# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email jhcheng@riken.jp _publ_contact_author_name 'Jianhua Cheng' loop_ _publ_author_name 'Jianhua Cheng.' 'Haiyu Wang.' 'Masayoshi Nishiura' 'Zhaomin Hou.' data_1-Y _database_code_depnum_ccdc_archive 'CCDC 859483' #TrackingRef '- Ln2H4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((Ph-NCN)YH2)2(THF)3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H106 N4 O3 Y2' _chemical_formula_weight 1277.45 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5958(16) _cell_length_b 15.800(2) _cell_length_c 20.902(3) _cell_angle_alpha 76.137(2) _cell_angle_beta 76.659(2) _cell_angle_gamma 83.229(2) _cell_volume 3921.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.082 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 1.515 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5825 _exptl_absorpt_correction_T_max 0.6429 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 21111 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0773 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13507 _reflns_number_gt 8719 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0896P)^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 13507 _refine_ls_number_parameters 735 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1518 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.971 _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 C4 C 0.7646(4) 0.3981(3) 0.2583(3) 0.0501(12) Uani 1 1 d . . . H4A H 0.7421 0.3604 0.3036 0.060 Uiso 1 1 calc R A 1 H4B H 0.7891 0.3611 0.2248 0.060 Uiso 1 1 calc R A 1 C5 C 0.6589(6) 0.4418(5) 0.2895(8) 0.064(3) Uani 0.78(2) 1 d P B 2 H5A H 0.5962 0.4275 0.2738 0.077 Uiso 0.78(2) 1 calc PR B 2 H5B H 0.6448 0.4249 0.3394 0.077 Uiso 0.78(2) 1 calc PR B 2 C5' C 0.674(2) 0.4632(19) 0.240(2) 0.059(10) Uani 0.22(2) 1 d P B 1 H5'1 H 0.6817 0.4796 0.1908 0.071 Uiso 0.22(2) 1 calc PR B 1 H5'2 H 0.6026 0.4379 0.2606 0.071 Uiso 0.22(2) 1 calc PR B 1 C6 C 0.6804(5) 0.5357(4) 0.2646(4) 0.091(2) Uani 1 1 d . . . H6A H 0.6356 0.5305 0.3108 0.110 Uiso 1 1 calc R B 1 H6B H 0.6544 0.5893 0.2352 0.110 Uiso 1 1 calc R B 1 C7 C 0.7971(4) 0.5383(3) 0.2645(3) 0.0661(16) Uani 1 1 d . B . H7A H 0.8309 0.5846 0.2268 0.079 Uiso 1 1 calc R . . H7B H 0.8056 0.5503 0.3074 0.079 Uiso 1 1 calc R . . C8 C 1.1993(16) 0.5502(12) 0.0119(8) 0.070(3) Uani 0.50(3) 1 d P C 2 H8A H 1.1383 0.5117 0.0330 0.084 Uiso 0.50(3) 1 calc PR C 2 H8B H 1.2697 0.5153 0.0134 0.084 Uiso 0.50(3) 1 calc PR C 2 C9 C 1.192(3) 0.5981(11) -0.0617(10) 0.070(3) Uani 0.50(3) 1 d P C 2 H9A H 1.2289 0.5618 -0.0942 0.084 Uiso 0.50(3) 1 calc PR C 2 H9B H 1.1154 0.6126 -0.0661 0.084 Uiso 0.50(3) 1 calc PR C 2 C10 C 1.246(2) 0.6724(10) -0.0720(6) 0.070(3) Uani 0.50(3) 1 d P C 2 H10A H 1.2149 0.7205 -0.1038 0.084 Uiso 0.50(3) 1 calc PR C 2 H10B H 1.3246 0.6619 -0.0918 0.084 Uiso 0.50(3) 1 calc PR C 2 C11 C 1.2335(16) 0.6977(12) -0.0041(8) 0.070(3) Uani 0.50(3) 1 d P C 2 H11A H 1.3048 0.7099 0.0029 0.084 Uiso 0.50(3) 1 calc PR C 2 H11B H 1.1819 0.7496 -0.0009 0.084 Uiso 0.50(3) 1 calc PR C 2 C8' C 1.1539(17) 0.5553(12) 0.0121(8) 0.072(3) Uani 0.50(3) 1 d P C 1 H8'1 H 1.1867 0.4963 0.0286 0.087 Uiso 0.50(3) 1 calc PR C 1 H8'2 H 1.0734 0.5535 0.0249 0.087 Uiso 0.50(3) 1 calc PR C 1 C9' C 1.187(3) 0.5802(10) -0.0587(11) 0.072(3) Uani 0.50(3) 1 d P C 1 H9C H 1.1363 0.5621 -0.0817 0.087 Uiso 0.50(3) 1 calc PR C 1 H9D H 1.2621 0.5555 -0.0746 0.087 Uiso 0.50(3) 1 calc PR C 1 C10' C 1.183(2) 0.6853(9) -0.0702(7) 0.072(3) Uani 0.50(3) 1 d P C 1 H10C H 1.2460 0.7085 -0.1060 0.087 Uiso 0.50(3) 1 calc PR C 1 H10D H 1.1149 0.7118 -0.0842 0.087 Uiso 0.50(3) 1 calc PR C 1 C11' C 1.1886(17) 0.7058(11) -0.0100(8) 0.072(3) Uani 0.50(3) 1 d P C 1 H11C H 1.1241 0.7445 0.0041 0.087 Uiso 0.50(3) 1 calc PR C 1 H11D H 1.2552 0.7370 -0.0162 0.087 Uiso 0.50(3) 1 calc PR C 1 C12 C 1.4307(17) 0.6398(16) 0.1242(14) 0.084(4) Uani 0.52(4) 1 d P C 2 H12A H 1.4625 0.6609 0.1562 0.101 Uiso 0.52(4) 1 calc PR C 2 H12B H 1.4058 0.6897 0.0911 0.101 Uiso 0.52(4) 1 calc PR C 2 C13 C 1.5145(15) 0.5649(14) 0.0877(17) 0.084(4) Uani 0.52(4) 1 d P C 2 H13A H 1.5028 0.5700 0.0416 0.101 Uiso 0.52(4) 1 calc PR C 2 H13B H 1.5916 0.5758 0.0841 0.101 Uiso 0.52(4) 1 calc PR C 2 C12' C 1.4318(18) 0.6267(18) 0.0996(15) 0.084(4) Uani 0.48(4) 1 d P C 1 H12C H 1.4039 0.6366 0.0576 0.101 Uiso 0.48(4) 1 calc PR C 1 H12D H 1.4380 0.6848 0.1079 0.101 Uiso 0.48(4) 1 calc PR C 1 C13' C 1.5292(16) 0.5884(14) 0.0892(18) 0.084(4) Uani 0.48(4) 1 d P C 1 H13C H 1.5782 0.6077 0.1129 0.101 Uiso 0.48(4) 1 calc PR C 1 H13D H 1.5630 0.5965 0.0406 0.101 Uiso 0.48(4) 1 calc PR C 1 C14 C 1.4946(5) 0.4862(4) 0.1236(3) 0.0830(19) Uani 1 1 d . . . H14A H 1.4733 0.4597 0.0904 0.100 Uiso 1 1 calc R C 1 H14B H 1.5560 0.4497 0.1406 0.100 Uiso 1 1 calc R C 1 C15 C 1.4010(4) 0.4944(3) 0.1795(3) 0.0661(16) Uani 1 1 d . C . H15A H 1.3509 0.4474 0.1876 0.079 Uiso 1 1 calc R . . H15B H 1.4262 0.4916 0.2215 0.079 Uiso 1 1 calc R . . C20 C 1.0949(3) 0.2644(2) 0.32129(19) 0.0320(9) Uani 1 1 d . B . C21 C 1.1201(3) 0.1771(3) 0.3635(2) 0.0390(10) Uani 1 1 d . . . C22 C 1.1808(4) 0.1133(3) 0.3334(3) 0.0541(13) Uani 1 1 d . . . H22 H 1.2079 0.1257 0.2861 0.065 Uiso 1 1 calc R . . C23 C 1.2030(4) 0.0297(3) 0.3724(4) 0.081(2) Uani 1 1 d . . . H23 H 1.2421 -0.0151 0.3515 0.098 Uiso 1 1 calc R . . C24 C 1.1671(5) 0.0143(4) 0.4413(4) 0.085(2) Uani 1 1 d . . . H24 H 1.1844 -0.0411 0.4681 0.102 Uiso 1 1 calc R . . C25 C 1.1074(5) 0.0768(4) 0.4717(3) 0.0757(18) Uani 1 1 d . . . H25 H 1.0829 0.0646 0.5193 0.091 Uiso 1 1 calc R . . C26 C 1.0820(4) 0.1589(3) 0.4331(3) 0.0553(13) Uani 1 1 d . . . H26 H 1.0389 0.2021 0.4543 0.066 Uiso 1 1 calc R . . C27 C 1.2838(3) 0.2818(2) 0.2619(2) 0.0341(10) Uani 1 1 d . . . C28 C 1.3409(4) 0.2915(3) 0.3100(2) 0.0418(11) Uani 1 1 d . . . C29 C 1.2832(4) 0.3209(3) 0.3746(2) 0.0507(12) Uani 1 1 d . . . H29 H 1.2028 0.3178 0.3794 0.061 Uiso 1 1 calc R . . C30 C 1.3159(5) 0.2607(4) 0.4373(3) 0.0703(16) Uani 1 1 d . . . H30A H 1.3011 0.2005 0.4394 0.105 Uiso 1 1 calc R . . H30B H 1.2735 0.2793 0.4777 0.105 Uiso 1 1 calc R . . H30C H 1.3940 0.2639 0.4347 0.105 Uiso 1 1 calc R . . C31 C 1.3040(5) 0.4168(3) 0.3687(3) 0.0670(15) Uani 1 1 d . . . H31A H 1.2654 0.4353 0.4100 0.100 Uiso 1 1 calc R . . H31B H 1.2774 0.4537 0.3300 0.100 Uiso 1 1 calc R . . H31C H 1.3827 0.4224 0.3624 0.100 Uiso 1 1 calc R . . C32 C 1.4547(4) 0.2769(3) 0.2965(3) 0.0533(13) Uani 1 1 d . . . H32 H 1.4937 0.2832 0.3288 0.064 Uiso 1 1 calc R . . C33 C 1.5117(4) 0.2537(3) 0.2385(3) 0.0550(13) Uani 1 1 d . . . H33 H 1.5892 0.2452 0.2300 0.066 Uiso 1 1 calc R . . C34 C 1.4543(4) 0.2429(3) 0.1928(2) 0.0479(12) Uani 1 1 d . . . H34 H 1.4933 0.2256 0.1528 0.057 Uiso 1 1 calc R . . C35 C 1.3422(3) 0.2564(2) 0.2030(2) 0.0367(10) Uani 1 1 d . . . C36 C 1.2847(4) 0.2416(3) 0.1505(2) 0.0423(11) Uani 1 1 d . . . H36 H 1.2040 0.2489 0.1680 0.051 Uiso 1 1 calc R . . C37 C 1.3107(4) 0.1510(3) 0.1373(3) 0.0543(13) Uani 1 1 d . . . H37A H 1.2904 0.1078 0.1795 0.081 Uiso 1 1 calc R . . H37B H 1.3892 0.1428 0.1189 0.081 Uiso 1 1 calc R . . H37C H 1.2695 0.1435 0.1048 0.081 Uiso 1 1 calc R . . C38 C 1.3143(5) 0.3098(3) 0.0844(3) 0.0645(14) Uani 1 1 d . . . H38A H 1.2756 0.2999 0.0515 0.097 Uiso 1 1 calc R . . H38B H 1.3934 0.3046 0.0667 0.097 Uiso 1 1 calc R . . H38C H 1.2929 0.3685 0.0929 0.097 Uiso 1 1 calc R . . C39 C 0.9017(3) 0.2758(3) 0.3759(2) 0.0374(10) Uani 1 1 d . . . C40 C 0.8523(4) 0.3258(3) 0.4237(2) 0.0412(10) Uani 1 1 d . . . C41 C 0.9032(4) 0.4070(3) 0.4269(2) 0.0494(12) Uani 1 1 d . . . H41 H 0.9372 0.4361 0.3798 0.059 Uiso 1 1 calc R . . C42 C 0.9925(5) 0.3847(4) 0.4672(3) 0.0749(17) Uani 1 1 d . . . H42A H 1.0240 0.4385 0.4674 0.112 Uiso 1 1 calc R . . H42B H 1.0497 0.3458 0.4468 0.112 Uiso 1 1 calc R . . H42C H 0.9614 0.3555 0.5137 0.112 Uiso 1 1 calc R . . C43 C 0.8187(5) 0.4733(3) 0.4566(3) 0.0711(16) Uani 1 1 d . . . H43A H 0.7617 0.4897 0.4301 0.107 Uiso 1 1 calc R . . H43B H 0.8550 0.5255 0.4554 0.107 Uiso 1 1 calc R . . H43C H 0.7856 0.4471 0.5034 0.107 Uiso 1 1 calc R . . C44 C 0.7559(4) 0.2982(3) 0.4687(2) 0.0560(13) Uani 1 1 d . . . H44 H 0.7229 0.3304 0.5021 0.067 Uiso 1 1 calc R . . C45 C 0.7078(4) 0.2263(3) 0.4662(3) 0.0574(13) Uani 1 1 d . . . H45 H 0.6427 0.2084 0.4977 0.069 Uiso 1 1 calc R . . C46 C 0.7543(4) 0.1808(3) 0.4180(2) 0.0504(12) Uani 1 1 d . . . H46 H 0.7197 0.1316 0.4159 0.060 Uiso 1 1 calc R . . C47 C 0.8507(3) 0.2039(3) 0.3717(2) 0.0390(10) Uani 1 1 d . . . C48 C 0.8933(4) 0.1505(3) 0.3184(2) 0.0428(11) Uani 1 1 d . . . H48 H 0.9638 0.1738 0.2904 0.051 Uiso 1 1 calc R . . C49 C 0.9157(4) 0.0548(3) 0.3505(3) 0.0542(13) Uani 1 1 d . . . H49A H 0.9456 0.0223 0.3151 0.081 Uiso 1 1 calc R . . H49B H 0.8474 0.0305 0.3778 0.081 Uiso 1 1 calc R . . H49C H 0.9686 0.0500 0.3792 0.081 Uiso 1 1 calc R . . C50 C 0.8144(5) 0.1575(3) 0.2720(3) 0.0629(14) Uani 1 1 d . . . H50A H 0.8457 0.1238 0.2376 0.094 Uiso 1 1 calc R . . H50B H 0.8017 0.2190 0.2502 0.094 Uiso 1 1 calc R . . H50C H 0.7449 0.1344 0.2984 0.094 Uiso 1 1 calc R . . C51 C 1.0969(4) 0.7896(3) 0.1565(2) 0.0376(10) Uani 1 1 d . . . C52 C 1.0618(4) 0.8855(3) 0.1507(2) 0.0429(11) Uani 1 1 d . . . C53 C 0.9990(4) 0.9254(3) 0.1039(3) 0.0579(14) Uani 1 1 d . . . H53 H 0.9776 0.8920 0.0773 0.069 Uiso 1 1 calc R . . C54 C 0.9674(5) 1.0129(3) 0.0956(4) 0.0804(19) Uani 1 1 d . . . H54 H 0.9241 1.0391 0.0635 0.097 Uiso 1 1 calc R . . C55 C 0.9966(5) 1.0620(3) 0.1321(4) 0.0758(18) Uani 1 1 d . . . H55 H 0.9750 1.1227 0.1250 0.091 Uiso 1 1 calc R . . C56 C 1.0576(5) 1.0252(3) 0.1796(3) 0.0675(16) Uani 1 1 d . . . H56 H 1.0773 1.0598 0.2059 0.081 Uiso 1 1 calc R . . C57 C 1.0906(4) 0.9360(3) 0.1889(2) 0.0490(12) Uani 1 1 d . . . H57 H 1.1330 0.9101 0.2216 0.059 Uiso 1 1 calc R . . C58 C 0.9121(4) 0.7475(3) 0.1759(3) 0.0548(14) Uani 1 1 d . . . C59 C 0.8581(10) 0.7375(9) 0.1186(6) 0.0630(15) Uani 0.496(10) 1 d PD D 2 C60 C 0.9178(9) 0.7076(7) 0.0563(6) 0.0630(15) Uani 0.496(10) 1 d PD D 2 H60 H 0.9953 0.6867 0.0583 0.076 Uiso 0.496(10) 1 calc PR D 2 C61 C 0.8427(9) 0.6293(7) 0.0679(7) 0.0630(15) Uani 0.496(10) 1 d PD D 2 H61A H 0.8621 0.6024 0.0287 0.095 Uiso 0.496(10) 1 calc PR D 2 H61B H 0.7658 0.6515 0.0738 0.095 Uiso 0.496(10) 1 calc PR D 2 H61C H 0.8535 0.5857 0.1083 0.095 Uiso 0.496(10) 1 calc PR D 2 C62 C 0.9094(10) 0.7749(7) -0.0088(6) 0.0630(15) Uani 0.496(10) 1 d PD D 2 H62A H 0.9268 0.8321 -0.0049 0.095 Uiso 0.496(10) 1 calc PR D 2 H62B H 0.8350 0.7787 -0.0164 0.095 Uiso 0.496(10) 1 calc PR D 2 H62C H 0.9613 0.7570 -0.0467 0.095 Uiso 0.496(10) 1 calc PR D 2 C63 C 0.7426(9) 0.7472(7) 0.1295(7) 0.0630(15) Uani 0.496(10) 1 d PD D 2 H63 H 0.7049 0.7378 0.0976 0.076 Uiso 0.496(10) 1 calc PR D 2 C64 C 0.6874(9) 0.7708(7) 0.1878(8) 0.0630(15) Uani 0.496(10) 1 d PD D 2 H64 H 0.6100 0.7784 0.1951 0.076 Uiso 0.496(10) 1 calc PR D 2 C65 C 0.7372(9) 0.7845(7) 0.2379(7) 0.0630(15) Uani 0.496(10) 1 d PD D 2 H65 H 0.6951 0.8024 0.2769 0.076 Uiso 0.496(10) 1 calc PR D 2 C66 C 0.8514(9) 0.7708(8) 0.2279(7) 0.0630(15) Uani 0.496(10) 1 d PD D 2 C67 C 0.9035(10) 0.7758(6) 0.2845(6) 0.0630(15) Uani 0.496(10) 1 d PD D 2 H67 H 0.9823 0.7860 0.2646 0.076 Uiso 0.496(10) 1 calc PR D 2 C68 C 0.8997(10) 0.6917(7) 0.3379(6) 0.0630(15) Uani 0.496(10) 1 d PD D 2 H68A H 0.9201 0.6419 0.3161 0.095 Uiso 0.496(10) 1 calc PR D 2 H68B H 0.8255 0.6864 0.3655 0.095 Uiso 0.496(10) 1 calc PR D 2 H68C H 0.9510 0.6924 0.3665 0.095 Uiso 0.496(10) 1 calc PR D 2 C69 C 0.8540(10) 0.8528(6) 0.3169(6) 0.0630(15) Uani 0.496(10) 1 d PD D 2 H69A H 0.8539 0.9065 0.2818 0.095 Uiso 0.496(10) 1 calc PR D 2 H69B H 0.8978 0.8593 0.3484 0.095 Uiso 0.496(10) 1 calc PR D 2 H69C H 0.7789 0.8418 0.3413 0.095 Uiso 0.496(10) 1 calc PR D 2 C59' C 0.8432(10) 0.7382(9) 0.1394(6) 0.0633(15) Uani 0.504(10) 1 d PD D 1 C60' C 0.8810(10) 0.7201(6) 0.0733(6) 0.0633(15) Uani 0.504(10) 1 d PD D 1 H60' H 0.9612 0.7266 0.0658 0.076 Uiso 0.504(10) 1 calc PR D 1 C61' C 0.8815(10) 0.6270(7) 0.0519(7) 0.0633(15) Uani 0.504(10) 1 d PD D 1 H61D H 0.9265 0.6298 0.0065 0.095 Uiso 0.504(10) 1 calc PR D 1 H61E H 0.8066 0.6155 0.0524 0.095 Uiso 0.504(10) 1 calc PR D 1 H61F H 0.9118 0.5800 0.0840 0.095 Uiso 0.504(10) 1 calc PR D 1 C62' C 0.8496(10) 0.7938(6) 0.0156(6) 0.0633(15) Uani 0.504(10) 1 d PD D 1 H62D H 0.8883 0.7817 -0.0279 0.095 Uiso 0.504(10) 1 calc PR D 1 H62E H 0.8703 0.8498 0.0198 0.095 Uiso 0.504(10) 1 calc PR D 1 H62F H 0.7706 0.7965 0.0186 0.095 Uiso 0.504(10) 1 calc PR D 1 C63' C 0.7287(10) 0.7529(8) 0.1628(7) 0.0633(15) Uani 0.504(10) 1 d PD D 1 H63' H 0.6790 0.7505 0.1354 0.076 Uiso 0.504(10) 1 calc PR D 1 C64' C 0.6920(9) 0.7703(7) 0.2243(7) 0.0633(15) Uani 0.504(10) 1 d PD D 1 H64' H 0.6156 0.7829 0.2379 0.076 Uiso 0.504(10) 1 calc PR D 1 C65' C 0.7580(9) 0.7715(7) 0.2705(7) 0.0633(15) Uani 0.504(10) 1 d PD D 1 H65' H 0.7263 0.7787 0.3149 0.076 Uiso 0.504(10) 1 calc PR D 1 C66' C 0.8706(9) 0.7618(8) 0.2486(6) 0.0633(15) Uani 0.504(10) 1 d PD D 1 C67' C 0.9424(10) 0.7580(7) 0.2980(6) 0.0633(15) Uani 0.504(10) 1 d PD D 1 H67' H 1.0182 0.7689 0.2713 0.076 Uiso 0.504(10) 1 calc PR D 1 C68' C 0.9471(10) 0.6684(7) 0.3444(6) 0.0633(15) Uani 0.504(10) 1 d PD D 1 H68D H 0.9816 0.6253 0.3179 0.095 Uiso 0.504(10) 1 calc PR D 1 H68E H 0.8728 0.6527 0.3675 0.095 Uiso 0.504(10) 1 calc PR D 1 H68F H 0.9900 0.6694 0.3778 0.095 Uiso 0.504(10) 1 calc PR D 1 C69' C 0.9071(10) 0.8294(7) 0.3385(6) 0.0633(15) Uani 0.504(10) 1 d PD D 1 H69D H 0.9094 0.8868 0.3075 0.095 Uiso 0.504(10) 1 calc PR D 1 H69E H 0.9568 0.8258 0.3689 0.095 Uiso 0.504(10) 1 calc PR D 1 H69F H 0.8324 0.8211 0.3648 0.095 Uiso 0.504(10) 1 calc PR D 1 C70 C 1.2810(4) 0.8101(3) 0.1618(3) 0.0601(15) Uani 1 1 d . . . C71 C 1.3371(13) 0.8710(10) 0.1133(7) 0.0554(17) Uani 0.434(11) 1 d PD E 2 C72 C 1.3170(10) 0.8878(8) 0.0439(7) 0.0554(17) Uani 0.434(11) 1 d PD E 2 H72 H 1.2571 0.8518 0.0435 0.067 Uiso 0.434(11) 1 calc PR E 2 C73 C 1.2859(11) 0.9839(8) 0.0183(9) 0.0554(17) Uani 0.434(11) 1 d PD E 2 H73A H 1.2772 0.9936 -0.0283 0.083 Uiso 0.434(11) 1 calc PR E 2 H73B H 1.3436 1.0193 0.0202 0.083 Uiso 0.434(11) 1 calc PR E 2 H73C H 1.2170 1.0008 0.0466 0.083 Uiso 0.434(11) 1 calc PR E 2 C74 C 1.4257(10) 0.8608(7) -0.0039(7) 0.0554(17) Uani 0.434(11) 1 d PD E 2 H74A H 1.4457 0.7986 0.0116 0.083 Uiso 0.434(11) 1 calc PR E 2 H74B H 1.4846 0.8955 -0.0029 0.083 Uiso 0.434(11) 1 calc PR E 2 H74C H 1.4142 0.8715 -0.0500 0.083 Uiso 0.434(11) 1 calc PR E 2 C75 C 1.4097(11) 0.9235(8) 0.1290(7) 0.0554(17) Uani 0.434(11) 1 d PD E 2 H75 H 1.4451 0.9685 0.0947 0.067 Uiso 0.434(11) 1 calc PR E 2 C76 C 1.4286(10) 0.9090(7) 0.1940(7) 0.0554(17) Uani 0.434(11) 1 d PD E 2 H76 H 1.4811 0.9408 0.2028 0.067 Uiso 0.434(11) 1 calc PR E 2 C77 C 1.3728(10) 0.8503(7) 0.2440(7) 0.0554(17) Uani 0.434(11) 1 d PD E 2 H77 H 1.3838 0.8407 0.2888 0.067 Uiso 0.434(11) 1 calc PR E 2 C78 C 1.2983(10) 0.8040(7) 0.2285(6) 0.0554(17) Uani 0.434(11) 1 d PD E 2 C79 C 1.2779(10) 0.7181(7) 0.2811(6) 0.0554(17) Uani 0.434(11) 1 d PD E 2 H79 H 1.2161 0.6890 0.2745 0.067 Uiso 0.434(11) 1 calc PR E 2 C80 C 1.3734(11) 0.6522(6) 0.2934(7) 0.0554(17) Uani 0.434(11) 1 d PD E 2 H80A H 1.3937 0.6202 0.2571 0.083 Uiso 0.434(11) 1 calc PR E 2 H80B H 1.3521 0.6111 0.3367 0.083 Uiso 0.434(11) 1 calc PR E 2 H80C H 1.4360 0.6830 0.2944 0.083 Uiso 0.434(11) 1 calc PR E 2 C81 C 1.2400(11) 0.7649(7) 0.3405(6) 0.0554(17) Uani 0.434(11) 1 d PD E 2 H81A H 1.2059 0.7235 0.3808 0.083 Uiso 0.434(11) 1 calc PR E 2 H81B H 1.1869 0.8136 0.3289 0.083 Uiso 0.434(11) 1 calc PR E 2 H81C H 1.3033 0.7874 0.3493 0.083 Uiso 0.434(11) 1 calc PR E 2 C71' C 1.3299(12) 0.8705(9) 0.0971(6) 0.0787(16) Uani 0.566(11) 1 d PD E 1 C72' C 1.2906(10) 0.8948(7) 0.0313(6) 0.0787(16) Uani 0.566(11) 1 d PD E 1 H72' H 1.2246 0.8617 0.0375 0.094 Uiso 0.566(11) 1 calc PR E 1 C73' C 1.2578(10) 0.9907(7) 0.0107(8) 0.0787(16) Uani 0.566(11) 1 d PD E 1 H73D H 1.2331 1.0021 -0.0319 0.118 Uiso 0.566(11) 1 calc PR E 1 H73E H 1.3208 1.0249 0.0049 0.118 Uiso 0.566(11) 1 calc PR E 1 H73F H 1.1984 1.0076 0.0458 0.118 Uiso 0.566(11) 1 calc PR E 1 C74' C 1.3790(10) 0.8674(6) -0.0275(6) 0.0787(16) Uani 0.566(11) 1 d PD E 1 H74D H 1.4000 0.8049 -0.0149 0.118 Uiso 0.566(11) 1 calc PR E 1 H74E H 1.4434 0.9010 -0.0361 0.118 Uiso 0.566(11) 1 calc PR E 1 H74F H 1.3490 0.8793 -0.0682 0.118 Uiso 0.566(11) 1 calc PR E 1 C75' C 1.4190(9) 0.9133(7) 0.1025(7) 0.0787(16) Uani 0.566(11) 1 d PD E 1 H75' H 1.4558 0.9526 0.0640 0.094 Uiso 0.566(11) 1 calc PR E 1 C76' C 1.4535(9) 0.8996(7) 0.1618(7) 0.0787(16) Uani 0.566(11) 1 d PD E 1 H76' H 1.5099 0.9328 0.1644 0.094 Uiso 0.566(11) 1 calc PR E 1 C77' C 1.4091(9) 0.8396(6) 0.2172(7) 0.0787(16) Uani 0.566(11) 1 d PD E 1 H77' H 1.4383 0.8311 0.2565 0.094 Uiso 0.566(11) 1 calc PR E 1 C78' C 1.3227(9) 0.7896(7) 0.2197(6) 0.0787(16) Uani 0.566(11) 1 d PD E 1 C79' C 1.2409(9) 0.7434(7) 0.2914(6) 0.0787(16) Uani 0.566(11) 1 d PD E 1 H79' H 1.1813 0.7218 0.2764 0.094 Uiso 0.566(11) 1 calc PR E 1 C80' C 1.3076(11) 0.6588(6) 0.3185(6) 0.0787(16) Uani 0.566(11) 1 d PD E 1 H80D H 1.3370 0.6278 0.2821 0.118 Uiso 0.566(11) 1 calc PR E 1 H80E H 1.2599 0.6211 0.3554 0.118 Uiso 0.566(11) 1 calc PR E 1 H80F H 1.3680 0.6739 0.3350 0.118 Uiso 0.566(11) 1 calc PR E 1 C81' C 1.1822(10) 0.7842(7) 0.3479(6) 0.0787(16) Uani 0.566(11) 1 d PD E 1 H81D H 1.1459 0.7394 0.3850 0.118 Uiso 0.566(11) 1 calc PR E 1 H81E H 1.1273 0.8289 0.3323 0.118 Uiso 0.566(11) 1 calc PR E 1 H81F H 1.2345 0.8113 0.3637 0.118 Uiso 0.566(11) 1 calc PR E 1 N3 N 1.1696(3) 0.3047(2) 0.26956(16) 0.0325(8) Uani 1 1 d . B . N4 N 0.9971(3) 0.3084(2) 0.32880(16) 0.0338(8) Uani 1 1 d . B . N1 N 1.0270(3) 0.7312(2) 0.15854(18) 0.0394(9) Uani 1 1 d . B . N2 N 1.1991(3) 0.7577(2) 0.1559(2) 0.0454(9) Uani 1 1 d . B . O3 O 0.8482(2) 0.45348(17) 0.25669(16) 0.0461(8) Uani 1 1 d . B . O2 O 1.1910(3) 0.6216(2) 0.04381(16) 0.0691(11) Uani 1 1 d . . . O1 O 1.3475(3) 0.5794(2) 0.1572(2) 0.0692(11) Uani 1 1 d . . . Y2 Y 1.04151(3) 0.41522(2) 0.22496(2) 0.03295(13) Uani 1 1 d . . . Y1 Y 1.15480(3) 0.60802(2) 0.16075(2) 0.03708(14) Uani 1 1 d . B . H4 H 1.001(3) 0.340(2) 0.1471(18) 0.035 Uiso 1 1 d . . . H1 H 1.017(3) 0.549(3) 0.165(2) 0.046(11) Uiso 1 1 d . . . H3 H 1.105(4) 0.531(3) 0.252(2) 0.063(14) Uiso 1 1 d . . . H2 H 1.185(3) 0.472(3) 0.159(2) 0.049(12) 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 C4 0.043(3) 0.043(3) 0.065(3) -0.013(2) -0.006(2) -0.015(2) C5 0.039(4) 0.060(5) 0.091(9) -0.011(5) -0.011(4) -0.012(3) C5' 0.056(17) 0.074(19) 0.05(2) 0.005(15) -0.023(15) -0.036(14) C6 0.051(4) 0.061(4) 0.149(7) -0.014(4) -0.008(4) 0.004(3) C7 0.043(3) 0.040(3) 0.109(5) -0.023(3) 0.000(3) 0.002(2) C8 0.098(7) 0.050(4) 0.055(4) -0.005(3) -0.010(4) -0.008(5) C9 0.098(7) 0.050(4) 0.055(4) -0.005(3) -0.010(4) -0.008(5) C10 0.098(7) 0.050(4) 0.055(4) -0.005(3) -0.010(4) -0.008(5) C11 0.098(7) 0.050(4) 0.055(4) -0.005(3) -0.010(4) -0.008(5) C8' 0.103(7) 0.048(4) 0.054(4) 0.005(3) -0.009(4) -0.006(5) C9' 0.103(7) 0.048(4) 0.054(4) 0.005(3) -0.009(4) -0.006(5) C10' 0.103(7) 0.048(4) 0.054(4) 0.005(3) -0.009(4) -0.006(5) C11' 0.103(7) 0.048(4) 0.054(4) 0.005(3) -0.009(4) -0.006(5) C12 0.065(4) 0.040(6) 0.115(6) 0.010(8) 0.025(5) -0.017(3) C13 0.065(4) 0.040(6) 0.115(6) 0.010(8) 0.025(5) -0.017(3) C12' 0.065(4) 0.040(6) 0.115(6) 0.010(8) 0.025(5) -0.017(3) C13' 0.065(4) 0.040(6) 0.115(6) 0.010(8) 0.025(5) -0.017(3) C14 0.082(4) 0.058(3) 0.086(4) -0.001(3) 0.012(4) 0.003(3) C15 0.052(3) 0.036(3) 0.092(4) 0.014(3) -0.008(3) -0.004(2) C20 0.041(3) 0.0250(19) 0.029(2) -0.0029(17) -0.0056(19) -0.0083(18) C21 0.039(3) 0.035(2) 0.038(3) 0.005(2) -0.007(2) -0.0086(19) C22 0.044(3) 0.034(2) 0.073(4) 0.005(2) -0.004(3) -0.008(2) C23 0.052(4) 0.036(3) 0.134(6) 0.016(3) -0.008(4) -0.006(2) C24 0.068(4) 0.046(3) 0.114(6) 0.041(4) -0.019(4) -0.014(3) C25 0.071(4) 0.075(4) 0.064(4) 0.039(3) -0.027(3) -0.027(3) C26 0.054(3) 0.049(3) 0.056(3) 0.014(2) -0.018(3) -0.017(2) C27 0.031(2) 0.027(2) 0.041(3) 0.0000(18) -0.004(2) -0.0087(17) C28 0.049(3) 0.030(2) 0.045(3) 0.001(2) -0.009(2) -0.018(2) C29 0.058(3) 0.056(3) 0.042(3) -0.008(2) -0.011(2) -0.022(2) C30 0.097(5) 0.071(4) 0.044(3) -0.003(3) -0.020(3) -0.025(3) C31 0.091(4) 0.056(3) 0.057(3) -0.017(3) -0.008(3) -0.024(3) C32 0.048(3) 0.054(3) 0.059(3) 0.001(3) -0.022(3) -0.016(2) C33 0.035(3) 0.058(3) 0.069(4) -0.004(3) -0.012(3) -0.006(2) C34 0.038(3) 0.050(3) 0.051(3) -0.008(2) -0.003(2) -0.001(2) C35 0.033(3) 0.029(2) 0.042(3) -0.0010(19) -0.004(2) -0.0028(18) C36 0.039(3) 0.046(2) 0.042(3) -0.013(2) -0.004(2) -0.002(2) C37 0.060(3) 0.045(3) 0.054(3) -0.011(2) -0.003(3) -0.008(2) C38 0.082(4) 0.056(3) 0.055(3) -0.007(3) -0.019(3) -0.005(3) C39 0.037(2) 0.037(2) 0.033(2) -0.0015(19) -0.003(2) -0.0046(19) C40 0.044(3) 0.041(2) 0.034(2) -0.007(2) 0.002(2) -0.010(2) C41 0.053(3) 0.055(3) 0.040(3) -0.016(2) 0.003(2) -0.018(2) C42 0.065(4) 0.087(4) 0.088(4) -0.047(4) -0.014(3) -0.012(3) C43 0.074(4) 0.058(3) 0.082(4) -0.033(3) 0.003(3) -0.013(3) C44 0.053(3) 0.057(3) 0.051(3) -0.018(3) 0.010(2) -0.008(3) C45 0.049(3) 0.056(3) 0.056(3) -0.010(3) 0.016(2) -0.017(2) C46 0.047(3) 0.045(3) 0.054(3) -0.005(2) 0.000(2) -0.017(2) C47 0.037(3) 0.035(2) 0.040(3) -0.0011(19) -0.002(2) -0.0099(19) C48 0.048(3) 0.038(2) 0.041(3) -0.005(2) -0.006(2) -0.009(2) C49 0.065(3) 0.033(2) 0.059(3) -0.004(2) -0.003(3) -0.015(2) C50 0.083(4) 0.053(3) 0.058(3) -0.018(3) -0.018(3) -0.006(3) C51 0.042(3) 0.029(2) 0.039(3) -0.0047(19) -0.003(2) -0.0097(19) C52 0.044(3) 0.033(2) 0.048(3) -0.006(2) 0.000(2) -0.016(2) C53 0.063(3) 0.035(2) 0.073(4) -0.003(2) -0.018(3) -0.007(2) C54 0.079(4) 0.036(3) 0.127(6) -0.009(3) -0.037(4) 0.002(3) C55 0.069(4) 0.035(3) 0.113(5) -0.020(3) 0.002(4) 0.000(3) C56 0.076(4) 0.045(3) 0.077(4) -0.029(3) 0.022(3) -0.029(3) C57 0.056(3) 0.037(2) 0.050(3) -0.009(2) 0.006(2) -0.020(2) C58 0.044(3) 0.021(2) 0.092(4) -0.007(2) -0.002(3) -0.009(2) C59 0.054(3) 0.047(2) 0.088(3) -0.0122(19) -0.015(2) -0.0057(18) C60 0.054(3) 0.047(2) 0.088(3) -0.0122(19) -0.015(2) -0.0057(18) C61 0.054(3) 0.047(2) 0.088(3) -0.0122(19) -0.015(2) -0.0057(18) C62 0.054(3) 0.047(2) 0.088(3) -0.0122(19) -0.015(2) -0.0057(18) C63 0.054(3) 0.047(2) 0.088(3) -0.0122(19) -0.015(2) -0.0057(18) C64 0.054(3) 0.047(2) 0.088(3) -0.0122(19) -0.015(2) -0.0057(18) C65 0.054(3) 0.047(2) 0.088(3) -0.0122(19) -0.015(2) -0.0057(18) C66 0.054(3) 0.047(2) 0.088(3) -0.0122(19) -0.015(2) -0.0057(18) C67 0.054(3) 0.047(2) 0.088(3) -0.0122(19) -0.015(2) -0.0057(18) C68 0.054(3) 0.047(2) 0.088(3) -0.0122(19) -0.015(2) -0.0057(18) C69 0.054(3) 0.047(2) 0.088(3) -0.0122(19) -0.015(2) -0.0057(18) C59' 0.056(3) 0.054(2) 0.077(3) -0.0096(19) -0.011(2) -0.0104(18) C60' 0.056(3) 0.054(2) 0.077(3) -0.0096(19) -0.011(2) -0.0104(18) C61' 0.056(3) 0.054(2) 0.077(3) -0.0096(19) -0.011(2) -0.0104(18) C62' 0.056(3) 0.054(2) 0.077(3) -0.0096(19) -0.011(2) -0.0104(18) C63' 0.056(3) 0.054(2) 0.077(3) -0.0096(19) -0.011(2) -0.0104(18) C64' 0.056(3) 0.054(2) 0.077(3) -0.0096(19) -0.011(2) -0.0104(18) C65' 0.056(3) 0.054(2) 0.077(3) -0.0096(19) -0.011(2) -0.0104(18) C66' 0.056(3) 0.054(2) 0.077(3) -0.0096(19) -0.011(2) -0.0104(18) C67' 0.056(3) 0.054(2) 0.077(3) -0.0096(19) -0.011(2) -0.0104(18) C68' 0.056(3) 0.054(2) 0.077(3) -0.0096(19) -0.011(2) -0.0104(18) C69' 0.056(3) 0.054(2) 0.077(3) -0.0096(19) -0.011(2) -0.0104(18) C70 0.051(3) 0.031(2) 0.101(4) -0.003(3) -0.027(3) -0.011(2) C71 0.045(3) 0.038(2) 0.083(3) -0.016(2) -0.009(2) -0.0034(17) C72 0.045(3) 0.038(2) 0.083(3) -0.016(2) -0.009(2) -0.0034(17) C73 0.045(3) 0.038(2) 0.083(3) -0.016(2) -0.009(2) -0.0034(17) C74 0.045(3) 0.038(2) 0.083(3) -0.016(2) -0.009(2) -0.0034(17) C75 0.045(3) 0.038(2) 0.083(3) -0.016(2) -0.009(2) -0.0034(17) C76 0.045(3) 0.038(2) 0.083(3) -0.016(2) -0.009(2) -0.0034(17) C77 0.045(3) 0.038(2) 0.083(3) -0.016(2) -0.009(2) -0.0034(17) C78 0.045(3) 0.038(2) 0.083(3) -0.016(2) -0.009(2) -0.0034(17) C79 0.045(3) 0.038(2) 0.083(3) -0.016(2) -0.009(2) -0.0034(17) C80 0.045(3) 0.038(2) 0.083(3) -0.016(2) -0.009(2) -0.0034(17) C81 0.045(3) 0.038(2) 0.083(3) -0.016(2) -0.009(2) -0.0034(17) C71' 0.062(3) 0.048(2) 0.118(4) -0.003(2) -0.017(2) -0.0072(17) C72' 0.062(3) 0.048(2) 0.118(4) -0.003(2) -0.017(2) -0.0072(17) C73' 0.062(3) 0.048(2) 0.118(4) -0.003(2) -0.017(2) -0.0072(17) C74' 0.062(3) 0.048(2) 0.118(4) -0.003(2) -0.017(2) -0.0072(17) C75' 0.062(3) 0.048(2) 0.118(4) -0.003(2) -0.017(2) -0.0072(17) C76' 0.062(3) 0.048(2) 0.118(4) -0.003(2) -0.017(2) -0.0072(17) C77' 0.062(3) 0.048(2) 0.118(4) -0.003(2) -0.017(2) -0.0072(17) C78' 0.062(3) 0.048(2) 0.118(4) -0.003(2) -0.017(2) -0.0072(17) C79' 0.062(3) 0.048(2) 0.118(4) -0.003(2) -0.017(2) -0.0072(17) C80' 0.062(3) 0.048(2) 0.118(4) -0.003(2) -0.017(2) -0.0072(17) C81' 0.062(3) 0.048(2) 0.118(4) -0.003(2) -0.017(2) -0.0072(17) N3 0.0294(19) 0.0290(16) 0.0348(19) -0.0034(15) 0.0002(15) -0.0065(14) N4 0.032(2) 0.0323(17) 0.0321(19) -0.0025(15) 0.0010(15) -0.0071(15) N1 0.037(2) 0.0289(17) 0.049(2) -0.0046(16) -0.0053(17) -0.0064(16) N2 0.035(2) 0.0318(18) 0.065(3) 0.0004(18) -0.0074(19) -0.0107(16) O3 0.0332(17) 0.0330(15) 0.068(2) -0.0076(15) -0.0047(15) -0.0062(13) O2 0.117(3) 0.0342(17) 0.043(2) -0.0040(15) 0.008(2) -0.0102(18) O1 0.038(2) 0.0383(17) 0.112(3) 0.0100(19) -0.0023(19) -0.0074(15) Y2 0.0334(2) 0.0255(2) 0.0353(2) -0.00054(17) -0.00216(18) -0.00656(16) Y1 0.0350(3) 0.0251(2) 0.0438(3) 0.00026(18) 0.0006(2) -0.00706(17) _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 C4 O3 1.436(5) . ? C4 C5' 1.49(3) . ? C4 C5 1.508(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.485(10) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5' C6 1.38(3) . ? C5' H5'1 0.9900 . ? C5' H5'2 0.9900 . ? C6 C7 1.475(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O3 1.445(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O2 1.424(18) . ? C8 C9 1.56(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.37(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.535(18) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O2 1.436(18) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C8' C9' 1.41(3) . ? C8' O2 1.531(19) . ? C8' H8'1 0.9900 . ? C8' H8'2 0.9900 . ? C9' C10' 1.62(2) . ? C9' H9C 0.9900 . ? C9' H9D 0.9900 . ? C10' C11' 1.387(18) . ? C10' H10C 0.9900 . ? C10' H10D 0.9900 . ? C11' O2 1.525(16) . ? C11' H11C 0.9900 . ? C11' H11D 0.9900 . ? C12 O1 1.44(2) . ? C12 C13 1.69(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.309(18) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C12' C13' 1.30(3) . ? C12' O1 1.52(2) . ? C12' H12C 0.9900 . ? C12' H12D 0.9900 . ? C13' C14 1.67(2) . ? C13' H13C 0.9900 . ? C13' H13D 0.9900 . ? C14 C15 1.474(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O1 1.451(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C20 N4 1.337(5) . ? C20 N3 1.342(5) . ? C20 C21 1.491(5) . ? C20 Y2 2.852(4) . ? C21 C22 1.377(6) . ? C21 C26 1.393(6) . ? C22 C23 1.409(7) . ? C22 H22 0.9500 . ? C23 C24 1.377(9) . ? C23 H23 0.9500 . ? C24 C25 1.360(9) . ? C24 H24 0.9500 . ? C25 C26 1.399(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C35 1.403(6) . ? C27 C28 1.409(6) . ? C27 N3 1.423(5) . ? C28 C32 1.397(6) . ? C28 C29 1.528(6) . ? C29 C30 1.533(7) . ? C29 C31 1.539(6) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.368(7) . ? C32 H32 0.9500 . ? C33 C34 1.376(6) . ? C33 H33 0.9500 . ? C34 C35 1.377(6) . ? C34 H34 0.9500 . ? C35 C36 1.520(6) . ? C36 C37 1.507(6) . ? C36 C38 1.533(6) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C47 1.399(6) . ? C39 C40 1.408(6) . ? C39 N4 1.427(5) . ? C40 C44 1.396(6) . ? C40 C41 1.522(6) . ? C41 C42 1.518(7) . ? C41 C43 1.536(7) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.367(7) . ? C44 H44 0.9500 . ? C45 C46 1.360(7) . ? C45 H45 0.9500 . ? C46 C47 1.393(6) . ? C46 H46 0.9500 . ? C47 C48 1.519(6) . ? C48 C50 1.518(6) . ? C48 C49 1.523(6) . ? C48 H48 1.0000 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 N2 1.324(5) . ? C51 N1 1.335(5) . ? C51 C52 1.511(6) . ? C51 Y1 2.861(4) . ? C52 C57 1.383(6) . ? C52 C53 1.388(6) . ? C53 C54 1.373(7) . ? C53 H53 0.9500 . ? C54 C55 1.341(8) . ? C54 H54 0.9500 . ? C55 C56 1.373(8) . ? C55 H55 0.9500 . ? C56 C57 1.402(7) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 C66 1.281(13) . ? C58 C59' 1.321(13) . ? C58 N1 1.417(6) . ? C58 C66' 1.549(13) . ? C58 C59 1.554(13) . ? C59 C63 1.416(12) . ? C59 C60 1.497(12) . ? C60 C62 1.528(12) . ? C60 C61 1.585(12) . ? C60 H60 1.0000 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.370(14) . ? C63 H63 0.9500 . ? C64 C65 1.406(15) . ? C64 H64 0.9500 . ? C65 C66 1.404(13) . ? C65 H65 0.9500 . ? C66 C67 1.500(13) . ? C67 C68 1.514(12) . ? C67 C69 1.534(12) . ? C67 H67 1.0000 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C59' C63' 1.422(13) . ? C59' C60' 1.441(12) . ? C60' C62' 1.550(12) . ? C60' C61' 1.634(12) . ? C60' H60' 1.0000 . ? C61' H61D 0.9800 . ? C61' H61E 0.9800 . ? C61' H61F 0.9800 . ? C62' H62D 0.9800 . ? C62' H62E 0.9800 . ? C62' H62F 0.9800 . ? C63' C64' 1.345(14) . ? C63' H63' 0.9500 . ? C64' C65' 1.415(15) . ? C64' H64' 0.9500 . ? C65' C66' 1.389(12) . ? C65' H65' 0.9500 . ? C66' C67' 1.509(12) . ? C67' C68' 1.514(12) . ? C67' C69' 1.533(12) . ? C67' H67' 1.0000 . ? C68' H68D 0.9800 . ? C68' H68E 0.9800 . ? C68' H68F 0.9800 . ? C69' H69D 0.9800 . ? C69' H69E 0.9800 . ? C69' H69F 0.9800 . ? C70 C71 1.347(14) . ? C70 C78' 1.381(13) . ? C70 C78 1.439(14) . ? C70 N2 1.441(6) . ? C70 C71' 1.502(13) . ? C71 C75 1.443(13) . ? C71 C72 1.486(13) . ? C72 C73 1.521(12) . ? C72 C74 1.577(12) . ? C72 H72 1.0000 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C76 1.393(14) . ? C75 H75 0.9500 . ? C76 C77 1.341(13) . ? C76 H76 0.9500 . ? C77 C78 1.393(12) . ? C77 H77 0.9500 . ? C78 C79 1.534(13) . ? C79 C80 1.522(13) . ? C79 C81 1.549(13) . ? C79 H79 1.0000 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C71' C75' 1.417(12) . ? C71' C72' 1.516(12) . ? C72' C73' 1.509(11) . ? C72' C74' 1.564(12) . ? C72' H72' 1.0000 . ? C73' H73D 0.9800 . ? C73' H73E 0.9800 . ? C73' H73F 0.9800 . ? C74' H74D 0.9800 . ? C74' H74E 0.9800 . ? C74' H74F 0.9800 . ? C75' C76' 1.367(13) . ? C75' H75' 0.9500 . ? C76' C77' 1.361(12) . ? C76' H76' 0.9500 . ? C77' C78' 1.403(11) . ? C77' H77' 0.9500 . ? C78' C79' 1.669(12) . ? C79' C81' 1.486(13) . ? C79' C80' 1.551(12) . ? C79' H79' 1.0000 . ? C80' H80D 0.9800 . ? C80' H80E 0.9800 . ? C80' H80F 0.9800 . ? C81' H81D 0.9800 . ? C81' H81E 0.9800 . ? C81' H81F 0.9800 . ? N3 Y2 2.403(3) . ? N4 Y2 2.404(3) . ? N1 Y1 2.374(3) . ? N2 Y1 2.466(3) . ? O3 Y2 2.415(3) . ? O2 Y1 2.342(3) . ? O1 Y1 2.403(3) . ? Y2 Y1 3.3614(6) . ? Y2 H4 2.40(4) . ? Y2 H1 2.21(4) . ? Y2 H3 2.32(4) . ? Y2 H2 2.15(4) . ? Y1 H1 2.03(4) . ? Y1 H3 2.00(4) . ? Y1 H2 2.15(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 C4 C5' 102.0(10) . . ? O3 C4 C5 105.3(4) . . ? C5' C4 C5 38.3(13) . . ? O3 C4 H4A 111.4 . . ? C5' C4 H4A 111.4 . . ? C5 C4 H4A 75.0 . . ? O3 C4 H4B 111.4 . . ? C5' C4 H4B 111.4 . . ? C5 C4 H4B 137.5 . . ? H4A C4 H4B 109.2 . . ? C6 C5 C4 101.8(7) . . ? C6 C5 H5A 111.4 . . ? C4 C5 H5A 111.4 . . ? C6 C5 H5B 111.4 . . ? C4 C5 H5B 111.4 . . ? H5A C5 H5B 109.3 . . ? C6 C5' C4 108.0(17) . . ? C6 C5' H5'1 110.1 . . ? C4 C5' H5'1 110.1 . . ? C6 C5' H5'2 110.1 . . ? C4 C5' H5'2 110.1 . . ? H5'1 C5' H5'2 108.4 . . ? C5' C6 C7 105.3(12) . . ? C5' C6 C5 40.0(14) . . ? C7 C6 C5 104.2(5) . . ? C5' C6 H6A 110.7 . . ? C7 C6 H6A 110.7 . . ? C5 C6 H6A 74.3 . . ? C5' C6 H6B 110.7 . . ? C7 C6 H6B 110.7 . . ? C5 C6 H6B 140.5 . . ? H6A C6 H6B 108.8 . . ? O3 C7 C6 106.5(4) . . ? O3 C7 H7A 110.4 . . ? C6 C7 H7A 110.4 . . ? O3 C7 H7B 110.4 . . ? C6 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? O2 C8 C9 101.8(13) . . ? O2 C8 H8A 111.4 . . ? C9 C8 H8A 111.4 . . ? O2 C8 H8B 111.4 . . ? C9 C8 H8B 111.4 . . ? H8A C8 H8B 109.3 . . ? C10 C9 C8 103.5(19) . . ? C10 C9 H9A 111.1 . . ? C8 C9 H9A 111.1 . . ? C10 C9 H9B 111.1 . . ? C8 C9 H9B 111.1 . . ? H9A C9 H9B 109.0 . . ? C9 C10 C11 108.6(13) . . ? C9 C10 H10A 110.0 . . ? C11 C10 H10A 110.0 . . ? C9 C10 H10B 110.0 . . ? C11 C10 H10B 110.0 . . ? H10A C10 H10B 108.3 . . ? O2 C11 C10 103.1(10) . . ? O2 C11 H11A 111.1 . . ? C10 C11 H11A 111.1 . . ? O2 C11 H11B 111.1 . . ? C10 C11 H11B 111.1 . . ? H11A C11 H11B 109.1 . . ? C9' C8' O2 108.9(11) . . ? C9' C8' H8'1 109.9 . . ? O2 C8' H8'1 109.9 . . ? C9' C8' H8'2 109.9 . . ? O2 C8' H8'2 109.9 . . ? H8'1 C8' H8'2 108.3 . . ? C8' C9' C10' 101.4(16) . . ? C8' C9' H9C 111.5 . . ? C10' C9' H9C 111.5 . . ? C8' C9' H9D 111.5 . . ? C10' C9' H9D 111.5 . . ? H9C C9' H9D 109.3 . . ? C11' C10' C9' 108.4(12) . . ? C11' C10' H10C 110.0 . . ? C9' C10' H10C 110.0 . . ? C11' C10' H10D 110.0 . . ? C9' C10' H10D 110.0 . . ? H10C C10' H10D 108.4 . . ? C10' C11' O2 109.0(11) . . ? C10' C11' H11C 109.9 . . ? O2 C11' H11C 109.9 . . ? C10' C11' H11D 109.9 . . ? O2 C11' H11D 109.9 . . ? H11C C11' H11D 108.3 . . ? O1 C12 C13 93(2) . . ? O1 C12 H12A 113.0 . . ? C13 C12 H12A 113.0 . . ? O1 C12 H12B 113.0 . . ? C13 C12 H12B 113.0 . . ? H12A C12 H12B 110.4 . . ? C14 C13 C12 110.0(14) . . ? C14 C13 H13A 109.7 . . ? C12 C13 H13A 109.7 . . ? C14 C13 H13B 109.7 . . ? C12 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C13' C12' O1 116.7(16) . . ? C13' C12' H12C 108.1 . . ? O1 C12' H12C 108.1 . . ? C13' C12' H12D 108.1 . . ? O1 C12' H12D 108.1 . . ? H12C C12' H12D 107.3 . . ? C12' C13' C14 97.7(17) . . ? C12' C13' H13C 112.2 . . ? C14 C13' H13C 112.2 . . ? C12' C13' H13D 112.2 . . ? C14 C13' H13D 112.2 . . ? H13C C13' H13D 109.8 . . ? C13 C14 C15 107.6(13) . . ? C13 C14 C13' 10(3) . . ? C15 C14 C13' 104.6(11) . . ? C13 C14 H14A 100.8 . . ? C15 C14 H14A 110.8 . . ? C13' C14 H14A 110.8 . . ? C13 C14 H14B 117.4 . . ? C15 C14 H14B 110.8 . . ? C13' C14 H14B 110.8 . . ? H14A C14 H14B 108.9 . . ? O1 C15 C14 104.5(4) . . ? O1 C15 H15A 110.9 . . ? C14 C15 H15A 110.9 . . ? O1 C15 H15B 110.9 . . ? C14 C15 H15B 110.9 . . ? H15A C15 H15B 108.9 . . ? N4 C20 N3 113.6(3) . . ? N4 C20 C21 124.5(4) . . ? N3 C20 C21 121.9(4) . . ? N4 C20 Y2 57.11(19) . . ? N3 C20 Y2 57.08(19) . . ? C21 C20 Y2 170.4(3) . . ? C22 C21 C26 119.4(4) . . ? C22 C21 C20 119.8(4) . . ? C26 C21 C20 120.8(4) . . ? C21 C22 C23 120.6(5) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 118.8(6) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C25 C24 C23 121.2(5) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C26 120.2(6) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C21 C26 C25 119.7(5) . . ? C21 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C35 C27 C28 119.3(4) . . ? C35 C27 N3 119.6(4) . . ? C28 C27 N3 120.8(4) . . ? C32 C28 C27 118.4(4) . . ? C32 C28 C29 119.3(4) . . ? C27 C28 C29 122.3(4) . . ? C28 C29 C30 112.0(4) . . ? C28 C29 C31 110.2(4) . . ? C30 C29 C31 111.8(4) . . ? C28 C29 H29 107.5 . . ? C30 C29 H29 107.5 . . ? C31 C29 H29 107.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C28 122.2(5) . . ? C33 C32 H32 118.9 . . ? C28 C32 H32 118.9 . . ? C32 C33 C34 118.4(5) . . ? C32 C33 H33 120.8 . . ? C34 C33 H33 120.8 . . ? C33 C34 C35 122.2(5) . . ? C33 C34 H34 118.9 . . ? C35 C34 H34 118.9 . . ? C34 C35 C27 119.3(4) . . ? C34 C35 C36 118.9(4) . . ? C27 C35 C36 121.7(4) . . ? C37 C36 C35 112.3(4) . . ? C37 C36 C38 109.9(4) . . ? C35 C36 C38 110.6(4) . . ? C37 C36 H36 108.0 . . ? C35 C36 H36 108.0 . . ? C38 C36 H36 108.0 . . ? 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 . . ? C47 C39 C40 120.1(4) . . ? C47 C39 N4 123.1(4) . . ? C40 C39 N4 116.4(4) . . ? C44 C40 C39 118.2(4) . . ? C44 C40 C41 120.7(4) . . ? C39 C40 C41 121.0(4) . . ? C42 C41 C40 112.0(4) . . ? C42 C41 C43 108.6(4) . . ? C40 C41 C43 112.8(4) . . ? C42 C41 H41 107.7 . . ? C40 C41 H41 107.7 . . ? C43 C41 H41 107.7 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C40 121.8(5) . . ? C45 C44 H44 119.1 . . ? C40 C44 H44 119.1 . . ? C46 C45 C44 119.1(4) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? C45 C46 C47 122.3(4) . . ? C45 C46 H46 118.8 . . ? C47 C46 H46 118.8 . . ? C46 C47 C39 118.3(4) . . ? C46 C47 C48 118.0(4) . . ? C39 C47 C48 123.7(4) . . ? C50 C48 C47 111.9(4) . . ? C50 C48 C49 109.4(4) . . ? C47 C48 C49 111.1(4) . . ? C50 C48 H48 108.1 . . ? C47 C48 H48 108.1 . . ? C49 C48 H48 108.1 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N2 C51 N1 114.8(3) . . ? N2 C51 C52 123.3(4) . . ? N1 C51 C52 121.7(4) . . ? N2 C51 Y1 59.4(2) . . ? N1 C51 Y1 55.4(2) . . ? C52 C51 Y1 176.1(3) . . ? C57 C52 C53 118.1(4) . . ? C57 C52 C51 123.4(4) . . ? C53 C52 C51 118.5(4) . . ? C54 C53 C52 120.6(5) . . ? C54 C53 H53 119.7 . . ? C52 C53 H53 119.7 . . ? C55 C54 C53 121.2(6) . . ? C55 C54 H54 119.4 . . ? C53 C54 H54 119.4 . . ? C54 C55 C56 120.3(5) . . ? C54 C55 H55 119.8 . . ? C56 C55 H55 119.8 . . ? C55 C56 C57 119.3(5) . . ? C55 C56 H56 120.3 . . ? C57 C56 H56 120.3 . . ? C52 C57 C56 120.4(5) . . ? C52 C57 H57 119.8 . . ? C56 C57 H57 119.8 . . ? C66 C58 C59' 104.8(7) . . ? C66 C58 N1 130.6(7) . . ? C59' C58 N1 124.6(6) . . ? C66 C58 C66' 18.5(6) . . ? C59' C58 C66' 121.1(7) . . ? N1 C58 C66' 113.4(6) . . ? C66 C58 C59 118.9(7) . . ? C59' C58 C59 14.8(7) . . ? N1 C58 C59 110.5(6) . . ? C66' C58 C59 135.8(7) . . ? C63 C59 C60 117.1(10) . . ? C63 C59 C58 117.6(9) . . ? C60 C59 C58 124.8(9) . . ? C59 C60 C62 113.4(9) . . ? C59 C60 C61 94.5(9) . . ? C62 C60 C61 111.6(9) . . ? C59 C60 H60 112.1 . . ? C62 C60 H60 112.1 . . ? C61 C60 H60 112.1 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 C59 117.2(11) . . ? C64 C63 H63 121.4 . . ? C59 C63 H63 121.4 . . ? C63 C64 C65 124.7(11) . . ? C63 C64 H64 117.6 . . ? C65 C64 H64 117.6 . . ? C66 C65 C64 117.4(11) . . ? C66 C65 H65 121.3 . . ? C64 C65 H65 121.3 . . ? C58 C66 C65 123.9(10) . . ? C58 C66 C67 118.4(9) . . ? C65 C66 C67 117.5(11) . . ? C66 C67 C68 112.9(9) . . ? C66 C67 C69 112.2(9) . . ? C68 C67 C69 110.0(9) . . ? C66 C67 H67 107.1 . . ? C68 C67 H67 107.1 . . ? C69 C67 H67 107.1 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C58 C59' C63' 120.1(10) . . ? C58 C59' C60' 121.6(10) . . ? C63' C59' C60' 118.1(11) . . ? C59' C60' C62' 114.2(9) . . ? C59' C60' C61' 127.3(10) . . ? C62' C60' C61' 107.7(9) . . ? C59' C60' H60' 101.0 . . ? C62' C60' H60' 101.0 . . ? C61' C60' H60' 101.0 . . ? C60' C61' H61D 109.5 . . ? C60' C61' H61E 109.5 . . ? H61D C61' H61E 109.5 . . ? C60' C61' H61F 109.5 . . ? H61D C61' H61F 109.5 . . ? H61E C61' H61F 109.5 . . ? C60' C62' H62D 109.5 . . ? C60' C62' H62E 109.5 . . ? H62D C62' H62E 109.5 . . ? C60' C62' H62F 109.5 . . ? H62D C62' H62F 109.5 . . ? H62E C62' H62F 109.5 . . ? C64' C63' C59' 118.8(11) . . ? C64' C63' H63' 120.6 . . ? C59' C63' H63' 120.6 . . ? C63' C64' C65' 125.3(11) . . ? C63' C64' H64' 117.3 . . ? C65' C64' H64' 117.3 . . ? C66' C65' C64' 117.7(11) . . ? C66' C65' H65' 121.2 . . ? C64' C65' H65' 121.2 . . ? C65' C66' C67' 118.6(10) . . ? C65' C66' C58 116.3(9) . . ? C67' C66' C58 124.9(9) . . ? C66' C67' C68' 111.6(8) . . ? C66' C67' C69' 111.9(9) . . ? C68' C67' C69' 111.0(9) . . ? C66' C67' H67' 107.3 . . ? C68' C67' H67' 107.3 . . ? C69' C67' H67' 107.3 . . ? C67' C68' H68D 109.5 . . ? C67' C68' H68E 109.5 . . ? H68D C68' H68E 109.5 . . ? C67' C68' H68F 109.5 . . ? H68D C68' H68F 109.5 . . ? H68E C68' H68F 109.5 . . ? C67' C69' H69D 109.5 . . ? C67' C69' H69E 109.5 . . ? H69D C69' H69E 109.5 . . ? C67' C69' H69F 109.5 . . ? H69D C69' H69F 109.5 . . ? H69E C69' H69F 109.5 . . ? C71 C70 C78' 112.2(7) . . ? C71 C70 C78 114.9(7) . . ? C78' C70 C78 16.0(7) . . ? C71 C70 N2 127.9(7) . . ? C78' C70 N2 119.1(6) . . ? C78 C70 N2 117.0(6) . . ? C71 C70 C71' 13.7(7) . . ? C78' C70 C71' 125.3(7) . . ? C78 C70 C71' 128.6(7) . . ? N2 C70 C71' 114.2(6) . . ? C70 C71 C75 120.9(10) . . ? C70 C71 C72 118.8(10) . . ? C75 C71 C72 120.1(11) . . ? C71 C72 C73 111.3(10) . . ? C71 C72 C74 108.1(10) . . ? C73 C72 C74 108.8(10) . . ? C71 C72 H72 109.5 . . ? C73 C72 H72 109.5 . . ? C74 C72 H72 109.5 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C74 H74A 109.5 . . ? C72 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C72 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C76 C75 C71 120.8(11) . . ? C76 C75 H75 119.6 . . ? C71 C75 H75 119.6 . . ? C77 C76 C75 120.1(11) . . ? C77 C76 H76 120.0 . . ? C75 C76 H76 120.0 . . ? C76 C77 C78 118.0(11) . . ? C76 C77 H77 121.0 . . ? C78 C77 H77 121.0 . . ? C77 C78 C70 125.0(9) . . ? C77 C78 C79 110.4(10) . . ? C70 C78 C79 119.0(9) . . ? C80 C79 C78 119.7(10) . . ? C80 C79 C81 110.0(9) . . ? C78 C79 C81 93.3(9) . . ? C80 C79 H79 110.8 . . ? C78 C79 H79 110.8 . . ? C81 C79 H79 110.8 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C75' C71' C70 113.0(9) . . ? C75' C71' C72' 118.5(10) . . ? C70 C71' C72' 128.4(9) . . ? C73' C72' C71' 113.5(10) . . ? C73' C72' C74' 108.8(9) . . ? C71' C72' C74' 111.4(9) . . ? C73' C72' H72' 107.7 . . ? C71' C72' H72' 107.7 . . ? C74' C72' H72' 107.7 . . ? C72' C73' H73D 109.5 . . ? C72' C73' H73E 109.5 . . ? H73D C73' H73E 109.5 . . ? C72' C73' H73F 109.5 . . ? H73D C73' H73F 109.5 . . ? H73E C73' H73F 109.5 . . ? C72' C74' H74D 109.5 . . ? C72' C74' H74E 109.5 . . ? H74D C74' H74E 109.5 . . ? C72' C74' H74F 109.5 . . ? H74D C74' H74F 109.5 . . ? H74E C74' H74F 109.5 . . ? C76' C75' C71' 121.6(10) . . ? C76' C75' H75' 119.2 . . ? C71' C75' H75' 119.2 . . ? C77' C76' C75' 121.7(10) . . ? C77' C76' H76' 119.1 . . ? C75' C76' H76' 119.1 . . ? C76' C77' C78' 123.8(11) . . ? C76' C77' H77' 118.1 . . ? C78' C77' H77' 118.1 . . ? C70 C78' C77' 114.1(9) . . ? C70 C78' C79' 117.7(9) . . ? C77' C78' C79' 123.2(11) . . ? C81' C79' C80' 110.2(9) . . ? C81' C79' C78' 128.3(9) . . ? C80' C79' C78' 104.0(8) . . ? C81' C79' H79' 104.0 . . ? C80' C79' H79' 104.0 . . ? C78' C79' H79' 104.0 . . ? C79' C80' H80D 109.5 . . ? C79' C80' H80E 109.5 . . ? H80D C80' H80E 109.5 . . ? C79' C80' H80F 109.5 . . ? H80D C80' H80F 109.5 . . ? H80E C80' H80F 109.5 . . ? C79' C81' H81D 109.5 . . ? C79' C81' H81E 109.5 . . ? H81D C81' H81E 109.5 . . ? C79' C81' H81F 109.5 . . ? H81D C81' H81F 109.5 . . ? H81E C81' H81F 109.5 . . ? C20 N3 C27 123.0(3) . . ? C20 N3 Y2 95.0(2) . . ? C27 N3 Y2 141.5(2) . . ? C20 N4 C39 124.3(3) . . ? C20 N4 Y2 95.0(2) . . ? C39 N4 Y2 138.3(3) . . ? C51 N1 C58 122.5(3) . . ? C51 N1 Y1 97.0(3) . . ? C58 N1 Y1 137.5(3) . . ? C51 N2 C70 121.2(4) . . ? C51 N2 Y1 93.1(2) . . ? C70 N2 Y1 144.9(3) . . ? C4 O3 C7 108.5(3) . . ? C4 O3 Y2 123.6(2) . . ? C7 O3 Y2 127.0(3) . . ? C8 O2 C11 110.5(9) . . ? C8 O2 C11' 107.8(10) . . ? C11 O2 C11' 23.1(9) . . ? C8 O2 C8' 21.7(8) . . ? C11 O2 C8' 113.9(9) . . ? C11' O2 C8' 102.5(9) . . ? C8 O2 Y1 124.2(7) . . ? C11 O2 Y1 123.6(7) . . ? C11' O2 Y1 127.1(7) . . ? C8' O2 Y1 121.8(6) . . ? C12 O1 C15 108.2(9) . . ? C12 O1 C12' 23.0(15) . . ? C15 O1 C12' 104.7(9) . . ? C12 O1 Y1 126.0(9) . . ? C15 O1 Y1 125.3(3) . . ? C12' O1 Y1 121.6(10) . . ? N3 Y2 N4 55.59(11) . . ? N3 Y2 O3 135.93(10) . . ? N4 Y2 O3 80.40(10) . . ? N3 Y2 C20 27.96(11) . . ? N4 Y2 C20 27.85(11) . . ? O3 Y2 C20 107.98(11) . . ? N3 Y2 Y1 111.31(7) . . ? N4 Y2 Y1 141.49(8) . . ? O3 Y2 Y1 104.51(7) . . ? C20 Y2 Y1 132.44(8) . . ? N3 Y2 H4 96.9(8) . . ? N4 Y2 H4 100.7(9) . . ? O3 Y2 H4 88.3(9) . . ? C20 Y2 H4 97.4(8) . . ? Y1 Y2 H4 117.5(9) . . ? N3 Y2 H1 146.3(10) . . ? N4 Y2 H1 149.4(10) . . ? O3 Y2 H1 75.1(10) . . ? C20 Y2 H1 165.6(10) . . ? Y1 Y2 H1 35.7(10) . . ? H4 Y2 H1 96.7(13) . . ? N3 Y2 H3 96.7(11) . . ? N4 Y2 H3 106.2(11) . . ? O3 Y2 H3 97.8(11) . . ? C20 Y2 H3 105.5(11) . . ? Y1 Y2 H3 35.6(11) . . ? H4 Y2 H3 153.1(14) . . ? H1 Y2 H3 60.2(15) . . ? N3 Y2 H2 84.2(10) . . ? N4 Y2 H2 137.9(10) . . ? O3 Y2 H2 138.9(10) . . ? C20 Y2 H2 111.9(10) . . ? Y1 Y2 H2 38.5(10) . . ? H4 Y2 H2 95.8(14) . . ? H1 Y2 H2 63.8(14) . . ? H3 Y2 H2 62.6(15) . . ? O2 Y1 N1 93.92(12) . . ? O2 Y1 O1 88.86(14) . . ? N1 Y1 O1 136.95(11) . . ? O2 Y1 N2 95.60(12) . . ? N1 Y1 N2 55.12(11) . . ? O1 Y1 N2 81.85(11) . . ? O2 Y1 C51 95.56(11) . . ? N1 Y1 C51 27.59(11) . . ? O1 Y1 C51 109.37(12) . . ? N2 Y1 C51 27.53(11) . . ? O2 Y1 Y2 104.60(8) . . ? N1 Y1 Y2 114.18(8) . . ? O1 Y1 Y2 106.50(7) . . ? N2 Y1 Y2 158.13(9) . . ? C51 Y1 Y2 138.90(9) . . ? O2 Y1 H1 87.3(11) . . ? N1 Y1 H1 80.6(11) . . ? O1 Y1 H1 142.5(11) . . ? N2 Y1 H1 135.7(11) . . ? C51 Y1 H1 108.2(11) . . ? Y2 Y1 H1 39.5(11) . . ? O2 Y1 H3 146.6(12) . . ? N1 Y1 H3 104.1(12) . . ? O1 Y1 H3 96.3(12) . . ? N2 Y1 H3 117.7(12) . . ? C51 Y1 H3 113.4(12) . . ? Y2 Y1 H3 42.4(12) . . ? H1 Y1 H3 68.7(17) . . ? O2 Y1 H2 81.5(11) . . ? N1 Y1 H2 147.3(10) . . ? O1 Y1 H2 75.6(10) . . ? N2 Y1 H2 157.2(11) . . ? C51 Y1 H2 174.3(10) . . ? Y2 Y1 H2 38.6(11) . . ? H1 Y1 H2 67.0(15) . . ? H3 Y1 H2 68.2(16) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.861 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.076 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.000 0.214 0.565 7 0 ' ' 2 -0.017 0.250 0.133 9 0 ' ' 3 0.017 0.750 0.867 9 0 ' ' 4 0.000 0.786 0.435 7 0 ' ' 5 0.118 0.557 0.381 20 0 ' ' 6 0.500 0.075 0.500 690 106 ' ' 7 0.392 0.194 0.968 20 1 ' ' 8 0.445 0.662 0.958 11 0 ' ' 9 0.555 0.338 0.042 11 0 ' ' 10 0.608 0.806 0.032 20 1 ' ' 11 0.882 0.443 0.619 20 0 ' ' _platon_squeeze_details ; One disorder hexane molecule per formual unit of [(Ph-NCN)YH2]2(THF)3 was not modelled and the disordered density was taken into account using the SQUEEZE/PLATON procedure.(Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194?01) as implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst. 2003, 36, 7?3. PLATON - a multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands). ; _vrf_PLAT305_II-035-02 ; PROBLEM: Isolated Hydrogen Atom (Outside Bond Range ??) H4 RESPONSE: All the hydrides (H1~H4) were located by difference Fourier syntheses. The coordinates and isotropic parameters were refined for H1, H2 and H3. Only the displace parameter was refined for H4 while the coordinates were constrained. ; data_1-Lu _database_code_depnum_ccdc_archive 'CCDC 859484' #TrackingRef '- Ln2H4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((Ph-NCN)LuH2)2(THF)3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H114 Lu2 N4 O3' _chemical_formula_weight 1541.70 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' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2117(18) _cell_length_b 14.827(2) _cell_length_c 23.057(3) _cell_angle_alpha 81.780(2) _cell_angle_beta 73.628(2) _cell_angle_gamma 66.103(2) _cell_volume 3960.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 2.524 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4720 _exptl_absorpt_correction_T_max 0.7033 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 21538 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.04 _reflns_number_total 13729 _reflns_number_gt 11107 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0713P)^2^+5.5405P] 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 13729 _refine_ls_number_parameters 798 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1317 _refine_ls_wR_factor_gt 0.1252 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 O3 O 0.3165(6) 0.6182(4) 0.8108(3) 0.0719(19) Uani 1 1 d . . . C5 C 0.2618(18) 0.659(2) 0.8775(13) 0.092(3) Uani 0.440(14) 1 d PD A 2 H5A H 0.1904 0.7181 0.8795 0.110 Uiso 0.440(14) 1 calc PR A 2 H5B H 0.2458 0.6079 0.9070 0.110 Uiso 0.440(14) 1 calc PR A 2 C6 C 0.3487(19) 0.682(2) 0.8877(14) 0.092(3) Uani 0.440(14) 1 d PD A 2 H6A H 0.3649 0.6532 0.9271 0.110 Uiso 0.440(14) 1 calc PR A 2 H6B H 0.3250 0.7544 0.8880 0.110 Uiso 0.440(14) 1 calc PR A 2 C7 C 0.454(2) 0.6386(19) 0.8364(12) 0.092(3) Uani 0.440(14) 1 d PD A 2 H7A H 0.5264 0.6224 0.8482 0.110 Uiso 0.440(14) 1 calc PR A 2 H7B H 0.4527 0.6811 0.7992 0.110 Uiso 0.440(14) 1 calc PR A 2 C8 C 0.431(2) 0.5424(18) 0.8309(14) 0.092(3) Uani 0.440(14) 1 d PD A 2 H8A H 0.4165 0.5060 0.8698 0.110 Uiso 0.440(14) 1 calc PR A 2 H8B H 0.4888 0.4975 0.7989 0.110 Uiso 0.440(14) 1 calc PR A 2 C5' C 0.3033(17) 0.7052(15) 0.8303(10) 0.092(3) Uani 0.560(14) 1 d PD A 1 H5'1 H 0.2231 0.7383 0.8533 0.110 Uiso 0.560(14) 1 calc PR A 1 H5'2 H 0.3182 0.7484 0.7948 0.110 Uiso 0.560(14) 1 calc PR A 1 C6' C 0.3773(17) 0.6944(18) 0.8677(11) 0.092(3) Uani 0.560(14) 1 d PD A 1 H6'1 H 0.3364 0.6957 0.9110 0.110 Uiso 0.560(14) 1 calc PR A 1 H6'2 H 0.4057 0.7485 0.8589 0.110 Uiso 0.560(14) 1 calc PR A 1 C7' C 0.4754(16) 0.5958(16) 0.8533(12) 0.092(3) Uani 0.560(14) 1 d PD A 1 H7'1 H 0.4821 0.5507 0.8894 0.110 Uiso 0.560(14) 1 calc PR A 1 H7'2 H 0.5491 0.6030 0.8346 0.110 Uiso 0.560(14) 1 calc PR A 1 C8' C 0.4312(18) 0.5616(17) 0.8063(12) 0.092(3) Uani 0.560(14) 1 d PD A 1 H8'1 H 0.4760 0.5684 0.7647 0.110 Uiso 0.560(14) 1 calc PR A 1 H8'2 H 0.4424 0.4912 0.8144 0.110 Uiso 0.560(14) 1 calc PR A 1 C9 C 0.0994(7) 0.2660(6) 0.7830(4) 0.059(2) Uani 1 1 d . . . H9A H 0.0570 0.3197 0.8122 0.071 Uiso 1 1 calc R B 1 H9B H 0.0817 0.2074 0.8000 0.071 Uiso 1 1 calc R B 1 C10 C 0.0810(18) 0.2403(19) 0.7257(9) 0.064(3) Uani 0.511(16) 1 d P C 2 H10A H 0.1003 0.1687 0.7243 0.077 Uiso 0.511(16) 1 calc PR C 2 H10B H 0.0015 0.2774 0.7220 0.077 Uiso 0.511(16) 1 calc PR C 2 C11 C 0.164(2) 0.2731(19) 0.6784(11) 0.064(3) Uani 0.511(16) 1 d P C 2 H11A H 0.1394 0.3459 0.6760 0.077 Uiso 0.511(16) 1 calc PR C 2 H11B H 0.1776 0.2486 0.6381 0.077 Uiso 0.511(16) 1 calc PR C 2 C10' C 0.0699(19) 0.2990(19) 0.7216(10) 0.064(3) Uani 0.489(16) 1 d P C 1 H10C H 0.0655 0.3671 0.7099 0.077 Uiso 0.489(16) 1 calc PR C 1 H10D H -0.0031 0.2948 0.7217 0.077 Uiso 0.489(16) 1 calc PR C 1 C11' C 0.172(2) 0.2228(19) 0.6800(11) 0.064(3) Uani 0.489(16) 1 d P C 1 H11C H 0.1811 0.2451 0.6369 0.077 Uiso 0.489(16) 1 calc PR C 1 H11D H 0.1671 0.1574 0.6849 0.077 Uiso 0.489(16) 1 calc PR C 1 C12 C 0.2698(7) 0.2221(8) 0.7051(4) 0.066(2) Uani 1 1 d . . . H12A H 0.3341 0.1570 0.6995 0.079 Uiso 1 1 calc R C 1 H12B H 0.2984 0.2733 0.6838 0.079 Uiso 1 1 calc R C 1 C13 C 0.1800(8) 0.2097(7) 0.9284(5) 0.0909(18) Uani 1 1 d . . . H13A H 0.2537 0.1784 0.9400 0.109 Uiso 1 1 calc R . . H13B H 0.1751 0.1638 0.9030 0.109 Uiso 1 1 calc R . . C14 C 0.0823(8) 0.2327(7) 0.9838(5) 0.0909(18) Uani 1 1 d . . . H14A H 0.0502 0.1810 0.9928 0.109 Uiso 1 1 calc R . . H14B H 0.1069 0.2386 1.0194 0.109 Uiso 1 1 calc R . . C15 C -0.0028(8) 0.3291(7) 0.9676(5) 0.0909(18) Uani 1 1 d . . . H15A H -0.0555 0.3183 0.9487 0.109 Uiso 1 1 calc R . . H15B H -0.0482 0.3685 1.0040 0.109 Uiso 1 1 calc R . . C16 C 0.0635(8) 0.3806(7) 0.9245(5) 0.0909(18) Uani 1 1 d . . . H16A H 0.0782 0.4255 0.9459 0.109 Uiso 1 1 calc R . . H16B H 0.0215 0.4197 0.8940 0.109 Uiso 1 1 calc R . . C20 C 0.1399(5) 0.6761(4) 0.6770(3) 0.0289(13) Uani 1 1 d . . . C21 C 0.0915(5) 0.7499(5) 0.6303(3) 0.0307(13) Uani 1 1 d . A . C22 C 0.1602(6) 0.7823(5) 0.5819(3) 0.0382(15) Uani 1 1 d . . . H22 H 0.2405 0.7568 0.5772 0.046 Uiso 1 1 calc R A . C23 C 0.1114(6) 0.8520(5) 0.5405(3) 0.0465(17) Uani 1 1 d . A . H23 H 0.1587 0.8742 0.5076 0.056 Uiso 1 1 calc R . . C24 C -0.0043(7) 0.8892(5) 0.5463(4) 0.0501(19) Uani 1 1 d . . . H24 H -0.0367 0.9370 0.5176 0.060 Uiso 1 1 calc R A . C25 C -0.0727(6) 0.8576(5) 0.5934(4) 0.0513(19) Uani 1 1 d . A . H25 H -0.1527 0.8823 0.5971 0.062 Uiso 1 1 calc R . . C26 C -0.0250(6) 0.7887(5) 0.6360(3) 0.0416(16) Uani 1 1 d . . . H26 H -0.0732 0.7684 0.6694 0.050 Uiso 1 1 calc R A . C27 C 0.0343(5) 0.5759(4) 0.6746(3) 0.0332(14) Uani 1 1 d . . . C28 C 0.0779(6) 0.5390(5) 0.6156(3) 0.0387(15) Uani 1 1 d . A . C29 C 0.1942(6) 0.5284(5) 0.5776(3) 0.0469(17) Uani 1 1 d . . . H29 H 0.2174 0.5731 0.5948 0.056 Uiso 1 1 calc R A . C30 C 0.1961(8) 0.5628(8) 0.5125(4) 0.082(3) Uani 1 1 d . A . H30A H 0.2742 0.5548 0.4903 0.124 Uiso 1 1 calc R . . H30B H 0.1454 0.6325 0.5110 0.124 Uiso 1 1 calc R . . H30C H 0.1699 0.5234 0.4940 0.124 Uiso 1 1 calc R . . C31 C 0.2826(7) 0.4253(7) 0.5826(5) 0.081(3) Uani 1 1 d . A . H31A H 0.3574 0.4219 0.5574 0.121 Uiso 1 1 calc R . . H31B H 0.2610 0.3777 0.5687 0.121 Uiso 1 1 calc R . . H31C H 0.2867 0.4094 0.6248 0.121 Uiso 1 1 calc R . . C32 C 0.0106(7) 0.5057(6) 0.5938(4) 0.053(2) Uani 1 1 d . . . H32 H 0.0381 0.4800 0.5544 0.064 Uiso 1 1 calc R A . C33 C -0.0949(7) 0.5096(6) 0.6285(4) 0.059(2) Uani 1 1 d . A . H33 H -0.1398 0.4877 0.6127 0.071 Uiso 1 1 calc R . . C34 C -0.1344(7) 0.5447(6) 0.6853(4) 0.054(2) Uani 1 1 d . . . H34 H -0.2067 0.5461 0.7087 0.064 Uiso 1 1 calc R A . C35 C -0.0731(6) 0.5785(5) 0.7100(3) 0.0394(15) Uani 1 1 d . A . C36 C -0.1237(6) 0.6197(6) 0.7735(3) 0.053(2) Uani 1 1 d . . . H36 H -0.0679 0.6401 0.7843 0.064 Uiso 1 1 calc R A . C37 C -0.2377(9) 0.7094(7) 0.7778(5) 0.090(3) Uani 1 1 d . A . H37A H -0.2668 0.7343 0.8189 0.135 Uiso 1 1 calc R . . H37B H -0.2934 0.6896 0.7683 0.135 Uiso 1 1 calc R . . H37C H -0.2253 0.7615 0.7489 0.135 Uiso 1 1 calc R . . C38 C -0.1475(9) 0.5425(7) 0.8194(4) 0.082(3) Uani 1 1 d . A . H38A H -0.1789 0.5699 0.8598 0.123 Uiso 1 1 calc R . . H38B H -0.0762 0.4848 0.8187 0.123 Uiso 1 1 calc R . . H38C H -0.2027 0.5226 0.8094 0.123 Uiso 1 1 calc R . . C39 C 0.2715(5) 0.7494(5) 0.6832(3) 0.0359(15) Uani 1 1 d . . . C40 C 0.3887(6) 0.7160(6) 0.6555(3) 0.0484(19) Uani 1 1 d . A . C41 C 0.4583(6) 0.6106(6) 0.6396(4) 0.064(2) Uani 1 1 d . . . H41 H 0.4211 0.5695 0.6686 0.077 Uiso 1 1 calc R A . C42 C 0.4594(7) 0.5921(8) 0.5777(5) 0.089(3) Uani 1 1 d . A . H42A H 0.5050 0.5224 0.5689 0.133 Uiso 1 1 calc R . . H42B H 0.4929 0.6333 0.5482 0.133 Uiso 1 1 calc R . . H42C H 0.3810 0.6086 0.5752 0.133 Uiso 1 1 calc R . . C43 C 0.5825(7) 0.5740(8) 0.6449(5) 0.091(4) Uani 1 1 d . A . H43A H 0.6226 0.5045 0.6341 0.137 Uiso 1 1 calc R . . H43B H 0.5827 0.5805 0.6866 0.137 Uiso 1 1 calc R . . H43C H 0.6211 0.6135 0.6174 0.137 Uiso 1 1 calc R . . C44 C 0.4369(7) 0.7874(7) 0.6399(4) 0.066(3) Uani 1 1 d . . . H44 H 0.5160 0.7667 0.6204 0.079 Uiso 1 1 calc R A . C45 C 0.3773(7) 0.8837(7) 0.6512(4) 0.059(2) Uani 1 1 d . A . H45 H 0.4131 0.9298 0.6384 0.071 Uiso 1 1 calc R . . C46 C 0.2643(7) 0.9146(6) 0.6814(3) 0.0513(19) Uani 1 1 d . . . H46 H 0.2228 0.9821 0.6912 0.062 Uiso 1 1 calc R A . C47 C 0.2086(6) 0.8488(5) 0.6981(3) 0.0403(16) Uani 1 1 d . A . C48 C 0.0845(6) 0.8876(5) 0.7328(3) 0.0435(16) Uani 1 1 d . . . H48 H 0.0567 0.8326 0.7390 0.052 Uiso 1 1 calc R A . C49 C 0.0108(7) 0.9721(6) 0.6972(4) 0.057(2) Uani 1 1 d . A . H49A H -0.0690 0.9957 0.7206 0.085 Uiso 1 1 calc R . . H49B H 0.0166 0.9481 0.6585 0.085 Uiso 1 1 calc R . . H49C H 0.0378 1.0263 0.6899 0.085 Uiso 1 1 calc R . . C50 C 0.0716(8) 0.9223(8) 0.7956(4) 0.074(3) Uani 1 1 d . A . H50A H -0.0091 0.9469 0.8175 0.111 Uiso 1 1 calc R . . H50B H 0.1001 0.9753 0.7904 0.111 Uiso 1 1 calc R . . H50C H 0.1158 0.8668 0.8186 0.111 Uiso 1 1 calc R . . C51 C 0.5090(5) 0.1826(4) 0.8263(3) 0.0317(14) Uani 1 1 d . A . C52 C 0.6007(5) 0.0957(4) 0.8478(3) 0.0354(15) Uani 1 1 d . . . C53 C 0.5902(7) 0.0799(5) 0.9095(3) 0.0491(18) Uani 1 1 d . . . H53 H 0.5286 0.1257 0.9367 0.059 Uiso 1 1 calc R . . C54 C 0.6697(8) -0.0032(6) 0.9323(4) 0.063(2) Uani 1 1 d . . . H54 H 0.6606 -0.0140 0.9748 0.076 Uiso 1 1 calc R . . C55 C 0.7608(8) -0.0690(6) 0.8933(4) 0.063(2) Uani 1 1 d . . . H55 H 0.8155 -0.1248 0.9084 0.076 Uiso 1 1 calc R . . C56 C 0.7708(6) -0.0527(5) 0.8331(4) 0.0513(19) Uani 1 1 d . . . H56 H 0.8333 -0.0979 0.8060 0.062 Uiso 1 1 calc R . . C57 C 0.6920(5) 0.0286(5) 0.8097(3) 0.0416(16) Uani 1 1 d . . . H57 H 0.7012 0.0377 0.7671 0.050 Uiso 1 1 calc R . . C58 C 0.5079(5) 0.0930(5) 0.7470(3) 0.0344(14) Uani 1 1 d . . . C59 C 0.4875(5) 0.0074(5) 0.7716(3) 0.0357(14) Uani 1 1 d . . . C60 C 0.4139(6) 0.0018(5) 0.8337(3) 0.0418(16) Uani 1 1 d . . . H60 H 0.3921 0.0645 0.8542 0.050 Uiso 1 1 calc R . . C61 C 0.3038(6) -0.0048(6) 0.8282(4) 0.0526(19) Uani 1 1 d . . . H61A H 0.2555 -0.0084 0.8687 0.079 Uiso 1 1 calc R . . H61B H 0.3233 -0.0640 0.8065 0.079 Uiso 1 1 calc R . . H61C H 0.2626 0.0538 0.8060 0.079 Uiso 1 1 calc R . . C62 C 0.4754(7) -0.0845(6) 0.8729(4) 0.0535(19) Uani 1 1 d . . . H62A H 0.4238 -0.0845 0.9129 0.080 Uiso 1 1 calc R . . H62B H 0.5434 -0.0773 0.8773 0.080 Uiso 1 1 calc R . . H62C H 0.4983 -0.1468 0.8535 0.080 Uiso 1 1 calc R . . C63 C 0.5351(6) -0.0739(5) 0.7354(3) 0.0480(18) Uani 1 1 d . . . H63 H 0.5234 -0.1326 0.7515 0.058 Uiso 1 1 calc R . . C64 C 0.5983(6) -0.0725(6) 0.6771(4) 0.054(2) Uani 1 1 d . . . H64 H 0.6327 -0.1303 0.6540 0.065 Uiso 1 1 calc R . . C65 C 0.6117(6) 0.0133(6) 0.6521(4) 0.054(2) Uani 1 1 d . . . H65 H 0.6524 0.0150 0.6111 0.065 Uiso 1 1 calc R . . C66 C 0.5669(6) 0.0975(5) 0.6859(3) 0.0432(16) Uani 1 1 d . . . C67 C 0.5868(7) 0.1895(6) 0.6567(3) 0.054(2) Uani 1 1 d . . . H67 H 0.5378 0.2456 0.6843 0.065 Uiso 1 1 calc R . . C68 C 0.5557(8) 0.2164(8) 0.5965(4) 0.084(3) Uani 1 1 d . . . H68A H 0.5691 0.2762 0.5792 0.125 Uiso 1 1 calc R . . H68B H 0.4749 0.2285 0.6023 0.125 Uiso 1 1 calc R . . H68C H 0.6030 0.1621 0.5688 0.125 Uiso 1 1 calc R . . C69 C 0.7121(7) 0.1749(6) 0.6473(4) 0.061(2) Uani 1 1 d . . . H69A H 0.7230 0.2351 0.6288 0.091 Uiso 1 1 calc R . . H69B H 0.7615 0.1196 0.6206 0.091 Uiso 1 1 calc R . . H69C H 0.7319 0.1606 0.6864 0.091 Uiso 1 1 calc R . . C70 C 0.5149(6) 0.3012(4) 0.8869(3) 0.0362(15) Uani 1 1 d . . . C71 C 0.4571(6) 0.3358(5) 0.9454(3) 0.0417(16) Uani 1 1 d . . . C72 C 0.3410(6) 0.3341(5) 0.9782(3) 0.0472(17) Uani 1 1 d . . . H72 H 0.3157 0.3063 0.9504 0.057 Uiso 1 1 calc R . . C73 C 0.2504(7) 0.4367(6) 0.9951(4) 0.060(2) Uani 1 1 d . . . H73A H 0.1771 0.4314 1.0157 0.090 Uiso 1 1 calc R . . H73B H 0.2424 0.4786 0.9583 0.090 Uiso 1 1 calc R . . H73C H 0.2734 0.4660 1.0221 0.090 Uiso 1 1 calc R . . C74 C 0.3481(8) 0.2664(6) 1.0355(4) 0.068(2) Uani 1 1 d . . . H74A H 0.2723 0.2662 1.0557 0.101 Uiso 1 1 calc R . . H74B H 0.3752 0.2908 1.0630 0.101 Uiso 1 1 calc R . . H74C H 0.4014 0.1991 1.0242 0.101 Uiso 1 1 calc R . . C75 C 0.5088(8) 0.3733(6) 0.9760(4) 0.056(2) Uani 1 1 d . . . H75 H 0.4704 0.3957 1.0159 0.067 Uiso 1 1 calc R . . C76 C 0.6124(8) 0.3787(6) 0.9502(5) 0.069(3) Uani 1 1 d . . . H76 H 0.6454 0.4052 0.9716 0.083 Uiso 1 1 calc R . . C77 C 0.6690(7) 0.3451(6) 0.8925(4) 0.059(2) Uani 1 1 d . . . H77 H 0.7414 0.3487 0.8746 0.071 Uiso 1 1 calc R . . C78 C 0.6230(6) 0.3061(5) 0.8598(3) 0.0454(17) Uani 1 1 d . . . C79 C 0.6912(6) 0.2744(6) 0.7959(4) 0.054(2) Uani 1 1 d . . . H79 H 0.6525 0.2407 0.7804 0.064 Uiso 1 1 calc R . . C80 C 0.6945(11) 0.3633(8) 0.7535(5) 0.105(4) Uani 1 1 d . . . H80A H 0.7389 0.3405 0.7128 0.157 Uiso 1 1 calc R . . H80B H 0.7302 0.3987 0.7685 0.157 Uiso 1 1 calc R . . H80C H 0.6164 0.4078 0.7521 0.157 Uiso 1 1 calc R . . C81 C 0.8124(7) 0.2008(8) 0.7954(5) 0.087(3) Uani 1 1 d . . . H81A H 0.8544 0.1812 0.7538 0.130 Uiso 1 1 calc R . . H81B H 0.8091 0.1423 0.8205 0.130 Uiso 1 1 calc R . . H81C H 0.8514 0.2315 0.8116 0.130 Uiso 1 1 calc R . . C101 C 0.1402(9) 0.2538(7) 0.5110(4) 0.069(2) Uani 1 1 d . . . H101 H 0.0848 0.3176 0.5056 0.083 Uiso 1 1 calc R . . C102 C 0.2532(10) 0.2287(9) 0.4789(5) 0.084(3) Uani 1 1 d . . . H102 H 0.2749 0.2763 0.4520 0.101 Uiso 1 1 calc R . . C103 C 0.3343(10) 0.1365(10) 0.4851(5) 0.095(4) Uani 1 1 d . . . H103 H 0.4118 0.1202 0.4634 0.114 Uiso 1 1 calc R . . C104 C 0.3012(9) 0.0681(8) 0.5235(4) 0.086(3) Uani 1 1 d . . . H104 H 0.3561 0.0037 0.5279 0.103 Uiso 1 1 calc R . . C105 C 0.1892(8) 0.0921(7) 0.5555(4) 0.068(2) Uani 1 1 d . . . H105 H 0.1669 0.0437 0.5810 0.081 Uiso 1 1 calc R . . C106 C 0.1091(7) 0.1864(7) 0.5506(4) 0.059(2) Uani 1 1 d . . . C107 C -0.0133(8) 0.2162(8) 0.5865(4) 0.082(3) Uani 1 1 d . . . H10E H -0.0228 0.1605 0.6128 0.124 Uiso 1 1 calc R . . H10F H -0.0634 0.2351 0.5588 0.124 Uiso 1 1 calc R . . H10G H -0.0335 0.2723 0.6113 0.124 Uiso 1 1 calc R . . N3 N 0.1011(4) 0.6058(4) 0.7016(2) 0.0282(11) Uani 1 1 d . A . N4 N 0.2222(4) 0.6772(4) 0.6993(2) 0.0345(12) Uani 1 1 d . A . N1 N 0.4644(4) 0.1798(4) 0.7822(2) 0.0340(12) Uani 1 1 d . A . N2 N 0.4585(5) 0.2701(4) 0.8535(2) 0.0344(12) Uani 1 1 d . A . O1 O 0.2225(4) 0.2423(3) 0.7687(2) 0.0451(12) Uani 1 1 d . A . O2 O 0.1718(4) 0.3026(3) 0.8953(2) 0.0453(11) Uani 1 1 d . A . Lu2 Lu 0.19732(2) 0.562458(18) 0.779209(11) 0.03121(9) Uani 1 1 d . A . Lu1 Lu 0.30238(2) 0.327761(19) 0.809810(12) 0.03114(9) Uani 1 1 d . . . H2 H 0.262(5) 0.459(4) 0.848(3) 0.035(17) Uiso 1 1 d . . . H3 H 0.156(5) 0.438(4) 0.793(3) 0.032(16) Uiso 1 1 d . . . H4 H 0.0526 0.6599 0.8526 0.050 Uiso 1 1 d . . . H1 H 0.3440 0.4428 0.7508 0.08(3) 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 O3 0.141(6) 0.061(4) 0.060(4) 0.025(3) -0.069(4) -0.064(4) C5 0.087(5) 0.096(7) 0.114(9) -0.035(7) -0.045(5) -0.033(4) C6 0.087(5) 0.096(7) 0.114(9) -0.035(7) -0.045(5) -0.033(4) C7 0.087(5) 0.096(7) 0.114(9) -0.035(7) -0.045(5) -0.033(4) C8 0.087(5) 0.096(7) 0.114(9) -0.035(7) -0.045(5) -0.033(4) C5' 0.087(5) 0.096(7) 0.114(9) -0.035(7) -0.045(5) -0.033(4) C6' 0.087(5) 0.096(7) 0.114(9) -0.035(7) -0.045(5) -0.033(4) C7' 0.087(5) 0.096(7) 0.114(9) -0.035(7) -0.045(5) -0.033(4) C8' 0.087(5) 0.096(7) 0.114(9) -0.035(7) -0.045(5) -0.033(4) C9 0.052(5) 0.060(5) 0.073(6) -0.010(4) -0.013(4) -0.027(4) C10 0.070(5) 0.079(10) 0.072(6) 0.011(10) -0.039(4) -0.046(10) C11 0.070(5) 0.079(10) 0.072(6) 0.011(10) -0.039(4) -0.046(10) C10' 0.070(5) 0.079(10) 0.072(6) 0.011(10) -0.039(4) -0.046(10) C11' 0.070(5) 0.079(10) 0.072(6) 0.011(10) -0.039(4) -0.046(10) C12 0.051(5) 0.104(7) 0.049(5) -0.007(5) -0.024(4) -0.027(5) C13 0.071(3) 0.056(3) 0.104(4) 0.020(3) 0.011(3) -0.012(2) C14 0.071(3) 0.056(3) 0.104(4) 0.020(3) 0.011(3) -0.012(2) C15 0.071(3) 0.056(3) 0.104(4) 0.020(3) 0.011(3) -0.012(2) C16 0.071(3) 0.056(3) 0.104(4) 0.020(3) 0.011(3) -0.012(2) C20 0.030(3) 0.028(3) 0.025(3) 0.001(3) -0.005(2) -0.009(3) C21 0.038(3) 0.033(3) 0.029(3) 0.004(3) -0.013(3) -0.020(3) C22 0.046(4) 0.045(4) 0.027(3) 0.008(3) -0.016(3) -0.018(3) C23 0.065(5) 0.042(4) 0.039(4) 0.013(3) -0.015(3) -0.032(4) C24 0.073(5) 0.039(4) 0.061(5) 0.026(4) -0.046(4) -0.032(4) C25 0.045(4) 0.037(4) 0.076(5) 0.016(4) -0.029(4) -0.017(3) C26 0.044(4) 0.030(4) 0.053(4) 0.011(3) -0.016(3) -0.018(3) C27 0.043(4) 0.021(3) 0.038(4) 0.004(3) -0.015(3) -0.013(3) C28 0.057(4) 0.026(3) 0.035(4) 0.002(3) -0.019(3) -0.013(3) C29 0.054(4) 0.040(4) 0.037(4) -0.004(3) -0.009(3) -0.010(3) C30 0.081(6) 0.112(9) 0.048(5) 0.012(5) -0.019(5) -0.034(6) C31 0.056(5) 0.058(6) 0.101(8) 0.000(5) -0.010(5) 0.000(5) C32 0.069(5) 0.045(4) 0.052(5) -0.009(4) -0.028(4) -0.016(4) C33 0.068(5) 0.063(5) 0.072(6) 0.003(4) -0.036(5) -0.039(5) C34 0.052(4) 0.054(5) 0.070(5) 0.008(4) -0.027(4) -0.031(4) C35 0.044(4) 0.034(4) 0.045(4) 0.003(3) -0.013(3) -0.020(3) C36 0.047(4) 0.076(6) 0.043(4) -0.007(4) 0.000(3) -0.036(4) C37 0.105(8) 0.055(6) 0.072(7) 0.008(5) 0.003(6) -0.011(6) C38 0.092(7) 0.066(6) 0.051(5) 0.003(5) -0.011(5) 0.000(5) C39 0.040(3) 0.043(4) 0.037(4) 0.019(3) -0.019(3) -0.028(3) C40 0.037(4) 0.057(5) 0.056(5) 0.020(4) -0.015(3) -0.028(4) C41 0.038(4) 0.063(6) 0.084(6) 0.024(5) -0.007(4) -0.026(4) C42 0.044(5) 0.078(7) 0.115(9) -0.021(6) -0.002(5) 0.001(5) C43 0.043(5) 0.097(8) 0.115(9) 0.041(7) -0.018(5) -0.025(5) C44 0.042(4) 0.084(7) 0.079(6) 0.024(5) -0.015(4) -0.041(5) C45 0.059(5) 0.071(6) 0.074(6) 0.022(5) -0.026(4) -0.054(5) C46 0.064(5) 0.053(5) 0.051(4) 0.009(4) -0.020(4) -0.036(4) C47 0.048(4) 0.050(4) 0.037(4) 0.008(3) -0.016(3) -0.032(3) C48 0.049(4) 0.047(4) 0.042(4) -0.002(3) -0.011(3) -0.026(3) C49 0.054(5) 0.042(4) 0.065(5) -0.007(4) -0.007(4) -0.014(4) C50 0.073(6) 0.112(8) 0.056(5) -0.028(5) -0.001(4) -0.056(6) C51 0.036(3) 0.029(3) 0.035(3) 0.005(3) -0.014(3) -0.016(3) C52 0.046(4) 0.023(3) 0.048(4) 0.009(3) -0.022(3) -0.022(3) C53 0.071(5) 0.035(4) 0.052(5) 0.005(3) -0.029(4) -0.024(4) C54 0.094(7) 0.050(5) 0.063(5) 0.020(4) -0.053(5) -0.031(5) C55 0.073(6) 0.042(5) 0.095(7) 0.025(5) -0.055(5) -0.028(4) C56 0.043(4) 0.033(4) 0.083(6) 0.008(4) -0.024(4) -0.017(3) C57 0.041(4) 0.034(4) 0.061(5) 0.006(3) -0.025(3) -0.020(3) C58 0.031(3) 0.032(3) 0.041(4) -0.003(3) -0.015(3) -0.009(3) C59 0.036(3) 0.032(4) 0.047(4) -0.005(3) -0.016(3) -0.016(3) C60 0.047(4) 0.029(4) 0.054(4) -0.002(3) -0.012(3) -0.018(3) C61 0.046(4) 0.055(5) 0.061(5) -0.002(4) -0.008(4) -0.028(4) C62 0.063(5) 0.048(5) 0.059(5) 0.008(4) -0.022(4) -0.029(4) C63 0.050(4) 0.038(4) 0.061(5) -0.013(4) -0.015(4) -0.017(3) C64 0.055(5) 0.045(5) 0.060(5) -0.025(4) -0.008(4) -0.012(4) C65 0.037(4) 0.065(5) 0.048(4) -0.023(4) -0.007(3) -0.003(4) C66 0.035(4) 0.043(4) 0.047(4) -0.004(3) -0.013(3) -0.008(3) C67 0.058(5) 0.054(5) 0.040(4) 0.003(4) 0.000(3) -0.019(4) C68 0.069(6) 0.093(8) 0.061(6) 0.021(5) -0.011(5) -0.015(5) C69 0.065(5) 0.067(6) 0.050(5) 0.008(4) -0.005(4) -0.034(4) C70 0.056(4) 0.021(3) 0.039(4) 0.008(3) -0.023(3) -0.018(3) C71 0.060(4) 0.030(4) 0.042(4) 0.002(3) -0.024(3) -0.018(3) C72 0.069(5) 0.043(4) 0.037(4) -0.003(3) -0.020(3) -0.024(4) C73 0.066(5) 0.055(5) 0.050(5) -0.004(4) -0.013(4) -0.015(4) C74 0.093(7) 0.049(5) 0.049(5) 0.007(4) -0.012(4) -0.022(5) C75 0.080(6) 0.051(5) 0.050(5) -0.008(4) -0.026(4) -0.030(4) C76 0.075(6) 0.057(5) 0.098(7) -0.015(5) -0.039(5) -0.034(5) C77 0.061(5) 0.054(5) 0.079(6) -0.004(4) -0.025(4) -0.031(4) C78 0.051(4) 0.030(4) 0.060(5) 0.003(3) -0.015(3) -0.021(3) C79 0.058(5) 0.044(4) 0.067(5) 0.000(4) -0.005(4) -0.034(4) C80 0.145(10) 0.076(7) 0.082(8) -0.004(6) 0.017(7) -0.061(7) C81 0.056(5) 0.093(8) 0.128(9) -0.035(7) -0.012(5) -0.042(5) C101 0.093(7) 0.066(6) 0.056(5) -0.004(4) -0.009(5) -0.043(5) C102 0.113(9) 0.094(8) 0.067(6) -0.011(6) -0.004(6) -0.072(7) C103 0.088(8) 0.130(11) 0.058(6) -0.004(7) 0.011(5) -0.052(8) C104 0.086(7) 0.095(8) 0.061(6) 0.003(6) -0.019(5) -0.020(6) C105 0.077(6) 0.075(7) 0.055(5) 0.016(5) -0.016(5) -0.039(5) C106 0.069(5) 0.078(6) 0.047(5) -0.004(4) -0.017(4) -0.042(5) C107 0.073(6) 0.114(9) 0.062(6) 0.015(6) -0.022(5) -0.040(6) N3 0.031(3) 0.026(3) 0.029(3) 0.003(2) -0.008(2) -0.014(2) N4 0.029(3) 0.038(3) 0.037(3) 0.006(2) -0.011(2) -0.014(2) N1 0.043(3) 0.028(3) 0.033(3) 0.003(2) -0.013(2) -0.015(2) N2 0.051(3) 0.025(3) 0.035(3) 0.003(2) -0.020(2) -0.018(2) O1 0.043(3) 0.041(3) 0.060(3) -0.009(2) -0.019(2) -0.018(2) O2 0.043(3) 0.040(3) 0.048(3) 0.005(2) -0.006(2) -0.017(2) Lu2 0.04407(17) 0.02623(16) 0.02768(15) 0.00283(11) -0.01361(11) -0.01594(12) Lu1 0.03666(16) 0.02607(16) 0.03501(16) 0.00230(11) -0.01277(11) -0.01486(12) _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 O3 C5' 1.356(18) . ? O3 C8' 1.38(2) . ? O3 C5 1.59(2) . ? O3 C8 1.63(3) . ? O3 Lu2 2.360(5) . ? C5 C6 1.409(19) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.52(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.60(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C5' C6' 1.426(19) . ? C5' H5'1 0.9900 . ? C5' H5'2 0.9900 . ? C6' C7' 1.51(2) . ? C6' H6'1 0.9900 . ? C6' H6'2 0.9900 . ? C7' C8' 1.590(19) . ? C7' H7'1 0.9900 . ? C7' H7'2 0.9900 . ? C8' H8'1 0.9900 . ? C8' H8'2 0.9900 . ? C9 O1 1.465(9) . ? C9 C10 1.53(2) . ? C9 C10' 1.53(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.50(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.55(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C10' C11' 1.54(4) . ? C10' H10C 0.9900 . ? C10' H10D 0.9900 . ? C11' C12 1.55(2) . ? C11' H11C 0.9900 . ? C11' H11D 0.9900 . ? C12 O1 1.444(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O2 1.456(10) . ? C13 C14 1.501(12) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.494(12) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.472(12) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O2 1.476(10) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C20 N3 1.332(7) . ? C20 N4 1.332(8) . ? C20 C21 1.502(8) . ? C20 Lu2 2.793(6) . ? C21 C26 1.380(9) . ? C21 C22 1.389(8) . ? C22 C23 1.386(9) . ? C22 H22 0.9500 . ? C23 C24 1.371(10) . ? C23 H23 0.9500 . ? C24 C25 1.363(10) . ? C24 H24 0.9500 . ? C25 C26 1.396(9) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C35 1.412(9) . ? C27 C28 1.413(9) . ? C27 N3 1.439(8) . ? C28 C32 1.402(10) . ? C28 C29 1.496(10) . ? C29 C30 1.512(10) . ? C29 C31 1.514(11) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.380(11) . ? C32 H32 0.9500 . ? C33 C34 1.360(11) . ? C33 H33 0.9500 . ? C34 C35 1.378(10) . ? C34 H34 0.9500 . ? C35 C36 1.529(10) . ? C36 C38 1.512(12) . ? C36 C37 1.542(12) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.401(9) . ? C39 C47 1.405(10) . ? C39 N4 1.423(8) . ? C40 C44 1.403(11) . ? C40 C41 1.493(11) . ? C41 C42 1.487(13) . ? C41 C43 1.540(11) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.344(12) . ? C44 H44 0.9500 . ? C45 C46 1.370(11) . ? C45 H45 0.9500 . ? C46 C47 1.398(9) . ? C46 H46 0.9500 . ? C47 C48 1.512(9) . ? C48 C49 1.535(10) . ? C48 C50 1.547(10) . ? C48 H48 1.0000 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 N1 1.323(8) . ? C51 N2 1.348(8) . ? C51 C52 1.505(8) . ? C51 Lu1 2.796(6) . ? C52 C57 1.377(9) . ? C52 C53 1.386(10) . ? C53 C54 1.406(10) . ? C53 H53 0.9500 . ? C54 C55 1.378(12) . ? C54 H54 0.9500 . ? C55 C56 1.354(12) . ? C55 H55 0.9500 . ? C56 C57 1.393(9) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 C59 1.411(9) . ? C58 C66 1.412(9) . ? C58 N1 1.443(8) . ? C59 C63 1.387(9) . ? C59 C60 1.500(9) . ? C60 C62 1.535(10) . ? C60 C61 1.536(9) . ? C60 H60 1.0000 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.371(10) . ? C63 H63 0.9500 . ? C64 C65 1.376(11) . ? C64 H64 0.9500 . ? C65 C66 1.390(10) . ? C65 H65 0.9500 . ? C66 C67 1.520(10) . ? C67 C68 1.512(11) . ? C67 C69 1.535(11) . ? C67 H67 1.0000 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C71 1.402(9) . ? C70 C78 1.415(10) . ? C70 N2 1.437(8) . ? C71 C75 1.402(10) . ? C71 C72 1.515(10) . ? C72 C73 1.527(10) . ? C72 C74 1.543(10) . ? C72 H72 1.0000 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C76 1.360(12) . ? C75 H75 0.9500 . ? C76 C77 1.380(12) . ? C76 H76 0.9500 . ? C77 C78 1.394(10) . ? C77 H77 0.9500 . ? C78 C79 1.519(11) . ? C79 C81 1.527(12) . ? C79 C80 1.534(12) . ? C79 H79 1.0000 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C101 C106 1.365(12) . ? C101 C102 1.386(13) . ? C101 H101 0.9500 . ? C102 C103 1.372(15) . ? C102 H102 0.9500 . ? C103 C104 1.373(14) . ? C103 H103 0.9500 . ? C104 C105 1.376(13) . ? C104 H104 0.9500 . ? C105 C106 1.382(12) . ? C105 H105 0.9500 . ? C106 C107 1.506(12) . ? C107 H10E 0.9800 . ? C107 H10F 0.9800 . ? C107 H10G 0.9800 . ? N3 Lu2 2.349(5) . ? N4 Lu2 2.369(5) . ? N1 Lu1 2.373(5) . ? N2 Lu1 2.345(5) . ? O1 Lu1 2.368(4) . ? O2 Lu1 2.322(4) . ? Lu2 Lu1 3.2359(5) . ? Lu2 H2 2.15(6) . ? Lu2 H3 2.09(6) . ? Lu2 H4 2.2900(3) . ? Lu2 H1 2.0405(3) . ? Lu1 H2 2.06(6) . ? Lu1 H3 2.06(6) . ? Lu1 H1 2.1766(3) . ? 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 C5' O3 C8' 102.9(11) . . ? C5' O3 C5 52.0(12) . . ? C8' O3 C5 107.5(12) . . ? C5' O3 C8 101.8(11) . . ? C8' O3 C8 21.0(18) . . ? C5 O3 C8 90.1(12) . . ? C5' O3 Lu2 134.4(8) . . ? C8' O3 Lu2 122.5(8) . . ? C5 O3 Lu2 111.9(9) . . ? C8 O3 Lu2 122.2(8) . . ? C6 C5 O3 101.9(18) . . ? C6 C5 H5A 111.4 . . ? O3 C5 H5A 111.4 . . ? C6 C5 H5B 111.4 . . ? O3 C5 H5B 111.4 . . ? H5A C5 H5B 109.2 . . ? C5 C6 C7 107.0(16) . . ? C5 C6 H6A 110.3 . . ? C7 C6 H6A 110.3 . . ? C5 C6 H6B 110.3 . . ? C7 C6 H6B 110.3 . . ? H6A C6 H6B 108.6 . . ? C6 C7 C8 95.1(18) . . ? C6 C7 H7A 112.7 . . ? C8 C7 H7A 112.7 . . ? C6 C7 H7B 112.7 . . ? C8 C7 H7B 112.7 . . ? H7A C7 H7B 110.2 . . ? C7 C8 O3 86.1(17) . . ? C7 C8 H8A 114.3 . . ? O3 C8 H8A 114.3 . . ? C7 C8 H8B 114.3 . . ? O3 C8 H8B 114.3 . . ? H8A C8 H8B 111.4 . . ? O3 C5' C6' 113.3(15) . . ? O3 C5' H5'1 108.9 . . ? C6' C5' H5'1 108.9 . . ? O3 C5' H5'2 108.9 . . ? C6' C5' H5'2 108.9 . . ? H5'1 C5' H5'2 107.7 . . ? C5' C6' C7' 106.2(13) . . ? C5' C6' H6'1 110.5 . . ? C7' C6' H6'1 110.5 . . ? C5' C6' H6'2 110.5 . . ? C7' C6' H6'2 110.5 . . ? H6'1 C6' H6'2 108.7 . . ? C6' C7' C8' 98.0(14) . . ? C6' C7' H7'1 112.2 . . ? C8' C7' H7'1 112.2 . . ? C6' C7' H7'2 112.2 . . ? C8' C7' H7'2 112.2 . . ? H7'1 C7' H7'2 109.8 . . ? O3 C8' C7' 110.4(13) . . ? O3 C8' H8'1 109.6 . . ? C7' C8' H8'1 109.6 . . ? O3 C8' H8'2 109.6 . . ? C7' C8' H8'2 109.6 . . ? H8'1 C8' H8'2 108.1 . . ? O1 C9 C10 104.0(10) . . ? O1 C9 C10' 103.6(10) . . ? C10 C9 C10' 31.0(9) . . ? O1 C9 H9A 111.0 . . ? C10 C9 H9A 135.0 . . ? C10' C9 H9A 111.0 . . ? O1 C9 H9B 111.0 . . ? C10 C9 H9B 82.6 . . ? C10' C9 H9B 111.0 . . ? H9A C9 H9B 109.0 . . ? C11 C10 C9 100.1(16) . . ? C11 C10 H10A 111.8 . . ? C9 C10 H10A 111.8 . . ? C11 C10 H10B 111.8 . . ? C9 C10 H10B 111.8 . . ? H10A C10 H10B 109.5 . . ? C10 C11 C12 98.9(17) . . ? C10 C11 H11A 112.0 . . ? C12 C11 H11A 112.0 . . ? C10 C11 H11B 112.0 . . ? C12 C11 H11B 112.0 . . ? H11A C11 H11B 109.7 . . ? C9 C10' C11' 101.0(17) . . ? C9 C10' H10C 111.6 . . ? C11' C10' H10C 111.6 . . ? C9 C10' H10D 111.6 . . ? C11' C10' H10D 111.6 . . ? H10C C10' H10D 109.4 . . ? C10' C11' C12 99.3(17) . . ? C10' C11' H11C 111.9 . . ? C12 C11' H11C 111.9 . . ? C10' C11' H11D 111.9 . . ? C12 C11' H11D 111.9 . . ? H11C C11' H11D 109.6 . . ? O1 C12 C11 102.9(11) . . ? O1 C12 C11' 107.0(11) . . ? C11 C12 C11' 26.3(9) . . ? O1 C12 H12A 110.3 . . ? C11 C12 H12A 133.5 . . ? C11' C12 H12A 110.3 . . ? O1 C12 H12B 110.3 . . ? C11 C12 H12B 88.4 . . ? C11' C12 H12B 110.3 . . ? H12A C12 H12B 108.6 . . ? O2 C13 C14 107.3(7) . . ? O2 C13 H13A 110.3 . . ? C14 C13 H13A 110.3 . . ? O2 C13 H13B 110.3 . . ? C14 C13 H13B 110.3 . . ? H13A C13 H13B 108.5 . . ? C15 C14 C13 103.7(8) . . ? C15 C14 H14A 111.0 . . ? C13 C14 H14A 111.0 . . ? C15 C14 H14B 111.0 . . ? C13 C14 H14B 111.0 . . ? H14A C14 H14B 109.0 . . ? C16 C15 C14 106.3(8) . . ? C16 C15 H15A 110.5 . . ? C14 C15 H15A 110.5 . . ? C16 C15 H15B 110.5 . . ? C14 C15 H15B 110.5 . . ? H15A C15 H15B 108.7 . . ? C15 C16 O2 105.9(7) . . ? C15 C16 H16A 110.5 . . ? O2 C16 H16A 110.5 . . ? C15 C16 H16B 110.5 . . ? O2 C16 H16B 110.5 . . ? H16A C16 H16B 108.7 . . ? N3 C20 N4 114.0(5) . . ? N3 C20 C21 122.6(5) . . ? N4 C20 C21 123.4(5) . . ? N3 C20 Lu2 57.0(3) . . ? N4 C20 Lu2 57.8(3) . . ? C21 C20 Lu2 169.6(4) . . ? C26 C21 C22 118.7(6) . . ? C26 C21 C20 119.4(5) . . ? C22 C21 C20 121.9(5) . . ? C23 C22 C21 119.9(6) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C22 120.9(6) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C25 C24 C23 119.9(6) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 119.9(7) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C21 C26 C25 120.7(6) . . ? C21 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C35 C27 C28 120.7(6) . . ? C35 C27 N3 118.1(6) . . ? C28 C27 N3 121.0(6) . . ? C32 C28 C27 117.6(7) . . ? C32 C28 C29 119.2(6) . . ? C27 C28 C29 123.1(6) . . ? C28 C29 C30 113.5(7) . . ? C28 C29 C31 112.3(7) . . ? C30 C29 C31 111.9(7) . . ? C28 C29 H29 106.2 . . ? C30 C29 H29 106.2 . . ? C31 C29 H29 106.2 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C28 121.3(7) . . ? C33 C32 H32 119.4 . . ? C28 C32 H32 119.4 . . ? C34 C33 C32 119.9(7) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 122.3(7) . . ? C33 C34 H34 118.9 . . ? C35 C34 H34 118.9 . . ? C34 C35 C27 118.2(7) . . ? C34 C35 C36 119.7(6) . . ? C27 C35 C36 122.0(6) . . ? C38 C36 C35 110.7(7) . . ? C38 C36 C37 107.2(7) . . ? C35 C36 C37 111.8(7) . . ? C38 C36 H36 109.0 . . ? C35 C36 H36 109.0 . . ? C37 C36 H36 109.0 . . ? 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 . . ? C40 C39 C47 120.7(6) . . ? C40 C39 N4 117.0(6) . . ? C47 C39 N4 122.1(6) . . ? C39 C40 C44 116.8(7) . . ? C39 C40 C41 122.1(6) . . ? C44 C40 C41 121.0(7) . . ? C42 C41 C40 111.5(7) . . ? C42 C41 C43 108.8(8) . . ? C40 C41 C43 114.1(8) . . ? C42 C41 H41 107.4 . . ? C40 C41 H41 107.4 . . ? C43 C41 H41 107.4 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C40 123.5(7) . . ? C45 C44 H44 118.3 . . ? C40 C44 H44 118.3 . . ? C44 C45 C46 119.1(7) . . ? C44 C45 H45 120.4 . . ? C46 C45 H45 120.4 . . ? C45 C46 C47 121.3(8) . . ? C45 C46 H46 119.3 . . ? C47 C46 H46 119.3 . . ? C46 C47 C39 118.4(6) . . ? C46 C47 C48 118.4(7) . . ? C39 C47 C48 123.2(6) . . ? C47 C48 C49 111.2(6) . . ? C47 C48 C50 110.5(6) . . ? C49 C48 C50 110.3(7) . . ? C47 C48 H48 108.2 . . ? C49 C48 H48 108.2 . . ? C50 C48 H48 108.2 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N1 C51 N2 113.2(5) . . ? N1 C51 C52 124.2(6) . . ? N2 C51 C52 122.4(5) . . ? N1 C51 Lu1 57.8(3) . . ? N2 C51 Lu1 56.7(3) . . ? C52 C51 Lu1 165.7(4) . . ? C57 C52 C53 118.1(6) . . ? C57 C52 C51 123.7(6) . . ? C53 C52 C51 118.1(6) . . ? C52 C53 C54 120.6(8) . . ? C52 C53 H53 119.7 . . ? C54 C53 H53 119.7 . . ? C55 C54 C53 120.2(8) . . ? C55 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? C56 C55 C54 118.7(7) . . ? C56 C55 H55 120.7 . . ? C54 C55 H55 120.7 . . ? C55 C56 C57 121.9(8) . . ? C55 C56 H56 119.1 . . ? C57 C56 H56 119.1 . . ? C52 C57 C56 120.4(7) . . ? C52 C57 H57 119.8 . . ? C56 C57 H57 119.8 . . ? C59 C58 C66 120.4(6) . . ? C59 C58 N1 121.4(6) . . ? C66 C58 N1 118.2(6) . . ? C63 C59 C58 117.9(6) . . ? C63 C59 C60 119.0(6) . . ? C58 C59 C60 123.1(6) . . ? C59 C60 C62 112.8(6) . . ? C59 C60 C61 109.2(6) . . ? C62 C60 C61 110.8(6) . . ? C59 C60 H60 107.9 . . ? C62 C60 H60 107.9 . . ? C61 C60 H60 107.9 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 C59 122.2(7) . . ? C64 C63 H63 118.9 . . ? C59 C63 H63 118.9 . . ? C63 C64 C65 119.6(7) . . ? C63 C64 H64 120.2 . . ? C65 C64 H64 120.2 . . ? C64 C65 C66 121.3(7) . . ? C64 C65 H65 119.4 . . ? C66 C65 H65 119.4 . . ? C65 C66 C58 118.4(7) . . ? C65 C66 C67 119.2(7) . . ? C58 C66 C67 122.3(6) . . ? C68 C67 C66 111.8(8) . . ? C68 C67 C69 108.9(7) . . ? C66 C67 C69 110.8(6) . . ? C68 C67 H67 108.4 . . ? C66 C67 H67 108.4 . . ? C69 C67 H67 108.4 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C71 C70 C78 119.5(6) . . ? C71 C70 N2 119.2(6) . . ? C78 C70 N2 121.0(6) . . ? C75 C71 C70 118.9(7) . . ? C75 C71 C72 117.6(7) . . ? C70 C71 C72 123.4(6) . . ? C71 C72 C73 112.9(6) . . ? C71 C72 C74 111.0(6) . . ? C73 C72 C74 109.5(6) . . ? C71 C72 H72 107.8 . . ? C73 C72 H72 107.8 . . ? C74 C72 H72 107.8 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C74 H74A 109.5 . . ? C72 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C72 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C76 C75 C71 122.0(8) . . ? C76 C75 H75 119.0 . . ? C71 C75 H75 119.0 . . ? C75 C76 C77 119.0(7) . . ? C75 C76 H76 120.5 . . ? C77 C76 H76 120.5 . . ? C76 C77 C78 122.0(8) . . ? C76 C77 H77 119.0 . . ? C78 C77 H77 119.0 . . ? C77 C78 C70 118.5(7) . . ? C77 C78 C79 117.4(7) . . ? C70 C78 C79 124.1(6) . . ? C78 C79 C81 111.0(7) . . ? C78 C79 C80 111.5(7) . . ? C81 C79 C80 110.3(8) . . ? C78 C79 H79 108.0 . . ? C81 C79 H79 108.0 . . ? C80 C79 H79 108.0 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C106 C101 C102 119.6(10) . . ? C106 C101 H101 120.2 . . ? C102 C101 H101 120.2 . . ? C103 C102 C101 121.3(10) . . ? C103 C102 H102 119.4 . . ? C101 C102 H102 119.4 . . ? C102 C103 C104 118.6(10) . . ? C102 C103 H103 120.7 . . ? C104 C103 H103 120.7 . . ? C103 C104 C105 120.6(10) . . ? C103 C104 H104 119.7 . . ? C105 C104 H104 119.7 . . ? C104 C105 C106 120.3(9) . . ? C104 C105 H105 119.9 . . ? C106 C105 H105 119.9 . . ? C101 C106 C105 119.5(9) . . ? C101 C106 C107 118.7(9) . . ? C105 C106 C107 121.7(8) . . ? C106 C107 H10E 109.5 . . ? C106 C107 H10F 109.5 . . ? H10E C107 H10F 109.5 . . ? C106 C107 H10G 109.5 . . ? H10E C107 H10G 109.5 . . ? H10F C107 H10G 109.5 . . ? C20 N3 C27 122.6(5) . . ? C20 N3 Lu2 94.7(4) . . ? C27 N3 Lu2 142.3(4) . . ? C20 N4 C39 124.3(5) . . ? C20 N4 Lu2 93.8(4) . . ? C39 N4 Lu2 139.6(4) . . ? C51 N1 C58 121.6(5) . . ? C51 N1 Lu1 94.0(4) . . ? C58 N1 Lu1 142.6(4) . . ? C51 N2 C70 121.9(5) . . ? C51 N2 Lu1 94.6(4) . . ? C70 N2 Lu1 142.6(4) . . ? C12 O1 C9 108.6(5) . . ? C12 O1 Lu1 115.8(4) . . ? C9 O1 Lu1 122.7(4) . . ? C13 O2 C16 108.4(6) . . ? C13 O2 Lu1 127.1(4) . . ? C16 O2 Lu1 124.5(4) . . ? N3 Lu2 O3 136.04(17) . . ? N3 Lu2 N4 56.53(17) . . ? O3 Lu2 N4 79.85(18) . . ? N3 Lu2 C20 28.38(17) . . ? O3 Lu2 C20 107.67(18) . . ? N4 Lu2 C20 28.43(17) . . ? N3 Lu2 Lu1 114.11(12) . . ? O3 Lu2 Lu1 102.19(14) . . ? N4 Lu2 Lu1 139.59(13) . . ? C20 Lu2 Lu1 134.13(12) . . ? N3 Lu2 H2 150.0(16) . . ? O3 Lu2 H2 73.2(16) . . ? N4 Lu2 H2 149.3(16) . . ? C20 Lu2 H2 171.3(16) . . ? Lu1 Lu2 H2 38.9(16) . . ? N3 Lu2 H3 85.2(16) . . ? O3 Lu2 H3 137.7(16) . . ? N4 Lu2 H3 137.6(16) . . ? C20 Lu2 H3 112.8(16) . . ? Lu1 Lu2 H3 38.5(15) . . ? H2 Lu2 H3 65(2) . . ? N3 Lu2 H4 98.19(12) . . ? O3 Lu2 H4 85.68(18) . . ? N4 Lu2 H4 103.15(13) . . ? C20 Lu2 H4 99.19(12) . . ? Lu1 Lu2 H4 117.265(12) . . ? H2 Lu2 H4 89.5(15) . . ? H3 Lu2 H4 99.3(16) . . ? N3 Lu2 H1 106.50(12) . . ? O3 Lu2 H1 84.40(17) . . ? N4 Lu2 H1 99.93(12) . . ? C20 Lu2 H1 107.94(12) . . ? Lu1 Lu2 H1 41.457(8) . . ? H2 Lu2 H1 63.4(15) . . ? H3 Lu2 H1 72.1(15) . . ? H4 Lu2 H1 152.803(13) . . ? O2 Lu1 N2 96.39(17) . . ? O2 Lu1 O1 79.13(17) . . ? N2 Lu1 O1 131.22(17) . . ? O2 Lu1 N1 111.33(17) . . ? N2 Lu1 N1 56.42(18) . . ? O1 Lu1 N1 79.82(17) . . ? O2 Lu1 C51 102.08(17) . . ? N2 Lu1 C51 28.71(17) . . ? O1 Lu1 C51 104.11(17) . . ? N1 Lu1 C51 28.17(17) . . ? O2 Lu1 Lu2 104.85(11) . . ? N2 Lu1 Lu2 116.43(12) . . ? O1 Lu1 Lu2 111.55(12) . . ? N1 Lu1 Lu2 143.60(12) . . ? C51 Lu1 Lu2 138.47(12) . . ? O2 Lu1 H2 84.8(16) . . ? N2 Lu1 H2 84.3(16) . . ? O1 Lu1 H2 142.1(16) . . ? N1 Lu1 H2 138.1(16) . . ? C51 Lu1 H2 112.7(16) . . ? Lu2 Lu1 H2 40.9(16) . . ? O2 Lu1 H3 81.4(16) . . ? N2 Lu1 H3 151.1(17) . . ? O1 Lu1 H3 76.9(17) . . ? N1 Lu1 H3 150.7(16) . . ? C51 Lu1 H3 176.5(16) . . ? Lu2 Lu1 H3 39.0(16) . . ? H2 Lu1 H3 67(2) . . ? O2 Lu1 H1 142.70(12) . . ? N2 Lu1 H1 97.69(12) . . ? O1 Lu1 H1 115.14(12) . . ? N1 Lu1 H1 105.24(12) . . ? C51 Lu1 H1 106.78(12) . . ? Lu2 Lu1 H1 38.363(8) . . ? H2 Lu1 H1 62.6(17) . . ? H3 Lu1 H1 69.8(16) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 3.566 _refine_diff_density_min -1.041 _refine_diff_density_rms 0.136 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.000 0.000 0.000 260 46 ' ' 2 -0.005 0.224 0.118 7 0 ' ' 3 0.005 0.776 0.882 8 1 ' ' 4 0.079 0.343 0.096 23 2 ' ' 5 0.244 0.631 0.383 8 0 ' ' 6 0.386 0.614 0.406 11 0 ' ' 7 0.430 0.292 0.267 7 0 ' ' 8 0.476 0.407 0.667 14 1 ' ' 9 0.530 0.593 0.330 13 1 ' ' 10 0.569 0.708 0.733 7 0 ' ' 11 0.634 0.382 0.590 10 0 ' ' 12 0.766 0.369 0.619 8 0 ' ' 13 0.920 0.657 0.904 22 2 ' ' _platon_squeeze_details ; 1/2 disorder Et2O molecule per formual unit of [(Ph-NCN)LuH2]2(THF)3 was not modelled and the disordered density was taken into account using the SQUEEZE/PLATON procedure.(Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194?01) as implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst. 2003, 36, 7?3. PLATON - a multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands). ; _vrf_PLAT305_II-044 ; PROBLEM: Isolated Hydrogen Atom (Outside Bond Range ??) H4 RESPONSE: All the hydrides (H1~H4) were located by difference Fourier syntheses. The coordinates and isotropic parameters were refined for H2 and H3. Only the displace parameter was refined for H1 while the coordinates were constrained. The coordinates and isotropic parameters were constrained for H4. ; data_2-Y _database_code_depnum_ccdc_archive 'CCDC 859485' #TrackingRef '- Ln2H4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((PhNCN)2Y2H3(OC4H9))(THF)3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H123 N4 O4.50 Si Y2' _chemical_formula_weight 1430.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.0663(19) _cell_length_b 38.724(6) _cell_length_c 15.781(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.796(3) _cell_angle_gamma 90.00 _cell_volume 7967(2) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Fragment _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3060 _exptl_absorpt_coefficient_mu 1.513 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6766 _exptl_absorpt_correction_T_max 0.8048 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 43453 _diffrn_reflns_av_R_equivalents 0.1123 _diffrn_reflns_av_sigmaI/netI 0.1414 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 25.07 _reflns_number_total 14111 _reflns_number_gt 7447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0510P)^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 14111 _refine_ls_number_parameters 842 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1443 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1430 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C4 C 0.2661(4) 0.13399(14) 0.2218(3) 0.0442(15) Uani 1 1 d . . . H4A H 0.2934 0.1115 0.2431 0.053 Uiso 1 1 calc R . . H4B H 0.1985 0.1381 0.2448 0.053 Uiso 1 1 calc R . . C5 C 0.3386(4) 0.16249(15) 0.2452(3) 0.0527(16) Uani 1 1 d . . . H5A H 0.3731 0.1587 0.3022 0.063 Uiso 1 1 calc R . . H5B H 0.3027 0.1850 0.2447 0.063 Uiso 1 1 calc R . . C6 C 0.4153(4) 0.16100(14) 0.1763(3) 0.0520(16) Uani 1 1 d . . . H6A H 0.4308 0.1845 0.1559 0.062 Uiso 1 1 calc R . . H6B H 0.4800 0.1499 0.1982 0.062 Uiso 1 1 calc R . . C7 C 0.3626(4) 0.13967(15) 0.1059(3) 0.0531(16) Uani 1 1 d . . . H7A H 0.3633 0.1520 0.0509 0.064 Uiso 1 1 calc R . . H7B H 0.3976 0.1171 0.1007 0.064 Uiso 1 1 calc R . . C8 C 0.1591(6) 0.22940(17) 0.0742(5) 0.097(3) Uani 1 1 d . . . H8A H 0.1045 0.2446 0.0486 0.117 Uiso 1 1 calc R . . H8B H 0.1395 0.2219 0.1309 0.117 Uiso 1 1 calc R . . C9 C 0.2563(7) 0.24739(19) 0.0813(6) 0.114(3) Uani 1 1 d . . . H9A H 0.2968 0.2404 0.1337 0.137 Uiso 1 1 calc R . . H9B H 0.2454 0.2727 0.0826 0.137 Uiso 1 1 calc R . . C10 C 0.3109(6) 0.2372(2) 0.0035(6) 0.106(3) Uani 1 1 d . . . H10A H 0.3219 0.2575 -0.0328 0.127 Uiso 1 1 calc R . . H10B H 0.3782 0.2265 0.0199 0.127 Uiso 1 1 calc R . . C11 C 0.2406(5) 0.21184(16) -0.0413(4) 0.075(2) Uani 1 1 d . . . H11A H 0.2005 0.2231 -0.0890 0.090 Uiso 1 1 calc R . . H11B H 0.2801 0.1925 -0.0641 0.090 Uiso 1 1 calc R . . C12 C -0.3364(4) 0.16375(15) 0.1056(4) 0.0561(17) Uani 1 1 d . . . H12A H -0.3267 0.1714 0.1655 0.067 Uiso 1 1 calc R . . H12B H -0.3875 0.1448 0.1021 0.067 Uiso 1 1 calc R . . C13 C -0.3719(5) 0.19296(17) 0.0504(4) 0.072(2) Uani 1 1 d . . . H13A H -0.3638 0.2151 0.0813 0.086 Uiso 1 1 calc R . . H13B H -0.4449 0.1900 0.0308 0.086 Uiso 1 1 calc R . . C14 C -0.3034(5) 0.19199(16) -0.0251(4) 0.069(2) Uani 1 1 d . . . H14A H -0.3449 0.1936 -0.0798 0.083 Uiso 1 1 calc R . . H14B H -0.2526 0.2110 -0.0216 0.083 Uiso 1 1 calc R . . C15 C -0.2513(5) 0.15724(15) -0.0156(3) 0.0531(16) Uani 1 1 d . . . H15A H -0.2941 0.1389 -0.0436 0.064 Uiso 1 1 calc R . . H15B H -0.1836 0.1575 -0.0403 0.064 Uiso 1 1 calc R . . C16 C -0.1569(5) 0.23511(17) 0.2403(5) 0.083(2) Uani 1 1 d . . . H16A H -0.1301 0.2376 0.3002 0.099 Uiso 1 1 calc R A 1 H16B H -0.2323 0.2380 0.2380 0.099 Uiso 1 1 calc R A 1 C17 C -0.186(3) 0.2615(5) 0.1733(14) 0.108(3) Uani 0.432(19) 1 d P B 2 H17A H -0.2077 0.2835 0.1983 0.130 Uiso 0.432(19) 1 calc PR B 2 H17B H -0.2411 0.2529 0.1325 0.130 Uiso 0.432(19) 1 calc PR B 2 C18 C -0.081(3) 0.2651(5) 0.1311(17) 0.108(3) Uani 0.432(19) 1 d P B 2 H18A H -0.0605 0.2420 0.1113 0.130 Uiso 0.432(19) 1 calc PR B 2 H18B H -0.0282 0.2726 0.1753 0.130 Uiso 0.432(19) 1 calc PR B 2 C17' C -0.113(2) 0.2605(4) 0.1903(11) 0.108(3) Uani 0.568(19) 1 d P B 1 H17C H -0.0382 0.2579 0.1997 0.130 Uiso 0.568(19) 1 calc PR B 1 H17D H -0.1309 0.2830 0.2154 0.130 Uiso 0.568(19) 1 calc PR B 1 C18' C -0.1353(19) 0.2641(4) 0.0961(12) 0.108(3) Uani 0.568(19) 1 d P B 1 H18C H -0.1197 0.2417 0.0694 0.130 Uiso 0.568(19) 1 calc PR B 1 H18D H -0.2098 0.2683 0.0851 0.130 Uiso 0.568(19) 1 calc PR B 1 C19 C -0.0797(6) 0.29150(17) 0.0526(5) 0.108(3) Uani 1 1 d . . . H19A H -0.0411 0.2812 0.0078 0.162 Uiso 1 1 calc R B 1 H19B H -0.0322 0.3032 0.0938 0.162 Uiso 1 1 calc R B 1 H19C H -0.1290 0.3083 0.0273 0.162 Uiso 1 1 calc R B 1 C20 C 0.1303(4) 0.11665(12) -0.1246(3) 0.0356(13) Uani 1 1 d . . . C21 C 0.1347(4) 0.10053(14) -0.2099(3) 0.0394(14) Uani 1 1 d . . . C22 C 0.1548(4) 0.06562(14) -0.2203(3) 0.0444(15) Uani 1 1 d . . . H22 H 0.1692 0.0514 -0.1719 0.053 Uiso 1 1 calc R . . C23 C 0.1541(4) 0.05133(17) -0.3008(4) 0.0608(18) Uani 1 1 d . . . H23 H 0.1644 0.0272 -0.3071 0.073 Uiso 1 1 calc R . . C24 C 0.1385(5) 0.07171(19) -0.3714(4) 0.0656(19) Uani 1 1 d . . . H24 H 0.1404 0.0618 -0.4263 0.079 Uiso 1 1 calc R . . C25 C 0.1202(4) 0.10628(18) -0.3630(4) 0.0597(18) Uani 1 1 d . . . H25 H 0.1099 0.1205 -0.4120 0.072 Uiso 1 1 calc R . . C26 C 0.1168(4) 0.12043(16) -0.2824(3) 0.0516(16) Uani 1 1 d . . . H26 H 0.1018 0.1443 -0.2767 0.062 Uiso 1 1 calc R . . C27 C -0.0412(4) 0.13924(13) -0.1578(3) 0.0354(13) Uani 1 1 d . . . C28 C -0.0721(4) 0.17147(13) -0.1940(3) 0.0379(13) Uani 1 1 d . . . C29 C -0.0026(4) 0.20307(13) -0.1817(3) 0.0452(15) Uani 1 1 d . . . H29 H 0.0649 0.1950 -0.1552 0.054 Uiso 1 1 calc R . . C30 C -0.0470(5) 0.22876(14) -0.1214(4) 0.0654(19) Uani 1 1 d . . . H30A H -0.0008 0.2486 -0.1139 0.098 Uiso 1 1 calc R . . H30B H -0.0545 0.2177 -0.0664 0.098 Uiso 1 1 calc R . . H30C H -0.1142 0.2366 -0.1451 0.098 Uiso 1 1 calc R . . C31 C 0.0174(5) 0.22078(15) -0.2653(4) 0.075(2) Uani 1 1 d . . . H31A H 0.0631 0.2405 -0.2542 0.112 Uiso 1 1 calc R . . H31B H -0.0478 0.2288 -0.2929 0.112 Uiso 1 1 calc R . . H31C H 0.0496 0.2044 -0.3027 0.112 Uiso 1 1 calc R . . C32 C -0.1651(4) 0.17482(15) -0.2387(3) 0.0482(15) Uani 1 1 d . . . H32 H -0.1850 0.1966 -0.2622 0.058 Uiso 1 1 calc R . . C33 C -0.2307(5) 0.14685(16) -0.2500(4) 0.0572(17) Uani 1 1 d . . . H33 H -0.2948 0.1494 -0.2814 0.069 Uiso 1 1 calc R . . C34 C -0.2026(4) 0.11553(15) -0.2159(3) 0.0464(15) Uani 1 1 d . . . H34 H -0.2479 0.0964 -0.2236 0.056 Uiso 1 1 calc R . . C35 C -0.1087(4) 0.11114(13) -0.1701(3) 0.0367(13) Uani 1 1 d . . . C36 C -0.0849(4) 0.07620(13) -0.1297(3) 0.0439(15) Uani 1 1 d . . . H36 H -0.0113 0.0764 -0.1078 0.053 Uiso 1 1 calc R . . C37 C -0.1501(5) 0.07018(14) -0.0536(4) 0.0621(18) Uani 1 1 d . . . H37A H -0.1330 0.0477 -0.0281 0.093 Uiso 1 1 calc R . . H37B H -0.2230 0.0706 -0.0728 0.093 Uiso 1 1 calc R . . H37C H -0.1360 0.0884 -0.0113 0.093 Uiso 1 1 calc R . . C38 C -0.0990(5) 0.04618(13) -0.1928(4) 0.0616(18) Uani 1 1 d . . . H38A H -0.0816 0.0244 -0.1637 0.092 Uiso 1 1 calc R . . H38B H -0.0538 0.0495 -0.2393 0.092 Uiso 1 1 calc R . . H38C H -0.1705 0.0454 -0.2158 0.092 Uiso 1 1 calc R . . C39 C 0.2933(4) 0.09315(14) -0.0748(3) 0.0391(14) Uani 1 1 d . . . C40 C 0.3129(4) 0.06267(14) -0.0271(3) 0.0408(14) Uani 1 1 d . . . C41 C 0.2428(4) 0.05168(13) 0.0415(3) 0.0384(14) Uani 1 1 d . . . H41 H 0.2199 0.0731 0.0702 0.046 Uiso 1 1 calc R . . C42 C 0.1462(4) 0.03279(14) 0.0051(4) 0.0592(17) Uani 1 1 d . . . H42A H 0.1034 0.0266 0.0515 0.089 Uiso 1 1 calc R . . H42B H 0.1662 0.0118 -0.0243 0.089 Uiso 1 1 calc R . . H42C H 0.1074 0.0479 -0.0350 0.089 Uiso 1 1 calc R . . C43 C 0.2966(4) 0.02870(15) 0.1094(4) 0.0632(18) Uani 1 1 d . . . H43A H 0.2483 0.0226 0.1519 0.095 Uiso 1 1 calc R . . H43B H 0.3551 0.0412 0.1370 0.095 Uiso 1 1 calc R . . H43C H 0.3211 0.0076 0.0830 0.095 Uiso 1 1 calc R . . C44 C 0.3967(4) 0.04238(15) -0.0429(3) 0.0524(16) Uani 1 1 d . . . H44 H 0.4083 0.0215 -0.0121 0.063 Uiso 1 1 calc R . . C45 C 0.4637(5) 0.05192(18) -0.1025(4) 0.0639(19) Uani 1 1 d . . . H45 H 0.5197 0.0374 -0.1139 0.077 Uiso 1 1 calc R . . C46 C 0.4494(4) 0.08235(17) -0.1452(4) 0.0586(18) Uani 1 1 d . . . H46 H 0.4982 0.0893 -0.1839 0.070 Uiso 1 1 calc R . . C47 C 0.3653(4) 0.10362(14) -0.1336(3) 0.0459(15) Uani 1 1 d . . . C48 C 0.3585(5) 0.13739(15) -0.1793(4) 0.0552(17) Uani 1 1 d . . . H48 H 0.2896 0.1477 -0.1717 0.066 Uiso 1 1 calc R . . C49 C 0.4415(5) 0.16273(17) -0.1422(4) 0.075(2) Uani 1 1 d . . . H49A H 0.4360 0.1847 -0.1732 0.112 Uiso 1 1 calc R . . H49B H 0.5097 0.1528 -0.1478 0.112 Uiso 1 1 calc R . . H49C H 0.4314 0.1668 -0.0820 0.112 Uiso 1 1 calc R . . C50 C 0.3716(5) 0.13351(15) -0.2754(4) 0.0676(19) Uani 1 1 d . . . H50A H 0.3661 0.1562 -0.3026 0.101 Uiso 1 1 calc R . . H50B H 0.3179 0.1183 -0.3005 0.101 Uiso 1 1 calc R . . H50C H 0.4391 0.1236 -0.2840 0.101 Uiso 1 1 calc R . . C51 C -0.1222(4) 0.11788(12) 0.3285(3) 0.0324(13) Uani 1 1 d . B . C52 C -0.1392(4) 0.10031(14) 0.4115(3) 0.0356(13) Uani 1 1 d . . . C53 C -0.1047(4) 0.11557(15) 0.4873(4) 0.0486(16) Uani 1 1 d . . . H53 H -0.0698 0.1371 0.4867 0.058 Uiso 1 1 calc R . . C54 C -0.1207(5) 0.09950(18) 0.5651(4) 0.0644(19) Uani 1 1 d . . . H54 H -0.0972 0.1103 0.6168 0.077 Uiso 1 1 calc R . . C55 C -0.1698(5) 0.06851(19) 0.5669(4) 0.070(2) Uani 1 1 d . . . H55 H -0.1812 0.0578 0.6196 0.084 Uiso 1 1 calc R . . C56 C -0.2029(4) 0.05280(16) 0.4916(4) 0.0597(18) Uani 1 1 d . . . H56 H -0.2359 0.0310 0.4925 0.072 Uiso 1 1 calc R . . C57 C -0.1884(4) 0.06860(14) 0.4147(3) 0.0427(14) Uani 1 1 d . . . H57 H -0.2125 0.0576 0.3634 0.051 Uiso 1 1 calc R . . C58 C 0.0586(4) 0.12767(13) 0.3628(3) 0.0325(13) Uani 1 1 d . . . C59 C 0.1068(4) 0.09503(14) 0.3719(3) 0.0386(14) Uani 1 1 d . . . C60 C 0.0580(4) 0.06242(12) 0.3332(3) 0.0380(14) Uani 1 1 d . . . H60 H -0.0143 0.0680 0.3131 0.046 Uiso 1 1 calc R . . C61 C 0.0552(5) 0.03275(13) 0.3976(4) 0.0605(18) Uani 1 1 d . . . H61A H 0.0226 0.0125 0.3701 0.091 Uiso 1 1 calc R . . H61B H 0.0159 0.0399 0.4454 0.091 Uiso 1 1 calc R . . H61C H 0.1254 0.0269 0.4185 0.091 Uiso 1 1 calc R . . C62 C 0.1153(5) 0.05162(14) 0.2562(4) 0.0622(18) Uani 1 1 d . . . H62A H 0.0834 0.0308 0.2309 0.093 Uiso 1 1 calc R . . H62B H 0.1871 0.0468 0.2741 0.093 Uiso 1 1 calc R . . H62C H 0.1120 0.0703 0.2143 0.093 Uiso 1 1 calc R . . C63 C 0.2029(4) 0.09303(15) 0.4145(3) 0.0437(14) Uani 1 1 d . . . H63 H 0.2352 0.0711 0.4207 0.052 Uiso 1 1 calc R . . C64 C 0.2533(4) 0.12166(15) 0.4483(3) 0.0472(15) Uani 1 1 d . . . H64 H 0.3196 0.1197 0.4764 0.057 Uiso 1 1 calc R . . C65 C 0.2051(4) 0.15303(15) 0.4402(3) 0.0468(15) Uani 1 1 d . . . H65 H 0.2390 0.1728 0.4642 0.056 Uiso 1 1 calc R . . C66 C 0.1086(4) 0.15724(13) 0.3984(3) 0.0373(13) Uani 1 1 d . . . C67 C 0.0591(4) 0.19283(13) 0.3934(4) 0.0480(15) Uani 1 1 d . . . H67 H -0.0110 0.1904 0.3647 0.058 Uiso 1 1 calc R . . C68 C 0.0480(5) 0.20796(16) 0.4826(4) 0.076(2) Uani 1 1 d . . . H68A H 0.0069 0.1923 0.5153 0.114 Uiso 1 1 calc R . . H68B H 0.0140 0.2305 0.4775 0.114 Uiso 1 1 calc R . . H68C H 0.1161 0.2107 0.5117 0.114 Uiso 1 1 calc R . . C69 C 0.1197(5) 0.21762(14) 0.3415(4) 0.0653(19) Uani 1 1 d . . . H69A H 0.0854 0.2401 0.3387 0.098 Uiso 1 1 calc R . . H69B H 0.1237 0.2085 0.2839 0.098 Uiso 1 1 calc R . . H69C H 0.1890 0.2203 0.3683 0.098 Uiso 1 1 calc R . . C70 C -0.2990(4) 0.11043(12) 0.2790(3) 0.0321(12) Uani 1 1 d . . . C71 C -0.3552(4) 0.12663(13) 0.3406(3) 0.0349(13) Uani 1 1 d . . . C72 C -0.3180(4) 0.15816(13) 0.3907(3) 0.0465(15) Uani 1 1 d . . . H72 H -0.2427 0.1605 0.3839 0.056 Uiso 1 1 calc R . . C73 C -0.3330(5) 0.15520(15) 0.4865(3) 0.0650(19) Uani 1 1 d . . . H73A H -0.3066 0.1761 0.5155 0.098 Uiso 1 1 calc R . . H73B H -0.2958 0.1350 0.5097 0.098 Uiso 1 1 calc R . . H73C H -0.4062 0.1527 0.4952 0.098 Uiso 1 1 calc R . . C74 C -0.3705(5) 0.19063(14) 0.3531(4) 0.0659(19) Uani 1 1 d . . . H74A H -0.3456 0.2109 0.3853 0.099 Uiso 1 1 calc R . . H74B H -0.4449 0.1886 0.3565 0.099 Uiso 1 1 calc R . . H74C H -0.3547 0.1931 0.2936 0.099 Uiso 1 1 calc R . . C75 C -0.4521(4) 0.11377(14) 0.3545(4) 0.0470(15) Uani 1 1 d . . . H75 H -0.4896 0.1238 0.3977 0.056 Uiso 1 1 calc R . . C76 C -0.4954(4) 0.08691(15) 0.3075(4) 0.0517(16) Uani 1 1 d . . . H76 H -0.5608 0.0781 0.3192 0.062 Uiso 1 1 calc R . . C77 C -0.4421(4) 0.07306(13) 0.2432(3) 0.0409(14) Uani 1 1 d . . . H77 H -0.4727 0.0551 0.2094 0.049 Uiso 1 1 calc R . . C78 C -0.3448(4) 0.08465(12) 0.2263(3) 0.0324(12) Uani 1 1 d . . . C79 C -0.2886(4) 0.06862(13) 0.1547(3) 0.0409(14) Uani 1 1 d . . . H79 H -0.2445 0.0871 0.1320 0.049 Uiso 1 1 calc R . . C80 C -0.2170(5) 0.03927(15) 0.1856(4) 0.069(2) Uani 1 1 d . . . H80A H -0.1817 0.0300 0.1376 0.104 Uiso 1 1 calc R . . H80B H -0.2572 0.0209 0.2102 0.104 Uiso 1 1 calc R . . H80C H -0.1663 0.0481 0.2287 0.104 Uiso 1 1 calc R . . C81 C -0.3603(5) 0.05636(15) 0.0811(4) 0.0666(19) Uani 1 1 d . . . H81A H -0.3200 0.0464 0.0370 0.100 Uiso 1 1 calc R . . H81B H -0.4002 0.0760 0.0575 0.100 Uiso 1 1 calc R . . H81C H -0.4070 0.0388 0.1013 0.100 Uiso 1 1 calc R . . C101 C 0.3880(5) 0.01264(18) 0.6400(5) 0.096(3) Uani 1 1 d . . . H10C H 0.3286 0.0199 0.6031 0.144 Uiso 1 1 calc R . . H10D H 0.3898 0.0257 0.6932 0.144 Uiso 1 1 calc R . . H10E H 0.3827 -0.0121 0.6523 0.144 Uiso 1 1 calc R . . C102 C 0.5183(6) 0.06707(16) 0.5655(5) 0.109(3) Uani 1 1 d . . . H10F H 0.5819 0.0711 0.5373 0.163 Uiso 1 1 calc R . . H10G H 0.5207 0.0799 0.6192 0.163 Uiso 1 1 calc R . . H10H H 0.4597 0.0750 0.5287 0.163 Uiso 1 1 calc R . . C103 C 0.6163(6) 0.0065(2) 0.6560(6) 0.135(4) Uani 1 1 d . . . H10I H 0.6796 0.0111 0.6278 0.202 Uiso 1 1 calc R . . H10J H 0.6108 -0.0184 0.6669 0.202 Uiso 1 1 calc R . . H10K H 0.6178 0.0191 0.7099 0.202 Uiso 1 1 calc R . . N1 N 0.0518(3) 0.13707(10) -0.1054(2) 0.0335(10) Uani 1 1 d . . . N2 N 0.2031(3) 0.11278(10) -0.0617(3) 0.0347(11) Uani 1 1 d . . . N3 N -0.1962(3) 0.12039(9) 0.2656(2) 0.0329(10) Uani 1 1 d . B . N4 N -0.0334(3) 0.13247(9) 0.3122(2) 0.0309(10) Uani 1 1 d . B . O1 O 0.2582(2) 0.13475(8) 0.1295(2) 0.0413(9) Uani 1 1 d . . . O2 O 0.1743(3) 0.19952(9) 0.0197(2) 0.0520(11) Uani 1 1 d . . . O3 O -0.2402(2) 0.15200(8) 0.0757(2) 0.0411(9) Uani 1 1 d . B . O4 O -0.1332(3) 0.20316(9) 0.2110(2) 0.0548(11) Uani 1 1 d . B . Y1 Y 0.10457(4) 0.144412(12) 0.04151(3) 0.03370(15) Uani 1 1 d . B . Y2 Y -0.08816(4) 0.154719(12) 0.17294(3) 0.03314(15) Uani 1 1 d . . . Si1 Si 0.50481(15) 0.02075(5) 0.58676(12) 0.0667(6) Uani 1 1 d . . . O5 O 0.5000 0.0000 0.5000 0.172(4) Uani 1 2 d S . . H1 H -0.028(3) 0.1667(9) 0.049(2) 0.027(11) Uiso 1 1 d . . . H2 H -0.001(3) 0.1120(10) 0.107(3) 0.050(14) Uiso 1 1 d . . . H3 H 0.074(3) 0.1665(9) 0.160(2) 0.035(12) 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 C4 0.035(4) 0.065(4) 0.032(3) 0.010(3) 0.001(3) 0.004(3) C5 0.042(4) 0.076(4) 0.040(4) -0.005(3) 0.000(3) 0.010(3) C6 0.040(4) 0.070(4) 0.046(4) 0.002(3) 0.003(3) -0.009(3) C7 0.029(4) 0.087(5) 0.043(4) -0.011(3) 0.003(3) -0.001(3) C8 0.134(8) 0.061(5) 0.100(7) -0.023(4) 0.034(6) -0.007(5) C9 0.145(9) 0.067(6) 0.124(8) -0.009(5) -0.050(7) -0.041(6) C10 0.073(6) 0.087(6) 0.153(9) 0.039(6) -0.029(6) -0.038(5) C11 0.065(5) 0.070(5) 0.094(6) 0.013(4) 0.026(4) -0.017(4) C12 0.035(4) 0.080(5) 0.054(4) 0.006(3) 0.012(3) 0.016(3) C13 0.059(5) 0.083(5) 0.075(5) 0.025(4) 0.016(4) 0.021(4) C14 0.052(5) 0.088(5) 0.067(5) 0.028(4) 0.008(4) 0.008(4) C15 0.050(4) 0.073(4) 0.037(4) 0.000(3) 0.005(3) -0.002(3) C16 0.081(6) 0.075(5) 0.091(6) -0.006(5) -0.003(5) 0.021(4) C17 0.163(8) 0.073(3) 0.091(5) 0.012(4) 0.025(5) 0.033(5) C18 0.163(8) 0.073(3) 0.091(5) 0.012(4) 0.025(5) 0.033(5) C17' 0.163(8) 0.073(3) 0.091(5) 0.012(4) 0.025(5) 0.033(5) C18' 0.163(8) 0.073(3) 0.091(5) 0.012(4) 0.025(5) 0.033(5) C19 0.163(8) 0.073(3) 0.091(5) 0.012(4) 0.025(5) 0.033(5) C20 0.038(4) 0.033(3) 0.036(3) 0.004(3) 0.011(3) -0.005(3) C21 0.040(4) 0.053(4) 0.025(3) -0.003(3) 0.002(3) 0.002(3) C22 0.045(4) 0.059(4) 0.029(3) -0.010(3) -0.004(3) 0.007(3) C23 0.057(5) 0.079(5) 0.047(4) -0.018(4) 0.007(3) 0.008(4) C24 0.065(5) 0.099(6) 0.034(4) -0.015(4) 0.008(3) 0.011(4) C25 0.054(4) 0.094(5) 0.032(4) 0.004(3) 0.005(3) 0.022(4) C26 0.048(4) 0.072(4) 0.036(4) -0.004(3) 0.008(3) 0.003(3) C27 0.031(3) 0.043(3) 0.033(3) 0.006(3) 0.005(3) 0.003(3) C28 0.039(4) 0.039(3) 0.036(3) 0.003(3) 0.005(3) -0.005(3) C29 0.044(4) 0.039(3) 0.053(4) 0.017(3) -0.001(3) -0.003(3) C30 0.082(5) 0.051(4) 0.064(5) -0.012(3) 0.005(4) -0.022(4) C31 0.094(6) 0.065(4) 0.067(5) 0.015(4) 0.017(4) -0.018(4) C32 0.048(4) 0.051(4) 0.044(4) 0.004(3) -0.010(3) 0.003(3) C33 0.048(4) 0.076(5) 0.046(4) 0.004(4) -0.008(3) -0.003(4) C34 0.046(4) 0.057(4) 0.035(4) -0.005(3) 0.001(3) -0.013(3) C35 0.040(4) 0.042(3) 0.028(3) 0.000(3) 0.005(3) -0.006(3) C36 0.050(4) 0.043(3) 0.038(3) 0.003(3) 0.001(3) -0.013(3) C37 0.089(5) 0.048(4) 0.050(4) 0.007(3) 0.013(4) -0.011(3) C38 0.078(5) 0.051(4) 0.055(4) -0.005(3) 0.001(4) -0.008(3) C39 0.035(4) 0.052(4) 0.031(3) -0.005(3) 0.006(3) 0.003(3) C40 0.044(4) 0.051(4) 0.028(3) -0.004(3) 0.002(3) 0.010(3) C41 0.045(4) 0.037(3) 0.033(3) -0.001(3) 0.002(3) 0.012(3) C42 0.065(5) 0.066(4) 0.046(4) 0.008(3) 0.006(3) -0.003(4) C43 0.054(4) 0.087(5) 0.048(4) 0.012(4) 0.004(3) 0.018(4) C44 0.057(4) 0.064(4) 0.038(4) 0.002(3) 0.009(3) 0.017(3) C45 0.056(5) 0.089(5) 0.047(4) -0.001(4) -0.001(4) 0.021(4) C46 0.040(4) 0.089(5) 0.049(4) -0.009(4) 0.012(3) 0.015(4) C47 0.050(4) 0.051(4) 0.036(3) -0.004(3) -0.003(3) 0.003(3) C48 0.046(4) 0.071(4) 0.050(4) -0.002(3) 0.016(3) 0.000(3) C49 0.062(5) 0.094(5) 0.069(5) -0.008(4) 0.015(4) -0.023(4) C50 0.070(5) 0.081(5) 0.053(4) 0.003(4) 0.017(4) 0.002(4) C51 0.033(3) 0.034(3) 0.031(3) -0.001(2) 0.007(3) 0.004(3) C52 0.025(3) 0.053(4) 0.029(3) 0.002(3) 0.004(3) 0.000(3) C53 0.030(4) 0.072(4) 0.044(4) -0.003(3) 0.007(3) -0.011(3) C54 0.051(4) 0.112(6) 0.031(4) 0.006(4) 0.008(3) -0.008(4) C55 0.053(5) 0.106(6) 0.051(5) 0.029(4) 0.011(4) -0.007(4) C56 0.051(4) 0.076(5) 0.053(4) 0.022(4) 0.004(3) 0.000(3) C57 0.035(4) 0.058(4) 0.035(3) 0.004(3) 0.002(3) 0.001(3) C58 0.033(3) 0.042(3) 0.022(3) -0.003(2) 0.004(2) -0.001(3) C59 0.038(4) 0.049(4) 0.030(3) 0.003(3) 0.009(3) 0.006(3) C60 0.030(3) 0.043(3) 0.041(3) 0.002(3) 0.004(3) 0.008(3) C61 0.069(5) 0.046(4) 0.066(5) 0.006(3) 0.000(4) 0.002(3) C62 0.076(5) 0.051(4) 0.062(4) -0.024(3) 0.022(4) 0.002(3) C63 0.036(4) 0.054(4) 0.041(4) 0.000(3) -0.001(3) 0.011(3) C64 0.033(4) 0.067(4) 0.040(4) 0.003(3) -0.003(3) 0.003(3) C65 0.045(4) 0.054(4) 0.041(4) -0.014(3) -0.002(3) -0.012(3) C66 0.039(4) 0.040(3) 0.033(3) -0.007(3) 0.003(3) 0.000(3) C67 0.035(4) 0.048(4) 0.060(4) -0.018(3) -0.007(3) -0.005(3) C68 0.071(5) 0.078(5) 0.080(5) -0.025(4) 0.018(4) 0.005(4) C69 0.069(5) 0.050(4) 0.077(5) -0.004(3) 0.005(4) 0.009(3) C70 0.029(3) 0.031(3) 0.036(3) 0.004(2) -0.002(3) -0.002(2) C71 0.029(3) 0.040(3) 0.036(3) 0.007(3) 0.002(3) 0.005(3) C72 0.043(4) 0.045(3) 0.053(4) -0.009(3) 0.012(3) 0.008(3) C73 0.066(5) 0.086(5) 0.044(4) -0.015(3) 0.019(3) 0.005(4) C74 0.075(5) 0.048(4) 0.074(5) -0.016(3) 0.001(4) 0.008(3) C75 0.046(4) 0.050(4) 0.047(4) 0.012(3) 0.014(3) 0.012(3) C76 0.035(4) 0.054(4) 0.067(5) 0.011(3) 0.003(3) -0.008(3) C77 0.032(4) 0.046(3) 0.044(4) 0.002(3) -0.005(3) -0.013(3) C78 0.026(3) 0.037(3) 0.033(3) 0.005(2) -0.005(2) 0.000(2) C79 0.044(4) 0.040(3) 0.039(3) -0.003(3) 0.006(3) -0.008(3) C80 0.086(5) 0.070(4) 0.054(4) -0.014(3) 0.026(4) 0.018(4) C81 0.075(5) 0.078(5) 0.046(4) -0.008(3) 0.004(4) -0.027(4) C101 0.074(6) 0.107(6) 0.111(7) 0.007(5) 0.036(5) 0.010(5) C102 0.107(7) 0.079(5) 0.144(8) 0.032(5) 0.038(6) 0.025(5) C103 0.084(7) 0.138(8) 0.179(10) 0.095(7) -0.012(6) -0.020(6) N1 0.031(3) 0.038(3) 0.031(3) 0.002(2) 0.001(2) -0.003(2) N2 0.036(3) 0.039(3) 0.029(3) -0.004(2) 0.003(2) 0.003(2) N3 0.032(3) 0.038(3) 0.029(3) -0.001(2) 0.003(2) -0.004(2) N4 0.033(3) 0.027(2) 0.032(3) -0.0032(19) 0.002(2) 0.000(2) O1 0.024(2) 0.061(2) 0.039(2) -0.0003(18) 0.0018(17) -0.0050(18) O2 0.051(3) 0.045(2) 0.061(3) -0.005(2) 0.014(2) -0.008(2) O3 0.030(2) 0.056(2) 0.037(2) 0.0047(18) 0.0034(17) 0.0096(18) O4 0.059(3) 0.040(2) 0.065(3) -0.008(2) 0.003(2) 0.006(2) Y1 0.0295(3) 0.0408(3) 0.0309(3) -0.0023(2) 0.0022(2) -0.0007(2) Y2 0.0298(3) 0.0371(3) 0.0327(3) 0.0034(2) 0.0034(2) 0.0013(2) Si1 0.0672(14) 0.0720(13) 0.0629(14) 0.0102(10) 0.0192(11) 0.0113(11) O5 0.243(12) 0.171(8) 0.113(8) -0.079(6) 0.089(8) -0.028(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 C4 O1 1.454(6) . ? C4 C5 1.485(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.528(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.514(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O1 1.451(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.446(9) . ? C8 O2 1.463(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.512(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.491(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O2 1.420(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O3 1.446(5) . ? C12 C13 1.483(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.538(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.511(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O3 1.453(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O4 1.364(6) . ? C16 C17' 1.403(17) . ? C16 C17 1.50(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.57(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.61(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C17' C18' 1.50(3) . ? C17' H17C 0.9900 . ? C17' H17D 0.9900 . ? C18' C19 1.480(17) . ? C18' H18C 0.9900 . ? C18' H18D 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 N2 1.338(6) . ? C20 N1 1.346(6) . ? C20 C21 1.488(7) . ? C20 Y1 2.874(5) . ? C21 C26 1.386(7) . ? C21 C22 1.389(6) . ? C22 C23 1.384(7) . ? C22 H22 0.9500 . ? C23 C24 1.369(8) . ? C23 H23 0.9500 . ? C24 C25 1.368(8) . ? C24 H24 0.9500 . ? C25 C26 1.390(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C35 1.406(7) . ? C27 C28 1.420(7) . ? C27 N1 1.427(6) . ? C28 C32 1.371(7) . ? C28 C29 1.528(7) . ? C29 C30 1.518(7) . ? C29 C31 1.525(7) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.385(7) . ? C32 H32 0.9500 . ? C33 C34 1.367(7) . ? C33 H33 0.9500 . ? C34 C35 1.393(7) . ? C34 H34 0.9500 . ? C35 C36 1.519(7) . ? C36 C38 1.534(7) . ? C36 C37 1.536(7) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.414(7) . ? C39 C47 1.422(7) . ? C39 N2 1.429(6) . ? C40 C44 1.384(7) . ? C40 C41 1.524(7) . ? C41 C43 1.529(7) . ? C41 C42 1.536(7) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.378(7) . ? C44 H44 0.9500 . ? C45 C46 1.363(8) . ? C45 H45 0.9500 . ? C46 C47 1.396(7) . ? C46 H46 0.9500 . ? C47 C48 1.493(7) . ? C48 C50 1.544(7) . ? C48 C49 1.549(8) . ? C48 H48 1.0000 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 N4 1.331(6) . ? C51 N3 1.342(6) . ? C51 C52 1.505(6) . ? C51 Y2 2.899(5) . ? C52 C53 1.383(7) . ? C52 C57 1.389(7) . ? C53 C54 1.405(7) . ? C53 H53 0.9500 . ? C54 C55 1.362(8) . ? C54 H54 0.9500 . ? C55 C56 1.379(8) . ? C55 H55 0.9500 . ? C56 C57 1.383(7) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 N4 1.411(6) . ? C58 C59 1.415(7) . ? C58 C66 1.416(7) . ? C59 C63 1.387(7) . ? C59 C60 1.524(7) . ? C60 C62 1.527(6) . ? C60 C61 1.536(7) . ? C60 H60 1.0000 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.379(7) . ? C63 H63 0.9500 . ? C64 C65 1.370(7) . ? C64 H64 0.9500 . ? C65 C66 1.394(7) . ? C65 H65 0.9500 . ? C66 C67 1.522(7) . ? C67 C69 1.518(7) . ? C67 C68 1.541(7) . ? C67 H67 1.0000 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C71 1.404(6) . ? C70 C78 1.407(6) . ? C70 N3 1.427(6) . ? C71 C75 1.391(7) . ? C71 C72 1.517(7) . ? C72 C74 1.533(7) . ? C72 C73 1.542(7) . ? C72 H72 1.0000 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C76 1.377(7) . ? C75 H75 0.9500 . ? C76 C77 1.377(7) . ? C76 H76 0.9500 . ? C77 C78 1.391(6) . ? C77 H77 0.9500 . ? C78 C79 1.521(6) . ? C79 C81 1.519(7) . ? C79 C80 1.531(7) . ? C79 H79 1.0000 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C101 Si1 1.817(6) . ? C101 H10C 0.9800 . ? C101 H10D 0.9800 . ? C101 H10E 0.9800 . ? C102 Si1 1.836(6) . ? C102 H10F 0.9800 . ? C102 H10G 0.9800 . ? C102 H10H 0.9800 . ? C103 Si1 1.847(8) . ? C103 H10I 0.9800 . ? C103 H10J 0.9800 . ? C103 H10K 0.9800 . ? N1 Y1 2.391(4) . ? N2 Y1 2.468(4) . ? N3 Y2 2.485(4) . ? N4 Y2 2.424(4) . ? O1 Y1 2.394(3) . ? O2 Y1 2.354(3) . ? O3 Y2 2.430(3) . ? O4 Y2 2.067(3) . ? Y1 Y2 3.3903(8) . ? Y1 H1 1.95(4) . ? Y1 H2 2.17(4) . ? Y1 H3 2.12(4) . ? Y2 H1 2.20(4) . ? Y2 H2 2.30(4) . ? Y2 H3 2.19(4) . ? Si1 O5 1.585(2) . ? O5 Si1 1.585(2) 3_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C4 C5 103.7(4) . . ? O1 C4 H4A 111.0 . . ? C5 C4 H4A 111.0 . . ? O1 C4 H4B 111.0 . . ? C5 C4 H4B 111.0 . . ? H4A C4 H4B 109.0 . . ? C4 C5 C6 103.4(4) . . ? C4 C5 H5A 111.1 . . ? C6 C5 H5A 111.1 . . ? C4 C5 H5B 111.1 . . ? C6 C5 H5B 111.1 . . ? H5A C5 H5B 109.0 . . ? C7 C6 C5 104.8(4) . . ? C7 C6 H6A 110.8 . . ? C5 C6 H6A 110.8 . . ? C7 C6 H6B 110.8 . . ? C5 C6 H6B 110.8 . . ? H6A C6 H6B 108.9 . . ? O1 C7 C6 105.8(4) . . ? O1 C7 H7A 110.6 . . ? C6 C7 H7A 110.6 . . ? O1 C7 H7B 110.6 . . ? C6 C7 H7B 110.6 . . ? H7A C7 H7B 108.7 . . ? C9 C8 O2 105.9(6) . . ? C9 C8 H8A 110.6 . . ? O2 C8 H8A 110.6 . . ? C9 C8 H8B 110.6 . . ? O2 C8 H8B 110.6 . . ? H8A C8 H8B 108.7 . . ? C8 C9 C10 105.7(7) . . ? C8 C9 H9A 110.6 . . ? C10 C9 H9A 110.6 . . ? C8 C9 H9B 110.6 . . ? C10 C9 H9B 110.6 . . ? H9A C9 H9B 108.7 . . ? C11 C10 C9 104.3(6) . . ? C11 C10 H10A 110.9 . . ? C9 C10 H10A 110.9 . . ? C11 C10 H10B 110.9 . . ? C9 C10 H10B 110.9 . . ? H10A C10 H10B 108.9 . . ? O2 C11 C10 106.5(6) . . ? O2 C11 H11A 110.4 . . ? C10 C11 H11A 110.4 . . ? O2 C11 H11B 110.4 . . ? C10 C11 H11B 110.4 . . ? H11A C11 H11B 108.6 . . ? O3 C12 C13 107.1(4) . . ? O3 C12 H12A 110.3 . . ? C13 C12 H12A 110.3 . . ? O3 C12 H12B 110.3 . . ? C13 C12 H12B 110.3 . . ? H12A C12 H12B 108.6 . . ? C12 C13 C14 105.1(5) . . ? C12 C13 H13A 110.7 . . ? C14 C13 H13A 110.7 . . ? C12 C13 H13B 110.7 . . ? C14 C13 H13B 110.7 . . ? H13A C13 H13B 108.8 . . ? C15 C14 C13 103.0(5) . . ? C15 C14 H14A 111.2 . . ? C13 C14 H14A 111.2 . . ? C15 C14 H14B 111.2 . . ? C13 C14 H14B 111.2 . . ? H14A C14 H14B 109.1 . . ? O3 C15 C14 103.8(4) . . ? O3 C15 H15A 111.0 . . ? C14 C15 H15A 111.0 . . ? O3 C15 H15B 111.0 . . ? C14 C15 H15B 111.0 . . ? H15A C15 H15B 109.0 . . ? O4 C16 C17' 109.5(9) . . ? O4 C16 C17 115.5(10) . . ? C17' C16 C17 38.8(9) . . ? O4 C16 H16A 109.8 . . ? C17' C16 H16A 109.8 . . ? C17 C16 H16A 131.6 . . ? O4 C16 H16B 109.8 . . ? C17' C16 H16B 109.8 . . ? C17 C16 H16B 72.0 . . ? H16A C16 H16B 108.2 . . ? C16 C17 C18 100(2) . . ? C16 C17 H17A 111.8 . . ? C18 C17 H17A 111.8 . . ? C16 C17 H17B 111.8 . . ? C18 C17 H17B 111.8 . . ? H17A C17 H17B 109.5 . . ? C17 C18 C19 116(2) . . ? C17 C18 H18A 108.3 . . ? C19 C18 H18A 108.3 . . ? C17 C18 H18B 108.3 . . ? C19 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? C16 C17' C18' 124(2) . . ? C16 C17' H17C 106.2 . . ? C18' C17' H17C 106.2 . . ? C16 C17' H17D 106.2 . . ? C18' C17' H17D 106.2 . . ? H17C C17' H17D 106.4 . . ? C19 C18' C17' 117(2) . . ? C19 C18' H18C 108.0 . . ? C17' C18' H18C 108.0 . . ? C19 C18' H18D 108.0 . . ? C17' C18' H18D 108.0 . . ? H18C C18' H18D 107.2 . . ? C18' C19 C18 32.5(10) . . ? C18' C19 H19A 109.5 . . ? C18 C19 H19A 109.1 . . ? C18' C19 H19B 109.5 . . ? C18 C19 H19B 79.7 . . ? H19A C19 H19B 109.5 . . ? C18' C19 H19C 109.5 . . ? C18 C19 H19C 134.0 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 N1 114.4(5) . . ? N2 C20 C21 123.8(5) . . ? N1 C20 C21 121.8(5) . . ? N2 C20 Y1 59.0(3) . . ? N1 C20 Y1 55.8(3) . . ? C21 C20 Y1 174.7(4) . . ? C26 C21 C22 117.8(5) . . ? C26 C21 C20 119.9(5) . . ? C22 C21 C20 122.3(5) . . ? C23 C22 C21 120.5(5) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C22 120.5(6) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 120.2(6) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 119.4(6) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C21 C26 C25 121.5(6) . . ? C21 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C35 C27 C28 117.8(5) . . ? C35 C27 N1 122.5(5) . . ? C28 C27 N1 119.6(5) . . ? C32 C28 C27 120.6(5) . . ? C32 C28 C29 119.3(5) . . ? C27 C28 C29 120.1(5) . . ? C30 C29 C31 110.0(4) . . ? C30 C29 C28 110.9(4) . . ? C31 C29 C28 112.6(5) . . ? C30 C29 H29 107.7 . . ? C31 C29 H29 107.7 . . ? C28 C29 H29 107.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C28 C32 C33 120.8(5) . . ? C28 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C34 C33 C32 119.7(6) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 121.1(5) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C34 C35 C27 120.0(5) . . ? C34 C35 C36 118.4(5) . . ? C27 C35 C36 121.5(5) . . ? C35 C36 C38 113.0(5) . . ? C35 C36 C37 110.8(4) . . ? C38 C36 C37 110.1(4) . . ? C35 C36 H36 107.6 . . ? C38 C36 H36 107.6 . . ? C37 C36 H36 107.6 . . ? 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 . . ? C40 C39 C47 118.8(5) . . ? C40 C39 N2 119.2(4) . . ? C47 C39 N2 122.0(5) . . ? C44 C40 C39 119.7(5) . . ? C44 C40 C41 119.3(5) . . ? C39 C40 C41 121.0(4) . . ? C40 C41 C43 113.0(4) . . ? C40 C41 C42 112.7(4) . . ? C43 C41 C42 108.3(4) . . ? C40 C41 H41 107.6 . . ? C43 C41 H41 107.6 . . ? C42 C41 H41 107.6 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C40 121.2(6) . . ? C45 C44 H44 119.4 . . ? C40 C44 H44 119.4 . . ? C46 C45 C44 119.7(6) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C45 C46 C47 121.9(6) . . ? C45 C46 H46 119.0 . . ? C47 C46 H46 119.0 . . ? C46 C47 C39 118.5(5) . . ? C46 C47 C48 118.4(5) . . ? C39 C47 C48 123.0(5) . . ? C47 C48 C50 112.5(5) . . ? C47 C48 C49 110.8(5) . . ? C50 C48 C49 108.2(5) . . ? C47 C48 H48 108.4 . . ? C50 C48 H48 108.4 . . ? C49 C48 H48 108.4 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N4 C51 N3 114.9(4) . . ? N4 C51 C52 122.8(5) . . ? N3 C51 C52 122.4(5) . . ? N4 C51 Y2 56.1(2) . . ? N3 C51 Y2 58.8(2) . . ? C52 C51 Y2 177.3(3) . . ? C53 C52 C57 118.1(5) . . ? C53 C52 C51 120.1(5) . . ? C57 C52 C51 121.8(5) . . ? C52 C53 C54 120.5(5) . . ? C52 C53 H53 119.7 . . ? C54 C53 H53 119.7 . . ? C55 C54 C53 120.4(6) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C54 C55 C56 119.5(6) . . ? C54 C55 H55 120.3 . . ? C56 C55 H55 120.3 . . ? C55 C56 C57 120.5(6) . . ? C55 C56 H56 119.7 . . ? C57 C56 H56 119.7 . . ? C56 C57 C52 121.0(5) . . ? C56 C57 H57 119.5 . . ? C52 C57 H57 119.5 . . ? N4 C58 C59 122.1(5) . . ? N4 C58 C66 118.1(5) . . ? C59 C58 C66 119.5(5) . . ? C63 C59 C58 118.8(5) . . ? C63 C59 C60 119.3(5) . . ? C58 C59 C60 121.9(5) . . ? C59 C60 C62 109.4(4) . . ? C59 C60 C61 112.5(4) . . ? C62 C60 C61 110.9(4) . . ? C59 C60 H60 108.0 . . ? C62 C60 H60 108.0 . . ? C61 C60 H60 108.0 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 C59 122.4(5) . . ? C64 C63 H63 118.8 . . ? C59 C63 H63 118.8 . . ? C65 C64 C63 118.2(5) . . ? C65 C64 H64 120.9 . . ? C63 C64 H64 120.9 . . ? C64 C65 C66 122.9(5) . . ? C64 C65 H65 118.5 . . ? C66 C65 H65 118.5 . . ? C65 C66 C58 118.2(5) . . ? C65 C66 C67 119.9(5) . . ? C58 C66 C67 121.9(5) . . ? C69 C67 C66 111.5(4) . . ? C69 C67 C68 109.6(5) . . ? C66 C67 C68 111.2(5) . . ? C69 C67 H67 108.1 . . ? C66 C67 H67 108.1 . . ? C68 C67 H67 108.1 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C71 C70 C78 120.3(5) . . ? C71 C70 N3 121.5(4) . . ? C78 C70 N3 118.2(4) . . ? C75 C71 C70 118.1(5) . . ? C75 C71 C72 118.1(5) . . ? C70 C71 C72 123.8(5) . . ? C71 C72 C74 109.8(5) . . ? C71 C72 C73 113.2(4) . . ? C74 C72 C73 110.9(4) . . ? C71 C72 H72 107.6 . . ? C74 C72 H72 107.6 . . ? C73 C72 H72 107.6 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C74 H74A 109.5 . . ? C72 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C72 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C76 C75 C71 122.1(5) . . ? C76 C75 H75 118.9 . . ? C71 C75 H75 118.9 . . ? C77 C76 C75 118.8(5) . . ? C77 C76 H76 120.6 . . ? C75 C76 H76 120.6 . . ? C76 C77 C78 121.9(5) . . ? C76 C77 H77 119.0 . . ? C78 C77 H77 119.0 . . ? C77 C78 C70 118.3(5) . . ? C77 C78 C79 120.2(5) . . ? C70 C78 C79 121.5(4) . . ? C81 C79 C78 113.1(5) . . ? C81 C79 C80 110.2(5) . . ? C78 C79 C80 112.4(4) . . ? C81 C79 H79 106.9 . . ? C78 C79 H79 106.9 . . ? C80 C79 H79 106.9 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? Si1 C101 H10C 109.5 . . ? Si1 C101 H10D 109.5 . . ? H10C C101 H10D 109.5 . . ? Si1 C101 H10E 109.5 . . ? H10C C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? Si1 C102 H10F 109.5 . . ? Si1 C102 H10G 109.5 . . ? H10F C102 H10G 109.5 . . ? Si1 C102 H10H 109.5 . . ? H10F C102 H10H 109.5 . . ? H10G C102 H10H 109.5 . . ? Si1 C103 H10I 109.5 . . ? Si1 C103 H10J 109.5 . . ? H10I C103 H10J 109.5 . . ? Si1 C103 H10K 109.5 . . ? H10I C103 H10K 109.5 . . ? H10J C103 H10K 109.5 . . ? C20 N1 C27 122.4(4) . . ? C20 N1 Y1 96.5(3) . . ? C27 N1 Y1 137.3(3) . . ? C20 N2 C39 120.3(4) . . ? C20 N2 Y1 93.3(3) . . ? C39 N2 Y1 146.2(3) . . ? C51 N3 C70 120.7(4) . . ? C51 N3 Y2 93.7(3) . . ? C70 N3 Y2 144.0(3) . . ? C51 N4 C58 123.8(4) . . ? C51 N4 Y2 96.7(3) . . ? C58 N4 Y2 138.5(3) . . ? C7 O1 C4 104.7(4) . . ? C7 O1 Y1 126.7(3) . . ? C4 O1 Y1 125.9(3) . . ? C11 O2 C8 104.2(4) . . ? C11 O2 Y1 131.5(3) . . ? C8 O2 Y1 124.2(4) . . ? C12 O3 C15 104.3(4) . . ? C12 O3 Y2 118.2(3) . . ? C15 O3 Y2 130.1(3) . . ? C16 O4 Y2 175.8(4) . . ? O2 Y1 N1 93.21(13) . . ? O2 Y1 O1 84.75(12) . . ? N1 Y1 O1 136.12(13) . . ? O2 Y1 N2 97.45(12) . . ? N1 Y1 N2 55.31(14) . . ? O1 Y1 N2 81.42(13) . . ? O2 Y1 C20 97.82(13) . . ? N1 Y1 C20 27.73(13) . . ? O1 Y1 C20 109.05(14) . . ? N2 Y1 C20 27.69(13) . . ? O2 Y1 Y2 107.03(9) . . ? N1 Y1 Y2 115.39(10) . . ? O1 Y1 Y2 106.97(8) . . ? N2 Y1 Y2 154.62(9) . . ? C20 Y1 Y2 137.62(11) . . ? O2 Y1 H1 87.8(10) . . ? N1 Y1 H1 85.0(11) . . ? O1 Y1 H1 138.5(11) . . ? N2 Y1 H1 140.1(11) . . ? C20 Y1 H1 112.4(11) . . ? Y2 Y1 H1 37.7(11) . . ? O2 Y1 H2 148.9(11) . . ? N1 Y1 H2 103.9(11) . . ? O1 Y1 H2 99.6(11) . . ? N2 Y1 H2 113.6(11) . . ? C20 Y1 H2 109.4(11) . . ? Y2 Y1 H2 42.1(10) . . ? H1 Y1 H2 68.4(15) . . ? O2 Y1 H3 82.0(10) . . ? N1 Y1 H3 147.6(11) . . ? O1 Y1 H3 75.6(11) . . ? N2 Y1 H3 157.0(11) . . ? C20 Y1 H3 175.3(11) . . ? Y2 Y1 H3 38.8(10) . . ? H1 Y1 H3 62.9(15) . . ? H2 Y1 H3 69.6(15) . . ? O4 Y2 N4 97.58(14) . . ? O4 Y2 O3 89.22(13) . . ? N4 Y2 O3 137.46(12) . . ? O4 Y2 N3 97.52(13) . . ? N4 Y2 N3 54.64(13) . . ? O3 Y2 N3 82.88(13) . . ? O4 Y2 C51 97.94(14) . . ? N4 Y2 C51 27.13(13) . . ? O3 Y2 C51 110.40(13) . . ? N3 Y2 C51 27.52(13) . . ? O4 Y2 Y1 121.45(10) . . ? N4 Y2 Y1 109.03(9) . . ? O3 Y2 Y1 102.57(8) . . ? N3 Y2 Y1 140.46(9) . . ? C51 Y2 Y1 128.46(10) . . ? O4 Y2 H1 101.0(9) . . ? N4 Y2 H1 141.1(10) . . ? O3 Y2 H1 76.9(10) . . ? N3 Y2 H1 152.2(10) . . ? C51 Y2 H1 159.8(9) . . ? Y1 Y2 H1 32.8(10) . . ? O4 Y2 H2 160.8(10) . . ? N4 Y2 H2 91.7(11) . . ? O3 Y2 H2 95.3(11) . . ? N3 Y2 H2 101.6(10) . . ? C51 Y2 H2 97.9(10) . . ? Y1 Y2 H2 39.4(10) . . ? H1 Y2 H2 62.2(14) . . ? O4 Y2 H3 97.6(10) . . ? N4 Y2 H3 85.9(10) . . ? O3 Y2 H3 134.9(10) . . ? N3 Y2 H3 139.2(10) . . ? C51 Y2 H3 112.6(10) . . ? Y1 Y2 H3 37.4(10) . . ? H1 Y2 H3 58.1(14) . . ? H2 Y2 H3 66.2(14) . . ? O5 Si1 C101 109.0(3) . . ? O5 Si1 C102 109.7(3) . . ? C101 Si1 C102 110.3(3) . . ? O5 Si1 C103 110.1(3) . . ? C101 Si1 C103 109.2(4) . . ? C102 Si1 C103 108.6(4) . . ? Si1 O5 Si1 180.0 . 3_656 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.491 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.073 data_3-Y _database_code_depnum_ccdc_archive 'CCDC 859486' #TrackingRef '- Ln2H4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((PhNCN)YH)2(CH2NAr*)(THF)3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C83 H115 N5 O3 Y2' _chemical_formula_weight 1408.62 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 Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.898(3) _cell_length_b 23.121(6) _cell_length_c 35.564(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.028(4) _cell_angle_gamma 90.00 _cell_volume 9784(4) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.956 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3000 _exptl_absorpt_coefficient_mu 1.219 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5922 _exptl_absorpt_correction_T_max 0.6284 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 49823 _diffrn_reflns_av_R_equivalents 0.0663 _diffrn_reflns_av_sigmaI/netI 0.0932 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17087 _reflns_number_gt 10716 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0752P)^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 17087 _refine_ls_number_parameters 857 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1407 _refine_ls_wR_factor_gt 0.1301 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.936 _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 C3 C 0.1697(3) 0.09673(17) 0.77726(11) 0.0333(9) Uani 1 1 d D B . C4 C 0.3295(3) 0.04015(15) 0.80691(11) 0.0315(9) Uani 1 1 d . . . C5 C 0.3457(3) -0.00428(16) 0.78007(11) 0.0367(9) Uani 1 1 d . . . C6 C 0.2716(4) -0.01329(18) 0.74553(12) 0.0518(12) Uani 1 1 d . . . H6A H 0.2150 0.0174 0.7443 0.078 Uiso 1 1 calc R . . H6B H 0.2341 -0.0509 0.7473 0.078 Uiso 1 1 calc R . . H6C H 0.3182 -0.0122 0.7228 0.078 Uiso 1 1 calc R . . C7 C 0.4295(4) -0.04434(18) 0.78583(13) 0.0518(12) Uani 1 1 d . . . H7 H 0.4403 -0.0735 0.7673 0.062 Uiso 1 1 calc R . . C8 C 0.4988(4) -0.0446(2) 0.81706(14) 0.0580(13) Uani 1 1 d . . . H8 H 0.5562 -0.0727 0.8200 0.070 Uiso 1 1 calc R . . C9 C 0.4811(4) -0.00208(18) 0.84386(13) 0.0516(12) Uani 1 1 d . . . H9 H 0.5270 -0.0014 0.8657 0.062 Uiso 1 1 calc R . . C10 C 0.3993(3) 0.03885(16) 0.83958(11) 0.0341(9) Uani 1 1 d . . . C11 C 0.3841(3) 0.08334(18) 0.86954(11) 0.0446(10) Uani 1 1 d . . . H11A H 0.3231 0.1096 0.8624 0.067 Uiso 1 1 calc R . . H11B H 0.4539 0.1054 0.8725 0.067 Uiso 1 1 calc R . . H11C H 0.3654 0.0642 0.8933 0.067 Uiso 1 1 calc R . . C12 C 0.4140(4) 0.2027(2) 0.79868(13) 0.0563(12) Uani 1 1 d . B . H12A H 0.3730 0.2174 0.7764 0.068 Uiso 1 1 calc R . . H12B H 0.4288 0.1609 0.7951 0.068 Uiso 1 1 calc R . . C13 C 0.5206(4) 0.2347(3) 0.80394(16) 0.0819(18) Uani 1 1 d . . . H13A H 0.5769 0.2105 0.8171 0.098 Uiso 1 1 calc R A 1 H13B H 0.5519 0.2472 0.7795 0.098 Uiso 1 1 calc R A 1 C14 C 0.511(3) 0.2608(19) 0.8444(13) 0.088(4) Uani 0.25(2) 1 d P B 2 H14A H 0.5496 0.2360 0.8630 0.106 Uiso 0.25(2) 1 calc PR B 2 H14B H 0.5441 0.3001 0.8454 0.106 Uiso 0.25(2) 1 calc PR B 2 C14' C 0.4879(10) 0.2848(6) 0.8270(5) 0.088(4) Uani 0.75(2) 1 d P B 1 H14C H 0.4620 0.3172 0.8110 0.106 Uiso 0.75(2) 1 calc PR B 1 H14D H 0.5518 0.2982 0.8426 0.106 Uiso 0.75(2) 1 calc PR B 1 C15 C 0.3939(4) 0.2627(2) 0.85130(15) 0.0625(14) Uani 1 1 d . . . H15A H 0.4224 0.2523 0.8766 0.075 Uiso 1 1 calc R B 1 H15B H 0.3349 0.2926 0.8541 0.075 Uiso 1 1 calc R B 1 C16 C -0.1324(3) 0.06508(17) 0.79071(12) 0.0427(10) Uani 1 1 d . B . H16A H -0.1094 0.0805 0.8155 0.051 Uiso 1 1 calc R . . H16B H -0.0841 0.0315 0.7846 0.051 Uiso 1 1 calc R . . C17 C -0.2515(4) 0.0478(2) 0.79134(16) 0.0690(15) Uani 1 1 d . . . H17A H -0.2578 0.0052 0.7923 0.083 Uiso 1 1 calc R C 1 H17B H -0.2889 0.0640 0.8139 0.083 Uiso 1 1 calc R C 1 C18 C -0.3100(18) 0.0919(12) 0.7736(7) 0.074(4) Uani 0.46(2) 1 d P D 2 H18A H -0.3344 0.1212 0.7922 0.089 Uiso 0.46(2) 1 calc PR D 2 H18B H -0.3773 0.0763 0.7608 0.089 Uiso 0.46(2) 1 calc PR D 2 C18' C -0.3046(15) 0.0698(10) 0.7575(6) 0.074(4) Uani 0.54(2) 1 d P D 1 H18C H -0.3818 0.0835 0.7628 0.089 Uiso 0.54(2) 1 calc PR D 1 H18D H -0.3079 0.0396 0.7378 0.089 Uiso 0.54(2) 1 calc PR D 1 C19 C -0.2314(3) 0.1184(2) 0.74562(13) 0.0563(13) Uani 1 1 d . . . H19A H -0.2259 0.1196 0.7179 0.068 Uiso 1 1 calc R D 1 H19B H -0.2633 0.1556 0.7544 0.068 Uiso 1 1 calc R D 1 C20 C -0.1219(18) 0.2760(8) 0.8004(6) 0.071(2) Uani 0.356(13) 1 d PD E 2 H20A H -0.0585 0.2909 0.8156 0.086 Uiso 0.356(13) 1 calc PR E 2 H20B H -0.1589 0.2447 0.8149 0.086 Uiso 0.356(13) 1 calc PR E 2 C21 C -0.2036(18) 0.3233(8) 0.7933(4) 0.071(2) Uani 0.356(13) 1 d PD E 2 H21A H -0.1967 0.3551 0.8118 0.086 Uiso 0.356(13) 1 calc PR E 2 H21B H -0.2822 0.3092 0.7926 0.086 Uiso 0.356(13) 1 calc PR E 2 C22 C -0.159(2) 0.3408(6) 0.7532(4) 0.071(2) Uani 0.356(13) 1 d PD E 2 H22A H -0.2117 0.3660 0.7393 0.086 Uiso 0.356(13) 1 calc PR E 2 H22B H -0.0833 0.3589 0.7541 0.086 Uiso 0.356(13) 1 calc PR E 2 C23 C -0.156(2) 0.2782(8) 0.7379(6) 0.071(2) Uani 0.356(13) 1 d PD E 2 H23A H -0.2310 0.2599 0.7383 0.086 Uiso 0.356(13) 1 calc PR E 2 H23B H -0.1245 0.2764 0.7121 0.086 Uiso 0.356(13) 1 calc PR E 2 C20' C -0.0817(10) 0.2883(5) 0.8006(3) 0.071(2) Uani 0.644(13) 1 d PD E 1 H20C H -0.0059 0.3031 0.8067 0.086 Uiso 0.644(13) 1 calc PR E 1 H20D H -0.1099 0.2653 0.8222 0.086 Uiso 0.644(13) 1 calc PR E 1 C21' C -0.1605(10) 0.3367(5) 0.7915(3) 0.071(2) Uani 0.644(13) 1 d PD E 1 H21C H -0.1184 0.3735 0.7897 0.086 Uiso 0.644(13) 1 calc PR E 1 H21D H -0.2177 0.3406 0.8115 0.086 Uiso 0.644(13) 1 calc PR E 1 C22' C -0.2181(10) 0.3234(5) 0.7536(2) 0.071(2) Uani 0.644(13) 1 d PD E 1 H22C H -0.2873 0.3002 0.7567 0.086 Uiso 0.644(13) 1 calc PR E 1 H22D H -0.2348 0.3589 0.7390 0.086 Uiso 0.644(13) 1 calc PR E 1 C23' C -0.1224(10) 0.2886(6) 0.7365(3) 0.071(2) Uani 0.644(13) 1 d PD E 1 H23C H -0.1503 0.2646 0.7154 0.086 Uiso 0.644(13) 1 calc PR E 1 H23D H -0.0630 0.3147 0.7269 0.086 Uiso 0.644(13) 1 calc PR E 1 C24 C 0.1000(3) 0.14789(15) 0.91300(10) 0.0265(8) Uani 1 1 d . B . C25 C 0.0631(3) 0.14160(17) 0.95347(10) 0.0345(9) Uani 1 1 d . . . C26 C 0.0618(3) 0.08760(18) 0.97062(11) 0.0447(11) Uani 1 1 d . . . H26 H 0.0813 0.0542 0.9565 0.054 Uiso 1 1 calc R . . C27 C 0.0325(4) 0.0819(2) 1.00796(13) 0.0659(15) Uani 1 1 d . . . H27 H 0.0342 0.0449 1.0195 0.079 Uiso 1 1 calc R . . C28 C 0.0011(5) 0.1293(2) 1.02838(13) 0.0698(16) Uani 1 1 d . . . H28 H -0.0205 0.1251 1.0539 0.084 Uiso 1 1 calc R . . C29 C 0.0009(4) 0.1825(2) 1.01196(12) 0.0549(13) Uani 1 1 d . . . H29 H -0.0206 0.2153 1.0264 0.066 Uiso 1 1 calc R . . C30 C 0.0309(3) 0.18970(17) 0.97504(11) 0.0400(10) Uani 1 1 d . . . H30 H 0.0300 0.2272 0.9641 0.048 Uiso 1 1 calc R . . C31 C -0.0138(3) 0.06829(16) 0.88934(10) 0.0337(9) Uani 1 1 d . . . C32 C -0.1272(3) 0.08609(18) 0.89642(11) 0.0392(10) Uani 1 1 d . . . C33 C -0.1608(3) 0.14901(19) 0.90168(13) 0.0504(12) Uani 1 1 d . . . H33 H -0.0905 0.1728 0.9019 0.060 Uiso 1 1 calc R . . C34 C -0.2210(4) 0.1587(2) 0.93887(14) 0.0713(16) Uani 1 1 d . . . H34A H -0.2409 0.1997 0.9413 0.107 Uiso 1 1 calc R . . H34B H -0.1715 0.1475 0.9597 0.107 Uiso 1 1 calc R . . H34C H -0.2895 0.1352 0.9396 0.107 Uiso 1 1 calc R . . C35 C -0.2349(4) 0.1704(2) 0.86887(15) 0.0691(15) Uani 1 1 d . . . H35A H -0.2544 0.2111 0.8729 0.104 Uiso 1 1 calc R . . H35B H -0.3038 0.1472 0.8677 0.104 Uiso 1 1 calc R . . H35C H -0.1936 0.1665 0.8452 0.104 Uiso 1 1 calc R . . C36 C -0.2101(4) 0.0444(2) 0.89724(13) 0.0553(13) Uani 1 1 d . . . H36 H -0.2852 0.0558 0.9025 0.066 Uiso 1 1 calc R . . C37 C -0.1877(4) -0.0125(2) 0.89082(14) 0.0591(13) Uani 1 1 d . . . H37 H -0.2462 -0.0403 0.8925 0.071 Uiso 1 1 calc R . . C38 C -0.0802(4) -0.02974(18) 0.88194(12) 0.0466(11) Uani 1 1 d . . . H38 H -0.0661 -0.0694 0.8766 0.056 Uiso 1 1 calc R . . C39 C 0.0082(3) 0.00944(16) 0.88059(10) 0.0347(9) Uani 1 1 d . . . C40 C 0.1239(3) -0.01107(16) 0.87017(11) 0.0369(9) Uani 1 1 d . . . H40 H 0.1632 0.0229 0.8587 0.044 Uiso 1 1 calc R . . C41 C 0.1225(4) -0.0582(2) 0.84011(16) 0.0713(16) Uani 1 1 d . . . H41A H 0.0775 -0.0453 0.8186 0.107 Uiso 1 1 calc R . . H41B H 0.0897 -0.0936 0.8506 0.107 Uiso 1 1 calc R . . H41C H 0.1996 -0.0661 0.8318 0.107 Uiso 1 1 calc R . . C42 C 0.1925(4) -0.0287(2) 0.90353(15) 0.0720(16) Uani 1 1 d . . . H42A H 0.2670 -0.0414 0.8951 0.108 Uiso 1 1 calc R . . H42B H 0.1549 -0.0605 0.9167 0.108 Uiso 1 1 calc R . . H42C H 0.2007 0.0043 0.9206 0.108 Uiso 1 1 calc R . . C43 C 0.2066(3) 0.23604(16) 0.92527(10) 0.0312(9) Uani 1 1 d . . . C44 C 0.1682(3) 0.29306(16) 0.91946(12) 0.0405(10) Uani 1 1 d . . . C45 C 0.0823(4) 0.30709(18) 0.89016(13) 0.0561(13) Uani 1 1 d . . . H45 H 0.0864 0.2760 0.8707 0.067 Uiso 1 1 calc R . . C46 C -0.0359(5) 0.3074(3) 0.90516(16) 0.0824(17) Uani 1 1 d . . . H46A H -0.0884 0.3161 0.8847 0.124 Uiso 1 1 calc R . . H46B H -0.0427 0.3369 0.9248 0.124 Uiso 1 1 calc R . . H46C H -0.0536 0.2694 0.9158 0.124 Uiso 1 1 calc R . . C47 C 0.1042(5) 0.3654(2) 0.86993(16) 0.0849(18) Uani 1 1 d . . . H47A H 0.0459 0.3718 0.8509 0.127 Uiso 1 1 calc R . . H47B H 0.1780 0.3642 0.8577 0.127 Uiso 1 1 calc R . . H47C H 0.1026 0.3969 0.8883 0.127 Uiso 1 1 calc R . . C48 C 0.2095(5) 0.33628(19) 0.94264(14) 0.0614(14) Uani 1 1 d . . . H48 H 0.1822 0.3746 0.9396 0.074 Uiso 1 1 calc R . . C49 C 0.2879(4) 0.3256(2) 0.96964(14) 0.0606(13) Uani 1 1 d . . . H49 H 0.3137 0.3562 0.9853 0.073 Uiso 1 1 calc R . . C50 C 0.3295(3) 0.27114(19) 0.97417(12) 0.0476(11) Uani 1 1 d . . . H50 H 0.3859 0.2644 0.9926 0.057 Uiso 1 1 calc R . . C51 C 0.2908(3) 0.22512(16) 0.95232(11) 0.0355(9) Uani 1 1 d . . . C52 C 0.3419(3) 0.16590(18) 0.95917(11) 0.0410(10) Uani 1 1 d . . . H52 H 0.3022 0.1377 0.9425 0.049 Uiso 1 1 calc R . . C53 C 0.4651(3) 0.1654(2) 0.94852(15) 0.0650(14) Uani 1 1 d . . . H53A H 0.4962 0.1267 0.9528 0.097 Uiso 1 1 calc R . . H53B H 0.5058 0.1936 0.9639 0.097 Uiso 1 1 calc R . . H53C H 0.4730 0.1755 0.9219 0.097 Uiso 1 1 calc R . . C54 C 0.3267(4) 0.1456(2) 0.99976(12) 0.0572(12) Uani 1 1 d . . . H54A H 0.3601 0.1071 1.0028 0.086 Uiso 1 1 calc R . . H54B H 0.2464 0.1438 1.0057 0.086 Uiso 1 1 calc R . . H54C H 0.3638 0.1729 1.0168 0.086 Uiso 1 1 calc R . . C55 C 0.0991(3) 0.19261(15) 0.67919(11) 0.0302(9) Uani 1 1 d . . . C56 C 0.1309(3) 0.20551(17) 0.63951(11) 0.0341(9) Uani 1 1 d . . . C57 C 0.1269(3) 0.16430(19) 0.61155(11) 0.0451(11) Uani 1 1 d . . . H57 H 0.1037 0.1261 0.6176 0.054 Uiso 1 1 calc R . . C58 C 0.1561(4) 0.1776(2) 0.57478(13) 0.0594(13) Uani 1 1 d . . . H58 H 0.1536 0.1487 0.5558 0.071 Uiso 1 1 calc R . . C59 C 0.1887(4) 0.2330(3) 0.56612(14) 0.0622(14) Uani 1 1 d . . . H59 H 0.2087 0.2426 0.5410 0.075 Uiso 1 1 calc R . . C60 C 0.1926(4) 0.2743(2) 0.59332(14) 0.0620(14) Uani 1 1 d . . . H60 H 0.2147 0.3126 0.5871 0.074 Uiso 1 1 calc R . . C61 C 0.1648(3) 0.26076(19) 0.62986(12) 0.0447(11) Uani 1 1 d . . . H61 H 0.1689 0.2898 0.6487 0.054 Uiso 1 1 calc R . . C62 C -0.0661(3) 0.13613(18) 0.66212(11) 0.0398(10) Uani 1 1 d . . . C63 C -0.0681(4) 0.07495(19) 0.65944(12) 0.0484(11) Uani 1 1 d . . . C64 C 0.0127(4) 0.03741(19) 0.68128(14) 0.0579(13) Uani 1 1 d . . . H64 H 0.0515 0.0627 0.7000 0.070 Uiso 1 1 calc R . . C65 C 0.1022(5) 0.0108(2) 0.65668(17) 0.0851(17) Uani 1 1 d . . . H65A H 0.1527 -0.0128 0.6722 0.128 Uiso 1 1 calc R . . H65B H 0.1454 0.0415 0.6443 0.128 Uiso 1 1 calc R . . H65C H 0.0667 -0.0137 0.6376 0.128 Uiso 1 1 calc R . . C66 C -0.0461(5) -0.0102(2) 0.70297(15) 0.0716(15) Uani 1 1 d . . . H66A H 0.0096 -0.0330 0.7168 0.107 Uiso 1 1 calc R . . H66B H -0.0865 -0.0354 0.6854 0.107 Uiso 1 1 calc R . . H66C H -0.0996 0.0069 0.7207 0.107 Uiso 1 1 calc R . . C67 C -0.1461(5) 0.0496(2) 0.63563(15) 0.0719(16) Uani 1 1 d . . . H67 H -0.1481 0.0086 0.6337 0.086 Uiso 1 1 calc R . . C68 C -0.2197(5) 0.0814(3) 0.61493(17) 0.0861(18) Uani 1 1 d . . . H68 H -0.2728 0.0628 0.5991 0.103 Uiso 1 1 calc R . . C69 C -0.2169(4) 0.1407(3) 0.61707(14) 0.0704(15) Uani 1 1 d . . . H69 H -0.2682 0.1624 0.6022 0.085 Uiso 1 1 calc R . . C70 C -0.1417(3) 0.1702(2) 0.64012(11) 0.0458(11) Uani 1 1 d . . . C71 C -0.1438(3) 0.23515(19) 0.64075(12) 0.0466(11) Uani 1 1 d . . . H71 H -0.0851 0.2488 0.6588 0.056 Uiso 1 1 calc R . . C72 C -0.2567(4) 0.2581(2) 0.65357(14) 0.0687(15) Uani 1 1 d . . . H72A H -0.2546 0.3005 0.6540 0.103 Uiso 1 1 calc R . . H72B H -0.2731 0.2436 0.6789 0.103 Uiso 1 1 calc R . . H72C H -0.3153 0.2452 0.6361 0.103 Uiso 1 1 calc R . . C73 C -0.1176(4) 0.2605(2) 0.60216(12) 0.0588(13) Uani 1 1 d . . . H73A H -0.1191 0.3028 0.6036 0.088 Uiso 1 1 calc R . . H73B H -0.1739 0.2473 0.5840 0.088 Uiso 1 1 calc R . . H73C H -0.0428 0.2477 0.5941 0.088 Uiso 1 1 calc R . . C74 C 0.2638(3) 0.23859(15) 0.70545(10) 0.0297(9) Uani 1 1 d . . . C75 C 0.2782(3) 0.29590(16) 0.71864(11) 0.0357(9) Uani 1 1 d . . . C76 C 0.1828(4) 0.33126(17) 0.73384(13) 0.0481(11) Uani 1 1 d . . . H76 H 0.1165 0.3050 0.7366 0.058 Uiso 1 1 calc R . . C77 C 0.1490(6) 0.3801(3) 0.70739(17) 0.100(2) Uani 1 1 d . . . H77A H 0.0859 0.4015 0.7183 0.150 Uiso 1 1 calc R . . H77B H 0.1263 0.3638 0.6831 0.150 Uiso 1 1 calc R . . H77C H 0.2128 0.4062 0.7038 0.150 Uiso 1 1 calc R . . C78 C 0.2086(5) 0.3561(2) 0.77235(15) 0.0866(18) Uani 1 1 d . . . H78A H 0.1437 0.3783 0.7813 0.130 Uiso 1 1 calc R . . H78B H 0.2742 0.3816 0.7707 0.130 Uiso 1 1 calc R . . H78C H 0.2244 0.3246 0.7900 0.130 Uiso 1 1 calc R . . C79 C 0.3844(4) 0.32062(18) 0.71666(13) 0.0467(11) Uani 1 1 d . . . H79 H 0.3959 0.3588 0.7257 0.056 Uiso 1 1 calc R . . C80 C 0.4728(4) 0.2904(2) 0.70180(14) 0.0564(13) Uani 1 1 d . . . H80 H 0.5438 0.3087 0.6992 0.068 Uiso 1 1 calc R . . C81 C 0.4605(3) 0.23507(19) 0.69089(13) 0.0484(11) Uani 1 1 d . . . H81 H 0.5239 0.2144 0.6818 0.058 Uiso 1 1 calc R . . C82 C 0.3565(3) 0.20751(16) 0.69267(11) 0.0346(9) Uani 1 1 d . . . C83 C 0.3536(3) 0.14351(16) 0.68261(11) 0.0375(10) Uani 1 1 d . . . H83 H 0.2741 0.1299 0.6849 0.045 Uiso 1 1 calc R . . C84 C 0.3929(4) 0.1323(2) 0.64193(13) 0.0562(12) Uani 1 1 d . . . H84A H 0.3888 0.0908 0.6365 0.084 Uiso 1 1 calc R . . H84B H 0.4706 0.1456 0.6390 0.084 Uiso 1 1 calc R . . H84C H 0.3443 0.1534 0.6244 0.084 Uiso 1 1 calc R . . C85 C 0.4251(4) 0.10812(19) 0.70964(13) 0.0556(12) Uani 1 1 d . . . H85A H 0.4212 0.0672 0.7027 0.083 Uiso 1 1 calc R . . H85B H 0.3969 0.1131 0.7353 0.083 Uiso 1 1 calc R . . H85C H 0.5033 0.1213 0.7083 0.083 Uiso 1 1 calc R . . N1 N 0.0766(2) 0.10893(12) 0.88700(8) 0.0273(7) Uani 1 1 d . B . N2 N 0.1638(2) 0.19203(12) 0.90134(8) 0.0281(7) Uani 1 1 d . B . N3 N 0.0084(2) 0.16141(12) 0.68885(8) 0.0306(7) Uani 1 1 d . . . N4 N 0.1552(2) 0.21383(12) 0.70869(8) 0.0276(7) Uani 1 1 d . . . N5 N 0.2526(2) 0.08456(12) 0.80590(9) 0.0330(7) Uani 1 1 d . B . O1 O 0.3491(2) 0.21231(11) 0.83265(7) 0.0417(7) Uani 1 1 d . B . O2 O -0.1219(2) 0.10950(11) 0.76190(7) 0.0411(7) Uani 1 1 d . B . O3 O -0.0797(2) 0.25304(11) 0.76569(8) 0.0457(7) Uani 1 1 d . . . Y1 Y 0.17680(3) 0.156734(14) 0.836401(10) 0.02679(11) Uani 1 1 d . . . Y2 Y 0.04016(3) 0.172099(15) 0.757232(10) 0.02740(11) Uani 1 1 d . B . H1 H 0.021(3) 0.1703(17) 0.8162(12) 0.065(13) Uiso 1 1 d . . . H3A H 0.116(3) 0.0649(17) 0.7714(11) 0.052(12) Uiso 1 1 d . . . H3B H 0.208(4) 0.106(2) 0.7531(8) 0.099(18) Uiso 1 1 d D . . H2 H 0.158(4) 0.223(2) 0.7900(14) 0.095(16) 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 C3 0.034(2) 0.039(2) 0.026(2) 0.0007(18) -0.0010(18) 0.0021(19) C4 0.028(2) 0.029(2) 0.037(2) 0.0041(17) 0.0076(17) 0.0020(17) C5 0.039(2) 0.031(2) 0.040(3) -0.0019(18) 0.0025(18) 0.0003(18) C6 0.073(3) 0.037(2) 0.045(3) -0.013(2) 0.002(2) 0.004(2) C7 0.060(3) 0.036(2) 0.059(3) -0.008(2) 0.004(2) 0.014(2) C8 0.052(3) 0.057(3) 0.065(3) -0.005(3) -0.009(2) 0.029(2) C9 0.050(3) 0.053(3) 0.052(3) -0.001(2) -0.005(2) 0.015(2) C10 0.033(2) 0.034(2) 0.036(2) 0.0036(18) -0.0009(17) 0.0060(17) C11 0.043(3) 0.053(3) 0.038(3) 0.000(2) -0.0113(19) 0.013(2) C12 0.049(3) 0.077(3) 0.042(3) -0.006(2) 0.008(2) -0.016(2) C13 0.045(3) 0.129(5) 0.072(4) -0.005(4) 0.004(3) -0.025(3) C14 0.083(6) 0.071(8) 0.111(11) -0.022(6) 0.047(7) -0.053(6) C14' 0.083(6) 0.071(8) 0.111(11) -0.022(6) 0.047(7) -0.053(6) C15 0.056(3) 0.060(3) 0.071(4) -0.018(3) 0.017(3) -0.022(2) C16 0.042(3) 0.045(2) 0.042(3) 0.005(2) -0.0018(19) -0.008(2) C17 0.048(3) 0.078(4) 0.082(4) 0.026(3) -0.002(3) -0.019(3) C18 0.045(4) 0.120(15) 0.057(11) 0.023(7) -0.024(8) -0.036(8) C18' 0.045(4) 0.120(15) 0.057(11) 0.023(7) -0.024(8) -0.036(8) C19 0.032(3) 0.085(4) 0.052(3) 0.019(3) -0.014(2) -0.003(2) C20 0.078(5) 0.076(4) 0.0605(19) 0.000(2) -0.002(3) 0.036(4) C21 0.078(5) 0.076(4) 0.0605(19) 0.000(2) -0.002(3) 0.036(4) C22 0.078(5) 0.076(4) 0.0605(19) 0.000(2) -0.002(3) 0.036(4) C23 0.078(5) 0.076(4) 0.0605(19) 0.000(2) -0.002(3) 0.036(4) C20' 0.078(5) 0.076(4) 0.0605(19) 0.000(2) -0.002(3) 0.036(4) C21' 0.078(5) 0.076(4) 0.0605(19) 0.000(2) -0.002(3) 0.036(4) C22' 0.078(5) 0.076(4) 0.0605(19) 0.000(2) -0.002(3) 0.036(4) C23' 0.078(5) 0.076(4) 0.0605(19) 0.000(2) -0.002(3) 0.036(4) C24 0.023(2) 0.033(2) 0.024(2) 0.0008(16) 0.0004(15) 0.0016(16) C25 0.033(2) 0.044(2) 0.026(2) -0.0010(18) 0.0000(16) -0.0086(18) C26 0.062(3) 0.043(3) 0.029(2) -0.0006(19) 0.002(2) -0.010(2) C27 0.101(4) 0.063(3) 0.034(3) 0.010(2) 0.008(3) -0.032(3) C28 0.105(4) 0.079(4) 0.025(3) -0.018(3) 0.020(3) -0.037(3) C29 0.061(3) 0.063(3) 0.040(3) -0.015(2) 0.019(2) -0.017(2) C30 0.042(2) 0.043(2) 0.035(2) -0.0069(19) 0.0044(19) -0.0046(19) C31 0.035(2) 0.045(2) 0.022(2) -0.0010(17) 0.0000(16) -0.0070(18) C32 0.027(2) 0.054(3) 0.037(2) -0.008(2) -0.0011(18) -0.0033(19) C33 0.026(2) 0.060(3) 0.065(3) -0.018(2) 0.002(2) 0.002(2) C34 0.046(3) 0.099(4) 0.069(4) -0.031(3) 0.014(3) 0.004(3) C35 0.052(3) 0.070(3) 0.085(4) -0.009(3) -0.012(3) 0.010(3) C36 0.032(3) 0.076(4) 0.058(3) -0.004(3) 0.008(2) -0.011(2) C37 0.045(3) 0.065(3) 0.068(3) -0.006(3) 0.004(2) -0.028(2) C38 0.044(3) 0.045(3) 0.051(3) -0.006(2) -0.001(2) -0.012(2) C39 0.039(2) 0.035(2) 0.029(2) 0.0033(17) -0.0021(17) -0.0053(18) C40 0.041(2) 0.031(2) 0.039(2) 0.0004(18) 0.0048(19) -0.0027(18) C41 0.060(3) 0.064(3) 0.090(4) -0.028(3) 0.019(3) -0.006(3) C42 0.044(3) 0.100(4) 0.072(4) 0.032(3) 0.009(3) 0.016(3) C43 0.040(2) 0.035(2) 0.019(2) -0.0028(16) 0.0024(16) -0.0085(17) C44 0.055(3) 0.028(2) 0.039(3) -0.0028(19) 0.005(2) -0.0054(19) C45 0.083(4) 0.039(3) 0.047(3) -0.004(2) -0.007(3) 0.015(2) C46 0.081(4) 0.092(4) 0.074(4) 0.021(3) -0.021(3) 0.006(3) C47 0.113(5) 0.077(4) 0.064(4) 0.025(3) -0.008(3) 0.014(3) C48 0.100(4) 0.035(3) 0.050(3) -0.002(2) 0.003(3) 0.006(3) C49 0.092(4) 0.042(3) 0.047(3) -0.009(2) -0.004(3) -0.019(3) C50 0.045(3) 0.056(3) 0.041(3) -0.009(2) -0.006(2) -0.011(2) C51 0.037(2) 0.040(2) 0.030(2) -0.0012(18) 0.0028(18) -0.0058(18) C52 0.030(2) 0.059(3) 0.033(2) -0.013(2) -0.0091(17) -0.0050(19) C53 0.032(3) 0.087(4) 0.076(4) -0.024(3) -0.016(2) 0.002(2) C54 0.059(3) 0.067(3) 0.046(3) -0.004(2) -0.021(2) 0.003(2) C55 0.027(2) 0.031(2) 0.033(2) 0.0062(17) -0.0013(17) 0.0043(16) C56 0.024(2) 0.051(3) 0.028(2) 0.0081(19) -0.0015(16) -0.0017(18) C57 0.037(2) 0.062(3) 0.036(3) 0.007(2) -0.0003(18) -0.004(2) C58 0.054(3) 0.092(4) 0.032(3) -0.002(3) 0.005(2) 0.007(3) C59 0.050(3) 0.103(4) 0.034(3) 0.029(3) 0.006(2) -0.002(3) C60 0.054(3) 0.080(4) 0.051(3) 0.032(3) -0.001(2) -0.014(3) C61 0.043(3) 0.059(3) 0.033(2) 0.016(2) -0.0014(19) -0.005(2) C62 0.036(2) 0.055(3) 0.029(2) 0.0091(19) -0.0050(18) -0.019(2) C63 0.052(3) 0.053(3) 0.040(3) 0.005(2) -0.014(2) -0.017(2) C64 0.081(4) 0.043(3) 0.050(3) -0.005(2) -0.010(3) -0.012(2) C65 0.090(4) 0.082(4) 0.084(5) 0.018(3) -0.001(3) -0.011(3) C66 0.099(4) 0.049(3) 0.067(4) -0.002(3) 0.012(3) -0.007(3) C67 0.091(4) 0.064(3) 0.060(4) -0.004(3) -0.024(3) -0.034(3) C68 0.074(4) 0.097(5) 0.088(5) 0.005(4) -0.043(3) -0.031(4) C69 0.050(3) 0.107(5) 0.054(3) 0.016(3) -0.020(2) -0.020(3) C70 0.035(2) 0.076(3) 0.027(2) 0.008(2) -0.0089(18) -0.012(2) C71 0.034(2) 0.067(3) 0.039(3) 0.012(2) -0.0042(19) 0.002(2) C72 0.034(3) 0.109(4) 0.063(4) 0.023(3) 0.002(2) 0.012(3) C73 0.044(3) 0.088(4) 0.044(3) 0.021(3) -0.003(2) 0.005(2) C74 0.027(2) 0.032(2) 0.029(2) 0.0136(17) -0.0031(16) -0.0031(17) C75 0.041(2) 0.034(2) 0.033(2) 0.0093(18) -0.0038(18) -0.0033(18) C76 0.048(3) 0.031(2) 0.066(3) 0.002(2) 0.000(2) -0.004(2) C77 0.132(6) 0.090(4) 0.078(4) 0.010(3) -0.002(4) 0.066(4) C78 0.107(5) 0.089(4) 0.065(4) -0.013(3) 0.007(3) 0.035(4) C79 0.046(3) 0.036(2) 0.059(3) 0.003(2) -0.003(2) -0.012(2) C80 0.040(3) 0.065(3) 0.064(3) 0.005(3) 0.000(2) -0.024(2) C81 0.032(2) 0.051(3) 0.062(3) 0.006(2) 0.001(2) -0.006(2) C82 0.030(2) 0.043(2) 0.030(2) 0.0084(18) 0.0007(17) -0.0026(18) C83 0.028(2) 0.043(2) 0.042(3) 0.0031(19) 0.0011(18) 0.0009(18) C84 0.052(3) 0.065(3) 0.051(3) -0.002(2) 0.006(2) 0.007(2) C85 0.055(3) 0.054(3) 0.058(3) 0.009(2) -0.002(2) 0.011(2) N1 0.0269(17) 0.0292(16) 0.0257(17) -0.0019(13) -0.0023(13) -0.0017(13) N2 0.0310(18) 0.0314(17) 0.0221(17) -0.0009(13) -0.0016(13) -0.0003(14) N3 0.0254(17) 0.0418(19) 0.0246(17) 0.0057(14) -0.0043(13) -0.0092(14) N4 0.0252(17) 0.0317(17) 0.0260(18) 0.0038(13) -0.0027(13) -0.0039(13) N5 0.0364(19) 0.0319(17) 0.0307(19) 0.0017(14) -0.0027(14) 0.0036(14) O1 0.0379(16) 0.0513(17) 0.0360(17) -0.0044(13) 0.0050(12) -0.0100(13) O2 0.0354(16) 0.0476(17) 0.0403(17) 0.0111(13) -0.0055(12) -0.0069(12) O3 0.0532(19) 0.0440(17) 0.0400(18) 0.0027(13) 0.0007(14) 0.0158(13) Y1 0.0269(2) 0.0303(2) 0.0232(2) -0.00019(15) -0.00049(14) 0.00051(15) Y2 0.0262(2) 0.0323(2) 0.0237(2) 0.00259(15) -0.00138(14) 0.00049(15) _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 C3 N5 1.446(5) . ? C3 Y2 2.433(4) . ? C3 Y1 2.521(4) . ? C3 H3A 0.99(4) . ? C3 H3B 0.992(10) . ? C4 N5 1.376(4) . ? C4 C5 1.415(5) . ? C4 C10 1.428(5) . ? C5 C7 1.376(5) . ? C5 C6 1.526(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.383(6) . ? C7 H7 0.9500 . ? C8 C9 1.385(6) . ? C8 H8 0.9500 . ? C9 C10 1.366(5) . ? C9 H9 0.9500 . ? C10 C11 1.492(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 O1 1.451(5) . ? C12 C13 1.480(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14' 1.473(11) . ? C13 C14 1.56(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.42(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14' C15 1.503(12) . ? C14' H14C 0.9900 . ? C14' H14D 0.9900 . ? C15 O1 1.442(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O2 1.456(4) . ? C16 C17 1.473(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.38(3) . ? C17 C18' 1.452(19) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.50(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C18' C19 1.483(19) . ? C18' H18C 0.9900 . ? C18' H18D 0.9900 . ? C19 O2 1.440(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O3 1.43(2) . ? C20 C21 1.485(13) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.577(16) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.547(16) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O3 1.46(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C20' O3 1.486(11) . ? C20' C21' 1.496(9) . ? C20' H20C 0.9900 . ? C20' H20D 0.9900 . ? C21' C22' 1.542(11) . ? C21' H21C 0.9900 . ? C21' H21D 0.9900 . ? C22' C23' 1.520(11) . ? C22' H22C 0.9900 . ? C22' H22D 0.9900 . ? C23' O3 1.418(13) . ? C23' H23C 0.9900 . ? C23' H23D 0.9900 . ? C24 N1 1.321(4) . ? C24 N2 1.338(4) . ? C24 C25 1.512(5) . ? C24 Y1 2.881(3) . ? C25 C26 1.390(5) . ? C25 C30 1.404(5) . ? C26 C27 1.379(6) . ? C26 H26 0.9500 . ? C27 C28 1.366(6) . ? C27 H27 0.9500 . ? C28 C29 1.362(7) . ? C28 H28 0.9500 . ? C29 C30 1.371(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C39 1.420(5) . ? C31 N1 1.430(4) . ? C31 C32 1.434(5) . ? C32 C36 1.379(6) . ? C32 C33 1.520(6) . ? C33 C34 1.521(6) . ? C33 C35 1.544(7) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.361(6) . ? C36 H36 0.9500 . ? C37 C38 1.377(6) . ? C37 H37 0.9500 . ? C38 C39 1.389(5) . ? C38 H38 0.9500 . ? C39 C40 1.503(5) . ? C40 C42 1.496(6) . ? C40 C41 1.527(6) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.410(5) . ? C43 C51 1.411(5) . ? C43 N2 1.421(4) . ? C44 C48 1.385(6) . ? C44 C45 1.495(6) . ? C45 C46 1.504(7) . ? C45 C47 1.549(7) . ? C45 H45 1.0000 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.361(7) . ? C48 H48 0.9500 . ? C49 C50 1.363(6) . ? C49 H49 0.9500 . ? C50 C51 1.396(5) . ? C50 H50 0.9500 . ? C51 C52 1.518(5) . ? C52 C53 1.514(5) . ? C52 C54 1.529(6) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 N4 1.336(5) . ? C55 N3 1.343(4) . ? C55 C56 1.491(5) . ? C55 Y2 2.902(4) . ? C56 C57 1.378(5) . ? C56 C61 1.383(5) . ? C57 C58 1.388(6) . ? C57 H57 0.9500 . ? C58 C59 1.374(7) . ? C58 H58 0.9500 . ? C59 C60 1.359(7) . ? C59 H59 0.9500 . ? C60 C61 1.377(6) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 C63 1.418(6) . ? C62 N3 1.425(5) . ? C62 C70 1.428(6) . ? C63 C67 1.386(6) . ? C63 C64 1.510(6) . ? C64 C65 1.510(7) . ? C64 C66 1.516(6) . ? C64 H64 1.0000 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C68 1.361(7) . ? C67 H67 0.9500 . ? C68 C69 1.373(7) . ? C68 H68 0.9500 . ? C69 C70 1.392(6) . ? C69 H69 0.9500 . ? C70 C71 1.503(6) . ? C71 C72 1.515(6) . ? C71 C73 1.525(6) . ? C71 H71 1.0000 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 C82 1.393(5) . ? C74 C75 1.416(5) . ? C74 N4 1.418(4) . ? C75 C79 1.389(5) . ? C75 C76 1.500(5) . ? C76 C78 1.517(7) . ? C76 C77 1.523(6) . ? C76 H76 1.0000 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 C80 1.369(6) . ? C79 H79 0.9500 . ? C80 C81 1.345(6) . ? C80 H80 0.9500 . ? C81 C82 1.393(5) . ? C81 H81 0.9500 . ? C82 C83 1.523(5) . ? C83 C85 1.523(6) . ? C83 C84 1.543(5) . ? C83 H83 1.0000 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? N1 Y1 2.426(3) . ? N2 Y1 2.454(3) . ? N3 Y2 2.473(3) . ? N4 Y2 2.406(3) . ? N5 Y1 2.186(3) . ? O1 Y1 2.423(2) . ? O2 Y2 2.417(2) . ? O3 Y2 2.373(3) . ? Y1 Y2 3.2699(8) . ? Y1 H1 2.02(4) . ? Y1 H2 2.26(5) . ? Y2 H1 2.11(4) . ? Y2 H3B 2.52(5) . ? Y2 H2 2.17(5) . ? 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 N5 C3 Y2 141.1(3) . . ? N5 C3 Y1 59.78(18) . . ? Y2 C3 Y1 82.60(12) . . ? N5 C3 H3A 116(2) . . ? Y2 C3 H3A 94(2) . . ? Y1 C3 H3A 127(2) . . ? N5 C3 H3B 110(3) . . ? Y2 C3 H3B 84(3) . . ? Y1 C3 H3B 126(3) . . ? H3A C3 H3B 105(4) . . ? N5 C4 C5 127.9(4) . . ? N5 C4 C10 115.0(3) . . ? C5 C4 C10 117.0(3) . . ? C7 C5 C4 119.1(4) . . ? C7 C5 C6 116.5(4) . . ? C4 C5 C6 124.3(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 C8 123.6(4) . . ? C5 C7 H7 118.2 . . ? C8 C7 H7 118.2 . . ? C7 C8 C9 117.4(4) . . ? C7 C8 H8 121.3 . . ? C9 C8 H8 121.3 . . ? C10 C9 C8 121.5(4) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C4 121.3(4) . . ? C9 C10 C11 119.0(4) . . ? C4 C10 C11 119.7(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 . . ? O1 C12 C13 105.9(4) . . ? O1 C12 H12A 110.6 . . ? C13 C12 H12A 110.6 . . ? O1 C12 H12B 110.6 . . ? C13 C12 H12B 110.6 . . ? H12A C12 H12B 108.7 . . ? C14' C13 C12 103.7(5) . . ? C14' C13 C14 33.3(16) . . ? C12 C13 C14 104.3(11) . . ? C14' C13 H13A 111.0 . . ? C12 C13 H13A 111.0 . . ? C14 C13 H13A 80.4 . . ? C14' C13 H13B 111.0 . . ? C12 C13 H13B 111.0 . . ? C14 C13 H13B 136.2 . . ? H13A C13 H13B 109.0 . . ? C15 C14 C13 104(3) . . ? C15 C14 H14A 110.9 . . ? C13 C14 H14A 110.9 . . ? C15 C14 H14B 110.9 . . ? C13 C14 H14B 110.9 . . ? H14A C14 H14B 109.0 . . ? C13 C14' C15 104.4(8) . . ? C13 C14' H14C 110.9 . . ? C15 C14' H14C 110.9 . . ? C13 C14' H14D 110.9 . . ? C15 C14' H14D 110.9 . . ? H14C C14' H14D 108.9 . . ? C14 C15 O1 105.0(14) . . ? C14 C15 C14' 34.7(18) . . ? O1 C15 C14' 106.6(5) . . ? C14 C15 H15A 79.2 . . ? O1 C15 H15A 110.4 . . ? C14' C15 H15A 110.4 . . ? C14 C15 H15B 137.4 . . ? O1 C15 H15B 110.4 . . ? C14' C15 H15B 110.4 . . ? H15A C15 H15B 108.6 . . ? O2 C16 C17 106.5(3) . . ? O2 C16 H16A 110.4 . . ? C17 C16 H16A 110.4 . . ? O2 C16 H16B 110.4 . . ? C17 C16 H16B 110.4 . . ? H16A C16 H16B 108.6 . . ? C18 C17 C18' 31.5(10) . . ? C18 C17 C16 106.1(10) . . ? C18' C17 C16 108.1(8) . . ? C18 C17 H17A 135.3 . . ? C18' C17 H17A 110.1 . . ? C16 C17 H17A 110.1 . . ? C18 C17 H17B 82.2 . . ? C18' C17 H17B 110.1 . . ? C16 C17 H17B 110.1 . . ? H17A C17 H17B 108.4 . . ? C17 C18 C19 106.9(16) . . ? C17 C18 H18A 110.3 . . ? C19 C18 H18A 110.3 . . ? C17 C18 H18B 110.3 . . ? C19 C18 H18B 110.3 . . ? H18A C18 H18B 108.6 . . ? C17 C18' C19 104.2(11) . . ? C17 C18' H18C 110.9 . . ? C19 C18' H18C 110.9 . . ? C17 C18' H18D 110.9 . . ? C19 C18' H18D 110.9 . . ? H18C C18' H18D 108.9 . . ? O2 C19 C18' 108.0(8) . . ? O2 C19 C18 103.8(9) . . ? C18' C19 C18 30.0(9) . . ? O2 C19 H19A 110.1 . . ? C18' C19 H19A 110.1 . . ? C18 C19 H19A 135.8 . . ? O2 C19 H19B 110.1 . . ? C18' C19 H19B 110.1 . . ? C18 C19 H19B 84.7 . . ? H19A C19 H19B 108.4 . . ? O3 C20 C21 110.8(12) . . ? O3 C20 H20A 109.5 . . ? C21 C20 H20A 109.5 . . ? O3 C20 H20B 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? C20 C21 C22 96.9(13) . . ? C20 C21 H21A 112.4 . . ? C22 C21 H21A 112.4 . . ? C20 C21 H21B 112.4 . . ? C22 C21 H21B 112.4 . . ? H21A C21 H21B 109.9 . . ? C23 C22 C21 94.9(13) . . ? C23 C22 H22A 112.8 . . ? C21 C22 H22A 112.8 . . ? C23 C22 H22B 112.8 . . ? C21 C22 H22B 112.8 . . ? H22A C22 H22B 110.2 . . ? O3 C23 C22 98.5(15) . . ? O3 C23 H23A 112.1 . . ? C22 C23 H23A 112.1 . . ? O3 C23 H23B 112.1 . . ? C22 C23 H23B 112.1 . . ? H23A C23 H23B 109.7 . . ? O3 C20' C21' 103.7(6) . . ? O3 C20' H20C 111.0 . . ? C21' C20' H20C 111.0 . . ? O3 C20' H20D 111.0 . . ? C21' C20' H20D 111.0 . . ? H20C C20' H20D 109.0 . . ? C20' C21' C22' 108.6(7) . . ? C20' C21' H21C 110.0 . . ? C22' C21' H21C 110.0 . . ? C20' C21' H21D 110.0 . . ? C22' C21' H21D 110.0 . . ? H21C C21' H21D 108.3 . . ? C23' C22' C21' 97.0(9) . . ? C23' C22' H22C 112.4 . . ? C21' C22' H22C 112.4 . . ? C23' C22' H22D 112.4 . . ? C21' C22' H22D 112.4 . . ? H22C C22' H22D 109.9 . . ? O3 C23' C22' 106.4(9) . . ? O3 C23' H23C 110.4 . . ? C22' C23' H23C 110.4 . . ? O3 C23' H23D 110.4 . . ? C22' C23' H23D 110.4 . . ? H23C C23' H23D 108.6 . . ? N1 C24 N2 115.0(3) . . ? N1 C24 C25 122.6(3) . . ? N2 C24 C25 122.2(3) . . ? N1 C24 Y1 56.88(17) . . ? N2 C24 Y1 58.17(17) . . ? C25 C24 Y1 177.9(3) . . ? C26 C25 C30 117.9(4) . . ? C26 C25 C24 120.5(3) . . ? C30 C25 C24 121.6(3) . . ? C27 C26 C25 120.7(4) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C28 C27 C26 120.3(4) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C29 C28 C27 119.8(4) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 121.3(4) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C29 C30 C25 119.9(4) . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? C39 C31 N1 118.6(3) . . ? C39 C31 C32 119.1(3) . . ? N1 C31 C32 122.0(3) . . ? C36 C32 C31 118.5(4) . . ? C36 C32 C33 118.6(4) . . ? C31 C32 C33 122.9(3) . . ? C32 C33 C34 111.8(4) . . ? C32 C33 C35 111.3(4) . . ? C34 C33 C35 109.9(4) . . ? C32 C33 H33 107.9 . . ? C34 C33 H33 107.9 . . ? C35 C33 H33 107.9 . . ? 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 122.1(4) . . ? C37 C36 H36 118.9 . . ? C32 C36 H36 118.9 . . ? C36 C37 C38 120.1(4) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C37 C38 C39 121.5(4) . . ? C37 C38 H38 119.3 . . ? C39 C38 H38 119.3 . . ? C38 C39 C31 118.6(4) . . ? C38 C39 C40 119.8(3) . . ? C31 C39 C40 121.7(3) . . ? C42 C40 C39 113.0(3) . . ? C42 C40 C41 111.5(4) . . ? C39 C40 C41 112.9(3) . . ? C42 C40 H40 106.3 . . ? C39 C40 H40 106.3 . . ? C41 C40 H40 106.3 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C51 119.8(3) . . ? C44 C43 N2 117.8(3) . . ? C51 C43 N2 122.3(3) . . ? C48 C44 C43 118.2(4) . . ? C48 C44 C45 120.0(4) . . ? C43 C44 C45 121.8(4) . . ? C44 C45 C46 113.1(4) . . ? C44 C45 C47 113.4(4) . . ? C46 C45 C47 108.5(4) . . ? C44 C45 H45 107.1 . . ? C46 C45 H45 107.1 . . ? C47 C45 H45 107.1 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 C44 122.2(4) . . ? C49 C48 H48 118.9 . . ? C44 C48 H48 118.9 . . ? C48 C49 C50 119.9(4) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C49 C50 C51 121.3(4) . . ? C49 C50 H50 119.4 . . ? C51 C50 H50 119.4 . . ? C50 C51 C43 118.5(4) . . ? C50 C51 C52 117.8(4) . . ? C43 C51 C52 123.7(3) . . ? C53 C52 C51 110.8(3) . . ? C53 C52 C54 110.4(4) . . ? C51 C52 C54 112.4(3) . . ? C53 C52 H52 107.7 . . ? C51 C52 H52 107.7 . . ? C54 C52 H52 107.7 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N4 C55 N3 113.4(3) . . ? N4 C55 C56 122.9(3) . . ? N3 C55 C56 123.6(3) . . ? N4 C55 Y2 55.25(18) . . ? N3 C55 Y2 58.19(18) . . ? C56 C55 Y2 177.7(3) . . ? C57 C56 C61 118.0(4) . . ? C57 C56 C55 122.4(3) . . ? C61 C56 C55 119.6(4) . . ? C56 C57 C58 121.2(4) . . ? C56 C57 H57 119.4 . . ? C58 C57 H57 119.4 . . ? C59 C58 C57 119.3(5) . . ? C59 C58 H58 120.4 . . ? C57 C58 H58 120.4 . . ? C60 C59 C58 120.3(4) . . ? C60 C59 H59 119.9 . . ? C58 C59 H59 119.9 . . ? C59 C60 C61 120.3(5) . . ? C59 C60 H60 119.9 . . ? C61 C60 H60 119.9 . . ? C60 C61 C56 120.9(4) . . ? C60 C61 H61 119.5 . . ? C56 C61 H61 119.5 . . ? C63 C62 N3 117.7(4) . . ? C63 C62 C70 120.2(4) . . ? N3 C62 C70 122.0(4) . . ? C67 C63 C62 118.3(4) . . ? C67 C63 C64 119.8(4) . . ? C62 C63 C64 121.9(4) . . ? C65 C64 C63 112.7(4) . . ? C65 C64 C66 108.9(4) . . ? C63 C64 C66 112.6(4) . . ? C65 C64 H64 107.4 . . ? C63 C64 H64 107.4 . . ? C66 C64 H64 107.4 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C68 C67 C63 122.2(5) . . ? C68 C67 H67 118.9 . . ? C63 C67 H67 118.9 . . ? C67 C68 C69 119.6(5) . . ? C67 C68 H68 120.2 . . ? C69 C68 H68 120.2 . . ? C68 C69 C70 122.5(5) . . ? C68 C69 H69 118.7 . . ? C70 C69 H69 118.7 . . ? C69 C70 C62 117.2(4) . . ? C69 C70 C71 119.2(4) . . ? C62 C70 C71 123.6(4) . . ? C70 C71 C72 111.7(4) . . ? C70 C71 C73 111.6(4) . . ? C72 C71 C73 108.5(4) . . ? C70 C71 H71 108.3 . . ? C72 C71 H71 108.3 . . ? C73 C71 H71 108.3 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C71 C73 H73A 109.5 . . ? C71 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C71 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C82 C74 C75 119.7(3) . . ? C82 C74 N4 122.7(3) . . ? C75 C74 N4 117.4(3) . . ? C79 C75 C74 118.6(4) . . ? C79 C75 C76 118.9(4) . . ? C74 C75 C76 122.6(3) . . ? C75 C76 C78 112.3(4) . . ? C75 C76 C77 112.4(4) . . ? C78 C76 C77 109.3(4) . . ? C75 C76 H76 107.5 . . ? C78 C76 H76 107.5 . . ? C77 C76 H76 107.5 . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C76 C78 H78A 109.5 . . ? C76 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C76 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C80 C79 C75 120.6(4) . . ? C80 C79 H79 119.7 . . ? C75 C79 H79 119.7 . . ? C81 C80 C79 120.9(4) . . ? C81 C80 H80 119.6 . . ? C79 C80 H80 119.6 . . ? C80 C81 C82 121.3(4) . . ? C80 C81 H81 119.4 . . ? C82 C81 H81 119.4 . . ? C74 C82 C81 118.8(4) . . ? C74 C82 C83 124.1(3) . . ? C81 C82 C83 117.0(3) . . ? C85 C83 C82 111.2(3) . . ? C85 C83 C84 109.4(3) . . ? C82 C83 C84 112.1(3) . . ? C85 C83 H83 108.0 . . ? C82 C83 H83 108.0 . . ? C84 C83 H83 108.0 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C83 C85 H85A 109.5 . . ? C83 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C83 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C24 N1 C31 124.5(3) . . ? C24 N1 Y1 96.0(2) . . ? C31 N1 Y1 135.4(2) . . ? C24 N2 C43 124.3(3) . . ? C24 N2 Y1 94.2(2) . . ? C43 N2 Y1 141.2(2) . . ? C55 N3 C62 123.3(3) . . ? C55 N3 Y2 94.3(2) . . ? C62 N3 Y2 142.3(2) . . ? C55 N4 C74 122.6(3) . . ? C55 N4 Y2 97.6(2) . . ? C74 N4 Y2 137.6(2) . . ? C4 N5 C3 128.1(3) . . ? C4 N5 Y1 146.3(3) . . ? C3 N5 Y1 85.4(2) . . ? C15 O1 C12 108.1(3) . . ? C15 O1 Y1 135.7(2) . . ? C12 O1 Y1 114.5(2) . . ? C19 O2 C16 107.8(3) . . ? C19 O2 Y2 127.5(2) . . ? C16 O2 Y2 122.6(2) . . ? C23' O3 C20 106.9(8) . . ? C23' O3 C23 18.6(13) . . ? C20 O3 C23 102.7(11) . . ? C23' O3 C20' 106.8(6) . . ? C20 O3 C20' 21.8(11) . . ? C23 O3 C20' 109.7(7) . . ? C23' O3 Y2 125.4(4) . . ? C20 O3 Y2 127.6(7) . . ? C23 O3 Y2 126.9(6) . . ? C20' O3 Y2 123.2(4) . . ? N5 Y1 O1 91.60(10) . . ? N5 Y1 N1 102.92(10) . . ? O1 Y1 N1 134.32(9) . . ? N5 Y1 N2 138.34(10) . . ? O1 Y1 N2 85.93(9) . . ? N1 Y1 N2 54.71(9) . . ? N5 Y1 C3 34.86(11) . . ? O1 Y1 C3 105.90(11) . . ? N1 Y1 C3 110.60(12) . . ? N2 Y1 C3 165.00(11) . . ? N5 Y1 C24 123.12(10) . . ? O1 Y1 C24 110.99(9) . . ? N1 Y1 C24 27.13(9) . . ? N2 Y1 C24 27.59(9) . . ? C3 Y1 C24 137.68(12) . . ? N5 Y1 Y2 82.00(8) . . ? O1 Y1 Y2 108.38(7) . . ? N1 Y1 Y2 116.35(7) . . ? N2 Y1 Y2 137.95(7) . . ? C3 Y1 Y2 47.54(9) . . ? C24 Y1 Y2 131.62(7) . . ? N5 Y1 H1 108.8(11) . . ? O1 Y1 H1 132.6(11) . . ? N1 Y1 H1 83.2(12) . . ? N2 Y1 H1 103.0(12) . . ? C3 Y1 H1 75.9(11) . . ? C24 Y1 H1 93.2(12) . . ? Y2 Y1 H1 38.6(12) . . ? N5 Y1 H2 101.1(12) . . ? O1 Y1 H2 71.5(12) . . ? N1 Y1 H2 143.4(12) . . ? N2 Y1 H2 117.2(12) . . ? C3 Y1 H2 76.0(12) . . ? C24 Y1 H2 135.1(12) . . ? Y2 Y1 H2 41.3(12) . . ? H1 Y1 H2 62.9(16) . . ? O3 Y2 N4 96.72(9) . . ? O3 Y2 O2 89.07(9) . . ? N4 Y2 O2 138.05(10) . . ? O3 Y2 C3 155.35(12) . . ? N4 Y2 C3 97.87(12) . . ? O2 Y2 C3 93.23(12) . . ? O3 Y2 N3 96.42(10) . . ? N4 Y2 N3 54.63(9) . . ? O2 Y2 N3 83.46(9) . . ? C3 Y2 N3 108.23(11) . . ? O3 Y2 C55 97.93(10) . . ? N4 Y2 C55 27.16(9) . . ? O2 Y2 C55 110.90(10) . . ? C3 Y2 C55 104.11(11) . . ? N3 Y2 C55 27.48(9) . . ? O3 Y2 Y1 105.98(7) . . ? N4 Y2 Y1 112.25(7) . . ? O2 Y2 Y1 105.80(6) . . ? C3 Y2 Y1 49.86(9) . . ? N3 Y2 Y1 155.71(7) . . ? C55 Y2 Y1 136.14(7) . . ? O3 Y2 H1 79.8(11) . . ? N4 Y2 H1 141.6(11) . . ? O2 Y2 H1 80.3(11) . . ? C3 Y2 H1 76.4(11) . . ? N3 Y2 H1 163.4(11) . . ? C55 Y2 H1 168.6(11) . . ? Y1 Y2 H1 36.6(11) . . ? O3 Y2 H3B 164.5(12) . . ? N4 Y2 H3B 75.7(5) . . ? O2 Y2 H3B 105.6(10) . . ? C3 Y2 H3B 23.0(4) . . ? N3 Y2 H3B 90.2(8) . . ? C55 Y2 H3B 81.5(5) . . ? Y1 Y2 H3B 65.8(9) . . ? H1 Y2 H3B 97.6(12) . . ? O3 Y2 H2 84.0(13) . . ? N4 Y2 H2 78.5(13) . . ? O2 Y2 H2 143.5(13) . . ? C3 Y2 H2 79.5(13) . . ? N3 Y2 H2 132.9(13) . . ? C55 Y2 H2 105.6(13) . . ? Y1 Y2 H2 43.4(13) . . ? H1 Y2 H2 63.1(17) . . ? H3B Y2 H2 81.2(17) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.685 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.070 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 -0.185 0.402 0.000 1639 331 ' ' 2 -0.089 0.008 0.500 1639 331 ' ' _platon_squeeze_details ; Disorder solvents (one hexane and 2.5 toluene) per formual unit of [(PhNCN)YH]2(CH2NAr*)(THF)3 were not modelled and the disordered density was taken into account using the SQUEEZE/PLATON procedure. (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194?01) as implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst. 2003, 36, 7?3. PLATON - a multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands). ; data_4-Lu-a _database_code_depnum_ccdc_archive 'CCDC 859487' #TrackingRef '- Ln2H4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((Ph-NCN)2Lu2H3(THF)3)(PhCCHPh) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H116 Lu2 N4 O3' _chemical_formula_weight 1627.79 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' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.437(2) _cell_length_b 14.939(3) _cell_length_c 22.326(4) _cell_angle_alpha 107.399(3) _cell_angle_beta 102.549(3) _cell_angle_gamma 100.158(3) _cell_volume 4031.9(12) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Pale-Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1676 _exptl_absorpt_coefficient_mu 2.483 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5229 _exptl_absorpt_correction_T_max 0.5757 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 21877 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13956 _reflns_number_gt 9942 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0455P)^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 13956 _refine_ls_number_parameters 890 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1015 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _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 C4 C 0.6010(6) 0.3498(6) 0.3554(4) 0.057(2) Uani 1 1 d . . . C5 C 0.6492(5) 0.4430(5) 0.3674(3) 0.0419(16) Uani 1 1 d . . . C6 C 0.6991(6) 0.5019(5) 0.4390(4) 0.0531(19) Uani 1 1 d . . . C7 C 0.6790(6) 0.5902(6) 0.4660(4) 0.066(2) Uani 1 1 d . . . H7 H 0.6314 0.6119 0.4389 0.079 Uiso 1 1 calc R . . C8 C 0.7259(7) 0.6489(6) 0.5316(4) 0.078(3) Uani 1 1 d . . . H8 H 0.7063 0.7071 0.5493 0.093 Uiso 1 1 calc R . . C9 C 0.8012(7) 0.6221(6) 0.5709(4) 0.075(3) Uani 1 1 d . . . H9 H 0.8361 0.6629 0.6151 0.090 Uiso 1 1 calc R . . C10 C 0.8247(7) 0.5338(6) 0.5443(4) 0.077(3) Uani 1 1 d . . . H10 H 0.8745 0.5131 0.5707 0.093 Uiso 1 1 calc R . . C11 C 0.7749(7) 0.4766(6) 0.4793(4) 0.068(2) Uani 1 1 d . . . H11 H 0.7933 0.4177 0.4615 0.082 Uiso 1 1 calc R . . C12 C 0.5761(6) 0.2943(6) 0.3976(4) 0.0551(19) Uani 1 1 d . . . C13 C 0.5533(7) 0.3342(7) 0.4559(4) 0.076(3) Uani 1 1 d . . . H13 H 0.5562 0.4015 0.4713 0.091 Uiso 1 1 calc R . . C14 C 0.5265(7) 0.2786(7) 0.4918(4) 0.079(3) Uani 1 1 d . . . H14 H 0.5081 0.3081 0.5305 0.094 Uiso 1 1 calc R . . C15 C 0.5253(7) 0.1811(7) 0.4740(5) 0.080(3) Uani 1 1 d . . . H15 H 0.5107 0.1445 0.5008 0.096 Uiso 1 1 calc R . . C16 C 0.5463(7) 0.1400(7) 0.4157(5) 0.080(3) Uani 1 1 d . . . H16 H 0.5446 0.0730 0.4014 0.097 Uiso 1 1 calc R . . C17 C 0.5701(7) 0.1944(6) 0.3769(5) 0.076(3) Uani 1 1 d . . . H17 H 0.5823 0.1636 0.3363 0.091 Uiso 1 1 calc R . . C18 C 0.9475(7) 0.6140(7) 0.4354(4) 0.082(3) Uani 1 1 d . . . H18A H 0.9568 0.5475 0.4194 0.098 Uiso 1 1 calc R . . H18B H 0.8738 0.6095 0.4369 0.098 Uiso 1 1 calc R . . C19 C 1.0225(7) 0.6707(8) 0.5009(4) 0.100(4) Uani 1 1 d . . . H19A H 0.9886 0.7131 0.5286 0.120 Uiso 1 1 calc R . . H19B H 1.0468 0.6269 0.5231 0.120 Uiso 1 1 calc R . . C20 C 1.1120(7) 0.7295(6) 0.4896(4) 0.074(3) Uani 1 1 d . . . H20A H 1.1633 0.6919 0.4786 0.089 Uiso 1 1 calc R . . H20B H 1.1486 0.7891 0.5283 0.089 Uiso 1 1 calc R . . C21 C 1.0577(7) 0.7529(5) 0.4328(4) 0.076(3) Uani 1 1 d . . . H21A H 1.0294 0.8099 0.4478 0.091 Uiso 1 1 calc R . . H21B H 1.1070 0.7672 0.4078 0.091 Uiso 1 1 calc R . . C22 C 0.9670(5) 0.4312(4) 0.2261(3) 0.0444(17) Uani 1 1 d . . . H22A H 0.9699 0.4135 0.1803 0.053 Uiso 1 1 calc R . . H22B H 0.8951 0.4020 0.2264 0.053 Uiso 1 1 calc R . . C23 C 1.0480(5) 0.3983(5) 0.2660(4) 0.0509(19) Uani 1 1 d . . . H23A H 1.0554 0.3345 0.2402 0.061 Uiso 1 1 calc R . . H23B H 1.0303 0.3942 0.3061 0.061 Uiso 1 1 calc R . . C24 C 1.1470(5) 0.4786(4) 0.2825(4) 0.0458(17) Uani 1 1 d . . . H24A H 1.1984 0.4842 0.3234 0.055 Uiso 1 1 calc R . . H24B H 1.1807 0.4660 0.2466 0.055 Uiso 1 1 calc R . . C25 C 1.1093(5) 0.5691(5) 0.2907(4) 0.056(2) Uani 1 1 d . . . H25A H 1.1241 0.6074 0.3377 0.067 Uiso 1 1 calc R . . H25B H 1.1449 0.6099 0.2699 0.067 Uiso 1 1 calc R . . C26 C 0.5435(5) 0.6693(4) 0.2907(3) 0.0440(17) Uani 1 1 d . . . H26A H 0.5179 0.6693 0.2457 0.053 Uiso 1 1 calc R . . H26B H 0.6184 0.7068 0.3096 0.053 Uiso 1 1 calc R . . C27 C 0.4784(6) 0.7116(5) 0.3322(4) 0.057(2) Uani 1 1 d . . . H27A H 0.5200 0.7417 0.3789 0.068 Uiso 1 1 calc R . . H27B H 0.4503 0.7612 0.3178 0.068 Uiso 1 1 calc R . . C28 C 0.3919(6) 0.6268(5) 0.3217(4) 0.059(2) Uani 1 1 d . . . H28A H 0.3333 0.6152 0.2824 0.071 Uiso 1 1 calc R . . H28B H 0.3642 0.6370 0.3602 0.071 Uiso 1 1 calc R . . C29 C 0.4415(5) 0.5441(5) 0.3125(3) 0.0451(17) Uani 1 1 d . . . H29A H 0.4639 0.5328 0.3544 0.054 Uiso 1 1 calc R . . H29B H 0.3911 0.4840 0.2796 0.054 Uiso 1 1 calc R . . C30 C 0.9458(4) 0.8125(4) 0.2775(3) 0.0291(13) Uani 1 1 d . . . C31 C 0.9765(4) 0.9121(4) 0.2740(3) 0.0354(15) Uani 1 1 d . . . C32 C 0.9827(5) 0.9913(5) 0.3276(3) 0.0422(16) Uani 1 1 d . . . H32 H 0.9654 0.9811 0.3646 0.051 Uiso 1 1 calc R . . C33 C 1.0136(5) 1.0849(5) 0.3284(4) 0.0472(18) Uani 1 1 d . . . H33 H 1.0209 1.1388 0.3663 0.057 Uiso 1 1 calc R . . C34 C 1.0338(5) 1.0991(5) 0.2737(4) 0.056(2) Uani 1 1 d . . . H34 H 1.0516 1.1632 0.2730 0.067 Uiso 1 1 calc R . . C35 C 1.0284(5) 1.0216(5) 0.2201(4) 0.056(2) Uani 1 1 d . . . H35 H 1.0449 1.0324 0.1831 0.067 Uiso 1 1 calc R . . C36 C 0.9991(5) 0.9277(5) 0.2196(3) 0.0415(16) Uani 1 1 d . . . H36 H 0.9944 0.8741 0.1822 0.050 Uiso 1 1 calc R . . C37 C 0.7809(4) 0.8337(4) 0.2969(3) 0.0305(14) Uani 1 1 d . . . C38 C 0.7119(5) 0.8259(4) 0.2369(3) 0.0352(15) Uani 1 1 d . . . C39 C 0.7273(5) 0.7738(5) 0.1699(3) 0.0429(16) Uani 1 1 d . . . H39 H 0.7970 0.7578 0.1782 0.051 Uiso 1 1 calc R . . C40 C 0.7291(6) 0.8368(5) 0.1275(3) 0.056(2) Uani 1 1 d . . . H40A H 0.7847 0.8974 0.1513 0.083 Uiso 1 1 calc R . . H40B H 0.6606 0.8517 0.1172 0.083 Uiso 1 1 calc R . . H40C H 0.7432 0.8020 0.0868 0.083 Uiso 1 1 calc R . . C41 C 0.6420(6) 0.6786(5) 0.1344(3) 0.059(2) Uani 1 1 d . . . H41A H 0.6526 0.6452 0.0922 0.089 Uiso 1 1 calc R . . H41B H 0.5725 0.6920 0.1271 0.089 Uiso 1 1 calc R . . H41C H 0.6462 0.6372 0.1612 0.089 Uiso 1 1 calc R . . C42 C 0.6251(5) 0.8645(4) 0.2369(3) 0.0419(16) Uani 1 1 d . . . H42 H 0.5790 0.8598 0.1966 0.050 Uiso 1 1 calc R . . C43 C 0.6057(5) 0.9098(5) 0.2953(4) 0.0491(19) Uani 1 1 d . . . H43 H 0.5459 0.9356 0.2948 0.059 Uiso 1 1 calc R . . C44 C 0.6726(5) 0.9181(4) 0.3544(3) 0.0430(17) Uani 1 1 d . . . H44 H 0.6582 0.9495 0.3941 0.052 Uiso 1 1 calc R . . C45 C 0.7606(5) 0.8810(4) 0.3562(3) 0.0350(15) Uani 1 1 d . . . C46 C 0.8303(5) 0.8911(4) 0.4217(3) 0.0422(16) Uani 1 1 d . . . H46 H 0.8967 0.8745 0.4147 0.051 Uiso 1 1 calc R . . C47 C 0.8612(5) 0.9957(5) 0.4704(3) 0.055(2) Uani 1 1 d . . . H47A H 0.9071 0.9995 0.5122 0.082 Uiso 1 1 calc R . . H47B H 0.7974 1.0151 0.4774 0.082 Uiso 1 1 calc R . . H47C H 0.8988 1.0393 0.4527 0.082 Uiso 1 1 calc R . . C48 C 0.7810(6) 0.8213(5) 0.4509(3) 0.057(2) Uani 1 1 d . . . H48A H 0.7625 0.7547 0.4196 0.086 Uiso 1 1 calc R . . H48B H 0.7171 0.8375 0.4604 0.086 Uiso 1 1 calc R . . H48C H 0.8314 0.8266 0.4916 0.086 Uiso 1 1 calc R . . C49 C 1.0919(5) 0.7635(4) 0.2415(3) 0.0373(15) Uani 1 1 d . . . C50 C 1.1860(5) 0.8336(5) 0.2814(3) 0.0418(16) Uani 1 1 d . . . C51 C 1.2036(5) 0.8943(5) 0.3531(3) 0.0464(18) Uani 1 1 d . . . H51 H 1.1346 0.8826 0.3634 0.056 Uiso 1 1 calc R . . C52 C 1.2428(5) 1.0028(5) 0.3672(4) 0.063(2) Uani 1 1 d . . . H52A H 1.2522 1.0387 0.4135 0.095 Uiso 1 1 calc R . . H52B H 1.1910 1.0235 0.3397 0.095 Uiso 1 1 calc R . . H52C H 1.3104 1.0158 0.3574 0.095 Uiso 1 1 calc R . . C53 C 1.2827(6) 0.8597(5) 0.3975(4) 0.065(2) Uani 1 1 d . . . H53A H 1.2937 0.8980 0.4436 0.097 Uiso 1 1 calc R . . H53B H 1.3501 0.8685 0.3871 0.097 Uiso 1 1 calc R . . H53C H 1.2540 0.7909 0.3897 0.097 Uiso 1 1 calc R . . C54 C 1.2702(5) 0.8461(5) 0.2557(4) 0.059(2) Uani 1 1 d . . . H54 H 1.3344 0.8923 0.2831 0.071 Uiso 1 1 calc R . . C55 C 1.2651(6) 0.7946(6) 0.1921(4) 0.067(2) Uani 1 1 d . . . H55 H 1.3230 0.8076 0.1753 0.081 Uiso 1 1 calc R . . C56 C 1.1741(6) 0.7240(6) 0.1537(4) 0.062(2) Uani 1 1 d . . . H56 H 1.1707 0.6859 0.1104 0.074 Uiso 1 1 calc R . . C57 C 1.0869(5) 0.7073(5) 0.1769(3) 0.0462(17) Uani 1 1 d . . . C58 C 0.9887(6) 0.6262(5) 0.1319(3) 0.0527(19) Uani 1 1 d . . . H58 H 0.9434 0.6103 0.1593 0.063 Uiso 1 1 calc R . . C59 C 0.9247(6) 0.6576(6) 0.0804(4) 0.074(2) Uani 1 1 d . . . H59A H 0.9035 0.7155 0.1021 0.111 Uiso 1 1 calc R . . H59B H 0.8617 0.6050 0.0532 0.111 Uiso 1 1 calc R . . H59C H 0.9678 0.6726 0.0527 0.111 Uiso 1 1 calc R . . C60 C 1.0199(6) 0.5346(5) 0.0980(4) 0.064(2) Uani 1 1 d . . . H60A H 0.9561 0.4834 0.0699 0.096 Uiso 1 1 calc R . . H60B H 1.0583 0.5126 0.1312 0.096 Uiso 1 1 calc R . . H60C H 1.0651 0.5490 0.0713 0.096 Uiso 1 1 calc R . . C61 C 0.5356(4) 0.2969(4) 0.1683(3) 0.0293(13) Uani 1 1 d . . . C62 C 0.4792(5) 0.1980(4) 0.1183(3) 0.0363(15) Uani 1 1 d . . . C63 C 0.4003(5) 0.1829(4) 0.0623(3) 0.0402(16) Uani 1 1 d . . . H63 H 0.3796 0.2368 0.0542 0.048 Uiso 1 1 calc R . . C64 C 0.3502(5) 0.0883(5) 0.0170(3) 0.0505(19) Uani 1 1 d . . . H64 H 0.2952 0.0785 -0.0210 0.061 Uiso 1 1 calc R . . C65 C 0.3810(6) 0.0097(5) 0.0279(4) 0.056(2) Uani 1 1 d . . . H65 H 0.3484 -0.0541 -0.0028 0.068 Uiso 1 1 calc R . . C66 C 0.4582(6) 0.0245(5) 0.0828(4) 0.0531(19) Uani 1 1 d . . . H66 H 0.4795 -0.0294 0.0905 0.064 Uiso 1 1 calc R . . C67 C 0.5065(5) 0.1171(4) 0.1279(3) 0.0418(16) Uani 1 1 d . . . H67 H 0.5597 0.1254 0.1664 0.050 Uiso 1 1 calc R . . C68 C 0.3745(5) 0.3463(4) 0.1707(3) 0.0340(15) Uani 1 1 d . . . C69 C 0.3316(5) 0.4009(5) 0.1360(3) 0.0397(16) Uani 1 1 d . . . C70 C 0.3985(5) 0.4794(5) 0.1213(3) 0.0419(16) Uani 1 1 d . . . H70 H 0.4682 0.5044 0.1558 0.050 Uiso 1 1 calc R . . C71 C 0.4193(6) 0.4398(5) 0.0548(3) 0.0524(19) Uani 1 1 d . . . H71A H 0.4627 0.4926 0.0468 0.079 Uiso 1 1 calc R . . H71B H 0.3520 0.4124 0.0202 0.079 Uiso 1 1 calc R . . H71C H 0.4566 0.3890 0.0549 0.079 Uiso 1 1 calc R . . C72 C 0.3516(6) 0.5644(5) 0.1228(4) 0.058(2) Uani 1 1 d . . . H72A H 0.3985 0.6128 0.1130 0.086 Uiso 1 1 calc R . . H72B H 0.3433 0.5938 0.1664 0.086 Uiso 1 1 calc R . . H72C H 0.2825 0.5419 0.0899 0.086 Uiso 1 1 calc R . . C73 C 0.2203(5) 0.3795(5) 0.1122(3) 0.0491(18) Uani 1 1 d . . . H73 H 0.1893 0.4142 0.0872 0.059 Uiso 1 1 calc R . . C74 C 0.1562(6) 0.3084(6) 0.1250(4) 0.060(2) Uani 1 1 d . . . H74 H 0.0817 0.2932 0.1076 0.072 Uiso 1 1 calc R . . C75 C 0.1995(5) 0.2605(5) 0.1624(3) 0.0528(19) Uani 1 1 d . . . H75 H 0.1545 0.2142 0.1726 0.063 Uiso 1 1 calc R . . C76 C 0.3087(5) 0.2777(5) 0.1862(3) 0.0426(17) Uani 1 1 d . . . C77 C 0.3481(6) 0.2235(5) 0.2302(3) 0.0503(18) Uani 1 1 d . . . H77 H 0.4265 0.2370 0.2390 0.060 Uiso 1 1 calc R . . C78 C 0.3245(6) 0.2628(6) 0.2969(4) 0.065(2) Uani 1 1 d . . . H78A H 0.3513 0.2283 0.3253 0.097 Uiso 1 1 calc R . . H78B H 0.2481 0.2526 0.2895 0.097 Uiso 1 1 calc R . . H78C H 0.3592 0.3324 0.3179 0.097 Uiso 1 1 calc R . . C79 C 0.3028(6) 0.1135(5) 0.2005(4) 0.064(2) Uani 1 1 d . . . H79A H 0.3326 0.0837 0.2315 0.095 Uiso 1 1 calc R . . H79B H 0.3210 0.0882 0.1596 0.095 Uiso 1 1 calc R . . H79C H 0.2259 0.0980 0.1915 0.095 Uiso 1 1 calc R . . C80 C 0.7072(4) 0.2725(4) 0.1656(3) 0.0305(14) Uani 1 1 d . . . C81 C 0.7654(5) 0.2224(4) 0.1986(3) 0.0341(15) Uani 1 1 d . . . C82 C 0.7488(5) 0.2109(4) 0.2605(3) 0.0450(17) Uani 1 1 d . . . H82 H 0.6813 0.2280 0.2646 0.054 Uiso 1 1 calc R . . C83 C 0.8375(6) 0.2815(5) 0.3226(3) 0.0510(19) Uani 1 1 d . . . H83A H 0.8224 0.2724 0.3617 0.076 Uiso 1 1 calc R . . H83B H 0.8406 0.3486 0.3253 0.076 Uiso 1 1 calc R . . H83C H 0.9055 0.2679 0.3200 0.076 Uiso 1 1 calc R . . C84 C 0.7360(6) 0.1065(5) 0.2584(4) 0.060(2) Uani 1 1 d . . . H84A H 0.7240 0.1021 0.2994 0.089 Uiso 1 1 calc R . . H84B H 0.8001 0.0864 0.2532 0.089 Uiso 1 1 calc R . . H84C H 0.6755 0.0637 0.2214 0.089 Uiso 1 1 calc R . . C85 C 0.8377(5) 0.1821(5) 0.1718(4) 0.0465(18) Uani 1 1 d . . . H85 H 0.8764 0.1479 0.1937 0.056 Uiso 1 1 calc R . . C86 C 0.8563(5) 0.1890(5) 0.1148(4) 0.0484(18) Uani 1 1 d . . . H86 H 0.9076 0.1616 0.0980 0.058 Uiso 1 1 calc R . . C87 C 0.7979(5) 0.2368(5) 0.0829(3) 0.0474(18) Uani 1 1 d . . . H87 H 0.8094 0.2418 0.0434 0.057 Uiso 1 1 calc R . . C88 C 0.7227(5) 0.2780(4) 0.1063(3) 0.0347(15) Uani 1 1 d . . . C89 C 0.6615(5) 0.3275(4) 0.0666(3) 0.0383(15) Uani 1 1 d . . . H89 H 0.6091 0.3502 0.0891 0.046 Uiso 1 1 calc R . . C90 C 0.7316(6) 0.4156(5) 0.0627(3) 0.055(2) Uani 1 1 d . . . H90A H 0.6885 0.4457 0.0373 0.082 Uiso 1 1 calc R . . H90B H 0.7845 0.3957 0.0413 0.082 Uiso 1 1 calc R . . H90C H 0.7671 0.4626 0.1071 0.082 Uiso 1 1 calc R . . C91 C 0.6002(5) 0.2586(5) -0.0028(3) 0.0475(18) Uani 1 1 d . . . H91A H 0.5611 0.2934 -0.0263 0.071 Uiso 1 1 calc R . . H91B H 0.5506 0.2038 -0.0008 0.071 Uiso 1 1 calc R . . H91C H 0.6496 0.2344 -0.0260 0.071 Uiso 1 1 calc R . . N1 N 0.8627(4) 0.7842(3) 0.2974(2) 0.0297(11) Uani 1 1 d . . . N2 N 0.9995(4) 0.7452(3) 0.2630(2) 0.0339(12) Uani 1 1 d . . . N3 N 0.4874(4) 0.3648(3) 0.1907(2) 0.0316(12) Uani 1 1 d . . . N4 N 0.6397(3) 0.3222(3) 0.1954(2) 0.0285(11) Uani 1 1 d . . . O1 O 0.9728(3) 0.6670(3) 0.3930(2) 0.0472(12) Uani 1 1 d . . . O2 O 0.9963(3) 0.5366(3) 0.2588(2) 0.0424(11) Uani 1 1 d . . . O3 O 0.5319(3) 0.5708(3) 0.2904(2) 0.0393(11) Uani 1 1 d . . . Lu1 Lu 0.875229(19) 0.626853(17) 0.286998(13) 0.03086(8) Uani 1 1 d . . . Lu2 Lu 0.652923(19) 0.476568(17) 0.270553(12) 0.03054(8) Uani 1 1 d . . . H1 H 0.830(4) 0.500(3) 0.298(2) 0.027(14) Uiso 1 1 d . . . H3 H 0.738(5) 0.537(4) 0.212(3) 0.050(18) Uiso 1 1 d . . . H2 H 0.749(5) 0.616(4) 0.329(3) 0.06(2) Uiso 1 1 d . . . H4 H 0.572(5) 0.313(5) 0.314(3) 0.06(2) 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 C4 0.055(5) 0.076(6) 0.042(5) 0.017(5) 0.018(4) 0.023(4) C5 0.044(4) 0.039(4) 0.042(4) 0.004(3) 0.017(3) 0.020(3) C6 0.059(5) 0.045(4) 0.049(5) 0.009(4) 0.010(4) 0.022(4) C7 0.072(6) 0.065(5) 0.055(5) 0.013(4) 0.009(4) 0.025(5) C8 0.090(7) 0.057(5) 0.067(6) -0.005(5) 0.012(5) 0.032(5) C9 0.078(6) 0.076(6) 0.049(5) 0.004(5) -0.002(4) 0.018(5) C10 0.091(7) 0.079(6) 0.052(5) 0.010(5) 0.006(5) 0.038(5) C11 0.092(7) 0.058(5) 0.051(5) 0.012(4) 0.011(5) 0.039(5) C12 0.054(5) 0.062(5) 0.048(5) 0.018(4) 0.016(4) 0.013(4) C13 0.102(7) 0.076(6) 0.053(5) 0.020(5) 0.039(5) 0.012(5) C14 0.084(7) 0.087(7) 0.076(6) 0.028(6) 0.041(5) 0.028(5) C15 0.086(7) 0.080(7) 0.085(7) 0.039(6) 0.028(6) 0.029(6) C16 0.075(6) 0.067(6) 0.106(8) 0.033(6) 0.034(6) 0.020(5) C17 0.082(6) 0.069(6) 0.085(7) 0.030(5) 0.036(5) 0.023(5) C18 0.061(6) 0.102(7) 0.072(6) 0.037(6) 0.005(5) 0.000(5) C19 0.059(6) 0.169(11) 0.060(6) 0.043(7) -0.005(5) 0.022(7) C20 0.071(6) 0.063(5) 0.059(5) 0.008(4) -0.014(5) 0.011(5) C21 0.076(6) 0.039(4) 0.067(6) -0.002(4) -0.031(5) 0.002(4) C22 0.040(4) 0.025(3) 0.057(5) -0.001(3) 0.011(3) 0.010(3) C23 0.039(4) 0.047(4) 0.068(5) 0.022(4) 0.012(4) 0.014(3) C24 0.040(4) 0.038(4) 0.060(5) 0.016(4) 0.014(4) 0.015(3) C25 0.029(4) 0.038(4) 0.082(6) 0.001(4) 0.005(4) 0.011(3) C26 0.039(4) 0.035(4) 0.058(5) 0.013(3) 0.014(3) 0.016(3) C27 0.072(5) 0.038(4) 0.068(5) 0.014(4) 0.032(4) 0.025(4) C28 0.048(5) 0.056(5) 0.076(6) 0.013(4) 0.030(4) 0.020(4) C29 0.042(4) 0.046(4) 0.045(4) 0.006(3) 0.022(3) 0.012(3) C30 0.029(3) 0.027(3) 0.025(3) 0.000(3) 0.006(3) 0.010(3) C31 0.024(3) 0.030(3) 0.047(4) 0.009(3) 0.005(3) 0.009(3) C32 0.039(4) 0.037(4) 0.048(4) 0.014(3) 0.011(3) 0.007(3) C33 0.038(4) 0.034(4) 0.065(5) 0.012(4) 0.007(4) 0.014(3) C34 0.046(4) 0.029(4) 0.090(6) 0.022(4) 0.015(4) 0.009(3) C35 0.041(4) 0.054(5) 0.077(6) 0.033(5) 0.019(4) 0.008(4) C36 0.026(3) 0.045(4) 0.055(5) 0.019(4) 0.011(3) 0.011(3) C37 0.026(3) 0.022(3) 0.039(4) 0.006(3) 0.009(3) 0.005(3) C38 0.029(3) 0.027(3) 0.040(4) 0.006(3) 0.003(3) 0.001(3) C39 0.031(4) 0.052(4) 0.038(4) 0.011(3) 0.004(3) 0.009(3) C40 0.055(5) 0.068(5) 0.048(5) 0.025(4) 0.014(4) 0.019(4) C41 0.069(5) 0.052(5) 0.044(4) 0.006(4) 0.008(4) 0.013(4) C42 0.035(4) 0.035(4) 0.053(4) 0.015(3) 0.007(3) 0.010(3) C43 0.032(4) 0.041(4) 0.079(6) 0.022(4) 0.016(4) 0.018(3) C44 0.045(4) 0.025(3) 0.057(5) 0.002(3) 0.023(4) 0.014(3) C45 0.029(3) 0.025(3) 0.044(4) 0.003(3) 0.010(3) 0.008(3) C46 0.043(4) 0.035(4) 0.044(4) 0.003(3) 0.014(3) 0.014(3) C47 0.051(5) 0.048(4) 0.049(5) -0.008(4) 0.016(4) 0.013(4) C48 0.064(5) 0.048(4) 0.046(5) 0.009(4) 0.004(4) 0.006(4) C49 0.032(4) 0.037(4) 0.043(4) 0.007(3) 0.012(3) 0.016(3) C50 0.028(4) 0.036(4) 0.048(4) -0.001(3) 0.005(3) 0.012(3) C51 0.032(4) 0.039(4) 0.051(4) -0.002(3) 0.005(3) 0.007(3) C52 0.036(4) 0.044(4) 0.080(6) -0.012(4) 0.012(4) 0.002(3) C53 0.050(5) 0.064(5) 0.059(5) -0.003(4) -0.003(4) 0.031(4) C54 0.026(4) 0.054(5) 0.078(6) 0.002(4) 0.015(4) 0.000(3) C55 0.043(5) 0.067(5) 0.077(6) 0.001(5) 0.028(4) 0.008(4) C56 0.048(5) 0.074(6) 0.060(5) 0.008(4) 0.026(4) 0.021(4) C57 0.036(4) 0.049(4) 0.049(4) 0.006(4) 0.013(3) 0.020(3) C58 0.046(4) 0.055(5) 0.046(4) 0.004(4) 0.013(4) 0.013(4) C59 0.065(6) 0.069(6) 0.067(6) 0.007(5) 0.002(4) 0.017(5) C60 0.063(5) 0.052(5) 0.065(5) 0.000(4) 0.024(4) 0.012(4) C61 0.030(3) 0.022(3) 0.028(3) 0.004(3) 0.003(3) 0.004(3) C62 0.026(3) 0.036(4) 0.037(4) 0.002(3) 0.007(3) 0.005(3) C63 0.043(4) 0.031(4) 0.036(4) 0.005(3) 0.007(3) 0.002(3) C64 0.039(4) 0.055(5) 0.035(4) -0.005(3) 0.003(3) 0.001(4) C65 0.061(5) 0.031(4) 0.051(5) -0.009(3) 0.009(4) -0.003(4) C66 0.054(5) 0.023(3) 0.064(5) -0.002(3) 0.010(4) 0.005(3) C67 0.036(4) 0.032(4) 0.044(4) 0.006(3) 0.002(3) 0.003(3) C68 0.030(3) 0.035(3) 0.028(3) 0.000(3) 0.005(3) 0.010(3) C69 0.032(4) 0.044(4) 0.032(4) 0.000(3) 0.006(3) 0.012(3) C70 0.037(4) 0.046(4) 0.039(4) 0.010(3) 0.005(3) 0.015(3) C71 0.057(5) 0.056(5) 0.047(4) 0.018(4) 0.018(4) 0.016(4) C72 0.059(5) 0.062(5) 0.052(5) 0.015(4) 0.016(4) 0.029(4) C73 0.041(4) 0.052(4) 0.047(4) 0.008(4) 0.006(3) 0.019(4) C74 0.032(4) 0.069(5) 0.063(5) 0.007(4) 0.012(4) 0.007(4) C75 0.039(4) 0.053(5) 0.049(5) 0.003(4) 0.010(4) -0.001(4) C76 0.038(4) 0.039(4) 0.038(4) -0.005(3) 0.012(3) 0.009(3) C77 0.042(4) 0.050(4) 0.050(5) 0.009(4) 0.017(4) 0.002(3) C78 0.051(5) 0.080(6) 0.058(5) 0.018(5) 0.023(4) 0.007(4) C79 0.060(5) 0.052(5) 0.082(6) 0.022(4) 0.035(5) 0.006(4) C80 0.025(3) 0.019(3) 0.033(4) -0.004(3) 0.002(3) -0.002(2) C81 0.027(3) 0.021(3) 0.044(4) 0.003(3) 0.005(3) 0.002(3) C82 0.043(4) 0.029(4) 0.056(5) 0.010(3) 0.006(3) 0.013(3) C83 0.061(5) 0.052(4) 0.043(4) 0.023(4) 0.008(4) 0.018(4) C84 0.068(5) 0.040(4) 0.072(6) 0.025(4) 0.013(4) 0.015(4) C85 0.033(4) 0.039(4) 0.061(5) 0.013(4) 0.004(3) 0.015(3) C86 0.036(4) 0.044(4) 0.054(5) 0.003(4) 0.010(3) 0.016(3) C87 0.051(4) 0.041(4) 0.031(4) -0.011(3) 0.011(3) 0.005(3) C88 0.029(3) 0.024(3) 0.037(4) -0.002(3) 0.003(3) 0.002(3) C89 0.041(4) 0.040(4) 0.031(4) 0.006(3) 0.013(3) 0.011(3) C90 0.061(5) 0.046(4) 0.050(5) 0.015(4) 0.015(4) 0.006(4) C91 0.047(4) 0.047(4) 0.036(4) 0.007(3) 0.000(3) 0.007(3) N1 0.026(3) 0.029(3) 0.032(3) 0.006(2) 0.007(2) 0.012(2) N2 0.031(3) 0.027(3) 0.038(3) 0.006(2) 0.009(2) 0.007(2) N3 0.026(3) 0.030(3) 0.031(3) 0.002(2) 0.006(2) 0.005(2) N4 0.023(3) 0.019(2) 0.034(3) 0.000(2) 0.003(2) 0.005(2) O1 0.046(3) 0.040(3) 0.042(3) 0.004(2) 0.001(2) 0.010(2) O2 0.029(2) 0.028(2) 0.060(3) 0.003(2) 0.007(2) 0.0102(19) O3 0.032(2) 0.031(2) 0.051(3) 0.005(2) 0.016(2) 0.0100(19) Lu1 0.02561(15) 0.02370(15) 0.03519(17) 0.00160(12) 0.00337(12) 0.00843(11) Lu2 0.02845(16) 0.02414(15) 0.03160(16) 0.00077(12) 0.00608(12) 0.00747(12) _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 C4 C5 1.347(10) . ? C4 C12 1.481(10) . ? C4 H4 0.89(7) . ? C5 C6 1.503(9) . ? C5 Lu2 2.371(7) . ? C6 C7 1.376(10) . ? C6 C11 1.390(10) . ? C7 C8 1.397(10) . ? C7 H7 0.9500 . ? C8 C9 1.385(11) . ? C8 H8 0.9500 . ? C9 C10 1.397(11) . ? C9 H9 0.9500 . ? C10 C11 1.386(10) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.384(10) . ? C12 C17 1.405(11) . ? C13 C14 1.372(10) . ? C13 H13 0.9500 . ? C14 C15 1.387(11) . ? C14 H14 0.9500 . ? C15 C16 1.377(12) . ? C15 H15 0.9500 . ? C16 C17 1.402(11) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 O1 1.461(9) . ? C18 C19 1.480(11) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.473(11) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.489(10) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 O1 1.449(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O2 1.462(7) . ? C22 C23 1.498(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.518(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.500(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O2 1.453(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O3 1.450(7) . ? C26 C27 1.490(9) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.482(9) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.488(9) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O3 1.444(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 N1 1.336(7) . ? C30 N2 1.341(7) . ? C30 C31 1.502(8) . ? C30 Lu1 2.854(6) . ? C31 C32 1.385(9) . ? C31 C36 1.387(9) . ? C32 C33 1.380(8) . ? C32 H32 0.9500 . ? C33 C34 1.375(10) . ? C33 H33 0.9500 . ? C34 C35 1.372(10) . ? C34 H34 0.9500 . ? C35 C36 1.386(9) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C45 1.411(8) . ? C37 C38 1.413(8) . ? C37 N1 1.430(7) . ? C38 C42 1.389(8) . ? C38 C39 1.544(9) . ? C39 C40 1.522(9) . ? C39 C41 1.523(9) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.382(9) . ? C42 H42 0.9500 . ? C43 C44 1.382(9) . ? C43 H43 0.9500 . ? C44 C45 1.390(8) . ? C44 H44 0.9500 . ? C45 C46 1.504(9) . ? C46 C48 1.516(9) . ? C46 C47 1.534(8) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.406(8) . ? C49 C57 1.416(9) . ? C49 N2 1.436(7) . ? C50 C54 1.384(9) . ? C50 C51 1.528(9) . ? C51 C52 1.525(9) . ? C51 C53 1.555(9) . ? C51 H51 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.377(10) . ? C54 H54 0.9500 . ? C55 C56 1.376(10) . ? C55 H55 0.9500 . ? C56 C57 1.394(9) . ? C56 H56 0.9500 . ? C57 C58 1.533(9) . ? C58 C59 1.523(10) . ? C58 C60 1.529(9) . ? C58 H58 1.0000 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 N3 1.330(7) . ? C61 N4 1.331(7) . ? C61 C62 1.502(8) . ? C61 Lu2 2.860(5) . ? C62 C63 1.383(8) . ? C62 C67 1.385(8) . ? C63 C64 1.409(8) . ? C63 H63 0.9500 . ? C64 C65 1.381(10) . ? C64 H64 0.9500 . ? C65 C66 1.353(9) . ? C65 H65 0.9500 . ? C66 C67 1.384(8) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C68 C69 1.395(9) . ? C68 C76 1.406(9) . ? C68 N3 1.436(7) . ? C69 C73 1.417(9) . ? C69 C70 1.510(9) . ? C70 C72 1.509(9) . ? C70 C71 1.532(9) . ? C70 H70 1.0000 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C74 1.385(10) . ? C73 H73 0.9500 . ? C74 C75 1.357(10) . ? C74 H74 0.9500 . ? C75 C76 1.396(9) . ? C75 H75 0.9500 . ? C76 C77 1.517(10) . ? C77 C79 1.526(9) . ? C77 C78 1.553(9) . ? C77 H77 1.0000 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 C88 1.408(8) . ? C80 C81 1.413(8) . ? C80 N4 1.422(7) . ? C81 C85 1.381(9) . ? C81 C82 1.502(9) . ? C82 C84 1.525(8) . ? C82 C83 1.555(9) . ? C82 H82 1.0000 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 C86 1.380(9) . ? C85 H85 0.9500 . ? C86 C87 1.375(9) . ? C86 H86 0.9500 . ? C87 C88 1.389(9) . ? C87 H87 0.9500 . ? C88 C89 1.515(8) . ? C89 C90 1.515(8) . ? C89 C91 1.528(8) . ? C89 H89 1.0000 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? N1 Lu1 2.331(5) . ? N2 Lu1 2.474(5) . ? N3 Lu2 2.470(5) . ? N4 Lu2 2.361(4) . ? O1 Lu1 2.281(4) . ? O2 Lu1 2.361(4) . ? O3 Lu2 2.360(4) . ? Lu1 Lu2 3.2808(6) . ? Lu1 H1 1.98(5) . ? Lu1 H3 2.11(6) . ? Lu1 H2 2.12(6) . ? Lu2 H1 2.26(5) . ? Lu2 H3 2.20(6) . ? Lu2 H2 2.10(6) . ? 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 C5 C4 C12 133.8(8) . . ? C5 C4 H4 116(5) . . ? C12 C4 H4 110(5) . . ? C4 C5 C6 114.0(7) . . ? C4 C5 Lu2 112.9(5) . . ? C6 C5 Lu2 132.7(5) . . ? C7 C6 C11 116.5(7) . . ? C7 C6 C5 120.4(7) . . ? C11 C6 C5 122.8(7) . . ? C6 C7 C8 122.5(8) . . ? C6 C7 H7 118.8 . . ? C8 C7 H7 118.8 . . ? C9 C8 C7 119.9(8) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 118.7(8) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C11 C10 C9 119.7(8) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C6 122.6(8) . . ? C10 C11 H11 118.7 . . ? C6 C11 H11 118.7 . . ? C13 C12 C17 117.1(8) . . ? C13 C12 C4 123.7(8) . . ? C17 C12 C4 119.2(7) . . ? C14 C13 C12 121.3(9) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 122.6(9) . . ? C13 C14 H14 118.7 . . ? C15 C14 H14 118.7 . . ? C16 C15 C14 116.7(9) . . ? C16 C15 H15 121.7 . . ? C14 C15 H15 121.7 . . ? C15 C16 C17 121.7(9) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C16 C17 C12 120.5(8) . . ? C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? O1 C18 C19 105.3(7) . . ? O1 C18 H18A 110.7 . . ? C19 C18 H18A 110.7 . . ? O1 C18 H18B 110.7 . . ? C19 C18 H18B 110.7 . . ? H18A C18 H18B 108.8 . . ? C20 C19 C18 106.1(7) . . ? C20 C19 H19A 110.5 . . ? C18 C19 H19A 110.5 . . ? C20 C19 H19B 110.5 . . ? C18 C19 H19B 110.5 . . ? H19A C19 H19B 108.7 . . ? C19 C20 C21 101.6(7) . . ? C19 C20 H20A 111.5 . . ? C21 C20 H20A 111.5 . . ? C19 C20 H20B 111.5 . . ? C21 C20 H20B 111.5 . . ? H20A C20 H20B 109.3 . . ? O1 C21 C20 105.2(6) . . ? O1 C21 H21A 110.7 . . ? C20 C21 H21A 110.7 . . ? O1 C21 H21B 110.7 . . ? C20 C21 H21B 110.7 . . ? H21A C21 H21B 108.8 . . ? O2 C22 C23 103.9(5) . . ? O2 C22 H22A 111.0 . . ? C23 C22 H22A 111.0 . . ? O2 C22 H22B 111.0 . . ? C23 C22 H22B 111.0 . . ? H22A C22 H22B 109.0 . . ? C22 C23 C24 101.7(5) . . ? C22 C23 H23A 111.4 . . ? C24 C23 H23A 111.4 . . ? C22 C23 H23B 111.4 . . ? C24 C23 H23B 111.4 . . ? H23A C23 H23B 109.3 . . ? C25 C24 C23 104.7(5) . . ? C25 C24 H24A 110.8 . . ? C23 C24 H24A 110.8 . . ? C25 C24 H24B 110.8 . . ? C23 C24 H24B 110.8 . . ? H24A C24 H24B 108.9 . . ? O2 C25 C24 105.9(5) . . ? O2 C25 H25A 110.6 . . ? C24 C25 H25A 110.6 . . ? O2 C25 H25B 110.6 . . ? C24 C25 H25B 110.6 . . ? H25A C25 H25B 108.7 . . ? O3 C26 C27 105.4(5) . . ? O3 C26 H26A 110.7 . . ? C27 C26 H26A 110.7 . . ? O3 C26 H26B 110.7 . . ? C27 C26 H26B 110.7 . . ? H26A C26 H26B 108.8 . . ? C28 C27 C26 103.6(6) . . ? C28 C27 H27A 111.0 . . ? C26 C27 H27A 111.0 . . ? C28 C27 H27B 111.0 . . ? C26 C27 H27B 111.0 . . ? H27A C27 H27B 109.0 . . ? C27 C28 C29 104.5(6) . . ? C27 C28 H28A 110.8 . . ? C29 C28 H28A 110.8 . . ? C27 C28 H28B 110.8 . . ? C29 C28 H28B 110.8 . . ? H28A C28 H28B 108.9 . . ? O3 C29 C28 106.3(5) . . ? O3 C29 H29A 110.5 . . ? C28 C29 H29A 110.5 . . ? O3 C29 H29B 110.5 . . ? C28 C29 H29B 110.5 . . ? H29A C29 H29B 108.7 . . ? N1 C30 N2 113.8(5) . . ? N1 C30 C31 122.2(5) . . ? N2 C30 C31 124.0(5) . . ? N1 C30 Lu1 53.9(3) . . ? N2 C30 Lu1 60.0(3) . . ? C31 C30 Lu1 176.0(4) . . ? C32 C31 C36 119.0(6) . . ? C32 C31 C30 118.2(6) . . ? C36 C31 C30 122.9(6) . . ? C33 C32 C31 121.1(7) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C34 C33 C32 119.2(7) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C35 C34 C33 120.6(6) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 120.2(7) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 119.8(7) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? C45 C37 C38 119.3(6) . . ? C45 C37 N1 119.9(5) . . ? C38 C37 N1 120.3(5) . . ? C42 C38 C37 119.8(6) . . ? C42 C38 C39 117.5(6) . . ? C37 C38 C39 122.6(6) . . ? C40 C39 C41 111.1(6) . . ? C40 C39 C38 112.7(6) . . ? C41 C39 C38 109.7(5) . . ? C40 C39 H39 107.7 . . ? C41 C39 H39 107.7 . . ? C38 C39 H39 107.7 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C38 120.2(6) . . ? C43 C42 H42 119.9 . . ? C38 C42 H42 119.9 . . ? C42 C43 C44 120.6(6) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C43 C44 C45 120.7(6) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C44 C45 C37 119.3(6) . . ? C44 C45 C46 118.6(6) . . ? C37 C45 C46 122.1(5) . . ? C45 C46 C48 112.4(5) . . ? C45 C46 C47 111.9(5) . . ? C48 C46 C47 110.3(6) . . ? C45 C46 H46 107.3 . . ? C48 C46 H46 107.3 . . ? C47 C46 H46 107.3 . . ? 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 . . ? C50 C49 C57 119.0(6) . . ? C50 C49 N2 123.3(6) . . ? C57 C49 N2 117.7(5) . . ? C54 C50 C49 118.6(6) . . ? C54 C50 C51 117.3(6) . . ? C49 C50 C51 124.0(6) . . ? C52 C51 C50 112.3(6) . . ? C52 C51 C53 110.7(6) . . ? C50 C51 C53 109.1(6) . . ? C52 C51 H51 108.2 . . ? C50 C51 H51 108.2 . . ? C53 C51 H51 108.2 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 C50 123.0(7) . . ? C55 C54 H54 118.5 . . ? C50 C54 H54 118.5 . . ? C56 C55 C54 118.4(7) . . ? C56 C55 H55 120.8 . . ? C54 C55 H55 120.8 . . ? C55 C56 C57 121.3(7) . . ? C55 C56 H56 119.3 . . ? C57 C56 H56 119.3 . . ? C56 C57 C49 119.6(6) . . ? C56 C57 C58 118.7(6) . . ? C49 C57 C58 121.7(6) . . ? C59 C58 C60 109.5(6) . . ? C59 C58 C57 111.5(6) . . ? C60 C58 C57 110.6(6) . . ? C59 C58 H58 108.4 . . ? C60 C58 H58 108.4 . . ? C57 C58 H58 108.4 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N3 C61 N4 114.5(5) . . ? N3 C61 C62 123.9(5) . . ? N4 C61 C62 121.6(5) . . ? N3 C61 Lu2 59.6(3) . . ? N4 C61 Lu2 54.9(3) . . ? C62 C61 Lu2 174.7(4) . . ? C63 C62 C67 117.5(6) . . ? C63 C62 C61 123.1(6) . . ? C67 C62 C61 119.3(5) . . ? C62 C63 C64 120.6(6) . . ? C62 C63 H63 119.7 . . ? C64 C63 H63 119.7 . . ? C65 C64 C63 120.0(6) . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C66 C65 C64 119.4(6) . . ? C66 C65 H65 120.3 . . ? C64 C65 H65 120.3 . . ? C65 C66 C67 120.9(7) . . ? C65 C66 H66 119.6 . . ? C67 C66 H66 119.6 . . ? C66 C67 C62 121.6(6) . . ? C66 C67 H67 119.2 . . ? C62 C67 H67 119.2 . . ? C69 C68 C76 120.6(6) . . ? C69 C68 N3 117.3(5) . . ? C76 C68 N3 122.1(6) . . ? C68 C69 C73 118.2(6) . . ? C68 C69 C70 122.9(6) . . ? C73 C69 C70 118.9(6) . . ? C72 C70 C69 113.4(6) . . ? C72 C70 C71 108.7(6) . . ? C69 C70 C71 111.6(5) . . ? C72 C70 H70 107.6 . . ? C69 C70 H70 107.6 . . ? C71 C70 H70 107.6 . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 C69 120.6(7) . . ? C74 C73 H73 119.7 . . ? C69 C73 H73 119.7 . . ? C75 C74 C73 120.2(7) . . ? C75 C74 H74 119.9 . . ? C73 C74 H74 119.9 . . ? C74 C75 C76 121.4(7) . . ? C74 C75 H75 119.3 . . ? C76 C75 H75 119.3 . . ? C75 C76 C68 118.8(7) . . ? C75 C76 C77 116.8(6) . . ? C68 C76 C77 124.4(6) . . ? C76 C77 C79 114.3(6) . . ? C76 C77 C78 109.9(6) . . ? C79 C77 C78 109.4(6) . . ? C76 C77 H77 107.7 . . ? C79 C77 H77 107.7 . . ? C78 C77 H77 107.7 . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C77 C79 H79A 109.5 . . ? C77 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C77 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C88 C80 C81 119.5(6) . . ? C88 C80 N4 121.1(5) . . ? C81 C80 N4 119.2(5) . . ? C85 C81 C80 118.4(6) . . ? C85 C81 C82 119.9(6) . . ? C80 C81 C82 121.7(6) . . ? C81 C82 C84 112.3(6) . . ? C81 C82 C83 112.5(5) . . ? C84 C82 C83 110.5(6) . . ? C81 C82 H82 107.1 . . ? C84 C82 H82 107.1 . . ? C83 C82 H82 107.1 . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C82 C84 H84A 109.5 . . ? C82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C86 C85 C81 123.1(6) . . ? C86 C85 H85 118.5 . . ? C81 C85 H85 118.5 . . ? C87 C86 C85 117.7(6) . . ? C87 C86 H86 121.1 . . ? C85 C86 H86 121.1 . . ? C86 C87 C88 122.4(7) . . ? C86 C87 H87 118.8 . . ? C88 C87 H87 118.8 . . ? C87 C88 C80 118.8(6) . . ? C87 C88 C89 118.0(6) . . ? C80 C88 C89 123.2(6) . . ? C90 C89 C88 112.5(5) . . ? C90 C89 C91 108.9(5) . . ? C88 C89 C91 112.4(5) . . ? C90 C89 H89 107.6 . . ? C88 C89 H89 107.6 . . ? C91 C89 H89 107.6 . . ? C89 C90 H90A 109.5 . . ? C89 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C89 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C89 C91 H91A 109.5 . . ? C89 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C89 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C30 N1 C37 120.8(5) . . ? C30 N1 Lu1 98.6(3) . . ? C37 N1 Lu1 136.3(4) . . ? C30 N2 C49 121.5(5) . . ? C30 N2 Lu1 92.0(4) . . ? C49 N2 Lu1 146.5(4) . . ? C61 N3 C68 121.5(5) . . ? C61 N3 Lu2 92.7(3) . . ? C68 N3 Lu2 145.0(4) . . ? C61 N4 C80 121.9(5) . . ? C61 N4 Lu2 97.6(3) . . ? C80 N4 Lu2 137.8(3) . . ? C21 O1 C18 107.8(6) . . ? C21 O1 Lu1 128.2(4) . . ? C18 O1 Lu1 123.4(4) . . ? C25 O2 C22 108.7(4) . . ? C25 O2 Lu1 124.1(4) . . ? C22 O2 Lu1 123.7(3) . . ? C29 O3 C26 108.9(5) . . ? C29 O3 Lu2 125.0(4) . . ? C26 O3 Lu2 125.6(3) . . ? O1 Lu1 N1 95.07(16) . . ? O1 Lu1 O2 85.91(16) . . ? N1 Lu1 O2 134.71(15) . . ? O1 Lu1 N2 94.73(16) . . ? N1 Lu1 N2 55.56(16) . . ? O2 Lu1 N2 79.20(15) . . ? O1 Lu1 C30 96.07(16) . . ? N1 Lu1 C30 27.57(15) . . ? O2 Lu1 C30 107.20(15) . . ? N2 Lu1 C30 28.01(16) . . ? O1 Lu1 Lu2 105.52(12) . . ? N1 Lu1 Lu2 114.21(11) . . ? O2 Lu1 Lu2 108.96(10) . . ? N2 Lu1 Lu2 158.48(11) . . ? C30 Lu1 Lu2 138.79(11) . . ? O1 Lu1 H1 81.3(14) . . ? N1 Lu1 H1 152.0(15) . . ? O2 Lu1 H1 73.0(15) . . ? N2 Lu1 H1 152.1(15) . . ? C30 Lu1 H1 177.3(14) . . ? Lu2 Lu1 H1 42.4(14) . . ? O1 Lu1 H3 146.5(15) . . ? N1 Lu1 H3 104.4(16) . . ? O2 Lu1 H3 98.7(16) . . ? N2 Lu1 H3 118.8(15) . . ? C30 Lu1 H3 113.8(15) . . ? Lu2 Lu1 H3 41.5(15) . . ? H1 Lu1 H3 69(2) . . ? O1 Lu1 H2 82.1(16) . . ? N1 Lu1 H2 86.5(16) . . ? O2 Lu1 H2 138.0(17) . . ? N2 Lu1 H2 141.6(16) . . ? C30 Lu1 H2 114.0(16) . . ? Lu2 Lu1 H2 38.7(16) . . ? H1 Lu1 H2 66(2) . . ? H3 Lu1 H2 72(2) . . ? O3 Lu2 N4 134.13(14) . . ? O3 Lu2 C5 88.71(18) . . ? N4 Lu2 C5 102.32(19) . . ? O3 Lu2 N3 79.04(15) . . ? N4 Lu2 N3 55.15(16) . . ? C5 Lu2 N3 102.6(2) . . ? O3 Lu2 C61 106.73(15) . . ? N4 Lu2 C61 27.48(16) . . ? C5 Lu2 C61 103.4(2) . . ? N3 Lu2 C61 27.69(16) . . ? O3 Lu2 Lu1 106.84(10) . . ? N4 Lu2 Lu1 109.27(11) . . ? C5 Lu2 Lu1 112.64(16) . . ? N3 Lu2 Lu1 144.21(11) . . ? C61 Lu2 Lu1 130.53(12) . . ? O3 Lu2 H1 137.1(13) . . ? N4 Lu2 H1 87.9(13) . . ? C5 Lu2 H1 90.1(12) . . ? N3 Lu2 H1 142.5(13) . . ? C61 Lu2 H1 115.3(13) . . ? Lu1 Lu2 H1 36.4(12) . . ? O3 Lu2 H3 105.1(16) . . ? N4 Lu2 H3 86.3(15) . . ? C5 Lu2 H3 151.1(15) . . ? N3 Lu2 H3 104.8(15) . . ? C61 Lu2 H3 96.8(15) . . ? Lu1 Lu2 H3 39.4(15) . . ? H1 Lu2 H3 62.5(19) . . ? O3 Lu2 H2 75.8(17) . . ? N4 Lu2 H2 147.4(17) . . ? C5 Lu2 H2 88.8(16) . . ? N3 Lu2 H2 152.1(17) . . ? C61 Lu2 H2 167.5(16) . . ? Lu1 Lu2 H2 39.2(17) . . ? H1 Lu2 H2 61(2) . . ? H3 Lu2 H2 71(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.931 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.116 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.000 0.000 0.000 279 53 ' ' 2 0.500 0.000 0.500 47 4 ' ' 3 0.420 0.478 0.426 11 1 ' ' 4 0.459 0.998 0.227 21 2 ' ' 5 0.540 1.001 0.773 21 2 ' ' 6 0.580 0.522 0.574 11 1 ' ' _platon_squeeze_details ; 1/2 disorder hexane molecule per formual unit of [(Ph-NCN)2Lu2H3(THF)3][PhCCHPh] was not modelled and the disordered density was taken into account using the SQUEEZE/PLATON procedure. (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194?01) as implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst. 2003, 36, 7?3. PLATON - a multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands). ; data_4-Lu-b _database_code_depnum_ccdc_archive 'CCDC 859488' #TrackingRef '- Ln2H4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (PhNCNLuH(THF))2(PhCHCHPh) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H108 Lu2 N4 O2' _chemical_formula_weight 1555.68 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' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.530(5) _cell_length_b 16.733(5) _cell_length_c 22.194(5) _cell_angle_alpha 107.824(5) _cell_angle_beta 103.291(5) _cell_angle_gamma 91.970(5) _cell_volume 4284(2) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Fragment _exptl_crystal_colour Red-orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 2.333 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5611 _exptl_absorpt_correction_T_max 0.7210 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 23135 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0945 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14821 _reflns_number_gt 10053 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0444P)^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 14821 _refine_ls_number_parameters 851 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1081 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.928 _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 C3 C 0.7769(6) 0.8232(4) 0.4504(3) 0.0348(17) Uani 1 1 d D . . C4 C 0.7171(6) 0.8710(4) 0.4081(3) 0.0363(17) Uani 1 1 d D B . C5 C 0.7490(6) 0.9568(4) 0.4124(3) 0.0304(16) Uani 1 1 d . B . C6 C 0.6836(6) 0.9970(5) 0.3728(3) 0.0417(18) Uani 1 1 d D B . C7 C 0.7118(8) 1.0775(4) 0.3732(3) 0.053(2) Uani 1 1 d . . . H7 H 0.6633 1.1022 0.3461 0.064 Uiso 1 1 calc R . . C8 C 0.8091(8) 1.1213(5) 0.4122(4) 0.063(3) Uani 1 1 d . . . H8 H 0.8298 1.1766 0.4126 0.076 Uiso 1 1 calc R . . C9 C 0.8787(7) 1.0836(5) 0.4523(3) 0.053(2) Uani 1 1 d . . . H9 H 0.9470 1.1137 0.4799 0.064 Uiso 1 1 calc R . . C10 C 0.8490(6) 1.0034(4) 0.4519(3) 0.0367(17) Uani 1 1 d . . . H10 H 0.8978 0.9790 0.4791 0.044 Uiso 1 1 calc R . . C11 C 0.7693(6) 0.8418(4) 0.5184(3) 0.0389(18) Uani 1 1 d . . . C12 C 0.8413(7) 0.8087(5) 0.5611(4) 0.049(2) Uani 1 1 d . . . H12 H 0.8987 0.7785 0.5470 0.059 Uiso 1 1 calc R . . C13 C 0.8296(9) 0.8194(5) 0.6224(4) 0.069(3) Uani 1 1 d . . . H13 H 0.8801 0.7968 0.6502 0.083 Uiso 1 1 calc R . . C14 C 0.7488(10) 0.8611(6) 0.6458(4) 0.075(3) Uani 1 1 d . . . H14 H 0.7413 0.8665 0.6885 0.090 Uiso 1 1 calc R . . C15 C 0.6789(8) 0.8949(6) 0.6057(5) 0.072(3) Uani 1 1 d . . . H15 H 0.6215 0.9244 0.6205 0.086 Uiso 1 1 calc R . . C16 C 0.6909(7) 0.8866(5) 0.5438(4) 0.053(2) Uani 1 1 d . . . H16 H 0.6430 0.9128 0.5176 0.064 Uiso 1 1 calc R . . C17 C 0.4293(7) 0.8103(5) 0.4033(4) 0.052(2) Uani 1 1 d . . . H17A H 0.3884 0.8019 0.3576 0.062 Uiso 1 1 calc R . . H17B H 0.4685 0.8682 0.4222 0.062 Uiso 1 1 calc R . . C18 C 0.3525(9) 0.7983(7) 0.4420(6) 0.092(4) Uani 1 1 d . . . H18A H 0.3320 0.8534 0.4662 0.110 Uiso 1 1 calc R . . H18B H 0.2844 0.7621 0.4131 0.110 Uiso 1 1 calc R . . C19 C 0.4114(8) 0.7576(6) 0.4874(4) 0.071(3) Uani 1 1 d . . . H19A H 0.3597 0.7175 0.4947 0.085 Uiso 1 1 calc R . . H19B H 0.4480 0.8003 0.5300 0.085 Uiso 1 1 calc R . . C20 C 0.4961(7) 0.7113(5) 0.4555(4) 0.048(2) Uani 1 1 d . . . H20A H 0.5676 0.7190 0.4881 0.057 Uiso 1 1 calc R . . H20B H 0.4708 0.6501 0.4355 0.057 Uiso 1 1 calc R . . C21 C 0.9432(7) 0.9559(5) 0.2923(4) 0.053(2) Uani 1 1 d . . . H21A H 0.9297 1.0126 0.3182 0.064 Uiso 1 1 calc R A 1 H21B H 0.9103 0.9473 0.2454 0.064 Uiso 1 1 calc R A 1 C22 C 1.057(3) 0.977(3) 0.341(3) 0.074(6) Uani 0.33(3) 1 d P B 2 H22A H 1.1111 0.9996 0.3227 0.089 Uiso 0.33(3) 1 calc PR B 2 H22B H 1.0531 1.0201 0.3823 0.089 Uiso 0.33(3) 1 calc PR B 2 C22' C 1.0628(14) 0.9491(16) 0.3039(14) 0.074(6) Uani 0.67(3) 1 d P B 1 H22C H 1.1052 1.0058 0.3208 0.089 Uiso 0.67(3) 1 calc PR B 1 H22D H 1.0813 0.9165 0.2629 0.089 Uiso 0.67(3) 1 calc PR B 1 C23 C 1.0879(7) 0.9047(7) 0.3529(5) 0.083(3) Uani 1 1 d . . . H23A H 1.1254 0.9453 0.3963 0.099 Uiso 1 1 calc R B 1 H23B H 1.1375 0.8612 0.3403 0.099 Uiso 1 1 calc R B 1 C24 C 0.9823(6) 0.8643(5) 0.3558(4) 0.049(2) Uani 1 1 d . B . H24A H 0.9806 0.8021 0.3410 0.059 Uiso 1 1 calc R . . H24B H 0.9736 0.8834 0.4011 0.059 Uiso 1 1 calc R . . C25 C 0.6517(5) 0.5467(4) 0.3500(3) 0.0286(15) Uani 1 1 d . . . C26 C 0.6433(5) 0.4565(4) 0.3488(3) 0.0282(15) Uani 1 1 d . . . C27 C 0.5392(6) 0.4126(5) 0.3362(3) 0.0377(17) Uani 1 1 d . . . H27 H 0.4748 0.4404 0.3297 0.045 Uiso 1 1 calc R . . C28 C 0.5297(6) 0.3270(4) 0.3332(3) 0.0423(19) Uani 1 1 d . . . H28 H 0.4588 0.2970 0.3236 0.051 Uiso 1 1 calc R . . C29 C 0.6225(7) 0.2869(4) 0.3440(4) 0.047(2) Uani 1 1 d . . . H29 H 0.6159 0.2292 0.3416 0.056 Uiso 1 1 calc R . . C30 C 0.7251(7) 0.3305(5) 0.3583(3) 0.045(2) Uani 1 1 d . . . H30 H 0.7895 0.3031 0.3663 0.055 Uiso 1 1 calc R . . C31 C 0.7349(6) 0.4154(4) 0.3610(3) 0.0396(18) Uani 1 1 d . . . H31 H 0.8062 0.4450 0.3715 0.047 Uiso 1 1 calc R . . C32 C 0.5123(5) 0.5167(4) 0.2482(3) 0.0292(15) Uani 1 1 d . . . C33 C 0.3981(6) 0.5214(4) 0.2341(3) 0.0364(17) Uani 1 1 d . . . C34 C 0.3438(6) 0.5827(5) 0.2800(4) 0.0457(19) Uani 1 1 d . . . H34 H 0.4033 0.6149 0.3195 0.055 Uiso 1 1 calc R . . C35 C 0.2915(8) 0.6468(5) 0.2496(4) 0.066(3) Uani 1 1 d . . . H35A H 0.3471 0.6750 0.2360 0.100 Uiso 1 1 calc R . . H35B H 0.2630 0.6889 0.2818 0.100 Uiso 1 1 calc R . . H35C H 0.2307 0.6177 0.2114 0.100 Uiso 1 1 calc R . . C36 C 0.2613(8) 0.5402(6) 0.3029(4) 0.072(3) Uani 1 1 d . . . H36A H 0.2295 0.5831 0.3327 0.108 Uiso 1 1 calc R . . H36B H 0.2980 0.5032 0.3259 0.108 Uiso 1 1 calc R . . H36C H 0.2025 0.5066 0.2652 0.108 Uiso 1 1 calc R . . C37 C 0.3314(7) 0.4670(5) 0.1764(3) 0.047(2) Uani 1 1 d . . . H37 H 0.2543 0.4711 0.1665 0.056 Uiso 1 1 calc R . . C38 C 0.3738(7) 0.4066(5) 0.1328(4) 0.050(2) Uani 1 1 d . . . H38 H 0.3261 0.3676 0.0946 0.061 Uiso 1 1 calc R . . C39 C 0.4846(6) 0.4042(5) 0.1454(3) 0.0449(19) Uani 1 1 d . . . H39 H 0.5136 0.3639 0.1146 0.054 Uiso 1 1 calc R . . C40 C 0.5585(6) 0.4588(4) 0.2022(3) 0.0332(16) Uani 1 1 d . . . C41 C 0.6793(6) 0.4553(4) 0.2097(3) 0.0404(18) Uani 1 1 d . . . H41 H 0.7159 0.4849 0.2570 0.048 Uiso 1 1 calc R . . C42 C 0.7160(8) 0.3661(5) 0.1930(4) 0.066(3) Uani 1 1 d . . . H42A H 0.7963 0.3702 0.1997 0.099 Uiso 1 1 calc R . . H42B H 0.6805 0.3341 0.1472 0.099 Uiso 1 1 calc R . . H42C H 0.6944 0.3371 0.2214 0.099 Uiso 1 1 calc R . . C43 C 0.7232(7) 0.5058(6) 0.1705(4) 0.060(2) Uani 1 1 d . . . H43A H 0.8029 0.5034 0.1765 0.090 Uiso 1 1 calc R . . H43B H 0.7087 0.5648 0.1863 0.090 Uiso 1 1 calc R . . H43C H 0.6858 0.4812 0.1240 0.090 Uiso 1 1 calc R . . C44 C 0.8122(6) 0.5993(4) 0.4465(3) 0.0274(15) Uani 1 1 d . . . C45 C 0.7866(6) 0.5808(4) 0.5002(3) 0.0325(16) Uani 1 1 d . . . C46 C 0.6708(6) 0.5614(4) 0.5055(3) 0.0365(17) Uani 1 1 d . . . H46 H 0.6169 0.5637 0.4653 0.044 Uiso 1 1 calc R . . C47 C 0.6533(7) 0.4729(5) 0.5118(3) 0.052(2) Uani 1 1 d . . . H47A H 0.5776 0.4622 0.5148 0.078 Uiso 1 1 calc R . . H47B H 0.7054 0.4701 0.5513 0.078 Uiso 1 1 calc R . . H47C H 0.6657 0.4301 0.4734 0.078 Uiso 1 1 calc R . . C48 C 0.6475(6) 0.6268(5) 0.5656(3) 0.0450(19) Uani 1 1 d . . . H48A H 0.5720 0.6137 0.5679 0.068 Uiso 1 1 calc R . . H48B H 0.6559 0.6834 0.5619 0.068 Uiso 1 1 calc R . . H48C H 0.6998 0.6249 0.6054 0.068 Uiso 1 1 calc R . . C49 C 0.8733(6) 0.5837(5) 0.5529(3) 0.0438(19) Uani 1 1 d . . . H49 H 0.8571 0.5715 0.5892 0.053 Uiso 1 1 calc R . . C50 C 0.9807(6) 0.6032(5) 0.5547(4) 0.048(2) Uani 1 1 d . . . H50 H 1.0379 0.6062 0.5921 0.058 Uiso 1 1 calc R . . C51 C 1.0058(6) 0.6187(5) 0.5005(3) 0.0439(19) Uani 1 1 d . . . H51 H 1.0806 0.6302 0.5006 0.053 Uiso 1 1 calc R . . C52 C 0.9218(5) 0.6174(4) 0.4465(3) 0.0308(16) Uani 1 1 d . . . C53 C 0.9561(5) 0.6331(5) 0.3891(3) 0.0378(17) Uani 1 1 d . . . H53 H 0.8963 0.6615 0.3683 0.045 Uiso 1 1 calc R . . C54 C 0.9620(6) 0.5505(5) 0.3373(4) 0.048(2) Uani 1 1 d . . . H54A H 0.8928 0.5136 0.3255 0.072 Uiso 1 1 calc R . . H54B H 1.0236 0.5225 0.3546 0.072 Uiso 1 1 calc R . . H54C H 0.9735 0.5621 0.2984 0.072 Uiso 1 1 calc R . . C55 C 1.0615(6) 0.6905(5) 0.4075(4) 0.0459(19) Uani 1 1 d . . . H55A H 1.0771 0.6975 0.3680 0.069 Uiso 1 1 calc R . . H55B H 1.1223 0.6658 0.4293 0.069 Uiso 1 1 calc R . . H55C H 1.0539 0.7457 0.4373 0.069 Uiso 1 1 calc R . . C56 C 0.6637(5) 0.8520(4) 0.1593(3) 0.0290(15) Uani 1 1 d . B . C57 C 0.6486(6) 0.8589(4) 0.0925(3) 0.0380(18) Uani 1 1 d . . . C58 C 0.7350(7) 0.8457(5) 0.0616(4) 0.051(2) Uani 1 1 d . . . H58 H 0.8030 0.8329 0.0841 0.061 Uiso 1 1 calc R . . C59 C 0.7251(9) 0.8506(6) -0.0001(4) 0.072(3) Uani 1 1 d . . . H59 H 0.7847 0.8409 -0.0203 0.087 Uiso 1 1 calc R . . C60 C 0.6261(11) 0.8702(6) -0.0323(5) 0.084(3) Uani 1 1 d . . . H60 H 0.6173 0.8728 -0.0753 0.101 Uiso 1 1 calc R . . C61 C 0.5418(9) 0.8855(6) -0.0032(4) 0.073(3) Uani 1 1 d . . . H61 H 0.4754 0.9002 -0.0258 0.088 Uiso 1 1 calc R . . C62 C 0.5501(7) 0.8800(5) 0.0596(4) 0.052(2) Uani 1 1 d . . . H62 H 0.4899 0.8904 0.0793 0.062 Uiso 1 1 calc R . . C63 C 0.7193(6) 0.7142(4) 0.1255(3) 0.0309(16) Uani 1 1 d . . . C64 C 0.8221(6) 0.6859(4) 0.1218(3) 0.0348(17) Uani 1 1 d . . . C65 C 0.9286(6) 0.7324(5) 0.1707(4) 0.048(2) Uani 1 1 d . . . H65 H 0.9106 0.7868 0.1987 0.057 Uiso 1 1 calc R . . C66 C 0.9713(7) 0.6808(5) 0.2143(4) 0.064(3) Uani 1 1 d . . . H66A H 1.0397 0.7106 0.2463 0.096 Uiso 1 1 calc R . . H66B H 0.9860 0.6257 0.1877 0.096 Uiso 1 1 calc R . . H66C H 0.9160 0.6725 0.2373 0.096 Uiso 1 1 calc R . . C67 C 1.0169(7) 0.7534(5) 0.1398(5) 0.068(3) Uani 1 1 d . . . H67A H 1.0827 0.7832 0.1742 0.102 Uiso 1 1 calc R . . H67B H 0.9894 0.7894 0.1135 0.102 Uiso 1 1 calc R . . H67C H 1.0360 0.7011 0.1117 0.102 Uiso 1 1 calc R . . C68 C 0.8278(6) 0.6117(4) 0.0713(3) 0.0401(18) Uani 1 1 d . . . H68 H 0.8973 0.5920 0.0689 0.048 Uiso 1 1 calc R . . C69 C 0.7340(7) 0.5677(5) 0.0257(3) 0.050(2) Uani 1 1 d . . . H69 H 0.7393 0.5200 -0.0097 0.061 Uiso 1 1 calc R . . C70 C 0.6310(6) 0.5932(4) 0.0315(3) 0.0412(18) Uani 1 1 d . . . H70 H 0.5663 0.5607 0.0010 0.049 Uiso 1 1 calc R . . C71 C 0.6210(6) 0.6641(4) 0.0802(3) 0.0349(17) Uani 1 1 d . . . C72 C 0.5061(6) 0.6846(4) 0.0870(3) 0.0351(17) Uani 1 1 d . . . H72 H 0.5122 0.7453 0.1142 0.042 Uiso 1 1 calc R . . C73 C 0.4649(6) 0.6311(5) 0.1238(4) 0.047(2) Uani 1 1 d . . . H73A H 0.3910 0.6442 0.1285 0.071 Uiso 1 1 calc R . . H73B H 0.5155 0.6437 0.1672 0.071 Uiso 1 1 calc R . . H73C H 0.4618 0.5710 0.0993 0.071 Uiso 1 1 calc R . . C74 C 0.4240(6) 0.6725(5) 0.0216(3) 0.050(2) Uani 1 1 d . . . H74A H 0.3518 0.6865 0.0289 0.074 Uiso 1 1 calc R . . H74B H 0.4175 0.6136 -0.0064 0.074 Uiso 1 1 calc R . . H74C H 0.4501 0.7097 0.0001 0.074 Uiso 1 1 calc R . . C75 C 0.5775(6) 0.9797(4) 0.2032(3) 0.0313(16) Uani 1 1 d . . . C76 C 0.4695(6) 0.9761(5) 0.2090(3) 0.0421(19) Uani 1 1 d . . . C77 C 0.4089(6) 0.8961(5) 0.2111(4) 0.052(2) Uani 1 1 d . . . H77 H 0.4647 0.8554 0.2152 0.063 Uiso 1 1 calc R . . C78 C 0.3573(7) 0.9094(6) 0.2676(4) 0.066(3) Uani 1 1 d . . . H78A H 0.4136 0.9360 0.3087 0.099 Uiso 1 1 calc R . . H78B H 0.3262 0.8547 0.2674 0.099 Uiso 1 1 calc R . . H78C H 0.2985 0.9460 0.2636 0.099 Uiso 1 1 calc R . . C79 C 0.3205(7) 0.8536(5) 0.1481(4) 0.063(2) Uani 1 1 d . . . H79A H 0.3532 0.8436 0.1107 0.094 Uiso 1 1 calc R . . H79B H 0.2617 0.8902 0.1439 0.094 Uiso 1 1 calc R . . H79C H 0.2895 0.7996 0.1491 0.094 Uiso 1 1 calc R . . C80 C 0.4119(7) 1.0445(5) 0.2089(4) 0.048(2) Uani 1 1 d . . . H80 H 0.3375 1.0413 0.2117 0.058 Uiso 1 1 calc R . . C81 C 0.4594(7) 1.1174(5) 0.2048(3) 0.051(2) Uani 1 1 d . . . H81 H 0.4192 1.1649 0.2065 0.062 Uiso 1 1 calc R . . C82 C 0.5654(6) 1.1204(4) 0.1983(3) 0.0433(19) Uani 1 1 d . . . H82 H 0.5979 1.1702 0.1945 0.052 Uiso 1 1 calc R . . C83 C 0.6264(7) 1.0527(5) 0.1971(3) 0.0425(19) Uani 1 1 d . . . C84 C 0.7429(6) 1.0611(4) 0.1875(3) 0.0427(19) Uani 1 1 d . . . H84 H 0.7750 1.0071 0.1869 0.051 Uiso 1 1 calc R . . C85 C 0.8192(7) 1.1338(5) 0.2441(4) 0.055(2) Uani 1 1 d . . . H85A H 0.8931 1.1366 0.2367 0.083 Uiso 1 1 calc R . . H85B H 0.8236 1.1233 0.2857 0.083 Uiso 1 1 calc R . . H85C H 0.7890 1.1875 0.2459 0.083 Uiso 1 1 calc R . . C86 C 0.7445(7) 1.0766(5) 0.1234(4) 0.058(2) Uani 1 1 d . . . H86A H 0.8206 1.0801 0.1193 0.088 Uiso 1 1 calc R . . H86B H 0.7142 1.1298 0.1231 0.088 Uiso 1 1 calc R . . H86C H 0.6997 1.0300 0.0866 0.088 Uiso 1 1 calc R . . N1 N 0.5816(4) 0.5730(3) 0.3073(2) 0.0263(12) Uani 1 1 d . . . N2 N 0.7285(4) 0.6073(3) 0.3932(2) 0.0303(13) Uani 1 1 d . . . N3 N 0.7107(4) 0.7885(3) 0.1754(2) 0.0270(12) Uani 1 1 d . B . N4 N 0.6387(5) 0.9101(3) 0.2093(3) 0.0324(13) Uani 1 1 d . B . O1 O 0.5070(4) 0.7489(3) 0.4052(2) 0.0371(11) Uani 1 1 d . . . O2 O 0.8945(4) 0.8906(3) 0.3122(2) 0.0351(11) Uani 1 1 d . B . Lu1 Lu 0.65650(2) 0.717086(17) 0.358952(13) 0.02708(9) Uani 1 1 d . B . Lu2 Lu 0.71174(2) 0.845072(17) 0.285567(13) 0.02740(9) Uani 1 1 d . . . H2 H 0.576(5) 0.768(4) 0.285(3) 0.039(18) Uiso 1 1 d . . . H1 H 0.751(6) 0.720(5) 0.302(4) 0.08(3) Uiso 1 1 d . . . H3 H 0.8543(19) 0.814(4) 0.448(3) 0.027(17) Uiso 1 1 d D . . H6 H 0.6071(15) 0.980(4) 0.355(3) 0.050 Uiso 1 1 d D . . H4 H 0.6392(19) 0.844(4) 0.389(3) 0.050 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C3 0.038(4) 0.034(4) 0.031(4) 0.011(3) 0.006(3) 0.002(3) C4 0.039(4) 0.031(4) 0.026(4) -0.001(3) -0.001(3) 0.001(3) C5 0.037(4) 0.030(4) 0.026(4) 0.010(3) 0.009(3) 0.004(3) C6 0.040(5) 0.048(5) 0.028(4) 0.008(3) -0.003(3) 0.005(4) C7 0.093(7) 0.022(4) 0.034(4) 0.007(3) -0.003(4) 0.017(4) C8 0.104(8) 0.024(4) 0.049(5) 0.012(4) -0.006(5) -0.002(5) C9 0.077(6) 0.040(5) 0.032(4) 0.007(4) 0.004(4) -0.025(4) C10 0.045(5) 0.027(4) 0.029(4) 0.004(3) -0.002(3) 0.000(3) C11 0.043(5) 0.030(4) 0.035(4) 0.009(3) -0.002(4) -0.008(3) C12 0.067(6) 0.036(5) 0.037(5) 0.007(4) 0.007(4) -0.010(4) C13 0.117(9) 0.048(6) 0.029(5) 0.010(4) 0.000(5) -0.024(6) C14 0.106(9) 0.068(7) 0.037(5) 0.000(5) 0.023(6) -0.033(6) C15 0.071(7) 0.074(7) 0.052(6) -0.013(5) 0.030(5) -0.014(5) C16 0.048(5) 0.052(5) 0.039(5) -0.009(4) 0.007(4) -0.013(4) C17 0.045(5) 0.053(5) 0.064(6) 0.025(4) 0.015(4) 0.019(4) C18 0.075(8) 0.123(9) 0.133(10) 0.087(8) 0.066(7) 0.044(7) C19 0.066(7) 0.099(8) 0.062(6) 0.034(6) 0.031(5) 0.013(6) C20 0.058(5) 0.044(5) 0.049(5) 0.023(4) 0.019(4) 0.005(4) C21 0.053(5) 0.036(5) 0.071(6) 0.028(4) 0.003(4) -0.002(4) C22 0.041(7) 0.110(16) 0.093(17) 0.061(15) 0.023(11) -0.014(8) C22' 0.041(7) 0.110(16) 0.093(17) 0.061(15) 0.023(11) -0.014(8) C23 0.037(6) 0.134(10) 0.077(7) 0.053(7) -0.008(5) -0.009(6) C24 0.035(5) 0.063(6) 0.050(5) 0.023(4) 0.003(4) 0.013(4) C25 0.033(4) 0.027(4) 0.023(3) 0.004(3) 0.007(3) -0.006(3) C26 0.036(4) 0.028(4) 0.020(3) 0.011(3) 0.002(3) 0.002(3) C27 0.038(4) 0.045(5) 0.032(4) 0.014(3) 0.011(3) 0.002(4) C28 0.047(5) 0.033(4) 0.041(4) 0.011(3) 0.003(4) -0.007(4) C29 0.065(6) 0.023(4) 0.046(5) 0.009(3) 0.007(4) -0.002(4) C30 0.056(5) 0.035(5) 0.045(5) 0.019(4) 0.003(4) 0.008(4) C31 0.037(4) 0.039(5) 0.042(4) 0.016(4) 0.003(3) 0.004(3) C32 0.032(4) 0.029(4) 0.023(4) 0.011(3) -0.003(3) -0.008(3) C33 0.037(4) 0.039(4) 0.031(4) 0.013(3) 0.003(3) -0.004(3) C34 0.034(4) 0.057(5) 0.043(5) 0.014(4) 0.006(4) 0.005(4) C35 0.068(7) 0.069(6) 0.067(6) 0.021(5) 0.027(5) 0.022(5) C36 0.069(7) 0.094(8) 0.063(6) 0.028(6) 0.033(5) 0.014(6) C37 0.044(5) 0.062(5) 0.027(4) 0.011(4) -0.002(4) -0.007(4) C38 0.049(5) 0.054(5) 0.037(5) 0.006(4) 0.002(4) -0.013(4) C39 0.050(5) 0.048(5) 0.029(4) 0.002(4) 0.010(4) -0.001(4) C40 0.034(4) 0.041(4) 0.020(4) 0.011(3) -0.001(3) -0.002(3) C41 0.050(5) 0.036(4) 0.030(4) 0.005(3) 0.008(3) 0.004(4) C42 0.071(7) 0.042(5) 0.081(7) 0.015(5) 0.017(5) 0.026(5) C43 0.040(5) 0.093(7) 0.058(5) 0.037(5) 0.018(4) -0.005(5) C44 0.038(4) 0.018(3) 0.024(4) 0.007(3) 0.001(3) 0.002(3) C45 0.032(4) 0.029(4) 0.033(4) 0.007(3) 0.007(3) 0.006(3) C46 0.043(5) 0.035(4) 0.033(4) 0.016(3) 0.005(3) 0.004(3) C47 0.070(6) 0.050(5) 0.031(4) 0.014(4) 0.002(4) -0.007(4) C48 0.053(5) 0.045(5) 0.037(4) 0.013(4) 0.014(4) -0.002(4) C49 0.042(5) 0.053(5) 0.033(4) 0.018(4) -0.002(3) 0.000(4) C50 0.037(5) 0.062(6) 0.041(5) 0.021(4) -0.008(4) 0.002(4) C51 0.021(4) 0.059(5) 0.047(5) 0.016(4) 0.000(3) 0.006(4) C52 0.030(4) 0.030(4) 0.029(4) 0.010(3) -0.002(3) 0.005(3) C53 0.020(4) 0.050(5) 0.043(4) 0.019(4) 0.002(3) 0.002(3) C54 0.043(5) 0.058(5) 0.044(5) 0.018(4) 0.012(4) 0.003(4) C55 0.042(5) 0.049(5) 0.048(5) 0.016(4) 0.013(4) 0.010(4) C56 0.025(4) 0.031(4) 0.022(3) 0.005(3) -0.004(3) -0.011(3) C57 0.057(5) 0.025(4) 0.028(4) 0.008(3) 0.005(4) 0.000(3) C58 0.069(6) 0.044(5) 0.045(5) 0.020(4) 0.019(4) 0.007(4) C59 0.097(8) 0.080(7) 0.055(6) 0.035(5) 0.028(6) 0.026(6) C60 0.137(11) 0.081(8) 0.040(6) 0.026(5) 0.024(7) 0.010(7) C61 0.102(9) 0.062(6) 0.044(6) 0.030(5) -0.019(5) 0.002(6) C62 0.073(6) 0.037(5) 0.037(5) 0.010(4) 0.002(4) -0.005(4) C63 0.039(4) 0.026(4) 0.030(4) 0.012(3) 0.007(3) 0.006(3) C64 0.044(5) 0.032(4) 0.026(4) 0.009(3) 0.005(3) 0.002(3) C65 0.049(5) 0.040(5) 0.046(5) 0.001(4) 0.015(4) -0.003(4) C66 0.053(6) 0.073(7) 0.049(5) 0.004(5) 0.002(4) 0.010(5) C67 0.055(6) 0.056(6) 0.087(7) 0.016(5) 0.020(5) -0.013(5) C68 0.040(5) 0.038(4) 0.047(5) 0.015(4) 0.019(4) 0.011(4) C69 0.084(7) 0.033(4) 0.028(4) -0.001(3) 0.017(4) 0.007(4) C70 0.042(5) 0.036(4) 0.036(4) -0.003(3) 0.011(4) 0.007(4) C71 0.042(4) 0.032(4) 0.034(4) 0.015(3) 0.009(3) 0.000(3) C72 0.038(4) 0.033(4) 0.028(4) 0.005(3) 0.003(3) 0.003(3) C73 0.046(5) 0.045(5) 0.048(5) 0.011(4) 0.013(4) -0.002(4) C74 0.047(5) 0.059(5) 0.037(4) 0.013(4) 0.002(4) 0.006(4) C75 0.033(4) 0.031(4) 0.022(4) 0.006(3) -0.005(3) 0.001(3) C76 0.041(5) 0.037(5) 0.045(5) 0.013(4) 0.004(4) 0.015(4) C77 0.036(5) 0.049(5) 0.077(6) 0.029(5) 0.012(4) 0.020(4) C78 0.049(6) 0.072(7) 0.079(7) 0.034(5) 0.007(5) 0.007(5) C79 0.043(5) 0.062(6) 0.072(6) 0.009(5) 0.012(5) -0.002(4) C80 0.042(5) 0.048(5) 0.052(5) 0.014(4) 0.008(4) 0.015(4) C81 0.060(6) 0.040(5) 0.040(5) 0.003(4) -0.004(4) 0.017(4) C82 0.047(5) 0.028(4) 0.047(5) 0.010(3) 0.000(4) 0.010(4) C83 0.058(5) 0.039(5) 0.027(4) 0.012(3) 0.002(4) 0.007(4) C84 0.051(5) 0.033(4) 0.041(4) 0.016(4) 0.001(4) 0.000(4) C85 0.062(6) 0.053(5) 0.043(5) 0.013(4) 0.003(4) -0.004(4) C86 0.077(7) 0.049(5) 0.058(5) 0.028(4) 0.019(5) 0.013(5) N1 0.028(3) 0.024(3) 0.023(3) 0.007(2) 0.000(2) 0.002(2) N2 0.030(3) 0.034(3) 0.028(3) 0.014(3) 0.004(3) 0.003(3) N3 0.033(3) 0.016(3) 0.026(3) 0.005(2) -0.002(2) 0.003(2) N4 0.038(4) 0.022(3) 0.030(3) 0.006(3) -0.002(3) 0.006(3) O1 0.035(3) 0.038(3) 0.042(3) 0.017(2) 0.011(2) 0.005(2) O2 0.028(3) 0.041(3) 0.036(3) 0.020(2) -0.002(2) -0.004(2) Lu1 0.02716(18) 0.02581(18) 0.02628(17) 0.00826(13) 0.00344(13) 0.00073(13) Lu2 0.02890(18) 0.02588(18) 0.02443(17) 0.00776(13) 0.00175(13) 0.00108(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 C3 C11 1.472(9) . ? C3 C4 1.503(9) . ? C3 Lu1 2.398(7) . ? C3 H3 0.998(10) . ? C4 C5 1.445(9) . ? C4 Lu1 2.483(7) . ? C4 Lu2 2.604(7) . ? C4 H4 1.000(5) . ? C5 C10 1.398(9) . ? C5 C6 1.402(9) . ? C5 Lu2 2.785(6) . ? C6 C7 1.377(10) . ? C6 Lu2 2.775(7) . ? C6 H6 0.946(10) . ? C7 C8 1.356(11) . ? C7 H7 0.9500 . ? C8 C9 1.405(10) . ? C8 H8 0.9500 . ? C9 C10 1.377(9) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C16 1.374(10) . ? C11 C12 1.408(10) . ? C12 C13 1.360(10) . ? C12 H12 0.9500 . ? C13 C14 1.360(13) . ? C13 H13 0.9500 . ? C14 C15 1.365(13) . ? C14 H14 0.9500 . ? C15 C16 1.382(11) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 O1 1.443(8) . ? C17 C18 1.476(11) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.462(12) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.515(10) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O1 1.469(8) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 O2 1.463(8) . ? C21 C22' 1.476(19) . ? C21 C22 1.53(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.36(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22' C23 1.48(2) . ? C22' H22C 0.9900 . ? C22' H22D 0.9900 . ? C23 C24 1.488(11) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O2 1.464(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 N1 1.328(8) . ? C25 N2 1.336(8) . ? C25 C26 1.501(9) . ? C25 Lu1 2.794(6) . ? C26 C31 1.374(9) . ? C26 C27 1.399(9) . ? C27 C28 1.413(9) . ? C27 H27 0.9500 . ? C28 C29 1.371(10) . ? C28 H28 0.9500 . ? C29 C30 1.376(10) . ? C29 H29 0.9500 . ? C30 C31 1.402(9) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.403(9) . ? C32 C40 1.421(9) . ? C32 N1 1.423(8) . ? C33 C37 1.381(9) . ? C33 C34 1.510(10) . ? C34 C36 1.498(11) . ? C34 C35 1.523(10) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.384(10) . ? C37 H37 0.9500 . ? C38 C39 1.357(10) . ? C38 H38 0.9500 . ? C39 C40 1.408(9) . ? C39 H39 0.9500 . ? C40 C41 1.490(10) . ? C41 C42 1.537(9) . ? C41 C43 1.554(10) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C52 1.396(9) . ? C44 C45 1.420(9) . ? C44 N2 1.433(8) . ? C45 C49 1.388(9) . ? C45 C46 1.515(9) . ? C46 C48 1.539(9) . ? C46 C47 1.544(9) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.362(10) . ? C49 H49 0.9500 . ? C50 C51 1.404(10) . ? C50 H50 0.9500 . ? C51 C52 1.395(9) . ? C51 H51 0.9500 . ? C52 C53 1.526(9) . ? C53 C55 1.503(9) . ? C53 C54 1.521(10) . ? C53 H53 1.0000 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 N3 1.335(8) . ? C56 N4 1.341(8) . ? C56 C57 1.491(9) . ? C56 Lu2 2.767(6) . ? C57 C58 1.398(10) . ? C57 C62 1.400(10) . ? C58 C59 1.376(10) . ? C58 H58 0.9500 . ? C59 C60 1.385(13) . ? C59 H59 0.9500 . ? C60 C61 1.353(13) . ? C60 H60 0.9500 . ? C61 C62 1.405(11) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C64 1.399(9) . ? C63 N3 1.415(8) . ? C63 C71 1.440(9) . ? C64 C68 1.412(9) . ? C64 C65 1.519(10) . ? C65 C66 1.509(10) . ? C65 C67 1.512(10) . ? C65 H65 1.0000 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C69 1.373(10) . ? C68 H68 0.9500 . ? C69 C70 1.395(10) . ? C69 H69 0.9500 . ? C70 C71 1.372(9) . ? C70 H70 0.9500 . ? C71 C72 1.522(9) . ? C72 C74 1.526(9) . ? C72 C73 1.531(9) . ? C72 H72 1.0000 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C76 1.390(10) . ? C75 C83 1.406(10) . ? C75 N4 1.440(8) . ? C76 C80 1.373(9) . ? C76 C77 1.535(10) . ? C77 C78 1.500(11) . ? C77 C79 1.521(11) . ? C77 H77 1.0000 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 C81 1.376(11) . ? C80 H80 0.9500 . ? C81 C82 1.370(11) . ? C81 H81 0.9500 . ? C82 C83 1.386(9) . ? C82 H82 0.9500 . ? C83 C84 1.530(10) . ? C84 C86 1.528(9) . ? C84 C85 1.550(10) . ? C84 H84 1.0000 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? N1 Lu1 2.381(5) . ? N2 Lu1 2.327(5) . ? N3 Lu2 2.332(5) . ? N4 Lu2 2.317(5) . ? O1 Lu1 2.337(5) . ? O2 Lu2 2.270(4) . ? Lu1 Lu2 3.2047(7) . ? Lu1 H2 2.14(6) . ? Lu1 H1 1.93(7) . ? Lu1 H4 2.06(7) . ? Lu2 H2 2.09(6) . ? Lu2 H1 2.28(7) . ? 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 C11 C3 C4 120.7(6) . . ? C11 C3 Lu1 123.9(5) . . ? C4 C3 Lu1 75.2(4) . . ? C11 C3 H3 110(3) . . ? C4 C3 H3 116(3) . . ? Lu1 C3 H3 108(3) . . ? C5 C4 C3 126.0(6) . . ? C5 C4 Lu1 159.5(5) . . ? C3 C4 Lu1 69.0(4) . . ? C5 C4 Lu2 81.5(4) . . ? C3 C4 Lu2 126.1(5) . . ? Lu1 C4 Lu2 78.06(19) . . ? C5 C4 H4 122(4) . . ? C3 C4 H4 109(4) . . ? Lu1 C4 H4 54(4) . . ? Lu2 C4 H4 82(4) . . ? C10 C5 C6 115.1(6) . . ? C10 C5 C4 123.5(6) . . ? C6 C5 C4 121.2(6) . . ? C10 C5 Lu2 126.9(5) . . ? C6 C5 Lu2 75.0(4) . . ? C4 C5 Lu2 67.6(4) . . ? C7 C6 C5 123.7(7) . . ? C7 C6 Lu2 127.7(5) . . ? C5 C6 Lu2 75.8(4) . . ? C7 C6 H6 111(4) . . ? C5 C6 H6 122(4) . . ? Lu2 C6 H6 86(4) . . ? C8 C7 C6 119.8(7) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 118.9(7) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C10 C9 C8 120.7(8) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C5 121.7(7) . . ? C9 C10 H10 119.1 . . ? C5 C10 H10 119.1 . . ? C16 C11 C12 115.6(7) . . ? C16 C11 C3 124.4(7) . . ? C12 C11 C3 120.0(7) . . ? C13 C12 C11 120.7(8) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 C12 122.9(9) . . ? C14 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? C13 C14 C15 117.5(9) . . ? C13 C14 H14 121.3 . . ? C15 C14 H14 121.3 . . ? C14 C15 C16 120.6(9) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C11 C16 C15 122.6(9) . . ? C11 C16 H16 118.7 . . ? C15 C16 H16 118.7 . . ? O1 C17 C18 107.3(7) . . ? O1 C17 H17A 110.3 . . ? C18 C17 H17A 110.3 . . ? O1 C17 H17B 110.3 . . ? C18 C17 H17B 110.3 . . ? H17A C17 H17B 108.5 . . ? C19 C18 C17 106.0(8) . . ? C19 C18 H18A 110.5 . . ? C17 C18 H18A 110.5 . . ? C19 C18 H18B 110.5 . . ? C17 C18 H18B 110.5 . . ? H18A C18 H18B 108.7 . . ? C18 C19 C20 105.9(7) . . ? C18 C19 H19A 110.6 . . ? C20 C19 H19A 110.6 . . ? C18 C19 H19B 110.6 . . ? C20 C19 H19B 110.6 . . ? H19A C19 H19B 108.7 . . ? O1 C20 C19 105.6(6) . . ? O1 C20 H20A 110.6 . . ? C19 C20 H20A 110.6 . . ? O1 C20 H20B 110.6 . . ? C19 C20 H20B 110.6 . . ? H20A C20 H20B 108.8 . . ? O2 C21 C22' 107.2(9) . . ? O2 C21 C22 100.0(16) . . ? C22' C21 C22 32.2(16) . . ? O2 C21 H21A 110.3 . . ? C22' C21 H21A 110.3 . . ? C22 C21 H21A 84.4 . . ? O2 C21 H21B 110.3 . . ? C22' C21 H21B 110.3 . . ? C22 C21 H21B 139.3 . . ? H21A C21 H21B 108.5 . . ? C23 C22 C21 108(3) . . ? C23 C22 H22A 110.0 . . ? C21 C22 H22A 110.0 . . ? C23 C22 H22B 110.0 . . ? C21 C22 H22B 110.0 . . ? H22A C22 H22B 108.4 . . ? C21 C22' C23 105.4(13) . . ? C21 C22' H22C 110.7 . . ? C23 C22' H22C 110.7 . . ? C21 C22' H22D 110.7 . . ? C23 C22' H22D 110.7 . . ? H22C C22' H22D 108.8 . . ? C22 C23 C22' 33.8(19) . . ? C22 C23 C24 102.0(18) . . ? C22' C23 C24 108.4(9) . . ? C22 C23 H23A 82.1 . . ? C22' C23 H23A 110.0 . . ? C24 C23 H23A 110.0 . . ? C22 C23 H23B 139.5 . . ? C22' C23 H23B 110.0 . . ? C24 C23 H23B 110.0 . . ? H23A C23 H23B 108.4 . . ? O2 C24 C23 106.1(6) . . ? O2 C24 H24A 110.5 . . ? C23 C24 H24A 110.5 . . ? O2 C24 H24B 110.5 . . ? C23 C24 H24B 110.5 . . ? H24A C24 H24B 108.7 . . ? N1 C25 N2 114.0(6) . . ? N1 C25 C26 121.9(6) . . ? N2 C25 C26 124.1(6) . . ? N1 C25 Lu1 58.3(3) . . ? N2 C25 Lu1 56.0(3) . . ? C26 C25 Lu1 175.6(4) . . ? C31 C26 C27 118.3(6) . . ? C31 C26 C25 122.2(6) . . ? C27 C26 C25 119.5(6) . . ? C26 C27 C28 120.2(7) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 120.3(7) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 119.7(7) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C29 C30 C31 120.2(7) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C26 C31 C30 121.3(7) . . ? C26 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? C33 C32 C40 120.0(6) . . ? C33 C32 N1 119.5(6) . . ? C40 C32 N1 120.5(6) . . ? C37 C33 C32 119.1(7) . . ? C37 C33 C34 118.0(7) . . ? C32 C33 C34 122.8(6) . . ? C36 C34 C33 113.3(7) . . ? C36 C34 C35 110.6(7) . . ? C33 C34 C35 111.2(6) . . ? C36 C34 H34 107.1 . . ? C33 C34 H34 107.1 . . ? C35 C34 H34 107.1 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C33 C37 C38 121.9(8) . . ? C33 C37 H37 119.1 . . ? C38 C37 H37 119.1 . . ? C39 C38 C37 118.8(7) . . ? C39 C38 H38 120.6 . . ? C37 C38 H38 120.6 . . ? C38 C39 C40 122.8(7) . . ? C38 C39 H39 118.6 . . ? C40 C39 H39 118.6 . . ? C39 C40 C32 117.3(6) . . ? C39 C40 C41 118.9(6) . . ? C32 C40 C41 123.8(6) . . ? C40 C41 C42 115.4(7) . . ? C40 C41 C43 110.7(6) . . ? C42 C41 C43 110.4(6) . . ? C40 C41 H41 106.6 . . ? C42 C41 H41 106.6 . . ? C43 C41 H41 106.6 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C52 C44 C45 120.3(6) . . ? C52 C44 N2 117.2(6) . . ? C45 C44 N2 122.3(6) . . ? C49 C45 C44 118.0(6) . . ? C49 C45 C46 117.4(6) . . ? C44 C45 C46 124.6(6) . . ? C45 C46 C48 110.7(6) . . ? C45 C46 C47 111.5(6) . . ? C48 C46 C47 108.2(6) . . ? C45 C46 H46 108.8 . . ? C48 C46 H46 108.8 . . ? C47 C46 H46 108.8 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 C45 122.7(7) . . ? C50 C49 H49 118.7 . . ? C45 C49 H49 118.7 . . ? C49 C50 C51 119.1(7) . . ? C49 C50 H50 120.4 . . ? C51 C50 H50 120.4 . . ? C52 C51 C50 120.6(7) . . ? C52 C51 H51 119.7 . . ? C50 C51 H51 119.7 . . ? C51 C52 C44 119.3(6) . . ? C51 C52 C53 117.3(6) . . ? C44 C52 C53 123.4(5) . . ? C55 C53 C54 110.1(6) . . ? C55 C53 C52 114.8(6) . . ? C54 C53 C52 111.3(6) . . ? C55 C53 H53 106.7 . . ? C54 C53 H53 106.7 . . ? C52 C53 H53 106.7 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N3 C56 N4 113.8(5) . . ? N3 C56 C57 121.9(6) . . ? N4 C56 C57 124.2(6) . . ? N3 C56 Lu2 57.2(3) . . ? N4 C56 Lu2 56.6(3) . . ? C57 C56 Lu2 174.7(5) . . ? C58 C57 C62 118.2(7) . . ? C58 C57 C56 120.0(7) . . ? C62 C57 C56 121.8(7) . . ? C59 C58 C57 122.4(8) . . ? C59 C58 H58 118.8 . . ? C57 C58 H58 118.8 . . ? C58 C59 C60 118.5(9) . . ? C58 C59 H59 120.8 . . ? C60 C59 H59 120.8 . . ? C61 C60 C59 120.8(9) . . ? C61 C60 H60 119.6 . . ? C59 C60 H60 119.6 . . ? C60 C61 C62 121.6(9) . . ? C60 C61 H61 119.2 . . ? C62 C61 H61 119.2 . . ? C57 C62 C61 118.7(8) . . ? C57 C62 H62 120.7 . . ? C61 C62 H62 120.7 . . ? C64 C63 N3 120.8(6) . . ? C64 C63 C71 119.1(6) . . ? N3 C63 C71 120.0(6) . . ? C63 C64 C68 119.3(6) . . ? C63 C64 C65 122.1(6) . . ? C68 C64 C65 118.6(7) . . ? C66 C65 C67 110.4(7) . . ? C66 C65 C64 109.0(6) . . ? C67 C65 C64 114.2(6) . . ? C66 C65 H65 107.7 . . ? C67 C65 H65 107.7 . . ? C64 C65 H65 107.7 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C69 C68 C64 120.9(7) . . ? C69 C68 H68 119.6 . . ? C64 C68 H68 119.6 . . ? C68 C69 C70 119.8(7) . . ? C68 C69 H69 120.1 . . ? C70 C69 H69 120.1 . . ? C71 C70 C69 121.5(7) . . ? C71 C70 H70 119.3 . . ? C69 C70 H70 119.3 . . ? C70 C71 C63 119.2(7) . . ? C70 C71 C72 118.8(6) . . ? C63 C71 C72 122.0(6) . . ? C71 C72 C74 113.1(6) . . ? C71 C72 C73 109.2(6) . . ? C74 C72 C73 111.0(6) . . ? C71 C72 H72 107.8 . . ? C74 C72 H72 107.8 . . ? C73 C72 H72 107.8 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C74 H74A 109.5 . . ? C72 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C72 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C76 C75 C83 119.9(6) . . ? C76 C75 N4 117.8(6) . . ? C83 C75 N4 122.0(6) . . ? C80 C76 C75 119.3(7) . . ? C80 C76 C77 118.3(7) . . ? C75 C76 C77 122.3(6) . . ? C78 C77 C79 108.5(7) . . ? C78 C77 C76 114.7(7) . . ? C79 C77 C76 111.7(7) . . ? C78 C77 H77 107.2 . . ? C79 C77 H77 107.2 . . ? C76 C77 H77 107.2 . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C77 C79 H79A 109.5 . . ? C77 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C77 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C76 C80 C81 121.7(8) . . ? C76 C80 H80 119.1 . . ? C81 C80 H80 119.1 . . ? C82 C81 C80 118.9(7) . . ? C82 C81 H81 120.6 . . ? C80 C81 H81 120.6 . . ? C81 C82 C83 121.7(8) . . ? C81 C82 H82 119.2 . . ? C83 C82 H82 119.2 . . ? C82 C83 C75 118.5(8) . . ? C82 C83 C84 117.8(7) . . ? C75 C83 C84 123.7(6) . . ? C86 C84 C83 112.9(6) . . ? C86 C84 C85 107.9(6) . . ? C83 C84 C85 111.9(6) . . ? C86 C84 H84 108.0 . . ? C83 C84 H84 108.0 . . ? C85 C84 H84 108.0 . . ? C84 C85 H85A 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C84 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C84 C86 H86A 109.5 . . ? C84 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C84 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C25 N1 C32 122.9(5) . . ? C25 N1 Lu1 93.4(4) . . ? C32 N1 Lu1 142.2(4) . . ? C25 N2 C44 127.0(5) . . ? C25 N2 Lu1 95.6(4) . . ? C44 N2 Lu1 136.7(4) . . ? C56 N3 C63 119.6(5) . . ? C56 N3 Lu2 94.0(4) . . ? C63 N3 Lu2 144.6(4) . . ? C56 N4 C75 124.4(5) . . ? C56 N4 Lu2 94.5(4) . . ? C75 N4 Lu2 140.8(4) . . ? C17 O1 C20 108.9(5) . . ? C17 O1 Lu1 133.2(4) . . ? C20 O1 Lu1 117.0(4) . . ? C21 O2 C24 108.4(5) . . ? C21 O2 Lu2 125.4(4) . . ? C24 O2 Lu2 126.1(4) . . ? N2 Lu1 O1 105.52(17) . . ? N2 Lu1 N1 56.66(18) . . ? O1 Lu1 N1 91.73(17) . . ? N2 Lu1 C3 92.9(2) . . ? O1 Lu1 C3 90.8(2) . . ? N1 Lu1 C3 148.9(2) . . ? N2 Lu1 C4 128.5(2) . . ? O1 Lu1 C4 84.8(2) . . ? N1 Lu1 C4 174.5(2) . . ? C3 Lu1 C4 35.8(2) . . ? N2 Lu1 C25 28.42(18) . . ? O1 Lu1 C25 98.21(17) . . ? N1 Lu1 C25 28.32(17) . . ? C3 Lu1 C25 120.8(2) . . ? C4 Lu1 C25 156.6(2) . . ? N2 Lu1 Lu2 140.63(13) . . ? O1 Lu1 Lu2 113.40(11) . . ? N1 Lu1 Lu2 125.58(12) . . ? C3 Lu1 Lu2 81.12(16) . . ? C4 Lu1 Lu2 52.65(16) . . ? C25 Lu1 Lu2 141.79(12) . . ? N2 Lu1 H2 152.3(15) . . ? O1 Lu1 H2 87.0(16) . . ? N1 Lu1 H2 99.2(16) . . ? C3 Lu1 H2 111.9(16) . . ? C4 Lu1 H2 76.4(16) . . ? C25 Lu1 H2 126.8(16) . . ? Lu2 Lu1 H2 40.2(16) . . ? N2 Lu1 H1 97(2) . . ? O1 Lu1 H1 157(2) . . ? N1 Lu1 H1 97(2) . . ? C3 Lu1 H1 93(2) . . ? C4 Lu1 H1 85(2) . . ? C25 Lu1 H1 100(2) . . ? Lu2 Lu1 H1 45(2) . . ? H2 Lu1 H1 70(3) . . ? N2 Lu1 H4 144.4(16) . . ? O1 Lu1 H4 66.5(12) . . ? N1 Lu1 H4 151.6(5) . . ? C3 Lu1 H4 54.2(11) . . ? C4 Lu1 H4 23.1(5) . . ? C25 Lu1 H4 162.6(17) . . ? Lu2 Lu1 H4 55.6(18) . . ? H2 Lu1 H4 63(2) . . ? H1 Lu1 H4 97(3) . . ? O2 Lu2 N4 102.28(18) . . ? O2 Lu2 N3 91.02(17) . . ? N4 Lu2 N3 57.64(17) . . ? O2 Lu2 C4 90.9(2) . . ? N4 Lu2 C4 134.9(2) . . ? N3 Lu2 C4 166.22(19) . . ? O2 Lu2 C56 96.88(17) . . ? N4 Lu2 C56 28.88(18) . . ? N3 Lu2 C56 28.77(17) . . ? C4 Lu2 C56 163.5(2) . . ? O2 Lu2 C6 88.2(2) . . ? N4 Lu2 C6 82.41(19) . . ? N3 Lu2 C6 138.88(19) . . ? C4 Lu2 C6 54.8(2) . . ? C56 Lu2 C6 110.7(2) . . ? O2 Lu2 C5 76.64(18) . . ? N4 Lu2 C5 110.99(18) . . ? N3 Lu2 C5 161.46(19) . . ? C4 Lu2 C5 30.9(2) . . ? C56 Lu2 C5 137.98(19) . . ? C6 Lu2 C5 29.22(18) . . ? O2 Lu2 Lu1 112.80(11) . . ? N4 Lu2 Lu1 144.86(14) . . ? N3 Lu2 Lu1 117.76(12) . . ? C4 Lu2 Lu1 49.29(16) . . ? C56 Lu2 Lu1 137.64(13) . . ? C6 Lu2 Lu1 100.18(16) . . ? C5 Lu2 Lu1 80.17(13) . . ? O2 Lu2 H2 153.5(16) . . ? N4 Lu2 H2 103.7(16) . . ? N3 Lu2 H2 98.4(16) . . ? C4 Lu2 H2 74.4(16) . . ? C56 Lu2 H2 103.3(16) . . ? C6 Lu2 H2 100.4(16) . . ? C5 Lu2 H2 98.7(16) . . ? Lu1 Lu2 H2 41.2(16) . . ? O2 Lu2 H1 91(2) . . ? N4 Lu2 H1 145.6(19) . . ? N3 Lu2 H1 90.9(18) . . ? C4 Lu2 H1 75.5(18) . . ? C56 Lu2 H1 118.8(18) . . ? C6 Lu2 H1 130.2(18) . . ? C5 Lu2 H1 102.9(18) . . ? Lu1 Lu2 H1 36.6(18) . . ? H2 Lu2 H1 65(2) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.642 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.128 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.000 -0.001 0.000 978 229 ' ' 2 0.500 1.000 0.500 37 5 ' ' _platon_squeeze_details ; 1.5 disorder hexane molecules per formual unit of [(Ph-NCN)LuH(THF)]2(PhCHCHPh) were not modelled and the disordered density was taken into account using the SQUEEZE/PLATON procedure. (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194?01) as implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst. 2003, 36, 7?3. PLATON - a multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands). ; data_4-Lu-c _database_code_depnum_ccdc_archive 'CCDC 859489' #TrackingRef '- Ln2H4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((Ph-NCN)LuH)2(THF)(PhCHCHPh) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H100 Lu2 N4 O' _chemical_formula_weight 1483.58 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' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.161(2) _cell_length_b 17.449(3) _cell_length_c 18.270(3) _cell_angle_alpha 76.958(3) _cell_angle_beta 76.864(3) _cell_angle_gamma 70.969(3) _cell_volume 4388.8(12) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Fragment _exptl_crystal_colour Purple _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1516 _exptl_absorpt_coefficient_mu 2.274 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.4949 _exptl_absorpt_correction_T_max 0.7267 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 23847 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0932 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15180 _reflns_number_gt 10371 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0225P)^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 15180 _refine_ls_number_parameters 811 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.939 _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 C3 C 0.6606(5) 0.9387(4) 0.8619(4) 0.0371(16) Uani 1 1 d . . . C4 C 0.5736(4) 0.9764(4) 0.8325(3) 0.0338(15) Uani 1 1 d . . . C5 C 0.4968(4) 1.0407(3) 0.8548(3) 0.0324(14) Uani 1 1 d . . . C6 C 0.4879(5) 1.0803(4) 0.9206(3) 0.0383(16) Uani 1 1 d . . . C7 C 0.4121(5) 1.1447(4) 0.9380(3) 0.0355(16) Uani 1 1 d . . . C8 C 0.3396(4) 1.1795(4) 0.8936(4) 0.0361(16) Uani 1 1 d . . . C9 C 0.3412(5) 1.1387(4) 0.8361(4) 0.0364(17) Uani 1 1 d . . . C10 C 0.4160(5) 1.0739(4) 0.8144(4) 0.0396(16) Uani 1 1 d . . . C11 C 0.7097(4) 0.8511(4) 0.8616(3) 0.0333(14) Uani 1 1 d . . . C12 C 0.7766(4) 0.8085(4) 0.9087(3) 0.0389(16) Uani 1 1 d . . . H12 H 0.7911 0.8377 0.9402 0.047 Uiso 1 1 calc R . . C13 C 0.8226(5) 0.7256(4) 0.9116(4) 0.055(2) Uani 1 1 d . . . H13 H 0.8678 0.6993 0.9446 0.066 Uiso 1 1 calc R . . C14 C 0.8040(6) 0.6816(4) 0.8681(4) 0.069(3) Uani 1 1 d . . . H14 H 0.8355 0.6245 0.8703 0.083 Uiso 1 1 calc R . . C15 C 0.7386(6) 0.7210(5) 0.8207(4) 0.073(3) Uani 1 1 d . . . H15 H 0.7259 0.6911 0.7889 0.088 Uiso 1 1 calc R . . C16 C 0.6911(5) 0.8037(4) 0.8185(4) 0.055(2) Uani 1 1 d . . . H16 H 0.6444 0.8288 0.7866 0.066 Uiso 1 1 calc R . . C17 C 0.8061(5) 0.9191(4) 0.6491(4) 0.0516(19) Uani 1 1 d . . . H17A H 0.8069 0.8674 0.6855 0.062 Uiso 1 1 calc R . . H17B H 0.8632 0.9348 0.6491 0.062 Uiso 1 1 calc R . . C18 C 0.8022(6) 0.9091(5) 0.5720(4) 0.080(3) Uani 1 1 d . . . H18A H 0.8319 0.9466 0.5328 0.096 Uiso 1 1 calc R . . H18B H 0.8353 0.8518 0.5636 0.096 Uiso 1 1 calc R . . C19 C 0.7013(6) 0.9296(6) 0.5692(5) 0.085(3) Uani 1 1 d . . . H19A H 0.6791 0.8800 0.5864 0.102 Uiso 1 1 calc R . . H19B H 0.6888 0.9537 0.5167 0.102 Uiso 1 1 calc R . . C20 C 0.6529(5) 0.9908(5) 0.6218(4) 0.059(2) Uani 1 1 d . . . H20A H 0.6344 1.0471 0.5927 0.071 Uiso 1 1 calc R . . H20B H 0.5955 0.9783 0.6537 0.071 Uiso 1 1 calc R . . C21 C 0.8873(4) 1.0604(3) 0.7486(3) 0.0270(13) Uani 1 1 d . . . C22 C 0.9885(4) 1.0613(3) 0.7375(3) 0.0262(13) Uani 1 1 d . . . C23 C 1.0411(4) 1.0639(3) 0.6646(3) 0.0321(14) Uani 1 1 d . . . H23 H 1.0130 1.0642 0.6231 0.039 Uiso 1 1 calc R . . C24 C 1.1332(4) 1.0660(4) 0.6516(3) 0.0409(16) Uani 1 1 d . . . H24 H 1.1678 1.0680 0.6012 0.049 Uiso 1 1 calc R . . C25 C 1.1763(4) 1.0654(4) 0.7111(4) 0.0462(17) Uani 1 1 d . . . H25 H 1.2399 1.0671 0.7020 0.055 Uiso 1 1 calc R . . C26 C 1.1249(4) 1.0622(4) 0.7834(3) 0.0423(16) Uani 1 1 d . . . H26 H 1.1533 1.0621 0.8248 0.051 Uiso 1 1 calc R . . C27 C 1.0322(4) 1.0590(4) 0.7972(3) 0.0336(15) Uani 1 1 d . . . H27 H 0.9985 1.0552 0.8479 0.040 Uiso 1 1 calc R . . C28 C 0.8482(4) 1.1792(3) 0.6565(3) 0.0245(13) Uani 1 1 d . . . C29 C 0.8553(4) 1.1916(4) 0.5766(3) 0.0346(15) Uani 1 1 d . . . C30 C 0.8381(5) 1.1319(4) 0.5371(3) 0.0425(17) Uani 1 1 d . . . H30 H 0.8368 1.0814 0.5756 0.051 Uiso 1 1 calc R . . C31 C 0.9169(5) 1.1053(5) 0.4709(4) 0.064(2) Uani 1 1 d . . . H31A H 0.9020 1.0662 0.4480 0.096 Uiso 1 1 calc R . . H31B H 0.9771 1.0789 0.4898 0.096 Uiso 1 1 calc R . . H31C H 0.9221 1.1535 0.4324 0.096 Uiso 1 1 calc R . . C32 C 0.7415(5) 1.1655(5) 0.5119(4) 0.067(2) Uani 1 1 d . . . H32A H 0.7319 1.1253 0.4870 0.101 Uiso 1 1 calc R . . H32B H 0.7385 1.2170 0.4761 0.101 Uiso 1 1 calc R . . H32C H 0.6919 1.1757 0.5565 0.101 Uiso 1 1 calc R . . C33 C 0.8779(4) 1.2615(4) 0.5321(3) 0.0394(16) Uani 1 1 d . . . H33 H 0.8830 1.2697 0.4783 0.047 Uiso 1 1 calc R . . C34 C 0.8930(5) 1.3186(4) 0.5655(4) 0.0497(18) Uani 1 1 d . . . H34 H 0.9105 1.3647 0.5347 0.060 Uiso 1 1 calc R . . C35 C 0.8827(4) 1.3087(4) 0.6430(3) 0.0388(15) Uani 1 1 d . . . H35 H 0.8913 1.3492 0.6656 0.047 Uiso 1 1 calc R . . C36 C 0.8602(4) 1.2410(3) 0.6890(3) 0.0306(14) Uani 1 1 d . . . C37 C 0.8410(4) 1.2381(4) 0.7761(3) 0.0304(14) Uani 1 1 d . . . H37 H 0.8468 1.1796 0.8004 0.036 Uiso 1 1 calc R . . C38 C 0.9120(4) 1.2650(4) 0.8045(4) 0.0425(16) Uani 1 1 d . . . H38A H 0.9763 1.2315 0.7878 0.064 Uiso 1 1 calc R . . H38B H 0.8989 1.2577 0.8603 0.064 Uiso 1 1 calc R . . H38C H 0.9061 1.3230 0.7837 0.064 Uiso 1 1 calc R . . C39 C 0.7401(4) 1.2884(4) 0.8021(3) 0.0432(16) Uani 1 1 d . . . H39A H 0.7288 1.2853 0.8575 0.065 Uiso 1 1 calc R . . H39B H 0.6955 1.2663 0.7881 0.065 Uiso 1 1 calc R . . H39C H 0.7309 1.3458 0.7774 0.065 Uiso 1 1 calc R . . C40 C 0.8984(4) 0.9533(3) 0.8615(3) 0.0270(13) Uani 1 1 d . . . C41 C 0.9707(4) 0.8823(4) 0.8459(3) 0.0320(14) Uani 1 1 d . . . C42 C 1.0113(4) 0.8613(4) 0.7661(3) 0.0346(15) Uani 1 1 d . . . H42 H 0.9799 0.9082 0.7289 0.042 Uiso 1 1 calc R . . C43 C 0.9877(5) 0.7834(4) 0.7583(4) 0.0499(18) Uani 1 1 d . . . H43A H 1.0133 0.7707 0.7067 0.075 Uiso 1 1 calc R . . H43B H 0.9188 0.7936 0.7679 0.075 Uiso 1 1 calc R . . H43C H 1.0159 0.7368 0.7954 0.075 Uiso 1 1 calc R . . C44 C 1.1173(4) 0.8495(4) 0.7460(4) 0.0506(18) Uani 1 1 d . . . H44A H 1.1400 0.8371 0.6941 0.076 Uiso 1 1 calc R . . H44B H 1.1497 0.8038 0.7818 0.076 Uiso 1 1 calc R . . H44C H 1.1306 0.8999 0.7491 0.076 Uiso 1 1 calc R . . C45 C 1.0110(4) 0.8280(4) 0.9059(3) 0.0436(17) Uani 1 1 d . . . H45 H 1.0617 0.7805 0.8958 0.052 Uiso 1 1 calc R . . C46 C 0.9786(5) 0.8420(4) 0.9801(3) 0.0457(18) Uani 1 1 d . . . H46 H 1.0064 0.8042 1.0206 0.055 Uiso 1 1 calc R . . C47 C 0.9068(4) 0.9102(4) 0.9946(3) 0.0376(16) Uani 1 1 d . . . H47 H 0.8846 0.9188 1.0459 0.045 Uiso 1 1 calc R . . C48 C 0.8647(4) 0.9676(3) 0.9377(3) 0.0294(14) Uani 1 1 d . . . C49 C 0.7881(4) 1.0454(3) 0.9580(3) 0.0311(14) Uani 1 1 d . . . H49 H 0.7567 1.0730 0.9125 0.037 Uiso 1 1 calc R . . C50 C 0.8295(5) 1.1053(4) 0.9773(4) 0.0508(18) Uani 1 1 d . . . H50A H 0.7785 1.1545 0.9897 0.076 Uiso 1 1 calc R . . H50B H 0.8747 1.1210 0.9334 0.076 Uiso 1 1 calc R . . H50C H 0.8620 1.0792 1.0211 0.076 Uiso 1 1 calc R . . C51 C 0.7116(5) 1.0272(4) 1.0249(3) 0.0466(18) Uani 1 1 d . . . H51A H 0.6837 0.9890 1.0130 0.070 Uiso 1 1 calc R . . H51B H 0.6622 1.0785 1.0335 0.070 Uiso 1 1 calc R . . H51C H 0.7401 1.0024 1.0710 0.070 Uiso 1 1 calc R . . C52 C 0.3944(4) 1.3545(3) 0.7316(3) 0.0252(13) Uani 1 1 d . . . C53 C 0.3374(4) 1.4417(3) 0.7039(3) 0.0292(14) Uani 1 1 d . . . C54 C 0.3135(4) 1.5031(4) 0.7482(3) 0.0363(15) Uani 1 1 d . . . H54 H 0.3310 1.4902 0.7973 0.044 Uiso 1 1 calc R . . C55 C 0.2651(4) 1.5815(4) 0.7217(4) 0.0480(18) Uani 1 1 d . . . H55 H 0.2492 1.6229 0.7524 0.058 Uiso 1 1 calc R . . C56 C 0.2389(5) 1.6016(4) 0.6504(4) 0.053(2) Uani 1 1 d . . . H56 H 0.2053 1.6566 0.6324 0.063 Uiso 1 1 calc R . . C57 C 0.2608(4) 1.5434(4) 0.6064(4) 0.0469(18) Uani 1 1 d . . . H57 H 0.2424 1.5575 0.5575 0.056 Uiso 1 1 calc R . . C58 C 0.3096(4) 1.4634(4) 0.6318(3) 0.0378(15) Uani 1 1 d . . . H58 H 0.3246 1.4228 0.6004 0.045 Uiso 1 1 calc R . . C59 C 0.2989(4) 1.2891(3) 0.6882(3) 0.0312(14) Uani 1 1 d . . . C60 C 0.3202(4) 1.2495(4) 0.6239(3) 0.0348(15) Uani 1 1 d . . . C61 C 0.4228(4) 1.2118(4) 0.5884(3) 0.0376(16) Uani 1 1 d . . . H61 H 0.4610 1.1918 0.6306 0.045 Uiso 1 1 calc R . . C62 C 0.4605(5) 1.2761(5) 0.5336(4) 0.068(2) Uani 1 1 d . . . H62A H 0.4526 1.3219 0.5594 0.102 Uiso 1 1 calc R . . H62B H 0.4258 1.2960 0.4906 0.102 Uiso 1 1 calc R . . H62C H 0.5279 1.2523 0.5148 0.102 Uiso 1 1 calc R . . C63 C 0.4347(5) 1.1385(4) 0.5521(4) 0.060(2) Uani 1 1 d . . . H63A H 0.4113 1.0971 0.5902 0.090 Uiso 1 1 calc R . . H63B H 0.5019 1.1148 0.5327 0.090 Uiso 1 1 calc R . . H63C H 0.3987 1.1560 0.5099 0.090 Uiso 1 1 calc R . . C64 C 0.2461(5) 1.2482(4) 0.5932(4) 0.0480(18) Uani 1 1 d . . . H64 H 0.2598 1.2224 0.5497 0.058 Uiso 1 1 calc R . . C65 C 0.1526(5) 1.2826(4) 0.6226(4) 0.055(2) Uani 1 1 d . . . H65 H 0.1032 1.2822 0.5988 0.066 Uiso 1 1 calc R . . C66 C 0.1326(5) 1.3172(4) 0.6869(4) 0.0500(18) Uani 1 1 d . . . H66 H 0.0684 1.3393 0.7086 0.060 Uiso 1 1 calc R . . C67 C 0.2040(4) 1.3211(4) 0.7215(3) 0.0328(14) Uani 1 1 d . . . C68 C 0.1720(4) 1.3563(4) 0.7954(3) 0.0401(16) Uani 1 1 d . . . H68 H 0.2303 1.3540 0.8138 0.048 Uiso 1 1 calc R . . C69 C 0.1181(4) 1.3066(4) 0.8576(4) 0.0514(19) Uani 1 1 d . . . H69A H 0.1000 1.3312 0.9040 0.077 Uiso 1 1 calc R . . H69B H 0.1585 1.2500 0.8680 0.077 Uiso 1 1 calc R . . H69C H 0.0611 1.3066 0.8408 0.077 Uiso 1 1 calc R . . C70 C 0.1110(4) 1.4470(4) 0.7854(4) 0.055(2) Uani 1 1 d . . . H70A H 0.0937 1.4663 0.8346 0.083 Uiso 1 1 calc R . . H70B H 0.0535 1.4516 0.7668 0.083 Uiso 1 1 calc R . . H70C H 0.1471 1.4806 0.7486 0.083 Uiso 1 1 calc R . . C71 C 0.5031(4) 1.3954(3) 0.7834(3) 0.0287(14) Uani 1 1 d . . . C72 C 0.5436(4) 1.4469(4) 0.7238(3) 0.0341(15) Uani 1 1 d . . . C73 C 0.5533(4) 1.4392(4) 0.6393(3) 0.0354(15) Uani 1 1 d . . . H73 H 0.4981 1.4218 0.6353 0.043 Uiso 1 1 calc R . . C74 C 0.6418(6) 1.3715(6) 0.6169(4) 0.096(4) Uani 1 1 d . . . H74A H 0.6412 1.3205 0.6527 0.144 Uiso 1 1 calc R . . H74B H 0.6978 1.3872 0.6184 0.144 Uiso 1 1 calc R . . H74C H 0.6436 1.3632 0.5653 0.144 Uiso 1 1 calc R . . C75 C 0.5484(7) 1.5207(5) 0.5856(4) 0.094(3) Uani 1 1 d . . . H75A H 0.5537 1.5127 0.5332 0.141 Uiso 1 1 calc R . . H75B H 0.6005 1.5406 0.5891 0.141 Uiso 1 1 calc R . . H75C H 0.4879 1.5611 0.6000 0.141 Uiso 1 1 calc R . . C76 C 0.5795(5) 1.5023(4) 0.7427(4) 0.0483(18) Uani 1 1 d . . . H76 H 0.6049 1.5388 0.7031 0.058 Uiso 1 1 calc R . . C77 C 0.5792(5) 1.5058(4) 0.8165(4) 0.0505(18) Uani 1 1 d . . . H77 H 0.6041 1.5444 0.8279 0.061 Uiso 1 1 calc R . . C78 C 0.5427(4) 1.4532(4) 0.8746(4) 0.0429(16) Uani 1 1 d . . . H78 H 0.5427 1.4561 0.9259 0.051 Uiso 1 1 calc R . . C79 C 0.5063(4) 1.3965(3) 0.8602(3) 0.0340(15) Uani 1 1 d . . . C80 C 0.4689(5) 1.3388(4) 0.9244(3) 0.0422(17) Uani 1 1 d . . . H80 H 0.4797 1.2884 0.9022 0.051 Uiso 1 1 calc R . . C81 C 0.3622(6) 1.3689(6) 0.9487(5) 0.098(3) Uani 1 1 d . . . H81A H 0.3417 1.3286 0.9901 0.147 Uiso 1 1 calc R . . H81B H 0.3309 1.3758 0.9052 0.147 Uiso 1 1 calc R . . H81C H 0.3453 1.4217 0.9663 0.147 Uiso 1 1 calc R . . C82 C 0.5187(6) 1.3086(6) 0.9918(4) 0.098(3) Uani 1 1 d . . . H82A H 0.4889 1.2707 1.0292 0.146 Uiso 1 1 calc R . . H82B H 0.5147 1.3553 1.0149 0.146 Uiso 1 1 calc R . . H82C H 0.5853 1.2799 0.9753 0.146 Uiso 1 1 calc R . . N1 N 0.8284(3) 1.1085(3) 0.7013(2) 0.0243(11) Uani 1 1 d . . . N2 N 0.8491(3) 1.0106(3) 0.8041(2) 0.0254(11) Uani 1 1 d . . . N3 N 0.3765(3) 1.2889(3) 0.7195(2) 0.0248(11) Uani 1 1 d . . . N4 N 0.4650(3) 1.3355(3) 0.7708(2) 0.0254(11) Uani 1 1 d . . . O1 O 0.7219(3) 0.9832(2) 0.6687(2) 0.0388(10) Uani 1 1 d . . . Lu1 Lu 0.701434(17) 1.052915(15) 0.767037(13) 0.02790(8) Uani 1 1 d . . . Lu2 Lu 0.486305(18) 1.197066(15) 0.796168(13) 0.02866(8) Uani 1 1 d . . . H1 H 0.627(4) 1.149(3) 0.820(3) 0.050 Uiso 1 1 d . . . H2 H 0.584(4) 1.144(3) 0.697(3) 0.050 Uiso 1 1 d . . . H3 H 0.654(4) 0.960(4) 0.907(3) 0.050 Uiso 1 1 d . . . H4 H 0.558(4) 0.955(4) 0.799(3) 0.050 Uiso 1 1 d . . . H6 H 0.535(4) 1.055(4) 0.955(3) 0.050 Uiso 1 1 d . . . H7 H 0.406(4) 1.165(4) 0.977(3) 0.050 Uiso 1 1 d . . . H8 H 0.293(4) 1.223(4) 0.901(3) 0.050 Uiso 1 1 d . . . H9 H 0.304(4) 1.158(4) 0.806(3) 0.050 Uiso 1 1 d . . . H10 H 0.415(4) 1.045(4) 0.777(3) 0.050 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 C3 0.047(4) 0.028(3) 0.035(4) 0.001(3) -0.005(3) -0.014(3) C4 0.042(4) 0.038(4) 0.026(3) 0.003(3) -0.008(3) -0.022(3) C5 0.036(4) 0.025(3) 0.029(3) 0.002(3) 0.001(3) -0.009(3) C6 0.038(4) 0.039(4) 0.030(4) 0.014(3) 0.000(3) -0.016(3) C7 0.039(4) 0.040(4) 0.024(3) -0.001(3) 0.001(3) -0.014(3) C8 0.022(4) 0.036(4) 0.040(4) 0.005(3) 0.003(3) -0.007(3) C9 0.034(4) 0.040(4) 0.036(4) 0.015(3) -0.009(3) -0.023(3) C10 0.047(5) 0.038(4) 0.038(4) 0.006(3) -0.006(3) -0.026(4) C11 0.037(4) 0.034(3) 0.027(3) 0.002(3) 0.005(3) -0.020(3) C12 0.042(4) 0.033(4) 0.038(4) -0.004(3) 0.002(3) -0.013(3) C13 0.057(5) 0.047(5) 0.036(4) 0.015(4) 0.008(4) -0.008(4) C14 0.086(7) 0.030(4) 0.062(5) 0.000(4) 0.007(5) 0.005(4) C15 0.108(8) 0.051(5) 0.059(5) -0.018(4) 0.001(5) -0.023(5) C16 0.077(6) 0.042(4) 0.043(4) 0.002(3) -0.012(4) -0.017(4) C17 0.051(5) 0.048(4) 0.050(4) -0.015(4) -0.009(4) -0.001(4) C18 0.093(8) 0.086(7) 0.065(6) -0.044(5) -0.012(5) -0.014(5) C19 0.067(6) 0.130(8) 0.086(6) -0.072(6) -0.003(5) -0.034(6) C20 0.056(5) 0.092(6) 0.048(4) -0.021(4) -0.021(4) -0.031(4) C21 0.033(4) 0.032(3) 0.017(3) -0.003(3) 0.000(3) -0.016(3) C22 0.030(4) 0.026(3) 0.023(3) -0.002(2) -0.007(3) -0.008(3) C23 0.031(4) 0.040(4) 0.023(3) 0.000(3) -0.006(3) -0.009(3) C24 0.027(4) 0.063(5) 0.028(3) 0.001(3) 0.006(3) -0.020(3) C25 0.022(4) 0.070(5) 0.048(4) -0.005(4) 0.003(3) -0.024(3) C26 0.031(4) 0.066(5) 0.035(4) -0.009(3) -0.009(3) -0.018(3) C27 0.026(4) 0.044(4) 0.027(3) -0.004(3) 0.005(3) -0.013(3) C28 0.020(3) 0.025(3) 0.025(3) -0.003(2) 0.000(2) -0.004(2) C29 0.027(4) 0.037(4) 0.034(4) -0.001(3) 0.000(3) -0.009(3) C30 0.054(5) 0.054(4) 0.017(3) -0.003(3) -0.003(3) -0.018(4) C31 0.070(6) 0.084(6) 0.037(4) -0.018(4) -0.005(4) -0.018(4) C32 0.076(6) 0.074(6) 0.059(5) -0.010(4) -0.027(4) -0.024(5) C33 0.036(4) 0.043(4) 0.028(3) 0.006(3) -0.006(3) -0.004(3) C34 0.047(5) 0.049(4) 0.042(4) 0.022(3) -0.003(3) -0.023(4) C35 0.031(4) 0.039(4) 0.048(4) 0.001(3) -0.010(3) -0.014(3) C36 0.027(4) 0.034(3) 0.030(3) 0.003(3) -0.008(3) -0.012(3) C37 0.026(4) 0.039(3) 0.025(3) -0.001(3) 0.001(3) -0.015(3) C38 0.037(4) 0.044(4) 0.053(4) -0.013(3) -0.010(3) -0.015(3) C39 0.043(4) 0.044(4) 0.041(4) -0.008(3) -0.001(3) -0.014(3) C40 0.026(4) 0.028(3) 0.024(3) -0.001(3) -0.004(3) -0.007(3) C41 0.031(4) 0.036(4) 0.028(3) 0.000(3) -0.004(3) -0.012(3) C42 0.037(4) 0.031(3) 0.033(3) -0.001(3) -0.010(3) -0.006(3) C43 0.051(5) 0.053(4) 0.041(4) -0.008(3) -0.010(3) -0.007(4) C44 0.037(4) 0.054(4) 0.053(4) -0.006(4) -0.002(3) -0.009(3) C45 0.040(4) 0.039(4) 0.038(4) 0.005(3) -0.008(3) 0.000(3) C46 0.051(5) 0.044(4) 0.033(4) 0.014(3) -0.023(3) -0.005(3) C47 0.040(4) 0.046(4) 0.023(3) 0.004(3) -0.008(3) -0.013(3) C48 0.034(4) 0.035(3) 0.022(3) 0.003(3) -0.009(3) -0.017(3) C49 0.039(4) 0.036(3) 0.018(3) 0.003(3) -0.012(3) -0.009(3) C50 0.059(5) 0.055(4) 0.043(4) -0.016(3) 0.011(4) -0.032(4) C51 0.052(5) 0.054(4) 0.036(4) -0.006(3) 0.005(3) -0.027(4) C52 0.031(4) 0.029(3) 0.010(3) 0.004(2) 0.005(2) -0.012(3) C53 0.017(3) 0.038(4) 0.032(3) 0.003(3) -0.006(3) -0.013(3) C54 0.033(4) 0.033(3) 0.041(4) -0.005(3) -0.011(3) -0.005(3) C55 0.037(4) 0.037(4) 0.062(5) -0.006(3) -0.003(4) -0.005(3) C56 0.040(4) 0.038(4) 0.059(5) 0.022(4) -0.011(4) -0.003(3) C57 0.038(4) 0.051(4) 0.037(4) 0.012(3) -0.010(3) -0.003(3) C58 0.028(4) 0.051(4) 0.030(3) 0.005(3) -0.003(3) -0.016(3) C59 0.030(4) 0.035(3) 0.030(3) 0.008(3) -0.010(3) -0.016(3) C60 0.040(4) 0.043(4) 0.026(3) 0.004(3) -0.013(3) -0.020(3) C61 0.037(4) 0.046(4) 0.036(4) -0.011(3) -0.016(3) -0.011(3) C62 0.047(5) 0.074(6) 0.074(5) -0.019(5) 0.015(4) -0.019(4) C63 0.056(5) 0.069(5) 0.057(5) -0.018(4) -0.016(4) -0.011(4) C64 0.045(5) 0.065(5) 0.042(4) -0.011(4) -0.014(4) -0.019(4) C65 0.051(5) 0.075(5) 0.053(5) -0.006(4) -0.026(4) -0.027(4) C66 0.032(4) 0.070(5) 0.051(4) 0.004(4) -0.008(3) -0.026(4) C67 0.032(4) 0.048(4) 0.025(3) 0.001(3) -0.008(3) -0.023(3) C68 0.021(4) 0.057(4) 0.044(4) -0.010(3) -0.001(3) -0.016(3) C69 0.028(4) 0.077(5) 0.047(4) -0.002(4) -0.005(3) -0.018(4) C70 0.029(4) 0.065(5) 0.068(5) -0.016(4) -0.008(4) -0.005(4) C71 0.023(3) 0.024(3) 0.038(3) -0.005(3) -0.013(3) 0.001(3) C72 0.028(4) 0.035(4) 0.039(4) -0.001(3) -0.005(3) -0.012(3) C73 0.033(4) 0.045(4) 0.030(3) 0.006(3) -0.007(3) -0.020(3) C74 0.060(6) 0.155(9) 0.048(5) -0.041(6) -0.010(4) 0.020(6) C75 0.167(10) 0.078(6) 0.059(5) 0.031(4) -0.048(6) -0.074(6) C76 0.051(5) 0.047(4) 0.050(4) 0.000(3) -0.005(4) -0.027(4) C77 0.064(5) 0.038(4) 0.061(5) -0.009(4) -0.019(4) -0.023(4) C78 0.046(4) 0.047(4) 0.039(4) -0.014(3) -0.009(3) -0.012(3) C79 0.030(4) 0.028(3) 0.039(4) -0.009(3) -0.008(3) 0.002(3) C80 0.047(4) 0.057(4) 0.026(3) -0.013(3) -0.003(3) -0.018(3) C81 0.071(7) 0.106(8) 0.084(7) 0.006(6) 0.021(5) -0.018(6) C82 0.113(8) 0.137(9) 0.062(5) 0.045(5) -0.054(5) -0.077(7) N1 0.030(3) 0.032(3) 0.015(2) -0.001(2) -0.008(2) -0.012(2) N2 0.027(3) 0.023(2) 0.024(3) -0.003(2) -0.005(2) -0.004(2) N3 0.018(3) 0.029(3) 0.030(3) 0.000(2) -0.007(2) -0.011(2) N4 0.033(3) 0.022(2) 0.022(2) 0.001(2) -0.007(2) -0.009(2) O1 0.040(3) 0.050(3) 0.031(2) -0.016(2) -0.009(2) -0.011(2) Lu1 0.02924(17) 0.02987(15) 0.02505(15) -0.00232(11) -0.00537(12) -0.01009(12) Lu2 0.02820(17) 0.03063(15) 0.02550(15) 0.00087(11) -0.00326(12) -0.01084(12) _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 C3 C4 1.435(8) . ? C3 C11 1.467(8) . ? C3 Lu1 2.474(6) . ? C3 H3 0.94(5) . ? C4 C5 1.385(8) . ? C4 Lu1 2.624(6) . ? C4 H4 0.89(6) . ? C5 C10 1.461(8) . ? C5 C6 1.476(8) . ? C5 Lu2 2.662(5) . ? C6 C7 1.355(8) . ? C6 Lu2 2.687(6) . ? C6 H6 0.98(6) . ? C7 C8 1.409(8) . ? C7 Lu2 2.664(6) . ? C7 H7 0.84(5) . ? C8 C9 1.388(9) . ? C8 Lu2 2.571(6) . ? C8 H8 0.86(6) . ? C9 C10 1.372(9) . ? C9 Lu2 2.609(6) . ? C9 H9 0.82(6) . ? C10 Lu2 2.622(6) . ? C10 H10 0.95(6) . ? C11 C16 1.390(8) . ? C11 C12 1.392(8) . ? C12 C13 1.381(8) . ? C12 H12 0.9500 . ? C13 C14 1.348(10) . ? C13 H13 0.9500 . ? C14 C15 1.372(10) . ? C14 H14 0.9500 . ? C15 C16 1.382(9) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 O1 1.432(7) . ? C17 C18 1.473(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.463(10) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.495(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O1 1.453(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 N2 1.335(6) . ? C21 N1 1.336(6) . ? C21 C22 1.505(8) . ? C21 Lu1 2.804(6) . ? C22 C27 1.387(7) . ? C22 C23 1.387(7) . ? C23 C24 1.373(8) . ? C23 H23 0.9500 . ? C24 C25 1.385(8) . ? C24 H24 0.9500 . ? C25 C26 1.373(8) . ? C25 H25 0.9500 . ? C26 C27 1.387(8) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 N1 1.398(6) . ? C28 C29 1.411(7) . ? C28 C36 1.419(7) . ? C29 C33 1.403(8) . ? C29 C30 1.508(8) . ? C30 C32 1.526(9) . ? C30 C31 1.530(8) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.379(9) . ? C33 H33 0.9500 . ? C34 C35 1.366(8) . ? C34 H34 0.9500 . ? C35 C36 1.380(8) . ? C35 H35 0.9500 . ? C36 C37 1.543(7) . ? C37 C39 1.523(8) . ? C37 C38 1.530(8) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.396(8) . ? C40 C48 1.419(7) . ? C40 N2 1.433(6) . ? C41 C45 1.389(8) . ? C41 C42 1.525(7) . ? C42 C44 1.520(8) . ? C42 C43 1.557(8) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.380(8) . ? C45 H45 0.9500 . ? C46 C47 1.355(8) . ? C46 H46 0.9500 . ? C47 C48 1.381(7) . ? C47 H47 0.9500 . ? C48 C49 1.527(8) . ? C49 C50 1.518(8) . ? C49 C51 1.536(8) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 N3 1.333(6) . ? C52 N4 1.334(7) . ? C52 C53 1.521(7) . ? C52 Lu2 2.769(5) . ? C53 C54 1.392(7) . ? C53 C58 1.408(7) . ? C54 C55 1.361(8) . ? C54 H54 0.9500 . ? C55 C56 1.385(9) . ? C55 H55 0.9500 . ? C56 C57 1.347(9) . ? C56 H56 0.9500 . ? C57 C58 1.379(8) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C67 1.409(8) . ? C59 C60 1.418(8) . ? C59 N3 1.419(7) . ? C60 C64 1.374(8) . ? C60 C61 1.529(8) . ? C61 C62 1.496(9) . ? C61 C63 1.513(8) . ? C61 H61 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.379(9) . ? C64 H64 0.9500 . ? C65 C66 1.371(9) . ? C65 H65 0.9500 . ? C66 C67 1.397(8) . ? C66 H66 0.9500 . ? C67 C68 1.524(8) . ? C68 C69 1.519(8) . ? C68 C70 1.543(8) . ? C68 H68 1.0000 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C72 1.409(8) . ? C71 C79 1.419(7) . ? C71 N4 1.429(7) . ? C72 C76 1.389(8) . ? C72 C73 1.550(8) . ? C73 C74 1.515(9) . ? C73 C75 1.526(9) . ? C73 H73 1.0000 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 C77 1.362(8) . ? C76 H76 0.9500 . ? C77 C78 1.379(9) . ? C77 H77 0.9500 . ? C78 C79 1.375(8) . ? C78 H78 0.9500 . ? C79 C80 1.500(8) . ? C80 C82 1.494(9) . ? C80 C81 1.521(10) . ? C80 H80 1.0000 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? N1 Lu1 2.394(4) . ? N2 Lu1 2.324(4) . ? N3 Lu2 2.368(4) . ? N4 Lu2 2.282(4) . ? O1 Lu1 2.300(4) . ? Lu1 Lu2 3.4224(5) . ? Lu1 H1 2.00(5) . ? Lu1 H2 2.36(5) . ? Lu2 H1 2.12(5) . ? Lu2 H2 2.22(5) . ? 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 C4 C3 C11 120.6(6) . . ? C4 C3 Lu1 79.5(3) . . ? C11 C3 Lu1 125.4(4) . . ? C4 C3 H3 107(4) . . ? C11 C3 H3 118(4) . . ? Lu1 C3 H3 99(4) . . ? C5 C4 C3 129.5(6) . . ? C5 C4 Lu1 101.5(4) . . ? C3 C4 Lu1 68.0(3) . . ? C5 C4 H4 108(4) . . ? C3 C4 H4 122(4) . . ? Lu1 C4 H4 111(4) . . ? C4 C5 C10 121.4(6) . . ? C4 C5 C6 124.2(6) . . ? C10 C5 C6 114.4(5) . . ? C4 C5 Lu2 122.3(4) . . ? C10 C5 Lu2 72.4(3) . . ? C6 C5 Lu2 74.9(3) . . ? C7 C6 C5 121.2(6) . . ? C7 C6 Lu2 74.4(4) . . ? C5 C6 Lu2 73.0(3) . . ? C7 C6 H6 120(3) . . ? C5 C6 H6 118(3) . . ? Lu2 C6 H6 130(4) . . ? C6 C7 C8 122.5(6) . . ? C6 C7 Lu2 76.3(3) . . ? C8 C7 Lu2 70.8(3) . . ? C6 C7 H7 120(4) . . ? C8 C7 H7 117(4) . . ? Lu2 C7 H7 128(4) . . ? C9 C8 C7 117.3(6) . . ? C9 C8 Lu2 76.0(4) . . ? C7 C8 Lu2 78.1(4) . . ? C9 C8 H8 118(4) . . ? C7 C8 H8 125(4) . . ? Lu2 C8 H8 118(4) . . ? C10 C9 C8 122.9(6) . . ? C10 C9 Lu2 75.3(4) . . ? C8 C9 Lu2 72.9(4) . . ? C10 C9 H9 114(4) . . ? C8 C9 H9 121(4) . . ? Lu2 C9 H9 112(5) . . ? C9 C10 C5 120.9(6) . . ? C9 C10 Lu2 74.3(4) . . ? C5 C10 Lu2 75.5(3) . . ? C9 C10 H10 122(4) . . ? C5 C10 H10 116(4) . . ? Lu2 C10 H10 128(4) . . ? C16 C11 C12 115.1(6) . . ? C16 C11 C3 123.9(6) . . ? C12 C11 C3 120.9(6) . . ? C13 C12 C11 122.7(6) . . ? C13 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C14 C13 C12 120.8(7) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 118.6(7) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C14 C15 C16 121.0(8) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C11 121.8(7) . . ? C15 C16 H16 119.1 . . ? C11 C16 H16 119.1 . . ? O1 C17 C18 104.9(5) . . ? O1 C17 H17A 110.8 . . ? C18 C17 H17A 110.8 . . ? O1 C17 H17B 110.8 . . ? C18 C17 H17B 110.8 . . ? H17A C17 H17B 108.8 . . ? C19 C18 C17 105.0(6) . . ? C19 C18 H18A 110.7 . . ? C17 C18 H18A 110.7 . . ? C19 C18 H18B 110.7 . . ? C17 C18 H18B 110.7 . . ? H18A C18 H18B 108.8 . . ? C18 C19 C20 105.2(6) . . ? C18 C19 H19A 110.7 . . ? C20 C19 H19A 110.7 . . ? C18 C19 H19B 110.7 . . ? C20 C19 H19B 110.7 . . ? H19A C19 H19B 108.8 . . ? O1 C20 C19 105.4(6) . . ? O1 C20 H20A 110.7 . . ? C19 C20 H20A 110.7 . . ? O1 C20 H20B 110.7 . . ? C19 C20 H20B 110.7 . . ? H20A C20 H20B 108.8 . . ? N2 C21 N1 113.9(5) . . ? N2 C21 C22 124.0(5) . . ? N1 C21 C22 122.1(5) . . ? N2 C21 Lu1 55.4(3) . . ? N1 C21 Lu1 58.5(3) . . ? C22 C21 Lu1 177.7(4) . . ? C27 C22 C23 118.1(5) . . ? C27 C22 C21 122.9(5) . . ? C23 C22 C21 119.1(5) . . ? C24 C23 C22 121.1(5) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 120.8(6) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C25 C24 118.4(6) . . ? C26 C25 H25 120.8 . . ? C24 C25 H25 120.8 . . ? C25 C26 C27 121.1(6) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C26 C27 C22 120.4(5) . . ? C26 C27 H27 119.8 . . ? C22 C27 H27 119.8 . . ? N1 C28 C29 120.2(5) . . ? N1 C28 C36 121.9(5) . . ? C29 C28 C36 117.9(5) . . ? C33 C29 C28 119.7(6) . . ? C33 C29 C30 118.5(5) . . ? C28 C29 C30 121.8(5) . . ? C29 C30 C32 111.2(5) . . ? C29 C30 C31 113.4(6) . . ? C32 C30 C31 111.4(5) . . ? C29 C30 H30 106.8 . . ? C32 C30 H30 106.8 . . ? C31 C30 H30 106.8 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C29 120.8(6) . . ? C34 C33 H33 119.6 . . ? C29 C33 H33 119.6 . . ? C35 C34 C33 120.0(6) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 121.2(6) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C35 C36 C28 120.4(5) . . ? C35 C36 C37 118.0(5) . . ? C28 C36 C37 121.4(5) . . ? C39 C37 C38 110.7(5) . . ? C39 C37 C36 110.5(5) . . ? C38 C37 C36 113.6(5) . . ? C39 C37 H37 107.2 . . ? C38 C37 H37 107.2 . . ? C36 C37 H37 107.2 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C48 120.1(5) . . ? C41 C40 N2 122.9(5) . . ? C48 C40 N2 116.7(5) . . ? C45 C41 C40 118.8(5) . . ? C45 C41 C42 117.2(5) . . ? C40 C41 C42 124.0(5) . . ? C44 C42 C41 112.3(5) . . ? C44 C42 C43 110.6(5) . . ? C41 C42 C43 110.0(5) . . ? C44 C42 H42 107.9 . . ? C41 C42 H42 107.9 . . ? C43 C42 H42 107.9 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C41 121.1(6) . . ? C46 C45 H45 119.4 . . ? C41 C45 H45 119.4 . . ? C47 C46 C45 119.5(5) . . ? C47 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? C46 C47 C48 122.6(6) . . ? C46 C47 H47 118.7 . . ? C48 C47 H47 118.7 . . ? C47 C48 C40 117.8(5) . . ? C47 C48 C49 119.5(5) . . ? C40 C48 C49 122.6(5) . . ? C50 C49 C48 111.7(5) . . ? C50 C49 C51 108.6(5) . . ? C48 C49 C51 112.7(5) . . ? C50 C49 H49 107.9 . . ? C48 C49 H49 107.9 . . ? C51 C49 H49 107.9 . . ? 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 . . ? N3 C52 N4 113.4(5) . . ? N3 C52 C53 122.2(5) . . ? N4 C52 C53 124.4(5) . . ? N3 C52 Lu2 58.7(3) . . ? N4 C52 Lu2 55.0(3) . . ? C53 C52 Lu2 174.1(4) . . ? C54 C53 C58 118.0(5) . . ? C54 C53 C52 121.1(5) . . ? C58 C53 C52 121.0(5) . . ? C55 C54 C53 120.4(6) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C54 C55 C56 120.7(6) . . ? C54 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? C57 C56 C55 120.2(6) . . ? C57 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C56 C57 C58 120.4(6) . . ? C56 C57 H57 119.8 . . ? C58 C57 H57 119.8 . . ? C57 C58 C53 120.3(6) . . ? C57 C58 H58 119.8 . . ? C53 C58 H58 119.8 . . ? C67 C59 C60 119.9(5) . . ? C67 C59 N3 122.8(5) . . ? C60 C59 N3 117.2(5) . . ? C64 C60 C59 118.0(6) . . ? C64 C60 C61 121.2(5) . . ? C59 C60 C61 120.8(5) . . ? C62 C61 C63 111.9(6) . . ? C62 C61 C60 110.3(5) . . ? C63 C61 C60 112.6(5) . . ? C62 C61 H61 107.2 . . ? C63 C61 H61 107.2 . . ? C60 C61 H61 107.2 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C60 C64 C65 123.0(6) . . ? C60 C64 H64 118.5 . . ? C65 C64 H64 118.5 . . ? C66 C65 C64 118.5(6) . . ? C66 C65 H65 120.7 . . ? C64 C65 H65 120.7 . . ? C65 C66 C67 121.8(6) . . ? C65 C66 H66 119.1 . . ? C67 C66 H66 119.1 . . ? C66 C67 C59 118.5(6) . . ? C66 C67 C68 116.4(6) . . ? C59 C67 C68 125.0(5) . . ? C69 C68 C67 112.5(5) . . ? C69 C68 C70 108.6(5) . . ? C67 C68 C70 113.4(5) . . ? C69 C68 H68 107.4 . . ? C67 C68 H68 107.4 . . ? C70 C68 H68 107.4 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C72 C71 C79 120.0(5) . . ? C72 C71 N4 123.1(5) . . ? C79 C71 N4 116.7(5) . . ? C76 C72 C71 118.2(6) . . ? C76 C72 C73 120.4(5) . . ? C71 C72 C73 121.3(5) . . ? C74 C73 C75 112.6(6) . . ? C74 C73 C72 110.2(5) . . ? C75 C73 C72 112.7(5) . . ? C74 C73 H73 107.0 . . ? C75 C73 H73 107.0 . . ? C72 C73 H73 107.0 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C73 C75 H75A 109.5 . . ? C73 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C73 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C77 C76 C72 121.8(6) . . ? C77 C76 H76 119.1 . . ? C72 C76 H76 119.1 . . ? C76 C77 C78 119.7(6) . . ? C76 C77 H77 120.1 . . ? C78 C77 H77 120.1 . . ? C79 C78 C77 121.7(6) . . ? C79 C78 H78 119.2 . . ? C77 C78 H78 119.2 . . ? C78 C79 C71 118.4(6) . . ? C78 C79 C80 120.5(5) . . ? C71 C79 C80 121.1(5) . . ? C82 C80 C79 117.1(6) . . ? C82 C80 C81 111.4(6) . . ? C79 C80 C81 113.0(6) . . ? C82 C80 H80 104.7 . . ? C79 C80 H80 104.7 . . ? C81 C80 H80 104.7 . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C80 C82 H82A 109.5 . . ? C80 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C80 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C21 N1 C28 119.1(5) . . ? C21 N1 Lu1 93.1(3) . . ? C28 N1 Lu1 143.0(3) . . ? C21 N2 C40 124.2(5) . . ? C21 N2 Lu1 96.3(3) . . ? C40 N2 Lu1 139.5(4) . . ? C52 N3 C59 126.4(5) . . ? C52 N3 Lu2 92.6(3) . . ? C59 N3 Lu2 138.9(4) . . ? C52 N4 C71 123.1(4) . . ? C52 N4 Lu2 96.4(3) . . ? C71 N4 Lu2 140.5(3) . . ? C17 O1 C20 109.5(5) . . ? C17 O1 Lu1 122.9(3) . . ? C20 O1 Lu1 127.4(4) . . ? O1 Lu1 N2 104.52(14) . . ? O1 Lu1 N1 90.26(14) . . ? N2 Lu1 N1 56.66(15) . . ? O1 Lu1 C3 91.30(18) . . ? N2 Lu1 C3 88.55(19) . . ? N1 Lu1 C3 144.30(18) . . ? O1 Lu1 C4 84.30(17) . . ? N2 Lu1 C4 121.06(17) . . ? N1 Lu1 C4 173.34(17) . . ? C3 Lu1 C4 32.53(19) . . ? O1 Lu1 C21 98.20(15) . . ? N2 Lu1 C21 28.25(14) . . ? N1 Lu1 C21 28.41(14) . . ? C3 Lu1 C21 116.44(19) . . ? C4 Lu1 C21 148.90(17) . . ? O1 Lu1 Lu2 114.60(10) . . ? N2 Lu1 Lu2 140.21(10) . . ? N1 Lu1 Lu2 114.30(10) . . ? C3 Lu1 Lu2 97.29(15) . . ? C4 Lu1 Lu2 71.65(14) . . ? C21 Lu1 Lu2 132.26(11) . . ? O1 Lu1 H1 148.1(15) . . ? N2 Lu1 H1 105.2(16) . . ? N1 Lu1 H1 96.4(16) . . ? C3 Lu1 H1 100.8(16) . . ? C4 Lu1 H1 90.2(16) . . ? C21 Lu1 H1 102.4(16) . . ? Lu2 Lu1 H1 35.0(15) . . ? O1 Lu1 H2 79.3(12) . . ? N2 Lu1 H2 153.1(14) . . ? N1 Lu1 H2 97.2(13) . . ? C3 Lu1 H2 118.1(14) . . ? C4 Lu1 H2 85.6(13) . . ? C21 Lu1 H2 125.4(13) . . ? Lu2 Lu1 H2 40.2(12) . . ? H1 Lu1 H2 68.9(19) . . ? N4 Lu2 N3 57.24(15) . . ? N4 Lu2 C8 104.43(18) . . ? N3 Lu2 C8 85.28(17) . . ? N4 Lu2 C9 120.62(19) . . ? N3 Lu2 C9 76.67(17) . . ? C8 Lu2 C9 31.1(2) . . ? N4 Lu2 C10 148.86(19) . . ? N3 Lu2 C10 94.74(18) . . ? C8 Lu2 C10 55.7(2) . . ? C9 Lu2 C10 30.41(19) . . ? N4 Lu2 C5 168.36(16) . . ? N3 Lu2 C5 126.81(17) . . ? C8 Lu2 C5 66.75(19) . . ? C9 Lu2 C5 55.76(19) . . ? C10 Lu2 C5 32.09(18) . . ? N4 Lu2 C7 113.26(17) . . ? N3 Lu2 C7 115.43(17) . . ? C8 Lu2 C7 31.17(19) . . ? C9 Lu2 C7 53.9(2) . . ? C10 Lu2 C7 63.7(2) . . ? C5 Lu2 C7 55.22(18) . . ? N4 Lu2 C6 136.76(18) . . ? N3 Lu2 C6 138.55(18) . . ? C8 Lu2 C6 54.85(19) . . ? C9 Lu2 C6 63.4(2) . . ? C10 Lu2 C6 55.4(2) . . ? C5 Lu2 C6 32.04(17) . . ? C7 Lu2 C6 29.34(18) . . ? N4 Lu2 C52 28.60(15) . . ? N3 Lu2 C52 28.74(15) . . ? C8 Lu2 C52 93.86(17) . . ? C9 Lu2 C52 98.11(18) . . ? C10 Lu2 C52 121.85(19) . . ? C5 Lu2 C52 153.34(18) . . ? C7 Lu2 C52 116.28(17) . . ? C6 Lu2 C52 145.62(17) . . ? N4 Lu2 Lu1 124.10(11) . . ? N3 Lu2 Lu1 136.52(10) . . ? C8 Lu2 Lu1 127.20(14) . . ? C9 Lu2 Lu1 114.94(15) . . ? C10 Lu2 Lu1 84.97(15) . . ? C5 Lu2 Lu1 62.02(13) . . ? C7 Lu2 Lu1 103.34(14) . . ? C6 Lu2 Lu1 74.60(14) . . ? C52 Lu2 Lu1 138.76(10) . . ? N4 Lu2 H1 103.1(15) . . ? N3 Lu2 H1 149.8(15) . . ? C8 Lu2 H1 123.9(14) . . ? C9 Lu2 H1 132.1(15) . . ? C10 Lu2 H1 108.0(15) . . ? C5 Lu2 H1 77.4(15) . . ? C7 Lu2 H1 92.8(14) . . ? C6 Lu2 H1 71.7(15) . . ? C52 Lu2 H1 129.2(15) . . ? Lu1 Lu2 H1 32.7(14) . . ? N4 Lu2 H2 107.5(14) . . ? N3 Lu2 H2 93.2(14) . . ? C8 Lu2 H2 140.8(14) . . ? C9 Lu2 H2 110.6(14) . . ? C10 Lu2 H2 85.5(14) . . ? C5 Lu2 H2 83.7(14) . . ? C7 Lu2 H2 138.4(14) . . ? C6 Lu2 H2 110.2(14) . . ? C52 Lu2 H2 103.4(14) . . ? Lu1 Lu2 H2 43.4(14) . . ? H1 Lu2 H2 69.7(19) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.051 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.114 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.076 0.500 0.343 1449 460 ' ' _platon_squeeze_details ; 3 disorder cyclohexane molecules per formual unit of [(Ph-NCN)LuH]2(THF)(PhCHCHPh) were not modelled and the disordered density was taken into account using the SQUEEZE/PLATON procedure. (Sluis, P. van der; Spek, A. L. Acta Crystallogr.1990, A46, 194?01) as implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst. 2003, 36, 7?3. PLATON - a multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands). ; data_5-Y _database_code_depnum_ccdc_archive 'CCDC 859490' #TrackingRef '- Ln2H4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((PhNCN)YH(THF))2(PhCHCCCHPh) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H108 N4 O2 Y2' _chemical_formula_weight 1407.58 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.731(3) _cell_length_b 15.277(3) _cell_length_c 22.821(5) _cell_angle_alpha 97.855(3) _cell_angle_beta 98.334(3) _cell_angle_gamma 99.894(3) _cell_volume 4601.5(17) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow-brown _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.016 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 1.295 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5753 _exptl_absorpt_correction_T_max 0.6059 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 24189 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0777 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15874 _reflns_number_gt 11144 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0611P)^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 15874 _refine_ls_number_parameters 867 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _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 C3 C 0.3757(2) 0.1445(2) 0.38631(14) 0.0302(7) Uani 1 1 d . . . C4 C 0.4444(2) 0.0950(2) 0.36530(13) 0.0302(7) Uani 1 1 d . B . C5 C 0.5203(2) 0.08015(19) 0.34567(14) 0.0314(7) Uani 1 1 d . B . C6 C 0.5920(2) 0.0336(2) 0.32667(15) 0.0325(7) Uani 1 1 d . B . C7 C 0.6506(2) -0.0142(2) 0.36574(14) 0.0320(7) Uani 1 1 d . . . C8 C 0.7348(2) -0.0451(2) 0.34895(15) 0.0365(8) Uani 1 1 d . . . H8 H 0.7529 -0.0361 0.3113 0.044 Uiso 1 1 calc R . . C9 C 0.7914(3) -0.0883(2) 0.38598(18) 0.0479(9) Uani 1 1 d . . . H9 H 0.8483 -0.1079 0.3735 0.057 Uiso 1 1 calc R . . C10 C 0.7676(3) -0.1035(2) 0.44036(17) 0.0504(10) Uani 1 1 d . . . H10 H 0.8073 -0.1332 0.4657 0.060 Uiso 1 1 calc R . . C11 C 0.6845(3) -0.0748(2) 0.45742(16) 0.0484(9) Uani 1 1 d . . . H11 H 0.6663 -0.0857 0.4947 0.058 Uiso 1 1 calc R . . C12 C 0.6274(2) -0.0304(2) 0.42120(14) 0.0372(8) Uani 1 1 d . . . H12 H 0.5712 -0.0104 0.4344 0.045 Uiso 1 1 calc R . . C13 C 0.4075(2) 0.22780(19) 0.43072(13) 0.0284(7) Uani 1 1 d . . . C14 C 0.5056(3) 0.2762(2) 0.44318(14) 0.0383(8) Uani 1 1 d . . . H14 H 0.5550 0.2546 0.4232 0.046 Uiso 1 1 calc R . . C15 C 0.5326(3) 0.3556(2) 0.48426(16) 0.0474(9) Uani 1 1 d . . . H15 H 0.5997 0.3884 0.4914 0.057 Uiso 1 1 calc R . . C16 C 0.4627(3) 0.3875(2) 0.51502(16) 0.0460(9) Uani 1 1 d . . . H16 H 0.4818 0.4415 0.5436 0.055 Uiso 1 1 calc R . . C17 C 0.3653(3) 0.3405(2) 0.50380(15) 0.0438(9) Uani 1 1 d . . . H17 H 0.3168 0.3614 0.5249 0.053 Uiso 1 1 calc R . . C18 C 0.3384(2) 0.2626(2) 0.46169(14) 0.0345(8) Uani 1 1 d . . . H18 H 0.2704 0.2316 0.4535 0.041 Uiso 1 1 calc R . . C19 C 0.3318(3) -0.1033(3) 0.39569(18) 0.0577(11) Uani 1 1 d . B . H19A H 0.2575 -0.1155 0.3881 0.069 Uiso 1 1 calc R . . H19B H 0.3567 -0.0383 0.4109 0.069 Uiso 1 1 calc R . . C20 C 0.3704(3) -0.1583(3) 0.43941(18) 0.0645(12) Uani 1 1 d . . . H20A H 0.3295 -0.1640 0.4715 0.077 Uiso 1 1 calc R A 1 H20B H 0.4417 -0.1344 0.4575 0.077 Uiso 1 1 calc R A 1 C21 C 0.4020(15) -0.2305(13) 0.4087(8) 0.060(3) Uani 0.487(18) 1 d P B 2 H21A H 0.3581 -0.2880 0.4112 0.072 Uiso 0.487(18) 1 calc PR B 2 H21B H 0.4717 -0.2323 0.4263 0.072 Uiso 0.487(18) 1 calc PR B 2 C21' C 0.3557(14) -0.2513(12) 0.3936(8) 0.060(3) Uani 0.513(18) 1 d P B 1 H21C H 0.3946 -0.2937 0.4105 0.072 Uiso 0.513(18) 1 calc PR B 1 H21D H 0.2841 -0.2809 0.3817 0.072 Uiso 0.513(18) 1 calc PR B 1 C22 C 0.3962(4) -0.2168(3) 0.34444(19) 0.0696(13) Uani 1 1 d . . . H22A H 0.4701 -0.2107 0.3514 0.083 Uiso 1 1 calc R B 1 H22B H 0.3680 -0.2588 0.3064 0.083 Uiso 1 1 calc R B 1 C23 C 0.6027(3) 0.2583(3) 0.2843(2) 0.0559(10) Uani 1 1 d . . . H23A H 0.6052 0.2181 0.2468 0.067 Uiso 1 1 calc R . . H23B H 0.6306 0.2325 0.3191 0.067 Uiso 1 1 calc R . . C24 C 0.6599(3) 0.3520(3) 0.2853(2) 0.0783(14) Uani 1 1 d . . . H24A H 0.7317 0.3582 0.3027 0.094 Uiso 1 1 calc R . . H24B H 0.6547 0.3677 0.2445 0.094 Uiso 1 1 calc R . . C25 C 0.6097(4) 0.4093(3) 0.3242(2) 0.0775(15) Uani 1 1 d . . . H25A H 0.6198 0.4718 0.3158 0.093 Uiso 1 1 calc R . . H25B H 0.6346 0.4103 0.3672 0.093 Uiso 1 1 calc R . . C26 C 0.5014(3) 0.3636(2) 0.30679(18) 0.0539(10) Uani 1 1 d . . . H26A H 0.4663 0.3713 0.3415 0.065 Uiso 1 1 calc R . . H26B H 0.4676 0.3895 0.2739 0.065 Uiso 1 1 calc R . . C27 C 0.4222(2) -0.19257(19) 0.17507(13) 0.0254(7) Uani 1 1 d . B . C28 C 0.4208(2) -0.27582(19) 0.13150(13) 0.0297(7) Uani 1 1 d . . . C29 C 0.4911(3) -0.2811(2) 0.09352(14) 0.0370(8) Uani 1 1 d . . . H29 H 0.5419 -0.2301 0.0939 0.044 Uiso 1 1 calc R . . C30 C 0.4869(3) -0.3611(2) 0.05507(15) 0.0481(10) Uani 1 1 d . . . H30 H 0.5343 -0.3642 0.0288 0.058 Uiso 1 1 calc R . . C31 C 0.4150(3) -0.4356(2) 0.05469(16) 0.0501(10) Uani 1 1 d . . . H31 H 0.4128 -0.4899 0.0282 0.060 Uiso 1 1 calc R . . C32 C 0.3466(3) -0.4318(2) 0.09241(16) 0.0457(9) Uani 1 1 d . . . H32 H 0.2976 -0.4839 0.0925 0.055 Uiso 1 1 calc R . . C33 C 0.3481(2) -0.3528(2) 0.13042(15) 0.0371(8) Uani 1 1 d . . . H33 H 0.2995 -0.3507 0.1560 0.045 Uiso 1 1 calc R . . C34 C 0.2482(2) -0.19090(18) 0.14127(13) 0.0267(7) Uani 1 1 d . . . C35 C 0.2463(2) -0.17178(19) 0.08233(14) 0.0341(8) Uani 1 1 d . . . C36 C 0.3361(3) -0.1189(2) 0.06258(14) 0.0367(8) Uani 1 1 d . . . H36 H 0.3969 -0.1192 0.0925 0.044 Uiso 1 1 calc R . . C37 C 0.3256(3) -0.0209(2) 0.06289(17) 0.0506(10) Uani 1 1 d . . . H37A H 0.3845 0.0124 0.0503 0.076 Uiso 1 1 calc R . . H37B H 0.3207 0.0064 0.1035 0.076 Uiso 1 1 calc R . . H37C H 0.2650 -0.0187 0.0350 0.076 Uiso 1 1 calc R . . C38 C 0.3537(3) -0.1597(2) 0.00076(16) 0.0573(11) Uani 1 1 d . . . H38A H 0.4126 -0.1228 -0.0095 0.086 Uiso 1 1 calc R . . H38B H 0.2946 -0.1613 -0.0295 0.086 Uiso 1 1 calc R . . H38C H 0.3652 -0.2211 0.0017 0.086 Uiso 1 1 calc R . . C39 C 0.1564(3) -0.1971(2) 0.04247(15) 0.0444(9) Uani 1 1 d . . . H39 H 0.1546 -0.1851 0.0026 0.053 Uiso 1 1 calc R . . C40 C 0.0703(3) -0.2386(2) 0.05850(18) 0.0526(10) Uani 1 1 d . . . H40 H 0.0102 -0.2562 0.0298 0.063 Uiso 1 1 calc R . . C41 C 0.0710(3) -0.2547(2) 0.11646(17) 0.0451(9) Uani 1 1 d . . . H41 H 0.0106 -0.2822 0.1278 0.054 Uiso 1 1 calc R . . C42 C 0.1598(2) -0.2312(2) 0.15886(15) 0.0339(8) Uani 1 1 d . . . C43 C 0.1571(2) -0.2488(2) 0.22171(16) 0.0410(8) Uani 1 1 d . . . H43 H 0.2283 -0.2418 0.2420 0.049 Uiso 1 1 calc R . . C44 C 0.1112(3) -0.1805(3) 0.25683(19) 0.0596(11) Uani 1 1 d . . . H44A H 0.1109 -0.1937 0.2977 0.089 Uiso 1 1 calc R . . H44B H 0.0421 -0.1835 0.2370 0.089 Uiso 1 1 calc R . . H44C H 0.1506 -0.1200 0.2586 0.089 Uiso 1 1 calc R . . C45 C 0.1036(4) -0.3431(3) 0.2252(2) 0.0721(13) Uani 1 1 d . . . H45A H 0.1052 -0.3499 0.2674 0.108 Uiso 1 1 calc R . . H45B H 0.1374 -0.3875 0.2056 0.108 Uiso 1 1 calc R . . H45C H 0.0338 -0.3527 0.2049 0.108 Uiso 1 1 calc R . . C46 C 0.6034(2) -0.1619(2) 0.20679(13) 0.0290(7) Uani 1 1 d . . . C47 C 0.6348(2) -0.2377(2) 0.22654(14) 0.0356(8) Uani 1 1 d . . . C48 C 0.5701(2) -0.3052(2) 0.25390(14) 0.0356(8) Uani 1 1 d . . . H48 H 0.5018 -0.2897 0.2501 0.043 Uiso 1 1 calc R . . C49 C 0.6088(3) -0.2998(3) 0.32093(16) 0.0514(10) Uani 1 1 d . . . H49A H 0.5648 -0.3445 0.3371 0.077 Uiso 1 1 calc R . . H49B H 0.6095 -0.2394 0.3421 0.077 Uiso 1 1 calc R . . H49C H 0.6771 -0.3120 0.3265 0.077 Uiso 1 1 calc R . . C50 C 0.5574(3) -0.4026(2) 0.22143(17) 0.0498(10) Uani 1 1 d . . . H50A H 0.5147 -0.4433 0.2411 0.075 Uiso 1 1 calc R . . H50B H 0.6234 -0.4195 0.2230 0.075 Uiso 1 1 calc R . . H50C H 0.5262 -0.4070 0.1794 0.075 Uiso 1 1 calc R . . C51 C 0.7315(3) -0.2497(2) 0.22126(17) 0.0462(9) Uani 1 1 d . . . H51 H 0.7534 -0.3011 0.2336 0.055 Uiso 1 1 calc R . . C52 C 0.7963(3) -0.1894(3) 0.19866(18) 0.0525(10) Uani 1 1 d . . . H52 H 0.8620 -0.1993 0.1955 0.063 Uiso 1 1 calc R . . C53 C 0.7660(3) -0.1149(2) 0.18075(16) 0.0450(9) Uani 1 1 d . . . H53 H 0.8111 -0.0734 0.1652 0.054 Uiso 1 1 calc R . . C54 C 0.6703(2) -0.0987(2) 0.18487(15) 0.0368(8) Uani 1 1 d . . . C55 C 0.6394(3) -0.0163(2) 0.16280(16) 0.0420(9) Uani 1 1 d . . . H55 H 0.5757 -0.0082 0.1773 0.050 Uiso 1 1 calc R . . C56 C 0.7175(3) 0.0699(2) 0.1871(2) 0.0601(11) Uani 1 1 d . . . H56A H 0.6938 0.1210 0.1721 0.090 Uiso 1 1 calc R . . H56B H 0.7810 0.0637 0.1738 0.090 Uiso 1 1 calc R . . H56C H 0.7279 0.0805 0.2311 0.090 Uiso 1 1 calc R . . C57 C 0.6187(3) -0.0299(3) 0.09420(18) 0.0614(11) Uani 1 1 d . . . H57A H 0.5987 0.0239 0.0811 0.092 Uiso 1 1 calc R . . H57B H 0.5645 -0.0823 0.0788 0.092 Uiso 1 1 calc R . . H57C H 0.6796 -0.0400 0.0788 0.092 Uiso 1 1 calc R . . C58 C 0.2033(2) 0.23718(18) 0.22760(13) 0.0252(7) Uani 1 1 d . . . C59 C 0.1303(2) 0.2913(2) 0.20359(13) 0.0323(7) Uani 1 1 d . . . C60 C 0.1588(3) 0.3529(2) 0.16658(15) 0.0444(9) Uani 1 1 d . . . H60 H 0.2239 0.3592 0.1562 0.053 Uiso 1 1 calc R . . C61 C 0.0939(4) 0.4050(3) 0.14485(17) 0.0598(11) Uani 1 1 d . . . H61 H 0.1147 0.4474 0.1201 0.072 Uiso 1 1 calc R . . C62 C -0.0004(4) 0.3959(3) 0.15877(18) 0.0639(13) Uani 1 1 d . . . H62 H -0.0446 0.4323 0.1439 0.077 Uiso 1 1 calc R . . C63 C -0.0315(3) 0.3348(3) 0.19397(18) 0.0557(11) Uani 1 1 d . . . H63 H -0.0979 0.3277 0.2025 0.067 Uiso 1 1 calc R . . C64 C 0.0342(2) 0.2824(2) 0.21759(15) 0.0392(8) Uani 1 1 d . . . H64 H 0.0132 0.2412 0.2430 0.047 Uiso 1 1 calc R . . C65 C 0.2431(2) 0.18909(19) 0.12987(13) 0.0294(7) Uani 1 1 d . . . C66 C 0.3211(2) 0.22286(19) 0.09987(14) 0.0330(7) Uani 1 1 d . . . C67 C 0.4243(2) 0.2715(2) 0.13422(15) 0.0370(8) Uani 1 1 d . . . H67 H 0.4231 0.2712 0.1779 0.044 Uiso 1 1 calc R . . C68 C 0.5058(3) 0.2225(3) 0.1178(2) 0.0760(14) Uani 1 1 d . . . H68A H 0.5709 0.2555 0.1404 0.114 Uiso 1 1 calc R . . H68B H 0.5066 0.2188 0.0747 0.114 Uiso 1 1 calc R . . H68C H 0.4926 0.1616 0.1277 0.114 Uiso 1 1 calc R . . C69 C 0.4489(4) 0.3692(2) 0.1257(2) 0.0726(13) Uani 1 1 d . . . H69A H 0.3957 0.4001 0.1368 0.109 Uiso 1 1 calc R . . H69B H 0.4541 0.3719 0.0836 0.109 Uiso 1 1 calc R . . H69C H 0.5129 0.3988 0.1513 0.109 Uiso 1 1 calc R . . C70 C 0.3025(3) 0.2118(2) 0.03777(15) 0.0460(9) Uani 1 1 d . . . H70 H 0.3543 0.2349 0.0173 0.055 Uiso 1 1 calc R . . C71 C 0.2114(3) 0.1684(2) 0.00512(16) 0.0520(10) Uani 1 1 d . . . H71 H 0.1996 0.1632 -0.0374 0.062 Uiso 1 1 calc R . . C72 C 0.1368(3) 0.1322(2) 0.03433(15) 0.0440(9) Uani 1 1 d . . . H72 H 0.0742 0.1011 0.0113 0.053 Uiso 1 1 calc R . . C73 C 0.1509(2) 0.1401(2) 0.09663(14) 0.0340(8) Uani 1 1 d . . . C74 C 0.0698(2) 0.0907(2) 0.12544(15) 0.0367(8) Uani 1 1 d . . . H74 H 0.0814 0.1193 0.1686 0.044 Uiso 1 1 calc R . . C75 C -0.0360(3) 0.0977(3) 0.09798(18) 0.0595(11) Uani 1 1 d . . . H75A H -0.0846 0.0653 0.1188 0.089 Uiso 1 1 calc R . . H75B H -0.0496 0.0712 0.0553 0.089 Uiso 1 1 calc R . . H75C H -0.0418 0.1612 0.1022 0.089 Uiso 1 1 calc R . . C76 C 0.0795(3) -0.0078(2) 0.1237(2) 0.0601(11) Uani 1 1 d . . . H76A H 0.0269 -0.0390 0.1425 0.090 Uiso 1 1 calc R . . H76B H 0.1455 -0.0106 0.1456 0.090 Uiso 1 1 calc R . . H76C H 0.0724 -0.0370 0.0819 0.090 Uiso 1 1 calc R . . C77 C 0.1646(2) 0.2547(2) 0.32953(13) 0.0281(7) Uani 1 1 d . . . C78 C 0.1785(2) 0.3469(2) 0.35317(13) 0.0336(7) Uani 1 1 d . . . C79 C 0.2469(2) 0.4207(2) 0.33247(14) 0.0339(8) Uani 1 1 d . . . H79 H 0.2768 0.3918 0.2992 0.041 Uiso 1 1 calc R . . C80 C 0.3335(3) 0.4690(2) 0.38293(16) 0.0489(9) Uani 1 1 d . . . H80A H 0.3767 0.5159 0.3680 0.073 Uiso 1 1 calc R . . H80B H 0.3728 0.4254 0.3963 0.073 Uiso 1 1 calc R . . H80C H 0.3063 0.4966 0.4167 0.073 Uiso 1 1 calc R . . C81 C 0.1924(3) 0.4904(2) 0.30814(16) 0.0478(9) Uani 1 1 d . . . H81A H 0.2404 0.5357 0.2950 0.072 Uiso 1 1 calc R . . H81B H 0.1618 0.5196 0.3397 0.072 Uiso 1 1 calc R . . H81C H 0.1400 0.4606 0.2740 0.072 Uiso 1 1 calc R . . C82 C 0.1268(3) 0.3707(2) 0.39940(15) 0.0427(9) Uani 1 1 d . . . H82 H 0.1347 0.4325 0.4160 0.051 Uiso 1 1 calc R . . C83 C 0.0647(3) 0.3077(3) 0.42181(16) 0.0498(10) Uani 1 1 d . . . H83 H 0.0297 0.3259 0.4529 0.060 Uiso 1 1 calc R . . C84 C 0.0540(3) 0.2180(2) 0.39867(15) 0.0433(9) Uani 1 1 d . . . H84 H 0.0114 0.1745 0.4143 0.052 Uiso 1 1 calc R . . C85 C 0.1038(2) 0.1893(2) 0.35317(13) 0.0315(7) Uani 1 1 d . . . C86 C 0.0875(2) 0.0888(2) 0.32927(15) 0.0375(8) Uani 1 1 d . . . H86 H 0.1436 0.0788 0.3072 0.045 Uiso 1 1 calc R . . C87 C -0.0111(3) 0.0576(2) 0.28446(17) 0.0573(11) Uani 1 1 d . . . H87A H -0.0199 -0.0070 0.2694 0.086 Uiso 1 1 calc R . . H87B H -0.0092 0.0911 0.2508 0.086 Uiso 1 1 calc R . . H87C H -0.0673 0.0687 0.3045 0.086 Uiso 1 1 calc R . . C88 C 0.0885(3) 0.0308(2) 0.37869(17) 0.0495(9) Uani 1 1 d . . . H88A H 0.0785 -0.0328 0.3606 0.074 Uiso 1 1 calc R . . H88B H 0.0344 0.0396 0.4012 0.074 Uiso 1 1 calc R . . H88C H 0.1532 0.0483 0.4059 0.074 Uiso 1 1 calc R . . N1 N 0.33824(18) -0.16400(15) 0.18425(10) 0.0262(6) Uani 1 1 d . B . N2 N 0.50555(18) -0.14443(15) 0.21026(11) 0.0276(6) Uani 1 1 d . B . N3 N 0.26244(18) 0.20005(15) 0.19382(10) 0.0254(5) Uani 1 1 d . . . N4 N 0.21846(17) 0.22290(15) 0.28425(10) 0.0260(6) Uani 1 1 d . . . O1 O 0.37006(17) -0.13077(14) 0.34078(10) 0.0402(6) Uani 1 1 d . B . O2 O 0.50048(15) 0.26938(13) 0.28739(10) 0.0379(5) Uani 1 1 d . . . Y1 Y 0.41962(2) -0.049720(18) 0.266803(13) 0.02552(9) Uani 1 1 d . . . Y2 Y 0.35889(2) 0.153656(18) 0.275429(12) 0.02489(9) Uani 1 1 d . B . H2 H 0.291(2) 0.0121(19) 0.2639(13) 0.040(9) Uiso 1 1 d . . . H1 H 0.437(2) 0.0668(18) 0.2237(13) 0.039(9) Uiso 1 1 d . . . H6 H 0.618(2) 0.053(2) 0.2957(14) 0.033(9) Uiso 1 1 d . . . H3 H 0.310(3) 0.110(2) 0.3863(15) 0.047(10) 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 C3 0.0267(18) 0.0321(17) 0.0319(18) 0.0051(14) 0.0051(14) 0.0064(15) C4 0.0301(18) 0.0323(17) 0.0280(17) 0.0110(14) -0.0032(14) 0.0074(14) C5 0.0322(19) 0.0274(17) 0.0319(18) 0.0041(14) 0.0021(14) 0.0013(14) C6 0.0310(18) 0.0362(18) 0.0318(19) 0.0094(15) 0.0070(15) 0.0062(15) C7 0.0244(17) 0.0304(17) 0.0371(19) 0.0023(14) 0.0015(14) -0.0001(14) C8 0.0354(19) 0.0382(18) 0.0338(19) 0.0048(15) 0.0027(15) 0.0055(16) C9 0.035(2) 0.046(2) 0.062(3) 0.0074(19) 0.0016(18) 0.0125(17) C10 0.053(2) 0.052(2) 0.045(2) 0.0128(18) -0.0057(18) 0.0147(19) C11 0.055(2) 0.056(2) 0.036(2) 0.0154(18) 0.0045(18) 0.010(2) C12 0.0351(19) 0.0407(19) 0.0356(19) 0.0069(15) 0.0055(15) 0.0066(16) C13 0.0343(18) 0.0298(16) 0.0212(16) 0.0093(13) -0.0018(13) 0.0074(14) C14 0.036(2) 0.044(2) 0.0332(19) 0.0055(16) -0.0014(15) 0.0081(16) C15 0.042(2) 0.043(2) 0.046(2) 0.0060(17) -0.0096(18) -0.0042(18) C16 0.059(3) 0.0366(19) 0.035(2) 0.0013(16) -0.0100(18) 0.0083(19) C17 0.057(2) 0.042(2) 0.034(2) 0.0037(16) 0.0022(17) 0.0200(19) C18 0.0376(19) 0.0342(18) 0.0317(18) 0.0072(15) 0.0014(14) 0.0093(15) C19 0.081(3) 0.049(2) 0.060(3) 0.021(2) 0.044(2) 0.024(2) C20 0.075(3) 0.080(3) 0.049(3) 0.027(2) 0.031(2) 0.014(2) C21 0.074(10) 0.061(7) 0.055(8) 0.030(6) 0.020(7) 0.019(8) C21' 0.074(10) 0.061(7) 0.055(8) 0.030(6) 0.020(7) 0.019(8) C22 0.115(4) 0.058(3) 0.053(3) 0.024(2) 0.020(2) 0.050(3) C23 0.029(2) 0.060(2) 0.081(3) 0.021(2) 0.0124(19) 0.0030(18) C24 0.051(3) 0.074(3) 0.099(4) 0.028(3) 0.006(3) -0.023(2) C25 0.088(4) 0.043(2) 0.083(3) 0.019(2) -0.017(3) -0.018(2) C26 0.066(3) 0.0287(19) 0.063(3) 0.0093(17) 0.000(2) 0.0051(18) C27 0.0291(17) 0.0272(16) 0.0238(16) 0.0111(13) 0.0099(13) 0.0058(14) C28 0.0341(18) 0.0259(16) 0.0303(17) 0.0053(13) 0.0033(14) 0.0109(14) C29 0.048(2) 0.0368(18) 0.0301(18) 0.0074(15) 0.0076(15) 0.0169(16) C30 0.075(3) 0.044(2) 0.034(2) 0.0072(17) 0.0164(18) 0.027(2) C31 0.072(3) 0.037(2) 0.040(2) -0.0012(17) -0.003(2) 0.025(2) C32 0.049(2) 0.0306(19) 0.052(2) 0.0006(17) -0.0062(18) 0.0093(17) C33 0.0342(19) 0.0330(18) 0.045(2) 0.0080(15) 0.0028(15) 0.0101(15) C34 0.0302(17) 0.0185(15) 0.0315(17) 0.0028(13) 0.0033(13) 0.0078(13) C35 0.044(2) 0.0254(16) 0.0339(19) 0.0021(14) 0.0020(15) 0.0168(15) C36 0.046(2) 0.0369(18) 0.0334(19) 0.0132(15) 0.0090(15) 0.0165(16) C37 0.059(3) 0.041(2) 0.059(3) 0.0139(18) 0.018(2) 0.0162(18) C38 0.088(3) 0.050(2) 0.043(2) 0.0098(18) 0.024(2) 0.025(2) C39 0.053(2) 0.044(2) 0.033(2) 0.0046(16) -0.0064(17) 0.0141(19) C40 0.046(2) 0.048(2) 0.055(3) 0.0031(19) -0.0187(19) 0.0112(19) C41 0.033(2) 0.0343(19) 0.062(3) 0.0108(17) -0.0064(17) -0.0002(16) C42 0.0290(18) 0.0306(17) 0.043(2) 0.0129(15) 0.0007(15) 0.0078(14) C43 0.0274(18) 0.045(2) 0.052(2) 0.0206(17) 0.0061(16) 0.0033(16) C44 0.058(3) 0.063(3) 0.062(3) 0.017(2) 0.022(2) 0.011(2) C45 0.081(3) 0.052(3) 0.091(4) 0.034(2) 0.026(3) 0.008(2) C46 0.0268(17) 0.0318(17) 0.0282(17) 0.0032(13) 0.0056(13) 0.0060(14) C47 0.038(2) 0.0365(18) 0.0320(18) 0.0047(15) 0.0005(15) 0.0124(16) C48 0.0378(19) 0.0331(18) 0.0389(19) 0.0101(15) 0.0032(15) 0.0148(15) C49 0.055(2) 0.062(2) 0.041(2) 0.0161(18) 0.0038(18) 0.021(2) C50 0.054(2) 0.042(2) 0.057(2) 0.0129(18) 0.0061(19) 0.0193(18) C51 0.032(2) 0.050(2) 0.060(2) 0.0122(19) 0.0036(17) 0.0193(18) C52 0.028(2) 0.065(3) 0.067(3) 0.005(2) 0.0098(18) 0.0211(19) C53 0.031(2) 0.053(2) 0.052(2) 0.0087(18) 0.0179(17) 0.0040(17) C54 0.0352(19) 0.0416(19) 0.0363(19) 0.0073(15) 0.0110(15) 0.0101(16) C55 0.042(2) 0.043(2) 0.050(2) 0.0182(17) 0.0234(17) 0.0130(17) C56 0.062(3) 0.047(2) 0.081(3) 0.017(2) 0.040(2) 0.011(2) C57 0.069(3) 0.060(3) 0.064(3) 0.031(2) 0.019(2) 0.014(2) C58 0.0232(16) 0.0235(15) 0.0265(17) 0.0023(13) 0.0017(12) 0.0020(13) C59 0.040(2) 0.0348(18) 0.0228(16) -0.0007(14) -0.0005(14) 0.0185(15) C60 0.063(2) 0.044(2) 0.034(2) 0.0112(16) 0.0125(17) 0.0266(19) C61 0.089(3) 0.062(3) 0.041(2) 0.0182(19) 0.009(2) 0.043(3) C62 0.079(3) 0.067(3) 0.048(3) 0.005(2) -0.015(2) 0.048(3) C63 0.043(2) 0.067(3) 0.054(3) -0.011(2) -0.0052(19) 0.029(2) C64 0.036(2) 0.044(2) 0.0351(19) -0.0009(15) -0.0027(15) 0.0145(16) C65 0.042(2) 0.0280(16) 0.0226(16) 0.0071(13) 0.0069(14) 0.0169(15) C66 0.048(2) 0.0264(16) 0.0305(18) 0.0090(14) 0.0150(15) 0.0135(15) C67 0.045(2) 0.0332(18) 0.0376(19) 0.0109(15) 0.0208(16) 0.0059(16) C68 0.051(3) 0.066(3) 0.108(4) 0.003(3) 0.016(3) 0.013(2) C69 0.081(3) 0.040(2) 0.092(4) 0.013(2) 0.011(3) 0.004(2) C70 0.071(3) 0.043(2) 0.031(2) 0.0075(16) 0.0212(19) 0.018(2) C71 0.083(3) 0.054(2) 0.0231(19) 0.0106(17) 0.010(2) 0.022(2) C72 0.058(2) 0.042(2) 0.0290(19) -0.0008(16) -0.0036(17) 0.0180(18) C73 0.042(2) 0.0283(17) 0.0318(18) 0.0017(14) 0.0021(15) 0.0125(15) C74 0.0350(19) 0.0354(18) 0.0344(19) -0.0031(15) -0.0011(15) 0.0051(15) C75 0.041(2) 0.080(3) 0.053(3) -0.001(2) -0.0007(18) 0.018(2) C76 0.060(3) 0.039(2) 0.084(3) 0.010(2) 0.024(2) 0.0081(19) C77 0.0255(17) 0.0378(18) 0.0206(16) 0.0026(13) 0.0013(12) 0.0090(14) C78 0.0352(19) 0.0386(18) 0.0258(17) 0.0032(14) -0.0002(14) 0.0099(15) C79 0.0390(19) 0.0333(17) 0.0283(17) 0.0031(14) 0.0011(14) 0.0095(15) C80 0.053(2) 0.043(2) 0.043(2) 0.0021(17) -0.0041(17) 0.0026(18) C81 0.057(2) 0.038(2) 0.048(2) 0.0036(17) 0.0020(18) 0.0153(18) C82 0.047(2) 0.046(2) 0.036(2) -0.0028(16) 0.0090(16) 0.0178(18) C83 0.056(2) 0.065(3) 0.037(2) 0.0042(19) 0.0235(18) 0.025(2) C84 0.037(2) 0.050(2) 0.044(2) 0.0074(17) 0.0147(16) 0.0046(17) C85 0.0257(17) 0.0408(18) 0.0283(17) 0.0053(14) 0.0068(13) 0.0059(15) C86 0.0310(19) 0.0410(19) 0.041(2) 0.0054(16) 0.0131(15) 0.0040(15) C87 0.056(3) 0.050(2) 0.056(3) 0.0074(19) -0.002(2) -0.007(2) C88 0.051(2) 0.045(2) 0.056(2) 0.0137(18) 0.0152(19) 0.0087(18) N1 0.0270(14) 0.0272(13) 0.0258(14) 0.0060(11) 0.0037(11) 0.0090(11) N2 0.0255(14) 0.0280(13) 0.0316(14) 0.0076(11) 0.0071(11) 0.0079(11) N3 0.0291(14) 0.0269(13) 0.0224(13) 0.0057(10) 0.0051(11) 0.0096(11) N4 0.0274(14) 0.0310(14) 0.0209(13) 0.0052(11) 0.0056(10) 0.0072(11) O1 0.0534(15) 0.0366(13) 0.0384(13) 0.0124(10) 0.0189(11) 0.0159(11) O2 0.0291(12) 0.0317(12) 0.0529(15) 0.0112(10) 0.0054(10) 0.0036(10) Y1 0.02685(17) 0.02520(16) 0.02610(17) 0.00612(12) 0.00541(12) 0.00726(13) Y2 0.02439(17) 0.02438(16) 0.02669(17) 0.00597(12) 0.00424(12) 0.00570(12) _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 C3 C4 1.403(4) . ? C3 C13 1.471(4) . ? C3 Y2 2.533(3) . ? C3 H3 0.96(3) . ? C4 C5 1.237(4) . ? C4 Y2 2.560(3) . ? C4 Y1 2.867(3) . ? C5 C6 1.393(4) . ? C5 Y1 2.539(3) . ? C5 Y2 3.010(3) . ? C6 C7 1.466(4) . ? C6 Y1 2.576(3) . ? C6 H6 0.90(3) . ? C7 C12 1.393(4) . ? C7 C8 1.404(4) . ? C8 C9 1.375(5) . ? C8 H8 0.9500 . ? C9 C10 1.368(5) . ? C9 H9 0.9500 . ? C10 C11 1.378(5) . ? C10 H10 0.9500 . ? C11 C12 1.381(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.389(4) . ? C13 C18 1.396(4) . ? C14 C15 1.386(5) . ? C14 H14 0.9500 . ? C15 C16 1.383(5) . ? C15 H15 0.9500 . ? C16 C17 1.375(5) . ? C16 H16 0.9500 . ? C17 C18 1.382(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 O1 1.465(4) . ? C19 C20 1.486(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.39(2) . ? C20 C21' 1.61(2) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.501(18) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21' C22 1.446(17) . ? C21' H21C 0.9900 . ? C21' H21D 0.9900 . ? C22 O1 1.430(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O2 1.453(4) . ? C23 C24 1.506(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.484(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.500(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O2 1.444(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 N2 1.333(4) . ? C27 N1 1.335(4) . ? C27 C28 1.499(4) . ? C27 Y1 2.819(3) . ? C28 C29 1.393(4) . ? C28 C33 1.400(4) . ? C29 C30 1.391(4) . ? C29 H29 0.9500 . ? C30 C31 1.370(5) . ? C30 H30 0.9500 . ? C31 C32 1.366(5) . ? C31 H31 0.9500 . ? C32 C33 1.382(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C42 1.402(4) . ? C34 C35 1.412(4) . ? C34 N1 1.422(4) . ? C35 C39 1.384(4) . ? C35 C36 1.515(5) . ? C36 C37 1.527(4) . ? C36 C38 1.532(5) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.365(5) . ? C39 H39 0.9500 . ? C40 C41 1.377(5) . ? C40 H40 0.9500 . ? C41 C42 1.401(4) . ? C41 H41 0.9500 . ? C42 C43 1.499(5) . ? C43 C44 1.507(5) . ? C43 C45 1.519(5) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C54 1.409(4) . ? C46 C47 1.410(4) . ? C46 N2 1.426(4) . ? C47 C51 1.392(5) . ? C47 C48 1.505(5) . ? C48 C49 1.531(4) . ? C48 C50 1.538(4) . ? C48 H48 1.0000 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.375(5) . ? C51 H51 0.9500 . ? C52 C53 1.370(5) . ? C52 H52 0.9500 . ? C53 C54 1.392(5) . ? C53 H53 0.9500 . ? C54 C55 1.521(4) . ? C55 C56 1.528(5) . ? C55 C57 1.529(5) . ? C55 H55 1.0000 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 N4 1.333(4) . ? C58 N3 1.340(4) . ? C58 C59 1.496(4) . ? C58 Y2 2.833(3) . ? C59 C64 1.391(5) . ? C59 C60 1.393(5) . ? C60 C61 1.377(5) . ? C60 H60 0.9500 . ? C61 C62 1.365(6) . ? C61 H61 0.9500 . ? C62 C63 1.367(6) . ? C62 H62 0.9500 . ? C63 C64 1.403(5) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 C73 1.407(4) . ? C65 C66 1.415(4) . ? C65 N3 1.426(4) . ? C66 C70 1.385(4) . ? C66 C67 1.526(5) . ? C67 C68 1.511(5) . ? C67 C69 1.519(5) . ? C67 H67 1.0000 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C71 1.366(5) . ? C70 H70 0.9500 . ? C71 C72 1.380(5) . ? C71 H71 0.9500 . ? C72 C73 1.392(4) . ? C72 H72 0.9500 . ? C73 C74 1.517(5) . ? C74 C75 1.523(5) . ? C74 C76 1.530(4) . ? C74 H74 1.0000 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C85 1.407(4) . ? C77 C78 1.407(4) . ? C77 N4 1.435(4) . ? C78 C82 1.397(4) . ? C78 C79 1.512(4) . ? C79 C81 1.522(4) . ? C79 C80 1.534(4) . ? C79 H79 1.0000 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C83 1.376(5) . ? C82 H82 0.9500 . ? C83 C84 1.374(5) . ? C83 H83 0.9500 . ? C84 C85 1.386(4) . ? C84 H84 0.9500 . ? C85 C86 1.523(4) . ? C86 C88 1.527(5) . ? C86 C87 1.534(5) . ? C86 H86 1.0000 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? N1 Y1 2.380(2) . ? N2 Y1 2.381(2) . ? N3 Y2 2.386(2) . ? N4 Y2 2.373(2) . ? O1 Y1 2.337(2) . ? O2 Y2 2.348(2) . ? Y1 Y2 3.3404(7) . ? Y1 H2 2.14(3) . ? Y1 H1 2.14(3) . ? Y2 H2 2.17(3) . ? Y2 H1 2.18(3) . ? 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 C4 C3 C13 122.3(3) . . ? C4 C3 Y2 75.06(17) . . ? C13 C3 Y2 119.5(2) . . ? C4 C3 H3 115(2) . . ? C13 C3 H3 116(2) . . ? Y2 C3 H3 99(2) . . ? C5 C4 C3 158.6(3) . . ? C5 C4 Y2 98.9(2) . . ? C3 C4 Y2 72.95(17) . . ? C5 C4 Y1 62.25(19) . . ? C3 C4 Y1 131.2(2) . . ? Y2 C4 Y1 75.75(8) . . ? C4 C5 C6 160.1(3) . . ? C4 C5 Y1 92.2(2) . . ? C6 C5 Y1 75.68(18) . . ? C4 C5 Y2 57.13(18) . . ? C6 C5 Y2 130.9(2) . . ? Y1 C5 Y2 73.46(8) . . ? C5 C6 C7 123.0(3) . . ? C5 C6 Y1 72.73(18) . . ? C7 C6 Y1 119.0(2) . . ? C5 C6 H6 113.7(19) . . ? C7 C6 H6 119(2) . . ? Y1 C6 H6 97(2) . . ? C12 C7 C8 116.6(3) . . ? C12 C7 C6 122.5(3) . . ? C8 C7 C6 121.0(3) . . ? C9 C8 C7 121.2(3) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C10 C9 C8 121.5(3) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 118.3(3) . . ? C9 C10 H10 120.9 . . ? C11 C10 H10 120.9 . . ? C10 C11 C12 121.1(3) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C7 121.3(3) . . ? C11 C12 H12 119.4 . . ? C7 C12 H12 119.4 . . ? C14 C13 C18 116.9(3) . . ? C14 C13 C3 122.6(3) . . ? C18 C13 C3 120.5(3) . . ? C15 C14 C13 121.1(3) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C16 C15 C14 120.6(3) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 C15 119.3(3) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 119.7(3) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C17 C18 C13 122.3(3) . . ? C17 C18 H18 118.9 . . ? C13 C18 H18 118.9 . . ? O1 C19 C20 105.3(3) . . ? O1 C19 H19A 110.7 . . ? C20 C19 H19A 110.7 . . ? O1 C19 H19B 110.7 . . ? C20 C19 H19B 110.7 . . ? H19A C19 H19B 108.8 . . ? C21 C20 C19 109.2(8) . . ? C21 C20 C21' 24.8(7) . . ? C19 C20 C21' 97.9(7) . . ? C21 C20 H20A 123.6 . . ? C19 C20 H20A 112.2 . . ? C21' C20 H20A 112.2 . . ? C21 C20 H20B 87.4 . . ? C19 C20 H20B 112.2 . . ? C21' C20 H20B 112.2 . . ? H20A C20 H20B 109.8 . . ? C20 C21 C22 107.2(12) . . ? C20 C21 H21A 110.3 . . ? C22 C21 H21A 110.3 . . ? C20 C21 H21B 110.3 . . ? C22 C21 H21B 110.3 . . ? H21A C21 H21B 108.5 . . ? C22 C21' C20 99.2(10) . . ? C22 C21' H21C 111.9 . . ? C20 C21' H21C 111.9 . . ? C22 C21' H21D 111.9 . . ? C20 C21' H21D 111.9 . . ? H21C C21' H21D 109.6 . . ? O1 C22 C21' 108.3(8) . . ? O1 C22 C21 107.5(8) . . ? C21' C22 C21 26.5(6) . . ? O1 C22 H22A 110.0 . . ? C21' C22 H22A 110.0 . . ? C21 C22 H22A 86.3 . . ? O1 C22 H22B 110.0 . . ? C21' C22 H22B 110.0 . . ? C21 C22 H22B 131.2 . . ? H22A C22 H22B 108.4 . . ? O2 C23 C24 104.7(3) . . ? O2 C23 H23A 110.8 . . ? C24 C23 H23A 110.8 . . ? O2 C23 H23B 110.8 . . ? C24 C23 H23B 110.8 . . ? H23A C23 H23B 108.9 . . ? C25 C24 C23 103.2(4) . . ? C25 C24 H24A 111.1 . . ? C23 C24 H24A 111.1 . . ? C25 C24 H24B 111.1 . . ? C23 C24 H24B 111.1 . . ? H24A C24 H24B 109.1 . . ? C24 C25 C26 102.6(3) . . ? C24 C25 H25A 111.2 . . ? C26 C25 H25A 111.2 . . ? C24 C25 H25B 111.2 . . ? C26 C25 H25B 111.2 . . ? H25A C25 H25B 109.2 . . ? O2 C26 C25 106.5(3) . . ? O2 C26 H26A 110.4 . . ? C25 C26 H26A 110.4 . . ? O2 C26 H26B 110.4 . . ? C25 C26 H26B 110.4 . . ? H26A C26 H26B 108.6 . . ? N2 C27 N1 114.6(3) . . ? N2 C27 C28 123.3(3) . . ? N1 C27 C28 122.0(3) . . ? N2 C27 Y1 57.35(15) . . ? N1 C27 Y1 57.33(15) . . ? C28 C27 Y1 173.2(2) . . ? C29 C28 C33 118.4(3) . . ? C29 C28 C27 122.8(3) . . ? C33 C28 C27 118.8(3) . . ? C30 C29 C28 119.9(3) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C31 C30 C29 120.7(3) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C32 C31 C30 119.9(3) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.5(3) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C32 C33 C28 120.5(3) . . ? C32 C33 H33 119.8 . . ? C28 C33 H33 119.8 . . ? C42 C34 C35 120.1(3) . . ? C42 C34 N1 119.5(3) . . ? C35 C34 N1 120.2(3) . . ? C39 C35 C34 118.2(3) . . ? C39 C35 C36 118.9(3) . . ? C34 C35 C36 122.7(3) . . ? C35 C36 C37 110.6(3) . . ? C35 C36 C38 113.2(3) . . ? C37 C36 C38 109.9(3) . . ? C35 C36 H36 107.6 . . ? C37 C36 H36 107.6 . . ? C38 C36 H36 107.6 . . ? 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 . . ? C40 C39 C35 122.2(3) . . ? C40 C39 H39 118.9 . . ? C35 C39 H39 118.9 . . ? C39 C40 C41 119.8(3) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C40 C41 C42 120.7(3) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C41 C42 C34 118.9(3) . . ? C41 C42 C43 119.1(3) . . ? C34 C42 C43 122.0(3) . . ? C42 C43 C44 111.5(3) . . ? C42 C43 C45 113.9(3) . . ? C44 C43 C45 109.4(3) . . ? C42 C43 H43 107.2 . . ? C44 C43 H43 107.2 . . ? C45 C43 H43 107.2 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C54 C46 C47 120.4(3) . . ? C54 C46 N2 117.7(3) . . ? C47 C46 N2 121.8(3) . . ? C51 C47 C46 118.0(3) . . ? C51 C47 C48 118.4(3) . . ? C46 C47 C48 123.6(3) . . ? C47 C48 C49 111.9(3) . . ? C47 C48 C50 113.2(3) . . ? C49 C48 C50 109.8(3) . . ? C47 C48 H48 107.2 . . ? C49 C48 H48 107.2 . . ? C50 C48 H48 107.2 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 C47 121.8(3) . . ? C52 C51 H51 119.1 . . ? C47 C51 H51 119.1 . . ? C53 C52 C51 119.8(3) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C52 C53 C54 121.4(3) . . ? C52 C53 H53 119.3 . . ? C54 C53 H53 119.3 . . ? C53 C54 C46 118.6(3) . . ? C53 C54 C55 119.2(3) . . ? C46 C54 C55 122.1(3) . . ? C54 C55 C56 112.7(3) . . ? C54 C55 C57 111.0(3) . . ? C56 C55 C57 109.5(3) . . ? C54 C55 H55 107.8 . . ? C56 C55 H55 107.8 . . ? C57 C55 H55 107.8 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N4 C58 N3 113.2(2) . . ? N4 C58 C59 124.3(3) . . ? N3 C58 C59 122.5(3) . . ? N4 C58 Y2 56.50(14) . . ? N3 C58 Y2 57.07(14) . . ? C59 C58 Y2 173.3(2) . . ? C64 C59 C60 118.6(3) . . ? C64 C59 C58 121.8(3) . . ? C60 C59 C58 119.6(3) . . ? C61 C60 C59 120.9(4) . . ? C61 C60 H60 119.6 . . ? C59 C60 H60 119.6 . . ? C62 C61 C60 120.2(4) . . ? C62 C61 H61 119.9 . . ? C60 C61 H61 119.9 . . ? C61 C62 C63 120.5(4) . . ? C61 C62 H62 119.7 . . ? C63 C62 H62 119.7 . . ? C62 C63 C64 120.2(4) . . ? C62 C63 H63 119.9 . . ? C64 C63 H63 119.9 . . ? C59 C64 C63 119.6(3) . . ? C59 C64 H64 120.2 . . ? C63 C64 H64 120.2 . . ? C73 C65 C66 120.1(3) . . ? C73 C65 N3 121.0(3) . . ? C66 C65 N3 118.7(3) . . ? C70 C66 C65 118.7(3) . . ? C70 C66 C67 119.6(3) . . ? C65 C66 C67 121.7(3) . . ? C68 C67 C69 110.5(3) . . ? C68 C67 C66 111.4(3) . . ? C69 C67 C66 112.6(3) . . ? C68 C67 H67 107.4 . . ? C69 C67 H67 107.4 . . ? C66 C67 H67 107.4 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C71 C70 C66 121.7(3) . . ? C71 C70 H70 119.2 . . ? C66 C70 H70 119.2 . . ? C70 C71 C72 119.5(3) . . ? C70 C71 H71 120.2 . . ? C72 C71 H71 120.2 . . ? C71 C72 C73 121.8(3) . . ? C71 C72 H72 119.1 . . ? C73 C72 H72 119.1 . . ? C72 C73 C65 118.1(3) . . ? C72 C73 C74 119.0(3) . . ? C65 C73 C74 122.8(3) . . ? C73 C74 C75 113.5(3) . . ? C73 C74 C76 110.2(3) . . ? C75 C74 C76 110.9(3) . . ? C73 C74 H74 107.3 . . ? C75 C74 H74 107.3 . . ? C76 C74 H74 107.3 . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C74 C76 H76A 109.5 . . ? C74 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C74 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C85 C77 C78 121.1(3) . . ? C85 C77 N4 117.1(3) . . ? C78 C77 N4 121.6(3) . . ? C82 C78 C77 117.3(3) . . ? C82 C78 C79 118.5(3) . . ? C77 C78 C79 124.2(3) . . ? C78 C79 C81 113.4(3) . . ? C78 C79 C80 111.5(3) . . ? C81 C79 C80 108.9(3) . . ? C78 C79 H79 107.6 . . ? C81 C79 H79 107.6 . . ? C80 C79 H79 107.6 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C83 C82 C78 122.3(3) . . ? C83 C82 H82 118.9 . . ? C78 C82 H82 118.9 . . ? C84 C83 C82 119.1(3) . . ? C84 C83 H83 120.4 . . ? C82 C83 H83 120.4 . . ? C83 C84 C85 121.8(3) . . ? C83 C84 H84 119.1 . . ? C85 C84 H84 119.1 . . ? C84 C85 C77 118.3(3) . . ? C84 C85 C86 118.9(3) . . ? C77 C85 C86 122.8(3) . . ? C85 C86 C88 113.3(3) . . ? C85 C86 C87 110.8(3) . . ? C88 C86 C87 109.5(3) . . ? C85 C86 H86 107.7 . . ? C88 C86 H86 107.7 . . ? C87 C86 H86 107.7 . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C86 C88 H88A 109.5 . . ? C86 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C86 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C27 N1 C34 121.6(2) . . ? C27 N1 Y1 94.49(17) . . ? C34 N1 Y1 141.81(18) . . ? C27 N2 C46 123.7(2) . . ? C27 N2 Y1 94.52(17) . . ? C46 N2 Y1 141.73(19) . . ? C58 N3 C65 122.0(2) . . ? C58 N3 Y2 94.81(17) . . ? C65 N3 Y2 142.30(18) . . ? C58 N4 C77 124.5(2) . . ? C58 N4 Y2 95.58(17) . . ? C77 N4 Y2 139.55(18) . . ? C22 O1 C19 107.1(3) . . ? C22 O1 Y1 120.3(2) . . ? C19 O1 Y1 131.30(19) . . ? C26 O2 C23 108.6(3) . . ? C26 O2 Y2 124.5(2) . . ? C23 O2 Y2 126.46(19) . . ? O1 Y1 N1 95.45(8) . . ? O1 Y1 N2 104.66(8) . . ? N1 Y1 N2 56.26(8) . . ? O1 Y1 C5 91.42(9) . . ? N1 Y1 C5 172.65(9) . . ? N2 Y1 C5 119.35(10) . . ? O1 Y1 C6 97.00(10) . . ? N1 Y1 C6 144.04(9) . . ? N2 Y1 C6 87.93(9) . . ? C5 Y1 C6 31.59(10) . . ? O1 Y1 C27 100.23(8) . . ? N1 Y1 C27 28.18(8) . . ? N2 Y1 C27 28.13(8) . . ? C5 Y1 C27 147.34(10) . . ? C6 Y1 C27 116.05(9) . . ? O1 Y1 C4 79.99(8) . . ? N1 Y1 C4 159.35(9) . . ? N2 Y1 C4 144.38(9) . . ? C5 Y1 C4 25.53(9) . . ? C6 Y1 C4 56.53(10) . . ? C27 Y1 C4 172.40(9) . . ? O1 Y1 Y2 114.37(5) . . ? N1 Y1 Y2 119.09(6) . . ? N2 Y1 Y2 140.92(6) . . ? C5 Y1 Y2 59.76(7) . . ? C6 Y1 Y2 85.65(7) . . ? C27 Y1 Y2 136.77(6) . . ? C4 Y1 Y2 47.96(6) . . ? O1 Y1 H2 91.7(8) . . ? N1 Y1 H2 91.9(8) . . ? N2 Y1 H2 144.8(8) . . ? C5 Y1 H2 90.5(8) . . ? C6 Y1 H2 121.2(8) . . ? C27 Y1 H2 119.2(8) . . ? C4 Y1 H2 68.3(8) . . ? Y2 Y1 H2 39.4(8) . . ? O1 Y1 H1 154.0(8) . . ? N1 Y1 H1 101.1(8) . . ? N2 Y1 H1 101.2(8) . . ? C5 Y1 H1 73.4(8) . . ? C6 Y1 H1 81.2(8) . . ? C27 Y1 H1 103.8(8) . . ? C4 Y1 H1 77.5(8) . . ? Y2 Y1 H1 39.7(8) . . ? H2 Y1 H1 68.0(11) . . ? O2 Y2 N4 107.33(8) . . ? O2 Y2 N3 96.80(8) . . ? N4 Y2 N3 55.94(8) . . ? O2 Y2 C3 94.44(9) . . ? N4 Y2 C3 88.39(9) . . ? N3 Y2 C3 144.32(9) . . ? O2 Y2 C4 88.91(9) . . ? N4 Y2 C4 120.04(9) . . ? N3 Y2 C4 173.82(9) . . ? C3 Y2 C4 31.99(10) . . ? O2 Y2 C58 101.83(8) . . ? N4 Y2 C58 27.93(8) . . ? N3 Y2 C58 28.12(8) . . ? C3 Y2 C58 116.27(9) . . ? C4 Y2 C58 147.95(10) . . ? O2 Y2 C5 77.09(8) . . ? N4 Y2 C5 143.36(8) . . ? N3 Y2 C5 160.66(9) . . ? C3 Y2 C5 55.00(9) . . ? C4 Y2 C5 23.94(9) . . ? C58 Y2 C5 170.74(8) . . ? O2 Y2 Y1 112.13(5) . . ? N4 Y2 Y1 140.08(6) . . ? N3 Y2 Y1 122.93(5) . . ? C3 Y2 Y1 82.93(7) . . ? C4 Y2 Y1 56.29(7) . . ? C58 Y2 Y1 139.66(6) . . ? C5 Y2 Y1 46.78(6) . . ? O2 Y2 H2 150.9(8) . . ? N4 Y2 H2 101.7(8) . . ? N3 Y2 H2 101.3(8) . . ? C3 Y2 H2 84.0(8) . . ? C4 Y2 H2 74.4(8) . . ? C58 Y2 H2 104.9(8) . . ? C5 Y2 H2 78.3(8) . . ? Y1 Y2 H2 38.8(8) . . ? O2 Y2 H1 88.2(7) . . ? N4 Y2 H1 150.7(8) . . ? N3 Y2 H1 98.4(8) . . ? C3 Y2 H1 115.7(8) . . ? C4 Y2 H1 84.1(8) . . ? C58 Y2 H1 125.9(8) . . ? C5 Y2 H1 63.4(8) . . ? Y1 Y2 H1 39.0(8) . . ? H2 Y2 H1 66.9(11) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.524 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.067 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.000 0.009 0.499 1274 260 ' ' 2 0.358 0.537 0.248 30 1 ' ' 3 0.642 0.463 0.752 30 1 ' ' _platon_squeeze_details ; Three disorder Benzene molecules per formual unit of [(PhNCN)YH(THF)]2(PhCHCCCHPh)were not modelled and the disordered density was taken into accountusing the SQUEEZE/PLATON procedure. (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194?01) as implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst. 2003, 36, 7?3. PLATON - a multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands). ; _vrf_PLAT366_II-140-02 ; PROBLEM: PLAT366_ALERT_2_B Short? C(sp?)-C(sp?) Bond C4 - C5 ... 1.24 Ang. RESPONSE: C4-C5 is the triple bond of the alkyne ligand. ;