# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 # Attachment '- Dalton.cif' # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Yingming Yao' _publ_contact_author_email yaoym@suda.edu.cn _publ_contact_author_fax 86-512-65880305 _publ_contact_author_phone 86-512-65882806 _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category FM _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and Characterization of Anionic Rare-Earth Metal Amides Stabilized by Phenoxy-Amido Ligands and Their Catalytic Behavior for the Polymerization of L-Lactide ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_address 'Min Lu' ; College of Chemistry, Chemical Engineering and Materials Science Dushu Lake Campus Soochow University Suzhou, 215123 P. R. China ; 'Yingming Yao' ; College of Chemistry, Chemical Engineering and Materials Science Dushu Lake Campus Soochow University Suzhou, 215123 P. R. China ; 'Yong Zhang' ; College of Chemistry, Chemical Engineering and Materials Science Dushu Lake Campus Soochow University Suzhou, 215123 P. R. China ; 'Qi Shen' ; College of Chemistry, Chemical Engineering and Materials Science Dushu Lake Campus Soochow University Suzhou, 215123 P. R. China ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2003). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.5.1. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #============================================================================== data_complex1 _database_code_depnum_ccdc_archive 'CCDC 767732' #TrackingRef '- Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H76 Li2 N2 O4, 2(C4 H8 O)' _chemical_formula_sum 'C60 H92 Li2 N2 O6' _chemical_formula_weight 951.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _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 10.552(2) _cell_length_b 10.813(2) _cell_length_c 13.658(3) _cell_angle_alpha 82.717(8) _cell_angle_beta 69.214(6) _cell_angle_gamma 80.185(8) _cell_volume 1432.0(5) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4332 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.103 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.808 _exptl_absorpt_correction_T_max 0.980 _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 10199 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5143 _reflns_number_gt 3506 _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^)+(0.1939P)^2^+0.6556P] 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 mix _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5143 _refine_ls_number_parameters 313 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1244 _refine_ls_R_factor_gt 0.0991 _refine_ls_wR_factor_ref 0.3331 _refine_ls_wR_factor_gt 0.3037 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.173 _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 O1 O 0.5276(3) 0.0935(2) 0.41519(18) 0.0372(7) Uani 1 1 d . . . O2 O 0.3676(3) -0.1426(3) 0.4048(2) 0.0596(9) Uani 1 1 d . . . O3 O 0.5955(5) 0.8485(4) 1.1059(3) 0.0886(13) Uani 1 1 d . . . N1 N 0.6990(3) -0.1402(3) 0.3109(2) 0.0341(7) Uani 1 1 d . . . H1 H 0.666(4) -0.129(4) 0.256(3) 0.039(11) Uiso 1 1 d . . . C1 C 0.5937(4) 0.1456(3) 0.3220(3) 0.0314(8) Uani 1 1 d . . . C2 C 0.5434(4) 0.2610(3) 0.2769(3) 0.0324(8) Uani 1 1 d . . . C3 C 0.6209(4) 0.3032(3) 0.1755(3) 0.0355(9) Uani 1 1 d . . . H3 H 0.5858 0.3784 0.1458 0.043 Uiso 1 1 calc R . . C4 C 0.7461(4) 0.2413(3) 0.1157(3) 0.0384(9) Uani 1 1 d . . . C5 C 0.7961(4) 0.1307(3) 0.1620(3) 0.0373(9) Uani 1 1 d . . . H5 H 0.8817 0.0875 0.1249 0.045 Uiso 1 1 calc R . . C6 C 0.7234(4) 0.0827(3) 0.2611(3) 0.0348(8) Uani 1 1 d . . . C7 C 0.7799(4) -0.0396(3) 0.3064(3) 0.0359(9) Uani 1 1 d . . . H7A H 0.8753 -0.0634 0.2629 0.043 Uiso 1 1 calc R . . H7B H 0.7775 -0.0288 0.3773 0.043 Uiso 1 1 calc R . . C8 C 0.7660(4) -0.2666(3) 0.3095(3) 0.0322(8) Uani 1 1 d . . . C9 C 0.7150(4) -0.3584(4) 0.2782(3) 0.0406(9) Uani 1 1 d . . . H9 H 0.6357 -0.3368 0.2600 0.049 Uiso 1 1 calc R . . C10 C 0.7781(4) -0.4805(4) 0.2733(3) 0.0418(9) Uani 1 1 d . . . H10 H 0.7414 -0.5406 0.2511 0.050 Uiso 1 1 calc R . . C11 C 0.8944(4) -0.5176(3) 0.3002(3) 0.0414(9) Uani 1 1 d . . . C12 C 0.9421(4) -0.4270(4) 0.3358(3) 0.0433(10) Uani 1 1 d . . . H12 H 1.0180 -0.4501 0.3581 0.052 Uiso 1 1 calc R . . C13 C 0.8804(4) -0.3024(3) 0.3393(3) 0.0372(9) Uani 1 1 d . . . H13 H 0.9165 -0.2423 0.3620 0.045 Uiso 1 1 calc R . . C14 C 0.4111(4) 0.3395(3) 0.3400(3) 0.0368(9) Uani 1 1 d . . . C15 C 0.3716(5) 0.4589(4) 0.2773(3) 0.0517(11) Uani 1 1 d . . . H15A H 0.2889 0.5063 0.3216 0.078 Uiso 1 1 calc R . . H15B H 0.3556 0.4355 0.2168 0.078 Uiso 1 1 calc R . . H15C H 0.4452 0.5103 0.2538 0.078 Uiso 1 1 calc R . . C16 C 0.4294(4) 0.3837(4) 0.4360(3) 0.0427(10) Uani 1 1 d . . . H16A H 0.4451 0.3112 0.4820 0.064 Uiso 1 1 calc R . . H16B H 0.3475 0.4377 0.4736 0.064 Uiso 1 1 calc R . . H16C H 0.5071 0.4300 0.4131 0.064 Uiso 1 1 calc R . . C17 C 0.2905(4) 0.2639(4) 0.3761(3) 0.0474(10) Uani 1 1 d . . . H17A H 0.3090 0.1903 0.4200 0.071 Uiso 1 1 calc R . . H17B H 0.2777 0.2376 0.3153 0.071 Uiso 1 1 calc R . . H17C H 0.2082 0.3159 0.4159 0.071 Uiso 1 1 calc R . . C18 C 0.8295(4) 0.2920(4) 0.0043(3) 0.0504(11) Uani 1 1 d D . . C19 C 0.8996(12) 0.1871(10) -0.0676(9) 0.071(2) Uiso 0.50 1 d PD . . C19' C 0.8334(13) 0.2019(11) -0.0759(9) 0.071(2) Uiso 0.50 1 d PD . . C20 C 0.9493(14) 0.3442(15) 0.0132(13) 0.092(3) Uiso 0.50 1 d PD . . C20' C 0.9786(13) 0.2978(15) -0.0063(13) 0.092(3) Uiso 0.50 1 d PD . . C21 C 0.7413(12) 0.3988(11) -0.0390(9) 0.071(2) Uiso 0.50 1 d PD . . C21' C 0.7756(12) 0.4283(10) -0.0225(10) 0.071(2) Uiso 0.50 1 d PD . . C22 C 0.9668(5) -0.6502(4) 0.2885(4) 0.0612(13) Uani 1 1 d . . . H22A H 1.0442 -0.6534 0.2235 0.092 Uiso 1 1 calc R . . H22B H 0.9041 -0.7055 0.2873 0.092 Uiso 1 1 calc R . . H22C H 0.9987 -0.6773 0.3472 0.092 Uiso 1 1 calc R . . C23 C 0.3197(11) -0.0704(12) 0.3216(9) 0.053(3) Uiso 0.50 1 d PD . . C23' C 0.3362(12) -0.1111(13) 0.3108(10) 0.065(4) Uiso 0.50 1 d PD . . C24 C 0.1713(12) -0.0823(12) 0.3631(10) 0.079(2) Uiso 0.50 1 d PD . . C24' C 0.1984(12) -0.1475(13) 0.3345(9) 0.079(2) Uiso 0.50 1 d PD . . C25 C 0.1606(13) -0.2062(12) 0.4262(10) 0.080(2) Uiso 0.50 1 d PD . . C25' C 0.1336(12) -0.1565(13) 0.4551(9) 0.080(2) Uiso 0.50 1 d PD . . C26 C 0.2819(11) -0.2352(11) 0.4642(9) 0.054(3) Uiso 0.50 1 d PD . . C26' C 0.2569(11) -0.1998(11) 0.4854(9) 0.051(3) Uiso 0.50 1 d PD . . C27 C 0.5941(12) 0.7484(8) 1.0526(6) 0.138(4) Uani 1 1 d . . . H27A H 0.5000 0.7303 1.0720 0.166 Uiso 1 1 calc R . . H27B H 0.6485 0.6733 1.0727 0.166 Uiso 1 1 calc R . . C28 C 0.6498(8) 0.7773(7) 0.9394(5) 0.097(2) Uani 1 1 d . . . H28A H 0.5781 0.7862 0.9080 0.117 Uiso 1 1 calc R . . H28B H 0.7226 0.7109 0.9060 0.117 Uiso 1 1 calc R . . C29 C 0.7041(8) 0.8968(7) 0.9273(5) 0.093(2) Uani 1 1 d . . . H29A H 0.6543 0.9637 0.8942 0.112 Uiso 1 1 calc R . . H29B H 0.8015 0.8884 0.8845 0.112 Uiso 1 1 calc R . . C30 C 0.6831(8) 0.9248(6) 1.0374(5) 0.0910(19) Uani 1 1 d . . . H30A H 0.7709 0.9099 1.0494 0.109 Uiso 1 1 calc R . . H30B H 0.6447 1.0132 1.0481 0.109 Uiso 1 1 calc R . . Li1 Li 0.5106(6) -0.0835(6) 0.4402(5) 0.0372(14) 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 O1 0.0447(15) 0.0350(14) 0.0249(13) 0.0042(10) -0.0057(11) -0.0054(11) O2 0.0538(18) 0.080(2) 0.0514(19) 0.0118(16) -0.0233(15) -0.0275(16) O3 0.126(4) 0.077(3) 0.051(2) -0.0035(19) -0.017(2) -0.013(2) N1 0.0361(17) 0.0321(16) 0.0335(17) 0.0015(12) -0.0127(14) -0.0042(13) C1 0.0348(19) 0.0317(18) 0.0255(17) 0.0004(14) -0.0065(15) -0.0087(14) C2 0.039(2) 0.0325(18) 0.0253(17) -0.0008(14) -0.0098(15) -0.0073(15) C3 0.046(2) 0.0290(18) 0.0296(19) 0.0018(14) -0.0112(17) -0.0063(15) C4 0.044(2) 0.035(2) 0.0291(19) 0.0005(15) -0.0045(17) -0.0074(16) C5 0.0352(19) 0.035(2) 0.034(2) -0.0033(15) -0.0019(16) -0.0049(15) C6 0.037(2) 0.0312(19) 0.035(2) 0.0019(15) -0.0106(16) -0.0067(15) C7 0.0349(19) 0.0315(19) 0.039(2) 0.0009(15) -0.0108(17) -0.0051(15) C8 0.0349(19) 0.0314(18) 0.0248(17) 0.0007(13) -0.0045(15) -0.0041(14) C9 0.039(2) 0.044(2) 0.041(2) -0.0048(17) -0.0152(18) -0.0055(17) C10 0.043(2) 0.039(2) 0.041(2) -0.0068(16) -0.0089(18) -0.0085(17) C11 0.042(2) 0.034(2) 0.039(2) 0.0017(16) -0.0049(18) -0.0051(16) C12 0.037(2) 0.045(2) 0.044(2) 0.0027(17) -0.0136(18) -0.0020(17) C13 0.037(2) 0.036(2) 0.040(2) -0.0017(15) -0.0143(17) -0.0054(15) C14 0.039(2) 0.038(2) 0.0294(19) -0.0018(15) -0.0097(16) 0.0003(16) C15 0.053(2) 0.044(2) 0.049(2) 0.0008(19) -0.014(2) 0.0077(19) C16 0.048(2) 0.043(2) 0.032(2) -0.0079(16) -0.0070(18) -0.0022(18) C17 0.039(2) 0.055(3) 0.045(2) -0.0016(19) -0.0125(19) -0.0056(18) C18 0.060(3) 0.041(2) 0.033(2) 0.0045(17) 0.003(2) -0.0090(19) C22 0.063(3) 0.040(2) 0.072(3) -0.003(2) -0.017(3) 0.004(2) C27 0.242(11) 0.093(6) 0.075(5) -0.005(4) -0.030(6) -0.067(7) C28 0.134(6) 0.093(5) 0.069(4) -0.015(3) -0.036(4) -0.019(4) C29 0.120(5) 0.100(5) 0.059(4) 0.009(3) -0.032(4) -0.024(4) C30 0.122(5) 0.085(4) 0.071(4) -0.007(3) -0.037(4) -0.020(4) Li1 0.042(3) 0.037(3) 0.030(3) 0.001(2) -0.009(3) -0.011(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 O1 C1 1.322(4) . ? O1 Li1 1.864(6) 2_656 ? O1 Li1 1.929(7) . ? O2 C23' 1.423(13) . ? O2 C26 1.435(11) . ? O2 C26' 1.456(11) . ? O2 C23 1.485(12) . ? O2 Li1 1.960(7) . ? O3 C30 1.364(7) . ? O3 C27 1.384(8) . ? N1 C8 1.427(4) . ? N1 C7 1.476(5) . ? N1 Li1 2.193(7) . ? N1 H1 0.92(4) . ? C1 C2 1.425(5) . ? C1 C6 1.430(5) . ? C2 C3 1.399(5) . ? C2 C14 1.530(5) . ? C3 C4 1.390(5) . ? C3 H3 0.9400 . ? C4 C5 1.392(5) . ? C4 C18 1.546(5) . ? C5 C6 1.382(5) . ? C5 H5 0.9400 . ? C6 C7 1.507(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.382(5) . ? C8 C13 1.387(5) . ? C9 C10 1.372(5) . ? C9 H9 0.9400 . ? C10 C11 1.384(6) . ? C10 H10 0.9400 . ? C11 C12 1.383(6) . ? C11 C22 1.504(6) . ? C12 C13 1.391(5) . ? C12 H12 0.9400 . ? C13 H13 0.9400 . ? C14 C17 1.529(6) . ? C14 C16 1.534(5) . ? C14 C15 1.538(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? 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 C19 1.509(11) . ? C18 C20 1.517(13) . ? C18 C21' 1.535(11) . ? C18 C20' 1.539(13) . ? C18 C19' 1.541(11) . ? C18 C21 1.550(11) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 C24 1.487(13) . ? C23' C24' 1.484(14) . ? C24 C25 1.497(14) . ? C24' C25' 1.541(14) . ? C25 C26 1.517(13) . ? C25' C26' 1.485(13) . ? C27 C28 1.459(9) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.469(9) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.502(8) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? Li1 O1 1.864(6) 2_656 ? Li1 Li1 2.517(12) 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 C1 O1 Li1 147.5(3) . 2_656 ? C1 O1 Li1 122.9(3) . . ? Li1 O1 Li1 83.2(3) 2_656 . ? C23' O2 C26 106.1(7) . . ? C23' O2 C26' 110.3(6) . . ? C26 O2 C26' 19.5(6) . . ? C23' O2 C23 18.3(6) . . ? C26 O2 C23 113.1(6) . . ? C26' O2 C23 111.0(6) . . ? C23' O2 Li1 127.0(5) . . ? C26 O2 Li1 126.8(5) . . ? C26' O2 Li1 121.0(5) . . ? C23 O2 Li1 118.9(5) . . ? C30 O3 C27 107.9(5) . . ? C8 N1 C7 117.2(3) . . ? C8 N1 Li1 120.6(3) . . ? C7 N1 Li1 100.7(3) . . ? C8 N1 H1 106(3) . . ? C7 N1 H1 111(2) . . ? Li1 N1 H1 100(2) . . ? O1 C1 C2 124.2(3) . . ? O1 C1 C6 118.6(3) . . ? C2 C1 C6 117.2(3) . . ? C3 C2 C1 118.4(3) . . ? C3 C2 C14 121.0(3) . . ? C1 C2 C14 120.5(3) . . ? C4 C3 C2 124.5(3) . . ? C4 C3 H3 117.8 . . ? C2 C3 H3 117.8 . . ? C3 C4 C5 116.5(3) . . ? C3 C4 C18 122.9(3) . . ? C5 C4 C18 120.6(3) . . ? C6 C5 C4 121.9(3) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C1 121.5(3) . . ? C5 C6 C7 119.9(3) . . ? C1 C6 C7 118.6(3) . . ? N1 C7 C6 110.5(3) . . ? N1 C7 H7A 109.5 . . ? C6 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C9 C8 C13 118.0(3) . . ? C9 C8 N1 119.3(3) . . ? C13 C8 N1 122.8(3) . . ? C10 C9 C8 121.2(4) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 121.8(4) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C12 C11 C10 117.1(4) . . ? C12 C11 C22 121.9(4) . . ? C10 C11 C22 121.0(4) . . ? C11 C12 C13 121.6(4) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C8 C13 C12 120.3(4) . . ? C8 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C17 C14 C2 111.3(3) . . ? C17 C14 C16 109.5(3) . . ? C2 C14 C16 109.5(3) . . ? C17 C14 C15 106.9(3) . . ? C2 C14 C15 112.9(3) . . ? C16 C14 C15 106.5(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C20 102.5(8) . . ? C19 C18 C21' 129.2(7) . . ? C20 C18 C21' 86.6(8) . . ? C19 C18 C20' 81.0(8) . . ? C20 C18 C20' 22.0(8) . . ? C21' C18 C20' 103.8(8) . . ? C19 C18 C19' 27.9(5) . . ? C20 C18 C19' 127.4(8) . . ? C21' C18 C19' 112.2(7) . . ? C20' C18 C19' 107.2(8) . . ? C19 C18 C4 111.8(5) . . ? C20 C18 C4 107.2(7) . . ? C21' C18 C4 112.7(6) . . ? C20' C18 C4 111.7(7) . . ? C19' C18 C4 109.0(5) . . ? C19 C18 C21 114.8(7) . . ? C20 C18 C21 109.0(8) . . ? C21' C18 C21 23.6(6) . . ? C20' C18 C21 123.4(8) . . ? C19' C18 C21 92.1(7) . . ? C4 C18 C21 110.9(5) . . ? C11 C22 H22A 109.5 . . ? C11 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C11 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O2 C23 C24 101.9(8) . . ? O2 C23' C24' 105.7(9) . . ? C23 C24 C25 105.3(10) . . ? C23' C24' C25' 105.7(10) . . ? C24 C25 C26 107.5(10) . . ? C26' C25' C24' 100.8(10) . . ? O2 C26 C25 103.0(8) . . ? O2 C26' C25' 105.6(8) . . ? O3 C27 C28 110.5(6) . . ? O3 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? O3 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C27 C28 C29 104.8(6) . . ? C27 C28 H28A 110.8 . . ? C29 C28 H28A 110.8 . . ? C27 C28 H28B 110.8 . . ? C29 C28 H28B 110.8 . . ? H28A C28 H28B 108.9 . . ? C28 C29 C30 104.6(5) . . ? C28 C29 H29A 110.8 . . ? C30 C29 H29A 110.8 . . ? C28 C29 H29B 110.8 . . ? C30 C29 H29B 110.8 . . ? H29A C29 H29B 108.9 . . ? O3 C30 C29 108.7(5) . . ? O3 C30 H30A 110.0 . . ? C29 C30 H30A 110.0 . . ? O3 C30 H30B 110.0 . . ? C29 C30 H30B 110.0 . . ? H30A C30 H30B 108.3 . . ? O1 Li1 O1 96.8(3) 2_656 . ? O1 Li1 O2 111.7(3) 2_656 . ? O1 Li1 O2 118.1(3) . . ? O1 Li1 N1 131.3(3) 2_656 . ? O1 Li1 N1 94.6(3) . . ? O2 Li1 N1 103.8(3) . . ? O1 Li1 Li1 49.5(2) 2_656 2_656 ? O1 Li1 Li1 47.3(2) . 2_656 ? O2 Li1 Li1 129.3(4) . 2_656 ? N1 Li1 Li1 123.4(4) . 2_656 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.798 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.075 #===================================================end data_complex2 _database_code_depnum_ccdc_archive 'CCDC 767733' #TrackingRef '- Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H92 Li2 N3 Nd O4 Si2' _chemical_formula_sum 'C58 H92 Li2 N3 Nd O4 Si2' _chemical_formula_weight 1109.65 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' Nd Nd -0.1943 3.0179 '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' _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 21.635(4) _cell_length_b 21.635(4) _cell_length_c 26.662(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12479(4) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10275 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4696 _exptl_absorpt_coefficient_mu 0.913 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.612 _exptl_absorpt_correction_T_max 0.833 _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 12516 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4165 _reflns_number_gt 3423 _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^)+(0.0243P)^2^+44.7719P] 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 0.09(4) _refine_ls_number_reflns 4165 _refine_ls_number_parameters 299 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0731 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1064 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 1.176 _refine_ls_restrained_S_all 1.177 _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 Nd1 Nd 0.5000 1.0000 0.46372(8) 0.03144(13) Uani 1 2 d S . . Si1 Si 0.56770(12) 0.98340(12) 0.34556(9) 0.0528(6) Uani 1 1 d . . . O1 O 0.5059(2) 0.8984(2) 0.49238(18) 0.0337(11) Uani 1 1 d . . . O2 O 0.4231(3) 0.8654(3) 0.5953(3) 0.083(2) Uani 1 1 d D . . N1 N 0.5893(3) 1.0081(3) 0.5184(2) 0.0384(15) Uani 1 1 d . . . N2 N 0.5000 1.0000 0.3766(3) 0.042(2) Uani 1 2 d S . . C1 C 0.5571(3) 0.8661(3) 0.5047(2) 0.0247(15) Uani 1 1 d . . . C2 C 0.5677(3) 0.8063(3) 0.4862(3) 0.0332(17) Uani 1 1 d . . . C3 C 0.6224(4) 0.7773(3) 0.5004(3) 0.044(2) Uani 1 1 d . . . H3 H 0.6306 0.7379 0.4870 0.053 Uiso 1 1 calc R . . C4 C 0.6663(4) 0.8027(4) 0.5335(3) 0.0414(19) Uani 1 1 d . . . C5 C 0.6531(4) 0.8616(3) 0.5503(3) 0.042(2) Uani 1 1 d . . . H5 H 0.6814 0.8812 0.5718 0.050 Uiso 1 1 calc R . . C6 C 0.6002(3) 0.8928(3) 0.5369(3) 0.0342(17) Uani 1 1 d . . . C7 C 0.5875(4) 0.9585(3) 0.5565(3) 0.0390(19) Uani 1 1 d . . . H7A H 0.5467 0.9589 0.5724 0.047 Uiso 1 1 calc R . . H7B H 0.6181 0.9681 0.5825 0.047 Uiso 1 1 calc R . . C8 C 0.6472(4) 1.0282(3) 0.5037(3) 0.042(2) Uani 1 1 d . . . C9 C 0.6498(4) 1.0735(3) 0.4662(4) 0.057(2) Uani 1 1 d . . . H9 H 0.6125 1.0897 0.4537 0.069 Uiso 1 1 calc R . . C10 C 0.7044(5) 1.0954(4) 0.4469(4) 0.069(3) Uani 1 1 d . . . H10 H 0.7032 1.1244 0.4206 0.083 Uiso 1 1 calc R . . C11 C 0.7607(4) 1.0764(4) 0.4647(5) 0.066(3) Uani 1 1 d . . . C12 C 0.7587(4) 1.0343(4) 0.5026(4) 0.058(3) Uani 1 1 d . . . H12 H 0.7965 1.0210 0.5163 0.070 Uiso 1 1 calc R . . C13 C 0.7046(4) 1.0098(3) 0.5225(4) 0.044(2) Uani 1 1 d . . . H13 H 0.7066 0.9807 0.5486 0.053 Uiso 1 1 calc R . . C14 C 0.8217(4) 1.0985(5) 0.4430(4) 0.083(3) Uani 1 1 d . . . H14A H 0.8551 1.0738 0.4566 0.125 Uiso 1 1 calc R . . H14B H 0.8280 1.1415 0.4518 0.125 Uiso 1 1 calc R . . H14C H 0.8209 1.0943 0.4068 0.125 Uiso 1 1 calc R . . C15 C 0.5213(4) 0.7732(4) 0.4508(3) 0.046(2) Uani 1 1 d . . . C16 C 0.5430(4) 0.7080(3) 0.4357(4) 0.054(2) Uani 1 1 d . . . H16A H 0.5825 0.7109 0.4186 0.081 Uiso 1 1 calc R . . H16B H 0.5128 0.6895 0.4134 0.081 Uiso 1 1 calc R . . H16C H 0.5474 0.6827 0.4654 0.081 Uiso 1 1 calc R . . C17 C 0.4596(4) 0.7648(4) 0.4784(3) 0.060(3) Uani 1 1 d . . . H17A H 0.4327 0.7383 0.4587 0.090 Uiso 1 1 calc R . . H17B H 0.4401 0.8047 0.4830 0.090 Uiso 1 1 calc R . . H17C H 0.4670 0.7459 0.5108 0.090 Uiso 1 1 calc R . . C18 C 0.5118(4) 0.8094(4) 0.4031(3) 0.058(3) Uani 1 1 d . . . H18A H 0.5501 0.8105 0.3842 0.087 Uiso 1 1 calc R . . H18B H 0.4992 0.8512 0.4113 0.087 Uiso 1 1 calc R . . H18C H 0.4799 0.7897 0.3831 0.087 Uiso 1 1 calc R . . C19 C 0.7261(5) 0.7683(5) 0.5468(5) 0.091(2) Uani 1 1 d . . . C20 C 0.7612(5) 0.7565(5) 0.4968(4) 0.091(2) Uani 1 1 d . . . H20A H 0.7673 0.7954 0.4794 0.137 Uiso 1 1 calc R . . H20B H 0.7371 0.7289 0.4758 0.137 Uiso 1 1 calc R . . H20C H 0.8009 0.7378 0.5039 0.137 Uiso 1 1 calc R . . C21 C 0.7696(4) 0.8042(5) 0.5779(5) 0.091(2) Uani 1 1 d . . . H21A H 0.7546 0.8055 0.6122 0.137 Uiso 1 1 calc R . . H21B H 0.7727 0.8459 0.5649 0.137 Uiso 1 1 calc R . . H21C H 0.8099 0.7847 0.5771 0.137 Uiso 1 1 calc R . . C22 C 0.7130(5) 0.7061(5) 0.5689(5) 0.091(2) Uani 1 1 d . . . H22A H 0.7512 0.6828 0.5713 0.137 Uiso 1 1 calc R . . H22B H 0.6841 0.6841 0.5476 0.137 Uiso 1 1 calc R . . H22C H 0.6953 0.7111 0.6020 0.137 Uiso 1 1 calc R . . C23 C 0.5589(5) 0.9299(5) 0.2900(4) 0.090(4) Uani 1 1 d . . . H23A H 0.5297 0.9476 0.2664 0.134 Uiso 1 1 calc R . . H23B H 0.5438 0.8901 0.3013 0.134 Uiso 1 1 calc R . . H23C H 0.5986 0.9246 0.2737 0.134 Uiso 1 1 calc R . . C24 C 0.6087(5) 1.0552(5) 0.3215(4) 0.081(3) Uani 1 1 d . . . H24A H 0.6116 1.0854 0.3483 0.121 Uiso 1 1 calc R . . H24B H 0.5855 1.0726 0.2938 0.121 Uiso 1 1 calc R . . H24C H 0.6499 1.0442 0.3103 0.121 Uiso 1 1 calc R . . C25 C 0.6226(4) 0.9431(4) 0.3889(4) 0.063(3) Uani 1 1 d . . . H25A H 0.6022 0.9076 0.4039 0.094 Uiso 1 1 calc R . . H25B H 0.6355 0.9713 0.4151 0.094 Uiso 1 1 calc R . . H25C H 0.6585 0.9293 0.3702 0.094 Uiso 1 1 calc R . . C26 C 0.4311(10) 0.7997(7) 0.6096(8) 0.074(2) Uiso 0.50 1 d PD A 1 H26A H 0.4120 0.7728 0.5844 0.089 Uiso 0.50 1 calc PR A 1 H26B H 0.4752 0.7896 0.6118 0.089 Uiso 0.50 1 calc PR A 1 C26' C 0.4512(9) 0.8135(9) 0.6200(7) 0.074(2) Uiso 0.50 1 d PD A 2 H26C H 0.4958 0.8199 0.6241 0.089 Uiso 0.50 1 calc PR A 2 H26D H 0.4443 0.7753 0.6011 0.089 Uiso 0.50 1 calc PR A 2 C27 C 0.4010(10) 0.7911(8) 0.6589(8) 0.074(2) Uiso 0.50 1 d PD A 1 H27A H 0.4302 0.7743 0.6834 0.089 Uiso 0.50 1 calc PR A 1 H27B H 0.3657 0.7628 0.6561 0.089 Uiso 0.50 1 calc PR A 1 C27' C 0.4200(9) 0.8115(10) 0.6689(8) 0.074(2) Uiso 0.50 1 d PD A 2 H27C H 0.4455 0.8321 0.6942 0.089 Uiso 0.50 1 calc PR A 2 H27D H 0.4141 0.7684 0.6792 0.089 Uiso 0.50 1 calc PR A 2 C28 C 0.3798(10) 0.8546(8) 0.6742(8) 0.074(2) Uiso 0.50 1 d PD A 1 H28A H 0.3348 0.8545 0.6785 0.089 Uiso 0.50 1 calc PR A 1 H28B H 0.3985 0.8656 0.7064 0.089 Uiso 0.50 1 calc PR A 1 C28' C 0.3569(8) 0.8441(9) 0.6647(8) 0.074(2) Uiso 0.50 1 d PD A 2 H28C H 0.3241 0.8154 0.6546 0.089 Uiso 0.50 1 calc PR A 2 H28D H 0.3453 0.8645 0.6962 0.089 Uiso 0.50 1 calc PR A 2 C29 C 0.3968(10) 0.9004(9) 0.6368(7) 0.074(2) Uiso 0.50 1 d PD A 1 H29A H 0.4272 0.9295 0.6504 0.089 Uiso 0.50 1 calc PR A 1 H29B H 0.3604 0.9237 0.6257 0.089 Uiso 0.50 1 calc PR A 1 C29' C 0.3711(8) 0.8888(9) 0.6252(7) 0.074(2) Uiso 0.50 1 d PD A 2 H29C H 0.3820 0.9287 0.6401 0.089 Uiso 0.50 1 calc PR A 2 H29D H 0.3349 0.8947 0.6037 0.089 Uiso 0.50 1 calc PR A 2 Li1 Li 0.4373(8) 0.9026(6) 0.5356(6) 0.056(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0276(3) 0.0338(3) 0.0328(2) 0.000 0.000 0.0008(3) Si1 0.0593(15) 0.0615(16) 0.0377(12) -0.0081(13) 0.0136(12) -0.0111(14) O1 0.034(3) 0.023(2) 0.044(3) 0.002(2) -0.007(2) 0.002(2) O2 0.113(6) 0.064(4) 0.072(5) 0.016(4) 0.050(4) 0.025(4) N1 0.035(3) 0.028(3) 0.051(4) -0.005(3) -0.013(3) -0.002(3) N2 0.040(5) 0.046(5) 0.039(5) 0.000 0.000 -0.001(5) C1 0.025(4) 0.030(4) 0.019(3) -0.001(3) -0.004(3) 0.005(3) C2 0.032(4) 0.031(4) 0.037(4) 0.005(3) -0.003(3) 0.000(3) C3 0.049(5) 0.028(4) 0.055(5) -0.008(4) -0.004(4) 0.005(4) C4 0.041(4) 0.040(4) 0.044(5) 0.003(4) -0.006(4) 0.007(4) C5 0.046(5) 0.043(5) 0.036(4) -0.003(4) -0.013(4) -0.002(4) C6 0.040(4) 0.034(4) 0.029(4) 0.010(3) 0.000(3) 0.002(3) C7 0.042(5) 0.034(4) 0.041(5) -0.005(4) -0.008(4) -0.002(4) C8 0.054(5) 0.030(4) 0.042(5) -0.022(4) -0.016(4) 0.005(4) C9 0.051(5) 0.037(4) 0.083(7) 0.010(5) -0.033(6) -0.003(4) C10 0.077(7) 0.057(6) 0.075(8) 0.012(5) -0.022(6) -0.034(5) C11 0.056(6) 0.063(6) 0.079(7) -0.007(7) -0.006(7) -0.022(5) C12 0.036(5) 0.053(6) 0.086(8) -0.026(5) -0.017(5) -0.003(4) C13 0.042(5) 0.032(5) 0.058(6) -0.006(4) -0.020(4) 0.007(4) C14 0.074(7) 0.071(7) 0.104(10) -0.006(6) 0.018(7) -0.023(6) C15 0.048(5) 0.038(4) 0.051(6) -0.008(4) -0.002(4) 0.006(4) C16 0.052(5) 0.032(4) 0.077(7) -0.021(5) -0.006(5) -0.001(4) C17 0.058(6) 0.044(5) 0.077(8) -0.017(5) -0.001(5) -0.015(4) C18 0.062(6) 0.065(6) 0.046(6) -0.004(5) -0.016(5) 0.005(5) C19 0.058(4) 0.080(4) 0.136(6) 0.005(4) -0.029(3) 0.023(3) C20 0.058(4) 0.080(4) 0.136(6) 0.005(4) -0.029(3) 0.023(3) C21 0.058(4) 0.080(4) 0.136(6) 0.005(4) -0.029(3) 0.023(3) C22 0.058(4) 0.080(4) 0.136(6) 0.005(4) -0.029(3) 0.023(3) C23 0.099(9) 0.125(10) 0.045(6) -0.034(7) 0.014(6) -0.005(8) C24 0.080(8) 0.094(8) 0.068(7) 0.017(6) 0.028(6) -0.021(6) C25 0.050(6) 0.066(6) 0.073(7) -0.005(5) 0.008(5) -0.004(5) Li1 0.076(11) 0.023(7) 0.070(11) 0.024(7) 0.034(9) 0.006(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 Nd1 N2 2.324(9) . ? Nd1 O1 2.330(4) . ? Nd1 O1 2.330(4) 11_564 ? Nd1 N1 2.426(6) 11_564 ? Nd1 N1 2.426(6) . ? Nd1 Li1 3.154(13) 11_564 ? Nd1 Li1 3.154(12) . ? Si1 N2 1.720(5) . ? Si1 C25 1.873(9) . ? Si1 C23 1.890(9) . ? Si1 C24 1.900(10) . ? O1 C1 1.350(7) . ? O1 Li1 1.882(15) . ? O2 C26' 1.436(15) . ? O2 C29 1.457(15) . ? O2 C29' 1.468(15) . ? O2 C26 1.480(15) . ? O2 Li1 1.811(15) . ? N1 C8 1.385(10) . ? N1 C7 1.476(9) . ? N1 Li1 2.067(14) 11_564 ? N2 Si1 1.720(5) 11_564 ? C1 C6 1.393(9) . ? C1 C2 1.406(9) . ? C2 C3 1.391(10) . ? C2 C15 1.553(10) . ? C3 C4 1.408(11) . ? C3 H3 0.9400 . ? C4 C5 1.380(10) . ? C4 C19 1.534(12) . ? C5 C6 1.375(10) . ? C5 H5 0.9400 . ? C6 C7 1.539(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C13 1.396(10) . ? C8 C9 1.402(11) . ? C8 Li1 2.511(17) 11_564 ? C9 C10 1.373(12) . ? C9 Li1 2.69(2) 11_564 ? C9 H9 0.9400 . ? C10 C11 1.369(12) . ? C10 H10 0.9400 . ? C11 C12 1.361(13) . ? C11 C14 1.519(12) . ? C12 C13 1.390(12) . ? C12 H12 0.9400 . ? C13 H13 0.9400 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 C18 1.506(11) . ? C15 C17 1.535(11) . ? C15 C16 1.540(10) . ? 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 C21 1.475(14) . ? C19 C22 1.496(15) . ? C19 C20 1.555(16) . ? 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 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 C27 1.480(16) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26' C27' 1.468(17) . ? C26' H26C 0.9800 . ? C26' H26D 0.9800 . ? C27 C28 1.505(17) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27' C28' 1.541(17) . ? C27' H27C 0.9800 . ? C27' H27D 0.9800 . ? C28 C29 1.454(17) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28' C29' 1.464(17) . ? C28' H28C 0.9800 . ? C28' H28D 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29' H29C 0.9800 . ? C29' H29D 0.9800 . ? Li1 N1 2.067(14) 11_564 ? Li1 C8 2.511(17) 11_564 ? Li1 C9 2.69(2) 11_564 ? 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 N2 Nd1 O1 109.14(13) . . ? N2 Nd1 O1 109.14(13) . 11_564 ? O1 Nd1 O1 141.7(3) . 11_564 ? N2 Nd1 N1 126.96(16) . 11_564 ? O1 Nd1 N1 77.22(19) . 11_564 ? O1 Nd1 N1 80.04(19) 11_564 11_564 ? N2 Nd1 N1 126.96(16) . . ? O1 Nd1 N1 80.04(19) . . ? O1 Nd1 N1 77.22(19) 11_564 . ? N1 Nd1 N1 106.1(3) 11_564 . ? N2 Nd1 Li1 127.4(3) . 11_564 ? O1 Nd1 Li1 114.0(3) . 11_564 ? O1 Nd1 Li1 36.4(3) 11_564 11_564 ? N1 Nd1 Li1 91.5(4) 11_564 11_564 ? N1 Nd1 Li1 40.9(3) . 11_564 ? N2 Nd1 Li1 127.4(3) . . ? O1 Nd1 Li1 36.4(3) . . ? O1 Nd1 Li1 114.0(3) 11_564 . ? N1 Nd1 Li1 40.9(3) 11_564 . ? N1 Nd1 Li1 91.5(4) . . ? Li1 Nd1 Li1 105.2(6) 11_564 . ? N2 Si1 C25 109.9(4) . . ? N2 Si1 C23 114.8(4) . . ? C25 Si1 C23 105.2(5) . . ? N2 Si1 C24 112.9(4) . . ? C25 Si1 C24 107.1(5) . . ? C23 Si1 C24 106.5(5) . . ? C1 O1 Li1 121.6(6) . . ? C1 O1 Nd1 127.8(4) . . ? Li1 O1 Nd1 96.4(4) . . ? C26' O2 C29 103.0(13) . . ? C26' O2 C29' 110.2(12) . . ? C29 O2 C29' 27.0(12) . . ? C26' O2 C26 23.5(12) . . ? C29 O2 C26 110.5(12) . . ? C29' O2 C26 106.3(12) . . ? C26' O2 Li1 132.7(10) . . ? C29 O2 Li1 120.1(10) . . ? C29' O2 Li1 117.0(10) . . ? C26 O2 Li1 129.3(10) . . ? C8 N1 C7 116.6(6) . . ? C8 N1 Li1 91.1(6) . 11_564 ? C7 N1 Li1 121.3(7) . 11_564 ? C8 N1 Nd1 124.9(5) . . ? C7 N1 Nd1 109.9(4) . . ? Li1 N1 Nd1 88.8(5) 11_564 . ? Si1 N2 Si1 122.6(6) 11_564 . ? Si1 N2 Nd1 118.7(3) 11_564 . ? Si1 N2 Nd1 118.7(3) . . ? O1 C1 C6 119.0(6) . . ? O1 C1 C2 121.7(6) . . ? C6 C1 C2 119.3(6) . . ? C3 C2 C1 117.3(6) . . ? C3 C2 C15 120.6(7) . . ? C1 C2 C15 122.1(6) . . ? C2 C3 C4 124.6(7) . . ? C2 C3 H3 117.7 . . ? C4 C3 H3 117.7 . . ? C5 C4 C3 115.1(7) . . ? C5 C4 C19 123.2(8) . . ? C3 C4 C19 121.6(8) . . ? C6 C5 C4 122.8(7) . . ? C6 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C5 C6 C1 120.9(7) . . ? C5 C6 C7 120.9(7) . . ? C1 C6 C7 118.2(6) . . ? N1 C7 C6 115.6(6) . . ? N1 C7 H7A 108.4 . . ? C6 C7 H7A 108.4 . . ? N1 C7 H7B 108.4 . . ? C6 C7 H7B 108.4 . . ? H7A C7 H7B 107.4 . . ? N1 C8 C13 127.8(8) . . ? N1 C8 C9 117.4(7) . . ? C13 C8 C9 114.8(8) . . ? N1 C8 Li1 55.4(5) . 11_564 ? C13 C8 Li1 134.1(6) . 11_564 ? C9 C8 Li1 81.6(6) . 11_564 ? C10 C9 C8 122.9(8) . . ? C10 C9 Li1 142.6(7) . 11_564 ? C8 C9 Li1 67.4(6) . 11_564 ? C10 C9 H9 118.5 . . ? C8 C9 H9 118.5 . . ? Li1 C9 H9 64.6 11_564 . ? C11 C10 C9 122.1(9) . . ? C11 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? C12 C11 C10 115.5(9) . . ? C12 C11 C14 121.3(9) . . ? C10 C11 C14 123.1(10) . . ? C11 C12 C13 124.3(9) . . ? C11 C12 H12 117.8 . . ? C13 C12 H12 117.8 . . ? C12 C13 C8 120.2(9) . . ? C12 C13 H13 119.9 . . ? C8 C13 H13 119.9 . . ? 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 . . ? C18 C15 C17 110.3(7) . . ? C18 C15 C16 107.3(7) . . ? C17 C15 C16 106.4(7) . . ? C18 C15 C2 111.2(7) . . ? C17 C15 C2 109.0(6) . . ? C16 C15 C2 112.5(6) . . ? 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 . . ? C21 C19 C22 111.9(11) . . ? C21 C19 C4 114.4(9) . . ? C22 C19 C4 111.6(9) . . ? C21 C19 C20 104.9(10) . . ? C22 C19 C20 106.4(10) . . ? C4 C19 C20 107.0(9) . . ? 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 . . ? 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 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 O2 107.4(14) . . ? C27 C26 H26A 110.2 . . ? O2 C26 H26A 110.2 . . ? C27 C26 H26B 110.2 . . ? O2 C26 H26B 110.2 . . ? H26A C26 H26B 108.5 . . ? O2 C26' C27' 103.6(15) . . ? O2 C26' H26C 111.0 . . ? C27' C26' H26C 111.0 . . ? O2 C26' H26D 111.0 . . ? C27' C26' H26D 111.0 . . ? H26C C26' H26D 109.0 . . ? C26 C27 C28 105.0(16) . . ? C26 C27 H27A 110.8 . . ? C28 C27 H27A 110.8 . . ? C26 C27 H27B 110.8 . . ? C28 C27 H27B 110.8 . . ? H27A C27 H27B 108.8 . . ? C26' C27' C28' 109.3(17) . . ? C26' C27' H27C 109.8 . . ? C28' C27' H27C 109.8 . . ? C26' C27' H27D 109.8 . . ? C28' C27' H27D 109.8 . . ? H27C C27' H27D 108.3 . . ? C29 C28 C27 111.1(18) . . ? C29 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? C29 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C29' C28' C27' 99.6(16) . . ? C29' C28' H28C 111.9 . . ? C27' C28' H28C 111.9 . . ? C29' C28' H28D 111.9 . . ? C27' C28' H28D 111.9 . . ? H28C C28' H28D 109.6 . . ? C28 C29 O2 105.3(15) . . ? C28 C29 H29A 110.7 . . ? O2 C29 H29A 110.7 . . ? C28 C29 H29B 110.7 . . ? O2 C29 H29B 110.7 . . ? H29A C29 H29B 108.8 . . ? C28' C29' O2 108.9(15) . . ? C28' C29' H29C 109.9 . . ? O2 C29' H29C 109.9 . . ? C28' C29' H29D 109.9 . . ? O2 C29' H29D 109.9 . . ? H29C C29' H29D 108.3 . . ? O2 Li1 O1 130.6(9) . . ? O2 Li1 N1 124.3(8) . 11_564 ? O1 Li1 N1 97.4(6) . 11_564 ? O2 Li1 C8 116.1(8) . 11_564 ? O1 Li1 C8 113.3(7) . 11_564 ? N1 Li1 C8 33.5(3) 11_564 11_564 ? O2 Li1 C9 124.9(8) . 11_564 ? O1 Li1 C9 98.1(7) . 11_564 ? N1 Li1 C9 58.3(5) 11_564 11_564 ? C8 Li1 C9 31.0(3) 11_564 11_564 ? O2 Li1 Nd1 154.7(9) . . ? O1 Li1 Nd1 47.2(3) . . ? N1 Li1 Nd1 50.3(3) 11_564 . ? C8 Li1 Nd1 73.1(3) 11_564 . ? C9 Li1 Nd1 75.8(4) 11_564 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.610 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.062 #===================================================end data_complex3 _database_code_depnum_ccdc_archive 'CCDC 767734' #TrackingRef '- Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H92 Li2 N3 O4 Si2 Sm' _chemical_formula_sum 'C58 H92 Li2 N3 O4 Si2 Sm' _chemical_formula_weight 1115.76 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' Sm Sm -0.1638 3.4418 '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 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 21.5715(19) _cell_length_b 21.5715(19) _cell_length_c 26.577(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12367(2) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 14330 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4712 _exptl_absorpt_coefficient_mu 1.031 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.561 _exptl_absorpt_correction_T_max 0.797 _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 17634 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4937 _reflns_number_gt 3796 _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^)+(0.0000P)^2^+43.6343P] 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 0.00(3) _refine_ls_number_reflns 4937 _refine_ls_number_parameters 316 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1011 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 1.171 _refine_ls_restrained_S_all 1.174 _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 Sm1 Sm 0.5000 1.0000 0.46465(7) 0.03533(13) Uani 1 2 d S . . Si1 Si 0.56768(12) 0.98335(11) 0.34694(10) 0.0543(6) Uani 1 1 d . . . O1 O 0.5059(2) 0.8990(2) 0.49185(18) 0.0371(12) Uani 1 1 d . . . O2 O 0.4227(3) 0.8648(3) 0.5957(3) 0.082(2) Uani 1 1 d . . . N1 N 0.5882(3) 1.0078(3) 0.5186(2) 0.0398(15) Uani 1 1 d . . . N2 N 0.5000 1.0000 0.3775(3) 0.044(2) Uani 1 2 d S . . C1 C 0.5573(3) 0.8663(3) 0.5044(3) 0.0329(17) Uani 1 1 d . . . C2 C 0.5675(3) 0.8060(3) 0.4863(3) 0.0413(19) Uani 1 1 d . . . C3 C 0.6226(4) 0.7759(3) 0.5008(3) 0.048(2) Uani 1 1 d . . . H3 H 0.6306 0.7361 0.4879 0.058 Uiso 1 1 calc R . . C4 C 0.6666(4) 0.8027(3) 0.5338(3) 0.045(2) Uani 1 1 d . . . C5 C 0.6530(4) 0.8605(3) 0.5515(3) 0.049(2) Uani 1 1 d . . . H5 H 0.6806 0.8792 0.5742 0.059 Uiso 1 1 calc R . . C6 C 0.5999(3) 0.8929(3) 0.5373(3) 0.0395(19) Uani 1 1 d . . . C7 C 0.5877(4) 0.9584(3) 0.5579(3) 0.0400(19) Uani 1 1 d . . . H7A H 0.5473 0.9587 0.5748 0.048 Uiso 1 1 calc R . . H7B H 0.6193 0.9681 0.5832 0.048 Uiso 1 1 calc R . . C8 C 0.6462(4) 1.0287(3) 0.5038(3) 0.044(2) Uani 1 1 d . . . C9 C 0.6498(4) 1.0738(3) 0.4659(4) 0.057(2) Uani 1 1 d . . . H9 H 0.6127 1.0895 0.4526 0.069 Uiso 1 1 calc R . . C10 C 0.7040(4) 1.0960(4) 0.4476(4) 0.069(3) Uani 1 1 d . . . H10 H 0.7029 1.1256 0.4217 0.083 Uiso 1 1 calc R . . C11 C 0.7602(4) 1.0769(4) 0.4654(5) 0.063(2) Uani 1 1 d . . . C12 C 0.7580(4) 1.0342(4) 0.5038(4) 0.059(3) Uani 1 1 d . . . H12 H 0.7958 1.0208 0.5177 0.071 Uiso 1 1 calc R . . C13 C 0.7037(4) 1.0096(4) 0.5235(4) 0.052(2) Uani 1 1 d . . . H13 H 0.7053 0.9804 0.5498 0.063 Uiso 1 1 calc R . . C14 C 0.8215(4) 1.0987(5) 0.4441(4) 0.091(4) Uani 1 1 d . . . H14A H 0.8399 1.1288 0.4667 0.136 Uiso 1 1 calc R . . H14B H 0.8146 1.1178 0.4115 0.136 Uiso 1 1 calc R . . H14C H 0.8492 1.0636 0.4403 0.136 Uiso 1 1 calc R . . C15 C 0.5209(3) 0.7725(4) 0.4508(3) 0.048(2) Uani 1 1 d . . . C16 C 0.5426(4) 0.7077(3) 0.4361(4) 0.060(3) Uani 1 1 d . . . H16A H 0.5124 0.6889 0.4137 0.090 Uiso 1 1 calc R . . H16B H 0.5470 0.6824 0.4660 0.090 Uiso 1 1 calc R . . H16C H 0.5822 0.7105 0.4190 0.090 Uiso 1 1 calc R . . C17 C 0.4584(4) 0.7657(4) 0.4781(3) 0.061(3) Uani 1 1 d . . . H17A H 0.4413 0.8065 0.4848 0.092 Uiso 1 1 calc R . . H17B H 0.4646 0.7440 0.5097 0.092 Uiso 1 1 calc R . . H17C H 0.4299 0.7424 0.4572 0.092 Uiso 1 1 calc R . . C18 C 0.5121(4) 0.8087(4) 0.4021(3) 0.060(3) Uani 1 1 d . . . H18A H 0.5499 0.8069 0.3824 0.090 Uiso 1 1 calc R . . H18B H 0.5025 0.8516 0.4099 0.090 Uiso 1 1 calc R . . H18C H 0.4783 0.7907 0.3830 0.090 Uiso 1 1 calc R . . C19 C 0.7254(4) 0.7675(4) 0.5474(4) 0.059(3) Uani 1 1 d . . . C20 C 0.7612(5) 0.7568(5) 0.4971(4) 0.102(2) Uani 1 1 d . . . H20A H 0.8008 0.7375 0.5042 0.152 Uiso 1 1 calc R . . H20B H 0.7679 0.7963 0.4805 0.152 Uiso 1 1 calc R . . H20C H 0.7370 0.7299 0.4754 0.152 Uiso 1 1 calc R . . C21 C 0.7671(5) 0.8034(5) 0.5781(5) 0.102(2) Uani 1 1 d . . . H21A H 0.7478 0.8120 0.6103 0.152 Uiso 1 1 calc R . . H21B H 0.7766 0.8422 0.5613 0.152 Uiso 1 1 calc R . . H21C H 0.8051 0.7803 0.5835 0.152 Uiso 1 1 calc R . . C22 C 0.7127(5) 0.7054(5) 0.5690(5) 0.102(2) Uani 1 1 d . . . H22A H 0.7510 0.6821 0.5712 0.152 Uiso 1 1 calc R . . H22B H 0.6836 0.6835 0.5476 0.152 Uiso 1 1 calc R . . H22C H 0.6951 0.7100 0.6024 0.152 Uiso 1 1 calc R . . C23 C 0.5574(5) 0.9298(5) 0.2912(4) 0.088(4) Uani 1 1 d . . . H23A H 0.5435 0.8895 0.3028 0.131 Uiso 1 1 calc R . . H23B H 0.5967 0.9253 0.2737 0.131 Uiso 1 1 calc R . . H23C H 0.5268 0.9471 0.2684 0.131 Uiso 1 1 calc R . . C24 C 0.6086(5) 1.0552(5) 0.3238(4) 0.084(3) Uani 1 1 d . . . H24A H 0.5781 1.0863 0.3146 0.126 Uiso 1 1 calc R . . H24B H 0.6336 1.0450 0.2946 0.126 Uiso 1 1 calc R . . H24C H 0.6351 1.0714 0.3502 0.126 Uiso 1 1 calc R . . C25 C 0.6233(4) 0.9431(4) 0.3898(4) 0.067(3) Uani 1 1 d . . . H25A H 0.6320 0.9694 0.4186 0.101 Uiso 1 1 calc R . . H25B H 0.6616 0.9348 0.3718 0.101 Uiso 1 1 calc R . . H25C H 0.6054 0.9044 0.4012 0.101 Uiso 1 1 calc R . . C26 C 0.4415(5) 0.8060(5) 0.6147(4) 0.100(4) Uani 1 1 d . . . H26A H 0.4867 0.8039 0.6173 0.120 Uiso 1 1 calc R . . H26B H 0.4274 0.7728 0.5922 0.120 Uiso 1 1 calc R . . C27 C 0.4134(7) 0.7992(7) 0.6640(6) 0.141(6) Uani 1 1 d D . . H27A H 0.4452 0.8010 0.6903 0.169 Uiso 1 1 calc R . . H27B H 0.3919 0.7593 0.6665 0.169 Uiso 1 1 calc R . . C28 C 0.3692(7) 0.8507(6) 0.6698(5) 0.127(5) Uani 1 1 d D . . H28A H 0.3266 0.8363 0.6644 0.152 Uiso 1 1 calc R . . H28B H 0.3722 0.8688 0.7035 0.152 Uiso 1 1 calc R . . C29 C 0.3866(7) 0.8962(6) 0.6316(5) 0.133(6) Uani 1 1 d D . . H29A H 0.3495 0.9137 0.6158 0.159 Uiso 1 1 calc R . . H29B H 0.4104 0.9300 0.6468 0.159 Uiso 1 1 calc R . . Li1 Li 0.4382(7) 0.9036(6) 0.5361(6) 0.056(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.0327(3) 0.0375(3) 0.0358(2) 0.000 0.000 0.0001(2) Si1 0.0621(16) 0.0596(16) 0.0412(13) -0.0074(13) 0.0098(12) -0.0089(13) O1 0.030(3) 0.033(3) 0.049(3) -0.005(2) 0.000(2) 0.001(2) O2 0.116(6) 0.061(4) 0.068(5) 0.011(4) 0.048(4) 0.022(4) N1 0.042(4) 0.024(3) 0.053(4) 0.000(3) -0.005(3) -0.002(3) N2 0.040(5) 0.064(6) 0.026(5) 0.000 0.000 -0.011(5) C1 0.023(4) 0.040(5) 0.036(5) 0.003(3) 0.000(3) 0.009(3) C2 0.043(5) 0.038(4) 0.043(5) 0.007(4) -0.003(4) 0.002(4) C3 0.070(6) 0.030(4) 0.044(5) 0.000(4) 0.004(4) 0.004(4) C4 0.044(5) 0.039(5) 0.052(6) -0.003(4) -0.006(4) -0.001(4) C5 0.054(5) 0.043(5) 0.050(5) -0.004(4) -0.012(4) -0.006(4) C6 0.035(4) 0.045(5) 0.038(5) -0.002(4) 0.006(4) 0.004(4) C7 0.047(5) 0.036(4) 0.037(5) -0.011(4) 0.000(4) -0.003(4) C8 0.059(6) 0.036(4) 0.036(5) -0.010(4) -0.015(4) -0.002(4) C9 0.067(6) 0.039(4) 0.066(6) 0.010(5) -0.019(6) -0.005(4) C10 0.067(7) 0.070(7) 0.070(8) 0.008(5) -0.011(5) -0.023(5) C11 0.062(6) 0.051(5) 0.078(7) -0.010(6) 0.005(6) -0.020(4) C12 0.041(5) 0.056(6) 0.082(8) -0.024(5) -0.015(5) 0.006(4) C13 0.046(5) 0.040(5) 0.070(7) -0.005(5) -0.004(5) 0.008(4) C14 0.076(7) 0.078(7) 0.118(12) 0.008(7) 0.017(7) -0.030(6) C15 0.041(5) 0.042(5) 0.060(7) -0.007(4) -0.002(4) 0.001(4) C16 0.066(6) 0.029(5) 0.083(7) -0.024(4) -0.001(5) 0.003(4) C17 0.048(5) 0.059(6) 0.077(8) -0.015(5) 0.001(5) 0.001(4) C18 0.080(7) 0.058(6) 0.042(6) -0.011(5) -0.016(5) 0.008(5) C19 0.035(5) 0.047(5) 0.094(8) -0.009(5) -0.025(5) 0.010(4) C20 0.071(5) 0.101(5) 0.133(7) 0.022(5) -0.015(4) 0.030(4) C21 0.071(5) 0.101(5) 0.133(7) 0.022(5) -0.015(4) 0.030(4) C22 0.071(5) 0.101(5) 0.133(7) 0.022(5) -0.015(4) 0.030(4) C23 0.113(9) 0.099(8) 0.051(7) -0.049(6) 0.011(6) 0.011(7) C24 0.085(8) 0.092(8) 0.074(8) 0.015(6) 0.035(6) -0.024(6) C25 0.050(6) 0.067(7) 0.084(8) -0.001(6) 0.005(5) 0.000(4) C26 0.115(10) 0.110(10) 0.075(9) 0.033(7) 0.007(8) 0.054(8) C27 0.178(16) 0.128(12) 0.116(14) 0.057(10) 0.034(11) 0.072(11) C28 0.200(16) 0.110(10) 0.071(10) -0.009(8) 0.038(10) 0.019(11) C29 0.200(15) 0.103(10) 0.095(11) 0.043(8) 0.095(11) 0.047(10) Li1 0.089(11) 0.025(7) 0.054(10) 0.012(7) 0.033(8) 0.016(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 Sm1 O1 2.299(4) 11_564 ? Sm1 O1 2.299(4) . ? Sm1 N2 2.317(8) . ? Sm1 N1 2.388(6) . ? Sm1 N1 2.388(6) 11_564 ? Sm1 Li1 3.117(13) 11_564 ? Sm1 Li1 3.117(13) . ? Si1 N2 1.708(5) . ? Si1 C25 1.868(9) . ? Si1 C24 1.888(9) . ? Si1 C23 1.892(8) . ? O1 C1 1.357(8) . ? O1 Li1 1.878(15) . ? O2 C29 1.405(12) . ? O2 C26 1.425(11) . ? O2 Li1 1.822(15) . ? N1 C8 1.387(10) . ? N1 C7 1.492(9) . ? N1 Li1 2.048(13) 11_564 ? N2 Si1 1.708(5) 11_564 ? C1 C6 1.392(10) . ? C1 C2 1.404(10) . ? C2 C3 1.407(10) . ? C2 C15 1.558(10) . ? C3 C4 1.414(11) . ? C3 H3 0.9400 . ? C4 C5 1.365(10) . ? C4 C19 1.522(10) . ? C5 C6 1.394(10) . ? C5 H5 0.9400 . ? C6 C7 1.539(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.402(11) . ? C8 C13 1.409(11) . ? C8 Li1 2.487(17) 11_564 ? C9 C10 1.352(11) . ? C9 Li1 2.706(19) 11_564 ? C9 H9 0.9400 . ? C10 C11 1.366(12) . ? C10 H10 0.9400 . ? C11 C12 1.375(13) . ? C11 C14 1.514(12) . ? C12 C13 1.389(12) . ? C12 H12 0.9400 . ? C13 H13 0.9400 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 C18 1.524(12) . ? C15 C16 1.526(10) . ? C15 C17 1.537(10) . ? 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 C21 1.442(13) . ? C19 C22 1.484(13) . ? C19 C20 1.560(14) . ? 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 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 C27 1.451(15) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.474(12) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.460(12) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? Li1 N1 2.048(13) 11_564 ? Li1 C8 2.487(17) 11_564 ? Li1 C9 2.706(19) 11_564 ? 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 Sm1 O1 143.3(2) 11_564 . ? O1 Sm1 N2 108.33(13) 11_564 . ? O1 Sm1 N2 108.33(12) . . ? O1 Sm1 N1 77.77(19) 11_564 . ? O1 Sm1 N1 80.44(18) . . ? N2 Sm1 N1 126.92(16) . . ? O1 Sm1 N1 80.44(18) 11_564 11_564 ? O1 Sm1 N1 77.77(19) . 11_564 ? N2 Sm1 N1 126.92(16) . 11_564 ? N1 Sm1 N1 106.2(3) . 11_564 ? O1 Sm1 Li1 36.8(3) 11_564 11_564 ? O1 Sm1 Li1 114.7(3) . 11_564 ? N2 Sm1 Li1 127.6(3) . 11_564 ? N1 Sm1 Li1 41.1(3) . 11_564 ? N1 Sm1 Li1 91.2(4) 11_564 11_564 ? O1 Sm1 Li1 114.7(3) 11_564 . ? O1 Sm1 Li1 36.8(3) . . ? N2 Sm1 Li1 127.6(3) . . ? N1 Sm1 Li1 91.2(4) . . ? N1 Sm1 Li1 41.1(3) 11_564 . ? Li1 Sm1 Li1 104.9(6) 11_564 . ? N2 Si1 C25 110.9(4) . . ? N2 Si1 C24 112.4(4) . . ? C25 Si1 C24 106.2(5) . . ? N2 Si1 C23 113.6(4) . . ? C25 Si1 C23 105.6(5) . . ? C24 Si1 C23 107.5(5) . . ? C1 O1 Li1 120.6(6) . . ? C1 O1 Sm1 128.0(4) . . ? Li1 O1 Sm1 96.0(4) . . ? C29 O2 C26 110.3(8) . . ? C29 O2 Li1 118.1(7) . . ? C26 O2 Li1 131.6(7) . . ? C8 N1 C7 115.9(6) . . ? C8 N1 Li1 90.7(6) . 11_564 ? C7 N1 Li1 120.4(6) . 11_564 ? C8 N1 Sm1 124.8(5) . . ? C7 N1 Sm1 111.4(4) . . ? Li1 N1 Sm1 88.9(4) 11_564 . ? Si1 N2 Si1 123.3(5) 11_564 . ? Si1 N2 Sm1 118.4(3) 11_564 . ? Si1 N2 Sm1 118.4(3) . . ? O1 C1 C6 118.7(6) . . ? O1 C1 C2 121.7(6) . . ? C6 C1 C2 119.5(6) . . ? C1 C2 C3 117.8(7) . . ? C1 C2 C15 122.4(6) . . ? C3 C2 C15 119.9(7) . . ? C2 C3 C4 123.2(7) . . ? C2 C3 H3 118.4 . . ? C4 C3 H3 118.4 . . ? C5 C4 C3 116.3(7) . . ? C5 C4 C19 123.5(7) . . ? C3 C4 C19 120.2(7) . . ? C4 C5 C6 122.7(7) . . ? C4 C5 H5 118.6 . . ? C6 C5 H5 118.6 . . ? C1 C6 C5 120.4(7) . . ? C1 C6 C7 119.3(6) . . ? C5 C6 C7 120.3(7) . . ? N1 C7 C6 113.9(6) . . ? N1 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? N1 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N1 C8 C9 118.7(7) . . ? N1 C8 C13 126.4(7) . . ? C9 C8 C13 114.9(8) . . ? N1 C8 Li1 55.4(5) . 11_564 ? C9 C8 Li1 83.2(6) . 11_564 ? C13 C8 Li1 133.5(7) . 11_564 ? C10 C9 C8 123.5(8) . . ? C10 C9 Li1 142.2(7) . 11_564 ? C8 C9 Li1 65.8(6) . 11_564 ? C10 C9 H9 118.2 . . ? C8 C9 H9 118.2 . . ? Li1 C9 H9 66.2 11_564 . ? C9 C10 C11 122.4(9) . . ? C9 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C10 C11 C12 115.4(8) . . ? C10 C11 C14 123.5(10) . . ? C12 C11 C14 121.1(9) . . ? C11 C12 C13 124.4(9) . . ? C11 C12 H12 117.8 . . ? C13 C12 H12 117.8 . . ? C12 C13 C8 119.4(9) . . ? C12 C13 H13 120.3 . . ? C8 C13 H13 120.3 . . ? 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 . . ? C18 C15 C16 106.8(7) . . ? C18 C15 C17 110.0(7) . . ? C16 C15 C17 107.7(7) . . ? C18 C15 C2 110.9(7) . . ? C16 C15 C2 112.5(6) . . ? C17 C15 C2 108.9(7) . . ? 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 . . ? C21 C19 C22 112.4(9) . . ? C21 C19 C4 112.8(7) . . ? C22 C19 C4 112.8(7) . . ? C21 C19 C20 104.9(9) . . ? C22 C19 C20 106.8(8) . . ? C4 C19 C20 106.4(8) . . ? 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 . . ? 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 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O2 C26 C27 106.9(9) . . ? O2 C26 H26A 110.3 . . ? C27 C26 H26A 110.3 . . ? O2 C26 H26B 110.3 . . ? C27 C26 H26B 110.3 . . ? H26A C26 H26B 108.6 . . ? C26 C27 C28 106.7(10) . . ? C26 C27 H27A 110.4 . . ? C28 C27 H27A 110.4 . . ? C26 C27 H27B 110.4 . . ? C28 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? C29 C28 C27 105.6(11) . . ? C29 C28 H28A 110.6 . . ? C27 C28 H28A 110.6 . . ? C29 C28 H28B 110.6 . . ? C27 C28 H28B 110.6 . . ? H28A C28 H28B 108.8 . . ? O2 C29 C28 106.9(9) . . ? O2 C29 H29A 110.3 . . ? C28 C29 H29A 110.3 . . ? O2 C29 H29B 110.3 . . ? C28 C29 H29B 110.3 . . ? H29A C29 H29B 108.6 . . ? O2 Li1 O1 131.6(8) . . ? O2 Li1 N1 125.1(8) . 11_564 ? O1 Li1 N1 97.0(6) . 11_564 ? O2 Li1 C8 115.8(7) . 11_564 ? O1 Li1 C8 112.5(7) . 11_564 ? N1 Li1 C8 33.9(3) 11_564 11_564 ? O2 Li1 C9 123.6(8) . 11_564 ? O1 Li1 C9 97.1(6) . 11_564 ? N1 Li1 C9 58.7(4) 11_564 11_564 ? C8 Li1 C9 31.0(3) 11_564 11_564 ? O2 Li1 Sm1 156.2(8) . . ? O1 Li1 Sm1 47.2(3) . . ? N1 Li1 Sm1 50.0(3) 11_564 . ? C8 Li1 Sm1 73.2(4) 11_564 . ? C9 Li1 Sm1 76.1(4) 11_564 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.337 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.062 #===================================================end data_complex4 _database_code_depnum_ccdc_archive 'CCDC 767735' #TrackingRef '- Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H92 Li2 N3 O4 Si2 Yb' _chemical_formula_sum 'C58 H92 Li2 N3 O4 Si2 Yb' _chemical_formula_weight 1138.45 _chemical_absolute_configuration unk 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' 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 21.5166(11) _cell_length_b 21.5166(11) _cell_length_c 26.4564(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12248.4(12) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 24127 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4776 _exptl_absorpt_coefficient_mu 1.609 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.480 _exptl_absorpt_correction_T_max 0.669 _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 53635 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6576 _reflns_number_gt 5940 _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 'CrystalStructure 3.8' _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^)+(0.0935P)^2^+34.3443P] 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 0.05(4) _refine_ls_number_reflns 6576 _refine_ls_number_parameters 318 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1821 _refine_ls_wR_factor_gt 0.1765 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.134 _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 0.5000 0.5000 0.53342(12) 0.03029(14) Uani 1 2 d S . . Si1 Si 0.43303(9) 0.51686(10) 0.65001(7) 0.0466(4) Uani 1 1 d . . . O1 O 0.49373(17) 0.59825(18) 0.51152(19) 0.0332(9) Uani 1 1 d . . . O2 O 0.5762(3) 0.6360(3) 0.4067(2) 0.0784(19) Uani 1 1 d D . . N1 N 0.4129(3) 0.4919(2) 0.4836(2) 0.0358(12) Uani 1 1 d . . . N2 N 0.5000 0.5000 0.6168(4) 0.034(2) Uani 1 2 d S . . C1 C 0.4429(2) 0.6317(3) 0.4979(2) 0.0286(11) Uani 1 1 d . . . C2 C 0.4336(2) 0.6929(2) 0.5154(2) 0.0293(11) Uani 1 1 d . . . C3 C 0.3791(3) 0.7236(3) 0.5007(2) 0.0405(14) Uani 1 1 d . . . H3 H 0.3716 0.7637 0.5134 0.049 Uiso 1 1 calc R . . C4 C 0.3350(3) 0.6973(3) 0.4678(3) 0.0406(14) Uani 1 1 d . . . C5 C 0.3487(3) 0.6385(3) 0.4495(3) 0.0422(16) Uani 1 1 d . . . H5 H 0.3214 0.6200 0.4262 0.051 Uiso 1 1 calc R . . C6 C 0.4008(3) 0.6064(3) 0.4643(2) 0.0309(13) Uani 1 1 d . . . C7 C 0.4151(3) 0.5417(3) 0.4432(2) 0.0367(13) Uani 1 1 d . . . H7A H 0.3848 0.5316 0.4168 0.044 Uiso 1 1 calc R . . H7B H 0.4565 0.5420 0.4278 0.044 Uiso 1 1 calc R . . C8 C 0.3546(3) 0.4706(3) 0.4976(2) 0.0387(15) Uani 1 1 d . . . C9 C 0.3512(3) 0.4259(3) 0.5362(3) 0.0528(18) Uani 1 1 d . . . H9 H 0.3882 0.4103 0.5501 0.063 Uiso 1 1 calc R . . C10 C 0.2955(4) 0.4043(4) 0.5543(3) 0.065(2) Uani 1 1 d . . . H10 H 0.2957 0.3756 0.5810 0.078 Uiso 1 1 calc R . . C11 C 0.2390(3) 0.4232(3) 0.5346(3) 0.0556(18) Uani 1 1 d . . . C12 C 0.2422(3) 0.4654(4) 0.4956(3) 0.057(2) Uani 1 1 d . . . H12 H 0.2049 0.4785 0.4803 0.068 Uiso 1 1 calc R . . C13 C 0.2975(3) 0.4895(3) 0.4777(3) 0.0456(16) Uani 1 1 d . . . H13 H 0.2968 0.5192 0.4517 0.055 Uiso 1 1 calc R . . C14 C 0.1790(4) 0.3989(5) 0.5559(5) 0.090(3) Uani 1 1 d . . . H14A H 0.1444 0.4166 0.5373 0.135 Uiso 1 1 calc R . . H14B H 0.1758 0.4104 0.5912 0.135 Uiso 1 1 calc R . . H14C H 0.1781 0.3540 0.5528 0.135 Uiso 1 1 calc R . . C15 C 0.4800(3) 0.7262(3) 0.5518(3) 0.0443(15) Uani 1 1 d . . . C16 C 0.4590(3) 0.7924(3) 0.5661(3) 0.0503(17) Uani 1 1 d . . . H16A H 0.4187 0.7904 0.5825 0.075 Uiso 1 1 calc R . . H16B H 0.4559 0.8175 0.5358 0.075 Uiso 1 1 calc R . . H16C H 0.4890 0.8108 0.5889 0.075 Uiso 1 1 calc R . . C17 C 0.5433(3) 0.7333(4) 0.5238(4) 0.065(2) Uani 1 1 d . . . H17A H 0.5726 0.7551 0.5453 0.098 Uiso 1 1 calc R . . H17B H 0.5372 0.7567 0.4928 0.098 Uiso 1 1 calc R . . H17C H 0.5597 0.6925 0.5156 0.098 Uiso 1 1 calc R . . C18 C 0.4891(4) 0.6910(4) 0.6002(3) 0.0560(19) Uani 1 1 d . . . H18A H 0.5221 0.7103 0.6197 0.084 Uiso 1 1 calc R . . H18B H 0.5002 0.6483 0.5926 0.084 Uiso 1 1 calc R . . H18C H 0.4509 0.6917 0.6196 0.084 Uiso 1 1 calc R . . C19 C 0.2740(3) 0.7314(3) 0.4546(3) 0.054(2) Uani 1 1 d D . . C20 C 0.2388(5) 0.7427(6) 0.5029(6) 0.088(4) Uani 1 1 d D . . H20A H 0.1991 0.7619 0.4952 0.132 Uiso 1 1 calc R . . H20B H 0.2628 0.7700 0.5246 0.132 Uiso 1 1 calc R . . H20C H 0.2319 0.7034 0.5200 0.132 Uiso 1 1 calc R . . C21 C 0.2409(8) 0.7022(8) 0.4095(6) 0.060(4) Uiso 0.50 1 d PD . . C21' C 0.2261(9) 0.6880(8) 0.4313(8) 0.068(5) Uiso 0.50 1 d PD . . C22 C 0.2881(5) 0.7958(5) 0.4326(5) 0.085(4) Uani 1 1 d . . . H22A H 0.3056 0.7912 0.3990 0.127 Uiso 1 1 calc R . . H22B H 0.3177 0.8171 0.4542 0.127 Uiso 1 1 calc R . . H22C H 0.2500 0.8197 0.4307 0.127 Uiso 1 1 calc R . . C23 C 0.4444(5) 0.5696(5) 0.7064(4) 0.077(3) Uani 1 1 d . . . H23A H 0.4760 0.5522 0.7284 0.115 Uiso 1 1 calc R . . H23B H 0.4056 0.5732 0.7248 0.115 Uiso 1 1 calc R . . H23C H 0.4574 0.6104 0.6950 0.115 Uiso 1 1 calc R . . C24 C 0.3926(4) 0.4459(4) 0.6743(4) 0.070(2) Uani 1 1 d . . . H24A H 0.3984 0.4119 0.6506 0.105 Uiso 1 1 calc R . . H24B H 0.3485 0.4545 0.6779 0.105 Uiso 1 1 calc R . . H24C H 0.4098 0.4345 0.7069 0.105 Uiso 1 1 calc R . . C25 C 0.3753(3) 0.5595(4) 0.6091(3) 0.0556(18) Uani 1 1 d . . . H25A H 0.3966 0.5915 0.5900 0.083 Uiso 1 1 calc R . . H25B H 0.3438 0.5786 0.6304 0.083 Uiso 1 1 calc R . . H25C H 0.3557 0.5305 0.5861 0.083 Uiso 1 1 calc R . . C26 C 0.5646(7) 0.7002(6) 0.3891(5) 0.063(3) Uiso 0.620(14) 1 d PD A 1 C27 C 0.5964(8) 0.7067(7) 0.3393(6) 0.078(4) Uiso 0.620(14) 1 d PD A 1 C28 C 0.6386(9) 0.6512(7) 0.3347(7) 0.077(4) Uiso 0.620(14) 1 d PD A 1 C29 C 0.6229(7) 0.6070(7) 0.3749(5) 0.065(3) Uiso 0.620(14) 1 d PD A 1 C26' C 0.5421(12) 0.6852(12) 0.3832(8) 0.063(3) Uiso 0.380(14) 1 d PD A 2 C27' C 0.5683(14) 0.6907(12) 0.3297(9) 0.078(4) Uiso 0.380(14) 1 d PD A 2 C28' C 0.6145(13) 0.6391(11) 0.3234(11) 0.077(4) Uiso 0.380(14) 1 d PD A 2 C29' C 0.5927(12) 0.5957(9) 0.3640(7) 0.065(3) Uiso 0.380(14) 1 d PD A 2 Li1 Li 0.5631(6) 0.5964(5) 0.4694(5) 0.054(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 0.02851(19) 0.0309(2) 0.0315(2) 0.000 0.000 0.00044(11) Si1 0.0498(10) 0.0580(11) 0.0319(9) -0.0081(9) 0.0125(8) -0.0086(9) O1 0.037(2) 0.0198(18) 0.043(3) -0.0013(18) -0.0001(17) 0.0012(14) O2 0.108(5) 0.058(3) 0.069(4) 0.018(3) 0.045(3) 0.025(3) N1 0.036(3) 0.027(2) 0.044(3) -0.006(2) -0.011(2) -0.0018(19) N2 0.025(4) 0.057(5) 0.018(5) 0.000 0.000 -0.003(3) C1 0.026(3) 0.039(3) 0.021(3) 0.000(2) -0.002(2) 0.006(2) C2 0.026(3) 0.030(3) 0.031(3) 0.005(2) 0.000(2) 0.004(2) C3 0.059(4) 0.021(3) 0.042(4) -0.014(2) 0.001(3) 0.002(2) C4 0.045(3) 0.030(3) 0.046(4) -0.005(3) 0.002(3) 0.009(3) C5 0.054(4) 0.039(3) 0.034(4) 0.000(3) -0.008(3) -0.003(3) C6 0.036(3) 0.024(3) 0.033(3) 0.003(2) 0.001(2) -0.004(2) C7 0.042(3) 0.037(3) 0.031(3) 0.000(2) -0.008(3) 0.002(3) C8 0.052(4) 0.026(3) 0.038(4) -0.002(2) -0.020(3) -0.011(2) C9 0.053(4) 0.037(3) 0.069(5) 0.009(3) -0.015(4) -0.011(3) C10 0.059(5) 0.072(5) 0.064(6) 0.015(4) -0.011(4) -0.017(4) C11 0.050(4) 0.045(4) 0.072(5) -0.014(4) -0.001(4) -0.013(3) C12 0.039(4) 0.056(4) 0.076(6) -0.008(4) -0.018(4) 0.009(3) C13 0.047(4) 0.040(3) 0.050(4) -0.005(3) -0.010(3) -0.002(3) C14 0.060(5) 0.077(6) 0.134(10) -0.007(6) 0.014(6) -0.033(5) C15 0.040(3) 0.039(3) 0.054(4) -0.010(3) 0.001(3) -0.003(3) C16 0.049(4) 0.028(3) 0.074(5) -0.017(3) 0.002(3) 0.001(3) C17 0.044(4) 0.060(4) 0.092(7) -0.023(4) 0.015(4) -0.011(3) C18 0.068(5) 0.051(4) 0.049(5) 0.001(4) -0.011(4) 0.010(3) C19 0.040(4) 0.047(4) 0.076(6) -0.011(4) -0.012(3) 0.016(3) C20 0.060(5) 0.099(8) 0.105(12) 0.031(7) 0.017(6) 0.020(6) C22 0.067(6) 0.098(7) 0.090(8) 0.042(6) 0.001(5) 0.021(6) C23 0.111(8) 0.079(6) 0.040(5) -0.032(4) 0.003(5) 0.007(6) C24 0.062(5) 0.079(6) 0.070(6) 0.009(4) 0.036(4) -0.019(4) C25 0.048(4) 0.058(4) 0.061(5) -0.006(4) 0.002(3) 0.003(3) Li1 0.056(7) 0.034(6) 0.071(9) 0.024(6) 0.029(6) -0.006(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 2.196(4) 11_554 ? Yb1 O1 2.196(4) . ? Yb1 N2 2.205(11) . ? Yb1 N1 2.298(6) . ? Yb1 N1 2.298(6) 11_554 ? Yb1 Li1 3.001(10) 11_554 ? Yb1 Li1 3.001(10) . ? Yb1 C7 3.136(6) 11_554 ? Yb1 Si1 3.424(3) 11_554 ? Si1 N2 1.727(6) . ? Si1 C25 1.886(8) . ? Si1 C24 1.871(8) . ? Si1 C23 1.891(8) . ? O1 C1 1.359(6) . ? O1 Li1 1.862(13) . ? O2 C26' 1.43(2) . ? O2 C29 1.451(10) . ? O2 C29' 1.466(16) . ? O2 C26 1.479(13) . ? O2 Li1 1.888(13) . ? N1 C8 1.386(9) . ? N1 C7 1.513(8) . ? N1 Li1 2.005(13) 11_554 ? N2 Si1 1.727(6) 11_554 ? C1 C6 1.380(8) . ? C1 C2 1.409(8) . ? C2 C3 1.402(8) . ? C2 C15 1.561(9) . ? C3 C4 1.406(9) . ? C3 H3 0.9400 . ? C4 C5 1.387(9) . ? C4 C19 1.543(9) . ? C5 C6 1.376(10) . ? C5 H5 0.9400 . ? C6 C7 1.531(8) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C13 1.396(9) . ? C8 C9 1.404(9) . ? C8 Li1 2.401(15) 11_554 ? C9 C10 1.371(10) . ? C9 Li1 2.598(17) 11_554 ? C9 H9 0.9400 . ? C10 C11 1.383(11) . ? C10 H10 0.9400 . ? C11 C12 1.376(11) . ? C11 C14 1.503(11) . ? C12 C13 1.382(11) . ? C12 H12 0.9400 . ? C13 H13 0.9400 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 C18 1.499(11) . ? C15 C16 1.541(8) . ? C15 C17 1.559(10) . ? 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 1.506(14) . ? C19 C22 1.532(13) . ? C19 C21' 1.521(15) . ? C19 C21 1.526(14) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? 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 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 C27 1.492(15) . ? C27 C28 1.504(15) . ? C28 C29 1.465(16) . ? C26' C27' 1.530(18) . ? C27' C28' 1.500(18) . ? C28' C29' 1.497(18) . ? Li1 N1 2.005(13) 11_554 ? Li1 C8 2.401(15) 11_554 ? Li1 C9 2.598(16) 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 Yb1 O1 149.4(3) 11_554 . ? O1 Yb1 N2 105.30(15) 11_554 . ? O1 Yb1 N2 105.30(15) . . ? O1 Yb1 N1 79.99(16) 11_554 . ? O1 Yb1 N1 82.60(17) . . ? N2 Yb1 N1 124.98(18) . . ? O1 Yb1 N1 82.60(17) 11_554 11_554 ? O1 Yb1 N1 79.99(16) . 11_554 ? N2 Yb1 N1 124.98(18) . 11_554 ? N1 Yb1 N1 110.0(4) . 11_554 ? O1 Yb1 Li1 38.2(3) 11_554 11_554 ? O1 Yb1 Li1 119.2(3) . 11_554 ? N2 Yb1 Li1 124.3(3) . 11_554 ? N1 Yb1 Li1 41.9(3) . 11_554 ? N1 Yb1 Li1 95.6(3) 11_554 11_554 ? O1 Yb1 Li1 119.2(3) 11_554 . ? O1 Yb1 Li1 38.2(3) . . ? N2 Yb1 Li1 124.3(3) . . ? N1 Yb1 Li1 95.6(3) . . ? N1 Yb1 Li1 41.9(3) 11_554 . ? Li1 Yb1 Li1 111.3(6) 11_554 . ? O1 Yb1 C7 59.22(16) 11_554 11_554 ? O1 Yb1 C7 96.33(19) . 11_554 ? N2 Yb1 C7 139.54(12) . 11_554 ? N1 Yb1 C7 91.0(2) . 11_554 ? N1 Yb1 C7 27.14(18) 11_554 11_554 ? Li1 Yb1 C7 68.7(3) 11_554 11_554 ? Li1 Yb1 C7 60.3(3) . 11_554 ? O1 Yb1 Si1 96.31(14) 11_554 11_554 ? O1 Yb1 Si1 111.44(14) . 11_554 ? N2 Yb1 Si1 25.72(4) . 11_554 ? N1 Yb1 Si1 148.41(18) . 11_554 ? N1 Yb1 Si1 100.43(17) 11_554 11_554 ? Li1 Yb1 Si1 128.7(3) 11_554 11_554 ? Li1 Yb1 Si1 113.0(3) . 11_554 ? C7 Yb1 Si1 114.20(13) 11_554 11_554 ? N2 Si1 C25 111.1(4) . . ? N2 Si1 C24 113.1(3) . . ? C25 Si1 C24 106.7(4) . . ? N2 Si1 C23 114.8(4) . . ? C25 Si1 C23 104.2(4) . . ? C24 Si1 C23 106.2(4) . . ? C1 O1 Li1 119.9(6) . . ? C1 O1 Yb1 129.0(3) . . ? Li1 O1 Yb1 95.0(4) . . ? C26' O2 C29 115.0(11) . . ? C26' O2 C29' 103.2(14) . . ? C29 O2 C29' 29.8(10) . . ? C26' O2 C26 23.8(10) . . ? C29 O2 C26 109.7(8) . . ? C29' O2 C26 110.6(10) . . ? C26' O2 Li1 129.7(10) . . ? C29 O2 Li1 114.8(7) . . ? C29' O2 Li1 116.6(10) . . ? C26 O2 Li1 132.2(7) . . ? C8 N1 C7 116.8(5) . . ? C8 N1 Li1 88.2(5) . 11_554 ? C7 N1 Li1 122.0(6) . 11_554 ? C8 N1 Yb1 127.6(4) . . ? C7 N1 Yb1 109.0(4) . . ? Li1 N1 Yb1 88.2(4) 11_554 . ? Si1 N2 Si1 118.8(7) . 11_554 ? Si1 N2 Yb1 120.6(3) . . ? Si1 N2 Yb1 120.6(3) 11_554 . ? O1 C1 C6 119.2(5) . . ? O1 C1 C2 121.5(5) . . ? C6 C1 C2 119.2(5) . . ? C3 C2 C1 117.8(5) . . ? C3 C2 C15 119.4(5) . . ? C1 C2 C15 122.7(5) . . ? C4 C3 C2 123.2(5) . . ? C4 C3 H3 118.4 . . ? C2 C3 H3 118.4 . . ? C5 C4 C3 116.1(6) . . ? C5 C4 C19 122.4(6) . . ? C3 C4 C19 121.5(5) . . ? C6 C5 C4 122.2(6) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C1 121.3(6) . . ? C5 C6 C7 121.1(5) . . ? C1 C6 C7 117.6(5) . . ? N1 C7 C6 112.3(5) . . ? N1 C7 H7A 109.2 . . ? C6 C7 H7A 109.2 . . ? N1 C7 H7B 109.2 . . ? C6 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N1 C8 C13 126.8(6) . . ? N1 C8 C9 117.9(6) . . ? C13 C8 C9 115.3(6) . . ? N1 C8 Li1 56.6(4) . 11_554 ? C13 C8 Li1 135.0(5) . 11_554 ? C9 C8 Li1 81.6(5) . 11_554 ? C10 C9 C8 122.1(7) . . ? C10 C9 Li1 142.7(6) . 11_554 ? C8 C9 Li1 66.1(5) . 11_554 ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? Li1 C9 H9 66.2 11_554 . ? C9 C10 C11 122.5(8) . . ? C9 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C10 C11 C12 115.6(7) . . ? C10 C11 C14 120.8(8) . . ? C12 C11 C14 123.6(8) . . ? C11 C12 C13 123.1(7) . . ? C11 C12 H12 118.5 . . ? C13 C12 H12 118.5 . . ? C12 C13 C8 121.4(7) . . ? C12 C13 H13 119.3 . . ? C8 C13 H13 119.3 . . ? 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 . . ? C18 C15 C16 107.2(6) . . ? C18 C15 C17 110.0(7) . . ? C16 C15 C17 106.5(6) . . ? C18 C15 C2 112.3(6) . . ? C16 C15 C2 112.7(5) . . ? C17 C15 C2 108.0(6) . . ? 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 C22 106.1(8) . . ? C20 C19 C21' 95.8(11) . . ? C22 C19 C21' 122.4(11) . . ? C20 C19 C21 119.7(11) . . ? C22 C19 C21 99.7(11) . . ? C21' C19 C21 27.6(8) . . ? C20 C19 C4 108.2(7) . . ? C22 C19 C4 110.3(6) . . ? C21' C19 C4 112.1(9) . . ? C21 C19 C4 112.2(9) . . ? 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 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 . . ? 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 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O2 C26 C27 106.6(10) . . ? C26 C27 C28 105.9(13) . . ? C29 C28 C27 108.5(13) . . ? C28 C29 O2 107.5(10) . . ? O2 C26' C27' 105.6(17) . . ? C28' C27' C26' 106.8(19) . . ? C27' C28' C29' 100.1(18) . . ? O2 C29' C28' 105.1(17) . . ? O1 Li1 O2 129.5(8) . . ? O1 Li1 N1 96.6(5) . 11_554 ? O2 Li1 N1 123.7(7) . 11_554 ? O1 Li1 C8 114.7(6) . 11_554 ? O2 Li1 C8 115.7(6) . 11_554 ? N1 Li1 C8 35.2(3) 11_554 11_554 ? O1 Li1 C9 99.6(6) . 11_554 ? O2 Li1 C9 125.1(6) . 11_554 ? N1 Li1 C9 61.0(4) 11_554 11_554 ? C8 Li1 C9 32.3(3) 11_554 11_554 ? O1 Li1 Yb1 46.8(3) . . ? O2 Li1 Yb1 151.1(7) . . ? N1 Li1 Yb1 49.9(3) 11_554 . ? C8 Li1 Yb1 75.2(3) 11_554 . ? C9 Li1 Yb1 79.1(3) 11_554 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.486 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.072 #===================================================end data_complex5 _database_code_depnum_ccdc_archive 'CCDC 767736' #TrackingRef '- Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H92 Li2 N3 O4 Si2 Y' _chemical_formula_sum 'C58 H92 Li2 N3 O4 Si2 Y' _chemical_formula_weight 1054.32 _chemical_absolute_configuration unk 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' 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 21.5684(13) _cell_length_b 21.5684(13) _cell_length_c 26.5034(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12329.3(13) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 13261 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4528 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.403 _exptl_absorpt_correction_T_max 0.663 _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 17958 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5997 _reflns_number_gt 4479 _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^)+(0.0471P)^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 -0.025(11) _refine_ls_number_reflns 5997 _refine_ls_number_parameters 316 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1214 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.056 _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 1.0000 0.46557(5) 0.03506(13) Uani 1 2 d S . . Si1 Si 0.56715(6) 0.98284(6) 0.34874(4) 0.0578(3) Uani 1 1 d . . . O1 O 0.50597(11) 0.90087(12) 0.48956(9) 0.0412(6) Uani 1 1 d . . . O2 O 0.42341(18) 0.86443(17) 0.59373(12) 0.0844(11) Uani 1 1 d . . . N1 N 0.58807(16) 1.00814(14) 0.51697(12) 0.0452(8) Uani 1 1 d . . . N2 N 0.5000 1.0000 0.38033(19) 0.0453(13) Uani 1 2 d S . . C1 C 0.55719(18) 0.86701(17) 0.50254(13) 0.0408(9) Uani 1 1 d . . . C2 C 0.56706(18) 0.80611(18) 0.48458(13) 0.0420(9) Uani 1 1 d . . . C3 C 0.6216(2) 0.77659(19) 0.49975(15) 0.0502(10) Uani 1 1 d . . . H3 H 0.6294 0.7365 0.4873 0.060 Uiso 1 1 calc R . . C4 C 0.6652(2) 0.80299(18) 0.53233(16) 0.0498(10) Uani 1 1 d . . . C5 C 0.6524(2) 0.86159(19) 0.55000(15) 0.0498(10) Uani 1 1 d . . . H5 H 0.6804 0.8805 0.5724 0.060 Uiso 1 1 calc R . . C6 C 0.59969(18) 0.89337(17) 0.53579(14) 0.0409(9) Uani 1 1 d . . . C7 C 0.5869(2) 0.95907(18) 0.55558(14) 0.0450(9) Uani 1 1 d . . . H7A H 0.5462 0.9594 0.5719 0.054 Uiso 1 1 calc R . . H7B H 0.6179 0.9690 0.5814 0.054 Uiso 1 1 calc R . . C8 C 0.64639(19) 1.02924(18) 0.50186(14) 0.0461(10) Uani 1 1 d . . . C9 C 0.6494(2) 1.07402(19) 0.46361(16) 0.0592(11) Uani 1 1 d . . . H9 H 0.6124 1.0893 0.4497 0.071 Uiso 1 1 calc R . . C10 C 0.7048(2) 1.0961(2) 0.44594(18) 0.0740(15) Uani 1 1 d . . . H10 H 0.7044 1.1258 0.4200 0.089 Uiso 1 1 calc R . . C11 C 0.7612(2) 1.0766(2) 0.4646(2) 0.0645(12) Uani 1 1 d . . . C12 C 0.7584(2) 1.0342(2) 0.50366(19) 0.0649(13) Uani 1 1 d . . . H12 H 0.7958 1.0208 0.5183 0.078 Uiso 1 1 calc R . . C13 C 0.7037(2) 1.01049(18) 0.52231(17) 0.0508(10) Uani 1 1 d . . . H13 H 0.7047 0.9816 0.5489 0.061 Uiso 1 1 calc R . . C14 C 0.8221(3) 1.1002(3) 0.4443(2) 0.0957(19) Uani 1 1 d . . . H14A H 0.8424 1.1254 0.4697 0.144 Uiso 1 1 calc R . . H14B H 0.8146 1.1251 0.4144 0.144 Uiso 1 1 calc R . . H14C H 0.8484 1.0654 0.4356 0.144 Uiso 1 1 calc R . . C15 C 0.52018(19) 0.77329(18) 0.44946(15) 0.0497(10) Uani 1 1 d . . . C16 C 0.5413(2) 0.7079(2) 0.43508(17) 0.0584(11) Uani 1 1 d . . . H16A H 0.5112 0.6894 0.4125 0.088 Uiso 1 1 calc R . . H16B H 0.5449 0.6827 0.4653 0.088 Uiso 1 1 calc R . . H16C H 0.5813 0.7101 0.4184 0.088 Uiso 1 1 calc R . . C17 C 0.4574(2) 0.7657(2) 0.47678(19) 0.0672(13) Uani 1 1 d . . . H17A H 0.4384 0.8061 0.4813 0.101 Uiso 1 1 calc R . . H17B H 0.4641 0.7467 0.5095 0.101 Uiso 1 1 calc R . . H17C H 0.4303 0.7396 0.4567 0.101 Uiso 1 1 calc R . . C18 C 0.5115(2) 0.8096(2) 0.40080(17) 0.0620(13) Uani 1 1 d . . . H18A H 0.5007 0.8522 0.4087 0.093 Uiso 1 1 calc R . . H18B H 0.4785 0.7910 0.3811 0.093 Uiso 1 1 calc R . . H18C H 0.5497 0.8089 0.3815 0.093 Uiso 1 1 calc R . . C19 C 0.7249(2) 0.7677(2) 0.5451(2) 0.0597(12) Uani 1 1 d . . . C20 C 0.7610(3) 0.7567(3) 0.4962(3) 0.1092(14) Uani 1 1 d . . . H20A H 0.7696 0.7962 0.4801 0.164 Uiso 1 1 calc R . . H20B H 0.7365 0.7311 0.4737 0.164 Uiso 1 1 calc R . . H20C H 0.7998 0.7360 0.5039 0.164 Uiso 1 1 calc R . . C21 C 0.7650(3) 0.8036(3) 0.5803(3) 0.1092(14) Uani 1 1 d . . . H21A H 0.7425 0.8115 0.6114 0.164 Uiso 1 1 calc R . . H21B H 0.7765 0.8427 0.5648 0.164 Uiso 1 1 calc R . . H21C H 0.8021 0.7799 0.5878 0.164 Uiso 1 1 calc R . . C22 C 0.7131(3) 0.7059(3) 0.5682(3) 0.1092(14) Uani 1 1 d . . . H22A H 0.7519 0.6834 0.5712 0.164 Uiso 1 1 calc R . . H22B H 0.6847 0.6827 0.5471 0.164 Uiso 1 1 calc R . . H22C H 0.6951 0.7114 0.6014 0.164 Uiso 1 1 calc R . . C23 C 0.5558(3) 0.9301(3) 0.2926(2) 0.0916(19) Uani 1 1 d . . . H23A H 0.5393 0.8906 0.3039 0.137 Uiso 1 1 calc R . . H23B H 0.5953 0.9235 0.2759 0.137 Uiso 1 1 calc R . . H23C H 0.5269 0.9491 0.2692 0.137 Uiso 1 1 calc R . . C24 C 0.6076(3) 1.0537(3) 0.3248(2) 0.0848(17) Uani 1 1 d . . . H24A H 0.5858 1.0696 0.2956 0.127 Uiso 1 1 calc R . . H24B H 0.6498 1.0432 0.3154 0.127 Uiso 1 1 calc R . . H24C H 0.6083 1.0850 0.3511 0.127 Uiso 1 1 calc R . . C25 C 0.6237(2) 0.9415(2) 0.39004(18) 0.0684(13) Uani 1 1 d . . . H25A H 0.6310 0.9657 0.4203 0.103 Uiso 1 1 calc R . . H25B H 0.6625 0.9361 0.3720 0.103 Uiso 1 1 calc R . . H25C H 0.6072 0.9013 0.3992 0.103 Uiso 1 1 calc R . . C26 C 0.4416(3) 0.8054(3) 0.6137(2) 0.106(2) Uani 1 1 d . . . H26A H 0.4868 0.8030 0.6166 0.127 Uiso 1 1 calc R . . H26B H 0.4274 0.7719 0.5916 0.127 Uiso 1 1 calc R . . C27 C 0.4123(4) 0.8004(4) 0.6638(2) 0.139(3) Uani 1 1 d D . . H27A H 0.3901 0.7609 0.6668 0.167 Uiso 1 1 calc R . . H27B H 0.4439 0.8022 0.6904 0.167 Uiso 1 1 calc R . . C28 C 0.3703(4) 0.8509(3) 0.6689(3) 0.137(3) Uani 1 1 d D . . H28A H 0.3743 0.8696 0.7024 0.165 Uiso 1 1 calc R . . H28B H 0.3275 0.8364 0.6647 0.165 Uiso 1 1 calc R . . C29 C 0.3855(4) 0.8958(3) 0.6302(2) 0.134(3) Uani 1 1 d D . . H29A H 0.3477 0.9116 0.6143 0.161 Uiso 1 1 calc R . . H29B H 0.4082 0.9308 0.6449 0.161 Uiso 1 1 calc R . . Li1 Li 0.4397(4) 0.9025(3) 0.5324(3) 0.063(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0337(3) 0.0359(3) 0.0356(2) 0.000 0.000 0.00061(19) Si1 0.0607(8) 0.0673(8) 0.0454(6) -0.0064(6) 0.0112(6) -0.0096(7) O1 0.0414(15) 0.0342(14) 0.0480(14) -0.0010(12) -0.0019(11) 0.0051(11) O2 0.114(3) 0.066(2) 0.073(2) 0.0194(18) 0.042(2) 0.029(2) N1 0.046(2) 0.0380(19) 0.0517(19) -0.0014(15) -0.0094(16) 0.0014(14) N2 0.043(3) 0.059(3) 0.034(3) 0.000 0.000 -0.004(2) C1 0.042(2) 0.038(2) 0.043(2) 0.0012(16) 0.0032(17) 0.0051(17) C2 0.044(2) 0.038(2) 0.044(2) 0.0020(16) 0.0018(18) 0.0024(16) C3 0.057(3) 0.038(2) 0.056(2) -0.0089(18) 0.000(2) 0.0050(19) C4 0.049(2) 0.043(2) 0.058(2) 0.002(2) -0.001(2) 0.0094(18) C5 0.053(3) 0.047(2) 0.049(2) -0.0026(19) -0.0100(19) 0.0038(19) C6 0.047(2) 0.034(2) 0.041(2) 0.0006(17) -0.0049(17) 0.0071(17) C7 0.052(3) 0.039(2) 0.045(2) -0.0013(17) -0.0111(19) 0.0021(18) C8 0.044(2) 0.042(2) 0.052(2) -0.0120(19) -0.0122(19) -0.0051(18) C9 0.063(3) 0.048(2) 0.067(3) 0.010(2) -0.019(2) -0.006(2) C10 0.077(4) 0.069(3) 0.076(3) 0.012(3) -0.016(3) -0.024(3) C11 0.051(3) 0.062(3) 0.080(3) -0.010(3) -0.002(3) -0.016(2) C12 0.043(3) 0.065(3) 0.087(3) -0.011(3) -0.011(2) -0.001(2) C13 0.049(3) 0.044(2) 0.059(3) -0.003(2) -0.015(2) 0.0017(18) C14 0.073(4) 0.103(5) 0.112(5) -0.016(4) 0.021(3) -0.027(3) C15 0.050(2) 0.041(2) 0.058(2) -0.0080(19) -0.004(2) 0.0028(19) C16 0.063(3) 0.049(3) 0.063(3) -0.017(2) -0.004(2) 0.002(2) C17 0.061(3) 0.056(3) 0.085(3) -0.016(2) 0.008(3) -0.012(2) C18 0.075(3) 0.057(3) 0.054(3) -0.009(2) -0.019(2) 0.002(2) C19 0.049(3) 0.047(3) 0.084(3) -0.013(2) -0.017(2) 0.009(2) C20 0.076(2) 0.100(3) 0.152(4) 0.017(3) -0.012(2) 0.032(2) C21 0.076(2) 0.100(3) 0.152(4) 0.017(3) -0.012(2) 0.032(2) C22 0.076(2) 0.100(3) 0.152(4) 0.017(3) -0.012(2) 0.032(2) C23 0.108(5) 0.106(5) 0.061(3) -0.028(3) 0.013(3) -0.001(4) C24 0.082(4) 0.095(4) 0.077(3) 0.011(3) 0.029(3) -0.023(3) C25 0.053(3) 0.070(3) 0.082(3) -0.017(3) 0.008(2) -0.001(2) C26 0.140(6) 0.100(5) 0.078(4) 0.029(3) 0.015(4) 0.050(4) C27 0.174(8) 0.152(7) 0.091(5) 0.054(5) 0.035(5) 0.087(6) C28 0.221(10) 0.106(5) 0.085(4) 0.029(4) 0.060(5) 0.047(6) C29 0.211(9) 0.094(5) 0.098(4) 0.032(4) 0.086(5) 0.057(6) Li1 0.067(5) 0.044(4) 0.077(5) 0.018(4) 0.032(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 Y1 O1 2.234(3) 11_564 ? Y1 O1 2.234(3) . ? Y1 N2 2.259(5) . ? Y1 N1 2.344(3) . ? Y1 N1 2.344(3) 11_564 ? Y1 Li1 3.042(7) . ? Y1 Li1 3.042(7) 11_564 ? Y1 Si1 3.4384(16) 11_564 ? Y1 Si1 3.4384(16) . ? Si1 N2 1.713(3) . ? Si1 C25 1.866(5) . ? Si1 C24 1.871(5) . ? Si1 C23 1.889(5) . ? O1 C1 1.368(4) . ? O1 Li1 1.825(7) . ? O2 C26 1.433(6) . ? O2 C29 1.436(6) . ? O2 Li1 1.855(8) . ? N1 C8 1.396(5) . ? N1 C7 1.472(5) . ? N1 Li1 2.060(8) 11_564 ? N2 Si1 1.713(3) 11_564 ? C1 C6 1.393(5) . ? C1 C2 1.413(5) . ? C1 Li1 2.762(9) . ? C2 C3 1.397(5) . ? C2 C15 1.546(5) . ? C3 C4 1.398(6) . ? C3 H3 0.9400 . ? C4 C5 1.376(5) . ? C4 C19 1.533(6) . ? C5 C6 1.380(6) . ? C5 H5 0.9400 . ? C6 C7 1.536(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.402(5) . ? C8 C13 1.410(5) . ? C8 Li1 2.505(9) 11_564 ? C9 C10 1.369(6) . ? C9 Li1 2.697(10) 11_564 ? C9 H9 0.9400 . ? C10 C11 1.378(7) . ? C10 H10 0.9400 . ? C11 C12 1.384(7) . ? C11 C14 1.507(6) . ? C12 C13 1.378(6) . ? C12 H12 0.9400 . ? C13 H13 0.9400 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 C18 1.521(6) . ? C15 C16 1.531(5) . ? C15 C17 1.544(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 C21 1.489(8) . ? C19 C22 1.489(8) . ? C19 C20 1.529(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 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 C27 1.477(8) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.422(8) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.449(8) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? Li1 N1 2.060(8) 11_564 ? Li1 C8 2.505(9) 11_564 ? Li1 C9 2.697(10) 11_564 ? 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 146.93(14) 11_564 . ? O1 Y1 N2 106.53(7) 11_564 . ? O1 Y1 N2 106.53(7) . . ? O1 Y1 N1 79.03(10) 11_564 . ? O1 Y1 N1 81.93(10) . . ? N2 Y1 N1 125.53(9) . . ? O1 Y1 N1 81.93(10) 11_564 11_564 ? O1 Y1 N1 79.03(10) . 11_564 ? N2 Y1 N1 125.53(9) . 11_564 ? N1 Y1 N1 108.94(18) . 11_564 ? O1 Y1 Li1 118.13(17) 11_564 . ? O1 Y1 Li1 36.60(16) . . ? N2 Y1 Li1 125.60(16) . . ? N1 Y1 Li1 93.44(19) . . ? N1 Y1 Li1 42.56(17) 11_564 . ? O1 Y1 Li1 36.60(16) 11_564 11_564 ? O1 Y1 Li1 118.13(17) . 11_564 ? N2 Y1 Li1 125.60(16) . 11_564 ? N1 Y1 Li1 42.56(17) . 11_564 ? N1 Y1 Li1 93.44(19) 11_564 11_564 ? Li1 Y1 Li1 108.8(3) . 11_564 ? O1 Y1 Si1 97.41(7) 11_564 11_564 ? O1 Y1 Si1 112.55(7) . 11_564 ? N2 Y1 Si1 25.77(3) . 11_564 ? N1 Y1 Si1 148.94(10) . 11_564 ? N1 Y1 Si1 100.96(9) 11_564 11_564 ? Li1 Y1 Si1 114.75(17) . 11_564 ? Li1 Y1 Si1 129.04(15) 11_564 11_564 ? O1 Y1 Si1 112.55(7) 11_564 . ? O1 Y1 Si1 97.41(7) . . ? N2 Y1 Si1 25.77(3) . . ? N1 Y1 Si1 100.96(9) . . ? N1 Y1 Si1 148.94(10) 11_564 . ? Li1 Y1 Si1 129.04(15) . . ? Li1 Y1 Si1 114.75(17) 11_564 . ? Si1 Y1 Si1 51.54(5) 11_564 . ? N2 Si1 C25 111.7(2) . . ? N2 Si1 C24 112.6(2) . . ? C25 Si1 C24 106.5(3) . . ? N2 Si1 C23 113.9(2) . . ? C25 Si1 C23 105.0(3) . . ? C24 Si1 C23 106.6(3) . . ? N2 Si1 Y1 34.98(15) . . ? C25 Si1 Y1 78.38(15) . . ? C24 Si1 Y1 114.45(18) . . ? C23 Si1 Y1 136.01(19) . . ? C1 O1 Li1 119.1(3) . . ? C1 O1 Y1 129.0(2) . . ? Li1 O1 Y1 96.5(2) . . ? C26 O2 C29 109.0(4) . . ? C26 O2 Li1 131.6(4) . . ? C29 O2 Li1 119.3(4) . . ? C8 N1 C7 116.7(3) . . ? C8 N1 Li1 90.8(3) . 11_564 ? C7 N1 Li1 122.0(3) . 11_564 ? C8 N1 Y1 126.0(3) . . ? C7 N1 Y1 109.7(2) . . ? Li1 N1 Y1 87.1(2) 11_564 . ? Si1 N2 Si1 121.5(3) 11_564 . ? Si1 N2 Y1 119.25(15) 11_564 . ? Si1 N2 Y1 119.25(15) . . ? O1 C1 C6 118.2(3) . . ? O1 C1 C2 122.2(3) . . ? C6 C1 C2 119.5(3) . . ? O1 C1 Li1 35.3(2) . . ? C6 C1 Li1 108.0(3) . . ? C2 C1 Li1 119.5(3) . . ? C3 C2 C1 117.0(4) . . ? C3 C2 C15 121.0(3) . . ? C1 C2 C15 122.0(3) . . ? C2 C3 C4 124.0(4) . . ? C2 C3 H3 118.0 . . ? C4 C3 H3 118.0 . . ? C5 C4 C3 116.7(4) . . ? C5 C4 C19 123.3(4) . . ? C3 C4 C19 120.0(4) . . ? C4 C5 C6 121.9(4) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 120.8(4) . . ? C5 C6 C7 120.8(3) . . ? C1 C6 C7 118.3(3) . . ? N1 C7 C6 115.0(3) . . ? N1 C7 H7A 108.5 . . ? C6 C7 H7A 108.5 . . ? N1 C7 H7B 108.5 . . ? C6 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? N1 C8 C9 118.3(4) . . ? N1 C8 C13 125.9(4) . . ? C9 C8 C13 115.8(4) . . ? N1 C8 Li1 55.3(3) . 11_564 ? C9 C8 Li1 82.1(3) . 11_564 ? C13 C8 Li1 134.0(3) . 11_564 ? C10 C9 C8 121.8(4) . . ? C10 C9 Li1 142.0(4) . 11_564 ? C8 C9 Li1 66.9(3) . 11_564 ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? Li1 C9 H9 66.0 11_564 . ? C9 C10 C11 122.8(5) . . ? C9 C10 H10 118.6 . . ? C11 C10 H10 118.6 . . ? C10 C11 C12 115.6(4) . . ? C10 C11 C14 122.6(5) . . ? C12 C11 C14 121.9(5) . . ? C13 C12 C11 123.4(4) . . ? C13 C12 H12 118.3 . . ? C11 C12 H12 118.3 . . ? C12 C13 C8 120.5(4) . . ? C12 C13 H13 119.8 . . ? C8 C13 H13 119.8 . . ? 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 . . ? C18 C15 C16 107.5(3) . . ? C18 C15 C17 110.1(4) . . ? C16 C15 C17 106.3(4) . . ? C18 C15 C2 110.8(3) . . ? C16 C15 C2 112.2(3) . . ? C17 C15 C2 109.9(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 . . ? C21 C19 C22 107.8(5) . . ? C21 C19 C20 108.5(5) . . ? C22 C19 C20 107.3(5) . . ? C21 C19 C4 111.6(4) . . ? C22 C19 C4 113.0(4) . . ? C20 C19 C4 108.5(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 . . ? 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 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O2 C26 C27 106.3(5) . . ? O2 C26 H26A 110.5 . . ? C27 C26 H26A 110.5 . . ? O2 C26 H26B 110.5 . . ? C27 C26 H26B 110.5 . . ? H26A C26 H26B 108.7 . . ? C28 C27 C26 107.6(5) . . ? C28 C27 H27A 110.2 . . ? C26 C27 H27A 110.2 . . ? C28 C27 H27B 110.2 . . ? C26 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? C27 C28 C29 107.5(6) . . ? C27 C28 H28A 110.2 . . ? C29 C28 H28A 110.2 . . ? C27 C28 H28B 110.2 . . ? C29 C28 H28B 110.2 . . ? H28A C28 H28B 108.5 . . ? O2 C29 C28 106.9(5) . . ? O2 C29 H29A 110.3 . . ? C28 C29 H29A 110.3 . . ? O2 C29 H29B 110.3 . . ? C28 C29 H29B 110.3 . . ? H29A C29 H29B 108.6 . . ? O1 Li1 O2 133.2(5) . . ? O1 Li1 N1 97.0(3) . 11_564 ? O2 Li1 N1 122.2(4) . 11_564 ? O1 Li1 C8 113.0(3) . 11_564 ? O2 Li1 C8 113.7(4) . 11_564 ? N1 Li1 C8 33.88(18) 11_564 11_564 ? O1 Li1 C9 98.1(3) . 11_564 ? O2 Li1 C9 122.7(4) . 11_564 ? N1 Li1 C9 58.8(2) 11_564 11_564 ? C8 Li1 C9 30.98(16) 11_564 11_564 ? O1 Li1 C1 25.64(16) . . ? O2 Li1 C1 107.6(4) . . ? N1 Li1 C1 118.0(3) 11_564 . ? C8 Li1 C1 138.6(3) 11_564 . ? C9 Li1 C1 120.8(3) 11_564 . ? O1 Li1 Y1 46.88(17) . . ? O2 Li1 Y1 153.8(4) . . ? N1 Li1 Y1 50.33(17) 11_564 . ? C8 Li1 Y1 73.9(2) 11_564 . ? C9 Li1 Y1 77.4(2) 11_564 . ? C1 Li1 Y1 68.45(17) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.381 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.047 #===================================================end of CIF