# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'M. Lappert' 'Peter B. Hitchcock' 'Alexei V. Khvostov' 'Andrey V. Protchenko' _publ_contact_author_name 'M. Lappert' _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_section_title ; Heteroleptic ytterbium(II) complexes supported by a bulky beta-diketiminato ligand ; _publ_requested_category FM # Attachment 'mfl_sep2008.cif' data_(1)-feb203 _database_code_depnum_ccdc_archive 'CCDC 706860' _audit_creation_date 2003-02-03T16:25:33-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C66 H98 I2 N4 O2 Yb2' _chemical_formula_sum 'C66 H98 I2 N4 O2 Yb2' _chemical_formula_weight 1579.36 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.3326(4) _cell_length_b 12.4318(2) _cell_length_c 21.8144(4) _cell_angle_alpha 90 _cell_angle_beta 116.695(1) _cell_angle_gamma 90 _cell_volume 6864.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22011 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.649 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6387 _exptl_absorpt_correction_T_max 0.7759 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_unetI/netI 0.0418 _diffrn_reflns_number 31737 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 25.06 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 6020 _reflns_number_gt 5009 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0283P)^2^+55.3102P] 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_number_reflns 6020 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.052 _refine_ls_R_factor_gt 0.038 _refine_ls_wR_factor_ref 0.0825 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.247 _refine_diff_density_min -1.494 _refine_diff_density_rms 0.107 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.385 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Yb Yb 0.161150(9) 0.793735(18) 0.459842(12) 0.02925(8) Uani 1 1 d . . . I I 0.232143(17) 0.58680(3) 0.49429(3) 0.06566(17) Uani 1 1 d . . . O O 0.12709(17) 0.7653(4) 0.3404(2) 0.0526(12) Uani 1 1 d . . . N1 N 0.11127(17) 0.9540(3) 0.4542(2) 0.0308(10) Uani 1 1 d . . . N2 N 0.08956(17) 0.7205(3) 0.4767(2) 0.0289(10) Uani 1 1 d . . . C1 C 0.0604(2) 0.9589(4) 0.4375(3) 0.0329(13) Uani 1 1 d . . . C2 C 0.0290(2) 0.8697(5) 0.4353(3) 0.0367(13) Uani 1 1 d . . . H2 H -0.0079 0.8838 0.4139 0.044 Uiso 1 1 calc R . . C3 C 0.0424(2) 0.7641(4) 0.4590(3) 0.0305(12) Uani 1 1 d . . . C4 C 0.0314(3) 1.0669(5) 0.4221(4) 0.0522(17) Uani 1 1 d . . . H4A H 0.052 1.1188 0.458 0.078 Uiso 1 1 calc R . . H4B H -0.0034 1.0572 0.4209 0.078 Uiso 1 1 calc R . . H4C H 0.0269 1.0938 0.3775 0.078 Uiso 1 1 calc R . . C5 C 0.0003(2) 0.7017(5) 0.4685(3) 0.0421(14) Uani 1 1 d . . . H5A H -0.0063 0.6334 0.4435 0.063 Uiso 1 1 calc R . . H5B H -0.0324 0.7439 0.4506 0.063 Uiso 1 1 calc R . . H5C H 0.0122 0.6874 0.5174 0.063 Uiso 1 1 calc R . . C6 C 0.1391(2) 1.0548(4) 0.4659(3) 0.0360(13) Uani 1 1 d . . . C7 C 0.1665(2) 1.0928(4) 0.5337(3) 0.0388(14) Uani 1 1 d . . . C8 C 0.1916(3) 1.1917(5) 0.5444(4) 0.0568(19) Uani 1 1 d . . . H8 H 0.2097 1.2184 0.59 0.068 Uiso 1 1 calc R . . C9 C 0.1912(3) 1.2524(5) 0.4918(5) 0.063(2) Uani 1 1 d . . . H9 H 0.2074 1.3214 0.5005 0.075 Uiso 1 1 calc R . . C10 C 0.1676(3) 1.2127(5) 0.4275(5) 0.062(2) Uani 1 1 d . . . H10 H 0.1687 1.2535 0.3914 0.075 Uiso 1 1 calc R . . C11 C 0.1411(3) 1.1126(5) 0.4118(4) 0.0506(17) Uani 1 1 d . . . C12 C 0.1679(3) 1.0279(5) 0.5931(3) 0.0525(17) Uani 1 1 d . . . H12 H 0.1631 0.9507 0.5787 0.063 Uiso 1 1 calc R . . C13 C 0.1227(4) 1.0577(10) 0.6089(5) 0.115(4) Uani 1 1 d . . . H13A H 0.1244 1.0136 0.647 0.173 Uiso 1 1 calc R . . H13B H 0.0891 1.0448 0.5683 0.173 Uiso 1 1 calc R . . H13C H 0.1254 1.1339 0.6215 0.173 Uiso 1 1 calc R . . C14 C 0.2200(4) 1.0365(9) 0.6575(5) 0.102(3) Uani 1 1 d . . . H14A H 0.2188 0.9915 0.6937 0.152 Uiso 1 1 calc R . . H14B H 0.2262 1.1115 0.6729 0.152 Uiso 1 1 calc R . . H14C H 0.2488 1.0118 0.6476 0.152 Uiso 1 1 calc R . . C15 C 0.1171(4) 1.0709(7) 0.3402(4) 0.080(3) Uani 1 1 d . . . H15 H 0.098 1.0026 0.339 0.096 Uiso 1 1 calc R . . C16 C 0.1592(5) 1.0454(7) 0.3172(5) 0.103(4) Uani 1 1 d . . . H16A H 0.1424 1.0172 0.2703 0.155 Uiso 1 1 calc R . . H16B H 0.1836 0.9915 0.348 0.155 Uiso 1 1 calc R . . H16C H 0.1788 1.1111 0.3186 0.155 Uiso 1 1 calc R . . C17 C 0.0768(4) 1.1502(11) 0.2885(5) 0.126(4) Uani 1 1 d . . . H17A H 0.0621 1.1192 0.2423 0.188 Uiso 1 1 calc R . . H17B H 0.0945 1.2182 0.2892 0.188 Uiso 1 1 calc R . . H17C H 0.0482 1.1634 0.3011 0.188 Uiso 1 1 calc R . . C18 C 0.1008(2) 0.6164(4) 0.5099(3) 0.0279(11) Uani 1 1 d . . . C19 C 0.1310(2) 0.6138(5) 0.5817(3) 0.0350(13) Uani 1 1 d . . . C20 C 0.1445(2) 0.5147(5) 0.6134(3) 0.0426(15) Uani 1 1 d . . . H20 H 0.1644 0.5115 0.6619 0.051 Uiso 1 1 calc R . . C21 C 0.1299(3) 0.4206(5) 0.5764(3) 0.0448(15) Uani 1 1 d . . . H21 H 0.1401 0.3533 0.5993 0.054 Uiso 1 1 calc R . . C22 C 0.1007(2) 0.4239(5) 0.5066(3) 0.0380(14) Uani 1 1 d . . . H22 H 0.0907 0.3584 0.4815 0.046 Uiso 1 1 calc R . . C23 C 0.0854(2) 0.5211(4) 0.4718(3) 0.0325(12) Uani 1 1 d . . . C24 C 0.1483(3) 0.7171(5) 0.6232(3) 0.0454(15) Uani 1 1 d . . . H24 H 0.1418 0.7776 0.5902 0.055 Uiso 1 1 calc R . . C25 C 0.1168(6) 0.7384(11) 0.6604(8) 0.191(8) Uani 1 1 d . . . H25A H 0.0792 0.7381 0.628 0.286 Uiso 1 1 calc R . . H25B H 0.1265 0.8088 0.6829 0.286 Uiso 1 1 calc R . . H25C H 0.1239 0.6824 0.6951 0.286 Uiso 1 1 calc R . . C26 C 0.2057(4) 0.7168(9) 0.6713(7) 0.144(6) Uani 1 1 d . . . H26A H 0.226 0.7046 0.6456 0.216 Uiso 1 1 calc R . . H26B H 0.2132 0.6593 0.7052 0.216 Uiso 1 1 calc R . . H26C H 0.2156 0.7863 0.6949 0.216 Uiso 1 1 calc R . . C27 C 0.0532(2) 0.5191(5) 0.3938(3) 0.0416(14) Uani 1 1 d . . . H27 H 0.0426 0.5948 0.378 0.05 Uiso 1 1 calc R . . C28 C 0.0021(3) 0.4521(6) 0.3704(4) 0.0598(19) Uani 1 1 d . . . H28A H -0.0175 0.4539 0.3202 0.09 Uiso 1 1 calc R . . H28B H -0.0198 0.4823 0.3904 0.09 Uiso 1 1 calc R . . H28C H 0.0113 0.3775 0.3858 0.09 Uiso 1 1 calc R . . C29 C 0.0863(3) 0.4780(6) 0.3600(3) 0.0560(18) Uani 1 1 d . . . H29A H 0.0648 0.4767 0.3101 0.084 Uiso 1 1 calc R . . H29B H 0.0988 0.4052 0.3765 0.084 Uiso 1 1 calc R . . H29C H 0.1167 0.5257 0.3717 0.084 Uiso 1 1 calc R . . C30 C 0.0731(3) 0.7760(7) 0.2917(4) 0.071(2) Uani 1 1 d . . . H30A H 0.0502 0.7434 0.3101 0.085 Uiso 1 1 calc R . . H30B H 0.0638 0.8531 0.2826 0.085 Uiso 1 1 calc R . . C31 C 0.0651(6) 0.7253(14) 0.2320(6) 0.177(8) Uani 1 1 d . . . H31A H 0.0485 0.7754 0.1928 0.212 Uiso 1 1 calc R . . H31B H 0.0413 0.6629 0.2237 0.212 Uiso 1 1 calc R . . C32 C 0.1157(5) 0.6896(10) 0.2383(5) 0.126(5) Uani 1 1 d . . . H32A H 0.1219 0.7191 0.2004 0.151 Uiso 1 1 calc R . . H32B H 0.1167 0.6101 0.2364 0.151 Uiso 1 1 calc R . . C33 C 0.1566(4) 0.7289(8) 0.3051(4) 0.081(3) Uani 1 1 d . . . H33A H 0.1812 0.6704 0.3309 0.097 Uiso 1 1 calc R . . H33B H 0.177 0.7887 0.2987 0.097 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 Yb 0.02681(13) 0.03265(14) 0.03229(14) -0.00199(11) 0.01683(10) -0.00154(10) I 0.0322(2) 0.0309(2) 0.1290(5) 0.0014(2) 0.0319(3) -0.00163(17) O 0.044(3) 0.082(3) 0.033(2) -0.013(2) 0.019(2) -0.008(2) N1 0.033(3) 0.031(2) 0.034(3) 0.001(2) 0.020(2) -0.0018(19) N2 0.028(2) 0.031(2) 0.032(2) 0.0042(19) 0.018(2) -0.0011(19) C1 0.036(3) 0.032(3) 0.037(3) 0.003(2) 0.022(3) 0.006(2) C2 0.029(3) 0.045(3) 0.036(3) 0.003(3) 0.015(3) 0.004(3) C3 0.027(3) 0.037(3) 0.031(3) -0.002(2) 0.016(2) -0.004(2) C4 0.049(4) 0.044(4) 0.072(5) 0.013(3) 0.035(4) 0.010(3) C5 0.038(3) 0.042(3) 0.057(4) 0.008(3) 0.031(3) -0.003(3) C6 0.033(3) 0.024(3) 0.059(4) 0.004(3) 0.028(3) 0.004(2) C7 0.034(3) 0.031(3) 0.054(4) -0.005(3) 0.023(3) 0.006(2) C8 0.052(4) 0.034(4) 0.086(5) -0.017(4) 0.033(4) 0.000(3) C9 0.059(5) 0.030(3) 0.111(7) -0.007(4) 0.048(5) -0.006(3) C10 0.064(5) 0.041(4) 0.100(6) 0.018(4) 0.053(5) 0.001(3) C11 0.058(4) 0.042(4) 0.061(4) 0.011(3) 0.035(4) -0.004(3) C12 0.064(5) 0.042(4) 0.045(4) -0.009(3) 0.019(3) 0.003(3) C13 0.119(9) 0.176(11) 0.087(7) 0.044(7) 0.078(7) 0.045(8) C14 0.082(7) 0.125(9) 0.066(6) 0.004(6) 0.005(5) 0.001(6) C15 0.119(8) 0.074(6) 0.063(5) 0.009(4) 0.054(5) -0.031(5) C16 0.185(11) 0.065(6) 0.078(6) 0.016(5) 0.076(7) 0.028(6) C17 0.084(7) 0.216(14) 0.076(7) 0.043(8) 0.035(6) -0.003(8) C18 0.028(3) 0.030(3) 0.033(3) 0.003(2) 0.020(2) 0.000(2) C19 0.039(3) 0.040(3) 0.033(3) -0.001(3) 0.021(3) -0.001(3) C20 0.051(4) 0.049(4) 0.032(3) 0.009(3) 0.023(3) 0.001(3) C21 0.059(4) 0.040(3) 0.046(4) 0.012(3) 0.032(3) 0.008(3) C22 0.044(4) 0.033(3) 0.044(4) 0.000(3) 0.026(3) -0.008(3) C23 0.032(3) 0.035(3) 0.034(3) 0.005(2) 0.018(3) -0.004(2) C24 0.057(4) 0.043(3) 0.032(3) -0.005(3) 0.016(3) -0.008(3) C25 0.191(14) 0.203(14) 0.270(18) -0.200(14) 0.185(14) -0.118(11) C26 0.065(7) 0.099(8) 0.188(13) -0.070(8) -0.015(7) -0.012(6) C27 0.051(4) 0.035(3) 0.034(3) 0.000(3) 0.014(3) -0.006(3) C28 0.054(4) 0.070(5) 0.046(4) -0.003(4) 0.014(4) -0.017(4) C29 0.074(5) 0.059(4) 0.040(4) -0.003(3) 0.030(4) -0.003(4) C30 0.049(5) 0.110(7) 0.040(4) -0.008(4) 0.008(4) -0.020(4) C31 0.145(12) 0.249(18) 0.073(8) -0.057(9) -0.007(8) 0.096(12) C32 0.182(13) 0.148(11) 0.076(7) -0.041(7) 0.084(8) -0.007(10) C33 0.098(7) 0.100(7) 0.079(6) -0.017(5) 0.071(6) -0.002(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Yb O 2.364(4) . ? Yb N2 2.398(4) . ? Yb N1 2.414(4) . ? Yb I 3.1031(5) 7_566 ? Yb I 3.1418(5) . ? I Yb 3.1031(5) 7_566 ? O C30 1.424(8) . ? O C33 1.439(8) . ? N1 C1 1.318(7) . ? N1 C6 1.441(7) . ? N2 C3 1.330(7) . ? N2 C18 1.447(6) . ? C1 C2 1.411(8) . ? C1 C4 1.531(8) . ? C2 C3 1.399(8) . ? C3 C5 1.512(7) . ? C6 C11 1.404(8) . ? C6 C7 1.409(8) . ? C7 C8 1.387(9) . ? C7 C12 1.511(9) . ? C8 C9 1.370(11) . ? C9 C10 1.348(11) . ? C10 C11 1.414(9) . ? C11 C15 1.489(10) . ? C12 C13 1.514(11) . ? C12 C14 1.517(10) . ? C15 C16 1.521(13) . ? C15 C17 1.546(13) . ? C18 C23 1.400(7) . ? C18 C19 1.407(8) . ? C19 C20 1.380(8) . ? C19 C24 1.520(8) . ? C20 C21 1.375(9) . ? C21 C22 1.369(8) . ? C22 C23 1.389(8) . ? C23 C27 1.528(8) . ? C24 C25 1.474(11) . ? C24 C26 1.486(11) . ? C27 C29 1.519(9) . ? C27 C28 1.543(9) . ? C30 C31 1.372(13) . ? C31 C32 1.448(16) . ? C32 C33 1.479(13) . ? 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 O Yb N2 99.08(15) . . ? O Yb N1 97.33(16) . . ? N2 Yb N1 78.77(14) . . ? O Yb I 106.44(11) . 7_566 ? N2 Yb I 154.30(10) . 7_566 ? N1 Yb I 94.85(10) . 7_566 ? O Yb I 92.38(12) . . ? N2 Yb I 98.46(10) . . ? N1 Yb I 170.20(10) . . ? I Yb I 83.595(12) 7_566 . ? Yb I Yb 96.405(12) 7_566 . ? C30 O C33 108.6(6) . . ? C30 O Yb 125.3(4) . . ? C33 O Yb 126.1(5) . . ? C1 N1 C6 116.9(4) . . ? C1 N1 Yb 126.4(4) . . ? C6 N1 Yb 116.6(3) . . ? C3 N2 C18 118.5(4) . . ? C3 N2 Yb 127.6(3) . . ? C18 N2 Yb 113.9(3) . . ? N1 C1 C2 124.7(5) . . ? N1 C1 C4 121.0(5) . . ? C2 C1 C4 114.3(5) . . ? C3 C2 C1 131.5(5) . . ? N2 C3 C2 124.1(5) . . ? N2 C3 C5 120.2(5) . . ? C2 C3 C5 115.6(5) . . ? C11 C6 C7 120.0(5) . . ? C11 C6 N1 121.5(5) . . ? C7 C6 N1 118.5(5) . . ? C8 C7 C6 118.2(6) . . ? C8 C7 C12 121.0(6) . . ? C6 C7 C12 120.8(5) . . ? C9 C8 C7 122.5(7) . . ? C10 C9 C8 118.9(6) . . ? C9 C10 C11 122.4(7) . . ? C6 C11 C10 117.7(7) . . ? C6 C11 C15 122.1(6) . . ? C10 C11 C15 120.2(6) . . ? C7 C12 C13 111.4(6) . . ? C7 C12 C14 113.4(7) . . ? C13 C12 C14 110.1(7) . . ? C11 C15 C16 111.1(8) . . ? C11 C15 C17 112.6(8) . . ? C16 C15 C17 108.9(7) . . ? C23 C18 C19 120.9(5) . . ? C23 C18 N2 121.3(5) . . ? C19 C18 N2 117.7(5) . . ? C20 C19 C18 118.2(5) . . ? C20 C19 C24 120.8(5) . . ? C18 C19 C24 121.0(5) . . ? C21 C20 C19 121.5(6) . . ? C22 C21 C20 120.0(6) . . ? C21 C22 C23 121.3(6) . . ? C22 C23 C18 118.3(5) . . ? C22 C23 C27 118.6(5) . . ? C18 C23 C27 123.1(5) . . ? C25 C24 C26 110.6(9) . . ? C25 C24 C19 111.5(6) . . ? C26 C24 C19 112.1(6) . . ? C29 C27 C23 110.8(5) . . ? C29 C27 C28 110.5(5) . . ? C23 C27 C28 112.3(5) . . ? C31 C30 O 109.1(8) . . ? C30 C31 C32 108.5(10) . . ? C31 C32 C33 107.2(8) . . ? O C33 C32 104.2(7) . . ? #===END data_(2)-jun1001 _database_code_depnum_ccdc_archive 'CCDC 706861' _audit_creation_date 2001-06-19T15:49:04-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[{YbI(thf)(Me3SiNCPhCHCPhNSiMe3)}2]' _chemical_formula_moiety 'C50 H74 I2 N4 O2 Si4 Yb2' _chemical_formula_structural 'C50 H74 I2 N4 O2 Si4 Yb2' _chemical_formula_sum 'C50 H74 I2 N4 O2 Si4 Yb2' _chemical_formula_weight 1475.37 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.0479(4) _cell_length_b 15.8523(7) _cell_length_c 12.3722(6) _cell_angle_alpha 90 _cell_angle_beta 96.760(3) _cell_angle_gamma 90 _cell_volume 2930.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8713 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.345 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.454 _exptl_absorpt_correction_T_max 0.527 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 14868 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_unetI/netI 0.0573 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 5121 _reflns_number_gt 4096 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0364P)^2^+1.1085P] 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_number_reflns 5121 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.053 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.895 _refine_diff_density_min -1.071 _refine_diff_density_rms 0.214 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.385 5.5486 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Yb Yb -0.140542(15) 0.034092(16) 0.02248(2) 0.02145(10) Uani 1 1 d . . . I I 0.04722(2) 0.02572(3) 0.17433(3) 0.02928(12) Uani 1 1 d . . . Si1 Si -0.20119(10) -0.16719(11) 0.15181(14) 0.0271(4) Uani 1 1 d . . . Si2 Si -0.35553(10) 0.05520(11) -0.15880(14) 0.0263(4) Uani 1 1 d . . . O O -0.1216(3) 0.1851(3) 0.0139(3) 0.0345(10) Uani 1 1 d . . . N1 N -0.2070(3) -0.0578(3) 0.1375(4) 0.0212(11) Uani 1 1 d . . . N2 N -0.2948(3) 0.0637(3) -0.0311(4) 0.0227(11) Uani 1 1 d . . . C1 C -0.2366(3) -0.0006(4) 0.2024(5) 0.0237(13) Uani 1 1 d . . . C2 C -0.2725(3) 0.0792(4) 0.1653(5) 0.0237(13) Uani 1 1 d . . . H2 H -0.2693 0.1228 0.2183 0.028 Uiso 1 1 calc R . . C3 C -0.3124(3) 0.1019(4) 0.0591(5) 0.0217(13) Uani 1 1 d . . . C4 C -0.2309(4) -0.0147(4) 0.3231(5) 0.0240(13) Uani 1 1 d . . . C5 C -0.1500(4) -0.0352(4) 0.3821(5) 0.0302(14) Uani 1 1 d . . . H5 H -0.0976 -0.0401 0.3464 0.036 Uiso 1 1 calc R . . C6 C -0.1452(4) -0.0487(4) 0.4945(5) 0.0359(16) Uani 1 1 d . . . H6 H -0.0896 -0.0628 0.5349 0.043 Uiso 1 1 calc R . . C7 C -0.2205(4) -0.0418(4) 0.5466(5) 0.0380(16) Uani 1 1 d . . . H7 H -0.2167 -0.0512 0.6229 0.046 Uiso 1 1 calc R . . C8 C -0.3003(5) -0.0215(4) 0.4897(5) 0.0406(18) Uani 1 1 d . . . H8 H -0.3523 -0.0173 0.5261 0.049 Uiso 1 1 calc R . . C9 C -0.3062(4) -0.0069(4) 0.3780(5) 0.0334(15) Uani 1 1 d . . . H9 H -0.362 0.0086 0.3389 0.04 Uiso 1 1 calc R . . C10 C -0.3776(3) 0.1738(4) 0.0548(5) 0.0256(13) Uani 1 1 d . . . C11 C -0.4453(4) 0.1767(4) 0.1214(5) 0.0334(15) Uani 1 1 d . . . H11 H -0.4487 0.1341 0.1748 0.04 Uiso 1 1 calc R . . C12 C -0.5076(4) 0.2405(5) 0.1114(6) 0.0466(19) Uani 1 1 d . . . H12 H -0.5546 0.2405 0.1564 0.056 Uiso 1 1 calc R . . C13 C -0.5028(4) 0.3045(5) 0.0367(7) 0.050(2) Uani 1 1 d . . . H13 H -0.546 0.3485 0.0299 0.061 Uiso 1 1 calc R . . C14 C -0.4340(5) 0.3034(4) -0.0281(6) 0.0468(19) Uani 1 1 d . . . H14 H -0.4291 0.3477 -0.0787 0.056 Uiso 1 1 calc R . . C15 C -0.3722(4) 0.2385(4) -0.0201(5) 0.0295(14) Uani 1 1 d . . . H15 H -0.3258 0.2382 -0.0659 0.035 Uiso 1 1 calc R . . C16 C -0.1952(6) -0.2060(5) 0.0110(6) 0.064(2) Uani 1 1 d . . . H16A H -0.2473 -0.1857 -0.0368 0.096 Uiso 1 1 calc R . . H16B H -0.1947 -0.2678 0.0109 0.096 Uiso 1 1 calc R . . H16C H -0.1404 -0.185 -0.0153 0.096 Uiso 1 1 calc R . . C17 C -0.3039(4) -0.2094(5) 0.2028(7) 0.053(2) Uani 1 1 d . . . H17A H -0.3071 -0.1889 0.2769 0.08 Uiso 1 1 calc R . . H17B H -0.3018 -0.2712 0.203 0.08 Uiso 1 1 calc R . . H17C H -0.3567 -0.1903 0.1552 0.08 Uiso 1 1 calc R . . C18 C -0.1018(4) -0.2068(5) 0.2414(6) 0.0438(18) Uani 1 1 d . . . H18A H -0.1043 -0.1868 0.3159 0.066 Uiso 1 1 calc R . . H18B H -0.0471 -0.186 0.2148 0.066 Uiso 1 1 calc R . . H18C H -0.1018 -0.2687 0.2407 0.066 Uiso 1 1 calc R . . C19 C -0.3436(4) -0.0564(4) -0.1978(5) 0.0369(16) Uani 1 1 d . . . H19A H -0.28 -0.0701 -0.1968 0.055 Uiso 1 1 calc R . . H19B H -0.3743 -0.0656 -0.2711 0.055 Uiso 1 1 calc R . . H19C H -0.3701 -0.0928 -0.1461 0.055 Uiso 1 1 calc R . . C20 C -0.4775(4) 0.0773(5) -0.1624(6) 0.0442(18) Uani 1 1 d . . . H20A H -0.4861 0.1362 -0.1418 0.066 Uiso 1 1 calc R . . H20B H -0.5032 0.0399 -0.1111 0.066 Uiso 1 1 calc R . . H20C H -0.5072 0.0675 -0.2361 0.066 Uiso 1 1 calc R . . C21 C -0.3044(5) 0.1225(4) -0.2584(5) 0.0399(17) Uani 1 1 d . . . H21A H -0.31 0.182 -0.2388 0.06 Uiso 1 1 calc R . . H21B H -0.3354 0.1128 -0.3315 0.06 Uiso 1 1 calc R . . H21C H -0.241 0.108 -0.2572 0.06 Uiso 1 1 calc R . . C22 C -0.1209(5) 0.2458(5) 0.1012(6) 0.0483(19) Uani 1 1 d . . . H22A H -0.0711 0.2339 0.1589 0.058 Uiso 1 1 calc R . . H22B H -0.178 0.244 0.1335 0.058 Uiso 1 1 calc R . . C23 C -0.1084(6) 0.3308(5) 0.0502(7) 0.066(2) Uani 1 1 d . . . H23A H -0.1658 0.3618 0.039 0.079 Uiso 1 1 calc R . . H23B H -0.0643 0.3651 0.097 0.079 Uiso 1 1 calc R . . C24 C -0.0758(8) 0.3126(6) -0.0537(10) 0.099(4) Uani 1 1 d . . . H24A H -0.1024 0.3524 -0.1102 0.119 Uiso 1 1 calc R . . H24B H -0.0099 0.3182 -0.0471 0.119 Uiso 1 1 calc R . . C25 C -0.1018(6) 0.2280(5) -0.0824(7) 0.066(2) Uani 1 1 d . . . H25A H -0.0527 0.1988 -0.1139 0.079 Uiso 1 1 calc R . . H25B H -0.1552 0.2283 -0.1374 0.079 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 Yb 0.01932(14) 0.02259(16) 0.02277(16) 0.00274(11) 0.00381(10) 0.00214(10) I 0.0226(2) 0.0418(3) 0.0230(2) -0.00381(18) 0.00141(16) 0.00143(16) Si1 0.0299(9) 0.0203(9) 0.0319(10) 0.0035(8) 0.0072(7) 0.0031(7) Si2 0.0266(8) 0.0275(10) 0.0235(9) -0.0005(8) -0.0024(7) 0.0012(7) O 0.045(2) 0.023(3) 0.036(3) 0.000(2) 0.008(2) -0.0045(18) N1 0.025(2) 0.018(3) 0.021(3) 0.000(2) 0.007(2) -0.0008(19) N2 0.017(2) 0.022(3) 0.029(3) 0.001(2) 0.003(2) 0.0025(18) C1 0.019(3) 0.031(3) 0.021(3) 0.002(3) 0.000(2) -0.003(2) C2 0.024(3) 0.024(3) 0.022(3) 0.000(3) -0.001(2) 0.003(2) C3 0.020(3) 0.016(3) 0.030(3) 0.000(3) 0.002(2) 0.001(2) C4 0.028(3) 0.020(3) 0.024(3) -0.003(3) 0.002(2) -0.004(2) C5 0.036(3) 0.026(4) 0.027(3) 0.000(3) -0.002(3) 0.004(3) C6 0.048(4) 0.029(4) 0.028(4) 0.001(3) -0.009(3) 0.006(3) C7 0.053(4) 0.038(4) 0.023(3) 0.004(3) 0.004(3) 0.000(3) C8 0.046(4) 0.054(5) 0.023(4) -0.004(3) 0.011(3) -0.011(3) C9 0.035(3) 0.040(4) 0.025(4) -0.002(3) 0.004(3) -0.007(3) C10 0.023(3) 0.021(3) 0.031(3) 0.001(3) -0.005(2) 0.002(2) C11 0.033(3) 0.027(4) 0.043(4) 0.000(3) 0.016(3) 0.003(3) C12 0.034(4) 0.039(5) 0.068(5) -0.015(4) 0.011(3) 0.012(3) C13 0.041(4) 0.031(4) 0.077(6) -0.008(4) -0.007(4) 0.015(3) C14 0.066(5) 0.026(4) 0.046(4) 0.000(3) -0.006(4) 0.009(3) C15 0.032(3) 0.030(4) 0.027(4) 0.000(3) 0.006(3) 0.002(3) C16 0.124(7) 0.029(4) 0.037(4) -0.007(4) 0.004(4) 0.024(5) C17 0.039(4) 0.033(4) 0.089(6) 0.010(4) 0.014(4) -0.004(3) C18 0.044(4) 0.031(4) 0.056(5) 0.009(4) 0.004(3) 0.002(3) C19 0.045(4) 0.034(4) 0.032(4) -0.001(3) 0.003(3) -0.006(3) C20 0.023(3) 0.061(5) 0.046(4) -0.014(4) -0.008(3) 0.003(3) C21 0.059(4) 0.031(4) 0.028(4) 0.002(3) -0.002(3) -0.001(3) C22 0.059(5) 0.044(5) 0.041(4) -0.011(4) 0.003(3) -0.012(4) C23 0.092(6) 0.033(5) 0.071(6) -0.009(4) 0.002(5) -0.007(4) C24 0.162(10) 0.026(5) 0.123(9) -0.004(6) 0.074(8) -0.018(6) C25 0.103(7) 0.042(5) 0.058(6) 0.003(4) 0.036(5) -0.014(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Yb N1 2.342(4) . ? Yb N2 2.385(4) . ? Yb O 2.414(4) . ? Yb C1 2.847(6) . ? Yb C3 2.885(5) . ? Yb C2 2.899(6) . ? Yb I 3.0993(5) 3 ? Yb I 3.2063(4) . ? I Yb 3.0993(5) 3 ? Si1 N1 1.745(5) . ? Si1 C16 1.860(7) . ? Si1 C17 1.861(7) . ? Si1 C18 1.863(6) . ? Si2 N2 1.734(5) . ? Si2 C19 1.848(7) . ? Si2 C21 1.863(7) . ? Si2 C20 1.863(6) . ? O C25 1.434(8) . ? O C22 1.445(8) . ? N1 C1 1.323(8) . ? N2 C3 1.324(7) . ? C1 C2 1.429(8) . ? C1 C4 1.502(8) . ? C2 C3 1.425(8) . ? C3 C10 1.501(7) . ? C4 C5 1.383(8) . ? C4 C9 1.392(8) . ? C5 C6 1.401(9) . ? C6 C7 1.372(9) . ? C7 C8 1.358(9) . ? C8 C9 1.395(9) . ? C10 C11 1.385(8) . ? C10 C15 1.391(8) . ? C11 C12 1.375(9) . ? C12 C13 1.381(10) . ? C13 C14 1.382(10) . ? C14 C15 1.382(9) . ? C22 C23 1.509(10) . ? C23 C24 1.457(12) . ? C24 C25 1.430(11) . ? 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 Yb N2 79.63(15) . . ? N1 Yb O 134.78(15) . . ? N2 Yb O 84.75(15) . . ? N1 Yb C1 27.38(17) . . ? N2 Yb C1 71.83(15) . . ? O Yb C1 107.40(16) . . ? N1 Yb C3 71.41(15) . . ? N2 Yb C3 27.02(15) . . ? O Yb C3 75.53(15) . . ? C1 Yb C3 53.27(16) . . ? N1 Yb C2 53.87(15) . . ? N2 Yb C2 53.61(15) . . ? O Yb C2 82.83(15) . . ? C1 Yb C2 28.78(16) . . ? C3 Yb C2 28.53(15) . . ? N1 Yb I 123.57(11) . 3 ? N2 Yb I 110.97(12) . 3 ? O Yb I 101.66(10) . 3 ? C1 Yb I 150.94(13) . 3 ? C3 Yb I 137.28(11) . 3 ? C2 Yb I 163.87(10) . 3 ? N1 Yb I 91.62(11) . . ? N2 Yb I 158.90(12) . . ? O Yb I 88.08(9) . . ? C1 Yb I 91.58(10) . . ? C3 Yb I 131.90(11) . . ? C2 Yb I 105.83(10) . . ? I Yb I 89.894(11) 3 . ? Yb I Yb 90.106(11) 3 . ? N1 Si1 C16 104.0(3) . . ? N1 Si1 C17 111.0(3) . . ? C16 Si1 C17 109.4(4) . . ? N1 Si1 C18 115.0(3) . . ? C16 Si1 C18 108.8(3) . . ? C17 Si1 C18 108.5(3) . . ? N2 Si2 C19 104.8(3) . . ? N2 Si2 C21 110.1(3) . . ? C19 Si2 C21 108.4(3) . . ? N2 Si2 C20 114.7(3) . . ? C19 Si2 C20 107.5(3) . . ? C21 Si2 C20 111.0(3) . . ? C25 O C22 108.7(5) . . ? C25 O Yb 123.0(4) . . ? C22 O Yb 128.2(4) . . ? C1 N1 Si1 129.6(4) . . ? C1 N1 Yb 98.1(4) . . ? Si1 N1 Yb 131.3(2) . . ? C3 N2 Si2 131.9(4) . . ? C3 N2 Yb 98.1(3) . . ? Si2 N2 Yb 129.0(2) . . ? N1 C1 C2 123.6(5) . . ? N1 C1 C4 121.1(5) . . ? C2 C1 C4 115.3(5) . . ? N1 C1 Yb 54.5(3) . . ? C2 C1 Yb 77.6(3) . . ? C4 C1 Yb 146.2(4) . . ? C3 C2 C1 128.5(5) . . ? C3 C2 Yb 75.2(3) . . ? C1 C2 Yb 73.6(3) . . ? N2 C3 C2 123.9(5) . . ? N2 C3 C10 120.8(5) . . ? C2 C3 C10 115.3(5) . . ? N2 C3 Yb 54.9(3) . . ? C2 C3 Yb 76.3(3) . . ? C10 C3 Yb 150.6(4) . . ? C5 C4 C9 118.7(6) . . ? C5 C4 C1 120.2(5) . . ? C9 C4 C1 121.1(5) . . ? C4 C5 C6 119.9(6) . . ? C7 C6 C5 120.4(6) . . ? C8 C7 C6 120.3(6) . . ? C7 C8 C9 120.2(6) . . ? C4 C9 C8 120.5(6) . . ? C11 C10 C15 118.4(5) . . ? C11 C10 C3 121.8(5) . . ? C15 C10 C3 119.7(5) . . ? C12 C11 C10 120.9(6) . . ? C11 C12 C13 120.8(6) . . ? C12 C13 C14 118.7(6) . . ? C13 C14 C15 120.8(7) . . ? C14 C15 C10 120.3(6) . . ? O C22 C23 105.9(6) . . ? C24 C23 C22 105.3(7) . . ? C25 C24 C23 107.1(8) . . ? C24 C25 O 108.4(7) . . ? #===END data_(4)-mar2604 _database_code_depnum_ccdc_archive 'CCDC 706862' _audit_creation_date 2004-03-24T14:15:26-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C31 H55 N3 O1 Si4 Yb1' _chemical_formula_sum 'C31 H55 N3 O1 Si4 Yb1' _chemical_formula_weight 771.18 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 9.8514(2) _cell_length_b 21.2659(4) _cell_length_c 19.0709(4) _cell_angle_alpha 90 _cell_angle_beta 101.922(1) _cell_angle_gamma 90 _cell_volume 3909.15(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 21206 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.31 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.54 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6083 _exptl_absorpt_correction_T_max 0.6915 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.299811E-1 _diffrn_orient_matrix_ub_12 -0.105378E-1 _diffrn_orient_matrix_ub_13 -0.520032E-1 _diffrn_orient_matrix_ub_21 -0.976484E-1 _diffrn_orient_matrix_ub_22 0.114787E-1 _diffrn_orient_matrix_ub_23 0.18223E-2 _diffrn_orient_matrix_ub_31 0.181429E-1 _diffrn_orient_matrix_ub_32 0.443668E-1 _diffrn_orient_matrix_ub_33 -0.12823E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_unetI/netI 0.0417 _diffrn_reflns_number 33366 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.8 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 6902 _reflns_number_gt 5605 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; There is disorder of one C atom in the thf ligand, and the two alternative positions were left isotropic. 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^)+(0.0231P)^2^+3.0555P] 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_number_reflns 6902 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0602 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.411 _refine_diff_density_min -0.8 _refine_diff_density_rms 0.081 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.385 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Yb Yb 0.398191(16) 0.070022(7) 0.732495(8) 0.02484(6) Uani 1 1 d . B . Si1 Si 0.23300(12) 0.11840(6) 0.56592(6) 0.0381(3) Uani 1 1 d . B . Si2 Si 0.39150(11) 0.10599(6) 0.90636(6) 0.0343(3) Uani 1 1 d . B . Si3 Si 0.29445(14) -0.08642(5) 0.74328(7) 0.0401(3) Uani 1 1 d . B . Si4 Si 0.59012(13) -0.06177(5) 0.73057(6) 0.0364(3) Uani 1 1 d . B . O O 0.5392(3) 0.16386(13) 0.73728(17) 0.0428(7) Uani 1 1 d . . . N1 N 0.1994(3) 0.11269(14) 0.65203(16) 0.0277(7) Uani 1 1 d . . . N2 N 0.2802(3) 0.10583(14) 0.82276(16) 0.0267(7) Uani 1 1 d . . . N3 N 0.4268(3) -0.03928(14) 0.73271(17) 0.0324(8) Uani 1 1 d . . . C1 C 0.0818(4) 0.12690(18) 0.6718(2) 0.0293(8) Uani 1 1 d . B . C2 C 0.0575(4) 0.12751(19) 0.7417(2) 0.0335(9) Uani 1 1 d . . . H2 H -0.0363 0.1356 0.744 0.04 Uiso 1 1 calc R B . C3 C 0.1451(4) 0.11842(17) 0.8090(2) 0.0273(8) Uani 1 1 d . B . C4 C -0.0463(4) 0.1432(2) 0.6172(2) 0.0355(10) Uani 1 1 d . . . C5 C -0.0896(5) 0.2053(2) 0.6054(3) 0.0516(12) Uani 1 1 d . B . H5 H -0.0349 0.2382 0.6305 0.062 Uiso 1 1 calc R . . C6 C -0.2119(5) 0.2198(3) 0.5574(3) 0.0663(16) Uani 1 1 d . . . H6 H -0.2406 0.2623 0.5495 0.08 Uiso 1 1 calc R B . C7 C -0.2907(5) 0.1724(3) 0.5216(3) 0.0676(16) Uani 1 1 d . B . H7 H -0.374 0.1822 0.4885 0.081 Uiso 1 1 calc R . . C8 C -0.2513(5) 0.1108(3) 0.5329(3) 0.0643(15) Uani 1 1 d . . . H8 H -0.3071 0.0783 0.5076 0.077 Uiso 1 1 calc R B . C9 C -0.1280(4) 0.0958(3) 0.5819(2) 0.0502(12) Uani 1 1 d . B . H9 H -0.1013 0.0532 0.5905 0.06 Uiso 1 1 calc R . . C10 C 0.0683(4) 0.12245(19) 0.86982(19) 0.0296(9) Uani 1 1 d . . . C11 C 0.0051(4) 0.0689(2) 0.8904(2) 0.0436(10) Uani 1 1 d . B . H11 H 0.012 0.0301 0.8667 0.052 Uiso 1 1 calc R . . C12 C -0.0674(5) 0.0719(3) 0.9450(3) 0.0557(13) Uani 1 1 d . . . H12 H -0.1104 0.0352 0.9588 0.067 Uiso 1 1 calc R B . C13 C -0.0776(5) 0.1280(3) 0.9797(3) 0.0706(17) Uani 1 1 d . B . H13 H -0.1269 0.1299 1.0175 0.085 Uiso 1 1 calc R . . C14 C -0.0165(6) 0.1811(3) 0.9596(3) 0.0738(18) Uani 1 1 d . . . H14 H -0.0235 0.2197 0.9837 0.089 Uiso 1 1 calc R B . C15 C 0.0559(5) 0.1790(2) 0.9041(3) 0.0498(12) Uani 1 1 d . B . H15 H 0.0965 0.2161 0.8898 0.06 Uiso 1 1 calc R . . C16 C 0.2467(7) 0.2013(3) 0.5380(3) 0.091(2) Uani 1 1 d . . . H16A H 0.3081 0.2245 0.5764 0.136 Uiso 1 1 calc R B . H16B H 0.1545 0.2207 0.5284 0.136 Uiso 1 1 calc R . . H16C H 0.2849 0.2026 0.4945 0.136 Uiso 1 1 calc R . . C17 C 0.1169(6) 0.0754(4) 0.4931(3) 0.101(3) Uani 1 1 d . . . H17A H 0.1093 0.0315 0.5074 0.152 Uiso 1 1 calc R B . H17B H 0.155 0.077 0.4496 0.152 Uiso 1 1 calc R . . H17C H 0.0248 0.0949 0.4838 0.152 Uiso 1 1 calc R . . C18 C 0.4082(5) 0.0812(3) 0.5744(3) 0.0627(15) Uani 1 1 d . . . H18A H 0.4038 0.0372 0.589 0.094 Uiso 1 1 calc R B . H18B H 0.4758 0.1039 0.6105 0.094 Uiso 1 1 calc R . . H18C H 0.4365 0.0832 0.5281 0.094 Uiso 1 1 calc R . . C19 C 0.4409(6) 0.1876(3) 0.9364(3) 0.0707(16) Uani 1 1 d . . . H19A H 0.3594 0.2098 0.9458 0.106 Uiso 1 1 calc R B . H19B H 0.4766 0.2097 0.8989 0.106 Uiso 1 1 calc R . . H19C H 0.5129 0.1862 0.9804 0.106 Uiso 1 1 calc R . . C20 C 0.3348(5) 0.0617(3) 0.9794(2) 0.0588(14) Uani 1 1 d . . . H20A H 0.2505 0.081 0.9895 0.088 Uiso 1 1 calc R B . H20B H 0.4084 0.0629 1.0227 0.088 Uiso 1 1 calc R . . H20C H 0.3154 0.018 0.9645 0.088 Uiso 1 1 calc R . . C21 C 0.5519(4) 0.0670(2) 0.8897(2) 0.0435(10) Uani 1 1 d . . . H21A H 0.5304 0.0236 0.8739 0.065 Uiso 1 1 calc R B . H21B H 0.6231 0.0669 0.934 0.065 Uiso 1 1 calc R . . H21C H 0.5864 0.09 0.8524 0.065 Uiso 1 1 calc R . . C22 C 0.1236(5) -0.0468(2) 0.7088(3) 0.0660(15) Uani 1 1 d . . . H22A H 0.1166 -0.0351 0.6585 0.099 Uiso 1 1 calc R B . H22B H 0.1169 -0.0089 0.7372 0.099 Uiso 1 1 calc R . . H22C H 0.0479 -0.0757 0.7127 0.099 Uiso 1 1 calc R . . C23 C 0.2988(7) -0.1068(3) 0.8391(3) 0.0818(19) Uani 1 1 d . . . H23A H 0.3866 -0.1279 0.8595 0.123 Uiso 1 1 calc R B . H23B H 0.2213 -0.135 0.8419 0.123 Uiso 1 1 calc R . . H23C H 0.2907 -0.0683 0.8662 0.123 Uiso 1 1 calc R . . C24 C 0.2871(7) -0.1635(2) 0.6949(3) 0.0804(19) Uani 1 1 d . . . H24A H 0.2847 -0.1558 0.644 0.121 Uiso 1 1 calc R B . H24B H 0.2034 -0.1864 0.7 0.121 Uiso 1 1 calc R . . H24C H 0.3693 -0.1885 0.7154 0.121 Uiso 1 1 calc R . . C25 C 0.6798(6) -0.1070(2) 0.8118(2) 0.0597(14) Uani 1 1 d . . . H25A H 0.6268 -0.1451 0.8168 0.09 Uiso 1 1 calc R B . H25B H 0.6861 -0.0808 0.8547 0.09 Uiso 1 1 calc R . . H25C H 0.7734 -0.1186 0.8064 0.09 Uiso 1 1 calc R . . C26 C 0.6060(5) -0.1092(2) 0.6493(2) 0.0543(13) Uani 1 1 d . . . H26A H 0.5605 -0.0867 0.6059 0.081 Uiso 1 1 calc R B . H26B H 0.5615 -0.1502 0.6511 0.081 Uiso 1 1 calc R . . H26C H 0.7043 -0.1153 0.6485 0.081 Uiso 1 1 calc R . . C27 C 0.7016(5) 0.0096(2) 0.7272(3) 0.0519(12) Uani 1 1 d . . . H27A H 0.6604 0.0355 0.6857 0.078 Uiso 1 1 calc R B . H27B H 0.7947 -0.0037 0.7228 0.078 Uiso 1 1 calc R . . H27C H 0.7077 0.0341 0.7712 0.078 Uiso 1 1 calc R . . C28 C 0.6857(5) 0.1769(2) 0.7443(4) 0.0698(17) Uani 1 1 d . B . H28A H 0.741 0.1505 0.7826 0.084 Uiso 1 1 calc R A 1 H28B H 0.715 0.1676 0.6988 0.084 Uiso 1 1 calc R A 1 C29 C 0.7066(7) 0.2420(3) 0.7618(5) 0.124(3) Uani 0.474(15) 1 d P B 1 H29A H 0.7816 0.2599 0.7406 0.149 Uiso 0.474(15) 1 calc PR B 1 H29B H 0.7299 0.2483 0.8144 0.149 Uiso 0.474(15) 1 calc PR B 1 C30 C 0.5651(12) 0.2718(5) 0.7286(8) 0.062(4) Uiso 0.474(15) 1 d P B 1 H30C H 0.5492 0.3109 0.754 0.074 Uiso 0.474(15) 1 calc PR B 1 H30D H 0.5578 0.2812 0.6771 0.074 Uiso 0.474(15) 1 calc PR B 1 C31 C 0.4688(5) 0.2225(2) 0.7390(3) 0.0606(15) Uani 0.474(15) 1 d P B 1 H31A H 0.4411 0.2279 0.7856 0.073 Uiso 0.474(15) 1 calc PR B 1 H31B H 0.3844 0.2239 0.7004 0.073 Uiso 0.474(15) 1 calc PR B 1 C29A C 0.7066(7) 0.2420(3) 0.7618(5) 0.124(3) Uani 0.526(15) 1 d P B 2 H29C H 0.7813 0.2463 0.8051 0.149 Uiso 0.526(15) 1 calc PR B 2 H29D H 0.7364 0.2641 0.7219 0.149 Uiso 0.526(15) 1 calc PR B 2 C30A C 0.5830(10) 0.2701(5) 0.7747(7) 0.059(3) Uiso 0.526(15) 1 d P B 2 H30A H 0.5677 0.312 0.752 0.071 Uiso 0.526(15) 1 calc PR B 2 H30B H 0.5858 0.2742 0.8267 0.071 Uiso 0.526(15) 1 calc PR B 2 C31A C 0.4688(5) 0.2225(2) 0.7390(3) 0.0606(15) Uani 0.526(15) 1 d P B 2 H31C H 0.3958 0.2187 0.7675 0.073 Uiso 0.526(15) 1 calc PR B 2 H31D H 0.4254 0.2362 0.6899 0.073 Uiso 0.526(15) 1 calc PR B 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 Yb 0.02001(8) 0.02600(9) 0.03031(9) 0.00117(7) 0.00935(6) 0.00157(7) Si1 0.0259(6) 0.0596(8) 0.0307(6) 0.0102(5) 0.0106(5) -0.0023(5) Si2 0.0250(6) 0.0492(7) 0.0279(6) -0.0056(5) 0.0034(4) 0.0019(5) Si3 0.0502(8) 0.0305(6) 0.0440(7) -0.0017(5) 0.0199(6) -0.0059(5) Si4 0.0420(7) 0.0345(6) 0.0349(6) 0.0019(5) 0.0129(5) 0.0123(5) O 0.0278(15) 0.0335(16) 0.072(2) -0.0007(14) 0.0222(14) -0.0031(13) N1 0.0201(16) 0.0349(18) 0.0290(17) 0.0059(14) 0.0073(13) 0.0008(14) N2 0.0185(16) 0.0333(18) 0.0296(17) -0.0006(13) 0.0083(13) 0.0042(13) N3 0.037(2) 0.0243(16) 0.0391(19) -0.0019(14) 0.0138(16) 0.0015(14) C1 0.0222(19) 0.034(2) 0.032(2) 0.0043(16) 0.0066(16) -0.0002(16) C2 0.0190(19) 0.054(3) 0.028(2) 0.0077(18) 0.0068(16) 0.0063(18) C3 0.024(2) 0.029(2) 0.031(2) -0.0006(16) 0.0108(16) 0.0001(16) C4 0.022(2) 0.059(3) 0.027(2) 0.0101(19) 0.0097(16) 0.0061(19) C5 0.038(3) 0.062(3) 0.055(3) 0.024(2) 0.009(2) 0.005(2) C6 0.046(3) 0.084(4) 0.068(4) 0.041(3) 0.009(3) 0.020(3) C7 0.037(3) 0.115(5) 0.048(3) 0.028(3) 0.003(2) 0.015(3) C8 0.031(3) 0.113(5) 0.048(3) -0.013(3) 0.006(2) -0.003(3) C9 0.028(2) 0.078(3) 0.043(3) -0.004(2) 0.004(2) 0.006(2) C10 0.0175(18) 0.045(2) 0.027(2) -0.0002(17) 0.0048(15) -0.0008(17) C11 0.028(2) 0.061(3) 0.043(2) 0.005(2) 0.0123(18) 0.002(2) C12 0.032(2) 0.092(4) 0.046(3) 0.018(3) 0.015(2) -0.002(3) C13 0.037(3) 0.134(6) 0.048(3) -0.007(3) 0.025(2) -0.006(3) C14 0.057(3) 0.100(5) 0.076(4) -0.040(3) 0.038(3) -0.007(3) C15 0.041(3) 0.059(3) 0.057(3) -0.014(2) 0.028(2) -0.001(2) C16 0.109(5) 0.083(4) 0.096(5) 0.049(4) 0.059(4) 0.020(4) C17 0.067(4) 0.202(8) 0.043(3) -0.035(4) 0.030(3) -0.053(5) C18 0.050(3) 0.106(5) 0.039(3) 0.013(3) 0.026(2) 0.019(3) C19 0.061(4) 0.076(4) 0.070(4) -0.032(3) 0.001(3) -0.005(3) C20 0.040(3) 0.108(4) 0.029(2) 0.015(3) 0.007(2) 0.009(3) C21 0.025(2) 0.067(3) 0.038(2) 0.007(2) 0.0030(17) 0.007(2) C22 0.041(3) 0.057(3) 0.101(4) 0.006(3) 0.018(3) -0.012(2) C23 0.095(5) 0.098(5) 0.061(4) 0.012(3) 0.035(3) -0.024(4) C24 0.098(5) 0.045(3) 0.113(5) -0.021(3) 0.057(4) -0.026(3) C25 0.072(4) 0.064(3) 0.045(3) 0.005(2) 0.016(3) 0.034(3) C26 0.062(3) 0.057(3) 0.047(3) -0.004(2) 0.019(2) 0.013(3) C27 0.037(3) 0.058(3) 0.064(3) 0.003(2) 0.018(2) 0.009(2) C28 0.031(3) 0.052(3) 0.134(5) 0.004(3) 0.037(3) -0.006(2) C29 0.048(4) 0.055(4) 0.266(11) -0.021(5) 0.024(5) -0.017(3) C31 0.038(3) 0.032(3) 0.113(5) 0.000(3) 0.020(3) 0.002(2) C29A 0.048(4) 0.055(4) 0.266(11) -0.021(5) 0.024(5) -0.017(3) C31A 0.038(3) 0.032(3) 0.113(5) 0.000(3) 0.020(3) 0.002(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Yb N3 2.341(3) . ? Yb N2 2.392(3) . ? Yb N1 2.403(3) . ? Yb O 2.422(3) . ? Si1 N1 1.745(3) . ? Si1 C17 1.848(5) . ? Si1 C16 1.855(6) . ? Si1 C18 1.874(5) . ? Si2 N2 1.738(3) . ? Si2 C19 1.860(5) . ? Si2 C20 1.860(5) . ? Si2 C21 1.869(4) . ? Si3 N3 1.690(3) . ? Si3 C23 1.871(5) . ? Si3 C24 1.875(5) . ? Si3 C22 1.876(5) . ? Si4 N3 1.687(3) . ? Si4 C27 1.882(5) . ? Si4 C25 1.882(5) . ? Si4 C26 1.883(4) . ? O C31 1.430(5) . ? O C28 1.449(5) . ? N1 C1 1.325(5) . ? N2 C3 1.330(5) . ? C1 C2 1.402(5) . ? C1 C4 1.501(5) . ? C2 C3 1.404(5) . ? C3 C10 1.512(5) . ? C4 C9 1.375(6) . ? C4 C5 1.393(6) . ? C5 C6 1.389(6) . ? C6 C7 1.366(8) . ? C7 C8 1.370(8) . ? C8 C9 1.408(6) . ? C10 C15 1.385(6) . ? C10 C11 1.393(6) . ? C11 C12 1.382(6) . ? C12 C13 1.378(8) . ? C13 C14 1.371(8) . ? C14 C15 1.395(6) . ? C28 C29 1.428(7) . ? C29 C30 1.544(13) . ? C30 C31 1.455(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Yb N2 113.03(11) . . ? N3 Yb N1 117.27(11) . . ? N2 Yb N1 83.46(10) . . ? N3 Yb O 138.58(10) . . ? N2 Yb O 94.05(10) . . ? N1 Yb O 95.64(10) . . ? N1 Si1 C17 117.6(2) . . ? N1 Si1 C16 112.0(2) . . ? C17 Si1 C16 109.0(3) . . ? N1 Si1 C18 103.89(18) . . ? C17 Si1 C18 105.8(3) . . ? C16 Si1 C18 107.8(3) . . ? N2 Si2 C19 111.1(2) . . ? N2 Si2 C20 117.10(19) . . ? C19 Si2 C20 109.9(3) . . ? N2 Si2 C21 103.78(17) . . ? C19 Si2 C21 106.8(2) . . ? C20 Si2 C21 107.4(2) . . ? N3 Si3 C23 113.1(2) . . ? N3 Si3 C24 114.3(2) . . ? C23 Si3 C24 105.6(3) . . ? N3 Si3 C22 110.5(2) . . ? C23 Si3 C22 106.5(3) . . ? C24 Si3 C22 106.2(3) . . ? N3 Si4 C27 109.78(18) . . ? N3 Si4 C25 114.4(2) . . ? C27 Si4 C25 105.2(2) . . ? N3 Si4 C26 114.4(2) . . ? C27 Si4 C26 104.8(2) . . ? C25 Si4 C26 107.4(2) . . ? C31 O C28 108.0(3) . . ? C31 O Yb 116.2(2) . . ? C28 O Yb 135.5(3) . . ? C1 N1 Si1 126.8(3) . . ? C1 N1 Yb 123.3(2) . . ? Si1 N1 Yb 109.81(14) . . ? C3 N2 Si2 126.6(3) . . ? C3 N2 Yb 122.5(2) . . ? Si2 N2 Yb 110.64(14) . . ? Si4 N3 Si3 126.7(2) . . ? Si4 N3 Yb 113.37(16) . . ? Si3 N3 Yb 119.57(16) . . ? N1 C1 C2 127.1(3) . . ? N1 C1 C4 120.9(3) . . ? C2 C1 C4 111.9(3) . . ? C1 C2 C3 132.4(4) . . ? N2 C3 C2 127.5(3) . . ? N2 C3 C10 119.9(3) . . ? C2 C3 C10 112.5(3) . . ? C9 C4 C5 119.1(4) . . ? C9 C4 C1 119.6(4) . . ? C5 C4 C1 121.1(4) . . ? C6 C5 C4 120.7(5) . . ? C7 C6 C5 119.5(5) . . ? C6 C7 C8 120.9(5) . . ? C7 C8 C9 119.9(5) . . ? C4 C9 C8 119.8(5) . . ? C15 C10 C11 119.3(4) . . ? C15 C10 C3 121.2(4) . . ? C11 C10 C3 119.5(3) . . ? C12 C11 C10 120.4(5) . . ? C13 C12 C11 120.1(5) . . ? C14 C13 C12 120.0(5) . . ? C13 C14 C15 120.5(5) . . ? C10 C15 C14 119.7(5) . . ? C29 C28 O 107.5(4) . . ? C28 C29 C30 103.1(7) . . ? C31 C30 C29 101.9(8) . . ? O C31 C30 107.0(6) . . ? #===END data_(5)-apr1503 _database_code_depnum_ccdc_archive 'CCDC 706863' _audit_creation_date 2003-04-14T10:56:34-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C45 H67 N3 O Yb, C6 H6' _chemical_formula_sum 'C51 H73 N3 O Yb' _chemical_formula_weight 917.16 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 10.1873(1) _cell_length_b 12.2671(1) _cell_length_c 20.0249(2) _cell_angle_alpha 79.262(1) _cell_angle_beta 80.762(1) _cell_angle_gamma 76.620(1) _cell_volume 2373.81(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 41437 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.007 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6231 _exptl_absorpt_correction_T_max 0.7422 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.733132E-1 _diffrn_orient_matrix_ub_12 0.293178E-1 _diffrn_orient_matrix_ub_13 0.142733E-1 _diffrn_orient_matrix_ub_21 -0.660032E-1 _diffrn_orient_matrix_ub_22 0.722037E-1 _diffrn_orient_matrix_ub_23 0.7416E-2 _diffrn_orient_matrix_ub_31 -0.246092E-1 _diffrn_orient_matrix_ub_32 -0.334968E-1 _diffrn_orient_matrix_ub_33 0.486243E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_unetI/netI 0.0352 _diffrn_reflns_number 46538 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 10787 _reflns_number_gt 9950 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The H atom on N3 was refined; other H atoms were riding. 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^)+(0.0247P)^2^+1.4580P] 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_number_reflns 10787 _refine_ls_number_parameters 538 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0582 _refine_ls_wR_factor_gt 0.0564 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.839 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.068 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.385 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Yb Yb 0.140379(9) 0.278441(7) 0.229887(4) 0.02318(4) Uani 1 1 d . C . O O -0.09794(15) 0.34671(14) 0.22202(8) 0.0319(3) Uani 1 1 d . . . N1 N 0.19094(19) 0.14178(16) 0.15414(9) 0.0279(4) Uani 1 1 d . . . N2 N 0.1419(2) 0.11345(16) 0.31047(9) 0.0305(4) Uani 1 1 d . . . N3 N 0.2748(2) 0.36345(18) 0.27914(10) 0.0321(4) Uani 1 1 d . . . H3N H 0.271(3) 0.335(2) 0.3185(15) 0.039(8) Uiso 1 1 d . . . C1 C 0.1536(3) 0.0426(2) 0.16918(11) 0.0335(5) Uani 1 1 d . C . C2 C 0.1044(3) -0.0061(2) 0.23509(12) 0.0413(6) Uani 1 1 d . . . H2 H 0.0625 -0.068 0.2359 0.05 Uiso 1 1 calc R C . C3 C 0.1066(3) 0.0215(2) 0.30004(12) 0.0359(5) Uani 1 1 d . C . C4 C 0.1629(4) -0.0297(2) 0.11376(13) 0.0507(7) Uani 1 1 d . . . H4A H 0.1978 0.0095 0.0696 0.076 Uiso 0.5 1 calc PR C . H4B H 0.0725 -0.0421 0.111 0.076 Uiso 0.5 1 calc PR . . H4C H 0.2246 -0.1029 0.125 0.076 Uiso 0.5 1 calc PR . . H4D H 0.1321 -0.0999 0.1342 0.076 Uiso 0.5 1 calc PR . . H4E H 0.2574 -0.0482 0.0927 0.076 Uiso 0.5 1 calc PR . . H4F H 0.1054 0.0125 0.0787 0.076 Uiso 0.5 1 calc PR . . C5 C 0.0652(4) -0.0643(3) 0.36011(13) 0.0556(8) Uani 1 1 d . . . H5A H 0.0695 -0.0387 0.4031 0.083 Uiso 0.5 1 calc PR C . H5B H 0.1272 -0.1381 0.3578 0.083 Uiso 0.5 1 calc PR . . H5C H -0.0279 -0.0717 0.3582 0.083 Uiso 0.5 1 calc PR . . H5D H 0.043 -0.1269 0.343 0.083 Uiso 0.5 1 calc PR . . H5E H -0.0146 -0.0276 0.3883 0.083 Uiso 0.5 1 calc PR . . H5F H 0.1404 -0.094 0.3878 0.083 Uiso 0.5 1 calc PR . . C6 C 0.2457(2) 0.18210(19) 0.08583(11) 0.0295(5) Uani 1 1 d . C . C7 C 0.3871(3) 0.1772(2) 0.07220(13) 0.0363(5) Uani 1 1 d . . . C8 C 0.4396(3) 0.2255(2) 0.00771(15) 0.0467(7) Uani 1 1 d . C . H8 H 0.5347 0.2218 -0.0023 0.056 Uiso 1 1 calc R . . C9 C 0.3565(3) 0.2784(3) -0.04168(14) 0.0492(7) Uani 1 1 d . . . H9 H 0.3941 0.3119 -0.085 0.059 Uiso 1 1 calc R C . C10 C 0.2184(3) 0.2828(2) -0.02824(12) 0.0410(6) Uani 1 1 d . C . H10 H 0.1616 0.3195 -0.0626 0.049 Uiso 1 1 calc R . . C11 C 0.1607(2) 0.2340(2) 0.03520(11) 0.0326(5) Uani 1 1 d . . . C12 C 0.4799(3) 0.1177(3) 0.12617(16) 0.0504(7) Uani 1 1 d . C . H12 H 0.4256 0.1321 0.1711 0.06 Uiso 1 1 calc R . . C13 C 0.6040(4) 0.1645(4) 0.1228(2) 0.0860(13) Uani 1 1 d . . . H13C H 0.6486 0.1317 0.164 0.129 Uiso 1 1 calc R C . H13B H 0.5781 0.2471 0.1201 0.129 Uiso 1 1 calc R . . H13A H 0.6666 0.1454 0.0822 0.129 Uiso 1 1 calc R . . C14 C 0.5118(5) -0.0075(4) 0.1294(3) 0.1111(19) Uani 1 1 d . . . H14C H 0.5716 -0.0276 0.0881 0.167 Uiso 1 1 calc R C . H14B H 0.4273 -0.0344 0.1322 0.167 Uiso 1 1 calc R . . H14A H 0.5574 -0.0431 0.1699 0.167 Uiso 1 1 calc R . . C15 C 0.0085(3) 0.2375(2) 0.04614(12) 0.0358(5) Uani 1 1 d . C . H15 H -0.0138 0.1932 0.0921 0.043 Uiso 1 1 calc R . . C16 C -0.0745(3) 0.3590(2) 0.04518(14) 0.0438(6) Uani 1 1 d . . . H16C H -0.0517 0.3923 0.0816 0.066 Uiso 1 1 calc R C . H16B H -0.1716 0.3579 0.0527 0.066 Uiso 1 1 calc R . . H16A H -0.0531 0.4044 0.0007 0.066 Uiso 1 1 calc R . . C17 C -0.0331(3) 0.1825(3) -0.00817(14) 0.0492(7) Uani 1 1 d . . . H17C H -0.0103 0.2238 -0.0538 0.074 Uiso 1 1 calc R C . H17B H -0.1313 0.1855 0.0002 0.074 Uiso 1 1 calc R . . H17A H 0.0157 0.1033 -0.0055 0.074 Uiso 1 1 calc R . . C18 C 0.1665(2) 0.12350(19) 0.37768(11) 0.0313(5) Uani 1 1 d . C . C19 C 0.2994(3) 0.0857(2) 0.39536(12) 0.0415(6) Uani 1 1 d . . . C20 C 0.3256(3) 0.1040(2) 0.45817(13) 0.0465(7) Uani 1 1 d . C . H20 H 0.4152 0.0788 0.4705 0.056 Uiso 1 1 calc R . . C21 C 0.2248(3) 0.1575(2) 0.50278(12) 0.0436(6) Uani 1 1 d . . . H21 H 0.2447 0.1685 0.5455 0.052 Uiso 1 1 calc R C . C22 C 0.0955(3) 0.1949(2) 0.48504(12) 0.0380(6) Uani 1 1 d . C . H22 H 0.0262 0.2323 0.5158 0.046 Uiso 1 1 calc R . . C23 C 0.0636(3) 0.1790(2) 0.42250(11) 0.0325(5) Uani 1 1 d . . . C24 C 0.4123(3) 0.0224(3) 0.34865(16) 0.0641(10) Uani 1 1 d . C . H24 H 0.3796 0.0305 0.3031 0.077 Uiso 1 1 calc R . . C25 C 0.5398(4) 0.0698(4) 0.3377(2) 0.0949(15) Uani 1 1 d . . . H25C H 0.5194 0.1497 0.3169 0.142 Uiso 1 1 calc R C . H25B H 0.6097 0.0269 0.3074 0.142 Uiso 1 1 calc R . . H25A H 0.5729 0.0634 0.3819 0.142 Uiso 1 1 calc R . . C26 C 0.4445(5) -0.1038(4) 0.3779(3) 0.1057(17) Uani 1 1 d . . . H26C H 0.4756 -0.1136 0.4229 0.159 Uiso 1 1 calc R C . H26B H 0.5161 -0.1438 0.3469 0.159 Uiso 1 1 calc R . . H26A H 0.3625 -0.1349 0.3826 0.159 Uiso 1 1 calc R . . C27 C -0.0799(3) 0.2253(2) 0.40418(13) 0.0417(6) Uani 1 1 d . C . H27 H -0.0848 0.201 0.3598 0.05 Uiso 1 1 calc R . . C28 C -0.1097(3) 0.3542(3) 0.39326(16) 0.0580(8) Uani 1 1 d . . . H28C H -0.1019 0.3803 0.4355 0.087 Uiso 1 1 calc R C . H28B H -0.2021 0.3834 0.381 0.087 Uiso 1 1 calc R . . H28A H -0.0444 0.3818 0.3562 0.087 Uiso 1 1 calc R . . C29 C -0.1876(3) 0.1797(3) 0.45777(17) 0.0657(9) Uani 1 1 d . . . H29C H -0.1697 0.0968 0.4621 0.099 Uiso 1 1 calc R C . H29B H -0.2779 0.2118 0.4434 0.099 Uiso 1 1 calc R . . H29A H -0.1839 0.2012 0.5021 0.099 Uiso 1 1 calc R . . C30 C 0.3104(2) 0.46648(19) 0.27128(11) 0.0262(4) Uani 1 1 d . B . C31 C 0.3251(2) 0.52930(19) 0.20388(11) 0.0272(4) Uani 1 1 d . . . C32 C 0.3504(2) 0.6380(2) 0.19394(13) 0.0341(5) Uani 1 1 d . C . H32 H 0.3576 0.6793 0.1489 0.041 Uiso 1 1 calc R . . C33 C 0.3656(2) 0.6876(2) 0.24825(15) 0.0410(6) Uani 1 1 d . . . H33 H 0.3804 0.7629 0.241 0.049 Uiso 1 1 calc R C . C34 C 0.3586(2) 0.6254(2) 0.31309(14) 0.0406(6) Uani 1 1 d . B . H34 H 0.3719 0.6583 0.3502 0.049 Uiso 1 1 calc R . . C35 C 0.3330(2) 0.5165(2) 0.32631(12) 0.0341(5) Uani 1 1 d . . . C36 C 0.3073(2) 0.4756(2) 0.14462(11) 0.0310(5) Uani 1 1 d . C . H36 H 0.339 0.3918 0.1569 0.037 Uiso 1 1 calc R . . C37 C 0.3871(3) 0.5120(3) 0.07633(14) 0.0540(8) Uani 1 1 d . . . H37C H 0.3591 0.5942 0.0628 0.081 Uiso 1 1 calc R C . H37B H 0.3691 0.4729 0.0414 0.081 Uiso 1 1 calc R . . H37A H 0.4845 0.4925 0.0808 0.081 Uiso 1 1 calc R . . C38 C 0.1558(3) 0.4976(2) 0.13629(13) 0.0371(5) Uani 1 1 d . . . H38A H 0.1447 0.4628 0.0979 0.056 Uiso 1 1 calc R C . H38B H 0.1197 0.5796 0.1273 0.056 Uiso 1 1 calc R . . H38C H 0.1062 0.4646 0.1784 0.056 Uiso 1 1 calc R . . C42 C -0.1742(2) 0.4637(2) 0.21786(14) 0.0375(5) Uani 1 1 d . C . H42B H -0.1517 0.5075 0.1723 0.045 Uiso 1 1 calc R A 1 H42A H -0.1526 0.5008 0.2534 0.045 Uiso 1 1 calc R A 1 C46 C -0.0123(3) 0.6815(3) 0.2895(2) 0.0566(8) Uani 1 1 d . . . H46 H 0.0799 0.663 0.2981 0.068 Uiso 1 1 calc R . . C47 C -0.1112(4) 0.6561(3) 0.34054(17) 0.0624(9) Uani 1 1 d . . . H47 H -0.0888 0.6215 0.385 0.075 Uiso 1 1 calc R . . C48 C -0.2474(4) 0.6817(3) 0.3266(2) 0.0688(11) Uani 1 1 d . . . H48 H -0.3182 0.6638 0.3611 0.083 Uiso 1 1 calc R . . C49 C -0.2752(3) 0.7334(3) 0.2618(2) 0.0652(10) Uani 1 1 d . . . H49 H -0.3662 0.7513 0.2513 0.078 Uiso 1 1 calc R . . C50 C -0.1734(4) 0.7591(3) 0.21272(18) 0.0606(8) Uani 1 1 d . . . H50 H -0.1935 0.7958 0.1683 0.073 Uiso 1 1 calc R . . C51 C -0.0440(3) 0.7325(3) 0.22717(19) 0.0578(8) Uani 1 1 d . . . H51 H 0.0264 0.7503 0.1924 0.069 Uiso 1 1 calc R . . C39 C 0.3234(3) 0.4511(3) 0.39890(13) 0.0469(7) Uani 0.528(6) 1 d P B 1 H39 H 0.3481 0.3684 0.3956 0.056 Uiso 0.528(6) 1 calc PR B 1 C40 C 0.4329(7) 0.4779(7) 0.4407(3) 0.071(2) Uani 0.528(6) 1 d P B 1 H40A H 0.5239 0.4615 0.4152 0.107 Uiso 0.528(6) 1 calc PR B 1 H40B H 0.4321 0.4304 0.4859 0.107 Uiso 0.528(6) 1 calc PR B 1 H40C H 0.409 0.5581 0.4464 0.107 Uiso 0.528(6) 1 calc PR B 1 C41 C 0.1896(6) 0.4740(6) 0.4345(3) 0.0562(17) Uani 0.528(6) 1 d P B 1 H41A H 0.1886 0.4302 0.4808 0.084 Uiso 0.528(6) 1 calc PR B 1 H41B H 0.1264 0.4523 0.4098 0.084 Uiso 0.528(6) 1 calc PR B 1 H41C H 0.1617 0.5551 0.4375 0.084 Uiso 0.528(6) 1 calc PR B 1 C43 C -0.3216(3) 0.4572(3) 0.2293(3) 0.0825(13) Uani 0.575(12) 1 d P C 1 H43A H -0.363 0.4822 0.186 0.099 Uiso 0.575(12) 1 calc PR C 1 H43B H -0.3728 0.5049 0.2636 0.099 Uiso 0.575(12) 1 calc PR C 1 C44 C -0.3206(6) 0.3303(6) 0.2558(4) 0.0487(17) Uani 0.575(12) 1 d P C 1 H44A H -0.3274 0.3144 0.3065 0.058 Uiso 0.575(12) 1 calc PR C 1 H44B H -0.3968 0.3071 0.241 0.058 Uiso 0.575(12) 1 calc PR C 1 C45 C -0.1925(3) 0.2727(2) 0.22561(14) 0.0418(6) Uani 0.575(12) 1 d P C 1 H45A H -0.1999 0.2592 0.1792 0.05 Uiso 0.575(12) 1 calc PR C 1 H45B H -0.1617 0.1987 0.2541 0.05 Uiso 0.575(12) 1 calc PR C 1 C39A C 0.3234(3) 0.4511(3) 0.39890(13) 0.0469(7) Uani 0.472(6) 1 d P B 2 H39A H 0.2582 0.4013 0.3993 0.056 Uiso 0.472(6) 1 calc PR B 2 C40A C 0.4468(6) 0.3736(6) 0.4168(3) 0.0507(18) Uani 0.472(6) 1 d P B 2 H40D H 0.4317 0.3355 0.4641 0.076 Uiso 0.472(6) 1 calc PR B 2 H40E H 0.5194 0.4157 0.4126 0.076 Uiso 0.472(6) 1 calc PR B 2 H40F H 0.4733 0.3169 0.3858 0.076 Uiso 0.472(6) 1 calc PR B 2 C41A C 0.2567(9) 0.5253(8) 0.4553(3) 0.076(3) Uani 0.472(6) 1 d P B 2 H41D H 0.1735 0.5766 0.441 0.113 Uiso 0.472(6) 1 calc PR B 2 H41E H 0.3202 0.5699 0.4623 0.113 Uiso 0.472(6) 1 calc PR B 2 H41F H 0.2342 0.4762 0.4982 0.113 Uiso 0.472(6) 1 calc PR B 2 C43A C -0.3216(3) 0.4572(3) 0.2293(3) 0.0825(13) Uani 0.425(12) 1 d P C 2 H43C H -0.3592 0.4655 0.2773 0.099 Uiso 0.425(12) 1 calc PR C 2 H43D H -0.3733 0.5195 0.1987 0.099 Uiso 0.425(12) 1 calc PR C 2 C44A C -0.3335(8) 0.3599(9) 0.2166(8) 0.059(3) Uani 0.425(12) 1 d P C 2 H44C H -0.3556 0.3679 0.1694 0.071 Uiso 0.425(12) 1 calc PR C 2 H44D H -0.4075 0.3321 0.2488 0.071 Uiso 0.425(12) 1 calc PR C 2 C45A C -0.1925(3) 0.2727(2) 0.22561(14) 0.0418(6) Uani 0.425(12) 1 d P C 2 H45C H -0.197 0.2221 0.2703 0.05 Uiso 0.425(12) 1 calc PR C 2 H45D H -0.1665 0.2259 0.1884 0.05 Uiso 0.425(12) 1 calc PR 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 Yb 0.02791(5) 0.02001(5) 0.02190(5) -0.00202(3) -0.00542(3) -0.00487(4) O 0.0289(8) 0.0300(9) 0.0374(9) -0.0033(7) -0.0066(7) -0.0073(6) N1 0.0388(10) 0.0264(10) 0.0193(8) -0.0010(7) -0.0052(7) -0.0094(8) N2 0.0464(11) 0.0260(10) 0.0194(9) -0.0025(7) -0.0062(8) -0.0075(8) N3 0.0408(11) 0.0343(11) 0.0230(10) 0.0002(8) -0.0057(8) -0.0136(9) C1 0.0538(14) 0.0266(12) 0.0237(11) -0.0033(9) -0.0099(10) -0.0124(10) C2 0.0727(18) 0.0315(13) 0.0264(12) 0.0005(10) -0.0085(11) -0.0266(13) C3 0.0548(15) 0.0272(12) 0.0258(11) 0.0026(9) -0.0061(10) -0.0129(11) C4 0.096(2) 0.0316(14) 0.0304(13) -0.0059(11) -0.0087(14) -0.0236(15) C5 0.102(2) 0.0438(17) 0.0276(13) 0.0048(12) -0.0069(14) -0.0375(17) C6 0.0430(12) 0.0235(11) 0.0237(10) -0.0051(9) -0.0023(9) -0.0107(9) C7 0.0435(13) 0.0337(13) 0.0349(13) -0.0076(10) -0.0034(10) -0.0135(11) C8 0.0456(15) 0.0482(17) 0.0480(16) -0.0098(13) 0.0063(12) -0.0192(13) C9 0.0683(19) 0.0505(17) 0.0299(13) -0.0022(12) 0.0071(12) -0.0267(15) C10 0.0598(16) 0.0398(15) 0.0243(11) 0.0014(10) -0.0044(11) -0.0175(12) C11 0.0468(13) 0.0301(12) 0.0225(10) -0.0040(9) -0.0027(9) -0.0126(10) C12 0.0410(14) 0.0575(19) 0.0532(17) -0.0032(14) -0.0121(12) -0.0114(13) C13 0.066(2) 0.096(3) 0.109(3) -0.005(3) -0.037(2) -0.031(2) C14 0.109(4) 0.055(3) 0.176(5) -0.009(3) -0.083(4) 0.006(2) C15 0.0465(14) 0.0385(14) 0.0242(11) 0.0016(10) -0.0086(10) -0.0146(11) C16 0.0511(15) 0.0487(16) 0.0342(13) -0.0047(12) -0.0148(11) -0.0106(12) C17 0.0635(18) 0.0527(18) 0.0398(15) -0.0074(13) -0.0151(13) -0.0227(14) C18 0.0494(13) 0.0241(11) 0.0196(10) 0.0005(8) -0.0067(9) -0.0072(10) C19 0.0521(15) 0.0425(15) 0.0256(12) -0.0046(11) -0.0087(11) 0.0012(12) C20 0.0518(16) 0.0501(17) 0.0357(14) -0.0049(12) -0.0176(12) 0.0000(13) C21 0.0666(18) 0.0426(15) 0.0239(12) -0.0054(11) -0.0131(11) -0.0105(13) C22 0.0551(15) 0.0342(13) 0.0220(11) -0.0048(10) -0.0039(10) -0.0041(11) C23 0.0487(14) 0.0264(12) 0.0208(10) 0.0016(9) -0.0064(9) -0.0070(10) C24 0.0512(17) 0.091(3) 0.0400(16) -0.0225(17) -0.0114(13) 0.0188(17) C25 0.077(3) 0.091(3) 0.089(3) -0.001(2) 0.031(2) -0.001(2) C26 0.083(3) 0.079(3) 0.154(5) -0.068(3) 0.013(3) 0.007(2) C27 0.0464(14) 0.0482(16) 0.0268(12) -0.0047(11) -0.0050(10) -0.0028(12) C28 0.0653(19) 0.0519(19) 0.0461(17) -0.0038(14) -0.0128(14) 0.0101(15) C29 0.0545(18) 0.086(3) 0.0520(18) 0.0017(17) -0.0027(15) -0.0186(18) C30 0.0196(9) 0.0314(12) 0.0286(11) -0.0083(9) -0.0034(8) -0.0042(8) C31 0.0206(10) 0.0291(12) 0.0325(11) -0.0049(9) -0.0018(8) -0.0073(8) C32 0.0250(11) 0.0338(13) 0.0435(13) -0.0032(10) -0.0027(9) -0.0093(9) C33 0.0306(12) 0.0316(13) 0.0652(18) -0.0147(13) -0.0064(11) -0.0090(10) C34 0.0324(12) 0.0435(15) 0.0536(16) -0.0247(13) -0.0102(11) -0.0063(11) C35 0.0290(11) 0.0420(14) 0.0342(12) -0.0152(11) -0.0067(9) -0.0039(10) C36 0.0353(12) 0.0331(12) 0.0247(11) -0.0026(9) 0.0000(9) -0.0111(10) C37 0.0659(19) 0.068(2) 0.0313(14) -0.0087(13) 0.0116(13) -0.0318(16) C38 0.0461(14) 0.0323(13) 0.0374(13) 0.0017(10) -0.0175(11) -0.0143(11) C42 0.0298(12) 0.0348(13) 0.0443(14) -0.0045(11) -0.0044(10) -0.0010(10) C46 0.0397(15) 0.0483(18) 0.091(3) -0.0335(18) -0.0170(16) -0.0033(13) C47 0.095(3) 0.0399(17) 0.0491(18) -0.0115(14) -0.0192(18) 0.0031(17) C48 0.060(2) 0.0496(19) 0.087(3) -0.0225(18) 0.0351(19) -0.0135(16) C49 0.0387(16) 0.058(2) 0.103(3) -0.033(2) -0.0208(17) 0.0074(14) C50 0.079(2) 0.0453(18) 0.0557(19) -0.0161(15) -0.0153(17) 0.0021(16) C51 0.0585(19) 0.0439(17) 0.073(2) -0.0219(16) 0.0108(16) -0.0166(15) C39 0.0600(17) 0.0544(18) 0.0314(13) -0.0150(12) -0.0141(12) -0.0097(14) C40 0.088(5) 0.095(6) 0.044(3) -0.002(3) -0.038(3) -0.032(4) C41 0.068(4) 0.068(4) 0.033(3) -0.004(3) 0.000(3) -0.023(3) C43 0.0250(14) 0.063(2) 0.151(4) -0.005(2) -0.0070(18) -0.0033(14) C44 0.033(3) 0.070(4) 0.049(4) -0.011(3) 0.004(3) -0.026(3) C45 0.0453(14) 0.0420(15) 0.0444(15) -0.0021(12) -0.0114(11) -0.0214(12) C39A 0.0600(17) 0.0544(18) 0.0314(13) -0.0150(12) -0.0141(12) -0.0097(14) C40A 0.047(3) 0.060(4) 0.041(3) -0.004(3) -0.008(3) -0.005(3) C41A 0.080(5) 0.104(7) 0.036(3) -0.032(4) 0.001(3) 0.005(5) C43A 0.0250(14) 0.063(2) 0.151(4) -0.005(2) -0.0070(18) -0.0033(14) C44A 0.034(4) 0.060(6) 0.088(8) -0.017(6) -0.014(5) -0.009(3) C45A 0.0453(14) 0.0420(15) 0.0444(15) -0.0021(12) -0.0114(11) -0.0214(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Yb N3 2.327(2) . ? Yb N2 2.3403(18) . ? Yb N1 2.3820(18) . ? Yb O 2.3986(15) . ? O C45 1.455(3) . ? O C42 1.459(3) . ? N1 C1 1.325(3) . ? N1 C6 1.434(3) . ? N2 C3 1.322(3) . ? N2 C18 1.440(3) . ? N3 C30 1.369(3) . ? C1 C2 1.408(3) . ? C1 C4 1.523(3) . ? C2 C3 1.408(3) . ? C3 C5 1.518(3) . ? C6 C11 1.403(3) . ? C6 C7 1.412(3) . ? C7 C8 1.395(4) . ? C7 C12 1.519(4) . ? C8 C9 1.375(4) . ? C9 C10 1.380(4) . ? C10 C11 1.399(3) . ? C11 C15 1.522(3) . ? C12 C14 1.486(5) . ? C12 C13 1.492(4) . ? C15 C16 1.531(4) . ? C15 C17 1.540(4) . ? C18 C23 1.401(3) . ? C18 C19 1.405(4) . ? C19 C20 1.394(4) . ? C19 C24 1.521(4) . ? C20 C21 1.377(4) . ? C21 C22 1.372(4) . ? C22 C23 1.401(3) . ? C23 C27 1.518(3) . ? C24 C25 1.511(6) . ? C24 C26 1.528(6) . ? C27 C28 1.520(4) . ? C27 C29 1.533(4) . ? C30 C31 1.428(3) . ? C30 C35 1.429(3) . ? C31 C32 1.388(3) . ? C31 C36 1.513(3) . ? C32 C33 1.386(4) . ? C33 C34 1.378(4) . ? C34 C35 1.389(4) . ? C35 C39 1.524(4) . ? C36 C37 1.521(3) . ? C36 C38 1.535(3) . ? C42 C43 1.501(4) . ? C46 C51 1.341(5) . ? C46 C47 1.361(5) . ? C47 C48 1.411(5) . ? C48 C49 1.376(5) . ? C49 C50 1.360(5) . ? C50 C51 1.348(5) . ? C39 C41 1.426(7) . ? C39 C40 1.621(6) . ? C43 C44 1.547(8) . ? C44 C45 1.431(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Yb N2 98.83(7) . . ? N3 Yb N1 133.29(7) . . ? N2 Yb N1 80.67(6) . . ? N3 Yb O 125.28(6) . . ? N2 Yb O 101.99(6) . . ? N1 Yb O 99.91(6) . . ? C45 O C42 108.69(18) . . ? C45 O Yb 123.47(14) . . ? C42 O Yb 127.71(13) . . ? C1 N1 C6 120.98(19) . . ? C1 N1 Yb 123.80(15) . . ? C6 N1 Yb 114.45(13) . . ? C3 N2 C18 120.29(19) . . ? C3 N2 Yb 124.48(15) . . ? C18 N2 Yb 114.69(14) . . ? C30 N3 Yb 138.15(16) . . ? N1 C1 C2 125.0(2) . . ? N1 C1 C4 120.8(2) . . ? C2 C1 C4 114.2(2) . . ? C1 C2 C3 131.0(2) . . ? N2 C3 C2 124.6(2) . . ? N2 C3 C5 120.5(2) . . ? C2 C3 C5 114.8(2) . . ? C11 C6 C7 120.4(2) . . ? C11 C6 N1 121.3(2) . . ? C7 C6 N1 118.1(2) . . ? C8 C7 C6 118.5(2) . . ? C8 C7 C12 121.0(2) . . ? C6 C7 C12 120.5(2) . . ? C9 C8 C7 121.4(3) . . ? C8 C9 C10 120.0(2) . . ? C9 C10 C11 121.0(2) . . ? C10 C11 C6 118.8(2) . . ? C10 C11 C15 118.7(2) . . ? C6 C11 C15 122.6(2) . . ? C14 C12 C13 112.4(3) . . ? C14 C12 C7 112.2(3) . . ? C13 C12 C7 114.8(3) . . ? C11 C15 C16 111.7(2) . . ? C11 C15 C17 111.2(2) . . ? C16 C15 C17 109.6(2) . . ? C23 C18 C19 120.1(2) . . ? C23 C18 N2 121.0(2) . . ? C19 C18 N2 118.6(2) . . ? C20 C19 C18 118.6(2) . . ? C20 C19 C24 120.0(2) . . ? C18 C19 C24 121.3(2) . . ? C21 C20 C19 121.6(3) . . ? C22 C21 C20 119.5(2) . . ? C21 C22 C23 121.2(2) . . ? C22 C23 C18 118.9(2) . . ? C22 C23 C27 119.3(2) . . ? C18 C23 C27 121.8(2) . . ? C25 C24 C19 112.1(3) . . ? C25 C24 C26 109.9(3) . . ? C19 C24 C26 110.3(3) . . ? C23 C27 C28 109.9(2) . . ? C23 C27 C29 112.8(2) . . ? C28 C27 C29 110.7(3) . . ? N3 C30 C31 118.3(2) . . ? N3 C30 C35 124.4(2) . . ? C31 C30 C35 117.3(2) . . ? C32 C31 C30 120.4(2) . . ? C32 C31 C36 121.5(2) . . ? C30 C31 C36 118.09(19) . . ? C33 C32 C31 121.5(2) . . ? C34 C33 C32 118.5(2) . . ? C33 C34 C35 122.6(2) . . ? C34 C35 C30 119.5(2) . . ? C34 C35 C39 121.1(2) . . ? C30 C35 C39 119.4(2) . . ? C31 C36 C37 115.5(2) . . ? C31 C36 C38 109.73(19) . . ? C37 C36 C38 109.5(2) . . ? O C42 C43 106.0(2) . . ? C51 C46 C47 120.6(3) . . ? C46 C47 C48 119.1(3) . . ? C49 C48 C47 118.4(3) . . ? C50 C49 C48 120.5(3) . . ? C51 C50 C49 119.9(3) . . ? C46 C51 C50 121.5(3) . . ? C41 C39 C35 112.5(3) . . ? C41 C39 C40 111.1(4) . . ? C35 C39 C40 109.9(3) . . ? C42 C43 C44 104.2(3) . . ? C45 C44 C43 104.0(4) . . ? C44 C45 O 106.0(3) . . ? #===END data_(6)-aug603 _database_code_depnum_ccdc_archive 'CCDC 706864' _audit_creation_date 2003-08-21T14:05:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H68 N2 O1 Si2 Yb1' _chemical_formula_sum 'C40 H68 N2 O1 Si2 Yb1' _chemical_formula_weight 822.18 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 13.6465(2) _cell_length_b 16.2031(2) _cell_length_c 19.7654(3) _cell_angle_alpha 98.537(1) _cell_angle_beta 97.971(1) _cell_angle_gamma 89.946(1) _cell_volume 4279.39(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 51464 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.271 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.465 _exptl_absorpt_correction_T_max 0.6474 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.179564E-1 _diffrn_orient_matrix_ub_12 0.195114E-1 _diffrn_orient_matrix_ub_13 -0.457232E-1 _diffrn_orient_matrix_ub_21 -0.711531E-1 _diffrn_orient_matrix_ub_22 0.17663E-2 _diffrn_orient_matrix_ub_23 0.7111E-2 _diffrn_orient_matrix_ub_31 0.95952E-2 _diffrn_orient_matrix_ub_32 0.592666E-1 _diffrn_orient_matrix_ub_33 0.229911E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_unetI/netI 0.0451 _diffrn_reflns_number 44846 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.06 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.978 _reflns_number_total 14833 _reflns_number_gt 12434 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0838P)^2^+20.2547P] 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_number_reflns 14833 _refine_ls_number_parameters 833 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1477 _refine_ls_wR_factor_gt 0.1381 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 5.655 _refine_diff_density_min -1.805 _refine_diff_density_rms 0.137 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.385 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Yb Yb 0.576940(18) 0.774310(17) 0.756073(13) 0.02819(10) Uani 1 1 d . . . Si1 Si 0.84122(16) 0.77997(16) 0.76299(14) 0.0547(6) Uani 1 1 d . . . Si2 Si 0.75558(17) 0.90675(19) 0.87410(12) 0.0595(7) Uani 1 1 d . . . O1 O 0.5439(3) 0.6666(3) 0.8203(2) 0.0390(11) Uani 1 1 d . . . N1 N 0.4138(4) 0.8314(3) 0.7505(3) 0.0333(12) Uani 1 1 d . . . N2 N 0.5073(4) 0.7074(3) 0.6431(3) 0.0313(12) Uani 1 1 d . . . C1 C 0.3342(5) 0.7954(4) 0.7120(3) 0.0325(14) Uani 1 1 d . . . C2 C 0.3352(5) 0.7285(4) 0.6570(3) 0.0307(14) Uani 1 1 d . . . H2 H 0.2727 0.7014 0.6414 0.037 Uiso 1 1 calc R . . C3 C 0.4117(5) 0.6950(4) 0.6216(3) 0.0332(14) Uani 1 1 d . . . C4 C 0.2312(5) 0.8255(5) 0.7223(4) 0.0453(18) Uani 1 1 d . . . H4A H 0.1992 0.7866 0.7463 0.068 Uiso 1 1 calc R . . H4B H 0.192 0.8281 0.6772 0.068 Uiso 1 1 calc R . . H4C H 0.236 0.8811 0.75 0.068 Uiso 1 1 calc R . . C5 C 0.3753(6) 0.6429(5) 0.5513(4) 0.0475(18) Uani 1 1 d . . . H5A H 0.3608 0.68 0.5164 0.071 Uiso 1 1 calc R . . H5B H 0.3152 0.6115 0.5544 0.071 Uiso 1 1 calc R . . H5C H 0.4268 0.6039 0.5381 0.071 Uiso 1 1 calc R . . C6 C 0.4044(5) 0.9063(5) 0.7979(4) 0.0392(16) Uani 1 1 d . . . C7 C 0.4301(6) 0.9828(5) 0.7792(4) 0.056(2) Uani 1 1 d . . . C8 C 0.4302(8) 1.0551(6) 0.8283(6) 0.082(4) Uani 1 1 d . . . H8 H 0.4452 1.1076 0.8159 0.099 Uiso 1 1 calc R . . C9 C 0.4094(8) 1.0515(7) 0.8928(6) 0.085(4) Uani 1 1 d . . . H9 H 0.4122 1.1011 0.9254 0.103 Uiso 1 1 calc R . . C10 C 0.3840(6) 0.9758(6) 0.9120(5) 0.063(3) Uani 1 1 d . . . H10 H 0.3705 0.9747 0.9577 0.075 Uiso 1 1 calc R . . C11 C 0.3780(5) 0.9020(5) 0.8658(4) 0.0415(17) Uani 1 1 d . . . C12 C 0.4545(7) 0.9897(5) 0.7086(5) 0.061(2) Uani 1 1 d . . . H12 H 0.4778 0.9336 0.6895 0.073 Uiso 1 1 calc R . . C13 C 0.3622(10) 1.0078(9) 0.6596(6) 0.100(4) Uani 1 1 d . . . H13A H 0.3804 1.0112 0.6139 0.15 Uiso 1 1 calc R . . H13B H 0.3343 1.0609 0.6779 0.15 Uiso 1 1 calc R . . H13C H 0.3129 0.9628 0.6559 0.15 Uiso 1 1 calc R . . C14 C 0.5375(11) 1.0519(9) 0.7075(7) 0.110(5) Uani 1 1 d . . . H14A H 0.549 1.0524 0.6597 0.165 Uiso 1 1 calc R . . H14B H 0.5982 1.0356 0.7346 0.165 Uiso 1 1 calc R . . H14C H 0.5189 1.1077 0.7274 0.165 Uiso 1 1 calc R . . C15 C 0.3500(6) 0.8211(5) 0.8878(4) 0.052(2) Uani 1 1 d . . . H15 H 0.3479 0.7758 0.8473 0.063 Uiso 1 1 calc R . . C16 C 0.4233(9) 0.7972(9) 0.9465(5) 0.093(4) Uani 1 1 d . . . H16A H 0.4022 0.744 0.9585 0.139 Uiso 1 1 calc R . . H16B H 0.4258 0.8407 0.9869 0.139 Uiso 1 1 calc R . . H16C H 0.4891 0.7914 0.9321 0.139 Uiso 1 1 calc R . . C17 C 0.2469(7) 0.8270(6) 0.9107(5) 0.058(2) Uani 1 1 d . . . H17A H 0.2291 0.7738 0.9242 0.087 Uiso 1 1 calc R . . H17B H 0.1983 0.8394 0.8723 0.087 Uiso 1 1 calc R . . H17C H 0.2475 0.8717 0.9501 0.087 Uiso 1 1 calc R . . C18 C 0.5726(5) 0.6801(5) 0.5934(3) 0.0381(16) Uani 1 1 d . . . C19 C 0.6237(5) 0.6038(5) 0.5968(4) 0.0437(17) Uani 1 1 d . . . C20 C 0.6866(7) 0.5802(6) 0.5482(5) 0.061(2) Uani 1 1 d . . . H20 H 0.72 0.5288 0.5491 0.073 Uiso 1 1 calc R . . C21 C 0.7025(7) 0.6277(7) 0.4993(5) 0.070(3) Uani 1 1 d . . . H21 H 0.7459 0.6092 0.4667 0.084 Uiso 1 1 calc R . . C22 C 0.6551(7) 0.7031(7) 0.4975(4) 0.067(3) Uani 1 1 d . . . H22 H 0.6672 0.7369 0.464 0.08 Uiso 1 1 calc R . . C23 C 0.5889(6) 0.7301(5) 0.5448(4) 0.0478(18) Uani 1 1 d . . . C24 C 0.6088(6) 0.5479(5) 0.6494(4) 0.0477(18) Uani 1 1 d . . . H24 H 0.591 0.585 0.6909 0.057 Uiso 1 1 calc R . . C25 C 0.7021(9) 0.5024(8) 0.6739(7) 0.098(4) Uani 1 1 d . . . H25A H 0.6878 0.4677 0.708 0.147 Uiso 1 1 calc R . . H25B H 0.7545 0.5434 0.695 0.147 Uiso 1 1 calc R . . H25C H 0.7241 0.467 0.6344 0.147 Uiso 1 1 calc R . . C26 C 0.5239(8) 0.4866(6) 0.6251(5) 0.073(3) Uani 1 1 d . . . H26A H 0.5172 0.4521 0.661 0.109 Uiso 1 1 calc R . . H26B H 0.5366 0.4507 0.5828 0.109 Uiso 1 1 calc R . . H26C H 0.4626 0.517 0.6155 0.109 Uiso 1 1 calc R . . C27 C 0.5428(6) 0.8147(6) 0.5429(4) 0.056(2) Uani 1 1 d . . . H27 H 0.4899 0.8191 0.5736 0.067 Uiso 1 1 calc R . . C28 C 0.4940(10) 0.8271(9) 0.4707(6) 0.101(4) Uani 1 1 d . . . H28A H 0.4651 0.8826 0.4728 0.151 Uiso 1 1 calc R . . H28B H 0.4419 0.7844 0.454 0.151 Uiso 1 1 calc R . . H28C H 0.5439 0.8221 0.4392 0.151 Uiso 1 1 calc R . . C29 C 0.6191(8) 0.8851(7) 0.5721(6) 0.076(3) Uani 1 1 d . . . H29A H 0.5875 0.9392 0.5703 0.114 Uiso 1 1 calc R . . H29B H 0.6737 0.8808 0.5444 0.114 Uiso 1 1 calc R . . H29C H 0.6448 0.8801 0.6201 0.114 Uiso 1 1 calc R . . C30 C 0.7442(5) 0.8523(5) 0.7861(4) 0.0444(17) Uani 1 1 d . . . H30 H 0.7427 0.8961 0.7552 0.053 Uiso 1 1 calc R . . C31 C 0.9737(7) 0.8127(8) 0.7920(7) 0.092(4) Uani 1 1 d . . . H31A H 1.0168 0.7677 0.7758 0.138 Uiso 1 1 calc R . . H31B H 0.9857 0.8245 0.8426 0.138 Uiso 1 1 calc R . . H31C H 0.9881 0.863 0.7728 0.138 Uiso 1 1 calc R . . C32 C 0.8221(11) 0.6796(8) 0.7980(9) 0.116(5) Uani 1 1 d . . . H32A H 0.8738 0.6403 0.7859 0.174 Uiso 1 1 calc R . . H32B H 0.757 0.6551 0.7779 0.174 Uiso 1 1 calc R . . H32C H 0.8257 0.6914 0.8484 0.174 Uiso 1 1 calc R . . C33 C 0.8371(7) 0.7505(7) 0.6685(6) 0.075(3) Uani 1 1 d . . . H33A H 0.8904 0.7117 0.6591 0.113 Uiso 1 1 calc R . . H33B H 0.8457 0.8006 0.6475 0.113 Uiso 1 1 calc R . . H33C H 0.7731 0.7236 0.6489 0.113 Uiso 1 1 calc R . . C34 C 0.8666(13) 0.9772(13) 0.9066(10) 0.168(9) Uani 1 1 d . . . H34A H 0.8808 1.0082 0.87 0.252 Uiso 1 1 calc R . . H34B H 0.9238 0.9436 0.9199 0.252 Uiso 1 1 calc R . . H34C H 0.8531 1.0165 0.9468 0.252 Uiso 1 1 calc R . . C35 C 0.6662(19) 1.0013(13) 0.8832(8) 0.190(11) Uani 1 1 d . . . H35A H 0.6786 1.0393 0.8511 0.285 Uiso 1 1 calc R . . H35B H 0.6779 1.031 0.9307 0.285 Uiso 1 1 calc R . . H35C H 0.5975 0.9807 0.8726 0.285 Uiso 1 1 calc R . . C36 C 0.717(3) 0.8515(11) 0.9318(9) 0.34(3) Uani 1 1 d . . . H36A H 0.7253 0.8855 0.9777 0.511 Uiso 1 1 calc R . . H36B H 0.7557 0.8008 0.9335 0.511 Uiso 1 1 calc R . . H36C H 0.6466 0.8361 0.9178 0.511 Uiso 1 1 calc R . . C37 C 0.5963(6) 0.6313(6) 0.8771(5) 0.058(2) Uani 1 1 d . . . H37A H 0.6051 0.6731 0.9195 0.07 Uiso 1 1 calc R . . H37B H 0.6624 0.6127 0.8666 0.07 Uiso 1 1 calc R . . C38 C 0.5340(7) 0.5572(6) 0.8871(5) 0.058(2) Uani 1 1 d . . . H38A H 0.576 0.5108 0.9004 0.069 Uiso 1 1 calc R . . H38B H 0.4899 0.5734 0.9224 0.069 Uiso 1 1 calc R . . C39 C 0.4754(6) 0.5342(5) 0.8157(4) 0.0454(17) Uani 1 1 d . . . H39A H 0.515 0.5004 0.7839 0.055 Uiso 1 1 calc R . . H39B H 0.4136 0.5032 0.8176 0.055 Uiso 1 1 calc R . . C40 C 0.4541(5) 0.6174(4) 0.7945(4) 0.0380(15) Uani 1 1 d . . . H40A H 0.4393 0.6128 0.7436 0.046 Uiso 1 1 calc R . . H40B H 0.3971 0.6428 0.8153 0.046 Uiso 1 1 calc R . . Yb1B Yb 0.028083(19) 0.273707(16) 0.755819(13) 0.02706(10) Uani 1 1 d . A 1 Si1B Si -0.10607(16) 0.39959(15) 0.87839(11) 0.0474(5) Uani 1 1 d . A 1 Si2B Si -0.23485(15) 0.27676(15) 0.76397(14) 0.0530(6) Uani 1 1 d . A 1 O1B O 0.0859(4) 0.1655(3) 0.8188(3) 0.0466(13) Uani 1 1 d . A 1 N1B N 0.0496(4) 0.2090(3) 0.6413(3) 0.0301(11) Uani 1 1 d . A 1 N2B N 0.1854(4) 0.3353(3) 0.7481(3) 0.0288(11) Uani 1 1 d . A 1 C1B C 0.1368(5) 0.1977(4) 0.6198(3) 0.0324(14) Uani 1 1 d . A 1 C2B C 0.2288(5) 0.2318(4) 0.6554(3) 0.0311(14) Uani 1 1 d . A 1 H2B H 0.2852 0.2045 0.6402 0.037 Uiso 1 1 calc R A 1 C3B C 0.2508(5) 0.2996(4) 0.7095(3) 0.0289(13) Uani 1 1 d . A 1 C4B C 0.1454(6) 0.1475(5) 0.5492(4) 0.0476(19) Uani 1 1 d . A 1 H4B1 H 0.0911 0.1061 0.5366 0.071 Uiso 1 1 calc R A 1 H4B2 H 0.2088 0.1188 0.5512 0.071 Uiso 1 1 calc R A 1 H4B3 H 0.1419 0.1851 0.5145 0.071 Uiso 1 1 calc R A 1 C5B C 0.3561(5) 0.3312(5) 0.7197(4) 0.0426(17) Uani 1 1 d . A 1 H5B1 H 0.3578 0.3921 0.7323 0.064 Uiso 1 1 calc R A 1 H5B2 H 0.3846 0.3161 0.6768 0.064 Uiso 1 1 calc R A 1 H5B3 H 0.3947 0.3061 0.7568 0.064 Uiso 1 1 calc R A 1 C6B C -0.0358(5) 0.1821(5) 0.5925(3) 0.0379(16) Uani 1 1 d . A 1 C7B C -0.0721(6) 0.2341(5) 0.5436(4) 0.0471(19) Uani 1 1 d . A 1 C8B C -0.1576(7) 0.2067(7) 0.4974(4) 0.065(3) Uani 1 1 d . A 1 H8B H -0.1845 0.2412 0.4649 0.078 Uiso 1 1 calc R A 1 C9B C -0.2033(7) 0.1310(7) 0.4980(5) 0.067(3) Uani 1 1 d . A 1 H9B H -0.259 0.1127 0.4647 0.081 Uiso 1 1 calc R A 1 C10B C -0.1686(7) 0.0823(6) 0.5465(5) 0.061(2) Uani 1 1 d . A 1 H10B H -0.2021 0.0314 0.5477 0.073 Uiso 1 1 calc R A 1 C11B C -0.0849(5) 0.1061(5) 0.5942(4) 0.0436(17) Uani 1 1 d . A 1 C12B C -0.0259(7) 0.3177(6) 0.5426(4) 0.057(2) Uani 1 1 d . A 1 H12B H 0.0393 0.3213 0.5732 0.068 Uiso 1 1 calc R A 1 C13B C -0.0063(11) 0.3307(10) 0.4700(6) 0.104(5) Uani 1 1 d . A 1 H13D H 0.024 0.3861 0.4723 0.156 Uiso 1 1 calc R A 1 H13E H -0.069 0.3265 0.4386 0.156 Uiso 1 1 calc R A 1 H13F H 0.0386 0.2879 0.4527 0.156 Uiso 1 1 calc R A 1 C14B C -0.0906(8) 0.3879(6) 0.5724(6) 0.073(3) Uani 1 1 d . A 1 H14D H -0.0596 0.4421 0.5714 0.109 Uiso 1 1 calc R A 1 H14E H -0.0974 0.3821 0.6202 0.109 Uiso 1 1 calc R A 1 H14F H -0.1562 0.3842 0.5446 0.109 Uiso 1 1 calc R A 1 C15B C -0.0474(6) 0.0491(5) 0.6463(4) 0.051(2) Uani 1 1 d . A 1 H15B H -0.0166 0.0856 0.6892 0.061 Uiso 1 1 calc R A 1 C16B C -0.1317(9) -0.0007(7) 0.6660(7) 0.089(3) Uani 1 1 d . A 1 H16D H -0.1046 -0.0366 0.6995 0.133 Uiso 1 1 calc R A 1 H16E H -0.166 -0.0353 0.6246 0.133 Uiso 1 1 calc R A 1 H16F H -0.1785 0.0379 0.6866 0.133 Uiso 1 1 calc R A 1 C17B C 0.0316(9) -0.0092(6) 0.6224(5) 0.077(3) Uani 1 1 d . A 1 H17D H 0.0528 -0.0444 0.6578 0.115 Uiso 1 1 calc R A 1 H17E H 0.0883 0.0236 0.6149 0.115 Uiso 1 1 calc R A 1 H17F H 0.0048 -0.0445 0.5792 0.115 Uiso 1 1 calc R A 1 C18B C 0.2153(5) 0.4094(4) 0.7965(3) 0.0338(15) Uani 1 1 d . A 1 C19B C 0.2675(5) 0.4051(4) 0.8618(4) 0.0382(16) Uani 1 1 d . A 1 C20B C 0.2836(6) 0.4786(5) 0.9097(4) 0.0428(17) Uani 1 1 d . A 1 H20B H 0.3169 0.476 0.9548 0.051 Uiso 1 1 calc R A 1 C21B C 0.2517(6) 0.5548(5) 0.8924(4) 0.050(2) Uani 1 1 d . A 1 H21B H 0.2645 0.6041 0.9251 0.06 Uiso 1 1 calc R A 1 C22B C 0.2009(6) 0.5591(5) 0.8270(5) 0.053(2) Uani 1 1 d . A 1 H22B H 0.1793 0.6116 0.8153 0.063 Uiso 1 1 calc R A 1 C23B C 0.1813(5) 0.4869(4) 0.7781(4) 0.0395(16) Uani 1 1 d . A 1 C24B C 0.3035(7) 0.3240(5) 0.8845(4) 0.052(2) Uani 1 1 d . A 1 H24B H 0.2912 0.2793 0.8434 0.062 Uiso 1 1 calc R A 1 C25B C 0.2450(10) 0.3003(7) 0.9399(5) 0.093(4) Uani 1 1 d . A 1 H25D H 0.2693 0.2475 0.9539 0.139 Uiso 1 1 calc R A 1 H25E H 0.1746 0.2938 0.9211 0.139 Uiso 1 1 calc R A 1 H25F H 0.2536 0.3443 0.9801 0.139 Uiso 1 1 calc R A 1 C26B C 0.4156(8) 0.3277(6) 0.9103(5) 0.076(3) Uani 1 1 d . A 1 H26D H 0.4362 0.2741 0.9243 0.114 Uiso 1 1 calc R A 1 H26E H 0.43 0.3722 0.9498 0.114 Uiso 1 1 calc R A 1 H26F H 0.4517 0.3393 0.873 0.114 Uiso 1 1 calc R A 1 C27B C 0.1249(6) 0.4935(5) 0.7076(4) 0.0490(19) Uani 1 1 d . A 1 H27B H 0.0923 0.4379 0.6893 0.059 Uiso 1 1 calc R A 1 C28B C 0.1942(10) 0.5106(9) 0.6579(6) 0.096(4) Uani 1 1 d . A 1 H28D H 0.2459 0.4685 0.6571 0.143 Uiso 1 1 calc R A 1 H28E H 0.2248 0.5662 0.6728 0.143 Uiso 1 1 calc R A 1 H28F H 0.157 0.5081 0.6115 0.143 Uiso 1 1 calc R A 1 C29B C 0.0454(10) 0.5566(9) 0.7091(6) 0.101(4) Uani 1 1 d . A 1 H29D H 0.0117 0.5573 0.6621 0.151 Uiso 1 1 calc R A 1 H29E H 0.0747 0.6118 0.7279 0.151 Uiso 1 1 calc R A 1 H29F H -0.0024 0.542 0.7383 0.151 Uiso 1 1 calc R A 1 C30B C -0.1273(5) 0.3474(5) 0.7889(4) 0.0439(17) Uani 1 1 d . A 1 H30B H -0.1387 0.3928 0.7596 0.053 Uiso 1 1 calc R A 1 C31B C 0.0114(10) 0.4620(14) 0.8972(7) 0.167(10) Uani 1 1 d . A 1 H31D H 0.0207 0.4886 0.9455 0.251 Uiso 1 1 calc R A 1 H31E H 0.0086 0.505 0.867 0.251 Uiso 1 1 calc R A 1 H31F H 0.067 0.4253 0.8889 0.251 Uiso 1 1 calc R A 1 C32B C -0.1054(14) 0.3279(9) 0.9445(6) 0.120(6) Uani 1 1 d . A 1 H32D H -0.0936 0.3605 0.9909 0.179 Uiso 1 1 calc R A 1 H32E H -0.0527 0.2873 0.9391 0.179 Uiso 1 1 calc R A 1 H32F H -0.1694 0.2985 0.9381 0.179 Uiso 1 1 calc R A 1 C33B C -0.2010(11) 0.4797(8) 0.9025(6) 0.098(4) Uani 1 1 d . A 1 H33D H -0.1842 0.5041 0.9512 0.147 Uiso 1 1 calc R A 1 H33E H -0.2666 0.4527 0.8953 0.147 Uiso 1 1 calc R A 1 H33F H -0.2014 0.5238 0.8735 0.147 Uiso 1 1 calc R A 1 C34B C -0.3615(7) 0.2970(8) 0.7822(9) 0.132(7) Uani 1 1 d . A 1 H34D H -0.4037 0.2479 0.7632 0.198 Uiso 1 1 calc R A 1 H34E H -0.387 0.3451 0.7609 0.198 Uiso 1 1 calc R A 1 H34F H -0.3615 0.309 0.8323 0.198 Uiso 1 1 calc R A 1 C35B C -0.2716(8) 0.2550(8) 0.6689(5) 0.084(3) Uani 1 1 d . A 1 H35D H -0.2127 0.2426 0.6463 0.126 Uiso 1 1 calc R A 1 H35E H -0.3039 0.304 0.6528 0.126 Uiso 1 1 calc R A 1 H35F H -0.3177 0.207 0.6575 0.126 Uiso 1 1 calc R A 1 C36B C -0.2075(10) 0.1716(8) 0.7919(9) 0.116(5) Uani 1 1 d . A 1 H36D H -0.1398 0.1561 0.7849 0.174 Uiso 1 1 calc R A 1 H36E H -0.2543 0.1296 0.7645 0.174 Uiso 1 1 calc R A 1 H36F H -0.2142 0.1746 0.841 0.174 Uiso 1 1 calc R A 1 C37B C 0.1674(7) 0.1173(5) 0.7941(5) 0.054(2) Uani 1 1 d . A 1 H37C H 0.2319 0.1423 0.817 0.065 Uiso 1 1 calc R A 1 H37D H 0.1646 0.1148 0.7435 0.065 Uiso 1 1 calc R A 1 C38B C 0.1536(8) 0.0322(5) 0.8123(5) 0.065(3) Uani 1 1 d . A 1 H38C H 0.1033 -0.0012 0.7782 0.078 Uiso 1 1 calc R A 1 H38D H 0.2165 0.0016 0.8156 0.078 Uiso 1 1 calc R A 1 C39B C 0.1196(10) 0.0519(7) 0.8797(6) 0.081(3) Uani 1 1 d . A 1 H39C H 0.1764 0.0653 0.9167 0.097 Uiso 1 1 calc R A 1 H39D H 0.0815 0.0043 0.8897 0.097 Uiso 1 1 calc R A 1 C40B C 0.0535(8) 0.1281(6) 0.8740(5) 0.065(2) Uani 1 1 d . A 1 H40C H -0.0171 0.1109 0.8627 0.078 Uiso 1 1 calc R A 1 H40D H 0.0628 0.1677 0.9178 0.078 Uiso 1 1 calc R A 1 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 Yb 0.02331(15) 0.03281(17) 0.02897(16) 0.00653(11) 0.00343(11) -0.00174(11) Si1 0.0277(10) 0.0614(15) 0.0796(16) 0.0201(12) 0.0134(10) -0.0042(9) Si2 0.0371(12) 0.102(2) 0.0389(12) 0.0115(12) 0.0009(9) -0.0241(12) O1 0.038(3) 0.041(3) 0.040(3) 0.016(2) 0.000(2) -0.008(2) N1 0.029(3) 0.038(3) 0.031(3) -0.003(2) 0.002(2) 0.001(2) N2 0.029(3) 0.039(3) 0.027(3) 0.005(2) 0.008(2) 0.006(2) C1 0.033(3) 0.031(3) 0.033(3) 0.005(3) 0.004(3) 0.001(3) C2 0.027(3) 0.033(3) 0.030(3) 0.001(3) -0.001(3) -0.002(3) C3 0.040(4) 0.032(3) 0.027(3) 0.002(3) 0.005(3) -0.001(3) C4 0.024(3) 0.052(5) 0.054(4) -0.006(4) 0.001(3) 0.002(3) C5 0.039(4) 0.059(5) 0.039(4) -0.008(3) 0.002(3) -0.002(3) C6 0.028(3) 0.044(4) 0.039(4) -0.009(3) 0.001(3) -0.005(3) C7 0.056(5) 0.049(5) 0.060(5) -0.017(4) 0.019(4) -0.019(4) C8 0.087(7) 0.059(6) 0.099(8) -0.031(5) 0.049(6) -0.035(5) C9 0.087(7) 0.072(7) 0.086(7) -0.050(6) 0.041(6) -0.045(6) C10 0.048(5) 0.078(6) 0.053(5) -0.028(5) 0.016(4) -0.015(4) C11 0.027(3) 0.053(4) 0.036(4) -0.011(3) -0.005(3) 0.003(3) C12 0.072(6) 0.036(4) 0.077(6) -0.006(4) 0.031(5) -0.013(4) C13 0.102(10) 0.120(11) 0.077(8) 0.009(7) 0.010(7) -0.021(8) C14 0.124(11) 0.122(11) 0.086(8) -0.003(7) 0.040(8) -0.079(9) C15 0.058(5) 0.060(5) 0.038(4) 0.003(4) 0.009(4) 0.026(4) C16 0.084(8) 0.138(11) 0.054(6) 0.014(6) 0.004(5) 0.052(8) C17 0.066(6) 0.058(5) 0.052(5) 0.006(4) 0.017(4) 0.002(4) C18 0.030(3) 0.056(5) 0.026(3) -0.001(3) 0.005(3) -0.003(3) C19 0.038(4) 0.047(4) 0.042(4) -0.008(3) 0.010(3) 0.000(3) C20 0.062(5) 0.064(6) 0.056(5) -0.014(4) 0.028(4) 0.002(4) C21 0.063(6) 0.086(7) 0.059(6) -0.014(5) 0.028(5) -0.005(5) C22 0.062(6) 0.100(8) 0.040(5) 0.003(5) 0.020(4) -0.019(5) C23 0.044(4) 0.062(5) 0.038(4) 0.006(4) 0.008(3) -0.007(4) C24 0.055(5) 0.041(4) 0.048(4) 0.001(3) 0.015(4) 0.017(4) C25 0.086(8) 0.085(8) 0.134(11) 0.044(8) 0.028(8) 0.037(7) C26 0.091(8) 0.066(6) 0.060(6) 0.002(5) 0.016(5) -0.024(5) C27 0.050(5) 0.078(6) 0.046(4) 0.028(4) 0.010(4) -0.003(4) C28 0.121(11) 0.114(10) 0.069(7) 0.058(7) -0.025(7) -0.013(8) C29 0.078(7) 0.067(6) 0.084(7) 0.009(5) 0.018(6) 0.003(5) C30 0.041(4) 0.054(5) 0.040(4) 0.016(3) 0.003(3) 0.000(3) C31 0.030(5) 0.105(9) 0.143(11) 0.016(8) 0.016(6) 0.009(5) C32 0.103(10) 0.081(9) 0.188(15) 0.060(9) 0.064(10) 0.012(7) C33 0.051(5) 0.079(7) 0.094(8) -0.005(6) 0.024(5) -0.001(5) C34 0.130(14) 0.20(2) 0.153(15) -0.081(14) 0.053(12) -0.073(14) C35 0.29(3) 0.181(19) 0.077(10) -0.025(11) -0.004(13) 0.12(2) C36 0.84(8) 0.107(13) 0.103(13) -0.041(10) 0.22(3) -0.20(3) C37 0.047(5) 0.065(6) 0.066(5) 0.035(4) -0.010(4) -0.012(4) C38 0.055(5) 0.061(5) 0.062(5) 0.030(4) 0.002(4) -0.008(4) C39 0.045(4) 0.041(4) 0.052(4) 0.004(3) 0.016(4) -0.002(3) C40 0.035(4) 0.038(4) 0.041(4) 0.008(3) 0.006(3) -0.006(3) Yb1B 0.02888(16) 0.02505(15) 0.02843(16) 0.00439(11) 0.00775(11) 0.00182(11) Si1B 0.0372(11) 0.0585(14) 0.0466(12) -0.0019(10) 0.0166(9) 0.0002(9) Si2B 0.0256(10) 0.0569(14) 0.0718(15) -0.0022(11) 0.0038(10) 0.0013(9) O1B 0.063(3) 0.033(3) 0.048(3) 0.018(2) 0.008(3) 0.007(2) N1B 0.029(3) 0.029(3) 0.031(3) 0.003(2) 0.003(2) 0.001(2) N2B 0.037(3) 0.021(3) 0.029(3) 0.004(2) 0.004(2) 0.002(2) C1B 0.037(4) 0.031(3) 0.028(3) 0.003(3) 0.005(3) 0.002(3) C2B 0.034(3) 0.030(3) 0.030(3) 0.001(3) 0.010(3) 0.002(3) C3B 0.033(3) 0.027(3) 0.030(3) 0.009(3) 0.009(3) 0.000(3) C4B 0.040(4) 0.060(5) 0.037(4) -0.016(3) 0.010(3) -0.006(4) C5B 0.038(4) 0.042(4) 0.046(4) -0.006(3) 0.012(3) -0.007(3) C6B 0.035(4) 0.047(4) 0.031(3) -0.002(3) 0.009(3) 0.007(3) C7B 0.042(4) 0.064(5) 0.033(4) 0.002(3) 0.003(3) 0.014(4) C8B 0.052(5) 0.099(8) 0.037(4) 0.000(4) -0.002(4) 0.023(5) C9B 0.049(5) 0.086(7) 0.054(5) -0.021(5) -0.005(4) 0.001(5) C10B 0.053(5) 0.057(5) 0.062(5) -0.016(4) 0.001(4) -0.002(4) C11B 0.037(4) 0.046(4) 0.042(4) -0.007(3) 0.004(3) -0.004(3) C12B 0.058(5) 0.070(6) 0.049(5) 0.031(4) 0.006(4) 0.011(4) C13B 0.130(11) 0.137(12) 0.063(7) 0.058(7) 0.027(7) 0.021(9) C14B 0.074(7) 0.065(6) 0.078(7) 0.009(5) 0.006(5) 0.007(5) C15B 0.062(5) 0.037(4) 0.051(5) -0.005(3) 0.005(4) -0.018(4) C16B 0.082(8) 0.074(7) 0.115(9) 0.028(7) 0.015(7) -0.021(6) C17B 0.097(8) 0.060(6) 0.062(6) -0.009(5) -0.005(5) 0.026(6) C18B 0.036(3) 0.035(4) 0.033(3) -0.001(3) 0.017(3) -0.018(3) C19B 0.036(4) 0.041(4) 0.039(4) 0.001(3) 0.013(3) -0.006(3) C20B 0.043(4) 0.049(5) 0.034(4) -0.008(3) 0.013(3) -0.013(3) C21B 0.049(4) 0.036(4) 0.061(5) -0.017(4) 0.022(4) -0.009(3) C22B 0.050(5) 0.026(4) 0.080(6) -0.007(4) 0.021(4) 0.001(3) C23B 0.044(4) 0.023(3) 0.052(4) -0.003(3) 0.016(3) 0.002(3) C24B 0.078(6) 0.048(5) 0.027(4) 0.006(3) -0.003(4) -0.014(4) C25B 0.145(11) 0.089(8) 0.047(5) 0.024(5) 0.004(6) -0.053(8) C26B 0.089(7) 0.059(6) 0.065(6) -0.001(5) -0.025(5) 0.008(5) C27B 0.058(5) 0.033(4) 0.056(5) 0.004(3) 0.010(4) 0.006(3) C28B 0.109(10) 0.123(11) 0.065(7) 0.028(7) 0.032(7) 0.029(8) C29B 0.110(10) 0.104(10) 0.085(8) 0.013(7) 0.002(7) 0.059(8) C30B 0.032(4) 0.050(4) 0.049(4) 0.000(3) 0.013(3) 0.005(3) C31B 0.089(10) 0.32(3) 0.073(8) -0.077(12) 0.039(7) -0.089(13) C32B 0.212(18) 0.095(9) 0.053(6) 0.012(6) 0.022(8) 0.057(10) C33B 0.134(11) 0.078(8) 0.080(8) -0.007(6) 0.029(8) 0.034(8) C34B 0.039(5) 0.132(10) 0.289(19) 0.166(12) 0.101(8) 0.061(6) C35B 0.056(6) 0.106(9) 0.074(7) -0.034(6) 0.002(5) -0.002(6) C36B 0.086(9) 0.075(8) 0.188(15) 0.054(9) -0.020(9) -0.030(7) C37B 0.058(5) 0.039(4) 0.065(5) 0.012(4) 0.004(4) 0.013(4) C38B 0.099(7) 0.026(4) 0.062(5) 0.004(4) -0.009(5) 0.005(4) C39B 0.113(9) 0.059(6) 0.081(7) 0.034(5) 0.018(6) 0.017(6) C40B 0.079(7) 0.055(5) 0.068(6) 0.034(5) 0.012(5) 0.005(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Yb O1 2.383(4) . ? Yb N2 2.401(5) . ? Yb N1 2.404(5) . ? Yb C30 2.562(8) . ? Si1 C30 1.828(8) . ? Si1 C33 1.850(11) . ? Si1 C31 1.872(10) . ? Si1 C32 1.891(12) . ? Si2 C36 1.691(14) . ? Si2 C30 1.817(8) . ? Si2 C34 1.878(15) . ? Si2 C35 1.960(17) . ? O1 C37 1.438(9) . ? O1 C40 1.451(8) . ? N1 C1 1.319(8) . ? N1 C6 1.437(9) . ? N2 C3 1.320(9) . ? N2 C18 1.438(8) . ? C1 C2 1.418(9) . ? C1 C4 1.517(9) . ? C2 C3 1.400(9) . ? C3 C5 1.534(9) . ? C6 C7 1.403(11) . ? C6 C11 1.448(10) . ? C7 C8 1.406(12) . ? C7 C12 1.498(12) . ? C8 C9 1.355(15) . ? C9 C10 1.395(15) . ? C10 C11 1.388(11) . ? C11 C15 1.507(12) . ? C12 C14 1.522(13) . ? C12 C13 1.535(16) . ? C15 C16 1.519(12) . ? C15 C17 1.535(12) . ? C18 C23 1.386(11) . ? C18 C19 1.425(11) . ? C19 C20 1.388(11) . ? C19 C24 1.510(11) . ? C20 C21 1.361(14) . ? C21 C22 1.385(15) . ? C22 C23 1.413(12) . ? C23 C27 1.511(12) . ? C24 C26 1.506(12) . ? C24 C25 1.527(13) . ? C27 C28 1.530(12) . ? C27 C29 1.536(14) . ? C37 C38 1.524(11) . ? C38 C39 1.517(11) . ? C39 C40 1.486(10) . ? Yb1B O1B 2.371(5) . ? Yb1B N2B 2.401(5) . ? Yb1B N1B 2.405(5) . ? Yb1B C30B 2.549(7) . ? Si1B C30B 1.829(8) . ? Si1B C31B 1.860(13) . ? Si1B C32B 1.872(13) . ? Si1B C33B 1.890(11) . ? Si2B C30B 1.828(8) . ? Si2B C34B 1.834(7) . ? Si2B C35B 1.857(10) . ? Si2B C36B 1.889(12) . ? O1B C40B 1.443(10) . ? O1B C37B 1.457(10) . ? N1B C1B 1.323(9) . ? N1B C6B 1.430(9) . ? N2B C3B 1.331(8) . ? N2B C18B 1.441(8) . ? C1B C2B 1.420(9) . ? C1B C4B 1.526(9) . ? C2B C3B 1.416(9) . ? C3B C5B 1.503(9) . ? C6B C11B 1.410(11) . ? C6B C7B 1.412(11) . ? C7B C8B 1.407(12) . ? C7B C12B 1.499(13) . ? C8B C9B 1.379(15) . ? C9B C10B 1.365(14) . ? C10B C11B 1.391(11) . ? C11B C15B 1.519(12) . ? C12B C14B 1.538(13) . ? C12B C13B 1.541(12) . ? C15B C17B 1.510(13) . ? C15B C16B 1.532(13) . ? C18B C19B 1.395(10) . ? C18B C23B 1.420(10) . ? C19B C20B 1.406(10) . ? C19B C24B 1.510(11) . ? C20B C21B 1.383(12) . ? C21B C22B 1.390(12) . ? C22B C23B 1.404(10) . ? C23B C27B 1.513(11) . ? C24B C25B 1.535(13) . ? C24B C26B 1.541(13) . ? C27B C29B 1.491(13) . ? C27B C28B 1.509(14) . ? C37B C38B 1.494(11) . ? C38B C39B 1.461(14) . ? C39B C40B 1.537(13) . ? 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 Yb N2 98.65(18) . . ? O1 Yb N1 95.66(18) . . ? N2 Yb N1 80.57(18) . . ? O1 Yb C30 118.7(2) . . ? N2 Yb C30 125.5(2) . . ? N1 Yb C30 128.3(2) . . ? C30 Si1 C33 112.9(4) . . ? C30 Si1 C31 118.9(5) . . ? C33 Si1 C31 102.8(5) . . ? C30 Si1 C32 108.7(5) . . ? C33 Si1 C32 106.0(6) . . ? C31 Si1 C32 106.5(6) . . ? C36 Si2 C30 115.0(6) . . ? C36 Si2 C34 116.1(13) . . ? C30 Si2 C34 118.0(6) . . ? C36 Si2 C35 99.5(14) . . ? C30 Si2 C35 112.2(5) . . ? C34 Si2 C35 91.4(10) . . ? C37 O1 C40 108.5(5) . . ? C37 O1 Yb 135.5(4) . . ? C40 O1 Yb 115.7(4) . . ? C1 N1 C6 119.6(5) . . ? C1 N1 Yb 124.7(4) . . ? C6 N1 Yb 115.4(4) . . ? C3 N2 C18 116.3(5) . . ? C3 N2 Yb 124.9(4) . . ? C18 N2 Yb 118.9(4) . . ? N1 C1 C2 124.8(6) . . ? N1 C1 C4 121.4(6) . . ? C2 C1 C4 113.8(6) . . ? C3 C2 C1 131.7(6) . . ? N2 C3 C2 125.6(6) . . ? N2 C3 C5 120.6(6) . . ? C2 C3 C5 113.8(6) . . ? C7 C6 N1 118.3(6) . . ? C7 C6 C11 121.0(7) . . ? N1 C6 C11 120.5(7) . . ? C6 C7 C8 118.2(8) . . ? C6 C7 C12 122.2(7) . . ? C8 C7 C12 119.6(8) . . ? C9 C8 C7 121.4(10) . . ? C8 C9 C10 120.8(8) . . ? C11 C10 C9 121.5(9) . . ? C10 C11 C6 117.0(8) . . ? C10 C11 C15 120.3(8) . . ? C6 C11 C15 122.5(6) . . ? C7 C12 C14 114.6(8) . . ? C7 C12 C13 111.5(8) . . ? C14 C12 C13 110.5(10) . . ? C11 C15 C16 112.7(9) . . ? C11 C15 C17 110.3(6) . . ? C16 C15 C17 108.6(8) . . ? C23 C18 C19 120.6(7) . . ? C23 C18 N2 119.7(7) . . ? C19 C18 N2 119.6(6) . . ? C20 C19 C18 117.6(8) . . ? C20 C19 C24 120.1(8) . . ? C18 C19 C24 122.2(6) . . ? C21 C20 C19 122.7(9) . . ? C20 C21 C22 119.5(8) . . ? C21 C22 C23 120.6(9) . . ? C18 C23 C22 118.9(8) . . ? C18 C23 C27 122.4(7) . . ? C22 C23 C27 118.6(8) . . ? C26 C24 C19 112.7(7) . . ? C26 C24 C25 110.3(9) . . ? C19 C24 C25 113.4(8) . . ? C23 C27 C28 113.1(9) . . ? C23 C27 C29 111.0(7) . . ? C28 C27 C29 110.0(8) . . ? Si2 C30 Si1 118.2(4) . . ? Si2 C30 Yb 109.2(3) . . ? Si1 C30 Yb 108.6(4) . . ? O1 C37 C38 106.7(6) . . ? C39 C38 C37 101.6(6) . . ? C40 C39 C38 102.2(6) . . ? O1 C40 C39 104.6(6) . . ? O1B Yb1B N2B 98.37(18) . . ? O1B Yb1B N1B 99.56(18) . . ? N2B Yb1B N1B 80.85(17) . . ? O1B Yb1B C30B 116.6(2) . . ? N2B Yb1B C30B 128.0(2) . . ? N1B Yb1B C30B 125.2(2) . . ? C30B Si1B C31B 111.7(5) . . ? C30B Si1B C32B 114.5(5) . . ? C31B Si1B C32B 108.4(9) . . ? C30B Si1B C33B 115.0(5) . . ? C31B Si1B C33B 102.6(8) . . ? C32B Si1B C33B 103.6(6) . . ? C30B Si2B C34B 127.2(6) . . ? C30B Si2B C35B 112.6(5) . . ? C34B Si2B C35B 94.1(6) . . ? C30B Si2B C36B 111.0(5) . . ? C34B Si2B C36B 103.8(5) . . ? C35B Si2B C36B 105.5(7) . . ? C40B O1B C37B 108.5(6) . . ? C40B O1B Yb1B 135.1(5) . . ? C37B O1B Yb1B 116.0(4) . . ? C1B N1B C6B 117.0(5) . . ? C1B N1B Yb1B 123.8(4) . . ? C6B N1B Yb1B 119.2(4) . . ? C3B N2B C18B 118.6(5) . . ? C3B N2B Yb1B 124.3(4) . . ? C18B N2B Yb1B 116.4(4) . . ? N1B C1B C2B 126.0(6) . . ? N1B C1B C4B 120.7(6) . . ? C2B C1B C4B 113.2(6) . . ? C3B C2B C1B 131.1(6) . . ? N2B C3B C2B 124.5(6) . . ? N2B C3B C5B 121.2(6) . . ? C2B C3B C5B 114.4(6) . . ? C11B C6B C7B 120.5(7) . . ? C11B C6B N1B 120.6(6) . . ? C7B C6B N1B 118.9(7) . . ? C8B C7B C6B 117.4(8) . . ? C8B C7B C12B 120.3(8) . . ? C6B C7B C12B 122.2(7) . . ? C9B C8B C7B 121.8(9) . . ? C10B C9B C8B 120.0(8) . . ? C9B C10B C11B 121.2(9) . . ? C10B C11B C6B 119.1(8) . . ? C10B C11B C15B 119.4(8) . . ? C6B C11B C15B 121.5(6) . . ? C7B C12B C14B 110.4(8) . . ? C7B C12B C13B 112.9(9) . . ? C14B C12B C13B 110.1(8) . . ? C17B C15B C11B 113.0(7) . . ? C17B C15B C16B 110.2(8) . . ? C11B C15B C16B 112.0(8) . . ? C19B C18B C23B 120.8(6) . . ? C19B C18B N2B 121.7(6) . . ? C23B C18B N2B 117.2(6) . . ? C18B C19B C20B 118.8(7) . . ? C18B C19B C24B 122.9(6) . . ? C20B C19B C24B 118.2(7) . . ? C21B C20B C19B 121.1(7) . . ? C20B C21B C22B 120.0(7) . . ? C21B C22B C23B 120.7(7) . . ? C22B C23B C18B 118.5(7) . . ? C22B C23B C27B 119.6(7) . . ? C18B C23B C27B 121.9(6) . . ? C19B C24B C25B 110.7(8) . . ? C19B C24B C26B 111.8(7) . . ? C25B C24B C26B 110.9(8) . . ? C29B C27B C28B 110.2(9) . . ? C29B C27B C23B 113.7(7) . . ? C28B C27B C23B 111.1(8) . . ? Si2B C30B Si1B 117.1(4) . . ? Si2B C30B Yb1B 110.2(3) . . ? Si1B C30B Yb1B 110.7(3) . . ? O1B C37B C38B 105.0(7) . . ? C39B C38B C37B 101.6(7) . . ? C38B C39B C40B 105.1(8) . . ? O1B C40B C39B 104.4(8) . . ? #===END data_(8)-feb1403 _database_code_depnum_ccdc_archive 'CCDC 706865' _audit_creation_date 2003-02-12T14:54:47-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[Yb(thf)(Ph3C)(C6H3iPr2NCMeCHCMeNC6H3iPr2)]' ; _chemical_formula_moiety 'C52 H64 N2 O1 Yb1' _chemical_formula_sum 'C52 H64 N2 O1 Yb1' _chemical_formula_weight 906.09 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.6608(5) _cell_length_b 9.0274(2) _cell_length_c 21.7827(4) _cell_angle_alpha 90 _cell_angle_beta 100.391(1) _cell_angle_gamma 90 _cell_volume 4576.38(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 99348 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.5934 _exptl_absorpt_correction_T_max 0.9822 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0891 _diffrn_reflns_av_unetI/netI 0.051 _diffrn_reflns_number 32206 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 22.97 _diffrn_reflns_theta_full 22.97 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 6287 _reflns_number_gt 4811 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The duffraction was weak and limited in extent. 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^)+(0.0000P)^2^+41.2413P] 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_number_reflns 6287 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.1458 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 1.231 _refine_ls_restrained_S_all 1.231 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.06 _refine_diff_density_min -1.439 _refine_diff_density_rms 0.097 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.385 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Yb Yb 0.73850(2) 0.49678(6) 0.37426(2) 0.04741(17) Uani 1 1 d . . . O O 0.8039(4) 0.6715(9) 0.4280(4) 0.070(2) Uani 1 1 d . A 1 N1 N 0.7080(3) 0.6270(9) 0.2812(4) 0.041(2) Uani 1 1 d . A 1 N2 N 0.6492(4) 0.5808(10) 0.3926(4) 0.053(2) Uani 1 1 d . A 1 C1 C 0.8817(5) 0.2596(12) 0.4368(6) 0.052(3) Uani 1 1 d . A 1 C2 C 0.8233(5) 0.2542(11) 0.4077(5) 0.048(3) Uani 1 1 d . A 1 C3 C 0.7742(4) 0.2233(12) 0.4374(6) 0.051(3) Uani 1 1 d . A 1 H3 H 0.7805 0.2184 0.4817 0.061 Uiso 1 1 calc R A 1 C4 C 0.7201(5) 0.2012(11) 0.4061(6) 0.051(3) Uani 1 1 d . A 1 H4 H 0.6907 0.1796 0.4292 0.061 Uiso 1 1 calc R A 1 C5 C 0.7058(5) 0.2088(11) 0.3410(6) 0.053(3) Uani 1 1 d . A 1 H5 H 0.6677 0.1914 0.3196 0.064 Uiso 1 1 calc R A 1 C6 C 0.7506(5) 0.2436(11) 0.3089(5) 0.050(3) Uani 1 1 d . A 1 H6 H 0.743 0.2503 0.2647 0.06 Uiso 1 1 calc R A 1 C7 C 0.8050(5) 0.2679(11) 0.3409(5) 0.051(3) Uani 1 1 d . A 1 H7 H 0.8333 0.2962 0.3172 0.061 Uiso 1 1 calc R A 1 C8 C 0.9026(5) 0.2449(13) 0.5047(6) 0.061(3) Uani 1 1 d . A 1 C9 C 0.8732(6) 0.3018(14) 0.5501(6) 0.070(4) Uani 1 1 d . A 1 H9 H 0.8398 0.3604 0.5376 0.084 Uiso 1 1 calc R A 1 C10 C 0.8928(7) 0.2729(19) 0.6139(7) 0.093(5) Uani 1 1 d . A 1 H10 H 0.8718 0.3097 0.6439 0.112 Uiso 1 1 calc R A 1 C11 C 0.9418(8) 0.193(2) 0.6332(8) 0.107(6) Uani 1 1 d . A 1 H11 H 0.9549 0.1735 0.6763 0.128 Uiso 1 1 calc R A 1 C12 C 0.9716(7) 0.1401(17) 0.5894(8) 0.092(5) Uani 1 1 d . A 1 H12 H 1.0062 0.0862 0.6023 0.11 Uiso 1 1 calc R A 1 C13 C 0.9523(6) 0.1644(15) 0.5275(6) 0.070(4) Uani 1 1 d . A 1 H13 H 0.9737 0.1246 0.4985 0.084 Uiso 1 1 calc R A 1 C14 C 0.9264(5) 0.2723(14) 0.3990(6) 0.057(3) Uani 1 1 d . A 1 C15 C 0.9693(5) 0.3803(16) 0.4114(7) 0.074(4) Uani 1 1 d . A 1 H15 H 0.9698 0.4443 0.4462 0.089 Uiso 1 1 calc R A 1 C16 C 1.0105(6) 0.397(2) 0.3752(11) 0.107(7) Uani 1 1 d . A 1 H16 H 1.0375 0.4754 0.3842 0.129 Uiso 1 1 calc R A 1 C17 C 1.0139(8) 0.307(3) 0.3279(11) 0.125(9) Uani 1 1 d . A 1 H17 H 1.0435 0.3197 0.3042 0.151 Uiso 1 1 calc R A 1 C18 C 0.9733(7) 0.192(2) 0.3129(8) 0.106(6) Uani 1 1 d . A 1 H18 H 0.9754 0.1256 0.2795 0.127 Uiso 1 1 calc R A 1 C19 C 0.9298(6) 0.1779(19) 0.3485(7) 0.088(5) Uani 1 1 d . A 1 H19 H 0.9018 0.1023 0.3382 0.105 Uiso 1 1 calc R A 1 C20 C 0.6294(5) 0.7156(13) 0.3747(6) 0.062(3) Uani 1 1 d . A 1 C21 C 0.6478(5) 0.7998(13) 0.3264(5) 0.057(3) Uani 1 1 d . A 1 H21 H 0.6374 0.9015 0.325 0.068 Uiso 1 1 calc R A 1 C22 C 0.6791(4) 0.7543(12) 0.2807(5) 0.046(3) Uani 1 1 d . A 1 C23 C 0.5848(6) 0.7954(14) 0.4049(7) 0.085(5) Uani 1 1 d . A 1 H23A H 0.5738 0.7324 0.4375 0.128 Uiso 0.5 1 calc PR A 1 H23B H 0.5508 0.8166 0.3732 0.128 Uiso 0.5 1 calc PR A 1 H23C H 0.601 0.8885 0.4235 0.128 Uiso 0.5 1 calc PR A 1 H23D H 0.5766 0.8926 0.3853 0.128 Uiso 0.5 1 calc PR A 1 H23E H 0.5996 0.8084 0.4496 0.128 Uiso 0.5 1 calc PR A 1 H23F H 0.5494 0.7366 0.3993 0.128 Uiso 0.5 1 calc PR A 1 C24 C 0.6769(5) 0.8662(13) 0.2268(6) 0.064(3) Uani 1 1 d . A 1 H24A H 0.6994 0.8281 0.1967 0.096 Uiso 0.5 1 calc PR A 1 H24B H 0.693 0.9611 0.2435 0.096 Uiso 0.5 1 calc PR A 1 H24C H 0.6369 0.8804 0.2061 0.096 Uiso 0.5 1 calc PR A 1 H24D H 0.6535 0.9516 0.2342 0.096 Uiso 0.5 1 calc PR A 1 H24E H 0.6599 0.8186 0.1874 0.096 Uiso 0.5 1 calc PR A 1 H24F H 0.716 0.8993 0.2247 0.096 Uiso 0.5 1 calc PR A 1 C25 C 0.6199(5) 0.5037(14) 0.4350(5) 0.058(3) Uani 1 1 d . A 1 C26 C 0.5711(4) 0.4189(14) 0.4111(6) 0.056(3) Uani 1 1 d . A 1 C27 C 0.5437(5) 0.3449(16) 0.4546(7) 0.076(4) Uani 1 1 d . A 1 H27 H 0.5095 0.2912 0.4397 0.091 Uiso 1 1 calc R A 1 C28 C 0.5639(7) 0.3470(19) 0.5160(7) 0.091(5) Uani 1 1 d . A 1 H28 H 0.5442 0.295 0.5437 0.109 Uiso 1 1 calc R A 1 C29 C 0.6127(7) 0.423(2) 0.5390(7) 0.102(6) Uani 1 1 d . A 1 H29 H 0.626 0.4265 0.5828 0.123 Uiso 1 1 calc R A 1 C30 C 0.6437(7) 0.4978(18) 0.4994(6) 0.092(5) Uani 1 1 d . A 1 C31 C 0.5474(5) 0.4097(18) 0.3421(6) 0.077(4) Uani 1 1 d . A 1 H31 H 0.5763 0.4552 0.3195 0.093 Uiso 1 1 calc R A 1 C32 C 0.5389(7) 0.249(2) 0.3207(8) 0.112(6) Uani 1 1 d . A 1 H32A H 0.5244 0.2457 0.2756 0.168 Uiso 1 1 calc R A 1 H32B H 0.5112 0.2006 0.3427 0.168 Uiso 1 1 calc R A 1 H32C H 0.5757 0.196 0.33 0.168 Uiso 1 1 calc R A 1 C33 C 0.4921(8) 0.491(2) 0.3232(10) 0.162(9) Uani 1 1 d . A 1 H33A H 0.479 0.4812 0.278 0.242 Uiso 1 1 calc R A 1 H33B H 0.4979 0.5964 0.3338 0.242 Uiso 1 1 calc R A 1 H33C H 0.4631 0.4499 0.3452 0.242 Uiso 1 1 calc R A 1 C34 C 0.7003(11) 0.574(3) 0.5265(8) 0.170(13) Uani 1 1 d . A 1 H34 H 0.7223 0.5862 0.4918 0.204 Uiso 1 1 calc R A 1 C35 C 0.7373(8) 0.496(3) 0.5766(9) 0.184(14) Uani 1 1 d . A 1 H35A H 0.7422 0.3931 0.5637 0.276 Uiso 1 1 calc R A 1 H35B H 0.7197 0.4964 0.6141 0.276 Uiso 1 1 calc R A 1 H35C H 0.7748 0.5445 0.5857 0.276 Uiso 1 1 calc R A 1 C36 C 0.6898(16) 0.730(2) 0.5501(11) 0.27(2) Uani 1 1 d . A 1 H36A H 0.6662 0.7866 0.5166 0.403 Uiso 1 1 calc R A 1 H36B H 0.7267 0.7803 0.5632 0.403 Uiso 1 1 calc R A 1 H36C H 0.6699 0.7226 0.5857 0.403 Uiso 1 1 calc R A 1 C37 C 0.7286(4) 0.5822(13) 0.2262(5) 0.049(3) Uani 1 1 d . A 1 C38 C 0.6920(5) 0.4980(17) 0.1815(6) 0.077(4) Uani 1 1 d . A 1 C39 C 0.7132(6) 0.4371(16) 0.1324(7) 0.081(4) Uani 1 1 d . A 1 H39 H 0.6883 0.3812 0.1018 0.097 Uiso 1 1 calc R A 1 C40 C 0.7694(6) 0.4556(14) 0.1267(6) 0.071(4) Uani 1 1 d . A 1 H40 H 0.7837 0.4105 0.0932 0.085 Uiso 1 1 calc R A 1 C41 C 0.8041(5) 0.5378(18) 0.1689(6) 0.081(5) Uani 1 1 d . A 1 H41 H 0.8427 0.5539 0.1639 0.097 Uiso 1 1 calc R A 1 C42 C 0.7850(5) 0.5996(15) 0.2194(5) 0.061(3) Uani 1 1 d . A 1 C43 C 0.6284(8) 0.472(3) 0.1857(10) 0.164(12) Uani 1 1 d . A 1 H43 H 0.6206 0.5176 0.2252 0.197 Uiso 1 1 calc R A 1 C44 C 0.5890(9) 0.545(3) 0.130(2) 0.32(3) Uani 1 1 d . A 1 H44A H 0.5976 0.6513 0.1294 0.477 Uiso 1 1 calc R A 1 H44B H 0.5488 0.5312 0.1341 0.477 Uiso 1 1 calc R A 1 H44C H 0.5956 0.4995 0.0911 0.477 Uiso 1 1 calc R A 1 C45 C 0.6117(8) 0.315(3) 0.1847(7) 0.164(11) Uani 1 1 d . A 1 H45A H 0.6434 0.256 0.2079 0.246 Uiso 1 1 calc R A 1 H45B H 0.6029 0.2797 0.1414 0.246 Uiso 1 1 calc R A 1 H45C H 0.5776 0.3031 0.204 0.246 Uiso 1 1 calc R A 1 C46 C 0.8251(5) 0.697(2) 0.2652(6) 0.100(6) Uani 1 1 d . A 1 H46 H 0.8075 0.711 0.3032 0.12 Uiso 1 1 calc R A 1 C47 C 0.8355(7) 0.851(2) 0.2394(12) 0.161(10) Uani 1 1 d . A 1 H47A H 0.8603 0.9085 0.2717 0.241 Uiso 1 1 calc R A 1 H47B H 0.7987 0.9021 0.2271 0.241 Uiso 1 1 calc R A 1 H47C H 0.8541 0.8401 0.203 0.241 Uiso 1 1 calc R A 1 C48 C 0.8849(6) 0.622(2) 0.2856(8) 0.128(8) Uani 1 1 d . A 1 H48A H 0.9097 0.6864 0.3151 0.192 Uiso 1 1 calc R A 1 H48B H 0.9026 0.6054 0.2488 0.192 Uiso 1 1 calc R A 1 H48C H 0.88 0.5268 0.3056 0.192 Uiso 1 1 calc R A 1 C49 C 0.8617(7) 0.6499(17) 0.4604(10) 0.125(7) Uani 1 1 d . A 1 H49A H 0.8627 0.5663 0.49 0.15 Uiso 1 1 calc R A 1 H49B H 0.8867 0.6246 0.4301 0.15 Uiso 1 1 calc R A 1 C50 C 0.8815(8) 0.7728(17) 0.4917(11) 0.158(11) Uani 1 1 d . A 1 H50A H 0.9167 0.8076 0.4777 0.189 Uiso 1 1 calc R A 1 H50B H 0.8911 0.7514 0.537 0.189 Uiso 1 1 calc R A 1 C51 C 0.8377(7) 0.8854(18) 0.4802(9) 0.132(8) Uani 1 1 d . A 1 H51A H 0.8215 0.9048 0.5182 0.158 Uiso 1 1 calc R A 1 H51B H 0.8537 0.9789 0.4668 0.158 Uiso 1 1 calc R A 1 C52 C 0.7943(5) 0.8275(13) 0.4313(6) 0.065(4) Uani 1 1 d . A 1 H52A H 0.7556 0.8469 0.4407 0.078 Uiso 1 1 calc R A 1 H52B H 0.797 0.8752 0.391 0.078 Uiso 1 1 calc R A 1 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 Yb 0.0608(3) 0.0387(3) 0.0454(3) -0.0052(3) 0.01668(19) -0.0146(3) O 0.078(6) 0.042(5) 0.082(6) -0.007(4) -0.007(5) -0.015(4) N1 0.030(4) 0.042(5) 0.054(5) -0.013(4) 0.014(4) -0.007(4) N2 0.083(7) 0.035(5) 0.053(6) -0.003(4) 0.045(5) -0.021(5) C1 0.042(7) 0.044(7) 0.067(8) 0.005(6) 0.002(6) -0.012(5) C2 0.059(7) 0.030(6) 0.057(7) 0.004(5) 0.010(6) -0.014(5) C3 0.040(7) 0.047(7) 0.066(8) 0.000(6) 0.010(6) 0.006(5) C4 0.054(7) 0.026(6) 0.075(9) -0.001(5) 0.017(6) -0.005(5) C5 0.057(7) 0.033(6) 0.067(8) -0.006(6) 0.004(6) -0.005(5) C6 0.076(9) 0.026(6) 0.048(7) -0.006(5) 0.010(6) 0.001(6) C7 0.053(7) 0.031(6) 0.069(8) 0.007(6) 0.016(6) -0.001(5) C8 0.056(8) 0.053(7) 0.071(9) -0.008(7) 0.006(7) -0.026(6) C9 0.063(8) 0.065(8) 0.076(9) -0.012(7) -0.001(7) -0.032(7) C10 0.090(12) 0.119(14) 0.071(10) -0.025(10) 0.014(9) -0.052(11) C11 0.092(13) 0.137(17) 0.079(12) 0.004(12) -0.021(10) -0.044(12) C12 0.092(12) 0.078(11) 0.096(12) 0.005(10) -0.012(10) -0.028(9) C13 0.068(9) 0.070(9) 0.066(9) 0.008(7) -0.006(7) -0.008(7) C14 0.047(7) 0.061(8) 0.061(8) 0.014(7) 0.004(6) -0.004(6) C15 0.040(7) 0.085(10) 0.093(10) 0.029(8) -0.002(7) -0.009(7) C16 0.041(9) 0.113(15) 0.17(2) 0.066(14) 0.025(11) 0.003(9) C17 0.052(11) 0.17(2) 0.16(2) 0.080(18) 0.049(13) 0.037(13) C18 0.081(12) 0.151(17) 0.093(12) 0.022(12) 0.033(10) 0.027(12) C19 0.062(9) 0.106(12) 0.104(12) 0.018(10) 0.037(8) 0.010(8) C20 0.076(9) 0.053(8) 0.071(8) -0.014(7) 0.049(7) -0.016(6) C21 0.065(8) 0.043(7) 0.071(8) -0.005(6) 0.040(7) -0.003(6) C22 0.043(6) 0.043(6) 0.056(7) -0.006(5) 0.022(5) -0.012(5) C23 0.107(11) 0.050(8) 0.122(12) 0.000(8) 0.085(10) 0.008(7) C24 0.069(8) 0.059(8) 0.074(8) 0.008(7) 0.044(7) 0.004(6) C25 0.082(8) 0.050(6) 0.054(6) -0.010(7) 0.047(6) 0.000(7) C26 0.031(6) 0.071(8) 0.071(8) 0.020(7) 0.022(6) 0.003(6) C27 0.040(7) 0.088(10) 0.105(12) 0.034(9) 0.028(7) -0.006(7) C28 0.091(11) 0.116(13) 0.073(10) 0.024(10) 0.037(9) -0.026(10) C29 0.119(13) 0.137(15) 0.061(9) -0.006(9) 0.045(9) -0.052(12) C30 0.138(13) 0.093(10) 0.063(8) -0.037(9) 0.063(8) -0.054(11) C31 0.046(7) 0.105(11) 0.079(10) 0.031(9) 0.007(7) -0.023(7) C32 0.082(11) 0.156(18) 0.102(13) -0.011(13) 0.026(9) -0.013(12) C33 0.128(15) 0.133(17) 0.19(2) 0.054(17) -0.068(15) 0.011(15) C34 0.23(2) 0.25(3) 0.050(9) -0.049(14) 0.077(13) -0.18(2) C35 0.133(16) 0.33(4) 0.116(15) -0.14(2) 0.092(14) -0.13(2) C36 0.54(6) 0.100(17) 0.115(18) 0.012(15) -0.08(3) -0.12(3) C37 0.042(6) 0.056(7) 0.055(7) -0.003(6) 0.027(5) -0.002(5) C38 0.068(8) 0.090(9) 0.087(9) -0.048(9) 0.047(7) -0.023(8) C39 0.069(9) 0.096(10) 0.086(10) -0.025(8) 0.035(8) 0.004(8) C40 0.069(9) 0.079(10) 0.075(8) 0.001(8) 0.037(7) 0.031(7) C41 0.046(7) 0.133(14) 0.069(8) -0.002(9) 0.025(7) -0.003(8) C42 0.037(6) 0.096(10) 0.051(7) 0.022(7) 0.016(5) 0.018(6) C43 0.096(13) 0.25(3) 0.171(19) -0.18(2) 0.076(13) -0.101(17) C44 0.065(13) 0.097(18) 0.80(9) -0.10(3) 0.10(3) -0.020(13) C45 0.128(15) 0.29(3) 0.057(10) 0.034(14) -0.028(10) -0.137(19) C46 0.042(8) 0.21(2) 0.055(8) -0.025(11) 0.017(6) -0.029(10) C47 0.071(12) 0.112(16) 0.28(3) -0.063(18) -0.014(15) -0.014(11) C48 0.058(9) 0.170(18) 0.137(15) 0.068(14) -0.033(10) -0.039(11) C49 0.108(14) 0.070(11) 0.174(19) -0.038(12) -0.038(13) -0.010(10) C50 0.128(16) 0.067(11) 0.23(2) -0.064(13) -0.097(16) 0.041(11) C51 0.109(13) 0.075(11) 0.179(19) -0.016(12) -0.061(13) 0.010(10) C52 0.069(9) 0.048(7) 0.071(9) 0.004(6) -0.005(7) -0.017(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Yb N1 2.342(9) . ? Yb N2 2.345(9) . ? Yb O 2.366(8) . ? Yb C6 2.734(10) . ? Yb C5 2.771(10) . ? Yb C7 2.773(11) . ? Yb C4 2.810(10) . ? Yb C3 2.878(11) . ? Yb C2 2.971(11) . ? O C52 1.430(14) . ? O C49 1.434(16) . ? N1 C22 1.336(13) . ? N1 C37 1.433(12) . ? N2 C20 1.337(15) . ? N2 C25 1.432(13) . ? C1 C2 1.413(14) . ? C1 C14 1.457(16) . ? C1 C8 1.477(16) . ? C2 C7 1.446(15) . ? C2 C3 1.458(15) . ? C3 C4 1.351(14) . ? C4 C5 1.399(15) . ? C5 C6 1.407(15) . ? C6 C7 1.367(15) . ? C8 C13 1.396(17) . ? C8 C9 1.405(17) . ? C9 C10 1.408(19) . ? C10 C11 1.37(2) . ? C11 C12 1.37(2) . ? C12 C13 1.360(18) . ? C14 C15 1.397(16) . ? C14 C19 1.405(18) . ? C15 C16 1.37(2) . ? C16 C17 1.33(3) . ? C17 C18 1.41(3) . ? C18 C19 1.40(2) . ? C20 C21 1.429(15) . ? C20 C23 1.522(15) . ? C21 C22 1.403(14) . ? C22 C24 1.542(15) . ? C25 C26 1.404(16) . ? C25 C30 1.415(17) . ? C26 C27 1.409(16) . ? C26 C31 1.509(17) . ? C27 C28 1.337(18) . ? C28 C29 1.361(19) . ? C29 C30 1.401(18) . ? C30 C34 1.53(2) . ? C31 C33 1.49(2) . ? C31 C32 1.53(2) . ? C34 C35 1.45(3) . ? C34 C36 1.53(3) . ? C37 C42 1.377(14) . ? C37 C38 1.404(15) . ? C38 C39 1.375(16) . ? C38 C43 1.542(19) . ? C39 C40 1.369(17) . ? C40 C41 1.341(17) . ? C41 C42 1.380(16) . ? C42 C46 1.526(19) . ? C43 C45 1.47(3) . ? C43 C44 1.54(4) . ? C46 C47 1.53(2) . ? C46 C48 1.56(2) . ? C49 C50 1.342(19) . ? C50 C51 1.44(2) . ? C51 C52 1.437(17) . ? 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 Yb N2 80.7(3) . . ? N1 Yb O 99.5(3) . . ? N2 Yb O 103.2(3) . . ? N1 Yb C6 90.8(3) . . ? N2 Yb C6 122.8(3) . . ? O Yb C6 133.9(3) . . ? N1 Yb C5 102.5(3) . . ? N2 Yb C5 97.5(3) . . ? O Yb C5 151.8(3) . . ? C6 Yb C5 29.6(3) . . ? N1 Yb C7 104.4(3) . . ? N2 Yb C7 149.0(3) . . ? O Yb C7 105.9(3) . . ? C6 Yb C7 28.7(3) . . ? C5 Yb C7 51.5(3) . . ? N1 Yb C4 130.8(3) . . ? N2 Yb C4 94.6(3) . . ? O Yb C4 128.9(3) . . ? C6 Yb C4 51.0(3) . . ? C5 Yb C4 29.0(3) . . ? C7 Yb C4 58.5(3) . . ? N1 Yb C3 149.6(3) . . ? N2 Yb C3 113.0(3) . . ? O Yb C3 103.1(3) . . ? C6 Yb C3 58.9(3) . . ? C5 Yb C3 50.5(3) . . ? C7 Yb C3 49.8(3) . . ? C4 Yb C3 27.5(3) . . ? N1 Yb C2 132.2(3) . . ? N2 Yb C2 141.8(3) . . ? O Yb C2 91.0(3) . . ? C6 Yb C2 51.8(3) . . ? C5 Yb C2 61.1(3) . . ? C7 Yb C2 28.9(3) . . ? C4 Yb C2 50.8(3) . . ? C3 Yb C2 28.8(3) . . ? C52 O C49 104.8(9) . . ? C52 O Yb 125.8(7) . . ? C49 O Yb 129.3(8) . . ? C22 N1 C37 119.2(9) . . ? C22 N1 Yb 121.1(7) . . ? C37 N1 Yb 119.0(6) . . ? C20 N2 C25 116.4(9) . . ? C20 N2 Yb 121.6(7) . . ? C25 N2 Yb 120.6(7) . . ? C2 C1 C14 119.9(10) . . ? C2 C1 C8 124.7(11) . . ? C14 C1 C8 115.2(10) . . ? C1 C2 C7 122.7(10) . . ? C1 C2 C3 126.9(11) . . ? C7 C2 C3 110.2(10) . . ? C1 C2 Yb 130.3(7) . . ? C7 C2 Yb 67.9(6) . . ? C3 C2 Yb 72.0(6) . . ? C4 C3 C2 124.2(11) . . ? C4 C3 Yb 73.5(6) . . ? C2 C3 Yb 79.1(6) . . ? C3 C4 C5 122.6(11) . . ? C3 C4 Yb 79.0(6) . . ? C5 C4 Yb 73.9(6) . . ? C4 C5 C6 116.6(10) . . ? C4 C5 Yb 77.1(6) . . ? C6 C5 Yb 73.8(6) . . ? C7 C6 C5 120.5(11) . . ? C7 C6 Yb 77.2(6) . . ? C5 C6 Yb 76.6(6) . . ? C6 C7 C2 125.6(11) . . ? C6 C7 Yb 74.1(6) . . ? C2 C7 Yb 83.2(7) . . ? C13 C8 C9 115.5(12) . . ? C13 C8 C1 120.8(12) . . ? C9 C8 C1 123.6(12) . . ? C8 C9 C10 120.7(14) . . ? C11 C10 C9 120.8(16) . . ? C10 C11 C12 118.9(16) . . ? C13 C12 C11 120.7(17) . . ? C12 C13 C8 123.3(15) . . ? C15 C14 C19 115.6(13) . . ? C15 C14 C1 121.4(12) . . ? C19 C14 C1 123.0(11) . . ? C16 C15 C14 122.2(16) . . ? C17 C16 C15 122.0(19) . . ? C16 C17 C18 119.8(18) . . ? C19 C18 C17 118.4(18) . . ? C18 C19 C14 122.0(16) . . ? N2 C20 C21 124.1(10) . . ? N2 C20 C23 122.7(10) . . ? C21 C20 C23 113.2(11) . . ? C22 C21 C20 129.5(11) . . ? N1 C22 C21 125.5(10) . . ? N1 C22 C24 121.0(9) . . ? C21 C22 C24 113.5(10) . . ? C26 C25 C30 120.1(11) . . ? C26 C25 N2 119.2(10) . . ? C30 C25 N2 120.2(11) . . ? C25 C26 C27 117.1(11) . . ? C25 C26 C31 122.1(10) . . ? C27 C26 C31 120.7(11) . . ? C28 C27 C26 122.8(13) . . ? C27 C28 C29 120.1(13) . . ? C28 C29 C30 121.4(14) . . ? C29 C30 C25 117.9(13) . . ? C29 C30 C34 119.8(13) . . ? C25 C30 C34 122.2(12) . . ? C33 C31 C26 113.4(14) . . ? C33 C31 C32 108.9(13) . . ? C26 C31 C32 111.2(12) . . ? C35 C34 C30 115.9(18) . . ? C35 C34 C36 108.0(17) . . ? C30 C34 C36 111(2) . . ? C42 C37 C38 118.5(10) . . ? C42 C37 N1 122.7(10) . . ? C38 C37 N1 118.1(9) . . ? C39 C38 C37 119.2(11) . . ? C39 C38 C43 118.8(12) . . ? C37 C38 C43 121.9(10) . . ? C40 C39 C38 121.2(13) . . ? C41 C40 C39 119.4(12) . . ? C40 C41 C42 121.5(11) . . ? C37 C42 C41 120.1(12) . . ? C37 C42 C46 119.7(11) . . ? C41 C42 C46 120.0(11) . . ? C45 C43 C44 106.2(14) . . ? C45 C43 C38 114.1(19) . . ? C44 C43 C38 110(2) . . ? C42 C46 C47 113.9(13) . . ? C42 C46 C48 111.0(15) . . ? C47 C46 C48 107.5(12) . . ? C50 C49 O 110.6(14) . . ? C49 C50 C51 108.7(14) . . ? C52 C51 C50 105.5(14) . . ? O C52 C51 107.3(11) . . ? #===END data_(9)-may804 _database_code_depnum_ccdc_archive 'CCDC 706866' _audit_creation_date 2004-05-13T11:47:01-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C46 H46 O2 Yb, C7 H8' _chemical_formula_sum 'C53 H54 O2 Yb' _chemical_formula_weight 896 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 10.1293(2) _cell_length_b 20.7321(4) _cell_length_c 21.6554(5) _cell_angle_alpha 111.214(1) _cell_angle_beta 96.485(1) _cell_angle_gamma 91.056(1) _cell_volume 4203.73(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 92121 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.682 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.265 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6447 _exptl_absorpt_correction_T_max 0.7668 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.262183E-1 _diffrn_orient_matrix_ub_12 0.392123E-1 _diffrn_orient_matrix_ub_13 -0.143447E-1 _diffrn_orient_matrix_ub_21 0.904339E-1 _diffrn_orient_matrix_ub_22 0.29304E-2 _diffrn_orient_matrix_ub_23 -0.135236E-1 _diffrn_orient_matrix_ub_31 -0.323606E-1 _diffrn_orient_matrix_ub_32 -0.337919E-1 _diffrn_orient_matrix_ub_33 -0.458922E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0714 _diffrn_reflns_av_unetI/netI 0.0472 _diffrn_reflns_number 63001 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 25.7 _diffrn_reflns_theta_full 25.7 _diffrn_measured_fraction_theta_full 0.949 _diffrn_measured_fraction_theta_max 0.949 _reflns_number_total 15191 _reflns_number_gt 12460 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; There are two independent molecules of the Yb complex. There are two independent molecules of toluene sovate, one ordered and one disordered. Both solvate molecules were refined with isotropic C atoms , and the disordered solvate molecule had SADI constraints and H atoms omitted. 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^)+(0.0372P)^2^+27.7120P] 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_number_reflns 15191 _refine_ls_number_parameters 952 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1334 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.158 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.11 _refine_diff_density_min -1.741 _refine_diff_density_rms 0.121 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.385 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Yb Yb 0.32234(3) 0.157614(16) 0.249762(16) 0.03689(10) Uani 1 1 d . . . O1 O 0.3865(6) 0.2229(3) 0.3647(3) 0.0507(14) Uani 1 1 d . A 1 O2 O 0.5177(5) 0.2013(3) 0.2232(3) 0.0529(15) Uani 1 1 d . A 1 C1 C 0.3721(7) 0.0263(4) 0.2099(4) 0.0355(16) Uani 1 1 d . A 1 C2 C 0.3160(7) 0.0286(4) 0.2702(4) 0.0342(16) Uani 1 1 d . A 1 C3 C 0.1840(7) 0.0467(4) 0.2798(4) 0.0359(16) Uani 1 1 d . A 1 H3 H 0.1318 0.0574 0.2459 0.043 Uiso 1 1 calc R A 1 C4 C 0.1269(7) 0.0498(4) 0.3352(4) 0.0380(17) Uani 1 1 d . A 1 H4 H 0.0379 0.063 0.3389 0.046 Uiso 1 1 calc R A 1 C5 C 0.1976(8) 0.0340(4) 0.3859(4) 0.0445(19) Uani 1 1 d . A 1 H5 H 0.1589 0.036 0.4245 0.053 Uiso 1 1 calc R A 1 C6 C 0.3280(8) 0.0151(4) 0.3782(4) 0.0452(19) Uani 1 1 d . A 1 H6 H 0.3788 0.0035 0.412 0.054 Uiso 1 1 calc R A 1 C7 C 0.3835(7) 0.0128(4) 0.3233(4) 0.0391(17) Uani 1 1 d . A 1 H7 H 0.4728 -0.0001 0.3204 0.047 Uiso 1 1 calc R A 1 C8 C 0.5182(7) 0.0286(4) 0.2119(4) 0.0339(16) Uani 1 1 d . A 1 C9 C 0.6042(8) 0.0728(4) 0.2695(4) 0.0433(18) Uani 1 1 d . A 1 H9 H 0.5666 0.1009 0.3078 0.052 Uiso 1 1 calc R A 1 C10 C 0.7419(8) 0.0753(4) 0.2704(5) 0.046(2) Uani 1 1 d . A 1 H10 H 0.7968 0.1048 0.3094 0.055 Uiso 1 1 calc R A 1 C11 C 0.7985(8) 0.0363(5) 0.2164(5) 0.058(2) Uani 1 1 d . A 1 H11 H 0.8925 0.0391 0.2176 0.069 Uiso 1 1 calc R A 1 C12 C 0.7203(8) -0.0074(5) 0.1599(5) 0.051(2) Uani 1 1 d . A 1 H12 H 0.7604 -0.0351 0.1223 0.061 Uiso 1 1 calc R A 1 C13 C 0.5835(8) -0.0108(4) 0.1580(4) 0.0443(19) Uani 1 1 d . A 1 H13 H 0.5314 -0.0411 0.1185 0.053 Uiso 1 1 calc R A 1 C14 C 0.2891(7) -0.0041(4) 0.1444(4) 0.0377(17) Uani 1 1 d . A 1 C15 C 0.1802(8) -0.0514(4) 0.1332(4) 0.0450(19) Uani 1 1 d . A 1 H15 H 0.1604 -0.0653 0.1686 0.054 Uiso 1 1 calc R A 1 C16 C 0.1001(9) -0.0788(5) 0.0718(4) 0.058(2) Uani 1 1 d . A 1 H16 H 0.027 -0.1105 0.0663 0.069 Uiso 1 1 calc R A 1 C17 C 0.1254(10) -0.0606(6) 0.0192(5) 0.071(3) Uani 1 1 d . A 1 H17 H 0.0695 -0.0786 -0.0224 0.085 Uiso 1 1 calc R A 1 C18 C 0.2335(10) -0.0155(5) 0.0280(4) 0.058(2) Uani 1 1 d . A 1 H18 H 0.2544 -0.0038 -0.0085 0.07 Uiso 1 1 calc R A 1 C19 C 0.3125(9) 0.0131(4) 0.0893(4) 0.0470(19) Uani 1 1 d . A 1 H19 H 0.3846 0.0452 0.0942 0.056 Uiso 1 1 calc R A 1 C20 C 0.0549(7) 0.3051(4) 0.3328(3) 0.0343(16) Uani 1 1 d . A 1 C21 C 0.0957(7) 0.2584(4) 0.2740(3) 0.0320(15) Uani 1 1 d . A 1 C22 C 0.0492(7) 0.1873(4) 0.2411(3) 0.0360(16) Uani 1 1 d . A 1 H22 H -0.0031 0.1668 0.2638 0.043 Uiso 1 1 calc R A 1 C23 C 0.0765(8) 0.1468(4) 0.1781(4) 0.0378(17) Uani 1 1 d . A 1 H23 H 0.0352 0.1013 0.1574 0.045 Uiso 1 1 calc R A 1 C24 C 0.1629(8) 0.1706(4) 0.1438(4) 0.0410(18) Uani 1 1 d . A 1 H24 H 0.1817 0.1423 0.1006 0.049 Uiso 1 1 calc R A 1 C25 C 0.2205(8) 0.2384(4) 0.1764(4) 0.0399(17) Uani 1 1 d . A 1 H25 H 0.2799 0.2563 0.1547 0.048 Uiso 1 1 calc R A 1 C26 C 0.1935(7) 0.2797(4) 0.2390(4) 0.0348(16) Uani 1 1 d . A 1 H26 H 0.2401 0.3239 0.2603 0.042 Uiso 1 1 calc R A 1 C27 C 0.0682(7) 0.3809(4) 0.3494(4) 0.0394(17) Uani 1 1 d . A 1 C28 C 0.0448(8) 0.4096(4) 0.3000(4) 0.0457(19) Uani 1 1 d . A 1 H28 H 0.0226 0.3795 0.2548 0.055 Uiso 1 1 calc R A 1 C29 C 0.0531(10) 0.4807(5) 0.3153(5) 0.060(2) Uani 1 1 d . A 1 H29 H 0.0369 0.4984 0.2805 0.072 Uiso 1 1 calc R A 1 C30 C 0.0847(10) 0.5260(5) 0.3805(6) 0.064(3) Uani 1 1 d . A 1 H30 H 0.0916 0.5746 0.3908 0.077 Uiso 1 1 calc R A 1 C31 C 0.1062(9) 0.4993(4) 0.4307(5) 0.057(2) Uani 1 1 d . A 1 H31 H 0.1261 0.5299 0.4759 0.069 Uiso 1 1 calc R A 1 C32 C 0.0987(8) 0.4283(4) 0.4154(4) 0.048(2) Uani 1 1 d . A 1 H32 H 0.1147 0.4111 0.4505 0.057 Uiso 1 1 calc R A 1 C33 C -0.0146(8) 0.2807(4) 0.3776(4) 0.0365(16) Uani 1 1 d . A 1 C34 C 0.0216(8) 0.2236(4) 0.3936(4) 0.0402(17) Uani 1 1 d . A 1 H34 H 0.0934 0.1984 0.3743 0.048 Uiso 1 1 calc R A 1 C35 C -0.0435(9) 0.2022(4) 0.4369(4) 0.0460(19) Uani 1 1 d . A 1 H35 H -0.0163 0.1628 0.4464 0.055 Uiso 1 1 calc R A 1 C36 C -0.1471(9) 0.2381(5) 0.4658(4) 0.052(2) Uani 1 1 d . A 1 H36 H -0.192 0.2236 0.4952 0.062 Uiso 1 1 calc R A 1 C37 C -0.1851(9) 0.2950(5) 0.4518(4) 0.052(2) Uani 1 1 d . A 1 H37 H -0.2564 0.3201 0.4719 0.063 Uiso 1 1 calc R A 1 C38 C -0.1210(8) 0.3162(4) 0.4089(4) 0.0473(19) Uani 1 1 d . A 1 H38 H -0.1491 0.3559 0.4001 0.057 Uiso 1 1 calc R A 1 C39 C 0.3905(12) 0.2980(4) 0.3943(4) 0.065(3) Uani 1 1 d . A 1 H39A H 0.4708 0.3185 0.3844 0.077 Uiso 1 1 calc R A 1 H39B H 0.3109 0.3153 0.3758 0.077 Uiso 1 1 calc R A 1 C40 C 0.3932(17) 0.3165(5) 0.4634(5) 0.096(5) Uani 1 1 d . A 1 H40A H 0.306 0.333 0.4769 0.115 Uiso 1 1 calc R A 1 H40B H 0.4624 0.3544 0.4873 0.115 Uiso 1 1 calc R A 1 C41 C 0.4230(14) 0.2548(5) 0.4806(5) 0.080(4) Uani 1 1 d . A 1 H41A H 0.5109 0.2621 0.5081 0.096 Uiso 1 1 calc R A 1 H41B H 0.3543 0.2455 0.5059 0.096 Uiso 1 1 calc R A 1 C42 C 0.4232(12) 0.1976(5) 0.4178(5) 0.069(3) Uani 1 1 d . A 1 H42A H 0.5129 0.1794 0.4145 0.083 Uiso 1 1 calc R A 1 H42B H 0.3588 0.1597 0.4147 0.083 Uiso 1 1 calc R A 1 C43 C 0.5660(10) 0.1754(6) 0.1592(5) 0.073(3) Uani 1 1 d . A 1 H43A H 0.5015 0.1826 0.1247 0.087 Uiso 1 1 calc R A 1 H43B H 0.579 0.1252 0.1457 0.087 Uiso 1 1 calc R A 1 C44 C 0.6929(12) 0.2141(10) 0.1665(7) 0.119(6) Uani 1 1 d . A 1 H44A H 0.761 0.1818 0.1472 0.143 Uiso 1 1 calc R A 1 H44B H 0.6823 0.2468 0.1428 0.143 Uiso 1 1 calc R A 1 C45 C 0.7321(11) 0.2501(7) 0.2341(8) 0.106(5) Uani 1 1 d . A 1 H45A H 0.7638 0.2982 0.2416 0.127 Uiso 1 1 calc R A 1 H45B H 0.8061 0.2274 0.2503 0.127 Uiso 1 1 calc R A 1 C46 C 0.6176(10) 0.2510(5) 0.2707(6) 0.069(3) Uani 1 1 d . A 1 H46A H 0.6435 0.2375 0.3096 0.082 Uiso 1 1 calc R A 1 H46B H 0.5833 0.2979 0.2868 0.082 Uiso 1 1 calc R A 1 Yb1B Yb 0.88156(3) 0.768876(16) 0.255170(16) 0.03664(10) Uani 1 1 d . . . O1B O 0.8402(6) 0.6473(3) 0.1957(3) 0.0458(13) Uani 1 1 d . B 1 O2B O 0.6641(5) 0.7966(3) 0.2227(3) 0.0434(12) Uani 1 1 d . B 1 C1B C 0.8809(7) 0.8044(3) 0.3830(3) 0.0324(15) Uani 1 1 d . B 1 C2B C 0.8183(7) 0.8708(3) 0.4012(3) 0.0319(15) Uani 1 1 d . B 1 C3B C 0.8693(8) 0.9286(4) 0.3885(4) 0.0381(17) Uani 1 1 d . B 1 H3B H 0.9509 0.9251 0.3701 0.046 Uiso 1 1 calc R B 1 C4B C 0.8062(8) 0.9889(4) 0.4015(4) 0.0432(18) Uani 1 1 d . B 1 H4B H 0.846 1.0264 0.3933 0.052 Uiso 1 1 calc R B 1 C5B C 0.6847(8) 0.9961(4) 0.4266(4) 0.0442(19) Uani 1 1 d . B 1 H5B H 0.6382 1.037 0.4334 0.053 Uiso 1 1 calc R B 1 C6B C 0.6341(8) 0.9421(4) 0.4412(4) 0.0421(18) Uani 1 1 d . B 1 H6B H 0.5529 0.9466 0.46 0.05 Uiso 1 1 calc R B 1 C7B C 0.6984(7) 0.8812(4) 0.4292(3) 0.0345(16) Uani 1 1 d . B 1 H7B H 0.6602 0.8453 0.4404 0.041 Uiso 1 1 calc R B 1 C8B C 0.7982(7) 0.7415(3) 0.3746(4) 0.0344(16) Uani 1 1 d . B 1 C9B C 0.6696(7) 0.7274(4) 0.3376(4) 0.0377(17) Uani 1 1 d . B 1 H9B H 0.6359 0.7594 0.3186 0.045 Uiso 1 1 calc R B 1 C10B C 0.5913(8) 0.6682(4) 0.3283(4) 0.048(2) Uani 1 1 d . B 1 H10B H 0.5052 0.6608 0.3035 0.058 Uiso 1 1 calc R B 1 C11B C 0.6368(9) 0.6201(4) 0.3547(5) 0.053(2) Uani 1 1 d . B 1 H11B H 0.5838 0.5792 0.3477 0.064 Uiso 1 1 calc R B 1 C12B C 0.7619(9) 0.6329(4) 0.3916(4) 0.049(2) Uani 1 1 d . B 1 H12B H 0.7942 0.6003 0.4103 0.059 Uiso 1 1 calc R B 1 C13B C 0.8407(8) 0.6915(4) 0.4020(4) 0.0393(17) Uani 1 1 d . B 1 H13B H 0.9254 0.6987 0.428 0.047 Uiso 1 1 calc R B 1 C14B C 1.0264(7) 0.8009(4) 0.3874(3) 0.0339(15) Uani 1 1 d . B 1 C15B C 1.1168(7) 0.8586(4) 0.4227(4) 0.0389(17) Uani 1 1 d . B 1 H15B H 1.0837 0.9014 0.4481 0.047 Uiso 1 1 calc R B 1 C16B C 1.2511(8) 0.8543(4) 0.4212(4) 0.0441(18) Uani 1 1 d . B 1 H16B H 1.3082 0.8948 0.4446 0.053 Uiso 1 1 calc R B 1 C17B C 1.3067(8) 0.7934(5) 0.3868(4) 0.047(2) Uani 1 1 d . B 1 H17B H 1.4002 0.7915 0.3863 0.057 Uiso 1 1 calc R B 1 C18B C 1.2220(8) 0.7351(4) 0.3533(4) 0.0423(18) Uani 1 1 d . B 1 H18B H 1.2576 0.6922 0.3303 0.051 Uiso 1 1 calc R B 1 C19B C 1.0857(7) 0.7389(4) 0.3529(4) 0.0378(17) Uani 1 1 d . B 1 H19B H 1.0296 0.6982 0.3286 0.045 Uiso 1 1 calc R B 1 C20B C 1.0999(8) 0.6824(4) 0.0967(4) 0.0414(18) Uani 1 1 d . B 1 C21B C 1.0592(8) 0.7447(4) 0.1428(4) 0.0387(17) Uani 1 1 d . B 1 C22B C 1.1267(8) 0.7818(4) 0.2088(4) 0.0400(17) Uani 1 1 d . B 1 H22B H 1.1962 0.7605 0.226 0.048 Uiso 1 1 calc R B 1 C23B C 1.0947(8) 0.8481(4) 0.2488(4) 0.0427(18) Uani 1 1 d . B 1 H23B H 1.1484 0.8729 0.2899 0.051 Uiso 1 1 calc R B 1 C24B C 0.9833(9) 0.8779(4) 0.2280(4) 0.0454(19) Uani 1 1 d . B 1 H24B H 0.9595 0.9224 0.2553 0.055 Uiso 1 1 calc R B 1 C25B C 0.9087(9) 0.8414(4) 0.1671(4) 0.0439(19) Uani 1 1 d . B 1 H25B H 0.8326 0.861 0.1529 0.053 Uiso 1 1 calc R B 1 C26B C 0.9429(8) 0.7771(4) 0.1268(4) 0.0418(18) Uani 1 1 d . B 1 H26B H 0.8867 0.753 0.0863 0.05 Uiso 1 1 calc R B 1 C27B C 1.0490(8) 0.6619(4) 0.0251(4) 0.0443(19) Uani 1 1 d . B 1 C28B C 1.0515(9) 0.7074(5) -0.0090(4) 0.052(2) Uani 1 1 d . B 1 H28B H 1.0878 0.7536 0.0146 0.063 Uiso 1 1 calc R B 1 C29B C 1.0033(11) 0.6878(6) -0.0754(5) 0.069(3) Uani 1 1 d . B 1 H29B H 1.0071 0.7202 -0.0971 0.083 Uiso 1 1 calc R B 1 C30B C 0.9496(11) 0.6216(7) -0.1106(5) 0.073(3) Uani 1 1 d . B 1 H30B H 0.914 0.6086 -0.1563 0.088 Uiso 1 1 calc R B 1 C31B C 0.9472(11) 0.5744(6) -0.0802(5) 0.074(3) Uani 1 1 d . B 1 H31B H 0.9126 0.5282 -0.105 0.089 Uiso 1 1 calc R B 1 C32B C 0.9955(10) 0.5939(5) -0.0131(4) 0.059(2) Uani 1 1 d . B 1 H32B H 0.9925 0.5607 0.0077 0.071 Uiso 1 1 calc R B 1 C33B C 1.1915(8) 0.6368(4) 0.1159(4) 0.0420(18) Uani 1 1 d . B 1 C34B C 1.1990(8) 0.6281(4) 0.1777(4) 0.0442(19) Uani 1 1 d . B 1 H34B H 1.1423 0.6531 0.2091 0.053 Uiso 1 1 calc R B 1 C35B C 1.2846(9) 0.5853(4) 0.1943(4) 0.054(2) Uani 1 1 d . B 1 H35B H 1.2867 0.5812 0.2367 0.065 Uiso 1 1 calc R B 1 C36B C 1.3686(10) 0.5475(5) 0.1501(5) 0.064(3) Uani 1 1 d . B 1 H36B H 1.4297 0.5183 0.1618 0.077 Uiso 1 1 calc R B 1 C37B C 1.3604(11) 0.5539(5) 0.0889(5) 0.069(3) Uani 1 1 d . B 1 H37B H 1.415 0.5273 0.0573 0.083 Uiso 1 1 calc R B 1 C38B C 1.2754(10) 0.5977(5) 0.0716(5) 0.059(2) Uani 1 1 d . B 1 H38B H 1.2742 0.6014 0.0291 0.07 Uiso 1 1 calc R B 1 C39B C 0.8136(13) 0.6141(5) 0.1241(5) 0.076(3) Uani 1 1 d . B 1 H39C H 0.7515 0.6409 0.1057 0.091 Uiso 1 1 calc R B 1 H39D H 0.8973 0.6118 0.104 0.091 Uiso 1 1 calc R B 1 C40B C 0.7571(17) 0.5472(6) 0.1086(6) 0.109(5) Uani 1 1 d . B 1 H40C H 0.803 0.5132 0.0741 0.131 Uiso 1 1 calc R B 1 H40D H 0.6618 0.5444 0.091 0.131 Uiso 1 1 calc R B 1 C41B C 0.7717(15) 0.5314(5) 0.1705(5) 0.088(4) Uani 1 1 d . B 1 H41C H 0.8193 0.4886 0.164 0.106 Uiso 1 1 calc R B 1 H41D H 0.6834 0.5253 0.1839 0.106 Uiso 1 1 calc R B 1 C42B C 0.8501(10) 0.5924(4) 0.2218(5) 0.054(2) Uani 1 1 d . B 1 H42C H 0.8129 0.6058 0.2647 0.065 Uiso 1 1 calc R B 1 H42D H 0.9441 0.5817 0.229 0.065 Uiso 1 1 calc R B 1 C43B C 0.6060(8) 0.8638(4) 0.2476(4) 0.0438(18) Uani 1 1 d . B 1 H43C H 0.6505 0.8979 0.2332 0.053 Uiso 1 1 calc R B 1 H43D H 0.6134 0.8821 0.297 0.053 Uiso 1 1 calc R B 1 C44B C 0.4618(11) 0.8484(6) 0.2168(7) 0.094(4) Uani 1 1 d . B 1 H44C H 0.4042 0.8486 0.2509 0.113 Uiso 1 1 calc R B 1 H44D H 0.433 0.8838 0.1983 0.113 Uiso 1 1 calc R B 1 C45B C 0.4531(12) 0.7834(9) 0.1664(7) 0.147(8) Uani 1 1 d . B 1 H45C H 0.4345 0.7885 0.1226 0.176 Uiso 1 1 calc R B 1 H45D H 0.3781 0.755 0.1711 0.176 Uiso 1 1 calc R B 1 C46B C 0.5743(11) 0.7485(5) 0.1684(5) 0.069(3) Uani 1 1 d . B 1 H46C H 0.6119 0.7367 0.1257 0.083 Uiso 1 1 calc R B 1 H46D H 0.5574 0.7052 0.1766 0.083 Uiso 1 1 calc R B 1 C1S C 0.5275(13) 0.4307(10) 0.2848(7) 0.062(5) Uiso 0.5 1 d PD C 1 C2S C 0.4358(12) 0.4484(6) 0.3286(6) 0.083(3) Uiso 1 1 d D C 1 C3S C 0.4793(17) 0.4718(10) 0.3970(8) 0.065(5) Uiso 0.5 1 d PD C 1 C4S C 0.6111(14) 0.4753(8) 0.4226(8) 0.116(5) Uiso 1 1 d D C 1 C5S C 0.7030(19) 0.4611(10) 0.3770(7) 0.067(5) Uiso 0.5 1 d PD C 1 C6S C 0.6647(11) 0.4374(6) 0.3114(6) 0.079(3) Uiso 1 1 d D C 1 C7S C 0.497(2) 0.4058(10) 0.2160(9) 0.145(7) Uiso 1 1 d D C 1 C8S C 0.572(3) 0.4503(13) 0.3558(13) 0.085(7) Uiso 0.5 1 d P C 1 C9S C 0.664(3) 0.4163(14) 0.2458(9) 0.095(8) Uiso 0.5 1 d PD C 1 C10S C 0.426(3) 0.4248(13) 0.2477(13) 0.086(7) Uiso 0.5 1 d P C 1 C11S C 0.5444(16) 0.7013(8) -0.0226(7) 0.105(4) Uiso 1 1 d . D 1 C12S C 0.4378(14) 0.7421(7) -0.0123(6) 0.092(4) Uiso 1 1 d . D 1 H12S H 0.3543 0.7191 -0.0147 0.111 Uiso 1 1 calc R D 1 C13S C 0.437(2) 0.8093(10) 0.0006(9) 0.136(6) Uiso 1 1 d . D 1 H13S H 0.3594 0.835 0.0068 0.163 Uiso 1 1 calc R D 1 C14S C 0.5799(19) 0.8406(10) 0.0044(9) 0.134(6) Uiso 1 1 d . D 1 H14S H 0.5995 0.8885 0.0142 0.161 Uiso 1 1 calc R D 1 C15S C 0.669(2) 0.7958(10) -0.0069(8) 0.130(6) Uiso 1 1 d . D 1 H15S H 0.7553 0.816 -0.0048 0.156 Uiso 1 1 calc R D 1 C16S C 0.6691(14) 0.7336(7) -0.0197(6) 0.090(4) Uiso 1 1 d . D 1 H16S H 0.7474 0.7088 -0.027 0.108 Uiso 1 1 calc R D 1 C17S C 0.5373(19) 0.6330(9) -0.0346(9) 0.139(6) Uiso 1 1 d . D 1 H17A H 0.6259 0.6152 -0.0405 0.209 Uiso 0.5 1 calc PR D 1 H17C H 0.4757 0.609 -0.0753 0.209 Uiso 0.5 1 calc PR D 1 H17D H 0.5052 0.625 0.0031 0.209 Uiso 0.5 1 calc PR D 1 H17E H 0.4453 0.6175 -0.0346 0.209 Uiso 0.5 1 calc PR D 1 H17F H 0.5955 0.6238 0.0002 0.209 Uiso 0.5 1 calc PR D 1 H17G H 0.566 0.6078 -0.0783 0.209 Uiso 0.5 1 calc PR D 1 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 Yb 0.03859(19) 0.03336(18) 0.0410(2) 0.01744(14) 0.00150(14) 0.00073(14) O1 0.069(4) 0.038(3) 0.042(3) 0.014(2) -0.003(3) 0.003(3) O2 0.035(3) 0.058(4) 0.071(4) 0.032(3) -0.002(3) -0.006(3) C1 0.033(4) 0.032(4) 0.042(4) 0.016(3) 0.002(3) -0.001(3) C2 0.031(4) 0.031(4) 0.038(4) 0.010(3) 0.002(3) 0.002(3) C3 0.035(4) 0.034(4) 0.040(4) 0.017(3) 0.000(3) -0.001(3) C4 0.029(4) 0.035(4) 0.049(5) 0.014(3) 0.006(3) 0.000(3) C5 0.047(5) 0.044(4) 0.043(4) 0.018(4) 0.006(4) -0.005(4) C6 0.047(5) 0.049(5) 0.044(5) 0.023(4) -0.001(4) -0.001(4) C7 0.032(4) 0.039(4) 0.048(4) 0.020(3) 0.000(3) 0.002(3) C8 0.033(4) 0.033(4) 0.043(4) 0.024(3) 0.004(3) 0.001(3) C9 0.040(4) 0.042(4) 0.053(5) 0.026(4) -0.001(4) -0.001(4) C10 0.033(4) 0.050(5) 0.061(5) 0.032(4) -0.008(4) -0.006(4) C11 0.031(4) 0.072(6) 0.092(7) 0.058(6) 0.002(5) -0.004(4) C12 0.039(5) 0.058(5) 0.070(6) 0.035(5) 0.021(4) 0.011(4) C13 0.039(4) 0.045(4) 0.052(5) 0.023(4) 0.004(4) 0.006(4) C14 0.031(4) 0.038(4) 0.047(4) 0.018(3) 0.005(3) 0.007(3) C15 0.040(4) 0.053(5) 0.041(4) 0.017(4) 0.003(3) -0.001(4) C16 0.046(5) 0.066(6) 0.053(5) 0.017(5) -0.005(4) -0.012(4) C17 0.056(6) 0.089(8) 0.055(6) 0.021(5) -0.020(5) -0.006(6) C18 0.071(6) 0.067(6) 0.041(5) 0.026(4) 0.001(4) 0.005(5) C19 0.053(5) 0.046(5) 0.046(5) 0.022(4) 0.005(4) 0.004(4) C20 0.035(4) 0.036(4) 0.034(4) 0.015(3) 0.008(3) 0.002(3) C21 0.032(4) 0.033(4) 0.035(4) 0.017(3) 0.005(3) -0.002(3) C22 0.037(4) 0.037(4) 0.034(4) 0.015(3) 0.002(3) 0.000(3) C23 0.040(4) 0.037(4) 0.038(4) 0.017(3) 0.002(3) 0.003(3) C24 0.045(4) 0.046(4) 0.033(4) 0.014(3) 0.007(3) 0.010(4) C25 0.040(4) 0.046(4) 0.043(4) 0.026(4) 0.012(3) 0.006(3) C26 0.033(4) 0.032(4) 0.044(4) 0.018(3) 0.005(3) -0.002(3) C27 0.035(4) 0.038(4) 0.046(4) 0.016(3) 0.008(3) 0.002(3) C28 0.041(4) 0.047(5) 0.052(5) 0.021(4) 0.008(4) 0.007(4) C29 0.069(6) 0.048(5) 0.078(7) 0.038(5) 0.019(5) 0.015(5) C30 0.061(6) 0.035(5) 0.098(8) 0.024(5) 0.016(5) 0.004(4) C31 0.051(5) 0.041(5) 0.070(6) 0.008(4) 0.010(4) 0.004(4) C32 0.050(5) 0.037(4) 0.054(5) 0.015(4) 0.006(4) 0.007(4) C33 0.041(4) 0.034(4) 0.034(4) 0.011(3) 0.004(3) 0.000(3) C34 0.044(4) 0.036(4) 0.039(4) 0.013(3) 0.002(3) 0.001(3) C35 0.058(5) 0.043(4) 0.040(4) 0.020(4) 0.003(4) -0.004(4) C36 0.051(5) 0.065(6) 0.042(5) 0.022(4) 0.013(4) -0.006(4) C37 0.043(5) 0.064(6) 0.055(5) 0.024(4) 0.020(4) 0.006(4) C38 0.050(5) 0.048(5) 0.050(5) 0.021(4) 0.015(4) 0.006(4) C39 0.098(8) 0.040(5) 0.051(5) 0.017(4) -0.007(5) -0.001(5) C40 0.183(15) 0.051(6) 0.054(6) 0.019(5) 0.016(8) 0.025(7) C41 0.141(11) 0.060(6) 0.048(6) 0.027(5) 0.017(6) 0.023(7) C42 0.104(9) 0.049(5) 0.052(6) 0.020(4) -0.008(5) 0.011(5) C43 0.060(6) 0.092(8) 0.069(7) 0.035(6) 0.008(5) -0.020(6) C44 0.053(7) 0.204(17) 0.104(11) 0.067(11) -0.004(7) -0.051(9) C45 0.042(6) 0.092(9) 0.161(14) 0.019(9) 0.014(8) -0.002(6) C46 0.063(6) 0.046(5) 0.094(8) 0.025(5) -0.003(5) -0.009(5) Yb1B 0.0432(2) 0.02974(17) 0.03803(19) 0.01364(14) 0.00544(14) 0.00250(14) O1B 0.056(3) 0.031(3) 0.046(3) 0.009(2) 0.006(3) 0.001(2) O2B 0.043(3) 0.035(3) 0.051(3) 0.015(2) -0.002(2) -0.002(2) C1B 0.027(4) 0.029(3) 0.036(4) 0.006(3) 0.004(3) -0.002(3) C2B 0.032(4) 0.032(4) 0.030(4) 0.010(3) 0.001(3) -0.002(3) C3B 0.039(4) 0.033(4) 0.044(4) 0.016(3) 0.006(3) 0.001(3) C4B 0.049(5) 0.029(4) 0.051(5) 0.016(3) 0.001(4) 0.001(3) C5B 0.045(5) 0.036(4) 0.048(5) 0.012(3) 0.000(4) 0.010(4) C6B 0.040(4) 0.045(4) 0.036(4) 0.010(3) 0.004(3) 0.007(4) C7B 0.035(4) 0.033(4) 0.036(4) 0.013(3) 0.006(3) 0.003(3) C8B 0.032(4) 0.029(4) 0.041(4) 0.010(3) 0.008(3) 0.003(3) C9B 0.031(4) 0.037(4) 0.042(4) 0.009(3) 0.009(3) 0.001(3) C10B 0.034(4) 0.040(4) 0.063(5) 0.010(4) 0.007(4) -0.005(3) C11B 0.047(5) 0.034(4) 0.078(6) 0.018(4) 0.018(4) -0.008(4) C12B 0.054(5) 0.038(4) 0.066(6) 0.027(4) 0.019(4) 0.003(4) C13B 0.036(4) 0.040(4) 0.042(4) 0.013(3) 0.008(3) 0.002(3) C14B 0.029(4) 0.040(4) 0.033(4) 0.014(3) 0.005(3) 0.001(3) C15B 0.037(4) 0.039(4) 0.037(4) 0.010(3) 0.004(3) 0.001(3) C16B 0.035(4) 0.049(5) 0.048(5) 0.019(4) 0.002(3) -0.007(4) C17B 0.028(4) 0.068(6) 0.045(5) 0.020(4) 0.001(3) -0.003(4) C18B 0.034(4) 0.051(5) 0.040(4) 0.013(4) 0.008(3) 0.009(4) C19B 0.034(4) 0.038(4) 0.037(4) 0.009(3) 0.005(3) 0.000(3) C20B 0.050(5) 0.038(4) 0.033(4) 0.010(3) 0.004(3) 0.007(4) C21B 0.045(4) 0.034(4) 0.037(4) 0.013(3) 0.005(3) 0.001(3) C22B 0.044(4) 0.040(4) 0.038(4) 0.017(3) 0.006(3) 0.003(3) C23B 0.053(5) 0.032(4) 0.043(4) 0.013(3) 0.012(4) -0.004(4) C24B 0.060(5) 0.029(4) 0.051(5) 0.015(4) 0.020(4) 0.004(4) C25B 0.054(5) 0.034(4) 0.053(5) 0.025(4) 0.015(4) 0.008(4) C26B 0.052(5) 0.041(4) 0.037(4) 0.019(3) 0.008(4) 0.005(4) C27B 0.052(5) 0.044(4) 0.036(4) 0.013(3) 0.008(4) 0.014(4) C28B 0.053(5) 0.062(5) 0.049(5) 0.026(4) 0.012(4) 0.010(4) C29B 0.070(7) 0.102(9) 0.053(6) 0.045(6) 0.023(5) 0.026(6) C30B 0.063(6) 0.115(10) 0.035(5) 0.020(6) 0.004(4) 0.014(6) C31B 0.072(7) 0.091(8) 0.042(5) 0.004(5) 0.007(5) -0.001(6) C32B 0.070(6) 0.059(6) 0.041(5) 0.009(4) 0.008(4) 0.003(5) C33B 0.046(5) 0.038(4) 0.035(4) 0.007(3) 0.001(3) 0.002(3) C34B 0.043(5) 0.036(4) 0.043(4) 0.005(3) -0.004(4) 0.004(3) C35B 0.063(6) 0.043(5) 0.052(5) 0.018(4) -0.013(4) 0.002(4) C36B 0.064(6) 0.053(5) 0.070(7) 0.017(5) -0.005(5) 0.022(5) C37B 0.069(7) 0.055(6) 0.072(7) 0.009(5) 0.012(5) 0.026(5) C38B 0.070(6) 0.050(5) 0.050(5) 0.010(4) 0.011(4) 0.022(5) C39B 0.122(10) 0.046(5) 0.047(6) 0.007(4) -0.005(6) -0.005(6) C40B 0.169(15) 0.079(8) 0.057(7) 0.007(6) -0.005(8) -0.053(9) C41B 0.143(12) 0.043(5) 0.074(7) 0.019(5) 0.011(7) -0.027(6) C42B 0.064(6) 0.040(4) 0.057(5) 0.017(4) 0.004(4) -0.004(4) C43B 0.040(4) 0.039(4) 0.050(5) 0.015(4) -0.001(4) -0.003(3) C44B 0.045(6) 0.073(7) 0.148(12) 0.032(8) -0.025(7) -0.004(5) C45B 0.049(7) 0.164(15) 0.114(11) -0.075(10) -0.015(7) 0.011(8) C46B 0.072(7) 0.053(6) 0.059(6) -0.002(5) -0.013(5) -0.007(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Yb O1 2.369(5) . ? Yb O2 2.374(6) . ? Yb C1 2.619(7) . ? Yb C23 2.742(7) . ? Yb C24 2.752(7) . ? Yb C25 2.831(7) . ? Yb C22 2.845(7) . ? Yb C2 2.864(7) . ? Yb C26 2.941(7) . ? Yb C3 2.973(7) . ? Yb C21 3.093(7) . ? Yb1B O2B 2.381(5) . ? Yb1B O1B 2.382(5) . ? Yb1B C1B 2.596(7) . ? Yb1B C23B 2.735(8) . ? Yb1B C24B 2.744(7) . ? Yb1B C22B 2.825(8) . ? Yb1B C25B 2.855(7) . ? Yb1B C14B 2.903(7) . ? Yb1B C26B 2.979(7) . ? Yb1B C19B 3.026(7) . ? Yb1B C8B 3.043(7) . ? O1 C42 1.443(10) . ? O1 C39 1.452(10) . ? O2 C43 1.439(12) . ? O2 C46 1.451(11) . ? C1 C2 1.466(10) . ? C1 C8 1.475(10) . ? C1 C14 1.478(10) . ? C2 C3 1.413(10) . ? C2 C7 1.416(10) . ? C3 C4 1.371(10) . ? C4 C5 1.385(11) . ? C5 C6 1.396(11) . ? C6 C7 1.358(11) . ? C8 C13 1.405(11) . ? C8 C9 1.431(11) . ? C9 C10 1.393(11) . ? C10 C11 1.354(13) . ? C11 C12 1.378(13) . ? C12 C13 1.381(11) . ? C14 C15 1.402(11) . ? C14 C19 1.404(11) . ? C15 C16 1.392(12) . ? C16 C17 1.371(14) . ? C17 C18 1.376(14) . ? C18 C19 1.388(12) . ? C20 C21 1.404(10) . ? C20 C33 1.479(10) . ? C20 C27 1.479(10) . ? C21 C22 1.428(10) . ? C21 C26 1.466(10) . ? C22 C23 1.382(10) . ? C23 C24 1.399(11) . ? C24 C25 1.406(11) . ? C25 C26 1.378(10) . ? C27 C28 1.400(11) . ? C27 C32 1.405(11) . ? C28 C29 1.387(12) . ? C29 C30 1.381(14) . ? C30 C31 1.384(14) . ? C31 C32 1.387(11) . ? C33 C34 1.392(10) . ? C33 C38 1.413(11) . ? C34 C35 1.393(11) . ? C35 C36 1.374(12) . ? C36 C37 1.372(12) . ? C37 C38 1.379(11) . ? C39 C40 1.400(13) . ? C40 C41 1.484(13) . ? C41 C42 1.444(13) . ? C43 C44 1.464(15) . ? C44 C45 1.386(18) . ? C45 C46 1.475(16) . ? O1B C39B 1.441(10) . ? O1B C42B 1.445(10) . ? O2B C46B 1.443(10) . ? O2B C43B 1.461(9) . ? C1B C2B 1.465(9) . ? C1B C14B 1.471(10) . ? C1B C8B 1.479(10) . ? C2B C7B 1.404(10) . ? C2B C3B 1.425(10) . ? C3B C4B 1.365(10) . ? C4B C5B 1.390(11) . ? C5B C6B 1.375(11) . ? C6B C7B 1.384(10) . ? C8B C9B 1.416(10) . ? C8B C13B 1.420(10) . ? C9B C10B 1.386(11) . ? C10B C11B 1.381(12) . ? C11B C12B 1.386(13) . ? C12B C13B 1.374(11) . ? C14B C15B 1.413(10) . ? C14B C19B 1.417(10) . ? C15B C16B 1.368(11) . ? C16B C17B 1.382(11) . ? C17B C18B 1.381(11) . ? C18B C19B 1.384(10) . ? C20B C21B 1.420(10) . ? C20B C33B 1.469(11) . ? C20B C27B 1.479(11) . ? C21B C22B 1.436(10) . ? C21B C26B 1.436(11) . ? C22B C23B 1.401(10) . ? C23B C24B 1.404(12) . ? C24B C25B 1.384(12) . ? C25B C26B 1.380(11) . ? C27B C28B 1.395(11) . ? C27B C32B 1.411(12) . ? C28B C29B 1.373(13) . ? C29B C30B 1.372(16) . ? C30B C31B 1.365(16) . ? C31B C32B 1.387(13) . ? C33B C38B 1.395(11) . ? C33B C34B 1.408(11) . ? C34B C35B 1.363(11) . ? C35B C36B 1.385(13) . ? C36B C37B 1.374(14) . ? C37B C38B 1.381(13) . ? C39B C40B 1.398(15) . ? C40B C41B 1.484(16) . ? C41B C42B 1.486(13) . ? C43B C44B 1.513(12) . ? C44B C45B 1.387(16) . ? C45B C46B 1.441(16) . ? C1S C10S 1.20(3) . ? C1S C2S 1.363(12) . ? C1S C7S 1.382(13) . ? C1S C6S 1.428(12) . ? C1S C8S 1.46(3) . ? C1S C9S 1.68(3) . ? C2S C3S 1.395(13) . ? C2S C8S 1.43(3) . ? C2S C10S 1.63(3) . ? C3S C8S 1.34(3) . ? C3S C4S 1.376(13) . ? C4S C8S 1.36(3) . ? C4S C5S 1.391(13) . ? C5S C6S 1.331(13) . ? C5S C8S 1.34(3) . ? C6S C9S 1.327(14) . ? C6S C8S 1.38(3) . ? C7S C10S 1.03(3) . ? C7S C9S 1.72(3) . ? C11S C17S 1.34(2) . ? C11S C12S 1.373(18) . ? C11S C16S 1.402(19) . ? C12S C13S 1.32(2) . ? C13S C14S 1.56(2) . ? C14S C15S 1.29(2) . ? C15S C16S 1.218(19) . ? 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 Yb O2 90.3(2) . . ? O1 Yb C1 115.7(2) . . ? O2 Yb C1 98.7(2) . . ? O1 Yb C23 127.4(2) . . ? O2 Yb C23 123.0(2) . . ? C1 Yb C23 99.5(2) . . ? O1 Yb C24 138.2(2) . . ? O2 Yb C24 93.5(2) . . ? C1 Yb C24 104.9(2) . . ? C23 Yb C24 29.5(2) . . ? O1 Yb C25 113.5(2) . . ? O2 Yb C25 77.1(2) . . ? C1 Yb C25 130.7(2) . . ? C23 Yb C25 50.7(2) . . ? C24 Yb C25 29.1(2) . . ? O1 Yb C22 98.9(2) . . ? O2 Yb C22 134.5(2) . . ? C1 Yb C22 116.3(2) . . ? C23 Yb C22 28.6(2) . . ? C24 Yb C22 51.5(2) . . ? C25 Yb C22 58.3(2) . . ? O1 Yb C2 92.95(19) . . ? O2 Yb C2 121.1(2) . . ? C1 Yb C2 30.6(2) . . ? C23 Yb C2 100.3(2) . . ? C24 Yb C2 119.7(2) . . ? C25 Yb C2 148.7(2) . . ? C22 Yb C2 103.0(2) . . ? O1 Yb C26 88.21(19) . . ? O2 Yb C26 87.18(19) . . ? C1 Yb C26 155.2(2) . . ? C23 Yb C26 58.1(2) . . ? C24 Yb C26 50.5(2) . . ? C25 Yb C26 27.5(2) . . ? C22 Yb C26 49.1(2) . . ? C2 Yb C26 151.7(2) . . ? O1 Yb C3 92.0(2) . . ? O2 Yb C3 149.0(2) . . ? C1 Yb C3 53.0(2) . . ? C23 Yb C3 78.8(2) . . ? C24 Yb C3 105.1(2) . . ? C25 Yb C3 129.3(2) . . ? C22 Yb C3 75.6(2) . . ? C2 Yb C3 27.9(2) . . ? C26 Yb C3 123.8(2) . . ? O1 Yb C21 81.03(19) . . ? O2 Yb C21 114.08(19) . . ? C1 Yb C21 143.6(2) . . ? C23 Yb C21 49.7(2) . . ? C24 Yb C21 59.5(2) . . ? C25 Yb C21 49.59(19) . . ? C22 Yb C21 27.42(19) . . ? C2 Yb C21 124.54(19) . . ? C26 Yb C21 27.98(18) . . ? C3 Yb C21 96.81(19) . . ? C42 O1 C39 107.6(6) . . ? C42 O1 Yb 128.2(5) . . ? C39 O1 Yb 124.2(5) . . ? C43 O2 C46 108.6(7) . . ? C43 O2 Yb 125.3(5) . . ? C46 O2 Yb 125.5(6) . . ? C2 C1 C8 118.2(6) . . ? C2 C1 C14 119.1(6) . . ? C8 C1 C14 118.6(6) . . ? C2 C1 Yb 84.0(4) . . ? C8 C1 Yb 102.7(4) . . ? C14 C1 Yb 103.2(4) . . ? C3 C2 C7 113.1(7) . . ? C3 C2 C1 121.6(6) . . ? C7 C2 C1 125.3(7) . . ? C3 C2 Yb 80.3(4) . . ? C7 C2 Yb 128.3(5) . . ? C1 C2 Yb 65.4(4) . . ? C4 C3 C2 123.9(7) . . ? C4 C3 Yb 130.3(5) . . ? C2 C3 Yb 71.7(4) . . ? C3 C4 C5 120.7(7) . . ? C4 C5 C6 117.4(7) . . ? C7 C6 C5 121.2(7) . . ? C6 C7 C2 123.7(7) . . ? C13 C8 C9 114.9(7) . . ? C13 C8 C1 123.3(7) . . ? C9 C8 C1 121.8(7) . . ? C13 C8 Yb 138.9(5) . . ? C9 C8 Yb 84.5(4) . . ? C1 C8 Yb 51.2(3) . . ? C10 C9 C8 121.3(8) . . ? C11 C10 C9 120.8(8) . . ? C10 C11 C12 120.3(8) . . ? C11 C12 C13 119.9(8) . . ? C12 C13 C8 122.9(8) . . ? C15 C14 C19 115.4(7) . . ? C15 C14 C1 122.2(7) . . ? C19 C14 C1 122.5(7) . . ? C15 C14 Yb 126.5(5) . . ? C19 C14 Yb 94.1(5) . . ? C1 C14 Yb 50.9(3) . . ? C16 C15 C14 122.1(8) . . ? C17 C16 C15 121.0(9) . . ? C16 C17 C18 118.4(8) . . ? C17 C18 C19 121.1(9) . . ? C18 C19 C14 122.0(8) . . ? C21 C20 C33 121.4(6) . . ? C21 C20 C27 121.3(6) . . ? C33 C20 C27 117.0(6) . . ? C20 C21 C22 126.1(6) . . ? C20 C21 C26 121.5(6) . . ? C22 C21 C26 112.4(6) . . ? C20 C21 Yb 132.0(5) . . ? C22 C21 Yb 66.6(4) . . ? C26 C21 Yb 70.2(4) . . ? C23 C22 C21 123.4(7) . . ? C23 C22 Yb 71.5(4) . . ? C21 C22 Yb 86.0(4) . . ? C22 C23 C24 122.1(7) . . ? C22 C23 Yb 79.9(4) . . ? C24 C23 Yb 75.7(4) . . ? C23 C24 C25 116.6(7) . . ? C23 C24 Yb 74.8(4) . . ? C25 C24 Yb 78.5(4) . . ? C26 C25 C24 122.0(7) . . ? C26 C25 Yb 80.7(4) . . ? C24 C25 Yb 72.3(4) . . ? C25 C26 C21 122.7(7) . . ? C25 C26 Yb 71.8(4) . . ? C21 C26 Yb 81.8(4) . . ? C28 C27 C32 116.2(7) . . ? C28 C27 C20 121.5(7) . . ? C32 C27 C20 122.3(7) . . ? C29 C28 C27 121.9(8) . . ? C30 C29 C28 120.7(9) . . ? C29 C30 C31 118.9(8) . . ? C30 C31 C32 120.4(9) . . ? C31 C32 C27 121.9(8) . . ? C34 C33 C38 115.5(7) . . ? C34 C33 C20 123.3(7) . . ? C38 C33 C20 121.1(7) . . ? C33 C34 C35 122.5(7) . . ? C36 C35 C34 119.9(8) . . ? C37 C36 C35 119.4(8) . . ? C36 C37 C38 120.7(8) . . ? C37 C38 C33 121.9(8) . . ? C40 C39 O1 107.6(8) . . ? C39 C40 C41 108.7(8) . . ? C42 C41 C40 106.0(8) . . ? O1 C42 C41 108.0(7) . . ? O2 C43 C44 106.8(10) . . ? C45 C44 C43 108.2(11) . . ? C44 C45 C46 108.9(10) . . ? O2 C46 C45 105.5(9) . . ? O2B Yb1B O1B 94.50(18) . . ? O2B Yb1B C1B 101.0(2) . . ? O1B Yb1B C1B 113.0(2) . . ? O2B Yb1B C23B 118.3(2) . . ? O1B Yb1B C23B 125.7(2) . . ? C1B Yb1B C23B 102.2(2) . . ? O2B Yb1B C24B 88.6(2) . . ? O1B Yb1B C24B 135.5(2) . . ? C1B Yb1B C24B 109.8(2) . . ? C23B Yb1B C24B 29.7(2) . . ? O2B Yb1B C22B 130.8(2) . . ? O1B Yb1B C22B 96.7(2) . . ? C1B Yb1B C22B 117.7(2) . . ? C23B Yb1B C22B 29.1(2) . . ? C24B Yb1B C22B 51.7(2) . . ? O2B Yb1B C25B 73.0(2) . . ? O1B Yb1B C25B 111.7(2) . . ? C1B Yb1B C25B 135.2(2) . . ? C23B Yb1B C25B 50.8(2) . . ? C24B Yb1B C25B 28.5(2) . . ? C22B Yb1B C25B 58.4(2) . . ? O2B Yb1B C14B 130.08(19) . . ? O1B Yb1B C14B 112.40(19) . . ? C1B Yb1B C14B 30.4(2) . . ? C23B Yb1B C14B 79.5(2) . . ? C24B Yb1B C14B 98.5(2) . . ? C22B Yb1B C14B 88.4(2) . . ? C25B Yb1B C14B 126.9(2) . . ? O2B Yb1B C26B 84.6(2) . . ? O1B Yb1B C26B 86.5(2) . . ? C1B Yb1B C26B 158.8(2) . . ? C23B Yb1B C26B 57.9(2) . . ? C24B Yb1B C26B 49.5(2) . . ? C22B Yb1B C26B 48.7(2) . . ? C25B Yb1B C26B 27.3(2) . . ? C14B Yb1B C26B 135.8(2) . . ? O2B Yb1B C19B 151.95(19) . . ? O1B Yb1B C19B 89.16(19) . . ? C1B Yb1B C19B 52.5(2) . . ? C23B Yb1B C19B 80.7(2) . . ? C24B Yb1B C19B 108.0(2) . . ? C22B Yb1B C19B 76.0(2) . . ? C25B Yb1B C19B 130.9(2) . . ? C14B Yb1B C19B 27.56(19) . . ? C26B Yb1B C19B 123.4(2) . . ? O2B Yb1B C8B 93.22(19) . . ? O1B Yb1B C8B 86.04(18) . . ? C1B Yb1B C8B 29.1(2) . . ? C23B Yb1B C8B 129.3(2) . . ? C24B Yb1B C8B 138.2(2) . . ? C22B Yb1B C8B 135.2(2) . . ? C25B Yb1B C8B 157.9(2) . . ? C14B Yb1B C8B 50.46(19) . . ? C26B Yb1B C8B 172.1(2) . . ? C19B Yb1B C8B 59.24(19) . . ? C39B O1B C42B 106.3(6) . . ? C39B O1B Yb1B 125.3(5) . . ? C42B O1B Yb1B 128.1(5) . . ? C46B O2B C43B 109.8(6) . . ? C46B O2B Yb1B 122.6(5) . . ? C43B O2B Yb1B 127.3(4) . . ? C2B C1B C14B 121.6(6) . . ? C2B C1B C8B 118.3(6) . . ? C14B C1B C8B 118.7(6) . . ? C2B C1B Yb1B 102.6(4) . . ? C14B C1B Yb1B 86.5(4) . . ? C8B C1B Yb1B 92.5(4) . . ? C7B C2B C3B 114.4(6) . . ? C7B C2B C1B 122.4(6) . . ? C3B C2B C1B 123.1(6) . . ? C7B C2B Yb1B 130.7(5) . . ? C3B C2B Yb1B 89.5(4) . . ? C1B C2B Yb1B 51.3(3) . . ? C4B C3B C2B 123.0(7) . . ? C3B C4B C5B 120.9(7) . . ? C6B C5B C4B 117.7(7) . . ? C5B C6B C7B 121.8(7) . . ? C6B C7B C2B 122.1(7) . . ? C9B C8B C13B 115.5(7) . . ? C9B C8B C1B 121.2(6) . . ? C13B C8B C1B 123.3(7) . . ? C9B C8B Yb1B 84.6(4) . . ? C13B C8B Yb1B 129.9(5) . . ? C1B C8B Yb1B 58.5(4) . . ? C10B C9B C8B 122.1(7) . . ? C10B C9B Yb1B 135.2(5) . . ? C8B C9B Yb1B 69.6(4) . . ? C11B C10B C9B 120.8(8) . . ? C10B C11B C12B 118.3(7) . . ? C13B C12B C11B 121.8(8) . . ? C12B C13B C8B 121.5(7) . . ? C15B C14B C19B 115.0(6) . . ? C15B C14B C1B 123.5(6) . . ? C19B C14B C1B 121.4(6) . . ? C15B C14B Yb1B 126.5(5) . . ? C19B C14B Yb1B 81.0(4) . . ? C1B C14B Yb1B 63.2(4) . . ? C16B C15B C14B 121.6(7) . . ? C15B C16B C17B 122.4(8) . . ? C18B C17B C16B 117.9(7) . . ? C17B C18B C19B 120.5(7) . . ? C18B C19B C14B 122.6(7) . . ? C18B C19B Yb1B 129.6(5) . . ? C14B C19B Yb1B 71.4(4) . . ? C21B C20B C33B 123.7(7) . . ? C21B C20B C27B 118.8(7) . . ? C33B C20B C27B 117.5(6) . . ? C20B C21B C22B 125.0(7) . . ? C20B C21B C26B 121.8(7) . . ? C22B C21B C26B 113.1(7) . . ? C20B C21B Yb1B 130.8(5) . . ? C22B C21B Yb1B 65.9(4) . . ? C26B C21B Yb1B 72.1(4) . . ? C23B C22B C21B 122.9(7) . . ? C23B C22B Yb1B 71.9(4) . . ? C21B C22B Yb1B 86.5(5) . . ? C22B C23B C24B 119.9(8) . . ? C22B C23B Yb1B 79.0(4) . . ? C24B C23B Yb1B 75.5(5) . . ? C25B C24B C23B 118.8(7) . . ? C25B C24B Yb1B 80.2(4) . . ? C23B C24B Yb1B 74.8(4) . . ? C26B C25B C24B 121.1(8) . . ? C26B C25B Yb1B 81.4(4) . . ? C24B C25B Yb1B 71.3(4) . . ? C25B C26B C21B 123.4(8) . . ? C25B C26B Yb1B 71.4(4) . . ? C21B C26B Yb1B 80.6(4) . . ? C28B C27B C32B 116.0(8) . . ? C28B C27B C20B 122.8(8) . . ? C32B C27B C20B 121.2(7) . . ? C29B C28B C27B 122.2(9) . . ? C30B C29B C28B 120.2(10) . . ? C31B C30B C29B 120.1(9) . . ? C30B C31B C32B 119.9(11) . . ? C31B C32B C27B 121.5(10) . . ? C38B C33B C34B 116.0(7) . . ? C38B C33B C20B 120.4(7) . . ? C34B C33B C20B 123.6(7) . . ? C35B C34B C33B 122.5(8) . . ? C34B C35B C36B 120.9(9) . . ? C37B C36B C35B 117.6(8) . . ? C36B C37B C38B 122.2(9) . . ? C37B C38B C33B 120.9(9) . . ? C40B C39B O1B 108.7(9) . . ? C39B C40B C41B 108.1(9) . . ? C40B C41B C42B 105.1(8) . . ? O1B C42B C41B 105.8(8) . . ? O2B C43B C44B 104.0(7) . . ? C45B C44B C43B 106.9(10) . . ? C44B C45B C46B 111.6(10) . . ? C45B C46B O2B 105.6(8) . . ? C10S C1S C2S 78.6(16) . . ? C10S C1S C7S 46.5(14) . . ? C2S C1S C7S 124.8(15) . . ? C10S C1S C6S 162.7(19) . . ? C2S C1S C6S 117.9(13) . . ? C7S C1S C6S 117.3(14) . . ? C10S C1S C8S 139(2) . . ? C2S C1S C8S 60.8(12) . . ? C7S C1S C8S 172.7(19) . . ? C6S C1S C8S 57.3(12) . . ? C10S C1S C9S 113.5(17) . . ? C2S C1S C9S 167.5(14) . . ? C7S C1S C9S 67.6(13) . . ? C6S C1S C9S 49.8(8) . . ? C8S C1S C9S 107.0(15) . . ? C1S C2S C3S 119.1(13) . . ? C1S C2S C8S 62.8(13) . . ? C3S C2S C8S 56.4(13) . . ? C1S C2S C10S 46.3(12) . . ? C3S C2S C10S 164.8(15) . . ? C8S C2S C10S 109.1(15) . . ? C8S C3S C4S 60.0(14) . . ? C8S C3S C2S 63.0(14) . . ? C4S C3S C2S 123.0(16) . . ? C8S C4S C3S 58.5(14) . . ? C8S C4S C5S 58.6(14) . . ? C3S C4S C5S 116.6(16) . . ? C6S C5S C8S 62.2(14) . . ? C6S C5S C4S 121.6(16) . . ? C8S C5S C4S 59.4(14) . . ? C9S C6S C5S 163.3(18) . . ? C9S C6S C8S 137.3(19) . . ? C5S C6S C8S 59.4(14) . . ? C9S C6S C1S 75.0(15) . . ? C5S C6S C1S 121.5(13) . . ? C8S C6S C1S 62.4(13) . . ? C10S C7S C1S 57.5(18) . . ? C10S C7S C9S 121(2) . . ? C1S C7S C9S 64.4(11) . . ? C3S C8S C5S 123(2) . . ? C3S C8S C4S 61.5(12) . . ? C5S C8S C4S 62.0(13) . . ? C3S C8S C6S 171(2) . . ? C5S C8S C6S 58.4(12) . . ? C4S C8S C6S 120(2) . . ? C3S C8S C2S 60.5(12) . . ? C5S C8S C2S 170(2) . . ? C4S C8S C2S 122.0(19) . . ? C6S C8S C2S 116.6(19) . . ? C3S C8S C1S 116.8(19) . . ? C5S C8S C1S 118.5(19) . . ? C4S C8S C1S 174(2) . . ? C6S C8S C1S 60.3(12) . . ? C2S C8S C1S 56.4(11) . . ? C6S C9S C1S 55.2(10) . . ? C6S C9S C7S 103.1(17) . . ? C1S C9S C7S 47.9(9) . . ? C7S C10S C1S 75.9(19) . . ? C7S C10S C2S 131(2) . . ? C1S C10S C2S 55.1(12) . . ? C17S C11S C12S 124.4(16) . . ? C17S C11S C16S 118.2(16) . . ? C12S C11S C16S 117.4(14) . . ? C13S C12S C11S 128.2(16) . . ? C12S C13S C14S 110.5(17) . . ? C15S C14S C13S 114.1(19) . . ? C16S C15S C14S 135(2) . . ? C15S C16S C11S 114.8(16) . . ? #====END