# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Helmut Sitzmann' _publ_contact_author_address ; FB Chemie TU Kaiserslautern Erwin-Schroedinger-Str. 54 Kaiserslautern D-67663 GERMANY ; _publ_contact_author_email SITZMANN@CHEMIE.UNI-KL.DE _publ_section_title ; Cation size dependent reactivity of lanthanide trihalides with bulky alkylcyclopentadienyl anions ; loop_ _publ_author_name 'Helmut Sitzmann' 'Dirk Bentz' 'Oliver Schmitt' 'Marc D. Walter' 'Frank Weber' ; G.Wolmershauser ; data_0179 _database_code_depnum_ccdc_archive 'CCDC 604031' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H45 Ce0.50 Cl N2 Na0.50' _chemical_formula_weight 466.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 18.7950(9) _cell_length_b 18.7950(9) _cell_length_c 29.9286(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10572.3(10) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 26 _exptl_crystal_description 'irregular shaped transparent block' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3976 _exptl_absorpt_coefficient_mu 1.002 _exptl_absorpt_correction_type 'empirical (MULABS/PLATON 98)' _exptl_absorpt_correction_T_min 0.57291 _exptl_absorpt_correction_T_max 0.69259 _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 'Stoe IPDS' _diffrn_measurement_method Phi-Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70557 _diffrn_reflns_av_R_equivalents 0.1095 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.68 _reflns_number_total 5027 _reflns_number_gt 3416 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS V2.63' _computing_cell_refinement 'Stoe IPDS V2.63' _computing_data_reduction 'Stoe IPDS V2.63' _computing_structure_solution 'SIR97 (Giacovazzo et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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 w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5027 _refine_ls_number_parameters 282 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.917 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.5000 0.2500 0.645670(8) 0.04411(9) Uani 1 d S . . Cl1 Cl 0.50800(5) 0.14360(5) 0.58173(3) 0.0642(2) Uani 1 d . . . C1 C 0.6193(2) 0.2206(2) 0.70409(12) 0.0631(10) Uani 1 d . . . C2 C 0.6498(2) 0.2142(2) 0.66078(13) 0.0587(9) Uani 1 d . . . C3 C 0.64812(18) 0.28309(18) 0.64054(11) 0.0509(8) Uani 1 d . . . C4 C 0.6168(2) 0.33143(19) 0.67160(11) 0.0550(8) Uani 1 d . . . C5 C 0.5992(2) 0.2918(2) 0.70979(12) 0.0610(9) Uani 1 d . . . H5 H 0.5774 0.3101 0.7352 0.073 Uiso 1 calc R . . C11 C 0.6215(3) 0.1669(3) 0.74234(16) 0.0912(15) Uani 1 d D . . H11 H 0.6244 0.1180 0.7311 0.109 Uiso 1 calc R A 1 C12 C 0.6870(11) 0.186(2) 0.7711(10) 0.279(18) Uani 0.62(3) d PD B 1 H12A H 0.6794 0.2309 0.7855 0.418 Uiso 0.62(3) calc PR B 1 H12B H 0.7284 0.1887 0.7524 0.418 Uiso 0.62(3) calc PR B 1 H12C H 0.6940 0.1498 0.7934 0.418 Uiso 0.62(3) calc PR B 1 C13 C 0.5618(10) 0.1753(14) 0.7737(6) 0.213(13) Uani 0.62(3) d PD B 1 H13A H 0.5703 0.1470 0.7999 0.319 Uiso 0.62(3) calc PR B 1 H13B H 0.5185 0.1600 0.7597 0.319 Uiso 0.62(3) calc PR B 1 H13C H 0.5576 0.2245 0.7821 0.319 Uiso 0.62(3) calc PR B 1 C12A C 0.6925(7) 0.1447(9) 0.7576(6) 0.076(6) Uani 0.38(3) d PD B 2 H12D H 0.7166 0.1846 0.7706 0.115 Uiso 0.38(3) calc PR B 2 H12E H 0.7194 0.1273 0.7326 0.115 Uiso 0.38(3) calc PR B 2 H12F H 0.6877 0.1076 0.7794 0.115 Uiso 0.38(3) calc PR B 2 C13A C 0.5758(9) 0.1771(13) 0.7818(5) 0.087(6) Uani 0.38(3) d PD B 2 H13D H 0.5744 0.1339 0.7989 0.131 Uiso 0.38(3) calc PR B 2 H13E H 0.5285 0.1892 0.7723 0.131 Uiso 0.38(3) calc PR B 2 H13F H 0.5946 0.2148 0.7999 0.131 Uiso 0.38(3) calc PR B 2 C21 C 0.6866(3) 0.1505(2) 0.63987(17) 0.0874(14) Uani 1 d . . . H21 H 0.6832 0.1575 0.6075 0.105 Uiso 1 calc R . . C22 C 0.7655(3) 0.1486(4) 0.6503(4) 0.187(4) Uani 1 d . . . H22A H 0.7729 0.1251 0.6784 0.281 Uiso 1 calc R . . H22B H 0.7835 0.1963 0.6519 0.281 Uiso 1 calc R . . H22C H 0.7900 0.1231 0.6271 0.281 Uiso 1 calc R . . C23 C 0.6550(3) 0.0779(2) 0.64895(17) 0.0927(15) Uani 1 d . . . H23A H 0.6795 0.0428 0.6315 0.139 Uiso 1 calc R . . H23B H 0.6055 0.0781 0.6410 0.139 Uiso 1 calc R . . H23C H 0.6599 0.0668 0.6801 0.139 Uiso 1 calc R . . C31 C 0.6791(2) 0.3079(2) 0.59627(12) 0.0616(9) Uani 1 d . . . H31 H 0.6569 0.3542 0.5906 0.074 Uiso 1 calc R . . C32 C 0.7590(3) 0.3229(4) 0.59871(19) 0.118(2) Uani 1 d . . . H32A H 0.7843 0.2789 0.6020 0.176 Uiso 1 calc R . . H32B H 0.7687 0.3531 0.6239 0.176 Uiso 1 calc R . . H32C H 0.7740 0.3462 0.5718 0.176 Uiso 1 calc R . . C33 C 0.6637(2) 0.2639(2) 0.55479(13) 0.0747(11) Uani 1 d . . . H33A H 0.6904 0.2204 0.5560 0.112 Uiso 1 calc R . . H33B H 0.6773 0.2903 0.5287 0.112 Uiso 1 calc R . . H33C H 0.6138 0.2532 0.5534 0.112 Uiso 1 calc R . . C41 C 0.6097(2) 0.4111(2) 0.66713(14) 0.0681(11) Uani 1 d . . . H41 H 0.6001 0.4210 0.6356 0.082 Uiso 1 calc R . . C42 C 0.6775(3) 0.4501(3) 0.6789(3) 0.136(3) Uani 1 d . . . H42A H 0.6714 0.5000 0.6733 0.204 Uiso 1 calc R . . H42B H 0.7159 0.4322 0.6611 0.204 Uiso 1 calc R . . H42C H 0.6881 0.4429 0.7100 0.204 Uiso 1 calc R . . C43 C 0.5487(3) 0.4418(3) 0.69343(17) 0.0995(16) Uani 1 d . . . H43A H 0.5556 0.4322 0.7246 0.149 Uiso 1 calc R . . H43B H 0.5050 0.4205 0.6837 0.149 Uiso 1 calc R . . H43C H 0.5467 0.4923 0.6888 0.149 Uiso 1 calc R . . Na1 Na 0.49967(16) 0.02437(16) 0.51459(10) 0.0635(7) Uani 0.50 d P . . N1 N 0.62505(18) 0.0367(2) 0.48224(12) 0.0747(9) Uani 1 d . . . N2 N 0.4876(2) 0.0944(2) 0.44461(13) 0.0840(11) Uani 1 d . . . C50 C 0.6627(3) 0.0616(3) 0.5216(2) 0.122(2) Uani 1 d . . . H50A H 0.7075 0.0818 0.5129 0.183 Uiso 1 calc R . . H50B H 0.6708 0.0224 0.5415 0.183 Uiso 1 calc R . . H50C H 0.6347 0.0971 0.5365 0.183 Uiso 1 calc R . . C51 C 0.6686(3) -0.0205(3) 0.4642(2) 0.123(2) Uani 1 d . . . H51A H 0.6485 -0.0367 0.4365 0.185 Uiso 1 calc R . . H51B H 0.6700 -0.0593 0.4851 0.185 Uiso 1 calc R . . H51C H 0.7160 -0.0034 0.4590 0.185 Uiso 1 calc R . . C52 C 0.6174(4) 0.0917(4) 0.4501(3) 0.160(3) Uani 1 d . . . H52A H 0.6513 0.1284 0.4582 0.192 Uiso 1 calc R . . H52B H 0.6336 0.0721 0.4219 0.192 Uiso 1 calc R . . C53 C 0.5580(4) 0.1240(5) 0.4417(4) 0.197(5) Uani 1 d . . . H53A H 0.5624 0.1419 0.4115 0.237 Uiso 1 calc R . . H53B H 0.5576 0.1655 0.4610 0.237 Uiso 1 calc R . . C54 C 0.4603(6) 0.0658(4) 0.4038(2) 0.180(4) Uani 1 d . . . H54A H 0.4581 0.1027 0.3817 0.269 Uiso 1 calc R . . H54B H 0.4134 0.0471 0.4089 0.269 Uiso 1 calc R . . H54C H 0.4910 0.0284 0.3935 0.269 Uiso 1 calc R . . C55 C 0.4401(4) 0.1509(4) 0.4581(2) 0.128(2) Uani 1 d . . . H55A H 0.4407 0.1880 0.4360 0.192 Uiso 1 calc R . . H55B H 0.4553 0.1699 0.4863 0.192 Uiso 1 calc R . . H55C H 0.3927 0.1325 0.4609 0.192 Uiso 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 Ce1 0.04908(18) 0.04264(17) 0.04061(12) 0.000 0.000 -0.00253(15) Cl1 0.0625(6) 0.0683(6) 0.0619(5) -0.0125(4) 0.0062(4) 0.0007(5) C1 0.066(2) 0.064(2) 0.059(2) 0.0111(18) -0.0123(18) -0.0015(19) C2 0.061(2) 0.052(2) 0.063(2) 0.0100(16) -0.0108(17) 0.0043(18) C3 0.0492(18) 0.0462(18) 0.0575(19) 0.0057(15) -0.0090(15) -0.0032(15) C4 0.062(2) 0.0469(19) 0.056(2) 0.0006(15) -0.0127(16) -0.0065(17) C5 0.067(2) 0.068(2) 0.0472(19) 0.0005(17) -0.0092(17) -0.004(2) C11 0.109(4) 0.087(3) 0.077(3) 0.036(3) -0.012(3) 0.003(3) C12 0.211(18) 0.36(4) 0.26(2) 0.24(3) -0.181(18) -0.133(19) C13 0.135(12) 0.39(3) 0.117(12) 0.180(17) -0.035(10) -0.040(16) C12A 0.081(10) 0.076(10) 0.073(8) 0.015(7) -0.021(7) 0.014(7) C13A 0.099(11) 0.132(14) 0.031(6) 0.006(9) -0.024(7) 0.026(10) C21 0.094(3) 0.061(3) 0.107(4) 0.019(2) 0.011(3) 0.029(2) C22 0.076(4) 0.103(5) 0.382(14) 0.014(6) 0.018(6) 0.032(4) C23 0.119(4) 0.058(3) 0.102(3) 0.005(2) -0.013(3) 0.023(3) C31 0.061(2) 0.057(2) 0.067(2) 0.0096(18) 0.0002(18) -0.0001(18) C32 0.073(3) 0.169(6) 0.111(4) 0.014(4) 0.006(3) -0.046(4) C33 0.079(3) 0.079(3) 0.066(2) 0.006(2) 0.009(2) 0.002(2) C41 0.085(3) 0.049(2) 0.070(2) -0.0055(18) -0.014(2) -0.011(2) C42 0.115(5) 0.068(3) 0.226(8) -0.018(4) -0.041(5) -0.028(3) C43 0.129(5) 0.070(3) 0.099(4) -0.015(3) 0.000(3) 0.017(3) Na1 0.0574(16) 0.068(2) 0.0652(19) 0.0237(13) -0.0008(14) -0.0009(15) N1 0.063(2) 0.081(2) 0.080(2) 0.0009(19) 0.0018(17) -0.0071(18) N2 0.085(3) 0.085(3) 0.082(3) 0.030(2) -0.003(2) 0.010(2) C50 0.106(4) 0.135(5) 0.126(5) -0.052(4) -0.018(4) 0.033(4) C51 0.130(5) 0.113(5) 0.128(5) -0.052(4) 0.012(4) -0.009(4) C52 0.092(5) 0.174(7) 0.215(8) 0.112(7) -0.003(5) -0.024(5) C53 0.099(5) 0.175(8) 0.318(12) 0.167(8) 0.063(6) 0.015(5) C54 0.334(13) 0.102(5) 0.103(5) 0.002(4) -0.053(7) 0.038(6) C55 0.127(5) 0.139(6) 0.117(5) 0.009(4) -0.007(4) 0.030(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 Cl1 2.7719(9) . ? Ce1 Cl1 2.7720(9) 6_554 ? Ce1 C4 2.786(3) 6_554 ? Ce1 C4 2.786(3) . ? Ce1 C5 2.789(4) . ? Ce1 C5 2.789(4) 6_554 ? Ce1 C3 2.857(3) 6_554 ? Ce1 C3 2.857(3) . ? Ce1 C1 2.897(4) . ? Ce1 C1 2.897(4) 6_554 ? Ce1 C2 2.930(4) . ? Ce1 C2 2.930(4) 6_554 ? Cl1 Na1 3.014(3) . ? C1 C5 1.400(5) . ? C1 C2 1.422(5) . ? C1 C11 1.527(5) . ? C2 C3 1.430(5) . ? C2 C21 1.517(6) . ? C3 C4 1.427(5) . ? C3 C31 1.520(5) . ? C4 C5 1.404(5) . ? C4 C41 1.509(5) . ? C11 C13A 1.473(11) . ? C11 C12A 1.471(12) . ? C11 C13 1.472(12) . ? C11 C12 1.546(14) . ? C21 C23 1.513(7) . ? C21 C22 1.514(8) . ? C31 C33 1.519(6) . ? C31 C32 1.530(6) . ? C41 C43 1.506(6) . ? C41 C42 1.511(6) . ? Na1 Na1 1.266(6) 9_656 ? Na1 N2 2.484(4) . ? Na1 N2 2.556(5) 9_656 ? Na1 N1 2.558(5) . ? Na1 N1 2.612(5) 9_656 ? N1 C52 1.420(7) . ? N1 C50 1.453(6) . ? N1 C51 1.456(6) . ? N1 Na1 2.612(5) 9_656 ? N2 C54 1.430(8) . ? N2 C53 1.437(8) . ? N2 C55 1.445(7) . ? N2 Na1 2.556(5) 9_656 ? C52 C53 1.295(8) . ? 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 Cl1 Ce1 Cl1 92.68(4) . 6_554 ? Cl1 Ce1 C4 80.72(7) . 6_554 ? Cl1 Ce1 C4 123.08(8) 6_554 6_554 ? Cl1 Ce1 C4 123.08(8) . . ? Cl1 Ce1 C4 80.72(7) 6_554 . ? C4 Ce1 C4 147.66(14) 6_554 . ? Cl1 Ce1 C5 129.93(9) . . ? Cl1 Ce1 C5 107.96(8) 6_554 . ? C4 Ce1 C5 119.33(11) 6_554 . ? C4 Ce1 C5 29.17(10) . . ? Cl1 Ce1 C5 107.95(8) . 6_554 ? Cl1 Ce1 C5 129.93(9) 6_554 6_554 ? C4 Ce1 C5 29.17(10) 6_554 6_554 ? C4 Ce1 C5 119.33(11) . 6_554 ? C5 Ce1 C5 93.04(16) . 6_554 ? Cl1 Ce1 C3 81.88(7) . 6_554 ? Cl1 Ce1 C3 93.85(7) 6_554 6_554 ? C4 Ce1 C3 29.26(10) 6_554 6_554 ? C4 Ce1 C3 154.46(10) . 6_554 ? C5 Ce1 C3 138.59(11) . 6_554 ? C5 Ce1 C3 47.46(11) 6_554 6_554 ? Cl1 Ce1 C3 93.85(7) . . ? Cl1 Ce1 C3 81.88(7) 6_554 . ? C4 Ce1 C3 154.46(10) 6_554 . ? C4 Ce1 C3 29.27(10) . . ? C5 Ce1 C3 47.47(11) . . ? C5 Ce1 C3 138.59(11) 6_554 . ? C3 Ce1 C3 173.84(13) 6_554 . ? Cl1 Ce1 C1 103.72(8) . . ? Cl1 Ce1 C1 126.60(8) 6_554 . ? C4 Ce1 C1 109.70(11) 6_554 . ? C4 Ce1 C1 47.67(11) . . ? C5 Ce1 C1 28.42(11) . . ? C5 Ce1 C1 92.80(11) 6_554 . ? C3 Ce1 C1 138.20(11) 6_554 . ? C3 Ce1 C1 47.11(10) . . ? Cl1 Ce1 C1 126.59(8) . 6_554 ? Cl1 Ce1 C1 103.72(8) 6_554 6_554 ? C4 Ce1 C1 47.67(11) 6_554 6_554 ? C4 Ce1 C1 109.70(11) . 6_554 ? C5 Ce1 C1 92.80(11) . 6_554 ? C5 Ce1 C1 28.42(11) 6_554 6_554 ? C3 Ce1 C1 47.11(10) 6_554 6_554 ? C3 Ce1 C1 138.20(11) . 6_554 ? C1 Ce1 C1 105.75(16) . 6_554 ? Cl1 Ce1 C2 83.61(8) . . ? Cl1 Ce1 C2 108.93(7) 6_554 . ? C4 Ce1 C2 126.01(11) 6_554 . ? C4 Ce1 C2 47.64(11) . . ? C5 Ce1 C2 46.83(11) . . ? C5 Ce1 C2 118.15(11) 6_554 . ? C3 Ce1 C2 153.48(10) 6_554 . ? C3 Ce1 C2 28.58(10) . . ? C1 Ce1 C2 28.25(11) . . ? C1 Ce1 C2 133.99(12) 6_554 . ? Cl1 Ce1 C2 108.93(8) . 6_554 ? Cl1 Ce1 C2 83.61(8) 6_554 6_554 ? C4 Ce1 C2 47.63(11) 6_554 6_554 ? C4 Ce1 C2 126.01(11) . 6_554 ? C5 Ce1 C2 118.15(11) . 6_554 ? C5 Ce1 C2 46.82(11) 6_554 6_554 ? C3 Ce1 C2 28.58(10) 6_554 6_554 ? C3 Ce1 C2 153.48(10) . 6_554 ? C1 Ce1 C2 133.99(12) . 6_554 ? C1 Ce1 C2 28.25(11) 6_554 6_554 ? C2 Ce1 C2 162.24(15) . 6_554 ? Ce1 Cl1 Na1 173.63(7) . . ? C5 C1 C2 107.5(3) . . ? C5 C1 C11 123.2(4) . . ? C2 C1 C11 128.0(4) . . ? C5 C1 Ce1 71.5(2) . . ? C2 C1 Ce1 77.2(2) . . ? C11 C1 Ce1 126.8(3) . . ? C1 C2 C3 107.5(3) . . ? C1 C2 C21 128.8(3) . . ? C3 C2 C21 123.3(3) . . ? C1 C2 Ce1 74.6(2) . . ? C3 C2 Ce1 72.9(2) . . ? C21 C2 Ce1 123.8(3) . . ? C4 C3 C2 108.0(3) . . ? C4 C3 C31 122.0(3) . . ? C2 C3 C31 129.7(3) . . ? C4 C3 Ce1 72.6(2) . . ? C2 C3 Ce1 78.6(2) . . ? C31 C3 Ce1 119.1(2) . . ? C5 C4 C3 106.8(3) . . ? C5 C4 C41 125.3(3) . . ? C3 C4 C41 127.6(3) . . ? C5 C4 Ce1 75.5(2) . . ? C3 C4 Ce1 78.11(19) . . ? C41 C4 Ce1 116.8(2) . . ? C1 C5 C4 110.2(3) . . ? C1 C5 Ce1 80.1(2) . . ? C4 C5 Ce1 75.3(2) . . ? C13A C11 C12A 108.5(9) . . ? C13A C11 C13 14.0(13) . . ? C12A C11 C13 121.6(12) . . ? C13A C11 C1 120.0(10) . . ? C12A C11 C1 116.4(8) . . ? C13 C11 C1 112.8(9) . . ? C13A C11 C12 89.3(17) . . ? C12A C11 C12 33.8(18) . . ? C13 C11 C12 103.1(11) . . ? C1 C11 C12 106.6(8) . . ? C23 C21 C22 109.0(4) . . ? C23 C21 C2 117.2(4) . . ? C22 C21 C2 112.4(5) . . ? C33 C31 C3 118.2(3) . . ? C33 C31 C32 109.0(4) . . ? C3 C31 C32 113.0(4) . . ? C43 C41 C42 109.5(4) . . ? C43 C41 C4 113.6(4) . . ? C42 C41 C4 112.7(4) . . ? Na1 Na1 N2 78.6(3) 9_656 . ? Na1 Na1 N2 72.3(3) 9_656 9_656 ? N2 Na1 N2 150.95(14) . 9_656 ? Na1 Na1 N1 78.2(3) 9_656 . ? N2 Na1 N1 73.54(15) . . ? N2 Na1 N1 100.03(16) 9_656 . ? Na1 Na1 N1 73.5(3) 9_656 9_656 ? N2 Na1 N1 100.48(16) . 9_656 ? N2 Na1 N1 71.48(14) 9_656 9_656 ? N1 Na1 N1 151.69(14) . 9_656 ? Na1 Na1 Cl1 176.0(3) 9_656 . ? N2 Na1 Cl1 99.94(14) . . ? N2 Na1 Cl1 109.04(14) 9_656 . ? N1 Na1 Cl1 97.87(13) . . ? N1 Na1 Cl1 110.44(13) 9_656 . ? C52 N1 C50 111.4(5) . . ? C52 N1 C51 110.0(5) . . ? C50 N1 C51 105.4(4) . . ? C52 N1 Na1 103.3(4) . . ? C50 N1 Na1 99.9(3) . . ? C51 N1 Na1 126.2(3) . . ? C52 N1 Na1 104.7(3) . 9_656 ? C50 N1 Na1 123.3(3) . 9_656 ? C51 N1 Na1 101.1(3) . 9_656 ? Na1 N1 Na1 28.32(14) . 9_656 ? C54 N2 C53 115.2(7) . . ? C54 N2 C55 107.0(5) . . ? C53 N2 C55 107.5(6) . . ? C54 N2 Na1 123.6(4) . . ? C53 N2 Na1 99.9(4) . . ? C55 N2 Na1 102.2(3) . . ? C54 N2 Na1 96.5(4) . 9_656 ? C53 N2 Na1 106.3(3) . 9_656 ? C55 N2 Na1 124.5(3) . 9_656 ? Na1 N2 Na1 29.04(14) . 9_656 ? C53 C52 N1 124.0(6) . . ? C52 C53 N2 126.9(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.333 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.054 #end #3-Sm data_0167 _database_code_depnum_ccdc_archive 'CCDC 604032' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H78 Cl2 Na O4 Sm' _chemical_formula_weight 891.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall -P_2yn 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 12.6251(13) _cell_length_b 15.9950(13) _cell_length_c 24.079(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.451(16) _cell_angle_gamma 90.00 _cell_volume 4781.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1876 _exptl_absorpt_coefficient_mu 1.383 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details (STOE/XRED) _exptl_absorpt_correction_T_min 0.506 _exptl_absorpt_correction_T_max 0.813 _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 'Stoe IPDS' _diffrn_measurement_method Phi-Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45300 _diffrn_reflns_av_R_equivalents 0.0924 _diffrn_reflns_av_sigmaI/netI 0.0928 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 25.68 _reflns_number_total 8813 _reflns_number_gt 5204 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS V2.63' _computing_cell_refinement 'Stoe IPDS V2.63' _computing_data_reduction 'Stoe IPDS V2.63' _computing_structure_solution 'SIR97 (Giacovazzo et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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 'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8813 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 0.820 _refine_ls_restrained_S_all 0.820 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.096659(16) 0.760156(14) 0.846687(10) 0.03961(7) Uani 1 d . . . Cl1 Cl 0.01314(11) 0.86954(8) 0.91169(6) 0.0570(3) Uani 1 d . . . Cl2 Cl 0.01096(11) 0.64409(8) 0.90574(7) 0.0566(4) Uani 1 d . . . Na1 Na -0.07719(13) 0.75344(16) 0.97918(7) 0.0674(5) Uani 1 d . . . O1 O -0.0268(5) 0.8290(4) 1.0662(3) 0.1157(19) Uani 1 d . . . O2 O -0.0393(5) 0.6626(4) 1.0649(3) 0.1112(19) Uani 1 d . . . O3 O -0.2350(6) 0.6653(7) 0.9660(4) 0.184(4) Uani 1 d . . . O4 O -0.2432(5) 0.8351(7) 0.9771(4) 0.186(4) Uani 1 d . . . C1 C -0.0244(4) 0.6783(3) 0.7572(2) 0.0486(13) Uani 1 d . . . C2 C -0.0978(3) 0.7396(4) 0.76845(17) 0.0489(11) Uani 1 d . . . C3 C -0.0613(4) 0.8190(3) 0.7525(2) 0.0510(13) Uani 1 d . . . C4 C 0.0356(4) 0.8056(3) 0.7318(2) 0.0516(13) Uani 1 d . . . C5 C 0.0569(4) 0.7206(3) 0.7348(2) 0.0520(13) Uani 1 d . . . H5 H 0.1159 0.6951 0.7237 0.062 Uiso 1 calc R . . C6 C 0.3088(4) 0.7063(3) 0.8563(2) 0.0462(12) Uani 1 d . . . C7 C 0.2888(3) 0.6969(3) 0.9125(2) 0.0430(12) Uani 1 d . . . C8 C 0.2752(3) 0.7786(3) 0.93459(19) 0.0424(12) Uani 1 d . . . C9 C 0.2862(3) 0.8372(3) 0.8920(2) 0.0447(12) Uani 1 d . . . C10 C 0.3071(3) 0.7927(3) 0.8448(2) 0.0462(12) Uani 1 d . . . H10 H 0.3180 0.8167 0.8112 0.055 Uiso 1 calc R . . C11 C -0.0406(4) 0.5840(3) 0.7585(2) 0.0648(15) Uani 1 d . . . H11 H -0.0775 0.5708 0.7899 0.078 Uiso 1 calc R . . C12 C 0.0668(5) 0.5365(4) 0.7677(3) 0.093(2) Uani 1 d . . . H12A H 0.1045 0.5491 0.7375 0.140 Uiso 1 calc R . . H12B H 0.0533 0.4775 0.7684 0.140 Uiso 1 calc R . . H12C H 0.1099 0.5533 0.8030 0.140 Uiso 1 calc R . . C13 C -0.1095(5) 0.5521(4) 0.7041(3) 0.109(3) Uani 1 d . . . H13A H -0.1785 0.5792 0.6984 0.164 Uiso 1 calc R . . H13B H -0.1191 0.4928 0.7067 0.164 Uiso 1 calc R . . H13C H -0.0743 0.5642 0.6728 0.164 Uiso 1 calc R . . C14 C -0.0070(10) 0.9145(6) 1.0706(5) 0.175(5) Uani 1 d . . . H14A H 0.0021 0.9310 1.1095 0.262 Uiso 1 calc R . . H14B H -0.0668 0.9443 1.0491 0.262 Uiso 1 calc R . . H14C H 0.0572 0.9273 1.0562 0.262 Uiso 1 calc R . . C15 C -0.0428(9) 0.7894(9) 1.1126(4) 0.143(4) Uani 1 d . . . H15A H -0.1176 0.7966 1.1160 0.172 Uiso 1 calc R . . H15B H 0.0008 0.8163 1.1450 0.172 Uiso 1 calc R . . C16 C -0.0194(10) 0.7037(9) 1.1153(4) 0.150(4) Uani 1 d . . . H16A H 0.0561 0.6966 1.1318 0.180 Uiso 1 calc R . . H16B H -0.0613 0.6775 1.1405 0.180 Uiso 1 calc R . . C17 C 0.0064(8) 0.5833(5) 1.0669(4) 0.145(4) Uani 1 d . . . H17A H 0.0832 0.5883 1.0707 0.217 Uiso 1 calc R . . H17B H -0.0218 0.5537 1.0328 0.217 Uiso 1 calc R . . H17C H -0.0106 0.5533 1.0987 0.217 Uiso 1 calc R . . C21 C -0.2046(3) 0.7198(3) 0.7868(2) 0.0617(15) Uani 1 d . . . H21 H -0.1989 0.6613 0.7992 0.074 Uiso 1 calc R . . C22 C -0.2329(4) 0.7679(4) 0.8357(2) 0.0825(18) Uani 1 d . . . H22A H -0.1775 0.7602 0.8683 0.124 Uiso 1 calc R . . H22B H -0.3003 0.7480 0.8438 0.124 Uiso 1 calc R . . H22C H -0.2390 0.8263 0.8263 0.124 Uiso 1 calc R . . C23 C -0.2964(4) 0.7216(5) 0.7356(3) 0.100(2) Uani 1 d . . . H23A H -0.3597 0.6969 0.7455 0.151 Uiso 1 calc R . . H23B H -0.2756 0.6906 0.7051 0.151 Uiso 1 calc R . . H23C H -0.3113 0.7785 0.7240 0.151 Uiso 1 calc R . . C24 C -0.2548(9) 0.5898(9) 0.9402(6) 0.201(7) Uani 1 d . . . H24A H -0.2908 0.5542 0.9630 0.301 Uiso 1 calc R . . H24B H -0.1880 0.5646 0.9356 0.301 Uiso 1 calc R . . H24C H -0.2997 0.5974 0.9039 0.301 Uiso 1 calc R . . C25 C -0.3024(9) 0.6904(11) 0.9927(6) 0.198(7) Uani 1 d . . . H25A H -0.2722 0.6880 1.0327 0.237 Uiso 1 calc R . . H25B H -0.3642 0.6533 0.9858 0.237 Uiso 1 calc R . . C26 C -0.3383(7) 0.7755(10) 0.9782(5) 0.176(6) Uani 1 d . . . H26A H -0.3800 0.7955 1.0056 0.212 Uiso 1 calc R . . H26B H -0.3848 0.7755 0.9414 0.212 Uiso 1 calc R . . C27 C -0.2655(12) 0.9129(10) 0.9581(7) 0.261(11) Uani 1 d . . . H27A H -0.2629 0.9152 0.9186 0.392 Uiso 1 calc R . . H27B H -0.2134 0.9509 0.9783 0.392 Uiso 1 calc R . . H27C H -0.3362 0.9283 0.9639 0.392 Uiso 1 calc R . . C31 C -0.1254(4) 0.8995(3) 0.7494(2) 0.0662(15) Uani 1 d . . . H31 H -0.1823 0.8881 0.7712 0.079 Uiso 1 calc R . . C32 C -0.0683(5) 0.9753(4) 0.7770(3) 0.0850(19) Uani 1 d . . . H32A H -0.0476 0.9656 0.8169 0.128 Uiso 1 calc R . . H32B H -0.1157 1.0227 0.7708 0.128 Uiso 1 calc R . . H32C H -0.0053 0.9861 0.7611 0.128 Uiso 1 calc R . . C33 C -0.1849(6) 0.9186(5) 0.6905(3) 0.122(3) Uani 1 d . . . H33A H -0.2403 0.9591 0.6924 0.183 Uiso 1 calc R . . H33B H -0.2170 0.8683 0.6733 0.183 Uiso 1 calc R . . H33C H -0.1354 0.9406 0.6683 0.183 Uiso 1 calc R . . C41 C 0.0843(4) 0.8642(4) 0.6935(2) 0.0653(15) Uani 1 d . . . H41 H 0.0648 0.9216 0.7017 0.078 Uiso 1 calc R . . C42 C 0.2035(5) 0.8606(5) 0.6984(3) 0.104(2) Uani 1 d . . . H42A H 0.2371 0.8796 0.7352 0.156 Uiso 1 calc R . . H42B H 0.2251 0.8957 0.6701 0.156 Uiso 1 calc R . . H42C H 0.2250 0.8040 0.6931 0.156 Uiso 1 calc R . . C43 C 0.0363(7) 0.8457(6) 0.6320(3) 0.146(4) Uani 1 d . . . H43A H 0.0499 0.8920 0.6089 0.219 Uiso 1 calc R . . H43B H -0.0399 0.8375 0.6283 0.219 Uiso 1 calc R . . H43C H 0.0688 0.7961 0.6202 0.219 Uiso 1 calc R . . C61 C 0.3565(4) 0.6426(3) 0.8209(2) 0.0606(14) Uani 1 d . . . H61 H 0.3159 0.5904 0.8208 0.073 Uiso 1 calc R . . C62 C 0.3553(5) 0.6680(4) 0.7601(3) 0.089(2) Uani 1 d . . . H62A H 0.2822 0.6704 0.7402 0.134 Uiso 1 calc R . . H62B H 0.3946 0.6277 0.7424 0.134 Uiso 1 calc R . . H62C H 0.3882 0.7220 0.7592 0.134 Uiso 1 calc R . . C63 C 0.4736(4) 0.6255(5) 0.8482(3) 0.100(2) Uani 1 d . . . H63A H 0.5026 0.5827 0.8274 0.150 Uiso 1 calc R . . H63B H 0.4765 0.6072 0.8865 0.150 Uiso 1 calc R . . H63C H 0.5151 0.6757 0.8480 0.150 Uiso 1 calc R . . C71 C 0.2918(4) 0.6165(3) 0.9469(2) 0.0641(15) Uani 1 d . . . H71 H 0.2360 0.6239 0.9699 0.077 Uiso 1 calc R . . C72 C 0.2625(5) 0.5361(4) 0.9149(3) 0.0821(19) Uani 1 d . . . H72A H 0.3189 0.5211 0.8949 0.123 Uiso 1 calc R . . H72B H 0.1964 0.5437 0.8885 0.123 Uiso 1 calc R . . H72C H 0.2535 0.4925 0.9410 0.123 Uiso 1 calc R . . C73 C 0.3965(5) 0.6069(4) 0.9893(3) 0.090(2) Uani 1 d . . . H73A H 0.3927 0.5578 1.0117 0.135 Uiso 1 calc R . . H73B H 0.4070 0.6551 1.0134 0.135 Uiso 1 calc R . . H73C H 0.4556 0.6019 0.9695 0.135 Uiso 1 calc R . . C81 C 0.2630(4) 0.8065(3) 0.9936(2) 0.0598(13) Uani 1 d . . . H81 H 0.2182 0.8569 0.9879 0.072 Uiso 1 calc R . . C82 C 0.2064(4) 0.7484(5) 1.0285(2) 0.0868(17) Uani 1 d . . . H82A H 0.1399 0.7296 1.0061 0.130 Uiso 1 calc R . . H82B H 0.1918 0.7777 1.0611 0.130 Uiso 1 calc R . . H82C H 0.2517 0.7011 1.0404 0.130 Uiso 1 calc R . . C83 C 0.3697(4) 0.8348(4) 1.0294(3) 0.0819(19) Uani 1 d . . . H83A H 0.3567 0.8573 1.0645 0.123 Uiso 1 calc R . . H83B H 0.4017 0.8770 1.0094 0.123 Uiso 1 calc R . . H83C H 0.4176 0.7879 1.0367 0.123 Uiso 1 calc R . . C91 C 0.2933(4) 0.9315(3) 0.8980(3) 0.0626(15) Uani 1 d . . . H91 H 0.2640 0.9472 0.9315 0.075 Uiso 1 calc R . . C92 C 0.2283(5) 0.9774(4) 0.8472(3) 0.0840(19) Uani 1 d . . . H92A H 0.2593 0.9667 0.8143 0.126 Uiso 1 calc R . . H92B H 0.2297 1.0364 0.8547 0.126 Uiso 1 calc R . . H92C H 0.1552 0.9580 0.8408 0.126 Uiso 1 calc R . . C93 C 0.4097(5) 0.9625(4) 0.9062(4) 0.107(3) Uani 1 d . . . H93A H 0.4515 0.9357 0.9386 0.161 Uiso 1 calc R . . H93B H 0.4112 1.0220 0.9118 0.161 Uiso 1 calc R . . H93C H 0.4395 0.9493 0.8733 0.161 Uiso 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 Sm1 0.03969(9) 0.04062(15) 0.03858(10) 0.00031(15) 0.00729(7) -0.00156(13) Cl1 0.0638(8) 0.0482(9) 0.0610(10) -0.0060(6) 0.0168(7) 0.0059(6) Cl2 0.0615(8) 0.0489(9) 0.0617(10) 0.0059(6) 0.0174(7) -0.0090(6) Na1 0.0652(9) 0.0778(15) 0.0631(11) -0.0081(13) 0.0217(8) -0.0070(12) O1 0.183(6) 0.090(5) 0.075(4) -0.022(3) 0.026(4) 0.012(3) O2 0.136(5) 0.082(4) 0.106(5) 0.027(3) -0.003(4) -0.002(3) O3 0.106(5) 0.269(11) 0.186(8) 0.014(7) 0.050(5) -0.082(6) O4 0.077(5) 0.282(11) 0.195(8) -0.102(7) 0.009(5) 0.040(5) C1 0.052(3) 0.044(4) 0.046(3) -0.009(2) -0.001(2) -0.004(2) C2 0.050(2) 0.052(4) 0.043(2) 0.002(3) 0.0018(17) -0.008(3) C3 0.048(3) 0.058(4) 0.041(3) 0.005(2) -0.005(2) -0.005(2) C4 0.056(3) 0.055(4) 0.041(3) 0.003(2) 0.000(2) -0.011(2) C5 0.054(3) 0.064(4) 0.041(3) -0.006(2) 0.016(2) -0.006(2) C6 0.043(3) 0.049(3) 0.047(3) -0.007(2) 0.009(2) -0.001(2) C7 0.037(2) 0.046(3) 0.044(3) 0.000(2) 0.003(2) 0.000(2) C8 0.035(2) 0.049(4) 0.042(3) -0.004(2) 0.0016(18) 0.0015(18) C9 0.038(2) 0.040(3) 0.055(3) 0.000(2) 0.002(2) -0.0055(19) C10 0.040(3) 0.061(4) 0.039(3) 0.003(2) 0.010(2) -0.003(2) C11 0.076(4) 0.056(4) 0.063(4) -0.012(3) 0.014(3) -0.012(3) C12 0.110(5) 0.048(4) 0.111(6) -0.015(4) -0.008(4) 0.010(3) C13 0.094(5) 0.087(6) 0.133(7) -0.048(5) -0.020(4) -0.017(4) C14 0.266(14) 0.087(9) 0.159(11) -0.049(7) 0.007(10) -0.004(7) C15 0.174(9) 0.189(12) 0.079(8) -0.040(7) 0.054(6) -0.020(8) C16 0.221(12) 0.154(11) 0.078(8) 0.036(7) 0.037(7) 0.018(9) C17 0.175(9) 0.078(7) 0.168(11) 0.031(6) -0.007(7) -0.002(6) C21 0.043(2) 0.068(4) 0.070(3) 0.007(3) 0.000(2) -0.006(2) C22 0.057(3) 0.115(6) 0.077(4) -0.006(4) 0.018(3) -0.010(3) C23 0.052(3) 0.147(7) 0.093(5) -0.019(4) -0.012(3) -0.020(3) C24 0.154(10) 0.222(15) 0.215(15) 0.039(11) 0.005(10) -0.109(10) C25 0.082(8) 0.37(2) 0.152(11) -0.032(12) 0.043(8) -0.029(10) C26 0.057(5) 0.33(2) 0.154(9) 0.040(10) 0.042(5) 0.069(8) C27 0.226(16) 0.27(2) 0.269(19) -0.107(15) -0.014(13) 0.160(16) C31 0.064(3) 0.060(4) 0.068(4) 0.017(3) -0.007(3) 0.008(3) C32 0.094(4) 0.052(5) 0.103(5) 0.010(4) 0.001(4) 0.011(3) C33 0.114(6) 0.101(6) 0.126(7) 0.017(5) -0.044(5) 0.021(4) C41 0.075(3) 0.077(4) 0.041(3) 0.017(3) 0.004(2) -0.015(3) C42 0.079(4) 0.126(7) 0.109(6) 0.047(5) 0.026(4) -0.017(4) C43 0.149(7) 0.225(11) 0.054(5) 0.032(5) -0.008(5) -0.085(7) C61 0.050(3) 0.066(4) 0.068(4) -0.015(3) 0.018(2) 0.007(2) C62 0.093(4) 0.111(6) 0.068(4) -0.020(4) 0.023(4) 0.019(4) C63 0.058(3) 0.138(7) 0.102(6) -0.033(5) 0.008(3) 0.034(4) C71 0.062(3) 0.055(4) 0.070(4) 0.011(3) -0.002(3) 0.008(2) C72 0.088(4) 0.056(5) 0.095(5) 0.009(3) -0.001(4) -0.002(3) C73 0.080(4) 0.075(5) 0.100(5) 0.019(4) -0.020(4) 0.013(3) C81 0.057(3) 0.075(4) 0.044(3) -0.008(3) 0.000(2) 0.007(2) C82 0.084(3) 0.123(6) 0.057(3) -0.003(5) 0.023(3) -0.010(4) C83 0.071(4) 0.107(6) 0.062(4) -0.014(4) -0.004(3) -0.002(3) C91 0.059(3) 0.050(4) 0.078(4) -0.003(3) 0.010(3) -0.006(2) C92 0.090(4) 0.050(4) 0.106(5) 0.020(3) 0.001(4) -0.006(3) C93 0.077(4) 0.070(5) 0.161(8) 0.003(4) -0.012(4) -0.038(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 Sm1 Cl2 2.6827(14) . ? Sm1 Cl1 2.6873(14) . ? Sm1 C10 2.715(4) . ? Sm1 C5 2.725(5) . ? Sm1 C9 2.737(4) . ? Sm1 C1 2.739(5) . ? Sm1 C6 2.783(4) . ? Sm1 C8 2.814(4) . ? Sm1 C4 2.828(5) . ? Sm1 C2 2.829(4) . ? Sm1 C7 2.832(4) . ? Sm1 C3 2.892(5) . ? Cl1 Na1 2.839(3) . ? Cl2 Na1 2.853(3) . ? Na1 O1 2.402(6) . ? Na1 O3 2.414(7) . ? Na1 O4 2.462(7) . ? Na1 O2 2.498(6) . ? Na1 C25 3.089(12) . ? O1 C15 1.333(11) . ? O1 C14 1.391(9) . ? O2 C16 1.363(11) . ? O2 C17 1.390(9) . ? O3 C25 1.224(12) . ? O3 C24 1.360(14) . ? O4 C27 1.338(17) . ? O4 C26 1.537(14) . ? C1 C2 1.409(7) . ? C1 C5 1.415(7) . ? C1 C11 1.522(7) . ? C2 C3 1.426(7) . ? C2 C21 1.527(6) . ? C3 C4 1.420(7) . ? C3 C31 1.515(7) . ? C4 C5 1.385(7) . ? C4 C41 1.523(7) . ? C6 C10 1.408(6) . ? C6 C7 1.428(7) . ? C6 C61 1.521(7) . ? C7 C8 1.433(6) . ? C7 C71 1.526(7) . ? C8 C9 1.414(6) . ? C8 C81 1.524(6) . ? C9 C10 1.405(7) . ? C9 C91 1.516(7) . ? C11 C13 1.523(8) . ? C11 C12 1.535(8) . ? C15 C16 1.402(11) . ? C21 C22 1.504(7) . ? C21 C23 1.532(7) . ? C25 C26 1.457(17) . ? C31 C32 1.503(8) . ? C31 C33 1.511(8) . ? C41 C42 1.488(7) . ? C41 C43 1.522(8) . ? C61 C62 1.516(8) . ? C61 C63 1.530(7) . ? C71 C72 1.509(8) . ? C71 C73 1.524(7) . ? C81 C82 1.516(7) . ? C81 C83 1.529(7) . ? C91 C93 1.530(7) . ? C91 C92 1.531(8) . ? 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 Cl2 Sm1 Cl1 84.45(4) . . ? Cl2 Sm1 C10 129.14(11) . . ? Cl1 Sm1 C10 111.90(11) . . ? Cl2 Sm1 C5 110.10(11) . . ? Cl1 Sm1 C5 134.90(12) . . ? C10 Sm1 C5 91.94(15) . . ? Cl2 Sm1 C9 120.51(12) . . ? Cl1 Sm1 C9 83.20(11) . . ? C10 Sm1 C9 29.87(14) . . ? C5 Sm1 C9 119.35(15) . . ? Cl2 Sm1 C1 82.25(12) . . ? Cl1 Sm1 C1 123.22(11) . . ? C10 Sm1 C1 119.13(16) . . ? C5 Sm1 C1 30.02(14) . . ? C9 Sm1 C1 148.42(16) . . ? Cl2 Sm1 C6 102.49(11) . . ? Cl1 Sm1 C6 128.78(11) . . ? C10 Sm1 C6 29.65(13) . . ? C5 Sm1 C6 90.72(15) . . ? C9 Sm1 C6 49.25(14) . . ? C1 Sm1 C6 107.99(15) . . ? Cl2 Sm1 C8 91.09(10) . . ? Cl1 Sm1 C8 80.73(10) . . ? C10 Sm1 C8 48.67(14) . . ? C5 Sm1 C8 138.35(13) . . ? C9 Sm1 C8 29.48(13) . . ? C1 Sm1 C8 153.98(14) . . ? C6 Sm1 C8 48.87(14) . . ? Cl2 Sm1 C4 129.16(11) . . ? Cl1 Sm1 C4 109.65(12) . . ? C10 Sm1 C4 91.64(15) . . ? C5 Sm1 C4 28.81(14) . . ? C9 Sm1 C4 109.75(15) . . ? C1 Sm1 C4 48.62(15) . . ? C6 Sm1 C4 104.38(15) . . ? C8 Sm1 C4 138.40(14) . . ? Cl2 Sm1 C2 83.56(11) . . ? Cl1 Sm1 C2 94.52(10) . . ? C10 Sm1 C2 138.13(14) . . ? C5 Sm1 C2 48.12(13) . . ? C9 Sm1 C2 155.26(15) . . ? C1 Sm1 C2 29.26(14) . . ? C6 Sm1 C2 136.48(14) . . ? C8 Sm1 C2 173.19(12) . . ? C4 Sm1 C2 47.86(13) . . ? Cl2 Sm1 C7 80.98(10) . . ? Cl1 Sm1 C7 107.07(11) . . ? C10 Sm1 C7 48.43(15) . . ? C5 Sm1 C7 117.11(15) . . ? C9 Sm1 C7 48.66(14) . . ? C1 Sm1 C7 124.63(15) . . ? C6 Sm1 C7 29.45(14) . . ? C8 Sm1 C7 29.41(13) . . ? C4 Sm1 C7 133.83(15) . . ? C2 Sm1 C7 151.93(17) . . ? Cl2 Sm1 C3 110.70(11) . . ? Cl1 Sm1 C3 87.53(12) . . ? C10 Sm1 C3 117.55(15) . . ? C5 Sm1 C3 47.40(16) . . ? C9 Sm1 C3 126.52(15) . . ? C1 Sm1 C3 48.06(14) . . ? C6 Sm1 C3 133.05(16) . . ? C8 Sm1 C3 154.17(15) . . ? C4 Sm1 C3 28.71(14) . . ? C2 Sm1 C3 28.85(14) . . ? C7 Sm1 C3 162.48(15) . . ? Sm1 Cl1 Na1 98.53(6) . . ? Sm1 Cl2 Na1 98.31(6) . . ? O1 Na1 O3 119.4(3) . . ? O1 Na1 O4 80.8(2) . . ? O3 Na1 O4 68.2(3) . . ? O1 Na1 O2 65.92(19) . . ? O3 Na1 O2 78.4(3) . . ? O4 Na1 O2 111.1(3) . . ? O1 Na1 Cl1 95.71(19) . . ? O3 Na1 Cl1 135.6(2) . . ? O4 Na1 Cl1 94.0(3) . . ? O2 Na1 Cl1 144.74(15) . . ? O1 Na1 Cl2 141.05(17) . . ? O3 Na1 Cl2 88.0(3) . . ? O4 Na1 Cl2 137.7(2) . . ? O2 Na1 Cl2 96.75(18) . . ? Cl1 Na1 Cl2 78.69(5) . . ? O1 Na1 C25 100.1(3) . . ? O3 Na1 C25 21.5(4) . . ? O4 Na1 C25 51.6(4) . . ? O2 Na1 C25 76.4(3) . . ? Cl1 Na1 C25 138.3(3) . . ? Cl2 Na1 C25 109.6(3) . . ? C15 O1 C14 117.1(8) . . ? C15 O1 Na1 115.8(6) . . ? C14 O1 Na1 125.3(6) . . ? C16 O2 C17 113.5(8) . . ? C16 O2 Na1 115.6(6) . . ? C17 O2 Na1 125.2(6) . . ? C25 O3 C24 116.3(10) . . ? C25 O3 Na1 112.0(10) . . ? C24 O3 Na1 131.1(8) . . ? C27 O4 C26 117.7(9) . . ? C27 O4 Na1 128.7(10) . . ? C26 O4 Na1 109.6(7) . . ? C2 C1 C5 106.7(5) . . ? C2 C1 C11 126.2(5) . . ? C5 C1 C11 126.2(5) . . ? C2 C1 Sm1 78.9(3) . . ? C5 C1 Sm1 74.4(3) . . ? C11 C1 Sm1 121.0(3) . . ? C1 C2 C3 108.2(4) . . ? C1 C2 C21 123.9(5) . . ? C3 C2 C21 127.4(4) . . ? C1 C2 Sm1 71.8(2) . . ? C3 C2 Sm1 78.0(3) . . ? C21 C2 Sm1 122.5(3) . . ? C4 C3 C2 107.5(4) . . ? C4 C3 C31 126.7(5) . . ? C2 C3 C31 125.1(5) . . ? C4 C3 Sm1 73.1(3) . . ? C2 C3 Sm1 73.1(3) . . ? C31 C3 Sm1 127.0(4) . . ? C5 C4 C3 107.6(4) . . ? C5 C4 C41 122.7(5) . . ? C3 C4 C41 126.1(5) . . ? C5 C4 Sm1 71.5(3) . . ? C3 C4 Sm1 78.2(3) . . ? C41 C4 Sm1 133.1(3) . . ? C4 C5 C1 110.0(5) . . ? C4 C5 Sm1 79.7(3) . . ? C1 C5 Sm1 75.6(3) . . ? C10 C6 C7 106.9(4) . . ? C10 C6 C61 122.7(5) . . ? C7 C6 C61 128.0(5) . . ? C10 C6 Sm1 72.5(3) . . ? C7 C6 Sm1 77.2(3) . . ? C61 C6 Sm1 129.3(3) . . ? C6 C7 C8 108.0(4) . . ? C6 C7 C71 127.7(5) . . ? C8 C7 C71 124.0(4) . . ? C6 C7 Sm1 73.3(3) . . ? C8 C7 Sm1 74.6(3) . . ? C71 C7 Sm1 122.6(3) . . ? C9 C8 C7 107.5(4) . . ? C9 C8 C81 121.4(5) . . ? C7 C8 C81 130.7(4) . . ? C9 C8 Sm1 72.3(3) . . ? C7 C8 Sm1 76.0(3) . . ? C81 C8 Sm1 122.0(3) . . ? C10 C9 C8 107.9(4) . . ? C10 C9 C91 124.3(5) . . ? C8 C9 C91 127.0(5) . . ? C10 C9 Sm1 74.2(3) . . ? C8 C9 Sm1 78.3(3) . . ? C91 C9 Sm1 121.2(3) . . ? C9 C10 C6 109.7(5) . . ? C9 C10 Sm1 75.9(3) . . ? C6 C10 Sm1 77.8(3) . . ? C1 C11 C13 111.8(5) . . ? C1 C11 C12 112.0(5) . . ? C13 C11 C12 108.1(5) . . ? O1 C15 C16 116.2(9) . . ? O2 C16 C15 115.3(10) . . ? C22 C21 C2 117.9(4) . . ? C22 C21 C23 111.6(4) . . ? C2 C21 C23 110.0(4) . . ? O3 C25 C26 113.3(14) . . ? O3 C25 Na1 46.4(7) . . ? C26 C25 Na1 85.5(7) . . ? C25 C26 O4 111.9(8) . . ? C32 C31 C3 117.0(5) . . ? C32 C31 C33 111.7(5) . . ? C3 C31 C33 112.9(5) . . ? C42 C41 C4 116.1(5) . . ? C42 C41 C43 106.8(6) . . ? C4 C41 C43 109.7(5) . . ? C62 C61 C6 115.2(5) . . ? C62 C61 C63 107.7(5) . . ? C6 C61 C63 109.2(4) . . ? C72 C71 C73 111.0(5) . . ? C72 C71 C7 117.5(5) . . ? C73 C71 C7 112.4(4) . . ? C82 C81 C8 118.3(5) . . ? C82 C81 C83 109.0(4) . . ? C8 C81 C83 112.6(4) . . ? C9 C91 C93 111.9(4) . . ? C9 C91 C92 112.8(5) . . ? C93 C91 C92 108.1(5) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.498 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.068 #===end #6-Nd data_0178 _database_code_depnum_ccdc_archive 'CCDC 604033' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H67 Al Cl Nd' _chemical_formula_weight 718.58 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.6235(7) _cell_length_b 18.0143(10) _cell_length_c 35.025(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7964.9(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 24.15 _exptl_crystal_description 'transparent block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3032 _exptl_absorpt_coefficient_mu 1.414 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(ABST/PLATON 98)' _exptl_absorpt_correction_T_min 0.53052 _exptl_absorpt_correction_T_max 0.72046 _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 'Stoe IPDS' _diffrn_measurement_method Phi-Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56112 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 24.08 _reflns_number_total 6231 _reflns_number_gt 4141 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS V2.63' _computing_cell_refinement 'Stoe IPDS V2.63' _computing_data_reduction 'Stoe IPDS V2.63' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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 'w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+9.9225P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6231 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.004 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.858870(19) 0.153238(16) 0.375246(8) 0.05056(11) Uani 1 d . . . Al1 Al 1.10019(16) 0.36295(13) 0.37064(7) 0.0861(6) Uani 1 d . . . Cl1 Cl 0.93818(12) 0.29292(10) 0.37208(6) 0.0896(5) Uani 1 d . . . C1 C 0.7918(4) 0.1613(3) 0.29770(15) 0.0575(14) Uani 1 d . . . C2 C 0.7611(4) 0.0887(4) 0.31079(16) 0.0620(15) Uani 1 d . . . C3 C 0.6822(4) 0.1019(4) 0.34018(18) 0.0644(16) Uani 1 d . . . H3 H 0.6483 0.0647 0.3540 0.077 Uiso 1 calc R . . C4 C 0.6640(4) 0.1767(3) 0.34497(16) 0.0548(14) Uani 1 d . . . C5 C 0.7332(4) 0.2132(3) 0.32012(15) 0.0567(14) Uani 1 d . . . H5 H 0.7401 0.2645 0.3184 0.068 Uiso 1 calc R . . C6 C 1.0121(4) 0.0710(4) 0.40770(17) 0.0674(16) Uani 1 d . . . C7 C 1.0057(4) 0.1337(4) 0.43048(17) 0.0690(18) Uani 1 d . . . H7 H 1.0562 0.1712 0.4307 0.083 Uiso 1 calc R . . C8 C 0.9132(5) 0.1339(4) 0.45349(16) 0.0685(17) Uani 1 d . . . C9 C 0.8556(4) 0.0677(4) 0.44310(17) 0.0697(17) Uani 1 d . . . C10 C 0.9190(5) 0.0309(4) 0.41439(17) 0.0686(16) Uani 1 d . . . H10 H 0.9005 -0.0130 0.4021 0.082 Uiso 1 calc R . . C11 C 0.8570(5) 0.1896(4) 0.26332(16) 0.0688(16) Uani 1 d . . . C12 C 0.8529(7) 0.2751(5) 0.2615(2) 0.109(3) Uani 1 d . . . H12A H 0.8803 0.2954 0.2849 0.164 Uiso 1 calc R . . H12B H 0.7809 0.2910 0.2581 0.164 Uiso 1 calc R . . H12C H 0.8949 0.2922 0.2404 0.164 Uiso 1 calc R . . C13 C 0.9725(6) 0.1714(6) 0.2639(2) 0.114(3) Uani 1 d . . . H13A H 0.9814 0.1188 0.2670 0.170 Uiso 1 calc R . . H13B H 1.0058 0.1968 0.2848 0.170 Uiso 1 calc R . . H13C H 1.0044 0.1868 0.2404 0.170 Uiso 1 calc R . . C14 C 0.8050(7) 0.1628(5) 0.2263(2) 0.109(3) Uani 1 d . . . H14A H 0.8345 0.1894 0.2051 0.164 Uiso 1 calc R . . H14B H 0.7301 0.1717 0.2275 0.164 Uiso 1 calc R . . H14C H 0.8178 0.1107 0.2232 0.164 Uiso 1 calc R . . C21 C 0.7725(6) 0.0098(4) 0.2946(2) 0.0745(18) Uani 1 d . . . C22 C 0.6850(6) -0.0005(5) 0.2644(2) 0.106(3) Uani 1 d . . . H22A H 0.6919 -0.0486 0.2528 0.159 Uiso 1 calc R . . H22B H 0.6918 0.0371 0.2452 0.159 Uiso 1 calc R . . H22C H 0.6169 0.0035 0.2764 0.159 Uiso 1 calc R . . C23 C 0.7563(7) -0.0477(4) 0.3252(2) 0.112(3) Uani 1 d . . . H23A H 0.7697 -0.0962 0.3149 0.168 Uiso 1 calc R . . H23B H 0.6846 -0.0453 0.3343 0.168 Uiso 1 calc R . . H23C H 0.8041 -0.0384 0.3460 0.168 Uiso 1 calc R . . C24 C 0.8775(6) -0.0073(5) 0.2744(3) 0.123(3) Uani 1 d . . . H24A H 0.9345 -0.0049 0.2925 0.185 Uiso 1 calc R . . H24B H 0.8893 0.0284 0.2545 0.185 Uiso 1 calc R . . H24C H 0.8746 -0.0562 0.2635 0.185 Uiso 1 calc R . . C30 C 1.2072(7) 0.2932(8) 0.3853(5) 0.226(8) Uani 1 d . . . H30A H 1.2510 0.2820 0.3636 0.339 Uiso 1 calc R . . H30B H 1.1743 0.2485 0.3943 0.339 Uiso 1 calc R . . H30C H 1.2500 0.3142 0.4052 0.339 Uiso 1 calc R . . C31 C 1.0710(11) 0.4315(8) 0.4113(5) 0.290(11) Uani 1 d . . . H31A H 1.0484 0.4781 0.4008 0.435 Uiso 1 calc R . . H31B H 1.1339 0.4389 0.4262 0.435 Uiso 1 calc R . . H31C H 1.0159 0.4118 0.4273 0.435 Uiso 1 calc R . . C32 C 1.0972(13) 0.4024(15) 0.3227(5) 0.44(2) Uani 1 d . . . H32A H 1.1605 0.3885 0.3093 0.666 Uiso 1 calc R . . H32B H 1.0931 0.4555 0.3244 0.666 Uiso 1 calc R . . H32C H 1.0365 0.3838 0.3092 0.666 Uiso 1 calc R . . C41 C 0.5854(4) 0.2140(4) 0.37161(17) 0.0646(15) Uani 1 d . . . C42 C 0.5290(7) 0.2757(6) 0.3508(3) 0.140(4) Uani 1 d . . . H42A H 0.4892 0.2553 0.3299 0.210 Uiso 1 calc R . . H42B H 0.5801 0.3104 0.3411 0.210 Uiso 1 calc R . . H42C H 0.4818 0.3006 0.3680 0.210 Uiso 1 calc R . . C43 C 0.5019(6) 0.1620(5) 0.3855(3) 0.122(3) Uani 1 d . . . H43A H 0.5347 0.1203 0.3978 0.183 Uiso 1 calc R . . H43B H 0.4603 0.1450 0.3643 0.183 Uiso 1 calc R . . H43C H 0.4569 0.1872 0.4034 0.183 Uiso 1 calc R . . C44 C 0.6455(6) 0.2453(7) 0.4050(2) 0.134(4) Uani 1 d . . . H44A H 0.5967 0.2586 0.4249 0.201 Uiso 1 calc R . . H44B H 0.6839 0.2887 0.3970 0.201 Uiso 1 calc R . . H44C H 0.6943 0.2088 0.4144 0.201 Uiso 1 calc R . . C61 C 1.1002(5) 0.0526(4) 0.37964(19) 0.0781(19) Uani 1 d . . . C62 C 1.2059(5) 0.0719(7) 0.3959(3) 0.142(4) Uani 1 d . . . H62A H 1.2603 0.0593 0.3778 0.213 Uiso 1 calc R . . H62B H 1.2170 0.0445 0.4191 0.213 Uiso 1 calc R . . H62C H 1.2086 0.1241 0.4012 0.213 Uiso 1 calc R . . C63 C 1.0785(6) 0.0966(5) 0.3436(2) 0.100(3) Uani 1 d . . . H63A H 1.0724 0.1483 0.3499 0.149 Uiso 1 calc R . . H63B H 1.0136 0.0796 0.3323 0.149 Uiso 1 calc R . . H63C H 1.1357 0.0896 0.3259 0.149 Uiso 1 calc R . . C64 C 1.0986(7) -0.0306(5) 0.3705(3) 0.124(3) Uani 1 d . . . H64A H 1.1572 -0.0425 0.3541 0.186 Uiso 1 calc R . . H64B H 1.0335 -0.0429 0.3578 0.186 Uiso 1 calc R . . H64C H 1.1041 -0.0585 0.3937 0.186 Uiso 1 calc R . . C81 C 0.9000(5) 0.1918(5) 0.48515(18) 0.085(2) Uani 1 d . . . C82 C 0.9134(10) 0.1536(6) 0.5239(2) 0.156(4) Uani 1 d . . . H82A H 0.9084 0.1899 0.5439 0.235 Uiso 1 calc R . . H82B H 0.9814 0.1299 0.5249 0.235 Uiso 1 calc R . . H82C H 0.8587 0.1171 0.5271 0.235 Uiso 1 calc R . . C83 C 0.8034(8) 0.2365(7) 0.4842(3) 0.184(6) Uani 1 d . . . H83A H 0.7968 0.2637 0.5077 0.276 Uiso 1 calc R . . H83B H 0.7431 0.2046 0.4811 0.276 Uiso 1 calc R . . H83C H 0.8067 0.2707 0.4632 0.276 Uiso 1 calc R . . C84 C 0.9930(9) 0.2440(6) 0.4845(3) 0.174(6) Uani 1 d . . . H84A H 0.9919 0.2723 0.4613 0.261 Uiso 1 calc R . . H84B H 1.0576 0.2160 0.4859 0.261 Uiso 1 calc R . . H84C H 0.9888 0.2771 0.5060 0.261 Uiso 1 calc R . . C91 C 0.7662(6) 0.0235(5) 0.4619(2) 0.086(2) Uani 1 d . . . C92 C 0.8120(8) -0.0212(7) 0.4948(3) 0.170(5) Uani 1 d . . . H92A H 0.8505 0.0113 0.5115 0.256 Uiso 1 calc R . . H92B H 0.8589 -0.0585 0.4849 0.256 Uiso 1 calc R . . H92C H 0.7555 -0.0446 0.5086 0.256 Uiso 1 calc R . . C93 C 0.7197(9) -0.0312(7) 0.4337(3) 0.181(6) Uani 1 d . . . H93A H 0.6577 -0.0538 0.4446 0.272 Uiso 1 calc R . . H93B H 0.7711 -0.0689 0.4281 0.272 Uiso 1 calc R . . H93C H 0.7006 -0.0057 0.4107 0.272 Uiso 1 calc R . . C94 C 0.6741(7) 0.0678(7) 0.4768(3) 0.170(5) Uani 1 d . . . H94A H 0.6349 0.0881 0.4558 0.255 Uiso 1 calc R . . H94B H 0.6999 0.1075 0.4926 0.255 Uiso 1 calc R . . H94C H 0.6288 0.0362 0.4917 0.255 Uiso 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 Nd1 0.04742(15) 0.05561(19) 0.04864(16) -0.00051(16) -0.00169(13) 0.00109(13) Al1 0.0652(10) 0.0829(16) 0.1103(17) 0.0099(14) -0.0043(11) -0.0141(9) Cl1 0.0734(9) 0.0762(12) 0.1194(14) 0.0091(11) -0.0165(10) -0.0204(8) C1 0.061(3) 0.057(4) 0.054(3) -0.006(3) -0.005(2) 0.004(3) C2 0.060(3) 0.062(4) 0.064(3) -0.007(3) -0.009(3) 0.010(3) C3 0.050(3) 0.065(5) 0.078(4) 0.000(3) -0.009(3) -0.005(3) C4 0.055(3) 0.045(4) 0.064(3) -0.007(3) -0.003(2) 0.006(2) C5 0.048(3) 0.055(4) 0.067(3) -0.001(3) -0.004(3) 0.006(3) C6 0.063(3) 0.076(5) 0.063(4) 0.012(3) -0.005(3) 0.012(3) C7 0.054(3) 0.088(5) 0.064(4) 0.012(3) -0.006(3) -0.008(3) C8 0.062(3) 0.088(5) 0.055(3) 0.005(3) -0.001(3) -0.001(3) C9 0.062(3) 0.085(5) 0.062(3) 0.011(3) 0.000(3) -0.005(3) C10 0.068(4) 0.065(4) 0.073(4) 0.009(3) -0.004(3) 0.001(3) C11 0.078(4) 0.077(5) 0.051(3) -0.001(3) 0.003(3) 0.007(4) C12 0.140(7) 0.099(7) 0.088(6) 0.015(5) 0.021(5) -0.003(6) C13 0.078(5) 0.178(10) 0.085(5) 0.029(6) 0.016(4) 0.018(5) C14 0.121(6) 0.141(9) 0.065(4) 0.010(5) -0.015(4) -0.004(5) C21 0.090(4) 0.058(5) 0.075(5) -0.018(3) -0.016(4) 0.015(3) C22 0.122(6) 0.088(6) 0.108(6) -0.023(5) -0.050(5) 0.003(5) C23 0.177(8) 0.048(5) 0.111(6) -0.013(5) -0.032(6) 0.015(5) C24 0.111(6) 0.091(7) 0.167(9) -0.054(6) -0.005(6) 0.034(5) C30 0.072(6) 0.185(13) 0.42(2) 0.067(14) -0.026(9) -0.022(7) C31 0.209(14) 0.210(17) 0.45(3) -0.180(18) 0.127(16) -0.114(13) C32 0.282(17) 0.77(5) 0.278(19) 0.36(3) -0.168(16) -0.37(3) C41 0.046(3) 0.081(4) 0.067(4) -0.014(4) -0.003(3) 0.000(3) C42 0.110(6) 0.142(9) 0.169(9) 0.027(7) 0.038(6) 0.078(6) C43 0.075(5) 0.124(8) 0.167(9) 0.001(6) 0.053(5) 0.000(5) C44 0.075(5) 0.242(13) 0.086(6) -0.075(6) 0.029(4) -0.022(6) C61 0.060(3) 0.100(6) 0.074(4) 0.019(4) 0.002(3) 0.022(3) C62 0.060(4) 0.242(14) 0.125(7) -0.006(8) -0.001(4) 0.039(6) C63 0.087(5) 0.125(7) 0.086(5) 0.012(5) 0.021(4) 0.026(5) C64 0.131(6) 0.106(7) 0.134(8) 0.005(6) 0.039(6) 0.052(5) C81 0.084(4) 0.120(6) 0.050(4) -0.013(4) -0.004(3) -0.013(4) C82 0.215(11) 0.192(12) 0.062(5) -0.003(6) -0.024(6) 0.017(9) C83 0.159(10) 0.210(14) 0.183(12) -0.121(10) -0.066(8) 0.096(9) C84 0.220(12) 0.182(12) 0.120(9) -0.069(8) 0.046(8) -0.095(10) C91 0.082(4) 0.102(6) 0.075(4) 0.023(4) 0.007(4) -0.023(4) C92 0.155(9) 0.195(13) 0.160(10) 0.110(9) -0.011(7) -0.050(8) C93 0.222(12) 0.203(14) 0.119(8) -0.002(8) 0.039(8) -0.143(11) C94 0.110(7) 0.187(13) 0.213(13) 0.039(10) 0.071(8) -0.015(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 C6 2.689(6) . ? Nd1 C7 2.703(5) . ? Nd1 C10 2.704(6) . ? Nd1 C3 2.709(5) . ? Nd1 Cl1 2.7105(17) . ? Nd1 C4 2.712(5) . ? Nd1 C5 2.722(5) . ? Nd1 C2 2.824(6) . ? Nd1 C9 2.833(6) . ? Nd1 C8 2.846(6) . ? Nd1 C1 2.848(5) . ? Al1 C32 1.823(12) . ? Al1 C30 1.914(11) . ? Al1 C31 1.921(13) . ? Al1 Cl1 2.403(2) . ? C1 C5 1.428(7) . ? C1 C2 1.440(8) . ? C1 C11 1.544(8) . ? C2 C3 1.452(8) . ? C2 C21 1.537(9) . ? C3 C4 1.377(8) . ? C4 C5 1.397(8) . ? C4 C41 1.519(8) . ? C6 C7 1.384(8) . ? C6 C10 1.400(8) . ? C6 C61 1.521(8) . ? C7 C8 1.419(8) . ? C8 C9 1.443(9) . ? C8 C81 1.531(9) . ? C9 C10 1.445(8) . ? C9 C91 1.531(9) . ? C11 C13 1.494(9) . ? C11 C14 1.531(9) . ? C11 C12 1.543(10) . ? C21 C23 1.507(10) . ? C21 C24 1.534(10) . ? C21 C22 1.539(9) . ? C41 C43 1.493(9) . ? C41 C44 1.503(9) . ? C41 C42 1.508(10) . ? C61 C62 1.491(10) . ? C61 C63 1.514(9) . ? C61 C64 1.533(11) . ? C81 C83 1.462(11) . ? C81 C84 1.504(11) . ? C81 C82 1.530(10) . ? C91 C94 1.504(12) . ? C91 C93 1.513(11) . ? C91 C92 1.518(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 C6 Nd1 C7 29.75(18) . . ? C6 Nd1 C10 30.10(17) . . ? C7 Nd1 C10 48.57(19) . . ? C6 Nd1 C3 126.6(2) . . ? C7 Nd1 C3 147.66(19) . . ? C10 Nd1 C3 100.53(19) . . ? C6 Nd1 Cl1 105.24(15) . . ? C7 Nd1 Cl1 84.09(15) . . ? C10 Nd1 Cl1 132.36(14) . . ? C3 Nd1 Cl1 127.04(14) . . ? C6 Nd1 C4 154.68(19) . . ? C7 Nd1 C4 157.29(17) . . ? C10 Nd1 C4 125.43(18) . . ? C3 Nd1 C4 29.42(18) . . ? Cl1 Nd1 C4 100.04(13) . . ? C6 Nd1 C5 159.68(17) . . ? C7 Nd1 C5 163.58(19) . . ? C10 Nd1 C5 147.83(19) . . ? C3 Nd1 C5 48.24(19) . . ? Cl1 Nd1 C5 79.51(13) . . ? C4 Nd1 C5 29.80(16) . . ? C6 Nd1 C2 115.20(19) . . ? C7 Nd1 C2 144.92(19) . . ? C10 Nd1 C2 101.08(19) . . ? C3 Nd1 C2 30.35(16) . . ? Cl1 Nd1 C2 120.74(14) . . ? C4 Nd1 C2 49.84(16) . . ? C5 Nd1 C2 48.83(17) . . ? C6 Nd1 C9 49.91(17) . . ? C7 Nd1 C9 48.57(17) . . ? C10 Nd1 C9 30.15(18) . . ? C3 Nd1 C9 100.54(18) . . ? Cl1 Nd1 C9 123.00(14) . . ? C4 Nd1 C9 113.56(17) . . ? C5 Nd1 C9 143.36(16) . . ? C2 Nd1 C9 116.13(19) . . ? C6 Nd1 C8 49.63(18) . . ? C7 Nd1 C8 29.50(16) . . ? C10 Nd1 C8 49.06(19) . . ? C3 Nd1 C8 126.38(18) . . ? Cl1 Nd1 C8 93.66(14) . . ? C4 Nd1 C8 127.88(17) . . ? C5 Nd1 C8 150.65(17) . . ? C2 Nd1 C8 145.56(19) . . ? C9 Nd1 C8 29.45(18) . . ? C6 Nd1 C1 130.17(18) . . ? C7 Nd1 C1 153.25(17) . . ? C10 Nd1 C1 127.48(19) . . ? C3 Nd1 C1 48.74(18) . . ? Cl1 Nd1 C1 91.33(13) . . ? C4 Nd1 C1 49.43(16) . . ? C5 Nd1 C1 29.59(15) . . ? C2 Nd1 C1 29.41(17) . . ? C9 Nd1 C1 145.43(18) . . ? C8 Nd1 C1 174.78(18) . . ? C32 Al1 C30 121.1(10) . . ? C32 Al1 C31 115.4(12) . . ? C30 Al1 C31 111.0(8) . . ? C32 Al1 Cl1 101.9(4) . . ? C30 Al1 Cl1 104.5(3) . . ? C31 Al1 Cl1 99.1(4) . . ? Al1 Cl1 Nd1 143.36(10) . . ? C5 C1 C2 106.3(5) . . ? C5 C1 C11 119.3(6) . . ? C2 C1 C11 133.7(5) . . ? C5 C1 Nd1 70.3(3) . . ? C2 C1 Nd1 74.3(3) . . ? C11 C1 Nd1 127.0(4) . . ? C1 C2 C3 105.1(5) . . ? C1 C2 C21 134.2(6) . . ? C3 C2 C21 118.6(6) . . ? C1 C2 Nd1 76.2(3) . . ? C3 C2 Nd1 70.4(3) . . ? C21 C2 Nd1 129.5(4) . . ? C4 C3 C2 111.2(6) . . ? C4 C3 Nd1 75.4(3) . . ? C2 C3 Nd1 79.2(3) . . ? C3 C4 C5 106.3(5) . . ? C3 C4 C41 128.1(5) . . ? C5 C4 C41 125.6(5) . . ? C3 C4 Nd1 75.2(3) . . ? C5 C4 Nd1 75.5(3) . . ? C41 C4 Nd1 114.9(4) . . ? C4 C5 C1 111.0(5) . . ? C4 C5 Nd1 74.7(3) . . ? C1 C5 Nd1 80.1(3) . . ? C7 C6 C10 106.0(5) . . ? C7 C6 C61 126.4(6) . . ? C10 C6 C61 127.6(7) . . ? C7 C6 Nd1 75.7(3) . . ? C10 C6 Nd1 75.6(3) . . ? C61 C6 Nd1 111.9(4) . . ? C6 C7 C8 112.2(6) . . ? C6 C7 Nd1 74.6(3) . . ? C8 C7 Nd1 80.9(3) . . ? C7 C8 C9 105.6(6) . . ? C7 C8 C81 120.2(6) . . ? C9 C8 C81 133.7(6) . . ? C7 C8 Nd1 69.6(3) . . ? C9 C8 Nd1 74.8(3) . . ? C81 C8 Nd1 126.0(5) . . ? C8 C9 C10 106.0(5) . . ? C8 C9 C91 133.8(6) . . ? C10 C9 C91 117.9(6) . . ? C8 C9 Nd1 75.8(3) . . ? C10 C9 Nd1 70.0(3) . . ? C91 C9 Nd1 130.9(4) . . ? C6 C10 C9 110.1(6) . . ? C6 C10 Nd1 74.3(3) . . ? C9 C10 Nd1 79.9(4) . . ? C13 C11 C14 111.2(6) . . ? C13 C11 C1 115.8(5) . . ? C14 C11 C1 109.2(6) . . ? C13 C11 C12 104.6(6) . . ? C14 C11 C12 105.4(6) . . ? C1 C11 C12 110.1(5) . . ? C23 C21 C24 108.0(6) . . ? C23 C21 C2 111.1(6) . . ? C24 C21 C2 115.9(6) . . ? C23 C21 C22 108.0(7) . . ? C24 C21 C22 106.2(6) . . ? C2 C21 C22 107.3(5) . . ? C43 C41 C44 109.8(7) . . ? C43 C41 C42 106.7(6) . . ? C44 C41 C42 109.8(8) . . ? C43 C41 C4 112.6(6) . . ? C44 C41 C4 108.3(5) . . ? C42 C41 C4 109.7(6) . . ? C62 C61 C63 111.0(7) . . ? C62 C61 C6 110.9(6) . . ? C63 C61 C6 106.9(5) . . ? C62 C61 C64 108.6(7) . . ? C63 C61 C64 109.6(7) . . ? C6 C61 C64 109.8(6) . . ? C83 C81 C84 107.8(10) . . ? C83 C81 C8 116.7(6) . . ? C84 C81 C8 109.3(6) . . ? C83 C81 C82 111.1(8) . . ? C84 C81 C82 102.0(7) . . ? C8 C81 C82 108.9(7) . . ? C94 C91 C93 105.8(8) . . ? C94 C91 C92 108.2(8) . . ? C93 C91 C92 107.3(9) . . ? C94 C91 C9 116.3(8) . . ? C93 C91 C9 110.1(6) . . ? C92 C91 C9 108.7(6) . . ? _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 24.08 _diffrn_measured_fraction_theta_full 0.893 _refine_diff_density_max 0.579 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.066 #===end #12-Yb data_0534corr _database_code_depnum_ccdc_archive 'CCDC 604034' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H45 Cl2 O2 Yb' _chemical_formula_sum 'C25 H45 Cl2 O2 Yb' _chemical_formula_weight 621.55 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' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 '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 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.2826(8) _cell_length_b 11.7557(5) _cell_length_c 34.576(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.344(8) _cell_angle_gamma 90.00 _cell_volume 5354.6(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7997 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.05 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 3.711 _exptl_absorpt_correction_type numeric _exptl_absorpt_correction_T_min 0.3567 _exptl_absorpt_correction_T_max 0.4957 _exptl_absorpt_process_details DECAY _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 'Stoe IPDS' _diffrn_measurement_method \F-Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50981 _diffrn_reflns_av_R_equivalents 0.0908 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 28.07 _reflns_number_total 12895 _reflns_number_gt 10137 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS V2.63' _computing_cell_refinement 'Stoe IPDS V2.63' _computing_data_reduction 'Stoe IPDS V2.63' _computing_structure_solution 'SIR97 (Giacovazzo et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0445P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12895 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0825 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _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 C1 C -0.1738(3) 0.8356(3) 0.13803(12) 0.0212(7) Uani 1 1 d . . . C2 C -0.0908(3) 0.7781(3) 0.16101(11) 0.0218(7) Uani 1 1 d . . . C3 C -0.0348(3) 0.7237(3) 0.13345(12) 0.0223(7) Uani 1 1 d . . . H3 H 0.0252 0.6805 0.1403 0.027 Uiso 1 1 calc R . . C4 C -0.0796(3) 0.7420(3) 0.09534(12) 0.0244(8) Uani 1 1 d . . . C5 C -0.1651(3) 0.8124(3) 0.09811(12) 0.0240(8) Uani 1 1 d . . . H5 H -0.2099 0.8400 0.0766 0.029 Uiso 1 1 calc R . . C6 C 0.4003(3) 0.4830(3) 0.16412(11) 0.0195(7) Uani 1 1 d . . . C7 C 0.3174(3) 0.4220(3) 0.14268(11) 0.0208(7) Uani 1 1 d . . . C8 C 0.3196(3) 0.4474(3) 0.10228(11) 0.0202(7) Uani 1 1 d . . . H8 H 0.2735 0.4179 0.0814 0.024 Uiso 1 1 calc R . . C9 C 0.4004(3) 0.5225(3) 0.09792(12) 0.0217(7) Uani 1 1 d . . . C10 C 0.4499(3) 0.5404(3) 0.13570(11) 0.0208(7) Uani 1 1 d . . . H10 H 0.5093 0.5853 0.1416 0.025 Uiso 1 1 calc R . . C11 C -0.2704(3) 0.8970(3) 0.14769(13) 0.0278(8) Uani 1 1 d . . . C12 C -0.2630(3) 0.9596(4) 0.18658(15) 0.0341(10) Uani 1 1 d . . . H12A H -0.2527 0.9044 0.2080 0.051 Uiso 1 1 calc R . . H12B H -0.3260 1.0018 0.1881 0.051 Uiso 1 1 calc R . . H12C H -0.2057 1.0126 0.1887 0.051 Uiso 1 1 calc R . . C13 C -0.3058(4) 0.9868(4) 0.11586(15) 0.0402(11) Uani 1 1 d . . . H13A H -0.3669 1.0251 0.1224 0.060 Uiso 1 1 calc R . . H13B H -0.3209 0.9489 0.0905 0.060 Uiso 1 1 calc R . . H13C H -0.2518 1.0430 0.1146 0.060 Uiso 1 1 calc R . . C14 C -0.3557(4) 0.8078(4) 0.14682(19) 0.0472(13) Uani 1 1 d . . . H14A H -0.3396 0.7544 0.1685 0.071 Uiso 1 1 calc R . . H14B H -0.3616 0.7662 0.1221 0.071 Uiso 1 1 calc R . . H14C H -0.4200 0.8461 0.1493 0.071 Uiso 1 1 calc R . . C21 C -0.0666(3) 0.7544(3) 0.20506(12) 0.0283(8) Uani 1 1 d . . . C22 C -0.0404(4) 0.8597(4) 0.23039(13) 0.0334(9) Uani 1 1 d . . . H22A H -0.0316 0.8377 0.2580 0.050 Uiso 1 1 calc R . . H22B H -0.0955 0.9154 0.2256 0.050 Uiso 1 1 calc R . . H22C H 0.0228 0.8934 0.2238 0.050 Uiso 1 1 calc R . . C23 C 0.0239(4) 0.6740(4) 0.21295(13) 0.0391(11) Uani 1 1 d . . . H23A H 0.0847 0.7113 0.2056 0.059 Uiso 1 1 calc R . . H23B H 0.0103 0.6045 0.1975 0.059 Uiso 1 1 calc R . . H23C H 0.0348 0.6546 0.2407 0.059 Uiso 1 1 calc R . . C24 C -0.1568(4) 0.6911(4) 0.21901(14) 0.0376(11) Uani 1 1 d . . . H24A H -0.1738 0.6244 0.2024 0.056 Uiso 1 1 calc R . . H24B H -0.2156 0.7420 0.2174 0.056 Uiso 1 1 calc R . . H24C H -0.1384 0.6665 0.2461 0.056 Uiso 1 1 calc R . . C41 C -0.0571(4) 0.6773(3) 0.05918(13) 0.0309(9) Uani 1 1 d . . . C42 C 0.0575(4) 0.6556(4) 0.05956(15) 0.0406(11) Uani 1 1 d . . . H42A H 0.0931 0.7284 0.0590 0.061 Uiso 1 1 calc R . . H42B H 0.0686 0.6105 0.0366 0.061 Uiso 1 1 calc R . . H42C H 0.0836 0.6139 0.0833 0.061 Uiso 1 1 calc R . . C43 C -0.0940(4) 0.7405(5) 0.02177(14) 0.0437(12) Uani 1 1 d . . . H43A H -0.1677 0.7509 0.0197 0.066 Uiso 1 1 calc R . . H43B H -0.0773 0.6965 -0.0006 0.066 Uiso 1 1 calc R . . H43C H -0.0608 0.8150 0.0220 0.066 Uiso 1 1 calc R . . C44 C -0.1106(6) 0.5621(4) 0.0593(2) 0.0627(19) Uani 1 1 d . . . H44A H -0.0828 0.5190 0.0825 0.094 Uiso 1 1 calc R . . H44B H -0.0998 0.5194 0.0358 0.094 Uiso 1 1 calc R . . H44C H -0.1835 0.5740 0.0597 0.094 Uiso 1 1 calc R . . C61 C 0.4290(3) 0.5067(3) 0.20794(11) 0.0233(8) Uani 1 1 d . . . C62 C 0.5190(4) 0.5895(4) 0.21433(14) 0.0349(9) Uani 1 1 d . . . H62A H 0.5786 0.5545 0.2051 0.052 Uiso 1 1 calc R . . H62B H 0.5342 0.6070 0.2422 0.052 Uiso 1 1 calc R . . H62C H 0.5017 0.6598 0.1998 0.052 Uiso 1 1 calc R . . C63 C 0.4610(3) 0.4014(4) 0.23285(13) 0.0315(9) Uani 1 1 d . . . H63A H 0.5248 0.3712 0.2256 0.047 Uiso 1 1 calc R . . H63B H 0.4081 0.3431 0.2284 0.047 Uiso 1 1 calc R . . H63C H 0.4707 0.4226 0.2605 0.047 Uiso 1 1 calc R . . C64 C 0.3404(4) 0.5670(3) 0.22413(14) 0.0327(9) Uani 1 1 d . . . H64A H 0.3621 0.5912 0.2510 0.049 Uiso 1 1 calc R . . H64B H 0.2829 0.5145 0.2236 0.049 Uiso 1 1 calc R . . H64C H 0.3198 0.6337 0.2080 0.049 Uiso 1 1 calc R . . C71 C 0.2243(3) 0.3568(3) 0.15379(13) 0.0254(8) Uani 1 1 d . . . C72 C 0.1889(4) 0.2657(4) 0.12270(15) 0.0385(11) Uani 1 1 d . . . H72A H 0.2435 0.2103 0.1213 0.058 Uiso 1 1 calc R . . H72B H 0.1721 0.3024 0.0972 0.058 Uiso 1 1 calc R . . H72C H 0.1288 0.2267 0.1299 0.058 Uiso 1 1 calc R . . C73 C 0.2379(3) 0.2946(3) 0.19262(13) 0.0294(8) Uani 1 1 d . . . H73A H 0.1759 0.2522 0.1957 0.044 Uiso 1 1 calc R . . H73B H 0.2517 0.3498 0.2139 0.044 Uiso 1 1 calc R . . H73C H 0.2951 0.2415 0.1933 0.044 Uiso 1 1 calc R . . C74 C 0.1365(3) 0.4421(4) 0.15389(17) 0.0422(12) Uani 1 1 d . . . H74A H 0.0755 0.4020 0.1597 0.063 Uiso 1 1 calc R . . H74B H 0.1229 0.4784 0.1282 0.063 Uiso 1 1 calc R . . H74C H 0.1551 0.5003 0.1738 0.063 Uiso 1 1 calc R . . C91 C 0.4144(3) 0.5903(3) 0.06148(12) 0.0274(8) Uani 1 1 d . . . C92 C 0.3551(6) 0.5400(6) 0.02503(16) 0.0656(19) Uani 1 1 d . . . H92A H 0.3840 0.4660 0.0195 0.098 Uiso 1 1 calc R . . H92B H 0.3592 0.5913 0.0029 0.098 Uiso 1 1 calc R . . H92C H 0.2840 0.5304 0.0291 0.098 Uiso 1 1 calc R . . C93 C 0.5263(4) 0.6026(4) 0.05611(18) 0.0480(14) Uani 1 1 d . . . H93A H 0.5537 0.5281 0.0501 0.072 Uiso 1 1 calc R . . H93B H 0.5642 0.6324 0.0802 0.072 Uiso 1 1 calc R . . H93C H 0.5328 0.6553 0.0346 0.072 Uiso 1 1 calc R . . C94 C 0.3736(5) 0.7106(4) 0.06706(16) 0.0492(14) Uani 1 1 d . . . H94A H 0.3871 0.7587 0.0452 0.074 Uiso 1 1 calc R . . H94B H 0.4075 0.7427 0.0915 0.074 Uiso 1 1 calc R . . H94C H 0.3003 0.7070 0.0681 0.074 Uiso 1 1 calc R . . C100 C -0.0992(7) 1.1927(4) 0.0819(2) 0.074(2) Uani 1 1 d . . . H10A H -0.0287 1.2199 0.0889 0.089 Uiso 1 1 calc R . . H10B H -0.1392 1.2146 0.1030 0.089 Uiso 1 1 calc R . . C110 C -0.1442(4) 1.2446(4) 0.04426(15) 0.0380(11) Uani 1 1 d . . . H11A H -0.0906 1.2760 0.0299 0.046 Uiso 1 1 calc R . . H11B H -0.1921 1.3063 0.0488 0.046 Uiso 1 1 calc R . . C120 C -0.1989(4) 1.1474(4) 0.02199(14) 0.0365(10) Uani 1 1 d . . . H12D H -0.2008 1.1576 -0.0065 0.044 Uiso 1 1 calc R . . H12E H -0.2691 1.1393 0.0284 0.044 Uiso 1 1 calc R . . C130 C -0.1340(4) 1.0465(4) 0.03640(14) 0.0365(10) Uani 1 1 d . . . H13D H -0.1741 0.9753 0.0337 0.044 Uiso 1 1 calc R . . H13E H -0.0754 1.0387 0.0216 0.044 Uiso 1 1 calc R . . C140 C 0.2128(4) 0.8082(4) 0.14744(16) 0.0407(11) Uani 1 1 d . . . H14D H 0.2026 0.7978 0.1188 0.049 Uiso 1 1 calc R . . H14E H 0.2014 0.7345 0.1600 0.049 Uiso 1 1 calc R . . C150 C 0.3183(3) 0.8522(4) 0.16086(18) 0.0451(13) Uani 1 1 d . . . H15A H 0.3666 0.7890 0.1676 0.054 Uiso 1 1 calc R . . H15B H 0.3435 0.9004 0.1407 0.054 Uiso 1 1 calc R . . C160 C 0.3029(4) 0.9203(4) 0.19617(19) 0.0489(13) Uani 1 1 d . . . H16A H 0.3577 0.9769 0.2023 0.059 Uiso 1 1 calc R . . H16B H 0.2999 0.8706 0.2191 0.059 Uiso 1 1 calc R . . C170 C 0.2029(4) 0.9773(4) 0.18419(17) 0.0401(11) Uani 1 1 d . . . H17A H 0.1688 0.9954 0.2073 0.048 Uiso 1 1 calc R . . H17B H 0.2122 1.0485 0.1698 0.048 Uiso 1 1 calc R . . C180 C 0.7009(3) 0.4655(4) 0.14407(17) 0.0403(11) Uani 1 1 d . . . H18A H 0.6931 0.5371 0.1585 0.048 Uiso 1 1 calc R . . H18B H 0.6814 0.4798 0.1159 0.048 Uiso 1 1 calc R . . C190 C 0.8085(4) 0.4229(4) 0.15172(18) 0.0439(12) Uani 1 1 d . . . H19A H 0.8264 0.3768 0.1296 0.053 Uiso 1 1 calc R . . H19B H 0.8572 0.4865 0.1566 0.053 Uiso 1 1 calc R . . C200 C 0.8059(3) 0.3514(4) 0.18762(18) 0.0452(13) Uani 1 1 d . . . H20A H 0.8093 0.3993 0.2113 0.054 Uiso 1 1 calc R . . H20B H 0.8626 0.2962 0.1908 0.054 Uiso 1 1 calc R . . C210 C 0.7051(3) 0.2919(4) 0.17958(16) 0.0384(10) Uani 1 1 d . . . H21A H 0.7110 0.2223 0.1639 0.046 Uiso 1 1 calc R . . H21B H 0.6794 0.2707 0.2042 0.046 Uiso 1 1 calc R . . C220 C 0.4044(5) 0.0708(4) 0.08077(17) 0.0473(12) Uani 1 1 d . . . H22D H 0.4677 0.0508 0.0977 0.057 Uiso 1 1 calc R . . H22E H 0.3468 0.0321 0.0908 0.057 Uiso 1 1 calc R . . C230 C 0.4109(9) 0.0364(6) 0.0409(2) 0.100(3) Uani 1 1 d . . . H23D H 0.3661 -0.0298 0.0341 0.120 Uiso 1 1 calc R . . H23E H 0.4814 0.0140 0.0381 0.120 Uiso 1 1 calc R . . C240 C 0.3800(6) 0.1307(5) 0.01511(18) 0.0661(18) Uani 1 1 d . . . H24D H 0.3238 0.1080 -0.0050 0.079 Uiso 1 1 calc R . . H24E H 0.4375 0.1580 0.0020 0.079 Uiso 1 1 calc R . . C250 C 0.3464(5) 0.2199(5) 0.04097(16) 0.0618(18) Uani 1 1 d . . . H25A H 0.3701 0.2956 0.0334 0.074 Uiso 1 1 calc R . . H25B H 0.2713 0.2213 0.0389 0.074 Uiso 1 1 calc R . . Cl1 Cl -0.02198(7) 1.09845(8) 0.16862(3) 0.02776(19) Uani 1 1 d . . . Cl2 Cl 0.11243(8) 0.96799(10) 0.07016(3) 0.0357(2) Uani 1 1 d . . . Cl3 Cl 0.59693(9) 0.29808(10) 0.07000(4) 0.0394(3) Uani 1 1 d . . . Cl4 Cl 0.48129(8) 0.16334(8) 0.16978(3) 0.0292(2) Uani 1 1 d . . . Yb1 Yb -0.009031(11) 0.940583(12) 0.120522(5) 0.01903(5) Uani 1 1 d . . . Yb2 Yb 0.481503(11) 0.325302(12) 0.122284(5) 0.01942(5) Uani 1 1 d . . . O1 O -0.1001(2) 1.0710(2) 0.07734(9) 0.0276(6) Uani 1 1 d . . . O2 O 0.1438(2) 0.8948(2) 0.15911(9) 0.0281(6) Uani 1 1 d . . . O3 O 0.6377(2) 0.3749(2) 0.15782(10) 0.0294(6) Uani 1 1 d . . . O4 O 0.3894(2) 0.1928(2) 0.08017(9) 0.0306(6) 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 C1 0.0217(16) 0.0193(16) 0.0230(19) -0.0045(14) 0.0044(15) -0.0037(13) C2 0.0272(18) 0.0188(16) 0.0194(18) -0.0020(13) 0.0032(15) -0.0023(14) C3 0.0245(17) 0.0204(17) 0.0214(19) 0.0008(14) 0.0006(15) 0.0047(14) C4 0.0291(19) 0.0199(17) 0.025(2) -0.0047(15) 0.0062(17) 0.0010(15) C5 0.0286(18) 0.0216(17) 0.022(2) -0.0038(14) 0.0026(16) 0.0001(14) C6 0.0225(16) 0.0200(16) 0.0168(18) 0.0024(13) 0.0054(14) 0.0025(13) C7 0.0210(16) 0.0209(16) 0.0212(19) 0.0056(14) 0.0053(14) 0.0054(13) C8 0.0225(16) 0.0217(16) 0.0166(18) 0.0016(13) 0.0035(14) 0.0031(14) C9 0.0248(17) 0.0199(16) 0.0216(19) 0.0014(14) 0.0072(15) 0.0027(14) C10 0.0250(17) 0.0187(16) 0.0194(18) 0.0011(14) 0.0053(15) 0.0004(14) C11 0.0232(17) 0.0293(19) 0.032(2) -0.0036(17) 0.0096(16) -0.0004(16) C12 0.034(2) 0.031(2) 0.041(3) -0.0082(18) 0.017(2) 0.0042(17) C13 0.033(2) 0.051(3) 0.037(3) 0.004(2) 0.007(2) 0.016(2) C14 0.030(2) 0.048(3) 0.067(4) -0.013(3) 0.016(2) -0.012(2) C21 0.040(2) 0.0235(18) 0.023(2) 0.0006(15) 0.0101(18) 0.0010(17) C22 0.043(2) 0.032(2) 0.025(2) -0.0032(17) 0.0052(19) -0.0047(19) C23 0.055(3) 0.043(2) 0.019(2) 0.0045(18) 0.005(2) 0.017(2) C24 0.057(3) 0.030(2) 0.030(2) -0.0005(17) 0.019(2) -0.009(2) C41 0.043(2) 0.0261(19) 0.024(2) -0.0061(15) 0.0071(19) 0.0011(17) C42 0.051(3) 0.042(2) 0.030(2) -0.003(2) 0.010(2) 0.022(2) C43 0.054(3) 0.054(3) 0.022(2) -0.008(2) 0.002(2) 0.020(2) C44 0.099(5) 0.037(3) 0.058(4) -0.028(3) 0.035(4) -0.029(3) C61 0.0321(19) 0.0226(17) 0.0155(18) 0.0003(14) 0.0039(15) 0.0022(15) C62 0.045(2) 0.033(2) 0.027(2) -0.0026(18) 0.0038(19) -0.0080(19) C63 0.040(2) 0.030(2) 0.022(2) 0.0050(17) -0.0025(17) 0.0034(18) C64 0.046(2) 0.0266(19) 0.029(2) -0.0003(16) 0.017(2) 0.0059(18) C71 0.0201(16) 0.0288(18) 0.029(2) 0.0041(16) 0.0084(16) 0.0018(15) C72 0.034(2) 0.049(3) 0.033(3) 0.000(2) 0.008(2) -0.017(2) C73 0.034(2) 0.0270(18) 0.029(2) 0.0049(17) 0.0107(18) -0.0038(17) C74 0.027(2) 0.048(3) 0.054(3) 0.019(2) 0.016(2) 0.009(2) C91 0.039(2) 0.0274(18) 0.0182(19) 0.0069(15) 0.0106(17) 0.0030(17) C92 0.107(5) 0.069(4) 0.019(2) 0.010(2) 0.001(3) -0.036(4) C93 0.049(3) 0.046(3) 0.055(3) 0.024(2) 0.031(3) 0.007(2) C94 0.072(4) 0.037(2) 0.042(3) 0.021(2) 0.024(3) 0.025(3) C100 0.129(6) 0.021(2) 0.060(4) 0.003(2) -0.035(4) -0.002(3) C110 0.043(2) 0.031(2) 0.041(3) 0.0098(19) 0.009(2) 0.0054(19) C120 0.042(2) 0.037(2) 0.030(2) 0.0043(18) 0.003(2) 0.0136(19) C130 0.052(3) 0.033(2) 0.024(2) -0.0003(18) -0.001(2) 0.012(2) C140 0.035(2) 0.043(2) 0.043(3) -0.004(2) 0.002(2) 0.017(2) C150 0.025(2) 0.049(3) 0.063(4) 0.024(3) 0.010(2) 0.008(2) C160 0.031(2) 0.048(3) 0.062(4) 0.010(3) -0.017(2) -0.006(2) C170 0.034(2) 0.037(2) 0.046(3) -0.006(2) -0.006(2) -0.0021(19) C180 0.032(2) 0.036(2) 0.052(3) 0.002(2) 0.004(2) -0.0101(19) C190 0.031(2) 0.040(2) 0.063(4) -0.016(2) 0.018(2) -0.0051(19) C200 0.024(2) 0.043(2) 0.064(4) -0.013(3) -0.010(2) 0.0059(19) C210 0.029(2) 0.032(2) 0.052(3) 0.004(2) -0.004(2) 0.0059(18) C220 0.062(3) 0.032(2) 0.044(3) -0.006(2) -0.006(3) 0.000(2) C230 0.217(11) 0.043(3) 0.040(4) -0.016(3) 0.019(5) 0.003(5) C240 0.111(5) 0.051(3) 0.034(3) -0.014(3) -0.002(3) 0.013(3) C250 0.087(4) 0.063(3) 0.027(3) -0.017(3) -0.028(3) 0.034(3) Cl1 0.0333(5) 0.0242(4) 0.0266(5) -0.0054(4) 0.0070(4) -0.0011(4) Cl2 0.0312(5) 0.0452(6) 0.0334(6) 0.0025(5) 0.0143(4) 0.0025(4) Cl3 0.0426(6) 0.0397(5) 0.0406(6) -0.0031(5) 0.0241(5) 0.0003(5) Cl4 0.0348(5) 0.0245(4) 0.0285(5) 0.0067(4) 0.0046(4) 0.0017(4) Yb1 0.01966(8) 0.01832(8) 0.01940(8) -0.00113(6) 0.00362(6) 0.00112(6) Yb2 0.01981(8) 0.01932(8) 0.01957(8) 0.00103(6) 0.00429(6) 0.00238(5) O1 0.0349(14) 0.0222(13) 0.0259(15) 0.0013(11) 0.0042(13) 0.0065(11) O2 0.0254(13) 0.0298(14) 0.0281(16) -0.0059(12) -0.0012(12) 0.0051(11) O3 0.0225(13) 0.0265(13) 0.0374(18) 0.0023(12) -0.0025(12) -0.0018(11) O4 0.0324(14) 0.0329(15) 0.0250(16) -0.0065(12) -0.0022(13) 0.0046(12) _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 C1 C5 1.426(5) . ? C1 C2 1.442(6) . ? C1 C11 1.545(5) . ? C1 Yb1 2.649(3) . ? C2 C3 1.432(5) . ? C2 C21 1.541(6) . ? C2 Yb1 2.679(4) . ? C3 C4 1.392(6) . ? C3 Yb1 2.619(4) . ? C3 H3 0.9500 . ? C4 C5 1.418(5) . ? C4 C41 1.525(5) . ? C4 Yb1 2.623(4) . ? C5 Yb1 2.599(4) . ? C5 H5 0.9500 . ? C6 C10 1.421(5) . ? C6 C7 1.438(5) . ? C6 C61 1.540(5) . ? C6 Yb2 2.663(3) . ? C7 C8 1.432(5) . ? C7 C71 1.545(5) . ? C7 Yb2 2.633(3) . ? C8 C9 1.413(5) . ? C8 Yb2 2.604(4) . ? C8 H8 0.9500 . ? C9 C10 1.401(6) . ? C9 C91 1.522(5) . ? C9 Yb2 2.648(4) . ? C10 Yb2 2.614(3) . ? C10 H10 0.9500 . ? C11 C12 1.525(6) . ? C11 C14 1.541(6) . ? C11 C13 1.554(7) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C21 C23 1.525(6) . ? C21 C22 1.531(6) . ? C21 C24 1.539(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C41 C43 1.518(7) . ? C41 C44 1.530(6) . ? C41 C42 1.542(6) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C61 C62 1.536(6) . ? C61 C63 1.537(5) . ? C61 C64 1.539(5) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C71 C73 1.519(6) . ? C71 C74 1.539(6) . ? C71 C72 1.547(6) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C91 C92 1.517(7) . ? C91 C93 1.529(6) . ? C91 C94 1.535(6) . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? C100 O1 1.439(5) . ? C100 C110 1.492(8) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? C110 C120 1.512(7) . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C120 C130 1.513(6) . ? C120 H12D 0.9900 . ? C120 H12E 0.9900 . ? C130 O1 1.458(5) . ? C130 H13D 0.9900 . ? C130 H13E 0.9900 . ? C140 O2 1.461(5) . ? C140 C150 1.510(7) . ? C140 H14D 0.9900 . ? C140 H14E 0.9900 . ? C150 C160 1.496(8) . ? C150 H15A 0.9900 . ? C150 H15B 0.9900 . ? C160 C170 1.497(7) . ? C160 H16A 0.9900 . ? C160 H16B 0.9900 . ? C170 O2 1.462(6) . ? C170 H17A 0.9900 . ? C170 H17B 0.9900 . ? C180 O3 1.473(5) . ? C180 C190 1.505(7) . ? C180 H18A 0.9900 . ? C180 H18B 0.9900 . ? C190 C200 1.503(8) . ? C190 H19A 0.9900 . ? C190 H19B 0.9900 . ? C200 C210 1.505(6) . ? C200 H20A 0.9900 . ? C200 H20B 0.9900 . ? C210 O3 1.466(5) . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C220 C230 1.448(8) . ? C220 O4 1.449(5) . ? C220 H22D 0.9900 . ? C220 H22E 0.9900 . ? C230 C240 1.449(10) . ? C230 H23D 0.9900 . ? C230 H23E 0.9900 . ? C240 C250 1.484(7) . ? C240 H24D 0.9900 . ? C240 H24E 0.9900 . ? C250 O4 1.437(6) . ? C250 H25A 0.9900 . ? C250 H25B 0.9900 . ? Cl1 Yb1 2.5124(9) . ? Cl2 Yb1 2.5409(10) . ? Cl3 Yb2 2.5356(10) . ? Cl4 Yb2 2.5147(9) . ? Yb1 O2 2.344(3) . ? Yb1 O1 2.362(3) . ? Yb2 O3 2.345(3) . ? Yb2 O4 2.364(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C2 107.0(3) . . ? C5 C1 C11 118.1(4) . . ? C2 C1 C11 134.2(4) . . ? C5 C1 Yb1 72.3(2) . . ? C2 C1 Yb1 75.4(2) . . ? C11 C1 Yb1 124.4(2) . . ? C3 C2 C1 105.5(3) . . ? C3 C2 C21 121.1(3) . . ? C1 C2 C21 132.7(3) . . ? C3 C2 Yb1 72.0(2) . . ? C1 C2 Yb1 73.2(2) . . ? C21 C2 Yb1 126.8(2) . . ? C4 C3 C2 111.5(3) . . ? C4 C3 Yb1 74.8(2) . . ? C2 C3 Yb1 76.6(2) . . ? C4 C3 H3 124.3 . . ? C2 C3 H3 124.3 . . ? Yb1 C3 H3 116.0 . . ? C3 C4 C5 106.0(3) . . ? C3 C4 C41 126.5(4) . . ? C5 C4 C41 126.1(4) . . ? C3 C4 Yb1 74.5(2) . . ? C5 C4 Yb1 73.3(2) . . ? C41 C4 Yb1 128.1(3) . . ? C4 C5 C1 110.0(4) . . ? C4 C5 Yb1 75.2(2) . . ? C1 C5 Yb1 76.2(2) . . ? C4 C5 H5 125.0 . . ? C1 C5 H5 125.0 . . ? Yb1 C5 H5 115.6 . . ? C10 C6 C7 105.8(3) . . ? C10 C6 C61 121.1(3) . . ? C7 C6 C61 132.4(3) . . ? C10 C6 Yb2 72.50(19) . . ? C7 C6 Yb2 73.12(19) . . ? C61 C6 Yb2 126.4(2) . . ? C8 C7 C6 106.8(3) . . ? C8 C7 C71 117.6(3) . . ? C6 C7 C71 134.8(3) . . ? C8 C7 Yb2 73.00(19) . . ? C6 C7 Yb2 75.38(19) . . ? C71 C7 Yb2 124.6(2) . . ? C9 C8 C7 110.2(3) . . ? C9 C8 Yb2 76.1(2) . . ? C7 C8 Yb2 75.3(2) . . ? C9 C8 H8 124.9 . . ? C7 C8 H8 124.9 . . ? Yb2 C8 H8 115.6 . . ? C10 C9 C8 105.5(3) . . ? C10 C9 C91 127.0(3) . . ? C8 C9 C91 126.2(4) . . ? C10 C9 Yb2 73.2(2) . . ? C8 C9 Yb2 72.7(2) . . ? C91 C9 Yb2 129.3(2) . . ? C9 C10 C6 111.7(3) . . ? C9 C10 Yb2 75.9(2) . . ? C6 C10 Yb2 76.3(2) . . ? C9 C10 H10 124.1 . . ? C6 C10 H10 124.1 . . ? Yb2 C10 H10 115.4 . . ? C12 C11 C14 108.0(4) . . ? C12 C11 C1 117.0(4) . . ? C14 C11 C1 107.9(3) . . ? C12 C11 C13 106.0(4) . . ? C14 C11 C13 107.0(4) . . ? C1 C11 C13 110.4(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C23 C21 C22 106.4(4) . . ? C23 C21 C24 105.8(4) . . ? C22 C21 C24 109.9(3) . . ? C23 C21 C2 110.4(3) . . ? C22 C21 C2 115.0(3) . . ? C24 C21 C2 109.0(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C43 C41 C4 112.2(3) . . ? C43 C41 C44 109.7(5) . . ? C4 C41 C44 107.4(4) . . ? C43 C41 C42 107.4(4) . . ? C4 C41 C42 111.9(4) . . ? C44 C41 C42 108.1(4) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C62 C61 C63 106.0(4) . . ? C62 C61 C64 105.8(3) . . ? C63 C61 C64 109.7(3) . . ? C62 C61 C6 110.2(3) . . ? C63 C61 C6 115.0(3) . . ? C64 C61 C6 109.7(3) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C73 C71 C74 108.4(3) . . ? C73 C71 C7 116.7(3) . . ? C74 C71 C7 107.9(3) . . ? C73 C71 C72 105.8(3) . . ? C74 C71 C72 106.9(4) . . ? C7 C71 C72 110.7(3) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C71 C73 H73A 109.5 . . ? C71 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C71 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C71 C74 H74A 109.5 . . ? C71 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C71 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C92 C91 C9 112.3(4) . . ? C92 C91 C93 110.2(4) . . ? C9 C91 C93 111.9(4) . . ? C92 C91 C94 108.0(5) . . ? C9 C91 C94 107.2(3) . . ? C93 C91 C94 107.0(4) . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C91 C93 H93A 109.5 . . ? C91 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C91 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C91 C94 H94A 109.5 . . ? C91 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C91 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? O1 C100 C110 108.3(5) . . ? O1 C100 H10A 110.0 . . ? C110 C100 H10A 110.0 . . ? O1 C100 H10B 110.0 . . ? C110 C100 H10B 110.0 . . ? H10A C100 H10B 108.4 . . ? C100 C110 C120 104.3(4) . . ? C100 C110 H11A 110.9 . . ? C120 C110 H11A 110.9 . . ? C100 C110 H11B 110.9 . . ? C120 C110 H11B 110.9 . . ? H11A C110 H11B 108.9 . . ? C110 C120 C130 102.0(4) . . ? C110 C120 H12D 111.4 . . ? C130 C120 H12D 111.4 . . ? C110 C120 H12E 111.4 . . ? C130 C120 H12E 111.4 . . ? H12D C120 H12E 109.2 . . ? O1 C130 C120 104.9(3) . . ? O1 C130 H13D 110.8 . . ? C120 C130 H13D 110.8 . . ? O1 C130 H13E 110.8 . . ? C120 C130 H13E 110.8 . . ? H13D C130 H13E 108.8 . . ? O2 C140 C150 105.5(4) . . ? O2 C140 H14D 110.6 . . ? C150 C140 H14D 110.6 . . ? O2 C140 H14E 110.6 . . ? C150 C140 H14E 110.6 . . ? H14D C140 H14E 108.8 . . ? C160 C150 C140 102.4(4) . . ? C160 C150 H15A 111.3 . . ? C140 C150 H15A 111.3 . . ? C160 C150 H15B 111.3 . . ? C140 C150 H15B 111.3 . . ? H15A C150 H15B 109.2 . . ? C150 C160 C170 102.9(4) . . ? C150 C160 H16A 111.2 . . ? C170 C160 H16A 111.2 . . ? C150 C160 H16B 111.2 . . ? C170 C160 H16B 111.2 . . ? H16A C160 H16B 109.1 . . ? O2 C170 C160 104.9(4) . . ? O2 C170 H17A 110.8 . . ? C160 C170 H17A 110.8 . . ? O2 C170 H17B 110.8 . . ? C160 C170 H17B 110.8 . . ? H17A C170 H17B 108.8 . . ? O3 C180 C190 105.7(4) . . ? O3 C180 H18A 110.6 . . ? C190 C180 H18A 110.6 . . ? O3 C180 H18B 110.6 . . ? C190 C180 H18B 110.6 . . ? H18A C180 H18B 108.7 . . ? C200 C190 C180 102.1(4) . . ? C200 C190 H19A 111.3 . . ? C180 C190 H19A 111.3 . . ? C200 C190 H19B 111.3 . . ? C180 C190 H19B 111.3 . . ? H19A C190 H19B 109.2 . . ? C190 C200 C210 102.7(4) . . ? C190 C200 H20A 111.2 . . ? C210 C200 H20A 111.2 . . ? C190 C200 H20B 111.2 . . ? C210 C200 H20B 111.2 . . ? H20A C200 H20B 109.1 . . ? O3 C210 C200 104.9(4) . . ? O3 C210 H21A 110.8 . . ? C200 C210 H21A 110.8 . . ? O3 C210 H21B 110.8 . . ? C200 C210 H21B 110.8 . . ? H21A C210 H21B 108.8 . . ? C230 C220 O4 106.7(5) . . ? C230 C220 H22D 110.4 . . ? O4 C220 H22D 110.4 . . ? C230 C220 H22E 110.4 . . ? O4 C220 H22E 110.4 . . ? H22D C220 H22E 108.6 . . ? C220 C230 C240 109.1(5) . . ? C220 C230 H23D 109.9 . . ? C240 C230 H23D 109.9 . . ? C220 C230 H23E 109.9 . . ? C240 C230 H23E 109.9 . . ? H23D C230 H23E 108.3 . . ? C230 C240 C250 104.6(5) . . ? C230 C240 H24D 110.8 . . ? C250 C240 H24D 110.8 . . ? C230 C240 H24E 110.8 . . ? C250 C240 H24E 110.8 . . ? H24D C240 H24E 108.9 . . ? O4 C250 C240 107.3(4) . . ? O4 C250 H25A 110.3 . . ? C240 C250 H25A 110.3 . . ? O4 C250 H25B 110.3 . . ? C240 C250 H25B 110.3 . . ? H25A C250 H25B 108.5 . . ? O2 Yb1 O1 147.65(10) . . ? O2 Yb1 Cl1 85.44(7) . . ? O1 Yb1 Cl1 82.32(7) . . ? O2 Yb1 Cl2 80.78(8) . . ? O1 Yb1 Cl2 78.65(7) . . ? Cl1 Yb1 Cl2 117.59(3) . . ? O2 Yb1 C5 129.48(11) . . ? O1 Yb1 C5 82.15(12) . . ? Cl1 Yb1 C5 120.41(8) . . ? Cl2 Yb1 C5 114.90(9) . . ? O2 Yb1 C3 78.58(11) . . ? O1 Yb1 C3 132.22(11) . . ? Cl1 Yb1 C3 125.78(9) . . ? Cl2 Yb1 C3 110.42(8) . . ? C5 Yb1 C3 50.92(12) . . ? O2 Yb1 C4 103.37(11) . . ? O1 Yb1 C4 103.60(12) . . ? Cl1 Yb1 C4 145.63(8) . . ? Cl2 Yb1 C4 96.71(9) . . ? C5 Yb1 C4 31.50(11) . . ? C3 Yb1 C4 30.79(12) . . ? O2 Yb1 C1 116.31(11) . . ? O1 Yb1 C1 94.34(11) . . ? Cl1 Yb1 C1 93.70(8) . . ? Cl2 Yb1 C1 146.21(9) . . ? C5 Yb1 C1 31.52(11) . . ? C3 Yb1 C1 51.48(11) . . ? C4 Yb1 C1 52.44(11) . . ? O2 Yb1 C2 85.30(11) . . ? O1 Yb1 C2 125.73(11) . . ? Cl1 Yb1 C2 96.55(8) . . ? Cl2 Yb1 C2 141.61(8) . . ? C5 Yb1 C2 51.79(12) . . ? C3 Yb1 C2 31.34(11) . . ? C4 Yb1 C2 52.21(12) . . ? C1 Yb1 C2 31.40(12) . . ? O3 Yb2 O4 147.15(10) . . ? O3 Yb2 Cl4 85.45(8) . . ? O4 Yb2 Cl4 81.95(8) . . ? O3 Yb2 Cl3 80.21(8) . . ? O4 Yb2 Cl3 77.90(8) . . ? Cl4 Yb2 Cl3 114.92(4) . . ? O3 Yb2 C8 130.33(11) . . ? O4 Yb2 C8 81.63(11) . . ? Cl4 Yb2 C8 121.40(8) . . ? Cl3 Yb2 C8 115.73(8) . . ? O3 Yb2 C10 79.51(11) . . ? O4 Yb2 C10 131.62(11) . . ? Cl4 Yb2 C10 127.07(8) . . ? Cl3 Yb2 C10 111.96(8) . . ? C8 Yb2 C10 50.82(12) . . ? O3 Yb2 C7 117.34(11) . . ? O4 Yb2 C7 93.92(11) . . ? Cl4 Yb2 C7 94.70(8) . . ? Cl3 Yb2 C7 147.36(9) . . ? C8 Yb2 C7 31.74(11) . . ? C10 Yb2 C7 51.51(11) . . ? O3 Yb2 C9 104.22(11) . . ? O4 Yb2 C9 102.90(11) . . ? Cl4 Yb2 C9 146.75(8) . . ? Cl3 Yb2 C9 98.17(8) . . ? C8 Yb2 C9 31.19(11) . . ? C10 Yb2 C9 30.87(12) . . ? C7 Yb2 C9 52.42(11) . . ? O3 Yb2 C6 86.26(11) . . ? O4 Yb2 C6 125.42(11) . . ? Cl4 Yb2 C6 97.94(8) . . ? Cl3 Yb2 C6 143.02(8) . . ? C8 Yb2 C6 51.88(12) . . ? C10 Yb2 C6 31.22(10) . . ? C7 Yb2 C6 31.50(12) . . ? C9 Yb2 C6 52.17(11) . . ? C100 O1 C130 107.5(4) . . ? C100 O1 Yb1 125.4(3) . . ? C130 O1 Yb1 123.7(2) . . ? C140 O2 C170 108.5(3) . . ? C140 O2 Yb1 122.1(3) . . ? C170 O2 Yb1 123.1(2) . . ? C210 O3 C180 108.1(3) . . ? C210 O3 Yb2 123.1(2) . . ? C180 O3 Yb2 120.9(3) . . ? C250 O4 C220 105.7(4) . . ? C250 O4 Yb2 123.2(3) . . ? C220 O4 Yb2 125.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 0.7(4) . . . . ? C11 C1 C2 C3 170.6(4) . . . . ? Yb1 C1 C2 C3 -65.2(2) . . . . ? C5 C1 C2 C21 -169.2(4) . . . . ? C11 C1 C2 C21 0.7(7) . . . . ? Yb1 C1 C2 C21 124.8(4) . . . . ? C5 C1 C2 Yb1 65.9(2) . . . . ? C11 C1 C2 Yb1 -124.1(4) . . . . ? C1 C2 C3 C4 -1.4(4) . . . . ? C21 C2 C3 C4 169.9(3) . . . . ? Yb1 C2 C3 C4 -67.4(3) . . . . ? C1 C2 C3 Yb1 66.0(2) . . . . ? C21 C2 C3 Yb1 -122.6(3) . . . . ? C2 C3 C4 C5 1.5(4) . . . . ? Yb1 C3 C4 C5 -67.1(3) . . . . ? C2 C3 C4 C41 -165.2(4) . . . . ? Yb1 C3 C4 C41 126.2(4) . . . . ? C2 C3 C4 Yb1 68.6(3) . . . . ? C3 C4 C5 C1 -1.1(4) . . . . ? C41 C4 C5 C1 165.8(4) . . . . ? Yb1 C4 C5 C1 -68.9(3) . . . . ? C3 C4 C5 Yb1 67.9(3) . . . . ? C41 C4 C5 Yb1 -125.3(4) . . . . ? C2 C1 C5 C4 0.2(4) . . . . ? C11 C1 C5 C4 -171.6(3) . . . . ? Yb1 C1 C5 C4 68.3(3) . . . . ? C2 C1 C5 Yb1 -68.1(2) . . . . ? C11 C1 C5 Yb1 120.1(3) . . . . ? C10 C6 C7 C8 -1.1(4) . . . . ? C61 C6 C7 C8 168.9(3) . . . . ? Yb2 C6 C7 C8 -66.8(2) . . . . ? C10 C6 C7 C71 -169.7(4) . . . . ? C61 C6 C7 C71 0.4(7) . . . . ? Yb2 C6 C7 C71 124.6(4) . . . . ? C10 C6 C7 Yb2 65.6(2) . . . . ? C61 C6 C7 Yb2 -124.3(4) . . . . ? C6 C7 C8 C9 -0.5(4) . . . . ? C71 C7 C8 C9 170.4(3) . . . . ? Yb2 C7 C8 C9 -68.9(3) . . . . ? C6 C7 C8 Yb2 68.4(2) . . . . ? C71 C7 C8 Yb2 -120.7(3) . . . . ? C7 C8 C9 C10 1.9(4) . . . . ? Yb2 C8 C9 C10 -66.4(2) . . . . ? C7 C8 C9 C91 -165.2(3) . . . . ? Yb2 C8 C9 C91 126.5(4) . . . . ? C7 C8 C9 Yb2 68.3(2) . . . . ? C8 C9 C10 C6 -2.7(4) . . . . ? C91 C9 C10 C6 164.3(3) . . . . ? Yb2 C9 C10 C6 -68.7(3) . . . . ? C8 C9 C10 Yb2 66.0(2) . . . . ? C91 C9 C10 Yb2 -127.0(4) . . . . ? C7 C6 C10 C9 2.4(4) . . . . ? C61 C6 C10 C9 -169.0(3) . . . . ? Yb2 C6 C10 C9 68.5(3) . . . . ? C7 C6 C10 Yb2 -66.1(2) . . . . ? C61 C6 C10 Yb2 122.5(3) . . . . ? C5 C1 C11 C12 -157.8(4) . . . . ? C2 C1 C11 C12 33.1(6) . . . . ? Yb1 C1 C11 C12 -70.8(4) . . . . ? C5 C1 C11 C14 80.2(5) . . . . ? C2 C1 C11 C14 -88.9(5) . . . . ? Yb1 C1 C11 C14 167.2(3) . . . . ? C5 C1 C11 C13 -36.5(5) . . . . ? C2 C1 C11 C13 154.5(4) . . . . ? Yb1 C1 C11 C13 50.6(5) . . . . ? C3 C2 C21 C23 2.8(5) . . . . ? C1 C2 C21 C23 171.5(4) . . . . ? Yb1 C2 C21 C23 -87.2(4) . . . . ? C3 C2 C21 C22 123.2(4) . . . . ? C1 C2 C21 C22 -68.2(5) . . . . ? Yb1 C2 C21 C22 33.1(5) . . . . ? C3 C2 C21 C24 -112.9(4) . . . . ? C1 C2 C21 C24 55.7(5) . . . . ? Yb1 C2 C21 C24 157.0(3) . . . . ? C3 C4 C41 C43 -162.6(4) . . . . ? C5 C4 C41 C43 33.2(6) . . . . ? Yb1 C4 C41 C43 -63.7(5) . . . . ? C3 C4 C41 C44 76.8(6) . . . . ? C5 C4 C41 C44 -87.4(5) . . . . ? Yb1 C4 C41 C44 175.7(4) . . . . ? C3 C4 C41 C42 -41.7(5) . . . . ? C5 C4 C41 C42 154.1(4) . . . . ? Yb1 C4 C41 C42 57.2(5) . . . . ? C10 C6 C61 C62 -4.2(5) . . . . ? C7 C6 C61 C62 -173.0(4) . . . . ? Yb2 C6 C61 C62 86.4(3) . . . . ? C10 C6 C61 C63 -123.8(4) . . . . ? C7 C6 C61 C63 67.3(5) . . . . ? Yb2 C6 C61 C63 -33.3(4) . . . . ? C10 C6 C61 C64 112.0(4) . . . . ? C7 C6 C61 C64 -56.8(5) . . . . ? Yb2 C6 C61 C64 -157.5(2) . . . . ? C8 C7 C71 C73 158.9(3) . . . . ? C6 C7 C71 C73 -33.4(6) . . . . ? Yb2 C7 C71 C73 71.3(4) . . . . ? C8 C7 C71 C74 -78.7(4) . . . . ? C6 C7 C71 C74 89.0(5) . . . . ? Yb2 C7 C71 C74 -166.4(3) . . . . ? C8 C7 C71 C72 37.9(5) . . . . ? C6 C7 C71 C72 -154.4(4) . . . . ? Yb2 C7 C71 C72 -49.8(4) . . . . ? C10 C9 C91 C92 174.8(5) . . . . ? C8 C9 C91 C92 -20.8(6) . . . . ? Yb2 C9 C91 C92 76.2(5) . . . . ? C10 C9 C91 C93 50.3(5) . . . . ? C8 C9 C91 C93 -145.3(4) . . . . ? Yb2 C9 C91 C93 -48.3(5) . . . . ? C10 C9 C91 C94 -66.7(5) . . . . ? C8 C9 C91 C94 97.7(5) . . . . ? Yb2 C9 C91 C94 -165.3(3) . . . . ? O1 C100 C110 C120 16.4(7) . . . . ? C100 C110 C120 C130 -31.5(6) . . . . ? C110 C120 C130 O1 35.8(4) . . . . ? O2 C140 C150 C160 30.3(5) . . . . ? C140 C150 C160 C170 -39.5(5) . . . . ? C150 C160 C170 O2 34.4(5) . . . . ? O3 C180 C190 C200 -31.6(5) . . . . ? C180 C190 C200 C210 40.4(5) . . . . ? C190 C200 C210 O3 -34.6(5) . . . . ? O4 C220 C230 C240 -11.4(10) . . . . ? C220 C230 C240 C250 -4.6(10) . . . . ? C230 C240 C250 O4 19.2(9) . . . . ? C4 C5 Yb1 O2 -39.6(3) . . . . ? C1 C5 Yb1 O2 75.8(2) . . . . ? C4 C5 Yb1 O1 132.8(2) . . . . ? C1 C5 Yb1 O1 -111.8(2) . . . . ? C4 C5 Yb1 Cl1 -150.9(2) . . . . ? C1 C5 Yb1 Cl1 -35.5(2) . . . . ? C4 C5 Yb1 Cl2 59.3(2) . . . . ? C1 C5 Yb1 Cl2 174.66(19) . . . . ? C4 C5 Yb1 C3 -37.6(2) . . . . ? C1 C5 Yb1 C3 77.9(2) . . . . ? C1 C5 Yb1 C4 115.4(3) . . . . ? C4 C5 Yb1 C1 -115.4(3) . . . . ? C4 C5 Yb1 C2 -78.0(2) . . . . ? C1 C5 Yb1 C2 37.4(2) . . . . ? C4 C3 Yb1 O2 -143.1(2) . . . . ? C2 C3 Yb1 O2 99.8(2) . . . . ? C4 C3 Yb1 O1 25.5(3) . . . . ? C2 C3 Yb1 O1 -91.5(3) . . . . ? C4 C3 Yb1 Cl1 141.09(19) . . . . ? C2 C3 Yb1 Cl1 24.1(3) . . . . ? C4 C3 Yb1 Cl2 -67.6(2) . . . . ? C2 C3 Yb1 Cl2 175.4(2) . . . . ? C4 C3 Yb1 C5 38.5(2) . . . . ? C2 C3 Yb1 C5 -78.6(2) . . . . ? C2 C3 Yb1 C4 -117.0(3) . . . . ? C4 C3 Yb1 C1 79.3(2) . . . . ? C2 C3 Yb1 C1 -37.8(2) . . . . ? C4 C3 Yb1 C2 117.0(3) . . . . ? C3 C4 Yb1 O2 37.2(2) . . . . ? C5 C4 Yb1 O2 149.6(2) . . . . ? C41 C4 Yb1 O2 -87.2(4) . . . . ? C3 C4 Yb1 O1 -160.8(2) . . . . ? C5 C4 Yb1 O1 -48.4(2) . . . . ? C41 C4 Yb1 O1 74.7(4) . . . . ? C3 C4 Yb1 Cl1 -64.5(3) . . . . ? C5 C4 Yb1 Cl1 47.9(3) . . . . ? C41 C4 Yb1 Cl1 171.1(3) . . . . ? C3 C4 Yb1 Cl2 119.3(2) . . . . ? C5 C4 Yb1 Cl2 -128.3(2) . . . . ? C41 C4 Yb1 Cl2 -5.2(4) . . . . ? C3 C4 Yb1 C5 -112.4(3) . . . . ? C41 C4 Yb1 C5 123.1(5) . . . . ? C5 C4 Yb1 C3 112.4(3) . . . . ? C41 C4 Yb1 C3 -124.4(5) . . . . ? C3 C4 Yb1 C1 -75.9(2) . . . . ? C5 C4 Yb1 C1 36.6(2) . . . . ? C41 C4 Yb1 C1 159.7(4) . . . . ? C3 C4 Yb1 C2 -35.9(2) . . . . ? C5 C4 Yb1 C2 76.5(2) . . . . ? C41 C4 Yb1 C2 -160.3(4) . . . . ? C5 C1 Yb1 O2 -123.4(2) . . . . ? C2 C1 Yb1 O2 -9.8(2) . . . . ? C11 C1 Yb1 O2 124.2(3) . . . . ? C5 C1 Yb1 O1 67.3(2) . . . . ? C2 C1 Yb1 O1 -179.1(2) . . . . ? C11 C1 Yb1 O1 -45.1(3) . . . . ? C5 C1 Yb1 Cl1 149.9(2) . . . . ? C2 C1 Yb1 Cl1 -96.5(2) . . . . ? C11 C1 Yb1 Cl1 37.5(3) . . . . ? C5 C1 Yb1 Cl2 -8.7(3) . . . . ? C2 C1 Yb1 Cl2 104.9(2) . . . . ? C11 C1 Yb1 Cl2 -121.1(3) . . . . ? C2 C1 Yb1 C5 113.6(3) . . . . ? C11 C1 Yb1 C5 -112.4(4) . . . . ? C5 C1 Yb1 C3 -75.9(2) . . . . ? C2 C1 Yb1 C3 37.7(2) . . . . ? C11 C1 Yb1 C3 171.7(4) . . . . ? C5 C1 Yb1 C4 -36.5(2) . . . . ? C2 C1 Yb1 C4 77.1(2) . . . . ? C11 C1 Yb1 C4 -148.9(4) . . . . ? C5 C1 Yb1 C2 -113.6(3) . . . . ? C11 C1 Yb1 C2 134.0(4) . . . . ? C3 C2 Yb1 O2 -75.7(2) . . . . ? C1 C2 Yb1 O2 171.2(2) . . . . ? C21 C2 Yb1 O2 40.1(3) . . . . ? C3 C2 Yb1 O1 114.2(2) . . . . ? C1 C2 Yb1 O1 1.1(3) . . . . ? C21 C2 Yb1 O1 -130.0(3) . . . . ? C3 C2 Yb1 Cl1 -160.5(2) . . . . ? C1 C2 Yb1 Cl1 86.4(2) . . . . ? C21 C2 Yb1 Cl1 -44.8(3) . . . . ? C3 C2 Yb1 Cl2 -7.0(3) . . . . ? C1 C2 Yb1 Cl2 -120.06(19) . . . . ? C21 C2 Yb1 Cl2 108.8(3) . . . . ? C3 C2 Yb1 C5 75.5(2) . . . . ? C1 C2 Yb1 C5 -37.6(2) . . . . ? C21 C2 Yb1 C5 -168.7(3) . . . . ? C1 C2 Yb1 C3 -113.1(3) . . . . ? C21 C2 Yb1 C3 115.8(4) . . . . ? C3 C2 Yb1 C4 35.2(2) . . . . ? C1 C2 Yb1 C4 -77.9(2) . . . . ? C21 C2 Yb1 C4 151.0(3) . . . . ? C3 C2 Yb1 C1 113.1(3) . . . . ? C21 C2 Yb1 C1 -131.1(4) . . . . ? C9 C8 Yb2 O3 38.7(3) . . . . ? C7 C8 Yb2 O3 -76.9(2) . . . . ? C9 C8 Yb2 O4 -132.7(2) . . . . ? C7 C8 Yb2 O4 111.7(2) . . . . ? C9 C8 Yb2 Cl4 152.07(19) . . . . ? C7 C8 Yb2 Cl4 36.5(2) . . . . ? C9 C8 Yb2 Cl3 -60.6(2) . . . . ? C7 C8 Yb2 Cl3 -176.16(18) . . . . ? C9 C8 Yb2 C10 37.6(2) . . . . ? C7 C8 Yb2 C10 -78.0(2) . . . . ? C9 C8 Yb2 C7 115.6(3) . . . . ? C7 C8 Yb2 C9 -115.6(3) . . . . ? C9 C8 Yb2 C6 77.9(2) . . . . ? C7 C8 Yb2 C6 -37.7(2) . . . . ? C9 C10 Yb2 O3 142.8(2) . . . . ? C6 C10 Yb2 O3 -100.2(2) . . . . ? C9 C10 Yb2 O4 -25.3(3) . . . . ? C6 C10 Yb2 O4 91.7(2) . . . . ? C9 C10 Yb2 Cl4 -141.15(18) . . . . ? C6 C10 Yb2 Cl4 -24.2(3) . . . . ? C9 C10 Yb2 Cl3 67.9(2) . . . . ? C6 C10 Yb2 Cl3 -175.1(2) . . . . ? C9 C10 Yb2 C8 -38.1(2) . . . . ? C6 C10 Yb2 C8 78.9(2) . . . . ? C9 C10 Yb2 C7 -79.1(2) . . . . ? C6 C10 Yb2 C7 37.8(2) . . . . ? C6 C10 Yb2 C9 117.0(3) . . . . ? C9 C10 Yb2 C6 -117.0(3) . . . . ? C8 C7 Yb2 O3 123.3(2) . . . . ? C6 C7 Yb2 O3 10.2(2) . . . . ? C71 C7 Yb2 O3 -124.6(3) . . . . ? C8 C7 Yb2 O4 -67.2(2) . . . . ? C6 C7 Yb2 O4 179.7(2) . . . . ? C71 C7 Yb2 O4 45.0(3) . . . . ? C8 C7 Yb2 Cl4 -149.4(2) . . . . ? C6 C7 Yb2 Cl4 97.5(2) . . . . ? C71 C7 Yb2 Cl4 -37.3(3) . . . . ? C8 C7 Yb2 Cl3 6.4(3) . . . . ? C6 C7 Yb2 Cl3 -106.7(2) . . . . ? C71 C7 Yb2 Cl3 118.6(3) . . . . ? C6 C7 Yb2 C8 -113.1(3) . . . . ? C71 C7 Yb2 C8 112.1(4) . . . . ? C8 C7 Yb2 C10 75.6(2) . . . . ? C6 C7 Yb2 C10 -37.5(2) . . . . ? C71 C7 Yb2 C10 -172.3(4) . . . . ? C8 C7 Yb2 C9 36.1(2) . . . . ? C6 C7 Yb2 C9 -77.0(2) . . . . ? C71 C7 Yb2 C9 148.2(4) . . . . ? C8 C7 Yb2 C6 113.1(3) . . . . ? C71 C7 Yb2 C6 -134.8(4) . . . . ? C10 C9 Yb2 O3 -37.8(2) . . . . ? C8 C9 Yb2 O3 -150.5(2) . . . . ? C91 C9 Yb2 O3 86.6(4) . . . . ? C10 C9 Yb2 O4 160.9(2) . . . . ? C8 C9 Yb2 O4 48.2(2) . . . . ? C91 C9 Yb2 O4 -74.7(4) . . . . ? C10 C9 Yb2 Cl4 65.9(3) . . . . ? C8 C9 Yb2 Cl4 -46.8(3) . . . . ? C91 C9 Yb2 Cl4 -169.7(3) . . . . ? C10 C9 Yb2 Cl3 -119.74(19) . . . . ? C8 C9 Yb2 Cl3 127.6(2) . . . . ? C91 C9 Yb2 Cl3 4.7(4) . . . . ? C10 C9 Yb2 C8 112.7(3) . . . . ? C91 C9 Yb2 C8 -122.9(5) . . . . ? C8 C9 Yb2 C10 -112.7(3) . . . . ? C91 C9 Yb2 C10 124.4(4) . . . . ? C10 C9 Yb2 C7 75.9(2) . . . . ? C8 C9 Yb2 C7 -36.8(2) . . . . ? C91 C9 Yb2 C7 -159.7(4) . . . . ? C10 C9 Yb2 C6 35.8(2) . . . . ? C8 C9 Yb2 C6 -76.9(2) . . . . ? C91 C9 Yb2 C6 160.2(4) . . . . ? C10 C6 Yb2 O3 75.9(2) . . . . ? C7 C6 Yb2 O3 -170.9(2) . . . . ? C61 C6 Yb2 O3 -40.3(3) . . . . ? C10 C6 Yb2 O4 -113.5(2) . . . . ? C7 C6 Yb2 O4 -0.3(3) . . . . ? C61 C6 Yb2 O4 130.3(3) . . . . ? C10 C6 Yb2 Cl4 160.8(2) . . . . ? C7 C6 Yb2 Cl4 -86.0(2) . . . . ? C61 C6 Yb2 Cl4 44.6(3) . . . . ? C10 C6 Yb2 Cl3 7.6(3) . . . . ? C7 C6 Yb2 Cl3 120.81(19) . . . . ? C61 C6 Yb2 Cl3 -108.5(3) . . . . ? C10 C6 Yb2 C8 -75.2(2) . . . . ? C7 C6 Yb2 C8 38.0(2) . . . . ? C61 C6 Yb2 C8 168.6(3) . . . . ? C7 C6 Yb2 C10 113.2(3) . . . . ? C61 C6 Yb2 C10 -116.1(4) . . . . ? C10 C6 Yb2 C7 -113.2(3) . . . . ? C61 C6 Yb2 C7 130.6(4) . . . . ? C10 C6 Yb2 C9 -35.4(2) . . . . ? C7 C6 Yb2 C9 77.8(2) . . . . ? C61 C6 Yb2 C9 -151.5(3) . . . . ? C110 C100 O1 C130 6.3(7) . . . . ? C110 C100 O1 Yb1 166.0(3) . . . . ? C120 C130 O1 C100 -26.6(6) . . . . ? C120 C130 O1 Yb1 173.3(3) . . . . ? O2 Yb1 O1 C100 -43.2(6) . . . . ? Cl1 Yb1 O1 C100 25.5(5) . . . . ? Cl2 Yb1 O1 C100 -94.7(5) . . . . ? C5 Yb1 O1 C100 147.8(5) . . . . ? C3 Yb1 O1 C100 157.9(5) . . . . ? C4 Yb1 O1 C100 171.0(5) . . . . ? C1 Yb1 O1 C100 118.7(5) . . . . ? C2 Yb1 O1 C100 118.1(5) . . . . ? O2 Yb1 O1 C130 113.3(3) . . . . ? Cl1 Yb1 O1 C130 -178.0(3) . . . . ? Cl2 Yb1 O1 C130 61.7(3) . . . . ? C5 Yb1 O1 C130 -55.7(3) . . . . ? C3 Yb1 O1 C130 -45.6(3) . . . . ? C4 Yb1 O1 C130 -32.5(3) . . . . ? C1 Yb1 O1 C130 -84.9(3) . . . . ? C2 Yb1 O1 C130 -85.5(3) . . . . ? C150 C140 O2 C170 -9.3(5) . . . . ? C150 C140 O2 Yb1 143.5(3) . . . . ? C160 C170 O2 C140 -15.6(5) . . . . ? C160 C170 O2 Yb1 -168.0(3) . . . . ? O1 Yb1 O2 C140 -105.0(3) . . . . ? Cl1 Yb1 O2 C140 -172.9(3) . . . . ? Cl2 Yb1 O2 C140 -54.0(3) . . . . ? C5 Yb1 O2 C140 60.8(3) . . . . ? C3 Yb1 O2 C140 59.2(3) . . . . ? C4 Yb1 O2 C140 40.8(3) . . . . ? C1 Yb1 O2 C140 95.2(3) . . . . ? C2 Yb1 O2 C140 90.1(3) . . . . ? O1 Yb1 O2 C170 43.8(4) . . . . ? Cl1 Yb1 O2 C170 -24.1(3) . . . . ? Cl2 Yb1 O2 C170 94.8(3) . . . . ? C5 Yb1 O2 C170 -150.4(3) . . . . ? C3 Yb1 O2 C170 -152.0(3) . . . . ? C4 Yb1 O2 C170 -170.4(3) . . . . ? C1 Yb1 O2 C170 -116.0(3) . . . . ? C2 Yb1 O2 C170 -121.1(3) . . . . ? C200 C210 O3 C180 15.0(5) . . . . ? C200 C210 O3 Yb2 164.0(3) . . . . ? C190 C180 O3 C210 10.5(5) . . . . ? C190 C180 O3 Yb2 -139.3(3) . . . . ? O4 Yb2 O3 C210 -40.5(4) . . . . ? Cl4 Yb2 O3 C210 27.0(3) . . . . ? Cl3 Yb2 O3 C210 -89.2(3) . . . . ? C8 Yb2 O3 C210 155.2(3) . . . . ? C10 Yb2 O3 C210 156.1(3) . . . . ? C7 Yb2 O3 C210 120.0(3) . . . . ? C9 Yb2 O3 C210 174.7(3) . . . . ? C6 Yb2 O3 C210 125.3(3) . . . . ? O4 Yb2 O3 C180 104.7(3) . . . . ? Cl4 Yb2 O3 C180 172.2(3) . . . . ? Cl3 Yb2 O3 C180 56.0(3) . . . . ? C8 Yb2 O3 C180 -59.6(3) . . . . ? C10 Yb2 O3 C180 -58.7(3) . . . . ? C7 Yb2 O3 C180 -94.8(3) . . . . ? C9 Yb2 O3 C180 -40.1(3) . . . . ? C6 Yb2 O3 C180 -89.5(3) . . . . ? C240 C250 O4 C220 -26.4(7) . . . . ? C240 C250 O4 Yb2 128.9(5) . . . . ? C230 C220 O4 C250 23.2(7) . . . . ? C230 C220 O4 Yb2 -131.2(6) . . . . ? O3 Yb2 O4 C250 -115.8(4) . . . . ? Cl4 Yb2 O4 C250 175.7(4) . . . . ? Cl3 Yb2 O4 C250 -66.5(4) . . . . ? C8 Yb2 O4 C250 52.2(4) . . . . ? C10 Yb2 O4 C250 42.2(4) . . . . ? C7 Yb2 O4 C250 81.5(4) . . . . ? C9 Yb2 O4 C250 29.2(4) . . . . ? C6 Yb2 O4 C250 81.7(4) . . . . ? O3 Yb2 O4 C220 34.4(5) . . . . ? Cl4 Yb2 O4 C220 -34.0(4) . . . . ? Cl3 Yb2 O4 C220 83.7(4) . . . . ? C8 Yb2 O4 C220 -157.6(4) . . . . ? C10 Yb2 O4 C220 -167.6(3) . . . . ? C7 Yb2 O4 C220 -128.2(4) . . . . ? C9 Yb2 O4 C220 179.4(4) . . . . ? C6 Yb2 O4 C220 -128.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.07 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.592 _refine_diff_density_min -1.359 _refine_diff_density_rms 0.143 #===end #14 data_0168 _database_code_depnum_ccdc_archive 'CCDC 604035' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C40 H72 Cl2 O4 Yb2' _chemical_formula_sum 'C40 H72 Cl2 O4 Yb2' _chemical_formula_weight 1033.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Rhombohedral _symmetry_space_group_name_H-M r-3:r _symmetry_space_group_name_Hall -p3* loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' _cell_length_a 16.2836(11) _cell_length_b 16.2836(11) _cell_length_c 16.2836(11) _cell_angle_alpha 109.604(7) _cell_angle_beta 109.604(7) _cell_angle_gamma 109.604(7) _cell_volume 3307.3(6) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description 'transparent block' _exptl_crystal_colour red _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1554 _exptl_absorpt_coefficient_mu 4.371 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(ABST/PLATON 98)' _exptl_absorpt_correction_T_min 0.22160 _exptl_absorpt_correction_T_max 0.39087 _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 'STOE IPDS' _diffrn_measurement_method Phi-Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46593 _diffrn_reflns_av_R_equivalents 0.2189 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4177 _reflns_number_gt 3674 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS V2.63' _computing_cell_refinement 'Stoe IPDS V2.63' _computing_data_reduction 'Stoe IPDS V2.63' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1.3688P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4177 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.579083(14) 0.632430(13) 0.050812(14) 0.02815(9) Uani 1 d . . . Cl1 Cl 0.54813(12) 0.71521(11) 0.18911(11) 0.0513(3) Uani 1 d . . . O1 O 0.7298(3) 0.6717(3) 0.1839(3) 0.0422(8) Uani 1 d . . . O2 O 0.5771(2) 0.4932(2) 0.0391(3) 0.0349(7) Uani 1 d . . . C1 C 0.6080(4) 0.6524(4) -0.0951(4) 0.0363(10) Uani 1 d . . . C2 C 0.7029(4) 0.7256(4) -0.0051(4) 0.0361(10) Uani 1 d . . . C3 C 0.6877(4) 0.7977(4) 0.0562(4) 0.0379(10) Uani 1 d . . . H3 H 0.7369 0.8524 0.1205 0.045 Uiso 1 calc R . . C4 C 0.5872(4) 0.7743(4) 0.0051(4) 0.0370(10) Uani 1 d . . . C5 C 0.5389(4) 0.6844(4) -0.0852(4) 0.0371(10) Uani 1 d . . . H5 H 0.4705 0.6499 -0.1328 0.044 Uiso 1 calc R . . C6 C 0.7856(5) 0.7609(5) 0.2811(5) 0.0672(18) Uani 1 d . . . H6A H 0.7637 0.7463 0.3250 0.101 Uiso 1 calc R . . H6B H 0.7741 0.8130 0.2745 0.101 Uiso 1 calc R . . H6C H 0.8563 0.7833 0.3092 0.101 Uiso 1 calc R . . C7 C 0.7373(4) 0.5886(4) 0.1909(5) 0.0487(13) Uani 1 d . . . H7A H 0.7157 0.5765 0.2365 0.058 Uiso 1 calc R . . H7B H 0.8066 0.6032 0.2163 0.058 Uiso 1 calc R . . C8 C 0.6701(4) 0.4977(4) 0.0866(5) 0.0444(12) Uani 1 d . . . H8A H 0.7030 0.5015 0.0471 0.053 Uiso 1 calc R . . H8B H 0.6581 0.4369 0.0905 0.053 Uiso 1 calc R . . C11 C 0.5750(5) 0.5667(5) -0.1977(4) 0.0474(12) Uani 1 d . . . C12 C 0.5830(6) 0.6120(6) -0.2659(5) 0.073(2) Uani 1 d . . . H12A H 0.5398 0.6404 -0.2737 0.109 Uiso 1 calc R . . H12B H 0.5626 0.5600 -0.3308 0.109 Uiso 1 calc R . . H12C H 0.6515 0.6640 -0.2355 0.109 Uiso 1 calc R . . C13 C 0.6318(6) 0.5081(5) -0.1948(5) 0.0696(18) Uani 1 d . . . H13A H 0.7015 0.5526 -0.1702 0.104 Uiso 1 calc R . . H13B H 0.6023 0.4533 -0.2616 0.104 Uiso 1 calc R . . H13C H 0.6270 0.4820 -0.1508 0.104 Uiso 1 calc R . . C14 C 0.4626(5) 0.4866(5) -0.2507(4) 0.0578(15) Uani 1 d . . . H14A H 0.4519 0.4608 -0.2079 0.087 Uiso 1 calc R . . H14B H 0.4441 0.4324 -0.3133 0.087 Uiso 1 calc R . . H14C H 0.4219 0.5168 -0.2637 0.087 Uiso 1 calc R . . C21 C 0.8134(4) 0.7484(5) 0.0252(5) 0.0493(13) Uani 1 d . . . C22 C 0.8375(6) 0.7649(6) -0.0532(7) 0.074(2) Uani 1 d . . . H22A H 0.8213 0.8137 -0.0628 0.111 Uiso 1 calc R . . H22B H 0.7982 0.7021 -0.1161 0.111 Uiso 1 calc R . . H22C H 0.9080 0.7891 -0.0298 0.111 Uiso 1 calc R . . C23 C 0.8360(5) 0.6688(5) 0.0393(6) 0.0618(17) Uani 1 d . . . H23A H 0.9041 0.6874 0.0548 0.093 Uiso 1 calc R . . H23B H 0.7902 0.6045 -0.0217 0.093 Uiso 1 calc R . . H23C H 0.8279 0.6646 0.0938 0.093 Uiso 1 calc R . . C24 C 0.8885(5) 0.8462(5) 0.1256(6) 0.074(2) Uani 1 d . . . H24A H 0.8728 0.8416 0.1763 0.110 Uiso 1 calc R . . H24B H 0.8845 0.9014 0.1190 0.110 Uiso 1 calc R . . H24C H 0.9556 0.8575 0.1450 0.110 Uiso 1 calc R . . C41 C 0.5463(4) 0.8453(4) 0.0322(5) 0.0467(13) Uani 1 d . . . C42 C 0.5545(7) 0.8989(6) -0.0291(7) 0.077(2) Uani 1 d . . . H42A H 0.5352 0.9489 -0.0106 0.115 Uiso 1 calc R . . H42B H 0.5104 0.8503 -0.0998 0.115 Uiso 1 calc R . . H42C H 0.6228 0.9309 -0.0148 0.115 Uiso 1 calc R . . C43 C 0.6072(5) 0.9229(4) 0.1441(5) 0.0617(17) Uani 1 d . . . H43A H 0.6074 0.8890 0.1823 0.092 Uiso 1 calc R . . H43B H 0.5775 0.9639 0.1586 0.092 Uiso 1 calc R . . H43C H 0.6754 0.9650 0.1622 0.092 Uiso 1 calc R . . C44 C 0.4352(4) 0.7860(5) 0.0010(5) 0.0558(15) Uani 1 d . . . H44A H 0.4294 0.7529 0.0394 0.084 Uiso 1 calc R . . H44B H 0.3966 0.7364 -0.0696 0.084 Uiso 1 calc R . . H44C H 0.4099 0.8316 0.0138 0.084 Uiso 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 0.02857(12) 0.02607(12) 0.03405(13) 0.01623(9) 0.01651(9) 0.01622(9) Cl1 0.0653(9) 0.0525(8) 0.0568(8) 0.0270(7) 0.0419(7) 0.0395(7) O1 0.0325(17) 0.0403(19) 0.0412(19) 0.0149(16) 0.0113(16) 0.0191(16) O2 0.0250(15) 0.0312(16) 0.0487(19) 0.0231(15) 0.0146(15) 0.0156(13) C1 0.045(3) 0.038(3) 0.042(3) 0.027(2) 0.028(2) 0.025(2) C2 0.035(2) 0.035(2) 0.052(3) 0.028(2) 0.028(2) 0.019(2) C3 0.033(2) 0.033(2) 0.046(3) 0.020(2) 0.019(2) 0.017(2) C4 0.039(3) 0.033(2) 0.050(3) 0.026(2) 0.026(2) 0.021(2) C5 0.038(3) 0.042(3) 0.045(3) 0.030(2) 0.023(2) 0.024(2) C6 0.049(4) 0.057(4) 0.047(3) 0.003(3) 0.009(3) 0.018(3) C7 0.038(3) 0.058(3) 0.057(3) 0.038(3) 0.018(3) 0.028(3) C8 0.033(2) 0.040(3) 0.068(4) 0.031(3) 0.022(3) 0.026(2) C11 0.057(3) 0.054(3) 0.043(3) 0.026(3) 0.032(3) 0.032(3) C12 0.084(5) 0.094(5) 0.059(4) 0.048(4) 0.046(4) 0.045(5) C13 0.077(5) 0.067(4) 0.062(4) 0.019(3) 0.036(4) 0.046(4) C14 0.065(4) 0.057(4) 0.040(3) 0.018(3) 0.025(3) 0.027(3) C21 0.036(3) 0.055(3) 0.073(4) 0.040(3) 0.035(3) 0.024(3) C22 0.060(4) 0.097(6) 0.110(6) 0.075(5) 0.061(5) 0.042(4) C23 0.057(4) 0.080(5) 0.088(5) 0.054(4) 0.048(4) 0.050(4) C24 0.032(3) 0.063(4) 0.098(6) 0.031(4) 0.023(3) 0.017(3) C41 0.052(3) 0.036(3) 0.069(4) 0.031(3) 0.035(3) 0.030(3) C42 0.105(6) 0.076(5) 0.131(7) 0.082(5) 0.083(6) 0.074(5) C43 0.068(4) 0.040(3) 0.085(5) 0.026(3) 0.046(4) 0.034(3) C44 0.051(3) 0.056(3) 0.077(4) 0.034(3) 0.035(3) 0.039(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 O2 2.191(3) 4_665 ? Yb1 O2 2.198(3) . ? Yb1 O1 2.362(3) . ? Yb1 Cl1 2.5145(13) . ? Yb1 C5 2.590(5) . ? Yb1 C4 2.630(4) . ? Yb1 C3 2.631(5) . ? Yb1 C1 2.671(4) . ? Yb1 C2 2.703(4) . ? Yb1 C8 3.133(4) . ? Yb1 Yb1 3.5874(8) 4_665 ? O1 C6 1.431(7) . ? O1 C7 1.437(6) . ? O2 C8 1.414(5) . ? O2 Yb1 2.191(3) 4_665 ? C1 C5 1.422(7) . ? C1 C2 1.424(7) . ? C1 C11 1.536(7) . ? C2 C3 1.419(7) . ? C2 C21 1.566(7) . ? C3 C4 1.403(7) . ? C3 H3 0.9300 . ? C4 C5 1.389(7) . ? C4 C41 1.532(6) . ? C5 H5 0.9300 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.501(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C11 C13 1.536(8) . ? C11 C12 1.540(8) . ? C11 C14 1.542(9) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C21 C24 1.520(9) . ? C21 C23 1.527(8) . ? C21 C22 1.533(8) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C41 C43 1.518(9) . ? C41 C44 1.531(8) . ? C41 C42 1.539(8) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Yb1 O2 70.36(12) 4_665 . ? O2 Yb1 O1 134.67(12) 4_665 . ? O2 Yb1 O1 69.69(12) . . ? O2 Yb1 Cl1 90.90(10) 4_665 . ? O2 Yb1 Cl1 111.73(9) . . ? O1 Yb1 Cl1 84.66(9) . . ? O2 Yb1 C5 88.67(14) 4_665 . ? O2 Yb1 C5 130.02(15) . . ? O1 Yb1 C5 134.17(14) . . ? Cl1 Yb1 C5 113.48(11) . . ? O2 Yb1 C4 108.81(14) 4_665 . ? O2 Yb1 C4 158.76(14) . . ? O1 Yb1 C4 116.21(14) . . ? Cl1 Yb1 C4 89.42(11) . . ? C5 Yb1 C4 30.85(16) . . ? O2 Yb1 C3 138.19(14) 4_665 . ? O2 Yb1 C3 140.25(13) . . ? O1 Yb1 C3 87.04(14) . . ? Cl1 Yb1 C3 97.00(11) . . ? C5 Yb1 C3 50.59(16) . . ? C4 Yb1 C3 30.92(15) . . ? O2 Yb1 C1 100.35(14) 4_665 . ? O2 Yb1 C1 107.03(13) . . ? O1 Yb1 C1 111.06(14) . . ? Cl1 Yb1 C1 141.19(10) . . ? C5 Yb1 C1 31.31(14) . . ? C4 Yb1 C1 51.78(15) . . ? C3 Yb1 C1 51.09(16) . . ? O2 Yb1 C2 131.04(14) 4_665 . ? O2 Yb1 C2 112.32(13) . . ? O1 Yb1 C2 84.25(14) . . ? Cl1 Yb1 C2 127.00(11) . . ? C5 Yb1 C2 50.76(15) . . ? C4 Yb1 C2 51.27(14) . . ? C3 Yb1 C2 30.81(15) . . ? C1 Yb1 C2 30.72(16) . . ? O2 Yb1 C8 93.69(12) 4_665 . ? O2 Yb1 C8 23.33(12) . . ? O1 Yb1 C8 48.53(13) . . ? Cl1 Yb1 C8 112.87(12) . . ? C5 Yb1 C8 133.54(15) . . ? C4 Yb1 C8 148.30(14) . . ? C3 Yb1 C8 120.00(14) . . ? C1 Yb1 C8 103.40(15) . . ? C2 Yb1 C8 97.12(14) . . ? O2 Yb1 Yb1 35.25(7) 4_665 4_665 ? O2 Yb1 Yb1 35.11(8) . 4_665 ? O1 Yb1 Yb1 102.51(9) . 4_665 ? Cl1 Yb1 Yb1 103.68(4) . 4_665 ? C5 Yb1 Yb1 112.33(12) . 4_665 ? C4 Yb1 Yb1 140.18(12) . 4_665 ? C3 Yb1 Yb1 157.87(11) . 4_665 ? C1 Yb1 Yb1 106.81(11) . 4_665 ? C2 Yb1 Yb1 129.32(11) . 4_665 ? C8 Yb1 Yb1 58.44(10) . 4_665 ? C6 O1 C7 111.6(5) . . ? C6 O1 Yb1 122.9(3) . . ? C7 O1 Yb1 117.1(3) . . ? C8 O2 Yb1 131.7(3) . 4_665 ? C8 O2 Yb1 118.7(3) . . ? Yb1 O2 Yb1 109.64(12) 4_665 . ? C5 C1 C2 105.9(4) . . ? C5 C1 C11 119.0(5) . . ? C2 C1 C11 133.9(5) . . ? C5 C1 Yb1 71.2(3) . . ? C2 C1 Yb1 75.9(3) . . ? C11 C1 Yb1 126.7(3) . . ? C3 C2 C1 107.1(4) . . ? C3 C2 C21 119.0(5) . . ? C1 C2 C21 132.8(5) . . ? C3 C2 Yb1 71.8(3) . . ? C1 C2 Yb1 73.4(3) . . ? C21 C2 Yb1 128.8(3) . . ? C4 C3 C2 109.8(5) . . ? C4 C3 Yb1 74.5(3) . . ? C2 C3 Yb1 77.4(3) . . ? C4 C3 H3 125.1 . . ? C2 C3 H3 125.1 . . ? Yb1 C3 H3 115.0 . . ? C5 C4 C3 106.1(4) . . ? C5 C4 C41 126.4(5) . . ? C3 C4 C41 126.1(5) . . ? C5 C4 Yb1 73.0(3) . . ? C3 C4 Yb1 74.6(3) . . ? C41 C4 Yb1 128.0(3) . . ? C4 C5 C1 110.9(5) . . ? C4 C5 Yb1 76.2(3) . . ? C1 C5 Yb1 77.5(3) . . ? C4 C5 H5 124.5 . . ? C1 C5 H5 124.5 . . ? Yb1 C5 H5 113.6 . . ? O1 C6 H6A 109.5 . . ? O1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 C7 C8 107.2(4) . . ? O1 C7 H7A 110.3 . . ? C8 C7 H7A 110.3 . . ? O1 C7 H7B 110.3 . . ? C8 C7 H7B 110.3 . . ? H7A C7 H7B 108.5 . . ? O2 C8 C7 110.0(4) . . ? O2 C8 Yb1 38.01(18) . . ? C7 C8 Yb1 81.9(3) . . ? O2 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? Yb1 C8 H8A 97.1 . . ? O2 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? Yb1 C8 H8B 145.7 . . ? H8A C8 H8B 108.2 . . ? C1 C11 C13 115.9(5) . . ? C1 C11 C12 107.6(5) . . ? C13 C11 C12 111.0(5) . . ? C1 C11 C14 110.6(4) . . ? C13 C11 C14 105.4(5) . . ? C12 C11 C14 105.9(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C24 C21 C23 105.3(6) . . ? C24 C21 C22 106.4(6) . . ? C23 C21 C22 110.2(5) . . ? C24 C21 C2 110.3(5) . . ? C23 C21 C2 115.2(4) . . ? C22 C21 C2 109.0(5) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C43 C41 C4 111.9(5) . . ? C43 C41 C44 109.4(5) . . ? C4 C41 C44 111.1(4) . . ? C43 C41 C42 109.7(5) . . ? C4 C41 C42 105.8(4) . . ? C44 C41 C42 108.8(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.119 _refine_diff_density_min -1.017 _refine_diff_density_rms 0.125 #===end #15-Tm data_0409 _database_code_depnum_ccdc_archive 'CCDC 604036' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C34 H58 I Tm' _chemical_formula_sum 'C34 H58 I Tm' _chemical_formula_weight 762.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 '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 11.7891(6) _cell_length_b 15.4829(8) _cell_length_c 18.5865(10) _cell_angle_alpha 90.00 _cell_angle_beta 95.586(6) _cell_angle_gamma 90.00 _cell_volume 3376.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.1 _exptl_crystal_description 'transparent plate' _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 3.561 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.36475 _exptl_absorpt_correction_T_max 0.77167 _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Stoe IPDS' _diffrn_measurement_method \F-Oscillation _diffrn_detector_area_resol_mean 18.4 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36088 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 26.73 _reflns_number_total 7156 _reflns_number_gt 5553 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS V2.63' _computing_cell_refinement 'Stoe IPDS V2.63' _computing_data_reduction 'Stoe IPDS V2.63' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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 w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7156 _refine_ls_number_parameters 341 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0244 _refine_ls_wR_factor_ref 0.0502 _refine_ls_wR_factor_gt 0.0483 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.885 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tm1 Tm 0.276911(11) 0.218119(9) 0.053795(7) 0.02094(4) Uani 1 d . . . I1 I 0.32081(2) 0.035545(17) 0.071390(14) 0.04574(8) Uani 1 d . . . C1 C 0.0960(2) 0.2794(2) 0.10761(15) 0.0249(6) Uani 1 d . . . C2 C 0.1155(2) 0.1987(2) 0.14346(15) 0.0234(7) Uani 1 d . . . C3 C 0.2211(2) 0.2056(2) 0.18979(15) 0.0223(6) Uani 1 d . . . C4 C 0.2647(2) 0.2902(2) 0.18113(15) 0.0231(6) Uani 1 d . . . C5 C 0.1881(3) 0.3339(2) 0.13050(16) 0.0256(7) Uani 1 d . . . H5 H 0.1974 0.3915 0.1143 0.031 Uiso 1 calc R . . C6 C 0.4607(3) 0.2311(2) -0.01194(15) 0.0229(7) Uani 1 d . . . C7 C 0.3782(3) 0.1960(2) -0.06572(15) 0.0244(7) Uani 1 d . . . C8 C 0.2939(3) 0.2615(2) -0.08195(15) 0.0251(7) Uani 1 d . . . C9 C 0.3251(3) 0.3365(2) -0.04087(16) 0.0246(7) Uani 1 d . . . C10 C 0.4272(3) 0.3165(2) 0.00328(16) 0.0239(7) Uani 1 d . . . H10 H 0.4665 0.3543 0.0374 0.029 Uiso 1 calc R . . C11 C -0.0148(3) 0.3115(3) 0.06787(17) 0.0309(8) Uani 1 d . . . H11 H -0.0579 0.2603 0.0469 0.037 Uiso 1 calc R . . C12 C 0.0005(3) 0.3748(3) 0.0068(2) 0.0457(10) Uani 1 d . . . H12A H 0.0413 0.4261 0.0264 0.069 Uiso 1 calc R . . H12B H -0.0744 0.3918 -0.0164 0.069 Uiso 1 calc R . . H12C H 0.0445 0.3471 -0.0290 0.069 Uiso 1 calc R . . C13 C -0.0871(4) 0.3553(4) 0.1220(2) 0.0643(16) Uani 1 d . . . H13A H -0.0494 0.4084 0.1402 0.096 Uiso 1 calc R . . H13B H -0.0957 0.3160 0.1625 0.096 Uiso 1 calc R . . H13C H -0.1625 0.3693 0.0978 0.096 Uiso 1 calc R . . C21 C 0.0381(3) 0.1200(2) 0.14103(17) 0.0309(8) Uani 1 d . . . H21 H 0.0836 0.0721 0.1657 0.037 Uiso 1 calc R . . C22 C -0.0062(4) 0.0866(3) 0.0664(2) 0.0445(10) Uani 1 d . . . H22A H -0.0576 0.1295 0.0420 0.067 Uiso 1 calc R . . H22B H -0.0475 0.0324 0.0715 0.067 Uiso 1 calc R . . H22C H 0.0581 0.0765 0.0378 0.067 Uiso 1 calc R . . C23 C -0.0652(4) 0.1351(4) 0.1845(3) 0.0675(16) Uani 1 d . . . H23A H -0.0395 0.1621 0.2310 0.101 Uiso 1 calc R . . H23B H -0.1017 0.0797 0.1931 0.101 Uiso 1 calc R . . H23C H -0.1200 0.1732 0.1571 0.101 Uiso 1 calc R . . C31 C 0.2614(3) 0.1357(2) 0.24407(17) 0.0286(7) Uani 1 d . . . H31 H 0.2335 0.0797 0.2221 0.034 Uiso 1 calc R . . C32 C 0.3891(4) 0.1250(3) 0.2622(2) 0.0541(12) Uani 1 d . . . H32A H 0.4267 0.1240 0.2174 0.081 Uiso 1 calc R . . H32B H 0.4043 0.0708 0.2885 0.081 Uiso 1 calc R . . H32C H 0.4187 0.1735 0.2924 0.081 Uiso 1 calc R . . C33 C 0.2031(5) 0.1457(3) 0.3138(2) 0.0670(15) Uani 1 d . . . H33A H 0.2229 0.0964 0.3457 0.100 Uiso 1 calc R . . H33B H 0.1203 0.1478 0.3021 0.100 Uiso 1 calc R . . H33C H 0.2290 0.1992 0.3383 0.100 Uiso 1 calc R . . C41 C 0.3583(3) 0.3350(2) 0.22991(17) 0.0278(7) Uani 1 d . . . H41 H 0.4143 0.2902 0.2491 0.033 Uiso 1 calc R . . C42 C 0.4227(4) 0.4045(3) 0.1930(2) 0.0522(12) Uani 1 d . . . H42A H 0.3694 0.4493 0.1739 0.078 Uiso 1 calc R . . H42B H 0.4599 0.3788 0.1532 0.078 Uiso 1 calc R . . H42C H 0.4806 0.4302 0.2280 0.078 Uiso 1 calc R . . C43 C 0.3063(4) 0.3752(3) 0.2935(2) 0.0483(11) Uani 1 d . . . H43A H 0.2506 0.4192 0.2759 0.072 Uiso 1 calc R . . H43B H 0.3664 0.4020 0.3262 0.072 Uiso 1 calc R . . H43C H 0.2681 0.3304 0.3195 0.072 Uiso 1 calc R . . C61 C 0.5680(3) 0.1893(2) 0.02149(16) 0.0268(7) Uani 1 d . . . H61 H 0.5586 0.1253 0.0167 0.032 Uiso 1 calc R . . C62 C 0.5910(3) 0.2108(3) 0.10226(17) 0.0438(9) Uani 1 d . . . H62A H 0.6078 0.2726 0.1080 0.066 Uiso 1 calc R . . H62B H 0.6562 0.1771 0.1234 0.066 Uiso 1 calc R . . H62C H 0.5235 0.1966 0.1269 0.066 Uiso 1 calc R . . C63 C 0.6718(3) 0.2155(3) -0.01648(19) 0.0428(9) Uani 1 d . . . H63A H 0.6608 0.1975 -0.0672 0.064 Uiso 1 calc R . . H63B H 0.7399 0.1874 0.0073 0.064 Uiso 1 calc R . . H63C H 0.6813 0.2783 -0.0138 0.064 Uiso 1 calc R . . C71 C 0.4036(3) 0.1130(2) -0.10585(17) 0.0325(8) Uani 1 d . . . H71 H 0.4597 0.0805 -0.0722 0.039 Uiso 1 calc R . . C72 C 0.3100(4) 0.0488(3) -0.1292(2) 0.0478(10) Uani 1 d . . . H72A H 0.2712 0.0316 -0.0872 0.072 Uiso 1 calc R . . H72B H 0.3434 -0.0022 -0.1502 0.072 Uiso 1 calc R . . H72C H 0.2550 0.0757 -0.1654 0.072 Uiso 1 calc R . . C73 C 0.4683(3) 0.1369(3) -0.17147(18) 0.0438(10) Uani 1 d . . . H73A H 0.4966 0.0842 -0.1928 0.066 Uiso 1 calc R . . H73B H 0.5327 0.1746 -0.1556 0.066 Uiso 1 calc R . . H73C H 0.4166 0.1671 -0.2076 0.066 Uiso 1 calc R . . C81 C 0.1821(3) 0.2577(3) -0.13064(16) 0.0319(8) Uani 1 d . . . H81 H 0.1462 0.3158 -0.1265 0.038 Uiso 1 calc R . . C82 C 0.0985(3) 0.1936(3) -0.10233(19) 0.0426(10) Uani 1 d . . . H82A H 0.1276 0.1347 -0.1068 0.064 Uiso 1 calc R . . H82B H 0.0243 0.1988 -0.1306 0.064 Uiso 1 calc R . . H82C H 0.0902 0.2061 -0.0514 0.064 Uiso 1 calc R . . C83 C 0.1934(3) 0.2452(3) -0.21172(18) 0.0454(11) Uani 1 d . . . H83A H 0.2457 0.2887 -0.2280 0.068 Uiso 1 calc R . . H83B H 0.1185 0.2517 -0.2390 0.068 Uiso 1 calc R . . H83C H 0.2234 0.1874 -0.2199 0.068 Uiso 1 calc R . . C91 C 0.2826(3) 0.4283(2) -0.05636(18) 0.0323(8) Uani 1 d . . . H91 H 0.1975 0.4271 -0.0638 0.039 Uiso 1 calc R . . C92 C 0.3182(4) 0.4924(2) 0.0034(2) 0.0412(9) Uani 1 d . . . H92A H 0.2867 0.4746 0.0480 0.062 Uiso 1 calc R . . H92B H 0.2894 0.5499 -0.0108 0.062 Uiso 1 calc R . . H92C H 0.4016 0.4942 0.0116 0.062 Uiso 1 calc R . . C93 C 0.3278(4) 0.4587(3) -0.1267(2) 0.0542(12) Uani 1 d . . . H93A H 0.3046 0.5187 -0.1363 0.081 Uiso 1 calc R . . H93B H 0.2966 0.4219 -0.1667 0.081 Uiso 1 calc R . . H93C H 0.4112 0.4549 -0.1219 0.081 Uiso 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 Tm1 0.02073(6) 0.01999(7) 0.02237(6) 0.00101(6) 0.00342(4) 0.00168(7) I1 0.06345(17) 0.02505(13) 0.05390(15) 0.00959(11) 0.03203(13) 0.01466(12) C1 0.0193(14) 0.0278(18) 0.0282(14) -0.0042(14) 0.0055(11) 0.0045(15) C2 0.0196(14) 0.0270(19) 0.0239(14) -0.0034(12) 0.0035(11) -0.0005(14) C3 0.0236(15) 0.0226(17) 0.0209(13) -0.0019(12) 0.0030(11) -0.0002(14) C4 0.0236(14) 0.0232(17) 0.0228(13) -0.0045(13) 0.0029(11) 0.0002(15) C5 0.0269(17) 0.0212(17) 0.0297(16) 0.0003(13) 0.0085(13) 0.0036(14) C6 0.0209(14) 0.0261(18) 0.0225(13) 0.0030(13) 0.0057(11) 0.0010(14) C7 0.0245(15) 0.0284(19) 0.0205(14) 0.0010(12) 0.0028(12) 0.0000(14) C8 0.0204(15) 0.035(2) 0.0199(13) 0.0046(13) -0.0001(11) 0.0026(14) C9 0.0218(16) 0.0249(18) 0.0274(15) 0.0033(13) 0.0037(13) 0.0032(14) C10 0.0231(15) 0.0278(18) 0.0210(14) 0.0033(12) 0.0028(12) 0.0011(14) C11 0.0222(16) 0.040(2) 0.0302(16) 0.0006(14) 0.0016(13) 0.0050(16) C12 0.037(2) 0.050(3) 0.051(2) 0.0142(19) 0.0040(18) 0.013(2) C13 0.044(2) 0.107(5) 0.043(2) 0.001(2) 0.0076(19) 0.043(3) C21 0.0255(17) 0.036(2) 0.0319(16) -0.0043(14) 0.0045(13) -0.0065(16) C22 0.045(2) 0.041(2) 0.046(2) -0.0081(18) -0.0033(18) -0.013(2) C23 0.057(3) 0.079(4) 0.073(3) -0.027(3) 0.038(3) -0.035(3) C31 0.0348(19) 0.0219(19) 0.0292(16) 0.0011(13) 0.0032(14) -0.0007(15) C32 0.041(2) 0.055(3) 0.061(3) 0.031(2) -0.020(2) -0.005(2) C33 0.118(4) 0.052(3) 0.036(2) 0.014(2) 0.032(3) 0.018(3) C41 0.0262(17) 0.0246(18) 0.0321(16) -0.0041(14) -0.0006(13) 0.0010(15) C42 0.062(3) 0.054(3) 0.041(2) -0.0145(19) 0.0053(19) -0.036(2) C43 0.050(2) 0.054(3) 0.042(2) -0.0220(19) 0.0112(18) -0.017(2) C61 0.0209(15) 0.0301(19) 0.0290(15) 0.0010(13) -0.0001(12) 0.0035(14) C62 0.040(2) 0.059(3) 0.0309(17) 0.0034(19) -0.0047(14) 0.010(2) C63 0.0238(16) 0.061(3) 0.0440(19) 0.005(2) 0.0053(14) 0.002(2) C71 0.0352(19) 0.033(2) 0.0290(16) -0.0069(14) 0.0013(14) 0.0026(17) C72 0.056(3) 0.038(2) 0.048(2) -0.0145(18) -0.0004(19) -0.002(2) C73 0.045(2) 0.058(3) 0.0298(17) -0.0082(17) 0.0085(16) 0.008(2) C81 0.0209(16) 0.048(2) 0.0261(15) 0.0044(14) -0.0019(12) 0.0022(16) C82 0.0336(19) 0.056(3) 0.0379(19) -0.0013(17) 0.0001(15) -0.004(2) C83 0.036(2) 0.072(3) 0.0273(17) 0.0053(17) -0.0043(15) 0.003(2) C91 0.0312(19) 0.029(2) 0.0370(18) 0.0094(15) 0.0073(15) 0.0059(16) C92 0.047(2) 0.0185(19) 0.058(2) 0.0089(16) 0.0052(19) 0.0041(17) C93 0.072(3) 0.039(2) 0.055(2) 0.025(2) 0.026(2) 0.016(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 Tm1 C5 2.576(3) . ? Tm1 C10 2.582(3) . ? Tm1 C6 2.597(3) . ? Tm1 C1 2.620(3) . ? Tm1 C4 2.633(3) . ? Tm1 C8 2.637(3) . ? Tm1 C9 2.640(3) . ? Tm1 C7 2.645(3) . ? Tm1 C2 2.666(3) . ? Tm1 C3 2.680(3) . ? Tm1 I1 2.8866(3) . ? C1 C5 1.409(5) . ? C1 C2 1.424(5) . ? C1 C11 1.520(4) . ? C2 C3 1.447(4) . ? C2 C21 1.520(5) . ? C3 C4 1.423(4) . ? C3 C31 1.523(4) . ? C4 C5 1.412(5) . ? C4 C41 1.525(4) . ? C6 C10 1.416(5) . ? C6 C7 1.433(4) . ? C6 C61 1.500(4) . ? C7 C8 1.431(5) . ? C7 C71 1.530(5) . ? C8 C9 1.418(5) . ? C8 C81 1.526(4) . ? C9 C10 1.424(4) . ? C9 C91 1.525(5) . ? C11 C12 1.524(5) . ? C11 C13 1.538(5) . ? C21 C22 1.524(5) . ? C21 C23 1.544(5) . ? C31 C32 1.519(5) . ? C31 C33 1.533(5) . ? C41 C43 1.517(5) . ? C41 C42 1.518(5) . ? C61 C63 1.526(4) . ? C61 C62 1.536(4) . ? C71 C72 1.517(5) . ? C71 C73 1.545(5) . ? C81 C83 1.538(4) . ? C81 C82 1.528(5) . ? C91 C92 1.519(5) . ? C91 C93 1.533(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Tm1 C10 96.93(10) . . ? C5 Tm1 C6 127.51(10) . . ? C10 Tm1 C6 31.74(10) . . ? C5 Tm1 C1 31.46(10) . . ? C10 Tm1 C1 122.56(11) . . ? C6 Tm1 C1 154.04(11) . . ? C5 Tm1 C4 31.42(10) . . ? C10 Tm1 C4 100.14(10) . . ? C6 Tm1 C4 120.72(10) . . ? C1 Tm1 C4 52.11(9) . . ? C5 Tm1 C8 115.16(10) . . ? C10 Tm1 C8 51.92(10) . . ? C6 Tm1 C8 52.10(9) . . ? C1 Tm1 C8 114.43(10) . . ? C4 Tm1 C8 140.15(11) . . ? C5 Tm1 C9 90.62(10) . . ? C10 Tm1 C9 31.62(10) . . ? C6 Tm1 C9 52.36(10) . . ? C1 Tm1 C9 103.82(10) . . ? C4 Tm1 C9 109.79(10) . . ? C8 Tm1 C9 31.18(10) . . ? C5 Tm1 C7 142.75(10) . . ? C10 Tm1 C7 52.33(10) . . ? C6 Tm1 C7 31.70(10) . . ? C1 Tm1 C7 144.92(10) . . ? C4 Tm1 C7 151.44(10) . . ? C8 Tm1 C7 31.43(10) . . ? C9 Tm1 C7 52.12(10) . . ? C5 Tm1 C2 51.64(10) . . ? C10 Tm1 C2 148.30(10) . . ? C6 Tm1 C2 169.09(9) . . ? C1 Tm1 C2 31.24(10) . . ? C4 Tm1 C2 51.78(9) . . ? C8 Tm1 C2 138.78(9) . . ? C9 Tm1 C2 135.06(10) . . ? C7 Tm1 C2 156.73(10) . . ? C5 Tm1 C3 51.55(10) . . ? C10 Tm1 C3 128.76(10) . . ? C6 Tm1 C3 137.91(9) . . ? C1 Tm1 C3 51.86(9) . . ? C4 Tm1 C3 31.06(10) . . ? C8 Tm1 C3 165.73(10) . . ? C9 Tm1 C3 140.11(10) . . ? C7 Tm1 C3 162.79(9) . . ? C2 Tm1 C3 31.40(9) . . ? C5 Tm1 I1 134.20(7) . . ? C10 Tm1 I1 119.82(7) . . ? C6 Tm1 I1 88.89(7) . . ? C1 Tm1 I1 117.05(8) . . ? C4 Tm1 I1 109.77(7) . . ? C8 Tm1 I1 109.16(8) . . ? C9 Tm1 I1 135.03(7) . . ? C7 Tm1 I1 82.99(7) . . ? C2 Tm1 I1 87.11(7) . . ? C3 Tm1 I1 83.10(7) . . ? C5 C1 C2 107.4(3) . . ? C5 C1 C11 123.5(3) . . ? C2 C1 C11 127.4(3) . . ? C5 C1 Tm1 72.52(16) . . ? C2 C1 Tm1 76.14(16) . . ? C11 C1 Tm1 128.73(19) . . ? C1 C2 C3 107.7(3) . . ? C1 C2 C21 128.3(3) . . ? C3 C2 C21 123.8(3) . . ? C1 C2 Tm1 72.62(15) . . ? C3 C2 Tm1 74.86(15) . . ? C21 C2 Tm1 122.33(19) . . ? C4 C3 C2 107.5(3) . . ? C4 C3 C31 129.5(3) . . ? C2 C3 C31 122.5(3) . . ? C4 C3 Tm1 72.65(15) . . ? C2 C3 Tm1 73.74(15) . . ? C31 C3 Tm1 125.9(2) . . ? C5 C4 C3 107.6(3) . . ? C5 C4 C41 123.8(3) . . ? C3 C4 C41 126.9(3) . . ? C5 C4 Tm1 72.03(16) . . ? C3 C4 Tm1 76.30(16) . . ? C41 C4 Tm1 128.88(18) . . ? C4 C5 C1 109.8(3) . . ? C4 C5 Tm1 76.54(17) . . ? C1 C5 Tm1 76.02(17) . . ? C10 C6 C7 108.0(3) . . ? C10 C6 C61 124.1(3) . . ? C7 C6 C61 127.8(3) . . ? C10 C6 Tm1 73.53(15) . . ? C7 C6 Tm1 75.97(16) . . ? C61 C6 Tm1 118.67(18) . . ? C6 C7 C8 106.8(3) . . ? C6 C7 C71 120.5(3) . . ? C8 C7 C71 131.1(3) . . ? C6 C7 Tm1 72.33(15) . . ? C8 C7 Tm1 74.00(16) . . ? C71 C7 Tm1 130.1(2) . . ? C9 C8 C7 109.2(3) . . ? C9 C8 C81 120.9(3) . . ? C7 C8 C81 129.8(3) . . ? C9 C8 Tm1 74.53(16) . . ? C7 C8 Tm1 74.57(16) . . ? C81 C8 Tm1 114.59(18) . . ? C8 C9 C10 107.0(3) . . ? C8 C9 C91 126.8(3) . . ? C10 C9 C91 123.7(3) . . ? C8 C9 Tm1 74.28(18) . . ? C10 C9 Tm1 71.93(17) . . ? C91 C9 Tm1 133.22(19) . . ? C6 C10 C9 108.9(3) . . ? C6 C10 Tm1 74.72(17) . . ? C9 C10 Tm1 76.46(18) . . ? C12 C11 C1 114.5(3) . . ? C12 C11 C13 108.5(4) . . ? C1 C11 C13 109.3(3) . . ? C2 C21 C22 116.8(3) . . ? C2 C21 C23 111.4(3) . . ? C22 C21 C23 108.0(3) . . ? C32 C31 C3 117.6(3) . . ? C32 C31 C33 109.8(3) . . ? C3 C31 C33 110.6(3) . . ? C43 C41 C4 109.0(3) . . ? C43 C41 C42 108.6(3) . . ? C4 C41 C42 114.7(3) . . ? C6 C61 C63 112.0(3) . . ? C6 C61 C62 111.9(3) . . ? C63 C61 C62 108.7(3) . . ? C72 C71 C7 121.2(3) . . ? C72 C71 C73 109.4(3) . . ? C7 C71 C73 108.6(3) . . ? C8 C81 C83 115.7(3) . . ? C8 C81 C82 111.7(3) . . ? C83 C81 C82 112.1(3) . . ? C92 C91 C9 114.2(3) . . ? C92 C91 C93 109.2(3) . . ? C9 C91 C93 108.2(3) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.789 _refine_diff_density_min -1.008 _refine_diff_density_rms 0.091 #===end #===end #9-Tm data_0129 _database_code_depnum_ccdc_archive 'CCDC 604428' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H39 Cl2 O2 Tm' _chemical_formula_weight 563.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 '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) _symmetry_space_group_name_Hall P_2yb loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.8947(6) _cell_length_b 13.8338(7) _cell_length_c 10.3037(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.603(8) _cell_angle_gamma 90.00 _cell_volume 1221.12(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25,5 _exptl_crystal_description 'transparent block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 3.863 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(ABST/PLATON 99)' _exptl_absorpt_correction_T_min 0.364 _exptl_absorpt_correction_T_max 0.717 _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 'Stoe IPDS' _diffrn_measurement_method Phi-Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17167 _diffrn_reflns_av_R_equivalents 0.1315 _diffrn_reflns_av_sigmaI/netI 0.0951 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4553 _reflns_number_gt 3573 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS V2.63' _computing_cell_refinement 'Stoe IPDS V2.63' _computing_data_reduction 'Stoe IPDS V2.63' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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 'w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.011(15) _refine_ls_number_reflns 4553 _refine_ls_number_parameters 245 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 0.901 _refine_ls_restrained_S_all 0.901 _refine_ls_shift/su_max 0.005 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tm Tm 0.07600(4) 0.2462 0.31509(3) 0.03329(9) Uani 1 d . . . Cl1 Cl -0.0775(3) 0.10644(17) 0.1825(3) 0.0565(6) Uani 1 d . . . Cl2 Cl 0.1061(3) 0.16000(18) 0.5363(3) 0.0542(6) Uani 1 d . . . O1 O -0.1794(8) 0.3197(5) 0.2513(7) 0.0565(18) Uani 1 d . . . O2 O 0.0534(9) 0.3863(5) 0.4509(7) 0.0573(19) Uani 1 d . . . C1 C 0.3787(9) 0.2255(6) 0.3493(8) 0.028(3) Uani 1 d . . . C2 C 0.3086(13) 0.1798(8) 0.2242(12) 0.037(3) Uani 1 d . . . C3 C 0.2352(9) 0.2578(11) 0.1298(7) 0.031(2) Uani 1 d . . . C4 C 0.2607(12) 0.3441(8) 0.1989(10) 0.033(2) Uani 1 d . . . C5 C 0.3469(10) 0.3266(7) 0.3309(9) 0.033(2) Uani 1 d . . . H5 H 0.3790 0.3736 0.3972 0.040 Uiso 1 calc R . . C6 C -0.3037(13) 0.3048(9) 0.1391(12) 0.080(4) Uani 1 d . . . H6A H -0.3999 0.3109 0.1638 0.120 Uiso 1 calc R . . H6B H -0.2967 0.2411 0.1040 0.120 Uiso 1 calc R . . H6C H -0.3007 0.3520 0.0715 0.120 Uiso 1 calc R . . C7 C -0.2101(14) 0.3987(8) 0.3294(15) 0.077(4) Uani 1 d . . . H7A H -0.1972 0.4594 0.2864 0.092 Uiso 1 calc R . . H7B H -0.3167 0.3952 0.3361 0.092 Uiso 1 calc R . . C8 C -0.0993(15) 0.3942(8) 0.4666(15) 0.076(4) Uani 1 d . . . H8A H -0.1083 0.4521 0.5170 0.092 Uiso 1 calc R . . H8B H -0.1228 0.3387 0.5153 0.092 Uiso 1 calc R . . C9 C 0.1618(15) 0.4168(9) 0.5696(10) 0.077(4) Uani 1 d . . . H9A H 0.1445 0.4838 0.5853 0.115 Uiso 1 calc R . . H9B H 0.2657 0.4085 0.5605 0.115 Uiso 1 calc R . . H9C H 0.1494 0.3790 0.6441 0.115 Uiso 1 calc R . . C11 C 0.4844(11) 0.1841(6) 0.4761(9) 0.044(2) Uani 1 d . . . H11 H 0.4351 0.1247 0.4966 0.053 Uiso 1 calc R . . C12 C 0.5093(11) 0.2495(17) 0.5985(8) 0.071(3) Uani 1 d . . . H12A H 0.5177 0.3154 0.5718 0.106 Uiso 1 calc R . . H12B H 0.6035 0.2311 0.6643 0.106 Uiso 1 calc R . . H12C H 0.4224 0.2434 0.6366 0.106 Uiso 1 calc R . . C13 C 0.6445(12) 0.1554(8) 0.4564(14) 0.078(4) Uani 1 d . . . H13A H 0.7135 0.2100 0.4751 0.117 Uiso 1 calc R . . H13B H 0.6315 0.1347 0.3651 0.117 Uiso 1 calc R . . H13C H 0.6881 0.1035 0.5167 0.117 Uiso 1 calc R . . C21 C 0.3061(13) 0.0750(7) 0.1842(11) 0.046(2) Uani 1 d . . . H21 H 0.2073 0.0647 0.1153 0.055 Uiso 1 calc R . . C22 C 0.3111(13) 0.0002(7) 0.2962(12) 0.066(3) Uani 1 d . . . H22A H 0.4134 -0.0002 0.3581 0.100 Uiso 1 calc R . . H22B H 0.2878 -0.0628 0.2568 0.100 Uiso 1 calc R . . H22C H 0.2354 0.0171 0.3434 0.100 Uiso 1 calc R . . C23 C 0.4395(14) 0.0537(8) 0.1150(14) 0.079(4) Uani 1 d . . . H23A H 0.4189 0.0878 0.0309 0.118 Uiso 1 calc R . . H23B H 0.4438 -0.0144 0.0989 0.118 Uiso 1 calc R . . H23C H 0.5376 0.0748 0.1729 0.118 Uiso 1 calc R . . C31 C 0.1635(10) 0.2417(18) -0.0204(7) 0.056(2) Uani 1 d . . . H31 H 0.1544 0.1713 -0.0308 0.067 Uiso 1 calc R . . C32 C 0.0029(15) 0.2788(8) -0.0806(11) 0.084(5) Uani 1 d . . . H32A H -0.0581 0.2711 -0.0174 0.126 Uiso 1 calc R . . H32B H -0.0445 0.2432 -0.1613 0.126 Uiso 1 calc R . . H32C H 0.0077 0.3460 -0.1022 0.126 Uiso 1 calc R . . C33 C 0.2801(15) 0.2714(9) -0.0990(9) 0.080(5) Uani 1 d . . . H33A H 0.2959 0.3400 -0.0922 0.119 Uiso 1 calc R . . H33B H 0.2396 0.2537 -0.1920 0.119 Uiso 1 calc R . . H33C H 0.3777 0.2389 -0.0621 0.119 Uiso 1 calc R . . C41 C 0.2218(12) 0.4446(7) 0.1357(10) 0.045(2) Uani 1 d . . . H41 H 0.1920 0.4363 0.0376 0.054 Uiso 1 calc R . . C42 C 0.0853(15) 0.4938(8) 0.1731(15) 0.089(5) Uani 1 d . . . H42A H 0.1100 0.5016 0.2691 0.133 Uiso 1 calc R . . H42B H -0.0067 0.4547 0.1431 0.133 Uiso 1 calc R . . H42C H 0.0670 0.5561 0.1306 0.133 Uiso 1 calc R . . C43 C 0.3628(13) 0.5117(8) 0.1717(14) 0.075(4) Uani 1 d . . . H43A H 0.4013 0.5161 0.2680 0.112 Uiso 1 calc R . . H43B H 0.3327 0.5747 0.1350 0.112 Uiso 1 calc R . . H43C H 0.4431 0.4864 0.1350 0.112 Uiso 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 Tm 0.03510(15) 0.03166(16) 0.03471(15) -0.0011(5) 0.01215(11) -0.0007(5) Cl1 0.0556(14) 0.0529(14) 0.0590(14) -0.0124(14) 0.0118(12) -0.0138(14) Cl2 0.0743(18) 0.0481(15) 0.0416(13) 0.0073(12) 0.0179(13) -0.0043(13) O1 0.039(4) 0.061(5) 0.065(5) 0.003(4) 0.006(4) 0.016(3) O2 0.076(5) 0.040(4) 0.068(5) -0.015(4) 0.039(4) -0.002(3) C1 0.032(4) 0.021(9) 0.028(4) 0.006(4) 0.005(3) -0.002(3) C2 0.041(7) 0.030(7) 0.047(7) -0.003(5) 0.025(6) -0.006(4) C3 0.041(4) 0.022(7) 0.033(3) -0.003(5) 0.014(3) -0.003(5) C4 0.040(6) 0.036(7) 0.027(5) 0.003(4) 0.015(5) 0.006(5) C5 0.040(5) 0.033(5) 0.029(5) 0.000(4) 0.013(4) 0.001(4) C6 0.045(7) 0.095(9) 0.085(9) 0.007(7) -0.006(7) 0.010(6) C7 0.060(8) 0.050(7) 0.140(13) 0.016(7) 0.060(9) 0.028(6) C8 0.086(9) 0.043(7) 0.125(12) -0.017(7) 0.072(10) 0.003(6) C9 0.112(11) 0.073(9) 0.040(6) -0.027(6) 0.011(7) 0.008(7) C11 0.048(6) 0.033(5) 0.050(6) 0.008(4) 0.011(5) 0.005(4) C12 0.085(7) 0.067(7) 0.040(4) -0.011(12) -0.018(4) 0.014(14) C13 0.035(6) 0.079(8) 0.119(11) 0.035(8) 0.020(7) 0.015(5) C21 0.060(7) 0.028(6) 0.056(7) -0.008(5) 0.026(6) -0.002(5) C22 0.068(7) 0.046(7) 0.086(9) -0.007(6) 0.023(7) -0.002(5) C23 0.095(9) 0.052(7) 0.111(11) -0.021(7) 0.063(9) 0.006(6) C31 0.068(5) 0.066(6) 0.030(4) -0.001(11) 0.008(4) 0.000(13) C32 0.098(10) 0.085(12) 0.047(6) -0.001(5) -0.019(6) -0.004(6) C33 0.131(10) 0.088(14) 0.035(5) -0.009(5) 0.048(7) -0.022(8) C41 0.060(7) 0.035(6) 0.040(6) 0.014(4) 0.013(5) 0.006(5) C42 0.077(9) 0.061(8) 0.143(13) 0.039(8) 0.056(10) 0.023(6) C43 0.063(7) 0.043(7) 0.114(10) 0.032(6) 0.016(7) -0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tm O1 2.414(6) . ? Tm O2 2.430(6) . ? Tm Cl2 2.522(2) . ? Tm Cl1 2.542(2) . ? Tm C1 2.636(8) . ? Tm C5 2.619(9) . ? Tm C4 2.651(10) . ? Tm C2 2.654(10) . ? Tm C3 2.670(6) . ? O1 C6 1.383(13) . ? O1 C7 1.427(12) . ? O2 C8 1.415(12) . ? O2 C9 1.403(13) . ? C1 C2 1.420(14) . ? C1 C5 1.430(14) . ? C1 C11 1.503(12) . ? C2 C3 1.482(17) . ? C2 C21 1.505(13) . ? C3 C4 1.377(18) . ? C3 C31 1.524(11) . ? C4 C5 1.391(13) . ? C4 C41 1.535(13) . ? C7 C8 1.491(18) . ? C11 C12 1.519(17) . ? C11 C13 1.544(12) . ? C21 C23 1.568(12) . ? C21 C22 1.541(14) . ? C31 C33 1.534(12) . ? C31 C32 1.487(16) . ? C41 C43 1.523(14) . ? C41 C42 1.529(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 Tm O2 66.6(2) . . ? O1 Tm Cl2 107.97(17) . . ? O2 Tm Cl2 82.1(2) . . ? O1 Tm Cl1 81.02(18) . . ? O2 Tm Cl1 143.14(18) . . ? Cl2 Tm Cl1 92.13(9) . . ? O1 Tm C1 159.3(2) . . ? O2 Tm C1 104.5(3) . . ? Cl2 Tm C1 88.37(18) . . ? Cl1 Tm C1 111.77(19) . . ? O1 Tm C5 128.4(3) . . ? O2 Tm C5 80.9(2) . . ? Cl2 Tm C5 105.8(2) . . ? Cl1 Tm C5 135.1(2) . . ? C1 Tm C5 31.6(3) . . ? O1 Tm C4 108.3(3) . . ? O2 Tm C4 90.6(3) . . ? Cl2 Tm C4 136.2(2) . . ? Cl1 Tm C4 117.0(2) . . ? C1 Tm C4 51.8(3) . . ? C5 Tm C4 30.6(3) . . ? O1 Tm C2 144.7(3) . . ? O2 Tm C2 132.2(3) . . ? Cl2 Tm C2 104.6(3) . . ? Cl1 Tm C2 84.5(2) . . ? C1 Tm C2 31.1(3) . . ? C5 Tm C2 51.5(3) . . ? C4 Tm C2 51.8(3) . . ? O1 Tm C3 114.9(3) . . ? O2 Tm C3 120.4(4) . . ? Cl2 Tm C3 136.6(3) . . ? Cl1 Tm C3 88.5(3) . . ? C1 Tm C3 51.9(2) . . ? C5 Tm C3 50.4(3) . . ? C4 Tm C3 30.0(4) . . ? C2 Tm C3 32.3(4) . . ? C6 O1 C7 110.8(9) . . ? C6 O1 Tm 130.3(6) . . ? C7 O1 Tm 118.6(7) . . ? C8 O2 C9 109.4(8) . . ? C8 O2 Tm 111.0(6) . . ? C9 O2 Tm 126.7(7) . . ? C2 C1 C5 107.0(8) . . ? C2 C1 C11 129.7(9) . . ? C5 C1 C11 122.9(8) . . ? C2 C1 Tm 75.1(5) . . ? C5 C1 Tm 73.6(5) . . ? C11 C1 Tm 122.4(5) . . ? C3 C2 C1 106.2(9) . . ? C3 C2 C21 123.4(10) . . ? C1 C2 C21 130.4(11) . . ? C3 C2 Tm 74.4(5) . . ? C1 C2 Tm 73.7(5) . . ? C21 C2 Tm 118.3(6) . . ? C4 C3 C2 108.1(9) . . ? C4 C3 C31 128.2(14) . . ? C2 C3 C31 123.4(14) . . ? C4 C3 Tm 74.2(5) . . ? C2 C3 Tm 73.2(5) . . ? C31 C3 Tm 124.0(5) . . ? C3 C4 C5 109.0(10) . . ? C3 C4 C41 125.4(9) . . ? C5 C4 C41 125.1(10) . . ? C3 C4 Tm 75.8(6) . . ? C5 C4 Tm 73.4(5) . . ? C41 C4 Tm 123.9(6) . . ? C4 C5 C1 109.7(9) . . ? C4 C5 Tm 76.0(6) . . ? C1 C5 Tm 74.9(5) . . ? C8 C7 O1 108.9(8) . . ? O2 C8 C7 107.7(9) . . ? C12 C11 C1 114.3(9) . . ? C12 C11 C13 109.2(9) . . ? C1 C11 C13 111.5(8) . . ? C2 C21 C23 110.4(8) . . ? C2 C21 C22 116.5(9) . . ? C23 C21 C22 109.9(9) . . ? C3 C31 C33 109.8(9) . . ? C3 C31 C32 117.8(11) . . ? C33 C31 C32 113.4(11) . . ? C43 C41 C4 111.8(9) . . ? C43 C41 C42 108.9(9) . . ? C4 C41 C42 113.6(7) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.243 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.111