Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Glen B. Deacon' 'Craig M. Forsyth' _publ_contact_author_name 'Prof Glen B Deacon' _publ_contact_author_address ; School of Chemistry Monash University Wellington Rd Clayton Victoria 3800 AUSTRALIA ; _publ_contact_author_email 'GLEN.DEACON@SCI.MONASH.EDU.AU' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Linkage Isomerism and C-H activation in an ytterbium(II) tetraphenylborate ; data_1a _database_code_CSD 192054 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(bis(trimethylsilyl)amido)(tetrahydrofuran) (eta6,eta4-tetraphenylborato)ytterbium(II)] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H46 B N O Si2 Yb' _chemical_formula_weight 724.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 9.6210(1) _cell_length_b 15.7886(2) _cell_length_c 22.2434(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.931(1) _cell_angle_gamma 90.00 _cell_volume 3374.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 2.868 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'none' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius KAPPA CCD' _diffrn_measurement_method '1 deg scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42816 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_sigmaI/netI 0.0684 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8258 _reflns_number_gt 5754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1994)' _computing_cell_refinement 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_data_reduction 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'POVRAY 3.0' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8258 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0578 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.227652(14) 0.211688(9) 0.920959(5) 0.02375(5) Uani 1 1 d . . . Si1 Si 0.32474(11) 0.30091(7) 1.06558(4) 0.0333(2) Uani 1 1 d . . . Si2 Si 0.54323(10) 0.23725(8) 0.98639(4) 0.0441(3) Uani 1 1 d . . . O1 O 0.1244(2) 0.34625(14) 0.91556(9) 0.0304(5) Uani 1 1 d . . . N1 N 0.3743(3) 0.25602(18) 1.00052(11) 0.0273(6) Uani 1 1 d . . . C1 C 0.1314(4) 0.3190(2) 1.06593(15) 0.0388(9) Uani 1 1 d . . . H1A H 0.1012 0.3534 1.0310 0.058 Uiso 1 1 calc R . . H1B H 0.1092 0.3486 1.1030 0.058 Uiso 1 1 calc R . . H1C H 0.0830 0.2643 1.0640 0.058 Uiso 1 1 calc R . . C2 C 0.3673(5) 0.2366(3) 1.13445(16) 0.0699(15) Uani 1 1 d . . . H2A H 0.4673 0.2244 1.1373 0.105 Uiso 1 1 calc R . . H2B H 0.3150 0.1834 1.1321 0.105 Uiso 1 1 calc R . . H2C H 0.3420 0.2684 1.1701 0.105 Uiso 1 1 calc R . . C3 C 0.4027(4) 0.4088(3) 1.07924(16) 0.0550(12) Uani 1 1 d . . . H3A H 0.3830 0.4446 1.0438 0.083 Uiso 1 1 calc R . . H3B H 0.5036 0.4035 1.0866 0.083 Uiso 1 1 calc R . . H3C H 0.3621 0.4346 1.1144 0.083 Uiso 1 1 calc R . . C4 C 0.6696(5) 0.2369(4) 1.05311(19) 0.104(2) Uani 1 1 d . . . H4A H 0.6389 0.1961 1.0829 0.156 Uiso 1 1 calc R . . H4B H 0.6741 0.2936 1.0710 0.156 Uiso 1 1 calc R . . H4C H 0.7619 0.2207 1.0404 0.156 Uiso 1 1 calc R . . C5 C 0.6108(5) 0.3168(3) 0.93306(19) 0.0769(16) Uani 1 1 d . . . H5A H 0.5483 0.3197 0.8969 0.115 Uiso 1 1 calc R . . H5B H 0.7040 0.3000 0.9218 0.115 Uiso 1 1 calc R . . H5C H 0.6156 0.3725 0.9525 0.115 Uiso 1 1 calc R . . C6 C 0.5585(4) 0.1306(3) 0.94935(15) 0.0516(11) Uani 1 1 d . . . H6A H 0.4938 0.1277 0.9139 0.077 Uiso 1 1 calc R . . H6B H 0.5358 0.0860 0.9779 0.077 Uiso 1 1 calc R . . H6C H 0.6539 0.1226 0.9370 0.077 Uiso 1 1 calc R . . C7 C 0.2084(4) 0.4237(2) 0.91509(14) 0.0357(9) Uani 1 1 d . . . H7A H 0.2477 0.4322 0.8753 0.043 Uiso 1 1 calc R . . H7B H 0.2857 0.4211 0.9462 0.043 Uiso 1 1 calc R . . C8 C 0.1091(4) 0.4938(2) 0.92853(14) 0.0391(9) Uani 1 1 d . . . H8A H 0.1402 0.5487 0.9123 0.047 Uiso 1 1 calc R . . H8B H 0.0977 0.4995 0.9723 0.047 Uiso 1 1 calc R . . C9 C -0.0243(4) 0.4636(2) 0.89595(15) 0.0417(10) Uani 1 1 d . . . H9A H -0.1069 0.4892 0.9135 0.050 Uiso 1 1 calc R . . H9B H -0.0251 0.4777 0.8526 0.050 Uiso 1 1 calc R . . C10 C -0.0209(3) 0.3691(2) 0.90559(15) 0.0383(9) Uani 1 1 d . . . H10A H -0.0740 0.3536 0.9409 0.046 Uiso 1 1 calc R . . H10B H -0.0622 0.3394 0.8698 0.046 Uiso 1 1 calc R . . C11 C 0.0719(3) 0.0632(2) 0.88861(12) 0.0234(7) Uani 1 1 d . . . C12 C -0.0225(3) 0.1168(2) 0.91676(13) 0.0277(8) Uani 1 1 d . . . H12 H -0.0979 0.1404 0.8931 0.033 Uiso 1 1 calc R . . C13 C -0.0095(4) 0.1364(2) 0.97794(14) 0.0338(8) Uani 1 1 d . . . H13 H -0.0757 0.1725 0.9952 0.041 Uiso 1 1 calc R . . C14 C 0.0993(4) 0.1035(2) 1.01351(14) 0.0342(9) Uani 1 1 d . . . H14 H 0.1086 0.1172 1.0551 0.041 Uiso 1 1 calc R . . C15 C 0.1941(4) 0.0506(2) 0.98834(13) 0.0312(8) Uani 1 1 d . . . H15 H 0.2688 0.0274 1.0126 0.037 Uiso 1 1 calc R . . C16 C 0.1806(3) 0.0309(2) 0.92663(12) 0.0262(8) Uani 1 1 d . . . H16 H 0.2472 -0.0056 0.9100 0.031 Uiso 1 1 calc R . . C21 C 0.1616(3) 0.1403(2) 0.80048(11) 0.0229(7) Uani 1 1 d . . . C22 C 0.1018(3) 0.2206(2) 0.78866(12) 0.0263(8) Uani 1 1 d . . . H22 H 0.0035 0.2245 0.7827 0.032 Uiso 1 1 calc R . . C23 C 0.1807(4) 0.2944(2) 0.78535(13) 0.0314(8) Uani 1 1 d . . . H23 H 0.1363 0.3469 0.7762 0.038 Uiso 1 1 calc R . . C24 C 0.3250(4) 0.2911(2) 0.79541(14) 0.0332(8) Uani 1 1 d . . . H24 H 0.3793 0.3413 0.7942 0.040 Uiso 1 1 calc R . . C25 C 0.3877(3) 0.2137(2) 0.80714(13) 0.0295(8) Uani 1 1 d . . . H25 H 0.4859 0.2105 0.8138 0.035 Uiso 1 1 calc R . . C26 C 0.3075(3) 0.1401(2) 0.80920(12) 0.0269(8) Uani 1 1 d . . . H26 H 0.3535 0.0876 0.8168 0.032 Uiso 1 1 calc R . . C31 C -0.0888(3) 0.0545(2) 0.78576(13) 0.0231(7) Uani 1 1 d . . . C32 C -0.1266(3) 0.0892(2) 0.72932(13) 0.0282(8) Uani 1 1 d . . . H32 H -0.0578 0.1170 0.7074 0.034 Uiso 1 1 calc R . . C33 C -0.2627(4) 0.0840(2) 0.70431(14) 0.0331(8) Uani 1 1 d . . . H33 H -0.2846 0.1091 0.6662 0.040 Uiso 1 1 calc R . . C34 C -0.3649(4) 0.0435(2) 0.73383(14) 0.0347(9) Uani 1 1 d . . . H34 H -0.4571 0.0404 0.7166 0.042 Uiso 1 1 calc R . . C35 C -0.3314(3) 0.0074(2) 0.78892(14) 0.0354(9) Uani 1 1 d . . . H35 H -0.4007 -0.0214 0.8100 0.043 Uiso 1 1 calc R . . C36 C -0.1963(3) 0.0130(2) 0.81383(14) 0.0309(8) Uani 1 1 d . . . H36 H -0.1759 -0.0127 0.8519 0.037 Uiso 1 1 calc R . . C41 C 0.1453(3) -0.0307(2) 0.79310(12) 0.0245(7) Uani 1 1 d . . . C42 C 0.2295(3) -0.0340(2) 0.74353(13) 0.0311(8) Uani 1 1 d . . . H42 H 0.2483 0.0171 0.7228 0.037 Uiso 1 1 calc R . . C43 C 0.2866(4) -0.1092(3) 0.72361(15) 0.0406(10) Uani 1 1 d . . . H43 H 0.3432 -0.1084 0.6899 0.049 Uiso 1 1 calc R . . C44 C 0.2623(4) -0.1841(3) 0.75181(16) 0.0416(10) Uani 1 1 d . . . H44 H 0.3021 -0.2353 0.7383 0.050 Uiso 1 1 calc R . . C45 C 0.1783(4) -0.1838(2) 0.80077(15) 0.0369(9) Uani 1 1 d . . . H45 H 0.1590 -0.2353 0.8209 0.044 Uiso 1 1 calc R . . C46 C 0.1229(3) -0.1086(2) 0.82006(13) 0.0303(8) Uani 1 1 d . . . H46 H 0.0661 -0.1101 0.8537 0.036 Uiso 1 1 calc R . . B1 B 0.0700(4) 0.0553(2) 0.81474(14) 0.0227(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.02455(9) 0.02332(9) 0.02352(9) -0.00032(6) 0.00258(5) 0.00084(7) Si1 0.0330(6) 0.0441(7) 0.0227(5) 0.0001(4) 0.0008(4) 0.0063(5) Si2 0.0240(6) 0.0759(9) 0.0320(5) -0.0109(5) -0.0030(4) 0.0079(6) O1 0.0245(13) 0.0274(15) 0.0390(12) 0.0023(10) -0.0010(9) 0.0019(11) N1 0.0207(15) 0.0357(18) 0.0254(14) 0.0024(12) 0.0005(11) 0.0072(13) C1 0.037(2) 0.042(2) 0.038(2) -0.0090(17) 0.0074(16) 0.0073(19) C2 0.072(3) 0.106(4) 0.032(2) 0.025(2) 0.007(2) 0.032(3) C3 0.051(3) 0.064(3) 0.049(2) -0.023(2) -0.0023(19) -0.005(2) C4 0.042(3) 0.216(7) 0.051(3) -0.053(3) -0.019(2) 0.055(4) C5 0.054(3) 0.112(5) 0.067(3) -0.023(3) 0.025(2) -0.039(3) C6 0.036(2) 0.079(3) 0.040(2) 0.001(2) 0.0045(16) 0.026(2) C7 0.036(2) 0.033(2) 0.038(2) 0.0007(16) 0.0002(15) -0.0007(18) C8 0.050(3) 0.035(2) 0.0330(19) -0.0016(16) 0.0044(16) 0.005(2) C9 0.044(2) 0.040(3) 0.040(2) -0.0007(17) -0.0086(17) 0.0179(19) C10 0.028(2) 0.043(3) 0.044(2) -0.0027(18) -0.0020(15) 0.0103(19) C11 0.0214(18) 0.0209(19) 0.0285(17) 0.0045(14) 0.0064(13) -0.0023(14) C12 0.0230(19) 0.027(2) 0.0335(19) -0.0013(15) 0.0061(13) -0.0007(15) C13 0.035(2) 0.034(2) 0.034(2) -0.0061(16) 0.0187(15) -0.0023(18) C14 0.051(2) 0.030(2) 0.0232(18) -0.0003(15) 0.0113(16) -0.0083(18) C15 0.043(2) 0.023(2) 0.0267(18) 0.0060(14) -0.0011(15) -0.0023(17) C16 0.0299(19) 0.021(2) 0.0281(18) 0.0024(14) 0.0041(14) -0.0014(15) C21 0.0226(18) 0.031(2) 0.0151(15) -0.0004(13) 0.0021(12) -0.0001(16) C22 0.0286(19) 0.031(2) 0.0194(16) 0.0017(14) 0.0003(13) 0.0019(17) C23 0.047(2) 0.025(2) 0.0226(17) 0.0004(14) 0.0004(15) 0.0012(18) C24 0.039(2) 0.037(2) 0.0238(18) -0.0043(16) 0.0043(14) -0.014(2) C25 0.0255(18) 0.043(2) 0.0205(17) -0.0054(15) 0.0054(13) -0.0096(19) C26 0.0258(19) 0.035(2) 0.0196(16) -0.0016(14) 0.0024(12) 0.0012(17) C31 0.0229(18) 0.0181(18) 0.0285(17) -0.0020(13) 0.0030(13) 0.0054(14) C32 0.031(2) 0.026(2) 0.0275(18) -0.0035(14) 0.0007(14) -0.0007(16) C33 0.042(2) 0.026(2) 0.0300(18) -0.0031(15) -0.0101(16) 0.0012(17) C34 0.026(2) 0.036(2) 0.041(2) -0.0078(17) -0.0072(16) 0.0015(17) C35 0.025(2) 0.036(2) 0.046(2) -0.0016(17) 0.0049(16) -0.0021(17) C36 0.026(2) 0.035(2) 0.0321(18) 0.0040(15) 0.0011(14) -0.0028(16) C41 0.0195(18) 0.029(2) 0.0244(17) -0.0034(14) -0.0043(13) 0.0006(15) C42 0.0267(19) 0.037(2) 0.0295(18) -0.0071(15) 0.0006(14) -0.0035(17) C43 0.029(2) 0.053(3) 0.041(2) -0.0199(19) 0.0053(15) 0.0025(19) C44 0.029(2) 0.042(3) 0.053(2) -0.021(2) -0.0081(17) 0.0080(19) C45 0.043(2) 0.026(2) 0.040(2) -0.0069(16) -0.0114(17) 0.0043(18) C46 0.033(2) 0.032(2) 0.0258(17) -0.0067(15) -0.0019(14) 0.0027(17) B1 0.021(2) 0.023(2) 0.0240(19) 0.0006(15) 0.0015(14) 0.0018(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N1 2.314(3) . ? Yb1 O1 2.346(2) . ? Yb1 C12 2.833(3) . ? Yb1 C11 2.855(3) . ? Yb1 C26 2.871(3) . ? Yb1 C16 2.894(3) . ? Yb1 C13 2.919(3) . ? Yb1 C21 2.946(3) . ? Yb1 C15 2.978(3) . ? Yb1 C14 2.990(3) . ? Yb1 C25 3.030(3) . ? Yb1 C22 3.128(3) . ? Si1 N1 1.701(3) . ? Si1 C2 1.865(4) . ? Si1 C3 1.880(4) . ? Si1 C1 1.882(4) . ? Si2 N1 1.697(3) . ? Si2 C5 1.867(5) . ? Si2 C4 1.870(4) . ? Si2 C6 1.883(4) . ? O1 C10 1.450(4) . ? O1 C7 1.466(4) . ? C7 C8 1.502(5) . ? C8 C9 1.518(5) . ? C9 C10 1.508(5) . ? C11 C16 1.406(4) . ? C11 C12 1.411(4) . ? C11 B1 1.647(4) . ? C12 C13 1.395(4) . ? C13 C14 1.381(5) . ? C14 C15 1.377(5) . ? C15 C16 1.407(4) . ? C21 C26 1.408(4) . ? C21 C22 1.410(4) . ? C21 B1 1.645(5) . ? C22 C23 1.396(4) . ? C23 C24 1.396(5) . ? C24 C25 1.382(5) . ? C25 C26 1.397(4) . ? C31 C36 1.399(4) . ? C31 C32 1.400(4) . ? C31 B1 1.627(5) . ? C32 C33 1.398(4) . ? C33 C34 1.369(5) . ? C34 C35 1.375(4) . ? C35 C36 1.390(4) . ? C41 C46 1.390(4) . ? C41 C42 1.402(4) . ? C41 B1 1.624(5) . ? C42 C43 1.390(5) . ? C43 C44 1.365(5) . ? C44 C45 1.389(5) . ? C45 C46 1.379(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Yb1 O1 90.30(9) . . ? N1 Yb1 C12 131.98(9) . . ? O1 Yb1 C12 96.92(9) . . ? N1 Yb1 C11 137.11(9) . . ? O1 Yb1 C11 121.03(9) . . ? C12 Yb1 C11 28.74(8) . . ? N1 Yb1 C26 126.97(9) . . ? O1 Yb1 C26 116.34(8) . . ? C12 Yb1 C26 91.59(9) . . ? C11 Yb1 C26 67.58(9) . . ? N1 Yb1 C16 110.83(9) . . ? O1 Yb1 C16 145.97(9) . . ? C12 Yb1 C16 49.09(9) . . ? C11 Yb1 C16 28.30(8) . . ? C26 Yb1 C16 72.46(9) . . ? N1 Yb1 C13 104.51(9) . . ? O1 Yb1 C13 93.02(9) . . ? C12 Yb1 C13 28.02(8) . . ? C11 Yb1 C13 50.44(9) . . ? C26 Yb1 C13 117.72(10) . . ? C16 Yb1 C13 56.76(10) . . ? N1 Yb1 C21 154.94(9) . . ? O1 Yb1 C21 103.21(8) . . ? C12 Yb1 C21 67.93(9) . . ? C11 Yb1 C21 51.00(8) . . ? C26 Yb1 C21 27.97(8) . . ? C16 Yb1 C21 68.62(8) . . ? C13 Yb1 C21 95.86(9) . . ? N1 Yb1 C15 87.18(9) . . ? O1 Yb1 C15 137.97(9) . . ? C12 Yb1 C15 56.71(9) . . ? C11 Yb1 C15 49.95(9) . . ? C26 Yb1 C15 98.05(10) . . ? C16 Yb1 C15 27.68(8) . . ? C13 Yb1 C15 47.66(10) . . ? C21 Yb1 C15 96.16(9) . . ? N1 Yb1 C14 84.46(9) . . ? O1 Yb1 C14 111.34(9) . . ? C12 Yb1 C14 48.72(9) . . ? C11 Yb1 C14 58.29(8) . . ? C26 Yb1 C14 120.61(10) . . ? C16 Yb1 C14 48.35(9) . . ? C13 Yb1 C14 26.99(9) . . ? C21 Yb1 C14 109.28(9) . . ? C15 Yb1 C14 26.68(9) . . ? N1 Yb1 C25 108.66(9) . . ? O1 Yb1 C25 100.36(9) . . ? C12 Yb1 C25 116.43(9) . . ? C11 Yb1 C25 94.61(9) . . ? C26 Yb1 C25 27.21(9) . . ? C16 Yb1 C25 97.70(9) . . ? C13 Yb1 C25 143.98(9) . . ? C21 Yb1 C25 48.64(8) . . ? C15 Yb1 C25 120.14(10) . . ? C14 Yb1 C25 145.75(10) . . ? N1 Yb1 C22 153.82(9) . . ? O1 Yb1 C22 76.62(8) . . ? C12 Yb1 C22 72.86(9) . . ? C11 Yb1 C22 68.08(9) . . ? C26 Yb1 C22 46.44(9) . . ? C16 Yb1 C22 91.79(8) . . ? C13 Yb1 C22 98.81(9) . . ? C21 Yb1 C22 26.64(8) . . ? C15 Yb1 C22 117.73(9) . . ? C14 Yb1 C22 121.31(9) . . ? C25 Yb1 C22 53.28(9) . . ? N1 Si1 C2 114.37(18) . . ? N1 Si1 C3 112.85(16) . . ? C2 Si1 C3 106.9(2) . . ? N1 Si1 C1 112.75(14) . . ? C2 Si1 C1 104.74(19) . . ? C3 Si1 C1 104.36(18) . . ? N1 Si2 C5 111.60(19) . . ? N1 Si2 C4 116.32(17) . . ? C5 Si2 C4 105.8(3) . . ? N1 Si2 C6 109.51(16) . . ? C5 Si2 C6 106.6(2) . . ? C4 Si2 C6 106.4(2) . . ? C10 O1 C7 108.6(3) . . ? C10 O1 Yb1 129.5(2) . . ? C7 O1 Yb1 121.60(18) . . ? Si2 N1 Si1 122.88(16) . . ? Si2 N1 Yb1 110.96(13) . . ? Si1 N1 Yb1 126.16(13) . . ? O1 C7 C8 104.9(3) . . ? C7 C8 C9 101.8(3) . . ? C10 C9 C8 103.4(3) . . ? O1 C10 C9 106.3(3) . . ? C16 C11 C12 115.2(3) . . ? C16 C11 B1 122.9(3) . . ? C12 C11 B1 120.9(3) . . ? C16 C11 Yb1 77.42(18) . . ? C12 C11 Yb1 74.76(18) . . ? B1 C11 Yb1 106.99(19) . . ? C13 C12 C11 122.5(3) . . ? C13 C12 Yb1 79.44(19) . . ? C11 C12 Yb1 76.50(18) . . ? C14 C13 C12 120.2(3) . . ? C14 C13 Yb1 79.38(19) . . ? C12 C13 Yb1 72.54(18) . . ? C15 C14 C13 119.6(3) . . ? C15 C14 Yb1 76.16(18) . . ? C13 C14 Yb1 73.63(18) . . ? C14 C15 C16 120.0(3) . . ? C14 C15 Yb1 77.17(19) . . ? C16 C15 Yb1 72.86(18) . . ? C11 C16 C15 122.4(3) . . ? C11 C16 Yb1 74.28(19) . . ? C15 C16 Yb1 79.46(19) . . ? C26 C21 C22 115.0(3) . . ? C26 C21 B1 120.7(3) . . ? C22 C21 B1 123.5(3) . . ? C26 C21 Yb1 73.05(16) . . ? C22 C21 Yb1 83.86(17) . . ? B1 C21 Yb1 103.26(16) . . ? C23 C22 C21 122.9(3) . . ? C23 C22 Yb1 84.35(18) . . ? C21 C22 Yb1 69.50(15) . . ? C22 C23 C24 120.0(3) . . ? C22 C23 Yb1 70.73(17) . . ? C24 C23 Yb1 75.52(18) . . ? C25 C24 C23 118.9(3) . . ? C25 C24 Yb1 68.77(17) . . ? C23 C24 Yb1 79.86(19) . . ? C24 C25 C26 120.4(3) . . ? C24 C25 Yb1 86.07(19) . . ? C26 C25 Yb1 70.07(16) . . ? C25 C26 C21 122.8(3) . . ? C25 C26 Yb1 82.72(17) . . ? C21 C26 Yb1 78.98(16) . . ? C36 C31 C32 114.8(3) . . ? C36 C31 B1 121.8(3) . . ? C32 C31 B1 123.2(3) . . ? C33 C32 C31 122.0(3) . . ? C34 C33 C32 121.1(3) . . ? C33 C34 C35 118.7(3) . . ? C34 C35 C36 120.1(3) . . ? C35 C36 C31 123.3(3) . . ? C46 C41 C42 114.5(3) . . ? C46 C41 B1 122.1(3) . . ? C42 C41 B1 123.3(3) . . ? C43 C42 C41 122.4(3) . . ? C44 C43 C42 121.0(3) . . ? C43 C44 C45 118.5(4) . . ? C46 C45 C44 119.7(4) . . ? C45 C46 C41 123.9(3) . . ? C41 B1 C31 107.5(3) . . ? C41 B1 C21 111.9(3) . . ? C31 B1 C21 115.5(3) . . ? C41 B1 C11 112.1(3) . . ? C31 B1 C11 111.0(2) . . ? C21 B1 C11 98.8(2) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.349 _refine_diff_density_min -0.864 _refine_diff_density_rms 0.114 #====END data_1b _database_code_CSD 192055 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(bis(trimethylsilyl)amido)(tetrahydrofuran) (eta6,eta1-tetraphenylborato)ytterbium(II)] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H46 B N O Si2 Yb' _chemical_formula_weight 724.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 14.1600(2) _cell_length_b 14.5302(2) _cell_length_c 16.3056(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3354.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 2.885 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'none' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius KAPPA CCD' _diffrn_measurement_method '1 deg scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46392 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.27 _reflns_number_total 7833 _reflns_number_gt 5736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1994)' _computing_cell_refinement 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_data_reduction 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'POVRAY 3.0' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.022(8) _refine_ls_number_reflns 7833 _refine_ls_number_parameters 362 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0634 _refine_ls_wR_factor_gt 0.0577 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.012308(9) 0.246739(9) 0.25945(4) 0.01525(5) Uani 1 1 d . . . Si1 Si 0.12753(10) 0.43685(8) 0.29794(7) 0.0261(3) Uani 1 1 d . . . O1 O -0.0898(2) 0.25322(17) 0.37308(17) 0.0220(7) Uani 1 1 d . . . N1 N 0.0715(3) 0.3856(2) 0.21835(19) 0.0194(8) Uani 1 1 d . . . C1 C 0.1140(3) 0.3636(3) 0.3938(2) 0.0304(12) Uani 1 1 d . . . H1A H 0.1404 0.3022 0.3837 0.046 Uiso 1 1 calc R . . H1B H 0.0469 0.3580 0.4076 0.046 Uiso 1 1 calc R . . H1C H 0.1478 0.3926 0.4394 0.046 Uiso 1 1 calc R . . B1 B -0.0343(3) 0.0555(3) 0.1129(3) 0.0173(10) Uani 1 1 d . . . Si2 Si 0.07037(9) 0.42956(8) 0.12082(7) 0.0237(3) Uani 1 1 d . . . C2 C 0.2584(3) 0.4481(3) 0.2854(3) 0.0459(14) Uani 1 1 d . . . H2A H 0.2852 0.3883 0.2703 0.069 Uiso 1 1 calc R . . H2B H 0.2864 0.4691 0.3371 0.069 Uiso 1 1 calc R . . H2C H 0.2721 0.4930 0.2421 0.069 Uiso 1 1 calc R . . C3 C 0.0772(4) 0.5528(3) 0.3270(3) 0.0475(15) Uani 1 1 d . . . H3A H 0.0808 0.5944 0.2797 0.071 Uiso 1 1 calc R . . H3B H 0.1137 0.5787 0.3726 0.071 Uiso 1 1 calc R . . H3C H 0.0112 0.5456 0.3437 0.071 Uiso 1 1 calc R . . C4 C 0.1117(4) 0.3442(3) 0.0425(2) 0.0368(13) Uani 1 1 d . . . H4A H 0.0735 0.2881 0.0465 0.055 Uiso 1 1 calc R . . H4B H 0.1782 0.3292 0.0526 0.055 Uiso 1 1 calc R . . H4C H 0.1050 0.3707 -0.0124 0.055 Uiso 1 1 calc R . . C5 C 0.1491(4) 0.5323(3) 0.1051(3) 0.0441(14) Uani 1 1 d . . . H5A H 0.1324 0.5804 0.1446 0.066 Uiso 1 1 calc R . . H5B H 0.1409 0.5558 0.0492 0.066 Uiso 1 1 calc R . . H5C H 0.2151 0.5142 0.1132 0.066 Uiso 1 1 calc R . . C6 C -0.0511(4) 0.4679(3) 0.0881(3) 0.0409(13) Uani 1 1 d . . . H6A H -0.0755 0.5129 0.1276 0.061 Uiso 1 1 calc R . . H6B H -0.0934 0.4146 0.0861 0.061 Uiso 1 1 calc R . . H6C H -0.0475 0.4963 0.0337 0.061 Uiso 1 1 calc R . . C7 C -0.1526(3) 0.3290(3) 0.3927(3) 0.0269(11) Uani 1 1 d . . . H7A H -0.1798 0.3559 0.3422 0.032 Uiso 1 1 calc R . . H7B H -0.1185 0.3777 0.4230 0.032 Uiso 1 1 calc R . . C8 C -0.2289(3) 0.2871(3) 0.4454(2) 0.0284(11) Uani 1 1 d . . . H8A H -0.2783 0.2573 0.4115 0.034 Uiso 1 1 calc R . . H8B H -0.2587 0.3338 0.4812 0.034 Uiso 1 1 calc R . . C9 C -0.1743(4) 0.2169(4) 0.4949(3) 0.0379(13) Uani 1 1 d . . . H9A H -0.1441 0.2458 0.5432 0.046 Uiso 1 1 calc R . . H9B H -0.2159 0.1663 0.5135 0.046 Uiso 1 1 calc R . . C10 C -0.1010(3) 0.1822(3) 0.4351(3) 0.0327(12) Uani 1 1 d . . . H10A H -0.0403 0.1710 0.4636 0.039 Uiso 1 1 calc R . . H10B H -0.1221 0.1239 0.4096 0.039 Uiso 1 1 calc R . . C11 C 0.0485(3) 0.0765(3) 0.1822(2) 0.0171(10) Uani 1 1 d . . . C12 C 0.0317(3) 0.0509(2) 0.2650(3) 0.0177(8) Uani 1 1 d . . . H12 H -0.0214 0.0135 0.2774 0.021 Uiso 1 1 calc R . . C13 C 0.0911(3) 0.0792(3) 0.3288(2) 0.0227(11) Uani 1 1 d . . . H13 H 0.0779 0.0606 0.3835 0.027 Uiso 1 1 calc R . . C14 C 0.1687(3) 0.1338(3) 0.3128(2) 0.0224(11) Uani 1 1 d . . . H14 H 0.2083 0.1542 0.3562 0.027 Uiso 1 1 calc R . . C15 C 0.1880(3) 0.1588(3) 0.2317(2) 0.0205(10) Uani 1 1 d . . . H15 H 0.2416 0.1958 0.2198 0.025 Uiso 1 1 calc R . . C16 C 0.1291(3) 0.1296(3) 0.1682(2) 0.0170(9) Uani 1 1 d . . . H16 H 0.1444 0.1464 0.1135 0.020 Uiso 1 1 calc R . . C21 C -0.1223(3) 0.1177(3) 0.1476(2) 0.0163(9) Uani 1 1 d . . . C22 C -0.1229(3) 0.2141(3) 0.1408(2) 0.0155(9) Uani 1 1 d . . . H22 H -0.0748 0.2437 0.1099 0.019 Uiso 1 1 calc R . . C23 C -0.1931(3) 0.2677(3) 0.1787(2) 0.0246(10) Uani 1 1 d . . . H23 H -0.1921 0.3327 0.1726 0.029 Uiso 1 1 calc R . . C24 C -0.2633(3) 0.2269(3) 0.2245(3) 0.0258(11) Uani 1 1 d . . . H24 H -0.3107 0.2634 0.2499 0.031 Uiso 1 1 calc R . . C25 C -0.2638(3) 0.1322(3) 0.2331(2) 0.0222(10) Uani 1 1 d . . . H25 H -0.3115 0.1032 0.2650 0.027 Uiso 1 1 calc R . . C26 C -0.1951(3) 0.0796(3) 0.1955(2) 0.0205(10) Uani 1 1 d . . . H26 H -0.1971 0.0146 0.2022 0.025 Uiso 1 1 calc R . . C31 C 0.0028(3) 0.0849(3) 0.0216(2) 0.0165(9) Uani 1 1 d . . . C32 C -0.0447(3) 0.1423(3) -0.0330(2) 0.0216(9) Uani 1 1 d . . . H32 H -0.1045 0.1664 -0.0175 0.026 Uiso 1 1 calc R . . C33 C -0.0082(3) 0.1658(3) -0.1092(3) 0.0255(11) Uani 1 1 d . . . H33 H -0.0422 0.2066 -0.1437 0.031 Uiso 1 1 calc R . . C34 C 0.0764(3) 0.1306(3) -0.1349(2) 0.0262(11) Uani 1 1 d . . . H34 H 0.1014 0.1471 -0.1870 0.031 Uiso 1 1 calc R . . C35 C 0.1253(3) 0.0703(3) -0.0837(2) 0.0227(10) Uani 1 1 d . . . H35 H 0.1836 0.0444 -0.1009 0.027 Uiso 1 1 calc R . . C36 C 0.0882(3) 0.0484(3) -0.0078(2) 0.0191(9) Uani 1 1 d . . . H36 H 0.1221 0.0067 0.0261 0.023 Uiso 1 1 calc R . . C40 C -0.0622(3) -0.0542(2) 0.1077(2) 0.0154(9) Uani 1 1 d . . . C41 C -0.1374(3) -0.0822(3) 0.0593(2) 0.0180(9) Uani 1 1 d . . . H41 H -0.1732 -0.0365 0.0316 0.022 Uiso 1 1 calc R . . C42 C -0.1632(3) -0.1740(3) 0.0495(2) 0.0226(10) Uani 1 1 d . . . H42 H -0.2156 -0.1899 0.0159 0.027 Uiso 1 1 calc R . . C43 C -0.1121(3) -0.2417(3) 0.0886(3) 0.0253(10) Uani 1 1 d . . . H43 H -0.1288 -0.3047 0.0824 0.030 Uiso 1 1 calc R . . C44 C -0.0365(3) -0.2169(3) 0.1370(3) 0.0262(10) Uani 1 1 d . . . H44 H -0.0015 -0.2631 0.1648 0.031 Uiso 1 1 calc R . . C45 C -0.0108(3) -0.1248(3) 0.1456(2) 0.0200(10) Uani 1 1 d . . . H45 H 0.0428 -0.1096 0.1780 0.024 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 Yb1 0.01965(8) 0.01029(7) 0.01580(8) 0.00083(10) 0.0017(2) 0.00005(8) Si1 0.0371(9) 0.0163(6) 0.0250(6) 0.0017(5) -0.0040(6) -0.0082(6) O1 0.030(2) 0.0153(17) 0.0213(16) 0.0011(12) 0.0090(13) 0.0031(14) N1 0.028(2) 0.0114(17) 0.0182(17) 0.0029(14) -0.0011(16) -0.0062(16) C1 0.046(3) 0.021(3) 0.024(2) 0.0004(19) -0.006(2) -0.004(2) B1 0.012(3) 0.017(2) 0.023(3) 0.0053(19) 0.004(2) 0.000(2) Si2 0.0309(8) 0.0171(6) 0.0232(6) 0.0068(5) -0.0009(5) -0.0048(6) C2 0.044(3) 0.048(3) 0.046(3) 0.005(2) -0.009(2) -0.017(3) C3 0.082(5) 0.020(3) 0.040(3) -0.001(2) -0.006(3) -0.001(3) C4 0.048(4) 0.036(3) 0.026(3) 0.008(2) 0.007(2) 0.000(2) C5 0.063(4) 0.037(3) 0.032(3) 0.016(2) -0.007(2) -0.021(3) C6 0.047(4) 0.039(3) 0.037(3) 0.013(2) 0.004(3) 0.010(3) C7 0.035(3) 0.020(2) 0.025(2) -0.0048(19) 0.004(2) 0.006(2) C8 0.029(3) 0.031(3) 0.025(2) -0.003(2) 0.001(2) 0.004(2) C9 0.035(3) 0.049(3) 0.030(3) 0.014(2) 0.007(2) 0.010(3) C10 0.046(3) 0.025(3) 0.027(2) 0.010(2) 0.011(2) 0.006(2) C11 0.023(3) 0.009(2) 0.019(2) -0.0029(16) 0.0052(19) 0.0045(19) C12 0.027(2) 0.0072(15) 0.019(2) 0.004(2) 0.001(2) 0.0040(14) C13 0.039(3) 0.016(2) 0.013(2) -0.0006(17) -0.010(2) 0.011(2) C14 0.023(3) 0.017(2) 0.027(3) -0.0062(19) -0.011(2) 0.007(2) C15 0.014(2) 0.016(2) 0.032(3) -0.0044(17) -0.0026(17) 0.0007(18) C16 0.015(2) 0.015(2) 0.020(2) -0.0026(18) 0.0038(19) 0.0065(19) C21 0.019(2) 0.014(2) 0.016(2) -0.0003(16) -0.0048(17) 0.0029(17) C22 0.017(3) 0.015(2) 0.014(2) -0.0019(19) -0.0006(17) 0.001(2) C23 0.030(3) 0.025(3) 0.019(2) -0.0001(18) -0.0031(18) 0.006(2) C24 0.019(3) 0.032(3) 0.026(2) -0.0074(18) 0.0004(18) 0.0075(19) C25 0.014(2) 0.027(2) 0.026(3) 0.0000(17) 0.0031(16) -0.0037(19) C26 0.022(3) 0.019(2) 0.021(2) -0.0013(17) 0.0006(17) 0.0000(19) C31 0.020(3) 0.0107(19) 0.019(2) -0.0023(16) -0.0002(16) -0.0056(16) C32 0.024(3) 0.020(2) 0.021(2) -0.0027(17) -0.0024(19) 0.0025(19) C33 0.034(3) 0.022(3) 0.021(2) 0.002(2) -0.004(2) -0.002(2) C34 0.039(3) 0.025(3) 0.014(2) -0.0003(18) 0.001(2) -0.013(2) C35 0.025(3) 0.021(2) 0.023(2) -0.0080(19) 0.003(2) -0.007(2) C36 0.021(3) 0.012(2) 0.024(2) -0.0027(17) 0.0016(18) -0.0028(17) C40 0.021(3) 0.010(2) 0.015(2) -0.0025(15) 0.0032(17) 0.0010(18) C41 0.020(3) 0.015(2) 0.019(2) -0.0015(17) 0.0019(18) -0.0009(18) C42 0.024(3) 0.027(3) 0.017(2) -0.0062(18) 0.0034(17) -0.007(2) C43 0.033(3) 0.014(2) 0.029(2) -0.0053(18) 0.0066(19) 0.000(2) C44 0.037(3) 0.015(2) 0.026(2) -0.0012(19) -0.003(2) 0.007(2) C45 0.021(3) 0.023(2) 0.017(2) -0.0043(18) -0.0034(18) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N1 2.285(3) . ? Yb1 O1 2.352(3) . ? Yb1 C22 2.763(4) . ? Yb1 C16 2.802(4) . ? Yb1 C11 2.823(4) . ? Yb1 C15 2.834(4) . ? Yb1 C12 2.860(3) . ? Yb1 C14 2.890(4) . ? Yb1 C13 2.907(4) . ? Yb1 C1 3.123(4) . ? Yb1 C23 3.207(5) . ? Si1 N1 1.694(3) . ? Si1 C2 1.872(5) . ? Si1 C3 1.890(5) . ? Si1 C1 1.900(4) . ? O1 C7 1.451(5) . ? O1 C10 1.453(5) . ? N1 Si2 1.714(3) . ? B1 C31 1.636(6) . ? B1 C21 1.640(6) . ? B1 C40 1.645(6) . ? B1 C11 1.657(6) . ? Si2 C4 1.873(4) . ? Si2 C5 1.881(5) . ? Si2 C6 1.885(5) . ? C7 C8 1.509(6) . ? C8 C9 1.514(6) . ? C9 C10 1.510(6) . ? C11 C16 1.396(6) . ? C11 C12 1.419(6) . ? C12 C13 1.399(6) . ? C13 C14 1.381(6) . ? C14 C15 1.398(5) . ? C15 C16 1.396(5) . ? C21 C22 1.405(5) . ? C21 C26 1.406(5) . ? C22 C23 1.406(6) . ? C23 C24 1.377(6) . ? C24 C25 1.384(5) . ? C25 C26 1.381(5) . ? C31 C32 1.394(6) . ? C31 C36 1.406(5) . ? C32 C33 1.387(6) . ? C33 C34 1.367(6) . ? C34 C35 1.396(6) . ? C35 C36 1.381(5) . ? C40 C41 1.386(5) . ? C40 C45 1.403(6) . ? C41 C42 1.392(5) . ? C42 C43 1.378(6) . ? C43 C44 1.377(6) . ? C44 C45 1.393(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 N1 Yb1 O1 114.90(11) . . ? N1 Yb1 C22 101.55(12) . . ? O1 Yb1 C22 97.62(12) . . ? N1 Yb1 C16 99.46(12) . . ? O1 Yb1 C16 143.68(11) . . ? C22 Yb1 C16 86.15(12) . . ? N1 Yb1 C11 125.20(13) . . ? O1 Yb1 C11 119.88(11) . . ? C22 Yb1 C11 70.31(12) . . ? C16 Yb1 C11 28.75(11) . . ? N1 Yb1 C15 91.69(12) . . ? O1 Yb1 C15 133.12(11) . . ? C22 Yb1 C15 114.78(12) . . ? C16 Yb1 C15 28.68(10) . . ? C11 Yb1 C15 51.24(12) . . ? N1 Yb1 C12 148.47(12) . . ? O1 Yb1 C12 94.25(11) . . ? C22 Yb1 C12 85.29(12) . . ? C16 Yb1 C12 49.87(12) . . ? C11 Yb1 C12 28.92(11) . . ? C15 Yb1 C12 58.12(11) . . ? N1 Yb1 C14 107.98(13) . . ? O1 Yb1 C14 104.87(11) . . ? C22 Yb1 C14 130.11(12) . . ? C16 Yb1 C14 50.39(12) . . ? C11 Yb1 C14 59.83(12) . . ? C15 Yb1 C14 28.26(11) . . ? C12 Yb1 C14 49.61(11) . . ? N1 Yb1 C13 135.47(13) . . ? O1 Yb1 C13 87.88(11) . . ? C22 Yb1 C13 113.23(13) . . ? C16 Yb1 C13 58.06(12) . . ? C11 Yb1 C13 50.92(11) . . ? C15 Yb1 C13 49.26(12) . . ? C12 Yb1 C13 28.06(11) . . ? C14 Yb1 C13 27.55(11) . . ? N1 Yb1 C1 63.68(11) . . ? O1 Yb1 C1 73.10(11) . . ? C22 Yb1 C1 154.70(12) . . ? C16 Yb1 C1 115.49(13) . . ? C11 Yb1 C1 134.85(12) . . ? C15 Yb1 C1 87.25(12) . . ? C12 Yb1 C1 118.31(12) . . ? C14 Yb1 C1 75.17(12) . . ? C13 Yb1 C1 90.32(12) . . ? N1 Yb1 C23 97.36(12) . . ? O1 Yb1 C23 76.24(11) . . ? C22 Yb1 C23 25.90(11) . . ? C16 Yb1 C23 112.03(11) . . ? C11 Yb1 C23 93.72(11) . . ? C15 Yb1 C23 140.68(11) . . ? C12 Yb1 C23 101.23(11) . . ? C14 Yb1 C23 150.74(11) . . ? C13 Yb1 C23 125.96(12) . . ? C1 Yb1 C23 130.89(11) . . ? N1 Si1 C2 114.75(19) . . ? N1 Si1 C3 114.0(2) . . ? C2 Si1 C3 108.8(2) . . ? N1 Si1 C1 109.66(18) . . ? C2 Si1 C1 103.8(2) . . ? C3 Si1 C1 104.8(2) . . ? C7 O1 C10 108.6(3) . . ? C7 O1 Yb1 125.5(2) . . ? C10 O1 Yb1 125.9(2) . . ? Si1 N1 Si2 123.46(19) . . ? Si1 N1 Yb1 109.59(16) . . ? Si2 N1 Yb1 126.72(17) . . ? Si1 C1 Yb1 76.96(13) . . ? C31 B1 C21 114.5(3) . . ? C31 B1 C40 106.4(3) . . ? C21 B1 C40 111.7(3) . . ? C31 B1 C11 110.2(3) . . ? C21 B1 C11 101.6(3) . . ? C40 B1 C11 112.6(3) . . ? N1 Si2 C4 112.50(18) . . ? N1 Si2 C5 114.64(18) . . ? C4 Si2 C5 104.3(2) . . ? N1 Si2 C6 112.4(2) . . ? C4 Si2 C6 106.7(2) . . ? C5 Si2 C6 105.5(2) . . ? O1 C7 C8 105.0(3) . . ? C7 C8 C9 102.0(4) . . ? C10 C9 C8 103.4(3) . . ? O1 C10 C9 106.7(3) . . ? C16 C11 C12 115.9(4) . . ? C16 C11 B1 124.6(3) . . ? C12 C11 B1 118.8(4) . . ? C16 C11 Yb1 74.8(2) . . ? C12 C11 Yb1 77.0(2) . . ? B1 C11 Yb1 109.7(2) . . ? C13 C12 C11 122.0(4) . . ? C13 C12 Yb1 77.9(2) . . ? C11 C12 Yb1 74.1(2) . . ? C14 C13 C12 120.4(4) . . ? C14 C13 Yb1 75.5(2) . . ? C12 C13 Yb1 74.1(2) . . ? C13 C14 C15 118.9(4) . . ? C13 C14 Yb1 76.9(2) . . ? C15 C14 Yb1 73.6(2) . . ? C16 C15 C14 120.4(4) . . ? C16 C15 Yb1 74.4(2) . . ? C14 C15 Yb1 78.1(3) . . ? C15 C16 C11 122.3(4) . . ? C15 C16 Yb1 76.9(2) . . ? C11 C16 Yb1 76.5(2) . . ? C22 C21 C26 115.6(4) . . ? C22 C21 B1 121.7(4) . . ? C26 C21 B1 122.1(3) . . ? C21 C22 C23 121.4(4) . . ? C21 C22 Yb1 96.4(2) . . ? C23 C22 Yb1 95.0(2) . . ? C24 C23 C22 120.7(4) . . ? C24 C23 Yb1 113.0(3) . . ? C22 C23 Yb1 59.1(2) . . ? C23 C24 C25 119.1(4) . . ? C26 C25 C24 120.1(4) . . ? C25 C26 C21 123.0(4) . . ? C32 C31 C36 115.0(4) . . ? C32 C31 B1 125.7(4) . . ? C36 C31 B1 119.2(4) . . ? C33 C32 C31 122.6(4) . . ? C34 C33 C32 120.7(4) . . ? C33 C34 C35 119.0(4) . . ? C36 C35 C34 119.5(4) . . ? C35 C36 C31 123.1(4) . . ? C41 C40 C45 115.8(4) . . ? C41 C40 B1 119.9(3) . . ? C45 C40 B1 124.2(4) . . ? C40 C41 C42 123.2(4) . . ? C43 C42 C41 119.6(4) . . ? C44 C43 C42 119.0(4) . . ? C43 C44 C45 120.9(4) . . ? C44 C45 C40 121.5(4) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.395 _refine_diff_density_min -1.487 _refine_diff_density_rms 0.107 #====END data_2 _database_code_CSD 192056 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(trimethylsilyl)(eta2, eta2-triphenyl)boramethylene (dimethylsilyl)amido)bis(tetrahydrofuran)ytterbium(II)] (2) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H48 B N O2 Si2 Yb' _chemical_formula_weight 718.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 9.9426(1) _cell_length_b 18.7251(2) _cell_length_c 18.3353(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.633(1) _cell_angle_gamma 90.00 _cell_volume 3343.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 2.896 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'none' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius KAPPA CCD' _diffrn_measurement_method '1 deg scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35579 _diffrn_reflns_av_R_equivalents 0.0794 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.30 _reflns_number_total 8208 _reflns_number_gt 7220 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1994)' _computing_cell_refinement 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_data_reduction 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'POVRAY 3.0' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+1.0471P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8208 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.614483(10) 0.297098(6) 0.769141(6) 0.01803(6) Uani 1 1 d . . . Si1 Si 0.59575(7) 0.38734(4) 0.61297(4) 0.02113(16) Uani 1 1 d . . . O1 O 0.5231(2) 0.22841(12) 0.85917(12) 0.0283(4) Uani 1 1 d . . . N1 N 0.5253(2) 0.38749(12) 0.69039(13) 0.0217(5) Uani 1 1 d . . . C1 C 0.6722(3) 0.29786(13) 0.59510(19) 0.0229(6) Uani 1 1 d . . . H1A H 0.6074 0.2785 0.5531 0.028 Uiso 1 1 calc R . . H1B H 0.7531 0.3103 0.5758 0.028 Uiso 1 1 calc R . . B1 B 0.7211(3) 0.22746(17) 0.64888(18) 0.0195(6) Uani 1 1 d . . . Si2 Si 0.40278(8) 0.44378(4) 0.70742(5) 0.02416(17) Uani 1 1 d . . . O2 O 0.7215(2) 0.36902(11) 0.87141(11) 0.0257(4) Uani 1 1 d . . . C2 C 0.7312(3) 0.45892(17) 0.6182(2) 0.0334(7) Uani 1 1 d . . . H2A H 0.8010 0.4520 0.6621 0.050 Uiso 1 1 calc R . . H2B H 0.6898 0.5050 0.6201 0.050 Uiso 1 1 calc R . . H2C H 0.7716 0.4562 0.5749 0.050 Uiso 1 1 calc R . . C3 C 0.4652(3) 0.40685(17) 0.52533(17) 0.0302(7) Uani 1 1 d . . . H3A H 0.4215 0.4518 0.5305 0.045 Uiso 1 1 calc R . . H3B H 0.3974 0.3697 0.5172 0.045 Uiso 1 1 calc R . . H3C H 0.5103 0.4091 0.4838 0.045 Uiso 1 1 calc R . . C4 C 0.4482(4) 0.54047(18) 0.6984(2) 0.0477(10) Uani 1 1 d . . . H4A H 0.4616 0.5494 0.6488 0.072 Uiso 1 1 calc R . . H4B H 0.5311 0.5513 0.7335 0.072 Uiso 1 1 calc R . . H4C H 0.3750 0.5700 0.7083 0.072 Uiso 1 1 calc R . . C5 C 0.2286(3) 0.4296(2) 0.6472(2) 0.0504(10) Uani 1 1 d . . . H5A H 0.2338 0.4361 0.5959 0.076 Uiso 1 1 calc R . . H5B H 0.1651 0.4634 0.6605 0.076 Uiso 1 1 calc R . . H5C H 0.1978 0.3820 0.6543 0.076 Uiso 1 1 calc R . . C6 C 0.3780(3) 0.43012(18) 0.80559(17) 0.0334(7) Uani 1 1 d . . . H6A H 0.3543 0.3812 0.8122 0.050 Uiso 1 1 calc R . . H6B H 0.3056 0.4606 0.8147 0.050 Uiso 1 1 calc R . . H6C H 0.4616 0.4416 0.8399 0.050 Uiso 1 1 calc R . . C7 C 0.5952(3) 0.17081(19) 0.9040(2) 0.0387(8) Uani 1 1 d . . . H7A H 0.6855 0.1864 0.9296 0.046 Uiso 1 1 calc R . . H7B H 0.6058 0.1300 0.8730 0.046 Uiso 1 1 calc R . . C9 C 0.3661(5) 0.1687(3) 0.9175(3) 0.0673(14) Uani 1 1 d . . . H9A H 0.3286 0.1294 0.8853 0.081 Uiso 1 1 calc R . . H9B H 0.3055 0.1786 0.9517 0.081 Uiso 1 1 calc R . . C10 C 0.3840(3) 0.23303(19) 0.8733(2) 0.0374(8) Uani 1 1 d . . . H10A H 0.3171 0.2335 0.8268 0.045 Uiso 1 1 calc R . . H10B H 0.3730 0.2761 0.9008 0.045 Uiso 1 1 calc R . . C11 C 0.7986(3) 0.17236(14) 0.60115(15) 0.0186(5) Uani 1 1 d . . . C12 C 0.7239(3) 0.14362(15) 0.53444(15) 0.0213(5) Uani 1 1 d . . . H12 H 0.6303 0.1531 0.5213 0.026 Uiso 1 1 calc R . . C13 C 0.7841(3) 0.10150(15) 0.48708(16) 0.0233(6) Uani 1 1 d . . . H13 H 0.7312 0.0839 0.4431 0.028 Uiso 1 1 calc R . . C14 C 0.9237(3) 0.08581(16) 0.50598(16) 0.0255(6) Uani 1 1 d . . . H14 H 0.9653 0.0584 0.4745 0.031 Uiso 1 1 calc R . . C15 C 0.9992(3) 0.11164(17) 0.57215(17) 0.0288(6) Uani 1 1 d . . . H15 H 1.0921 0.1007 0.5859 0.035 Uiso 1 1 calc R . . C16 C 0.9373(3) 0.15417(16) 0.61874(17) 0.0262(6) Uani 1 1 d . . . H16 H 0.9905 0.1709 0.6630 0.031 Uiso 1 1 calc R . . C17 C 0.7626(3) 0.34971(15) 0.94977(16) 0.0260(6) Uani 1 1 d . . . H17A H 0.8292 0.3112 0.9562 0.031 Uiso 1 1 calc R . . H17B H 0.6837 0.3346 0.9695 0.031 Uiso 1 1 calc R . . C18 C 0.8255(3) 0.41709(16) 0.98871(16) 0.0259(6) Uani 1 1 d . . . H18A H 0.8980 0.4057 1.0310 0.031 Uiso 1 1 calc R . . H18B H 0.7566 0.4461 1.0054 0.031 Uiso 1 1 calc R . . C19 C 0.7721(3) 0.44084(16) 0.86027(18) 0.0278(6) Uani 1 1 d . . . H19A H 0.6989 0.4757 0.8566 0.033 Uiso 1 1 calc R . . H19B H 0.8091 0.4428 0.8152 0.033 Uiso 1 1 calc R . . C20 C 0.8825(3) 0.45479(16) 0.92770(16) 0.0257(6) Uani 1 1 d . . . H20A H 0.8942 0.5055 0.9376 0.031 Uiso 1 1 calc R . . H20B H 0.9695 0.4343 0.9222 0.031 Uiso 1 1 calc R . . C21 C 0.8344(3) 0.24882(14) 0.72553(15) 0.0201(5) Uani 1 1 d . . . C22 C 0.8607(3) 0.20874(14) 0.79141(18) 0.0234(6) Uani 1 1 d . . . H22 H 0.8077 0.1683 0.7945 0.028 Uiso 1 1 calc R . . C23 C 0.9626(3) 0.22683(17) 0.85241(18) 0.0278(6) Uani 1 1 d . . . H23 H 0.9760 0.1987 0.8951 0.033 Uiso 1 1 calc R . . C24 C 1.0429(3) 0.28544(19) 0.8501(2) 0.0337(8) Uani 1 1 d . . . H24 H 1.1119 0.2969 0.8907 0.040 Uiso 1 1 calc R . . C25 C 1.0209(3) 0.32799(18) 0.78638(19) 0.0322(7) Uani 1 1 d . . . H25 H 1.0747 0.3683 0.7846 0.039 Uiso 1 1 calc R . . C26 C 0.9183(3) 0.31023(17) 0.72535(19) 0.0264(6) Uani 1 1 d . . . H26 H 0.9043 0.3393 0.6834 0.032 Uiso 1 1 calc R . . C31 C 0.5873(3) 0.18372(16) 0.66833(16) 0.0207(5) Uani 1 1 d . . . C32 C 0.4519(3) 0.21218(16) 0.65387(18) 0.0245(6) Uani 1 1 d . . . H32 H 0.4370 0.2571 0.6320 0.029 Uiso 1 1 calc R . . C33 C 0.3410(3) 0.17530(19) 0.67119(19) 0.0335(7) Uani 1 1 d . . . H33 H 0.2544 0.1962 0.6620 0.040 Uiso 1 1 calc R . . C34 C 0.3586(3) 0.10809(19) 0.70186(19) 0.0351(7) Uani 1 1 d . . . H34 H 0.2845 0.0838 0.7141 0.042 Uiso 1 1 calc R . . C35 C 0.4882(3) 0.07663(17) 0.71447(19) 0.0335(7) Uani 1 1 d . . . H35 H 0.5007 0.0308 0.7342 0.040 Uiso 1 1 calc R . . C36 C 0.5983(2) 0.11390(14) 0.69755(14) 0.0247(6) Uani 1 1 d . . . H36 H 0.6838 0.0917 0.7059 0.030 Uiso 1 1 calc R . . C8 C 0.5072(2) 0.15202(14) 0.95874(14) 0.090(2) Uani 1 1 d R . . H8A H 0.5161 0.1019 0.9721 0.108 Uiso 1 1 calc R . . H8B H 0.5312 0.1807 1.0036 0.108 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 Yb1 0.01474(7) 0.02063(9) 0.01866(10) -0.00061(4) 0.00322(5) 0.00070(4) Si1 0.0214(3) 0.0213(4) 0.0206(4) 0.0013(3) 0.0039(3) 0.0007(3) O1 0.0223(10) 0.0328(11) 0.0310(12) 0.0044(10) 0.0087(9) 0.0014(8) N1 0.0222(11) 0.0225(11) 0.0197(12) 0.0011(10) 0.0021(9) 0.0013(9) C1 0.0208(13) 0.0238(15) 0.0238(17) -0.0002(11) 0.0036(12) 0.0011(9) B1 0.0146(12) 0.0223(14) 0.0221(16) -0.0005(13) 0.0053(11) 0.0002(11) Si2 0.0242(4) 0.0251(4) 0.0238(4) 0.0025(3) 0.0065(3) 0.0038(3) O2 0.0275(10) 0.0251(10) 0.0228(11) -0.0009(9) 0.0010(8) -0.0058(8) C2 0.0312(15) 0.0293(15) 0.0402(19) 0.0018(15) 0.0084(14) -0.0024(12) C3 0.0350(16) 0.0307(16) 0.0239(16) 0.0034(13) 0.0038(12) 0.0057(12) C4 0.068(2) 0.0263(16) 0.061(3) 0.0023(17) 0.042(2) 0.0086(16) C5 0.0274(16) 0.084(3) 0.038(2) 0.002(2) 0.0020(14) 0.0149(18) C6 0.0280(15) 0.0438(18) 0.0306(17) 0.0030(15) 0.0109(13) 0.0017(13) C7 0.0307(16) 0.0411(19) 0.043(2) 0.0150(17) 0.0045(14) 0.0032(14) C9 0.053(2) 0.078(3) 0.083(3) 0.029(3) 0.040(2) 0.003(2) C10 0.0303(16) 0.0439(19) 0.043(2) 0.0035(17) 0.0200(15) 0.0058(14) C11 0.0152(11) 0.0204(13) 0.0210(14) 0.0016(11) 0.0053(10) -0.0019(9) C12 0.0153(11) 0.0262(13) 0.0223(14) 0.0004(12) 0.0033(10) -0.0003(10) C13 0.0237(13) 0.0262(14) 0.0203(14) -0.0011(12) 0.0049(10) -0.0007(11) C14 0.0250(13) 0.0296(14) 0.0242(15) -0.0004(13) 0.0106(11) 0.0076(11) C15 0.0175(12) 0.0401(16) 0.0294(16) -0.0008(14) 0.0063(11) 0.0085(12) C16 0.0168(12) 0.0366(16) 0.0248(15) -0.0064(13) 0.0035(11) 0.0016(11) C17 0.0257(13) 0.0271(14) 0.0248(15) -0.0008(13) 0.0042(11) -0.0008(11) C18 0.0252(13) 0.0299(14) 0.0223(15) -0.0039(13) 0.0040(11) -0.0034(11) C19 0.0273(14) 0.0263(14) 0.0274(16) 0.0031(13) -0.0005(12) -0.0069(11) C20 0.0203(13) 0.0286(14) 0.0274(15) -0.0018(13) 0.0027(11) -0.0041(11) C21 0.0137(11) 0.0234(13) 0.0243(14) -0.0048(12) 0.0062(10) -0.0010(10) C22 0.0182(13) 0.0260(14) 0.0259(17) -0.0016(11) 0.0044(11) 0.0029(10) C23 0.0208(13) 0.0357(16) 0.0250(16) -0.0018(14) -0.0002(11) 0.0083(12) C24 0.0145(13) 0.0523(19) 0.0323(19) -0.0125(16) 0.0004(12) 0.0007(12) C25 0.0209(13) 0.0354(17) 0.0396(19) -0.0080(15) 0.0043(12) -0.0078(12) C26 0.0176(12) 0.0318(15) 0.0298(18) 0.0010(13) 0.0049(11) -0.0035(11) C31 0.0150(12) 0.0279(13) 0.0195(14) -0.0074(12) 0.0041(10) -0.0018(10) C32 0.0163(13) 0.0281(14) 0.0287(17) -0.0093(12) 0.0038(12) -0.0011(10) C33 0.0152(12) 0.0432(18) 0.042(2) -0.0191(16) 0.0062(12) -0.0056(12) C34 0.0238(14) 0.0480(19) 0.0363(18) -0.0117(16) 0.0129(13) -0.0157(13) C35 0.0349(16) 0.0314(16) 0.0368(18) -0.0013(15) 0.0132(14) -0.0102(13) C36 0.0198(12) 0.0278(14) 0.0261(15) -0.0031(12) 0.0041(11) -0.0025(11) C8 0.061(3) 0.122(5) 0.091(4) 0.075(4) 0.029(3) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N1 2.285(2) . ? Yb1 O2 2.378(2) . ? Yb1 O1 2.410(2) . ? Yb1 C21 2.635(3) . ? Yb1 C31 2.792(3) . ? Yb1 C32 2.869(3) . ? Yb1 C22 2.914(3) . ? Si1 N1 1.705(3) . ? Si1 C3 1.886(3) . ? Si1 C2 1.889(3) . ? Si1 C1 1.896(3) . ? O1 C7 1.454(4) . ? O1 C10 1.460(3) . ? N1 Si2 1.687(2) . ? C1 B1 1.659(4) . ? B1 C11 1.641(4) . ? B1 C31 1.661(4) . ? B1 C21 1.663(4) . ? Si2 C5 1.876(4) . ? Si2 C4 1.881(4) . ? Si2 C6 1.883(3) . ? O2 C17 1.458(4) . ? O2 C19 1.465(3) . ? C7 C8 1.501(4) . ? C9 C10 1.483(6) . ? C9 C8 1.486(5) . ? C11 C16 1.394(4) . ? C11 C12 1.404(4) . ? C12 C13 1.394(4) . ? C13 C14 1.393(4) . ? C14 C15 1.379(4) . ? C15 C16 1.398(4) . ? C17 C18 1.521(4) . ? C18 C20 1.525(4) . ? C19 C20 1.501(4) . ? C21 C22 1.401(4) . ? C21 C26 1.421(4) . ? C22 C23 1.391(4) . ? C23 C24 1.363(5) . ? C24 C25 1.394(5) . ? C25 C26 1.394(4) . ? C31 C36 1.409(4) . ? C31 C32 1.422(4) . ? C32 C33 1.391(4) . ? C33 C34 1.375(5) . ? C34 C35 1.393(5) . ? C35 C36 1.385(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Yb1 O2 97.69(8) . . ? N1 Yb1 O1 132.56(8) . . ? O2 Yb1 O1 86.13(7) . . ? N1 Yb1 C21 107.60(9) . . ? O2 Yb1 C21 99.61(8) . . ? O1 Yb1 C21 118.37(8) . . ? N1 Yb1 C31 99.87(9) . . ? O2 Yb1 C31 157.03(7) . . ? O1 Yb1 C31 92.75(8) . . ? C21 Yb1 C31 60.91(8) . . ? N1 Yb1 C32 81.71(9) . . ? O2 Yb1 C32 172.15(8) . . ? O1 Yb1 C32 88.55(9) . . ? C21 Yb1 C32 88.00(8) . . ? C31 Yb1 C32 29.06(8) . . ? N1 Yb1 C22 135.82(9) . . ? O2 Yb1 C22 88.94(8) . . ? O1 Yb1 C22 91.31(8) . . ? C21 Yb1 C22 28.69(9) . . ? C31 Yb1 C22 68.13(8) . . ? C32 Yb1 C22 96.96(9) . . ? N1 Si1 C3 112.41(13) . . ? N1 Si1 C2 111.42(14) . . ? C3 Si1 C2 105.45(15) . . ? N1 Si1 C1 113.07(13) . . ? C3 Si1 C1 104.78(14) . . ? C2 Si1 C1 109.22(14) . . ? C7 O1 C10 108.7(2) . . ? C7 O1 Yb1 124.87(18) . . ? C10 O1 Yb1 126.22(18) . . ? Si2 N1 Si1 126.04(15) . . ? Si2 N1 Yb1 123.28(13) . . ? Si1 N1 Yb1 110.65(11) . . ? B1 C1 Si1 132.8(2) . . ? C11 B1 C1 107.2(2) . . ? C11 B1 C31 106.7(2) . . ? C1 B1 C31 111.6(2) . . ? C11 B1 C21 106.9(2) . . ? C1 B1 C21 112.2(2) . . ? C31 B1 C21 111.9(2) . . ? N1 Si2 C5 114.70(16) . . ? N1 Si2 C4 112.96(15) . . ? C5 Si2 C4 107.1(2) . . ? N1 Si2 C6 109.30(14) . . ? C5 Si2 C6 105.10(16) . . ? C4 Si2 C6 107.15(17) . . ? C17 O2 C19 109.2(2) . . ? C17 O2 Yb1 128.94(16) . . ? C19 O2 Yb1 121.43(16) . . ? O1 C7 C8 105.3(2) . . ? C10 C9 C8 104.1(3) . . ? O1 C10 C9 105.7(3) . . ? C16 C11 C12 115.6(2) . . ? C16 C11 B1 125.4(2) . . ? C12 C11 B1 118.9(2) . . ? C13 C12 C11 122.8(2) . . ? C14 C13 C12 119.7(3) . . ? C15 C14 C13 118.9(3) . . ? C14 C15 C16 120.6(3) . . ? C11 C16 C15 122.3(3) . . ? O2 C17 C18 105.3(2) . . ? C17 C18 C20 102.6(2) . . ? O2 C19 C20 105.0(2) . . ? C19 C20 C18 101.9(2) . . ? C22 C21 C26 115.3(3) . . ? C22 C21 B1 125.2(2) . . ? C26 C21 B1 119.4(3) . . ? C22 C21 Yb1 86.77(17) . . ? C26 C21 Yb1 104.26(19) . . ? B1 C21 Yb1 82.93(14) . . ? C23 C22 C21 122.8(3) . . ? C23 C22 Yb1 115.43(19) . . ? C21 C22 Yb1 64.53(14) . . ? C24 C23 C22 120.5(3) . . ? C23 C24 C25 119.5(3) . . ? C26 C25 C24 120.1(3) . . ? C25 C26 C21 121.7(3) . . ? C36 C31 C32 114.7(2) . . ? C36 C31 B1 122.3(2) . . ? C32 C31 B1 123.0(3) . . ? C36 C31 Yb1 117.66(19) . . ? C32 C31 Yb1 78.47(17) . . ? B1 C31 Yb1 78.02(15) . . ? C33 C32 C31 122.4(3) . . ? C33 C32 Yb1 117.5(2) . . ? C31 C32 Yb1 72.47(16) . . ? C34 C33 C32 120.4(3) . . ? C33 C34 C35 119.5(3) . . ? C36 C35 C34 119.8(3) . . ? C35 C36 C31 123.2(3) . . ? C9 C8 C7 103.2(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.201 _refine_diff_density_min -3.071 _refine_diff_density_rms 0.151