Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Reiner Anwander' _publ_contact_author_address ; Department of Chemistry University of Bergen Realfagbygget Allegaten 41 Bergen N-5007 NORWAY ; _publ_contact_author_email REINER.ANWANDER@KJ.UIB.NO _publ_section_title ; Characterization and reactivity of peralkylated LnIIAlIII heterobimetallic complexes ; loop_ _publ_author_name 'Reiner Anwander' 'Niels Age Froystein' 'Christian Meermann' 'Robert J. Miller' 'Ernst-Wilhelm Scheidt' ; W.Scherer ; 'Marcus G. Schrems' 'Hanne-Marthe Sommerfeldt' 'Karl W. Tornroos' data_Compound2a _database_code_depnum_ccdc_archive 'CCDC 664734' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H80 Al4 Sm2' _chemical_formula_sum 'C32 H80 Al4 Sm2' _chemical_formula_weight 873.58 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 32' _symmetry_space_group_name_HALL 'P 32' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _cell_length_a 11.8527(3) _cell_length_b 11.8527(3) _cell_length_c 27.0300(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3288.60(18) _cell_formula_units_Z 3 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 24955 _cell_measurement_theta_min 2.260 _cell_measurement_theta_max 25.504 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 2.749 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.526 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; Sheldrick, G.M. (2003). SADABS. Version 2004/1. University of G\"ottingen, Germany. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS SMART 2K CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean '48 \um' _diffrn_standards_number 919 _diffrn_standards_interval_count 1 _diffrn_standards_interval_time 28h _diffrn_standards_decay_% 0 _diffrn_reflns_number 40367 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.54 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.54 _diffrn_measured_fraction_theta_full 1.000 _reflns_number_total 8209 _reflns_number_gt 7602 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; Bruker (1999). SMART, version 5.054, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_cell_refinement ; Bruker (2004). SAINT, version 6.45a, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_data_reduction ; Bruker (2004). SAINT, version 6.45a, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_structure_solution ; Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of G\"ottingen, Germany. ; _computing_structure_refinement ; Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of G\"ottingen, Germany. ; _computing_molecular_graphics ; Brandenburg, K. (2005). DIAMOND. Version 3.1. Crystal Impact GbR, Bonn, Germany. ; _computing_publication_material ; Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, Wisconsin, USA. ; _refine_special_details ; Refinement of F^2^ against ALL reflections, except for 2 reflections which were evidently in error due to shadowing or removed during integration due to too large Lorentz functions (peak width). The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The four ethyl groups around Al1 are heavily disordered. C-atoms C5 and C7 were therefore refined isotropically. Also one ethyl group C9-C10 around Al2 is disordered over two positions. Distance constraints (SADI 0.005) were applied Al-C and C-C distances within all ethyl groups in the structure. All H-atoms of CH(2) groups were put in their geometric positions (AFIX 23) with U~iso~ set to be 1.2 that of the parent carbon atom. Equally the methyl group H-atoms were put in their geometric positions (AFIX 33) with U~iso~ set to be 1.5 that of the parent carbon atom. The largest positive residual density (3.23 e/\%A^3^) is located 0.85 \%A from atom Sm1. The largest negative residual density (-1.87 e/\%A^3^) is located 0.77 \%A from atom Sm1. COMMENT on checkCIF alerts: The A-alerts stem from the extensive ethyl group disorder in the structure. The last A-alert on short intra H--H interactions for atoms C3 and C5 derives from a misunderstanding by the checkCIF program. Ton Spek writes as follows: The problem is caused by the agostic C-H...Sm contact that confuses the analysis. This causes the program think that this is a 1-4 contact. Since we also have here a 1-3 contact, there should be no problem. I will include some extra Fortran code to have this particular ALERT go away. The bug has now been removed from the PLATON validation tool, but still it will be some time before this version is incorporated into the IUCr checkCIF version. The B-alerts stem from the distance contraints on the disordered (Al)methyl groups. The requested standard uncertainty is 0.005 A in order to improve convergence. The standard unceratinty calculated by PLATON is however higher. ; _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^)+(0.0509P)^2^+14.8073P] 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 0.03(2) _refine_ls_number_reflns 8209 _refine_ls_number_parameters 346 _refine_ls_number_restraints 269 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1235 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 3.231 _refine_diff_density_min -1.868 _refine_diff_density_rms 0.119 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 1.32519(5) 1.07959(5) 0.46420(3) 0.05982(16) Uani 1 1 d . . . Sm2 Sm 0.69718(4) 0.69043(4) 0.31757(3) 0.04867(12) Uani 1 1 d . . . Al1 Al 1.5150(4) 0.9891(5) 0.48224(17) 0.0902(12) Uani 1 1 d D . . Al2 Al 1.2265(3) 1.3329(3) 0.57705(13) 0.0637(8) Uani 1 1 d D . . Al3 Al 0.9587(3) 0.7398(4) 0.38037(16) 0.0820(11) Uani 1 1 d D . . Al4 Al 0.4425(3) 0.3953(3) 0.33000(11) 0.0561(7) Uani 1 1 d D . . C1 C 1.628(2) 0.905(2) 0.4840(11) 0.212(14) Uani 1 1 d D . . H1A H 1.6038 0.8465 0.5129 0.255 Uiso 1 1 calc R . . H1B H 1.6131 0.8529 0.4537 0.255 Uiso 1 1 calc R . . C2 C 1.772(2) 1.011(3) 0.4875(11) 0.25(2) Uani 1 1 d D . . H2A H 1.8263 0.9695 0.4861 0.376 Uiso 1 1 calc R . . H2B H 1.7881 1.0581 0.5188 0.376 Uiso 1 1 calc R . . H2C H 1.7948 1.0716 0.4598 0.376 Uiso 1 1 calc R . . C3 C 1.4901(17) 1.016(2) 0.4100(3) 0.157(11) Uani 1 1 d D . . H3A H 1.4515 1.0733 0.4071 0.188 Uiso 1 1 calc R . . H3B H 1.5754 1.0593 0.3929 0.188 Uiso 1 1 calc R . . C4 C 1.3995(18) 0.884(3) 0.3858(9) 0.220(18) Uani 1 1 d D . . H4A H 1.3868 0.8968 0.3509 0.331 Uiso 1 1 calc R . . H4B H 1.3151 0.8418 0.4028 0.331 Uiso 1 1 calc R . . H4C H 1.4387 0.8282 0.3883 0.331 Uiso 1 1 calc R . . C5 C 1.3423(14) 0.889(3) 0.5177(8) 0.226(14) Uiso 1 1 d D . . H5A H 1.2751 0.9039 0.5023 0.272 Uiso 1 1 calc R . . H5B H 1.3111 0.7944 0.5182 0.272 Uiso 1 1 calc R . . C6 C 1.378(3) 0.948(3) 0.5700(8) 0.196(12) Uani 1 1 d DU . . H6A H 1.3002 0.9063 0.5911 0.294 Uiso 1 1 calc R . . H6B H 1.4097 1.0417 0.5682 0.294 Uiso 1 1 calc R . . H6C H 1.4456 0.9333 0.5839 0.294 Uiso 1 1 calc R . . C7 C 1.593(4) 1.1688(15) 0.5125(12) 0.30(2) Uiso 1 1 d D . . H7A H 1.5207 1.1876 0.5156 0.358 Uiso 1 1 calc R . . H7B H 1.6188 1.1613 0.5466 0.358 Uiso 1 1 calc R . . C8 C 1.708(2) 1.292(3) 0.4902(12) 0.219(14) Uani 1 1 d DU . . H8A H 1.7334 1.3655 0.5126 0.328 Uiso 1 1 calc R . . H8B H 1.6831 1.3104 0.4581 0.328 Uiso 1 1 calc R . . H8C H 1.7823 1.2773 0.4858 0.328 Uiso 1 1 calc R . . C9 C 1.4031(13) 1.4954(16) 0.570(2) 0.088(8) Uani 0.48(2) 1 d PD A 1 H9A H 1.4654 1.4904 0.5930 0.105 Uiso 0.48(2) 1 calc PR A 1 H9B H 1.4357 1.5004 0.5359 0.105 Uiso 0.48(2) 1 calc PR A 1 C9A C 1.371(2) 1.512(3) 0.5618(18) 0.088(8) Uani 0.52(2) 1 d PD A 2 H9A1 H 1.3642 1.5316 0.5267 0.105 Uiso 0.52(2) 1 calc PR A 2 H9A2 H 1.3596 1.5751 0.5823 0.105 Uiso 0.52(2) 1 calc PR A 2 C10 C 1.396(3) 1.619(2) 0.5812(11) 0.094(11) Uani 0.48(2) 1 d PD A 1 H10A H 1.4794 1.6961 0.5727 0.141 Uiso 0.48(2) 1 calc PR A 1 H10B H 1.3783 1.6214 0.6165 0.141 Uiso 0.48(2) 1 calc PR A 1 H10C H 1.3262 1.6183 0.5616 0.141 Uiso 0.48(2) 1 calc PR A 1 C10A C 1.507(2) 1.530(3) 0.5713(12) 0.099(10) Uani 0.52(2) 1 d PD A 2 H10D H 1.5726 1.6221 0.5664 0.148 Uiso 0.52(2) 1 calc PR A 2 H10E H 1.5226 1.4761 0.5482 0.148 Uiso 0.52(2) 1 calc PR A 2 H10F H 1.5115 1.5046 0.6054 0.148 Uiso 0.52(2) 1 calc PR A 2 C11 C 1.2092(10) 1.2694(11) 0.6477(2) 0.075(3) Uani 1 1 d D . . H11A H 1.2212 1.3398 0.6706 0.089 Uiso 1 1 calc R . . H11B H 1.1205 1.1945 0.6529 0.089 Uiso 1 1 calc R . . C12 C 1.3101(15) 1.2279(18) 0.6599(6) 0.109(6) Uani 1 1 d D . . H12A H 1.2980 1.1966 0.6941 0.163 Uiso 1 1 calc R A . H12B H 1.3981 1.3027 0.6559 0.163 Uiso 1 1 calc R . . H12C H 1.2984 1.1580 0.6374 0.163 Uiso 1 1 calc R . . C13 C 1.0697(7) 1.3429(9) 0.5529(3) 0.055(2) Uani 1 1 d D . . H13A H 0.9888 1.2594 0.5592 0.066 Uiso 1 1 calc R . . H13B H 1.0639 1.4129 0.5706 0.066 Uiso 1 1 calc R . . C14 C 1.0860(15) 1.3717(16) 0.4970(3) 0.093(4) Uani 1 1 d D . . H14A H 1.0107 1.3763 0.4845 0.139 Uiso 1 1 calc R A . H14B H 1.0918 1.3020 0.4797 0.139 Uiso 1 1 calc R . . H14C H 1.1657 1.4550 0.4911 0.139 Uiso 1 1 calc R . . C15 C 1.2338(9) 1.1939(7) 0.5360(4) 0.065(3) Uani 1 1 d D A . H15A H 1.2364 1.2162 0.5006 0.078 Uiso 1 1 calc R . . H15B H 1.3157 1.1944 0.5437 0.078 Uiso 1 1 calc R . . C16 C 1.1184(8) 1.0554(8) 0.5444(4) 0.057(2) Uani 1 1 d D . . H16A H 1.1287 0.9938 0.5234 0.085 Uiso 1 1 calc R A . H16B H 1.0369 1.0532 0.5360 0.085 Uiso 1 1 calc R . . H16C H 1.1163 1.0312 0.5792 0.085 Uiso 1 1 calc R . . C17 C 1.0039(15) 0.6022(10) 0.3996(7) 0.118(6) Uani 1 1 d D . . H17A H 1.0968 0.6350 0.3918 0.142 Uiso 1 1 calc R . . H17B H 0.9931 0.5887 0.4358 0.142 Uiso 1 1 calc R . . C18 C 0.921(2) 0.4702(15) 0.3737(9) 0.144(8) Uani 1 1 d D . . H18A H 0.9493 0.4092 0.3848 0.216 Uiso 1 1 calc R . . H18B H 0.9326 0.4819 0.3378 0.216 Uiso 1 1 calc R . . H18C H 0.8292 0.4352 0.3821 0.216 Uiso 1 1 calc R . . C19 C 1.0875(9) 0.9128(7) 0.4110(5) 0.084(4) Uani 1 1 d D . . H19A H 1.0974 0.8986 0.4464 0.101 Uiso 1 1 calc R . . H19B H 1.1733 0.9444 0.3950 0.101 Uiso 1 1 calc R . . C20 C 1.0508(12) 1.0199(10) 0.4069(5) 0.082(4) Uani 1 1 d D . . H20A H 1.1182 1.0996 0.4227 0.123 Uiso 1 1 calc R . . H20B H 0.9671 0.9909 0.4233 0.123 Uiso 1 1 calc R . . H20C H 1.0437 1.0373 0.3719 0.123 Uiso 1 1 calc R . . C21 C 0.9625(8) 0.7767(14) 0.3070(2) 0.084(4) Uani 1 1 d D . . H21A H 0.9063 0.6954 0.2885 0.101 Uiso 1 1 calc R . . H21B H 0.9318 0.8392 0.3007 0.101 Uiso 1 1 calc R . . C22 C 1.1058(10) 0.835(3) 0.2914(7) 0.173(12) Uani 1 1 d D . . H22A H 1.1146 0.8570 0.2561 0.259 Uiso 1 1 calc R . . H22B H 1.1340 0.7714 0.2974 0.259 Uiso 1 1 calc R . . H22C H 1.1601 0.9140 0.3107 0.259 Uiso 1 1 calc R . . C23 C 0.7883(7) 0.6979(12) 0.4132(3) 0.080(4) Uani 1 1 d D . . H23A H 0.7672 0.7670 0.4055 0.096 Uiso 1 1 calc R . . H23B H 0.7170 0.6142 0.4003 0.096 Uiso 1 1 calc R . . C24 C 0.8009(18) 0.6886(18) 0.4695(4) 0.129(7) Uani 1 1 d D . . H24A H 0.7194 0.6703 0.4855 0.193 Uiso 1 1 calc R . . H24B H 0.8724 0.7713 0.4819 0.193 Uiso 1 1 calc R . . H24C H 0.8190 0.6182 0.4769 0.193 Uiso 1 1 calc R . . C25 C 0.4368(9) 0.5587(6) 0.3468(4) 0.071(3) Uani 1 1 d D . . H25A H 0.5013 0.6084 0.3729 0.085 Uiso 1 1 calc R . . H25B H 0.4578 0.6148 0.3172 0.085 Uiso 1 1 calc R . . C26 C 0.2984(9) 0.5170(13) 0.3651(6) 0.097(5) Uani 1 1 d D . . H26A H 0.2926 0.5946 0.3731 0.146 Uiso 1 1 calc R . . H26B H 0.2792 0.4626 0.3947 0.146 Uiso 1 1 calc R . . H26C H 0.2353 0.4673 0.3391 0.146 Uiso 1 1 calc R . . C27 C 0.6190(7) 0.4294(8) 0.3061(4) 0.068(3) Uani 1 1 d D . . H27A H 0.6448 0.4836 0.2759 0.081 Uiso 1 1 calc R . . H27B H 0.6858 0.4761 0.3319 0.081 Uiso 1 1 calc R . . C28 C 0.6074(14) 0.2966(9) 0.2952(6) 0.092(4) Uani 1 1 d D . . H28A H 0.6917 0.3100 0.2838 0.138 Uiso 1 1 calc R . . H28B H 0.5417 0.2517 0.2694 0.138 Uiso 1 1 calc R . . H28C H 0.5813 0.2436 0.3253 0.138 Uiso 1 1 calc R . . C29 C 0.4067(9) 0.2938(9) 0.3938(2) 0.058(2) Uani 1 1 d D . . H29A H 0.3127 0.2529 0.4015 0.069 Uiso 1 1 calc R . . H29B H 0.4269 0.2230 0.3888 0.069 Uiso 1 1 calc R . . C30 C 0.4850(14) 0.3761(14) 0.4383(4) 0.112(6) Uani 1 1 d D . . H30A H 0.4623 0.3206 0.4677 0.168 Uiso 1 1 calc R . . H30B H 0.4642 0.4453 0.4442 0.168 Uiso 1 1 calc R . . H30C H 0.5783 0.4151 0.4315 0.168 Uiso 1 1 calc R . . C31 C 0.3068(10) 0.2893(12) 0.2784(3) 0.090(4) Uani 1 1 d D . . H31A H 0.3057 0.2063 0.2725 0.108 Uiso 1 1 calc R . . H31B H 0.2195 0.2687 0.2903 0.108 Uiso 1 1 calc R . . C32 C 0.3393(18) 0.3678(17) 0.2301(5) 0.130(7) Uani 1 1 d D . . H32A H 0.2725 0.3175 0.2052 0.196 Uiso 1 1 calc R . . H32B H 0.4245 0.3854 0.2180 0.196 Uiso 1 1 calc R . . H32C H 0.3415 0.4503 0.2362 0.196 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.0611(3) 0.0608(3) 0.0641(3) 0.0148(3) 0.0266(3) 0.0354(3) Sm2 0.0412(2) 0.0430(3) 0.0562(2) 0.0092(2) 0.0076(2) 0.01689(19) Al1 0.076(2) 0.124(3) 0.098(3) -0.011(3) -0.011(2) 0.070(3) Al2 0.0398(15) 0.0515(17) 0.093(2) -0.0217(16) 0.0007(15) 0.0175(13) Al3 0.057(2) 0.082(3) 0.108(3) -0.029(2) -0.015(2) 0.0358(19) Al4 0.0500(15) 0.0440(15) 0.0712(19) 0.0082(13) 0.0140(14) 0.0211(13) C1 0.17(2) 0.32(4) 0.22(3) 0.06(3) -0.03(2) 0.18(3) C2 0.13(2) 0.46(6) 0.20(3) 0.03(3) 0.05(2) 0.19(3) C3 0.149(17) 0.26(3) 0.147(16) 0.120(18) 0.096(15) 0.17(2) C4 0.084(13) 0.39(5) 0.17(2) -0.15(3) -0.010(13) 0.10(2) C6 0.23(3) 0.28(3) 0.134(19) -0.08(2) -0.022(19) 0.16(3) C8 0.112(18) 0.17(2) 0.31(4) -0.01(3) -0.03(2) 0.029(18) C9 0.021(10) 0.085(12) 0.12(2) -0.013(11) -0.019(13) 0.000(8) C9A 0.021(10) 0.085(12) 0.12(2) -0.013(11) -0.019(13) 0.000(8) C10 0.09(2) 0.044(14) 0.086(18) 0.013(12) -0.001(15) -0.013(13) C10A 0.067(16) 0.10(2) 0.13(3) -0.017(18) 0.002(15) 0.049(16) C11 0.075(7) 0.077(8) 0.077(7) -0.036(6) -0.024(6) 0.042(6) C12 0.105(11) 0.147(14) 0.115(11) -0.058(10) -0.055(9) 0.094(11) C13 0.054(5) 0.053(5) 0.058(6) -0.003(4) 0.007(4) 0.027(5) C14 0.101(10) 0.123(12) 0.066(8) 0.005(7) 0.015(7) 0.064(9) C15 0.051(6) 0.056(6) 0.085(7) -0.013(5) 0.005(5) 0.025(5) C16 0.051(5) 0.060(6) 0.055(5) -0.006(4) 0.008(4) 0.025(5) C17 0.078(10) 0.088(10) 0.199(19) -0.025(11) -0.036(11) 0.049(8) C18 0.143(17) 0.101(13) 0.21(2) -0.042(13) -0.056(16) 0.078(13) C19 0.062(7) 0.079(8) 0.084(8) -0.014(7) 0.018(6) 0.016(6) C20 0.056(6) 0.064(7) 0.104(9) -0.030(7) 0.001(6) 0.013(6) C21 0.036(5) 0.114(10) 0.077(8) -0.022(7) 0.014(5) 0.018(6) C22 0.051(8) 0.33(3) 0.098(12) -0.043(15) 0.018(8) 0.064(13) C23 0.047(6) 0.077(8) 0.077(8) 0.009(6) -0.006(5) 0.001(5) C24 0.108(12) 0.126(14) 0.076(9) 0.009(9) -0.009(9) 0.001(10) C25 0.049(6) 0.081(8) 0.072(7) 0.036(6) 0.028(5) 0.024(5) C26 0.047(6) 0.082(9) 0.165(15) 0.016(9) 0.031(8) 0.033(6) C27 0.086(8) 0.053(6) 0.085(7) 0.016(5) 0.031(6) 0.051(6) C28 0.108(10) 0.056(7) 0.127(11) 0.020(7) 0.052(9) 0.052(7) C29 0.051(5) 0.065(6) 0.061(6) 0.010(5) 0.019(5) 0.032(5) C30 0.088(10) 0.096(10) 0.083(9) 0.030(8) 0.022(8) -0.005(8) C31 0.074(8) 0.088(9) 0.084(9) 0.000(7) 0.008(7) 0.023(7) C32 0.114(13) 0.143(16) 0.072(9) -0.013(10) 0.005(9) 0.018(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 Sm1 C5 2.77(4) . ? Sm1 C3 2.827(15) . ? Sm1 C15 2.871(6) . ? Sm1 C19 2.888(8) . ? Sm1 C29 2.924(6) 1_665 ? Sm1 Al1 2.978(4) . ? Sm2 C13 2.763(8) 2_764 ? Sm2 C27 2.768(8) . ? Sm2 C11 2.781(10) 2_764 ? Sm2 C23 2.785(10) . ? Sm2 C25 2.787(8) . ? Sm2 C21 2.793(9) . ? Sm2 Al2 3.282(3) 2_764 ? Sm2 Al4 3.302(3) . ? Sm2 Al3 3.320(4) . ? Al1 C5 2.022(5) . ? Al1 C7 2.023(5) . ? Al1 C1 2.025(5) . ? Al1 C3 2.025(5) . ? Al2 C9A 1.99(3) . ? Al2 C15 2.024(5) . ? Al2 C9 2.024(5) . ? Al2 C11 2.026(5) . ? Al2 C13 2.028(5) . ? Al2 Sm2 3.282(3) 3_675 ? Al3 C17 2.022(5) . ? Al3 C19 2.023(5) . ? Al3 C21 2.027(5) . ? Al3 C23 2.027(5) . ? Al4 C29 2.022(5) . ? Al4 C31 2.022(5) . ? Al4 C25 2.022(5) . ? Al4 C27 2.027(5) . ? C1 C2 1.537(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.537(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.539(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.537(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.538(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9A C10A 1.538(6) . ? C9A H9A1 0.9900 . ? C9A H9A2 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10A H10D 0.9800 . ? C10A H10E 0.9800 . ? C10A H10F 0.9800 . ? C11 C12 1.538(6) . ? C11 Sm2 2.781(10) 3_675 ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.540(6) . ? C13 Sm2 2.763(8) 3_675 ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.539(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.538(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.538(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.539(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.539(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.539(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.538(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.536(6) . ? C29 Sm1 2.924(6) 1_445 ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.537(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? 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 Sm1 C3 73.3(4) . . ? C5 Sm1 C15 103.3(5) . . ? C3 Sm1 C15 161.7(4) . . ? C5 Sm1 C19 98.4(5) . . ? C3 Sm1 C19 97.3(4) . . ? C15 Sm1 C19 101.0(3) . . ? C5 Sm1 C29 156.9(3) . 1_665 ? C3 Sm1 C29 85.5(4) . 1_665 ? C15 Sm1 C29 94.0(3) . 1_665 ? C19 Sm1 C29 93.2(3) . 1_665 ? C5 Sm1 Al1 41.0(2) . . ? C3 Sm1 Al1 40.72(13) . . ? C15 Sm1 Al1 126.2(3) . . ? C19 Sm1 Al1 119.3(2) . . ? C29 Sm1 Al1 116.0(2) 1_665 . ? C13 Sm2 C27 94.6(3) 2_764 . ? C13 Sm2 C11 75.45(18) 2_764 2_764 ? C27 Sm2 C11 167.2(3) . 2_764 ? C13 Sm2 C23 168.2(3) 2_764 . ? C27 Sm2 C23 92.7(4) . . ? C11 Sm2 C23 98.5(3) 2_764 . ? C13 Sm2 C25 97.5(3) 2_764 . ? C27 Sm2 C25 75.35(18) . . ? C11 Sm2 C25 97.7(3) 2_764 . ? C23 Sm2 C25 93.3(3) . . ? C13 Sm2 C21 95.4(2) 2_764 . ? C27 Sm2 C21 94.8(3) . . ? C11 Sm2 C21 94.1(4) 2_764 . ? C23 Sm2 C21 74.66(18) . . ? C25 Sm2 C21 164.3(3) . . ? C13 Sm2 Al2 38.00(10) 2_764 2_764 ? C27 Sm2 Al2 130.8(3) . 2_764 ? C11 Sm2 Al2 37.93(11) 2_764 2_764 ? C23 Sm2 Al2 136.4(3) . 2_764 ? C25 Sm2 Al2 95.0(2) . 2_764 ? C21 Sm2 Al2 100.6(2) . 2_764 ? C13 Sm2 Al4 97.21(19) 2_764 . ? C27 Sm2 Al4 37.74(10) . . ? C11 Sm2 Al4 134.3(2) 2_764 . ? C23 Sm2 Al4 94.2(2) . . ? C25 Sm2 Al4 37.61(10) . . ? C21 Sm2 Al4 131.6(3) . . ? Al2 Sm2 Al4 117.53(8) 2_764 . ? C13 Sm2 Al3 132.9(2) 2_764 . ? C27 Sm2 Al3 90.9(2) . . ? C11 Sm2 Al3 101.8(2) 2_764 . ? C23 Sm2 Al3 37.51(11) . . ? C25 Sm2 Al3 128.9(3) . . ? C21 Sm2 Al3 37.49(11) . . ? Al2 Sm2 Al3 128.04(10) 2_764 . ? Al4 Sm2 Al3 114.40(9) . . ? C5 Al1 C7 102.8(12) . . ? C5 Al1 C1 115.1(14) . . ? C7 Al1 C1 116.1(15) . . ? C5 Al1 C3 111.4(9) . . ? C7 Al1 C3 104.4(13) . . ? C1 Al1 C3 106.6(10) . . ? C5 Al1 Sm1 64.1(11) . . ? C7 Al1 Sm1 73.5(14) . . ? C1 Al1 Sm1 169.6(8) . . ? C3 Al1 Sm1 65.6(4) . . ? C9A Al2 C15 113.0(14) . . ? C9A Al2 C9 16.0(13) . . ? C15 Al2 C9 106.2(12) . . ? C9A Al2 C11 117.7(14) . . ? C15 Al2 C11 104.6(5) . . ? C9 Al2 C11 107.8(16) . . ? C9A Al2 C13 101.1(8) . . ? C15 Al2 C13 106.5(4) . . ? C9 Al2 C13 117.1(10) . . ? C11 Al2 C13 113.6(4) . . ? C9A Al2 Sm2 117.9(13) . 3_675 ? C15 Al2 Sm2 128.4(3) . 3_675 ? C9 Al2 Sm2 125.1(12) . 3_675 ? C11 Al2 Sm2 57.5(3) . 3_675 ? C13 Al2 Sm2 57.0(2) . 3_675 ? C17 Al3 C19 110.0(5) . . ? C17 Al3 C21 116.1(7) . . ? C19 Al3 C21 104.9(6) . . ? C17 Al3 C23 108.9(7) . . ? C19 Al3 C23 102.9(5) . . ? C21 Al3 C23 113.1(4) . . ? C17 Al3 Sm2 126.2(4) . . ? C19 Al3 Sm2 123.6(4) . . ? C21 Al3 Sm2 57.0(3) . . ? C23 Al3 Sm2 56.8(3) . . ? C29 Al4 C31 110.7(5) . . ? C29 Al4 C25 106.3(4) . . ? C31 Al4 C25 110.6(6) . . ? C29 Al4 C27 106.2(4) . . ? C31 Al4 C27 109.0(6) . . ? C25 Al4 C27 113.9(4) . . ? C29 Al4 Sm2 121.7(3) . . ? C31 Al4 Sm2 127.6(4) . . ? C25 Al4 Sm2 57.3(2) . . ? C27 Al4 Sm2 56.7(2) . . ? C2 C1 Al1 110.2(13) . . ? C2 C1 H1A 109.6 . . ? Al1 C1 H1A 109.6 . . ? C2 C1 H1B 109.6 . . ? Al1 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Al1 109.3(12) . . ? C4 C3 Sm1 105.6(11) . . ? Al1 C3 Sm1 73.6(4) . . ? C4 C3 H3A 109.8 . . ? Al1 C3 H3A 109.8 . . ? Sm1 C3 H3A 40.9 . . ? C4 C3 H3B 109.8 . . ? Al1 C3 H3B 109.8 . . ? Sm1 C3 H3B 140.3 . . ? H3A C3 H3B 108.3 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 Al1 101.7(14) . . ? C6 C5 Sm1 103(2) . . ? Al1 C5 Sm1 74.9(9) . . ? C6 C5 H5A 111.4 . . ? Al1 C5 H5A 111.4 . . ? Sm1 C5 H5A 40.7 . . ? C6 C5 H5B 111.4 . . ? Al1 C5 H5B 111.4 . . ? Sm1 C5 H5B 142.3 . . ? H5A C5 H5B 109.3 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 Al1 124.1(19) . . ? C8 C7 H7A 106.3 . . ? Al1 C7 H7A 106.3 . . ? C8 C7 H7B 106.3 . . ? Al1 C7 H7B 106.3 . . ? H7A C7 H7B 106.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 Al2 111.5(13) . . ? C10 C9 H9A 109.3 . . ? Al2 C9 H9A 109.3 . . ? C10 C9 H9B 109.3 . . ? Al2 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C10A C9A Al2 113(2) . . ? C10A C9A H9A1 108.9 . . ? Al2 C9A H9A1 108.9 . . ? C10A C9A H9A2 108.9 . . ? Al2 C9A H9A2 108.9 . . ? H9A1 C9A H9A2 107.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9A C10A H10D 109.5 . . ? C9A C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? C9A C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? C12 C11 Al2 111.7(9) . . ? C12 C11 Sm2 163.1(9) . 3_675 ? Al2 C11 Sm2 84.6(3) . 3_675 ? C12 C11 H11A 109.3 . . ? Al2 C11 H11A 109.3 . . ? Sm2 C11 H11A 67.3 3_675 . ? C12 C11 H11B 109.3 . . ? Al2 C11 H11B 109.3 . . ? Sm2 C11 H11B 58.8 3_675 . ? H11A C11 H11B 107.9 . . ? 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 . . ? C14 C13 Al2 108.2(7) . . ? C14 C13 Sm2 166.6(7) . 3_675 ? Al2 C13 Sm2 85.0(3) . 3_675 ? C14 C13 H13A 110.1 . . ? Al2 C13 H13A 110.1 . . ? Sm2 C13 H13A 65.9 3_675 . ? C14 C13 H13B 110.1 . . ? Al2 C13 H13B 110.1 . . ? Sm2 C13 H13B 61.7 3_675 . ? H13A C13 H13B 108.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 Al2 114.2(6) . . ? C16 C15 Sm1 86.6(4) . . ? Al2 C15 Sm1 159.2(4) . . ? C16 C15 H15A 108.7 . . ? Al2 C15 H15A 108.7 . . ? Sm1 C15 H15A 60.2 . . ? C16 C15 H15B 108.7 . . ? Al2 C15 H15B 108.7 . . ? Sm1 C15 H15B 62.9 . . ? H15A C15 H15B 107.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 Al3 114.4(9) . . ? C18 C17 H17A 108.7 . . ? Al3 C17 H17A 108.7 . . ? C18 C17 H17B 108.7 . . ? Al3 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 Al3 115.2(7) . . ? C20 C19 Sm1 93.0(5) . . ? Al3 C19 Sm1 151.8(5) . . ? C20 C19 H19A 108.5 . . ? Al3 C19 H19A 108.5 . . ? Sm1 C19 H19A 58.4 . . ? C20 C19 H19B 108.5 . . ? Al3 C19 H19B 108.5 . . ? Sm1 C19 H19B 59.5 . . ? H19A C19 H19B 107.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 Al3 105.4(9) . . ? C22 C21 Sm2 168.7(10) . . ? Al3 C21 Sm2 85.5(3) . . ? C22 C21 H21A 110.7 . . ? Al3 C21 H21A 110.7 . . ? Sm2 C21 H21A 67.0 . . ? C22 C21 H21B 110.7 . . ? Al3 C21 H21B 110.7 . . ? Sm2 C21 H21B 61.5 . . ? H21A C21 H21B 108.8 . . ? 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 . . ? C24 C23 Al3 109.2(9) . . ? C24 C23 Sm2 164.9(8) . . ? Al3 C23 Sm2 85.7(3) . . ? C24 C23 H23A 109.8 . . ? Al3 C23 H23A 109.8 . . ? Sm2 C23 H23A 65.1 . . ? C24 C23 H23B 109.8 . . ? Al3 C23 H23B 109.8 . . ? Sm2 C23 H23B 61.3 . . ? H23A C23 H23B 108.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 Al4 107.8(7) . . ? C26 C25 Sm2 167.1(6) . . ? Al4 C25 Sm2 85.1(2) . . ? C26 C25 H25A 110.2 . . ? Al4 C25 H25A 110.2 . . ? Sm2 C25 H25A 63.8 . . ? C26 C25 H25B 110.2 . . ? Al4 C25 H25B 110.2 . . ? Sm2 C25 H25B 63.8 . . ? H25A C25 H25B 108.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 Al4 107.6(6) . . ? C28 C27 Sm2 166.8(6) . . ? Al4 C27 Sm2 85.6(2) . . ? C28 C27 H27A 110.2 . . ? Al4 C27 H27A 110.2 . . ? Sm2 C27 H27A 62.9 . . ? C28 C27 H27B 110.2 . . ? Al4 C27 H27B 110.2 . . ? Sm2 C27 H27B 64.5 . . ? H27A C27 H27B 108.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 Al4 114.2(7) . . ? C30 C29 Sm1 82.7(6) . 1_445 ? Al4 C29 Sm1 162.1(5) . 1_445 ? C30 C29 H29A 108.7 . . ? Al4 C29 H29A 108.7 . . ? Sm1 C29 H29A 68.6 1_445 . ? C30 C29 H29B 108.7 . . ? Al4 C29 H29B 108.7 . . ? Sm1 C29 H29B 57.8 1_445 . ? H29A C29 H29B 107.6 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 Al4 109.2(8) . . ? C32 C31 H31A 109.8 . . ? Al4 C31 H31A 109.8 . . ? C32 C31 H31B 109.8 . . ? Al4 C31 H31B 109.8 . . ? H31A C31 H31B 108.3 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? 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 C3 Sm1 Al1 C5 -131.7(10) . . . . ? C15 Sm1 Al1 C5 65.9(8) . . . . ? C19 Sm1 Al1 C5 -67.0(8) . . . . ? C29 Sm1 Al1 C5 -177.1(7) 1_665 . . . ? C5 Sm1 Al1 C7 -113.6(12) . . . . ? C3 Sm1 Al1 C7 114.7(12) . . . . ? C15 Sm1 Al1 C7 -47.6(10) . . . . ? C19 Sm1 Al1 C7 179.4(10) . . . . ? C29 Sm1 Al1 C7 69.3(10) 1_665 . . . ? C5 Sm1 Al1 C1 88(5) . . . . ? C3 Sm1 Al1 C1 -44(5) . . . . ? C15 Sm1 Al1 C1 154(5) . . . . ? C19 Sm1 Al1 C1 21(5) . . . . ? C29 Sm1 Al1 C1 -89(5) 1_665 . . . ? C5 Sm1 Al1 C3 131.7(10) . . . . ? C15 Sm1 Al1 C3 -162.4(7) . . . . ? C19 Sm1 Al1 C3 64.7(8) . . . . ? C29 Sm1 Al1 C3 -45.5(7) 1_665 . . . ? C13 Sm2 Al3 C17 -100.3(8) 2_764 . . . ? C27 Sm2 Al3 C17 -3.3(8) . . . . ? C11 Sm2 Al3 C17 178.6(8) 2_764 . . . ? C23 Sm2 Al3 C17 90.0(9) . . . . ? C25 Sm2 Al3 C17 68.5(8) . . . . ? C21 Sm2 Al3 C17 -100.1(9) . . . . ? Al2 Sm2 Al3 C17 -150.6(8) 2_764 . . . ? Al4 Sm2 Al3 C17 27.3(8) . . . . ? C13 Sm2 Al3 C19 86.1(5) 2_764 . . . ? C27 Sm2 Al3 C19 -176.8(5) . . . . ? C11 Sm2 Al3 C19 5.1(5) 2_764 . . . ? C23 Sm2 Al3 C19 -83.5(6) . . . . ? C25 Sm2 Al3 C19 -105.0(5) . . . . ? C21 Sm2 Al3 C19 86.4(7) . . . . ? Al2 Sm2 Al3 C19 35.8(5) 2_764 . . . ? Al4 Sm2 Al3 C19 -146.3(5) . . . . ? C13 Sm2 Al3 C21 -0.3(6) 2_764 . . . ? C27 Sm2 Al3 C21 96.8(5) . . . . ? C11 Sm2 Al3 C21 -81.3(5) 2_764 . . . ? C23 Sm2 Al3 C21 -169.9(7) . . . . ? C25 Sm2 Al3 C21 168.6(5) . . . . ? Al2 Sm2 Al3 C21 -50.6(5) 2_764 . . . ? Al4 Sm2 Al3 C21 127.3(5) . . . . ? C13 Sm2 Al3 C23 169.6(5) 2_764 . . . ? C27 Sm2 Al3 C23 -93.3(5) . . . . ? C11 Sm2 Al3 C23 88.6(5) 2_764 . . . ? C25 Sm2 Al3 C23 -21.5(5) . . . . ? C21 Sm2 Al3 C23 169.9(7) . . . . ? Al2 Sm2 Al3 C23 119.3(5) 2_764 . . . ? Al4 Sm2 Al3 C23 -62.8(5) . . . . ? C13 Sm2 Al4 C29 177.3(4) 2_764 . . . ? C27 Sm2 Al4 C29 89.2(6) . . . . ? C11 Sm2 Al4 C29 -106.0(4) 2_764 . . . ? C23 Sm2 Al4 C29 0.2(4) . . . . ? C25 Sm2 Al4 C29 -89.7(5) . . . . ? C21 Sm2 Al4 C29 73.4(4) . . . . ? Al2 Sm2 Al4 C29 -148.7(3) 2_764 . . . ? Al3 Sm2 Al4 C29 33.1(4) . . . . ? C13 Sm2 Al4 C31 -1.0(6) 2_764 . . . ? C27 Sm2 Al4 C31 -89.2(7) . . . . ? C11 Sm2 Al4 C31 75.7(6) 2_764 . . . ? C23 Sm2 Al4 C31 -178.1(6) . . . . ? C25 Sm2 Al4 C31 91.9(7) . . . . ? C21 Sm2 Al4 C31 -104.9(6) . . . . ? Al2 Sm2 Al4 C31 32.9(6) 2_764 . . . ? Al3 Sm2 Al4 C31 -145.2(6) . . . . ? C13 Sm2 Al4 C25 -92.9(4) 2_764 . . . ? C27 Sm2 Al4 C25 178.9(6) . . . . ? C11 Sm2 Al4 C25 -16.3(5) 2_764 . . . ? C23 Sm2 Al4 C25 90.0(5) . . . . ? C21 Sm2 Al4 C25 163.2(5) . . . . ? Al2 Sm2 Al4 C25 -59.0(4) 2_764 . . . ? Al3 Sm2 Al4 C25 122.8(4) . . . . ? C13 Sm2 Al4 C27 88.2(5) 2_764 . . . ? C11 Sm2 Al4 C27 164.9(5) 2_764 . . . ? C23 Sm2 Al4 C27 -88.9(5) . . . . ? C25 Sm2 Al4 C27 -178.9(6) . . . . ? C21 Sm2 Al4 C27 -15.7(5) . . . . ? Al2 Sm2 Al4 C27 122.1(4) 2_764 . . . ? Al3 Sm2 Al4 C27 -56.0(4) . . . . ? C5 Al1 C1 C2 -144.5(19) . . . . ? C7 Al1 C1 C2 -24(3) . . . . ? C3 Al1 C1 C2 91(2) . . . . ? Sm1 Al1 C1 C2 132(4) . . . . ? C5 Al1 C3 C4 -55.0(16) . . . . ? C7 Al1 C3 C4 -165.3(16) . . . . ? C1 Al1 C3 C4 71.3(14) . . . . ? Sm1 Al1 C3 C4 -101.2(12) . . . . ? C5 Al1 C3 Sm1 46.2(11) . . . . ? C7 Al1 C3 Sm1 -64.0(12) . . . . ? C1 Al1 C3 Sm1 172.5(8) . . . . ? C5 Sm1 C3 C4 75.3(13) . . . . ? C15 Sm1 C3 C4 157.1(16) . . . . ? C19 Sm1 C3 C4 -21.3(12) . . . . ? C29 Sm1 C3 C4 -114.0(12) 1_665 . . . ? Al1 Sm1 C3 C4 106.0(13) . . . . ? C5 Sm1 C3 Al1 -30.8(6) . . . . ? C15 Sm1 C3 Al1 51.1(15) . . . . ? C19 Sm1 C3 Al1 -127.3(6) . . . . ? C29 Sm1 C3 Al1 140.0(6) 1_665 . . . ? C7 Al1 C5 C6 -36(3) . . . . ? C1 Al1 C5 C6 91(2) . . . . ? C3 Al1 C5 C6 -147.3(19) . . . . ? Sm1 Al1 C5 C6 -100(2) . . . . ? C7 Al1 C5 Sm1 64.3(15) . . . . ? C1 Al1 C5 Sm1 -168.5(9) . . . . ? C3 Al1 C5 Sm1 -46.9(9) . . . . ? C3 Sm1 C5 C6 129.4(13) . . . . ? C15 Sm1 C5 C6 -31.9(13) . . . . ? C19 Sm1 C5 C6 -135.4(12) . . . . ? C29 Sm1 C5 C6 105.4(17) 1_665 . . . ? Al1 Sm1 C5 C6 98.9(13) . . . . ? C3 Sm1 C5 Al1 30.6(6) . . . . ? C15 Sm1 C5 Al1 -130.8(5) . . . . ? C19 Sm1 C5 Al1 125.8(6) . . . . ? C29 Sm1 C5 Al1 6.5(17) 1_665 . . . ? C5 Al1 C7 C8 -164(3) . . . . ? C1 Al1 C7 C8 69(4) . . . . ? C3 Al1 C7 C8 -48(4) . . . . ? Sm1 Al1 C7 C8 -107(4) . . . . ? C9A Al2 C9 C10 40(8) . . . . ? C15 Al2 C9 C10 158(3) . . . . ? C11 Al2 C9 C10 -91(3) . . . . ? C13 Al2 C9 C10 39(4) . . . . ? Sm2 Al2 C9 C10 -28(4) 3_675 . . . ? C15 Al2 C9A C10A -60(3) . . . . ? C9 Al2 C9A C10A 7(7) . . . . ? C11 Al2 C9A C10A 62(3) . . . . ? C13 Al2 C9A C10A -174(3) . . . . ? Sm2 Al2 C9A C10A 128(3) 3_675 . . . ? C9A Al2 C11 C12 -77.7(14) . . . . ? C15 Al2 C11 C12 48.7(10) . . . . ? C9 Al2 C11 C12 -64.0(13) . . . . ? C13 Al2 C11 C12 164.5(9) . . . . ? Sm2 Al2 C11 C12 175.3(10) 3_675 . . . ? C9A Al2 C11 Sm2 107.0(11) . . . 3_675 ? C15 Al2 C11 Sm2 -126.6(3) . . . 3_675 ? C9 Al2 C11 Sm2 120.7(9) . . . 3_675 ? C13 Al2 C11 Sm2 -10.8(5) . . . 3_675 ? C9A Al2 C13 C14 61.5(17) . . . . ? C15 Al2 C13 C14 -56.8(9) . . . . ? C9 Al2 C13 C14 61.8(19) . . . . ? C11 Al2 C13 C14 -171.5(8) . . . . ? Sm2 Al2 C13 C14 177.7(9) 3_675 . . . ? C9A Al2 C13 Sm2 -116.2(15) . . . 3_675 ? C15 Al2 C13 Sm2 125.5(3) . . . 3_675 ? C9 Al2 C13 Sm2 -115.9(17) . . . 3_675 ? C11 Al2 C13 Sm2 10.9(5) . . . 3_675 ? C9A Al2 C15 C16 -176.0(12) . . . . ? C9 Al2 C15 C16 168.6(16) . . . . ? C11 Al2 C15 C16 54.7(9) . . . . ? C13 Al2 C15 C16 -65.8(9) . . . . ? Sm2 Al2 C15 C16 -5.1(11) 3_675 . . . ? C9A Al2 C15 Sm1 0(2) . . . . ? C9 Al2 C15 Sm1 -15(2) . . . . ? C11 Al2 C15 Sm1 -129.4(16) . . . . ? C13 Al2 C15 Sm1 110.1(16) . . . . ? Sm2 Al2 C15 Sm1 170.7(14) 3_675 . . . ? C5 Sm1 C15 C16 -56.0(7) . . . . ? C3 Sm1 C15 C16 -132.9(11) . . . . ? C19 Sm1 C15 C16 45.5(7) . . . . ? C29 Sm1 C15 C16 139.5(6) 1_665 . . . ? Al1 Sm1 C15 C16 -93.9(6) . . . . ? C5 Sm1 C15 Al2 127.8(17) . . . . ? C3 Sm1 C15 Al2 51(2) . . . . ? C19 Sm1 C15 Al2 -130.8(17) . . . . ? C29 Sm1 C15 Al2 -36.7(17) 1_665 . . . ? Al1 Sm1 C15 Al2 89.8(17) . . . . ? C19 Al3 C17 C18 -173.6(14) . . . . ? C21 Al3 C17 C18 -54.7(17) . . . . ? C23 Al3 C17 C18 74.3(16) . . . . ? Sm2 Al3 C17 C18 12.2(19) . . . . ? C17 Al3 C19 C20 -169.8(10) . . . . ? C21 Al3 C19 C20 64.7(10) . . . . ? C23 Al3 C19 C20 -53.9(10) . . . . ? Sm2 Al3 C19 C20 4.7(11) . . . . ? C17 Al3 C19 Sm1 9.0(15) . . . . ? C21 Al3 C19 Sm1 -116.5(12) . . . . ? C23 Al3 C19 Sm1 124.9(12) . . . . ? Sm2 Al3 C19 Sm1 -176.6(10) . . . . ? C5 Sm1 C19 C20 151.5(8) . . . . ? C3 Sm1 C19 C20 -134.4(8) . . . . ? C15 Sm1 C19 C20 46.1(8) . . . . ? C29 Sm1 C19 C20 -48.6(7) 1_665 . . . ? Al1 Sm1 C19 C20 -170.9(6) . . . . ? C5 Sm1 C19 Al3 -27.4(13) . . . . ? C3 Sm1 C19 Al3 46.7(13) . . . . ? C15 Sm1 C19 Al3 -132.8(12) . . . . ? C29 Sm1 C19 Al3 132.5(12) 1_665 . . . ? Al1 Sm1 C19 Al3 10.2(14) . . . . ? C17 Al3 C21 C22 -65.3(14) . . . . ? C19 Al3 C21 C22 56.3(14) . . . . ? C23 Al3 C21 C22 167.8(13) . . . . ? Sm2 Al3 C21 C22 177.0(15) . . . . ? C17 Al3 C21 Sm2 117.7(5) . . . . ? C19 Al3 C21 Sm2 -120.6(4) . . . . ? C23 Al3 C21 Sm2 -9.2(6) . . . . ? C13 Sm2 C21 C22 15(6) 2_764 . . . ? C27 Sm2 C21 C22 110(6) . . . . ? C11 Sm2 C21 C22 -61(6) 2_764 . . . ? C23 Sm2 C21 C22 -159(6) . . . . ? C25 Sm2 C21 C22 160(6) . . . . ? Al2 Sm2 C21 C22 -23(6) 2_764 . . . ? Al4 Sm2 C21 C22 120(6) . . . . ? Al3 Sm2 C21 C22 -165(7) . . . . ? C13 Sm2 C21 Al3 179.8(4) 2_764 . . . ? C27 Sm2 C21 Al3 -85.1(5) . . . . ? C11 Sm2 C21 Al3 104.1(4) 2_764 . . . ? C23 Sm2 C21 Al3 6.4(4) . . . . ? C25 Sm2 C21 Al3 -34.7(15) . . . . ? Al2 Sm2 C21 Al3 141.8(4) 2_764 . . . ? Al4 Sm2 C21 Al3 -75.5(5) . . . . ? C17 Al3 C23 C24 56.5(12) . . . . ? C19 Al3 C23 C24 -60.2(12) . . . . ? C21 Al3 C23 C24 -172.9(11) . . . . ? Sm2 Al3 C23 C24 177.9(12) . . . . ? C17 Al3 C23 Sm2 -121.4(5) . . . . ? C19 Al3 C23 Sm2 121.8(4) . . . . ? C21 Al3 C23 Sm2 9.2(6) . . . . ? C13 Sm2 C23 C24 148(4) 2_764 . . . ? C27 Sm2 C23 C24 -85(4) . . . . ? C11 Sm2 C23 C24 89(4) 2_764 . . . ? C25 Sm2 C23 C24 -9(4) . . . . ? C21 Sm2 C23 C24 -179(4) . . . . ? Al2 Sm2 C23 C24 92(4) 2_764 . . . ? Al4 Sm2 C23 C24 -47(4) . . . . ? Al3 Sm2 C23 C24 -172(5) . . . . ? C13 Sm2 C23 Al3 -40.0(16) 2_764 . . . ? C27 Sm2 C23 Al3 87.9(4) . . . . ? C11 Sm2 C23 Al3 -98.3(4) 2_764 . . . ? C25 Sm2 C23 Al3 163.4(4) . . . . ? C21 Sm2 C23 Al3 -6.3(4) . . . . ? Al2 Sm2 C23 Al3 -95.8(4) 2_764 . . . ? Al4 Sm2 C23 Al3 125.7(4) . . . . ? C29 Al4 C25 C26 -62.4(10) . . . . ? C31 Al4 C25 C26 57.8(10) . . . . ? C27 Al4 C25 C26 -179.0(9) . . . . ? Sm2 Al4 C25 C26 180.0(11) . . . . ? C29 Al4 C25 Sm2 117.6(3) . . . . ? C31 Al4 C25 Sm2 -122.2(4) . . . . ? C27 Al4 C25 Sm2 1.0(6) . . . . ? C13 Sm2 C25 C26 -88(4) 2_764 . . . ? C11 Sm2 C25 C26 -12(4) 2_764 . . . ? C23 Sm2 C25 C26 87(4) . . . . ? C21 Sm2 C25 C26 127(4) . . . . ? Al2 Sm2 C25 C26 -50(4) 2_764 . . . ? Al3 Sm2 C25 C26 100(4) . . . . ? C13 Sm2 C25 Al4 92.1(3) 2_764 . . . ? C27 Sm2 C25 Al4 -0.7(4) . . . . ? C11 Sm2 C25 Al4 168.3(3) 2_764 . . . ? C23 Sm2 C25 Al4 -92.6(4) . . . . ? C21 Sm2 C25 Al4 -53.2(13) . . . . ? Al2 Sm2 C25 Al4 130.3(3) 2_764 . . . ? Al3 Sm2 C25 Al4 -79.7(4) . . . . ? C29 Al4 C27 C28 63.2(10) . . . . ? C31 Al4 C27 C28 -56.1(11) . . . . ? C25 Al4 C27 C28 179.8(9) . . . . ? Sm2 Al4 C27 C28 -179.1(11) . . . . ? C29 Al4 C27 Sm2 -117.7(4) . . . . ? C31 Al4 C27 Sm2 123.1(5) . . . . ? C25 Al4 C27 Sm2 -1.0(6) . . . . ? C13 Sm2 C27 C28 80(4) 2_764 . . . ? C11 Sm2 C27 C28 119(4) 2_764 . . . ? C23 Sm2 C27 C28 -90(4) . . . . ? C25 Sm2 C27 C28 177(5) . . . . ? C21 Sm2 C27 C28 -15(4) . . . . ? Al2 Sm2 C27 C28 93(4) 2_764 . . . ? Al4 Sm2 C27 C28 176(5) . . . . ? Al3 Sm2 C27 C28 -53(4) . . . . ? C13 Sm2 C27 Al4 -95.9(4) 2_764 . . . ? C11 Sm2 C27 Al4 -57.5(14) 2_764 . . . ? C23 Sm2 C27 Al4 93.4(4) . . . . ? C25 Sm2 C27 Al4 0.7(4) . . . . ? C21 Sm2 C27 Al4 168.3(4) . . . . ? Al2 Sm2 C27 Al4 -83.2(4) 2_764 . . . ? Al3 Sm2 C27 Al4 130.9(4) . . . . ? C31 Al4 C29 C30 -166.8(10) . . . . ? C25 Al4 C29 C30 -46.6(10) . . . . ? C27 Al4 C29 C30 75.0(10) . . . . ? Sm2 Al4 C29 C30 14.6(11) . . . . ? C31 Al4 C29 Sm1 32.9(16) . . . 1_445 ? C25 Al4 C29 Sm1 153.1(14) . . . 1_445 ? C27 Al4 C29 Sm1 -85.2(15) . . . 1_445 ? Sm2 Al4 C29 Sm1 -145.7(13) . . . 1_445 ? C29 Al4 C31 C32 -178.4(11) . . . . ? C25 Al4 C31 C32 64.1(13) . . . . ? C27 Al4 C31 C32 -62.0(13) . . . . ? Sm2 Al4 C31 C32 0.1(14) . . . . ? # Attachment 'Compound3b.cif' #Project name MGS64 Prepared by KWT October 2007 data_Compound3b _database_code_depnum_ccdc_archive 'CCDC 664735' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common bis(tetramethyl-aluminate)-phenanthroline-ytterbium _chemical_melting_point ? _chemical_formula_moiety 'C20 H32 Al2 N2 Yb' _chemical_formula_sum 'C20 H32 Al2 N2 Yb' _chemical_formula_weight 527.48 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 16.8663(6) _cell_length_b 22.3747(8) _cell_length_c 12.3257(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.0840(10) _cell_angle_gamma 90.00 _cell_volume 4633.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 20268 _cell_measurement_theta_min 2.424 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 4.118 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.33003 _exptl_absorpt_correction_T_max 0.95948 _exptl_absorpt_process_details ; Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, Wisconsin, USA. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS SMART 2K CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean '48 \um' _diffrn_standards_number 747 _diffrn_standards_interval_count 1 _diffrn_standards_interval_time '28 h' _diffrn_standards_decay_% 0 _diffrn_reflns_number 66391 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 27.89 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 1.000 _reflns_number_total 11073 _reflns_number_gt 9774 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; Bruker (1999). SMART, version 5.059, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_cell_refinement ; Bruker (2001). SAINT, version 6.02a, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_data_reduction ; Bruker (2001). SAINT, version 6.02a, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_structure_solution ; Altomare, A. et al. (1994). SIR92. J. Appl. Cryst. 27, 435. ; _computing_structure_refinement ; Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of G\"ottingen, Germany. ; _computing_molecular_graphics ; Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_publication_material ; Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, Wisconsin, USA. ; _refine_special_details ; The asymmetric unit contains two complexes. One has a phenathroline ligand disordered over two positions in a 62:38 ratio. The disorder was treated such that bond distances within phen groups were constrained to be equal (SADI) with an s.u. of 0.01 \%A. Likewise the anisotropic displacement parameters were constrained to be equal (EADP). The methyl groups were treated as rotating refined rigid groups (AFIX 137) with a C-H distance constrained to be 0.98 \%A and with an U(iso) of H constrained to be 1.5 times that of the parent C atom. Remaining hydrogens (aromatic CH) were assigned to ride on respective pivot atom with a C-H distance of 0.95 \%A and an U(iso) of restrained to be 1.2 times that of the pivot atom. Largest positive residual density peak (1.7 \%A^3^) was situated 0.73 \%A from Yb1. Largest negative residual density peak (-1.5 \%A^3^) was located 0.72 \%A from Yb1. 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. COMMENT on checkCIF alerts: The A alerts all pertain to calculations of M-C-H angles of the refined coordinated methyl groups. The refinement allows for the threefold axis of the pyramidal rigid body to be non-parallel with the C-Al bond axis, which generates the alerts. This is however a bona fide structural feature of the coordinated methyl groups. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+18.0591P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11073 _refine_ls_number_parameters 510 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0887 _refine_ls_goodness_of_fit_ref 1.505 _refine_ls_restrained_S_all 1.502 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.698 _refine_diff_density_min -1.491 _refine_diff_density_rms 0.113 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.491869(13) 0.075508(10) 0.744447(18) 0.02646(6) Uani 1 1 d . . . Yb2 Yb -0.004461(14) 0.177096(10) 0.733395(18) 0.02711(6) Uani 1 1 d . . . Al1 Al 0.65525(10) 0.00662(8) 0.76903(13) 0.0300(3) Uani 1 1 d . . . Al2 Al 0.32977(10) 0.00739(8) 0.73960(14) 0.0303(3) Uani 1 1 d . . . Al3 Al -0.16894(10) 0.24306(7) 0.71294(13) 0.0302(3) Uani 1 1 d . A . Al4 Al 0.15585(10) 0.24843(8) 0.74316(14) 0.0336(4) Uani 1 1 d . A . N1 N 0.5400(3) 0.16084(19) 0.6377(4) 0.0300(10) Uani 1 1 d D . . C1 C 0.5852(4) 0.1544(3) 0.5553(5) 0.0376(13) Uani 1 1 d D . . H1A H 0.5969 0.1150 0.5327 0.045 Uiso 1 1 calc R . . N2 N 0.4522(3) 0.1748(2) 0.8142(4) 0.0320(10) Uani 1 1 d D . . C2 C 0.6165(4) 0.2025(3) 0.5002(5) 0.0435(15) Uani 1 1 d D . . H2 H 0.6484 0.1958 0.4417 0.052 Uiso 1 1 calc R . . C3 C 0.6002(4) 0.2589(3) 0.5324(5) 0.0434(15) Uani 1 1 d D . . H3 H 0.6213 0.2923 0.4968 0.052 Uiso 1 1 calc R . . C4 C 0.5523(4) 0.2678(2) 0.6182(5) 0.0382(14) Uani 1 1 d D . . C5 C 0.5333(5) 0.3260(3) 0.6559(6) 0.0520(18) Uani 1 1 d D . . H5 H 0.5538 0.3602 0.6223 0.062 Uiso 1 1 calc R . . C6 C 0.4875(5) 0.3329(3) 0.7370(7) 0.058(2) Uani 1 1 d D . . H6 H 0.4740 0.3723 0.7576 0.070 Uiso 1 1 calc R . . C7 C 0.4572(4) 0.2832(2) 0.7950(5) 0.0436(15) Uani 1 1 d D . . C8 C 0.4094(4) 0.2888(3) 0.8811(6) 0.0546(19) Uani 1 1 d D . . H8 H 0.3940 0.3274 0.9038 0.066 Uiso 1 1 calc R . . C9 C 0.3850(4) 0.2393(3) 0.9324(6) 0.0539(19) Uani 1 1 d D . . H9 H 0.3533 0.2428 0.9920 0.065 Uiso 1 1 calc R . . C10 C 0.4073(4) 0.1827(3) 0.8962(5) 0.0424(14) Uani 1 1 d D . . H10 H 0.3894 0.1483 0.9322 0.051 Uiso 1 1 calc R . . C11 C 0.4758(3) 0.2244(2) 0.7612(4) 0.0299(11) Uani 1 1 d D . . C12 C 0.5237(3) 0.2171(2) 0.6704(4) 0.0299(11) Uani 1 1 d D . . C13 C 0.5643(3) -0.0105(2) 0.6489(4) 0.0307(11) Uani 1 1 d . . . H13A H 0.5542 0.0253 0.6039 0.037 Uiso 1 1 calc R . . H13B H 0.5159 -0.0213 0.6828 0.037 Uiso 1 1 calc R . . H13C H 0.5797 -0.0436 0.6031 0.037 Uiso 1 1 calc R . . C14 C 0.6266(3) 0.0761(2) 0.8680(4) 0.0324(12) Uani 1 1 d . . . H14A H 0.6708 0.0832 0.9235 0.039 Uiso 1 1 calc R . . H14B H 0.5787 0.0658 0.9035 0.039 Uiso 1 1 calc R . . H14C H 0.6167 0.1122 0.8240 0.039 Uiso 1 1 calc R . . C15 C 0.7464(4) 0.0304(4) 0.6883(6) 0.0526(18) Uani 1 1 d . . . H15A H 0.7852 -0.0023 0.6904 0.079 Uiso 1 1 calc R . . H15B H 0.7716 0.0661 0.7221 0.079 Uiso 1 1 calc R . . H15C H 0.7276 0.0392 0.6125 0.079 Uiso 1 1 calc R . . C16 C 0.6702(4) -0.0655(3) 0.8612(5) 0.0442(15) Uani 1 1 d . . . H16A H 0.6845 -0.0994 0.8165 0.066 Uiso 1 1 calc R . . H16B H 0.6206 -0.0745 0.8939 0.066 Uiso 1 1 calc R . . H16C H 0.7129 -0.0584 0.9191 0.066 Uiso 1 1 calc R . . C17 C 0.4192(3) 0.0016(3) 0.8648(4) 0.0335(12) Uani 1 1 d . . . H17A H 0.4023 -0.0248 0.9218 0.040 Uiso 1 1 calc R . . H17B H 0.4305 0.0415 0.8953 0.040 Uiso 1 1 calc R . . H17C H 0.4674 -0.0146 0.8368 0.040 Uiso 1 1 calc R . . C18 C 0.3574(4) 0.0680(3) 0.6237(5) 0.0370(13) Uani 1 1 d . . . H18A H 0.3140 0.0696 0.5654 0.044 Uiso 1 1 calc R . . H18B H 0.4066 0.0558 0.5934 0.044 Uiso 1 1 calc R . . H18C H 0.3647 0.1076 0.6571 0.044 Uiso 1 1 calc R . . C19 C 0.2357(4) 0.0356(4) 0.8095(6) 0.0541(18) Uani 1 1 d . . . H19A H 0.2054 0.0011 0.8323 0.081 Uiso 1 1 calc R . . H19B H 0.2020 0.0597 0.7576 0.081 Uiso 1 1 calc R . . H19C H 0.2531 0.0599 0.8734 0.081 Uiso 1 1 calc R . . C20 C 0.3201(4) -0.0718(3) 0.6674(6) 0.0504(17) Uani 1 1 d . . . H20A H 0.2996 -0.1010 0.7172 0.076 Uiso 1 1 calc R . . H20B H 0.3726 -0.0847 0.6479 0.076 Uiso 1 1 calc R . . H20C H 0.2834 -0.0689 0.6013 0.076 Uiso 1 1 calc R . . N3 N -0.052(3) 0.0887(11) 0.834(4) 0.031(2) Uani 0.378(7) 1 d PD A 1 N4 N 0.040(2) 0.0779(10) 0.660(2) 0.027(2) Uani 0.378(7) 1 d PD A 1 C21 C -0.096(3) 0.0918(11) 0.917(3) 0.043(3) Uani 0.378(7) 1 d PD A 1 H21 H -0.1132 0.1301 0.9393 0.052 Uiso 0.378(7) 1 calc PR A 1 C22 C -0.1196(18) 0.0417(10) 0.9750(18) 0.054(4) Uani 0.378(7) 1 d PD A 1 H22 H -0.1494 0.0462 1.0364 0.064 Uiso 0.378(7) 1 calc PR A 1 C23 C -0.0987(16) -0.0134(10) 0.9411(19) 0.052(4) Uani 0.378(7) 1 d PD A 1 H23 H -0.1151 -0.0479 0.9781 0.062 Uiso 0.378(7) 1 calc PR A 1 C24 C -0.0532(13) -0.0197(8) 0.852(2) 0.047(4) Uani 0.378(7) 1 d PD A 1 C25 C -0.0216(14) -0.0756(9) 0.820(2) 0.058(4) Uani 0.378(7) 1 d PD A 1 H25 H -0.0341 -0.1107 0.8586 0.069 Uiso 0.378(7) 1 calc PR A 1 C26 C 0.0246(15) -0.0803(10) 0.739(2) 0.051(3) Uani 0.378(7) 1 d PD A 1 H26 H 0.0428 -0.1186 0.7195 0.061 Uiso 0.378(7) 1 calc PR A 1 C27 C 0.0480(11) -0.0286(7) 0.6799(15) 0.035(3) Uani 0.378(7) 1 d PD A 1 C28 C 0.0943(12) -0.0313(8) 0.5920(16) 0.042(3) Uani 0.378(7) 1 d PD A 1 H28 H 0.1118 -0.0689 0.5675 0.051 Uiso 0.378(7) 1 calc PR A 1 C29 C 0.1149(13) 0.0196(8) 0.5409(17) 0.041(3) Uani 0.378(7) 1 d PD A 1 H29 H 0.1487 0.0184 0.4832 0.049 Uiso 0.378(7) 1 calc PR A 1 C30 C 0.0845(15) 0.0738(8) 0.5764(18) 0.035(2) Uani 0.378(7) 1 d PD A 1 H30 H 0.0961 0.1094 0.5388 0.042 Uiso 0.378(7) 1 calc PR A 1 C31 C 0.0189(14) 0.0276(7) 0.7126(17) 0.025(2) Uani 0.378(7) 1 d PD A 1 C32 C -0.0295(16) 0.0334(9) 0.8027(19) 0.027(3) Uani 0.378(7) 1 d PD A 1 N3A N -0.0417(19) 0.0804(7) 0.815(2) 0.031(2) Uani 0.622(7) 1 d PD A 2 N4A N 0.0454(11) 0.0906(5) 0.6378(12) 0.027(2) Uani 0.622(7) 1 d PD A 2 C21A C -0.0875(15) 0.0753(6) 0.8973(16) 0.043(3) Uani 0.622(7) 1 d PD A 2 H21B H -0.1061 0.1107 0.9294 0.052 Uiso 0.622(7) 1 calc PR A 2 C22A C -0.1093(9) 0.0198(6) 0.9383(10) 0.054(4) Uani 0.622(7) 1 d PD A 2 H22A H -0.1437 0.0178 0.9952 0.064 Uiso 0.622(7) 1 calc PR A 2 C23A C -0.0808(8) -0.0311(6) 0.8956(11) 0.052(4) Uani 0.622(7) 1 d PD A 2 H23A H -0.0940 -0.0689 0.9243 0.062 Uiso 0.622(7) 1 calc PR A 2 C24A C -0.0323(7) -0.0279(5) 0.8095(12) 0.047(4) Uani 0.622(7) 1 d PD A 2 C25A C 0.0001(9) -0.0796(5) 0.7604(12) 0.058(4) Uani 0.622(7) 1 d PD A 2 H25A H -0.0116 -0.1182 0.7866 0.069 Uiso 0.622(7) 1 calc PR A 2 C26A C 0.0463(7) -0.0744(4) 0.6790(11) 0.051(3) Uani 0.622(7) 1 d PD A 2 H26A H 0.0688 -0.1094 0.6505 0.061 Uiso 0.622(7) 1 calc PR A 2 C27A C 0.0633(6) -0.0173(4) 0.6328(9) 0.035(3) Uani 0.622(7) 1 d PD A 2 C28A C 0.1097(7) -0.0108(5) 0.5457(9) 0.042(3) Uani 0.622(7) 1 d PD A 2 H28A H 0.1327 -0.0449 0.5150 0.051 Uiso 0.622(7) 1 calc PR A 2 C29A C 0.1220(7) 0.0445(5) 0.5047(9) 0.041(3) Uani 0.622(7) 1 d PD A 2 H29A H 0.1521 0.0494 0.4437 0.049 Uiso 0.622(7) 1 calc PR A 2 C30A C 0.0895(9) 0.0942(5) 0.5539(10) 0.035(2) Uani 0.622(7) 1 d PD A 2 H30A H 0.0995 0.1327 0.5255 0.042 Uiso 0.622(7) 1 calc PR A 2 C31A C 0.0323(8) 0.0352(4) 0.6789(9) 0.025(2) Uani 0.622(7) 1 d PD A 2 C32A C -0.0139(8) 0.0296(5) 0.7714(11) 0.027(3) Uani 0.622(7) 1 d PD A 2 C33 C -0.0821(4) 0.2558(3) 0.8398(4) 0.0345(12) Uani 1 1 d . . . H33A H -0.1001 0.2860 0.8898 0.041 Uiso 1 1 calc R A . H33B H -0.0329 0.2694 0.8108 0.041 Uiso 1 1 calc R . . H33C H -0.0722 0.2180 0.8789 0.041 Uiso 1 1 calc R . . C34 C -0.1392(4) 0.1763(2) 0.6098(4) 0.0326(12) Uani 1 1 d . . . H34A H -0.1306 0.1390 0.6508 0.039 Uiso 1 1 calc R A . H34B H -0.0904 0.1872 0.5771 0.039 Uiso 1 1 calc R . . H34C H -0.1825 0.1708 0.5522 0.039 Uiso 1 1 calc R . . C35 C -0.2631(4) 0.2173(3) 0.7854(5) 0.0471(16) Uani 1 1 d . . . H35A H -0.2881 0.2523 0.8161 0.071 Uiso 1 1 calc R A . H35B H -0.2466 0.1892 0.8440 0.071 Uiso 1 1 calc R . . H35C H -0.3012 0.1978 0.7322 0.071 Uiso 1 1 calc R . . C36 C -0.1794(4) 0.3178(3) 0.6267(6) 0.0471(16) Uani 1 1 d . . . H36A H -0.1972 0.3502 0.6723 0.071 Uiso 1 1 calc R A . H36B H -0.2185 0.3120 0.5638 0.071 Uiso 1 1 calc R . . H36C H -0.1277 0.3283 0.6013 0.071 Uiso 1 1 calc R . . C37 C 0.0638(4) 0.2595(3) 0.6230(4) 0.0375(13) Uani 1 1 d . . . H37A H 0.0767 0.2922 0.5746 0.045 Uiso 1 1 calc R A . H37B H 0.0148 0.2692 0.6565 0.045 Uiso 1 1 calc R . . H37C H 0.0562 0.2225 0.5809 0.045 Uiso 1 1 calc R . . C38 C 0.1302(4) 0.1842(3) 0.8531(5) 0.0400(14) Uani 1 1 d . . . H38A H 0.1220 0.1457 0.8156 0.048 Uiso 1 1 calc R A . H38B H 0.0818 0.1953 0.8866 0.048 Uiso 1 1 calc R . . H38C H 0.1747 0.1807 0.9096 0.048 Uiso 1 1 calc R . . C39 C 0.2480(4) 0.2240(4) 0.6658(6) 0.062(2) Uani 1 1 d . . . H39A H 0.2638 0.2571 0.6205 0.092 Uiso 1 1 calc R A . H39B H 0.2334 0.1894 0.6196 0.092 Uiso 1 1 calc R . . H39C H 0.2924 0.2134 0.7190 0.092 Uiso 1 1 calc R . . C40 C 0.1695(4) 0.3247(3) 0.8252(6) 0.0515(17) Uani 1 1 d . . . H40A H 0.1848 0.3564 0.7762 0.077 Uiso 1 1 calc R A . H40B H 0.2113 0.3199 0.8851 0.077 Uiso 1 1 calc R . . H40C H 0.1193 0.3354 0.8547 0.077 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.02832(12) 0.02274(11) 0.02937(11) 0.00321(8) 0.00845(9) 0.00140(8) Yb2 0.03213(13) 0.02346(11) 0.02666(11) -0.00121(8) 0.00776(9) 0.00121(8) Al1 0.0263(8) 0.0338(9) 0.0305(8) 0.0030(7) 0.0051(6) 0.0021(7) Al2 0.0243(8) 0.0332(9) 0.0337(8) -0.0020(7) 0.0046(7) 0.0014(7) Al3 0.0331(9) 0.0304(8) 0.0276(8) 0.0001(6) 0.0062(7) 0.0013(7) Al4 0.0284(9) 0.0416(10) 0.0303(8) -0.0047(7) 0.0006(7) 0.0009(7) N1 0.031(2) 0.023(2) 0.038(2) 0.0054(18) 0.0089(19) 0.0025(18) C1 0.041(3) 0.032(3) 0.042(3) 0.007(2) 0.015(3) 0.002(2) N2 0.030(2) 0.031(2) 0.036(2) -0.005(2) 0.0070(19) 0.0046(19) C2 0.042(3) 0.044(4) 0.046(3) 0.016(3) 0.011(3) -0.006(3) C3 0.041(3) 0.042(3) 0.046(3) 0.021(3) -0.005(3) -0.011(3) C4 0.036(3) 0.024(3) 0.051(4) 0.006(2) -0.015(3) -0.005(2) C5 0.060(5) 0.027(3) 0.066(4) 0.002(3) -0.010(4) -0.003(3) C6 0.064(5) 0.020(3) 0.087(6) -0.012(3) -0.019(4) 0.003(3) C7 0.049(4) 0.033(3) 0.046(3) -0.016(3) -0.008(3) 0.009(3) C8 0.046(4) 0.043(4) 0.072(5) -0.027(4) -0.008(4) 0.018(3) C9 0.037(4) 0.075(5) 0.049(4) -0.028(4) 0.004(3) 0.015(3) C10 0.034(3) 0.056(4) 0.038(3) -0.009(3) 0.008(3) 0.009(3) C11 0.027(3) 0.025(2) 0.036(3) -0.005(2) -0.007(2) 0.005(2) C12 0.030(3) 0.026(3) 0.032(3) 0.003(2) -0.004(2) 0.001(2) C13 0.034(3) 0.030(3) 0.028(3) 0.000(2) 0.007(2) 0.006(2) C14 0.033(3) 0.033(3) 0.031(3) 0.001(2) 0.002(2) -0.003(2) C15 0.035(3) 0.066(5) 0.059(4) 0.004(4) 0.018(3) -0.002(3) C16 0.045(4) 0.041(3) 0.045(3) 0.005(3) -0.004(3) 0.009(3) C17 0.033(3) 0.034(3) 0.034(3) 0.010(2) 0.008(2) -0.001(2) C18 0.037(3) 0.042(3) 0.031(3) 0.003(2) -0.002(2) 0.006(3) C19 0.035(4) 0.070(5) 0.059(4) -0.013(4) 0.013(3) 0.009(3) C20 0.046(4) 0.041(4) 0.064(4) -0.010(3) 0.004(3) -0.003(3) N3 0.025(8) 0.032(5) 0.038(9) 0.006(5) 0.011(4) 0.004(5) N4 0.032(4) 0.020(5) 0.029(7) 0.001(4) 0.008(4) 0.000(5) C21 0.038(7) 0.052(9) 0.041(9) 0.005(7) 0.014(5) -0.001(8) C22 0.053(7) 0.076(12) 0.032(8) 0.020(6) 0.002(6) -0.023(8) C23 0.042(8) 0.053(9) 0.058(10) 0.028(7) -0.015(7) -0.022(6) C24 0.015(7) 0.034(5) 0.089(13) 0.017(6) -0.013(5) -0.009(4) C25 0.063(10) 0.028(5) 0.078(12) 0.010(8) -0.020(8) -0.007(6) C26 0.050(7) 0.022(4) 0.078(10) -0.001(6) -0.015(6) 0.006(4) C27 0.025(5) 0.028(5) 0.051(8) -0.006(5) -0.016(5) 0.006(4) C28 0.030(5) 0.037(7) 0.058(9) -0.022(5) -0.007(5) 0.009(5) C29 0.039(5) 0.048(8) 0.037(6) -0.013(5) 0.005(5) 0.006(6) C30 0.037(4) 0.035(7) 0.034(6) -0.005(5) 0.011(4) -0.003(6) C31 0.016(5) 0.023(4) 0.033(8) 0.001(4) -0.005(4) -0.003(3) C32 0.010(6) 0.034(4) 0.036(9) 0.004(4) -0.003(5) -0.003(3) N3A 0.025(8) 0.032(5) 0.038(9) 0.006(5) 0.011(4) 0.004(5) N4A 0.032(4) 0.020(5) 0.029(7) 0.001(4) 0.008(4) 0.000(5) C21A 0.038(7) 0.052(9) 0.041(9) 0.005(7) 0.014(5) -0.001(8) C22A 0.053(7) 0.076(12) 0.032(8) 0.020(6) 0.002(6) -0.023(8) C23A 0.042(8) 0.053(9) 0.058(10) 0.028(7) -0.015(7) -0.022(6) C24A 0.015(7) 0.034(5) 0.089(13) 0.017(6) -0.013(5) -0.009(4) C25A 0.063(10) 0.028(5) 0.078(12) 0.010(8) -0.020(8) -0.007(6) C26A 0.050(7) 0.022(4) 0.078(10) -0.001(6) -0.015(6) 0.006(4) C27A 0.025(5) 0.028(5) 0.051(8) -0.006(5) -0.016(5) 0.006(4) C28A 0.030(5) 0.037(7) 0.058(9) -0.022(5) -0.007(5) 0.009(5) C29A 0.039(5) 0.048(8) 0.037(6) -0.013(5) 0.005(5) 0.006(6) C30A 0.037(4) 0.035(7) 0.034(6) -0.005(5) 0.011(4) -0.003(6) C31A 0.016(5) 0.023(4) 0.033(8) 0.001(4) -0.005(4) -0.003(3) C32A 0.010(6) 0.034(4) 0.036(9) 0.004(4) -0.003(5) -0.003(3) C33 0.038(3) 0.034(3) 0.032(3) -0.005(2) 0.005(2) 0.008(2) C34 0.037(3) 0.034(3) 0.027(2) -0.003(2) 0.005(2) -0.005(2) C35 0.039(4) 0.062(4) 0.042(3) 0.000(3) 0.014(3) 0.000(3) C36 0.049(4) 0.039(3) 0.052(4) 0.008(3) -0.004(3) 0.002(3) C37 0.044(3) 0.043(3) 0.027(3) 0.008(2) 0.007(2) -0.007(3) C38 0.042(3) 0.046(3) 0.031(3) -0.003(2) -0.002(2) 0.011(3) C39 0.038(4) 0.092(6) 0.057(4) -0.018(4) 0.014(3) 0.005(4) C40 0.049(4) 0.042(4) 0.063(4) -0.015(3) -0.001(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N1 2.494(4) . ? Yb1 N2 2.496(4) . ? Yb1 Al2 3.1260(17) . ? Yb1 Al1 3.1486(17) . ? Yb2 N4A 2.453(12) . ? Yb2 N3A 2.492(16) . ? Yb2 N3 2.50(3) . ? Yb2 N4 2.54(2) . ? Yb2 Al3 3.1328(17) . ? Yb2 Al4 3.1329(18) . ? Al1 C15 1.976(6) . ? Al1 C16 1.978(6) . ? Al1 C14 2.059(6) . ? Al1 C13 2.071(6) . ? Al2 C19 1.974(6) . ? Al2 C20 1.984(7) . ? Al2 C18 2.053(6) . ? Al2 C17 2.065(6) . ? Al3 C35 1.975(6) . ? Al3 C36 1.982(6) . ? Al3 C34 2.052(5) . ? Al3 C33 2.065(6) . ? Al4 C39 1.970(7) . ? Al4 C40 1.986(7) . ? Al4 C38 2.048(6) . ? Al4 C37 2.063(6) . ? N1 C1 1.331(6) . ? N1 C12 1.357(6) . ? C1 C2 1.400(7) . ? C1 H1A 0.9500 . ? N2 C10 1.328(6) . ? N2 C11 1.364(6) . ? C2 C3 1.359(9) . ? C2 H2 0.9500 . ? C3 C4 1.401(8) . ? C3 H3 0.9500 . ? C4 C12 1.409(7) . ? C4 C5 1.429(8) . ? C5 C6 1.326(10) . ? C5 H5 0.9500 . ? C6 C7 1.441(9) . ? C6 H6 0.9500 . ? C7 C8 1.394(9) . ? C7 C11 1.422(6) . ? C8 C9 1.359(9) . ? C8 H8 0.9500 . ? C9 C10 1.405(8) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.446(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? N3 C21 1.331(9) . ? N3 C32 1.357(9) . ? N4 C30 1.328(9) . ? N4 C31 1.363(9) . ? C21 C22 1.401(10) . ? C21 H21 0.9500 . ? C22 C23 1.359(12) . ? C22 H22 0.9500 . ? C23 C24 1.399(12) . ? C23 H23 0.9500 . ? C24 C32 1.410(10) . ? C24 C25 1.430(11) . ? C25 C26 1.326(13) . ? C25 H25 0.9500 . ? C26 C27 1.440(12) . ? C26 H26 0.9500 . ? C27 C28 1.392(12) . ? C27 C31 1.422(9) . ? C28 C29 1.360(12) . ? C28 H28 0.9500 . ? C29 C30 1.403(10) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.442(10) . ? N3A C21A 1.331(8) . ? N3A C32A 1.359(8) . ? N4A C30A 1.328(8) . ? N4A C31A 1.366(8) . ? C21A C22A 1.401(9) . ? C21A H21B 0.9500 . ? C22A C23A 1.361(11) . ? C22A H22A 0.9500 . ? C23A C24A 1.399(11) . ? C23A H23A 0.9500 . ? C24A C32A 1.413(8) . ? C24A C25A 1.435(11) . ? C25A C26A 1.329(12) . ? C25A H25A 0.9500 . ? C26A C27A 1.439(10) . ? C26A H26A 0.9500 . ? C27A C28A 1.391(11) . ? C27A C31A 1.423(8) . ? C28A C29A 1.360(11) . ? C28A H28A 0.9500 . ? C29A C30A 1.401(9) . ? C29A H29A 0.9500 . ? C30A H30A 0.9500 . ? C31A C32A 1.443(9) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Yb1 N2 67.01(14) . . ? N1 Yb1 Al2 133.46(11) . . ? N2 Yb1 Al2 100.37(11) . . ? N1 Yb1 Al1 95.90(11) . . ? N2 Yb1 Al1 131.45(11) . . ? Al2 Yb1 Al1 121.31(4) . . ? N4A Yb2 N3A 67.6(3) . . ? N4A Yb2 N3 75.6(5) . . ? N3A Yb2 N3 8.0(6) . . ? N4A Yb2 N4 9.2(4) . . ? N3A Yb2 N4 58.5(4) . . ? N3 Yb2 N4 66.5(5) . . ? N4A Yb2 Al3 132.2(5) . . ? N3A Yb2 Al3 100.9(6) . . ? N3 Yb2 Al3 95.3(11) . . ? N4 Yb2 Al3 132.3(9) . . ? N4A Yb2 Al4 95.1(4) . . ? N3A Yb2 Al4 132.4(8) . . ? N3 Yb2 Al4 134.2(15) . . ? N4 Yb2 Al4 100.2(7) . . ? Al3 Yb2 Al4 121.21(5) . . ? C15 Al1 C16 116.3(3) . . ? C15 Al1 C14 109.2(3) . . ? C16 Al1 C14 107.5(3) . . ? C15 Al1 C13 104.5(3) . . ? C16 Al1 C13 108.0(3) . . ? C14 Al1 C13 111.4(2) . . ? C15 Al1 Yb1 122.2(2) . . ? C16 Al1 Yb1 121.4(2) . . ? C14 Al1 Yb1 55.82(16) . . ? C13 Al1 Yb1 55.62(15) . . ? C19 Al2 C20 116.4(3) . . ? C19 Al2 C18 109.5(3) . . ? C20 Al2 C18 107.0(3) . . ? C19 Al2 C17 104.8(3) . . ? C20 Al2 C17 107.8(3) . . ? C18 Al2 C17 111.5(2) . . ? C19 Al2 Yb1 124.8(2) . . ? C20 Al2 Yb1 118.7(2) . . ? C18 Al2 Yb1 55.90(17) . . ? C17 Al2 Yb1 55.69(15) . . ? C35 Al3 C36 116.9(3) . . ? C35 Al3 C34 108.6(3) . . ? C36 Al3 C34 107.3(3) . . ? C35 Al3 C33 104.0(3) . . ? C36 Al3 C33 108.3(3) . . ? C34 Al3 C33 111.9(2) . . ? C35 Al3 Yb2 124.6(2) . . ? C36 Al3 Yb2 118.5(2) . . ? C34 Al3 Yb2 56.21(17) . . ? C33 Al3 Yb2 55.97(16) . . ? C39 Al4 C40 115.0(3) . . ? C39 Al4 C38 110.3(3) . . ? C40 Al4 C38 106.7(3) . . ? C39 Al4 C37 105.2(3) . . ? C40 Al4 C37 107.9(3) . . ? C38 Al4 C37 111.7(3) . . ? C39 Al4 Yb2 123.7(3) . . ? C40 Al4 Yb2 121.2(2) . . ? C38 Al4 Yb2 55.65(18) . . ? C37 Al4 Yb2 56.07(16) . . ? C1 N1 C12 118.1(5) . . ? C1 N1 Yb1 123.7(3) . . ? C12 N1 Yb1 118.0(3) . . ? N1 C1 C2 123.6(6) . . ? N1 C1 H1A 118.2 . . ? C2 C1 H1A 118.2 . . ? C10 N2 C11 117.9(5) . . ? C10 N2 Yb1 124.6(4) . . ? C11 N2 Yb1 117.5(3) . . ? C3 C2 C1 118.5(6) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 119.8(5) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C12 118.3(5) . . ? C3 C4 C5 122.3(6) . . ? C12 C4 C5 119.3(6) . . ? C6 C5 C4 120.9(6) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 122.6(6) . . ? C5 C6 H6 118.7 . . ? C7 C6 H6 118.7 . . ? C8 C7 C11 117.7(6) . . ? C8 C7 C6 124.1(6) . . ? C11 C7 C6 118.2(6) . . ? C9 C8 C7 120.0(6) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 119.1(6) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N2 C10 C9 123.2(6) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? N2 C11 C7 122.0(5) . . ? N2 C11 C12 119.0(4) . . ? C7 C11 C12 118.9(5) . . ? N1 C12 C4 121.6(5) . . ? N1 C12 C11 118.4(4) . . ? C4 C12 C11 120.0(5) . . ? Al1 C13 H13A 109.5 . . ? Al1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Al1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Al1 C14 H14A 109.5 . . ? Al1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Al1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Al1 C15 H15A 109.5 . . ? Al1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Al1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Al1 C16 H16A 109.5 . . ? Al1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Al1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Al2 C17 H17A 109.5 . . ? Al2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Al2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Al2 C18 H18A 109.5 . . ? Al2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Al2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Al2 C19 H19A 109.5 . . ? Al2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Al2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Al2 C20 H20A 109.5 . . ? Al2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Al2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21 N3 C32 117(2) . . ? C21 N3 Yb2 124.7(16) . . ? C32 N3 Yb2 118.3(15) . . ? C30 N4 C31 120.2(18) . . ? C30 N4 Yb2 122.8(12) . . ? C31 N4 Yb2 117.0(12) . . ? N3 C21 C22 124(2) . . ? N3 C21 H21 118.2 . . ? C22 C21 H21 118.2 . . ? C23 C22 C21 119(2) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? C22 C23 C24 120.4(19) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C32 116.8(16) . . ? C23 C24 C25 123.2(18) . . ? C32 C24 C25 119.5(19) . . ? C26 C25 C24 122(2) . . ? C26 C25 H25 118.8 . . ? C24 C25 H25 118.8 . . ? C25 C26 C27 122(2) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C28 C27 C31 119.3(15) . . ? C28 C27 C26 123.9(16) . . ? C31 C27 C26 116.7(16) . . ? C29 C28 C27 120.6(16) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 117.7(17) . . ? C28 C29 H29 121.2 . . ? C30 C29 H29 121.2 . . ? N4 C30 C29 123.1(17) . . ? N4 C30 H30 118.4 . . ? C29 C30 H30 118.4 . . ? N4 C31 C27 118.9(16) . . ? N4 C31 C32 118.9(15) . . ? C27 C31 C32 122.2(16) . . ? N3 C32 C24 123.4(19) . . ? N3 C32 C31 119.3(17) . . ? C24 C32 C31 117.3(18) . . ? C21A N3A C32A 118.3(12) . . ? C21A N3A Yb2 124.4(8) . . ? C32A N3A Yb2 117.2(8) . . ? C30A N4A C31A 117.7(9) . . ? C30A N4A Yb2 124.5(7) . . ? C31A N4A Yb2 117.7(6) . . ? N3A C21A C22A 122.5(12) . . ? N3A C21A H21B 118.7 . . ? C22A C21A H21B 118.7 . . ? C23A C22A C21A 119.3(11) . . ? C23A C22A H22A 120.3 . . ? C21A C22A H22A 120.3 . . ? C22A C23A C24A 120.0(10) . . ? C22A C23A H23A 120.0 . . ? C24A C23A H23A 120.0 . . ? C23A C24A C32A 117.3(9) . . ? C23A C24A C25A 123.3(10) . . ? C32A C24A C25A 119.4(10) . . ? C26A C25A C24A 121.3(11) . . ? C26A C25A H25A 119.4 . . ? C24A C25A H25A 119.4 . . ? C25A C26A C27A 121.8(10) . . ? C25A C26A H26A 119.1 . . ? C27A C26A H26A 119.1 . . ? C28A C27A C31A 118.3(8) . . ? C28A C27A C26A 122.9(9) . . ? C31A C27A C26A 118.8(9) . . ? C29A C28A C27A 119.8(9) . . ? C29A C28A H28A 120.1 . . ? C27A C28A H28A 120.1 . . ? C28A C29A C30A 118.8(9) . . ? C28A C29A H29A 120.6 . . ? C30A C29A H29A 120.6 . . ? N4A C30A C29A 123.8(10) . . ? N4A C30A H30A 118.1 . . ? C29A C30A H30A 118.1 . . ? N4A C31A C27A 121.5(9) . . ? N4A C31A C32A 119.3(8) . . ? C27A C31A C32A 119.1(8) . . ? N3A C32A C24A 122.5(10) . . ? N3A C32A C31A 118.0(9) . . ? C24A C32A C31A 119.4(9) . . ? Al3 C33 H33A 109.5 . . ? Al3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Al3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Al3 C34 H34A 109.5 . . ? Al3 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Al3 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Al3 C35 H35A 109.5 . . ? Al3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Al3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Al3 C36 H36A 109.5 . . ? Al3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Al3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Al4 C37 H37A 109.5 . . ? Al4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Al4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Al4 C38 H38A 109.5 . . ? Al4 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Al4 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Al4 C39 H39A 109.5 . . ? Al4 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Al4 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Al4 C40 H40A 109.5 . . ? Al4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Al4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Yb1 Al1 C15 -9.6(3) . . . . ? N2 Yb1 Al1 C15 -74.0(3) . . . . ? Al2 Yb1 Al1 C15 141.1(3) . . . . ? N1 Yb1 Al1 C16 173.4(3) . . . . ? N2 Yb1 Al1 C16 109.1(3) . . . . ? Al2 Yb1 Al1 C16 -35.9(3) . . . . ? N1 Yb1 Al1 C14 82.8(2) . . . . ? N2 Yb1 Al1 C14 18.4(2) . . . . ? Al2 Yb1 Al1 C14 -126.49(19) . . . . ? N1 Yb1 Al1 C13 -95.4(2) . . . . ? N2 Yb1 Al1 C13 -159.8(2) . . . . ? Al2 Yb1 Al1 C13 55.28(19) . . . . ? N1 Yb1 Al2 C19 -80.8(3) . . . . ? N2 Yb1 Al2 C19 -12.7(3) . . . . ? Al1 Yb1 Al2 C19 141.3(3) . . . . ? N1 Yb1 Al2 C20 102.2(3) . . . . ? N2 Yb1 Al2 C20 170.2(3) . . . . ? Al1 Yb1 Al2 C20 -35.7(3) . . . . ? N1 Yb1 Al2 C18 10.3(3) . . . . ? N2 Yb1 Al2 C18 78.4(2) . . . . ? Al1 Yb1 Al2 C18 -127.6(2) . . . . ? N1 Yb1 Al2 C17 -165.2(2) . . . . ? N2 Yb1 Al2 C17 -97.1(2) . . . . ? Al1 Yb1 Al2 C17 56.9(2) . . . . ? N4A Yb2 Al3 C35 83.4(4) . . . . ? N3A Yb2 Al3 C35 13.9(7) . . . . ? N3 Yb2 Al3 C35 8.0(12) . . . . ? N4 Yb2 Al3 C35 70.9(6) . . . . ? Al4 Yb2 Al3 C35 -143.0(3) . . . . ? N4A Yb2 Al3 C36 -99.3(3) . . . . ? N3A Yb2 Al3 C36 -168.8(7) . . . . ? N3 Yb2 Al3 C36 -174.7(12) . . . . ? N4 Yb2 Al3 C36 -111.8(6) . . . . ? Al4 Yb2 Al3 C36 34.3(3) . . . . ? N4A Yb2 Al3 C34 -6.8(3) . . . . ? N3A Yb2 Al3 C34 -76.3(7) . . . . ? N3 Yb2 Al3 C34 -82.2(12) . . . . ? N4 Yb2 Al3 C34 -19.3(5) . . . . ? Al4 Yb2 Al3 C34 126.78(19) . . . . ? N4A Yb2 Al3 C33 167.0(3) . . . . ? N3A Yb2 Al3 C33 97.5(7) . . . . ? N3 Yb2 Al3 C33 91.6(12) . . . . ? N4 Yb2 Al3 C33 154.5(5) . . . . ? Al4 Yb2 Al3 C33 -59.4(2) . . . . ? N4A Yb2 Al4 C39 8.7(5) . . . . ? N3A Yb2 Al4 C39 72.8(6) . . . . ? N3 Yb2 Al4 C39 83.6(8) . . . . ? N4 Yb2 Al4 C39 16.5(7) . . . . ? Al3 Yb2 Al4 C39 -138.7(3) . . . . ? N4A Yb2 Al4 C40 -173.8(4) . . . . ? N3A Yb2 Al4 C40 -109.7(5) . . . . ? N3 Yb2 Al4 C40 -98.9(8) . . . . ? N4 Yb2 Al4 C40 -166.0(7) . . . . ? Al3 Yb2 Al4 C40 38.8(3) . . . . ? N4A Yb2 Al4 C38 -84.1(4) . . . . ? N3A Yb2 Al4 C38 -20.0(5) . . . . ? N3 Yb2 Al4 C38 -9.2(7) . . . . ? N4 Yb2 Al4 C38 -76.3(7) . . . . ? Al3 Yb2 Al4 C38 128.5(2) . . . . ? N4A Yb2 Al4 C37 94.7(4) . . . . ? N3A Yb2 Al4 C37 158.8(5) . . . . ? N3 Yb2 Al4 C37 169.6(7) . . . . ? N4 Yb2 Al4 C37 102.5(7) . . . . ? Al3 Yb2 Al4 C37 -52.7(2) . . . . ? N2 Yb1 N1 C1 177.1(5) . . . . ? Al2 Yb1 N1 C1 -100.6(5) . . . . ? Al1 Yb1 N1 C1 44.3(5) . . . . ? N2 Yb1 N1 C12 1.8(4) . . . . ? Al2 Yb1 N1 C12 84.2(4) . . . . ? Al1 Yb1 N1 C12 -131.0(4) . . . . ? C12 N1 C1 C2 -0.3(9) . . . . ? Yb1 N1 C1 C2 -175.6(5) . . . . ? N1 Yb1 N2 C10 177.2(5) . . . . ? Al2 Yb1 N2 C10 44.2(5) . . . . ? Al1 Yb1 N2 C10 -105.8(5) . . . . ? N1 Yb1 N2 C11 -0.1(4) . . . . ? Al2 Yb1 N2 C11 -133.1(4) . . . . ? Al1 Yb1 N2 C11 76.9(4) . . . . ? N1 C1 C2 C3 0.2(10) . . . . ? C1 C2 C3 C4 -0.7(10) . . . . ? C2 C3 C4 C12 1.4(9) . . . . ? C2 C3 C4 C5 179.8(6) . . . . ? C3 C4 C5 C6 179.7(7) . . . . ? C12 C4 C5 C6 -1.9(10) . . . . ? C4 C5 C6 C7 2.9(11) . . . . ? C5 C6 C7 C8 179.5(7) . . . . ? C5 C6 C7 C11 -1.9(10) . . . . ? C11 C7 C8 C9 2.7(10) . . . . ? C6 C7 C8 C9 -178.7(7) . . . . ? C7 C8 C9 C10 -1.2(10) . . . . ? C11 N2 C10 C9 -1.7(9) . . . . ? Yb1 N2 C10 C9 -179.0(5) . . . . ? C8 C9 C10 N2 0.7(10) . . . . ? C10 N2 C11 C7 3.3(8) . . . . ? Yb1 N2 C11 C7 -179.2(4) . . . . ? C10 N2 C11 C12 -179.0(5) . . . . ? Yb1 N2 C11 C12 -1.6(6) . . . . ? C8 C7 C11 N2 -3.8(9) . . . . ? C6 C7 C11 N2 177.5(6) . . . . ? C8 C7 C11 C12 178.5(5) . . . . ? C6 C7 C11 C12 -0.2(8) . . . . ? C1 N1 C12 C4 1.1(8) . . . . ? Yb1 N1 C12 C4 176.6(4) . . . . ? C1 N1 C12 C11 -178.9(5) . . . . ? Yb1 N1 C12 C11 -3.3(6) . . . . ? C3 C4 C12 N1 -1.6(8) . . . . ? C5 C4 C12 N1 179.9(5) . . . . ? C3 C4 C12 C11 178.3(5) . . . . ? C5 C4 C12 C11 -0.1(8) . . . . ? N2 C11 C12 N1 3.3(7) . . . . ? C7 C11 C12 N1 -179.0(5) . . . . ? N2 C11 C12 C4 -176.6(5) . . . . ? C7 C11 C12 C4 1.1(8) . . . . ? N4A Yb2 N3 C21 -178(6) . . . . ? N3A Yb2 N3 C21 -180(22) . . . . ? N4 Yb2 N3 C21 -180(6) . . . . ? Al3 Yb2 N3 C21 -46(6) . . . . ? Al4 Yb2 N3 C21 99(5) . . . . ? N4A Yb2 N3 C32 4(4) . . . . ? N3A Yb2 N3 C32 2(13) . . . . ? N4 Yb2 N3 C32 2(4) . . . . ? Al3 Yb2 N3 C32 136(4) . . . . ? Al4 Yb2 N3 C32 -79(5) . . . . ? N4A Yb2 N4 C30 11(6) . . . . ? N3A Yb2 N4 C30 180(4) . . . . ? N3 Yb2 N4 C30 180(4) . . . . ? Al3 Yb2 N4 C30 105(3) . . . . ? Al4 Yb2 N4 C30 -46(3) . . . . ? N4A Yb2 N4 C31 -171(11) . . . . ? N3A Yb2 N4 C31 -2(2) . . . . ? N3 Yb2 N4 C31 -2(3) . . . . ? Al3 Yb2 N4 C31 -77(3) . . . . ? Al4 Yb2 N4 C31 132(3) . . . . ? C32 N3 C21 C22 1(9) . . . . ? Yb2 N3 C21 C22 -177(3) . . . . ? N3 C21 C22 C23 -3(7) . . . . ? C21 C22 C23 C24 2(5) . . . . ? C22 C23 C24 C32 1(4) . . . . ? C22 C23 C24 C25 173(3) . . . . ? C23 C24 C25 C26 -177(3) . . . . ? C32 C24 C25 C26 -6(4) . . . . ? C24 C25 C26 C27 2(5) . . . . ? C25 C26 C27 C28 -178(3) . . . . ? C25 C26 C27 C31 0(4) . . . . ? C31 C27 C28 C29 3(3) . . . . ? C26 C27 C28 C29 -179(2) . . . . ? C27 C28 C29 C30 -3(4) . . . . ? C31 N4 C30 C29 -3(5) . . . . ? Yb2 N4 C30 C29 175(2) . . . . ? C28 C29 C30 N4 3(4) . . . . ? C30 N4 C31 C27 3(5) . . . . ? Yb2 N4 C31 C27 -175.0(18) . . . . ? C30 N4 C31 C32 -180(3) . . . . ? Yb2 N4 C31 C32 2(4) . . . . ? C28 C27 C31 N4 -3(4) . . . . ? C26 C27 C31 N4 179(3) . . . . ? C28 C27 C31 C32 180(2) . . . . ? C26 C27 C31 C32 2(4) . . . . ? C21 N3 C32 C24 2(8) . . . . ? Yb2 N3 C32 C24 -179(2) . . . . ? C21 N3 C32 C31 -180(4) . . . . ? Yb2 N3 C32 C31 -1(6) . . . . ? C23 C24 C32 N3 -3(5) . . . . ? C25 C24 C32 N3 -175(4) . . . . ? C23 C24 C32 C31 179(3) . . . . ? C25 C24 C32 C31 7(4) . . . . ? N4 C31 C32 N3 -1(5) . . . . ? C27 C31 C32 N3 177(4) . . . . ? N4 C31 C32 C24 177(3) . . . . ? C27 C31 C32 C24 -5(4) . . . . ? N4A Yb2 N3A C21A -176(3) . . . . ? N3 Yb2 N3A C21A 2(15) . . . . ? N4 Yb2 N3A C21A -178(4) . . . . ? Al3 Yb2 N3A C21A -45(3) . . . . ? Al4 Yb2 N3A C21A 108(3) . . . . ? N4A Yb2 N3A C32A 3(2) . . . . ? N3 Yb2 N3A C32A -179(19) . . . . ? N4 Yb2 N3A C32A 1(2) . . . . ? Al3 Yb2 N3A C32A 134(2) . . . . ? Al4 Yb2 N3A C32A -73(3) . . . . ? N3A Yb2 N4A C30A -178(2) . . . . ? N3 Yb2 N4A C30A -178(2) . . . . ? N4 Yb2 N4A C30A -168(10) . . . . ? Al3 Yb2 N4A C30A 97.6(17) . . . . ? Al4 Yb2 N4A C30A -43.9(17) . . . . ? N3A Yb2 N4A C31A -3.4(16) . . . . ? N3 Yb2 N4A C31A -4(2) . . . . ? N4 Yb2 N4A C31A 7(7) . . . . ? Al3 Yb2 N4A C31A -87.7(15) . . . . ? Al4 Yb2 N4A C31A 130.7(14) . . . . ? C32A N3A C21A C22A -1(5) . . . . ? Yb2 N3A C21A C22A 177.7(18) . . . . ? N3A C21A C22A C23A 2(4) . . . . ? C21A C22A C23A C24A -2(2) . . . . ? C22A C23A C24A C32A 1(2) . . . . ? C22A C23A C24A C25A 179.9(14) . . . . ? C23A C24A C25A C26A -179.7(14) . . . . ? C32A C24A C25A C26A -1(2) . . . . ? C24A C25A C26A C27A -3(2) . . . . ? C25A C26A C27A C28A -178.2(13) . . . . ? C25A C26A C27A C31A 2.7(18) . . . . ? C31A C27A C28A C29A -2.2(17) . . . . ? C26A C27A C28A C29A 178.7(11) . . . . ? C27A C28A C29A C30A 2.1(19) . . . . ? C31A N4A C30A C29A 1(3) . . . . ? Yb2 N4A C30A C29A 175.5(12) . . . . ? C28A C29A C30A N4A -1(2) . . . . ? C30A N4A C31A C27A -1(3) . . . . ? Yb2 N4A C31A C27A -176.1(10) . . . . ? C30A N4A C31A C32A 178.8(16) . . . . ? Yb2 N4A C31A C32A 4(2) . . . . ? C28A C27A C31A N4A 2(2) . . . . ? C26A C27A C31A N4A -179.1(15) . . . . ? C28A C27A C31A C32A -178.1(12) . . . . ? C26A C27A C31A C32A 1.0(18) . . . . ? C21A N3A C32A C24A 0(4) . . . . ? Yb2 N3A C32A C24A -178.8(13) . . . . ? C21A N3A C32A C31A 177(3) . . . . ? Yb2 N3A C32A C31A -2(3) . . . . ? C23A C24A C32A N3A 0(3) . . . . ? C25A C24A C32A N3A -179(2) . . . . ? C23A C24A C32A C31A -176.6(14) . . . . ? C25A C24A C32A C31A 4(2) . . . . ? N4A C31A C32A N3A -1(3) . . . . ? C27A C31A C32A N3A 179(2) . . . . ? N4A C31A C32A C24A 175.7(16) . . . . ? C27A C31A C32A C24A -5(2) . . . . ? # # END of CIF for compound 3b # # Attachment 'Compound4b.cif' #Project name HMS57 Prepared by KWT October 2007 data_Compound4b _database_code_depnum_ccdc_archive 'CCDC 664736' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H47 O4 Yb, C4 H12 Al' _chemical_formula_sum 'C30 H59 Al O4 Yb' _chemical_formula_weight 683.79 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_HALL '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6603(6) _cell_length_b 11.1847(7) _cell_length_c 15.1345(9) _cell_angle_alpha 81.305(1) _cell_angle_beta 79.778(1) _cell_angle_gamma 71.997(1) _cell_volume 1679.96(17) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 15098 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 29.99 _exptl_crystal_description lath _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 2.838 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6755 _exptl_absorpt_correction_T_max 0.8711 _exptl_absorpt_process_details ; Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, Wisconsin, USA. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS SMART 2K CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean '48 \um' _diffrn_standards_number 433 _diffrn_standards_interval_count 1 _diffrn_standards_interval_time '28 h' _diffrn_standards_decay_% 0 _diffrn_reflns_number 28265 _diffrn_reflns_av_R_equivalents 0.0651 _diffrn_reflns_av_sigmaI/netI 0.0795 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 30.04 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.994 _reflns_number_total 9765 _reflns_number_gt 7749 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; Bruker (1999). SMART, version 5.059, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_cell_refinement ; Bruker (2001). SAINT, version 6.02a, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_data_reduction ; Bruker (2001). SAINT, version 6.02a, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_structure_solution ; Altomare, A. et al. (1994). SIR92. J. Appl. Cryst. 27, 435. ; _computing_structure_refinement ; Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of G\"ottingen, Germany. ; _computing_molecular_graphics ; Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_publication_material ; Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, Wisconsin, USA. ; _refine_special_details ; The Cp-star group is rotationally disordered in two positions (49:51). One THF is partially disordered (C11-14, O1). Atom C13a was refined isotropically whilst atom C13 was refined anisotropically. Distance constraints (SADI 0.01) were applied within this THF molecule. All H-atoms of CH(2) groups were put in their geometric positions (AFIX 23) with U~iso~ set to be 1.2 that of the parent carbon atom. Equally the methyl group H-atoms were put in their geometric positions (AFIX 33) with U~iso~ set to be 1.5 that of the parent carbon atom. Largest positive residual density peak (11.31 \%A^3^) was situated 0.96 \%A from Yb1. Largest negative residual density peak (-1.85 \%A^3^) was located 0.79 \%A from Yb1. 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. COMMENT on checkCIF alerts: The A alert pertains to a disordered THF molecule where atom C13A in the minor component has been refined isotropically in contrast to C13 in the main component which is anistropically refined. The top B alerts stem from the fact that the crystal was pseudo-merohedrally twinned. The deconvolution of the two components was as expected rather poor for the low order reflections. The numerical absorption correction was consequently also not of the best quality. All of this is reflected also in a relatively high wR2 value. The Cp-star disorder also triggers some C-alerts. ; _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^)+(0.1773P)^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 9765 _refine_ls_number_parameters 358 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.1054 _refine_ls_R_factor_gt 0.0842 _refine_ls_wR_factor_ref 0.2419 _refine_ls_wR_factor_gt 0.2245 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 11.309 _refine_diff_density_min -1.847 _refine_diff_density_rms 0.390 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.28775(3) 0.77895(3) 0.70342(2) 0.02134(13) Uani 1 1 d . . . Al1 Al -0.1101(3) 0.3782(3) 0.8328(2) 0.0326(6) Uani 1 1 d . . . O1 O 0.3585(6) 0.8163(6) 0.8384(4) 0.0297(13) Uani 1 1 d . A . O2 O 0.3774(7) 0.5660(6) 0.7708(5) 0.0321(14) Uani 1 1 d . A . O3 O 0.1456(7) 0.6671(6) 0.6641(4) 0.0315(14) Uani 1 1 d . A . O4 O 0.0745(6) 0.8947(6) 0.7760(5) 0.0320(14) Uani 1 1 d . A . C1 C 0.3046(19) 0.9707(14) 0.5839(12) 0.021(2) Uani 0.490(6) 1 d PD A 1 C2 C 0.422(2) 0.929(2) 0.6200(12) 0.024(3) Uani 0.490(6) 1 d PD A 1 C3 C 0.4935(15) 0.8056(17) 0.5955(12) 0.021(2) Uani 0.490(6) 1 d PD A 1 C4 C 0.4171(19) 0.7737(15) 0.5418(11) 0.020(2) Uani 0.490(6) 1 d PD A 1 C5 C 0.2995(18) 0.8766(18) 0.5339(11) 0.022(2) Uani 0.490(6) 1 d PD A 1 C6 C 0.205(2) 1.1001(15) 0.5888(14) 0.042(4) Uani 0.490(6) 1 d PD A 1 H6A H 0.2291 1.1581 0.5382 0.063 Uiso 0.490(6) 1 calc PR A 1 H6B H 0.2041 1.1318 0.6458 0.063 Uiso 0.490(6) 1 calc PR A 1 H6C H 0.1156 1.0942 0.5857 0.063 Uiso 0.490(6) 1 calc PR A 1 C7 C 0.479(2) 1.008(2) 0.6655(13) 0.044(4) Uani 0.490(6) 1 d PD A 1 H7A H 0.5274 1.0558 0.6195 0.065 Uiso 0.490(6) 1 calc PR A 1 H7B H 0.5410 0.9527 0.7056 0.065 Uiso 0.490(6) 1 calc PR A 1 H7C H 0.4071 1.0671 0.7008 0.065 Uiso 0.490(6) 1 calc PR A 1 C8 C 0.6327(17) 0.728(2) 0.6117(17) 0.046(4) Uani 0.490(6) 1 d PD A 1 H8A H 0.6974 0.7512 0.5630 0.070 Uiso 0.490(6) 1 calc PR A 1 H8B H 0.6409 0.6379 0.6129 0.070 Uiso 0.490(6) 1 calc PR A 1 H8C H 0.6500 0.7440 0.6696 0.070 Uiso 0.490(6) 1 calc PR A 1 C9 C 0.459(2) 0.6593(19) 0.4893(13) 0.041(3) Uani 0.490(6) 1 d PD A 1 H9A H 0.5064 0.6788 0.4299 0.061 Uiso 0.490(6) 1 calc PR A 1 H9B H 0.3794 0.6373 0.4816 0.061 Uiso 0.490(6) 1 calc PR A 1 H9C H 0.5172 0.5878 0.5224 0.061 Uiso 0.490(6) 1 calc PR A 1 C10 C 0.198(2) 0.886(2) 0.4720(14) 0.045(4) Uani 0.490(6) 1 d PD A 1 H10A H 0.2243 0.9252 0.4122 0.067 Uiso 0.490(6) 1 calc PR A 1 H10B H 0.1100 0.9366 0.4974 0.067 Uiso 0.490(6) 1 calc PR A 1 H10C H 0.1941 0.8005 0.4666 0.067 Uiso 0.490(6) 1 calc PR A 1 C1A C 0.375(2) 0.9734(14) 0.6000(11) 0.021(2) Uani 0.510(6) 1 d PD A 2 C2A C 0.4916(17) 0.873(2) 0.6069(11) 0.024(3) Uani 0.510(6) 1 d PD A 2 C3A C 0.4859(16) 0.7761(15) 0.5604(11) 0.021(2) Uani 0.510(6) 1 d PD A 2 C4A C 0.3680(19) 0.8178(17) 0.5215(10) 0.020(2) Uani 0.510(6) 1 d PD A 2 C5A C 0.2988(15) 0.9428(17) 0.5473(12) 0.022(2) Uani 0.510(6) 1 d PD A 2 C6A C 0.346(2) 1.1016(15) 0.6331(13) 0.042(4) Uani 0.510(6) 1 d PD A 2 H6AA H 0.3863 1.1560 0.5872 0.063 Uiso 0.510(6) 1 calc PR A 2 H6AB H 0.3846 1.0916 0.6891 0.063 Uiso 0.510(6) 1 calc PR A 2 H6AC H 0.2499 1.1402 0.6445 0.063 Uiso 0.510(6) 1 calc PR A 2 C7A C 0.6089(19) 0.874(2) 0.6504(13) 0.044(4) Uani 0.510(6) 1 d PD A 2 H7AA H 0.6689 0.9113 0.6062 0.065 Uiso 0.510(6) 1 calc PR A 2 H7AB H 0.6571 0.7873 0.6713 0.065 Uiso 0.510(6) 1 calc PR A 2 H7AC H 0.5764 0.9243 0.7019 0.065 Uiso 0.510(6) 1 calc PR A 2 C8A C 0.595(2) 0.6541(19) 0.5429(17) 0.046(4) Uani 0.510(6) 1 d PD A 2 H8AA H 0.6572 0.6693 0.4893 0.070 Uiso 0.510(6) 1 calc PR A 2 H8AB H 0.5557 0.5898 0.5330 0.070 Uiso 0.510(6) 1 calc PR A 2 H8AC H 0.6436 0.6244 0.5952 0.070 Uiso 0.510(6) 1 calc PR A 2 C9A C 0.329(2) 0.752(2) 0.4536(12) 0.041(3) Uani 0.510(6) 1 d PD A 2 H9AA H 0.3653 0.7799 0.3923 0.061 Uiso 0.510(6) 1 calc PR A 2 H9AB H 0.2321 0.7749 0.4590 0.061 Uiso 0.510(6) 1 calc PR A 2 H9AC H 0.3658 0.6607 0.4657 0.061 Uiso 0.510(6) 1 calc PR A 2 C10A C 0.1752(18) 1.029(2) 0.5098(15) 0.045(4) Uani 0.510(6) 1 d PD A 2 H10D H 0.2016 1.0795 0.4548 0.067 Uiso 0.510(6) 1 calc PR A 2 H10E H 0.1216 1.0862 0.5548 0.067 Uiso 0.510(6) 1 calc PR A 2 H10F H 0.1226 0.9785 0.4957 0.067 Uiso 0.510(6) 1 calc PR A 2 C11 C 0.4821(10) 0.7451(10) 0.8717(7) 0.034(2) Uani 1 1 d . . . H11A H 0.5480 0.7048 0.8221 0.041 Uiso 1 1 calc R A . H11B H 0.4669 0.6780 0.9194 0.041 Uiso 1 1 calc R . . C12 C 0.5319(14) 0.8332(11) 0.9085(11) 0.068(4) Uani 1 1 d D A . H12A H 0.6210 0.8341 0.8763 0.081 Uiso 1 1 calc R B 3 H12B H 0.5385 0.8084 0.9735 0.081 Uiso 1 1 calc R B 3 C13 C 0.4293(18) 0.9649(16) 0.8941(19) 0.041(9) Uani 0.40(5) 1 d PD A 3 H13A H 0.4123 1.0115 0.9477 0.049 Uiso 0.40(5) 1 calc PR A 3 H13B H 0.4621 1.0157 0.8407 0.049 Uiso 0.40(5) 1 calc PR A 3 C13A C 0.4165(10) 0.9332(10) 0.9301(8) 0.079(10) Uiso 0.60(5) 1 d PD A 4 H13C H 0.4387 1.0142 0.9152 0.095 Uiso 0.60(5) 1 calc PR A 4 H13D H 0.3867 0.9236 0.9959 0.095 Uiso 0.60(5) 1 calc PR A 4 C14 C 0.3016(10) 0.9378(10) 0.8792(8) 0.045(3) Uani 1 1 d RD . . H14A H 0.2434 0.9284 0.9370 0.054 Uiso 1 1 calc R A 3 H14B H 0.2509 1.0049 0.8376 0.054 Uiso 1 1 calc R A 3 C15 C 0.2927(11) 0.5230(11) 0.8487(6) 0.038(2) Uani 1 1 d . . . H15A H 0.2070 0.5244 0.8312 0.046 Uiso 1 1 calc R A . H15B H 0.2741 0.5782 0.8977 0.046 Uiso 1 1 calc R . . C16 C 0.3709(12) 0.3880(11) 0.8796(9) 0.049(3) Uani 1 1 d . A . H16A H 0.4248 0.3870 0.9269 0.059 Uiso 1 1 calc R . . H16B H 0.3107 0.3350 0.9031 0.059 Uiso 1 1 calc R . . C17 C 0.4574(13) 0.3441(11) 0.7952(10) 0.055(3) Uani 1 1 d . . . H17A H 0.4082 0.3152 0.7570 0.067 Uiso 1 1 calc R A . H17B H 0.5373 0.2743 0.8087 0.067 Uiso 1 1 calc R . . C18 C 0.4955(11) 0.4624(10) 0.7488(8) 0.041(2) Uani 1 1 d . A . H18A H 0.5727 0.4710 0.7726 0.049 Uiso 1 1 calc R . . H18B H 0.5177 0.4591 0.6827 0.049 Uiso 1 1 calc R . . C19 C 0.1891(11) 0.5387(9) 0.6391(7) 0.037(2) Uani 1 1 d . . . H19A H 0.1674 0.4793 0.6907 0.045 Uiso 1 1 calc R A . H19B H 0.2865 0.5120 0.6194 0.045 Uiso 1 1 calc R . . C20 C 0.1143(13) 0.5419(11) 0.5624(7) 0.045(3) Uani 1 1 d . A . H20A H 0.1608 0.5691 0.5038 0.054 Uiso 1 1 calc R . . H20B H 0.1029 0.4582 0.5594 0.054 Uiso 1 1 calc R . . C21 C -0.0173(15) 0.6375(11) 0.5867(10) 0.060(4) Uani 1 1 d . . . H21A H -0.0798 0.5976 0.6276 0.072 Uiso 1 1 calc R A . H21B H -0.0582 0.6799 0.5321 0.072 Uiso 1 1 calc R . . C22 C 0.0193(13) 0.7300(9) 0.6337(8) 0.046(3) Uani 1 1 d . A . H22A H 0.0251 0.8054 0.5914 0.055 Uiso 1 1 calc R . . H22B H -0.0494 0.7577 0.6857 0.055 Uiso 1 1 calc R . . C23 C -0.0248(11) 1.0109(10) 0.7487(9) 0.044(2) Uani 1 1 d . . . H23A H -0.0298 1.0174 0.6834 0.052 Uiso 1 1 calc R A . H23B H -0.0018 1.0855 0.7611 0.052 Uiso 1 1 calc R . . C24 C -0.1530(13) 1.0043(13) 0.8024(10) 0.060(4) Uani 1 1 d . A . H24A H -0.1954 0.9550 0.7744 0.072 Uiso 1 1 calc R . . H24B H -0.2154 1.0898 0.8095 0.072 Uiso 1 1 calc R . . C25 C -0.1116(15) 0.9381(15) 0.8915(11) 0.073(5) Uani 1 1 d . . . H25A H -0.1791 0.8987 0.9263 0.087 Uiso 1 1 calc R A . H25B H -0.0963 0.9969 0.9284 0.087 Uiso 1 1 calc R . . C26 C 0.0179(10) 0.8385(12) 0.8615(7) 0.041(2) Uani 1 1 d . A . H26A H 0.0797 0.8190 0.9069 0.049 Uiso 1 1 calc R . . H26B H 0.0000 0.7596 0.8528 0.049 Uiso 1 1 calc R . . C27 C -0.2556(12) 0.3342(14) 0.9211(8) 0.052(3) Uani 1 1 d . . . H27A H -0.2450 0.3452 0.9821 0.077 Uiso 1 1 calc R . . H27B H -0.2514 0.2461 0.9183 0.077 Uiso 1 1 calc R . . H27C H -0.3419 0.3897 0.9063 0.077 Uiso 1 1 calc R . . C28 C 0.0650(12) 0.2638(11) 0.8678(9) 0.047(3) Uani 1 1 d . . . H28A H 0.0725 0.2760 0.9292 0.070 Uiso 1 1 calc R . . H28B H 0.1385 0.2842 0.8257 0.070 Uiso 1 1 calc R . . H28C H 0.0691 0.1756 0.8654 0.070 Uiso 1 1 calc R . . C29 C -0.1294(11) 0.3558(10) 0.7065(7) 0.036(2) Uani 1 1 d . . . H29A H -0.0579 0.3785 0.6636 0.053 Uiso 1 1 calc R . . H29B H -0.2159 0.4106 0.6913 0.053 Uiso 1 1 calc R . . H29C H -0.1239 0.2674 0.7031 0.053 Uiso 1 1 calc R . . C30 C -0.1206(12) 0.5577(11) 0.8431(8) 0.049(3) Uani 1 1 d . . . H30A H -0.1107 0.5661 0.9048 0.073 Uiso 1 1 calc R . . H30B H -0.2070 0.6134 0.8286 0.073 Uiso 1 1 calc R . . H30C H -0.0491 0.5813 0.8007 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.02475(19) 0.02299(19) 0.01862(19) -0.00447(12) -0.00738(12) -0.00679(13) Al1 0.0308(14) 0.0400(15) 0.0288(14) -0.0057(12) -0.0036(11) -0.0121(12) O1 0.031(3) 0.042(4) 0.021(3) -0.013(3) -0.007(2) -0.012(3) O2 0.031(3) 0.032(3) 0.028(3) 0.000(3) -0.006(3) -0.002(3) O3 0.046(4) 0.024(3) 0.032(3) -0.001(2) -0.020(3) -0.014(3) O4 0.026(3) 0.032(3) 0.036(4) -0.007(3) -0.002(3) -0.003(3) C1 0.033(7) 0.018(5) 0.013(5) 0.002(4) -0.004(5) -0.008(6) C2 0.027(7) 0.038(9) 0.017(5) 0.002(5) -0.011(6) -0.022(6) C3 0.024(5) 0.029(7) 0.017(7) 0.000(5) -0.005(5) -0.014(5) C4 0.029(9) 0.020(7) 0.014(6) 0.007(4) -0.006(5) -0.015(6) C5 0.027(5) 0.024(6) 0.018(5) 0.000(5) -0.006(4) -0.010(6) C6 0.066(10) 0.026(6) 0.026(6) 0.009(5) 0.004(6) -0.014(6) C7 0.047(8) 0.070(10) 0.027(7) 0.003(7) -0.002(6) -0.040(8) C8 0.031(7) 0.053(9) 0.049(9) -0.005(7) 0.007(6) -0.009(7) C9 0.061(9) 0.047(8) 0.025(6) -0.008(6) 0.012(6) -0.038(7) C10 0.035(7) 0.059(9) 0.043(8) 0.018(7) -0.011(6) -0.026(7) C1A 0.033(7) 0.018(5) 0.013(5) 0.002(4) -0.004(5) -0.008(6) C2A 0.027(7) 0.038(9) 0.017(5) 0.002(5) -0.011(6) -0.022(6) C3A 0.024(5) 0.029(7) 0.017(7) 0.000(5) -0.005(5) -0.014(5) C4A 0.029(9) 0.020(7) 0.014(6) 0.007(4) -0.006(5) -0.015(6) C5A 0.027(5) 0.024(6) 0.018(5) 0.000(5) -0.006(4) -0.010(6) C6A 0.066(10) 0.026(6) 0.026(6) 0.009(5) 0.004(6) -0.014(6) C7A 0.047(8) 0.070(10) 0.027(7) 0.003(7) -0.002(6) -0.040(8) C8A 0.031(7) 0.053(9) 0.049(9) -0.005(7) 0.007(6) -0.009(7) C9A 0.061(9) 0.047(8) 0.025(6) -0.008(6) 0.012(6) -0.038(7) C10A 0.035(7) 0.059(9) 0.043(8) 0.018(7) -0.011(6) -0.026(7) C11 0.032(5) 0.047(5) 0.028(4) -0.007(4) -0.006(4) -0.015(4) C12 0.075(9) 0.052(7) 0.095(11) 0.008(7) -0.059(9) -0.028(7) C13 0.07(2) 0.042(15) 0.035(15) 0.006(11) -0.033(13) -0.043(14) C14 0.036(5) 0.053(6) 0.052(7) -0.030(5) -0.009(5) -0.009(5) C15 0.049(6) 0.052(6) 0.013(4) 0.002(4) -0.005(4) -0.016(5) C16 0.042(6) 0.046(6) 0.064(8) 0.021(6) -0.024(5) -0.022(5) C17 0.046(6) 0.030(5) 0.079(9) 0.009(5) -0.016(6) 0.003(5) C18 0.041(5) 0.034(5) 0.043(6) -0.003(4) -0.003(4) -0.004(4) C19 0.052(6) 0.034(5) 0.032(5) -0.015(4) -0.011(4) -0.014(4) C20 0.074(8) 0.052(6) 0.029(5) -0.009(4) -0.014(5) -0.040(6) C21 0.086(10) 0.039(6) 0.077(9) -0.008(6) -0.058(8) -0.022(6) C22 0.065(7) 0.030(5) 0.057(7) 0.001(4) -0.045(6) -0.017(5) C23 0.039(5) 0.032(5) 0.056(7) -0.009(5) -0.012(5) 0.000(4) C24 0.039(6) 0.056(8) 0.075(9) -0.016(7) -0.016(6) 0.009(6) C25 0.049(8) 0.064(9) 0.076(10) -0.004(7) 0.015(7) 0.011(7) C26 0.031(5) 0.054(6) 0.033(5) -0.004(4) 0.006(4) -0.013(5) C27 0.045(6) 0.082(9) 0.040(6) -0.016(6) -0.006(5) -0.030(6) C28 0.042(6) 0.043(6) 0.054(7) -0.006(5) -0.015(5) -0.006(5) C29 0.040(5) 0.040(5) 0.028(4) -0.001(4) -0.004(4) -0.017(4) C30 0.047(6) 0.053(7) 0.047(6) -0.025(5) -0.010(5) -0.005(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 Yb1 O4 2.403(6) . ? Yb1 O2 2.415(7) . ? Yb1 O1 2.432(6) . ? Yb1 O3 2.436(6) . ? Yb1 C3 2.560(16) . ? Yb1 C2 2.578(17) . ? Yb1 C4 2.585(16) . ? Yb1 C1 2.618(15) . ? Yb1 C5 2.630(16) . ? Yb1 C3A 2.739(16) . ? Yb1 C4A 2.745(15) . ? Yb1 C5A 2.771(16) . ? Al1 C27 1.992(13) . ? Al1 C30 2.004(12) . ? Al1 C28 2.017(11) . ? Al1 C29 2.020(10) . ? O1 C11 1.446(11) . ? O1 C14 1.486(11) . ? O2 C18 1.450(12) . ? O2 C15 1.468(12) . ? O3 C22 1.433(12) . ? O3 C19 1.453(11) . ? O4 C23 1.457(12) . ? O4 C26 1.463(12) . ? C1 C2 1.37(3) . ? C1 C5 1.40(2) . ? C1 C6 1.513(14) . ? C2 C3 1.42(3) . ? C2 C7 1.521(15) . ? C3 C4 1.40(2) . ? C3 C8 1.511(15) . ? C4 C5 1.43(2) . ? C4 C9 1.516(14) . ? C5 C10 1.525(14) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C1A C5A 1.38(3) . ? C1A C2A 1.40(3) . ? C1A C6A 1.514(14) . ? C2A C3A 1.39(2) . ? C2A C7A 1.519(14) . ? C3A C4A 1.40(2) . ? C3A C8A 1.519(15) . ? C4A C5A 1.44(2) . ? C4A C9A 1.524(14) . ? C5A C10A 1.519(14) . ? C6A H6AA 0.9800 . ? C6A H6AB 0.9800 . ? C6A H6AC 0.9800 . ? C7A H7AA 0.9800 . ? C7A H7AB 0.9800 . ? C7A H7AC 0.9800 . ? C8A H8AA 0.9800 . ? C8A H8AB 0.9800 . ? C8A H8AC 0.9800 . ? C9A H9AA 0.9800 . ? C9A H9AB 0.9800 . ? C9A H9AC 0.9800 . ? C10A H10D 0.9800 . ? C10A H10E 0.9800 . ? C10A H10F 0.9800 . ? C11 C12 1.469(15) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13A 1.410(14) . ? C12 C13 1.551(16) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.543(15) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13A C14 1.5425 . ? C13A H13C 0.9900 . ? C13A H13D 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.530(15) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.49(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.536(16) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.511(13) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.502(19) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.516(13) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.478(18) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.51(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.528(16) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? 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 O4 Yb1 O2 115.5(2) . . ? O4 Yb1 O1 81.4(2) . . ? O2 Yb1 O1 78.3(2) . . ? O4 Yb1 O3 79.5(2) . . ? O2 Yb1 O3 77.1(2) . . ? O1 Yb1 O3 138.3(2) . . ? O4 Yb1 C3 143.0(4) . . ? O2 Yb1 C3 99.8(4) . . ? O1 Yb1 C3 95.9(5) . . ? O3 Yb1 C3 121.1(5) . . ? O4 Yb1 C2 111.3(6) . . ? O2 Yb1 C2 126.7(6) . . ? O1 Yb1 C2 84.9(4) . . ? O3 Yb1 C2 136.7(4) . . ? C3 Yb1 C2 32.2(7) . . ? O4 Yb1 C4 136.9(5) . . ? O2 Yb1 C4 102.6(4) . . ? O1 Yb1 C4 127.4(4) . . ? O3 Yb1 C4 90.8(4) . . ? C3 Yb1 C4 31.5(6) . . ? C2 Yb1 C4 51.9(5) . . ? O4 Yb1 C1 92.6(4) . . ? O2 Yb1 C1 151.8(4) . . ? O1 Yb1 C1 106.2(5) . . ? O3 Yb1 C1 111.5(5) . . ? C3 Yb1 C1 52.4(5) . . ? C2 Yb1 C1 30.6(6) . . ? C4 Yb1 C1 52.1(5) . . ? O4 Yb1 C5 105.3(5) . . ? O2 Yb1 C5 131.3(5) . . ? O1 Yb1 C5 135.2(4) . . ? O3 Yb1 C5 85.8(4) . . ? C3 Yb1 C5 52.2(5) . . ? C2 Yb1 C5 51.1(5) . . ? C4 Yb1 C5 31.7(5) . . ? C1 Yb1 C5 31.0(6) . . ? O4 Yb1 C3A 146.6(4) . . ? O2 Yb1 C3A 97.7(4) . . ? O1 Yb1 C3A 109.7(4) . . ? O3 Yb1 C3A 106.6(4) . . ? C3 Yb1 C3A 14.6(5) . . ? C2 Yb1 C3A 42.4(6) . . ? C4 Yb1 C3A 17.9(5) . . ? C1 Yb1 C3A 54.3(5) . . ? C5 Yb1 C3A 44.5(5) . . ? O4 Yb1 C4A 122.7(5) . . ? O2 Yb1 C4A 114.8(4) . . ? O1 Yb1 C4A 134.6(4) . . ? O3 Yb1 C4A 86.6(3) . . ? C3 Yb1 C4A 40.7(5) . . ? C2 Yb1 C4A 51.6(5) . . ? C4 Yb1 C4A 14.3(5) . . ? C1 Yb1 C4A 42.7(5) . . ? C5 Yb1 C4A 17.7(5) . . ? C3A Yb1 C4A 29.6(5) . . ? O4 Yb1 C5A 97.9(4) . . ? O2 Yb1 C5A 144.6(4) . . ? O1 Yb1 C5A 120.2(5) . . ? O3 Yb1 C5A 99.0(4) . . ? C3 Yb1 C5A 51.6(5) . . ? C2 Yb1 C5A 39.4(5) . . ? C4 Yb1 C5A 42.0(5) . . ? C1 Yb1 C5A 14.5(4) . . ? C5 Yb1 C5A 16.6(5) . . ? C3A Yb1 C5A 49.0(5) . . ? C4A Yb1 C5A 30.3(5) . . ? C27 Al1 C30 107.9(6) . . ? C27 Al1 C28 107.8(6) . . ? C30 Al1 C28 109.1(5) . . ? C27 Al1 C29 110.2(5) . . ? C30 Al1 C29 111.0(5) . . ? C28 Al1 C29 110.7(5) . . ? C11 O1 C14 110.3(7) . . ? C11 O1 Yb1 124.8(5) . . ? C14 O1 Yb1 122.3(6) . . ? C18 O2 C15 109.2(8) . . ? C18 O2 Yb1 134.8(6) . . ? C15 O2 Yb1 115.8(6) . . ? C22 O3 C19 108.2(7) . . ? C22 O3 Yb1 123.2(5) . . ? C19 O3 Yb1 125.7(6) . . ? C23 O4 C26 107.9(8) . . ? C23 O4 Yb1 133.1(6) . . ? C26 O4 Yb1 118.7(6) . . ? C2 C1 C5 108.0(15) . . ? C2 C1 C6 126(2) . . ? C5 C1 C6 125.5(19) . . ? C2 C1 Yb1 73.1(10) . . ? C5 C1 Yb1 75.0(9) . . ? C6 C1 Yb1 122.4(11) . . ? C1 C2 C3 109.8(14) . . ? C1 C2 C7 126(2) . . ? C3 C2 C7 124(2) . . ? C1 C2 Yb1 76.3(10) . . ? C3 C2 Yb1 73.2(10) . . ? C7 C2 Yb1 125.0(12) . . ? C4 C3 C2 106.5(14) . . ? C4 C3 C8 124.5(19) . . ? C2 C3 C8 128.6(19) . . ? C4 C3 Yb1 75.2(9) . . ? C2 C3 Yb1 74.6(10) . . ? C8 C3 Yb1 121.7(13) . . ? C3 C4 C5 108.1(14) . . ? C3 C4 C9 126.7(18) . . ? C5 C4 C9 124.6(18) . . ? C3 C4 Yb1 73.2(9) . . ? C5 C4 Yb1 75.9(9) . . ? C9 C4 Yb1 123.7(11) . . ? C1 C5 C4 107.7(13) . . ? C1 C5 C10 127.5(19) . . ? C4 C5 C10 124.4(18) . . ? C1 C5 Yb1 74.0(9) . . ? C4 C5 Yb1 72.4(9) . . ? C10 C5 Yb1 124.9(12) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5A C1A C2A 108.5(13) . . ? C5A C1A C6A 124.9(19) . . ? C2A C1A C6A 126.1(19) . . ? C5A C1A Yb1 75.0(9) . . ? C2A C1A Yb1 75.5(9) . . ? C6A C1A Yb1 122.2(11) . . ? C3A C2A C1A 108.6(13) . . ? C3A C2A C7A 126.1(19) . . ? C1A C2A C7A 125.1(19) . . ? C3A C2A Yb1 73.5(9) . . ? C1A C2A Yb1 75.4(9) . . ? C7A C2A Yb1 121.6(11) . . ? C2A C3A C4A 108.1(14) . . ? C2A C3A C8A 126.8(18) . . ? C4A C3A C8A 124.6(17) . . ? C2A C3A Yb1 77.3(10) . . ? C4A C3A Yb1 75.4(9) . . ? C8A C3A Yb1 120.0(12) . . ? C3A C4A C5A 107.1(13) . . ? C3A C4A C9A 126.6(18) . . ? C5A C4A C9A 125.8(18) . . ? C3A C4A Yb1 75.0(9) . . ? C5A C4A Yb1 75.9(9) . . ? C9A C4A Yb1 121.6(10) . . ? C1A C5A C4A 107.7(13) . . ? C1A C5A C10A 127.3(19) . . ? C4A C5A C10A 124.4(19) . . ? C1A C5A Yb1 76.2(9) . . ? C4A C5A Yb1 73.8(9) . . ? C10A C5A Yb1 122.9(12) . . ? C1A C6A H6AA 109.5 . . ? C1A C6A H6AB 109.5 . . ? H6AA C6A H6AB 109.5 . . ? C1A C6A H6AC 109.5 . . ? H6AA C6A H6AC 109.5 . . ? H6AB C6A H6AC 109.5 . . ? C2A C7A H7AA 109.5 . . ? C2A C7A H7AB 109.5 . . ? H7AA C7A H7AB 109.5 . . ? C2A C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? C3A C8A H8AA 109.5 . . ? C3A C8A H8AB 109.5 . . ? H8AA C8A H8AB 109.5 . . ? C3A C8A H8AC 109.5 . . ? H8AA C8A H8AC 109.5 . . ? H8AB C8A H8AC 109.5 . . ? C4A C9A H9AA 109.5 . . ? C4A C9A H9AB 109.5 . . ? H9AA C9A H9AB 109.5 . . ? C4A C9A H9AC 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? C5A C10A H10D 109.5 . . ? C5A C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? C5A C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? O1 C11 C12 107.9(8) . . ? O1 C11 H11A 110.1 . . ? C12 C11 H11A 110.1 . . ? O1 C11 H11B 110.1 . . ? C12 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? C13A C12 C11 103.8(10) . . ? C11 C12 C13 105.8(9) . . ? C13A C12 H12A 130.8 . . ? C11 C12 H12A 110.6 . . ? C13 C12 H12A 110.6 . . ? C13A C12 H12B 90.1 . . ? C11 C12 H12B 110.6 . . ? C13 C12 H12B 110.6 . . ? H12A C12 H12B 108.7 . . ? C14 C13 C12 105.3(11) . . ? C14 C13 H13A 110.7 . . ? C12 C13 H13A 110.7 . . ? C14 C13 H13B 110.7 . . ? C12 C13 H13B 110.7 . . ? H13A C13 H13B 108.8 . . ? C12 C13A C14 112.7(6) . . ? C12 C13A H13C 109.1 . . ? C14 C13A H13C 109.1 . . ? C12 C13A H13D 109.1 . . ? C14 C13A H13D 109.1 . . ? H13C C13A H13D 107.8 . . ? O1 C14 C13 101.1(9) . . ? O1 C14 C13A 99.9(4) . . ? O1 C14 H14A 111.6 . . ? C13 C14 H14A 111.6 . . ? C13A C14 H14A 91.0 . . ? O1 C14 H14B 111.6 . . ? C13 C14 H14B 111.6 . . ? C13A C14 H14B 131.5 . . ? H14A C14 H14B 109.4 . . ? O2 C15 C16 106.0(9) . . ? O2 C15 H15A 110.5 . . ? C16 C15 H15A 110.5 . . ? O2 C15 H15B 110.5 . . ? C16 C15 H15B 110.5 . . ? H15A C15 H15B 108.7 . . ? C17 C16 C15 102.7(9) . . ? C17 C16 H16A 111.2 . . ? C15 C16 H16A 111.2 . . ? C17 C16 H16B 111.2 . . ? C15 C16 H16B 111.2 . . ? H16A C16 H16B 109.1 . . ? C16 C17 C18 103.3(10) . . ? C16 C17 H17A 111.1 . . ? C18 C17 H17A 111.1 . . ? C16 C17 H17B 111.1 . . ? C18 C17 H17B 111.1 . . ? H17A C17 H17B 109.1 . . ? O2 C18 C17 104.1(9) . . ? O2 C18 H18A 110.9 . . ? C17 C18 H18A 110.9 . . ? O2 C18 H18B 110.9 . . ? C17 C18 H18B 110.9 . . ? H18A C18 H18B 109.0 . . ? O3 C19 C20 105.4(8) . . ? O3 C19 H19A 110.7 . . ? C20 C19 H19A 110.7 . . ? O3 C19 H19B 110.7 . . ? C20 C19 H19B 110.7 . . ? H19A C19 H19B 108.8 . . ? C21 C20 C19 102.8(9) . . ? C21 C20 H20A 111.2 . . ? C19 C20 H20A 111.2 . . ? C21 C20 H20B 111.2 . . ? C19 C20 H20B 111.2 . . ? H20A C20 H20B 109.1 . . ? C20 C21 C22 103.2(10) . . ? C20 C21 H21A 111.1 . . ? C22 C21 H21A 111.1 . . ? C20 C21 H21B 111.1 . . ? C22 C21 H21B 111.1 . . ? H21A C21 H21B 109.1 . . ? O3 C22 C21 107.9(9) . . ? O3 C22 H22A 110.1 . . ? C21 C22 H22A 110.1 . . ? O3 C22 H22B 110.1 . . ? C21 C22 H22B 110.1 . . ? H22A C22 H22B 108.4 . . ? O4 C23 C24 106.3(10) . . ? O4 C23 H23A 110.5 . . ? C24 C23 H23A 110.5 . . ? O4 C23 H23B 110.5 . . ? C24 C23 H23B 110.5 . . ? H23A C23 H23B 108.7 . . ? C23 C24 C25 102.4(10) . . ? C23 C24 H24A 111.3 . . ? C25 C24 H24A 111.3 . . ? C23 C24 H24B 111.3 . . ? C25 C24 H24B 111.3 . . ? H24A C24 H24B 109.2 . . ? C24 C25 C26 101.8(11) . . ? C24 C25 H25A 111.4 . . ? C26 C25 H25A 111.4 . . ? C24 C25 H25B 111.4 . . ? C26 C25 H25B 111.4 . . ? H25A C25 H25B 109.3 . . ? O4 C26 C25 105.3(10) . . ? O4 C26 H26A 110.7 . . ? C25 C26 H26A 110.7 . . ? O4 C26 H26B 110.7 . . ? C25 C26 H26B 110.7 . . ? H26A C26 H26B 108.8 . . ? Al1 C27 H27A 109.5 . . ? Al1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Al1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Al1 C28 H28A 109.5 . . ? Al1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Al1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Al1 C29 H29A 109.5 . . ? Al1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Al1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Al1 C30 H30A 109.5 . . ? Al1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Al1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? # # END of CIF for compound 4b # # END OF FILE