# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Wiecko, Michal' 'Deacon, Glen' 'Junk, Peter' _publ_contact_author_name 'Peter Junk' _publ_contact_author_address ; School of Chemistry Monash University Melbourne Victoria Australia 3800 ; _publ_contact_author_email peter.junk@sci.monash.edu.au # Attachment 'compound-1.CIF.txt' data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 776742' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H43 Eu I N2 O4' _chemical_formula_sum 'C31 H43 Eu I N2 O4' _chemical_formula_weight 786.53 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' 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' I I -0.4742 1.8119 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pmn21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 17.7513(3) _cell_length_b 8.7645(2) _cell_length_c 10.3139(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1604.65(6) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 13764 _cell_measurement_theta_min 3.26 _cell_measurement_theta_max 27.50 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 782 _exptl_absorpt_coefficient_mu 2.952 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1563 _exptl_absorpt_correction_T_max 0.3200 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13764 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3616 _reflns_number_gt 3573 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(7) _refine_ls_number_reflns 3616 _refine_ls_number_parameters 212 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0139 _refine_ls_R_factor_gt 0.0136 _refine_ls_wR_factor_ref 0.0320 _refine_ls_wR_factor_gt 0.0319 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 1.0000 0.185327(14) 0.599522(13) 0.01670(4) Uani 1 2 d S . . I1 I 1.0000 0.46510(2) 0.400436(17) 0.02334(5) Uani 1 2 d S . . O1 O 1.14195(8) 0.14207(18) 0.56225(15) 0.0271(3) Uani 1 1 d . E . N1 N 1.03887(9) 0.28318(19) 0.82096(17) 0.0185(3) Uani 1 1 d . . . C1 C 1.06202(12) 0.3242(2) 0.9404(2) 0.0189(4) Uani 1 1 d . . . O2 O 1.0000 -0.0006(3) 0.4011(3) 0.0263(4) Uani 1 2 d S . . C2 C 1.0000 0.3497(4) 1.0202(3) 0.0206(6) Uani 1 2 d S . . H2 H 1.0000 0.3780 1.1091 0.025 Uiso 1 2 calc SR . . O3 O 1.0000 -0.0715(2) 0.7173(2) 0.0255(5) Uani 1 2 d S . . C3 C 1.14243(12) 0.3394(2) 0.9718(2) 0.0195(4) Uani 1 1 d . . . C4 C 1.19706(13) 0.3407(3) 0.8742(2) 0.0256(5) Uani 1 1 d . . . H4 H 1.1822 0.3295 0.7863 0.031 Uiso 1 1 calc R . . C5 C 1.27285(13) 0.3582(3) 0.9044(3) 0.0301(5) Uani 1 1 d . . . H5 H 1.3094 0.3598 0.8371 0.036 Uiso 1 1 calc R . . C6 C 1.29520(13) 0.3735(3) 1.0324(3) 0.0281(5) Uani 1 1 d . . . H6 H 1.3471 0.3842 1.0530 0.034 Uiso 1 1 calc R . . C7 C 1.24226(13) 0.3730(3) 1.1295(2) 0.0270(5) Uani 1 1 d . . . H7 H 1.2575 0.3843 1.2173 0.032 Uiso 1 1 calc R . . C8 C 1.16622(11) 0.3560(2) 1.0994(3) 0.0239(4) Uani 1 1 d . . . H8 H 1.1300 0.3558 1.1672 0.029 Uiso 1 1 calc R . . C9 C 1.19418(16) 0.2157(3) 0.4761(3) 0.0434(7) Uani 1 1 d . . . H9A H 1.1809 0.3249 0.4670 0.052 Uiso 1 1 calc R A 1 H9B H 1.1916 0.1678 0.3892 0.052 Uiso 1 1 calc R A 1 C11 C 1.26404(14) 0.0531(3) 0.6130(5) 0.0562(9) Uani 1 1 d . . . H11A H 1.2848 -0.0359 0.5659 0.067 Uiso 1 1 calc R B 1 H11B H 1.2923 0.0660 0.6951 0.067 Uiso 1 1 calc R B 1 C12 C 1.18148(14) 0.0314(3) 0.6395(3) 0.0385(6) Uani 1 1 d . E . H12A H 1.1657 -0.0732 0.6156 0.046 Uiso 1 1 calc R . . H12B H 1.1707 0.0475 0.7327 0.046 Uiso 1 1 calc R . . C14 C 1.04248(15) -0.1006(6) 0.2031(3) 0.0603(10) Uani 1 1 d . . . H14A H 1.0629 -0.0120 0.1550 0.072 Uiso 1 1 calc R C 1 H14B H 1.0629 -0.1959 0.1654 0.072 Uiso 1 1 calc R C 1 C15 C 1.0000 -0.2213(4) 0.6584(4) 0.0329(8) Uani 1 2 d S . . H15A H 1.0308 -0.2229 0.5785 0.040 Uiso 0.50 1 calc PR . . H15B H 0.9482 -0.2551 0.6376 0.040 Uiso 0.50 1 calc PR . . C16 C 1.0357(4) -0.3228(5) 0.7665(5) 0.0386(13) Uani 0.50 1 d P D -1 H16A H 1.0224 -0.4317 0.7553 0.046 Uiso 0.50 1 calc PR D -1 H16B H 1.0912 -0.3120 0.7691 0.046 Uiso 0.50 1 calc PR D -1 C17 C 1.0000 -0.2571(4) 0.8823(4) 0.0421(9) Uani 1 2 d S . . H17A H 1.0293 -0.2818 0.9613 0.051 Uiso 0.50 1 calc PR D . H17B H 0.9480 -0.2959 0.8928 0.051 Uiso 0.50 1 calc PR . . C18 C 1.0000 -0.0878(4) 0.8572(3) 0.0448(11) Uani 1 2 d S D . H18A H 0.9547 -0.0396 0.8953 0.054 Uiso 0.50 1 calc PR . . H18B H 1.0453 -0.0396 0.8953 0.054 Uiso 0.50 1 calc PR . . C10B C 1.2696(3) 0.2014(11) 0.5276(9) 0.039(2) Uani 0.498(17) 1 d P E 1 H10D H 1.2833 0.2912 0.5808 0.047 Uiso 0.498(17) 1 calc PR E 1 H10C H 1.3071 0.1891 0.4573 0.047 Uiso 0.498(17) 1 calc PR E 1 C10A C 1.2633(4) 0.1173(14) 0.4867(7) 0.044(2) Uani 0.502(17) 1 d P E 2 H10A H 1.2620 0.0355 0.4206 0.053 Uiso 0.502(17) 1 calc PR E 2 H10B H 1.3092 0.1794 0.4726 0.053 Uiso 0.502(17) 1 calc PR E 2 C13B C 1.0597(3) -0.0893(7) 0.3467(6) 0.0335(12) Uani 0.50 1 d P F 1 H13D H 1.0612 -0.1920 0.3866 0.040 Uiso 0.50 1 calc PR F 1 H13C H 1.1089 -0.0387 0.3609 0.040 Uiso 0.50 1 calc PR F 1 C13A C 1.0633(3) -0.0026(8) 0.3138(6) 0.0374(13) Uani 0.50 1 d P F 2 H13A H 1.1084 -0.0439 0.3581 0.045 Uiso 0.50 1 calc PR F 2 H13B H 1.0748 0.1020 0.2835 0.045 Uiso 0.50 1 calc PR F 2 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 0.01608(6) 0.01871(7) 0.01532(6) -0.00165(6) 0.000 0.000 I1 0.02790(10) 0.02320(10) 0.01892(9) 0.00045(8) 0.000 0.000 O1 0.0185(7) 0.0308(8) 0.0319(9) 0.0001(6) 0.0016(6) 0.0033(6) N1 0.0184(8) 0.0193(8) 0.0177(9) -0.0010(7) -0.0003(7) -0.0003(6) C1 0.0212(10) 0.0164(10) 0.0192(10) 0.0017(7) -0.0003(8) -0.0005(8) O2 0.0273(11) 0.0318(12) 0.0198(10) -0.0076(11) 0.000 0.000 C2 0.0221(15) 0.0230(16) 0.0167(14) -0.0024(12) 0.000 0.000 O3 0.0412(13) 0.0202(11) 0.0150(10) -0.0009(8) 0.000 0.000 C3 0.0201(10) 0.0148(9) 0.0236(10) 0.0006(9) -0.0012(8) 0.0003(8) C4 0.0241(11) 0.0327(12) 0.0200(11) 0.0000(9) 0.0008(9) -0.0010(9) C5 0.0226(10) 0.0363(12) 0.0315(11) -0.0003(11) 0.0045(10) -0.0007(10) C6 0.0191(11) 0.0268(12) 0.0385(12) 0.0034(10) -0.0040(10) -0.0021(9) C7 0.0277(11) 0.0268(11) 0.0264(13) 0.0004(9) -0.0065(8) -0.0032(8) C8 0.0243(9) 0.0250(9) 0.0223(9) 0.0003(12) -0.0017(12) -0.0005(7) C9 0.0291(14) 0.0433(17) 0.0578(17) 0.0089(14) 0.0110(13) -0.0018(11) C11 0.0215(12) 0.0452(15) 0.102(3) 0.010(2) -0.0012(17) 0.0055(10) C12 0.0278(12) 0.0298(13) 0.0580(18) 0.0076(11) -0.0057(12) 0.0019(9) C14 0.0279(14) 0.121(3) 0.0320(14) -0.0319(18) 0.0035(12) -0.0008(18) C15 0.057(2) 0.0206(15) 0.0213(16) -0.0035(14) 0.000 0.000 C16 0.066(4) 0.022(2) 0.027(3) 0.0017(18) -0.004(2) 0.013(2) C17 0.077(3) 0.0247(18) 0.0246(19) 0.0048(15) 0.000 0.000 C18 0.090(4) 0.0251(19) 0.0189(16) -0.0009(14) 0.000 0.000 C10B 0.021(3) 0.042(5) 0.053(4) 0.004(4) 0.006(3) -0.003(2) C10A 0.024(3) 0.058(6) 0.052(4) -0.017(4) 0.013(2) 0.001(3) C13B 0.036(3) 0.035(3) 0.029(3) -0.011(3) -0.003(2) 0.004(3) C13A 0.031(3) 0.057(4) 0.025(3) -0.016(3) 0.005(2) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 N1 2.5353(17) . ? Eu1 N1 2.5353(17) 3_755 ? Eu1 O3 2.558(2) . ? Eu1 O1 2.5770(14) 3_755 ? Eu1 O1 2.5770(14) . ? Eu1 O2 2.616(2) . ? Eu1 I1 3.1983(2) . ? O1 C9 1.438(3) . ? O1 C12 1.438(3) . ? N1 C1 1.348(3) . ? N1 N1 1.380(3) 3_755 ? C1 C2 1.393(3) . ? C1 C3 1.470(3) . ? O2 C13B 1.429(6) 3_755 ? O2 C13B 1.429(6) . ? O2 C13A 1.440(6) 3_755 ? O2 C13A 1.440(6) . ? C2 C1 1.393(3) 3_755 ? O3 C15 1.447(4) . ? O3 C18 1.450(4) . ? C3 C8 1.390(4) . ? C3 C4 1.398(3) . ? C4 C5 1.389(3) . ? C5 C6 1.385(4) . ? C6 C7 1.373(3) . ? C7 C8 1.393(3) . ? C9 C10B 1.446(7) . ? C9 C10A 1.504(8) . ? C11 C10A 1.419(8) . ? C11 C12 1.503(4) . ? C11 C10B 1.573(8) . ? C14 C13A 1.475(6) . ? C14 C14 1.508(5) 3_755 ? C14 C13B 1.515(7) . ? C15 C16 1.560(6) . ? C15 C16 1.560(6) 3_755 ? C16 C17 1.470(6) . ? C17 C16 1.470(6) 3_755 ? C17 C18 1.506(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Eu1 N1 31.58(8) . 3_755 ? N1 Eu1 O3 82.52(6) . . ? N1 Eu1 O3 82.52(6) 3_755 . ? N1 Eu1 O1 116.76(5) . 3_755 ? N1 Eu1 O1 85.30(5) 3_755 3_755 ? O3 Eu1 O1 86.64(4) . 3_755 ? N1 Eu1 O1 85.30(5) . . ? N1 Eu1 O1 116.76(5) 3_755 . ? O3 Eu1 O1 86.64(4) . . ? O1 Eu1 O1 155.81(7) 3_755 . ? N1 Eu1 O2 156.27(6) . . ? N1 Eu1 O2 156.27(6) 3_755 . ? O3 Eu1 O2 79.83(7) . . ? O1 Eu1 O2 77.97(3) 3_755 . ? O1 Eu1 O2 77.97(3) . . ? N1 Eu1 I1 108.60(4) . . ? N1 Eu1 I1 108.60(4) 3_755 . ? O3 Eu1 I1 168.42(5) . . ? O1 Eu1 I1 90.98(3) 3_755 . ? O1 Eu1 I1 90.98(3) . . ? O2 Eu1 I1 88.58(5) . . ? C9 O1 C12 109.31(18) . . ? C9 O1 Eu1 131.06(14) . . ? C12 O1 Eu1 119.58(14) . . ? C1 N1 N1 107.75(12) . 3_755 ? C1 N1 Eu1 175.44(15) . . ? N1 N1 Eu1 74.21(4) 3_755 . ? N1 C1 C2 110.00(19) . . ? N1 C1 C3 121.44(19) . . ? C2 C1 C3 128.6(2) . . ? C13B O2 C13B 95.7(5) 3_755 . ? C13B O2 C13A 33.8(3) 3_755 3_755 ? C13B O2 C13A 109.0(3) . 3_755 ? C13B O2 C13A 109.0(3) 3_755 . ? C13B O2 C13A 33.8(3) . . ? C13A O2 C13A 102.5(5) 3_755 . ? C13B O2 Eu1 130.2(2) 3_755 . ? C13B O2 Eu1 130.2(2) . . ? C13A O2 Eu1 119.8(2) 3_755 . ? C13A O2 Eu1 119.8(2) . . ? C1 C2 C1 104.5(3) 3_755 . ? C15 O3 C18 109.1(3) . . ? C15 O3 Eu1 126.82(19) . . ? C18 O3 Eu1 124.0(2) . . ? C8 C3 C4 118.04(19) . . ? C8 C3 C1 120.9(2) . . ? C4 C3 C1 121.08(19) . . ? C5 C4 C3 120.8(2) . . ? C6 C5 C4 120.1(2) . . ? C7 C6 C5 119.9(2) . . ? C6 C7 C8 120.1(2) . . ? C3 C8 C7 121.1(2) . . ? O1 C9 C10B 109.3(3) . . ? O1 C9 C10A 102.9(4) . . ? C10B C9 C10A 33.7(3) . . ? C10A C11 C12 102.0(4) . . ? C10A C11 C10B 32.8(3) . . ? C12 C11 C10B 105.5(3) . . ? O1 C12 C11 106.9(2) . . ? C13A C14 C14 104.5(2) . 3_755 ? C13A C14 C13B 32.4(3) . . ? C14 C14 C13B 101.6(3) 3_755 . ? O3 C15 C16 102.6(3) . . ? O3 C15 C16 102.6(3) . 3_755 ? C16 C15 C16 47.9(5) . 3_755 ? C17 C16 C15 100.5(3) . . ? C16 C17 C16 51.1(5) 3_755 . ? C16 C17 C18 104.3(3) 3_755 . ? C16 C17 C18 104.3(3) . . ? O3 C18 C17 105.6(3) . . ? C9 C10B C11 102.7(4) . . ? C11 C10A C9 107.5(4) . . ? O2 C13B C14 105.6(4) . . ? O2 C13A C14 107.2(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.413 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.053 # Attachment 'compound-2.CIF.txt' data_D:\X-Tals\crystalwork\63a2\Publ\MW63A3.CIF _database_code_depnum_ccdc_archive 'CCDC 776743' #TrackingRef 'compound-2.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety 'C31 H43 I N2 O4 Yb' _chemical_formula_sum 'C31 H43 I N2 O4 Yb' _chemical_formula_weight 807.61 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' I I -0.4742 1.8119 '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 orthorhombic _symmetry_space_group_name_H-M Pmn21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 17.6761(8) _cell_length_b 8.7327(4) _cell_length_c 10.1877(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1572.57(13) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 13478 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 27.50 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 3.991 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2402 _exptl_absorpt_correction_T_max 0.3806 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13478 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3722 _reflns_number_gt 3515 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(8) _refine_ls_number_reflns 3722 _refine_ls_number_parameters 213 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0500 _refine_ls_wR_factor_gt 0.0489 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.5000 0.82316(2) 0.348851(17) 0.01485(6) Uani 1 2 d S . . I1 I 0.5000 0.55014(4) 0.15490(4) 0.02091(9) Uani 1 2 d S . . O1 O 0.36314(16) 0.8633(3) 0.3122(3) 0.0229(7) Uani 1 1 d . C . N1 N 0.46088(18) 0.7209(3) 0.5604(3) 0.0172(7) Uani 1 1 d . . . C1 C 0.4375(2) 0.6778(4) 0.6822(4) 0.0183(8) Uani 1 1 d . A 2 O2 O 0.5000 1.0009(4) 0.1542(4) 0.0223(9) Uani 1 2 d S . . C2 C 0.5000 0.6520(6) 0.7623(5) 0.0187(14) Uani 1 2 d S . 2 H2 H 0.5000 0.6231 0.8522 0.022 Uiso 1 2 calc SR . 2 O3 O 0.5000 1.0697(4) 0.4618(4) 0.0202(9) Uani 1 2 d S . . C3 C 0.3574(3) 0.6623(4) 0.7137(4) 0.0195(8) Uani 1 1 d . . . C4 C 0.3020(3) 0.6549(5) 0.6161(4) 0.0261(10) Uani 1 1 d . A . H4 H 0.3166 0.6617 0.5265 0.031 Uiso 1 1 calc R . . C5 C 0.2258(3) 0.6377(5) 0.6474(5) 0.0266(9) Uani 1 1 d . . . H5 H 0.1888 0.6343 0.5797 0.032 Uiso 1 1 calc R A . C6 C 0.2039(3) 0.6257(5) 0.7783(5) 0.0274(10) Uani 1 1 d . A . H6 H 0.1520 0.6134 0.8003 0.033 Uiso 1 1 calc R . . C7 C 0.2579(3) 0.6317(5) 0.8756(4) 0.0258(11) Uani 1 1 d . . . H7 H 0.2430 0.6239 0.9649 0.031 Uiso 1 1 calc R A . C8 C 0.3335(2) 0.6490(4) 0.8447(6) 0.0227(8) Uani 1 1 d . A . H8 H 0.3700 0.6520 0.9131 0.027 Uiso 1 1 calc R . . C9 C 0.3105(3) 0.7837(6) 0.2273(6) 0.0388(12) Uani 1 1 d . . . H9A H 0.3139 0.8262 0.1374 0.047 Uiso 1 1 calc R B 1 H9B H 0.3241 0.6739 0.2233 0.047 Uiso 1 1 calc R B 1 C10A C 0.2405(6) 0.885(2) 0.2373(11) 0.036(4) Uani 0.54(3) 1 d P C 2 H10A H 0.2426 0.9671 0.1708 0.043 Uiso 0.54(3) 1 calc PR C 2 H10B H 0.1943 0.8230 0.2219 0.043 Uiso 0.54(3) 1 calc PR C 2 C11 C 0.2393(3) 0.9470(5) 0.3634(8) 0.0513(16) Uani 1 1 d . . . H11A H 0.2190 1.0371 0.3160 0.062 Uiso 1 1 calc R C 1 H11B H 0.2099 0.9326 0.4452 0.062 Uiso 1 1 calc R C 1 C12 C 0.3219(3) 0.9687(5) 0.3939(5) 0.0338(12) Uani 1 1 d . C . H12A H 0.3374 1.0754 0.3748 0.041 Uiso 1 1 calc R . . H12B H 0.3318 0.9473 0.4877 0.041 Uiso 1 1 calc R . . C14 C 0.4570(3) 1.0993(9) -0.0475(6) 0.0617(19) Uani 1 1 d . . . H14A H 0.4372 1.2044 -0.0357 0.074 Uiso 1 1 calc R A 1 H14B H 0.4372 1.0572 -0.1309 0.074 Uiso 1 1 calc R A 1 C13A C 0.4354(5) 1.0016(12) 0.0635(10) 0.028(2) Uani 0.50 1 d P A 1 H13A H 0.3899 1.0428 0.1076 0.034 Uiso 0.50 1 calc PR A 1 H13B H 0.4243 0.8963 0.0329 0.034 Uiso 0.50 1 calc PR A 1 C15 C 0.5000 1.2217(7) 0.4030(7) 0.0329(16) Uani 1 2 d S . . H15A H 0.4679 1.2248 0.3235 0.039 Uiso 0.50 1 calc PR . . H15B H 0.5519 1.2544 0.3796 0.039 Uiso 0.50 1 calc PR . . C16 C 0.4667(7) 1.3235(9) 0.5136(9) 0.036(3) Uani 0.50 1 d P A -1 H16A H 0.4821 1.4318 0.5032 0.043 Uiso 0.50 1 calc PR A -1 H16B H 0.4108 1.3173 0.5160 0.043 Uiso 0.50 1 calc PR A -1 C17 C 0.5000 1.2562(7) 0.6294(7) 0.043(2) Uani 1 2 d S . . H17A H 0.4697 1.2812 0.7083 0.051 Uiso 0.50 1 calc PR A . H17B H 0.5522 1.2942 0.6424 0.051 Uiso 0.50 1 calc PR . . C18 C 0.5000 1.0866(7) 0.6048(6) 0.0364(18) Uani 1 2 d S A . H18A H 0.5455 1.0384 0.6435 0.044 Uiso 0.50 1 calc PR . . H18B H 0.4545 1.0384 0.6435 0.044 Uiso 0.50 1 calc PR . . C10B C 0.2348(8) 0.799(3) 0.2744(19) 0.041(5) Uani 0.46(3) 1 d P C 1 H10D H 0.2194 0.7084 0.3263 0.049 Uiso 0.46(3) 1 calc PR C 1 H10C H 0.1987 0.8134 0.2011 0.049 Uiso 0.46(3) 1 calc PR C 1 C13B C 0.4393(7) 1.0893(13) 0.0981(10) 0.033(2) Uani 0.50 1 d P A 2 H13D H 0.4374 1.1927 0.1377 0.040 Uiso 0.50 1 calc PR A 2 H13C H 0.3901 1.0379 0.1126 0.040 Uiso 0.50 1 calc PR A 2 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 0.01534(11) 0.01872(10) 0.01050(9) 0.00112(11) 0.000 0.000 I1 0.0261(2) 0.02199(18) 0.01461(17) -0.00124(15) 0.000 0.000 O1 0.0168(14) 0.0296(15) 0.0224(16) 0.0003(10) -0.0008(12) 0.0016(12) N1 0.0172(17) 0.0214(16) 0.0131(14) 0.0012(13) -0.0008(15) 0.0010(13) C1 0.023(2) 0.0170(18) 0.0151(17) -0.0021(14) 0.0022(17) -0.0011(16) O2 0.028(2) 0.024(2) 0.0146(18) 0.0092(19) 0.000 0.000 C2 0.025(4) 0.020(3) 0.011(2) 0.000(2) 0.000 0.000 O3 0.032(2) 0.0168(19) 0.0120(18) 0.0022(15) 0.000 0.000 C3 0.023(2) 0.0152(19) 0.0203(19) 0.0007(15) 0.0002(18) -0.0028(17) C4 0.026(3) 0.032(2) 0.021(2) -0.0027(17) -0.0006(19) -0.0001(19) C5 0.023(2) 0.033(2) 0.024(2) -0.0004(19) -0.004(2) 0.0006(19) C6 0.020(2) 0.029(2) 0.034(2) -0.0027(19) 0.005(2) -0.001(2) C7 0.029(2) 0.027(2) 0.022(3) -0.0015(16) 0.0085(19) -0.0021(17) C8 0.0257(19) 0.0239(18) 0.0184(16) -0.002(2) 0.004(3) 0.0009(14) C9 0.029(3) 0.042(3) 0.045(3) -0.010(2) -0.014(3) -0.001(2) C10A 0.020(6) 0.051(10) 0.037(5) 0.011(6) -0.015(4) 0.008(5) C11 0.021(2) 0.041(3) 0.092(5) -0.002(4) 0.003(4) 0.0042(19) C12 0.026(3) 0.027(2) 0.048(3) -0.0055(19) 0.004(2) 0.0041(19) C14 0.028(3) 0.122(6) 0.034(3) 0.033(3) -0.004(3) 0.006(4) C13A 0.018(5) 0.046(6) 0.021(5) 0.017(5) -0.007(4) 0.000(5) C15 0.054(5) 0.020(3) 0.025(3) 0.011(2) 0.000 0.000 C16 0.053(7) 0.020(4) 0.035(6) -0.003(4) 0.005(5) 0.005(4) C17 0.084(7) 0.020(3) 0.024(4) -0.001(3) 0.000 0.000 C18 0.065(6) 0.028(4) 0.016(3) -0.001(3) 0.000 0.000 C10B 0.030(7) 0.044(11) 0.048(9) -0.020(8) -0.020(6) 0.007(6) C13B 0.036(6) 0.039(6) 0.026(5) 0.018(5) -0.004(4) 0.007(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N1 2.433(3) 3_655 ? Yb1 N1 2.433(3) . ? Yb1 O3 2.441(4) . ? Yb1 O1 2.473(3) . ? Yb1 O1 2.473(3) 3_655 ? Yb1 O2 2.518(4) . ? Yb1 I1 3.0966(4) . ? O1 C12 1.440(5) . ? O1 C9 1.448(5) . ? N1 C1 1.361(5) . ? N1 N1 1.383(6) 3_655 ? C1 C2 1.392(5) . ? C1 C3 1.458(6) . ? O2 C13B 1.439(11) . ? O2 C13B 1.439(11) 3_655 ? O2 C13A 1.468(10) . ? O2 C13A 1.468(10) 3_655 ? C2 C1 1.392(5) 3_655 ? C2 H2 0.9500 . ? O3 C15 1.457(7) . ? O3 C18 1.464(7) . ? C3 C4 1.398(6) . ? C3 C8 1.404(7) . ? C4 C5 1.392(7) . ? C4 H4 0.9500 . ? C5 C6 1.392(7) . ? C5 H5 0.9500 . ? C6 C7 1.378(6) . ? C6 H6 0.9500 . ? C7 C8 1.381(6) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10B 1.427(16) . ? C9 C10A 1.521(13) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10A C11 1.396(14) . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? C11 C12 1.504(7) . ? C11 C10B 1.581(15) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C14 C13A 1.467(11) . ? C14 C13B 1.518(12) . ? C14 C14 1.520(11) 3_655 ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C13A H13A 0.9900 . ? C13A H13B 0.9900 . ? C15 C16 1.551(11) 3_655 ? C15 C16 1.551(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.443(11) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C16 1.443(11) 3_655 ? C17 C18 1.501(9) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C10B H10D 0.9900 . ? C10B H10C 0.9900 . ? C13B H13D 0.9900 . ? C13B H13C 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 N1 Yb1 N1 33.02(15) 3_655 . ? N1 Yb1 O3 84.61(11) 3_655 . ? N1 Yb1 O3 84.61(11) . . ? N1 Yb1 O1 117.63(10) 3_655 . ? N1 Yb1 O1 84.71(10) . . ? O3 Yb1 O1 86.91(7) . . ? N1 Yb1 O1 84.71(10) 3_655 3_655 ? N1 Yb1 O1 117.63(10) . 3_655 ? O3 Yb1 O1 86.91(7) . 3_655 ? O1 Yb1 O1 156.09(13) . 3_655 ? N1 Yb1 O2 157.47(10) 3_655 . ? N1 Yb1 O2 157.47(10) . . ? O3 Yb1 O2 80.07(13) . . ? O1 Yb1 O2 78.09(6) . . ? O1 Yb1 O2 78.09(6) 3_655 . ? N1 Yb1 I1 106.42(7) 3_655 . ? N1 Yb1 I1 106.42(7) . . ? O3 Yb1 I1 168.48(9) . . ? O1 Yb1 I1 90.74(6) . . ? O1 Yb1 I1 90.74(6) 3_655 . ? O2 Yb1 I1 88.40(9) . . ? C12 O1 C9 109.0(4) . . ? C12 O1 Yb1 120.0(3) . . ? C9 O1 Yb1 130.6(3) . . ? C1 N1 N1 107.7(2) . 3_655 ? C1 N1 Yb1 174.5(3) . . ? N1 N1 Yb1 73.49(8) 3_655 . ? N1 C1 C2 109.8(4) . . ? N1 C1 C3 121.5(4) . . ? C2 C1 C3 128.8(4) . . ? C13B O2 C13B 96.3(9) . 3_655 ? C13B O2 C13A 33.8(5) . . ? C13B O2 C13A 109.1(5) 3_655 . ? C13B O2 C13A 109.1(5) . 3_655 ? C13B O2 C13A 33.8(5) 3_655 3_655 ? C13A O2 C13A 102.0(9) . 3_655 ? C13B O2 Yb1 130.0(5) . . ? C13B O2 Yb1 130.0(5) 3_655 . ? C13A O2 Yb1 119.9(4) . . ? C13A O2 Yb1 119.9(4) 3_655 . ? C1 C2 C1 105.1(5) . 3_655 ? C1 C2 H2 127.5 . . ? C1 C2 H2 127.5 3_655 . ? C15 O3 C18 108.5(4) . . ? C15 O3 Yb1 127.6(3) . . ? C18 O3 Yb1 123.9(4) . . ? C4 C3 C8 117.5(4) . . ? C4 C3 C1 121.9(4) . . ? C8 C3 C1 120.6(4) . . ? C5 C4 C3 121.3(4) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 C6 119.8(4) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 119.6(4) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C8 120.7(4) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C7 C8 C3 121.1(5) . . ? C7 C8 H8 119.4 . . ? C3 C8 H8 119.4 . . ? C10B C9 O1 110.9(6) . . ? C10B C9 C10A 33.0(7) . . ? O1 C9 C10A 101.8(6) . . ? C10B C9 H9A 109.5 . . ? O1 C9 H9A 109.5 . . ? C10A C9 H9A 84.0 . . ? C10B C9 H9B 109.5 . . ? O1 C9 H9B 109.5 . . ? C10A C9 H9B 139.6 . . ? H9A C9 H9B 108.0 . . ? C11 C10A C9 107.5(7) . . ? C11 C10A H10A 110.2 . . ? C9 C10A H10A 110.2 . . ? C11 C10A H10B 110.2 . . ? C9 C10A H10B 110.2 . . ? H10A C10A H10B 108.5 . . ? C10A C11 C12 103.0(6) . . ? C10A C11 C10B 32.1(6) . . ? C12 C11 C10B 105.7(6) . . ? C10A C11 H11A 82.4 . . ? C12 C11 H11A 110.6 . . ? C10B C11 H11A 110.6 . . ? C10A C11 H11B 137.1 . . ? C12 C11 H11B 110.6 . . ? C10B C11 H11B 110.6 . . ? H11A C11 H11B 108.7 . . ? O1 C12 C11 107.0(4) . . ? O1 C12 H12A 110.3 . . ? C11 C12 H12A 110.3 . . ? O1 C12 H12B 110.3 . . ? C11 C12 H12B 110.3 . . ? H12A C12 H12B 108.6 . . ? C13A C14 C13B 32.9(5) . . ? C13A C14 C14 105.1(4) . 3_655 ? C13B C14 C14 101.9(5) . 3_655 ? C13A C14 H14A 110.7 . . ? C13B C14 H14A 82.1 . . ? C14 C14 H14A 110.7 3_655 . ? C13A C14 H14B 110.7 . . ? C13B C14 H14B 138.1 . . ? C14 C14 H14B 110.7 3_655 . ? H14A C14 H14B 108.8 . . ? O2 C13A C14 106.6(7) . . ? O2 C13A H13A 110.4 . . ? C14 C13A H13A 110.4 . . ? O2 C13A H13B 110.4 . . ? C14 C13A H13B 110.4 . . ? H13A C13A H13B 108.6 . . ? O3 C15 C16 102.9(5) . 3_655 ? O3 C15 C16 102.9(5) . . ? C16 C15 C16 44.6(9) 3_655 . ? O3 C15 H15A 111.2 . . ? C16 C15 H15A 142.8 3_655 . ? C16 C15 H15A 111.2 . . ? O3 C15 H15B 111.2 . . ? C16 C15 H15B 70.0 3_655 . ? C16 C15 H15B 111.2 . . ? H15A C15 H15B 109.1 . . ? C17 C16 C15 101.9(6) . . ? C17 C16 H16A 111.4 . . ? C15 C16 H16A 111.4 . . ? C17 C16 H16B 111.4 . . ? C15 C16 H16B 111.4 . . ? H16A C16 H16B 109.3 . . ? C16 C17 C16 48.1(9) . 3_655 ? C16 C17 C18 105.4(5) . . ? C16 C17 C18 105.4(5) 3_655 . ? C16 C17 H17A 110.7 . . ? C16 C17 H17A 142.5 3_655 . ? C18 C17 H17A 110.7 . . ? C16 C17 H17B 110.7 . . ? C16 C17 H17B 66.0 3_655 . ? C18 C17 H17B 110.7 . . ? H17A C17 H17B 108.8 . . ? O3 C18 C17 105.4(5) . . ? O3 C18 H18A 110.7 . . ? C17 C18 H18A 110.7 . . ? O3 C18 H18B 110.7 . . ? C17 C18 H18B 110.7 . . ? H18A C18 H18B 108.8 . . ? C9 C10B C11 102.8(10) . . ? C9 C10B H10D 111.2 . . ? C11 C10B H10D 111.2 . . ? C9 C10B H10C 111.2 . . ? C11 C10B H10C 111.2 . . ? H10D C10B H10C 109.1 . . ? O2 C13B C14 105.4(8) . . ? O2 C13B H13D 110.7 . . ? C14 C13B H13D 110.7 . . ? O2 C13B H13C 110.7 . . ? C14 C13B H13C 110.7 . . ? H13D C13B H13C 108.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Yb1 O1 C12 61.6(3) 3_655 . . . ? N1 Yb1 O1 C12 64.2(3) . . . . ? O3 Yb1 O1 C12 -20.6(3) . . . . ? O1 Yb1 O1 C12 -95.9(4) 3_655 . . . ? O2 Yb1 O1 C12 -101.1(3) . . . . ? I1 Yb1 O1 C12 170.6(3) . . . . ? N1 Yb1 O1 C9 -110.3(4) 3_655 . . . ? N1 Yb1 O1 C9 -107.7(4) . . . . ? O3 Yb1 O1 C9 167.4(4) . . . . ? O1 Yb1 O1 C9 92.2(5) 3_655 . . . ? O2 Yb1 O1 C9 86.9(4) . . . . ? I1 Yb1 O1 C9 -1.3(4) . . . . ? N1 Yb1 N1 C1 103(3) 3_655 . . . ? O3 Yb1 N1 C1 15(3) . . . . ? O1 Yb1 N1 C1 -72(3) . . . . ? O1 Yb1 N1 C1 99(3) 3_655 . . . ? O2 Yb1 N1 C1 -32(3) . . . . ? I1 Yb1 N1 C1 -162(3) . . . . ? O3 Yb1 N1 N1 -88.40(3) . . . 3_655 ? O1 Yb1 N1 N1 -175.78(7) . . . 3_655 ? O1 Yb1 N1 N1 -4.74(7) 3_655 . . 3_655 ? O2 Yb1 N1 N1 -135.6(3) . . . 3_655 ? I1 Yb1 N1 N1 95.01(3) . . . 3_655 ? N1 N1 C1 C2 1.0(4) 3_655 . . . ? Yb1 N1 C1 C2 -101(3) . . . . ? N1 N1 C1 C3 -178.3(3) 3_655 . . . ? Yb1 N1 C1 C3 80(3) . . . . ? N1 Yb1 O2 C13B -124.5(7) 3_655 . . . ? N1 Yb1 O2 C13B -28.7(8) . . . . ? O3 Yb1 O2 C13B -76.6(7) . . . . ? O1 Yb1 O2 C13B 12.3(7) . . . . ? O1 Yb1 O2 C13B -165.5(7) 3_655 . . . ? I1 Yb1 O2 C13B 103.4(7) . . . . ? N1 Yb1 O2 C13B 28.7(8) 3_655 . . 3_655 ? N1 Yb1 O2 C13B 124.5(7) . . . 3_655 ? O3 Yb1 O2 C13B 76.6(7) . . . 3_655 ? O1 Yb1 O2 C13B 165.5(7) . . . 3_655 ? O1 Yb1 O2 C13B -12.3(7) 3_655 . . 3_655 ? I1 Yb1 O2 C13B -103.4(7) . . . 3_655 ? N1 Yb1 O2 C13A -164.2(6) 3_655 . . . ? N1 Yb1 O2 C13A -68.5(7) . . . . ? O3 Yb1 O2 C13A -116.3(6) . . . . ? O1 Yb1 O2 C13A -27.4(6) . . . . ? O1 Yb1 O2 C13A 154.7(6) 3_655 . . . ? I1 Yb1 O2 C13A 63.7(6) . . . . ? N1 Yb1 O2 C13A 68.5(7) 3_655 . . 3_655 ? N1 Yb1 O2 C13A 164.2(6) . . . 3_655 ? O3 Yb1 O2 C13A 116.3(6) . . . 3_655 ? O1 Yb1 O2 C13A -154.7(6) . . . 3_655 ? O1 Yb1 O2 C13A 27.4(6) 3_655 . . 3_655 ? I1 Yb1 O2 C13A -63.7(6) . . . 3_655 ? N1 C1 C2 C1 -1.5(6) . . . 3_655 ? C3 C1 C2 C1 177.7(2) . . . 3_655 ? N1 Yb1 O3 C15 163.42(8) 3_655 . . . ? N1 Yb1 O3 C15 -163.42(8) . . . . ? O1 Yb1 O3 C15 -78.45(6) . . . . ? O1 Yb1 O3 C15 78.45(6) 3_655 . . . ? O2 Yb1 O3 C15 0.000(2) . . . . ? I1 Yb1 O3 C15 0.000(4) . . . . ? N1 Yb1 O3 C18 -16.58(8) 3_655 . . . ? N1 Yb1 O3 C18 16.58(8) . . . . ? O1 Yb1 O3 C18 101.55(6) . . . . ? O1 Yb1 O3 C18 -101.55(6) 3_655 . . . ? O2 Yb1 O3 C18 180.000(3) . . . . ? I1 Yb1 O3 C18 180.000(4) . . . . ? N1 C1 C3 C4 15.4(6) . . . . ? C2 C1 C3 C4 -163.7(5) . . . . ? N1 C1 C3 C8 -166.7(3) . . . . ? C2 C1 C3 C8 14.1(6) . . . . ? C8 C3 C4 C5 1.1(6) . . . . ? C1 C3 C4 C5 179.0(4) . . . . ? C3 C4 C5 C6 -0.8(7) . . . . ? C4 C5 C6 C7 0.4(7) . . . . ? C5 C6 C7 C8 -0.2(6) . . . . ? C6 C7 C8 C3 0.5(6) . . . . ? C4 C3 C8 C7 -1.0(5) . . . . ? C1 C3 C8 C7 -178.9(3) . . . . ? C12 O1 C9 C10B -16.8(13) . . . . ? Yb1 O1 C9 C10B 155.9(12) . . . . ? C12 O1 C9 C10A 16.4(8) . . . . ? Yb1 O1 C9 C10A -171.0(6) . . . . ? C10B C9 C10A C11 78.0(12) . . . . ? O1 C9 C10A C11 -32.4(12) . . . . ? C9 C10A C11 C12 34.1(12) . . . . ? C9 C10A C11 C10B -64.8(14) . . . . ? C9 O1 C12 C11 3.2(6) . . . . ? Yb1 O1 C12 C11 -170.3(3) . . . . ? C10A C11 C12 O1 -23.4(9) . . . . ? C10B C11 C12 O1 9.7(12) . . . . ? C13B O2 C13A C14 69.4(11) . . . . ? C13B O2 C13A C14 -2.6(13) 3_655 . . . ? C13A O2 C13A C14 -37.0(12) 3_655 . . . ? Yb1 O2 C13A C14 -172.2(5) . . . . ? C13B C14 C13A O2 -65.5(11) . . . . ? C14 C14 C13A O2 23.1(8) 3_655 . . . ? C18 O3 C15 C16 22.9(5) . . . 3_655 ? Yb1 O3 C15 C16 -157.1(5) . . . 3_655 ? C18 O3 C15 C16 -22.9(5) . . . . ? Yb1 O3 C15 C16 157.1(5) . . . . ? O3 C15 C16 C17 37.8(6) . . . . ? C16 C15 C16 C17 -57.6(6) 3_655 . . . ? C15 C16 C17 C16 58.8(6) . . . 3_655 ? C15 C16 C17 C18 -38.3(6) . . . . ? C15 O3 C18 C17 0.000(3) . . . . ? Yb1 O3 C18 C17 180.000(3) . . . . ? C16 C17 C18 O3 25.0(5) . . . . ? C16 C17 C18 O3 -25.0(5) 3_655 . . . ? O1 C9 C10B C11 21.7(17) . . . . ? C10A C9 C10B C11 -57.6(12) . . . . ? C10A C11 C10B C9 70.6(17) . . . . ? C12 C11 C10B C9 -18.9(16) . . . . ? C13B O2 C13B C14 51.1(12) 3_655 . . . ? C13A O2 C13B C14 -64.1(11) . . . . ? C13A O2 C13B C14 19.0(12) 3_655 . . . ? Yb1 O2 C13B C14 -149.2(5) . . . . ? C13A C14 C13B O2 67.4(10) . . . . ? C14 C14 C13B O2 -32.1(8) 3_655 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.967 _refine_diff_density_min -1.462 _refine_diff_density_rms 0.100 # Attachment 'compound-3.CIF.txt' data_D:\X-Tals\crystalwork\109b\Craig\publ\MW109B.CIF _database_code_depnum_ccdc_archive 'CCDC 776744' #TrackingRef 'compound-3.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H110 O14 Yb3' _chemical_formula_sum 'C152 H220 O28 Yb6' _chemical_formula_weight 3533.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 20.1461(7) _cell_length_b 20.3068(6) _cell_length_c 22.5761(12) _cell_angle_alpha 110.121(2) _cell_angle_beta 103.298(2) _cell_angle_gamma 106.657(2) _cell_volume 7734.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 54801 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3552 _exptl_absorpt_coefficient_mu 3.656 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5284 _exptl_absorpt_correction_T_max 0.7113 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54801 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.1084 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.00 _reflns_number_total 27110 _reflns_number_gt 17319 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 27110 _refine_ls_number_parameters 1756 _refine_ls_number_restraints 180 _refine_ls_R_factor_all 0.0978 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1156 _refine_ls_wR_factor_gt 0.0972 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.03016(2) 0.46019(2) 1.23338(2) 0.022 Uani 1 1 d . . . Yb2 Yb 0.48283(2) 0.64607(2) 1.41597(2) 0.021 Uani 1 1 d . . . Yb3 Yb -0.02528(2) 0.19090(2) 0.865860(19) 0.022 Uani 1 1 d . D . Yb4 Yb 0.47525(2) 0.00139(2) 0.73002(2) 0.024 Uani 1 1 d . . . Yb5 Yb 0.03251(2) -0.17212(2) 0.57591(2) 0.024 Uani 1 1 d . . . Yb6 Yb 0.57517(2) 0.32301(2) 1.09931(2) 0.026 Uani 1 1 d . . . O1 O 0.1115(3) 0.4369(3) 1.1638(3) 0.039 Uani 1 1 d . . . O2 O -0.0082(3) 0.3262(3) 1.1525(3) 0.032 Uani 1 1 d . . . O3 O 0.0810(3) 0.5989(3) 1.2577(3) 0.025 Uani 1 1 d . . . O4 O -0.0131(3) 0.4848(3) 1.1319(3) 0.028 Uani 1 1 d . . . O5 O -0.0044(3) 0.5235(3) 1.3337(3) 0.031 Uani 1 1 d . . . O6 O -0.1066(3) 0.4249(3) 1.2080(3) 0.029 Uani 1 1 d . . . O7 O 0.1555(3) 0.4967(3) 1.3167(3) 0.025 Uani 1 1 d . . . O8 O 0.0325(3) 0.3865(3) 1.3024(3) 0.028 Uani 1 1 d . . . O9 O 0.5727(3) 0.5885(3) 1.4306(3) 0.023 Uani 1 1 d . . . O10 O 0.5445(3) 0.6351(3) 1.3318(3) 0.030 Uani 1 1 d . . . O11 O 0.0400(3) 0.1149(3) 0.8152(3) 0.032 Uani 1 1 d . . . O12 O -0.0980(3) 0.0547(3) 0.8194(3) 0.028 Uani 1 1 d . . . O13 O 0.3865(4) -0.1198(4) 0.7184(4) 0.071 Uani 1 1 d . . . O14 O 0.3517(4) 0.0007(4) 0.7297(4) 0.051 Uani 1 1 d . . . O15 O 0.5125(4) 0.1181(4) 0.7089(4) 0.067 Uani 1 1 d . . . O16 O 0.5049(4) 0.1217(4) 0.8247(4) 0.052 Uani 1 1 d . . . O17 O 0.6122(4) 0.0529(5) 0.7764(5) 0.082 Uani 1 1 d . . . O18 O 0.5320(5) -0.0212(5) 0.8294(4) 0.081 Uani 1 1 d . . . O19 O 0.4015(4) -0.0444(4) 0.6079(4) 0.057 Uani 1 1 d . . . O20 O 0.5045(4) -0.0960(4) 0.6510(4) 0.069 Uani 1 1 d . . . O21 O -0.0106(3) -0.1958(3) 0.4568(3) 0.028 Uani 1 1 d . . . O22 O -0.0554(3) -0.1157(3) 0.5498(3) 0.032 Uani 1 1 d . . . O23 O 0.4995(3) 0.3997(3) 1.1146(3) 0.032 Uani 1 1 d . E . O24 O 0.5157(3) 0.3122(3) 1.1817(3) 0.031 Uani 1 1 d . E . O25 O 0.3146(6) 0.1357(6) 1.2223(6) 0.028 Uiso 0.50 1 d P A 1 O26 O 0.2622(8) 0.0275(8) 1.0839(7) 0.042 Uiso 0.50 1 d P A 1 O27 O 0.2484(9) 0.1531(9) 1.2095(9) 0.069 Uiso 0.50 1 d P B 2 O28 O 0.2305(9) 0.0367(9) 1.0916(9) 0.060 Uiso 0.50 1 d P B 2 O29 O 0.3230(11) 0.3828(11) 1.0229(10) 0.218 Uiso 1 1 d . C 2 O30 O 0.2981(18) 0.281(2) 0.8660(17) 0.396 Uiso 1 1 d . C 2 C1 C 0.1813(5) 0.4926(6) 1.1756(5) 0.047 Uani 1 1 d . . . H1A H 0.2218 0.4846 1.2018 0.070 Uiso 1 1 calc R . . H1B H 0.1841 0.5440 1.2011 0.070 Uiso 1 1 calc R . . H1C H 0.1859 0.4874 1.1321 0.070 Uiso 1 1 calc R . . C2 C 0.1079(6) 0.3614(5) 1.1404(5) 0.049 Uani 1 1 d . . . H2A H 0.1369 0.3554 1.1786 0.058 Uiso 1 1 calc R . . H2B H 0.1307 0.3522 1.1056 0.058 Uiso 1 1 calc R . . C3 C 0.0320(5) 0.3052(5) 1.1119(5) 0.043 Uani 1 1 d . . . H3A H 0.0073 0.2997 1.0661 0.052 Uiso 1 1 calc R . . H3B H 0.0323 0.2550 1.1072 0.052 Uiso 1 1 calc R . . C4 C -0.0732(6) 0.2642(5) 1.1358(5) 0.044 Uani 1 1 d . . . H4A H -0.0985 0.2373 1.0864 0.066 Uiso 1 1 calc R . . H4B H -0.1060 0.2826 1.1565 0.066 Uiso 1 1 calc R . . H4C H -0.0607 0.2291 1.1526 0.066 Uiso 1 1 calc R . . C5 C 0.1068(5) 0.6600(5) 1.3246(5) 0.041 Uani 1 1 d . . . H5A H 0.1356 0.7083 1.3252 0.062 Uiso 1 1 calc R . . H5B H 0.1384 0.6496 1.3571 0.062 Uiso 1 1 calc R . . H5C H 0.0641 0.6639 1.3369 0.062 Uiso 1 1 calc R . . C6 C 0.0366(5) 0.6139(5) 1.2099(4) 0.029 Uani 1 1 d . . . H6A H 0.0617 0.6673 1.2175 0.035 Uiso 1 1 calc R . . H6B H -0.0119 0.6075 1.2154 0.035 Uiso 1 1 calc R . . C7 C 0.0246(5) 0.5609(5) 1.1411(5) 0.032 Uani 1 1 d . . . H7A H -0.0059 0.5715 1.1073 0.038 Uiso 1 1 calc R . . H7B H 0.0729 0.5672 1.1353 0.038 Uiso 1 1 calc R . . C8 C -0.0351(6) 0.4302(5) 1.0633(5) 0.045 Uani 1 1 d . . . H8A H -0.0702 0.4403 1.0333 0.067 Uiso 1 1 calc R . . H8B H -0.0590 0.3785 1.0589 0.067 Uiso 1 1 calc R . . H8C H 0.0089 0.4344 1.0508 0.067 Uiso 1 1 calc R . . C9 C 0.0394(5) 0.5492(5) 1.4040(5) 0.042 Uani 1 1 d . . . H9A H 0.0307 0.5922 1.4326 0.063 Uiso 1 1 calc R . . H9B H 0.0923 0.5658 1.4104 0.063 Uiso 1 1 calc R . . H9C H 0.0249 0.5072 1.4166 0.063 Uiso 1 1 calc R . . C10 C -0.0820(5) 0.5003(5) 1.3244(5) 0.035 Uani 1 1 d . . . H10A H -0.0901 0.5424 1.3560 0.042 Uiso 1 1 calc R . . H10B H -0.0988 0.4553 1.3337 0.042 Uiso 1 1 calc R . . C11 C -0.1239(5) 0.4808(5) 1.2535(5) 0.039 Uani 1 1 d . . . H11A H -0.1780 0.4603 1.2444 0.047 Uiso 1 1 calc R . . H11B H -0.1109 0.5275 1.2462 0.047 Uiso 1 1 calc R . . C12 C -0.1611(5) 0.3901(5) 1.1406(5) 0.043 Uani 1 1 d . . . H12A H -0.2097 0.3616 1.1401 0.065 Uiso 1 1 calc R . . H12B H -0.1465 0.3549 1.1094 0.065 Uiso 1 1 calc R . . H12C H -0.1641 0.4299 1.1263 0.065 Uiso 1 1 calc R . . C13 C 0.2216(5) 0.5630(5) 1.3418(5) 0.040 Uani 1 1 d . . . H13A H 0.2315 0.5961 1.3890 0.060 Uiso 1 1 calc R . . H13B H 0.2156 0.5907 1.3143 0.060 Uiso 1 1 calc R . . H13C H 0.2633 0.5480 1.3393 0.060 Uiso 1 1 calc R . . C14 C 0.1643(5) 0.4554(5) 1.3572(5) 0.033 Uani 1 1 d . . . H14A H 0.1641 0.4839 1.4026 0.039 Uiso 1 1 calc R . . H14B H 0.2124 0.4499 1.3632 0.039 Uiso 1 1 calc R . . C15 C 0.1023(5) 0.3793(5) 1.3221(5) 0.042 Uani 1 1 d . . . H15A H 0.1089 0.3471 1.2815 0.051 Uiso 1 1 calc R . . H15B H 0.1023 0.3539 1.3526 0.051 Uiso 1 1 calc R . . C16 C -0.0255(6) 0.3330(6) 1.3072(5) 0.049 Uani 1 1 d . . . H16A H -0.0291 0.2813 1.2815 0.073 Uiso 1 1 calc R . . H16B H -0.0725 0.3368 1.2885 0.073 Uiso 1 1 calc R . . H16C H -0.0153 0.3435 1.3548 0.073 Uiso 1 1 calc R . . C17 C 0.5659(5) 0.5407(5) 1.4649(5) 0.034 Uani 1 1 d . . . H17A H 0.5207 0.4937 1.4373 0.051 Uiso 1 1 calc R . . H17B H 0.5630 0.5680 1.5088 0.051 Uiso 1 1 calc R . . H17C H 0.6094 0.5278 1.4720 0.051 Uiso 1 1 calc R . . C18 C 0.5879(5) 0.5557(5) 1.3706(5) 0.032 Uani 1 1 d . . . H18A H 0.5436 0.5098 1.3357 0.039 Uiso 1 1 calc R . . H18B H 0.6299 0.5404 1.3811 0.039 Uiso 1 1 calc R . . C19 C 0.6069(5) 0.6142(5) 1.3454(5) 0.034 Uani 1 1 d . . . H19A H 0.6519 0.6596 1.3798 0.041 Uiso 1 1 calc R . . H19B H 0.6171 0.5933 1.3035 0.041 Uiso 1 1 calc R . . C20 C 0.5594(6) 0.6914(6) 1.3072(6) 0.051 Uani 1 1 d . . . H20A H 0.6038 0.7368 1.3409 0.076 Uiso 1 1 calc R . . H20B H 0.5168 0.7055 1.2988 0.076 Uiso 1 1 calc R . . H20C H 0.5680 0.6707 1.2648 0.076 Uiso 1 1 calc R . . C21 C 0.5913(5) 0.7689(5) 1.4823(5) 0.031 Uani 1 1 d . . . C22 C 0.5901(5) 0.8393(5) 1.4893(5) 0.035 Uani 1 1 d . . . H22 H 0.5458 0.8395 1.4635 0.042 Uiso 1 1 calc R . . C23 C 0.6503(6) 0.9103(5) 1.5321(5) 0.044 Uani 1 1 d . . . H23 H 0.6451 0.9562 1.5348 0.053 Uiso 1 1 calc R . . C24 C 0.7166(5) 0.9140(5) 1.5700(5) 0.044 Uani 1 1 d . . . H24 H 0.7574 0.9617 1.5989 0.053 Uiso 1 1 calc R . . C25 C 0.7217(6) 0.8455(6) 1.5646(6) 0.055 Uani 1 1 d . . . H25 H 0.7663 0.8461 1.5908 0.065 Uiso 1 1 calc R . . C26 C 0.6615(5) 0.7759(5) 1.5209(5) 0.042 Uani 1 1 d . . . H26 H 0.6680 0.7302 1.5167 0.050 Uiso 1 1 calc R . . C27 C 0.4576(5) 0.6522(5) 1.5174(5) 0.028 Uani 1 1 d . . . C28 C 0.5152(5) 0.6722(4) 1.5784(4) 0.024 Uani 1 1 d . . . H28 H 0.5651 0.6908 1.5806 0.029 Uiso 1 1 calc R . . C29 C 0.5036(5) 0.6662(5) 1.6352(5) 0.032 Uani 1 1 d . . . H29 H 0.5448 0.6790 1.6738 0.038 Uiso 1 1 calc R . . C30 C 0.4330(5) 0.6421(5) 1.6357(5) 0.036 Uani 1 1 d . . . H30 H 0.4249 0.6384 1.6744 0.043 Uiso 1 1 calc R . . C31 C 0.3741(5) 0.6233(5) 1.5792(5) 0.029 Uani 1 1 d . . . H31 H 0.3248 0.6076 1.5790 0.035 Uiso 1 1 calc R . . C32 C 0.3873(5) 0.6275(5) 1.5224(5) 0.031 Uani 1 1 d . . . H32 H 0.3451 0.6122 1.4837 0.037 Uiso 1 1 calc R . . C33 C 0.3972(5) 0.6866(5) 1.3574(5) 0.028 Uani 1 1 d . . . C34 C 0.3670(5) 0.7331(5) 1.3930(5) 0.027 Uani 1 1 d . . . H34 H 0.3838 0.7514 1.4408 0.033 Uiso 1 1 calc R . . C35 C 0.3146(5) 0.7540(5) 1.3631(5) 0.031 Uani 1 1 d . . . H35 H 0.2966 0.7867 1.3900 0.038 Uiso 1 1 calc R . . C36 C 0.2876(5) 0.7270(5) 1.2926(5) 0.031 Uani 1 1 d . . . H36 H 0.2511 0.7410 1.2713 0.037 Uiso 1 1 calc R . . C37 C 0.3145(5) 0.6799(5) 1.2548(5) 0.032 Uani 1 1 d . . . H37 H 0.2969 0.6611 1.2069 0.038 Uiso 1 1 calc R . . C38 C 0.3666(5) 0.6600(5) 1.2860(5) 0.033 Uani 1 1 d . . . H38 H 0.3834 0.6264 1.2585 0.039 Uiso 1 1 calc R . . C39 C 0.3977(4) 0.5101(5) 1.3438(4) 0.025 Uani 1 1 d . . . C40 C 0.3702(5) 0.4744(5) 1.2728(5) 0.030 Uani 1 1 d . . . H40 H 0.3885 0.5028 1.2500 0.036 Uiso 1 1 calc R . . C41 C 0.3171(5) 0.3990(5) 1.2336(5) 0.040 Uani 1 1 d . . . H41 H 0.3011 0.3770 1.1855 0.049 Uiso 1 1 calc R . . C42 C 0.2889(5) 0.3580(6) 1.2646(5) 0.042 Uani 1 1 d . . . H42 H 0.2525 0.3072 1.2380 0.051 Uiso 1 1 calc R . . C43 C 0.3119(5) 0.3883(5) 1.3335(5) 0.039 Uani 1 1 d . . . H43 H 0.2923 0.3593 1.3553 0.046 Uiso 1 1 calc R . . C44 C 0.3654(5) 0.4636(5) 1.3710(5) 0.036 Uani 1 1 d . . . H44 H 0.3808 0.4845 1.4190 0.043 Uiso 1 1 calc R . . C45 C 0.1187(5) 0.1450(5) 0.8420(5) 0.041 Uani 1 1 d . . . H45A H 0.1355 0.1433 0.8856 0.062 Uiso 1 1 calc R . . H45B H 0.1387 0.1981 0.8486 0.062 Uiso 1 1 calc R . . H45C H 0.1363 0.1144 0.8103 0.062 Uiso 1 1 calc R . . C46 C 0.0097(5) 0.0369(5) 0.8065(5) 0.040 Uani 1 1 d . . . H46A H 0.0246 0.0355 0.8509 0.048 Uiso 1 1 calc R . . H46B H 0.0286 0.0051 0.7766 0.048 Uiso 1 1 calc R . . C47 C -0.0720(5) 0.0074(5) 0.7761(5) 0.037 Uani 1 1 d . . . H47A H -0.0867 0.0073 0.7311 0.044 Uiso 1 1 calc R . . H47B H -0.0946 -0.0459 0.7699 0.044 Uiso 1 1 calc R . . C48 C -0.1769(5) 0.0241(6) 0.7990(5) 0.047 Uani 1 1 d . . . H48A H -0.1994 0.0123 0.7513 0.070 Uiso 1 1 calc R . . H48B H -0.1919 0.0617 0.8269 0.070 Uiso 1 1 calc R . . H48C H -0.1937 -0.0228 0.8048 0.070 Uiso 1 1 calc R . . C49 C 0.0343(5) 0.1719(5) 0.9630(4) 0.027 Uani 1 1 d . . . C50 C -0.0048(5) 0.1142(5) 0.9786(4) 0.028 Uani 1 1 d . . . H50 H -0.0554 0.0823 0.9505 0.033 Uiso 1 1 calc R . . C51 C 0.0272(6) 0.1017(6) 1.0333(5) 0.042 Uani 1 1 d . . . H51 H -0.0020 0.0633 1.0425 0.050 Uiso 1 1 calc R . . C52 C 0.0988(6) 0.1435(6) 1.0725(5) 0.045 Uani 1 1 d . . . H52 H 0.1208 0.1342 1.1091 0.054 Uiso 1 1 calc R . . C53 C 0.1409(6) 0.2000(6) 1.0598(5) 0.046 Uani 1 1 d . . . H53 H 0.1918 0.2301 1.0879 0.055 Uiso 1 1 calc R . . C54 C 0.1089(5) 0.2129(5) 1.0065(4) 0.028 Uani 1 1 d . . . H54 H 0.1393 0.2520 0.9987 0.034 Uiso 1 1 calc R . . C55 C 0.0718(4) 0.3137(4) 0.8970(4) 0.034 Uani 1 1 d D . . C56A C 0.0960(11) 0.3217(7) 0.8453(6) 0.044 Uani 0.50 1 d PDU D 1 H56 H 0.0784 0.2790 0.8025 0.053 Uiso 0.50 1 calc PR D 1 C56B C 0.1064(11) 0.3447(6) 0.8600(6) 0.032 Uani 0.50 1 d PDU D 2 H56' H 0.0999 0.3121 0.8153 0.038 Uiso 0.50 1 calc PR D 2 C57A C 0.1460(9) 0.3929(8) 0.8574(7) 0.043 Uani 0.50 1 d PDU D 1 H57 H 0.1605 0.3998 0.8221 0.051 Uiso 0.50 1 calc PR D 1 C57B C 0.1500(10) 0.4224(7) 0.8874(8) 0.039 Uani 0.50 1 d PDU D 2 H57' H 0.1747 0.4419 0.8621 0.047 Uiso 0.50 1 calc PR D 2 C58A C 0.1744(8) 0.4536(7) 0.9216(7) 0.032 Uani 0.50 1 d PDU D 1 H58 H 0.2088 0.5020 0.9301 0.038 Uiso 0.50 1 calc PR D 1 C58B C 0.1579(9) 0.4719(6) 0.9514(7) 0.037 Uani 0.50 1 d PDU D 2 H58' H 0.1864 0.5252 0.9694 0.044 Uiso 0.50 1 calc PR D 2 C59A C 0.1531(9) 0.4443(6) 0.9736(6) 0.053 Uani 0.50 1 d PDU D 1 H59 H 0.1750 0.4851 1.0181 0.064 Uiso 0.50 1 calc PR D 1 C59B C 0.1234(10) 0.4424(6) 0.9889(6) 0.051 Uani 0.50 1 d PDU D 2 H59' H 0.1280 0.4758 1.0326 0.061 Uiso 0.50 1 calc PR D 2 C60A C 0.0992(12) 0.3746(7) 0.9600(6) 0.047 Uani 0.50 1 d PDU D 1 H60 H 0.0814 0.3691 0.9942 0.056 Uiso 0.50 1 calc PR D 1 C60B C 0.0824(13) 0.3642(7) 0.9627(7) 0.045 Uani 0.50 1 d PDU D 2 H60B H 0.0611 0.3444 0.9896 0.054 Uiso 0.50 1 calc PR D 2 C61 C -0.1177(4) 0.2255(4) 0.9062(4) 0.022 Uani 1 1 d . . . C62 C -0.1454(5) 0.2747(5) 0.8887(5) 0.038 Uani 1 1 d . D . H62 H -0.1254 0.2962 0.8622 0.046 Uiso 1 1 calc R . . C63 C -0.2012(6) 0.2939(6) 0.9080(5) 0.048 Uani 1 1 d . . . H63 H -0.2186 0.3271 0.8942 0.058 Uiso 1 1 calc R D . C64 C -0.2301(5) 0.2644(6) 0.9467(5) 0.048 Uani 1 1 d . D . H64 H -0.2681 0.2768 0.9601 0.057 Uiso 1 1 calc R . . C65 C -0.2044(5) 0.2175(6) 0.9661(5) 0.041 Uani 1 1 d . . . H65 H -0.2239 0.1972 0.9936 0.050 Uiso 1 1 calc R D . C66 C -0.1496(5) 0.1990(5) 0.9458(5) 0.033 Uani 1 1 d . D . H66 H -0.1330 0.1657 0.9601 0.039 Uiso 1 1 calc R . . C67 C -0.0903(5) 0.1621(5) 0.7474(4) 0.024 Uani 1 1 d . . . C68 C -0.1635(5) 0.1526(5) 0.7236(4) 0.024 Uani 1 1 d . D . H68 H -0.1866 0.1637 0.7560 0.029 Uiso 1 1 calc R . . C69 C -0.2062(5) 0.1283(5) 0.6568(5) 0.029 Uani 1 1 d . . . H69 H -0.2570 0.1213 0.6444 0.035 Uiso 1 1 calc R D . C70 C -0.1742(5) 0.1141(5) 0.6080(4) 0.027 Uani 1 1 d . D . H70 H -0.2024 0.0987 0.5620 0.032 Uiso 1 1 calc R . . C71 C -0.1010(5) 0.1226(5) 0.6274(5) 0.036 Uani 1 1 d . . . H71 H -0.0783 0.1124 0.5947 0.043 Uiso 1 1 calc R D . C72 C -0.0607(5) 0.1463(5) 0.6955(5) 0.037 Uani 1 1 d . D . H72 H -0.0102 0.1523 0.7077 0.044 Uiso 1 1 calc R . . C73 C 0.3967(7) -0.1903(6) 0.6966(6) 0.075 Uani 1 1 d . . . H73A H 0.4001 -0.2073 0.7324 0.113 Uiso 1 1 calc R . . H73B H 0.4427 -0.1822 0.6870 0.113 Uiso 1 1 calc R . . H73C H 0.3543 -0.2294 0.6555 0.113 Uiso 1 1 calc R . . C74 C 0.3065(6) -0.1299(8) 0.6924(8) 0.092 Uani 1 1 d . . . H74A H 0.2904 -0.1439 0.6433 0.110 Uiso 1 1 calc R . . H74B H 0.2747 -0.1724 0.6985 0.110 Uiso 1 1 calc R . . C75 C 0.2964(7) -0.0630(7) 0.7261(9) 0.107 Uani 1 1 d . . . H75A H 0.2466 -0.0676 0.7014 0.128 Uiso 1 1 calc R . . H75B H 0.2994 -0.0561 0.7724 0.128 Uiso 1 1 calc R . . C76 C 0.3320(6) 0.0651(7) 0.7497(6) 0.077 Uani 1 1 d . . . H76A H 0.2887 0.0565 0.7130 0.115 Uiso 1 1 calc R . . H76B H 0.3740 0.1113 0.7594 0.115 Uiso 1 1 calc R . . H76C H 0.3199 0.0716 0.7905 0.115 Uiso 1 1 calc R . . C77 C 0.5012(10) 0.1214(9) 0.6480(7) 0.145 Uani 1 1 d . . . H77A H 0.4516 0.1208 0.6308 0.218 Uiso 1 1 calc R . . H77B H 0.5048 0.0771 0.6155 0.218 Uiso 1 1 calc R . . H77C H 0.5390 0.1685 0.6541 0.218 Uiso 1 1 calc R . . C78 C 0.5314(7) 0.1909(6) 0.7646(6) 0.075 Uani 1 1 d . . . H78A H 0.4867 0.2026 0.7621 0.090 Uiso 1 1 calc R . . H78B H 0.5695 0.2320 0.7618 0.090 Uiso 1 1 calc R . . C79 C 0.5611(7) 0.1872(6) 0.8309(6) 0.068 Uani 1 1 d . . . H79A H 0.6090 0.1813 0.8367 0.082 Uiso 1 1 calc R . . H79B H 0.5684 0.2338 0.8699 0.082 Uiso 1 1 calc R . . C80 C 0.4862(8) 0.1345(7) 0.8807(6) 0.078 Uani 1 1 d . . . H80A H 0.5313 0.1575 0.9211 0.117 Uiso 1 1 calc R . . H80B H 0.4530 0.0859 0.8766 0.117 Uiso 1 1 calc R . . H80C H 0.4607 0.1695 0.8846 0.117 Uiso 1 1 calc R . . C81 C 0.6575(8) 0.0815(8) 0.7458(10) 0.118 Uani 1 1 d . . . H81A H 0.6957 0.1322 0.7787 0.176 Uiso 1 1 calc R . . H81B H 0.6275 0.0856 0.7074 0.176 Uiso 1 1 calc R . . H81C H 0.6816 0.0469 0.7295 0.176 Uiso 1 1 calc R . . C82 C 0.6513(7) 0.0389(8) 0.8313(8) 0.128 Uani 1 1 d . . . H82A H 0.6599 -0.0083 0.8122 0.154 Uiso 1 1 calc R . . H82B H 0.7001 0.0822 0.8601 0.154 Uiso 1 1 calc R . . C83 C 0.6064(7) 0.0309(9) 0.8698(7) 0.101 Uani 1 1 d . . . H83A H 0.6070 0.0816 0.8961 0.122 Uiso 1 1 calc R . . H83B H 0.6276 0.0132 0.9024 0.122 Uiso 1 1 calc R . . C84 C 0.4927(11) -0.0441(9) 0.8668(7) 0.131 Uani 1 1 d . . . H84A H 0.5156 -0.0713 0.8875 0.197 Uiso 1 1 calc R . . H84B H 0.4411 -0.0781 0.8369 0.197 Uiso 1 1 calc R . . H84C H 0.4938 0.0010 0.9024 0.197 Uiso 1 1 calc R . . C85 C 0.3384(6) -0.0311(8) 0.5846(6) 0.075 Uani 1 1 d . . . H85A H 0.3328 -0.0320 0.5400 0.113 Uiso 1 1 calc R . . H85B H 0.3440 0.0190 0.6165 0.113 Uiso 1 1 calc R . . H85C H 0.2943 -0.0711 0.5808 0.113 Uiso 1 1 calc R . . C86 C 0.4006(7) -0.1120(8) 0.5612(7) 0.093 Uani 1 1 d . . . H86A H 0.3902 -0.1119 0.5162 0.111 Uiso 1 1 calc R . . H86B H 0.3600 -0.1566 0.5571 0.111 Uiso 1 1 calc R . . C87 C 0.4705(9) -0.1198(12) 0.5814(7) 0.179 Uani 1 1 d . . . H87A H 0.4618 -0.1742 0.5570 0.214 Uiso 1 1 calc R . . H87B H 0.5056 -0.0898 0.5667 0.214 Uiso 1 1 calc R . . C88 C 0.5631(7) -0.1198(6) 0.6676(6) 0.075 Uani 1 1 d . . . H88A H 0.5435 -0.1758 0.6460 0.112 Uiso 1 1 calc R . . H88B H 0.5846 -0.1007 0.7168 0.112 Uiso 1 1 calc R . . H88C H 0.6016 -0.0993 0.6513 0.112 Uiso 1 1 calc R . . C89 C -0.0231(5) -0.2689(5) 0.4045(5) 0.041 Uani 1 1 d . . . H89A H -0.0722 -0.3067 0.3945 0.062 Uiso 1 1 calc R . . H89B H 0.0154 -0.2859 0.4203 0.062 Uiso 1 1 calc R . . H89C H -0.0212 -0.2634 0.3634 0.062 Uiso 1 1 calc R . . C90 C -0.0686(6) -0.1710(6) 0.4373(5) 0.051 Uani 1 1 d . . . H90A H -0.1178 -0.2108 0.4258 0.062 Uiso 1 1 calc R . . H90B H -0.0683 -0.1618 0.3970 0.062 Uiso 1 1 calc R . . C91 C -0.0553(6) -0.1000(5) 0.4945(5) 0.044 Uani 1 1 d . . . H91A H -0.0068 -0.0597 0.5053 0.053 Uiso 1 1 calc R . . H91B H -0.0949 -0.0818 0.4829 0.053 Uiso 1 1 calc R . . C92 C -0.0643(5) -0.0574(5) 0.6017(5) 0.041 Uani 1 1 d . . . H92A H -0.0260 -0.0073 0.6144 0.062 Uiso 1 1 calc R . . H92B H -0.0592 -0.0677 0.6415 0.062 Uiso 1 1 calc R . . H92C H -0.1136 -0.0575 0.5846 0.062 Uiso 1 1 calc R . . C93 C -0.0788(5) -0.2906(5) 0.5320(5) 0.029 Uani 1 1 d . . . C94 C -0.0794(5) -0.3655(5) 0.5125(4) 0.028 Uani 1 1 d . . . H94 H -0.0351 -0.3717 0.5096 0.034 Uiso 1 1 calc R . . C95 C -0.1400(5) -0.4292(5) 0.4977(5) 0.035 Uani 1 1 d . . . H95 H -0.1363 -0.4773 0.4859 0.043 Uiso 1 1 calc R . . C96 C -0.2059(5) -0.4240(5) 0.4998(5) 0.035 Uani 1 1 d . . . H96 H -0.2479 -0.4678 0.4898 0.043 Uiso 1 1 calc R . . C97 C -0.2095(5) -0.3532(5) 0.5168(5) 0.041 Uani 1 1 d . . . H97 H -0.2547 -0.3485 0.5184 0.050 Uiso 1 1 calc R . . C98 C -0.1479(5) -0.2887(5) 0.5318(5) 0.037 Uani 1 1 d . . . H98 H -0.1529 -0.2414 0.5423 0.044 Uiso 1 1 calc R . . C99 C 0.0354(5) -0.1439(5) 0.6895(5) 0.035 Uani 1 1 d . . . C100 C -0.0255(6) -0.1687(5) 0.7075(5) 0.039 Uani 1 1 d . . . H100 H -0.0734 -0.1977 0.6726 0.047 Uiso 1 1 calc R . . C101 C -0.0201(7) -0.1533(6) 0.7736(6) 0.051 Uani 1 1 d . . . H101 H -0.0636 -0.1730 0.7823 0.061 Uiso 1 1 calc R . . C102 C 0.0464(7) -0.1106(6) 0.8260(6) 0.054 Uani 1 1 d . . . H102 H 0.0495 -0.0995 0.8713 0.065 Uiso 1 1 calc R . . C103 C 0.1085(7) -0.0841(7) 0.8123(6) 0.061 Uani 1 1 d . . . H103 H 0.1559 -0.0547 0.8479 0.074 Uiso 1 1 calc R . . C104 C 0.1015(6) -0.1009(6) 0.7446(5) 0.047 Uani 1 1 d . . . H104 H 0.1454 -0.0813 0.7363 0.056 Uiso 1 1 calc R . . C105 C 0.1196(5) -0.0414(5) 0.6052(4) 0.024 Uani 1 1 d . . . C106 C 0.1274(5) 0.0249(5) 0.6572(5) 0.037 Uani 1 1 d . . . H106 H 0.1012 0.0189 0.6863 0.044 Uiso 1 1 calc R . . C107 C 0.1688(6) 0.0973(6) 0.6702(5) 0.051 Uani 1 1 d . . . H107 H 0.1696 0.1396 0.7062 0.062 Uiso 1 1 calc R . . C108 C 0.2099(5) 0.1089(6) 0.6305(5) 0.043 Uani 1 1 d . . . H108 H 0.2409 0.1593 0.6401 0.052 Uiso 1 1 calc R . . C109 C 0.2054(5) 0.0474(6) 0.5776(5) 0.040 Uani 1 1 d . . . H109 H 0.2320 0.0538 0.5488 0.048 Uiso 1 1 calc R . . C110 C 0.1612(5) -0.0241(5) 0.5671(5) 0.034 Uani 1 1 d . . . H110 H 0.1588 -0.0662 0.5300 0.041 Uiso 1 1 calc R . . C111 C 0.1193(4) -0.2325(5) 0.5566(4) 0.026 Uani 1 1 d . . . C112 C 0.1595(4) -0.2278(5) 0.5138(4) 0.026 Uani 1 1 d . . . H112 H 0.1540 -0.1972 0.4908 0.031 Uiso 1 1 calc R . . C113 C 0.2067(5) -0.2649(5) 0.5032(5) 0.036 Uani 1 1 d . . . H113 H 0.2330 -0.2591 0.4741 0.043 Uiso 1 1 calc R . . C114 C 0.2149(5) -0.3104(6) 0.5353(6) 0.054 Uani 1 1 d . . . H114 H 0.2468 -0.3365 0.5285 0.064 Uiso 1 1 calc R . . C115 C 0.1771(6) -0.3175(6) 0.5766(6) 0.049 Uani 1 1 d . . . H115 H 0.1822 -0.3487 0.5991 0.059 Uiso 1 1 calc R . . C116 C 0.1310(5) -0.2789(5) 0.5859(5) 0.039 Uani 1 1 d . . . H116 H 0.1053 -0.2851 0.6152 0.047 Uiso 1 1 calc R . . C117 C 0.5203(5) 0.4708(5) 1.1073(6) 0.048 Uani 1 1 d . . . H11C H 0.4771 0.4840 1.0988 0.072 Uiso 1 1 calc R E . H11D H 0.5374 0.4639 1.0691 0.072 Uiso 1 1 calc R . . H11E H 0.5605 0.5120 1.1489 0.072 Uiso 1 1 calc R . . C118 C 0.4796(6) 0.4094(6) 1.1724(5) 0.049 Uani 1 1 d . . . H11F H 0.4392 0.4281 1.1694 0.058 Uiso 1 1 calc R E . H11G H 0.5230 0.4477 1.2139 0.058 Uiso 1 1 calc R . . C119 C 0.4542(5) 0.3351(6) 1.1759(5) 0.041 Uani 1 1 d . E . H11H H 0.4393 0.3408 1.2156 0.049 Uiso 1 1 calc R . . H11I H 0.4109 0.2963 1.1344 0.049 Uiso 1 1 calc R . . C120 C 0.4964(6) 0.2407(5) 1.1870(5) 0.047 Uani 1 1 d . . . H12D H 0.4887 0.2482 1.2297 0.070 Uiso 1 1 calc R E . H12E H 0.5368 0.2232 1.1858 0.070 Uiso 1 1 calc R . . H12F H 0.4506 0.2022 1.1490 0.070 Uiso 1 1 calc R . . C121 C 0.6676(10) 0.4368(6) 1.2047(5) 0.028 Uani 0.50 1 d PDU E 1 C122 C 0.6793(8) 0.4327(6) 1.2664(6) 0.025 Uani 0.50 1 d PDU E 1 H122 H 0.6528 0.3863 1.2673 0.030 Uiso 0.50 1 calc PR E 1 C123 C 0.7291(7) 0.4953(7) 1.3263(5) 0.020 Uani 0.50 1 d PDU E 1 H123 H 0.7403 0.4905 1.3674 0.024 Uiso 0.50 1 calc PR E 1 C124 C 0.7630(8) 0.5657(6) 1.3263(5) 0.021 Uani 0.50 1 d PDU E 1 H124 H 0.7930 0.6099 1.3679 0.025 Uiso 0.50 1 calc PR E 1 C125 C 0.7526(9) 0.5708(6) 1.2655(6) 0.032 Uani 0.50 1 d PDU E 1 H125 H 0.7784 0.6177 1.2650 0.038 Uiso 0.50 1 calc PR E 1 C126 C 0.7042(9) 0.5070(7) 1.2051(5) 0.025 Uani 0.50 1 d PDU E 1 H126 H 0.6960 0.5111 1.1636 0.030 Uiso 0.50 1 calc PR E 1 C127 C 0.6520(5) 0.2536(5) 1.1230(5) 0.037 Uani 1 1 d . E . C128 C 0.7005(5) 0.2714(7) 1.1867(6) 0.055 Uani 1 1 d . . . H128 H 0.7038 0.3128 1.2250 0.066 Uiso 1 1 calc R E . C129 C 0.7439(6) 0.2317(8) 1.1968(8) 0.080 Uani 1 1 d . E . H129 H 0.7745 0.2449 1.2414 0.095 Uiso 1 1 calc R . . C130 C 0.7432(8) 0.1753(9) 1.1446(10) 0.100 Uani 1 1 d . . . H130 H 0.7738 0.1488 1.1524 0.120 Uiso 1 1 calc R E . C131 C 0.6985(7) 0.1542(7) 1.0788(8) 0.075 Uani 1 1 d . E . H131 H 0.6980 0.1139 1.0412 0.090 Uiso 1 1 calc R . . C132 C 0.6541(6) 0.1945(6) 1.0699(6) 0.051 Uani 1 1 d . . . H132 H 0.6236 0.1808 1.0251 0.061 Uiso 1 1 calc R E . C133 C 0.5868(5) 0.3499(5) 1.0049(5) 0.032 Uani 1 1 d . E . C134 C 0.6526(5) 0.3742(5) 0.9936(5) 0.040 Uani 1 1 d . . . H134 H 0.6966 0.3793 1.0248 0.048 Uiso 1 1 calc R E . C135 C 0.6592(6) 0.3919(5) 0.9402(5) 0.045 Uani 1 1 d . E . H135 H 0.7062 0.4075 0.9355 0.054 Uiso 1 1 calc R . . C136 C 0.5980(6) 0.3866(5) 0.8948(5) 0.045 Uani 1 1 d . . . H136 H 0.6016 0.3988 0.8583 0.055 Uiso 1 1 calc R E . C137 C 0.5317(6) 0.3636(6) 0.9025(5) 0.045 Uani 1 1 d . E . H137 H 0.4887 0.3601 0.8712 0.053 Uiso 1 1 calc R . . C138 C 0.5252(6) 0.3449(6) 0.9559(5) 0.041 Uani 1 1 d . . . H138 H 0.4776 0.3282 0.9591 0.050 Uiso 1 1 calc R E . C139 C 0.4581(6) 0.2091(5) 1.0273(5) 0.042 Uani 1 1 d . E . C140 C 0.4521(7) 0.1348(7) 1.0147(5) 0.064 Uani 1 1 d . . . H140 H 0.4946 0.1286 1.0367 0.077 Uiso 1 1 calc R E . C141 C 0.3870(9) 0.0689(7) 0.9715(7) 0.100 Uani 1 1 d . E . H141 H 0.3852 0.0192 0.9636 0.120 Uiso 1 1 calc R . . C142 C 0.3254(9) 0.0794(10) 0.9409(7) 0.121 Uani 1 1 d . . . H142 H 0.2801 0.0361 0.9123 0.145 Uiso 1 1 calc R E . C143 C 0.3283(7) 0.1491(10) 0.9507(7) 0.105 Uani 1 1 d . E . H143 H 0.2862 0.1548 0.9274 0.125 Uiso 1 1 calc R . . C144 C 0.3922(5) 0.2121(7) 0.9944(6) 0.060 Uani 1 1 d . . . H144 H 0.3916 0.2610 1.0028 0.072 Uiso 1 1 calc R E . C145 C 0.3031(14) 0.1758(16) 1.2772(15) 0.063 Uiso 0.50 1 d P A 1 H14E H 0.3177 0.1597 1.3126 0.094 Uiso 0.50 1 calc PR A 1 H14F H 0.2503 0.1666 1.2651 0.094 Uiso 0.50 1 calc PR A 1 H14G H 0.3329 0.2305 1.2939 0.094 Uiso 0.50 1 calc PR A 1 C146 C 0.2957(7) 0.1560(7) 1.1749(6) 0.063 Uiso 0.50 1 d P A 1 H14H H 0.3281 0.2102 1.1900 0.076 Uiso 0.50 1 calc PR A 1 H14I H 0.2436 0.1513 1.1651 0.076 Uiso 0.50 1 calc PR A 1 C14A C 0.2957(7) 0.1560(7) 1.1749(6) 0.063 Uiso 0.50 1 d P B 2 H14C H 0.3175 0.2096 1.1818 0.076 Uiso 0.50 1 calc PR B 2 H14D H 0.3370 0.1457 1.1978 0.076 Uiso 0.50 1 calc PR B 2 C147 C 0.3030(16) 0.1062(17) 1.1122(17) 0.086 Uiso 0.50 1 d P A 1 H14J H 0.2887 0.1236 1.0771 0.103 Uiso 0.50 1 calc PR A 1 H14K H 0.3562 0.1154 1.1226 0.103 Uiso 0.50 1 calc PR A 1 C148 C 0.2024(7) -0.0069(7) 1.0224(7) 0.070 Uiso 0.50 1 d P A 1 H14L H 0.1756 -0.0608 1.0112 0.106 Uiso 0.50 1 calc PR A 1 H14M H 0.2209 -0.0035 0.9866 0.106 Uiso 0.50 1 calc PR A 1 H14N H 0.1687 0.0195 1.0263 0.106 Uiso 0.50 1 calc PR A 1 C14B C 0.2024(7) -0.0069(7) 1.0224(7) 0.070 Uiso 0.50 1 d P B 2 H14R H 0.1714 -0.0596 1.0115 0.106 Uiso 0.50 1 calc PR B 2 H14S H 0.2436 -0.0064 1.0062 0.106 Uiso 0.50 1 calc PR B 2 H14T H 0.1722 0.0143 1.0005 0.106 Uiso 0.50 1 calc PR B 2 C149 C 0.2778(15) 0.1832(17) 1.2829(15) 0.071 Uiso 0.50 1 d P B 2 H14O H 0.2365 0.1761 1.2993 0.107 Uiso 0.50 1 calc PR B 2 H14P H 0.3096 0.2379 1.3030 0.107 Uiso 0.50 1 calc PR B 2 H14Q H 0.3071 0.1559 1.2958 0.107 Uiso 0.50 1 calc PR B 2 C150 C 0.2734(11) 0.1123(12) 1.1096(11) 0.033 Uiso 0.50 1 d P B 2 H15C H 0.3175 0.1150 1.0967 0.040 Uiso 0.50 1 calc PR B 2 H15D H 0.2441 0.1321 1.0842 0.040 Uiso 0.50 1 calc PR B 2 C158 C 0.6687(10) 0.4514(7) 1.1942(6) 0.027 Uani 0.50 1 d PDU E 2 C159 C 0.6864(9) 0.4642(7) 1.2619(7) 0.031 Uani 0.50 1 d PDU E 2 H159 H 0.6638 0.4241 1.2727 0.038 Uiso 0.50 1 calc PR E 2 C160 C 0.7368(12) 0.5351(9) 1.3135(6) 0.068 Uani 0.50 1 d PDU E 2 H160 H 0.7505 0.5428 1.3593 0.082 Uiso 0.50 1 calc PR E 2 C161 C 0.7672(10) 0.5950(7) 1.2982(7) 0.044 Uani 0.50 1 d PDU E 2 H158 H 0.8011 0.6438 1.3336 0.053 Uiso 0.50 1 calc PR E 2 C162 C 0.7483(11) 0.5837(8) 1.2314(8) 0.064 Uani 0.50 1 d PDU E 2 H16D H 0.7681 0.6251 1.2211 0.077 Uiso 0.50 1 calc PR E 2 C163 C 0.7003(11) 0.5119(8) 1.1794(6) 0.041 Uani 0.50 1 d PDU E 2 H163 H 0.6888 0.5038 1.1336 0.050 Uiso 0.50 1 calc PR E 2 C151 C 0.2863(14) 0.3912(15) 1.0621(13) 0.233 Uiso 1 1 d . . . H15J H 0.3077 0.4448 1.0959 0.349 Uiso 1 1 calc R C 2 H15K H 0.2888 0.3584 1.0852 0.349 Uiso 1 1 calc R C 2 H15L H 0.2342 0.3767 1.0355 0.349 Uiso 1 1 calc R C 2 C152 C 0.3266(19) 0.3955(18) 0.9722(18) 0.276 Uiso 1 1 d . . . H15M H 0.3728 0.4426 0.9932 0.331 Uiso 1 1 calc R C 2 H15N H 0.2859 0.4130 0.9635 0.331 Uiso 1 1 calc R C 2 C153 C 0.3263(11) 0.3577(12) 0.9032(11) 0.139 Uiso 1 1 d . C . H15E H 0.2999 0.3775 0.8754 0.167 Uiso 1 1 calc R F 2 H15F H 0.3788 0.3772 0.9067 0.167 Uiso 1 1 calc R F 2 C154 C 0.325(2) 0.272(2) 0.8076(18) 0.372 Uiso 1 1 d . . . H15G H 0.3161 0.2186 0.7821 0.558 Uiso 1 1 calc R C 2 H15H H 0.3787 0.3039 0.8254 0.558 Uiso 1 1 calc R C 2 H15I H 0.2985 0.2891 0.7776 0.558 Uiso 1 1 calc R C 2 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 0.019 0.020 0.023 0.008 0.005 0.009 Yb2 0.021 0.021 0.023 0.010 0.007 0.011 Yb3 0.024 0.022 0.023 0.011 0.010 0.011 Yb4 0.021 0.021 0.026 0.008 0.004 0.007 Yb5 0.023 0.026 0.027 0.011 0.012 0.014 Yb6 0.021 0.030 0.022 0.007 0.004 0.010 O1 0.027 0.038 0.036 0.000 0.014 0.012 O2 0.036 0.021 0.035 0.007 0.011 0.013 O3 0.026 0.022 0.025 0.010 0.002 0.012 O4 0.033 0.021 0.018 0.006 0.001 0.004 O5 0.020 0.039 0.031 0.008 0.008 0.016 O6 0.019 0.028 0.031 0.010 0.001 0.009 O7 0.016 0.024 0.021 0.009 -0.004 0.001 O8 0.023 0.034 0.038 0.027 0.013 0.011 O9 0.032 0.025 0.019 0.012 0.011 0.016 O10 0.038 0.039 0.037 0.031 0.026 0.020 O11 0.031 0.045 0.033 0.020 0.016 0.026 O12 0.029 0.025 0.030 0.012 0.010 0.010 O13 0.056 0.065 0.089 0.050 0.017 0.009 O14 0.035 0.058 0.070 0.026 0.027 0.027 O15 0.080 0.050 0.049 0.022 0.015 0.003 O16 0.064 0.029 0.050 0.003 0.025 0.013 O17 0.033 0.073 0.109 0.015 0.019 0.014 O18 0.112 0.074 0.038 0.022 -0.002 0.039 O19 0.046 0.076 0.034 0.012 -0.001 0.031 O20 0.053 0.071 0.056 0.001 -0.004 0.040 O21 0.027 0.029 0.026 0.010 0.004 0.015 O22 0.033 0.025 0.043 0.012 0.014 0.021 O23 0.031 0.025 0.038 0.010 0.010 0.013 O24 0.031 0.036 0.023 0.011 0.007 0.013 C1 0.020 0.048 0.042 0.004 0.002 0.000 C2 0.059 0.052 0.041 0.012 0.019 0.040 C3 0.029 0.042 0.033 -0.005 0.002 0.015 C4 0.064 0.017 0.039 0.012 0.012 0.004 C5 0.048 0.030 0.026 -0.002 0.004 0.013 C6 0.031 0.020 0.040 0.019 0.006 0.013 C7 0.036 0.024 0.039 0.023 0.011 0.009 C8 0.062 0.028 0.030 0.011 -0.002 0.016 C9 0.045 0.040 0.031 0.003 0.013 0.020 C10 0.024 0.039 0.041 0.013 0.020 0.012 C11 0.026 0.030 0.050 0.007 0.011 0.013 C12 0.025 0.044 0.043 0.016 -0.002 0.005 C13 0.027 0.041 0.041 0.017 0.005 0.007 C14 0.029 0.035 0.044 0.027 0.014 0.015 C15 0.045 0.037 0.053 0.030 0.012 0.021 C16 0.051 0.046 0.051 0.030 0.020 0.010 C17 0.037 0.036 0.044 0.022 0.020 0.024 C18 0.040 0.034 0.034 0.019 0.017 0.022 C19 0.034 0.045 0.042 0.022 0.030 0.025 C20 0.045 0.065 0.061 0.046 0.024 0.021 C21 0.040 0.026 0.037 0.016 0.023 0.017 C22 0.033 0.031 0.032 0.010 0.005 0.010 C23 0.065 0.025 0.048 0.020 0.030 0.015 C24 0.037 0.027 0.051 0.010 0.012 -0.001 C25 0.035 0.038 0.068 0.012 0.010 0.005 C26 0.040 0.029 0.063 0.025 0.019 0.016 C27 0.033 0.026 0.028 0.015 0.007 0.016 C28 0.018 0.014 0.036 0.008 0.008 0.004 C29 0.033 0.029 0.026 0.010 0.006 0.008 C30 0.045 0.035 0.030 0.009 0.022 0.020 C31 0.025 0.028 0.032 0.008 0.014 0.010 C32 0.021 0.029 0.037 0.010 0.002 0.015 C33 0.022 0.035 0.043 0.028 0.016 0.017 C34 0.031 0.025 0.029 0.016 0.010 0.012 C35 0.026 0.023 0.040 0.008 0.011 0.013 C36 0.027 0.034 0.038 0.025 0.003 0.018 C37 0.039 0.037 0.027 0.019 0.014 0.019 C38 0.044 0.030 0.040 0.019 0.023 0.025 C39 0.017 0.029 0.027 0.008 0.003 0.015 C40 0.031 0.028 0.037 0.015 0.016 0.017 C41 0.049 0.038 0.025 0.002 0.008 0.023 C42 0.028 0.049 0.035 0.000 -0.001 0.026 C43 0.034 0.029 0.060 0.021 0.021 0.017 C44 0.038 0.038 0.037 0.013 0.017 0.023 C45 0.032 0.049 0.052 0.022 0.023 0.023 C46 0.043 0.042 0.040 0.012 0.013 0.032 C47 0.050 0.025 0.039 0.005 0.022 0.026 C48 0.033 0.044 0.054 0.010 0.024 0.011 C49 0.043 0.016 0.024 0.006 0.017 0.016 C50 0.035 0.028 0.021 0.006 0.014 0.017 C51 0.067 0.046 0.048 0.033 0.038 0.042 C52 0.058 0.059 0.043 0.034 0.019 0.042 C53 0.050 0.055 0.039 0.019 0.009 0.036 C54 0.032 0.031 0.028 0.015 0.012 0.018 C55 0.026 0.048 0.056 0.043 0.022 0.021 C56A 0.037 0.031 0.065 0.026 0.009 0.015 C56B 0.032 0.031 0.036 0.023 0.006 0.012 C57A 0.044 0.042 0.048 0.033 0.013 0.011 C57B 0.039 0.037 0.041 0.016 0.016 0.015 C58A 0.035 0.027 0.035 0.021 0.004 0.010 C58B 0.035 0.038 0.036 0.020 0.008 0.011 C59A 0.048 0.057 0.048 0.040 0.006 0.000 C59B 0.050 0.053 0.050 0.028 0.014 0.016 C60A 0.047 0.035 0.049 0.024 0.003 0.007 C60B 0.045 0.039 0.049 0.023 0.009 0.014 C61 0.019 0.020 0.021 0.003 0.008 0.005 C62 0.054 0.029 0.032 0.009 0.017 0.021 C63 0.059 0.056 0.024 0.006 0.002 0.038 C64 0.036 0.060 0.029 -0.006 0.009 0.030 C65 0.035 0.052 0.038 0.021 0.020 0.010 C66 0.036 0.029 0.033 0.007 0.015 0.018 C67 0.032 0.023 0.019 0.014 0.008 0.011 C68 0.027 0.027 0.027 0.013 0.015 0.014 C69 0.019 0.027 0.037 0.012 0.004 0.011 C70 0.030 0.034 0.017 0.017 0.002 0.011 C71 0.041 0.055 0.020 0.019 0.019 0.022 C72 0.027 0.039 0.044 0.016 0.014 0.013 C73 0.094 0.030 0.071 0.018 -0.016 0.024 C74 0.016 0.108 0.146 0.084 0.008 0.001 C75 0.052 0.046 0.222 0.043 0.068 0.023 C76 0.058 0.074 0.084 0.007 0.019 0.049 C77 0.192 0.118 0.058 0.047 -0.009 0.003 C78 0.082 0.026 0.079 0.005 0.014 0.005 C79 0.063 0.046 0.054 -0.005 0.001 0.015 C80 0.113 0.073 0.066 0.027 0.059 0.044 C81 0.096 0.078 0.230 0.083 0.104 0.051 C82 0.062 0.098 0.121 -0.036 -0.042 0.056 C83 0.058 0.170 0.056 0.022 0.005 0.064 C84 0.248 0.107 0.054 0.060 0.049 0.067 C85 0.056 0.125 0.071 0.059 0.016 0.057 C86 0.059 0.093 0.061 -0.015 0.018 0.006 C87 0.131 0.299 0.053 -0.019 -0.014 0.171 C88 0.086 0.059 0.083 0.016 0.024 0.056 C89 0.047 0.048 0.028 0.011 0.016 0.025 C90 0.049 0.071 0.042 0.026 0.007 0.041 C91 0.053 0.033 0.044 0.012 0.003 0.031 C92 0.040 0.041 0.052 0.014 0.024 0.031 C93 0.021 0.034 0.033 0.019 0.008 0.009 C94 0.027 0.047 0.022 0.019 0.014 0.021 C95 0.041 0.038 0.025 0.017 0.011 0.009 C96 0.034 0.034 0.031 0.020 0.009 -0.001 C97 0.029 0.047 0.052 0.027 0.010 0.018 C98 0.039 0.037 0.042 0.019 0.021 0.019 C99 0.048 0.037 0.045 0.024 0.029 0.034 C100 0.056 0.024 0.042 0.018 0.016 0.020 C101 0.090 0.043 0.069 0.044 0.060 0.043 C102 0.099 0.067 0.042 0.039 0.039 0.064 C103 0.078 0.083 0.048 0.037 0.019 0.059 C104 0.038 0.063 0.045 0.023 0.013 0.030 C105 0.026 0.023 0.027 0.010 0.005 0.018 C106 0.023 0.046 0.037 0.011 0.014 0.014 C107 0.064 0.039 0.036 0.001 0.009 0.028 C108 0.038 0.031 0.043 0.013 -0.003 0.009 C109 0.036 0.050 0.046 0.037 0.015 0.015 C110 0.039 0.041 0.040 0.022 0.019 0.031 C111 0.015 0.030 0.028 0.006 0.006 0.011 C112 0.018 0.017 0.027 0.001 -0.004 0.005 C113 0.015 0.042 0.033 0.001 0.011 0.006 C114 0.030 0.047 0.063 0.003 0.002 0.025 C115 0.047 0.042 0.053 0.022 0.006 0.019 C116 0.025 0.045 0.056 0.034 0.018 0.009 C117 0.042 0.034 0.076 0.027 0.027 0.018 C118 0.048 0.065 0.048 0.026 0.033 0.030 C119 0.031 0.055 0.051 0.027 0.028 0.023 C120 0.057 0.047 0.054 0.028 0.028 0.031 C121 0.025 0.028 0.030 0.010 0.012 0.015 C122 0.024 0.026 0.026 0.014 0.013 0.006 C123 0.017 0.023 0.016 0.004 0.008 0.007 C124 0.019 0.018 0.024 0.003 0.013 0.009 C125 0.032 0.033 0.031 0.013 0.011 0.015 C126 0.022 0.025 0.025 0.009 0.010 0.008 C127 0.028 0.043 0.045 0.022 0.018 0.015 C128 0.033 0.071 0.063 0.039 0.017 0.013 C129 0.040 0.128 0.130 0.108 0.033 0.047 C130 0.079 0.120 0.186 0.122 0.067 0.072 C131 0.091 0.068 0.125 0.060 0.080 0.057 C132 0.069 0.067 0.057 0.039 0.046 0.048 C133 0.032 0.033 0.032 0.014 0.007 0.018 C134 0.031 0.033 0.030 -0.002 -0.004 0.009 C135 0.044 0.041 0.043 0.014 0.027 0.006 C136 0.064 0.036 0.034 0.020 0.016 0.011 C137 0.055 0.048 0.046 0.029 0.020 0.031 C138 0.041 0.051 0.037 0.019 0.020 0.020 C139 0.045 0.031 0.034 0.011 0.015 -0.002 C140 0.078 0.070 0.027 0.014 0.028 0.007 C141 0.155 0.039 0.072 0.005 0.076 -0.010 C142 0.079 0.151 0.055 0.043 0.014 -0.046 C143 0.043 0.159 0.075 0.066 0.006 -0.013 C144 0.021 0.080 0.047 0.023 0.000 -0.005 C158 0.025 0.031 0.027 0.010 0.012 0.014 C159 0.029 0.034 0.030 0.011 0.012 0.013 C160 0.065 0.070 0.067 0.022 0.027 0.031 C161 0.037 0.046 0.042 0.009 0.017 0.018 C162 0.061 0.063 0.068 0.024 0.027 0.028 C163 0.039 0.041 0.043 0.016 0.014 0.020 _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 O2 2.462(5) . ? Yb1 O7 2.500(5) . ? Yb1 O8 2.506(6) . ? Yb1 O6 2.509(5) . ? Yb1 O3 2.511(5) . ? Yb1 O4 2.524(6) . ? Yb1 O1 2.547(6) . ? Yb1 O5 2.550(6) . ? Yb2 C27 2.427(9) . ? Yb2 C33 2.432(8) . ? Yb2 O9 2.441(5) . ? Yb2 C21 2.458(9) . ? Yb2 C39 2.475(9) . ? Yb2 O10 2.481(6) . ? Yb3 O12 2.423(6) . ? Yb3 C61 2.424(8) . ? Yb3 C55 2.430(6) . ? Yb3 C49 2.456(9) . ? Yb3 O11 2.461(5) . ? Yb3 C67 2.466(8) . ? Yb4 O16 2.424(6) . ? Yb4 O17 2.462(7) . ? Yb4 O13 2.477(7) . ? Yb4 O14 2.483(6) . ? Yb4 O20 2.483(7) . ? Yb4 O19 2.496(7) . ? Yb4 O15 2.515(7) . ? Yb4 O18 2.526(8) . ? Yb5 C99 2.409(10) . ? Yb5 O22 2.439(5) . ? Yb5 C111 2.442(8) . ? Yb5 O21 2.453(6) . ? Yb5 C93 2.459(9) . ? Yb5 C105 2.481(9) . ? Yb6 C133 2.419(10) . ? Yb6 C127 2.462(9) . ? Yb6 C139 2.466(10) . ? Yb6 O23 2.469(5) . ? Yb6 O24 2.469(6) . ? Yb6 C121 2.486(10) . ? Yb6 C158 2.534(11) . ? O1 C2 1.413(10) . ? O1 C1 1.427(10) . ? O2 C4 1.394(10) . ? O2 C3 1.397(10) . ? O3 C6 1.412(9) . ? O3 C5 1.438(10) . ? O4 C7 1.428(10) . ? O4 C8 1.430(10) . ? O5 C10 1.438(9) . ? O5 C9 1.446(10) . ? O6 C11 1.434(10) . ? O6 C12 1.437(10) . ? O7 C13 1.417(10) . ? O7 C14 1.452(10) . ? O8 C16 1.402(10) . ? O8 C15 1.441(10) . ? O9 C17 1.430(10) . ? O9 C18 1.436(10) . ? O10 C20 1.423(10) . ? O10 C19 1.440(9) . ? O11 C45 1.415(10) . ? O11 C46 1.449(11) . ? O12 C48 1.423(10) . ? O12 C47 1.426(9) . ? O13 C73 1.437(11) . ? O13 C74 1.509(12) . ? O14 C75 1.408(13) . ? O14 C76 1.430(11) . ? O15 C77 1.370(15) . ? O15 C78 1.445(12) . ? O16 C80 1.362(12) . ? O16 C79 1.417(13) . ? O17 C81 1.384(15) . ? O17 C82 1.469(17) . ? O18 C84 1.386(16) . ? O18 C83 1.413(15) . ? O19 C85 1.397(11) . ? O19 C86 1.406(13) . ? O20 C87 1.402(15) . ? O20 C88 1.418(11) . ? O21 C90 1.439(10) . ? O21 C89 1.449(10) . ? O22 C91 1.392(11) . ? O22 C92 1.438(10) . ? O23 C118 1.418(11) . ? O23 C117 1.462(10) . ? O24 C119 1.439(10) . ? O24 C120 1.445(10) . ? O25 C146 1.292(15) . ? O25 C145 1.34(3) . ? O26 C147 1.39(3) . ? O26 C148 1.394(17) . ? O27 C149 1.45(3) . ? O28 C150 1.38(2) . ? O29 C152 1.27(3) . ? O29 C151 1.28(3) . ? O30 C153 1.35(3) . ? O30 C154 1.51(4) . ? C2 C3 1.447(13) . ? C6 C7 1.468(12) . ? C10 C11 1.478(13) . ? C14 C15 1.474(12) . ? C18 C19 1.477(12) . ? C21 C22 1.390(11) . ? C21 C26 1.419(12) . ? C22 C23 1.409(13) . ? C23 C24 1.376(13) . ? C24 C25 1.390(13) . ? C25 C26 1.397(13) . ? C27 C32 1.405(12) . ? C27 C28 1.422(12) . ? C28 C29 1.395(12) . ? C29 C30 1.368(12) . ? C30 C31 1.373(12) . ? C31 C32 1.394(12) . ? C33 C34 1.392(11) . ? C33 C38 1.421(13) . ? C34 C35 1.371(11) . ? C35 C36 1.398(12) . ? C36 C37 1.375(11) . ? C37 C38 1.364(11) . ? C39 C44 1.388(12) . ? C39 C40 1.401(12) . ? C40 C41 1.401(12) . ? C41 C42 1.348(14) . ? C42 C43 1.363(13) . ? C43 C44 1.400(12) . ? C46 C47 1.473(12) . ? C49 C54 1.400(12) . ? C49 C50 1.416(12) . ? C50 C51 1.395(12) . ? C51 C52 1.333(13) . ? C52 C53 1.378(14) . ? C53 C54 1.375(12) . ? C55 C60A 1.377(8) . ? C55 C56B 1.399(8) . ? C55 C56A 1.403(8) . ? C55 C60B 1.407(8) . ? C56A C57A 1.395(8) . ? C56B C57B 1.389(8) . ? C57A C58A 1.390(8) . ? C57B C58B 1.387(8) . ? C58A C59A 1.392(8) . ? C58B C59B 1.393(8) . ? C59A C60A 1.393(8) . ? C59B C60B 1.389(8) . ? C61 C66 1.379(12) . ? C61 C62 1.397(11) . ? C62 C63 1.401(13) . ? C63 C64 1.364(14) . ? C64 C65 1.354(13) . ? C65 C66 1.387(12) . ? C67 C68 1.379(11) . ? C67 C72 1.417(12) . ? C68 C69 1.381(12) . ? C69 C70 1.387(12) . ? C70 C71 1.379(12) . ? C71 C72 1.394(13) . ? C74 C75 1.409(16) . ? C78 C79 1.515(16) . ? C82 C83 1.40(2) . ? C86 C87 1.450(16) . ? C90 C91 1.468(13) . ? C93 C98 1.403(12) . ? C93 C94 1.425(11) . ? C94 C95 1.374(12) . ? C95 C96 1.371(12) . ? C96 C97 1.383(12) . ? C97 C98 1.393(13) . ? C99 C104 1.381(13) . ? C99 C100 1.394(13) . ? C100 C101 1.385(13) . ? C101 C102 1.358(15) . ? C102 C103 1.365(15) . ? C103 C104 1.409(14) . ? C105 C106 1.385(12) . ? C105 C110 1.391(12) . ? C106 C107 1.353(13) . ? C107 C108 1.387(14) . ? C108 C109 1.362(13) . ? C109 C110 1.372(12) . ? C111 C116 1.365(12) . ? C111 C112 1.407(12) . ? C112 C113 1.386(11) . ? C113 C114 1.378(14) . ? C114 C115 1.351(15) . ? C115 C116 1.384(12) . ? C118 C119 1.483(13) . ? C121 C122 1.394(8) . ? C121 C126 1.400(8) . ? C122 C123 1.384(8) . ? C123 C124 1.395(8) . ? C124 C125 1.385(8) . ? C125 C126 1.392(8) . ? C127 C132 1.392(13) . ? C127 C128 1.396(14) . ? C128 C129 1.380(14) . ? C129 C130 1.324(19) . ? C130 C131 1.390(19) . ? C131 C132 1.401(13) . ? C133 C134 1.391(13) . ? C133 C138 1.412(12) . ? C134 C135 1.395(13) . ? C135 C136 1.360(13) . ? C136 C137 1.357(13) . ? C137 C138 1.405(13) . ? C139 C144 1.395(14) . ? C139 C140 1.397(14) . ? C140 C141 1.405(17) . ? C141 C142 1.39(2) . ? C142 C143 1.34(2) . ? C143 C144 1.367(16) . ? C146 C147 1.50(3) . ? C158 C163 1.398(8) . ? C158 C159 1.399(8) . ? C159 C160 1.388(8) . ? C160 C161 1.391(8) . ? C161 C162 1.386(8) . ? C162 C163 1.390(8) . ? C152 C153 1.48(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Yb1 O7 105.50(18) . . ? O2 Yb1 O8 73.9(2) . . ? O7 Yb1 O8 64.84(18) . . ? O2 Yb1 O6 84.69(19) . . ? O7 Yb1 O6 148.18(19) . . ? O8 Yb1 O6 90.37(18) . . ? O2 Yb1 O3 147.7(2) . . ? O7 Yb1 O3 83.38(17) . . ? O8 Yb1 O3 135.73(19) . . ? O6 Yb1 O3 104.18(17) . . ? O2 Yb1 O4 87.02(19) . . ? O7 Yb1 O4 133.55(19) . . ? O8 Yb1 O4 157.57(19) . . ? O6 Yb1 O4 75.94(19) . . ? O3 Yb1 O4 65.93(18) . . ? O2 Yb1 O1 64.5(2) . . ? O7 Yb1 O1 74.19(19) . . ? O8 Yb1 O1 109.00(19) . . ? O6 Yb1 O1 135.7(2) . . ? O3 Yb1 O1 89.39(19) . . ? O4 Yb1 O1 71.6(2) . . ? O2 Yb1 O5 133.4(2) . . ? O7 Yb1 O5 87.76(18) . . ? O8 Yb1 O5 72.13(19) . . ? O6 Yb1 O5 64.78(18) . . ? O3 Yb1 O5 76.85(19) . . ? O4 Yb1 O5 115.87(18) . . ? O1 Yb1 O5 158.5(2) . . ? C27 Yb2 C33 106.8(3) . . ? C27 Yb2 O9 95.4(2) . . ? C33 Yb2 O9 157.2(3) . . ? C27 Yb2 C21 90.9(3) . . ? C33 Yb2 C21 99.7(3) . . ? O9 Yb2 C21 85.2(2) . . ? C27 Yb2 C39 95.6(3) . . ? C33 Yb2 C39 90.8(3) . . ? O9 Yb2 C39 81.3(2) . . ? C21 Yb2 C39 165.5(3) . . ? C27 Yb2 O10 161.3(2) . . ? C33 Yb2 O10 91.5(2) . . ? O9 Yb2 O10 66.94(18) . . ? C21 Yb2 O10 82.1(3) . . ? C39 Yb2 O10 87.8(2) . . ? O12 Yb3 C61 93.7(2) . . ? O12 Yb3 C55 162.8(2) . . ? C61 Yb3 C55 103.5(3) . . ? O12 Yb3 C49 82.5(2) . . ? C61 Yb3 C49 96.6(3) . . ? C55 Yb3 C49 96.6(3) . . ? O12 Yb3 O11 68.12(19) . . ? C61 Yb3 O11 161.7(2) . . ? C55 Yb3 O11 94.8(2) . . ? C49 Yb3 O11 80.4(2) . . ? O12 Yb3 C67 79.6(2) . . ? C61 Yb3 C67 94.7(3) . . ? C55 Yb3 C67 97.5(3) . . ? C49 Yb3 C67 159.4(3) . . ? O11 Yb3 C67 83.5(2) . . ? O16 Yb4 O17 78.6(3) . . ? O16 Yb4 O13 120.2(3) . . ? O17 Yb4 O13 127.6(3) . . ? O16 Yb4 O14 76.0(2) . . ? O17 Yb4 O14 154.5(3) . . ? O13 Yb4 O14 65.4(2) . . ? O16 Yb4 O20 155.1(2) . . ? O17 Yb4 O20 76.6(3) . . ? O13 Yb4 O20 77.8(3) . . ? O14 Yb4 O20 128.9(2) . . ? O16 Yb4 O19 128.2(2) . . ? O17 Yb4 O19 123.0(3) . . ? O13 Yb4 O19 85.3(3) . . ? O14 Yb4 O19 76.3(2) . . ? O20 Yb4 O19 66.1(2) . . ? O16 Yb4 O15 64.3(3) . . ? O17 Yb4 O15 77.0(3) . . ? O13 Yb4 O15 154.9(3) . . ? O14 Yb4 O15 94.3(3) . . ? O20 Yb4 O15 107.4(3) . . ? O19 Yb4 O15 75.2(3) . . ? O16 Yb4 O18 78.6(3) . . ? O17 Yb4 O18 64.2(3) . . ? O13 Yb4 O18 72.2(3) . . ? O14 Yb4 O18 107.5(3) . . ? O20 Yb4 O18 92.6(3) . . ? O19 Yb4 O18 152.1(3) . . ? O15 Yb4 O18 130.7(3) . . ? C99 Yb5 O22 95.1(2) . . ? C99 Yb5 C111 108.3(3) . . ? O22 Yb5 C111 156.5(3) . . ? C99 Yb5 O21 160.5(2) . . ? O22 Yb5 O21 66.78(19) . . ? C111 Yb5 O21 90.3(2) . . ? C99 Yb5 C93 89.9(3) . . ? O22 Yb5 C93 85.1(2) . . ? C111 Yb5 C93 96.9(3) . . ? O21 Yb5 C93 81.6(3) . . ? C99 Yb5 C105 95.0(3) . . ? O22 Yb5 C105 79.5(2) . . ? C111 Yb5 C105 95.7(3) . . ? O21 Yb5 C105 89.0(2) . . ? C93 Yb5 C105 164.2(3) . . ? C133 Yb6 C127 110.6(3) . . ? C133 Yb6 C139 92.8(3) . . ? C127 Yb6 C139 96.4(3) . . ? C133 Yb6 O23 88.1(2) . . ? C127 Yb6 O23 160.5(3) . . ? C139 Yb6 O23 87.8(3) . . ? C133 Yb6 O24 153.8(2) . . ? C127 Yb6 O24 94.8(3) . . ? C139 Yb6 O24 77.8(3) . . ? O23 Yb6 O24 67.4(2) . . ? C133 Yb6 C121 107.3(4) . . ? C127 Yb6 C121 87.4(5) . . ? C139 Yb6 C121 156.8(5) . . ? O23 Yb6 C121 81.6(5) . . ? O24 Yb6 C121 79.1(4) . . ? C133 Yb6 C158 98.0(4) . . ? C127 Yb6 C158 94.1(5) . . ? C139 Yb6 C158 161.3(5) . . ? O23 Yb6 C158 77.3(5) . . ? O24 Yb6 C158 85.9(4) . . ? C121 Yb6 C158 9.9(4) . . ? C2 O1 C1 113.8(7) . . ? C2 O1 Yb1 113.0(6) . . ? C1 O1 Yb1 124.7(5) . . ? C4 O2 C3 111.2(7) . . ? C4 O2 Yb1 127.0(5) . . ? C3 O2 Yb1 121.5(5) . . ? C6 O3 C5 110.2(6) . . ? C6 O3 Yb1 112.1(5) . . ? C5 O3 Yb1 122.8(5) . . ? C7 O4 C8 111.3(7) . . ? C7 O4 Yb1 115.2(5) . . ? C8 O4 Yb1 123.9(5) . . ? C10 O5 C9 109.5(7) . . ? C10 O5 Yb1 118.2(5) . . ? C9 O5 Yb1 125.0(5) . . ? C11 O6 C12 110.4(6) . . ? C11 O6 Yb1 114.0(5) . . ? C12 O6 Yb1 123.6(5) . . ? C13 O7 C14 109.6(6) . . ? C13 O7 Yb1 129.3(5) . . ? C14 O7 Yb1 120.1(5) . . ? C16 O8 C15 113.0(7) . . ? C16 O8 Yb1 131.0(5) . . ? C15 O8 Yb1 112.6(5) . . ? C17 O9 C18 111.7(6) . . ? C17 O9 Yb2 119.3(5) . . ? C18 O9 Yb2 113.6(5) . . ? C20 O10 C19 110.5(7) . . ? C20 O10 Yb2 120.3(5) . . ? C19 O10 Yb2 115.1(5) . . ? C45 O11 C46 110.0(6) . . ? C45 O11 Yb3 119.5(5) . . ? C46 O11 Yb3 112.5(5) . . ? C48 O12 C47 113.0(7) . . ? C48 O12 Yb3 121.7(5) . . ? C47 O12 Yb3 114.8(5) . . ? C73 O13 C74 113.9(9) . . ? C73 O13 Yb4 123.4(7) . . ? C74 O13 Yb4 112.7(6) . . ? C75 O14 C76 109.4(8) . . ? C75 O14 Yb4 121.3(6) . . ? C76 O14 Yb4 127.5(6) . . ? C77 O15 C78 112.9(10) . . ? C77 O15 Yb4 128.1(8) . . ? C78 O15 Yb4 117.1(7) . . ? C80 O16 C79 112.9(9) . . ? C80 O16 Yb4 129.3(7) . . ? C79 O16 Yb4 116.5(6) . . ? C81 O17 C82 113.5(10) . . ? C81 O17 Yb4 124.5(9) . . ? C82 O17 Yb4 120.6(9) . . ? C84 O18 C83 112.6(11) . . ? C84 O18 Yb4 123.4(9) . . ? C83 O18 Yb4 113.8(9) . . ? C85 O19 C86 112.5(9) . . ? C85 O19 Yb4 124.4(7) . . ? C86 O19 Yb4 117.3(7) . . ? C87 O20 C88 113.9(9) . . ? C87 O20 Yb4 117.6(7) . . ? C88 O20 Yb4 127.1(7) . . ? C90 O21 C89 111.3(7) . . ? C90 O21 Yb5 115.1(5) . . ? C89 O21 Yb5 119.3(5) . . ? C91 O22 C92 111.8(6) . . ? C91 O22 Yb5 112.6(5) . . ? C92 O22 Yb5 122.2(5) . . ? C118 O23 C117 110.8(7) . . ? C118 O23 Yb6 113.6(5) . . ? C117 O23 Yb6 120.3(5) . . ? C119 O24 C120 110.7(7) . . ? C119 O24 Yb6 113.3(5) . . ? C120 O24 Yb6 117.0(5) . . ? C146 O25 C145 110.5(15) . . ? C147 O26 C148 118.3(17) . . ? C152 O29 C151 137(3) . . ? C153 O30 C154 103(3) . . ? O1 C2 C3 111.9(8) . . ? O2 C3 C2 111.4(8) . . ? O3 C6 C7 109.6(6) . . ? O4 C7 C6 107.9(7) . . ? O5 C10 C11 107.7(8) . . ? O6 C11 C10 110.1(7) . . ? O7 C14 C15 108.6(7) . . ? O8 C15 C14 110.1(7) . . ? O9 C18 C19 107.9(7) . . ? O10 C19 C18 107.7(7) . . ? C22 C21 C26 112.5(8) . . ? C22 C21 Yb2 124.4(7) . . ? C26 C21 Yb2 123.0(6) . . ? C21 C22 C23 124.4(9) . . ? C24 C23 C22 120.7(9) . . ? C23 C24 C25 117.7(9) . . ? C24 C25 C26 120.3(10) . . ? C25 C26 C21 124.3(9) . . ? C32 C27 C28 111.1(8) . . ? C32 C27 Yb2 126.8(7) . . ? C28 C27 Yb2 121.5(6) . . ? C29 C28 C27 124.5(8) . . ? C30 C29 C28 120.2(9) . . ? C29 C30 C31 119.0(9) . . ? C30 C31 C32 119.4(8) . . ? C31 C32 C27 125.7(9) . . ? C34 C33 C38 113.7(7) . . ? C34 C33 Yb2 120.3(6) . . ? C38 C33 Yb2 125.6(6) . . ? C35 C34 C33 123.9(9) . . ? C34 C35 C36 119.7(8) . . ? C37 C36 C35 119.0(8) . . ? C38 C37 C36 120.0(9) . . ? C37 C38 C33 123.7(8) . . ? C44 C39 C40 112.8(8) . . ? C44 C39 Yb2 121.5(7) . . ? C40 C39 Yb2 125.3(7) . . ? C39 C40 C41 123.6(9) . . ? C42 C41 C40 119.4(9) . . ? C41 C42 C43 121.1(10) . . ? C42 C43 C44 117.9(10) . . ? C39 C44 C43 125.2(9) . . ? O11 C46 C47 107.7(7) . . ? O12 C47 C46 109.3(7) . . ? C54 C49 C50 112.8(8) . . ? C54 C49 Yb3 125.4(7) . . ? C50 C49 Yb3 121.7(6) . . ? C51 C50 C49 123.3(9) . . ? C52 C51 C50 120.1(10) . . ? C51 C52 C53 120.0(10) . . ? C54 C53 C52 119.8(10) . . ? C53 C54 C49 123.9(9) . . ? C60A C55 C56B 103.4(7) . . ? C60A C55 C56A 120.6(7) . . ? C56B C55 C56A 17.3(6) . . ? C60A C55 C60B 15.4(10) . . ? C56B C55 C60B 117.6(6) . . ? C56A C55 C60B 134.8(7) . . ? C60A C55 Yb3 123.1(6) . . ? C56B C55 Yb3 133.1(7) . . ? C56A C55 Yb3 116.2(6) . . ? C60B C55 Yb3 108.2(6) . . ? C57A C56A C55 119.5(7) . . ? C57B C56B C55 121.2(7) . . ? C58A C57A C56A 119.4(7) . . ? C58B C57B C56B 120.6(7) . . ? C57A C58A C59A 120.8(7) . . ? C57B C58B C59B 119.2(7) . . ? C58A C59A C60A 119.5(7) . . ? C60B C59B C58B 120.1(7) . . ? C55 C60A C59A 120.0(7) . . ? C59B C60B C55 121.2(7) . . ? C66 C61 C62 113.1(8) . . ? C66 C61 Yb3 125.6(6) . . ? C62 C61 Yb3 121.3(7) . . ? C61 C62 C63 123.8(10) . . ? C64 C63 C62 119.2(9) . . ? C65 C64 C63 119.6(9) . . ? C64 C65 C66 119.8(10) . . ? C61 C66 C65 124.5(9) . . ? C68 C67 C72 112.6(8) . . ? C68 C67 Yb3 122.1(6) . . ? C72 C67 Yb3 125.0(6) . . ? C67 C68 C69 125.5(8) . . ? C68 C69 C70 119.4(8) . . ? C71 C70 C69 118.9(8) . . ? C70 C71 C72 119.4(9) . . ? C71 C72 C67 124.1(8) . . ? C75 C74 O13 112.1(11) . . ? O14 C75 C74 109.6(10) . . ? O15 C78 C79 109.2(9) . . ? O16 C79 C78 103.6(9) . . ? C83 C82 O17 107.7(10) . . ? C82 C83 O18 112.7(11) . . ? O19 C86 C87 112.1(11) . . ? O20 C87 C86 115.3(12) . . ? O21 C90 C91 108.2(8) . . ? O22 C91 C90 107.8(8) . . ? C98 C93 C94 113.1(8) . . ? C98 C93 Yb5 121.2(6) . . ? C94 C93 Yb5 125.3(6) . . ? C95 C94 C93 124.1(8) . . ? C96 C95 C94 120.5(9) . . ? C95 C96 C97 118.3(9) . . ? C96 C97 C98 121.0(9) . . ? C97 C98 C93 123.0(9) . . ? C104 C99 C100 112.8(9) . . ? C104 C99 Yb5 121.1(7) . . ? C100 C99 Yb5 126.0(7) . . ? C101 C100 C99 123.5(11) . . ? C102 C101 C100 121.3(11) . . ? C101 C102 C103 118.5(11) . . ? C102 C103 C104 119.0(12) . . ? C99 C104 C103 124.8(11) . . ? C106 C105 C110 110.8(8) . . ? C106 C105 Yb5 124.6(7) . . ? C110 C105 Yb5 124.3(6) . . ? C107 C106 C105 126.0(10) . . ? C106 C107 C108 119.2(9) . . ? C109 C108 C107 119.3(10) . . ? C108 C109 C110 117.8(10) . . ? C109 C110 C105 126.9(9) . . ? C116 C111 C112 112.4(8) . . ? C116 C111 Yb5 121.3(7) . . ? C112 C111 Yb5 126.3(6) . . ? C113 C112 C111 124.1(9) . . ? C114 C113 C112 119.1(9) . . ? C115 C114 C113 119.4(9) . . ? C114 C115 C116 119.2(10) . . ? C111 C116 C115 125.8(10) . . ? O23 C118 C119 109.4(8) . . ? O24 C119 C118 106.9(7) . . ? C122 C121 C126 118.5(7) . . ? C122 C121 Yb6 119.0(7) . . ? C126 C121 Yb6 122.3(7) . . ? C123 C122 C121 120.7(7) . . ? C122 C123 C124 120.0(7) . . ? C125 C124 C123 119.8(7) . . ? C124 C125 C126 119.7(7) . . ? C125 C126 C121 120.9(7) . . ? C132 C127 C128 113.9(9) . . ? C132 C127 Yb6 120.2(7) . . ? C128 C127 Yb6 125.7(8) . . ? C129 C128 C127 123.2(12) . . ? C130 C129 C128 120.6(14) . . ? C129 C130 C131 120.9(11) . . ? C130 C131 C132 117.5(12) . . ? C127 C132 C131 123.9(11) . . ? C134 C133 C138 112.6(9) . . ? C134 C133 Yb6 125.6(7) . . ? C138 C133 Yb6 121.8(7) . . ? C133 C134 C135 125.2(9) . . ? C136 C135 C134 119.6(10) . . ? C137 C136 C135 118.8(10) . . ? C136 C137 C138 121.3(10) . . ? C137 C138 C133 122.5(10) . . ? C144 C139 C140 113.6(10) . . ? C144 C139 Yb6 123.6(8) . . ? C140 C139 Yb6 122.8(8) . . ? C139 C140 C141 123.8(13) . . ? C142 C141 C140 117.1(14) . . ? C143 C142 C141 121.6(14) . . ? C142 C143 C144 119.6(15) . . ? C143 C144 C139 124.2(13) . . ? O25 C146 C147 109.8(15) . . ? O26 C147 C146 118(2) . . ? C163 C158 C159 119.0(7) . . ? C163 C158 Yb6 120.0(8) . . ? C159 C158 Yb6 120.8(8) . . ? C160 C159 C158 120.3(7) . . ? C159 C160 C161 120.0(7) . . ? C162 C161 C160 120.2(7) . . ? C161 C162 C163 119.9(7) . . ? C162 C163 C158 120.4(7) . . ? O29 C152 C153 141(3) . . ? O30 C153 C152 124(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.420 _refine_diff_density_min -1.175 _refine_diff_density_rms 0.178