Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Qi Shen' _publ_contact_author_address ; Department of Chemistry Key Laboratory of Organic Synthesis of Jiangsu Province Suzhou 215123 CHINA ; _publ_contact_author_email QSHEN@SUDA.EDU.CN _publ_section_title ; Synthesis and structural characterization of novel mixed-valent samarium and divalent ytterbium and europium complexes supported by amine bis(phenolate) ligands ; loop_ _publ_author_name 'Qi Shen' 'Huadong Guo' 'Yingming Yao' 'Yong Zhang' 'Hui Zhou' data_complexl _database_code_depnum_ccdc_archive 'CCDC 643504' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H108 Eu2 N4 O4, C4 H8 O' _chemical_formula_sum 'C72 H116 Eu2 N4 O5' _chemical_formula_weight 1421.61 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' Eu Eu -0.1578 3.6682 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' _symmetry_space_group_name_Hall '-p 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6760(11) _cell_length_b 14.2953(19) _cell_length_c 27.072(4) _cell_angle_alpha 88.847(9) _cell_angle_beta 86.999(9) _cell_angle_gamma 84.992(7) _cell_volume 3724.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 14696 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour orange-yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1484 _exptl_absorpt_coefficient_mu 1.715 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5618 _exptl_absorpt_correction_T_max 0.7364 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39679 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0821 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 16724 _reflns_number_gt 12279 _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. The bond lengths of the THF molecule are unreasonable, so that 5 restraints were used for the refinement of the THF molecule. ; _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^)+(0.0671P)^2^+31.8314P] 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 16724 _refine_ls_number_parameters 752 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1171 _refine_ls_R_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.2103 _refine_ls_wR_factor_gt 0.1894 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.107 _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 Eu1 Eu 0.04945(4) 0.09440(3) 0.191709(15) 0.03192(12) Uani 1 1 d . . . Eu2 Eu 0.04633(5) -0.06004(3) 0.306212(16) 0.03664(13) Uani 1 1 d . . . O1 O -0.0137(6) 0.1027(4) 0.2785(2) 0.0330(12) Uani 1 1 d . . . O2 O 0.2587(6) 0.0313(4) 0.1563(2) 0.0332(12) Uani 1 1 d . . . O3 O -0.0183(6) -0.0593(4) 0.2216(2) 0.0333(12) Uani 1 1 d . . . O4 O 0.2574(7) -0.0228(4) 0.3331(2) 0.0426(15) Uani 1 1 d . . . O5 O 0.676(3) 0.5825(17) 0.2198(9) 0.233(9) Uiso 1 1 d D . . N1 N 0.2300(7) 0.2033(5) 0.2262(3) 0.0358(16) Uani 1 1 d . . . N2 N -0.0209(9) 0.2750(6) 0.1689(3) 0.0464(19) Uani 1 1 d . . . N3 N 0.2166(7) -0.1960(5) 0.2647(3) 0.0389(17) Uani 1 1 d . . . N4 N -0.0274(9) -0.2291(6) 0.3369(3) 0.052(2) Uani 1 1 d . . . C1 C -0.0093(8) 0.1730(6) 0.3110(3) 0.0309(17) Uani 1 1 d . . . C2 C -0.1247(9) 0.2008(6) 0.3432(3) 0.0346(18) Uani 1 1 d . . . C3 C -0.1058(10) 0.2701(6) 0.3775(3) 0.039(2) Uani 1 1 d . . . H3 H -0.1815 0.2880 0.4001 0.046 Uiso 1 1 calc R . . C4 C 0.0152(10) 0.3143(6) 0.3810(3) 0.040(2) Uani 1 1 d . . . C5 C 0.1247(9) 0.2879(6) 0.3473(3) 0.0370(19) Uani 1 1 d . . . H5 H 0.2084 0.3180 0.3477 0.044 Uiso 1 1 calc R . . C6 C 0.1131(9) 0.2177(6) 0.3131(3) 0.0313(17) Uani 1 1 d . . . C7 C 0.3144(8) 0.0940(6) 0.1264(3) 0.0299(16) Uani 1 1 d . . . C8 C 0.3132(9) 0.0913(6) 0.0741(3) 0.0324(17) Uani 1 1 d . . . C9 C 0.3696(9) 0.1635(6) 0.0465(3) 0.039(2) Uani 1 1 d . . . H9 H 0.3668 0.1622 0.0115 0.046 Uiso 1 1 calc R . . C10 C 0.4298(8) 0.2375(6) 0.0674(3) 0.0359(19) Uani 1 1 d . . . C11 C 0.4308(9) 0.2377(7) 0.1189(3) 0.0376(19) Uani 1 1 d . . . H11 H 0.4711 0.2868 0.1346 0.045 Uiso 1 1 calc R . . C12 C 0.3747(8) 0.1684(6) 0.1475(3) 0.0314(17) Uani 1 1 d . . . C13 C 0.2399(9) 0.1872(6) 0.2808(3) 0.0329(17) Uani 1 1 d . . . H13A H 0.3184 0.2204 0.2916 0.040 Uiso 1 1 calc R . . H13B H 0.2632 0.1192 0.2867 0.040 Uiso 1 1 calc R . . C14 C 0.3722(9) 0.1746(6) 0.2037(3) 0.0362(19) Uani 1 1 d . . . H14A H 0.4057 0.1127 0.2177 0.043 Uiso 1 1 calc R . . H14B H 0.4369 0.2207 0.2128 0.043 Uiso 1 1 calc R . . C15 C 0.1906(10) 0.3037(6) 0.2148(3) 0.039(2) Uani 1 1 d . . . H15A H 0.2429 0.3214 0.1842 0.047 Uiso 1 1 calc R . . H15B H 0.2201 0.3418 0.2419 0.047 Uiso 1 1 calc R . . C16 C 0.0385(12) 0.3288(7) 0.2083(4) 0.057(3) Uani 1 1 d . . . H16A H -0.0132 0.3177 0.2401 0.068 Uiso 1 1 calc R . . H16B H 0.0241 0.3967 0.2002 0.068 Uiso 1 1 calc R . . C17 C -0.1715(13) 0.3000(10) 0.1734(5) 0.078(4) Uani 1 1 d . . . H17A H -0.1911 0.3666 0.1649 0.116 Uiso 1 1 calc R . . H17B H -0.2057 0.2883 0.2075 0.116 Uiso 1 1 calc R . . H17C H -0.2180 0.2618 0.1508 0.116 Uiso 1 1 calc R . . C18 C 0.0311(14) 0.2992(8) 0.1200(4) 0.066(3) Uani 1 1 d . . . H18A H -0.0101 0.2616 0.0957 0.099 Uiso 1 1 calc R . . H18B H 0.1324 0.2864 0.1177 0.099 Uiso 1 1 calc R . . H18C H 0.0065 0.3660 0.1133 0.099 Uiso 1 1 calc R . . C19 C -0.2647(10) 0.1598(7) 0.3416(3) 0.041(2) Uani 1 1 d . . . C20 C -0.3732(11) 0.2065(8) 0.3792(4) 0.056(3) Uani 1 1 d . . . H20A H -0.3429 0.1936 0.4128 0.085 Uiso 1 1 calc R . . H20B H -0.4629 0.1811 0.3756 0.085 Uiso 1 1 calc R . . H20C H -0.3827 0.2745 0.3730 0.085 Uiso 1 1 calc R . . C21 C -0.3213(10) 0.1757(8) 0.2903(4) 0.052(3) Uani 1 1 d . . . H21A H -0.3393 0.2432 0.2838 0.078 Uiso 1 1 calc R . . H21B H -0.4079 0.1453 0.2887 0.078 Uiso 1 1 calc R . . H21C H -0.2530 0.1487 0.2653 0.078 Uiso 1 1 calc R . . C22 C -0.2505(11) 0.0527(7) 0.3526(4) 0.055(3) Uani 1 1 d . . . H22A H -0.2027 0.0200 0.3243 0.082 Uiso 1 1 calc R . . H22B H -0.3431 0.0305 0.3585 0.082 Uiso 1 1 calc R . . H22C H -0.1968 0.0399 0.3821 0.082 Uiso 1 1 calc R . . C23 C 0.0270(11) 0.3855(7) 0.4227(4) 0.053(3) Uani 1 1 d . . . C24 C -0.0947(14) 0.4594(8) 0.4210(5) 0.075(4) Uani 1 1 d . . . H24A H -0.0945 0.5008 0.4494 0.113 Uiso 1 1 calc R . . H24B H -0.1816 0.4288 0.4222 0.113 Uiso 1 1 calc R . . H24C H -0.0868 0.4965 0.3903 0.113 Uiso 1 1 calc R . . C25 C 0.0217(15) 0.3297(9) 0.4729(4) 0.070(3) Uani 1 1 d . . . H25A H 0.0986 0.2803 0.4729 0.105 Uiso 1 1 calc R . . H25B H -0.0667 0.3012 0.4771 0.105 Uiso 1 1 calc R . . H25C H 0.0299 0.3726 0.5002 0.105 Uiso 1 1 calc R . . C26 C 0.1590(15) 0.4347(10) 0.4174(5) 0.082(4) Uani 1 1 d . . . H26A H 0.1606 0.4708 0.3862 0.122 Uiso 1 1 calc R . . H26B H 0.2394 0.3879 0.4173 0.122 Uiso 1 1 calc R . . H26C H 0.1627 0.4772 0.4451 0.122 Uiso 1 1 calc R . . C27 C 0.2462(9) 0.0119(7) 0.0494(3) 0.041(2) Uani 1 1 d . . . C28 C 0.2574(11) 0.0202(8) -0.0069(4) 0.052(2) Uani 1 1 d . . . H28A H 0.2102 0.0802 -0.0174 0.078 Uiso 1 1 calc R . . H28B H 0.2137 -0.0316 -0.0212 0.078 Uiso 1 1 calc R . . H28C H 0.3555 0.0174 -0.0182 0.078 Uiso 1 1 calc R . . C29 C 0.3146(11) -0.0848(7) 0.0651(4) 0.048(2) Uani 1 1 d . . . H29A H 0.4128 -0.0901 0.0538 0.072 Uiso 1 1 calc R . . H29B H 0.2674 -0.1344 0.0503 0.072 Uiso 1 1 calc R . . H29C H 0.3070 -0.0913 0.1012 0.072 Uiso 1 1 calc R . . C30 C 0.0896(10) 0.0161(8) 0.0650(4) 0.053(3) Uani 1 1 d . . . H30A H 0.0783 0.0016 0.1005 0.079 Uiso 1 1 calc R . . H30B H 0.0452 -0.0299 0.0463 0.079 Uiso 1 1 calc R . . H30C H 0.0461 0.0792 0.0583 0.079 Uiso 1 1 calc R . . C31 C 0.4846(11) 0.3184(7) 0.0361(4) 0.047(2) Uani 1 1 d . . . C32 C 0.3947(19) 0.4069(8) 0.0498(6) 0.101(6) Uani 1 1 d . . . H32A H 0.4380 0.4396 0.0757 0.151 Uiso 1 1 calc R . . H32B H 0.3027 0.3905 0.0622 0.151 Uiso 1 1 calc R . . H32C H 0.3851 0.4481 0.0206 0.151 Uiso 1 1 calc R . . C33 C 0.6336(14) 0.3267(12) 0.0451(5) 0.093(5) Uani 1 1 d . . . H33A H 0.6859 0.2652 0.0410 0.140 Uiso 1 1 calc R . . H33B H 0.6417 0.3484 0.0788 0.140 Uiso 1 1 calc R . . H33C H 0.6711 0.3718 0.0214 0.140 Uiso 1 1 calc R . . C34 C 0.4737(13) 0.3081(8) -0.0192(4) 0.061(3) Uani 1 1 d . . . H34A H 0.5083 0.3629 -0.0365 0.092 Uiso 1 1 calc R . . H34B H 0.3764 0.3037 -0.0265 0.092 Uiso 1 1 calc R . . H34C H 0.5294 0.2511 -0.0302 0.092 Uiso 1 1 calc R . . C35 C -0.0200(8) -0.1311(6) 0.1899(3) 0.0328(18) Uani 1 1 d . . . C36 C -0.1408(8) -0.1447(5) 0.1635(3) 0.0281(16) Uani 1 1 d . . . C37 C -0.1294(10) -0.2163(6) 0.1293(3) 0.042(2) Uani 1 1 d . . . H37 H -0.2081 -0.2234 0.1106 0.050 Uiso 1 1 calc R . . C38 C -0.0133(10) -0.2780(6) 0.1200(3) 0.040(2) Uani 1 1 d . . . C39 C 0.0996(10) -0.2664(6) 0.1487(3) 0.042(2) Uani 1 1 d . . . H39 H 0.1812 -0.3081 0.1443 0.050 Uiso 1 1 calc R . . C40 C 0.0964(9) -0.1950(6) 0.1837(3) 0.0365(19) Uani 1 1 d . . . C41 C 0.3114(9) -0.0950(6) 0.3600(4) 0.040(2) Uani 1 1 d . . . C42 C 0.3144(9) -0.0896(6) 0.4132(3) 0.040(2) Uani 1 1 d . . . C43 C 0.3720(9) -0.1688(7) 0.4393(4) 0.045(2) Uani 1 1 d . . . H43 H 0.3745 -0.1658 0.4743 0.053 Uiso 1 1 calc R . . C44 C 0.4255(9) -0.2514(7) 0.4161(4) 0.042(2) Uani 1 1 d . . . C45 C 0.4238(9) -0.2533(7) 0.3651(4) 0.044(2) Uani 1 1 d . . . H45 H 0.4639 -0.3076 0.3484 0.052 Uiso 1 1 calc R . . C46 C 0.3657(9) -0.1784(7) 0.3375(3) 0.041(2) Uani 1 1 d . . . C47 C 0.2267(9) -0.1836(6) 0.2100(3) 0.0344(18) Uani 1 1 d . . . H47A H 0.3009 -0.2295 0.1965 0.041 Uiso 1 1 calc R . . H47B H 0.2559 -0.1200 0.2023 0.041 Uiso 1 1 calc R . . C48 C 0.3588(9) -0.1838(7) 0.2824(3) 0.043(2) Uani 1 1 d . . . H48A H 0.4235 -0.2370 0.2705 0.052 Uiso 1 1 calc R . . H48B H 0.3916 -0.1255 0.2672 0.052 Uiso 1 1 calc R . . C49 C 0.1739(10) -0.2886(7) 0.2799(4) 0.045(2) Uani 1 1 d . . . H49A H 0.2262 -0.3116 0.3089 0.054 Uiso 1 1 calc R . . H49B H 0.1982 -0.3332 0.2527 0.054 Uiso 1 1 calc R . . C50 C 0.0241(15) -0.2873(10) 0.2929(6) 0.087(4) Uani 1 1 d . . . H50A H 0.0012 -0.3527 0.2994 0.104 Uiso 1 1 calc R . . H50B H -0.0272 -0.2634 0.2639 0.104 Uiso 1 1 calc R . . C51 C -0.1761(16) -0.2335(12) 0.3367(7) 0.110(6) Uani 1 1 d . . . H51A H -0.1969 -0.2989 0.3336 0.165 Uiso 1 1 calc R . . H51B H -0.2127 -0.1963 0.3088 0.165 Uiso 1 1 calc R . . H51C H -0.2196 -0.2081 0.3677 0.165 Uiso 1 1 calc R . . C52 C 0.0182(18) -0.2570(11) 0.3841(6) 0.103(6) Uani 1 1 d . . . H52A H -0.0022 -0.2049 0.4070 0.155 Uiso 1 1 calc R . . H52B H 0.1186 -0.2743 0.3817 0.155 Uiso 1 1 calc R . . H52C H -0.0300 -0.3111 0.3962 0.155 Uiso 1 1 calc R . . C53 C -0.2746(8) -0.0797(6) 0.1712(3) 0.0346(18) Uani 1 1 d . . . C54 C -0.3927(9) -0.1068(7) 0.1399(4) 0.048(2) Uani 1 1 d . . . H54A H -0.3644 -0.1021 0.1047 0.072 Uiso 1 1 calc R . . H54B H -0.4760 -0.0642 0.1470 0.072 Uiso 1 1 calc R . . H54C H -0.4129 -0.1715 0.1481 0.072 Uiso 1 1 calc R . . C55 C -0.3299(9) -0.0852(7) 0.2256(4) 0.045(2) Uani 1 1 d . . . H55A H -0.3559 -0.1488 0.2332 0.067 Uiso 1 1 calc R . . H55B H -0.4115 -0.0401 0.2307 0.067 Uiso 1 1 calc R . . H55C H -0.2574 -0.0701 0.2473 0.067 Uiso 1 1 calc R . . C56 C -0.2530(11) 0.0242(7) 0.1582(4) 0.052(3) Uani 1 1 d . . . H56A H -0.2051 0.0513 0.1848 0.078 Uiso 1 1 calc R . . H56B H -0.3434 0.0595 0.1545 0.078 Uiso 1 1 calc R . . H56C H -0.1968 0.0274 0.1271 0.078 Uiso 1 1 calc R . . C57 C -0.0093(11) -0.3512(7) 0.0794(4) 0.049(2) Uani 1 1 d . . . C58 C -0.1292(13) -0.4140(8) 0.0888(5) 0.062(3) Uani 1 1 d . . . H58A H -0.1275 -0.4596 0.0621 0.094 Uiso 1 1 calc R . . H58B H -0.2178 -0.3751 0.0897 0.094 Uiso 1 1 calc R . . H58C H -0.1187 -0.4474 0.1205 0.094 Uiso 1 1 calc R . . C59 C -0.0245(14) -0.3004(8) 0.0290(4) 0.062(3) Uani 1 1 d . . . H59A H 0.0503 -0.2588 0.0234 0.093 Uiso 1 1 calc R . . H59B H -0.1145 -0.2632 0.0290 0.093 Uiso 1 1 calc R . . H59C H -0.0190 -0.3469 0.0027 0.093 Uiso 1 1 calc R . . C60 C 0.1250(13) -0.4149(9) 0.0769(5) 0.071(4) Uani 1 1 d . . . H60A H 0.2040 -0.3767 0.0714 0.106 Uiso 1 1 calc R . . H60B H 0.1236 -0.4587 0.0496 0.106 Uiso 1 1 calc R . . H60C H 0.1342 -0.4503 0.1081 0.106 Uiso 1 1 calc R . . C61 C 0.2543(10) -0.0019(7) 0.4412(4) 0.048(2) Uani 1 1 d . . . C62 C 0.2613(12) -0.0121(9) 0.4972(4) 0.059(3) Uani 1 1 d . . . H62A H 0.2012 -0.0602 0.5094 0.089 Uiso 1 1 calc R . . H62B H 0.2299 0.0480 0.5126 0.089 Uiso 1 1 calc R . . H62C H 0.3572 -0.0306 0.5056 0.089 Uiso 1 1 calc R . . C63 C 0.3367(12) 0.0817(8) 0.4238(4) 0.055(3) Uani 1 1 d . . . H63A H 0.4341 0.0687 0.4320 0.083 Uiso 1 1 calc R . . H63B H 0.2970 0.1388 0.4405 0.083 Uiso 1 1 calc R . . H63C H 0.3314 0.0904 0.3879 0.083 Uiso 1 1 calc R . . C64 C 0.1012(11) 0.0230(9) 0.4303(4) 0.060(3) Uani 1 1 d . . . H64A H 0.0943 0.0420 0.3955 0.090 Uiso 1 1 calc R . . H64B H 0.0625 0.0747 0.4514 0.090 Uiso 1 1 calc R . . H64C H 0.0489 -0.0320 0.4371 0.090 Uiso 1 1 calc R . . C65 C 0.4838(11) -0.3348(7) 0.4467(4) 0.051(3) Uani 1 1 d . . . C66 C 0.3758(18) -0.3652(11) 0.4822(7) 0.119(7) Uani 1 1 d . . . H66A H 0.3569 -0.3184 0.5082 0.178 Uiso 1 1 calc R . . H66B H 0.4078 -0.4258 0.4971 0.178 Uiso 1 1 calc R . . H66C H 0.2906 -0.3717 0.4650 0.178 Uiso 1 1 calc R . . C67 C 0.530(2) -0.4222(12) 0.4138(6) 0.127(8) Uani 1 1 d . . . H67A H 0.5671 -0.4743 0.4348 0.190 Uiso 1 1 calc R . . H67B H 0.6024 -0.4059 0.3892 0.190 Uiso 1 1 calc R . . H67C H 0.4502 -0.4412 0.3969 0.190 Uiso 1 1 calc R . . C68 C 0.6124(18) -0.3097(14) 0.4719(8) 0.136(9) Uani 1 1 d . . . H68A H 0.6684 -0.2728 0.4489 0.204 Uiso 1 1 calc R . . H68B H 0.6674 -0.3674 0.4815 0.204 Uiso 1 1 calc R . . H68C H 0.5842 -0.2729 0.5014 0.204 Uiso 1 1 calc R . . C69 C 0.761(3) 0.537(2) 0.2581(12) 0.237(16) Uiso 1 1 d D . . H69A H 0.7913 0.5844 0.2804 0.285 Uiso 1 1 calc R . . H69B H 0.8446 0.5016 0.2429 0.285 Uiso 1 1 calc R . . C70 C 0.671(3) 0.4705(18) 0.2869(9) 0.158(9) Uiso 1 1 d D . . H70A H 0.6563 0.4891 0.3219 0.190 Uiso 1 1 calc R . . H70B H 0.7141 0.4051 0.2855 0.190 Uiso 1 1 calc R . . C71 C 0.534(3) 0.481(2) 0.2600(11) 0.215(13) Uiso 1 1 d D . . H71A H 0.4595 0.5094 0.2828 0.258 Uiso 1 1 calc R . . H71B H 0.5094 0.4182 0.2512 0.258 Uiso 1 1 calc R . . C72 C 0.543(4) 0.543(3) 0.2126(13) 0.260(18) Uiso 1 1 d D . . H72A H 0.5467 0.5050 0.1823 0.312 Uiso 1 1 calc R . . H72B H 0.4646 0.5922 0.2117 0.312 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0326(2) 0.0317(2) 0.0319(2) 0.00236(17) -0.00263(17) -0.00535(17) Eu2 0.0375(3) 0.0360(2) 0.0365(2) 0.00706(18) -0.00278(18) -0.00477(18) O1 0.037(3) 0.033(3) 0.031(3) -0.005(2) -0.001(2) -0.008(2) O2 0.037(3) 0.028(3) 0.035(3) 0.003(2) 0.002(2) -0.008(2) O3 0.030(3) 0.033(3) 0.037(3) 0.002(2) -0.003(2) -0.006(2) O4 0.046(4) 0.038(3) 0.045(4) 0.013(3) -0.016(3) -0.006(3) N1 0.036(4) 0.029(3) 0.042(4) 0.011(3) -0.004(3) -0.001(3) N2 0.048(5) 0.043(4) 0.049(5) 0.015(4) -0.019(4) 0.001(4) N3 0.031(4) 0.036(4) 0.050(4) 0.014(3) -0.004(3) -0.008(3) N4 0.054(5) 0.048(5) 0.052(5) 0.018(4) 0.010(4) -0.013(4) C1 0.026(4) 0.037(4) 0.029(4) 0.009(3) 0.000(3) 0.000(3) C2 0.037(5) 0.037(4) 0.029(4) -0.001(3) -0.004(3) -0.003(4) C3 0.043(5) 0.043(5) 0.029(4) -0.004(4) 0.005(4) -0.005(4) C4 0.047(5) 0.037(5) 0.037(5) -0.010(4) -0.006(4) -0.003(4) C5 0.036(5) 0.041(5) 0.035(4) -0.003(4) -0.007(4) -0.008(4) C6 0.032(4) 0.032(4) 0.030(4) 0.003(3) -0.006(3) -0.005(3) C7 0.022(4) 0.033(4) 0.033(4) 0.000(3) 0.007(3) 0.001(3) C8 0.037(5) 0.032(4) 0.027(4) 0.004(3) -0.003(3) 0.000(3) C9 0.034(5) 0.043(5) 0.037(5) 0.007(4) -0.002(4) 0.004(4) C10 0.024(4) 0.034(4) 0.047(5) 0.010(4) 0.006(4) 0.005(3) C11 0.027(4) 0.046(5) 0.039(5) 0.002(4) 0.001(3) 0.000(4) C12 0.024(4) 0.037(4) 0.032(4) 0.007(3) 0.001(3) -0.001(3) C13 0.031(4) 0.039(4) 0.029(4) 0.002(3) -0.005(3) -0.003(3) C14 0.036(5) 0.039(5) 0.033(4) -0.002(4) 0.000(4) -0.003(4) C15 0.047(5) 0.032(4) 0.037(5) 0.002(4) 0.002(4) -0.005(4) C16 0.069(7) 0.036(5) 0.060(7) 0.016(5) 0.004(6) 0.011(5) C17 0.051(7) 0.089(10) 0.089(9) 0.025(8) -0.007(7) 0.010(7) C18 0.095(10) 0.050(6) 0.048(6) 0.005(5) 0.002(6) 0.014(6) C19 0.039(5) 0.046(5) 0.040(5) -0.009(4) -0.003(4) -0.007(4) C20 0.037(5) 0.071(7) 0.060(6) -0.008(6) 0.017(5) -0.003(5) C21 0.039(6) 0.073(7) 0.046(6) -0.003(5) -0.011(4) -0.010(5) C22 0.049(6) 0.056(6) 0.060(6) 0.013(5) -0.004(5) -0.015(5) C23 0.049(6) 0.053(6) 0.058(6) -0.030(5) 0.004(5) -0.002(5) C24 0.089(10) 0.057(7) 0.080(9) -0.033(7) 0.000(7) -0.004(7) C25 0.089(10) 0.074(8) 0.047(6) -0.018(6) -0.019(6) 0.000(7) C26 0.088(10) 0.078(9) 0.084(9) -0.048(7) -0.003(7) -0.027(7) C27 0.029(4) 0.054(6) 0.040(5) 0.004(4) -0.004(4) -0.007(4) C28 0.055(6) 0.061(6) 0.039(5) -0.002(5) 0.000(4) -0.008(5) C29 0.046(6) 0.044(5) 0.055(6) -0.009(5) -0.004(5) -0.006(4) C30 0.040(6) 0.068(7) 0.052(6) -0.015(5) -0.004(4) -0.008(5) C31 0.053(6) 0.039(5) 0.047(5) 0.006(4) 0.011(4) -0.005(4) C32 0.152(15) 0.042(7) 0.098(11) 0.016(7) 0.061(10) 0.009(8) C33 0.066(8) 0.157(15) 0.064(8) 0.052(9) -0.010(6) -0.064(9) C34 0.078(8) 0.059(7) 0.047(6) 0.016(5) -0.001(6) -0.017(6) C35 0.026(4) 0.035(4) 0.038(4) 0.009(4) -0.002(3) -0.011(3) C36 0.027(4) 0.021(3) 0.037(4) 0.003(3) -0.006(3) 0.000(3) C37 0.040(5) 0.042(5) 0.043(5) 0.002(4) -0.011(4) -0.003(4) C38 0.045(5) 0.037(5) 0.039(5) -0.001(4) 0.001(4) -0.010(4) C39 0.044(5) 0.034(4) 0.047(5) 0.000(4) -0.008(4) 0.002(4) C40 0.038(5) 0.035(4) 0.037(5) 0.004(4) -0.006(4) -0.005(4) C41 0.031(5) 0.040(5) 0.050(5) 0.012(4) -0.002(4) -0.007(4) C42 0.035(5) 0.041(5) 0.046(5) 0.007(4) -0.014(4) -0.005(4) C43 0.033(5) 0.054(6) 0.047(5) 0.017(5) -0.010(4) -0.004(4) C44 0.030(5) 0.045(5) 0.049(5) 0.020(4) -0.008(4) -0.004(4) C45 0.031(5) 0.040(5) 0.059(6) 0.005(4) -0.003(4) 0.000(4) C46 0.031(5) 0.051(5) 0.041(5) 0.013(4) -0.005(4) -0.003(4) C47 0.031(4) 0.029(4) 0.044(5) 0.002(4) -0.004(4) -0.004(3) C48 0.033(5) 0.049(5) 0.047(5) 0.012(4) -0.003(4) -0.002(4) C49 0.043(5) 0.042(5) 0.052(6) 0.009(4) -0.007(4) -0.012(4) C50 0.080(10) 0.071(9) 0.112(12) 0.027(8) -0.021(9) -0.019(7) C51 0.076(11) 0.106(13) 0.154(16) 0.047(12) -0.041(11) -0.037(9) C52 0.121(13) 0.097(11) 0.105(11) 0.054(9) -0.057(10) -0.071(10) C53 0.023(4) 0.039(4) 0.042(5) -0.001(4) 0.001(3) -0.002(3) C54 0.026(5) 0.050(6) 0.068(7) -0.004(5) -0.013(4) 0.005(4) C55 0.026(4) 0.054(6) 0.054(6) -0.005(5) 0.004(4) -0.004(4) C56 0.042(6) 0.043(5) 0.068(7) 0.005(5) 0.002(5) 0.005(4) C57 0.058(7) 0.044(5) 0.044(5) -0.009(4) -0.002(5) 0.008(5) C58 0.071(8) 0.049(6) 0.068(7) -0.018(5) -0.010(6) -0.005(6) C59 0.084(9) 0.058(7) 0.044(6) -0.012(5) 0.000(6) 0.003(6) C60 0.067(8) 0.071(8) 0.072(8) -0.032(7) -0.004(6) 0.013(6) C61 0.038(5) 0.050(6) 0.056(6) 0.013(5) -0.015(4) -0.011(4) C62 0.064(7) 0.069(7) 0.044(6) 0.005(5) -0.007(5) -0.001(6) C63 0.062(7) 0.054(6) 0.053(6) 0.004(5) -0.014(5) -0.015(5) C64 0.042(6) 0.069(7) 0.068(7) -0.004(6) -0.008(5) 0.000(5) C65 0.043(6) 0.053(6) 0.055(6) 0.021(5) -0.003(5) 0.006(5) C66 0.111(14) 0.083(11) 0.151(16) 0.067(11) 0.042(12) 0.012(10) C67 0.141(16) 0.121(14) 0.098(12) 0.047(11) 0.020(11) 0.080(13) C68 0.092(13) 0.138(16) 0.19(2) 0.090(15) -0.081(13) -0.033(11) _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 Eu1 O2 2.312(6) . ? Eu1 O1 2.400(5) . ? Eu1 O3 2.457(5) . ? Eu1 N1 2.656(7) . ? Eu1 N2 2.680(8) . ? Eu1 C7 3.037(7) . ? Eu1 Eu2 3.7697(7) . ? Eu2 O4 2.313(6) . ? Eu2 O3 2.406(6) . ? Eu2 O1 2.459(6) . ? Eu2 N3 2.663(8) . ? Eu2 N4 2.683(8) . ? Eu2 C41 3.014(9) . ? O1 C1 1.352(10) . ? O2 C7 1.326(9) . ? O3 C35 1.353(10) . ? O4 C41 1.335(10) . ? O5 C69 1.468(18) . ? O5 C72 1.472(18) . ? N1 C15 1.482(10) . ? N1 C13 1.497(10) . ? N1 C14 1.502(11) . ? N2 C18 1.439(13) . ? N2 C17 1.468(14) . ? N2 C16 1.494(14) . ? N3 C49 1.466(11) . ? N3 C47 1.486(11) . ? N3 C48 1.506(11) . ? N4 C52 1.412(15) . ? N4 C51 1.446(16) . ? N4 C50 1.505(18) . ? C1 C6 1.398(11) . ? C1 C2 1.414(11) . ? C2 C3 1.402(12) . ? C2 C19 1.525(13) . ? C3 C4 1.387(13) . ? C3 H3 0.9500 . ? C4 C5 1.393(13) . ? C4 C23 1.551(12) . ? C5 C6 1.395(12) . ? C5 H5 0.9500 . ? C6 C13 1.507(12) . ? C7 C12 1.402(11) . ? C7 C8 1.418(11) . ? C8 C9 1.394(12) . ? C8 C27 1.535(12) . ? C9 C10 1.395(13) . ? C9 H9 0.9500 . ? C10 C11 1.394(12) . ? C10 C31 1.535(12) . ? C11 C12 1.376(12) . ? C11 H11 0.9500 . ? C12 C14 1.524(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.503(14) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C21 1.525(13) . ? C19 C20 1.542(13) . ? C19 C22 1.550(14) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C26 1.510(16) . ? C23 C24 1.513(16) . ? C23 C25 1.562(16) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.526(13) . ? C27 C29 1.541(13) . ? C27 C30 1.548(13) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.490(16) . ? C31 C32 1.514(15) . ? C31 C34 1.515(14) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C40 1.391(12) . ? C35 C36 1.432(11) . ? C36 C37 1.386(12) . ? C36 C53 1.535(11) . ? C37 C38 1.382(13) . ? C37 H37 0.9500 . ? C38 C39 1.396(13) . ? C38 C57 1.530(13) . ? C39 C40 1.404(12) . ? C39 H39 0.9500 . ? C40 C47 1.504(11) . ? C41 C46 1.398(13) . ? C41 C42 1.445(13) . ? C42 C43 1.413(12) . ? C42 C61 1.533(14) . ? C43 C44 1.394(14) . ? C43 H43 0.9500 . ? C44 C45 1.383(14) . ? C44 C65 1.522(12) . ? C45 C46 1.387(13) . ? C45 H45 0.9500 . ? C46 C48 1.502(13) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.472(17) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.538(12) . ? C53 C55 1.543(12) . ? C53 C56 1.548(13) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C60 1.520(15) . ? C57 C58 1.535(16) . ? C57 C59 1.538(15) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.523(14) . ? C61 C64 1.536(14) . ? C61 C63 1.545(14) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.470(17) . ? C65 C68 1.522(18) . ? C65 C67 1.57(2) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C70 1.517(18) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.540(17) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.545(18) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? 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 O2 Eu1 O1 126.4(2) . . ? O2 Eu1 O3 93.16(19) . . ? O1 Eu1 O3 70.75(19) . . ? O2 Eu1 N1 77.4(2) . . ? O1 Eu1 N1 76.3(2) . . ? O3 Eu1 N1 130.19(19) . . ? O2 Eu1 N2 115.6(2) . . ? O1 Eu1 N2 97.3(2) . . ? O3 Eu1 N2 149.6(2) . . ? N1 Eu1 N2 69.5(2) . . ? O2 Eu1 C7 24.2(2) . . ? O1 Eu1 C7 137.0(2) . . ? O3 Eu1 C7 116.6(2) . . ? N1 Eu1 C7 67.6(2) . . ? N2 Eu1 C7 91.4(2) . . ? O2 Eu1 Eu2 97.34(14) . . ? O1 Eu1 Eu2 39.70(13) . . ? O3 Eu1 Eu2 38.68(13) . . ? N1 Eu1 Eu2 93.44(15) . . ? N2 Eu1 Eu2 136.98(19) . . ? C7 Eu1 Eu2 118.97(15) . . ? O4 Eu2 O3 125.9(2) . . ? O4 Eu2 O1 91.9(2) . . ? O3 Eu2 O1 70.62(18) . . ? O4 Eu2 N3 79.3(2) . . ? O3 Eu2 N3 75.9(2) . . ? O1 Eu2 N3 130.5(2) . . ? O4 Eu2 N4 114.4(2) . . ? O3 Eu2 N4 100.5(2) . . ? O1 Eu2 N4 151.0(2) . . ? N3 Eu2 N4 69.5(2) . . ? O4 Eu2 C41 24.8(2) . . ? O3 Eu2 C41 136.4(2) . . ? O1 Eu2 C41 116.2(2) . . ? N3 Eu2 C41 68.2(2) . . ? N4 Eu2 C41 89.6(3) . . ? O4 Eu2 Eu1 96.32(15) . . ? O3 Eu2 Eu1 39.67(13) . . ? O1 Eu2 Eu1 38.57(13) . . ? N3 Eu2 Eu1 93.67(15) . . ? N4 Eu2 Eu1 140.2(2) . . ? C41 Eu2 Eu1 118.19(16) . . ? C1 O1 Eu1 131.0(5) . . ? C1 O1 Eu2 119.0(5) . . ? Eu1 O1 Eu2 101.7(2) . . ? C7 O2 Eu1 110.2(5) . . ? C35 O3 Eu2 130.1(5) . . ? C35 O3 Eu1 120.4(5) . . ? Eu2 O3 Eu1 101.6(2) . . ? C41 O4 Eu2 108.5(5) . . ? C69 O5 C72 116(3) . . ? C15 N1 C13 110.8(7) . . ? C15 N1 C14 110.1(7) . . ? C13 N1 C14 105.8(6) . . ? C15 N1 Eu1 111.1(5) . . ? C13 N1 Eu1 109.8(5) . . ? C14 N1 Eu1 109.1(5) . . ? C18 N2 C17 109.4(9) . . ? C18 N2 C16 112.7(9) . . ? C17 N2 C16 105.4(9) . . ? C18 N2 Eu1 111.5(6) . . ? C17 N2 Eu1 112.9(7) . . ? C16 N2 Eu1 104.6(5) . . ? C49 N3 C47 112.4(7) . . ? C49 N3 C48 110.1(7) . . ? C47 N3 C48 106.3(7) . . ? C49 N3 Eu2 110.8(6) . . ? C47 N3 Eu2 110.9(5) . . ? C48 N3 Eu2 106.2(5) . . ? C52 N4 C51 109.0(11) . . ? C52 N4 C50 118.9(12) . . ? C51 N4 C50 102.4(12) . . ? C52 N4 Eu2 114.0(7) . . ? C51 N4 Eu2 111.4(8) . . ? C50 N4 Eu2 100.3(6) . . ? O1 C1 C6 119.0(7) . . ? O1 C1 C2 121.4(7) . . ? C6 C1 C2 119.6(8) . . ? C3 C2 C1 116.7(8) . . ? C3 C2 C19 120.1(8) . . ? C1 C2 C19 123.2(8) . . ? C4 C3 C2 124.8(8) . . ? C4 C3 H3 117.6 . . ? C2 C3 H3 117.6 . . ? C3 C4 C5 116.9(8) . . ? C3 C4 C23 120.1(8) . . ? C5 C4 C23 122.9(8) . . ? C4 C5 C6 120.8(8) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 121.2(8) . . ? C5 C6 C13 117.7(7) . . ? C1 C6 C13 121.0(7) . . ? O2 C7 C12 118.4(7) . . ? O2 C7 C8 123.5(7) . . ? C12 C7 C8 118.1(7) . . ? O2 C7 Eu1 45.6(4) . . ? C12 C7 Eu1 99.5(5) . . ? C8 C7 Eu1 122.0(5) . . ? C9 C8 C7 118.3(8) . . ? C9 C8 C27 121.9(7) . . ? C7 C8 C27 119.8(7) . . ? C8 C9 C10 123.8(8) . . ? C8 C9 H9 118.1 . . ? C10 C9 H9 118.1 . . ? C11 C10 C9 116.6(8) . . ? C11 C10 C31 121.0(8) . . ? C9 C10 C31 122.3(8) . . ? C12 C11 C10 121.5(9) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C12 C7 121.7(8) . . ? C11 C12 C14 119.3(8) . . ? C7 C12 C14 118.9(7) . . ? N1 C13 C6 117.0(7) . . ? N1 C13 H13A 108.1 . . ? C6 C13 H13A 108.1 . . ? N1 C13 H13B 108.1 . . ? C6 C13 H13B 108.1 . . ? H13A C13 H13B 107.3 . . ? N1 C14 C12 112.8(7) . . ? N1 C14 H14A 109.0 . . ? C12 C14 H14A 109.0 . . ? N1 C14 H14B 109.0 . . ? C12 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? N1 C15 C16 115.3(8) . . ? N1 C15 H15A 108.4 . . ? C16 C15 H15A 108.4 . . ? N1 C15 H15B 108.4 . . ? C16 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? N2 C16 C15 114.3(8) . . ? N2 C16 H16A 108.7 . . ? C15 C16 H16A 108.7 . . ? N2 C16 H16B 108.7 . . ? C15 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C2 C19 C21 109.7(8) . . ? C2 C19 C20 112.0(8) . . ? C21 C19 C20 107.5(8) . . ? C2 C19 C22 111.1(8) . . ? C21 C19 C22 108.1(8) . . ? C20 C19 C22 108.3(8) . . ? 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 . . ? C26 C23 C24 108.0(10) . . ? C26 C23 C4 112.7(9) . . ? C24 C23 C4 108.6(9) . . ? C26 C23 C25 109.9(10) . . ? C24 C23 C25 110.4(10) . . ? C4 C23 C25 107.2(9) . . ? 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 . . ? C28 C27 C8 111.9(8) . . ? C28 C27 C29 108.7(8) . . ? C8 C27 C29 110.8(7) . . ? C28 C27 C30 107.1(8) . . ? C8 C27 C30 109.9(8) . . ? C29 C27 C30 108.3(8) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C32 111.9(12) . . ? C33 C31 C34 107.3(9) . . ? C32 C31 C34 105.8(10) . . ? C33 C31 C10 110.2(9) . . ? C32 C31 C10 107.4(8) . . ? C34 C31 C10 114.3(8) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O3 C35 C40 119.7(7) . . ? O3 C35 C36 121.4(7) . . ? C40 C35 C36 118.9(8) . . ? C37 C36 C35 117.1(7) . . ? C37 C36 C53 121.8(7) . . ? C35 C36 C53 121.0(7) . . ? C38 C37 C36 125.6(8) . . ? C38 C37 H37 117.2 . . ? C36 C37 H37 117.2 . . ? C37 C38 C39 115.6(8) . . ? C37 C38 C57 121.3(9) . . ? C39 C38 C57 123.1(9) . . ? C38 C39 C40 122.0(9) . . ? C38 C39 H39 119.0 . . ? C40 C39 H39 119.0 . . ? C35 C40 C39 120.4(8) . . ? C35 C40 C47 121.2(8) . . ? C39 C40 C47 118.1(8) . . ? O4 C41 C46 120.9(8) . . ? O4 C41 C42 121.0(8) . . ? C46 C41 C42 118.1(8) . . ? O4 C41 Eu2 46.7(4) . . ? C46 C41 Eu2 99.6(6) . . ? C42 C41 Eu2 122.4(6) . . ? C43 C42 C41 118.0(9) . . ? C43 C42 C61 120.2(9) . . ? C41 C42 C61 121.8(8) . . ? C44 C43 C42 123.0(9) . . ? C44 C43 H43 118.5 . . ? C42 C43 H43 118.5 . . ? C45 C44 C43 117.4(8) . . ? C45 C44 C65 122.5(9) . . ? C43 C44 C65 120.1(9) . . ? C44 C45 C46 122.2(9) . . ? C44 C45 H45 118.9 . . ? C46 C45 H45 118.9 . . ? C45 C46 C41 121.3(9) . . ? C45 C46 C48 121.4(9) . . ? C41 C46 C48 117.4(8) . . ? N3 C47 C40 116.0(7) . . ? N3 C47 H47A 108.3 . . ? C40 C47 H47A 108.3 . . ? N3 C47 H47B 108.3 . . ? C40 C47 H47B 108.3 . . ? H47A C47 H47B 107.4 . . ? C46 C48 N3 114.7(8) . . ? C46 C48 H48A 108.6 . . ? N3 C48 H48A 108.6 . . ? C46 C48 H48B 108.6 . . ? N3 C48 H48B 108.6 . . ? H48A C48 H48B 107.6 . . ? N3 C49 C50 112.8(9) . . ? N3 C49 H49A 109.0 . . ? C50 C49 H49A 109.0 . . ? N3 C49 H49B 109.0 . . ? C50 C49 H49B 109.0 . . ? H49A C49 H49B 107.8 . . ? C49 C50 N4 115.6(11) . . ? C49 C50 H50A 108.4 . . ? N4 C50 H50A 108.4 . . ? C49 C50 H50B 108.4 . . ? N4 C50 H50B 108.4 . . ? H50A C50 H50B 107.4 . . ? N4 C51 H51A 109.5 . . ? N4 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N4 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N4 C52 H52A 109.5 . . ? N4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C36 C53 C54 112.9(7) . . ? C36 C53 C55 110.1(7) . . ? C54 C53 C55 106.0(7) . . ? C36 C53 C56 112.6(7) . . ? C54 C53 C56 106.7(8) . . ? C55 C53 C56 108.2(8) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C60 C57 C38 112.8(9) . . ? C60 C57 C58 107.4(9) . . ? C38 C57 C58 109.9(8) . . ? C60 C57 C59 108.3(9) . . ? C38 C57 C59 109.1(8) . . ? C58 C57 C59 109.3(9) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 C42 113.6(8) . . ? C62 C61 C64 107.0(9) . . ? C42 C61 C64 111.1(8) . . ? C62 C61 C63 108.3(9) . . ? C42 C61 C63 108.6(9) . . ? C64 C61 C63 108.0(9) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 C68 112.5(14) . . ? C66 C65 C44 110.0(10) . . ? C68 C65 C44 110.0(10) . . ? C66 C65 C67 105.9(12) . . ? C68 C65 C67 106.6(13) . . ? C44 C65 C67 111.9(9) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O5 C69 C70 107(2) . . ? O5 C69 H69A 110.3 . . ? C70 C69 H69A 110.3 . . ? O5 C69 H69B 110.3 . . ? C70 C69 H69B 110.3 . . ? H69A C69 H69B 108.6 . . ? C69 C70 C71 103(2) . . ? C69 C70 H70A 111.1 . . ? C71 C70 H70A 111.1 . . ? C69 C70 H70B 111.1 . . ? C71 C70 H70B 111.1 . . ? H70A C70 H70B 109.1 . . ? C70 C71 C72 113(3) . . ? C70 C71 H71A 109.0 . . ? C72 C71 H71A 109.0 . . ? C70 C71 H71B 109.0 . . ? C72 C71 H71B 109.0 . . ? H71A C71 H71B 107.8 . . ? O5 C72 C71 99(2) . . ? O5 C72 H72A 111.9 . . ? C71 C72 H72A 111.9 . . ? O5 C72 H72B 111.9 . . ? C71 C72 H72B 111.9 . . ? H72A C72 H72B 109.6 . . ? 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 O2 Eu1 Eu2 O4 56.4(2) . . . . ? O1 Eu1 Eu2 O4 -85.0(3) . . . . ? O3 Eu1 Eu2 O4 142.3(3) . . . . ? N1 Eu1 Eu2 O4 -21.3(2) . . . . ? N2 Eu1 Eu2 O4 -84.5(3) . . . . ? C7 Eu1 Eu2 O4 44.9(2) . . . . ? O2 Eu1 Eu2 O3 -85.9(3) . . . . ? O1 Eu1 Eu2 O3 132.7(3) . . . . ? N1 Eu1 Eu2 O3 -163.6(3) . . . . ? N2 Eu1 Eu2 O3 133.2(3) . . . . ? C7 Eu1 Eu2 O3 -97.4(3) . . . . ? O2 Eu1 Eu2 O1 141.4(3) . . . . ? O3 Eu1 Eu2 O1 -132.7(3) . . . . ? N1 Eu1 Eu2 O1 63.7(3) . . . . ? N2 Eu1 Eu2 O1 0.5(3) . . . . ? C7 Eu1 Eu2 O1 129.9(3) . . . . ? O2 Eu1 Eu2 N3 -23.2(2) . . . . ? O1 Eu1 Eu2 N3 -164.6(3) . . . . ? O3 Eu1 Eu2 N3 62.6(3) . . . . ? N1 Eu1 Eu2 N3 -100.9(2) . . . . ? N2 Eu1 Eu2 N3 -164.2(3) . . . . ? C7 Eu1 Eu2 N3 -34.7(2) . . . . ? O2 Eu1 Eu2 N4 -85.2(3) . . . . ? O1 Eu1 Eu2 N4 133.4(4) . . . . ? O3 Eu1 Eu2 N4 0.7(4) . . . . ? N1 Eu1 Eu2 N4 -162.9(3) . . . . ? N2 Eu1 Eu2 N4 133.9(4) . . . . ? C7 Eu1 Eu2 N4 -96.7(4) . . . . ? O2 Eu1 Eu2 C41 43.9(3) . . . . ? O1 Eu1 Eu2 C41 -97.5(3) . . . . ? O3 Eu1 Eu2 C41 129.8(3) . . . . ? N1 Eu1 Eu2 C41 -33.8(3) . . . . ? N2 Eu1 Eu2 C41 -97.0(3) . . . . ? C7 Eu1 Eu2 C41 32.4(3) . . . . ? O2 Eu1 O1 C1 96.5(7) . . . . ? O3 Eu1 O1 C1 175.8(7) . . . . ? N1 Eu1 O1 C1 33.8(6) . . . . ? N2 Eu1 O1 C1 -32.9(7) . . . . ? C7 Eu1 O1 C1 67.1(7) . . . . ? Eu2 Eu1 O1 C1 146.7(7) . . . . ? O2 Eu1 O1 Eu2 -50.2(3) . . . . ? O3 Eu1 O1 Eu2 29.11(19) . . . . ? N1 Eu1 O1 Eu2 -112.9(2) . . . . ? N2 Eu1 O1 Eu2 -179.7(2) . . . . ? C7 Eu1 O1 Eu2 -79.7(3) . . . . ? O4 Eu2 O1 C1 -53.9(5) . . . . ? O3 Eu2 O1 C1 178.4(6) . . . . ? N3 Eu2 O1 C1 -131.4(5) . . . . ? N4 Eu2 O1 C1 102.1(7) . . . . ? C41 Eu2 O1 C1 -48.6(6) . . . . ? Eu1 Eu2 O1 C1 -151.8(6) . . . . ? O4 Eu2 O1 Eu1 97.8(2) . . . . ? O3 Eu2 O1 Eu1 -29.81(19) . . . . ? N3 Eu2 O1 Eu1 20.4(3) . . . . ? N4 Eu2 O1 Eu1 -106.2(5) . . . . ? C41 Eu2 O1 Eu1 103.2(3) . . . . ? O1 Eu1 O2 C7 -125.2(5) . . . . ? O3 Eu1 O2 C7 166.5(5) . . . . ? N1 Eu1 O2 C7 -62.9(5) . . . . ? N2 Eu1 O2 C7 -3.3(6) . . . . ? Eu2 Eu1 O2 C7 -154.8(5) . . . . ? O4 Eu2 O3 C35 99.6(6) . . . . ? O1 Eu2 O3 C35 177.3(7) . . . . ? N3 Eu2 O3 C35 34.3(6) . . . . ? N4 Eu2 O3 C35 -31.3(7) . . . . ? C41 Eu2 O3 C35 69.3(7) . . . . ? Eu1 Eu2 O3 C35 148.2(7) . . . . ? O4 Eu2 O3 Eu1 -48.7(3) . . . . ? O1 Eu2 O3 Eu1 29.05(19) . . . . ? N3 Eu2 O3 Eu1 -114.0(2) . . . . ? N4 Eu2 O3 Eu1 -179.5(2) . . . . ? C41 Eu2 O3 Eu1 -78.9(3) . . . . ? O2 Eu1 O3 C35 -54.4(6) . . . . ? O1 Eu1 O3 C35 178.0(6) . . . . ? N1 Eu1 O3 C35 -130.5(5) . . . . ? N2 Eu1 O3 C35 107.3(6) . . . . ? C7 Eu1 O3 C35 -48.2(6) . . . . ? Eu2 Eu1 O3 C35 -152.2(6) . . . . ? O2 Eu1 O3 Eu2 97.8(2) . . . . ? O1 Eu1 O3 Eu2 -29.8(2) . . . . ? N1 Eu1 O3 Eu2 21.7(3) . . . . ? N2 Eu1 O3 Eu2 -100.5(4) . . . . ? C7 Eu1 O3 Eu2 103.9(2) . . . . ? O3 Eu2 O4 C41 -124.3(6) . . . . ? O1 Eu2 O4 C41 168.5(6) . . . . ? N3 Eu2 O4 C41 -60.6(6) . . . . ? N4 Eu2 O4 C41 1.0(7) . . . . ? Eu1 Eu2 O4 C41 -153.1(6) . . . . ? O2 Eu1 N1 C15 125.1(6) . . . . ? O1 Eu1 N1 C15 -102.1(6) . . . . ? O3 Eu1 N1 C15 -151.5(5) . . . . ? N2 Eu1 N1 C15 1.3(5) . . . . ? C7 Eu1 N1 C15 101.8(6) . . . . ? Eu2 Eu1 N1 C15 -138.2(5) . . . . ? O2 Eu1 N1 C13 -112.0(5) . . . . ? O1 Eu1 N1 C13 20.9(5) . . . . ? O3 Eu1 N1 C13 -28.6(6) . . . . ? N2 Eu1 N1 C13 124.2(5) . . . . ? C7 Eu1 N1 C13 -135.2(5) . . . . ? Eu2 Eu1 N1 C13 -15.2(5) . . . . ? O2 Eu1 N1 C14 3.5(5) . . . . ? O1 Eu1 N1 C14 136.4(5) . . . . ? O3 Eu1 N1 C14 86.9(5) . . . . ? N2 Eu1 N1 C14 -120.3(5) . . . . ? C7 Eu1 N1 C14 -19.7(5) . . . . ? Eu2 Eu1 N1 C14 100.3(5) . . . . ? O2 Eu1 N2 C18 31.5(8) . . . . ? O1 Eu1 N2 C18 168.0(7) . . . . ? O3 Eu1 N2 C18 -128.1(8) . . . . ? N1 Eu1 N2 C18 95.6(8) . . . . ? C7 Eu1 N2 C18 30.2(8) . . . . ? Eu2 Eu1 N2 C18 167.7(7) . . . . ? O2 Eu1 N2 C17 155.3(8) . . . . ? O1 Eu1 N2 C17 -68.3(8) . . . . ? O3 Eu1 N2 C17 -4.3(10) . . . . ? N1 Eu1 N2 C17 -140.7(8) . . . . ? C7 Eu1 N2 C17 153.9(8) . . . . ? Eu2 Eu1 N2 C17 -68.6(8) . . . . ? O2 Eu1 N2 C16 -90.6(6) . . . . ? O1 Eu1 N2 C16 45.8(6) . . . . ? O3 Eu1 N2 C16 109.7(7) . . . . ? N1 Eu1 N2 C16 -26.6(6) . . . . ? C7 Eu1 N2 C16 -92.0(6) . . . . ? Eu2 Eu1 N2 C16 45.5(7) . . . . ? O4 Eu2 N3 C49 123.3(6) . . . . ? O3 Eu2 N3 C49 -105.2(6) . . . . ? O1 Eu2 N3 C49 -153.5(5) . . . . ? N4 Eu2 N3 C49 2.0(6) . . . . ? C41 Eu2 N3 C49 100.1(6) . . . . ? Eu1 Eu2 N3 C49 -140.9(6) . . . . ? O4 Eu2 N3 C47 -111.2(5) . . . . ? O3 Eu2 N3 C47 20.3(5) . . . . ? O1 Eu2 N3 C47 -28.0(6) . . . . ? N4 Eu2 N3 C47 127.4(6) . . . . ? C41 Eu2 N3 C47 -134.4(5) . . . . ? Eu1 Eu2 N3 C47 -15.5(5) . . . . ? O4 Eu2 N3 C48 3.8(5) . . . . ? O3 Eu2 N3 C48 135.3(5) . . . . ? O1 Eu2 N3 C48 87.0(5) . . . . ? N4 Eu2 N3 C48 -117.5(6) . . . . ? C41 Eu2 N3 C48 -19.4(5) . . . . ? Eu1 Eu2 N3 C48 99.5(5) . . . . ? O4 Eu2 N4 C52 32.8(11) . . . . ? O3 Eu2 N4 C52 170.5(10) . . . . ? O1 Eu2 N4 C52 -120.7(10) . . . . ? N3 Eu2 N4 C52 100.0(11) . . . . ? C41 Eu2 N4 C52 33.2(11) . . . . ? Eu1 Eu2 N4 C52 170.0(9) . . . . ? O4 Eu2 N4 C51 156.7(10) . . . . ? O3 Eu2 N4 C51 -65.5(10) . . . . ? O1 Eu2 N4 C51 3.3(13) . . . . ? N3 Eu2 N4 C51 -136.0(11) . . . . ? C41 Eu2 N4 C51 157.1(10) . . . . ? Eu1 Eu2 N4 C51 -66.0(11) . . . . ? O4 Eu2 N4 C50 -95.4(7) . . . . ? O3 Eu2 N4 C50 42.3(7) . . . . ? O1 Eu2 N4 C50 111.1(8) . . . . ? N3 Eu2 N4 C50 -28.2(7) . . . . ? C41 Eu2 N4 C50 -95.0(7) . . . . ? Eu1 Eu2 N4 C50 41.9(8) . . . . ? Eu1 O1 C1 C6 -50.0(10) . . . . ? Eu2 O1 C1 C6 92.2(7) . . . . ? Eu1 O1 C1 C2 131.2(7) . . . . ? Eu2 O1 C1 C2 -86.7(8) . . . . ? O1 C1 C2 C3 175.8(7) . . . . ? C6 C1 C2 C3 -3.0(12) . . . . ? O1 C1 C2 C19 -4.6(12) . . . . ? C6 C1 C2 C19 176.6(8) . . . . ? C1 C2 C3 C4 2.0(13) . . . . ? C19 C2 C3 C4 -177.6(9) . . . . ? C2 C3 C4 C5 0.6(14) . . . . ? C2 C3 C4 C23 -176.2(9) . . . . ? C3 C4 C5 C6 -2.2(13) . . . . ? C23 C4 C5 C6 174.5(9) . . . . ? C4 C5 C6 C1 1.2(13) . . . . ? C4 C5 C6 C13 -175.0(8) . . . . ? O1 C1 C6 C5 -177.3(7) . . . . ? C2 C1 C6 C5 1.5(12) . . . . ? O1 C1 C6 C13 -1.3(11) . . . . ? C2 C1 C6 C13 177.6(7) . . . . ? Eu1 O2 C7 C12 74.5(8) . . . . ? Eu1 O2 C7 C8 -103.8(7) . . . . ? O1 Eu1 C7 O2 74.7(6) . . . . ? O3 Eu1 C7 O2 -15.1(6) . . . . ? N1 Eu1 C7 O2 110.0(5) . . . . ? N2 Eu1 C7 O2 177.0(5) . . . . ? Eu2 Eu1 C7 O2 28.8(5) . . . . ? O2 Eu1 C7 C12 -120.7(8) . . . . ? O1 Eu1 C7 C12 -46.0(6) . . . . ? O3 Eu1 C7 C12 -135.8(5) . . . . ? N1 Eu1 C7 C12 -10.8(5) . . . . ? N2 Eu1 C7 C12 56.3(5) . . . . ? Eu2 Eu1 C7 C12 -91.9(5) . . . . ? O2 Eu1 C7 C8 107.5(8) . . . . ? O1 Eu1 C7 C8 -177.8(5) . . . . ? O3 Eu1 C7 C8 92.4(6) . . . . ? N1 Eu1 C7 C8 -142.6(7) . . . . ? N2 Eu1 C7 C8 -75.5(6) . . . . ? Eu2 Eu1 C7 C8 136.3(6) . . . . ? O2 C7 C8 C9 177.1(8) . . . . ? C12 C7 C8 C9 -1.2(12) . . . . ? Eu1 C7 C8 C9 122.3(7) . . . . ? O2 C7 C8 C27 -0.7(12) . . . . ? C12 C7 C8 C27 -179.1(7) . . . . ? Eu1 C7 C8 C27 -55.5(9) . . . . ? C7 C8 C9 C10 1.4(13) . . . . ? C27 C8 C9 C10 179.2(8) . . . . ? C8 C9 C10 C11 -0.7(13) . . . . ? C8 C9 C10 C31 -177.0(8) . . . . ? C9 C10 C11 C12 -0.2(12) . . . . ? C31 C10 C11 C12 176.2(8) . . . . ? C10 C11 C12 C7 0.3(13) . . . . ? C10 C11 C12 C14 -177.0(8) . . . . ? O2 C7 C12 C11 -178.0(7) . . . . ? C8 C7 C12 C11 0.5(12) . . . . ? Eu1 C7 C12 C11 -133.7(7) . . . . ? O2 C7 C12 C14 -0.7(11) . . . . ? C8 C7 C12 C14 177.7(7) . . . . ? Eu1 C7 C12 C14 43.5(8) . . . . ? C15 N1 C13 C6 56.0(9) . . . . ? C14 N1 C13 C6 175.3(7) . . . . ? Eu1 N1 C13 C6 -67.1(8) . . . . ? C5 C6 C13 N1 -117.1(8) . . . . ? C1 C6 C13 N1 66.7(10) . . . . ? C15 N1 C14 C12 -71.4(9) . . . . ? C13 N1 C14 C12 168.8(7) . . . . ? Eu1 N1 C14 C12 50.8(8) . . . . ? C11 C12 C14 N1 105.3(9) . . . . ? C7 C12 C14 N1 -72.0(10) . . . . ? C13 N1 C15 C16 -96.5(9) . . . . ? C14 N1 C15 C16 146.9(8) . . . . ? Eu1 N1 C15 C16 25.9(9) . . . . ? C18 N2 C16 C15 -68.5(11) . . . . ? C17 N2 C16 C15 172.2(9) . . . . ? Eu1 N2 C16 C15 52.9(9) . . . . ? N1 C15 C16 N2 -57.2(11) . . . . ? C3 C2 C19 C21 121.7(9) . . . . ? C1 C2 C19 C21 -58.0(11) . . . . ? C3 C2 C19 C20 2.4(12) . . . . ? C1 C2 C19 C20 -177.3(8) . . . . ? C3 C2 C19 C22 -118.8(9) . . . . ? C1 C2 C19 C22 61.5(11) . . . . ? C3 C4 C23 C26 -173.5(10) . . . . ? C5 C4 C23 C26 9.9(15) . . . . ? C3 C4 C23 C24 -53.9(13) . . . . ? C5 C4 C23 C24 129.5(11) . . . . ? C3 C4 C23 C25 65.4(12) . . . . ? C5 C4 C23 C25 -111.2(11) . . . . ? C9 C8 C27 C28 3.2(12) . . . . ? C7 C8 C27 C28 -179.1(8) . . . . ? C9 C8 C27 C29 124.6(9) . . . . ? C7 C8 C27 C29 -57.6(11) . . . . ? C9 C8 C27 C30 -115.7(9) . . . . ? C7 C8 C27 C30 62.1(10) . . . . ? C11 C10 C31 C33 60.1(13) . . . . ? C9 C10 C31 C33 -123.7(11) . . . . ? C11 C10 C31 C32 -61.9(13) . . . . ? C9 C10 C31 C32 114.2(12) . . . . ? C11 C10 C31 C34 -179.0(9) . . . . ? C9 C10 C31 C34 -2.8(13) . . . . ? Eu2 O3 C35 C40 -49.8(10) . . . . ? Eu1 O3 C35 C40 93.4(8) . . . . ? Eu2 O3 C35 C36 128.3(7) . . . . ? Eu1 O3 C35 C36 -88.4(8) . . . . ? O3 C35 C36 C37 175.6(7) . . . . ? C40 C35 C36 C37 -6.2(12) . . . . ? O3 C35 C36 C53 -1.6(12) . . . . ? C40 C35 C36 C53 176.6(7) . . . . ? C35 C36 C37 C38 2.9(13) . . . . ? C53 C36 C37 C38 -179.9(8) . . . . ? C36 C37 C38 C39 1.0(14) . . . . ? C36 C37 C38 C57 -176.6(9) . . . . ? C37 C38 C39 C40 -1.6(14) . . . . ? C57 C38 C39 C40 176.0(9) . . . . ? O3 C35 C40 C39 -176.0(8) . . . . ? C36 C35 C40 C39 5.8(12) . . . . ? O3 C35 C40 C47 -2.5(12) . . . . ? C36 C35 C40 C47 179.3(7) . . . . ? C38 C39 C40 C35 -1.8(14) . . . . ? C38 C39 C40 C47 -175.6(8) . . . . ? Eu2 O4 C41 C46 72.6(9) . . . . ? Eu2 O4 C41 C42 -107.0(8) . . . . ? O3 Eu2 C41 O4 76.0(7) . . . . ? O1 Eu2 C41 O4 -12.9(7) . . . . ? N3 Eu2 C41 O4 112.8(6) . . . . ? N4 Eu2 C41 O4 -179.1(6) . . . . ? Eu1 Eu2 C41 O4 30.7(6) . . . . ? O4 Eu2 C41 C46 -123.9(9) . . . . ? O3 Eu2 C41 C46 -47.9(7) . . . . ? O1 Eu2 C41 C46 -136.7(5) . . . . ? N3 Eu2 C41 C46 -11.0(5) . . . . ? N4 Eu2 C41 C46 57.0(6) . . . . ? Eu1 Eu2 C41 C46 -93.2(5) . . . . ? O4 Eu2 C41 C42 103.9(10) . . . . ? O3 Eu2 C41 C42 179.9(6) . . . . ? O1 Eu2 C41 C42 91.1(7) . . . . ? N3 Eu2 C41 C42 -143.2(7) . . . . ? N4 Eu2 C41 C42 -75.2(7) . . . . ? Eu1 Eu2 C41 C42 134.6(6) . . . . ? O4 C41 C42 C43 179.5(8) . . . . ? C46 C41 C42 C43 -0.1(13) . . . . ? Eu2 C41 C42 C43 124.0(8) . . . . ? O4 C41 C42 C61 1.0(13) . . . . ? C46 C41 C42 C61 -178.6(8) . . . . ? Eu2 C41 C42 C61 -54.5(10) . . . . ? C41 C42 C43 C44 -0.1(14) . . . . ? C61 C42 C43 C44 178.5(8) . . . . ? C42 C43 C44 C45 1.6(14) . . . . ? C42 C43 C44 C65 -178.9(9) . . . . ? C43 C44 C45 C46 -3.1(14) . . . . ? C65 C44 C45 C46 177.5(9) . . . . ? C44 C45 C46 C41 3.1(14) . . . . ? C44 C45 C46 C48 -177.0(8) . . . . ? O4 C41 C46 C45 179.0(8) . . . . ? C42 C41 C46 C45 -1.4(13) . . . . ? Eu2 C41 C46 C45 -136.2(8) . . . . ? O4 C41 C46 C48 -1.0(13) . . . . ? C42 C41 C46 C48 178.6(8) . . . . ? Eu2 C41 C46 C48 43.8(8) . . . . ? C49 N3 C47 C40 58.2(10) . . . . ? C48 N3 C47 C40 178.7(7) . . . . ? Eu2 N3 C47 C40 -66.4(8) . . . . ? C35 C40 C47 N3 67.2(10) . . . . ? C39 C40 C47 N3 -119.1(9) . . . . ? C45 C46 C48 N3 105.4(10) . . . . ? C41 C46 C48 N3 -74.7(11) . . . . ? C49 N3 C48 C46 -67.3(10) . . . . ? C47 N3 C48 C46 170.7(8) . . . . ? Eu2 N3 C48 C46 52.6(8) . . . . ? C47 N3 C49 C50 -97.5(11) . . . . ? C48 N3 C49 C50 144.3(10) . . . . ? Eu2 N3 C49 C50 27.1(11) . . . . ? N3 C49 C50 N4 -63.9(13) . . . . ? C52 N4 C50 C49 -65.8(14) . . . . ? C51 N4 C50 C49 174.0(11) . . . . ? Eu2 N4 C50 C49 59.1(11) . . . . ? C37 C36 C53 C54 3.6(12) . . . . ? C35 C36 C53 C54 -179.3(8) . . . . ? C37 C36 C53 C55 121.9(9) . . . . ? C35 C36 C53 C55 -61.0(10) . . . . ? C37 C36 C53 C56 -117.3(9) . . . . ? C35 C36 C53 C56 59.8(11) . . . . ? C37 C38 C57 C60 -177.3(10) . . . . ? C39 C38 C57 C60 5.2(14) . . . . ? C37 C38 C57 C58 -57.5(12) . . . . ? C39 C38 C57 C58 125.0(10) . . . . ? C37 C38 C57 C59 62.3(12) . . . . ? C39 C38 C57 C59 -115.2(11) . . . . ? C43 C42 C61 C62 -1.4(13) . . . . ? C41 C42 C61 C62 177.1(9) . . . . ? C43 C42 C61 C64 -122.2(10) . . . . ? C41 C42 C61 C64 56.3(12) . . . . ? C43 C42 C61 C63 119.1(9) . . . . ? C41 C42 C61 C63 -62.4(11) . . . . ? C45 C44 C65 C66 -121.3(13) . . . . ? C43 C44 C65 C66 59.3(15) . . . . ? C45 C44 C65 C68 114.3(14) . . . . ? C43 C44 C65 C68 -65.2(15) . . . . ? C45 C44 C65 C67 -3.9(15) . . . . ? C43 C44 C65 C67 176.6(12) . . . . ? C72 O5 C69 C70 -11(4) . . . . ? O5 C69 C70 C71 2(4) . . . . ? C69 C70 C71 C72 6(4) . . . . ? C69 O5 C72 C71 14(4) . . . . ? C70 C71 C72 O5 -12(4) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 2.908 _refine_diff_density_min -1.682 _refine_diff_density_rms 0.166 #===========================================================================END data_complex2 _database_code_depnum_ccdc_archive 'CCDC 643505' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C136 H212 N4 O8 Sm3, C4 H8 O, 1.5(C7 H8)' _chemical_formula_sum 'C150.50 H232 N4 O9 Sm3' _chemical_formula_weight 2692.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' _symmetry_space_group_name_Hall '-p 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.9171(4) _cell_length_b 20.2284(3) _cell_length_c 30.2896(6) _cell_angle_alpha 108.104(9) _cell_angle_beta 95.546(10) _cell_angle_gamma 104.692(13) _cell_volume 8248.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14923 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour dark-Red _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2842 _exptl_absorpt_coefficient_mu 1.102 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4727 _exptl_absorpt_correction_T_max 0.8791 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83648 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 37232 _reflns_number_gt 28501 _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. The bond lengths of the THF solvent are unreasonable, so that 5 restraints were used for the refinement of the THF molecule. The bond lengths of the tioluene molecules are unreasonable, so that 14 restraints were used for the refinement of the THF molecule. The methyl groups of the tert-butyl groups and the end groups of the n-butyl groups of the ligands are disordered and the bond lengths of them are unreasonable, so that 49 restraints were used for the refinement of These groups. The end groups of the n-butyl groups of the ligands are disordered and the hydrogen atoms of the methlene groups were found from electron density map, and were fixed (6 restraints). One of the two toluene molecules is disordered, one carbon atom of this toluene molecule lies on a special position, and the hydrogen atoms can not be added reasonably (C80). ; _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^)+(0.0917P)^2^+26.7677P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 37232 _refine_ls_number_parameters 1483 _refine_ls_number_restraints 77 _refine_ls_R_factor_all 0.1184 _refine_ls_R_factor_gt 0.0904 _refine_ls_wR_factor_ref 0.2294 _refine_ls_wR_factor_gt 0.2139 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.93317(3) 0.71111(2) 0.746969(13) 0.04623(10) Uani 1 1 d . . . Sm2A Sm 1.00667(2) 0.601778(19) 0.825739(12) 0.03939(10) Uani 1 1 d . . . Sm2B Sm 0.85450(2) 0.816705(19) 0.666454(12) 0.04156(10) Uani 1 1 d . . . O1A O 0.9330(3) 0.5904(2) 0.74997(16) 0.0427(10) Uani 1 1 d . . . O2A O 0.9874(3) 0.6176(3) 0.89817(17) 0.0515(12) Uani 1 1 d . . . O3A O 1.0133(3) 0.7203(3) 0.82669(16) 0.0457(10) Uani 1 1 d . . . O4A O 1.0695(3) 0.5133(3) 0.80319(18) 0.0491(11) Uani 1 1 d . . . O1B O 0.8523(3) 0.6999(2) 0.66782(15) 0.0425(10) Uani 1 1 d . . . O2B O 0.9376(4) 0.9168(3) 0.65920(18) 0.0539(12) Uani 1 1 d . . . O3B O 0.9327(3) 0.8306(3) 0.74164(16) 0.0479(11) Uani 1 1 d . . . O4B O 0.7157(3) 0.7823(3) 0.62165(17) 0.0516(12) Uani 1 1 d . . . O5 O 0.4494(16) 0.8007(14) 0.7902(9) 0.286(9) Uiso 1 1 d D . . N1A N 0.8292(4) 0.5294(3) 0.82051(19) 0.0456(13) Uani 1 1 d . . . N2A N 1.1906(4) 0.6665(3) 0.8395(2) 0.0483(13) Uani 1 1 d . . . N1B N 0.9567(4) 0.7756(3) 0.60266(19) 0.0403(12) Uani 1 1 d . . . N2B N 0.7434(5) 0.8688(4) 0.7225(2) 0.0551(15) Uani 1 1 d . . . C1A C 0.8884(5) 0.5205(4) 0.7203(2) 0.0407(14) Uani 1 1 d . . . C2A C 0.9187(5) 0.4862(4) 0.6789(2) 0.0464(15) Uani 1 1 d . . . C3A C 0.8674(6) 0.4140(4) 0.6533(3) 0.062(2) Uani 1 1 d . . . H3A H 0.8883 0.3906 0.6266 0.074 Uiso 1 1 calc R . . C4A C 0.7888(6) 0.3740(4) 0.6639(3) 0.064(2) Uani 1 1 d . . . C5A C 0.7588(6) 0.4098(4) 0.7039(3) 0.0597(19) Uani 1 1 d . . . H5A H 0.7051 0.3853 0.7121 0.072 Uiso 1 1 calc R . . C6A C 0.8073(5) 0.4820(4) 0.7321(2) 0.0461(15) Uani 1 1 d . . . C7A C 0.9264(4) 0.6059(4) 0.9270(2) 0.0437(15) Uani 1 1 d . . . C8A C 0.9561(5) 0.6145(4) 0.9744(2) 0.0463(15) Uani 1 1 d . . . C9A C 0.8871(6) 0.6027(5) 1.0015(3) 0.0587(19) Uani 1 1 d . . . H9A H 0.9067 0.6091 1.0331 0.070 Uiso 1 1 calc R . . C10A C 0.7903(5) 0.5820(5) 0.9840(3) 0.062(2) Uani 1 1 d . . . C11A C 0.7635(5) 0.5733(5) 0.9372(3) 0.058(2) Uani 1 1 d . . . H11A H 0.6995 0.5588 0.9242 0.070 Uiso 1 1 calc R . . C12A C 0.8288(5) 0.5855(4) 0.9088(3) 0.0525(18) Uani 1 1 d . . . C13A C 0.7721(5) 0.5201(4) 0.7747(2) 0.0485(16) Uani 1 1 d . . . H13A H 0.7720 0.5678 0.7741 0.058 Uiso 1 1 calc R . . H13B H 0.7074 0.4925 0.7727 0.058 Uiso 1 1 calc R . . C14A C 0.7953(5) 0.5784(4) 0.8582(2) 0.0514(17) Uani 1 1 d . . . H14A H 0.7268 0.5614 0.8516 0.062 Uiso 1 1 calc R . . H14B H 0.8141 0.6267 0.8561 0.062 Uiso 1 1 calc R . . C15A C 0.8230(5) 0.4585(4) 0.8271(3) 0.0533(17) Uani 1 1 d . . . H15A H 0.8659 0.4681 0.8561 0.064 Uiso 1 1 calc R . . H15B H 0.8454 0.4290 0.8012 0.064 Uiso 1 1 calc R . . C16A C 0.7251(7) 0.4130(6) 0.8295(4) 0.073(3) Uani 1 1 d D . . H16A H 0.713(7) 0.438(5) 0.8604(17) 0.11(4) Uiso 1 1 d D . . H16B H 0.687(4) 0.400(4) 0.7984(11) 0.043(19) Uiso 1 1 d D . . C17A C 0.7334(17) 0.3391(11) 0.8289(11) 0.108(7) Uiso 0.60 1 d PD . . H17A H 0.7864 0.3464 0.8530 0.129 Uiso 0.60 1 calc PR . . H17B H 0.7454 0.3130 0.7984 0.129 Uiso 0.60 1 calc PR . . C17C C 0.729(2) 0.3559(14) 0.8505(10) 0.077(7) Uiso 0.40 1 d PD . . H17C H 0.6737 0.3418 0.8637 0.092 Uiso 0.40 1 calc PR . . H17D H 0.7856 0.3710 0.8744 0.092 Uiso 0.40 1 calc PR . . C18A C 0.643(2) 0.294(2) 0.8381(14) 0.213(16) Uiso 0.60 1 d PD . . H18A H 0.6500 0.2474 0.8375 0.320 Uiso 0.60 1 calc PR . . H18B H 0.5907 0.2856 0.8140 0.320 Uiso 0.60 1 calc PR . . H18C H 0.6317 0.3189 0.8685 0.320 Uiso 0.60 1 calc PR . . C18C C 0.732(4) 0.296(2) 0.8058(13) 0.18(2) Uiso 0.40 1 d PD . . H18D H 0.6682 0.2679 0.7894 0.274 Uiso 0.40 1 calc PR . . H18E H 0.7631 0.2641 0.8142 0.274 Uiso 0.40 1 calc PR . . H18F H 0.7650 0.3169 0.7856 0.274 Uiso 0.40 1 calc PR . . C19A C 1.0058(6) 0.5210(4) 0.6615(3) 0.0536(17) Uani 1 1 d . . . C20A C 1.0868(6) 0.4924(5) 0.6762(3) 0.071(2) Uani 1 1 d . . . H20A H 1.1428 0.5140 0.6664 0.107 Uiso 1 1 calc R . . H20B H 1.0687 0.4403 0.6613 0.107 Uiso 1 1 calc R . . H20C H 1.0989 0.5050 0.7099 0.107 Uiso 1 1 calc R . . C21A C 1.0397(6) 0.6043(4) 0.6793(3) 0.060(2) Uani 1 1 d . . . H21A H 0.9881 0.6222 0.6725 0.090 Uiso 1 1 calc R . . H21B H 1.0895 0.6205 0.6637 0.090 Uiso 1 1 calc R . . H21C H 1.0627 0.6226 0.7128 0.090 Uiso 1 1 calc R . . C22A C 0.9855(8) 0.4966(6) 0.6065(3) 0.079(3) Uani 1 1 d . . . H22A H 0.9270 0.5039 0.5960 0.118 Uiso 1 1 calc R . . H22B H 0.9810 0.4459 0.5931 0.118 Uiso 1 1 calc R . . H22C H 1.0358 0.5250 0.5964 0.118 Uiso 1 1 calc R . . C23A C 0.7360(8) 0.2947(5) 0.6329(4) 0.085(3) Uani 1 1 d D . . C24A C 0.648(2) 0.264(2) 0.6492(14) 0.208(17) Uiso 0.60 1 d PD . . H24A H 0.6178 0.2146 0.6289 0.313 Uiso 0.60 1 calc PR . . H24B H 0.6057 0.2927 0.6481 0.313 Uiso 0.60 1 calc PR . . H24C H 0.6640 0.2660 0.6811 0.313 Uiso 0.60 1 calc PR . . C24C C 0.6297(12) 0.2813(14) 0.6258(9) 0.074(6) Uiso 0.40 1 d PD . . H24D H 0.6144 0.3188 0.6162 0.111 Uiso 0.40 1 calc PR . . H24E H 0.6089 0.2821 0.6549 0.111 Uiso 0.40 1 calc PR . . H24F H 0.5988 0.2347 0.6017 0.111 Uiso 0.40 1 calc PR . . C25A C 0.7987(16) 0.2482(12) 0.6358(9) 0.110(6) Uiso 0.60 1 d P . . H25A H 0.7677 0.1989 0.6151 0.165 Uiso 0.60 1 calc PR . . H25B H 0.8119 0.2493 0.6677 0.165 Uiso 0.60 1 calc PR . . H25C H 0.8568 0.2666 0.6263 0.165 Uiso 0.60 1 calc PR . . C25C C 0.742(2) 0.2477(16) 0.6625(10) 0.106(9) Uiso 0.40 1 d PD . . H25D H 0.7179 0.1973 0.6428 0.159 Uiso 0.40 1 calc PR . . H25E H 0.7058 0.2578 0.6869 0.159 Uiso 0.40 1 calc PR . . H25F H 0.8069 0.2582 0.6767 0.159 Uiso 0.40 1 calc PR . . C26A C 0.7230(17) 0.2903(13) 0.5812(6) 0.112(7) Uiso 0.60 1 d PD . . H26A H 0.7838 0.3034 0.5727 0.169 Uiso 0.60 1 calc PR . . H26B H 0.6894 0.3234 0.5772 0.169 Uiso 0.60 1 calc PR . . H26C H 0.6878 0.2415 0.5611 0.169 Uiso 0.60 1 calc PR . . C26C C 0.781(3) 0.263(2) 0.5927(13) 0.158(16) Uiso 0.40 1 d PD . . H26D H 0.7435 0.2133 0.5753 0.237 Uiso 0.40 1 calc PR . . H26E H 0.8432 0.2639 0.6047 0.237 Uiso 0.40 1 calc PR . . H26F H 0.7841 0.2907 0.5721 0.237 Uiso 0.40 1 calc PR . . C27A C 1.0620(5) 0.6387(5) 0.9962(3) 0.0555(18) Uani 1 1 d . . . C28A C 1.0789(6) 0.6428(7) 1.0487(3) 0.093(4) Uani 1 1 d . . . H28A H 1.0521 0.5953 1.0502 0.140 Uiso 1 1 calc R . . H28B H 1.0494 0.6762 1.0670 0.140 Uiso 1 1 calc R . . H28C H 1.1454 0.6594 1.0611 0.140 Uiso 1 1 calc R . . C29A C 1.1100(7) 0.7144(5) 0.9945(3) 0.076(3) Uani 1 1 d . . . H29A H 1.1767 0.7277 1.0059 0.114 Uiso 1 1 calc R . . H29B H 1.0844 0.7496 1.0140 0.114 Uiso 1 1 calc R . . H29C H 1.0990 0.7133 0.9624 0.114 Uiso 1 1 calc R . . C30A C 1.1083(6) 0.5835(5) 0.9698(3) 0.072(2) Uani 1 1 d . . . H30A H 1.0815 0.5377 0.9738 0.108 Uiso 1 1 calc R . . H30B H 1.1749 0.6007 0.9823 0.108 Uiso 1 1 calc R . . H30C H 1.0977 0.5772 0.9368 0.108 Uiso 1 1 calc R . . C31A C 0.7138(6) 0.5686(6) 1.0142(3) 0.085(3) Uani 1 1 d D . . C32A C 0.7582(13) 0.5822(11) 1.0653(6) 0.080(4) Uiso 0.60 1 d P . . H32A H 0.7092 0.5724 1.0828 0.121 Uiso 0.60 1 calc PR . . H32B H 0.7965 0.6321 1.0798 0.121 Uiso 0.60 1 calc PR . . H32C H 0.7967 0.5507 1.0653 0.121 Uiso 0.60 1 calc PR . . C32C C 0.739(2) 0.5304(18) 1.0469(11) 0.112(10) Uiso 0.40 1 d PD . . H32D H 0.7832 0.5652 1.0744 0.168 Uiso 0.40 1 calc PR . . H32E H 0.7665 0.4939 1.0308 0.168 Uiso 0.40 1 calc PR . . H32F H 0.6828 0.5077 1.0562 0.168 Uiso 0.40 1 calc PR . . C33A C 0.6528(12) 0.4876(8) 0.9913(6) 0.082(5) Uiso 0.60 1 d PD . . H33A H 0.6927 0.4567 0.9894 0.123 Uiso 0.60 1 calc PR . . H33B H 0.6208 0.4791 0.9601 0.123 Uiso 0.60 1 calc PR . . H33C H 0.6070 0.4768 1.0103 0.123 Uiso 0.60 1 calc PR . . C33C C 0.6163(17) 0.570(2) 0.9957(14) 0.129(12) Uiso 0.40 1 d PD . . H33D H 0.5832 0.5241 0.9712 0.194 Uiso 0.40 1 calc PR . . H33E H 0.6221 0.6086 0.9832 0.194 Uiso 0.40 1 calc PR . . H33F H 0.5819 0.5777 1.0211 0.194 Uiso 0.40 1 calc PR . . C34A C 0.6564(13) 0.6213(10) 1.0144(7) 0.085(5) Uiso 0.60 1 d PD . . H34A H 0.6065 0.6126 1.0315 0.127 Uiso 0.60 1 calc PR . . H34B H 0.6300 0.6140 0.9824 0.127 Uiso 0.60 1 calc PR . . H34C H 0.6968 0.6705 1.0293 0.127 Uiso 0.60 1 calc PR . . C34C C 0.744(4) 0.6414(18) 1.0549(14) 0.19(2) Uiso 0.40 1 d PD . . H34D H 0.7121 0.6365 1.0803 0.288 Uiso 0.40 1 calc PR . . H34E H 0.7280 0.6776 1.0442 0.288 Uiso 0.40 1 calc PR . . H34F H 0.8110 0.6558 1.0659 0.288 Uiso 0.40 1 calc PR . . C35A C 1.0708(5) 0.7793(4) 0.8628(2) 0.0473(16) Uani 1 1 d . . . C36A C 1.0375(6) 0.8307(4) 0.8957(3) 0.0558(18) Uani 1 1 d . . . C37A C 1.1048(7) 0.8874(5) 0.9315(3) 0.078(3) Uani 1 1 d . . . H37A H 1.0831 0.9201 0.9535 0.094 Uiso 1 1 calc R . . C38A C 1.2009(7) 0.8991(5) 0.9371(4) 0.081(3) Uani 1 1 d . . . C39A C 1.2309(6) 0.8487(5) 0.9042(3) 0.068(2) Uani 1 1 d . . . H39A H 1.2952 0.8543 0.9066 0.082 Uiso 1 1 calc R . . C40A C 1.1681(6) 0.7901(4) 0.8677(3) 0.0544(18) Uani 1 1 d . . . C41A C 1.1501(5) 0.4957(4) 0.8039(2) 0.0444(15) Uani 1 1 d . . . C42A C 1.1566(5) 0.4278(4) 0.8038(2) 0.0487(16) Uani 1 1 d . . . C43A C 1.2460(5) 0.4184(5) 0.8083(3) 0.0581(19) Uani 1 1 d . . . H43A H 1.2499 0.3737 0.8092 0.070 Uiso 1 1 calc R . . C44A C 1.3281(5) 0.4697(5) 0.8115(3) 0.060(2) Uani 1 1 d . . . C45A C 1.3201(5) 0.5356(5) 0.8090(3) 0.060(2) Uani 1 1 d . . . H45A H 1.3742 0.5715 0.8099 0.072 Uiso 1 1 calc R . . C46A C 1.2331(5) 0.5491(4) 0.8051(3) 0.0478(16) Uani 1 1 d . . . C47A C 1.2063(5) 0.7382(4) 0.8336(3) 0.0524(17) Uani 1 1 d . . . H47A H 1.1772 0.7306 0.8017 0.063 Uiso 1 1 calc R . . H47B H 1.2736 0.7603 0.8373 0.063 Uiso 1 1 calc R . . C48A C 1.2260(5) 0.6198(4) 0.8005(3) 0.0519(17) Uani 1 1 d . . . H48A H 1.2880 0.6479 0.7989 0.062 Uiso 1 1 calc R . . H48B H 1.1845 0.6087 0.7708 0.062 Uiso 1 1 calc R . . C49A C 1.2373(5) 0.6734(5) 0.8869(3) 0.0590(19) Uani 1 1 d . . . H49A H 1.2212 0.6252 0.8894 0.071 Uiso 1 1 calc R . . H49B H 1.2102 0.7030 0.9104 0.071 Uiso 1 1 calc R . . C50A C 1.3447(7) 0.7060(7) 0.9003(3) 0.080(3) Uani 1 1 d D . . H50A H 1.354(9) 0.753(4) 0.896(5) 0.15(5) Uiso 1 1 d D . . H50B H 1.372(6) 0.691(5) 0.8723(19) 0.08(3) Uiso 1 1 d D . . C51A C 1.3850(16) 0.7146(14) 0.9503(6) 0.109(7) Uiso 0.60 1 d PD . . H51A H 1.3739 0.6668 0.9531 0.130 Uiso 0.60 1 calc PR . . H51B H 1.3526 0.7416 0.9722 0.130 Uiso 0.60 1 calc PR . . C51C C 1.382(2) 0.678(2) 0.9380(12) 0.120(13) Uiso 0.40 1 d PD . . H51C H 1.3488 0.6884 0.9641 0.144 Uiso 0.40 1 calc PR . . H51D H 1.3676 0.6254 0.9243 0.144 Uiso 0.40 1 calc PR . . C52A C 1.4914(19) 0.755(2) 0.9640(14) 0.186(15) Uiso 0.60 1 d PD . . H52A H 1.5144 0.7590 0.9958 0.279 Uiso 0.60 1 calc PR . . H52B H 1.5026 0.8024 0.9619 0.279 Uiso 0.60 1 calc PR . . H52C H 1.5239 0.7277 0.9427 0.279 Uiso 0.60 1 calc PR . . C52C C 1.487(2) 0.710(2) 0.9573(14) 0.124(12) Uiso 0.40 1 d PD . . H52D H 1.5195 0.6793 0.9393 0.186 Uiso 0.40 1 calc PR . . H52E H 1.4991 0.7138 0.9898 0.186 Uiso 0.40 1 calc PR . . H52F H 1.5080 0.7577 0.9552 0.186 Uiso 0.40 1 calc PR . . C53A C 0.9313(6) 0.8228(5) 0.8966(3) 0.060(2) Uani 1 1 d . . . C54A C 0.9175(7) 0.8996(5) 0.9161(4) 0.085(3) Uani 1 1 d . . . H54A H 0.8523 0.8945 0.9178 0.127 Uiso 1 1 calc R . . H54B H 0.9359 0.9260 0.8953 0.127 Uiso 1 1 calc R . . H54C H 0.9557 0.9258 0.9471 0.127 Uiso 1 1 calc R . . C55A C 0.8996(7) 0.7805(6) 0.9287(3) 0.077(3) Uani 1 1 d . . . H55A H 0.8341 0.7752 0.9296 0.116 Uiso 1 1 calc R . . H55B H 0.9364 0.8063 0.9601 0.116 Uiso 1 1 calc R . . H55C H 0.9083 0.7331 0.9168 0.116 Uiso 1 1 calc R . . C56A C 0.8669(6) 0.7857(5) 0.8473(3) 0.064(2) Uani 1 1 d . . . H56A H 0.8656 0.7356 0.8349 0.096 Uiso 1 1 calc R . . H56B H 0.8908 0.8102 0.8264 0.096 Uiso 1 1 calc R . . H56C H 0.8041 0.7883 0.8499 0.096 Uiso 1 1 calc R . . C57A C 1.2710(9) 0.9630(6) 0.9771(4) 0.106(4) Uani 1 1 d D . . C58A C 1.3712(18) 0.9681(16) 0.9767(10) 0.133(8) Uiso 0.60 1 d P . . H58A H 1.4098 1.0082 1.0038 0.199 Uiso 0.60 1 calc PR . . H58B H 1.3872 0.9759 0.9484 0.199 Uiso 0.60 1 calc PR . . H58C H 1.3818 0.9237 0.9776 0.199 Uiso 0.60 1 calc PR . . C58C C 1.336(2) 0.935(2) 1.0034(13) 0.129(12) Uiso 0.40 1 d PD . . H58D H 1.3830 0.9758 1.0271 0.193 Uiso 0.40 1 calc PR . . H58E H 1.3668 0.9074 0.9815 0.193 Uiso 0.40 1 calc PR . . H58F H 1.3002 0.9048 1.0183 0.193 Uiso 0.40 1 calc PR . . C59A C 1.2409(19) 0.9599(16) 1.0231(8) 0.142(9) Uiso 0.60 1 d PD . . H59A H 1.2756 1.0041 1.0486 0.213 Uiso 0.60 1 calc PR . . H59B H 1.2534 0.9191 1.0294 0.213 Uiso 0.60 1 calc PR . . H59C H 1.1745 0.9545 1.0205 0.213 Uiso 0.60 1 calc PR . . C59C C 1.223(2) 1.0109(18) 1.0092(12) 0.119(11) Uiso 0.40 1 d PD . . H59D H 1.2687 1.0561 1.0285 0.179 Uiso 0.40 1 calc PR . . H59E H 1.1937 0.9865 1.0291 0.179 Uiso 0.40 1 calc PR . . H59F H 1.1755 1.0203 0.9903 0.179 Uiso 0.40 1 calc PR . . C60A C 1.253(2) 1.0337(12) 0.9766(11) 0.153(10) Uiso 0.60 1 d PD . . H60A H 1.2968 1.0741 1.0019 0.229 Uiso 0.60 1 calc PR . . H60B H 1.1898 1.0320 0.9808 0.229 Uiso 0.60 1 calc PR . . H60C H 1.2617 1.0395 0.9469 0.229 Uiso 0.60 1 calc PR . . C60C C 1.350(2) 1.0048(18) 0.9592(12) 0.117(11) Uiso 0.40 1 d PD . . H60D H 1.3239 1.0251 0.9382 0.176 Uiso 0.40 1 calc PR . . H60E H 1.3825 0.9724 0.9427 0.176 Uiso 0.40 1 calc PR . . H60F H 1.3934 1.0434 0.9855 0.176 Uiso 0.40 1 calc PR . . C61A C 1.0673(5) 0.3662(4) 0.7994(3) 0.0565(18) Uani 1 1 d . . . C62A C 1.0877(7) 0.2945(5) 0.7963(4) 0.085(3) Uani 1 1 d . . . H62A H 1.1195 0.2804 0.7704 0.127 Uiso 1 1 calc R . . H62B H 1.0294 0.2571 0.7913 0.127 Uiso 1 1 calc R . . H62C H 1.1271 0.3010 0.8253 0.127 Uiso 1 1 calc R . . C63A C 1.0221(6) 0.3867(5) 0.8427(3) 0.066(2) Uani 1 1 d . . . H63A H 1.0660 0.3947 0.8705 0.100 Uiso 1 1 calc R . . H63B H 0.9663 0.3479 0.8393 0.100 Uiso 1 1 calc R . . H63C H 1.0055 0.4305 0.8455 0.100 Uiso 1 1 calc R . . C64A C 0.9955(6) 0.3512(5) 0.7543(3) 0.070(2) Uani 1 1 d . . . H64A H 0.9783 0.3945 0.7562 0.105 Uiso 1 1 calc R . . H64B H 0.9402 0.3126 0.7517 0.105 Uiso 1 1 calc R . . H64C H 1.0235 0.3372 0.7270 0.105 Uiso 1 1 calc R . . C65A C 1.4263(6) 0.4585(6) 0.8185(4) 0.082(3) Uani 1 1 d D . . C66A C 1.4848(14) 0.5149(11) 0.8653(7) 0.093(5) Uiso 0.60 1 d P . . H66A H 1.5434 0.5051 0.8718 0.140 Uiso 0.60 1 calc PR . . H66B H 1.4505 0.5126 0.8903 0.140 Uiso 0.60 1 calc PR . . H66C H 1.4975 0.5627 0.8632 0.140 Uiso 0.60 1 calc PR . . C66C C 1.446(3) 0.443(3) 0.8640(11) 0.162(16) Uiso 0.40 1 d PD . . H66D H 1.5131 0.4605 0.8762 0.243 Uiso 0.40 1 calc PR . . H66E H 1.4247 0.3910 0.8573 0.243 Uiso 0.40 1 calc PR . . H66F H 1.4142 0.4665 0.8869 0.243 Uiso 0.40 1 calc PR . . C67A C 1.4715(14) 0.4630(12) 0.7756(6) 0.092(6) Uiso 0.60 1 d PD . . H67A H 1.4836 0.5115 0.7748 0.138 Uiso 0.60 1 calc PR . . H67B H 1.4294 0.4290 0.7470 0.138 Uiso 0.60 1 calc PR . . H67C H 1.5299 0.4513 0.7781 0.138 Uiso 0.60 1 calc PR . . C67C C 1.497(2) 0.5017(18) 0.7967(12) 0.109(10) Uiso 0.40 1 d PD . . H67D H 1.5133 0.5527 0.8149 0.164 Uiso 0.40 1 calc PR . . H67E H 1.4691 0.4932 0.7648 0.164 Uiso 0.40 1 calc PR . . H67F H 1.5527 0.4862 0.7968 0.164 Uiso 0.40 1 calc PR . . C68A C 1.4219(14) 0.3838(10) 0.8194(7) 0.092(5) Uiso 0.60 1 d P . . H68A H 1.3842 0.3475 0.7904 0.138 Uiso 0.60 1 calc PR . . H68B H 1.3943 0.3768 0.8456 0.138 Uiso 0.60 1 calc PR . . H68C H 1.4846 0.3794 0.8229 0.138 Uiso 0.60 1 calc PR . . C68C C 1.423(3) 0.3850(14) 0.7816(12) 0.130(12) Uiso 0.40 1 d PD . . H68D H 1.3940 0.3812 0.7510 0.195 Uiso 0.40 1 calc PR . . H68E H 1.3881 0.3456 0.7902 0.195 Uiso 0.40 1 calc PR . . H68F H 1.4867 0.3824 0.7808 0.195 Uiso 0.40 1 calc PR . . C1B C 0.8234(5) 0.6436(4) 0.6259(2) 0.0426(14) Uani 1 1 d . . . C2B C 0.7399(5) 0.5845(4) 0.6140(2) 0.0479(16) Uani 1 1 d . . . C3B C 0.7197(6) 0.5326(4) 0.5684(3) 0.061(2) Uani 1 1 d . . . H3B H 0.6637 0.4946 0.5601 0.073 Uiso 1 1 calc R . . C4B C 0.7753(6) 0.5330(4) 0.5351(3) 0.062(2) Uani 1 1 d . . . C5B C 0.8588(6) 0.5901(4) 0.5478(3) 0.0566(18) Uani 1 1 d . . . H5B H 0.8994 0.5915 0.5265 0.068 Uiso 1 1 calc R . . C6B C 0.8826(5) 0.6452(4) 0.5921(2) 0.0432(14) Uani 1 1 d . . . C7B C 0.9977(5) 0.9455(4) 0.6349(3) 0.0502(16) Uani 1 1 d . . . C8B C 1.0070(6) 1.0145(4) 0.6307(3) 0.062(2) Uani 1 1 d . . . C9B C 1.0665(7) 1.0347(5) 0.6018(4) 0.077(3) Uani 1 1 d . . . H9B H 1.0717 1.0796 0.5985 0.093 Uiso 1 1 calc R . . C10B C 1.1192(7) 0.9937(5) 0.5775(4) 0.076(3) Uani 1 1 d . . . C11B C 1.1123(5) 0.9281(4) 0.5845(3) 0.060(2) Uani 1 1 d . . . H11B H 1.1489 0.8998 0.5702 0.072 Uiso 1 1 calc R . . C12B C 1.0534(5) 0.9036(4) 0.6119(3) 0.0503(17) Uani 1 1 d . . . C13B C 0.9724(5) 0.7058(4) 0.6038(3) 0.0443(15) Uani 1 1 d . . . H13C H 1.0122 0.6915 0.5813 0.053 Uiso 1 1 calc R . . H13D H 1.0056 0.7139 0.6350 0.053 Uiso 1 1 calc R . . C14B C 1.0501(5) 0.8324(4) 0.6184(3) 0.0471(16) Uani 1 1 d . . . H14C H 1.0946 0.8127 0.6013 0.056 Uiso 1 1 calc R . . H14D H 1.0716 0.8422 0.6517 0.056 Uiso 1 1 calc R . . C15B C 0.9105(5) 0.7681(4) 0.5545(3) 0.0516(17) Uani 1 1 d . . . H15C H 0.8987 0.8138 0.5565 0.062 Uiso 1 1 calc R . . H15D H 0.8496 0.7311 0.5461 0.062 Uiso 1 1 calc R . . C16B C 0.9642(6) 0.7482(5) 0.5140(3) 0.064(2) Uani 1 1 d . . . H16C H 1.0253 0.7847 0.5217 0.076 Uiso 1 1 calc R . . H16D H 0.9747 0.7016 0.5107 0.076 Uiso 1 1 calc R . . C17B C 0.9105(10) 0.7436(8) 0.4678(4) 0.106(4) Uani 1 1 d . . . H17E H 0.8963 0.7891 0.4717 0.127 Uiso 1 1 calc R . . H17F H 0.8512 0.7049 0.4591 0.127 Uiso 1 1 calc R . . C18B C 0.9657(12) 0.7289(8) 0.4284(4) 0.135(6) Uani 1 1 d . . . H18G H 1.0303 0.7587 0.4398 0.203 Uiso 1 1 calc R . . H18H H 0.9388 0.7402 0.4026 0.203 Uiso 1 1 calc R . . H18I H 0.9632 0.6784 0.4176 0.203 Uiso 1 1 calc R . . C19B C 0.6670(5) 0.5774(4) 0.6465(3) 0.0537(17) Uani 1 1 d . . . C20B C 0.6240(7) 0.4961(5) 0.6394(4) 0.081(3) Uani 1 1 d . . . H20D H 0.6731 0.4768 0.6477 0.121 Uiso 1 1 calc R . . H20E H 0.5942 0.4697 0.6068 0.121 Uiso 1 1 calc R . . H20F H 0.5780 0.4912 0.6592 0.121 Uiso 1 1 calc R . . C21B C 0.5892(6) 0.6068(6) 0.6319(3) 0.072(2) Uani 1 1 d . . . H21D H 0.5443 0.6048 0.6525 0.108 Uiso 1 1 calc R . . H21E H 0.5581 0.5778 0.5999 0.108 Uiso 1 1 calc R . . H21F H 0.6162 0.6564 0.6341 0.108 Uiso 1 1 calc R . . C22B C 0.7068(6) 0.6156(5) 0.6991(3) 0.066(2) Uani 1 1 d . . . H22D H 0.7289 0.6673 0.7061 0.099 Uiso 1 1 calc R . . H22E H 0.7582 0.5988 0.7078 0.099 Uiso 1 1 calc R . . H22F H 0.6583 0.6047 0.7167 0.099 Uiso 1 1 calc R . . C23B C 0.7522(8) 0.4731(6) 0.4855(3) 0.093(3) Uani 1 1 d D . . C24B C 0.7481(16) 0.5084(11) 0.4470(6) 0.096(6) Uiso 0.60 1 d PD . . H24G H 0.8098 0.5394 0.4487 0.144 Uiso 0.60 1 calc PR . . H24H H 0.7048 0.5367 0.4520 0.144 Uiso 0.60 1 calc PR . . H24I H 0.7272 0.4708 0.4163 0.144 Uiso 0.60 1 calc PR . . C24D C 0.6460(16) 0.456(3) 0.4690(16) 0.163(17) Uiso 0.40 1 d PD . . H24J H 0.6338 0.4973 0.4628 0.244 Uiso 0.40 1 calc PR . . H24K H 0.6132 0.4470 0.4932 0.244 Uiso 0.40 1 calc PR . . H24L H 0.6243 0.4142 0.4406 0.244 Uiso 0.40 1 calc PR . . C25B C 0.6581(13) 0.4115(11) 0.4765(7) 0.088(5) Uiso 0.60 1 d P . . H25G H 0.6061 0.4314 0.4765 0.132 Uiso 0.60 1 calc PR . . H25H H 0.6596 0.3907 0.5010 0.132 Uiso 0.60 1 calc PR . . H25I H 0.6505 0.3743 0.4463 0.132 Uiso 0.60 1 calc PR . . C25D C 0.727(5) 0.402(2) 0.494(2) 0.22(3) Uiso 0.40 1 d PD . . H25J H 0.7829 0.3949 0.5083 0.331 Uiso 0.40 1 calc PR . . H25K H 0.6990 0.3623 0.4649 0.331 Uiso 0.40 1 calc PR . . H25L H 0.6828 0.4024 0.5154 0.331 Uiso 0.40 1 calc PR . . C26B C 0.8307(12) 0.4358(9) 0.4796(6) 0.085(5) Uiso 0.60 1 d PD . . H26G H 0.8176 0.4007 0.4481 0.127 Uiso 0.60 1 calc PR . . H26H H 0.8329 0.4116 0.5022 0.127 Uiso 0.60 1 calc PR . . H26I H 0.8903 0.4718 0.4847 0.127 Uiso 0.60 1 calc PR . . C26D C 0.799(3) 0.497(2) 0.4481(11) 0.118(11) Uiso 0.40 1 d PD . . H26J H 0.7789 0.4566 0.4184 0.176 Uiso 0.40 1 calc PR . . H26K H 0.8659 0.5106 0.4575 0.176 Uiso 0.40 1 calc PR . . H26L H 0.7800 0.5371 0.4446 0.176 Uiso 0.40 1 calc PR . . C27B C 0.9493(8) 1.0630(5) 0.6561(4) 0.079(3) Uani 1 1 d . . . C28B C 0.8451(8) 1.0254(6) 0.6361(4) 0.090(3) Uani 1 1 d . . . H28D H 0.8286 0.9773 0.6379 0.134 Uiso 1 1 calc R . . H28E H 0.8319 1.0218 0.6037 0.134 Uiso 1 1 calc R . . H28F H 0.8089 1.0530 0.6541 0.134 Uiso 1 1 calc R . . C29B C 0.9755(11) 1.1372(6) 0.6482(6) 0.131(6) Uani 1 1 d . . . H29D H 0.9538 1.1296 0.6156 0.196 Uiso 1 1 calc R . . H29E H 1.0428 1.1587 0.6562 0.196 Uiso 1 1 calc R . . H29F H 0.9461 1.1692 0.6680 0.196 Uiso 1 1 calc R . . C30B C 0.9714(9) 1.0773(6) 0.7096(4) 0.102(4) Uani 1 1 d . . . H30D H 0.9365 1.1080 0.7257 0.153 Uiso 1 1 calc R . . H30E H 1.0378 1.1010 0.7214 0.153 Uiso 1 1 calc R . . H30F H 0.9539 1.0318 0.7150 0.153 Uiso 1 1 calc R . . C31B C 1.1809(9) 1.0165(6) 0.5438(5) 0.102(4) Uani 1 1 d D . . C32B C 1.220(2) 0.9616(13) 0.5140(9) 0.139(9) Uiso 0.60 1 d PD . . H32G H 1.1696 0.9243 0.4901 0.209 Uiso 0.60 1 calc PR . . H32H H 1.2486 0.9401 0.5333 0.209 Uiso 0.60 1 calc PR . . H32I H 1.2660 0.9846 0.4992 0.209 Uiso 0.60 1 calc PR . . C32D C 1.157(2) 0.9539(13) 0.4963(8) 0.091(8) Uiso 0.40 1 d PD . . H32J H 1.1968 0.9679 0.4756 0.137 Uiso 0.40 1 calc PR . . H32K H 1.0921 0.9430 0.4822 0.137 Uiso 0.40 1 calc PR . . H32L H 1.1672 0.9115 0.5012 0.137 Uiso 0.40 1 calc PR . . C33B C 1.262(2) 1.0814(16) 0.5720(12) 0.203(16) Uiso 0.60 1 d PD . . H33G H 1.2987 1.0693 0.5945 0.305 Uiso 0.60 1 calc PR . . H33H H 1.2392 1.1207 0.5884 0.305 Uiso 0.60 1 calc PR . . H33I H 1.3012 1.0961 0.5512 0.305 Uiso 0.60 1 calc PR . . C33D C 1.2826(15) 1.0354(18) 0.5671(10) 0.096(8) Uiso 0.40 1 d PD . . H33J H 1.2928 0.9945 0.5741 0.144 Uiso 0.40 1 calc PR . . H33K H 1.2966 1.0765 0.5959 0.144 Uiso 0.40 1 calc PR . . H33L H 1.3231 1.0473 0.5461 0.144 Uiso 0.40 1 calc PR . . C34B C 1.1312(18) 1.0455(14) 0.5102(8) 0.122(8) Uiso 0.60 1 d PD . . H34G H 1.1744 1.0623 0.4917 0.184 Uiso 0.60 1 calc PR . . H34H H 1.1108 1.0851 0.5284 0.184 Uiso 0.60 1 calc PR . . H34I H 1.0775 1.0071 0.4896 0.184 Uiso 0.60 1 calc PR . . C34D C 1.169(3) 1.0833(15) 0.5359(13) 0.109(10) Uiso 0.40 1 d PD . . H34J H 1.2013 1.0915 0.5114 0.164 Uiso 0.40 1 calc PR . . H34K H 1.1943 1.1245 0.5646 0.164 Uiso 0.40 1 calc PR . . H34L H 1.1028 1.0767 0.5266 0.164 Uiso 0.40 1 calc PR . . C35B C 0.9560(6) 0.8978(4) 0.7757(2) 0.0513(17) Uani 1 1 d . . . C36B C 1.0494(7) 0.9417(4) 0.7957(3) 0.062(2) Uani 1 1 d . . . C37B C 1.0622(8) 1.0112(5) 0.8296(3) 0.078(3) Uani 1 1 d . . . H37B H 1.1236 1.0414 0.8426 0.094 Uiso 1 1 calc R . . C38B C 0.9888(10) 1.0368(5) 0.8445(3) 0.088(3) Uani 1 1 d D . . C39B C 0.8990(8) 0.9919(5) 0.8257(3) 0.076(3) Uani 1 1 d . . . H39B H 0.8489 1.0076 0.8362 0.091 Uiso 1 1 calc R . . C40B C 0.8800(7) 0.9233(5) 0.7911(3) 0.062(2) Uani 1 1 d . . . C41B C 0.6271(5) 0.7864(4) 0.6182(3) 0.0534(18) Uani 1 1 d . . . C42B C 0.5691(5) 0.7737(5) 0.5750(3) 0.0547(18) Uani 1 1 d . . . C43B C 0.4789(5) 0.7827(5) 0.5765(3) 0.060(2) Uani 1 1 d . . . H43B H 0.4407 0.7751 0.5481 0.072 Uiso 1 1 calc R . . C44B C 0.4438(5) 0.8020(5) 0.6172(3) 0.063(2) Uani 1 1 d . . . C45B C 0.5005(6) 0.8117(5) 0.6587(3) 0.067(2) Uani 1 1 d . . . H45B H 0.4773 0.8231 0.6867 0.081 Uiso 1 1 calc R . . C46B C 0.5911(5) 0.8051(4) 0.6605(3) 0.0546(18) Uani 1 1 d . . . C47B C 0.7813(6) 0.8750(5) 0.7718(3) 0.059(2) Uani 1 1 d . . . H47C H 0.7408 0.8935 0.7926 0.071 Uiso 1 1 calc R . . H47D H 0.7783 0.8267 0.7721 0.071 Uiso 1 1 calc R . . C48B C 0.6476(5) 0.8115(5) 0.7067(3) 0.061(2) Uani 1 1 d . . . H48C H 0.6567 0.7646 0.7036 0.073 Uiso 1 1 calc R . . H48D H 0.6109 0.8225 0.7313 0.073 Uiso 1 1 calc R . . C49B C 0.7399(7) 0.9403(5) 0.7197(3) 0.069(2) Uani 1 1 d . . . H49C H 0.7192 0.9334 0.6868 0.083 Uiso 1 1 calc R . . H49D H 0.8036 0.9735 0.7297 0.083 Uiso 1 1 calc R . . C50B C 0.6757(12) 0.9771(8) 0.7490(6) 0.105(4) Uani 1 1 d D . . H50C H 0.614(3) 0.941(4) 0.740(3) 0.08(3) Uiso 1 1 d D . . H50D H 0.709(9) 0.988(7) 0.7809(19) 0.14(6) Uiso 1 1 d D . . C51B C 0.655(3) 1.0380(18) 0.7346(17) 0.161(9) Uiso 0.50 1 d PD . . H51G H 0.5944 1.0437 0.7414 0.193 Uiso 0.50 1 calc PR . . H51H H 0.6545 1.0288 0.7012 0.193 Uiso 0.50 1 calc PR . . C51D C 0.692(4) 1.0543(15) 0.7480(17) 0.161(9) Uiso 0.50 1 d PD . . H51E H 0.7590 1.0766 0.7506 0.193 Uiso 0.50 1 calc PR . . H51F H 0.6720 1.0833 0.7750 0.193 Uiso 0.50 1 calc PR . . C52B C 0.737(4) 1.107(3) 0.766(2) 0.32(4) Uiso 0.50 1 d PD . . H52G H 0.7310 1.1483 0.7585 0.482 Uiso 0.50 1 calc PR . . H52H H 0.7965 1.0989 0.7591 0.482 Uiso 0.50 1 calc PR . . H52I H 0.7360 1.1147 0.7985 0.482 Uiso 0.50 1 calc PR . . C52D C 0.638(4) 1.055(4) 0.7023(19) 0.31(3) Uiso 0.50 1 d PD . . H52J H 0.6501 1.1039 0.7029 0.464 Uiso 0.50 1 calc PR . . H52K H 0.5713 1.0338 0.7001 0.464 Uiso 0.50 1 calc PR . . H52L H 0.6579 1.0265 0.6755 0.464 Uiso 0.50 1 calc PR . . C53B C 1.1382(6) 0.9236(5) 0.7799(3) 0.065(2) Uani 1 1 d . . . C54B C 1.2224(8) 0.9549(7) 0.8235(4) 0.102(4) Uani 1 1 d . . . H54D H 1.2379 1.0071 0.8360 0.153 Uiso 1 1 calc R . . H54E H 1.2764 0.9415 0.8135 0.153 Uiso 1 1 calc R . . H54F H 1.2042 0.9354 0.8475 0.153 Uiso 1 1 calc R . . C55B C 1.1638(8) 0.9596(6) 0.7425(4) 0.086(3) Uani 1 1 d . . . H55D H 1.1096 0.9446 0.7178 0.129 Uiso 1 1 calc R . . H55E H 1.2145 0.9448 0.7293 0.129 Uiso 1 1 calc R . . H55F H 1.1830 1.0117 0.7574 0.129 Uiso 1 1 calc R . . C56B C 1.1283(6) 0.8422(5) 0.7596(3) 0.067(2) Uani 1 1 d . . . H56D H 1.1016 0.8186 0.7804 0.101 Uiso 1 1 calc R . . H56E H 1.1893 0.8358 0.7566 0.101 Uiso 1 1 calc R . . H56F H 1.0876 0.8211 0.7290 0.101 Uiso 1 1 calc R . . C57B C 1.0058(10) 1.1131(7) 0.8820(5) 0.113(4) Uiso 1 1 d D . . C58B C 0.9818(19) 1.1095(14) 0.9275(7) 0.134(8) Uiso 0.60 1 d PD . . H58G H 1.0224 1.0877 0.9408 0.201 Uiso 0.60 1 calc PR . . H58H H 0.9173 1.0807 0.9224 0.201 Uiso 0.60 1 calc PR . . H58I H 0.9902 1.1579 0.9490 0.201 Uiso 0.60 1 calc PR . . C58D C 1.085(2) 1.125(2) 0.9215(11) 0.134(13) Uiso 0.40 1 d PD . . H58J H 1.0826 1.1635 0.9492 0.200 Uiso 0.40 1 calc PR . . H58K H 1.1443 1.1383 0.9120 0.200 Uiso 0.40 1 calc PR . . H58L H 1.0772 1.0810 0.9285 0.200 Uiso 0.40 1 calc PR . . C59B C 0.942(2) 1.1523(15) 0.8647(11) 0.150(10) Uiso 0.60 1 d PD . . H59G H 0.8772 1.1260 0.8617 0.225 Uiso 0.60 1 calc PR . . H59H H 0.9535 1.1546 0.8344 0.225 Uiso 0.60 1 calc PR . . H59I H 0.9558 1.2008 0.8870 0.225 Uiso 0.60 1 calc PR . . C59D C 0.912(2) 1.121(3) 0.8929(19) 0.177(19) Uiso 0.40 1 d PD . . H59J H 0.9210 1.1684 0.9162 0.266 Uiso 0.40 1 calc PR . . H59K H 0.8823 1.0841 0.9049 0.266 Uiso 0.40 1 calc PR . . H59L H 0.8717 1.1164 0.8645 0.266 Uiso 0.40 1 calc PR . . C60B C 1.096(3) 1.1629(19) 0.8806(13) 0.186(13) Uiso 0.60 1 d P . . H60G H 1.1060 1.2102 0.9040 0.279 Uiso 0.60 1 calc PR . . H60H H 1.0938 1.1669 0.8498 0.279 Uiso 0.60 1 calc PR . . H60I H 1.1466 1.1441 0.8873 0.279 Uiso 0.60 1 calc PR . . C60D C 1.023(3) 1.1714(15) 0.8594(11) 0.107(9) Uiso 0.40 1 d PD . . H60J H 0.9689 1.1622 0.8362 0.161 Uiso 0.40 1 calc PR . . H60K H 1.0772 1.1704 0.8444 0.161 Uiso 0.40 1 calc PR . . H60L H 1.0353 1.2184 0.8833 0.161 Uiso 0.40 1 calc PR . . C61B C 0.6045(6) 0.7519(5) 0.5285(3) 0.063(2) Uani 1 1 d . . . C62B C 0.5296(7) 0.7377(7) 0.4856(3) 0.098(4) Uani 1 1 d . . . H62D H 0.4751 0.6989 0.4839 0.147 Uiso 1 1 calc R . . H62E H 0.5549 0.7241 0.4573 0.147 Uiso 1 1 calc R . . H62F H 0.5119 0.7811 0.4887 0.147 Uiso 1 1 calc R . . C63B C 0.6313(7) 0.6809(5) 0.5212(3) 0.074(2) Uani 1 1 d . . . H63D H 0.6793 0.6881 0.5472 0.111 Uiso 1 1 calc R . . H63E H 0.6547 0.6680 0.4923 0.111 Uiso 1 1 calc R . . H63F H 0.5766 0.6423 0.5196 0.111 Uiso 1 1 calc R . . C64B C 0.6902(6) 0.8135(6) 0.5292(3) 0.074(3) Uani 1 1 d . . . H64D H 0.6718 0.8566 0.5319 0.111 Uiso 1 1 calc R . . H64E H 0.7135 0.7988 0.5003 0.111 Uiso 1 1 calc R . . H64F H 0.7390 0.8237 0.5556 0.111 Uiso 1 1 calc R . . C65B C 0.3446(6) 0.8119(6) 0.6172(4) 0.077(3) Uani 1 1 d . . . C66B C 0.3538(9) 0.8897(8) 0.6456(6) 0.142(6) Uani 1 1 d . . . H66G H 0.3909 0.9216 0.6319 0.213 Uiso 1 1 calc R . . H66H H 0.3843 0.9010 0.6776 0.213 Uiso 1 1 calc R . . H66I H 0.2923 0.8962 0.6454 0.213 Uiso 1 1 calc R . . C67B C 0.2855(7) 0.7602(8) 0.6385(5) 0.109(4) Uani 1 1 d . . . H67G H 0.3107 0.7755 0.6717 0.163 Uiso 1 1 calc R . . H67H H 0.2875 0.7115 0.6230 0.163 Uiso 1 1 calc R . . H67I H 0.2214 0.7613 0.6342 0.163 Uiso 1 1 calc R . . C68B C 0.2915(7) 0.7941(8) 0.5670(4) 0.112(4) Uani 1 1 d . . . H68G H 0.2282 0.7964 0.5681 0.168 Uiso 1 1 calc R . . H68H H 0.2897 0.7460 0.5476 0.168 Uiso 1 1 calc R . . H68I H 0.3234 0.8289 0.5538 0.168 Uiso 1 1 calc R . . C69 C 0.6842(16) 0.5882(15) 0.3414(8) 0.212(10) Uiso 1 1 d D . . C70 C 0.6371(18) 0.6328(17) 0.3673(8) 0.254(12) Uiso 1 1 d D . . H70 H 0.5946 0.6161 0.3848 0.304 Uiso 1 1 calc R . . C71 C 0.6548(19) 0.7027(18) 0.3664(10) 0.317(17) Uiso 1 1 d D . . H71 H 0.6245 0.7330 0.3847 0.380 Uiso 1 1 calc R . . C72 C 0.716(2) 0.7307(18) 0.3398(12) 0.37(2) Uiso 1 1 d D . . H72 H 0.7211 0.7754 0.3360 0.441 Uiso 1 1 calc R . . C73 C 0.7668(17) 0.6843(13) 0.3196(8) 0.214(10) Uiso 1 1 d D . . H73 H 0.8187 0.7038 0.3080 0.257 Uiso 1 1 calc R . . C74 C 0.7478(15) 0.6120(12) 0.3153(7) 0.176(7) Uiso 1 1 d D . . H74 H 0.7760 0.5811 0.2960 0.211 Uiso 1 1 calc R . . C75 C 0.666(3) 0.5084(18) 0.3322(13) 0.38(2) Uiso 1 1 d D . . H75A H 0.6251 0.4938 0.3522 0.570 Uiso 1 1 calc R . . H75B H 0.7249 0.4988 0.3387 0.570 Uiso 1 1 calc R . . H75C H 0.6369 0.4815 0.2996 0.570 Uiso 1 1 calc R . . C76 C 0.469(2) 0.7305(15) 0.7695(10) 0.263(13) Uiso 1 1 d D . . H76A H 0.4910 0.7271 0.7400 0.315 Uiso 1 1 calc R . . H76B H 0.4132 0.6897 0.7638 0.315 Uiso 1 1 calc R . . C77 C 0.5468(18) 0.7317(13) 0.8073(9) 0.224(10) Uiso 1 1 d D . . H77A H 0.6028 0.7273 0.7942 0.269 Uiso 1 1 calc R . . H77B H 0.5251 0.6914 0.8185 0.269 Uiso 1 1 calc R . . C78 C 0.5694(19) 0.8050(13) 0.8483(9) 0.229(10) Uiso 1 1 d D . . H78A H 0.5595 0.7962 0.8775 0.274 Uiso 1 1 calc R . . H78B H 0.6350 0.8326 0.8525 0.274 Uiso 1 1 calc R . . C79 C 0.507(2) 0.8472(17) 0.8377(11) 0.314(17) Uiso 1 1 d D . . H79A H 0.4673 0.8558 0.8610 0.377 Uiso 1 1 calc R . . H79B H 0.5443 0.8938 0.8372 0.377 Uiso 1 1 calc R . . C80 C 0.542(3) 0.000(2) 0.5420(12) 0.290(15) Uiso 1 1 d D . . C81 C 0.552(2) 0.0609(12) 0.5286(11) 0.316(17) Uiso 1 1 d D . . H81 H 0.5839 0.1050 0.5525 0.380 Uiso 1 1 calc R . . C82 C 0.521(3) 0.0676(19) 0.4850(14) 0.40(2) Uiso 1 1 d D . . H82 H 0.5397 0.1084 0.4762 0.482 Uiso 1 1 calc R . . C83 C 0.575(3) 0.013(3) 0.5937(12) 0.24(2) Uiso 0.50 1 d PD . . H83A H 0.5413 -0.0278 0.6015 0.357 Uiso 0.50 1 calc PR . . H83B H 0.5638 0.0564 0.6130 0.357 Uiso 0.50 1 calc PR . . H83C H 0.6415 0.0183 0.5993 0.357 Uiso 0.50 1 calc PR . . 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 0.0527(2) 0.0484(2) 0.04352(19) 0.02107(15) 0.00822(15) 0.01930(16) Sm2A 0.03199(17) 0.0523(2) 0.04230(18) 0.02389(15) 0.01164(13) 0.01605(14) Sm2B 0.04131(19) 0.0503(2) 0.0482(2) 0.02706(16) 0.01859(15) 0.02325(16) O1A 0.042(2) 0.044(2) 0.044(2) 0.016(2) 0.012(2) 0.014(2) O2A 0.042(3) 0.076(3) 0.046(3) 0.031(2) 0.015(2) 0.019(2) O3A 0.044(3) 0.049(3) 0.046(3) 0.015(2) 0.010(2) 0.017(2) O4A 0.037(2) 0.054(3) 0.063(3) 0.026(2) 0.013(2) 0.017(2) O1B 0.045(2) 0.048(3) 0.040(2) 0.022(2) 0.0118(19) 0.013(2) O2B 0.064(3) 0.051(3) 0.060(3) 0.029(2) 0.028(3) 0.024(2) O3B 0.052(3) 0.048(3) 0.047(3) 0.016(2) 0.011(2) 0.021(2) O4B 0.036(2) 0.077(3) 0.059(3) 0.034(3) 0.021(2) 0.027(2) N1A 0.035(3) 0.062(4) 0.045(3) 0.025(3) 0.007(2) 0.015(3) N2A 0.035(3) 0.054(3) 0.054(3) 0.018(3) 0.013(3) 0.009(3) N1B 0.035(3) 0.045(3) 0.050(3) 0.023(2) 0.016(2) 0.018(2) N2B 0.064(4) 0.071(4) 0.050(3) 0.029(3) 0.023(3) 0.037(3) C1A 0.040(3) 0.046(4) 0.040(3) 0.019(3) 0.003(3) 0.015(3) C2A 0.051(4) 0.054(4) 0.039(3) 0.016(3) 0.008(3) 0.022(3) C3A 0.073(5) 0.060(5) 0.047(4) 0.008(4) 0.005(4) 0.027(4) C4A 0.064(5) 0.052(4) 0.066(5) 0.016(4) 0.002(4) 0.010(4) C5A 0.052(4) 0.061(5) 0.065(5) 0.025(4) 0.005(4) 0.012(4) C6A 0.046(4) 0.053(4) 0.039(3) 0.017(3) 0.001(3) 0.016(3) C7A 0.037(3) 0.058(4) 0.039(3) 0.017(3) 0.010(3) 0.017(3) C8A 0.045(4) 0.056(4) 0.040(3) 0.017(3) 0.011(3) 0.017(3) C9A 0.063(5) 0.078(5) 0.042(4) 0.027(4) 0.016(3) 0.023(4) C10A 0.045(4) 0.102(7) 0.051(4) 0.035(4) 0.022(3) 0.029(4) C11A 0.039(4) 0.094(6) 0.055(4) 0.038(4) 0.016(3) 0.025(4) C12A 0.044(4) 0.079(5) 0.051(4) 0.038(4) 0.014(3) 0.024(4) C13A 0.032(3) 0.070(5) 0.044(4) 0.022(3) 0.008(3) 0.011(3) C14A 0.042(4) 0.078(5) 0.047(4) 0.031(4) 0.013(3) 0.027(4) C15A 0.047(4) 0.065(5) 0.055(4) 0.030(4) 0.008(3) 0.018(4) C16A 0.064(5) 0.077(6) 0.092(7) 0.058(6) 0.019(5) 0.009(5) C19A 0.064(5) 0.061(4) 0.047(4) 0.025(3) 0.021(3) 0.026(4) C20A 0.074(6) 0.075(6) 0.081(6) 0.030(5) 0.028(5) 0.041(5) C21A 0.063(5) 0.063(5) 0.064(5) 0.030(4) 0.030(4) 0.019(4) C22A 0.103(7) 0.091(7) 0.053(5) 0.027(5) 0.030(5) 0.038(6) C23A 0.095(7) 0.060(5) 0.082(7) 0.007(5) 0.015(6) 0.011(5) C27A 0.047(4) 0.076(5) 0.046(4) 0.023(4) 0.010(3) 0.020(4) C28A 0.057(5) 0.166(11) 0.046(5) 0.040(6) -0.002(4) 0.013(6) C29A 0.070(6) 0.075(6) 0.062(5) 0.013(5) 0.010(4) 0.002(5) C30A 0.057(5) 0.094(7) 0.074(6) 0.037(5) 0.014(4) 0.028(5) C31A 0.062(5) 0.162(11) 0.051(5) 0.051(6) 0.030(4) 0.046(6) C35A 0.049(4) 0.046(4) 0.041(3) 0.013(3) 0.004(3) 0.008(3) C36A 0.067(5) 0.060(5) 0.047(4) 0.019(3) 0.018(4) 0.027(4) C37A 0.080(6) 0.077(6) 0.055(5) -0.006(4) 0.002(4) 0.026(5) C38A 0.072(6) 0.067(6) 0.076(6) -0.003(5) 0.000(5) 0.014(5) C39A 0.052(5) 0.065(5) 0.076(6) 0.016(4) 0.007(4) 0.010(4) C40A 0.057(4) 0.048(4) 0.055(4) 0.015(3) 0.011(4) 0.015(3) C41A 0.035(3) 0.057(4) 0.045(4) 0.020(3) 0.011(3) 0.016(3) C42A 0.042(4) 0.065(4) 0.049(4) 0.025(3) 0.015(3) 0.026(3) C43A 0.055(5) 0.067(5) 0.063(5) 0.025(4) 0.016(4) 0.033(4) C44A 0.042(4) 0.081(6) 0.072(5) 0.029(4) 0.016(4) 0.036(4) C45A 0.036(4) 0.075(5) 0.074(5) 0.029(4) 0.018(4) 0.019(4) C46A 0.033(3) 0.063(4) 0.053(4) 0.022(3) 0.013(3) 0.020(3) C47A 0.044(4) 0.054(4) 0.055(4) 0.017(3) 0.013(3) 0.010(3) C48A 0.039(4) 0.063(4) 0.060(4) 0.026(4) 0.023(3) 0.014(3) C49A 0.053(4) 0.074(5) 0.051(4) 0.025(4) 0.011(3) 0.017(4) C50A 0.050(5) 0.121(9) 0.065(6) 0.031(6) -0.002(4) 0.023(5) C53A 0.075(5) 0.071(5) 0.047(4) 0.020(4) 0.023(4) 0.042(4) C54A 0.088(7) 0.072(6) 0.095(7) 0.015(5) 0.021(6) 0.043(5) C55A 0.086(7) 0.101(7) 0.055(5) 0.039(5) 0.022(5) 0.027(6) C56A 0.058(5) 0.086(6) 0.057(5) 0.025(4) 0.018(4) 0.034(4) C57A 0.097(8) 0.092(8) 0.085(8) -0.019(6) -0.002(6) 0.022(7) C61A 0.050(4) 0.056(4) 0.071(5) 0.031(4) 0.013(4) 0.016(3) C62A 0.083(7) 0.070(6) 0.113(8) 0.045(6) 0.016(6) 0.026(5) C63A 0.059(5) 0.082(6) 0.069(5) 0.039(5) 0.018(4) 0.021(4) C64A 0.065(5) 0.064(5) 0.069(5) 0.018(4) -0.006(4) 0.014(4) C65A 0.059(5) 0.106(8) 0.097(7) 0.042(6) 0.022(5) 0.043(5) C1B 0.043(4) 0.042(3) 0.042(3) 0.016(3) 0.005(3) 0.013(3) C2B 0.049(4) 0.052(4) 0.046(4) 0.023(3) 0.009(3) 0.013(3) C3B 0.055(5) 0.054(4) 0.061(5) 0.017(4) 0.004(4) 0.001(4) C4B 0.071(5) 0.058(5) 0.044(4) 0.013(3) 0.007(4) 0.005(4) C5B 0.065(5) 0.052(4) 0.055(4) 0.024(4) 0.022(4) 0.013(4) C6B 0.049(4) 0.042(3) 0.044(4) 0.021(3) 0.013(3) 0.014(3) C7B 0.051(4) 0.043(4) 0.062(4) 0.025(3) 0.017(3) 0.013(3) C8B 0.068(5) 0.054(4) 0.078(5) 0.034(4) 0.026(4) 0.024(4) C9B 0.093(7) 0.058(5) 0.111(8) 0.056(5) 0.041(6) 0.034(5) C10B 0.074(6) 0.073(6) 0.108(7) 0.062(6) 0.037(5) 0.020(5) C11B 0.048(4) 0.058(5) 0.090(6) 0.041(4) 0.029(4) 0.019(4) C12B 0.042(4) 0.049(4) 0.072(5) 0.034(4) 0.018(3) 0.015(3) C13B 0.043(4) 0.045(4) 0.053(4) 0.022(3) 0.016(3) 0.019(3) C14B 0.037(3) 0.044(4) 0.067(4) 0.026(3) 0.016(3) 0.012(3) C15B 0.049(4) 0.062(4) 0.053(4) 0.026(4) 0.015(3) 0.022(3) C16B 0.073(5) 0.075(5) 0.059(5) 0.033(4) 0.028(4) 0.031(4) C17B 0.143(11) 0.154(11) 0.063(6) 0.056(7) 0.040(7) 0.085(9) C18B 0.214(17) 0.148(12) 0.067(7) 0.043(8) 0.051(9) 0.078(12) C19B 0.045(4) 0.060(4) 0.061(5) 0.031(4) 0.008(3) 0.012(3) C20B 0.078(6) 0.075(6) 0.086(7) 0.038(5) 0.027(5) 0.001(5) C21B 0.053(5) 0.100(7) 0.072(6) 0.034(5) 0.015(4) 0.032(5) C22B 0.058(5) 0.093(6) 0.060(5) 0.040(5) 0.028(4) 0.021(4) C23B 0.104(8) 0.079(7) 0.063(6) 0.014(5) -0.003(6) -0.007(6) C27B 0.110(8) 0.056(5) 0.095(7) 0.039(5) 0.041(6) 0.043(5) C28B 0.099(8) 0.108(8) 0.106(8) 0.061(7) 0.050(7) 0.066(7) C29B 0.176(14) 0.070(7) 0.200(15) 0.076(9) 0.095(12) 0.069(8) C30B 0.141(11) 0.061(6) 0.099(8) 0.014(6) 0.041(8) 0.032(7) C31B 0.113(9) 0.080(7) 0.151(11) 0.075(8) 0.071(8) 0.034(7) C35B 0.070(5) 0.043(4) 0.038(3) 0.009(3) 0.006(3) 0.019(4) C36B 0.082(6) 0.050(4) 0.049(4) 0.017(3) 0.013(4) 0.013(4) C37B 0.111(8) 0.049(5) 0.059(5) 0.009(4) 0.013(5) 0.010(5) C38B 0.151(11) 0.050(5) 0.064(6) 0.013(4) 0.036(7) 0.032(6) C39B 0.113(8) 0.068(6) 0.067(6) 0.026(5) 0.037(6) 0.050(6) C40B 0.084(6) 0.064(5) 0.052(4) 0.025(4) 0.020(4) 0.037(5) C41B 0.044(4) 0.067(5) 0.065(5) 0.037(4) 0.021(3) 0.023(4) C42B 0.043(4) 0.074(5) 0.065(5) 0.037(4) 0.024(3) 0.026(4) C43B 0.045(4) 0.076(5) 0.076(5) 0.037(4) 0.019(4) 0.030(4) C44B 0.043(4) 0.079(6) 0.085(6) 0.037(5) 0.019(4) 0.033(4) C45B 0.057(5) 0.089(6) 0.075(6) 0.037(5) 0.032(4) 0.035(5) C46B 0.048(4) 0.071(5) 0.064(5) 0.035(4) 0.027(4) 0.030(4) C47B 0.071(5) 0.077(5) 0.048(4) 0.028(4) 0.028(4) 0.039(4) C48B 0.057(5) 0.086(6) 0.067(5) 0.043(4) 0.035(4) 0.039(4) C49B 0.090(6) 0.075(6) 0.072(5) 0.039(5) 0.036(5) 0.049(5) C50B 0.125(12) 0.093(9) 0.131(12) 0.042(9) 0.048(10) 0.080(9) C53B 0.068(5) 0.057(5) 0.061(5) 0.018(4) 0.012(4) 0.008(4) C54B 0.085(7) 0.106(9) 0.083(7) 0.016(6) -0.010(6) 0.005(6) C55B 0.098(8) 0.079(6) 0.080(7) 0.032(5) 0.031(6) 0.015(6) C56B 0.055(5) 0.063(5) 0.083(6) 0.025(5) 0.011(4) 0.017(4) C61B 0.048(4) 0.089(6) 0.064(5) 0.037(5) 0.019(4) 0.026(4) C62B 0.067(6) 0.179(12) 0.062(6) 0.047(7) 0.010(5) 0.054(7) C63B 0.067(6) 0.085(6) 0.072(6) 0.022(5) 0.024(5) 0.028(5) C64B 0.065(5) 0.103(7) 0.083(6) 0.058(6) 0.031(5) 0.034(5) C65B 0.052(5) 0.104(7) 0.095(7) 0.041(6) 0.029(5) 0.046(5) C66B 0.095(9) 0.137(12) 0.187(15) 0.013(11) 0.026(9) 0.078(9) C67B 0.051(6) 0.154(12) 0.127(10) 0.054(9) 0.027(6) 0.031(7) C68B 0.066(6) 0.187(13) 0.122(10) 0.069(9) 0.026(6) 0.082(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O1A 2.470(4) . ? Sm1 O3B 2.475(5) . ? Sm1 O1B 2.493(4) . ? Sm1 O3A 2.519(5) . ? Sm1 Sm2A 3.9736(5) . ? Sm1 Sm2B 3.9803(5) . ? Sm2A O2A 2.175(4) . ? Sm2A O4A 2.182(5) . ? Sm2A O1A 2.363(4) . ? Sm2A O3A 2.365(5) . ? Sm2A N1A 2.643(5) . ? Sm2A N2A 2.651(5) . ? Sm2B O2B 2.177(5) . ? Sm2B O4B 2.180(5) . ? Sm2B O3B 2.355(5) . ? Sm2B O1B 2.369(4) . ? Sm2B N1B 2.639(5) . ? Sm2B N2B 2.657(6) . ? O1A C1A 1.368(8) . ? O2A C7A 1.350(7) . ? O3A C35A 1.359(8) . ? O4A C41A 1.339(8) . ? O1B C1B 1.355(8) . ? O2B C7B 1.345(8) . ? O3B C35B 1.361(8) . ? O4B C41B 1.341(8) . ? O5 C76 1.481(17) . ? O5 C79 1.485(18) . ? N1A C14A 1.485(9) . ? N1A C13A 1.489(8) . ? N1A C15A 1.490(9) . ? N2A C47A 1.479(9) . ? N2A C49A 1.484(9) . ? N2A C48A 1.499(9) . ? N1B C14B 1.486(8) . ? N1B C13B 1.497(8) . ? N1B C15B 1.497(9) . ? N2B C49B 1.487(10) . ? N2B C47B 1.500(9) . ? N2B C48B 1.516(11) . ? C1A C6A 1.408(9) . ? C1A C2A 1.408(9) . ? C2A C3A 1.390(11) . ? C2A C19A 1.538(10) . ? C3A C4A 1.372(12) . ? C3A H3A 0.9300 . ? C4A C5A 1.385(12) . ? C4A C23A 1.534(12) . ? C5A C6A 1.397(10) . ? C5A H5A 0.9300 . ? C6A C13A 1.499(9) . ? C7A C8A 1.405(9) . ? C7A C12A 1.412(9) . ? C8A C9A 1.397(10) . ? C8A C27A 1.541(10) . ? C9A C10A 1.396(11) . ? C9A H9A 0.9300 . ? C10A C11A 1.381(10) . ? C10A C31A 1.551(10) . ? C11A C12A 1.386(9) . ? C11A H11A 0.9300 . ? C12A C14A 1.514(9) . ? C13A H13A 0.9700 . ? C13A H13B 0.9700 . ? C14A H14A 0.9700 . ? C14A H14B 0.9700 . ? C15A C16A 1.537(11) . ? C15A H15A 0.9700 . ? C15A H15B 0.9700 . ? C16A C17C 1.49(3) . ? C16A C17A 1.526(16) . ? C16A H16A 0.970(10) . ? C16A H16B 0.969(10) . ? C17A C18A 1.532(19) . ? C17A H17A 0.9700 . ? C17A H17B 0.9700 . ? C17C C18C 1.526(19) . ? C17C H17C 0.9700 . ? C17C H17D 0.9700 . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? C18C H18D 0.9600 . ? C18C H18E 0.9600 . ? C18C H18F 0.9600 . ? C19A C21A 1.528(11) . ? C19A C20A 1.551(11) . ? C19A C22A 1.557(11) . ? C20A H20A 0.9600 . ? C20A H20B 0.9600 . ? C20A H20C 0.9600 . ? C21A H21A 0.9600 . ? C21A H21B 0.9600 . ? C21A H21C 0.9600 . ? C22A H22A 0.9600 . ? C22A H22B 0.9600 . ? C22A H22C 0.9600 . ? C23A C26C 1.495(19) . ? C23A C25A 1.50(2) . ? C23A C24A 1.500(18) . ? C23A C25C 1.507(17) . ? C23A C24C 1.521(16) . ? C23A C26A 1.534(15) . ? C24A H24A 0.9600 . ? C24A H24B 0.9600 . ? C24A H24C 0.9600 . ? C24C H24D 0.9600 . ? C24C H24E 0.9600 . ? C24C H24F 0.9600 . ? C25A H25A 0.9600 . ? C25A H25B 0.9600 . ? C25A H25C 0.9600 . ? C25C H25D 0.9600 . ? C25C H25E 0.9600 . ? C25C H25F 0.9600 . ? C26A H26A 0.9600 . ? C26A H26B 0.9600 . ? C26A H26C 0.9600 . ? C26C H26D 0.9600 . ? C26C H26E 0.9600 . ? C26C H26F 0.9600 . ? C27A C30A 1.517(11) . ? C27A C29A 1.536(12) . ? C27A C28A 1.559(11) . ? C28A H28A 0.9600 . ? C28A H28B 0.9600 . ? C28A H28C 0.9600 . ? C29A H29A 0.9600 . ? C29A H29B 0.9600 . ? C29A H29C 0.9600 . ? C30A H30A 0.9600 . ? C30A H30B 0.9600 . ? C30A H30C 0.9600 . ? C31A C32C 1.507(17) . ? C31A C33C 1.515(18) . ? C31A C34C 1.523(19) . ? C31A C34A 1.526(14) . ? C31A C32A 1.536(19) . ? C31A C33A 1.552(14) . ? C32A H32A 0.9600 . ? C32A H32B 0.9600 . ? C32A H32C 0.9600 . ? C32C H32D 0.9600 . ? C32C H32E 0.9600 . ? C32C H32F 0.9600 . ? C33A H33A 0.9600 . ? C33A H33B 0.9600 . ? C33A H33C 0.9600 . ? C33C H33D 0.9600 . ? C33C H33E 0.9600 . ? C33C H33F 0.9600 . ? C34A H34A 0.9600 . ? C34A H34B 0.9600 . ? C34A H34C 0.9600 . ? C34C H34D 0.9600 . ? C34C H34E 0.9600 . ? C34C H34F 0.9600 . ? C35A C40A 1.398(10) . ? C35A C36A 1.425(10) . ? C36A C37A 1.390(12) . ? C36A C53A 1.555(11) . ? C37A C38A 1.378(13) . ? C37A H37A 0.9300 . ? C38A C39A 1.386(12) . ? C38A C57A 1.526(13) . ? C39A C40A 1.388(11) . ? C39A H39A 0.9300 . ? C40A C47A 1.494(10) . ? C41A C42A 1.398(10) . ? C41A C46A 1.411(10) . ? C42A C43A 1.394(10) . ? C42A C61A 1.538(10) . ? C43A C44A 1.363(11) . ? C43A H43A 0.9300 . ? C44A C45A 1.391(11) . ? C44A C65A 1.542(11) . ? C45A C46A 1.394(9) . ? C45A H45A 0.9300 . ? C46A C48A 1.508(10) . ? C47A H47A 0.9700 . ? C47A H47B 0.9700 . ? C48A H48A 0.9700 . ? C48A H48B 0.9700 . ? C49A C50A 1.529(12) . ? C49A H49A 0.9700 . ? C49A H49B 0.9700 . ? C50A C51A 1.513(16) . ? C50A C51C 1.542(18) . ? C50A H50A 0.971(10) . ? C50A H50B 0.970(10) . ? C51A C52A 1.536(18) . ? C51A H51A 0.9700 . ? C51A H51B 0.9700 . ? C51C C52C 1.506(19) . ? C51C H51C 0.9700 . ? C51C H51D 0.9700 . ? C52A H52A 0.9600 . ? C52A H52B 0.9600 . ? C52A H52C 0.9600 . ? C52C H52D 0.9600 . ? C52C H52E 0.9600 . ? C52C H52F 0.9600 . ? C53A C55A 1.520(11) . ? C53A C56A 1.540(11) . ? C53A C54A 1.556(11) . ? C54A H54A 0.9600 . ? C54A H54B 0.9600 . ? C54A H54C 0.9600 . ? C55A H55A 0.9600 . ? C55A H55B 0.9600 . ? C55A H55C 0.9600 . ? C56A H56A 0.9600 . ? C56A H56B 0.9600 . ? C56A H56C 0.9600 . ? C57A C58A 1.47(3) . ? C57A C60C 1.516(18) . ? C57A C59C 1.516(18) . ? C57A C58C 1.518(18) . ? C57A C59A 1.519(17) . ? C57A C60A 1.523(17) . ? C58A H58A 0.9600 . ? C58A H58B 0.9600 . ? C58A H58C 0.9600 . ? C58C H58D 0.9600 . ? C58C H58E 0.9600 . ? C58C H58F 0.9600 . ? C59A H59A 0.9600 . ? C59A H59B 0.9600 . ? C59A H59C 0.9600 . ? C59C H59D 0.9600 . ? C59C H59E 0.9600 . ? C59C H59F 0.9600 . ? C60A H60A 0.9600 . ? C60A H60B 0.9600 . ? C60A H60C 0.9600 . ? C60C H60D 0.9600 . ? C60C H60E 0.9600 . ? C60C H60F 0.9600 . ? C61A C63A 1.524(11) . ? C61A C62A 1.535(11) . ? C61A C64A 1.548(11) . ? C62A H62A 0.9600 . ? C62A H62B 0.9600 . ? C62A H62C 0.9600 . ? C63A H63A 0.9600 . ? C63A H63B 0.9600 . ? C63A H63C 0.9600 . ? C64A H64A 0.9600 . ? C64A H64B 0.9600 . ? C64A H64C 0.9600 . ? C65A C68A 1.51(2) . ? C65A C66A 1.52(2) . ? C65A C66C 1.528(19) . ? C65A C67C 1.528(18) . ? C65A C67A 1.538(15) . ? C65A C68C 1.546(18) . ? C66A H66A 0.9600 . ? C66A H66B 0.9600 . ? C66A H66C 0.9600 . ? C66C H66D 0.9600 . ? C66C H66E 0.9600 . ? C66C H66F 0.9600 . ? C67A H67A 0.9600 . ? C67A H67B 0.9600 . ? C67A H67C 0.9600 . ? C67C H67D 0.9600 . ? C67C H67E 0.9600 . ? C67C H67F 0.9600 . ? C68A H68A 0.9600 . ? C68A H68B 0.9600 . ? C68A H68C 0.9600 . ? C68C H68D 0.9600 . ? C68C H68E 0.9600 . ? C68C H68F 0.9600 . ? C1B C2B 1.415(10) . ? C1B C6B 1.418(9) . ? C2B C3B 1.400(10) . ? C2B C19B 1.545(10) . ? C3B C4B 1.368(11) . ? C3B H3B 0.9300 . ? C4B C5B 1.391(11) . ? C4B C23B 1.548(12) . ? C5B C6B 1.394(10) . ? C5B H5B 0.9300 . ? C6B C13B 1.492(9) . ? C7B C12B 1.414(10) . ? C7B C8B 1.414(10) . ? C8B C9B 1.381(12) . ? C8B C27B 1.544(12) . ? C9B C10B 1.383(13) . ? C9B H9B 0.9300 . ? C10B C11B 1.388(11) . ? C10B C31B 1.535(13) . ? C11B C12B 1.373(10) . ? C11B H11B 0.9300 . ? C12B C14B 1.500(9) . ? C13B H13C 0.9700 . ? C13B H13D 0.9700 . ? C14B H14C 0.9700 . ? C14B H14D 0.9700 . ? C15B C16B 1.534(10) . ? C15B H15C 0.9700 . ? C15B H15D 0.9700 . ? C16B C17B 1.509(13) . ? C16B H16C 0.9700 . ? C16B H16D 0.9700 . ? C17B C18B 1.511(15) . ? C17B H17E 0.9700 . ? C17B H17F 0.9700 . ? C18B H18G 0.9600 . ? C18B H18H 0.9600 . ? C18B H18I 0.9600 . ? C19B C21B 1.519(11) . ? C19B C22B 1.520(11) . ? C19B C20B 1.543(11) . ? C20B H20D 0.9600 . ? C20B H20E 0.9600 . ? C20B H20F 0.9600 . ? C21B H21D 0.9600 . ? C21B H21E 0.9600 . ? C21B H21F 0.9600 . ? C22B H22D 0.9600 . ? C22B H22E 0.9600 . ? C22B H22F 0.9600 . ? C23B C25D 1.512(19) . ? C23B C26D 1.519(18) . ? C23B C24D 1.531(19) . ? C23B C26B 1.542(14) . ? C23B C24B 1.549(15) . ? C23B C25B 1.56(2) . ? C24B H24G 0.9600 . ? C24B H24H 0.9600 . ? C24B H24I 0.9600 . ? C24D H24J 0.9600 . ? C24D H24K 0.9600 . ? C24D H24L 0.9600 . ? C25B H25G 0.9600 . ? C25B H25H 0.9600 . ? C25B H25I 0.9600 . ? C25D H25J 0.9600 . ? C25D H25K 0.9600 . ? C25D H25L 0.9600 . ? C26B H26G 0.9600 . ? C26B H26H 0.9600 . ? C26B H26I 0.9600 . ? C26D H26J 0.9600 . ? C26D H26K 0.9600 . ? C26D H26L 0.9600 . ? C27B C28B 1.514(15) . ? C27B C30B 1.540(15) . ? C27B C29B 1.550(13) . ? C28B H28D 0.9600 . ? C28B H28E 0.9600 . ? C28B H28F 0.9600 . ? C29B H29D 0.9600 . ? C29B H29E 0.9600 . ? C29B H29F 0.9600 . ? C30B H30D 0.9600 . ? C30B H30E 0.9600 . ? C30B H30F 0.9600 . ? C31B C32B 1.479(16) . ? C31B C33B 1.490(18) . ? C31B C34D 1.494(18) . ? C31B C33D 1.509(17) . ? C31B C32D 1.530(17) . ? C31B C34B 1.540(16) . ? C32B H32G 0.9600 . ? C32B H32H 0.9600 . ? C32B H32I 0.9600 . ? C32D H32J 0.9600 . ? C32D H32K 0.9600 . ? C32D H32L 0.9600 . ? C33B H33G 0.9600 . ? C33B H33H 0.9600 . ? C33B H33I 0.9600 . ? C33D H33J 0.9600 . ? C33D H33K 0.9600 . ? C33D H33L 0.9600 . ? C34B H34G 0.9600 . ? C34B H34H 0.9600 . ? C34B H34I 0.9600 . ? C34D H34J 0.9600 . ? C34D H34K 0.9600 . ? C34D H34L 0.9600 . ? C35B C36B 1.404(11) . ? C35B C40B 1.421(11) . ? C36B C37B 1.413(11) . ? C36B C53B 1.542(12) . ? C37B C38B 1.383(15) . ? C37B H37B 0.9300 . ? C38B C39B 1.363(15) . ? C38B C57B 1.546(13) . ? C39B C40B 1.394(12) . ? C39B H39B 0.9300 . ? C40B C47B 1.488(12) . ? C41B C42B 1.409(11) . ? C41B C46B 1.418(10) . ? C42B C43B 1.406(10) . ? C42B C61B 1.527(11) . ? C43B C44B 1.368(11) . ? C43B H43B 0.9300 . ? C44B C45B 1.377(12) . ? C44B C65B 1.543(10) . ? C45B C46B 1.388(10) . ? C45B H45B 0.9300 . ? C46B C48B 1.514(11) . ? C47B H47C 0.9700 . ? C47B H47D 0.9700 . ? C48B H48C 0.9700 . ? C48B H48D 0.9700 . ? C49B C50B 1.540(13) . ? C49B H49C 0.9700 . ? C49B H49D 0.9700 . ? C50B C51B 1.520(18) . ? C50B C51D 1.531(19) . ? C50B H50C 0.969(10) . ? C50B H50D 0.972(10) . ? C51B C52B 1.56(2) . ? C51B H51G 0.9700 . ? C51B H51H 0.9700 . ? C51D C52D 1.54(2) . ? C51D H51E 0.9700 . ? C51D H51F 0.9700 . ? C52B H52G 0.9600 . ? C52B H52H 0.9600 . ? C52B H52I 0.9600 . ? C52D H52J 0.9600 . ? C52D H52K 0.9600 . ? C52D H52L 0.9600 . ? C53B C56B 1.529(12) . ? C53B C55B 1.553(12) . ? C53B C54B 1.574(13) . ? C54B H54D 0.9600 . ? C54B H54E 0.9600 . ? C54B H54F 0.9600 . ? C55B H55D 0.9600 . ? C55B H55E 0.9600 . ? C55B H55F 0.9600 . ? C56B H56D 0.9600 . ? C56B H56E 0.9600 . ? C56B H56F 0.9600 . ? C57B C60B 1.47(3) . ? C57B C58B 1.478(16) . ? C57B C58D 1.511(18) . ? C57B C59D 1.511(19) . ? C57B C60D 1.517(18) . ? C57B C59B 1.532(17) . ? C58B H58G 0.9600 . ? C58B H58H 0.9600 . ? C58B H58I 0.9600 . ? C58D H58J 0.9600 . ? C58D H58K 0.9600 . ? C58D H58L 0.9600 . ? C59B H59G 0.9600 . ? C59B H59H 0.9600 . ? C59B H59I 0.9600 . ? C59D H59J 0.9600 . ? C59D H59K 0.9600 . ? C59D H59L 0.9600 . ? C60B H60G 0.9600 . ? C60B H60H 0.9600 . ? C60B H60I 0.9600 . ? C60D H60J 0.9600 . ? C60D H60K 0.9600 . ? C60D H60L 0.9600 . ? C61B C62B 1.532(12) . ? C61B C64B 1.537(12) . ? C61B C63B 1.544(12) . ? C62B H62D 0.9600 . ? C62B H62E 0.9600 . ? C62B H62F 0.9600 . ? C63B H63D 0.9600 . ? C63B H63E 0.9600 . ? C63B H63F 0.9600 . ? C64B H64D 0.9600 . ? C64B H64E 0.9600 . ? C64B H64F 0.9600 . ? C65B C66B 1.504(16) . ? C65B C67B 1.532(15) . ? C65B C68B 1.533(15) . ? C66B H66G 0.9600 . ? C66B H66H 0.9600 . ? C66B H66I 0.9600 . ? C67B H67G 0.9600 . ? C67B H67H 0.9600 . ? C67B H67I 0.9600 . ? C68B H68G 0.9600 . ? C68B H68H 0.9600 . ? C68B H68I 0.9600 . ? C69 C70 1.380(17) . ? C69 C74 1.381(16) . ? C69 C75 1.497(18) . ? C70 C71 1.381(18) . ? C70 H70 0.9300 . ? C71 C72 1.400(19) . ? C71 H71 0.9300 . ? C72 C73 1.392(18) . ? C72 H72 0.9300 . ? C73 C74 1.377(16) . ? C73 H73 0.9300 . ? C74 H74 0.9300 . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C76 C77 1.538(17) . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C77 C78 1.542(17) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 C79 1.488(18) . ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 C82 1.386(18) 2_656 ? C80 C81 1.395(18) . ? C80 C83 1.515(19) . ? C81 C82 1.412(19) . ? C81 H81 0.9300 . ? C82 C80 1.386(18) 2_656 ? C82 H82 0.9300 . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? 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 O1A Sm1 O3B 178.48(15) . . ? O1A Sm1 O1B 111.01(15) . . ? O3B Sm1 O1B 67.58(15) . . ? O1A Sm1 O3A 68.10(15) . . ? O3B Sm1 O3A 113.32(16) . . ? O1B Sm1 O3A 179.03(15) . . ? O1A Sm1 Sm2A 33.84(10) . . ? O3B Sm1 Sm2A 147.59(11) . . ? O1B Sm1 Sm2A 144.83(10) . . ? O3A Sm1 Sm2A 34.27(11) . . ? O1A Sm1 Sm2B 145.04(11) . . ? O3B Sm1 Sm2B 33.54(11) . . ? O1B Sm1 Sm2B 34.04(10) . . ? O3A Sm1 Sm2B 146.85(11) . . ? Sm2A Sm1 Sm2B 178.697(14) . . ? O2A Sm2A O4A 108.13(19) . . ? O2A Sm2A O1A 144.15(16) . . ? O4A Sm2A O1A 97.65(17) . . ? O2A Sm2A O3A 97.70(18) . . ? O4A Sm2A O3A 144.69(17) . . ? O1A Sm2A O3A 72.45(16) . . ? O2A Sm2A N1A 73.60(18) . . ? O4A Sm2A N1A 101.67(18) . . ? O1A Sm2A N1A 77.15(16) . . ? O3A Sm2A N1A 108.58(17) . . ? O2A Sm2A N2A 100.84(18) . . ? O4A Sm2A N2A 74.63(18) . . ? O1A Sm2A N2A 109.90(17) . . ? O3A Sm2A N2A 77.22(17) . . ? N1A Sm2A N2A 172.25(18) . . ? O2A Sm2A Sm1 125.89(13) . . ? O4A Sm2A Sm1 125.96(13) . . ? O1A Sm2A Sm1 35.59(11) . . ? O3A Sm2A Sm1 36.87(11) . . ? N1A Sm2A Sm1 92.64(12) . . ? N2A Sm2A Sm1 95.02(13) . . ? O2B Sm2B O4B 108.05(19) . . ? O2B Sm2B O3B 99.35(19) . . ? O4B Sm2B O3B 143.52(17) . . ? O2B Sm2B O1B 145.86(17) . . ? O4B Sm2B O1B 96.38(18) . . ? O3B Sm2B O1B 71.58(16) . . ? O2B Sm2B N1B 74.55(17) . . ? O4B Sm2B N1B 100.81(17) . . ? O3B Sm2B N1B 109.53(16) . . ? O1B Sm2B N1B 77.77(15) . . ? O2B Sm2B N2B 100.03(19) . . ? O4B Sm2B N2B 74.08(19) . . ? O3B Sm2B N2B 77.87(17) . . ? O1B Sm2B N2B 109.57(17) . . ? N1B Sm2B N2B 171.26(17) . . ? O2B Sm2B Sm1 127.58(14) . . ? O4B Sm2B Sm1 124.37(13) . . ? O3B Sm2B Sm1 35.49(11) . . ? O1B Sm2B Sm1 36.09(11) . . ? N1B Sm2B Sm1 94.71(11) . . ? N2B Sm2B Sm1 94.03(13) . . ? C1A O1A Sm2A 115.1(4) . . ? C1A O1A Sm1 133.5(4) . . ? Sm2A O1A Sm1 110.57(17) . . ? C7A O2A Sm2A 146.6(4) . . ? C35A O3A Sm2A 119.7(4) . . ? C35A O3A Sm1 130.0(4) . . ? Sm2A O3A Sm1 108.86(18) . . ? C41A O4A Sm2A 145.1(4) . . ? C1B O1B Sm2B 117.1(4) . . ? C1B O1B Sm1 132.0(4) . . ? Sm2B O1B Sm1 109.87(17) . . ? C7B O2B Sm2B 145.5(4) . . ? C35B O3B Sm2B 117.3(4) . . ? C35B O3B Sm1 130.9(4) . . ? Sm2B O3B Sm1 110.97(18) . . ? C41B O4B Sm2B 146.9(5) . . ? C76 O5 C79 115(2) . . ? C14A N1A C13A 106.6(5) . . ? C14A N1A C15A 112.3(5) . . ? C13A N1A C15A 112.4(6) . . ? C14A N1A Sm2A 105.3(4) . . ? C13A N1A Sm2A 109.3(4) . . ? C15A N1A Sm2A 110.6(4) . . ? C47A N2A C49A 111.8(6) . . ? C47A N2A C48A 107.3(5) . . ? C49A N2A C48A 112.0(6) . . ? C47A N2A Sm2A 109.4(4) . . ? C49A N2A Sm2A 110.1(4) . . ? C48A N2A Sm2A 106.0(4) . . ? C14B N1B C13B 107.5(5) . . ? C14B N1B C15B 111.1(5) . . ? C13B N1B C15B 111.9(5) . . ? C14B N1B Sm2B 106.3(4) . . ? C13B N1B Sm2B 108.6(4) . . ? C15B N1B Sm2B 111.1(4) . . ? C49B N2B C47B 112.0(7) . . ? C49B N2B C48B 113.0(6) . . ? C47B N2B C48B 107.0(6) . . ? C49B N2B Sm2B 110.0(4) . . ? C47B N2B Sm2B 107.9(4) . . ? C48B N2B Sm2B 106.7(4) . . ? O1A C1A C6A 117.0(6) . . ? O1A C1A C2A 123.7(6) . . ? C6A C1A C2A 119.3(6) . . ? C3A C2A C1A 116.6(7) . . ? C3A C2A C19A 118.2(7) . . ? C1A C2A C19A 125.2(6) . . ? C4A C3A C2A 126.2(8) . . ? C4A C3A H3A 116.9 . . ? C2A C3A H3A 116.9 . . ? C3A C4A C5A 115.9(7) . . ? C3A C4A C23A 122.4(8) . . ? C5A C4A C23A 121.7(8) . . ? C4A C5A C6A 121.7(8) . . ? C4A C5A H5A 119.2 . . ? C6A C5A H5A 119.2 . . ? C5A C6A C1A 120.3(7) . . ? C5A C6A C13A 120.6(7) . . ? C1A C6A C13A 119.1(6) . . ? O2A C7A C8A 122.7(6) . . ? O2A C7A C12A 118.3(6) . . ? C8A C7A C12A 119.0(6) . . ? C9A C8A C7A 118.0(6) . . ? C9A C8A C27A 121.3(6) . . ? C7A C8A C27A 120.7(6) . . ? C10A C9A C8A 123.9(7) . . ? C10A C9A H9A 118.1 . . ? C8A C9A H9A 118.1 . . ? C11A C10A C9A 116.6(7) . . ? C11A C10A C31A 119.7(7) . . ? C9A C10A C31A 123.7(7) . . ? C10A C11A C12A 122.2(7) . . ? C10A C11A H11A 118.9 . . ? C12A C11A H11A 118.9 . . ? C11A C12A C7A 120.3(6) . . ? C11A C12A C14A 119.8(6) . . ? C7A C12A C14A 119.9(6) . . ? N1A C13A C6A 113.8(6) . . ? N1A C13A H13A 108.8 . . ? C6A C13A H13A 108.8 . . ? N1A C13A H13B 108.8 . . ? C6A C13A H13B 108.8 . . ? H13A C13A H13B 107.7 . . ? N1A C14A C12A 117.2(6) . . ? N1A C14A H14A 108.0 . . ? C12A C14A H14A 108.0 . . ? N1A C14A H14B 108.0 . . ? C12A C14A H14B 108.0 . . ? H14A C14A H14B 107.2 . . ? N1A C15A C16A 116.9(6) . . ? N1A C15A H15A 108.1 . . ? C16A C15A H15A 108.1 . . ? N1A C15A H15B 108.1 . . ? C16A C15A H15B 108.1 . . ? H15A C15A H15B 107.3 . . ? C17C C16A C17A 25.0(12) . . ? C17C C16A C15A 113.2(13) . . ? C17A C16A C15A 107.2(11) . . ? C17C C16A H16A 82(6) . . ? C17A C16A H16A 107(7) . . ? C15A C16A H16A 106(7) . . ? C17C C16A H16B 121(4) . . ? C17A C16A H16B 101(4) . . ? C15A C16A H16B 105(4) . . ? H16A C16A H16B 129(8) . . ? C16A C17A C18A 111(2) . . ? C16A C17A H17A 109.4 . . ? C18A C17A H17A 109.4 . . ? C16A C17A H17B 109.4 . . ? C18A C17A H17B 109.4 . . ? H17A C17A H17B 108.0 . . ? C16A C17C C18C 99(3) . . ? C16A C17C H17C 112.1 . . ? C18C C17C H17C 112.1 . . ? C16A C17C H17D 112.1 . . ? C18C C17C H17D 112.1 . . ? H17C C17C H17D 109.7 . . ? C17A C18A H18A 109.5 . . ? C17A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C17C C18C H18D 109.5 . . ? C17C C18C H18E 109.5 . . ? H18D C18C H18E 109.5 . . ? C17C C18C H18F 109.5 . . ? H18D C18C H18F 109.5 . . ? H18E C18C H18F 109.5 . . ? C21A C19A C2A 116.0(6) . . ? C21A C19A C20A 109.4(7) . . ? C2A C19A C20A 107.4(6) . . ? C21A C19A C22A 105.6(7) . . ? C2A C19A C22A 110.3(7) . . ? C20A C19A C22A 107.9(7) . . ? C19A C20A H20A 109.5 . . ? C19A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? C19A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C19A C21A H21A 109.5 . . ? C19A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C19A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C19A C22A H22A 109.5 . . ? C19A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? C19A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C26C C23A C25A 57.5(19) . . ? C26C C23A C24A 132(3) . . ? C25A C23A C24A 106.7(19) . . ? C26C C23A C25C 102(2) . . ? C25A C23A C25C 48.1(14) . . ? C24A C23A C25C 62.9(18) . . ? C26C C23A C24C 120(2) . . ? C25A C23A C24C 134.0(15) . . ? C24A C23A C24C 35.7(16) . . ? C25C C23A C24C 97.7(17) . . ? C26C C23A C26A 47.3(19) . . ? C25A C23A C26A 104.4(14) . . ? C24A C23A C26A 116(2) . . ? C25C C23A C26A 140.9(17) . . ? C24C C23A C26A 84.1(14) . . ? C26C C23A C4A 115(2) . . ? C25A C23A C4A 108.9(12) . . ? C24A C23A C4A 112.7(17) . . ? C25C C23A C4A 107.8(14) . . ? C24C C23A C4A 111.1(12) . . ? C26A C23A C4A 107.9(11) . . ? C23A C24A H24A 109.5 . . ? C23A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C23A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? C23A C24C H24D 109.5 . . ? C23A C24C H24E 109.5 . . ? H24D C24C H24E 109.5 . . ? C23A C24C H24F 109.5 . . ? H24D C24C H24F 109.5 . . ? H24E C24C H24F 109.5 . . ? C23A C25A H25A 109.5 . . ? C23A C25A H25B 109.5 . . ? H25A C25A H25B 109.5 . . ? C23A C25A H25C 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? C23A C25C H25D 109.5 . . ? C23A C25C H25E 109.5 . . ? H25D C25C H25E 109.5 . . ? C23A C25C H25F 109.5 . . ? H25D C25C H25F 109.5 . . ? H25E C25C H25F 109.5 . . ? C23A C26A H26A 109.5 . . ? C23A C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? C23A C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? C23A C26C H26D 109.5 . . ? C23A C26C H26E 109.5 . . ? H26D C26C H26E 109.5 . . ? C23A C26C H26F 109.5 . . ? H26D C26C H26F 109.5 . . ? H26E C26C H26F 109.5 . . ? C30A C27A C29A 110.6(7) . . ? C30A C27A C8A 110.2(7) . . ? C29A C27A C8A 109.8(7) . . ? C30A C27A C28A 105.8(7) . . ? C29A C27A C28A 108.3(8) . . ? C8A C27A C28A 112.0(6) . . ? C27A C28A H28A 109.5 . . ? C27A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C27A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C27A C30A H30A 109.5 . . ? C27A C30A H30B 109.5 . . ? H30A C30A H30B 109.5 . . ? C27A C30A H30C 109.5 . . ? H30A C30A H30C 109.5 . . ? H30B C30A H30C 109.5 . . ? C32C C31A C33C 127(2) . . ? C32C C31A C34C 91(2) . . ? C33C C31A C34C 98(3) . . ? C32C C31A C34A 135.9(16) . . ? C33C C31A C34A 38.7(15) . . ? C34C C31A C34A 62(2) . . ? C32C C31A C32A 37.3(13) . . ? C33C C31A C32A 128.0(18) . . ? C34C C31A C32A 54(2) . . ? C34A C31A C32A 109.1(12) . . ? C32C C31A C10A 111.8(15) . . ? C33C C31A C10A 116.9(16) . . ? C34C C31A C10A 101(2) . . ? C34A C31A C10A 107.7(10) . . ? C32A C31A C10A 111.5(9) . . ? C32C C31A C33A 73.4(16) . . ? C33C C31A C33A 74.1(17) . . ? C34C C31A C33A 151(2) . . ? C34A C31A C33A 112.5(12) . . ? C32A C31A C33A 108.5(12) . . ? C10A C31A C33A 107.5(9) . . ? C31A C32A H32A 109.5 . . ? C31A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C31A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C31A C32C H32D 109.5 . . ? C31A C32C H32E 109.5 . . ? H32D C32C H32E 109.5 . . ? C31A C32C H32F 109.5 . . ? H32D C32C H32F 109.5 . . ? H32E C32C H32F 109.5 . . ? C31A C33A H33A 109.5 . . ? C31A C33A H33B 109.5 . . ? H33A C33A H33B 109.5 . . ? C31A C33A H33C 109.5 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? C31A C33C H33D 109.5 . . ? C31A C33C H33E 109.5 . . ? H33D C33C H33E 109.5 . . ? C31A C33C H33F 109.5 . . ? H33D C33C H33F 109.5 . . ? H33E C33C H33F 109.5 . . ? C31A C34A H34A 109.5 . . ? C31A C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? C31A C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? C31A C34C H34D 109.5 . . ? C31A C34C H34E 109.5 . . ? H34D C34C H34E 109.5 . . ? C31A C34C H34F 109.5 . . ? H34D C34C H34F 109.5 . . ? H34E C34C H34F 109.5 . . ? O3A C35A C40A 117.7(6) . . ? O3A C35A C36A 123.7(7) . . ? C40A C35A C36A 118.5(7) . . ? C37A C36A C35A 117.1(8) . . ? C37A C36A C53A 118.6(7) . . ? C35A C36A C53A 124.0(7) . . ? C38A C37A C36A 125.4(8) . . ? C38A C37A H37A 117.3 . . ? C36A C37A H37A 117.3 . . ? C37A C38A C39A 115.9(8) . . ? C37A C38A C57A 122.7(9) . . ? C39A C38A C57A 121.5(9) . . ? C38A C39A C40A 122.2(8) . . ? C38A C39A H39A 118.9 . . ? C40A C39A H39A 118.9 . . ? C39A C40A C35A 120.8(7) . . ? C39A C40A C47A 118.9(7) . . ? C35A C40A C47A 120.4(7) . . ? O4A C41A C42A 123.9(6) . . ? O4A C41A C46A 117.6(6) . . ? C42A C41A C46A 118.5(6) . . ? C43A C42A C41A 118.0(7) . . ? C43A C42A C61A 121.5(7) . . ? C41A C42A C61A 120.4(6) . . ? C44A C43A C42A 125.0(8) . . ? C44A C43A H43A 117.5 . . ? C42A C43A H43A 117.5 . . ? C43A C44A C45A 116.3(7) . . ? C43A C44A C65A 123.6(8) . . ? C45A C44A C65A 120.1(8) . . ? C44A C45A C46A 121.7(7) . . ? C44A C45A H45A 119.1 . . ? C46A C45A H45A 119.1 . . ? C45A C46A C41A 120.2(7) . . ? C45A C46A C48A 120.5(7) . . ? C41A C46A C48A 119.2(6) . . ? N2A C47A C40A 114.4(6) . . ? N2A C47A H47A 108.7 . . ? C40A C47A H47A 108.7 . . ? N2A C47A H47B 108.7 . . ? C40A C47A H47B 108.7 . . ? H47A C47A H47B 107.6 . . ? N2A C48A C46A 115.7(6) . . ? N2A C48A H48A 108.3 . . ? C46A C48A H48A 108.3 . . ? N2A C48A H48B 108.3 . . ? C46A C48A H48B 108.3 . . ? H48A C48A H48B 107.4 . . ? N2A C49A C50A 117.8(7) . . ? N2A C49A H49A 107.9 . . ? C50A C49A H49A 107.9 . . ? N2A C49A H49B 107.9 . . ? C50A C49A H49B 107.9 . . ? H49A C49A H49B 107.2 . . ? C51A C50A C49A 113.7(12) . . ? C51A C50A C51C 26.8(17) . . ? C49A C50A C51C 108.8(15) . . ? C51A C50A H50A 112(9) . . ? C49A C50A H50A 102(8) . . ? C51C C50A H50A 136(9) . . ? C51A C50A H50B 127(6) . . ? C49A C50A H50B 109(6) . . ? C51C C50A H50B 110(6) . . ? H50A C50A H50B 88(9) . . ? C50A C51A C52A 112(2) . . ? C50A C51A H51A 109.2 . . ? C52A C51A H51A 109.2 . . ? C50A C51A H51B 109.2 . . ? C52A C51A H51B 109.2 . . ? H51A C51A H51B 107.9 . . ? C52C C51C C50A 115(3) . . ? C52C C51C H51C 108.6 . . ? C50A C51C H51C 108.6 . . ? C52C C51C H51D 108.6 . . ? C50A C51C H51D 108.6 . . ? H51C C51C H51D 107.6 . . ? C51A C52A H52A 109.5 . . ? C51A C52A H52B 109.5 . . ? H52A C52A H52B 109.5 . . ? C51A C52A H52C 109.5 . . ? H52A C52A H52C 109.5 . . ? H52B C52A H52C 109.5 . . ? C51C C52C H52D 109.5 . . ? C51C C52C H52E 109.5 . . ? H52D C52C H52E 109.5 . . ? C51C C52C H52F 109.5 . . ? H52D C52C H52F 109.5 . . ? H52E C52C H52F 109.5 . . ? C55A C53A C56A 110.1(8) . . ? C55A C53A C36A 108.6(7) . . ? C56A C53A C36A 113.8(6) . . ? C55A C53A C54A 109.4(7) . . ? C56A C53A C54A 105.2(7) . . ? C36A C53A C54A 109.8(7) . . ? C53A C54A H54A 109.5 . . ? C53A C54A H54B 109.5 . . ? H54A C54A H54B 109.5 . . ? C53A C54A H54C 109.5 . . ? H54A C54A H54C 109.5 . . ? H54B C54A H54C 109.5 . . ? C53A C55A H55A 109.5 . . ? C53A C55A H55B 109.5 . . ? H55A C55A H55B 109.5 . . ? C53A C55A H55C 109.5 . . ? H55A C55A H55C 109.5 . . ? H55B C55A H55C 109.5 . . ? C53A C56A H56A 109.5 . . ? C53A C56A H56B 109.5 . . ? H56A C56A H56B 109.5 . . ? C53A C56A H56C 109.5 . . ? H56A C56A H56C 109.5 . . ? H56B C56A H56C 109.5 . . ? C58A C57A C60C 44.1(15) . . ? C58A C57A C59C 132(2) . . ? C60C C57A C59C 114(2) . . ? C58A C57A C58C 50.2(16) . . ? C60C C57A C58C 94(2) . . ? C59C C57A C58C 114(2) . . ? C58A C57A C59A 113.9(18) . . ? C60C C57A C59A 140.7(19) . . ? C59C C57A C59A 51.0(16) . . ? C58C C57A C59A 69.1(19) . . ? C58A C57A C60A 110.2(19) . . ? C60C C57A C60A 70.6(19) . . ? C59C C57A C60A 50.0(16) . . ? C58C C57A C60A 141(2) . . ? C59A C57A C60A 100.4(16) . . ? C58A C57A C38A 115.1(14) . . ? C60C C57A C38A 112.1(17) . . ? C59C C57A C38A 112.6(17) . . ? C58C C57A C38A 109.8(17) . . ? C59A C57A C38A 107.1(15) . . ? C60A C57A C38A 109.1(15) . . ? C57A C58A H58A 109.5 . . ? C57A C58A H58B 109.5 . . ? H58A C58A H58B 109.5 . . ? C57A C58A H58C 109.5 . . ? H58A C58A H58C 109.5 . . ? H58B C58A H58C 109.5 . . ? C57A C58C H58D 109.5 . . ? C57A C58C H58E 109.5 . . ? H58D C58C H58E 109.5 . . ? C57A C58C H58F 109.5 . . ? H58D C58C H58F 109.5 . . ? H58E C58C H58F 109.5 . . ? C57A C59A H59A 109.5 . . ? C57A C59A H59B 109.5 . . ? H59A C59A H59B 109.5 . . ? C57A C59A H59C 109.5 . . ? H59A C59A H59C 109.5 . . ? H59B C59A H59C 109.5 . . ? C57A C59C H59D 109.5 . . ? C57A C59C H59E 109.5 . . ? H59D C59C H59E 109.5 . . ? C57A C59C H59F 109.5 . . ? H59D C59C H59F 109.5 . . ? H59E C59C H59F 109.5 . . ? C57A C60A H60A 109.5 . . ? C57A C60A H60B 109.5 . . ? H60A C60A H60B 109.5 . . ? C57A C60A H60C 109.5 . . ? H60A C60A H60C 109.5 . . ? H60B C60A H60C 109.5 . . ? C57A C60C H60D 109.5 . . ? C57A C60C H60E 109.5 . . ? H60D C60C H60E 109.5 . . ? C57A C60C H60F 109.5 . . ? H60D C60C H60F 109.5 . . ? H60E C60C H60F 109.5 . . ? C63A C61A C62A 106.1(7) . . ? C63A C61A C42A 110.4(7) . . ? C62A C61A C42A 112.9(7) . . ? C63A C61A C64A 109.5(7) . . ? C62A C61A C64A 107.7(7) . . ? C42A C61A C64A 110.1(6) . . ? C61A C62A H62A 109.5 . . ? C61A C62A H62B 109.5 . . ? H62A C62A H62B 109.5 . . ? C61A C62A H62C 109.5 . . ? H62A C62A H62C 109.5 . . ? H62B C62A H62C 109.5 . . ? C61A C63A H63A 109.5 . . ? C61A C63A H63B 109.5 . . ? H63A C63A H63B 109.5 . . ? C61A C63A H63C 109.5 . . ? H63A C63A H63C 109.5 . . ? H63B C63A H63C 109.5 . . ? C61A C64A H64A 109.5 . . ? C61A C64A H64B 109.5 . . ? H64A C64A H64B 109.5 . . ? C61A C64A H64C 109.5 . . ? H64A C64A H64C 109.5 . . ? H64B C64A H64C 109.5 . . ? C68A C65A C66A 108.5(12) . . ? C68A C65A C66C 56.4(19) . . ? C66A C65A C66C 55.3(19) . . ? C68A C65A C67C 124.8(17) . . ? C66A C65A C67C 83.9(17) . . ? C66C C65A C67C 127(2) . . ? C68A C65A C67A 104.5(12) . . ? C66A C65A C67A 113.2(13) . . ? C66C C65A C67A 140(2) . . ? C67C C65A C67A 30.6(14) . . ? C68A C65A C44A 113.1(11) . . ? C66A C65A C44A 108.7(10) . . ? C66C C65A C44A 111.4(19) . . ? C67C C65A C44A 112.7(15) . . ? C67A C65A C44A 108.9(10) . . ? C68A C65A C68C 44.5(15) . . ? C66A C65A C68C 140.7(18) . . ? C66C C65A C68C 100(2) . . ? C67C C65A C68C 92(2) . . ? C67A C65A C68C 64.0(16) . . ? C44A C65A C68C 108.8(16) . . ? C65A C66A H66A 109.5 . . ? C65A C66A H66B 109.5 . . ? H66A C66A H66B 109.5 . . ? C65A C66A H66C 109.5 . . ? H66A C66A H66C 109.5 . . ? H66B C66A H66C 109.5 . . ? C65A C66C H66D 109.5 . . ? C65A C66C H66E 109.5 . . ? H66D C66C H66E 109.5 . . ? C65A C66C H66F 109.5 . . ? H66D C66C H66F 109.5 . . ? H66E C66C H66F 109.5 . . ? C65A C67A H67A 109.5 . . ? C65A C67A H67B 109.5 . . ? H67A C67A H67B 109.5 . . ? C65A C67A H67C 109.5 . . ? H67A C67A H67C 109.5 . . ? H67B C67A H67C 109.5 . . ? C65A C67C H67D 109.5 . . ? C65A C67C H67E 109.5 . . ? H67D C67C H67E 109.5 . . ? C65A C67C H67F 109.5 . . ? H67D C67C H67F 109.5 . . ? H67E C67C H67F 109.5 . . ? C65A C68A H68A 109.5 . . ? C65A C68A H68B 109.5 . . ? H68A C68A H68B 109.5 . . ? C65A C68A H68C 109.5 . . ? H68A C68A H68C 109.5 . . ? H68B C68A H68C 109.5 . . ? C65A C68C H68D 109.5 . . ? C65A C68C H68E 109.5 . . ? H68D C68C H68E 109.5 . . ? C65A C68C H68F 109.5 . . ? H68D C68C H68F 109.5 . . ? H68E C68C H68F 109.5 . . ? O1B C1B C2B 124.9(6) . . ? O1B C1B C6B 116.5(6) . . ? C2B C1B C6B 118.6(6) . . ? C3B C2B C1B 117.0(7) . . ? C3B C2B C19B 118.7(7) . . ? C1B C2B C19B 124.1(6) . . ? C4B C3B C2B 125.5(7) . . ? C4B C3B H3B 117.2 . . ? C2B C3B H3B 117.2 . . ? C3B C4B C5B 116.9(7) . . ? C3B C4B C23B 124.0(8) . . ? C5B C4B C23B 119.1(8) . . ? C4B C5B C6B 121.1(7) . . ? C4B C5B H5B 119.4 . . ? C6B C5B H5B 119.4 . . ? C5B C6B C1B 120.9(6) . . ? C5B C6B C13B 119.0(6) . . ? C1B C6B C13B 120.1(6) . . ? O2B C7B C12B 117.8(6) . . ? O2B C7B C8B 123.7(7) . . ? C12B C7B C8B 118.5(7) . . ? C9B C8B C7B 117.3(7) . . ? C9B C8B C27B 122.3(7) . . ? C7B C8B C27B 120.4(7) . . ? C8B C9B C10B 125.5(7) . . ? C8B C9B H9B 117.3 . . ? C10B C9B H9B 117.3 . . ? C9B C10B C11B 115.6(8) . . ? C9B C10B C31B 123.8(8) . . ? C11B C10B C31B 120.6(9) . . ? C12B C11B C10B 122.4(8) . . ? C12B C11B H11B 118.8 . . ? C10B C11B H11B 118.8 . . ? C11B C12B C7B 120.5(7) . . ? C11B C12B C14B 119.6(6) . . ? C7B C12B C14B 119.9(6) . . ? C6B C13B N1B 112.9(5) . . ? C6B C13B H13C 109.0 . . ? N1B C13B H13C 109.0 . . ? C6B C13B H13D 109.0 . . ? N1B C13B H13D 109.0 . . ? H13C C13B H13D 107.8 . . ? N1B C14B C12B 116.4(6) . . ? N1B C14B H14C 108.2 . . ? C12B C14B H14C 108.2 . . ? N1B C14B H14D 108.2 . . ? C12B C14B H14D 108.2 . . ? H14C C14B H14D 107.3 . . ? N1B C15B C16B 117.2(6) . . ? N1B C15B H15C 108.0 . . ? C16B C15B H15C 108.0 . . ? N1B C15B H15D 108.0 . . ? C16B C15B H15D 108.0 . . ? H15C C15B H15D 107.3 . . ? C17B C16B C15B 111.7(7) . . ? C17B C16B H16C 109.3 . . ? C15B C16B H16C 109.3 . . ? C17B C16B H16D 109.3 . . ? C15B C16B H16D 109.3 . . ? H16C C16B H16D 107.9 . . ? C16B C17B C18B 112.0(10) . . ? C16B C17B H17E 109.2 . . ? C18B C17B H17E 109.2 . . ? C16B C17B H17F 109.2 . . ? C18B C17B H17F 109.2 . . ? H17E C17B H17F 107.9 . . ? C17B C18B H18G 109.5 . . ? C17B C18B H18H 109.5 . . ? H18G C18B H18H 109.5 . . ? C17B C18B H18I 109.5 . . ? H18G C18B H18I 109.5 . . ? H18H C18B H18I 109.5 . . ? C21B C19B C22B 109.8(7) . . ? C21B C19B C20B 109.0(7) . . ? C22B C19B C20B 105.9(7) . . ? C21B C19B C2B 108.0(6) . . ? C22B C19B C2B 115.0(6) . . ? C20B C19B C2B 109.0(7) . . ? C19B C20B H20D 109.5 . . ? C19B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C19B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C19B C21B H21D 109.5 . . ? C19B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C19B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C19B C22B H22D 109.5 . . ? C19B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C19B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? C25D C23B C26D 133(3) . . ? C25D C23B C24D 86(3) . . ? C26D C23B C24D 106(2) . . ? C25D C23B C26B 67(3) . . ? C26D C23B C26B 76.4(17) . . ? C24D C23B C26B 140(2) . . ? C25D C23B C4B 105(2) . . ? C26D C23B C4B 115.2(16) . . ? C24D C23B C4B 105(2) . . ? C26B C23B C4B 110.1(10) . . ? C25D C23B C24B 144(3) . . ? C26D C23B C24B 32.0(14) . . ? C24D C23B C24B 77(2) . . ? C26B C23B C24B 107.6(13) . . ? C4B C23B C24B 109.5(11) . . ? C25D C23B C25B 46(2) . . ? C26D C23B C25B 126.2(18) . . ? C24D C23B C25B 39.9(18) . . ? C26B C23B C25B 106.4(12) . . ? C4B C23B C25B 113.7(11) . . ? C24B C23B C25B 109.4(13) . . ? C23B C24B H24G 109.5 . . ? C23B C24B H24H 109.5 . . ? H24G C24B H24H 109.5 . . ? C23B C24B H24I 109.5 . . ? H24G C24B H24I 109.5 . . ? H24H C24B H24I 109.5 . . ? C23B C24D H24J 109.5 . . ? C23B C24D H24K 109.5 . . ? H24J C24D H24K 109.5 . . ? C23B C24D H24L 109.5 . . ? H24J C24D H24L 109.5 . . ? H24K C24D H24L 109.5 . . ? C23B C25B H25G 109.5 . . ? C23B C25B H25H 109.5 . . ? H25G C25B H25H 109.5 . . ? C23B C25B H25I 109.5 . . ? H25G C25B H25I 109.5 . . ? H25H C25B H25I 109.5 . . ? C23B C25D H25J 109.5 . . ? C23B C25D H25K 109.5 . . ? H25J C25D H25K 109.5 . . ? C23B C25D H25L 109.5 . . ? H25J C25D H25L 109.5 . . ? H25K C25D H25L 109.5 . . ? C23B C26B H26G 109.5 . . ? C23B C26B H26H 109.5 . . ? H26G C26B H26H 109.5 . . ? C23B C26B H26I 109.5 . . ? H26G C26B H26I 109.5 . . ? H26H C26B H26I 109.5 . . ? C23B C26D H26J 109.5 . . ? C23B C26D H26K 109.5 . . ? H26J C26D H26K 109.5 . . ? C23B C26D H26L 109.5 . . ? H26J C26D H26L 109.5 . . ? H26K C26D H26L 109.5 . . ? C28B C27B C30B 111.0(9) . . ? C28B C27B C8B 109.4(8) . . ? C30B C27B C8B 109.0(8) . . ? C28B C27B C29B 108.0(9) . . ? C30B C27B C29B 108.7(10) . . ? C8B C27B C29B 110.7(8) . . ? C27B C28B H28D 109.5 . . ? C27B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C27B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C27B C30B H30D 109.5 . . ? C27B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? C27B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? C32B C31B C33B 107(2) . . ? C32B C31B C34D 127.5(19) . . ? C33B C31B C34D 69.6(19) . . ? C32B C31B C33D 73.6(17) . . ? C33B C31B C33D 39.9(17) . . ? C34D C31B C33D 107(2) . . ? C32B C31B C32D 38.0(13) . . ? C33B C31B C32D 138(2) . . ? C34D C31B C32D 109(2) . . ? C33D C31B C32D 111.2(18) . . ? C32B C31B C10B 117.4(13) . . ? C33B C31B C10B 108.9(18) . . ? C34D C31B C10B 112.3(16) . . ? C33D C31B C10B 107.4(15) . . ? C32D C31B C10B 109.7(14) . . ? C32B C31B C34B 106.6(17) . . ? C33B C31B C34B 102.4(19) . . ? C34D C31B C34B 35.0(14) . . ? C33D C31B C34B 132.8(17) . . ? C32D C31B C34B 77.2(16) . . ? C10B C31B C34B 113.0(13) . . ? C31B C32B H32G 109.5 . . ? C31B C32B H32H 109.5 . . ? H32G C32B H32H 109.5 . . ? C31B C32B H32I 109.5 . . ? H32G C32B H32I 109.5 . . ? H32H C32B H32I 109.5 . . ? C31B C32D H32J 109.5 . . ? C31B C32D H32K 109.5 . . ? H32J C32D H32K 109.5 . . ? C31B C32D H32L 109.5 . . ? H32J C32D H32L 109.5 . . ? H32K C32D H32L 109.5 . . ? C31B C33B H33G 109.5 . . ? C31B C33B H33H 109.5 . . ? H33G C33B H33H 109.5 . . ? C31B C33B H33I 109.5 . . ? H33G C33B H33I 109.5 . . ? H33H C33B H33I 109.5 . . ? C31B C33D H33J 109.5 . . ? C31B C33D H33K 109.5 . . ? H33J C33D H33K 109.5 . . ? C31B C33D H33L 109.5 . . ? H33J C33D H33L 109.5 . . ? H33K C33D H33L 109.5 . . ? C31B C34B H34G 109.5 . . ? C31B C34B H34H 109.5 . . ? H34G C34B H34H 109.5 . . ? C31B C34B H34I 109.5 . . ? H34G C34B H34I 109.5 . . ? H34H C34B H34I 109.5 . . ? C31B C34D H34J 109.5 . . ? C31B C34D H34K 109.5 . . ? H34J C34D H34K 109.5 . . ? C31B C34D H34L 109.5 . . ? H34J C34D H34L 109.5 . . ? H34K C34D H34L 109.5 . . ? O3B C35B C36B 123.5(7) . . ? O3B C35B C40B 116.7(7) . . ? C36B C35B C40B 119.8(7) . . ? C35B C36B C37B 116.9(9) . . ? C35B C36B C53B 125.3(7) . . ? C37B C36B C53B 117.5(8) . . ? C38B C37B C36B 123.9(10) . . ? C38B C37B H37B 118.1 . . ? C36B C37B H37B 118.1 . . ? C39B C38B C37B 117.8(8) . . ? C39B C38B C57B 119.9(11) . . ? C37B C38B C57B 122.3(12) . . ? C38B C39B C40B 122.1(9) . . ? C38B C39B H39B 119.0 . . ? C40B C39B H39B 119.0 . . ? C39B C40B C35B 119.6(9) . . ? C39B C40B C47B 120.8(8) . . ? C35B C40B C47B 119.6(7) . . ? O4B C41B C42B 123.5(7) . . ? O4B C41B C46B 117.7(7) . . ? C42B C41B C46B 118.8(6) . . ? C43B C42B C41B 117.8(7) . . ? C43B C42B C61B 121.7(7) . . ? C41B C42B C61B 120.5(6) . . ? C44B C43B C42B 124.0(8) . . ? C44B C43B H43B 118.0 . . ? C42B C43B H43B 118.0 . . ? C43B C44B C45B 117.2(7) . . ? C43B C44B C65B 122.2(8) . . ? C45B C44B C65B 120.6(8) . . ? C44B C45B C46B 122.5(8) . . ? C44B C45B H45B 118.8 . . ? C46B C45B H45B 118.8 . . ? C45B C46B C41B 119.7(7) . . ? C45B C46B C48B 120.0(7) . . ? C41B C46B C48B 120.1(6) . . ? C40B C47B N2B 114.4(6) . . ? C40B C47B H47C 108.7 . . ? N2B C47B H47C 108.7 . . ? C40B C47B H47D 108.7 . . ? N2B C47B H47D 108.7 . . ? H47C C47B H47D 107.6 . . ? C46B C48B N2B 115.1(6) . . ? C46B C48B H48C 108.5 . . ? N2B C48B H48C 108.5 . . ? C46B C48B H48D 108.5 . . ? N2B C48B H48D 108.5 . . ? H48C C48B H48D 107.5 . . ? N2B C49B C50B 116.7(8) . . ? N2B C49B H49C 108.1 . . ? C50B C49B H49C 108.1 . . ? N2B C49B H49D 108.1 . . ? C50B C49B H49D 108.1 . . ? H49C C49B H49D 107.3 . . ? C51B C50B C51D 23(2) . . ? C51B C50B C49B 114(2) . . ? C51D C50B C49B 110(2) . . ? C51B C50B H50C 102(6) . . ? C51D C50B H50C 124(6) . . ? C49B C50B H50C 105(6) . . ? C51B C50B H50D 120(9) . . ? C51D C50B H50D 101(8) . . ? C49B C50B H50D 100(8) . . ? H50C C50B H50D 115(10) . . ? C50B C51B C52B 103(4) . . ? C50B C51B H51G 111.1 . . ? C52B C51B H51G 111.1 . . ? C50B C51B H51H 111.1 . . ? C52B C51B H51H 111.1 . . ? H51G C51B H51H 109.1 . . ? C50B C51D C52D 112(4) . . ? C50B C51D H51E 109.2 . . ? C52D C51D H51E 109.2 . . ? C50B C51D H51F 109.2 . . ? C52D C51D H51F 109.2 . . ? H51E C51D H51F 107.9 . . ? C51B C52B H52G 109.5 . . ? C51B C52B H52H 109.5 . . ? H52G C52B H52H 109.5 . . ? C51B C52B H52I 109.5 . . ? H52G C52B H52I 109.5 . . ? H52H C52B H52I 109.5 . . ? C51D C52D H52J 109.5 . . ? C51D C52D H52K 109.5 . . ? H52J C52D H52K 109.5 . . ? C51D C52D H52L 109.5 . . ? H52J C52D H52L 109.5 . . ? H52K C52D H52L 109.5 . . ? C56B C53B C36B 115.0(7) . . ? C56B C53B C55B 109.9(7) . . ? C36B C53B C55B 107.3(8) . . ? C56B C53B C54B 104.6(8) . . ? C36B C53B C54B 110.1(8) . . ? C55B C53B C54B 109.9(8) . . ? C53B C54B H54D 109.5 . . ? C53B C54B H54E 109.5 . . ? H54D C54B H54E 109.5 . . ? C53B C54B H54F 109.5 . . ? H54D C54B H54F 109.5 . . ? H54E C54B H54F 109.5 . . ? C53B C55B H55D 109.5 . . ? C53B C55B H55E 109.5 . . ? H55D C55B H55E 109.5 . . ? C53B C55B H55F 109.5 . . ? H55D C55B H55F 109.5 . . ? H55E C55B H55F 109.5 . . ? C53B C56B H56D 109.5 . . ? C53B C56B H56E 109.5 . . ? H56D C56B H56E 109.5 . . ? C53B C56B H56F 109.5 . . ? H56D C56B H56F 109.5 . . ? H56E C56B H56F 109.5 . . ? C60B C57B C58B 121(2) . . ? C60B C57B C58D 67(2) . . ? C58B C57B C58D 61.4(18) . . ? C60B C57B C59D 135(3) . . ? C58B C57B C59D 61(2) . . ? C58D C57B C59D 120(3) . . ? C60B C57B C60D 50.7(17) . . ? C58B C57B C60D 135.2(19) . . ? C58D C57B C60D 114(2) . . ? C59D C57B C60D 95(2) . . ? C60B C57B C59B 96.3(19) . . ? C58B C57B C59B 106.1(18) . . ? C58D C57B C59B 142(2) . . ? C59D C57B C59B 49(2) . . ? C60D C57B C59B 47.1(15) . . ? C60B C57B C38B 109.9(17) . . ? C58B C57B C38B 112.6(14) . . ? C58D C57B C38B 108.4(18) . . ? C59D C57B C38B 108(2) . . ? C60D C57B C38B 110.8(16) . . ? C59B C57B C38B 109.7(15) . . ? C57B C58B H58G 109.5 . . ? C57B C58B H58H 109.5 . . ? H58G C58B H58H 109.5 . . ? C57B C58B H58I 109.5 . . ? H58G C58B H58I 109.5 . . ? H58H C58B H58I 109.5 . . ? C57B C58D H58J 109.5 . . ? C57B C58D H58K 109.5 . . ? H58J C58D H58K 109.5 . . ? C57B C58D H58L 109.5 . . ? H58J C58D H58L 109.5 . . ? H58K C58D H58L 109.5 . . ? C57B C59B H59G 109.5 . . ? C57B C59B H59H 109.5 . . ? H59G C59B H59H 109.5 . . ? C57B C59B H59I 109.5 . . ? H59G C59B H59I 109.5 . . ? H59H C59B H59I 109.5 . . ? C57B C59D H59J 109.5 . . ? C57B C59D H59K 109.5 . . ? H59J C59D H59K 109.5 . . ? C57B C59D H59L 109.5 . . ? H59J C59D H59L 109.5 . . ? H59K C59D H59L 109.5 . . ? C57B C60B H60G 109.5 . . ? C57B C60B H60H 109.5 . . ? H60G C60B H60H 109.5 . . ? C57B C60B H60I 109.5 . . ? H60G C60B H60I 109.5 . . ? H60H C60B H60I 109.5 . . ? C57B C60D H60J 109.5 . . ? C57B C60D H60K 109.5 . . ? H60J C60D H60K 109.5 . . ? C57B C60D H60L 109.5 . . ? H60J C60D H60L 109.5 . . ? H60K C60D H60L 109.5 . . ? C42B C61B C62B 112.4(7) . . ? C42B C61B C64B 109.8(7) . . ? C62B C61B C64B 107.2(8) . . ? C42B C61B C63B 109.9(7) . . ? C62B C61B C63B 107.1(8) . . ? C64B C61B C63B 110.3(7) . . ? C61B C62B H62D 109.5 . . ? C61B C62B H62E 109.5 . . ? H62D C62B H62E 109.5 . . ? C61B C62B H62F 109.5 . . ? H62D C62B H62F 109.5 . . ? H62E C62B H62F 109.5 . . ? C61B C63B H63D 109.5 . . ? C61B C63B H63E 109.5 . . ? H63D C63B H63E 109.5 . . ? C61B C63B H63F 109.5 . . ? H63D C63B H63F 109.5 . . ? H63E C63B H63F 109.5 . . ? C61B C64B H64D 109.5 . . ? C61B C64B H64E 109.5 . . ? H64D C64B H64E 109.5 . . ? C61B C64B H64F 109.5 . . ? H64D C64B H64F 109.5 . . ? H64E C64B H64F 109.5 . . ? C66B C65B C67B 110.2(10) . . ? C66B C65B C68B 108.4(10) . . ? C67B C65B C68B 107.3(9) . . ? C66B C65B C44B 109.3(9) . . ? C67B C65B C44B 109.7(8) . . ? C68B C65B C44B 111.9(8) . . ? C65B C66B H66G 109.5 . . ? C65B C66B H66H 109.5 . . ? H66G C66B H66H 109.5 . . ? C65B C66B H66I 109.5 . . ? H66G C66B H66I 109.5 . . ? H66H C66B H66I 109.5 . . ? C65B C67B H67G 109.5 . . ? C65B C67B H67H 109.5 . . ? H67G C67B H67H 109.5 . . ? C65B C67B H67I 109.5 . . ? H67G C67B H67I 109.5 . . ? H67H C67B H67I 109.5 . . ? C65B C68B H68G 109.5 . . ? C65B C68B H68H 109.5 . . ? H68G C68B H68H 109.5 . . ? C65B C68B H68I 109.5 . . ? H68G C68B H68I 109.5 . . ? H68H C68B H68I 109.5 . . ? C70 C69 C74 122(3) . . ? C70 C69 C75 127(3) . . ? C74 C69 C75 111(3) . . ? C69 C70 C71 118(3) . . ? C69 C70 H70 120.9 . . ? C71 C70 H70 120.9 . . ? C70 C71 C72 124(3) . . ? C70 C71 H71 118.0 . . ? C72 C71 H71 118.0 . . ? C73 C72 C71 112(3) . . ? C73 C72 H72 123.8 . . ? C71 C72 H72 123.8 . . ? C74 C73 C72 126(2) . . ? C74 C73 H73 116.9 . . ? C72 C73 H73 116.9 . . ? C73 C74 C69 116(2) . . ? C73 C74 H74 122.0 . . ? C69 C74 H74 122.0 . . ? C69 C75 H75A 109.5 . . ? C69 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C69 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? O5 C76 C77 104(2) . . ? O5 C76 H76A 110.9 . . ? C77 C76 H76A 110.9 . . ? O5 C76 H76B 110.9 . . ? C77 C76 H76B 110.9 . . ? H76A C76 H76B 109.0 . . ? C76 C77 C78 107(2) . . ? C76 C77 H77A 110.3 . . ? C78 C77 H77A 110.3 . . ? C76 C77 H77B 110.3 . . ? C78 C77 H77B 110.3 . . ? H77A C77 H77B 108.6 . . ? C79 C78 C77 110(2) . . ? C79 C78 H78A 109.7 . . ? C77 C78 H78A 109.7 . . ? C79 C78 H78B 109.7 . . ? C77 C78 H78B 109.7 . . ? H78A C78 H78B 108.2 . . ? O5 C79 C78 105(2) . . ? O5 C79 H79A 110.8 . . ? C78 C79 H79A 110.8 . . ? O5 C79 H79B 110.8 . . ? C78 C79 H79B 110.8 . . ? H79A C79 H79B 108.9 . . ? C82 C80 C81 122(3) 2_656 . ? C82 C80 C83 117(3) 2_656 . ? C81 C80 C83 117(4) . . ? C80 C81 C82 131(2) . . ? C80 C81 H81 114.4 . . ? C82 C81 H81 114.4 . . ? C80 C82 C81 105(3) 2_656 . ? C80 C82 H82 127.4 2_656 . ? C81 C82 H82 127.4 . . ? C80 C83 H83A 109.5 . . ? C80 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C80 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? 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 O1A Sm1 Sm2A O2A -135.1(2) . . . . ? O3B Sm1 Sm2A O2A 45.9(3) . . . . ? O1B Sm1 Sm2A O2A -132.9(2) . . . . ? O3A Sm1 Sm2A O2A 46.4(2) . . . . ? Sm2B Sm1 Sm2A O2A -103.9(6) . . . . ? O1A Sm1 Sm2A O4A 43.0(2) . . . . ? O3B Sm1 Sm2A O4A -136.0(3) . . . . ? O1B Sm1 Sm2A O4A 45.2(2) . . . . ? O3A Sm1 Sm2A O4A -135.5(2) . . . . ? Sm2B Sm1 Sm2A O4A 74.2(6) . . . . ? O3B Sm1 Sm2A O1A -179.0(3) . . . . ? O1B Sm1 Sm2A O1A 2.1(2) . . . . ? O3A Sm1 Sm2A O1A -178.5(2) . . . . ? Sm2B Sm1 Sm2A O1A 31.1(6) . . . . ? O1A Sm1 Sm2A O3A 178.5(2) . . . . ? O3B Sm1 Sm2A O3A -0.5(3) . . . . ? O1B Sm1 Sm2A O3A -179.4(2) . . . . ? Sm2B Sm1 Sm2A O3A -150.3(6) . . . . ? O1A Sm1 Sm2A N1A -63.5(2) . . . . ? O3B Sm1 Sm2A N1A 117.5(2) . . . . ? O1B Sm1 Sm2A N1A -61.3(2) . . . . ? O3A Sm1 Sm2A N1A 118.0(2) . . . . ? Sm2B Sm1 Sm2A N1A -32.3(6) . . . . ? O1A Sm1 Sm2A N2A 117.7(2) . . . . ? O3B Sm1 Sm2A N2A -61.4(2) . . . . ? O1B Sm1 Sm2A N2A 119.8(2) . . . . ? O3A Sm1 Sm2A N2A -60.8(2) . . . . ? Sm2B Sm1 Sm2A N2A 148.8(6) . . . . ? O1A Sm1 Sm2B O2B -135.6(2) . . . . ? O3B Sm1 Sm2B O2B 43.4(3) . . . . ? O1B Sm1 Sm2B O2B -135.8(2) . . . . ? O3A Sm1 Sm2B O2B 44.9(2) . . . . ? Sm2A Sm1 Sm2B O2B -165.8(6) . . . . ? O1A Sm1 Sm2B O4B 45.0(2) . . . . ? O3B Sm1 Sm2B O4B -136.0(2) . . . . ? O1B Sm1 Sm2B O4B 44.8(2) . . . . ? O3A Sm1 Sm2B O4B -134.5(2) . . . . ? Sm2A Sm1 Sm2B O4B 14.9(6) . . . . ? O1A Sm1 Sm2B O3B -179.0(3) . . . . ? O1B Sm1 Sm2B O3B -179.2(3) . . . . ? O3A Sm1 Sm2B O3B 1.4(3) . . . . ? Sm2A Sm1 Sm2B O3B 150.8(6) . . . . ? O1A Sm1 Sm2B O1B 0.2(2) . . . . ? O3B Sm1 Sm2B O1B 179.2(3) . . . . ? O3A Sm1 Sm2B O1B -179.3(3) . . . . ? Sm2A Sm1 Sm2B O1B -29.9(6) . . . . ? O1A Sm1 Sm2B N1B -61.5(2) . . . . ? O3B Sm1 Sm2B N1B 117.5(2) . . . . ? O1B Sm1 Sm2B N1B -61.7(2) . . . . ? O3A Sm1 Sm2B N1B 119.0(2) . . . . ? Sm2A Sm1 Sm2B N1B -91.7(6) . . . . ? O1A Sm1 Sm2B N2B 118.5(2) . . . . ? O3B Sm1 Sm2B N2B -62.5(3) . . . . ? O1B Sm1 Sm2B N2B 118.2(2) . . . . ? O3A Sm1 Sm2B N2B -61.1(2) . . . . ? Sm2A Sm1 Sm2B N2B 88.3(6) . . . . ? O2A Sm2A O1A C1A -93.4(5) . . . . ? O4A Sm2A O1A C1A 42.8(4) . . . . ? O3A Sm2A O1A C1A -172.0(4) . . . . ? N1A Sm2A O1A C1A -57.5(4) . . . . ? N2A Sm2A O1A C1A 119.2(4) . . . . ? Sm1 Sm2A O1A C1A -171.0(5) . . . . ? O2A Sm2A O1A Sm1 77.7(3) . . . . ? O4A Sm2A O1A Sm1 -146.13(18) . . . . ? O3A Sm2A O1A Sm1 -0.94(16) . . . . ? N1A Sm2A O1A Sm1 113.6(2) . . . . ? N2A Sm2A O1A Sm1 -69.8(2) . . . . ? O3B Sm1 O1A C1A -31(6) . . . . ? O1B Sm1 O1A C1A -9.9(6) . . . . ? O3A Sm1 O1A C1A 169.7(6) . . . . ? Sm2A Sm1 O1A C1A 168.8(6) . . . . ? Sm2B Sm1 O1A C1A -10.0(6) . . . . ? O3B Sm1 O1A Sm2A 160(5) . . . . ? O1B Sm1 O1A Sm2A -178.68(14) . . . . ? O3A Sm1 O1A Sm2A 0.91(15) . . . . ? Sm2B Sm1 O1A Sm2A -178.82(2) . . . . ? O4A Sm2A O2A C7A -102.1(8) . . . . ? O1A Sm2A O2A C7A 31.7(10) . . . . ? O3A Sm2A O2A C7A 102.3(8) . . . . ? N1A Sm2A O2A C7A -4.9(8) . . . . ? N2A Sm2A O2A C7A -179.3(8) . . . . ? Sm1 Sm2A O2A C7A 76.3(8) . . . . ? O2A Sm2A O3A C35A 48.8(5) . . . . ? O4A Sm2A O3A C35A -88.4(5) . . . . ? O1A Sm2A O3A C35A -166.6(5) . . . . ? N1A Sm2A O3A C35A 124.1(5) . . . . ? N2A Sm2A O3A C35A -50.6(5) . . . . ? Sm1 Sm2A O3A C35A -167.5(6) . . . . ? O2A Sm2A O3A Sm1 -143.68(18) . . . . ? O4A Sm2A O3A Sm1 79.1(3) . . . . ? O1A Sm2A O3A Sm1 0.91(15) . . . . ? N1A Sm2A O3A Sm1 -68.5(2) . . . . ? N2A Sm2A O3A Sm1 116.9(2) . . . . ? O1A Sm1 O3A C35A 164.9(6) . . . . ? O3B Sm1 O3A C35A -14.5(6) . . . . ? O1B Sm1 O3A C35A -172(41) . . . . ? Sm2A Sm1 O3A C35A 165.8(6) . . . . ? Sm2B Sm1 O3A C35A -15.4(6) . . . . ? O1A Sm1 O3A Sm2A -0.90(15) . . . . ? O3B Sm1 O3A Sm2A 179.69(15) . . . . ? O1B Sm1 O3A Sm2A 22(9) . . . . ? Sm2B Sm1 O3A Sm2A 178.82(2) . . . . ? O2A Sm2A O4A C41A -82.9(8) . . . . ? O1A Sm2A O4A C41A 122.4(7) . . . . ? O3A Sm2A O4A C41A 52.1(9) . . . . ? N1A Sm2A O4A C41A -159.2(7) . . . . ? N2A Sm2A O4A C41A 13.8(7) . . . . ? Sm1 Sm2A O4A C41A 98.8(7) . . . . ? O2B Sm2B O1B C1B -90.1(5) . . . . ? O4B Sm2B O1B C1B 46.0(4) . . . . ? O3B Sm2B O1B C1B -169.4(5) . . . . ? N1B Sm2B O1B C1B -53.8(4) . . . . ? N2B Sm2B O1B C1B 121.3(4) . . . . ? Sm1 Sm2B O1B C1B -169.9(5) . . . . ? O2B Sm2B O1B Sm1 79.7(3) . . . . ? O4B Sm2B O1B Sm1 -144.18(18) . . . . ? O3B Sm2B O1B Sm1 0.46(16) . . . . ? N1B Sm2B O1B Sm1 116.1(2) . . . . ? N2B Sm2B O1B Sm1 -68.8(2) . . . . ? O1A Sm1 O1B C1B -12.0(6) . . . . ? O3B Sm1 O1B C1B 167.4(6) . . . . ? O3A Sm1 O1B C1B -35(9) . . . . ? Sm2A Sm1 O1B C1B -13.3(6) . . . . ? Sm2B Sm1 O1B C1B 167.8(6) . . . . ? O1A Sm1 O1B Sm2B -179.86(14) . . . . ? O3B Sm1 O1B Sm2B -0.45(15) . . . . ? O3A Sm1 O1B Sm2B 157(9) . . . . ? Sm2A Sm1 O1B Sm2B 178.87(2) . . . . ? O4B Sm2B O2B C7B -89.8(9) . . . . ? O3B Sm2B O2B C7B 114.6(8) . . . . ? O1B Sm2B O2B C7B 43.8(10) . . . . ? N1B Sm2B O2B C7B 6.8(8) . . . . ? N2B Sm2B O2B C7B -166.1(8) . . . . ? Sm1 Sm2B O2B C7B 90.8(8) . . . . ? O2B Sm2B O3B C35B 43.1(5) . . . . ? O4B Sm2B O3B C35B -95.5(6) . . . . ? O1B Sm2B O3B C35B -170.9(5) . . . . ? N1B Sm2B O3B C35B 119.9(5) . . . . ? N2B Sm2B O3B C35B -55.2(5) . . . . ? Sm1 Sm2B O3B C35B -170.4(6) . . . . ? O2B Sm2B O3B Sm1 -146.5(2) . . . . ? O4B Sm2B O3B Sm1 74.9(3) . . . . ? O1B Sm2B O3B Sm1 -0.47(16) . . . . ? N1B Sm2B O3B Sm1 -69.7(2) . . . . ? N2B Sm2B O3B Sm1 115.2(2) . . . . ? O1A Sm1 O3B C35B -170(5) . . . . ? O1B Sm1 O3B C35B 169.1(6) . . . . ? O3A Sm1 O3B C35B -10.5(6) . . . . ? Sm2A Sm1 O3B C35B -10.1(7) . . . . ? Sm2B Sm1 O3B C35B 168.7(7) . . . . ? O1A Sm1 O3B Sm2B 22(6) . . . . ? O1B Sm1 O3B Sm2B 0.46(16) . . . . ? O3A Sm1 O3B Sm2B -179.14(15) . . . . ? Sm2A Sm1 O3B Sm2B -178.81(3) . . . . ? O2B Sm2B O4B C41B -89.3(8) . . . . ? O3B Sm2B O4B C41B 47.4(10) . . . . ? O1B Sm2B O4B C41B 114.9(8) . . . . ? N1B Sm2B O4B C41B -166.4(8) . . . . ? N2B Sm2B O4B C41B 6.3(8) . . . . ? Sm1 Sm2B O4B C41B 90.2(9) . . . . ? O2A Sm2A N1A C14A 42.9(4) . . . . ? O4A Sm2A N1A C14A 148.6(4) . . . . ? O1A Sm2A N1A C14A -116.1(4) . . . . ? O3A Sm2A N1A C14A -49.9(4) . . . . ? N2A Sm2A N1A C14A 87.8(14) . . . . ? Sm1 Sm2A N1A C14A -83.9(4) . . . . ? O2A Sm2A N1A C13A 157.0(5) . . . . ? O4A Sm2A N1A C13A -97.3(4) . . . . ? O1A Sm2A N1A C13A -2.0(4) . . . . ? O3A Sm2A N1A C13A 64.2(5) . . . . ? N2A Sm2A N1A C13A -158.1(12) . . . . ? Sm1 Sm2A N1A C13A 30.3(4) . . . . ? O2A Sm2A N1A C15A -78.7(4) . . . . ? O4A Sm2A N1A C15A 27.0(5) . . . . ? O1A Sm2A N1A C15A 122.3(5) . . . . ? O3A Sm2A N1A C15A -171.5(4) . . . . ? N2A Sm2A N1A C15A -33.8(15) . . . . ? Sm1 Sm2A N1A C15A 154.5(4) . . . . ? O2A Sm2A N2A C47A -104.2(4) . . . . ? O4A Sm2A N2A C47A 149.8(5) . . . . ? O1A Sm2A N2A C47A 57.1(5) . . . . ? O3A Sm2A N2A C47A -8.7(4) . . . . ? N1A Sm2A N2A C47A -147.8(12) . . . . ? Sm1 Sm2A N2A C47A 23.8(4) . . . . ? O2A Sm2A N2A C49A 19.0(5) . . . . ? O4A Sm2A N2A C49A -87.0(5) . . . . ? O1A Sm2A N2A C49A -179.7(5) . . . . ? O3A Sm2A N2A C49A 114.5(5) . . . . ? N1A Sm2A N2A C49A -24.6(16) . . . . ? Sm1 Sm2A N2A C49A 147.0(5) . . . . ? O2A Sm2A N2A C48A 140.4(4) . . . . ? O4A Sm2A N2A C48A 34.4(4) . . . . ? O1A Sm2A N2A C48A -58.3(5) . . . . ? O3A Sm2A N2A C48A -124.1(4) . . . . ? N1A Sm2A N2A C48A 96.8(14) . . . . ? Sm1 Sm2A N2A C48A -91.6(4) . . . . ? O2B Sm2B N1B C14B 37.2(4) . . . . ? O4B Sm2B N1B C14B 143.1(4) . . . . ? O3B Sm2B N1B C14B -57.4(4) . . . . ? O1B Sm2B N1B C14B -122.6(4) . . . . ? N2B Sm2B N1B C14B 89.7(13) . . . . ? Sm1 Sm2B N1B C14B -90.5(4) . . . . ? O2B Sm2B N1B C13B 152.7(4) . . . . ? O4B Sm2B N1B C13B -101.4(4) . . . . ? O3B Sm2B N1B C13B 58.0(4) . . . . ? O1B Sm2B N1B C13B -7.1(4) . . . . ? N2B Sm2B N1B C13B -154.8(12) . . . . ? Sm1 Sm2B N1B C13B 24.9(4) . . . . ? O2B Sm2B N1B C15B -83.8(4) . . . . ? O4B Sm2B N1B C15B 22.1(5) . . . . ? O3B Sm2B N1B C15B -178.4(4) . . . . ? O1B Sm2B N1B C15B 116.4(4) . . . . ? N2B Sm2B N1B C15B -31.3(15) . . . . ? Sm1 Sm2B N1B C15B 148.4(4) . . . . ? O2B Sm2B N2B C49B 20.6(6) . . . . ? O4B Sm2B N2B C49B -85.5(6) . . . . ? O3B Sm2B N2B C49B 118.1(6) . . . . ? O1B Sm2B N2B C49B -176.7(5) . . . . ? N1B Sm2B N2B C49B -30.4(16) . . . . ? Sm1 Sm2B N2B C49B 149.9(5) . . . . ? O2B Sm2B N2B C47B -101.8(5) . . . . ? O4B Sm2B N2B C47B 152.1(5) . . . . ? O3B Sm2B N2B C47B -4.3(5) . . . . ? O1B Sm2B N2B C47B 60.9(5) . . . . ? N1B Sm2B N2B C47B -152.8(11) . . . . ? Sm1 Sm2B N2B C47B 27.5(5) . . . . ? O2B Sm2B N2B C48B 143.5(4) . . . . ? O4B Sm2B N2B C48B 37.4(4) . . . . ? O3B Sm2B N2B C48B -119.0(4) . . . . ? O1B Sm2B N2B C48B -53.8(4) . . . . ? N1B Sm2B N2B C48B 92.5(13) . . . . ? Sm1 Sm2B N2B C48B -87.2(4) . . . . ? Sm2A O1A C1A C6A 68.0(6) . . . . ? Sm1 O1A C1A C6A -100.4(6) . . . . ? Sm2A O1A C1A C2A -112.8(6) . . . . ? Sm1 O1A C1A C2A 78.8(8) . . . . ? O1A C1A C2A C3A 178.0(6) . . . . ? C6A C1A C2A C3A -2.9(9) . . . . ? O1A C1A C2A C19A 1.1(10) . . . . ? C6A C1A C2A C19A -179.8(6) . . . . ? C1A C2A C3A C4A 2.1(12) . . . . ? C19A C2A C3A C4A 179.2(8) . . . . ? C2A C3A C4A C5A 0.0(13) . . . . ? C2A C3A C4A C23A 179.0(8) . . . . ? C3A C4A C5A C6A -1.3(12) . . . . ? C23A C4A C5A C6A 179.7(8) . . . . ? C4A C5A C6A C1A 0.4(11) . . . . ? C4A C5A C6A C13A 178.6(7) . . . . ? O1A C1A C6A C5A -179.0(6) . . . . ? C2A C1A C6A C5A 1.8(10) . . . . ? O1A C1A C6A C13A 2.8(9) . . . . ? C2A C1A C6A C13A -176.5(6) . . . . ? Sm2A O2A C7A C8A 164.5(6) . . . . ? Sm2A O2A C7A C12A -16.8(12) . . . . ? O2A C7A C8A C9A 178.4(7) . . . . ? C12A C7A C8A C9A -0.3(11) . . . . ? O2A C7A C8A C27A 0.5(11) . . . . ? C12A C7A C8A C27A -178.3(7) . . . . ? C7A C8A C9A C10A 0.9(12) . . . . ? C27A C8A C9A C10A 178.9(8) . . . . ? C8A C9A C10A C11A -0.3(13) . . . . ? C8A C9A C10A C31A 179.7(9) . . . . ? C9A C10A C11A C12A -1.0(13) . . . . ? C31A C10A C11A C12A 179.0(9) . . . . ? C10A C11A C12A C7A 1.6(13) . . . . ? C10A C11A C12A C14A -177.2(8) . . . . ? O2A C7A C12A C11A -179.7(7) . . . . ? C8A C7A C12A C11A -0.9(11) . . . . ? O2A C7A C12A C14A -0.9(11) . . . . ? C8A C7A C12A C14A 177.9(7) . . . . ? C14A N1A C13A C6A 170.6(6) . . . . ? C15A N1A C13A C6A -66.0(7) . . . . ? Sm2A N1A C13A C6A 57.2(7) . . . . ? C5A C6A C13A N1A 106.1(8) . . . . ? C1A C6A C13A N1A -75.7(8) . . . . ? C13A N1A C14A C12A 168.7(6) . . . . ? C15A N1A C14A C12A 45.2(8) . . . . ? Sm2A N1A C14A C12A -75.3(7) . . . . ? C11A C12A C14A N1A -126.6(8) . . . . ? C7A C12A C14A N1A 54.6(10) . . . . ? C14A N1A C15A C16A 57.3(9) . . . . ? C13A N1A C15A C16A -62.9(9) . . . . ? Sm2A N1A C15A C16A 174.6(6) . . . . ? N1A C15A C16A C17C -162.2(13) . . . . ? N1A C15A C16A C17A 171.9(13) . . . . ? C17C C16A C17A C18A 64(4) . . . . ? C15A C16A C17A C18A 172(2) . . . . ? C17A C16A C17C C18C -5(4) . . . . ? C15A C16A C17C C18C -86(3) . . . . ? C3A C2A C19A C21A 160.1(7) . . . . ? C1A C2A C19A C21A -23.1(10) . . . . ? C3A C2A C19A C20A -77.2(8) . . . . ? C1A C2A C19A C20A 99.7(8) . . . . ? C3A C2A C19A C22A 40.1(9) . . . . ? C1A C2A C19A C22A -143.0(7) . . . . ? C3A C4A C23A C26C 4(3) . . . . ? C5A C4A C23A C26C -177(2) . . . . ? C3A C4A C23A C25A 66.5(15) . . . . ? C5A C4A C23A C25A -114.5(13) . . . . ? C3A C4A C23A C24A -175.3(19) . . . . ? C5A C4A C23A C24A 4(2) . . . . ? C3A C4A C23A C25C 117.3(17) . . . . ? C5A C4A C23A C25C -63.7(18) . . . . ? C3A C4A C23A C24C -136.7(14) . . . . ? C5A C4A C23A C24C 42.3(16) . . . . ? C3A C4A C23A C26A -46.2(15) . . . . ? C5A C4A C23A C26A 132.8(13) . . . . ? C9A C8A C27A C30A 121.1(8) . . . . ? C7A C8A C27A C30A -61.0(9) . . . . ? C9A C8A C27A C29A -116.8(8) . . . . ? C7A C8A C27A C29A 61.0(9) . . . . ? C9A C8A C27A C28A 3.6(11) . . . . ? C7A C8A C27A C28A -178.5(8) . . . . ? C11A C10A C31A C32C 140.7(17) . . . . ? C9A C10A C31A C32C -39(2) . . . . ? C11A C10A C31A C33C -19(2) . . . . ? C9A C10A C31A C33C 161(2) . . . . ? C11A C10A C31A C34C -124(2) . . . . ? C9A C10A C31A C34C 56(2) . . . . ? C11A C10A C31A C34A -59.5(14) . . . . ? C9A C10A C31A C34A 120.5(12) . . . . ? C11A C10A C31A C32A -179.1(11) . . . . ? C9A C10A C31A C32A 0.9(15) . . . . ? C11A C10A C31A C33A 62.0(12) . . . . ? C9A C10A C31A C33A -118.0(11) . . . . ? Sm2A O3A C35A C40A 64.4(7) . . . . ? Sm1 O3A C35A C40A -100.1(7) . . . . ? Sm2A O3A C35A C36A -115.7(7) . . . . ? Sm1 O3A C35A C36A 79.8(8) . . . . ? O3A C35A C36A C37A 178.4(7) . . . . ? C40A C35A C36A C37A -1.8(11) . . . . ? O3A C35A C36A C53A 4.4(11) . . . . ? C40A C35A C36A C53A -175.8(7) . . . . ? C35A C36A C37A C38A 1.9(15) . . . . ? C53A C36A C37A C38A 176.2(10) . . . . ? C36A C37A C38A C39A -1.1(17) . . . . ? C36A C37A C38A C57A 179.6(11) . . . . ? C37A C38A C39A C40A 0.3(16) . . . . ? C57A C38A C39A C40A 179.6(10) . . . . ? C38A C39A C40A C35A -0.4(14) . . . . ? C38A C39A C40A C47A 179.9(9) . . . . ? O3A C35A C40A C39A -179.1(7) . . . . ? C36A C35A C40A C39A 1.1(12) . . . . ? O3A C35A C40A C47A 0.6(11) . . . . ? C36A C35A C40A C47A -179.2(7) . . . . ? Sm2A O4A C41A C42A 148.5(6) . . . . ? Sm2A O4A C41A C46A -31.2(11) . . . . ? O4A C41A C42A C43A -175.1(7) . . . . ? C46A C41A C42A C43A 4.6(10) . . . . ? O4A C41A C42A C61A 4.2(11) . . . . ? C46A C41A C42A C61A -176.0(7) . . . . ? C41A C42A C43A C44A -2.0(12) . . . . ? C61A C42A C43A C44A 178.6(8) . . . . ? C42A C43A C44A C45A -1.4(13) . . . . ? C42A C43A C44A C65A 177.4(8) . . . . ? C43A C44A C45A C46A 2.1(12) . . . . ? C65A C44A C45A C46A -176.7(8) . . . . ? C44A C45A C46A C41A 0.5(12) . . . . ? C44A C45A C46A C48A -177.6(7) . . . . ? O4A C41A C46A C45A 175.8(7) . . . . ? C42A C41A C46A C45A -4.0(11) . . . . ? O4A C41A C46A C48A -6.0(10) . . . . ? C42A C41A C46A C48A 174.2(6) . . . . ? C49A N2A C47A C40A -61.2(8) . . . . ? C48A N2A C47A C40A 175.6(6) . . . . ? Sm2A N2A C47A C40A 61.0(7) . . . . ? C39A C40A C47A N2A 106.9(8) . . . . ? C35A C40A C47A N2A -72.8(9) . . . . ? C47A N2A C48A C46A 169.2(6) . . . . ? C49A N2A C48A C46A 46.2(8) . . . . ? Sm2A N2A C48A C46A -74.0(6) . . . . ? C45A C46A C48A N2A -118.2(8) . . . . ? C41A C46A C48A N2A 63.6(9) . . . . ? C47A N2A C49A C50A -61.3(10) . . . . ? C48A N2A C49A C50A 59.2(10) . . . . ? Sm2A N2A C49A C50A 176.9(7) . . . . ? N2A C49A C50A C51A 176.8(13) . . . . ? N2A C49A C50A C51C -154.9(19) . . . . ? C49A C50A C51A C52A -174(2) . . . . ? C51C C50A C51A C52A 101(4) . . . . ? C51A C50A C51C C52C -70(4) . . . . ? C49A C50A C51C C52C -176(3) . . . . ? C37A C36A C53A C55A -84.3(10) . . . . ? C35A C36A C53A C55A 89.6(9) . . . . ? C37A C36A C53A C56A 152.7(8) . . . . ? C35A C36A C53A C56A -33.3(11) . . . . ? C37A C36A C53A C54A 35.2(11) . . . . ? C35A C36A C53A C54A -150.9(8) . . . . ? C37A C38A C57A C58A -178.3(17) . . . . ? C39A C38A C57A C58A 2(2) . . . . ? C37A C38A C57A C60C -130.0(19) . . . . ? C39A C38A C57A C60C 51(2) . . . . ? C37A C38A C57A C59C 0(2) . . . . ? C39A C38A C57A C59C -179.5(19) . . . . ? C37A C38A C57A C58C 127(2) . . . . ? C39A C38A C57A C58C -52(2) . . . . ? C37A C38A C57A C59A 53.9(19) . . . . ? C39A C38A C57A C59A -125.3(16) . . . . ? C37A C38A C57A C60A -54(2) . . . . ? C39A C38A C57A C60A 126.9(16) . . . . ? C43A C42A C61A C63A 113.8(8) . . . . ? C41A C42A C61A C63A -65.5(9) . . . . ? C43A C42A C61A C62A -4.8(11) . . . . ? C41A C42A C61A C62A 175.9(7) . . . . ? C43A C42A C61A C64A -125.2(8) . . . . ? C41A C42A C61A C64A 55.5(9) . . . . ? C43A C44A C65A C68A 2.4(15) . . . . ? C45A C44A C65A C68A -178.8(11) . . . . ? C43A C44A C65A C66A -118.1(12) . . . . ? C45A C44A C65A C66A 60.7(13) . . . . ? C43A C44A C65A C66C -59(2) . . . . ? C45A C44A C65A C66C 120(2) . . . . ? C43A C44A C65A C67C 150.7(17) . . . . ? C45A C44A C65A C67C -30.5(19) . . . . ? C43A C44A C65A C67A 118.1(13) . . . . ? C45A C44A C65A C67A -63.1(14) . . . . ? C43A C44A C65A C68C 50(2) . . . . ? C45A C44A C65A C68C -131.2(18) . . . . ? Sm2B O1B C1B C2B -113.5(6) . . . . ? Sm1 O1B C1B C2B 79.4(8) . . . . ? Sm2B O1B C1B C6B 66.6(6) . . . . ? Sm1 O1B C1B C6B -100.5(6) . . . . ? O1B C1B C2B C3B 177.8(6) . . . . ? C6B C1B C2B C3B -2.3(10) . . . . ? O1B C1B C2B C19B 2.8(11) . . . . ? C6B C1B C2B C19B -177.3(6) . . . . ? C1B C2B C3B C4B 2.2(12) . . . . ? C19B C2B C3B C4B 177.5(8) . . . . ? C2B C3B C4B C5B 0.0(13) . . . . ? C2B C3B C4B C23B 177.9(9) . . . . ? C3B C4B C5B C6B -1.9(12) . . . . ? C23B C4B C5B C6B -180.0(8) . . . . ? C4B C5B C6B C1B 1.7(11) . . . . ? C4B C5B C6B C13B -179.1(7) . . . . ? O1B C1B C6B C5B -179.6(6) . . . . ? C2B C1B C6B C5B 0.5(10) . . . . ? O1B C1B C6B C13B 1.2(9) . . . . ? C2B C1B C6B C13B -178.7(6) . . . . ? Sm2B O2B C7B C12B -25.1(13) . . . . ? Sm2B O2B C7B C8B 154.0(7) . . . . ? O2B C7B C8B C9B -175.4(8) . . . . ? C12B C7B C8B C9B 3.6(13) . . . . ? O2B C7B C8B C27B 2.4(13) . . . . ? C12B C7B C8B C27B -178.5(8) . . . . ? C7B C8B C9B C10B -1.3(16) . . . . ? C27B C8B C9B C10B -179.0(10) . . . . ? C8B C9B C10B C11B -2.2(17) . . . . ? C8B C9B C10B C31B 176.8(11) . . . . ? C9B C10B C11B C12B 3.3(15) . . . . ? C31B C10B C11B C12B -175.8(10) . . . . ? C10B C11B C12B C7B -0.9(13) . . . . ? C10B C11B C12B C14B -179.5(8) . . . . ? O2B C7B C12B C11B 176.5(7) . . . . ? C8B C7B C12B C11B -2.6(12) . . . . ? O2B C7B C12B C14B -4.9(11) . . . . ? C8B C7B C12B C14B 175.9(7) . . . . ? C5B C6B C13B N1B 105.4(7) . . . . ? C1B C6B C13B N1B -75.4(8) . . . . ? C14B N1B C13B C6B 175.7(6) . . . . ? C15B N1B C13B C6B -61.9(7) . . . . ? Sm2B N1B C13B C6B 61.1(6) . . . . ? C13B N1B C14B C12B 169.7(6) . . . . ? C15B N1B C14B C12B 46.9(8) . . . . ? Sm2B N1B C14B C12B -74.1(6) . . . . ? C11B C12B C14B N1B -120.9(8) . . . . ? C7B C12B C14B N1B 60.5(10) . . . . ? C14B N1B C15B C16B 58.9(8) . . . . ? C13B N1B C15B C16B -61.4(8) . . . . ? Sm2B N1B C15B C16B 177.0(5) . . . . ? N1B C15B C16B C17B -179.1(8) . . . . ? C15B C16B C17B C18B 176.2(10) . . . . ? C3B C2B C19B C21B -79.3(9) . . . . ? C1B C2B C19B C21B 95.6(9) . . . . ? C3B C2B C19B C22B 157.8(7) . . . . ? C1B C2B C19B C22B -27.3(10) . . . . ? C3B C2B C19B C20B 39.0(9) . . . . ? C1B C2B C19B C20B -146.0(7) . . . . ? C3B C4B C23B C25D -48(3) . . . . ? C5B C4B C23B C25D 130(3) . . . . ? C3B C4B C23B C26D 157.2(18) . . . . ? C5B C4B C23B C26D -25(2) . . . . ? C3B C4B C23B C24D 42(2) . . . . ? C5B C4B C23B C24D -140(2) . . . . ? C3B C4B C23B C26B -118.8(12) . . . . ? C5B C4B C23B C26B 59.1(13) . . . . ? C3B C4B C23B C24B 123.1(13) . . . . ? C5B C4B C23B C24B -59.0(14) . . . . ? C3B C4B C23B C25B 0.4(16) . . . . ? C5B C4B C23B C25B 178.3(12) . . . . ? C9B C8B C27B C28B 113.7(10) . . . . ? C7B C8B C27B C28B -64.0(11) . . . . ? C9B C8B C27B C30B -124.8(10) . . . . ? C7B C8B C27B C30B 57.5(12) . . . . ? C9B C8B C27B C29B -5.2(15) . . . . ? C7B C8B C27B C29B 177.0(10) . . . . ? C9B C10B C31B C32B -169.6(16) . . . . ? C11B C10B C31B C32B 9(2) . . . . ? C9B C10B C31B C33B 68(2) . . . . ? C11B C10B C31B C33B -112.8(19) . . . . ? C9B C10B C31B C34D -7(2) . . . . ? C11B C10B C31B C34D 172.2(18) . . . . ? C9B C10B C31B C33D 110.3(17) . . . . ? C11B C10B C31B C33D -70.8(18) . . . . ? C9B C10B C31B C32D -128.8(16) . . . . ? C11B C10B C31B C32D 50.2(18) . . . . ? C9B C10B C31B C34B -44.8(19) . . . . ? C11B C10B C31B C34B 134.2(14) . . . . ? Sm2B O3B C35B C36B -114.0(7) . . . . ? Sm1 O3B C35B C36B 77.9(9) . . . . ? Sm2B O3B C35B C40B 65.9(7) . . . . ? Sm1 O3B C35B C40B -102.2(7) . . . . ? O3B C35B C36B C37B 177.9(7) . . . . ? C40B C35B C36B C37B -2.0(11) . . . . ? O3B C35B C36B C53B 4.7(12) . . . . ? C40B C35B C36B C53B -175.2(7) . . . . ? C35B C36B C37B C38B 1.5(13) . . . . ? C53B C36B C37B C38B 175.2(9) . . . . ? C36B C37B C38B C39B 0.7(15) . . . . ? C36B C37B C38B C57B 179.6(10) . . . . ? C37B C38B C39B C40B -2.4(15) . . . . ? C57B C38B C39B C40B 178.6(9) . . . . ? C38B C39B C40B C35B 1.8(13) . . . . ? C38B C39B C40B C47B 178.9(8) . . . . ? O3B C35B C40B C39B -179.5(7) . . . . ? C36B C35B C40B C39B 0.5(12) . . . . ? O3B C35B C40B C47B 3.4(10) . . . . ? C36B C35B C40B C47B -176.6(7) . . . . ? Sm2B O4B C41B C42B 155.5(6) . . . . ? Sm2B O4B C41B C46B -23.9(13) . . . . ? O4B C41B C42B C43B -177.4(7) . . . . ? C46B C41B C42B C43B 2.0(12) . . . . ? O4B C41B C42B C61B 1.9(12) . . . . ? C46B C41B C42B C61B -178.7(7) . . . . ? C41B C42B C43B C44B -0.9(13) . . . . ? C61B C42B C43B C44B 179.8(8) . . . . ? C42B C43B C44B C45B -1.2(14) . . . . ? C42B C43B C44B C65B 179.4(8) . . . . ? C43B C44B C45B C46B 2.2(14) . . . . ? C65B C44B C45B C46B -178.3(9) . . . . ? C44B C45B C46B C41B -1.2(13) . . . . ? C44B C45B C46B C48B -175.9(8) . . . . ? O4B C41B C46B C45B 178.5(7) . . . . ? C42B C41B C46B C45B -1.0(12) . . . . ? O4B C41B C46B C48B -6.8(11) . . . . ? C42B C41B C46B C48B 173.7(7) . . . . ? C39B C40B C47B N2B 106.5(8) . . . . ? C35B C40B C47B N2B -76.4(9) . . . . ? C49B N2B C47B C40B -62.0(8) . . . . ? C48B N2B C47B C40B 173.6(6) . . . . ? Sm2B N2B C47B C40B 59.1(7) . . . . ? C45B C46B C48B N2B -124.6(8) . . . . ? C41B C46B C48B N2B 60.7(10) . . . . ? C49B N2B C48B C46B 47.5(8) . . . . ? C47B N2B C48B C46B 171.2(6) . . . . ? Sm2B N2B C48B C46B -73.5(6) . . . . ? C47B N2B C49B C50B -61.9(12) . . . . ? C48B N2B C49B C50B 59.1(12) . . . . ? Sm2B N2B C49B C50B 178.1(9) . . . . ? N2B C49B C50B C51B -164(2) . . . . ? N2B C49B C50B C51D 171(2) . . . . ? C51D C50B C51B C52B -4(8) . . . . ? C49B C50B C51B C52B -89(4) . . . . ? C51B C50B C51D C52D -24(8) . . . . ? C49B C50B C51D C52D 81(4) . . . . ? C35B C36B C53B C56B -29.8(12) . . . . ? C37B C36B C53B C56B 157.0(8) . . . . ? C35B C36B C53B C55B 92.7(10) . . . . ? C37B C36B C53B C55B -80.4(10) . . . . ? C35B C36B C53B C54B -147.6(9) . . . . ? C37B C36B C53B C54B 39.2(11) . . . . ? C39B C38B C57B C60B -153.3(19) . . . . ? C37B C38B C57B C60B 28(2) . . . . ? C39B C38B C57B C58B 69.3(18) . . . . ? C37B C38B C57B C58B -109.6(17) . . . . ? C39B C38B C57B C58D 135(2) . . . . ? C37B C38B C57B C58D -44(2) . . . . ? C39B C38B C57B C59D 3(3) . . . . ? C37B C38B C57B C59D -175(2) . . . . ? C39B C38B C57B C60D -99(2) . . . . ? C37B C38B C57B C60D 82(2) . . . . ? C39B C38B C57B C59B -49(2) . . . . ? C37B C38B C57B C59B 132.4(18) . . . . ? C43B C42B C61B C62B -3.1(12) . . . . ? C41B C42B C61B C62B 177.7(9) . . . . ? C43B C42B C61B C64B 116.2(9) . . . . ? C41B C42B C61B C64B -63.1(10) . . . . ? C43B C42B C61B C63B -122.3(8) . . . . ? C41B C42B C61B C63B 58.4(10) . . . . ? C43B C44B C65B C66B -117.3(12) . . . . ? C45B C44B C65B C66B 63.3(13) . . . . ? C43B C44B C65B C67B 121.8(10) . . . . ? C45B C44B C65B C67B -57.6(13) . . . . ? C43B C44B C65B C68B 2.7(14) . . . . ? C45B C44B C65B C68B -176.7(10) . . . . ? C74 C69 C70 C71 0.2(18) . . . . ? C75 C69 C70 C71 -171(2) . . . . ? C69 C70 C71 C72 2(2) . . . . ? C70 C71 C72 C73 -9(4) . . . . ? C71 C72 C73 C74 15(4) . . . . ? C72 C73 C74 C69 -14(4) . . . . ? C70 C69 C74 C73 5(3) . . . . ? C75 C69 C74 C73 177(2) . . . . ? C79 O5 C76 C77 0(3) . . . . ? O5 C76 C77 C78 -1(3) . . . . ? C76 C77 C78 C79 2(3) . . . . ? C76 O5 C79 C78 1(4) . . . . ? C77 C78 C79 O5 -1(4) . . . . ? C82 C80 C81 C82 -15(10) 2_656 . . . ? C83 C80 C81 C82 -174(4) . . . . ? C80 C81 C82 C80 13(9) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.363 _refine_diff_density_min -0.864 _refine_diff_density_rms 0.110 #===========================================================================END data_complex3 _database_code_depnum_ccdc_archive 'CCDC 643506' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H77 N O5 Yb, C4 H8 O' _chemical_formula_sum 'C50 H85 N O6 Yb' _chemical_formula_weight 969.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 10.6010(7) _cell_length_b 16.5373(11) _cell_length_c 29.2953(19) _cell_angle_alpha 90.00 _cell_angle_beta 98.501(2) _cell_angle_gamma 90.00 _cell_volume 5079.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 20832 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour orange-yellow _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 1.885 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3648 _exptl_absorpt_correction_T_max 0.7277 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53584 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11630 _reflns_number_gt 10531 _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. The THF molecule and the methyl groups of the tert-butyl groups of the ligands are disordered and the bond lengths of them are unreasonable, so that 16 restraints were used for the refinement of the THF molecule and the methyl groups. ; _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^)+(0.0398P)^2^+7.8704P] 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 11630 _refine_ls_number_parameters 532 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1007 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.146 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.365039(14) 0.560394(9) 0.323348(5) 0.03144(6) Uani 1 1 d . . . O1 O 0.2373(2) 0.54464(17) 0.25573(9) 0.0396(6) Uani 1 1 d . . . O2 O 0.5550(3) 0.54391(16) 0.37157(9) 0.0388(6) Uani 1 1 d . . . O3 O 0.3468(3) 0.70495(16) 0.33947(11) 0.0460(7) Uani 1 1 d . . . O4 O 0.1808(3) 0.5564(2) 0.36513(13) 0.0670(10) Uani 1 1 d . . . O5 O 0.3687(3) 0.41405(19) 0.33433(13) 0.0629(10) Uani 1 1 d . . . O6A O 0.6938(13) 0.6638(8) 0.0389(5) 0.158(4) Uiso 0.60 1 d PD . . O6B O 0.790(2) 0.7831(12) 0.0410(8) 0.176(8) Uiso 0.40 1 d PD . . N1 N 0.5113(3) 0.59818(17) 0.26372(10) 0.0293(6) Uani 1 1 d . . . C1 C 0.2391(3) 0.5533(2) 0.21133(13) 0.0327(7) Uani 1 1 d . . . C2 C 0.1251(3) 0.5619(2) 0.17871(13) 0.0341(8) Uani 1 1 d . . . C3 C 0.1355(4) 0.5681(2) 0.13212(14) 0.0385(8) Uani 1 1 d . . . H3 H 0.0595 0.5756 0.1109 0.046 Uiso 1 1 calc R . . C4 C 0.2506(4) 0.5640(2) 0.11466(14) 0.0404(9) Uani 1 1 d . . . C5 C 0.3607(4) 0.5568(2) 0.14643(13) 0.0367(8) Uani 1 1 d . . . H5 H 0.4409 0.5555 0.1357 0.044 Uiso 1 1 calc R . . C6 C 0.3571(3) 0.5516(2) 0.19389(13) 0.0310(7) Uani 1 1 d . . . C7 C 0.6414(3) 0.6013(2) 0.37326(12) 0.0310(7) Uani 1 1 d . . . C8 C 0.6991(3) 0.6378(2) 0.41546(13) 0.0337(8) Uani 1 1 d . . . C9 C 0.7737(3) 0.7059(2) 0.41279(13) 0.0360(8) Uani 1 1 d . . . H9 H 0.8076 0.7321 0.4408 0.043 Uiso 1 1 calc R . . C10 C 0.8022(3) 0.7386(2) 0.37165(13) 0.0341(8) Uani 1 1 d . . . C11 C 0.7591(3) 0.6962(2) 0.33151(13) 0.0327(7) Uani 1 1 d . . . H11 H 0.7833 0.7141 0.3032 0.039 Uiso 1 1 calc R . . C12 C 0.6812(3) 0.6280(2) 0.33147(13) 0.0305(7) Uani 1 1 d . . . C13 C 0.4797(4) 0.5377(2) 0.22606(13) 0.0344(8) Uani 1 1 d . . . H13A H 0.4756 0.4837 0.2403 0.041 Uiso 1 1 calc R . . H13B H 0.5505 0.5366 0.2075 0.041 Uiso 1 1 calc R . . C14 C 0.6413(3) 0.5800(2) 0.28852(13) 0.0325(7) Uani 1 1 d . . . H14A H 0.7037 0.5895 0.2671 0.039 Uiso 1 1 calc R . . H14B H 0.6451 0.5219 0.2967 0.039 Uiso 1 1 calc R . . C15 C 0.5012(3) 0.6823(2) 0.24655(13) 0.0319(7) Uani 1 1 d . . . H15A H 0.5184 0.7188 0.2735 0.038 Uiso 1 1 calc R . . H15B H 0.4117 0.6915 0.2323 0.038 Uiso 1 1 calc R . . C16 C 0.5874(4) 0.7080(2) 0.21178(15) 0.0417(9) Uani 1 1 d . . . H16A H 0.6741 0.6861 0.2214 0.050 Uiso 1 1 calc R . . H16B H 0.5542 0.6849 0.1812 0.050 Uiso 1 1 calc R . . C17 C 0.5945(5) 0.7991(3) 0.2079(2) 0.0606(13) Uani 1 1 d . . . H17A H 0.5100 0.8196 0.1937 0.073 Uiso 1 1 calc R . . H17B H 0.6133 0.8223 0.2393 0.073 Uiso 1 1 calc R . . C18 C 0.6933(7) 0.8286(4) 0.1799(3) 0.099(2) Uani 1 1 d . . . H18A H 0.7767 0.8062 0.1926 0.149 Uiso 1 1 calc R . . H18B H 0.6971 0.8878 0.1811 0.149 Uiso 1 1 calc R . . H18C H 0.6704 0.8109 0.1478 0.149 Uiso 1 1 calc R . . C19 C -0.0057(4) 0.5675(2) 0.19541(15) 0.0394(9) Uani 1 1 d . . . C20 C -0.1160(4) 0.5814(3) 0.15626(18) 0.0549(12) Uani 1 1 d . . . H20A H -0.1042 0.6333 0.1413 0.082 Uiso 1 1 calc R . . H20B H -0.1967 0.5822 0.1688 0.082 Uiso 1 1 calc R . . H20C H -0.1179 0.5377 0.1336 0.082 Uiso 1 1 calc R . . C21 C -0.0066(4) 0.6379(3) 0.22978(17) 0.0505(11) Uani 1 1 d . . . H21A H 0.0652 0.6320 0.2548 0.076 Uiso 1 1 calc R . . H21B H -0.0868 0.6372 0.2427 0.076 Uiso 1 1 calc R . . H21C H 0.0012 0.6893 0.2138 0.076 Uiso 1 1 calc R . . C22 C -0.0322(4) 0.4874(3) 0.21904(17) 0.0489(10) Uani 1 1 d . . . H22A H -0.0418 0.4437 0.1962 0.073 Uiso 1 1 calc R . . H22B H -0.1109 0.4924 0.2327 0.073 Uiso 1 1 calc R . . H22C H 0.0391 0.4750 0.2433 0.073 Uiso 1 1 calc R . . C23 C 0.2534(5) 0.5671(3) 0.06193(16) 0.0589(13) Uani 1 1 d D . . C24A C 0.1981(12) 0.6431(7) 0.0416(4) 0.087(3) Uiso 0.60 1 d PD . . H24A H 0.2476 0.6890 0.0558 0.131 Uiso 0.60 1 calc PR . . H24B H 0.1096 0.6478 0.0472 0.131 Uiso 0.60 1 calc PR . . H24C H 0.2005 0.6430 0.0083 0.131 Uiso 0.60 1 calc PR . . C24B C 0.1377(13) 0.6070(9) 0.0355(5) 0.062(3) Uiso 0.40 1 d P . . H24D H 0.1228 0.6589 0.0500 0.093 Uiso 0.40 1 calc PR . . H24E H 0.0632 0.5719 0.0358 0.093 Uiso 0.40 1 calc PR . . H24F H 0.1515 0.6161 0.0036 0.093 Uiso 0.40 1 calc PR . . C25A C 0.1769(9) 0.4942(6) 0.0397(3) 0.072(2) Uiso 0.60 1 d PD . . H25A H 0.0865 0.5012 0.0424 0.108 Uiso 0.60 1 calc PR . . H25B H 0.2087 0.4445 0.0555 0.108 Uiso 0.60 1 calc PR . . H25C H 0.1868 0.4907 0.0070 0.108 Uiso 0.60 1 calc PR . . C25B C 0.3382(16) 0.5044(10) 0.0461(6) 0.087(5) Uiso 0.40 1 d PD . . H25D H 0.3187 0.4986 0.0125 0.131 Uiso 0.40 1 calc PR . . H25E H 0.3241 0.4526 0.0608 0.131 Uiso 0.40 1 calc PR . . H25F H 0.4274 0.5207 0.0546 0.131 Uiso 0.40 1 calc PR . . C26A C 0.3847(10) 0.5508(6) 0.0494(4) 0.072(3) Uiso 0.60 1 d P . . H26A H 0.3782 0.5434 0.0160 0.108 Uiso 0.60 1 calc PR . . H26B H 0.4199 0.5017 0.0652 0.108 Uiso 0.60 1 calc PR . . H26C H 0.4409 0.5967 0.0590 0.108 Uiso 0.60 1 calc PR . . C26B C 0.3374(18) 0.6419(11) 0.0562(7) 0.108(6) Uiso 0.40 1 d PD . . H26D H 0.3414 0.6507 0.0234 0.162 Uiso 0.40 1 calc PR . . H26E H 0.4236 0.6328 0.0727 0.162 Uiso 0.40 1 calc PR . . H26F H 0.3004 0.6897 0.0690 0.162 Uiso 0.40 1 calc PR . . C27 C 0.6781(4) 0.6013(3) 0.46173(13) 0.0400(9) Uani 1 1 d . . . C28 C 0.7625(5) 0.6413(3) 0.50274(15) 0.0587(13) Uani 1 1 d . . . H28A H 0.7404 0.6987 0.5041 0.088 Uiso 1 1 calc R . . H28B H 0.8523 0.6359 0.4988 0.088 Uiso 1 1 calc R . . H28C H 0.7485 0.6146 0.5315 0.088 Uiso 1 1 calc R . . C29 C 0.7137(4) 0.5110(3) 0.46269(15) 0.0471(10) Uani 1 1 d . . . H29A H 0.6976 0.4871 0.4919 0.071 Uiso 1 1 calc R . . H29B H 0.8042 0.5052 0.4599 0.071 Uiso 1 1 calc R . . H29C H 0.6619 0.4832 0.4369 0.071 Uiso 1 1 calc R . . C30 C 0.5382(5) 0.6105(3) 0.46910(18) 0.0632(13) Uani 1 1 d . . . H30A H 0.5266 0.5860 0.4987 0.095 Uiso 1 1 calc R . . H30B H 0.4828 0.5833 0.4440 0.095 Uiso 1 1 calc R . . H30C H 0.5161 0.6680 0.4693 0.095 Uiso 1 1 calc R . . C31 C 0.8794(4) 0.8174(2) 0.37248(15) 0.0444(9) Uani 1 1 d . . . C32 C 0.8069(5) 0.8851(3) 0.3933(2) 0.0718(16) Uani 1 1 d . . . H32A H 0.8015 0.8725 0.4256 0.108 Uiso 1 1 calc R . . H32B H 0.7208 0.8897 0.3760 0.108 Uiso 1 1 calc R . . H32C H 0.8523 0.9364 0.3916 0.108 Uiso 1 1 calc R . . C33 C 0.9019(5) 0.8427(3) 0.32423(17) 0.0643(14) Uani 1 1 d . . . H33A H 0.8201 0.8554 0.3054 0.096 Uiso 1 1 calc R . . H33B H 0.9432 0.7984 0.3099 0.096 Uiso 1 1 calc R . . H33C H 0.9570 0.8906 0.3264 0.096 Uiso 1 1 calc R . . C34 C 1.0097(4) 0.8063(3) 0.40208(18) 0.0603(13) Uani 1 1 d . . . H34A H 1.0596 0.8561 0.4014 0.090 Uiso 1 1 calc R . . H34B H 1.0549 0.7614 0.3898 0.090 Uiso 1 1 calc R . . H34C H 0.9980 0.7944 0.4339 0.090 Uiso 1 1 calc R . . C35 C 0.2494(4) 0.7515(3) 0.31192(18) 0.0509(11) Uani 1 1 d . . . H35A H 0.1648 0.7400 0.3209 0.061 Uiso 1 1 calc R . . H35B H 0.2464 0.7386 0.2788 0.061 Uiso 1 1 calc R . . C36 C 0.2855(6) 0.8386(3) 0.3211(2) 0.0788(18) Uani 1 1 d . . . H36A H 0.3326 0.8600 0.2970 0.095 Uiso 1 1 calc R . . H36B H 0.2087 0.8723 0.3221 0.095 Uiso 1 1 calc R . . C37 C 0.3667(7) 0.8380(3) 0.3661(2) 0.0854(19) Uani 1 1 d . . . H37A H 0.4307 0.8819 0.3681 0.102 Uiso 1 1 calc R . . H37B H 0.3150 0.8448 0.3913 0.102 Uiso 1 1 calc R . . C38 C 0.4285(6) 0.7596(3) 0.3690(2) 0.0698(15) Uani 1 1 d . . . H38A H 0.5131 0.7635 0.3587 0.084 Uiso 1 1 calc R . . H38B H 0.4406 0.7398 0.4013 0.084 Uiso 1 1 calc R . . C39 C 0.1834(5) 0.5776(5) 0.41139(18) 0.0820(19) Uani 1 1 d . . . H39A H 0.2024 0.6360 0.4157 0.098 Uiso 1 1 calc R . . H39B H 0.2505 0.5466 0.4310 0.098 Uiso 1 1 calc R . . C40 C 0.0552(5) 0.5589(4) 0.42478(19) 0.0692(15) Uani 1 1 d . . . H40A H 0.0642 0.5272 0.4537 0.083 Uiso 1 1 calc R . . H40B H 0.0077 0.6093 0.4290 0.083 Uiso 1 1 calc R . . C41 C -0.0102(5) 0.5114(5) 0.3857(2) 0.0835(19) Uani 1 1 d D . . H41A H 0.0005 0.4527 0.3917 0.100 Uiso 1 1 calc R . . H41B H -0.1025 0.5241 0.3800 0.100 Uiso 1 1 calc R . . C42 C 0.0512(7) 0.5354(7) 0.3464(2) 0.142(4) Uani 1 1 d D . . H42A H 0.0500 0.4903 0.3241 0.170 Uiso 1 1 calc R . . H42B H 0.0068 0.5824 0.3305 0.170 Uiso 1 1 calc R . . C43 C 0.4568(6) 0.3715(4) 0.3669(3) 0.127(4) Uani 1 1 d D . . H43A H 0.4752 0.4034 0.3957 0.153 Uiso 1 1 calc R . . H43B H 0.5378 0.3637 0.3544 0.153 Uiso 1 1 calc R . . C44 C 0.4049(6) 0.2943(3) 0.3766(2) 0.0760(17) Uani 1 1 d D . . H44A H 0.3890 0.2915 0.4091 0.091 Uiso 1 1 calc R . . H44B H 0.4637 0.2500 0.3711 0.091 Uiso 1 1 calc R . . C45 C 0.2823(6) 0.2886(4) 0.3440(3) 0.104(3) Uani 1 1 d . . . H45A H 0.2767 0.2363 0.3273 0.124 Uiso 1 1 calc R . . H45B H 0.2083 0.2934 0.3608 0.124 Uiso 1 1 calc R . . C46 C 0.2851(8) 0.3555(4) 0.3120(3) 0.123(3) Uani 1 1 d . . . H46A H 0.3156 0.3368 0.2835 0.147 Uiso 1 1 calc R . . H46B H 0.1986 0.3786 0.3037 0.147 Uiso 1 1 calc R . . C47A C 0.627(4) 0.7222(14) 0.0616(13) 0.33(2) Uiso 0.60 1 d PD . . H47A H 0.6572 0.7218 0.0952 0.392 Uiso 0.60 1 calc PR . . H47B H 0.5342 0.7106 0.0564 0.392 Uiso 0.60 1 calc PR . . C47B C 0.662(2) 0.793(2) 0.0145(12) 0.172(13) Uiso 0.40 1 d PD . . H47C H 0.6594 0.7753 -0.0178 0.206 Uiso 0.40 1 calc PR . . H47D H 0.6334 0.8503 0.0149 0.206 Uiso 0.40 1 calc PR . . C48A C 0.6538(15) 0.8040(10) 0.0407(6) 0.117(5) Uiso 0.60 1 d PD . . H48A H 0.5734 0.8286 0.0255 0.141 Uiso 0.60 1 calc PR . . H48B H 0.6937 0.8411 0.0652 0.141 Uiso 0.60 1 calc PR . . C48B C 0.5858(16) 0.7401(11) 0.0403(6) 0.084(5) Uiso 0.40 1 d PD . . H48C H 0.5475 0.6934 0.0222 0.100 Uiso 0.40 1 calc PR . . H48D H 0.5211 0.7692 0.0552 0.100 Uiso 0.40 1 calc PR . . C49A C 0.743(2) 0.7893(12) 0.0057(7) 0.161(7) Uiso 0.60 1 d PD . . H49A H 0.6983 0.7953 -0.0262 0.193 Uiso 0.60 1 calc PR . . H49B H 0.8163 0.8274 0.0104 0.193 Uiso 0.60 1 calc PR . . C49B C 0.707(2) 0.720(2) 0.0730(10) 0.201(17) Uiso 0.40 1 d PD . . H49C H 0.7331 0.7667 0.0931 0.241 Uiso 0.40 1 calc PR . . H49D H 0.6902 0.6738 0.0930 0.241 Uiso 0.40 1 calc PR . . C50A C 0.7870(17) 0.7050(10) 0.0148(7) 0.147(6) Uiso 0.60 1 d PD . . H50A H 0.8721 0.7045 0.0340 0.177 Uiso 0.60 1 calc PR . . H50B H 0.7937 0.6771 -0.0146 0.177 Uiso 0.60 1 calc PR . . C50B C 0.812(2) 0.6977(13) 0.0468(9) 0.128(8) Uiso 0.40 1 d PD . . H50C H 0.8939 0.6817 0.0653 0.153 Uiso 0.40 1 calc PR . . H50D H 0.7882 0.6637 0.0190 0.153 Uiso 0.40 1 calc PR . . 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 0.03220(10) 0.02865(9) 0.03429(10) 0.00034(6) 0.00767(6) -0.00230(6) O1 0.0331(14) 0.0492(16) 0.0370(14) -0.0033(12) 0.0064(11) -0.0050(12) O2 0.0382(14) 0.0371(14) 0.0395(15) 0.0067(11) 0.0008(11) -0.0121(11) O3 0.0520(17) 0.0282(13) 0.0571(18) -0.0040(12) 0.0055(14) 0.0041(12) O4 0.057(2) 0.090(3) 0.060(2) -0.0179(19) 0.0310(17) -0.0168(18) O5 0.064(2) 0.0315(15) 0.083(2) 0.0115(16) -0.0211(18) -0.0121(14) N1 0.0266(14) 0.0270(14) 0.0340(15) -0.0040(12) 0.0030(11) 0.0011(11) C1 0.0332(18) 0.0258(16) 0.0386(19) -0.0043(14) 0.0040(15) -0.0023(14) C2 0.034(2) 0.0258(17) 0.041(2) 0.0005(15) 0.0014(16) -0.0035(14) C3 0.039(2) 0.0327(19) 0.041(2) 0.0011(16) -0.0026(16) 0.0027(15) C4 0.047(2) 0.040(2) 0.0333(19) 0.0023(16) 0.0043(16) 0.0048(17) C5 0.037(2) 0.0358(19) 0.038(2) -0.0017(15) 0.0076(16) 0.0025(15) C6 0.0306(18) 0.0268(16) 0.0354(18) -0.0034(14) 0.0038(14) 0.0002(13) C7 0.0281(17) 0.0277(16) 0.0367(19) 0.0043(14) 0.0028(14) -0.0005(13) C8 0.0296(18) 0.0357(18) 0.0357(19) 0.0028(15) 0.0046(14) -0.0019(14) C9 0.0338(19) 0.0329(18) 0.040(2) -0.0024(15) 0.0009(15) -0.0027(15) C10 0.0265(17) 0.0306(17) 0.044(2) 0.0047(15) 0.0004(14) -0.0027(14) C11 0.0272(17) 0.0356(18) 0.0356(18) 0.0071(15) 0.0057(14) -0.0017(14) C12 0.0235(16) 0.0296(17) 0.0384(19) 0.0026(14) 0.0048(13) 0.0019(13) C13 0.0361(19) 0.0295(17) 0.038(2) -0.0051(15) 0.0079(15) 0.0040(14) C14 0.0282(17) 0.0321(17) 0.0373(19) -0.0001(15) 0.0054(14) 0.0057(14) C15 0.0303(17) 0.0277(16) 0.0384(19) -0.0012(15) 0.0072(14) 0.0024(14) C16 0.043(2) 0.037(2) 0.046(2) 0.0053(17) 0.0121(17) 0.0015(16) C17 0.050(3) 0.042(2) 0.091(4) 0.024(2) 0.015(3) 0.000(2) C18 0.107(5) 0.076(4) 0.119(6) 0.045(4) 0.034(4) -0.023(4) C19 0.0283(19) 0.040(2) 0.049(2) -0.0019(17) 0.0033(16) -0.0006(15) C20 0.034(2) 0.064(3) 0.064(3) -0.001(2) -0.002(2) 0.002(2) C21 0.035(2) 0.048(2) 0.071(3) -0.012(2) 0.015(2) 0.0015(18) C22 0.039(2) 0.047(2) 0.061(3) 0.002(2) 0.0102(19) -0.0075(18) C23 0.065(3) 0.075(3) 0.037(2) 0.010(2) 0.008(2) 0.016(2) C27 0.038(2) 0.046(2) 0.036(2) 0.0047(17) 0.0067(16) -0.0073(17) C28 0.074(3) 0.070(3) 0.032(2) -0.001(2) 0.007(2) -0.020(3) C29 0.051(2) 0.049(2) 0.041(2) 0.0125(19) 0.0031(18) -0.0055(19) C30 0.055(3) 0.079(4) 0.060(3) 0.018(3) 0.025(2) 0.006(3) C31 0.040(2) 0.035(2) 0.055(2) 0.0083(18) -0.0025(18) -0.0095(17) C32 0.071(3) 0.033(2) 0.110(5) -0.009(3) 0.010(3) -0.010(2) C33 0.067(3) 0.056(3) 0.067(3) 0.022(2) 0.000(2) -0.031(2) C34 0.044(2) 0.062(3) 0.069(3) 0.012(2) -0.009(2) -0.022(2) C35 0.041(2) 0.046(2) 0.067(3) 0.001(2) 0.010(2) 0.0065(19) C36 0.077(4) 0.039(3) 0.113(5) 0.015(3) -0.010(3) 0.004(2) C37 0.117(5) 0.041(3) 0.094(5) -0.010(3) 0.001(4) -0.008(3) C38 0.079(4) 0.051(3) 0.072(4) -0.021(3) -0.013(3) 0.011(3) C39 0.056(3) 0.148(6) 0.044(3) -0.006(3) 0.014(2) -0.021(3) C40 0.051(3) 0.105(5) 0.054(3) 0.001(3) 0.018(2) -0.002(3) C41 0.053(3) 0.121(5) 0.081(4) -0.020(4) 0.022(3) -0.021(3) C42 0.084(5) 0.276(12) 0.073(5) -0.052(6) 0.038(4) -0.078(6) C43 0.079(4) 0.054(3) 0.222(9) 0.064(5) -0.067(5) -0.022(3) C44 0.083(4) 0.050(3) 0.088(4) 0.012(3) -0.011(3) -0.010(3) C45 0.080(4) 0.057(3) 0.157(7) 0.027(4) -0.037(4) -0.027(3) C46 0.161(7) 0.049(3) 0.128(6) 0.018(4) -0.077(5) -0.048(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 2.243(3) . ? Yb1 O2 2.299(3) . ? Yb1 O5 2.441(3) . ? Yb1 O3 2.450(3) . ? Yb1 O4 2.454(3) . ? Yb1 N1 2.578(3) . ? Yb1 C7 3.148(3) . ? O1 C1 1.312(5) . ? O2 C7 1.314(4) . ? O3 C35 1.436(5) . ? O3 C38 1.448(6) . ? O4 C39 1.396(6) . ? O4 C42 1.444(8) . ? O5 C46 1.407(6) . ? O5 C43 1.420(6) . ? O6A C47A 1.419(19) . ? O6A C50A 1.466(15) . ? O6B C50B 1.437(18) . ? O6B C47B 1.465(19) . ? N1 C15 1.478(4) . ? N1 C13 1.490(4) . ? N1 C14 1.490(4) . ? C1 C6 1.419(5) . ? C1 C2 1.433(5) . ? C2 C3 1.390(5) . ? C2 C19 1.539(5) . ? C3 C4 1.393(6) . ? C3 H3 0.9500 . ? C4 C5 1.386(6) . ? C4 C23 1.550(6) . ? C5 C6 1.399(5) . ? C5 H5 0.9500 . ? C6 C13 1.506(5) . ? C7 C12 1.423(5) . ? C7 C8 1.430(5) . ? C8 C9 1.385(5) . ? C8 C27 1.530(5) . ? C9 C10 1.394(5) . ? C9 H9 0.9500 . ? C10 C11 1.387(5) . ? C10 C31 1.537(5) . ? C11 C12 1.398(5) . ? C11 H11 0.9500 . ? C12 C14 1.496(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.526(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.514(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.503(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.530(6) . ? C19 C22 1.539(6) . ? C19 C21 1.540(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24A 1.474(10) . ? C23 C25B 1.491(14) . ? C23 C24B 1.503(14) . ? C23 C26A 1.515(11) . ? C23 C25A 1.543(10) . ? C23 C26B 1.548(15) . ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C24A H24C 0.9800 . ? C24B H24D 0.9800 . ? C24B H24E 0.9800 . ? C24B H24F 0.9800 . ? C25A H25A 0.9800 . ? C25A H25B 0.9800 . ? C25A H25C 0.9800 . ? C25B H25D 0.9800 . ? C25B H25E 0.9800 . ? C25B H25F 0.9800 . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C26B H26F 0.9800 . ? C27 C28 1.537(6) . ? C27 C30 1.537(6) . ? C27 C29 1.540(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.526(6) . ? C31 C34 1.530(6) . ? C31 C32 1.534(7) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.506(7) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.463(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.448(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.501(7) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.476(8) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.458(8) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.436(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.499(8) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.452(9) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47A C48A 1.528(19) . ? C47A H47A 0.9900 . ? C47A H47B 0.9900 . ? C47B C48B 1.478(19) . ? C47B H47C 0.9900 . ? C47B H47D 0.9900 . ? C48A C49A 1.517(16) . ? C48A H48A 0.9900 . ? C48A H48B 0.9900 . ? C48B C49B 1.52(2) . ? C48B H48C 0.9900 . ? C48B H48D 0.9900 . ? C49A C50A 1.480(16) . ? C49A H49A 0.9900 . ? C49A H49B 0.9900 . ? C49B C50B 1.488(19) . ? C49B H49C 0.9900 . ? C49B H49D 0.9900 . ? C50A H50A 0.9900 . ? C50A H50B 0.9900 . ? C50B H50C 0.9900 . ? C50B H50D 0.9900 . ? 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 152.69(10) . . ? O1 Yb1 O5 89.82(11) . . ? O2 Yb1 O5 78.82(10) . . ? O1 Yb1 O3 103.24(10) . . ? O2 Yb1 O3 94.83(10) . . ? O5 Yb1 O3 160.42(13) . . ? O1 Yb1 O4 90.93(11) . . ? O2 Yb1 O4 112.32(12) . . ? O5 Yb1 O4 84.59(13) . . ? O3 Yb1 O4 80.72(11) . . ? O1 Yb1 N1 77.00(9) . . ? O2 Yb1 N1 83.40(9) . . ? O5 Yb1 N1 109.29(11) . . ? O3 Yb1 N1 88.09(10) . . ? O4 Yb1 N1 161.28(12) . . ? O1 Yb1 C7 146.50(10) . . ? O2 Yb1 C7 21.48(9) . . ? O5 Yb1 C7 98.98(9) . . ? O3 Yb1 C7 78.21(9) . . ? O4 Yb1 C7 121.91(11) . . ? N1 Yb1 C7 69.58(9) . . ? C1 O1 Yb1 140.1(2) . . ? C7 O2 Yb1 118.7(2) . . ? C35 O3 C38 108.6(3) . . ? C35 O3 Yb1 119.0(2) . . ? C38 O3 Yb1 131.9(3) . . ? C39 O4 C42 108.0(4) . . ? C39 O4 Yb1 125.1(3) . . ? C42 O4 Yb1 126.9(3) . . ? C46 O5 C43 106.1(4) . . ? C46 O5 Yb1 128.7(3) . . ? C43 O5 Yb1 125.2(3) . . ? C47A O6A C50A 109.1(17) . . ? C50B O6B C47B 107(2) . . ? C15 N1 C13 112.5(3) . . ? C15 N1 C14 111.8(3) . . ? C13 N1 C14 108.5(3) . . ? C15 N1 Yb1 116.0(2) . . ? C13 N1 Yb1 104.3(2) . . ? C14 N1 Yb1 103.1(2) . . ? O1 C1 C6 119.9(3) . . ? O1 C1 C2 122.5(3) . . ? C6 C1 C2 117.6(3) . . ? C3 C2 C1 118.7(4) . . ? C3 C2 C19 120.9(3) . . ? C1 C2 C19 120.3(3) . . ? C2 C3 C4 123.9(4) . . ? C2 C3 H3 118.0 . . ? C4 C3 H3 118.0 . . ? C5 C4 C3 117.0(4) . . ? C5 C4 C23 122.3(4) . . ? C3 C4 C23 120.7(4) . . ? C4 C5 C6 121.9(4) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 120.8(3) . . ? C5 C6 C13 118.9(3) . . ? C1 C6 C13 120.2(3) . . ? O2 C7 C12 119.1(3) . . ? O2 C7 C8 123.0(3) . . ? C12 C7 C8 118.0(3) . . ? O2 C7 Yb1 39.83(16) . . ? C12 C7 Yb1 92.4(2) . . ? C8 C7 Yb1 137.9(2) . . ? C9 C8 C7 118.0(3) . . ? C9 C8 C27 122.0(3) . . ? C7 C8 C27 120.0(3) . . ? C8 C9 C10 124.3(3) . . ? C8 C9 H9 117.9 . . ? C10 C9 H9 117.9 . . ? C11 C10 C9 116.8(3) . . ? C11 C10 C31 123.3(3) . . ? C9 C10 C31 119.9(3) . . ? C10 C11 C12 121.9(3) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C11 C12 C7 120.0(3) . . ? C11 C12 C14 121.5(3) . . ? C7 C12 C14 118.4(3) . . ? N1 C13 C6 116.2(3) . . ? N1 C13 H13A 108.2 . . ? C6 C13 H13A 108.2 . . ? N1 C13 H13B 108.2 . . ? C6 C13 H13B 108.2 . . ? H13A C13 H13B 107.4 . . ? N1 C14 C12 115.4(3) . . ? N1 C14 H14A 108.4 . . ? C12 C14 H14A 108.4 . . ? N1 C14 H14B 108.4 . . ? C12 C14 H14B 108.4 . . ? H14A C14 H14B 107.5 . . ? N1 C15 C16 117.9(3) . . ? N1 C15 H15A 107.8 . . ? C16 C15 H15A 107.8 . . ? N1 C15 H15B 107.8 . . ? C16 C15 H15B 107.8 . . ? H15A C15 H15B 107.2 . . ? C17 C16 C15 111.6(3) . . ? C17 C16 H16A 109.3 . . ? C15 C16 H16A 109.3 . . ? C17 C16 H16B 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? C18 C17 C16 114.2(5) . . ? C18 C17 H17A 108.7 . . ? C16 C17 H17A 108.7 . . ? C18 C17 H17B 108.7 . . ? C16 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C2 113.3(4) . . ? C20 C19 C22 107.2(3) . . ? C2 C19 C22 108.9(3) . . ? C20 C19 C21 107.3(4) . . ? C2 C19 C21 110.3(3) . . ? C22 C19 C21 109.7(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 . . ? C24A C23 C25B 133.6(9) . . ? C24A C23 C24B 34.2(6) . . ? C25B C23 C24B 129.0(9) . . ? C24A C23 C26A 112.3(7) . . ? C25B C23 C26A 35.2(7) . . ? C24B C23 C26A 131.5(7) . . ? C24A C23 C25A 110.0(7) . . ? C25B C23 C25A 68.2(8) . . ? C24B C23 C25A 77.7(7) . . ? C26A C23 C25A 101.7(6) . . ? C24A C23 C26B 58.4(9) . . ? C25B C23 C26B 98.1(11) . . ? C24B C23 C26B 91.9(10) . . ? C26A C23 C26B 63.4(9) . . ? C25A C23 C26B 148.7(9) . . ? C24A C23 C4 111.5(6) . . ? C25B C23 C4 112.8(8) . . ? C24B C23 C4 113.2(6) . . ? C26A C23 C4 112.9(5) . . ? C25A C23 C4 108.0(5) . . ? C26B C23 C4 103.3(8) . . ? C23 C24A H24A 109.5 . . ? C23 C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C23 C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? C23 C24B H24D 109.5 . . ? C23 C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C23 C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C23 C25A H25A 109.5 . . ? C23 C25A H25B 109.5 . . ? H25A C25A H25B 109.5 . . ? C23 C25A H25C 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? C23 C25B H25D 109.5 . . ? C23 C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C23 C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C23 C26A H26A 109.5 . . ? C23 C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? C23 C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? C23 C26B H26D 109.5 . . ? C23 C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? C23 C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C8 C27 C28 112.3(3) . . ? C8 C27 C30 110.8(3) . . ? C28 C27 C30 108.1(4) . . ? C8 C27 C29 109.4(3) . . ? C28 C27 C29 106.8(4) . . ? C30 C27 C29 109.4(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C34 107.8(4) . . ? C33 C31 C32 108.9(4) . . ? C34 C31 C32 109.0(4) . . ? C33 C31 C10 111.9(4) . . ? C34 C31 C10 109.9(3) . . ? C32 C31 C10 109.2(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O3 C35 C36 105.6(4) . . ? O3 C35 H35A 110.6 . . ? C36 C35 H35A 110.6 . . ? O3 C35 H35B 110.6 . . ? C36 C35 H35B 110.6 . . ? H35A C35 H35B 108.7 . . ? C37 C36 C35 104.7(4) . . ? C37 C36 H36A 110.8 . . ? C35 C36 H36A 110.8 . . ? C37 C36 H36B 110.8 . . ? C35 C36 H36B 110.8 . . ? H36A C36 H36B 108.9 . . ? C38 C37 C36 105.1(5) . . ? C38 C37 H37A 110.7 . . ? C36 C37 H37A 110.7 . . ? C38 C37 H37B 110.7 . . ? C36 C37 H37B 110.7 . . ? H37A C37 H37B 108.8 . . ? O3 C38 C37 107.4(4) . . ? O3 C38 H38A 110.2 . . ? C37 C38 H38A 110.2 . . ? O3 C38 H38B 110.2 . . ? C37 C38 H38B 110.2 . . ? H38A C38 H38B 108.5 . . ? O4 C39 C40 108.3(4) . . ? O4 C39 H39A 110.0 . . ? C40 C39 H39A 110.0 . . ? O4 C39 H39B 110.0 . . ? C40 C39 H39B 110.0 . . ? H39A C39 H39B 108.4 . . ? C41 C40 C39 104.3(4) . . ? C41 C40 H40A 110.9 . . ? C39 C40 H40A 110.9 . . ? C41 C40 H40B 110.9 . . ? C39 C40 H40B 110.9 . . ? H40A C40 H40B 108.9 . . ? C42 C41 C40 104.7(5) . . ? C42 C41 H41A 110.8 . . ? C40 C41 H41A 110.8 . . ? C42 C41 H41B 110.8 . . ? C40 C41 H41B 110.8 . . ? H41A C41 H41B 108.9 . . ? O4 C42 C41 106.1(6) . . ? O4 C42 H42A 110.5 . . ? C41 C42 H42A 110.5 . . ? O4 C42 H42B 110.5 . . ? C41 C42 H42B 110.5 . . ? H42A C42 H42B 108.7 . . ? O5 C43 C44 109.9(5) . . ? O5 C43 H43A 109.7 . . ? C44 C43 H43A 109.7 . . ? O5 C43 H43B 109.7 . . ? C44 C43 H43B 109.7 . . ? H43A C43 H43B 108.2 . . ? C43 C44 C45 104.5(5) . . ? C43 C44 H44A 110.8 . . ? C45 C44 H44A 110.8 . . ? C43 C44 H44B 110.9 . . ? C45 C44 H44B 110.8 . . ? H44A C44 H44B 108.9 . . ? C46 C45 C44 105.4(5) . . ? C46 C45 H45A 110.7 . . ? C44 C45 H45A 110.7 . . ? C46 C45 H45B 110.7 . . ? C44 C45 H45B 110.7 . . ? H45A C45 H45B 108.8 . . ? O5 C46 C45 107.2(5) . . ? O5 C46 H46A 110.3 . . ? C45 C46 H46A 110.3 . . ? O5 C46 H46B 110.3 . . ? C45 C46 H46B 110.3 . . ? H46A C46 H46B 108.5 . . ? O6A C47A C48A 106.3(19) . . ? O6A C47A H47A 110.5 . . ? C48A C47A H47A 110.5 . . ? O6A C47A H47B 110.5 . . ? C48A C47A H47B 110.5 . . ? H47A C47A H47B 108.7 . . ? O6B C47B C48B 101(2) . . ? O6B C47B H47C 111.6 . . ? C48B C47B H47C 111.6 . . ? O6B C47B H47D 111.6 . . ? C48B C47B H47D 111.6 . . ? H47C C47B H47D 109.4 . . ? C49A C48A C47A 107.5(15) . . ? C49A C48A H48A 110.2 . . ? C47A C48A H48A 110.2 . . ? C49A C48A H48B 110.2 . . ? C47A C48A H48B 110.2 . . ? H48A C48A H48B 108.5 . . ? C47B C48B C49B 89(2) . . ? C47B C48B H48C 113.8 . . ? C49B C48B H48C 113.9 . . ? C47B C48B H48D 113.9 . . ? C49B C48B H48D 113.8 . . ? H48C C48B H48D 111.1 . . ? C50A C49A C48A 103.9(14) . . ? C50A C49A H49A 111.0 . . ? C48A C49A H49A 111.0 . . ? C50A C49A H49B 111.0 . . ? C48A C49A H49B 111.0 . . ? H49A C49A H49B 109.0 . . ? C50B C49B C48B 111(2) . . ? C50B C49B H49C 109.5 . . ? C48B C49B H49C 109.5 . . ? C50B C49B H49D 109.5 . . ? C48B C49B H49D 109.5 . . ? H49C C49B H49D 108.1 . . ? C49A C50A O6A 108.0(15) . . ? C49A C50A H50A 110.1 . . ? O6A C50A H50A 110.1 . . ? C49A C50A H50B 110.1 . . ? O6A C50A H50B 110.1 . . ? H50A C50A H50B 108.4 . . ? O6B C50B C49B 72(2) . . ? O6B C50B H50C 116.3 . . ? C49B C50B H50C 116.3 . . ? O6B C50B H50D 116.3 . . ? C49B C50B H50D 116.3 . . ? H50C C50B H50D 113.3 . . ? 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 O2 Yb1 O1 C1 -47.2(5) . . . . ? O5 Yb1 O1 C1 -111.9(4) . . . . ? O3 Yb1 O1 C1 82.8(4) . . . . ? O4 Yb1 O1 C1 163.5(4) . . . . ? N1 Yb1 O1 C1 -2.0(4) . . . . ? C7 Yb1 O1 C1 -5.7(5) . . . . ? O1 Yb1 O2 C7 92.4(3) . . . . ? O5 Yb1 O2 C7 159.5(3) . . . . ? O3 Yb1 O2 C7 -39.2(3) . . . . ? O4 Yb1 O2 C7 -121.1(3) . . . . ? N1 Yb1 O2 C7 48.3(3) . . . . ? O1 Yb1 O3 C35 11.2(3) . . . . ? O2 Yb1 O3 C35 170.6(3) . . . . ? O5 Yb1 O3 C35 -119.5(4) . . . . ? O4 Yb1 O3 C35 -77.5(3) . . . . ? N1 Yb1 O3 C35 87.4(3) . . . . ? C7 Yb1 O3 C35 156.9(3) . . . . ? O1 Yb1 O3 C38 -159.2(4) . . . . ? O2 Yb1 O3 C38 0.2(4) . . . . ? O5 Yb1 O3 C38 70.1(6) . . . . ? O4 Yb1 O3 C38 112.0(5) . . . . ? N1 Yb1 O3 C38 -83.0(4) . . . . ? C7 Yb1 O3 C38 -13.5(4) . . . . ? O1 Yb1 O4 C39 -167.7(5) . . . . ? O2 Yb1 O4 C39 27.0(5) . . . . ? O5 Yb1 O4 C39 102.6(5) . . . . ? O3 Yb1 O4 C39 -64.4(5) . . . . ? N1 Yb1 O4 C39 -118.4(5) . . . . ? C7 Yb1 O4 C39 5.4(5) . . . . ? O1 Yb1 O4 C42 9.6(7) . . . . ? O2 Yb1 O4 C42 -155.7(7) . . . . ? O5 Yb1 O4 C42 -80.2(7) . . . . ? O3 Yb1 O4 C42 112.8(7) . . . . ? N1 Yb1 O4 C42 58.8(8) . . . . ? C7 Yb1 O4 C42 -177.4(7) . . . . ? O1 Yb1 O5 C46 -17.4(6) . . . . ? O2 Yb1 O5 C46 -172.4(7) . . . . ? O3 Yb1 O5 C46 115.0(7) . . . . ? O4 Yb1 O5 C46 73.5(6) . . . . ? N1 Yb1 O5 C46 -93.6(6) . . . . ? C7 Yb1 O5 C46 -165.0(6) . . . . ? O1 Yb1 O5 C43 164.9(6) . . . . ? O2 Yb1 O5 C43 9.9(6) . . . . ? O3 Yb1 O5 C43 -62.7(7) . . . . ? O4 Yb1 O5 C43 -104.1(6) . . . . ? N1 Yb1 O5 C43 88.8(6) . . . . ? C7 Yb1 O5 C43 17.4(6) . . . . ? O1 Yb1 N1 C15 83.7(2) . . . . ? O2 Yb1 N1 C15 -115.5(2) . . . . ? O5 Yb1 N1 C15 168.8(2) . . . . ? O3 Yb1 N1 C15 -20.4(2) . . . . ? O4 Yb1 N1 C15 32.7(4) . . . . ? C7 Yb1 N1 C15 -98.5(2) . . . . ? O1 Yb1 N1 C13 -40.6(2) . . . . ? O2 Yb1 N1 C13 120.2(2) . . . . ? O5 Yb1 N1 C13 44.6(2) . . . . ? O3 Yb1 N1 C13 -144.7(2) . . . . ? O4 Yb1 N1 C13 -91.6(4) . . . . ? C7 Yb1 N1 C13 137.2(2) . . . . ? O1 Yb1 N1 C14 -153.8(2) . . . . ? O2 Yb1 N1 C14 7.0(2) . . . . ? O5 Yb1 N1 C14 -68.7(2) . . . . ? O3 Yb1 N1 C14 102.1(2) . . . . ? O4 Yb1 N1 C14 155.2(3) . . . . ? C7 Yb1 N1 C14 23.98(19) . . . . ? Yb1 O1 C1 C6 23.2(5) . . . . ? Yb1 O1 C1 C2 -159.0(3) . . . . ? O1 C1 C2 C3 -177.9(3) . . . . ? C6 C1 C2 C3 -0.1(5) . . . . ? O1 C1 C2 C19 4.5(5) . . . . ? C6 C1 C2 C19 -177.6(3) . . . . ? C1 C2 C3 C4 2.1(5) . . . . ? C19 C2 C3 C4 179.6(3) . . . . ? C2 C3 C4 C5 -2.9(6) . . . . ? C2 C3 C4 C23 176.9(4) . . . . ? C3 C4 C5 C6 1.8(5) . . . . ? C23 C4 C5 C6 -178.0(4) . . . . ? C4 C5 C6 C1 0.1(5) . . . . ? C4 C5 C6 C13 175.5(3) . . . . ? O1 C1 C6 C5 177.0(3) . . . . ? C2 C1 C6 C5 -1.0(5) . . . . ? O1 C1 C6 C13 1.5(5) . . . . ? C2 C1 C6 C13 -176.4(3) . . . . ? Yb1 O2 C7 C12 -53.7(4) . . . . ? Yb1 O2 C7 C8 127.1(3) . . . . ? O1 Yb1 C7 O2 -123.8(3) . . . . ? O5 Yb1 C7 O2 -20.3(3) . . . . ? O3 Yb1 C7 O2 139.9(3) . . . . ? O4 Yb1 C7 O2 68.9(3) . . . . ? N1 Yb1 C7 O2 -127.7(3) . . . . ? O1 Yb1 C7 C12 11.4(3) . . . . ? O2 Yb1 C7 C12 135.2(4) . . . . ? O5 Yb1 C7 C12 114.8(2) . . . . ? O3 Yb1 C7 C12 -84.9(2) . . . . ? O4 Yb1 C7 C12 -156.0(2) . . . . ? N1 Yb1 C7 C12 7.50(19) . . . . ? O1 Yb1 C7 C8 149.6(3) . . . . ? O2 Yb1 C7 C8 -86.6(4) . . . . ? O5 Yb1 C7 C8 -106.9(4) . . . . ? O3 Yb1 C7 C8 53.4(4) . . . . ? O4 Yb1 C7 C8 -17.7(4) . . . . ? N1 Yb1 C7 C8 145.7(4) . . . . ? O2 C7 C8 C9 -170.1(3) . . . . ? C12 C7 C8 C9 10.7(5) . . . . ? Yb1 C7 C8 C9 -120.4(4) . . . . ? O2 C7 C8 C27 10.3(5) . . . . ? C12 C7 C8 C27 -169.0(3) . . . . ? Yb1 C7 C8 C27 59.9(5) . . . . ? C7 C8 C9 C10 -3.8(6) . . . . ? C27 C8 C9 C10 175.9(4) . . . . ? C8 C9 C10 C11 -4.4(6) . . . . ? C8 C9 C10 C31 176.3(4) . . . . ? C9 C10 C11 C12 5.6(5) . . . . ? C31 C10 C11 C12 -175.2(3) . . . . ? C10 C11 C12 C7 1.4(5) . . . . ? C10 C11 C12 C14 -176.5(3) . . . . ? O2 C7 C12 C11 171.0(3) . . . . ? C8 C7 C12 C11 -9.7(5) . . . . ? Yb1 C7 C12 C11 139.9(3) . . . . ? O2 C7 C12 C14 -10.9(5) . . . . ? C8 C7 C12 C14 168.3(3) . . . . ? Yb1 C7 C12 C14 -42.0(3) . . . . ? C15 N1 C13 C6 -49.6(4) . . . . ? C14 N1 C13 C6 -173.8(3) . . . . ? Yb1 N1 C13 C6 76.9(3) . . . . ? C5 C6 C13 N1 124.4(4) . . . . ? C1 C6 C13 N1 -60.0(4) . . . . ? C15 N1 C14 C12 63.3(4) . . . . ? C13 N1 C14 C12 -172.0(3) . . . . ? Yb1 N1 C14 C12 -61.9(3) . . . . ? C11 C12 C14 N1 -98.7(4) . . . . ? C7 C12 C14 N1 83.3(4) . . . . ? C13 N1 C15 C16 -61.0(4) . . . . ? C14 N1 C15 C16 61.3(4) . . . . ? Yb1 N1 C15 C16 179.0(3) . . . . ? N1 C15 C16 C17 -163.6(4) . . . . ? C15 C16 C17 C18 170.9(5) . . . . ? C3 C2 C19 C20 -0.9(5) . . . . ? C1 C2 C19 C20 176.6(3) . . . . ? C3 C2 C19 C22 118.3(4) . . . . ? C1 C2 C19 C22 -64.1(4) . . . . ? C3 C2 C19 C21 -121.2(4) . . . . ? C1 C2 C19 C21 56.3(5) . . . . ? C5 C4 C23 C24A -120.0(7) . . . . ? C3 C4 C23 C24A 60.2(8) . . . . ? C5 C4 C23 C25B 45.7(10) . . . . ? C3 C4 C23 C25B -134.0(9) . . . . ? C5 C4 C23 C24B -157.0(7) . . . . ? C3 C4 C23 C24B 23.2(8) . . . . ? C5 C4 C23 C26A 7.4(7) . . . . ? C3 C4 C23 C26A -172.4(6) . . . . ? C5 C4 C23 C25A 119.0(6) . . . . ? C3 C4 C23 C25A -60.8(6) . . . . ? C5 C4 C23 C26B -59.1(9) . . . . ? C3 C4 C23 C26B 121.1(9) . . . . ? C9 C8 C27 C28 -7.9(5) . . . . ? C7 C8 C27 C28 171.8(4) . . . . ? C9 C8 C27 C30 113.0(4) . . . . ? C7 C8 C27 C30 -67.3(5) . . . . ? C9 C8 C27 C29 -126.3(4) . . . . ? C7 C8 C27 C29 53.3(4) . . . . ? C11 C10 C31 C33 0.1(6) . . . . ? C9 C10 C31 C33 179.3(4) . . . . ? C11 C10 C31 C34 -119.7(4) . . . . ? C9 C10 C31 C34 59.5(5) . . . . ? C11 C10 C31 C32 120.8(4) . . . . ? C9 C10 C31 C32 -60.0(5) . . . . ? C38 O3 C35 C36 7.6(6) . . . . ? Yb1 O3 C35 C36 -164.9(4) . . . . ? O3 C35 C36 C37 -23.1(6) . . . . ? C35 C36 C37 C38 29.6(7) . . . . ? C35 O3 C38 C37 11.0(7) . . . . ? Yb1 O3 C38 C37 -177.9(4) . . . . ? C36 C37 C38 O3 -25.5(7) . . . . ? C42 O4 C39 C40 7.9(8) . . . . ? Yb1 O4 C39 C40 -174.5(4) . . . . ? O4 C39 C40 C41 10.7(7) . . . . ? C39 C40 C41 C42 -24.7(8) . . . . ? C39 O4 C42 C41 -23.8(10) . . . . ? Yb1 O4 C42 C41 158.5(5) . . . . ? C40 C41 C42 O4 30.1(9) . . . . ? C46 O5 C43 C44 -20.1(10) . . . . ? Yb1 O5 C43 C44 158.0(5) . . . . ? O5 C43 C44 C45 5.4(10) . . . . ? C43 C44 C45 C46 10.7(10) . . . . ? C43 O5 C46 C45 26.8(10) . . . . ? Yb1 O5 C46 C45 -151.2(5) . . . . ? C44 C45 C46 O5 -23.3(10) . . . . ? C50A O6A C47A C48A 15(4) . . . . ? C50B O6B C47B C48B 49(3) . . . . ? O6A C47A C48A C49A -2(4) . . . . ? O6B C47B C48B C49B 0(3) . . . . ? C47A C48A C49A C50A -12(3) . . . . ? C47B C48B C49B C50B -48(3) . . . . ? C48A C49A C50A O6A 21(2) . . . . ? C47A O6A C50A C49A -24(3) . . . . ? C47B O6B C50B C49B -66(3) . . . . ? C48B C49B C50B O6B 71(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.879 _refine_diff_density_min -1.263 _refine_diff_density_rms 0.085