# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email swwang@mail.ahnu.edu.cn _publ_contact_author_name 'Wang Shaowu' loop_ _publ_author_name 'Zhu Xiancui' 'Zhou Shuangliu' 'Wang Shaowu' 'Yun Wei' 'Zhang Lijun' 'Fenhua Wang' 'Shaoyin Wang' 'Zhijun Feng' data_090714a_0m _database_code_depnum_ccdc_archive 'CCDC 842358' #TrackingRef '- 090714a_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H70 Cl2 Li N7 O Si2 Yb2' _chemical_formula_weight 1253.22 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.0250(14) _cell_length_b 15.9524(15) _cell_length_c 16.6905(16) _cell_angle_alpha 84.3230(10) _cell_angle_beta 65.1050(10) _cell_angle_gamma 78.8840(10) _cell_volume 3560.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7289 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 25.63 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 2.750 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5349 _exptl_absorpt_correction_T_max 0.6373 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30653 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.1090 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.58 _reflns_number_total 15993 _reflns_number_gt 8088 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1341P)^2^+0.5624P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15993 _refine_ls_number_parameters 580 _refine_ls_number_restraints 129 _refine_ls_R_factor_all 0.1450 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.2530 _refine_ls_wR_factor_gt 0.2055 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.107 0.500 0.569 1134 323 ' ' _platon_squeeze_details ; ; 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 C17 C 0.8704(6) 0.6286(5) 0.8444(5) 0.057(3) Uani 1 1 d G . . C18 C 0.8051(6) 0.5751(6) 0.8498(5) 0.079(4) Uani 1 1 d G . . H18 H 0.7684 0.5506 0.9038 0.095 Uiso 1 1 calc R . . C19 C 0.7946(7) 0.5583(6) 0.7743(7) 0.108(6) Uani 1 1 d G . . H19 H 0.7509 0.5226 0.7779 0.130 Uiso 1 1 calc R . . C20 C 0.8495(8) 0.5949(7) 0.6936(6) 0.104(6) Uani 1 1 d G . . H20 H 0.8425 0.5837 0.6431 0.125 Uiso 1 1 calc R . . C21 C 0.9148(7) 0.6484(6) 0.6882(5) 0.079(4) Uani 1 1 d G . . H21 H 0.9515 0.6729 0.6342 0.095 Uiso 1 1 calc R . . C16 C 0.9253(6) 0.6652(5) 0.7637(6) 0.058(3) Uani 1 1 d G . . Yb1 Yb 0.86533(3) 0.58530(3) 1.04796(3) 0.04842(18) Uani 1 1 d . . . Yb2 Yb 0.66699(3) 0.78352(3) 1.12614(3) 0.04964(18) Uani 1 1 d . . . Cl1 Cl 0.8518(2) 0.7347(2) 1.1101(2) 0.0633(9) Uani 1 1 d . . . Cl2 Cl 1.0599(2) 0.5714(2) 1.0144(2) 0.0578(8) Uani 1 1 d . . . Si1 Si 0.6033(3) 0.8032(3) 1.3329(3) 0.0789(12) Uani 1 1 d U . . Si2 Si 0.6729(3) 0.9606(3) 1.2340(3) 0.0826(13) Uani 1 1 d . . . Li1 Li 0.8990(19) 0.814(2) 0.695(2) 0.104(10) Uani 1 1 d . . . N1 N 0.7210(7) 0.5500(6) 1.0806(6) 0.054(2) Uani 1 1 d . . . N2 N 0.5071(7) 0.7830(7) 1.1313(7) 0.062(3) Uani 1 1 d . . . N3 N 0.8981(7) 0.6477(7) 0.9104(7) 0.058(3) Uani 1 1 d . . . N4 N 1.0469(8) 0.7985(8) 0.6469(8) 0.074(3) Uani 1 1 d . . . N5 N 0.7232(7) 0.8408(7) 0.9873(7) 0.060(3) Uani 1 1 d . . . N6 N 0.7650(9) 0.8545(8) 0.6939(8) 0.079(3) Uani 1 1 d . . . N7 N 0.6364(7) 0.8630(7) 1.2385(6) 0.059(3) Uani 1 1 d . . . O1 O 0.8478(7) 0.5353(6) 1.1897(6) 0.070(2) Uani 1 1 d U . . C1 C 0.6710(7) 0.6321(7) 1.0949(7) 0.046(3) Uani 1 1 d . . . C2 C 0.5723(8) 0.6345(8) 1.1066(8) 0.054(3) Uani 1 1 d . . . C3 C 0.5628(9) 0.5467(9) 1.1002(8) 0.060(3) Uani 1 1 d . . . C4 C 0.6590(9) 0.4958(9) 1.0831(9) 0.064(3) Uani 1 1 d . . . C5 C 0.6794(11) 0.4102(10) 1.0744(10) 0.085(5) Uani 1 1 d . . . H5 H 0.7419 0.3783 1.0634 0.102 Uiso 1 1 calc R . . C6 C 0.5927(14) 0.3716(11) 1.0840(12) 0.104(6) Uani 1 1 d . . . H6 H 0.6025 0.3126 1.0789 0.125 Uiso 1 1 calc R . . C7 C 0.4975(13) 0.4174(12) 1.1001(12) 0.099(6) Uani 1 1 d . . . H7 H 0.4450 0.3903 1.1073 0.119 Uiso 1 1 calc R . . C8 C 0.4869(10) 0.4991(11) 1.1044(10) 0.082(4) Uani 1 1 d . . . H8 H 0.4254 0.5306 1.1108 0.098 Uiso 1 1 calc R . . C9 C 0.4971(8) 0.7078(8) 1.1223(8) 0.058(3) Uani 1 1 d . . . H9 H 0.4356 0.7001 1.1262 0.070 Uiso 1 1 calc R . . C10 C 0.4236(11) 0.8550(10) 1.1452(12) 0.081(5) Uani 1 1 d . . . C11 C 0.4589(13) 0.9321(11) 1.1425(14) 0.116(7) Uani 1 1 d . . . H11A H 0.4948 0.9258 1.1791 0.174 Uiso 1 1 calc R . . H11B H 0.4035 0.9779 1.1637 0.174 Uiso 1 1 calc R . . H11C H 0.5022 0.9446 1.0827 0.174 Uiso 1 1 calc R . . C12 C 0.3892(14) 0.8515(14) 1.0689(14) 0.137(8) Uani 1 1 d . . . H12A H 0.4108 0.8969 1.0268 0.206 Uiso 1 1 calc R . . H12B H 0.3179 0.8580 1.0933 0.206 Uiso 1 1 calc R . . H12C H 0.4178 0.7975 1.0402 0.206 Uiso 1 1 calc R . . C13 C 0.3443(14) 0.8491(14) 1.2391(12) 0.133(8) Uani 1 1 d . . . H13A H 0.3183 0.7971 1.2467 0.199 Uiso 1 1 calc R . . H13B H 0.2915 0.8970 1.2494 0.199 Uiso 1 1 calc R . . H13C H 0.3734 0.8495 1.2805 0.199 Uiso 1 1 calc R . . C14 C 0.9656(9) 0.6989(8) 0.8709(9) 0.058(3) Uani 1 1 d . . . H14 H 0.9955 0.7223 0.9001 0.069 Uiso 1 1 calc R . . C15 C 0.9866(9) 0.7138(8) 0.7819(9) 0.061(3) Uani 1 1 d . . . C22 C 1.0533(9) 0.7671(9) 0.7207(10) 0.069(4) Uani 1 1 d . . . H22 H 1.1034 0.7800 0.7338 0.082 Uiso 1 1 calc R . . C23 C 1.1195(14) 0.8495(14) 0.5851(13) 0.112(5) Uani 1 1 d U . . C24 C 1.1854(15) 0.8790(15) 0.6152(13) 0.140(6) Uani 1 1 d U . . H24A H 1.1477 0.9210 0.6598 0.210 Uiso 1 1 calc R . . H24B H 1.2353 0.9039 0.5663 0.210 Uiso 1 1 calc R . . H24C H 1.2169 0.8316 0.6394 0.210 Uiso 1 1 calc R . . C25 C 1.1894(17) 0.7877(15) 0.5203(14) 0.164(7) Uani 1 1 d U . . H25A H 1.1890 0.7316 0.5472 0.246 Uiso 1 1 calc R . . H25B H 1.2551 0.8016 0.4990 0.246 Uiso 1 1 calc R . . H25C H 1.1706 0.7888 0.4719 0.246 Uiso 1 1 calc R . . C26 C 1.0670(16) 0.9204(16) 0.5538(15) 0.166(8) Uani 1 1 d U . . H26A H 1.0205 0.9006 0.5377 0.249 Uiso 1 1 calc R . . H26B H 1.1136 0.9465 0.5032 0.249 Uiso 1 1 calc R . . H26C H 1.0318 0.9616 0.5997 0.249 Uiso 1 1 calc R . . C27 C 0.6834(10) 0.8221(8) 0.9328(9) 0.061(3) Uani 1 1 d . . . H27 H 0.6331 0.7894 0.9499 0.073 Uiso 1 1 calc R . . C28 C 0.7274(9) 0.8581(9) 0.8474(8) 0.065(4) Uani 1 1 d . . . C29 C 0.7982(9) 0.9014(7) 0.8492(9) 0.054(3) Uani 1 1 d . . . C30 C 0.7936(9) 0.8878(9) 0.9364(9) 0.061(3) Uani 1 1 d . . . C31 C 0.8591(12) 0.9193(11) 0.9597(12) 0.092(5) Uani 1 1 d . . . H31 H 0.8590 0.9092 1.0155 0.110 Uiso 1 1 calc R . . C32 C 0.9255(13) 0.9672(11) 0.8948(14) 0.110(7) Uani 1 1 d . . . H32 H 0.9710 0.9875 0.9090 0.132 Uiso 1 1 calc R . . C33 C 0.9280(14) 0.9865(12) 0.8104(13) 0.105(6) Uani 1 1 d . . . H33 H 0.9722 1.0199 0.7704 0.126 Uiso 1 1 calc R . . C34 C 0.8625(13) 0.9541(10) 0.7888(11) 0.088(5) Uani 1 1 d . . . H34 H 0.8608 0.9671 0.7338 0.106 Uiso 1 1 calc R . . C35 C 0.7032(11) 0.8457(10) 0.7752(9) 0.077(4) Uani 1 1 d . . . H35 H 0.6418 0.8312 0.7872 0.092 Uiso 1 1 calc R . . C36 C 0.7291(11) 0.8513(12) 0.6235(10) 0.084(5) Uani 1 1 d . . . C37 C 0.6539(15) 0.7980(14) 0.6422(13) 0.133(8) Uani 1 1 d . . . H37A H 0.6790 0.7403 0.6542 0.199 Uiso 1 1 calc R . . H37B H 0.6380 0.7991 0.5921 0.199 Uiso 1 1 calc R . . H37C H 0.5950 0.8193 0.6927 0.199 Uiso 1 1 calc R . . C38 C 0.8231(14) 0.8131(17) 0.5467(10) 0.162(11) Uani 1 1 d . . . H38A H 0.8676 0.8540 0.5240 0.243 Uiso 1 1 calc R . . H38B H 0.8063 0.7987 0.5009 0.243 Uiso 1 1 calc R . . H38C H 0.8549 0.7625 0.5666 0.243 Uiso 1 1 calc R . . C39 C 0.6881(15) 0.9448(13) 0.6060(13) 0.137(8) Uani 1 1 d . . . H39A H 0.6380 0.9692 0.6603 0.205 Uiso 1 1 calc R . . H39B H 0.6597 0.9458 0.5640 0.205 Uiso 1 1 calc R . . H39C H 0.7414 0.9775 0.5828 0.205 Uiso 1 1 calc R . . C40 C 0.5987(12) 0.6944(10) 1.3050(11) 0.093(4) Uani 1 1 d U . . H40A H 0.5359 0.6943 1.3027 0.140 Uiso 1 1 calc R . . H40B H 0.6061 0.6541 1.3493 0.140 Uiso 1 1 calc R . . H40C H 0.6517 0.6789 1.2486 0.140 Uiso 1 1 calc R . . C41 C 0.4815(13) 0.8462(12) 1.4201(12) 0.119(5) Uani 1 1 d U . . H41A H 0.4909 0.8827 1.4573 0.178 Uiso 1 1 calc R . . H41B H 0.4505 0.7999 1.4550 0.178 Uiso 1 1 calc R . . H41C H 0.4397 0.8784 1.3934 0.178 Uiso 1 1 calc R . . C42 C 0.6961(14) 0.7807(13) 1.3831(13) 0.120(6) Uani 1 1 d U . . H42A H 0.7577 0.7503 1.3419 0.180 Uiso 1 1 calc R . . H42B H 0.6711 0.7467 1.4361 0.180 Uiso 1 1 calc R . . H42C H 0.7072 0.8337 1.3972 0.180 Uiso 1 1 calc R . . C43 C 0.6040(13) 1.0193(10) 1.3426(11) 0.106(6) Uani 1 1 d . . . H43A H 0.5379 1.0440 1.3490 0.159 Uiso 1 1 calc R . . H43B H 0.6388 1.0637 1.3429 0.159 Uiso 1 1 calc R . . H43C H 0.6005 0.9798 1.3908 0.159 Uiso 1 1 calc R . . C44 C 0.8068(11) 0.9545(12) 1.2103(13) 0.118(7) Uani 1 1 d . . . H44A H 0.8147 0.9485 1.2648 0.176 Uiso 1 1 calc R . . H44B H 0.8292 1.0057 1.1797 0.176 Uiso 1 1 calc R . . H44C H 0.8453 0.9061 1.1742 0.176 Uiso 1 1 calc R . . C45 C 0.6465(14) 1.0302(12) 1.1528(12) 0.123(7) Uani 1 1 d . . . H45A H 0.6590 0.9977 1.1027 0.185 Uiso 1 1 calc R . . H45B H 0.6884 1.0731 1.1345 0.185 Uiso 1 1 calc R . . H45C H 0.5780 1.0571 1.1778 0.185 Uiso 1 1 calc R . . C46 C 0.9038(11) 0.5535(10) 1.2363(9) 0.088(4) Uani 1 1 d DU . . H46A H 0.9070 0.6140 1.2322 0.105 Uiso 1 1 calc R . . H46B H 0.9710 0.5217 1.2117 0.105 Uiso 1 1 calc R . . C47 C 0.8493(13) 0.5266(11) 1.3302(9) 0.104(4) Uani 1 1 d DU . . H47A H 0.8960 0.5009 1.3554 0.125 Uiso 1 1 calc R . . H47B H 0.8067 0.5755 1.3651 0.125 Uiso 1 1 calc R . . C48 C 0.7885(13) 0.4634(11) 1.3294(10) 0.113(4) Uani 1 1 d DU . . H48A H 0.7210 0.4769 1.3739 0.136 Uiso 1 1 calc R . . H48B H 0.8171 0.4062 1.3413 0.136 Uiso 1 1 calc R . . C49 C 0.7894(12) 0.4695(10) 1.2370(9) 0.092(4) Uani 1 1 d DU . . H49A H 0.8194 0.4153 1.2074 0.111 Uiso 1 1 calc R . . H49B H 0.7222 0.4848 1.2405 0.111 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C17 0.051(7) 0.050(7) 0.064(9) -0.004(6) -0.021(6) -0.003(5) C18 0.069(9) 0.089(11) 0.083(11) 0.001(9) -0.030(8) -0.028(8) C19 0.129(15) 0.125(15) 0.110(15) -0.001(12) -0.070(13) -0.062(12) C20 0.123(14) 0.148(17) 0.073(12) 0.020(11) -0.057(11) -0.070(13) C21 0.082(10) 0.099(12) 0.051(9) 0.017(8) -0.027(7) -0.016(9) C16 0.052(7) 0.068(8) 0.056(8) -0.001(7) -0.026(6) -0.009(6) Yb1 0.0385(3) 0.0538(3) 0.0499(3) -0.0049(2) -0.0150(2) -0.0063(2) Yb2 0.0435(3) 0.0582(4) 0.0474(3) -0.0071(3) -0.0194(2) -0.0043(2) Cl1 0.0477(15) 0.068(2) 0.080(2) -0.0212(17) -0.0322(15) 0.0006(14) Cl2 0.0420(14) 0.0594(19) 0.073(2) -0.0162(16) -0.0234(14) -0.0025(13) Si1 0.076(2) 0.105(3) 0.055(2) -0.019(2) -0.029(2) 0.000(2) Si2 0.070(3) 0.090(3) 0.092(3) -0.034(3) -0.034(2) -0.003(2) Li1 0.062(15) 0.15(3) 0.11(2) 0.03(2) -0.045(16) -0.034(16) N1 0.043(5) 0.060(7) 0.055(6) -0.003(5) -0.016(4) -0.007(5) N2 0.046(5) 0.076(8) 0.068(7) -0.001(6) -0.025(5) -0.014(5) N3 0.057(6) 0.062(7) 0.055(7) 0.001(5) -0.021(5) -0.016(5) N4 0.054(6) 0.077(8) 0.075(8) 0.001(7) -0.013(6) -0.005(6) N5 0.060(6) 0.071(7) 0.049(6) 0.005(5) -0.023(5) -0.013(5) N6 0.092(9) 0.076(8) 0.069(8) -0.009(7) -0.038(7) -0.002(7) N7 0.058(6) 0.067(7) 0.051(6) -0.020(5) -0.019(5) -0.005(5) O1 0.068(5) 0.078(5) 0.065(5) 0.000(4) -0.028(4) -0.013(4) C1 0.032(5) 0.058(7) 0.049(7) 0.001(6) -0.016(5) -0.012(5) C2 0.051(6) 0.063(8) 0.048(7) -0.008(6) -0.015(5) -0.018(6) C3 0.054(7) 0.072(9) 0.054(8) -0.003(7) -0.020(6) -0.016(6) C4 0.060(7) 0.065(9) 0.064(9) -0.009(7) -0.020(6) -0.015(7) C5 0.071(9) 0.082(11) 0.093(12) -0.027(9) -0.016(8) -0.022(8) C6 0.108(14) 0.077(12) 0.119(15) -0.019(10) -0.033(12) -0.021(10) C7 0.084(11) 0.090(13) 0.132(16) -0.030(12) -0.044(11) -0.024(10) C8 0.053(8) 0.098(13) 0.095(12) -0.014(10) -0.027(8) -0.015(8) C9 0.043(6) 0.066(9) 0.063(8) 0.010(7) -0.022(6) -0.009(6) C10 0.061(8) 0.078(11) 0.111(13) -0.011(9) -0.051(9) 0.014(8) C11 0.096(13) 0.068(11) 0.18(2) -0.019(13) -0.062(14) 0.018(10) C12 0.112(14) 0.18(2) 0.149(19) 0.014(16) -0.103(15) 0.026(14) C13 0.105(14) 0.17(2) 0.085(14) -0.037(13) -0.027(11) 0.055(14) C14 0.051(7) 0.052(8) 0.071(9) 0.005(7) -0.031(6) 0.000(6) C15 0.057(7) 0.056(8) 0.067(9) 0.009(7) -0.027(7) -0.004(6) C22 0.045(7) 0.070(9) 0.080(10) 0.009(8) -0.019(7) -0.006(6) C23 0.087(10) 0.147(13) 0.088(10) 0.049(8) -0.019(7) -0.052(8) C24 0.131(13) 0.181(16) 0.108(12) 0.044(11) -0.032(9) -0.093(11) C25 0.150(15) 0.184(16) 0.101(13) 0.010(10) 0.016(11) -0.065(11) C26 0.132(13) 0.193(16) 0.139(14) 0.110(12) -0.037(10) -0.054(11) C27 0.059(7) 0.065(8) 0.057(8) -0.003(7) -0.027(6) 0.000(6) C28 0.062(8) 0.079(10) 0.046(8) -0.001(7) -0.023(6) 0.008(7) C29 0.054(7) 0.044(7) 0.059(8) -0.004(6) -0.020(6) -0.003(5) C30 0.051(7) 0.066(9) 0.064(9) -0.005(7) -0.021(6) -0.005(6) C31 0.090(11) 0.094(12) 0.092(13) -0.017(10) -0.037(10) -0.009(9) C32 0.088(12) 0.094(13) 0.131(18) -0.033(12) -0.011(12) -0.040(10) C33 0.109(14) 0.100(14) 0.086(14) -0.009(11) -0.007(11) -0.045(11) C34 0.103(12) 0.068(10) 0.069(11) 0.003(8) -0.011(9) -0.018(9) C35 0.068(9) 0.102(12) 0.050(9) -0.007(8) -0.021(7) 0.003(8) C36 0.066(9) 0.128(14) 0.053(9) -0.014(9) -0.023(7) -0.003(9) C37 0.155(19) 0.18(2) 0.106(16) 0.013(15) -0.081(15) -0.061(17) C38 0.111(15) 0.31(3) 0.042(10) -0.052(15) -0.026(10) 0.023(18) C39 0.146(18) 0.16(2) 0.112(16) 0.048(15) -0.083(15) -0.010(15) C40 0.102(8) 0.094(7) 0.081(8) 0.005(6) -0.038(6) -0.012(6) C41 0.106(7) 0.122(9) 0.104(9) -0.011(7) -0.025(6) -0.001(7) C42 0.123(8) 0.141(10) 0.121(10) -0.006(7) -0.077(8) -0.015(7) C43 0.127(14) 0.093(12) 0.119(15) -0.062(11) -0.066(12) 0.003(10) C44 0.073(10) 0.151(17) 0.147(18) -0.041(14) -0.053(12) -0.023(11) C45 0.132(17) 0.107(15) 0.112(16) -0.029(13) -0.026(13) -0.018(12) C46 0.088(6) 0.104(7) 0.082(6) 0.001(6) -0.048(5) -0.011(5) C47 0.113(8) 0.115(8) 0.081(6) 0.005(6) -0.042(6) -0.010(6) C48 0.125(8) 0.112(8) 0.088(6) 0.010(6) -0.032(6) -0.020(6) C49 0.095(7) 0.089(7) 0.086(7) 0.012(6) -0.030(5) -0.023(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 C17 C18 1.3900 . ? C17 C16 1.3900 . ? C17 N3 1.407(12) . ? C18 C19 1.3900 . ? C18 H18 0.9300 . ? C19 C20 1.3900 . ? C19 H19 0.9300 . ? C20 C21 1.3900 . ? C20 H20 0.9300 . ? C21 C16 1.3900 . ? C21 Li1 2.61(4) . ? C21 H21 0.9300 . ? C16 C15 1.448(15) . ? C16 Li1 2.56(3) . ? Yb1 N1 2.176(9) . ? Yb1 N3 2.299(10) . ? Yb1 O1 2.342(9) . ? Yb1 Cl1 2.631(3) . ? Yb1 Cl2 2.654(3) 2_767 ? Yb1 C1 2.654(10) . ? Yb1 Cl2 2.703(3) . ? Yb1 Yb2 3.8068(7) . ? Yb2 N7 2.203(9) . ? Yb2 N5 2.269(10) . ? Yb2 N2 2.368(9) . ? Yb2 C1 2.505(12) . ? Yb2 Cl1 2.641(3) . ? Yb2 C2 3.104(12) . ? Yb2 C27 3.139(13) . ? Cl2 Yb1 2.654(3) 2_767 ? Si1 N7 1.693(11) . ? Si1 C41 1.846(17) . ? Si1 C40 1.862(17) . ? Si1 C42 1.873(16) . ? Si2 N7 1.732(11) . ? Si2 C45 1.792(19) . ? Si2 C44 1.864(15) . ? Si2 C43 1.902(15) . ? Li1 N4 1.99(3) . ? Li1 N6 2.00(3) . ? Li1 C22 2.49(3) . ? Li1 C15 2.59(3) . ? Li1 C35 2.64(3) . ? Li1 C34 2.70(4) . ? Li1 C29 2.74(4) . ? Li1 C28 2.78(3) . ? N1 C4 1.372(15) . ? N1 C1 1.368(14) . ? N2 C9 1.269(15) . ? N2 C10 1.483(16) . ? N3 C14 1.334(15) . ? N4 C22 1.318(17) . ? N4 C23 1.465(19) . ? N5 C30 1.351(16) . ? N5 C27 1.363(16) . ? N6 C35 1.294(17) . ? N6 C36 1.493(18) . ? O1 C46 1.444(16) . ? O1 C49 1.451(17) . ? C1 C2 1.406(14) . ? C2 C9 1.420(16) . ? C2 C3 1.452(17) . ? C3 C4 1.441(17) . ? C3 C8 1.464(18) . ? C4 C5 1.350(19) . ? C5 C6 1.49(2) . ? C5 H5 0.9300 . ? C6 C7 1.40(2) . ? C6 H6 0.9300 . ? C7 C8 1.29(2) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.42(2) . ? C10 C13 1.53(2) . ? C10 C12 1.57(2) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.389(18) . ? C14 H14 0.9300 . ? C15 C22 1.437(18) . ? C22 H22 0.9300 . ? C23 C26 1.44(3) . ? C23 C25 1.45(3) . ? C23 C24 1.45(3) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.410(18) . ? C27 H27 0.9300 . ? C28 C29 1.387(18) . ? C28 C35 1.438(19) . ? C29 C34 1.408(19) . ? C29 C30 1.423(18) . ? C30 C31 1.387(19) . ? C31 C32 1.40(2) . ? C31 H31 0.9300 . ? C32 C33 1.40(2) . ? C32 H32 0.9300 . ? C33 C34 1.38(2) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.46(2) . ? C36 C38 1.52(2) . ? C36 C39 1.55(2) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C47 1.494(14) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.489(15) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.529(15) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C18 C17 C16 120.0 . . ? C18 C17 N3 128.8(7) . . ? C16 C17 N3 111.0(7) . . ? C17 C18 C19 120.0 . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 120.0 . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.0 . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C16 C21 C20 120.0 . . ? C16 C21 Li1 72.5(8) . . ? C20 C21 Li1 133.7(7) . . ? C16 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? Li1 C21 H21 67.1 . . ? C21 C16 C17 120.0 . . ? C21 C16 C15 134.8(8) . . ? C17 C16 C15 105.1(8) . . ? C21 C16 Li1 76.4(9) . . ? C17 C16 Li1 131.9(8) . . ? C15 C16 Li1 74.8(9) . . ? N1 Yb1 N3 101.0(4) . . ? N1 Yb1 O1 86.9(3) . . ? N3 Yb1 O1 171.1(3) . . ? N1 Yb1 Cl1 113.0(3) . . ? N3 Yb1 Cl1 89.5(3) . . ? O1 Yb1 Cl1 83.7(2) . . ? N1 Yb1 Cl2 85.4(3) . 2_767 ? N3 Yb1 Cl2 93.8(3) . 2_767 ? O1 Yb1 Cl2 90.7(2) . 2_767 ? Cl1 Yb1 Cl2 160.30(9) . 2_767 ? N1 Yb1 C1 30.9(3) . . ? N3 Yb1 C1 90.9(3) . . ? O1 Yb1 C1 94.1(3) . . ? Cl1 Yb1 C1 84.0(3) . . ? Cl2 Yb1 C1 115.3(3) 2_767 . ? N1 Yb1 Cl2 160.5(3) . . ? N3 Yb1 Cl2 89.1(3) . . ? O1 Yb1 Cl2 84.5(2) . . ? Cl1 Yb1 Cl2 83.38(9) . . ? Cl2 Yb1 Cl2 77.27(10) 2_767 . ? C1 Yb1 Cl2 167.3(3) . . ? N1 Yb1 Yb2 71.6(3) . . ? N3 Yb1 Yb2 83.6(3) . . ? O1 Yb1 Yb2 95.3(2) . . ? Cl1 Yb1 Yb2 43.88(6) . . ? Cl2 Yb1 Yb2 155.81(6) 2_767 . ? C1 Yb1 Yb2 41.0(3) . . ? Cl2 Yb1 Yb2 126.57(7) . . ? N1 Yb1 Yb1 123.9(3) . 2_767 ? N3 Yb1 Yb1 91.8(3) . 2_767 ? O1 Yb1 Yb1 86.9(2) . 2_767 ? Cl1 Yb1 Yb1 121.51(6) . 2_767 ? Cl2 Yb1 Yb1 39.05(6) 2_767 2_767 ? C1 Yb1 Yb1 154.4(3) . 2_767 ? Cl2 Yb1 Yb1 38.21(6) . 2_767 ? Yb2 Yb1 Yb1 164.44(2) . 2_767 ? N7 Yb2 N5 119.4(4) . . ? N7 Yb2 N2 103.7(4) . . ? N5 Yb2 N2 93.0(4) . . ? N7 Yb2 C1 139.6(4) . . ? N5 Yb2 C1 100.9(4) . . ? N2 Yb2 C1 75.8(4) . . ? N7 Yb2 Cl1 89.5(3) . . ? N5 Yb2 Cl1 90.3(3) . . ? N2 Yb2 Cl1 162.6(3) . . ? C1 Yb2 Cl1 86.8(2) . . ? N7 Yb2 C2 132.8(3) . . ? N5 Yb2 C2 102.1(4) . . ? N2 Yb2 C2 49.6(4) . . ? C1 Yb2 C2 26.4(3) . . ? Cl1 Yb2 C2 113.0(2) . . ? N7 Yb2 C27 134.6(4) . . ? N5 Yb2 C27 22.7(4) . . ? N2 Yb2 C27 73.4(4) . . ? C1 Yb2 C27 84.9(4) . . ? Cl1 Yb2 C27 105.5(2) . . ? C2 Yb2 C27 80.6(3) . . ? N7 Yb2 Yb1 126.3(3) . . ? N5 Yb2 Yb1 90.7(3) . . ? N2 Yb2 Yb1 119.1(3) . . ? C1 Yb2 Yb1 44.0(2) . . ? Cl1 Yb2 Yb1 43.68(7) . . ? C2 Yb2 Yb1 70.3(2) . . ? C27 Yb2 Yb1 90.2(2) . . ? Yb1 Cl1 Yb2 92.44(9) . . ? Yb1 Cl2 Yb1 102.73(10) 2_767 . ? N7 Si1 C41 114.0(7) . . ? N7 Si1 C40 107.7(6) . . ? C41 Si1 C40 108.7(8) . . ? N7 Si1 C42 115.5(8) . . ? C41 Si1 C42 107.8(9) . . ? C40 Si1 C42 102.5(8) . . ? N7 Si2 C45 110.7(7) . . ? N7 Si2 C44 114.9(7) . . ? C45 Si2 C44 108.2(9) . . ? N7 Si2 C43 112.6(7) . . ? C45 Si2 C43 106.0(8) . . ? C44 Si2 C43 103.9(8) . . ? N4 Li1 N6 155.6(17) . . ? N4 Li1 C22 31.7(6) . . ? N6 Li1 C22 171.4(18) . . ? N4 Li1 C16 83.3(11) . . ? N6 Li1 C16 116.5(13) . . ? C22 Li1 C16 61.4(7) . . ? N4 Li1 C15 62.3(8) . . ? N6 Li1 C15 141.8(14) . . ? C22 Li1 C15 32.8(5) . . ? C16 Li1 C15 32.7(5) . . ? N4 Li1 C21 88.5(12) . . ? N6 Li1 C21 101.6(12) . . ? C22 Li1 C21 80.5(10) . . ? C16 Li1 C21 31.2(4) . . ? C15 Li1 C21 60.5(8) . . ? N4 Li1 C35 172.3(19) . . ? N6 Li1 C35 28.4(6) . . ? C22 Li1 C35 143.4(14) . . ? C16 Li1 C35 97.8(10) . . ? C15 Li1 C35 115.2(12) . . ? C21 Li1 C35 96.4(10) . . ? N4 Li1 C34 96.3(13) . . ? N6 Li1 C34 86.1(13) . . ? C22 Li1 C34 88.1(11) . . ? C16 Li1 C34 119.7(12) . . ? C15 Li1 C34 95.6(11) . . ? C21 Li1 C34 149.8(13) . . ? C35 Li1 C34 76.5(10) . . ? N4 Li1 C29 115.5(14) . . ? N6 Li1 C29 77.6(11) . . ? C22 Li1 C29 94.2(11) . . ? C16 Li1 C29 97.5(10) . . ? C15 Li1 C29 85.0(10) . . ? C21 Li1 C29 122.8(11) . . ? C35 Li1 C29 56.8(8) . . ? C34 Li1 C29 30.0(6) . . ? N4 Li1 C28 142.2(15) . . ? N6 Li1 C28 57.0(8) . . ? C22 Li1 C28 114.4(12) . . ? C16 Li1 C28 89.1(9) . . ? C15 Li1 C28 92.6(10) . . ? C21 Li1 C28 103.7(10) . . ? C35 Li1 C28 30.6(5) . . ? C34 Li1 C28 56.1(8) . . ? C29 Li1 C28 29.1(5) . . ? C4 N1 C1 110.4(10) . . ? C4 N1 Yb1 154.3(9) . . ? C1 N1 Yb1 94.2(7) . . ? C9 N2 C10 120.2(11) . . ? C9 N2 Yb2 110.4(8) . . ? C10 N2 Yb2 129.3(9) . . ? C14 N3 C17 105.2(10) . . ? C14 N3 Yb1 124.4(9) . . ? C17 N3 Yb1 129.2(7) . . ? C22 N4 C23 120.8(13) . . ? C22 N4 Li1 95.6(12) . . ? C23 N4 Li1 132.8(14) . . ? C30 N5 C27 104.6(11) . . ? C30 N5 Yb2 137.9(9) . . ? C27 N5 Yb2 117.4(9) . . ? C35 N6 C36 117.8(13) . . ? C35 N6 Li1 104.2(13) . . ? C36 N6 Li1 130.8(14) . . ? Si1 N7 Si2 120.7(6) . . ? Si1 N7 Yb2 109.8(5) . . ? Si2 N7 Yb2 127.1(6) . . ? C46 O1 C49 110.0(10) . . ? C46 O1 Yb1 126.2(8) . . ? C49 O1 Yb1 123.1(8) . . ? N1 C1 C2 109.6(10) . . ? N1 C1 Yb2 148.6(7) . . ? C2 C1 Yb2 101.3(8) . . ? N1 C1 Yb1 54.9(5) . . ? C2 C1 Yb1 162.8(9) . . ? Yb2 C1 Yb1 95.1(3) . . ? C1 C2 C9 126.8(11) . . ? C1 C2 C3 106.0(10) . . ? C9 C2 C3 127.2(11) . . ? C1 C2 Yb2 52.3(6) . . ? C9 C2 Yb2 74.7(7) . . ? C3 C2 Yb2 157.6(8) . . ? C4 C3 C2 106.5(10) . . ? C4 C3 C8 115.0(12) . . ? C2 C3 C8 138.5(12) . . ? C5 C4 N1 128.5(13) . . ? C5 C4 C3 124.0(13) . . ? N1 C4 C3 107.5(11) . . ? C4 C5 C6 113.9(14) . . ? C4 C5 H5 123.0 . . ? C6 C5 H5 123.0 . . ? C7 C6 C5 124.9(16) . . ? C7 C6 H6 117.6 . . ? C5 C6 H6 117.6 . . ? C8 C7 C6 116.2(15) . . ? C8 C7 H7 121.9 . . ? C6 C7 H7 121.9 . . ? C7 C8 C3 125.8(14) . . ? C7 C8 H8 117.1 . . ? C3 C8 H8 117.1 . . ? N2 C9 C2 125.3(11) . . ? N2 C9 H9 117.4 . . ? C2 C9 H9 117.4 . . ? C11 C10 N2 108.1(12) . . ? C11 C10 C13 104.6(16) . . ? N2 C10 C13 109.1(13) . . ? C11 C10 C12 112.2(16) . . ? N2 C10 C12 106.6(13) . . ? C13 C10 C12 116.0(15) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 C15 113.3(12) . . ? N3 C14 H14 123.4 . . ? C15 C14 H14 123.4 . . ? C14 C15 C22 127.7(13) . . ? C14 C15 C16 105.3(11) . . ? C22 C15 C16 127.0(12) . . ? C14 C15 Li1 134.4(12) . . ? C22 C15 Li1 69.9(9) . . ? C16 C15 Li1 72.6(9) . . ? N4 C22 C15 123.1(13) . . ? N4 C22 Li1 52.6(9) . . ? C15 C22 Li1 77.3(10) . . ? N4 C22 H22 118.4 . . ? C15 C22 H22 118.4 . . ? Li1 C22 H22 150.2 . . ? C26 C23 C25 117(2) . . ? C26 C23 C24 110(2) . . ? C25 C23 C24 100.6(19) . . ? C26 C23 N4 108.2(16) . . ? C25 C23 N4 103.0(17) . . ? C24 C23 N4 117.8(16) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N5 C27 C28 112.0(13) . . ? N5 C27 Yb2 40.0(6) . . ? C28 C27 Yb2 151.9(10) . . ? N5 C27 H27 124.0 . . ? C28 C27 H27 124.0 . . ? Yb2 C27 H27 84.1 . . ? C29 C28 C27 105.9(12) . . ? C29 C28 C35 129.8(13) . . ? C27 C28 C35 124.2(14) . . ? C29 C28 Li1 73.6(10) . . ? C27 C28 Li1 135.9(11) . . ? C35 C28 Li1 69.0(9) . . ? C28 C29 C34 134.7(14) . . ? C28 C29 C30 105.2(11) . . ? C34 C29 C30 120.1(13) . . ? C28 C29 Li1 77.3(9) . . ? C34 C29 Li1 73.4(11) . . ? C30 C29 Li1 134.5(10) . . ? N5 C30 C31 127.4(14) . . ? N5 C30 C29 112.2(12) . . ? C31 C30 C29 120.3(13) . . ? C30 C31 C32 116.8(17) . . ? C30 C31 H31 121.6 . . ? C32 C31 H31 121.6 . . ? C33 C32 C31 124.5(18) . . ? C33 C32 H32 117.7 . . ? C31 C32 H32 117.7 . . ? C34 C33 C32 117.5(17) . . ? C34 C33 H33 121.2 . . ? C32 C33 H33 121.2 . . ? C33 C34 C29 120.5(16) . . ? C33 C34 Li1 127.9(14) . . ? C29 C34 Li1 76.6(10) . . ? C33 C34 H34 119.8 . . ? C29 C34 H34 119.8 . . ? Li1 C34 H34 67.3 . . ? N6 C35 C28 121.5(14) . . ? N6 C35 Li1 47.4(10) . . ? C28 C35 Li1 80.4(11) . . ? N6 C35 H35 119.3 . . ? C28 C35 H35 119.3 . . ? Li1 C35 H35 149.7 . . ? C37 C36 N6 116.5(14) . . ? C37 C36 C38 108.3(17) . . ? N6 C36 C38 102.5(12) . . ? C37 C36 C39 109.7(15) . . ? N6 C36 C39 106.3(14) . . ? C38 C36 C39 113.5(17) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si1 C40 H40A 109.5 . . ? Si1 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si1 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si1 C41 H41A 109.5 . . ? Si1 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si1 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si1 C42 H42A 109.5 . . ? Si1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si2 C43 H43A 109.5 . . ? Si2 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si2 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si2 C44 H44A 109.5 . . ? Si2 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si2 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si2 C45 H45A 109.5 . . ? Si2 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si2 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O1 C46 C47 105.8(11) . . ? O1 C46 H46A 110.6 . . ? C47 C46 H46A 110.6 . . ? O1 C46 H46B 110.6 . . ? C47 C46 H46B 110.6 . . ? H46A C46 H46B 108.7 . . ? C48 C47 C46 106.7(10) . . ? C48 C47 H47A 110.4 . . ? C46 C47 H47A 110.4 . . ? C48 C47 H47B 110.4 . . ? C46 C47 H47B 110.4 . . ? H47A C47 H47B 108.6 . . ? C47 C48 C49 106.3(10) . . ? C47 C48 H48A 110.5 . . ? C49 C48 H48A 110.5 . . ? C47 C48 H48B 110.5 . . ? C49 C48 H48B 110.5 . . ? H48A C48 H48B 108.7 . . ? O1 C49 C48 105.9(11) . . ? O1 C49 H49A 110.6 . . ? C48 C49 H49A 110.6 . . ? O1 C49 H49B 110.6 . . ? C48 C49 H49B 110.6 . . ? H49A C49 H49B 108.7 . . ? 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 C16 C17 C18 C19 0.0 . . . . ? N3 C17 C18 C19 -173.9(10) . . . . ? C17 C18 C19 C20 0.0 . . . . ? C18 C19 C20 C21 0.0 . . . . ? C19 C20 C21 C16 0.0 . . . . ? C19 C20 C21 Li1 -94.0(11) . . . . ? C20 C21 C16 C17 0.0 . . . . ? Li1 C21 C16 C17 130.8(7) . . . . ? C20 C21 C16 C15 177.6(11) . . . . ? Li1 C21 C16 C15 -51.6(11) . . . . ? C20 C21 C16 Li1 -130.8(7) . . . . ? C18 C17 C16 C21 0.0 . . . . ? N3 C17 C16 C21 174.9(8) . . . . ? C18 C17 C16 C15 -178.2(8) . . . . ? N3 C17 C16 C15 -3.3(9) . . . . ? C18 C17 C16 Li1 98.8(10) . . . . ? N3 C17 C16 Li1 -86.3(12) . . . . ? N1 Yb1 Yb2 N7 121.7(4) . . . . ? N3 Yb1 Yb2 N7 -134.4(4) . . . . ? O1 Yb1 Yb2 N7 36.7(4) . . . . ? Cl1 Yb1 Yb2 N7 -38.4(4) . . . . ? Cl2 Yb1 Yb2 N7 140.6(4) 2_767 . . . ? C1 Yb1 Yb2 N7 126.8(5) . . . . ? Cl2 Yb1 Yb2 N7 -50.3(4) . . . . ? Yb1 Yb1 Yb2 N7 -60.9(4) 2_767 . . . ? N1 Yb1 Yb2 N5 -110.1(4) . . . . ? N3 Yb1 Yb2 N5 -6.3(4) . . . . ? O1 Yb1 Yb2 N5 164.9(4) . . . . ? Cl1 Yb1 Yb2 N5 89.7(3) . . . . ? Cl2 Yb1 Yb2 N5 -91.2(3) 2_767 . . . ? C1 Yb1 Yb2 N5 -105.0(5) . . . . ? Cl2 Yb1 Yb2 N5 77.9(3) . . . . ? Yb1 Yb1 Yb2 N5 67.3(3) 2_767 . . . ? N1 Yb1 Yb2 N2 -16.4(4) . . . . ? N3 Yb1 Yb2 N2 87.5(4) . . . . ? O1 Yb1 Yb2 N2 -101.3(4) . . . . ? Cl1 Yb1 Yb2 N2 -176.5(3) . . . . ? Cl2 Yb1 Yb2 N2 2.5(3) 2_767 . . . ? C1 Yb1 Yb2 N2 -11.2(5) . . . . ? Cl2 Yb1 Yb2 N2 171.6(3) . . . . ? Yb1 Yb1 Yb2 N2 161.1(3) 2_767 . . . ? N1 Yb1 Yb2 C1 -5.2(5) . . . . ? N3 Yb1 Yb2 C1 98.7(4) . . . . ? O1 Yb1 Yb2 C1 -90.1(4) . . . . ? Cl1 Yb1 Yb2 C1 -165.3(4) . . . . ? Cl2 Yb1 Yb2 C1 13.7(4) 2_767 . . . ? Cl2 Yb1 Yb2 C1 -177.2(4) . . . . ? Yb1 Yb1 Yb2 C1 172.3(4) 2_767 . . . ? N1 Yb1 Yb2 Cl1 160.1(3) . . . . ? N3 Yb1 Yb2 Cl1 -96.0(3) . . . . ? O1 Yb1 Yb2 Cl1 75.2(3) . . . . ? Cl2 Yb1 Yb2 Cl1 179.0(2) 2_767 . . . ? C1 Yb1 Yb2 Cl1 165.3(4) . . . . ? Cl2 Yb1 Yb2 Cl1 -11.90(14) . . . . ? Yb1 Yb1 Yb2 Cl1 -22.46(14) 2_767 . . . ? N1 Yb1 Yb2 C2 -7.6(4) . . . . ? N3 Yb1 Yb2 C2 96.3(3) . . . . ? O1 Yb1 Yb2 C2 -92.5(3) . . . . ? Cl1 Yb1 Yb2 C2 -167.7(3) . . . . ? Cl2 Yb1 Yb2 C2 11.3(3) 2_767 . . . ? C1 Yb1 Yb2 C2 -2.4(4) . . . . ? Cl2 Yb1 Yb2 C2 -179.6(3) . . . . ? Yb1 Yb1 Yb2 C2 169.9(3) 2_767 . . . ? N1 Yb1 Yb2 C27 -87.5(4) . . . . ? N3 Yb1 Yb2 C27 16.4(4) . . . . ? O1 Yb1 Yb2 C27 -172.4(3) . . . . ? Cl1 Yb1 Yb2 C27 112.4(3) . . . . ? Cl2 Yb1 Yb2 C27 -68.6(3) 2_767 . . . ? C1 Yb1 Yb2 C27 -82.3(5) . . . . ? Cl2 Yb1 Yb2 C27 100.5(3) . . . . ? Yb1 Yb1 Yb2 C27 90.0(3) 2_767 . . . ? N1 Yb1 Cl1 Yb2 -20.5(3) . . . . ? N3 Yb1 Cl1 Yb2 81.3(3) . . . . ? O1 Yb1 Cl1 Yb2 -104.5(2) . . . . ? Cl2 Yb1 Cl1 Yb2 -178.8(3) 2_767 . . . ? C1 Yb1 Cl1 Yb2 -9.7(2) . . . . ? Cl2 Yb1 Cl1 Yb2 170.40(11) . . . . ? Yb1 Yb1 Cl1 Yb2 173.10(4) 2_767 . . . ? N7 Yb2 Cl1 Yb1 149.9(3) . . . . ? N5 Yb2 Cl1 Yb1 -90.7(3) . . . . ? N2 Yb2 Cl1 Yb1 10.4(9) . . . . ? C1 Yb2 Cl1 Yb1 10.2(3) . . . . ? C2 Yb2 Cl1 Yb1 12.6(3) . . . . ? C27 Yb2 Cl1 Yb1 -73.6(3) . . . . ? N1 Yb1 Cl2 Yb1 27.9(8) . . . 2_767 ? N3 Yb1 Cl2 Yb1 -94.1(3) . . . 2_767 ? O1 Yb1 Cl2 Yb1 92.0(3) . . . 2_767 ? Cl1 Yb1 Cl2 Yb1 176.29(12) . . . 2_767 ? Cl2 Yb1 Cl2 Yb1 0.0 2_767 . . 2_767 ? C1 Yb1 Cl2 Yb1 176.0(11) . . . 2_767 ? Yb2 Yb1 Cl2 Yb1 -175.44(5) . . . 2_767 ? C21 C16 Li1 N4 -98.2(11) . . . . ? C17 C16 Li1 N4 143.6(8) . . . . ? C15 C16 Li1 N4 46.7(10) . . . . ? C21 C16 Li1 N6 67.0(15) . . . . ? C17 C16 Li1 N6 -51(2) . . . . ? C15 C16 Li1 N6 -148.2(18) . . . . ? C21 C16 Li1 C22 -122.5(8) . . . . ? C17 C16 Li1 C22 119.3(8) . . . . ? C15 C16 Li1 C22 22.4(8) . . . . ? C21 C16 Li1 C15 -144.8(8) . . . . ? C17 C16 Li1 C15 96.9(10) . . . . ? C17 C16 Li1 C21 -118.3(7) . . . . ? C15 C16 Li1 C21 144.8(8) . . . . ? C21 C16 Li1 C35 89.5(9) . . . . ? C17 C16 Li1 C35 -28.8(15) . . . . ? C15 C16 Li1 C35 -125.7(12) . . . . ? C21 C16 Li1 C34 168.3(12) . . . . ? C17 C16 Li1 C34 50.0(14) . . . . ? C15 C16 Li1 C34 -46.8(11) . . . . ? C21 C16 Li1 C29 146.8(8) . . . . ? C17 C16 Li1 C29 28.6(13) . . . . ? C15 C16 Li1 C29 -68.3(9) . . . . ? C21 C16 Li1 C28 118.9(8) . . . . ? C17 C16 Li1 C28 0.6(13) . . . . ? C15 C16 Li1 C28 -96.2(10) . . . . ? C16 C21 Li1 N4 79.6(9) . . . . ? C20 C21 Li1 N4 -165.4(7) . . . . ? C16 C21 Li1 N6 -122.8(13) . . . . ? C20 C21 Li1 N6 -7.7(18) . . . . ? C16 C21 Li1 C22 48.7(7) . . . . ? C20 C21 Li1 C22 163.7(6) . . . . ? C20 C21 Li1 C16 115.0(7) . . . . ? C16 C21 Li1 C15 20.9(5) . . . . ? C20 C21 Li1 C15 136.0(7) . . . . ? C16 C21 Li1 C35 -94.5(9) . . . . ? C20 C21 Li1 C35 20.6(15) . . . . ? C16 C21 Li1 C34 -20(2) . . . . ? C20 C21 Li1 C34 95(2) . . . . ? C16 C21 Li1 C29 -40.2(10) . . . . ? C20 C21 Li1 C29 74.9(15) . . . . ? C16 C21 Li1 C28 -64.3(8) . . . . ? C20 C21 Li1 C28 50.8(14) . . . . ? N3 Yb1 N1 C4 91(2) . . . . ? O1 Yb1 N1 C4 -93(2) . . . . ? Cl1 Yb1 N1 C4 -175(2) . . . . ? Cl2 Yb1 N1 C4 -2(2) 2_767 . . . ? C1 Yb1 N1 C4 164(2) . . . . ? Cl2 Yb1 N1 C4 -29(3) . . . . ? Yb2 Yb1 N1 C4 170(2) . . . . ? Yb1 Yb1 N1 C4 -9(2) 2_767 . . . ? N3 Yb1 N1 C1 -72.8(7) . . . . ? O1 Yb1 N1 C1 103.2(7) . . . . ? Cl1 Yb1 N1 C1 21.4(7) . . . . ? Cl2 Yb1 N1 C1 -165.8(7) 2_767 . . . ? Cl2 Yb1 N1 C1 167.0(6) . . . . ? Yb2 Yb1 N1 C1 6.6(6) . . . . ? Yb1 Yb1 N1 C1 -172.6(6) 2_767 . . . ? N7 Yb2 N2 C9 -133.9(9) . . . . ? N5 Yb2 N2 C9 104.8(9) . . . . ? C1 Yb2 N2 C9 4.4(9) . . . . ? Cl1 Yb2 N2 C9 4.2(16) . . . . ? C2 Yb2 N2 C9 1.5(8) . . . . ? C27 Yb2 N2 C9 93.2(9) . . . . ? Yb1 Yb2 N2 C9 12.4(10) . . . . ? N7 Yb2 N2 C10 44.5(12) . . . . ? N5 Yb2 N2 C10 -76.8(12) . . . . ? C1 Yb2 N2 C10 -177.2(12) . . . . ? Cl1 Yb2 N2 C10 -177.4(9) . . . . ? C2 Yb2 N2 C10 179.9(14) . . . . ? C27 Yb2 N2 C10 -88.4(12) . . . . ? Yb1 Yb2 N2 C10 -169.2(11) . . . . ? C18 C17 N3 C14 177.3(8) . . . . ? C16 C17 N3 C14 3.0(10) . . . . ? C18 C17 N3 Yb1 9.6(13) . . . . ? C16 C17 N3 Yb1 -164.8(6) . . . . ? N1 Yb1 N3 C14 162.3(10) . . . . ? O1 Yb1 N3 C14 9(3) . . . . ? Cl1 Yb1 N3 C14 48.9(10) . . . . ? Cl2 Yb1 N3 C14 -111.6(10) 2_767 . . . ? C1 Yb1 N3 C14 132.9(10) . . . . ? Cl2 Yb1 N3 C14 -34.4(10) . . . . ? Yb2 Yb1 N3 C14 92.5(10) . . . . ? Yb1 Yb1 N3 C14 -72.6(10) 2_767 . . . ? N1 Yb1 N3 C17 -32.1(10) . . . . ? O1 Yb1 N3 C17 174.5(17) . . . . ? Cl1 Yb1 N3 C17 -145.4(9) . . . . ? Cl2 Yb1 N3 C17 54.0(9) 2_767 . . . ? C1 Yb1 N3 C17 -61.5(9) . . . . ? Cl2 Yb1 N3 C17 131.2(9) . . . . ? Yb2 Yb1 N3 C17 -101.8(9) . . . . ? Yb1 Yb1 N3 C17 93.1(9) 2_767 . . . ? N6 Li1 N4 C22 170(5) . . . . ? C16 Li1 N4 C22 -43.4(12) . . . . ? C15 Li1 N4 C22 -17.1(10) . . . . ? C21 Li1 N4 C22 -74.3(11) . . . . ? C35 Li1 N4 C22 55(12) . . . . ? C34 Li1 N4 C22 75.9(12) . . . . ? C29 Li1 N4 C22 51.7(16) . . . . ? C28 Li1 N4 C22 36(3) . . . . ? N6 Li1 N4 C23 28(6) . . . . ? C22 Li1 N4 C23 -142(2) . . . . ? C16 Li1 N4 C23 174.1(17) . . . . ? C15 Li1 N4 C23 -159.6(19) . . . . ? C21 Li1 N4 C23 143.3(17) . . . . ? C35 Li1 N4 C23 -87(12) . . . . ? C34 Li1 N4 C23 -67(2) . . . . ? C29 Li1 N4 C23 -91(2) . . . . ? C28 Li1 N4 C23 -106(3) . . . . ? N7 Yb2 N5 C30 47.3(14) . . . . ? N2 Yb2 N5 C30 154.9(13) . . . . ? C1 Yb2 N5 C30 -129.0(13) . . . . ? Cl1 Yb2 N5 C30 -42.3(13) . . . . ? C2 Yb2 N5 C30 -155.9(13) . . . . ? C27 Yb2 N5 C30 -174.9(19) . . . . ? Yb1 Yb2 N5 C30 -86.0(13) . . . . ? N7 Yb2 N5 C27 -137.7(9) . . . . ? N2 Yb2 N5 C27 -30.2(9) . . . . ? C1 Yb2 N5 C27 45.9(9) . . . . ? Cl1 Yb2 N5 C27 132.7(9) . . . . ? C2 Yb2 N5 C27 19.0(9) . . . . ? Yb1 Yb2 N5 C27 89.0(9) . . . . ? N4 Li1 N6 C35 -165(5) . . . . ? C22 Li1 N6 C35 -21(12) . . . . ? C16 Li1 N6 C35 52.8(19) . . . . ? C15 Li1 N6 C35 25(3) . . . . ? C21 Li1 N6 C35 81.9(14) . . . . ? C34 Li1 N6 C35 -68.6(13) . . . . ? C29 Li1 N6 C35 -39.5(12) . . . . ? C28 Li1 N6 C35 -17.0(11) . . . . ? N4 Li1 N6 C36 46(6) . . . . ? C22 Li1 N6 C36 -170(11) . . . . ? C16 Li1 N6 C36 -96(2) . . . . ? C15 Li1 N6 C36 -123(3) . . . . ? C21 Li1 N6 C36 -66.8(19) . . . . ? C35 Li1 N6 C36 -149(2) . . . . ? C34 Li1 N6 C36 142.7(15) . . . . ? C29 Li1 N6 C36 171.8(15) . . . . ? C28 Li1 N6 C36 -165.7(17) . . . . ? C41 Si1 N7 Si2 72.5(10) . . . . ? C40 Si1 N7 Si2 -166.8(7) . . . . ? C42 Si1 N7 Si2 -53.0(10) . . . . ? C41 Si1 N7 Yb2 -124.0(8) . . . . ? C40 Si1 N7 Yb2 -3.3(8) . . . . ? C42 Si1 N7 Yb2 110.5(8) . . . . ? C45 Si2 N7 Si1 -152.4(8) . . . . ? C44 Si2 N7 Si1 84.7(9) . . . . ? C43 Si2 N7 Si1 -34.0(9) . . . . ? C45 Si2 N7 Yb2 47.2(10) . . . . ? C44 Si2 N7 Yb2 -75.7(10) . . . . ? C43 Si2 N7 Yb2 165.6(7) . . . . ? N5 Yb2 N7 Si1 -176.1(4) . . . . ? N2 Yb2 N7 Si1 82.5(6) . . . . ? C1 Yb2 N7 Si1 -1.6(8) . . . . ? Cl1 Yb2 N7 Si1 -86.0(5) . . . . ? C2 Yb2 N7 Si1 35.7(7) . . . . ? C27 Yb2 N7 Si1 162.6(4) . . . . ? Yb1 Yb2 N7 Si1 -60.6(6) . . . . ? N5 Yb2 N7 Si2 -13.9(8) . . . . ? N2 Yb2 N7 Si2 -115.4(7) . . . . ? C1 Yb2 N7 Si2 160.6(5) . . . . ? Cl1 Yb2 N7 Si2 76.2(6) . . . . ? C2 Yb2 N7 Si2 -162.1(5) . . . . ? C27 Yb2 N7 Si2 -35.3(9) . . . . ? Yb1 Yb2 N7 Si2 101.6(6) . . . . ? N1 Yb1 O1 C46 -163.2(11) . . . . ? N3 Yb1 O1 C46 -9(3) . . . . ? Cl1 Yb1 O1 C46 -49.7(11) . . . . ? Cl2 Yb1 O1 C46 111.4(11) 2_767 . . . ? C1 Yb1 O1 C46 -133.1(11) . . . . ? Cl2 Yb1 O1 C46 34.3(10) . . . . ? Yb2 Yb1 O1 C46 -92.1(11) . . . . ? Yb1 Yb1 O1 C46 72.5(11) 2_767 . . . ? N1 Yb1 O1 C49 27.4(10) . . . . ? N3 Yb1 O1 C49 -178.7(19) . . . . ? Cl1 Yb1 O1 C49 141.0(10) . . . . ? Cl2 Yb1 O1 C49 -57.9(10) 2_767 . . . ? C1 Yb1 O1 C49 57.5(11) . . . . ? Cl2 Yb1 O1 C49 -135.1(10) . . . . ? Yb2 Yb1 O1 C49 98.6(10) . . . . ? Yb1 Yb1 O1 C49 -96.8(10) 2_767 . . . ? C4 N1 C1 C2 -0.7(14) . . . . ? Yb1 N1 C1 C2 171.9(8) . . . . ? C4 N1 C1 Yb2 168.9(12) . . . . ? Yb1 N1 C1 Yb2 -18.5(16) . . . . ? C4 N1 C1 Yb1 -172.6(11) . . . . ? N7 Yb2 C1 N1 -80.5(17) . . . . ? N5 Yb2 C1 N1 94.7(16) . . . . ? N2 Yb2 C1 N1 -175.0(16) . . . . ? Cl1 Yb2 C1 N1 5.0(15) . . . . ? C2 Yb2 C1 N1 -170(2) . . . . ? C27 Yb2 C1 N1 110.8(16) . . . . ? Yb1 Yb2 C1 N1 15.1(13) . . . . ? N7 Yb2 C1 C2 89.6(9) . . . . ? N5 Yb2 C1 C2 -95.3(8) . . . . ? N2 Yb2 C1 C2 -4.9(7) . . . . ? Cl1 Yb2 C1 C2 175.0(7) . . . . ? C27 Yb2 C1 C2 -79.1(8) . . . . ? Yb1 Yb2 C1 C2 -174.9(9) . . . . ? N7 Yb2 C1 Yb1 -95.6(5) . . . . ? N5 Yb2 C1 Yb1 79.6(4) . . . . ? N2 Yb2 C1 Yb1 169.9(4) . . . . ? Cl1 Yb2 C1 Yb1 -10.1(3) . . . . ? C2 Yb2 C1 Yb1 174.9(9) . . . . ? C27 Yb2 C1 Yb1 95.7(4) . . . . ? N3 Yb1 C1 N1 110.3(7) . . . . ? O1 Yb1 C1 N1 -77.0(7) . . . . ? Cl1 Yb1 C1 N1 -160.2(7) . . . . ? Cl2 Yb1 C1 N1 15.7(7) 2_767 . . . ? Cl2 Yb1 C1 N1 -160.0(9) . . . . ? Yb2 Yb1 C1 N1 -170.5(9) . . . . ? Yb1 Yb1 C1 N1 14.3(11) 2_767 . . . ? N1 Yb1 C1 C2 -27(3) . . . . ? N3 Yb1 C1 C2 83(3) . . . . ? O1 Yb1 C1 C2 -104(3) . . . . ? Cl1 Yb1 C1 C2 173(3) . . . . ? Cl2 Yb1 C1 C2 -11(3) 2_767 . . . ? Cl2 Yb1 C1 C2 173(2) . . . . ? Yb2 Yb1 C1 C2 163(3) . . . . ? Yb1 Yb1 C1 C2 -13(3) 2_767 . . . ? N1 Yb1 C1 Yb2 170.5(9) . . . . ? N3 Yb1 C1 Yb2 -79.2(4) . . . . ? O1 Yb1 C1 Yb2 93.4(4) . . . . ? Cl1 Yb1 C1 Yb2 10.2(3) . . . . ? Cl2 Yb1 C1 Yb2 -173.81(18) 2_767 . . . ? Cl2 Yb1 C1 Yb2 10.5(14) . . . . ? Yb1 Yb1 C1 Yb2 -175.2(2) 2_767 . . . ? N1 C1 C2 C9 -179.4(12) . . . . ? Yb2 C1 C2 C9 6.0(15) . . . . ? Yb1 C1 C2 C9 -156(2) . . . . ? N1 C1 C2 C3 1.0(13) . . . . ? Yb2 C1 C2 C3 -173.5(8) . . . . ? Yb1 C1 C2 C3 24(3) . . . . ? N1 C1 C2 Yb2 174.5(12) . . . . ? Yb1 C1 C2 Yb2 -162(3) . . . . ? N7 Yb2 C2 C1 -117.8(8) . . . . ? N5 Yb2 C2 C1 90.1(8) . . . . ? N2 Yb2 C2 C1 173.7(9) . . . . ? Cl1 Yb2 C2 C1 -5.4(8) . . . . ? C27 Yb2 C2 C1 97.5(8) . . . . ? Yb1 Yb2 C2 C1 3.8(7) . . . . ? N7 Yb2 C2 C9 67.2(9) . . . . ? N5 Yb2 C2 C9 -84.8(7) . . . . ? N2 Yb2 C2 C9 -1.3(7) . . . . ? C1 Yb2 C2 C9 -175.0(12) . . . . ? Cl1 Yb2 C2 C9 179.6(6) . . . . ? C27 Yb2 C2 C9 -77.5(7) . . . . ? Yb1 Yb2 C2 C9 -171.2(8) . . . . ? N7 Yb2 C2 C3 -101(2) . . . . ? N5 Yb2 C2 C3 107(2) . . . . ? N2 Yb2 C2 C3 -170(2) . . . . ? C1 Yb2 C2 C3 17(2) . . . . ? Cl1 Yb2 C2 C3 11(2) . . . . ? C27 Yb2 C2 C3 114(2) . . . . ? Yb1 Yb2 C2 C3 20(2) . . . . ? C1 C2 C3 C4 -1.0(14) . . . . ? C9 C2 C3 C4 179.5(13) . . . . ? Yb2 C2 C3 C4 -15(3) . . . . ? C1 C2 C3 C8 -179.5(16) . . . . ? C9 C2 C3 C8 1(3) . . . . ? Yb2 C2 C3 C8 166.8(15) . . . . ? C1 N1 C4 C5 -178.1(15) . . . . ? Yb1 N1 C4 C5 19(3) . . . . ? C1 N1 C4 C3 0.1(14) . . . . ? Yb1 N1 C4 C3 -162.7(15) . . . . ? C2 C3 C4 C5 178.9(14) . . . . ? C8 C3 C4 C5 -2(2) . . . . ? C2 C3 C4 N1 0.5(14) . . . . ? C8 C3 C4 N1 179.5(11) . . . . ? N1 C4 C5 C6 177.9(14) . . . . ? C3 C4 C5 C6 0(2) . . . . ? C4 C5 C6 C7 0(3) . . . . ? C5 C6 C7 C8 2(3) . . . . ? C6 C7 C8 C3 -5(3) . . . . ? C4 C3 C8 C7 5(2) . . . . ? C2 C3 C8 C7 -176.7(17) . . . . ? C10 N2 C9 C2 178.4(13) . . . . ? Yb2 N2 C9 C2 -3.0(17) . . . . ? C1 C2 C9 N2 -3(2) . . . . ? C3 C2 C9 N2 176.7(13) . . . . ? Yb2 C2 C9 N2 2.3(12) . . . . ? C9 N2 C10 C11 -173.1(15) . . . . ? Yb2 N2 C10 C11 9(2) . . . . ? C9 N2 C10 C13 73.7(18) . . . . ? Yb2 N2 C10 C13 -104.6(15) . . . . ? C9 N2 C10 C12 -52.3(19) . . . . ? Yb2 N2 C10 C12 129.5(13) . . . . ? C17 N3 C14 C15 -1.4(13) . . . . ? Yb1 N3 C14 C15 167.1(8) . . . . ? N3 C14 C15 C22 178.4(12) . . . . ? N3 C14 C15 C16 -0.6(14) . . . . ? N3 C14 C15 Li1 79.8(18) . . . . ? C21 C16 C15 C14 -175.5(8) . . . . ? C17 C16 C15 C14 2.3(10) . . . . ? Li1 C16 C15 C14 132.4(12) . . . . ? C21 C16 C15 C22 5.5(18) . . . . ? C17 C16 C15 C22 -176.7(11) . . . . ? Li1 C16 C15 C22 -46.6(14) . . . . ? C21 C16 C15 Li1 52.1(11) . . . . ? C17 C16 C15 Li1 -130.1(9) . . . . ? N4 Li1 C15 C14 140.2(16) . . . . ? N6 Li1 C15 C14 -45(4) . . . . ? C22 Li1 C15 C14 123.6(18) . . . . ? C16 Li1 C15 C14 -94.5(16) . . . . ? C21 Li1 C15 C14 -114.6(16) . . . . ? C35 Li1 C15 C14 -32(2) . . . . ? C34 Li1 C15 C14 45.9(18) . . . . ? C29 Li1 C15 C14 17.8(18) . . . . ? C28 Li1 C15 C14 -10(2) . . . . ? N4 Li1 C15 C22 16.6(10) . . . . ? N6 Li1 C15 C22 -168(3) . . . . ? C16 Li1 C15 C22 141.9(13) . . . . ? C21 Li1 C15 C22 121.8(11) . . . . ? C35 Li1 C15 C22 -155.3(17) . . . . ? C34 Li1 C15 C22 -77.7(11) . . . . ? C29 Li1 C15 C22 -105.8(11) . . . . ? C28 Li1 C15 C22 -133.9(13) . . . . ? N4 Li1 C15 C16 -125.3(12) . . . . ? N6 Li1 C15 C16 50(3) . . . . ? C22 Li1 C15 C16 -141.9(13) . . . . ? C21 Li1 C15 C16 -20.0(5) . . . . ? C35 Li1 C15 C16 62.8(13) . . . . ? C34 Li1 C15 C16 140.5(10) . . . . ? C29 Li1 C15 C16 112.4(9) . . . . ? C28 Li1 C15 C16 84.3(9) . . . . ? C23 N4 C22 C15 -177.3(15) . . . . ? Li1 N4 C22 C15 34.0(18) . . . . ? C23 N4 C22 Li1 149(2) . . . . ? C14 C15 C22 N4 -158.3(13) . . . . ? C16 C15 C22 N4 20(2) . . . . ? Li1 C15 C22 N4 -27.1(15) . . . . ? C14 C15 C22 Li1 -131.2(16) . . . . ? C16 C15 C22 Li1 47.5(14) . . . . ? N6 Li1 C22 N4 -153(12) . . . . ? C16 Li1 C22 N4 129.0(14) . . . . ? C15 Li1 C22 N4 151.3(17) . . . . ? C21 Li1 C22 N4 102.7(14) . . . . ? C35 Li1 C22 N4 -169(3) . . . . ? C34 Li1 C22 N4 -105.3(13) . . . . ? C29 Li1 C22 N4 -134.8(16) . . . . ? C28 Li1 C22 N4 -156.5(19) . . . . ? N4 Li1 C22 C15 -151.3(17) . . . . ? N6 Li1 C22 C15 56(12) . . . . ? C16 Li1 C22 C15 -22.3(8) . . . . ? C21 Li1 C22 C15 -48.6(9) . . . . ? C35 Li1 C22 C15 39(3) . . . . ? C34 Li1 C22 C15 103.4(11) . . . . ? C29 Li1 C22 C15 74.0(11) . . . . ? C28 Li1 C22 C15 52.3(14) . . . . ? C22 N4 C23 C26 -138.3(19) . . . . ? Li1 N4 C23 C26 -3(3) . . . . ? C22 N4 C23 C25 97(2) . . . . ? Li1 N4 C23 C25 -128(2) . . . . ? C22 N4 C23 C24 -13(3) . . . . ? Li1 N4 C23 C24 123(2) . . . . ? C30 N5 C27 C28 -0.8(15) . . . . ? Yb2 N5 C27 C28 -177.3(8) . . . . ? C30 N5 C27 Yb2 176.5(13) . . . . ? N7 Yb2 C27 N5 55.3(10) . . . . ? N2 Yb2 C27 N5 148.4(10) . . . . ? C1 Yb2 C27 N5 -134.9(9) . . . . ? Cl1 Yb2 C27 N5 -49.7(9) . . . . ? C2 Yb2 C27 N5 -161.2(9) . . . . ? Yb1 Yb2 C27 N5 -91.2(9) . . . . ? N7 Yb2 C27 C28 61(2) . . . . ? N5 Yb2 C27 C28 5.3(16) . . . . ? N2 Yb2 C27 C28 154(2) . . . . ? C1 Yb2 C27 C28 -129.6(19) . . . . ? Cl1 Yb2 C27 C28 -44.4(19) . . . . ? C2 Yb2 C27 C28 -155.8(19) . . . . ? Yb1 Yb2 C27 C28 -85.8(19) . . . . ? N5 C27 C28 C29 -0.1(15) . . . . ? Yb2 C27 C28 C29 -4(2) . . . . ? N5 C27 C28 C35 177.2(12) . . . . ? Yb2 C27 C28 C35 173.5(13) . . . . ? N5 C27 C28 Li1 82.7(19) . . . . ? Yb2 C27 C28 Li1 79(3) . . . . ? N4 Li1 C28 C29 29(3) . . . . ? N6 Li1 C28 C29 -129.9(12) . . . . ? C22 Li1 C28 C29 49.4(14) . . . . ? C16 Li1 C28 C29 107.2(10) . . . . ? C15 Li1 C28 C29 74.8(11) . . . . ? C21 Li1 C28 C29 135.0(11) . . . . ? C35 Li1 C28 C29 -145.8(14) . . . . ? C34 Li1 C28 C29 -20.2(8) . . . . ? N4 Li1 C28 C27 -67(3) . . . . ? N6 Li1 C28 C27 133.9(17) . . . . ? C22 Li1 C28 C27 -47(2) . . . . ? C16 Li1 C28 C27 11.0(19) . . . . ? C15 Li1 C28 C27 -21(2) . . . . ? C21 Li1 C28 C27 39(2) . . . . ? C35 Li1 C28 C27 118(2) . . . . ? C34 Li1 C28 C27 -116.4(17) . . . . ? C29 Li1 C28 C27 -96.2(17) . . . . ? N4 Li1 C28 C35 175(3) . . . . ? N6 Li1 C28 C35 15.9(10) . . . . ? C22 Li1 C28 C35 -164.8(16) . . . . ? C16 Li1 C28 C35 -107.0(12) . . . . ? C15 Li1 C28 C35 -139.4(13) . . . . ? C21 Li1 C28 C35 -79.2(12) . . . . ? C34 Li1 C28 C35 125.6(12) . . . . ? C29 Li1 C28 C35 145.8(14) . . . . ? C27 C28 C29 C34 -175.5(15) . . . . ? C35 C28 C29 C34 7(3) . . . . ? Li1 C28 C29 C34 50.5(17) . . . . ? C27 C28 C29 C30 0.8(14) . . . . ? C35 C28 C29 C30 -176.2(13) . . . . ? Li1 C28 C29 C30 -133.1(11) . . . . ? C27 C28 C29 Li1 134.0(11) . . . . ? C35 C28 C29 Li1 -43.1(15) . . . . ? N4 Li1 C29 C28 -160.6(16) . . . . ? N6 Li1 C29 C28 41.2(10) . . . . ? C22 Li1 C29 C28 -136.1(12) . . . . ? C16 Li1 C29 C28 -74.4(10) . . . . ? C15 Li1 C29 C28 -104.6(10) . . . . ? C21 Li1 C29 C28 -54.7(12) . . . . ? C35 Li1 C29 C28 20.0(8) . . . . ? C34 Li1 C29 C28 145.0(14) . . . . ? N4 Li1 C29 C34 54.4(16) . . . . ? N6 Li1 C29 C34 -103.8(13) . . . . ? C22 Li1 C29 C34 78.8(12) . . . . ? C16 Li1 C29 C34 140.6(12) . . . . ? C15 Li1 C29 C34 110.3(11) . . . . ? C21 Li1 C29 C34 160.2(14) . . . . ? C35 Li1 C29 C34 -125.0(12) . . . . ? C28 Li1 C29 C34 -145.0(14) . . . . ? N4 Li1 C29 C30 -62(2) . . . . ? N6 Li1 C29 C30 140.1(14) . . . . ? C22 Li1 C29 C30 -37.2(18) . . . . ? C16 Li1 C29 C30 24.5(17) . . . . ? C15 Li1 C29 C30 -5.7(17) . . . . ? C21 Li1 C29 C30 44.2(19) . . . . ? C35 Li1 C29 C30 118.9(14) . . . . ? C34 Li1 C29 C30 -116.1(18) . . . . ? C28 Li1 C29 C30 98.9(16) . . . . ? C27 N5 C30 C31 -176.6(14) . . . . ? Yb2 N5 C30 C31 -1(2) . . . . ? C27 N5 C30 C29 1.3(14) . . . . ? Yb2 N5 C30 C29 176.7(9) . . . . ? C28 C29 C30 N5 -1.4(15) . . . . ? C34 C29 C30 N5 175.6(12) . . . . ? Li1 C29 C30 N5 -88.4(16) . . . . ? C28 C29 C30 C31 176.7(13) . . . . ? C34 C29 C30 C31 -6(2) . . . . ? Li1 C29 C30 C31 89.7(19) . . . . ? N5 C30 C31 C32 -179.7(14) . . . . ? C29 C30 C31 C32 3(2) . . . . ? C30 C31 C32 C33 2(3) . . . . ? C31 C32 C33 C34 -2(3) . . . . ? C32 C33 C34 C29 -2(3) . . . . ? C32 C33 C34 Li1 -99(2) . . . . ? C28 C29 C34 C33 -178.1(16) . . . . ? C30 C29 C34 C33 6(2) . . . . ? Li1 C29 C34 C33 -126.3(17) . . . . ? C28 C29 C34 Li1 -51.8(17) . . . . ? C30 C29 C34 Li1 132.3(12) . . . . ? N4 Li1 C34 C33 -14(2) . . . . ? N6 Li1 C34 C33 -169.7(17) . . . . ? C22 Li1 C34 C33 17(2) . . . . ? C16 Li1 C34 C33 72(2) . . . . ? C15 Li1 C34 C33 48.6(19) . . . . ? C21 Li1 C34 C33 84(3) . . . . ? C35 Li1 C34 C33 163.2(17) . . . . ? C29 Li1 C34 C33 118(2) . . . . ? C28 Li1 C34 C33 138.0(18) . . . . ? N4 Li1 C34 C29 -132.4(14) . . . . ? N6 Li1 C34 C29 71.9(12) . . . . ? C22 Li1 C34 C29 -101.7(12) . . . . ? C16 Li1 C34 C29 -46.5(13) . . . . ? C15 Li1 C34 C29 -69.8(11) . . . . ? C21 Li1 C34 C29 -34(2) . . . . ? C35 Li1 C34 C29 44.8(10) . . . . ? C28 Li1 C34 C29 19.6(8) . . . . ? C36 N6 C35 C28 -172.5(13) . . . . ? Li1 N6 C35 C28 34(2) . . . . ? C36 N6 C35 Li1 153.6(19) . . . . ? C29 C28 C35 N6 20(2) . . . . ? C27 C28 C35 N6 -156.6(14) . . . . ? Li1 C28 C35 N6 -24.6(14) . . . . ? C29 C28 C35 Li1 44.6(16) . . . . ? C27 C28 C35 Li1 -132.0(14) . . . . ? N4 Li1 C35 N6 128(13) . . . . ? C22 Li1 C35 N6 175(3) . . . . ? C16 Li1 C35 N6 -134.0(18) . . . . ? C15 Li1 C35 N6 -163(2) . . . . ? C21 Li1 C35 N6 -102.6(16) . . . . ? C34 Li1 C35 N6 107.2(15) . . . . ? C29 Li1 C35 N6 132.1(15) . . . . ? C28 Li1 C35 N6 151.2(18) . . . . ? N4 Li1 C35 C28 -23(12) . . . . ? N6 Li1 C35 C28 -151.2(18) . . . . ? C22 Li1 C35 C28 24(3) . . . . ? C16 Li1 C35 C28 74.8(12) . . . . ? C15 Li1 C35 C28 45.9(15) . . . . ? C21 Li1 C35 C28 106.2(11) . . . . ? C34 Li1 C35 C28 -44.0(10) . . . . ? C29 Li1 C35 C28 -19.1(8) . . . . ? C35 N6 C36 C37 -31(2) . . . . ? Li1 N6 C36 C37 115(2) . . . . ? C35 N6 C36 C38 -148.8(17) . . . . ? Li1 N6 C36 C38 -4(2) . . . . ? C35 N6 C36 C39 91.8(17) . . . . ? Li1 N6 C36 C39 -122.9(18) . . . . ? C49 O1 C46 C47 -23.4(17) . . . . ? Yb1 O1 C46 C47 166.1(9) . . . . ? O1 C46 C47 C48 22.1(19) . . . . ? C46 C47 C48 C49 -13(2) . . . . ? C46 O1 C49 C48 15.2(17) . . . . ? Yb1 O1 C49 C48 -173.9(10) . . . . ? C47 C48 C49 O1 -0.9(19) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.779 _refine_diff_density_min -1.007 _refine_diff_density_rms 0.207 # Attachment '- 101217a_0m.cif' data_101217a_0m _database_code_depnum_ccdc_archive 'CCDC 842359' #TrackingRef '- 101217a_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H70 Cl2 Li N7 O Si2 Y2' _chemical_formula_weight 1084.96 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.0187(13) _cell_length_b 16.0047(14) _cell_length_c 16.6926(14) _cell_angle_alpha 84.1590(10) _cell_angle_beta 64.9450(10) _cell_angle_gamma 78.9000(10) _cell_volume 3565.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5921 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 22.84 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6676 _exptl_absorpt_correction_T_max 0.7542 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31129 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.1229 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.54 _reflns_number_total 16071 _reflns_number_gt 7134 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1983P)^2^+0.6645P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16071 _refine_ls_number_parameters 592 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1914 _refine_ls_R_factor_gt 0.0888 _refine_ls_wR_factor_ref 0.3462 _refine_ls_wR_factor_gt 0.2847 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.003 _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 0.86346(6) 0.58631(5) 1.04835(5) 0.0511(3) Uani 1 1 d . . . Y2 Y 0.66451(6) 0.78597(5) 1.12665(5) 0.0523(3) Uani 1 1 d . . . Cl1 Cl 0.85165(16) 0.73687(14) 1.11009(16) 0.0653(6) Uani 1 1 d . . . Cl2 Cl 1.06108(15) 0.57156(13) 1.01409(15) 0.0630(6) Uani 1 1 d . . . Si1 Si 0.6011(2) 0.8047(2) 1.33534(18) 0.0814(9) Uani 1 1 d . . . Si2 Si 0.6706(2) 0.9622(2) 1.2353(2) 0.0833(9) Uani 1 1 d . . . Li1 Li 0.8976(14) 0.8138(12) 0.6934(13) 0.091(5) Uani 1 1 d . . . N1 N 0.7167(5) 0.5496(4) 1.0815(5) 0.0595(18) Uani 1 1 d . . . N2 N 0.5041(5) 0.7821(5) 1.1321(5) 0.0641(19) Uani 1 1 d . . . N3 N 0.8967(5) 0.6480(4) 0.9072(5) 0.0591(18) Uani 1 1 d . . . N4 N 1.0468(5) 0.7986(5) 0.6467(5) 0.074(2) Uani 1 1 d . . . N5 N 0.7224(6) 0.8437(5) 0.9852(5) 0.0657(19) Uani 1 1 d . . . N6 N 0.7638(6) 0.8529(5) 0.6928(5) 0.078(2) Uani 1 1 d . . . N7 N 0.6350(5) 0.8663(5) 1.2402(5) 0.068(2) Uani 1 1 d . . . O1 O 0.8459(5) 0.5369(4) 1.1912(4) 0.0722(17) Uani 1 1 d . . . C1 C 0.6679(6) 0.6321(5) 1.0962(5) 0.0501(19) Uani 1 1 d . . . C2 C 0.5695(6) 0.6325(5) 1.1088(5) 0.0533(19) Uani 1 1 d . . . C3 C 0.5576(6) 0.5477(6) 1.1038(5) 0.062(2) Uani 1 1 d . . . C4 C 0.6512(7) 0.4973(6) 1.0851(6) 0.063(2) Uani 1 1 d . . . C5 C 0.6680(9) 0.4111(7) 1.0766(8) 0.094(3) Uani 1 1 d . . . H5 H 0.7297 0.3783 1.0674 0.113 Uiso 1 1 calc R . . C6 C 0.5873(10) 0.3739(8) 1.0824(9) 0.106(4) Uani 1 1 d . . . H6 H 0.5970 0.3159 1.0735 0.127 Uiso 1 1 calc R . . C7 C 0.4949(9) 0.4219(7) 1.1008(8) 0.093(3) Uani 1 1 d . . . H7 H 0.4424 0.3952 1.1072 0.111 Uiso 1 1 calc R . . C8 C 0.4794(8) 0.5052(7) 1.1096(7) 0.081(3) Uani 1 1 d . . . H8 H 0.4169 0.5367 1.1196 0.098 Uiso 1 1 calc R . . C9 C 0.4923(6) 0.7046(6) 1.1249(5) 0.061(2) Uani 1 1 d . . . H9 H 0.4303 0.6962 1.1306 0.073 Uiso 1 1 calc R . . C10 C 0.4177(7) 0.8552(7) 1.1449(7) 0.079(3) Uani 1 1 d . . . C11 C 0.4566(9) 0.9356(7) 1.1377(10) 0.117(5) Uani 1 1 d . . . H11A H 0.4915 0.9314 1.1750 0.175 Uiso 1 1 calc R . . H11B H 0.4020 0.9823 1.1561 0.175 Uiso 1 1 calc R . . H11C H 0.5012 0.9451 1.0775 0.175 Uiso 1 1 calc R . . C12 C 0.3838(12) 0.8585(9) 1.0726(10) 0.140(6) Uani 1 1 d . . . H12A H 0.4369 0.8696 1.0172 0.209 Uiso 1 1 calc R . . H12B H 0.3274 0.9030 1.0836 0.209 Uiso 1 1 calc R . . H12C H 0.3652 0.8049 1.0705 0.209 Uiso 1 1 calc R . . C13 C 0.3313(10) 0.8418(9) 1.2384(9) 0.134(5) Uani 1 1 d . . . H13A H 0.3017 0.7943 1.2367 0.201 Uiso 1 1 calc R . . H13B H 0.2816 0.8922 1.2533 0.201 Uiso 1 1 calc R . . H13C H 0.3580 0.8307 1.2822 0.201 Uiso 1 1 calc R . . C14 C 0.9651(7) 0.7013(6) 0.8674(6) 0.069(2) Uani 1 1 d . . . H14 H 0.9942 0.7252 0.8968 0.083 Uiso 1 1 calc R . . C15 C 0.9865(6) 0.7159(6) 0.7771(6) 0.062(2) Uani 1 1 d . . . C16 C 0.9263(6) 0.6665(5) 0.7625(6) 0.061(2) Uani 1 1 d . . . C17 C 0.8722(6) 0.6282(5) 0.8434(5) 0.0522(19) Uani 1 1 d . . . C18 C 0.8071(8) 0.5731(7) 0.8500(7) 0.086(3) Uani 1 1 d . . . H18 H 0.7716 0.5465 0.9033 0.103 Uiso 1 1 calc R . . C19 C 0.7986(10) 0.5604(9) 0.7727(9) 0.112(4) Uani 1 1 d . . . H19 H 0.7548 0.5252 0.7755 0.134 Uiso 1 1 calc R . . C20 C 0.8508(10) 0.5966(9) 0.6929(8) 0.108(4) Uani 1 1 d . . . H20 H 0.8422 0.5856 0.6432 0.130 Uiso 1 1 calc R . . C21 C 0.9159(9) 0.6495(7) 0.6857(7) 0.086(3) Uani 1 1 d . . . H21 H 0.9526 0.6736 0.6313 0.104 Uiso 1 1 calc R . . C22 C 1.0554(7) 0.7680(6) 0.7176(7) 0.071(3) Uani 1 1 d . . . H22 H 1.1063 0.7797 0.7303 0.086 Uiso 1 1 calc R . . C23 C 1.1240(9) 0.8465(8) 0.5805(8) 0.102(3) Uani 1 1 d U . . C24 C 1.1828(11) 0.8849(10) 0.6122(10) 0.135(4) Uani 1 1 d U . . H24A H 1.1392 0.9223 0.6597 0.203 Uiso 1 1 calc R . . H24B H 1.2264 0.9167 0.5648 0.203 Uiso 1 1 calc R . . H24C H 1.2217 0.8410 0.6331 0.203 Uiso 1 1 calc R . . C25 C 1.1937(12) 0.7826(11) 0.5111(10) 0.161(5) Uani 1 1 d U . . H25A H 1.2002 0.7275 0.5388 0.241 Uiso 1 1 calc R . . H25B H 1.2580 0.7999 0.4821 0.241 Uiso 1 1 calc R . . H25C H 1.1673 0.7798 0.4684 0.241 Uiso 1 1 calc R . . C26 C 1.0694(11) 0.9137(10) 0.5414(11) 0.156(5) Uani 1 1 d U . . H26A H 1.0351 0.8876 0.5161 0.235 Uiso 1 1 calc R . . H26B H 1.1160 0.9450 0.4961 0.235 Uiso 1 1 calc R . . H26C H 1.0221 0.9519 0.5867 0.235 Uiso 1 1 calc R . . C27 C 0.6830(7) 0.8243(6) 0.9307(6) 0.065(2) Uani 1 1 d . . . H27 H 0.6319 0.7924 0.9489 0.078 Uiso 1 1 calc R . . C28 C 0.7271(7) 0.8571(6) 0.8450(6) 0.065(2) Uani 1 1 d . . . C29 C 0.7996(7) 0.9019(5) 0.8474(6) 0.059(2) Uani 1 1 d . . . C30 C 0.7949(7) 0.8895(6) 0.9331(6) 0.062(2) Uani 1 1 d . . . C31 C 0.8579(9) 0.9218(7) 0.9554(8) 0.092(3) Uani 1 1 d . . . H31 H 0.8568 0.9123 1.0117 0.110 Uiso 1 1 calc R . . C32 C 0.9239(10) 0.9694(8) 0.8926(10) 0.113(4) Uani 1 1 d . . . H32 H 0.9678 0.9913 0.9074 0.135 Uiso 1 1 calc R . . C33 C 0.9271(10) 0.9863(8) 0.8063(9) 0.103(4) Uani 1 1 d . . . H33 H 0.9695 1.0210 0.7659 0.124 Uiso 1 1 calc R . . C34 C 0.8675(9) 0.9507(6) 0.7860(7) 0.087(3) Uani 1 1 d . . . H34 H 0.8707 0.9582 0.7289 0.104 Uiso 1 1 calc R . . C35 C 0.7037(8) 0.8458(7) 0.7720(6) 0.075(3) Uani 1 1 d . . . H35 H 0.6415 0.8326 0.7840 0.090 Uiso 1 1 calc R . . C36 C 0.7330(9) 0.8472(10) 0.6199(7) 0.106(3) Uani 1 1 d U . . C37 C 0.6554(12) 0.7945(11) 0.6455(9) 0.144(5) Uani 1 1 d U . . H37A H 0.6685 0.7468 0.6811 0.217 Uiso 1 1 calc R . . H37B H 0.6552 0.7743 0.5934 0.217 Uiso 1 1 calc R . . H37C H 0.5917 0.8277 0.6789 0.217 Uiso 1 1 calc R . . C38 C 0.8295(11) 0.8126(11) 0.5419(8) 0.149(5) Uani 1 1 d U . . H38A H 0.8352 0.8470 0.4899 0.223 Uiso 1 1 calc R . . H38B H 0.8285 0.7550 0.5317 0.223 Uiso 1 1 calc R . . H38C H 0.8854 0.8143 0.5551 0.223 Uiso 1 1 calc R . . C39 C 0.6930(11) 0.9370(10) 0.6000(9) 0.141(4) Uani 1 1 d U . . H39A H 0.6449 0.9634 0.6539 0.212 Uiso 1 1 calc R . . H39B H 0.6619 0.9358 0.5604 0.212 Uiso 1 1 calc R . . H39C H 0.7469 0.9689 0.5728 0.212 Uiso 1 1 calc R . . C40 C 0.5910(10) 0.6986(7) 1.3074(7) 0.101(4) Uani 1 1 d . . . H40A H 0.5389 0.7047 1.2873 0.151 Uiso 1 1 calc R . . H40B H 0.5757 0.6619 1.3590 0.151 Uiso 1 1 calc R . . H40C H 0.6530 0.6745 1.2616 0.151 Uiso 1 1 calc R . . C41 C 0.4741(10) 0.8464(9) 1.4244(8) 0.132(5) Uani 1 1 d . . . H41A H 0.4770 0.8980 1.4473 0.197 Uiso 1 1 calc R . . H41B H 0.4554 0.8046 1.4714 0.197 Uiso 1 1 calc R . . H41C H 0.4257 0.8578 1.3996 0.197 Uiso 1 1 calc R . . C42 C 0.6935(10) 0.7843(9) 1.3839(8) 0.120(5) Uani 1 1 d . . . H42A H 0.7356 0.7305 1.3644 0.180 Uiso 1 1 calc R . . H42B H 0.6595 0.7831 1.4473 0.180 Uiso 1 1 calc R . . H42C H 0.7334 0.8287 1.3653 0.180 Uiso 1 1 calc R . . C43 C 0.6041(10) 1.0231(8) 1.3416(8) 0.123(5) Uani 1 1 d . . . H43A H 0.5334 1.0290 1.3603 0.184 Uiso 1 1 calc R . . H43B H 0.6229 1.0786 1.3320 0.184 Uiso 1 1 calc R . . H43C H 0.6222 0.9928 1.3866 0.184 Uiso 1 1 calc R . . C44 C 0.8059(8) 0.9496(8) 1.2115(9) 0.114(4) Uani 1 1 d . . . H44A H 0.8155 0.9284 1.2636 0.171 Uiso 1 1 calc R . . H44B H 0.8277 1.0038 1.1940 0.171 Uiso 1 1 calc R . . H44C H 0.8438 0.9101 1.1646 0.171 Uiso 1 1 calc R . . C45 C 0.6409(11) 1.0311(7) 1.1508(9) 0.120(4) Uani 1 1 d . . . H45A H 0.6671 1.0008 1.0967 0.180 Uiso 1 1 calc R . . H45B H 0.6704 1.0815 1.1405 0.180 Uiso 1 1 calc R . . H45C H 0.5699 1.0468 1.1714 0.180 Uiso 1 1 calc R . . C46 C 0.9002(9) 0.5541(9) 1.2400(8) 0.102(4) Uani 1 1 d . . . H46A H 0.9682 0.5237 1.2148 0.122 Uiso 1 1 calc R . . H46B H 0.9020 0.6145 1.2379 0.122 Uiso 1 1 calc R . . C47 C 0.8482(12) 0.5252(11) 1.3305(8) 0.125(5) Uani 1 1 d . . . H47A H 0.8065 0.5731 1.3672 0.150 Uiso 1 1 calc R . . H47B H 0.8956 0.4976 1.3543 0.150 Uiso 1 1 calc R . . C48 C 0.7860(13) 0.4639(10) 1.3288(8) 0.134(5) Uani 1 1 d . . . H48A H 0.7179 0.4786 1.3723 0.160 Uiso 1 1 calc R . . H48B H 0.8124 0.4065 1.3419 0.160 Uiso 1 1 calc R . . C49 C 0.7892(10) 0.4696(8) 1.2376(8) 0.106(4) Uani 1 1 d . . . H49A H 0.8213 0.4159 1.2078 0.127 Uiso 1 1 calc R . . H49B H 0.7223 0.4832 1.2400 0.127 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 0.0409(4) 0.0549(5) 0.0538(5) -0.0074(4) -0.0156(4) -0.0058(3) Y2 0.0462(5) 0.0600(5) 0.0516(5) -0.0104(4) -0.0212(4) -0.0041(4) Cl1 0.0525(12) 0.0661(13) 0.0840(15) -0.0214(11) -0.0330(12) -0.0031(10) Cl2 0.0452(11) 0.0602(13) 0.0839(15) -0.0167(11) -0.0244(11) -0.0072(9) Si1 0.0759(19) 0.111(2) 0.0549(15) -0.0218(15) -0.0276(14) 0.0017(17) Si2 0.0700(18) 0.087(2) 0.098(2) -0.0366(17) -0.0348(17) -0.0065(15) Li1 0.077(12) 0.094(13) 0.095(13) 0.012(10) -0.031(10) -0.018(10) N1 0.051(4) 0.055(4) 0.068(5) -0.007(3) -0.017(4) -0.014(3) N2 0.047(4) 0.079(5) 0.059(4) -0.005(4) -0.019(3) -0.001(4) N3 0.058(4) 0.060(4) 0.060(4) 0.004(3) -0.024(4) -0.013(4) N4 0.054(5) 0.082(5) 0.079(5) 0.008(4) -0.021(4) -0.014(4) N5 0.068(5) 0.071(5) 0.063(5) -0.002(4) -0.031(4) -0.013(4) N6 0.073(5) 0.095(6) 0.066(5) -0.002(4) -0.032(5) -0.008(5) N7 0.054(4) 0.084(5) 0.064(5) -0.028(4) -0.025(4) 0.007(4) O1 0.066(4) 0.082(4) 0.063(4) 0.007(3) -0.023(3) -0.016(3) C1 0.047(5) 0.053(5) 0.049(4) -0.007(4) -0.016(4) -0.010(4) C2 0.043(5) 0.061(5) 0.055(5) -0.008(4) -0.019(4) -0.008(4) C3 0.054(5) 0.076(6) 0.058(5) -0.004(4) -0.024(4) -0.012(5) C4 0.061(6) 0.067(6) 0.060(5) -0.013(4) -0.019(4) -0.014(5) C5 0.082(8) 0.074(7) 0.114(9) -0.027(6) -0.024(7) -0.016(6) C6 0.090(9) 0.079(8) 0.148(12) -0.012(7) -0.036(8) -0.037(7) C7 0.088(8) 0.075(7) 0.126(10) -0.005(7) -0.043(7) -0.039(7) C8 0.062(6) 0.086(7) 0.097(8) -0.006(6) -0.027(6) -0.025(5) C9 0.038(4) 0.080(6) 0.064(5) -0.002(5) -0.019(4) -0.013(4) C10 0.051(6) 0.085(7) 0.103(8) -0.020(6) -0.041(6) 0.016(5) C11 0.086(8) 0.070(7) 0.201(15) -0.015(8) -0.071(10) 0.005(6) C12 0.158(14) 0.119(11) 0.188(15) -0.028(10) -0.133(13) 0.031(9) C13 0.093(10) 0.138(12) 0.116(11) -0.025(9) -0.008(8) 0.038(8) C14 0.066(6) 0.068(6) 0.078(6) 0.009(5) -0.034(5) -0.017(5) C15 0.055(5) 0.068(6) 0.066(6) 0.001(5) -0.029(5) -0.003(4) C16 0.057(5) 0.062(5) 0.067(6) -0.005(4) -0.031(5) -0.002(4) C17 0.047(5) 0.053(5) 0.055(5) -0.006(4) -0.021(4) -0.003(4) C18 0.081(7) 0.093(8) 0.087(7) -0.001(6) -0.032(6) -0.029(6) C19 0.125(11) 0.133(11) 0.116(10) -0.002(8) -0.069(9) -0.063(9) C20 0.134(11) 0.142(11) 0.075(8) 0.002(7) -0.050(8) -0.068(9) C21 0.105(9) 0.084(7) 0.074(7) 0.002(5) -0.040(6) -0.022(6) C22 0.055(6) 0.074(6) 0.081(7) 0.012(5) -0.025(5) -0.015(5) C23 0.089(7) 0.119(8) 0.096(7) 0.030(5) -0.033(5) -0.038(6) C24 0.125(10) 0.149(11) 0.140(10) 0.017(8) -0.046(8) -0.074(8) C25 0.151(12) 0.177(11) 0.105(10) -0.018(8) 0.007(8) -0.048(8) C26 0.128(10) 0.170(11) 0.158(11) 0.095(9) -0.056(8) -0.055(8) C27 0.054(5) 0.070(6) 0.065(6) -0.005(5) -0.018(5) -0.007(4) C28 0.056(5) 0.073(6) 0.058(5) -0.006(5) -0.021(4) 0.005(5) C29 0.057(5) 0.046(5) 0.066(6) -0.004(4) -0.020(4) -0.002(4) C30 0.059(6) 0.062(5) 0.063(6) -0.015(4) -0.021(5) -0.006(4) C31 0.084(8) 0.104(8) 0.090(8) -0.010(7) -0.037(7) -0.017(7) C32 0.094(9) 0.101(9) 0.142(13) -0.035(9) -0.033(9) -0.035(7) C33 0.109(10) 0.088(8) 0.100(9) -0.005(7) -0.016(8) -0.049(7) C34 0.106(9) 0.064(6) 0.073(7) 0.001(5) -0.019(6) -0.018(6) C35 0.063(6) 0.100(8) 0.062(6) -0.004(5) -0.028(5) -0.005(5) C36 0.089(7) 0.176(9) 0.066(6) 0.011(6) -0.048(5) -0.023(6) C37 0.145(10) 0.218(12) 0.105(9) -0.002(9) -0.070(8) -0.066(9) C38 0.124(9) 0.255(14) 0.063(7) -0.023(8) -0.046(6) 0.003(9) C39 0.126(10) 0.194(10) 0.109(9) 0.037(8) -0.069(8) -0.012(8) C40 0.130(11) 0.101(8) 0.064(7) 0.006(6) -0.028(7) -0.031(8) C41 0.114(11) 0.145(12) 0.083(8) -0.015(8) -0.005(8) 0.018(9) C42 0.142(12) 0.153(12) 0.101(9) -0.008(8) -0.089(9) -0.011(9) C43 0.133(12) 0.118(10) 0.120(10) -0.064(8) -0.051(9) -0.002(9) C44 0.075(8) 0.136(11) 0.143(11) -0.048(9) -0.041(8) -0.027(7) C45 0.133(12) 0.084(8) 0.144(12) -0.012(8) -0.057(10) -0.019(8) C46 0.093(9) 0.132(10) 0.096(9) 0.002(7) -0.054(7) -0.021(7) C47 0.147(13) 0.160(14) 0.065(8) 0.007(8) -0.054(8) -0.001(11) C48 0.155(14) 0.135(12) 0.079(9) 0.015(8) -0.017(9) -0.034(11) C49 0.120(10) 0.101(9) 0.080(8) 0.016(7) -0.029(7) -0.021(8) _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 2.216(7) . ? Y1 N3 2.344(7) . ? Y1 O1 2.354(6) . ? Y1 Cl1 2.662(2) . ? Y1 C1 2.665(8) . ? Y1 Cl2 2.681(2) 2_767 ? Y1 Cl2 2.741(2) . ? Y2 N7 2.238(7) . ? Y2 N5 2.305(7) . ? Y2 N2 2.385(7) . ? Y2 C1 2.551(8) . ? Y2 Cl1 2.670(2) . ? Y2 Si1 3.229(3) . ? Cl2 Y1 2.681(2) 2_767 ? Si1 N7 1.715(8) . ? Si1 C42 1.848(11) . ? Si1 C40 1.855(11) . ? Si1 C41 1.898(12) . ? Si2 N7 1.703(8) . ? Si2 C45 1.853(13) . ? Si2 C44 1.871(11) . ? Si2 C43 1.890(11) . ? Li1 N6 1.99(2) . ? Li1 N4 2.01(2) . ? Li1 C22 2.53(2) . ? Li1 C15 2.55(2) . ? Li1 C16 2.56(2) . ? Li1 C21 2.60(2) . ? Li1 C35 2.61(2) . ? Li1 C34 2.67(2) . ? Li1 C29 2.74(2) . ? Li1 C28 2.76(2) . ? N1 C1 1.371(10) . ? N1 C4 1.389(10) . ? N2 C9 1.310(11) . ? N2 C10 1.526(11) . ? N3 C17 1.347(10) . ? N3 C14 1.366(11) . ? N4 C22 1.282(11) . ? N4 C23 1.496(13) . ? N5 C30 1.361(11) . ? N5 C27 1.364(11) . ? N6 C35 1.255(11) . ? N6 C36 1.490(12) . ? O1 C46 1.449(12) . ? O1 C49 1.454(13) . ? C1 C2 1.401(11) . ? C2 C3 1.418(12) . ? C2 C9 1.427(11) . ? C3 C4 1.403(12) . ? C3 C8 1.430(12) . ? C4 C5 1.365(13) . ? C5 C6 1.414(14) . ? C5 H5 0.9300 . ? C6 C7 1.372(15) . ? C6 H6 0.9300 . ? C7 C8 1.322(13) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.486(14) . ? C10 C12 1.489(15) . ? C10 C13 1.578(16) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.406(12) . ? C14 H14 0.9300 . ? C15 C16 1.415(12) . ? C15 C22 1.431(12) . ? C16 C17 1.397(12) . ? C16 C21 1.414(13) . ? C17 C18 1.403(13) . ? C18 C19 1.387(15) . ? C18 H18 0.9300 . ? C19 C20 1.363(16) . ? C19 H19 0.9300 . ? C20 C21 1.373(15) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.452(16) . ? C23 C26 1.493(16) . ? C23 C25 1.512(19) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.393(12) . ? C27 H27 0.9300 . ? C28 C29 1.429(13) . ? C28 C35 1.440(12) . ? C29 C30 1.398(12) . ? C29 C34 1.400(13) . ? C30 C31 1.351(13) . ? C31 C32 1.382(16) . ? C31 H31 0.9300 . ? C32 C33 1.420(17) . ? C32 H32 0.9300 . ? C33 C34 1.316(15) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.461(17) . ? C36 C39 1.508(18) . ? C36 C38 1.531(17) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C47 1.450(16) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.490(19) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.497(16) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Y1 N3 100.5(3) . . ? N1 Y1 O1 87.2(2) . . ? N3 Y1 O1 171.6(2) . . ? N1 Y1 Cl1 113.84(18) . . ? N3 Y1 Cl1 90.18(18) . . ? O1 Y1 Cl1 83.48(17) . . ? N1 Y1 C1 30.9(2) . . ? N3 Y1 C1 91.0(2) . . ? O1 Y1 C1 94.0(2) . . ? Cl1 Y1 C1 84.70(17) . . ? N1 Y1 Cl2 85.08(18) . 2_767 ? N3 Y1 Cl2 93.19(18) . 2_767 ? O1 Y1 Cl2 90.90(17) . 2_767 ? Cl1 Y1 Cl2 159.83(7) . 2_767 ? C1 Y1 Cl2 115.08(17) . 2_767 ? N1 Y1 Cl2 159.98(19) . . ? N3 Y1 Cl2 89.51(18) . . ? O1 Y1 Cl2 84.21(16) . . ? Cl1 Y1 Cl2 83.12(7) . . ? C1 Y1 Cl2 167.81(17) . . ? Cl2 Y1 Cl2 77.04(7) 2_767 . ? N7 Y2 N5 119.3(3) . . ? N7 Y2 N2 105.0(3) . . ? N5 Y2 N2 93.6(3) . . ? N7 Y2 C1 139.4(3) . . ? N5 Y2 C1 101.1(3) . . ? N2 Y2 C1 74.5(3) . . ? N7 Y2 Cl1 89.01(18) . . ? N5 Y2 Cl1 90.1(2) . . ? N2 Y2 Cl1 161.3(2) . . ? C1 Y2 Cl1 86.81(18) . . ? N7 Y2 Si1 30.2(2) . . ? N5 Y2 Si1 149.4(2) . . ? N2 Y2 Si1 98.56(18) . . ? C1 Y2 Si1 109.22(18) . . ? Cl1 Y2 Si1 87.34(8) . . ? Y1 Cl1 Y2 92.01(7) . . ? Y1 Cl2 Y1 102.96(7) 2_767 . ? N7 Si1 C42 114.1(6) . . ? N7 Si1 C40 107.9(4) . . ? C42 Si1 C40 105.7(6) . . ? N7 Si1 C41 114.1(5) . . ? C42 Si1 C41 108.9(6) . . ? C40 Si1 C41 105.5(6) . . ? N7 Si1 Y2 41.0(2) . . ? C42 Si1 Y2 122.1(5) . . ? C40 Si1 Y2 67.0(3) . . ? C41 Si1 Y2 128.7(5) . . ? N7 Si2 C45 108.8(5) . . ? N7 Si2 C44 111.5(5) . . ? C45 Si2 C44 111.5(7) . . ? N7 Si2 C43 114.4(5) . . ? C45 Si2 C43 105.9(6) . . ? C44 Si2 C43 104.6(6) . . ? N6 Li1 N4 156.9(11) . . ? N6 Li1 C22 171.8(11) . . ? N4 Li1 C22 30.1(4) . . ? N6 Li1 C15 142.2(9) . . ? N4 Li1 C15 60.6(6) . . ? C22 Li1 C15 32.7(4) . . ? N6 Li1 C16 116.8(9) . . ? N4 Li1 C16 82.0(7) . . ? C22 Li1 C16 61.1(5) . . ? C15 Li1 C16 32.1(3) . . ? N6 Li1 C21 101.7(8) . . ? N4 Li1 C21 87.7(8) . . ? C22 Li1 C21 80.3(6) . . ? C15 Li1 C21 60.3(5) . . ? C16 Li1 C21 31.8(4) . . ? N6 Li1 C35 27.8(4) . . ? N4 Li1 C35 171.8(11) . . ? C22 Li1 C35 144.4(9) . . ? C15 Li1 C35 116.5(7) . . ? C16 Li1 C35 98.8(7) . . ? C21 Li1 C35 97.3(7) . . ? N6 Li1 C34 88.4(8) . . ? N4 Li1 C34 94.1(8) . . ? C22 Li1 C34 86.1(7) . . ? C15 Li1 C34 94.3(7) . . ? C16 Li1 C34 118.4(8) . . ? C21 Li1 C34 149.5(8) . . ? C35 Li1 C34 78.3(6) . . ? N6 Li1 C29 78.6(7) . . ? N4 Li1 C29 113.8(9) . . ? C22 Li1 C29 93.6(7) . . ? C15 Li1 C29 85.1(6) . . ? C16 Li1 C29 97.5(7) . . ? C21 Li1 C29 123.7(7) . . ? C35 Li1 C29 58.0(5) . . ? C34 Li1 C29 30.0(4) . . ? N6 Li1 C28 57.0(6) . . ? N4 Li1 C28 141.3(10) . . ? C22 Li1 C28 114.9(8) . . ? C15 Li1 C28 93.3(6) . . ? C16 Li1 C28 89.3(6) . . ? C21 Li1 C28 104.3(7) . . ? C35 Li1 C28 30.9(3) . . ? C34 Li1 C28 57.5(5) . . ? C29 Li1 C28 30.1(3) . . ? C1 N1 C4 109.5(7) . . ? C1 N1 Y1 92.9(5) . . ? C4 N1 Y1 156.5(6) . . ? C9 N2 C10 119.0(8) . . ? C9 N2 Y2 112.1(5) . . ? C10 N2 Y2 128.9(6) . . ? C17 N3 C14 105.6(7) . . ? C17 N3 Y1 129.9(5) . . ? C14 N3 Y1 123.3(6) . . ? C22 N4 C23 119.9(9) . . ? C22 N4 Li1 98.0(8) . . ? C23 N4 Li1 134.0(9) . . ? C30 N5 C27 104.7(7) . . ? C30 N5 Y2 137.9(6) . . ? C27 N5 Y2 117.2(6) . . ? C35 N6 C36 120.4(9) . . ? C35 N6 Li1 104.6(8) . . ? C36 N6 Li1 128.0(9) . . ? Si2 N7 Si1 121.6(4) . . ? Si2 N7 Y2 127.4(4) . . ? Si1 N7 Y2 108.8(4) . . ? C46 O1 C49 108.5(8) . . ? C46 O1 Y1 128.1(6) . . ? C49 O1 Y1 122.5(6) . . ? N1 C1 C2 107.4(7) . . ? N1 C1 Y2 149.7(6) . . ? C2 C1 Y2 102.5(5) . . ? N1 C1 Y1 56.1(4) . . ? C2 C1 Y1 162.2(6) . . ? Y2 C1 Y1 94.7(2) . . ? C1 C2 C3 108.6(7) . . ? C1 C2 C9 126.9(8) . . ? C3 C2 C9 124.5(8) . . ? C4 C3 C2 106.1(8) . . ? C4 C3 C8 117.0(9) . . ? C2 C3 C8 136.9(9) . . ? C5 C4 N1 128.8(9) . . ? C5 C4 C3 122.8(9) . . ? N1 C4 C3 108.4(8) . . ? C4 C5 C6 116.8(11) . . ? C4 C5 H5 121.6 . . ? C6 C5 H5 121.6 . . ? C7 C6 C5 121.3(11) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C8 C7 C6 121.1(10) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C3 120.8(10) . . ? C7 C8 H8 119.6 . . ? C3 C8 H8 119.6 . . ? N2 C9 C2 123.5(8) . . ? N2 C9 H9 118.3 . . ? C2 C9 H9 118.3 . . ? C11 C10 C12 106.7(11) . . ? C11 C10 N2 107.1(8) . . ? C12 C10 N2 110.9(9) . . ? C11 C10 C13 112.8(10) . . ? C12 C10 C13 111.6(11) . . ? N2 C10 C13 107.8(8) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 C15 112.6(8) . . ? N3 C14 H14 123.7 . . ? C15 C14 H14 123.7 . . ? C14 C15 C16 103.4(8) . . ? C14 C15 C22 125.8(9) . . ? C16 C15 C22 130.8(9) . . ? C14 C15 Li1 133.5(8) . . ? C16 C15 Li1 74.2(6) . . ? C22 C15 Li1 72.7(7) . . ? C17 C16 C21 119.8(9) . . ? C17 C16 C15 107.5(8) . . ? C21 C16 C15 132.7(9) . . ? C17 C16 Li1 132.7(7) . . ? C21 C16 Li1 75.8(7) . . ? C15 C16 Li1 73.7(7) . . ? N3 C17 C16 111.0(7) . . ? N3 C17 C18 127.8(8) . . ? C16 C17 C18 121.1(8) . . ? C19 C18 C17 116.4(10) . . ? C19 C18 H18 121.8 . . ? C17 C18 H18 121.8 . . ? C20 C19 C18 123.8(11) . . ? C20 C19 H19 118.1 . . ? C18 C19 H19 118.1 . . ? C19 C20 C21 120.1(11) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C16 118.9(10) . . ? C20 C21 Li1 133.0(10) . . ? C16 C21 Li1 72.5(7) . . ? C20 C21 H21 120.6 . . ? C16 C21 H21 120.6 . . ? Li1 C21 H21 68.0 . . ? N4 C22 C15 119.8(9) . . ? N4 C22 Li1 51.9(6) . . ? C15 C22 Li1 74.5(7) . . ? N4 C22 H22 120.1 . . ? C15 C22 H22 120.1 . . ? Li1 C22 H22 151.8 . . ? C24 C23 C26 109.8(13) . . ? C24 C23 N4 117.3(10) . . ? C26 C23 N4 105.7(10) . . ? C24 C23 C25 108.4(13) . . ? C26 C23 C25 109.9(13) . . ? N4 C23 C25 105.5(11) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N5 C27 C28 113.2(8) . . ? N5 C27 H27 123.4 . . ? C28 C27 H27 123.4 . . ? C27 C28 C29 104.2(8) . . ? C27 C28 C35 126.4(9) . . ? C29 C28 C35 129.4(9) . . ? C27 C28 Li1 137.3(7) . . ? C29 C28 Li1 74.0(7) . . ? C35 C28 Li1 68.6(7) . . ? C30 C29 C34 119.4(9) . . ? C30 C29 C28 106.0(8) . . ? C34 C29 C28 134.6(9) . . ? C30 C29 Li1 135.4(7) . . ? C34 C29 Li1 72.2(7) . . ? C28 C29 Li1 75.9(6) . . ? C31 C30 N5 128.0(9) . . ? C31 C30 C29 120.2(10) . . ? N5 C30 C29 111.8(8) . . ? C30 C31 C32 118.4(11) . . ? C30 C31 H31 120.8 . . ? C32 C31 H31 120.8 . . ? C31 C32 C33 122.5(12) . . ? C31 C32 H32 118.7 . . ? C33 C32 H32 118.7 . . ? C34 C33 C32 117.2(11) . . ? C34 C33 H33 121.4 . . ? C32 C33 H33 121.4 . . ? C33 C34 C29 122.2(11) . . ? C33 C34 Li1 132.7(10) . . ? C29 C34 Li1 77.8(7) . . ? C33 C34 H34 118.9 . . ? C29 C34 H34 118.9 . . ? Li1 C34 H34 61.0 . . ? N6 C35 C28 122.6(10) . . ? N6 C35 Li1 47.7(6) . . ? C28 C35 Li1 80.5(7) . . ? N6 C35 H35 118.7 . . ? C28 C35 H35 118.7 . . ? Li1 C35 H35 150.9 . . ? C37 C36 N6 111.8(10) . . ? C37 C36 C39 109.5(12) . . ? N6 C36 C39 106.4(11) . . ? C37 C36 C38 113.6(14) . . ? N6 C36 C38 104.6(9) . . ? C39 C36 C38 110.6(12) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si1 C40 H40A 109.5 . . ? Si1 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si1 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si1 C41 H41A 109.5 . . ? Si1 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si1 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si1 C42 H42A 109.5 . . ? Si1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si2 C43 H43A 109.5 . . ? Si2 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si2 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si2 C44 H44A 109.5 . . ? Si2 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si2 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si2 C45 H45A 109.5 . . ? Si2 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si2 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 O1 106.9(10) . . ? C47 C46 H46A 110.4 . . ? O1 C46 H46A 110.4 . . ? C47 C46 H46B 110.4 . . ? O1 C46 H46B 110.4 . . ? H46A C46 H46B 108.6 . . ? C46 C47 C48 107.1(11) . . ? C46 C47 H47A 110.3 . . ? C48 C47 H47A 110.3 . . ? C46 C47 H47B 110.3 . . ? C48 C47 H47B 110.3 . . ? H47A C47 H47B 108.6 . . ? C47 C48 C49 106.6(11) . . ? C47 C48 H48A 110.4 . . ? C49 C48 H48A 110.4 . . ? C47 C48 H48B 110.4 . . ? C49 C48 H48B 110.4 . . ? H48A C48 H48B 108.6 . . ? O1 C49 C48 106.1(11) . . ? O1 C49 H49A 110.5 . . ? C48 C49 H49A 110.5 . . ? O1 C49 H49B 110.5 . . ? C48 C49 H49B 110.5 . . ? H49A C49 H49B 108.7 . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.115 0.500 0.578 1108 240 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.855 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.178 # Attachment '- 110307a_0m.cif' data_110307a_0m _database_code_depnum_ccdc_archive 'CCDC 842360' #TrackingRef '- 110307a_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H66 Li4 N6 Si4' _chemical_formula_weight 747.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1116(8) _cell_length_b 11.2374(10) _cell_length_c 12.0801(11) _cell_angle_alpha 97.2570(10) _cell_angle_beta 100.0590(10) _cell_angle_gamma 101.9070(10) _cell_volume 1174.63(18) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4019 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.04 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.056 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 0.157 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9529 _exptl_absorpt_correction_T_max 0.9633 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9138 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4549 _reflns_number_gt 3447 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+0.2602P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4549 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1340 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4054(3) 0.82381(19) 1.06495(17) 0.0495(5) Uani 1 1 d . . . Li1 Li 0.2550(5) 0.6666(3) 0.7933(3) 0.0604(9) Uani 1 1 d . . . N1 N 0.5463(2) 0.88557(15) 1.04948(15) 0.0555(5) Uani 1 1 d . . . Si1 Si 0.32124(6) 0.84548(5) 0.62872(5) 0.04472(17) Uani 1 1 d . . . C2 C 0.3137(3) 0.8647(2) 1.1353(2) 0.0644(6) Uani 1 1 d . . . H2 H 0.3421 0.9444 1.1768 0.077 Uiso 1 1 calc R . . N2 N 0.3616(2) 0.52715(15) 0.79285(15) 0.0531(5) Uani 1 1 d . . . Si2 Si 0.05162(6) 0.82895(6) 0.74175(5) 0.04915(18) Uani 1 1 d . . . C3 C 0.1816(3) 0.7858(3) 1.1421(2) 0.0818(8) Uani 1 1 d . . . H3 H 0.1197 0.8120 1.1891 0.098 Uiso 1 1 calc R . . N3 N 0.23650(17) 0.82268(14) 0.74203(13) 0.0393(4) Uani 1 1 d . . . C4 C 0.1376(3) 0.6665(3) 1.0798(3) 0.0902(10) Uani 1 1 d . . . H4 H 0.0471 0.6143 1.0865 0.108 Uiso 1 1 calc R . . C5 C 0.2248(3) 0.6244(2) 1.0089(2) 0.0738(7) Uani 1 1 d . . . H5 H 0.1938 0.5447 0.9674 0.089 Uiso 1 1 calc R . . C6 C 0.3615(3) 0.70310(19) 0.99990(17) 0.0520(5) Uani 1 1 d . . . C7 C 0.4841(3) 0.69046(18) 0.94343(17) 0.0499(5) Uani 1 1 d . . . C8 C 0.5910(3) 0.80306(19) 0.97864(18) 0.0538(5) Uani 1 1 d . . . H8 H 0.6843 0.8200 0.9557 0.065 Uiso 1 1 calc R . . C9 C 0.4864(3) 0.58738(19) 0.85929(18) 0.0546(5) Uani 1 1 d . . . H9 H 0.5781 0.5653 0.8538 0.066 Uiso 1 1 calc R . . C10 C 0.3521(3) 0.41523(19) 0.70986(19) 0.0596(6) Uani 1 1 d . . . C11 C 0.2745(4) 0.4373(3) 0.5954(2) 0.1003(11) Uani 1 1 d . . . H11A H 0.1748 0.4507 0.5999 0.150 Uiso 1 1 calc R . . H11B H 0.2642 0.3667 0.5384 0.150 Uiso 1 1 calc R . . H11C H 0.3352 0.5087 0.5752 0.150 Uiso 1 1 calc R . . C12 C 0.2483(4) 0.3105(2) 0.7480(3) 0.0929(10) Uani 1 1 d . . . H12A H 0.2975 0.2971 0.8209 0.139 Uiso 1 1 calc R . . H12B H 0.2290 0.2365 0.6931 0.139 Uiso 1 1 calc R . . H12C H 0.1530 0.3319 0.7542 0.139 Uiso 1 1 calc R . . C13 C 0.5054(4) 0.3848(3) 0.7026(3) 0.0915(9) Uani 1 1 d . . . H13A H 0.5708 0.4526 0.6811 0.137 Uiso 1 1 calc R . . H13B H 0.4895 0.3122 0.6466 0.137 Uiso 1 1 calc R . . H13C H 0.5527 0.3702 0.7756 0.137 Uiso 1 1 calc R . . C14 C 0.5109(3) 0.8023(2) 0.6518(2) 0.0594(6) Uani 1 1 d . . . H14A H 0.5751 0.8504 0.7213 0.089 Uiso 1 1 calc R . . H14B H 0.5594 0.8182 0.5890 0.089 Uiso 1 1 calc R . . H14C H 0.4954 0.7162 0.6571 0.089 Uiso 1 1 calc R . . C15 C 0.3588(3) 1.0109(2) 0.6087(2) 0.0697(7) Uani 1 1 d . . . H15A H 0.2633 1.0317 0.5817 0.105 Uiso 1 1 calc R . . H15B H 0.4229 1.0229 0.5539 0.105 Uiso 1 1 calc R . . H15C H 0.4093 1.0629 0.6801 0.105 Uiso 1 1 calc R . . C16 C 0.2096(3) 0.7509(3) 0.4888(2) 0.0760(8) Uani 1 1 d . . . H16A H 0.1765 0.6666 0.4982 0.114 Uiso 1 1 calc R . . H16B H 0.2735 0.7551 0.4333 0.114 Uiso 1 1 calc R . . H16C H 0.1218 0.7826 0.4632 0.114 Uiso 1 1 calc R . . C17 C -0.0454(3) 0.8986(3) 0.6261(2) 0.0801(8) Uani 1 1 d . . . H17A H 0.0103 0.9820 0.6302 0.120 Uiso 1 1 calc R . . H17B H -0.1481 0.8982 0.6351 0.120 Uiso 1 1 calc R . . H17C H -0.0483 0.8515 0.5533 0.120 Uiso 1 1 calc R . . C18 C -0.0705(3) 0.6710(3) 0.7345(3) 0.0987(11) Uani 1 1 d . . . H18A H -0.0586 0.6168 0.6703 0.148 Uiso 1 1 calc R . . H18B H -0.1760 0.6751 0.7261 0.148 Uiso 1 1 calc R . . H18C H -0.0395 0.6402 0.8033 0.148 Uiso 1 1 calc R . . C19 C 0.0416(3) 0.9241(4) 0.8772(3) 0.0996(11) Uani 1 1 d . . . H19A H 0.0775 0.8867 0.9406 0.149 Uiso 1 1 calc R . . H19B H -0.0626 0.9289 0.8762 0.149 Uiso 1 1 calc R . . H19C H 0.1046 1.0056 0.8845 0.149 Uiso 1 1 calc R . . Li2 Li 0.6429(5) 1.0613(3) 1.1137(3) 0.0616(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0592(13) 0.0446(11) 0.0392(11) 0.0066(8) 0.0014(9) 0.0073(9) Li1 0.077(3) 0.048(2) 0.055(2) 0.0071(16) 0.0067(18) 0.0187(18) N1 0.0633(12) 0.0419(9) 0.0528(11) 0.0009(8) 0.0061(9) 0.0027(8) Si1 0.0486(3) 0.0486(3) 0.0409(3) 0.0079(2) 0.0138(2) 0.0163(2) C2 0.0737(16) 0.0609(14) 0.0515(13) -0.0024(11) 0.0067(12) 0.0125(12) N2 0.0679(12) 0.0381(9) 0.0462(10) -0.0014(7) -0.0026(9) 0.0134(8) Si2 0.0405(3) 0.0599(4) 0.0478(3) 0.0071(3) 0.0110(2) 0.0130(3) C3 0.0738(18) 0.102(2) 0.0658(16) 0.0015(15) 0.0245(14) 0.0116(16) N3 0.0392(8) 0.0389(8) 0.0398(9) 0.0027(6) 0.0090(7) 0.0109(6) C4 0.0721(18) 0.100(2) 0.0790(19) -0.0025(17) 0.0235(15) -0.0182(16) C5 0.0756(17) 0.0657(15) 0.0610(15) -0.0025(12) 0.0097(13) -0.0145(13) C6 0.0601(13) 0.0451(11) 0.0397(11) 0.0039(9) -0.0016(9) -0.0007(9) C7 0.0588(13) 0.0425(11) 0.0412(11) 0.0031(8) -0.0001(9) 0.0071(9) C8 0.0545(13) 0.0496(12) 0.0508(12) 0.0033(10) 0.0048(10) 0.0058(10) C9 0.0634(14) 0.0485(12) 0.0490(12) 0.0057(9) 0.0031(10) 0.0147(10) C10 0.0806(16) 0.0394(11) 0.0514(13) -0.0033(9) -0.0012(11) 0.0170(11) C11 0.156(3) 0.0672(17) 0.0576(16) -0.0115(13) -0.0204(18) 0.0308(18) C12 0.124(3) 0.0464(14) 0.100(2) -0.0042(14) 0.028(2) 0.0068(15) C13 0.099(2) 0.0795(19) 0.090(2) -0.0207(16) 0.0145(17) 0.0321(17) C14 0.0547(13) 0.0668(14) 0.0658(15) 0.0135(11) 0.0249(11) 0.0224(11) C15 0.0800(18) 0.0621(14) 0.0829(18) 0.0316(13) 0.0333(14) 0.0265(13) C16 0.0882(19) 0.0936(19) 0.0455(13) -0.0027(13) 0.0094(12) 0.0318(15) C17 0.0560(15) 0.109(2) 0.0850(19) 0.0313(16) 0.0093(13) 0.0362(15) C18 0.0596(17) 0.093(2) 0.133(3) 0.034(2) 0.0136(18) -0.0080(15) C19 0.0741(19) 0.155(3) 0.0758(19) -0.0147(19) 0.0250(15) 0.053(2) Li2 0.076(3) 0.0454(19) 0.053(2) -0.0044(16) 0.0123(19) -0.0014(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.383(3) . ? C1 C2 1.393(3) . ? C1 C6 1.419(3) . ? C1 Li2 2.669(5) 2_677 ? Li1 N3 1.962(4) . ? Li1 N2 2.007(4) . ? Li1 C7 2.458(5) . ? Li1 C6 2.464(4) . ? Li1 C9 2.498(5) . ? Li1 Li2 3.012(5) 2_677 ? N1 C8 1.355(3) . ? N1 Li2 1.983(4) . ? N1 Li2 2.598(5) 2_677 ? Si1 N3 1.7063(16) . ? Si1 C15 1.874(2) . ? Si1 C14 1.874(2) . ? Si1 C16 1.877(2) . ? Si1 Li2 3.093(4) 2_677 ? C2 C3 1.361(4) . ? C2 H2 0.9300 . ? N2 C9 1.273(3) . ? N2 C10 1.484(3) . ? Si2 N3 1.7000(16) . ? Si2 C19 1.865(3) . ? Si2 C17 1.865(3) . ? Si2 C18 1.873(3) . ? Si2 Li2 2.943(4) 2_677 ? C3 C4 1.394(4) . ? C3 H3 0.9300 . ? N3 Li2 2.028(4) 2_677 ? C4 C5 1.371(4) . ? C4 H4 0.9300 . ? C5 C6 1.401(3) . ? C5 H5 0.9300 . ? C6 C7 1.428(3) . ? C7 C8 1.393(3) . ? C7 C9 1.448(3) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.514(4) . ? C10 C13 1.519(4) . ? C10 C12 1.524(4) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? Li2 N3 2.028(4) 2_677 ? Li2 N1 2.598(5) 2_677 ? Li2 C1 2.669(5) 2_677 ? Li2 Si2 2.943(4) 2_677 ? Li2 Li1 3.012(5) 2_677 ? Li2 Si1 3.093(4) 2_677 ? Li2 Li2 3.360(8) 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 N1 C1 C2 128.37(19) . . ? N1 C1 C6 110.63(19) . . ? C2 C1 C6 121.0(2) . . ? N1 C1 Li2 71.94(15) . 2_677 ? C2 C1 Li2 103.54(18) . 2_677 ? C6 C1 Li2 95.28(15) . 2_677 ? N3 Li1 N2 147.8(2) . . ? N3 Li1 C7 112.59(18) . . ? N2 Li1 C7 62.57(13) . . ? N3 Li1 C6 110.20(17) . . ? N2 Li1 C6 83.14(16) . . ? C7 Li1 C6 33.74(9) . . ? N3 Li1 C9 130.8(2) . . ? N2 Li1 C9 30.42(9) . . ? C7 Li1 C9 33.95(9) . . ? C6 Li1 C9 62.35(12) . . ? N3 Li1 Li2 41.81(12) . 2_677 ? N2 Li1 Li2 133.6(2) . 2_677 ? C7 Li1 Li2 74.41(14) . 2_677 ? C6 Li1 Li2 69.05(13) . 2_677 ? C9 Li1 Li2 103.44(16) . 2_677 ? C8 N1 C1 104.99(17) . . ? C8 N1 Li2 130.7(2) . . ? C1 N1 Li2 124.14(19) . . ? C8 N1 Li2 93.79(15) . 2_677 ? C1 N1 Li2 77.64(15) . 2_677 ? Li2 N1 Li2 93.37(15) . 2_677 ? N3 Si1 C15 112.07(10) . . ? N3 Si1 C14 110.05(9) . . ? C15 Si1 C14 107.08(11) . . ? N3 Si1 C16 114.65(11) . . ? C15 Si1 C16 106.97(13) . . ? C14 Si1 C16 105.56(12) . . ? N3 Si1 Li2 37.56(9) . 2_677 ? C15 Si1 Li2 87.68(11) . 2_677 ? C14 Si1 Li2 92.14(11) . 2_677 ? C16 Si1 Li2 151.99(12) . 2_677 ? C3 C2 C1 118.7(2) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C9 N2 C10 122.8(2) . . ? C9 N2 Li1 96.65(18) . . ? C10 N2 Li1 134.52(18) . . ? N3 Si2 C19 109.62(11) . . ? N3 Si2 C17 116.90(11) . . ? C19 Si2 C17 105.03(15) . . ? N3 Si2 C18 110.64(12) . . ? C19 Si2 C18 107.18(17) . . ? C17 Si2 C18 106.93(15) . . ? N3 Si2 Li2 41.97(9) . 2_677 ? C19 Si2 Li2 67.83(12) . 2_677 ? C17 Si2 Li2 125.23(13) . 2_677 ? C18 Si2 Li2 127.43(13) . 2_677 ? C2 C3 C4 121.1(3) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? Si2 N3 Si1 123.24(9) . . ? Si2 N3 Li1 104.69(15) . . ? Si1 N3 Li1 112.16(14) . . ? Si2 N3 Li2 103.93(14) . 2_677 ? Si1 N3 Li2 111.58(14) . 2_677 ? Li1 N3 Li2 98.03(18) . 2_677 ? C5 C4 C3 121.4(3) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 C6 119.0(2) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C5 C6 C1 118.8(2) . . ? C5 C6 C7 135.0(2) . . ? C1 C6 C7 105.96(18) . . ? C5 C6 Li1 86.36(17) . . ? C1 C6 Li1 121.45(17) . . ? C7 C6 Li1 72.91(15) . . ? C8 C7 C6 104.70(18) . . ? C8 C7 C9 128.4(2) . . ? C6 C7 C9 126.57(19) . . ? C8 C7 Li1 121.26(17) . . ? C6 C7 Li1 73.36(16) . . ? C9 C7 Li1 74.54(15) . . ? N1 C8 C7 113.7(2) . . ? N1 C8 H8 123.2 . . ? C7 C8 H8 123.2 . . ? N2 C9 C7 119.4(2) . . ? N2 C9 Li1 52.93(14) . . ? C7 C9 Li1 71.51(15) . . ? N2 C9 H9 120.3 . . ? C7 C9 H9 120.3 . . ? Li1 C9 H9 155.7 . . ? N2 C10 C11 106.09(19) . . ? N2 C10 C13 114.66(19) . . ? C11 C10 C13 110.5(3) . . ? N2 C10 C12 105.3(2) . . ? C11 C10 C12 109.6(2) . . ? C13 C10 C12 110.4(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 Li2 N3 143.4(2) . 2_677 ? N1 Li2 N1 86.63(15) . 2_677 ? N3 Li2 N1 126.42(19) 2_677 2_677 ? N1 Li2 C1 103.51(16) . 2_677 ? N3 Li2 C1 113.03(17) 2_677 2_677 ? N1 Li2 C1 30.42(8) 2_677 2_677 ? N1 Li2 Si2 129.1(2) . 2_677 ? N3 Li2 Si2 34.10(8) 2_677 2_677 ? N1 Li2 Si2 138.77(15) 2_677 2_677 ? C1 Li2 Si2 110.86(14) 2_677 2_677 ? N1 Li2 Li1 172.1(2) . 2_677 ? N3 Li2 Li1 40.16(11) 2_677 2_677 ? N1 Li2 Li1 87.70(14) 2_677 2_677 ? C1 Li2 Li1 73.90(13) 2_677 2_677 ? Si2 Li2 Li1 58.35(10) 2_677 2_677 ? N1 Li2 Si1 119.76(17) . 2_677 ? N3 Li2 Si1 30.86(7) 2_677 2_677 ? N1 Li2 Si1 125.48(16) 2_677 2_677 ? C1 Li2 Si1 130.47(14) 2_677 2_677 ? Si2 Li2 Si1 59.48(7) 2_677 2_677 ? Li1 Li2 Si1 59.87(10) 2_677 2_677 ? N1 Li2 Li2 50.52(11) . 2_677 ? N3 Li2 Li2 158.9(3) 2_677 2_677 ? N1 Li2 Li2 36.11(10) 2_677 2_677 ? C1 Li2 Li2 58.07(13) 2_677 2_677 ? Si2 Li2 Li2 162.5(2) 2_677 2_677 ? Li1 Li2 Li2 123.6(2) 2_677 2_677 ? Si1 Li2 Li2 137.9(2) 2_677 2_677 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.260 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.039 # Attachment '- 110811a_0m.cif' data_110811a_0m _database_code_depnum_ccdc_archive 'CCDC 842361' #TrackingRef '- 110811a_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H70 Li N6 Si4 Yb' _chemical_formula_weight 903.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 'P2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 12.454(3) _cell_length_b 15.076(3) _cell_length_c 15.519(3) _cell_angle_alpha 90.00 _cell_angle_beta 124.822(13) _cell_angle_gamma 90.00 _cell_volume 2392.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4807 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 21.58 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 938 _exptl_absorpt_coefficient_mu 2.085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5928 _exptl_absorpt_correction_T_max 0.6685 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19741 _diffrn_reflns_av_R_equivalents 0.0814 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.64 _reflns_number_total 5505 _reflns_number_gt 3249 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+6.6576P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5505 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1321 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1726 _refine_ls_wR_factor_gt 0.1418 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.007 _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 1.0000 0.26543(3) 0.7500 0.0610(2) Uani 1 2 d S . . Si1 Si 0.7214(3) 0.3326(3) 0.7378(3) 0.1101(11) Uani 1 1 d . . . Si2 Si 0.7794(3) 0.4008(2) 0.5876(3) 0.0956(9) Uani 1 1 d . . . N1 N 1.0333(7) 0.1528(4) 0.8603(6) 0.075(2) Uani 1 1 d . . . N2 N 0.8463(6) -0.1140(4) 0.7580(5) 0.0633(17) Uani 1 1 d . . . H2 H 0.7779 -0.0831 0.7042 0.076 Uiso 1 1 d R . . N3 N 0.8163(7) 0.3367(5) 0.6931(6) 0.087(2) Uani 1 1 d . . . C1 C 0.9306(8) 0.0972(6) 0.8321(6) 0.074(2) Uani 1 1 d . . . H1 H 0.8438 0.1158 0.7914 0.088 Uiso 1 1 calc R . . C2 C 0.9663(9) 0.0134(5) 0.8685(6) 0.064(2) Uani 1 1 d . . . C3 C 1.1048(8) 0.0128(5) 0.9264(6) 0.062(2) Uani 1 1 d . . . C4 C 1.1408(8) 0.0997(5) 0.9182(6) 0.063(2) Uani 1 1 d . . . C5 C 1.2742(9) 0.1209(6) 0.9651(8) 0.080(3) Uani 1 1 d . . . H5 H 1.2993 0.1776 0.9600 0.096 Uiso 1 1 calc R . . C6 C 1.3637(11) 0.0559(8) 1.0176(9) 0.105(3) Uani 1 1 d . . . H6 H 1.4514 0.0683 1.0474 0.126 Uiso 1 1 calc R . . C7 C 1.3285(12) -0.0294(8) 1.0284(8) 0.106(4) Uani 1 1 d . . . H7 H 1.3933 -0.0718 1.0665 0.127 Uiso 1 1 calc R . . C8 C 1.2024(11) -0.0513(6) 0.9845(7) 0.086(3) Uani 1 1 d . . . H8 H 1.1803 -0.1082 0.9926 0.103 Uiso 1 1 calc R . . C9 C 0.8788(10) -0.0624(5) 0.8521(7) 0.077(2) Uani 1 1 d . . . H9A H 0.9225 -0.1004 0.9135 0.092 Uiso 1 1 calc R . . H9B H 0.7993 -0.0400 0.8418 0.092 Uiso 1 1 calc R . . C10 C 0.7882(8) -0.2033(5) 0.7486(6) 0.070(2) Uani 1 1 d . . . C11 C 0.7309(12) -0.2349(6) 0.6367(8) 0.097(3) Uani 1 1 d . . . H11A H 0.6612 -0.1959 0.5878 0.145 Uiso 1 1 calc R . . H11B H 0.6975 -0.2940 0.6280 0.145 Uiso 1 1 calc R . . H11C H 0.7979 -0.2345 0.6241 0.145 Uiso 1 1 calc R . . C12 C 0.6802(11) -0.2007(8) 0.7663(9) 0.109(4) Uani 1 1 d . . . H12A H 0.7177 -0.1904 0.8393 0.163 Uiso 1 1 calc R . . H12B H 0.6345 -0.2563 0.7456 0.163 Uiso 1 1 calc R . . H12C H 0.6202 -0.1538 0.7253 0.163 Uiso 1 1 calc R . . C13 C 0.8968(11) -0.2651(6) 0.8267(8) 0.099(3) Uani 1 1 d . . . H13A H 0.9624 -0.2680 0.8126 0.148 Uiso 1 1 calc R . . H13B H 0.8616 -0.3233 0.8205 0.148 Uiso 1 1 calc R . . H13C H 0.9352 -0.2432 0.8966 0.148 Uiso 1 1 calc R . . C16 C 0.6600(19) 0.4411(12) 0.7446(16) 0.218(10) Uani 1 1 d . . . H16A H 0.7227 0.4862 0.7588 0.327 Uiso 1 1 calc R . . H16B H 0.6465 0.4406 0.7996 0.327 Uiso 1 1 calc R . . H16C H 0.5787 0.4535 0.6788 0.327 Uiso 1 1 calc R . . C15 C 0.5805(15) 0.2544(14) 0.6607(15) 0.220(11) Uani 1 1 d . . . H15A H 0.5123 0.2828 0.5970 0.329 Uiso 1 1 calc R . . H15B H 0.5478 0.2383 0.7016 0.329 Uiso 1 1 calc R . . H15C H 0.6091 0.2022 0.6439 0.329 Uiso 1 1 calc R . . C14 C 0.8010(11) 0.2906(8) 0.8763(9) 0.111(4) Uani 1 1 d . . . H14A H 0.8455 0.2359 0.8850 0.166 Uiso 1 1 calc R . . H14B H 0.7352 0.2809 0.8892 0.166 Uiso 1 1 calc R . . H14C H 0.8627 0.3337 0.9250 0.166 Uiso 1 1 calc R . . C17 C 0.6140(13) 0.3815(11) 0.4641(10) 0.180(7) Uani 1 1 d . . . H17A H 0.5946 0.3192 0.4562 0.271 Uiso 1 1 calc R . . H17B H 0.6129 0.4024 0.4052 0.271 Uiso 1 1 calc R . . H17C H 0.5495 0.4130 0.4675 0.271 Uiso 1 1 calc R . . C19 C 0.8869(12) 0.3784(9) 0.5446(10) 0.132(4) Uani 1 1 d . . . H19A H 0.9765 0.3833 0.6034 0.199 Uiso 1 1 calc R . . H19B H 0.8696 0.4207 0.4918 0.199 Uiso 1 1 calc R . . H19C H 0.8707 0.3196 0.5160 0.199 Uiso 1 1 calc R . . C18 C 0.7921(17) 0.5225(7) 0.6049(15) 0.187(8) Uani 1 1 d . . . H18A H 0.7550 0.5402 0.6421 0.281 Uiso 1 1 calc R . . H18B H 0.7454 0.5508 0.5374 0.281 Uiso 1 1 calc R . . H18C H 0.8824 0.5398 0.6442 0.281 Uiso 1 1 calc R . . Li1 Li 1.0000 -0.0758(13) 0.7500 0.078(6) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.0509(3) 0.0447(3) 0.0745(3) 0.000 0.0282(2) 0.000 Si1 0.0696(18) 0.140(3) 0.099(2) -0.0037(19) 0.0355(17) 0.0181(18) Si2 0.0836(19) 0.0796(19) 0.101(2) 0.0028(15) 0.0395(17) 0.0182(14) N1 0.059(4) 0.053(4) 0.088(5) 0.009(3) 0.028(4) 0.002(3) N2 0.069(4) 0.052(4) 0.058(4) -0.002(3) 0.030(3) -0.008(3) N3 0.062(4) 0.074(5) 0.094(5) -0.022(4) 0.027(4) 0.005(3) C1 0.061(5) 0.070(6) 0.072(5) 0.004(4) 0.027(4) -0.010(4) C2 0.082(6) 0.050(5) 0.060(5) -0.006(4) 0.041(4) -0.013(4) C3 0.080(6) 0.055(5) 0.052(4) -0.006(3) 0.038(4) -0.001(4) C4 0.073(5) 0.048(4) 0.064(5) -0.002(3) 0.036(4) -0.011(4) C5 0.076(6) 0.062(5) 0.101(7) -0.004(5) 0.049(6) -0.004(5) C6 0.079(7) 0.095(8) 0.105(8) -0.020(6) 0.031(6) 0.004(6) C7 0.088(8) 0.088(8) 0.096(8) 0.012(6) 0.026(6) 0.034(6) C8 0.121(9) 0.055(5) 0.069(6) 0.005(4) 0.046(6) 0.014(5) C9 0.103(7) 0.065(5) 0.074(6) -0.015(4) 0.057(5) -0.022(5) C10 0.073(5) 0.055(5) 0.064(5) -0.004(4) 0.028(4) -0.016(4) C11 0.111(8) 0.073(6) 0.082(6) -0.015(5) 0.040(6) -0.024(6) C12 0.097(8) 0.105(8) 0.127(9) -0.013(7) 0.065(7) -0.035(6) C13 0.108(8) 0.065(6) 0.093(7) 0.015(5) 0.039(6) -0.004(5) C16 0.24(2) 0.23(2) 0.28(2) 0.053(17) 0.21(2) 0.129(17) C15 0.098(10) 0.40(3) 0.168(15) -0.087(16) 0.077(11) -0.117(14) C14 0.096(8) 0.137(10) 0.115(9) 0.005(7) 0.070(7) 0.013(7) C17 0.107(10) 0.174(14) 0.122(11) 0.040(10) -0.016(8) 0.027(10) C19 0.119(10) 0.146(11) 0.122(10) 0.009(8) 0.063(9) 0.011(9) C18 0.223(18) 0.061(8) 0.29(2) 0.014(10) 0.155(18) 0.034(9) Li1 0.103(16) 0.060(12) 0.061(11) 0.000 0.041(12) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N3 2.205(7) 2_756 ? Yb1 N3 2.205(7) . ? Yb1 N1 2.275(7) 2_756 ? Yb1 N1 2.275(7) . ? Yb1 C19 3.150(13) 2_756 ? Yb1 C1 3.172(8) 2_756 ? Yb1 Si2 3.187(3) 2_756 ? Yb1 Si1 3.514(3) 2_756 ? Si1 N3 1.678(9) . ? Si1 C16 1.834(15) . ? Si1 C15 1.871(14) . ? Si1 C14 1.889(12) . ? Si2 N3 1.724(9) . ? Si2 C19 1.836(13) . ? Si2 C18 1.848(12) . ? Si2 C17 1.869(12) . ? N1 C4 1.366(10) . ? N1 C1 1.376(10) . ? N2 C9 1.492(10) . ? N2 C10 1.496(10) . ? N2 Li1 2.069(8) . ? N2 H2 0.9099 . ? C1 C2 1.352(11) . ? C1 H1 0.9300 . ? C2 C3 1.419(11) . ? C2 C9 1.496(11) . ? C2 Li1 2.499(13) . ? C3 C8 1.404(12) . ? C3 C4 1.414(10) . ? C3 Li1 2.627(12) . ? C4 C5 1.418(12) . ? C5 C6 1.352(13) . ? C5 H5 0.9300 . ? C6 C7 1.400(15) . ? C6 H6 0.9300 . ? C7 C8 1.349(15) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 Li1 2.749(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C13 1.515(13) . ? C10 C12 1.519(13) . ? C10 C11 1.528(12) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? Li1 N2 2.069(8) 2_756 ? Li1 C2 2.499(13) 2_756 ? Li1 C3 2.627(12) 2_756 ? Li1 C9 2.749(9) 2_756 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Yb1 N3 121.7(4) 2_756 . ? N3 Yb1 N1 111.5(3) 2_756 2_756 ? N3 Yb1 N1 111.1(3) . 2_756 ? N3 Yb1 N1 111.1(2) 2_756 . ? N3 Yb1 N1 111.5(3) . . ? N1 Yb1 N1 83.5(4) 2_756 . ? N3 Yb1 C19 64.5(3) 2_756 2_756 ? N3 Yb1 C19 84.5(3) . 2_756 ? N1 Yb1 C19 161.7(3) 2_756 2_756 ? N1 Yb1 C19 81.8(3) . 2_756 ? N3 Yb1 C1 95.2(3) 2_756 2_756 ? N3 Yb1 C1 133.4(2) . 2_756 ? N1 Yb1 C1 22.4(2) 2_756 2_756 ? N1 Yb1 C1 74.4(2) . 2_756 ? C19 Yb1 C1 140.5(3) 2_756 2_756 ? N3 Yb1 Si2 31.0(2) 2_756 2_756 ? N3 Yb1 Si2 103.49(19) . 2_756 ? N1 Yb1 Si2 141.06(18) 2_756 2_756 ? N1 Yb1 Si2 100.27(18) . 2_756 ? C19 Yb1 Si2 33.7(2) 2_756 2_756 ? C1 Yb1 Si2 121.35(17) 2_756 2_756 ? N3 Yb1 Si1 21.7(2) 2_756 2_756 ? N3 Yb1 Si1 130.4(2) . 2_756 ? N1 Yb1 Si1 90.33(19) 2_756 2_756 ? N1 Yb1 Si1 115.11(18) . 2_756 ? C19 Yb1 Si1 86.1(2) 2_756 2_756 ? C1 Yb1 Si1 76.39(18) 2_756 2_756 ? Si2 Yb1 Si1 52.73(9) 2_756 2_756 ? N3 Si1 C16 113.9(7) . . ? N3 Si1 C15 112.5(6) . . ? C16 Si1 C15 109.2(10) . . ? N3 Si1 C14 116.5(5) . . ? C16 Si1 C14 101.5(7) . . ? C15 Si1 C14 102.0(8) . . ? N3 Si2 C19 112.9(5) . . ? N3 Si2 C18 117.7(7) . . ? C19 Si2 C18 102.5(7) . . ? N3 Si2 C17 115.2(6) . . ? C19 Si2 C17 101.8(7) . . ? C18 Si2 C17 104.9(8) . . ? C4 N1 C1 103.7(6) . . ? C4 N1 Yb1 128.4(6) . . ? C1 N1 Yb1 118.6(5) . . ? C9 N2 C10 114.3(6) . . ? C9 N2 Li1 99.8(6) . . ? C10 N2 Li1 131.1(8) . . ? C9 N2 H2 102.7 . . ? C10 N2 H2 102.9 . . ? Li1 N2 H2 102.5 . . ? Si1 N3 Si2 123.0(4) . . ? Si1 N3 Yb1 129.2(5) . . ? Si2 N3 Yb1 107.8(4) . . ? C2 C1 N1 114.3(8) . . ? C2 C1 H1 122.8 . . ? N1 C1 H1 122.8 . . ? C1 C2 C3 105.2(7) . . ? C1 C2 C9 127.5(8) . . ? C3 C2 C9 127.3(8) . . ? C1 C2 Li1 110.5(7) . . ? C3 C2 Li1 79.0(5) . . ? C9 C2 Li1 82.9(6) . . ? C8 C3 C4 119.5(9) . . ? C8 C3 C2 134.8(8) . . ? C4 C3 C2 105.7(7) . . ? C8 C3 Li1 93.0(6) . . ? C4 C3 Li1 111.8(6) . . ? C2 C3 Li1 69.0(4) . . ? N1 C4 C3 111.1(7) . . ? N1 C4 C5 128.8(7) . . ? C3 C4 C5 120.1(8) . . ? C6 C5 C4 117.9(9) . . ? C6 C5 H5 121.1 . . ? C4 C5 H5 121.1 . . ? C5 C6 C7 122.1(10) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C8 C7 C6 121.3(9) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C3 119.2(9) . . ? C7 C8 H8 120.4 . . ? C3 C8 H8 120.4 . . ? N2 C9 C2 109.2(7) . . ? N2 C9 Li1 47.9(4) . . ? C2 C9 Li1 64.4(6) . . ? N2 C9 H9A 109.8 . . ? C2 C9 H9A 109.8 . . ? Li1 C9 H9A 109.8 . . ? N2 C9 H9B 109.8 . . ? C2 C9 H9B 109.8 . . ? Li1 C9 H9B 141.0 . . ? H9A C9 H9B 108.3 . . ? N2 C10 C13 108.3(7) . . ? N2 C10 C12 112.8(8) . . ? C13 C10 C12 110.4(8) . . ? N2 C10 C11 106.1(7) . . ? C13 C10 C11 110.0(8) . . ? C12 C10 C11 109.0(8) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 Li1 N2 147.7(11) . 2_756 ? N2 Li1 C2 63.6(3) . . ? N2 Li1 C2 138.0(4) 2_756 . ? N2 Li1 C2 138.0(4) . 2_756 ? N2 Li1 C2 63.6(3) 2_756 2_756 ? C2 Li1 C2 114.9(8) . 2_756 ? N2 Li1 C3 90.3(3) . . ? N2 Li1 C3 106.1(3) 2_756 . ? C2 Li1 C3 32.0(3) . . ? C2 Li1 C3 107.5(7) 2_756 . ? N2 Li1 C3 106.1(3) . 2_756 ? N2 Li1 C3 90.3(3) 2_756 2_756 ? C2 Li1 C3 107.5(7) . 2_756 ? C2 Li1 C3 32.0(3) 2_756 2_756 ? C3 Li1 C3 118.9(8) . 2_756 ? N2 Li1 C9 32.3(2) . . ? N2 Li1 C9 152.4(5) 2_756 . ? C2 Li1 C9 32.7(2) . . ? C2 Li1 C9 139.7(8) 2_756 . ? C3 Li1 C9 58.1(3) . . ? C3 Li1 C9 117.0(5) 2_756 . ? N2 Li1 C9 152.4(5) . 2_756 ? N2 Li1 C9 32.3(2) 2_756 2_756 ? C2 Li1 C9 139.7(8) . 2_756 ? C2 Li1 C9 32.7(2) 2_756 2_756 ? C3 Li1 C9 117.0(5) . 2_756 ? C3 Li1 C9 58.1(3) 2_756 2_756 ? C9 Li1 C9 171.5(9) . 2_756 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Yb1 N1 C4 -34.1(8) 2_756 . . . ? N3 Yb1 N1 C4 -173.4(7) . . . . ? N1 Yb1 N1 C4 76.4(7) 2_756 . . . ? C19 Yb1 N1 C4 -92.7(7) 2_756 . . . ? C1 Yb1 N1 C4 55.5(7) 2_756 . . . ? Si2 Yb1 N1 C4 -64.4(7) 2_756 . . . ? Si1 Yb1 N1 C4 -10.9(8) 2_756 . . . ? N3 Yb1 N1 C1 -175.0(6) 2_756 . . . ? N3 Yb1 N1 C1 45.8(7) . . . . ? N1 Yb1 N1 C1 -64.4(6) 2_756 . . . ? C19 Yb1 N1 C1 126.5(7) 2_756 . . . ? C1 Yb1 N1 C1 -85.3(7) 2_756 . . . ? Si2 Yb1 N1 C1 154.8(6) 2_756 . . . ? Si1 Yb1 N1 C1 -151.7(6) 2_756 . . . ? C16 Si1 N3 Si2 -42.9(9) . . . . ? C15 Si1 N3 Si2 82.1(9) . . . . ? C14 Si1 N3 Si2 -160.7(6) . . . . ? C16 Si1 N3 Yb1 138.0(8) . . . . ? C15 Si1 N3 Yb1 -97.0(9) . . . . ? C14 Si1 N3 Yb1 20.3(8) . . . . ? C19 Si2 N3 Si1 -171.0(6) . . . . ? C18 Si2 N3 Si1 69.9(8) . . . . ? C17 Si2 N3 Si1 -54.7(8) . . . . ? C19 Si2 N3 Yb1 8.2(6) . . . . ? C18 Si2 N3 Yb1 -110.9(7) . . . . ? C17 Si2 N3 Yb1 124.6(6) . . . . ? N3 Yb1 N3 Si1 -120.5(5) 2_756 . . . ? N1 Yb1 N3 Si1 105.0(5) 2_756 . . . ? N1 Yb1 N3 Si1 13.8(6) . . . . ? C19 Yb1 N3 Si1 -65.2(5) 2_756 . . . ? C1 Yb1 N3 Si1 102.4(5) 2_756 . . . ? Si2 Yb1 N3 Si1 -93.2(5) 2_756 . . . ? Si1 Yb1 N3 Si1 -145.3(4) 2_756 . . . ? N3 Yb1 N3 Si2 60.3(3) 2_756 . . . ? N1 Yb1 N3 Si2 -74.2(4) 2_756 . . . ? N1 Yb1 N3 Si2 -165.4(3) . . . . ? C19 Yb1 N3 Si2 115.7(4) 2_756 . . . ? C1 Yb1 N3 Si2 -76.8(5) 2_756 . . . ? Si2 Yb1 N3 Si2 87.7(3) 2_756 . . . ? Si1 Yb1 N3 Si2 35.5(5) 2_756 . . . ? C4 N1 C1 C2 0.2(10) . . . . ? Yb1 N1 C1 C2 149.6(6) . . . . ? N1 C1 C2 C3 0.3(10) . . . . ? N1 C1 C2 C9 179.8(8) . . . . ? N1 C1 C2 Li1 -83.4(8) . . . . ? C1 C2 C3 C8 179.2(9) . . . . ? C9 C2 C3 C8 -0.3(15) . . . . ? Li1 C2 C3 C8 -72.4(10) . . . . ? C1 C2 C3 C4 -0.6(9) . . . . ? C9 C2 C3 C4 179.9(7) . . . . ? Li1 C2 C3 C4 107.8(7) . . . . ? C1 C2 C3 Li1 -108.4(7) . . . . ? C9 C2 C3 Li1 72.1(9) . . . . ? C1 N1 C4 C3 -0.6(9) . . . . ? Yb1 N1 C4 C3 -145.8(6) . . . . ? C1 N1 C4 C5 177.9(9) . . . . ? Yb1 N1 C4 C5 32.7(13) . . . . ? C8 C3 C4 N1 -179.1(8) . . . . ? C2 C3 C4 N1 0.8(9) . . . . ? Li1 C3 C4 N1 74.0(8) . . . . ? C8 C3 C4 C5 2.3(12) . . . . ? C2 C3 C4 C5 -177.8(8) . . . . ? Li1 C3 C4 C5 -104.6(8) . . . . ? N1 C4 C5 C6 -178.8(10) . . . . ? C3 C4 C5 C6 -0.4(14) . . . . ? C4 C5 C6 C7 -1.5(17) . . . . ? C5 C6 C7 C8 1.5(19) . . . . ? C6 C7 C8 C3 0.4(17) . . . . ? C4 C3 C8 C7 -2.2(13) . . . . ? C2 C3 C8 C7 177.9(10) . . . . ? Li1 C3 C8 C7 114.9(9) . . . . ? C10 N2 C9 C2 165.4(7) . . . . ? Li1 N2 C9 C2 21.4(9) . . . . ? C10 N2 C9 Li1 144.0(9) . . . . ? C1 C2 C9 N2 92.9(11) . . . . ? C3 C2 C9 N2 -87.7(10) . . . . ? Li1 C2 C9 N2 -17.4(7) . . . . ? C1 C2 C9 Li1 110.4(9) . . . . ? C3 C2 C9 Li1 -70.3(8) . . . . ? C9 N2 C10 C13 -75.9(10) . . . . ? Li1 N2 C10 C13 53.9(10) . . . . ? C9 N2 C10 C12 46.7(10) . . . . ? Li1 N2 C10 C12 176.5(6) . . . . ? C9 N2 C10 C11 166.0(8) . . . . ? Li1 N2 C10 C11 -64.2(9) . . . . ? C9 N2 Li1 N2 126.9(5) . . . 2_756 ? C10 N2 Li1 N2 -7.8(6) . . . 2_756 ? C9 N2 Li1 C2 -13.3(5) . . . . ? C10 N2 Li1 C2 -148.0(7) . . . . ? C9 N2 Li1 C2 -112.0(11) . . . 2_756 ? C10 N2 Li1 C2 113.3(13) . . . 2_756 ? C9 N2 Li1 C3 5.1(7) . . . . ? C10 N2 Li1 C3 -129.6(7) . . . . ? C9 N2 Li1 C3 -115.2(7) . . . 2_756 ? C10 N2 Li1 C3 110.1(9) . . . 2_756 ? C10 N2 Li1 C9 -134.7(9) . . . . ? C9 N2 Li1 C9 -165.9(17) . . . 2_756 ? C10 N2 Li1 C9 59(2) . . . 2_756 ? C1 C2 Li1 N2 -114.3(7) . . . . ? C3 C2 Li1 N2 143.5(6) . . . . ? C9 C2 Li1 N2 13.2(5) . . . . ? C1 C2 Li1 N2 96.4(12) . . . 2_756 ? C3 C2 Li1 N2 -5.8(12) . . . 2_756 ? C9 C2 Li1 N2 -136.1(12) . . . 2_756 ? C1 C2 Li1 C2 18.9(5) . . . 2_756 ? C3 C2 Li1 C2 -83.3(4) . . . 2_756 ? C9 C2 Li1 C2 146.4(6) . . . 2_756 ? C1 C2 Li1 C3 102.2(8) . . . . ? C9 C2 Li1 C3 -130.3(7) . . . . ? C1 C2 Li1 C3 -14.6(7) . . . 2_756 ? C3 C2 Li1 C3 -116.8(6) . . . 2_756 ? C9 C2 Li1 C3 112.9(6) . . . 2_756 ? C1 C2 Li1 C9 -127.5(9) . . . . ? C3 C2 Li1 C9 130.3(7) . . . . ? C1 C2 Li1 C9 46.4(9) . . . 2_756 ? C3 C2 Li1 C9 -55.8(7) . . . 2_756 ? C9 C2 Li1 C9 173.9(6) . . . 2_756 ? C8 C3 Li1 N2 105.2(8) . . . . ? C4 C3 Li1 N2 -131.3(7) . . . . ? C2 C3 Li1 N2 -32.2(6) . . . . ? C8 C3 Li1 N2 -46.6(9) . . . 2_756 ? C4 C3 Li1 N2 76.9(9) . . . 2_756 ? C2 C3 Li1 N2 176.0(9) . . . 2_756 ? C8 C3 Li1 C2 137.4(8) . . . . ? C4 C3 Li1 C2 -99.1(8) . . . . ? C8 C3 Li1 C2 -113.5(7) . . . 2_756 ? C4 C3 Li1 C2 10.1(7) . . . 2_756 ? C2 C3 Li1 C2 109.2(7) . . . 2_756 ? C8 C3 Li1 C3 -146.2(7) . . . 2_756 ? C4 C3 Li1 C3 -22.7(5) . . . 2_756 ? C2 C3 Li1 C3 76.4(5) . . . 2_756 ? C8 C3 Li1 C9 108.4(7) . . . . ? C4 C3 Li1 C9 -128.1(7) . . . . ? C2 C3 Li1 C9 -29.0(5) . . . . ? C8 C3 Li1 C9 -79.5(8) . . . 2_756 ? C4 C3 Li1 C9 44.0(9) . . . 2_756 ? C2 C3 Li1 C9 143.1(8) . . . 2_756 ? C2 C9 Li1 N2 -157.6(9) . . . . ? N2 C9 Li1 N2 -113(2) . . . 2_756 ? C2 C9 Li1 N2 89.5(18) . . . 2_756 ? N2 C9 Li1 C2 157.6(9) . . . . ? N2 C9 Li1 C2 106.7(6) . . . 2_756 ? C2 C9 Li1 C2 -50.9(10) . . . 2_756 ? N2 C9 Li1 C3 -174.0(8) . . . . ? C2 C9 Li1 C3 28.4(5) . . . . ? N2 C9 Li1 C3 77.2(6) . . . 2_756 ? C2 C9 Li1 C3 -80.3(8) . . . 2_756 ? N2 C9 Li1 C9 129.7(6) . . . 2_756 ? C2 C9 Li1 C9 -27.9(5) . . . 2_756 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.64 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.063 _refine_diff_density_min -1.036 _refine_diff_density_rms 0.130 # Attachment '- 110817a_0m.cif' data_110817a_0m _database_code_depnum_ccdc_archive 'CCDC 842362' #TrackingRef '- 110817a_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H70 Li N6 Si4 Y' _chemical_formula_weight 819.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 12.431(2) _cell_length_b 15.176(3) _cell_length_c 15.3466(17) _cell_angle_alpha 90.00 _cell_angle_beta 124.166(9) _cell_angle_gamma 90.00 _cell_volume 2395.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 1.348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7041 _exptl_absorpt_correction_T_max 0.7650 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20090 _diffrn_reflns_av_R_equivalents 0.1383 _diffrn_reflns_av_sigmaI/netI 0.1691 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.52 _reflns_number_total 5483 _reflns_number_gt 2306 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+1.0000P] 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 5483 _refine_ls_number_parameters 240 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1974 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.0870 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.173 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 1.0000 0.26362(4) 0.7500 0.0451(2) Uani 1 2 d S . . Si1 Si 0.71852(14) 0.33502(11) 0.73885(12) 0.0757(5) Uani 1 1 d U . . Si2 Si 0.77530(15) 0.40131(9) 0.58640(11) 0.0654(5) Uani 1 1 d . . . N1 N 1.0330(4) 0.1505(2) 0.8628(3) 0.0591(11) Uani 1 1 d . . . N2 N 0.8471(4) -0.1157(3) 0.7595(3) 0.0545(11) Uani 1 1 d . . . N3 N 0.8158(3) 0.3371(2) 0.6928(3) 0.0486(10) Uani 1 1 d . . . C1 C 0.9316(5) 0.0947(4) 0.8354(4) 0.0647(15) Uani 1 1 d . . . H1 H 0.8455 0.1135 0.7958 0.078 Uiso 1 1 calc R . . C2 C 0.9646(5) 0.0115(3) 0.8694(4) 0.0531(13) Uani 1 1 d . . . C3 C 1.1036(6) 0.0102(3) 0.9261(4) 0.0530(14) Uani 1 1 d . . . C4 C 1.1411(5) 0.0964(3) 0.9184(3) 0.0488(12) Uani 1 1 d . . . C5 C 1.2714(6) 0.1187(4) 0.9655(4) 0.0739(16) Uani 1 1 d . . . H5 H 1.2962 0.1757 0.9620 0.089 Uiso 1 1 calc R . . C6 C 1.3607(6) 0.0533(5) 1.0169(5) 0.0902(19) Uani 1 1 d . . . H6 H 1.4478 0.0657 1.0457 0.108 Uiso 1 1 calc R . . C7 C 1.3271(7) -0.0307(5) 1.0279(5) 0.094(2) Uani 1 1 d . . . H7 H 1.3917 -0.0726 1.0660 0.112 Uiso 1 1 calc R . . C8 C 1.1996(7) -0.0529(3) 0.9832(4) 0.0731(17) Uani 1 1 d . . . H8 H 1.1774 -0.1095 0.9910 0.088 Uiso 1 1 calc R . . C9 C 0.8802(5) -0.0645(3) 0.8536(4) 0.0722(16) Uani 1 1 d . . . H9A H 0.9249 -0.1022 0.9153 0.087 Uiso 1 1 calc R . . H9B H 0.8011 -0.0433 0.8449 0.087 Uiso 1 1 calc R . . C10 C 0.7886(5) -0.2042(3) 0.7488(4) 0.0632(15) Uani 1 1 d . . . C11 C 0.7347(5) -0.2356(3) 0.6384(4) 0.0915(18) Uani 1 1 d . . . H11A H 0.6741 -0.1930 0.5888 0.137 Uiso 1 1 calc R . . H11B H 0.6913 -0.2910 0.6268 0.137 Uiso 1 1 calc R . . H11C H 0.8045 -0.2429 0.6292 0.137 Uiso 1 1 calc R . . C12 C 0.6804(6) -0.2020(4) 0.7671(4) 0.105(2) Uani 1 1 d . . . H12A H 0.7149 -0.1827 0.8377 0.157 Uiso 1 1 calc R . . H12B H 0.6441 -0.2599 0.7569 0.157 Uiso 1 1 calc R . . H12C H 0.6137 -0.1619 0.7181 0.157 Uiso 1 1 calc R . . C13 C 0.8964(5) -0.2660(3) 0.8280(4) 0.0915(18) Uani 1 1 d . . . H13A H 0.9619 -0.2700 0.8134 0.137 Uiso 1 1 calc R . . H13B H 0.8608 -0.3234 0.8226 0.137 Uiso 1 1 calc R . . H13C H 0.9345 -0.2435 0.8979 0.137 Uiso 1 1 calc R . . C16 C 0.6619(7) 0.4445(4) 0.7473(6) 0.173(3) Uani 1 1 d U . . H16A H 0.7338 0.4848 0.7802 0.259 Uiso 1 1 calc R . . H16B H 0.6255 0.4408 0.7883 0.259 Uiso 1 1 calc R . . H16C H 0.5967 0.4651 0.6777 0.259 Uiso 1 1 calc R . . C15 C 0.5761(6) 0.2629(5) 0.6576(5) 0.171(3) Uani 1 1 d U . . H15A H 0.5063 0.2965 0.6008 0.257 Uiso 1 1 calc R . . H15B H 0.5488 0.2392 0.7002 0.257 Uiso 1 1 calc R . . H15C H 0.5990 0.2156 0.6294 0.257 Uiso 1 1 calc R . . C14 C 0.7977(5) 0.2914(4) 0.8736(4) 0.0986(19) Uani 1 1 d U . . H14A H 0.8494 0.2410 0.8820 0.148 Uiso 1 1 calc R . . H14B H 0.7325 0.2745 0.8855 0.148 Uiso 1 1 calc R . . H14C H 0.8524 0.3360 0.9234 0.148 Uiso 1 1 calc R . . C17 C 0.6092(5) 0.3802(4) 0.4655(4) 0.122(2) Uani 1 1 d . . . H17A H 0.5943 0.3178 0.4556 0.183 Uiso 1 1 calc R . . H17B H 0.6031 0.4051 0.4054 0.183 Uiso 1 1 calc R . . H17C H 0.5452 0.4067 0.4735 0.183 Uiso 1 1 calc R . . C19 C 0.8910(5) 0.3760(3) 0.5494(4) 0.0858(18) Uani 1 1 d . . . H19A H 0.9779 0.3896 0.6074 0.129 Uiso 1 1 calc R . . H19B H 0.8696 0.4108 0.4894 0.129 Uiso 1 1 calc R . . H19C H 0.8854 0.3146 0.5323 0.129 Uiso 1 1 calc R . . C18 C 0.7892(6) 0.5212(3) 0.6103(5) 0.125(2) Uani 1 1 d . . . H18A H 0.7321 0.5387 0.6308 0.187 Uiso 1 1 calc R . . H18B H 0.7654 0.5518 0.5471 0.187 Uiso 1 1 calc R . . H18C H 0.8772 0.5357 0.6656 0.187 Uiso 1 1 calc R . . Li1 Li 1.0000 -0.0796(7) 0.7500 0.065(3) Uani 1 2 d S . . H2 H 0.774(4) -0.082(3) 0.699(3) 0.079(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0426(4) 0.0348(4) 0.0567(4) 0.000 0.0271(3) 0.000 Si1 0.0517(10) 0.1084(14) 0.0694(11) -0.0051(9) 0.0355(9) 0.0128(9) Si2 0.0651(11) 0.0585(10) 0.0676(10) 0.0103(8) 0.0341(9) 0.0195(8) N1 0.061(3) 0.044(3) 0.071(3) 0.000(2) 0.036(3) -0.002(2) N2 0.073(3) 0.047(3) 0.047(3) -0.008(2) 0.036(3) -0.013(2) N3 0.045(2) 0.050(2) 0.056(2) -0.006(2) 0.032(2) 0.0031(19) C1 0.068(4) 0.067(4) 0.060(3) 0.001(3) 0.036(3) -0.011(3) C2 0.082(4) 0.041(3) 0.049(3) -0.006(3) 0.045(3) -0.018(3) C3 0.092(4) 0.036(3) 0.038(3) -0.001(2) 0.041(3) 0.001(3) C4 0.061(4) 0.050(3) 0.043(3) -0.005(3) 0.033(3) -0.002(3) C5 0.076(4) 0.059(4) 0.081(4) -0.016(3) 0.041(4) -0.011(4) C6 0.064(4) 0.091(5) 0.100(5) -0.016(4) 0.036(4) 0.000(4) C7 0.099(6) 0.077(5) 0.083(5) 0.010(4) 0.038(4) 0.032(4) C8 0.113(5) 0.049(4) 0.068(4) 0.002(3) 0.058(4) 0.008(4) C9 0.109(5) 0.059(4) 0.063(4) -0.021(3) 0.057(4) -0.031(3) C10 0.080(4) 0.051(3) 0.059(4) -0.005(3) 0.039(3) -0.020(3) C11 0.120(5) 0.075(4) 0.059(4) -0.022(3) 0.038(3) -0.031(4) C12 0.113(5) 0.103(5) 0.117(5) -0.018(4) 0.075(5) -0.039(4) C13 0.111(4) 0.060(4) 0.081(4) 0.014(3) 0.040(4) -0.010(4) C16 0.223(7) 0.176(5) 0.186(6) 0.048(4) 0.156(6) 0.108(5) C15 0.108(5) 0.303(7) 0.135(5) -0.056(5) 0.088(4) -0.072(5) C14 0.091(4) 0.124(5) 0.110(4) 0.017(3) 0.074(3) 0.009(3) C17 0.069(4) 0.147(6) 0.101(5) 0.047(4) 0.017(4) 0.016(4) C19 0.107(5) 0.097(4) 0.073(4) 0.023(3) 0.062(4) 0.030(4) C18 0.185(7) 0.064(4) 0.162(7) 0.017(4) 0.120(6) 0.029(4) Li1 0.098(10) 0.056(8) 0.060(8) 0.000 0.055(8) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N3 2.236(3) 2_756 ? Y1 N3 2.236(3) . ? Y1 N1 2.306(4) 2_756 ? Y1 N1 2.306(4) . ? Y1 Si2 3.2551(15) 2_756 ? Si1 N3 1.710(4) . ? Si1 C16 1.837(6) . ? Si1 C14 1.842(5) . ? Si1 C15 1.846(6) . ? Si2 N3 1.716(4) . ? Si2 C18 1.846(5) . ? Si2 C19 1.859(5) . ? Si2 C17 1.872(5) . ? N1 C1 1.373(5) . ? N1 C4 1.385(5) . ? N2 C9 1.480(5) . ? N2 C10 1.492(5) . ? N2 Li1 2.061(5) . ? N2 H2 1.00(4) . ? C1 C2 1.340(6) . ? C1 H1 0.9300 . ? C2 C3 1.434(6) . ? C2 C9 1.484(6) . ? C3 C8 1.390(6) . ? C3 C4 1.416(6) . ? C3 Li1 2.629(7) . ? C4 C5 1.395(6) . ? C5 C6 1.362(7) . ? C5 H5 0.9300 . ? C6 C7 1.381(7) . ? C6 H6 0.9300 . ? C7 C8 1.370(7) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.507(6) . ? C10 C13 1.524(6) . ? C10 C12 1.522(6) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? Li1 N2 2.061(5) 2_756 ? Li1 C2 2.523(8) 2_756 ? Li1 C3 2.629(7) 2_756 ? Li1 C9 2.731(5) 2_756 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Y1 N3 120.16(17) 2_756 . ? N3 Y1 N1 112.16(14) 2_756 2_756 ? N3 Y1 N1 111.45(14) . 2_756 ? N3 Y1 N1 111.45(13) 2_756 . ? N3 Y1 N1 112.16(14) . . ? N1 Y1 N1 83.75(18) 2_756 . ? N3 Y1 Si2 29.66(9) 2_756 2_756 ? N3 Y1 Si2 103.21(9) . 2_756 ? N1 Y1 Si2 140.43(11) 2_756 2_756 ? N1 Y1 Si2 100.67(10) . 2_756 ? N3 Si1 C16 113.6(3) . . ? N3 Si1 C14 114.5(2) . . ? C16 Si1 C14 103.3(3) . . ? N3 Si1 C15 111.4(2) . . ? C16 Si1 C15 108.9(4) . . ? C14 Si1 C15 104.5(3) . . ? N3 Si2 C18 115.2(2) . . ? N3 Si2 C19 108.0(2) . . ? C18 Si2 C19 105.2(3) . . ? N3 Si2 C17 114.6(2) . . ? C18 Si2 C17 107.1(3) . . ? C19 Si2 C17 105.9(3) . . ? C1 N1 C4 103.3(4) . . ? C1 N1 Y1 118.9(3) . . ? C4 N1 Y1 127.3(3) . . ? C9 N2 C10 115.6(4) . . ? C9 N2 Li1 99.7(3) . . ? C10 N2 Li1 130.0(4) . . ? C9 N2 H2 105(3) . . ? C10 N2 H2 103(2) . . ? Li1 N2 H2 101(3) . . ? Si1 N3 Si2 120.4(2) . . ? Si1 N3 Y1 129.39(19) . . ? Si2 N3 Y1 110.20(17) . . ? C2 C1 N1 115.7(5) . . ? C2 C1 H1 122.1 . . ? N1 C1 H1 122.1 . . ? C1 C2 C3 104.5(4) . . ? C1 C2 C9 129.4(5) . . ? C3 C2 C9 126.1(5) . . ? C8 C3 C4 118.9(5) . . ? C8 C3 C2 135.0(5) . . ? C4 C3 C2 106.1(5) . . ? C8 C3 Li1 92.5(4) . . ? C4 C3 Li1 112.8(3) . . ? C2 C3 Li1 69.8(3) . . ? N1 C4 C5 128.2(5) . . ? N1 C4 C3 110.4(5) . . ? C5 C4 C3 121.4(5) . . ? C6 C5 C4 117.1(5) . . ? C6 C5 H5 121.5 . . ? C4 C5 H5 121.5 . . ? C5 C6 C7 122.6(6) . . ? C5 C6 H6 118.7 . . ? C7 C6 H6 118.7 . . ? C8 C7 C6 120.7(6) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C3 119.2(6) . . ? C7 C8 H8 120.4 . . ? C3 C8 H8 120.4 . . ? N2 C9 C2 110.5(4) . . ? N2 C9 H9A 109.5 . . ? C2 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? C2 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? N2 C10 C11 106.9(4) . . ? N2 C10 C13 108.1(4) . . ? C11 C10 C13 109.8(4) . . ? N2 C10 C12 112.7(4) . . ? C11 C10 C12 109.5(4) . . ? C13 C10 C12 109.8(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 Li1 N2 149.2(6) . 2_756 ? N2 Li1 C2 137.8(3) . 2_756 ? N2 Li1 C2 63.24(17) 2_756 2_756 ? N2 Li1 C3 90.20(18) . . ? N2 Li1 C3 105.8(2) 2_756 . ? C2 Li1 C3 106.2(4) 2_756 . ? N2 Li1 C3 105.8(2) . 2_756 ? N2 Li1 C3 90.20(18) 2_756 2_756 ? C2 Li1 C3 32.24(16) 2_756 2_756 ? C3 Li1 C3 117.6(5) . 2_756 ? N2 Li1 C9 152.9(3) . 2_756 ? N2 Li1 C9 32.29(13) 2_756 2_756 ? C2 Li1 C9 32.50(13) 2_756 2_756 ? C3 Li1 C9 116.3(3) . 2_756 ? C3 Li1 C9 58.02(17) 2_756 2_756 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Y1 N1 C1 -175.4(3) 2_756 . . . ? N3 Y1 N1 C1 46.7(4) . . . . ? N1 Y1 N1 C1 -64.0(3) 2_756 . . . ? Si2 Y1 N1 C1 155.8(3) 2_756 . . . ? N3 Y1 N1 C4 -36.8(4) 2_756 . . . ? N3 Y1 N1 C4 -174.8(3) . . . . ? N1 Y1 N1 C4 74.6(4) 2_756 . . . ? Si2 Y1 N1 C4 -65.7(4) 2_756 . . . ? C16 Si1 N3 Si2 -44.0(4) . . . . ? C14 Si1 N3 Si2 -162.4(2) . . . . ? C15 Si1 N3 Si2 79.4(4) . . . . ? C16 Si1 N3 Y1 137.0(3) . . . . ? C14 Si1 N3 Y1 18.6(3) . . . . ? C15 Si1 N3 Y1 -99.6(3) . . . . ? C18 Si2 N3 Si1 69.7(3) . . . . ? C19 Si2 N3 Si1 -173.0(2) . . . . ? C17 Si2 N3 Si1 -55.3(3) . . . . ? C18 Si2 N3 Y1 -111.1(3) . . . . ? C19 Si2 N3 Y1 6.1(3) . . . . ? C17 Si2 N3 Y1 123.9(2) . . . . ? N3 Y1 N3 Si1 -120.0(2) 2_756 . . . ? N1 Y1 N3 Si1 105.8(2) 2_756 . . . ? N1 Y1 N3 Si1 13.9(3) . . . . ? Si2 Y1 N3 Si1 -93.6(2) 2_756 . . . ? N3 Y1 N3 Si2 60.91(14) 2_756 . . . ? N1 Y1 N3 Si2 -73.3(2) 2_756 . . . ? N1 Y1 N3 Si2 -165.21(16) . . . . ? Si2 Y1 N3 Si2 87.27(16) 2_756 . . . ? C4 N1 C1 C2 1.1(5) . . . . ? Y1 N1 C1 C2 148.3(3) . . . . ? N1 C1 C2 C3 -0.1(6) . . . . ? N1 C1 C2 C9 -179.8(4) . . . . ? C1 C2 C3 C8 177.8(5) . . . . ? C9 C2 C3 C8 -2.5(8) . . . . ? C1 C2 C3 C4 -1.0(5) . . . . ? C9 C2 C3 C4 178.8(4) . . . . ? C1 C2 C3 Li1 -109.8(4) . . . . ? C9 C2 C3 Li1 69.9(5) . . . . ? C1 N1 C4 C5 -179.7(5) . . . . ? Y1 N1 C4 C5 36.9(7) . . . . ? C1 N1 C4 C3 -1.6(5) . . . . ? Y1 N1 C4 C3 -145.1(3) . . . . ? C8 C3 C4 N1 -177.3(4) . . . . ? C2 C3 C4 N1 1.7(5) . . . . ? Li1 C3 C4 N1 76.1(4) . . . . ? C8 C3 C4 C5 0.9(7) . . . . ? C2 C3 C4 C5 179.9(4) . . . . ? Li1 C3 C4 C5 -105.7(5) . . . . ? N1 C4 C5 C6 179.5(5) . . . . ? C3 C4 C5 C6 1.7(7) . . . . ? C4 C5 C6 C7 -3.4(9) . . . . ? C5 C6 C7 C8 2.6(10) . . . . ? C6 C7 C8 C3 0.2(9) . . . . ? C4 C3 C8 C7 -1.8(7) . . . . ? C2 C3 C8 C7 179.6(5) . . . . ? Li1 C3 C8 C7 116.0(5) . . . . ? C10 N2 C9 C2 166.7(4) . . . . ? Li1 N2 C9 C2 23.1(5) . . . . ? C1 C2 C9 N2 92.8(6) . . . . ? C3 C2 C9 N2 -86.9(6) . . . . ? C9 N2 C10 C11 167.3(4) . . . . ? Li1 N2 C10 C11 -62.6(6) . . . . ? C9 N2 C10 C13 -74.6(6) . . . . ? Li1 N2 C10 C13 55.5(5) . . . . ? C9 N2 C10 C12 46.9(6) . . . . ? Li1 N2 C10 C12 177.1(3) . . . . ? C9 N2 Li1 N2 126.8(3) . . . 2_756 ? C10 N2 Li1 N2 -8.8(4) . . . 2_756 ? C9 N2 Li1 C2 -110.4(6) . . . 2_756 ? C10 N2 Li1 C2 114.0(8) . . . 2_756 ? C9 N2 Li1 C3 4.4(4) . . . . ? C10 N2 Li1 C3 -131.3(4) . . . . ? C9 N2 Li1 C3 -114.5(4) . . . 2_756 ? C10 N2 Li1 C3 109.9(5) . . . 2_756 ? C9 N2 Li1 C9 -163.5(10) . . . 2_756 ? C10 N2 Li1 C9 60.9(12) . . . 2_756 ? C8 C3 Li1 N2 105.7(4) . . . . ? C4 C3 Li1 N2 -131.4(5) . . . . ? C2 C3 Li1 N2 -31.8(4) . . . . ? C8 C3 Li1 N2 -47.6(5) . . . 2_756 ? C4 C3 Li1 N2 75.3(6) . . . 2_756 ? C2 C3 Li1 N2 174.8(5) . . . 2_756 ? C8 C3 Li1 C2 -113.7(4) . . . 2_756 ? C4 C3 Li1 C2 9.2(4) . . . 2_756 ? C2 C3 Li1 C2 108.8(4) . . . 2_756 ? C8 C3 Li1 C3 -146.3(4) . . . 2_756 ? C4 C3 Li1 C3 -23.4(3) . . . 2_756 ? C2 C3 Li1 C3 76.1(3) . . . 2_756 ? C8 C3 Li1 C9 -80.4(5) . . . 2_756 ? C4 C3 Li1 C9 42.5(6) . . . 2_756 ? C2 C3 Li1 C9 142.0(5) . . . 2_756 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.413 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.067 data_111024b_0m _database_code_depnum_ccdc_archive 'CCDC 896821' #TrackingRef '111024b_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H81 N6 O2 Yb' _chemical_formula_weight 1079.34 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9972(8) _cell_length_b 13.3074(9) _cell_length_c 21.3606(15) _cell_angle_alpha 105.7870(10) _cell_angle_beta 102.5530(10) _cell_angle_gamma 92.6190(10) _cell_volume 3183.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9901 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.29 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.126 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1126 _exptl_absorpt_coefficient_mu 1.509 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7523 _exptl_absorpt_correction_T_max 0.7729 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14509 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.79 _reflns_number_total 14509 _reflns_number_gt 12382 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+0.5000P] 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 14509 _refine_ls_number_parameters 646 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0741(3) 0.3905(3) 0.32594(17) 0.0542(7) Uani 1 1 d . . . H1 H 0.0363 0.3517 0.2826 0.065 Uiso 1 1 calc R . . C2 C 0.0563(3) 0.3676(3) 0.38171(17) 0.0543(7) Uani 1 1 d . . . C3 C 0.1308(3) 0.4442(3) 0.43739(17) 0.0575(8) Uani 1 1 d . . . C4 C 0.1900(3) 0.5087(3) 0.40954(16) 0.0538(7) Uani 1 1 d . . . C5 C 0.2737(4) 0.5905(3) 0.45004(19) 0.0708(10) Uani 1 1 d . . . H5 H 0.3127 0.6321 0.4313 0.085 Uiso 1 1 calc R . . C6 C 0.2968(4) 0.6078(4) 0.5180(2) 0.0928(14) Uani 1 1 d . . . H6 H 0.3537 0.6607 0.5457 0.111 Uiso 1 1 calc R . . C7 C 0.2366(5) 0.5476(4) 0.5460(2) 0.1059(17) Uani 1 1 d . . . H7 H 0.2520 0.5627 0.5924 0.127 Uiso 1 1 calc R . . C8 C 0.1543(4) 0.4658(4) 0.5070(2) 0.0875(13) Uani 1 1 d . . . H8 H 0.1153 0.4258 0.5266 0.105 Uiso 1 1 calc R . . C9 C -0.0182(3) 0.2800(3) 0.3833(2) 0.0670(10) Uani 1 1 d . . . H9 H -0.0263 0.2742 0.4246 0.080 Uiso 1 1 calc R . . C10 C -0.1475(4) 0.1234(3) 0.3349(3) 0.0812(12) Uani 1 1 d . . . C11 C -0.2703(4) 0.1449(5) 0.3126(4) 0.125(2) Uani 1 1 d . . . H11A H -0.2861 0.2047 0.3451 0.188 Uiso 1 1 calc R . . H11B H -0.3216 0.0847 0.3084 0.188 Uiso 1 1 calc R . . H11C H -0.2812 0.1592 0.2701 0.188 Uiso 1 1 calc R . . C12 C -0.1253(6) 0.0286(4) 0.2846(4) 0.148(3) Uani 1 1 d . . . H12A H -0.1406 0.0401 0.2412 0.223 Uiso 1 1 calc R . . H12B H -0.1745 -0.0314 0.2831 0.223 Uiso 1 1 calc R . . H12C H -0.0464 0.0162 0.2971 0.223 Uiso 1 1 calc R . . C13 C -0.1285(6) 0.1046(6) 0.4032(4) 0.151(3) Uani 1 1 d . . . H13A H -0.0490 0.0963 0.4187 0.227 Uiso 1 1 calc R . . H13B H -0.1754 0.0420 0.3999 0.227 Uiso 1 1 calc R . . H13C H -0.1489 0.1634 0.4344 0.227 Uiso 1 1 calc R . . C14 C 0.3514(3) 0.6933(3) 0.2126(2) 0.0694(10) Uani 1 1 d . A . H14 H 0.2862 0.6851 0.1781 0.083 Uiso 1 1 calc R . . C15 C 0.4455(4) 0.7605(3) 0.2223(2) 0.0769(12) Uani 1 1 d . . . C16 C 0.5257(3) 0.7505(3) 0.2797(2) 0.0692(10) Uani 1 1 d . A . C17 C 0.4712(3) 0.6749(3) 0.30089(18) 0.0567(8) Uani 1 1 d . . . C18 C 0.5262(3) 0.6444(3) 0.3557(2) 0.0719(10) Uani 1 1 d . A . H18 H 0.4900 0.5942 0.3697 0.086 Uiso 1 1 calc R . . C19 C 0.6348(4) 0.6898(5) 0.3885(3) 0.1051(18) Uani 1 1 d . . . H19 H 0.6722 0.6692 0.4252 0.126 Uiso 1 1 calc R A . C20 C 0.6906(5) 0.7637(6) 0.3700(4) 0.138(3) Uani 1 1 d . A . H20 H 0.7646 0.7931 0.3941 0.166 Uiso 1 1 calc R . . C21 C 0.6386(5) 0.7948(4) 0.3165(4) 0.114(2) Uani 1 1 d . . . H21 H 0.6770 0.8455 0.3038 0.137 Uiso 1 1 calc R A . C22 C 0.4785(8) 0.8346(6) 0.1886(4) 0.057(2) Uani 0.599(16) 1 d P A 1 H22 H 0.5483 0.8771 0.2046 0.068 Uiso 0.599(16) 1 calc PR A 1 C22' C 0.4190(16) 0.8166(13) 0.1606(8) 0.064(3) Uani 0.401(16) 1 d P A 2 H22' H 0.3519 0.8000 0.1267 0.077 Uiso 0.401(16) 1 calc PR A 2 C23 C 0.4521(8) 0.9226(6) 0.1046(4) 0.132(3) Uani 1 1 d . . . C24 C 0.5750(10) 0.9625(9) 0.1126(6) 0.222(5) Uani 1 1 d . A . H24A H 0.5775 1.0229 0.0964 0.333 Uiso 1 1 calc R . . H24B H 0.6116 0.9085 0.0874 0.333 Uiso 1 1 calc R . . H24C H 0.6144 0.9815 0.1591 0.333 Uiso 1 1 calc R . . C25 C 0.4182(12) 0.8565(9) 0.0356(5) 0.283(7) Uani 1 1 d . A . H25A H 0.3500 0.8786 0.0126 0.424 Uiso 1 1 calc R . . H25B H 0.4033 0.7847 0.0348 0.424 Uiso 1 1 calc R . . H25C H 0.4790 0.8628 0.0137 0.424 Uiso 1 1 calc R . . C26 C 0.3915(12) 1.0109(9) 0.1231(7) 0.330(10) Uani 1 1 d . A . H26A H 0.3404 1.0189 0.0838 0.495 Uiso 1 1 calc R . . H26B H 0.4453 1.0729 0.1438 0.495 Uiso 1 1 calc R . . H26C H 0.3480 1.0006 0.1540 0.495 Uiso 1 1 calc R . . C27 C 0.1701(3) 0.3356(3) 0.10133(15) 0.0531(7) Uani 1 1 d . . . C28 C 0.2467(3) 0.3514(3) 0.06264(18) 0.0665(9) Uani 1 1 d . . . C29 C 0.2695(4) 0.2630(4) 0.0164(2) 0.0880(14) Uani 1 1 d . . . H29 H 0.3195 0.2716 -0.0100 0.106 Uiso 1 1 calc R . . C30 C 0.2212(5) 0.1654(4) 0.0088(2) 0.1023(17) Uani 1 1 d . . . H30 H 0.2389 0.1079 -0.0220 0.123 Uiso 1 1 calc R . . C31 C 0.1468(5) 0.1513(3) 0.0460(2) 0.0916(14) Uani 1 1 d . . . H31 H 0.1132 0.0838 0.0398 0.110 Uiso 1 1 calc R . . C32 C 0.1194(3) 0.2345(3) 0.09292(18) 0.0653(9) Uani 1 1 d . . . C33 C 0.2995(3) 0.4595(4) 0.0687(2) 0.0802(12) Uani 1 1 d . . . H33 H 0.2914 0.5062 0.1113 0.096 Uiso 1 1 calc R . . C34 C 0.4264(5) 0.4664(7) 0.0699(4) 0.149(3) Uani 1 1 d . . . H34A H 0.4690 0.4560 0.1108 0.223 Uiso 1 1 calc R . . H34B H 0.4514 0.5344 0.0673 0.223 Uiso 1 1 calc R . . H34C H 0.4392 0.4131 0.0324 0.223 Uiso 1 1 calc R . . C35 C 0.2358(5) 0.5015(4) 0.0136(3) 0.1087(17) Uani 1 1 d . . . H35A H 0.2437 0.4586 -0.0290 0.163 Uiso 1 1 calc R . . H35B H 0.2672 0.5725 0.0207 0.163 Uiso 1 1 calc R . . H35C H 0.1559 0.5000 0.0140 0.163 Uiso 1 1 calc R . . C36 C 0.0375(4) 0.2130(3) 0.1343(2) 0.0727(10) Uani 1 1 d . . . H36 H 0.0200 0.2812 0.1596 0.087 Uiso 1 1 calc R . . C37 C -0.0746(5) 0.1517(6) 0.0925(4) 0.154(3) Uani 1 1 d . . . H37A H -0.1054 0.1829 0.0578 0.231 Uiso 1 1 calc R . . H37B H -0.1277 0.1525 0.1203 0.231 Uiso 1 1 calc R . . H37C H -0.0622 0.0805 0.0727 0.231 Uiso 1 1 calc R . . C38 C 0.0978(5) 0.1594(5) 0.1856(3) 0.1148(19) Uani 1 1 d . . . H38A H 0.0511 0.1570 0.2165 0.172 Uiso 1 1 calc R . . H38B H 0.1709 0.1985 0.2096 0.172 Uiso 1 1 calc R . . H38C H 0.1090 0.0892 0.1627 0.172 Uiso 1 1 calc R . . C39 C 0.0543(2) 0.4677(2) 0.13966(14) 0.0446(6) Uani 1 1 d . A . H39 H 0.0003 0.4427 0.0989 0.053 Uiso 1 1 calc R . . C40 C -0.0640(3) 0.5989(2) 0.17782(15) 0.0495(7) Uani 1 1 d . . . C41 C -0.0608(3) 0.6936(3) 0.16089(17) 0.0585(8) Uani 1 1 d . . . C42 C -0.1611(4) 0.7434(3) 0.1549(2) 0.0731(11) Uani 1 1 d . . . H42 H -0.1604 0.8064 0.1439 0.088 Uiso 1 1 calc R . . C43 C -0.2580(4) 0.7033(4) 0.1646(2) 0.0822(13) Uani 1 1 d . . . H43 H -0.3233 0.7384 0.1600 0.099 Uiso 1 1 calc R . . C44 C -0.2619(3) 0.6111(4) 0.1812(2) 0.0830(12) Uani 1 1 d . . . H44 H -0.3302 0.5846 0.1878 0.100 Uiso 1 1 calc R . . C45 C -0.1656(3) 0.5555(3) 0.18862(18) 0.0628(9) Uani 1 1 d . . . C46 C 0.0465(3) 0.7389(3) 0.1479(2) 0.0684(10) Uani 1 1 d . . . H46 H 0.1113 0.7116 0.1722 0.082 Uiso 1 1 calc R . . C47 C 0.0463(5) 0.7005(4) 0.0753(3) 0.1066(17) Uani 1 1 d . . . H47A H 0.0450 0.6254 0.0623 0.160 Uiso 1 1 calc R . . H47B H 0.1142 0.7316 0.0679 0.160 Uiso 1 1 calc R . . H47C H -0.0205 0.7198 0.0492 0.160 Uiso 1 1 calc R . . C48 C 0.0675(5) 0.8565(4) 0.1739(3) 0.119(2) Uani 1 1 d . . . H48A H 0.0081 0.8866 0.1493 0.179 Uiso 1 1 calc R . . H48B H 0.1408 0.8799 0.1685 0.179 Uiso 1 1 calc R . . H48C H 0.0669 0.8782 0.2205 0.179 Uiso 1 1 calc R . . C49 C -0.1733(3) 0.4544(4) 0.2077(2) 0.0815(13) Uani 1 1 d . . . H49 H -0.0966 0.4307 0.2133 0.098 Uiso 1 1 calc R . . C50 C -0.2545(6) 0.3684(5) 0.1527(4) 0.125(2) Uani 1 1 d . . . H50A H -0.3304 0.3900 0.1452 0.187 Uiso 1 1 calc R . . H50B H -0.2563 0.3051 0.1660 0.187 Uiso 1 1 calc R . . H50C H -0.2283 0.3557 0.1121 0.187 Uiso 1 1 calc R . . C51 C -0.2074(5) 0.4694(5) 0.2736(3) 0.1109(19) Uani 1 1 d . . . H51A H -0.1489 0.5156 0.3091 0.166 Uiso 1 1 calc R . . H51B H -0.2162 0.4026 0.2821 0.166 Uiso 1 1 calc R . . H51C H -0.2789 0.4995 0.2713 0.166 Uiso 1 1 calc R . . C52 C 0.4247(4) 0.3960(4) 0.2324(2) 0.0809(11) Uani 1 1 d U . . H52A H 0.3831 0.3769 0.1858 0.097 Uiso 1 1 calc R . . H52B H 0.4798 0.4568 0.2411 0.097 Uiso 1 1 calc R . . C53 C 0.4824(6) 0.3105(6) 0.2464(4) 0.1396(19) Uani 1 1 d U . . H53A H 0.5645 0.3261 0.2527 0.168 Uiso 1 1 calc R . . H53B H 0.4561 0.2474 0.2092 0.168 Uiso 1 1 calc R . . C54 C 0.4582(5) 0.2942(5) 0.3068(3) 0.1199(17) Uani 1 1 d U . . H54A H 0.5270 0.3140 0.3430 0.144 Uiso 1 1 calc R . . H54B H 0.4327 0.2206 0.2991 0.144 Uiso 1 1 calc R . . C55 C 0.3670(4) 0.3598(4) 0.3245(2) 0.0861(12) Uani 1 1 d U . . H55A H 0.2979 0.3161 0.3214 0.103 Uiso 1 1 calc R . . H55B H 0.3924 0.4065 0.3697 0.103 Uiso 1 1 calc R . . C56 C 0.0580(4) 0.7019(3) 0.3484(2) 0.0801(11) Uani 1 1 d U . . H56A H -0.0076 0.6767 0.3104 0.096 Uiso 1 1 calc R . . H56B H 0.0560 0.6601 0.3791 0.096 Uiso 1 1 calc R . . C57 C 0.0560(6) 0.8090(5) 0.3809(4) 0.145(2) Uani 1 1 d U . . H57A H 0.0356 0.8163 0.4233 0.174 Uiso 1 1 calc R . . H57B H -0.0014 0.8380 0.3534 0.174 Uiso 1 1 calc R . . C58 C 0.1672(5) 0.8657(4) 0.3924(3) 0.1205(18) Uani 1 1 d U . . H58A H 0.2076 0.8815 0.4391 0.145 Uiso 1 1 calc R . . H58B H 0.1592 0.9312 0.3810 0.145 Uiso 1 1 calc R . . C59 C 0.2313(4) 0.7970(3) 0.3491(2) 0.0857(12) Uani 1 1 d U . . H59A H 0.2370 0.8229 0.3115 0.103 Uiso 1 1 calc R . . H59B H 0.3082 0.7940 0.3742 0.103 Uiso 1 1 calc R . . N1 N 0.1535(2) 0.4766(2) 0.34009(13) 0.0543(6) Uani 1 1 d . A . N2 N -0.0721(3) 0.2119(3) 0.33111(19) 0.0732(9) Uani 1 1 d . . . N3 N 0.3621(2) 0.6378(2) 0.25970(15) 0.0599(7) Uani 1 1 d . A . N4 N 0.4071(8) 0.8378(7) 0.1369(5) 0.071(3) Uani 0.599(16) 1 d P A 1 N4' N 0.4973(9) 0.8821(7) 0.1648(5) 0.073(4) Uani 0.401(16) 1 d P A 2 N5 N 0.1496(2) 0.4242(2) 0.15171(12) 0.0464(5) Uani 1 1 d . A . N6 N 0.0380(2) 0.5483(2) 0.18751(12) 0.0460(5) Uani 1 1 d . A . O1 O 0.3456(2) 0.41998(19) 0.27576(13) 0.0636(6) Uani 1 1 d . A . O2 O 0.1659(2) 0.69445(17) 0.32604(12) 0.0613(6) Uani 1 1 d . A . Yb1 Yb 0.208611(10) 0.535516(9) 0.261083(6) 0.04196(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0585(18) 0.0555(18) 0.0490(17) 0.0177(14) 0.0115(14) 0.0025(14) C2 0.0552(17) 0.0589(18) 0.0591(19) 0.0276(15) 0.0215(15) 0.0067(14) C3 0.065(2) 0.065(2) 0.0502(18) 0.0267(15) 0.0170(15) 0.0096(16) C4 0.0605(18) 0.0572(18) 0.0466(17) 0.0191(14) 0.0134(14) 0.0064(14) C5 0.083(3) 0.068(2) 0.058(2) 0.0189(18) 0.0131(19) -0.0065(19) C6 0.111(4) 0.096(3) 0.057(2) 0.016(2) 0.003(2) -0.015(3) C7 0.148(5) 0.113(4) 0.045(2) 0.022(2) 0.007(3) -0.015(3) C8 0.113(3) 0.103(3) 0.057(2) 0.039(2) 0.026(2) -0.001(3) C9 0.065(2) 0.072(2) 0.079(3) 0.039(2) 0.030(2) 0.0057(18) C10 0.075(3) 0.067(2) 0.112(4) 0.035(2) 0.034(2) -0.0027(19) C11 0.076(3) 0.109(4) 0.189(7) 0.038(4) 0.038(4) -0.010(3) C12 0.146(5) 0.073(3) 0.234(9) 0.015(4) 0.102(6) -0.012(3) C13 0.152(6) 0.141(6) 0.178(7) 0.094(5) 0.026(5) -0.046(5) C14 0.070(2) 0.070(2) 0.084(3) 0.041(2) 0.025(2) 0.0159(18) C15 0.103(3) 0.0500(19) 0.107(3) 0.035(2) 0.069(3) 0.0177(19) C16 0.066(2) 0.055(2) 0.090(3) 0.0093(19) 0.043(2) -0.0008(16) C17 0.0476(16) 0.0545(18) 0.069(2) 0.0144(16) 0.0212(15) 0.0045(13) C18 0.062(2) 0.081(3) 0.070(2) 0.018(2) 0.0133(18) 0.0103(18) C19 0.071(3) 0.129(5) 0.086(3) -0.003(3) 0.002(3) 0.009(3) C20 0.062(3) 0.159(7) 0.137(6) -0.027(5) 0.005(3) -0.026(4) C21 0.085(3) 0.086(3) 0.156(6) -0.016(3) 0.070(4) -0.033(3) C22 0.064(4) 0.056(4) 0.060(5) 0.021(3) 0.028(4) 0.011(3) C22' 0.066(8) 0.070(9) 0.057(9) 0.022(6) 0.010(7) 0.013(7) C23 0.203(7) 0.144(6) 0.115(5) 0.094(5) 0.091(5) 0.093(5) C24 0.223(11) 0.266(13) 0.242(12) 0.189(11) 0.043(10) 0.044(10) C25 0.46(2) 0.274(13) 0.119(7) 0.115(9) 0.040(10) -0.072(13) C26 0.49(2) 0.332(15) 0.46(2) 0.344(16) 0.373(18) 0.330(16) C27 0.0533(17) 0.069(2) 0.0394(15) 0.0156(14) 0.0115(13) 0.0251(15) C28 0.059(2) 0.094(3) 0.0487(19) 0.0186(18) 0.0158(15) 0.0267(19) C29 0.099(3) 0.115(4) 0.064(3) 0.026(3) 0.041(2) 0.047(3) C30 0.149(5) 0.088(3) 0.082(3) 0.016(3) 0.053(3) 0.065(3) C31 0.143(4) 0.067(3) 0.077(3) 0.023(2) 0.045(3) 0.044(3) C32 0.086(3) 0.059(2) 0.054(2) 0.0170(16) 0.0203(18) 0.0234(18) C33 0.069(2) 0.113(3) 0.056(2) 0.011(2) 0.0281(19) -0.003(2) C34 0.080(3) 0.257(9) 0.145(6) 0.112(6) 0.036(4) -0.006(4) C35 0.121(4) 0.087(3) 0.113(4) 0.033(3) 0.013(3) 0.009(3) C36 0.100(3) 0.051(2) 0.069(2) 0.0161(17) 0.025(2) 0.0095(19) C37 0.101(4) 0.197(8) 0.127(5) -0.011(5) 0.034(4) -0.023(5) C38 0.146(5) 0.118(4) 0.120(5) 0.075(4) 0.057(4) 0.037(4) C39 0.0424(14) 0.0540(16) 0.0366(14) 0.0142(12) 0.0063(11) 0.0068(12) C40 0.0481(15) 0.0581(18) 0.0411(15) 0.0118(13) 0.0093(12) 0.0183(13) C41 0.0585(19) 0.063(2) 0.0508(18) 0.0160(15) 0.0055(15) 0.0167(15) C42 0.078(3) 0.073(2) 0.073(2) 0.023(2) 0.017(2) 0.038(2) C43 0.072(3) 0.108(3) 0.079(3) 0.033(2) 0.026(2) 0.055(2) C44 0.054(2) 0.119(4) 0.090(3) 0.039(3) 0.032(2) 0.032(2) C45 0.0488(17) 0.088(3) 0.060(2) 0.0277(18) 0.0191(15) 0.0203(16) C46 0.062(2) 0.064(2) 0.081(3) 0.0300(19) 0.0079(18) 0.0122(16) C47 0.106(4) 0.111(4) 0.108(4) 0.019(3) 0.054(3) -0.002(3) C48 0.147(5) 0.077(3) 0.130(5) 0.018(3) 0.044(4) -0.019(3) C49 0.053(2) 0.113(3) 0.103(3) 0.056(3) 0.035(2) 0.021(2) C50 0.125(5) 0.106(4) 0.140(6) 0.035(4) 0.027(4) 0.003(4) C51 0.093(4) 0.157(5) 0.109(4) 0.074(4) 0.036(3) 0.008(3) C52 0.072(2) 0.107(3) 0.081(3) 0.040(2) 0.034(2) 0.036(2) C53 0.141(4) 0.139(4) 0.180(5) 0.074(4) 0.078(4) 0.066(3) C54 0.113(4) 0.125(4) 0.156(5) 0.082(3) 0.041(3) 0.064(3) C55 0.093(3) 0.090(3) 0.101(3) 0.067(3) 0.022(2) 0.030(2) C56 0.076(2) 0.079(2) 0.078(3) 0.002(2) 0.031(2) 0.010(2) C57 0.136(4) 0.099(3) 0.186(5) -0.011(4) 0.072(4) 0.011(3) C58 0.129(4) 0.074(3) 0.134(4) -0.016(3) 0.038(3) 0.006(3) C59 0.104(3) 0.050(2) 0.095(3) 0.009(2) 0.027(2) -0.007(2) N1 0.0636(16) 0.0564(15) 0.0450(14) 0.0186(12) 0.0141(12) -0.0011(12) N2 0.073(2) 0.0635(19) 0.087(2) 0.0238(18) 0.0266(18) -0.0025(16) N3 0.0492(14) 0.0648(17) 0.0744(19) 0.0348(15) 0.0146(13) 0.0047(12) N4 0.063(5) 0.085(5) 0.081(6) 0.047(4) 0.019(4) 0.008(3) N4' 0.087(8) 0.072(6) 0.081(7) 0.045(5) 0.035(5) 0.007(5) N5 0.0455(13) 0.0556(14) 0.0392(12) 0.0146(11) 0.0102(10) 0.0132(10) N6 0.0422(12) 0.0555(14) 0.0410(13) 0.0153(11) 0.0081(10) 0.0119(10) O1 0.0590(13) 0.0698(15) 0.0702(16) 0.0354(13) 0.0120(12) 0.0146(11) O2 0.0680(14) 0.0502(12) 0.0635(14) 0.0113(11) 0.0185(11) 0.0010(10) Yb1 0.04092(7) 0.04721(8) 0.03952(7) 0.01804(5) 0.00708(5) 0.00124(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.364(4) . ? C1 N1 1.378(4) . ? C1 H1 0.9300 . ? C2 C3 1.431(5) . ? C2 C9 1.449(5) . ? C3 C8 1.396(5) . ? C3 C4 1.414(5) . ? C4 N1 1.389(4) . ? C4 C5 1.397(5) . ? C5 C6 1.370(5) . ? C5 H5 0.9300 . ? C6 C7 1.385(7) . ? C6 H6 0.9300 . ? C7 C8 1.380(7) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 N2 1.251(5) . ? C9 H9 0.9300 . ? C10 N2 1.483(5) . ? C10 C12 1.495(7) . ? C10 C11 1.512(7) . ? C10 C13 1.519(8) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.349(5) . ? C14 N3 1.389(4) . ? C14 Yb1 3.169(4) . ? C14 H14 0.9300 . ? C15 C16 1.427(6) . ? C15 C22 1.456(9) . ? C15 C22' 1.663(16) . ? C16 C17 1.401(5) . ? C16 C21 1.418(7) . ? C17 C18 1.385(5) . ? C17 N3 1.391(4) . ? C18 C19 1.361(6) . ? C18 H18 0.9300 . ? C19 C20 1.357(10) . ? C19 H19 0.9300 . ? C20 C21 1.357(10) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 N4 1.254(14) . ? C22 H22 0.9300 . ? C22' N4' 1.22(2) . ? C22' H22' 0.9300 . ? C23 C26 1.419(9) . ? C23 C25 1.454(12) . ? C23 C24 1.502(12) . ? C23 N4' 1.527(11) . ? C23 N4 1.602(10) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C32 1.400(5) . ? C27 C28 1.407(5) . ? C27 N5 1.435(4) . ? C28 C29 1.396(6) . ? C28 C33 1.506(6) . ? C29 C30 1.351(7) . ? C29 H29 0.9300 . ? C30 C31 1.356(7) . ? C30 H30 0.9300 . ? C31 C32 1.382(5) . ? C31 H31 0.9300 . ? C32 C36 1.523(6) . ? C33 C35 1.513(7) . ? C33 C34 1.514(6) . ? C33 H33 0.9800 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.500(7) . ? C36 C38 1.536(6) . ? C36 H36 0.9800 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 N5 1.313(4) . ? C39 N6 1.321(4) . ? C39 Yb1 2.730(3) . ? C39 H39 0.9300 . ? C40 C41 1.404(5) . ? C40 C45 1.414(5) . ? C40 N6 1.426(4) . ? C41 C42 1.399(5) . ? C41 C46 1.508(5) . ? C42 C43 1.337(6) . ? C42 H42 0.9300 . ? C43 C44 1.369(6) . ? C43 H43 0.9300 . ? C44 C45 1.404(5) . ? C44 H44 0.9300 . ? C45 C49 1.513(6) . ? C46 C47 1.493(6) . ? C46 C48 1.500(6) . ? C46 H46 0.9800 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C51 1.514(7) . ? C49 C50 1.520(8) . ? C49 H49 0.9800 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 C53 1.425(7) . ? C52 O1 1.453(4) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.450(8) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.480(6) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 O1 1.465(4) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.410(7) . ? C56 O2 1.472(4) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.440(8) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.482(7) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 O2 1.445(4) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? N1 Yb1 2.249(3) . ? N3 Yb1 2.250(3) . ? N5 Yb1 2.336(2) . ? N6 Yb1 2.339(2) . ? O1 Yb1 2.331(2) . ? O2 Yb1 2.339(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 C2 C1 N1 113.4(3) . . ? C2 C1 H1 123.3 . . ? N1 C1 H1 123.3 . . ? C1 C2 C3 105.7(3) . . ? C1 C2 C9 126.6(3) . . ? C3 C2 C9 127.6(3) . . ? C8 C3 C4 118.8(4) . . ? C8 C3 C2 135.3(4) . . ? C4 C3 C2 105.9(3) . . ? N1 C4 C5 128.2(3) . . ? N1 C4 C3 110.4(3) . . ? C5 C4 C3 121.4(3) . . ? C6 C5 C4 118.3(4) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C5 C6 C7 120.9(4) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C8 C7 C6 121.7(4) . . ? C8 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C7 C8 C3 118.8(4) . . ? C7 C8 H8 120.6 . . ? C3 C8 H8 120.6 . . ? N2 C9 C2 122.2(4) . . ? N2 C9 H9 118.9 . . ? C2 C9 H9 118.9 . . ? N2 C10 C12 105.4(4) . . ? N2 C10 C11 107.2(4) . . ? C12 C10 C11 108.8(5) . . ? N2 C10 C13 115.4(4) . . ? C12 C10 C13 110.0(5) . . ? C11 C10 C13 109.8(5) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 N3 112.9(4) . . ? C15 C14 Yb1 150.7(3) . . ? N3 C14 Yb1 38.31(16) . . ? C15 C14 H14 123.5 . . ? N3 C14 H14 123.5 . . ? Yb1 C14 H14 85.5 . . ? C14 C15 C16 106.7(3) . . ? C14 C15 C22 135.1(6) . . ? C16 C15 C22 118.2(5) . . ? C14 C15 C22' 106.2(8) . . ? C16 C15 C22' 147.1(8) . . ? C22 C15 C22' 28.9(6) . . ? C17 C16 C21 117.7(5) . . ? C17 C16 C15 105.5(3) . . ? C21 C16 C15 136.9(5) . . ? C18 C17 N3 128.0(3) . . ? C18 C17 C16 120.9(4) . . ? N3 C17 C16 111.1(3) . . ? C19 C18 C17 118.4(5) . . ? C19 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? C20 C19 C18 122.8(6) . . ? C20 C19 H19 118.6 . . ? C18 C19 H19 118.6 . . ? C19 C20 C21 120.0(5) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C16 120.3(5) . . ? C20 C21 H21 119.9 . . ? C16 C21 H21 119.9 . . ? N4 C22 C15 116.0(8) . . ? N4 C22 H22 122.0 . . ? C15 C22 H22 122.0 . . ? N4' C22' C15 112.7(14) . . ? N4' C22' H22' 123.6 . . ? C15 C22' H22' 123.6 . . ? C26 C23 C25 117.6(9) . . ? C26 C23 C24 107.8(10) . . ? C25 C23 C24 103.4(8) . . ? C26 C23 N4' 110.7(7) . . ? C25 C23 N4' 124.3(7) . . ? C24 C23 N4' 85.9(7) . . ? C26 C23 N4 105.7(6) . . ? C25 C23 N4 96.1(7) . . ? C24 C23 N4 126.7(7) . . ? N4' C23 N4 43.4(5) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 120.4(3) . . ? C32 C27 N5 120.7(3) . . ? C28 C27 N5 118.8(3) . . ? C29 C28 C27 117.4(4) . . ? C29 C28 C33 120.7(4) . . ? C27 C28 C33 121.8(3) . . ? C30 C29 C28 122.0(4) . . ? C30 C29 H29 119.0 . . ? C28 C29 H29 119.0 . . ? C29 C30 C31 120.0(4) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C30 C31 C32 121.8(5) . . ? C30 C31 H31 119.1 . . ? C32 C31 H31 119.1 . . ? C31 C32 C27 118.3(4) . . ? C31 C32 C36 119.2(4) . . ? C27 C32 C36 122.5(3) . . ? C28 C33 C35 111.3(4) . . ? C28 C33 C34 114.2(5) . . ? C35 C33 C34 109.4(4) . . ? C28 C33 H33 107.2 . . ? C35 C33 H33 107.2 . . ? C34 C33 H33 107.2 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C32 113.4(4) . . ? C37 C36 C38 111.8(5) . . ? C32 C36 C38 109.8(4) . . ? C37 C36 H36 107.2 . . ? C32 C36 H36 107.2 . . ? C38 C36 H36 107.2 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N5 C39 N6 117.5(3) . . ? N5 C39 Yb1 58.72(15) . . ? N6 C39 Yb1 58.85(14) . . ? N5 C39 H39 121.2 . . ? N6 C39 H39 121.2 . . ? Yb1 C39 H39 177.7 . . ? C41 C40 C45 120.9(3) . . ? C41 C40 N6 119.5(3) . . ? C45 C40 N6 119.5(3) . . ? C42 C41 C40 117.9(3) . . ? C42 C41 C46 121.0(3) . . ? C40 C41 C46 121.1(3) . . ? C43 C42 C41 122.0(4) . . ? C43 C42 H42 119.0 . . ? C41 C42 H42 119.0 . . ? C42 C43 C44 120.5(4) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C43 C44 C45 121.6(4) . . ? C43 C44 H44 119.2 . . ? C45 C44 H44 119.2 . . ? C44 C45 C40 117.0(4) . . ? C44 C45 C49 119.9(3) . . ? C40 C45 C49 123.0(3) . . ? C47 C46 C48 111.9(4) . . ? C47 C46 C41 110.8(3) . . ? C48 C46 C41 113.5(4) . . ? C47 C46 H46 106.8 . . ? C48 C46 H46 106.8 . . ? C41 C46 H46 106.8 . . ? 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 . . ? C45 C49 C51 112.5(5) . . ? C45 C49 C50 111.6(4) . . ? C51 C49 C50 110.3(5) . . ? C45 C49 H49 107.4 . . ? C51 C49 H49 107.4 . . ? C50 C49 H49 107.4 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 O1 107.4(4) . . ? C53 C52 H52A 110.2 . . ? O1 C52 H52A 110.2 . . ? C53 C52 H52B 110.2 . . ? O1 C52 H52B 110.2 . . ? H52A C52 H52B 108.5 . . ? C52 C53 C54 108.8(5) . . ? C52 C53 H53A 109.9 . . ? C54 C53 H53A 109.9 . . ? C52 C53 H53B 109.9 . . ? C54 C53 H53B 109.9 . . ? H53A C53 H53B 108.3 . . ? C53 C54 C55 108.0(4) . . ? C53 C54 H54A 110.1 . . ? C55 C54 H54A 110.1 . . ? C53 C54 H54B 110.1 . . ? C55 C54 H54B 110.1 . . ? H54A C54 H54B 108.4 . . ? O1 C55 C54 105.4(4) . . ? O1 C55 H55A 110.7 . . ? C54 C55 H55A 110.7 . . ? O1 C55 H55B 110.7 . . ? C54 C55 H55B 110.7 . . ? H55A C55 H55B 108.8 . . ? C57 C56 O2 106.3(4) . . ? C57 C56 H56A 110.5 . . ? O2 C56 H56A 110.5 . . ? C57 C56 H56B 110.5 . . ? O2 C56 H56B 110.5 . . ? H56A C56 H56B 108.7 . . ? C56 C57 C58 109.8(5) . . ? C56 C57 H57A 109.7 . . ? C58 C57 H57A 109.7 . . ? C56 C57 H57B 109.7 . . ? C58 C57 H57B 109.7 . . ? H57A C57 H57B 108.2 . . ? C57 C58 C59 106.8(4) . . ? C57 C58 H58A 110.4 . . ? C59 C58 H58A 110.4 . . ? C57 C58 H58B 110.4 . . ? C59 C58 H58B 110.4 . . ? H58A C58 H58B 108.6 . . ? O2 C59 C58 105.5(4) . . ? O2 C59 H59A 110.6 . . ? C58 C59 H59A 110.6 . . ? O2 C59 H59B 110.6 . . ? C58 C59 H59B 110.6 . . ? H59A C59 H59B 108.8 . . ? C1 N1 C4 104.5(3) . . ? C1 N1 Yb1 123.7(2) . . ? C4 N1 Yb1 131.7(2) . . ? C9 N2 C10 120.6(4) . . ? C14 N3 C17 103.8(3) . . ? C14 N3 Yb1 119.2(2) . . ? C17 N3 Yb1 136.4(2) . . ? C22 N4 C23 111.6(8) . . ? C22' N4' C23 102.6(12) . . ? C39 N5 C27 119.3(2) . . ? C39 N5 Yb1 92.57(17) . . ? C27 N5 Yb1 147.97(18) . . ? C39 N6 C40 120.4(2) . . ? C39 N6 Yb1 92.25(17) . . ? C40 N6 Yb1 147.24(19) . . ? C52 O1 C55 109.2(3) . . ? C52 O1 Yb1 121.3(2) . . ? C55 O1 Yb1 129.5(2) . . ? C59 O2 C56 109.3(3) . . ? C59 O2 Yb1 129.3(2) . . ? C56 O2 Yb1 121.4(2) . . ? N1 Yb1 N3 134.38(10) . . ? N1 Yb1 O1 80.37(9) . . ? N3 Yb1 O1 82.24(9) . . ? N1 Yb1 N5 115.69(9) . . ? N3 Yb1 N5 104.31(10) . . ? O1 Yb1 N5 84.98(9) . . ? N1 Yb1 N6 105.32(9) . . ? N3 Yb1 N6 114.47(9) . . ? O1 Yb1 N6 141.18(9) . . ? N5 Yb1 N6 57.59(8) . . ? N1 Yb1 O2 81.47(9) . . ? N3 Yb1 O2 82.44(10) . . ? O1 Yb1 O2 135.89(9) . . ? N5 Yb1 O2 138.98(8) . . ? N6 Yb1 O2 82.51(8) . . ? N1 Yb1 C39 112.72(9) . . ? N3 Yb1 C39 112.90(10) . . ? O1 Yb1 C39 112.99(9) . . ? N5 Yb1 C39 28.71(8) . . ? N6 Yb1 C39 28.90(8) . . ? O2 Yb1 C39 111.09(9) . . ? N1 Yb1 C14 153.25(10) . . ? N3 Yb1 C14 22.51(10) . . ? O1 Yb1 C14 98.84(9) . . ? N5 Yb1 C14 90.72(10) . . ? N6 Yb1 C14 92.08(10) . . ? O2 Yb1 C14 80.84(9) . . ? C39 Yb1 C14 92.36(10) . . ? 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 C1 C2 C3 -0.6(4) . . . . ? N1 C1 C2 C9 -177.5(3) . . . . ? C1 C2 C3 C8 179.6(5) . . . . ? C9 C2 C3 C8 -3.5(7) . . . . ? C1 C2 C3 C4 -0.4(4) . . . . ? C9 C2 C3 C4 176.5(3) . . . . ? C8 C3 C4 N1 -178.8(4) . . . . ? C2 C3 C4 N1 1.3(4) . . . . ? C8 C3 C4 C5 2.3(6) . . . . ? C2 C3 C4 C5 -177.7(3) . . . . ? N1 C4 C5 C6 -179.4(4) . . . . ? C3 C4 C5 C6 -0.6(6) . . . . ? C4 C5 C6 C7 -1.7(8) . . . . ? C5 C6 C7 C8 2.4(9) . . . . ? C6 C7 C8 C3 -0.7(9) . . . . ? C4 C3 C8 C7 -1.6(7) . . . . ? C2 C3 C8 C7 178.3(5) . . . . ? C1 C2 C9 N2 3.0(6) . . . . ? C3 C2 C9 N2 -173.3(4) . . . . ? N3 C14 C15 C16 -0.1(5) . . . . ? Yb1 C14 C15 C16 9.0(7) . . . . ? N3 C14 C15 C22 179.9(5) . . . . ? Yb1 C14 C15 C22 -171.0(5) . . . . ? N3 C14 C15 C22' 178.3(6) . . . . ? Yb1 C14 C15 C22' -172.6(7) . . . . ? C14 C15 C16 C17 0.0(4) . . . . ? C22 C15 C16 C17 -180.0(4) . . . . ? C22' C15 C16 C17 -177.2(11) . . . . ? C14 C15 C16 C21 179.2(5) . . . . ? C22 C15 C16 C21 -0.8(7) . . . . ? C22' C15 C16 C21 2.0(13) . . . . ? C21 C16 C17 C18 -0.3(5) . . . . ? C15 C16 C17 C18 179.0(3) . . . . ? C21 C16 C17 N3 -179.3(3) . . . . ? C15 C16 C17 N3 0.1(4) . . . . ? N3 C17 C18 C19 178.8(4) . . . . ? C16 C17 C18 C19 0.0(6) . . . . ? C17 C18 C19 C20 0.4(8) . . . . ? C18 C19 C20 C21 -0.4(10) . . . . ? C19 C20 C21 C16 0.1(10) . . . . ? C17 C16 C21 C20 0.3(7) . . . . ? C15 C16 C21 C20 -178.8(5) . . . . ? C14 C15 C22 N4 -2.7(10) . . . . ? C16 C15 C22 N4 177.3(7) . . . . ? C22' C15 C22 N4 0.4(14) . . . . ? C14 C15 C22' N4' 178.1(10) . . . . ? C16 C15 C22' N4' -4.7(19) . . . . ? C22 C15 C22' N4' 0.4(7) . . . . ? C32 C27 C28 C29 -0.1(5) . . . . ? N5 C27 C28 C29 176.8(3) . . . . ? C32 C27 C28 C33 177.8(3) . . . . ? N5 C27 C28 C33 -5.3(5) . . . . ? C27 C28 C29 C30 -0.4(6) . . . . ? C33 C28 C29 C30 -178.4(4) . . . . ? C28 C29 C30 C31 1.0(8) . . . . ? C29 C30 C31 C32 -0.9(8) . . . . ? C30 C31 C32 C27 0.4(7) . . . . ? C30 C31 C32 C36 -178.5(5) . . . . ? C28 C27 C32 C31 0.1(5) . . . . ? N5 C27 C32 C31 -176.7(3) . . . . ? C28 C27 C32 C36 179.0(3) . . . . ? N5 C27 C32 C36 2.1(5) . . . . ? C29 C28 C33 C35 79.1(5) . . . . ? C27 C28 C33 C35 -98.7(4) . . . . ? C29 C28 C33 C34 -45.4(6) . . . . ? C27 C28 C33 C34 136.8(4) . . . . ? C31 C32 C36 C37 -53.8(6) . . . . ? C27 C32 C36 C37 127.3(5) . . . . ? C31 C32 C36 C38 71.9(5) . . . . ? C27 C32 C36 C38 -106.9(4) . . . . ? C45 C40 C41 C42 -0.1(5) . . . . ? N6 C40 C41 C42 -177.0(3) . . . . ? C45 C40 C41 C46 -178.7(3) . . . . ? N6 C40 C41 C46 4.5(5) . . . . ? C40 C41 C42 C43 -0.2(6) . . . . ? C46 C41 C42 C43 178.3(4) . . . . ? C41 C42 C43 C44 0.4(7) . . . . ? C42 C43 C44 C45 -0.1(7) . . . . ? C43 C44 C45 C40 -0.3(6) . . . . ? C43 C44 C45 C49 179.4(4) . . . . ? C41 C40 C45 C44 0.4(5) . . . . ? N6 C40 C45 C44 177.2(3) . . . . ? C41 C40 C45 C49 -179.3(4) . . . . ? N6 C40 C45 C49 -2.4(5) . . . . ? C42 C41 C46 C47 -87.6(5) . . . . ? C40 C41 C46 C47 90.9(4) . . . . ? C42 C41 C46 C48 39.2(5) . . . . ? C40 C41 C46 C48 -142.3(4) . . . . ? C44 C45 C49 C51 -58.3(6) . . . . ? C40 C45 C49 C51 121.4(4) . . . . ? C44 C45 C49 C50 66.4(6) . . . . ? C40 C45 C49 C50 -114.0(5) . . . . ? O1 C52 C53 C54 -11.4(8) . . . . ? C52 C53 C54 C55 9.7(9) . . . . ? C53 C54 C55 O1 -4.0(7) . . . . ? O2 C56 C57 C58 -12.0(8) . . . . ? C56 C57 C58 C59 15.9(9) . . . . ? C57 C58 C59 O2 -13.0(7) . . . . ? C2 C1 N1 C4 1.3(4) . . . . ? C2 C1 N1 Yb1 178.4(2) . . . . ? C5 C4 N1 C1 177.3(4) . . . . ? C3 C4 N1 C1 -1.6(4) . . . . ? C5 C4 N1 Yb1 0.6(6) . . . . ? C3 C4 N1 Yb1 -178.3(2) . . . . ? C2 C9 N2 C10 180.0(4) . . . . ? C12 C10 N2 C9 -138.1(5) . . . . ? C11 C10 N2 C9 106.1(5) . . . . ? C13 C10 N2 C9 -16.6(7) . . . . ? C15 C14 N3 C17 0.1(4) . . . . ? Yb1 C14 N3 C17 -172.7(4) . . . . ? C15 C14 N3 Yb1 172.8(3) . . . . ? C18 C17 N3 C14 -179.0(4) . . . . ? C16 C17 N3 C14 -0.1(4) . . . . ? C18 C17 N3 Yb1 10.3(6) . . . . ? C16 C17 N3 Yb1 -170.8(3) . . . . ? C15 C22 N4 C23 179.5(5) . . . . ? C26 C23 N4 C22 -102.9(11) . . . . ? C25 C23 N4 C22 136.2(10) . . . . ? C24 C23 N4 C22 24.4(13) . . . . ? N4' C23 N4 C22 0.8(7) . . . . ? C15 C22' N4' C23 -179.0(8) . . . . ? C26 C23 N4' C22' 91.2(12) . . . . ? C25 C23 N4' C22' -57.9(14) . . . . ? C24 C23 N4' C22' -161.3(11) . . . . ? N4 C23 N4' C22' -0.1(11) . . . . ? N6 C39 N5 C27 179.3(3) . . . . ? Yb1 C39 N5 C27 176.6(3) . . . . ? N6 C39 N5 Yb1 2.7(3) . . . . ? C32 C27 N5 C39 -80.7(4) . . . . ? C28 C27 N5 C39 102.4(3) . . . . ? C32 C27 N5 Yb1 93.0(5) . . . . ? C28 C27 N5 Yb1 -83.9(5) . . . . ? N5 C39 N6 C40 -179.7(3) . . . . ? Yb1 C39 N6 C40 -177.0(3) . . . . ? N5 C39 N6 Yb1 -2.7(3) . . . . ? C41 C40 N6 C39 -100.5(4) . . . . ? C45 C40 N6 C39 82.6(4) . . . . ? C41 C40 N6 Yb1 85.1(4) . . . . ? C45 C40 N6 Yb1 -91.8(4) . . . . ? C53 C52 O1 C55 8.8(6) . . . . ? C53 C52 O1 Yb1 -170.0(4) . . . . ? C54 C55 O1 C52 -2.9(5) . . . . ? C54 C55 O1 Yb1 175.8(3) . . . . ? C58 C59 O2 C56 5.9(5) . . . . ? C58 C59 O2 Yb1 -175.7(3) . . . . ? C57 C56 O2 C59 3.5(6) . . . . ? C57 C56 O2 Yb1 -175.0(4) . . . . ? C1 N1 Yb1 N3 -159.8(2) . . . . ? C4 N1 Yb1 N3 16.4(4) . . . . ? C1 N1 Yb1 O1 -90.7(3) . . . . ? C4 N1 Yb1 O1 85.4(3) . . . . ? C1 N1 Yb1 N5 -11.1(3) . . . . ? C4 N1 Yb1 N5 165.1(3) . . . . ? C1 N1 Yb1 N6 49.9(3) . . . . ? C4 N1 Yb1 N6 -133.9(3) . . . . ? C1 N1 Yb1 O2 129.7(3) . . . . ? C4 N1 Yb1 O2 -54.2(3) . . . . ? C1 N1 Yb1 C39 20.3(3) . . . . ? C4 N1 Yb1 C39 -163.5(3) . . . . ? C1 N1 Yb1 C14 178.7(2) . . . . ? C4 N1 Yb1 C14 -5.1(4) . . . . ? C14 N3 Yb1 N1 -154.5(3) . . . . ? C17 N3 Yb1 N1 15.2(4) . . . . ? C14 N3 Yb1 O1 137.2(3) . . . . ? C17 N3 Yb1 O1 -53.1(3) . . . . ? C14 N3 Yb1 N5 54.4(3) . . . . ? C17 N3 Yb1 N5 -135.9(3) . . . . ? C14 N3 Yb1 N6 -6.1(3) . . . . ? C17 N3 Yb1 N6 163.6(3) . . . . ? C14 N3 Yb1 O2 -84.3(3) . . . . ? C17 N3 Yb1 O2 85.4(3) . . . . ? C14 N3 Yb1 C39 25.5(3) . . . . ? C17 N3 Yb1 C39 -164.9(3) . . . . ? C17 N3 Yb1 C14 169.7(5) . . . . ? C52 O1 Yb1 N1 172.9(3) . . . . ? C55 O1 Yb1 N1 -5.7(3) . . . . ? C52 O1 Yb1 N3 -49.5(3) . . . . ? C55 O1 Yb1 N3 132.0(3) . . . . ? C52 O1 Yb1 N5 55.7(3) . . . . ? C55 O1 Yb1 N5 -122.8(3) . . . . ? C52 O1 Yb1 N6 70.3(3) . . . . ? C55 O1 Yb1 N6 -108.2(3) . . . . ? C52 O1 Yb1 O2 -120.2(3) . . . . ? C55 O1 Yb1 O2 61.3(4) . . . . ? C52 O1 Yb1 C39 62.1(3) . . . . ? C55 O1 Yb1 C39 -116.4(3) . . . . ? C52 O1 Yb1 C14 -34.2(3) . . . . ? C55 O1 Yb1 C14 147.3(3) . . . . ? C39 N5 Yb1 N1 90.81(19) . . . . ? C27 N5 Yb1 N1 -83.7(4) . . . . ? C39 N5 Yb1 N3 -111.73(18) . . . . ? C27 N5 Yb1 N3 73.8(4) . . . . ? C39 N5 Yb1 O1 167.60(18) . . . . ? C27 N5 Yb1 O1 -6.9(4) . . . . ? C39 N5 Yb1 N6 -1.59(16) . . . . ? C27 N5 Yb1 N6 -176.1(4) . . . . ? C39 N5 Yb1 O2 -16.8(2) . . . . ? C27 N5 Yb1 O2 168.7(4) . . . . ? C27 N5 Yb1 C39 -174.5(5) . . . . ? C39 N5 Yb1 C14 -93.59(18) . . . . ? C27 N5 Yb1 C14 91.9(4) . . . . ? C39 N6 Yb1 N1 -109.43(18) . . . . ? C40 N6 Yb1 N1 65.8(4) . . . . ? C39 N6 Yb1 N3 93.45(19) . . . . ? C40 N6 Yb1 N3 -91.4(4) . . . . ? C39 N6 Yb1 O1 -15.8(2) . . . . ? C40 N6 Yb1 O1 159.4(3) . . . . ? C39 N6 Yb1 N5 1.58(16) . . . . ? C40 N6 Yb1 N5 176.8(4) . . . . ? C39 N6 Yb1 O2 171.58(18) . . . . ? C40 N6 Yb1 O2 -13.2(4) . . . . ? C40 N6 Yb1 C39 175.2(5) . . . . ? C39 N6 Yb1 C14 91.11(18) . . . . ? C40 N6 Yb1 C14 -93.7(4) . . . . ? C59 O2 Yb1 N1 134.2(3) . . . . ? C56 O2 Yb1 N1 -47.5(3) . . . . ? C59 O2 Yb1 N3 -3.0(3) . . . . ? C56 O2 Yb1 N3 175.3(3) . . . . ? C59 O2 Yb1 O1 67.6(4) . . . . ? C56 O2 Yb1 O1 -114.1(3) . . . . ? C59 O2 Yb1 N5 -106.1(3) . . . . ? C56 O2 Yb1 N5 72.2(3) . . . . ? C59 O2 Yb1 N6 -119.0(3) . . . . ? C56 O2 Yb1 N6 59.3(3) . . . . ? C59 O2 Yb1 C39 -114.6(3) . . . . ? C56 O2 Yb1 C39 63.6(3) . . . . ? C59 O2 Yb1 C14 -25.7(3) . . . . ? C56 O2 Yb1 C14 152.6(3) . . . . ? N5 C39 Yb1 N1 -102.33(19) . . . . ? N6 C39 Yb1 N1 80.44(19) . . . . ? N5 C39 Yb1 N3 77.72(19) . . . . ? N6 C39 Yb1 N3 -99.51(19) . . . . ? N5 C39 Yb1 O1 -13.4(2) . . . . ? N6 C39 Yb1 O1 169.34(17) . . . . ? N6 C39 Yb1 N5 -177.2(3) . . . . ? N5 C39 Yb1 N6 177.2(3) . . . . ? N5 C39 Yb1 O2 168.28(17) . . . . ? N6 C39 Yb1 O2 -8.95(19) . . . . ? N5 C39 Yb1 C14 87.20(18) . . . . ? N6 C39 Yb1 C14 -90.03(18) . . . . ? C15 C14 Yb1 N1 29.6(7) . . . . ? N3 C14 Yb1 N1 43.2(4) . . . . ? C15 C14 Yb1 N3 -13.6(5) . . . . ? C15 C14 Yb1 O1 -56.5(6) . . . . ? N3 C14 Yb1 O1 -42.9(3) . . . . ? C15 C14 Yb1 N5 -141.6(6) . . . . ? N3 C14 Yb1 N5 -128.0(3) . . . . ? C15 C14 Yb1 N6 160.8(6) . . . . ? N3 C14 Yb1 N6 174.4(3) . . . . ? C15 C14 Yb1 O2 78.8(6) . . . . ? N3 C14 Yb1 O2 92.4(3) . . . . ? C15 C14 Yb1 C39 -170.2(6) . . . . ? N3 C14 Yb1 C39 -156.6(3) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.055 -0.004 0.500 540 88 ' ' 2 0.125 0.921 0.060 20 1 ' ' 3 0.154 0.027 0.865 11 0 ' ' 4 0.204 0.710 0.984 11 1 ' ' 5 0.236 0.849 0.824 10 0 ' ' 6 0.474 0.776 0.904 17 1 ' ' 7 0.483 0.333 0.944 7 0 ' ' 8 0.526 0.224 0.096 17 1 ' ' 9 0.517 0.667 0.056 7 1 ' ' 10 0.764 0.150 0.176 10 0 ' ' 11 0.796 0.288 0.015 11 1 ' ' 12 0.875 0.078 0.940 19 1 ' ' 13 0.846 0.972 0.135 11 0 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.79 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.691 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.069 # Attachment 'shelxl.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 896822' #TrackingRef 'shelxl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H89 N6 O2 Y' _chemical_formula_sum 'C66 H89 N6 O2 Y' _chemical_formula_weight 1087.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8630(12) _cell_length_b 13.3410(14) _cell_length_c 20.967(2) _cell_angle_alpha 106.190(6) _cell_angle_beta 102.549(13) _cell_angle_gamma 91.116(7) _cell_volume 3099.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 12224 _cell_measurement_theta_min 1.60 _cell_measurement_theta_max 27.90 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 0.987 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7976 _exptl_absorpt_correction_T_max 0.8270 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn724 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.222 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 40064 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0844 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.94 _reflns_number_total 14725 _reflns_number_gt 10846 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r2' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure 4.0' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2009)' _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^)+(0.0366P)^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 14725 _refine_ls_number_parameters 918 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.0982 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.702745(15) 0.035903(15) 0.759264(9) 0.02323(6) Uani 1 1 d . . . O1 O 0.84158(11) -0.08254(11) 0.77863(7) 0.0304(3) Uani 1 1 d . . . O2 O 0.66239(11) 0.19982(11) 0.82542(7) 0.0303(3) Uani 1 1 d . . . N1 N 0.85985(14) 0.13178(14) 0.75271(9) 0.0316(4) Uani 1 1 d . . . N2 N 0.99658(17) 0.39424(16) 0.67157(9) 0.0436(5) Uani 1 1 d . . . N3 N 0.64252(14) -0.01625(13) 0.84232(8) 0.0285(4) Uani 1 1 d . . . N4 N 0.42410(14) -0.28061(14) 0.83906(9) 0.0309(4) Uani 1 1 d . . . N5 N 0.64100(13) -0.08114(13) 0.64818(8) 0.0232(4) Uani 1 1 d . . . N6 N 0.53333(13) 0.05376(13) 0.68141(8) 0.0240(4) Uani 1 1 d . . . C1 C 0.84005(18) 0.18396(17) 0.70349(11) 0.0335(5) Uani 1 1 d . . . H1 H 0.7722 0.1690 0.6675 0.040 Uiso 1 1 calc R . . C2 C 0.92628(18) 0.25916(17) 0.71078(11) 0.0328(5) Uani 1 1 d . . . C3 C 1.01173(17) 0.25518(16) 0.77006(11) 0.0311(5) Uani 1 1 d . . . C4 C 0.96865(16) 0.17567(16) 0.79400(10) 0.0278(5) Uani 1 1 d . . . C5 C 1.03092(18) 0.14796(18) 0.84975(10) 0.0352(5) Uani 1 1 d . . . H5 H 1.0009 0.0949 0.8653 0.042 Uiso 1 1 calc R . . C6 C 1.13885(19) 0.2011(2) 0.88181(11) 0.0431(6) Uani 1 1 d . . . H6 H 1.1852 0.1835 0.9195 0.052 Uiso 1 1 calc R . . C7 C 1.18067(19) 0.2817(2) 0.85866(12) 0.0456(6) Uani 1 1 d . . . H7 H 1.2543 0.3180 0.8821 0.055 Uiso 1 1 calc R . . C8 C 1.11908(19) 0.30906(19) 0.80407(12) 0.0406(6) Uani 1 1 d . . . H8 H 1.1488 0.3635 0.7896 0.049 Uiso 1 1 calc R . . C9 C 0.92030(19) 0.32436(17) 0.66274(12) 0.0366(5) Uani 1 1 d . . . H9 H 0.8562 0.3117 0.6245 0.044 Uiso 1 1 calc R . . C10 C 0.9825(2) 0.4566(2) 0.62120(12) 0.0475(6) Uani 1 1 d . . . C11 C 0.9131(3) 0.3981(3) 0.55055(15) 0.1091(15) Uani 1 1 d . . . H11A H 0.9448 0.3307 0.5347 0.131 Uiso 1 1 calc R . . H11B H 0.9174 0.4397 0.5192 0.131 Uiso 1 1 calc R . . H11C H 0.8321 0.3859 0.5519 0.131 Uiso 1 1 calc R . . C12 C 0.9277(3) 0.5556(3) 0.65221(17) 0.0938(12) Uani 1 1 d . . . H12A H 0.8456 0.5382 0.6489 0.113 Uiso 1 1 calc R . . H12B H 0.9348 0.6068 0.6274 0.113 Uiso 1 1 calc R . . H12C H 0.9676 0.5854 0.7003 0.113 Uiso 1 1 calc R . . C13 C 1.1038(2) 0.4850(2) 0.61814(14) 0.0672(8) Uani 1 1 d . . . H13A H 1.1484 0.5236 0.6640 0.081 Uiso 1 1 calc R . . H13B H 1.1017 0.5290 0.5875 0.081 Uiso 1 1 calc R . . H13C H 1.1406 0.4211 0.6010 0.081 Uiso 1 1 calc R . . C14 C 0.56444(16) -0.10051(16) 0.83021(10) 0.0269(4) Uani 1 1 d . . . H14 H 0.5217 -0.1386 0.7858 0.032 Uiso 1 1 calc R . . C15 C 0.55376(16) -0.12474(16) 0.88887(10) 0.0266(4) Uani 1 1 d . . . C16 C 0.63180(17) -0.04928(17) 0.94337(10) 0.0292(5) Uani 1 1 d . . . C17 C 0.68491(17) 0.01494(16) 0.91310(10) 0.0275(5) Uani 1 1 d . . . C18 C 0.77090(19) 0.09517(17) 0.95194(11) 0.0360(5) Uani 1 1 d . . . H18 H 0.8075 0.1369 0.9309 0.043 Uiso 1 1 calc R . . C19 C 0.8007(2) 0.1118(2) 1.02131(11) 0.0472(6) Uani 1 1 d . . . H19 H 0.8593 0.1653 1.0488 0.057 Uiso 1 1 calc R . . C20 C 0.7457(2) 0.0505(2) 1.05203(12) 0.0514(7) Uani 1 1 d . . . H20 H 0.7668 0.0644 1.1002 0.062 Uiso 1 1 calc R . . C21 C 0.6620(2) -0.02916(19) 1.01422(11) 0.0419(6) Uani 1 1 d . . . H21 H 0.6254 -0.0698 1.0359 0.050 Uiso 1 1 calc R . . C22 C 0.48196(17) -0.21191(17) 0.89214(11) 0.0299(5) Uani 1 1 d . . . H22 H 0.4780 -0.2179 0.9357 0.036 Uiso 1 1 calc R . . C23 C 0.35356(17) -0.36941(17) 0.84393(11) 0.0334(5) Uani 1 1 d . . . C24 C 0.22700(18) -0.34949(18) 0.82045(12) 0.0425(6) Uani 1 1 d . . . H24A H 0.2081 -0.2883 0.8537 0.051 Uiso 1 1 calc R . . H24B H 0.1767 -0.4110 0.8168 0.051 Uiso 1 1 calc R . . H24C H 0.2150 -0.3364 0.7758 0.051 Uiso 1 1 calc R . . C25 C 0.3825(2) -0.46633(18) 0.79357(13) 0.0476(6) Uani 1 1 d . . . H25A H 0.3688 -0.4560 0.7481 0.057 Uiso 1 1 calc R . . H25B H 0.3333 -0.5273 0.7918 0.057 Uiso 1 1 calc R . . H25C H 0.4641 -0.4781 0.8084 0.057 Uiso 1 1 calc R . . C26 C 0.3740(2) -0.3863(2) 0.91473(12) 0.0496(7) Uani 1 1 d . . . H26A H 0.4557 -0.3970 0.9301 0.060 Uiso 1 1 calc R . . H26B H 0.3254 -0.4481 0.9124 0.060 Uiso 1 1 calc R . . H26C H 0.3539 -0.3246 0.9470 0.060 Uiso 1 1 calc R . . C27 C 0.54539(17) -0.03314(16) 0.63503(10) 0.0251(4) Uani 1 1 d . . . H27 H 0.4788(16) -0.0656(15) 0.5903(10) 0.032(6) Uiso 1 1 d . . . C28 C 0.65994(16) -0.17497(16) 0.59893(9) 0.0251(4) Uani 1 1 d . . . C29 C 0.74205(17) -0.16682(17) 0.56053(10) 0.0298(5) Uani 1 1 d . . . C30 C 0.76413(19) -0.2596(2) 0.51525(11) 0.0366(6) Uani 1 1 d . . . H30 H 0.8165(18) -0.2499(17) 0.4897(11) 0.043(7) Uiso 1 1 d . . . C31 C 0.7090(2) -0.3551(2) 0.50792(12) 0.0405(6) Uani 1 1 d . . . H31 H 0.7269(18) -0.4209(18) 0.4743(11) 0.047(7) Uiso 1 1 d . . . C32 C 0.6301(2) -0.36186(18) 0.54653(11) 0.0366(5) Uani 1 1 d . . . H32 H 0.5928(17) -0.4314(17) 0.5412(10) 0.036(6) Uiso 1 1 d . . . C33 C 0.60380(17) -0.27248(16) 0.59251(10) 0.0286(5) Uani 1 1 d . . . C34 C 0.80147(18) -0.0627(2) 0.56600(11) 0.0355(5) Uani 1 1 d . . . H34 H 0.8055(15) -0.0206(15) 0.6096(10) 0.026(5) Uiso 1 1 d . . . C35 C 0.9281(2) -0.0696(3) 0.55944(18) 0.0589(8) Uani 1 1 d . . . H35A H 0.975(2) -0.110(2) 0.5886(14) 0.074(9) Uiso 1 1 d . . . H35B H 0.956(2) 0.000(2) 0.5773(12) 0.051(8) Uiso 1 1 d . . . H35C H 0.934(2) -0.109(2) 0.5105(14) 0.076(9) Uiso 1 1 d . . . C36 C 0.7349(2) -0.0135(2) 0.51325(13) 0.0418(6) Uani 1 1 d . . . H36A H 0.7384(17) -0.0577(18) 0.4665(11) 0.043(7) Uiso 1 1 d . . . H36B H 0.7764(18) 0.0530(18) 0.5170(10) 0.041(7) Uiso 1 1 d . . . H36C H 0.654(2) -0.0091(19) 0.5142(11) 0.054(8) Uiso 1 1 d . . . C37 C 0.52302(18) -0.28553(17) 0.63707(11) 0.0310(5) Uani 1 1 d . . . H37 H 0.4978(16) -0.2181(16) 0.6556(9) 0.027(5) Uiso 1 1 d . . . C38 C 0.5876(2) -0.3259(2) 0.69517(13) 0.0417(6) Uani 1 1 d . . . H38A H 0.6083(19) -0.3980(19) 0.6760(11) 0.049(7) Uiso 1 1 d . . . H38B H 0.5366(19) -0.3272(18) 0.7263(11) 0.051(7) Uiso 1 1 d . . . H38C H 0.662(2) -0.279(2) 0.7218(12) 0.058(8) Uiso 1 1 d . . . C39 C 0.4139(2) -0.3579(3) 0.59842(15) 0.0521(7) Uani 1 1 d . . . H39A H 0.3775(16) -0.3322(16) 0.5616(10) 0.024(6) Uiso 1 1 d . . . H39B H 0.357(2) -0.359(2) 0.6289(12) 0.062(8) Uiso 1 1 d . . . H39C H 0.431(2) -0.430(2) 0.5750(14) 0.084(10) Uiso 1 1 d . . . C40 C 0.42814(16) 0.10505(16) 0.67347(9) 0.0260(4) Uani 1 1 d . . . C41 C 0.43079(17) 0.20339(16) 0.66011(9) 0.0281(5) Uani 1 1 d . . . C42 C 0.32953(19) 0.25493(19) 0.65569(11) 0.0339(5) Uani 1 1 d . . . H42 H 0.3308(16) 0.3175(15) 0.6455(9) 0.022(5) Uiso 1 1 d . . . C43 C 0.22851(19) 0.2116(2) 0.66408(11) 0.0377(6) Uani 1 1 d . . . H43 H 0.1596(17) 0.2469(16) 0.6606(10) 0.033(6) Uiso 1 1 d . . . C44 C 0.22801(19) 0.1170(2) 0.67819(11) 0.0362(5) Uani 1 1 d . . . H44 H 0.1602(16) 0.0881(15) 0.6848(9) 0.025(5) Uiso 1 1 d . . . C45 C 0.32683(17) 0.06156(18) 0.68385(10) 0.0302(5) Uani 1 1 d . . . C46 C 0.53962(18) 0.24902(17) 0.64851(11) 0.0299(5) Uani 1 1 d . . . H46 H 0.6002(16) 0.2280(15) 0.6773(9) 0.026(5) Uiso 1 1 d . . . C47 C 0.5520(2) 0.3690(2) 0.66662(14) 0.0432(6) Uani 1 1 d . . . H47A H 0.498(2) 0.393(2) 0.6343(12) 0.061(8) Uiso 1 1 d . . . H47B H 0.6333(19) 0.3906(17) 0.6631(10) 0.042(6) Uiso 1 1 d . . . H47C H 0.545(2) 0.401(2) 0.7146(13) 0.061(8) Uiso 1 1 d . . . C48 C 0.5495(2) 0.2027(2) 0.57516(12) 0.0367(5) Uani 1 1 d . . . H48A H 0.5406(19) 0.127(2) 0.5600(11) 0.049(7) Uiso 1 1 d . . . H48B H 0.6260(18) 0.2293(17) 0.5674(10) 0.044(6) Uiso 1 1 d . . . H48C H 0.4887(17) 0.2214(16) 0.5460(10) 0.029(6) Uiso 1 1 d . . . C49 C 0.32191(18) -0.04063(19) 0.70239(12) 0.0362(5) Uani 1 1 d . . . H49 H 0.3974(16) -0.0658(15) 0.7074(9) 0.025(5) Uiso 1 1 d . . . C50 C 0.2861(3) -0.0258(3) 0.77009(17) 0.0536(8) Uani 1 1 d . . . H50A H 0.341(3) 0.021(2) 0.8057(15) 0.095(12) Uiso 1 1 d . . . H50B H 0.287(2) -0.090(2) 0.7790(12) 0.051(8) Uiso 1 1 d . . . H50C H 0.207(2) 0.0039(19) 0.7676(11) 0.054(7) Uiso 1 1 d . . . C51 C 0.2444(3) -0.1272(3) 0.64590(19) 0.0612(8) Uani 1 1 d . . . H51A H 0.162(2) -0.105(2) 0.6420(13) 0.074(9) Uiso 1 1 d . . . H51B H 0.2420(19) -0.192(2) 0.6586(11) 0.051(7) Uiso 1 1 d . . . H51C H 0.267(2) -0.139(2) 0.6040(14) 0.073(10) Uiso 1 1 d . . . C52 C 0.9207(2) -0.1142(2) 0.73341(12) 0.0358(5) Uani 1 1 d . . . H52A H 0.9554(14) -0.0521(15) 0.7305(8) 0.013(5) Uiso 1 1 d . . . H52B H 0.881(2) -0.165(2) 0.6945(12) 0.055(8) Uiso 1 1 d . . . C53 C 1.0122(2) -0.1688(2) 0.77224(16) 0.0518(7) Uani 1 1 d . . . H53A H 1.038(2) -0.222(2) 0.7355(13) 0.072(9) Uiso 1 1 d . . . H53B H 1.084(2) -0.107(2) 0.8120(13) 0.072(8) Uiso 1 1 d . . . C54 C 0.9425(2) -0.2201(2) 0.80835(15) 0.0448(6) Uani 1 1 d . . . H54A H 0.894(2) -0.286(2) 0.7725(12) 0.063(8) Uiso 1 1 d . . . H54B H 0.987(2) -0.236(2) 0.8469(12) 0.059(8) Uiso 1 1 d . . . C55 C 0.8637(2) -0.13742(19) 0.83154(12) 0.0358(5) Uani 1 1 d . . . H55A H 0.7915(18) -0.1650(17) 0.8324(10) 0.039(7) Uiso 1 1 d . . . H55B H 0.9042(17) -0.0822(17) 0.8754(11) 0.039(6) Uiso 1 1 d . . . C56 C 0.7278(2) 0.30269(18) 0.84577(12) 0.0366(5) Uani 1 1 d . . . H56A H 0.722(2) 0.3248(19) 0.8032(12) 0.063(8) Uiso 1 1 d . . . H56B H 0.8103(18) 0.2938(17) 0.8675(10) 0.043(7) Uiso 1 1 d . . . C57 C 0.6684(2) 0.3733(2) 0.89560(14) 0.0453(6) Uani 1 1 d . . . H57A H 0.6975(18) 0.3660(17) 0.9414(11) 0.042(7) Uiso 1 1 d . . . H57B H 0.6772(19) 0.4434(19) 0.8980(11) 0.049(7) Uiso 1 1 d . . . C58 C 0.5439(2) 0.3280(2) 0.87088(16) 0.0488(7) Uani 1 1 d . . . H58A H 0.5038(17) 0.3490(17) 0.9073(11) 0.037(6) Uiso 1 1 d . . . H58B H 0.500(3) 0.340(3) 0.826(2) 0.155(16) Uiso 1 1 d . . . C59 C 0.5545(2) 0.21203(19) 0.84979(12) 0.0348(5) Uani 1 1 d . . . H59A H 0.5616(17) 0.1858(17) 0.8877(11) 0.038(6) Uiso 1 1 d . . . H59B H 0.4919(18) 0.1688(17) 0.8122(11) 0.040(6) Uiso 1 1 d . . . C60 C 1.0723(3) 0.5608(3) 0.94885(18) 0.0668(9) Uani 1 1 d . . . H60A H 1.129(4) 0.628(4) 0.957(2) 0.18(2) Uiso 1 1 d . . . H60B H 1.098(5) 0.476(5) 0.910(3) 0.29(3) Uiso 1 1 d . . . H60C H 1.073(2) 0.597(2) 1.0011(14) 0.069(9) Uiso 1 1 d . . . C61 C 0.95316(19) 0.58255(19) 0.91521(12) 0.0402(6) Uani 1 1 d . . . C62 C 0.8894(2) 0.6554(2) 0.94883(13) 0.0494(7) Uani 1 1 d . . . H62 H 0.929(2) 0.694(2) 0.9941(12) 0.064(8) Uiso 1 1 d . . . C63 C 0.7837(3) 0.6768(2) 0.91874(15) 0.0559(7) Uani 1 1 d . . . H63 H 0.742(2) 0.734(2) 0.9455(14) 0.085(10) Uiso 1 1 d . . . C64 C 0.7357(2) 0.6251(2) 0.85267(15) 0.0513(7) Uani 1 1 d . . . H64 H 0.655(2) 0.642(2) 0.8326(12) 0.069(8) Uiso 1 1 d . . . C65 C 0.7934(3) 0.5509(2) 0.81634(13) 0.0516(8) Uani 1 1 d . . . H65 H 0.760(2) 0.5179(19) 0.7735(12) 0.053(8) Uiso 1 1 d . . . C66 C 0.9041(3) 0.5287(2) 0.84724(14) 0.0488(7) Uani 1 1 d . . . H66 H 0.941(2) 0.484(2) 0.8264(13) 0.059(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.02352(11) 0.02308(11) 0.02392(11) 0.00964(8) 0.00349(8) 0.00288(8) O1 0.0309(8) 0.0317(8) 0.0335(8) 0.0178(7) 0.0062(6) 0.0105(6) O2 0.0337(8) 0.0236(8) 0.0338(8) 0.0078(6) 0.0091(6) 0.0014(6) N1 0.0268(9) 0.0307(10) 0.0411(11) 0.0166(8) 0.0073(8) 0.0066(8) N2 0.0455(12) 0.0439(13) 0.0422(12) 0.0125(10) 0.0112(9) 0.0092(10) N3 0.0356(10) 0.0254(10) 0.0261(9) 0.0087(7) 0.0091(8) 0.0028(8) N4 0.0308(9) 0.0283(10) 0.0378(10) 0.0132(8) 0.0115(8) 0.0059(8) N5 0.0210(8) 0.0258(9) 0.0237(8) 0.0085(7) 0.0049(7) 0.0071(7) N6 0.0230(8) 0.0261(9) 0.0236(8) 0.0083(7) 0.0046(7) 0.0083(7) C1 0.0286(11) 0.0335(13) 0.0431(13) 0.0178(10) 0.0092(10) 0.0062(10) C2 0.0351(12) 0.0266(12) 0.0438(13) 0.0131(10) 0.0193(10) 0.0102(10) C3 0.0296(11) 0.0222(11) 0.0419(13) 0.0008(9) 0.0201(10) 0.0008(9) C4 0.0238(10) 0.0248(11) 0.0349(12) 0.0061(9) 0.0098(9) 0.0050(9) C5 0.0334(12) 0.0351(13) 0.0342(12) 0.0051(10) 0.0076(10) 0.0077(10) C6 0.0373(13) 0.0524(17) 0.0323(13) 0.0030(11) 0.0038(11) 0.0131(12) C7 0.0278(12) 0.0489(17) 0.0504(15) -0.0024(12) 0.0114(11) -0.0057(11) C8 0.0390(13) 0.0387(14) 0.0426(14) 0.0060(11) 0.0144(11) -0.0022(11) C9 0.0321(12) 0.0295(13) 0.0489(14) 0.0040(10) 0.0202(11) 0.0021(10) C10 0.0681(17) 0.0470(16) 0.0406(14) 0.0266(12) 0.0205(13) 0.0228(13) C11 0.133(3) 0.129(3) 0.069(2) 0.071(2) -0.021(2) -0.053(3) C12 0.135(3) 0.089(3) 0.111(3) 0.074(2) 0.077(2) 0.075(2) C13 0.083(2) 0.071(2) 0.0635(19) 0.0383(16) 0.0268(16) 0.0126(17) C14 0.0288(11) 0.0257(11) 0.0257(11) 0.0091(9) 0.0025(9) 0.0048(9) C15 0.0272(10) 0.0278(11) 0.0284(11) 0.0116(9) 0.0088(9) 0.0068(9) C16 0.0321(11) 0.0313(12) 0.0275(11) 0.0117(9) 0.0089(9) 0.0085(9) C17 0.0316(11) 0.0262(11) 0.0240(10) 0.0067(8) 0.0055(9) 0.0054(9) C18 0.0418(13) 0.0332(13) 0.0330(12) 0.0100(10) 0.0083(10) 0.0015(10) C19 0.0523(15) 0.0441(16) 0.0338(13) 0.0026(11) -0.0016(12) -0.0087(12) C20 0.0643(17) 0.0594(18) 0.0251(12) 0.0103(12) 0.0025(12) -0.0044(14) C21 0.0510(15) 0.0494(16) 0.0285(12) 0.0149(11) 0.0115(11) 0.0041(12) C22 0.0290(11) 0.0349(13) 0.0336(12) 0.0190(10) 0.0112(10) 0.0105(10) C23 0.0293(11) 0.0320(13) 0.0451(13) 0.0176(10) 0.0130(10) 0.0063(10) C24 0.0353(12) 0.0368(14) 0.0566(15) 0.0149(12) 0.0114(11) 0.0063(11) C25 0.0416(14) 0.0279(13) 0.0785(18) 0.0171(13) 0.0223(13) 0.0054(11) C26 0.0464(14) 0.0500(17) 0.0614(17) 0.0344(14) 0.0081(13) -0.0060(12) C27 0.0243(10) 0.0287(12) 0.0252(11) 0.0121(9) 0.0057(9) 0.0040(9) C28 0.0231(10) 0.0302(12) 0.0203(10) 0.0062(8) 0.0024(8) 0.0071(9) C29 0.0249(10) 0.0398(13) 0.0246(11) 0.0108(9) 0.0033(9) 0.0075(10) C30 0.0314(12) 0.0505(16) 0.0305(12) 0.0105(11) 0.0135(10) 0.0124(11) C31 0.0478(14) 0.0385(15) 0.0357(13) 0.0068(11) 0.0146(11) 0.0173(12) C32 0.0468(14) 0.0281(13) 0.0356(13) 0.0076(10) 0.0125(11) 0.0101(11) C33 0.0301(11) 0.0293(12) 0.0252(11) 0.0077(9) 0.0040(9) 0.0092(9) C34 0.0320(12) 0.0469(15) 0.0266(12) 0.0083(10) 0.0079(10) 0.0007(11) C35 0.0361(15) 0.078(3) 0.070(2) 0.032(2) 0.0141(15) 0.0033(16) C36 0.0427(15) 0.0370(15) 0.0444(15) 0.0119(12) 0.0068(12) 0.0045(12) C37 0.0374(12) 0.0233(12) 0.0334(12) 0.0069(9) 0.0122(10) 0.0053(10) C38 0.0530(16) 0.0383(15) 0.0425(14) 0.0186(12) 0.0199(13) 0.0119(13) C39 0.0458(16) 0.0529(19) 0.0485(17) 0.0020(14) 0.0098(14) -0.0055(14) C40 0.0253(10) 0.0312(12) 0.0197(10) 0.0064(8) 0.0023(8) 0.0102(9) C41 0.0300(11) 0.0291(12) 0.0222(10) 0.0040(8) 0.0030(9) 0.0121(9) C42 0.0378(13) 0.0345(13) 0.0307(12) 0.0112(10) 0.0071(10) 0.0179(11) C43 0.0344(13) 0.0483(15) 0.0347(13) 0.0141(11) 0.0127(10) 0.0235(11) C44 0.0257(11) 0.0495(16) 0.0381(13) 0.0161(11) 0.0118(10) 0.0131(11) C45 0.0251(11) 0.0396(13) 0.0278(11) 0.0122(9) 0.0066(9) 0.0107(9) C46 0.0296(11) 0.0273(12) 0.0329(12) 0.0116(9) 0.0033(10) 0.0086(9) C47 0.0478(16) 0.0320(14) 0.0477(16) 0.0100(12) 0.0086(13) 0.0064(12) C48 0.0355(13) 0.0356(15) 0.0391(14) 0.0103(11) 0.0092(11) 0.0037(11) C49 0.0239(11) 0.0450(15) 0.0473(14) 0.0232(11) 0.0106(11) 0.0117(10) C50 0.0479(17) 0.064(2) 0.072(2) 0.0406(18) 0.0326(16) 0.0147(16) C51 0.0535(19) 0.0436(19) 0.080(2) 0.0204(17) -0.0009(17) 0.0056(15) C52 0.0349(13) 0.0351(14) 0.0414(14) 0.0133(11) 0.0136(11) 0.0090(11) C53 0.0405(15) 0.0517(18) 0.078(2) 0.0389(16) 0.0173(15) 0.0145(13) C54 0.0402(14) 0.0436(16) 0.0602(18) 0.0311(14) 0.0094(13) 0.0157(12) C55 0.0403(14) 0.0314(13) 0.0397(14) 0.0216(11) 0.0028(11) 0.0079(11) C56 0.0496(15) 0.0222(12) 0.0368(13) 0.0055(10) 0.0123(12) -0.0036(11) C57 0.0574(17) 0.0279(14) 0.0495(16) 0.0045(12) 0.0191(14) 0.0007(12) C58 0.0522(16) 0.0360(15) 0.0627(18) 0.0140(13) 0.0224(15) 0.0144(12) C59 0.0333(12) 0.0332(13) 0.0366(13) 0.0050(11) 0.0118(11) 0.0042(10) C60 0.0492(17) 0.093(3) 0.072(2) 0.043(2) 0.0164(16) 0.0223(18) C61 0.0372(13) 0.0464(15) 0.0472(15) 0.0280(12) 0.0118(11) 0.0082(11) C62 0.0553(16) 0.0518(18) 0.0382(15) 0.0071(13) 0.0127(13) 0.0056(14) C63 0.0624(18) 0.0526(19) 0.0600(19) 0.0232(15) 0.0193(16) 0.0210(15) C64 0.0440(15) 0.0591(19) 0.0645(19) 0.0397(16) 0.0126(15) 0.0090(14) C65 0.0659(19) 0.0506(18) 0.0329(14) 0.0133(13) 0.0012(14) -0.0257(15) C66 0.0674(19) 0.0293(14) 0.0630(18) 0.0144(13) 0.0411(16) 0.0100(13) _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 N3 2.2857(16) . ? Y1 N1 2.2901(17) . ? Y1 O1 2.3544(14) . ? Y1 N6 2.3602(16) . ? Y1 O2 2.3608(14) . ? Y1 N5 2.3633(15) . ? Y1 C27 2.757(2) . ? O1 C52 1.462(3) . ? O1 C55 1.473(2) . ? O2 C56 1.468(3) . ? O2 C59 1.474(2) . ? N1 C1 1.381(3) . ? N1 C4 1.400(2) . ? N2 C9 1.233(3) . ? N2 C10 1.501(3) . ? N3 C14 1.373(2) . ? N3 C17 1.397(2) . ? N4 C22 1.275(3) . ? N4 C23 1.477(3) . ? N5 C27 1.328(2) . ? N5 C28 1.440(2) . ? N6 C27 1.322(2) . ? N6 C40 1.435(2) . ? C1 C2 1.372(3) . ? C1 H1 0.9500 . ? C2 C3 1.438(3) . ? C2 C9 1.495(3) . ? C3 C8 1.390(3) . ? C3 C4 1.423(3) . ? C4 C5 1.388(3) . ? C5 C6 1.385(3) . ? C5 H5 0.9500 . ? C6 C7 1.419(3) . ? C6 H6 0.9500 . ? C7 C8 1.363(3) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C13 1.500(3) . ? C10 C11 1.511(4) . ? C10 C12 1.526(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.386(3) . ? C14 H14 0.9500 . ? C15 C16 1.428(3) . ? C15 C22 1.454(3) . ? C16 C21 1.396(3) . ? C16 C17 1.411(3) . ? C17 C18 1.400(3) . ? C18 C19 1.372(3) . ? C18 H18 0.9500 . ? C19 C20 1.402(3) . ? C19 H19 0.9500 . ? C20 C21 1.375(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C25 1.523(3) . ? C23 C24 1.528(3) . ? C23 C26 1.531(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27 1.063(19) . ? C28 C33 1.408(3) . ? C28 C29 1.412(3) . ? C29 C30 1.403(3) . ? C29 C34 1.509(3) . ? C30 C31 1.374(3) . ? C30 H30 0.93(2) . ? C31 C32 1.381(3) . ? C31 H31 1.02(2) . ? C32 C33 1.397(3) . ? C32 H32 0.99(2) . ? C33 C37 1.515(3) . ? C34 C36 1.524(3) . ? C34 C35 1.540(3) . ? C34 H34 0.920(18) . ? C35 H35A 1.01(3) . ? C35 H35B 0.93(2) . ? C35 H35C 1.03(3) . ? C36 H36A 1.00(2) . ? C36 H36B 0.98(2) . ? C36 H36C 0.97(2) . ? C37 C39 1.524(3) . ? C37 C38 1.529(3) . ? C37 H37 0.96(2) . ? C38 H38A 0.99(2) . ? C38 H38B 0.98(2) . ? C38 H38C 1.02(2) . ? C39 H39A 0.95(2) . ? C39 H39B 1.03(2) . ? C39 H39C 0.99(3) . ? C40 C45 1.409(3) . ? C40 C41 1.417(3) . ? C41 C42 1.394(3) . ? C41 C46 1.512(3) . ? C42 C43 1.387(3) . ? C42 H42 0.918(19) . ? C43 C44 1.374(3) . ? C43 H43 0.95(2) . ? C44 C45 1.399(3) . ? C44 H44 0.938(18) . ? C45 C49 1.522(3) . ? C46 C48 1.521(3) . ? C46 C47 1.534(3) . ? C46 H46 0.935(19) . ? C47 H47A 0.96(3) . ? C47 H47B 1.03(2) . ? C47 H47C 1.00(2) . ? C48 H48A 0.96(2) . ? C48 H48B 1.03(2) . ? C48 H48C 0.93(2) . ? C49 C51 1.518(4) . ? C49 C50 1.531(4) . ? C49 H49 0.957(19) . ? C50 H50A 0.94(3) . ? C50 H50B 0.92(3) . ? C50 H50C 1.03(2) . ? C51 H51A 1.02(3) . ? C51 H51B 0.98(3) . ? C51 H51C 0.95(3) . ? C52 C53 1.533(3) . ? C52 H52A 0.941(18) . ? C52 H52B 0.93(2) . ? C53 C54 1.505(3) . ? C53 H53A 0.99(3) . ? C53 H53B 1.18(2) . ? C54 C55 1.506(3) . ? C54 H54A 1.04(2) . ? C54 H54B 0.95(2) . ? C55 H55A 0.93(2) . ? C55 H55B 1.02(2) . ? C56 C57 1.507(3) . ? C56 H56A 1.01(2) . ? C56 H56B 1.01(2) . ? C57 C58 1.508(4) . ? C57 H57A 0.98(2) . ? C57 H57B 0.93(2) . ? C58 C59 1.501(3) . ? C58 H58A 0.97(2) . ? C58 H58B 1.03(4) . ? C59 H59A 0.94(2) . ? C59 H59B 0.99(2) . ? C60 C61 1.509(3) . ? C60 H60A 1.06(5) . ? C60 H60B 1.27(6) . ? C60 H60C 1.06(3) . ? C61 C62 1.375(3) . ? C61 C66 1.392(3) . ? C62 C63 1.351(4) . ? C62 H62 0.96(2) . ? C63 C64 1.352(4) . ? C63 H63 1.02(3) . ? C64 C65 1.364(4) . ? C64 H64 1.01(3) . ? C65 C66 1.409(4) . ? C65 H65 0.88(2) . ? C66 H66 0.83(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 N3 Y1 N1 136.42(6) . . ? N3 Y1 O1 80.20(5) . . ? N1 Y1 O1 82.66(5) . . ? N3 Y1 N6 106.39(6) . . ? N1 Y1 N6 111.52(6) . . ? O1 Y1 N6 142.42(5) . . ? N3 Y1 O2 80.79(5) . . ? N1 Y1 O2 82.99(5) . . ? O1 Y1 O2 133.93(5) . . ? N6 Y1 O2 83.35(5) . . ? N3 Y1 N5 114.69(6) . . ? N1 Y1 N5 103.63(6) . . ? O1 Y1 N5 85.97(5) . . ? N6 Y1 N5 57.32(5) . . ? O2 Y1 N5 140.02(5) . . ? N3 Y1 C27 111.95(6) . . ? N1 Y1 C27 111.62(6) . . ? O1 Y1 C27 114.11(5) . . ? N6 Y1 C27 28.63(5) . . ? O2 Y1 C27 111.89(5) . . ? N5 Y1 C27 28.77(5) . . ? C52 O1 C55 109.43(16) . . ? C52 O1 Y1 120.71(12) . . ? C55 O1 Y1 129.84(12) . . ? C56 O2 C59 108.93(16) . . ? C56 O2 Y1 129.86(12) . . ? C59 O2 Y1 121.12(12) . . ? C1 N1 C4 104.06(17) . . ? C1 N1 Y1 115.89(13) . . ? C4 N1 Y1 138.02(14) . . ? C9 N2 C10 117.8(2) . . ? C14 N3 C17 104.22(16) . . ? C14 N3 Y1 124.59(13) . . ? C17 N3 Y1 130.51(13) . . ? C22 N4 C23 121.64(18) . . ? C27 N5 C28 119.96(16) . . ? C27 N5 Y1 92.29(12) . . ? C28 N5 Y1 147.50(12) . . ? C27 N6 C40 120.63(16) . . ? C27 N6 Y1 92.58(12) . . ? C40 N6 Y1 145.23(12) . . ? C2 C1 N1 114.55(19) . . ? C2 C1 H1 122.7 . . ? N1 C1 H1 122.7 . . ? C1 C2 C3 104.67(19) . . ? C1 C2 C9 122.5(2) . . ? C3 C2 C9 132.9(2) . . ? C8 C3 C4 119.4(2) . . ? C8 C3 C2 134.0(2) . . ? C4 C3 C2 106.61(17) . . ? C5 C4 N1 127.45(19) . . ? C5 C4 C3 122.45(19) . . ? N1 C4 C3 110.09(18) . . ? C6 C5 C4 117.0(2) . . ? C6 C5 H5 121.5 . . ? C4 C5 H5 121.5 . . ? C5 C6 C7 120.4(2) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 122.4(2) . . ? C8 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? C7 C8 C3 118.3(2) . . ? C7 C8 H8 120.9 . . ? C3 C8 H8 120.9 . . ? N2 C9 C2 121.5(2) . . ? N2 C9 H9 119.2 . . ? C2 C9 H9 119.2 . . ? C13 C10 N2 104.8(2) . . ? C13 C10 C11 109.7(2) . . ? N2 C10 C11 114.3(2) . . ? C13 C10 C12 109.5(2) . . ? N2 C10 C12 106.43(19) . . ? C11 C10 C12 111.7(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 C15 113.64(18) . . ? N3 C14 H14 123.2 . . ? C15 C14 H14 123.2 . . ? C14 C15 C16 105.02(18) . . ? C14 C15 C22 126.35(19) . . ? C16 C15 C22 128.57(18) . . ? C21 C16 C17 119.08(19) . . ? C21 C16 C15 134.5(2) . . ? C17 C16 C15 106.42(17) . . ? N3 C17 C18 127.59(19) . . ? N3 C17 C16 110.70(17) . . ? C18 C17 C16 121.68(18) . . ? C19 C18 C17 118.0(2) . . ? C19 C18 H18 121.0 . . ? C17 C18 H18 121.0 . . ? C18 C19 C20 120.7(2) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C21 C20 C19 121.7(2) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C20 C21 C16 118.8(2) . . ? C20 C21 H21 120.6 . . ? C16 C21 H21 120.6 . . ? N4 C22 C15 122.82(19) . . ? N4 C22 H22 118.6 . . ? C15 C22 H22 118.6 . . ? N4 C23 C25 105.79(17) . . ? N4 C23 C24 106.33(18) . . ? C25 C23 C24 109.74(19) . . ? N4 C23 C26 115.65(18) . . ? C25 C23 C26 109.3(2) . . ? C24 C23 C26 109.81(18) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N6 C27 N5 117.49(18) . . ? N6 C27 Y1 58.79(10) . . ? N5 C27 Y1 58.94(10) . . ? N6 C27 H27 121.1(11) . . ? N5 C27 H27 121.3(11) . . ? Y1 C27 H27 172.3(10) . . ? C33 C28 C29 121.25(19) . . ? C33 C28 N5 120.93(17) . . ? C29 C28 N5 117.70(18) . . ? C30 C29 C28 117.2(2) . . ? C30 C29 C34 120.92(19) . . ? C28 C29 C34 121.86(19) . . ? C31 C30 C29 122.2(2) . . ? C31 C30 H30 123.7(14) . . ? C29 C30 H30 114.1(14) . . ? C30 C31 C32 119.9(2) . . ? C30 C31 H31 120.0(13) . . ? C32 C31 H31 120.1(13) . . ? C31 C32 C33 120.9(2) . . ? C31 C32 H32 118.6(12) . . ? C33 C32 H32 120.5(12) . . ? C32 C33 C28 118.57(19) . . ? C32 C33 C37 118.6(2) . . ? C28 C33 C37 122.68(18) . . ? C29 C34 C36 111.32(18) . . ? C29 C34 C35 113.2(2) . . ? C36 C34 C35 109.5(2) . . ? C29 C34 H34 106.6(12) . . ? C36 C34 H34 110.8(13) . . ? C35 C34 H34 105.3(12) . . ? C34 C35 H35A 114.1(15) . . ? C34 C35 H35B 100.9(16) . . ? H35A C35 H35B 108(2) . . ? C34 C35 H35C 112.3(14) . . ? H35A C35 H35C 104(2) . . ? H35B C35 H35C 119(2) . . ? C34 C36 H36A 108.9(13) . . ? C34 C36 H36B 109.7(13) . . ? H36A C36 H36B 102.5(17) . . ? C34 C36 H36C 112.9(14) . . ? H36A C36 H36C 107.5(18) . . ? H36B C36 H36C 114.6(19) . . ? C33 C37 C39 113.90(19) . . ? C33 C37 C38 109.90(18) . . ? C39 C37 C38 109.4(2) . . ? C33 C37 H37 107.5(12) . . ? C39 C37 H37 106.5(11) . . ? C38 C37 H37 109.6(11) . . ? C37 C38 H38A 109.3(13) . . ? C37 C38 H38B 109.0(14) . . ? H38A C38 H38B 109.1(19) . . ? C37 C38 H38C 111.3(14) . . ? H38A C38 H38C 108.6(18) . . ? H38B C38 H38C 109.4(18) . . ? C37 C39 H39A 107.2(12) . . ? C37 C39 H39B 111.9(13) . . ? H39A C39 H39B 109.0(18) . . ? C37 C39 H39C 113.2(16) . . ? H39A C39 H39C 103(2) . . ? H39B C39 H39C 112(2) . . ? C45 C40 C41 121.00(18) . . ? C45 C40 N6 120.14(18) . . ? C41 C40 N6 118.69(17) . . ? C42 C41 C40 118.3(2) . . ? C42 C41 C46 121.1(2) . . ? C40 C41 C46 120.61(17) . . ? C43 C42 C41 121.2(2) . . ? C43 C42 H42 120.7(12) . . ? C41 C42 H42 118.0(12) . . ? C44 C43 C42 119.8(2) . . ? C44 C43 H43 119.5(13) . . ? C42 C43 H43 120.8(13) . . ? C43 C44 C45 122.0(2) . . ? C43 C44 H44 120.0(12) . . ? C45 C44 H44 118.0(13) . . ? C44 C45 C40 117.8(2) . . ? C44 C45 C49 119.38(19) . . ? C40 C45 C49 122.85(18) . . ? C41 C46 C48 110.90(18) . . ? C41 C46 C47 114.83(18) . . ? C48 C46 C47 109.2(2) . . ? C41 C46 H46 104.6(12) . . ? C48 C46 H46 108.6(12) . . ? C47 C46 H46 108.5(12) . . ? C46 C47 H47A 111.2(15) . . ? C46 C47 H47B 107.4(13) . . ? H47A C47 H47B 106.8(19) . . ? C46 C47 H47C 110.8(15) . . ? H47A C47 H47C 112(2) . . ? H47B C47 H47C 108.3(18) . . ? C46 C48 H48A 113.6(14) . . ? C46 C48 H48B 111.7(11) . . ? H48A C48 H48B 109.9(18) . . ? C46 C48 H48C 109.4(12) . . ? H48A C48 H48C 103.5(17) . . ? H48B C48 H48C 108.2(17) . . ? C51 C49 C45 112.4(2) . . ? C51 C49 C50 110.9(3) . . ? C45 C49 C50 111.9(2) . . ? C51 C49 H49 104.8(12) . . ? C45 C49 H49 108.9(12) . . ? C50 C49 H49 107.7(11) . . ? C49 C50 H50A 109.7(18) . . ? C49 C50 H50B 107.7(15) . . ? H50A C50 H50B 108(2) . . ? C49 C50 H50C 110.2(13) . . ? H50A C50 H50C 109(2) . . ? H50B C50 H50C 113(2) . . ? C49 C51 H51A 106.4(15) . . ? C49 C51 H51B 111.5(14) . . ? H51A C51 H51B 105(2) . . ? C49 C51 H51C 111.7(17) . . ? H51A C51 H51C 112(2) . . ? H51B C51 H51C 111(2) . . ? O1 C52 C53 103.89(19) . . ? O1 C52 H52A 106.6(11) . . ? C53 C52 H52A 109.3(11) . . ? O1 C52 H52B 107.8(14) . . ? C53 C52 H52B 107.0(16) . . ? H52A C52 H52B 121.0(18) . . ? C54 C53 C52 102.4(2) . . ? C54 C53 H53A 111.2(16) . . ? C52 C53 H53A 103.9(16) . . ? C54 C53 H53B 110.5(12) . . ? C52 C53 H53B 110.4(13) . . ? H53A C53 H53B 117.2(19) . . ? C53 C54 C55 102.6(2) . . ? C53 C54 H54A 107.9(14) . . ? C55 C54 H54A 110.2(14) . . ? C53 C54 H54B 113.9(14) . . ? C55 C54 H54B 109.0(15) . . ? H54A C54 H54B 113(2) . . ? O1 C55 C54 105.06(19) . . ? O1 C55 H55A 106.0(13) . . ? C54 C55 H55A 113.3(14) . . ? O1 C55 H55B 105.5(12) . . ? C54 C55 H55B 111.7(12) . . ? H55A C55 H55B 114.4(17) . . ? O2 C56 C57 105.04(18) . . ? O2 C56 H56A 107.0(14) . . ? C57 C56 H56A 112.2(14) . . ? O2 C56 H56B 107.2(13) . . ? C57 C56 H56B 112.4(12) . . ? H56A C56 H56B 112.4(18) . . ? C56 C57 C58 103.1(2) . . ? C56 C57 H57A 110.1(13) . . ? C58 C57 H57A 107.8(13) . . ? C56 C57 H57B 114.1(14) . . ? C58 C57 H57B 113.0(14) . . ? H57A C57 H57B 108.5(19) . . ? C59 C58 C57 103.0(2) . . ? C59 C58 H58A 112.3(13) . . ? C57 C58 H58A 110.1(12) . . ? C59 C58 H58B 102(2) . . ? C57 C58 H58B 116(2) . . ? H58A C58 H58B 113(2) . . ? O2 C59 C58 105.04(19) . . ? O2 C59 H59A 109.3(13) . . ? C58 C59 H59A 110.2(13) . . ? O2 C59 H59B 106.8(12) . . ? C58 C59 H59B 116.6(13) . . ? H59A C59 H59B 108.6(18) . . ? C61 C60 H60A 107(2) . . ? C61 C60 H60B 107(3) . . ? H60A C60 H60B 115(3) . . ? C61 C60 H60C 100.2(14) . . ? H60A C60 H60C 82(2) . . ? H60B C60 H60C 140(3) . . ? C62 C61 C66 117.4(2) . . ? C62 C61 C60 122.6(3) . . ? C66 C61 C60 120.0(3) . . ? C63 C62 C61 123.0(3) . . ? C63 C62 H62 122.3(15) . . ? C61 C62 H62 114.5(15) . . ? C62 C63 C64 119.9(3) . . ? C62 C63 H63 119.5(16) . . ? C64 C63 H63 120.6(16) . . ? C63 C64 C65 120.3(3) . . ? C63 C64 H64 117.3(15) . . ? C65 C64 H64 122.5(15) . . ? C64 C65 C66 120.2(3) . . ? C64 C65 H65 118.5(17) . . ? C66 C65 H65 121.3(17) . . ? C61 C66 C65 119.3(2) . . ? C61 C66 H66 118.5(18) . . ? C65 C66 H66 122.3(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Y1 O1 C52 170.51(16) . . . . ? N1 Y1 O1 C52 -49.72(16) . . . . ? N6 Y1 O1 C52 66.33(18) . . . . ? O2 Y1 O1 C52 -122.57(15) . . . . ? N5 Y1 O1 C52 54.59(16) . . . . ? C27 Y1 O1 C52 60.73(16) . . . . ? N3 Y1 O1 C55 -7.68(17) . . . . ? N1 Y1 O1 C55 132.09(17) . . . . ? N6 Y1 O1 C55 -111.86(17) . . . . ? O2 Y1 O1 C55 59.24(19) . . . . ? N5 Y1 O1 C55 -123.59(17) . . . . ? C27 Y1 O1 C55 -117.46(17) . . . . ? N3 Y1 O2 C56 138.06(18) . . . . ? N1 Y1 O2 C56 -1.34(17) . . . . ? O1 Y1 O2 C56 71.37(19) . . . . ? N6 Y1 O2 C56 -114.08(18) . . . . ? N5 Y1 O2 C56 -104.22(18) . . . . ? C27 Y1 O2 C56 -111.88(17) . . . . ? N3 Y1 O2 C59 -45.90(15) . . . . ? N1 Y1 O2 C59 174.70(15) . . . . ? O1 Y1 O2 C59 -112.59(15) . . . . ? N6 Y1 O2 C59 61.96(15) . . . . ? N5 Y1 O2 C59 71.82(17) . . . . ? C27 Y1 O2 C59 64.16(15) . . . . ? N3 Y1 N1 C1 -151.41(14) . . . . ? O1 Y1 N1 C1 141.19(15) . . . . ? N6 Y1 N1 C1 -2.73(16) . . . . ? O2 Y1 N1 C1 -82.71(15) . . . . ? N5 Y1 N1 C1 57.17(15) . . . . ? C27 Y1 N1 C1 28.11(16) . . . . ? N3 Y1 N1 C4 9.2(2) . . . . ? O1 Y1 N1 C4 -58.2(2) . . . . ? N6 Y1 N1 C4 157.86(19) . . . . ? O2 Y1 N1 C4 77.9(2) . . . . ? N5 Y1 N1 C4 -142.24(19) . . . . ? C27 Y1 N1 C4 -171.30(19) . . . . ? N1 Y1 N3 C14 -157.64(14) . . . . ? O1 Y1 N3 C14 -89.33(16) . . . . ? N6 Y1 N3 C14 52.62(16) . . . . ? O2 Y1 N3 C14 132.83(16) . . . . ? N5 Y1 N3 C14 -8.41(17) . . . . ? C27 Y1 N3 C14 22.84(17) . . . . ? N1 Y1 N3 C17 11.3(2) . . . . ? O1 Y1 N3 C17 79.64(17) . . . . ? N6 Y1 N3 C17 -138.42(16) . . . . ? O2 Y1 N3 C17 -58.21(17) . . . . ? N5 Y1 N3 C17 160.55(16) . . . . ? C27 Y1 N3 C17 -168.20(16) . . . . ? N3 Y1 N5 C27 91.02(12) . . . . ? N1 Y1 N5 C27 -110.26(12) . . . . ? O1 Y1 N5 C27 168.30(12) . . . . ? N6 Y1 N5 C27 -3.23(11) . . . . ? O2 Y1 N5 C27 -14.88(15) . . . . ? N3 Y1 N5 C28 -82.2(2) . . . . ? N1 Y1 N5 C28 76.6(2) . . . . ? O1 Y1 N5 C28 -4.9(2) . . . . ? N6 Y1 N5 C28 -176.4(3) . . . . ? O2 Y1 N5 C28 171.9(2) . . . . ? C27 Y1 N5 C28 -173.2(3) . . . . ? N3 Y1 N6 C27 -105.94(12) . . . . ? N1 Y1 N6 C27 95.99(12) . . . . ? O1 Y1 N6 C27 -10.71(16) . . . . ? O2 Y1 N6 C27 175.73(12) . . . . ? N5 Y1 N6 C27 3.24(11) . . . . ? N3 Y1 N6 C40 57.7(2) . . . . ? N1 Y1 N6 C40 -100.4(2) . . . . ? O1 Y1 N6 C40 152.9(2) . . . . ? O2 Y1 N6 C40 -20.7(2) . . . . ? N5 Y1 N6 C40 166.8(2) . . . . ? C27 Y1 N6 C40 163.6(3) . . . . ? C4 N1 C1 C2 -1.3(2) . . . . ? Y1 N1 C1 C2 165.47(14) . . . . ? N1 C1 C2 C3 0.7(2) . . . . ? N1 C1 C2 C9 -179.67(18) . . . . ? C1 C2 C3 C8 179.1(2) . . . . ? C9 C2 C3 C8 -0.4(4) . . . . ? C1 C2 C3 C4 0.1(2) . . . . ? C9 C2 C3 C4 -179.4(2) . . . . ? C1 N1 C4 C5 -177.5(2) . . . . ? Y1 N1 C4 C5 20.5(3) . . . . ? C1 N1 C4 C3 1.3(2) . . . . ? Y1 N1 C4 C3 -160.75(15) . . . . ? C8 C3 C4 C5 -1.2(3) . . . . ? C2 C3 C4 C5 177.94(19) . . . . ? C8 C3 C4 N1 179.93(18) . . . . ? C2 C3 C4 N1 -0.9(2) . . . . ? N1 C4 C5 C6 178.36(19) . . . . ? C3 C4 C5 C6 -0.3(3) . . . . ? C4 C5 C6 C7 1.5(3) . . . . ? C5 C6 C7 C8 -1.3(4) . . . . ? C6 C7 C8 C3 -0.3(4) . . . . ? C4 C3 C8 C7 1.5(3) . . . . ? C2 C3 C8 C7 -177.4(2) . . . . ? C10 N2 C9 C2 -179.25(19) . . . . ? C1 C2 C9 N2 177.2(2) . . . . ? C3 C2 C9 N2 -3.3(4) . . . . ? C9 N2 C10 C13 -148.1(2) . . . . ? C9 N2 C10 C11 -27.9(3) . . . . ? C9 N2 C10 C12 95.9(3) . . . . ? C17 N3 C14 C15 0.4(2) . . . . ? Y1 N3 C14 C15 171.73(13) . . . . ? N3 C14 C15 C16 0.1(2) . . . . ? N3 C14 C15 C22 -177.28(18) . . . . ? C14 C15 C16 C21 179.3(2) . . . . ? C22 C15 C16 C21 -3.4(4) . . . . ? C14 C15 C16 C17 -0.5(2) . . . . ? C22 C15 C16 C17 176.79(19) . . . . ? C14 N3 C17 C18 177.1(2) . . . . ? Y1 N3 C17 C18 6.4(3) . . . . ? C14 N3 C17 C16 -0.7(2) . . . . ? Y1 N3 C17 C16 -171.31(13) . . . . ? C21 C16 C17 N3 -179.13(19) . . . . ? C15 C16 C17 N3 0.7(2) . . . . ? C21 C16 C17 C18 3.0(3) . . . . ? C15 C16 C17 C18 -177.18(19) . . . . ? N3 C17 C18 C19 -179.1(2) . . . . ? C16 C17 C18 C19 -1.6(3) . . . . ? C17 C18 C19 C20 -0.5(4) . . . . ? C18 C19 C20 C21 1.2(4) . . . . ? C19 C20 C21 C16 0.2(4) . . . . ? C17 C16 C21 C20 -2.2(3) . . . . ? C15 C16 C21 C20 178.0(2) . . . . ? C23 N4 C22 C15 178.86(18) . . . . ? C14 C15 C22 N4 4.0(3) . . . . ? C16 C15 C22 N4 -172.8(2) . . . . ? C22 N4 C23 C25 -133.3(2) . . . . ? C22 N4 C23 C24 110.0(2) . . . . ? C22 N4 C23 C26 -12.2(3) . . . . ? C40 N6 C27 N5 -174.69(17) . . . . ? Y1 N6 C27 N5 -5.48(18) . . . . ? C40 N6 C27 Y1 -169.21(19) . . . . ? C28 N5 C27 N6 -178.76(17) . . . . ? Y1 N5 C27 N6 5.47(18) . . . . ? C28 N5 C27 Y1 175.77(19) . . . . ? N3 Y1 C27 N6 84.05(12) . . . . ? N1 Y1 C27 N6 -95.59(12) . . . . ? O1 Y1 C27 N6 172.87(11) . . . . ? O2 Y1 C27 N6 -4.57(13) . . . . ? N5 Y1 C27 N6 -174.33(19) . . . . ? N3 Y1 C27 N5 -101.62(12) . . . . ? N1 Y1 C27 N5 78.74(12) . . . . ? O1 Y1 C27 N5 -12.81(13) . . . . ? N6 Y1 C27 N5 174.33(19) . . . . ? O2 Y1 C27 N5 169.76(11) . . . . ? C27 N5 C28 C33 -78.8(2) . . . . ? Y1 N5 C28 C33 93.3(3) . . . . ? C27 N5 C28 C29 105.1(2) . . . . ? Y1 N5 C28 C29 -82.7(3) . . . . ? C33 C28 C29 C30 0.8(3) . . . . ? N5 C28 C29 C30 176.81(17) . . . . ? C33 C28 C29 C34 178.98(18) . . . . ? N5 C28 C29 C34 -5.0(3) . . . . ? C28 C29 C30 C31 0.0(3) . . . . ? C34 C29 C30 C31 -178.3(2) . . . . ? C29 C30 C31 C32 -0.8(4) . . . . ? C30 C31 C32 C33 1.0(4) . . . . ? C31 C32 C33 C28 -0.2(3) . . . . ? C31 C32 C33 C37 -175.8(2) . . . . ? C29 C28 C33 C32 -0.6(3) . . . . ? N5 C28 C33 C32 -176.57(18) . . . . ? C29 C28 C33 C37 174.69(18) . . . . ? N5 C28 C33 C37 -1.2(3) . . . . ? C30 C29 C34 C36 86.7(3) . . . . ? C28 C29 C34 C36 -91.5(2) . . . . ? C30 C29 C34 C35 -37.1(3) . . . . ? C28 C29 C34 C35 144.7(2) . . . . ? C32 C33 C37 C39 -46.7(3) . . . . ? C28 C33 C37 C39 137.9(2) . . . . ? C32 C33 C37 C38 76.4(2) . . . . ? C28 C33 C37 C38 -98.9(2) . . . . ? C27 N6 C40 C45 73.5(2) . . . . ? Y1 N6 C40 C45 -87.3(3) . . . . ? C27 N6 C40 C41 -111.1(2) . . . . ? Y1 N6 C40 C41 88.1(3) . . . . ? C45 C40 C41 C42 -1.7(3) . . . . ? N6 C40 C41 C42 -177.01(17) . . . . ? C45 C40 C41 C46 -179.53(17) . . . . ? N6 C40 C41 C46 5.1(3) . . . . ? C40 C41 C42 C43 0.0(3) . . . . ? C46 C41 C42 C43 177.85(19) . . . . ? C41 C42 C43 C44 1.1(3) . . . . ? C42 C43 C44 C45 -0.6(3) . . . . ? C43 C44 C45 C40 -1.0(3) . . . . ? C43 C44 C45 C49 177.5(2) . . . . ? C41 C40 C45 C44 2.1(3) . . . . ? N6 C40 C45 C44 177.42(18) . . . . ? C41 C40 C45 C49 -176.35(19) . . . . ? N6 C40 C45 C49 -1.1(3) . . . . ? C42 C41 C46 C48 -95.7(2) . . . . ? C40 C41 C46 C48 82.1(2) . . . . ? C42 C41 C46 C47 28.6(3) . . . . ? C40 C41 C46 C47 -153.6(2) . . . . ? C44 C45 C49 C51 68.5(3) . . . . ? C40 C45 C49 C51 -113.0(2) . . . . ? C44 C45 C49 C50 -57.0(3) . . . . ? C40 C45 C49 C50 121.4(2) . . . . ? C55 O1 C52 C53 -14.2(2) . . . . ? Y1 O1 C52 C53 167.28(15) . . . . ? O1 C52 C53 C54 34.0(3) . . . . ? C52 C53 C54 C55 -40.7(3) . . . . ? C52 O1 C55 C54 -11.2(3) . . . . ? Y1 O1 C55 C54 167.15(14) . . . . ? C53 C54 C55 O1 32.4(3) . . . . ? C59 O2 C56 C57 11.5(3) . . . . ? Y1 O2 C56 C57 -172.10(15) . . . . ? O2 C56 C57 C58 -31.0(3) . . . . ? C56 C57 C58 C59 38.7(3) . . . . ? C56 O2 C59 C58 12.8(3) . . . . ? Y1 O2 C59 C58 -163.97(15) . . . . ? C57 C58 C59 O2 -31.8(3) . . . . ? C66 C61 C62 C63 -0.6(4) . . . . ? C60 C61 C62 C63 178.7(3) . . . . ? C61 C62 C63 C64 0.4(5) . . . . ? C62 C63 C64 C65 0.3(4) . . . . ? C63 C64 C65 C66 -0.7(4) . . . . ? C62 C61 C66 C65 0.2(4) . . . . ? C60 C61 C66 C65 -179.1(3) . . . . ? C64 C65 C66 C61 0.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.94 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.693 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.058