# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_complex1 _database_code_depnum_ccdc_archive 'CCDC 909529' #TrackingRef '909529.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H80 Li4 N12 O' _chemical_formula_sum 'C52 H80 Li4 N12 O' _chemical_formula_weight 917.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.100(2) _cell_length_b 12.745(3) _cell_length_c 21.549(6) _cell_angle_alpha 86.141(18) _cell_angle_beta 85.522(18) _cell_angle_gamma 64.633(12) _cell_volume 2744.4(11) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9372 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.6 _exptl_crystal_description chip _exptl_crystal_colour colorless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.110 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.789 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23279 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_unetI/netI 0.1119 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10188 _reflns_number_gt 4886 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Their N3-H3,N6-H6,N9-H9 and N12-H12 distances were constrained. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1163P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10188 _refine_ls_number_parameters 651 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1753 _refine_ls_R_factor_gt 0.0854 _refine_ls_wR_factor_ref 0.2497 _refine_ls_wR_factor_gt 0.1961 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.0132(3) 0.4625(3) 0.16422(13) 0.0638(8) Uani 1 1 d . . . N1 N 0.0952(3) 0.2776(3) 0.35189(13) 0.0451(8) Uani 1 1 d . . . N2 N 0.0376(3) 0.1233(3) 0.36846(13) 0.0467(8) Uani 1 1 d . . . N3 N 0.0212(4) 0.2362(3) 0.45368(15) 0.0616(10) Uani 1 1 d D . . H3 H 0.001(5) 0.184(3) 0.4741(19) 0.092 Uiso 1 1 d D . . N4 N 0.2928(3) 0.3417(3) 0.29318(14) 0.0446(8) Uani 1 1 d . . . N5 N 0.5118(3) 0.2357(3) 0.26157(13) 0.0436(8) Uani 1 1 d . . . N6 N 0.4609(3) 0.3909(3) 0.32901(16) 0.0563(9) Uani 1 1 d D . . H6 H 0.5453(16) 0.375(4) 0.323(2) 0.084 Uiso 1 1 d D . . N7 N 0.3071(3) 0.0854(2) 0.23045(12) 0.0397(7) Uani 1 1 d . . . N8 N 0.3877(3) 0.0358(2) 0.32763(12) 0.0418(7) Uani 1 1 d . . . N9 N 0.4540(4) -0.1134(3) 0.25574(15) 0.0591(10) Uani 1 1 d D . . H9 H 0.496(4) -0.160(3) 0.2862(15) 0.089 Uiso 1 1 d D . . N10 N 0.3193(3) 0.2432(3) 0.13355(13) 0.0400(7) Uani 1 1 d . . . N11 N 0.3142(3) 0.4240(3) 0.10845(14) 0.0467(8) Uani 1 1 d . . . N12 N 0.4732(4) 0.2626(3) 0.05467(16) 0.0584(9) Uani 1 1 d D . . H12 H 0.502(5) 0.312(3) 0.0367(19) 0.088 Uiso 1 1 d D . . C1 C 0.0478(4) 0.2105(3) 0.39167(16) 0.0464(9) Uani 1 1 d . . . C2 C 0.4251(4) 0.3231(3) 0.29301(16) 0.0432(9) Uani 1 1 d . . . C3 C 0.0089(3) 0.3955(3) 0.34214(16) 0.0443(9) Uani 1 1 d . . . C4 C -0.1268(4) 0.4353(4) 0.35974(18) 0.0608(11) Uani 1 1 d . . . H4 H -0.1581 0.3820 0.3780 0.073 Uiso 1 1 calc R . . C5 C -0.2184(4) 0.5520(5) 0.3512(2) 0.0728(14) Uani 1 1 d . . . H5 H -0.3086 0.5756 0.3645 0.087 Uiso 1 1 calc R . . C6 C -0.1769(4) 0.6307(4) 0.3238(2) 0.0643(12) Uani 1 1 d . . . H6A H -0.2389 0.7084 0.3178 0.077 Uiso 1 1 calc R . . C7 C -0.0427(4) 0.5973(3) 0.30443(17) 0.0513(10) Uani 1 1 d . . . C8 C -0.0063(5) 0.6846(4) 0.2762(2) 0.0692(13) Uani 1 1 d . . . H8 H -0.0714 0.7616 0.2718 0.083 Uiso 1 1 calc R . . C9 C 0.1208(6) 0.6574(4) 0.2559(2) 0.0778(14) Uani 1 1 d . . . H9A H 0.1448 0.7157 0.2383 0.093 Uiso 1 1 calc R . . C10 C 0.2178(4) 0.5423(3) 0.26085(19) 0.0561(11) Uani 1 1 d . . . H10 H 0.3044 0.5244 0.2434 0.067 Uiso 1 1 calc R . . C11 C 0.1914(4) 0.4536(3) 0.29037(16) 0.0425(9) Uani 1 1 d . . . C12 C 0.0550(3) 0.4782(3) 0.31232(15) 0.0373(8) Uani 1 1 d . . . C13 C 0.0053(4) 0.0411(3) 0.40920(17) 0.0518(10) Uani 1 1 d . . . H13 H 0.0519 0.0280 0.4483 0.062 Uiso 1 1 calc R . . C14 C -0.1442(4) 0.0867(5) 0.4253(2) 0.0742(14) Uani 1 1 d . . . H14A H -0.1758 0.1608 0.4449 0.111 Uiso 1 1 calc R . . H14B H -0.1613 0.0316 0.4536 0.111 Uiso 1 1 calc R . . H14C H -0.1908 0.0967 0.3875 0.111 Uiso 1 1 calc R . . C15 C 0.0558(5) -0.0731(4) 0.3769(2) 0.0773(14) Uani 1 1 d . . . H15A H 0.0120 -0.0611 0.3381 0.116 Uiso 1 1 calc R . . H15B H 0.0364 -0.1289 0.4037 0.116 Uiso 1 1 calc R . . H15C H 0.1515 -0.1025 0.3682 0.116 Uiso 1 1 calc R . . C16 C 0.0573(4) 0.3157(3) 0.48593(18) 0.0553(11) Uani 1 1 d . . . H16 H 0.0725 0.3702 0.4549 0.066 Uiso 1 1 calc R . . C17 C -0.0568(5) 0.3844(4) 0.5315(2) 0.0813(15) Uani 1 1 d . . . H17A H -0.1372 0.4272 0.5091 0.122 Uiso 1 1 calc R . . H17B H -0.0343 0.4384 0.5522 0.122 Uiso 1 1 calc R . . H17C H -0.0718 0.3315 0.5622 0.122 Uiso 1 1 calc R . . C18 C 0.1822(5) 0.2493(5) 0.5202(3) 0.105(2) Uani 1 1 d . . . H18A H 0.1694 0.1930 0.5493 0.157 Uiso 1 1 calc R . . H18B H 0.2021 0.3027 0.5428 0.157 Uiso 1 1 calc R . . H18C H 0.2559 0.2092 0.4906 0.157 Uiso 1 1 calc R . . C19 C 0.6548(4) 0.1916(3) 0.27140(18) 0.0505(10) Uani 1 1 d . . . H19 H 0.6652 0.2009 0.3156 0.061 Uiso 1 1 calc R . . C20 C 0.7205(5) 0.2569(4) 0.2311(2) 0.0756(14) Uani 1 1 d . . . H20A H 0.7143 0.2461 0.1875 0.113 Uiso 1 1 calc R . . H20B H 0.8137 0.2273 0.2404 0.113 Uiso 1 1 calc R . . H20C H 0.6755 0.3390 0.2395 0.113 Uiso 1 1 calc R . . C21 C 0.7222(4) 0.0629(4) 0.2584(2) 0.0640(12) Uani 1 1 d . . . H21A H 0.6763 0.0231 0.2830 0.096 Uiso 1 1 calc R . . H21B H 0.8146 0.0310 0.2694 0.096 Uiso 1 1 calc R . . H21C H 0.7187 0.0526 0.2145 0.096 Uiso 1 1 calc R . . C22 C 0.3903(4) 0.4469(4) 0.38617(19) 0.0597(12) Uani 1 1 d . . . H22 H 0.2949 0.4635 0.3844 0.072 Uiso 1 1 calc R . . C23 C 0.4004(7) 0.5617(5) 0.3899(3) 0.115(2) Uani 1 1 d . . . H23A H 0.4933 0.5470 0.3918 0.173 Uiso 1 1 calc R . . H23B H 0.3503 0.6008 0.4269 0.173 Uiso 1 1 calc R . . H23C H 0.3639 0.6104 0.3533 0.173 Uiso 1 1 calc R . . C24 C 0.4443(7) 0.3693(5) 0.4432(2) 0.122(2) Uani 1 1 d . . . H24A H 0.4325 0.2985 0.4409 0.183 Uiso 1 1 calc R . . H24B H 0.3965 0.4095 0.4803 0.183 Uiso 1 1 calc R . . H24C H 0.5386 0.3500 0.4450 0.183 Uiso 1 1 calc R . . C25 C 0.3830(4) 0.0002(3) 0.27245(16) 0.0422(9) Uani 1 1 d . . . C26 C 0.3691(4) 0.3137(3) 0.09787(15) 0.0412(9) Uani 1 1 d . . . C27 C 0.2273(3) 0.0614(3) 0.19126(15) 0.0359(8) Uani 1 1 d . . . C28 C 0.1713(4) -0.0135(3) 0.21249(18) 0.0493(10) Uani 1 1 d . . . H28 H 0.1924 -0.0500 0.2521 0.059 Uiso 1 1 calc R . . C29 C 0.0841(4) -0.0381(3) 0.17793(19) 0.0542(10) Uani 1 1 d . . . H29 H 0.0480 -0.0893 0.1944 0.065 Uiso 1 1 calc R . . C30 C 0.0537(4) 0.0126(3) 0.12131(19) 0.0507(10) Uani 1 1 d . . . H30 H -0.0031 -0.0042 0.0977 0.061 Uiso 1 1 calc R . . C31 C 0.1062(3) 0.0914(3) 0.09649(16) 0.0440(9) Uani 1 1 d . . . C32 C 0.0712(4) 0.1407(3) 0.03609(18) 0.0506(10) Uani 1 1 d . . . H32 H 0.0126 0.1230 0.0143 0.061 Uiso 1 1 calc R . . C33 C 0.1225(4) 0.2138(4) 0.00967(18) 0.0578(11) Uani 1 1 d . . . H33 H 0.1017 0.2432 -0.0312 0.069 Uiso 1 1 calc R . . C34 C 0.2052(4) 0.2463(3) 0.04147(16) 0.0488(10) Uani 1 1 d . . . H34 H 0.2366 0.2986 0.0218 0.059 Uiso 1 1 calc R . . C35 C 0.2429(3) 0.2028(3) 0.10235(15) 0.0389(8) Uani 1 1 d . . . C36 C 0.1941(3) 0.1202(3) 0.13075(15) 0.0358(8) Uani 1 1 d . . . C37 C 0.4837(4) -0.0411(3) 0.37136(16) 0.0488(10) Uani 1 1 d . . . H37 H 0.5655 -0.0925 0.3475 0.059 Uiso 1 1 calc R . . C38 C 0.4302(5) -0.1165(4) 0.4115(2) 0.0763(14) Uani 1 1 d . . . H38A H 0.3504 -0.0672 0.4354 0.114 Uiso 1 1 calc R . . H38B H 0.4974 -0.1663 0.4396 0.114 Uiso 1 1 calc R . . H38C H 0.4088 -0.1640 0.3850 0.114 Uiso 1 1 calc R . . C39 C 0.5190(4) 0.0340(4) 0.41148(18) 0.0614(12) Uani 1 1 d . . . H39A H 0.5484 0.0840 0.3850 0.092 Uiso 1 1 calc R . . H39B H 0.5900 -0.0153 0.4380 0.092 Uiso 1 1 calc R . . H39C H 0.4410 0.0812 0.4371 0.092 Uiso 1 1 calc R . . C40 C 0.5016(4) -0.1543(3) 0.19213(19) 0.0617(12) Uani 1 1 d . . . H40 H 0.4317 -0.1058 0.1634 0.074 Uiso 1 1 calc R . . C41 C 0.5165(7) -0.2773(5) 0.1911(3) 0.123(2) Uani 1 1 d . . . H41A H 0.5827 -0.3260 0.2200 0.184 Uiso 1 1 calc R . . H41B H 0.5451 -0.3058 0.1494 0.184 Uiso 1 1 calc R . . H41C H 0.4315 -0.2793 0.2032 0.184 Uiso 1 1 calc R . . C42 C 0.6273(6) -0.1425(5) 0.1715(2) 0.0946(17) Uani 1 1 d . . . H42A H 0.6096 -0.0610 0.1691 0.142 Uiso 1 1 calc R . . H42B H 0.6589 -0.1753 0.1309 0.142 Uiso 1 1 calc R . . H42C H 0.6948 -0.1836 0.2013 0.142 Uiso 1 1 calc R . . C43 C 0.3668(4) 0.5017(3) 0.07553(19) 0.0547(10) Uani 1 1 d . . . H43 H 0.3922 0.4774 0.0320 0.066 Uiso 1 1 calc R . . C44 C 0.2591(5) 0.6246(4) 0.0748(3) 0.1008(19) Uani 1 1 d . . . H44A H 0.1828 0.6277 0.0543 0.151 Uiso 1 1 calc R . . H44B H 0.2933 0.6757 0.0523 0.151 Uiso 1 1 calc R . . H44C H 0.2321 0.6495 0.1172 0.151 Uiso 1 1 calc R . . C45 C 0.4912(5) 0.4923(5) 0.1058(2) 0.0808(15) Uani 1 1 d . . . H45A H 0.4675 0.5178 0.1483 0.121 Uiso 1 1 calc R . . H45B H 0.5275 0.5408 0.0824 0.121 Uiso 1 1 calc R . . H45C H 0.5575 0.4121 0.1061 0.121 Uiso 1 1 calc R . . C46 C 0.5524(4) 0.1382(4) 0.04559(18) 0.0558(11) Uani 1 1 d . . . H46 H 0.5074 0.0946 0.0693 0.067 Uiso 1 1 calc R . . C47 C 0.5642(5) 0.1119(4) -0.0223(2) 0.0788(15) Uani 1 1 d . . . H47A H 0.4761 0.1322 -0.0368 0.118 Uiso 1 1 calc R . . H47B H 0.6194 0.0297 -0.0276 0.118 Uiso 1 1 calc R . . H47C H 0.6049 0.1567 -0.0462 0.118 Uiso 1 1 calc R . . C48 C 0.6907(5) 0.0995(5) 0.0695(2) 0.0870(16) Uani 1 1 d . . . H48A H 0.7374 0.1388 0.0450 0.130 Uiso 1 1 calc R . . H48B H 0.7402 0.0162 0.0658 0.130 Uiso 1 1 calc R . . H48C H 0.6828 0.1190 0.1128 0.130 Uiso 1 1 calc R . . C49 C -0.0727(5) 0.4069(4) 0.1819(2) 0.0705(13) Uani 1 1 d . . . H49A H -0.1306 0.4432 0.2183 0.085 Uiso 1 1 calc R . . H49B H -0.0199 0.3243 0.1922 0.085 Uiso 1 1 calc R . . C50 C -0.1540(5) 0.4204(5) 0.1278(2) 0.0810(15) Uani 1 1 d . . . H50A H -0.2479 0.4432 0.1413 0.097 Uiso 1 1 calc R . . H50B H -0.1209 0.3478 0.1057 0.097 Uiso 1 1 calc R . . C51 C -0.1382(5) 0.5141(5) 0.0872(2) 0.0861(16) Uani 1 1 d . . . H51A H -0.1018 0.4854 0.0456 0.103 Uiso 1 1 calc R . . H51B H -0.2249 0.5809 0.0829 0.103 Uiso 1 1 calc R . . C52 C -0.0478(6) 0.5477(5) 0.1164(3) 0.103(2) Uani 1 1 d . . . H52A H 0.0203 0.5514 0.0857 0.124 Uiso 1 1 calc R . . H52B H -0.0969 0.6244 0.1342 0.124 Uiso 1 1 calc R . . Li1 Li 0.1278(8) 0.1429(7) 0.2893(3) 0.067(2) Uani 1 1 d . . . Li2 Li 0.2863(7) 0.2066(6) 0.3347(3) 0.0564(17) Uani 1 1 d . . . Li3 Li 0.3906(6) 0.1934(5) 0.2154(3) 0.0472(15) Uani 1 1 d . . . Li4 Li 0.1962(7) 0.4115(7) 0.1783(3) 0.0616(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0515(17) 0.077(2) 0.0672(18) 0.0074(16) -0.0031(14) -0.0330(16) N1 0.0450(18) 0.0413(19) 0.0478(18) 0.0003(14) 0.0056(14) -0.0188(15) N2 0.053(2) 0.050(2) 0.0425(17) 0.0037(15) 0.0001(15) -0.0285(16) N3 0.088(3) 0.069(3) 0.0438(19) -0.0045(17) 0.0080(18) -0.050(2) N4 0.0349(17) 0.0422(19) 0.0580(19) -0.0070(14) 0.0018(14) -0.0176(14) N5 0.0329(16) 0.0499(19) 0.0427(16) -0.0042(14) -0.0009(13) -0.0123(14) N6 0.047(2) 0.063(2) 0.065(2) -0.0209(18) 0.0076(18) -0.0288(18) N7 0.0492(18) 0.0296(16) 0.0368(15) 0.0067(12) -0.0093(14) -0.0134(14) N8 0.0444(17) 0.0405(17) 0.0355(16) 0.0030(13) -0.0061(13) -0.0133(14) N9 0.073(2) 0.0366(19) 0.0462(19) -0.0046(15) -0.0193(17) 0.0004(17) N10 0.0393(17) 0.0489(19) 0.0377(16) 0.0045(14) -0.0028(13) -0.0250(15) N11 0.0491(19) 0.049(2) 0.0467(17) 0.0020(15) 0.0015(15) -0.0266(16) N12 0.065(2) 0.057(2) 0.056(2) -0.0031(17) 0.0177(18) -0.0320(19) C1 0.044(2) 0.052(2) 0.040(2) 0.0037(18) 0.0025(17) -0.0198(19) C2 0.045(2) 0.045(2) 0.045(2) 0.0003(17) -0.0049(17) -0.0235(18) C3 0.035(2) 0.053(2) 0.0371(18) -0.0030(17) -0.0015(16) -0.0113(18) C4 0.044(2) 0.076(3) 0.053(2) 0.005(2) 0.0027(19) -0.018(2) C5 0.039(2) 0.086(4) 0.069(3) 0.003(3) 0.003(2) -0.004(3) C6 0.051(3) 0.051(3) 0.065(3) 0.003(2) -0.010(2) 0.003(2) C7 0.054(3) 0.042(2) 0.045(2) 0.0037(18) -0.0066(19) -0.0084(19) C8 0.075(3) 0.038(2) 0.081(3) 0.011(2) -0.023(3) -0.010(2) C9 0.088(4) 0.051(3) 0.099(4) 0.021(3) -0.025(3) -0.033(3) C10 0.059(3) 0.047(2) 0.065(3) 0.010(2) -0.008(2) -0.027(2) C11 0.054(2) 0.037(2) 0.0394(19) 0.0059(16) -0.0097(17) -0.0220(19) C12 0.040(2) 0.036(2) 0.0308(17) 0.0020(15) -0.0043(15) -0.0119(16) C13 0.064(3) 0.057(3) 0.045(2) 0.0125(19) -0.0098(19) -0.037(2) C14 0.065(3) 0.109(4) 0.059(3) 0.023(3) -0.010(2) -0.049(3) C15 0.113(4) 0.070(3) 0.066(3) 0.004(2) -0.003(3) -0.058(3) C16 0.070(3) 0.054(3) 0.047(2) -0.0071(19) 0.006(2) -0.031(2) C17 0.092(4) 0.064(3) 0.073(3) -0.020(2) 0.012(3) -0.020(3) C18 0.078(4) 0.114(5) 0.115(5) -0.024(4) -0.020(3) -0.029(3) C19 0.044(2) 0.059(3) 0.044(2) -0.0001(18) -0.0055(18) -0.017(2) C20 0.059(3) 0.091(4) 0.085(3) -0.005(3) 0.006(3) -0.042(3) C21 0.048(2) 0.061(3) 0.065(3) -0.007(2) 0.002(2) -0.007(2) C22 0.055(3) 0.067(3) 0.061(3) -0.020(2) 0.000(2) -0.027(2) C23 0.132(5) 0.117(5) 0.132(5) -0.059(4) 0.033(4) -0.085(4) C24 0.146(6) 0.105(5) 0.063(3) -0.014(3) -0.020(4) 0.000(4) C25 0.048(2) 0.033(2) 0.043(2) 0.0041(16) -0.0064(17) -0.0146(17) C26 0.044(2) 0.046(2) 0.0342(18) 0.0014(16) -0.0056(16) -0.0190(18) C27 0.0387(19) 0.0323(19) 0.0377(18) -0.0003(15) -0.0007(15) -0.0163(16) C28 0.059(2) 0.040(2) 0.047(2) 0.0117(17) -0.0065(19) -0.022(2) C29 0.056(3) 0.048(2) 0.062(3) 0.004(2) -0.008(2) -0.026(2) C30 0.045(2) 0.053(2) 0.060(3) 0.003(2) -0.0100(19) -0.026(2) C31 0.036(2) 0.046(2) 0.045(2) -0.0007(17) -0.0064(17) -0.0131(17) C32 0.046(2) 0.054(2) 0.052(2) 0.0016(19) -0.0155(19) -0.021(2) C33 0.058(3) 0.077(3) 0.041(2) 0.007(2) -0.0189(19) -0.030(2) C34 0.055(2) 0.056(2) 0.0369(19) 0.0137(17) -0.0076(18) -0.027(2) C35 0.0344(19) 0.043(2) 0.0367(18) 0.0046(16) -0.0018(15) -0.0155(17) C36 0.0312(18) 0.037(2) 0.0353(17) -0.0017(15) -0.0021(15) -0.0112(15) C37 0.052(2) 0.041(2) 0.0389(19) 0.0012(17) -0.0086(18) -0.0050(18) C38 0.097(4) 0.072(3) 0.059(3) 0.027(2) -0.021(3) -0.036(3) C39 0.067(3) 0.066(3) 0.046(2) 0.002(2) -0.017(2) -0.021(2) C40 0.061(3) 0.050(3) 0.056(2) -0.019(2) -0.013(2) -0.002(2) C41 0.145(6) 0.094(5) 0.138(5) -0.072(4) 0.033(5) -0.056(4) C42 0.100(4) 0.119(5) 0.068(3) -0.019(3) 0.000(3) -0.048(4) C43 0.064(3) 0.058(3) 0.052(2) 0.0063(19) 0.002(2) -0.038(2) C44 0.096(4) 0.047(3) 0.153(5) 0.023(3) 0.013(4) -0.032(3) C45 0.092(4) 0.103(4) 0.077(3) 0.002(3) -0.006(3) -0.070(3) C46 0.055(3) 0.063(3) 0.051(2) -0.011(2) 0.008(2) -0.027(2) C47 0.077(3) 0.090(4) 0.064(3) -0.024(3) 0.006(2) -0.029(3) C48 0.081(4) 0.088(4) 0.077(3) -0.015(3) -0.018(3) -0.018(3) C49 0.059(3) 0.089(4) 0.071(3) 0.014(3) -0.004(2) -0.040(3) C50 0.082(3) 0.103(4) 0.073(3) 0.023(3) -0.026(3) -0.053(3) C51 0.075(3) 0.094(4) 0.079(3) 0.037(3) -0.018(3) -0.030(3) C52 0.076(4) 0.088(4) 0.149(5) 0.052(4) -0.029(4) -0.042(3) Li1 0.083(5) 0.071(5) 0.052(4) -0.013(4) 0.017(4) -0.040(4) Li2 0.050(4) 0.048(4) 0.058(4) 0.002(3) 0.010(3) -0.011(3) Li3 0.057(4) 0.042(4) 0.047(3) 0.013(3) -0.013(3) -0.025(3) Li4 0.055(4) 0.075(5) 0.060(4) -0.010(4) 0.006(3) -0.033(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C52 1.423(6) . ? O1 C49 1.429(5) . ? O1 Li4 1.892(7) . ? N1 C1 1.400(5) . ? N1 C3 1.406(4) . ? N1 Li2 1.932(7) . ? N1 Li1 2.145(7) . ? N2 C1 1.300(5) . ? N2 C13 1.465(5) . ? N2 Li1 1.966(8) . ? N3 C1 1.376(5) . ? N3 C16 1.467(5) . ? N3 H3 0.873(10) . ? N4 C2 1.383(4) . ? N4 C11 1.388(4) . ? N4 Li2 1.914(8) . ? N4 Li3 2.438(7) . ? N4 Li4 2.714(8) . ? N5 C2 1.307(4) . ? N5 C19 1.467(4) . ? N5 Li3 1.998(6) . ? N6 C2 1.393(4) . ? N6 C22 1.459(5) . ? N6 H6 0.871(10) . ? N7 C25 1.382(4) . ? N7 C27 1.405(4) . ? N7 Li3 1.960(7) . ? N7 Li1 2.142(8) . ? N8 C25 1.314(4) . ? N8 C37 1.457(4) . ? N8 Li2 1.986(7) . ? N9 C25 1.377(5) . ? N9 C40 1.475(5) . ? N9 H9 0.872(10) . ? N10 C35 1.394(4) . ? N10 C26 1.404(5) . ? N10 Li3 1.944(6) . ? N10 Li4 2.228(8) . ? N11 C26 1.299(4) . ? N11 C43 1.470(5) . ? N11 Li4 1.962(8) . ? N12 C26 1.376(5) . ? N12 C46 1.465(5) . ? N12 H12 0.873(10) . ? C1 Li1 2.386(7) . ? C2 Li3 2.587(7) . ? C2 Li2 2.637(8) . ? C3 C4 1.397(5) . ? C3 C12 1.451(5) . ? C4 C5 1.406(6) . ? C4 H4 0.9400 . ? C5 C6 1.357(6) . ? C5 H5 0.9400 . ? C6 C7 1.399(6) . ? C6 H6A 0.9400 . ? C7 C8 1.424(6) . ? C7 C12 1.447(5) . ? C8 C9 1.344(7) . ? C8 H8 0.9400 . ? C9 C10 1.403(6) . ? C9 H9A 0.9400 . ? C10 C11 1.388(5) . ? C10 H10 0.9400 . ? C11 C12 1.454(5) . ? C11 Li4 2.499(7) . ? C13 C15 1.515(6) . ? C13 C14 1.524(6) . ? C13 H13 0.9900 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C18 1.502(6) . ? C16 C17 1.518(6) . ? C16 H16 0.9900 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C20 1.518(6) . ? C19 C21 1.518(5) . ? C19 H19 0.9900 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 C24 1.514(7) . ? C22 C23 1.522(6) . ? C22 H22 0.9900 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 Li1 2.642(9) . ? C25 Li3 2.708(7) . ? C25 Li2 2.775(7) . ? C26 Li4 2.443(8) . ? C27 C28 1.384(5) . ? C27 C36 1.450(5) . ? C27 Li1 2.390(7) . ? C28 C29 1.412(5) . ? C28 H28 0.9400 . ? C29 C30 1.339(5) . ? C29 H29 0.9400 . ? C30 C31 1.420(5) . ? C30 H30 0.9400 . ? C31 C32 1.414(5) . ? C31 C36 1.445(5) . ? C32 C33 1.359(6) . ? C32 H32 0.9400 . ? C33 C34 1.395(5) . ? C33 H33 0.9400 . ? C34 C35 1.412(5) . ? C34 H34 0.9400 . ? C35 C36 1.458(5) . ? C37 C39 1.517(5) . ? C37 C38 1.523(6) . ? C37 H37 0.9900 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? C40 C42 1.497(7) . ? C40 C41 1.505(7) . ? C40 H40 0.9900 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? C43 C44 1.509(6) . ? C43 C45 1.528(6) . ? C43 H43 0.9900 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 H45C 0.9700 . ? C46 C47 1.507(5) . ? C46 C48 1.518(6) . ? C46 H46 0.9900 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C49 C50 1.484(6) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.495(7) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.445(7) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? Li1 Li2 2.511(10) . ? Li1 Li3 3.492(10) . ? Li2 Li3 2.720(9) . ? Li3 Li4 2.803(10) . ? 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 C52 O1 C49 107.7(3) . . ? C52 O1 Li4 120.7(4) . . ? C49 O1 Li4 129.1(4) . . ? C1 N1 C3 117.4(3) . . ? C1 N1 Li2 114.2(3) . . ? C3 N1 Li2 126.4(3) . . ? C1 N1 Li1 81.7(3) . . ? C3 N1 Li1 124.8(3) . . ? Li2 N1 Li1 75.8(3) . . ? C1 N2 C13 120.4(3) . . ? C1 N2 Li1 91.5(3) . . ? C13 N2 Li1 144.9(3) . . ? C1 N3 C16 126.6(3) . . ? C1 N3 H3 110(3) . . ? C16 N3 H3 122(3) . . ? C2 N4 C11 120.9(3) . . ? C2 N4 Li2 105.1(3) . . ? C11 N4 Li2 127.7(3) . . ? C2 N4 Li3 80.0(2) . . ? C11 N4 Li3 131.7(3) . . ? Li2 N4 Li3 76.3(3) . . ? C2 N4 Li4 111.1(3) . . ? C11 N4 Li4 66.1(2) . . ? Li2 N4 Li4 120.4(3) . . ? Li3 N4 Li4 65.7(2) . . ? C2 N5 C19 120.1(3) . . ? C2 N5 Li3 100.9(3) . . ? C19 N5 Li3 138.7(3) . . ? C2 N6 C22 125.9(3) . . ? C2 N6 H6 112(3) . . ? C22 N6 H6 118(3) . . ? C25 N7 C27 119.4(3) . . ? C25 N7 Li3 106.9(3) . . ? C27 N7 Li3 128.7(3) . . ? C25 N7 Li1 94.6(3) . . ? C27 N7 Li1 81.9(3) . . ? Li3 N7 Li1 116.7(3) . . ? C25 N8 C37 120.4(3) . . ? C25 N8 Li2 112.9(3) . . ? C37 N8 Li2 125.2(3) . . ? C25 N9 C40 126.5(3) . . ? C25 N9 H9 114(3) . . ? C40 N9 H9 116(3) . . ? C35 N10 C26 115.9(3) . . ? C35 N10 Li3 127.9(3) . . ? C26 N10 Li3 115.3(3) . . ? C35 N10 Li4 112.6(3) . . ? C26 N10 Li4 81.1(3) . . ? Li3 N10 Li4 84.1(3) . . ? C26 N11 C43 120.2(3) . . ? C26 N11 Li4 94.9(3) . . ? C43 N11 Li4 144.1(3) . . ? C26 N12 C46 127.4(3) . . ? C26 N12 H12 113(3) . . ? C46 N12 H12 119(3) . . ? N2 C1 N3 123.4(4) . . ? N2 C1 N1 117.9(3) . . ? N3 C1 N1 118.6(3) . . ? N2 C1 Li1 55.5(3) . . ? N3 C1 Li1 170.7(4) . . ? N1 C1 Li1 62.8(3) . . ? N5 C2 N4 116.8(3) . . ? N5 C2 N6 123.3(3) . . ? N4 C2 N6 119.7(3) . . ? N5 C2 Li3 49.3(2) . . ? N4 C2 Li3 68.2(2) . . ? N6 C2 Li3 171.3(3) . . ? N5 C2 Li2 92.7(3) . . ? N4 C2 Li2 44.5(2) . . ? N6 C2 Li2 125.1(3) . . ? Li3 C2 Li2 62.8(2) . . ? C4 C3 N1 119.8(4) . . ? C4 C3 C12 118.0(4) . . ? N1 C3 C12 122.1(3) . . ? C3 C4 C5 122.6(4) . . ? C3 C4 H4 118.7 . . ? C5 C4 H4 118.7 . . ? C6 C5 C4 120.1(4) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 120.6(4) . . ? C5 C6 H6A 119.7 . . ? C7 C6 H6A 119.7 . . ? C6 C7 C8 117.5(4) . . ? C6 C7 C12 121.1(4) . . ? C8 C7 C12 121.4(4) . . ? C9 C8 C7 120.2(4) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 120.3(5) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C11 C10 C9 122.7(4) . . ? C11 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N4 C11 C10 119.3(4) . . ? N4 C11 C12 121.6(3) . . ? C10 C11 C12 118.9(3) . . ? N4 C11 Li4 83.3(3) . . ? C10 C11 Li4 78.6(3) . . ? C12 C11 Li4 103.0(3) . . ? C3 C12 C7 117.4(3) . . ? C3 C12 C11 126.3(3) . . ? C7 C12 C11 116.3(3) . . ? N2 C13 C15 108.5(3) . . ? N2 C13 C14 111.9(3) . . ? C15 C13 C14 110.3(4) . . ? N2 C13 H13 108.7 . . ? C15 C13 H13 108.7 . . ? C14 C13 H13 108.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C18 110.6(4) . . ? N3 C16 C17 109.2(4) . . ? C18 C16 C17 109.8(4) . . ? N3 C16 H16 109.1 . . ? C18 C16 H16 109.1 . . ? C17 C16 H16 109.1 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N5 C19 C20 112.3(3) . . ? N5 C19 C21 108.8(3) . . ? C20 C19 C21 110.5(3) . . ? N5 C19 H19 108.4 . . ? C20 C19 H19 108.4 . . ? C21 C19 H19 108.4 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N6 C22 C24 111.6(4) . . ? N6 C22 C23 109.2(4) . . ? C24 C22 C23 110.9(5) . . ? N6 C22 H22 108.4 . . ? C24 C22 H22 108.4 . . ? C23 C22 H22 108.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N8 C25 N9 122.8(3) . . ? N8 C25 N7 115.8(3) . . ? N9 C25 N7 121.4(3) . . ? N8 C25 Li1 81.8(2) . . ? N9 C25 Li1 135.7(3) . . ? N7 C25 Li1 53.9(2) . . ? N8 C25 Li3 91.7(2) . . ? N9 C25 Li3 128.0(3) . . ? N7 C25 Li3 43.8(2) . . ? Li1 C25 Li3 81.5(2) . . ? N8 C25 Li2 41.2(2) . . ? N9 C25 Li2 163.6(3) . . ? N7 C25 Li2 74.5(2) . . ? Li1 C25 Li2 55.2(2) . . ? Li3 C25 Li2 59.5(2) . . ? N11 C26 N12 123.9(4) . . ? N11 C26 N10 117.3(3) . . ? N12 C26 N10 118.7(3) . . ? N11 C26 Li4 53.1(3) . . ? N12 C26 Li4 175.0(3) . . ? N10 C26 Li4 64.3(3) . . ? C28 C27 N7 119.4(3) . . ? C28 C27 C36 119.1(3) . . ? N7 C27 C36 121.4(3) . . ? C28 C27 Li1 79.7(3) . . ? N7 C27 Li1 62.5(3) . . ? C36 C27 Li1 125.7(3) . . ? C27 C28 C29 123.6(3) . . ? C27 C28 H28 118.2 . . ? C29 C28 H28 118.2 . . ? C30 C29 C28 119.0(4) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C29 C30 C31 120.8(3) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C32 C31 C30 117.8(3) . . ? C32 C31 C36 120.3(4) . . ? C30 C31 C36 121.9(3) . . ? C33 C32 C31 119.9(3) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 121.9(4) . . ? C32 C33 H33 119.1 . . ? C34 C33 H33 119.1 . . ? C33 C34 C35 121.8(4) . . ? C33 C34 H34 119.1 . . ? C35 C34 H34 119.1 . . ? N10 C35 C34 119.6(3) . . ? N10 C35 C36 122.9(3) . . ? C34 C35 C36 117.4(3) . . ? C31 C36 C27 115.7(3) . . ? C31 C36 C35 118.6(3) . . ? C27 C36 C35 125.7(3) . . ? N8 C37 C39 107.6(3) . . ? N8 C37 C38 112.4(3) . . ? C39 C37 C38 110.8(3) . . ? N8 C37 H37 108.6 . . ? C39 C37 H37 108.6 . . ? C38 C37 H37 108.6 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N9 C40 C42 111.9(3) . . ? N9 C40 C41 107.6(4) . . ? C42 C40 C41 113.0(4) . . ? N9 C40 H40 108.0 . . ? C42 C40 H40 108.0 . . ? C41 C40 H40 108.0 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N11 C43 C44 109.5(4) . . ? N11 C43 C45 110.4(3) . . ? C44 C43 C45 111.8(4) . . ? N11 C43 H43 108.4 . . ? C44 C43 H43 108.4 . . ? C45 C43 H43 108.4 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N12 C46 C47 110.6(4) . . ? N12 C46 C48 110.1(3) . . ? C47 C46 C48 109.6(4) . . ? N12 C46 H46 108.8 . . ? C47 C46 H46 108.8 . . ? C48 C46 H46 108.8 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O1 C49 C50 106.9(4) . . ? O1 C49 H49A 110.3 . . ? C50 C49 H49A 110.3 . . ? O1 C49 H49B 110.3 . . ? C50 C49 H49B 110.3 . . ? H49A C49 H49B 108.6 . . ? C49 C50 C51 104.7(4) . . ? C49 C50 H50A 110.8 . . ? C51 C50 H50A 110.8 . . ? C49 C50 H50B 110.8 . . ? C51 C50 H50B 110.8 . . ? H50A C50 H50B 108.9 . . ? C52 C51 C50 107.4(4) . . ? C52 C51 H51A 110.2 . . ? C50 C51 H51A 110.2 . . ? C52 C51 H51B 110.2 . . ? C50 C51 H51B 110.2 . . ? H51A C51 H51B 108.5 . . ? O1 C52 C51 107.5(4) . . ? O1 C52 H52A 110.2 . . ? C51 C52 H52A 110.2 . . ? O1 C52 H52B 110.2 . . ? C51 C52 H52B 110.2 . . ? H52A C52 H52B 108.5 . . ? N2 Li1 N7 148.0(5) . . ? N2 Li1 N1 68.4(2) . . ? N7 Li1 N1 116.9(4) . . ? N2 Li1 C27 146.0(4) . . ? N7 Li1 C27 35.59(15) . . ? N1 Li1 C27 145.4(4) . . ? N2 Li1 C1 33.01(16) . . ? N7 Li1 C1 140.4(4) . . ? N1 Li1 C1 35.50(16) . . ? C27 Li1 C1 174.4(4) . . ? N2 Li1 Li2 97.0(3) . . ? N7 Li1 Li2 72.0(3) . . ? N1 Li1 Li2 48.2(2) . . ? C27 Li1 Li2 107.0(3) . . ? C1 Li1 Li2 70.0(3) . . ? N2 Li1 C25 116.6(4) . . ? N7 Li1 C25 31.44(15) . . ? N1 Li1 C25 112.5(3) . . ? C27 Li1 C25 56.88(19) . . ? C1 Li1 C25 117.7(3) . . ? Li2 Li1 C25 65.1(3) . . ? N2 Li1 Li3 147.2(3) . . ? N7 Li1 Li3 30.10(17) . . ? N1 Li1 Li3 88.7(3) . . ? C27 Li1 Li3 58.8(2) . . ? C1 Li1 Li3 119.5(3) . . ? Li2 Li1 Li3 50.7(2) . . ? C25 Li1 Li3 50.06(18) . . ? N4 Li2 N1 95.0(3) . . ? N4 Li2 N8 136.0(4) . . ? N1 Li2 N8 121.5(4) . . ? N4 Li2 Li1 113.6(4) . . ? N1 Li2 Li1 55.9(3) . . ? N8 Li2 Li1 75.3(3) . . ? N4 Li2 C2 30.43(16) . . ? N1 Li2 C2 123.8(3) . . ? N8 Li2 C2 113.2(3) . . ? Li1 Li2 C2 135.6(3) . . ? N4 Li2 Li3 60.5(2) . . ? N1 Li2 Li3 120.4(3) . . ? N8 Li2 Li3 78.9(3) . . ? Li1 Li2 Li3 83.7(3) . . ? C2 Li2 Li3 57.7(2) . . ? N4 Li2 C25 119.6(3) . . ? N1 Li2 C25 114.8(3) . . ? N8 Li2 C25 25.86(14) . . ? Li1 Li2 C25 59.7(2) . . ? C2 Li2 C25 108.4(2) . . ? Li3 Li2 C25 59.0(2) . . ? N10 Li3 N7 93.2(3) . . ? N10 Li3 N5 131.3(4) . . ? N7 Li3 N5 135.5(3) . . ? N10 Li3 N4 114.2(3) . . ? N7 Li3 N4 107.4(3) . . ? N5 Li3 N4 61.25(19) . . ? N10 Li3 C2 125.8(3) . . ? N7 Li3 C2 129.2(3) . . ? N5 Li3 C2 29.74(14) . . ? N4 Li3 C2 31.78(13) . . ? N10 Li3 C25 119.3(3) . . ? N7 Li3 C25 29.24(14) . . ? N5 Li3 C25 107.8(3) . . ? N4 Li3 C25 104.6(2) . . ? C2 Li3 C25 112.0(2) . . ? N10 Li3 Li2 135.8(3) . . ? N7 Li3 Li2 69.8(3) . . ? N5 Li3 Li2 77.2(3) . . ? N4 Li3 Li2 43.12(19) . . ? C2 Li3 Li2 59.5(2) . . ? C25 Li3 Li2 61.5(2) . . ? N10 Li3 Li4 52.2(2) . . ? N7 Li3 Li4 108.9(3) . . ? N5 Li3 Li4 102.3(3) . . ? N4 Li3 Li4 61.9(2) . . ? C2 Li3 Li4 79.8(2) . . ? C25 Li3 Li4 134.4(3) . . ? Li2 Li3 Li4 93.9(3) . . ? N10 Li3 Li1 98.8(3) . . ? N7 Li3 Li1 33.24(18) . . ? N5 Li3 Li1 122.8(3) . . ? N4 Li3 Li1 75.3(2) . . ? C2 Li3 Li1 102.3(2) . . ? C25 Li3 Li1 48.42(18) . . ? Li2 Li3 Li1 45.6(2) . . ? Li4 Li3 Li1 86.5(3) . . ? O1 Li4 N11 117.9(4) . . ? O1 Li4 N10 110.9(3) . . ? N11 Li4 N10 66.5(2) . . ? O1 Li4 C26 121.0(3) . . ? N11 Li4 C26 32.00(16) . . ? N10 Li4 C26 34.59(15) . . ? O1 Li4 C11 102.8(3) . . ? N11 Li4 C11 129.2(3) . . ? N10 Li4 C11 126.5(4) . . ? C26 Li4 C11 135.9(3) . . ? O1 Li4 N4 122.1(3) . . ? N11 Li4 N4 119.8(3) . . ? N10 Li4 N4 96.0(3) . . ? C26 Li4 N4 110.4(3) . . ? C11 Li4 N4 30.54(13) . . ? O1 Li4 Li3 131.3(4) . . ? N11 Li4 Li3 91.2(3) . . ? N10 Li4 Li3 43.6(2) . . ? C26 Li4 Li3 65.2(2) . . ? C11 Li4 Li3 82.9(3) . . ? N4 Li4 Li3 52.42(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 N2 C1 N3 -4.3(6) . . . . ? Li1 N2 C1 N3 -168.9(4) . . . . ? C13 N2 C1 N1 172.1(3) . . . . ? Li1 N2 C1 N1 7.5(4) . . . . ? C13 N2 C1 Li1 164.6(4) . . . . ? C16 N3 C1 N2 165.8(4) . . . . ? C16 N3 C1 N1 -10.6(6) . . . . ? C16 N3 C1 Li1 86(2) . . . . ? C3 N1 C1 N2 118.2(4) . . . . ? Li2 N1 C1 N2 -77.3(4) . . . . ? Li1 N1 C1 N2 -6.9(4) . . . . ? C3 N1 C1 N3 -65.3(4) . . . . ? Li2 N1 C1 N3 99.3(4) . . . . ? Li1 N1 C1 N3 169.6(4) . . . . ? C3 N1 C1 Li1 125.1(4) . . . . ? Li2 N1 C1 Li1 -70.3(3) . . . . ? C19 N5 C2 N4 -164.5(3) . . . . ? Li3 N5 C2 N4 10.7(4) . . . . ? C19 N5 C2 N6 10.7(6) . . . . ? Li3 N5 C2 N6 -174.0(4) . . . . ? C19 N5 C2 Li3 -175.3(4) . . . . ? C19 N5 C2 Li2 -125.4(3) . . . . ? Li3 N5 C2 Li2 49.8(3) . . . . ? C11 N4 C2 N5 -141.8(3) . . . . ? Li2 N4 C2 N5 64.0(4) . . . . ? Li3 N4 C2 N5 -8.8(3) . . . . ? Li4 N4 C2 N5 -67.7(4) . . . . ? C11 N4 C2 N6 42.8(5) . . . . ? Li2 N4 C2 N6 -111.4(4) . . . . ? Li3 N4 C2 N6 175.8(4) . . . . ? Li4 N4 C2 N6 116.9(4) . . . . ? C11 N4 C2 Li3 -133.0(3) . . . . ? Li2 N4 C2 Li3 72.8(3) . . . . ? Li4 N4 C2 Li3 -58.9(2) . . . . ? C11 N4 C2 Li2 154.2(4) . . . . ? Li3 N4 C2 Li2 -72.8(3) . . . . ? Li4 N4 C2 Li2 -131.7(3) . . . . ? C22 N6 C2 N5 -147.8(4) . . . . ? C22 N6 C2 N4 27.3(6) . . . . ? C22 N6 C2 Li3 -179(100) . . . . ? C22 N6 C2 Li2 -25.6(6) . . . . ? C1 N1 C3 C4 -14.4(5) . . . . ? Li2 N1 C3 C4 -176.9(4) . . . . ? Li1 N1 C3 C4 84.9(5) . . . . ? C1 N1 C3 C12 167.5(3) . . . . ? Li2 N1 C3 C12 5.1(5) . . . . ? Li1 N1 C3 C12 -93.1(4) . . . . ? N1 C3 C4 C5 -179.9(3) . . . . ? C12 C3 C4 C5 -1.8(5) . . . . ? C3 C4 C5 C6 1.3(6) . . . . ? C4 C5 C6 C7 -0.8(6) . . . . ? C5 C6 C7 C8 -179.8(4) . . . . ? C5 C6 C7 C12 0.8(6) . . . . ? C6 C7 C8 C9 -179.1(4) . . . . ? C12 C7 C8 C9 0.4(6) . . . . ? C7 C8 C9 C10 1.7(7) . . . . ? C8 C9 C10 C11 -4.8(7) . . . . ? C2 N4 C11 C10 28.3(5) . . . . ? Li2 N4 C11 C10 176.2(4) . . . . ? Li3 N4 C11 C10 -77.0(4) . . . . ? Li4 N4 C11 C10 -72.9(3) . . . . ? C2 N4 C11 C12 -157.6(3) . . . . ? Li2 N4 C11 C12 -9.7(5) . . . . ? Li3 N4 C11 C12 97.1(4) . . . . ? Li4 N4 C11 C12 101.2(3) . . . . ? C2 N4 C11 Li4 101.2(3) . . . . ? Li2 N4 C11 Li4 -110.9(4) . . . . ? Li3 N4 C11 Li4 -4.1(4) . . . . ? C9 C10 C11 N4 179.9(4) . . . . ? C9 C10 C11 C12 5.6(5) . . . . ? C9 C10 C11 Li4 104.3(4) . . . . ? C4 C3 C12 C7 1.7(4) . . . . ? N1 C3 C12 C7 179.8(3) . . . . ? C4 C3 C12 C11 -179.6(3) . . . . ? N1 C3 C12 C11 -1.5(5) . . . . ? C6 C7 C12 C3 -1.2(5) . . . . ? C8 C7 C12 C3 179.4(3) . . . . ? C6 C7 C12 C11 179.9(3) . . . . ? C8 C7 C12 C11 0.5(5) . . . . ? N4 C11 C12 C3 3.8(5) . . . . ? C10 C11 C12 C3 177.9(3) . . . . ? Li4 C11 C12 C3 93.9(4) . . . . ? N4 C11 C12 C7 -177.5(3) . . . . ? C10 C11 C12 C7 -3.3(5) . . . . ? Li4 C11 C12 C7 -87.4(3) . . . . ? C1 N2 C13 C15 -156.4(4) . . . . ? Li1 N2 C13 C15 -3.8(7) . . . . ? C1 N2 C13 C14 81.7(4) . . . . ? Li1 N2 C13 C14 -125.7(6) . . . . ? C1 N3 C16 C18 -98.7(5) . . . . ? C1 N3 C16 C17 140.3(4) . . . . ? C2 N5 C19 C20 -86.5(4) . . . . ? Li3 N5 C19 C20 100.5(5) . . . . ? C2 N5 C19 C21 150.8(4) . . . . ? Li3 N5 C19 C21 -22.1(6) . . . . ? C2 N6 C22 C24 91.1(5) . . . . ? C2 N6 C22 C23 -146.0(4) . . . . ? C37 N8 C25 N9 8.6(6) . . . . ? Li2 N8 C25 N9 175.2(4) . . . . ? C37 N8 C25 N7 -168.3(3) . . . . ? Li2 N8 C25 N7 -1.6(5) . . . . ? C37 N8 C25 Li1 148.6(4) . . . . ? Li2 N8 C25 Li1 -44.7(3) . . . . ? C37 N8 C25 Li3 -130.2(3) . . . . ? Li2 N8 C25 Li3 36.5(3) . . . . ? C37 N8 C25 Li2 -166.6(5) . . . . ? C40 N9 C25 N8 -152.7(4) . . . . ? C40 N9 C25 N7 23.9(6) . . . . ? C40 N9 C25 Li1 92.7(6) . . . . ? C40 N9 C25 Li3 -29.5(6) . . . . ? C40 N9 C25 Li2 -141.5(10) . . . . ? C27 N7 C25 N8 -140.0(3) . . . . ? Li3 N7 C25 N8 62.9(4) . . . . ? Li1 N7 C25 N8 -56.8(4) . . . . ? C27 N7 C25 N9 43.1(5) . . . . ? Li3 N7 C25 N9 -114.0(4) . . . . ? Li1 N7 C25 N9 126.3(4) . . . . ? C27 N7 C25 Li1 -83.3(3) . . . . ? Li3 N7 C25 Li1 119.7(3) . . . . ? C27 N7 C25 Li3 157.0(4) . . . . ? Li1 N7 C25 Li3 -119.7(3) . . . . ? C27 N7 C25 Li2 -141.2(3) . . . . ? Li3 N7 C25 Li2 61.8(3) . . . . ? Li1 N7 C25 Li2 -57.9(3) . . . . ? C43 N11 C26 N12 -2.9(5) . . . . ? Li4 N11 C26 N12 -175.0(4) . . . . ? C43 N11 C26 N10 176.2(3) . . . . ? Li4 N11 C26 N10 4.2(4) . . . . ? C43 N11 C26 Li4 172.1(4) . . . . ? C46 N12 C26 N11 171.1(4) . . . . ? C46 N12 C26 N10 -8.1(5) . . . . ? C46 N12 C26 Li4 118(4) . . . . ? C35 N10 C26 N11 107.2(3) . . . . ? Li3 N10 C26 N11 -82.9(4) . . . . ? Li4 N10 C26 N11 -3.7(3) . . . . ? C35 N10 C26 N12 -73.6(4) . . . . ? Li3 N10 C26 N12 96.4(4) . . . . ? Li4 N10 C26 N12 175.5(4) . . . . ? C35 N10 C26 Li4 110.9(3) . . . . ? Li3 N10 C26 Li4 -79.1(3) . . . . ? C25 N7 C27 C28 32.4(5) . . . . ? Li3 N7 C27 C28 -176.2(3) . . . . ? Li1 N7 C27 C28 -58.4(4) . . . . ? C25 N7 C27 C36 -152.3(3) . . . . ? Li3 N7 C27 C36 -0.9(5) . . . . ? Li1 N7 C27 C36 116.9(4) . . . . ? C25 N7 C27 Li1 90.8(4) . . . . ? Li3 N7 C27 Li1 -117.8(4) . . . . ? N7 C27 C28 C29 176.5(3) . . . . ? C36 C27 C28 C29 1.1(5) . . . . ? Li1 C27 C28 C29 126.3(4) . . . . ? C27 C28 C29 C30 0.4(6) . . . . ? C28 C29 C30 C31 -1.0(6) . . . . ? C29 C30 C31 C32 179.3(3) . . . . ? C29 C30 C31 C36 0.1(6) . . . . ? C30 C31 C32 C33 -177.9(4) . . . . ? C36 C31 C32 C33 1.3(5) . . . . ? C31 C32 C33 C34 -2.9(6) . . . . ? C32 C33 C34 C35 1.6(6) . . . . ? C26 N10 C35 C34 -8.6(5) . . . . ? Li3 N10 C35 C34 -177.1(3) . . . . ? Li4 N10 C35 C34 82.3(4) . . . . ? C26 N10 C35 C36 174.1(3) . . . . ? Li3 N10 C35 C36 5.7(5) . . . . ? Li4 N10 C35 C36 -94.9(4) . . . . ? C33 C34 C35 N10 -176.3(3) . . . . ? C33 C34 C35 C36 1.1(5) . . . . ? C32 C31 C36 C27 -177.8(3) . . . . ? C30 C31 C36 C27 1.3(5) . . . . ? C32 C31 C36 C35 1.4(5) . . . . ? C30 C31 C36 C35 -179.4(3) . . . . ? C28 C27 C36 C31 -1.9(5) . . . . ? N7 C27 C36 C31 -177.2(3) . . . . ? Li1 C27 C36 C31 -100.3(4) . . . . ? C28 C27 C36 C35 178.9(3) . . . . ? N7 C27 C36 C35 3.6(5) . . . . ? Li1 C27 C36 C35 80.5(5) . . . . ? N10 C35 C36 C31 174.7(3) . . . . ? C34 C35 C36 C31 -2.6(5) . . . . ? N10 C35 C36 C27 -6.1(5) . . . . ? C34 C35 C36 C27 176.6(3) . . . . ? C25 N8 C37 C39 149.9(3) . . . . ? Li2 N8 C37 C39 -15.0(5) . . . . ? C25 N8 C37 C38 -87.7(4) . . . . ? Li2 N8 C37 C38 107.4(4) . . . . ? C25 N9 C40 C42 80.3(5) . . . . ? C25 N9 C40 C41 -154.9(4) . . . . ? C26 N11 C43 C44 157.1(4) . . . . ? Li4 N11 C43 C44 -36.5(7) . . . . ? C26 N11 C43 C45 -79.5(4) . . . . ? Li4 N11 C43 C45 86.9(6) . . . . ? C26 N12 C46 C47 131.9(4) . . . . ? C26 N12 C46 C48 -106.8(5) . . . . ? C52 O1 C49 C50 24.4(6) . . . . ? Li4 O1 C49 C50 -137.3(4) . . . . ? O1 C49 C50 C51 -16.0(6) . . . . ? C49 C50 C51 C52 2.1(6) . . . . ? C49 O1 C52 C51 -23.1(6) . . . . ? Li4 O1 C52 C51 140.5(4) . . . . ? C50 C51 C52 O1 12.6(7) . . . . ? C1 N2 Li1 N7 101.9(7) . . . . ? C13 N2 Li1 N7 -54.7(10) . . . . ? C1 N2 Li1 N1 -4.6(3) . . . . ? C13 N2 Li1 N1 -161.2(5) . . . . ? C1 N2 Li1 C27 170.0(7) . . . . ? C13 N2 Li1 C27 13.5(12) . . . . ? C13 N2 Li1 C1 -156.6(6) . . . . ? C1 N2 Li1 Li2 35.0(3) . . . . ? C13 N2 Li1 Li2 -121.6(5) . . . . ? C1 N2 Li1 C25 100.6(4) . . . . ? C13 N2 Li1 C25 -56.0(7) . . . . ? C1 N2 Li1 Li3 43.9(7) . . . . ? C13 N2 Li1 Li3 -112.6(7) . . . . ? C25 N7 Li1 N2 -2.2(8) . . . . ? C27 N7 Li1 N2 116.9(7) . . . . ? Li3 N7 Li1 N2 -113.8(7) . . . . ? C25 N7 Li1 N1 89.6(4) . . . . ? C27 N7 Li1 N1 -151.3(4) . . . . ? Li3 N7 Li1 N1 -21.9(5) . . . . ? C25 N7 Li1 C27 -119.0(3) . . . . ? Li3 N7 Li1 C27 129.4(3) . . . . ? C25 N7 Li1 C1 54.6(6) . . . . ? C27 N7 Li1 C1 173.6(6) . . . . ? Li3 N7 Li1 C1 -57.0(7) . . . . ? C25 N7 Li1 Li2 71.6(3) . . . . ? C27 N7 Li1 Li2 -169.4(3) . . . . ? Li3 N7 Li1 Li2 -40.0(3) . . . . ? C27 N7 Li1 C25 119.0(3) . . . . ? Li3 N7 Li1 C25 -111.6(3) . . . . ? C25 N7 Li1 Li3 111.6(3) . . . . ? C27 N7 Li1 Li3 -129.4(3) . . . . ? C1 N1 Li1 N2 4.3(2) . . . . ? C3 N1 Li1 N2 -113.3(4) . . . . ? Li2 N1 Li1 N2 122.0(3) . . . . ? C1 N1 Li1 N7 -140.9(4) . . . . ? C3 N1 Li1 N7 101.4(5) . . . . ? Li2 N1 Li1 N7 -23.3(4) . . . . ? C1 N1 Li1 C27 -170.4(7) . . . . ? C3 N1 Li1 C27 72.0(8) . . . . ? Li2 N1 Li1 C27 -52.8(7) . . . . ? C3 N1 Li1 C1 -117.7(4) . . . . ? Li2 N1 Li1 C1 117.6(3) . . . . ? C1 N1 Li1 Li2 -117.6(3) . . . . ? C3 N1 Li1 Li2 124.7(4) . . . . ? C1 N1 Li1 C25 -106.5(3) . . . . ? C3 N1 Li1 C25 135.8(3) . . . . ? Li2 N1 Li1 C25 11.1(3) . . . . ? C1 N1 Li1 Li3 -151.7(3) . . . . ? C3 N1 Li1 Li3 90.6(4) . . . . ? Li2 N1 Li1 Li3 -34.1(3) . . . . ? C28 C27 Li1 N2 8.8(8) . . . . ? N7 C27 Li1 N2 -122.3(8) . . . . ? C36 C27 Li1 N2 127.3(7) . . . . ? C28 C27 Li1 N7 131.1(3) . . . . ? C36 C27 Li1 N7 -110.4(4) . . . . ? C28 C27 Li1 N1 180.0(7) . . . . ? N7 C27 Li1 N1 48.9(7) . . . . ? C36 C27 Li1 N1 -61.5(8) . . . . ? C28 C27 Li1 C1 84(4) . . . . ? N7 C27 Li1 C1 -47(4) . . . . ? C36 C27 Li1 C1 -157(4) . . . . ? C28 C27 Li1 Li2 141.6(4) . . . . ? N7 C27 Li1 Li2 10.5(3) . . . . ? C36 C27 Li1 Li2 -99.9(4) . . . . ? C28 C27 Li1 C25 98.1(3) . . . . ? N7 C27 Li1 C25 -32.99(18) . . . . ? C36 C27 Li1 C25 -143.4(3) . . . . ? C28 C27 Li1 Li3 158.0(3) . . . . ? N7 C27 Li1 Li3 26.9(2) . . . . ? C36 C27 Li1 Li3 -83.5(3) . . . . ? N3 C1 Li1 N2 86(2) . . . . ? N1 C1 Li1 N2 -172.6(4) . . . . ? N2 C1 Li1 N7 -125.5(7) . . . . ? N3 C1 Li1 N7 -39(2) . . . . ? N1 C1 Li1 N7 61.9(6) . . . . ? N2 C1 Li1 N1 172.6(4) . . . . ? N3 C1 Li1 N1 -101(2) . . . . ? N2 C1 Li1 C27 -84(4) . . . . ? N3 C1 Li1 C27 2(6) . . . . ? N1 C1 Li1 C27 104(4) . . . . ? N2 C1 Li1 Li2 -142.7(4) . . . . ? N3 C1 Li1 Li2 -56(2) . . . . ? N1 C1 Li1 Li2 44.7(3) . . . . ? N2 C1 Li1 C25 -96.9(4) . . . . ? N3 C1 Li1 C25 -11(2) . . . . ? N1 C1 Li1 C25 90.6(4) . . . . ? N2 C1 Li1 Li3 -154.4(5) . . . . ? N3 C1 Li1 Li3 -68(2) . . . . ? N1 C1 Li1 Li3 33.0(3) . . . . ? N8 C25 Li1 N2 -50.9(4) . . . . ? N9 C25 Li1 N2 78.6(5) . . . . ? N7 C25 Li1 N2 178.7(5) . . . . ? Li3 C25 Li1 N2 -143.8(4) . . . . ? Li2 C25 Li1 N2 -85.3(4) . . . . ? N8 C25 Li1 N7 130.4(3) . . . . ? N9 C25 Li1 N7 -100.1(4) . . . . ? Li3 C25 Li1 N7 37.5(2) . . . . ? Li2 C25 Li1 N7 96.0(3) . . . . ? N8 C25 Li1 N1 25.3(4) . . . . ? N9 C25 Li1 N1 154.7(4) . . . . ? N7 C25 Li1 N1 -105.1(4) . . . . ? Li3 C25 Li1 N1 -67.7(3) . . . . ? Li2 C25 Li1 N1 -9.1(3) . . . . ? N8 C25 Li1 C27 167.9(3) . . . . ? N9 C25 Li1 C27 -62.7(4) . . . . ? N7 C25 Li1 C27 37.4(2) . . . . ? Li3 C25 Li1 C27 74.9(2) . . . . ? Li2 C25 Li1 C27 133.4(3) . . . . ? N8 C25 Li1 C1 -13.6(4) . . . . ? N9 C25 Li1 C1 115.8(4) . . . . ? N7 C25 Li1 C1 -144.1(4) . . . . ? Li3 C25 Li1 C1 -106.6(3) . . . . ? Li2 C25 Li1 C1 -48.1(3) . . . . ? N8 C25 Li1 Li2 34.4(3) . . . . ? N9 C25 Li1 Li2 163.8(4) . . . . ? N7 C25 Li1 Li2 -96.0(3) . . . . ? Li3 C25 Li1 Li2 -58.6(2) . . . . ? N8 C25 Li1 Li3 93.0(2) . . . . ? N9 C25 Li1 Li3 -137.6(4) . . . . ? N7 C25 Li1 Li3 -37.5(2) . . . . ? Li2 C25 Li1 Li3 58.6(2) . . . . ? C2 N4 Li2 N1 162.2(3) . . . . ? C11 N4 Li2 N1 10.4(5) . . . . ? Li3 N4 Li2 N1 -122.3(3) . . . . ? Li4 N4 Li2 N1 -71.6(3) . . . . ? C2 N4 Li2 N8 -50.0(6) . . . . ? C11 N4 Li2 N8 158.2(4) . . . . ? Li3 N4 Li2 N8 25.6(5) . . . . ? Li4 N4 Li2 N8 76.2(6) . . . . ? C2 N4 Li2 Li1 -142.9(3) . . . . ? C11 N4 Li2 Li1 65.3(5) . . . . ? Li3 N4 Li2 Li1 -67.4(3) . . . . ? Li4 N4 Li2 Li1 -16.7(4) . . . . ? C11 N4 Li2 C2 -151.8(5) . . . . ? Li3 N4 Li2 C2 75.5(3) . . . . ? Li4 N4 Li2 C2 126.2(4) . . . . ? C2 N4 Li2 Li3 -75.5(3) . . . . ? C11 N4 Li2 Li3 132.6(3) . . . . ? Li4 N4 Li2 Li3 50.6(3) . . . . ? C2 N4 Li2 C25 -75.6(4) . . . . ? C11 N4 Li2 C25 132.6(3) . . . . ? Li3 N4 Li2 C25 0.0(3) . . . . ? Li4 N4 Li2 C25 50.6(4) . . . . ? C1 N1 Li2 N4 -170.9(3) . . . . ? C3 N1 Li2 N4 -8.0(5) . . . . ? Li1 N1 Li2 N4 115.1(3) . . . . ? C1 N1 Li2 N8 34.8(5) . . . . ? C3 N1 Li2 N8 -162.2(3) . . . . ? Li1 N1 Li2 N8 -39.1(4) . . . . ? C1 N1 Li2 Li1 73.9(3) . . . . ? C3 N1 Li2 Li1 -123.1(4) . . . . ? C1 N1 Li2 C2 -160.2(3) . . . . ? C3 N1 Li2 C2 2.8(6) . . . . ? Li1 N1 Li2 C2 125.9(4) . . . . ? C1 N1 Li2 Li3 130.5(4) . . . . ? C3 N1 Li2 Li3 -66.6(5) . . . . ? Li1 N1 Li2 Li3 56.5(4) . . . . ? C1 N1 Li2 C25 63.2(4) . . . . ? C3 N1 Li2 C25 -133.8(3) . . . . ? Li1 N1 Li2 C25 -10.7(3) . . . . ? C25 N8 Li2 N4 -59.6(6) . . . . ? C37 N8 Li2 N4 106.3(6) . . . . ? C25 N8 Li2 N1 82.0(5) . . . . ? C37 N8 Li2 N1 -112.2(4) . . . . ? C25 N8 Li2 Li1 49.2(3) . . . . ? C37 N8 Li2 Li1 -144.9(4) . . . . ? C25 N8 Li2 C2 -84.5(4) . . . . ? C37 N8 Li2 C2 81.4(4) . . . . ? C25 N8 Li2 Li3 -37.0(3) . . . . ? C37 N8 Li2 Li3 128.8(3) . . . . ? C37 N8 Li2 C25 165.9(5) . . . . ? N2 Li1 Li2 N4 -132.3(4) . . . . ? N7 Li1 Li2 N4 78.6(3) . . . . ? N1 Li1 Li2 N4 -79.6(3) . . . . ? C27 Li1 Li2 N4 72.2(4) . . . . ? C1 Li1 Li2 N4 -112.8(3) . . . . ? C25 Li1 Li2 N4 111.7(3) . . . . ? Li3 Li1 Li2 N4 54.0(3) . . . . ? N2 Li1 Li2 N1 -52.6(3) . . . . ? N7 Li1 Li2 N1 158.2(4) . . . . ? C27 Li1 Li2 N1 151.8(4) . . . . ? C1 Li1 Li2 N1 -33.20(19) . . . . ? C25 Li1 Li2 N1 -168.7(3) . . . . ? Li3 Li1 Li2 N1 133.6(3) . . . . ? N2 Li1 Li2 N8 93.6(3) . . . . ? N7 Li1 Li2 N8 -55.6(2) . . . . ? N1 Li1 Li2 N8 146.2(4) . . . . ? C27 Li1 Li2 N8 -62.0(3) . . . . ? C1 Li1 Li2 N8 113.0(3) . . . . ? C25 Li1 Li2 N8 -22.49(17) . . . . ? Li3 Li1 Li2 N8 -80.2(2) . . . . ? N2 Li1 Li2 C2 -158.1(4) . . . . ? N7 Li1 Li2 C2 52.7(5) . . . . ? N1 Li1 Li2 C2 -105.5(5) . . . . ? C27 Li1 Li2 C2 46.3(6) . . . . ? C1 Li1 Li2 C2 -138.7(4) . . . . ? C25 Li1 Li2 C2 85.8(4) . . . . ? Li3 Li1 Li2 C2 28.1(4) . . . . ? N2 Li1 Li2 Li3 173.8(3) . . . . ? N7 Li1 Li2 Li3 24.6(2) . . . . ? N1 Li1 Li2 Li3 -133.6(3) . . . . ? C27 Li1 Li2 Li3 18.2(3) . . . . ? C1 Li1 Li2 Li3 -166.8(3) . . . . ? C25 Li1 Li2 Li3 57.7(2) . . . . ? N2 Li1 Li2 C25 116.1(3) . . . . ? N7 Li1 Li2 C25 -33.06(15) . . . . ? N1 Li1 Li2 C25 168.7(3) . . . . ? C27 Li1 Li2 C25 -39.5(3) . . . . ? C1 Li1 Li2 C25 135.5(3) . . . . ? Li3 Li1 Li2 C25 -57.7(2) . . . . ? N5 C2 Li2 N4 -126.5(4) . . . . ? N6 C2 Li2 N4 98.6(4) . . . . ? Li3 C2 Li2 N4 -85.8(3) . . . . ? N5 C2 Li2 N1 -148.0(4) . . . . ? N4 C2 Li2 N1 -21.5(3) . . . . ? N6 C2 Li2 N1 77.1(5) . . . . ? Li3 C2 Li2 N1 -107.3(4) . . . . ? N5 C2 Li2 N8 18.1(4) . . . . ? N4 C2 Li2 N8 144.6(5) . . . . ? N6 C2 Li2 N8 -116.8(4) . . . . ? Li3 C2 Li2 N8 58.8(3) . . . . ? N5 C2 Li2 Li1 -74.3(5) . . . . ? N4 C2 Li2 Li1 52.2(5) . . . . ? N6 C2 Li2 Li1 150.8(4) . . . . ? Li3 C2 Li2 Li1 -33.6(4) . . . . ? N5 C2 Li2 Li3 -40.7(2) . . . . ? N4 C2 Li2 Li3 85.8(3) . . . . ? N6 C2 Li2 Li3 -175.6(4) . . . . ? N5 C2 Li2 C25 -9.1(3) . . . . ? N4 C2 Li2 C25 117.4(4) . . . . ? N6 C2 Li2 C25 -144.0(3) . . . . ? Li3 C2 Li2 C25 31.6(2) . . . . ? N8 C25 Li2 N4 136.5(5) . . . . ? N9 C25 Li2 N4 122.0(11) . . . . ? N7 C25 Li2 N4 -45.1(4) . . . . ? Li1 C25 Li2 N4 -101.6(4) . . . . ? Li3 C25 Li2 N4 0.0(3) . . . . ? N8 C25 Li2 N1 -111.7(5) . . . . ? N9 C25 Li2 N1 -126.1(11) . . . . ? N7 C25 Li2 N1 66.8(4) . . . . ? Li1 C25 Li2 N1 10.3(3) . . . . ? Li3 C25 Li2 N1 111.9(4) . . . . ? N9 C25 Li2 N8 -14.4(11) . . . . ? N7 C25 Li2 N8 178.5(4) . . . . ? Li1 C25 Li2 N8 122.0(4) . . . . ? Li3 C25 Li2 N8 -136.4(4) . . . . ? N8 C25 Li2 Li1 -122.0(4) . . . . ? N9 C25 Li2 Li1 -136.4(11) . . . . ? N7 C25 Li2 Li1 56.5(3) . . . . ? Li3 C25 Li2 Li1 101.6(3) . . . . ? N8 C25 Li2 C2 105.3(4) . . . . ? N9 C25 Li2 C2 90.9(12) . . . . ? N7 C25 Li2 C2 -76.2(3) . . . . ? Li1 C25 Li2 C2 -132.7(4) . . . . ? Li3 C25 Li2 C2 -31.1(2) . . . . ? N8 C25 Li2 Li3 136.4(4) . . . . ? N9 C25 Li2 Li3 122.0(11) . . . . ? N7 C25 Li2 Li3 -45.1(2) . . . . ? Li1 C25 Li2 Li3 -101.6(3) . . . . ? C35 N10 Li3 N7 -2.7(4) . . . . ? C26 N10 Li3 N7 -171.2(3) . . . . ? Li4 N10 Li3 N7 111.5(3) . . . . ? C35 N10 Li3 N5 174.6(4) . . . . ? C26 N10 Li3 N5 6.1(6) . . . . ? Li4 N10 Li3 N5 -71.2(5) . . . . ? C35 N10 Li3 N4 -113.3(3) . . . . ? C26 N10 Li3 N4 78.1(4) . . . . ? Li4 N10 Li3 N4 0.9(3) . . . . ? C35 N10 Li3 C2 -147.7(3) . . . . ? C26 N10 Li3 C2 43.7(5) . . . . ? Li4 N10 Li3 C2 -33.5(4) . . . . ? C35 N10 Li3 C25 11.3(5) . . . . ? C26 N10 Li3 C25 -157.2(3) . . . . ? Li4 N10 Li3 C25 125.5(3) . . . . ? C35 N10 Li3 Li2 -66.7(6) . . . . ? C26 N10 Li3 Li2 124.8(4) . . . . ? Li4 N10 Li3 Li2 47.5(5) . . . . ? C35 N10 Li3 Li4 -114.2(4) . . . . ? C26 N10 Li3 Li4 77.3(3) . . . . ? C35 N10 Li3 Li1 -35.6(4) . . . . ? C26 N10 Li3 Li1 155.9(3) . . . . ? Li4 N10 Li3 Li1 78.6(3) . . . . ? C25 N7 Li3 N10 154.5(3) . . . . ? C27 N7 Li3 N10 0.3(5) . . . . ? Li1 N7 Li3 N10 -101.2(3) . . . . ? C25 N7 Li3 N5 -22.6(6) . . . . ? C27 N7 Li3 N5 -176.7(4) . . . . ? Li1 N7 Li3 N5 81.8(6) . . . . ? C25 N7 Li3 N4 -88.9(3) . . . . ? C27 N7 Li3 N4 116.9(3) . . . . ? Li1 N7 Li3 N4 15.4(4) . . . . ? C25 N7 Li3 C2 -62.3(4) . . . . ? C27 N7 Li3 C2 143.5(3) . . . . ? Li1 N7 Li3 C2 42.0(5) . . . . ? C27 N7 Li3 C25 -154.2(5) . . . . ? Li1 N7 Li3 C25 104.3(4) . . . . ? C25 N7 Li3 Li2 -67.4(3) . . . . ? C27 N7 Li3 Li2 138.4(3) . . . . ? Li1 N7 Li3 Li2 37.0(3) . . . . ? C25 N7 Li3 Li4 -154.5(3) . . . . ? C27 N7 Li3 Li4 51.3(5) . . . . ? Li1 N7 Li3 Li4 -50.2(4) . . . . ? C25 N7 Li3 Li1 -104.3(4) . . . . ? C27 N7 Li3 Li1 101.5(4) . . . . ? C2 N5 Li3 N10 91.9(5) . . . . ? C19 N5 Li3 N10 -94.4(6) . . . . ? C2 N5 Li3 N7 -92.1(5) . . . . ? C19 N5 Li3 N7 81.7(7) . . . . ? C2 N5 Li3 N4 -6.2(2) . . . . ? C19 N5 Li3 N4 167.6(4) . . . . ? C19 N5 Li3 C2 173.8(6) . . . . ? C2 N5 Li3 C25 -103.4(3) . . . . ? C19 N5 Li3 C25 70.4(5) . . . . ? C2 N5 Li3 Li2 -49.3(3) . . . . ? C19 N5 Li3 Li2 124.4(4) . . . . ? C2 N5 Li3 Li4 41.9(3) . . . . ? C19 N5 Li3 Li4 -144.4(4) . . . . ? C2 N5 Li3 Li1 -51.9(4) . . . . ? C19 N5 Li3 Li1 121.9(4) . . . . ? C2 N4 Li3 N10 -119.5(4) . . . . ? C11 N4 Li3 N10 3.3(5) . . . . ? Li2 N4 Li3 N10 132.1(4) . . . . ? Li4 N4 Li3 N10 -0.8(3) . . . . ? C2 N4 Li3 N7 138.7(3) . . . . ? C11 N4 Li3 N7 -98.5(4) . . . . ? Li2 N4 Li3 N7 30.3(3) . . . . ? Li4 N4 Li3 N7 -102.6(3) . . . . ? C2 N4 Li3 N5 5.8(2) . . . . ? C11 N4 Li3 N5 128.6(4) . . . . ? Li2 N4 Li3 N5 -102.5(3) . . . . ? Li4 N4 Li3 N5 124.5(3) . . . . ? C11 N4 Li3 C2 122.8(4) . . . . ? Li2 N4 Li3 C2 -108.3(3) . . . . ? Li4 N4 Li3 C2 118.7(3) . . . . ? C2 N4 Li3 C25 108.4(3) . . . . ? C11 N4 Li3 C25 -128.8(3) . . . . ? Li2 N4 Li3 C25 0.0(3) . . . . ? Li4 N4 Li3 C25 -132.9(3) . . . . ? C2 N4 Li3 Li2 108.3(3) . . . . ? C11 N4 Li3 Li2 -128.8(4) . . . . ? Li4 N4 Li3 Li2 -132.9(3) . . . . ? C2 N4 Li3 Li4 -118.7(3) . . . . ? C11 N4 Li3 Li4 4.1(4) . . . . ? Li2 N4 Li3 Li4 132.9(3) . . . . ? C2 N4 Li3 Li1 147.3(3) . . . . ? C11 N4 Li3 Li1 -89.9(4) . . . . ? Li2 N4 Li3 Li1 39.0(3) . . . . ? Li4 N4 Li3 Li1 -93.9(2) . . . . ? N5 C2 Li3 N10 -112.2(5) . . . . ? N4 C2 Li3 N10 78.2(4) . . . . ? N6 C2 Li3 N10 -77(2) . . . . ? Li2 C2 Li3 N10 127.0(4) . . . . ? N5 C2 Li3 N7 115.3(5) . . . . ? N4 C2 Li3 N7 -54.3(4) . . . . ? N6 C2 Li3 N7 150.2(19) . . . . ? Li2 C2 Li3 N7 -5.5(4) . . . . ? N4 C2 Li3 N5 -169.7(4) . . . . ? N6 C2 Li3 N5 35(2) . . . . ? Li2 C2 Li3 N5 -120.9(3) . . . . ? N5 C2 Li3 N4 169.7(4) . . . . ? N6 C2 Li3 N4 -155(2) . . . . ? Li2 C2 Li3 N4 48.8(2) . . . . ? N5 C2 Li3 C25 87.5(3) . . . . ? N4 C2 Li3 C25 -82.2(3) . . . . ? N6 C2 Li3 C25 122(2) . . . . ? Li2 C2 Li3 C25 -33.3(3) . . . . ? N5 C2 Li3 Li2 120.9(3) . . . . ? N4 C2 Li3 Li2 -48.8(2) . . . . ? N6 C2 Li3 Li2 156(2) . . . . ? N5 C2 Li3 Li4 -138.5(4) . . . . ? N4 C2 Li3 Li4 51.8(3) . . . . ? N6 C2 Li3 Li4 -104(2) . . . . ? Li2 C2 Li3 Li4 100.7(3) . . . . ? N5 C2 Li3 Li1 137.4(4) . . . . ? N4 C2 Li3 Li1 -32.3(3) . . . . ? N6 C2 Li3 Li1 172(2) . . . . ? Li2 C2 Li3 Li1 16.5(2) . . . . ? N8 C25 Li3 N10 -156.2(4) . . . . ? N9 C25 Li3 N10 68.5(5) . . . . ? N7 C25 Li3 N10 -29.5(3) . . . . ? Li1 C25 Li3 N10 -74.8(4) . . . . ? Li2 C25 Li3 N10 -129.1(4) . . . . ? N8 C25 Li3 N7 -126.7(4) . . . . ? N9 C25 Li3 N7 98.0(4) . . . . ? Li1 C25 Li3 N7 -45.2(3) . . . . ? Li2 C25 Li3 N7 -99.6(3) . . . . ? N8 C25 Li3 N5 36.9(3) . . . . ? N9 C25 Li3 N5 -98.4(4) . . . . ? N7 C25 Li3 N5 163.6(4) . . . . ? Li1 C25 Li3 N5 118.4(3) . . . . ? Li2 C25 Li3 N5 64.0(3) . . . . ? N8 C25 Li3 N4 -27.1(3) . . . . ? N9 C25 Li3 N4 -162.4(3) . . . . ? N7 C25 Li3 N4 99.6(3) . . . . ? Li1 C25 Li3 N4 54.4(2) . . . . ? Li2 C25 Li3 N4 0.0(2) . . . . ? N8 C25 Li3 C2 5.6(3) . . . . ? N9 C25 Li3 C2 -129.7(3) . . . . ? N7 C25 Li3 C2 132.2(4) . . . . ? Li1 C25 Li3 C2 87.0(3) . . . . ? Li2 C25 Li3 C2 32.6(3) . . . . ? N8 C25 Li3 Li2 -27.0(3) . . . . ? N9 C25 Li3 Li2 -162.3(4) . . . . ? N7 C25 Li3 Li2 99.6(3) . . . . ? Li1 C25 Li3 Li2 54.4(2) . . . . ? N8 C25 Li3 Li4 -91.9(4) . . . . ? N9 C25 Li3 Li4 132.8(4) . . . . ? N7 C25 Li3 Li4 34.8(4) . . . . ? Li1 C25 Li3 Li4 -10.5(4) . . . . ? Li2 C25 Li3 Li4 -64.8(4) . . . . ? N8 C25 Li3 Li1 -81.4(3) . . . . ? N9 C25 Li3 Li1 143.3(4) . . . . ? N7 C25 Li3 Li1 45.2(3) . . . . ? Li2 C25 Li3 Li1 -54.4(2) . . . . ? N4 Li2 Li3 N10 -76.1(5) . . . . ? N1 Li2 Li3 N10 1.5(7) . . . . ? N8 Li2 Li3 N10 121.7(4) . . . . ? Li1 Li2 Li3 N10 45.5(5) . . . . ? C2 Li2 Li3 N10 -111.6(5) . . . . ? C25 Li2 Li3 N10 103.8(4) . . . . ? N4 Li2 Li3 N7 -149.1(3) . . . . ? N1 Li2 Li3 N7 -71.5(4) . . . . ? N8 Li2 Li3 N7 48.7(2) . . . . ? Li1 Li2 Li3 N7 -27.5(3) . . . . ? C2 Li2 Li3 N7 175.4(3) . . . . ? C25 Li2 Li3 N7 30.87(15) . . . . ? N4 Li2 Li3 N5 61.4(2) . . . . ? N1 Li2 Li3 N5 139.0(4) . . . . ? N8 Li2 Li3 N5 -100.8(3) . . . . ? Li1 Li2 Li3 N5 -177.0(3) . . . . ? C2 Li2 Li3 N5 25.90(16) . . . . ? C25 Li2 Li3 N5 -118.7(3) . . . . ? N1 Li2 Li3 N4 77.6(4) . . . . ? N8 Li2 Li3 N4 -162.2(4) . . . . ? Li1 Li2 Li3 N4 121.6(3) . . . . ? C2 Li2 Li3 N4 -35.46(17) . . . . ? C25 Li2 Li3 N4 180.0(3) . . . . ? N4 Li2 Li3 C2 35.46(17) . . . . ? N1 Li2 Li3 C2 113.1(4) . . . . ? N8 Li2 Li3 C2 -126.7(3) . . . . ? Li1 Li2 Li3 C2 157.1(3) . . . . ? C25 Li2 Li3 C2 -144.6(3) . . . . ? N4 Li2 Li3 C25 -180.0(3) . . . . ? N1 Li2 Li3 C25 -102.4(4) . . . . ? N8 Li2 Li3 C25 17.84(17) . . . . ? Li1 Li2 Li3 C25 -58.3(2) . . . . ? C2 Li2 Li3 C25 144.6(3) . . . . ? N4 Li2 Li3 Li4 -40.4(2) . . . . ? N1 Li2 Li3 Li4 37.2(4) . . . . ? N8 Li2 Li3 Li4 157.4(3) . . . . ? Li1 Li2 Li3 Li4 81.3(3) . . . . ? C2 Li2 Li3 Li4 -75.8(2) . . . . ? C25 Li2 Li3 Li4 139.6(3) . . . . ? N4 Li2 Li3 Li1 -121.6(3) . . . . ? N1 Li2 Li3 Li1 -44.0(3) . . . . ? N8 Li2 Li3 Li1 76.2(3) . . . . ? C2 Li2 Li3 Li1 -157.1(3) . . . . ? C25 Li2 Li3 Li1 58.3(2) . . . . ? N2 Li1 Li3 N10 -161.3(6) . . . . ? N7 Li1 Li3 N10 82.4(4) . . . . ? N1 Li1 Li3 N10 -117.1(3) . . . . ? C27 Li1 Li3 N10 50.6(3) . . . . ? C1 Li1 Li3 N10 -135.5(4) . . . . ? Li2 Li1 Li3 N10 -149.8(4) . . . . ? C25 Li1 Li3 N10 121.6(3) . . . . ? N2 Li1 Li3 N7 116.4(8) . . . . ? N1 Li1 Li3 N7 160.5(5) . . . . ? C27 Li1 Li3 N7 -31.7(2) . . . . ? C1 Li1 Li3 N7 142.1(5) . . . . ? Li2 Li1 Li3 N7 127.8(4) . . . . ? C25 Li1 Li3 N7 39.2(2) . . . . ? N2 Li1 Li3 N5 -8.0(8) . . . . ? N7 Li1 Li3 N5 -124.4(5) . . . . ? N1 Li1 Li3 N5 36.2(4) . . . . ? C27 Li1 Li3 N5 -156.1(4) . . . . ? C1 Li1 Li3 N5 17.7(5) . . . . ? Li2 Li1 Li3 N5 3.5(4) . . . . ? C25 Li1 Li3 N5 -85.1(3) . . . . ? N2 Li1 Li3 N4 -48.5(7) . . . . ? N7 Li1 Li3 N4 -164.8(4) . . . . ? N1 Li1 Li3 N4 -4.3(2) . . . . ? C27 Li1 Li3 N4 163.4(3) . . . . ? C1 Li1 Li3 N4 -22.7(3) . . . . ? Li2 Li1 Li3 N4 -37.0(2) . . . . ? C25 Li1 Li3 N4 -125.6(2) . . . . ? N2 Li1 Li3 C2 -31.6(7) . . . . ? N7 Li1 Li3 C2 -147.9(4) . . . . ? N1 Li1 Li3 C2 12.6(3) . . . . ? C27 Li1 Li3 C2 -179.7(3) . . . . ? C1 Li1 Li3 C2 -5.8(4) . . . . ? Li2 Li1 Li3 C2 -20.1(3) . . . . ? C25 Li1 Li3 C2 -108.7(2) . . . . ? N2 Li1 Li3 C25 77.1(7) . . . . ? N7 Li1 Li3 C25 -39.2(2) . . . . ? N1 Li1 Li3 C25 121.3(3) . . . . ? C27 Li1 Li3 C25 -71.0(2) . . . . ? C1 Li1 Li3 C25 102.8(4) . . . . ? Li2 Li1 Li3 C25 88.6(3) . . . . ? N2 Li1 Li3 Li2 -11.5(6) . . . . ? N7 Li1 Li3 Li2 -127.8(4) . . . . ? N1 Li1 Li3 Li2 32.7(2) . . . . ? C27 Li1 Li3 Li2 -159.6(4) . . . . ? C1 Li1 Li3 Li2 14.3(3) . . . . ? C25 Li1 Li3 Li2 -88.6(3) . . . . ? N2 Li1 Li3 Li4 -110.3(7) . . . . ? N7 Li1 Li3 Li4 133.3(4) . . . . ? N1 Li1 Li3 Li4 -66.2(3) . . . . ? C27 Li1 Li3 Li4 101.6(3) . . . . ? C1 Li1 Li3 Li4 -84.6(4) . . . . ? Li2 Li1 Li3 Li4 -98.9(3) . . . . ? C25 Li1 Li3 Li4 172.5(3) . . . . ? C52 O1 Li4 N11 -25.4(6) . . . . ? C49 O1 Li4 N11 134.3(4) . . . . ? C52 O1 Li4 N10 -99.1(5) . . . . ? C49 O1 Li4 N10 60.6(5) . . . . ? C52 O1 Li4 C26 -62.1(6) . . . . ? C49 O1 Li4 C26 97.6(5) . . . . ? C52 O1 Li4 C11 123.2(4) . . . . ? C49 O1 Li4 C11 -77.1(5) . . . . ? C52 O1 Li4 N4 149.0(4) . . . . ? C49 O1 Li4 N4 -51.3(6) . . . . ? C52 O1 Li4 Li3 -145.1(5) . . . . ? C49 O1 Li4 Li3 14.6(7) . . . . ? C26 N11 Li4 O1 -104.7(4) . . . . ? C43 N11 Li4 O1 87.0(6) . . . . ? C26 N11 Li4 N10 -2.6(2) . . . . ? C43 N11 Li4 N10 -170.8(5) . . . . ? C43 N11 Li4 C26 -168.2(6) . . . . ? C26 N11 Li4 C11 116.3(5) . . . . ? C43 N11 Li4 C11 -51.9(8) . . . . ? C26 N11 Li4 N4 80.8(4) . . . . ? C43 N11 Li4 N4 -87.5(6) . . . . ? C26 N11 Li4 Li3 34.5(3) . . . . ? C43 N11 Li4 Li3 -133.8(5) . . . . ? C35 N10 Li4 O1 0.3(5) . . . . ? C26 N10 Li4 O1 114.7(4) . . . . ? Li3 N10 Li4 O1 -128.5(4) . . . . ? C35 N10 Li4 N11 -112.0(3) . . . . ? C26 N10 Li4 N11 2.4(2) . . . . ? Li3 N10 Li4 N11 119.2(3) . . . . ? C35 N10 Li4 C26 -114.4(3) . . . . ? Li3 N10 Li4 C26 116.8(3) . . . . ? C35 N10 Li4 C11 125.5(4) . . . . ? C26 N10 Li4 C11 -120.0(4) . . . . ? Li3 N10 Li4 C11 -3.2(4) . . . . ? C35 N10 Li4 N4 128.0(3) . . . . ? C26 N10 Li4 N4 -117.5(3) . . . . ? Li3 N10 Li4 N4 -0.7(3) . . . . ? C35 N10 Li4 Li3 128.7(3) . . . . ? C26 N10 Li4 Li3 -116.8(3) . . . . ? N11 C26 Li4 O1 93.8(5) . . . . ? N12 C26 Li4 O1 150(4) . . . . ? N10 C26 Li4 O1 -82.1(4) . . . . ? N12 C26 Li4 N11 56(4) . . . . ? N10 C26 Li4 N11 -175.9(4) . . . . ? N11 C26 Li4 N10 175.9(4) . . . . ? N12 C26 Li4 N10 -128(4) . . . . ? N11 C26 Li4 C11 -93.6(5) . . . . ? N12 C26 Li4 C11 -38(4) . . . . ? N10 C26 Li4 C11 90.5(5) . . . . ? N11 C26 Li4 N4 -114.0(4) . . . . ? N12 C26 Li4 N4 -58(4) . . . . ? N10 C26 Li4 N4 70.1(3) . . . . ? N11 C26 Li4 Li3 -141.4(3) . . . . ? N12 C26 Li4 Li3 -86(4) . . . . ? N10 C26 Li4 Li3 42.7(2) . . . . ? N4 C11 Li4 O1 133.5(4) . . . . ? C10 C11 Li4 O1 -104.8(4) . . . . ? C12 C11 Li4 O1 12.5(4) . . . . ? N4 C11 Li4 N11 -83.1(5) . . . . ? C10 C11 Li4 N11 38.6(5) . . . . ? C12 C11 Li4 N11 156.0(4) . . . . ? N4 C11 Li4 N10 4.9(4) . . . . ? C10 C11 Li4 N10 126.6(4) . . . . ? C12 C11 Li4 N10 -116.0(4) . . . . ? N4 C11 Li4 C26 -40.0(5) . . . . ? C10 C11 Li4 C26 81.7(5) . . . . ? C12 C11 Li4 C26 -161.0(5) . . . . ? C10 C11 Li4 N4 121.7(3) . . . . ? C12 C11 Li4 N4 -120.9(3) . . . . ? N4 C11 Li4 Li3 2.7(2) . . . . ? C10 C11 Li4 Li3 124.4(3) . . . . ? C12 C11 Li4 Li3 -118.3(3) . . . . ? C2 N4 Li4 O1 -172.2(4) . . . . ? C11 N4 Li4 O1 -56.7(4) . . . . ? Li2 N4 Li4 O1 64.4(5) . . . . ? Li3 N4 Li4 O1 120.0(4) . . . . ? C2 N4 Li4 N11 2.0(5) . . . . ? C11 N4 Li4 N11 117.6(4) . . . . ? Li2 N4 Li4 N11 -121.3(4) . . . . ? Li3 N4 Li4 N11 -65.8(4) . . . . ? C2 N4 Li4 N10 68.4(3) . . . . ? C11 N4 Li4 N10 -176.0(3) . . . . ? Li2 N4 Li4 N10 -54.9(4) . . . . ? Li3 N4 Li4 N10 0.6(2) . . . . ? C2 N4 Li4 C26 35.9(4) . . . . ? C11 N4 Li4 C26 151.5(4) . . . . ? Li2 N4 Li4 C26 -87.4(4) . . . . ? Li3 N4 Li4 C26 -31.9(3) . . . . ? C2 N4 Li4 C11 -115.6(3) . . . . ? Li2 N4 Li4 C11 121.1(4) . . . . ? Li3 N4 Li4 C11 176.7(3) . . . . ? C2 N4 Li4 Li3 67.8(3) . . . . ? C11 N4 Li4 Li3 -176.7(3) . . . . ? Li2 N4 Li4 Li3 -55.5(3) . . . . ? N10 Li3 Li4 O1 76.6(5) . . . . ? N7 Li3 Li4 O1 -2.4(6) . . . . ? N5 Li3 Li4 O1 -150.2(4) . . . . ? N4 Li3 Li4 O1 -102.5(5) . . . . ? C2 Li3 Li4 O1 -130.5(4) . . . . ? C25 Li3 Li4 O1 -19.5(7) . . . . ? Li2 Li3 Li4 O1 -72.4(5) . . . . ? Li1 Li3 Li4 O1 -27.4(5) . . . . ? N10 Li3 Li4 N11 -53.2(2) . . . . ? N7 Li3 Li4 N11 -132.2(3) . . . . ? N5 Li3 Li4 N11 80.0(3) . . . . ? N4 Li3 Li4 N11 127.7(3) . . . . ? C2 Li3 Li4 N11 99.7(3) . . . . ? C25 Li3 Li4 N11 -149.4(3) . . . . ? Li2 Li3 Li4 N11 157.8(3) . . . . ? Li1 Li3 Li4 N11 -157.2(3) . . . . ? N7 Li3 Li4 N10 -79.0(3) . . . . ? N5 Li3 Li4 N10 133.3(4) . . . . ? N4 Li3 Li4 N10 -179.1(3) . . . . ? C2 Li3 Li4 N10 152.9(3) . . . . ? C25 Li3 Li4 N10 -96.1(4) . . . . ? Li2 Li3 Li4 N10 -149.0(3) . . . . ? Li1 Li3 Li4 N10 -104.0(3) . . . . ? N10 Li3 Li4 C26 -33.92(18) . . . . ? N7 Li3 Li4 C26 -112.9(3) . . . . ? N5 Li3 Li4 C26 99.3(3) . . . . ? N4 Li3 Li4 C26 147.0(3) . . . . ? C2 Li3 Li4 C26 119.0(2) . . . . ? C25 Li3 Li4 C26 -130.1(4) . . . . ? Li2 Li3 Li4 C26 177.1(3) . . . . ? Li1 Li3 Li4 C26 -137.9(2) . . . . ? N10 Li3 Li4 C11 177.4(3) . . . . ? N7 Li3 Li4 C11 98.4(3) . . . . ? N5 Li3 Li4 C11 -49.4(3) . . . . ? N4 Li3 Li4 C11 -1.71(16) . . . . ? C2 Li3 Li4 C11 -29.7(2) . . . . ? C25 Li3 Li4 C11 81.3(4) . . . . ? Li2 Li3 Li4 C11 28.4(3) . . . . ? Li1 Li3 Li4 C11 73.4(2) . . . . ? N10 Li3 Li4 N4 179.1(3) . . . . ? N7 Li3 Li4 N4 100.1(3) . . . . ? N5 Li3 Li4 N4 -47.6(2) . . . . ? C2 Li3 Li4 N4 -27.98(14) . . . . ? C25 Li3 Li4 N4 83.0(4) . . . . ? Li2 Li3 Li4 N4 30.1(2) . . . . ? Li1 Li3 Li4 N4 75.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.230 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.049 data_complex2 _database_code_depnum_ccdc_archive 'CCDC 909530' #TrackingRef '909530.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H52 Cl N6 O2 Yb' _chemical_formula_sum 'C32 H52 Cl N6 O2 Yb' _chemical_formula_weight 761.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.8453(6) _cell_length_b 12.2986(4) _cell_length_c 20.3408(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.541(4) _cell_angle_gamma 90.00 _cell_volume 3457.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3738 _cell_measurement_theta_min 4.4310 _cell_measurement_theta_max 29.0540 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1556 _exptl_absorpt_coefficient_mu 2.819 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.54271 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3818 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6650 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_unetI/netI 0.0464 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.49 _reflns_number_total 3148 _reflns_number_gt 2859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3148 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0777 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.5000 0.686710(17) 0.7500 0.03651(11) Uani 1 2 d S . . Cl1 Cl 0.5000 0.89909(12) 0.7500 0.0570(4) Uani 1 2 d S . . O1 O 0.6684(2) 0.6824(2) 0.74650(16) 0.0481(7) Uani 1 1 d . . . N1 N 0.4921(2) 0.5372(2) 0.68326(15) 0.0391(8) Uani 1 1 d . . . N2 N 0.4815(3) 0.6960(2) 0.63143(19) 0.0449(8) Uani 1 1 d . . . N3 N 0.4267(3) 0.5392(3) 0.57138(18) 0.0513(10) Uani 1 1 d . . . H3 H 0.412(3) 0.577(4) 0.539(2) 0.062 Uiso 1 1 d . . . C1 C 0.4672(3) 0.5907(3) 0.62689(19) 0.0391(9) Uani 1 1 d . . . C2 C 0.5146(3) 0.4263(3) 0.68888(19) 0.0370(9) Uani 1 1 d . . . C3 C 0.5467(3) 0.3658(3) 0.6366(2) 0.0490(10) Uani 1 1 d . . . H3A H 0.5636 0.4019 0.5982 0.059 Uiso 1 1 calc R . . C4 C 0.5544(3) 0.2523(4) 0.6400(2) 0.0517(11) Uani 1 1 d . . . H4 H 0.5779 0.2137 0.6044 0.062 Uiso 1 1 calc R . . C5 C 0.5283(3) 0.1973(3) 0.6941(3) 0.0493(11) Uani 1 1 d . . . H5 H 0.5291 0.1209 0.6941 0.059 Uiso 1 1 calc R . . C6 C 0.5000 0.2536(4) 0.7500 0.0412(13) Uani 1 2 d S . . C7 C 0.5000 0.3714(4) 0.7500 0.0345(12) Uani 1 2 d S . . C8 C 0.4418(4) 0.7713(4) 0.5809(2) 0.0564(12) Uani 1 1 d . . . H8 H 0.4310 0.7311 0.5389 0.068 Uiso 1 1 calc R . . C9 C 0.5155(5) 0.8623(4) 0.5712(3) 0.0773(16) Uani 1 1 d . . . H9A H 0.5314 0.8979 0.6130 0.116 Uiso 1 1 calc R . . H9B H 0.4879 0.9149 0.5399 0.116 Uiso 1 1 calc R . . H9C H 0.5737 0.8314 0.5546 0.116 Uiso 1 1 calc R . . C10 C 0.3451(4) 0.8175(4) 0.6002(3) 0.0790(18) Uani 1 1 d . . . H10A H 0.2986 0.7590 0.6028 0.119 Uiso 1 1 calc R . . H10B H 0.3215 0.8699 0.5673 0.119 Uiso 1 1 calc R . . H10C H 0.3539 0.8531 0.6427 0.119 Uiso 1 1 calc R . . C11 C 0.3468(3) 0.4627(4) 0.5743(2) 0.0569(12) Uani 1 1 d . . . H11 H 0.3593 0.4157 0.6134 0.068 Uiso 1 1 calc R . . C12 C 0.2511(4) 0.5198(5) 0.5805(4) 0.096(2) Uani 1 1 d . . . H12A H 0.2550 0.5656 0.6194 0.143 Uiso 1 1 calc R . . H12B H 0.2004 0.4662 0.5843 0.143 Uiso 1 1 calc R . . H12C H 0.2366 0.5644 0.5418 0.143 Uiso 1 1 calc R . . C13 C 0.3436(5) 0.3917(6) 0.5136(3) 0.111(3) Uani 1 1 d . . . H13A H 0.3357 0.4369 0.4745 0.166 Uiso 1 1 calc R . . H13B H 0.2896 0.3416 0.5146 0.166 Uiso 1 1 calc R . . H13C H 0.4035 0.3509 0.5126 0.166 Uiso 1 1 calc R . . C14 C 0.7237(3) 0.5842(4) 0.7390(3) 0.0630(13) Uani 1 1 d . . . H14A H 0.6822 0.5201 0.7423 0.076 Uiso 1 1 calc R . . H14B H 0.7763 0.5796 0.7734 0.076 Uiso 1 1 calc R . . C15 C 0.7633(4) 0.5894(5) 0.6734(3) 0.0774(16) Uani 1 1 d . . . H15A H 0.7225 0.5484 0.6410 0.093 Uiso 1 1 calc R . . H15B H 0.8290 0.5597 0.6747 0.093 Uiso 1 1 calc R . . C16 C 0.7634(4) 0.7095(4) 0.6562(3) 0.0692(15) Uani 1 1 d . . . H16A H 0.8289 0.7345 0.6485 0.083 Uiso 1 1 calc R . . H16B H 0.7210 0.7241 0.6168 0.083 Uiso 1 1 calc R . . C17 C 0.7259(3) 0.7646(4) 0.7156(3) 0.0597(13) Uani 1 1 d . . . H17A H 0.7795 0.7887 0.7458 0.072 Uiso 1 1 calc R . . H17B H 0.6860 0.8277 0.7025 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.05137(17) 0.01988(14) 0.03760(17) 0.000 -0.00276(10) 0.000 Cl1 0.0823(11) 0.0233(7) 0.0641(11) 0.000 -0.0059(8) 0.000 O1 0.0495(16) 0.0359(17) 0.059(2) 0.0048(13) 0.0039(14) -0.0021(13) N1 0.064(2) 0.0231(16) 0.0304(18) 0.0004(13) 0.0016(14) -0.0040(15) N2 0.063(2) 0.0291(18) 0.042(2) 0.0078(14) -0.0031(16) -0.0019(15) N3 0.078(3) 0.045(2) 0.030(2) 0.0040(16) -0.0033(17) -0.0191(19) C1 0.049(2) 0.034(2) 0.035(2) -0.0016(17) 0.0049(16) -0.0024(18) C2 0.046(2) 0.0238(19) 0.041(2) -0.0045(17) 0.0015(16) -0.0054(17) C3 0.064(3) 0.038(2) 0.046(3) -0.006(2) 0.009(2) -0.003(2) C4 0.061(3) 0.037(2) 0.058(3) -0.015(2) 0.005(2) 0.004(2) C5 0.056(3) 0.024(2) 0.067(3) -0.009(2) -0.002(2) 0.0010(18) C6 0.043(3) 0.024(3) 0.056(4) 0.000 -0.004(3) 0.000 C7 0.040(3) 0.019(3) 0.044(3) 0.000 0.005(2) 0.000 C8 0.088(3) 0.039(2) 0.041(3) 0.012(2) -0.011(2) -0.005(2) C9 0.120(4) 0.046(3) 0.065(4) 0.025(3) 0.000(3) -0.018(3) C10 0.089(4) 0.055(3) 0.089(5) 0.020(3) -0.025(3) 0.015(3) C11 0.072(3) 0.051(3) 0.046(3) 0.002(2) -0.009(2) -0.022(2) C12 0.072(4) 0.093(5) 0.118(6) 0.018(4) -0.022(3) -0.020(3) C13 0.162(6) 0.099(5) 0.072(4) -0.038(4) 0.015(4) -0.081(5) C14 0.055(3) 0.042(3) 0.091(4) 0.010(3) 0.004(2) 0.001(2) C15 0.090(4) 0.058(3) 0.086(4) -0.009(3) 0.017(3) -0.002(3) C16 0.068(3) 0.068(3) 0.073(4) 0.015(3) 0.015(3) 0.003(3) C17 0.054(3) 0.036(2) 0.089(4) 0.007(3) 0.002(2) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N1 2.284(3) . ? Yb1 N1 2.284(3) 2_656 ? Yb1 O1 2.337(3) 2_656 ? Yb1 O1 2.337(3) . ? Yb1 N2 2.412(4) 2_656 ? Yb1 N2 2.412(4) . ? Yb1 Cl1 2.6120(14) . ? Yb1 C1 2.780(4) . ? Yb1 C1 2.780(4) 2_656 ? O1 C14 1.444(5) . ? O1 C17 1.453(5) . ? N1 C1 1.349(5) . ? N1 C2 1.402(5) . ? N2 C1 1.313(5) . ? N2 C8 1.465(5) . ? N3 C1 1.383(5) . ? N3 C11 1.455(6) . ? N3 H3 0.81(5) . ? C2 C3 1.393(6) . ? C2 C7 1.440(5) . ? C3 C4 1.401(7) . ? C3 H3A 0.9400 . ? C4 C5 1.360(7) . ? C4 H4 0.9400 . ? C5 C6 1.407(6) . ? C5 H5 0.9400 . ? C6 C5 1.407(6) 2_656 ? C6 C7 1.450(8) . ? C7 C2 1.440(5) 2_656 ? C8 C10 1.527(8) . ? C8 C9 1.535(7) . ? C8 H8 0.9900 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C13 1.511(7) . ? C11 C12 1.512(8) . ? C11 H11 0.9900 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 C15 1.476(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.518(7) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C17 1.506(8) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Yb1 N1 72.78(15) . 2_656 ? N1 Yb1 O1 89.37(11) . 2_656 ? N1 Yb1 O1 88.55(11) 2_656 2_656 ? N1 Yb1 O1 88.55(11) . . ? N1 Yb1 O1 89.37(10) 2_656 . ? O1 Yb1 O1 177.41(12) 2_656 . ? N1 Yb1 N2 129.10(10) . 2_656 ? N1 Yb1 N2 56.35(10) 2_656 2_656 ? O1 Yb1 N2 90.86(12) 2_656 2_656 ? O1 Yb1 N2 89.26(12) . 2_656 ? N1 Yb1 N2 56.35(10) . . ? N1 Yb1 N2 129.10(10) 2_656 . ? O1 Yb1 N2 89.26(12) 2_656 . ? O1 Yb1 N2 90.86(12) . . ? N2 Yb1 N2 174.55(14) 2_656 . ? N1 Yb1 Cl1 143.61(8) . . ? N1 Yb1 Cl1 143.61(8) 2_656 . ? O1 Yb1 Cl1 91.29(6) 2_656 . ? O1 Yb1 Cl1 91.29(6) . . ? N2 Yb1 Cl1 87.27(7) 2_656 . ? N2 Yb1 Cl1 87.27(7) . . ? N1 Yb1 C1 28.81(11) . . ? N1 Yb1 C1 101.10(11) 2_656 . ? O1 Yb1 C1 84.83(11) 2_656 . ? O1 Yb1 C1 94.07(11) . . ? N2 Yb1 C1 157.22(12) 2_656 . ? N2 Yb1 C1 28.16(10) . . ? Cl1 Yb1 C1 115.13(8) . . ? N1 Yb1 C1 101.10(11) . 2_656 ? N1 Yb1 C1 28.81(11) 2_656 2_656 ? O1 Yb1 C1 94.07(11) 2_656 2_656 ? O1 Yb1 C1 84.83(11) . 2_656 ? N2 Yb1 C1 28.16(10) 2_656 2_656 ? N2 Yb1 C1 157.22(11) . 2_656 ? Cl1 Yb1 C1 115.13(8) . 2_656 ? C1 Yb1 C1 129.75(17) . 2_656 ? C14 O1 C17 103.2(3) . . ? C14 O1 Yb1 124.0(2) . . ? C17 O1 Yb1 124.9(3) . . ? C1 N1 C2 126.0(3) . . ? C1 N1 Yb1 96.5(2) . . ? C2 N1 Yb1 137.1(2) . . ? C1 N2 C8 121.7(4) . . ? C1 N2 Yb1 91.7(2) . . ? C8 N2 Yb1 138.0(3) . . ? C1 N3 C11 122.3(3) . . ? C1 N3 H3 117(4) . . ? C11 N3 H3 105(3) . . ? N2 C1 N1 113.1(3) . . ? N2 C1 N3 124.2(4) . . ? N1 C1 N3 122.7(4) . . ? N2 C1 Yb1 60.1(2) . . ? N1 C1 Yb1 54.72(18) . . ? N3 C1 Yb1 164.9(3) . . ? C3 C2 N1 122.5(4) . . ? C3 C2 C7 118.5(4) . . ? N1 C2 C7 119.0(3) . . ? C2 C3 C4 121.5(4) . . ? C2 C3 H3A 119.3 . . ? C4 C3 H3A 119.3 . . ? C5 C4 C3 120.8(4) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 120.7(4) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C5 121.1(5) . 2_656 ? C5 C6 C7 119.4(3) . . ? C5 C6 C7 119.4(3) 2_656 . ? C2 C7 C2 124.1(5) 2_656 . ? C2 C7 C6 118.0(2) 2_656 . ? C2 C7 C6 118.0(2) . . ? N2 C8 C10 110.6(4) . . ? N2 C8 C9 109.1(4) . . ? C10 C8 C9 111.2(5) . . ? N2 C8 H8 108.6 . . ? C10 C8 H8 108.6 . . ? C9 C8 H8 108.6 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C13 108.9(4) . . ? N3 C11 C12 112.0(4) . . ? C13 C11 C12 110.8(5) . . ? N3 C11 H11 108.3 . . ? C13 C11 H11 108.3 . . ? C12 C11 H11 108.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O1 C14 C15 106.7(4) . . ? O1 C14 H14A 110.4 . . ? C15 C14 H14A 110.4 . . ? O1 C14 H14B 110.4 . . ? C15 C14 H14B 110.4 . . ? H14A C14 H14B 108.6 . . ? C14 C15 C16 104.8(4) . . ? C14 C15 H15A 110.8 . . ? C16 C15 H15A 110.8 . . ? C14 C15 H15B 110.8 . . ? C16 C15 H15B 110.8 . . ? H15A C15 H15B 108.9 . . ? C17 C16 C15 104.4(4) . . ? C17 C16 H16A 110.9 . . ? C15 C16 H16A 110.9 . . ? C17 C16 H16B 110.9 . . ? C15 C16 H16B 110.9 . . ? H16A C16 H16B 108.9 . . ? O1 C17 C16 105.0(4) . . ? O1 C17 H17A 110.7 . . ? C16 C17 H17A 110.7 . . ? O1 C17 H17B 110.7 . . ? C16 C17 H17B 110.7 . . ? H17A C17 H17B 108.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Yb1 O1 C14 -30.3(3) . . . . ? N1 Yb1 O1 C14 42.5(3) 2_656 . . . ? O1 Yb1 O1 C14 6.1(3) 2_656 . . . ? N2 Yb1 O1 C14 98.9(3) 2_656 . . . ? N2 Yb1 O1 C14 -86.6(3) . . . . ? Cl1 Yb1 O1 C14 -173.9(3) . . . . ? C1 Yb1 O1 C14 -58.5(3) . . . . ? C1 Yb1 O1 C14 71.0(3) 2_656 . . . ? N1 Yb1 O1 C17 113.3(3) . . . . ? N1 Yb1 O1 C17 -173.9(3) 2_656 . . . ? O1 Yb1 O1 C17 149.7(3) 2_656 . . . ? N2 Yb1 O1 C17 -117.5(3) 2_656 . . . ? N2 Yb1 O1 C17 57.0(3) . . . . ? Cl1 Yb1 O1 C17 -30.3(3) . . . . ? C1 Yb1 O1 C17 85.0(3) . . . . ? C1 Yb1 O1 C17 -145.4(4) 2_656 . . . ? N1 Yb1 N1 C1 169.1(3) 2_656 . . . ? O1 Yb1 N1 C1 80.4(2) 2_656 . . . ? O1 Yb1 N1 C1 -101.1(2) . . . . ? N2 Yb1 N1 C1 171.0(2) 2_656 . . . ? N2 Yb1 N1 C1 -9.1(2) . . . . ? Cl1 Yb1 N1 C1 -10.9(3) . . . . ? C1 Yb1 N1 C1 174.42(15) 2_656 . . . ? N1 Yb1 N1 C2 -18.4(3) 2_656 . . . ? O1 Yb1 N1 C2 -107.1(4) 2_656 . . . ? O1 Yb1 N1 C2 71.4(4) . . . . ? N2 Yb1 N1 C2 -16.5(4) 2_656 . . . ? N2 Yb1 N1 C2 163.4(4) . . . . ? Cl1 Yb1 N1 C2 161.6(3) . . . . ? C1 Yb1 N1 C2 172.5(5) . . . . ? C1 Yb1 N1 C2 -13.1(4) 2_656 . . . ? N1 Yb1 N2 C1 9.3(2) . . . . ? N1 Yb1 N2 C1 7.1(3) 2_656 . . . ? O1 Yb1 N2 C1 -80.4(2) 2_656 . . . ? O1 Yb1 N2 C1 97.0(2) . . . . ? N2 Yb1 N2 C1 -171.7(2) 2_656 . . . ? Cl1 Yb1 N2 C1 -171.7(2) . . . . ? C1 Yb1 N2 C1 18.4(5) 2_656 . . . ? N1 Yb1 N2 C8 154.4(5) . . . . ? N1 Yb1 N2 C8 152.2(4) 2_656 . . . ? O1 Yb1 N2 C8 64.6(4) 2_656 . . . ? O1 Yb1 N2 C8 -118.0(4) . . . . ? N2 Yb1 N2 C8 -26.7(4) 2_656 . . . ? Cl1 Yb1 N2 C8 -26.7(4) . . . . ? C1 Yb1 N2 C8 145.0(6) . . . . ? C1 Yb1 N2 C8 163.4(4) 2_656 . . . ? C8 N2 C1 N1 -167.6(4) . . . . ? Yb1 N2 C1 N1 -14.4(3) . . . . ? C8 N2 C1 N3 9.7(7) . . . . ? Yb1 N2 C1 N3 162.9(4) . . . . ? C8 N2 C1 Yb1 -153.2(5) . . . . ? C2 N1 C1 N2 -158.4(4) . . . . ? Yb1 N1 C1 N2 15.3(4) . . . . ? C2 N1 C1 N3 24.3(6) . . . . ? Yb1 N1 C1 N3 -162.0(3) . . . . ? C2 N1 C1 Yb1 -173.7(4) . . . . ? C11 N3 C1 N2 -129.7(5) . . . . ? C11 N3 C1 N1 47.3(6) . . . . ? C11 N3 C1 Yb1 -27.8(14) . . . . ? N1 Yb1 C1 N2 -163.7(4) . . . . ? N1 Yb1 C1 N2 -174.4(2) 2_656 . . . ? O1 Yb1 C1 N2 98.1(3) 2_656 . . . ? O1 Yb1 C1 N2 -84.2(3) . . . . ? N2 Yb1 C1 N2 177.98(8) 2_656 . . . ? Cl1 Yb1 C1 N2 9.1(3) . . . . ? C1 Yb1 C1 N2 -170.9(3) 2_656 . . . ? N1 Yb1 C1 N1 -10.6(3) 2_656 . . . ? O1 Yb1 C1 N1 -98.1(2) 2_656 . . . ? O1 Yb1 C1 N1 79.5(2) . . . . ? N2 Yb1 C1 N1 -18.3(4) 2_656 . . . ? N2 Yb1 C1 N1 163.7(4) . . . . ? Cl1 Yb1 C1 N1 172.9(2) . . . . ? C1 Yb1 C1 N1 -7.1(2) 2_656 . . . ? N1 Yb1 C1 N3 85.3(11) . . . . ? N1 Yb1 C1 N3 74.6(11) 2_656 . . . ? O1 Yb1 C1 N3 -12.9(11) 2_656 . . . ? O1 Yb1 C1 N3 164.8(11) . . . . ? N2 Yb1 C1 N3 67.0(12) 2_656 . . . ? N2 Yb1 C1 N3 -111.0(12) . . . . ? Cl1 Yb1 C1 N3 -101.9(11) . . . . ? C1 Yb1 C1 N3 78.1(11) 2_656 . . . ? C1 N1 C2 C3 23.2(6) . . . . ? Yb1 N1 C2 C3 -147.5(3) . . . . ? C1 N1 C2 C7 -154.0(3) . . . . ? Yb1 N1 C2 C7 35.2(5) . . . . ? N1 C2 C3 C4 -170.0(4) . . . . ? C7 C2 C3 C4 7.3(6) . . . . ? C2 C3 C4 C5 1.7(6) . . . . ? C3 C4 C5 C6 -5.0(7) . . . . ? C4 C5 C6 C5 179.2(5) . . . 2_656 ? C4 C5 C6 C7 -0.8(5) . . . . ? C3 C2 C7 C2 167.5(4) . . . 2_656 ? N1 C2 C7 C2 -15.2(2) . . . 2_656 ? C3 C2 C7 C6 -12.5(4) . . . . ? N1 C2 C7 C6 164.8(2) . . . . ? C5 C6 C7 C2 -170.5(3) . . . 2_656 ? C5 C6 C7 C2 9.5(3) 2_656 . . 2_656 ? C5 C6 C7 C2 9.5(3) . . . . ? C5 C6 C7 C2 -170.5(3) 2_656 . . . ? C1 N2 C8 C10 94.9(5) . . . . ? Yb1 N2 C8 C10 -42.7(6) . . . . ? C1 N2 C8 C9 -142.4(5) . . . . ? Yb1 N2 C8 C9 80.0(6) . . . . ? C1 N3 C11 C13 -159.4(5) . . . . ? C1 N3 C11 C12 77.6(6) . . . . ? C17 O1 C14 C15 -38.4(5) . . . . ? Yb1 O1 C14 C15 111.6(4) . . . . ? O1 C14 C15 C16 22.4(6) . . . . ? C14 C15 C16 C17 1.7(6) . . . . ? C14 O1 C17 C16 38.9(5) . . . . ? Yb1 O1 C17 C16 -110.7(4) . . . . ? C15 C16 C17 O1 -24.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.302 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.093 data_complex3 _database_code_depnum_ccdc_archive 'CCDC 909531' #TrackingRef '909531.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H52 Cl N6 O2 Y' _chemical_formula_sum 'C32 H52 Cl N6 O2 Y' _chemical_formula_weight 677.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.835(5) _cell_length_b 12.374(5) _cell_length_c 20.243(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.448(10) _cell_angle_gamma 90.00 _cell_volume 3459(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4772 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 1.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.248 _exptl_absorpt_correction_T_max 0.484 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8940 _diffrn_reflns_av_R_equivalents 0.0787 _diffrn_reflns_av_unetI/netI 0.1240 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.49 _reflns_number_total 3201 _reflns_number_gt 1862 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1110P)^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 0.0040(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3201 _refine_ls_number_parameters 189 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_gt 0.0717 _refine_ls_wR_factor_ref 0.2126 _refine_ls_wR_factor_gt 0.1750 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.5000 0.69056(6) 0.7500 0.0373(3) Uani 1 2 d S . . Cl1 Cl 0.5000 0.90579(18) 0.7500 0.0563(6) Uani 1 2 d S . . O1 O 0.6704(3) 0.6850(3) 0.74622(19) 0.0446(10) Uani 1 1 d . . . N1 N 0.4926(3) 0.5386(4) 0.68354(19) 0.0384(11) Uani 1 1 d . . . N2 N 0.4812(3) 0.6960(4) 0.6297(2) 0.0393(11) Uani 1 1 d . . . N3 N 0.4261(4) 0.5397(4) 0.5710(2) 0.0501(13) Uani 1 1 d D . . H3 H 0.412(4) 0.580(4) 0.543(2) 0.060 Uiso 1 1 d D . . C1 C 0.4667(4) 0.5920(5) 0.6264(3) 0.0437(14) Uani 1 1 d . . . C2 C 0.5133(4) 0.4297(5) 0.6886(2) 0.0362(12) Uani 1 1 d . . . C3 C 0.5484(4) 0.3693(5) 0.6375(3) 0.0460(15) Uani 1 1 d . . . H3A H 0.5682 0.4053 0.5997 0.055 Uiso 1 1 calc R . . C4 C 0.5552(4) 0.2554(5) 0.6402(3) 0.0462(14) Uani 1 1 d . . . H4 H 0.5789 0.2175 0.6044 0.055 Uiso 1 1 calc R . . C5 C 0.5278(4) 0.1998(5) 0.6944(3) 0.0469(15) Uani 1 1 d . . . H5 H 0.5275 0.1239 0.6945 0.056 Uiso 1 1 calc R . . C6 C 0.5000 0.2579(7) 0.7500 0.0401(18) Uani 1 2 d S . . C7 C 0.5000 0.3741(6) 0.7500 0.0317(17) Uani 1 2 d S . . C8 C 0.4413(5) 0.7710(6) 0.5792(3) 0.0564(17) Uani 1 1 d . . . H8 H 0.4314 0.7314 0.5368 0.068 Uiso 1 1 calc R . . C9 C 0.5127(6) 0.8619(7) 0.5700(4) 0.084(2) Uani 1 1 d . . . H9A H 0.5238 0.9007 0.6114 0.125 Uiso 1 1 calc R . . H9B H 0.4865 0.9110 0.5362 0.125 Uiso 1 1 calc R . . H9C H 0.5734 0.8321 0.5567 0.125 Uiso 1 1 calc R . . C10 C 0.3436(6) 0.8157(6) 0.5982(4) 0.075(2) Uani 1 1 d . . . H10A H 0.3010 0.7563 0.6079 0.112 Uiso 1 1 calc R . . H10B H 0.3146 0.8579 0.5618 0.112 Uiso 1 1 calc R . . H10C H 0.3533 0.8613 0.6370 0.112 Uiso 1 1 calc R . . C11 C 0.3466(6) 0.4625(7) 0.5739(4) 0.0786(14) Uani 1 1 d . . . H11 H 0.3602 0.4157 0.6130 0.094 Uiso 1 1 calc R . . C12 C 0.2496(5) 0.5181(7) 0.5817(3) 0.0786(14) Uani 1 1 d . . . H12A H 0.2572 0.5735 0.6155 0.118 Uiso 1 1 calc R . . H12B H 0.2025 0.4653 0.5945 0.118 Uiso 1 1 calc R . . H12C H 0.2275 0.5511 0.5400 0.118 Uiso 1 1 calc R . . C13 C 0.3420(5) 0.3925(7) 0.5140(3) 0.0786(14) Uani 1 1 d . . . H13A H 0.3483 0.4367 0.4749 0.118 Uiso 1 1 calc R . . H13B H 0.2804 0.3548 0.5105 0.118 Uiso 1 1 calc R . . H13C H 0.3943 0.3402 0.5175 0.118 Uiso 1 1 calc R . . C14 C 0.7252(4) 0.5877(6) 0.7389(3) 0.0592(18) Uani 1 1 d . . . H14A H 0.6839 0.5240 0.7430 0.071 Uiso 1 1 calc R . . H14B H 0.7788 0.5837 0.7727 0.071 Uiso 1 1 calc R . . C15 C 0.7623(6) 0.5934(8) 0.6722(4) 0.082(2) Uani 1 1 d . . . H15A H 0.7198 0.5533 0.6404 0.099 Uiso 1 1 calc R . . H15B H 0.8275 0.5625 0.6723 0.099 Uiso 1 1 calc R . . C16 C 0.7640(5) 0.7099(7) 0.6544(4) 0.070(2) Uani 1 1 d . . . H16A H 0.7223 0.7240 0.6144 0.084 Uiso 1 1 calc R . . H16B H 0.8301 0.7334 0.6466 0.084 Uiso 1 1 calc R . . C17 C 0.7264(5) 0.7675(6) 0.7136(4) 0.0633(19) Uani 1 1 d . . . H17A H 0.7799 0.7939 0.7432 0.076 Uiso 1 1 calc R . . H17B H 0.6852 0.8288 0.6996 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0453(5) 0.0245(5) 0.0412(5) 0.000 -0.0060(3) 0.000 Cl1 0.0804(15) 0.0234(12) 0.0636(13) 0.000 -0.0086(11) 0.000 O1 0.042(2) 0.037(3) 0.054(2) 0.0030(18) -0.0023(17) -0.0016(18) N1 0.051(3) 0.027(3) 0.037(2) 0.002(2) -0.0019(19) -0.001(2) N2 0.059(3) 0.026(3) 0.032(2) 0.0047(19) -0.007(2) -0.005(2) N3 0.079(3) 0.036(3) 0.033(2) 0.003(2) -0.010(2) -0.015(3) C1 0.048(3) 0.038(4) 0.044(3) 0.013(3) -0.003(2) -0.007(3) C2 0.038(3) 0.022(3) 0.048(3) -0.006(2) -0.001(2) -0.009(2) C3 0.058(4) 0.036(4) 0.046(3) -0.007(3) 0.011(3) -0.006(3) C4 0.057(4) 0.031(4) 0.051(3) -0.014(3) 0.003(3) 0.008(3) C5 0.044(3) 0.032(4) 0.063(4) -0.012(3) -0.009(3) 0.004(3) C6 0.035(4) 0.030(5) 0.054(4) 0.000 -0.007(3) 0.000 C7 0.031(4) 0.027(5) 0.036(4) 0.000 -0.004(3) 0.000 C8 0.082(5) 0.031(4) 0.055(4) 0.003(3) -0.010(3) -0.008(3) C9 0.112(6) 0.064(6) 0.074(5) 0.031(4) 0.002(4) -0.016(5) C10 0.082(5) 0.064(6) 0.076(5) 0.017(4) -0.022(4) 0.007(4) C11 0.090(3) 0.071(4) 0.075(3) -0.009(2) 0.001(2) -0.031(3) C12 0.090(3) 0.071(4) 0.075(3) -0.009(2) 0.001(2) -0.031(3) C13 0.090(3) 0.071(4) 0.075(3) -0.009(2) 0.001(2) -0.031(3) C14 0.049(4) 0.046(5) 0.082(5) -0.001(3) -0.002(3) 0.004(3) C15 0.086(5) 0.084(7) 0.077(5) -0.017(5) 0.008(4) 0.006(5) C16 0.060(4) 0.084(7) 0.068(4) 0.015(4) 0.009(3) -0.013(4) C17 0.051(4) 0.052(5) 0.087(5) 0.002(4) 0.000(3) -0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N1 2.311(5) . ? Y1 N1 2.311(5) 2_656 ? Y1 O1 2.365(4) 2_656 ? Y1 O1 2.365(4) . ? Y1 N2 2.433(4) . ? Y1 N2 2.433(4) 2_656 ? Y1 Cl1 2.663(3) . ? Y1 C1 2.797(6) . ? Y1 C1 2.797(6) 2_656 ? O1 C14 1.435(7) . ? O1 C17 1.463(8) . ? N1 C1 1.362(6) . ? N1 C2 1.379(7) . ? N2 C1 1.304(7) . ? N2 C8 1.465(7) . ? N3 C1 1.384(7) . ? N3 C11 1.460(9) . ? N3 H3 0.772(10) . ? C2 C3 1.388(7) . ? C2 C7 1.442(6) . ? C3 C4 1.412(9) . ? C3 H3A 0.9400 . ? C4 C5 1.367(9) . ? C4 H4 0.9400 . ? C5 C6 1.409(7) . ? C5 H5 0.9400 . ? C6 C5 1.409(7) 2_656 ? C6 C7 1.438(12) . ? C7 C2 1.442(6) 2_656 ? C8 C9 1.515(10) . ? C8 C10 1.532(11) . ? C8 H8 0.9900 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C13 1.489(9) . ? C11 C12 1.525(11) . ? C11 H11 0.9900 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 C15 1.475(9) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.487(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C17 1.515(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Y1 N1 71.1(2) . 2_656 ? N1 Y1 O1 89.19(14) . 2_656 ? N1 Y1 O1 88.09(14) 2_656 2_656 ? N1 Y1 O1 88.09(14) . . ? N1 Y1 O1 89.19(14) 2_656 . ? O1 Y1 O1 176.65(19) 2_656 . ? N1 Y1 N2 56.07(15) . . ? N1 Y1 N2 127.10(15) 2_656 . ? O1 Y1 N2 89.23(15) 2_656 . ? O1 Y1 N2 90.86(15) . . ? N1 Y1 N2 127.10(15) . 2_656 ? N1 Y1 N2 56.07(15) 2_656 2_656 ? O1 Y1 N2 90.86(15) 2_656 2_656 ? O1 Y1 N2 89.23(15) . 2_656 ? N2 Y1 N2 176.8(2) . 2_656 ? N1 Y1 Cl1 144.47(10) . . ? N1 Y1 Cl1 144.47(10) 2_656 . ? O1 Y1 Cl1 91.68(10) 2_656 . ? O1 Y1 Cl1 91.68(10) . . ? N2 Y1 Cl1 88.42(11) . . ? N2 Y1 Cl1 88.42(11) 2_656 . ? N1 Y1 C1 28.98(16) . . ? N1 Y1 C1 99.50(17) 2_656 . ? O1 Y1 C1 84.56(15) 2_656 . ? O1 Y1 C1 93.98(15) . . ? N2 Y1 C1 27.77(14) . . ? N2 Y1 C1 155.36(18) 2_656 . ? Cl1 Y1 C1 115.85(12) . . ? N1 Y1 C1 99.50(16) . 2_656 ? N1 Y1 C1 28.98(16) 2_656 2_656 ? O1 Y1 C1 93.98(15) 2_656 2_656 ? O1 Y1 C1 84.56(15) . 2_656 ? N2 Y1 C1 155.36(18) . 2_656 ? N2 Y1 C1 27.77(14) 2_656 2_656 ? Cl1 Y1 C1 115.85(12) . 2_656 ? C1 Y1 C1 128.3(2) . 2_656 ? C14 O1 C17 104.1(5) . . ? C14 O1 Y1 124.2(4) . . ? C17 O1 Y1 123.3(4) . . ? C1 N1 C2 125.4(5) . . ? C1 N1 Y1 95.7(4) . . ? C2 N1 Y1 138.5(3) . . ? C1 N2 C8 122.6(5) . . ? C1 N2 Y1 91.8(3) . . ? C8 N2 Y1 136.9(4) . . ? C1 N3 C11 122.9(5) . . ? C1 N3 H3 112(5) . . ? C11 N3 H3 107(5) . . ? N2 C1 N1 113.7(5) . . ? N2 C1 N3 123.9(5) . . ? N1 C1 N3 122.3(6) . . ? N2 C1 Y1 60.4(3) . . ? N1 C1 Y1 55.3(3) . . ? N3 C1 Y1 165.0(4) . . ? N1 C2 C3 123.4(5) . . ? N1 C2 C7 119.6(5) . . ? C3 C2 C7 117.0(6) . . ? C2 C3 C4 122.3(5) . . ? C2 C3 H3A 118.9 . . ? C4 C3 H3A 118.9 . . ? C5 C4 C3 120.8(5) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 119.1(6) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C5 C6 C5 118.7(8) . 2_656 ? C5 C6 C7 120.7(4) . . ? C5 C6 C7 120.7(4) 2_656 . ? C6 C7 C2 118.5(3) . . ? C6 C7 C2 118.5(3) . 2_656 ? C2 C7 C2 123.0(7) . 2_656 ? N2 C8 C9 109.6(5) . . ? N2 C8 C10 110.7(5) . . ? C9 C8 C10 110.7(7) . . ? N2 C8 H8 108.6 . . ? C9 C8 H8 108.6 . . ? C10 C8 H8 108.6 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C13 110.1(6) . . ? N3 C11 C12 112.2(7) . . ? C13 C11 C12 110.7(6) . . ? N3 C11 H11 107.9 . . ? C13 C11 H11 107.9 . . ? C12 C11 H11 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O1 C14 C15 105.6(6) . . ? O1 C14 H14A 110.6 . . ? C15 C14 H14A 110.6 . . ? O1 C14 H14B 110.6 . . ? C15 C14 H14B 110.6 . . ? H14A C14 H14B 108.7 . . ? C14 C15 C16 106.3(6) . . ? C14 C15 H15A 110.5 . . ? C16 C15 H15A 110.5 . . ? C14 C15 H15B 110.5 . . ? C16 C15 H15B 110.5 . . ? H15A C15 H15B 108.7 . . ? C15 C16 C17 104.7(6) . . ? C15 C16 H16A 110.8 . . ? C17 C16 H16A 110.8 . . ? C15 C16 H16B 110.8 . . ? C17 C16 H16B 110.8 . . ? H16A C16 H16B 108.9 . . ? O1 C17 C16 104.2(6) . . ? O1 C17 H17A 110.9 . . ? C16 C17 H17A 110.9 . . ? O1 C17 H17B 110.9 . . ? C16 C17 H17B 110.9 . . ? H17A C17 H17B 108.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Y1 O1 C14 -29.6(4) . . . . ? N1 Y1 O1 C14 41.5(4) 2_656 . . . ? O1 Y1 O1 C14 5.9(4) 2_656 . . . ? N2 Y1 O1 C14 -85.6(4) . . . . ? N2 Y1 O1 C14 97.6(4) 2_656 . . . ? Cl1 Y1 O1 C14 -174.1(4) . . . . ? C1 Y1 O1 C14 -58.0(4) . . . . ? C1 Y1 O1 C14 70.1(4) 2_656 . . . ? N1 Y1 O1 C17 113.3(4) . . . . ? N1 Y1 O1 C17 -175.6(4) 2_656 . . . ? O1 Y1 O1 C17 148.9(4) 2_656 . . . ? N2 Y1 O1 C17 57.3(4) . . . . ? N2 Y1 O1 C17 -119.5(4) 2_656 . . . ? Cl1 Y1 O1 C17 -31.1(4) . . . . ? C1 Y1 O1 C17 84.9(5) . . . . ? C1 Y1 O1 C17 -147.0(5) 2_656 . . . ? N1 Y1 N1 C1 168.5(4) 2_656 . . . ? O1 Y1 N1 C1 80.2(3) 2_656 . . . ? O1 Y1 N1 C1 -101.7(3) . . . . ? N2 Y1 N1 C1 -9.4(3) . . . . ? N2 Y1 N1 C1 170.7(3) 2_656 . . . ? Cl1 Y1 N1 C1 -11.5(4) . . . . ? C1 Y1 N1 C1 174.1(2) 2_656 . . . ? N1 Y1 N1 C2 -17.8(4) 2_656 . . . ? O1 Y1 N1 C2 -106.0(5) 2_656 . . . ? O1 Y1 N1 C2 72.0(5) . . . . ? N2 Y1 N1 C2 164.3(6) . . . . ? N2 Y1 N1 C2 -15.6(6) 2_656 . . . ? Cl1 Y1 N1 C2 162.2(4) . . . . ? C1 Y1 N1 C2 173.8(7) . . . . ? C1 Y1 N1 C2 -12.1(5) 2_656 . . . ? N1 Y1 N2 C1 9.8(3) . . . . ? N1 Y1 N2 C1 7.3(4) 2_656 . . . ? O1 Y1 N2 C1 -79.7(4) 2_656 . . . ? O1 Y1 N2 C1 96.9(4) . . . . ? N2 Y1 N2 C1 -171.4(3) 2_656 . . . ? Cl1 Y1 N2 C1 -171.4(3) . . . . ? C1 Y1 N2 C1 18.1(7) 2_656 . . . ? N1 Y1 N2 C8 155.0(6) . . . . ? N1 Y1 N2 C8 152.5(5) 2_656 . . . ? O1 Y1 N2 C8 65.5(6) 2_656 . . . ? O1 Y1 N2 C8 -117.8(6) . . . . ? N2 Y1 N2 C8 -26.2(6) 2_656 . . . ? Cl1 Y1 N2 C8 -26.2(6) . . . . ? C1 Y1 N2 C8 145.2(8) . . . . ? C1 Y1 N2 C8 163.4(5) 2_656 . . . ? C8 N2 C1 N1 -167.6(5) . . . . ? Y1 N2 C1 N1 -15.2(5) . . . . ? C8 N2 C1 N3 10.6(9) . . . . ? Y1 N2 C1 N3 163.0(5) . . . . ? C8 N2 C1 Y1 -152.5(6) . . . . ? C2 N1 C1 N2 -158.9(5) . . . . ? Y1 N1 C1 N2 16.1(5) . . . . ? C2 N1 C1 N3 22.9(8) . . . . ? Y1 N1 C1 N3 -162.2(5) . . . . ? C2 N1 C1 Y1 -174.9(6) . . . . ? C11 N3 C1 N2 -130.7(7) . . . . ? C11 N3 C1 N1 47.3(9) . . . . ? C11 N3 C1 Y1 -29(2) . . . . ? N1 Y1 C1 N2 -163.1(6) . . . . ? N1 Y1 C1 N2 -174.1(3) 2_656 . . . ? O1 Y1 C1 N2 98.7(4) 2_656 . . . ? O1 Y1 C1 N2 -84.3(4) . . . . ? N2 Y1 C1 N2 178.87(9) 2_656 . . . ? Cl1 Y1 C1 N2 9.5(4) . . . . ? C1 Y1 C1 N2 -170.5(4) 2_656 . . . ? N1 Y1 C1 N1 -11.1(4) 2_656 . . . ? O1 Y1 C1 N1 -98.2(3) 2_656 . . . ? O1 Y1 C1 N1 78.8(3) . . . . ? N2 Y1 C1 N1 163.1(6) . . . . ? N2 Y1 C1 N1 -18.1(6) 2_656 . . . ? Cl1 Y1 C1 N1 172.6(3) . . . . ? C1 Y1 C1 N1 -7.4(3) 2_656 . . . ? N1 Y1 C1 N3 85.9(17) . . . . ? N1 Y1 C1 N3 74.9(17) 2_656 . . . ? O1 Y1 C1 N3 -12.3(17) 2_656 . . . ? O1 Y1 C1 N3 164.7(17) . . . . ? N2 Y1 C1 N3 -111.0(18) . . . . ? N2 Y1 C1 N3 67.8(18) 2_656 . . . ? Cl1 Y1 C1 N3 -101.5(17) . . . . ? C1 Y1 C1 N3 78.5(17) 2_656 . . . ? C1 N1 C2 C3 27.0(8) . . . . ? Y1 N1 C2 C3 -145.4(4) . . . . ? C1 N1 C2 C7 -154.0(4) . . . . ? Y1 N1 C2 C7 33.6(7) . . . . ? N1 C2 C3 C4 -170.2(5) . . . . ? C7 C2 C3 C4 10.7(7) . . . . ? C2 C3 C4 C5 -0.5(8) . . . . ? C3 C4 C5 C6 -5.2(8) . . . . ? C4 C5 C6 C5 -179.8(6) . . . 2_656 ? C4 C5 C6 C7 0.2(6) . . . . ? C5 C6 C7 C2 10.1(3) . . . . ? C5 C6 C7 C2 -169.9(3) 2_656 . . . ? C5 C6 C7 C2 -169.9(3) . . . 2_656 ? C5 C6 C7 C2 10.1(3) 2_656 . . 2_656 ? N1 C2 C7 C6 165.7(3) . . . . ? C3 C2 C7 C6 -15.2(5) . . . . ? N1 C2 C7 C2 -14.3(3) . . . 2_656 ? C3 C2 C7 C2 164.8(5) . . . 2_656 ? C1 N2 C8 C9 -144.4(6) . . . . ? Y1 N2 C8 C9 78.1(8) . . . . ? C1 N2 C8 C10 93.1(7) . . . . ? Y1 N2 C8 C10 -44.3(8) . . . . ? C1 N3 C11 C13 -160.0(6) . . . . ? C1 N3 C11 C12 76.3(8) . . . . ? C17 O1 C14 C15 -38.2(7) . . . . ? Y1 O1 C14 C15 110.5(5) . . . . ? O1 C14 C15 C16 23.5(7) . . . . ? C14 C15 C16 C17 -0.2(8) . . . . ? C14 O1 C17 C16 37.6(6) . . . . ? Y1 O1 C17 C16 -111.5(5) . . . . ? C15 C16 C17 O1 -22.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.877 _refine_diff_density_min -1.520 _refine_diff_density_rms 0.118 data_complex4 _database_code_depnum_ccdc_archive 'CCDC 909532' #TrackingRef '909532.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H86 N12 O2 Yb2, 5(C4 H8 O)' _chemical_formula_sum 'C76 H126 N12 O7 Yb2' _chemical_formula_weight 1665.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.103(7) _cell_length_b 18.045(5) _cell_length_c 16.717(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.444(7) _cell_angle_gamma 90.00 _cell_volume 7881(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 18054 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3448 _exptl_absorpt_coefficient_mu 2.417 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.308 _exptl_absorpt_correction_T_max 0.431 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32764 _diffrn_reflns_av_R_equivalents 0.0827 _diffrn_reflns_av_unetI/netI 0.0787 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7308 _reflns_number_gt 6230 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Their C41-C42,C42-C43,C43- C44,O5-C41,O5-C44,C37-C38,C38-C39,C39-C40,O4-C37,O4-C40,C33-C34,C34-C35,C35 -C36,O3-C33,O3-C36,C29'-C30',C30'-C31',C31'-C32',O2'-C29',O2'-C32',C29-C30, C30-C31,C31-C32,O2-C29 and O2-C32 distances were constrained. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+146.0644P] 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 7308 _refine_ls_number_parameters 405 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0923 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.1702 _refine_ls_wR_factor_gt 0.1459 _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_restrained_S_all 1.188 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.248391(16) 0.15520(2) 0.43099(3) 0.02725(15) Uani 1 1 d . . . O1 O 0.2019(3) 0.1320(4) 0.2938(4) 0.0389(17) Uani 1 1 d . . . O2 O 0.4016(18) 0.848(4) 0.464(4) 0.102(3) Uiso 0.50 1 d PD A 1 O2' O 0.3988(18) 0.844(4) 0.463(4) 0.102(3) Uiso 0.50 1 d PD B 2 O3 O 1.0198(7) 0.1303(11) 0.2491(14) 0.092(4) Uiso 0.50 1 d PD . 1 O4 O 0.0166(18) 0.417(2) 0.237(4) 0.207(13) Uiso 0.50 1 d PD . 1 O5 O 0.0312(13) 0.8106(19) 0.258(2) 0.149(8) Uiso 0.50 1 d PD . 1 N1 N 0.1825(3) 0.1526(4) 0.4932(5) 0.0302(18) Uani 1 1 d . . . N2 N 0.1954(3) 0.2775(4) 0.4741(5) 0.0335(19) Uani 1 1 d . . . N3 N 0.2038(3) 0.2428(4) 0.6070(5) 0.0249(17) Uani 1 1 d . . . N4 N 0.2363(3) 0.0354(4) 0.4649(5) 0.0342(19) Uani 1 1 d . . . N5 N 0.3045(3) 0.0585(4) 0.4153(5) 0.0274(17) Uani 1 1 d . . . N6 N 0.3032(3) -0.0581(4) 0.4824(5) 0.0327(19) Uani 1 1 d D . . H6 H 0.331(2) -0.059(6) 0.468(6) 0.04(3) Uiso 1 1 d D . . C1 C 0.1903(3) 0.2211(5) 0.5267(6) 0.0224(19) Uani 1 1 d . . . C2 C 0.2820(4) 0.0097(5) 0.4530(6) 0.029(2) Uani 1 1 d . . . C3 C 0.1480(3) 0.1011(5) 0.5101(5) 0.0233(19) Uani 1 1 d . . . C4 C 0.1064(3) 0.1242(5) 0.5356(6) 0.028(2) Uani 1 1 d . . . H4 H 0.1035 0.1747 0.5477 0.034 Uiso 1 1 calc R . . C5 C 0.0687(4) 0.0759(6) 0.5440(7) 0.042(3) Uani 1 1 d . . . H5 H 0.0421 0.0933 0.5653 0.051 Uiso 1 1 calc R . . C6 C 0.0693(4) 0.0039(6) 0.5221(7) 0.040(3) Uani 1 1 d . . . H6A H 0.0427 -0.0280 0.5264 0.048 Uiso 1 1 calc R . . C7 C 0.1102(4) -0.0230(5) 0.4928(6) 0.032(2) Uani 1 1 d . . . C8 C 0.1098(4) -0.0978(6) 0.4658(7) 0.045(3) Uani 1 1 d . . . H8 H 0.0836 -0.1301 0.4709 0.054 Uiso 1 1 calc R . . C9 C 0.1478(5) -0.1227(5) 0.4323(7) 0.047(3) Uani 1 1 d . . . H9 H 0.1452 -0.1706 0.4094 0.056 Uiso 1 1 calc R . . C10 C 0.1890(4) -0.0802(5) 0.4311(7) 0.039(3) Uani 1 1 d . . . H10 H 0.2147 -0.0998 0.4090 0.047 Uiso 1 1 calc R . . C11 C 0.1937(4) -0.0085(5) 0.4621(6) 0.030(2) Uani 1 1 d . . . C12 C 0.1523(4) 0.0233(5) 0.4896(6) 0.030(2) Uani 1 1 d . . . C13 C 0.1580(4) 0.2873(5) 0.3921(6) 0.032(2) Uani 1 1 d . . . H13 H 0.1697 0.2577 0.3508 0.038 Uiso 1 1 calc R . . C14 C 0.1034(4) 0.2645(6) 0.3880(7) 0.043(3) Uani 1 1 d . . . H14A H 0.1026 0.2122 0.4011 0.065 Uiso 1 1 calc R . . H14B H 0.0817 0.2734 0.3325 0.065 Uiso 1 1 calc R . . H14C H 0.0910 0.2933 0.4277 0.065 Uiso 1 1 calc R . . C15 C 0.1600(4) 0.3674(5) 0.3703(7) 0.037(2) Uani 1 1 d . . . H15A H 0.1450 0.3970 0.4062 0.055 Uiso 1 1 calc R . . H15B H 0.1409 0.3750 0.3130 0.055 Uiso 1 1 calc R . . H15C H 0.1953 0.3821 0.3775 0.055 Uiso 1 1 calc R . . C16 C 0.2069(4) 0.1900(5) 0.6740(6) 0.028(2) Uani 1 1 d . . . H16 H 0.2036 0.1391 0.6511 0.034 Uiso 1 1 calc R . . C17 C 0.1633(4) 0.2044(7) 0.7146(7) 0.052(3) Uani 1 1 d . . . H17A H 0.1684 0.2521 0.7425 0.078 Uiso 1 1 calc R . . H17B H 0.1630 0.1657 0.7548 0.078 Uiso 1 1 calc R . . H17C H 0.1308 0.2046 0.6724 0.078 Uiso 1 1 calc R . . C18 C 0.2556(4) 0.1957(7) 0.7428(7) 0.047(3) Uani 1 1 d . . . H18A H 0.2848 0.1929 0.7195 0.071 Uiso 1 1 calc R . . H18B H 0.2573 0.1552 0.7816 0.071 Uiso 1 1 calc R . . H18C H 0.2563 0.2425 0.7715 0.071 Uiso 1 1 calc R . . C19 C 0.3562(4) 0.0440(5) 0.4076(7) 0.038(2) Uani 1 1 d . . . H19 H 0.3771 0.0223 0.4602 0.045 Uiso 1 1 calc R . . C20 C 0.3544(5) -0.0112(6) 0.3359(8) 0.052(3) Uani 1 1 d . . . H20A H 0.3386 -0.0571 0.3464 0.078 Uiso 1 1 calc R . . H20B H 0.3889 -0.0211 0.3323 0.078 Uiso 1 1 calc R . . H20C H 0.3345 0.0101 0.2840 0.078 Uiso 1 1 calc R . . C21 C 0.3797(5) 0.1162(6) 0.3923(9) 0.054(3) Uani 1 1 d . . . H21A H 0.3615 0.1353 0.3383 0.082 Uiso 1 1 calc R . . H21B H 0.4154 0.1083 0.3939 0.082 Uiso 1 1 calc R . . H21C H 0.3775 0.1515 0.4349 0.082 Uiso 1 1 calc R . . C22 C 0.2976(4) -0.0933(5) 0.5588(7) 0.041(3) Uani 1 1 d . . . H22 H 0.2664 -0.0739 0.5717 0.050 Uiso 1 1 calc R . . C23 C 0.3433(5) -0.0766(7) 0.6302(8) 0.064(4) Uani 1 1 d . . . H23A H 0.3741 -0.0935 0.6168 0.096 Uiso 1 1 calc R . . H23B H 0.3398 -0.1020 0.6795 0.096 Uiso 1 1 calc R . . H23C H 0.3454 -0.0236 0.6402 0.096 Uiso 1 1 calc R . . C24 C 0.2922(6) -0.1757(6) 0.5455(9) 0.070(4) Uani 1 1 d . . . H24A H 0.2596 -0.1865 0.5062 0.106 Uiso 1 1 calc R . . H24B H 0.2937 -0.2000 0.5979 0.106 Uiso 1 1 calc R . . H24C H 0.3198 -0.1938 0.5239 0.106 Uiso 1 1 calc R . . C25 C 0.2238(6) 0.1024(7) 0.2304(8) 0.064(3) Uani 1 1 d . . . H25A H 0.2613 0.1029 0.2491 0.077 Uiso 1 1 calc R . . H25B H 0.2127 0.1311 0.1790 0.077 Uiso 1 1 calc R . . C26 C 0.2038(6) 0.0241(7) 0.2179(8) 0.064(3) Uani 1 1 d . . . H26A H 0.2014 0.0072 0.1612 0.077 Uiso 1 1 calc R . . H26B H 0.2262 -0.0098 0.2571 0.077 Uiso 1 1 calc R . . C27 C 0.1517(5) 0.0278(8) 0.2333(9) 0.070(3) Uani 1 1 d . . . H27A H 0.1469 -0.0133 0.2688 0.084 Uiso 1 1 calc R . . H27B H 0.1249 0.0255 0.1809 0.084 Uiso 1 1 calc R . . C28 C 0.1503(6) 0.1018(8) 0.2763(9) 0.070(3) Uani 1 1 d . . . H28A H 0.1257 0.1354 0.2402 0.084 Uiso 1 1 calc R . . H28B H 0.1402 0.0947 0.3279 0.084 Uiso 1 1 calc R . . C29 C 0.4563(17) 0.8609(19) 0.485(3) 0.102(3) Uiso 0.50 1 d PD A 1 C29' C 0.4521(17) 0.841(2) 0.508(2) 0.102(3) Uiso 0.50 1 d PD B 2 C30 C 0.4772(15) 0.7816(19) 0.487(2) 0.102(3) Uiso 0.50 1 d PD A 1 C30' C 0.4753(14) 0.793(2) 0.452(2) 0.102(3) Uiso 0.50 1 d PD B 2 C31 C 0.4444(14) 0.750(2) 0.408(2) 0.102(3) Uiso 0.50 1 d PD A 1 C31' C 0.4302(12) 0.766(2) 0.385(2) 0.102(3) Uiso 0.50 1 d PD B 2 C32 C 0.3951(15) 0.794(2) 0.398(3) 0.102(3) Uiso 0.50 1 d PD A 1 C32' C 0.3820(15) 0.780(2) 0.411(3) 0.102(3) Uiso 0.50 1 d PD B 2 C33 C 0.9858(15) 0.090(2) 0.178(2) 0.092(4) Uiso 0.50 1 d PD . 1 C34 C 0.9836(15) 0.012(2) 0.205(3) 0.092(4) Uiso 0.50 1 d PD . 1 C35 C 1.0002(15) 0.015(2) 0.298(3) 0.092(4) Uiso 0.50 1 d PD . 1 C36 C 1.0030(16) 0.096(2) 0.318(2) 0.092(4) Uiso 0.50 1 d PD . 1 C37 C 0.023(3) 0.468(4) 0.308(4) 0.207(13) Uiso 0.50 1 d PD . 1 C38 C -0.014(3) 0.527(4) 0.266(5) 0.207(13) Uiso 0.50 1 d PD . 1 C39 C -0.006(3) 0.526(4) 0.180(4) 0.207(13) Uiso 0.50 1 d PD . 1 C40 C -0.009(3) 0.447(4) 0.156(4) 0.207(13) Uiso 0.50 1 d PD . 1 C41 C -0.0083(19) 0.791(3) 0.298(3) 0.149(8) Uiso 0.50 1 d PD . 1 C42 C -0.0471(19) 0.745(3) 0.232(3) 0.149(8) Uiso 0.50 1 d PD . 1 C43 C -0.012(2) 0.701(2) 0.196(3) 0.149(8) Uiso 0.50 1 d PD . 1 C44 C 0.038(2) 0.740(2) 0.223(3) 0.149(8) Uiso 0.50 1 d PD . 1 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 0.0331(3) 0.0220(2) 0.0277(3) -0.00086(18) 0.00999(18) -0.00424(17) O1 0.046(4) 0.038(4) 0.030(4) -0.006(3) 0.003(3) -0.007(3) N1 0.038(5) 0.030(4) 0.019(4) -0.004(3) 0.002(3) -0.002(4) N2 0.046(5) 0.025(4) 0.031(5) -0.001(4) 0.014(4) 0.000(4) N3 0.032(4) 0.017(4) 0.030(5) 0.006(3) 0.016(4) -0.005(3) N4 0.041(5) 0.020(4) 0.041(5) 0.000(4) 0.010(4) 0.005(4) N5 0.030(4) 0.018(4) 0.037(5) 0.001(3) 0.015(4) 0.000(3) N6 0.037(5) 0.026(4) 0.040(5) 0.011(4) 0.019(4) -0.003(4) C1 0.007(4) 0.029(5) 0.031(5) 0.001(4) 0.005(4) -0.002(3) C2 0.034(5) 0.029(5) 0.022(5) -0.003(4) 0.001(4) 0.000(4) C3 0.027(5) 0.023(4) 0.026(5) 0.003(4) 0.016(4) -0.015(4) C4 0.021(5) 0.027(5) 0.042(6) -0.006(4) 0.016(4) 0.004(4) C5 0.052(7) 0.045(6) 0.034(6) -0.009(5) 0.016(5) -0.005(5) C6 0.032(6) 0.047(6) 0.039(7) 0.008(5) 0.005(5) -0.008(5) C7 0.029(5) 0.031(5) 0.031(6) 0.006(4) 0.000(4) -0.015(4) C8 0.049(7) 0.034(6) 0.053(8) 0.000(5) 0.016(6) -0.017(5) C9 0.063(8) 0.021(5) 0.055(8) -0.001(5) 0.013(6) -0.010(5) C10 0.043(6) 0.023(5) 0.061(8) 0.000(5) 0.030(6) 0.002(4) C11 0.030(5) 0.027(5) 0.035(6) 0.003(4) 0.012(4) -0.009(4) C12 0.046(6) 0.019(4) 0.023(5) 0.001(4) 0.006(4) -0.006(4) C13 0.043(6) 0.034(5) 0.017(5) -0.003(4) 0.005(4) 0.006(4) C14 0.027(5) 0.051(7) 0.049(7) 0.008(5) 0.005(5) -0.008(5) C15 0.033(6) 0.035(5) 0.035(6) 0.006(5) -0.002(5) -0.011(4) C16 0.036(5) 0.019(4) 0.034(6) 0.001(4) 0.015(4) 0.002(4) C17 0.050(7) 0.075(8) 0.035(7) 0.012(6) 0.021(6) -0.011(6) C18 0.037(6) 0.063(8) 0.041(7) 0.012(6) 0.010(5) -0.008(5) C19 0.035(6) 0.036(6) 0.050(7) -0.003(5) 0.023(5) 0.008(4) C20 0.068(8) 0.038(6) 0.064(8) 0.005(6) 0.041(7) 0.011(6) C21 0.051(7) 0.041(6) 0.085(10) -0.007(6) 0.042(7) -0.013(5) C22 0.051(7) 0.027(5) 0.049(7) 0.007(5) 0.018(6) -0.004(5) C23 0.091(10) 0.053(8) 0.044(8) 0.009(6) 0.011(7) 0.004(7) C24 0.099(11) 0.035(7) 0.076(10) 0.017(6) 0.021(9) -0.015(7) C25 0.095(8) 0.055(5) 0.039(5) -0.013(4) 0.012(5) -0.004(5) C26 0.095(8) 0.055(5) 0.039(5) -0.013(4) 0.012(5) -0.004(5) C27 0.081(7) 0.061(6) 0.056(6) -0.010(5) -0.005(5) -0.018(5) C28 0.081(7) 0.061(6) 0.056(6) -0.010(5) -0.005(5) -0.018(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 2.241(8) 7_556 ? Yb1 N4 2.281(8) . ? Yb1 N1 2.293(8) . ? Yb1 O1 2.341(7) . ? Yb1 N5 2.375(7) . ? Yb1 N3 2.431(6) 7_556 ? Yb1 C1 2.760(8) 7_556 ? Yb1 C2 2.772(9) . ? Yb1 C1 2.792(8) . ? Yb1 N2 2.829(8) . ? Yb1 Yb1 4.1145(11) 7_556 ? O1 C25 1.448(14) . ? O1 C28 1.457(15) . ? O2 C29 1.448(19) . ? O2 C32 1.451(19) . ? O2' C29' 1.44(2) . ? O2' C32' 1.444(19) . ? O3 O3 1.08(4) 2_755 ? O3 C36 1.29(4) 2_755 ? O3 C33 1.46(5) 2_755 ? O3 C33 1.483(19) . ? O3 C36 1.487(19) . ? O4 O4 1.10(8) 2 ? O4 C40 1.44(2) . ? O4 C37 1.45(8) 2 ? O4 C37 1.47(2) . ? O4 C40 1.92(10) 2 ? O5 C41 1.04(5) 2 ? O5 C42 1.25(6) 2 ? O5 C41 1.455(19) . ? O5 C44 1.430(19) . ? O5 O5 1.64(7) 2 ? N1 C1 1.351(11) . ? N1 C3 1.400(11) . ? N2 C1 1.376(11) . ? N2 C13 1.483(12) . ? N2 Yb1 2.241(8) 7_556 ? N3 C1 1.351(11) . ? N3 C16 1.456(11) . ? N3 Yb1 2.431(6) 7_556 ? N4 C2 1.385(12) . ? N4 C11 1.391(12) . ? N5 C2 1.322(11) . ? N5 C19 1.465(11) . ? N6 C2 1.384(12) . ? N6 C22 1.472(13) . ? N6 H6 0.858(10) . ? C1 Yb1 2.760(8) 7_556 ? C3 C4 1.372(11) . ? C3 C12 1.459(12) . ? C4 C5 1.379(13) . ? C4 H4 0.9400 . ? C5 C6 1.351(14) . ? C5 H5 0.9400 . ? C6 C7 1.411(14) . ? C6 H6A 0.9400 . ? C7 C8 1.422(14) . ? C7 C12 1.428(12) . ? C8 C9 1.371(15) . ? C8 H8 0.9400 . ? C9 C10 1.360(14) . ? C9 H9 0.9400 . ? C10 C11 1.388(13) . ? C10 H10 0.9400 . ? C11 C12 1.439(13) . ? C13 C15 1.494(13) . ? C13 C14 1.521(13) . ? C13 H13 0.9900 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C18 1.507(14) . ? C16 C17 1.534(13) . ? C16 H16 0.9900 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C21 1.502(14) . ? C19 C20 1.549(15) . ? C19 H19 0.9900 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 C23 1.503(16) . ? C22 C24 1.505(15) . ? C22 H22 0.9900 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C26 1.508(17) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 C27 1.502(18) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.522(18) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.536(19) . ? C29' C30' 1.520(19) . ? C30 C31 1.491(19) . ? C30' C31' 1.506(19) . ? C31 C32 1.517(19) . ? C31' C32' 1.503(19) . ? C33 C36 0.31(7) 2_755 ? C33 C35 1.43(8) 2_755 ? C33 O3 1.46(5) 2_755 ? C33 C34 1.487(19) . ? C34 C35 0.47(6) 2_755 ? C34 C35 1.501(18) . ? C34 C34 1.52(10) 2_755 ? C34 C36 1.63(8) 2_755 ? C35 C34 0.47(6) 2_755 ? C35 C33 1.43(8) 2_755 ? C35 C36 1.494(19) . ? C35 C35 1.62(9) 2_755 ? C36 C33 0.31(7) 2_755 ? C36 O3 1.29(4) 2_755 ? C36 C34 1.63(8) 2_755 ? C37 C40 0.86(10) 2 ? C37 C39 1.18(10) 2 ? C37 O4 1.45(8) 2 ? C37 C38 1.50(2) . ? C37 C38 1.60(10) 2 ? C37 C37 2.00(14) 2 ? C38 C39 0.92(12) 2 ? C38 C38 1.03(14) 2 ? C38 C39 1.49(2) . ? C38 C37 1.60(10) 2 ? C38 C40 1.94(11) 2 ? C39 C38 0.92(12) 2 ? C39 C37 1.18(10) 2 ? C39 C40 1.49(2) . ? C40 C37 0.86(10) 2 ? C40 O4 1.92(10) 2 ? C40 C38 1.94(11) 2 ? C41 O5 1.04(5) 2 ? C41 C44 1.21(7) 2 ? C41 C42 1.54(2) . ? C41 C41 1.79(9) 2 ? C41 C43 1.70(7) 2 ? C41 C42 1.89(8) 2 ? C42 C44 0.73(7) 2 ? C42 O5 1.25(6) 2 ? C42 C43 1.48(2) . ? C42 C41 1.89(8) 2 ? C42 C43 1.91(7) 2 ? C43 C44 1.49(2) . ? C43 C41 1.70(7) 2 ? C43 C43 1.74(9) 2 ? C43 C44 1.81(8) 2 ? C43 C42 1.91(7) 2 ? C44 C42 0.73(7) 2 ? C44 C41 1.21(7) 2 ? C44 C43 1.81(8) 2 ? 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 N4 116.9(3) 7_556 . ? N2 Yb1 N1 98.9(3) 7_556 . ? N4 Yb1 N1 71.8(3) . . ? N2 Yb1 O1 151.3(3) 7_556 . ? N4 Yb1 O1 89.9(3) . . ? N1 Yb1 O1 99.2(3) . . ? N2 Yb1 N5 98.2(3) 7_556 . ? N4 Yb1 N5 57.9(3) . . ? N1 Yb1 N5 129.3(3) . . ? O1 Yb1 N5 87.3(3) . . ? N2 Yb1 N3 57.7(3) 7_556 7_556 ? N4 Yb1 N3 154.7(3) . 7_556 ? N1 Yb1 N3 131.9(2) . 7_556 ? O1 Yb1 N3 93.7(3) . 7_556 ? N5 Yb1 N3 97.2(2) . 7_556 ? N2 Yb1 C1 29.7(3) 7_556 7_556 ? N4 Yb1 C1 145.0(3) . 7_556 ? N1 Yb1 C1 112.9(2) . 7_556 ? O1 Yb1 C1 121.7(3) . 7_556 ? N5 Yb1 C1 105.3(2) . 7_556 ? N3 Yb1 C1 29.3(3) 7_556 7_556 ? N2 Yb1 C2 106.4(3) 7_556 . ? N4 Yb1 C2 29.9(3) . . ? N1 Yb1 C2 100.9(3) . . ? O1 Yb1 C2 91.9(3) . . ? N5 Yb1 C2 28.5(3) . . ? N3 Yb1 C2 124.9(3) 7_556 . ? C1 Yb1 C2 125.3(3) 7_556 . ? N2 Yb1 C1 75.2(3) 7_556 . ? N4 Yb1 C1 97.0(3) . . ? N1 Yb1 C1 28.7(2) . . ? O1 Yb1 C1 113.5(2) . . ? N5 Yb1 C1 148.4(3) . . ? N3 Yb1 C1 104.4(2) 7_556 . ? C1 Yb1 C1 84.4(2) 7_556 . ? C2 Yb1 C1 122.9(3) . . ? N2 Yb1 N2 72.1(3) 7_556 . ? N4 Yb1 N2 124.1(3) . . ? N1 Yb1 N2 52.5(2) . . ? O1 Yb1 N2 102.2(2) . . ? N5 Yb1 N2 170.0(3) . . ? N3 Yb1 N2 79.5(2) 7_556 . ? C1 Yb1 N2 67.4(2) 7_556 . ? C2 Yb1 N2 151.2(3) . . ? C1 Yb1 N2 28.3(2) . . ? N2 Yb1 Yb1 40.8(2) 7_556 7_556 ? N4 Yb1 Yb1 129.2(2) . 7_556 ? N1 Yb1 Yb1 70.47(19) . 7_556 ? O1 Yb1 Yb1 128.56(17) . 7_556 ? N5 Yb1 Yb1 138.99(19) . 7_556 ? N3 Yb1 Yb1 65.40(17) 7_556 7_556 ? C1 Yb1 Yb1 42.48(17) 7_556 7_556 ? C2 Yb1 Yb1 139.13(19) . 7_556 ? C1 Yb1 Yb1 41.88(17) . 7_556 ? N2 Yb1 Yb1 31.22(17) . 7_556 ? C25 O1 C28 105.9(9) . . ? C25 O1 Yb1 124.3(7) . . ? C28 O1 Yb1 120.1(7) . . ? C29 O2 C32 102(4) . . ? C29' O2' C32' 113(5) . . ? O3 O3 C36 77(2) 2_755 2_755 ? O3 O3 C33 70(2) 2_755 2_755 ? C36 O3 C33 111(3) 2_755 2_755 ? O3 O3 C33 67(3) 2_755 . ? C36 O3 C33 10(3) 2_755 . ? C33 O3 C33 104(3) 2_755 . ? O3 O3 C36 58(2) 2_755 . ? C36 O3 C36 107(4) 2_755 . ? C33 O3 C36 12(3) 2_755 . ? C33 O3 C36 99(2) . . ? O4 O4 C40 97(7) 2 . ? O4 O4 C37 69(4) 2 2 ? C40 O4 C37 35(4) . 2 ? O4 O4 C37 67(5) 2 . ? C40 O4 C37 117(5) . . ? C37 O4 C37 87(6) 2 . ? O4 O4 C40 48(4) 2 2 ? C40 O4 C40 128(5) . 2 ? C37 O4 C40 94(4) 2 2 ? C37 O4 C40 25(4) . 2 ? C41 O5 C42 84(3) 2 2 ? C41 O5 C41 90(5) 2 . ? C42 O5 C41 89(4) 2 . ? C41 O5 C44 56(4) 2 . ? C42 O5 C44 31(3) 2 . ? C41 O5 C44 99(4) . . ? C41 O5 O5 61(3) 2 2 ? C42 O5 O5 109(3) 2 2 ? C41 O5 O5 39(2) . 2 ? C44 O5 O5 100(3) . 2 ? C1 N1 C3 124.2(8) . . ? C1 N1 Yb1 96.6(5) . . ? C3 N1 Yb1 138.4(6) . . ? C1 N2 C13 121.2(8) . . ? C1 N2 Yb1 96.5(6) . 7_556 ? C13 N2 Yb1 139.3(6) . 7_556 ? C1 N2 Yb1 74.4(5) . . ? C13 N2 Yb1 97.3(5) . . ? Yb1 N2 Yb1 107.9(3) 7_556 . ? C1 N3 C16 121.3(7) . . ? C1 N3 Yb1 89.0(5) . 7_556 ? C16 N3 Yb1 140.4(6) . 7_556 ? C2 N4 C11 124.8(8) . . ? C2 N4 Yb1 95.1(6) . . ? C11 N4 Yb1 134.7(6) . . ? C2 N5 C19 119.8(8) . . ? C2 N5 Yb1 92.7(5) . . ? C19 N5 Yb1 142.8(6) . . ? C2 N6 C22 124.1(8) . . ? C2 N6 H6 104(7) . . ? C22 N6 H6 122(7) . . ? N1 C1 N3 130.5(8) . . ? N1 C1 N2 116.2(8) . . ? N3 C1 N2 111.9(7) . . ? N1 C1 Yb1 149.7(6) . 7_556 ? N3 C1 Yb1 61.7(4) . 7_556 ? N2 C1 Yb1 53.8(4) . 7_556 ? N1 C1 Yb1 54.7(4) . . ? N3 C1 Yb1 130.4(5) . . ? N2 C1 Yb1 77.3(5) . . ? Yb1 C1 Yb1 95.6(2) 7_556 . ? N5 C2 N6 123.8(8) . . ? N5 C2 N4 112.9(8) . . ? N6 C2 N4 123.2(8) . . ? N5 C2 Yb1 58.9(5) . . ? N6 C2 Yb1 167.1(7) . . ? N4 C2 Yb1 55.0(5) . . ? C4 C3 N1 120.7(8) . . ? C4 C3 C12 119.3(8) . . ? N1 C3 C12 119.4(8) . . ? C3 C4 C5 122.1(9) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C6 C5 C4 121.2(10) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 119.5(10) . . ? C5 C6 H6A 120.3 . . ? C7 C6 H6A 120.3 . . ? C6 C7 C8 119.8(9) . . ? C6 C7 C12 121.5(9) . . ? C8 C7 C12 118.7(9) . . ? C9 C8 C7 119.9(9) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C10 C9 C8 122.0(10) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C9 C10 C11 121.0(9) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C10 C11 N4 122.5(9) . . ? C10 C11 C12 119.3(8) . . ? N4 C11 C12 118.2(8) . . ? C7 C12 C11 118.6(8) . . ? C7 C12 C3 116.0(8) . . ? C11 C12 C3 125.3(8) . . ? N2 C13 C15 106.3(8) . . ? N2 C13 C14 115.3(8) . . ? C15 C13 C14 110.4(8) . . ? N2 C13 H13 108.2 . . ? C15 C13 H13 108.2 . . ? C14 C13 H13 108.2 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C18 113.7(8) . . ? N3 C16 C17 109.7(8) . . ? C18 C16 C17 105.9(9) . . ? N3 C16 H16 109.2 . . ? C18 C16 H16 109.2 . . ? C17 C16 H16 109.2 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N5 C19 C21 108.6(8) . . ? N5 C19 C20 110.4(9) . . ? C21 C19 C20 110.7(9) . . ? N5 C19 H19 109.0 . . ? C21 C19 H19 109.0 . . ? C20 C19 H19 109.0 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N6 C22 C23 110.4(9) . . ? N6 C22 C24 109.1(9) . . ? C23 C22 C24 110.0(10) . . ? N6 C22 H22 109.1 . . ? C23 C22 H22 109.1 . . ? C24 C22 H22 109.1 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O1 C25 C26 104.2(10) . . ? O1 C25 H25A 110.9 . . ? C26 C25 H25A 110.9 . . ? O1 C25 H25B 110.9 . . ? C26 C25 H25B 110.9 . . ? H25A C25 H25B 108.9 . . ? C27 C26 C25 104.7(11) . . ? C27 C26 H26A 110.8 . . ? C25 C26 H26A 110.8 . . ? C27 C26 H26B 110.8 . . ? C25 C26 H26B 110.8 . . ? H26A C26 H26B 108.9 . . ? C26 C27 C28 105.3(11) . . ? C26 C27 H27A 110.7 . . ? C28 C27 H27A 110.7 . . ? C26 C27 H27B 110.7 . . ? C28 C27 H27B 110.7 . . ? H27A C27 H27B 108.8 . . ? O1 C28 C27 106.2(11) . . ? O1 C28 H28A 110.5 . . ? C27 C28 H28A 110.5 . . ? O1 C28 H28B 110.5 . . ? C27 C28 H28B 110.5 . . ? H28A C28 H28B 108.7 . . ? O2 C29 C30 102(4) . . ? O2' C29' C30' 103(4) . . ? C31 C30 C29 101(3) . . ? C31' C30' C29' 105(3) . . ? C30 C31 C32 102(3) . . ? C32' C31' C30' 109(3) . . ? O2 C32 C31 110(4) . . ? O2' C32' C31' 99(4) . . ? C36 C33 C35 96(10) 2_755 2_755 ? C36 C33 O3 89(9) 2_755 2_755 ? C35 C33 O3 109(4) 2_755 2_755 ? C36 C33 O3 47(9) 2_755 . ? C35 C33 O3 101(3) 2_755 . ? O3 C33 O3 43.2(17) 2_755 . ? C36 C33 C34 113(10) 2_755 . ? C35 C33 C34 18(2) 2_755 . ? O3 C33 C34 102(3) 2_755 . ? O3 C33 C34 107(3) . . ? C35 C34 C33 74(10) 2_755 . ? C35 C34 C35 96(10) 2_755 . ? C33 C34 C35 105(4) . . ? C35 C34 C34 79(10) 2_755 2_755 ? C33 C34 C34 104(2) . 2_755 ? C35 C34 C34 18(2) . 2_755 ? C35 C34 C36 64(9) 2_755 2_755 ? C33 C34 C36 10(3) . 2_755 ? C35 C34 C36 101(4) . 2_755 ? C34 C34 C36 97(2) 2_755 2_755 ? C34 C35 C33 88(9) 2_755 2_755 ? C34 C35 C36 99(10) 2_755 . ? C33 C35 C36 12(3) 2_755 . ? C34 C35 C34 84(10) 2_755 . ? C33 C35 C34 108(4) 2_755 . ? C36 C35 C34 105(5) . . ? C34 C35 C35 68(10) 2_755 2_755 ? C33 C35 C35 102(2) 2_755 2_755 ? C36 C35 C35 102(2) . 2_755 ? C34 C35 C35 17(2) . 2_755 ? C33 C36 O3 123(10) 2_755 2_755 ? C33 C36 O3 79(10) 2_755 . ? O3 C36 O3 45.2(18) 2_755 . ? C33 C36 C35 72(10) 2_755 . ? O3 C36 C35 107(4) 2_755 . ? O3 C36 C35 104(3) . . ? C33 C36 C34 57(10) 2_755 2_755 ? O3 C36 C34 109(4) 2_755 2_755 ? O3 C36 C34 94(3) . 2_755 ? C35 C36 C34 16(2) . 2_755 ? C40 C37 C39 92(8) 2 2 ? C40 C37 O4 72(5) 2 2 ? C39 C37 O4 113(7) 2 2 ? C40 C37 O4 108(9) 2 . ? C39 C37 O4 136(7) 2 . ? O4 C37 O4 44(4) 2 . ? C40 C37 C38 107(10) 2 . ? C39 C37 C38 38(6) 2 . ? O4 C37 C38 84(5) 2 . ? O4 C37 C38 98(5) . . ? C40 C37 C38 145(10) 2 2 ? C39 C37 C38 63(4) 2 2 ? O4 C37 C38 95(7) 2 2 ? O4 C37 C38 80(5) . 2 ? C38 C37 C38 39(5) . 2 ? C40 C37 C37 114(9) 2 2 ? C39 C37 C37 90(5) 2 2 ? O4 C37 C37 47(4) 2 2 ? O4 C37 C37 46(3) . 2 ? C38 C37 C37 52(4) . 2 ? C38 C37 C37 48(3) 2 2 ? C39 C38 C38 99(10) 2 2 ? C39 C38 C39 137(8) 2 . ? C38 C38 C39 38(6) 2 . ? C39 C38 C37 52(6) 2 . ? C38 C38 C37 76(7) 2 . ? C39 C38 C37 102(6) . . ? C39 C38 C37 132(9) 2 2 ? C38 C38 C37 65(5) 2 2 ? C39 C38 C37 45(5) . 2 ? C37 C38 C37 80(6) . 2 ? C39 C38 C40 48(6) 2 2 ? C38 C38 C40 101(7) 2 2 ? C39 C38 C40 122(6) . 2 ? C37 C38 C40 25(4) . 2 ? C37 C38 C40 88(4) 2 2 ? C38 C39 C37 90(8) 2 2 ? C38 C39 C40 104(9) 2 . ? C37 C39 C40 35(5) 2 . ? C38 C39 C38 43(8) 2 . ? C37 C39 C38 73(6) 2 . ? C40 C39 C38 105(6) . . ? C37 C40 O4 73(6) 2 . ? C37 C40 C39 52(7) 2 . ? O4 C40 C39 97(5) . . ? C37 C40 O4 47(6) 2 2 ? O4 C40 O4 35(3) . 2 ? C39 C40 O4 92(5) . 2 ? C37 C40 C38 48(7) 2 2 ? O4 C40 C38 70(3) . 2 ? C39 C40 C38 28(4) . 2 ? O4 C40 C38 71(3) 2 2 ? O5 C41 C44 79(4) 2 2 ? O5 C41 O5 80(5) 2 . ? C44 C41 O5 124(5) 2 . ? O5 C41 C42 54(3) 2 . ? C44 C41 C42 27(3) 2 . ? O5 C41 C42 104(4) . . ? O5 C41 C41 55(4) 2 2 ? C44 C41 C41 92(4) 2 2 ? O5 C41 C41 36(2) . 2 ? C42 C41 C41 69(4) . 2 ? O5 C41 C43 119(5) 2 2 ? C44 C41 C43 59(3) 2 2 ? O5 C41 C43 89(4) . 2 ? C42 C41 C43 72(3) . 2 ? C41 C41 C43 84(2) 2 2 ? O5 C41 C42 104(5) 2 2 ? C44 C41 C42 96(4) 2 2 ? O5 C41 C42 41(2) . 2 ? C42 C41 C42 91(4) . 2 ? C41 C41 C42 49.5(19) 2 2 ? C43 C41 C42 48(2) 2 2 ? C44 C42 O5 88(5) 2 2 ? C44 C42 C43 106(7) 2 . ? O5 C42 C43 109(4) 2 . ? C44 C42 C41 50(5) 2 . ? O5 C42 C41 42(2) 2 . ? C43 C42 C41 101(4) . . ? C44 C42 C41 105(7) 2 2 ? O5 C42 C41 50(3) 2 2 ? C43 C42 C41 59(3) . 2 ? C41 C42 C41 62(4) . 2 ? C44 C42 C43 46(5) 2 2 ? O5 C42 C43 96(4) 2 2 ? C43 C42 C43 60(4) . 2 ? C41 C42 C43 58(3) . 2 ? C41 C42 C43 76(4) 2 2 ? C42 C43 C44 105(3) . . ? C42 C43 C41 73(3) . 2 ? C44 C43 C41 44(3) . 2 ? C42 C43 C43 72(4) . 2 ? C44 C43 C43 68(4) . 2 ? C41 C43 C43 85(3) 2 2 ? C42 C43 C44 23(3) . 2 ? C44 C43 C44 95(4) . 2 ? C41 C43 C44 77(3) 2 2 ? C43 C43 C44 50(2) 2 2 ? C42 C43 C42 93(4) . 2 ? C44 C43 C42 20(3) . 2 ? C41 C43 C42 50.2(17) 2 2 ? C43 C43 C42 47.5(18) 2 2 ? C44 C43 C42 78(3) 2 2 ? C42 C44 C41 103(6) 2 2 ? C42 C44 O5 61(5) 2 . ? C41 C44 O5 46(3) 2 . ? C42 C44 C43 114(7) 2 . ? C41 C44 C43 77(4) 2 . ? O5 C44 C43 110(4) . . ? C42 C44 C43 52(5) 2 2 ? C41 C44 C43 99(5) 2 2 ? O5 C44 C43 86(3) . 2 ? C43 C44 C43 63(4) . 2 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Yb1 O1 C25 73.8(10) 7_556 . . . ? N4 Yb1 O1 C25 -86.3(8) . . . . ? N1 Yb1 O1 C25 -157.8(8) . . . . ? N5 Yb1 O1 C25 -28.4(8) . . . . ? N3 Yb1 O1 C25 68.7(8) 7_556 . . . ? C1 Yb1 O1 C25 77.9(8) 7_556 . . . ? C2 Yb1 O1 C25 -56.5(8) . . . . ? C1 Yb1 O1 C25 176.1(8) . . . . ? N2 Yb1 O1 C25 148.7(8) . . . . ? Yb1 Yb1 O1 C25 129.9(7) 7_556 . . . ? N2 Yb1 O1 C28 -145.0(8) 7_556 . . . ? N4 Yb1 O1 C28 54.9(8) . . . . ? N1 Yb1 O1 C28 -16.6(8) . . . . ? N5 Yb1 O1 C28 112.8(8) . . . . ? N3 Yb1 O1 C28 -150.1(8) 7_556 . . . ? C1 Yb1 O1 C28 -140.9(8) 7_556 . . . ? C2 Yb1 O1 C28 84.7(8) . . . . ? C1 Yb1 O1 C28 -42.7(8) . . . . ? N2 Yb1 O1 C28 -70.1(8) . . . . ? Yb1 Yb1 O1 C28 -88.9(8) 7_556 . . . ? N2 Yb1 N1 C1 34.4(6) 7_556 . . . ? N4 Yb1 N1 C1 150.0(6) . . . . ? O1 Yb1 N1 C1 -123.1(5) . . . . ? N5 Yb1 N1 C1 142.8(5) . . . . ? N3 Yb1 N1 C1 -19.6(7) 7_556 . . . ? C1 Yb1 N1 C1 7.1(7) 7_556 . . . ? C2 Yb1 N1 C1 143.2(5) . . . . ? N2 Yb1 N1 C1 -24.7(5) . . . . ? Yb1 Yb1 N1 C1 4.7(5) 7_556 . . . ? N2 Yb1 N1 C3 -135.2(9) 7_556 . . . ? N4 Yb1 N1 C3 -19.7(9) . . . . ? O1 Yb1 N1 C3 67.2(9) . . . . ? N5 Yb1 N1 C3 -26.9(10) . . . . ? N3 Yb1 N1 C3 170.7(8) 7_556 . . . ? C1 Yb1 N1 C3 -162.6(9) 7_556 . . . ? C2 Yb1 N1 C3 -26.5(9) . . . . ? C1 Yb1 N1 C3 -169.7(12) . . . . ? N2 Yb1 N1 C3 165.6(10) . . . . ? Yb1 Yb1 N1 C3 -165.0(9) 7_556 . . . ? N2 Yb1 N2 C1 -91.9(6) 7_556 . . . ? N4 Yb1 N2 C1 18.9(6) . . . . ? N1 Yb1 N2 C1 25.0(5) . . . . ? O1 Yb1 N2 C1 117.3(5) . . . . ? N5 Yb1 N2 C1 -79.4(15) . . . . ? N3 Yb1 N2 C1 -151.1(5) 7_556 . . . ? C1 Yb1 N2 C1 -123.2(5) 7_556 . . . ? C2 Yb1 N2 C1 -0.4(8) . . . . ? Yb1 Yb1 N2 C1 -91.9(6) 7_556 . . . ? N2 Yb1 N2 C13 147.6(7) 7_556 . . . ? N4 Yb1 N2 C13 -101.5(6) . . . . ? N1 Yb1 N2 C13 -95.5(6) . . . . ? O1 Yb1 N2 C13 -3.2(6) . . . . ? N5 Yb1 N2 C13 160.1(12) . . . . ? N3 Yb1 N2 C13 88.4(5) 7_556 . . . ? C1 Yb1 N2 C13 116.3(6) 7_556 . . . ? C2 Yb1 N2 C13 -120.9(6) . . . . ? C1 Yb1 N2 C13 -120.5(8) . . . . ? Yb1 Yb1 N2 C13 147.6(7) 7_556 . . . ? N2 Yb1 N2 Yb1 0.0 7_556 . . 7_556 ? N4 Yb1 N2 Yb1 110.9(4) . . . 7_556 ? N1 Yb1 N2 Yb1 117.0(4) . . . 7_556 ? O1 Yb1 N2 Yb1 -150.8(3) . . . 7_556 ? N5 Yb1 N2 Yb1 12.5(15) . . . 7_556 ? N3 Yb1 N2 Yb1 -59.2(3) 7_556 . . 7_556 ? C1 Yb1 N2 Yb1 -31.3(3) 7_556 . . 7_556 ? C2 Yb1 N2 Yb1 91.5(6) . . . 7_556 ? C1 Yb1 N2 Yb1 91.9(6) . . . 7_556 ? N2 Yb1 N4 C2 -75.5(6) 7_556 . . . ? N1 Yb1 N4 C2 -166.4(6) . . . . ? O1 Yb1 N4 C2 93.9(6) . . . . ? N5 Yb1 N4 C2 7.0(5) . . . . ? N3 Yb1 N4 C2 -4.7(10) 7_556 . . . ? C1 Yb1 N4 C2 -62.3(7) 7_556 . . . ? C1 Yb1 N4 C2 -152.4(5) . . . . ? N2 Yb1 N4 C2 -161.3(5) . . . . ? Yb1 Yb1 N4 C2 -122.7(5) 7_556 . . . ? N2 Yb1 N4 C11 131.0(9) 7_556 . . . ? N1 Yb1 N4 C11 40.1(9) . . . . ? O1 Yb1 N4 C11 -59.5(9) . . . . ? N5 Yb1 N4 C11 -146.5(10) . . . . ? N3 Yb1 N4 C11 -158.2(8) 7_556 . . . ? C1 Yb1 N4 C11 144.2(8) 7_556 . . . ? C2 Yb1 N4 C11 -153.5(12) . . . . ? C1 Yb1 N4 C11 54.1(9) . . . . ? N2 Yb1 N4 C11 45.2(10) . . . . ? Yb1 Yb1 N4 C11 83.9(9) 7_556 . . . ? N2 Yb1 N5 C2 109.4(6) 7_556 . . . ? N4 Yb1 N5 C2 -7.3(5) . . . . ? N1 Yb1 N5 C2 0.8(7) . . . . ? O1 Yb1 N5 C2 -98.9(6) . . . . ? N3 Yb1 N5 C2 167.7(5) 7_556 . . . ? C1 Yb1 N5 C2 138.9(5) 7_556 . . . ? C1 Yb1 N5 C2 34.5(8) . . . . ? N2 Yb1 N5 C2 97.4(14) . . . . ? Yb1 Yb1 N5 C2 107.3(5) 7_556 . . . ? N2 Yb1 N5 C19 -42.6(11) 7_556 . . . ? N4 Yb1 N5 C19 -159.3(12) . . . . ? N1 Yb1 N5 C19 -151.2(10) . . . . ? O1 Yb1 N5 C19 109.1(11) . . . . ? N3 Yb1 N5 C19 15.7(11) 7_556 . . . ? C1 Yb1 N5 C19 -13.1(11) 7_556 . . . ? C2 Yb1 N5 C19 -152.0(14) . . . . ? C1 Yb1 N5 C19 -117.5(10) . . . . ? N2 Yb1 N5 C19 -55(2) . . . . ? Yb1 Yb1 N5 C19 -44.8(12) 7_556 . . . ? C3 N1 C1 N3 55.7(13) . . . . ? Yb1 N1 C1 N3 -116.1(8) . . . . ? C3 N1 C1 N2 -138.8(9) . . . . ? Yb1 N1 C1 N2 49.5(7) . . . . ? C3 N1 C1 Yb1 158.7(9) . . . 7_556 ? Yb1 N1 C1 Yb1 -13.1(13) . . . 7_556 ? C3 N1 C1 Yb1 171.7(10) . . . . ? C16 N3 C1 N1 -7.0(13) . . . . ? Yb1 N3 C1 N1 146.1(8) 7_556 . . . ? C16 N3 C1 N2 -173.0(7) . . . . ? Yb1 N3 C1 N2 -20.0(7) 7_556 . . . ? C16 N3 C1 Yb1 -153.0(8) . . . 7_556 ? C16 N3 C1 Yb1 -81.2(9) . . . . ? Yb1 N3 C1 Yb1 71.9(6) 7_556 . . . ? C13 N2 C1 N1 49.7(11) . . . . ? Yb1 N2 C1 N1 -146.3(6) 7_556 . . . ? Yb1 N2 C1 N1 -39.5(6) . . . . ? C13 N2 C1 N3 -142.2(8) . . . . ? Yb1 N2 C1 N3 21.9(7) 7_556 . . . ? Yb1 N2 C1 N3 128.7(6) . . . . ? C13 N2 C1 Yb1 -164.1(9) . . . 7_556 ? Yb1 N2 C1 Yb1 106.8(3) . . . 7_556 ? C13 N2 C1 Yb1 89.1(7) . . . . ? Yb1 N2 C1 Yb1 -106.8(3) 7_556 . . . ? N2 Yb1 C1 N1 -144.7(6) 7_556 . . . ? N4 Yb1 C1 N1 -28.6(6) . . . . ? O1 Yb1 C1 N1 64.4(6) . . . . ? N5 Yb1 C1 N1 -63.3(7) . . . . ? N3 Yb1 C1 N1 165.0(5) 7_556 . . . ? C1 Yb1 C1 N1 -173.4(7) 7_556 . . . ? C2 Yb1 C1 N1 -44.5(6) . . . . ? N2 Yb1 C1 N1 135.7(8) . . . . ? Yb1 Yb1 C1 N1 -173.4(7) 7_556 . . . ? N2 Yb1 C1 N3 -28.5(7) 7_556 . . . ? N4 Yb1 C1 N3 87.6(7) . . . . ? N1 Yb1 C1 N3 116.2(10) . . . . ? O1 Yb1 C1 N3 -179.4(7) . . . . ? N5 Yb1 C1 N3 52.9(9) . . . . ? N3 Yb1 C1 N3 -78.8(8) 7_556 . . . ? C1 Yb1 C1 N3 -57.2(6) 7_556 . . . ? C2 Yb1 C1 N3 71.7(8) . . . . ? N2 Yb1 C1 N3 -108.1(9) . . . . ? Yb1 Yb1 C1 N3 -57.2(6) 7_556 . . . ? N2 Yb1 C1 N2 79.6(6) 7_556 . . . ? N4 Yb1 C1 N2 -164.3(5) . . . . ? N1 Yb1 C1 N2 -135.7(8) . . . . ? O1 Yb1 C1 N2 -71.3(5) . . . . ? N5 Yb1 C1 N2 161.0(5) . . . . ? N3 Yb1 C1 N2 29.3(5) 7_556 . . . ? C1 Yb1 C1 N2 50.9(4) 7_556 . . . ? C2 Yb1 C1 N2 179.8(5) . . . . ? Yb1 Yb1 C1 N2 50.9(4) 7_556 . . . ? N2 Yb1 C1 Yb1 28.7(3) 7_556 . . 7_556 ? N4 Yb1 C1 Yb1 144.8(3) . . . 7_556 ? N1 Yb1 C1 Yb1 173.4(7) . . . 7_556 ? O1 Yb1 C1 Yb1 -122.2(2) . . . 7_556 ? N5 Yb1 C1 Yb1 110.1(4) . . . 7_556 ? N3 Yb1 C1 Yb1 -21.6(3) 7_556 . . 7_556 ? C1 Yb1 C1 Yb1 0.0 7_556 . . 7_556 ? C2 Yb1 C1 Yb1 128.9(3) . . . 7_556 ? N2 Yb1 C1 Yb1 -50.9(4) . . . 7_556 ? C19 N5 C2 N6 -4.0(14) . . . . ? Yb1 N5 C2 N6 -165.0(8) . . . . ? C19 N5 C2 N4 172.1(8) . . . . ? Yb1 N5 C2 N4 11.1(8) . . . . ? C19 N5 C2 Yb1 161.0(9) . . . . ? C22 N6 C2 N5 144.2(10) . . . . ? C22 N6 C2 N4 -31.6(14) . . . . ? C22 N6 C2 Yb1 46(3) . . . . ? C11 N4 C2 N5 145.7(9) . . . . ? Yb1 N4 C2 N5 -11.6(8) . . . . ? C11 N4 C2 N6 -38.2(14) . . . . ? Yb1 N4 C2 N6 164.5(8) . . . . ? C11 N4 C2 Yb1 157.3(11) . . . . ? N2 Yb1 C2 N5 -76.6(6) 7_556 . . . ? N4 Yb1 C2 N5 167.5(9) . . . . ? N1 Yb1 C2 N5 -179.4(5) . . . . ? O1 Yb1 C2 N5 80.9(6) . . . . ? N3 Yb1 C2 N5 -14.9(7) 7_556 . . . ? C1 Yb1 C2 N5 -51.0(6) 7_556 . . . ? C1 Yb1 C2 N5 -159.3(5) . . . . ? N2 Yb1 C2 N5 -159.1(6) . . . . ? Yb1 Yb1 C2 N5 -106.7(5) 7_556 . . . ? N2 Yb1 C2 N6 29(3) 7_556 . . . ? N4 Yb1 C2 N6 -87(3) . . . . ? N1 Yb1 C2 N6 -73(3) . . . . ? O1 Yb1 C2 N6 -173(3) . . . . ? N5 Yb1 C2 N6 106(3) . . . . ? N3 Yb1 C2 N6 91(3) 7_556 . . . ? C1 Yb1 C2 N6 55(3) 7_556 . . . ? C1 Yb1 C2 N6 -53(3) . . . . ? N2 Yb1 C2 N6 -53(3) . . . . ? Yb1 Yb1 C2 N6 -1(3) 7_556 . . . ? N2 Yb1 C2 N4 115.9(6) 7_556 . . . ? N1 Yb1 C2 N4 13.1(6) . . . . ? O1 Yb1 C2 N4 -86.6(6) . . . . ? N5 Yb1 C2 N4 -167.5(9) . . . . ? N3 Yb1 C2 N4 177.6(5) 7_556 . . . ? C1 Yb1 C2 N4 141.5(5) 7_556 . . . ? C1 Yb1 C2 N4 33.2(6) . . . . ? N2 Yb1 C2 N4 33.4(8) . . . . ? Yb1 Yb1 C2 N4 85.8(6) 7_556 . . . ? C1 N1 C3 C4 25.3(14) . . . . ? Yb1 N1 C3 C4 -167.1(7) . . . . ? C1 N1 C3 C12 -163.2(9) . . . . ? Yb1 N1 C3 C12 4.4(14) . . . . ? N1 C3 C4 C5 172.7(9) . . . . ? C12 C3 C4 C5 1.2(15) . . . . ? C3 C4 C5 C6 -4.4(17) . . . . ? C4 C5 C6 C7 2.2(17) . . . . ? C5 C6 C7 C8 -176.9(10) . . . . ? C5 C6 C7 C12 3.2(15) . . . . ? C6 C7 C8 C9 175.8(10) . . . . ? C12 C7 C8 C9 -4.3(16) . . . . ? C7 C8 C9 C10 6.5(18) . . . . ? C8 C9 C10 C11 -1.8(18) . . . . ? C9 C10 C11 N4 177.3(10) . . . . ? C9 C10 C11 C12 -5.0(16) . . . . ? C2 N4 C11 C10 -12.8(15) . . . . ? Yb1 N4 C11 C10 134.4(9) . . . . ? C2 N4 C11 C12 169.4(9) . . . . ? Yb1 N4 C11 C12 -43.4(13) . . . . ? C6 C7 C12 C11 177.7(9) . . . . ? C8 C7 C12 C11 -2.2(14) . . . . ? C6 C7 C12 C3 -6.1(14) . . . . ? C8 C7 C12 C3 174.0(9) . . . . ? C10 C11 C12 C7 6.8(14) . . . . ? N4 C11 C12 C7 -175.4(9) . . . . ? C10 C11 C12 C3 -169.0(10) . . . . ? N4 C11 C12 C3 8.8(14) . . . . ? C4 C3 C12 C7 3.9(13) . . . . ? N1 C3 C12 C7 -167.7(8) . . . . ? C4 C3 C12 C11 179.9(9) . . . . ? N1 C3 C12 C11 8.2(14) . . . . ? C1 N2 C13 C15 154.6(8) . . . . ? Yb1 N2 C13 C15 -0.6(13) 7_556 . . . ? Yb1 N2 C13 C15 -129.3(7) . . . . ? C1 N2 C13 C14 31.9(12) . . . . ? Yb1 N2 C13 C14 -123.4(9) 7_556 . . . ? Yb1 N2 C13 C14 108.0(8) . . . . ? C1 N3 C16 C18 131.5(9) . . . . ? Yb1 N3 C16 C18 -3.1(13) 7_556 . . . ? C1 N3 C16 C17 -110.2(9) . . . . ? Yb1 N3 C16 C17 115.2(9) 7_556 . . . ? C2 N5 C19 C21 -159.5(9) . . . . ? Yb1 N5 C19 C21 -12.1(16) . . . . ? C2 N5 C19 C20 79.0(11) . . . . ? Yb1 N5 C19 C20 -133.6(9) . . . . ? C2 N6 C22 C23 -96.4(12) . . . . ? C2 N6 C22 C24 142.6(11) . . . . ? C28 O1 C25 C26 -37.8(13) . . . . ? Yb1 O1 C25 C26 107.9(10) . . . . ? O1 C25 C26 C27 32.4(14) . . . . ? C25 C26 C27 C28 -15.0(14) . . . . ? C25 O1 C28 C27 28.3(13) . . . . ? Yb1 O1 C28 C27 -119.2(9) . . . . ? C26 C27 C28 O1 -7.5(14) . . . . ? C32 O2 C29 C30 -44(5) . . . . ? C32' O2' C29' C30' 27(6) . . . . ? O2 C29 C30 C31 48(4) . . . . ? O2' C29' C30' C31' -7(5) . . . . ? C29 C30 C31 C32 -30(4) . . . . ? C29' C30' C31' C32' -14(4) . . . . ? C29 O2 C32 C31 26(6) . . . . ? C30 C31 C32 O2 4(5) . . . . ? C29' O2' C32' C31' -34(6) . . . . ? C30' C31' C32' O2' 28(5) . . . . ? O3 O3 C33 C36 166(20) 2_755 . . 2_755 ? C33 O3 C33 C36 -134(19) 2_755 . . 2_755 ? C36 O3 C33 C36 -145(20) . . . 2_755 ? O3 O3 C33 C35 -107(3) 2_755 . . 2_755 ? C36 O3 C33 C35 88(19) 2_755 . . 2_755 ? C33 O3 C33 C35 -46(2) 2_755 . . 2_755 ? C36 O3 C33 C35 -57(4) . . . 2_755 ? C36 O3 C33 O3 -166(20) 2_755 . . 2_755 ? C33 O3 C33 O3 61(3) 2_755 . . 2_755 ? C36 O3 C33 O3 49(2) . . . 2_755 ? O3 O3 C33 C34 -89(3) 2_755 . . . ? C36 O3 C33 C34 106(20) 2_755 . . . ? C33 O3 C33 C34 -28(3) 2_755 . . . ? C36 O3 C33 C34 -40(4) . . . . ? C36 C33 C34 C35 -22(17) 2_755 . . 2_755 ? O3 C33 C34 C35 -116(12) 2_755 . . 2_755 ? O3 C33 C34 C35 -72(12) . . . 2_755 ? C36 C33 C34 C35 70(12) 2_755 . . . ? C35 C33 C34 C35 92(12) 2_755 . . . ? O3 C33 C34 C35 -24(3) 2_755 . . . ? O3 C33 C34 C35 20(4) . . . . ? C36 C33 C34 C34 52(12) 2_755 . . 2_755 ? C35 C33 C34 C34 74(11) 2_755 . . 2_755 ? O3 C33 C34 C34 -43(4) 2_755 . . 2_755 ? O3 C33 C34 C34 2(4) . . . 2_755 ? C35 C33 C34 C36 22(17) 2_755 . . 2_755 ? O3 C33 C34 C36 -94(11) 2_755 . . 2_755 ? O3 C33 C34 C36 -50(10) . . . 2_755 ? C35 C34 C35 C34 -15(19) 2_755 . . 2_755 ? C33 C34 C35 C34 -89(10) . . . 2_755 ? C36 C34 C35 C34 -80(11) 2_755 . . 2_755 ? C35 C34 C35 C33 71(11) 2_755 . . 2_755 ? C33 C34 C35 C33 -4(5) . . . 2_755 ? C34 C34 C35 C33 86(9) 2_755 . . 2_755 ? C36 C34 C35 C33 6(4) 2_755 . . 2_755 ? C35 C34 C35 C36 83(10) 2_755 . . . ? C33 C34 C35 C36 8(3) . . . . ? C34 C34 C35 C36 98(10) 2_755 . . . ? C36 C34 C35 C36 18(4) 2_755 . . . ? C33 C34 C35 C35 -75(10) . . . 2_755 ? C34 C34 C35 C35 15(19) 2_755 . . 2_755 ? C36 C34 C35 C35 -65(9) 2_755 . . 2_755 ? O3 O3 C36 C33 168(17) 2_755 . . 2_755 ? C36 O3 C36 C33 107(14) 2_755 . . 2_755 ? C33 O3 C36 C33 113(17) . . . 2_755 ? C36 O3 C36 O3 -62(4) 2_755 . . 2_755 ? C33 O3 C36 O3 -168(17) 2_755 . . 2_755 ? C33 O3 C36 O3 -56(3) . . . 2_755 ? O3 O3 C36 C35 100(3) 2_755 . . . ? C36 O3 C36 C35 39(3) 2_755 . . . ? C33 O3 C36 C35 -68(15) 2_755 . . . ? C33 O3 C36 C35 45(4) . . . . ? O3 O3 C36 C34 113(3) 2_755 . . 2_755 ? C36 O3 C36 C34 51(2) 2_755 . . 2_755 ? C33 O3 C36 C34 -55(14) 2_755 . . 2_755 ? C33 O3 C36 C34 58(4) . . . 2_755 ? C34 C35 C36 C33 -21(16) 2_755 . . 2_755 ? C34 C35 C36 C33 -106(11) . . . 2_755 ? C35 C35 C36 C33 -90(11) 2_755 . . 2_755 ? C34 C35 C36 O3 99(13) 2_755 . . 2_755 ? C33 C35 C36 O3 120(12) 2_755 . . 2_755 ? C34 C35 C36 O3 13(4) . . . 2_755 ? C35 C35 C36 O3 30(4) 2_755 . . 2_755 ? C34 C35 C36 O3 52(13) 2_755 . . . ? C33 C35 C36 O3 73(11) 2_755 . . . ? C34 C35 C36 O3 -34(3) . . . . ? C35 C35 C36 O3 -17(4) 2_755 . . . ? C33 C35 C36 C34 21(16) 2_755 . . 2_755 ? C34 C35 C36 C34 -86(13) . . . 2_755 ? C35 C35 C36 C34 -69(11) 2_755 . . 2_755 ? O4 O4 C37 C40 38(9) 2 . . 2 ? C40 O4 C37 C40 124(7) . . . 2 ? C37 O4 C37 C40 106(11) 2 . . 2 ? O4 O4 C37 C39 -76(11) 2 . . 2 ? C40 O4 C37 C39 11(13) . . . 2 ? C37 O4 C37 C39 -7(10) 2 . . 2 ? C40 O4 C37 C39 -113(15) 2 . . 2 ? C40 O4 C37 O4 87(7) . . . 2 ? C37 O4 C37 O4 69(4) 2 . . 2 ? C40 O4 C37 O4 -38(9) 2 . . 2 ? O4 O4 C37 C38 -73(5) 2 . . . ? C40 O4 C37 C38 13(7) . . . . ? C37 O4 C37 C38 -4(4) 2 . . . ? C40 O4 C37 C38 -111(11) 2 . . . ? O4 O4 C37 C38 -107(6) 2 . . 2 ? C40 O4 C37 C38 -21(7) . . . 2 ? C37 O4 C37 C38 -39(3) 2 . . 2 ? C40 O4 C37 C38 -145(12) 2 . . 2 ? O4 O4 C37 C37 -69(4) 2 . . 2 ? C40 O4 C37 C37 18(6) . . . 2 ? C40 O4 C37 C37 -106(11) 2 . . 2 ? C40 C37 C38 C39 71(10) 2 . . 2 ? O4 C37 C38 C39 141(11) 2 . . 2 ? O4 C37 C38 C39 -177(11) . . . 2 ? C38 C37 C38 C39 -114(10) 2 . . 2 ? C37 C37 C38 C39 179(12) 2 . . 2 ? C40 C37 C38 C38 -174(10) 2 . . 2 ? C39 C37 C38 C38 114(10) 2 . . 2 ? O4 C37 C38 C38 -105(7) 2 . . 2 ? O4 C37 C38 C38 -63(7) . . . 2 ? C37 C37 C38 C38 -67(6) 2 . . 2 ? C40 C37 C38 C39 -147(9) 2 . . . ? C39 C37 C38 C39 142(11) 2 . . . ? O4 C37 C38 C39 -77(6) 2 . . . ? O4 C37 C38 C39 -35(7) . . . . ? C38 C37 C38 C39 28(6) 2 . . . ? C37 C37 C38 C39 -39(5) 2 . . . ? C40 C37 C38 C37 -108(8) 2 . . 2 ? C39 C37 C38 C37 -179(12) 2 . . 2 ? O4 C37 C38 C37 -38(3) 2 . . 2 ? O4 C37 C38 C37 4(4) . . . 2 ? C38 C37 C38 C37 67(6) 2 . . 2 ? C39 C37 C38 C40 -71(10) 2 . . 2 ? O4 C37 C38 C40 70(6) 2 . . 2 ? O4 C37 C38 C40 112(9) . . . 2 ? C38 C37 C38 C40 174(10) 2 . . 2 ? C37 C37 C38 C40 108(8) 2 . . 2 ? C39 C38 C39 C38 -3(22) 2 . . 2 ? C37 C38 C39 C38 -48(9) . . . 2 ? C37 C38 C39 C38 -110(8) 2 . . 2 ? C40 C38 C39 C38 -64(10) 2 . . 2 ? C39 C38 C39 C37 108(16) 2 . . 2 ? C38 C38 C39 C37 110(8) 2 . . 2 ? C37 C38 C39 C37 63(8) . . . 2 ? C40 C38 C39 C37 46(7) 2 . . 2 ? C39 C38 C39 C40 93(16) 2 . . . ? C38 C38 C39 C40 95(8) 2 . . . ? C37 C38 C39 C40 48(7) . . . . ? C37 C38 C39 C40 -15(6) 2 . . . ? C40 C38 C39 C40 32(10) 2 . . . ? O4 O4 C40 C37 35(9) 2 . . 2 ? C37 O4 C40 C37 -33(11) . . . 2 ? C40 O4 C40 C37 -6(11) 2 . . 2 ? O4 O4 C40 C39 82(6) 2 . . . ? C37 O4 C40 C39 47(7) 2 . . . ? C37 O4 C40 C39 14(8) . . . . ? C40 O4 C40 C39 41(7) 2 . . . ? C37 O4 C40 O4 -35(9) 2 . . 2 ? C37 O4 C40 O4 -68(5) . . . 2 ? C40 O4 C40 O4 -41(3) 2 . . 2 ? O4 O4 C40 C38 86(3) 2 . . 2 ? C37 O4 C40 C38 51(7) 2 . . 2 ? C37 O4 C40 C38 18(6) . . . 2 ? C40 O4 C40 C38 45(5) 2 . . 2 ? C38 C39 C40 C37 69(12) 2 . . 2 ? C38 C39 C40 C37 25(10) . . . 2 ? C38 C39 C40 O4 8(11) 2 . . . ? C37 C39 C40 O4 -62(7) 2 . . . ? C38 C39 C40 O4 -37(8) . . . . ? C38 C39 C40 O4 42(10) 2 . . 2 ? C37 C39 C40 O4 -28(7) 2 . . 2 ? C38 C39 C40 O4 -3(6) . . . 2 ? C37 C39 C40 C38 -69(12) 2 . . 2 ? C38 C39 C40 C38 -44(9) . . . 2 ? C41 O5 C41 O5 -39(7) 2 . . 2 ? C42 O5 C41 O5 -123(6) 2 . . 2 ? C44 O5 C41 O5 -95(6) . . . 2 ? C41 O5 C41 C44 30(9) 2 . . 2 ? C42 O5 C41 C44 -54(8) 2 . . 2 ? C44 O5 C41 C44 -26(9) . . . 2 ? O5 O5 C41 C44 69(5) 2 . . 2 ? C41 O5 C41 C42 9(6) 2 . . . ? C42 O5 C41 C42 -75(6) 2 . . . ? C44 O5 C41 C42 -46(6) . . . . ? O5 O5 C41 C42 49(3) 2 . . . ? C42 O5 C41 C41 -84(3) 2 . . 2 ? C44 O5 C41 C41 -55(4) . . . 2 ? O5 O5 C41 C41 39(7) 2 . . 2 ? C41 O5 C41 C43 80(4) 2 . . 2 ? C42 O5 C41 C43 -4(4) 2 . . 2 ? C44 O5 C41 C43 25(5) . . . 2 ? O5 O5 C41 C43 120(4) 2 . . 2 ? C41 O5 C41 C42 84(3) 2 . . 2 ? C44 O5 C41 C42 29(3) . . . 2 ? O5 O5 C41 C42 123(6) 2 . . 2 ? O5 C41 C42 C44 -152(11) 2 . . 2 ? O5 C41 C42 C44 141(9) . . . 2 ? C41 C41 C42 C44 147(9) 2 . . 2 ? C43 C41 C42 C44 57(6) 2 . . 2 ? C42 C41 C42 C44 102(8) 2 . . 2 ? C44 C41 C42 O5 152(11) 2 . . 2 ? O5 C41 C42 O5 -66(5) . . . 2 ? C41 C41 C42 O5 -61(4) 2 . . 2 ? C43 C41 C42 O5 -151(6) 2 . . 2 ? C42 C41 C42 O5 -106(5) 2 . . 2 ? O5 C41 C42 C43 107(6) 2 . . . ? C44 C41 C42 C43 -101(9) 2 . . . ? O5 C41 C42 C43 40(6) . . . . ? C41 C41 C42 C43 46(3) 2 . . . ? C43 C41 C42 C43 -44(4) 2 . . . ? C42 C41 C42 C43 0(4) 2 . . . ? O5 C41 C42 C41 61(4) 2 . . 2 ? C44 C41 C42 C41 -147(9) 2 . . 2 ? O5 C41 C42 C41 -6(4) . . . 2 ? C43 C41 C42 C41 -90(3) 2 . . 2 ? C42 C41 C42 C41 -45(2) 2 . . 2 ? O5 C41 C42 C43 151(6) 2 . . 2 ? C44 C41 C42 C43 -57(6) 2 . . 2 ? O5 C41 C42 C43 84(4) . . . 2 ? C41 C41 C42 C43 90(3) 2 . . 2 ? C42 C41 C42 C43 45(2) 2 . . 2 ? C44 C42 C43 C44 -68(7) 2 . . . ? O5 C42 C43 C44 26(6) 2 . . . ? C41 C42 C43 C44 -17(5) . . . . ? C41 C42 C43 C44 30(4) 2 . . . ? C43 C42 C43 C44 -60(4) 2 . . . ? C44 C42 C43 C41 -98(8) 2 . . 2 ? O5 C42 C43 C41 -4(4) 2 . . 2 ? C41 C42 C43 C41 -47(5) . . . 2 ? C43 C42 C43 C41 -90(3) 2 . . 2 ? C44 C42 C43 C43 -8(6) 2 . . 2 ? O5 C42 C43 C43 86(4) 2 . . 2 ? C41 C42 C43 C43 43(3) . . . 2 ? C41 C42 C43 C43 90(3) 2 . . 2 ? O5 C42 C43 C44 94(6) 2 . . 2 ? C41 C42 C43 C44 51(5) . . . 2 ? C41 C42 C43 C44 98(8) 2 . . 2 ? C43 C42 C43 C44 8(6) 2 . . 2 ? C44 C42 C43 C42 -51(7) 2 . . 2 ? O5 C42 C43 C42 43(5) 2 . . 2 ? C41 C42 C43 C42 0(4) . . . 2 ? C41 C42 C43 C42 47(2) 2 . . 2 ? C43 C42 C43 C42 -44(2) 2 . . 2 ? C41 O5 C44 C42 -155(10) 2 . . 2 ? C41 O5 C44 C42 -71(8) . . . 2 ? O5 O5 C44 C42 -111(8) 2 . . 2 ? C42 O5 C44 C41 155(10) 2 . . 2 ? C41 O5 C44 C41 83(5) . . . 2 ? O5 O5 C44 C41 44(4) 2 . . 2 ? C41 O5 C44 C43 -48(6) 2 . . . ? C42 O5 C44 C43 107(8) 2 . . . ? C41 O5 C44 C43 36(6) . . . . ? O5 O5 C44 C43 -4(5) 2 . . . ? C41 O5 C44 C43 -107(6) 2 . . 2 ? C42 O5 C44 C43 48(5) 2 . . 2 ? C41 O5 C44 C43 -23(5) . . . 2 ? O5 O5 C44 C43 -63(4) 2 . . 2 ? C42 C43 C44 C42 55(7) . . . 2 ? C41 C43 C44 C42 99(7) 2 . . 2 ? C43 C43 C44 C42 -8(7) 2 . . 2 ? C44 C43 C44 C42 34(8) 2 . . 2 ? C42 C43 C44 C41 -44(5) . . . 2 ? C43 C43 C44 C41 -107(4) 2 . . 2 ? C44 C43 C44 C41 -65(4) 2 . . 2 ? C42 C43 C44 C41 -99(7) 2 . . 2 ? C42 C43 C44 O5 -11(5) . . . . ? C41 C43 C44 O5 33(3) 2 . . . ? C43 C43 C44 O5 -74(4) 2 . . . ? C44 C43 C44 O5 -32(5) 2 . . . ? C42 C43 C44 O5 -66(6) 2 . . . ? C42 C43 C44 C43 63(4) . . . 2 ? C41 C43 C44 C43 107(4) 2 . . 2 ? C44 C43 C44 C43 42(3) 2 . . 2 ? C42 C43 C44 C43 8(7) 2 . . 2 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.919 _refine_diff_density_min -1.152 _refine_diff_density_rms 0.186 data_complex5 _database_code_depnum_ccdc_archive 'CCDC 909533' #TrackingRef '909533.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H86 N12 O2 Y2, 5(C4 H8 O)' _chemical_formula_sum 'C76 H126 N12 O7 Y2' _chemical_formula_weight 1497.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.2799(11) _cell_length_b 18.1316(7) _cell_length_c 16.7684(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.244(4) _cell_angle_gamma 90.00 _cell_volume 8002.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 6045 _cell_measurement_theta_min 3.1647 _cell_measurement_theta_max 29.4252 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3200 _exptl_absorpt_coefficient_mu 1.500 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.73019 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4692 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18163 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_unetI/netI 0.0534 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7422 _reflns_number_gt 5618 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.Their C41-C42,C42-C43,C43- C44,O5-C41,O5-C44,C37-C38,C38-C39,C39-C40,O4-C37,O4-C40,C33-C34,C34-C35, C35-C36,O3-C33,O3-C36,C29'-C30',C30'-C31',C31'-C32',O2'-C29',O2'-C32',C29- C30,C30-C31,C31-C32,O2-C29 and O2-C32 distances were constrained. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+14.2119P] 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 7422 _refine_ls_number_parameters 416 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1374 _refine_ls_wR_factor_gt 0.1279 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.247111(12) 0.157056(18) 0.430264(19) 0.02153(13) Uani 1 1 d . . . O1 O 0.19982(11) 0.13176(16) 0.29123(15) 0.0377(7) Uani 1 1 d . . . O2 O 0.3977(6) 0.8396(9) 0.4667(10) 0.1023(13) Uiso 0.50 1 d PD A 1 O2' O 0.3995(6) 0.8523(9) 0.4605(10) 0.1023(13) Uiso 0.50 1 d PD B 2 O3 O 1.0184(3) 0.1308(5) 0.2483(5) 0.0817(15) Uiso 0.50 1 d PD . 1 O4 O 0.0160(7) 0.4184(10) 0.2327(14) 0.209(6) Uiso 0.50 1 d PD . 1 O5 O 0.0293(5) 0.8100(8) 0.2559(9) 0.139(3) Uiso 0.50 1 d PD . 1 N1 N 0.18021(11) 0.15157(16) 0.49238(18) 0.0247(7) Uani 1 1 d . . . N2 N 0.19516(11) 0.27534(16) 0.47352(17) 0.0239(6) Uani 1 1 d . . . N3 N 0.20256(11) 0.24113(16) 0.60617(17) 0.0241(6) Uani 1 1 d . . . N4 N 0.23605(11) 0.03512(16) 0.46495(18) 0.0271(7) Uani 1 1 d . . . N5 N 0.30289(11) 0.05687(17) 0.41455(18) 0.0271(7) Uani 1 1 d . . . N6 N 0.30178(13) -0.05736(18) 0.4830(2) 0.0329(8) Uani 1 1 d D . . H6 H 0.3299(8) -0.068(2) 0.472(2) 0.032(11) Uiso 1 1 d D . . C1 C 0.18870(12) 0.22087(19) 0.5273(2) 0.0218(7) Uani 1 1 d . . . C2 C 0.28070(14) 0.00920(19) 0.4534(2) 0.0257(8) Uani 1 1 d . . . C3 C 0.14710(13) 0.0998(2) 0.5094(2) 0.0244(8) Uani 1 1 d . . . C4 C 0.10521(13) 0.1221(2) 0.5360(2) 0.0303(8) Uani 1 1 d . . . H4 H 0.1022 0.1720 0.5489 0.036 Uiso 1 1 calc R . . C5 C 0.06761(14) 0.0727(2) 0.5442(2) 0.0348(9) Uani 1 1 d . . . H5 H 0.0407 0.0894 0.5649 0.042 Uiso 1 1 calc R . . C6 C 0.06956(14) 0.0009(2) 0.5226(2) 0.0354(9) Uani 1 1 d . . . H6A H 0.0438 -0.0317 0.5277 0.043 Uiso 1 1 calc R . . C7 C 0.11015(14) -0.0251(2) 0.4925(2) 0.0300(8) Uani 1 1 d . . . C8 C 0.10982(16) -0.0991(2) 0.4649(3) 0.0409(10) Uani 1 1 d . . . H8 H 0.0832 -0.1307 0.4687 0.049 Uiso 1 1 calc R . . C9 C 0.14746(17) -0.1249(2) 0.4331(3) 0.0422(10) Uani 1 1 d . . . H9 H 0.1459 -0.1732 0.4122 0.051 Uiso 1 1 calc R . . C10 C 0.18849(15) -0.0793(2) 0.4315(2) 0.0356(9) Uani 1 1 d . . . H10 H 0.2139 -0.0979 0.4085 0.043 Uiso 1 1 calc R . . C11 C 0.19349(13) -0.00820(19) 0.4622(2) 0.0245(8) Uani 1 1 d . . . C12 C 0.15126(13) 0.0231(2) 0.4886(2) 0.0250(8) Uani 1 1 d . . . C13 C 0.15764(13) 0.2857(2) 0.3928(2) 0.0269(8) Uani 1 1 d . . . H13 H 0.1684 0.2561 0.3508 0.032 Uiso 1 1 calc R . . C14 C 0.10327(15) 0.2644(3) 0.3911(3) 0.0454(11) Uani 1 1 d . . . H14A H 0.1019 0.2122 0.4029 0.068 Uiso 1 1 calc R . . H14B H 0.0810 0.2748 0.3368 0.068 Uiso 1 1 calc R . . H14C H 0.0923 0.2927 0.4324 0.068 Uiso 1 1 calc R . . C15 C 0.15951(18) 0.3669(2) 0.3711(3) 0.0454(11) Uani 1 1 d . . . H15A H 0.1451 0.3961 0.4078 0.068 Uiso 1 1 calc R . . H15B H 0.1401 0.3748 0.3144 0.068 Uiso 1 1 calc R . . H15C H 0.1945 0.3815 0.3774 0.068 Uiso 1 1 calc R . . C16 C 0.20499(14) 0.1879(2) 0.6735(2) 0.0296(8) Uani 1 1 d . . . H16 H 0.2018 0.1373 0.6507 0.036 Uiso 1 1 calc R . . C17 C 0.16202(17) 0.2018(3) 0.7147(3) 0.0486(12) Uani 1 1 d . . . H17A H 0.1673 0.2489 0.7430 0.073 Uiso 1 1 calc R . . H17B H 0.1617 0.1629 0.7542 0.073 Uiso 1 1 calc R . . H17C H 0.1298 0.2025 0.6729 0.073 Uiso 1 1 calc R . . C18 C 0.25479(16) 0.1946(3) 0.7406(2) 0.0443(11) Uani 1 1 d . . . H18A H 0.2831 0.1880 0.7162 0.066 Uiso 1 1 calc R . . H18B H 0.2561 0.1570 0.7822 0.066 Uiso 1 1 calc R . . H18C H 0.2569 0.2429 0.7659 0.066 Uiso 1 1 calc R . . C19 C 0.35432(15) 0.0415(2) 0.4065(2) 0.0342(9) Uani 1 1 d . . . H19 H 0.3747 0.0193 0.4587 0.041 Uiso 1 1 calc R . . C20 C 0.35233(19) -0.0124(3) 0.3358(3) 0.0502(12) Uani 1 1 d . . . H20A H 0.3350 -0.0571 0.3448 0.075 Uiso 1 1 calc R . . H20B H 0.3866 -0.0245 0.3338 0.075 Uiso 1 1 calc R . . H20C H 0.3341 0.0100 0.2839 0.075 Uiso 1 1 calc R . . C21 C 0.37913(17) 0.1128(3) 0.3915(3) 0.0531(13) Uani 1 1 d . . . H21A H 0.3594 0.1350 0.3406 0.080 Uiso 1 1 calc R . . H21B H 0.4133 0.1028 0.3872 0.080 Uiso 1 1 calc R . . H21C H 0.3807 0.1464 0.4372 0.080 Uiso 1 1 calc R . . C22 C 0.29663(17) -0.0934(2) 0.5587(3) 0.0395(10) Uani 1 1 d . . . H22 H 0.2661 -0.0737 0.5729 0.047 Uiso 1 1 calc R . . C23 C 0.3433(2) -0.0773(3) 0.6299(3) 0.0616(14) Uani 1 1 d . . . H23A H 0.3735 -0.0951 0.6159 0.092 Uiso 1 1 calc R . . H23B H 0.3398 -0.1020 0.6795 0.092 Uiso 1 1 calc R . . H23C H 0.3461 -0.0245 0.6396 0.092 Uiso 1 1 calc R . . C24 C 0.2906(2) -0.1763(3) 0.5460(4) 0.0700(16) Uani 1 1 d . . . H24A H 0.2622 -0.1862 0.4986 0.105 Uiso 1 1 calc R . . H24B H 0.2843 -0.1988 0.5948 0.105 Uiso 1 1 calc R . . H24C H 0.3214 -0.1966 0.5363 0.105 Uiso 1 1 calc R . . C25 C 0.2216(2) 0.1021(3) 0.2279(3) 0.0544(13) Uani 1 1 d . . . H25A H 0.2588 0.1036 0.2458 0.065 Uiso 1 1 calc R . . H25B H 0.2100 0.1299 0.1762 0.065 Uiso 1 1 calc R . . C26 C 0.2028(3) 0.0246(3) 0.2173(3) 0.0818(19) Uani 1 1 d . . . H26A H 0.2255 -0.0083 0.2567 0.098 Uiso 1 1 calc R . . H26B H 0.2003 0.0070 0.1611 0.098 Uiso 1 1 calc R . . C27 C 0.1514(3) 0.0275(3) 0.2335(3) 0.086(2) Uani 1 1 d . . . H27A H 0.1472 -0.0132 0.2695 0.103 Uiso 1 1 calc R . . H27B H 0.1246 0.0243 0.1816 0.103 Uiso 1 1 calc R . . C28 C 0.14916(17) 0.1005(3) 0.2751(3) 0.0538(13) Uani 1 1 d . . . H28A H 0.1243 0.1331 0.2390 0.065 Uiso 1 1 calc R . . H28B H 0.1395 0.0935 0.3268 0.065 Uiso 1 1 calc R . . C29 C 0.4514(6) 0.8657(9) 0.4860(10) 0.1023(13) Uiso 0.50 1 d PD A 1 C29' C 0.4499(6) 0.8391(9) 0.5111(10) 0.1023(13) Uiso 0.50 1 d PD B 2 C30 C 0.4762(6) 0.7826(9) 0.4838(9) 0.1023(13) Uiso 0.50 1 d PD A 1 C30' C 0.4726(6) 0.7943(9) 0.4474(9) 0.1023(13) Uiso 0.50 1 d PD B 2 C31 C 0.4438(6) 0.7493(9) 0.4077(10) 0.1023(13) Uiso 0.50 1 d PD A 1 C31' C 0.4278(6) 0.7683(10) 0.3814(9) 0.1023(13) Uiso 0.50 1 d PD B 2 C32 C 0.3920(6) 0.7913(10) 0.3938(10) 0.1023(13) Uiso 0.50 1 d PD A 1 C32' C 0.3822(6) 0.7827(9) 0.4159(10) 0.1023(13) Uiso 0.50 1 d PD B 2 C33 C 0.9836(5) 0.0918(9) 0.1788(10) 0.0817(15) Uiso 0.50 1 d PD . 1 C34 C 0.9826(5) 0.0147(9) 0.2031(10) 0.0817(15) Uiso 0.50 1 d PD . 1 C35 C 0.9990(5) 0.0144(9) 0.2969(10) 0.0817(15) Uiso 0.50 1 d PD . 1 C36 C 1.0027(6) 0.0944(9) 0.3192(10) 0.0817(15) Uiso 0.50 1 d PD . 1 C37 C 0.0213(13) 0.4630(17) 0.3121(18) 0.209(6) Uiso 0.50 1 d PD . 1 C38 C 0.0221(10) 0.5325(16) 0.2674(19) 0.209(6) Uiso 0.50 1 d PD . 1 C39 C -0.0012(13) 0.5248(18) 0.1805(17) 0.209(6) Uiso 0.50 1 d PD . 1 C40 C -0.0078(13) 0.4500(17) 0.1536(16) 0.209(6) Uiso 0.50 1 d PD . 1 C41 C -0.0117(8) 0.7874(12) 0.2980(12) 0.139(3) Uiso 0.50 1 d PD . 1 C42 C -0.0476(8) 0.7459(12) 0.2269(12) 0.139(3) Uiso 0.50 1 d PD . 1 C43 C -0.0114(8) 0.6995(11) 0.2007(11) 0.139(3) Uiso 0.50 1 d PD . 1 C44 C 0.0388(8) 0.7333(10) 0.2294(12) 0.139(3) Uiso 0.50 1 d PD . 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.02417(19) 0.0176(2) 0.02420(19) -0.00146(14) 0.00880(13) -0.00357(15) O1 0.0439(16) 0.0360(16) 0.0308(14) -0.0075(12) 0.0054(12) -0.0043(14) N1 0.0253(15) 0.0189(16) 0.0318(16) -0.0018(13) 0.0109(13) -0.0018(13) N2 0.0229(15) 0.0216(16) 0.0265(15) 0.0018(12) 0.0054(12) -0.0045(13) N3 0.0267(15) 0.0197(16) 0.0285(16) 0.0011(12) 0.0119(13) -0.0011(13) N4 0.0284(16) 0.0184(16) 0.0381(17) -0.0005(13) 0.0153(14) -0.0010(14) N5 0.0288(16) 0.0235(17) 0.0328(16) -0.0015(13) 0.0148(13) -0.0013(14) N6 0.0380(19) 0.0261(18) 0.0404(19) 0.0055(14) 0.0204(16) 0.0075(16) C1 0.0188(17) 0.0198(19) 0.0283(19) -0.0006(14) 0.0090(14) 0.0008(15) C2 0.033(2) 0.0176(19) 0.0288(19) -0.0048(15) 0.0116(16) 0.0004(16) C3 0.0241(18) 0.024(2) 0.0241(18) -0.0002(15) 0.0049(14) -0.0056(16) C4 0.0242(19) 0.031(2) 0.036(2) -0.0043(17) 0.0080(16) -0.0021(17) C5 0.0235(19) 0.043(3) 0.041(2) -0.0038(19) 0.0138(17) -0.0065(18) C6 0.0249(19) 0.035(2) 0.046(2) 0.0025(19) 0.0089(17) -0.0113(18) C7 0.0280(19) 0.026(2) 0.034(2) 0.0043(16) 0.0042(16) -0.0082(17) C8 0.038(2) 0.028(2) 0.055(3) 0.0035(19) 0.009(2) -0.0138(19) C9 0.047(3) 0.021(2) 0.055(3) -0.0042(19) 0.009(2) -0.006(2) C10 0.040(2) 0.026(2) 0.041(2) -0.0041(17) 0.0115(19) -0.0032(19) C11 0.0299(19) 0.0185(19) 0.0248(18) 0.0016(14) 0.0066(15) -0.0023(16) C12 0.0247(18) 0.023(2) 0.0254(18) 0.0024(15) 0.0040(14) -0.0048(16) C13 0.0260(18) 0.026(2) 0.0280(18) 0.0018(15) 0.0055(15) 0.0032(16) C14 0.028(2) 0.050(3) 0.051(3) 0.004(2) -0.0016(19) -0.001(2) C15 0.055(3) 0.035(2) 0.039(2) 0.0097(19) -0.001(2) 0.007(2) C16 0.040(2) 0.023(2) 0.0270(19) 0.0016(15) 0.0117(16) -0.0050(18) C17 0.050(3) 0.064(3) 0.037(2) 0.009(2) 0.022(2) -0.007(2) C18 0.043(2) 0.054(3) 0.035(2) 0.013(2) 0.0097(19) 0.000(2) C19 0.033(2) 0.031(2) 0.044(2) 0.0028(18) 0.0203(18) 0.0052(18) C20 0.067(3) 0.037(3) 0.059(3) -0.001(2) 0.040(2) 0.011(2) C21 0.041(2) 0.045(3) 0.086(4) -0.003(2) 0.038(3) -0.003(2) C22 0.049(2) 0.030(2) 0.044(2) 0.0112(19) 0.020(2) 0.008(2) C23 0.089(4) 0.049(3) 0.044(3) 0.005(2) 0.012(3) 0.000(3) C24 0.096(4) 0.031(3) 0.076(4) 0.018(2) 0.009(3) -0.007(3) C25 0.076(3) 0.054(3) 0.035(2) -0.011(2) 0.017(2) 0.005(3) C26 0.123(6) 0.054(4) 0.057(3) -0.027(3) 0.004(3) 0.005(4) C27 0.124(6) 0.066(4) 0.054(3) -0.015(3) 0.000(3) -0.043(4) C28 0.046(3) 0.058(3) 0.047(3) 0.001(2) -0.007(2) -0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N2 2.291(3) 7_556 ? Y1 N4 2.326(3) . ? Y1 N1 2.329(3) . ? Y1 O1 2.393(3) . ? Y1 N5 2.428(3) . ? Y1 N3 2.471(3) 7_556 ? Y1 N2 2.770(3) . ? Y1 C1 2.796(3) 7_556 ? Y1 C1 2.808(3) . ? Y1 C2 2.827(4) . ? O1 C25 1.450(5) . ? O1 C28 1.452(5) . ? O2 C32 1.478(16) . ? O2 C29 1.493(16) . ? O2' C29' 1.433(16) . ? O2' C32' 1.479(16) . ? O3 O3 1.019(14) 2_755 ? O3 C36 1.306(17) 2_755 ? O3 C33 1.425(17) 2_755 ? O3 C33 1.475(14) . ? O3 C36 1.517(15) . ? O4 O4 1.17(3) 2 ? O4 C37 1.36(3) 2 ? O4 C40 1.434(18) . ? O4 C37 1.533(17) . ? O5 C41 0.99(2) 2 ? O5 C42 1.27(2) 2 ? O5 C44 1.503(16) . ? O5 C41 1.527(15) . ? O5 O5 1.56(3) 2 ? N1 C1 1.380(4) . ? N1 C3 1.383(4) . ? N2 C1 1.379(4) . ? N2 C13 1.479(4) . ? N2 Y1 2.291(3) 7_556 ? N3 C1 1.329(4) . ? N3 C16 1.473(4) . ? N3 Y1 2.471(3) 7_556 ? N4 C2 1.366(4) . ? N4 C11 1.393(4) . ? N5 C2 1.321(4) . ? N5 C19 1.471(4) . ? N6 C2 1.372(5) . ? N6 C22 1.468(5) . ? N6 H6 0.854(10) . ? C1 Y1 2.796(3) 7_556 ? C3 C4 1.392(5) . ? C3 C12 1.445(5) . ? C4 C5 1.395(5) . ? C4 H4 0.9400 . ? C5 C6 1.356(6) . ? C5 H5 0.9400 . ? C6 C7 1.414(5) . ? C6 H6A 0.9400 . ? C7 C8 1.417(6) . ? C7 C12 1.437(5) . ? C8 C9 1.359(6) . ? C8 H8 0.9400 . ? C9 C10 1.397(6) . ? C9 H9 0.9400 . ? C10 C11 1.382(5) . ? C10 H10 0.9400 . ? C11 C12 1.454(5) . ? C13 C15 1.520(6) . ? C13 C14 1.526(5) . ? C13 H13 0.9900 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C18 1.524(6) . ? C16 C17 1.529(5) . ? C16 H16 0.9900 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C21 1.511(6) . ? C19 C20 1.528(6) . ? C19 H19 0.9900 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 C24 1.520(6) . ? C22 C23 1.526(7) . ? C22 H22 0.9900 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C26 1.492(7) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 C27 1.498(9) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.504(8) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.655(16) . ? C29' C30' 1.589(16) . ? C30 C31 1.477(16) . ? C30' C31' 1.491(16) . ? C31 C32 1.567(16) . ? C31' C32' 1.527(16) . ? C33 C36 0.37(2) 2_755 ? C33 O3 1.425(17) 2_755 ? C33 C34 1.457(15) . ? C33 C35 1.50(3) 2_755 ? C34 C35 0.50(2) 2_755 ? C34 C35 1.519(11) . ? C34 C36 1.57(3) 2_755 ? C34 C34 1.61(3) 2_755 ? C35 C34 0.50(2) 2_755 ? C35 C36 1.496(15) . ? C35 C33 1.50(3) 2_755 ? C35 C35 1.59(3) 2_755 ? C36 C33 0.37(2) 2_755 ? C36 O3 1.306(17) 2_755 ? C36 C34 1.57(3) 2_755 ? C37 C40 0.80(4) 2 ? C37 C39 1.27(4) 2 ? C37 O4 1.36(3) 2 ? C37 C38 1.468(19) . ? C37 C38 1.98(4) 2 ? C38 C39 1.17(4) 2 ? C38 C38 1.19(5) 2 ? C38 C39 1.435(19) . ? C38 C37 1.98(4) 2 ? C39 C38 1.17(4) 2 ? C39 C37 1.27(4) 2 ? C39 C40 1.427(19) . ? C40 C37 0.80(4) 2 ? C41 O5 0.99(2) 2 ? C41 C44 1.24(3) 2 ? C41 C42 1.527(17) . ? C41 C43 1.71(3) 2 ? C41 C41 1.88(4) 2 ? C41 C42 1.93(3) 2 ? C42 C44 0.75(3) 2 ? C42 O5 1.27(2) 2 ? C42 C43 1.452(17) . ? C42 C41 1.93(3) 2 ? C42 C43 1.93(3) 2 ? C43 C44 1.460(17) . ? C43 C43 1.61(4) 2 ? C43 C44 1.66(3) 2 ? C43 C41 1.71(3) 2 ? C43 C42 1.93(3) 2 ? C44 C42 0.75(3) 2 ? C44 C41 1.24(3) 2 ? C44 C43 1.66(3) 2 ? 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 Y1 N4 116.28(10) 7_556 . ? N2 Y1 N1 100.50(10) 7_556 . ? N4 Y1 N1 71.29(10) . . ? N2 Y1 O1 152.02(10) 7_556 . ? N4 Y1 O1 89.39(10) . . ? N1 Y1 O1 98.19(10) . . ? N2 Y1 N5 98.18(10) 7_556 . ? N4 Y1 N5 56.09(9) . . ? N1 Y1 N5 127.13(10) . . ? O1 Y1 N5 86.77(10) . . ? N2 Y1 N3 56.69(9) 7_556 7_556 ? N4 Y1 N3 152.74(10) . 7_556 ? N1 Y1 N3 133.95(10) . 7_556 ? O1 Y1 N3 95.42(9) . 7_556 ? N5 Y1 N3 97.31(10) . 7_556 ? N2 Y1 N2 72.89(10) 7_556 . ? N4 Y1 N2 124.16(9) . . ? N1 Y1 N2 53.20(9) . . ? O1 Y1 N2 102.80(9) . . ? N5 Y1 N2 170.38(9) . . ? N3 Y1 N2 80.92(9) 7_556 . ? N2 Y1 C1 29.38(10) 7_556 7_556 ? N4 Y1 C1 143.38(10) . 7_556 ? N1 Y1 C1 115.58(9) . 7_556 ? O1 Y1 C1 122.74(10) . 7_556 ? N5 Y1 C1 104.57(10) . 7_556 ? N3 Y1 C1 28.38(9) 7_556 7_556 ? N2 Y1 C1 69.49(9) . 7_556 ? N2 Y1 C1 76.20(10) 7_556 . ? N4 Y1 C1 96.67(10) . . ? N1 Y1 C1 29.30(10) . . ? O1 Y1 C1 113.61(10) . . ? N5 Y1 C1 146.96(10) . . ? N3 Y1 C1 105.79(9) 7_556 . ? N2 Y1 C1 28.62(9) . . ? C1 Y1 C1 86.51(9) 7_556 . ? N2 Y1 C2 105.83(10) 7_556 . ? N4 Y1 C2 28.71(10) . . ? N1 Y1 C2 99.33(10) . . ? O1 Y1 C2 91.38(10) . . ? N5 Y1 C2 27.81(9) . . ? N3 Y1 C2 124.13(10) 7_556 . ? N2 Y1 C2 150.24(9) . . ? C1 Y1 C2 123.86(10) 7_556 . ? C1 Y1 C2 121.62(10) . . ? C25 O1 C28 105.8(3) . . ? C25 O1 Y1 124.4(3) . . ? C28 O1 Y1 120.0(2) . . ? C32 O2 C29 104.5(14) . . ? C29' O2' C32' 106.6(14) . . ? O3 O3 C36 80.4(10) 2_755 2_755 ? O3 O3 C33 72.1(9) 2_755 2_755 ? C36 O3 C33 112.7(9) 2_755 2_755 ? O3 O3 C33 66.8(9) 2_755 . ? C36 O3 C33 13.6(10) 2_755 . ? C33 O3 C33 106.1(13) 2_755 . ? O3 O3 C36 58.1(9) 2_755 . ? C36 O3 C36 108.1(14) 2_755 . ? C33 O3 C36 14.0(9) 2_755 . ? C33 O3 C36 99.0(8) . . ? O4 O4 C37 74.0(17) 2 2 ? O4 O4 C40 104(3) 2 . ? C37 O4 C40 33.0(19) 2 . ? O4 O4 C37 58.7(18) 2 . ? C37 O4 C37 93(3) 2 . ? C40 O4 C37 121(2) . . ? C41 O5 C42 84.1(15) 2 2 ? C41 O5 C44 55.2(14) 2 . ? C42 O5 C44 29.7(11) 2 . ? C41 O5 C41 94(2) 2 . ? C42 O5 C41 86.6(17) 2 . ? C44 O5 C41 95.3(14) . . ? C41 O5 O5 69.6(16) 2 2 ? C42 O5 O5 111.0(12) 2 2 ? C44 O5 O5 102.3(11) . 2 ? C41 O5 O5 37.5(9) . 2 ? C1 N1 C3 125.2(3) . . ? C1 N1 Y1 94.97(19) . . ? C3 N1 Y1 138.7(2) . . ? C1 N2 C13 120.8(3) . . ? C1 N2 Y1 96.0(2) . 7_556 ? C13 N2 Y1 139.4(2) . 7_556 ? C1 N2 Y1 77.21(19) . . ? C13 N2 Y1 97.88(19) . . ? Y1 N2 Y1 107.11(10) 7_556 . ? C1 N3 C16 121.7(3) . . ? C1 N3 Y1 89.51(19) . 7_556 ? C16 N3 Y1 139.7(2) . 7_556 ? C2 N4 C11 124.6(3) . . ? C2 N4 Y1 96.4(2) . . ? C11 N4 Y1 133.6(2) . . ? C2 N5 C19 119.5(3) . . ? C2 N5 Y1 93.1(2) . . ? C19 N5 Y1 142.3(2) . . ? C2 N6 C22 125.4(3) . . ? C2 N6 H6 116(3) . . ? C22 N6 H6 112(3) . . ? N3 C1 N2 113.6(3) . . ? N3 C1 N1 130.3(3) . . ? N2 C1 N1 114.3(3) . . ? N3 C1 Y1 62.11(18) . 7_556 ? N2 C1 Y1 54.58(17) . 7_556 ? N1 C1 Y1 148.6(2) . 7_556 ? N3 C1 Y1 129.4(2) . . ? N2 C1 Y1 74.17(18) . . ? N1 C1 Y1 55.72(16) . . ? Y1 C1 Y1 93.49(9) 7_556 . ? N5 C2 N4 112.7(3) . . ? N5 C2 N6 123.5(3) . . ? N4 C2 N6 123.7(3) . . ? N5 C2 Y1 59.06(18) . . ? N4 C2 Y1 54.85(18) . . ? N6 C2 Y1 166.7(3) . . ? N1 C3 C4 120.3(3) . . ? N1 C3 C12 120.4(3) . . ? C4 C3 C12 118.7(3) . . ? C3 C4 C5 122.2(4) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C6 C5 C4 120.5(3) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 120.4(3) . . ? C5 C6 H6A 119.8 . . ? C7 C6 H6A 119.8 . . ? C6 C7 C8 119.6(3) . . ? C6 C7 C12 120.4(3) . . ? C8 C7 C12 119.9(3) . . ? C9 C8 C7 120.9(4) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 119.7(4) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 123.1(4) . . ? C11 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? C10 C11 N4 122.6(3) . . ? C10 C11 C12 118.0(3) . . ? N4 C11 C12 119.4(3) . . ? C7 C12 C3 117.6(3) . . ? C7 C12 C11 117.8(3) . . ? C3 C12 C11 124.6(3) . . ? N2 C13 C15 106.4(3) . . ? N2 C13 C14 114.9(3) . . ? C15 C13 C14 109.5(3) . . ? N2 C13 H13 108.6 . . ? C15 C13 H13 108.6 . . ? C14 C13 H13 108.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C18 111.4(3) . . ? N3 C16 C17 110.6(3) . . ? C18 C16 C17 107.1(3) . . ? N3 C16 H16 109.2 . . ? C18 C16 H16 109.2 . . ? C17 C16 H16 109.2 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N5 C19 C21 109.5(3) . . ? N5 C19 C20 110.6(3) . . ? C21 C19 C20 110.2(3) . . ? N5 C19 H19 108.9 . . ? C21 C19 H19 108.9 . . ? C20 C19 H19 108.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N6 C22 C24 110.5(4) . . ? N6 C22 C23 110.0(4) . . ? C24 C22 C23 109.7(4) . . ? N6 C22 H22 108.9 . . ? C24 C22 H22 108.9 . . ? C23 C22 H22 108.9 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O1 C25 C26 104.0(4) . . ? O1 C25 H25A 111.0 . . ? C26 C25 H25A 111.0 . . ? O1 C25 H25B 111.0 . . ? C26 C25 H25B 111.0 . . ? H25A C25 H25B 109.0 . . ? C25 C26 C27 104.7(5) . . ? C25 C26 H26A 110.8 . . ? C27 C26 H26A 110.8 . . ? C25 C26 H26B 110.8 . . ? C27 C26 H26B 110.8 . . ? H26A C26 H26B 108.9 . . ? C26 C27 C28 105.7(5) . . ? C26 C27 H27A 110.6 . . ? C28 C27 H27A 110.6 . . ? C26 C27 H27B 110.6 . . ? C28 C27 H27B 110.6 . . ? H27A C27 H27B 108.7 . . ? O1 C28 C27 106.1(4) . . ? O1 C28 H28A 110.5 . . ? C27 C28 H28A 110.5 . . ? O1 C28 H28B 110.5 . . ? C27 C28 H28B 110.5 . . ? H28A C28 H28B 108.7 . . ? O2 C29 C30 95.1(12) . . ? O2' C29' C30' 99.8(13) . . ? C31 C30 C29 103.7(12) . . ? C31' C30' C29' 105.9(13) . . ? C30 C31 C32 103.9(13) . . ? C30' C31' C32' 104.7(13) . . ? O2 C32 C31 105.7(14) . . ? O2' C32' C31' 98.8(13) . . ? C36 C33 O3 97(4) 2_755 2_755 ? C36 C33 C34 101(5) 2_755 . ? O3 C33 C34 103.2(13) 2_755 . ? C36 C33 O3 56(4) 2_755 . ? O3 C33 O3 41.1(7) 2_755 . ? C34 C33 O3 107.2(13) . . ? C36 C33 C35 82(5) 2_755 2_755 ? O3 C33 C35 108.2(13) 2_755 2_755 ? C34 C33 C35 19.5(8) . 2_755 ? O3 C33 C35 98.2(11) . 2_755 ? C35 C34 C33 85(3) 2_755 . ? C35 C34 C35 89(4) 2_755 . ? C33 C34 C35 105.7(16) . . ? C35 C34 C36 72(3) 2_755 2_755 ? C33 C34 C36 13.4(9) . 2_755 ? C35 C34 C36 103.1(14) . 2_755 ? C35 C34 C34 71(3) 2_755 2_755 ? C33 C34 C34 102.9(9) . 2_755 ? C35 C34 C34 18.2(8) . 2_755 ? C36 C34 C34 96.3(9) 2_755 2_755 ? C34 C35 C36 89(3) 2_755 . ? C34 C35 C33 75(3) 2_755 2_755 ? C36 C35 C33 14.2(9) . 2_755 ? C34 C35 C34 91(4) 2_755 . ? C36 C35 C34 103.7(15) . . ? C33 C35 C34 105.2(15) 2_755 . ? C34 C35 C35 73(3) 2_755 2_755 ? C36 C35 C35 103.3(8) . 2_755 ? C33 C35 C35 100.2(9) 2_755 2_755 ? C34 C35 C35 18.4(8) . 2_755 ? C33 C36 O3 110(4) 2_755 2_755 ? C33 C36 C35 84(5) 2_755 . ? O3 C36 C35 106.7(14) 2_755 . ? C33 C36 O3 69(4) 2_755 . ? O3 C36 O3 41.5(7) 2_755 . ? C35 C36 O3 103.8(12) . . ? C33 C36 C34 65(5) 2_755 2_755 ? O3 C36 C34 109.8(13) 2_755 2_755 ? C35 C36 C34 18.6(8) . 2_755 ? O3 C36 C34 94.0(11) . 2_755 ? C40 C37 C39 84(4) 2 2 ? C40 C37 O4 79(3) 2 2 ? C39 C37 O4 107(3) 2 2 ? C40 C37 C38 134(5) 2 . ? C39 C37 C38 50(2) 2 . ? O4 C37 C38 110(3) 2 . ? C40 C37 O4 121(4) 2 . ? C39 C37 O4 127(3) 2 . ? O4 C37 O4 47.3(17) 2 . ? C38 C37 O4 91(2) . . ? C40 C37 C38 112(4) 2 2 ? C39 C37 C38 46.2(14) 2 2 ? O4 C37 C38 77(2) 2 2 ? C38 C37 C38 36.7(19) . 2 ? O4 C37 C38 81(2) . 2 ? C39 C38 C38 75(3) 2 2 ? C39 C38 C39 125(3) 2 . ? C38 C38 C39 52(2) 2 . ? C39 C38 C37 56(3) 2 . ? C38 C38 C37 96(3) 2 . ? C39 C38 C37 112(3) . . ? C39 C38 C37 96(3) 2 2 ? C38 C38 C37 47.4(15) 2 2 ? C39 C38 C37 39.6(17) . 2 ? C37 C38 C37 73(2) . 2 ? C38 C39 C37 74(2) 2 2 ? C38 C39 C40 108(3) 2 . ? C37 C39 C40 34(2) 2 . ? C38 C39 C38 53(3) 2 . ? C37 C39 C38 94(2) 2 . ? C40 C39 C38 114(3) . . ? C37 C40 C39 62(3) 2 . ? C37 C40 O4 69(3) 2 . ? C39 C40 O4 96(2) . . ? O5 C41 C44 83.8(16) 2 2 ? O5 C41 O5 72.9(18) 2 . ? C44 C41 O5 118.6(18) 2 . ? O5 C41 C42 55.7(14) 2 . ? C44 C41 C42 28.9(11) 2 . ? O5 C41 C42 99.7(16) . . ? O5 C41 C43 119(2) 2 2 ? C44 C41 C43 56.7(12) 2 2 ? O5 C41 C43 86.8(14) . 2 ? C42 C41 C43 73.2(14) . 2 ? O5 C41 C41 54.1(15) 2 2 ? C44 C41 C41 89.2(15) 2 2 ? O5 C41 C41 31.8(9) . 2 ? C42 C41 C41 67.9(14) . 2 ? C43 C41 C41 78.8(9) 2 2 ? O5 C41 C42 101(2) 2 2 ? C44 C41 C42 93.7(17) 2 2 ? O5 C41 C42 41.1(9) . 2 ? C42 C41 C42 92.4(16) . 2 ? C43 C41 C42 46.6(9) 2 2 ? C41 C41 C42 47.3(8) 2 2 ? C44 C42 O5 93(2) 2 2 ? C44 C42 C43 93(3) 2 . ? O5 C42 C43 109.9(17) 2 . ? C44 C42 C41 54(2) 2 . ? O5 C42 C41 40.3(10) 2 . ? C43 C42 C41 99.9(16) . . ? C44 C42 C41 105(3) 2 2 ? O5 C42 C41 52.3(12) 2 2 ? C43 C42 C41 58.8(12) . 2 ? C41 C42 C41 64.8(15) . 2 ? C44 C42 C43 41(2) 2 2 ? O5 C42 C43 92.4(14) 2 2 ? C43 C42 C43 54.4(14) . 2 ? C41 C42 C43 57.8(13) . 2 ? C41 C42 C43 72.4(13) 2 2 ? C42 C43 C44 108.2(16) . . ? C42 C43 C43 78.3(14) . 2 ? C44 C43 C43 65.6(15) . 2 ? C42 C43 C44 26.6(11) . 2 ? C44 C43 C44 99.8(17) . 2 ? C43 C43 C44 53.0(10) 2 2 ? C42 C43 C41 74.6(14) . 2 ? C44 C43 C41 45.2(11) . 2 ? C43 C43 C41 86.9(10) 2 2 ? C44 C43 C41 83.1(13) 2 2 ? C42 C43 C42 94.5(16) . 2 ? C44 C43 C42 19.7(10) . 2 ? C43 C43 C42 47.3(8) 2 2 ? C44 C43 C42 81.5(12) 2 2 ? C41 C43 C42 49.1(8) 2 2 ? C42 C44 C41 97(2) 2 2 ? C42 C44 C43 119(3) 2 . ? C41 C44 C43 78.1(18) 2 . ? C42 C44 O5 57(2) 2 . ? C41 C44 O5 41.0(11) 2 . ? C43 C44 O5 105.4(16) . . ? C42 C44 C43 61(2) 2 2 ? C41 C44 C43 102.5(19) 2 2 ? C43 C44 C43 61.5(16) . 2 ? O5 C44 C43 89.3(13) . 2 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Y1 O1 C25 71.5(4) 7_556 . . . ? N4 Y1 O1 C25 -86.0(3) . . . . ? N1 Y1 O1 C25 -157.0(3) . . . . ? N5 Y1 O1 C25 -29.9(3) . . . . ? N3 Y1 O1 C25 67.1(3) 7_556 . . . ? N2 Y1 O1 C25 149.0(3) . . . . ? C1 Y1 O1 C25 75.3(3) 7_556 . . . ? C1 Y1 O1 C25 177.0(3) . . . . ? C2 Y1 O1 C25 -57.3(3) . . . . ? N2 Y1 O1 C28 -147.7(3) 7_556 . . . ? N4 Y1 O1 C28 54.8(3) . . . . ? N1 Y1 O1 C28 -16.1(3) . . . . ? N5 Y1 O1 C28 110.9(3) . . . . ? N3 Y1 O1 C28 -152.0(3) 7_556 . . . ? N2 Y1 O1 C28 -70.1(3) . . . . ? C1 Y1 O1 C28 -143.8(3) 7_556 . . . ? C1 Y1 O1 C28 -42.2(3) . . . . ? C2 Y1 O1 C28 83.5(3) . . . . ? N2 Y1 N1 C1 34.3(2) 7_556 . . . ? N4 Y1 N1 C1 148.7(2) . . . . ? O1 Y1 N1 C1 -124.8(2) . . . . ? N5 Y1 N1 C1 143.07(19) . . . . ? N3 Y1 N1 C1 -19.0(3) 7_556 . . . ? N2 Y1 N1 C1 -24.89(18) . . . . ? C1 Y1 N1 C1 7.6(3) 7_556 . . . ? C2 Y1 N1 C1 142.4(2) . . . . ? N2 Y1 N1 C3 -133.5(3) 7_556 . . . ? N4 Y1 N1 C3 -19.1(3) . . . . ? O1 Y1 N1 C3 67.4(4) . . . . ? N5 Y1 N1 C3 -24.7(4) . . . . ? N3 Y1 N1 C3 173.2(3) 7_556 . . . ? N2 Y1 N1 C3 167.3(4) . . . . ? C1 Y1 N1 C3 -160.1(3) 7_556 . . . ? C1 Y1 N1 C3 -167.8(5) . . . . ? C2 Y1 N1 C3 -25.3(4) . . . . ? N2 Y1 N2 C1 -92.5(2) 7_556 . . . ? N4 Y1 N2 C1 18.1(2) . . . . ? N1 Y1 N2 C1 25.47(18) . . . . ? O1 Y1 N2 C1 116.18(19) . . . . ? N5 Y1 N2 C1 -70.2(6) . . . . ? N3 Y1 N2 C1 -150.3(2) 7_556 . . . ? C1 Y1 N2 C1 -123.34(17) 7_556 . . . ? C2 Y1 N2 C1 -0.4(3) . . . . ? N2 Y1 N2 C13 147.6(2) 7_556 . . . ? N4 Y1 N2 C13 -101.9(2) . . . . ? N1 Y1 N2 C13 -94.5(2) . . . . ? O1 Y1 N2 C13 -3.8(2) . . . . ? N5 Y1 N2 C13 169.9(5) . . . . ? N3 Y1 N2 C13 89.78(19) 7_556 . . . ? C1 Y1 N2 C13 116.7(2) 7_556 . . . ? C1 Y1 N2 C13 -119.9(3) . . . . ? C2 Y1 N2 C13 -120.3(2) . . . . ? N2 Y1 N2 Y1 0.0 7_556 . . 7_556 ? N4 Y1 N2 Y1 110.54(12) . . . 7_556 ? N1 Y1 N2 Y1 117.93(15) . . . 7_556 ? O1 Y1 N2 Y1 -151.35(10) . . . 7_556 ? N5 Y1 N2 Y1 22.3(6) . . . 7_556 ? N3 Y1 N2 Y1 -57.81(11) 7_556 . . 7_556 ? C1 Y1 N2 Y1 -30.87(10) 7_556 . . 7_556 ? C1 Y1 N2 Y1 92.5(2) . . . 7_556 ? C2 Y1 N2 Y1 92.1(2) . . . 7_556 ? N2 Y1 N4 C2 -74.4(2) 7_556 . . . ? N1 Y1 N4 C2 -167.2(2) . . . . ? O1 Y1 N4 C2 94.0(2) . . . . ? N5 Y1 N4 C2 7.47(19) . . . . ? N3 Y1 N4 C2 -6.7(3) 7_556 . . . ? N2 Y1 N4 C2 -160.92(18) . . . . ? C1 Y1 N4 C2 -59.2(3) 7_556 . . . ? C1 Y1 N4 C2 -152.3(2) . . . . ? N2 Y1 N4 C11 131.8(3) 7_556 . . . ? N1 Y1 N4 C11 39.0(3) . . . . ? O1 Y1 N4 C11 -59.8(3) . . . . ? N5 Y1 N4 C11 -146.3(3) . . . . ? N3 Y1 N4 C11 -160.5(3) 7_556 . . . ? N2 Y1 N4 C11 45.3(3) . . . . ? C1 Y1 N4 C11 147.0(3) 7_556 . . . ? C1 Y1 N4 C11 53.9(3) . . . . ? C2 Y1 N4 C11 -153.8(4) . . . . ? N2 Y1 N5 C2 108.6(2) 7_556 . . . ? N4 Y1 N5 C2 -7.7(2) . . . . ? N1 Y1 N5 C2 -1.3(3) . . . . ? O1 Y1 N5 C2 -99.1(2) . . . . ? N3 Y1 N5 C2 165.8(2) 7_556 . . . ? N2 Y1 N5 C2 87.1(6) . . . . ? C1 Y1 N5 C2 137.8(2) 7_556 . . . ? C1 Y1 N5 C2 31.3(3) . . . . ? N2 Y1 N5 C19 -43.0(4) 7_556 . . . ? N4 Y1 N5 C19 -159.2(4) . . . . ? N1 Y1 N5 C19 -152.8(4) . . . . ? O1 Y1 N5 C19 109.4(4) . . . . ? N3 Y1 N5 C19 14.3(4) 7_556 . . . ? N2 Y1 N5 C19 -64.4(7) . . . . ? C1 Y1 N5 C19 -13.7(4) 7_556 . . . ? C1 Y1 N5 C19 -120.2(4) . . . . ? C2 Y1 N5 C19 -151.5(5) . . . . ? C16 N3 C1 N2 -171.7(3) . . . . ? Y1 N3 C1 N2 -18.7(3) 7_556 . . . ? C16 N3 C1 N1 -8.3(5) . . . . ? Y1 N3 C1 N1 144.8(3) 7_556 . . . ? C16 N3 C1 Y1 -153.0(3) . . . 7_556 ? C16 N3 C1 Y1 -83.2(4) . . . . ? Y1 N3 C1 Y1 69.8(3) 7_556 . . . ? C13 N2 C1 N3 -141.8(3) . . . . ? Y1 N2 C1 N3 20.3(3) 7_556 . . . ? Y1 N2 C1 N3 126.6(3) . . . . ? C13 N2 C1 N1 52.0(4) . . . . ? Y1 N2 C1 N1 -145.9(2) 7_556 . . . ? Y1 N2 C1 N1 -39.6(2) . . . . ? C13 N2 C1 Y1 -162.1(3) . . . 7_556 ? Y1 N2 C1 Y1 106.22(10) . . . 7_556 ? C13 N2 C1 Y1 91.6(3) . . . . ? Y1 N2 C1 Y1 -106.22(10) 7_556 . . . ? C3 N1 C1 N3 54.8(5) . . . . ? Y1 N1 C1 N3 -115.4(3) . . . . ? C3 N1 C1 N2 -141.9(3) . . . . ? Y1 N1 C1 N2 48.0(3) . . . . ? C3 N1 C1 Y1 156.9(3) . . . 7_556 ? Y1 N1 C1 Y1 -13.3(5) . . . 7_556 ? C3 N1 C1 Y1 170.2(4) . . . . ? N2 Y1 C1 N3 -28.3(3) 7_556 . . . ? N4 Y1 C1 N3 87.2(3) . . . . ? N1 Y1 C1 N3 116.9(4) . . . . ? O1 Y1 C1 N3 179.4(3) . . . . ? N5 Y1 C1 N3 55.4(4) . . . . ? N3 Y1 C1 N3 -77.2(3) 7_556 . . . ? N2 Y1 C1 N3 -107.8(4) . . . . ? C1 Y1 C1 N3 -56.2(3) 7_556 . . . ? C2 Y1 C1 N3 72.0(3) . . . . ? N2 Y1 C1 N2 79.5(2) 7_556 . . . ? N4 Y1 C1 N2 -165.02(18) . . . . ? N1 Y1 C1 N2 -135.3(3) . . . . ? O1 Y1 C1 N2 -72.8(2) . . . . ? N5 Y1 C1 N2 163.24(18) . . . . ? N3 Y1 C1 N2 30.6(2) 7_556 . . . ? C1 Y1 C1 N2 51.62(16) 7_556 . . . ? C2 Y1 C1 N2 179.79(17) . . . . ? N2 Y1 C1 N1 -145.2(2) 7_556 . . . ? N4 Y1 C1 N1 -29.7(2) . . . . ? O1 Y1 C1 N1 62.5(2) . . . . ? N5 Y1 C1 N1 -61.5(3) . . . . ? N3 Y1 C1 N1 165.87(19) 7_556 . . . ? N2 Y1 C1 N1 135.3(3) . . . . ? C1 Y1 C1 N1 -173.1(2) 7_556 . . . ? C2 Y1 C1 N1 -44.9(2) . . . . ? N2 Y1 C1 Y1 27.87(9) 7_556 . . 7_556 ? N4 Y1 C1 Y1 143.36(10) . . . 7_556 ? N1 Y1 C1 Y1 173.1(2) . . . 7_556 ? O1 Y1 C1 Y1 -124.38(10) . . . 7_556 ? N5 Y1 C1 Y1 111.61(17) . . . 7_556 ? N3 Y1 C1 Y1 -21.04(12) 7_556 . . 7_556 ? N2 Y1 C1 Y1 -51.62(16) . . . 7_556 ? C1 Y1 C1 Y1 0.0 7_556 . . 7_556 ? C2 Y1 C1 Y1 128.16(10) . . . 7_556 ? C19 N5 C2 N4 172.3(3) . . . . ? Y1 N5 C2 N4 11.8(3) . . . . ? C19 N5 C2 N6 -4.2(5) . . . . ? Y1 N5 C2 N6 -164.6(3) . . . . ? C19 N5 C2 Y1 160.4(3) . . . . ? C11 N4 C2 N5 144.7(3) . . . . ? Y1 N4 C2 N5 -12.4(3) . . . . ? C11 N4 C2 N6 -38.8(5) . . . . ? Y1 N4 C2 N6 164.0(3) . . . . ? C11 N4 C2 Y1 157.1(4) . . . . ? C22 N6 C2 N5 145.3(4) . . . . ? C22 N6 C2 N4 -30.7(6) . . . . ? C22 N6 C2 Y1 48.5(13) . . . . ? N2 Y1 C2 N5 -77.3(2) 7_556 . . . ? N4 Y1 C2 N5 166.6(3) . . . . ? N1 Y1 C2 N5 178.9(2) . . . . ? O1 Y1 C2 N5 80.4(2) . . . . ? N3 Y1 C2 N5 -17.1(2) 7_556 . . . ? N2 Y1 C2 N5 -160.3(2) . . . . ? C1 Y1 C2 N5 -51.5(2) 7_556 . . . ? C1 Y1 C2 N5 -160.6(2) . . . . ? N2 Y1 C2 N4 116.1(2) 7_556 . . . ? N1 Y1 C2 N4 12.3(2) . . . . ? O1 Y1 C2 N4 -86.2(2) . . . . ? N5 Y1 C2 N4 -166.6(3) . . . . ? N3 Y1 C2 N4 176.29(19) 7_556 . . . ? N2 Y1 C2 N4 33.0(3) . . . . ? C1 Y1 C2 N4 141.9(2) 7_556 . . . ? C1 Y1 C2 N4 32.8(2) . . . . ? N2 Y1 C2 N6 27.8(11) 7_556 . . . ? N4 Y1 C2 N6 -88.4(11) . . . . ? N1 Y1 C2 N6 -76.0(11) . . . . ? O1 Y1 C2 N6 -174.6(11) . . . . ? N5 Y1 C2 N6 105.0(12) . . . . ? N3 Y1 C2 N6 87.9(11) 7_556 . . . ? N2 Y1 C2 N6 -55.3(12) . . . . ? C1 Y1 C2 N6 53.5(11) 7_556 . . . ? C1 Y1 C2 N6 -55.5(11) . . . . ? C1 N1 C3 C4 26.5(5) . . . . ? Y1 N1 C3 C4 -168.4(3) . . . . ? C1 N1 C3 C12 -162.4(3) . . . . ? Y1 N1 C3 C12 2.7(5) . . . . ? N1 C3 C4 C5 172.1(3) . . . . ? C12 C3 C4 C5 0.8(5) . . . . ? C3 C4 C5 C6 -3.0(6) . . . . ? C4 C5 C6 C7 0.8(6) . . . . ? C5 C6 C7 C8 -175.7(4) . . . . ? C5 C6 C7 C12 3.4(6) . . . . ? C6 C7 C8 C9 177.8(4) . . . . ? C12 C7 C8 C9 -1.4(6) . . . . ? C7 C8 C9 C10 3.5(6) . . . . ? C8 C9 C10 C11 0.9(6) . . . . ? C9 C10 C11 N4 176.0(4) . . . . ? C9 C10 C11 C12 -7.1(6) . . . . ? C2 N4 C11 C10 -13.1(5) . . . . ? Y1 N4 C11 C10 134.7(3) . . . . ? C2 N4 C11 C12 170.1(3) . . . . ? Y1 N4 C11 C12 -42.1(5) . . . . ? C6 C7 C12 C3 -5.4(5) . . . . ? C8 C7 C12 C3 173.7(3) . . . . ? C6 C7 C12 C11 176.0(3) . . . . ? C8 C7 C12 C11 -4.8(5) . . . . ? N1 C3 C12 C7 -167.9(3) . . . . ? C4 C3 C12 C7 3.3(5) . . . . ? N1 C3 C12 C11 10.5(5) . . . . ? C4 C3 C12 C11 -178.2(3) . . . . ? C10 C11 C12 C7 8.9(5) . . . . ? N4 C11 C12 C7 -174.2(3) . . . . ? C10 C11 C12 C3 -169.6(3) . . . . ? N4 C11 C12 C3 7.4(5) . . . . ? C1 N2 C13 C15 151.3(3) . . . . ? Y1 N2 C13 C15 -0.8(5) 7_556 . . . ? Y1 N2 C13 C15 -128.9(3) . . . . ? C1 N2 C13 C14 29.9(5) . . . . ? Y1 N2 C13 C14 -122.1(3) 7_556 . . . ? Y1 N2 C13 C14 109.7(3) . . . . ? C1 N3 C16 C18 132.0(4) . . . . ? Y1 N3 C16 C18 -3.5(5) 7_556 . . . ? C1 N3 C16 C17 -108.9(4) . . . . ? Y1 N3 C16 C17 115.6(4) 7_556 . . . ? C2 N5 C19 C21 -158.1(4) . . . . ? Y1 N5 C19 C21 -11.3(6) . . . . ? C2 N5 C19 C20 80.3(4) . . . . ? Y1 N5 C19 C20 -132.9(3) . . . . ? C2 N6 C22 C24 141.3(4) . . . . ? C2 N6 C22 C23 -97.5(5) . . . . ? C28 O1 C25 C26 -37.8(5) . . . . ? Y1 O1 C25 C26 107.5(4) . . . . ? O1 C25 C26 C27 32.5(5) . . . . ? C25 C26 C27 C28 -15.3(6) . . . . ? C25 O1 C28 C27 28.1(5) . . . . ? Y1 O1 C28 C27 -119.0(4) . . . . ? C26 C27 C28 O1 -7.4(6) . . . . ? C32 O2 C29 C30 -49.7(15) . . . . ? C32' O2' C29' C30' 42.6(16) . . . . ? O2 C29 C30 C31 46.3(15) . . . . ? O2' C29' C30' C31' -17.7(17) . . . . ? C29 C30 C31 C32 -25.1(16) . . . . ? C29' C30' C31' C32' -11.8(17) . . . . ? C29 O2 C32 C31 37.5(17) . . . . ? C30 C31 C32 O2 -5.3(17) . . . . ? C29' O2' C32' C31' -50.7(16) . . . . ? C30' C31' C32' O2' 35.9(17) . . . . ? O3 O3 C33 C36 177(6) 2_755 . . 2_755 ? C33 O3 C33 C36 -121(5) 2_755 . . 2_755 ? C36 O3 C33 C36 -133(6) . . . 2_755 ? C36 O3 C33 O3 -177(6) 2_755 . . 2_755 ? C33 O3 C33 O3 61.8(10) 2_755 . . 2_755 ? C36 O3 C33 O3 49.5(8) . . . 2_755 ? O3 O3 C33 C34 -90.6(11) 2_755 . . . ? C36 O3 C33 C34 92(6) 2_755 . . . ? C33 O3 C33 C34 -28.7(10) 2_755 . . . ? C36 O3 C33 C34 -41.1(13) . . . . ? O3 O3 C33 C35 -108.3(11) 2_755 . . 2_755 ? C36 O3 C33 C35 74(5) 2_755 . . 2_755 ? C33 O3 C33 C35 -46.5(9) 2_755 . . 2_755 ? C36 O3 C33 C35 -58.8(13) . . . 2_755 ? C36 C33 C34 C35 -7(6) 2_755 . . 2_755 ? O3 C33 C34 C35 -107(4) 2_755 . . 2_755 ? O3 C33 C34 C35 -65(4) . . . 2_755 ? C36 C33 C34 C35 80(4) 2_755 . . . ? O3 C33 C34 C35 -20.0(13) 2_755 . . . ? O3 C33 C34 C35 22.5(14) . . . . ? C35 C33 C34 C35 87(4) 2_755 . . . ? O3 C33 C34 C36 -100(5) 2_755 . . 2_755 ? O3 C33 C34 C36 -58(4) . . . 2_755 ? C35 C33 C34 C36 7(6) 2_755 . . 2_755 ? C36 C33 C34 C34 62(5) 2_755 . . 2_755 ? O3 C33 C34 C34 -38.5(15) 2_755 . . 2_755 ? O3 C33 C34 C34 4.0(15) . . . 2_755 ? C35 C33 C34 C34 69(3) 2_755 . . 2_755 ? C35 C34 C35 C34 1(7) 2_755 . . 2_755 ? C33 C34 C35 C34 -83(4) . . . 2_755 ? C36 C34 C35 C34 -70(4) 2_755 . . 2_755 ? C35 C34 C35 C36 91(3) 2_755 . . . ? C33 C34 C35 C36 6.2(13) . . . . ? C36 C34 C35 C36 19.7(15) 2_755 . . . ? C34 C34 C35 C36 90(3) 2_755 . . . ? C35 C34 C35 C33 76(4) 2_755 . . 2_755 ? C33 C34 C35 C33 -8.4(16) . . . 2_755 ? C36 C34 C35 C33 5.2(14) 2_755 . . 2_755 ? C34 C34 C35 C33 75(3) 2_755 . . 2_755 ? C33 C34 C35 C35 -85(3) . . . 2_755 ? C36 C34 C35 C35 -71(3) 2_755 . . 2_755 ? C34 C34 C35 C35 -1(7) 2_755 . . 2_755 ? C34 C35 C36 C33 -7(5) 2_755 . . 2_755 ? C34 C35 C36 C33 -98(4) . . . 2_755 ? C35 C35 C36 C33 -79(4) 2_755 . . 2_755 ? C34 C35 C36 O3 103(4) 2_755 . . 2_755 ? C33 C35 C36 O3 109(4) 2_755 . . 2_755 ? C34 C35 C36 O3 11.4(14) . . . 2_755 ? C35 C35 C36 O3 30.3(16) 2_755 . . 2_755 ? C34 C35 C36 O3 60(4) 2_755 . . . ? C33 C35 C36 O3 66(4) 2_755 . . . ? C34 C35 C36 O3 -31.6(13) . . . . ? C35 C35 C36 O3 -12.6(16) 2_755 . . . ? C33 C35 C36 C34 7(5) 2_755 . . 2_755 ? C34 C35 C36 C34 -91(4) . . . 2_755 ? C35 C35 C36 C34 -72(3) 2_755 . . 2_755 ? O3 O3 C36 C33 177(6) 2_755 . . 2_755 ? C36 O3 C36 C33 112(5) 2_755 . . 2_755 ? C33 O3 C36 C33 122(6) . . . 2_755 ? C36 O3 C36 O3 -65.8(13) 2_755 . . 2_755 ? C33 O3 C36 O3 -177(6) 2_755 . . 2_755 ? C33 O3 C36 O3 -55.4(9) . . . 2_755 ? O3 O3 C36 C35 99.7(12) 2_755 . . . ? C36 O3 C36 C35 33.9(11) 2_755 . . . ? C33 O3 C36 C35 -78(5) 2_755 . . . ? C33 O3 C36 C35 44.3(13) . . . . ? O3 O3 C36 C34 115.7(12) 2_755 . . 2_755 ? C36 O3 C36 C34 49.9(8) 2_755 . . 2_755 ? C33 O3 C36 C34 -62(5) 2_755 . . 2_755 ? C33 O3 C36 C34 60.3(13) . . . 2_755 ? O4 O4 C37 C40 29(5) 2 . . 2 ? C37 O4 C37 C40 99(6) 2 . . 2 ? C40 O4 C37 C40 118(4) . . . 2 ? O4 O4 C37 C39 -79(4) 2 . . 2 ? C37 O4 C37 C39 -9(4) 2 . . 2 ? C40 O4 C37 C39 9(5) . . . 2 ? C37 O4 C37 O4 69(2) 2 . . 2 ? C40 O4 C37 O4 88(3) . . . 2 ? O4 O4 C37 C38 -116(3) 2 . . . ? C37 O4 C37 C38 -46.8(16) 2 . . . ? C40 O4 C37 C38 -28(3) . . . . ? O4 O4 C37 C38 -80.7(18) 2 . . 2 ? C37 O4 C37 C38 -11.3(16) 2 . . 2 ? C40 O4 C37 C38 8(3) . . . 2 ? C40 C37 C38 C39 3(6) 2 . . 2 ? O4 C37 C38 C39 97(4) 2 . . 2 ? O4 C37 C38 C39 141(4) . . . 2 ? C38 C37 C38 C39 67(3) 2 . . 2 ? C40 C37 C38 C38 -64(7) 2 . . 2 ? C39 C37 C38 C38 -67(3) 2 . . 2 ? O4 C37 C38 C38 29(4) 2 . . 2 ? O4 C37 C38 C38 74(3) . . . 2 ? C40 C37 C38 C39 -115(6) 2 . . . ? C39 C37 C38 C39 -118(3) 2 . . . ? O4 C37 C38 C39 -22(4) 2 . . . ? O4 C37 C38 C39 23(3) . . . . ? C38 C37 C38 C39 -51(2) 2 . . . ? C40 C37 C38 C37 -106(7) 2 . . 2 ? C39 C37 C38 C37 -110(3) 2 . . 2 ? O4 C37 C38 C37 -13.0(17) 2 . . 2 ? O4 C37 C38 C37 31.5(11) . . . 2 ? C38 C37 C38 C37 -42(3) 2 . . 2 ? C39 C38 C39 C38 17(6) 2 . . 2 ? C37 C38 C39 C38 80(3) . . . 2 ? C37 C38 C39 C38 66(2) 2 . . 2 ? C39 C38 C39 C37 -50(6) 2 . . 2 ? C38 C38 C39 C37 -66(2) 2 . . 2 ? C37 C38 C39 C37 13(4) . . . 2 ? C39 C38 C39 C40 -78(5) 2 . . . ? C38 C38 C39 C40 -95(3) 2 . . . ? C37 C38 C39 C40 -15(4) . . . . ? C37 C38 C39 C40 -29(2) 2 . . . ? C38 C39 C40 C37 3(5) 2 . . 2 ? C38 C39 C40 C37 59(4) . . . 2 ? C38 C39 C40 O4 -60(4) 2 . . . ? C37 C39 C40 O4 -62(3) 2 . . . ? C38 C39 C40 O4 -3(4) . . . . ? O4 O4 C40 C37 25(4) 2 . . 2 ? C37 O4 C40 C37 -37(5) . . . 2 ? O4 O4 C40 C39 82(2) 2 . . . ? C37 O4 C40 C39 57(3) 2 . . . ? C37 O4 C40 C39 21(4) . . . . ? C41 O5 C41 O5 -48(3) 2 . . 2 ? C42 O5 C41 O5 -132(2) 2 . . 2 ? C44 O5 C41 O5 -103(2) . . . 2 ? C41 O5 C41 C44 25(3) 2 . . 2 ? C42 O5 C41 C44 -59(3) 2 . . 2 ? C44 O5 C41 C44 -31(3) . . . 2 ? O5 O5 C41 C44 72.7(18) 2 . . 2 ? C41 O5 C41 C42 1(3) 2 . . . ? C42 O5 C41 C42 -82(2) 2 . . . ? C44 O5 C41 C42 -54(2) . . . . ? O5 O5 C41 C42 49.3(13) 2 . . . ? C41 O5 C41 C43 73.6(16) 2 . . 2 ? C42 O5 C41 C43 -10.2(14) 2 . . 2 ? C44 O5 C41 C43 18.3(16) . . . 2 ? O5 O5 C41 C43 121.7(17) 2 . . 2 ? C42 O5 C41 C41 -83.8(15) 2 . . 2 ? C44 O5 C41 C41 -55.4(15) . . . 2 ? O5 O5 C41 C41 48(3) 2 . . 2 ? C41 O5 C41 C42 83.8(15) 2 . . 2 ? C44 O5 C41 C42 28.4(12) . . . 2 ? O5 O5 C41 C42 132(2) 2 . . 2 ? O5 C41 C42 C44 -165(4) 2 . . 2 ? O5 C41 C42 C44 134(3) . . . 2 ? C43 C41 C42 C44 50(3) 2 . . 2 ? C41 C41 C42 C44 135(3) 2 . . 2 ? C42 C41 C42 C44 93(3) 2 . . 2 ? C44 C41 C42 O5 165(4) 2 . . 2 ? O5 C41 C42 O5 -61.4(18) . . . 2 ? C43 C41 C42 O5 -145(2) 2 . . 2 ? C41 C41 C42 O5 -60.7(16) 2 . . 2 ? C42 C41 C42 O5 -102(2) 2 . . 2 ? O5 C41 C42 C43 109(2) 2 . . . ? C44 C41 C42 C43 -86(3) 2 . . . ? O5 C41 C42 C43 48(2) . . . . ? C43 C41 C42 C43 -36.0(17) 2 . . . ? C41 C41 C42 C43 48.4(13) 2 . . . ? C42 C41 C42 C43 7.0(19) 2 . . . ? O5 C41 C42 C41 60.7(16) 2 . . 2 ? C44 C41 C42 C41 -135(3) 2 . . 2 ? O5 C41 C42 C41 -0.8(15) . . . 2 ? C43 C41 C42 C41 -84.4(13) 2 . . 2 ? C42 C41 C42 C41 -41.4(12) 2 . . 2 ? O5 C41 C42 C43 145(2) 2 . . 2 ? C44 C41 C42 C43 -50(3) 2 . . 2 ? O5 C41 C42 C43 83.7(16) . . . 2 ? C41 C41 C42 C43 84.4(13) 2 . . 2 ? C42 C41 C42 C43 43.0(9) 2 . . 2 ? C44 C42 C43 C44 -75(3) 2 . . . ? O5 C42 C43 C44 19(2) 2 . . . ? C41 C42 C43 C44 -21(2) . . . . ? C41 C42 C43 C44 30.8(14) 2 . . . ? C43 C42 C43 C44 -59.2(16) 2 . . . ? C44 C42 C43 C43 -16(2) 2 . . 2 ? O5 C42 C43 C43 78.2(16) 2 . . 2 ? C41 C42 C43 C43 37.7(15) . . . 2 ? C41 C42 C43 C43 90.0(13) 2 . . 2 ? O5 C42 C43 C44 94(3) 2 . . 2 ? C41 C42 C43 C44 54(2) . . . 2 ? C41 C42 C43 C44 106(3) 2 . . 2 ? C43 C42 C43 C44 16(2) 2 . . 2 ? C44 C42 C43 C41 -106(3) 2 . . 2 ? O5 C42 C43 C41 -11.8(17) 2 . . 2 ? C41 C42 C43 C41 -52.3(18) . . . 2 ? C43 C42 C43 C41 -90.0(13) 2 . . 2 ? C44 C42 C43 C42 -61(3) 2 . . 2 ? O5 C42 C43 C42 33.5(18) 2 . . 2 ? C41 C42 C43 C42 -7.0(18) . . . 2 ? C41 C42 C43 C42 45.3(9) 2 . . 2 ? C43 C42 C43 C42 -44.7(9) 2 . . 2 ? C42 C43 C44 C42 48(3) . . . 2 ? C43 C43 C44 C42 -20(3) 2 . . 2 ? C44 C43 C44 C42 22(4) 2 . . 2 ? C41 C43 C44 C42 92(3) 2 . . 2 ? C42 C43 C44 C41 -44.0(19) . . . 2 ? C43 C43 C44 C41 -111.5(15) 2 . . 2 ? C44 C43 C44 C41 -70.0(16) 2 . . 2 ? C42 C43 C44 C41 -92(3) 2 . . 2 ? C42 C43 C44 O5 -13(2) . . . . ? C43 C43 C44 O5 -80.5(13) 2 . . . ? C44 C43 C44 O5 -39.1(18) 2 . . . ? C41 C43 C44 O5 31.0(12) 2 . . . ? C42 C43 C44 O5 -61(3) 2 . . . ? C42 C43 C44 C43 67.5(17) . . . 2 ? C44 C43 C44 C43 41.5(14) 2 . . 2 ? C41 C43 C44 C43 111.5(15) 2 . . 2 ? C42 C43 C44 C43 20(3) 2 . . 2 ? C41 O5 C44 C42 -165(4) 2 . . 2 ? C41 O5 C44 C42 -74(3) . . . 2 ? O5 O5 C44 C42 -111(3) 2 . . 2 ? C42 O5 C44 C41 165(4) 2 . . 2 ? C41 O5 C44 C41 91(2) . . . 2 ? O5 O5 C44 C41 54.0(19) 2 . . 2 ? C41 O5 C44 C43 -50(2) 2 . . . ? C42 O5 C44 C43 115(3) 2 . . . ? C41 O5 C44 C43 41.3(19) . . . . ? O5 O5 C44 C43 4(2) 2 . . . ? C41 O5 C44 C43 -110(3) 2 . . 2 ? C42 O5 C44 C43 55(2) 2 . . 2 ? C41 O5 C44 C43 -18.8(18) . . . 2 ? O5 O5 C44 C43 -56.1(18) 2 . . 2 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.659 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.076 data_complex6 _database_code_depnum_ccdc_archive 'CCDC 909534' #TrackingRef '909534.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H82 Cl2 N14 Yb2, 3(C7 H8)' _chemical_formula_sum 'C81 H106 Cl2 N14 Yb2' _chemical_formula_weight 1692.78 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4364(18) _cell_length_b 12.8922(15) _cell_length_c 15.651(3) _cell_angle_alpha 72.96(2) _cell_angle_beta 84.03(3) _cell_angle_gamma 64.624(19) _cell_volume 1992.8(6) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10061 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.6 _exptl_crystal_description chip _exptl_crystal_colour orange _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 2.450 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.214 _exptl_absorpt_correction_T_max 0.378 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16645 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_unetI/netI 0.0754 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7370 _reflns_number_gt 6679 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Their N6-H6a,N7-H7,N3-H3a, C38-C44,C31-C37,C31-C32,C32-C33,C33-C34,C34-C35,C35-C36 and C36-C31 distances were constrained. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+2.9381P] 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 7370 _refine_ls_number_parameters 409 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1275 _refine_ls_wR_factor_gt 0.1167 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.06159(2) 1.00728(2) 0.389069(17) 0.02981(12) Uani 1 1 d . . . Cl1 Cl 0.5481(3) 1.2633(3) 0.17029(17) 0.0869(8) Uani 1 1 d . . . N1 N 0.1336(5) 0.8743(4) 0.5325(3) 0.0306(12) Uani 1 1 d . . . N2 N 0.1427(5) 0.9900(5) 0.6155(4) 0.0351(13) Uani 1 1 d . . . N3 N 0.3360(5) 0.8348(6) 0.5911(4) 0.0446(15) Uani 1 1 d D . . H3A H 0.372(7) 0.837(7) 0.644(3) 0.067 Uiso 1 1 d D . . N4 N 0.1938(5) 0.8326(5) 0.3633(3) 0.0343(12) Uani 1 1 d . . . N5 N 0.1218(5) 0.9923(5) 0.2434(4) 0.0338(12) Uani 1 1 d . . . N6 N 0.3009(6) 0.8192(6) 0.2241(4) 0.0497(16) Uani 1 1 d D . . H6A H 0.317(8) 0.859(7) 0.164(2) 0.075 Uiso 1 1 d D . . N7 N 0.1454(5) 1.1356(5) 0.3795(4) 0.0408(14) Uani 1 1 d D . . H7 H 0.100(6) 1.206(4) 0.400(5) 0.061 Uiso 1 1 d D . . C1 C 0.2076(6) 0.9014(6) 0.5813(4) 0.0349(15) Uani 1 1 d . . . C2 C 0.2056(6) 0.8804(6) 0.2744(4) 0.0354(15) Uani 1 1 d . . . C3 C 0.1571(5) 0.7498(6) 0.5579(4) 0.0331(15) Uani 1 1 d . . . C4 C 0.1601(6) 0.6951(7) 0.6481(5) 0.0468(18) Uani 1 1 d . . . H4 H 0.1612 0.7354 0.6890 0.056 Uiso 1 1 calc R . . C5 C 0.1615(7) 0.5792(7) 0.6810(6) 0.058(2) Uani 1 1 d . . . H5 H 0.1666 0.5419 0.7427 0.069 Uiso 1 1 calc R . . C6 C 0.1554(7) 0.5242(7) 0.6219(6) 0.058(2) Uani 1 1 d . . . H6 H 0.1507 0.4500 0.6440 0.069 Uiso 1 1 calc R . . C7 C 0.1556(6) 0.5716(6) 0.5290(5) 0.0434(18) Uani 1 1 d . . . C8 C 0.1526(7) 0.5092(7) 0.4702(6) 0.054(2) Uani 1 1 d . . . H8 H 0.1465 0.4357 0.4931 0.065 Uiso 1 1 calc R . . C9 C 0.1585(8) 0.5536(7) 0.3802(7) 0.059(2) Uani 1 1 d . . . H9 H 0.1522 0.5124 0.3415 0.071 Uiso 1 1 calc R . . C10 C 0.1738(7) 0.6602(7) 0.3448(6) 0.0498(19) Uani 1 1 d . . . H10 H 0.1804 0.6875 0.2826 0.060 Uiso 1 1 calc R . . C11 C 0.1795(6) 0.7262(6) 0.3981(5) 0.0375(16) Uani 1 1 d . . . C12 C 0.1637(5) 0.6863(6) 0.4945(5) 0.0350(15) Uani 1 1 d . . . C13 C 0.2075(6) 1.0441(7) 0.6531(5) 0.0459(18) Uani 1 1 d . . . H13 H 0.3022 0.9952 0.6552 0.055 Uiso 1 1 calc R . . C14 C 0.1623(10) 1.0479(10) 0.7468(6) 0.081(3) Uani 1 1 d . . . H14A H 0.0697 1.0960 0.7453 0.121 Uiso 1 1 calc R . . H14B H 0.2066 1.0828 0.7713 0.121 Uiso 1 1 calc R . . H14C H 0.1817 0.9674 0.7841 0.121 Uiso 1 1 calc R . . C15 C 0.1784(9) 1.1708(8) 0.5930(7) 0.073(3) Uani 1 1 d . . . H15A H 0.2076 1.1671 0.5331 0.110 Uiso 1 1 calc R . . H15B H 0.2233 1.2056 0.6170 0.110 Uiso 1 1 calc R . . H15C H 0.0859 1.2197 0.5911 0.110 Uiso 1 1 calc R . . C16 C 0.4203(7) 0.7639(7) 0.5322(5) 0.051(2) Uani 1 1 d . . . H16 H 0.3682 0.7761 0.4805 0.061 Uiso 1 1 calc R . . C17 C 0.5235(7) 0.8101(9) 0.4988(6) 0.068(3) Uani 1 1 d . . . H17A H 0.4826 0.8937 0.4658 0.103 Uiso 1 1 calc R . . H17B H 0.5811 0.7646 0.4600 0.103 Uiso 1 1 calc R . . H17C H 0.5728 0.8013 0.5494 0.103 Uiso 1 1 calc R . . C18 C 0.4810(7) 0.6308(8) 0.5822(7) 0.069(3) Uani 1 1 d . . . H18A H 0.5320 0.6183 0.6330 0.103 Uiso 1 1 calc R . . H18B H 0.5364 0.5859 0.5423 0.103 Uiso 1 1 calc R . . H18C H 0.4131 0.6039 0.6028 0.103 Uiso 1 1 calc R . . C19 C 0.1346(8) 1.0607(7) 0.1531(4) 0.0465(19) Uani 1 1 d . . . H19 H 0.2264 1.0459 0.1416 0.056 Uiso 1 1 calc R . . C20 C 0.0809(9) 1.0312(7) 0.0825(5) 0.061(2) Uani 1 1 d . . . H20A H 0.1245 0.9462 0.0885 0.091 Uiso 1 1 calc R . . H20B H 0.0951 1.0749 0.0234 0.091 Uiso 1 1 calc R . . H20C H -0.0112 1.0539 0.0906 0.091 Uiso 1 1 calc R . . C21 C 0.0516(9) 1.1954(7) 0.1482(5) 0.059(2) Uani 1 1 d . . . H21A H -0.0377 1.2085 0.1611 0.088 Uiso 1 1 calc R . . H21B H 0.0559 1.2445 0.0887 0.088 Uiso 1 1 calc R . . H21C H 0.0850 1.2168 0.1917 0.088 Uiso 1 1 calc R . . C22 C 0.4192(7) 0.7146(7) 0.2613(5) 0.053(2) Uani 1 1 d . . . H22 H 0.4013 0.6718 0.3212 0.064 Uiso 1 1 calc R . . C23 C 0.4606(9) 0.6314(8) 0.2008(6) 0.075(3) Uani 1 1 d . . . H23A H 0.3934 0.6054 0.1984 0.112 Uiso 1 1 calc R . . H23B H 0.5403 0.5624 0.2245 0.112 Uiso 1 1 calc R . . H23C H 0.4746 0.6737 0.1411 0.112 Uiso 1 1 calc R . . C24 C 0.5263(9) 0.7519(9) 0.2703(7) 0.076(3) Uani 1 1 d . . . H24A H 0.5445 0.7939 0.2118 0.114 Uiso 1 1 calc R . . H24B H 0.6039 0.6814 0.2956 0.114 Uiso 1 1 calc R . . H24C H 0.4984 0.8040 0.3092 0.114 Uiso 1 1 calc R . . C25 C 0.2389(6) 1.1651(6) 0.3321(4) 0.0342(15) Uani 1 1 d . . . C26 C 0.2327(7) 1.2803(7) 0.3097(5) 0.0477(18) Uani 1 1 d . . . H26 H 0.1629 1.3391 0.3301 0.057 Uiso 1 1 calc R . . C27 C 0.3248(8) 1.3118(7) 0.2589(5) 0.055(2) Uani 1 1 d . . . H27 H 0.3163 1.3910 0.2432 0.066 Uiso 1 1 calc R . . C28 C 0.4282(8) 1.2255(8) 0.2320(5) 0.055(2) Uani 1 1 d . . . C29 C 0.4397(7) 1.1103(8) 0.2519(5) 0.053(2) Uani 1 1 d . . . H29 H 0.5112 1.0524 0.2320 0.064 Uiso 1 1 calc R . . C30 C 0.3443(7) 1.0793(6) 0.3023(5) 0.0432(17) Uani 1 1 d . . . H30 H 0.3517 1.0007 0.3157 0.052 Uiso 1 1 calc R . . C31 C 0.2011(14) 0.5719(13) 0.0349(9) 0.128(5) Uiso 1 1 d D . . C32 C 0.1340(12) 0.5028(12) 0.0601(8) 0.106(4) Uiso 1 1 d D . . H32 H 0.1542 0.4362 0.0388 0.127 Uiso 1 1 calc R . . C33 C 0.0348(15) 0.5357(14) 0.1187(10) 0.145(6) Uiso 1 1 d D . . H33 H -0.0101 0.4869 0.1383 0.174 Uiso 1 1 calc R . . C34 C -0.0041(15) 0.6338(13) 0.1510(10) 0.131(5) Uiso 1 1 d D . . H34 H -0.0731 0.6553 0.1900 0.157 Uiso 1 1 calc R . . C35 C 0.0691(14) 0.6951(14) 0.1195(10) 0.139(5) Uiso 1 1 d D . . H35 H 0.0472 0.7635 0.1389 0.167 Uiso 1 1 calc R . . C36 C 0.1677(12) 0.6714(11) 0.0649(8) 0.104(4) Uiso 1 1 d D . . H36 H 0.2128 0.7201 0.0473 0.125 Uiso 1 1 calc R . . C37 C 0.3051(11) 0.5381(17) -0.0278(10) 0.199(8) Uiso 1 1 d D . . H37A H 0.3366 0.4535 -0.0222 0.299 Uiso 1 1 calc R . . H37B H 0.3753 0.5547 -0.0145 0.299 Uiso 1 1 calc R . . H37C H 0.2725 0.5837 -0.0883 0.299 Uiso 1 1 calc R . . C38 C 0.5603(9) 0.9174(10) 1.0023(8) 0.089(6) Uiso 0.50 1 d PRD . . C39 C 0.5829(9) 1.0018(10) 1.0280(8) 0.093(7) Uiso 0.50 1 d PRD . . C40 C 0.4858(9) 1.1165(10) 1.0168(8) 0.096(7) Uiso 0.50 1 d PR . . C41 C 0.3661(9) 1.1468(10) 0.9799(8) 0.143(12) Uiso 0.50 1 d PR . . C42 C 0.3435(9) 1.0624(10) 0.9542(8) 0.098(7) Uiso 0.50 1 d PR . . C43 C 0.4406(9) 0.9477(10) 0.9654(8) 0.086(6) Uiso 0.50 1 d PRD . . C44 C 0.651(3) 0.7917(19) 1.006(3) 0.176(15) 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 0.02363(16) 0.02715(18) 0.03709(19) -0.00850(13) -0.00024(11) -0.00924(12) Cl1 0.0775(17) 0.128(2) 0.0798(16) -0.0211(16) 0.0246(13) -0.0755(17) N1 0.025(3) 0.026(3) 0.036(3) -0.009(2) -0.002(2) -0.005(2) N2 0.019(3) 0.040(3) 0.049(3) -0.019(3) -0.004(2) -0.010(2) N3 0.020(3) 0.054(4) 0.055(4) -0.022(3) -0.007(2) -0.005(3) N4 0.035(3) 0.027(3) 0.033(3) -0.005(2) 0.004(2) -0.007(2) N5 0.029(3) 0.030(3) 0.043(3) -0.006(2) -0.001(2) -0.015(2) N6 0.050(4) 0.045(4) 0.036(3) -0.012(3) 0.008(3) -0.004(3) N7 0.039(3) 0.036(3) 0.059(4) -0.023(3) 0.007(3) -0.021(3) C1 0.028(3) 0.039(4) 0.036(4) -0.003(3) -0.006(3) -0.016(3) C2 0.036(4) 0.039(4) 0.036(4) -0.013(3) 0.001(3) -0.019(3) C3 0.018(3) 0.029(4) 0.044(4) -0.012(3) 0.005(3) -0.002(3) C4 0.032(4) 0.046(5) 0.049(5) -0.010(4) 0.003(3) -0.007(3) C5 0.042(4) 0.046(5) 0.060(5) 0.016(4) 0.003(4) -0.015(4) C6 0.042(4) 0.035(5) 0.080(6) 0.003(4) -0.002(4) -0.013(4) C7 0.020(3) 0.033(4) 0.072(5) -0.006(4) 0.006(3) -0.012(3) C8 0.041(4) 0.031(4) 0.100(7) -0.027(4) 0.009(4) -0.019(3) C9 0.050(5) 0.039(5) 0.097(7) -0.041(5) 0.006(5) -0.012(4) C10 0.045(4) 0.038(4) 0.066(5) -0.030(4) 0.001(4) -0.007(3) C11 0.023(3) 0.033(4) 0.051(4) -0.012(3) -0.001(3) -0.007(3) C12 0.008(3) 0.033(4) 0.064(5) -0.013(3) 0.002(3) -0.009(2) C13 0.024(3) 0.055(5) 0.071(5) -0.028(4) 0.000(3) -0.020(3) C14 0.092(7) 0.125(9) 0.068(6) -0.039(6) 0.001(5) -0.076(7) C15 0.080(7) 0.071(7) 0.094(7) -0.026(6) -0.011(5) -0.050(6) C16 0.033(4) 0.059(5) 0.058(5) -0.031(4) 0.001(3) -0.008(4) C17 0.030(4) 0.094(7) 0.076(6) -0.019(5) 0.003(4) -0.023(4) C18 0.030(4) 0.072(6) 0.100(7) -0.034(5) -0.002(4) -0.009(4) C19 0.076(5) 0.055(5) 0.022(3) -0.008(3) 0.012(3) -0.043(4) C20 0.081(6) 0.052(5) 0.039(4) -0.007(4) -0.011(4) -0.020(5) C21 0.080(6) 0.041(5) 0.043(5) -0.001(4) -0.012(4) -0.017(4) C22 0.041(4) 0.050(5) 0.048(5) -0.010(4) 0.004(3) -0.003(4) C23 0.064(6) 0.059(6) 0.081(7) -0.032(5) 0.015(5) -0.002(5) C24 0.052(5) 0.064(6) 0.096(7) -0.028(5) -0.008(5) -0.004(5) C25 0.032(3) 0.034(4) 0.042(4) -0.011(3) -0.003(3) -0.018(3) C26 0.043(4) 0.040(4) 0.065(5) -0.018(4) 0.000(4) -0.019(3) C27 0.060(5) 0.048(5) 0.070(5) -0.009(4) 0.003(4) -0.039(4) C28 0.050(5) 0.066(6) 0.049(5) -0.007(4) -0.001(4) -0.031(4) C29 0.041(4) 0.057(5) 0.052(5) -0.014(4) -0.003(4) -0.012(4) C30 0.043(4) 0.036(4) 0.050(4) -0.013(3) 0.005(3) -0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N7 2.205(5) . ? Yb1 N4 2.238(5) . ? Yb1 N2 2.330(5) 2_576 ? Yb1 N5 2.351(5) . ? Yb1 N1 2.361(5) . ? Yb1 N1 2.536(5) 2_576 ? Yb1 C2 2.721(7) . ? Yb1 C1 2.828(6) 2_576 ? Yb1 Yb1 3.5922(11) 2_576 ? Cl1 C28 1.753(8) . ? N1 C1 1.403(8) . ? N1 C3 1.443(8) . ? N1 Yb1 2.536(5) 2_576 ? N2 C1 1.300(8) . ? N2 C13 1.469(8) . ? N2 Yb1 2.330(5) 2_576 ? N3 C1 1.343(8) . ? N3 C16 1.471(9) . ? N3 H3A 0.970(10) . ? N4 C2 1.365(8) . ? N4 C11 1.393(8) . ? N5 C2 1.318(8) . ? N5 C19 1.461(8) . ? N6 C2 1.371(8) . ? N6 C22 1.459(9) . ? N6 H6A 0.970(10) . ? N7 C25 1.362(8) . ? N7 H7 0.966(10) . ? C1 Yb1 2.828(6) 2_576 ? C3 C4 1.377(10) . ? C3 C12 1.438(9) . ? C4 C5 1.425(10) . ? C4 H4 0.9400 . ? C5 C6 1.343(12) . ? C5 H5 0.9400 . ? C6 C7 1.402(11) . ? C6 H6 0.9400 . ? C7 C8 1.398(11) . ? C7 C12 1.459(9) . ? C8 C9 1.363(12) . ? C8 H8 0.9400 . ? C9 C10 1.402(11) . ? C9 H9 0.9400 . ? C10 C11 1.379(9) . ? C10 H10 0.9400 . ? C11 C12 1.463(10) . ? C13 C14 1.512(11) . ? C13 C15 1.536(11) . ? C13 H13 0.9900 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C17 1.521(11) . ? C16 C18 1.531(12) . ? C16 H16 0.9900 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C20 1.527(10) . ? C19 C21 1.564(11) . ? C19 H19 0.9900 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 C24 1.527(12) . ? C22 C23 1.528(11) . ? C22 H22 0.9900 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C30 1.392(9) . ? C25 C26 1.394(9) . ? C26 C27 1.383(10) . ? C26 H26 0.9400 . ? C27 C28 1.362(12) . ? C27 H27 0.9400 . ? C28 C29 1.374(11) . ? C29 C30 1.409(10) . ? C29 H29 0.9400 . ? C30 H30 0.9400 . ? C31 C32 1.362(13) . ? C31 C36 1.381(13) . ? C31 C37 1.460(13) . ? C32 C33 1.381(14) . ? C32 H32 0.9400 . ? C33 C34 1.377(14) . ? C33 H33 0.9400 . ? C34 C35 1.350(13) . ? C34 H34 0.9400 . ? C35 C36 1.324(13) . ? C35 H35 0.9400 . ? C36 H36 0.9400 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C38 C41 0.887(18) 2_677 ? C38 C40 0.93(2) 2_677 ? C38 C39 1.3900 . ? C38 C43 1.3908 . ? C38 C44 1.491(16) . ? C38 C42 1.50(2) 2_677 ? C38 C39 1.550(18) 2_677 ? C38 C43 1.94(2) 2_677 ? C38 C38 1.96(2) 2_677 ? C39 C43 0.62(2) 2_677 ? C39 C42 0.888(19) 2_677 ? C39 C40 1.3894 . ? C39 C38 1.550(18) 2_677 ? C39 C41 1.79(2) 2_677 ? C40 C43 0.887(19) 2_677 ? C40 C38 0.93(2) 2_677 ? C40 C41 1.3907 . ? C40 C44 1.50(3) 2_677 ? C41 C44 0.82(3) 2_677 ? C41 C38 0.887(19) 2_677 ? C41 C42 1.3901 . ? C41 C39 1.79(2) 2_677 ? C42 C39 0.888(19) 2_677 ? C42 C43 1.3895 . ? C42 C38 1.50(2) 2_677 ? C43 C39 0.62(2) 2_677 ? C43 C40 0.887(19) 2_677 ? C43 C38 1.94(2) 2_677 ? C44 C41 0.82(3) 2_677 ? C44 C40 1.50(3) 2_677 ? 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 N7 Yb1 N4 116.9(2) . . ? N7 Yb1 N2 138.0(2) . 2_576 ? N4 Yb1 N2 103.03(19) . 2_576 ? N7 Yb1 N5 92.7(2) . . ? N4 Yb1 N5 58.54(18) . . ? N2 Yb1 N5 97.56(18) 2_576 . ? N7 Yb1 N1 102.5(2) . . ? N4 Yb1 N1 75.36(18) . . ? N2 Yb1 N1 99.49(18) 2_576 . ? N5 Yb1 N1 133.34(18) . . ? N7 Yb1 N1 90.70(19) . 2_576 ? N4 Yb1 N1 149.12(18) . 2_576 ? N2 Yb1 N1 55.83(17) 2_576 2_576 ? N5 Yb1 N1 138.55(17) . 2_576 ? N1 Yb1 N1 85.69(17) . 2_576 ? N7 Yb1 C2 103.1(2) . . ? N4 Yb1 C2 29.98(19) . . ? N2 Yb1 C2 105.33(19) 2_576 . ? N5 Yb1 C2 28.96(18) . . ? N1 Yb1 C2 104.40(19) . . ? N1 Yb1 C2 160.39(18) 2_576 . ? N7 Yb1 C1 113.7(2) . 2_576 ? N4 Yb1 C1 129.22(19) . 2_576 ? N2 Yb1 C1 27.05(18) 2_576 2_576 ? N5 Yb1 C1 115.40(18) . 2_576 ? N1 Yb1 C1 98.38(18) . 2_576 ? N1 Yb1 C1 29.70(17) 2_576 2_576 ? C2 Yb1 C1 130.78(19) . 2_576 ? N7 Yb1 Yb1 98.71(16) . 2_576 ? N4 Yb1 Yb1 116.08(13) . 2_576 ? N2 Yb1 Yb1 73.25(14) 2_576 2_576 ? N5 Yb1 Yb1 168.57(12) . 2_576 ? N1 Yb1 Yb1 44.74(12) . 2_576 ? N1 Yb1 Yb1 40.95(11) 2_576 2_576 ? C2 Yb1 Yb1 145.93(14) . 2_576 ? C1 Yb1 Yb1 58.84(13) 2_576 2_576 ? C1 N1 C3 114.3(5) . . ? C1 N1 Yb1 115.4(4) . . ? C3 N1 Yb1 124.8(4) . . ? C1 N1 Yb1 86.8(4) . 2_576 ? C3 N1 Yb1 111.0(3) . 2_576 ? Yb1 N1 Yb1 94.31(17) . 2_576 ? C1 N2 C13 121.7(5) . . ? C1 N2 Yb1 98.3(4) . 2_576 ? C13 N2 Yb1 139.3(4) . 2_576 ? C1 N3 C16 127.2(6) . . ? C1 N3 H3A 112(5) . . ? C16 N3 H3A 121(5) . . ? C2 N4 C11 123.9(6) . . ? C2 N4 Yb1 95.0(4) . . ? C11 N4 Yb1 125.0(4) . . ? C2 N5 C19 119.8(6) . . ? C2 N5 Yb1 91.3(4) . . ? C19 N5 Yb1 143.4(4) . . ? C2 N6 C22 124.2(6) . . ? C2 N6 H6A 121(5) . . ? C22 N6 H6A 109(5) . . ? C25 N7 Yb1 137.5(5) . . ? C25 N7 H7 99(4) . . ? Yb1 N7 H7 121(5) . . ? N2 C1 N3 125.4(6) . . ? N2 C1 N1 115.4(5) . . ? N3 C1 N1 119.2(6) . . ? N2 C1 Yb1 54.6(3) . 2_576 ? N3 C1 Yb1 162.7(5) . 2_576 ? N1 C1 Yb1 63.5(3) . 2_576 ? N5 C2 N4 113.6(6) . . ? N5 C2 N6 123.6(6) . . ? N4 C2 N6 122.7(6) . . ? N5 C2 Yb1 59.7(3) . . ? N4 C2 Yb1 55.0(3) . . ? N6 C2 Yb1 166.8(5) . . ? C4 C3 C12 119.7(6) . . ? C4 C3 N1 116.6(6) . . ? C12 C3 N1 123.3(6) . . ? C3 C4 C5 121.8(8) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C6 C5 C4 118.6(8) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C5 C6 C7 123.5(7) . . ? C5 C6 H6 118.3 . . ? C7 C6 H6 118.3 . . ? C8 C7 C6 121.3(7) . . ? C8 C7 C12 120.2(7) . . ? C6 C7 C12 118.5(7) . . ? C9 C8 C7 120.9(7) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 120.5(8) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C11 C10 C9 122.2(8) . . ? C11 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C10 C11 N4 122.5(7) . . ? C10 C11 C12 118.8(6) . . ? N4 C11 C12 118.6(6) . . ? C3 C12 C7 117.5(6) . . ? C3 C12 C11 125.5(6) . . ? C7 C12 C11 117.0(6) . . ? N2 C13 C14 110.1(6) . . ? N2 C13 C15 109.6(6) . . ? C14 C13 C15 110.3(7) . . ? N2 C13 H13 108.9 . . ? C14 C13 H13 108.9 . . ? C15 C13 H13 108.9 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C17 107.5(6) . . ? N3 C16 C18 110.9(7) . . ? C17 C16 C18 111.2(6) . . ? N3 C16 H16 109.0 . . ? C17 C16 H16 109.0 . . ? C18 C16 H16 109.0 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N5 C19 C20 111.7(6) . . ? N5 C19 C21 106.6(6) . . ? C20 C19 C21 107.9(6) . . ? N5 C19 H19 110.2 . . ? C20 C19 H19 110.2 . . ? C21 C19 H19 110.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N6 C22 C24 110.5(7) . . ? N6 C22 C23 109.1(7) . . ? C24 C22 C23 110.7(7) . . ? N6 C22 H22 108.8 . . ? C24 C22 H22 108.8 . . ? C23 C22 H22 108.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N7 C25 C30 119.9(6) . . ? N7 C25 C26 122.6(6) . . ? C30 C25 C26 117.5(6) . . ? C27 C26 C25 122.9(7) . . ? C27 C26 H26 118.6 . . ? C25 C26 H26 118.6 . . ? C28 C27 C26 118.4(7) . . ? C28 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C27 C28 C29 121.4(7) . . ? C27 C28 Cl1 118.9(6) . . ? C29 C28 Cl1 119.7(7) . . ? C28 C29 C30 119.9(7) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C25 C30 C29 119.9(7) . . ? C25 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C32 C31 C36 121.0(13) . . ? C32 C31 C37 116.6(13) . . ? C36 C31 C37 122.4(13) . . ? C31 C32 C33 116.5(14) . . ? C31 C32 H32 121.8 . . ? C33 C32 H32 121.8 . . ? C34 C33 C32 125.7(16) . . ? C34 C33 H33 117.2 . . ? C32 C33 H33 117.2 . . ? C35 C34 C33 111.6(16) . . ? C35 C34 H34 124.2 . . ? C33 C34 H34 124.2 . . ? C36 C35 C34 128.4(16) . . ? C36 C35 H35 115.8 . . ? C34 C35 H35 115.8 . . ? C35 C36 C31 116.9(13) . . ? C35 C36 H36 121.5 . . ? C31 C36 H36 121.5 . . ? C31 C37 H37A 109.5 . . ? C31 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C31 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C41 C38 C40 100(2) 2_677 2_677 ? C41 C38 C39 101.1(15) 2_677 . ? C40 C38 C39 158.6(11) 2_677 . ? C41 C38 C43 138.7(15) 2_677 . ? C40 C38 C43 39.0(12) 2_677 . ? C39 C38 C43 120.0 . . ? C41 C38 C44 28.0(18) 2_677 . ? C40 C38 C44 72.6(18) 2_677 . ? C39 C38 C44 128.6(13) . . ? C43 C38 C44 111.3(13) . . ? C41 C38 C42 65.5(12) 2_677 2_677 ? C40 C38 C42 165(2) 2_677 2_677 ? C39 C38 C42 35.5(8) . 2_677 ? C43 C38 C42 155.4(8) . 2_677 ? C44 C38 C42 93.2(15) . 2_677 ? C41 C38 C39 162(2) 2_677 2_677 ? C40 C38 C39 62.4(10) 2_677 2_677 ? C39 C38 C39 96.4(8) . 2_677 ? C43 C38 C39 23.7(8) . 2_677 ? C44 C38 C39 135.0(17) . 2_677 ? C42 C38 C39 131.7(15) 2_677 2_677 ? C41 C38 C43 110.8(17) 2_677 2_677 ? C40 C38 C43 148.5(16) 2_677 2_677 ? C39 C38 C43 10.1(5) . 2_677 ? C43 C38 C43 110.1(5) . 2_677 ? C44 C38 C43 138.6(15) . 2_677 ? C42 C38 C43 45.4(6) 2_677 2_677 ? C39 C38 C43 86.4(9) 2_677 2_677 ? C41 C38 C38 152(2) 2_677 2_677 ? C40 C38 C38 107.1(14) 2_677 2_677 ? C39 C38 C38 51.7(6) . 2_677 ? C43 C38 C38 68.4(6) . 2_677 ? C44 C38 C38 179.5(18) . 2_677 ? C42 C38 C38 87.1(10) 2_677 2_677 ? C39 C38 C38 44.7(5) 2_677 2_677 ? C43 C38 C38 41.7(4) 2_677 2_677 ? C43 C39 C42 133(3) 2_677 2_677 ? C43 C39 C40 27.9(18) 2_677 . ? C42 C39 C40 160.8(14) 2_677 . ? C43 C39 C38 147.0(18) 2_677 . ? C42 C39 C38 78.9(15) 2_677 . ? C40 C39 C38 120.0 . . ? C43 C39 C38 63.7(15) 2_677 2_677 ? C42 C39 C38 162(2) 2_677 2_677 ? C40 C39 C38 36.4(8) . 2_677 ? C38 C39 C38 83.6(8) . 2_677 ? C43 C39 C41 172(3) 2_677 2_677 ? C42 C39 C41 49.8(11) 2_677 2_677 ? C40 C39 C41 149.0(6) . 2_677 ? C38 C39 C41 29.2(6) . 2_677 ? C38 C39 C41 112.6(13) 2_677 2_677 ? C43 C40 C38 100(2) 2_677 2_677 ? C43 C40 C39 19.2(14) 2_677 . ? C38 C40 C39 81.2(12) 2_677 . ? C43 C40 C41 138.7(14) 2_677 . ? C38 C40 C41 39.0(12) 2_677 . ? C39 C40 C41 120.0 . . ? C43 C40 C44 169(3) 2_677 2_677 ? C38 C40 C44 71.1(15) 2_677 2_677 ? C39 C40 C44 152.3(13) . 2_677 ? C41 C40 C44 32.7(13) . 2_677 ? C44 C41 C38 122(3) 2_677 2_677 ? C44 C41 C42 158(2) 2_677 . ? C38 C41 C42 79.0(14) 2_677 . ? C44 C41 C40 81(2) 2_677 . ? C38 C41 C40 41.3(14) 2_677 . ? C42 C41 C40 120.1 . . ? C44 C41 C39 169(3) 2_677 2_677 ? C38 C41 C39 49.8(11) 2_677 2_677 ? C42 C41 C39 29.2(6) . 2_677 ? C40 C41 C39 90.9(6) . 2_677 ? C39 C42 C43 19.2(14) 2_677 . ? C39 C42 C41 101.0(14) 2_677 . ? C43 C42 C41 119.9 . . ? C39 C42 C38 65.5(12) 2_677 2_677 ? C43 C42 C38 84.5(8) . 2_677 ? C41 C42 C38 35.5(8) . 2_677 ? C39 C43 C40 133(3) 2_677 2_677 ? C39 C43 C42 27.9(18) 2_677 . ? C40 C43 C42 160.8(15) 2_677 . ? C39 C43 C38 92.5(18) 2_677 . ? C40 C43 C38 41.3(15) 2_677 . ? C42 C43 C38 120.01(6) . . ? C39 C43 C38 22.9(13) 2_677 2_677 ? C40 C43 C38 110.8(17) 2_677 2_677 ? C42 C43 C38 50.1(6) . 2_677 ? C38 C43 C38 69.9(5) . 2_677 ? C41 C44 C38 30.5(15) 2_677 . ? C41 C44 C40 66.1(17) 2_677 2_677 ? C38 C44 C40 36.2(10) . 2_677 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7 Yb1 N1 C1 1.3(5) . . . . ? N4 Yb1 N1 C1 116.1(5) . . . . ? N2 Yb1 N1 C1 -142.8(4) 2_576 . . . ? N5 Yb1 N1 C1 107.3(4) . . . . ? N1 Yb1 N1 C1 -88.5(4) 2_576 . . . ? C2 Yb1 N1 C1 108.6(4) . . . . ? C1 Yb1 N1 C1 -115.4(4) 2_576 . . . ? Yb1 Yb1 N1 C1 -88.5(4) 2_576 . . . ? N7 Yb1 N1 C3 -151.0(4) . . . . ? N4 Yb1 N1 C3 -36.1(4) . . . . ? N2 Yb1 N1 C3 65.0(4) 2_576 . . . ? N5 Yb1 N1 C3 -44.9(5) . . . . ? N1 Yb1 N1 C3 119.3(5) 2_576 . . . ? C2 Yb1 N1 C3 -43.6(4) . . . . ? C1 Yb1 N1 C3 92.4(4) 2_576 . . . ? Yb1 Yb1 N1 C3 119.3(5) 2_576 . . . ? N7 Yb1 N1 Yb1 89.8(2) . . . 2_576 ? N4 Yb1 N1 Yb1 -155.4(2) . . . 2_576 ? N2 Yb1 N1 Yb1 -54.29(19) 2_576 . . 2_576 ? N5 Yb1 N1 Yb1 -164.23(16) . . . 2_576 ? N1 Yb1 N1 Yb1 0.0 2_576 . . 2_576 ? C2 Yb1 N1 Yb1 -162.93(17) . . . 2_576 ? C1 Yb1 N1 Yb1 -26.92(19) 2_576 . . 2_576 ? N7 Yb1 N4 C2 -68.4(4) . . . . ? N2 Yb1 N4 C2 98.2(4) 2_576 . . . ? N5 Yb1 N4 C2 7.2(3) . . . . ? N1 Yb1 N4 C2 -165.3(4) . . . . ? N1 Yb1 N4 C2 140.7(4) 2_576 . . . ? C1 Yb1 N4 C2 105.8(4) 2_576 . . . ? Yb1 Yb1 N4 C2 175.7(3) 2_576 . . . ? N7 Yb1 N4 C11 153.5(5) . . . . ? N2 Yb1 N4 C11 -39.9(5) 2_576 . . . ? N5 Yb1 N4 C11 -130.9(6) . . . . ? N1 Yb1 N4 C11 56.7(5) . . . . ? N1 Yb1 N4 C11 2.7(7) 2_576 . . . ? C2 Yb1 N4 C11 -138.1(7) . . . . ? C1 Yb1 N4 C11 -32.3(6) 2_576 . . . ? Yb1 Yb1 N4 C11 37.6(5) 2_576 . . . ? N7 Yb1 N5 C2 112.7(4) . . . . ? N4 Yb1 N5 C2 -7.4(3) . . . . ? N2 Yb1 N5 C2 -108.1(4) 2_576 . . . ? N1 Yb1 N5 C2 2.6(5) . . . . ? N1 Yb1 N5 C2 -153.2(3) 2_576 . . . ? C1 Yb1 N5 C2 -129.4(4) 2_576 . . . ? Yb1 Yb1 N5 C2 -72.3(8) 2_576 . . . ? N7 Yb1 N5 C19 -37.1(7) . . . . ? N4 Yb1 N5 C19 -157.2(8) . . . . ? N2 Yb1 N5 C19 102.1(7) 2_576 . . . ? N1 Yb1 N5 C19 -147.2(7) . . . . ? N1 Yb1 N5 C19 57.0(8) 2_576 . . . ? C2 Yb1 N5 C19 -149.7(9) . . . . ? C1 Yb1 N5 C19 80.8(7) 2_576 . . . ? Yb1 Yb1 N5 C19 138.0(7) 2_576 . . . ? N4 Yb1 N7 C25 31.3(8) . . . . ? N2 Yb1 N7 C25 -128.9(6) 2_576 . . . ? N5 Yb1 N7 C25 -24.5(7) . . . . ? N1 Yb1 N7 C25 111.1(7) . . . . ? N1 Yb1 N7 C25 -163.2(7) 2_576 . . . ? C2 Yb1 N7 C25 2.8(7) . . . . ? C1 Yb1 N7 C25 -143.8(7) 2_576 . . . ? Yb1 Yb1 N7 C25 156.5(7) 2_576 . . . ? C13 N2 C1 N3 13.6(11) . . . . ? Yb1 N2 C1 N3 -158.8(6) 2_576 . . . ? C13 N2 C1 N1 -167.9(6) . . . . ? Yb1 N2 C1 N1 19.6(6) 2_576 . . . ? C13 N2 C1 Yb1 172.4(7) . . . 2_576 ? C16 N3 C1 N2 -157.3(7) . . . . ? C16 N3 C1 N1 24.3(10) . . . . ? C16 N3 C1 Yb1 119.0(16) . . . 2_576 ? C3 N1 C1 N2 -129.4(6) . . . . ? Yb1 N1 C1 N2 75.4(6) . . . . ? Yb1 N1 C1 N2 -17.8(5) 2_576 . . . ? C3 N1 C1 N3 49.1(8) . . . . ? Yb1 N1 C1 N3 -106.1(6) . . . . ? Yb1 N1 C1 N3 160.7(6) 2_576 . . . ? C3 N1 C1 Yb1 -111.6(5) . . . 2_576 ? Yb1 N1 C1 Yb1 93.2(3) . . . 2_576 ? C19 N5 C2 N4 171.1(5) . . . . ? Yb1 N5 C2 N4 11.4(5) . . . . ? C19 N5 C2 N6 -5.2(9) . . . . ? Yb1 N5 C2 N6 -165.0(6) . . . . ? C19 N5 C2 Yb1 159.7(6) . . . . ? C11 N4 C2 N5 126.7(6) . . . . ? Yb1 N4 C2 N5 -12.0(6) . . . . ? C11 N4 C2 N6 -56.9(9) . . . . ? Yb1 N4 C2 N6 164.4(6) . . . . ? C11 N4 C2 Yb1 138.7(7) . . . . ? C22 N6 C2 N5 157.7(7) . . . . ? C22 N6 C2 N4 -18.3(11) . . . . ? C22 N6 C2 Yb1 57(2) . . . . ? N7 Yb1 C2 N5 -71.2(4) . . . . ? N4 Yb1 C2 N5 167.2(6) . . . . ? N2 Yb1 C2 N5 77.7(4) 2_576 . . . ? N1 Yb1 C2 N5 -178.1(3) . . . . ? N1 Yb1 C2 N5 62.6(7) 2_576 . . . ? C1 Yb1 C2 N5 67.1(4) 2_576 . . . ? Yb1 Yb1 C2 N5 160.3(3) 2_576 . . . ? N7 Yb1 C2 N4 121.6(4) . . . . ? N2 Yb1 C2 N4 -89.6(4) 2_576 . . . ? N5 Yb1 C2 N4 -167.2(6) . . . . ? N1 Yb1 C2 N4 14.7(4) . . . . ? N1 Yb1 C2 N4 -104.6(6) 2_576 . . . ? C1 Yb1 C2 N4 -100.1(4) 2_576 . . . ? Yb1 Yb1 C2 N4 -6.9(5) 2_576 . . . ? N7 Yb1 C2 N6 37(2) . . . . ? N4 Yb1 C2 N6 -84(2) . . . . ? N2 Yb1 C2 N6 -174(2) 2_576 . . . ? N5 Yb1 C2 N6 109(2) . . . . ? N1 Yb1 C2 N6 -70(2) . . . . ? N1 Yb1 C2 N6 171.2(19) 2_576 . . . ? C1 Yb1 C2 N6 176(2) 2_576 . . . ? Yb1 Yb1 C2 N6 -91(2) 2_576 . . . ? C1 N1 C3 C4 46.6(7) . . . . ? Yb1 N1 C3 C4 -160.8(4) . . . . ? Yb1 N1 C3 C4 -49.5(6) 2_576 . . . ? C1 N1 C3 C12 -140.0(6) . . . . ? Yb1 N1 C3 C12 12.5(7) . . . . ? Yb1 N1 C3 C12 123.8(5) 2_576 . . . ? C12 C3 C4 C5 -3.9(10) . . . . ? N1 C3 C4 C5 169.7(6) . . . . ? C3 C4 C5 C6 -2.3(11) . . . . ? C4 C5 C6 C7 4.0(12) . . . . ? C5 C6 C7 C8 178.2(7) . . . . ? C5 C6 C7 C12 0.4(11) . . . . ? C6 C7 C8 C9 -177.1(7) . . . . ? C12 C7 C8 C9 0.6(10) . . . . ? C7 C8 C9 C10 3.1(12) . . . . ? C8 C9 C10 C11 -2.1(12) . . . . ? C9 C10 C11 N4 -179.5(6) . . . . ? C9 C10 C11 C12 -2.6(10) . . . . ? C2 N4 C11 C10 -1.1(10) . . . . ? Yb1 N4 C11 C10 125.6(6) . . . . ? C2 N4 C11 C12 -178.1(6) . . . . ? Yb1 N4 C11 C12 -51.4(7) . . . . ? C4 C3 C12 C7 8.1(8) . . . . ? N1 C3 C12 C7 -165.0(5) . . . . ? C4 C3 C12 C11 -171.0(6) . . . . ? N1 C3 C12 C11 15.8(9) . . . . ? C8 C7 C12 C3 175.7(6) . . . . ? C6 C7 C12 C3 -6.4(9) . . . . ? C8 C7 C12 C11 -5.1(9) . . . . ? C6 C7 C12 C11 172.8(6) . . . . ? C10 C11 C12 C3 -174.9(6) . . . . ? N4 C11 C12 C3 2.2(9) . . . . ? C10 C11 C12 C7 5.9(8) . . . . ? N4 C11 C12 C7 -177.0(5) . . . . ? C1 N2 C13 C14 -127.6(8) . . . . ? Yb1 N2 C13 C14 40.9(10) 2_576 . . . ? C1 N2 C13 C15 110.9(8) . . . . ? Yb1 N2 C13 C15 -80.6(9) 2_576 . . . ? C1 N3 C16 C17 121.4(8) . . . . ? C1 N3 C16 C18 -116.8(8) . . . . ? C2 N5 C19 C20 79.7(8) . . . . ? Yb1 N5 C19 C20 -135.8(6) . . . . ? C2 N5 C19 C21 -162.6(6) . . . . ? Yb1 N5 C19 C21 -18.1(10) . . . . ? C2 N6 C22 C24 -90.5(9) . . . . ? C2 N6 C22 C23 147.6(7) . . . . ? Yb1 N7 C25 C30 -28.7(10) . . . . ? Yb1 N7 C25 C26 149.7(6) . . . . ? N7 C25 C26 C27 -177.5(7) . . . . ? C30 C25 C26 C27 0.9(11) . . . . ? C25 C26 C27 C28 -2.2(12) . . . . ? C26 C27 C28 C29 2.2(12) . . . . ? C26 C27 C28 Cl1 -178.2(6) . . . . ? C27 C28 C29 C30 -0.9(12) . . . . ? Cl1 C28 C29 C30 179.4(6) . . . . ? N7 C25 C30 C29 178.9(6) . . . . ? C26 C25 C30 C29 0.4(10) . . . . ? C28 C29 C30 C25 -0.4(11) . . . . ? C36 C31 C32 C33 -2(2) . . . . ? C37 C31 C32 C33 -179.4(14) . . . . ? C31 C32 C33 C34 2(2) . . . . ? C32 C33 C34 C35 -1(2) . . . . ? C33 C34 C35 C36 0(3) . . . . ? C34 C35 C36 C31 0(3) . . . . ? C32 C31 C36 C35 1(2) . . . . ? C37 C31 C36 C35 178.0(14) . . . . ? C41 C38 C39 C43 -166(6) 2_677 . . 2_677 ? C40 C38 C39 C43 0.04(19) 2_677 . . 2_677 ? C43 C38 C39 C43 10(4) . . . 2_677 ? C44 C38 C39 C43 -172(5) . . . 2_677 ? C42 C38 C39 C43 -166(6) 2_677 . . 2_677 ? C39 C38 C39 C43 8(3) 2_677 . . 2_677 ? C38 C38 C39 C43 8(3) 2_677 . . 2_677 ? C41 C38 C39 C42 0.0 2_677 . . 2_677 ? C40 C38 C39 C42 166(5) 2_677 . . 2_677 ? C43 C38 C39 C42 176.1(15) . . . 2_677 ? C44 C38 C39 C42 -6(2) . . . 2_677 ? C39 C38 C39 C42 174(2) 2_677 . . 2_677 ? C43 C38 C39 C42 166(6) 2_677 . . 2_677 ? C38 C38 C39 C42 174(2) 2_677 . . 2_677 ? C41 C38 C39 C40 -176.1(15) 2_677 . . . ? C40 C38 C39 C40 -10(4) 2_677 . . . ? C43 C38 C39 C40 0.0 . . . . ? C44 C38 C39 C40 178.3(19) . . . . ? C42 C38 C39 C40 -176.1(15) 2_677 . . . ? C39 C38 C39 C40 -2.2(9) 2_677 . . . ? C43 C38 C39 C40 -10(4) 2_677 . . . ? C38 C38 C39 C40 -2.2(9) 2_677 . . . ? C41 C38 C39 C38 -174(2) 2_677 . . 2_677 ? C40 C38 C39 C38 -8(3) 2_677 . . 2_677 ? C43 C38 C39 C38 2.2(9) . . . 2_677 ? C44 C38 C39 C38 -179(2) . . . 2_677 ? C42 C38 C39 C38 -174(2) 2_677 . . 2_677 ? C39 C38 C39 C38 0.0 2_677 . . 2_677 ? C43 C38 C39 C38 -8(3) 2_677 . . 2_677 ? C40 C38 C39 C41 166(5) 2_677 . . 2_677 ? C43 C38 C39 C41 176.2(15) . . . 2_677 ? C44 C38 C39 C41 -6(2) . . . 2_677 ? C42 C38 C39 C41 0.0 2_677 . . 2_677 ? C39 C38 C39 C41 174(2) 2_677 . . 2_677 ? C43 C38 C39 C41 166(6) 2_677 . . 2_677 ? C38 C38 C39 C41 174(2) 2_677 . . 2_677 ? C42 C39 C40 C43 0.00(6) 2_677 . . 2_677 ? C38 C39 C40 C43 168(5) . . . 2_677 ? C38 C39 C40 C43 165(6) 2_677 . . 2_677 ? C41 C39 C40 C43 165(6) 2_677 . . 2_677 ? C43 C39 C40 C38 -165(6) 2_677 . . 2_677 ? C42 C39 C40 C38 -165(6) 2_677 . . 2_677 ? C38 C39 C40 C38 3.6(15) . . . 2_677 ? C41 C39 C40 C38 -0.01(8) 2_677 . . 2_677 ? C43 C39 C40 C41 -168(5) 2_677 . . . ? C42 C39 C40 C41 -168(5) 2_677 . . . ? C38 C39 C40 C41 0.0 . . . . ? C38 C39 C40 C41 -3.6(15) 2_677 . . . ? C41 C39 C40 C41 -3.7(14) 2_677 . . . ? C43 C39 C40 C44 -161(7) 2_677 . . 2_677 ? C42 C39 C40 C44 -161(7) 2_677 . . 2_677 ? C38 C39 C40 C44 8(4) . . . 2_677 ? C38 C39 C40 C44 4(3) 2_677 . . 2_677 ? C41 C39 C40 C44 4(3) 2_677 . . 2_677 ? C43 C40 C41 C44 168(5) 2_677 . . 2_677 ? C38 C40 C41 C44 168(5) 2_677 . . 2_677 ? C39 C40 C41 C44 173(3) . . . 2_677 ? C43 C40 C41 C38 0.0 2_677 . . 2_677 ? C39 C40 C41 C38 6(2) . . . 2_677 ? C44 C40 C41 C38 -168(5) 2_677 . . 2_677 ? C43 C40 C41 C42 -6(2) 2_677 . . . ? C38 C40 C41 C42 -6(2) 2_677 . . . ? C39 C40 C41 C42 0.0 . . . . ? C44 C40 C41 C42 -173(3) 2_677 . . . ? C43 C40 C41 C39 -3.9(15) 2_677 . . 2_677 ? C38 C40 C41 C39 -3.9(15) 2_677 . . 2_677 ? C39 C40 C41 C39 1.9(7) . . . 2_677 ? C44 C40 C41 C39 -172(3) 2_677 . . 2_677 ? C44 C41 C42 C39 -159(9) 2_677 . . 2_677 ? C38 C41 C42 C39 0.0 2_677 . . 2_677 ? C40 C41 C42 C39 3.9(15) . . . 2_677 ? C44 C41 C42 C43 -163(8) 2_677 . . . ? C38 C41 C42 C43 -3.8(15) 2_677 . . . ? C40 C41 C42 C43 0.0 . . . . ? C39 C41 C42 C43 -3.9(15) 2_677 . . . ? C44 C41 C42 C38 -159(9) 2_677 . . 2_677 ? C40 C41 C42 C38 3.9(15) . . . 2_677 ? C39 C41 C42 C38 0.0 2_677 . . 2_677 ? C41 C42 C43 C39 12(5) . . . 2_677 ? C38 C42 C43 C39 9(4) 2_677 . . 2_677 ? C39 C42 C43 C40 0.0 2_677 . . 2_677 ? C41 C42 C43 C40 12(5) . . . 2_677 ? C38 C42 C43 C40 9(4) 2_677 . . 2_677 ? C39 C42 C43 C38 -12(5) 2_677 . . . ? C41 C42 C43 C38 0.0 . . . . ? C38 C42 C43 C38 -2.2(9) 2_677 . . . ? C39 C42 C43 C38 -9(4) 2_677 . . 2_677 ? C41 C42 C43 C38 2.2(9) . . . 2_677 ? C41 C38 C43 C39 169(4) 2_677 . . 2_677 ? C40 C38 C43 C39 169(4) 2_677 . . 2_677 ? C39 C38 C43 C39 -5(2) . . . 2_677 ? C44 C38 C43 C39 176(3) . . . 2_677 ? C42 C38 C43 C39 0.0 2_677 . . 2_677 ? C43 C38 C43 C39 -3.6(14) 2_677 . . 2_677 ? C38 C38 C43 C39 -3.6(14) 2_677 . . 2_677 ? C41 C38 C43 C40 0.0 2_677 . . 2_677 ? C39 C38 C43 C40 -174(2) . . . 2_677 ? C44 C38 C43 C40 7(3) . . . 2_677 ? C42 C38 C43 C40 -169(4) 2_677 . . 2_677 ? C39 C38 C43 C40 -169(4) 2_677 . . 2_677 ? C43 C38 C43 C40 -172(3) 2_677 . . 2_677 ? C38 C38 C43 C40 -172(3) 2_677 . . 2_677 ? C41 C38 C43 C42 174(2) 2_677 . . . ? C40 C38 C43 C42 174(2) 2_677 . . . ? C39 C38 C43 C42 0.0 . . . . ? C44 C38 C43 C42 -178.6(16) . . . . ? C42 C38 C43 C42 5(2) 2_677 . . . ? C39 C38 C43 C42 5(2) 2_677 . . . ? C43 C38 C43 C42 1.8(7) 2_677 . . . ? C38 C38 C43 C42 1.8(7) 2_677 . . . ? C41 C38 C43 C38 172(3) 2_677 . . 2_677 ? C40 C38 C43 C38 172(3) 2_677 . . 2_677 ? C39 C38 C43 C38 -1.8(7) . . . 2_677 ? C44 C38 C43 C38 179.6(19) . . . 2_677 ? C42 C38 C43 C38 3.5(14) 2_677 . . 2_677 ? C39 C38 C43 C38 3.6(14) 2_677 . . 2_677 ? C43 C38 C43 C38 0.0 2_677 . . 2_677 ? C40 C38 C44 C41 -165(5) 2_677 . . 2_677 ? C39 C38 C44 C41 12(5) . . . 2_677 ? C43 C38 C44 C41 -170(4) . . . 2_677 ? C42 C38 C44 C41 8(4) 2_677 . . 2_677 ? C39 C38 C44 C41 -168(5) 2_677 . . 2_677 ? C43 C38 C44 C41 9(5) 2_677 . . 2_677 ? C38 C38 C44 C41 -114(100) 2_677 . . 2_677 ? C41 C38 C44 C40 165(5) 2_677 . . 2_677 ? C39 C38 C44 C40 176.9(18) . . . 2_677 ? C43 C38 C44 C40 -4.7(17) . . . 2_677 ? C42 C38 C44 C40 174(2) 2_677 . . 2_677 ? C39 C38 C44 C40 -2(2) 2_677 . . 2_677 ? C43 C38 C44 C40 175(3) 2_677 . . 2_677 ? C38 C38 C44 C40 51(100) 2_677 . . 2_677 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.083 _refine_diff_density_min -1.530 _refine_diff_density_rms 0.138 data_complex7 _database_code_depnum_ccdc_archive 'CCDC 909535' #TrackingRef '909535.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H88 N14 Yb2, C4 H8 O' _chemical_formula_sum 'C66 H96 N14 O Yb2' _chemical_formula_weight 1447.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5151(6) _cell_length_b 12.9495(8) _cell_length_c 13.0112(7) _cell_angle_alpha 98.036(5) _cell_angle_beta 92.863(4) _cell_angle_gamma 116.207(6) _cell_volume 1709.95(17) _cell_formula_units_Z 1 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 8207 _cell_measurement_theta_min 3.1808 _cell_measurement_theta_max 29.4248 _exptl_crystal_description orange _exptl_crystal_colour prism _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 738 _exptl_absorpt_coefficient_mu 2.768 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.92597 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4692 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16040 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_unetI/netI 0.0665 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6363 _reflns_number_gt 5573 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Their O1-C32,O1-C35,C32-C33, C33-C34,C34-C35,C34-O1,C32-C34,N3-H3,N6-H6 and N7-H7 distances were constrained. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0606P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6363 _refine_ls_number_parameters 333 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.585957(18) 0.560605(18) 0.629417(18) 0.02592(10) Uani 1 1 d . . . O1 O 0.512(3) 0.033(3) 0.942(3) 0.260(16) Uiso 0.50 1 d PD . . N1 N 0.6252(4) 0.6128(4) 0.4640(4) 0.0279(10) Uani 1 1 d . . . N2 N 0.6214(4) 0.4508(4) 0.3648(4) 0.0328(11) Uani 1 1 d . . . N3 N 0.8197(4) 0.6279(5) 0.3985(5) 0.0442(13) Uani 1 1 d D . . H3 H 0.852(5) 0.598(4) 0.363(3) 0.019(15) Uiso 1 1 d D . . N4 N 0.7101(4) 0.7547(4) 0.6632(4) 0.0323(11) Uani 1 1 d . . . N5 N 0.6738(4) 0.6639(4) 0.8013(4) 0.0325(11) Uani 1 1 d . . . N6 N 0.8493(5) 0.8566(5) 0.8264(4) 0.0487(14) Uani 1 1 d D . . H6 H 0.849(6) 0.833(6) 0.879(3) 0.04(2) Uiso 1 1 d D . . N7 N 0.6857(5) 0.4520(5) 0.6357(4) 0.0413(13) Uani 1 1 d D . . H7 H 0.650(5) 0.396(3) 0.593(4) 0.031(18) Uiso 1 1 d D . . C1 C 0.6916(5) 0.5622(5) 0.4075(5) 0.0324(13) Uani 1 1 d . . . C2 C 0.7449(5) 0.7616(5) 0.7674(5) 0.0345(13) Uani 1 1 d . . . C3 C 0.6387(5) 0.7221(5) 0.4357(4) 0.0293(12) Uani 1 1 d . . . C4 C 0.6208(5) 0.7223(5) 0.3296(5) 0.0385(14) Uani 1 1 d . . . H4 H 0.6117 0.6572 0.2814 0.046 Uiso 1 1 calc R . . C5 C 0.6159(6) 0.8167(7) 0.2920(6) 0.0514(18) Uani 1 1 d . . . H5 H 0.6061 0.8155 0.2196 0.062 Uiso 1 1 calc R . . C6 C 0.6252(6) 0.9093(6) 0.3604(6) 0.0497(17) Uani 1 1 d . . . H6A H 0.6179 0.9708 0.3346 0.060 Uiso 1 1 calc R . . C7 C 0.6458(5) 0.9165(5) 0.4694(5) 0.0393(15) Uani 1 1 d . . . C8 C 0.6536(6) 1.0140(5) 0.5376(6) 0.0484(17) Uani 1 1 d . . . H8 H 0.6446 1.0738 0.5100 0.058 Uiso 1 1 calc R . . C9 C 0.6738(7) 1.0231(6) 0.6420(7) 0.0556(19) Uani 1 1 d . . . H9 H 0.6749 1.0872 0.6868 0.067 Uiso 1 1 calc R . . C10 C 0.6931(6) 0.9370(5) 0.6839(6) 0.0467(16) Uani 1 1 d . . . H10 H 0.7079 0.9452 0.7570 0.056 Uiso 1 1 calc R . . C11 C 0.6913(5) 0.8403(5) 0.6214(5) 0.0364(14) Uani 1 1 d . . . C12 C 0.6584(5) 0.8234(5) 0.5096(5) 0.0311(13) Uani 1 1 d . . . C13 C 0.6851(8) 0.3820(8) 0.3179(7) 0.0688(13) Uani 1 1 d . . . H13 H 0.7756 0.4347 0.3077 0.083 Uiso 1 1 calc R . . C14 C 0.6082(8) 0.3084(8) 0.2149(7) 0.0688(13) Uani 1 1 d . . . H14A H 0.5242 0.2494 0.2271 0.103 Uiso 1 1 calc R . . H14B H 0.6557 0.2706 0.1804 0.103 Uiso 1 1 calc R . . H14C H 0.5951 0.3579 0.1709 0.103 Uiso 1 1 calc R . . C15 C 0.6852(8) 0.2982(7) 0.3929(7) 0.0688(13) Uani 1 1 d . . . H15A H 0.7211 0.3426 0.4630 0.103 Uiso 1 1 calc R . . H15B H 0.7380 0.2607 0.3688 0.103 Uiso 1 1 calc R . . H15C H 0.5966 0.2390 0.3934 0.103 Uiso 1 1 calc R . . C16 C 0.9123(5) 0.7359(6) 0.4700(6) 0.0494(17) Uani 1 1 d . . . H16 H 0.8672 0.7539 0.5274 0.059 Uiso 1 1 calc R . . C17 C 0.9651(7) 0.8381(6) 0.4100(7) 0.068(2) Uani 1 1 d . . . H17A H 1.0035 0.8181 0.3506 0.102 Uiso 1 1 calc R . . H17B H 1.0309 0.9074 0.4560 0.102 Uiso 1 1 calc R . . H17C H 0.8942 0.8534 0.3856 0.102 Uiso 1 1 calc R . . C18 C 1.0211(6) 0.7126(8) 0.5150(7) 0.071(2) Uani 1 1 d . . . H18A H 0.9865 0.6546 0.5597 0.107 Uiso 1 1 calc R . . H18B H 1.0894 0.7846 0.5556 0.107 Uiso 1 1 calc R . . H18C H 1.0567 0.6836 0.4584 0.107 Uiso 1 1 calc R . . C19 C 0.7057(5) 0.6462(5) 0.9049(5) 0.0368(14) Uani 1 1 d . . . H19 H 0.8008 0.6725 0.9178 0.044 Uiso 1 1 calc R . . C20 C 0.6666(6) 0.7149(6) 0.9906(5) 0.0496(17) Uani 1 1 d . . . H20A H 0.7124 0.7978 0.9884 0.074 Uiso 1 1 calc R . . H20B H 0.6894 0.7015 1.0585 0.074 Uiso 1 1 calc R . . H20C H 0.5732 0.6888 0.9789 0.074 Uiso 1 1 calc R . . C21 C 0.6334(6) 0.5153(6) 0.9070(5) 0.0447(15) Uani 1 1 d . . . H21A H 0.5405 0.4878 0.8886 0.067 Uiso 1 1 calc R . . H21B H 0.6493 0.5018 0.9766 0.067 Uiso 1 1 calc R . . H21C H 0.6643 0.4733 0.8570 0.067 Uiso 1 1 calc R . . C22 C 0.9598(7) 0.9434(7) 0.7856(8) 0.0744(15) Uani 1 1 d . . . H22 H 0.9312 0.9458 0.7133 0.089 Uiso 1 1 calc R . . C23 C 1.0037(8) 1.0637(7) 0.8528(7) 0.0744(15) Uani 1 1 d . . . H23A H 0.9327 1.0846 0.8503 0.112 Uiso 1 1 calc R . . H23B H 1.0778 1.1212 0.8264 0.112 Uiso 1 1 calc R . . H23C H 1.0287 1.0616 0.9246 0.112 Uiso 1 1 calc R . . C24 C 1.0705(7) 0.9109(7) 0.7829(7) 0.0744(15) Uani 1 1 d . . . H24A H 1.0968 0.9046 0.8528 0.112 Uiso 1 1 calc R . . H24B H 1.1438 0.9708 0.7578 0.112 Uiso 1 1 calc R . . H24C H 1.0420 0.8365 0.7364 0.112 Uiso 1 1 calc R . . C25 C 0.7885(7) 0.4494(7) 0.6938(6) 0.0587(7) Uani 1 1 d . . . C26 C 0.8936(6) 0.5525(7) 0.7434(6) 0.0587(7) Uani 1 1 d . . . H26 H 0.8974 0.6246 0.7340 0.070 Uiso 1 1 calc R . . C27 C 0.9943(7) 0.5513(7) 0.8075(6) 0.0587(7) Uani 1 1 d . . . H27 H 1.0634 0.6225 0.8418 0.070 Uiso 1 1 calc R . . C28 C 0.9937(7) 0.4466(7) 0.8213(6) 0.0587(7) Uani 1 1 d . . . C29 C 0.8899(7) 0.3444(7) 0.7706(6) 0.0587(7) Uani 1 1 d . . . H29 H 0.8860 0.2722 0.7793 0.070 Uiso 1 1 calc R . . C30 C 0.7921(7) 0.3463(7) 0.7075(6) 0.0587(7) Uani 1 1 d . . . H30 H 0.7246 0.2748 0.6720 0.070 Uiso 1 1 calc R . . C31 C 1.0991(7) 0.4448(7) 0.8950(6) 0.0587(7) Uani 1 1 d . . . H31A H 1.1460 0.5204 0.9406 0.088 Uiso 1 1 calc R . . H31B H 1.1592 0.4281 0.8545 0.088 Uiso 1 1 calc R . . H31C H 1.0592 0.3847 0.9368 0.088 Uiso 1 1 calc R . . C32 C 0.603(3) 0.149(3) 0.929(3) 0.186(14) Uiso 0.50 1 d PD . . C33 C 0.742(3) 0.193(3) 0.968(4) 0.209(17) Uiso 0.50 1 d PD . . C34 C 0.677(3) 0.077(3) 0.994(3) 0.155(11) Uiso 0.50 1 d PD . . C35 C 0.558(4) -0.017(4) 1.018(4) 0.22(2) 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 0.01867(14) 0.02474(15) 0.03212(16) 0.00880(10) 0.00007(9) 0.00713(10) N1 0.022(2) 0.025(2) 0.034(3) 0.010(2) 0.0035(18) 0.0078(18) N2 0.026(2) 0.035(3) 0.035(3) 0.001(2) 0.002(2) 0.014(2) N3 0.024(2) 0.045(3) 0.058(4) 0.006(3) 0.013(2) 0.010(2) N4 0.034(2) 0.021(2) 0.034(3) 0.007(2) -0.003(2) 0.0061(19) N5 0.019(2) 0.038(3) 0.035(3) 0.006(2) -0.0025(19) 0.0084(19) N6 0.045(3) 0.040(3) 0.031(3) 0.011(3) -0.007(2) -0.007(2) N7 0.045(3) 0.041(3) 0.043(3) 0.002(3) -0.010(2) 0.027(3) C1 0.020(2) 0.043(4) 0.034(3) 0.010(3) 0.001(2) 0.014(2) C2 0.033(3) 0.033(3) 0.033(3) 0.005(3) 0.003(2) 0.011(2) C3 0.020(2) 0.028(3) 0.033(3) 0.007(2) 0.000(2) 0.005(2) C4 0.035(3) 0.043(4) 0.036(4) 0.013(3) 0.000(3) 0.015(3) C5 0.042(4) 0.069(5) 0.045(4) 0.029(4) 0.001(3) 0.023(3) C6 0.043(4) 0.054(4) 0.057(5) 0.031(4) 0.006(3) 0.020(3) C7 0.025(3) 0.039(4) 0.054(4) 0.021(3) 0.003(3) 0.012(2) C8 0.045(3) 0.027(3) 0.075(5) 0.017(3) 0.000(3) 0.016(3) C9 0.053(4) 0.031(4) 0.075(6) -0.001(4) -0.004(4) 0.016(3) C10 0.046(4) 0.033(4) 0.050(4) 0.007(3) -0.001(3) 0.009(3) C11 0.021(3) 0.020(3) 0.055(4) 0.011(3) 0.001(2) -0.004(2) C12 0.022(2) 0.023(3) 0.046(4) 0.014(3) 0.003(2) 0.006(2) C13 0.079(3) 0.076(3) 0.071(3) 0.000(3) 0.013(2) 0.056(3) C14 0.079(3) 0.076(3) 0.071(3) 0.000(3) 0.013(2) 0.056(3) C15 0.079(3) 0.076(3) 0.071(3) 0.000(3) 0.013(2) 0.056(3) C16 0.020(3) 0.051(4) 0.064(5) 0.011(3) 0.002(3) 0.004(3) C17 0.040(4) 0.048(4) 0.099(7) 0.020(4) 0.009(4) 0.003(3) C18 0.032(3) 0.087(6) 0.083(6) 0.024(5) -0.001(4) 0.015(4) C19 0.031(3) 0.046(4) 0.030(3) 0.007(3) -0.008(2) 0.016(3) C20 0.049(4) 0.050(4) 0.037(4) 0.005(3) 0.003(3) 0.012(3) C21 0.042(3) 0.046(4) 0.041(4) 0.019(3) 0.007(3) 0.012(3) C22 0.057(3) 0.051(3) 0.082(4) 0.018(3) -0.003(2) -0.006(2) C23 0.057(3) 0.051(3) 0.082(4) 0.018(3) -0.003(2) -0.006(2) C24 0.057(3) 0.051(3) 0.082(4) 0.018(3) -0.003(2) -0.006(2) C25 0.0507(15) 0.0656(19) 0.068(2) 0.0148(15) -0.0030(13) 0.0340(14) C26 0.0507(15) 0.0656(19) 0.068(2) 0.0148(15) -0.0030(13) 0.0340(14) C27 0.0507(15) 0.0656(19) 0.068(2) 0.0148(15) -0.0030(13) 0.0340(14) C28 0.0507(15) 0.0656(19) 0.068(2) 0.0148(15) -0.0030(13) 0.0340(14) C29 0.0507(15) 0.0656(19) 0.068(2) 0.0148(15) -0.0030(13) 0.0340(14) C30 0.0507(15) 0.0656(19) 0.068(2) 0.0148(15) -0.0030(13) 0.0340(14) C31 0.0507(15) 0.0656(19) 0.068(2) 0.0148(15) -0.0030(13) 0.0340(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N7 2.180(5) . ? Yb1 N4 2.238(4) . ? Yb1 N2 2.332(4) 2_666 ? Yb1 N1 2.351(5) . ? Yb1 N5 2.357(5) . ? Yb1 N1 2.560(4) 2_666 ? Yb1 C2 2.740(6) . ? Yb1 C1 2.850(5) 2_666 ? Yb1 C1 3.188(6) . ? Yb1 Yb1 3.5827(5) 2_666 ? Yb1 H7 2.55(5) . ? O1 C35 0.94(5) 2_657 ? O1 C32 1.436(19) . ? O1 C35 1.457(18) . ? O1 O1 1.81(9) 2_657 ? N1 C1 1.386(7) . ? N1 C3 1.456(7) . ? N1 Yb1 2.560(4) 2_666 ? N2 C1 1.321(7) . ? N2 C13 1.474(8) . ? N2 Yb1 2.332(4) 2_666 ? N3 C1 1.360(7) . ? N3 C16 1.476(8) . ? N3 H3 0.779(10) . ? N4 C2 1.374(7) . ? N4 C11 1.393(7) . ? N5 C2 1.320(7) . ? N5 C19 1.454(7) . ? N6 C2 1.373(8) . ? N6 C22 1.462(9) . ? N6 H6 0.782(10) . ? N7 C25 1.388(8) . ? N7 H7 0.779(10) . ? C1 Yb1 2.850(5) 2_666 ? C3 C4 1.387(8) . ? C3 C12 1.434(8) . ? C4 C5 1.400(9) . ? C4 H4 0.9400 . ? C5 C6 1.350(10) . ? C5 H5 0.9400 . ? C6 C7 1.410(9) . ? C6 H6A 0.9400 . ? C7 C8 1.403(9) . ? C7 C12 1.439(8) . ? C8 C9 1.347(10) . ? C8 H8 0.9400 . ? C9 C10 1.403(9) . ? C9 H9 0.9400 . ? C10 C11 1.386(9) . ? C10 H10 0.9400 . ? C11 C12 1.445(9) . ? C13 C14 1.506(11) . ? C13 C15 1.558(12) . ? C13 H13 0.9900 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C18 1.521(9) . ? C16 C17 1.535(10) . ? C16 H16 0.9900 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C21 1.528(9) . ? C19 C20 1.538(9) . ? C19 H19 0.9900 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 C24 1.508(12) . ? C22 C23 1.525(12) . ? C22 H22 0.9900 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C26 1.385(10) . ? C25 C30 1.390(10) . ? C26 C27 1.401(9) . ? C26 H26 0.9400 . ? C27 C28 1.389(10) . ? C27 H27 0.9400 . ? C28 C29 1.377(10) . ? C28 C31 1.519(9) . ? C29 C30 1.371(9) . ? C29 H29 0.9400 . ? C30 H30 0.9400 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 C33 1.473(19) . ? C33 C34 1.457(19) . ? C34 C35 1.46(2) . ? C35 O1 0.94(5) 2_657 ? C35 C35 1.65(10) 2_657 ? 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 N7 Yb1 N4 117.04(18) . . ? N7 Yb1 N2 140.3(2) . 2_666 ? N4 Yb1 N2 100.79(16) . 2_666 ? N7 Yb1 N1 101.03(19) . . ? N4 Yb1 N1 75.36(16) . . ? N2 Yb1 N1 99.55(16) 2_666 . ? N7 Yb1 N5 93.29(18) . . ? N4 Yb1 N5 58.28(17) . . ? N2 Yb1 N5 97.01(15) 2_666 . ? N1 Yb1 N5 132.88(16) . . ? N7 Yb1 N1 92.45(17) . 2_666 ? N4 Yb1 N1 147.51(15) . 2_666 ? N2 Yb1 N1 55.50(15) 2_666 2_666 ? N1 Yb1 N1 86.39(14) . 2_666 ? N5 Yb1 N1 137.95(15) . 2_666 ? N7 Yb1 C2 103.39(18) . . ? N4 Yb1 C2 29.93(17) . . ? N2 Yb1 C2 103.92(16) 2_666 . ? N1 Yb1 C2 104.13(17) . . ? N5 Yb1 C2 28.79(17) . . ? N1 Yb1 C2 158.69(16) 2_666 . ? N7 Yb1 C1 115.65(19) . 2_666 ? N4 Yb1 C1 127.16(16) . 2_666 ? N2 Yb1 C1 27.26(16) 2_666 2_666 ? N1 Yb1 C1 98.41(16) . 2_666 ? N5 Yb1 C1 115.26(16) . 2_666 ? N1 Yb1 C1 29.07(15) 2_666 2_666 ? C2 Yb1 C1 129.70(17) . 2_666 ? N7 Yb1 C1 77.79(18) . . ? N4 Yb1 C1 87.19(17) . . ? N2 Yb1 C1 117.52(15) 2_666 . ? N1 Yb1 C1 23.28(14) . . ? N5 Yb1 C1 135.77(14) . . ? N1 Yb1 C1 86.09(14) 2_666 . ? C2 Yb1 C1 110.92(16) . . ? C1 Yb1 C1 107.45(12) 2_666 . ? N7 Yb1 Yb1 98.98(14) . 2_666 ? N4 Yb1 Yb1 115.90(12) . 2_666 ? N2 Yb1 Yb1 72.79(12) 2_666 2_666 ? N1 Yb1 Yb1 45.48(10) . 2_666 ? N5 Yb1 Yb1 167.69(11) . 2_666 ? N1 Yb1 Yb1 40.90(10) 2_666 2_666 ? C2 Yb1 Yb1 145.67(13) . 2_666 ? C1 Yb1 Yb1 58.09(12) 2_666 2_666 ? C1 Yb1 Yb1 49.36(9) . 2_666 ? N7 Yb1 H7 16.8(8) . . ? N4 Yb1 H7 130.3(11) . . ? N2 Yb1 H7 129.0(11) 2_666 . ? N1 Yb1 H7 93.9(13) . . ? N5 Yb1 H7 108.9(9) . . ? N1 Yb1 H7 76.8(9) 2_666 . ? C2 Yb1 H7 120.1(8) . . ? C1 Yb1 H7 102.2(10) 2_666 . ? C1 Yb1 H7 71.1(14) . . ? Yb1 Yb1 H7 83.2(9) 2_666 . ? C35 O1 C32 124(5) 2_657 . ? C35 O1 C35 84(6) 2_657 . ? C32 O1 C35 116(2) . . ? C35 O1 O1 53(5) 2_657 2_657 ? C32 O1 O1 130(4) . 2_657 ? C35 O1 O1 31(2) . 2_657 ? C1 N1 C3 114.6(5) . . ? C1 N1 Yb1 114.6(3) . . ? C3 N1 Yb1 125.3(4) . . ? C1 N1 Yb1 87.1(3) . 2_666 ? C3 N1 Yb1 111.1(3) . 2_666 ? Yb1 N1 Yb1 93.61(14) . 2_666 ? C1 N2 C13 120.3(5) . . ? C1 N2 Yb1 98.7(3) . 2_666 ? C13 N2 Yb1 140.1(4) . 2_666 ? C1 N3 C16 126.5(5) . . ? C1 N3 H3 116(4) . . ? C16 N3 H3 115(4) . . ? C2 N4 C11 124.8(5) . . ? C2 N4 Yb1 95.7(3) . . ? C11 N4 Yb1 128.6(3) . . ? C2 N5 C19 121.6(5) . . ? C2 N5 Yb1 91.9(4) . . ? C19 N5 Yb1 141.3(4) . . ? C2 N6 C22 125.7(6) . . ? C2 N6 H6 100(5) . . ? C22 N6 H6 128(5) . . ? C25 N7 Yb1 140.1(5) . . ? C25 N7 H7 111(4) . . ? Yb1 N7 H7 109(4) . . ? N2 C1 N3 125.1(5) . . ? N2 C1 N1 115.3(4) . . ? N3 C1 N1 119.6(5) . . ? N2 C1 Yb1 54.0(3) . 2_666 ? N3 C1 Yb1 164.1(4) . 2_666 ? N1 C1 Yb1 63.8(3) . 2_666 ? N2 C1 Yb1 99.7(4) . . ? N3 C1 Yb1 121.1(4) . . ? N1 C1 Yb1 42.1(3) . . ? Yb1 C1 Yb1 72.55(12) 2_666 . ? N5 C2 N6 124.3(5) . . ? N5 C2 N4 112.5(5) . . ? N6 C2 N4 123.0(5) . . ? N5 C2 Yb1 59.3(3) . . ? N6 C2 Yb1 165.3(5) . . ? N4 C2 Yb1 54.4(3) . . ? C4 C3 C12 119.3(5) . . ? C4 C3 N1 116.1(5) . . ? C12 C3 N1 124.4(5) . . ? C3 C4 C5 122.0(6) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 119.5(6) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 121.8(6) . . ? C5 C6 H6A 119.1 . . ? C7 C6 H6A 119.1 . . ? C8 C7 C6 119.8(6) . . ? C8 C7 C12 120.7(6) . . ? C6 C7 C12 119.5(6) . . ? C9 C8 C7 120.8(6) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 120.0(7) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 122.3(7) . . ? C11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C10 C11 N4 122.2(6) . . ? C10 C11 C12 118.6(5) . . ? N4 C11 C12 119.1(5) . . ? C3 C12 C7 117.6(5) . . ? C3 C12 C11 125.3(5) . . ? C7 C12 C11 117.1(5) . . ? N2 C13 C14 109.7(6) . . ? N2 C13 C15 108.3(6) . . ? C14 C13 C15 108.1(7) . . ? N2 C13 H13 110.2 . . ? C14 C13 H13 110.2 . . ? C15 C13 H13 110.2 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C18 107.1(6) . . ? N3 C16 C17 109.8(6) . . ? C18 C16 C17 111.5(5) . . ? N3 C16 H16 109.4 . . ? C18 C16 H16 109.4 . . ? C17 C16 H16 109.4 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N5 C19 C21 107.9(5) . . ? N5 C19 C20 111.5(5) . . ? C21 C19 C20 110.0(5) . . ? N5 C19 H19 109.1 . . ? C21 C19 H19 109.1 . . ? C20 C19 H19 109.1 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N6 C22 C24 110.8(7) . . ? N6 C22 C23 109.3(7) . . ? C24 C22 C23 110.9(6) . . ? N6 C22 H22 108.6 . . ? C24 C22 H22 108.6 . . ? C23 C22 H22 108.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 N7 120.4(7) . . ? C26 C25 C30 116.4(6) . . ? N7 C25 C30 123.2(7) . . ? C25 C26 C27 121.1(7) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C28 C27 C26 121.1(7) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C29 C28 C27 117.5(7) . . ? C29 C28 C31 121.2(7) . . ? C27 C28 C31 121.2(7) . . ? C30 C29 C28 121.1(7) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C25 122.8(7) . . ? C29 C30 H30 118.6 . . ? C25 C30 H30 118.6 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O1 C32 C33 119(2) . . ? C34 C33 C32 74.8(17) . . ? C33 C34 C35 148(3) . . ? O1 C35 O1 96(6) 2_657 . ? O1 C35 C34 144(6) 2_657 . ? O1 C35 C34 75.9(19) . . ? O1 C35 C35 61(5) 2_657 2_657 ? O1 C35 C35 35(2) . 2_657 ? C34 C35 C35 104(3) . 2_657 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7 Yb1 N1 C1 3.3(4) . . . . ? N4 Yb1 N1 C1 118.6(4) . . . . ? N2 Yb1 N1 C1 -142.6(3) 2_666 . . . ? N5 Yb1 N1 C1 108.4(4) . . . . ? N1 Yb1 N1 C1 -88.5(4) 2_666 . . . ? C2 Yb1 N1 C1 110.3(4) . . . . ? C1 Yb1 N1 C1 -115.1(3) 2_666 . . . ? Yb1 Yb1 N1 C1 -88.5(4) 2_666 . . . ? N7 Yb1 N1 C3 -149.0(4) . . . . ? N4 Yb1 N1 C3 -33.7(4) . . . . ? N2 Yb1 N1 C3 65.0(4) 2_666 . . . ? N5 Yb1 N1 C3 -43.9(4) . . . . ? N1 Yb1 N1 C3 119.2(4) 2_666 . . . ? C2 Yb1 N1 C3 -42.0(4) . . . . ? C1 Yb1 N1 C3 92.6(4) 2_666 . . . ? C1 Yb1 N1 C3 -152.3(6) . . . . ? Yb1 Yb1 N1 C3 119.2(4) 2_666 . . . ? N7 Yb1 N1 Yb1 91.79(17) . . . 2_666 ? N4 Yb1 N1 Yb1 -152.88(18) . . . 2_666 ? N2 Yb1 N1 Yb1 -54.12(16) 2_666 . . 2_666 ? N5 Yb1 N1 Yb1 -163.09(15) . . . 2_666 ? N1 Yb1 N1 Yb1 0.0 2_666 . . 2_666 ? C2 Yb1 N1 Yb1 -161.21(15) . . . 2_666 ? C1 Yb1 N1 Yb1 -26.54(17) 2_666 . . 2_666 ? C1 Yb1 N1 Yb1 88.5(4) . . . 2_666 ? N7 Yb1 N4 C2 -68.5(4) . . . . ? N2 Yb1 N4 C2 99.2(3) 2_666 . . . ? N1 Yb1 N4 C2 -163.6(4) . . . . ? N5 Yb1 N4 C2 7.6(3) . . . . ? N1 Yb1 N4 C2 138.5(3) 2_666 . . . ? C1 Yb1 N4 C2 106.8(3) 2_666 . . . ? C1 Yb1 N4 C2 -143.3(3) . . . . ? Yb1 Yb1 N4 C2 175.2(3) 2_666 . . . ? N7 Yb1 N4 C11 147.1(5) . . . . ? N2 Yb1 N4 C11 -45.1(5) 2_666 . . . ? N1 Yb1 N4 C11 52.0(5) . . . . ? N5 Yb1 N4 C11 -136.8(6) . . . . ? N1 Yb1 N4 C11 -5.9(7) 2_666 . . . ? C2 Yb1 N4 C11 -144.3(7) . . . . ? C1 Yb1 N4 C11 -37.5(6) 2_666 . . . ? C1 Yb1 N4 C11 72.3(5) . . . . ? Yb1 Yb1 N4 C11 30.8(5) 2_666 . . . ? N7 Yb1 N5 C2 112.1(3) . . . . ? N4 Yb1 N5 C2 -7.9(3) . . . . ? N2 Yb1 N5 C2 -106.2(3) 2_666 . . . ? N1 Yb1 N5 C2 3.8(4) . . . . ? N1 Yb1 N5 C2 -150.5(3) 2_666 . . . ? C1 Yb1 N5 C2 -127.4(3) 2_666 . . . ? C1 Yb1 N5 C2 36.3(4) . . . . ? Yb1 Yb1 N5 C2 -72.8(6) 2_666 . . . ? N7 Yb1 N5 C19 -39.4(6) . . . . ? N4 Yb1 N5 C19 -159.3(6) . . . . ? N2 Yb1 N5 C19 102.3(6) 2_666 . . . ? N1 Yb1 N5 C19 -147.7(5) . . . . ? N1 Yb1 N5 C19 58.0(6) 2_666 . . . ? C2 Yb1 N5 C19 -151.5(7) . . . . ? C1 Yb1 N5 C19 81.1(6) 2_666 . . . ? C1 Yb1 N5 C19 -115.2(6) . . . . ? Yb1 Yb1 N5 C19 135.7(5) 2_666 . . . ? N4 Yb1 N7 C25 38.5(8) . . . . ? N2 Yb1 N7 C25 -122.4(7) 2_666 . . . ? N1 Yb1 N7 C25 117.6(8) . . . . ? N5 Yb1 N7 C25 -17.3(8) . . . . ? N1 Yb1 N7 C25 -155.6(8) 2_666 . . . ? C2 Yb1 N7 C25 10.0(8) . . . . ? C1 Yb1 N7 C25 -137.4(7) 2_666 . . . ? C1 Yb1 N7 C25 118.9(8) . . . . ? Yb1 Yb1 N7 C25 163.8(8) 2_666 . . . ? C13 N2 C1 N3 11.1(9) . . . . ? Yb1 N2 C1 N3 -160.4(5) 2_666 . . . ? C13 N2 C1 N1 -169.8(6) . . . . ? Yb1 N2 C1 N1 18.7(5) 2_666 . . . ? C13 N2 C1 Yb1 171.5(7) . . . 2_666 ? C13 N2 C1 Yb1 -128.5(5) . . . . ? Yb1 N2 C1 Yb1 60.0(2) 2_666 . . . ? C16 N3 C1 N2 -157.9(6) . . . . ? C16 N3 C1 N1 23.0(9) . . . . ? C16 N3 C1 Yb1 120.9(15) . . . 2_666 ? C16 N3 C1 Yb1 -26.2(8) . . . . ? C3 N1 C1 N2 -128.8(5) . . . . ? Yb1 N1 C1 N2 75.9(5) . . . . ? Yb1 N1 C1 N2 -16.8(5) 2_666 . . . ? C3 N1 C1 N3 50.4(7) . . . . ? Yb1 N1 C1 N3 -105.0(5) . . . . ? Yb1 N1 C1 N3 162.4(5) 2_666 . . . ? C3 N1 C1 Yb1 -112.0(4) . . . 2_666 ? Yb1 N1 C1 Yb1 92.7(2) . . . 2_666 ? C3 N1 C1 Yb1 155.3(5) . . . . ? Yb1 N1 C1 Yb1 -92.7(2) 2_666 . . . ? N7 Yb1 C1 N2 66.1(3) . . . . ? N4 Yb1 C1 N2 -175.4(3) . . . . ? N2 Yb1 C1 N2 -74.7(4) 2_666 . . . ? N1 Yb1 C1 N2 -117.2(5) . . . . ? N5 Yb1 C1 N2 148.2(3) . . . . ? N1 Yb1 C1 N2 -27.2(3) 2_666 . . . ? C2 Yb1 C1 N2 165.9(3) . . . . ? C1 Yb1 C1 N2 -47.2(3) 2_666 . . . ? Yb1 Yb1 C1 N2 -47.2(3) 2_666 . . . ? N7 Yb1 C1 N3 -75.7(5) . . . . ? N4 Yb1 C1 N3 42.8(5) . . . . ? N2 Yb1 C1 N3 143.5(4) 2_666 . . . ? N1 Yb1 C1 N3 101.1(6) . . . . ? N5 Yb1 C1 N3 6.4(6) . . . . ? N1 Yb1 C1 N3 -169.0(5) 2_666 . . . ? C2 Yb1 C1 N3 24.2(5) . . . . ? C1 Yb1 C1 N3 171.0(5) 2_666 . . . ? Yb1 Yb1 C1 N3 171.0(5) 2_666 . . . ? N7 Yb1 C1 N1 -176.7(4) . . . . ? N4 Yb1 C1 N1 -58.3(4) . . . . ? N2 Yb1 C1 N1 42.4(4) 2_666 . . . ? N5 Yb1 C1 N1 -94.6(4) . . . . ? N1 Yb1 C1 N1 89.9(4) 2_666 . . . ? C2 Yb1 C1 N1 -76.9(4) . . . . ? C1 Yb1 C1 N1 70.0(3) 2_666 . . . ? Yb1 Yb1 C1 N1 70.0(3) 2_666 . . . ? N7 Yb1 C1 Yb1 113.34(18) . . . 2_666 ? N4 Yb1 C1 Yb1 -128.21(15) . . . 2_666 ? N2 Yb1 C1 Yb1 -27.51(19) 2_666 . . 2_666 ? N1 Yb1 C1 Yb1 -70.0(3) . . . 2_666 ? N5 Yb1 C1 Yb1 -164.60(16) . . . 2_666 ? N1 Yb1 C1 Yb1 19.98(13) 2_666 . . 2_666 ? C2 Yb1 C1 Yb1 -146.82(14) . . . 2_666 ? C1 Yb1 C1 Yb1 0.0 2_666 . . 2_666 ? C19 N5 C2 N6 -3.6(9) . . . . ? Yb1 N5 C2 N6 -163.0(6) . . . . ? C19 N5 C2 N4 171.3(5) . . . . ? Yb1 N5 C2 N4 11.8(5) . . . . ? C19 N5 C2 Yb1 159.5(6) . . . . ? C22 N6 C2 N5 153.6(7) . . . . ? C22 N6 C2 N4 -20.8(10) . . . . ? C22 N6 C2 Yb1 54(2) . . . . ? C11 N4 C2 N5 133.8(5) . . . . ? Yb1 N4 C2 N5 -12.5(5) . . . . ? C11 N4 C2 N6 -51.3(8) . . . . ? Yb1 N4 C2 N6 162.4(5) . . . . ? C11 N4 C2 Yb1 146.3(6) . . . . ? N7 Yb1 C2 N5 -71.9(3) . . . . ? N4 Yb1 C2 N5 166.5(5) . . . . ? N2 Yb1 C2 N5 79.1(3) 2_666 . . . ? N1 Yb1 C2 N5 -177.1(3) . . . . ? N1 Yb1 C2 N5 65.0(6) 2_666 . . . ? C1 Yb1 C2 N5 69.0(4) 2_666 . . . ? C1 Yb1 C2 N5 -153.8(3) . . . . ? Yb1 Yb1 C2 N5 158.8(2) 2_666 . . . ? N7 Yb1 C2 N6 36.7(18) . . . . ? N4 Yb1 C2 N6 -84.9(18) . . . . ? N2 Yb1 C2 N6 -172.3(18) 2_666 . . . ? N1 Yb1 C2 N6 -68.5(18) . . . . ? N5 Yb1 C2 N6 108.6(19) . . . . ? N1 Yb1 C2 N6 173.7(16) 2_666 . . . ? C1 Yb1 C2 N6 177.6(17) 2_666 . . . ? C1 Yb1 C2 N6 -45.1(18) . . . . ? Yb1 Yb1 C2 N6 -92.6(18) 2_666 . . . ? N7 Yb1 C2 N4 121.6(4) . . . . ? N2 Yb1 C2 N4 -87.5(3) 2_666 . . . ? N1 Yb1 C2 N4 16.3(4) . . . . ? N5 Yb1 C2 N4 -166.5(5) . . . . ? N1 Yb1 C2 N4 -101.5(5) 2_666 . . . ? C1 Yb1 C2 N4 -97.6(4) 2_666 . . . ? C1 Yb1 C2 N4 39.7(4) . . . . ? Yb1 Yb1 C2 N4 -7.7(5) 2_666 . . . ? C1 N1 C3 C4 47.1(6) . . . . ? Yb1 N1 C3 C4 -160.6(4) . . . . ? Yb1 N1 C3 C4 -49.7(5) 2_666 . . . ? C1 N1 C3 C12 -138.0(5) . . . . ? Yb1 N1 C3 C12 14.4(6) . . . . ? Yb1 N1 C3 C12 125.2(4) 2_666 . . . ? C12 C3 C4 C5 -2.8(8) . . . . ? N1 C3 C4 C5 172.4(5) . . . . ? C3 C4 C5 C6 -1.8(9) . . . . ? C4 C5 C6 C7 2.9(10) . . . . ? C5 C6 C7 C8 -179.4(6) . . . . ? C5 C6 C7 C12 0.6(9) . . . . ? C6 C7 C8 C9 -179.7(6) . . . . ? C12 C7 C8 C9 0.3(9) . . . . ? C7 C8 C9 C10 2.9(10) . . . . ? C8 C9 C10 C11 -0.6(10) . . . . ? C9 C10 C11 N4 -179.8(6) . . . . ? C9 C10 C11 C12 -4.8(9) . . . . ? C2 N4 C11 C10 -6.8(8) . . . . ? Yb1 N4 C11 C10 128.2(5) . . . . ? C2 N4 C11 C12 178.2(5) . . . . ? Yb1 N4 C11 C12 -46.7(7) . . . . ? C4 C3 C12 C7 6.0(7) . . . . ? N1 C3 C12 C7 -168.8(5) . . . . ? C4 C3 C12 C11 -173.4(5) . . . . ? N1 C3 C12 C11 11.9(8) . . . . ? C8 C7 C12 C3 175.0(5) . . . . ? C6 C7 C12 C3 -5.0(8) . . . . ? C8 C7 C12 C11 -5.6(8) . . . . ? C6 C7 C12 C11 174.4(5) . . . . ? C10 C11 C12 C3 -173.0(5) . . . . ? N4 C11 C12 C3 2.2(8) . . . . ? C10 C11 C12 C7 7.6(7) . . . . ? N4 C11 C12 C7 -177.2(5) . . . . ? C1 N2 C13 C14 -136.4(7) . . . . ? Yb1 N2 C13 C14 30.5(11) 2_666 . . . ? C1 N2 C13 C15 105.9(7) . . . . ? Yb1 N2 C13 C15 -87.2(8) 2_666 . . . ? C1 N3 C16 C18 119.2(7) . . . . ? C1 N3 C16 C17 -119.5(7) . . . . ? C2 N5 C19 C21 -162.9(5) . . . . ? Yb1 N5 C19 C21 -17.0(8) . . . . ? C2 N5 C19 C20 76.1(7) . . . . ? Yb1 N5 C19 C20 -138.0(5) . . . . ? C2 N6 C22 C24 -93.4(9) . . . . ? C2 N6 C22 C23 144.1(7) . . . . ? Yb1 N7 C25 C26 -28.6(13) . . . . ? Yb1 N7 C25 C30 150.1(7) . . . . ? N7 C25 C26 C27 176.0(7) . . . . ? C30 C25 C26 C27 -2.8(12) . . . . ? C25 C26 C27 C28 1.6(12) . . . . ? C26 C27 C28 C29 -0.7(12) . . . . ? C26 C27 C28 C31 -176.9(7) . . . . ? C27 C28 C29 C30 1.1(12) . . . . ? C31 C28 C29 C30 177.3(8) . . . . ? C28 C29 C30 C25 -2.5(13) . . . . ? C26 C25 C30 C29 3.2(12) . . . . ? N7 C25 C30 C29 -175.5(8) . . . . ? C35 O1 C32 C33 118(7) 2_657 . . . ? C35 O1 C32 C33 17(6) . . . . ? O1 O1 C32 C33 50(7) 2_657 . . . ? O1 C32 C33 C34 -1(5) . . . . ? C32 C33 C34 C35 -27(7) . . . . ? C35 O1 C35 O1 0.000(6) 2_657 . . 2_657 ? C32 O1 C35 O1 125(6) . . . 2_657 ? C35 O1 C35 C34 -144(6) 2_657 . . . ? C32 O1 C35 C34 -19(4) . . . . ? O1 O1 C35 C34 -144(6) 2_657 . . . ? C32 O1 C35 C35 125(6) . . . 2_657 ? O1 O1 C35 C35 0.00(5) 2_657 . . 2_657 ? C33 C34 C35 O1 -45(14) . . . 2_657 ? C33 C34 C35 O1 35(7) . . . . ? C33 C34 C35 C35 15(10) . . . 2_657 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.635 _refine_diff_density_min -1.485 _refine_diff_density_rms 0.137