Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Arndt, Stefan' ; Institut fur Anorganische Chemie und Analytische Chemie Johannes Gutenberg Universitat Mainz Duesbergweg 10-14 D-55099 Mainz Germany ; 'Spaniol, Thomas P.' ; Institut fur Anorganische Chemie und Analytische Chemie Johannes Gutenberg Universitat Mainz Duesbergweg 10-14 D-55099 Mainz Germany ; 'Okuda, Jun' ; Institut fur Anorganische Chemie und Analytische Chemie Johannes Gutenberg Universitat Mainz Duesbergweg 10-14 D-55099 Mainz Germany ; _publ_contact_author_name 'Jun Okuda' _publ_contact_author_address ; Institut fur Anorganische Chemie und Analytische Chmie Universitat Mainz Duesbergweg 10-14 Mainz D-550099 GERMANY ; _publ_contact_author_phone '049 6131 39 23737' _publ_contact_author_fax '049 6131 39 25605' _publ_contact_author_email okuda@mail.uni-mainz.de _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name ? _publ_contact_letter ; These three crystal structures are part of a manuscript that is sent for publication in the Journal 'Chemical Communications'. The individual structures sa21, sa22 and sa23 are separated from each other by the sequence #===END at the beginning of a line. ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; The First Structurally Characterized Cationic Lanthanide-Alkyl Complexes ; #============================================================================== data_sa21 _database_code_CSD 179961 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrahydrofurane-1,4,7,10-tetraoxacyclododecane- bis(trimethylsilylmethyl)lutetium(III)- trimethylsilylmethyltriphenylborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H72 B Lu O5 Si3' _chemical_formula_weight 927.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Lu' 'Lu' -0.4720 5.8580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0820 0.0700 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0140(10) _cell_length_b 12.6330(10) _cell_length_c 17.4330(10) _cell_angle_alpha 93.706(2) _cell_angle_beta 94.301(2) _cell_angle_gamma 104.342(2) _cell_volume 2334.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prism' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.69 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.46 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 2.230 _exptl_absorpt_correction_type 'Saint' _exptl_absorpt_correction_T_min 0.3092 _exptl_absorpt_correction_T_max 0.4244 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS diffactometer with CCD detector' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20914 _diffrn_reflns_av_R_equivalents 0.0161 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 28.30 _reflns_number_total 11121 _reflns_number_gt 10486 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART' _computing_cell_refinement 'SAINT' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-III for Windows (Farraguia, 1997)' _computing_publication_material 'WinGX Publication Routines, Farraguia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+0.4007P] 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 SHELXL _refine_ls_extinction_coef 0.0038(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11121 _refine_ls_number_parameters 751 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0216 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0511 _refine_ls_wR_factor_gt 0.0505 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu Lu 0.015721(6) 0.254804(5) 0.192550(4) 0.02421(3) Uani 1 1 d . . . Si1 Si 0.21287(5) 0.44248(5) 0.05588(4) 0.03627(12) Uani 1 1 d . . . Si2 Si 0.16747(7) 0.03338(5) 0.12508(4) 0.04584(15) Uani 1 1 d . . . Si3 Si -0.40320(5) -0.19663(5) 0.25303(3) 0.03481(12) Uani 1 1 d . . . O1 O 0.17596(13) 0.40550(13) 0.26264(9) 0.0415(3) Uani 1 1 d . . . O2 O -0.06973(12) 0.39276(10) 0.25965(8) 0.0286(3) Uani 1 1 d . . . O3 O -0.11663(14) 0.18393(11) 0.29785(8) 0.0350(3) Uani 1 1 d . . . O4 O 0.13095(16) 0.20434(15) 0.30103(9) 0.0456(4) Uani 1 1 d . . . O5 O -0.19079(12) 0.21346(11) 0.13997(8) 0.0315(3) Uani 1 1 d . A . B B -0.2230(2) -0.27847(17) 0.36498(12) 0.0290(4) Uani 1 1 d . . . C1 C 0.1422(2) 0.49813(19) 0.29878(15) 0.0439(5) Uani 1 1 d . . . H1A H 0.205(3) 0.562(2) 0.2918(16) 0.052(7) Uiso 1 1 d . . . H1B H 0.139(2) 0.491(2) 0.3560(16) 0.048(7) Uiso 1 1 d . . . C2 C 0.0157(2) 0.50013(15) 0.26099(14) 0.0365(4) Uani 1 1 d . . . H2A H -0.018(2) 0.550(2) 0.2889(15) 0.043(6) Uiso 1 1 d . . . H2B H 0.021(2) 0.5141(19) 0.2080(15) 0.036(6) Uiso 1 1 d . . . C3 C -0.11942(19) 0.36923(16) 0.33232(11) 0.0317(4) Uani 1 1 d . . . H3A H -0.172(2) 0.414(2) 0.3471(15) 0.041(6) Uiso 1 1 d . . . H3B H -0.046(2) 0.3808(18) 0.3717(13) 0.030(5) Uiso 1 1 d . . . C4 C -0.1959(2) 0.25204(17) 0.32171(13) 0.0367(4) Uani 1 1 d . . . H4A H -0.233(2) 0.2295(18) 0.3703(13) 0.033(6) Uiso 1 1 d . . . H4B H -0.267(2) 0.245(2) 0.2766(15) 0.041(6) Uiso 1 1 d . . . C5 C -0.0585(3) 0.1420(2) 0.36239(14) 0.0502(6) Uani 1 1 d . . . H5A H -0.112(2) 0.075(2) 0.3786(15) 0.048(7) Uiso 1 1 d . . . H5B H -0.035(2) 0.195(2) 0.4049(16) 0.045(7) Uiso 1 1 d . . . C6 C 0.0553(3) 0.1126(2) 0.33543(15) 0.0568(7) Uani 1 1 d . . . H6A H 0.109(3) 0.093(3) 0.3816(19) 0.073(9) Uiso 1 1 d . . . H6B H 0.033(2) 0.052(2) 0.2944(16) 0.048(7) Uiso 1 1 d . . . C7 C 0.2170(3) 0.2841(3) 0.35423(15) 0.0586(7) Uani 1 1 d . . . H7A H 0.279(3) 0.248(2) 0.3791(17) 0.062(8) Uiso 1 1 d . . . H7B H 0.170(3) 0.311(2) 0.3959(17) 0.055(8) Uiso 1 1 d . . . C8 C 0.2747(2) 0.3726(3) 0.30646(16) 0.0569(7) Uani 1 1 d . . . H8A H 0.324(3) 0.439(3) 0.335(2) 0.073(10) Uiso 1 1 d . . . H8B H 0.326(3) 0.345(2) 0.2695(18) 0.062(8) Uiso 1 1 d . . . C9 C 0.0701(2) 0.3493(2) 0.08395(13) 0.0394(5) Uani 1 1 d . . . H9A H 0.044(3) 0.293(3) 0.0482(18) 0.059(8) Uiso 1 1 d . . . H9B H 0.006(3) 0.386(3) 0.0756(19) 0.076(10) Uiso 1 1 d . . . C10 C 0.2147(3) 0.58807(19) 0.08698(15) 0.0454(5) Uani 1 1 d . . . H10A H 0.282(3) 0.638(3) 0.0702(18) 0.063(9) Uiso 1 1 d . . . H10B H 0.223(3) 0.597(2) 0.1440(18) 0.059(8) Uiso 1 1 d . . . H10C H 0.139(3) 0.601(3) 0.0656(19) 0.070(9) Uiso 1 1 d . . . C11 C 0.2211(3) 0.4311(2) -0.05166(17) 0.0554(6) Uani 1 1 d . . . H11A H 0.295(3) 0.484(3) -0.0684(17) 0.062(8) Uiso 1 1 d . . . H11B H 0.142(3) 0.443(3) -0.081(2) 0.075(10) Uiso 1 1 d . . . H11C H 0.222(3) 0.366(3) -0.068(2) 0.085(12) Uiso 1 1 d . . . C12 C 0.3643(3) 0.4208(3) 0.1009(3) 0.0636(8) Uani 1 1 d . . . H12A H 0.432(4) 0.460(3) 0.079(2) 0.094(12) Uiso 1 1 d . . . H12B H 0.367(4) 0.356(3) 0.087(2) 0.090(13) Uiso 1 1 d . . . H12C H 0.376(4) 0.440(3) 0.154(3) 0.097(14) Uiso 1 1 d . . . C13 C 0.0253(2) 0.07988(17) 0.14221(13) 0.0362(4) Uani 1 1 d . . . H13A H -0.028(3) 0.025(2) 0.1681(16) 0.048(7) Uiso 1 1 d . . . H13B H -0.026(3) 0.072(2) 0.0879(18) 0.060(8) Uiso 1 1 d . . . C14 C 0.2380(3) 0.0998(3) 0.04029(19) 0.0599(7) Uani 1 1 d . . . H14A H 0.311(4) 0.080(3) 0.030(2) 0.089(12) Uiso 1 1 d . . . H14B H 0.256(4) 0.180(4) 0.049(3) 0.113(14) Uiso 1 1 d . . . H14C H 0.181(4) 0.084(3) -0.010(2) 0.093(12) Uiso 1 1 d . . . C15 C 0.2940(4) 0.0716(5) 0.2076(2) 0.0901(15) Uani 1 1 d . . . H15A H 0.362(5) 0.047(4) 0.197(3) 0.137(18) Uiso 1 1 d . . . H15B H 0.265(3) 0.047(3) 0.249(2) 0.074(12) Uiso 1 1 d . . . H15C H 0.329(4) 0.157(4) 0.216(2) 0.095(13) Uiso 1 1 d . . . C16 C 0.1335(5) -0.1193(3) 0.1028(3) 0.0840(12) Uani 1 1 d . . . H16A H 0.216(4) -0.143(3) 0.096(2) 0.090(11) Uiso 1 1 d . . . H16B H 0.079(5) -0.154(5) 0.054(3) 0.15(2) Uiso 1 1 d . . . H16C H 0.102(3) -0.154(3) 0.143(2) 0.074(11) Uiso 1 1 d . . . C17 C -0.2753(2) 0.1035(2) 0.12852(18) 0.0468(5) Uani 1 1 d . . . H17A H -0.283(4) 0.078(3) 0.176(2) 0.094(13) Uiso 1 1 d . . . H17B H -0.242(3) 0.061(3) 0.105(2) 0.068(10) Uiso 1 1 d . . . C18A C -0.3977(5) 0.1174(6) 0.1124(5) 0.0689(19) Uani 0.50 1 d P A 1 H18A H -0.4404 0.1145 0.1592 0.083 Uiso 0.50 1 calc PR A 1 H18B H -0.4462 0.0592 0.0750 0.083 Uiso 0.50 1 calc PR A 1 C18B C -0.3827(5) 0.1150(5) 0.0663(3) 0.0460(12) Uani 0.50 1 d P A 2 H18C H -0.3615 0.1009 0.0143 0.055 Uiso 0.50 1 calc PR A 2 H18D H -0.4627 0.0652 0.0736 0.055 Uiso 0.50 1 calc PR A 2 C19 C -0.3866(3) 0.2258(3) 0.0809(2) 0.0655(8) Uani 1 1 d . . . H19A H -0.4458 0.2624 0.1023 0.079 Uiso 0.50 1 calc PR A 1 H19B H -0.4029 0.2171 0.0251 0.079 Uiso 0.50 1 calc PR A 1 H19C H -0.4401 0.2326 0.1217 0.079 Uiso 0.50 1 calc PR A 2 H19D H -0.4194 0.2523 0.0348 0.079 Uiso 0.50 1 calc PR A 2 C20 C -0.2535(2) 0.2900(2) 0.10489(15) 0.0438(5) Uani 1 1 d . A . H20A H -0.201(3) 0.319(3) 0.0604(18) 0.065(9) Uiso 1 1 d . . . H20B H -0.240(3) 0.352(3) 0.1435(19) 0.069(9) Uiso 1 1 d . . . C21 C -0.24851(19) -0.22256(16) 0.28381(12) 0.0321(4) Uani 1 1 d . . . H21A H -0.228(2) -0.256(2) 0.2452(16) 0.044(7) Uiso 1 1 d . . . H21B H -0.193(2) -0.1503(19) 0.2863(13) 0.031(5) Uiso 1 1 d . . . C22 C -0.4156(3) -0.0631(2) 0.30078(16) 0.0474(5) Uani 1 1 d . . . H22A H -0.488(3) -0.040(3) 0.287(2) 0.077(10) Uiso 1 1 d . . . H22B H -0.348(3) -0.013(3) 0.290(2) 0.073(10) Uiso 1 1 d . . . H22C H -0.411(3) -0.061(3) 0.351(2) 0.069(9) Uiso 1 1 d . . . C23 C -0.5463(2) -0.3043(2) 0.27229(17) 0.0459(5) Uani 1 1 d . . . H23A H -0.622(3) -0.286(3) 0.2582(19) 0.071(9) Uiso 1 1 d . . . H23B H -0.542(3) -0.316(3) 0.317(2) 0.074(11) Uiso 1 1 d . . . H23C H -0.547(3) -0.371(3) 0.2412(18) 0.059(8) Uiso 1 1 d . . . C24 C -0.4181(3) -0.1888(3) 0.14573(15) 0.0546(6) Uani 1 1 d . . . H24A H -0.491(4) -0.163(3) 0.134(2) 0.098(13) Uiso 1 1 d . . . H24B H -0.425(3) -0.258(3) 0.1205(17) 0.060(8) Uiso 1 1 d . . . H24C H -0.346(3) -0.146(3) 0.1278(19) 0.070(10) Uiso 1 1 d . . . C25 C -0.30363(17) -0.40784(15) 0.36032(11) 0.0308(4) Uani 1 1 d . . . C26 C -0.34120(19) -0.47250(16) 0.29014(13) 0.0343(4) Uani 1 1 d . . . H26 H -0.325(2) -0.4384(19) 0.2441(14) 0.034(6) Uiso 1 1 d . . . C27 C -0.4049(2) -0.58332(18) 0.28579(15) 0.0414(5) Uani 1 1 d . . . H27 H -0.430(3) -0.621(2) 0.2383(16) 0.051(7) Uiso 1 1 d . . . C28 C -0.4323(2) -0.63464(18) 0.35192(17) 0.0458(6) Uani 1 1 d . . . H28 H -0.473(3) -0.704(2) 0.3506(16) 0.050(7) Uiso 1 1 d . . . C29 C -0.3969(2) -0.57431(19) 0.42232(16) 0.0443(5) Uani 1 1 d . . . H29 H -0.421(2) -0.609(2) 0.4670(15) 0.045(7) Uiso 1 1 d . . . C30 C -0.3345(2) -0.46364(18) 0.42612(13) 0.0376(4) Uani 1 1 d . . . H30 H -0.313(2) -0.4276(18) 0.4723(14) 0.029(5) Uiso 1 1 d . . . C31 C -0.07224(18) -0.27548(15) 0.38091(12) 0.0329(4) Uani 1 1 d . . . C32 C -0.0274(2) -0.3304(2) 0.44017(12) 0.0418(5) Uani 1 1 d . . . H32 H -0.086(2) -0.378(2) 0.4709(15) 0.040(6) Uiso 1 1 d . . . C33 C 0.0993(2) -0.3279(2) 0.45504(14) 0.0504(6) Uani 1 1 d . . . H33 H 0.121(3) -0.365(2) 0.4901(16) 0.048(7) Uiso 1 1 d . . . C34 C 0.1880(2) -0.2690(2) 0.41140(17) 0.0524(6) Uani 1 1 d . . . H34 H 0.271(3) -0.265(2) 0.4234(18) 0.061(8) Uiso 1 1 d . . . C35 C 0.1481(2) -0.21535(19) 0.35218(18) 0.0505(6) Uani 1 1 d . . . H35 H 0.201(3) -0.173(2) 0.3223(17) 0.053(8) Uiso 1 1 d . . . C36 C 0.0212(2) -0.21860(17) 0.33746(15) 0.0408(5) Uani 1 1 d . . . H36 H -0.006(2) -0.180(2) 0.2973(15) 0.046(7) Uiso 1 1 d . . . C37 C -0.26147(17) -0.20210(15) 0.43414(10) 0.0278(3) Uani 1 1 d . . . C38 C -0.38041(19) -0.22372(17) 0.46250(12) 0.0331(4) Uani 1 1 d . . . H38 H -0.435(2) -0.289(2) 0.4472(14) 0.042(7) Uiso 1 1 d . . . C39 C -0.4180(2) -0.14835(18) 0.51096(12) 0.0387(4) Uani 1 1 d . . . H39 H -0.505(2) -0.1662(19) 0.5270(14) 0.040(6) Uiso 1 1 d . . . C40 C -0.3361(2) -0.04707(18) 0.53396(12) 0.0390(4) Uani 1 1 d . . . H40 H -0.359(2) 0.000(2) 0.5660(16) 0.048(7) Uiso 1 1 d . . . C41 C -0.2164(2) -0.02332(17) 0.50933(12) 0.0343(4) Uani 1 1 d . . . H41 H -0.161(2) 0.038(2) 0.5237(14) 0.036(6) Uiso 1 1 d . . . C42 C -0.18019(19) -0.10018(15) 0.46126(11) 0.0300(4) Uani 1 1 d . . . H42 H -0.093(2) -0.0789(17) 0.4429(12) 0.028(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu 0.02666(5) 0.02406(5) 0.02230(5) 0.00145(3) 0.00041(3) 0.00785(3) Si1 0.0343(3) 0.0345(3) 0.0401(3) 0.0115(2) 0.0054(2) 0.0062(2) Si2 0.0531(4) 0.0454(3) 0.0446(3) -0.0086(3) 0.0003(3) 0.0273(3) Si3 0.0371(3) 0.0334(3) 0.0315(3) 0.0070(2) 0.0000(2) 0.0043(2) O1 0.0292(7) 0.0499(9) 0.0421(8) -0.0165(7) -0.0046(6) 0.0111(6) O2 0.0296(6) 0.0256(6) 0.0305(7) 0.0011(5) 0.0052(5) 0.0065(5) O3 0.0485(8) 0.0317(7) 0.0284(7) 0.0084(5) 0.0103(6) 0.0135(6) O4 0.0523(9) 0.0632(10) 0.0286(7) 0.0019(7) -0.0045(6) 0.0314(8) O5 0.0291(6) 0.0289(6) 0.0338(7) 0.0059(5) -0.0022(5) 0.0030(5) B 0.0295(10) 0.0291(10) 0.0282(10) 0.0017(8) 0.0060(8) 0.0064(8) C1 0.0374(11) 0.0378(11) 0.0479(13) -0.0157(9) 0.0086(9) -0.0027(9) C2 0.0431(11) 0.0219(8) 0.0437(12) 0.0000(8) 0.0103(9) 0.0054(8) C3 0.0300(9) 0.0349(10) 0.0307(9) -0.0011(7) 0.0070(7) 0.0088(8) C4 0.0363(10) 0.0375(10) 0.0360(11) 0.0028(8) 0.0131(8) 0.0063(8) C5 0.0763(17) 0.0483(13) 0.0344(12) 0.0192(10) 0.0121(11) 0.0258(12) C6 0.092(2) 0.0580(15) 0.0363(12) 0.0172(11) 0.0052(13) 0.0457(15) C7 0.0491(14) 0.098(2) 0.0335(12) -0.0108(13) -0.0133(10) 0.0376(15) C8 0.0320(11) 0.084(2) 0.0514(15) -0.0201(14) -0.0122(10) 0.0195(12) C9 0.0381(11) 0.0410(11) 0.0330(11) 0.0091(9) -0.0016(8) -0.0012(9) C10 0.0535(14) 0.0366(11) 0.0443(13) 0.0086(9) 0.0054(11) 0.0064(10) C11 0.0699(19) 0.0497(15) 0.0490(15) 0.0073(11) 0.0229(13) 0.0135(13) C12 0.0403(14) 0.0618(18) 0.089(3) 0.0141(17) -0.0013(15) 0.0142(13) C13 0.0413(11) 0.0316(10) 0.0375(11) -0.0008(8) 0.0027(9) 0.0140(8) C14 0.0565(17) 0.0599(17) 0.0629(18) -0.0087(13) 0.0170(14) 0.0145(13) C15 0.077(2) 0.148(4) 0.064(2) -0.026(2) -0.0144(19) 0.080(3) C16 0.120(3) 0.0492(17) 0.099(3) 0.0014(19) 0.027(3) 0.047(2) C17 0.0398(12) 0.0344(11) 0.0583(16) -0.0006(10) -0.0020(11) -0.0019(9) C18A 0.030(3) 0.057(3) 0.110(6) 0.018(4) -0.007(3) -0.005(2) C18B 0.032(2) 0.056(3) 0.043(3) -0.016(2) -0.007(2) 0.008(2) C19 0.0388(13) 0.0670(18) 0.082(2) 0.0162(15) -0.0204(13) 0.0025(12) C20 0.0324(10) 0.0494(13) 0.0495(13) 0.0189(11) -0.0060(9) 0.0092(9) C21 0.0340(10) 0.0318(9) 0.0285(9) 0.0038(7) 0.0076(7) 0.0031(8) C22 0.0602(16) 0.0426(12) 0.0421(13) 0.0070(10) -0.0022(11) 0.0191(12) C23 0.0348(12) 0.0487(13) 0.0503(15) 0.0074(11) -0.0001(10) 0.0039(10) C24 0.0682(18) 0.0526(15) 0.0374(13) 0.0083(11) -0.0046(12) 0.0064(13) C25 0.0276(9) 0.0307(9) 0.0357(10) 0.0034(7) 0.0047(7) 0.0098(7) C26 0.0314(9) 0.0329(9) 0.0386(11) 0.0003(8) 0.0000(8) 0.0099(8) C27 0.0295(10) 0.0350(10) 0.0571(14) -0.0065(9) -0.0049(9) 0.0082(8) C28 0.0268(10) 0.0293(10) 0.0811(18) 0.0077(10) 0.0067(10) 0.0052(8) C29 0.0374(11) 0.0373(11) 0.0629(15) 0.0182(10) 0.0172(10) 0.0110(9) C30 0.0395(11) 0.0363(10) 0.0390(11) 0.0070(9) 0.0099(9) 0.0104(8) C31 0.0323(9) 0.0294(9) 0.0355(10) -0.0072(7) 0.0050(8) 0.0071(7) C32 0.0395(11) 0.0579(13) 0.0300(10) -0.0056(9) 0.0031(8) 0.0186(10) C33 0.0493(14) 0.0701(16) 0.0358(12) -0.0150(11) -0.0053(10) 0.0304(12) C34 0.0317(11) 0.0561(14) 0.0661(17) -0.0260(12) -0.0027(11) 0.0149(10) C35 0.0334(11) 0.0363(11) 0.0783(18) -0.0092(11) 0.0137(11) 0.0036(9) C36 0.0350(11) 0.0293(10) 0.0575(14) -0.0015(9) 0.0108(10) 0.0064(8) C37 0.0322(9) 0.0282(8) 0.0251(8) 0.0070(7) 0.0036(7) 0.0101(7) C38 0.0336(10) 0.0335(10) 0.0330(10) 0.0060(8) 0.0060(8) 0.0085(8) C39 0.0392(11) 0.0476(12) 0.0354(11) 0.0095(9) 0.0121(8) 0.0187(9) C40 0.0516(13) 0.0402(11) 0.0318(10) 0.0027(8) 0.0075(9) 0.0233(10) C41 0.0424(11) 0.0285(9) 0.0326(10) 0.0024(7) -0.0008(8) 0.0117(8) C42 0.0341(10) 0.0301(9) 0.0277(9) 0.0059(7) 0.0029(7) 0.0108(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu O5 2.3072(13) . ? Lu C9 2.340(2) . ? Lu C13 2.354(2) . ? Lu O4 2.4063(14) . ? Lu O1 2.4379(14) . ? Lu O2 2.4507(12) . ? Lu O3 2.5028(13) . ? Si1 C9 1.836(2) . ? Si1 C10 1.878(3) . ? Si1 C12 1.879(3) . ? Si1 C11 1.882(3) . ? Si2 C13 1.841(2) . ? Si2 C14 1.872(3) . ? Si2 C15 1.876(4) . ? Si2 C16 1.880(3) . ? Si3 C21 1.860(2) . ? Si3 C22 1.873(3) . ? Si3 C24 1.877(3) . ? Si3 C23 1.877(2) . ? O1 C1 1.435(3) . ? O1 C8 1.442(3) . ? O2 C3 1.437(2) . ? O2 C2 1.444(2) . ? O3 C4 1.434(2) . ? O3 C5 1.446(3) . ? O4 C7 1.431(3) . ? O4 C6 1.443(4) . ? O5 C20 1.459(2) . ? O5 C17 1.459(3) . ? B C37 1.641(3) . ? B C25 1.649(3) . ? B C31 1.654(3) . ? B C21 1.658(3) . ? C1 C2 1.503(3) . ? C1 H1A 0.94(3) . ? C1 H1B 1.01(3) . ? C2 H2A 0.94(3) . ? C2 H2B 0.96(3) . ? C3 C4 1.503(3) . ? C3 H3A 0.94(3) . ? C3 H3B 0.99(2) . ? C4 H4A 1.00(2) . ? C4 H4B 1.05(3) . ? C5 C6 1.492(4) . ? C5 H5A 0.97(3) . ? C5 H5B 0.94(3) . ? C6 H6A 1.04(3) . ? C6 H6B 0.98(3) . ? C7 C8 1.481(5) . ? C7 H7A 1.00(3) . ? C7 H7B 1.01(3) . ? C8 H8A 0.97(4) . ? C8 H8B 0.99(3) . ? C9 H9A 0.89(3) . ? C9 H9B 0.94(4) . ? C10 H10A 0.93(3) . ? C10 H10B 0.99(3) . ? C10 H10C 0.94(3) . ? C11 H11A 1.00(3) . ? C11 H11B 1.02(4) . ? C11 H11C 0.86(4) . ? C12 H12A 0.92(4) . ? C12 H12B 0.85(4) . ? C12 H12C 0.94(4) . ? C13 H13A 0.95(3) . ? C13 H13B 1.05(3) . ? C14 H14A 0.92(4) . ? C14 H14B 0.98(5) . ? C14 H14C 1.03(4) . ? C15 H15A 0.90(5) . ? C15 H15B 0.86(4) . ? C15 H15C 1.05(4) . ? C16 H16A 1.04(4) . ? C16 H16B 1.02(6) . ? C16 H16C 0.89(4) . ? C17 C18A 1.412(7) . ? C17 C18B 1.584(6) . ? C17 H17A 0.90(4) . ? C17 H17B 0.83(3) . ? C18A C19 1.489(7) . ? C18A H18A 0.9700 . ? C18A H18B 0.9700 . ? C18B C19 1.417(6) . ? C18B H18C 0.9700 . ? C18B H18D 0.9700 . ? C19 C20 1.503(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C19 H19D 0.9700 . ? C20 H20A 1.03(3) . ? C20 H20B 0.97(3) . ? C21 H21A 0.85(3) . ? C21 H21B 0.96(2) . ? C22 H22A 0.93(4) . ? C22 H22B 0.89(4) . ? C22 H22C 0.88(4) . ? C23 H23A 0.94(3) . ? C23 H23B 0.80(4) . ? C23 H23C 0.97(3) . ? C24 H24A 0.95(4) . ? C24 H24B 0.93(3) . ? C24 H24C 0.94(3) . ? C25 C26 1.401(3) . ? C25 C30 1.405(3) . ? C26 C27 1.396(3) . ? C26 H26 0.94(2) . ? C27 C28 1.376(4) . ? C27 H27 0.92(3) . ? C28 C29 1.378(4) . ? C28 H28 0.88(3) . ? C29 C30 1.391(3) . ? C29 H29 0.94(3) . ? C30 H30 0.88(2) . ? C31 C36 1.404(3) . ? C31 C32 1.406(3) . ? C32 C33 1.393(3) . ? C32 H32 0.99(3) . ? C33 C34 1.383(4) . ? C33 H33 0.85(3) . ? C34 C35 1.374(4) . ? C34 H34 0.91(3) . ? C35 C36 1.392(3) . ? C35 H35 0.91(3) . ? C36 H36 0.95(3) . ? C37 C42 1.403(3) . ? C37 C38 1.404(3) . ? C38 C39 1.391(3) . ? C38 H38 0.90(3) . ? C39 C40 1.385(3) . ? C39 H39 0.99(2) . ? C40 C41 1.385(3) . ? C40 H40 0.89(3) . ? C41 C42 1.393(3) . ? C41 H41 0.87(2) . ? C42 H42 1.01(2) . ? 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 O5 Lu C9 87.62(6) . . ? O5 Lu C13 88.06(6) . . ? C9 Lu C13 97.97(9) . . ? O5 Lu O4 136.79(5) . . ? C9 Lu O4 135.13(7) . . ? C13 Lu O4 80.89(7) . . ? O5 Lu O1 140.56(5) . . ? C9 Lu O1 84.51(7) . . ? C13 Lu O1 131.29(6) . . ? O4 Lu O1 65.12(6) . . ? O5 Lu O2 76.75(5) . . ? C9 Lu O2 97.44(7) . . ? C13 Lu O2 157.83(7) . . ? O4 Lu O2 99.10(5) . . ? O1 Lu O2 66.13(5) . . ? O5 Lu O3 73.61(5) . . ? C9 Lu O3 157.09(7) . . ? C13 Lu O3 94.48(6) . . ? O4 Lu O3 65.88(5) . . ? O1 Lu O3 101.53(5) . . ? O2 Lu O3 65.97(4) . . ? C9 Si1 C10 109.72(12) . . ? C9 Si1 C12 114.61(14) . . ? C10 Si1 C12 105.70(15) . . ? C9 Si1 C11 111.79(12) . . ? C10 Si1 C11 108.01(12) . . ? C12 Si1 C11 106.64(17) . . ? C13 Si2 C14 108.69(13) . . ? C13 Si2 C15 114.12(13) . . ? C14 Si2 C15 106.2(2) . . ? C13 Si2 C16 112.82(17) . . ? C14 Si2 C16 107.68(18) . . ? C15 Si2 C16 106.9(2) . . ? C21 Si3 C22 110.20(11) . . ? C21 Si3 C24 109.56(13) . . ? C22 Si3 C24 108.33(13) . . ? C21 Si3 C23 116.16(11) . . ? C22 Si3 C23 107.36(13) . . ? C24 Si3 C23 104.87(14) . . ? C1 O1 C8 113.76(18) . . ? C1 O1 Lu 120.71(12) . . ? C8 O1 Lu 114.68(15) . . ? C3 O2 C2 113.70(15) . . ? C3 O2 Lu 118.18(11) . . ? C2 O2 Lu 110.34(11) . . ? C4 O3 C5 112.43(16) . . ? C4 O3 Lu 114.19(11) . . ? C5 O3 Lu 118.37(14) . . ? C7 O4 C6 115.1(2) . . ? C7 O4 Lu 122.28(16) . . ? C6 O4 Lu 111.54(15) . . ? C20 O5 C17 108.85(17) . . ? C20 O5 Lu 125.73(12) . . ? C17 O5 Lu 125.07(13) . . ? C37 B C25 112.77(15) . . ? C37 B C31 109.07(15) . . ? C25 B C31 107.51(15) . . ? C37 B C21 106.02(15) . . ? C25 B C21 111.23(16) . . ? C31 B C21 110.23(15) . . ? O1 C1 C2 107.12(17) . . ? O1 C1 H1A 108.0(17) . . ? C2 C1 H1A 112.3(17) . . ? O1 C1 H1B 110.3(15) . . ? C2 C1 H1B 110.7(15) . . ? H1A C1 H1B 108(2) . . ? O2 C2 C1 109.46(17) . . ? O2 C2 H2A 107.9(16) . . ? C1 C2 H2A 110.6(16) . . ? O2 C2 H2B 105.0(14) . . ? C1 C2 H2B 110.7(14) . . ? H2A C2 H2B 113(2) . . ? O2 C3 C4 105.97(15) . . ? O2 C3 H3A 113.0(16) . . ? C4 C3 H3A 109.0(15) . . ? O2 C3 H3B 106.9(13) . . ? C4 C3 H3B 112.6(13) . . ? H3A C3 H3B 109(2) . . ? O3 C4 C3 108.72(16) . . ? O3 C4 H4A 111.4(13) . . ? C3 C4 H4A 110.6(13) . . ? O3 C4 H4B 107.3(13) . . ? C3 C4 H4B 108.3(14) . . ? H4A C4 H4B 110.4(19) . . ? O3 C5 C6 106.71(18) . . ? O3 C5 H5A 113.1(16) . . ? C6 C5 H5A 106.6(16) . . ? O3 C5 H5B 111.5(16) . . ? C6 C5 H5B 109.8(16) . . ? H5A C5 H5B 109(2) . . ? O4 C6 C5 109.52(19) . . ? O4 C6 H6A 108.9(18) . . ? C5 C6 H6A 110.6(17) . . ? O4 C6 H6B 105.3(16) . . ? C5 C6 H6B 111.8(16) . . ? H6A C6 H6B 111(2) . . ? O4 C7 C8 104.7(2) . . ? O4 C7 H7A 108.5(17) . . ? C8 C7 H7A 113.1(17) . . ? O4 C7 H7B 110.0(16) . . ? C8 C7 H7B 112.5(17) . . ? H7A C7 H7B 108(2) . . ? O1 C8 C7 108.9(2) . . ? O1 C8 H8A 105(2) . . ? C7 C8 H8A 115(2) . . ? O1 C8 H8B 107.9(18) . . ? C7 C8 H8B 110.0(18) . . ? H8A C8 H8B 110(3) . . ? Si1 C9 Lu 135.44(11) . . ? Si1 C9 H9A 109.3(19) . . ? Lu C9 H9A 98.1(19) . . ? Si1 C9 H9B 105(2) . . ? Lu C9 H9B 104(2) . . ? H9A C9 H9B 100(3) . . ? Si1 C10 H10A 112.3(19) . . ? Si1 C10 H10B 107.9(17) . . ? H10A C10 H10B 108(3) . . ? Si1 C10 H10C 107(2) . . ? H10A C10 H10C 109(3) . . ? H10B C10 H10C 113(3) . . ? Si1 C11 H11A 113.0(17) . . ? Si1 C11 H11B 111.5(19) . . ? H11A C11 H11B 108(3) . . ? Si1 C11 H11C 111(3) . . ? H11A C11 H11C 109(3) . . ? H11B C11 H11C 103(3) . . ? Si1 C12 H12A 111(2) . . ? Si1 C12 H12B 108(3) . . ? H12A C12 H12B 101(3) . . ? Si1 C12 H12C 112(2) . . ? H12A C12 H12C 109(3) . . ? H12B C12 H12C 115(4) . . ? Si2 C13 Lu 127.31(11) . . ? Si2 C13 H13A 107.1(16) . . ? Lu C13 H13A 109.9(16) . . ? Si2 C13 H13B 105.8(16) . . ? Lu C13 H13B 101.8(16) . . ? H13A C13 H13B 102(2) . . ? Si2 C14 H14A 112(2) . . ? Si2 C14 H14B 110(3) . . ? H14A C14 H14B 110(3) . . ? Si2 C14 H14C 115(2) . . ? H14A C14 H14C 106(3) . . ? H14B C14 H14C 102(3) . . ? Si2 C15 H15A 112(3) . . ? Si2 C15 H15B 110(3) . . ? H15A C15 H15B 111(4) . . ? Si2 C15 H15C 110(2) . . ? H15A C15 H15C 104(4) . . ? H15B C15 H15C 110(3) . . ? Si2 C16 H16A 110(2) . . ? Si2 C16 H16B 119(3) . . ? H16A C16 H16B 103(3) . . ? Si2 C16 H16C 111(2) . . ? H16A C16 H16C 105(3) . . ? H16B C16 H16C 109(4) . . ? C18A C17 O5 106.4(3) . . ? C18A C17 C18B 31.6(4) . . ? O5 C17 C18B 103.8(3) . . ? C18A C17 H17A 99(2) . . ? O5 C17 H17A 107(2) . . ? C18B C17 H17A 128(2) . . ? C18A C17 H17B 127(2) . . ? O5 C17 H17B 110(2) . . ? C18B C17 H17B 102(2) . . ? H17A C17 H17B 105(3) . . ? C17 C18A C19 108.3(4) . . ? C17 C18A H18A 110.0 . . ? C19 C18A H18A 110.0 . . ? C17 C18A H18B 110.0 . . ? C19 C18A H18B 110.0 . . ? H18A C18A H18B 108.4 . . ? C19 C18B C17 103.0(3) . . ? C19 C18B H18C 111.2 . . ? C17 C18B H18C 111.2 . . ? C19 C18B H18D 111.2 . . ? C17 C18B H18D 111.2 . . ? H18C C18B H18D 109.1 . . ? C18B C19 C18A 33.2(3) . . ? C18B C19 C20 106.4(3) . . ? C18A C19 C20 105.2(3) . . ? C18B C19 H19A 135.1 . . ? C18A C19 H19A 110.7 . . ? C20 C19 H19A 110.7 . . ? C18B C19 H19B 79.9 . . ? C18A C19 H19B 110.7 . . ? C20 C19 H19B 110.7 . . ? H19A C19 H19B 108.8 . . ? C18B C19 H19C 110.5 . . ? C18A C19 H19C 80.6 . . ? C20 C19 H19C 110.5 . . ? H19A C19 H19C 32.0 . . ? H19B C19 H19C 132.1 . . ? C18B C19 H19D 110.5 . . ? C18A C19 H19D 136.3 . . ? C20 C19 H19D 110.5 . . ? H19A C19 H19D 79.4 . . ? H19B C19 H19D 32.5 . . ? H19C C19 H19D 108.6 . . ? O5 C20 C19 105.91(19) . . ? O5 C20 H20A 105.5(17) . . ? C19 C20 H20A 115.5(17) . . ? O5 C20 H20B 105.2(19) . . ? C19 C20 H20B 117.7(19) . . ? H20A C20 H20B 106(3) . . ? B C21 Si3 122.40(13) . . ? B C21 H21A 111.6(18) . . ? Si3 C21 H21A 106.2(18) . . ? B C21 H21B 108.9(14) . . ? Si3 C21 H21B 101.9(14) . . ? H21A C21 H21B 104(2) . . ? Si3 C22 H22A 118(2) . . ? Si3 C22 H22B 106(2) . . ? H22A C22 H22B 109(3) . . ? Si3 C22 H22C 113(2) . . ? H22A C22 H22C 104(3) . . ? H22B C22 H22C 106(3) . . ? Si3 C23 H23A 113(2) . . ? Si3 C23 H23B 110(3) . . ? H23A C23 H23B 110(3) . . ? Si3 C23 H23C 107.5(18) . . ? H23A C23 H23C 107(3) . . ? H23B C23 H23C 108(3) . . ? Si3 C24 H24A 106(2) . . ? Si3 C24 H24B 109.9(19) . . ? H24A C24 H24B 112(3) . . ? Si3 C24 H24C 113(2) . . ? H24A C24 H24C 113(3) . . ? H24B C24 H24C 103(3) . . ? C26 C25 C30 114.58(18) . . ? C26 C25 B 122.38(17) . . ? C30 C25 B 122.96(18) . . ? C27 C26 C25 122.8(2) . . ? C27 C26 H26 119.2(14) . . ? C25 C26 H26 117.9(14) . . ? C28 C27 C26 120.5(2) . . ? C28 C27 H27 120.2(17) . . ? C26 C27 H27 119.3(17) . . ? C27 C28 C29 118.7(2) . . ? C27 C28 H28 122.1(18) . . ? C29 C28 H28 119.2(18) . . ? C28 C29 C30 120.4(2) . . ? C28 C29 H29 118.1(16) . . ? C30 C29 H29 121.4(16) . . ? C29 C30 C25 123.0(2) . . ? C29 C30 H30 117.9(15) . . ? C25 C30 H30 119.1(15) . . ? C36 C31 C32 114.46(19) . . ? C36 C31 B 123.55(19) . . ? C32 C31 B 121.99(18) . . ? C33 C32 C31 122.9(2) . . ? C33 C32 H32 116.3(15) . . ? C31 C32 H32 120.6(15) . . ? C34 C33 C32 120.4(3) . . ? C34 C33 H33 120.7(19) . . ? C32 C33 H33 118.9(19) . . ? C35 C34 C33 118.7(2) . . ? C35 C34 H34 122(2) . . ? C33 C34 H34 120(2) . . ? C34 C35 C36 120.6(2) . . ? C34 C35 H35 123.5(18) . . ? C36 C35 H35 115.8(19) . . ? C35 C36 C31 123.0(2) . . ? C35 C36 H36 120.4(16) . . ? C31 C36 H36 116.6(16) . . ? C42 C37 C38 114.96(17) . . ? C42 C37 B 120.20(16) . . ? C38 C37 B 124.24(17) . . ? C39 C38 C37 122.97(19) . . ? C39 C38 H38 119.5(16) . . ? C37 C38 H38 117.5(16) . . ? C40 C39 C38 120.0(2) . . ? C40 C39 H39 120.3(14) . . ? C38 C39 H39 119.7(14) . . ? C41 C40 C39 119.08(19) . . ? C41 C40 H40 120.8(17) . . ? C39 C40 H40 120.1(17) . . ? C40 C41 C42 120.1(2) . . ? C40 C41 H41 122.4(16) . . ? C42 C41 H41 117.5(16) . . ? C41 C42 C37 122.82(18) . . ? C41 C42 H42 117.8(12) . . ? C37 C42 H42 119.3(12) . . ? 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 O5 Lu O1 C1 15.2(2) . . . . ? C9 Lu O1 C1 94.65(18) . . . . ? C13 Lu O1 C1 -169.55(16) . . . . ? O4 Lu O1 C1 -119.32(18) . . . . ? O2 Lu O1 C1 -5.99(16) . . . . ? O3 Lu O1 C1 -62.98(17) . . . . ? O5 Lu O1 C8 157.23(15) . . . . ? C9 Lu O1 C8 -123.28(17) . . . . ? C13 Lu O1 C8 -27.49(19) . . . . ? O4 Lu O1 C8 22.75(16) . . . . ? O2 Lu O1 C8 136.07(17) . . . . ? O3 Lu O1 C8 79.08(16) . . . . ? O5 Lu O2 C3 93.12(12) . . . . ? C9 Lu O2 C3 178.89(13) . . . . ? C13 Lu O2 C3 45.2(2) . . . . ? O4 Lu O2 C3 -42.98(13) . . . . ? O1 Lu O2 C3 -100.51(13) . . . . ? O3 Lu O2 C3 15.38(12) . . . . ? O5 Lu O2 C2 -133.65(13) . . . . ? C9 Lu O2 C2 -47.88(14) . . . . ? C13 Lu O2 C2 178.43(18) . . . . ? O4 Lu O2 C2 90.25(13) . . . . ? O1 Lu O2 C2 32.72(12) . . . . ? O3 Lu O2 C2 148.62(14) . . . . ? O5 Lu O3 C4 -65.07(13) . . . . ? C9 Lu O3 C4 -28.9(2) . . . . ? C13 Lu O3 C4 -151.72(14) . . . . ? O4 Lu O3 C4 130.35(14) . . . . ? O1 Lu O3 C4 74.53(14) . . . . ? O2 Lu O3 C4 17.43(13) . . . . ? O5 Lu O3 C5 159.04(16) . . . . ? C9 Lu O3 C5 -164.8(2) . . . . ? C13 Lu O3 C5 72.39(16) . . . . ? O4 Lu O3 C5 -5.54(15) . . . . ? O1 Lu O3 C5 -61.36(16) . . . . ? O2 Lu O3 C5 -118.45(16) . . . . ? O5 Lu O4 C7 -130.51(17) . . . . ? C9 Lu O4 C7 60.1(2) . . . . ? C13 Lu O4 C7 152.25(18) . . . . ? O1 Lu O4 C7 8.05(16) . . . . ? O2 Lu O4 C7 -50.21(18) . . . . ? O3 Lu O4 C7 -108.64(18) . . . . ? O5 Lu O4 C6 11.52(17) . . . . ? C9 Lu O4 C6 -157.90(15) . . . . ? C13 Lu O4 C6 -65.73(15) . . . . ? O1 Lu O4 C6 150.07(15) . . . . ? O2 Lu O4 C6 91.81(14) . . . . ? O3 Lu O4 C6 33.38(14) . . . . ? C9 Lu O5 C20 -44.63(18) . . . . ? C13 Lu O5 C20 -142.69(18) . . . . ? O4 Lu O5 C20 142.82(16) . . . . ? O1 Lu O5 C20 33.8(2) . . . . ? O2 Lu O5 C20 53.58(17) . . . . ? O3 Lu O5 C20 122.06(17) . . . . ? C9 Lu O5 C17 127.87(19) . . . . ? C13 Lu O5 C17 29.82(19) . . . . ? O4 Lu O5 C17 -44.7(2) . . . . ? O1 Lu O5 C17 -153.74(17) . . . . ? O2 Lu O5 C17 -133.91(18) . . . . ? O3 Lu O5 C17 -65.43(18) . . . . ? C8 O1 C1 C2 -162.5(2) . . . . ? Lu O1 C1 C2 -20.1(2) . . . . ? C3 O2 C2 C1 78.3(2) . . . . ? Lu O2 C2 C1 -57.12(19) . . . . ? O1 C1 C2 O2 49.7(2) . . . . ? C2 O2 C3 C4 -175.09(16) . . . . ? Lu O2 C3 C4 -43.34(18) . . . . ? C5 O3 C4 C3 92.3(2) . . . . ? Lu O3 C4 C3 -46.2(2) . . . . ? O2 C3 C4 O3 57.0(2) . . . . ? C4 O3 C5 C6 -158.0(2) . . . . ? Lu O3 C5 C6 -21.4(3) . . . . ? C7 O4 C6 C5 85.2(3) . . . . ? Lu O4 C6 C5 -59.7(2) . . . . ? O3 C5 C6 O4 51.4(3) . . . . ? C6 O4 C7 C8 -175.5(2) . . . . ? Lu O4 C7 C8 -34.7(2) . . . . ? C1 O1 C8 C7 94.8(2) . . . . ? Lu O1 C8 C7 -50.0(2) . . . . ? O4 C7 C8 O1 52.1(3) . . . . ? C10 Si1 C9 Lu -90.1(2) . . . . ? C12 Si1 C9 Lu 28.6(3) . . . . ? C11 Si1 C9 Lu 150.08(18) . . . . ? O5 Lu C9 Si1 169.88(19) . . . . ? C13 Lu C9 Si1 -102.42(19) . . . . ? O4 Lu C9 Si1 -17.4(3) . . . . ? O1 Lu C9 Si1 28.57(19) . . . . ? O2 Lu C9 Si1 93.58(19) . . . . ? O3 Lu C9 Si1 135.34(15) . . . . ? C14 Si2 C13 Lu -71.95(17) . . . . ? C15 Si2 C13 Lu 46.4(3) . . . . ? C16 Si2 C13 Lu 168.70(19) . . . . ? O5 Lu C13 Si2 160.61(14) . . . . ? C9 Lu C13 Si2 73.29(15) . . . . ? O4 Lu C13 Si2 -61.32(14) . . . . ? O1 Lu C13 Si2 -16.39(19) . . . . ? O2 Lu C13 Si2 -153.09(11) . . . . ? O3 Lu C13 Si2 -126.00(14) . . . . ? C20 O5 C17 C18A -19.8(5) . . . . ? Lu O5 C17 C18A 166.7(4) . . . . ? C20 O5 C17 C18B 12.9(3) . . . . ? Lu O5 C17 C18B -160.7(2) . . . . ? O5 C17 C18A C19 24.0(7) . . . . ? C18B C17 C18A C19 -65.9(7) . . . . ? C18A C17 C18B C19 69.1(7) . . . . ? O5 C17 C18B C19 -29.8(4) . . . . ? C17 C18B C19 C18A -58.1(5) . . . . ? C17 C18B C19 C20 34.8(4) . . . . ? C17 C18A C19 C18B 77.6(7) . . . . ? C17 C18A C19 C20 -19.1(7) . . . . ? C17 O5 C20 C19 7.6(3) . . . . ? Lu O5 C20 C19 -178.83(18) . . . . ? C18B C19 C20 O5 -27.9(4) . . . . ? C18A C19 C20 O5 6.6(5) . . . . ? C37 B C21 Si3 -54.8(2) . . . . ? C25 B C21 Si3 68.2(2) . . . . ? C31 B C21 Si3 -172.68(13) . . . . ? C22 Si3 C21 B 83.89(18) . . . . ? C24 Si3 C21 B -157.01(17) . . . . ? C23 Si3 C21 B -38.5(2) . . . . ? C37 B C25 C26 144.63(18) . . . . ? C31 B C25 C26 -95.1(2) . . . . ? C21 B C25 C26 25.7(2) . . . . ? C37 B C25 C30 -38.8(3) . . . . ? C31 B C25 C30 81.5(2) . . . . ? C21 B C25 C30 -157.73(18) . . . . ? C30 C25 C26 C27 0.4(3) . . . . ? B C25 C26 C27 177.23(18) . . . . ? C25 C26 C27 C28 -0.8(3) . . . . ? C26 C27 C28 C29 0.6(3) . . . . ? C27 C28 C29 C30 0.0(3) . . . . ? C28 C29 C30 C25 -0.4(3) . . . . ? C26 C25 C30 C29 0.3(3) . . . . ? B C25 C30 C29 -176.59(19) . . . . ? C37 B C31 C36 -107.2(2) . . . . ? C25 B C31 C36 130.21(19) . . . . ? C21 B C31 C36 8.8(2) . . . . ? C37 B C31 C32 72.6(2) . . . . ? C25 B C31 C32 -50.0(2) . . . . ? C21 B C31 C32 -171.41(17) . . . . ? C36 C31 C32 C33 0.5(3) . . . . ? B C31 C32 C33 -179.32(19) . . . . ? C31 C32 C33 C34 0.7(3) . . . . ? C32 C33 C34 C35 -1.6(3) . . . . ? C33 C34 C35 C36 1.3(3) . . . . ? C34 C35 C36 C31 -0.1(3) . . . . ? C32 C31 C36 C35 -0.8(3) . . . . ? B C31 C36 C35 179.01(19) . . . . ? C25 B C37 C42 161.39(16) . . . . ? C31 B C37 C42 42.0(2) . . . . ? C21 B C37 C42 -76.7(2) . . . . ? C25 B C37 C38 -28.0(3) . . . . ? C31 B C37 C38 -147.33(18) . . . . ? C21 B C37 C38 94.0(2) . . . . ? C42 C37 C38 C39 2.9(3) . . . . ? B C37 C38 C39 -168.20(19) . . . . ? C37 C38 C39 C40 -0.7(3) . . . . ? C38 C39 C40 C41 -1.3(3) . . . . ? C39 C40 C41 C42 0.8(3) . . . . ? C40 C41 C42 C37 1.6(3) . . . . ? C38 C37 C42 C41 -3.4(3) . . . . ? B C37 C42 C41 168.10(18) . . . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 1.077 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.066 #===END #============================================================================== data_sa22 _database_code_CSD 179962 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,4,7,10,13-pentaoxacyclopentadecane- bis(trimethylsilylmethyl)lutetium(III)- trimethylsilylmethyltriphenylborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H70 B Cl Lu O5 Si3' _chemical_formula_weight 948.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Lu' 'Lu' -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 17.0636(8) _cell_length_b 28.0660(10) _cell_length_c 19.7091(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9438.8(7) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3928 _exptl_absorpt_coefficient_mu 2.262 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.4648 _exptl_absorpt_correction_T_max 0.8857 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS diffactometer with CCD detector' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82918 _diffrn_reflns_av_R_equivalents 0.1670 _diffrn_reflns_av_sigmaI/netI 0.1409 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 28.30 _reflns_number_total 11723 _reflns_number_gt 5651 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART' _computing_cell_refinement 'SAINT' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-III for Windows, Farraguia, 1997)' _computing_publication_material 'WinGX Pulication Routines (Farraguia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00282(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11723 _refine_ls_number_parameters 477 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1445 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1591 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si -0.06824(17) 0.73163(10) 0.07145(12) 0.0482(7) Uani 1 1 d . . . Si2 Si 0.01450(14) 0.79518(8) 0.29762(12) 0.0336(6) Uani 1 1 d . . . Si3 Si 0.61879(13) 0.54065(8) 0.09292(11) 0.0309(5) Uani 1 1 d . . . O1 O 0.1575(3) 0.6879(2) 0.2516(3) 0.0315(13) Uani 1 1 d . . . O2 O 0.0636(3) 0.63467(19) 0.3268(2) 0.0301(13) Uani 1 1 d . . . O3 O -0.0777(3) 0.62844(19) 0.2711(2) 0.0331(13) Uani 1 1 d . . . O4 O -0.0242(3) 0.6046(2) 0.1553(3) 0.0441(16) Uani 1 1 d . . . O5 O 0.1251(3) 0.62029(19) 0.1659(3) 0.0353(14) Uani 1 1 d . . . Lu Lu 0.027508(17) 0.670350(11) 0.219500(14) 0.02171(12) Uani 1 1 d . . . Cl1 Cl 0.2818(3) 0.32503(19) 0.1172(3) 0.0459(12) Uiso 0.50 1 d P . . Cl2 Cl 0.2233(5) 0.1784(3) 0.1496(4) 0.093(2) Uiso 0.50 1 d P . . B B 0.7310(5) 0.4625(3) 0.0317(4) 0.027(2) Uani 1 1 d . . . C1 C 0.1873(5) 0.6715(3) 0.3184(4) 0.041(2) Uani 1 1 d . . . H1A H 0.2170 0.6414 0.3129 0.049 Uiso 1 1 calc R . . H1B H 0.2227 0.6958 0.3381 0.049 Uiso 1 1 calc R . . C2 C 0.1206(5) 0.6640(3) 0.3628(4) 0.038(2) Uani 1 1 d . . . H2A H 0.0968 0.6950 0.3753 0.045 Uiso 1 1 calc R . . H2B H 0.1375 0.6477 0.4049 0.045 Uiso 1 1 calc R . . C3 C -0.0002(5) 0.6207(4) 0.3705(4) 0.045(2) Uani 1 1 d . . . H3A H -0.0242 0.6490 0.3921 0.054 Uiso 1 1 calc R . . H3B H 0.0186 0.5989 0.4065 0.054 Uiso 1 1 calc R . . C4 C -0.0587(5) 0.5957(3) 0.3252(4) 0.045(2) Uani 1 1 d . . . H4A H -0.0357 0.5661 0.3064 0.054 Uiso 1 1 calc R . . H4B H -0.1064 0.5873 0.3512 0.054 Uiso 1 1 calc R . . C5 C -0.1334(5) 0.6089(3) 0.2235(4) 0.044(2) Uani 1 1 d . . . H5A H -0.1609 0.6351 0.1997 0.053 Uiso 1 1 calc R . . H5B H -0.1730 0.5897 0.2481 0.053 Uiso 1 1 calc R . . C6 C -0.0918(5) 0.5786(3) 0.1736(4) 0.050(3) Uani 1 1 d . . . H6A H -0.0773 0.5476 0.1941 0.059 Uiso 1 1 calc R . . H6B H -0.1252 0.5726 0.1334 0.059 Uiso 1 1 calc R . . C7 C 0.0228(5) 0.5830(4) 0.1033(5) 0.062(3) Uani 1 1 d . . . H7A H 0.0245 0.6038 0.0626 0.074 Uiso 1 1 calc R . . H7B H 0.0006 0.5518 0.0900 0.074 Uiso 1 1 calc R . . C8 C 0.1016(6) 0.5768(4) 0.1309(5) 0.062(3) Uani 1 1 d . . . H8A H 0.1022 0.5497 0.1629 0.074 Uiso 1 1 calc R . . H8B H 0.1388 0.5699 0.0937 0.074 Uiso 1 1 calc R . . C9 C 0.2076(5) 0.6290(3) 0.1739(4) 0.044(2) Uani 1 1 d . . . H9A H 0.2355 0.6246 0.1303 0.053 Uiso 1 1 calc R . . H9B H 0.2305 0.6072 0.2080 0.053 Uiso 1 1 calc R . . C10 C 0.2127(5) 0.6793(3) 0.1969(4) 0.040(2) Uani 1 1 d . . . H10A H 0.2666 0.6861 0.2128 0.048 Uiso 1 1 calc R . . H10B H 0.2010 0.7009 0.1585 0.048 Uiso 1 1 calc R . . C11 C 0.0203(5) 0.7135(3) 0.1167(4) 0.0346(19) Uani 1 1 d . . . H11A H 0.0501 0.7432 0.1247 0.041 Uiso 1 1 calc R . . H11B H 0.0513 0.6948 0.0835 0.041 Uiso 1 1 calc R . . C12 C -0.0482(6) 0.7721(4) -0.0030(5) 0.063(3) Uani 1 1 d . . . H12A H -0.0979 0.7823 -0.0231 0.095 Uiso 1 1 calc R . . H12B H -0.0173 0.7549 -0.0370 0.095 Uiso 1 1 calc R . . H12C H -0.0188 0.8001 0.0125 0.095 Uiso 1 1 calc R . . C13 C -0.1395(6) 0.7661(6) 0.1261(5) 0.103(5) Uani 1 1 d . . . H13A H -0.1608 0.7450 0.1612 0.154 Uiso 1 1 calc R . . H13B H -0.1824 0.7781 0.0978 0.154 Uiso 1 1 calc R . . H13C H -0.1124 0.7929 0.1475 0.154 Uiso 1 1 calc R . . C14 C -0.1226(8) 0.6784(4) 0.0387(6) 0.093(5) Uani 1 1 d . . . H14A H -0.1655 0.6890 0.0092 0.139 Uiso 1 1 calc R . . H14B H -0.1441 0.6603 0.0769 0.139 Uiso 1 1 calc R . . H14C H -0.0867 0.6581 0.0128 0.139 Uiso 1 1 calc R . . C15 C -0.0219(4) 0.7342(3) 0.2833(4) 0.0267(16) Uani 1 1 d . . . H15A H -0.0757 0.7388 0.2657 0.032 Uiso 1 1 calc R . . H15B H -0.0284 0.7209 0.3295 0.032 Uiso 1 1 calc R . . C16 C 0.0527(7) 0.8239(3) 0.2201(5) 0.059(3) Uani 1 1 d . . . H16A H 0.0663 0.8571 0.2300 0.088 Uiso 1 1 calc R . . H16B H 0.0126 0.8229 0.1845 0.088 Uiso 1 1 calc R . . H16C H 0.0995 0.8069 0.2046 0.088 Uiso 1 1 calc R . . C17 C -0.0601(6) 0.8372(3) 0.3312(7) 0.081(4) Uani 1 1 d . . . H17A H -0.1015 0.8416 0.2973 0.121 Uiso 1 1 calc R . . H17B H -0.0353 0.8679 0.3409 0.121 Uiso 1 1 calc R . . H17C H -0.0827 0.8242 0.3729 0.121 Uiso 1 1 calc R . . C18 C 0.1000(6) 0.7965(4) 0.3589(5) 0.076(4) Uani 1 1 d . . . H18A H 0.1161 0.8296 0.3666 0.115 Uiso 1 1 calc R . . H18B H 0.1439 0.7785 0.3397 0.115 Uiso 1 1 calc R . . H18C H 0.0842 0.7821 0.4021 0.115 Uiso 1 1 calc R . . C19 C 0.6474(4) 0.4793(3) 0.0699(4) 0.0291(18) Uani 1 1 d . . . H19A H 0.6449 0.4608 0.1126 0.035 Uiso 1 1 calc R . . H19B H 0.6046 0.4671 0.0408 0.035 Uiso 1 1 calc R . . C20 C 0.5281(5) 0.5379(4) 0.1450(5) 0.053(3) Uani 1 1 d . . . H20A H 0.4867 0.5218 0.1193 0.080 Uiso 1 1 calc R . . H20B H 0.5111 0.5703 0.1564 0.080 Uiso 1 1 calc R . . H20C H 0.5386 0.5201 0.1869 0.080 Uiso 1 1 calc R . . C21 C 0.6931(5) 0.5731(3) 0.1441(5) 0.053(3) Uani 1 1 d . . . H21A H 0.7054 0.5546 0.1849 0.080 Uiso 1 1 calc R . . H21B H 0.6722 0.6043 0.1572 0.080 Uiso 1 1 calc R . . H21C H 0.7408 0.5774 0.1171 0.080 Uiso 1 1 calc R . . C22 C 0.5959(6) 0.5770(3) 0.0169(4) 0.051(3) Uani 1 1 d . . . H22A H 0.6443 0.5839 -0.0079 0.077 Uiso 1 1 calc R . . H22B H 0.5713 0.6070 0.0311 0.077 Uiso 1 1 calc R . . H22C H 0.5598 0.5594 -0.0125 0.077 Uiso 1 1 calc R . . C23 C 0.7514(4) 0.4978(3) -0.0325(4) 0.0252(16) Uani 1 1 d . . . C24 C 0.7247(4) 0.4894(3) -0.0990(4) 0.0293(18) Uani 1 1 d . . . H24 H 0.6914 0.4629 -0.1071 0.035 Uiso 1 1 calc R . . C25 C 0.7455(5) 0.5187(3) -0.1535(4) 0.035(2) Uani 1 1 d . . . H25 H 0.7266 0.5111 -0.1976 0.042 Uiso 1 1 calc R . . C26 C 0.7917(5) 0.5576(3) -0.1454(4) 0.036(2) Uani 1 1 d . . . H26 H 0.8067 0.5769 -0.1828 0.043 Uiso 1 1 calc R . . C27 C 0.8162(5) 0.5680(3) -0.0797(4) 0.040(2) Uani 1 1 d . . . H27 H 0.8471 0.5956 -0.0717 0.047 Uiso 1 1 calc R . . C28 C 0.7960(5) 0.5386(3) -0.0258(4) 0.035(2) Uani 1 1 d . . . H28 H 0.8139 0.5471 0.0182 0.042 Uiso 1 1 calc R . . C29 C 0.7186(4) 0.4064(3) 0.0060(3) 0.0227(16) Uani 1 1 d . . . C30 C 0.7713(4) 0.3697(3) 0.0177(4) 0.0284(18) Uani 1 1 d . . . H30 H 0.8189 0.3771 0.0403 0.034 Uiso 1 1 calc R . . C31 C 0.7586(5) 0.3229(3) -0.0019(4) 0.0330(19) Uani 1 1 d . . . H31 H 0.7971 0.2993 0.0075 0.040 Uiso 1 1 calc R . . C32 C 0.6901(5) 0.3103(3) -0.0349(4) 0.034(2) Uani 1 1 d . . . H32 H 0.6805 0.2782 -0.0479 0.041 Uiso 1 1 calc R . . C33 C 0.6348(5) 0.3466(3) -0.0487(4) 0.0303(19) Uani 1 1 d . . . H33 H 0.5875 0.3393 -0.0718 0.036 Uiso 1 1 calc R . . C34 C 0.6500(4) 0.3924(3) -0.0285(4) 0.0279(18) Uani 1 1 d . . . H34 H 0.6119 0.4162 -0.0383 0.033 Uiso 1 1 calc R . . C35 C 0.8047(4) 0.4623(3) 0.0854(4) 0.0242(17) Uani 1 1 d . . . C36 C 0.7960(5) 0.4567(3) 0.1559(4) 0.0324(19) Uani 1 1 d . . . H36 H 0.7448 0.4574 0.1749 0.039 Uiso 1 1 calc R . . C37 C 0.8596(5) 0.4502(3) 0.1987(4) 0.036(2) Uani 1 1 d . . . H37 H 0.8511 0.4463 0.2460 0.043 Uiso 1 1 calc R . . C38 C 0.9342(5) 0.4492(3) 0.1740(5) 0.046(2) Uani 1 1 d . . . H38 H 0.9774 0.4447 0.2037 0.055 Uiso 1 1 calc R . . C39 C 0.9463(5) 0.4549(3) 0.1049(5) 0.042(2) Uani 1 1 d . . . H39 H 0.9978 0.4541 0.0867 0.050 Uiso 1 1 calc R . . C40 C 0.8827(5) 0.4616(3) 0.0629(4) 0.0331(19) Uani 1 1 d . . . H40 H 0.8922 0.4660 0.0158 0.040 Uiso 1 1 calc R . . C41 C 0.2758(14) 0.2607(10) 0.1152(12) 0.083(8) Uiso 0.50 1 d P . . H41A H 0.2451 0.2516 0.0746 0.100 Uiso 0.50 1 calc PR . . H41B H 0.3295 0.2481 0.1088 0.100 Uiso 0.50 1 calc PR . . C42 C 0.241(3) 0.2361(12) 0.1746(15) 0.129(12) Uiso 0.50 1 d P . . H42A H 0.1915 0.2519 0.1883 0.155 Uiso 0.50 1 calc PR . . H42B H 0.2776 0.2368 0.2135 0.155 Uiso 0.50 1 calc PR . . 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 Si1 0.0561(17) 0.0584(18) 0.0301(13) 0.0102(13) -0.0118(13) -0.0136(15) Si2 0.0361(14) 0.0275(12) 0.0373(13) -0.0068(10) 0.0102(10) -0.0060(10) Si3 0.0330(13) 0.0312(13) 0.0284(12) -0.0049(10) -0.0017(10) 0.0078(10) O1 0.020(3) 0.042(3) 0.033(3) 0.000(3) 0.001(2) 0.003(3) O2 0.024(3) 0.042(3) 0.025(3) 0.008(2) 0.000(2) 0.001(3) O3 0.034(3) 0.038(3) 0.027(3) -0.003(3) 0.004(2) -0.008(3) O4 0.034(3) 0.046(4) 0.052(4) -0.029(3) 0.021(3) -0.016(3) O5 0.030(3) 0.039(3) 0.037(3) -0.012(3) 0.002(3) 0.005(3) Lu 0.02232(17) 0.02426(18) 0.01856(16) -0.00088(15) 0.00091(14) -0.00072(15) B 0.033(5) 0.023(5) 0.023(4) -0.002(4) 0.001(4) 0.003(4) C1 0.034(5) 0.055(6) 0.032(5) 0.000(5) -0.014(4) 0.000(5) C2 0.041(5) 0.055(6) 0.016(4) 0.000(4) -0.010(3) 0.006(4) C3 0.036(5) 0.071(7) 0.027(5) 0.010(5) 0.006(4) 0.007(5) C4 0.046(5) 0.045(6) 0.043(5) 0.015(5) 0.017(4) 0.005(5) C5 0.030(5) 0.060(6) 0.043(5) -0.014(5) 0.003(4) -0.020(4) C6 0.050(6) 0.057(6) 0.042(6) -0.011(5) 0.013(5) -0.019(5) C7 0.049(6) 0.072(7) 0.065(7) -0.035(6) 0.022(6) -0.002(6) C8 0.062(7) 0.071(8) 0.053(6) -0.036(6) -0.003(5) 0.031(6) C9 0.029(5) 0.067(7) 0.037(5) 0.002(5) 0.008(4) 0.009(5) C10 0.027(5) 0.058(7) 0.033(5) 0.005(4) 0.002(4) 0.005(4) C11 0.041(5) 0.035(5) 0.028(4) 0.005(4) 0.004(4) 0.000(4) C12 0.068(7) 0.068(7) 0.053(6) 0.030(6) -0.021(5) -0.006(6) C13 0.044(7) 0.203(17) 0.063(8) 0.005(9) -0.015(6) 0.036(9) C14 0.134(12) 0.064(8) 0.081(9) 0.032(7) -0.073(8) -0.047(8) C15 0.023(4) 0.034(4) 0.024(4) 0.004(3) -0.001(4) 0.001(3) C16 0.071(7) 0.044(6) 0.062(7) -0.005(5) 0.024(6) -0.017(5) C17 0.064(7) 0.038(6) 0.140(12) -0.028(7) 0.055(8) -0.003(5) C18 0.075(8) 0.079(9) 0.075(8) -0.014(7) -0.015(6) -0.039(7) C19 0.030(4) 0.031(5) 0.027(4) 0.001(3) -0.003(3) 0.010(4) C20 0.057(6) 0.057(6) 0.045(6) 0.002(5) 0.015(5) 0.021(5) C21 0.061(6) 0.047(6) 0.052(6) -0.010(5) -0.015(5) 0.006(5) C22 0.056(6) 0.050(6) 0.048(6) 0.012(5) -0.001(5) 0.018(5) C23 0.024(4) 0.025(4) 0.027(4) -0.003(4) 0.003(3) 0.000(4) C24 0.028(4) 0.022(4) 0.037(5) -0.003(4) -0.004(4) 0.006(3) C25 0.049(5) 0.033(5) 0.023(4) 0.003(4) -0.003(4) 0.007(4) C26 0.038(5) 0.037(5) 0.033(5) 0.010(4) 0.000(4) -0.002(4) C27 0.046(5) 0.037(5) 0.036(5) 0.004(4) -0.005(4) -0.014(4) C28 0.043(5) 0.034(5) 0.028(4) -0.002(4) -0.004(4) -0.003(4) C29 0.021(4) 0.027(4) 0.021(4) 0.003(3) -0.004(3) 0.003(3) C30 0.030(4) 0.031(5) 0.025(4) -0.001(3) -0.006(3) 0.003(4) C31 0.037(5) 0.025(5) 0.037(5) 0.004(4) -0.005(4) 0.005(4) C32 0.054(6) 0.020(4) 0.028(4) -0.002(3) 0.000(4) -0.008(4) C33 0.035(5) 0.031(5) 0.024(4) -0.001(3) 0.002(4) -0.004(4) C34 0.023(4) 0.038(5) 0.022(4) -0.002(3) 0.001(3) -0.001(4) C35 0.028(4) 0.018(4) 0.027(4) -0.002(3) -0.002(3) 0.003(3) C36 0.043(5) 0.023(4) 0.032(4) -0.004(4) 0.001(4) 0.000(4) C37 0.052(6) 0.030(5) 0.026(4) 0.002(4) -0.011(4) 0.007(4) C38 0.053(6) 0.038(5) 0.046(6) -0.012(4) -0.028(5) 0.019(5) C39 0.031(5) 0.035(5) 0.059(6) -0.014(5) -0.003(4) 0.000(4) C40 0.039(5) 0.034(5) 0.026(4) -0.002(4) -0.008(4) 0.007(4) _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 Si1 C11 1.826(8) . ? Si1 C14 1.874(10) . ? Si1 C12 1.887(9) . ? Si1 C13 1.890(12) . ? Si2 C15 1.843(8) . ? Si2 C16 1.846(9) . ? Si2 C17 1.856(9) . ? Si2 C18 1.894(10) . ? Si3 C19 1.847(8) . ? Si3 C22 1.853(8) . ? Si3 C21 1.858(9) . ? Si3 C20 1.859(9) . ? O1 C10 1.451(9) . ? O1 C1 1.485(9) . ? O1 Lu 2.359(5) . ? O2 C3 1.443(9) . ? O2 C2 1.459(9) . ? O2 Lu 2.419(5) . ? O3 C5 1.443(9) . ? O3 C4 1.444(9) . ? O3 Lu 2.376(5) . ? O4 C6 1.411(9) . ? O4 C7 1.436(9) . ? O4 Lu 2.406(5) . ? O5 C9 1.437(9) . ? O5 C8 1.458(10) . ? O5 Lu 2.421(5) . ? Lu C15 2.345(7) . ? Lu C11 2.364(7) . ? Cl1 C41 1.81(3) . ? Cl2 C42 1.72(3) . ? B C35 1.643(11) . ? B C23 1.644(11) . ? B C29 1.666(11) . ? B C19 1.680(11) . ? C1 C2 1.451(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.511(12) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.482(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.459(12) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.486(12) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? 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 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C28 1.382(10) . ? C23 C24 1.407(10) . ? C24 C25 1.398(10) . ? C24 H24 0.9500 . ? C25 C26 1.357(11) . ? C25 H25 0.9500 . ? C26 C27 1.390(10) . ? C26 H26 0.9500 . ? C27 C28 1.388(11) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.386(10) . ? C29 C34 1.410(9) . ? C30 C31 1.388(10) . ? C30 H30 0.9500 . ? C31 C32 1.384(11) . ? C31 H31 0.9500 . ? C32 C33 1.415(11) . ? C32 H32 0.9500 . ? C33 C34 1.371(10) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C40 1.403(10) . ? C35 C36 1.407(10) . ? C36 C37 1.387(10) . ? C36 H36 0.9500 . ? C37 C38 1.364(12) . ? C37 H37 0.9500 . ? C38 C39 1.386(12) . ? C38 H38 0.9500 . ? C39 C40 1.378(11) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.48(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Si1 C14 110.8(5) . . ? C11 Si1 C12 113.4(4) . . ? C14 Si1 C12 107.6(5) . . ? C11 Si1 C13 113.4(4) . . ? C14 Si1 C13 106.6(6) . . ? C12 Si1 C13 104.6(6) . . ? C15 Si2 C16 113.4(4) . . ? C15 Si2 C17 114.4(4) . . ? C16 Si2 C17 105.1(5) . . ? C15 Si2 C18 112.1(4) . . ? C16 Si2 C18 104.3(5) . . ? C17 Si2 C18 106.8(6) . . ? C19 Si3 C22 111.7(4) . . ? C19 Si3 C21 114.2(4) . . ? C22 Si3 C21 108.2(5) . . ? C19 Si3 C20 108.5(4) . . ? C22 Si3 C20 107.1(4) . . ? C21 Si3 C20 106.8(4) . . ? C10 O1 C1 112.6(6) . . ? C10 O1 Lu 112.1(4) . . ? C1 O1 Lu 119.6(4) . . ? C3 O2 C2 111.4(6) . . ? C3 O2 Lu 116.3(4) . . ? C2 O2 Lu 111.2(4) . . ? C5 O3 C4 112.7(6) . . ? C5 O3 Lu 114.1(4) . . ? C4 O3 Lu 117.4(5) . . ? C6 O4 C7 115.0(7) . . ? C6 O4 Lu 124.2(5) . . ? C7 O4 Lu 119.5(5) . . ? C9 O5 C8 117.6(6) . . ? C9 O5 Lu 121.9(5) . . ? C8 O5 Lu 120.2(5) . . ? C15 Lu O1 92.0(2) . . ? C15 Lu C11 92.8(3) . . ? O1 Lu C11 99.9(2) . . ? C15 Lu O3 82.9(2) . . ? O1 Lu O3 134.41(18) . . ? C11 Lu O3 125.5(2) . . ? C15 Lu O4 137.4(2) . . ? O1 Lu O4 130.28(19) . . ? C11 Lu O4 85.6(3) . . ? O3 Lu O4 64.39(18) . . ? C15 Lu O2 86.5(2) . . ? O1 Lu O2 67.22(17) . . ? C11 Lu O2 167.1(2) . . ? O3 Lu O2 67.26(17) . . ? O4 Lu O2 103.6(2) . . ? C15 Lu O5 157.6(2) . . ? O1 Lu O5 65.90(18) . . ? C11 Lu O5 87.6(2) . . ? O3 Lu O5 114.79(18) . . ? O4 Lu O5 65.02(18) . . ? O2 Lu O5 88.04(17) . . ? C35 B C23 109.5(6) . . ? C35 B C29 106.9(6) . . ? C23 B C29 111.2(6) . . ? C35 B C19 111.2(6) . . ? C23 B C19 110.8(6) . . ? C29 B C19 107.1(6) . . ? C2 C1 O1 108.2(6) . . ? C2 C1 H1A 110.1 . . ? O1 C1 H1A 110.1 . . ? C2 C1 H1B 110.1 . . ? O1 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? C1 C2 O2 108.1(6) . . ? C1 C2 H2A 110.1 . . ? O2 C2 H2A 110.1 . . ? C1 C2 H2B 110.1 . . ? O2 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? O2 C3 C4 105.7(6) . . ? O2 C3 H3A 110.6 . . ? C4 C3 H3A 110.6 . . ? O2 C3 H3B 110.6 . . ? C4 C3 H3B 110.6 . . ? H3A C3 H3B 108.7 . . ? O3 C4 C3 106.9(7) . . ? O3 C4 H4A 110.3 . . ? C3 C4 H4A 110.3 . . ? O3 C4 H4B 110.3 . . ? C3 C4 H4B 110.3 . . ? H4A C4 H4B 108.6 . . ? O3 C5 C6 109.5(7) . . ? O3 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? O3 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? O4 C6 C5 105.4(7) . . ? O4 C6 H6A 110.7 . . ? C5 C6 H6A 110.7 . . ? O4 C6 H6B 110.7 . . ? C5 C6 H6B 110.7 . . ? H6A C6 H6B 108.8 . . ? O4 C7 C8 107.4(8) . . ? O4 C7 H7A 110.2 . . ? C8 C7 H7A 110.2 . . ? O4 C7 H7B 110.2 . . ? C8 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? O5 C8 C7 109.3(8) . . ? O5 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? O5 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.3 . . ? O5 C9 C10 104.6(7) . . ? O5 C9 H9A 110.8 . . ? C10 C9 H9A 110.8 . . ? O5 C9 H9B 110.8 . . ? C10 C9 H9B 110.8 . . ? H9A C9 H9B 108.9 . . ? O1 C10 C9 110.4(7) . . ? O1 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? O1 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? Si1 C11 Lu 127.2(4) . . ? Si1 C11 H11A 105.5 . . ? Lu C11 H11A 105.5 . . ? Si1 C11 H11B 105.5 . . ? Lu C11 H11B 105.5 . . ? H11A C11 H11B 106.1 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 Lu 132.1(4) . . ? Si2 C15 H15A 104.2 . . ? Lu C15 H15A 104.2 . . ? Si2 C15 H15B 104.2 . . ? Lu C15 H15B 104.2 . . ? H15A C15 H15B 105.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? B C19 Si3 126.6(6) . . ? B C19 H19A 105.7 . . ? Si3 C19 H19A 105.7 . . ? B C19 H19B 105.7 . . ? Si3 C19 H19B 105.7 . . ? H19A C19 H19B 106.1 . . ? Si3 C20 H20A 109.5 . . ? Si3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si3 C21 H21A 109.5 . . ? Si3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 C24 113.9(7) . . ? C28 C23 B 122.9(7) . . ? C24 C23 B 123.2(7) . . ? C25 C24 C23 122.4(7) . . ? C25 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? C26 C25 C24 121.9(8) . . ? C26 C25 H25 119.0 . . ? C24 C25 H25 119.0 . . ? C25 C26 C27 117.0(8) . . ? C25 C26 H26 121.5 . . ? C27 C26 H26 121.5 . . ? C28 C27 C26 120.8(8) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C23 C28 C27 123.8(8) . . ? C23 C28 H28 118.1 . . ? C27 C28 H28 118.1 . . ? C30 C29 C34 114.3(7) . . ? C30 C29 B 124.7(6) . . ? C34 C29 B 121.0(7) . . ? C29 C30 C31 123.9(7) . . ? C29 C30 H30 118.1 . . ? C31 C30 H30 118.1 . . ? C32 C31 C30 120.3(8) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 118.0(7) . . ? C31 C32 H32 121.0 . . ? C33 C32 H32 121.0 . . ? C34 C33 C32 119.6(7) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C29 124.0(8) . . ? C33 C34 H34 118.0 . . ? C29 C34 H34 118.0 . . ? C40 C35 C36 114.2(7) . . ? C40 C35 B 121.5(7) . . ? C36 C35 B 123.8(7) . . ? C37 C36 C35 122.2(8) . . ? C37 C36 H36 118.9 . . ? C35 C36 H36 118.9 . . ? C38 C37 C36 121.1(8) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C37 C38 C39 119.2(8) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C40 C39 C38 119.3(8) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C39 C40 C35 124.0(8) . . ? C39 C40 H40 118.0 . . ? C35 C40 H40 118.0 . . ? C42 C41 Cl1 118.0(19) . . ? C42 C41 H41A 107.8 . . ? Cl1 C41 H41A 107.8 . . ? C42 C41 H41B 107.8 . . ? Cl1 C41 H41B 107.8 . . ? H41A C41 H41B 107.1 . . ? C41 C42 Cl2 106.4(19) . . ? C41 C42 H42A 110.5 . . ? Cl2 C42 H42A 110.5 . . ? C41 C42 H42B 110.5 . . ? Cl2 C42 H42B 110.5 . . ? H42A C42 H42B 108.6 . . ? 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 C10 O1 Lu C15 -143.6(5) . . . . ? C1 O1 Lu C15 81.2(5) . . . . ? C10 O1 Lu C11 -50.4(5) . . . . ? C1 O1 Lu C11 174.5(5) . . . . ? C10 O1 Lu O3 134.3(5) . . . . ? C1 O1 Lu O3 -0.8(6) . . . . ? C10 O1 Lu O4 42.2(6) . . . . ? C1 O1 Lu O4 -92.9(6) . . . . ? C10 O1 Lu O2 131.0(5) . . . . ? C1 O1 Lu O2 -4.2(5) . . . . ? C10 O1 Lu O5 32.5(5) . . . . ? C1 O1 Lu O5 -102.6(5) . . . . ? C5 O3 Lu C15 119.9(6) . . . . ? C4 O3 Lu C15 -105.0(5) . . . . ? C5 O3 Lu O1 -154.3(5) . . . . ? C4 O3 Lu O1 -19.2(6) . . . . ? C5 O3 Lu C11 31.4(6) . . . . ? C4 O3 Lu C11 166.6(5) . . . . ? C5 O3 Lu O4 -32.0(5) . . . . ? C4 O3 Lu O4 103.1(6) . . . . ? C5 O3 Lu O2 -150.9(6) . . . . ? C4 O3 Lu O2 -15.8(5) . . . . ? C5 O3 Lu O5 -74.5(6) . . . . ? C4 O3 Lu O5 60.6(5) . . . . ? C6 O4 Lu C15 -36.6(8) . . . . ? C7 O4 Lu C15 157.0(6) . . . . ? C6 O4 Lu O1 134.8(6) . . . . ? C7 O4 Lu O1 -31.6(8) . . . . ? C6 O4 Lu C11 -126.0(7) . . . . ? C7 O4 Lu C11 67.7(7) . . . . ? C6 O4 Lu O3 7.1(6) . . . . ? C7 O4 Lu O3 -159.2(7) . . . . ? C6 O4 Lu O2 63.3(7) . . . . ? C7 O4 Lu O2 -103.1(7) . . . . ? C6 O4 Lu O5 144.6(7) . . . . ? C7 O4 Lu O5 -21.8(6) . . . . ? C3 O2 Lu C15 66.5(6) . . . . ? C2 O2 Lu C15 -62.4(5) . . . . ? C3 O2 Lu O1 160.1(6) . . . . ? C2 O2 Lu O1 31.2(4) . . . . ? C3 O2 Lu C11 154.1(10) . . . . ? C2 O2 Lu C11 25.2(12) . . . . ? C3 O2 Lu O3 -17.3(5) . . . . ? C2 O2 Lu O3 -146.2(5) . . . . ? C3 O2 Lu O4 -71.6(6) . . . . ? C2 O2 Lu O4 159.5(4) . . . . ? C3 O2 Lu O5 -135.3(6) . . . . ? C2 O2 Lu O5 95.8(5) . . . . ? C9 O5 Lu C15 3.6(9) . . . . ? C8 O5 Lu C15 176.4(7) . . . . ? C9 O5 Lu O1 -6.6(5) . . . . ? C8 O5 Lu O1 166.2(6) . . . . ? C9 O5 Lu C11 95.4(6) . . . . ? C8 O5 Lu C11 -91.9(6) . . . . ? C9 O5 Lu O3 -136.2(5) . . . . ? C8 O5 Lu O3 36.6(6) . . . . ? C9 O5 Lu O4 -178.4(6) . . . . ? C8 O5 Lu O4 -5.7(6) . . . . ? C9 O5 Lu O2 -72.4(6) . . . . ? C8 O5 Lu O2 100.3(6) . . . . ? C10 O1 C1 C2 -157.9(7) . . . . ? Lu O1 C1 C2 -23.0(9) . . . . ? O1 C1 C2 O2 49.9(9) . . . . ? C3 O2 C2 C1 172.9(7) . . . . ? Lu O2 C2 C1 -55.6(7) . . . . ? C2 O2 C3 C4 173.6(7) . . . . ? Lu O2 C3 C4 44.8(8) . . . . ? C5 O3 C4 C3 179.8(6) . . . . ? Lu O3 C4 C3 44.2(8) . . . . ? O2 C3 C4 O3 -55.4(9) . . . . ? C4 O3 C5 C6 -82.6(9) . . . . ? Lu O3 C5 C6 54.6(8) . . . . ? C7 O4 C6 C5 -176.0(8) . . . . ? Lu O4 C6 C5 17.1(10) . . . . ? O3 C5 C6 O4 -43.8(10) . . . . ? C6 O4 C7 C8 -122.8(9) . . . . ? Lu O4 C7 C8 44.7(11) . . . . ? C9 O5 C8 C7 -156.8(8) . . . . ? Lu O5 C8 C7 30.1(10) . . . . ? O4 C7 C8 O5 -45.2(11) . . . . ? C8 O5 C9 C10 168.1(7) . . . . ? Lu O5 C9 C10 -19.0(8) . . . . ? C1 O1 C10 C9 80.9(8) . . . . ? Lu O1 C10 C9 -57.5(7) . . . . ? O5 C9 C10 O1 47.4(8) . . . . ? C14 Si1 C11 Lu -66.1(7) . . . . ? C12 Si1 C11 Lu 172.8(5) . . . . ? C13 Si1 C11 Lu 53.7(8) . . . . ? C15 Lu C11 Si1 -69.5(5) . . . . ? O1 Lu C11 Si1 -162.0(5) . . . . ? O3 Lu C11 Si1 13.9(7) . . . . ? O4 Lu C11 Si1 67.9(5) . . . . ? O2 Lu C11 Si1 -156.4(7) . . . . ? O5 Lu C11 Si1 133.0(5) . . . . ? C16 Si2 C15 Lu 42.3(7) . . . . ? C17 Si2 C15 Lu 162.8(6) . . . . ? C18 Si2 C15 Lu -75.5(6) . . . . ? O1 Lu C15 Si2 39.0(5) . . . . ? C11 Lu C15 Si2 -61.0(5) . . . . ? O3 Lu C15 Si2 173.6(5) . . . . ? O4 Lu C15 Si2 -147.5(4) . . . . ? O2 Lu C15 Si2 106.1(5) . . . . ? O5 Lu C15 Si2 29.7(9) . . . . ? C35 B C19 Si3 76.9(8) . . . . ? C23 B C19 Si3 -45.2(9) . . . . ? C29 B C19 Si3 -166.7(5) . . . . ? C22 Si3 C19 B 70.5(7) . . . . ? C21 Si3 C19 B -52.8(8) . . . . ? C20 Si3 C19 B -171.7(6) . . . . ? C35 B C23 C28 -33.1(10) . . . . ? C29 B C23 C28 -151.0(7) . . . . ? C19 B C23 C28 89.9(9) . . . . ? C35 B C23 C24 147.3(7) . . . . ? C29 B C23 C24 29.3(10) . . . . ? C19 B C23 C24 -89.7(8) . . . . ? C28 C23 C24 C25 3.2(11) . . . . ? B C23 C24 C25 -177.1(7) . . . . ? C23 C24 C25 C26 -1.2(12) . . . . ? C24 C25 C26 C27 -1.6(12) . . . . ? C25 C26 C27 C28 2.2(13) . . . . ? C24 C23 C28 C27 -2.7(12) . . . . ? B C23 C28 C27 177.6(8) . . . . ? C26 C27 C28 C23 0.1(13) . . . . ? C35 B C29 C30 -11.9(10) . . . . ? C23 B C29 C30 107.6(8) . . . . ? C19 B C29 C30 -131.2(7) . . . . ? C35 B C29 C34 166.0(6) . . . . ? C23 B C29 C34 -74.5(9) . . . . ? C19 B C29 C34 46.7(9) . . . . ? C34 C29 C30 C31 -0.6(11) . . . . ? B C29 C30 C31 177.4(7) . . . . ? C29 C30 C31 C32 -0.2(12) . . . . ? C30 C31 C32 C33 0.9(12) . . . . ? C31 C32 C33 C34 -0.8(11) . . . . ? C32 C33 C34 C29 0.0(11) . . . . ? C30 C29 C34 C33 0.7(11) . . . . ? B C29 C34 C33 -177.4(7) . . . . ? C23 B C35 C40 -40.6(9) . . . . ? C29 B C35 C40 80.0(9) . . . . ? C19 B C35 C40 -163.4(7) . . . . ? C23 B C35 C36 148.0(7) . . . . ? C29 B C35 C36 -91.4(8) . . . . ? C19 B C35 C36 25.2(10) . . . . ? C40 C35 C36 C37 -1.0(11) . . . . ? B C35 C36 C37 170.9(7) . . . . ? C35 C36 C37 C38 0.3(13) . . . . ? C36 C37 C38 C39 0.1(13) . . . . ? C37 C38 C39 C40 0.3(13) . . . . ? C38 C39 C40 C35 -1.1(13) . . . . ? C36 C35 C40 C39 1.4(12) . . . . ? B C35 C40 C39 -170.7(8) . . . . ? Cl1 C41 C42 Cl2 166.6(18) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.614 _refine_diff_density_min -1.036 _refine_diff_density_rms 0.223 #===END #============================================================================== data_sa23 _database_code_CSD 179963 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,4,7,10,13,16-hexaoxacyclooctadecane- bis(trimethylsilylmethyl)lutetium(III)- trimethylsilylmethyltriphenylborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H74 B Cl Lu O6 Si3' _chemical_formula_weight 992.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Lu' 'Lu' -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.5050(5) _cell_length_b 16.3955(8) _cell_length_c 30.297(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5218.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prism' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2060 _exptl_absorpt_coefficient_mu 2.051 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.5736 _exptl_absorpt_correction_T_max 0.7324 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? 'Bruker AXS diffactometer with CCD detector' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48035 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0642 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 28.31 _reflns_number_total 12892 _reflns_number_gt 10241 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART' _computing_cell_refinement 'SAINT' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-III for Windows (Farraguia, 1997)' _computing_publication_material 'WinGX Publication Routines (Farraguia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0766P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.008(11) _refine_ls_number_reflns 12892 _refine_ls_number_parameters 480 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1300 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B B 1.0994(9) 0.4020(5) 0.8735(2) 0.0391(17) Uani 1 1 d . . . Lu Lu 0.60236(2) 0.054001(15) 0.847118(8) 0.02852(8) Uani 1 1 d . A . O1 O 0.7561(5) -0.0424(3) 0.88485(17) 0.0470(13) Uani 1 1 d . . . O2 O 0.6770(5) -0.0590(4) 0.80261(17) 0.0528(13) Uani 1 1 d . . . O3 O 0.8091(5) 0.0735(4) 0.81270(17) 0.0544(15) Uani 1 1 d . . . O4 O 0.6987(5) 0.1876(3) 0.8574(2) 0.0573(16) Uani 1 1 d . . . O5 O 0.4695(5) 0.1528(3) 0.88299(15) 0.0373(11) Uani 1 1 d . . . O6 O 0.6413(5) 0.0688(4) 0.92893(16) 0.0580(16) Uani 1 1 d . . . Si1A Si 0.2785(6) -0.0473(5) 0.8819(2) 0.0792(16) Uiso 0.50 1 d P A 1 Si1B Si 0.2732(3) -0.0411(2) 0.85279(14) 0.0338(8) Uiso 0.50 1 d P A 2 Si2 Si 0.5370(3) 0.17183(17) 0.73565(8) 0.0678(8) Uani 1 1 d . A . Si3 Si 1.0585(2) 0.58043(14) 0.90656(9) 0.0543(6) Uani 1 1 d . . . C1 C 0.8040(9) -0.1139(5) 0.8637(3) 0.059(2) Uani 1 1 d . . . H1A H 0.8067 -0.1600 0.8847 0.071 Uiso 1 1 calc R . . H1B H 0.8912 -0.1042 0.8524 0.071 Uiso 1 1 calc R . . C2 C 0.7128(9) -0.1332(5) 0.8253(3) 0.057(2) Uani 1 1 d . . . H2A H 0.7550 -0.1708 0.8043 0.068 Uiso 1 1 calc R . . H2B H 0.6357 -0.1606 0.8368 0.068 Uiso 1 1 calc R . . C3 C 0.7581(11) -0.0343(7) 0.7675(3) 0.081(4) Uani 1 1 d . . . H3A H 0.7079 -0.0031 0.7456 0.098 Uiso 1 1 calc R . . H3B H 0.7924 -0.0833 0.7526 0.098 Uiso 1 1 calc R . . C4 C 0.8626(9) 0.0154(6) 0.7828(3) 0.071(3) Uani 1 1 d . . . H4A H 0.9269 -0.0186 0.7980 0.085 Uiso 1 1 calc R . . H4B H 0.9040 0.0435 0.7577 0.085 Uiso 1 1 calc R . . C5 C 0.8927(11) 0.1353(8) 0.8274(6) 0.131(6) Uani 1 1 d . . . H5A H 0.9493 0.1129 0.8505 0.158 Uiso 1 1 calc R . . H5B H 0.9466 0.1535 0.8025 0.158 Uiso 1 1 calc R . . C6 C 0.8259(10) 0.2026(7) 0.8445(3) 0.082(4) Uani 1 1 d . . . H6A H 0.8256 0.2463 0.8219 0.098 Uiso 1 1 calc R . . H6B H 0.8732 0.2236 0.8704 0.098 Uiso 1 1 calc R . . C7 C 0.6285(9) 0.2567(5) 0.8713(3) 0.057(2) Uani 1 1 d . . . H7A H 0.6479 0.3042 0.8523 0.068 Uiso 1 1 calc R . . H7B H 0.6498 0.2708 0.9022 0.068 Uiso 1 1 calc R . . C8 C 0.4925(8) 0.2343(5) 0.8675(3) 0.051(2) Uani 1 1 d . . . H8A H 0.4407 0.2731 0.8850 0.061 Uiso 1 1 calc R . . H8B H 0.4658 0.2386 0.8363 0.061 Uiso 1 1 calc R . . C9 C 0.4527(8) 0.1445(6) 0.9290(2) 0.052(2) Uani 1 1 d . . . H9A H 0.3965 0.0973 0.9350 0.062 Uiso 1 1 calc R . . H9B H 0.4103 0.1940 0.9407 0.062 Uiso 1 1 calc R . . 10 C 0.5721(8) 0.1330(5) 0.9518(2) 0.055(2) Uani 1 1 d . . . H10A H 0.5565 0.1171 0.9829 0.066 Uiso 1 1 calc R . . H10B H 0.6220 0.1842 0.9516 0.066 Uiso 1 1 calc R . . C11 C 0.7432(9) 0.0336(5) 0.9503(3) 0.059(2) Uani 1 1 d . . . H11A H 0.8115 0.0748 0.9535 0.071 Uiso 1 1 calc R . . H11B H 0.7163 0.0170 0.9803 0.071 Uiso 1 1 calc R . . C12 C 0.7908(13) -0.0322(7) 0.9289(3) 0.093(4) Uani 1 1 d . . . H12A H 0.7642 -0.0816 0.9453 0.112 Uiso 1 1 calc R . . H12B H 0.8848 -0.0294 0.9304 0.112 Uiso 1 1 calc R . . C13 C 0.4440(7) -0.0404(5) 0.8688(3) 0.059(2) Uani 1 1 d . . . H13A H 0.4524 -0.0828 0.8457 0.070 Uiso 0.50 1 calc PR A 1 H13B H 0.4833 -0.0650 0.8954 0.070 Uiso 0.50 1 calc PR A 1 H13C H 0.4772 -0.0946 0.8602 0.070 Uiso 0.50 1 calc PR A 2 H13D H 0.4445 -0.0396 0.9015 0.070 Uiso 0.50 1 calc PR A 2 C14A C 0.1971(7) -0.1386(5) 0.8843(3) 0.102(10) Uiso 0.50 1 d PR A 1 H14A H 0.2149 -0.1701 0.8575 0.153 Uiso 0.50 1 d PR A 1 H14B H 0.1055 -0.1280 0.8864 0.153 Uiso 0.50 1 d PR A 1 H14C H 0.2249 -0.1697 0.9102 0.153 Uiso 0.50 1 d PR A 1 C15A C 0.254(3) -0.043(2) 0.8253(11) 0.130(10) Uiso 0.50 1 d P A 1 H15A H 0.2081 0.0078 0.8185 0.195 Uiso 0.50 1 d PR A 1 H15B H 0.2026 -0.0896 0.8158 0.195 Uiso 0.50 1 d PR A 1 H15C H 0.3355 -0.0433 0.8098 0.195 Uiso 0.50 1 d PR A 1 C16A C 0.194(3) 0.0416(17) 0.9010(9) 0.108(8) Uiso 0.50 1 d P A 1 H16A H 0.1055 0.0271 0.9071 0.162 Uiso 0.50 1 d PR A 1 H16B H 0.1972 0.0836 0.8781 0.162 Uiso 0.50 1 d PR A 1 H16C H 0.2340 0.0624 0.9281 0.162 Uiso 0.50 1 d PR A 1 C14B C 0.189(2) -0.1387(11) 0.8662(8) 0.065(5) Uiso 0.50 1 d P A 2 H14D H 0.1943 -0.1519 0.8977 0.097 Uiso 0.50 1 d PR A 2 H14E H 0.2270 -0.1828 0.8489 0.097 Uiso 0.50 1 d PR A 2 H14F H 0.0989 -0.1326 0.8579 0.097 Uiso 0.50 1 d PR A 2 C15B C 0.2453(17) -0.0335(10) 0.7911(6) 0.055(4) Uiso 0.50 1 d P A 2 H15D H 0.1601 -0.0541 0.7841 0.082 Uiso 0.50 1 d PR A 2 H15E H 0.3092 -0.0662 0.7756 0.082 Uiso 0.50 1 d PR A 2 H15F H 0.2522 0.0236 0.7819 0.082 Uiso 0.50 1 d PR A 2 C16B C 0.1800(16) 0.0417(10) 0.8715(6) 0.052(4) Uiso 0.50 1 d P A 2 H16D H 0.2324 0.0782 0.8895 0.078 Uiso 0.50 1 d PR A 2 H16E H 0.1090 0.0211 0.8893 0.078 Uiso 0.50 1 d PR A 2 H16F H 0.1465 0.0717 0.8460 0.078 Uiso 0.50 1 d PR A 2 C17 C 0.5035(8) 0.0990(5) 0.7811(3) 0.0473(18) Uiso 1 1 d . . . H17A H 0.4880 0.0473 0.7651 0.057 Uiso 1 1 calc R A . H17B H 0.4185 0.1167 0.7915 0.057 Uiso 1 1 calc R . . C18 C 0.6995(16) 0.1594(9) 0.7093(4) 0.138(7) Uani 1 1 d . . . H18A H 0.6938 0.1204 0.6849 0.207 Uiso 1 1 calc R A . H18B H 0.7600 0.1391 0.7314 0.207 Uiso 1 1 calc R . . H18C H 0.7288 0.2122 0.6981 0.207 Uiso 1 1 calc R . . C19 C 0.5237(12) 0.2807(6) 0.7513(3) 0.082(3) Uani 1 1 d . . . H19A H 0.5337 0.3148 0.7250 0.122 Uiso 1 1 calc R A . H19B H 0.5903 0.2942 0.7727 0.122 Uiso 1 1 calc R . . H19C H 0.4399 0.2907 0.7645 0.122 Uiso 1 1 calc R . . C20 C 0.4240(13) 0.1603(6) 0.6889(3) 0.099(5) Uani 1 1 d . . . H20A H 0.4504 0.1957 0.6645 0.149 Uiso 1 1 calc R A . H20B H 0.3382 0.1756 0.6986 0.149 Uiso 1 1 calc R . . H20C H 0.4236 0.1034 0.6790 0.149 Uiso 1 1 calc R . . C21 C 1.0413(8) 0.4949(5) 0.8673(3) 0.0484(19) Uani 1 1 d . . . H21A H 0.9485 0.4878 0.8629 0.058 Uiso 1 1 calc R . . H21B H 1.0755 0.5150 0.8389 0.058 Uiso 1 1 calc R . . C22 C 1.2220(11) 0.6136(6) 0.9152(4) 0.086(3) Uani 1 1 d . . . H22A H 1.2241 0.6557 0.9382 0.129 Uiso 1 1 calc R . . H22B H 1.2559 0.6361 0.8876 0.129 Uiso 1 1 calc R . . H22C H 1.2740 0.5670 0.9244 0.129 Uiso 1 1 calc R . . C23 C 0.9877(12) 0.5575(7) 0.9621(4) 0.089(3) Uani 1 1 d . . . H23A H 1.0453 0.5217 0.9786 0.134 Uiso 1 1 calc R . . H23B H 0.9054 0.5302 0.9582 0.134 Uiso 1 1 calc R . . H23C H 0.9754 0.6085 0.9784 0.134 Uiso 1 1 calc R . . C24 C 0.9722(10) 0.6721(6) 0.8851(4) 0.085(3) Uani 1 1 d . . . H24A H 0.8926 0.6550 0.8711 0.127 Uiso 1 1 calc R . . H24B H 1.0257 0.7002 0.8634 0.127 Uiso 1 1 calc R . . H24C H 0.9533 0.7092 0.9096 0.127 Uiso 1 1 calc R . . C25 C 1.2513(7) 0.4112(4) 0.8862(2) 0.0350(15) Uani 1 1 d . . . C26 C 1.3019(7) 0.4041(4) 0.9286(2) 0.0380(16) Uani 1 1 d . . . H26 H 1.2461 0.3875 0.9516 0.046 Uiso 1 1 calc R . . C27 C 1.4263(6) 0.4192(4) 0.9395(2) 0.0403(17) Uani 1 1 d . . . H27 H 1.4536 0.4139 0.9693 0.048 Uiso 1 1 calc R . . C28 C 1.5128(7) 0.4425(5) 0.9068(3) 0.0459(16) Uani 1 1 d . . . H28 H 1.5992 0.4541 0.9136 0.055 Uiso 1 1 calc R . . C29 C 1.4672(7) 0.4480(5) 0.8641(3) 0.0484(17) Uani 1 1 d . . . H29 H 1.5243 0.4628 0.8412 0.058 Uiso 1 1 calc R . . C30 C 1.3425(7) 0.4328(4) 0.8537(2) 0.0434(17) Uani 1 1 d . . . H30 H 1.3163 0.4369 0.8238 0.052 Uiso 1 1 calc R . . C31 C 1.0235(7) 0.3482(4) 0.9101(2) 0.0400(16) Uani 1 1 d . . . C32 C 0.9069(8) 0.3711(4) 0.9281(2) 0.0399(15) Uani 1 1 d . . . H32 H 0.8709 0.4219 0.9197 0.048 Uiso 1 1 calc R . . C33 C 0.8408(7) 0.3225(5) 0.9581(3) 0.0457(18) Uani 1 1 d . . . H33 H 0.7608 0.3406 0.9689 0.055 Uiso 1 1 calc R . . C34 C 0.8876(8) 0.2502(4) 0.9723(2) 0.0458(18) Uani 1 1 d . . . H34 H 0.8417 0.2173 0.9927 0.055 Uiso 1 1 calc R . . C35 C 1.0057(8) 0.2258(5) 0.9560(2) 0.0470(18) Uani 1 1 d . . . H35 H 1.0432 0.1764 0.9660 0.056 Uiso 1 1 calc R . . C36 C 1.0680(7) 0.2732(4) 0.9253(2) 0.0385(16) Uani 1 1 d . . . H36 H 1.1463 0.2536 0.9138 0.046 Uiso 1 1 calc R . . C37 C 1.0875(7) 0.3487(4) 0.8273(2) 0.0435(17) Uani 1 1 d . . . C38 C 0.9924(8) 0.3628(6) 0.7948(3) 0.057(2) Uani 1 1 d . . . H38 H 0.9340 0.4061 0.7995 0.068 Uiso 1 1 calc R . . C39 C 0.9803(10) 0.3172(6) 0.7570(3) 0.062(3) Uani 1 1 d . . . H39 H 0.9147 0.3297 0.7365 0.074 Uiso 1 1 calc R . . C40 C 1.0593(11) 0.2557(7) 0.7487(3) 0.074(3) Uani 1 1 d . . . H40 H 1.0503 0.2255 0.7221 0.089 Uiso 1 1 calc R . . C41 C 1.1575(9) 0.2344(6) 0.7792(3) 0.064(2) Uani 1 1 d . . . H41 H 1.2118 0.1891 0.7740 0.077 Uiso 1 1 calc R . . C42 C 1.1710(4) 0.2838(3) 0.81762(15) 0.050(2) Uani 1 1 d . . . H42 H 1.2387 0.2725 0.8375 0.060 Uiso 1 1 calc R . . Cl1 Cl 0.1146(4) -0.0567(3) 0.99217(15) 0.1048(18) Uiso 0.50 1 d PRD . . Cl2 Cl 0.0519(4) -0.2716(3) 1.06986(15) 0.151(3) Uiso 0.50 1 d PRD B . C43A C 0.1519(4) -0.1582(3) 1.00836(15) 0.58(17) Uiso 0.25 1 d PRD B 1 H43A H 0.1794 -0.1898 0.9822 0.695 Uiso 0.25 1 calc PR C 1 H43B H 0.2233 -0.1573 1.0297 0.695 Uiso 0.25 1 calc PR D 1 C43B C 0.035(2) -0.1527(14) 0.9854(9) 0.42(11) Uiso 0.25 1 d PD B 2 H43C H -0.0554 -0.1435 0.9769 0.509 Uiso 0.25 1 calc PR B 2 H43D H 0.0761 -0.1849 0.9618 0.509 Uiso 0.25 1 calc PR B 2 C44 C 0.041(2) -0.1987(14) 1.0288(9) 0.33(4) Uiso 0.50 1 d PRD . . H44A H -0.0076 -0.2240 1.0044 0.398 Uiso 0.25 1 calc PR B 1 H44B H -0.0135 -0.1546 1.0408 0.398 Uiso 0.25 1 calc PR B 1 H44C H -0.0379 -0.1739 1.0408 0.398 Uiso 0.25 1 calc PR B 2 H44D H 0.1089 -0.1638 1.0413 0.398 Uiso 0.25 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B 0.037(4) 0.045(4) 0.035(4) 0.018(3) -0.002(4) -0.001(4) Lu 0.02913(11) 0.02760(12) 0.02883(12) -0.00590(11) -0.00131(12) -0.00173(11) O1 0.051(3) 0.043(3) 0.046(3) -0.005(2) -0.010(2) 0.010(3) O2 0.054(3) 0.051(3) 0.053(3) -0.015(3) -0.011(2) 0.011(3) O3 0.034(3) 0.082(4) 0.047(3) 0.004(3) 0.010(2) -0.008(3) O4 0.043(3) 0.037(3) 0.092(5) 0.006(3) -0.004(3) -0.011(2) O5 0.044(3) 0.034(3) 0.034(3) -0.007(2) 0.001(2) 0.002(2) O6 0.067(4) 0.073(4) 0.034(3) -0.009(3) -0.007(2) 0.025(3) Si2 0.105(2) 0.0649(16) 0.0338(12) 0.0010(11) -0.0104(12) 0.0322(15) Si3 0.0637(15) 0.0381(12) 0.0612(14) 0.0117(10) -0.0060(11) 0.0063(10) C1 0.069(6) 0.059(5) 0.049(5) -0.001(4) -0.002(4) 0.027(5) C2 0.070(6) 0.037(4) 0.063(5) -0.018(4) -0.012(4) 0.013(4) C3 0.107(8) 0.109(9) 0.028(4) -0.006(5) 0.010(5) 0.063(7) C4 0.065(6) 0.091(7) 0.056(5) 0.012(5) 0.027(5) 0.026(5) C5 0.043(5) 0.087(8) 0.26(2) 0.000(10) 0.023(9) -0.022(6) C6 0.085(7) 0.117(8) 0.044(5) -0.009(6) 0.015(5) -0.077(7) C7 0.077(7) 0.033(4) 0.060(5) -0.005(4) -0.010(4) -0.019(4) C8 0.071(5) 0.040(4) 0.042(4) -0.009(3) -0.018(4) 0.010(4) C9 0.048(4) 0.072(6) 0.035(4) -0.013(4) 0.009(3) 0.011(4) 10 0.071(6) 0.066(5) 0.028(4) -0.006(3) 0.010(4) 0.007(4) C11 0.063(5) 0.059(6) 0.056(5) -0.012(4) -0.026(4) 0.017(4) C12 0.122(10) 0.097(9) 0.060(6) -0.014(6) -0.033(6) 0.061(8) C13 0.038(4) 0.044(5) 0.094(7) -0.008(5) 0.007(4) -0.004(3) C18 0.217(17) 0.112(10) 0.086(9) 0.056(8) 0.069(10) 0.046(12) C19 0.112(9) 0.075(7) 0.058(6) 0.023(5) 0.011(6) 0.024(6) C20 0.174(13) 0.069(7) 0.054(6) -0.015(5) -0.049(7) 0.044(8) C21 0.049(4) 0.056(5) 0.041(4) 0.018(4) -0.004(3) -0.003(4) C22 0.096(9) 0.052(6) 0.110(9) -0.016(6) -0.019(7) 0.008(6) C23 0.131(10) 0.051(5) 0.085(7) -0.014(6) 0.014(7) 0.001(7) C24 0.078(7) 0.052(6) 0.124(10) 0.021(6) -0.025(7) 0.002(5) C25 0.040(4) 0.029(3) 0.036(4) 0.002(3) -0.002(3) -0.014(3) C26 0.046(4) 0.037(4) 0.031(3) 0.005(3) 0.003(3) -0.006(3) C27 0.038(4) 0.042(4) 0.040(4) -0.001(3) -0.009(3) -0.002(3) C28 0.045(4) 0.032(4) 0.061(5) -0.004(4) -0.009(3) 0.001(4) C29 0.054(4) 0.034(4) 0.058(4) 0.009(4) 0.005(3) -0.010(4) C30 0.053(4) 0.040(4) 0.037(4) 0.011(3) -0.007(3) -0.013(3) C31 0.036(4) 0.039(4) 0.045(4) 0.009(3) -0.008(3) -0.006(3) C32 0.040(4) 0.045(4) 0.034(3) 0.002(3) -0.005(3) -0.005(4) C33 0.036(4) 0.056(5) 0.046(4) -0.009(4) -0.006(3) -0.019(3) C34 0.060(5) 0.049(4) 0.029(3) -0.004(3) 0.005(4) -0.025(4) C35 0.058(5) 0.041(4) 0.042(4) 0.003(3) -0.017(4) -0.015(4) C36 0.040(4) 0.040(4) 0.036(4) 0.000(3) -0.003(3) -0.010(3) C37 0.048(4) 0.047(4) 0.036(3) 0.015(3) -0.003(3) -0.021(4) C38 0.054(5) 0.066(6) 0.049(5) 0.027(4) -0.009(4) -0.028(4) C39 0.078(7) 0.064(6) 0.044(5) 0.022(4) -0.022(5) -0.039(5) C40 0.094(8) 0.093(8) 0.036(5) 0.005(5) -0.005(5) -0.052(7) C41 0.076(6) 0.061(6) 0.056(5) -0.004(4) 0.012(5) -0.025(5) C42 0.053(5) 0.053(5) 0.042(4) 0.006(4) -0.001(4) -0.023(4) _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 B C31 1.626(10) . ? B C25 1.648(12) . ? B C21 1.652(11) . ? B C37 1.655(11) . ? Lu C13 2.366(8) . ? Lu C17 2.371(8) . ? Lu O5 2.399(5) . ? Lu O2 2.422(5) . ? Lu O3 2.431(5) . ? Lu O4 2.433(5) . ? Lu O6 2.524(5) . ? Lu O1 2.532(5) . ? O1 C12 1.394(10) . ? O1 C1 1.428(9) . ? O2 C3 1.422(11) . ? O2 C2 1.447(10) . ? O3 C5 1.412(13) . ? O3 C4 1.429(10) . ? O4 C6 1.415(10) . ? O4 C7 1.416(10) . ? O5 C9 1.413(9) . ? O5 C8 1.436(9) . ? O6 C11 1.378(9) . ? O6 10 1.455(9) . ? Si1A C14A 1.726(11) . ? Si1A C15A 1.74(3) . ? Si1A C13 1.787(10) . ? Si1A C16A 1.80(3) . ? Si1A H14D 1.9880 . ? Si1B C16B 1.767(17) . ? Si1B C13 1.859(9) . ? Si1B C14B 1.876(19) . ? Si1B C15B 1.895(17) . ? Si1B H15A 1.4784 . ? Si1B H15B 1.5616 . ? Si1B H15C 1.4593 . ? Si2 C19 1.853(11) . ? Si2 C17 1.856(8) . ? Si2 C20 1.858(10) . ? Si2 C18 1.895(15) . ? Si3 C22 1.820(12) . ? Si3 C21 1.848(9) . ? Si3 C24 1.872(9) . ? Si3 C23 1.877(11) . ? C1 C2 1.540(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.444(15) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.406(16) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.479(12) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 10 1.444(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? 10 H10A 0.9900 . ? 10 H10B 0.9900 . ? C11 C12 1.354(12) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 H13C 0.9900 . ? C13 H13D 0.9900 . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C14A H14D 0.4613 . ? C14A H14E 1.3319 . ? C14A H14F 1.3102 . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C16A H16D 0.8030 . ? C16A H16E 1.0215 . ? C14B H14A 0.6404 . ? C14B H14B 1.0792 . ? C14B H14C 1.4766 . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C15B H15A 1.1399 . ? C15B H15B 1.2675 . ? C15B H15C 1.1148 . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? C16B H16A 1.3544 . ? C16B H16B 0.7385 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? 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 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.395(10) . ? C25 C30 1.419(10) . ? C26 C27 1.370(10) . ? C26 H26 0.9500 . ? C27 C28 1.398(10) . ? C27 H27 0.9500 . ? C28 C29 1.382(10) . ? C28 H28 0.9500 . ? C29 C30 1.370(10) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.393(11) . ? C31 C36 1.394(10) . ? C32 C33 1.393(10) . ? C32 H32 0.9500 . ? C33 C34 1.353(11) . ? C33 H33 0.9500 . ? C34 C35 1.394(12) . ? C34 H34 0.9500 . ? C35 C36 1.378(10) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.410(9) . ? C37 C38 1.421(11) . ? C38 C39 1.375(12) . ? C38 H38 0.9500 . ? C39 C40 1.329(15) . ? C39 H39 0.9500 . ? C40 C41 1.427(14) . ? C40 H40 0.9500 . ? C41 C42 1.425(10) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? Cl1 C43A 1.7787 . ? Cl1 C43B 1.797(18) . ? Cl2 C44 1.73(2) . ? C43A C44 1.477(19) . ? C43A H43A 0.9900 . ? C43A H43B 0.9900 . ? C43B C44 1.5172 . ? C43B H43C 0.9900 . ? C43B H43D 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C44 H44C 0.9900 . ? C44 H44D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C31 B C25 111.4(5) . . ? C31 B C21 113.3(7) . . ? C25 B C21 107.5(6) . . ? C31 B C37 104.7(6) . . ? C25 B C37 108.6(7) . . ? C21 B C37 111.3(6) . . ? C13 Lu C17 97.5(3) . . ? C13 Lu O5 84.7(2) . . ? C17 Lu O5 85.2(2) . . ? C13 Lu O2 83.2(3) . . ? C17 Lu O2 84.9(2) . . ? O5 Lu O2 163.19(17) . . ? C13 Lu O3 146.5(3) . . ? C17 Lu O3 89.4(2) . . ? O5 Lu O3 128.71(19) . . ? O2 Lu O3 64.71(19) . . ? C13 Lu O4 147.8(3) . . ? C17 Lu O4 90.6(2) . . ? O5 Lu O4 64.90(18) . . ? O2 Lu O4 128.7(2) . . ? O3 Lu O4 64.2(2) . . ? C13 Lu O6 84.5(3) . . ? C17 Lu O6 150.4(2) . . ? O5 Lu O6 65.45(16) . . ? O2 Lu O6 124.60(18) . . ? O3 Lu O6 105.29(19) . . ? O4 Lu O6 73.7(2) . . ? C13 Lu O1 85.1(2) . . ? C17 Lu O1 148.7(2) . . ? O5 Lu O1 126.02(17) . . ? O2 Lu O1 64.38(17) . . ? O3 Lu O1 72.90(18) . . ? O4 Lu O1 103.80(19) . . ? O6 Lu O1 60.88(17) . . ? C12 O1 C1 115.9(6) . . ? C12 O1 Lu 121.6(5) . . ? C1 O1 Lu 122.3(4) . . ? C3 O2 C2 116.0(7) . . ? C3 O2 Lu 113.1(5) . . ? C2 O2 Lu 117.6(4) . . ? C5 O3 C4 115.7(8) . . ? C5 O3 Lu 121.0(7) . . ? C4 O3 Lu 122.4(5) . . ? C6 O4 C7 115.8(7) . . ? C6 O4 Lu 121.0(6) . . ? C7 O4 Lu 122.8(4) . . ? C9 O5 C8 115.7(6) . . ? C9 O5 Lu 117.0(4) . . ? C8 O5 Lu 112.5(4) . . ? C11 O6 10 117.9(6) . . ? C11 O6 Lu 123.1(5) . . ? 10 O6 Lu 117.2(4) . . ? C14A Si1A C15A 90.2(12) . . ? C14A Si1A C13 123.1(7) . . ? C15A Si1A C13 85.6(12) . . ? C14A Si1A C16A 116.4(10) . . ? C15A Si1A C16A 102.2(15) . . ? C13 Si1A C16A 119.9(11) . . ? C14A Si1A H14D 11.8 . . ? C15A Si1A H14D 102.0 . . ? C13 Si1A H14D 122.7 . . ? C16A Si1A H14D 113.7 . . ? C16B Si1B C13 116.5(7) . . ? C16B Si1B C14B 108.9(8) . . ? C13 Si1B C14B 113.9(7) . . ? C16B Si1B C15B 100.4(8) . . ? C13 Si1B C15B 114.0(6) . . ? C14B Si1B C15B 101.3(9) . . ? C16B Si1B H15A 63.4 . . ? C13 Si1B H15A 128.8 . . ? C14B Si1B H15A 113.3 . . ? C15B Si1B H15A 37.0 . . ? C16B Si1B H15B 111.0 . . ? C13 Si1B H15B 130.4 . . ? C14B Si1B H15B 59.7 . . ? C15B Si1B H15B 41.6 . . ? H15A Si1B H15B 63.5 . . ? C16B Si1B H15C 123.6 . . ? C13 Si1B H15C 78.5 . . ? C14B Si1B H15C 112.7 . . ? C15B Si1B H15C 35.9 . . ? H15A Si1B H15C 66.0 . . ? H15B Si1B H15C 63.9 . . ? C19 Si2 C17 114.5(4) . . ? C19 Si2 C20 104.2(5) . . ? C17 Si2 C20 112.3(5) . . ? C19 Si2 C18 106.2(6) . . ? C17 Si2 C18 114.4(5) . . ? C20 Si2 C18 104.1(7) . . ? C22 Si3 C21 114.3(5) . . ? C22 Si3 C24 105.4(5) . . ? C21 Si3 C24 109.8(5) . . ? C22 Si3 C23 107.8(6) . . ? C21 Si3 C23 112.7(4) . . ? C24 Si3 C23 106.3(5) . . ? O1 C1 C2 106.8(6) . . ? O1 C1 H1A 110.4 . . ? C2 C1 H1A 110.4 . . ? O1 C1 H1B 110.4 . . ? C2 C1 H1B 110.4 . . ? H1A C1 H1B 108.6 . . ? O2 C2 C1 110.3(6) . . ? O2 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? O2 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? O2 C3 C4 112.1(7) . . ? O2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? O2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O3 C4 C3 106.3(7) . . ? O3 C4 H4A 110.5 . . ? C3 C4 H4A 110.5 . . ? O3 C4 H4B 110.5 . . ? C3 C4 H4B 110.5 . . ? H4A C4 H4B 108.7 . . ? C6 C5 O3 111.7(9) . . ? C6 C5 H5A 109.3 . . ? O3 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? O3 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? C5 C6 O4 115.9(8) . . ? C5 C6 H6A 108.3 . . ? O4 C6 H6A 108.3 . . ? C5 C6 H6B 108.3 . . ? O4 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? O4 C7 C8 106.3(6) . . ? O4 C7 H7A 110.5 . . ? C8 C7 H7A 110.5 . . ? O4 C7 H7B 110.5 . . ? C8 C7 H7B 110.5 . . ? H7A C7 H7B 108.7 . . ? O5 C8 C7 111.7(6) . . ? O5 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? O5 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? O5 C9 10 112.2(6) . . ? O5 C9 H9A 109.2 . . ? 10 C9 H9A 109.2 . . ? O5 C9 H9B 109.2 . . ? 10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 10 O6 107.5(6) . . ? C9 10 H10A 110.2 . . ? O6 10 H10A 110.2 . . ? C9 10 H10B 110.2 . . ? O6 10 H10B 110.2 . . ? H10A 10 H10B 108.5 . . ? C12 C11 O6 113.4(7) . . ? C12 C11 H11A 108.9 . . ? O6 C11 H11A 108.9 . . ? C12 C11 H11B 108.9 . . ? O6 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C11 C12 O1 117.2(8) . . ? C11 C12 H12A 108.0 . . ? O1 C12 H12A 108.0 . . ? C11 C12 H12B 108.0 . . ? O1 C12 H12B 108.0 . . ? H12A C12 H12B 107.3 . . ? Si1A C13 Si1B 28.2(2) . . ? Si1A C13 Lu 141.9(5) . . ? Si1B C13 Lu 127.6(5) . . ? Si1A C13 H13A 101.5 . . ? Si1B C13 H13A 84.1 . . ? Lu C13 H13A 101.5 . . ? Si1A C13 H13B 101.5 . . ? Si1B C13 H13B 127.8 . . ? Lu C13 H13B 101.5 . . ? H13A C13 H13B 104.6 . . ? Si1A C13 H13C 110.2 . . ? Si1B C13 H13C 105.4 . . ? Lu C13 H13C 105.4 . . ? H13A C13 H13C 32.0 . . ? H13B C13 H13C 72.7 . . ? Si1A C13 H13D 77.5 . . ? Si1B C13 H13D 105.4 . . ? Lu C13 H13D 105.4 . . ? H13A C13 H13D 135.8 . . ? H13B C13 H13D 36.0 . . ? H13C C13 H13D 106.0 . . ? Si1A C14A H14A 109.1 . . ? Si1A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? Si1A C14A H14C 109.7 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? Si1A C14A H14D 118.6 . . ? H14A C14A H14D 119.6 . . ? H14B C14A H14D 87.9 . . ? H14C C14A H14D 21.6 . . ? Si1A C14A H14E 108.8 . . ? H14A C14A H14E 3.1 . . ? H14B C14A H14E 112.3 . . ? H14C C14A H14E 107.0 . . ? H14D C14A H14E 117.9 . . ? Si1A C14A H14F 107.4 . . ? H14A C14A H14F 71.5 . . ? H14B C14A H14F 41.6 . . ? H14C C14A H14F 139.7 . . ? H14D C14A H14F 121.5 . . ? H14E C14A H14F 74.6 . . ? Si1A C15A H15A 108.4 . . ? Si1A C15A H15B 109.9 . . ? H15A C15A H15B 109.5 . . ? Si1A C15A H15C 110.1 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? Si1A C16A H16A 109.4 . . ? Si1A C16A H16B 109.0 . . ? H16A C16A H16B 109.5 . . ? Si1A C16A H16C 110.0 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? Si1A C16A H16D 102.7 . . ? H16A C16A H16D 137.6 . . ? H16B C16A H16D 31.6 . . ? H16C C16A H16D 83.7 . . ? Si1A C16A H16E 93.0 . . ? H16A C16A H16E 31.9 . . ? H16B C16A H16E 90.6 . . ? H16C C16A H16E 141.3 . . ? H16D C16A H16E 122.1 . . ? Si1B C14B H14A 113.0 . . ? Si1B C14B H14B 111.5 . . ? H14A C14B H14B 135.5 . . ? Si1B C14B H14C 111.5 . . ? H14A C14B H14C 89.1 . . ? H14B C14B H14C 75.8 . . ? Si1B C14B H14D 111.7 . . ? H14A C14B H14D 101.4 . . ? H14B C14B H14D 62.3 . . ? H14C C14B H14D 14.0 . . ? Si1B C14B H14E 108.6 . . ? H14A C14B H14E 8.0 . . ? H14B C14B H14E 139.1 . . ? H14C C14B H14E 97.0 . . ? H14D C14B H14E 109.5 . . ? Si1B C14B H14F 108.2 . . ? H14A C14B H14F 113.0 . . ? H14B C14B H14F 49.7 . . ? H14C C14B H14F 121.1 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? Si1B C15B H15A 51.2 . . ? Si1B C15B H15B 54.9 . . ? H15A C15B H15B 83.1 . . ? Si1B C15B H15C 50.2 . . ? H15A C15B H15C 90.4 . . ? H15B C15B H15C 84.1 . . ? Si1B C15B H15D 109.5 . . ? H15A C15B H15D 92.9 . . ? H15B C15B H15D 63.7 . . ? H15C C15B H15D 146.9 . . ? Si1B C15B H15E 109.4 . . ? H15A C15B H15E 155.4 . . ? H15B C15B H15E 97.4 . . ? H15C C15B H15E 65.3 . . ? H15D C15B H15E 109.5 . . ? Si1B C15B H15F 109.5 . . ? H15A C15B H15F 70.6 . . ? H15B C15B H15F 152.7 . . ? H15C C15B H15F 102.7 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? Si1B C16B H16A 116.1 . . ? Si1B C16B H16B 131.7 . . ? H16A C16B H16B 95.2 . . ? Si1B C16B H16D 109.6 . . ? H16A C16B H16D 89.4 . . ? H16B C16B H16D 30.9 . . ? Si1B C16B H16E 109.4 . . ? H16A C16B H16E 20.2 . . ? H16B C16B H16E 111.1 . . ? H16D C16B H16E 109.5 . . ? Si1B C16B H16F 109.4 . . ? H16A C16B H16F 120.6 . . ? H16B C16B H16F 80.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? Si2 C17 Lu 138.0(4) . . ? Si2 C17 H17A 102.6 . . ? Lu C17 H17A 102.6 . . ? Si2 C17 H17B 102.6 . . ? Lu C17 H17B 102.6 . . ? H17A C17 H17B 105.0 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si2 C20 H20A 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? B C21 Si3 126.2(5) . . ? B C21 H21A 105.8 . . ? Si3 C21 H21A 105.8 . . ? B C21 H21B 105.8 . . ? Si3 C21 H21B 105.8 . . ? H21A C21 H21B 106.2 . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si3 C24 H24A 109.5 . . ? Si3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 113.7(6) . . ? C26 C25 B 125.2(6) . . ? C30 C25 B 121.0(6) . . ? C27 C26 C25 124.8(7) . . ? C27 C26 H26 117.6 . . ? C25 C26 H26 117.6 . . ? C26 C27 C28 119.9(7) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C29 C28 C27 117.1(7) . . ? C29 C28 H28 121.4 . . ? C27 C28 H28 121.4 . . ? C30 C29 C28 122.4(7) . . ? C30 C29 H29 118.8 . . ? C28 C29 H29 118.8 . . ? C29 C30 C25 122.1(7) . . ? C29 C30 H30 119.0 . . ? C25 C30 H30 119.0 . . ? C32 C31 C36 113.7(6) . . ? C32 C31 B 123.6(7) . . ? C36 C31 B 122.7(7) . . ? C31 C32 C33 122.7(7) . . ? C31 C32 H32 118.7 . . ? C33 C32 H32 118.7 . . ? C34 C33 C32 121.8(8) . . ? C34 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? C33 C34 C35 117.5(7) . . ? C33 C34 H34 121.2 . . ? C35 C34 H34 121.2 . . ? C36 C35 C34 120.0(7) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C31 124.2(7) . . ? C35 C36 H36 117.9 . . ? C31 C36 H36 117.9 . . ? C42 C37 C38 114.6(7) . . ? C42 C37 B 121.8(6) . . ? C38 C37 B 123.6(8) . . ? C39 C38 C37 123.6(10) . . ? C39 C38 H38 118.2 . . ? C37 C38 H38 118.2 . . ? C40 C39 C38 120.8(9) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C39 C40 C41 120.9(9) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C42 C41 C40 117.5(9) . . ? C42 C41 H41 121.2 . . ? C40 C41 H41 121.2 . . ? C37 C42 C41 122.5(6) . . ? C37 C42 H42 118.8 . . ? C41 C42 H42 118.8 . . ? C43A Cl1 C43B 46.7(9) . . ? C44 C43A Cl1 111.2(11) . . ? C44 C43A H43A 109.4 . . ? Cl1 C43A H43A 109.4 . . ? C44 C43A H43B 109.4 . . ? Cl1 C43A H43B 109.4 . . ? H43A C43A H43B 108.0 . . ? C44 C43B Cl1 108.4(8) . . ? C44 C43B H43C 110.0 . . ? Cl1 C43B H43C 110.0 . . ? C44 C43B H43D 110.0 . . ? Cl1 C43B H43D 110.0 . . ? H43C C43B H43D 108.4 . . ? C43A C44 C43B 56.5(10) . . ? C43A C44 Cl2 124.0(17) . . ? C43B C44 Cl2 165.8(10) . . ? C43A C44 H44A 106.3 . . ? C43B C44 H44A 62.5 . . ? Cl2 C44 H44A 106.3 . . ? C43A C44 H44B 106.3 . . ? C43B C44 H44B 85.9 . . ? Cl2 C44 H44B 106.3 . . ? H44A C44 H44B 106.4 . . ? C43A C44 H44C 129.0 . . ? C43B C44 H44C 94.4 . . ? Cl2 C44 H44C 94.4 . . ? H44A C44 H44C 90.9 . . ? H44B C44 H44C 23.8 . . ? C43A C44 H44D 48.1 . . ? C43B C44 H44D 94.4 . . ? Cl2 C44 H44D 94.4 . . ? H44A C44 H44D 154.1 . . ? H44B C44 H44D 81.7 . . ? H44C C44 H44D 103.1 . . ? 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 C13 Lu O1 C12 -92.7(8) . . . . ? C17 Lu O1 C12 170.9(8) . . . . ? O5 Lu O1 C12 -13.0(9) . . . . ? O2 Lu O1 C12 -177.5(9) . . . . ? O3 Lu O1 C12 112.9(8) . . . . ? O4 Lu O1 C12 55.9(8) . . . . ? O6 Lu O1 C12 -6.3(8) . . . . ? C13 Lu O1 C1 81.9(7) . . . . ? C17 Lu O1 C1 -14.5(8) . . . . ? O5 Lu O1 C1 161.6(6) . . . . ? O2 Lu O1 C1 -2.9(6) . . . . ? O3 Lu O1 C1 -72.6(6) . . . . ? O4 Lu O1 C1 -129.6(6) . . . . ? O6 Lu O1 C1 168.3(7) . . . . ? C13 Lu O2 C3 160.8(6) . . . . ? C17 Lu O2 C3 62.6(6) . . . . ? O5 Lu O2 C3 116.7(8) . . . . ? O3 Lu O2 C3 -29.1(5) . . . . ? O4 Lu O2 C3 -24.0(6) . . . . ? O6 Lu O2 C3 -120.7(6) . . . . ? O1 Lu O2 C3 -111.4(6) . . . . ? C13 Lu O2 C2 -59.7(6) . . . . ? C17 Lu O2 C2 -157.9(6) . . . . ? O5 Lu O2 C2 -103.8(7) . . . . ? O3 Lu O2 C2 110.4(6) . . . . ? O4 Lu O2 C2 115.5(6) . . . . ? O6 Lu O2 C2 18.8(6) . . . . ? O1 Lu O2 C2 28.1(5) . . . . ? C13 Lu O3 C5 -145.4(9) . . . . ? C17 Lu O3 C5 111.9(9) . . . . ? O5 Lu O3 C5 28.6(9) . . . . ? O2 Lu O3 C5 -163.4(9) . . . . ? O4 Lu O3 C5 21.0(8) . . . . ? O6 Lu O3 C5 -42.0(9) . . . . ? O1 Lu O3 C5 -94.2(9) . . . . ? C13 Lu O3 C4 22.8(8) . . . . ? C17 Lu O3 C4 -79.9(6) . . . . ? O5 Lu O3 C4 -163.2(6) . . . . ? O2 Lu O3 C4 4.7(6) . . . . ? O4 Lu O3 C4 -170.8(6) . . . . ? O6 Lu O3 C4 126.2(6) . . . . ? O1 Lu O3 C4 73.9(6) . . . . ? C13 Lu O4 C6 156.8(7) . . . . ? C17 Lu O4 C6 -98.1(7) . . . . ? O5 Lu O4 C6 177.4(7) . . . . ? O2 Lu O4 C6 -14.2(8) . . . . ? O3 Lu O4 C6 -9.1(6) . . . . ? O6 Lu O4 C6 107.4(7) . . . . ? O1 Lu O4 C6 53.8(7) . . . . ? C13 Lu O4 C7 -31.2(9) . . . . ? C17 Lu O4 C7 73.9(6) . . . . ? O5 Lu O4 C7 -10.5(6) . . . . ? O2 Lu O4 C7 157.8(5) . . . . ? O3 Lu O4 C7 162.9(7) . . . . ? O6 Lu O4 C7 -80.6(6) . . . . ? O1 Lu O4 C7 -134.1(6) . . . . ? C13 Lu O5 C9 64.4(6) . . . . ? C17 Lu O5 C9 162.4(5) . . . . ? O2 Lu O5 C9 108.4(7) . . . . ? O3 Lu O5 C9 -112.2(5) . . . . ? O4 Lu O5 C9 -104.7(5) . . . . ? O6 Lu O5 C9 -21.9(5) . . . . ? O1 Lu O5 C9 -15.5(6) . . . . ? C13 Lu O5 C8 -158.1(5) . . . . ? C17 Lu O5 C8 -60.1(5) . . . . ? O2 Lu O5 C8 -114.2(7) . . . . ? O3 Lu O5 C8 25.2(5) . . . . ? O4 Lu O5 C8 32.8(4) . . . . ? O6 Lu O5 C8 115.6(5) . . . . ? O1 Lu O5 C8 121.9(4) . . . . ? C13 Lu O6 C11 103.5(7) . . . . ? C17 Lu O6 C11 -161.1(6) . . . . ? O5 Lu O6 C11 -169.9(7) . . . . ? O2 Lu O6 C11 25.7(7) . . . . ? O3 Lu O6 C11 -43.9(7) . . . . ? O4 Lu O6 C11 -100.5(7) . . . . ? O1 Lu O6 C11 16.0(6) . . . . ? C13 Lu O6 10 -92.2(6) . . . . ? C17 Lu O6 10 3.3(8) . . . . ? O5 Lu O6 10 -5.5(5) . . . . ? O2 Lu O6 10 -170.0(5) . . . . ? O3 Lu O6 10 120.5(5) . . . . ? O4 Lu O6 10 63.8(5) . . . . ? O1 Lu O6 10 -179.6(6) . . . . ? C12 O1 C1 C2 155.6(9) . . . . ? Lu O1 C1 C2 -19.2(9) . . . . ? C3 O2 C2 C1 88.7(9) . . . . ? Lu O2 C2 C1 -49.6(9) . . . . ? O1 C1 C2 O2 41.7(10) . . . . ? C2 O2 C3 C4 -87.2(9) . . . . ? Lu O2 C3 C4 53.0(8) . . . . ? C5 O3 C4 C3 -172.2(10) . . . . ? Lu O3 C4 C3 19.0(10) . . . . ? O2 C3 C4 O3 -45.3(10) . . . . ? C4 O3 C5 C6 161.1(10) . . . . ? Lu O3 C5 C6 -30.0(16) . . . . ? O3 C5 C6 O4 20.0(18) . . . . ? C7 O4 C6 C5 -175.1(11) . . . . ? Lu O4 C6 C5 -2.5(14) . . . . ? C6 O4 C7 C8 160.0(8) . . . . ? Lu O4 C7 C8 -12.4(9) . . . . ? C9 O5 C8 C7 83.7(8) . . . . ? Lu O5 C8 C7 -54.4(7) . . . . ? O4 C7 C8 O5 42.0(9) . . . . ? C8 O5 C9 10 -87.8(9) . . . . ? Lu O5 C9 10 48.3(9) . . . . ? O5 C9 10 O6 -49.2(10) . . . . ? C11 O6 10 C9 -164.9(8) . . . . ? Lu O6 10 C9 29.9(8) . . . . ? 10 O6 C11 C12 171.8(9) . . . . ? Lu O6 C11 C12 -23.9(12) . . . . ? O6 C11 C12 O1 16.4(16) . . . . ? C1 O1 C12 C11 -177.8(10) . . . . ? Lu O1 C12 C11 -2.9(15) . . . . ? C14A Si1A C13 Si1B 91.3(9) . . . . ? C15A Si1A C13 Si1B 3.9(12) . . . . ? C16A Si1A C13 Si1B -97.6(13) . . . . ? C14A Si1A C13 Lu 164.6(3) . . . . ? C15A Si1A C13 Lu 77.2(15) . . . . ? C16A Si1A C13 Lu -24.4(16) . . . . ? C16B Si1B C13 Si1A 66.5(9) . . . . ? C14B Si1B C13 Si1A -61.6(10) . . . . ? C15B Si1B C13 Si1A -177.3(9) . . . . ? C16B Si1B C13 Lu -65.3(9) . . . . ? C14B Si1B C13 Lu 166.6(8) . . . . ? C15B Si1B C13 Lu 51.0(8) . . . . ? C17 Lu C13 Si1A -58.2(9) . . . . ? O5 Lu C13 Si1A 26.2(9) . . . . ? O2 Lu C13 Si1A -142.1(9) . . . . ? O3 Lu C13 Si1A -158.5(7) . . . . ? O4 Lu C13 Si1A 44.9(12) . . . . ? O6 Lu C13 Si1A 92.0(9) . . . . ? O1 Lu C13 Si1A 153.1(9) . . . . ? C17 Lu C13 Si1B -23.5(6) . . . . ? O5 Lu C13 Si1B 61.0(6) . . . . ? O2 Lu C13 Si1B -107.4(6) . . . . ? O3 Lu C13 Si1B -123.7(5) . . . . ? O4 Lu C13 Si1B 79.7(8) . . . . ? O6 Lu C13 Si1B 126.8(6) . . . . ? O1 Lu C13 Si1B -172.1(6) . . . . ? C19 Si2 C17 Lu -71.7(8) . . . . ? C20 Si2 C17 Lu 169.7(6) . . . . ? C18 Si2 C17 Lu 51.3(9) . . . . ? C13 Lu C17 Si2 -179.7(6) . . . . ? O5 Lu C17 Si2 96.4(6) . . . . ? O2 Lu C17 Si2 -97.2(6) . . . . ? O3 Lu C17 Si2 -32.6(6) . . . . ? O4 Lu C17 Si2 31.6(6) . . . . ? O6 Lu C17 Si2 88.3(8) . . . . ? O1 Lu C17 Si2 -86.8(7) . . . . ? C31 B C21 Si3 73.3(8) . . . . ? C25 B C21 Si3 -50.3(8) . . . . ? C37 B C21 Si3 -169.1(6) . . . . ? C22 Si3 C21 B 63.1(8) . . . . ? C24 Si3 C21 B -178.6(7) . . . . ? C23 Si3 C21 B -60.4(8) . . . . ? C31 B C25 C26 -23.7(10) . . . . ? C21 B C25 C26 101.1(8) . . . . ? C37 B C25 C26 -138.5(7) . . . . ? C31 B C25 C30 160.4(6) . . . . ? C21 B C25 C30 -74.8(8) . . . . ? C37 B C25 C30 45.6(8) . . . . ? C30 C25 C26 C27 2.5(11) . . . . ? B C25 C26 C27 -173.6(7) . . . . ? C25 C26 C27 C28 -1.0(12) . . . . ? C26 C27 C28 C29 -0.9(12) . . . . ? C27 C28 C29 C30 1.0(13) . . . . ? C28 C29 C30 C25 0.6(13) . . . . ? C26 C25 C30 C29 -2.3(11) . . . . ? B C25 C30 C29 174.0(7) . . . . ? C25 B C31 C32 133.4(7) . . . . ? C21 B C31 C32 12.0(10) . . . . ? C37 B C31 C32 -109.4(8) . . . . ? C25 B C31 C36 -48.6(9) . . . . ? C21 B C31 C36 -169.9(7) . . . . ? C37 B C31 C36 68.6(9) . . . . ? C36 C31 C32 C33 -0.9(10) . . . . ? B C31 C32 C33 177.3(7) . . . . ? C31 C32 C33 C34 1.4(11) . . . . ? C32 C33 C34 C35 0.3(10) . . . . ? C33 C34 C35 C36 -2.4(10) . . . . ? C34 C35 C36 C31 3.0(11) . . . . ? C32 C31 C36 C35 -1.3(10) . . . . ? B C31 C36 C35 -179.5(7) . . . . ? C31 B C37 C42 -83.3(8) . . . . ? C25 B C37 C42 35.9(8) . . . . ? C21 B C37 C42 154.0(6) . . . . ? C31 B C37 C38 95.3(7) . . . . ? C25 B C37 C38 -145.5(6) . . . . ? C21 B C37 C38 -27.4(9) . . . . ? C42 C37 C38 C39 0.5(10) . . . . ? B C37 C38 C39 -178.2(7) . . . . ? C37 C38 C39 C40 0.1(13) . . . . ? C38 C39 C40 C41 1.1(14) . . . . ? C39 C40 C41 C42 -2.8(13) . . . . ? C38 C37 C42 C41 -2.3(9) . . . . ? B C37 C42 C41 176.4(6) . . . . ? C40 C41 C42 C37 3.5(10) . . . . ? C43B Cl1 C43A C44 -46.6(8) . . . . ? C43A Cl1 C43B C44 44.0(6) . . . . ? Cl1 C43A C44 C43B 48.7(6) . . . . ? Cl1 C43A C44 Cl2 -148.4(16) . . . . ? Cl1 C43B C44 C43A -46.9(7) . . . . ? Cl1 C43B C44 Cl2 -144(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.892 _refine_diff_density_min -1.002 _refine_diff_density_rms 0.134