88 -69(3) 2_776 . . 2_776 ? C90 C85 C86 C87 -62(7) 2_776 . . . ? C89 C85 C86 C87 -60(3) 2_776 . . . ? C89 C85 C86 C90 2(8) 2_776 . . 2_776 ? C89 C86 C87 C88 160(22) 2_776 . . 2_776 ? C85 C86 C87 C88 -134(20) . . . 2_776 ? C90 C86 C87 C88 -150(20) 2_776 . . 2_776 ? C88 C86 C87 C89 -160(22) 2_776 . . 2_776 ? C85 C86 C87 C89 66(4) . . . 2_776 ? C90 C86 C87 C89 50(3) 2_776 . . 2_776 ? C89 C86 C87 C88 109(4) 2_776 . . . ? C88 C86 C87 C88 -52(20) 2_776 . . . ? C85 C86 C87 C88 174(2) . . . . ? C90 C86 C87 C88 158.0(18) 2_776 . . . ? C89 C86 C87 C87 117(6) 2_776 . . 2_776 ? C88 C86 C87 C87 -43(18) 2_776 . . 2_776 ? C85 C86 C87 C87 -178(4) . . . 2_776 ? C90 C86 C87 C87 166(4) 2_776 . . 2_776 ? C88 C87 C88 C87 0.00(8) 2_776 . . 2_776 ? C89 C87 C88 C87 94(15) 2_776 . . 2_776 ? C86 C87 C88 C87 61(15) . . . 2_776 ? C89 C87 C88 C88 94(15) 2_776 . . 2_776 ? C86 C87 C88 C88 61(15) . . . 2_776 ? C87 C87 C88 C88 0.00(12) 2_776 . . 2_776 ? C88 C87 C88 C86 109(16) 2_776 . . 2_776 ? C89 C87 C88 C86 -157(4) 2_776 . . 2_776 ? C86 C87 C88 C86 170(3) . . . 2_776 ? C87 C87 C88 C86 109(16) 2_776 . . 2_776 ? C88 C87 C88 C89 75(15) 2_776 . . . ? C89 C87 C88 C89 168(3) 2_776 . . . ? C86 C87 C88 C89 135(3) . . . . ? C87 C87 C88 C89 75(15) 2_776 . . . ? C87 C88 C89 C86 -159(23) 2_776 . . 2_776 ? C88 C88 C89 C86 105(6) 2_776 . . 2_776 ? C87 C88 C89 C86 93(4) . . . 2_776 ? C88 C88 C89 C87 -96(22) 2_776 . . 2_776 ? C86 C88 C89 C87 159(23) 2_776 . . 2_776 ? C87 C88 C89 C87 -108(22) . . . 2_776 ? C87 C88 C89 C90 -74(22) 2_776 . . . ? C88 C88 C89 C90 -170(4) 2_776 . . . ? C86 C88 C89 C90 85(4) 2_776 . . . ? C87 C88 C89 C90 178(2) . . . . ? C87 C88 C89 C85 -96(22) 2_776 . . 2_776 ? C88 C88 C89 C85 168(4) 2_776 . . 2_776 ? C86 C88 C89 C85 63(3) 2_776 . . 2_776 ? C87 C88 C89 C85 156(2) . . . 2_776 ? C86 C89 C90 C85 2(7) 2_776 . . 2_776 ? C87 C89 C90 C85 -82(7) 2_776 . . 2_776 ? C88 C89 C90 C85 -70(7) . . . 2_776 ? C87 C89 C90 C86 -84(4) 2_776 . . 2_776 ? C88 C89 C90 C86 -72(4) . . . 2_776 ? C85 C89 C90 C86 -2(7) 2_776 . . 2_776 ? C67 O7 Li1 O1 -6.4(14) . . . . ? C70 O7 Li1 O1 -171.3(10) . . . . ? C67' O7 Li1 O1 -18.6(13) . . . . ? C70' O7 Li1 O1 -157.5(11) . . . . ? C67 O7 Li1 N2 130.2(11) . . . . ? C70 O7 Li1 N2 -34.7(12) . . . . ? C67' O7 Li1 N2 118.0(11) . . . . ? C70' O7 Li1 N2 -20.9(12) . . . . ? C67 O7 Li1 Y1 63.5(15) . . . . ? C70 O7 Li1 Y1 -101.4(13) . . . . ? C67' O7 Li1 Y1 51.3(15) . . . . ? C70' O7 Li1 Y1 -87.6(14) . . . . ? C1 O1 Li1 O7 -9.3(9) . . . . ? Y1 O1 Li1 O7 141.8(6) . . . . ? C1 O1 Li1 N2 -153.0(4) . . . . ? Y1 O1 Li1 N2 -1.9(4) . . . . ? C1 O1 Li1 Y1 -151.1(4) . . . . ? C30 N2 Li1 O7 -26.7(7) . . . . ? C29 N2 Li1 O7 98.0(6) . . . . ? Y1 N2 Li1 O7 -146.2(5) . . . . ? C30 N2 Li1 O1 121.3(4) . . . . ? C29 N2 Li1 O1 -114.0(4) . . . . ? Y1 N2 Li1 O1 1.7(4) . . . . ? C30 N2 Li1 Y1 119.6(3) . . . . ? C29 N2 Li1 Y1 -115.7(3) . . . . ? O5 Y1 Li1 O7 85.6(10) . . . . ? O1 Y1 Li1 O7 -96.0(10) . . . . ? O3 Y1 Li1 O7 157.9(10) . . . . ? N1 Y1 Li1 O7 -30.7(10) . . . . ? N3 Y1 Li1 O7 -110.5(9) . . . . ? N2 Y1 Li1 O7 86.4(10) . . . . ? Li2 Y1 Li1 O7 126.7(9) . . . . ? Li3 Y1 Li1 O7 -58.8(11) . . . . ? O5 Y1 Li1 O1 -178.36(19) . . . . ? O3 Y1 Li1 O1 -106.1(3) . . . . ? N1 Y1 Li1 O1 65.3(3) . . . . ? N3 Y1 Li1 O1 -14.5(6) . . . . ? N2 Y1 Li1 O1 -177.6(5) . . . . ? Li2 Y1 Li1 O1 -137.3(3) . . . . ? Li3 Y1 Li1 O1 37.2(4) . . . . ? O5 Y1 Li1 N2 -0.7(4) . . . . ? O1 Y1 Li1 N2 177.6(5) . . . . ? O3 Y1 Li1 N2 71.5(3) . . . . ? N1 Y1 Li1 N2 -117.1(3) . . . . ? N3 Y1 Li1 N2 163.1(3) . . . . ? Li2 Y1 Li1 N2 40.3(4) . . . . ? Li3 Y1 Li1 N2 -145.2(3) . . . . ? C23 O3 Li2 O5 -140.0(4) . . . . ? Y1 O3 Li2 O5 -3.4(4) . . . . ? C23 O3 Li2 O8 63.8(10) . . . . ? Y1 O3 Li2 O8 -159.6(7) . . . . ? C23 O3 Li2 C45 -160.8(4) . . . . ? Y1 O3 Li2 C45 -24.2(4) . . . . ? C23 O3 Li2 Y1 -136.6(5) . . . . ? C45 O5 Li2 O3 -138.8(4) . . . . ? Y1 O5 Li2 O3 3.5(4) . . . . ? C45 O5 Li2 O8 21.2(7) . . . . ? Y1 O5 Li2 O8 163.5(6) . . . . ? Y1 O5 Li2 C45 142.2(4) . . . . ? C45 O5 Li2 Y1 -142.2(4) . . . . ? C71 O8 Li2 O3 -89.0(10) . . . . ? C74 O8 Li2 O3 95.0(10) . . . . ? C71 O8 Li2 O5 120.4(8) . . . . ? C74 O8 Li2 O5 -55.7(9) . . . . ? C71 O8 Li2 C45 130.6(6) . . . . ? C74 O8 Li2 C45 -45.5(7) . . . . ? C71 O8 Li2 Y1 171.3(15) . . . . ? C74 O8 Li2 Y1 -5(2) . . . . ? O5 C45 Li2 O3 46.9(5) . . . . ? C46 C45 Li2 O3 154.0(5) . . . . ? C50 C45 Li2 O3 -69.9(6) . . . . ? C46 C45 Li2 O5 107.1(5) . . . . ? C50 C45 Li2 O5 -116.8(5) . . . . ? O5 C45 Li2 O8 -162.6(6) . . . . ? C46 C45 Li2 O8 -55.5(6) . . . . ? C50 C45 Li2 O8 80.6(5) . . . . ? O5 C45 Li2 Y1 27.9(3) . . . . ? C46 C45 Li2 Y1 135.1(4) . . . . ? C50 C45 Li2 Y1 -88.9(3) . . . . ? O5 Y1 Li2 O3 -175.4(5) . . . . ? O1 Y1 Li2 O3 22.9(5) . . . . ? N1 Y1 Li2 O3 -164.7(2) . . . . ? N3 Y1 Li2 O3 -96.3(3) . . . . ? N2 Y1 Li2 O3 84.0(3) . . . . ? Li1 Y1 Li2 O3 58.7(4) . . . . ? Li3 Y1 Li2 O3 -115.8(3) . . . . ? O1 Y1 Li2 O5 -161.78(19) . . . . ? O3 Y1 Li2 O5 175.4(5) . . . . ? N1 Y1 Li2 O5 10.6(5) . . . . ? N3 Y1 Li2 O5 79.1(3) . . . . ? N2 Y1 Li2 O5 -100.7(3) . . . . ? Li1 Y1 Li2 O5 -125.9(3) . . . . ? Li3 Y1 Li2 O5 59.5(4) . . . . ? O5 Y1 Li2 O8 -61.5(17) . . . . ? O1 Y1 Li2 O8 136.7(16) . . . . ? O3 Y1 Li2 O8 113.9(19) . . . . ? N1 Y1 Li2 O8 -51(2) . . . . ? N3 Y1 Li2 O8 17.6(17) . . . . ? N2 Y1 Li2 O8 -162.2(18) . . . . ? Li1 Y1 Li2 O8 172.6(17) . . . . ? Li3 Y1 Li2 O8 -2.0(19) . . . . ? O5 Y1 Li2 C45 -18.31(19) . . . . ? O1 Y1 Li2 C45 179.91(16) . . . . ? O3 Y1 Li2 C45 157.0(4) . . . . ? N1 Y1 Li2 C45 -7.7(5) . . . . ? N3 Y1 Li2 C45 60.8(2) . . . . ? N2 Y1 Li2 C45 -119.0(2) . . . . ? Li1 Y1 Li2 C45 -144.2(2) . . . . ? Li3 Y1 Li2 C45 41.2(3) . . . . ? C75 O9 Li3 N1 -128.0(8) . . . . ? C78 O9 Li3 N1 31.4(10) . . . . ? C75 O9 Li3 N3 41.5(15) . . . . ? C78 O9 Li3 N3 -159.1(10) . . . . ? C75 O9 Li3 C52 15.9(10) . . . . ? C78 O9 Li3 C52 175.3(7) . . . . ? C75 O9 Li3 C8 -162.4(7) . . . . ? C78 O9 Li3 C8 -2.9(9) . . . . ? C75 O9 Li3 C13 164.5(7) . . . . ? C78 O9 Li3 C13 -36.1(9) . . . . ? C75 O9 Li3 Y1 -90.7(16) . . . . ? C78 O9 Li3 Y1 68.7(18) . . . . ? C8 N1 Li3 O9 -78.3(6) . . . . ? C7 N1 Li3 O9 40.5(8) . . . . ? Y1 N1 Li3 O9 165.6(5) . . . . ? C8 N1 Li3 N3 108.0(4) . . . . ? C7 N1 Li3 N3 -133.2(4) . . . . ? Y1 N1 Li3 N3 -8.1(4) . . . . ? C8 N1 Li3 C52 139.0(5) . . . . ? C7 N1 Li3 C52 -102.2(5) . . . . ? Y1 N1 Li3 C52 22.9(5) . . . . ? C7 N1 Li3 C8 118.8(5) . . . . ? Y1 N1 Li3 C8 -116.2(3) . . . . ? C8 N1 Li3 C13 20.0(3) . . . . ? C7 N1 Li3 C13 138.7(4) . . . . ? Y1 N1 Li3 C13 -96.18(19) . . . . ? C8 N1 Li3 Y1 116.2(3) . . . . ? C7 N1 Li3 Y1 -125.1(4) . . . . ? C52 N3 Li3 O9 -43.7(10) . . . . ? C51 N3 Li3 O9 73.2(12) . . . . ? Y1 N3 Li3 O9 -162.4(10) . . . . ? C52 N3 Li3 N1 126.8(5) . . . . ? C51 N3 Li3 N1 -116.3(5) . . . . ? Y1 N3 Li3 N1 8.1(4) . . . . ? C51 N3 Li3 C52 116.9(5) . . . . ? Y1 N3 Li3 C52 -118.7(3) . . . . ? C52 N3 Li3 C8 160.4(5) . . . . ? C51 N3 Li3 C8 -82.7(6) . . . . ? Y1 N3 Li3 C8 41.7(4) . . . . ? C52 N3 Li3 C13 -171.0(4) . . . . ? C51 N3 Li3 C13 -54.2(6) . . . . ? Y1 N3 Li3 C13 70.2(3) . . . . ? C52 N3 Li3 Y1 118.7(3) . . . . ? C51 N3 Li3 Y1 -124.4(5) . . . . ? N3 C52 Li3 O9 153.2(7) . . . . ? C57 C52 Li3 O9 -70.3(6) . . . . ? C53 C52 Li3 O9 40.1(9) . . . . ? N3 C52 Li3 N1 -63.5(5) . . . . ? C57 C52 Li3 N1 73.1(6) . . . . ? C53 C52 Li3 N1 -176.6(5) . . . . ? C57 C52 Li3 N3 136.5(5) . . . . ? C53 C52 Li3 N3 -113.1(7) . . . . ? N3 C52 Li3 C8 -29.4(7) . . . . ? C57 C52 Li3 C8 107.1(8) . . . . ? C53 C52 Li3 C8 -142.5(7) . . . . ? N3 C52 Li3 C13 11.2(5) . . . . ? C57 C52 Li3 C13 147.7(6) . . . . ? C53 C52 Li3 C13 -101.9(7) . . . . ? N3 C52 Li3 Y1 -45.3(3) . . . . ? C57 C52 Li3 Y1 91.3(3) . . . . ? C53 C52 Li3 Y1 -158.3(6) . . . . ? C13 C8 Li3 O9 -100.5(5) . . . . ? N1 C8 Li3 O9 114.5(6) . . . . ? C9 C8 Li3 O9 12.3(11) . . . . ? C13 C8 Li3 N1 145.0(5) . . . . ? C9 C8 Li3 N1 -102.2(8) . . . . ? C13 C8 Li3 N3 64.9(5) . . . . ? N1 C8 Li3 N3 -80.1(5) . . . . ? C9 C8 Li3 N3 177.7(7) . . . . ? C13 C8 Li3 C52 81.9(8) . . . . ? N1 C8 Li3 C52 -63.1(7) . . . . ? C9 C8 Li3 C52 -165.3(7) . . . . ? N1 C8 Li3 C13 -145.0(5) . . . . ? C9 C8 Li3 C13 112.8(9) . . . . ? C13 C8 Li3 Y1 98.0(3) . . . . ? N1 C8 Li3 Y1 -47.0(3) . . . . ? C9 C8 Li3 Y1 -149.2(8) . . . . ? C8 C13 Li3 O9 89.6(5) . . . . ? C12 C13 Li3 O9 -37.5(10) . . . . ? C8 C13 Li3 N1 -21.1(3) . . . . ? C12 C13 Li3 N1 -148.2(8) . . . . ? C8 C13 Li3 N3 -120.3(4) . . . . ? C12 C13 Li3 N3 112.7(8) . . . . ? C8 C13 Li3 C52 -126.6(6) . . . . ? C12 C13 Li3 C52 106.3(8) . . . . ? C12 C13 Li3 C8 -127.1(9) . . . . ? C8 C13 Li3 Y1 -72.3(3) . . . . ? C12 C13 Li3 Y1 160.6(8) . . . . ? O5 Y1 Li3 O9 -152.2(15) . . . . ? O1 Y1 Li3 O9 22.2(15) . . . . ? O3 Y1 Li3 O9 128.7(14) . . . . ? N1 Y1 Li3 O9 -45.3(14) . . . . ? N3 Y1 Li3 O9 145.1(17) . . . . ? N2 Y1 Li3 O9 -47.2(18) . . . . ? Li2 Y1 Li3 O9 174.9(14) . . . . ? Li1 Y1 Li3 O9 0.9(16) . . . . ? O5 Y1 Li3 N1 -106.9(3) . . . . ? O1 Y1 Li3 N1 67.6(3) . . . . ? O3 Y1 Li3 N1 174.06(19) . . . . ? N3 Y1 Li3 N1 -169.5(5) . . . . ? N2 Y1 Li3 N1 -1.9(6) . . . . ? Li2 Y1 Li3 N1 -139.8(3) . . . . ? Li1 Y1 Li3 N1 46.2(4) . . . . ? O5 Y1 Li3 N3 62.6(3) . . . . ? O1 Y1 Li3 N3 -122.9(3) . . . . ? O3 Y1 Li3 N3 -16.4(4) . . . . ? N1 Y1 Li3 N3 169.5(5) . . . . ? N2 Y1 Li3 N3 167.7(3) . . . . ? Li2 Y1 Li3 N3 29.7(4) . . . . ? Li1 Y1 Li3 N3 -144.3(3) . . . . ? O5 Y1 Li3 C52 94.3(3) . . . . ? O1 Y1 Li3 C52 -91.2(2) . . . . ? O3 Y1 Li3 C52 15.3(4) . . . . ? N1 Y1 Li3 C52 -158.8(5) . . . . ? N3 Y1 Li3 C52 31.7(2) . . . . ? N2 Y1 Li3 C52 -160.6(3) . . . . ? Li2 Y1 Li3 C52 61.4(4) . . . . ? Li1 Y1 Li3 C52 -112.6(3) . . . . ? O5 Y1 Li3 C8 -74.7(2) . . . . ? O1 Y1 Li3 C8 99.7(2) . . . . ? O3 Y1 Li3 C8 -153.79(18) . . . . ? N1 Y1 Li3 C8 32.2(2) . . . . ? N3 Y1 Li3 C8 -137.4(4) . . . . ? N2 Y1 Li3 C8 30.3(6) . . . . ? Li2 Y1 Li3 C8 -107.6(3) . . . . ? Li1 Y1 Li3 C8 78.4(4) . . . . ? O5 Y1 Li3 C13 -42.4(3) . . . . ? O1 Y1 Li3 C13 132.1(2) . . . . ? O3 Y1 Li3 C13 -121.4(2) . . . . ? N1 Y1 Li3 C13 64.5(3) . . . . ? N3 Y1 Li3 C13 -105.0(4) . . . . ? N2 Y1 Li3 C13 62.7(5) . . . . ? Li2 Y1 Li3 C13 -75.3(3) . . . . ? Li1 Y1 Li3 C13 110.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.718 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.071 _database_code_depnum_ccdc_archive 'CCDC 932407' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H111 Li3 N3 O9 Yb, 1.5(C6 H14)' _chemical_formula_sum 'C87 H132 Li3 N3 O9 Yb' _chemical_formula_weight 1557.82 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' 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' Yb Yb -0.3850 5.5486 '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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.5384(10) _cell_length_b 16.5622(8) _cell_length_c 17.3853(13) _cell_angle_alpha 81.372(6) _cell_angle_beta 76.812(6) _cell_angle_gamma 68.451(5) _cell_volume 4300.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 20635 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1652 _exptl_absorpt_coefficient_mu 1.141 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.525 _exptl_absorpt_correction_T_max 0.818 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35169 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_unetI/netI 0.0936 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.50 _reflns_number_total 15881 _reflns_number_gt 14088 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Their C19-C22,C19-C22', C19-C21,C19-C20,C19-C21',C19-C20',C85-C86,C86-C87,C87-C88, C88-C89,C89-C90 C79-C80,C80-C81,C81-C82,C82-C83,C83-C84,C79'-C80',C80'-C81',C81'-C82', C82'-C83',C83'-C84',O7-C67,O7-C70,O7-C67',O7-C70',C67-C68,C68-C69,C69-C70 C67'-C68',C69'-C70',C63-C66,C63-C65',C73-C74 and C68'-C69' distances were constrained. ; _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^)+(0.0505P)^2^+0.2539P] 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 15881 _refine_ls_number_parameters 880 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1389 _refine_ls_wR_factor_gt 0.1327 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.159 _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 Yb1 Yb 0.536841(14) 0.198752(12) 0.194857(12) 0.03159(9) Uani 1 1 d . C . O1 O 0.6741(2) 0.1986(2) 0.1519(2) 0.0363(8) Uani 1 1 d . C . O2 O 0.1641(3) 0.5541(3) 0.1206(3) 0.0670(13) Uani 1 1 d . . . O3 O 0.5674(2) 0.05838(19) 0.24542(19) 0.0345(8) Uani 1 1 d . C . O4 O 0.3993(3) 0.2991(2) -0.1732(2) 0.0604(12) Uani 1 1 d . C . O5 O 0.4094(2) 0.1799(2) 0.2140(2) 0.0349(8) Uani 1 1 d . C . O6 O 0.7102(4) 0.2632(3) 0.5084(3) 0.0805(15) Uani 1 1 d . C . O7 O 0.7576(3) 0.1627(3) -0.0432(3) 0.0706(13) Uani 1 1 d D . . O8 O 0.3840(3) -0.0079(3) 0.3046(3) 0.0610(12) Uani 1 1 d . C . O9 O 0.4730(3) 0.4811(3) 0.3029(3) 0.0788(15) Uani 1 1 d . . . N1 N 0.5107(3) 0.3485(2) 0.1609(2) 0.0308(9) Uani 1 1 d . C . N2 N 0.5798(3) 0.1255(2) 0.0744(2) 0.0339(10) Uani 1 1 d . . . N3 N 0.4765(3) 0.2450(2) 0.3268(2) 0.0338(9) Uani 1 1 d . . . C1 C 0.7157(3) 0.2559(3) 0.1501(3) 0.0346(11) Uani 1 1 d . . . C2 C 0.8035(4) 0.2296(3) 0.1638(3) 0.0375(12) Uani 1 1 d . C . C3 C 0.8409(4) 0.2929(3) 0.1590(3) 0.0441(13) Uani 1 1 d . . . H3 H 0.8994 0.2753 0.1671 0.053 Uiso 1 1 calc R C . C4 C 0.7968(4) 0.3809(3) 0.1429(4) 0.0453(14) Uani 1 1 d . A . C5 C 0.7103(3) 0.4057(3) 0.1316(3) 0.0394(12) Uani 1 1 d . . . H5 H 0.6780 0.4651 0.1225 0.047 Uiso 1 1 calc R C . C6 C 0.6701(3) 0.3447(3) 0.1335(3) 0.0351(11) Uani 1 1 d . C . C7 C 0.5805(3) 0.3771(3) 0.1093(3) 0.0352(12) Uani 1 1 d . . . H7A H 0.5591 0.4408 0.1054 0.042 Uiso 1 1 calc R C . H7B H 0.5888 0.3588 0.0561 0.042 Uiso 1 1 calc R . . C8 C 0.4259(3) 0.4013(3) 0.1489(3) 0.0340(11) Uani 1 1 d . . . C9 C 0.4046(4) 0.4617(3) 0.0828(3) 0.0422(13) Uani 1 1 d . C . H9 H 0.4506 0.4687 0.0423 0.051 Uiso 1 1 calc R . . C10 C 0.3182(4) 0.5101(3) 0.0770(3) 0.0460(14) Uani 1 1 d . . . H10 H 0.3067 0.5495 0.0325 0.055 Uiso 1 1 calc R C . C11 C 0.2490(4) 0.5028(3) 0.1333(4) 0.0477(14) Uani 1 1 d . C . C12 C 0.2653(4) 0.4468(3) 0.1997(3) 0.0450(13) Uani 1 1 d . . . H12 H 0.2183 0.4414 0.2399 0.054 Uiso 1 1 calc R C . C13 C 0.3520(3) 0.3988(3) 0.2062(3) 0.0361(12) Uani 1 1 d . C . H13 H 0.3620 0.3618 0.2524 0.043 Uiso 1 1 calc R . . C14 C 0.0943(4) 0.5288(5) 0.1650(6) 0.090(3) Uani 1 1 d . . . H14A H 0.1077 0.4674 0.1603 0.135 Uiso 1 1 calc R . . H14B H 0.0404 0.5624 0.1454 0.135 Uiso 1 1 calc R . . H14C H 0.0865 0.5389 0.2202 0.135 Uiso 1 1 calc R . . C15 C 0.8588(4) 0.1325(3) 0.1821(4) 0.0464(14) Uani 1 1 d . . . C16 C 0.9520(4) 0.1215(4) 0.1925(5) 0.068(2) Uani 1 1 d . C . H16A H 0.9820 0.0616 0.2100 0.102 Uiso 1 1 calc R . . H16B H 0.9478 0.1596 0.2316 0.102 Uiso 1 1 calc R . . H16C H 0.9853 0.1365 0.1423 0.102 Uiso 1 1 calc R . . C17 C 0.8697(5) 0.0776(4) 0.1140(4) 0.0671(19) Uani 1 1 d . C . H17A H 0.9171 0.0223 0.1186 0.101 Uiso 1 1 calc R . . H17B H 0.8838 0.1085 0.0637 0.101 Uiso 1 1 calc R . . H17C H 0.8149 0.0675 0.1166 0.101 Uiso 1 1 calc R . . C18 C 0.8117(4) 0.0973(4) 0.2593(4) 0.0602(17) Uani 1 1 d . C . H18A H 0.7512 0.1075 0.2551 0.090 Uiso 1 1 calc R . . H18B H 0.8117 0.1269 0.3034 0.090 Uiso 1 1 calc R . . H18C H 0.8425 0.0353 0.2679 0.090 Uiso 1 1 calc R . . C19 C 0.8450(4) 0.4472(4) 0.1349(5) 0.068(2) Uani 1 1 d D . . C20 C 0.8875(11) 0.4325(10) 0.2085(9) 0.0830(19) Uiso 0.50 1 d PD A 1 H20A H 0.9168 0.3707 0.2197 0.124 Uiso 0.50 1 calc PR A 1 H20B H 0.8419 0.4559 0.2537 0.124 Uiso 0.50 1 calc PR A 1 H20C H 0.9304 0.4618 0.1985 0.124 Uiso 0.50 1 calc PR A 1 C20' C 0.8105(11) 0.4904(10) 0.2142(8) 0.0830(19) Uiso 0.50 1 d PD A 2 H20D H 0.8219 0.4460 0.2575 0.124 Uiso 0.50 1 calc PR A 2 H20E H 0.7473 0.5218 0.2199 0.124 Uiso 0.50 1 calc PR A 2 H20F H 0.8406 0.5306 0.2151 0.124 Uiso 0.50 1 calc PR A 2 C21 C 0.7887(11) 0.5381(9) 0.1140(10) 0.0830(19) Uiso 0.50 1 d PD A 1 H21A H 0.8218 0.5768 0.1100 0.124 Uiso 0.50 1 calc PR A 1 H21B H 0.7360 0.5561 0.1548 0.124 Uiso 0.50 1 calc PR A 1 H21C H 0.7718 0.5407 0.0636 0.124 Uiso 0.50 1 calc PR A 1 C21' C 0.8132(12) 0.5236(9) 0.0736(9) 0.0830(19) Uiso 0.50 1 d PD A 2 H21D H 0.8508 0.5586 0.0645 0.124 Uiso 0.50 1 calc PR A 2 H21E H 0.7526 0.5592 0.0936 0.124 Uiso 0.50 1 calc PR A 2 H21F H 0.8162 0.5010 0.0243 0.124 Uiso 0.50 1 calc PR A 2 C22 C 0.9258(10) 0.4185(10) 0.0688(9) 0.0830(19) Uiso 0.50 1 d PD A 1 H22A H 0.9561 0.4602 0.0592 0.124 Uiso 0.50 1 calc PR A 1 H22B H 0.9069 0.4152 0.0208 0.124 Uiso 0.50 1 calc PR A 1 H22C H 0.9656 0.3617 0.0843 0.124 Uiso 0.50 1 calc PR A 1 C22' C 0.9432(9) 0.4114(10) 0.1261(11) 0.0830(19) Uiso 0.50 1 d PD A 2 H22D H 0.9685 0.3779 0.0798 0.124 Uiso 0.50 1 calc PR A 2 H22E H 0.9593 0.3740 0.1729 0.124 Uiso 0.50 1 calc PR A 2 H22F H 0.9658 0.4588 0.1199 0.124 Uiso 0.50 1 calc PR A 2 C23 C 0.6440(3) -0.0049(3) 0.2198(3) 0.0305(11) Uani 1 1 d . . . C24 C 0.7000(3) -0.0614(3) 0.2711(3) 0.0351(12) Uani 1 1 d . C . C25 C 0.7802(4) -0.1196(3) 0.2359(3) 0.0393(12) Uani 1 1 d . . . H25 H 0.8185 -0.1555 0.2695 0.047 Uiso 1 1 calc R C . C26 C 0.8084(4) -0.1291(3) 0.1550(3) 0.0406(13) Uani 1 1 d . C . C27 C 0.7484(3) -0.0778(3) 0.1070(3) 0.0366(12) Uani 1 1 d . . . H27 H 0.7629 -0.0845 0.0523 0.044 Uiso 1 1 calc R C . C28 C 0.6685(3) -0.0175(3) 0.1377(3) 0.0327(11) Uani 1 1 d . C . C29 C 0.6009(4) 0.0296(3) 0.0848(3) 0.0361(12) Uani 1 1 d . C . H29A H 0.6235 0.0060 0.0326 0.043 Uiso 1 1 calc R . . H29B H 0.5461 0.0177 0.1074 0.043 Uiso 1 1 calc R . . C30 C 0.5342(3) 0.1639(3) 0.0122(3) 0.0323(11) Uani 1 1 d . C . C31 C 0.5128(4) 0.2540(3) -0.0074(3) 0.0433(13) Uani 1 1 d . . . H31 H 0.5287 0.2865 0.0227 0.052 Uiso 1 1 calc R C . C32 C 0.4697(4) 0.2962(3) -0.0687(3) 0.0485(15) Uani 1 1 d . C . H32 H 0.4582 0.3563 -0.0806 0.058 Uiso 1 1 calc R . . C33 C 0.4432(4) 0.2508(3) -0.1132(3) 0.0428(13) Uani 1 1 d . . . C34 C 0.4627(4) 0.1631(3) -0.0968(3) 0.0445(14) Uani 1 1 d . C . H34 H 0.4457 0.1316 -0.1270 0.053 Uiso 1 1 calc R . . C35 C 0.5077(4) 0.1198(3) -0.0351(3) 0.0417(13) Uani 1 1 d . . . H35 H 0.5207 0.0595 -0.0250 0.050 Uiso 1 1 calc R C . C36 C 0.3667(5) 0.2556(4) -0.2154(4) 0.068(2) Uani 1 1 d . . . H36A H 0.4159 0.2118 -0.2450 0.103 Uiso 1 1 calc R C . H36B H 0.3323 0.2970 -0.2517 0.103 Uiso 1 1 calc R . . H36C H 0.3295 0.2278 -0.1785 0.103 Uiso 1 1 calc R . . C37 C 0.6702(4) -0.0615(3) 0.3620(3) 0.0427(13) Uani 1 1 d . . . C38 C 0.7412(5) -0.1265(4) 0.4061(4) 0.076(2) Uani 1 1 d . C . H38A H 0.7919 -0.1078 0.3968 0.115 Uiso 1 1 calc R . . H38B H 0.7593 -0.1837 0.3869 0.115 Uiso 1 1 calc R . . H38C H 0.7171 -0.1289 0.4624 0.115 Uiso 1 1 calc R . . C39 C 0.5887(5) -0.0886(4) 0.3850(4) 0.0686(19) Uani 1 1 d . C . H39A H 0.5686 -0.0883 0.4420 0.103 Uiso 1 1 calc R . . H39B H 0.6036 -0.1468 0.3689 0.103 Uiso 1 1 calc R . . H39C H 0.5420 -0.0481 0.3589 0.103 Uiso 1 1 calc R . . C40 C 0.6472(5) 0.0279(3) 0.3932(3) 0.0583(17) Uani 1 1 d . C . H40A H 0.7010 0.0408 0.3878 0.088 Uiso 1 1 calc R . . H40B H 0.6189 0.0271 0.4485 0.088 Uiso 1 1 calc R . . H40C H 0.6072 0.0723 0.3628 0.088 Uiso 1 1 calc R . . C41 C 0.8960(4) -0.1966(3) 0.1203(4) 0.0463(14) Uani 1 1 d . . . C42 C 0.8793(4) -0.2773(4) 0.1045(4) 0.0670(19) Uani 1 1 d . C . H42A H 0.8611 -0.3065 0.1545 0.101 Uiso 1 1 calc R . . H42B H 0.9332 -0.3167 0.0755 0.101 Uiso 1 1 calc R . . H42C H 0.8329 -0.2598 0.0735 0.101 Uiso 1 1 calc R . . C43 C 0.9392(4) -0.1593(4) 0.0419(4) 0.0651(18) Uani 1 1 d . C . H43A H 0.8998 -0.1429 0.0041 0.098 Uiso 1 1 calc R . . H43B H 0.9947 -0.2030 0.0207 0.098 Uiso 1 1 calc R . . H43C H 0.9503 -0.1085 0.0516 0.098 Uiso 1 1 calc R . . C44 C 0.9629(4) -0.2262(5) 0.1760(4) 0.076(2) Uani 1 1 d . C . H44A H 0.9657 -0.1756 0.1957 0.114 Uiso 1 1 calc R . . H44B H 1.0209 -0.2587 0.1474 0.114 Uiso 1 1 calc R . . H44C H 0.9446 -0.2629 0.2202 0.114 Uiso 1 1 calc R . . C45 C 0.3284(3) 0.2145(3) 0.2587(3) 0.0355(11) Uani 1 1 d . C . C46 C 0.2501(4) 0.2278(4) 0.2309(3) 0.0443(13) Uani 1 1 d . . . C47 C 0.1703(4) 0.2633(4) 0.2819(4) 0.0488(14) Uani 1 1 d . . . H47 H 0.1180 0.2728 0.2636 0.059 Uiso 1 1 calc R . . C48 C 0.1616(4) 0.2859(4) 0.3582(4) 0.0483(14) Uani 1 1 d . B . C49 C 0.2404(4) 0.2708(3) 0.3829(3) 0.0433(13) Uani 1 1 d . B . H49 H 0.2376 0.2851 0.4340 0.052 Uiso 1 1 calc R . . C50 C 0.3231(3) 0.2358(3) 0.3358(3) 0.0356(11) Uani 1 1 d . . . C51 C 0.4051(3) 0.2150(3) 0.3714(3) 0.0391(12) Uani 1 1 d . C . H51A H 0.3858 0.2396 0.4232 0.047 Uiso 1 1 calc R . . H51B H 0.4300 0.1517 0.3810 0.047 Uiso 1 1 calc R . . C52 C 0.5335(3) 0.2480(3) 0.3743(3) 0.0314(11) Uani 1 1 d . C . C53 C 0.5228(4) 0.2315(3) 0.4575(3) 0.0419(13) Uani 1 1 d . . . H53 H 0.4742 0.2160 0.4856 0.050 Uiso 1 1 calc R C . C54 C 0.5826(4) 0.2377(4) 0.4978(3) 0.0492(15) Uani 1 1 d . C . H54 H 0.5739 0.2258 0.5530 0.059 Uiso 1 1 calc R . . C55 C 0.6544(4) 0.2605(4) 0.4607(4) 0.0508(15) Uani 1 1 d . . . C56 C 0.6667(4) 0.2779(4) 0.3791(4) 0.0509(15) Uani 1 1 d . C . H56 H 0.7151 0.2941 0.3519 0.061 Uiso 1 1 calc R . . C57 C 0.6071(4) 0.2712(3) 0.3379(3) 0.0430(13) Uani 1 1 d . . . H57 H 0.6168 0.2829 0.2826 0.052 Uiso 1 1 calc R C . C58 C 0.7948(5) 0.2593(6) 0.4694(6) 0.102(3) Uani 1 1 d . . . H58A H 0.8172 0.2160 0.4306 0.153 Uiso 1 1 calc R C . H58B H 0.8337 0.2434 0.5075 0.153 Uiso 1 1 calc R . . H58C H 0.7926 0.3157 0.4428 0.153 Uiso 1 1 calc R . . C59 C 0.2511(4) 0.2076(4) 0.1474(4) 0.0491(14) Uani 1 1 d . . . C60 C 0.1575(5) 0.2202(6) 0.1345(5) 0.096(3) Uani 1 1 d . . . H60A H 0.1342 0.1803 0.1712 0.145 Uiso 1 1 calc R . . H60B H 0.1609 0.2087 0.0806 0.145 Uiso 1 1 calc R . . H60C H 0.1188 0.2796 0.1438 0.145 Uiso 1 1 calc R . . C61 C 0.3088(5) 0.1123(4) 0.1323(4) 0.071(2) Uani 1 1 d . . . H61A H 0.3706 0.1048 0.1286 0.107 Uiso 1 1 calc R . . H61B H 0.3007 0.0980 0.0832 0.107 Uiso 1 1 calc R . . H61C H 0.2916 0.0742 0.1758 0.107 Uiso 1 1 calc R . . C62 C 0.2884(5) 0.2687(4) 0.0859(4) 0.0636(18) Uani 1 1 d . . . H62A H 0.2480 0.3282 0.0907 0.095 Uiso 1 1 calc R . . H62B H 0.2951 0.2520 0.0330 0.095 Uiso 1 1 calc R . . H62C H 0.3455 0.2643 0.0952 0.095 Uiso 1 1 calc R . . C63 C 0.0709(4) 0.3239(4) 0.4111(4) 0.0618(17) Uani 1 1 d D . . C64 C 0.0278(14) 0.2543(12) 0.4323(12) 0.106(3) Uiso 0.50 1 d P B 1 H64A H 0.0404 0.2216 0.3866 0.159 Uiso 0.50 1 calc PR B 1 H64B H -0.0357 0.2819 0.4481 0.159 Uiso 0.50 1 calc PR B 1 H64C H 0.0514 0.2153 0.4757 0.159 Uiso 0.50 1 calc PR B 1 C64' C 0.0026(14) 0.2958(13) 0.3895(13) 0.106(3) Uiso 0.50 1 d P B 2 H64D H -0.0060 0.3191 0.3362 0.159 Uiso 0.50 1 calc PR B 2 H64E H -0.0529 0.3174 0.4263 0.159 Uiso 0.50 1 calc PR B 2 H64F H 0.0227 0.2327 0.3920 0.159 Uiso 0.50 1 calc PR B 2 C65 C 0.0139(14) 0.4043(12) 0.3661(12) 0.106(3) Uiso 0.50 1 d P B 1 H65A H 0.0478 0.4420 0.3438 0.159 Uiso 0.50 1 calc PR B 1 H65B H -0.0387 0.4357 0.4024 0.159 Uiso 0.50 1 calc PR B 1 H65C H -0.0032 0.3857 0.3238 0.159 Uiso 0.50 1 calc PR B 1 C65' C 0.0393(14) 0.4234(9) 0.3949(12) 0.106(3) Uiso 0.50 1 d PD B 2 H65D H 0.0831 0.4451 0.4041 0.159 Uiso 0.50 1 calc PR B 2 H65E H -0.0165 0.4494 0.4301 0.159 Uiso 0.50 1 calc PR B 2 H65F H 0.0314 0.4386 0.3404 0.159 Uiso 0.50 1 calc PR B 2 C66 C 0.0772(15) 0.3570(12) 0.4874(10) 0.106(3) Uiso 0.50 1 d PD B 1 H66A H 0.0934 0.3083 0.5264 0.159 Uiso 0.50 1 calc PR B 1 H66B H 0.0204 0.3990 0.5085 0.159 Uiso 0.50 1 calc PR B 1 H66C H 0.1219 0.3843 0.4751 0.159 Uiso 0.50 1 calc PR B 1 C66' C 0.0761(15) 0.3076(12) 0.4993(12) 0.106(3) Uiso 0.50 1 d P B 2 H66D H 0.0894 0.2460 0.5150 0.159 Uiso 0.50 1 calc PR B 2 H66E H 0.0198 0.3406 0.5302 0.159 Uiso 0.50 1 calc PR B 2 H66F H 0.1223 0.3258 0.5085 0.159 Uiso 0.50 1 calc PR B 2 C67 C 0.7930(15) 0.2297(13) -0.0716(14) 0.100(2) Uiso 0.50 1 d PD C 1 H67A H 0.8560 0.2066 -0.0954 0.120 Uiso 0.50 1 calc PR C 1 H67B H 0.7844 0.2676 -0.0300 0.120 Uiso 0.50 1 calc PR C 1 C67' C 0.7743(17) 0.2429(12) -0.0677(12) 0.100(2) Uiso 0.50 1 d PD C 2 H67C H 0.8265 0.2401 -0.0482 0.120 Uiso 0.50 1 calc PR C 2 H67D H 0.7238 0.2908 -0.0432 0.120 Uiso 0.50 1 calc PR C 2 C68 C 0.7351(13) 0.2766(11) -0.1342(11) 0.100(2) Uiso 0.50 1 d PD C 1 H68A H 0.6801 0.3207 -0.1106 0.120 Uiso 0.50 1 calc PR C 1 H68B H 0.7669 0.3046 -0.1779 0.120 Uiso 0.50 1 calc PR C 1 C68' C 0.7893(14) 0.2623(12) -0.1547(10) 0.100(2) Uiso 0.50 1 d PD C 2 H68C H 0.7522 0.3216 -0.1696 0.120 Uiso 0.50 1 calc PR C 2 H68D H 0.8516 0.2543 -0.1766 0.120 Uiso 0.50 1 calc PR C 2 C69 C 0.7166(13) 0.2053(10) -0.1621(12) 0.100(2) Uiso 0.50 1 d PD C 1 H69A H 0.7406 0.1994 -0.2188 0.120 Uiso 0.50 1 calc PR C 1 H69B H 0.6527 0.2169 -0.1528 0.120 Uiso 0.50 1 calc PR C 1 C69' C 0.7623(13) 0.1967(11) -0.1801(11) 0.100(2) Uiso 0.50 1 d PD C 2 H69C H 0.8098 0.1644 -0.2211 0.120 Uiso 0.50 1 calc PR C 2 H69D H 0.7096 0.2265 -0.2038 0.120 Uiso 0.50 1 calc PR C 2 C70 C 0.7631(17) 0.1216(12) -0.1128(11) 0.100(2) Uiso 0.50 1 d PD C 1 H70A H 0.7305 0.0809 -0.1013 0.120 Uiso 0.50 1 calc PR C 1 H70B H 0.8244 0.0920 -0.1382 0.120 Uiso 0.50 1 calc PR C 1 C70' C 0.7426(17) 0.1341(13) -0.1144(11) 0.100(2) Uiso 0.50 1 d PD C 2 H70C H 0.7823 0.0745 -0.1245 0.120 Uiso 0.50 1 calc PR C 2 H70D H 0.6813 0.1367 -0.1075 0.120 Uiso 0.50 1 calc PR C 2 C71 C 0.3741(6) -0.0834(5) 0.2873(5) 0.0923(19) Uani 1 1 d . . . H71A H 0.4203 -0.1354 0.3047 0.111 Uiso 1 1 calc R . . H71B H 0.3781 -0.0837 0.2303 0.111 Uiso 1 1 calc R . . C72 C 0.2850(6) -0.0818(5) 0.3312(5) 0.0923(19) Uani 1 1 d . . . H72A H 0.2855 -0.1409 0.3495 0.111 Uiso 1 1 calc R . . H72B H 0.2405 -0.0548 0.2975 0.111 Uiso 1 1 calc R . . C73 C 0.2658(6) -0.0281(6) 0.4009(6) 0.116(3) Uani 1 1 d D . . H73A H 0.2040 0.0110 0.4103 0.139 Uiso 1 1 calc R . . H73B H 0.2782 -0.0656 0.4491 0.139 Uiso 1 1 calc R . . C74 C 0.3250(8) 0.0203(6) 0.3767(5) 0.117(4) Uani 1 1 d D . . H74A H 0.2905 0.0824 0.3696 0.140 Uiso 1 1 calc R . . H74B H 0.3590 0.0126 0.4182 0.140 Uiso 1 1 calc R . . C75 C 0.5208(7) 0.4958(5) 0.3562(6) 0.1208(19) Uani 1 1 d . . . H75A H 0.5848 0.4699 0.3377 0.145 Uiso 1 1 calc R . . H75B H 0.5052 0.4704 0.4097 0.145 Uiso 1 1 calc R . . C76 C 0.4932(8) 0.5923(5) 0.3556(7) 0.1208(19) Uani 1 1 d . . . H76A H 0.4636 0.6109 0.4089 0.145 Uiso 1 1 calc R . . H76B H 0.5454 0.6100 0.3399 0.145 Uiso 1 1 calc R . . C77 C 0.4335(8) 0.6333(6) 0.3005(6) 0.1208(19) Uani 1 1 d . . . H77A H 0.4508 0.6789 0.2656 0.145 Uiso 1 1 calc R . . H77B H 0.3724 0.6586 0.3285 0.145 Uiso 1 1 calc R . . C78 C 0.4445(8) 0.5591(5) 0.2555(6) 0.1208(19) Uani 1 1 d . . . H78A H 0.3880 0.5661 0.2414 0.145 Uiso 1 1 calc R . . H78B H 0.4881 0.5576 0.2064 0.145 Uiso 1 1 calc R . . C79 C 0.144(3) 0.636(2) 0.329(2) 0.195(4) Uiso 0.50 1 d PD D 1 C79' C 0.168(3) 0.622(2) 0.365(2) 0.195(4) Uiso 0.50 1 d PD E 2 C80 C 0.188(2) 0.562(2) 0.387(2) 0.195(4) Uiso 0.50 1 d PD D 1 C80' C 0.231(2) 0.5604(18) 0.414(2) 0.195(4) Uiso 0.50 1 d PD E 2 C81 C 0.265(2) 0.495(2) 0.4222(19) 0.195(4) Uiso 0.50 1 d PD D 1 C81' C 0.2126(18) 0.504(2) 0.4857(19) 0.195(4) Uiso 0.50 1 d PD E 2 C82 C 0.280(2) 0.449(2) 0.5007(19) 0.195(4) Uiso 0.50 1 d PD D 1 C82' C 0.270(2) 0.463(2) 0.5497(16) 0.195(4) Uiso 0.50 1 d PD E 2 C83 C 0.298(2) 0.392(2) 0.5763(19) 0.195(4) Uiso 0.50 1 d PD D 1 C83' C 0.3643(18) 0.440(2) 0.5111(18) 0.195(4) Uiso 0.50 1 d PD E 2 C84 C 0.215(2) 0.391(2) 0.6277(19) 0.195(4) Uiso 0.50 1 d PD D 1 C84' C 0.365(2) 0.4250(17) 0.4244(18) 0.195(4) Uiso 0.50 1 d PD E 2 C85 C 1.0062(18) -0.1066(18) 0.3618(17) 0.128(3) Uiso 0.50 1 d PD . . C86 C 0.9621(16) -0.0330(15) 0.4163(14) 0.128(3) Uiso 0.50 1 d PD . . C87 C 1.013(3) -0.028(2) 0.475(2) 0.128(3) Uiso 0.50 1 d PD . . C88 C 0.975(3) 0.047(2) 0.5266(18) 0.128(3) Uiso 0.50 1 d PD . . C89 C 0.9933(16) 0.0271(15) 0.6083(14) 0.128(3) Uiso 0.50 1 d PD . . C90 C 0.9634(18) 0.1053(18) 0.6539(17) 0.128(3) Uiso 0.50 1 d PD . . Li1 Li 0.6949(7) 0.1445(6) 0.0591(6) 0.051(2) Uani 1 1 d . C . Li2 Li 0.4541(7) 0.0594(6) 0.2493(6) 0.051(2) Uani 1 1 d . . . Li3 Li 0.4756(7) 0.3715(6) 0.2802(6) 0.049(2) Uani 1 1 d . C . 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 Yb1 0.02923(14) 0.03162(13) 0.03416(14) -0.00051(9) -0.00537(10) -0.01189(10) O1 0.0287(19) 0.0347(18) 0.048(2) -0.0014(15) -0.0076(16) -0.0139(15) O2 0.035(2) 0.063(3) 0.092(4) 0.020(2) -0.023(2) -0.008(2) O3 0.0309(19) 0.0323(17) 0.036(2) 0.0011(14) -0.0051(16) -0.0073(15) O4 0.077(3) 0.054(2) 0.057(3) 0.0109(19) -0.040(2) -0.020(2) O5 0.0296(19) 0.0398(18) 0.038(2) -0.0055(14) -0.0039(16) -0.0153(16) O6 0.074(4) 0.126(4) 0.070(3) -0.004(3) -0.035(3) -0.056(3) O7 0.073(3) 0.091(3) 0.054(3) -0.015(2) 0.007(2) -0.044(3) O8 0.078(3) 0.071(3) 0.052(3) 0.003(2) -0.008(2) -0.052(3) O9 0.097(4) 0.052(3) 0.093(4) -0.027(2) -0.039(3) -0.011(3) N1 0.022(2) 0.028(2) 0.038(2) -0.0009(16) -0.0039(18) -0.0045(17) N2 0.038(2) 0.031(2) 0.034(2) 0.0000(16) -0.013(2) -0.0097(18) N3 0.033(2) 0.035(2) 0.032(2) -0.0012(17) -0.0051(19) -0.0109(19) C1 0.034(3) 0.039(3) 0.037(3) 0.003(2) -0.005(2) -0.024(2) C2 0.037(3) 0.037(3) 0.044(3) 0.003(2) -0.011(2) -0.018(2) C3 0.029(3) 0.049(3) 0.057(4) -0.005(3) -0.012(3) -0.014(3) C4 0.041(3) 0.039(3) 0.060(4) -0.008(2) -0.011(3) -0.016(3) C5 0.034(3) 0.033(3) 0.050(3) -0.003(2) -0.007(3) -0.010(2) C6 0.036(3) 0.040(3) 0.032(3) 0.004(2) -0.005(2) -0.020(2) C7 0.035(3) 0.037(3) 0.040(3) 0.001(2) -0.012(2) -0.018(2) C8 0.030(3) 0.026(2) 0.044(3) 0.001(2) -0.007(2) -0.008(2) C9 0.042(3) 0.045(3) 0.046(3) 0.004(2) -0.015(3) -0.021(3) C10 0.045(4) 0.043(3) 0.049(4) 0.010(2) -0.018(3) -0.014(3) C11 0.039(3) 0.043(3) 0.063(4) 0.010(3) -0.020(3) -0.015(3) C12 0.036(3) 0.037(3) 0.052(4) -0.002(2) -0.002(3) -0.004(2) C13 0.027(3) 0.031(3) 0.042(3) 0.005(2) -0.004(2) -0.004(2) C14 0.027(4) 0.071(5) 0.148(8) 0.019(5) -0.021(4) 0.001(3) C15 0.034(3) 0.044(3) 0.061(4) 0.003(3) -0.012(3) -0.015(3) C16 0.039(4) 0.065(4) 0.097(6) 0.016(4) -0.025(4) -0.018(3) C17 0.063(5) 0.053(4) 0.082(5) -0.010(3) -0.018(4) -0.012(3) C18 0.048(4) 0.063(4) 0.068(4) 0.020(3) -0.018(3) -0.023(3) C19 0.055(4) 0.048(4) 0.113(6) -0.002(4) -0.030(4) -0.022(3) C23 0.021(2) 0.026(2) 0.038(3) -0.0042(19) 0.000(2) -0.0023(19) C24 0.040(3) 0.027(2) 0.039(3) 0.003(2) -0.015(2) -0.011(2) C25 0.039(3) 0.029(3) 0.045(3) 0.000(2) -0.015(3) -0.003(2) C26 0.039(3) 0.039(3) 0.045(3) -0.004(2) -0.008(3) -0.014(2) C27 0.041(3) 0.034(3) 0.036(3) -0.003(2) -0.006(2) -0.015(2) C28 0.040(3) 0.029(2) 0.031(3) -0.0001(19) -0.010(2) -0.013(2) C29 0.039(3) 0.034(3) 0.037(3) -0.002(2) -0.012(2) -0.011(2) C30 0.033(3) 0.035(3) 0.028(3) 0.0001(19) -0.005(2) -0.013(2) C31 0.053(4) 0.043(3) 0.040(3) 0.001(2) -0.016(3) -0.022(3) C32 0.065(4) 0.036(3) 0.047(3) 0.005(2) -0.021(3) -0.015(3) C33 0.047(3) 0.044(3) 0.035(3) 0.006(2) -0.013(3) -0.012(3) C34 0.053(4) 0.038(3) 0.044(3) -0.003(2) -0.021(3) -0.010(3) C35 0.055(4) 0.037(3) 0.037(3) -0.001(2) -0.017(3) -0.017(3) C36 0.069(5) 0.074(4) 0.069(5) 0.006(3) -0.041(4) -0.020(4) C37 0.053(4) 0.037(3) 0.035(3) 0.006(2) -0.011(3) -0.014(3) C38 0.098(6) 0.071(4) 0.037(4) 0.006(3) -0.029(4) 0.004(4) C39 0.086(5) 0.077(4) 0.047(4) 0.010(3) -0.004(4) -0.043(4) C40 0.089(5) 0.043(3) 0.038(3) -0.001(2) -0.009(3) -0.019(3) C41 0.034(3) 0.040(3) 0.058(4) -0.012(2) -0.006(3) -0.003(2) C42 0.058(4) 0.043(3) 0.090(5) -0.022(3) -0.007(4) -0.004(3) C43 0.045(4) 0.065(4) 0.070(5) -0.011(3) 0.008(3) -0.010(3) C44 0.038(4) 0.092(5) 0.082(5) -0.030(4) -0.017(4) 0.010(3) C45 0.031(3) 0.039(3) 0.036(3) -0.001(2) -0.002(2) -0.015(2) C46 0.033(3) 0.053(3) 0.046(3) -0.002(2) -0.005(3) -0.015(3) C47 0.033(3) 0.065(4) 0.050(4) 0.003(3) -0.011(3) -0.019(3) C48 0.034(3) 0.049(3) 0.052(4) -0.002(3) -0.002(3) -0.009(3) C49 0.037(3) 0.047(3) 0.040(3) -0.005(2) 0.001(3) -0.013(3) C50 0.029(3) 0.037(3) 0.039(3) -0.003(2) -0.004(2) -0.010(2) C51 0.038(3) 0.046(3) 0.036(3) -0.001(2) -0.006(2) -0.020(3) C52 0.036(3) 0.033(2) 0.030(3) -0.0015(19) -0.006(2) -0.018(2) C53 0.045(3) 0.049(3) 0.033(3) -0.003(2) -0.004(3) -0.019(3) C54 0.057(4) 0.059(4) 0.036(3) 0.002(3) -0.018(3) -0.021(3) C55 0.052(4) 0.052(3) 0.055(4) -0.012(3) -0.022(3) -0.015(3) C56 0.045(4) 0.059(4) 0.054(4) -0.004(3) -0.013(3) -0.023(3) C57 0.043(3) 0.051(3) 0.039(3) -0.007(2) -0.010(3) -0.018(3) C58 0.065(6) 0.145(8) 0.113(8) -0.031(6) -0.046(6) -0.031(5) C59 0.039(3) 0.067(4) 0.048(4) -0.007(3) -0.013(3) -0.022(3) C60 0.061(5) 0.176(9) 0.071(5) -0.033(5) -0.028(4) -0.044(5) C61 0.094(6) 0.078(5) 0.056(4) -0.015(3) -0.019(4) -0.040(4) C62 0.069(5) 0.071(4) 0.044(4) -0.004(3) -0.018(3) -0.013(4) C63 0.035(3) 0.078(5) 0.063(4) -0.012(3) 0.003(3) -0.014(3) C71 0.114(5) 0.093(4) 0.093(5) -0.025(3) 0.006(4) -0.070(4) C72 0.114(5) 0.093(4) 0.093(5) -0.025(3) 0.006(4) -0.070(4) C73 0.088(7) 0.133(8) 0.131(9) -0.055(7) 0.029(6) -0.057(6) C74 0.209(12) 0.132(7) 0.051(5) -0.024(5) 0.017(6) -0.124(8) C75 0.156(5) 0.076(3) 0.144(5) -0.036(3) -0.043(4) -0.036(3) C76 0.156(5) 0.076(3) 0.144(5) -0.036(3) -0.043(4) -0.036(3) C77 0.156(5) 0.076(3) 0.144(5) -0.036(3) -0.043(4) -0.036(3) C78 0.156(5) 0.076(3) 0.144(5) -0.036(3) -0.043(4) -0.036(3) Li1 0.053(6) 0.060(6) 0.046(6) -0.015(4) -0.001(5) -0.025(5) Li2 0.046(6) 0.047(5) 0.056(6) 0.001(4) 0.007(5) -0.024(5) Li3 0.059(7) 0.038(5) 0.050(6) -0.007(4) -0.012(5) -0.015(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 Yb1 O5 2.187(3) . ? Yb1 O1 2.222(3) . ? Yb1 O3 2.272(3) . ? Yb1 N1 2.361(4) . ? Yb1 N3 2.401(4) . ? Yb1 N2 2.411(4) . ? Yb1 Li2 3.029(9) . ? Yb1 Li1 3.051(10) . ? Yb1 Li3 3.142(9) . ? Yb1 C23 3.199(4) . ? O1 C1 1.355(5) . ? O1 Li1 1.866(10) . ? O2 C11 1.397(6) . ? O2 C14 1.399(8) . ? O3 C23 1.346(5) . ? O3 Li2 1.854(11) . ? O4 C33 1.388(6) . ? O4 C36 1.404(7) . ? O5 C45 1.350(6) . ? O5 Li2 1.913(10) . ? O6 C55 1.390(7) . ? O6 C58 1.392(9) . ? O7 C67 1.414(16) . ? O7 C67' 1.439(15) . ? O7 C70 1.444(15) . ? O7 C70' 1.490(15) . ? O7 Li1 1.886(11) . ? O8 C71 1.403(7) . ? O8 C74 1.423(9) . ? O8 Li2 1.904(10) . ? O9 C78 1.408(10) . ? O9 C75 1.443(9) . ? O9 Li3 1.899(10) . ? N1 C8 1.399(6) . ? N1 C7 1.470(6) . ? N1 Li3 2.075(11) . ? N2 C30 1.399(6) . ? N2 C29 1.486(6) . ? N2 Li1 1.994(11) . ? N3 C52 1.406(6) . ? N3 C51 1.463(6) . ? N3 Li3 2.127(10) . ? C1 C6 1.404(6) . ? C1 C2 1.419(7) . ? C1 Li1 2.761(10) . ? C2 C3 1.385(7) . ? C2 C15 1.556(7) . ? C3 C4 1.387(7) . ? C3 H3 0.9400 . ? C4 C5 1.388(7) . ? C4 C19 1.552(8) . ? C5 C6 1.392(7) . ? C5 H5 0.9400 . ? C6 C7 1.515(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C13 1.399(7) . ? C8 C9 1.424(7) . ? C8 Li3 2.519(11) . ? C9 C10 1.378(7) . ? C9 H9 0.9400 . ? C10 C11 1.355(8) . ? C10 H10 0.9400 . ? C11 C12 1.380(7) . ? C12 C13 1.382(7) . ? C12 H12 0.9400 . ? C13 H13 0.9400 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 C16 1.534(8) . ? C15 C18 1.539(8) . ? C15 C17 1.539(8) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C22' 1.490(13) . ? C19 C21 1.492(13) . ? C19 C22 1.526(13) . ? C19 C20' 1.540(13) . ? C19 C21' 1.541(13) . ? C19 C20 1.543(13) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C20' H20D 0.9700 . ? C20' H20E 0.9700 . ? C20' H20F 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C21' H21D 0.9700 . ? C21' H21E 0.9700 . ? C21' H21F 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C22' H22D 0.9700 . ? C22' H22E 0.9700 . ? C22' H22F 0.9700 . ? C23 C28 1.416(6) . ? C23 C24 1.421(6) . ? C24 C25 1.389(7) . ? C24 C37 1.544(7) . ? C25 C26 1.390(7) . ? C25 H25 0.9400 . ? C26 C27 1.396(7) . ? C26 C41 1.525(7) . ? C27 C28 1.377(7) . ? C27 H27 0.9400 . ? C28 C29 1.524(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 C31 1.407(6) . ? C30 C35 1.407(7) . ? C31 C32 1.375(7) . ? C31 H31 0.9400 . ? C32 C33 1.390(7) . ? C32 H32 0.9400 . ? C33 C34 1.367(7) . ? C34 C35 1.400(7) . ? C34 H34 0.9400 . ? C35 H35 0.9400 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C37 C39 1.523(9) . ? C37 C38 1.536(7) . ? C37 C40 1.539(7) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? C41 C44 1.535(8) . ? C41 C42 1.535(8) . ? C41 C43 1.542(8) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? C45 C50 1.412(7) . ? C45 C46 1.415(7) . ? C45 Li2 2.645(11) . ? C46 C47 1.389(8) . ? C46 C59 1.534(8) . ? C47 C48 1.394(8) . ? C47 H47 0.9400 . ? C48 C49 1.390(8) . ? C48 C63 1.530(8) . ? C49 C50 1.388(7) . ? C49 H49 0.9400 . ? C50 C51 1.521(7) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 C57 1.396(7) . ? C52 C53 1.414(7) . ? C52 Li3 2.459(10) . ? C53 C54 1.376(7) . ? C53 H53 0.9400 . ? C54 C55 1.369(8) . ? C54 H54 0.9400 . ? C55 C56 1.387(8) . ? C56 C57 1.387(7) . ? C56 H56 0.9400 . ? C57 H57 0.9400 . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C58 H58C 0.9700 . ? C59 C61 1.541(8) . ? C59 C62 1.543(9) . ? C59 C60 1.547(8) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C60 H60C 0.9700 . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C61 H61C 0.9700 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C62 H62C 0.9700 . ? C63 C64' 1.506(19) . ? C63 C64 1.526(19) . ? C63 C66' 1.53(2) . ? C63 C65' 1.538(14) . ? C63 C65 1.541(19) . ? C63 C66 1.546(14) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C64 H64C 0.9700 . ? C64' H64D 0.9700 . ? C64' H64E 0.9700 . ? C64' H64F 0.9700 . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C65 H65C 0.9700 . ? C65' H65D 0.9700 . ? C65' H65E 0.9700 . ? C65' H65F 0.9700 . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C66 H66C 0.9700 . ? C66' H66D 0.9700 . ? C66' H66E 0.9700 . ? C66' H66F 0.9700 . ? C67 C68 1.543(17) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67' C68' 1.481(17) . ? C67' H67C 0.9800 . ? C67' H67D 0.9800 . ? C68 C69 1.493(16) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68' C69' 1.471(15) . ? C68' H68C 0.9800 . ? C68' H68D 0.9800 . ? C69 C70 1.552(17) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69' C70' 1.487(17) . ? C69' H69C 0.9800 . ? C69' H69D 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70' H70C 0.9800 . ? C70' H70D 0.9800 . ? C71 C72 1.490(11) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C72 C73 1.517(11) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C73 C74 1.436(10) . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C75 C76 1.492(10) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C76 C77 1.447(12) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C77 C78 1.490(10) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C79 C80 1.541(19) . ? C79' C80' 1.488(18) . ? C80 C81 1.529(19) . ? C80' C81' 1.482(19) . ? C81 C82 1.485(19) . ? C81' C82' 1.543(19) . ? C82 C83 1.516(19) . ? C82' C83' 1.482(19) . ? C83 C84 1.460(19) . ? C83' C84' 1.562(19) . ? C85 C90 0.52(4) 2_756 ? C85 C89 1.49(4) 2_756 ? C85 C86 1.514(17) . ? C86 C89 0.80(3) 2_756 ? C86 C87 1.500(18) . ? C86 C88 1.54(4) 2_756 ? C86 C90 1.76(4) 2_756 ? C87 C88 0.31(7) 2_756 ? C87 C87 1.24(6) 2_756 ? C87 C89 1.48(4) 2_756 ? C87 C88 1.491(15) . ? C88 C87 0.31(7) 2_756 ? C88 C89 1.485(18) . ? C88 C86 1.54(4) 2_756 ? C88 C88 1.76(7) 2_756 ? C89 C86 0.80(3) 2_756 ? C89 C87 1.48(4) 2_756 ? C89 C90 1.488(17) . ? C89 C85 1.49(4) 2_756 ? C90 C85 0.52(4) 2_756 ? C90 C86 1.76(4) 2_756 ? 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 O5 Yb1 O1 166.55(12) . . ? O5 Yb1 O3 76.56(12) . . ? O1 Yb1 O3 99.29(12) . . ? O5 Yb1 N1 107.24(13) . . ? O1 Yb1 N1 78.84(12) . . ? O3 Yb1 N1 170.84(12) . . ? O5 Yb1 N3 80.12(13) . . ? O1 Yb1 N3 112.83(13) . . ? O3 Yb1 N3 89.04(12) . . ? N1 Yb1 N3 83.52(13) . . ? O5 Yb1 N2 88.46(13) . . ? O1 Yb1 N2 78.18(13) . . ? O3 Yb1 N2 79.70(12) . . ? N1 Yb1 N2 108.46(13) . . ? N3 Yb1 N2 165.58(14) . . ? O5 Yb1 Li2 39.0(2) . . ? O1 Yb1 Li2 134.9(2) . . ? O3 Yb1 Li2 37.6(2) . . ? N1 Yb1 Li2 146.0(2) . . ? N3 Yb1 Li2 85.2(2) . . ? N2 Yb1 Li2 80.4(2) . . ? O5 Yb1 Li1 129.2(2) . . ? O1 Yb1 Li1 37.5(2) . . ? O3 Yb1 Li1 90.9(2) . . ? N1 Yb1 Li1 92.9(2) . . ? N3 Yb1 Li1 149.7(2) . . ? N2 Yb1 Li1 40.7(2) . . ? Li2 Yb1 Li1 112.3(3) . . ? O5 Yb1 Li3 99.1(2) . . ? O1 Yb1 Li3 93.3(2) . . ? O3 Yb1 Li3 130.51(19) . . ? N1 Yb1 Li3 41.3(2) . . ? N3 Yb1 Li3 42.6(2) . . ? N2 Yb1 Li3 149.8(2) . . ? Li2 Yb1 Li3 123.0(3) . . ? Li1 Yb1 Li3 124.5(3) . . ? O5 Yb1 C23 93.21(12) . . ? O1 Yb1 C23 80.33(12) . . ? O3 Yb1 C23 20.85(12) . . ? N1 Yb1 C23 159.17(13) . . ? N3 Yb1 C23 104.37(13) . . ? N2 Yb1 C23 67.26(12) . . ? Li2 Yb1 C23 54.8(2) . . ? Li1 Yb1 C23 70.5(2) . . ? Li3 Yb1 C23 140.49(19) . . ? C1 O1 Li1 117.1(4) . . ? C1 O1 Yb1 135.2(3) . . ? Li1 O1 Yb1 96.2(3) . . ? C11 O2 C14 116.5(5) . . ? C23 O3 Li2 126.8(4) . . ? C23 O3 Yb1 122.2(3) . . ? Li2 O3 Yb1 93.9(3) . . ? C33 O4 C36 117.1(4) . . ? C45 O5 Li2 107.1(4) . . ? C45 O5 Yb1 136.1(3) . . ? Li2 O5 Yb1 95.0(3) . . ? C55 O6 C58 115.6(6) . . ? C67 O7 C67' 12.2(18) . . ? C67 O7 C70 105.2(15) . . ? C67' O7 C70 108.8(13) . . ? C67 O7 C70' 105.7(13) . . ? C67' O7 C70' 106.5(12) . . ? C70 O7 C70' 12.8(16) . . ? C67 O7 Li1 127.8(11) . . ? C67' O7 Li1 121.0(10) . . ? C70 O7 Li1 125.8(12) . . ? C70' O7 Li1 121.6(10) . . ? C71 O8 C74 107.9(5) . . ? C71 O8 Li2 132.6(5) . . ? C74 O8 Li2 119.4(5) . . ? C78 O9 C75 106.9(6) . . ? C78 O9 Li3 124.7(5) . . ? C75 O9 Li3 126.4(5) . . ? C8 N1 C7 112.6(4) . . ? C8 N1 Li3 90.8(4) . . ? C7 N1 Li3 120.1(4) . . ? C8 N1 Yb1 117.7(3) . . ? C7 N1 Yb1 120.0(3) . . ? Li3 N1 Yb1 90.0(3) . . ? C30 N2 C29 112.3(4) . . ? C30 N2 Li1 113.0(4) . . ? C29 N2 Li1 106.2(4) . . ? C30 N2 Yb1 119.1(3) . . ? C29 N2 Yb1 115.8(3) . . ? Li1 N2 Yb1 87.1(3) . . ? C52 N3 C51 113.0(4) . . ? C52 N3 Li3 85.7(4) . . ? C51 N3 Li3 130.9(4) . . ? C52 N3 Yb1 119.4(3) . . ? C51 N3 Yb1 116.2(3) . . ? Li3 N3 Yb1 87.7(3) . . ? O1 C1 C6 118.4(4) . . ? O1 C1 C2 122.6(4) . . ? C6 C1 C2 119.0(4) . . ? O1 C1 Li1 37.0(3) . . ? C6 C1 Li1 115.1(4) . . ? C2 C1 Li1 112.6(4) . . ? C3 C2 C1 118.2(5) . . ? C3 C2 C15 119.5(5) . . ? C1 C2 C15 122.3(4) . . ? C2 C3 C4 123.6(5) . . ? C2 C3 H3 118.2 . . ? C4 C3 H3 118.2 . . ? C3 C4 C5 117.4(5) . . ? C3 C4 C19 120.3(5) . . ? C5 C4 C19 122.3(5) . . ? C4 C5 C6 121.5(5) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 120.2(5) . . ? C5 C6 C7 117.3(4) . . ? C1 C6 C7 122.2(4) . . ? N1 C7 C6 117.1(4) . . ? N1 C7 H7A 108.0 . . ? C6 C7 H7A 108.0 . . ? N1 C7 H7B 108.0 . . ? C6 C7 H7B 108.0 . . ? H7A C7 H7B 107.3 . . ? N1 C8 C13 119.7(4) . . ? N1 C8 C9 126.4(5) . . ? C13 C8 C9 113.8(5) . . ? N1 C8 Li3 55.5(3) . . ? C13 C8 Li3 74.2(4) . . ? C9 C8 Li3 147.1(4) . . ? C10 C9 C8 121.4(5) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C11 C10 C9 122.1(5) . . ? C11 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C10 C11 C12 119.3(5) . . ? C10 C11 O2 117.2(5) . . ? C12 C11 O2 123.5(6) . . ? C11 C12 C13 118.8(5) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C12 C13 C8 124.5(5) . . ? C12 C13 H13 117.7 . . ? C8 C13 H13 117.7 . . ? O2 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C18 108.4(5) . . ? C16 C15 C17 107.2(5) . . ? C18 C15 C17 109.5(5) . . ? C16 C15 C2 111.8(5) . . ? C18 C15 C2 109.2(5) . . ? C17 C15 C2 110.6(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22' C19 C21 127.5(10) . . ? C22' C19 C22 41.9(8) . . ? C21 C19 C22 109.0(10) . . ? C22' C19 C20' 105.7(10) . . ? C21 C19 C20' 75.6(9) . . ? C22 C19 C20' 143.5(10) . . ? C22' C19 C21' 112.6(11) . . ? C21 C19 C21' 28.6(8) . . ? C22 C19 C21' 82.6(10) . . ? C20' C19 C21' 103.3(9) . . ? C22' C19 C20 60.5(9) . . ? C21 C19 C20 116.9(10) . . ? C22 C19 C20 102.4(10) . . ? C20' C19 C20 48.8(8) . . ? C21' C19 C20 136.0(10) . . ? C22' C19 C4 117.1(7) . . ? C21 C19 C4 112.8(8) . . ? C22 C19 C4 106.4(8) . . ? C20' C19 C4 104.5(8) . . ? C21' C19 C4 112.0(8) . . ? C20 C19 C4 108.4(8) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? C19 C20' H20D 109.5 . . ? C19 C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? C19 C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? C19 C21' H21D 109.5 . . ? C19 C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? C19 C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? C19 C22' H22D 109.5 . . ? C19 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C19 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? O3 C23 C28 118.2(4) . . ? O3 C23 C24 123.3(4) . . ? C28 C23 C24 118.5(4) . . ? O3 C23 Yb1 36.9(2) . . ? C28 C23 Yb1 94.3(3) . . ? C24 C23 Yb1 137.8(3) . . ? C25 C24 C23 117.0(5) . . ? C25 C24 C37 121.7(4) . . ? C23 C24 C37 121.2(4) . . ? C24 C25 C26 125.3(4) . . ? C24 C25 H25 117.3 . . ? C26 C25 H25 117.3 . . ? C25 C26 C27 116.0(5) . . ? C25 C26 C41 122.7(5) . . ? C27 C26 C41 121.1(5) . . ? C28 C27 C26 121.7(5) . . ? C28 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C27 C28 C23 121.1(4) . . ? C27 C28 C29 119.8(4) . . ? C23 C28 C29 118.9(4) . . ? N2 C29 C28 114.0(4) . . ? N2 C29 H29A 108.7 . . ? C28 C29 H29A 108.7 . . ? N2 C29 H29B 108.7 . . ? C28 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? N2 C30 C31 119.2(4) . . ? N2 C30 C35 125.6(4) . . ? C31 C30 C35 115.3(4) . . ? C32 C31 C30 122.7(5) . . ? C32 C31 H31 118.7 . . ? C30 C31 H31 118.7 . . ? C31 C32 C33 120.4(5) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C34 C33 O4 124.5(5) . . ? C34 C33 C32 119.2(5) . . ? O4 C33 C32 116.2(5) . . ? C33 C34 C35 120.4(5) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C34 C35 C30 122.1(5) . . ? C34 C35 H35 119.0 . . ? C30 C35 H35 119.0 . . ? O4 C36 H36A 109.5 . . ? O4 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O4 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 C38 107.4(5) . . ? C39 C37 C40 108.8(5) . . ? C38 C37 C40 106.5(5) . . ? C39 C37 C24 108.4(5) . . ? C38 C37 C24 112.6(5) . . ? C40 C37 C24 113.0(4) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C26 C41 C44 112.6(5) . . ? C26 C41 C42 109.4(5) . . ? C44 C41 C42 107.7(5) . . ? C26 C41 C43 110.6(4) . . ? C44 C41 C43 107.3(5) . . ? C42 C41 C43 109.1(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O5 C45 C50 118.2(4) . . ? O5 C45 C46 121.8(5) . . ? C50 C45 C46 120.0(5) . . ? O5 C45 Li2 43.7(3) . . ? C50 C45 Li2 103.0(4) . . ? C46 C45 Li2 118.5(4) . . ? C47 C46 C45 117.1(5) . . ? C47 C46 C59 120.2(5) . . ? C45 C46 C59 122.7(5) . . ? C46 C47 C48 125.1(5) . . ? C46 C47 H47 117.5 . . ? C48 C47 H47 117.5 . . ? C49 C48 C47 115.6(5) . . ? C49 C48 C63 122.6(5) . . ? C47 C48 C63 121.8(5) . . ? C50 C49 C48 123.2(5) . . ? C50 C49 H49 118.4 . . ? C48 C49 H49 118.4 . . ? C49 C50 C45 119.1(5) . . ? C49 C50 C51 118.7(5) . . ? C45 C50 C51 122.1(5) . . ? N3 C51 C50 118.5(4) . . ? N3 C51 H51A 107.7 . . ? C50 C51 H51A 107.7 . . ? N3 C51 H51B 107.7 . . ? C50 C51 H51B 107.7 . . ? H51A C51 H51B 107.1 . . ? C57 C52 N3 118.5(4) . . ? C57 C52 C53 115.4(5) . . ? N3 C52 C53 126.1(5) . . ? C57 C52 Li3 76.0(4) . . ? N3 C52 Li3 59.6(3) . . ? C53 C52 Li3 136.8(4) . . ? C54 C53 C52 120.8(5) . . ? C54 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? C55 C54 C53 122.7(5) . . ? C55 C54 H54 118.6 . . ? C53 C54 H54 118.6 . . ? C54 C55 C56 118.2(5) . . ? C54 C55 O6 116.7(6) . . ? C56 C55 O6 125.1(6) . . ? C57 C56 C55 119.5(6) . . ? C57 C56 H56 120.2 . . ? C55 C56 H56 120.2 . . ? C56 C57 C52 123.4(5) . . ? C56 C57 H57 118.3 . . ? C52 C57 H57 118.3 . . ? O6 C58 H58A 109.5 . . ? O6 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? O6 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C46 C59 C61 110.7(5) . . ? C46 C59 C62 109.2(5) . . ? C61 C59 C62 109.3(5) . . ? C46 C59 C60 112.3(5) . . ? C61 C59 C60 106.8(5) . . ? C62 C59 C60 108.4(6) . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C59 C62 H62A 109.5 . . ? C59 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C59 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64' C63 C64 38.1(9) . . ? C64' C63 C48 111.4(9) . . ? C64 C63 C48 108.8(9) . . ? C64' C63 C66' 114.2(12) . . ? C64 C63 C66' 82.0(11) . . ? C48 C63 C66' 112.1(10) . . ? C64' C63 C65' 105.6(11) . . ? C64 C63 C65' 136.4(12) . . ? C48 C63 C65' 107.8(9) . . ? C66' C63 C65' 105.1(11) . . ? C64' C63 C65 74.7(11) . . ? C64 C63 C65 111.0(12) . . ? C48 C63 C65 108.8(9) . . ? C66' C63 C65 129.8(12) . . ? C65' C63 C65 33.1(9) . . ? C64' C63 C66 133.1(13) . . ? C64 C63 C66 110.1(12) . . ? C48 C63 C66 112.3(9) . . ? C66' C63 C66 30.9(9) . . ? C65' C63 C66 76.0(10) . . ? C65 C63 C66 105.8(11) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? C63 C64' H64D 109.5 . . ? C63 C64' H64E 109.5 . . ? H64D C64' H64E 109.5 . . ? C63 C64' H64F 109.5 . . ? H64D C64' H64F 109.5 . . ? H64E C64' H64F 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? C63 C65' H65D 109.5 . . ? C63 C65' H65E 109.5 . . ? H65D C65' H65E 109.5 . . ? C63 C65' H65F 109.5 . . ? H65D C65' H65F 109.5 . . ? H65E C65' H65F 109.5 . . ? C63 C66 H66A 109.5 . . ? C63 C66 H66B 109.5 . . ? C63 C66 H66C 109.5 . . ? C63 C66' H66D 109.5 . . ? C63 C66' H66E 109.5 . . ? H66D C66' H66E 109.5 . . ? C63 C66' H66F 109.5 . . ? H66D C66' H66F 109.5 . . ? H66E C66' H66F 109.5 . . ? O7 C67 C68 98.9(13) . . ? O7 C67 H67A 112.0 . . ? C68 C67 H67A 112.0 . . ? O7 C67 H67B 112.0 . . ? C68 C67 H67B 112.0 . . ? H67A C67 H67B 109.7 . . ? O7 C67' C68' 113.5(15) . . ? O7 C67' H67C 108.9 . . ? C68' C67' H67C 108.9 . . ? O7 C67' H67D 108.9 . . ? C68' C67' H67D 108.9 . . ? H67C C67' H67D 107.7 . . ? C69 C68 C67 103.8(14) . . ? C69 C68 H68A 111.0 . . ? C67 C68 H68A 111.0 . . ? C69 C68 H68B 111.0 . . ? C67 C68 H68B 111.0 . . ? H68A C68 H68B 109.0 . . ? C69' C68' C67' 100.9(15) . . ? C69' C68' H68C 111.6 . . ? C67' C68' H68C 111.6 . . ? C69' C68' H68D 111.6 . . ? C67' C68' H68D 111.6 . . ? H68C C68' H68D 109.4 . . ? C68 C69 C70 105.3(14) . . ? C68 C69 H69A 110.7 . . ? C70 C69 H69A 110.7 . . ? C68 C69 H69B 110.7 . . ? C70 C69 H69B 110.7 . . ? H69A C69 H69B 108.8 . . ? C68' C69' C70' 113.3(16) . . ? C68' C69' H69C 108.9 . . ? C70' C69' H69C 108.9 . . ? C68' C69' H69D 108.9 . . ? C70' C69' H69D 108.9 . . ? H69C C69' H69D 107.7 . . ? O7 C70 C69 97.5(12) . . ? O7 C70 H70A 112.3 . . ? C69 C70 H70A 112.3 . . ? O7 C70 H70B 112.3 . . ? C69 C70 H70B 112.3 . . ? H70A C70 H70B 109.9 . . ? C69' C70' O7 104.4(15) . . ? C69' C70' H70C 110.9 . . ? O7 C70' H70C 110.9 . . ? C69' C70' H70D 110.9 . . ? O7 C70' H70D 110.9 . . ? H70C C70' H70D 108.9 . . ? O8 C71 C72 106.2(6) . . ? O8 C71 H71A 110.5 . . ? C72 C71 H71A 110.5 . . ? O8 C71 H71B 110.5 . . ? C72 C71 H71B 110.5 . . ? H71A C71 H71B 108.7 . . ? C71 C72 C73 104.7(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 103.6(7) . . ? C74 C73 H73A 111.0 . . ? C72 C73 H73A 111.0 . . ? C74 C73 H73B 111.0 . . ? C72 C73 H73B 111.0 . . ? H73A C73 H73B 109.0 . . ? O8 C74 C73 111.1(6) . . ? O8 C74 H74A 109.4 . . ? C73 C74 H74A 109.4 . . ? O8 C74 H74B 109.4 . . ? C73 C74 H74B 109.4 . . ? H74A C74 H74B 108.0 . . ? O9 C75 C76 105.2(7) . . ? O9 C75 H75A 110.7 . . ? C76 C75 H75A 110.7 . . ? O9 C75 H75B 110.7 . . ? C76 C75 H75B 110.7 . . ? H75A C75 H75B 108.8 . . ? C77 C76 C75 109.6(8) . . ? C77 C76 H76A 109.8 . . ? C75 C76 H76A 109.8 . . ? C77 C76 H76B 109.8 . . ? C75 C76 H76B 109.8 . . ? H76A C76 H76B 108.2 . . ? C76 C77 C78 102.4(8) . . ? C76 C77 H77A 111.3 . . ? C78 C77 H77A 111.3 . . ? C76 C77 H77B 111.3 . . ? C78 C77 H77B 111.3 . . ? H77A C77 H77B 109.2 . . ? O9 C78 C77 108.8(8) . . ? O9 C78 H78A 109.9 . . ? C77 C78 H78A 109.9 . . ? O9 C78 H78B 109.9 . . ? C77 C78 H78B 109.9 . . ? H78A C78 H78B 108.3 . . ? C81 C80 C79 157(3) . . ? C81' C80' C79' 128(3) . . ? C82 C81 C80 138(3) . . ? C80' C81' C82' 127(2) . . ? C81 C82 C83 173(4) . . ? C83' C82' C81' 108.5(17) . . ? C84 C83 C82 111(3) . . ? C82' C83' C84' 104(2) . . ? C90 C85 C89 80(5) 2_756 2_756 ? C90 C85 C86 110(5) 2_756 . ? C89 C85 C86 30.7(13) 2_756 . ? C89 C86 C87 73(3) 2_756 . ? C89 C86 C85 73(3) 2_756 . ? C87 C86 C85 117(2) . . ? C89 C86 C88 71(3) 2_756 2_756 ? C87 C86 C88 12(3) . 2_756 ? C85 C86 C88 106(2) . 2_756 ? C89 C86 C90 57(2) 2_756 2_756 ? C87 C86 C90 107(2) . 2_756 ? C85 C86 C90 16.0(16) . 2_756 ? C88 C86 C90 98(2) 2_756 2_756 ? C88 C87 C87 139(10) 2_756 2_756 ? C88 C87 C89 85(9) 2_756 2_756 ? C87 C87 C89 135(4) 2_756 2_756 ? C88 C87 C88 147(9) 2_756 . ? C87 C87 C88 8(3) 2_756 . ? C89 C87 C88 128(2) 2_756 . ? C88 C87 C86 91(10) 2_756 . ? C87 C87 C86 125(4) 2_756 . ? C89 C87 C86 31.0(13) 2_756 . ? C88 C87 C86 119(2) . . ? C87 C88 C89 83(9) 2_756 . ? C87 C88 C87 33(9) 2_756 . ? C89 C88 C87 115.7(19) . . ? C87 C88 C86 77(9) 2_756 2_756 ? C89 C88 C86 30.5(13) . 2_756 ? C87 C88 C86 107.3(19) . 2_756 ? C87 C88 C88 28(8) 2_756 2_756 ? C89 C88 C88 110(3) . 2_756 ? C87 C88 C88 5.5(17) . 2_756 ? C86 C88 C88 102(3) 2_756 2_756 ? C86 C89 C87 76(3) 2_756 2_756 ? C86 C89 C88 78(3) 2_756 . ? C87 C89 C88 12(3) 2_756 . ? C86 C89 C90 96(3) 2_756 . ? C87 C89 C90 125(3) 2_756 . ? C88 C89 C90 114(2) . . ? C86 C89 C85 76(3) 2_756 2_756 ? C87 C89 C85 120(2) 2_756 2_756 ? C88 C89 C85 110(2) . 2_756 ? C90 C89 C85 20.1(17) . 2_756 ? C85 C90 C89 80(5) 2_756 . ? C85 C90 C86 54(4) 2_756 2_756 ? C89 C90 C86 26.7(12) . 2_756 ? O1 Li1 O7 130.7(6) . . ? O1 Li1 N2 98.5(5) . . ? O7 Li1 N2 121.1(5) . . ? O1 Li1 C1 25.9(2) . . ? O7 Li1 C1 105.0(4) . . ? N2 Li1 C1 120.7(5) . . ? O1 Li1 Yb1 46.4(3) . . ? O7 Li1 Yb1 152.4(5) . . ? N2 Li1 Yb1 52.1(3) . . ? C1 Li1 Yb1 69.5(2) . . ? O3 Li2 O8 136.0(6) . . ? O3 Li2 O5 94.3(4) . . ? O8 Li2 O5 125.5(6) . . ? O3 Li2 C45 115.2(4) . . ? O8 Li2 C45 97.9(4) . . ? O5 Li2 C45 29.2(2) . . ? O3 Li2 Yb1 48.4(2) . . ? O8 Li2 Yb1 164.9(5) . . ? O5 Li2 Yb1 46.0(2) . . ? C45 Li2 Yb1 70.7(2) . . ? O9 Li3 N1 114.9(5) . . ? O9 Li3 N3 146.1(6) . . ? N1 Li3 N3 98.0(4) . . ? O9 Li3 C52 115.9(5) . . ? N1 Li3 C52 117.0(4) . . ? N3 Li3 C52 34.7(2) . . ? O9 Li3 C8 104.2(4) . . ? N1 Li3 C8 33.7(2) . . ? N3 Li3 C8 107.8(4) . . ? C52 Li3 C8 139.7(4) . . ? O9 Li3 Yb1 159.1(5) . . ? N1 Li3 Yb1 48.7(2) . . ? N3 Li3 Yb1 49.8(2) . . ? C52 Li3 Yb1 71.6(2) . . ? C8 Li3 Yb1 69.2(2) . . ? 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 O5 Yb1 O1 C1 147.7(5) . . . . ? O3 Yb1 O1 C1 -141.5(4) . . . . ? N1 Yb1 O1 C1 29.4(4) . . . . ? N3 Yb1 O1 C1 -48.6(4) . . . . ? N2 Yb1 O1 C1 141.2(4) . . . . ? Li2 Yb1 O1 C1 -155.5(5) . . . . ? Li1 Yb1 O1 C1 139.4(6) . . . . ? Li3 Yb1 O1 C1 -9.5(4) . . . . ? C23 Yb1 O1 C1 -150.2(4) . . . . ? O5 Yb1 O1 Li1 8.4(6) . . . . ? O3 Yb1 O1 Li1 79.2(3) . . . . ? N1 Yb1 O1 Li1 -109.9(3) . . . . ? N3 Yb1 O1 Li1 172.1(3) . . . . ? N2 Yb1 O1 Li1 1.8(3) . . . . ? Li2 Yb1 O1 Li1 65.1(5) . . . . ? Li3 Yb1 O1 Li1 -148.9(4) . . . . ? C23 Yb1 O1 Li1 70.4(3) . . . . ? O5 Yb1 O3 C23 142.1(3) . . . . ? O1 Yb1 O3 C23 -24.9(3) . . . . ? N1 Yb1 O3 C23 -102.3(8) . . . . ? N3 Yb1 O3 C23 -137.9(3) . . . . ? N2 Yb1 O3 C23 51.2(3) . . . . ? Li2 Yb1 O3 C23 138.8(5) . . . . ? Li1 Yb1 O3 C23 11.8(4) . . . . ? Li3 Yb1 O3 C23 -127.4(4) . . . . ? O5 Yb1 O3 Li2 3.3(3) . . . . ? O1 Yb1 O3 Li2 -163.7(3) . . . . ? N1 Yb1 O3 Li2 118.9(8) . . . . ? N3 Yb1 O3 Li2 83.3(4) . . . . ? N2 Yb1 O3 Li2 -87.6(4) . . . . ? Li1 Yb1 O3 Li2 -127.0(4) . . . . ? Li3 Yb1 O3 Li2 93.8(4) . . . . ? C23 Yb1 O3 Li2 -138.8(5) . . . . ? O1 Yb1 O5 C45 -168.7(5) . . . . ? O3 Yb1 O5 C45 117.9(4) . . . . ? N1 Yb1 O5 C45 -53.5(4) . . . . ? N3 Yb1 O5 C45 26.5(4) . . . . ? N2 Yb1 O5 C45 -162.3(4) . . . . ? Li2 Yb1 O5 C45 121.0(6) . . . . ? Li1 Yb1 O5 C45 -162.2(5) . . . . ? Li3 Yb1 O5 C45 -11.8(5) . . . . ? C23 Yb1 O5 C45 130.5(4) . . . . ? O1 Yb1 O5 Li2 70.2(6) . . . . ? O3 Yb1 O5 Li2 -3.2(3) . . . . ? N1 Yb1 O5 Li2 -174.5(3) . . . . ? N3 Yb1 O5 Li2 -94.5(3) . . . . ? N2 Yb1 O5 Li2 76.6(3) . . . . ? Li1 Yb1 O5 Li2 76.8(4) . . . . ? Li3 Yb1 O5 Li2 -132.8(4) . . . . ? C23 Yb1 O5 Li2 9.5(3) . . . . ? O5 Yb1 N1 C8 -6.8(4) . . . . ? O1 Yb1 N1 C8 160.8(4) . . . . ? O3 Yb1 N1 C8 -120.2(8) . . . . ? N3 Yb1 N1 C8 -84.4(3) . . . . ? N2 Yb1 N1 C8 87.4(4) . . . . ? Li2 Yb1 N1 C8 -13.0(6) . . . . ? Li1 Yb1 N1 C8 125.9(4) . . . . ? Li3 Yb1 N1 C8 -90.9(5) . . . . ? C23 Yb1 N1 C8 161.8(3) . . . . ? O5 Yb1 N1 C7 -150.5(3) . . . . ? O1 Yb1 N1 C7 17.1(3) . . . . ? O3 Yb1 N1 C7 96.2(8) . . . . ? N3 Yb1 N1 C7 132.0(3) . . . . ? N2 Yb1 N1 C7 -56.3(3) . . . . ? Li2 Yb1 N1 C7 -156.7(4) . . . . ? Li1 Yb1 N1 C7 -17.8(4) . . . . ? Li3 Yb1 N1 C7 125.4(5) . . . . ? C23 Yb1 N1 C7 18.2(6) . . . . ? O5 Yb1 N1 Li3 84.1(3) . . . . ? O1 Yb1 N1 Li3 -108.3(3) . . . . ? O3 Yb1 N1 Li3 -29.2(9) . . . . ? N3 Yb1 N1 Li3 6.6(3) . . . . ? N2 Yb1 N1 Li3 178.3(3) . . . . ? Li2 Yb1 N1 Li3 77.9(5) . . . . ? Li1 Yb1 N1 Li3 -143.2(4) . . . . ? C23 Yb1 N1 Li3 -107.3(5) . . . . ? O5 Yb1 N2 C30 65.0(4) . . . . ? O1 Yb1 N2 C30 -116.5(4) . . . . ? O3 Yb1 N2 C30 141.6(4) . . . . ? N1 Yb1 N2 C30 -42.7(4) . . . . ? N3 Yb1 N2 C30 102.4(6) . . . . ? Li2 Yb1 N2 C30 103.4(4) . . . . ? Li1 Yb1 N2 C30 -114.8(5) . . . . ? Li3 Yb1 N2 C30 -40.5(6) . . . . ? C23 Yb1 N2 C30 159.1(4) . . . . ? O5 Yb1 N2 C29 -73.6(3) . . . . ? O1 Yb1 N2 C29 104.9(3) . . . . ? O3 Yb1 N2 C29 3.0(3) . . . . ? N1 Yb1 N2 C29 178.7(3) . . . . ? N3 Yb1 N2 C29 -36.1(7) . . . . ? Li2 Yb1 N2 C29 -35.2(4) . . . . ? Li1 Yb1 N2 C29 106.6(4) . . . . ? Li3 Yb1 N2 C29 -179.1(4) . . . . ? C23 Yb1 N2 C29 20.5(3) . . . . ? O5 Yb1 N2 Li1 179.8(3) . . . . ? O1 Yb1 N2 Li1 -1.7(3) . . . . ? O3 Yb1 N2 Li1 -103.6(3) . . . . ? N1 Yb1 N2 Li1 72.1(3) . . . . ? N3 Yb1 N2 Li1 -142.7(5) . . . . ? Li2 Yb1 N2 Li1 -141.8(4) . . . . ? Li3 Yb1 N2 Li1 74.3(5) . . . . ? C23 Yb1 N2 Li1 -86.1(3) . . . . ? O5 Yb1 N3 C52 161.1(3) . . . . ? O1 Yb1 N3 C52 -15.1(3) . . . . ? O3 Yb1 N3 C52 84.5(3) . . . . ? N1 Yb1 N3 C52 -90.1(3) . . . . ? N2 Yb1 N3 C52 122.9(5) . . . . ? Li2 Yb1 N3 C52 122.0(4) . . . . ? Li1 Yb1 N3 C52 -5.6(6) . . . . ? Li3 Yb1 N3 C52 -83.7(4) . . . . ? C23 Yb1 N3 C52 70.3(3) . . . . ? O5 Yb1 N3 C51 20.1(3) . . . . ? O1 Yb1 N3 C51 -156.1(3) . . . . ? O3 Yb1 N3 C51 -56.5(3) . . . . ? N1 Yb1 N3 C51 128.9(3) . . . . ? N2 Yb1 N3 C51 -18.0(7) . . . . ? Li2 Yb1 N3 C51 -19.0(4) . . . . ? Li1 Yb1 N3 C51 -146.5(5) . . . . ? Li3 Yb1 N3 C51 135.3(5) . . . . ? C23 Yb1 N3 C51 -70.7(3) . . . . ? O5 Yb1 N3 Li3 -115.2(3) . . . . ? O1 Yb1 N3 Li3 68.6(3) . . . . ? O3 Yb1 N3 Li3 168.2(3) . . . . ? N1 Yb1 N3 Li3 -6.4(3) . . . . ? N2 Yb1 N3 Li3 -153.3(5) . . . . ? Li2 Yb1 N3 Li3 -154.2(4) . . . . ? Li1 Yb1 N3 Li3 78.2(5) . . . . ? C23 Yb1 N3 Li3 154.0(3) . . . . ? Li1 O1 C1 C6 94.9(6) . . . . ? Yb1 O1 C1 C6 -38.5(7) . . . . ? Li1 O1 C1 C2 -84.8(6) . . . . ? Yb1 O1 C1 C2 141.9(4) . . . . ? Yb1 O1 C1 Li1 -133.3(6) . . . . ? O1 C1 C2 C3 178.7(5) . . . . ? C6 C1 C2 C3 -0.9(8) . . . . ? Li1 C1 C2 C3 138.2(5) . . . . ? O1 C1 C2 C15 -0.1(8) . . . . ? C6 C1 C2 C15 -179.7(5) . . . . ? Li1 C1 C2 C15 -40.6(6) . . . . ? C1 C2 C3 C4 1.1(9) . . . . ? C15 C2 C3 C4 179.9(5) . . . . ? C2 C3 C4 C5 0.5(9) . . . . ? C2 C3 C4 C19 -177.3(6) . . . . ? C3 C4 C5 C6 -2.2(8) . . . . ? C19 C4 C5 C6 175.5(6) . . . . ? C4 C5 C6 C1 2.4(8) . . . . ? C4 C5 C6 C7 -171.6(5) . . . . ? O1 C1 C6 C5 179.6(5) . . . . ? C2 C1 C6 C5 -0.8(8) . . . . ? Li1 C1 C6 C5 -138.9(5) . . . . ? O1 C1 C6 C7 -6.6(7) . . . . ? C2 C1 C6 C7 173.0(5) . . . . ? Li1 C1 C6 C7 34.8(6) . . . . ? C8 N1 C7 C6 161.1(4) . . . . ? Li3 N1 C7 C6 56.0(6) . . . . ? Yb1 N1 C7 C6 -53.6(5) . . . . ? C5 C6 C7 N1 -133.2(5) . . . . ? C1 C6 C7 N1 52.9(7) . . . . ? C7 N1 C8 C13 -162.6(4) . . . . ? Li3 N1 C8 C13 -39.2(5) . . . . ? Yb1 N1 C8 C13 51.2(5) . . . . ? C7 N1 C8 C9 16.0(7) . . . . ? Li3 N1 C8 C9 139.3(5) . . . . ? Yb1 N1 C8 C9 -130.3(4) . . . . ? C7 N1 C8 Li3 -123.4(5) . . . . ? Yb1 N1 C8 Li3 90.4(4) . . . . ? N1 C8 C9 C10 179.5(5) . . . . ? C13 C8 C9 C10 -1.8(7) . . . . ? Li3 C8 C9 C10 -99.5(9) . . . . ? C8 C9 C10 C11 -0.2(8) . . . . ? C9 C10 C11 C12 1.7(9) . . . . ? C9 C10 C11 O2 -179.0(5) . . . . ? C14 O2 C11 C10 161.8(6) . . . . ? C14 O2 C11 C12 -19.0(9) . . . . ? C10 C11 C12 C13 -1.0(8) . . . . ? O2 C11 C12 C13 179.8(5) . . . . ? C11 C12 C13 C8 -1.3(8) . . . . ? N1 C8 C13 C12 -178.7(5) . . . . ? C9 C8 C13 C12 2.6(7) . . . . ? Li3 C8 C13 C12 148.6(6) . . . . ? C3 C2 C15 C16 -0.2(8) . . . . ? C1 C2 C15 C16 178.6(5) . . . . ? C3 C2 C15 C18 119.8(6) . . . . ? C1 C2 C15 C18 -61.4(7) . . . . ? C3 C2 C15 C17 -119.6(6) . . . . ? C1 C2 C15 C17 59.2(7) . . . . ? C3 C4 C19 C22' 14.1(12) . . . . ? C5 C4 C19 C22' -163.5(9) . . . . ? C3 C4 C19 C21 177.4(9) . . . . ? C5 C4 C19 C21 -0.2(11) . . . . ? C3 C4 C19 C22 58.0(10) . . . . ? C5 C4 C19 C22 -119.7(9) . . . . ? C3 C4 C19 C20' -102.4(9) . . . . ? C5 C4 C19 C20' 80.0(9) . . . . ? C3 C4 C19 C21' 146.4(9) . . . . ? C5 C4 C19 C21' -31.2(11) . . . . ? C3 C4 C19 C20 -51.5(10) . . . . ? C5 C4 C19 C20 130.9(9) . . . . ? Li2 O3 C23 C28 69.7(7) . . . . ? Yb1 O3 C23 C28 -55.2(5) . . . . ? Li2 O3 C23 C24 -108.1(6) . . . . ? Yb1 O3 C23 C24 127.0(4) . . . . ? Li2 O3 C23 Yb1 124.9(6) . . . . ? O5 Yb1 C23 O3 -36.8(3) . . . . ? O1 Yb1 C23 O3 155.1(3) . . . . ? N1 Yb1 C23 O3 154.1(4) . . . . ? N3 Yb1 C23 O3 43.8(4) . . . . ? N2 Yb1 C23 O3 -123.8(4) . . . . ? Li2 Yb1 C23 O3 -29.5(4) . . . . ? Li1 Yb1 C23 O3 -167.5(4) . . . . ? Li3 Yb1 C23 O3 71.6(5) . . . . ? O5 Yb1 C23 C28 96.7(3) . . . . ? O1 Yb1 C23 C28 -71.4(3) . . . . ? O3 Yb1 C23 C28 133.5(5) . . . . ? N1 Yb1 C23 C28 -72.5(5) . . . . ? N3 Yb1 C23 C28 177.3(3) . . . . ? N2 Yb1 C23 C28 9.7(3) . . . . ? Li2 Yb1 C23 C28 104.0(4) . . . . ? Li1 Yb1 C23 C28 -34.0(3) . . . . ? Li3 Yb1 C23 C28 -154.9(4) . . . . ? O5 Yb1 C23 C24 -120.6(5) . . . . ? O1 Yb1 C23 C24 71.2(5) . . . . ? O3 Yb1 C23 C24 -83.8(6) . . . . ? N1 Yb1 C23 C24 70.2(7) . . . . ? N3 Yb1 C23 C24 -40.0(5) . . . . ? N2 Yb1 C23 C24 152.4(6) . . . . ? Li2 Yb1 C23 C24 -113.3(6) . . . . ? Li1 Yb1 C23 C24 108.7(6) . . . . ? Li3 Yb1 C23 C24 -12.2(7) . . . . ? O3 C23 C24 C25 -175.4(4) . . . . ? C28 C23 C24 C25 6.7(7) . . . . ? Yb1 C23 C24 C25 -129.8(4) . . . . ? O3 C23 C24 C37 8.1(7) . . . . ? C28 C23 C24 C37 -169.7(5) . . . . ? Yb1 C23 C24 C37 53.7(7) . . . . ? C23 C24 C25 C26 -2.5(8) . . . . ? C37 C24 C25 C26 173.9(5) . . . . ? C24 C25 C26 C27 -2.8(8) . . . . ? C24 C25 C26 C41 -177.7(5) . . . . ? C25 C26 C27 C28 4.0(7) . . . . ? C41 C26 C27 C28 179.0(5) . . . . ? C26 C27 C28 C23 0.3(8) . . . . ? C26 C27 C28 C29 -173.2(5) . . . . ? O3 C23 C28 C27 176.2(4) . . . . ? C24 C23 C28 C27 -5.8(7) . . . . ? Yb1 C23 C28 C27 146.6(4) . . . . ? O3 C23 C28 C29 -10.3(7) . . . . ? C24 C23 C28 C29 167.7(4) . . . . ? Yb1 C23 C28 C29 -39.9(4) . . . . ? C30 N2 C29 C28 166.3(4) . . . . ? Li1 N2 C29 C28 42.3(6) . . . . ? Yb1 N2 C29 C28 -52.4(5) . . . . ? C27 C28 C29 N2 -117.4(5) . . . . ? C23 C28 C29 N2 69.0(6) . . . . ? C29 N2 C30 C31 -177.3(5) . . . . ? Li1 N2 C30 C31 -57.2(6) . . . . ? Yb1 N2 C30 C31 42.8(6) . . . . ? C29 N2 C30 C35 1.8(7) . . . . ? Li1 N2 C30 C35 121.8(6) . . . . ? Yb1 N2 C30 C35 -138.1(5) . . . . ? N2 C30 C31 C32 178.6(6) . . . . ? C35 C30 C31 C32 -0.5(8) . . . . ? C30 C31 C32 C33 1.7(9) . . . . ? C36 O4 C33 C34 5.3(9) . . . . ? C36 O4 C33 C32 -175.8(6) . . . . ? C31 C32 C33 C34 -1.8(9) . . . . ? C31 C32 C33 O4 179.3(6) . . . . ? O4 C33 C34 C35 179.7(6) . . . . ? C32 C33 C34 C35 0.9(9) . . . . ? C33 C34 C35 C30 0.3(9) . . . . ? N2 C30 C35 C34 -179.6(5) . . . . ? C31 C30 C35 C34 -0.5(8) . . . . ? C25 C24 C37 C39 -114.1(6) . . . . ? C23 C24 C37 C39 62.2(6) . . . . ? C25 C24 C37 C38 4.5(7) . . . . ? C23 C24 C37 C38 -179.2(5) . . . . ? C25 C24 C37 C40 125.2(5) . . . . ? C23 C24 C37 C40 -58.5(7) . . . . ? C25 C26 C41 C44 -22.3(8) . . . . ? C27 C26 C41 C44 163.0(5) . . . . ? C25 C26 C41 C42 97.4(6) . . . . ? C27 C26 C41 C42 -77.2(7) . . . . ? C25 C26 C41 C43 -142.4(6) . . . . ? C27 C26 C41 C43 42.9(7) . . . . ? Li2 O5 C45 C50 79.0(6) . . . . ? Yb1 O5 C45 C50 -37.8(7) . . . . ? Li2 O5 C45 C46 -99.5(6) . . . . ? Yb1 O5 C45 C46 143.7(4) . . . . ? Yb1 O5 C45 Li2 -116.8(5) . . . . ? O5 C45 C46 C47 179.5(5) . . . . ? C50 C45 C46 C47 1.0(8) . . . . ? Li2 C45 C46 C47 128.6(5) . . . . ? O5 C45 C46 C59 -2.6(8) . . . . ? C50 C45 C46 C59 179.0(5) . . . . ? Li2 C45 C46 C59 -53.5(7) . . . . ? C45 C46 C47 C48 -0.6(9) . . . . ? C59 C46 C47 C48 -178.6(5) . . . . ? C46 C47 C48 C49 0.0(9) . . . . ? C46 C47 C48 C63 -179.4(6) . . . . ? C47 C48 C49 C50 0.1(8) . . . . ? C63 C48 C49 C50 179.5(5) . . . . ? C48 C49 C50 C45 0.4(8) . . . . ? C48 C49 C50 C51 -174.9(5) . . . . ? O5 C45 C50 C49 -179.5(4) . . . . ? C46 C45 C50 C49 -0.9(7) . . . . ? Li2 C45 C50 C49 -135.3(5) . . . . ? O5 C45 C50 C51 -4.3(7) . . . . ? C46 C45 C50 C51 174.2(5) . . . . ? Li2 C45 C50 C51 39.8(6) . . . . ? C52 N3 C51 C50 160.4(4) . . . . ? Li3 N3 C51 C50 55.3(7) . . . . ? Yb1 N3 C51 C50 -56.2(5) . . . . ? C49 C50 C51 N3 -131.6(5) . . . . ? C45 C50 C51 N3 53.2(7) . . . . ? C51 N3 C52 C57 176.7(4) . . . . ? Li3 N3 C52 C57 -50.4(5) . . . . ? Yb1 N3 C52 C57 34.5(5) . . . . ? C51 N3 C52 C53 -4.8(7) . . . . ? Li3 N3 C52 C53 128.1(5) . . . . ? Yb1 N3 C52 C53 -147.0(4) . . . . ? C51 N3 C52 Li3 -132.9(5) . . . . ? Yb1 N3 C52 Li3 84.9(4) . . . . ? C57 C52 C53 C54 -0.5(7) . . . . ? N3 C52 C53 C54 -179.1(5) . . . . ? Li3 C52 C53 C54 -97.1(7) . . . . ? C52 C53 C54 C55 0.5(8) . . . . ? C53 C54 C55 C56 0.0(9) . . . . ? C53 C54 C55 O6 -179.1(5) . . . . ? C58 O6 C55 C54 160.7(6) . . . . ? C58 O6 C55 C56 -18.4(9) . . . . ? C54 C55 C56 C57 -0.4(8) . . . . ? O6 C55 C56 C57 178.6(5) . . . . ? C55 C56 C57 C52 0.4(8) . . . . ? N3 C52 C57 C56 178.7(5) . . . . ? C53 C52 C57 C56 0.1(7) . . . . ? Li3 C52 C57 C56 135.6(6) . . . . ? C47 C46 C59 C61 -126.5(6) . . . . ? C45 C46 C59 C61 55.6(7) . . . . ? C47 C46 C59 C62 113.1(6) . . . . ? C45 C46 C59 C62 -64.8(7) . . . . ? C47 C46 C59 C60 -7.2(8) . . . . ? C45 C46 C59 C60 174.9(6) . . . . ? C49 C48 C63 C64' -153.2(10) . . . . ? C47 C48 C63 C64' 26.1(11) . . . . ? C49 C48 C63 C64 -112.6(10) . . . . ? C47 C48 C63 C64 66.7(11) . . . . ? C49 C48 C63 C66' -23.8(11) . . . . ? C47 C48 C63 C66' 155.5(9) . . . . ? C49 C48 C63 C65' 91.4(10) . . . . ? C47 C48 C63 C65' -89.3(10) . . . . ? C49 C48 C63 C65 126.3(10) . . . . ? C47 C48 C63 C65 -54.4(11) . . . . ? C49 C48 C63 C66 9.6(11) . . . . ? C47 C48 C63 C66 -171.1(9) . . . . ? C67' O7 C67 C68 -56(7) . . . . ? C70 O7 C67 C68 53.3(19) . . . . ? C70' O7 C67 C68 40.0(18) . . . . ? Li1 O7 C67 C68 -115.1(13) . . . . ? C67 O7 C67' C68' 77(7) . . . . ? C70 O7 C67' C68' 2(2) . . . . ? C70' O7 C67' C68' -11(2) . . . . ? Li1 O7 C67' C68' -156.0(14) . . . . ? O7 C67 C68 C69 -31(2) . . . . ? O7 C67' C68' C69' 11(2) . . . . ? C67 C68 C69 C70 1(2) . . . . ? C67' C68' C69' C70' -7(2) . . . . ? C67 O7 C70 C69 -51.8(19) . . . . ? C67' O7 C70 C69 -39.6(19) . . . . ? C70' O7 C70 C69 42(7) . . . . ? Li1 O7 C70 C69 116.9(13) . . . . ? C68 C69 C70 O7 28(2) . . . . ? C68' C69' C70' O7 0(2) . . . . ? C67 O7 C70' C69' -6(2) . . . . ? C67' O7 C70' C69' 6(2) . . . . ? C70 O7 C70' C69' -96(8) . . . . ? Li1 O7 C70' C69' 150.7(13) . . . . ? C74 O8 C71 C72 22.0(9) . . . . ? Li2 O8 C71 C72 -155.1(7) . . . . ? O8 C71 C72 C73 -26.1(10) . . . . ? C71 C72 C73 C74 19.9(11) . . . . ? C71 O8 C74 C73 -9.2(11) . . . . ? Li2 O8 C74 C73 168.3(8) . . . . ? C72 C73 C74 O8 -7.3(12) . . . . ? C78 O9 C75 C76 18.2(11) . . . . ? Li3 O9 C75 C76 -177.6(7) . . . . ? O9 C75 C76 C77 -2.5(13) . . . . ? C75 C76 C77 C78 -13.1(13) . . . . ? C75 O9 C78 C77 -27.6(11) . . . . ? Li3 O9 C78 C77 167.9(7) . . . . ? C76 C77 C78 O9 25.0(12) . . . . ? C79 C80 C81 C82 153(7) . . . . ? C79' C80' C81' C82' -160(3) . . . . ? C80 C81 C82 C83 114(28) . . . . ? C80' C81' C82' C83' -34(5) . . . . ? C81 C82 C83 C84 -94(29) . . . . ? C81' C82' C83' C84' -27(4) . . . . ? C90 C85 C86 C89 3(8) 2_756 . . 2_756 ? C90 C85 C86 C87 -57(8) 2_756 . . . ? C89 C85 C86 C87 -60(3) 2_756 . . . ? C90 C85 C86 C88 -61(8) 2_756 . . 2_756 ? C89 C85 C86 C88 -64(3) 2_756 . . 2_756 ? C89 C85 C86 C90 -3(8) 2_756 . . 2_756 ? C89 C86 C87 C88 -79(16) 2_756 . . 2_756 ? C85 C86 C87 C88 -19(17) . . . 2_756 ? C90 C86 C87 C88 -33(16) 2_756 . . 2_756 ? C89 C86 C87 C87 121(7) 2_756 . . 2_756 ? C85 C86 C87 C87 -179(6) . . . 2_756 ? C88 C86 C87 C87 -160(22) 2_756 . . 2_756 ? C90 C86 C87 C87 167(6) 2_756 . . 2_756 ? C85 C86 C87 C89 60(3) . . . 2_756 ? C88 C86 C87 C89 79(16) 2_756 . . 2_756 ? C90 C86 C87 C89 46(3) 2_756 . . 2_756 ? C89 C86 C87 C88 116(3) 2_756 . . . ? C85 C86 C87 C88 176(2) . . . . ? C88 C86 C87 C88 -165(17) 2_756 . . . ? C90 C86 C87 C88 162.3(19) 2_756 . . . ? C88 C87 C88 C87 0.00(15) 2_756 . . 2_756 ? C89 C87 C88 C87 -174(32) 2_756 . . 2_756 ? C86 C87 C88 C87 151(32) . . . 2_756 ? C88 C87 C88 C89 -6(28) 2_756 . . . ? C87 C87 C88 C89 -6(28) 2_756 . . . ? C89 C87 C88 C89 -179(4) 2_756 . . . ? C86 C87 C88 C89 145(4) . . . . ? C88 C87 C88 C86 26(29) 2_756 . . 2_756 ? C87 C87 C88 C86 26(29) 2_756 . . 2_756 ? C89 C87 C88 C86 -148(4) 2_756 . . 2_756 ? C86 C87 C88 C86 177(4) . . . 2_756 ? C87 C87 C88 C88 0.00(12) 2_756 . . 2_756 ? C89 C87 C88 C88 -174(32) 2_756 . . 2_756 ? C86 C87 C88 C88 151(32) . . . 2_756 ? C87 C88 C89 C86 77(16) 2_756 . . 2_756 ? C87 C88 C89 C86 81(3) . . . 2_756 ? C88 C88 C89 C86 80(4) 2_756 . . 2_756 ? C87 C88 C89 C87 3(15) . . . 2_756 ? C86 C88 C89 C87 -77(16) 2_756 . . 2_756 ? C88 C88 C89 C87 3(12) 2_756 . . 2_756 ? C87 C88 C89 C90 169(15) 2_756 . . . ? C87 C88 C89 C90 172.6(18) . . . . ? C86 C88 C89 C90 92(3) 2_756 . . . ? C88 C88 C89 C90 172(3) 2_756 . . . ? C87 C88 C89 C85 148(15) 2_756 . . 2_756 ? C87 C88 C89 C85 151.3(19) . . . 2_756 ? C86 C88 C89 C85 71(3) 2_756 . . 2_756 ? C88 C88 C89 C85 151(3) 2_756 . . 2_756 ? C86 C89 C90 C85 -3(7) 2_756 . . 2_756 ? C87 C89 C90 C85 -80(7) 2_756 . . 2_756 ? C88 C89 C90 C85 -83(7) . . . 2_756 ? C87 C89 C90 C86 -77(4) 2_756 . . 2_756 ? C88 C89 C90 C86 -80(4) . . . 2_756 ? C85 C89 C90 C86 3(7) 2_756 . . 2_756 ? C1 O1 Li1 O7 -6.3(9) . . . . ? Yb1 O1 Li1 O7 142.6(7) . . . . ? C1 O1 Li1 N2 -151.2(4) . . . . ? Yb1 O1 Li1 N2 -2.2(4) . . . . ? Yb1 O1 Li1 C1 149.0(4) . . . . ? C1 O1 Li1 Yb1 -149.0(4) . . . . ? C67 O7 Li1 O1 -8.2(15) . . . . ? C67' O7 Li1 O1 -20.5(15) . . . . ? C70 O7 Li1 O1 -174.3(11) . . . . ? C70' O7 Li1 O1 -159.8(11) . . . . ? C67 O7 Li1 N2 130.1(12) . . . . ? C67' O7 Li1 N2 117.8(12) . . . . ? C70 O7 Li1 N2 -36.1(13) . . . . ? C70' O7 Li1 N2 -21.6(13) . . . . ? C67 O7 Li1 C1 -11.1(13) . . . . ? C67' O7 Li1 C1 -23.4(12) . . . . ? C70 O7 Li1 C1 -177.2(10) . . . . ? C70' O7 Li1 C1 -162.7(10) . . . . ? C67 O7 Li1 Yb1 63.3(16) . . . . ? C67' O7 Li1 Yb1 51.0(16) . . . . ? C70 O7 Li1 Yb1 -102.9(14) . . . . ? C70' O7 Li1 Yb1 -88.4(14) . . . . ? C30 N2 Li1 O1 122.5(4) . . . . ? C29 N2 Li1 O1 -114.0(4) . . . . ? Yb1 N2 Li1 O1 2.0(4) . . . . ? C30 N2 Li1 O7 -26.8(7) . . . . ? C29 N2 Li1 O7 96.7(6) . . . . ? Yb1 N2 Li1 O7 -147.3(6) . . . . ? C30 N2 Li1 C1 108.4(5) . . . . ? C29 N2 Li1 C1 -128.2(5) . . . . ? Yb1 N2 Li1 C1 -12.2(4) . . . . ? C30 N2 Li1 Yb1 120.5(4) . . . . ? C29 N2 Li1 Yb1 -116.0(3) . . . . ? C6 C1 Li1 O1 -104.5(6) . . . . ? C2 C1 Li1 O1 114.7(6) . . . . ? O1 C1 Li1 O7 175.0(7) . . . . ? C6 C1 Li1 O7 70.5(6) . . . . ? C2 C1 Li1 O7 -70.3(6) . . . . ? O1 C1 Li1 N2 33.7(5) . . . . ? C6 C1 Li1 N2 -70.8(6) . . . . ? C2 C1 Li1 N2 148.4(5) . . . . ? O1 C1 Li1 Yb1 23.5(3) . . . . ? C6 C1 Li1 Yb1 -81.0(4) . . . . ? C2 C1 Li1 Yb1 138.2(4) . . . . ? O5 Yb1 Li1 O1 -177.50(19) . . . . ? O3 Yb1 Li1 O1 -104.2(3) . . . . ? N1 Yb1 Li1 O1 67.4(3) . . . . ? N3 Yb1 Li1 O1 -14.6(6) . . . . ? N2 Yb1 Li1 O1 -177.2(5) . . . . ? Li2 Yb1 Li1 O1 -136.0(3) . . . . ? Li3 Yb1 Li1 O1 38.8(4) . . . . ? C23 Yb1 Li1 O1 -99.8(3) . . . . ? O5 Yb1 Li1 O7 85.4(10) . . . . ? O1 Yb1 Li1 O7 -97.1(11) . . . . ? O3 Yb1 Li1 O7 158.7(10) . . . . ? N1 Yb1 Li1 O7 -29.6(10) . . . . ? N3 Yb1 Li1 O7 -111.7(10) . . . . ? N2 Yb1 Li1 O7 85.7(10) . . . . ? Li2 Yb1 Li1 O7 126.9(10) . . . . ? Li3 Yb1 Li1 O7 -58.3(11) . . . . ? C23 Yb1 Li1 O7 163.2(11) . . . . ? O5 Yb1 Li1 N2 -0.3(4) . . . . ? O1 Yb1 Li1 N2 177.2(5) . . . . ? O3 Yb1 Li1 N2 73.0(3) . . . . ? N1 Yb1 Li1 N2 -115.3(3) . . . . ? N3 Yb1 Li1 N2 162.6(3) . . . . ? Li2 Yb1 Li1 N2 41.2(4) . . . . ? Li3 Yb1 Li1 N2 -144.0(3) . . . . ? C23 Yb1 Li1 N2 77.5(3) . . . . ? O5 Yb1 Li1 C1 168.59(15) . . . . ? O1 Yb1 Li1 C1 -13.9(2) . . . . ? O3 Yb1 Li1 C1 -118.1(2) . . . . ? N1 Yb1 Li1 C1 53.5(2) . . . . ? N3 Yb1 Li1 C1 -28.5(5) . . . . ? N2 Yb1 Li1 C1 168.8(4) . . . . ? Li2 Yb1 Li1 C1 -149.9(3) . . . . ? Li3 Yb1 Li1 C1 24.9(4) . . . . ? C23 Yb1 Li1 C1 -113.7(2) . . . . ? C23 O3 Li2 O8 64.2(10) . . . . ? Yb1 O3 Li2 O8 -159.9(8) . . . . ? C23 O3 Li2 O5 -139.6(4) . . . . ? Yb1 O3 Li2 O5 -3.6(4) . . . . ? C23 O3 Li2 C45 -160.8(4) . . . . ? Yb1 O3 Li2 C45 -24.9(5) . . . . ? C23 O3 Li2 Yb1 -135.9(5) . . . . ? C71 O8 Li2 O3 -88.9(11) . . . . ? C74 O8 Li2 O3 94.3(10) . . . . ? C71 O8 Li2 O5 120.6(8) . . . . ? C74 O8 Li2 O5 -56.2(10) . . . . ? C71 O8 Li2 C45 131.3(7) . . . . ? C74 O8 Li2 C45 -45.5(8) . . . . ? C71 O8 Li2 Yb1 171.3(17) . . . . ? C74 O8 Li2 Yb1 -5(2) . . . . ? C45 O5 Li2 O3 -137.8(4) . . . . ? Yb1 O5 Li2 O3 3.8(4) . . . . ? C45 O5 Li2 O8 22.1(8) . . . . ? Yb1 O5 Li2 O8 163.7(6) . . . . ? Yb1 O5 Li2 C45 141.6(4) . . . . ? C45 O5 Li2 Yb1 -141.6(4) . . . . ? O5 C45 Li2 O3 47.8(5) . . . . ? C50 C45 Li2 O3 -69.7(6) . . . . ? C46 C45 Li2 O3 155.1(5) . . . . ? O5 C45 Li2 O8 -162.0(7) . . . . ? C50 C45 Li2 O8 80.6(5) . . . . ? C46 C45 Li2 O8 -54.6(6) . . . . ? C50 C45 Li2 O5 -117.4(5) . . . . ? C46 C45 Li2 O5 107.4(6) . . . . ? O5 C45 Li2 Yb1 28.3(3) . . . . ? C50 C45 Li2 Yb1 -89.1(4) . . . . ? C46 C45 Li2 Yb1 135.7(4) . . . . ? O5 Yb1 Li2 O3 -175.0(5) . . . . ? O1 Yb1 Li2 O3 23.0(5) . . . . ? N1 Yb1 Li2 O3 -165.6(2) . . . . ? N3 Yb1 Li2 O3 -94.7(3) . . . . ? N2 Yb1 Li2 O3 85.5(3) . . . . ? Li1 Yb1 Li2 O3 59.7(4) . . . . ? Li3 Yb1 Li2 O3 -115.2(3) . . . . ? C23 Yb1 Li2 O3 16.7(2) . . . . ? O5 Yb1 Li2 O8 -61.2(19) . . . . ? O1 Yb1 Li2 O8 136.8(19) . . . . ? O3 Yb1 Li2 O8 114(2) . . . . ? N1 Yb1 Li2 O8 -52(2) . . . . ? N3 Yb1 Li2 O8 19(2) . . . . ? N2 Yb1 Li2 O8 -161(2) . . . . ? Li1 Yb1 Li2 O8 173(2) . . . . ? Li3 Yb1 Li2 O8 -1(2) . . . . ? C23 Yb1 Li2 O8 130(2) . . . . ? O1 Yb1 Li2 O5 -162.0(2) . . . . ? O3 Yb1 Li2 O5 175.0(5) . . . . ? N1 Yb1 Li2 O5 9.4(6) . . . . ? N3 Yb1 Li2 O5 80.3(3) . . . . ? N2 Yb1 Li2 O5 -99.5(3) . . . . ? Li1 Yb1 Li2 O5 -125.4(3) . . . . ? Li3 Yb1 Li2 O5 59.7(4) . . . . ? C23 Yb1 Li2 O5 -168.4(4) . . . . ? O5 Yb1 Li2 C45 -18.7(2) . . . . ? O1 Yb1 Li2 C45 179.27(17) . . . . ? O3 Yb1 Li2 C45 156.2(5) . . . . ? N1 Yb1 Li2 C45 -9.4(5) . . . . ? N3 Yb1 Li2 C45 61.5(2) . . . . ? N2 Yb1 Li2 C45 -118.2(2) . . . . ? Li1 Yb1 Li2 C45 -144.1(3) . . . . ? Li3 Yb1 Li2 C45 41.0(4) . . . . ? C23 Yb1 Li2 C45 172.9(3) . . . . ? C78 O9 Li3 N1 36.9(10) . . . . ? C75 O9 Li3 N1 -124.6(8) . . . . ? C78 O9 Li3 N3 -157.9(10) . . . . ? C75 O9 Li3 N3 40.6(15) . . . . ? C78 O9 Li3 C52 178.3(7) . . . . ? C75 O9 Li3 C52 16.8(10) . . . . ? C78 O9 Li3 C8 2.8(9) . . . . ? C75 O9 Li3 C8 -158.7(7) . . . . ? C78 O9 Li3 Yb1 71.5(16) . . . . ? C75 O9 Li3 Yb1 -90.0(15) . . . . ? C8 N1 Li3 O9 -78.0(6) . . . . ? C7 N1 Li3 O9 39.0(7) . . . . ? Yb1 N1 Li3 O9 164.3(5) . . . . ? C8 N1 Li3 N3 110.3(4) . . . . ? C7 N1 Li3 N3 -132.8(4) . . . . ? Yb1 N1 Li3 N3 -7.4(4) . . . . ? C8 N1 Li3 C52 141.0(5) . . . . ? C7 N1 Li3 C52 -102.1(5) . . . . ? Yb1 N1 Li3 C52 23.3(5) . . . . ? C7 N1 Li3 C8 116.9(4) . . . . ? Yb1 N1 Li3 C8 -117.7(3) . . . . ? C8 N1 Li3 Yb1 117.7(3) . . . . ? C7 N1 Li3 Yb1 -125.3(4) . . . . ? C52 N3 Li3 O9 -39.5(11) . . . . ? C51 N3 Li3 O9 77.4(12) . . . . ? Yb1 N3 Li3 O9 -159.2(11) . . . . ? C52 N3 Li3 N1 127.0(4) . . . . ? C51 N3 Li3 N1 -116.1(5) . . . . ? Yb1 N3 Li3 N1 7.3(4) . . . . ? C51 N3 Li3 C52 116.9(6) . . . . ? Yb1 N3 Li3 C52 -119.7(3) . . . . ? C52 N3 Li3 C8 160.2(5) . . . . ? C51 N3 Li3 C8 -82.9(6) . . . . ? Yb1 N3 Li3 C8 40.5(4) . . . . ? C52 N3 Li3 Yb1 119.7(3) . . . . ? C51 N3 Li3 Yb1 -123.4(5) . . . . ? C57 C52 Li3 O9 -67.4(6) . . . . ? N3 C52 Li3 O9 156.8(7) . . . . ? C53 C52 Li3 O9 45.0(9) . . . . ? C57 C52 Li3 N1 73.2(5) . . . . ? N3 C52 Li3 N1 -62.6(5) . . . . ? C53 C52 Li3 N1 -174.4(5) . . . . ? C57 C52 Li3 N3 135.8(5) . . . . ? C53 C52 Li3 N3 -111.8(7) . . . . ? C57 C52 Li3 C8 105.9(8) . . . . ? N3 C52 Li3 C8 -29.9(7) . . . . ? C53 C52 Li3 C8 -141.8(7) . . . . ? C57 C52 Li3 Yb1 91.5(3) . . . . ? N3 C52 Li3 Yb1 -44.3(3) . . . . ? C53 C52 Li3 Yb1 -156.2(6) . . . . ? N1 C8 Li3 O9 113.8(6) . . . . ? C13 C8 Li3 O9 -101.0(5) . . . . ? C9 C8 Li3 O9 8.5(11) . . . . ? C13 C8 Li3 N1 145.2(4) . . . . ? C9 C8 Li3 N1 -105.2(9) . . . . ? N1 C8 Li3 N3 -77.4(5) . . . . ? C13 C8 Li3 N3 67.8(5) . . . . ? C9 C8 Li3 N3 177.4(7) . . . . ? N1 C8 Li3 C52 -60.0(7) . . . . ? C13 C8 Li3 C52 85.2(8) . . . . ? C9 C8 Li3 C52 -165.2(7) . . . . ? N1 C8 Li3 Yb1 -45.4(2) . . . . ? C13 C8 Li3 Yb1 99.8(3) . . . . ? C9 C8 Li3 Yb1 -150.6(8) . . . . ? O5 Yb1 Li3 O9 -149.2(13) . . . . ? O1 Yb1 Li3 O9 25.6(13) . . . . ? O3 Yb1 Li3 O9 130.8(12) . . . . ? N1 Yb1 Li3 O9 -43.3(12) . . . . ? N3 Yb1 Li3 O9 146.3(15) . . . . ? N2 Yb1 Li3 O9 -46.5(16) . . . . ? Li2 Yb1 Li3 O9 177.4(12) . . . . ? Li1 Yb1 Li3 O9 3.2(15) . . . . ? C23 Yb1 Li3 O9 104.4(13) . . . . ? O5 Yb1 Li3 N1 -105.8(3) . . . . ? O1 Yb1 Li3 N1 68.9(3) . . . . ? O3 Yb1 Li3 N1 174.13(18) . . . . ? N3 Yb1 Li3 N1 -170.3(5) . . . . ? N2 Yb1 Li3 N1 -3.2(6) . . . . ? Li2 Yb1 Li3 N1 -139.2(3) . . . . ? Li1 Yb1 Li3 N1 46.5(4) . . . . ? C23 Yb1 Li3 N1 147.7(2) . . . . ? O5 Yb1 Li3 N3 64.5(3) . . . . ? O1 Yb1 Li3 N3 -120.7(3) . . . . ? O3 Yb1 Li3 N3 -15.5(4) . . . . ? N1 Yb1 Li3 N3 170.3(5) . . . . ? N2 Yb1 Li3 N3 167.2(3) . . . . ? Li2 Yb1 Li3 N3 31.1(4) . . . . ? Li1 Yb1 Li3 N3 -143.2(3) . . . . ? C23 Yb1 Li3 N3 -41.9(5) . . . . ? O5 Yb1 Li3 C52 95.9(3) . . . . ? O1 Yb1 Li3 C52 -89.3(3) . . . . ? O3 Yb1 Li3 C52 15.9(4) . . . . ? N1 Yb1 Li3 C52 -158.2(5) . . . . ? N3 Yb1 Li3 C52 31.4(2) . . . . ? N2 Yb1 Li3 C52 -161.4(3) . . . . ? Li2 Yb1 Li3 C52 62.5(4) . . . . ? Li1 Yb1 Li3 C52 -111.7(3) . . . . ? C23 Yb1 Li3 C52 -10.5(5) . . . . ? O5 Yb1 Li3 C8 -74.1(3) . . . . ? O1 Yb1 Li3 C8 100.6(2) . . . . ? O3 Yb1 Li3 C8 -154.16(18) . . . . ? N1 Yb1 Li3 C8 31.7(2) . . . . ? N3 Yb1 Li3 C8 -138.6(4) . . . . ? N2 Yb1 Li3 C8 28.6(6) . . . . ? Li2 Yb1 Li3 C8 -107.5(3) . . . . ? Li1 Yb1 Li3 C8 78.2(4) . . . . ? C23 Yb1 Li3 C8 179.45(19) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.051 _refine_diff_density_min -1.364 _refine_diff_density_rms 0.093 _database_code_depnum_ccdc_archive 'CCDC 932408'