#Electronic Supplementary Material for Dalton Transactions #This Journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Qi Shen' _publ_contact_author_email QSHEN@SUDA.EDU.CN _publ_section_title ; Migration of amide to imine group of lanthanide Schiff base complexes: Effect of amido group ; loop_ _publ_author_name 'Qi Shen' 'Fubin Han' 'Duwei Qin' 'Yingming Yao' 'Yong Zhang' # Attachment 'qinduwei-dalton.cif' data_complexl _database_code_depnum_ccdc_archive 'CCDC 723164' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H86 Li N6 O3 Y' _chemical_formula_sum 'C56 H86 Li N6 O3 Y' _chemical_formula_weight 987.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 10.236(2) _cell_length_b 24.703(6) _cell_length_c 21.836(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.411(4) _cell_angle_gamma 90.00 _cell_volume 5512(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10199 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 1.104 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.488 _exptl_absorpt_correction_T_max 0.876 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21146 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0957 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10219 _reflns_number_gt 7853 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+2.6152P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10219 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1068 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.1318 _refine_ls_wR_factor_gt 0.1219 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.13322(3) 0.228392(16) 0.420686(18) 0.02896(11) Uani 1 1 d . . . O1 O 0.0188(2) 0.16412(11) 0.45854(12) 0.0332(7) Uani 1 1 d . . . O2 O 0.0389(2) 0.30998(10) 0.43739(12) 0.0316(6) Uani 1 1 d . . . O3 O 0.2242(2) 0.22991(12) 0.52701(12) 0.0405(7) Uani 1 1 d . . . N1 N -0.0348(3) 0.22115(13) 0.33893(14) 0.0303(8) Uani 1 1 d . . . N2 N -0.1471(3) 0.29951(14) 0.31093(16) 0.0382(9) Uani 1 1 d . . . N3 N 0.1367(3) 0.16074(13) 0.32926(15) 0.0299(8) Uani 1 1 d . . . N4 N 0.2787(3) 0.29489(12) 0.38733(14) 0.0282(7) Uani 1 1 d . . . N5 N 0.3736(3) 0.21587(13) 0.41446(16) 0.0349(8) Uani 1 1 d . . . N6 N 0.1784(3) 0.37042(13) 0.33447(15) 0.0309(8) Uani 1 1 d . . . C1 C -0.0701(3) 0.12959(15) 0.43277(18) 0.0296(9) Uani 1 1 d . . . C2 C -0.1500(4) 0.09638(16) 0.46825(19) 0.0322(9) Uani 1 1 d . . . C3 C -0.2367(4) 0.06090(17) 0.4374(2) 0.0376(10) Uani 1 1 d . . . H3 H -0.2898 0.0392 0.4610 0.045 Uiso 1 1 calc R . . C4 C -0.2501(4) 0.05539(17) 0.3741(2) 0.0362(10) Uani 1 1 d . . . C5 C -0.1702(4) 0.08888(16) 0.3404(2) 0.0367(10) Uani 1 1 d . . . H5 H -0.1763 0.0865 0.2974 0.044 Uiso 1 1 calc R . . C6 C -0.0823(3) 0.12552(16) 0.36829(19) 0.0310(9) Uani 1 1 d . . . C7 C -0.0113(3) 0.16369(16) 0.32648(18) 0.0317(10) Uani 1 1 d . . . H7 H -0.0436 0.1562 0.2837 0.038 Uiso 1 1 calc R . . C8 C -0.1399(4) 0.24407(17) 0.3075(2) 0.0353(10) Uani 1 1 d . . . C9 C -0.2395(4) 0.21579(19) 0.2720(2) 0.0461(12) Uani 1 1 d . . . H9 H -0.2389 0.1777 0.2710 0.055 Uiso 1 1 calc R . . C10 C -0.3355(4) 0.2435(2) 0.2396(2) 0.0562(14) Uani 1 1 d . . . H10 H -0.3992 0.2245 0.2154 0.067 Uiso 1 1 calc R . . C11 C -0.3399(4) 0.2996(2) 0.2421(2) 0.0596(15) Uani 1 1 d . . . H11 H -0.4050 0.3193 0.2195 0.071 Uiso 1 1 calc R . . C12 C -0.2453(4) 0.3252(2) 0.2788(2) 0.0518(13) Uani 1 1 d . . . H12 H -0.2493 0.3632 0.2818 0.062 Uiso 1 1 calc R . . C13 C 0.1847(4) 0.19413(18) 0.27611(19) 0.0371(10) Uani 1 1 d . . . H13 H 0.1709 0.2323 0.2878 0.044 Uiso 1 1 calc R . . C14 C 0.3310(4) 0.1895(2) 0.2673(2) 0.0506(13) Uani 1 1 d . . . H14A H 0.3485 0.1557 0.2466 0.076 Uiso 1 1 calc R . . H14B H 0.3788 0.1901 0.3070 0.076 Uiso 1 1 calc R . . H14C H 0.3587 0.2196 0.2427 0.076 Uiso 1 1 calc R . . C15 C 0.1128(4) 0.1879(2) 0.2137(2) 0.0622(15) Uani 1 1 d . . . H15A H 0.1141 0.1501 0.2013 0.093 Uiso 1 1 calc R . . H15B H 0.1555 0.2097 0.1838 0.093 Uiso 1 1 calc R . . H15C H 0.0229 0.1997 0.2159 0.093 Uiso 1 1 calc R . . C16 C 0.1976(4) 0.10537(16) 0.3335(2) 0.0395(11) Uani 1 1 d . . . H16 H 0.2899 0.1109 0.3238 0.047 Uiso 1 1 calc R . . C17 C 0.2048(4) 0.08225(19) 0.3980(2) 0.0575(14) Uani 1 1 d . . . H17A H 0.2307 0.1105 0.4271 0.086 Uiso 1 1 calc R . . H17B H 0.2686 0.0532 0.4008 0.086 Uiso 1 1 calc R . . H17C H 0.1196 0.0683 0.4072 0.086 Uiso 1 1 calc R . . C18 C 0.1448(5) 0.06339(19) 0.2875(2) 0.0682(16) Uani 1 1 d . . . H18A H 0.0529 0.0570 0.2933 0.102 Uiso 1 1 calc R . . H18B H 0.1931 0.0298 0.2936 0.102 Uiso 1 1 calc R . . H18C H 0.1548 0.0766 0.2462 0.102 Uiso 1 1 calc R . . C19 C -0.1400(4) 0.09822(17) 0.5387(2) 0.0400(11) Uani 1 1 d . . . C20 C -0.2551(5) 0.0683(2) 0.5664(2) 0.0610(15) Uani 1 1 d . . . H20A H -0.3371 0.0847 0.5515 0.091 Uiso 1 1 calc R . . H20B H -0.2465 0.0710 0.6108 0.091 Uiso 1 1 calc R . . H20C H -0.2540 0.0305 0.5545 0.091 Uiso 1 1 calc R . . C21 C -0.1439(4) 0.15638(18) 0.56359(19) 0.0500(12) Uani 1 1 d . . . H21A H -0.0688 0.1763 0.5506 0.075 Uiso 1 1 calc R . . H21B H -0.1419 0.1555 0.6080 0.075 Uiso 1 1 calc R . . H21C H -0.2236 0.1740 0.5478 0.075 Uiso 1 1 calc R . . C22 C -0.0124(4) 0.07059(19) 0.5620(2) 0.0606(14) Uani 1 1 d . . . H22A H -0.0147 0.0328 0.5500 0.091 Uiso 1 1 calc R . . H22B H -0.0029 0.0733 0.6063 0.091 Uiso 1 1 calc R . . H22C H 0.0611 0.0883 0.5443 0.091 Uiso 1 1 calc R . . C23 C -0.3475(4) 0.01634(19) 0.3413(2) 0.0492(13) Uani 1 1 d . . . C24 C -0.4303(5) -0.0136(2) 0.3859(3) 0.089(2) Uani 1 1 d . . . H24A H -0.3737 -0.0340 0.4146 0.134 Uiso 1 1 calc R . . H24B H -0.4895 -0.0381 0.3633 0.134 Uiso 1 1 calc R . . H24C H -0.4805 0.0124 0.4082 0.134 Uiso 1 1 calc R . . C25 C -0.2754(5) -0.0254(2) 0.3045(3) 0.0657(16) Uani 1 1 d . . . H25A H -0.2221 -0.0070 0.2757 0.099 Uiso 1 1 calc R . . H25B H -0.3385 -0.0484 0.2822 0.099 Uiso 1 1 calc R . . H25C H -0.2198 -0.0473 0.3322 0.099 Uiso 1 1 calc R . . C26 C -0.4398(4) 0.0484(2) 0.2964(3) 0.0737(18) Uani 1 1 d . . . H26A H -0.4849 0.0760 0.3188 0.111 Uiso 1 1 calc R . . H26B H -0.5034 0.0240 0.2766 0.111 Uiso 1 1 calc R . . H26C H -0.3893 0.0655 0.2656 0.111 Uiso 1 1 calc R . . C27 C 0.1048(4) 0.34807(16) 0.47118(19) 0.0310(9) Uani 1 1 d . . . C28 C 0.0603(4) 0.36684(16) 0.52766(18) 0.0316(9) Uani 1 1 d . . . C29 C 0.1444(4) 0.39950(16) 0.56480(18) 0.0352(10) Uani 1 1 d . . . H29 H 0.1163 0.4112 0.6028 0.042 Uiso 1 1 calc R . . C30 C 0.2686(4) 0.41555(17) 0.54782(19) 0.0342(10) Uani 1 1 d . . . C31 C 0.3013(4) 0.40236(16) 0.48923(18) 0.0328(10) Uani 1 1 d . . . H31 H 0.3804 0.4155 0.4752 0.039 Uiso 1 1 calc R . . C32 C 0.2212(3) 0.37027(15) 0.44991(18) 0.0292(9) Uani 1 1 d . . . C33 C 0.2693(3) 0.35357(16) 0.38831(18) 0.0301(9) Uani 1 1 d . . . H33 H 0.3570 0.3694 0.3836 0.036 Uiso 1 1 calc R . . C34 C 0.3938(3) 0.26942(17) 0.40192(17) 0.0314(9) Uani 1 1 d . . . C35 C 0.5225(4) 0.29027(19) 0.4052(2) 0.0439(12) Uani 1 1 d . . . H35 H 0.5374 0.3275 0.3998 0.053 Uiso 1 1 calc R . . C36 C 0.6252(4) 0.2556(2) 0.4165(2) 0.0524(13) Uani 1 1 d . . . H36 H 0.7111 0.2692 0.4184 0.063 Uiso 1 1 calc R . . C37 C 0.6049(4) 0.2009(2) 0.4251(2) 0.0526(13) Uani 1 1 d . . . H37 H 0.6755 0.1768 0.4308 0.063 Uiso 1 1 calc R . . C38 C 0.4777(4) 0.18324(18) 0.4248(2) 0.0431(11) Uani 1 1 d . . . H38 H 0.4626 0.1464 0.4323 0.052 Uiso 1 1 calc R . . C39 C 0.2320(4) 0.35232(17) 0.27564(18) 0.0365(10) Uani 1 1 d . . . H39 H 0.2664 0.3153 0.2833 0.044 Uiso 1 1 calc R . . C40 C 0.1234(4) 0.34675(19) 0.22466(19) 0.0502(12) Uani 1 1 d . . . H40A H 0.0538 0.3242 0.2389 0.075 Uiso 1 1 calc R . . H40B H 0.1587 0.3302 0.1889 0.075 Uiso 1 1 calc R . . H40C H 0.0888 0.3823 0.2139 0.075 Uiso 1 1 calc R . . C41 C 0.3464(4) 0.38539(19) 0.2534(2) 0.0516(13) Uani 1 1 d . . . H41A H 0.3157 0.4211 0.2411 0.077 Uiso 1 1 calc R . . H41B H 0.3822 0.3673 0.2187 0.077 Uiso 1 1 calc R . . H41C H 0.4137 0.3887 0.2864 0.077 Uiso 1 1 calc R . . C42 C 0.1411(4) 0.42958(16) 0.3318(2) 0.0397(11) Uani 1 1 d . . . H42 H 0.1237 0.4380 0.2877 0.048 Uiso 1 1 calc R . . C43 C 0.0120(4) 0.44020(19) 0.3619(2) 0.0589(14) Uani 1 1 d . . . H43A H -0.0548 0.4158 0.3447 0.088 Uiso 1 1 calc R . . H43B H -0.0151 0.4773 0.3542 0.088 Uiso 1 1 calc R . . H43C H 0.0242 0.4342 0.4057 0.088 Uiso 1 1 calc R . . C44 C 0.2441(4) 0.47042(17) 0.3554(2) 0.0494(12) Uani 1 1 d . . . H44A H 0.2482 0.4709 0.3999 0.074 Uiso 1 1 calc R . . H44B H 0.2208 0.5062 0.3399 0.074 Uiso 1 1 calc R . . H44C H 0.3288 0.4602 0.3413 0.074 Uiso 1 1 calc R . . C45 C -0.0767(4) 0.35276(18) 0.5481(2) 0.0418(11) Uani 1 1 d . . . C46 C -0.1071(4) 0.3815(2) 0.6071(2) 0.0620(15) Uani 1 1 d . . . H46A H -0.0442 0.3706 0.6397 0.093 Uiso 1 1 calc R . . H46B H -0.1946 0.3718 0.6180 0.093 Uiso 1 1 calc R . . H46C H -0.1021 0.4203 0.6011 0.093 Uiso 1 1 calc R . . C47 C -0.0891(4) 0.29147(18) 0.5590(2) 0.0561(14) Uani 1 1 d . . . H47A H -0.0810 0.2724 0.5206 0.084 Uiso 1 1 calc R . . H47B H -0.1737 0.2837 0.5747 0.084 Uiso 1 1 calc R . . H47C H -0.0203 0.2798 0.5885 0.084 Uiso 1 1 calc R . . C48 C -0.1801(4) 0.3703(2) 0.4980(2) 0.0644(16) Uani 1 1 d . . . H48A H -0.1772 0.4093 0.4931 0.097 Uiso 1 1 calc R . . H48B H -0.2663 0.3597 0.5097 0.097 Uiso 1 1 calc R . . H48C H -0.1620 0.3531 0.4595 0.097 Uiso 1 1 calc R . . C49 C 0.3626(4) 0.44644(18) 0.5920(2) 0.0406(11) Uani 1 1 d . . . C50 C 0.5025(4) 0.4249(2) 0.5878(2) 0.0674(16) Uani 1 1 d . . . H50A H 0.5034 0.3861 0.5947 0.101 Uiso 1 1 calc R . . H50B H 0.5600 0.4425 0.6186 0.101 Uiso 1 1 calc R . . H50C H 0.5325 0.4326 0.5473 0.101 Uiso 1 1 calc R . . C51 C 0.3605(5) 0.5062(2) 0.5762(3) 0.085(2) Uani 1 1 d . . . H51A H 0.3835 0.5110 0.5341 0.127 Uiso 1 1 calc R . . H51B H 0.4231 0.5253 0.6035 0.127 Uiso 1 1 calc R . . H51C H 0.2735 0.5206 0.5810 0.127 Uiso 1 1 calc R . . C52 C 0.3297(5) 0.4409(3) 0.6583(2) 0.090(2) Uani 1 1 d . . . H52A H 0.2443 0.4566 0.6637 0.135 Uiso 1 1 calc R . . H52B H 0.3950 0.4597 0.6844 0.135 Uiso 1 1 calc R . . H52C H 0.3288 0.4029 0.6695 0.135 Uiso 1 1 calc R . . C53 C 0.3135(5) 0.26869(19) 0.5561(2) 0.0582(14) Uani 1 1 d . . . H53A H 0.2691 0.2901 0.5864 0.070 Uiso 1 1 calc R . . H53B H 0.3469 0.2933 0.5256 0.070 Uiso 1 1 calc R . . C54 C 0.4198(6) 0.2376(2) 0.5859(3) 0.102(3) Uani 1 1 d . . . H54A H 0.4447 0.2531 0.6262 0.122 Uiso 1 1 calc R . . H54B H 0.4964 0.2385 0.5610 0.122 Uiso 1 1 calc R . . C55 C 0.3741(5) 0.1818(2) 0.5925(3) 0.084(2) Uani 1 1 d . . . H55A H 0.3717 0.1720 0.6359 0.101 Uiso 1 1 calc R . . H55B H 0.4318 0.1564 0.5726 0.101 Uiso 1 1 calc R . . C56 C 0.2408(5) 0.1807(2) 0.5621(2) 0.0775(19) Uani 1 1 d . . . H56A H 0.2307 0.1491 0.5350 0.093 Uiso 1 1 calc R . . H56B H 0.1750 0.1785 0.5928 0.093 Uiso 1 1 calc R . . Li1 Li 0.0093(7) 0.3290(3) 0.3550(4) 0.0445(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0298(2) 0.0298(2) 0.0270(2) 0.0012(2) -0.00088(15) -0.00135(18) O1 0.0366(15) 0.0348(16) 0.0278(16) 0.0006(13) -0.0005(12) -0.0085(13) O2 0.0331(14) 0.0305(15) 0.0312(16) -0.0016(13) 0.0014(12) -0.0025(12) O3 0.0442(16) 0.0457(18) 0.0305(16) 0.0019(15) -0.0067(13) -0.0041(15) N1 0.0296(17) 0.033(2) 0.0285(19) 0.0002(16) -0.0010(14) 0.0013(15) N2 0.0351(19) 0.040(2) 0.039(2) 0.0075(18) -0.0032(16) 0.0020(16) N3 0.0264(16) 0.0335(19) 0.030(2) 0.0000(16) 0.0044(14) -0.0006(14) N4 0.0292(17) 0.0277(18) 0.0277(19) 0.0001(15) 0.0011(14) 0.0008(14) N5 0.0315(18) 0.034(2) 0.039(2) 0.0002(17) 0.0003(16) 0.0031(15) N6 0.0376(18) 0.0298(19) 0.0255(19) 0.0036(16) 0.0028(15) 0.0029(15) C1 0.030(2) 0.028(2) 0.031(2) 0.0022(19) 0.0033(18) 0.0027(17) C2 0.033(2) 0.030(2) 0.034(2) 0.002(2) 0.0050(18) 0.0001(18) C3 0.034(2) 0.035(2) 0.044(3) 0.005(2) 0.007(2) -0.0055(19) C4 0.031(2) 0.037(2) 0.040(3) -0.005(2) 0.004(2) -0.0044(19) C5 0.038(2) 0.041(3) 0.031(2) -0.005(2) -0.0009(19) -0.004(2) C6 0.030(2) 0.031(2) 0.032(2) -0.004(2) 0.0010(18) -0.0020(17) C7 0.030(2) 0.038(2) 0.027(2) 0.0018(19) -0.0011(17) -0.0050(18) C8 0.030(2) 0.042(3) 0.034(3) 0.004(2) 0.0048(19) -0.0008(19) C9 0.036(2) 0.053(3) 0.048(3) 0.005(2) -0.009(2) -0.001(2) C10 0.035(3) 0.075(4) 0.058(4) 0.003(3) -0.010(2) -0.003(3) C11 0.038(3) 0.078(4) 0.061(4) 0.013(3) -0.012(2) 0.010(3) C12 0.041(3) 0.054(3) 0.060(3) 0.020(3) -0.001(2) 0.011(2) C13 0.039(2) 0.040(3) 0.032(2) 0.000(2) 0.0040(19) 0.001(2) C14 0.040(2) 0.071(4) 0.041(3) -0.003(3) 0.009(2) -0.007(2) C15 0.048(3) 0.105(5) 0.034(3) 0.006(3) 0.004(2) -0.011(3) C16 0.039(2) 0.032(2) 0.048(3) -0.005(2) 0.007(2) 0.0050(19) C17 0.058(3) 0.047(3) 0.067(4) 0.014(3) 0.001(3) 0.015(2) C18 0.084(4) 0.046(3) 0.074(4) -0.024(3) -0.004(3) 0.011(3) C19 0.053(3) 0.036(3) 0.031(3) 0.008(2) 0.005(2) -0.007(2) C20 0.083(4) 0.062(4) 0.039(3) 0.009(3) 0.016(3) -0.020(3) C21 0.076(3) 0.047(3) 0.028(3) 0.002(2) 0.014(2) -0.008(3) C22 0.072(3) 0.057(3) 0.052(3) 0.010(3) -0.015(3) 0.004(3) C23 0.041(3) 0.052(3) 0.056(3) -0.009(3) 0.006(2) -0.016(2) C24 0.095(4) 0.101(5) 0.073(4) -0.021(4) 0.018(3) -0.071(4) C25 0.067(3) 0.049(3) 0.080(4) -0.021(3) -0.005(3) -0.012(3) C26 0.044(3) 0.080(4) 0.094(5) -0.023(4) -0.019(3) -0.008(3) C27 0.035(2) 0.027(2) 0.031(2) 0.0035(19) 0.0034(18) 0.0047(18) C28 0.038(2) 0.028(2) 0.029(2) 0.0013(19) 0.0032(18) 0.0019(18) C29 0.045(2) 0.037(2) 0.025(2) -0.005(2) 0.0082(19) 0.000(2) C30 0.040(2) 0.035(2) 0.027(2) -0.003(2) 0.0025(19) -0.0010(19) C31 0.034(2) 0.033(2) 0.031(2) 0.003(2) 0.0030(18) -0.0029(18) C32 0.035(2) 0.027(2) 0.026(2) 0.0009(18) 0.0048(18) 0.0038(17) C33 0.029(2) 0.031(2) 0.030(2) 0.0004(19) 0.0017(17) -0.0025(17) C34 0.033(2) 0.036(2) 0.025(2) -0.001(2) 0.0030(17) 0.0003(19) C35 0.034(2) 0.046(3) 0.052(3) 0.008(2) 0.001(2) -0.003(2) C36 0.031(2) 0.068(4) 0.058(3) 0.000(3) -0.001(2) 0.001(2) C37 0.036(3) 0.060(3) 0.061(4) 0.002(3) -0.003(2) 0.014(2) C38 0.047(3) 0.038(3) 0.043(3) 0.003(2) -0.001(2) 0.009(2) C39 0.049(2) 0.036(2) 0.024(2) 0.001(2) 0.0025(19) 0.003(2) C40 0.064(3) 0.060(3) 0.026(3) -0.002(2) -0.003(2) -0.003(3) C41 0.053(3) 0.066(3) 0.036(3) 0.006(3) 0.011(2) 0.002(3) C42 0.051(3) 0.032(2) 0.036(3) 0.005(2) 0.002(2) 0.005(2) C43 0.056(3) 0.046(3) 0.076(4) 0.008(3) 0.011(3) 0.015(2) C44 0.068(3) 0.032(3) 0.048(3) 0.003(2) 0.001(2) -0.003(2) C45 0.043(2) 0.036(3) 0.047(3) -0.004(2) 0.015(2) -0.001(2) C46 0.061(3) 0.068(4) 0.061(4) -0.015(3) 0.036(3) -0.010(3) C47 0.059(3) 0.048(3) 0.064(4) 0.001(3) 0.029(3) -0.007(2) C48 0.044(3) 0.075(4) 0.076(4) 0.006(3) 0.012(3) 0.006(3) C49 0.049(3) 0.044(3) 0.028(3) -0.009(2) -0.001(2) -0.004(2) C50 0.049(3) 0.089(4) 0.062(4) -0.015(3) -0.013(3) 0.000(3) C51 0.101(4) 0.043(3) 0.105(5) -0.011(3) -0.044(4) -0.005(3) C52 0.079(4) 0.150(6) 0.039(3) -0.021(4) -0.007(3) -0.029(4) C53 0.075(3) 0.050(3) 0.046(3) -0.007(3) -0.023(3) -0.014(3) C54 0.090(4) 0.080(5) 0.127(6) -0.002(4) -0.069(4) -0.009(4) C55 0.096(4) 0.067(4) 0.084(5) 0.020(4) -0.038(4) 0.008(4) C56 0.105(4) 0.061(4) 0.062(4) 0.032(3) -0.032(3) -0.026(3) Li1 0.046(4) 0.045(5) 0.041(5) 0.002(4) -0.001(4) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O1 2.166(3) . ? Y1 O2 2.274(3) . ? Y1 N4 2.362(3) . ? Y1 N1 2.411(3) . ? Y1 O3 2.450(3) . ? Y1 N5 2.492(3) . ? Y1 N3 2.605(3) . ? Y1 C34 2.905(4) . ? Y1 C7 2.935(4) . ? Y1 Li1 3.103(8) . ? O1 C1 1.346(4) . ? O2 C27 1.351(4) . ? O2 Li1 1.867(8) . ? O3 C56 1.442(5) . ? O3 C53 1.445(5) . ? N1 C8 1.364(5) . ? N1 C7 1.468(5) . ? N2 C12 1.350(5) . ? N2 C8 1.374(5) . ? N2 Li1 1.958(8) . ? N3 C16 1.504(5) . ? N3 C7 1.515(4) . ? N3 C13 1.528(5) . ? N4 C34 1.357(4) . ? N4 C33 1.453(5) . ? N5 C38 1.344(5) . ? N5 C34 1.369(5) . ? N6 C39 1.495(5) . ? N6 C42 1.511(5) . ? N6 C33 1.513(5) . ? N6 Li1 2.083(8) . ? C1 C6 1.410(5) . ? C1 C2 1.421(5) . ? C2 C3 1.393(5) . ? C2 C19 1.536(5) . ? C3 C4 1.388(5) . ? C3 H3 0.9400 . ? C4 C5 1.402(5) . ? C4 C23 1.533(5) . ? C5 C6 1.391(5) . ? C5 H5 0.9400 . ? C6 C7 1.526(5) . ? C7 H7 0.9900 . ? C8 C9 1.426(5) . ? C8 Li1 2.760(9) . ? C9 C10 1.361(6) . ? C9 H9 0.9400 . ? C10 C11 1.388(7) . ? C10 H10 0.9400 . ? C11 C12 1.374(6) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 C15 1.518(5) . ? C13 C14 1.526(5) . ? C13 H13 0.9900 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C17 1.516(6) . ? C16 C18 1.521(6) . ? C16 H16 0.9900 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C22 1.534(6) . ? C19 C21 1.538(6) . ? C19 C20 1.545(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 C24 1.520(6) . ? C23 C25 1.524(6) . ? C23 C26 1.540(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 C32 1.415(5) . ? C27 C28 1.418(5) . ? C27 Li1 2.706(9) . ? C28 C29 1.403(5) . ? C28 C45 1.537(5) . ? C29 C30 1.402(5) . ? C29 H29 0.9400 . ? C30 C31 1.381(5) . ? C30 C49 1.526(5) . ? C31 C32 1.398(5) . ? C31 H31 0.9400 . ? C32 C33 1.517(5) . ? C33 Li1 2.784(8) . ? C33 H33 0.9900 . ? C34 C35 1.413(5) . ? C35 C36 1.367(6) . ? C35 H35 0.9400 . ? C36 C37 1.380(6) . ? C36 H36 0.9400 . ? C37 C38 1.373(6) . ? C37 H37 0.9400 . ? C38 H38 0.9400 . ? C39 C41 1.530(5) . ? C39 C40 1.532(5) . ? C39 H39 0.9900 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 C44 1.527(5) . ? C42 C43 1.533(5) . ? C42 H42 0.9900 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? C45 C46 1.518(6) . ? C45 C47 1.539(6) . ? C45 C48 1.539(6) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C46 H46C 0.9700 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C49 C52 1.513(6) . ? C49 C51 1.516(6) . ? C49 C50 1.535(6) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C50 H50C 0.9700 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 H51C 0.9700 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 H52C 0.9700 . ? C53 C54 1.453(6) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.467(7) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.482(6) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Y1 O2 110.12(10) . . ? O1 Y1 N4 173.21(10) . . ? O2 Y1 N4 73.42(10) . . ? O1 Y1 N1 81.36(10) . . ? O2 Y1 N1 83.88(10) . . ? N4 Y1 N1 104.98(11) . . ? O1 Y1 O3 80.41(10) . . ? O2 Y1 O3 88.60(9) . . ? N4 Y1 O3 94.04(10) . . ? N1 Y1 O3 156.51(10) . . ? O1 Y1 N5 119.22(10) . . ? O2 Y1 N5 123.30(10) . . ? N4 Y1 N5 55.00(10) . . ? N1 Y1 N5 127.86(11) . . ? O3 Y1 N5 74.49(10) . . ? O1 Y1 N3 81.64(10) . . ? O2 Y1 N3 135.79(9) . . ? N4 Y1 N3 99.91(10) . . ? N1 Y1 N3 55.03(10) . . ? O3 Y1 N3 135.58(10) . . ? N5 Y1 N3 79.62(10) . . ? O1 Y1 C34 146.25(10) . . ? O2 Y1 C34 96.64(10) . . ? N4 Y1 C34 27.45(10) . . ? N1 Y1 C34 122.83(11) . . ? O3 Y1 C34 80.08(10) . . ? N5 Y1 C34 28.07(10) . . ? N3 Y1 C34 93.50(10) . . ? O1 Y1 C7 66.84(10) . . ? O2 Y1 C7 113.20(10) . . ? N4 Y1 C7 117.62(11) . . ? N1 Y1 C7 29.87(10) . . ? O3 Y1 C7 145.08(10) . . ? N5 Y1 C7 110.64(10) . . ? N3 Y1 C7 31.02(9) . . ? C34 Y1 C7 121.33(11) . . ? O1 Y1 Li1 123.23(15) . . ? O2 Y1 Li1 36.72(16) . . ? N4 Y1 Li1 63.14(15) . . ? N1 Y1 Li1 57.52(16) . . ? O3 Y1 Li1 123.23(16) . . ? N5 Y1 Li1 116.87(15) . . ? N3 Y1 Li1 100.56(16) . . ? C34 Y1 Li1 90.51(15) . . ? C7 Y1 Li1 86.38(16) . . ? C1 O1 Y1 132.3(2) . . ? C27 O2 Li1 113.5(3) . . ? C27 O2 Y1 120.1(2) . . ? Li1 O2 Y1 96.6(3) . . ? C56 O3 C53 105.9(3) . . ? C56 O3 Y1 121.1(3) . . ? C53 O3 Y1 128.5(3) . . ? C8 N1 C7 116.2(3) . . ? C8 N1 Y1 148.0(3) . . ? C7 N1 Y1 95.2(2) . . ? C12 N2 C8 118.8(4) . . ? C12 N2 Li1 129.9(4) . . ? C8 N2 Li1 110.7(3) . . ? C16 N3 C7 117.1(3) . . ? C16 N3 C13 112.8(3) . . ? C7 N3 C13 108.0(3) . . ? C16 N3 Y1 124.1(2) . . ? C7 N3 Y1 86.6(2) . . ? C13 N3 Y1 104.8(2) . . ? C34 N4 C33 121.1(3) . . ? C34 N4 Y1 99.2(2) . . ? C33 N4 Y1 130.2(2) . . ? C38 N5 C34 119.1(3) . . ? C38 N5 Y1 147.2(3) . . ? C34 N5 Y1 93.0(2) . . ? C39 N6 C42 111.2(3) . . ? C39 N6 C33 110.2(3) . . ? C42 N6 C33 116.0(3) . . ? C39 N6 Li1 112.9(3) . . ? C42 N6 Li1 105.8(3) . . ? C33 N6 Li1 100.3(3) . . ? O1 C1 C6 118.7(3) . . ? O1 C1 C2 122.3(4) . . ? C6 C1 C2 119.0(4) . . ? C3 C2 C1 118.1(4) . . ? C3 C2 C19 120.4(4) . . ? C1 C2 C19 121.5(4) . . ? C4 C3 C2 124.5(4) . . ? C4 C3 H3 117.8 . . ? C2 C3 H3 117.8 . . ? C3 C4 C5 116.0(4) . . ? C3 C4 C23 123.3(4) . . ? C5 C4 C23 120.7(4) . . ? C6 C5 C4 122.5(4) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 C1 120.0(4) . . ? C5 C6 C7 117.3(4) . . ? C1 C6 C7 122.5(3) . . ? N1 C7 N3 102.3(3) . . ? N1 C7 C6 113.4(3) . . ? N3 C7 C6 117.2(3) . . ? N1 C7 Y1 54.89(17) . . ? N3 C7 Y1 62.40(18) . . ? C6 C7 Y1 98.9(2) . . ? N1 C7 H7 107.8 . . ? N3 C7 H7 107.8 . . ? C6 C7 H7 107.8 . . ? Y1 C7 H7 152.8 . . ? N1 C8 N2 115.4(4) . . ? N1 C8 C9 125.9(4) . . ? N2 C8 C9 118.6(4) . . ? N1 C8 Li1 74.0(3) . . ? N2 C8 Li1 41.6(2) . . ? C9 C8 Li1 159.7(3) . . ? C10 C9 C8 120.4(4) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.4(5) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 117.3(4) . . ? C12 C11 H11 121.3 . . ? C10 C11 H11 121.3 . . ? N2 C12 C11 124.3(5) . . ? N2 C12 H12 117.9 . . ? C11 C12 H12 117.9 . . ? C15 C13 C14 107.8(4) . . ? C15 C13 N3 117.8(3) . . ? C14 C13 N3 114.6(3) . . ? C15 C13 H13 105.1 . . ? C14 C13 H13 105.1 . . ? N3 C13 H13 105.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C17 113.4(4) . . ? N3 C16 C18 116.7(4) . . ? C17 C16 C18 110.6(4) . . ? N3 C16 H16 104.9 . . ? C17 C16 H16 104.9 . . ? C18 C16 H16 104.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22 C19 C2 108.9(4) . . ? C22 C19 C21 109.8(4) . . ? C2 C19 C21 112.4(3) . . ? C22 C19 C20 108.1(4) . . ? C2 C19 C20 111.8(3) . . ? C21 C19 C20 105.7(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C25 108.4(4) . . ? C24 C23 C4 112.3(4) . . ? C25 C23 C4 110.5(3) . . ? C24 C23 C26 108.2(4) . . ? C25 C23 C26 108.1(4) . . ? C4 C23 C26 109.3(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O2 C27 C32 119.6(4) . . ? O2 C27 C28 121.8(3) . . ? C32 C27 C28 118.6(4) . . ? O2 C27 Li1 39.3(2) . . ? C32 C27 Li1 91.4(3) . . ? C28 C27 Li1 139.1(3) . . ? C29 C28 C27 118.2(3) . . ? C29 C28 C45 120.1(4) . . ? C27 C28 C45 121.7(4) . . ? C30 C29 C28 123.0(4) . . ? C30 C29 H29 118.5 . . ? C28 C29 H29 118.5 . . ? C31 C30 C29 116.9(4) . . ? C31 C30 C49 121.7(4) . . ? C29 C30 C49 121.5(4) . . ? C30 C31 C32 122.5(4) . . ? C30 C31 H31 118.7 . . ? C32 C31 H31 118.7 . . ? C31 C32 C27 119.5(4) . . ? C31 C32 C33 119.3(3) . . ? C27 C32 C33 120.6(3) . . ? N4 C33 N6 107.5(3) . . ? N4 C33 C32 108.0(3) . . ? N6 C33 C32 113.4(3) . . ? N4 C33 Li1 80.9(2) . . ? N6 C33 Li1 47.4(2) . . ? C32 C33 Li1 86.3(3) . . ? N4 C33 H33 109.3 . . ? N6 C33 H33 109.3 . . ? C32 C33 H33 109.3 . . ? Li1 C33 H33 156.6 . . ? N4 C34 N5 110.9(3) . . ? N4 C34 C35 129.6(4) . . ? N5 C34 C35 119.6(4) . . ? N4 C34 Y1 53.36(18) . . ? N5 C34 Y1 58.94(18) . . ? C35 C34 Y1 168.9(3) . . ? C36 C35 C34 119.1(4) . . ? C36 C35 H35 120.5 . . ? C34 C35 H35 120.5 . . ? C35 C36 C37 121.1(4) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? C38 C37 C36 117.5(4) . . ? C38 C37 H37 121.3 . . ? C36 C37 H37 121.3 . . ? N5 C38 C37 123.5(4) . . ? N5 C38 H38 118.3 . . ? C37 C38 H38 118.3 . . ? N6 C39 C41 116.1(3) . . ? N6 C39 C40 111.3(3) . . ? C41 C39 C40 110.7(4) . . ? N6 C39 H39 106.0 . . ? C41 C39 H39 106.0 . . ? C40 C39 H39 106.0 . . ? 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 . . ? N6 C42 C44 117.2(3) . . ? N6 C42 C43 111.8(3) . . ? C44 C42 C43 109.8(4) . . ? N6 C42 H42 105.7 . . ? C44 C42 H42 105.7 . . ? C43 C42 H42 105.7 . . ? 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 C28 112.2(4) . . ? C46 C45 C47 107.8(4) . . ? C28 C45 C47 110.6(3) . . ? C46 C45 C48 107.7(4) . . ? C28 C45 C48 109.3(4) . . ? C47 C45 C48 109.2(4) . . ? 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 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C52 C49 C51 107.7(5) . . ? C52 C49 C30 113.1(4) . . ? C51 C49 C30 110.1(4) . . ? C52 C49 C50 106.7(4) . . ? C51 C49 C50 108.9(4) . . ? C30 C49 C50 110.2(4) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O3 C53 C54 106.5(4) . . ? O3 C53 H53A 110.4 . . ? C54 C53 H53A 110.4 . . ? O3 C53 H53B 110.4 . . ? C54 C53 H53B 110.4 . . ? H53A C53 H53B 108.6 . . ? C53 C54 C55 107.8(4) . . ? C53 C54 H54A 110.1 . . ? C55 C54 H54A 110.1 . . ? C53 C54 H54B 110.1 . . ? C55 C54 H54B 110.1 . . ? H54A C54 H54B 108.5 . . ? C54 C55 C56 105.2(4) . . ? C54 C55 H55A 110.7 . . ? C56 C55 H55A 110.7 . . ? C54 C55 H55B 110.7 . . ? C56 C55 H55B 110.7 . . ? H55A C55 H55B 108.8 . . ? O3 C56 C55 107.4(4) . . ? O3 C56 H56A 110.2 . . ? C55 C56 H56A 110.2 . . ? O3 C56 H56B 110.2 . . ? C55 C56 H56B 110.2 . . ? H56A C56 H56B 108.5 . . ? O2 Li1 N2 117.4(4) . . ? O2 Li1 N6 104.0(3) . . ? N2 Li1 N6 138.0(4) . . ? O2 Li1 C27 27.26(16) . . ? N2 Li1 C27 139.8(4) . . ? N6 Li1 C27 81.8(3) . . ? O2 Li1 C8 103.0(3) . . ? N2 Li1 C8 27.75(16) . . ? N6 Li1 C8 137.8(4) . . ? C27 Li1 C8 130.2(3) . . ? O2 Li1 C33 72.8(2) . . ? N2 Li1 C33 161.9(4) . . ? N6 Li1 C33 32.33(15) . . ? C27 Li1 C33 55.28(18) . . ? C8 Li1 C33 139.7(3) . . ? O2 Li1 Y1 46.71(19) . . ? N2 Li1 Y1 103.2(3) . . ? N6 Li1 Y1 99.8(3) . . ? C27 Li1 Y1 65.84(18) . . ? C8 Li1 Y1 76.5(2) . . ? C33 Li1 Y1 72.27(18) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.262 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.059 #===================================================end data_complex2 _database_code_depnum_ccdc_archive 'CCDC 723165' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H86 Li N6 O3 Sm' _chemical_formula_sum 'C56 H86 Li N6 O3 Sm' _chemical_formula_weight 1048.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 10.3390(14) _cell_length_b 24.566(3) _cell_length_c 21.831(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.388(2) _cell_angle_gamma 90.00 _cell_volume 5535.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 17477 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2212 _exptl_absorpt_coefficient_mu 1.107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.638 _exptl_absorpt_correction_T_max 0.866 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43498 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12576 _reflns_number_gt 11512 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0834P)^2^+13.5308P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12576 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.1752 _refine_ls_wR_factor_gt 0.1688 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 Sm1 Sm 0.13520(2) 0.229566(10) 0.423787(11) 0.02694(10) Uani 1 1 d . . . O1 O 0.0155(4) 0.16375(14) 0.45999(16) 0.0320(8) Uani 1 1 d . . . O2 O 0.0407(3) 0.31439(14) 0.43901(16) 0.0327(8) Uani 1 1 d . . . O3 O 0.2281(4) 0.23021(17) 0.53297(19) 0.0442(10) Uani 1 1 d . . . N1 N -0.0382(4) 0.22252(17) 0.34071(19) 0.0296(9) Uani 1 1 d . . . N2 N -0.1452(4) 0.3017(2) 0.3137(2) 0.0401(11) Uani 1 1 d . . . N3 N 0.1294(4) 0.16037(17) 0.3300(2) 0.0304(9) Uani 1 1 d . . . N4 N 0.2812(4) 0.29832(16) 0.38913(18) 0.0272(8) Uani 1 1 d . . . N5 N 0.3811(5) 0.21983(18) 0.4166(2) 0.0348(10) Uani 1 1 d . . . N6 N 0.1779(4) 0.37342(17) 0.33654(18) 0.0298(9) Uani 1 1 d . . . C1 C -0.0738(5) 0.1299(2) 0.4351(2) 0.0295(10) Uani 1 1 d . . . C2 C -0.1532(5) 0.0969(2) 0.4704(2) 0.0325(11) Uani 1 1 d . . . C3 C -0.2409(5) 0.0618(2) 0.4395(3) 0.0365(12) Uani 1 1 d . . . H3 H -0.2934 0.0400 0.4632 0.044 Uiso 1 1 calc R . . C4 C -0.2558(5) 0.0569(2) 0.3760(3) 0.0391(12) Uani 1 1 d . . . C5 C -0.1774(5) 0.0902(2) 0.3425(2) 0.0360(12) Uani 1 1 d . . . H5 H -0.1849 0.0883 0.2995 0.043 Uiso 1 1 calc R . . C6 C -0.0876(5) 0.1263(2) 0.3705(2) 0.0281(10) Uani 1 1 d . . . C7 C -0.0162(5) 0.1641(2) 0.3282(2) 0.0301(10) Uani 1 1 d . . . H7 H -0.0493 0.1566 0.2855 0.036 Uiso 1 1 calc R . . C8 C -0.1411(5) 0.2457(2) 0.3105(2) 0.0320(11) Uani 1 1 d . . . C9 C -0.2426(6) 0.2183(3) 0.2765(3) 0.0462(14) Uani 1 1 d . . . H9 H -0.2441 0.1801 0.2757 0.055 Uiso 1 1 calc R . . C10 C -0.3383(6) 0.2471(3) 0.2450(3) 0.0577(18) Uani 1 1 d . . . H10 H -0.4037 0.2285 0.2218 0.069 Uiso 1 1 calc R . . C11 C -0.3397(7) 0.3036(3) 0.2471(4) 0.063(2) Uani 1 1 d . . . H11 H -0.4038 0.3240 0.2250 0.075 Uiso 1 1 calc R . . C12 C -0.2436(6) 0.3281(3) 0.2826(3) 0.0516(16) Uani 1 1 d . . . H12 H -0.2458 0.3662 0.2858 0.062 Uiso 1 1 calc R . . C13 C 0.1769(6) 0.1923(2) 0.2764(3) 0.0415(13) Uani 1 1 d . . . H13 H 0.1541 0.2306 0.2846 0.050 Uiso 1 1 calc R . . C14 C 0.3216(6) 0.1923(3) 0.2710(3) 0.0556(18) Uani 1 1 d . . . H14A H 0.3644 0.2012 0.3104 0.083 Uiso 1 1 calc R . . H14B H 0.3442 0.2191 0.2408 0.083 Uiso 1 1 calc R . . H14C H 0.3493 0.1565 0.2583 0.083 Uiso 1 1 calc R . . C15 C 0.1133(7) 0.1797(5) 0.2146(3) 0.092(4) Uani 1 1 d . . . H15A H 0.1506 0.2024 0.1839 0.138 Uiso 1 1 calc R . . H15B H 0.0211 0.1869 0.2150 0.138 Uiso 1 1 calc R . . H15C H 0.1269 0.1417 0.2049 0.138 Uiso 1 1 calc R . . C16 C 0.1881(6) 0.1048(2) 0.3357(3) 0.0442(14) Uani 1 1 d . . . H16 H 0.2763 0.1096 0.3212 0.053 Uiso 1 1 calc R . . C17 C 0.2111(8) 0.0858(3) 0.3998(4) 0.065(2) Uani 1 1 d . . . H17A H 0.2467 0.1154 0.4249 0.097 Uiso 1 1 calc R . . H17B H 0.2718 0.0557 0.4011 0.097 Uiso 1 1 calc R . . H17C H 0.1299 0.0740 0.4155 0.097 Uiso 1 1 calc R . . C18 C 0.1289(8) 0.0601(3) 0.2941(4) 0.072(2) Uani 1 1 d . . . H18A H 0.0455 0.0494 0.3084 0.108 Uiso 1 1 calc R . . H18B H 0.1862 0.0288 0.2950 0.108 Uiso 1 1 calc R . . H18C H 0.1174 0.0736 0.2524 0.108 Uiso 1 1 calc R . . C19 C -0.1418(6) 0.0981(2) 0.5410(3) 0.0417(13) Uani 1 1 d . . . C20 C -0.2527(8) 0.0673(3) 0.5686(3) 0.062(2) Uani 1 1 d . . . H20A H -0.3344 0.0842 0.5554 0.093 Uiso 1 1 calc R . . H20B H -0.2417 0.0685 0.6130 0.093 Uiso 1 1 calc R . . H20C H -0.2524 0.0298 0.5549 0.093 Uiso 1 1 calc R . . C21 C -0.1461(7) 0.1560(3) 0.5658(3) 0.0531(17) Uani 1 1 d . . . H21A H -0.0751 0.1769 0.5506 0.080 Uiso 1 1 calc R . . H21B H -0.1383 0.1552 0.6103 0.080 Uiso 1 1 calc R . . H21C H -0.2278 0.1728 0.5523 0.080 Uiso 1 1 calc R . . C22 C -0.0140(7) 0.0707(3) 0.5630(3) 0.0589(18) Uani 1 1 d . . . H22A H -0.0174 0.0323 0.5525 0.088 Uiso 1 1 calc R . . H22B H -0.0009 0.0747 0.6071 0.088 Uiso 1 1 calc R . . H22C H 0.0572 0.0878 0.5432 0.088 Uiso 1 1 calc R . . C23 C -0.3535(6) 0.0182(2) 0.3434(3) 0.0449(14) Uani 1 1 d . . . C24 C -0.4375(9) -0.0105(4) 0.3879(4) 0.084(3) Uani 1 1 d . . . H24A H -0.3831 -0.0311 0.4172 0.126 Uiso 1 1 calc R . . H24B H -0.4968 -0.0349 0.3654 0.126 Uiso 1 1 calc R . . H24C H -0.4865 0.0163 0.4095 0.126 Uiso 1 1 calc R . . C25 C -0.2813(8) -0.0247(3) 0.3081(4) 0.065(2) Uani 1 1 d . . . H25A H -0.2281 -0.0467 0.3367 0.098 Uiso 1 1 calc R . . H25B H -0.2265 -0.0069 0.2796 0.098 Uiso 1 1 calc R . . H25C H -0.3433 -0.0479 0.2855 0.098 Uiso 1 1 calc R . . C26 C -0.4422(8) 0.0505(3) 0.2977(4) 0.075(2) Uani 1 1 d . . . H26A H -0.5091 0.0267 0.2798 0.112 Uiso 1 1 calc R . . H26B H -0.3914 0.0650 0.2654 0.112 Uiso 1 1 calc R . . H26C H -0.4819 0.0803 0.3189 0.112 Uiso 1 1 calc R . . C27 C 0.1081(5) 0.35115(19) 0.4733(2) 0.0290(10) Uani 1 1 d . . . C28 C 0.0653(6) 0.3692(2) 0.5309(2) 0.0353(11) Uani 1 1 d . . . C29 C 0.1504(5) 0.4012(2) 0.5677(2) 0.0339(11) Uani 1 1 d . . . H29 H 0.1248 0.4116 0.6066 0.041 Uiso 1 1 calc R . . C30 C 0.2698(6) 0.4185(2) 0.5502(2) 0.0361(12) Uani 1 1 d . . . C31 C 0.3018(5) 0.4060(2) 0.4906(2) 0.0336(11) Uani 1 1 d . . . H31 H 0.3794 0.4196 0.4763 0.040 Uiso 1 1 calc R . . C32 C 0.2225(5) 0.37416(18) 0.4520(2) 0.0264(10) Uani 1 1 d . . . C33 C 0.2685(5) 0.35734(19) 0.3898(2) 0.0259(9) Uani 1 1 d . . . H33 H 0.3544 0.3738 0.3844 0.031 Uiso 1 1 calc R . . C34 C 0.3958(5) 0.2746(2) 0.4047(2) 0.0309(10) Uani 1 1 d . . . C35 C 0.5213(5) 0.2974(2) 0.4101(3) 0.0410(13) Uani 1 1 d . . . H35 H 0.5330 0.3352 0.4064 0.049 Uiso 1 1 calc R . . C36 C 0.6263(6) 0.2635(3) 0.4208(3) 0.0524(17) Uani 1 1 d . . . H36 H 0.7103 0.2783 0.4225 0.063 Uiso 1 1 calc R . . C37 C 0.6102(6) 0.2084(3) 0.4291(3) 0.0554(17) Uani 1 1 d . . . H37 H 0.6819 0.1851 0.4356 0.066 Uiso 1 1 calc R . . C38 C 0.4858(6) 0.1888(3) 0.4276(3) 0.0461(14) Uani 1 1 d . . . H38 H 0.4736 0.1514 0.4347 0.055 Uiso 1 1 calc R . . C39 C 0.2292(6) 0.3538(2) 0.2773(2) 0.0385(12) Uani 1 1 d . . . H39 H 0.2622 0.3165 0.2857 0.046 Uiso 1 1 calc R . . C40 C 0.1218(7) 0.3478(3) 0.2271(3) 0.0511(16) Uani 1 1 d . . . H40A H 0.0522 0.3260 0.2422 0.077 Uiso 1 1 calc R . . H40B H 0.1558 0.3301 0.1918 0.077 Uiso 1 1 calc R . . H40C H 0.0888 0.3835 0.2154 0.077 Uiso 1 1 calc R . . C41 C 0.3437(6) 0.3859(3) 0.2544(3) 0.0491(15) Uani 1 1 d . . . H41A H 0.3158 0.4226 0.2436 0.074 Uiso 1 1 calc R . . H41B H 0.3751 0.3681 0.2185 0.074 Uiso 1 1 calc R . . H41C H 0.4126 0.3875 0.2865 0.074 Uiso 1 1 calc R . . C42 C 0.1401(6) 0.4323(2) 0.3325(2) 0.0363(12) Uani 1 1 d . . . H42 H 0.1221 0.4399 0.2883 0.044 Uiso 1 1 calc R . . C43 C 0.0135(7) 0.4432(3) 0.3629(3) 0.0532(16) Uani 1 1 d . . . H43A H -0.0533 0.4190 0.3456 0.080 Uiso 1 1 calc R . . H43B H -0.0125 0.4807 0.3558 0.080 Uiso 1 1 calc R . . H43C H 0.0259 0.4367 0.4067 0.080 Uiso 1 1 calc R . . C44 C 0.2430(6) 0.4734(2) 0.3549(3) 0.0476(15) Uani 1 1 d . . . H44A H 0.2501 0.4736 0.3994 0.071 Uiso 1 1 calc R . . H44B H 0.2185 0.5094 0.3400 0.071 Uiso 1 1 calc R . . H44C H 0.3258 0.4634 0.3394 0.071 Uiso 1 1 calc R . . C45 C -0.0684(6) 0.3538(2) 0.5523(3) 0.0408(13) Uani 1 1 d . . . C46 C -0.0955(8) 0.3791(3) 0.6146(3) 0.065(2) Uani 1 1 d . . . H46A H -0.0327 0.3657 0.6458 0.098 Uiso 1 1 calc R . . H46B H -0.1821 0.3693 0.6254 0.098 Uiso 1 1 calc R . . H46C H -0.0887 0.4184 0.6120 0.098 Uiso 1 1 calc R . . C47 C -0.0837(7) 0.2919(3) 0.5594(3) 0.0533(17) Uani 1 1 d . . . H47A H -0.0793 0.2745 0.5197 0.080 Uiso 1 1 calc R . . H47B H -0.1669 0.2840 0.5759 0.080 Uiso 1 1 calc R . . H47C H -0.0148 0.2781 0.5872 0.080 Uiso 1 1 calc R . . C48 C -0.1712(6) 0.3754(3) 0.5052(4) 0.0589(18) Uani 1 1 d . . . H48A H -0.1657 0.4148 0.5035 0.088 Uiso 1 1 calc R . . H48B H -0.2565 0.3649 0.5171 0.088 Uiso 1 1 calc R . . H48C H -0.1565 0.3604 0.4652 0.088 Uiso 1 1 calc R . . C49 C 0.3661(6) 0.4496(2) 0.5937(3) 0.0401(13) Uani 1 1 d . . . C50 C 0.5021(7) 0.4253(3) 0.5902(3) 0.0563(17) Uani 1 1 d . . . H50A H 0.5341 0.4328 0.5502 0.084 Uiso 1 1 calc R . . H50B H 0.4983 0.3862 0.5964 0.084 Uiso 1 1 calc R . . H50C H 0.5599 0.4414 0.6218 0.084 Uiso 1 1 calc R . . C51 C 0.3692(8) 0.5091(3) 0.5754(4) 0.070(2) Uani 1 1 d . . . H51A H 0.3958 0.5121 0.5337 0.105 Uiso 1 1 calc R . . H51B H 0.4302 0.5285 0.6029 0.105 Uiso 1 1 calc R . . H51C H 0.2835 0.5247 0.5779 0.105 Uiso 1 1 calc R . . C52 C 0.3304(8) 0.4469(4) 0.6603(3) 0.072(2) Uani 1 1 d . . . H52A H 0.3947 0.4664 0.6859 0.108 Uiso 1 1 calc R . . H52B H 0.3278 0.4092 0.6733 0.108 Uiso 1 1 calc R . . H52C H 0.2460 0.4634 0.6641 0.108 Uiso 1 1 calc R . . C53 C 0.3176(9) 0.2690(3) 0.5621(3) 0.0591(19) Uani 1 1 d . . . H53A H 0.3508 0.2937 0.5314 0.071 Uiso 1 1 calc R . . H53B H 0.2744 0.2906 0.5925 0.071 Uiso 1 1 calc R . . C54 C 0.4218(11) 0.2378(4) 0.5912(6) 0.109(4) Uani 1 1 d . . . H54A H 0.4459 0.2528 0.6319 0.131 Uiso 1 1 calc R . . H54B H 0.4979 0.2391 0.5665 0.131 Uiso 1 1 calc R . . C55 C 0.3769(10) 0.1815(4) 0.5968(5) 0.093(3) Uani 1 1 d . . . H55A H 0.3758 0.1710 0.6400 0.111 Uiso 1 1 calc R . . H55B H 0.4340 0.1565 0.5761 0.111 Uiso 1 1 calc R . . C56 C 0.2460(9) 0.1798(3) 0.5675(4) 0.077(3) Uani 1 1 d . . . H56A H 0.2363 0.1483 0.5401 0.092 Uiso 1 1 calc R . . H56B H 0.1817 0.1770 0.5986 0.092 Uiso 1 1 calc R . . Li1 Li 0.0100(10) 0.3315(4) 0.3567(5) 0.044(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02810(16) 0.02695(14) 0.02561(14) 0.00164(9) 0.00016(10) -0.00251(10) O1 0.036(2) 0.0324(18) 0.0271(17) 0.0032(14) 0.0013(15) -0.0104(15) O2 0.036(2) 0.0301(18) 0.0322(18) -0.0022(14) 0.0042(15) -0.0018(15) O3 0.047(2) 0.049(2) 0.036(2) 0.0047(17) -0.0079(18) -0.0038(18) N1 0.027(2) 0.035(2) 0.028(2) 0.0018(16) 0.0017(17) 0.0005(17) N2 0.032(2) 0.048(3) 0.040(3) 0.005(2) -0.002(2) 0.002(2) N3 0.029(2) 0.030(2) 0.033(2) 0.0015(17) 0.0060(17) 0.0024(17) N4 0.030(2) 0.028(2) 0.0245(19) -0.0008(15) 0.0021(16) 0.0025(16) N5 0.037(3) 0.033(2) 0.034(2) 0.0030(17) 0.0022(19) 0.0023(18) N6 0.037(2) 0.029(2) 0.0230(19) 0.0053(16) 0.0011(17) 0.0022(17) C1 0.029(3) 0.031(2) 0.028(2) 0.0012(19) 0.002(2) 0.000(2) C2 0.037(3) 0.026(2) 0.035(3) 0.0001(19) 0.007(2) -0.003(2) C3 0.040(3) 0.028(3) 0.042(3) 0.002(2) 0.010(2) -0.008(2) C4 0.035(3) 0.040(3) 0.042(3) -0.007(2) 0.005(2) -0.010(2) C5 0.041(3) 0.036(3) 0.031(3) -0.004(2) 0.003(2) -0.004(2) C6 0.028(2) 0.032(2) 0.025(2) -0.0009(18) 0.0037(19) -0.0046(19) C7 0.028(3) 0.035(3) 0.028(2) -0.0036(19) 0.003(2) -0.005(2) C8 0.028(3) 0.037(3) 0.032(3) 0.006(2) 0.003(2) -0.003(2) C9 0.033(3) 0.059(4) 0.046(3) 0.003(3) -0.007(3) -0.004(3) C10 0.036(3) 0.080(5) 0.055(4) 0.005(4) -0.018(3) -0.005(3) C11 0.038(4) 0.082(5) 0.066(5) 0.018(4) -0.015(3) 0.006(4) C12 0.042(3) 0.049(4) 0.063(4) 0.014(3) -0.003(3) 0.012(3) C13 0.046(3) 0.041(3) 0.039(3) 0.008(2) 0.018(3) 0.003(3) C14 0.042(3) 0.087(5) 0.039(3) -0.008(3) 0.015(3) -0.020(3) C15 0.045(4) 0.185(11) 0.045(4) 0.045(5) -0.002(3) -0.026(5) C16 0.046(3) 0.031(3) 0.056(4) -0.001(2) 0.007(3) 0.001(2) C17 0.073(5) 0.049(4) 0.072(5) 0.010(3) -0.001(4) 0.022(4) C18 0.088(6) 0.046(4) 0.080(6) -0.025(4) -0.008(5) 0.015(4) C19 0.053(4) 0.038(3) 0.034(3) 0.006(2) 0.004(3) -0.010(3) C20 0.082(5) 0.062(4) 0.044(4) 0.006(3) 0.021(4) -0.024(4) C21 0.082(5) 0.045(4) 0.033(3) 0.004(2) 0.014(3) -0.014(3) C22 0.073(5) 0.057(4) 0.046(4) 0.013(3) -0.006(3) -0.003(4) C23 0.043(3) 0.043(3) 0.049(3) -0.011(3) 0.007(3) -0.016(3) C24 0.087(6) 0.094(6) 0.072(5) -0.013(5) 0.013(5) -0.062(5) C25 0.076(5) 0.045(4) 0.074(5) -0.016(3) 0.006(4) -0.015(4) C26 0.055(5) 0.073(5) 0.094(6) -0.006(5) -0.023(4) -0.014(4) C27 0.037(3) 0.025(2) 0.025(2) 0.0010(18) 0.004(2) 0.001(2) C28 0.043(3) 0.031(3) 0.032(3) 0.003(2) 0.009(2) 0.002(2) C29 0.045(3) 0.026(2) 0.031(3) -0.0038(19) 0.010(2) 0.003(2) C30 0.047(3) 0.034(3) 0.027(2) -0.004(2) 0.003(2) -0.001(2) C31 0.038(3) 0.032(3) 0.031(3) 0.003(2) 0.003(2) -0.001(2) C32 0.033(3) 0.023(2) 0.023(2) -0.0008(17) 0.0054(19) -0.0007(18) C33 0.027(2) 0.031(2) 0.020(2) 0.0003(17) 0.0024(18) 0.0007(19) C34 0.030(3) 0.038(3) 0.025(2) 0.0010(19) 0.004(2) -0.002(2) C35 0.035(3) 0.040(3) 0.048(3) 0.003(2) 0.004(2) -0.004(2) C36 0.032(3) 0.060(4) 0.065(5) 0.004(3) -0.002(3) 0.001(3) C37 0.040(4) 0.069(5) 0.057(4) 0.000(3) -0.002(3) 0.018(3) C38 0.044(3) 0.048(3) 0.047(3) 0.002(3) 0.001(3) 0.013(3) C39 0.049(3) 0.043(3) 0.023(2) 0.004(2) 0.003(2) 0.003(3) C40 0.060(4) 0.063(4) 0.030(3) 0.000(3) 0.000(3) -0.002(3) C41 0.049(4) 0.073(4) 0.027(3) 0.005(3) 0.012(3) -0.003(3) C42 0.048(3) 0.029(3) 0.031(3) 0.008(2) 0.003(2) 0.006(2) C43 0.055(4) 0.044(4) 0.061(4) 0.010(3) 0.008(3) 0.010(3) C44 0.063(4) 0.030(3) 0.050(4) 0.002(2) 0.002(3) 0.003(3) C45 0.043(3) 0.039(3) 0.042(3) -0.001(2) 0.015(3) -0.002(2) C46 0.072(5) 0.069(5) 0.060(4) -0.018(4) 0.044(4) -0.012(4) C47 0.058(4) 0.045(3) 0.060(4) 0.000(3) 0.028(3) -0.010(3) C48 0.041(4) 0.059(4) 0.079(5) -0.001(4) 0.019(3) 0.005(3) C49 0.046(3) 0.043(3) 0.031(3) -0.003(2) 0.000(2) -0.003(3) C50 0.053(4) 0.069(5) 0.045(4) -0.002(3) -0.012(3) -0.004(3) C51 0.080(6) 0.055(4) 0.071(5) -0.004(4) -0.028(4) -0.013(4) C52 0.069(5) 0.117(7) 0.031(3) -0.014(4) 0.002(3) -0.017(5) C53 0.083(5) 0.047(4) 0.044(4) 0.002(3) -0.021(4) -0.006(3) C54 0.089(7) 0.087(7) 0.144(11) -0.013(7) -0.061(7) -0.008(6) C55 0.102(7) 0.069(6) 0.101(7) 0.023(5) -0.046(6) 0.007(5) C56 0.102(7) 0.066(5) 0.059(5) 0.029(4) -0.036(4) -0.033(5) Li1 0.044(6) 0.043(5) 0.045(6) 0.008(4) 0.001(4) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O1 2.210(3) . ? Sm1 O2 2.334(4) . ? Sm1 N4 2.416(4) . ? Sm1 N1 2.480(4) . ? Sm1 O3 2.517(4) . ? Sm1 N5 2.567(5) . ? Sm1 N3 2.658(4) . ? Sm1 C34 2.965(5) . ? Sm1 C7 3.001(5) . ? Sm1 Li1 3.141(10) . ? O1 C1 1.334(6) . ? O2 C27 1.342(6) . ? O2 Li1 1.854(11) . ? O3 C53 1.449(8) . ? O3 C56 1.456(8) . ? N1 C8 1.345(7) . ? N1 C7 1.482(6) . ? N2 C12 1.353(7) . ? N2 C8 1.378(7) . ? N2 Li1 1.953(11) . ? N3 C16 1.497(7) . ? N3 C7 1.506(6) . ? N3 C13 1.515(6) . ? N4 C34 1.347(7) . ? N4 C33 1.456(6) . ? N5 C38 1.334(7) . ? N5 C34 1.380(6) . ? N6 C42 1.499(6) . ? N6 C33 1.501(6) . ? N6 C39 1.505(6) . ? N6 Li1 2.087(11) . ? C1 C6 1.412(7) . ? C1 C2 1.414(7) . ? C2 C3 1.396(7) . ? C2 C19 1.539(7) . ? C3 C4 1.389(8) . ? C3 H3 0.9400 . ? C4 C5 1.390(7) . ? C4 C23 1.533(7) . ? C5 C6 1.398(7) . ? C5 H5 0.9400 . ? C6 C7 1.529(7) . ? C7 H7 0.9900 . ? C8 C9 1.418(8) . ? C8 Li1 2.778(12) . ? C9 C10 1.368(9) . ? C9 H9 0.9400 . ? C10 C11 1.388(12) . ? C10 H10 0.9400 . ? C11 C12 1.364(10) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 C15 1.498(9) . ? C13 C14 1.508(8) . ? C13 H13 0.9900 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C17 1.481(9) . ? C16 C18 1.530(9) . ? C16 H16 0.9900 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C21 1.524(9) . ? C19 C20 1.526(8) . ? C19 C22 1.534(9) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 C24 1.513(9) . ? C23 C25 1.527(9) . ? C23 C26 1.537(10) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 C32 1.415(7) . ? C27 C28 1.427(7) . ? C27 Li1 2.726(12) . ? C28 C29 1.398(8) . ? C28 C45 1.533(8) . ? C29 C30 1.380(8) . ? C29 H29 0.9400 . ? C30 C31 1.397(7) . ? C30 C49 1.538(8) . ? C31 C32 1.383(7) . ? C31 H31 0.9400 . ? C32 C33 1.522(6) . ? C33 H33 0.9900 . ? C34 C35 1.412(7) . ? C35 C36 1.377(8) . ? C35 H35 0.9400 . ? C36 C37 1.378(11) . ? C36 H36 0.9400 . ? C37 C38 1.373(9) . ? C37 H37 0.9400 . ? C38 H38 0.9400 . ? C39 C41 1.531(8) . ? C39 C40 1.521(8) . ? C39 H39 0.9900 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 C43 1.526(8) . ? C42 C44 1.527(8) . ? C42 H42 0.9900 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? C45 C48 1.530(9) . ? C45 C47 1.537(8) . ? C45 C46 1.537(8) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C46 H46C 0.9700 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C49 C51 1.516(10) . ? C49 C52 1.521(8) . ? C49 C50 1.533(9) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C50 H50C 0.9700 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 H51C 0.9700 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 H52C 0.9700 . ? C53 C54 1.439(12) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.467(13) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.462(11) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sm1 O2 110.75(13) . . ? O1 Sm1 N4 175.24(13) . . ? O2 Sm1 N4 72.24(13) . . ? O1 Sm1 N1 79.32(13) . . ? O2 Sm1 N1 82.87(13) . . ? N4 Sm1 N1 104.93(13) . . ? O1 Sm1 O3 81.73(13) . . ? O2 Sm1 O3 89.95(13) . . ? N4 Sm1 O3 94.69(14) . . ? N1 Sm1 O3 155.80(15) . . ? O1 Sm1 N5 122.06(14) . . ? O2 Sm1 N5 121.09(13) . . ? N4 Sm1 N5 53.63(13) . . ? N1 Sm1 N5 128.64(14) . . ? O3 Sm1 N5 74.61(15) . . ? O1 Sm1 N3 79.62(13) . . ? O2 Sm1 N3 133.64(13) . . ? N4 Sm1 N3 101.07(13) . . ? N1 Sm1 N3 53.83(13) . . ? O3 Sm1 N3 136.31(13) . . ? N5 Sm1 N3 82.57(14) . . ? O1 Sm1 C34 148.83(14) . . ? O2 Sm1 C34 94.52(13) . . ? N4 Sm1 C34 26.57(14) . . ? N1 Sm1 C34 123.16(14) . . ? O3 Sm1 C34 80.31(14) . . ? N5 Sm1 C34 27.71(13) . . ? N3 Sm1 C34 96.29(13) . . ? O1 Sm1 C7 64.95(13) . . ? O2 Sm1 C7 111.85(13) . . ? N4 Sm1 C7 117.82(13) . . ? N1 Sm1 C7 29.45(13) . . ? O3 Sm1 C7 144.70(13) . . ? N5 Sm1 C7 112.65(14) . . ? N3 Sm1 C7 30.09(13) . . ? C34 Sm1 C7 122.89(14) . . ? O1 Sm1 Li1 121.7(2) . . ? O2 Sm1 Li1 35.9(2) . . ? N4 Sm1 Li1 62.9(2) . . ? N1 Sm1 Li1 57.0(2) . . ? O3 Sm1 Li1 124.1(2) . . ? N5 Sm1 Li1 115.3(2) . . ? N3 Sm1 Li1 99.3(2) . . ? C34 Sm1 Li1 89.4(2) . . ? C7 Sm1 Li1 85.4(2) . . ? C1 O1 Sm1 134.3(3) . . ? C27 O2 Li1 116.2(4) . . ? C27 O2 Sm1 118.2(3) . . ? Li1 O2 Sm1 96.5(4) . . ? C53 O3 C56 105.9(5) . . ? C53 O3 Sm1 128.1(4) . . ? C56 O3 Sm1 121.0(4) . . ? C8 N1 C7 116.5(4) . . ? C8 N1 Sm1 147.8(4) . . ? C7 N1 Sm1 95.2(3) . . ? C12 N2 C8 118.4(5) . . ? C12 N2 Li1 129.3(5) . . ? C8 N2 Li1 111.8(5) . . ? C16 N3 C7 117.2(4) . . ? C16 N3 C13 112.8(4) . . ? C7 N3 C13 108.5(4) . . ? C16 N3 Sm1 122.0(3) . . ? C7 N3 Sm1 87.7(3) . . ? C13 N3 Sm1 105.7(3) . . ? C34 N4 C33 120.5(4) . . ? C34 N4 Sm1 100.1(3) . . ? C33 N4 Sm1 129.4(3) . . ? C38 N5 C34 119.6(5) . . ? C38 N5 Sm1 146.9(4) . . ? C34 N5 Sm1 92.4(3) . . ? C42 N6 C33 116.6(4) . . ? C42 N6 C39 111.3(4) . . ? C33 N6 C39 110.2(4) . . ? C42 N6 Li1 105.7(4) . . ? C33 N6 Li1 101.3(4) . . ? C39 N6 Li1 111.3(4) . . ? O1 C1 C6 118.2(4) . . ? O1 C1 C2 123.1(4) . . ? C6 C1 C2 118.8(5) . . ? C3 C2 C1 118.1(5) . . ? C3 C2 C19 120.4(5) . . ? C1 C2 C19 121.5(5) . . ? C4 C3 C2 124.5(5) . . ? C4 C3 H3 117.7 . . ? C2 C3 H3 117.7 . . ? C3 C4 C5 116.1(5) . . ? C3 C4 C23 123.3(5) . . ? C5 C4 C23 120.7(5) . . ? C4 C5 C6 122.5(5) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C1 120.0(5) . . ? C5 C6 C7 117.0(4) . . ? C1 C6 C7 122.8(4) . . ? N1 C7 N3 102.6(4) . . ? N1 C7 C6 113.0(4) . . ? N3 C7 C6 117.7(4) . . ? N1 C7 Sm1 55.4(2) . . ? N3 C7 Sm1 62.3(2) . . ? C6 C7 Sm1 99.0(3) . . ? N1 C7 H7 107.7 . . ? N3 C7 H7 107.7 . . ? C6 C7 H7 107.7 . . ? Sm1 C7 H7 152.9 . . ? N1 C8 N2 115.1(5) . . ? N1 C8 C9 126.5(5) . . ? N2 C8 C9 118.4(5) . . ? N1 C8 Li1 74.4(4) . . ? N2 C8 Li1 40.8(3) . . ? C9 C8 Li1 158.9(5) . . ? C10 C9 C8 120.6(6) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 120.6(6) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 116.7(6) . . ? C12 C11 H11 121.6 . . ? C10 C11 H11 121.6 . . ? N2 C12 C11 125.1(6) . . ? N2 C12 H12 117.4 . . ? C11 C12 H12 117.4 . . ? C15 C13 C14 108.3(5) . . ? C15 C13 N3 116.4(5) . . ? C14 C13 N3 115.4(5) . . ? C15 C13 H13 105.2 . . ? C14 C13 H13 105.2 . . ? N3 C13 H13 105.2 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N3 114.0(5) . . ? C17 C16 C18 111.9(6) . . ? N3 C16 C18 117.4(5) . . ? C17 C16 H16 103.9 . . ? N3 C16 H16 103.9 . . ? C18 C16 H16 103.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C19 C20 106.5(5) . . ? C21 C19 C2 111.7(5) . . ? C20 C19 C2 111.8(5) . . ? C21 C19 C22 110.0(5) . . ? C20 C19 C22 108.3(6) . . ? C2 C19 C22 108.6(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C25 108.6(6) . . ? C24 C23 C4 112.2(5) . . ? C25 C23 C4 109.5(5) . . ? C24 C23 C26 108.3(7) . . ? C25 C23 C26 108.7(6) . . ? C4 C23 C26 109.4(5) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O2 C27 C32 120.1(4) . . ? O2 C27 C28 121.5(5) . . ? C32 C27 C28 118.4(4) . . ? O2 C27 Li1 37.6(3) . . ? C32 C27 Li1 92.0(4) . . ? C28 C27 Li1 139.4(4) . . ? C29 C28 C27 117.6(5) . . ? C29 C28 C45 120.8(5) . . ? C27 C28 C45 121.6(5) . . ? C30 C29 C28 123.9(5) . . ? C30 C29 H29 118.1 . . ? C28 C29 H29 118.1 . . ? C29 C30 C31 117.1(5) . . ? C29 C30 C49 122.6(5) . . ? C31 C30 C49 120.3(5) . . ? C32 C31 C30 121.8(5) . . ? C32 C31 H31 119.1 . . ? C30 C31 H31 119.1 . . ? C31 C32 C27 120.2(4) . . ? C31 C32 C33 119.4(4) . . ? C27 C32 C33 119.8(4) . . ? N4 C33 N6 107.9(4) . . ? N4 C33 C32 108.2(4) . . ? N6 C33 C32 113.9(4) . . ? N4 C33 H33 108.9 . . ? N6 C33 H33 108.9 . . ? C32 C33 H33 108.9 . . ? N4 C34 N5 111.4(4) . . ? N4 C34 C35 129.8(5) . . ? N5 C34 C35 118.9(5) . . ? N4 C34 Sm1 53.4(2) . . ? N5 C34 Sm1 59.9(3) . . ? C35 C34 Sm1 167.1(4) . . ? C36 C35 C34 119.0(6) . . ? C36 C35 H35 120.5 . . ? C34 C35 H35 120.5 . . ? C35 C36 C37 121.1(6) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? C38 C37 C36 117.5(6) . . ? C38 C37 H37 121.2 . . ? C36 C37 H37 121.2 . . ? N5 C38 C37 123.5(6) . . ? N5 C38 H38 118.2 . . ? C37 C38 H38 118.2 . . ? N6 C39 C41 115.8(5) . . ? N6 C39 C40 111.7(5) . . ? C41 C39 C40 111.1(5) . . ? N6 C39 H39 105.8 . . ? C41 C39 H39 105.8 . . ? C40 C39 H39 105.8 . . ? 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 . . ? N6 C42 C43 111.7(5) . . ? N6 C42 C44 116.5(5) . . ? C43 C42 C44 110.2(5) . . ? N6 C42 H42 105.9 . . ? C43 C42 H42 105.9 . . ? C44 C42 H42 105.9 . . ? 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 . . ? C48 C45 C47 109.9(6) . . ? C48 C45 C28 108.2(5) . . ? C47 C45 C28 112.1(5) . . ? C48 C45 C46 107.3(6) . . ? C47 C45 C46 106.6(5) . . ? C28 C45 C46 112.6(5) . . ? 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 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C51 C49 C52 107.7(6) . . ? C51 C49 C50 109.2(6) . . ? C52 C49 C50 107.8(6) . . ? C51 C49 C30 109.8(5) . . ? C52 C49 C30 112.5(5) . . ? C50 C49 C30 109.7(5) . . ? 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 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 O3 106.6(6) . . ? C54 C53 H53A 110.4 . . ? O3 C53 H53A 110.4 . . ? C54 C53 H53B 110.4 . . ? O3 C53 H53B 110.4 . . ? H53A C53 H53B 108.6 . . ? C53 C54 C55 107.8(8) . . ? C53 C54 H54A 110.1 . . ? C55 C54 H54A 110.1 . . ? C53 C54 H54B 110.1 . . ? C55 C54 H54B 110.1 . . ? H54A C54 H54B 108.5 . . ? C54 C55 C56 106.3(7) . . ? C54 C55 H55A 110.5 . . ? C56 C55 H55A 110.5 . . ? C54 C55 H55B 110.5 . . ? C56 C55 H55B 110.5 . . ? H55A C55 H55B 108.7 . . ? O3 C56 C55 106.8(6) . . ? O3 C56 H56A 110.4 . . ? C55 C56 H56A 110.4 . . ? O3 C56 H56B 110.4 . . ? C55 C56 H56B 110.4 . . ? H56A C56 H56B 108.6 . . ? O2 Li1 N2 118.0(6) . . ? O2 Li1 N6 102.7(5) . . ? N2 Li1 N6 138.9(6) . . ? O2 Li1 C27 26.2(2) . . ? N2 Li1 C27 139.9(5) . . ? N6 Li1 C27 80.9(4) . . ? O2 Li1 C8 103.9(4) . . ? N2 Li1 C8 27.4(2) . . ? N6 Li1 C8 139.0(5) . . ? C27 Li1 C8 130.1(4) . . ? O2 Li1 Sm1 47.6(3) . . ? N2 Li1 Sm1 103.3(4) . . ? N6 Li1 Sm1 99.6(4) . . ? C27 Li1 Sm1 65.5(2) . . ? C8 Li1 Sm1 76.8(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.510 _refine_diff_density_min -0.871 _refine_diff_density_rms 0.084 #============================================================end data_complex3 _database_code_depnum_ccdc_archive 'CCDC 723166' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H86 Li N6 O3 Yb' _chemical_formula_sum 'C56 H86 Li N6 O3 Yb' _chemical_formula_weight 1071.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 10.1840(11) _cell_length_b 24.704(3) _cell_length_c 21.786(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.562(2) _cell_angle_gamma 90.00 _cell_volume 5470.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 17161 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2244 _exptl_absorpt_coefficient_mu 1.756 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.573 _exptl_absorpt_correction_T_max 0.768 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38866 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10118 _reflns_number_gt 9421 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+17.0054P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10118 _refine_ls_number_parameters 625 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.0976 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.132108(19) 0.227985(8) 0.418928(9) 0.02274(7) Uani 1 1 d . . . O1 O 0.0192(3) 0.16444(13) 0.45704(14) 0.0264(7) Uani 1 1 d . . . O2 O 0.0382(3) 0.30803(12) 0.43631(14) 0.0252(7) Uani 1 1 d . . . O3 O 0.2221(3) 0.22964(14) 0.52476(15) 0.0346(8) Uani 1 1 d . . . N1 N -0.0349(4) 0.22078(15) 0.33758(17) 0.0239(8) Uani 1 1 d . . . N2 N -0.1478(4) 0.29852(18) 0.30972(19) 0.0340(10) Uani 1 1 d . . . N3 N 0.1387(4) 0.16086(15) 0.32883(17) 0.0241(8) Uani 1 1 d . . . N4 N 0.2770(4) 0.29311(15) 0.38641(17) 0.0228(8) Uani 1 1 d . . . N5 N 0.3698(4) 0.21375(15) 0.41378(17) 0.0248(8) Uani 1 1 d . . . N6 N 0.1784(4) 0.36914(16) 0.33368(17) 0.0271(9) Uani 1 1 d . . . C1 C -0.0684(4) 0.12990(18) 0.4315(2) 0.0243(10) Uani 1 1 d . . . C2 C -0.1476(5) 0.09658(19) 0.4673(2) 0.0280(11) Uani 1 1 d . . . C3 C -0.2340(5) 0.0603(2) 0.4365(2) 0.0320(11) Uani 1 1 d . . . H3 H -0.2860 0.0381 0.4602 0.038 Uiso 1 1 calc R . . C4 C -0.2477(5) 0.0552(2) 0.3731(2) 0.0314(11) Uani 1 1 d . . . C5 C -0.1692(4) 0.0881(2) 0.3395(2) 0.0283(11) Uani 1 1 d . . . H5 H -0.1754 0.0853 0.2964 0.034 Uiso 1 1 calc R . . C6 C -0.0811(4) 0.12529(19) 0.3672(2) 0.0261(10) Uani 1 1 d . . . C7 C -0.0099(4) 0.16353(19) 0.3249(2) 0.0241(10) Uani 1 1 d . . . H7 H -0.0417 0.1559 0.2820 0.029 Uiso 1 1 calc R . . C8 C -0.1393(5) 0.2434(2) 0.3065(2) 0.0285(11) Uani 1 1 d . . . C9 C -0.2385(5) 0.2150(2) 0.2704(2) 0.0364(12) Uani 1 1 d . . . H9 H -0.2374 0.1769 0.2693 0.044 Uiso 1 1 calc R . . C10 C -0.3348(5) 0.2425(3) 0.2376(3) 0.0487(15) Uani 1 1 d . . . H10 H -0.3983 0.2233 0.2132 0.058 Uiso 1 1 calc R . . C11 C -0.3402(6) 0.2979(3) 0.2398(3) 0.0545(17) Uani 1 1 d . . . H11 H -0.4054 0.3174 0.2167 0.065 Uiso 1 1 calc R . . C12 C -0.2467(5) 0.3237(2) 0.2770(3) 0.0457(14) Uani 1 1 d . . . H12 H -0.2518 0.3616 0.2799 0.055 Uiso 1 1 calc R . . C13 C 0.1879(5) 0.1944(2) 0.2759(2) 0.0294(11) Uani 1 1 d . . . H13 H 0.1761 0.2326 0.2883 0.035 Uiso 1 1 calc R . . C14 C 0.3338(5) 0.1888(2) 0.2662(2) 0.0418(14) Uani 1 1 d . . . H14A H 0.3834 0.1897 0.3057 0.063 Uiso 1 1 calc R . . H14B H 0.3617 0.2184 0.2409 0.063 Uiso 1 1 calc R . . H14C H 0.3495 0.1547 0.2459 0.063 Uiso 1 1 calc R . . C15 C 0.1114(5) 0.1890(3) 0.2138(3) 0.0500(15) Uani 1 1 d . . . H15A H 0.1085 0.1513 0.2016 0.075 Uiso 1 1 calc R . . H15B H 0.1545 0.2100 0.1833 0.075 Uiso 1 1 calc R . . H15C H 0.0225 0.2023 0.2171 0.075 Uiso 1 1 calc R . . C16 C 0.2006(5) 0.1057(2) 0.3333(2) 0.0346(12) Uani 1 1 d . . . H16 H 0.2943 0.1116 0.3254 0.041 Uiso 1 1 calc R . . C17 C 0.2025(6) 0.0805(2) 0.3966(3) 0.0493(15) Uani 1 1 d . . . H17A H 0.2259 0.1078 0.4274 0.074 Uiso 1 1 calc R . . H17B H 0.2668 0.0515 0.3995 0.074 Uiso 1 1 calc R . . H17C H 0.1161 0.0661 0.4035 0.074 Uiso 1 1 calc R . . C18 C 0.1506(6) 0.0647(2) 0.2846(3) 0.0541(17) Uani 1 1 d . . . H18A H 0.0570 0.0590 0.2878 0.081 Uiso 1 1 calc R . . H18B H 0.1968 0.0307 0.2912 0.081 Uiso 1 1 calc R . . H18C H 0.1663 0.0785 0.2440 0.081 Uiso 1 1 calc R . . C19 C -0.1382(5) 0.0981(2) 0.5378(2) 0.0346(12) Uani 1 1 d . . . C20 C -0.2545(6) 0.0686(3) 0.5653(3) 0.0535(17) Uani 1 1 d . . . H20A H -0.3364 0.0857 0.5510 0.080 Uiso 1 1 calc R . . H20B H -0.2447 0.0705 0.6099 0.080 Uiso 1 1 calc R . . H20C H -0.2553 0.0310 0.5525 0.080 Uiso 1 1 calc R . . C21 C -0.1429(6) 0.1563(2) 0.5623(2) 0.0441(14) Uani 1 1 d . . . H21A H -0.0678 0.1764 0.5491 0.066 Uiso 1 1 calc R . . H21B H -0.1404 0.1557 0.6069 0.066 Uiso 1 1 calc R . . H21C H -0.2234 0.1737 0.5464 0.066 Uiso 1 1 calc R . . C22 C -0.0105(6) 0.0707(2) 0.5612(3) 0.0541(17) Uani 1 1 d . . . H22A H -0.0124 0.0329 0.5490 0.081 Uiso 1 1 calc R . . H22B H -0.0014 0.0731 0.6057 0.081 Uiso 1 1 calc R . . H22C H 0.0635 0.0886 0.5439 0.081 Uiso 1 1 calc R . . C23 C -0.3456(5) 0.0154(2) 0.3406(3) 0.0404(13) Uani 1 1 d . . . C24 C -0.4253(8) -0.0152(3) 0.3854(3) 0.080(3) Uani 1 1 d . . . H24A H -0.3666 -0.0357 0.4135 0.121 Uiso 1 1 calc R . . H24B H -0.4850 -0.0398 0.3630 0.121 Uiso 1 1 calc R . . H24C H -0.4754 0.0102 0.4086 0.121 Uiso 1 1 calc R . . C25 C -0.2732(7) -0.0259(2) 0.3034(3) 0.0593(18) Uani 1 1 d . . . H25A H -0.2186 -0.0485 0.3310 0.089 Uiso 1 1 calc R . . H25B H -0.2183 -0.0072 0.2754 0.089 Uiso 1 1 calc R . . H25C H -0.3366 -0.0483 0.2801 0.089 Uiso 1 1 calc R . . C26 C -0.4400(6) 0.0475(3) 0.2964(3) 0.065(2) Uani 1 1 d . . . H26A H -0.5019 0.0228 0.2755 0.098 Uiso 1 1 calc R . . H26B H -0.3901 0.0661 0.2664 0.098 Uiso 1 1 calc R . . H26C H -0.4877 0.0737 0.3195 0.098 Uiso 1 1 calc R . . C27 C 0.1027(4) 0.34682(18) 0.4702(2) 0.0251(10) Uani 1 1 d . . . C28 C 0.0567(5) 0.36597(19) 0.5260(2) 0.0273(10) Uani 1 1 d . . . C29 C 0.1415(5) 0.39858(19) 0.5627(2) 0.0303(11) Uani 1 1 d . . . H29 H 0.1126 0.4104 0.6006 0.036 Uiso 1 1 calc R . . C30 C 0.2662(5) 0.41489(19) 0.5470(2) 0.0277(10) Uani 1 1 d . . . C31 C 0.3002(5) 0.40110(19) 0.4882(2) 0.0272(10) Uani 1 1 d . . . H31 H 0.3798 0.4140 0.4743 0.033 Uiso 1 1 calc R . . C32 C 0.2197(5) 0.36860(18) 0.4492(2) 0.0246(10) Uani 1 1 d . . . C33 C 0.2698(5) 0.35191(19) 0.3878(2) 0.0252(10) Uani 1 1 d . . . H33 H 0.3584 0.3674 0.3835 0.030 Uiso 1 1 calc R . . C34 C 0.3914(5) 0.2668(2) 0.4008(2) 0.0266(10) Uani 1 1 d . . . C35 C 0.5217(5) 0.2867(2) 0.4032(2) 0.0362(12) Uani 1 1 d . . . H35 H 0.5377 0.3238 0.3973 0.043 Uiso 1 1 calc R . . C36 C 0.6245(5) 0.2515(3) 0.4140(3) 0.0445(14) Uani 1 1 d . . . H36 H 0.7115 0.2643 0.4146 0.053 Uiso 1 1 calc R . . C37 C 0.6007(5) 0.1972(3) 0.4241(3) 0.0444(14) Uani 1 1 d . . . H37 H 0.6705 0.1725 0.4306 0.053 Uiso 1 1 calc R . . C38 C 0.4731(5) 0.1805(2) 0.4244(2) 0.0362(12) Uani 1 1 d . . . H38 H 0.4566 0.1438 0.4325 0.043 Uiso 1 1 calc R . . C39 C 0.2337(5) 0.3514(2) 0.2750(2) 0.0309(11) Uani 1 1 d . . . H39 H 0.2688 0.3144 0.2827 0.037 Uiso 1 1 calc R . . C40 C 0.1255(6) 0.3459(2) 0.2237(2) 0.0446(14) Uani 1 1 d . . . H40A H 0.0563 0.3226 0.2373 0.067 Uiso 1 1 calc R . . H40B H 0.1619 0.3302 0.1876 0.067 Uiso 1 1 calc R . . H40C H 0.0895 0.3813 0.2135 0.067 Uiso 1 1 calc R . . C41 C 0.3472(6) 0.3847(2) 0.2532(2) 0.0454(14) Uani 1 1 d . . . H41A H 0.3162 0.4207 0.2422 0.068 Uiso 1 1 calc R . . H41B H 0.3817 0.3674 0.2176 0.068 Uiso 1 1 calc R . . H41C H 0.4160 0.3871 0.2859 0.068 Uiso 1 1 calc R . . C42 C 0.1420(5) 0.4281(2) 0.3312(2) 0.0333(12) Uani 1 1 d . . . H42 H 0.1246 0.4366 0.2870 0.040 Uiso 1 1 calc R . . C43 C 0.0119(6) 0.4390(2) 0.3611(3) 0.0486(15) Uani 1 1 d . . . H43A H -0.0559 0.4152 0.3431 0.073 Uiso 1 1 calc R . . H43B H -0.0141 0.4763 0.3541 0.073 Uiso 1 1 calc R . . H43C H 0.0234 0.4322 0.4050 0.073 Uiso 1 1 calc R . . C44 C 0.2459(6) 0.4690(2) 0.3552(3) 0.0449(14) Uani 1 1 d . . . H44A H 0.2498 0.4694 0.3998 0.067 Uiso 1 1 calc R . . H44B H 0.2228 0.5047 0.3396 0.067 Uiso 1 1 calc R . . H44C H 0.3311 0.4587 0.3413 0.067 Uiso 1 1 calc R . . C45 C -0.0817(5) 0.3515(2) 0.5461(2) 0.0345(12) Uani 1 1 d . . . C46 C -0.1147(6) 0.3816(3) 0.6041(3) 0.0539(17) Uani 1 1 d . . . H46A H -0.1049 0.4202 0.5979 0.081 Uiso 1 1 calc R . . H46B H -0.0555 0.3700 0.6382 0.081 Uiso 1 1 calc R . . H46C H -0.2047 0.3737 0.6133 0.081 Uiso 1 1 calc R . . C47 C -0.0922(6) 0.2909(2) 0.5584(3) 0.0489(16) Uani 1 1 d . . . H47A H -0.1780 0.2828 0.5731 0.073 Uiso 1 1 calc R . . H47B H -0.0243 0.2802 0.5892 0.073 Uiso 1 1 calc R . . H47C H -0.0809 0.2710 0.5206 0.073 Uiso 1 1 calc R . . C48 C -0.1838(5) 0.3681(3) 0.4957(3) 0.0511(16) Uani 1 1 d . . . H48A H -0.2708 0.3581 0.5076 0.077 Uiso 1 1 calc R . . H48B H -0.1659 0.3499 0.4577 0.077 Uiso 1 1 calc R . . H48C H -0.1800 0.4070 0.4897 0.077 Uiso 1 1 calc R . . C49 C 0.3608(5) 0.4461(2) 0.5915(2) 0.0350(12) Uani 1 1 d . . . C50 C 0.5004(6) 0.4254(3) 0.5869(3) 0.0604(19) Uani 1 1 d . . . H50A H 0.5582 0.4429 0.6179 0.091 Uiso 1 1 calc R . . H50B H 0.5298 0.4336 0.5464 0.091 Uiso 1 1 calc R . . H50C H 0.5024 0.3866 0.5933 0.091 Uiso 1 1 calc R . . C51 C 0.3545(8) 0.5058(3) 0.5757(4) 0.084(3) Uani 1 1 d . . . H51A H 0.2676 0.5197 0.5827 0.126 Uiso 1 1 calc R . . H51B H 0.3720 0.5107 0.5327 0.126 Uiso 1 1 calc R . . H51C H 0.4198 0.5253 0.6013 0.126 Uiso 1 1 calc R . . C52 C 0.3284(8) 0.4386(4) 0.6581(3) 0.086(3) Uani 1 1 d . . . H52A H 0.2424 0.4538 0.6642 0.128 Uiso 1 1 calc R . . H52B H 0.3941 0.4568 0.6848 0.128 Uiso 1 1 calc R . . H52C H 0.3280 0.4003 0.6679 0.128 Uiso 1 1 calc R . . C53 C 0.3112(6) 0.2688(2) 0.5540(3) 0.0497(16) Uani 1 1 d D . . H53A H 0.2662 0.2900 0.5844 0.060 Uiso 1 1 calc R . . H53B H 0.3439 0.2936 0.5233 0.060 Uiso 1 1 calc R . . C54 C 0.4200(8) 0.2381(3) 0.5839(5) 0.096(3) Uani 1 1 d D . . H54A H 0.4458 0.2540 0.6241 0.115 Uiso 1 1 calc R . . H54B H 0.4962 0.2388 0.5587 0.115 Uiso 1 1 calc R . . C55 C 0.3746(8) 0.1821(3) 0.5915(4) 0.077(2) Uani 1 1 d . . . H55A H 0.3698 0.1732 0.6352 0.092 Uiso 1 1 calc R . . H55B H 0.4342 0.1565 0.5731 0.092 Uiso 1 1 calc R . . C56 C 0.2413(7) 0.1802(3) 0.5591(3) 0.066(2) Uani 1 1 d . . . H56A H 0.2347 0.1490 0.5312 0.079 Uiso 1 1 calc R . . H56B H 0.1738 0.1766 0.5889 0.079 Uiso 1 1 calc R . . Li1 Li 0.0092(9) 0.3268(4) 0.3541(4) 0.038(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.02167(11) 0.02577(12) 0.02076(10) 0.00116(8) 0.00099(7) -0.00117(9) O1 0.0272(17) 0.0315(19) 0.0201(16) 0.0001(13) -0.0015(13) -0.0090(14) O2 0.0273(17) 0.0227(17) 0.0259(17) -0.0026(13) 0.0033(13) 0.0001(14) O3 0.040(2) 0.040(2) 0.0227(17) 0.0029(15) -0.0038(15) -0.0014(17) N1 0.0217(19) 0.029(2) 0.0207(19) 0.0005(16) 0.0017(15) -0.0003(17) N2 0.028(2) 0.042(3) 0.032(2) 0.0063(19) -0.0005(18) 0.0052(19) N3 0.0200(19) 0.029(2) 0.024(2) 0.0015(16) 0.0037(15) -0.0009(16) N4 0.026(2) 0.0205(19) 0.0216(19) 0.0017(15) 0.0030(16) -0.0023(16) N5 0.025(2) 0.025(2) 0.025(2) -0.0001(16) -0.0013(16) 0.0023(16) N6 0.031(2) 0.028(2) 0.022(2) 0.0024(16) 0.0038(17) 0.0016(18) C1 0.023(2) 0.025(3) 0.025(2) 0.0005(19) 0.0017(19) -0.0004(19) C2 0.031(3) 0.026(3) 0.027(3) 0.005(2) 0.004(2) 0.005(2) C3 0.030(3) 0.028(3) 0.039(3) 0.003(2) 0.008(2) -0.005(2) C4 0.030(3) 0.030(3) 0.035(3) -0.004(2) 0.004(2) -0.003(2) C5 0.025(2) 0.038(3) 0.023(2) -0.004(2) 0.0043(19) 0.001(2) C6 0.025(2) 0.026(3) 0.028(2) 0.001(2) 0.0038(19) -0.003(2) C7 0.019(2) 0.032(3) 0.022(2) -0.0029(19) 0.0014(18) -0.0025(19) C8 0.024(2) 0.035(3) 0.027(3) 0.004(2) 0.006(2) -0.001(2) C9 0.027(3) 0.043(3) 0.038(3) -0.002(2) -0.005(2) -0.001(2) C10 0.029(3) 0.070(5) 0.047(4) 0.002(3) -0.006(3) 0.000(3) C11 0.030(3) 0.074(5) 0.058(4) 0.014(3) -0.012(3) 0.012(3) C12 0.037(3) 0.046(4) 0.054(4) 0.014(3) 0.004(3) 0.011(3) C13 0.028(3) 0.036(3) 0.025(2) 0.004(2) 0.008(2) -0.004(2) C14 0.032(3) 0.061(4) 0.033(3) -0.011(3) 0.011(2) -0.005(3) C15 0.036(3) 0.078(5) 0.036(3) 0.006(3) 0.003(2) -0.005(3) C16 0.028(3) 0.033(3) 0.043(3) -0.004(2) 0.005(2) 0.005(2) C17 0.049(4) 0.036(3) 0.064(4) 0.012(3) 0.008(3) 0.010(3) C18 0.061(4) 0.038(3) 0.063(4) -0.019(3) 0.006(3) 0.009(3) C19 0.042(3) 0.031(3) 0.032(3) 0.005(2) 0.003(2) -0.007(2) C20 0.066(4) 0.062(4) 0.034(3) 0.006(3) 0.016(3) -0.022(3) C21 0.066(4) 0.039(3) 0.029(3) 0.000(2) 0.015(3) -0.007(3) C22 0.066(4) 0.050(4) 0.044(4) 0.008(3) -0.012(3) 0.003(3) C23 0.034(3) 0.041(3) 0.047(3) -0.009(3) 0.005(2) -0.011(2) C24 0.084(6) 0.088(6) 0.071(5) -0.022(4) 0.020(4) -0.060(5) C25 0.066(4) 0.043(4) 0.068(5) -0.019(3) -0.001(4) -0.007(3) C26 0.040(4) 0.066(5) 0.086(5) -0.021(4) -0.017(3) -0.009(3) C27 0.027(2) 0.025(3) 0.023(2) 0.0068(19) 0.0014(19) 0.003(2) C28 0.028(2) 0.025(3) 0.030(3) 0.002(2) 0.007(2) 0.004(2) C29 0.035(3) 0.031(3) 0.026(2) -0.001(2) 0.009(2) 0.003(2) C30 0.036(3) 0.028(3) 0.019(2) 0.0001(19) 0.001(2) 0.002(2) C31 0.028(2) 0.029(3) 0.025(2) 0.001(2) 0.0020(19) -0.004(2) C32 0.029(2) 0.023(2) 0.023(2) 0.0032(19) 0.0074(19) 0.003(2) C33 0.028(2) 0.031(3) 0.018(2) -0.0003(19) 0.0047(18) 0.000(2) C34 0.029(2) 0.033(3) 0.018(2) -0.002(2) -0.0002(18) -0.001(2) C35 0.026(3) 0.038(3) 0.045(3) 0.005(2) 0.004(2) -0.005(2) C36 0.025(3) 0.057(4) 0.052(4) 0.000(3) 0.002(2) 0.001(3) C37 0.029(3) 0.054(4) 0.050(4) 0.003(3) -0.004(3) 0.013(3) C38 0.039(3) 0.034(3) 0.035(3) 0.001(2) 0.001(2) 0.009(2) C39 0.043(3) 0.029(3) 0.021(2) 0.003(2) 0.004(2) 0.004(2) C40 0.052(4) 0.054(4) 0.029(3) -0.002(3) 0.003(3) -0.002(3) C41 0.053(4) 0.059(4) 0.026(3) 0.001(3) 0.016(3) -0.002(3) C42 0.042(3) 0.029(3) 0.029(3) 0.005(2) 0.003(2) 0.006(2) C43 0.049(4) 0.042(3) 0.056(4) 0.008(3) 0.014(3) 0.018(3) C44 0.062(4) 0.025(3) 0.048(4) 0.006(2) 0.007(3) 0.000(3) C45 0.036(3) 0.034(3) 0.034(3) -0.002(2) 0.011(2) 0.001(2) C46 0.052(4) 0.057(4) 0.056(4) -0.019(3) 0.033(3) -0.008(3) C47 0.053(4) 0.042(3) 0.055(4) 0.005(3) 0.031(3) -0.003(3) C48 0.033(3) 0.063(4) 0.059(4) 0.002(3) 0.010(3) 0.006(3) C49 0.042(3) 0.039(3) 0.024(3) -0.005(2) 0.003(2) -0.002(2) C50 0.047(4) 0.077(5) 0.055(4) -0.020(4) -0.014(3) -0.002(3) C51 0.093(6) 0.043(4) 0.110(7) -0.014(4) -0.041(5) -0.005(4) C52 0.077(5) 0.152(8) 0.027(3) -0.009(4) -0.004(3) -0.038(5) C53 0.069(4) 0.040(3) 0.038(3) -0.001(3) -0.018(3) -0.007(3) C54 0.078(6) 0.070(6) 0.130(8) -0.002(5) -0.070(6) -0.005(4) C55 0.085(6) 0.067(5) 0.073(5) 0.012(4) -0.035(4) 0.010(4) C56 0.080(5) 0.060(4) 0.053(4) 0.023(3) -0.032(4) -0.026(4) Li1 0.041(5) 0.038(5) 0.033(5) 0.006(4) -0.004(4) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O1 2.144(3) . ? Yb1 O2 2.239(3) . ? Yb1 N4 2.323(4) . ? Yb1 N1 2.386(4) . ? Yb1 O3 2.428(3) . ? Yb1 N5 2.456(4) . ? Yb1 N3 2.574(4) . ? Yb1 C34 2.859(5) . ? Yb1 C7 2.907(4) . ? Yb1 Li1 3.050(9) . ? Yb1 C27 3.162(5) . ? Yb1 C1 3.191(5) . ? O1 C1 1.330(5) . ? O2 C27 1.355(5) . ? O2 Li1 1.856(9) . ? O3 C56 1.439(7) . ? O3 C53 1.446(6) . ? N1 C8 1.346(6) . ? N1 C7 1.466(6) . ? N1 Li1 2.677(10) . ? N2 C12 1.349(6) . ? N2 C8 1.367(6) . ? N2 Li1 1.946(10) . ? N3 C16 1.502(6) . ? N3 C7 1.512(5) . ? N3 C13 1.529(6) . ? N4 C34 1.353(6) . ? N4 C33 1.455(6) . ? N5 C38 1.343(6) . ? N5 C34 1.362(6) . ? N6 C39 1.494(6) . ? N6 C42 1.503(6) . ? N6 C33 1.517(6) . ? N6 Li1 2.087(10) . ? C1 C6 1.404(6) . ? C1 C2 1.419(6) . ? C2 C3 1.398(7) . ? C2 C19 1.534(7) . ? C3 C4 1.384(7) . ? C3 H3 0.9400 . ? C4 C5 1.382(7) . ? C4 C23 1.542(7) . ? C5 C6 1.395(6) . ? C5 H5 0.9400 . ? C6 C7 1.532(6) . ? C7 H7 0.9900 . ? C8 C9 1.425(7) . ? C8 Li1 2.723(10) . ? C9 C10 1.359(7) . ? C9 H9 0.9400 . ? C10 C11 1.371(9) . ? C10 H10 0.9400 . ? C11 C12 1.368(8) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 C14 1.520(6) . ? C13 C15 1.525(7) . ? C13 H13 0.9900 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C17 1.512(8) . ? C16 C18 1.530(7) . ? C16 H16 0.9900 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C22 1.526(8) . ? C19 C21 1.536(7) . ? C19 C20 1.544(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 C24 1.510(8) . ? C23 C25 1.521(8) . ? C23 C26 1.538(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 C32 1.409(6) . ? C27 C28 1.412(6) . ? C27 Li1 2.694(10) . ? C28 C29 1.395(7) . ? C28 C45 1.543(7) . ? C29 C30 1.396(7) . ? C29 H29 0.9400 . ? C30 C31 1.388(6) . ? C30 C49 1.532(7) . ? C31 C32 1.398(6) . ? C31 H31 0.9400 . ? C32 C33 1.518(6) . ? C33 Li1 2.779(10) . ? C33 H33 0.9900 . ? C34 C35 1.413(7) . ? C35 C36 1.372(7) . ? C35 H35 0.9400 . ? C36 C37 1.383(8) . ? C36 H36 0.9400 . ? C37 C38 1.364(7) . ? C37 H37 0.9400 . ? C38 H38 0.9400 . ? C39 C41 1.518(7) . ? C39 C40 1.527(7) . ? C39 H39 0.9900 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 C44 1.532(7) . ? C42 C43 1.536(7) . ? C42 H42 0.9900 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? C45 C48 1.521(8) . ? C45 C46 1.523(7) . ? C45 C47 1.527(7) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C46 H46C 0.9700 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C49 C51 1.515(8) . ? C49 C52 1.519(8) . ? C49 C50 1.521(8) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C50 H50C 0.9700 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 H51C 0.9700 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 H52C 0.9700 . ? C53 C54 1.462(8) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.472(10) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.492(8) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Yb1 O2 109.64(12) . . ? O1 Yb1 N4 172.51(12) . . ? O2 Yb1 N4 74.11(12) . . ? O1 Yb1 N1 81.84(12) . . ? O2 Yb1 N1 84.21(12) . . ? N4 Yb1 N1 105.20(13) . . ? O1 Yb1 O3 79.90(11) . . ? O2 Yb1 O3 87.97(11) . . ? N4 Yb1 O3 93.92(12) . . ? N1 Yb1 O3 156.40(12) . . ? O1 Yb1 N5 117.84(12) . . ? O2 Yb1 N5 124.54(12) . . ? N4 Yb1 N5 55.85(13) . . ? N1 Yb1 N5 127.94(12) . . ? O3 Yb1 N5 74.38(12) . . ? O1 Yb1 N3 82.16(12) . . ? O2 Yb1 N3 136.85(11) . . ? N4 Yb1 N3 99.58(12) . . ? N1 Yb1 N3 55.70(12) . . ? O3 Yb1 N3 135.14(12) . . ? N5 Yb1 N3 78.49(12) . . ? O1 Yb1 C34 145.23(13) . . ? O2 Yb1 C34 97.74(12) . . ? N4 Yb1 C34 27.89(13) . . ? N1 Yb1 C34 123.00(12) . . ? O3 Yb1 C34 80.08(12) . . ? N5 Yb1 C34 28.42(13) . . ? N3 Yb1 C34 92.48(12) . . ? O1 Yb1 C7 67.43(12) . . ? O2 Yb1 C7 113.81(12) . . ? N4 Yb1 C7 117.53(13) . . ? N1 Yb1 C7 30.16(13) . . ? O3 Yb1 C7 145.08(12) . . ? N5 Yb1 C7 109.77(12) . . ? N3 Yb1 C7 31.28(11) . . ? C34 Yb1 C7 120.67(12) . . ? O1 Yb1 Li1 123.43(19) . . ? O2 Yb1 Li1 37.27(19) . . ? N4 Yb1 Li1 63.6(2) . . ? N1 Yb1 Li1 57.48(19) . . ? O3 Yb1 Li1 123.12(19) . . ? N5 Yb1 Li1 118.1(2) . . ? N3 Yb1 Li1 101.05(19) . . ? C34 Yb1 Li1 91.3(2) . . ? C7 Yb1 Li1 86.57(19) . . ? O1 Yb1 C27 118.57(12) . . ? O2 Yb1 C27 21.49(11) . . ? N4 Yb1 C27 62.66(12) . . ? N1 Yb1 C27 104.66(12) . . ? O3 Yb1 C27 71.77(12) . . ? N5 Yb1 C27 105.32(12) . . ? N3 Yb1 C27 151.08(12) . . ? C34 Yb1 C27 81.11(13) . . ? C7 Yb1 C27 134.72(12) . . ? Li1 Yb1 C27 51.36(19) . . ? O1 Yb1 C1 18.04(11) . . ? O2 Yb1 C1 111.94(11) . . ? N4 Yb1 C1 166.87(12) . . ? N1 Yb1 C1 64.96(12) . . ? O3 Yb1 C1 97.87(12) . . ? N5 Yb1 C1 122.20(12) . . ? N3 Yb1 C1 67.88(12) . . ? C34 Yb1 C1 150.21(13) . . ? C7 Yb1 C1 49.59(12) . . ? Li1 Yb1 C1 113.65(19) . . ? C27 Yb1 C1 126.83(12) . . ? C1 O1 Yb1 132.0(3) . . ? C27 O2 Li1 113.1(4) . . ? C27 O2 Yb1 121.2(3) . . ? Li1 O2 Yb1 95.8(3) . . ? C56 O3 C53 106.1(4) . . ? C56 O3 Yb1 120.7(3) . . ? C53 O3 Yb1 128.2(3) . . ? C8 N1 C7 116.5(4) . . ? C8 N1 Yb1 148.0(3) . . ? C7 N1 Yb1 95.0(2) . . ? C8 N1 Li1 77.5(3) . . ? C7 N1 Li1 159.9(3) . . ? Yb1 N1 Li1 73.8(2) . . ? C12 N2 C8 118.7(5) . . ? C12 N2 Li1 131.3(5) . . ? C8 N2 Li1 109.3(4) . . ? C16 N3 C7 117.3(4) . . ? C16 N3 C13 112.6(4) . . ? C7 N3 C13 107.9(3) . . ? C16 N3 Yb1 124.5(3) . . ? C7 N3 Yb1 86.6(2) . . ? C13 N3 Yb1 104.5(3) . . ? C34 N4 C33 121.2(4) . . ? C34 N4 Yb1 98.7(3) . . ? C33 N4 Yb1 130.6(3) . . ? C38 N5 C34 119.3(4) . . ? C38 N5 Yb1 147.5(3) . . ? C34 N5 Yb1 92.5(3) . . ? C39 N6 C42 111.0(4) . . ? C39 N6 C33 109.7(4) . . ? C42 N6 C33 116.0(4) . . ? C39 N6 Li1 113.3(4) . . ? C42 N6 Li1 106.8(4) . . ? C33 N6 Li1 99.7(4) . . ? O1 C1 C6 119.1(4) . . ? O1 C1 C2 122.1(4) . . ? C6 C1 C2 118.7(4) . . ? O1 C1 Yb1 29.93(19) . . ? C6 C1 Yb1 89.7(3) . . ? C2 C1 Yb1 151.2(3) . . ? C3 C2 C1 118.1(4) . . ? C3 C2 C19 119.6(4) . . ? C1 C2 C19 122.2(4) . . ? C4 C3 C2 123.9(5) . . ? C4 C3 H3 118.0 . . ? C2 C3 H3 118.0 . . ? C5 C4 C3 116.7(5) . . ? C5 C4 C23 120.7(5) . . ? C3 C4 C23 122.6(5) . . ? C4 C5 C6 122.4(4) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C1 120.1(4) . . ? C5 C6 C7 117.5(4) . . ? C1 C6 C7 122.1(4) . . ? N1 C7 N3 102.5(3) . . ? N1 C7 C6 112.8(4) . . ? N3 C7 C6 116.6(4) . . ? N1 C7 Yb1 54.8(2) . . ? N3 C7 Yb1 62.1(2) . . ? C6 C7 Yb1 98.5(3) . . ? N1 C7 H7 108.2 . . ? N3 C7 H7 108.2 . . ? C6 C7 H7 108.2 . . ? Yb1 C7 H7 152.9 . . ? N1 C8 N2 116.0(4) . . ? N1 C8 C9 125.8(5) . . ? N2 C8 C9 118.3(4) . . ? N1 C8 Li1 73.7(3) . . ? N2 C8 Li1 42.4(3) . . ? C9 C8 Li1 160.1(4) . . ? C10 C9 C8 120.5(5) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.7(6) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 117.2(5) . . ? C12 C11 H11 121.4 . . ? C10 C11 H11 121.4 . . ? N2 C12 C11 124.6(6) . . ? N2 C12 H12 117.7 . . ? C11 C12 H12 117.7 . . ? C14 C13 C15 108.6(4) . . ? C14 C13 N3 115.1(4) . . ? C15 C13 N3 116.6(4) . . ? C14 C13 H13 105.1 . . ? C15 C13 H13 105.1 . . ? N3 C13 H13 105.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C17 114.4(4) . . ? N3 C16 C18 115.8(4) . . ? C17 C16 C18 110.2(5) . . ? N3 C16 H16 105.1 . . ? C17 C16 H16 105.1 . . ? C18 C16 H16 105.1 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22 C19 C2 108.9(4) . . ? C22 C19 C21 110.1(5) . . ? C2 C19 C21 111.7(4) . . ? C22 C19 C20 108.5(5) . . ? C2 C19 C20 112.1(4) . . ? C21 C19 C20 105.4(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C25 107.9(5) . . ? C24 C23 C26 108.8(6) . . ? C25 C23 C26 108.5(5) . . ? C24 C23 C4 112.3(5) . . ? C25 C23 C4 110.6(5) . . ? C26 C23 C4 108.7(5) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O2 C27 C32 118.9(4) . . ? O2 C27 C28 122.1(4) . . ? C32 C27 C28 119.0(4) . . ? O2 C27 Li1 39.3(3) . . ? C32 C27 Li1 91.2(3) . . ? C28 C27 Li1 138.9(4) . . ? O2 C27 Yb1 37.26(19) . . ? C32 C27 Yb1 98.0(3) . . ? C28 C27 Yb1 131.3(3) . . ? Li1 C27 Yb1 62.2(2) . . ? C29 C28 C27 117.4(4) . . ? C29 C28 C45 121.0(4) . . ? C27 C28 C45 121.6(4) . . ? C28 C29 C30 124.5(4) . . ? C28 C29 H29 117.8 . . ? C30 C29 H29 117.8 . . ? C31 C30 C29 116.0(4) . . ? C31 C30 C49 121.7(4) . . ? C29 C30 C49 122.4(4) . . ? C30 C31 C32 122.1(4) . . ? C30 C31 H31 118.9 . . ? C32 C31 H31 118.9 . . ? C31 C32 C27 119.8(4) . . ? C31 C32 C33 118.4(4) . . ? C27 C32 C33 121.3(4) . . ? N4 C33 N6 107.1(4) . . ? N4 C33 C32 108.0(4) . . ? N6 C33 C32 112.7(4) . . ? N4 C33 Li1 79.7(3) . . ? N6 C33 Li1 47.8(3) . . ? C32 C33 Li1 85.8(3) . . ? N4 C33 H33 109.7 . . ? N6 C33 H33 109.7 . . ? C32 C33 H33 109.7 . . ? Li1 C33 H33 157.2 . . ? N4 C34 N5 111.3(4) . . ? N4 C34 C35 129.3(5) . . ? N5 C34 C35 119.4(4) . . ? N4 C34 Yb1 53.4(2) . . ? N5 C34 Yb1 59.1(2) . . ? C35 C34 Yb1 170.0(3) . . ? C36 C35 C34 119.4(5) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 C37 120.2(5) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C38 C37 C36 118.0(5) . . ? C38 C37 H37 121.0 . . ? C36 C37 H37 121.0 . . ? N5 C38 C37 123.4(5) . . ? N5 C38 H38 118.3 . . ? C37 C38 H38 118.3 . . ? N6 C39 C41 116.3(4) . . ? N6 C39 C40 111.0(4) . . ? C41 C39 C40 110.4(4) . . ? N6 C39 H39 106.1 . . ? C41 C39 H39 106.1 . . ? C40 C39 H39 106.1 . . ? 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 . . ? N6 C42 C44 117.6(4) . . ? N6 C42 C43 111.8(4) . . ? C44 C42 C43 109.6(5) . . ? N6 C42 H42 105.6 . . ? C44 C42 H42 105.6 . . ? C43 C42 H42 105.6 . . ? 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 . . ? C48 C45 C46 106.9(5) . . ? C48 C45 C47 109.9(5) . . ? C46 C45 C47 108.1(5) . . ? C48 C45 C28 109.2(4) . . ? C46 C45 C28 112.0(4) . . ? C47 C45 C28 110.6(4) . . ? 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 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C51 C49 C52 109.2(6) . . ? C51 C49 C50 109.8(6) . . ? C52 C49 C50 106.4(5) . . ? C51 C49 C30 109.2(5) . . ? C52 C49 C30 112.2(5) . . ? C50 C49 C30 110.0(4) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O3 C53 C54 106.7(5) . . ? O3 C53 H53A 110.4 . . ? C54 C53 H53A 110.4 . . ? O3 C53 H53B 110.4 . . ? C54 C53 H53B 110.4 . . ? H53A C53 H53B 108.6 . . ? C53 C54 C55 107.7(6) . . ? C53 C54 H54A 110.2 . . ? C55 C54 H54A 110.2 . . ? C53 C54 H54B 110.2 . . ? C55 C54 H54B 110.2 . . ? H54A C54 H54B 108.5 . . ? C54 C55 C56 105.0(6) . . ? C54 C55 H55A 110.7 . . ? C56 C55 H55A 110.7 . . ? C54 C55 H55B 110.7 . . ? C56 C55 H55B 110.7 . . ? H55A C55 H55B 108.8 . . ? O3 C56 C55 108.1(5) . . ? O3 C56 H56A 110.1 . . ? C55 C56 H56A 110.1 . . ? O3 C56 H56B 110.1 . . ? C55 C56 H56B 110.1 . . ? H56A C56 H56B 108.4 . . ? O2 Li1 N2 117.8(5) . . ? O2 Li1 N6 104.3(4) . . ? N2 Li1 N6 137.6(5) . . ? O2 Li1 N1 84.3(3) . . ? N2 Li1 N1 57.1(3) . . ? N6 Li1 N1 126.6(4) . . ? O2 Li1 C27 27.56(19) . . ? N2 Li1 C27 139.8(5) . . ? N6 Li1 C27 81.9(3) . . ? N1 Li1 C27 110.6(3) . . ? O2 Li1 C8 103.3(4) . . ? N2 Li1 C8 28.3(2) . . ? N6 Li1 C8 138.1(4) . . ? N1 Li1 C8 28.84(16) . . ? C27 Li1 C8 130.7(4) . . ? O2 Li1 C33 73.1(3) . . ? N2 Li1 C33 162.4(5) . . ? N6 Li1 C33 32.55(19) . . ? N1 Li1 C33 113.8(3) . . ? C27 Li1 C33 55.6(2) . . ? C8 Li1 C33 140.2(4) . . ? O2 Li1 Yb1 46.9(2) . . ? N2 Li1 Yb1 104.1(4) . . ? N6 Li1 Yb1 100.3(3) . . ? N1 Li1 Yb1 48.70(17) . . ? C27 Li1 Yb1 66.5(2) . . ? C8 Li1 Yb1 76.9(2) . . ? C33 Li1 Yb1 72.5(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.625 _refine_diff_density_min -1.034 _refine_diff_density_rms 0.082 #============================================================end data_complex4 _database_code_depnum_ccdc_archive 'CCDC 723167' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H68 N5 O2 Si2 Sm, 2(C4 H8 O), 0.5(C6 H14)' _chemical_formula_sum 'C57 H91 N5 O4 Si2 Sm' _chemical_formula_weight 1116.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 13.7307(15) _cell_length_b 16.2318(16) _cell_length_c 28.992(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.296(2) _cell_angle_gamma 90.00 _cell_volume 6288.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 16681 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.180 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 1.015 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.548 _exptl_absorpt_correction_T_max 0.784 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25627 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.50 _reflns_number_total 11635 _reflns_number_gt 9960 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+8.2476P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11635 _refine_ls_number_parameters 602 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1474 _refine_ls_wR_factor_gt 0.1393 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.125 _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 Sm1 Sm 0.322417(17) 0.610989(14) 0.163246(8) 0.03147(10) Uani 1 1 d . . . Si1 Si 0.13769(12) 0.76566(10) 0.15666(6) 0.0487(4) Uani 1 1 d . . . Si2 Si 0.23781(13) 0.74507(10) 0.07451(6) 0.0484(4) Uani 1 1 d . . . O1 O 0.2726(2) 0.52917(19) 0.21646(11) 0.0351(7) Uani 1 1 d . . . O2 O 0.4831(2) 0.5695(2) 0.16579(12) 0.0389(8) Uani 1 1 d . . . O3 O 0.4037(8) 0.2102(4) 0.1078(3) 0.170(4) Uani 1 1 d . . . O4 O 0.6670(9) 0.6755(6) 0.0088(4) 0.178(4) Uiso 1 1 d . . . N1 N 0.3844(3) 0.6661(2) 0.24518(14) 0.0323(8) Uani 1 1 d . . . N2 N 0.4332(3) 0.7467(2) 0.19217(15) 0.0373(9) Uani 1 1 d . . . N3 N 0.3270(3) 0.4788(3) 0.11747(14) 0.0375(9) Uani 1 1 d . . . N4 N 0.1722(3) 0.5282(3) 0.10603(16) 0.0440(10) Uani 1 1 d . . . N5 N 0.2177(3) 0.7195(3) 0.12764(15) 0.0400(10) Uani 1 1 d . . . C1 C 0.2783(3) 0.5144(3) 0.26105(17) 0.0330(10) Uani 1 1 d . . . C2 C 0.2263(4) 0.4463(3) 0.27571(18) 0.0365(11) Uani 1 1 d . . . C3 C 0.2432(4) 0.4284(3) 0.32327(18) 0.0383(11) Uani 1 1 d . . . H3 H 0.2102 0.3824 0.3322 0.046 Uiso 1 1 calc R . . C4 C 0.3066(4) 0.4744(3) 0.35990(18) 0.0395(11) Uani 1 1 d . A . C5 C 0.3511(4) 0.5422(3) 0.34571(18) 0.0380(11) Uani 1 1 d . . . H5 H 0.3916 0.5756 0.3689 0.046 Uiso 1 1 calc R . . C6 C 0.3385(3) 0.5642(3) 0.29734(17) 0.0333(10) Uani 1 1 d . . . C7 C 0.3880(4) 0.6370(3) 0.28742(18) 0.0364(11) Uani 1 1 d . . . H7 H 0.4262 0.6663 0.3133 0.044 Uiso 1 1 calc R . . C8 C 0.4311(4) 0.7409(3) 0.23804(17) 0.0332(10) Uani 1 1 d . . . C9 C 0.4663(4) 0.8030(3) 0.2707(2) 0.0451(13) Uani 1 1 d . . . H9 H 0.4630 0.7977 0.3025 0.054 Uiso 1 1 calc R . . C10 C 0.5059(4) 0.8721(3) 0.2551(2) 0.0478(14) Uani 1 1 d . . . H10 H 0.5304 0.9151 0.2763 0.057 Uiso 1 1 calc R . . C11 C 0.5097(4) 0.8784(3) 0.2084(2) 0.0451(13) Uani 1 1 d . . . H11 H 0.5371 0.9254 0.1973 0.054 Uiso 1 1 calc R . . C12 C 0.4731(4) 0.8151(3) 0.1780(2) 0.0430(12) Uani 1 1 d . . . H12 H 0.4759 0.8198 0.1461 0.052 Uiso 1 1 calc R . . C13 C 0.1540(4) 0.3944(3) 0.23885(19) 0.0426(12) Uani 1 1 d . . . C14 C 0.0980(4) 0.3299(4) 0.2617(2) 0.0548(15) Uani 1 1 d . . . H14A H 0.1457 0.2913 0.2799 0.082 Uiso 1 1 calc R . . H14B H 0.0511 0.3004 0.2371 0.082 Uiso 1 1 calc R . . H14C H 0.0619 0.3572 0.2824 0.082 Uiso 1 1 calc R . . C15 C 0.0731(4) 0.4491(4) 0.2074(2) 0.0573(16) Uani 1 1 d . . . H15A H 0.0362 0.4782 0.2271 0.086 Uiso 1 1 calc R . . H15B H 0.0275 0.4148 0.1848 0.086 Uiso 1 1 calc R . . H15C H 0.1048 0.4887 0.1905 0.086 Uiso 1 1 calc R . . C16 C 0.2131(5) 0.3478(3) 0.2082(2) 0.0533(15) Uani 1 1 d . . . H16A H 0.2480 0.3869 0.1924 0.080 Uiso 1 1 calc R . . H16B H 0.1674 0.3154 0.1846 0.080 Uiso 1 1 calc R . . H16C H 0.2614 0.3116 0.2281 0.080 Uiso 1 1 calc R . . C17 C 0.3244(4) 0.4481(3) 0.41224(19) 0.0475(13) Uani 1 1 d D . . C18 C 0.4220(11) 0.3998(10) 0.4254(6) 0.085(4) Uiso 0.50 1 d PD A 1 H18A H 0.4775 0.4359 0.4238 0.128 Uiso 0.50 1 calc PR A 1 H18B H 0.4198 0.3545 0.4034 0.128 Uiso 0.50 1 calc PR A 1 H18C H 0.4308 0.3784 0.4573 0.128 Uiso 0.50 1 calc PR A 1 C18' C 0.3710(13) 0.3630(9) 0.4182(6) 0.085(4) Uiso 0.50 1 d PD A 2 H18D H 0.4358 0.3647 0.4102 0.128 Uiso 0.50 1 calc PR A 2 H18E H 0.3278 0.3246 0.3974 0.128 Uiso 0.50 1 calc PR A 2 H18F H 0.3792 0.3453 0.4508 0.128 Uiso 0.50 1 calc PR A 2 C19 C 0.2474(12) 0.3871(9) 0.4216(6) 0.083(3) Uiso 0.50 1 d PD A 1 H19A H 0.2634 0.3721 0.4549 0.124 Uiso 0.50 1 calc PR A 1 H19B H 0.2480 0.3381 0.4025 0.124 Uiso 0.50 1 calc PR A 1 H19C H 0.1814 0.4120 0.4134 0.124 Uiso 0.50 1 calc PR A 1 C19' C 0.2278(11) 0.4416(11) 0.4278(6) 0.083(3) Uiso 0.50 1 d PD A 2 H19D H 0.2417 0.4304 0.4615 0.124 Uiso 0.50 1 calc PR A 2 H19E H 0.1878 0.3972 0.4107 0.124 Uiso 0.50 1 calc PR A 2 H19F H 0.1913 0.4931 0.4212 0.124 Uiso 0.50 1 calc PR A 2 C20 C 0.3307(12) 0.5216(8) 0.4449(5) 0.071(3) Uiso 0.50 1 d PD A 1 H20A H 0.2676 0.5511 0.4377 0.106 Uiso 0.50 1 calc PR A 1 H20B H 0.3839 0.5580 0.4405 0.106 Uiso 0.50 1 calc PR A 1 H20C H 0.3448 0.5029 0.4776 0.106 Uiso 0.50 1 calc PR A 1 C20' C 0.3898(11) 0.5084(8) 0.4457(5) 0.071(3) Uiso 0.50 1 d PD A 2 H20D H 0.3604 0.5629 0.4410 0.106 Uiso 0.50 1 calc PR A 2 H20E H 0.4561 0.5095 0.4393 0.106 Uiso 0.50 1 calc PR A 2 H20F H 0.3946 0.4912 0.4782 0.106 Uiso 0.50 1 calc PR A 2 C21 C 0.5411(4) 0.5128(3) 0.15475(17) 0.0342(10) Uani 1 1 d . . . C22 C 0.6486(4) 0.5186(3) 0.17078(17) 0.0366(11) Uani 1 1 d . . . C23 C 0.7056(4) 0.4560(3) 0.15954(19) 0.0415(12) Uani 1 1 d . . . H23 H 0.7753 0.4597 0.1710 0.050 Uiso 1 1 calc R . . C24 C 0.6672(4) 0.3851(3) 0.13162(18) 0.0373(11) Uani 1 1 d . . . C25 C 0.5659(4) 0.3816(3) 0.11571(17) 0.0380(11) Uani 1 1 d . . . H25 H 0.5377 0.3372 0.0964 0.046 Uiso 1 1 calc R . . C26 C 0.5020(4) 0.4419(3) 0.12703(16) 0.0339(10) Uani 1 1 d . . . C27 C 0.3973(4) 0.4299(3) 0.10981(17) 0.0373(11) Uani 1 1 d . . . H27 H 0.3769 0.3828 0.0913 0.045 Uiso 1 1 calc R . . C28 C 0.2258(4) 0.4634(3) 0.09808(18) 0.0405(12) Uani 1 1 d . . . C29 C 0.1814(5) 0.3928(4) 0.0748(2) 0.0594(17) Uani 1 1 d . . . H29 H 0.2196 0.3465 0.0707 0.071 Uiso 1 1 calc R . . C30 C 0.0792(5) 0.3940(4) 0.0582(3) 0.0677(19) Uani 1 1 d . . . H30 H 0.0469 0.3476 0.0422 0.081 Uiso 1 1 calc R . . C31 C 0.0238(4) 0.4608(4) 0.0644(2) 0.0588(16) Uani 1 1 d . . . H31 H -0.0458 0.4620 0.0521 0.071 Uiso 1 1 calc R . . C32 C 0.0729(4) 0.5263(4) 0.0890(2) 0.0527(14) Uani 1 1 d . . . H32 H 0.0351 0.5722 0.0942 0.063 Uiso 1 1 calc R . . C33 C 0.6960(4) 0.5919(3) 0.2000(2) 0.0468(13) Uani 1 1 d . . . C34 C 0.8110(4) 0.5862(4) 0.2134(3) 0.071(2) Uani 1 1 d . . . H34A H 0.8310 0.5356 0.2307 0.106 Uiso 1 1 calc R . . H34B H 0.8380 0.6330 0.2330 0.106 Uiso 1 1 calc R . . H34C H 0.8363 0.5866 0.1848 0.106 Uiso 1 1 calc R . . C35 C 0.6611(5) 0.5959(4) 0.2467(2) 0.0620(17) Uani 1 1 d . . . H35A H 0.5888 0.6012 0.2398 0.093 Uiso 1 1 calc R . . H35B H 0.6915 0.6431 0.2650 0.093 Uiso 1 1 calc R . . H35C H 0.6810 0.5459 0.2647 0.093 Uiso 1 1 calc R . . C36 C 0.6679(4) 0.6721(3) 0.1715(3) 0.0598(16) Uani 1 1 d . . . H36A H 0.6981 0.6722 0.1444 0.090 Uiso 1 1 calc R . . H36B H 0.6922 0.7191 0.1916 0.090 Uiso 1 1 calc R . . H36C H 0.5957 0.6755 0.1607 0.090 Uiso 1 1 calc R . . C37 C 0.7401(4) 0.3194(3) 0.1230(2) 0.0446(12) Uani 1 1 d . . . C38 C 0.7918(5) 0.2812(4) 0.1711(2) 0.0650(18) Uani 1 1 d . . . H38A H 0.8299 0.3233 0.1912 0.097 Uiso 1 1 calc R . . H38B H 0.8365 0.2376 0.1660 0.097 Uiso 1 1 calc R . . H38C H 0.7416 0.2586 0.1862 0.097 Uiso 1 1 calc R . . C39 C 0.8187(5) 0.3590(4) 0.0995(2) 0.0601(17) Uani 1 1 d . . . H39A H 0.7859 0.3800 0.0685 0.090 Uiso 1 1 calc R . . H39B H 0.8679 0.3180 0.0961 0.090 Uiso 1 1 calc R . . H39C H 0.8517 0.4040 0.1191 0.090 Uiso 1 1 calc R . . C40 C 0.6866(5) 0.2519(3) 0.0902(2) 0.0631(18) Uani 1 1 d . . . H40A H 0.6343 0.2280 0.1034 0.095 Uiso 1 1 calc R . . H40B H 0.7343 0.2095 0.0869 0.095 Uiso 1 1 calc R . . H40C H 0.6573 0.2753 0.0593 0.095 Uiso 1 1 calc R . . C41 C 0.1889(6) 0.8635(4) 0.1877(3) 0.079(2) Uani 1 1 d . . . H41A H 0.2566 0.8541 0.2059 0.119 Uiso 1 1 calc R . . H41B H 0.1472 0.8805 0.2089 0.119 Uiso 1 1 calc R . . H41C H 0.1892 0.9063 0.1644 0.119 Uiso 1 1 calc R . . C42 C 0.1109(5) 0.6955(4) 0.2029(2) 0.0632(17) Uani 1 1 d . . . H42A H 0.0819 0.6447 0.1882 0.095 Uiso 1 1 calc R . . H42B H 0.0642 0.7218 0.2188 0.095 Uiso 1 1 calc R . . H42C H 0.1726 0.6833 0.2259 0.095 Uiso 1 1 calc R . . C43 C 0.0133(5) 0.7937(5) 0.1164(3) 0.079(2) Uani 1 1 d . . . H43A H 0.0241 0.8312 0.0920 0.119 Uiso 1 1 calc R . . H43B H -0.0286 0.8202 0.1348 0.119 Uiso 1 1 calc R . . H43C H -0.0195 0.7442 0.1017 0.119 Uiso 1 1 calc R . . C44 C 0.2624(6) 0.8573(4) 0.0668(3) 0.075(2) Uani 1 1 d . . . H44A H 0.2021 0.8887 0.0666 0.112 Uiso 1 1 calc R . . H44B H 0.2819 0.8655 0.0370 0.112 Uiso 1 1 calc R . . H44C H 0.3157 0.8759 0.0927 0.112 Uiso 1 1 calc R . . C45 C 0.1337(6) 0.7156(5) 0.0238(2) 0.077(2) Uani 1 1 d . . . H45A H 0.1253 0.6563 0.0233 0.116 Uiso 1 1 calc R . . H45B H 0.1494 0.7333 -0.0057 0.116 Uiso 1 1 calc R . . H45C H 0.0723 0.7419 0.0272 0.116 Uiso 1 1 calc R . . C46 C 0.3493(5) 0.6862(4) 0.0649(2) 0.0622(17) Uani 1 1 d . . . H46A H 0.4066 0.6977 0.0906 0.093 Uiso 1 1 calc R . . H46B H 0.3639 0.7028 0.0351 0.093 Uiso 1 1 calc R . . H46C H 0.3348 0.6276 0.0641 0.093 Uiso 1 1 calc R . . C47 C 0.3832(10) 0.1625(6) 0.0669(3) 0.128(4) Uani 1 1 d . . . H47A H 0.4458 0.1492 0.0577 0.153 Uiso 1 1 calc R . . H47B H 0.3405 0.1934 0.0409 0.153 Uiso 1 1 calc R . . C48 C 0.3340(12) 0.0884(7) 0.0749(4) 0.161(6) Uani 1 1 d . . . H48A H 0.3692 0.0400 0.0667 0.193 Uiso 1 1 calc R . . H48B H 0.2647 0.0875 0.0564 0.193 Uiso 1 1 calc R . . C49 C 0.3377(10) 0.0903(7) 0.1260(4) 0.135(5) Uani 1 1 d . . . H49A H 0.3963 0.0606 0.1442 0.163 Uiso 1 1 calc R . . H49B H 0.2771 0.0665 0.1329 0.163 Uiso 1 1 calc R . . C50 C 0.3450(9) 0.1803(7) 0.1366(4) 0.121(4) Uani 1 1 d . . . H50A H 0.2786 0.2061 0.1291 0.145 Uiso 1 1 calc R . . H50B H 0.3764 0.1902 0.1701 0.145 Uiso 1 1 calc R . . C51 C 0.7572(11) 0.6627(8) 0.0384(5) 0.169(5) Uiso 1 1 d D . . H51A H 0.7631 0.6909 0.0688 0.203 Uiso 1 1 calc R . . H51B H 0.8124 0.6794 0.0242 0.203 Uiso 1 1 calc R . . C52 C 0.7520(10) 0.5713(7) 0.0433(5) 0.150(5) Uiso 1 1 d D . . H52A H 0.7758 0.5566 0.0768 0.180 Uiso 1 1 calc R . . H52B H 0.7972 0.5456 0.0258 0.180 Uiso 1 1 calc R . . C53 C 0.6480(11) 0.5366(9) 0.0254(5) 0.173(6) Uiso 1 1 d D . . H53A H 0.6282 0.4993 0.0481 0.208 Uiso 1 1 calc R . . H53B H 0.6396 0.5095 -0.0055 0.208 Uiso 1 1 calc R . . C54 C 0.5939(12) 0.6210(9) 0.0220(6) 0.175(6) Uiso 1 1 d . . . H54A H 0.5310 0.6203 -0.0023 0.210 Uiso 1 1 calc R . . H54B H 0.5801 0.6369 0.0525 0.210 Uiso 1 1 calc R . . C55 C -0.027(2) 0.073(2) 0.1693(12) 0.187(5) Uiso 0.50 1 d PD B 3 C56 C 0.034(2) 0.1395(19) 0.1512(11) 0.187(5) Uiso 0.50 1 d PD B 3 C57 C 0.014(2) 0.1495(18) 0.0986(11) 0.187(5) Uiso 0.50 1 d PD B 3 C58 C 0.029(2) 0.0626(18) 0.0860(11) 0.187(5) Uiso 0.50 1 d PD B 3 C59 C 0.017(2) 0.0761(15) 0.0329(10) 0.187(5) Uiso 0.50 1 d PD B 3 C60 C 0.0000 0.0000 0.0000 0.187(5) Uiso 1 2 d SD . 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.03090(15) 0.03228(15) 0.03088(15) -0.00019(10) 0.00636(10) -0.00321(10) Si1 0.0463(9) 0.0473(8) 0.0493(9) -0.0035(7) 0.0043(7) 0.0136(7) Si2 0.0537(9) 0.0478(8) 0.0397(8) 0.0050(7) 0.0027(7) -0.0002(7) O1 0.0381(18) 0.0344(17) 0.0329(18) 0.0015(14) 0.0085(14) -0.0073(15) O2 0.0314(17) 0.0406(19) 0.044(2) -0.0090(16) 0.0065(15) -0.0027(15) O3 0.305(12) 0.106(5) 0.135(7) -0.041(5) 0.125(8) -0.098(7) N1 0.035(2) 0.0282(19) 0.036(2) -0.0023(16) 0.0114(17) -0.0044(17) N2 0.042(2) 0.031(2) 0.039(2) 0.0016(17) 0.0093(19) -0.0018(18) N3 0.033(2) 0.046(2) 0.033(2) -0.0027(18) 0.0054(17) -0.0084(19) N4 0.033(2) 0.046(2) 0.050(3) 0.000(2) 0.004(2) -0.008(2) N5 0.039(2) 0.038(2) 0.039(2) -0.0039(18) 0.0022(19) 0.0063(19) C1 0.031(2) 0.034(2) 0.036(3) 0.004(2) 0.011(2) 0.006(2) C2 0.032(2) 0.033(2) 0.045(3) 0.003(2) 0.008(2) 0.001(2) C3 0.038(3) 0.039(3) 0.040(3) 0.008(2) 0.012(2) -0.002(2) C4 0.041(3) 0.040(3) 0.040(3) 0.004(2) 0.015(2) 0.003(2) C5 0.038(3) 0.038(3) 0.037(3) -0.002(2) 0.007(2) 0.002(2) C6 0.033(2) 0.031(2) 0.036(3) 0.000(2) 0.010(2) 0.004(2) C7 0.037(3) 0.032(2) 0.040(3) -0.007(2) 0.008(2) 0.001(2) C8 0.034(2) 0.028(2) 0.039(3) -0.0012(19) 0.010(2) -0.002(2) C9 0.057(3) 0.038(3) 0.045(3) -0.009(2) 0.022(3) -0.011(3) C10 0.054(3) 0.037(3) 0.052(3) -0.010(2) 0.012(3) -0.010(3) C11 0.045(3) 0.030(3) 0.060(4) 0.000(2) 0.012(3) -0.008(2) C12 0.048(3) 0.039(3) 0.044(3) 0.007(2) 0.013(2) -0.005(2) C13 0.041(3) 0.044(3) 0.041(3) 0.004(2) 0.004(2) -0.012(2) C14 0.053(3) 0.052(3) 0.057(4) 0.006(3) 0.008(3) -0.021(3) C15 0.043(3) 0.060(4) 0.065(4) 0.016(3) 0.004(3) -0.013(3) C16 0.064(4) 0.044(3) 0.053(3) -0.008(3) 0.013(3) -0.018(3) C17 0.054(3) 0.050(3) 0.038(3) 0.007(2) 0.012(3) -0.004(3) C21 0.035(2) 0.035(2) 0.032(2) 0.000(2) 0.007(2) -0.002(2) C22 0.033(2) 0.040(3) 0.037(3) -0.003(2) 0.008(2) -0.005(2) C23 0.034(3) 0.041(3) 0.049(3) 0.002(2) 0.008(2) -0.001(2) C24 0.041(3) 0.033(2) 0.041(3) 0.004(2) 0.016(2) -0.001(2) C25 0.048(3) 0.037(3) 0.031(3) -0.002(2) 0.013(2) -0.005(2) C26 0.036(3) 0.035(2) 0.032(2) -0.003(2) 0.011(2) -0.006(2) C27 0.043(3) 0.034(2) 0.034(3) -0.005(2) 0.007(2) -0.008(2) C28 0.040(3) 0.045(3) 0.036(3) -0.002(2) 0.007(2) -0.007(2) C29 0.046(3) 0.061(4) 0.067(4) -0.020(3) 0.006(3) -0.011(3) C30 0.053(4) 0.075(5) 0.069(4) -0.021(4) 0.001(3) -0.027(4) C31 0.035(3) 0.085(5) 0.052(4) 0.002(3) 0.000(3) -0.014(3) C32 0.036(3) 0.062(4) 0.056(4) 0.003(3) 0.003(3) -0.003(3) C33 0.034(3) 0.045(3) 0.057(3) -0.009(3) 0.002(2) -0.004(2) C34 0.037(3) 0.064(4) 0.101(6) -0.027(4) -0.006(3) -0.004(3) C35 0.063(4) 0.067(4) 0.050(4) -0.021(3) 0.000(3) -0.004(3) C36 0.043(3) 0.044(3) 0.089(5) -0.009(3) 0.008(3) -0.009(3) C37 0.045(3) 0.041(3) 0.053(3) 0.002(2) 0.020(3) 0.002(2) C38 0.068(4) 0.059(4) 0.069(4) 0.017(3) 0.017(3) 0.020(3) C39 0.063(4) 0.058(4) 0.071(4) -0.004(3) 0.039(4) 0.004(3) C40 0.067(4) 0.045(3) 0.081(5) -0.016(3) 0.026(4) 0.008(3) C41 0.086(5) 0.060(4) 0.095(6) -0.020(4) 0.025(5) 0.009(4) C42 0.068(4) 0.065(4) 0.062(4) 0.001(3) 0.027(3) 0.019(3) C43 0.059(4) 0.105(6) 0.069(5) 0.005(4) 0.005(4) 0.035(4) C44 0.084(5) 0.057(4) 0.079(5) 0.023(4) 0.010(4) 0.000(4) C45 0.082(5) 0.100(6) 0.041(4) -0.002(4) -0.001(3) -0.012(4) C46 0.070(4) 0.075(4) 0.045(3) 0.005(3) 0.022(3) 0.003(4) C47 0.230(14) 0.085(6) 0.086(7) -0.004(5) 0.072(8) -0.002(8) C48 0.273(18) 0.118(8) 0.124(10) -0.056(7) 0.112(11) -0.095(10) C49 0.189(13) 0.106(8) 0.133(10) -0.017(7) 0.082(10) -0.057(8) C50 0.131(9) 0.129(9) 0.110(8) -0.039(7) 0.042(7) -0.039(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O1 2.258(3) . ? Sm1 O2 2.291(3) . ? Sm1 N5 2.356(4) . ? Sm1 N1 2.497(4) . ? Sm1 N3 2.531(4) . ? Sm1 N4 2.691(4) . ? Sm1 N2 2.699(4) . ? Sm1 Si2 3.3660(16) . ? Si1 N5 1.703(4) . ? Si1 C42 1.860(6) . ? Si1 C41 1.880(7) . ? Si1 C43 1.890(7) . ? Si2 N5 1.679(5) . ? Si2 C45 1.862(7) . ? Si2 C44 1.876(7) . ? Si2 C46 1.878(7) . ? O1 C1 1.299(5) . ? O2 C21 1.305(6) . ? O3 C50 1.377(11) . ? O3 C47 1.389(11) . ? O4 C51 1.352(15) . ? O4 C54 1.454(15) . ? N1 C7 1.303(6) . ? N1 C8 1.411(6) . ? N2 C8 1.340(6) . ? N2 C12 1.343(6) . ? N3 C27 1.308(6) . ? N3 C28 1.397(6) . ? N4 C28 1.334(7) . ? N4 C32 1.339(7) . ? C1 C6 1.429(7) . ? C1 C2 1.433(7) . ? C2 C3 1.376(7) . ? C2 C13 1.533(7) . ? C3 C4 1.421(7) . ? C3 H3 0.9400 . ? C4 C5 1.366(7) . ? C4 C17 1.541(7) . ? C5 C6 1.419(7) . ? C5 H5 0.9400 . ? C6 C7 1.425(7) . ? C7 H7 0.9400 . ? C8 C9 1.391(7) . ? C9 C10 1.366(7) . ? C9 H9 0.9400 . ? C10 C11 1.372(8) . ? C10 H10 0.9400 . ? C11 C12 1.370(7) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 C16 1.534(8) . ? C13 C14 1.536(7) . ? C13 C15 1.546(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 C19' 1.500(13) . ? C17 C20 1.514(12) . ? C17 C18' 1.515(13) . ? C17 C20' 1.518(12) . ? C17 C19 1.519(13) . ? C17 C18 1.522(13) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C18' H18D 0.9700 . ? C18' H18E 0.9700 . ? C18' H18F 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C19' H19D 0.9700 . ? C19' H19E 0.9700 . ? C19' H19F 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C20' H20D 0.9700 . ? C20' H20E 0.9700 . ? C20' H20F 0.9700 . ? C21 C26 1.435(6) . ? C21 C22 1.445(6) . ? C22 C23 1.367(7) . ? C22 C33 1.518(7) . ? C23 C24 1.436(7) . ? C23 H23 0.9400 . ? C24 C25 1.362(7) . ? C24 C37 1.522(7) . ? C25 C26 1.402(7) . ? C25 H25 0.9400 . ? C26 C27 1.422(7) . ? C27 H27 0.9400 . ? C28 C29 1.396(7) . ? C29 C30 1.374(9) . ? C29 H29 0.9400 . ? C30 C31 1.360(9) . ? C30 H30 0.9400 . ? C31 C32 1.369(8) . ? C31 H31 0.9400 . ? C32 H32 0.9400 . ? C33 C35 1.537(9) . ? C33 C34 1.539(7) . ? C33 C36 1.542(8) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C37 C40 1.525(8) . ? C37 C38 1.541(8) . ? C37 C39 1.544(8) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 H45C 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C46 H46C 0.9700 . ? C47 C48 1.424(13) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 C49 1.471(14) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.492(13) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.493(13) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 C53 1.512(13) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.550(16) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.535(18) . ? C56 C57 1.495(18) . ? C57 C58 1.482(18) . ? C58 C59 1.526(18) . ? C59 C60 1.546(18) . ? C60 C59 1.546(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 O1 Sm1 O2 104.23(12) . . ? O1 Sm1 N5 119.25(14) . . ? O2 Sm1 N5 136.04(14) . . ? O1 Sm1 N1 69.60(12) . . ? O2 Sm1 N1 87.68(12) . . ? N5 Sm1 N1 100.91(13) . . ? O1 Sm1 N3 84.70(12) . . ? O2 Sm1 N3 68.16(12) . . ? N5 Sm1 N3 119.34(14) . . ? N1 Sm1 N3 139.30(13) . . ? O1 Sm1 N4 79.49(13) . . ? O2 Sm1 N4 117.97(13) . . ? N5 Sm1 N4 78.41(14) . . ? N1 Sm1 N4 144.16(13) . . ? N3 Sm1 N4 50.30(13) . . ? O1 Sm1 N2 120.37(12) . . ? O2 Sm1 N2 76.12(12) . . ? N5 Sm1 N2 76.69(14) . . ? N1 Sm1 N2 50.77(12) . . ? N3 Sm1 N2 140.77(13) . . ? N4 Sm1 N2 153.74(13) . . ? O1 Sm1 Si2 142.85(9) . . ? O2 Sm1 Si2 112.03(9) . . ? N5 Sm1 Si2 27.54(11) . . ? N1 Sm1 Si2 118.53(9) . . ? N3 Sm1 Si2 101.13(10) . . ? N4 Sm1 Si2 76.75(10) . . ? N2 Sm1 Si2 77.33(9) . . ? N5 Si1 C42 110.1(2) . . ? N5 Si1 C41 113.3(3) . . ? C42 Si1 C41 106.6(3) . . ? N5 Si1 C43 113.3(3) . . ? C42 Si1 C43 107.0(3) . . ? C41 Si1 C43 106.1(4) . . ? N5 Si2 C45 113.8(3) . . ? N5 Si2 C44 115.0(3) . . ? C45 Si2 C44 106.3(3) . . ? N5 Si2 C46 108.8(2) . . ? C45 Si2 C46 104.8(3) . . ? C44 Si2 C46 107.6(3) . . ? N5 Si2 Sm1 40.47(14) . . ? C45 Si2 Sm1 120.3(2) . . ? C44 Si2 Sm1 132.8(2) . . ? C46 Si2 Sm1 68.57(19) . . ? C1 O1 Sm1 146.1(3) . . ? C21 O2 Sm1 146.9(3) . . ? C50 O3 C47 106.8(8) . . ? C51 O4 C54 109.0(12) . . ? C7 N1 C8 122.0(4) . . ? C7 N1 Sm1 134.0(3) . . ? C8 N1 Sm1 103.6(3) . . ? C8 N2 C12 117.6(4) . . ? C8 N2 Sm1 96.5(3) . . ? C12 N2 Sm1 145.1(4) . . ? C27 N3 C28 121.8(4) . . ? C27 N3 Sm1 135.4(3) . . ? C28 N3 Sm1 102.8(3) . . ? C28 N4 C32 118.3(5) . . ? C28 N4 Sm1 97.2(3) . . ? C32 N4 Sm1 144.1(4) . . ? Si2 N5 Si1 127.2(3) . . ? Si2 N5 Sm1 112.0(2) . . ? Si1 N5 Sm1 120.7(2) . . ? O1 C1 C6 121.4(4) . . ? O1 C1 C2 121.1(4) . . ? C6 C1 C2 117.5(4) . . ? C3 C2 C1 118.7(5) . . ? C3 C2 C13 121.0(4) . . ? C1 C2 C13 120.3(4) . . ? C2 C3 C4 124.8(5) . . ? C2 C3 H3 117.6 . . ? C4 C3 H3 117.6 . . ? C5 C4 C3 115.9(5) . . ? C5 C4 C17 122.6(5) . . ? C3 C4 C17 121.4(4) . . ? C4 C5 C6 122.7(5) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C7 117.0(4) . . ? C5 C6 C1 120.2(4) . . ? C7 C6 C1 122.8(4) . . ? N1 C7 C6 125.0(5) . . ? N1 C7 H7 117.5 . . ? C6 C7 H7 117.5 . . ? N2 C8 C9 122.8(4) . . ? N2 C8 N1 108.6(4) . . ? C9 C8 N1 128.5(5) . . ? C10 C9 C8 118.2(5) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? C9 C10 C11 119.7(5) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 119.0(5) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? N2 C12 C11 122.7(5) . . ? N2 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C2 C13 C16 109.4(4) . . ? C2 C13 C14 112.5(4) . . ? C16 C13 C14 107.3(5) . . ? C2 C13 C15 110.9(4) . . ? C16 C13 C15 110.2(5) . . ? C14 C13 C15 106.4(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19' C17 C20 78.1(9) . . ? C19' C17 C18' 106.4(10) . . ? C20 C17 C18' 133.2(10) . . ? C19' C17 C20' 106.7(9) . . ? C20 C17 C20' 31.9(7) . . ? C18' C17 C20' 110.0(10) . . ? C19' C17 C19 36.8(8) . . ? C20 C17 C19 110.1(9) . . ? C18' C17 C19 71.3(9) . . ? C20' C17 C19 129.8(10) . . ? C19' C17 C18 132.6(10) . . ? C20 C17 C18 109.2(10) . . ? C18' C17 C18 34.8(8) . . ? C20' C17 C18 79.3(9) . . ? C19 C17 C18 103.2(10) . . ? C19' C17 C4 111.3(8) . . ? C20 C17 C4 111.8(7) . . ? C18' C17 C4 109.4(8) . . ? C20' C17 C4 112.8(7) . . ? C19 C17 C4 113.5(8) . . ? C18 C17 C4 108.7(8) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? C17 C18' H18D 109.5 . . ? C17 C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C17 C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? C17 C19' H19D 109.5 . . ? C17 C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? C17 C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? C17 C20' H20D 109.5 . . ? C17 C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? C17 C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? O2 C21 C26 122.1(4) . . ? O2 C21 C22 120.8(4) . . ? C26 C21 C22 117.1(4) . . ? C23 C22 C21 118.3(5) . . ? C23 C22 C33 121.3(5) . . ? C21 C22 C33 120.4(4) . . ? C22 C23 C24 125.0(5) . . ? C22 C23 H23 117.5 . . ? C24 C23 H23 117.5 . . ? C25 C24 C23 116.0(5) . . ? C25 C24 C37 125.1(5) . . ? C23 C24 C37 118.9(5) . . ? C24 C25 C26 122.5(5) . . ? C24 C25 H25 118.8 . . ? C26 C25 H25 118.8 . . ? C25 C26 C27 117.3(4) . . ? C25 C26 C21 121.1(4) . . ? C27 C26 C21 121.6(4) . . ? N3 C27 C26 125.7(4) . . ? N3 C27 H27 117.1 . . ? C26 C27 H27 117.1 . . ? N4 C28 C29 122.2(5) . . ? N4 C28 N3 109.0(4) . . ? C29 C28 N3 128.7(5) . . ? C30 C29 C28 117.0(6) . . ? C30 C29 H29 121.5 . . ? C28 C29 H29 121.5 . . ? C31 C30 C29 121.5(6) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C30 C31 C32 117.7(6) . . ? C30 C31 H31 121.1 . . ? C32 C31 H31 121.1 . . ? N4 C32 C31 123.2(6) . . ? N4 C32 H32 118.4 . . ? C31 C32 H32 118.4 . . ? C22 C33 C35 110.1(5) . . ? C22 C33 C34 112.2(5) . . ? C35 C33 C34 106.9(5) . . ? C22 C33 C36 109.9(5) . . ? C35 C33 C36 110.2(5) . . ? C34 C33 C36 107.5(5) . . ? 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 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C24 C37 C40 111.4(5) . . ? C24 C37 C38 108.6(5) . . ? C40 C37 C38 109.3(5) . . ? C24 C37 C39 109.5(4) . . ? C40 C37 C39 107.9(5) . . ? C38 C37 C39 110.1(5) . . ? 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 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si1 C41 H41A 109.5 . . ? Si1 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si1 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si1 C42 H42A 109.5 . . ? Si1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si1 C43 H43A 109.5 . . ? Si1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si2 C44 H44A 109.5 . . ? Si2 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si2 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si2 C45 H45A 109.5 . . ? Si2 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si2 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si2 C46 H46A 109.5 . . ? Si2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O3 C47 C48 110.0(8) . . ? O3 C47 H47A 109.7 . . ? C48 C47 H47A 109.7 . . ? O3 C47 H47B 109.7 . . ? C48 C47 H47B 109.7 . . ? H47A C47 H47B 108.2 . . ? C47 C48 C49 103.8(9) . . ? C47 C48 H48A 111.0 . . ? C49 C48 H48A 111.0 . . ? C47 C48 H48B 111.0 . . ? C49 C48 H48B 111.0 . . ? H48A C48 H48B 109.0 . . ? C48 C49 C50 102.3(9) . . ? C48 C49 H49A 111.3 . . ? C50 C49 H49A 111.3 . . ? C48 C49 H49B 111.3 . . ? C50 C49 H49B 111.3 . . ? H49A C49 H49B 109.2 . . ? O3 C50 C49 103.9(8) . . ? O3 C50 H50A 111.0 . . ? C49 C50 H50A 111.0 . . ? O3 C50 H50B 111.0 . . ? C49 C50 H50B 111.0 . . ? H50A C50 H50B 109.0 . . ? O4 C51 C52 99.0(11) . . ? O4 C51 H51A 112.0 . . ? C52 C51 H51A 112.0 . . ? O4 C51 H51B 112.0 . . ? C52 C51 H51B 112.0 . . ? H51A C51 H51B 109.7 . . ? C51 C52 C53 113.5(12) . . ? C51 C52 H52A 108.9 . . ? C53 C52 H52A 108.9 . . ? C51 C52 H52B 108.9 . . ? C53 C52 H52B 108.9 . . ? H52A C52 H52B 107.7 . . ? C52 C53 C54 95.4(11) . . ? C52 C53 H53A 112.7 . . ? C54 C53 H53A 112.7 . . ? C52 C53 H53B 112.7 . . ? C54 C53 H53B 112.7 . . ? H53A C53 H53B 110.1 . . ? O4 C54 C53 101.8(12) . . ? O4 C54 H54A 111.4 . . ? C53 C54 H54A 111.4 . . ? O4 C54 H54B 111.4 . . ? C53 C54 H54B 111.4 . . ? H54A C54 H54B 109.3 . . ? C57 C56 C55 116(3) . . ? C58 C57 C56 98(3) . . ? C57 C58 C59 97(2) . . ? C58 C59 C60 118(2) . . ? C59 C60 C59 180(3) 3 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Sm1 Si2 N5 38.7(3) . . . . ? O2 Sm1 Si2 N5 -154.6(2) . . . . ? N1 Sm1 Si2 N5 -54.8(2) . . . . ? N3 Sm1 Si2 N5 134.6(2) . . . . ? N4 Sm1 Si2 N5 90.3(2) . . . . ? N2 Sm1 Si2 N5 -85.5(2) . . . . ? O1 Sm1 Si2 C45 -53.3(3) . . . . ? O2 Sm1 Si2 C45 113.5(3) . . . . ? N5 Sm1 Si2 C45 -91.9(4) . . . . ? N1 Sm1 Si2 C45 -146.7(3) . . . . ? N3 Sm1 Si2 C45 42.7(3) . . . . ? N4 Sm1 Si2 C45 -1.6(3) . . . . ? N2 Sm1 Si2 C45 -177.4(3) . . . . ? O1 Sm1 Si2 C44 117.2(4) . . . . ? O2 Sm1 Si2 C44 -76.1(4) . . . . ? N5 Sm1 Si2 C44 78.5(4) . . . . ? N1 Sm1 Si2 C44 23.7(4) . . . . ? N3 Sm1 Si2 C44 -146.8(4) . . . . ? N4 Sm1 Si2 C44 168.8(4) . . . . ? N2 Sm1 Si2 C44 -6.9(4) . . . . ? O1 Sm1 Si2 C46 -148.3(3) . . . . ? O2 Sm1 Si2 C46 18.4(3) . . . . ? N5 Sm1 Si2 C46 173.0(3) . . . . ? N1 Sm1 Si2 C46 118.2(3) . . . . ? N3 Sm1 Si2 C46 -52.4(3) . . . . ? N4 Sm1 Si2 C46 -96.7(3) . . . . ? N2 Sm1 Si2 C46 87.5(3) . . . . ? O2 Sm1 O1 C1 76.3(5) . . . . ? N5 Sm1 O1 C1 -97.0(5) . . . . ? N1 Sm1 O1 C1 -5.7(5) . . . . ? N3 Sm1 O1 C1 142.2(5) . . . . ? N4 Sm1 O1 C1 -167.2(5) . . . . ? N2 Sm1 O1 C1 -5.7(6) . . . . ? Si2 Sm1 O1 C1 -116.3(5) . . . . ? O1 Sm1 O2 C21 73.0(6) . . . . ? N5 Sm1 O2 C21 -115.4(6) . . . . ? N1 Sm1 O2 C21 141.3(6) . . . . ? N3 Sm1 O2 C21 -5.2(6) . . . . ? N4 Sm1 O2 C21 -12.5(6) . . . . ? N2 Sm1 O2 C21 -168.7(6) . . . . ? Si2 Sm1 O2 C21 -98.8(6) . . . . ? O1 Sm1 N1 C7 11.1(4) . . . . ? O2 Sm1 N1 C7 -95.1(4) . . . . ? N5 Sm1 N1 C7 128.4(4) . . . . ? N3 Sm1 N1 C7 -43.2(5) . . . . ? N4 Sm1 N1 C7 43.1(5) . . . . ? N2 Sm1 N1 C7 -169.0(5) . . . . ? Si2 Sm1 N1 C7 151.0(4) . . . . ? O1 Sm1 N1 C8 -175.7(3) . . . . ? O2 Sm1 N1 C8 78.2(3) . . . . ? N5 Sm1 N1 C8 -58.4(3) . . . . ? N3 Sm1 N1 C8 130.0(3) . . . . ? N4 Sm1 N1 C8 -143.6(3) . . . . ? N2 Sm1 N1 C8 4.2(3) . . . . ? Si2 Sm1 N1 C8 -35.8(3) . . . . ? O1 Sm1 N2 C8 -4.3(3) . . . . ? O2 Sm1 N2 C8 -102.9(3) . . . . ? N5 Sm1 N2 C8 112.0(3) . . . . ? N1 Sm1 N2 C8 -4.4(3) . . . . ? N3 Sm1 N2 C8 -127.6(3) . . . . ? N4 Sm1 N2 C8 130.9(3) . . . . ? Si2 Sm1 N2 C8 140.3(3) . . . . ? O1 Sm1 N2 C12 -172.2(6) . . . . ? O2 Sm1 N2 C12 89.3(6) . . . . ? N5 Sm1 N2 C12 -55.9(6) . . . . ? N1 Sm1 N2 C12 -172.2(7) . . . . ? N3 Sm1 N2 C12 64.6(7) . . . . ? N4 Sm1 N2 C12 -37.0(7) . . . . ? Si2 Sm1 N2 C12 -27.6(6) . . . . ? O1 Sm1 N3 C27 -104.6(5) . . . . ? O2 Sm1 N3 C27 3.0(4) . . . . ? N5 Sm1 N3 C27 134.7(5) . . . . ? N1 Sm1 N3 C27 -54.8(5) . . . . ? N4 Sm1 N3 C27 174.7(5) . . . . ? N2 Sm1 N3 C27 29.0(6) . . . . ? Si2 Sm1 N3 C27 112.5(5) . . . . ? O1 Sm1 N3 C28 75.7(3) . . . . ? O2 Sm1 N3 C28 -176.7(3) . . . . ? N5 Sm1 N3 C28 -45.0(3) . . . . ? N1 Sm1 N3 C28 125.5(3) . . . . ? N4 Sm1 N3 C28 -5.0(3) . . . . ? N2 Sm1 N3 C28 -150.7(3) . . . . ? Si2 Sm1 N3 C28 -67.2(3) . . . . ? O1 Sm1 N4 C28 -86.6(3) . . . . ? O2 Sm1 N4 C28 14.0(4) . . . . ? N5 Sm1 N4 C28 150.3(3) . . . . ? N1 Sm1 N4 C28 -117.1(3) . . . . ? N3 Sm1 N4 C28 5.2(3) . . . . ? N2 Sm1 N4 C28 131.5(3) . . . . ? Si2 Sm1 N4 C28 122.1(3) . . . . ? O1 Sm1 N4 C32 84.4(7) . . . . ? O2 Sm1 N4 C32 -175.0(6) . . . . ? N5 Sm1 N4 C32 -38.7(6) . . . . ? N1 Sm1 N4 C32 54.0(7) . . . . ? N3 Sm1 N4 C32 176.2(7) . . . . ? N2 Sm1 N4 C32 -57.4(8) . . . . ? Si2 Sm1 N4 C32 -66.9(6) . . . . ? C45 Si2 N5 Si1 -73.6(4) . . . . ? C44 Si2 N5 Si1 49.4(4) . . . . ? C46 Si2 N5 Si1 170.0(3) . . . . ? Sm1 Si2 N5 Si1 176.9(5) . . . . ? C45 Si2 N5 Sm1 109.5(3) . . . . ? C44 Si2 N5 Sm1 -127.5(3) . . . . ? C46 Si2 N5 Sm1 -6.9(3) . . . . ? C42 Si1 N5 Si2 161.1(3) . . . . ? C41 Si1 N5 Si2 -79.7(4) . . . . ? C43 Si1 N5 Si2 41.3(5) . . . . ? C42 Si1 N5 Sm1 -22.3(4) . . . . ? C41 Si1 N5 Sm1 97.0(4) . . . . ? C43 Si1 N5 Sm1 -142.1(3) . . . . ? O1 Sm1 N5 Si2 -154.37(19) . . . . ? O2 Sm1 N5 Si2 35.0(3) . . . . ? N1 Sm1 N5 Si2 133.0(2) . . . . ? N3 Sm1 N5 Si2 -53.2(3) . . . . ? N4 Sm1 N5 Si2 -83.5(2) . . . . ? N2 Sm1 N5 Si2 88.1(2) . . . . ? O1 Sm1 N5 Si1 28.5(3) . . . . ? O2 Sm1 N5 Si1 -142.2(2) . . . . ? N1 Sm1 N5 Si1 -44.1(3) . . . . ? N3 Sm1 N5 Si1 129.7(2) . . . . ? N4 Sm1 N5 Si1 99.3(3) . . . . ? N2 Sm1 N5 Si1 -89.1(2) . . . . ? Si2 Sm1 N5 Si1 -177.1(4) . . . . ? Sm1 O1 C1 C6 -0.5(8) . . . . ? Sm1 O1 C1 C2 -179.0(4) . . . . ? O1 C1 C2 C3 173.3(4) . . . . ? C6 C1 C2 C3 -5.2(7) . . . . ? O1 C1 C2 C13 -6.2(7) . . . . ? C6 C1 C2 C13 175.2(4) . . . . ? C1 C2 C3 C4 2.2(8) . . . . ? C13 C2 C3 C4 -178.3(5) . . . . ? C2 C3 C4 C5 1.7(8) . . . . ? C2 C3 C4 C17 -177.6(5) . . . . ? C3 C4 C5 C6 -2.5(7) . . . . ? C17 C4 C5 C6 176.9(5) . . . . ? C4 C5 C6 C7 179.2(5) . . . . ? C4 C5 C6 C1 -0.7(7) . . . . ? O1 C1 C6 C5 -174.0(4) . . . . ? C2 C1 C6 C5 4.6(7) . . . . ? O1 C1 C6 C7 6.1(7) . . . . ? C2 C1 C6 C7 -175.3(4) . . . . ? C8 N1 C7 C6 176.6(4) . . . . ? Sm1 N1 C7 C6 -11.1(7) . . . . ? C5 C6 C7 N1 -179.9(4) . . . . ? C1 C6 C7 N1 0.0(8) . . . . ? C12 N2 C8 C9 1.3(7) . . . . ? Sm1 N2 C8 C9 -170.9(4) . . . . ? C12 N2 C8 N1 178.5(4) . . . . ? Sm1 N2 C8 N1 6.3(4) . . . . ? C7 N1 C8 N2 167.3(4) . . . . ? Sm1 N1 C8 N2 -7.0(4) . . . . ? C7 N1 C8 C9 -15.7(8) . . . . ? Sm1 N1 C8 C9 170.0(5) . . . . ? N2 C8 C9 C10 -1.0(8) . . . . ? N1 C8 C9 C10 -177.6(5) . . . . ? C8 C9 C10 C11 0.1(9) . . . . ? C9 C10 C11 C12 0.4(9) . . . . ? C8 N2 C12 C11 -0.8(8) . . . . ? Sm1 N2 C12 C11 165.5(4) . . . . ? C10 C11 C12 N2 0.0(9) . . . . ? C3 C2 C13 C16 -113.1(5) . . . . ? C1 C2 C13 C16 66.5(6) . . . . ? C3 C2 C13 C14 6.1(7) . . . . ? C1 C2 C13 C14 -174.4(5) . . . . ? C3 C2 C13 C15 125.1(5) . . . . ? C1 C2 C13 C15 -55.3(6) . . . . ? C5 C4 C17 C19' 123.9(9) . . . . ? C3 C4 C17 C19' -56.8(9) . . . . ? C5 C4 C17 C20 38.6(9) . . . . ? C3 C4 C17 C20 -142.1(8) . . . . ? C5 C4 C17 C18' -118.8(9) . . . . ? C3 C4 C17 C18' 60.5(10) . . . . ? C5 C4 C17 C20' 4.0(9) . . . . ? C3 C4 C17 C20' -176.7(8) . . . . ? C5 C4 C17 C19 163.8(8) . . . . ? C3 C4 C17 C19 -16.9(10) . . . . ? C5 C4 C17 C18 -82.0(9) . . . . ? C3 C4 C17 C18 97.3(9) . . . . ? Sm1 O2 C21 C26 4.7(9) . . . . ? Sm1 O2 C21 C22 -174.4(4) . . . . ? O2 C21 C22 C23 177.8(4) . . . . ? C26 C21 C22 C23 -1.4(7) . . . . ? O2 C21 C22 C33 -1.2(7) . . . . ? C26 C21 C22 C33 179.6(5) . . . . ? C21 C22 C23 C24 1.9(8) . . . . ? C33 C22 C23 C24 -179.1(5) . . . . ? C22 C23 C24 C25 -0.1(8) . . . . ? C22 C23 C24 C37 -178.6(5) . . . . ? C23 C24 C25 C26 -2.1(7) . . . . ? C37 C24 C25 C26 176.3(5) . . . . ? C24 C25 C26 C27 -177.7(5) . . . . ? C24 C25 C26 C21 2.5(7) . . . . ? O2 C21 C26 C25 -179.8(4) . . . . ? C22 C21 C26 C25 -0.7(7) . . . . ? O2 C21 C26 C27 0.4(7) . . . . ? C22 C21 C26 C27 179.5(4) . . . . ? C28 N3 C27 C26 178.3(5) . . . . ? Sm1 N3 C27 C26 -1.4(8) . . . . ? C25 C26 C27 N3 178.9(5) . . . . ? C21 C26 C27 N3 -1.3(8) . . . . ? C32 N4 C28 C29 -3.2(8) . . . . ? Sm1 N4 C28 C29 170.8(5) . . . . ? C32 N4 C28 N3 178.3(5) . . . . ? Sm1 N4 C28 N3 -7.7(4) . . . . ? C27 N3 C28 N4 -171.5(4) . . . . ? Sm1 N3 C28 N4 8.3(5) . . . . ? C27 N3 C28 C29 10.2(9) . . . . ? Sm1 N3 C28 C29 -170.1(5) . . . . ? N4 C28 C29 C30 3.0(10) . . . . ? N3 C28 C29 C30 -178.8(6) . . . . ? C28 C29 C30 C31 -0.4(11) . . . . ? C29 C30 C31 C32 -1.9(11) . . . . ? C28 N4 C32 C31 0.8(9) . . . . ? Sm1 N4 C32 C31 -169.1(5) . . . . ? C30 C31 C32 N4 1.7(10) . . . . ? C23 C22 C33 C35 -117.8(6) . . . . ? C21 C22 C33 C35 61.2(7) . . . . ? C23 C22 C33 C34 1.1(8) . . . . ? C21 C22 C33 C34 -179.9(5) . . . . ? C23 C22 C33 C36 120.6(6) . . . . ? C21 C22 C33 C36 -60.4(7) . . . . ? C25 C24 C37 C40 5.4(7) . . . . ? C23 C24 C37 C40 -176.3(5) . . . . ? C25 C24 C37 C38 -115.1(6) . . . . ? C23 C24 C37 C38 63.2(6) . . . . ? C25 C24 C37 C39 124.7(6) . . . . ? C23 C24 C37 C39 -57.0(7) . . . . ? C50 O3 C47 C48 -16.6(16) . . . . ? O3 C47 C48 C49 -6.9(17) . . . . ? C47 C48 C49 C50 25.5(15) . . . . ? C47 O3 C50 C49 32.6(14) . . . . ? C48 C49 C50 O3 -36.1(14) . . . . ? C54 O4 C51 C52 38.4(15) . . . . ? O4 C51 C52 C53 -13.9(16) . . . . ? C51 C52 C53 C54 -13.4(16) . . . . ? C51 O4 C54 C53 -49.7(15) . . . . ? C52 C53 C54 O4 33.8(15) . . . . ? C55 C56 C57 C58 -53(4) . . . . ? C56 C57 C58 C59 -175(3) . . . . ? C57 C58 C59 C60 -165(2) . . . . ? C58 C59 C60 C59 -98(3) . . . 3 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.956 _refine_diff_density_min -0.873 _refine_diff_density_rms 0.098 #============================================================end data_complex5 _database_code_depnum_ccdc_archive 'CCDC 723168' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H68 N5 Nd O2 Si2, 2(C4 H8 O), 0.5(C6 H14)' _chemical_formula_sum 'C57 H91 N5 Nd O4 Si2' _chemical_formula_weight 1110.77 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 13.7390(12) _cell_length_b 16.2325(13) _cell_length_c 29.038(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.3660(10) _cell_angle_gamma 90.00 _cell_volume 6300.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 17251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 0.905 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.549 _exptl_absorpt_correction_T_max 0.705 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43880 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.50 _reflns_number_total 11622 _reflns_number_gt 10437 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0726P)^2^+7.0645P] 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 constr _refine_ls_number_reflns 11622 _refine_ls_number_parameters 602 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1330 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.073 _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 Nd1 Nd 0.322670(13) 0.610870(12) 0.163208(6) 0.02845(9) Uani 1 1 d . . . Si1 Si 0.13723(9) 0.76645(8) 0.15570(5) 0.0462(3) Uani 1 1 d . . . Si2 Si 0.23797(10) 0.74607(8) 0.07378(4) 0.0459(3) Uani 1 1 d . . . O1 O 0.27216(19) 0.52975(16) 0.21739(9) 0.0335(6) Uani 1 1 d . . . O2 O 0.48413(19) 0.56880(17) 0.16455(10) 0.0370(6) Uani 1 1 d . . . O3 O 0.4050(6) 0.2103(4) 0.1093(2) 0.140(3) Uani 1 1 d . . . O4 O 0.6677(6) 0.6752(5) 0.0085(3) 0.152(3) Uiso 1 1 d . . . N1 N 0.3854(2) 0.66600(19) 0.24650(11) 0.0317(7) Uani 1 1 d . . . N2 N 0.4344(2) 0.74725(19) 0.19339(11) 0.0340(7) Uani 1 1 d . . . N3 N 0.3283(2) 0.4768(2) 0.11706(11) 0.0351(7) Uani 1 1 d . . . N4 N 0.1727(2) 0.5259(2) 0.10495(12) 0.0422(8) Uani 1 1 d . . . N5 N 0.2173(2) 0.7208(2) 0.12684(12) 0.0382(8) Uani 1 1 d . . . C1 C 0.2785(3) 0.5143(2) 0.26189(13) 0.0304(8) Uani 1 1 d . . . C2 C 0.2261(3) 0.4464(2) 0.27641(14) 0.0332(8) Uani 1 1 d . . . C3 C 0.2434(3) 0.4283(3) 0.32391(14) 0.0369(9) Uani 1 1 d . . . H3 H 0.2102 0.3825 0.3329 0.044 Uiso 1 1 calc R . . C4 C 0.3074(3) 0.4737(2) 0.36024(14) 0.0361(9) Uani 1 1 d . A . C5 C 0.3523(3) 0.5412(2) 0.34649(14) 0.0370(9) Uani 1 1 d . . . H5 H 0.3935 0.5739 0.3698 0.044 Uiso 1 1 calc R . . C6 C 0.3391(3) 0.5641(2) 0.29829(13) 0.0312(8) Uani 1 1 d . . . C7 C 0.3888(3) 0.6367(2) 0.28861(13) 0.0318(8) Uani 1 1 d . . . H7 H 0.4271 0.6658 0.3146 0.038 Uiso 1 1 calc R . . C8 C 0.4318(3) 0.7409(2) 0.23947(13) 0.0313(8) Uani 1 1 d . . . C9 C 0.4669(3) 0.8032(3) 0.27185(15) 0.0420(10) Uani 1 1 d . . . H9 H 0.4636 0.7978 0.3037 0.050 Uiso 1 1 calc R . . C10 C 0.5063(4) 0.8724(3) 0.25663(17) 0.0472(11) Uani 1 1 d . . . H10 H 0.5309 0.9152 0.2779 0.057 Uiso 1 1 calc R . . C11 C 0.5098(3) 0.8790(2) 0.20972(17) 0.0437(10) Uani 1 1 d . . . H11 H 0.5366 0.9262 0.1986 0.052 Uiso 1 1 calc R . . C12 C 0.4734(3) 0.8156(3) 0.17973(15) 0.0416(9) Uani 1 1 d . . . H12 H 0.4762 0.8204 0.1478 0.050 Uiso 1 1 calc R . . C13 C 0.1542(3) 0.3944(2) 0.23948(15) 0.0397(9) Uani 1 1 d . . . C14 C 0.0972(3) 0.3304(3) 0.26258(17) 0.0515(11) Uani 1 1 d . . . H14A H 0.1445 0.2922 0.2814 0.077 Uiso 1 1 calc R . . H14B H 0.0508 0.3003 0.2381 0.077 Uiso 1 1 calc R . . H14C H 0.0604 0.3584 0.2827 0.077 Uiso 1 1 calc R . . C15 C 0.0737(3) 0.4501(3) 0.20825(18) 0.0560(12) Uani 1 1 d . . . H15A H 0.0372 0.4792 0.2281 0.084 Uiso 1 1 calc R . . H15B H 0.0277 0.4164 0.1855 0.084 Uiso 1 1 calc R . . H15C H 0.1058 0.4896 0.1915 0.084 Uiso 1 1 calc R . . C16 C 0.2126(4) 0.3481(3) 0.20875(16) 0.0508(11) Uani 1 1 d . . . H16A H 0.2492 0.3872 0.1939 0.076 Uiso 1 1 calc R . . H16B H 0.1665 0.3174 0.1845 0.076 Uiso 1 1 calc R . . H16C H 0.2593 0.3104 0.2283 0.076 Uiso 1 1 calc R . . C17 C 0.3257(3) 0.4468(3) 0.41264(14) 0.0455(10) Uani 1 1 d D . . C18 C 0.4225(9) 0.3959(7) 0.4246(5) 0.080(3) Uiso 0.564(7) 1 d PD A 1 H18A H 0.4788 0.4307 0.4226 0.120 Uiso 0.564(7) 1 calc PR A 1 H18B H 0.4176 0.3506 0.4024 0.120 Uiso 0.564(7) 1 calc PR A 1 H18C H 0.4323 0.3742 0.4565 0.120 Uiso 0.564(7) 1 calc PR A 1 C18' C 0.3727(13) 0.3616(9) 0.4188(6) 0.080(3) Uiso 0.436(7) 1 d PD A 2 H18D H 0.4261 0.3588 0.4021 0.120 Uiso 0.436(7) 1 calc PR A 2 H18E H 0.3223 0.3206 0.4061 0.120 Uiso 0.436(7) 1 calc PR A 2 H18F H 0.3997 0.3510 0.4522 0.120 Uiso 0.436(7) 1 calc PR A 2 C19 C 0.2442(8) 0.3896(7) 0.4224(4) 0.072(2) Uiso 0.564(7) 1 d PD A 1 H19A H 0.2595 0.3751 0.4557 0.108 Uiso 0.564(7) 1 calc PR A 1 H19B H 0.2414 0.3400 0.4036 0.108 Uiso 0.564(7) 1 calc PR A 1 H19C H 0.1801 0.4175 0.4142 0.108 Uiso 0.564(7) 1 calc PR A 1 C19' C 0.2269(9) 0.4461(10) 0.4278(5) 0.072(2) Uiso 0.436(7) 1 d PD A 2 H19D H 0.2390 0.4332 0.4612 0.108 Uiso 0.436(7) 1 calc PR A 2 H19E H 0.1831 0.4048 0.4097 0.108 Uiso 0.436(7) 1 calc PR A 2 H19F H 0.1956 0.4998 0.4220 0.108 Uiso 0.436(7) 1 calc PR A 2 C20 C 0.3366(9) 0.5203(6) 0.4458(4) 0.066(2) Uiso 0.564(7) 1 d PD A 1 H20A H 0.3464 0.5010 0.4782 0.099 Uiso 0.564(7) 1 calc PR A 1 H20B H 0.2765 0.5537 0.4378 0.099 Uiso 0.564(7) 1 calc PR A 1 H20C H 0.3937 0.5530 0.4427 0.099 Uiso 0.564(7) 1 calc PR A 1 C20' C 0.3940(11) 0.5057(8) 0.4472(4) 0.066(2) Uiso 0.436(7) 1 d PD A 2 H20D H 0.3687 0.5615 0.4418 0.099 Uiso 0.436(7) 1 calc PR A 2 H20E H 0.4613 0.5031 0.4421 0.099 Uiso 0.436(7) 1 calc PR A 2 H20F H 0.3951 0.4895 0.4795 0.099 Uiso 0.436(7) 1 calc PR A 2 C21 C 0.5424(3) 0.5128(2) 0.15392(13) 0.0317(8) Uani 1 1 d . . . C22 C 0.6495(3) 0.5180(2) 0.17001(13) 0.0347(8) Uani 1 1 d . . . C23 C 0.7071(3) 0.4551(2) 0.15881(14) 0.0377(9) Uani 1 1 d . . . H23 H 0.7768 0.4589 0.1702 0.045 Uiso 1 1 calc R . . C24 C 0.6691(3) 0.3849(2) 0.13143(14) 0.0355(9) Uani 1 1 d . . . C25 C 0.5671(3) 0.3805(2) 0.11535(14) 0.0363(9) Uani 1 1 d . . . H25 H 0.5392 0.3355 0.0965 0.044 Uiso 1 1 calc R . . C26 C 0.5031(3) 0.4417(2) 0.12640(13) 0.0322(8) Uani 1 1 d . . . C27 C 0.3987(3) 0.4293(2) 0.10892(13) 0.0342(8) Uani 1 1 d . . . H27 H 0.3788 0.3828 0.0898 0.041 Uiso 1 1 calc R . . C28 C 0.2265(3) 0.4610(3) 0.09771(14) 0.0384(9) Uani 1 1 d . . . C29 C 0.1838(4) 0.3897(3) 0.0751(2) 0.0572(13) Uani 1 1 d . . . H29 H 0.2231 0.3438 0.0715 0.069 Uiso 1 1 calc R . . C30 C 0.0811(4) 0.3893(3) 0.0581(2) 0.0663(16) Uani 1 1 d . . . H30 H 0.0493 0.3425 0.0424 0.080 Uiso 1 1 calc R . . C31 C 0.0256(3) 0.4567(3) 0.06386(17) 0.0555(12) Uani 1 1 d . . . H31 H -0.0440 0.4573 0.0515 0.067 Uiso 1 1 calc R . . C32 C 0.0731(3) 0.5233(3) 0.08797(17) 0.0512(11) Uani 1 1 d . . . H32 H 0.0346 0.5690 0.0928 0.061 Uiso 1 1 calc R . . C33 C 0.6972(3) 0.5918(3) 0.19921(16) 0.0435(10) Uani 1 1 d . . . C34 C 0.8120(3) 0.5867(3) 0.2122(2) 0.0662(15) Uani 1 1 d . . . H34A H 0.8328 0.5390 0.2322 0.099 Uiso 1 1 calc R . . H34B H 0.8393 0.6362 0.2291 0.099 Uiso 1 1 calc R . . H34C H 0.8365 0.5816 0.1836 0.099 Uiso 1 1 calc R . . C35 C 0.6623(4) 0.5960(3) 0.24556(18) 0.0588(13) Uani 1 1 d . . . H35A H 0.5906 0.6051 0.2386 0.088 Uiso 1 1 calc R . . H35B H 0.6961 0.6410 0.2648 0.088 Uiso 1 1 calc R . . H35C H 0.6780 0.5446 0.2627 0.088 Uiso 1 1 calc R . . C36 C 0.6687(3) 0.6716(3) 0.17082(19) 0.0559(12) Uani 1 1 d . . . H36A H 0.6975 0.6710 0.1433 0.084 Uiso 1 1 calc R . . H36B H 0.6943 0.7186 0.1906 0.084 Uiso 1 1 calc R . . H36C H 0.5965 0.6755 0.1607 0.084 Uiso 1 1 calc R . . C37 C 0.7417(3) 0.3185(3) 0.12319(16) 0.0433(10) Uani 1 1 d . . . C38 C 0.7936(4) 0.2806(3) 0.17104(19) 0.0608(13) Uani 1 1 d . . . H38A H 0.8324 0.3226 0.1909 0.091 Uiso 1 1 calc R . . H38B H 0.8376 0.2365 0.1660 0.091 Uiso 1 1 calc R . . H38C H 0.7435 0.2587 0.1864 0.091 Uiso 1 1 calc R . . C39 C 0.8210(4) 0.3568(3) 0.1001(2) 0.0600(13) Uani 1 1 d . . . H39A H 0.7888 0.3789 0.0693 0.090 Uiso 1 1 calc R . . H39B H 0.8690 0.3149 0.0964 0.090 Uiso 1 1 calc R . . H39C H 0.8553 0.4008 0.1200 0.090 Uiso 1 1 calc R . . C40 C 0.6884(4) 0.2504(3) 0.09076(19) 0.0612(14) Uani 1 1 d . . . H40A H 0.6373 0.2259 0.1045 0.092 Uiso 1 1 calc R . . H40B H 0.7365 0.2085 0.0871 0.092 Uiso 1 1 calc R . . H40C H 0.6577 0.2734 0.0600 0.092 Uiso 1 1 calc R . . C41 C 0.1892(5) 0.8644(3) 0.1869(2) 0.0763(17) Uani 1 1 d . . . H41A H 0.2533 0.8531 0.2082 0.115 Uiso 1 1 calc R . . H41B H 0.1431 0.8854 0.2048 0.115 Uiso 1 1 calc R . . H41C H 0.1978 0.9050 0.1637 0.115 Uiso 1 1 calc R . . C42 C 0.1113(4) 0.6956(3) 0.20196(19) 0.0637(14) Uani 1 1 d . . . H42A H 0.0834 0.6445 0.1873 0.096 Uiso 1 1 calc R . . H42B H 0.0639 0.7213 0.2176 0.096 Uiso 1 1 calc R . . H42C H 0.1731 0.6842 0.2250 0.096 Uiso 1 1 calc R . . C43 C 0.0128(4) 0.7932(4) 0.1157(2) 0.0798(18) Uani 1 1 d . . . H43A H 0.0229 0.8308 0.0912 0.120 Uiso 1 1 calc R . . H43B H -0.0293 0.8194 0.1341 0.120 Uiso 1 1 calc R . . H43C H -0.0194 0.7434 0.1012 0.120 Uiso 1 1 calc R . . C44 C 0.2641(5) 0.8583(3) 0.0662(2) 0.0762(17) Uani 1 1 d . . . H44A H 0.2048 0.8903 0.0667 0.114 Uiso 1 1 calc R . . H44B H 0.2824 0.8664 0.0362 0.114 Uiso 1 1 calc R . . H44C H 0.3187 0.8760 0.0918 0.114 Uiso 1 1 calc R . . C45 C 0.1336(5) 0.7167(4) 0.02286(18) 0.0731(16) Uani 1 1 d . . . H45A H 0.1237 0.6576 0.0229 0.110 Uiso 1 1 calc R . . H45B H 0.1502 0.7330 -0.0065 0.110 Uiso 1 1 calc R . . H45C H 0.0727 0.7443 0.0258 0.110 Uiso 1 1 calc R . . C46 C 0.3490(4) 0.6866(4) 0.06453(18) 0.0618(14) Uani 1 1 d . . . H46A H 0.4067 0.6990 0.0899 0.093 Uiso 1 1 calc R . . H46B H 0.3629 0.7019 0.0344 0.093 Uiso 1 1 calc R . . H46C H 0.3347 0.6281 0.0645 0.093 Uiso 1 1 calc R . . C47 C 0.3851(8) 0.1627(5) 0.0675(3) 0.114(3) Uani 1 1 d . . . H47A H 0.4480 0.1486 0.0590 0.136 Uiso 1 1 calc R . . H47B H 0.3437 0.1943 0.0415 0.136 Uiso 1 1 calc R . . C48 C 0.3341(9) 0.0894(6) 0.0753(3) 0.142(4) Uani 1 1 d . . . H48A H 0.3679 0.0406 0.0667 0.171 Uiso 1 1 calc R . . H48B H 0.2648 0.0900 0.0567 0.171 Uiso 1 1 calc R . . C49 C 0.3375(8) 0.0900(6) 0.1261(3) 0.126(3) Uani 1 1 d . . . H49A H 0.3960 0.0600 0.1440 0.151 Uiso 1 1 calc R . . H49B H 0.2768 0.0656 0.1326 0.151 Uiso 1 1 calc R . . C50 C 0.3445(6) 0.1793(5) 0.1377(3) 0.107(3) Uani 1 1 d . . . H50A H 0.2783 0.2053 0.1301 0.129 Uiso 1 1 calc R . . H50B H 0.3751 0.1882 0.1713 0.129 Uiso 1 1 calc R . . C51 C 0.7575(9) 0.6618(6) 0.0384(4) 0.149(4) Uiso 1 1 d D . . H51A H 0.7631 0.6905 0.0686 0.178 Uiso 1 1 calc R . . H51B H 0.8128 0.6788 0.0244 0.178 Uiso 1 1 calc R . . C52 C 0.7549(8) 0.5719(6) 0.0442(4) 0.136(3) Uiso 1 1 d D . . H52A H 0.7782 0.5583 0.0778 0.163 Uiso 1 1 calc R . . H52B H 0.8010 0.5464 0.0272 0.163 Uiso 1 1 calc R . . C53 C 0.6534(8) 0.5369(7) 0.0263(4) 0.154(4) Uiso 1 1 d D . . H53A H 0.6344 0.4990 0.0491 0.185 Uiso 1 1 calc R . . H53B H 0.6463 0.5094 -0.0043 0.185 Uiso 1 1 calc R . . C54 C 0.5941(10) 0.6204(7) 0.0220(5) 0.168(5) Uiso 1 1 d . . . H54A H 0.5318 0.6179 -0.0025 0.202 Uiso 1 1 calc R . . H54B H 0.5795 0.6367 0.0522 0.202 Uiso 1 1 calc R . . C55 C -0.026(2) 0.0713(17) 0.1692(10) 0.184(4) Uiso 0.50 1 d PD B 3 C56 C 0.032(2) 0.1410(17) 0.1524(9) 0.184(4) Uiso 0.50 1 d PD B 3 C57 C 0.018(2) 0.1498(16) 0.1006(9) 0.184(4) Uiso 0.50 1 d PD B 3 C58 C 0.025(2) 0.0624(15) 0.0855(9) 0.184(4) Uiso 0.50 1 d PD B 3 C59 C 0.015(2) 0.0758(13) 0.0320(8) 0.184(4) Uiso 0.50 1 d PD B 3 C60 C 0.0000 0.0000 0.0000 0.184(4) Uiso 1 2 d SD . 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.02704(12) 0.03039(14) 0.02742(12) -0.00056(7) 0.00529(8) -0.00264(7) Si1 0.0435(6) 0.0454(7) 0.0468(7) -0.0042(5) 0.0043(5) 0.0141(5) Si2 0.0497(7) 0.0469(7) 0.0370(6) 0.0049(5) 0.0014(5) 0.0003(6) O1 0.0342(13) 0.0343(14) 0.0310(13) 0.0014(11) 0.0057(11) -0.0062(11) O2 0.0281(13) 0.0378(15) 0.0441(16) -0.0125(12) 0.0063(11) -0.0024(11) O3 0.230(7) 0.103(4) 0.107(4) -0.028(3) 0.083(5) -0.073(4) N1 0.0312(16) 0.0301(17) 0.0344(17) -0.0040(13) 0.0089(13) -0.0041(13) N2 0.0338(16) 0.0333(17) 0.0335(17) 0.0007(13) 0.0051(13) -0.0024(14) N3 0.0290(16) 0.0411(19) 0.0333(16) -0.0041(14) 0.0031(13) -0.0070(14) N4 0.0318(17) 0.046(2) 0.045(2) -0.0004(16) 0.0015(15) -0.0023(15) N5 0.0376(18) 0.0375(19) 0.0360(18) 0.0000(14) 0.0014(14) 0.0061(14) C1 0.0268(17) 0.0311(19) 0.0336(19) 0.0023(15) 0.0074(15) 0.0033(15) C2 0.0287(18) 0.031(2) 0.040(2) 0.0019(16) 0.0086(16) 0.0012(15) C3 0.037(2) 0.036(2) 0.039(2) 0.0077(17) 0.0122(17) -0.0017(17) C4 0.038(2) 0.036(2) 0.036(2) 0.0054(16) 0.0124(17) 0.0015(17) C5 0.039(2) 0.038(2) 0.032(2) -0.0022(16) 0.0058(16) 0.0019(17) C6 0.0309(18) 0.032(2) 0.0312(19) 0.0007(15) 0.0090(15) 0.0037(15) C7 0.0316(18) 0.0312(19) 0.0322(19) -0.0053(15) 0.0065(15) -0.0003(15) C8 0.0294(18) 0.0265(19) 0.038(2) -0.0013(15) 0.0078(15) -0.0022(15) C9 0.052(2) 0.037(2) 0.038(2) -0.0078(17) 0.0141(19) -0.0086(19) C10 0.054(3) 0.036(2) 0.052(3) -0.013(2) 0.014(2) -0.013(2) C11 0.045(2) 0.032(2) 0.054(3) 0.0016(18) 0.012(2) -0.0104(18) C12 0.043(2) 0.043(2) 0.038(2) 0.0035(18) 0.0097(18) -0.0090(18) C13 0.038(2) 0.040(2) 0.040(2) 0.0047(17) 0.0066(18) -0.0112(17) C14 0.049(3) 0.052(3) 0.052(3) 0.007(2) 0.007(2) -0.020(2) C15 0.037(2) 0.061(3) 0.063(3) 0.016(2) -0.002(2) -0.013(2) C16 0.060(3) 0.046(3) 0.046(3) -0.009(2) 0.012(2) -0.018(2) C17 0.055(3) 0.049(3) 0.033(2) 0.0063(18) 0.0116(19) -0.004(2) C21 0.0306(18) 0.034(2) 0.0310(18) -0.0010(15) 0.0079(15) -0.0045(16) C22 0.0289(18) 0.039(2) 0.035(2) -0.0051(16) 0.0055(15) -0.0033(16) C23 0.0299(19) 0.039(2) 0.044(2) 0.0005(17) 0.0078(16) -0.0010(16) C24 0.039(2) 0.036(2) 0.034(2) 0.0031(16) 0.0145(17) -0.0003(16) C25 0.044(2) 0.034(2) 0.032(2) -0.0013(15) 0.0106(17) -0.0030(17) C26 0.0324(19) 0.035(2) 0.0291(18) -0.0024(15) 0.0075(15) -0.0037(16) C27 0.039(2) 0.031(2) 0.0307(19) -0.0050(15) 0.0058(16) -0.0076(17) C28 0.0318(19) 0.047(2) 0.034(2) -0.0055(17) 0.0045(16) -0.0087(18) C29 0.038(2) 0.058(3) 0.072(3) -0.019(2) 0.005(2) -0.013(2) C30 0.049(3) 0.075(4) 0.068(4) -0.020(3) 0.000(3) -0.027(3) C31 0.029(2) 0.079(4) 0.053(3) 0.002(2) -0.0006(19) -0.015(2) C32 0.033(2) 0.061(3) 0.056(3) 0.002(2) 0.0016(19) -0.001(2) C33 0.030(2) 0.044(2) 0.053(3) -0.011(2) 0.0013(18) -0.0041(17) C34 0.033(2) 0.061(3) 0.095(4) -0.025(3) -0.004(2) -0.004(2) C35 0.056(3) 0.064(3) 0.050(3) -0.021(2) 0.000(2) -0.002(2) C36 0.042(2) 0.046(3) 0.077(3) -0.009(2) 0.009(2) -0.011(2) C37 0.042(2) 0.039(2) 0.051(3) 0.0031(19) 0.0167(19) 0.0040(18) C38 0.060(3) 0.057(3) 0.066(3) 0.015(2) 0.016(3) 0.015(2) C39 0.056(3) 0.061(3) 0.074(3) -0.001(3) 0.037(3) 0.007(2) C40 0.062(3) 0.046(3) 0.081(4) -0.013(3) 0.026(3) 0.006(2) C41 0.087(4) 0.054(3) 0.089(4) -0.020(3) 0.022(4) 0.009(3) C42 0.066(3) 0.069(3) 0.062(3) 0.002(3) 0.027(3) 0.022(3) C43 0.056(3) 0.109(5) 0.070(4) 0.003(3) 0.006(3) 0.040(3) C44 0.082(4) 0.058(3) 0.085(4) 0.020(3) 0.012(3) -0.004(3) C45 0.080(4) 0.091(4) 0.038(3) 0.003(3) -0.008(3) -0.008(3) C46 0.073(3) 0.074(4) 0.043(3) 0.007(2) 0.023(2) 0.007(3) C47 0.195(10) 0.084(5) 0.073(5) -0.001(4) 0.054(5) -0.004(6) C48 0.219(12) 0.123(7) 0.106(7) -0.053(6) 0.079(7) -0.092(8) C49 0.158(9) 0.114(7) 0.121(7) -0.004(6) 0.061(7) -0.053(6) C50 0.117(6) 0.117(6) 0.097(6) -0.033(5) 0.044(5) -0.031(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O1 2.280(2) . ? Nd1 O2 2.313(3) . ? Nd1 N5 2.385(3) . ? Nd1 N1 2.536(3) . ? Nd1 N3 2.566(3) . ? Nd1 N4 2.720(3) . ? Nd1 N2 2.721(3) . ? Nd1 Si2 3.3936(12) . ? Si1 N5 1.699(4) . ? Si1 C42 1.864(5) . ? Si1 C43 1.882(5) . ? Si1 C41 1.886(6) . ? Si2 N5 1.681(4) . ? Si2 C45 1.868(5) . ? Si2 C46 1.876(5) . ? Si2 C44 1.879(6) . ? O1 C1 1.299(4) . ? O2 C21 1.294(5) . ? O3 C50 1.395(9) . ? O3 C47 1.409(8) . ? O4 C51 1.352(11) . ? O4 C54 1.467(13) . ? N1 C7 1.303(5) . ? N1 C8 1.409(5) . ? N2 C12 1.332(5) . ? N2 C8 1.351(5) . ? N3 C27 1.301(5) . ? N3 C28 1.404(5) . ? N4 C28 1.331(5) . ? N4 C32 1.344(5) . ? C1 C2 1.432(5) . ? C1 C6 1.434(5) . ? C2 C3 1.376(5) . ? C2 C13 1.533(5) . ? C3 C4 1.414(6) . ? C3 H3 0.9400 . ? C4 C5 1.362(6) . ? C4 C17 1.547(5) . ? C5 C6 1.418(5) . ? C5 H5 0.9400 . ? C6 C7 1.423(5) . ? C7 H7 0.9400 . ? C8 C9 1.390(5) . ? C9 C10 1.364(6) . ? C9 H9 0.9400 . ? C10 C11 1.378(6) . ? C10 H10 0.9400 . ? C11 C12 1.366(6) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 C16 1.529(6) . ? C13 C14 1.545(6) . ? C13 C15 1.549(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 C18' 1.520(13) . ? C17 C20 1.519(10) . ? C17 C19' 1.521(12) . ? C17 C19 1.531(10) . ? C17 C18 1.536(11) . ? C17 C20' 1.537(12) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C18' H18D 0.9700 . ? C18' H18E 0.9700 . ? C18' H18F 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C19' H19D 0.9700 . ? C19' H19E 0.9700 . ? C19' H19F 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C20' H20D 0.9700 . ? C20' H20E 0.9700 . ? C20' H20F 0.9700 . ? C21 C26 1.436(5) . ? C21 C22 1.440(5) . ? C22 C23 1.377(5) . ? C22 C33 1.525(5) . ? C23 C24 1.418(6) . ? C23 H23 0.9400 . ? C24 C25 1.372(6) . ? C24 C37 1.525(6) . ? C25 C26 1.412(5) . ? C25 H25 0.9400 . ? C26 C27 1.421(5) . ? C27 H27 0.9400 . ? C28 C29 1.392(6) . ? C29 C30 1.383(7) . ? C29 H29 0.9400 . ? C30 C31 1.366(7) . ? C30 H30 0.9400 . ? C31 C32 1.369(7) . ? C31 H31 0.9400 . ? C32 H32 0.9400 . ? C33 C35 1.531(7) . ? C33 C36 1.536(7) . ? C33 C34 1.538(6) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C37 C40 1.525(6) . ? C37 C38 1.536(6) . ? C37 C39 1.536(6) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 H45C 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C46 H46C 0.9700 . ? C47 C48 1.425(10) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 C49 1.465(11) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.487(11) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.471(11) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 C53 1.484(11) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.571(14) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.525(18) . ? C56 C57 1.480(18) . ? C57 C58 1.494(18) . ? C58 C59 1.545(17) . ? C59 C60 1.526(17) . ? C60 C59 1.526(17) 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 O1 Nd1 O2 105.17(10) . . ? O1 Nd1 N5 119.16(11) . . ? O2 Nd1 N5 135.24(11) . . ? O1 Nd1 N1 68.66(9) . . ? O2 Nd1 N1 88.57(9) . . ? N5 Nd1 N1 101.30(11) . . ? O1 Nd1 N3 85.49(10) . . ? O2 Nd1 N3 67.29(9) . . ? N5 Nd1 N3 119.44(11) . . ? N1 Nd1 N3 138.84(10) . . ? O1 Nd1 N4 80.13(10) . . ? O2 Nd1 N4 116.51(10) . . ? N5 Nd1 N4 79.00(11) . . ? N1 Nd1 N4 144.46(10) . . ? N3 Nd1 N4 49.82(10) . . ? O1 Nd1 N2 119.12(9) . . ? O2 Nd1 N2 76.55(9) . . ? N5 Nd1 N2 76.90(11) . . ? N1 Nd1 N2 50.47(10) . . ? N3 Nd1 N2 140.85(10) . . ? N4 Nd1 N2 154.54(10) . . ? O1 Nd1 Si2 142.80(7) . . ? O2 Nd1 Si2 111.21(7) . . ? N5 Nd1 Si2 27.34(8) . . ? N1 Nd1 Si2 118.84(7) . . ? N3 Nd1 Si2 101.25(8) . . ? N4 Nd1 Si2 77.04(8) . . ? N2 Nd1 Si2 77.79(7) . . ? N5 Si1 C42 109.9(2) . . ? N5 Si1 C43 113.3(2) . . ? C42 Si1 C43 106.8(3) . . ? N5 Si1 C41 112.8(2) . . ? C42 Si1 C41 106.7(3) . . ? C43 Si1 C41 106.9(3) . . ? N5 Si2 C45 113.7(2) . . ? N5 Si2 C46 108.7(2) . . ? C45 Si2 C46 104.8(3) . . ? N5 Si2 C44 114.9(2) . . ? C45 Si2 C44 106.7(3) . . ? C46 Si2 C44 107.4(3) . . ? N5 Si2 Nd1 40.66(11) . . ? C45 Si2 Nd1 120.36(19) . . ? C46 Si2 Nd1 68.31(16) . . ? C44 Si2 Nd1 132.5(2) . . ? C1 O1 Nd1 146.8(2) . . ? C21 O2 Nd1 147.8(2) . . ? C50 O3 C47 106.8(6) . . ? C51 O4 C54 108.3(9) . . ? C7 N1 C8 122.1(3) . . ? C7 N1 Nd1 134.2(3) . . ? C8 N1 Nd1 103.4(2) . . ? C12 N2 C8 117.6(3) . . ? C12 N2 Nd1 144.9(3) . . ? C8 N2 Nd1 96.6(2) . . ? C27 N3 C28 122.1(3) . . ? C27 N3 Nd1 135.3(2) . . ? C28 N3 Nd1 102.6(2) . . ? C28 N4 C32 118.3(4) . . ? C28 N4 Nd1 97.5(2) . . ? C32 N4 Nd1 143.6(3) . . ? Si2 N5 Si1 127.7(2) . . ? Si2 N5 Nd1 112.00(17) . . ? Si1 N5 Nd1 120.25(17) . . ? O1 C1 C2 121.3(3) . . ? O1 C1 C6 121.2(3) . . ? C2 C1 C6 117.5(3) . . ? C3 C2 C1 118.5(4) . . ? C3 C2 C13 121.2(3) . . ? C1 C2 C13 120.3(3) . . ? C2 C3 C4 124.7(4) . . ? C2 C3 H3 117.6 . . ? C4 C3 H3 117.6 . . ? C5 C4 C3 116.5(4) . . ? C5 C4 C17 122.3(4) . . ? C3 C4 C17 121.2(3) . . ? C4 C5 C6 122.4(4) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C7 117.0(3) . . ? C5 C6 C1 120.0(3) . . ? C7 C6 C1 123.0(3) . . ? N1 C7 C6 125.0(3) . . ? N1 C7 H7 117.5 . . ? C6 C7 H7 117.5 . . ? N2 C8 C9 122.0(3) . . ? N2 C8 N1 109.0(3) . . ? C9 C8 N1 128.9(4) . . ? C10 C9 C8 118.8(4) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C9 C10 C11 119.4(4) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 118.7(4) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? N2 C12 C11 123.4(4) . . ? N2 C12 H12 118.3 . . ? C11 C12 H12 118.3 . . ? C16 C13 C2 109.8(3) . . ? C16 C13 C14 108.1(4) . . ? C2 C13 C14 112.1(4) . . ? C16 C13 C15 110.2(4) . . ? C2 C13 C15 110.2(3) . . ? C14 C13 C15 106.4(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18' C17 C20 131.5(8) . . ? C18' C17 C19' 110.0(9) . . ? C20 C17 C19' 77.6(7) . . ? C18' C17 C19 74.6(8) . . ? C20 C17 C19 109.1(7) . . ? C19' C17 C19 37.0(6) . . ? C18' C17 C18 33.0(6) . . ? C20 C17 C18 109.0(7) . . ? C19' C17 C18 135.6(8) . . ? C19 C17 C18 105.3(7) . . ? C18' C17 C20' 108.1(9) . . ? C20 C17 C20' 31.0(5) . . ? C19' C17 C20' 105.5(8) . . ? C19 C17 C20' 128.2(7) . . ? C18 C17 C20' 79.7(7) . . ? C18' C17 C4 110.0(7) . . ? C20 C17 C4 111.9(5) . . ? C19' C17 C4 109.5(6) . . ? C19 C17 C4 113.2(5) . . ? C18 C17 C4 108.1(6) . . ? C20' C17 C4 113.7(6) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? C17 C18' H18D 109.5 . . ? C17 C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C17 C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? C17 C19' H19D 109.5 . . ? C17 C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? C17 C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? C17 C20' H20D 109.5 . . ? C17 C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? C17 C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? O2 C21 C26 121.6(3) . . ? O2 C21 C22 121.5(3) . . ? C26 C21 C22 116.9(3) . . ? C23 C22 C21 118.7(3) . . ? C23 C22 C33 121.2(3) . . ? C21 C22 C33 120.1(3) . . ? C22 C23 C24 124.9(4) . . ? C22 C23 H23 117.6 . . ? C24 C23 H23 117.6 . . ? C25 C24 C23 116.6(4) . . ? C25 C24 C37 124.3(4) . . ? C23 C24 C37 119.1(4) . . ? C24 C25 C26 121.8(4) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C25 C26 C27 116.7(3) . . ? C25 C26 C21 121.2(3) . . ? C27 C26 C21 122.0(3) . . ? N3 C27 C26 125.7(3) . . ? N3 C27 H27 117.2 . . ? C26 C27 H27 117.2 . . ? N4 C28 C29 122.9(4) . . ? N4 C28 N3 109.2(3) . . ? C29 C28 N3 127.8(4) . . ? C30 C29 C28 117.1(5) . . ? C30 C29 H29 121.4 . . ? C28 C29 H29 121.4 . . ? C31 C30 C29 120.4(5) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 118.8(4) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? N4 C32 C31 122.5(5) . . ? N4 C32 H32 118.8 . . ? C31 C32 H32 118.8 . . ? C22 C33 C35 110.0(4) . . ? C22 C33 C36 109.9(4) . . ? C35 C33 C36 110.0(4) . . ? C22 C33 C34 112.2(4) . . ? C35 C33 C34 107.4(4) . . ? C36 C33 C34 107.2(4) . . ? 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 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C24 C37 C40 111.8(4) . . ? C24 C37 C38 109.0(4) . . ? C40 C37 C38 108.9(4) . . ? C24 C37 C39 109.7(4) . . ? C40 C37 C39 108.1(4) . . ? C38 C37 C39 109.2(4) . . ? 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 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si1 C41 H41A 109.5 . . ? Si1 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si1 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si1 C42 H42A 109.5 . . ? Si1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si1 C43 H43A 109.5 . . ? Si1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si2 C44 H44A 109.5 . . ? Si2 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si2 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si2 C45 H45A 109.5 . . ? Si2 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si2 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si2 C46 H46A 109.5 . . ? Si2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O3 C47 C48 109.0(6) . . ? O3 C47 H47A 109.9 . . ? C48 C47 H47A 109.9 . . ? O3 C47 H47B 109.9 . . ? C48 C47 H47B 109.9 . . ? H47A C47 H47B 108.3 . . ? C47 C48 C49 104.6(7) . . ? C47 C48 H48A 110.8 . . ? C49 C48 H48A 110.8 . . ? C47 C48 H48B 110.8 . . ? C49 C48 H48B 110.8 . . ? H48A C48 H48B 108.9 . . ? C48 C49 C50 102.7(7) . . ? C48 C49 H49A 111.2 . . ? C50 C49 H49A 111.2 . . ? C48 C49 H49B 111.2 . . ? C50 C49 H49B 111.2 . . ? H49A C49 H49B 109.1 . . ? O3 C50 C49 103.5(6) . . ? O3 C50 H50A 111.1 . . ? C49 C50 H50A 111.1 . . ? O3 C50 H50B 111.1 . . ? C49 C50 H50B 111.1 . . ? H50A C50 H50B 109.0 . . ? O4 C51 C52 100.9(9) . . ? O4 C51 H51A 111.6 . . ? C52 C51 H51A 111.6 . . ? O4 C51 H51B 111.6 . . ? C52 C51 H51B 111.6 . . ? H51A C51 H51B 109.4 . . ? C51 C52 C53 112.7(9) . . ? C51 C52 H52A 109.0 . . ? C53 C52 H52A 109.0 . . ? C51 C52 H52B 109.0 . . ? C53 C52 H52B 109.0 . . ? H52A C52 H52B 107.8 . . ? C52 C53 C54 97.2(9) . . ? C52 C53 H53A 112.3 . . ? C54 C53 H53A 112.3 . . ? C52 C53 H53B 112.3 . . ? C54 C53 H53B 112.3 . . ? H53A C53 H53B 109.9 . . ? O4 C54 C53 99.7(10) . . ? O4 C54 H54A 111.8 . . ? C53 C54 H54A 111.8 . . ? O4 C54 H54B 111.8 . . ? C53 C54 H54B 111.8 . . ? H54A C54 H54B 109.6 . . ? C57 C56 C55 116(2) . . ? C56 C57 C58 102(2) . . ? C57 C58 C59 99.5(19) . . ? C58 C59 C60 117.8(19) . . ? C59 C60 C59 180(2) 3 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Nd1 Si2 N5 37.5(2) . . . . ? O2 Nd1 Si2 N5 -155.23(19) . . . . ? N1 Nd1 Si2 N5 -54.7(2) . . . . ? N3 Nd1 Si2 N5 134.95(19) . . . . ? N4 Nd1 Si2 N5 91.1(2) . . . . ? N2 Nd1 Si2 N5 -85.1(2) . . . . ? O1 Nd1 Si2 C45 -54.4(3) . . . . ? O2 Nd1 Si2 C45 112.9(2) . . . . ? N5 Nd1 Si2 C45 -91.9(3) . . . . ? N1 Nd1 Si2 C45 -146.5(3) . . . . ? N3 Nd1 Si2 C45 43.1(3) . . . . ? N4 Nd1 Si2 C45 -0.8(3) . . . . ? N2 Nd1 Si2 C45 -176.9(3) . . . . ? O1 Nd1 Si2 C46 -149.3(2) . . . . ? O2 Nd1 Si2 C46 17.9(2) . . . . ? N5 Nd1 Si2 C46 173.2(3) . . . . ? N1 Nd1 Si2 C46 118.5(2) . . . . ? N3 Nd1 Si2 C46 -51.9(2) . . . . ? N4 Nd1 Si2 C46 -95.8(2) . . . . ? N2 Nd1 Si2 C46 88.1(2) . . . . ? O1 Nd1 Si2 C44 116.6(3) . . . . ? O2 Nd1 Si2 C44 -76.1(3) . . . . ? N5 Nd1 Si2 C44 79.1(3) . . . . ? N1 Nd1 Si2 C44 24.4(3) . . . . ? N3 Nd1 Si2 C44 -145.9(3) . . . . ? N4 Nd1 Si2 C44 170.2(3) . . . . ? N2 Nd1 Si2 C44 -6.0(3) . . . . ? O2 Nd1 O1 C1 75.0(4) . . . . ? N5 Nd1 O1 C1 -98.6(4) . . . . ? N1 Nd1 O1 C1 -7.3(4) . . . . ? N3 Nd1 O1 C1 140.0(4) . . . . ? N4 Nd1 O1 C1 -170.0(4) . . . . ? N2 Nd1 O1 C1 -7.8(5) . . . . ? Si2 Nd1 O1 C1 -117.3(4) . . . . ? O1 Nd1 O2 C21 72.0(5) . . . . ? N5 Nd1 O2 C21 -115.9(5) . . . . ? N1 Nd1 O2 C21 139.4(5) . . . . ? N3 Nd1 O2 C21 -6.4(5) . . . . ? N4 Nd1 O2 C21 -14.4(5) . . . . ? N2 Nd1 O2 C21 -171.1(5) . . . . ? Si2 Nd1 O2 C21 -100.1(5) . . . . ? O1 Nd1 N1 C7 11.5(3) . . . . ? O2 Nd1 N1 C7 -95.4(3) . . . . ? N5 Nd1 N1 C7 128.6(3) . . . . ? N3 Nd1 N1 C7 -43.4(4) . . . . ? N4 Nd1 N1 C7 41.8(4) . . . . ? N2 Nd1 N1 C7 -169.1(4) . . . . ? Si2 Nd1 N1 C7 151.1(3) . . . . ? O1 Nd1 N1 C8 -175.1(2) . . . . ? O2 Nd1 N1 C8 78.0(2) . . . . ? N5 Nd1 N1 C8 -58.0(2) . . . . ? N3 Nd1 N1 C8 130.1(2) . . . . ? N4 Nd1 N1 C8 -144.8(2) . . . . ? N2 Nd1 N1 C8 4.4(2) . . . . ? Si2 Nd1 N1 C8 -35.5(2) . . . . ? O1 Nd1 N2 C12 -171.0(5) . . . . ? O2 Nd1 N2 C12 89.0(5) . . . . ? N5 Nd1 N2 C12 -54.7(5) . . . . ? N1 Nd1 N2 C12 -171.6(5) . . . . ? N3 Nd1 N2 C12 66.2(5) . . . . ? N4 Nd1 N2 C12 -35.5(6) . . . . ? Si2 Nd1 N2 C12 -26.7(5) . . . . ? O1 Nd1 N2 C8 -3.8(3) . . . . ? O2 Nd1 N2 C8 -103.9(2) . . . . ? N5 Nd1 N2 C8 112.5(2) . . . . ? N1 Nd1 N2 C8 -4.5(2) . . . . ? N3 Nd1 N2 C8 -126.6(2) . . . . ? N4 Nd1 N2 C8 131.7(3) . . . . ? Si2 Nd1 N2 C8 140.5(2) . . . . ? O1 Nd1 N3 C27 -106.3(4) . . . . ? O2 Nd1 N3 C27 2.2(4) . . . . ? N5 Nd1 N3 C27 132.6(4) . . . . ? N1 Nd1 N3 C27 -56.5(4) . . . . ? N4 Nd1 N3 C27 172.8(4) . . . . ? N2 Nd1 N3 C27 26.3(4) . . . . ? Si2 Nd1 N3 C27 110.7(4) . . . . ? O1 Nd1 N3 C28 75.3(2) . . . . ? O2 Nd1 N3 C28 -176.2(3) . . . . ? N5 Nd1 N3 C28 -45.8(3) . . . . ? N1 Nd1 N3 C28 125.2(2) . . . . ? N4 Nd1 N3 C28 -5.6(2) . . . . ? N2 Nd1 N3 C28 -152.1(2) . . . . ? Si2 Nd1 N3 C28 -67.7(2) . . . . ? O1 Nd1 N4 C28 -86.7(3) . . . . ? O2 Nd1 N4 C28 15.5(3) . . . . ? N5 Nd1 N4 C28 150.8(3) . . . . ? N1 Nd1 N4 C28 -115.1(3) . . . . ? N3 Nd1 N4 C28 5.8(2) . . . . ? N2 Nd1 N4 C28 131.8(3) . . . . ? Si2 Nd1 N4 C28 122.9(3) . . . . ? O1 Nd1 N4 C32 82.8(5) . . . . ? O2 Nd1 N4 C32 -175.1(5) . . . . ? N5 Nd1 N4 C32 -39.7(5) . . . . ? N1 Nd1 N4 C32 54.4(6) . . . . ? N3 Nd1 N4 C32 175.2(6) . . . . ? N2 Nd1 N4 C32 -58.8(6) . . . . ? Si2 Nd1 N4 C32 -67.6(5) . . . . ? C45 Si2 N5 Si1 -73.2(4) . . . . ? C46 Si2 N5 Si1 170.5(3) . . . . ? C44 Si2 N5 Si1 50.2(4) . . . . ? Nd1 Si2 N5 Si1 177.2(4) . . . . ? C45 Si2 N5 Nd1 109.7(3) . . . . ? C46 Si2 N5 Nd1 -6.7(3) . . . . ? C44 Si2 N5 Nd1 -127.0(3) . . . . ? C42 Si1 N5 Si2 161.2(3) . . . . ? C43 Si1 N5 Si2 41.8(4) . . . . ? C41 Si1 N5 Si2 -79.8(3) . . . . ? C42 Si1 N5 Nd1 -21.9(3) . . . . ? C43 Si1 N5 Nd1 -141.2(3) . . . . ? C41 Si1 N5 Nd1 97.1(3) . . . . ? O1 Nd1 N5 Si2 -155.06(15) . . . . ? O2 Nd1 N5 Si2 33.7(2) . . . . ? N1 Nd1 N5 Si2 133.21(17) . . . . ? N3 Nd1 N5 Si2 -52.9(2) . . . . ? N4 Nd1 N5 Si2 -83.03(18) . . . . ? N2 Nd1 N5 Si2 88.68(18) . . . . ? O1 Nd1 N5 Si1 27.5(2) . . . . ? O2 Nd1 N5 Si1 -143.73(16) . . . . ? N1 Nd1 N5 Si1 -44.2(2) . . . . ? N3 Nd1 N5 Si1 129.73(18) . . . . ? N4 Nd1 N5 Si1 99.6(2) . . . . ? N2 Nd1 N5 Si1 -88.7(2) . . . . ? Si2 Nd1 N5 Si1 -177.4(3) . . . . ? Nd1 O1 C1 C2 -177.8(3) . . . . ? Nd1 O1 C1 C6 1.5(6) . . . . ? O1 C1 C2 C3 173.8(3) . . . . ? C6 C1 C2 C3 -5.6(5) . . . . ? O1 C1 C2 C13 -5.0(5) . . . . ? C6 C1 C2 C13 175.6(3) . . . . ? C1 C2 C3 C4 2.1(6) . . . . ? C13 C2 C3 C4 -179.1(4) . . . . ? C2 C3 C4 C5 1.8(6) . . . . ? C2 C3 C4 C17 -177.5(4) . . . . ? C3 C4 C5 C6 -2.1(6) . . . . ? C17 C4 C5 C6 177.2(4) . . . . ? C4 C5 C6 C7 179.0(4) . . . . ? C4 C5 C6 C1 -1.5(6) . . . . ? O1 C1 C6 C5 -174.0(3) . . . . ? C2 C1 C6 C5 5.4(5) . . . . ? O1 C1 C6 C7 5.5(6) . . . . ? C2 C1 C6 C7 -175.2(3) . . . . ? C8 N1 C7 C6 176.3(3) . . . . ? Nd1 N1 C7 C6 -11.2(6) . . . . ? C5 C6 C7 N1 179.5(4) . . . . ? C1 C6 C7 N1 0.0(6) . . . . ? C12 N2 C8 C9 0.9(6) . . . . ? Nd1 N2 C8 C9 -170.8(3) . . . . ? C12 N2 C8 N1 178.2(3) . . . . ? Nd1 N2 C8 N1 6.5(3) . . . . ? C7 N1 C8 N2 167.3(3) . . . . ? Nd1 N1 C8 N2 -7.2(3) . . . . ? C7 N1 C8 C9 -15.7(6) . . . . ? Nd1 N1 C8 C9 169.9(4) . . . . ? N2 C8 C9 C10 -0.8(6) . . . . ? N1 C8 C9 C10 -177.6(4) . . . . ? C8 C9 C10 C11 0.3(7) . . . . ? C9 C10 C11 C12 0.0(7) . . . . ? C8 N2 C12 C11 -0.6(6) . . . . ? Nd1 N2 C12 C11 165.0(3) . . . . ? C10 C11 C12 N2 0.1(7) . . . . ? C3 C2 C13 C16 -112.9(4) . . . . ? C1 C2 C13 C16 65.9(5) . . . . ? C3 C2 C13 C14 7.3(5) . . . . ? C1 C2 C13 C14 -174.0(4) . . . . ? C3 C2 C13 C15 125.6(4) . . . . ? C1 C2 C13 C15 -55.7(5) . . . . ? C5 C4 C17 C18' -118.3(8) . . . . ? C3 C4 C17 C18' 61.0(9) . . . . ? C5 C4 C17 C20 36.7(7) . . . . ? C3 C4 C17 C20 -144.0(6) . . . . ? C5 C4 C17 C19' 120.8(7) . . . . ? C3 C4 C17 C19' -59.9(8) . . . . ? C5 C4 C17 C19 160.4(6) . . . . ? C3 C4 C17 C19 -20.3(7) . . . . ? C5 C4 C17 C18 -83.3(7) . . . . ? C3 C4 C17 C18 95.9(7) . . . . ? C5 C4 C17 C20' 3.1(8) . . . . ? C3 C4 C17 C20' -177.7(7) . . . . ? Nd1 O2 C21 C26 6.2(7) . . . . ? Nd1 O2 C21 C22 -172.5(3) . . . . ? O2 C21 C22 C23 177.9(4) . . . . ? C26 C21 C22 C23 -0.9(5) . . . . ? O2 C21 C22 C33 -1.6(6) . . . . ? C26 C21 C22 C33 179.7(4) . . . . ? C21 C22 C23 C24 1.3(6) . . . . ? C33 C22 C23 C24 -179.2(4) . . . . ? C22 C23 C24 C25 -0.2(6) . . . . ? C22 C23 C24 C37 -178.0(4) . . . . ? C23 C24 C25 C26 -1.4(6) . . . . ? C37 C24 C25 C26 176.2(4) . . . . ? C24 C25 C26 C27 -178.2(4) . . . . ? C24 C25 C26 C21 1.9(6) . . . . ? O2 C21 C26 C25 -179.4(3) . . . . ? C22 C21 C26 C25 -0.6(5) . . . . ? O2 C21 C26 C27 0.7(6) . . . . ? C22 C21 C26 C27 179.4(4) . . . . ? C28 N3 C27 C26 178.9(4) . . . . ? Nd1 N3 C27 C26 0.7(6) . . . . ? C25 C26 C27 N3 176.9(4) . . . . ? C21 C26 C27 N3 -3.1(6) . . . . ? C32 N4 C28 C29 -2.6(7) . . . . ? Nd1 N4 C28 C29 170.3(4) . . . . ? C32 N4 C28 N3 178.5(4) . . . . ? Nd1 N4 C28 N3 -8.5(3) . . . . ? C27 N3 C28 N4 -169.4(4) . . . . ? Nd1 N3 C28 N4 9.2(4) . . . . ? C27 N3 C28 C29 11.8(7) . . . . ? Nd1 N3 C28 C29 -169.6(4) . . . . ? N4 C28 C29 C30 2.6(8) . . . . ? N3 C28 C29 C30 -178.8(5) . . . . ? C28 C29 C30 C31 -0.2(9) . . . . ? C29 C30 C31 C32 -1.9(9) . . . . ? C28 N4 C32 C31 0.2(7) . . . . ? Nd1 N4 C32 C31 -167.9(4) . . . . ? C30 C31 C32 N4 2.0(8) . . . . ? C23 C22 C33 C35 -118.0(4) . . . . ? C21 C22 C33 C35 61.5(5) . . . . ? C23 C22 C33 C36 120.7(4) . . . . ? C21 C22 C33 C36 -59.8(5) . . . . ? C23 C22 C33 C34 1.5(6) . . . . ? C21 C22 C33 C34 -179.0(4) . . . . ? C25 C24 C37 C40 5.7(6) . . . . ? C23 C24 C37 C40 -176.7(4) . . . . ? C25 C24 C37 C38 -114.8(5) . . . . ? C23 C24 C37 C38 62.8(5) . . . . ? C25 C24 C37 C39 125.7(5) . . . . ? C23 C24 C37 C39 -56.7(5) . . . . ? C50 O3 C47 C48 -15.7(12) . . . . ? O3 C47 C48 C49 -8.0(13) . . . . ? C47 C48 C49 C50 26.9(12) . . . . ? C47 O3 C50 C49 32.4(10) . . . . ? C48 C49 C50 O3 -36.6(11) . . . . ? C54 O4 C51 C52 38.5(11) . . . . ? O4 C51 C52 C53 -13.5(13) . . . . ? C51 C52 C53 C54 -14.1(13) . . . . ? C51 O4 C54 C53 -48.4(12) . . . . ? C52 C53 C54 O4 34.1(11) . . . . ? C55 C56 C57 C58 -44(3) . . . . ? C56 C57 C58 C59 -177(2) . . . . ? C57 C58 C59 C60 -170(2) . . . . ? C58 C59 C60 C59 -99(2) . . . 3 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.132 _refine_diff_density_min -1.010 _refine_diff_density_rms 0.093 #==================================================END OF CIF