Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Xie, Zuowei' 'Chan, Hoi-Shan' 'Li, Hung-Wing' _publ_contact_author_name 'Prof Zuowei Xie' _publ_contact_author_address ; Chemistry Chinese University of Hong Kong Shatin NT Hong Kong CHINA ; _publ_contact_author_email 'ZXIE@CUHK.EDU.HK' _publ_section_title ; Synthesis and structural characterization of imido-lanthanide complexes with a metal-nitrogen multiple bond ; data_complex_1 _database_code_CSD 175639 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H80 N4 Na O Yb' _chemical_formula_weight 973.23 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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 24.5164(11) _cell_length_b 19.8148(10) _cell_length_c 24.5415(12) _cell_angle_alpha 90.00 _cell_angle_beta 117.6830(10) _cell_angle_gamma 90.00 _cell_volume 10557.3(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4072 _exptl_absorpt_coefficient_mu 1.817 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.7206 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58633 _diffrn_reflns_av_R_equivalents 0.0860 _diffrn_reflns_av_sigmaI/netI 0.1324 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.00 _reflns_number_total 18578 _reflns_number_gt 8502 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000042(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 18578 _refine_ls_number_parameters 1067 _refine_ls_number_restraints 189 _refine_ls_R_factor_all 0.1206 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.0927 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 0.809 _refine_ls_restrained_S_all 0.817 _refine_ls_shift/su_max 0.00 _refine_ls_shift/su_mean 0.00 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 0.225253(3) 0.289137(5) 0.247165(4) 0.05793(3) Uani 1 1 d . C . Yb1' Yb 0.786184(4) 0.083805(5) 0.247975(4) 0.05972(3) Uani 1 1 d . . . N1 N 0.20645(6) 0.25135(9) 0.15350(6) 0.0755(7) Uani 1 1 d . C . N1' N 0.70027(6) 0.13979(9) 0.18730(7) 0.0794(7) Uani 1 1 d . . . N2 N 0.15080(6) 0.36061(8) 0.22207(6) 0.0713(6) Uani 1 1 d . . . H2A H 0.1387 0.3706 0.1841 0.086 Uiso 1 1 calc R . . N2' N 0.77121(6) 0.00277(8) 0.18316(6) 0.0675(6) Uani 1 1 d . . . H2'A H 0.7324 -0.0059 0.1652 0.081 Uiso 1 1 calc R . . N3' N 0.81740(6) 0.06897(8) 0.34590(6) 0.0731(7) Uani 1 1 d . . . H3'A H 0.8570 0.0708 0.3638 0.088 Uiso 1 1 calc R . . N3 N 0.31763(6) 0.31322(8) 0.31694(6) 0.0735(7) Uani 1 1 d . . . H3A H 0.3231 0.2916 0.3495 0.088 Uiso 1 1 calc R . . N4 N 0.22162(6) 0.18452(8) 0.28419(6) 0.0687(6) Uani 1 1 d . C . N4' N 0.85329(6) 0.16349(9) 0.25645(7) 0.0780(7) Uani 1 1 d . . . C1 C 0.24147(7) 0.24978(10) 0.12074(8) 0.0661(7) Uani 1 1 d . . . C1' C 0.64880(8) 0.16677(11) 0.19133(9) 0.0825(9) Uani 1 1 d . . . C2 C 0.21573(8) 0.27743(11) 0.06072(8) 0.0769(8) Uani 1 1 d . . . C2' C 0.58858(9) 0.15028(12) 0.14568(11) 0.1060(12) Uani 1 1 d . B . C3 C 0.25083(9) 0.27530(12) 0.02977(9) 0.1103(10) Uani 1 1 d . . . H3B H 0.2343 0.2928 -0.0099 0.132 Uiso 1 1 calc R . . C3' C 0.53871(11) 0.17990(16) 0.14832(14) 0.1600(17) Uani 1 1 d . . . H3'B H 0.4990 0.1700 0.1181 0.192 Uiso 1 1 calc R . . C4 C 0.30839(9) 0.24854(14) 0.05534(10) 0.1321(11) Uani 1 1 d . . . H4A H 0.3311 0.2495 0.0338 0.159 Uiso 1 1 calc R . . C4' C 0.54684(11) 0.22393(16) 0.19507(14) 0.1705(17) Uani 1 1 d . . . H4'A H 0.5131 0.2435 0.1965 0.205 Uiso 1 1 calc R . . C5 C 0.33332(9) 0.21990(13) 0.11315(9) 0.1113(10) Uani 1 1 d . . . H5A H 0.3722 0.2003 0.1300 0.134 Uiso 1 1 calc R . . C5' C 0.60580(10) 0.23847(14) 0.23951(13) 0.1481(14) Uani 1 1 d . . . H5'A H 0.6110 0.2677 0.2712 0.178 Uiso 1 1 calc R . . C6 C 0.30011(8) 0.22053(11) 0.14586(8) 0.0810(8) Uani 1 1 d . . . C6' C 0.65734(8) 0.21156(11) 0.23901(10) 0.0888(10) Uani 1 1 d . . . C7 C 0.15242(9) 0.30913(12) 0.03119(9) 0.0961(10) Uani 1 1 d . . . H7A H 0.1259 0.2821 0.0427 0.115 Uiso 1 1 calc R . . C7' C 0.57939(11) 0.09798(16) 0.09596(13) 0.1539(16) Uani 1 1 d . . . H7'A H 0.6175 0.0718 0.1175 0.185 Uiso 1 1 calc R A 1 C8 C 0.15373(9) 0.38007(12) 0.05401(10) 0.1163(12) Uani 1 1 d . . . H8A H 0.1724 0.3799 0.0981 0.174 Uiso 1 1 calc R . . H8B H 0.1124 0.3970 0.0375 0.174 Uiso 1 1 calc R . . H8C H 0.1772 0.4084 0.0409 0.174 Uiso 1 1 calc R . . C8' C 0.5857(2) 0.1213(3) 0.0406(2) 0.146(2) Uiso 0.50 1 d P B 1 H8'A H 0.5684 0.0879 0.0087 0.219 Uiso 0.50 1 calc PR B 1 H8'B H 0.6285 0.1275 0.0520 0.219 Uiso 0.50 1 calc PR B 1 H8'C H 0.5642 0.1632 0.0260 0.219 Uiso 0.50 1 calc PR B 1 C8A C 0.5340(3) 0.1287(5) 0.0335(4) 0.279(5) Uiso 0.50 1 d P B 2 H8'D H 0.5349 0.1028 0.0009 0.419 Uiso 0.50 1 calc PR B 2 H8'E H 0.5458 0.1744 0.0312 0.419 Uiso 0.50 1 calc PR B 2 H8'F H 0.4932 0.1281 0.0295 0.419 Uiso 0.50 1 calc PR B 2 C9 C 0.12170(12) 0.31215(15) -0.03970(10) 0.1544(16) Uani 1 1 d . . . H9A H 0.0819 0.3328 -0.0550 0.232 Uiso 1 1 calc R . . H9B H 0.1173 0.2672 -0.0559 0.232 Uiso 1 1 calc R . . H9C H 0.1469 0.3383 -0.0523 0.232 Uiso 1 1 calc R . . C9' C 0.53331(16) 0.04556(18) 0.08837(15) 0.266(3) Uani 1 1 d . B . H9'A H 0.5315 0.0128 0.0587 0.399 Uiso 1 1 calc R . . H9'B H 0.4936 0.0662 0.0743 0.399 Uiso 1 1 calc R . . H9'C H 0.5450 0.0237 0.1271 0.399 Uiso 1 1 calc R . . C10 C 0.32887(8) 0.18566(12) 0.20752(10) 0.0987(10) Uani 1 1 d . . . H10A H 0.3050 0.1991 0.2286 0.118 Uiso 1 1 calc R . . C10' C 0.72024(9) 0.22993(12) 0.28935(9) 0.0959(10) Uani 1 1 d . . . H10B H 0.7503 0.2008 0.2850 0.115 Uiso 1 1 calc R . . C11 C 0.39589(9) 0.20458(14) 0.25000(11) 0.1417(14) Uani 1 1 d . . . H11A H 0.3994 0.2527 0.2546 0.213 Uiso 1 1 calc R . . H11B H 0.4214 0.1889 0.2325 0.213 Uiso 1 1 calc R . . H11C H 0.4090 0.1840 0.2895 0.213 Uiso 1 1 calc R . . C11' C 0.72760(11) 0.21993(12) 0.35331(10) 0.1332(13) Uani 1 1 d . . . H11D H 0.7187 0.1738 0.3583 0.200 Uiso 1 1 calc R . . H11E H 0.6997 0.2492 0.3594 0.200 Uiso 1 1 calc R . . H11F H 0.7691 0.2304 0.3830 0.200 Uiso 1 1 calc R . . C12 C 0.32575(10) 0.10785(13) 0.20280(11) 0.1337(14) Uani 1 1 d . C . H12A H 0.2841 0.0941 0.1762 0.201 Uiso 1 1 calc R . . H12B H 0.3390 0.0888 0.2430 0.201 Uiso 1 1 calc R . . H12E H 0.3521 0.0922 0.1863 0.201 Uiso 1 1 calc R . . C12' C 0.73511(9) 0.30321(12) 0.28067(10) 0.1162(12) Uani 1 1 d . . . H12C H 0.7304 0.3088 0.2399 0.174 Uiso 1 1 calc R . . H12D H 0.7768 0.3135 0.3102 0.174 Uiso 1 1 calc R . . H12F H 0.7075 0.3331 0.2865 0.174 Uiso 1 1 calc R . . C13 C 0.11325(7) 0.39822(10) 0.24075(8) 0.0606(8) Uani 1 1 d . . . C13' C 0.79856(7) -0.04126(10) 0.15845(8) 0.0606(7) Uani 1 1 d . . . C14 C 0.12251(7) 0.39017(10) 0.30091(8) 0.0674(8) Uani 1 1 d . . . C14' C 0.86201(7) -0.05588(10) 0.19265(8) 0.0675(8) Uani 1 1 d . . . C15 C 0.08705(8) 0.42845(11) 0.31992(9) 0.0897(10) Uani 1 1 d . . . H15A H 0.0935 0.4239 0.3602 0.108 Uiso 1 1 calc R . . C15' C 0.88871(8) -0.10002(11) 0.16950(9) 0.0830(9) Uani 1 1 d . . . H15B H 0.9304 -0.1099 0.1926 0.100 Uiso 1 1 calc R . . C16 C 0.04322(8) 0.47245(13) 0.28198(10) 0.1068(10) Uani 1 1 d . . . H16A H 0.0200 0.4972 0.2960 0.128 Uiso 1 1 calc R . . C16' C 0.85622(9) -0.12999(11) 0.11363(9) 0.0982(9) Uani 1 1 d . . . H16B H 0.8752 -0.1608 0.0993 0.118 Uiso 1 1 calc R . . C17 C 0.03396(8) 0.47959(12) 0.22264(9) 0.0935(10) Uani 1 1 d . . . H17A H 0.0038 0.5092 0.1963 0.112 Uiso 1 1 calc R . . C17' C 0.79497(8) -0.11412(11) 0.07855(9) 0.0942(10) Uani 1 1 d . . . H17B H 0.7730 -0.1337 0.0399 0.113 Uiso 1 1 calc R . . C18 C 0.06816(8) 0.44397(11) 0.20119(8) 0.0736(9) Uani 1 1 d D . . C18' C 0.76528(8) -0.06952(11) 0.09955(8) 0.0755(8) Uani 1 1 d D . . C19 C 0.17024(8) 0.34187(12) 0.34577(8) 0.0854(9) Uani 1 1 d . . . H19A H 0.1790 0.3082 0.3217 0.103 Uiso 1 1 calc R . . C19' C 0.89858(8) -0.02495(11) 0.25562(9) 0.0815(9) Uani 1 1 d . . . H19B H 0.8802 0.0193 0.2546 0.098 Uiso 1 1 calc R . . C20 C 0.22876(9) 0.38020(15) 0.38376(11) 0.1396(15) Uani 1 1 d . . . H20A H 0.2413 0.4034 0.3570 0.209 Uiso 1 1 calc R . . H20B H 0.2605 0.3493 0.4094 0.209 Uiso 1 1 calc R . . H20C H 0.2219 0.4124 0.4091 0.209 Uiso 1 1 calc R . . C20' C 0.96733(9) -0.01276(15) 0.27611(12) 0.1633(16) Uani 1 1 d . . . H20D H 0.9717 0.0139 0.2457 0.245 Uiso 1 1 calc R . . H20E H 0.9878 -0.0553 0.2807 0.245 Uiso 1 1 calc R . . H20F H 0.9855 0.0108 0.3147 0.245 Uiso 1 1 calc R . . C21 C 0.15020(10) 0.30411(13) 0.38796(9) 0.1243(12) Uani 1 1 d . . . H21A H 0.1137 0.2784 0.3634 0.186 Uiso 1 1 calc R . . H21B H 0.1417 0.3360 0.4125 0.186 Uiso 1 1 calc R . . H21C H 0.1826 0.2743 0.4144 0.186 Uiso 1 1 calc R . . C21' C 0.89569(10) -0.06379(14) 0.30558(10) 0.1348(14) Uani 1 1 d . . . H21D H 0.8534 -0.0712 0.2957 0.202 Uiso 1 1 calc R . . H21E H 0.9159 -0.0390 0.3434 0.202 Uiso 1 1 calc R . . H21F H 0.9159 -0.1065 0.3101 0.202 Uiso 1 1 calc R . . C22 C 0.05586(9) 0.45303(10) 0.13484(9) 0.0911(10) Uani 1 1 d D . . H22A H 0.0954 0.4486 0.1343 0.109 Uiso 1 1 calc R . . C22' C 0.69842(8) -0.05045(12) 0.05894(8) 0.0966(10) Uani 1 1 d D . . H22B H 0.6919 -0.0057 0.0720 0.116 Uiso 1 1 calc R . . C23 C 0.02833(12) 0.52049(12) 0.10590(11) 0.1706(17) Uani 1 1 d D . . H23A H 0.0220 0.5215 0.0642 0.256 Uiso 1 1 calc R . . H23B H 0.0560 0.5561 0.1289 0.256 Uiso 1 1 calc R . . H23C H -0.0104 0.5266 0.1062 0.256 Uiso 1 1 calc R . . C23' C 0.65585(9) -0.09844(14) 0.06733(11) 0.1609(15) Uani 1 1 d D . . H23D H 0.6665 -0.1010 0.1102 0.241 Uiso 1 1 calc R . . H23E H 0.6596 -0.1423 0.0528 0.241 Uiso 1 1 calc R . . H23F H 0.6142 -0.0828 0.0444 0.241 Uiso 1 1 calc R . . C24 C 0.01442(12) 0.39862(14) 0.09458(11) 0.1792(17) Uani 1 1 d D . . H24A H 0.0315 0.3553 0.1114 0.269 Uiso 1 1 calc R . . H24B H 0.0107 0.4026 0.0540 0.269 Uiso 1 1 calc R . . H24C H -0.0255 0.4030 0.0924 0.269 Uiso 1 1 calc R . . C24' C 0.67930(11) -0.04657(16) -0.00845(10) 0.1546(16) Uani 1 1 d D . . H24D H 0.6367 -0.0340 -0.0304 0.232 Uiso 1 1 calc R . . H24E H 0.6851 -0.0898 -0.0227 0.232 Uiso 1 1 calc R . . H24F H 0.7039 -0.0134 -0.0155 0.232 Uiso 1 1 calc R . . C25 C 0.37212(7) 0.34828(10) 0.33237(8) 0.0591(7) Uani 1 1 d . . . C25' C 0.79983(7) 0.05778(10) 0.39158(8) 0.0675(8) Uani 1 1 d . . . C26 C 0.37546(7) 0.39334(11) 0.28976(8) 0.0681(8) Uani 1 1 d . . . C26' C 0.83963(9) 0.06606(12) 0.45528(9) 0.0878(9) Uani 1 1 d . . . C27 C 0.42882(8) 0.42955(11) 0.30462(9) 0.0905(9) Uani 1 1 d . . . H27A H 0.4308 0.4597 0.2765 0.109 Uiso 1 1 calc R . . C27' C 0.81718(9) 0.05528(13) 0.49642(9) 0.1106(11) Uani 1 1 d . . . H27B H 0.8432 0.0620 0.5381 0.133 Uiso 1 1 calc R . . C28 C 0.47912(9) 0.42043(13) 0.36171(10) 0.1073(11) Uani 1 1 d . . . H28A H 0.5150 0.4450 0.3721 0.129 Uiso 1 1 calc R . . C28' C 0.75907(9) 0.03546(12) 0.47867(9) 0.1133(10) Uani 1 1 d . . . H28B H 0.7460 0.0273 0.5081 0.136 Uiso 1 1 calc R . . C29 C 0.47681(9) 0.37620(13) 0.40264(10) 0.1059(12) Uani 1 1 d . . . H29A H 0.5116 0.3706 0.4404 0.127 Uiso 1 1 calc R . . C29' C 0.71878(8) 0.02706(11) 0.41765(9) 0.0980(9) Uani 1 1 d . . . H29B H 0.6783 0.0143 0.4059 0.118 Uiso 1 1 calc R . . C30 C 0.42531(8) 0.33954(11) 0.39059(8) 0.0777(9) Uani 1 1 d D . . C30' C 0.73813(8) 0.03752(11) 0.37277(8) 0.0766(8) Uani 1 1 d D . . C31' C 0.90598(10) 0.08774(14) 0.47558(10) 0.1256(13) Uani 1 1 d . . . H31A H 0.9197 0.0688 0.4471 0.151 Uiso 1 1 calc R . . C31 C 0.32035(8) 0.40470(12) 0.22652(9) 0.0922(10) Uani 1 1 d . . . H31B H 0.2955 0.3635 0.2168 0.111 Uiso 1 1 calc R . . C32 C 0.33593(10) 0.41499(14) 0.17495(9) 0.1480(12) Uani 1 1 d . . . H32A H 0.2987 0.4207 0.1371 0.222 Uiso 1 1 calc R . . H32B H 0.3580 0.3764 0.1718 0.222 Uiso 1 1 calc R . . H32C H 0.3611 0.4545 0.1829 0.222 Uiso 1 1 calc R . . C32' C 0.94903(14) 0.0648(2) 0.54000(14) 0.280(3) Uani 1 1 d . . . H32D H 0.9900 0.0800 0.5511 0.421 Uiso 1 1 calc R . . H32E H 0.9486 0.0164 0.5419 0.421 Uiso 1 1 calc R . . H32F H 0.9359 0.0834 0.5681 0.421 Uiso 1 1 calc R . . C33 C 0.28089(9) 0.46019(13) 0.23015(10) 0.1201(13) Uani 1 1 d . . . H33A H 0.2458 0.4663 0.1906 0.180 Uiso 1 1 calc R . . H33B H 0.3043 0.5013 0.2424 0.180 Uiso 1 1 calc R . . H33C H 0.2672 0.4486 0.2598 0.180 Uiso 1 1 calc R . . C33' C 0.91048(11) 0.16152(17) 0.47540(15) 0.226(2) Uani 1 1 d . . . H33D H 0.8831 0.1784 0.4352 0.339 Uiso 1 1 calc R . . H33E H 0.9520 0.1743 0.4860 0.339 Uiso 1 1 calc R . . H33F H 0.8993 0.1802 0.5049 0.339 Uiso 1 1 calc R . . C34 C 0.42372(10) 0.28980(10) 0.43732(9) 0.1035(12) Uani 1 1 d D . . H34A H 0.3821 0.2901 0.4335 0.124 Uiso 1 1 calc R . . C34' C 0.69487(8) 0.02830(11) 0.30659(9) 0.1011(10) Uani 1 1 d D . . H34B H 0.7042 0.0634 0.2840 0.121 Uiso 1 1 calc R . . C35' C 0.62673(8) 0.03386(14) 0.28832(11) 0.1458(14) Uani 1 1 d D . . H35A H 0.6186 0.0771 0.3007 0.219 Uiso 1 1 calc R . . H35B H 0.6155 -0.0012 0.3082 0.219 Uiso 1 1 calc R . . H35C H 0.6031 0.0292 0.2445 0.219 Uiso 1 1 calc R . . C35 C 0.46845(15) 0.30499(16) 0.50292(11) 0.209(2) Uani 1 1 d D . . H35D H 0.4640 0.2722 0.5293 0.314 Uiso 1 1 calc R . . H35E H 0.4604 0.3492 0.5135 0.314 Uiso 1 1 calc R . . H35F H 0.5097 0.3033 0.5080 0.314 Uiso 1 1 calc R . . C36 C 0.43690(12) 0.22081(12) 0.42351(13) 0.1756(18) Uani 1 1 d D . . H36A H 0.4345 0.1896 0.4522 0.263 Uiso 1 1 calc R . . H36B H 0.4775 0.2195 0.4269 0.263 Uiso 1 1 calc R . . H36C H 0.4072 0.2086 0.3825 0.263 Uiso 1 1 calc R . . C36' C 0.70512(9) -0.04049(12) 0.28321(9) 0.1291(12) Uani 1 1 d D . . H36D H 0.7477 -0.0448 0.2929 0.194 Uiso 1 1 calc R . . H36E H 0.6799 -0.0432 0.2395 0.194 Uiso 1 1 calc R . . H36F H 0.6942 -0.0762 0.3028 0.194 Uiso 1 1 calc R . . C37 C 0.18705(7) 0.15766(9) 0.31121(7) 0.0511(7) Uani 1 1 d . . . C37' C 0.86998(7) 0.21106(10) 0.22632(8) 0.0622(7) Uani 1 1 d . . . C38' C 0.90252(7) 0.26977(10) 0.25809(8) 0.0645(8) Uani 1 1 d . . . C39 C 0.08959(8) 0.12285(11) 0.30443(8) 0.0815(9) Uani 1 1 d . . . H39A H 0.0468 0.1212 0.2829 0.098 Uiso 1 1 calc R . . C39' C 0.91506(8) 0.32006(11) 0.22764(9) 0.0843(9) Uani 1 1 d . . . H39B H 0.9373 0.3578 0.2490 0.101 Uiso 1 1 calc R . . C40 C 0.12015(8) 0.09440(11) 0.36257(9) 0.0844(9) Uani 1 1 d . . . H40A H 0.0982 0.0716 0.3793 0.101 Uiso 1 1 calc R . . C40' C 0.89464(8) 0.31503(11) 0.16457(9) 0.0887(9) Uani 1 1 d . . . H40B H 0.9007 0.3508 0.1434 0.106 Uiso 1 1 calc R . . C41 C 0.18262(8) 0.10013(11) 0.39502(9) 0.0824(9) Uani 1 1 d . . . H41A H 0.2025 0.0825 0.4347 0.099 Uiso 1 1 calc R . . C41' C 0.86598(8) 0.25828(11) 0.13391(9) 0.0855(9) Uani 1 1 d . . . H41B H 0.8551 0.2542 0.0924 0.103 Uiso 1 1 calc R . . C42 C 0.21768(7) 0.13124(10) 0.37122(8) 0.0572(7) Uani 1 1 d . . . C42' C 0.85254(7) 0.20612(11) 0.16341(8) 0.0665(8) Uani 1 1 d . . . C38 C 0.12232(7) 0.15373(10) 0.27815(7) 0.0612(7) Uani 1 1 d D . . C43 C 0.08631(7) 0.18154(10) 0.21405(8) 0.0712(8) Uani 1 1 d D . . H43A H 0.1154 0.2066 0.2046 0.085 Uiso 1 1 calc R . . C44 C 0.06008(9) 0.12416(12) 0.16700(9) 0.1058(11) Uani 1 1 d D . . H44A H 0.0927 0.0941 0.1718 0.159 Uiso 1 1 calc R . . H44B H 0.0413 0.1426 0.1262 0.159 Uiso 1 1 calc R . . H44C H 0.0298 0.0998 0.1735 0.159 Uiso 1 1 calc R . . C45 C 0.03506(8) 0.22983(11) 0.20553(9) 0.0909(10) Uani 1 1 d D . . H45A H 0.0517 0.2663 0.2344 0.136 Uiso 1 1 calc R . . H45B H 0.0045 0.2063 0.2124 0.136 Uiso 1 1 calc R . . H45C H 0.0165 0.2475 0.1644 0.136 Uiso 1 1 calc R . . C43' C 0.92689(8) 0.27447(11) 0.32755(9) 0.0809(9) Uani 1 1 d . . . H43B H 0.8942 0.2575 0.3363 0.097 Uiso 1 1 calc R . . C44' C 0.94220(10) 0.34597(12) 0.35406(10) 0.1248(13) Uani 1 1 d . . . H44D H 0.9068 0.3744 0.3331 0.187 Uiso 1 1 calc R . . H44E H 0.9758 0.3635 0.3486 0.187 Uiso 1 1 calc R . . H44F H 0.9536 0.3448 0.3971 0.187 Uiso 1 1 calc R . . C45' C 0.98245(9) 0.22875(13) 0.36173(10) 0.1141(13) Uani 1 1 d . . . H45D H 0.9725 0.1838 0.3455 0.171 Uiso 1 1 calc R . . H45E H 0.9934 0.2282 0.4047 0.171 Uiso 1 1 calc R . . H45F H 1.0165 0.2454 0.3565 0.171 Uiso 1 1 calc R . . C46 C 0.28661(8) 0.13816(11) 0.41051(8) 0.0734(9) Uani 1 1 d . . . H46A H 0.2996 0.1762 0.3937 0.088 Uiso 1 1 calc R . . C46' C 0.82692(8) 0.14161(11) 0.12844(8) 0.0833(9) Uani 1 1 d . . . H46B H 0.8148 0.1137 0.1540 0.100 Uiso 1 1 calc R . . C47 C 0.31965(10) 0.07788(13) 0.40530(13) 0.1580(17) Uani 1 1 d . . . H47A H 0.3632 0.0844 0.4296 0.237 Uiso 1 1 calc R . . H47B H 0.3101 0.0713 0.3630 0.237 Uiso 1 1 calc R . . H47C H 0.3071 0.0389 0.4199 0.237 Uiso 1 1 calc R . . C47' C 0.76988(12) 0.14993(15) 0.06684(12) 0.1650(17) Uani 1 1 d . . . H47D H 0.7392 0.1746 0.0725 0.247 Uiso 1 1 calc R . . H47E H 0.7540 0.1063 0.0499 0.247 Uiso 1 1 calc R . . H47F H 0.7804 0.1742 0.0392 0.247 Uiso 1 1 calc R . . C48 C 0.30781(10) 0.15348(18) 0.47690(11) 0.1755(17) Uani 1 1 d . . . H48A H 0.3518 0.1579 0.4977 0.263 Uiso 1 1 calc R . . H48B H 0.2958 0.1175 0.4952 0.263 Uiso 1 1 calc R . . H48C H 0.2894 0.1949 0.4805 0.263 Uiso 1 1 calc R . . C48' C 0.87435(10) 0.10332(13) 0.12057(11) 0.1412(13) Uani 1 1 d . . . H48D H 0.9097 0.0970 0.1599 0.212 Uiso 1 1 calc R . . H48E H 0.8861 0.1279 0.0940 0.212 Uiso 1 1 calc R . . H48F H 0.8581 0.0601 0.1027 0.212 Uiso 1 1 calc R . . O1 O 0.16802(10) 0.06097(13) 0.10594(10) 0.1032(11) Uiso 0.50 1 d PD C 1 C51 C 0.17574(17) 0.07550(17) 0.05377(13) 0.135(2) Uiso 0.50 1 d PD C 1 H51A H 0.2181 0.0880 0.0661 0.162 Uiso 0.50 1 calc PR C 1 H51B H 0.1493 0.1127 0.0309 0.162 Uiso 0.50 1 calc PR C 1 C52 C 0.15958(14) 0.01537(18) 0.01632(15) 0.149(2) Uiso 0.50 1 d PD C 1 H52B H 0.1945 -0.0150 0.0297 0.179 Uiso 0.50 1 calc PR C 1 H52C H 0.1452 0.0265 -0.0267 0.179 Uiso 0.50 1 calc PR C 1 C53 C 0.11062(10) -0.01441(13) 0.02583(8) 0.1564(15) Uani 1 1 d D . . H53A H 0.1063 -0.0624 0.0171 0.188 Uiso 1 1 calc R C 1 H53B H 0.0714 0.0080 0.0019 0.188 Uiso 1 1 calc R C 1 C54 C 0.13637(17) -0.00019(18) 0.09200(14) 0.130(2) Uiso 0.50 1 d PD C 1 H54A H 0.1034 0.0019 0.1033 0.156 Uiso 0.50 1 calc PR C 1 H54B H 0.1642 -0.0362 0.1154 0.156 Uiso 0.50 1 calc PR C 1 O1A O 0.14563(9) 0.07674(12) 0.09302(9) 0.0652(8) Uiso 0.50 1 d PD C 2 C51A C 0.14988(15) 0.09255(17) 0.04055(13) 0.0896(15) Uiso 0.50 1 d PD C 2 H51E H 0.1906 0.1101 0.0514 0.107 Uiso 0.50 1 calc PR C 2 H51F H 0.1198 0.1269 0.0174 0.107 Uiso 0.50 1 calc PR C 2 C52A C 0.13869(16) 0.03272(18) 0.00414(15) 0.1046(18) Uiso 0.50 1 d PD C 2 H52E H 0.1119 0.0428 -0.0389 0.126 Uiso 0.50 1 calc PR C 2 H52F H 0.1772 0.0148 0.0080 0.126 Uiso 0.50 1 calc PR C 2 C54A C 0.10583(14) 0.02134(17) 0.07457(14) 0.0860(15) Uiso 0.50 1 d PD C 2 H54E H 0.0638 0.0366 0.0603 0.103 Uiso 0.50 1 calc PR C 2 H54F H 0.1163 -0.0087 0.1093 0.103 Uiso 0.50 1 calc PR C 2 O1' O 0.68839(6) 0.30636(9) 0.10403(7) 0.1485(8) Uani 1 1 d D . . C51' C 0.63143(14) 0.3289(2) 0.09706(16) 0.125(2) Uiso 0.50 1 d PD D 1 H51C H 0.6369 0.3496 0.1351 0.150 Uiso 0.50 1 calc PR D 1 H51D H 0.6038 0.2908 0.0884 0.150 Uiso 0.50 1 calc PR D 1 C52' C 0.60498(17) 0.3765(3) 0.0485(2) 0.265(4) Uiso 0.50 1 d PD D 1 H52A H 0.5678 0.3583 0.0150 0.318 Uiso 0.50 1 calc PR D 1 H52D H 0.5946 0.4177 0.0629 0.318 Uiso 0.50 1 calc PR D 1 C53' C 0.64781(14) 0.3891(2) 0.02929(16) 0.120(2) Uiso 0.50 1 d PD D 1 H53C H 0.6530 0.4372 0.0261 0.144 Uiso 0.50 1 calc PR D 1 H53D H 0.6365 0.3682 -0.0103 0.144 Uiso 0.50 1 calc PR D 1 C54' C 0.70161(15) 0.3600(2) 0.07570(18) 0.129(2) Uiso 0.50 1 d PD D 1 H54C H 0.7273 0.3442 0.0579 0.155 Uiso 0.50 1 calc PR D 1 H54D H 0.7245 0.3939 0.1063 0.155 Uiso 0.50 1 calc PR D 1 C51B C 0.62412(16) 0.2907(2) 0.0721(2) 0.181(3) Uiso 0.50 1 d PD D 2 H51G H 0.6177 0.2470 0.0521 0.218 Uiso 0.50 1 calc PR D 2 H51H H 0.6068 0.2896 0.1004 0.218 Uiso 0.50 1 calc PR D 2 C52B C 0.59651(14) 0.3413(2) 0.02851(16) 0.135(2) Uiso 0.50 1 d PD D 2 H52G H 0.5557 0.3287 -0.0028 0.162 Uiso 0.50 1 calc PR D 2 H52H H 0.5947 0.3839 0.0471 0.162 Uiso 0.50 1 calc PR D 2 C53B C 0.63838(15) 0.3426(3) 0.00625(17) 0.180(3) Uiso 0.50 1 d PD D 2 H53G H 0.6380 0.3867 -0.0112 0.217 Uiso 0.50 1 calc PR D 2 H53H H 0.6275 0.3091 -0.0260 0.217 Uiso 0.50 1 calc PR D 2 C54B C 0.69612(13) 0.3293(2) 0.05325(14) 0.1005(17) Uiso 0.50 1 d PD D 2 H54G H 0.7212 0.3698 0.0642 0.121 Uiso 0.50 1 calc PR D 2 H54H H 0.7163 0.2949 0.0408 0.121 Uiso 0.50 1 calc PR D 2 Na1' Na 0.75275(4) 0.24252(5) 0.17968(4) 0.1053(4) Uani 1 1 d . D . Na1 Na 0.19421(4) 0.13389(5) 0.18295(4) 0.0995(4) Uani 1 1 d . . . H4C H 0.2149(8) 0.2066(11) 0.2715(9) 0.150 Uiso 1 1 d . . . H4D H 0.8367(8) 0.1409(11) 0.2497(9) 0.150 Uiso 1 1 d . . . H1B H 0.7082(8) 0.1276(11) 0.1706(9) 0.150 Uiso 1 1 d . . . H1A H 0.2214(8) 0.2632(11) 0.1714(9) 0.150 Uiso 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 0.05050(4) 0.07216(6) 0.05182(4) 0.00593(5) 0.02435(3) 0.00008(5) Yb1' 0.06335(4) 0.06618(6) 0.04695(4) -0.00164(5) 0.02336(3) -0.00920(5) N1 0.0896(9) 0.0895(13) 0.0574(8) -0.0051(9) 0.0425(6) -0.0137(9) N1' 0.0831(9) 0.0860(14) 0.0664(9) -0.0096(10) 0.0323(7) -0.0070(9) N2 0.0752(8) 0.0934(14) 0.0520(8) -0.0020(9) 0.0351(5) -0.0011(9) N2' 0.0599(8) 0.0690(12) 0.0685(9) -0.0088(9) 0.0255(6) -0.0138(8) N3' 0.0577(8) 0.0995(14) 0.0567(9) 0.0074(9) 0.0220(6) -0.0078(9) N3 0.0653(8) 0.0901(13) 0.0601(9) 0.0145(9) 0.0248(6) -0.0081(9) N4 0.0641(7) 0.0887(13) 0.0595(8) 0.0120(9) 0.0339(5) -0.0018(8) N4' 0.0947(9) 0.0810(13) 0.0595(9) -0.0046(9) 0.0368(6) -0.0269(9) C1 0.0869(10) 0.0629(14) 0.0667(9) -0.0155(10) 0.0511(6) -0.0180(10) C1' 0.0759(12) 0.0744(16) 0.0828(14) 0.0040(13) 0.0246(9) 0.0069(12) C2 0.1122(11) 0.0692(16) 0.0631(10) -0.0158(11) 0.0524(7) -0.0210(11) C2' 0.0662(14) 0.0918(19) 0.1153(19) -0.0106(16) 0.0045(12) -0.0050(14) C3 0.1643(13) 0.121(2) 0.0800(11) -0.0159(13) 0.0862(8) -0.0117(15) C3' 0.0750(16) 0.165(3) 0.197(3) -0.007(3) 0.0271(16) 0.0101(18) C4 0.1666(12) 0.158(3) 0.1389(12) -0.0226(15) 0.1273(8) -0.0199(15) C4' 0.1006(16) 0.173(3) 0.233(3) -0.046(2) 0.0731(15) 0.0032(19) C5 0.1232(12) 0.136(2) 0.1091(12) -0.0147(15) 0.0828(8) 0.0052(14) C5' 0.0863(15) 0.128(2) 0.225(2) -0.056(2) 0.0680(14) -0.0030(15) C6 0.0873(10) 0.0915(18) 0.0800(11) -0.0202(12) 0.0523(7) -0.0115(12) C6' 0.0662(11) 0.0807(17) 0.1057(15) 0.0013(14) 0.0284(9) 0.0141(12) C7 0.1255(13) 0.103(2) 0.0670(12) 0.0126(13) 0.0505(9) -0.0116(13) C7' 0.0835(17) 0.195(3) 0.127(2) -0.036(2) 0.0019(16) -0.0327(19) C8 0.1295(15) 0.107(2) 0.1211(17) -0.0180(16) 0.0657(11) -0.0095(15) C9 0.206(2) 0.159(3) 0.0695(17) 0.0105(19) 0.0401(15) 0.018(2) C9' 0.410(5) 0.177(4) 0.219(3) -0.053(3) 0.152(3) -0.061(4) C10 0.0666(10) 0.135(2) 0.1005(13) -0.0120(14) 0.0439(8) 0.0187(12) C10' 0.1097(14) 0.0964(19) 0.0735(13) 0.0008(14) 0.0357(10) 0.0242(14) C11 0.0876(14) 0.198(3) 0.1322(19) -0.034(2) 0.0454(12) 0.0099(18) C11' 0.193(2) 0.099(2) 0.1081(17) 0.0005(16) 0.0705(13) 0.0428(17) C12 0.1183(17) 0.124(2) 0.146(2) 0.0302(19) 0.0505(14) 0.0343(17) C12' 0.1023(15) 0.113(2) 0.1215(17) -0.0476(16) 0.0418(12) -0.0248(15) C13 0.0498(9) 0.0603(14) 0.0644(11) -0.0013(10) 0.0204(7) -0.0003(9) C13' 0.0715(9) 0.0542(13) 0.0620(10) -0.0010(10) 0.0360(7) -0.0116(10) C14 0.0643(10) 0.0768(15) 0.0631(10) -0.0138(11) 0.0313(7) -0.0067(10) C14' 0.0700(10) 0.0674(15) 0.0714(11) 0.0005(11) 0.0382(7) -0.0127(10) C15 0.0833(11) 0.108(2) 0.0844(12) -0.0072(13) 0.0445(8) 0.0110(12) C15' 0.0792(10) 0.0762(17) 0.1079(13) 0.0058(12) 0.0555(8) 0.0079(11) C16 0.0956(11) 0.124(2) 0.1228(14) -0.0139(15) 0.0697(9) 0.0124(13) C16' 0.1379(12) 0.0693(17) 0.1242(13) -0.0178(13) 0.0920(8) -0.0026(12) C17 0.0738(11) 0.1011(19) 0.1064(15) 0.0123(14) 0.0424(9) 0.0181(12) C17' 0.1206(13) 0.0944(19) 0.0839(12) -0.0189(13) 0.0614(9) -0.0208(13) C18 0.0532(10) 0.0750(16) 0.0817(13) 0.0028(12) 0.0222(8) -0.0011(11) C18' 0.0861(11) 0.0863(17) 0.0593(10) -0.0022(11) 0.0382(7) -0.0103(11) C19 0.0901(11) 0.1050(19) 0.0651(11) -0.0010(13) 0.0393(8) 0.0034(13) C19' 0.0862(11) 0.0719(16) 0.0900(13) -0.0003(12) 0.0440(8) -0.0070(11) C20 0.0848(16) 0.199(3) 0.1101(19) -0.020(2) 0.0243(13) -0.0033(18) C20' 0.0937(16) 0.219(3) 0.157(2) -0.026(2) 0.0413(14) -0.0707(18) C21 0.1667(17) 0.127(2) 0.0902(14) 0.0197(16) 0.0695(11) 0.0259(17) C21' 0.1450(19) 0.146(3) 0.0987(18) -0.0251(18) 0.0447(13) -0.0297(19) C22 0.0634(12) 0.1031(18) 0.0831(15) 0.0242(14) 0.0140(10) 0.0276(12) C22' 0.0955(13) 0.123(2) 0.0623(12) -0.0327(14) 0.0287(9) -0.0191(14) C23 0.230(3) 0.127(3) 0.140(2) 0.064(2) 0.0736(18) 0.045(2) C23' 0.0877(16) 0.209(3) 0.159(2) 0.076(2) 0.0345(14) -0.0114(18) C24 0.202(2) 0.221(3) 0.0834(19) -0.021(2) 0.0403(16) -0.086(2) C24' 0.139(2) 0.195(3) 0.106(2) 0.015(2) 0.0370(15) -0.009(2) C25 0.0448(9) 0.0669(14) 0.0612(10) 0.0006(10) 0.0210(7) -0.0028(9) C25' 0.0731(10) 0.0771(16) 0.0578(10) 0.0096(11) 0.0350(7) 0.0040(10) C26 0.0581(9) 0.0800(16) 0.0660(11) -0.0140(11) 0.0286(7) -0.0150(10) C26' 0.1133(13) 0.0938(19) 0.0585(11) 0.0127(12) 0.0418(8) 0.0133(13) C27 0.0869(11) 0.1018(19) 0.0944(13) -0.0259(13) 0.0519(8) -0.0346(12) C27' 0.1576(15) 0.124(2) 0.0715(12) 0.0155(14) 0.0716(9) 0.0151(16) C28 0.0696(11) 0.126(2) 0.1219(16) -0.0261(17) 0.0412(10) -0.0338(13) C28' 0.1691(13) 0.107(2) 0.1117(12) 0.0419(13) 0.1058(8) 0.0310(14) C29 0.0638(13) 0.127(2) 0.0992(17) -0.0094(17) 0.0149(11) -0.0114(14) C29' 0.1229(11) 0.0884(18) 0.1212(12) 0.0286(13) 0.0892(8) 0.0204(12) C30 0.0581(10) 0.0869(17) 0.0775(13) -0.0009(13) 0.0227(8) 0.0068(12) C30' 0.0859(11) 0.0793(16) 0.0746(11) 0.0206(12) 0.0457(8) 0.0065(11) C31' 0.1189(17) 0.175(3) 0.0527(14) -0.0184(18) 0.0145(12) -0.0416(18) C31 0.0910(13) 0.1076(19) 0.0668(13) 0.0163(13) 0.0271(9) -0.0222(13) C32 0.1791(17) 0.182(3) 0.0855(14) 0.0138(16) 0.0639(11) -0.0851(17) C32' 0.165(3) 0.469(6) 0.115(3) 0.113(3) -0.013(2) -0.067(4) C33 0.0822(16) 0.139(2) 0.0950(19) 0.0233(18) 0.0038(13) 0.0043(16) C33' 0.169(2) 0.213(4) 0.330(3) -0.080(3) 0.1448(18) -0.075(2) C34 0.0788(15) 0.0894(19) 0.0837(17) 0.0092(16) -0.0118(13) 0.0041(14) C34' 0.0806(11) 0.114(2) 0.1190(15) 0.0087(15) 0.0553(9) -0.0235(13) C35' 0.0793(14) 0.196(3) 0.155(2) 0.050(2) 0.0482(12) -0.0196(17) C35 0.285(4) 0.161(3) 0.095(2) 0.019(3) 0.015(2) -0.007(3) C36 0.237(3) 0.119(3) 0.179(3) 0.010(2) 0.1031(18) 0.025(2) C36' 0.1121(13) 0.192(3) 0.0948(14) -0.0265(17) 0.0583(10) -0.0707(16) C37 0.0576(9) 0.0523(13) 0.0459(9) -0.0068(9) 0.0261(6) -0.0069(9) C37' 0.0543(9) 0.0748(15) 0.0592(10) 0.0005(11) 0.0277(6) -0.0040(10) C38' 0.0580(9) 0.0711(15) 0.0702(10) 0.0056(11) 0.0346(7) 0.0039(10) C39 0.0690(10) 0.1145(19) 0.0652(11) 0.0024(13) 0.0346(7) -0.0101(12) C39' 0.0893(11) 0.0739(16) 0.0987(13) 0.0004(13) 0.0512(8) -0.0050(12) C40 0.0849(10) 0.0983(18) 0.0790(11) 0.0019(12) 0.0458(8) -0.0290(12) C40' 0.1040(12) 0.0797(17) 0.0924(13) 0.0283(12) 0.0541(9) 0.0079(12) C41 0.0911(12) 0.0897(18) 0.0646(12) 0.0081(12) 0.0346(8) -0.0096(12) C41' 0.1026(12) 0.0874(18) 0.0796(12) 0.0142(12) 0.0535(8) 0.0105(12) C42 0.0684(10) 0.0563(14) 0.0428(9) 0.0028(10) 0.0224(7) -0.0026(10) C42' 0.0659(9) 0.0781(16) 0.0583(10) 0.0071(11) 0.0311(7) -0.0052(11) C38 0.0679(9) 0.0637(14) 0.0563(10) 0.0033(10) 0.0325(7) -0.0019(10) C43 0.0651(10) 0.0862(16) 0.0598(11) 0.0073(11) 0.0270(7) -0.0032(11) C44 0.0910(14) 0.143(2) 0.0728(14) -0.0087(16) 0.0287(10) -0.0006(15) C45 0.0739(12) 0.0937(19) 0.0891(15) 0.0074(14) 0.0244(10) 0.0087(13) C43' 0.0681(10) 0.0999(18) 0.0724(12) -0.0233(13) 0.0308(8) -0.0302(11) C44' 0.1516(18) 0.113(2) 0.1003(17) -0.0439(16) 0.0500(12) -0.0278(17) C45' 0.0827(15) 0.156(3) 0.0680(16) -0.0039(17) 0.0050(12) 0.0129(16) C46 0.0672(11) 0.0795(16) 0.0601(12) 0.0165(12) 0.0183(8) -0.0016(11) C46' 0.1014(12) 0.1060(19) 0.0470(10) -0.0114(12) 0.0382(8) -0.0244(12) C47 0.0775(16) 0.137(3) 0.214(3) -0.041(2) 0.0292(16) 0.0171(17) C47' 0.159(2) 0.191(3) 0.082(2) -0.023(2) 0.0028(17) -0.050(2) C48 0.1039(18) 0.312(4) 0.0803(18) -0.073(2) 0.0173(13) -0.039(2) C48' 0.2018(18) 0.092(2) 0.1694(19) -0.0306(17) 0.1202(12) -0.0241(17) C53 0.216(2) 0.163(3) 0.0917(16) -0.0440(19) 0.0733(14) -0.061(2) O1' 0.1121(9) 0.1655(16) 0.1763(12) 0.0944(12) 0.0741(8) 0.0467(10) Na1' 0.0942(5) 0.1021(7) 0.1144(6) 0.0261(6) 0.0441(4) 0.0256(5) Na1 0.1250(5) 0.0946(7) 0.0959(5) -0.0186(5) 0.0656(3) -0.0171(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 N2 2.1616(15) . ? Yb1 N3 2.1646(12) . ? Yb1 N1 2.2521(16) . ? Yb1 N4 2.2816(17) . ? Yb1 Na1 3.3781(9) . ? Yb1' N2' 2.1682(15) . ? Yb1' N3' 2.1768(15) . ? Yb1' N4' 2.2191(17) . ? Yb1' N1' 2.2293(14) . ? Yb1' Na1' 3.4777(10) . ? N1 C1 1.423(3) . ? N1 Na1 2.496(2) . ? N1' C1' 1.416(3) . ? N1' Na1' 2.461(2) . ? N2 C13 1.416(3) . ? N2' C13' 1.398(3) . ? N3' C25' 1.393(3) . ? N3 C25 1.393(2) . ? N4 C37 1.402(3) . ? N4 Na1 2.4657(18) . ? N4' C37' 1.373(3) . ? N4' Na1' 2.7861(16) . ? C1 C6 1.400(2) . ? C1 C2 1.416(2) . ? C1' C6' 1.405(3) . ? C1' C2' 1.416(2) . ? C1' Na1' 3.083(3) . ? C2 C3 1.388(3) . ? C2 C7 1.511(3) . ? C2' C3' 1.385(4) . ? C2' C7' 1.536(4) . ? C3 C4 1.358(3) . ? C3' C4' 1.380(5) . ? C4 C5 1.380(3) . ? C4' C5' 1.377(3) . ? C5 C6 1.384(3) . ? C5' C6' 1.376(4) . ? C6 C10 1.508(3) . ? C6' C10' 1.506(2) . ? C7 C8 1.508(3) . ? C7 C9 1.543(3) . ? C7' C9' 1.481(5) . ? C7' C8' 1.508(7) . ? C7' C8A 1.541(8) . ? C10 C11 1.528(3) . ? C10 C12 1.546(3) . ? C10' C11' 1.508(3) . ? C10' C12' 1.536(3) . ? C12 Na1 3.073(3) . ? C12' Na1' 2.962(3) . ? C13 C14 1.395(3) . ? C13 C18 1.410(2) . ? C13' C18' 1.405(2) . ? C13' C14' 1.412(2) . ? C14 C15 1.388(3) . ? C14 C19 1.517(3) . ? C14' C15' 1.365(3) . ? C14' C19' 1.510(3) . ? C15 C16 1.361(3) . ? C15' C16' 1.361(3) . ? C16 C17 1.373(3) . ? C16' C17' 1.376(2) . ? C17 C18 1.374(3) . ? C17' C18' 1.387(3) . ? C18 C22 1.523(3) . ? C18' C22' 1.518(2) . ? C19 C20 1.504(3) . ? C19 C21 1.532(3) . ? C19' C21' 1.477(3) . ? C19' C20' 1.538(3) . ? C22 C24 1.496(3) . ? C22 C23 1.517(3) . ? C22' C23' 1.495(3) . ? C22' C24' 1.497(3) . ? C25 C26 1.406(3) . ? C25 C30 1.428(2) . ? C25' C26' 1.416(2) . ? C25' C30' 1.419(3) . ? C26 C27 1.384(3) . ? C26 C31 1.528(2) . ? C26' C27' 1.373(3) . ? C26' C31' 1.525(3) . ? C27 C28 1.382(2) . ? C27' C28' 1.341(3) . ? C28 C29 1.354(4) . ? C28' C29' 1.368(3) . ? C29 C30 1.365(3) . ? C29' C30' 1.402(3) . ? C30 C34 1.527(3) . ? C30' C34' 1.482(2) . ? C31' C33' 1.466(4) . ? C31' C32' 1.507(4) . ? C31 C33 1.494(3) . ? C31 C32 1.496(4) . ? C34 C36 1.480(3) . ? C34 C35 1.498(3) . ? C34' C35' 1.519(3) . ? C34' C36' 1.544(3) . ? C37 C42 1.407(2) . ? C37 C38 1.409(2) . ? C37' C42' 1.401(3) . ? C37' C38' 1.421(3) . ? C37' Na1' 2.6272(18) . ? C38' C39' 1.363(3) . ? C38' C43' 1.525(3) . ? C39 C38 1.384(3) . ? C39 C40 1.386(3) . ? C39' C40' 1.392(3) . ? C40 C41 1.364(2) . ? C40' C41' 1.354(3) . ? C41 C42 1.388(3) . ? C41' C42' 1.387(3) . ? C42 C46 1.513(2) . ? C42' C46' 1.505(3) . ? C42' Na1' 2.752(2) . ? C38 C43 1.506(2) . ? C43 C45 1.515(3) . ? C43 C44 1.533(3) . ? C43' C45' 1.522(3) . ? C43' C44' 1.531(3) . ? C46 C47 1.482(3) . ? C46 C48 1.493(3) . ? C46' C48' 1.474(3) . ? C46' C47' 1.518(3) . ? O1 C54 1.393(4) . ? O1 C51 1.408(5) . ? O1 Na1 2.223(3) . ? C51 C52 1.443(5) . ? C52 C53 1.451(4) . ? C53 C52A 1.403(5) . ? C53 C54A 1.441(4) . ? C53 C54 1.470(4) . ? O1A C51A 1.375(4) . ? O1A C54A 1.397(4) . ? O1A Na1 2.265(2) . ? C51A C52A 1.432(5) . ? O1' C54' 1.388(5) . ? O1' C51' 1.399(4) . ? O1' C54B 1.420(4) . ? O1' C51B 1.431(4) . ? O1' Na1' 2.1942(17) . ? C51' C52' 1.419(6) . ? C52' C53' 1.359(6) . ? C53' C54' 1.405(4) . ? C51B C52B 1.391(6) . ? C52B C53B 1.369(6) . ? C53B C54B 1.374(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Yb1 N3 121.04(6) . . ? N2 Yb1 N1 100.47(5) . . ? N3 Yb1 N1 121.57(6) . . ? N2 Yb1 N4 121.65(6) . . ? N3 Yb1 N4 96.05(5) . . ? N1 Yb1 N4 94.42(6) . . ? N2 Yb1 Na1 119.10(4) . . ? N3 Yb1 Na1 119.73(5) . . ? N1 Yb1 Na1 47.64(5) . . ? N4 Yb1 Na1 46.87(4) . . ? N2' Yb1' N3' 124.25(6) . . ? N2' Yb1' N4' 117.46(6) . . ? N3' Yb1' N4' 97.32(6) . . ? N2' Yb1' N1' 95.34(5) . . ? N3' Yb1' N1' 122.89(6) . . ? N4' Yb1' N1' 97.92(6) . . ? N2' Yb1' Na1' 113.23(4) . . ? N3' Yb1' Na1' 122.51(5) . . ? N4' Yb1' Na1' 53.15(4) . . ? N1' Yb1' Na1' 44.78(5) . . ? C1 N1 Yb1 133.83(10) . . ? C1 N1 Na1 109.16(12) . . ? Yb1 N1 Na1 90.56(6) . . ? C1' N1' Yb1' 137.52(14) . . ? C1' N1' Na1' 101.97(13) . . ? Yb1' N1' Na1' 95.58(6) . . ? C13 N2 Yb1 147.40(11) . . ? C13' N2' Yb1' 145.91(10) . . ? C25' N3' Yb1' 145.94(10) . . ? C25 N3 Yb1 147.54(13) . . ? C37 N4 Yb1 132.65(12) . . ? C37 N4 Na1 112.38(10) . . ? Yb1 N4 Na1 90.64(6) . . ? C37' N4' Yb1' 146.27(10) . . ? C37' N4' Na1' 68.97(9) . . ? Yb1' N4' Na1' 87.25(5) . . ? C6 C1 C2 119.2(2) . . ? C6 C1 N1 121.73(16) . . ? C2 C1 N1 119.01(16) . . ? C6' C1' N1' 120.28(15) . . ? C6' C1' C2' 120.1(2) . . ? N1' C1' C2' 119.5(2) . . ? C6' C1' Na1' 87.71(14) . . ? N1' C1' Na1' 51.34(10) . . ? C2' C1' Na1' 129.93(18) . . ? C3 C2 C1 117.88(17) . . ? C3 C2 C7 120.65(18) . . ? C1 C2 C7 121.5(2) . . ? C3' C2' C1' 118.9(2) . . ? C3' C2' C7' 121.10(19) . . ? C1' C2' C7' 119.9(2) . . ? C4 C3 C2 122.3(2) . . ? C4' C3' C2' 121.2(2) . . ? C3 C4 C5 120.3(2) . . ? C5' C4' C3' 118.9(3) . . ? C4 C5 C6 119.6(2) . . ? C6' C5' C4' 122.8(3) . . ? C5 C6 C1 120.60(18) . . ? C5 C6 C10 116.83(17) . . ? C1 C6 C10 122.5(2) . . ? C5' C6' C1' 118.03(18) . . ? C5' C6' C10' 119.6(2) . . ? C1' C6' C10' 122.4(2) . . ? C8 C7 C2 111.67(16) . . ? C8 C7 C9 107.32(19) . . ? C2 C7 C9 114.3(2) . . ? C9' C7' C8' 119.5(3) . . ? C9' C7' C2' 113.3(3) . . ? C8' C7' C2' 118.1(3) . . ? C9' C7' C8A 89.8(4) . . ? C8' C7' C8A 46.5(4) . . ? C2' C7' C8A 107.2(4) . . ? C6 C10 C11 115.2(2) . . ? C6 C10 C12 113.46(18) . . ? C11 C10 C12 107.21(18) . . ? C6' C10' C11' 113.8(2) . . ? C6' C10' C12' 109.47(17) . . ? C11' C10' C12' 110.32(19) . . ? C10 C12 Na1 81.73(13) . . ? C10' C12' Na1' 82.44(14) . . ? C14 C13 C18 119.48(19) . . ? C14 C13 N2 118.17(15) . . ? C18 C13 N2 122.34(18) . . ? N2' C13' C18' 121.92(14) . . ? N2' C13' C14' 119.20(15) . . ? C18' C13' C14' 118.84(19) . . ? C15 C14 C13 118.30(17) . . ? C15 C14 C19 119.57(19) . . ? C13 C14 C19 122.13(19) . . ? C15' C14' C13' 119.54(16) . . ? C15' C14' C19' 120.98(15) . . ? C13' C14' C19' 119.41(18) . . ? C16 C15 C14 122.6(2) . . ? C16' C15' C14' 121.99(17) . . ? C15 C16 C17 118.7(2) . . ? C15' C16' C17' 119.2(2) . . ? C16 C17 C18 121.58(19) . . ? C16' C17' C18' 121.44(18) . . ? C17 C18 C13 119.28(19) . . ? C17 C18 C22 119.74(17) . . ? C13 C18 C22 120.97(19) . . ? C17' C18' C13' 118.82(15) . . ? C17' C18' C22' 120.50(16) . . ? C13' C18' C22' 120.66(19) . . ? C20 C19 C14 108.87(19) . . ? C20 C19 C21 109.93(17) . . ? C14 C19 C21 114.67(18) . . ? C21' C19' C14' 113.80(18) . . ? C21' C19' C20' 106.17(17) . . ? C14' C19' C20' 116.0(2) . . ? C24 C22 C23 107.93(16) . . ? C24 C22 C18 111.0(2) . . ? C23 C22 C18 115.4(2) . . ? C23' C22' C24' 107.73(18) . . ? C23' C22' C18' 111.17(18) . . ? C24' C22' C18' 115.2(2) . . ? N3 C25 C26 119.62(13) . . ? N3 C25 C30 121.73(18) . . ? C26 C25 C30 118.65(16) . . ? N3' C25' C26' 123.92(17) . . ? N3' C25' C30' 117.69(14) . . ? C26' C25' C30' 118.4(2) . . ? C27 C26 C25 120.51(15) . . ? C27 C26 C31 118.21(19) . . ? C25 C26 C31 121.28(16) . . ? C27' C26' C25' 119.21(19) . . ? C27' C26' C31' 122.33(17) . . ? C25' C26' C31' 118.5(2) . . ? C28 C27 C26 119.2(2) . . ? C28' C27' C26' 122.36(18) . . ? C29 C28 C27 120.8(2) . . ? C27' C28' C29' 120.6(2) . . ? C28 C29 C30 122.49(17) . . ? C28' C29' C30' 120.40(19) . . ? C29 C30 C25 118.4(2) . . ? C29 C30 C34 121.65(16) . . ? C25 C30 C34 119.98(17) . . ? C29' C30' C25' 119.00(15) . . ? C29' C30' C34' 120.77(17) . . ? C25' C30' C34' 120.23(19) . . ? C33' C31' C32' 106.7(2) . . ? C33' C31' C26' 110.5(2) . . ? C32' C31' C26' 112.3(2) . . ? C33 C31 C32 112.1(2) . . ? C33 C31 C26 109.83(18) . . ? C32 C31 C26 115.23(18) . . ? C36 C34 C35 107.65(19) . . ? C36 C34 C30 109.9(2) . . ? C35 C34 C30 114.6(2) . . ? C30' C34' C35' 116.3(2) . . ? C30' C34' C36' 111.04(16) . . ? C35' C34' C36' 107.51(17) . . ? N4 C37 C42 119.38(14) . . ? N4 C37 C38 121.02(14) . . ? C42 C37 C38 119.53(18) . . ? N4' C37' C42' 122.08(17) . . ? N4' C37' C38' 119.90(17) . . ? C42' C37' C38' 117.90(19) . . ? N4' C37' Na1' 81.84(10) . . ? C42' C37' Na1' 79.88(10) . . ? C38' C37' Na1' 105.45(12) . . ? C39' C38' C37' 120.63(18) . . ? C39' C38' C43' 119.80(17) . . ? C37' C38' C43' 119.46(18) . . ? C38 C39 C40 120.43(16) . . ? C38' C39' C40' 120.07(19) . . ? C41 C40 C39 119.4(2) . . ? C41' C40' C39' 120.2(2) . . ? C40 C41 C42 122.57(18) . . ? C40' C41' C42' 121.1(2) . . ? C41 C42 C37 118.16(15) . . ? C41 C42 C46 119.91(16) . . ? C37 C42 C46 121.89(18) . . ? C41' C42' C37' 119.90(18) . . ? C41' C42' C46' 118.22(18) . . ? C37' C42' C46' 121.38(19) . . ? C41' C42' Na1' 108.87(14) . . ? C37' C42' Na1' 70.04(11) . . ? C46' C42' Na1' 98.15(12) . . ? C39 C38 C37 119.85(15) . . ? C39 C38 C43 117.59(14) . . ? C37 C38 C43 122.56(18) . . ? C38 C43 C45 114.93(18) . . ? C38 C43 C44 110.66(16) . . ? C45 C43 C44 109.50(14) . . ? C45' C43' C38' 111.42(19) . . ? C45' C43' C44' 109.67(15) . . ? C38' C43' C44' 115.02(18) . . ? C47 C46 C48 109.32(19) . . ? C47 C46 C42 111.43(17) . . ? C48 C46 C42 115.67(19) . . ? C48' C46' C42' 111.49(17) . . ? C48' C46' C47' 110.1(2) . . ? C42' C46' C47' 115.03(19) . . ? C54 O1 C51 104.4(3) . . ? C54 O1 Na1 133.0(2) . . ? C51 O1 Na1 122.2(2) . . ? O1 C51 C52 107.3(3) . . ? C51 C52 C53 103.7(3) . . ? C52A C53 C54A 103.4(3) . . ? C52A C53 C52 23.1(2) . . ? C54A C53 C52 109.0(2) . . ? C52A C53 C54 104.9(2) . . ? C54A C53 C54 31.6(2) . . ? C52 C53 C54 97.9(2) . . ? O1 C54 C53 110.0(3) . . ? C51A O1A C54A 102.8(2) . . ? C51A O1A Na1 124.34(19) . . ? C54A O1A Na1 132.9(2) . . ? O1A C51A C52A 108.6(3) . . ? C53 C52A C51A 107.4(3) . . ? O1A C54A C53 110.0(3) . . ? C54' O1' C51' 98.4(3) . . ? C54' O1' C54B 32.6(3) . . ? C51' O1' C54B 108.8(2) . . ? C54' O1' C51B 110.2(2) . . ? C51' O1' C51B 38.7(3) . . ? C54B O1' C51B 98.6(2) . . ? C54' O1' Na1' 128.44(15) . . ? C51' O1' Na1' 124.9(2) . . ? C54B O1' Na1' 126.20(17) . . ? C51B O1' Na1' 121.0(2) . . ? O1' C51' C52' 110.8(4) . . ? C53' C52' C51' 106.8(4) . . ? C52' C53' C54' 103.2(4) . . ? O1' C54' C53' 111.8(3) . . ? C52B C51B O1' 106.5(3) . . ? C53B C52B C51B 97.7(4) . . ? C52B C53B C54B 109.4(4) . . ? C53B C54B O1' 107.0(3) . . ? O1' Na1' N1' 110.20(6) . . ? O1' Na1' C37' 135.77(8) . . ? N1' Na1' C37' 105.98(7) . . ? O1' Na1' C42' 111.51(8) . . ? N1' Na1' C42' 109.01(7) . . ? C37' Na1' C42' 30.08(5) . . ? O1' Na1' N4' 163.48(8) . . ? N1' Na1' N4' 79.23(5) . . ? C37' Na1' N4' 29.19(6) . . ? C42' Na1' N4' 51.97(6) . . ? O1' Na1' C12' 98.44(7) . . ? N1' Na1' C12' 89.28(7) . . ? C37' Na1' C12' 106.69(6) . . ? C42' Na1' C12' 135.49(6) . . ? N4' Na1' C12' 95.14(6) . . ? O1' Na1' C1' 93.36(6) . . ? N1' Na1' C1' 26.69(6) . . ? C37' Na1' C1' 128.91(7) . . ? C42' Na1' C1' 135.62(7) . . ? N4' Na1' C1' 99.98(6) . . ? C12' Na1' C1' 70.83(7) . . ? O1' Na1' Yb1' 147.66(5) . . ? N1' Na1' Yb1' 39.64(4) . . ? C37' Na1' Yb1' 67.06(5) . . ? C42' Na1' Yb1' 78.85(5) . . ? N4' Na1' Yb1' 39.60(4) . . ? C12' Na1' Yb1' 93.28(5) . . ? C1' Na1' Yb1' 62.29(4) . . ? O1 Na1 O1A 14.84(8) . . ? O1 Na1 N4 163.09(9) . . ? O1A Na1 N4 163.56(9) . . ? O1 Na1 N1 112.70(9) . . ? O1A Na1 N1 105.29(8) . . ? N4 Na1 N1 84.21(6) . . ? O1 Na1 C12 83.86(9) . . ? O1A Na1 C12 96.24(8) . . ? N4 Na1 C12 97.70(6) . . ? N1 Na1 C12 86.80(7) . . ? O1 Na1 Yb1 154.39(8) . . ? O1A Na1 Yb1 144.34(7) . . ? N4 Na1 Yb1 42.48(4) . . ? N1 Na1 Yb1 41.81(4) . . ? C12 Na1 Yb1 94.97(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.536 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.074 #===END data_complex_2.(0.5C6H6) _database_code_CSD 175640 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C91 H139 Li2 N6 Na2 O4 Yb2' _chemical_formula_weight 1787.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.839(4) _cell_length_b 22.603(5) _cell_length_c 25.919(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.75(3) _cell_angle_gamma 90.00 _cell_volume 10428(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3708 _exptl_absorpt_coefficient_mu 1.834 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.8751 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11887 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1016 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11887 _reflns_number_gt 10143 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0956P)^2^+24.8733P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11887 _refine_ls_number_parameters 929 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.1095 _refine_ls_R_factor_gt 0.0891 _refine_ls_wR_factor_ref 0.2348 _refine_ls_wR_factor_gt 0.2231 _refine_ls_goodness_of_fit_ref 1.196 _refine_ls_restrained_S_all 1.197 _refine_ls_shift/su_max 0.00 _refine_ls_shift/su_mean 0.00 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 0.075061(11) 0.212709(8) 0.653207(9) 0.06638(6) Uani 1 1 d . . . Yb2 Yb -0.097514(11) 0.268887(9) 0.658355(9) 0.06777(7) Uani 1 1 d . . . Na1 Na 0.18182(12) 0.32355(9) 0.59109(9) 0.1019(8) Uani 1 1 d . . . Na2 Na -0.21763(12) 0.16672(10) 0.58328(9) 0.1017(8) Uani 1 1 d . . . Li1 Li 0.2172(4) 0.1563(4) 0.6683(4) 0.088(3) Uani 1 1 d . . . Li2 Li -0.2376(4) 0.3136(5) 0.6825(4) 0.099(3) Uani 1 1 d . . . N1 N 0.01527(19) 0.30357(14) 0.65502(14) 0.0627(11) Uani 1 1 d . . . C1 C 0.0604(3) 0.35297(19) 0.6500(2) 0.095(2) Uani 1 1 d . . . C2 C 0.0543(3) 0.3895(2) 0.6067(2) 0.094(2) Uani 1 1 d . . . C3 C 0.1028(3) 0.4377(2) 0.6016(3) 0.113(2) Uani 1 1 d . . . H3A H 0.0993 0.4595 0.5711 0.135 Uiso 1 1 calc R . . C4 C 0.1539(3) 0.4530(2) 0.6390(3) 0.113(2) Uani 1 1 d . . . H4A H 0.1828 0.4869 0.6358 0.135 Uiso 1 1 calc R . . C5 C 0.1630(3) 0.4181(2) 0.6823(3) 0.107(2) Uani 1 1 d . . . H5A H 0.1996 0.4279 0.7081 0.129 Uiso 1 1 calc R . . C6 C 0.1184(3) 0.3683(2) 0.6883(2) 0.0798(17) Uani 1 1 d . . . C7 C -0.0032(3) 0.3730(2) 0.5624(2) 0.095(2) Uani 1 1 d . . . H7A H -0.0472 0.3561 0.5777 0.114 Uiso 1 1 calc R . . C8 C -0.0291(4) 0.4275(2) 0.5310(3) 0.132(3) Uani 1 1 d . . . H8A H -0.0656 0.4158 0.5040 0.198 Uiso 1 1 calc R . . H8B H 0.0132 0.4453 0.5161 0.198 Uiso 1 1 calc R . . H8C H -0.0513 0.4555 0.5533 0.198 Uiso 1 1 calc R . . C9 C 0.0257(4) 0.3278(3) 0.5266(2) 0.116(2) Uani 1 1 d . . . H9A H 0.0410 0.2931 0.5459 0.174 Uiso 1 1 calc R . . H9B H 0.0679 0.3437 0.5101 0.174 Uiso 1 1 calc R . . H9C H -0.0133 0.3176 0.5008 0.174 Uiso 1 1 calc R . . C10 C 0.1281(3) 0.3355(3) 0.7417(2) 0.108(2) Uani 1 1 d . . . H10A H 0.1224 0.2933 0.7339 0.130 Uiso 1 1 calc R . . C11 C 0.2044(4) 0.3420(3) 0.7712(3) 0.149(3) Uani 1 1 d . . . H11A H 0.2048 0.3196 0.8027 0.223 Uiso 1 1 calc R . . H11B H 0.2134 0.3829 0.7792 0.223 Uiso 1 1 calc R . . H11C H 0.2429 0.3275 0.7503 0.223 Uiso 1 1 calc R . . C12 C 0.0630(4) 0.3516(4) 0.7751(3) 0.180(4) Uani 1 1 d . . . H12A H 0.0161 0.3460 0.7553 0.270 Uiso 1 1 calc R . . H12B H 0.0676 0.3922 0.7856 0.270 Uiso 1 1 calc R . . H12C H 0.0646 0.3266 0.8051 0.270 Uiso 1 1 calc R . . N2 N -0.0462(2) 0.17984(16) 0.65250(17) 0.0806(14) Uani 1 1 d . . . C13 C -0.08978(12) 0.12992(9) 0.64288(10) 0.0652(14) Uani 1 1 d G . . C14 C -0.08873(17) 0.10237(12) 0.59499(11) 0.0741(16) Uani 1 1 d G . . C15 C -0.1341(2) 0.05338(14) 0.58389(15) 0.107(2) Uani 1 1 d G . . H15A H -0.1334 0.0350 0.5518 0.129 Uiso 1 1 calc R . . C16 C -0.1804(2) 0.03194(13) 0.62069(19) 0.118(3) Uani 1 1 d G . . H16A H -0.2108 -0.0008 0.6133 0.142 Uiso 1 1 calc R . . C17 C -0.18147(18) 0.05949(14) 0.66858(17) 0.108(2) Uani 1 1 d G . . H17A H -0.2125 0.0451 0.6932 0.130 Uiso 1 1 calc R . . C18 C -0.13614(16) 0.10847(12) 0.67968(12) 0.091(2) Uani 1 1 d G . . C19 C -0.0393(3) 0.1234(2) 0.5535(2) 0.096(2) Uani 1 1 d . . . H19A H 0.0084 0.1352 0.5715 0.116 Uiso 1 1 calc R . . C20 C -0.0195(4) 0.0762(3) 0.5141(2) 0.131(3) Uani 1 1 d . . . H20A H 0.0008 0.0420 0.5320 0.197 Uiso 1 1 calc R . . H20B H 0.0170 0.0918 0.4921 0.197 Uiso 1 1 calc R . . H20C H -0.0640 0.0652 0.4935 0.197 Uiso 1 1 calc R . . C21 C -0.0692(4) 0.1767(2) 0.5272(2) 0.114(2) Uani 1 1 d . . . H21A H -0.0354 0.1893 0.5020 0.136 Uiso 1 1 calc R . . H21B H -0.0744 0.2077 0.5521 0.136 Uiso 1 1 calc R . . H21C H -0.1175 0.1681 0.5102 0.136 Uiso 1 1 calc R . . C22 C -0.1335(3) 0.1323(3) 0.7346(2) 0.108(2) Uani 1 1 d . . . H22A H -0.1304 0.1754 0.7314 0.129 Uiso 1 1 calc R . . C23 C -0.0666(4) 0.1146(5) 0.7685(3) 0.219(5) Uani 1 1 d . . . H23A H -0.0217 0.1232 0.7514 0.328 Uiso 1 1 calc R . . H23B H -0.0689 0.0729 0.7755 0.328 Uiso 1 1 calc R . . H23C H -0.0660 0.1361 0.8004 0.328 Uiso 1 1 calc R . . C24 C -0.2075(4) 0.1198(4) 0.7629(3) 0.181(4) Uani 1 1 d . . . H24A H -0.2505 0.1293 0.7402 0.272 Uiso 1 1 calc R . . H24B H -0.2078 0.1437 0.7935 0.272 Uiso 1 1 calc R . . H24C H -0.2092 0.0787 0.7723 0.272 Uiso 1 1 calc R . . N3 N 0.1766(2) 0.21909(15) 0.61674(15) 0.0726(13) Uani 1 1 d . . . C25 C 0.2446(2) 0.21539(19) 0.58940(18) 0.0700(15) Uani 1 1 d . . . C26 C 0.3103(2) 0.2456(2) 0.61068(19) 0.0730(16) Uani 1 1 d . . . C27 C 0.3766(3) 0.2385(2) 0.5832(3) 0.105(2) Uani 1 1 d . . . H27A H 0.4192 0.2586 0.5963 0.125 Uiso 1 1 calc R . . C28 C 0.3842(3) 0.2051(2) 0.5394(2) 0.100(2) Uani 1 1 d . . . H28A H 0.4300 0.2020 0.5245 0.120 Uiso 1 1 calc R . . C29 C 0.3201(3) 0.1760(2) 0.5185(2) 0.102(2) Uani 1 1 d . . . H29A H 0.3214 0.1554 0.4875 0.122 Uiso 1 1 calc R . . C30 C 0.2507(3) 0.17822(18) 0.54588(19) 0.0755(16) Uani 1 1 d . . . C31 C 0.3142(3) 0.2810(2) 0.6598(2) 0.095(2) Uani 1 1 d . . . H31A H 0.2626 0.2861 0.6699 0.114 Uiso 1 1 calc R . . C32 C 0.3570(4) 0.2533(3) 0.7031(3) 0.131(3) Uani 1 1 d . . . H32A H 0.4096 0.2609 0.7005 0.197 Uiso 1 1 calc R . . H32B H 0.3483 0.2114 0.7024 0.197 Uiso 1 1 calc R . . H32C H 0.3414 0.2694 0.7350 0.197 Uiso 1 1 calc R . . C33 C 0.3450(4) 0.3418(3) 0.6501(3) 0.139(3) Uani 1 1 d . . . H33A H 0.3937 0.3457 0.6677 0.209 Uiso 1 1 calc R . . H33B H 0.3118 0.3711 0.6628 0.209 Uiso 1 1 calc R . . H33C H 0.3489 0.3473 0.6137 0.209 Uiso 1 1 calc R . . C34 C 0.1801(3) 0.1481(2) 0.5198(2) 0.096(2) Uani 1 1 d . . . H34A H 0.1430 0.1458 0.5460 0.115 Uiso 1 1 calc R . . C35 C 0.1462(4) 0.1804(4) 0.4777(3) 0.204(4) Uani 1 1 d . . . H35A H 0.1021 0.1600 0.4641 0.306 Uiso 1 1 calc R . . H35B H 0.1811 0.1841 0.4512 0.306 Uiso 1 1 calc R . . H35C H 0.1326 0.2191 0.4893 0.306 Uiso 1 1 calc R . . C36 C 0.2003(5) 0.0835(3) 0.5060(4) 0.216(5) Uani 1 1 d . . . H36A H 0.1564 0.0638 0.4910 0.324 Uiso 1 1 calc R . . H36B H 0.2184 0.0630 0.5367 0.324 Uiso 1 1 calc R . . H36C H 0.2386 0.0837 0.4816 0.324 Uiso 1 1 calc R . . N4 N 0.1234(3) 0.1505(2) 0.71037(18) 0.1125(18) Uani 1 1 d . . . C37 C 0.1314(3) 0.1032(2) 0.7418(2) 0.0867(18) Uani 1 1 d . . . C38 C 0.1471(3) 0.1114(2) 0.7947(2) 0.104(2) Uani 1 1 d . . . C39 C 0.1549(4) 0.0650(3) 0.8284(3) 0.148(3) Uani 1 1 d . . . H39A H 0.1678 0.0707 0.8634 0.178 Uiso 1 1 calc R . . C40 C 0.1419(4) 0.0054(3) 0.8065(3) 0.143(3) Uani 1 1 d . . . H40A H 0.1449 -0.0272 0.8284 0.172 Uiso 1 1 calc R . . C41 C 0.1256(4) -0.0030(3) 0.7552(3) 0.117(3) Uani 1 1 d . . . H41A H 0.1191 -0.0410 0.7419 0.140 Uiso 1 1 calc R . . C42 C 0.1190(3) 0.0442(2) 0.7239(2) 0.0943(19) Uani 1 1 d . . . C43 C 0.1572(4) 0.1716(3) 0.8171(3) 0.132(3) Uani 1 1 d . . . H43A H 0.1472 0.1989 0.7881 0.158 Uiso 1 1 calc R . . C44 C 0.1095(6) 0.1883(4) 0.8534(6) 0.319(8) Uani 1 1 d . . . H44A H 0.1190 0.2287 0.8630 0.478 Uiso 1 1 calc R . . H44B H 0.1172 0.1635 0.8833 0.478 Uiso 1 1 calc R . . H44C H 0.0585 0.1843 0.8394 0.478 Uiso 1 1 calc R . . C45 C 0.2320(6) 0.1839(4) 0.8362(4) 0.225(5) Uani 1 1 d . . . H45A H 0.2351 0.2238 0.8487 0.337 Uiso 1 1 calc R . . H45B H 0.2653 0.1788 0.8090 0.337 Uiso 1 1 calc R . . H45C H 0.2461 0.1572 0.8640 0.337 Uiso 1 1 calc R . . C46 C 0.0976(3) 0.0319(3) 0.6662(2) 0.119(3) Uani 1 1 d . . . H46A H 0.0901 0.0696 0.6479 0.143 Uiso 1 1 calc R . . C47 C 0.0323(4) -0.0042(3) 0.6568(3) 0.153(4) Uani 1 1 d . . . H47A H 0.0225 -0.0095 0.6202 0.230 Uiso 1 1 calc R . . H47B H -0.0100 0.0148 0.6708 0.230 Uiso 1 1 calc R . . H47C H 0.0405 -0.0420 0.6730 0.230 Uiso 1 1 calc R . . C48 C 0.1593(5) 0.0007(5) 0.6455(4) 0.246(6) Uani 1 1 d . . . H48A H 0.1480 -0.0068 0.6093 0.370 Uiso 1 1 calc R . . H48B H 0.1670 -0.0362 0.6634 0.370 Uiso 1 1 calc R . . H48C H 0.2040 0.0242 0.6499 0.370 Uiso 1 1 calc R . . N5 N -0.1405(3) 0.3137(2) 0.7255(2) 0.1192(19) Uani 1 1 d . . . C49 C -0.13553(14) 0.35988(14) 0.76356(13) 0.0901(18) Uani 1 1 d G . . C50 C -0.1415(2) 0.34700(19) 0.81557(13) 0.157(3) Uani 1 1 d G . . C51 C -0.1430(3) 0.3926(3) 0.85147(14) 0.167(4) Uani 1 1 d G . . H51A H -0.1470 0.3840 0.8863 0.201 Uiso 1 1 calc R . . C52 C -0.1386(3) 0.4511(2) 0.8354(2) 0.166(4) Uani 1 1 d G . . H52A H -0.1396 0.4816 0.8594 0.199 Uiso 1 1 calc R . . C53 C -0.1326(3) 0.46396(14) 0.7834(2) 0.147(3) Uani 1 1 d G . . H53A H -0.1297 0.5031 0.7726 0.177 Uiso 1 1 calc R . . C54 C -0.1311(2) 0.41836(15) 0.74745(16) 0.128(3) Uani 1 1 d G . . C55 C -0.1352(7) 0.2801(4) 0.8389(4) 0.208(5) Uani 1 1 d . . . H55A H -0.1157 0.2543 0.8124 0.250 Uiso 1 1 calc R . . C56 C -0.0888(7) 0.2717(5) 0.8869(5) 0.275(7) Uani 1 1 d . . . H56A H -0.0894 0.2307 0.8967 0.413 Uiso 1 1 calc R . . H56B H -0.1082 0.2953 0.9138 0.413 Uiso 1 1 calc R . . H56C H -0.0381 0.2835 0.8818 0.413 Uiso 1 1 calc R . . C57 C -0.2112(5) 0.2597(5) 0.8489(5) 0.302(6) Uani 1 1 d . . . H57A H -0.2088 0.2199 0.8619 0.453 Uiso 1 1 calc R . . H57B H -0.2426 0.2608 0.8174 0.453 Uiso 1 1 calc R . . H57C H -0.2319 0.2851 0.8741 0.453 Uiso 1 1 calc R . . C58 C -0.1244(5) 0.4363(3) 0.6897(3) 0.163(4) Uani 1 1 d . . . H58A H -0.1180 0.3992 0.6709 0.195 Uiso 1 1 calc R . . C59 C -0.1948(6) 0.4658(5) 0.6639(5) 0.294(7) Uani 1 1 d . . . H59A H -0.2374 0.4404 0.6670 0.440 Uiso 1 1 calc R . . H59B H -0.1875 0.4726 0.6280 0.440 Uiso 1 1 calc R . . H59C H -0.2033 0.5029 0.6806 0.440 Uiso 1 1 calc R . . C60 C -0.0533(6) 0.4741(4) 0.6810(4) 0.215(5) Uani 1 1 d . . . H60A H -0.0522 0.4837 0.6449 0.323 Uiso 1 1 calc R . . H60B H -0.0090 0.4520 0.6918 0.323 Uiso 1 1 calc R . . H60C H -0.0547 0.5099 0.7008 0.323 Uiso 1 1 calc R . . N6 N -0.2084(2) 0.26601(15) 0.62304(17) 0.0810(14) Uani 1 1 d . . . C61 C -0.2774(3) 0.27130(18) 0.5979(2) 0.0781(16) Uani 1 1 d . . . C62 C -0.3416(3) 0.2365(2) 0.6132(2) 0.0825(18) Uani 1 1 d . . . C63 C -0.4138(3) 0.2442(3) 0.5867(3) 0.114(2) Uani 1 1 d . . . H63A H -0.4544 0.2220 0.5967 0.137 Uiso 1 1 calc R . . C64 C -0.4243(3) 0.2851(3) 0.5456(3) 0.139(3) Uani 1 1 d . . . H64A H -0.4705 0.2885 0.5270 0.167 Uiso 1 1 calc R . . C65 C -0.3666(3) 0.3186(2) 0.5343(2) 0.097(2) Uani 1 1 d . . . H65A H -0.3745 0.3484 0.5098 0.116 Uiso 1 1 calc R . . C66 C -0.2953(3) 0.3110(2) 0.5573(2) 0.093(2) Uani 1 1 d . . . C67 C -0.3359(3) 0.1926(3) 0.6535(2) 0.101(2) Uani 1 1 d . . . H67A H -0.2822 0.1883 0.6636 0.121 Uiso 1 1 calc R . . C68 C -0.3648(4) 0.1289(3) 0.6346(3) 0.146(3) Uani 1 1 d . . . H68A H -0.4100 0.1192 0.6509 0.218 Uiso 1 1 calc R . . H68B H -0.3269 0.0998 0.6438 0.218 Uiso 1 1 calc R . . H68C H -0.3747 0.1292 0.5977 0.218 Uiso 1 1 calc R . . C69 C -0.3744(4) 0.2100(3) 0.7031(3) 0.153(3) Uani 1 1 d . . . H69A H -0.4276 0.2044 0.6977 0.229 Uiso 1 1 calc R . . H69B H -0.3640 0.2507 0.7111 0.229 Uiso 1 1 calc R . . H69C H -0.3554 0.1856 0.7313 0.229 Uiso 1 1 calc R . . C70 C -0.2271(3) 0.3485(2) 0.5372(2) 0.096(2) Uani 1 1 d . . . H70A H -0.1867 0.3504 0.5647 0.115 Uiso 1 1 calc R . . C71 C -0.2471(4) 0.4129(3) 0.5186(4) 0.171(4) Uani 1 1 d . . . H71A H -0.2029 0.4318 0.5072 0.257 Uiso 1 1 calc R . . H71B H -0.2656 0.4350 0.5467 0.257 Uiso 1 1 calc R . . H71C H -0.2849 0.4114 0.4906 0.257 Uiso 1 1 calc R . . C72 C -0.1977(4) 0.3180(3) 0.4901(3) 0.148(3) Uani 1 1 d . . . H72A H -0.1569 0.3406 0.4777 0.222 Uiso 1 1 calc R . . H72B H -0.2373 0.3152 0.4633 0.222 Uiso 1 1 calc R . . H72C H -0.1803 0.2791 0.4995 0.222 Uiso 1 1 calc R . . O1 O 0.22892(16) 0.36592(10) 0.51861(9) 0.146(2) Uani 1 1 d D . . O2 O 0.30361(11) 0.10505(12) 0.68250(9) 0.1138(15) Uani 1 1 d D . . O3 O -0.32159(12) 0.36106(13) 0.70230(9) 0.1390(17) Uani 1 1 d D . . O4 O -0.27636(16) 0.13482(10) 0.50562(9) 0.1345(18) Uani 1 1 d D . . C73 C 0.22920(19) 0.42597(12) 0.50424(12) 0.215(5) Uani 1 1 d D . . H73A H 0.2485 0.4502 0.5330 0.258 Uiso 1 1 calc R . . H73B H 0.1787 0.4391 0.4937 0.258 Uiso 1 1 calc R . . C74 C 0.2797(2) 0.43083(10) 0.45939(12) 0.385(9) Uani 1 1 d D . . H74A H 0.3209 0.4578 0.4679 0.462 Uiso 1 1 calc R . . H74B H 0.2515 0.4453 0.4287 0.462 Uiso 1 1 calc R . . C75 C 0.30917(17) 0.36847(12) 0.45042(11) 0.398(9) Uani 1 1 d D . . H75A H 0.2987 0.3567 0.4147 0.477 Uiso 1 1 calc R . . H75B H 0.3630 0.3666 0.4586 0.477 Uiso 1 1 calc R . . C76 C 0.2678(2) 0.32865(11) 0.48645(14) 0.204(5) Uani 1 1 d D . . H76A H 0.2330 0.3030 0.4667 0.244 Uiso 1 1 calc R . . H76B H 0.3032 0.3042 0.5069 0.244 Uiso 1 1 calc R . . C77 C 0.35803(16) 0.09235(17) 0.64648(10) 0.132(3) Uani 1 1 d D . . H77A H 0.3767 0.1286 0.6320 0.158 Uiso 1 1 calc R . . H77B H 0.3364 0.0680 0.6185 0.158 Uiso 1 1 calc R . . C78 C 0.42096(13) 0.0595(2) 0.67643(10) 0.254(5) Uani 1 1 d D . . H78A H 0.4655 0.0841 0.6806 0.305 Uiso 1 1 calc R . . H78B H 0.4335 0.0236 0.6585 0.305 Uiso 1 1 calc R . . C79 C 0.39184(15) 0.04497(16) 0.72871(10) 0.211(5) Uani 1 1 d D . . H79A H 0.3849 0.0026 0.7322 0.253 Uiso 1 1 calc R . . H79B H 0.4270 0.0583 0.7564 0.253 Uiso 1 1 calc R . . C80 C 0.31755(15) 0.07695(19) 0.73090(11) 0.169(3) Uani 1 1 d D . . H80A H 0.2777 0.0491 0.7370 0.203 Uiso 1 1 calc R . . H80B H 0.3203 0.1060 0.7585 0.203 Uiso 1 1 calc R . . C81 C -0.38632(17) 0.37763(19) 0.67168(10) 0.178(4) Uani 1 1 d D . . H81A H -0.4127 0.3429 0.6580 0.214 Uiso 1 1 calc R . . H81B H -0.3730 0.4022 0.6430 0.214 Uiso 1 1 calc R . . C82 C -0.43518(13) 0.41203(18) 0.70714(11) 0.279(5) Uani 1 1 d D . . H82A H -0.4466 0.4510 0.6930 0.334 Uiso 1 1 calc R . . H82B H -0.4820 0.3912 0.7113 0.334 Uiso 1 1 calc R . . C83 C -0.38996(17) 0.41716(16) 0.75877(9) 0.277(7) Uani 1 1 d D . . H83A H -0.3726 0.4574 0.7645 0.332 Uiso 1 1 calc R . . H83B H -0.4202 0.4058 0.7869 0.332 Uiso 1 1 calc R . . C84 C -0.32391(16) 0.37530(19) 0.75532(11) 0.227(4) Uani 1 1 d D . . H84A H -0.2776 0.3943 0.7680 0.273 Uiso 1 1 calc R . . H84B H -0.3311 0.3399 0.7756 0.273 Uiso 1 1 calc R . . C85 C -0.2676(2) 0.08179(13) 0.47781(11) 0.206(4) Uani 1 1 d D . . H85A H -0.2866 0.0484 0.4966 0.247 Uiso 1 1 calc R . . H85B H -0.2151 0.0749 0.4724 0.247 Uiso 1 1 calc R . . C86 C -0.3126(2) 0.08959(12) 0.42623(10) 0.235(5) Uani 1 1 d D . . H86A H -0.2793 0.0918 0.3982 0.282 Uiso 1 1 calc R . . H86B H -0.3468 0.0567 0.4198 0.282 Uiso 1 1 calc R . . C87 C -0.35576(18) 0.14702(13) 0.43070(10) 0.230(5) Uani 1 1 d D . . H87A H -0.3456 0.1735 0.4025 0.276 Uiso 1 1 calc R . . H87B H -0.4093 0.1393 0.4296 0.276 Uiso 1 1 calc R . . C88 C -0.3292(2) 0.17424(13) 0.48217(11) 0.181(4) Uani 1 1 d D . . H88A H -0.3062 0.2125 0.4769 0.217 Uiso 1 1 calc R . . H88B H -0.3711 0.1795 0.5038 0.217 Uiso 1 1 calc R . . C89 C 0.5509(4) -0.0453(2) 0.5249(2) 0.259(6) Uiso 1 1 d D . . C90 C 0.5202(2) -0.00035(13) 0.55371(17) 0.280(6) Uiso 1 1 d D . . C91 C 0.4717(3) 0.0440(2) 0.5350(4) 0.243(11) Uiso 0.50 1 d PD . . C91' C 0.4742(3) 0.0420(2) 0.5291(3) 0.230(10) Uiso 0.50 1 d PD . . 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 0.05412(10) 0.05909(10) 0.08614(14) 0.00290(10) 0.00614(10) 0.00276(8) Yb2 0.05642(10) 0.06152(10) 0.08516(14) -0.00896(10) 0.00297(10) 0.00392(9) Na1 0.0980(13) 0.0813(12) 0.1288(17) 0.0188(12) 0.0243(13) 0.0099(11) Na2 0.0838(13) 0.1067(14) 0.1137(16) -0.0272(13) -0.0004(12) 0.0108(11) Li1 0.055(4) 0.113(6) 0.094(6) 0.017(5) -0.002(4) 0.012(4) Li2 0.051(4) 0.139(7) 0.104(7) -0.009(6) -0.020(4) 0.031(4) N1 0.064(2) 0.0519(17) 0.073(2) 0.0046(18) 0.0077(18) -0.0045(16) C1 0.072(3) 0.051(2) 0.165(5) -0.032(3) 0.030(3) -0.004(2) C2 0.068(3) 0.063(3) 0.148(5) 0.021(3) -0.014(3) -0.010(2) C3 0.109(4) 0.068(3) 0.161(6) 0.023(4) 0.014(4) -0.013(3) C4 0.103(4) 0.073(3) 0.164(6) -0.013(4) 0.019(4) -0.035(3) C5 0.083(3) 0.089(3) 0.148(5) -0.009(4) 0.002(4) -0.026(3) C6 0.068(3) 0.075(3) 0.097(4) -0.023(3) 0.012(3) -0.014(2) C7 0.089(3) 0.077(3) 0.119(4) 0.018(3) 0.012(3) 0.000(3) C8 0.121(5) 0.094(4) 0.174(6) 0.051(4) -0.043(4) -0.008(3) C9 0.135(5) 0.122(4) 0.089(4) -0.003(4) -0.021(4) -0.020(4) C10 0.098(4) 0.095(3) 0.127(5) -0.007(4) -0.028(4) -0.028(3) C11 0.118(5) 0.213(7) 0.111(5) -0.048(5) -0.020(4) 0.043(5) C12 0.110(5) 0.323(11) 0.110(5) -0.009(7) 0.034(4) 0.019(7) N2 0.066(2) 0.070(2) 0.108(3) 0.005(2) 0.027(2) 0.0072(18) C13 0.046(2) 0.057(2) 0.091(3) -0.025(2) -0.008(2) -0.0045(18) C14 0.076(3) 0.055(2) 0.091(3) -0.010(2) -0.002(3) -0.014(2) C15 0.092(4) 0.094(4) 0.138(5) -0.011(4) 0.026(4) -0.008(3) C16 0.097(4) 0.060(3) 0.193(7) 0.002(4) -0.021(4) -0.020(3) C17 0.093(4) 0.082(3) 0.150(5) 0.005(4) 0.010(4) -0.006(3) C18 0.072(3) 0.067(3) 0.131(5) 0.009(3) -0.004(3) -0.015(2) C19 0.091(3) 0.072(3) 0.126(5) 0.005(3) 0.006(3) -0.014(3) C20 0.128(5) 0.131(4) 0.140(5) -0.074(4) 0.047(4) -0.029(4) C21 0.130(5) 0.099(4) 0.109(4) -0.017(4) -0.007(4) -0.010(4) C22 0.121(4) 0.094(4) 0.107(4) -0.001(3) 0.003(4) -0.008(3) C23 0.132(6) 0.399(14) 0.117(6) -0.031(8) -0.060(5) 0.055(8) C24 0.130(6) 0.285(10) 0.133(6) 0.054(6) 0.035(5) 0.002(7) N3 0.058(2) 0.069(2) 0.090(3) 0.006(2) 0.0088(19) -0.0008(17) C25 0.060(3) 0.075(3) 0.075(3) 0.013(2) 0.000(2) 0.003(2) C26 0.051(2) 0.076(3) 0.091(3) -0.007(3) 0.007(2) 0.001(2) C27 0.079(3) 0.084(3) 0.150(5) 0.000(4) 0.002(4) -0.011(3) C28 0.067(3) 0.103(4) 0.133(5) -0.009(4) 0.025(3) 0.006(3) C29 0.103(3) 0.092(3) 0.116(4) 0.002(3) 0.052(3) 0.009(3) C30 0.089(3) 0.054(2) 0.084(3) 0.011(2) 0.008(3) -0.013(2) C31 0.082(3) 0.070(3) 0.133(5) -0.003(3) 0.004(3) -0.005(3) C32 0.122(5) 0.109(4) 0.158(6) -0.004(5) -0.022(5) -0.001(4) C33 0.116(4) 0.107(4) 0.199(7) -0.035(5) 0.043(5) -0.031(4) C34 0.082(3) 0.099(4) 0.109(4) -0.008(3) 0.013(3) -0.006(3) C35 0.116(5) 0.286(10) 0.201(8) 0.066(8) -0.053(5) -0.069(6) C36 0.151(7) 0.120(4) 0.373(12) -0.121(6) -0.018(8) 0.001(5) N4 0.112(3) 0.117(3) 0.113(3) 0.044(3) 0.043(3) 0.033(3) C37 0.066(3) 0.101(3) 0.097(3) 0.032(3) 0.028(3) 0.022(2) C38 0.098(4) 0.084(3) 0.130(5) 0.040(3) 0.007(4) -0.010(3) C39 0.154(6) 0.184(7) 0.107(5) 0.010(5) -0.001(5) 0.021(6) C40 0.143(6) 0.105(4) 0.184(6) 0.063(4) 0.021(5) 0.015(4) C41 0.121(5) 0.107(4) 0.123(5) 0.006(4) 0.014(4) 0.027(4) C42 0.070(3) 0.108(3) 0.108(4) 0.026(3) 0.029(3) 0.029(3) C43 0.107(4) 0.128(5) 0.161(6) 0.022(5) 0.015(4) 0.016(4) C44 0.178(9) 0.184(8) 0.60(2) -0.141(11) 0.105(12) -0.054(7) C45 0.222(10) 0.229(9) 0.219(10) -0.047(8) -0.020(9) -0.054(8) C46 0.092(4) 0.158(5) 0.112(4) 0.015(4) 0.037(3) 0.013(4) C47 0.098(5) 0.180(7) 0.183(7) 0.013(6) 0.009(5) 0.015(5) C48 0.161(8) 0.330(13) 0.248(12) -0.001(11) 0.014(8) -0.085(8) N5 0.096(3) 0.127(3) 0.133(4) -0.067(3) -0.009(3) 0.019(3) C49 0.073(3) 0.089(3) 0.107(4) -0.040(3) -0.008(3) 0.032(2) C50 0.102(4) 0.250(7) 0.122(5) -0.087(5) 0.034(4) -0.005(5) C51 0.196(8) 0.181(7) 0.127(6) -0.045(5) 0.023(5) 0.024(6) C52 0.214(8) 0.153(6) 0.129(6) -0.048(5) -0.004(6) 0.025(6) C53 0.132(5) 0.106(4) 0.203(7) -0.052(5) 0.005(5) 0.000(4) C54 0.091(4) 0.150(5) 0.140(5) -0.051(4) -0.017(4) 0.040(3) C55 0.339(12) 0.137(6) 0.160(7) -0.023(6) 0.103(7) -0.043(7) C56 0.195(10) 0.233(10) 0.396(18) 0.100(11) 0.012(11) 0.013(9) C57 0.179(7) 0.429(12) 0.299(12) 0.124(9) 0.026(7) -0.163(7) C58 0.167(7) 0.133(5) 0.180(7) -0.030(5) -0.052(6) -0.009(5) C59 0.174(8) 0.335(14) 0.354(14) 0.111(12) -0.116(8) -0.015(10) C60 0.204(9) 0.184(8) 0.263(11) 0.017(9) 0.060(8) 0.010(7) N6 0.059(2) 0.066(2) 0.117(3) -0.011(2) 0.001(2) 0.0157(17) C61 0.077(3) 0.060(2) 0.096(3) -0.027(2) -0.007(3) 0.019(2) C62 0.057(3) 0.073(3) 0.118(4) -0.007(3) 0.007(3) -0.007(2) C63 0.054(3) 0.112(4) 0.176(6) 0.038(4) 0.012(3) -0.007(3) C64 0.050(3) 0.126(5) 0.236(8) 0.010(5) -0.029(4) 0.015(3) C65 0.072(3) 0.096(3) 0.122(4) 0.007(4) 0.004(3) -0.005(3) C66 0.067(3) 0.102(3) 0.109(4) -0.007(3) -0.002(3) 0.021(3) C67 0.079(3) 0.120(4) 0.105(4) -0.002(4) 0.023(3) -0.005(3) C68 0.107(4) 0.115(4) 0.214(8) 0.023(5) 0.009(5) -0.033(4) C69 0.125(5) 0.195(7) 0.139(6) -0.002(6) 0.017(5) 0.042(5) C70 0.078(3) 0.078(3) 0.131(5) 0.025(3) -0.013(3) -0.014(3) C71 0.106(5) 0.119(5) 0.288(11) 0.027(6) 0.005(6) 0.014(4) C72 0.125(5) 0.148(6) 0.172(7) -0.018(6) 0.029(5) -0.008(5) O1 0.150(4) 0.107(3) 0.186(4) 0.034(3) 0.043(3) 0.007(3) O2 0.079(2) 0.131(3) 0.132(3) 0.045(2) 0.014(2) 0.028(2) O3 0.077(2) 0.158(3) 0.181(4) -0.080(3) -0.001(3) 0.023(2) O4 0.144(3) 0.121(3) 0.132(3) -0.041(3) -0.044(3) 0.025(3) C73 0.282(10) 0.095(5) 0.280(10) 0.058(6) 0.116(8) 0.000(6) C74 0.63(2) 0.231(9) 0.326(11) 0.163(8) 0.247(12) 0.149(13) C75 0.66(2) 0.146(8) 0.417(16) -0.006(10) 0.296(14) -0.083(12) C76 0.248(9) 0.125(5) 0.247(10) 0.032(7) 0.089(7) 0.051(6) C77 0.095(4) 0.124(4) 0.181(6) 0.012(5) 0.052(4) 0.030(3) C78 0.172(7) 0.324(9) 0.268(10) 0.146(7) 0.029(7) 0.132(6) C79 0.120(6) 0.359(12) 0.152(7) 0.047(8) 0.011(5) 0.083(7) C80 0.095(4) 0.248(7) 0.169(6) 0.112(5) 0.039(4) 0.065(4) C81 0.124(5) 0.181(6) 0.227(9) -0.061(7) -0.017(6) 0.042(5) C82 0.182(7) 0.357(10) 0.299(11) -0.129(9) 0.032(7) 0.129(6) C83 0.240(12) 0.406(16) 0.182(9) -0.117(10) -0.002(9) -0.037(12) C84 0.067(4) 0.307(8) 0.309(9) -0.180(6) 0.021(5) 0.028(5) C85 0.236(9) 0.190(7) 0.180(7) -0.071(6) -0.082(7) 0.050(7) C86 0.223(9) 0.212(8) 0.256(10) -0.095(7) -0.095(8) 0.073(7) C87 0.204(7) 0.254(9) 0.216(8) -0.053(8) -0.111(6) 0.101(7) C88 0.189(7) 0.190(7) 0.154(7) -0.029(6) -0.066(6) 0.021(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 Yb1 N3 2.101(4) . ? Yb1 N4 2.179(5) . ? Yb1 N2 2.286(4) . ? Yb1 N1 2.316(3) . ? Yb1 Li1 2.842(8) . ? Yb1 C1 3.182(4) . ? Yb1 Yb2 3.3409(6) . ? Yb1 Na1 3.591(2) . ? Yb2 N6 2.126(4) . ? Yb2 N1 2.166(3) . ? Yb2 N5 2.196(5) . ? Yb2 N2 2.221(4) . ? Yb2 Li2 2.804(8) . ? Yb2 C13 3.171(2) . ? Yb2 Na2 3.628(2) . ? Na1 O1 2.315(3) . ? Na1 N3 2.456(4) . ? Na1 C25 2.691(5) . ? Na1 C2 2.771(5) . ? Na1 C1 2.811(6) . ? Na1 C26 2.909(5) . ? Na1 C3 2.960(6) . ? Na1 C6 3.003(6) . ? Na1 C31 3.020(6) . ? Na2 O4 2.322(3) . ? Na2 N6 2.471(4) . ? Na2 C61 2.631(5) . ? Na2 C14 2.721(4) . ? Na2 C62 2.863(5) . ? Na2 C67 2.934(6) . ? Na2 C18 3.101(4) . ? Li1 O2 1.944(9) . ? Li1 N3 2.050(10) . ? Li1 N4 2.060(10) . ? Li1 C25 2.518(10) . ? Li1 C37 2.790(10) . ? Li2 O3 1.939(9) . ? Li2 N6 1.977(11) . ? Li2 N5 1.997(9) . ? Li2 C61 2.455(11) . ? N1 C1 1.387(6) . ? C1 C2 1.392(8) . ? C1 C6 1.428(7) . ? C2 C3 1.402(7) . ? C2 C7 1.535(8) . ? C3 C4 1.333(9) . ? C4 C5 1.373(9) . ? C5 C6 1.394(7) . ? C6 C10 1.569(8) . ? C7 C9 1.493(8) . ? C7 C8 1.531(8) . ? C10 C11 1.524(8) . ? C10 C12 1.537(9) . ? N2 C13 1.384(4) . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C14 C19 1.512(7) . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C18 C22 1.520(7) . ? C19 C21 1.469(8) . ? C19 C20 1.533(8) . ? C22 C23 1.490(10) . ? C22 C24 1.578(10) . ? N3 C25 1.448(6) . ? C25 C30 1.416(7) . ? C25 C26 1.435(6) . ? C26 C27 1.429(8) . ? C26 C31 1.501(8) . ? C27 C28 1.377(9) . ? C28 C29 1.399(8) . ? C29 C30 1.468(7) . ? C30 C34 1.547(7) . ? C31 C32 1.457(9) . ? C31 C33 1.506(8) . ? C34 C35 1.416(10) . ? C34 C36 1.552(9) . ? N4 C37 1.345(7) . ? C37 C38 1.394(8) . ? C37 C42 1.425(7) . ? C38 C39 1.365(9) . ? C38 C43 1.487(9) . ? C39 C40 1.474(10) . ? C40 C41 1.355(10) . ? C41 C42 1.341(8) . ? C42 C46 1.545(8) . ? C43 C44 1.363(15) . ? C43 C45 1.419(12) . ? C46 C47 1.429(9) . ? C46 C48 1.440(12) . ? N5 C49 1.435(6) . ? C49 C50 1.3900 . ? C49 C54 1.3900 . ? C50 C51 1.3900 . ? C50 C55 1.630(9) . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C58 1.562(9) . ? C55 C56 1.462(16) . ? C55 C57 1.472(14) . ? C58 C59 1.536(13) . ? C58 C60 1.559(13) . ? N6 C61 1.361(6) . ? C61 C66 1.403(7) . ? C61 C62 1.465(7) . ? C62 C63 1.430(7) . ? C62 C67 1.440(8) . ? C63 C64 1.414(10) . ? C64 C65 1.326(8) . ? C65 C66 1.379(7) . ? C66 C70 1.599(8) . ? C67 C69 1.547(9) . ? C67 C68 1.596(8) . ? C70 C72 1.526(9) . ? C70 C71 1.567(8) . ? O1 C76 1.400(4) . ? O1 C73 1.407(3) . ? O2 C80 1.414(4) . ? O2 C77 1.419(4) . ? O3 C81 1.408(4) . ? O3 C84 1.414(4) . ? O4 C88 1.406(4) . ? O4 C85 1.412(4) . ? C73 C74 1.520(4) . ? C74 C75 1.528(4) . ? C75 C76 1.522(4) . ? C77 C78 1.516(4) . ? C78 C79 1.519(4) . ? C79 C80 1.514(4) . ? C81 C82 1.521(4) . ? C82 C83 1.521(4) . ? C83 C84 1.518(4) . ? C85 C86 1.523(4) . ? C86 C87 1.518(4) . ? C87 C88 1.517(4) . ? C89 C90 1.394(6) . ? C89 C91' 1.442(10) 3_656 ? C89 C91 1.579(12) 3_656 ? C90 C91' 1.390(6) . ? C90 C91 1.390(6) . ? C91 C89 1.579(12) 3_656 ? C91' C89 1.442(10) 3_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 N3 Yb1 N4 92.06(16) . . ? N3 Yb1 N2 149.46(15) . . ? N4 Yb1 N2 97.33(16) . . ? N3 Yb1 N1 111.08(13) . . ? N4 Yb1 N1 136.11(15) . . ? N2 Yb1 N1 81.47(12) . . ? N3 Yb1 Li1 46.0(2) . . ? N4 Yb1 Li1 46.1(2) . . ? N2 Yb1 Li1 133.7(2) . . ? N1 Yb1 Li1 143.4(2) . . ? N3 Yb1 C1 89.54(13) . . ? N4 Yb1 C1 133.55(16) . . ? N2 Yb1 C1 104.32(13) . . ? N1 Yb1 C1 23.03(12) . . ? Li1 Yb1 C1 121.5(2) . . ? N3 Yb1 Yb2 144.61(10) . . ? N4 Yb1 Yb2 122.86(13) . . ? N2 Yb1 Yb2 41.41(9) . . ? N1 Yb1 Yb2 40.13(8) . . ? Li1 Yb1 Yb2 168.83(19) . . ? C1 Yb1 Yb2 63.11(9) . . ? N3 Yb1 Na1 41.65(10) . . ? N4 Yb1 Na1 123.87(13) . . ? N2 Yb1 Na1 138.80(11) . . ? N1 Yb1 Na1 69.45(9) . . ? Li1 Yb1 Na1 83.13(19) . . ? C1 Yb1 Na1 48.58(10) . . ? Yb2 Yb1 Na1 105.66(4) . . ? N6 Yb2 N1 146.57(14) . . ? N6 Yb2 N5 89.52(17) . . ? N1 Yb2 N5 103.80(16) . . ? N6 Yb2 N2 108.61(14) . . ? N1 Yb2 N2 86.39(13) . . ? N5 Yb2 N2 129.75(17) . . ? N6 Yb2 Li2 44.7(2) . . ? N1 Yb2 Li2 136.3(2) . . ? N5 Yb2 Li2 45.1(2) . . ? N2 Yb2 Li2 136.0(2) . . ? N6 Yb2 C13 87.83(10) . . ? N1 Yb2 C13 107.77(9) . . ? N5 Yb2 C13 125.28(14) . . ? N2 Yb2 C13 21.85(10) . . ? Li2 Yb2 C13 115.6(2) . . ? N6 Yb2 Yb1 143.63(11) . . ? N1 Yb2 Yb1 43.55(8) . . ? N5 Yb2 Yb1 125.30(13) . . ? N2 Yb2 Yb1 42.91(9) . . ? Li2 Yb2 Yb1 169.4(2) . . ? C13 Yb2 Yb1 64.57(4) . . ? N6 Yb2 Na2 41.35(10) . . ? N1 Yb2 Na2 136.58(10) . . ? N5 Yb2 Na2 119.60(13) . . ? N2 Yb2 Na2 67.55(10) . . ? Li2 Yb2 Na2 81.1(2) . . ? C13 Yb2 Na2 47.99(5) . . ? Yb1 Yb2 Na2 104.48(4) . . ? O1 Na1 N3 129.77(15) . . ? O1 Na1 C25 100.89(14) . . ? N3 Na1 C25 32.27(13) . . ? O1 Na1 C2 103.95(16) . . ? N3 Na1 C2 115.54(16) . . ? C25 Na1 C2 146.90(16) . . ? O1 Na1 C1 132.58(15) . . ? N3 Na1 C1 92.05(15) . . ? C25 Na1 C1 124.09(16) . . ? C2 Na1 C1 28.86(16) . . ? O1 Na1 C26 93.92(14) . . ? N3 Na1 C26 54.16(13) . . ? C25 Na1 C26 29.36(13) . . ? C2 Na1 C26 160.92(19) . . ? C1 Na1 C26 132.45(17) . . ? O1 Na1 C3 85.07(16) . . ? N3 Na1 C3 141.81(18) . . ? C25 Na1 C3 173.94(19) . . ? C2 Na1 C3 28.08(15) . . ? C1 Na1 C3 49.88(16) . . ? C26 Na1 C3 152.38(17) . . ? O1 Na1 C6 135.89(13) . . ? N3 Na1 C6 94.21(15) . . ? C25 Na1 C6 119.98(16) . . ? C2 Na1 C6 48.59(16) . . ? C1 Na1 C6 28.19(14) . . ? C26 Na1 C6 113.16(16) . . ? C3 Na1 C6 54.70(17) . . ? O1 Na1 C31 107.37(16) . . ? N3 Na1 C31 64.97(13) . . ? C25 Na1 C31 53.85(14) . . ? C2 Na1 C31 134.64(19) . . ? C1 Na1 C31 110.84(18) . . ? C26 Na1 C31 29.26(14) . . ? C3 Na1 C31 125.58(18) . . ? C6 Na1 C31 86.31(16) . . ? O1 Na1 Yb1 152.09(11) . . ? N3 Na1 Yb1 34.64(9) . . ? C25 Na1 Yb1 66.87(11) . . ? C2 Na1 Yb1 81.10(12) . . ? C1 Na1 Yb1 58.08(10) . . ? C26 Na1 Yb1 86.23(11) . . ? C3 Na1 Yb1 107.29(14) . . ? C6 Na1 Yb1 67.60(10) . . ? C31 Na1 Yb1 86.04(12) . . ? O4 Na2 N6 131.11(15) . . ? O4 Na2 C61 103.84(15) . . ? N6 Na2 C61 30.73(14) . . ? O4 Na2 C14 105.11(12) . . ? N6 Na2 C14 113.98(13) . . ? C61 Na2 C14 144.29(15) . . ? O4 Na2 C62 95.32(14) . . ? N6 Na2 C62 54.45(13) . . ? C61 Na2 C62 30.57(14) . . ? C14 Na2 C62 157.83(15) . . ? O4 Na2 C67 107.33(15) . . ? N6 Na2 C67 65.86(15) . . ? C61 Na2 C67 54.35(16) . . ? C14 Na2 C67 132.37(15) . . ? C62 Na2 C67 28.74(16) . . ? O4 Na2 C18 136.70(12) . . ? N6 Na2 C18 91.99(13) . . ? C61 Na2 C18 116.04(14) . . ? C14 Na2 C18 48.32(6) . . ? C62 Na2 C18 110.21(14) . . ? C67 Na2 C18 84.42(14) . . ? O4 Na2 Yb2 151.59(11) . . ? N6 Na2 Yb2 34.64(9) . . ? C61 Na2 Yb2 65.29(11) . . ? C14 Na2 Yb2 79.36(8) . . ? C62 Na2 Yb2 86.79(11) . . ? C67 Na2 Yb2 87.92(12) . . ? C18 Na2 Yb2 66.97(7) . . ? O2 Li1 N3 141.1(5) . . ? O2 Li1 N4 121.6(5) . . ? N3 Li1 N4 97.1(4) . . ? O2 Li1 C25 106.0(4) . . ? N3 Li1 C25 35.1(2) . . ? N4 Li1 C25 132.2(4) . . ? O2 Li1 C37 94.5(4) . . ? N3 Li1 C37 123.8(4) . . ? N4 Li1 C37 27.3(2) . . ? C25 Li1 C37 158.0(4) . . ? O2 Li1 Yb1 169.3(4) . . ? N3 Li1 Yb1 47.5(2) . . ? N4 Li1 Yb1 49.7(2) . . ? C25 Li1 Yb1 82.5(3) . . ? C37 Li1 Yb1 76.3(2) . . ? O3 Li2 N6 139.0(5) . . ? O3 Li2 N5 120.5(5) . . ? N6 Li2 N5 100.0(4) . . ? O3 Li2 C61 105.6(4) . . ? N6 Li2 C61 33.6(2) . . ? N5 Li2 C61 133.6(5) . . ? O3 Li2 Yb2 166.8(5) . . ? N6 Li2 Yb2 49.1(2) . . ? N5 Li2 Yb2 51.1(2) . . ? C61 Li2 Yb2 82.6(3) . . ? C1 N1 Yb2 147.2(3) . . ? C1 N1 Yb1 116.2(3) . . ? Yb2 N1 Yb1 96.32(12) . . ? N1 C1 C2 122.6(5) . . ? N1 C1 C6 121.9(5) . . ? C2 C1 C6 115.5(4) . . ? N1 C1 Na1 109.4(3) . . ? C2 C1 Na1 74.0(3) . . ? C6 C1 Na1 83.4(3) . . ? N1 C1 Yb1 40.78(19) . . ? C2 C1 Yb1 127.9(4) . . ? C6 C1 Yb1 99.7(3) . . ? Na1 C1 Yb1 73.34(11) . . ? C1 C2 C3 121.4(5) . . ? C1 C2 C7 118.2(4) . . ? C3 C2 C7 120.2(5) . . ? C1 C2 Na1 77.2(3) . . ? C3 C2 Na1 83.5(3) . . ? C7 C2 Na1 105.9(3) . . ? C4 C3 C2 121.9(6) . . ? C4 C3 Na1 89.3(3) . . ? C2 C3 Na1 68.5(3) . . ? C3 C4 C5 119.0(5) . . ? C4 C5 C6 121.1(5) . . ? C5 C6 C1 120.8(5) . . ? C5 C6 C10 116.6(5) . . ? C1 C6 C10 122.1(4) . . ? C5 C6 Na1 86.0(4) . . ? C1 C6 Na1 68.4(3) . . ? C10 C6 Na1 123.7(3) . . ? C9 C7 C8 109.0(5) . . ? C9 C7 C2 113.0(5) . . ? C8 C7 C2 111.4(4) . . ? C11 C10 C12 112.1(5) . . ? C11 C10 C6 116.2(5) . . ? C12 C10 C6 110.0(5) . . ? C13 N2 Yb2 121.5(2) . . ? C13 N2 Yb1 141.9(3) . . ? Yb2 N2 Yb1 95.68(14) . . ? N2 C13 C14 119.1(2) . . ? N2 C13 C18 120.9(2) . . ? C14 C13 C18 120.0 . . ? N2 C13 Yb2 36.67(16) . . ? C14 C13 Yb2 124.05(10) . . ? C18 C13 Yb2 103.05(10) . . ? C13 C14 C15 120.0 . . ? C13 C14 C19 122.5(3) . . ? C15 C14 C19 117.5(3) . . ? C13 C14 Na2 78.44(11) . . ? C15 C14 Na2 85.80(10) . . ? C19 C14 Na2 106.3(3) . . ? C14 C15 C16 120.0 . . ? C17 C16 C15 120.0 . . ? C18 C17 C16 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 C22 117.3(3) . . ? C13 C18 C22 122.4(3) . . ? C17 C18 Na2 86.32(9) . . ? C13 C18 Na2 64.38(10) . . ? C22 C18 Na2 126.0(3) . . ? C21 C19 C14 112.1(5) . . ? C21 C19 C20 110.7(5) . . ? C14 C19 C20 115.2(4) . . ? C23 C22 C18 115.6(5) . . ? C23 C22 C24 109.8(6) . . ? C18 C22 C24 113.3(5) . . ? C25 N3 Li1 90.4(3) . . ? C25 N3 Yb1 172.3(3) . . ? Li1 N3 Yb1 86.4(3) . . ? C25 N3 Na1 82.8(2) . . ? Li1 N3 Na1 145.5(3) . . ? Yb1 N3 Na1 103.71(15) . . ? C30 C25 C26 119.1(4) . . ? C30 C25 N3 122.3(4) . . ? C26 C25 N3 118.3(4) . . ? C30 C25 Li1 111.2(4) . . ? C26 C25 Li1 97.9(4) . . ? N3 C25 Li1 54.5(3) . . ? C30 C25 Na1 127.2(3) . . ? C26 C25 Na1 83.8(3) . . ? N3 C25 Na1 64.9(2) . . ? Li1 C25 Na1 111.4(3) . . ? C27 C26 C25 115.9(4) . . ? C27 C26 C31 119.2(4) . . ? C25 C26 C31 124.8(4) . . ? C27 C26 Na1 130.5(4) . . ? C25 C26 Na1 66.9(2) . . ? C31 C26 Na1 79.5(3) . . ? C28 C27 C26 127.0(5) . . ? C27 C28 C29 117.1(5) . . ? C28 C29 C30 119.4(5) . . ? C25 C30 C29 121.1(4) . . ? C25 C30 C34 120.5(4) . . ? C29 C30 C34 117.5(4) . . ? C32 C31 C26 114.6(4) . . ? C32 C31 C33 110.0(5) . . ? C26 C31 C33 110.0(5) . . ? C32 C31 Na1 160.2(4) . . ? C26 C31 Na1 71.3(3) . . ? C33 C31 Na1 83.7(3) . . ? C35 C34 C30 113.8(5) . . ? C35 C34 C36 113.7(7) . . ? C30 C34 C36 108.7(5) . . ? C37 N4 Li1 108.2(4) . . ? C37 N4 Yb1 161.1(4) . . ? Li1 N4 Yb1 84.2(3) . . ? N4 C37 C38 119.8(5) . . ? N4 C37 C42 122.6(5) . . ? C38 C37 C42 117.4(5) . . ? N4 C37 Li1 44.5(3) . . ? C38 C37 Li1 122.1(4) . . ? C42 C37 Li1 105.2(4) . . ? C39 C38 C37 122.2(6) . . ? C39 C38 C43 116.7(6) . . ? C37 C38 C43 121.1(5) . . ? C38 C39 C40 116.7(6) . . ? C41 C40 C39 121.6(6) . . ? C42 C41 C40 119.1(6) . . ? C41 C42 C37 122.9(5) . . ? C41 C42 C46 116.7(5) . . ? C37 C42 C46 120.5(5) . . ? C44 C43 C45 108.7(8) . . ? C44 C43 C38 117.1(7) . . ? C45 C43 C38 113.7(6) . . ? C47 C46 C48 106.9(7) . . ? C47 C46 C42 114.6(6) . . ? C48 C46 C42 107.6(6) . . ? C49 N5 Li2 113.4(4) . . ? C49 N5 Yb2 150.6(3) . . ? Li2 N5 Yb2 83.8(3) . . ? C50 C49 C54 120.0 . . ? C50 C49 N5 120.6(3) . . ? C54 C49 N5 119.2(3) . . ? C51 C50 C49 120.0 . . ? C51 C50 C55 116.4(4) . . ? C49 C50 C55 123.1(4) . . ? C52 C51 C50 120.0 . . ? C53 C52 C51 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C49 120.0 . . ? C53 C54 C58 117.1(4) . . ? C49 C54 C58 122.9(4) . . ? C56 C55 C57 106.6(9) . . ? C56 C55 C50 117.2(7) . . ? C57 C55 C50 108.3(8) . . ? C59 C58 C60 110.4(7) . . ? C59 C58 C54 114.7(7) . . ? C60 C58 C54 113.3(6) . . ? C61 N6 Li2 92.9(4) . . ? C61 N6 Yb2 172.5(3) . . ? Li2 N6 Yb2 86.2(3) . . ? C61 N6 Na2 81.2(3) . . ? Li2 N6 Na2 143.7(4) . . ? Yb2 N6 Na2 104.01(15) . . ? N6 C61 C66 124.8(4) . . ? N6 C61 C62 121.4(4) . . ? C66 C61 C62 113.8(4) . . ? N6 C61 Li2 53.5(3) . . ? C66 C61 Li2 117.4(4) . . ? C62 C61 Li2 98.8(4) . . ? N6 C61 Na2 68.1(2) . . ? C66 C61 Na2 122.8(4) . . ? C62 C61 Na2 83.5(3) . . ? Li2 C61 Na2 112.4(3) . . ? C63 C62 C67 116.8(5) . . ? C63 C62 C61 120.0(5) . . ? C67 C62 C61 123.2(4) . . ? C63 C62 Na2 128.7(4) . . ? C67 C62 Na2 78.3(3) . . ? C61 C62 Na2 65.9(2) . . ? C64 C63 C62 120.8(5) . . ? C65 C64 C63 118.3(5) . . ? C64 C65 C66 122.8(6) . . ? C65 C66 C61 124.1(5) . . ? C65 C66 C70 119.6(5) . . ? C61 C66 C70 116.2(4) . . ? C62 C67 C69 114.5(5) . . ? C62 C67 C68 113.1(5) . . ? C69 C67 C68 109.4(5) . . ? C62 C67 Na2 72.9(3) . . ? C69 C67 Na2 160.5(4) . . ? C68 C67 Na2 82.0(4) . . ? C72 C70 C71 104.9(6) . . ? C72 C70 C66 109.3(5) . . ? C71 C70 C66 115.5(5) . . ? C76 O1 C73 114.3(2) . . ? C76 O1 Na1 117.02(18) . . ? C73 O1 Na1 128.4(2) . . ? C80 O2 C77 113.9(2) . . ? C80 O2 Li1 121.8(3) . . ? C77 O2 Li1 124.4(3) . . ? C81 O3 C84 114.3(2) . . ? C81 O3 Li2 128.1(3) . . ? C84 O3 Li2 117.1(3) . . ? C88 O4 C85 114.2(2) . . ? C88 O4 Na2 115.44(18) . . ? C85 O4 Na2 130.3(2) . . ? O1 C73 C74 106.5(2) . . ? C73 C74 C75 106.1(2) . . ? C76 C75 C74 105.5(2) . . ? O1 C76 C75 106.8(2) . . ? O2 C77 C78 106.1(2) . . ? C77 C78 C79 106.1(2) . . ? C80 C79 C78 106.3(2) . . ? O2 C80 C79 106.5(2) . . ? O3 C81 C82 106.0(2) . . ? C83 C82 C81 106.2(2) . . ? C84 C83 C82 105.6(2) . . ? O3 C84 C83 105.7(2) . . ? O4 C85 C86 106.3(2) . . ? C87 C86 C85 105.8(2) . . ? C88 C87 C86 106.4(2) . . ? O4 C88 C87 106.6(2) . . ? C90 C89 C91' 112.0(5) . 3_656 ? C90 C89 C91 115.5(4) . 3_656 ? C91' C89 C91 3.8(3) 3_656 3_656 ? C91' C90 C91 7.0(6) . . ? C91' C90 C89 119.8(5) . . ? C91 C90 C89 126.6(6) . . ? C90 C91 C89 117.9(6) . 3_656 ? C90 C91' C89 128.1(6) . 3_656 ? _diffrn_measured_fraction_theta_max 0.873 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.873 _refine_diff_density_max 1.338 _refine_diff_density_min -1.069 _refine_diff_density_rms 0.122 #===END data_complex_3.(0.5C6H6) _database_code_CSD 175641 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C91 H137 Li4 N6 Na2 O4 Yb2' _chemical_formula_weight 1798.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.912(4) _cell_length_b 25.454(5) _cell_length_c 22.850(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10418(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3724 _exptl_absorpt_coefficient_mu 1.836 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18983 _diffrn_reflns_av_R_equivalents 0.1126 _diffrn_reflns_av_sigmaI/netI 0.0756 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6245 _reflns_number_gt 5667 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1064P)^2^+6.5561P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00091(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6245 _refine_ls_number_parameters 504 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.1874 _refine_ls_wR_factor_gt 0.1790 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_restrained_S_all 1.187 _refine_ls_shift/su_max 0.00 _refine_ls_shift/su_mean 0.00 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 0.911750(5) 0.152849(4) 0.223120(4) 0.05688(4) Uani 1 1 d . . . Na1 Na 0.79572(6) 0.08305(4) 0.32856(4) 0.0891(4) Uani 1 1 d . . . Li1 Li 0.9834(2) 0.2046(2) 0.13117(19) 0.0950(16) Uani 1 1 d . . . Li2 Li 0.7799(3) 0.1695(2) 0.1630(2) 0.0917(16) Uani 1 1 d . . . N1 N 1.03187(10) 0.15356(7) 0.18704(8) 0.0609(6) Uani 1 1 d . . . N2 N 0.87811(10) 0.20647(8) 0.15706(8) 0.0736(7) Uani 1 1 d . . . N3 N 0.80632(10) 0.11502(8) 0.22691(7) 0.0633(6) Uani 1 1 d . . . O1 O 0.69363(8) 0.18630(7) 0.11453(8) 0.1134(7) Uani 1 1 d D . . O2 O 0.74506(11) 0.00658(7) 0.36403(7) 0.1264(9) Uani 1 1 d D . . C1 C 0.92404(12) 0.14384(9) 0.35900(10) 0.0609(7) Uani 1 1 d . . . C2 C 0.87136(15) 0.18372(11) 0.37999(10) 0.0779(8) Uani 1 1 d . . . C3 C 0.82649(15) 0.17319(12) 0.42953(11) 0.0897(10) Uani 1 1 d . . . H3A H 0.7939 0.1990 0.4430 0.108 Uiso 1 1 calc R . . C4 C 0.82966(16) 0.12637(13) 0.45806(11) 0.0983(11) Uani 1 1 d . . . H4A H 0.7987 0.1200 0.4900 0.118 Uiso 1 1 calc R . . C5 C 0.87923(15) 0.08843(12) 0.43926(10) 0.0856(9) Uani 1 1 d . . . H5A H 0.8810 0.0564 0.4587 0.103 Uiso 1 1 calc R . . C6 C 0.92600(13) 0.09679(11) 0.39248(10) 0.0705(8) Uani 1 1 d . . . C7 C 0.86630(13) 0.23841(9) 0.35043(12) 0.1015(11) Uani 1 1 d D . . C8 C 0.7894(2) 0.26460(15) 0.3546(2) 0.1715(19) Uani 1 1 d . . . H8A H 0.7536 0.2443 0.3329 0.257 Uiso 1 1 calc R . . H8B H 0.7921 0.2994 0.3387 0.257 Uiso 1 1 calc R . . H8C H 0.7743 0.2664 0.3949 0.257 Uiso 1 1 calc R . . C9 C 0.9140(3) 0.27679(18) 0.3882(2) 0.104(2) Uiso 0.40 1 d PD . . C9' C 0.93252(19) 0.27583(16) 0.3521(3) 0.1231(19) Uiso 0.60 1 d PD . . C10 C 0.97896(15) 0.05393(10) 0.37338(10) 0.0813(9) Uani 1 1 d . . . H10A H 1.0242 0.0715 0.3593 0.098 Uiso 1 1 calc R . . C11 C 1.00408(18) 0.01540(13) 0.42279(11) 0.1206(13) Uani 1 1 d . . . H11A H 1.0232 0.0351 0.4553 0.181 Uiso 1 1 calc R . . H11B H 1.0423 -0.0075 0.4081 0.181 Uiso 1 1 calc R . . H11C H 0.9621 -0.0052 0.4354 0.181 Uiso 1 1 calc R . . C12 C 0.94888(19) 0.02109(12) 0.32160(11) 0.1008(11) Uani 1 1 d . . . H12A H 0.9334 0.0442 0.2907 0.151 Uiso 1 1 calc R . . H12B H 0.9071 0.0005 0.3344 0.151 Uiso 1 1 calc R . . H12C H 0.9875 -0.0018 0.3075 0.151 Uiso 1 1 calc R . . C13 C 0.87257(13) 0.24423(10) 0.11271(11) 0.0762(8) Uani 1 1 d . . . C14 C 0.88213(15) 0.22920(12) 0.05259(12) 0.0933(10) Uani 1 1 d . . . C15 C 0.87375(18) 0.26742(13) 0.00886(13) 0.1199(13) Uani 1 1 d . . . H15A H 0.8767 0.2575 -0.0302 0.144 Uiso 1 1 calc R . . C16 C 0.8613(2) 0.31905(14) 0.02244(16) 0.1393(14) Uani 1 1 d . . . H16A H 0.8574 0.3440 -0.0071 0.167 Uiso 1 1 calc R . . C17 C 0.8545(2) 0.33363(13) 0.07963(15) 0.1224(14) Uani 1 1 d . . . H17A H 0.8455 0.3687 0.0887 0.147 Uiso 1 1 calc R . . C18 C 0.86065(17) 0.29735(12) 0.12421(12) 0.1002(11) Uani 1 1 d . . . C19 C 0.89439(17) 0.17228(14) 0.03435(13) 0.1036(11) Uani 1 1 d . . . H19A H 0.9009 0.1512 0.0699 0.124 Uiso 1 1 calc R . . C20 C 0.9665(2) 0.16639(15) -0.00369(15) 0.1351(16) Uani 1 1 d . . . H20A H 1.0089 0.1783 0.0182 0.203 Uiso 1 1 calc R . . H20B H 0.9615 0.1871 -0.0386 0.203 Uiso 1 1 calc R . . H20C H 0.9732 0.1301 -0.0141 0.203 Uiso 1 1 calc R . . C21 C 0.8268(2) 0.15050(16) 0.0007(2) 0.177(2) Uani 1 1 d . . . H21A H 0.7828 0.1537 0.0245 0.265 Uiso 1 1 calc R . . H21B H 0.8352 0.1142 -0.0085 0.265 Uiso 1 1 calc R . . H21C H 0.8201 0.1701 -0.0348 0.265 Uiso 1 1 calc R . . C22 C 0.8522(2) 0.31584(13) 0.18658(17) 0.1277(14) Uani 1 1 d . . . H22A H 0.8617 0.2845 0.2103 0.153 Uiso 1 1 calc R . . C23 C 0.7797(4) 0.3342(3) 0.2058(3) 0.262(4) Uani 1 1 d . . . H23A H 0.7421 0.3096 0.1939 0.393 Uiso 1 1 calc R . . H23B H 0.7696 0.3679 0.1886 0.393 Uiso 1 1 calc R . . H23C H 0.7794 0.3373 0.2477 0.393 Uiso 1 1 calc R . . C24 C 0.9079(3) 0.3558(2) 0.2086(3) 0.212(4) Uani 1 1 d . . . H24A H 0.8971 0.3642 0.2486 0.317 Uiso 1 1 calc R . . H24B H 0.9045 0.3871 0.1852 0.317 Uiso 1 1 calc R . . H24C H 0.9574 0.3416 0.2057 0.317 Uiso 1 1 calc R . . C25 C 0.73983(12) 0.08993(9) 0.22054(9) 0.0655(8) Uani 1 1 d . . . C26 C 0.67159(12) 0.10528(11) 0.25304(11) 0.0716(8) Uani 1 1 d . . . C27 C 0.60666(13) 0.07677(13) 0.24490(14) 0.0963(11) Uani 1 1 d . . . H27A H 0.5656 0.0856 0.2678 0.116 Uiso 1 1 calc R . . C28 C 0.59820(16) 0.03612(14) 0.20519(15) 0.1106(12) Uani 1 1 d . . . H28A H 0.5523 0.0202 0.1986 0.133 Uiso 1 1 calc R . . C29 C 0.66033(15) 0.02103(12) 0.17661(11) 0.0912(10) Uani 1 1 d . . . H29A H 0.6566 -0.0075 0.1514 0.109 Uiso 1 1 calc R . . C30 C 0.72908(12) 0.04482(10) 0.18207(10) 0.0685(7) Uani 1 1 d . . . C31 C 0.67353(19) 0.15243(12) 0.29398(14) 0.0994(12) Uani 1 1 d . . . H31A H 0.7260 0.1616 0.3004 0.119 Uiso 1 1 calc R . . C32 C 0.6343(2) 0.20142(15) 0.26614(16) 0.1292(15) Uani 1 1 d . . . H32A H 0.5815 0.1992 0.2727 0.194 Uiso 1 1 calc R . . H32B H 0.6441 0.2021 0.2248 0.194 Uiso 1 1 calc R . . H32C H 0.6534 0.2329 0.2838 0.194 Uiso 1 1 calc R . . C33 C 0.63852(19) 0.14150(15) 0.35392(15) 0.1260(15) Uani 1 1 d . . . H33A H 0.5923 0.1604 0.3573 0.189 Uiso 1 1 calc R . . H33B H 0.6721 0.1527 0.3842 0.189 Uiso 1 1 calc R . . H33C H 0.6292 0.1045 0.3579 0.189 Uiso 1 1 calc R . . C34 C 0.79548(15) 0.02471(11) 0.14819(10) 0.0800(9) Uani 1 1 d . . . H34A H 0.8323 0.0532 0.1470 0.096 Uiso 1 1 calc R . . C35 C 0.8311(2) -0.02049(15) 0.17876(17) 0.1550(18) Uani 1 1 d . . . H35A H 0.8414 -0.0110 0.2186 0.232 Uiso 1 1 calc R . . H35B H 0.8770 -0.0294 0.1594 0.232 Uiso 1 1 calc R . . H35C H 0.7980 -0.0501 0.1780 0.232 Uiso 1 1 calc R . . C36 C 0.7777(2) 0.0096(2) 0.08359(14) 0.183(2) Uani 1 1 d . . . H36A H 0.7538 0.0386 0.0644 0.275 Uiso 1 1 calc R . . H36B H 0.7451 -0.0204 0.0830 0.275 Uiso 1 1 calc R . . H36C H 0.8232 0.0011 0.0635 0.275 Uiso 1 1 calc R . . C37 C 0.63254(12) 0.15249(8) 0.10449(15) 0.1442(17) Uani 1 1 d D . . H37A H 0.6176 0.1354 0.1406 0.173 Uiso 1 1 calc R . . H37B H 0.6458 0.1256 0.0762 0.173 Uiso 1 1 calc R . . C38 C 0.56998(11) 0.18619(10) 0.08129(18) 0.269(3) Uani 1 1 d D . . H38A H 0.5333 0.1929 0.1116 0.323 Uiso 1 1 calc R . . H38B H 0.5454 0.1691 0.0486 0.323 Uiso 1 1 calc R . . C39 C 0.60660(12) 0.23686(9) 0.06190(15) 0.240(3) Uani 1 1 d D . . H39A H 0.6075 0.2392 0.0195 0.288 Uiso 1 1 calc R . . H39B H 0.5798 0.2669 0.0773 0.288 Uiso 1 1 calc R . . C40 C 0.68499(12) 0.23496(10) 0.08605(15) 0.1668(18) Uani 1 1 d D . . H40A H 0.7211 0.2383 0.0546 0.200 Uiso 1 1 calc R . . H40B H 0.6928 0.2635 0.1135 0.200 Uiso 1 1 calc R . . C41 C 0.70361(18) -0.02408(10) 0.32434(9) 0.1711(19) Uani 1 1 d D . . H41A H 0.7367 -0.0408 0.2964 0.205 Uiso 1 1 calc R . . H41B H 0.6686 -0.0022 0.3030 0.205 Uiso 1 1 calc R . . C42 C 0.66241(15) -0.06487(10) 0.35919(10) 0.222(3) Uani 1 1 d D . . H42A H 0.6714 -0.0996 0.3433 0.266 Uiso 1 1 calc R . . H42B H 0.6091 -0.0581 0.3585 0.266 Uiso 1 1 calc R . . C43 C 0.69235(18) -0.06085(10) 0.42114(9) 0.213(2) Uani 1 1 d D . . H43A H 0.7204 -0.0922 0.4313 0.256 Uiso 1 1 calc R . . H43B H 0.6517 -0.0567 0.4488 0.256 Uiso 1 1 calc R . . C44 C 0.74288(17) -0.01267(10) 0.42183(10) 0.205(2) Uani 1 1 d D . . H44A H 0.7231 0.0138 0.4481 0.246 Uiso 1 1 calc R . . H44B H 0.7926 -0.0221 0.4349 0.246 Uiso 1 1 calc R . . C45 C 0.5187(2) 0.02561(9) 0.0493(2) 0.217(3) Uani 1 1 d D . . C46 C 0.5554(3) -0.02160(12) 0.03924(18) 0.207(4) Uiso 0.50 1 d PD . . C46' C 0.5214(6) -0.02872(11) 0.05141(14) 0.180(4) Uiso 0.50 1 d PD . . C47 C 0.5222(3) -0.05210(16) -0.00381(12) 0.252(3) Uani 1 1 d 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 0.05187(6) 0.06567(7) 0.05310(6) 0.00618(4) -0.00336(4) -0.00166(4) Na1 0.0831(6) 0.1082(7) 0.0760(5) 0.0259(5) -0.0082(5) -0.0127(6) Li1 0.045(2) 0.146(4) 0.094(3) 0.047(3) 0.008(2) 0.003(2) Li2 0.092(3) 0.094(3) 0.089(3) 0.020(2) -0.026(2) -0.010(3) N1 0.0622(11) 0.0712(12) 0.0493(9) -0.0019(8) 0.0029(9) -0.0022(9) N2 0.0580(10) 0.0866(13) 0.0761(12) 0.0166(10) -0.0020(10) 0.0006(11) N3 0.0585(10) 0.0672(12) 0.0643(11) 0.0064(9) -0.0054(9) -0.0063(10) O1 0.0767(10) 0.1289(15) 0.1344(13) 0.0568(12) -0.0390(10) -0.0133(11) O2 0.1621(19) 0.1230(16) 0.0942(12) 0.0322(12) -0.0138(14) -0.0307(15) C1 0.0510(12) 0.0805(16) 0.0511(12) -0.0038(11) -0.0046(10) -0.0036(11) C2 0.0829(16) 0.0834(16) 0.0676(13) -0.0162(13) -0.0053(13) 0.0044(15) C3 0.0885(17) 0.107(2) 0.0732(15) -0.0186(15) 0.0206(14) 0.0018(16) C4 0.0924(18) 0.138(2) 0.0646(14) 0.0059(17) 0.0277(14) -0.0042(19) C5 0.0864(16) 0.110(2) 0.0607(13) 0.0154(14) 0.0208(13) -0.0037(16) C6 0.0648(13) 0.0884(17) 0.0584(12) 0.0000(13) -0.0005(12) -0.0021(12) C7 0.116(2) 0.0874(18) 0.1008(19) -0.0032(16) 0.0207(17) 0.0377(16) C8 0.121(3) 0.117(3) 0.277(5) 0.009(3) -0.066(3) 0.014(2) C10 0.0848(16) 0.0842(17) 0.0749(14) 0.0274(12) 0.0048(13) 0.0148(14) C11 0.120(2) 0.138(3) 0.1042(18) 0.0538(17) -0.002(2) 0.028(2) C12 0.121(2) 0.096(2) 0.0854(17) 0.0038(16) -0.0002(18) 0.0265(18) C13 0.0615(13) 0.0821(16) 0.0851(15) 0.0245(13) -0.0175(12) 0.0005(13) C14 0.0782(15) 0.123(2) 0.0788(15) 0.0287(15) -0.0202(14) -0.0288(16) C15 0.129(2) 0.143(3) 0.0876(17) 0.0427(18) -0.0340(18) -0.018(2) C16 0.152(3) 0.118(2) 0.148(2) 0.0756(19) -0.040(2) -0.021(2) C17 0.149(3) 0.101(2) 0.118(2) 0.0306(19) -0.019(2) 0.007(2) C18 0.109(2) 0.0893(19) 0.1024(18) 0.0351(16) -0.0137(17) 0.0022(17) C19 0.115(2) 0.117(2) 0.0789(18) 0.0181(18) -0.0144(17) -0.0239(19) C20 0.129(3) 0.165(3) 0.111(2) 0.022(2) -0.007(2) 0.004(3) C21 0.110(3) 0.208(4) 0.212(4) -0.074(3) 0.008(3) -0.056(2) C22 0.146(3) 0.0792(19) 0.158(3) 0.031(2) 0.002(2) 0.0340(19) C23 0.201(5) 0.341(8) 0.243(5) -0.051(5) 0.069(4) 0.070(5) C24 0.176(6) 0.238(7) 0.220(6) -0.066(4) 0.000(4) -0.005(4) C25 0.0530(12) 0.0724(15) 0.0711(14) 0.0129(11) -0.0122(11) -0.0043(12) C26 0.0499(12) 0.0907(17) 0.0744(14) 0.0118(14) 0.0001(12) 0.0047(13) C27 0.0464(12) 0.139(3) 0.1036(18) 0.022(2) -0.0025(14) -0.0194(15) C28 0.0882(17) 0.138(3) 0.106(2) -0.011(2) 0.0135(16) -0.0497(17) C29 0.0941(17) 0.097(2) 0.0820(16) 0.0065(15) -0.0149(15) -0.0171(16) C30 0.0526(11) 0.0835(15) 0.0693(13) 0.0025(12) -0.0067(11) -0.0156(12) C31 0.085(2) 0.122(3) 0.0905(18) -0.0171(17) -0.0060(17) 0.0053(17) C32 0.121(3) 0.112(3) 0.155(3) 0.008(2) -0.019(2) 0.021(2) C33 0.105(2) 0.172(3) 0.101(2) -0.018(2) 0.028(2) -0.012(2) C34 0.0811(15) 0.0912(18) 0.0676(13) -0.0128(13) -0.0021(13) -0.0048(15) C35 0.175(3) 0.130(3) 0.159(3) 0.037(3) 0.050(3) 0.037(3) C36 0.108(3) 0.349(6) 0.094(2) -0.037(3) -0.020(2) 0.038(3) C37 0.095(2) 0.182(4) 0.156(3) 0.045(2) -0.057(2) -0.030(2) C38 0.152(3) 0.258(5) 0.397(6) 0.175(4) -0.143(3) -0.052(3) C39 0.131(3) 0.246(5) 0.343(6) 0.122(5) -0.084(4) -0.017(4) C40 0.129(3) 0.141(3) 0.230(4) 0.080(3) -0.043(3) -0.008(3) C41 0.234(4) 0.160(3) 0.119(3) 0.024(3) -0.018(3) -0.082(3) C42 0.258(5) 0.220(5) 0.187(4) 0.038(4) -0.076(4) -0.089(4) C43 0.232(5) 0.217(4) 0.191(4) 0.103(3) -0.054(4) -0.072(4) C44 0.232(4) 0.240(4) 0.144(3) 0.091(3) -0.049(3) -0.114(3) C45 0.226(5) 0.223(6) 0.201(4) -0.026(4) -0.088(4) -0.020(4) C47 0.250(6) 0.267(7) 0.239(5) -0.056(5) -0.073(5) 0.009(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 N2 2.122(2) . ? Yb1 N3 2.1216(19) . ? Yb1 N1 2.2879(18) 3_755 ? Yb1 N1 2.3041(18) . ? Yb1 Li2 2.764(5) . ? Yb1 Li1 2.793(4) . ? Yb1 C1 3.121(2) . ? Yb1 Yb1 3.3917(6) 3_755 ? Yb1 Na1 3.6442(11) . ? Na1 O2 2.295(2) . ? Na1 N3 2.468(2) . ? Na1 C25 2.669(2) . ? Na1 C6 2.775(3) . ? Na1 C1 2.857(2) . ? Na1 C26 2.871(3) . ? Na1 C2 3.128(3) . ? Li1 N2 1.977(4) . ? Li1 N1 2.018(5) . ? Li1 C13 2.266(5) . ? Li1 C1 2.279(5) 3_755 ? Li1 C9' 2.387(6) 3_755 ? Li1 C14 2.628(5) . ? Li1 C9 2.635(7) 3_755 ? Li1 C2 2.667(5) 3_755 ? Li2 O1 1.950(5) . ? Li2 N2 1.999(5) . ? Li2 N3 2.068(5) . ? Li2 C25 2.519(5) . ? Li2 C13 2.774(5) . ? N1 C1 1.339(3) 3_755 ? N1 Yb1 2.2879(18) 3_755 ? N2 C13 1.400(3) . ? N3 C25 1.359(3) . ? O1 C40 1.408(3) . ? O1 C37 1.411(3) . ? O2 C41 1.408(3) . ? O2 C44 1.409(3) . ? C1 N1 1.339(3) 3_755 ? C1 C6 1.422(4) . ? C1 C2 1.466(3) . ? C1 Li1 2.279(5) 3_755 ? C2 C3 1.414(4) . ? C2 C7 1.550(4) . ? C2 Li1 2.667(5) 3_755 ? C3 C4 1.360(4) . ? C4 C5 1.380(4) . ? C5 C6 1.375(3) . ? C6 C10 1.510(4) . ? C7 C9' 1.522(4) . ? C7 C8 1.533(4) . ? C7 C9 1.560(5) . ? C9 C9' 0.891(8) . ? C9 Li1 2.635(7) 3_755 ? C9' Li1 2.387(6) 3_755 ? C10 C12 1.546(4) . ? C10 C11 1.562(4) . ? C13 C18 1.394(4) . ? C13 C14 1.436(4) . ? C14 C15 1.402(4) . ? C14 C19 1.524(5) . ? C15 C16 1.369(5) . ? C16 C17 1.364(5) . ? C17 C18 1.379(4) . ? C18 C22 1.509(5) . ? C19 C21 1.537(5) . ? C19 C20 1.564(5) . ? C22 C23 1.448(7) . ? C22 C24 1.511(7) . ? C25 C30 1.459(3) . ? C25 C26 1.483(3) . ? C26 C27 1.384(4) . ? C26 C31 1.522(4) . ? C27 C28 1.384(5) . ? C28 C29 1.346(4) . ? C29 C30 1.378(4) . ? C30 C34 1.509(3) . ? C31 C33 1.532(5) . ? C31 C32 1.566(5) . ? C34 C35 1.490(5) . ? C34 C36 1.559(4) . ? C37 C38 1.507(3) . ? C38 C39 1.513(3) . ? C39 C40 1.509(3) . ? C41 C42 1.502(3) . ? C42 C43 1.517(3) . ? C43 C44 1.524(4) . ? C45 C46' 1.385(4) . ? C45 C46 1.389(4) . ? C45 C47 1.440(6) 5_655 ? C46 C46' 0.693(10) . ? C46 C47 1.387(5) . ? C46' C47 1.395(4) . ? C47 C45 1.440(6) 5_655 ? 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 Yb1 N3 93.91(7) . . ? N2 Yb1 N1 139.32(7) . 3_755 ? N3 Yb1 N1 111.09(6) . 3_755 ? N2 Yb1 N1 90.32(7) . . ? N3 Yb1 N1 148.14(7) . . ? N1 Yb1 N1 84.77(7) 3_755 . ? N2 Yb1 Li2 46.02(11) . . ? N3 Yb1 Li2 47.89(11) . . ? N1 Yb1 Li2 145.26(11) 3_755 . ? N1 Yb1 Li2 128.21(11) . . ? N2 Yb1 Li1 44.91(10) . . ? N3 Yb1 Li1 130.85(10) . . ? N1 Yb1 Li1 117.93(10) 3_755 . ? N1 Yb1 Li1 45.41(10) . . ? Li2 Yb1 Li1 86.93(13) . . ? N2 Yb1 C1 140.79(7) . . ? N3 Yb1 C1 89.36(6) . . ? N1 Yb1 C1 22.61(6) 3_755 . ? N1 Yb1 C1 106.90(6) . . ? Li2 Yb1 C1 124.47(10) . . ? Li1 Yb1 C1 138.65(10) . . ? N2 Yb1 Yb1 121.48(5) . 3_755 ? N3 Yb1 Yb1 144.58(5) . 3_755 ? N1 Yb1 Yb1 42.57(4) 3_755 3_755 ? N1 Yb1 Yb1 42.20(4) . 3_755 ? Li2 Yb1 Yb1 167.46(10) . 3_755 ? Li1 Yb1 Yb1 81.03(8) . 3_755 ? C1 Yb1 Yb1 64.78(4) . 3_755 ? N2 Yb1 Na1 128.45(5) . . ? N3 Yb1 Na1 40.89(5) . . ? N1 Yb1 Na1 70.27(5) 3_755 . ? N1 Yb1 Na1 140.62(5) . . ? Li2 Yb1 Na1 85.19(10) . . ? Li1 Yb1 Na1 171.73(8) . . ? C1 Yb1 Na1 49.21(4) . . ? Yb1 Yb1 Na1 106.98(2) 3_755 . ? O2 Na1 N3 129.96(7) . . ? O2 Na1 C25 103.53(8) . . ? N3 Na1 C25 30.36(7) . . ? O2 Na1 C6 104.68(8) . . ? N3 Na1 C6 112.90(8) . . ? C25 Na1 C6 142.54(8) . . ? O2 Na1 C1 133.74(8) . . ? N3 Na1 C1 89.35(7) . . ? C25 Na1 C1 119.43(8) . . ? C6 Na1 C1 29.19(7) . . ? O2 Na1 C26 94.20(8) . . ? N3 Na1 C26 55.18(7) . . ? C25 Na1 C26 30.77(7) . . ? C6 Na1 C26 160.53(9) . . ? C1 Na1 C26 131.51(8) . . ? O2 Na1 C2 137.16(7) . . ? N3 Na1 C2 92.88(7) . . ? C25 Na1 C2 117.14(8) . . ? C6 Na1 C2 48.30(8) . . ? C1 Na1 C2 27.90(7) . . ? C26 Na1 C2 113.57(8) . . ? O2 Na1 Yb1 150.73(6) . . ? N3 Na1 Yb1 34.24(5) . . ? C25 Na1 Yb1 64.57(5) . . ? C6 Na1 Yb1 78.87(6) . . ? C1 Na1 Yb1 55.81(5) . . ? C26 Na1 Yb1 87.03(6) . . ? C2 Na1 Yb1 66.55(5) . . ? N2 Li1 N1 103.7(2) . . ? N2 Li1 C13 37.77(11) . . ? N1 Li1 C13 141.4(2) . . ? N2 Li1 C1 132.9(3) . 3_755 ? N1 Li1 C1 35.65(11) . 3_755 ? C13 Li1 C1 163.3(3) . 3_755 ? N2 Li1 C9' 122.4(3) . 3_755 ? N1 Li1 C9' 96.7(2) . 3_755 ? C13 Li1 C9' 104.2(2) . 3_755 ? C1 Li1 C9' 92.34(17) 3_755 3_755 ? N2 Li1 C14 62.64(14) . . ? N1 Li1 C14 151.9(3) . . ? C13 Li1 C14 33.09(10) . . ? C1 Li1 C14 137.0(2) 3_755 . ? C9' Li1 C14 111.4(2) 3_755 . ? N2 Li1 C9 134.3(3) . 3_755 ? N1 Li1 C9 104.81(19) . 3_755 ? C13 Li1 C9 105.6(2) . 3_755 ? C1 Li1 C9 89.01(17) 3_755 3_755 ? C9' Li1 C9 19.64(18) 3_755 3_755 ? C14 Li1 C9 101.6(2) . 3_755 ? N2 Li1 C2 164.5(3) . 3_755 ? N1 Li1 C2 60.82(13) . 3_755 ? C13 Li1 C2 157.7(2) . 3_755 ? C1 Li1 C2 33.33(10) 3_755 3_755 ? C9' Li1 C2 63.36(14) 3_755 3_755 ? C14 Li1 C2 130.94(18) . 3_755 ? C9 Li1 C2 56.17(14) 3_755 3_755 ? N2 Li1 Yb1 49.28(11) . . ? N1 Li1 Yb1 54.39(12) . . ? C13 Li1 Yb1 86.98(14) . . ? C1 Li1 Yb1 86.54(17) 3_755 . ? C9' Li1 Yb1 121.8(2) 3_755 . ? C14 Li1 Yb1 108.01(15) . . ? C9 Li1 Yb1 140.9(2) 3_755 . ? C2 Li1 Yb1 115.21(17) 3_755 . ? O1 Li2 N2 123.7(3) . . ? O1 Li2 N3 136.9(3) . . ? N2 Li2 N3 99.4(2) . . ? O1 Li2 C25 104.3(2) . . ? N2 Li2 C25 131.7(2) . . ? N3 Li2 C25 32.63(10) . . ? O1 Li2 Yb1 173.4(2) . . ? N2 Li2 Yb1 49.81(12) . . ? N3 Li2 Yb1 49.56(11) . . ? C25 Li2 Yb1 82.02(15) . . ? O1 Li2 C13 95.06(19) . . ? N2 Li2 C13 28.68(10) . . ? N3 Li2 C13 128.0(2) . . ? C25 Li2 C13 159.8(2) . . ? Yb1 Li2 C13 78.46(14) . . ? C1 N1 Li1 82.85(18) 3_755 . ? C1 N1 Yb1 116.32(14) 3_755 3_755 ? Li1 N1 Yb1 139.69(17) . 3_755 ? C1 N1 Yb1 146.17(15) 3_755 . ? Li1 N1 Yb1 80.20(13) . . ? Yb1 N1 Yb1 95.23(7) 3_755 . ? C13 N2 Li1 82.37(19) . . ? C13 N2 Li2 108.1(2) . . ? Li1 N2 Li2 148.0(2) . . ? C13 N2 Yb1 167.50(16) . . ? Li1 N2 Yb1 85.81(16) . . ? Li2 N2 Yb1 84.17(16) . . ? C25 N3 Li2 92.23(19) . . ? C25 N3 Yb1 171.43(14) . . ? Li2 N3 Yb1 82.55(15) . . ? C25 N3 Na1 83.03(12) . . ? Li2 N3 Na1 150.21(17) . . ? Yb1 N3 Na1 104.86(7) . . ? C40 O1 C37 112.10(17) . . ? C40 O1 Li2 122.9(2) . . ? C37 O1 Li2 125.0(2) . . ? C41 O2 C44 113.35(19) . . ? C41 O2 Na1 116.80(13) . . ? C44 O2 Na1 129.55(15) . . ? N1 C1 C6 124.3(2) 3_755 . ? N1 C1 C2 120.6(2) 3_755 . ? C6 C1 C2 115.0(2) . . ? N1 C1 Li1 61.49(16) 3_755 3_755 ? C6 C1 Li1 120.1(2) . 3_755 ? C2 C1 Li1 88.04(19) . 3_755 ? N1 C1 Na1 112.54(15) 3_755 . ? C6 C1 Na1 72.21(13) . . ? C2 C1 Na1 86.38(14) . . ? Li1 C1 Na1 167.71(16) 3_755 . ? N1 C1 Yb1 41.07(10) 3_755 . ? C6 C1 Yb1 126.80(16) . . ? C2 C1 Yb1 103.25(14) . . ? Li1 C1 Yb1 95.71(13) 3_755 . ? Na1 C1 Yb1 74.97(6) . . ? C3 C2 C1 119.8(2) . . ? C3 C2 C7 119.1(2) . . ? C1 C2 C7 121.1(2) . . ? C3 C2 Li1 132.0(2) . 3_755 ? C1 C2 Li1 58.63(17) . 3_755 ? C7 C2 Li1 80.57(18) . 3_755 ? C3 C2 Na1 84.22(17) . . ? C1 C2 Na1 65.72(13) . . ? C7 C2 Na1 123.14(15) . . ? Li1 C2 Na1 123.37(14) 3_755 . ? C4 C3 C2 121.8(3) . . ? C3 C4 C5 119.4(2) . . ? C6 C5 C4 121.7(3) . . ? C5 C6 C1 122.3(2) . . ? C5 C6 C10 119.7(2) . . ? C1 C6 C10 117.9(2) . . ? C5 C6 Na1 82.95(15) . . ? C1 C6 Na1 78.59(13) . . ? C10 C6 Na1 106.56(15) . . ? C9' C7 C8 115.3(3) . . ? C9' C7 C2 120.4(3) . . ? C8 C7 C2 114.6(2) . . ? C9' C7 C9 33.6(3) . . ? C8 C7 C9 100.7(3) . . ? C2 C7 C9 106.8(3) . . ? C9' C9 C7 70.9(4) . . ? C9' C9 Li1 64.3(4) . 3_755 ? C7 C9 Li1 81.5(2) . 3_755 ? C9 C9' C7 75.5(4) . . ? C9 C9' Li1 96.1(5) . 3_755 ? C7 C9' Li1 91.2(2) . 3_755 ? C6 C10 C12 113.1(2) . . ? C6 C10 C11 115.2(2) . . ? C12 C10 C11 108.3(2) . . ? C18 C13 N2 122.7(2) . . ? C18 C13 C14 117.2(2) . . ? N2 C13 C14 120.1(2) . . ? C18 C13 Li1 122.0(2) . . ? N2 C13 Li1 59.86(16) . . ? C14 C13 Li1 87.43(19) . . ? C18 C13 Li2 119.7(2) . . ? N2 C13 Li2 43.25(14) . . ? C14 C13 Li2 106.5(2) . . ? Li1 C13 Li2 98.15(18) . . ? C15 C14 C13 118.9(3) . . ? C15 C14 C19 118.7(3) . . ? C13 C14 C19 122.1(2) . . ? C15 C14 Li1 136.5(2) . . ? C13 C14 Li1 59.48(16) . . ? C19 C14 Li1 82.0(2) . . ? C16 C15 C14 121.5(3) . . ? C17 C16 C15 119.5(3) . . ? C16 C17 C18 121.2(3) . . ? C17 C18 C13 121.5(3) . . ? C17 C18 C22 118.7(3) . . ? C13 C18 C22 119.7(3) . . ? C14 C19 C21 111.5(3) . . ? C14 C19 C20 111.2(3) . . ? C21 C19 C20 109.7(3) . . ? C23 C22 C24 105.9(4) . . ? C23 C22 C18 118.5(4) . . ? C24 C22 C18 117.3(3) . . ? N3 C25 C30 123.4(2) . . ? N3 C25 C26 123.0(2) . . ? C30 C25 C26 113.6(2) . . ? N3 C25 Li2 55.14(15) . . ? C30 C25 Li2 110.84(18) . . ? C26 C25 Li2 106.56(19) . . ? N3 C25 Na1 66.62(11) . . ? C30 C25 Na1 123.70(16) . . ? C26 C25 Na1 82.14(13) . . ? Li2 C25 Na1 115.37(14) . . ? C27 C26 C25 119.2(2) . . ? C27 C26 C31 121.0(2) . . ? C25 C26 C31 119.8(2) . . ? C27 C26 Na1 128.9(2) . . ? C25 C26 Na1 67.09(12) . . ? C31 C26 Na1 76.61(16) . . ? C26 C27 C28 124.9(3) . . ? C29 C28 C27 116.1(3) . . ? C28 C29 C30 124.7(3) . . ? C29 C30 C25 121.2(2) . . ? C29 C30 C34 120.6(2) . . ? C25 C30 C34 118.2(2) . . ? C26 C31 C33 113.4(3) . . ? C26 C31 C32 111.6(3) . . ? C33 C31 C32 108.9(3) . . ? C35 C34 C30 111.1(2) . . ? C35 C34 C36 109.9(3) . . ? C30 C34 C36 114.1(2) . . ? O1 C37 C38 106.66(17) . . ? C37 C38 C39 105.40(17) . . ? C40 C39 C38 105.6(2) . . ? O1 C40 C39 107.42(18) . . ? O2 C41 C42 107.50(18) . . ? C41 C42 C43 105.9(2) . . ? C42 C43 C44 105.90(18) . . ? O2 C44 C43 106.64(19) . . ? C46' C45 C46 28.9(4) . . ? C46' C45 C47 120.7(4) . 5_655 ? C46 C45 C47 121.7(4) . 5_655 ? C46' C46 C47 76.3(5) . . ? C46' C46 C45 75.2(5) . . ? C47 C46 C45 113.5(4) . . ? C46 C46' C45 75.9(4) . . ? C46 C46' C47 74.9(5) . . ? C45 C46' C47 113.3(3) . . ? C46 C47 C46' 28.8(4) . . ? C46 C47 C45 117.9(3) . 5_655 ? C46' C47 C45 116.7(4) . 5_655 ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 1.302 _refine_diff_density_min -1.205 _refine_diff_density_rms 0.133 #===END