Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 loop_ _publ_author_name _publ_author_address M.Konkol ; Institut fur Anorganische Chemie RWTH Aachen Landoltweg 1 D-52074 Aachen Germany ; T.P.Spaniol ; Institut fur Anorganische Chemie RWTH Aachen Landoltweg 1 D-52074 Aachen Germany ; M.Kondracka ; Institut fur Anorganische Chemie RWTH Aachen Landoltweg 1 D-52074 Aachen Germany ; J.Okuda ; Institut fur Anorganische Chemie RWTH Aachen Landoltweg 1 D-52074 Aachen Germany ; _publ_contact_author_name 'Jun Okuda' _publ_contact_author_address ; Institut fur Anorganische Chemie RWTH Aachen Landoltweg 1 Aachen D-52074 Germany ; _publ_contact_author_phone '049 241 89 4645' _publ_contact_author_fax '049 241 80 92644' _publ_contact_author_email jun.okuda@ac.rwth-aachen.de _publ_requested_coeditor_name ? _publ_contact_letter ; These five crystal structures are a part of a manuscript that is sent for publication in the Journal 'Chemical Communications'. The individual structures mk1, mk2, mk5, mk6 and mk7 are separated from each other by the sequence #===END at the beginning of a line. ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Lutetium alkyl and hydride complexes in a non-cyclopentadienyl coordination environment ; #============================================================================== data_mk1 _database_code_depnum_ccdc_archive 'CCDC 643864' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(tetrahydrofurane)-thiobis(6-tert-butyl-4-methylphenolato)- trimethylsilylmethyl-lutetium(III) ; _chemical_name_common ; Bis(tetrahydrofurane)-thiobis(6-tert-butyl-4-methylphenolato)- trimethylsilylmethyl-lutetium(iii) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H55 Lu O4 S Si' _chemical_formula_weight 762.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' 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' '-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 17.657(3) _cell_length_b 18.687(3) _cell_length_c 22.178(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7318(2) _cell_formula_units_Z 8 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 884 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 21.56 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 2.820 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5391 _exptl_absorpt_correction_T_max 0.7657 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81995 _diffrn_reflns_av_R_equivalents 0.1015 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.42 _reflns_number_total 9170 _reflns_number_gt 7868 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9170 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0848 _refine_ls_wR_factor_ref 0.1552 _refine_ls_wR_factor_gt 0.1504 _refine_ls_goodness_of_fit_ref 1.570 _refine_ls_restrained_S_all 1.570 _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 Lu Lu 0.641815(15) 0.099635(15) 0.675103(12) 0.01662(9) Uani 1 1 d . . . Si Si 0.60045(14) 0.22334(12) 0.54447(10) 0.0328(5) Uani 1 1 d . . . S S 0.73078(9) -0.00469(9) 0.74590(8) 0.0166(3) Uani 1 1 d . . . O1 O 0.7145(3) 0.1527(2) 0.7351(2) 0.0188(10) Uani 1 1 d . . . O2 O 0.7259(2) 0.0543(2) 0.6202(2) 0.0171(10) Uani 1 1 d . . . O3 O 0.5694(3) -0.0003(3) 0.6499(2) 0.0257(11) Uani 1 1 d . . . O4 O 0.5525(3) 0.1032(3) 0.7526(2) 0.0253(11) Uani 1 1 d . . . C1 C 0.7585(4) 0.1339(4) 0.7807(3) 0.0165(14) Uani 1 1 d . . . C2 C 0.7745(3) 0.0619(3) 0.7926(3) 0.0142(13) Uani 1 1 d . . . C3 C 0.8187(4) 0.0400(4) 0.8410(3) 0.0177(14) Uani 1 1 d . . . H3 H 0.8280 -0.0094 0.8476 0.021 Uiso 1 1 calc R . . C4 C 0.8491(4) 0.0908(4) 0.8796(3) 0.0244(16) Uani 1 1 d . . . C5 C 0.8340(4) 0.1624(4) 0.8680(3) 0.0193(14) Uani 1 1 d . . . H5 H 0.8550 0.1972 0.8944 0.023 Uiso 1 1 calc R . . C6 C 0.7899(4) 0.1863(4) 0.8199(3) 0.0197(14) Uani 1 1 d . . . C7 C 0.8988(4) 0.0693(5) 0.9321(4) 0.0307(18) Uani 1 1 d . . . H7A H 0.8968 0.0172 0.9373 0.046 Uiso 1 1 calc R . . H7B H 0.8807 0.0927 0.9689 0.046 Uiso 1 1 calc R . . H7C H 0.9511 0.0840 0.9241 0.046 Uiso 1 1 calc R . . C8 C 0.7739(4) 0.2658(4) 0.8101(3) 0.0208(15) Uani 1 1 d . . . C9 C 0.8028(4) 0.2888(4) 0.7482(4) 0.0287(17) Uani 1 1 d . . . H9A H 0.8577 0.2818 0.7463 0.043 Uiso 1 1 calc R . . H9B H 0.7910 0.3395 0.7417 0.043 Uiso 1 1 calc R . . H9C H 0.7783 0.2599 0.7170 0.043 Uiso 1 1 calc R . . C10 C 0.6877(5) 0.2800(4) 0.8145(4) 0.0329(19) Uani 1 1 d . . . H10A H 0.6782 0.3316 0.8116 0.049 Uiso 1 1 calc R . . H10B H 0.6687 0.2622 0.8532 0.049 Uiso 1 1 calc R . . H10C H 0.6616 0.2553 0.7815 0.049 Uiso 1 1 calc R . . C11 C 0.8111(5) 0.3131(4) 0.8582(4) 0.038(2) Uani 1 1 d . . . H11A H 0.8663 0.3088 0.8553 0.057 Uiso 1 1 calc R . . H11B H 0.7944 0.2977 0.8983 0.057 Uiso 1 1 calc R . . H11C H 0.7963 0.3631 0.8517 0.057 Uiso 1 1 calc R . . C12 C 0.7988(4) -0.0185(4) 0.6869(3) 0.0177(14) Uani 1 1 d . . . C13 C 0.7872(4) 0.0148(4) 0.6312(3) 0.0192(14) Uani 1 1 d . . . C14 C 0.8436(3) 0.0049(4) 0.5859(3) 0.0189(14) Uani 1 1 d . . . C15 C 0.9054(4) -0.0378(4) 0.5998(3) 0.0217(15) Uani 1 1 d . . . H15 H 0.9428 -0.0444 0.5695 0.026 Uiso 1 1 calc R . . C16 C 0.9165(4) -0.0720(4) 0.6554(3) 0.0213(15) Uani 1 1 d . . . C17 C 0.8615(4) -0.0616(4) 0.6988(3) 0.0218(14) Uani 1 1 d . . . H17 H 0.8664 -0.0840 0.7370 0.026 Uiso 1 1 calc R . . C18 C 0.9848(4) -0.1193(4) 0.6658(3) 0.0266(17) Uani 1 1 d . . . H18A H 1.0308 -0.0901 0.6656 0.040 Uiso 1 1 calc R . . H18B H 0.9878 -0.1553 0.6337 0.040 Uiso 1 1 calc R . . H18C H 0.9799 -0.1434 0.7049 0.040 Uiso 1 1 calc R . . C19 C 0.8352(4) 0.0393(4) 0.5239(3) 0.0251(16) Uani 1 1 d . . . C20 C 0.8279(4) 0.1206(4) 0.5306(4) 0.0298(18) Uani 1 1 d . . . H20A H 0.7855 0.1317 0.5575 0.045 Uiso 1 1 calc R . . H20B H 0.8188 0.1421 0.4909 0.045 Uiso 1 1 calc R . . H20C H 0.8748 0.1400 0.5476 0.045 Uiso 1 1 calc R . . C21 C 0.7652(4) 0.0083(5) 0.4915(3) 0.0321(19) Uani 1 1 d . . . H21A H 0.7731 -0.0429 0.4840 0.048 Uiso 1 1 calc R . . H21B H 0.7578 0.0332 0.4531 0.048 Uiso 1 1 calc R . . H21C H 0.7204 0.0148 0.5169 0.048 Uiso 1 1 calc R . . C22 C 0.9031(4) 0.0256(5) 0.4819(4) 0.039(2) Uani 1 1 d . . . H22A H 0.9492 0.0451 0.5002 0.058 Uiso 1 1 calc R . . H22B H 0.8942 0.0490 0.4430 0.058 Uiso 1 1 calc R . . H22C H 0.9092 -0.0260 0.4757 0.058 Uiso 1 1 calc R . . C23 C 0.5828(4) 0.1921(4) 0.6210(3) 0.0257(16) Uani 1 1 d . . . H23A H 0.5282 0.1802 0.6218 0.031 Uiso 1 1 calc R . . H23B H 0.5887 0.2351 0.6466 0.031 Uiso 1 1 calc R . . C24 C 0.6093(5) 0.1452(4) 0.4916(4) 0.040(2) Uani 1 1 d . . . H24A H 0.6512 0.1146 0.5045 0.060 Uiso 1 1 calc R . . H24B H 0.6191 0.1627 0.4507 0.060 Uiso 1 1 calc R . . H24C H 0.5621 0.1176 0.4919 0.060 Uiso 1 1 calc R . . C25 C 0.6881(7) 0.2788(5) 0.5408(6) 0.070(4) Uani 1 1 d . . . H25A H 0.6808 0.3227 0.5643 0.105 Uiso 1 1 calc R . . H25B H 0.6988 0.2912 0.4988 0.105 Uiso 1 1 calc R . . H25C H 0.7307 0.2516 0.5575 0.105 Uiso 1 1 calc R . . C26 C 0.5204(7) 0.2775(6) 0.5120(4) 0.064(3) Uani 1 1 d . . . H26A H 0.4734 0.2495 0.5137 0.095 Uiso 1 1 calc R . . H26B H 0.5317 0.2895 0.4699 0.095 Uiso 1 1 calc R . . H26C H 0.5142 0.3216 0.5353 0.095 Uiso 1 1 calc R . . C27 C 0.5836(5) -0.0412(5) 0.5949(4) 0.036(2) Uani 1 1 d . . . H27A H 0.6354 -0.0320 0.5796 0.043 Uiso 1 1 calc R . . H27B H 0.5467 -0.0283 0.5631 0.043 Uiso 1 1 calc R . . C28 C 0.5749(6) -0.1180(5) 0.6127(4) 0.045(2) Uani 1 1 d . . . H28A H 0.6220 -0.1370 0.6308 0.054 Uiso 1 1 calc R . . H28B H 0.5603 -0.1481 0.5779 0.054 Uiso 1 1 calc R . . C29 C 0.5120(7) -0.1139(5) 0.6585(5) 0.055(3) Uani 1 1 d . . . H29A H 0.4619 -0.1124 0.6385 0.066 Uiso 1 1 calc R . . H29B H 0.5136 -0.1553 0.6862 0.066 Uiso 1 1 calc R . . C30 C 0.5276(5) -0.0451(5) 0.6917(4) 0.038(2) Uani 1 1 d . . . H30A H 0.4795 -0.0217 0.7036 0.045 Uiso 1 1 calc R . . H30B H 0.5579 -0.0544 0.7284 0.045 Uiso 1 1 calc R . . C31 C 0.4784(4) 0.1370(5) 0.7472(4) 0.0298(18) Uani 1 1 d . . . H31A H 0.4471 0.1121 0.7166 0.036 Uiso 1 1 calc R . . H31B H 0.4836 0.1878 0.7353 0.036 Uiso 1 1 calc R . . C32 C 0.4432(5) 0.1308(5) 0.8085(4) 0.035(2) Uani 1 1 d . . . H32A H 0.4144 0.0856 0.8125 0.042 Uiso 1 1 calc R . . H32B H 0.4089 0.1716 0.8167 0.042 Uiso 1 1 calc R . . C33 C 0.5116(4) 0.1318(5) 0.8511(4) 0.0312(18) Uani 1 1 d . . . H33A H 0.5314 0.1808 0.8572 0.037 Uiso 1 1 calc R . . H33B H 0.4998 0.1097 0.8906 0.037 Uiso 1 1 calc R . . C34 C 0.5651(5) 0.0861(5) 0.8142(4) 0.043(2) Uani 1 1 d . . . H34A H 0.6182 0.0964 0.8254 0.052 Uiso 1 1 calc R . . H34B H 0.5550 0.0347 0.8214 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu 0.01370(14) 0.02204(15) 0.01414(15) -0.00188(12) -0.00147(11) 0.00152(11) Si 0.0459(14) 0.0294(12) 0.0231(12) 0.0051(9) 0.0029(10) 0.0137(10) S 0.0158(7) 0.0167(8) 0.0174(8) -0.0008(7) 0.0021(6) -0.0027(6) O1 0.017(2) 0.020(2) 0.019(3) 0.0018(19) -0.0041(19) 0.0018(19) O2 0.011(2) 0.023(2) 0.017(2) 0.0008(19) -0.0013(18) 0.0049(18) O3 0.022(3) 0.037(3) 0.019(3) -0.008(2) 0.007(2) -0.011(2) O4 0.017(2) 0.040(3) 0.019(3) -0.006(2) 0.0000(19) 0.005(2) C1 0.014(3) 0.024(4) 0.011(3) -0.003(3) -0.007(2) 0.004(3) C2 0.011(3) 0.018(3) 0.014(3) 0.001(3) -0.004(2) 0.000(2) C3 0.017(3) 0.024(4) 0.012(3) 0.005(3) 0.004(2) -0.001(3) C4 0.016(3) 0.038(4) 0.019(4) 0.015(3) -0.001(3) -0.011(3) C5 0.019(3) 0.028(4) 0.010(3) -0.004(3) -0.002(3) -0.007(3) C6 0.016(3) 0.024(3) 0.019(4) 0.002(3) -0.002(3) -0.001(3) C7 0.024(4) 0.041(5) 0.026(4) 0.007(4) -0.010(3) 0.002(3) C8 0.022(4) 0.020(3) 0.021(4) -0.002(3) -0.002(3) 0.001(3) C9 0.029(4) 0.022(4) 0.035(5) 0.006(3) -0.001(3) 0.006(3) C10 0.032(4) 0.029(4) 0.038(5) -0.007(4) -0.003(4) 0.005(3) C11 0.048(5) 0.024(4) 0.041(5) -0.011(4) -0.016(4) -0.004(4) C12 0.015(3) 0.020(3) 0.018(4) 0.000(3) 0.000(3) -0.005(3) C13 0.012(3) 0.021(3) 0.024(4) 0.000(3) 0.000(3) -0.003(3) C14 0.012(3) 0.028(4) 0.017(3) -0.001(3) 0.001(2) -0.003(3) C15 0.015(3) 0.029(4) 0.021(4) 0.001(3) 0.009(3) -0.002(3) C16 0.018(3) 0.020(3) 0.026(4) -0.001(3) -0.003(3) -0.001(3) C17 0.025(4) 0.017(3) 0.024(4) 0.007(3) -0.004(3) -0.001(3) C18 0.025(4) 0.026(4) 0.029(5) -0.001(3) -0.001(3) 0.009(3) C19 0.014(3) 0.045(5) 0.016(4) 0.004(3) -0.003(3) 0.006(3) C20 0.019(3) 0.045(5) 0.025(4) 0.015(4) -0.002(3) 0.000(3) C21 0.023(4) 0.056(5) 0.017(4) -0.003(4) -0.005(3) 0.009(4) C22 0.027(4) 0.069(6) 0.020(4) 0.010(4) 0.006(3) 0.015(4) C23 0.030(4) 0.032(4) 0.015(4) -0.002(3) -0.003(3) 0.006(3) C24 0.050(5) 0.039(5) 0.031(5) -0.001(4) 0.001(4) 0.015(4) C25 0.078(8) 0.043(6) 0.089(10) -0.001(6) 0.027(7) -0.008(6) C26 0.103(9) 0.066(7) 0.022(5) 0.005(5) -0.007(5) 0.053(6) C27 0.035(5) 0.046(5) 0.027(5) -0.015(4) 0.009(4) -0.008(4) C28 0.053(6) 0.044(5) 0.039(5) -0.020(4) -0.010(5) 0.010(4) C29 0.077(8) 0.047(6) 0.042(6) -0.003(4) 0.008(5) -0.031(5) C30 0.042(5) 0.047(5) 0.025(4) -0.008(4) 0.013(4) -0.028(4) C31 0.017(4) 0.046(5) 0.026(4) -0.009(4) -0.003(3) 0.010(3) C32 0.032(5) 0.042(5) 0.030(5) 0.002(4) 0.011(4) 0.003(4) C33 0.027(4) 0.046(5) 0.020(4) -0.005(4) 0.008(3) -0.002(4) C34 0.042(5) 0.055(6) 0.032(5) -0.023(4) -0.014(4) -0.015(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 Lu O1 2.098(5) . ? Lu O2 2.099(4) . ? Lu O3 2.332(5) . ? Lu O4 2.334(5) . ? Lu C23 2.348(7) . ? Lu S 2.9553(17) . ? Si C23 1.821(7) . ? Si C25 1.864(11) . ? Si C24 1.879(8) . ? Si C26 1.882(9) . ? S C2 1.794(7) . ? S C12 1.794(7) . ? O1 C1 1.323(8) . ? O2 C13 1.332(8) . ? O3 C30 1.451(9) . ? O3 C27 1.461(9) . ? O4 C34 1.419(10) . ? O4 C31 1.459(8) . ? C1 C2 1.399(9) . ? C1 C6 1.420(9) . ? C2 C3 1.388(9) . ? C3 C4 1.386(10) . ? C3 H3 0.9500 . ? C4 C5 1.389(10) . ? C4 C7 1.513(10) . ? C5 C6 1.395(9) . ? C5 H5 0.9500 . ? C6 C8 1.529(9) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.525(10) . ? C8 C11 1.533(10) . ? C8 C10 1.548(10) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C17 1.395(9) . ? C12 C13 1.399(9) . ? C13 C14 1.426(9) . ? C14 C15 1.386(9) . ? C14 C19 1.526(10) . ? C15 C16 1.403(10) . ? C15 H15 0.9500 . ? C16 C17 1.380(10) . ? C16 C18 1.514(10) . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.531(11) . ? C19 C21 1.543(10) . ? C19 C22 1.540(10) . ? 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 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.497(12) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.505(13) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.506(12) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.500(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.532(11) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.513(12) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 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 O1 Lu O2 97.26(18) . . ? O1 Lu O3 150.02(18) . . ? O2 Lu O3 85.74(17) . . ? O1 Lu O4 86.10(18) . . ? O2 Lu O4 156.49(18) . . ? O3 Lu O4 80.16(17) . . ? O1 Lu C23 104.4(2) . . ? O2 Lu C23 108.3(2) . . ? O3 Lu C23 102.9(2) . . ? O4 Lu C23 93.2(2) . . ? O1 Lu S 69.48(13) . . ? O2 Lu S 70.51(13) . . ? O3 Lu S 83.73(14) . . ? O4 Lu S 89.22(13) . . ? C23 Lu S 173.23(19) . . ? C23 Si C25 111.1(5) . . ? C23 Si C24 110.3(4) . . ? C25 Si C24 109.6(5) . . ? C23 Si C26 113.6(4) . . ? C25 Si C26 108.0(6) . . ? C24 Si C26 103.9(4) . . ? C2 S C12 103.5(3) . . ? C2 S Lu 94.5(2) . . ? C12 S Lu 93.6(2) . . ? C1 O1 Lu 136.0(4) . . ? C13 O2 Lu 133.7(4) . . ? C30 O3 C27 108.6(6) . . ? C30 O3 Lu 126.0(4) . . ? C27 O3 Lu 121.7(4) . . ? C34 O4 C31 108.5(6) . . ? C34 O4 Lu 126.6(5) . . ? C31 O4 Lu 123.9(4) . . ? O1 C1 C2 121.2(6) . . ? O1 C1 C6 120.9(6) . . ? C2 C1 C6 117.9(6) . . ? C3 C2 C1 122.9(6) . . ? C3 C2 S 118.9(5) . . ? C1 C2 S 118.1(5) . . ? C2 C3 C4 119.5(6) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 118.2(6) . . ? C5 C4 C7 120.6(7) . . ? C3 C4 C7 121.3(7) . . ? C4 C5 C6 123.7(6) . . ? C4 C5 H5 118.1 . . ? C6 C5 H5 118.1 . . ? C5 C6 C1 117.8(6) . . ? C5 C6 C8 121.5(6) . . ? C1 C6 C8 120.7(6) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C6 109.9(6) . . ? C9 C8 C11 108.6(6) . . ? C6 C8 C11 112.5(6) . . ? C9 C8 C10 109.8(6) . . ? C6 C8 C10 109.9(6) . . ? C11 C8 C10 106.1(6) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 122.7(6) . . ? C17 C12 S 118.5(5) . . ? C13 C12 S 118.8(5) . . ? O2 C13 C12 121.8(6) . . ? O2 C13 C14 120.7(6) . . ? C12 C13 C14 117.5(6) . . ? C15 C14 C13 118.0(6) . . ? C15 C14 C19 121.2(6) . . ? C13 C14 C19 120.8(6) . . ? C14 C15 C16 124.5(6) . . ? C14 C15 H15 117.8 . . ? C16 C15 H15 117.8 . . ? C17 C16 C15 116.8(6) . . ? C17 C16 C18 122.4(7) . . ? C15 C16 C18 120.7(7) . . ? C16 C17 C12 120.5(7) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 C20 109.8(6) . . ? C14 C19 C21 109.8(6) . . ? C20 C19 C21 110.5(6) . . ? C14 C19 C22 113.6(6) . . ? C20 C19 C22 106.8(7) . . ? C21 C19 C22 106.2(7) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si C23 Lu 129.5(4) . . ? Si C23 H23A 104.9 . . ? Lu C23 H23A 104.9 . . ? Si C23 H23B 104.9 . . ? Lu C23 H23B 104.9 . . ? H23A C23 H23B 105.8 . . ? Si C24 H24A 109.5 . . ? Si C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si C25 H25A 109.5 . . ? Si C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si C26 H26A 109.5 . . ? Si C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O3 C27 C28 105.2(7) . . ? O3 C27 H27A 110.7 . . ? C28 C27 H27A 110.7 . . ? O3 C27 H27B 110.7 . . ? C28 C27 H27B 110.7 . . ? H27A C27 H27B 108.8 . . ? C27 C28 C29 101.9(7) . . ? C27 C28 H28A 111.4 . . ? C29 C28 H28A 111.4 . . ? C27 C28 H28B 111.4 . . ? C29 C28 H28B 111.4 . . ? H28A C28 H28B 109.3 . . ? C30 C29 C28 103.8(7) . . ? C30 C29 H29A 111.0 . . ? C28 C29 H29A 111.0 . . ? C30 C29 H29B 111.0 . . ? C28 C29 H29B 111.0 . . ? H29A C29 H29B 109.0 . . ? O3 C30 C29 105.8(7) . . ? O3 C30 H30A 110.6 . . ? C29 C30 H30A 110.6 . . ? O3 C30 H30B 110.6 . . ? C29 C30 H30B 110.6 . . ? H30A C30 H30B 108.7 . . ? O4 C31 C32 105.2(6) . . ? O4 C31 H31A 110.7 . . ? C32 C31 H31A 110.7 . . ? O4 C31 H31B 110.7 . . ? C32 C31 H31B 110.7 . . ? H31A C31 H31B 108.8 . . ? C31 C32 C33 103.4(6) . . ? C31 C32 H32A 111.1 . . ? C33 C32 H32A 111.1 . . ? C31 C32 H32B 111.1 . . ? C33 C32 H32B 111.1 . . ? H32A C32 H32B 109.1 . . ? C34 C33 C32 98.8(6) . . ? C34 C33 H33A 112.0 . . ? C32 C33 H33A 112.0 . . ? C34 C33 H33B 112.0 . . ? C32 C33 H33B 112.0 . . ? H33A C33 H33B 109.7 . . ? O4 C34 C33 107.2(7) . . ? O4 C34 H34A 110.3 . . ? C33 C34 H34A 110.3 . . ? O4 C34 H34B 110.3 . . ? C33 C34 H34B 110.3 . . ? H34A C34 H34B 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Lu S C2 5.0(3) . . . . ? O2 Lu S C2 111.0(3) . . . . ? O3 Lu S C2 -161.3(2) . . . . ? O4 Lu S C2 -81.1(2) . . . . ? C23 Lu S C2 30.1(15) . . . . ? O1 Lu S C12 -98.8(3) . . . . ? O2 Lu S C12 7.2(2) . . . . ? O3 Lu S C12 94.9(2) . . . . ? O4 Lu S C12 175.0(2) . . . . ? C23 Lu S C12 -73.7(15) . . . . ? O2 Lu O1 C1 -75.7(6) . . . . ? O3 Lu O1 C1 18.3(8) . . . . ? O4 Lu O1 C1 80.9(6) . . . . ? C23 Lu O1 C1 173.2(6) . . . . ? S Lu O1 C1 -9.7(6) . . . . ? O1 Lu O2 C13 52.3(6) . . . . ? O3 Lu O2 C13 -97.7(6) . . . . ? O4 Lu O2 C13 -44.6(8) . . . . ? C23 Lu O2 C13 160.1(6) . . . . ? S Lu O2 C13 -12.8(5) . . . . ? O1 Lu O3 C30 35.0(8) . . . . ? O2 Lu O3 C30 132.2(6) . . . . ? O4 Lu O3 C30 -28.9(6) . . . . ? C23 Lu O3 C30 -120.0(6) . . . . ? S Lu O3 C30 61.4(6) . . . . ? O1 Lu O3 C27 -120.7(6) . . . . ? O2 Lu O3 C27 -23.5(6) . . . . ? O4 Lu O3 C27 175.3(6) . . . . ? C23 Lu O3 C27 84.3(6) . . . . ? S Lu O3 C27 -94.4(5) . . . . ? O1 Lu O4 C34 -45.7(6) . . . . ? O2 Lu O4 C34 53.6(8) . . . . ? O3 Lu O4 C34 107.6(6) . . . . ? C23 Lu O4 C34 -149.9(6) . . . . ? S Lu O4 C34 23.8(6) . . . . ? O1 Lu O4 C31 121.7(5) . . . . ? O2 Lu O4 C31 -139.1(6) . . . . ? O3 Lu O4 C31 -85.1(5) . . . . ? C23 Lu O4 C31 17.5(6) . . . . ? S Lu O4 C31 -168.9(5) . . . . ? Lu O1 C1 C2 11.2(10) . . . . ? Lu O1 C1 C6 -167.7(5) . . . . ? O1 C1 C2 C3 -178.2(6) . . . . ? C6 C1 C2 C3 0.7(10) . . . . ? O1 C1 C2 S -2.3(9) . . . . ? C6 C1 C2 S 176.6(5) . . . . ? C12 S C2 C3 -92.2(6) . . . . ? Lu S C2 C3 173.0(5) . . . . ? C12 S C2 C1 91.8(6) . . . . ? Lu S C2 C1 -3.0(5) . . . . ? C1 C2 C3 C4 -0.3(10) . . . . ? S C2 C3 C4 -176.2(5) . . . . ? C2 C3 C4 C5 -0.2(10) . . . . ? C2 C3 C4 C7 -178.8(6) . . . . ? C3 C4 C5 C6 0.2(11) . . . . ? C7 C4 C5 C6 178.8(7) . . . . ? C4 C5 C6 C1 0.2(10) . . . . ? C4 C5 C6 C8 178.7(6) . . . . ? O1 C1 C6 C5 178.2(6) . . . . ? C2 C1 C6 C5 -0.7(10) . . . . ? O1 C1 C6 C8 -0.3(10) . . . . ? C2 C1 C6 C8 -179.2(6) . . . . ? C5 C6 C8 C9 121.1(7) . . . . ? C1 C6 C8 C9 -60.5(8) . . . . ? C5 C6 C8 C11 -0.1(10) . . . . ? C1 C6 C8 C11 178.3(7) . . . . ? C5 C6 C8 C10 -118.1(7) . . . . ? C1 C6 C8 C10 60.3(9) . . . . ? C2 S C12 C17 79.2(6) . . . . ? Lu S C12 C17 174.7(5) . . . . ? C2 S C12 C13 -100.3(6) . . . . ? Lu S C12 C13 -4.9(5) . . . . ? Lu O2 C13 C12 14.3(9) . . . . ? Lu O2 C13 C14 -165.7(5) . . . . ? C17 C12 C13 O2 178.2(6) . . . . ? S C12 C13 O2 -2.2(9) . . . . ? C17 C12 C13 C14 -1.7(10) . . . . ? S C12 C13 C14 177.8(5) . . . . ? O2 C13 C14 C15 -178.9(6) . . . . ? C12 C13 C14 C15 1.1(9) . . . . ? O2 C13 C14 C19 0.0(10) . . . . ? C12 C13 C14 C19 180.0(6) . . . . ? C13 C14 C15 C16 -0.2(11) . . . . ? C19 C14 C15 C16 -179.1(7) . . . . ? C14 C15 C16 C17 -0.1(11) . . . . ? C14 C15 C16 C18 178.3(7) . . . . ? C15 C16 C17 C12 -0.6(10) . . . . ? C18 C16 C17 C12 -178.9(7) . . . . ? C13 C12 C17 C16 1.5(10) . . . . ? S C12 C17 C16 -178.0(5) . . . . ? C15 C14 C19 C20 -123.2(7) . . . . ? C13 C14 C19 C20 57.9(8) . . . . ? C15 C14 C19 C21 115.1(7) . . . . ? C13 C14 C19 C21 -63.8(9) . . . . ? C15 C14 C19 C22 -3.6(10) . . . . ? C13 C14 C19 C22 177.5(7) . . . . ? C25 Si C23 Lu -76.6(6) . . . . ? C24 Si C23 Lu 45.2(6) . . . . ? C26 Si C23 Lu 161.4(5) . . . . ? O1 Lu C23 Si 103.7(5) . . . . ? O2 Lu C23 Si 0.9(6) . . . . ? O3 Lu C23 Si -88.8(5) . . . . ? O4 Lu C23 Si -169.5(5) . . . . ? S Lu C23 Si 79.5(16) . . . . ? C30 O3 C27 C28 -20.1(9) . . . . ? Lu O3 C27 C28 139.3(6) . . . . ? O3 C27 C28 C29 35.3(9) . . . . ? C27 C28 C29 C30 -37.3(10) . . . . ? C27 O3 C30 C29 -3.7(10) . . . . ? Lu O3 C30 C29 -162.0(6) . . . . ? C28 C29 C30 O3 25.8(11) . . . . ? C34 O4 C31 C32 -6.8(8) . . . . ? Lu O4 C31 C32 -176.1(5) . . . . ? O4 C31 C32 C33 29.9(8) . . . . ? C31 C32 C33 C34 -39.6(8) . . . . ? C31 O4 C34 C33 -19.6(8) . . . . ? Lu O4 C34 C33 149.4(5) . . . . ? C32 C33 C34 O4 36.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.42 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.994 _refine_diff_density_min -4.259 _refine_diff_density_rms 0.170 #===END #============================================================================== data_mk1_tBu _database_code_depnum_ccdc_archive 'CCDC 643865' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(tetrahydrofurane)-thiobis(4,6-di-tert-butylphenolato)- trimethylsilylmethyl-lutetium(III) ; _chemical_name_common ; Bis(tetrahydrofurane)-thiobis(4,6-di-tert-butylphenolato)- trimethylsilylmethyl-lutetium(iii) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H67 Lu O4 S Si' _chemical_formula_weight 847.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.820(3) _cell_length_b 23.858(6) _cell_length_c 16.458(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.261(4) _cell_angle_gamma 90.00 _cell_volume 4241.6(19) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 932 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 2.440 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6637 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43156 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 28.37 _reflns_number_total 10572 _reflns_number_gt 8546 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SIR-97 (Altomare et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+0.6476P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10572 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0697 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.006 _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 Si Si -0.23673(8) 0.14985(4) 0.95402(5) 0.02472(18) Uani 1 1 d . . . S S 0.36006(7) 0.18561(3) 1.03895(4) 0.01859(14) Uani 1 1 d . . . Lu Lu 0.105939(11) 0.148945(5) 1.006080(7) 0.01795(4) Uani 1 1 d . . . O1 O 0.10294(18) 0.23323(8) 1.04627(12) 0.0214(4) Uani 1 1 d . . . O2 O 0.17642(19) 0.11170(8) 1.11485(12) 0.0226(4) Uani 1 1 d . . . O3 O 0.1790(2) 0.06911(8) 0.94348(12) 0.0258(5) Uani 1 1 d . . . O4 O 0.1549(2) 0.18540(8) 0.87799(12) 0.0239(4) Uani 1 1 d . . . C1 C 0.1915(3) 0.27085(11) 1.06513(16) 0.0186(6) Uani 1 1 d . . . C2 C 0.3179(3) 0.25563(11) 1.06555(16) 0.0181(6) Uani 1 1 d . . . C3 C 0.4126(3) 0.29441(12) 1.08334(16) 0.0200(6) Uani 1 1 d . . . H3 H 0.4946 0.2829 1.0818 0.024 Uiso 1 1 calc R . . C4 C 0.3871(3) 0.34946(11) 1.10310(17) 0.0200(6) Uani 1 1 d . . . C5 C 0.2607(3) 0.36413(12) 1.10306(17) 0.0220(6) Uani 1 1 d . . . H5 H 0.2415 0.4009 1.1161 0.026 Uiso 1 1 calc R . . C6 C 0.1627(3) 0.32755(12) 1.08496(17) 0.0205(6) Uani 1 1 d . . . C7 C 0.4868(3) 0.39386(12) 1.12260(18) 0.0227(6) Uani 1 1 d . . . C8 C 0.6178(3) 0.36978(14) 1.1228(2) 0.0322(7) Uani 1 1 d . . . H8A H 0.6769 0.3990 1.1351 0.048 Uiso 1 1 calc R . . H8B H 0.6315 0.3544 1.0701 0.048 Uiso 1 1 calc R . . H8C H 0.6272 0.3408 1.1631 0.048 Uiso 1 1 calc R . . C9 C 0.4692(3) 0.42020(14) 1.20616(19) 0.0334(8) Uani 1 1 d . . . H9A H 0.4810 0.3921 1.2476 0.050 Uiso 1 1 calc R . . H9B H 0.3871 0.4353 1.2073 0.050 Uiso 1 1 calc R . . H9C H 0.5286 0.4497 1.2159 0.050 Uiso 1 1 calc R . . C10 C 0.4741(3) 0.44025(13) 1.0572(2) 0.0322(7) Uani 1 1 d . . . H10A H 0.5361 0.4684 1.0685 0.048 Uiso 1 1 calc R . . H10B H 0.3935 0.4569 1.0579 0.048 Uiso 1 1 calc R . . H10C H 0.4849 0.4242 1.0045 0.048 Uiso 1 1 calc R . . C11 C 0.0269(3) 0.34718(12) 1.08707(19) 0.0263(7) Uani 1 1 d . . . C12 C 0.0171(3) 0.40926(14) 1.1113(2) 0.0417(9) Uani 1 1 d . . . H12A H 0.0570 0.4148 1.1643 0.063 Uiso 1 1 calc R . . H12B H -0.0686 0.4196 1.1124 0.063 Uiso 1 1 calc R . . H12C H 0.0566 0.4321 1.0724 0.063 Uiso 1 1 calc R . . C13 C -0.0406(3) 0.31214(14) 1.14974(19) 0.0315(7) Uani 1 1 d . . . H13A H -0.0026 0.3184 1.2031 0.047 Uiso 1 1 calc R . . H13B H -0.0352 0.2731 1.1362 0.047 Uiso 1 1 calc R . . H13C H -0.1260 0.3231 1.1488 0.047 Uiso 1 1 calc R . . C14 C -0.0386(3) 0.34119(13) 1.00211(19) 0.0295(7) Uani 1 1 d . . . H14A H -0.1228 0.3537 1.0038 0.044 Uiso 1 1 calc R . . H14B H -0.0374 0.3026 0.9856 0.044 Uiso 1 1 calc R . . H14C H 0.0035 0.3636 0.9639 0.044 Uiso 1 1 calc R . . C15 C 0.3786(3) 0.15067(11) 1.13534(17) 0.0191(6) Uani 1 1 d . . . C16 C 0.2794(3) 0.11839(11) 1.16231(16) 0.0182(6) Uani 1 1 d . . . C17 C 0.2944(3) 0.09376(11) 1.24122(17) 0.0203(6) Uani 1 1 d . . . C18 C 0.4079(3) 0.10096(11) 1.28487(17) 0.0214(6) Uani 1 1 d . . . H18 H 0.4176 0.0844 1.3360 0.026 Uiso 1 1 calc R . . C19 C 0.5089(3) 0.13158(12) 1.25695(17) 0.0212(6) Uani 1 1 d . . . C20 C 0.4902(3) 0.15663(11) 1.18084(17) 0.0214(6) Uani 1 1 d . . . H20 H 0.5534 0.1777 1.1600 0.026 Uiso 1 1 calc R . . C21 C 0.6292(3) 0.13775(13) 1.31033(19) 0.0262(7) Uani 1 1 d . . . C22 C 0.7346(3) 0.16246(16) 1.2631(2) 0.0390(9) Uani 1 1 d . . . H22A H 0.7475 0.1396 1.2164 0.059 Uiso 1 1 calc R . . H22B H 0.8091 0.1635 1.2977 0.059 Uiso 1 1 calc R . . H22C H 0.7132 0.1998 1.2458 0.059 Uiso 1 1 calc R . . C23 C 0.6040(3) 0.17685(14) 1.3820(2) 0.0359(8) Uani 1 1 d . . . H23A H 0.5816 0.2134 1.3616 0.054 Uiso 1 1 calc R . . H23B H 0.6773 0.1797 1.4176 0.054 Uiso 1 1 calc R . . H23C H 0.5376 0.1619 1.4116 0.054 Uiso 1 1 calc R . . C24 C 0.6724(3) 0.08050(14) 1.3444(2) 0.0317(7) Uani 1 1 d . . . H24A H 0.6123 0.0663 1.3798 0.048 Uiso 1 1 calc R . . H24B H 0.7506 0.0848 1.3743 0.048 Uiso 1 1 calc R . . H24C H 0.6813 0.0548 1.3003 0.048 Uiso 1 1 calc R . . C25 C 0.1888(3) 0.05980(13) 1.27615(18) 0.0243(6) Uani 1 1 d . . . C26 C 0.2178(3) 0.04244(15) 1.36523(19) 0.0347(8) Uani 1 1 d . . . H26A H 0.2894 0.0186 1.3685 0.052 Uiso 1 1 calc R . . H26B H 0.1484 0.0226 1.3849 0.052 Uiso 1 1 calc R . . H26C H 0.2337 0.0753 1.3978 0.052 Uiso 1 1 calc R . . C27 C 0.1677(3) 0.00607(13) 1.2256(2) 0.0322(7) Uani 1 1 d . . . H27A H 0.1483 0.0158 1.1697 0.048 Uiso 1 1 calc R . . H27B H 0.1002 -0.0147 1.2461 0.048 Uiso 1 1 calc R . . H27C H 0.2414 -0.0164 1.2294 0.048 Uiso 1 1 calc R . . C28 C 0.0678(3) 0.09433(14) 1.2744(2) 0.0326(8) Uani 1 1 d . . . H28A H 0.0798 0.1268 1.3083 0.049 Uiso 1 1 calc R . . H28B H 0.0025 0.0718 1.2943 0.049 Uiso 1 1 calc R . . H28C H 0.0459 0.1058 1.2196 0.049 Uiso 1 1 calc R . . C29 C -0.1001(3) 0.11429(14) 1.00172(19) 0.0294(7) Uani 1 1 d . . . H29A H -0.0973 0.0777 0.9762 0.035 Uiso 1 1 calc R . . H29B H -0.1188 0.1077 1.0579 0.035 Uiso 1 1 calc R . . C30 C -0.2070(4) 0.17333(18) 0.8478(2) 0.0464(10) Uani 1 1 d . . . H30A H -0.1402 0.1999 0.8498 0.070 Uiso 1 1 calc R . . H30B H -0.2803 0.1906 0.8236 0.070 Uiso 1 1 calc R . . H30C H -0.1853 0.1415 0.8159 0.070 Uiso 1 1 calc R . . C31 C -0.2726(3) 0.21207(14) 1.0175(2) 0.0356(8) Uani 1 1 d . . . H31A H -0.2816 0.2004 1.0726 0.053 Uiso 1 1 calc R . . H31B H -0.3482 0.2290 0.9964 0.053 Uiso 1 1 calc R . . H31C H -0.2064 0.2388 1.0160 0.053 Uiso 1 1 calc R . . C32 C -0.3821(3) 0.10665(14) 0.9420(2) 0.0372(8) Uani 1 1 d . . . H32A H -0.3662 0.0735 0.9112 0.056 Uiso 1 1 calc R . . H32B H -0.4461 0.1282 0.9138 0.056 Uiso 1 1 calc R . . H32C H -0.4082 0.0962 0.9947 0.056 Uiso 1 1 calc R . . C33 C 0.2842(3) 0.03374(14) 0.9678(2) 0.0344(8) Uani 1 1 d . . . H33A H 0.2619 0.0063 1.0079 0.041 Uiso 1 1 calc R . . H33B H 0.3528 0.0561 0.9904 0.041 Uiso 1 1 calc R . . C34 C 0.3178(4) 0.00518(16) 0.8895(2) 0.0478(10) Uani 1 1 d . . . H34A H 0.3839 0.0253 0.8647 0.057 Uiso 1 1 calc R . . H34B H 0.3446 -0.0331 0.9001 0.057 Uiso 1 1 calc R . . C35 C 0.2007(4) 0.00610(16) 0.8345(2) 0.0436(9) Uani 1 1 d . . . H35A H 0.2151 0.0247 0.7835 0.052 Uiso 1 1 calc R . . H35B H 0.1717 -0.0317 0.8229 0.052 Uiso 1 1 calc R . . C36 C 0.1076(3) 0.03823(14) 0.8814(2) 0.0357(8) Uani 1 1 d . . . H36A H 0.0604 0.0637 0.8457 0.043 Uiso 1 1 calc R . . H36B H 0.0508 0.0127 0.9060 0.043 Uiso 1 1 calc R . . C37 C 0.1325(3) 0.24463(13) 0.85508(19) 0.0308(7) Uani 1 1 d . . . H37A H 0.1361 0.2683 0.9031 0.037 Uiso 1 1 calc R . . H37B H 0.0516 0.2488 0.8272 0.037 Uiso 1 1 calc R . . C38 C 0.2313(5) 0.26030(18) 0.8005(4) 0.0835(18) Uani 1 1 d . . . H38A H 0.1976 0.2633 0.7448 0.100 Uiso 1 1 calc R . . H38B H 0.2669 0.2962 0.8167 0.100 Uiso 1 1 calc R . . C39 C 0.3253(4) 0.21682(15) 0.8069(2) 0.0408(9) Uani 1 1 d . . . H39A H 0.3893 0.2260 0.8484 0.049 Uiso 1 1 calc R . . H39B H 0.3632 0.2116 0.7554 0.049 Uiso 1 1 calc R . . C40 C 0.2553(3) 0.16533(13) 0.82971(19) 0.0301(7) Uani 1 1 d . . . H40A H 0.2224 0.1459 0.7814 0.036 Uiso 1 1 calc R . . H40B H 0.3088 0.1399 0.8614 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si 0.0218(5) 0.0286(4) 0.0237(4) 0.0023(3) 0.0006(3) -0.0010(4) S 0.0203(4) 0.0183(3) 0.0172(3) 0.0000(3) 0.0014(3) 0.0005(3) Lu 0.01833(7) 0.01832(7) 0.01703(6) 0.00072(5) -0.00055(4) -0.00162(5) O1 0.0199(11) 0.0225(10) 0.0217(10) -0.0020(8) 0.0008(8) -0.0025(8) O2 0.0237(11) 0.0236(10) 0.0199(10) 0.0031(8) -0.0024(8) -0.0037(9) O3 0.0278(12) 0.0211(11) 0.0280(11) -0.0042(8) -0.0026(9) -0.0001(9) O4 0.0305(12) 0.0206(10) 0.0211(10) 0.0029(8) 0.0038(9) 0.0001(9) C1 0.0202(15) 0.0213(14) 0.0144(13) 0.0028(10) 0.0008(11) -0.0024(11) C2 0.0223(15) 0.0163(13) 0.0161(13) 0.0003(10) 0.0034(11) 0.0018(11) C3 0.0181(15) 0.0218(14) 0.0201(14) 0.0019(11) 0.0024(11) 0.0026(11) C4 0.0210(15) 0.0191(13) 0.0199(14) 0.0006(11) -0.0007(11) -0.0003(12) C5 0.0262(17) 0.0182(14) 0.0217(14) -0.0023(11) 0.0016(12) 0.0019(12) C6 0.0200(15) 0.0227(14) 0.0188(14) -0.0014(11) 0.0006(12) 0.0030(12) C7 0.0230(16) 0.0223(15) 0.0227(14) -0.0015(11) 0.0005(12) -0.0025(12) C8 0.0236(18) 0.0307(17) 0.042(2) -0.0040(15) -0.0004(15) -0.0074(14) C9 0.034(2) 0.0349(18) 0.0310(18) -0.0078(14) 0.0004(15) -0.0076(15) C10 0.036(2) 0.0266(16) 0.0342(18) 0.0052(14) 0.0012(15) -0.0074(14) C11 0.0232(17) 0.0254(16) 0.0302(16) -0.0041(13) 0.0009(13) 0.0030(13) C12 0.028(2) 0.0341(19) 0.063(3) -0.0137(17) 0.0016(18) 0.0071(15) C13 0.0237(18) 0.044(2) 0.0271(17) -0.0040(14) 0.0033(14) 0.0068(15) C14 0.0243(18) 0.0315(18) 0.0325(17) 0.0027(13) -0.0009(14) 0.0032(13) C15 0.0222(15) 0.0188(13) 0.0163(13) 0.0004(11) 0.0006(11) 0.0025(12) C16 0.0195(15) 0.0164(13) 0.0182(13) -0.0026(10) -0.0025(11) 0.0012(11) C17 0.0231(16) 0.0152(13) 0.0226(14) -0.0016(11) 0.0013(12) 0.0009(11) C18 0.0267(17) 0.0204(14) 0.0170(13) 0.0004(11) -0.0005(12) 0.0020(12) C19 0.0188(16) 0.0217(14) 0.0228(15) -0.0028(11) -0.0011(12) 0.0016(12) C20 0.0224(16) 0.0194(14) 0.0226(15) -0.0004(11) 0.0020(12) -0.0007(11) C21 0.0251(17) 0.0283(17) 0.0247(16) -0.0003(12) -0.0036(13) -0.0010(13) C22 0.0250(19) 0.050(2) 0.041(2) 0.0095(17) -0.0080(15) -0.0060(16) C23 0.036(2) 0.0326(19) 0.0375(19) -0.0056(15) -0.0109(16) 0.0013(15) C24 0.0283(19) 0.0324(18) 0.0335(18) -0.0007(14) -0.0060(14) 0.0054(14) C25 0.0231(16) 0.0261(16) 0.0235(15) 0.0051(12) -0.0003(12) -0.0036(12) C26 0.0314(19) 0.042(2) 0.0305(17) 0.0117(15) 0.0005(14) -0.0094(15) C27 0.036(2) 0.0262(16) 0.0337(18) 0.0000(13) -0.0020(15) -0.0096(14) C28 0.0258(18) 0.042(2) 0.0305(17) 0.0099(14) 0.0038(14) -0.0011(14) C29 0.0237(17) 0.0300(17) 0.0345(18) 0.0043(13) 0.0015(14) -0.0023(13) C30 0.046(2) 0.061(3) 0.032(2) 0.0094(18) 0.0025(17) 0.002(2) C31 0.033(2) 0.0374(19) 0.0365(19) -0.0014(15) 0.0025(15) -0.0017(15) C32 0.029(2) 0.0339(19) 0.048(2) -0.0014(16) -0.0062(16) -0.0001(15) C33 0.036(2) 0.0282(17) 0.0382(19) 0.0000(14) -0.0013(16) 0.0051(14) C34 0.056(3) 0.043(2) 0.046(2) 0.0006(18) 0.012(2) 0.0183(19) C35 0.057(3) 0.037(2) 0.038(2) -0.0129(16) 0.0139(19) -0.0114(18) C36 0.042(2) 0.0312(18) 0.0336(18) -0.0125(14) -0.0035(16) -0.0068(15) C37 0.042(2) 0.0243(16) 0.0259(16) 0.0073(12) 0.0019(15) 0.0053(14) C38 0.083(4) 0.036(2) 0.138(5) 0.026(3) 0.063(4) 0.006(2) C39 0.045(2) 0.036(2) 0.043(2) 0.0035(16) 0.0174(18) -0.0072(17) C40 0.037(2) 0.0294(16) 0.0241(16) 0.0004(12) 0.0087(14) 0.0022(14) _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 Si C29 1.841(3) . ? Si C31 1.868(3) . ? Si C30 1.880(4) . ? Si C32 1.882(3) . ? S C2 1.793(3) . ? S C15 1.793(3) . ? S Lu 2.9066(10) . ? Lu O2 2.103(2) . ? Lu O1 2.118(2) . ? Lu O3 2.325(2) . ? Lu O4 2.368(2) . ? Lu C29 2.375(3) . ? O1 C1 1.337(3) . ? O2 C16 1.334(3) . ? O3 C36 1.447(4) . ? O3 C33 1.455(4) . ? O4 C40 1.462(4) . ? O4 C37 1.479(3) . ? C1 C2 1.414(4) . ? C1 C6 1.430(4) . ? C2 C3 1.399(4) . ? C3 C4 1.385(4) . ? C3 H3 0.9300 . ? C4 C5 1.411(4) . ? C4 C7 1.533(4) . ? C5 C6 1.393(4) . ? C5 H5 0.9300 . ? C6 C11 1.544(4) . ? C7 C8 1.529(4) . ? C7 C9 1.534(4) . ? C7 C10 1.545(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C14 1.538(4) . ? C11 C12 1.539(4) . ? C11 C13 1.543(4) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C20 1.392(4) . ? C15 C16 1.412(4) . ? C16 C17 1.426(4) . ? C17 C18 1.397(4) . ? C17 C25 1.539(4) . ? C18 C19 1.413(4) . ? C18 H18 0.9300 . ? C19 C20 1.392(4) . ? C19 C21 1.536(4) . ? C20 H20 0.9300 . ? C21 C22 1.534(5) . ? C21 C24 1.539(4) . ? C21 C23 1.541(4) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C27 1.538(4) . ? C25 C26 1.539(4) . ? C25 C28 1.546(4) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.519(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.515(5) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.513(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.483(5) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.452(6) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.502(4) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? 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 C29 Si C31 108.37(16) . . ? C29 Si C30 110.97(17) . . ? C31 Si C30 109.56(18) . . ? C29 Si C32 116.02(15) . . ? C31 Si C32 107.16(16) . . ? C30 Si C32 104.56(18) . . ? C2 S C15 103.54(12) . . ? C2 S Lu 94.27(10) . . ? C15 S Lu 94.68(10) . . ? O2 Lu O1 98.43(8) . . ? O2 Lu O3 85.13(8) . . ? O1 Lu O3 158.10(8) . . ? O2 Lu O4 145.53(8) . . ? O1 Lu O4 86.42(7) . . ? O3 Lu O4 78.90(7) . . ? O2 Lu C29 99.96(9) . . ? O1 Lu C29 108.00(10) . . ? O3 Lu C29 92.50(10) . . ? O4 Lu C29 110.99(9) . . ? O2 Lu S 71.05(6) . . ? O1 Lu S 71.77(6) . . ? O3 Lu S 89.27(6) . . ? O4 Lu S 78.34(5) . . ? C29 Lu S 170.67(8) . . ? C1 O1 Lu 133.37(18) . . ? C16 O2 Lu 134.31(17) . . ? C36 O3 C33 106.1(2) . . ? C36 O3 Lu 123.28(19) . . ? C33 O3 Lu 129.33(18) . . ? C40 O4 C37 106.9(2) . . ? C40 O4 Lu 125.04(17) . . ? C37 O4 Lu 122.41(16) . . ? O1 C1 C2 120.6(2) . . ? O1 C1 C6 121.7(3) . . ? C2 C1 C6 117.7(3) . . ? C3 C2 C1 121.9(3) . . ? C3 C2 S 118.3(2) . . ? C1 C2 S 119.8(2) . . ? C4 C3 C2 121.5(3) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 116.2(3) . . ? C3 C4 C7 123.9(3) . . ? C5 C4 C7 119.9(2) . . ? C6 C5 C4 124.8(3) . . ? C6 C5 H5 117.6 . . ? C4 C5 H5 117.6 . . ? C5 C6 C1 117.9(3) . . ? C5 C6 C11 121.3(3) . . ? C1 C6 C11 120.8(3) . . ? C8 C7 C4 112.5(2) . . ? C8 C7 C9 108.4(3) . . ? C4 C7 C9 110.4(2) . . ? C8 C7 C10 108.4(3) . . ? C4 C7 C10 108.4(2) . . ? C9 C7 C10 108.7(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C12 106.9(3) . . ? C14 C11 C13 110.3(3) . . ? C12 C11 C13 107.8(3) . . ? C14 C11 C6 109.9(2) . . ? C12 C11 C6 112.2(3) . . ? C13 C11 C6 109.7(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 122.5(3) . . ? C20 C15 S 118.6(2) . . ? C16 C15 S 118.9(2) . . ? O2 C16 C15 120.4(2) . . ? O2 C16 C17 122.1(3) . . ? C15 C16 C17 117.5(3) . . ? C18 C17 C16 117.9(3) . . ? C18 C17 C25 121.5(3) . . ? C16 C17 C25 120.6(3) . . ? C17 C18 C19 124.7(3) . . ? C17 C18 H18 117.6 . . ? C19 C18 H18 117.6 . . ? C20 C19 C18 116.1(3) . . ? C20 C19 C21 123.3(3) . . ? C18 C19 C21 120.7(3) . . ? C15 C20 C19 121.2(3) . . ? C15 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C22 C21 C19 112.2(3) . . ? C22 C21 C24 107.9(3) . . ? C19 C21 C24 110.7(3) . . ? C22 C21 C23 108.9(3) . . ? C19 C21 C23 108.4(3) . . ? C24 C21 C23 108.8(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C26 107.9(3) . . ? C27 C25 C17 109.1(2) . . ? C26 C25 C17 112.5(3) . . ? C27 C25 C28 109.6(3) . . ? C26 C25 C28 106.7(3) . . ? C17 C25 C28 111.0(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si C29 Lu 125.59(16) . . ? Si C29 H29A 105.9 . . ? Lu C29 H29A 105.9 . . ? Si C29 H29B 105.9 . . ? Lu C29 H29B 105.9 . . ? H29A C29 H29B 106.2 . . ? Si C30 H30A 109.5 . . ? Si C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si C31 H31A 109.5 . . ? Si C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si C32 H32A 109.5 . . ? Si C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O3 C33 C34 104.4(3) . . ? O3 C33 H33A 110.9 . . ? C34 C33 H33A 110.9 . . ? O3 C33 H33B 110.9 . . ? C34 C33 H33B 110.9 . . ? H33A C33 H33B 108.9 . . ? C35 C34 C33 105.5(3) . . ? C35 C34 H34A 110.6 . . ? C33 C34 H34A 110.6 . . ? C35 C34 H34B 110.6 . . ? C33 C34 H34B 110.6 . . ? H34A C34 H34B 108.8 . . ? C36 C35 C34 105.1(3) . . ? C36 C35 H35A 110.7 . . ? C34 C35 H35A 110.7 . . ? C36 C35 H35B 110.7 . . ? C34 C35 H35B 110.7 . . ? H35A C35 H35B 108.8 . . ? O3 C36 C35 105.9(3) . . ? O3 C36 H36A 110.5 . . ? C35 C36 H36A 110.5 . . ? O3 C36 H36B 110.5 . . ? C35 C36 H36B 110.5 . . ? H36A C36 H36B 108.7 . . ? O4 C37 C38 106.4(3) . . ? O4 C37 H37A 110.5 . . ? C38 C37 H37A 110.5 . . ? O4 C37 H37B 110.5 . . ? C38 C37 H37B 110.5 . . ? H37A C37 H37B 108.6 . . ? C39 C38 C37 107.6(3) . . ? C39 C38 H38A 110.2 . . ? C37 C38 H38A 110.2 . . ? C39 C38 H38B 110.2 . . ? C37 C38 H38B 110.2 . . ? H38A C38 H38B 108.5 . . ? C38 C39 C40 103.9(3) . . ? C38 C39 H39A 111.0 . . ? C40 C39 H39A 111.0 . . ? C38 C39 H39B 111.0 . . ? C40 C39 H39B 111.0 . . ? H39A C39 H39B 109.0 . . ? O4 C40 C39 105.6(3) . . ? O4 C40 H40A 110.6 . . ? C39 C40 H40A 110.6 . . ? O4 C40 H40B 110.6 . . ? C39 C40 H40B 110.6 . . ? H40A C40 H40B 108.8 . . ? 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 C2 S Lu O2 -108.24(10) . . . . ? C15 S Lu O2 -4.25(11) . . . . ? C2 S Lu O1 -2.20(10) . . . . ? C15 S Lu O1 101.79(11) . . . . ? C2 S Lu O3 166.66(10) . . . . ? C15 S Lu O3 -89.35(10) . . . . ? C2 S Lu O4 87.85(10) . . . . ? C15 S Lu O4 -168.16(10) . . . . ? C2 S Lu C29 -92.3(5) . . . . ? C15 S Lu C29 11.7(5) . . . . ? O2 Lu O1 C1 70.9(2) . . . . ? O3 Lu O1 C1 -27.1(4) . . . . ? O4 Lu O1 C1 -74.8(2) . . . . ? C29 Lu O1 C1 174.3(2) . . . . ? S Lu O1 C1 4.1(2) . . . . ? O1 Lu O2 C16 -58.3(2) . . . . ? O3 Lu O2 C16 99.9(2) . . . . ? O4 Lu O2 C16 37.7(3) . . . . ? C29 Lu O2 C16 -168.4(2) . . . . ? S Lu O2 C16 9.0(2) . . . . ? O2 Lu O3 C36 134.7(2) . . . . ? O1 Lu O3 C36 -124.8(3) . . . . ? O4 Lu O3 C36 -76.0(2) . . . . ? C29 Lu O3 C36 34.9(2) . . . . ? S Lu O3 C36 -154.3(2) . . . . ? O2 Lu O3 C33 -30.3(2) . . . . ? O1 Lu O3 C33 70.2(3) . . . . ? O4 Lu O3 C33 119.0(2) . . . . ? C29 Lu O3 C33 -130.1(2) . . . . ? S Lu O3 C33 40.8(2) . . . . ? O2 Lu O4 C40 31.8(3) . . . . ? O1 Lu O4 C40 131.5(2) . . . . ? O3 Lu O4 C40 -32.2(2) . . . . ? C29 Lu O4 C40 -120.6(2) . . . . ? S Lu O4 C40 59.4(2) . . . . ? O2 Lu O4 C37 -118.1(2) . . . . ? O1 Lu O4 C37 -18.4(2) . . . . ? O3 Lu O4 C37 177.9(2) . . . . ? C29 Lu O4 C37 89.5(2) . . . . ? S Lu O4 C37 -90.6(2) . . . . ? Lu O1 C1 C2 -4.7(4) . . . . ? Lu O1 C1 C6 174.90(19) . . . . ? O1 C1 C2 C3 178.6(2) . . . . ? C6 C1 C2 C3 -1.0(4) . . . . ? O1 C1 C2 S 1.0(4) . . . . ? C6 C1 C2 S -178.6(2) . . . . ? C15 S C2 C3 87.8(2) . . . . ? Lu S C2 C3 -176.3(2) . . . . ? C15 S C2 C1 -94.5(2) . . . . ? Lu S C2 C1 1.3(2) . . . . ? C1 C2 C3 C4 1.4(4) . . . . ? S C2 C3 C4 179.0(2) . . . . ? C2 C3 C4 C5 -0.9(4) . . . . ? C2 C3 C4 C7 -179.6(3) . . . . ? C3 C4 C5 C6 0.1(4) . . . . ? C7 C4 C5 C6 178.9(3) . . . . ? C4 C5 C6 C1 0.2(4) . . . . ? C4 C5 C6 C11 179.5(3) . . . . ? O1 C1 C6 C5 -179.4(2) . . . . ? C2 C1 C6 C5 0.3(4) . . . . ? O1 C1 C6 C11 1.3(4) . . . . ? C2 C1 C6 C11 -179.1(3) . . . . ? C3 C4 C7 C8 -3.4(4) . . . . ? C5 C4 C7 C8 177.9(3) . . . . ? C3 C4 C7 C9 -124.6(3) . . . . ? C5 C4 C7 C9 56.8(4) . . . . ? C3 C4 C7 C10 116.5(3) . . . . ? C5 C4 C7 C10 -62.2(3) . . . . ? C5 C6 C11 C14 118.4(3) . . . . ? C1 C6 C11 C14 -62.3(3) . . . . ? C5 C6 C11 C12 -0.4(4) . . . . ? C1 C6 C11 C12 178.9(3) . . . . ? C5 C6 C11 C13 -120.2(3) . . . . ? C1 C6 C11 C13 59.1(3) . . . . ? C2 S C15 C20 -82.4(2) . . . . ? Lu S C15 C20 -177.9(2) . . . . ? C2 S C15 C16 97.4(2) . . . . ? Lu S C15 C16 1.9(2) . . . . ? Lu O2 C16 C15 -11.0(4) . . . . ? Lu O2 C16 C17 168.99(19) . . . . ? C20 C15 C16 O2 -176.8(2) . . . . ? S C15 C16 O2 3.5(4) . . . . ? C20 C15 C16 C17 3.3(4) . . . . ? S C15 C16 C17 -176.5(2) . . . . ? O2 C16 C17 C18 177.1(2) . . . . ? C15 C16 C17 C18 -3.0(4) . . . . ? O2 C16 C17 C25 -2.2(4) . . . . ? C15 C16 C17 C25 177.8(2) . . . . ? C16 C17 C18 C19 0.9(4) . . . . ? C25 C17 C18 C19 -179.9(3) . . . . ? C17 C18 C19 C20 1.1(4) . . . . ? C17 C18 C19 C21 179.1(3) . . . . ? C16 C15 C20 C19 -1.3(4) . . . . ? S C15 C20 C19 178.5(2) . . . . ? C18 C19 C20 C15 -0.9(4) . . . . ? C21 C19 C20 C15 -178.8(3) . . . . ? C20 C19 C21 C22 -13.2(4) . . . . ? C18 C19 C21 C22 169.1(3) . . . . ? C20 C19 C21 C24 -133.7(3) . . . . ? C18 C19 C21 C24 48.5(4) . . . . ? C20 C19 C21 C23 107.1(3) . . . . ? C18 C19 C21 C23 -70.6(3) . . . . ? C18 C17 C25 C27 -112.5(3) . . . . ? C16 C17 C25 C27 66.7(3) . . . . ? C18 C17 C25 C26 7.2(4) . . . . ? C16 C17 C25 C26 -173.6(3) . . . . ? C18 C17 C25 C28 126.6(3) . . . . ? C16 C17 C25 C28 -54.1(4) . . . . ? C31 Si C29 Lu -70.9(2) . . . . ? C30 Si C29 Lu 49.4(3) . . . . ? C32 Si C29 Lu 168.55(18) . . . . ? O2 Lu C29 Si 151.03(18) . . . . ? O1 Lu C29 Si 48.7(2) . . . . ? O3 Lu C29 Si -123.48(19) . . . . ? O4 Lu C29 Si -44.4(2) . . . . ? S Lu C29 Si 135.8(4) . . . . ? C36 O3 C33 C34 36.1(3) . . . . ? Lu O3 C33 C34 -156.9(2) . . . . ? O3 C33 C34 C35 -23.8(4) . . . . ? C33 C34 C35 C36 3.4(4) . . . . ? C33 O3 C36 C35 -34.3(3) . . . . ? Lu O3 C36 C35 157.7(2) . . . . ? C34 C35 C36 O3 18.4(4) . . . . ? C40 O4 C37 C38 -6.7(4) . . . . ? Lu O4 C37 C38 147.9(3) . . . . ? O4 C37 C38 C39 -13.3(5) . . . . ? C37 C38 C39 C40 27.3(5) . . . . ? C37 O4 C40 C39 23.4(3) . . . . ? Lu O4 C40 C39 -130.3(2) . . . . ? C38 C39 C40 O4 -31.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.191 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.105 #===END #============================================================================== data_mk2 _database_code_depnum_ccdc_archive 'CCDC 643866' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrahydrofurane-1,4-dithiabutanediyl-bis(6-tert-butyl-4-methylphenolato)- trimethylsilylmethyl-lutetium(III) ; _chemical_name_common ; Tetrahydrofurane-1,4-dithiabutanediyl-bis(6-tert-butyl-4- methylphenolato)-trimethylsilylmethyl-lutetium(iii) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H51 Lu O3 S2 Si' _chemical_formula_weight 750.94 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' 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' S S 0.1250 0.1230 '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 8.7517(17) _cell_length_b 12.703(2) _cell_length_c 16.986(3) _cell_angle_alpha 75.023(4) _cell_angle_beta 82.049(5) _cell_angle_gamma 75.436(4) _cell_volume 1760.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 982 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 23.41 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 2.985 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4781 _exptl_absorpt_correction_T_max 0.8651 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24117 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.35 _reflns_number_total 8702 _reflns_number_gt 7813 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8702 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si Si 0.11966(15) 0.34348(10) 0.37775(8) 0.0352(3) Uani 1 1 d . . . S1 S 0.04311(14) 0.04481(8) 0.13083(7) 0.0327(2) Uani 1 1 d . . . S2 S 0.36062(13) 0.13197(8) 0.17985(7) 0.0330(2) Uani 1 1 d . . . Lu Lu 0.068524(19) 0.125466(13) 0.276223(10) 0.02507(6) Uani 1 1 d . . . O1 O -0.0544(3) 0.2542(2) 0.18691(17) 0.0290(6) Uani 1 1 d . . . O2 O 0.2234(3) -0.0340(2) 0.30515(17) 0.0313(6) Uani 1 1 d . . . O3 O -0.1501(3) 0.0641(2) 0.32943(18) 0.0364(7) Uani 1 1 d . . . C1 C -0.1053(5) 0.2662(3) 0.1140(2) 0.0283(9) Uani 1 1 d . . . C2 C -0.0713(5) 0.1737(3) 0.0778(3) 0.0302(9) Uani 1 1 d . . . C3 C -0.1250(5) 0.1812(4) 0.0028(3) 0.0350(10) Uani 1 1 d . . . H3 H -0.1011 0.1171 -0.0196 0.042 Uiso 1 1 calc R . . C4 C -0.2125(5) 0.2805(4) -0.0393(3) 0.0357(10) Uani 1 1 d . . . C5 C -0.2425(5) 0.3721(4) -0.0048(3) 0.0334(10) Uani 1 1 d . . . H5 H -0.3014 0.4412 -0.0342 0.040 Uiso 1 1 calc R . . C6 C -0.1922(5) 0.3698(3) 0.0699(2) 0.0268(8) Uani 1 1 d . . . C7 C -0.2698(6) 0.2913(4) -0.1217(3) 0.0520(14) Uani 1 1 d . . . H7A H -0.2029 0.2327 -0.1471 0.078 Uiso 1 1 calc R . . H7B H -0.2640 0.3649 -0.1568 0.078 Uiso 1 1 calc R . . H7C H -0.3797 0.2832 -0.1144 0.078 Uiso 1 1 calc R . . C8 C -0.2296(5) 0.4745(3) 0.1051(3) 0.0324(9) Uani 1 1 d . . . C9 C -0.0758(5) 0.4979(4) 0.1231(3) 0.0403(11) Uani 1 1 d . . . H9A H -0.1012 0.5624 0.1479 0.060 Uiso 1 1 calc R . . H9B H -0.0095 0.5139 0.0720 0.060 Uiso 1 1 calc R . . H9C H -0.0186 0.4322 0.1609 0.060 Uiso 1 1 calc R . . C10 C -0.3410(5) 0.4569(4) 0.1827(3) 0.0401(11) Uani 1 1 d . . . H10A H -0.4390 0.4433 0.1697 0.060 Uiso 1 1 calc R . . H10B H -0.3659 0.5238 0.2049 0.060 Uiso 1 1 calc R . . H10C H -0.2895 0.3923 0.2234 0.060 Uiso 1 1 calc R . . C11 C -0.3126(6) 0.5787(3) 0.0446(3) 0.0436(12) Uani 1 1 d . . . H11A H -0.4136 0.5676 0.0333 0.065 Uiso 1 1 calc R . . H11B H -0.2451 0.5909 -0.0065 0.065 Uiso 1 1 calc R . . H11C H -0.3322 0.6439 0.0683 0.065 Uiso 1 1 calc R . . C12 C 0.2351(5) 0.0434(4) 0.0742(3) 0.0389(11) Uani 1 1 d . . . H12A H 0.3071 -0.0295 0.0950 0.047 Uiso 1 1 calc R . . H12B H 0.2226 0.0488 0.0161 0.047 Uiso 1 1 calc R . . C13 C 0.3123(6) 0.1344(4) 0.0782(3) 0.0400(11) Uani 1 1 d . . . H13A H 0.2410 0.2075 0.0567 0.048 Uiso 1 1 calc R . . H13B H 0.4110 0.1293 0.0416 0.048 Uiso 1 1 calc R . . C14 C 0.4527(5) -0.0113(3) 0.2163(2) 0.0272(9) Uani 1 1 d . . . C15 C 0.3675(5) -0.0787(3) 0.2767(2) 0.0280(9) Uani 1 1 d . . . C16 C 0.4437(5) -0.1933(3) 0.3066(2) 0.0272(9) Uani 1 1 d . . . C17 C 0.5955(5) -0.2307(3) 0.2741(3) 0.0326(9) Uani 1 1 d . . . H17 H 0.6461 -0.3069 0.2937 0.039 Uiso 1 1 calc R . . C18 C 0.6801(5) -0.1637(3) 0.2141(3) 0.0347(10) Uani 1 1 d . . . C19 C 0.6064(5) -0.0530(3) 0.1864(3) 0.0319(9) Uani 1 1 d . . . H19 H 0.6608 -0.0049 0.1465 0.038 Uiso 1 1 calc R . . C20 C 0.8469(5) -0.2106(4) 0.1838(3) 0.0496(13) Uani 1 1 d . . . H20A H 0.8458 -0.2310 0.1321 0.074 Uiso 1 1 calc R . . H20B H 0.8937 -0.2772 0.2244 0.074 Uiso 1 1 calc R . . H20C H 0.9099 -0.1542 0.1752 0.074 Uiso 1 1 calc R . . C21 C 0.3589(5) -0.2695(3) 0.3738(3) 0.0297(9) Uani 1 1 d . . . C22 C 0.2061(5) -0.2792(4) 0.3440(3) 0.0367(10) Uani 1 1 d . . . H22A H 0.1424 -0.2042 0.3226 0.055 Uiso 1 1 calc R . . H22B H 0.1455 -0.3192 0.3897 0.055 Uiso 1 1 calc R . . H22C H 0.2331 -0.3203 0.3006 0.055 Uiso 1 1 calc R . . C23 C 0.3216(6) -0.2225(4) 0.4505(3) 0.0403(11) Uani 1 1 d . . . H23A H 0.4193 -0.2125 0.4667 0.060 Uiso 1 1 calc R . . H23B H 0.2762 -0.2748 0.4950 0.060 Uiso 1 1 calc R . . H23C H 0.2456 -0.1502 0.4389 0.060 Uiso 1 1 calc R . . C24 C 0.4604(5) -0.3886(3) 0.3976(3) 0.0396(11) Uani 1 1 d . . . H24A H 0.4816 -0.4222 0.3502 0.059 Uiso 1 1 calc R . . H24B H 0.4037 -0.4336 0.4421 0.059 Uiso 1 1 calc R . . H24C H 0.5608 -0.3862 0.4157 0.059 Uiso 1 1 calc R . . C25 C 0.1001(5) 0.2005(4) 0.3832(3) 0.0356(10) Uani 1 1 d . . . H25A H 0.0092 0.1890 0.4235 0.043 Uiso 1 1 calc R . . H25B H 0.1951 0.1503 0.4091 0.043 Uiso 1 1 calc R . . C26 C 0.2654(6) 0.3872(4) 0.2919(3) 0.0562(14) Uani 1 1 d . . . H26A H 0.3700 0.3375 0.3015 0.084 Uiso 1 1 calc R . . H26B H 0.2710 0.4643 0.2887 0.084 Uiso 1 1 calc R . . H26C H 0.2317 0.3827 0.2404 0.084 Uiso 1 1 calc R . . C27 C 0.1906(6) 0.3578(5) 0.4731(3) 0.0550(14) Uani 1 1 d . . . H27A H 0.1192 0.3334 0.5203 0.082 Uiso 1 1 calc R . . H27B H 0.1919 0.4362 0.4681 0.082 Uiso 1 1 calc R . . H27C H 0.2978 0.3113 0.4807 0.082 Uiso 1 1 calc R . . C28 C -0.0748(6) 0.4460(4) 0.3615(3) 0.0485(13) Uani 1 1 d . . . H28A H -0.1181 0.4393 0.3132 0.073 Uiso 1 1 calc R . . H28B H -0.0594 0.5220 0.3530 0.073 Uiso 1 1 calc R . . H28C H -0.1487 0.4304 0.4096 0.073 Uiso 1 1 calc R . . C29 C -0.3086(5) 0.1299(4) 0.3148(4) 0.0567(15) Uani 1 1 d . . . H29A H -0.3358 0.1300 0.2601 0.068 Uiso 1 1 calc R . . H29B H -0.3168 0.2081 0.3174 0.068 Uiso 1 1 calc R . . C30 C -0.4177(6) 0.0776(5) 0.3797(4) 0.0569(15) Uani 1 1 d . . . H30A H -0.5157 0.0769 0.3569 0.068 Uiso 1 1 calc R . . H30B H -0.4465 0.1179 0.4241 0.068 Uiso 1 1 calc R . . C31 C -0.3239(7) -0.0390(5) 0.4099(4) 0.0700(19) Uani 1 1 d . . . H31A H -0.3491 -0.0656 0.4693 0.084 Uiso 1 1 calc R . . H31B H -0.3481 -0.0906 0.3811 0.084 Uiso 1 1 calc R . . C32 C -0.1612(7) -0.0339(5) 0.3934(4) 0.090(3) Uani 1 1 d . . . H32A H -0.0986 -0.1018 0.3761 0.108 Uiso 1 1 calc R . . H32B H -0.1186 -0.0298 0.4433 0.108 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si 0.0333(7) 0.0345(7) 0.0393(7) -0.0126(6) -0.0031(5) -0.0060(5) S1 0.0423(6) 0.0213(5) 0.0328(6) -0.0066(4) -0.0052(5) -0.0028(4) S2 0.0315(6) 0.0213(5) 0.0420(6) -0.0036(4) 0.0034(5) -0.0054(4) Lu 0.02366(10) 0.02139(9) 0.02731(10) -0.00422(7) -0.00161(7) -0.00166(6) O1 0.0348(16) 0.0209(13) 0.0281(15) -0.0049(11) -0.0049(12) -0.0004(12) O2 0.0280(15) 0.0225(14) 0.0350(16) 0.0007(12) 0.0017(12) -0.0006(12) O3 0.0304(16) 0.0341(16) 0.0400(18) 0.0016(14) -0.0041(13) -0.0088(13) C1 0.027(2) 0.027(2) 0.029(2) -0.0052(17) -0.0009(17) -0.0055(17) C2 0.034(2) 0.0222(19) 0.032(2) -0.0052(17) -0.0040(18) -0.0025(17) C3 0.035(2) 0.033(2) 0.037(2) -0.0130(19) -0.0041(19) -0.0032(19) C4 0.030(2) 0.044(3) 0.032(2) -0.012(2) -0.0062(18) -0.0003(19) C5 0.029(2) 0.033(2) 0.030(2) -0.0009(18) -0.0012(17) -0.0001(18) C6 0.022(2) 0.025(2) 0.030(2) -0.0036(17) -0.0010(16) -0.0037(16) C7 0.050(3) 0.057(3) 0.044(3) -0.023(3) -0.017(2) 0.013(3) C8 0.035(2) 0.024(2) 0.034(2) -0.0046(18) -0.0005(18) -0.0028(18) C9 0.044(3) 0.026(2) 0.051(3) -0.012(2) -0.001(2) -0.007(2) C10 0.037(3) 0.034(2) 0.043(3) -0.010(2) 0.006(2) -0.001(2) C11 0.047(3) 0.025(2) 0.048(3) -0.003(2) -0.003(2) 0.004(2) C12 0.042(3) 0.036(2) 0.031(2) -0.012(2) 0.000(2) 0.006(2) C13 0.041(3) 0.031(2) 0.036(3) 0.0017(19) 0.004(2) 0.001(2) C14 0.028(2) 0.0181(18) 0.033(2) -0.0023(16) -0.0057(17) -0.0023(16) C15 0.028(2) 0.025(2) 0.032(2) -0.0064(17) -0.0043(17) -0.0067(17) C16 0.029(2) 0.026(2) 0.028(2) -0.0063(17) -0.0111(17) -0.0039(17) C17 0.033(2) 0.026(2) 0.038(2) -0.0081(18) -0.0058(19) -0.0027(18) C18 0.028(2) 0.030(2) 0.046(3) -0.016(2) 0.0037(19) -0.0033(18) C19 0.027(2) 0.029(2) 0.039(2) -0.0058(19) 0.0039(18) -0.0104(17) C20 0.037(3) 0.033(2) 0.075(4) -0.019(3) 0.016(3) -0.004(2) C21 0.030(2) 0.028(2) 0.029(2) -0.0043(17) -0.0059(17) -0.0033(17) C22 0.037(3) 0.030(2) 0.043(3) -0.0013(19) -0.005(2) -0.0134(19) C23 0.043(3) 0.043(3) 0.033(2) -0.006(2) -0.004(2) -0.008(2) C24 0.041(3) 0.029(2) 0.042(3) -0.001(2) -0.005(2) -0.004(2) C25 0.036(2) 0.036(2) 0.031(2) -0.0088(19) -0.0028(19) -0.0011(19) C26 0.054(3) 0.049(3) 0.067(4) -0.015(3) 0.008(3) -0.019(3) C27 0.056(3) 0.057(3) 0.060(4) -0.024(3) -0.019(3) -0.008(3) C28 0.044(3) 0.048(3) 0.051(3) -0.019(3) -0.005(2) 0.001(2) C29 0.026(3) 0.052(3) 0.081(4) 0.002(3) -0.007(3) -0.005(2) C30 0.037(3) 0.067(4) 0.065(4) -0.016(3) 0.005(3) -0.013(3) C31 0.047(3) 0.083(5) 0.068(4) 0.013(3) 0.000(3) -0.025(3) C32 0.052(4) 0.067(4) 0.107(6) 0.047(4) 0.010(4) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si C25 1.844(5) . ? Si C26 1.867(5) . ? Si C28 1.870(5) . ? Si C27 1.879(5) . ? S1 C2 1.777(4) . ? S1 C12 1.815(5) . ? S1 Lu 2.9619(12) . ? S2 C14 1.779(4) . ? S2 C13 1.825(5) . ? S2 Lu 2.8461(12) . ? Lu O1 2.101(3) . ? Lu O2 2.115(3) . ? Lu O3 2.234(3) . ? Lu C25 2.335(4) . ? O1 C1 1.333(5) . ? O2 C15 1.327(5) . ? O3 C32 1.440(6) . ? O3 C29 1.446(5) . ? C1 C2 1.412(6) . ? C1 C6 1.420(5) . ? C2 C3 1.391(6) . ? C3 C4 1.374(6) . ? C3 H3 0.9500 . ? C4 C5 1.388(6) . ? C4 C7 1.512(6) . ? C5 C6 1.390(6) . ? C5 H5 0.9500 . ? C6 C8 1.540(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C10 1.530(6) . ? C8 C11 1.535(6) . ? C8 C9 1.535(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.498(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C19 1.393(5) . ? C14 C15 1.412(5) . ? C15 C16 1.431(5) . ? C16 C17 1.382(6) . ? C16 C21 1.531(6) . ? C17 C18 1.404(6) . ? C17 H17 0.9500 . ? C18 C19 1.378(6) . ? C18 C20 1.505(6) . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23 1.532(6) . ? C21 C24 1.533(5) . ? C21 C22 1.537(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.489(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.497(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.427(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 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 C25 Si C26 110.7(2) . . ? C25 Si C28 110.9(2) . . ? C26 Si C28 108.4(2) . . ? C25 Si C27 113.2(2) . . ? C26 Si C27 106.6(3) . . ? C28 Si C27 106.8(2) . . ? C2 S1 C12 101.2(2) . . ? C2 S1 Lu 95.44(14) . . ? C12 S1 Lu 104.10(15) . . ? C14 S2 C13 102.1(2) . . ? C14 S2 Lu 96.36(14) . . ? C13 S2 Lu 103.31(16) . . ? O1 Lu O2 147.93(11) . . ? O1 Lu O3 92.55(11) . . ? O2 Lu O3 94.76(11) . . ? O1 Lu C25 108.71(13) . . ? O2 Lu C25 101.10(13) . . ? O3 Lu C25 98.08(14) . . ? O1 Lu S2 91.15(8) . . ? O2 Lu S2 71.07(8) . . ? O3 Lu S2 157.46(8) . . ? C25 Lu S2 101.76(12) . . ? O1 Lu S1 68.62(8) . . ? O2 Lu S1 80.72(8) . . ? O3 Lu S1 86.42(8) . . ? C25 Lu S1 174.95(11) . . ? S2 Lu S1 74.28(3) . . ? C1 O1 Lu 137.9(2) . . ? C15 O2 Lu 134.3(2) . . ? C32 O3 C29 108.3(4) . . ? C32 O3 Lu 127.3(3) . . ? C29 O3 Lu 123.6(3) . . ? O1 C1 C2 119.7(4) . . ? O1 C1 C6 122.5(4) . . ? C2 C1 C6 117.9(4) . . ? C3 C2 C1 121.9(4) . . ? C3 C2 S1 119.9(3) . . ? C1 C2 S1 118.3(3) . . ? C4 C3 C2 120.6(4) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 117.6(4) . . ? C3 C4 C7 121.6(4) . . ? C5 C4 C7 120.8(4) . . ? C4 C5 C6 124.5(4) . . ? C4 C5 H5 117.8 . . ? C6 C5 H5 117.8 . . ? C5 C6 C1 117.6(4) . . ? C5 C6 C8 122.0(4) . . ? C1 C6 C8 120.4(4) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C10 C8 C11 107.6(4) . . ? C10 C8 C9 110.9(4) . . ? C11 C8 C9 107.3(4) . . ? C10 C8 C6 109.4(3) . . ? C11 C8 C6 111.6(4) . . ? C9 C8 C6 110.1(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 S1 115.6(3) . . ? C13 C12 H12A 108.4 . . ? S1 C12 H12A 108.4 . . ? C13 C12 H12B 108.4 . . ? S1 C12 H12B 108.4 . . ? H12A C12 H12B 107.4 . . ? C12 C13 S2 115.2(3) . . ? C12 C13 H13A 108.5 . . ? S2 C13 H13A 108.5 . . ? C12 C13 H13B 108.5 . . ? S2 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C19 C14 C15 122.1(4) . . ? C19 C14 S2 119.6(3) . . ? C15 C14 S2 118.3(3) . . ? O2 C15 C14 119.8(3) . . ? O2 C15 C16 122.4(4) . . ? C14 C15 C16 117.8(4) . . ? C17 C16 C15 117.7(4) . . ? C17 C16 C21 122.2(4) . . ? C15 C16 C21 120.1(4) . . ? C16 C17 C18 124.4(4) . . ? C16 C17 H17 117.8 . . ? C18 C17 H17 117.8 . . ? C19 C18 C17 117.4(4) . . ? C19 C18 C20 121.6(4) . . ? C17 C18 C20 120.9(4) . . ? C18 C19 C14 120.5(4) . . ? C18 C19 H19 119.8 . . ? C14 C19 H19 119.8 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 C23 109.6(3) . . ? C16 C21 C24 112.1(4) . . ? C23 C21 C24 107.7(3) . . ? C16 C21 C22 110.2(3) . . ? C23 C21 C22 110.5(4) . . ? C24 C21 C22 106.7(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si C25 Lu 127.9(2) . . ? Si C25 H25A 105.3 . . ? Lu C25 H25A 105.3 . . ? Si C25 H25B 105.3 . . ? Lu C25 H25B 105.3 . . ? H25A C25 H25B 106.0 . . ? Si C26 H26A 109.5 . . ? Si C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si C27 H27A 109.5 . . ? Si C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si C28 H28A 109.5 . . ? Si C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C29 C30 107.0(4) . . ? O3 C29 H29A 110.3 . . ? C30 C29 H29A 110.3 . . ? O3 C29 H29B 110.3 . . ? C30 C29 H29B 110.3 . . ? H29A C29 H29B 108.6 . . ? C29 C30 C31 103.8(4) . . ? C29 C30 H30A 111.0 . . ? C31 C30 H30A 111.0 . . ? C29 C30 H30B 111.0 . . ? C31 C30 H30B 111.0 . . ? H30A C30 H30B 109.0 . . ? C32 C31 C30 106.3(5) . . ? C32 C31 H31A 110.5 . . ? C30 C31 H31A 110.5 . . ? C32 C31 H31B 110.5 . . ? C30 C31 H31B 110.5 . . ? H31A C31 H31B 108.7 . . ? C31 C32 O3 108.3(5) . . ? C31 C32 H32A 110.0 . . ? O3 C32 H32A 110.0 . . ? C31 C32 H32B 110.0 . . ? O3 C32 H32B 110.0 . . ? H32A C32 H32B 108.4 . . ? 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 C14 S2 Lu O1 -150.60(15) . . . . ? C13 S2 Lu O1 -46.57(16) . . . . ? C14 S2 Lu O2 2.17(16) . . . . ? C13 S2 Lu O2 106.20(17) . . . . ? C14 S2 Lu O3 -51.1(2) . . . . ? C13 S2 Lu O3 52.9(3) . . . . ? C14 S2 Lu C25 100.02(17) . . . . ? C13 S2 Lu C25 -155.96(18) . . . . ? C14 S2 Lu S1 -83.21(14) . . . . ? C13 S2 Lu S1 20.82(14) . . . . ? C2 S1 Lu O1 -2.50(16) . . . . ? C12 S1 Lu O1 100.52(17) . . . . ? C2 S1 Lu O2 -172.92(16) . . . . ? C12 S1 Lu O2 -69.91(17) . . . . ? C2 S1 Lu O3 91.66(16) . . . . ? C12 S1 Lu O3 -165.33(17) . . . . ? C2 S1 Lu C25 -61.4(12) . . . . ? C12 S1 Lu C25 41.6(12) . . . . ? C2 S1 Lu S2 -100.11(14) . . . . ? C12 S1 Lu S2 2.90(15) . . . . ? O2 Lu O1 C1 21.3(5) . . . . ? O3 Lu O1 C1 -81.8(4) . . . . ? C25 Lu O1 C1 178.7(4) . . . . ? S2 Lu O1 C1 75.9(4) . . . . ? S1 Lu O1 C1 3.3(4) . . . . ? O1 Lu O2 C15 55.5(4) . . . . ? O3 Lu O2 C15 158.1(4) . . . . ? C25 Lu O2 C15 -102.7(4) . . . . ? S2 Lu O2 C15 -4.0(3) . . . . ? S1 Lu O2 C15 72.5(4) . . . . ? O1 Lu O3 C32 174.6(5) . . . . ? O2 Lu O3 C32 25.9(5) . . . . ? C25 Lu O3 C32 -76.0(5) . . . . ? S2 Lu O3 C32 75.5(6) . . . . ? S1 Lu O3 C32 106.3(5) . . . . ? O1 Lu O3 C29 -17.7(4) . . . . ? O2 Lu O3 C29 -166.5(4) . . . . ? C25 Lu O3 C29 91.6(4) . . . . ? S2 Lu O3 C29 -116.9(4) . . . . ? S1 Lu O3 C29 -86.1(4) . . . . ? Lu O1 C1 C2 -2.5(6) . . . . ? Lu O1 C1 C6 178.2(3) . . . . ? O1 C1 C2 C3 178.4(4) . . . . ? C6 C1 C2 C3 -2.3(6) . . . . ? O1 C1 C2 S1 -1.4(5) . . . . ? C6 C1 C2 S1 177.9(3) . . . . ? C12 S1 C2 C3 77.4(4) . . . . ? Lu S1 C2 C3 -177.0(3) . . . . ? C12 S1 C2 C1 -102.8(4) . . . . ? Lu S1 C2 C1 2.8(3) . . . . ? C1 C2 C3 C4 0.8(7) . . . . ? S1 C2 C3 C4 -179.5(4) . . . . ? C2 C3 C4 C5 0.9(7) . . . . ? C2 C3 C4 C7 178.9(4) . . . . ? C3 C4 C5 C6 -1.0(7) . . . . ? C7 C4 C5 C6 -179.0(4) . . . . ? C4 C5 C6 C1 -0.5(6) . . . . ? C4 C5 C6 C8 -179.9(4) . . . . ? O1 C1 C6 C5 -178.5(4) . . . . ? C2 C1 C6 C5 2.1(6) . . . . ? O1 C1 C6 C8 0.8(6) . . . . ? C2 C1 C6 C8 -178.5(4) . . . . ? C5 C6 C8 C10 113.7(4) . . . . ? C1 C6 C8 C10 -65.6(5) . . . . ? C5 C6 C8 C11 -5.2(6) . . . . ? C1 C6 C8 C11 175.5(4) . . . . ? C5 C6 C8 C9 -124.3(4) . . . . ? C1 C6 C8 C9 56.4(5) . . . . ? C2 S1 C12 C13 64.0(4) . . . . ? Lu S1 C12 C13 -34.6(4) . . . . ? S1 C12 C13 S2 62.9(4) . . . . ? C14 S2 C13 C12 46.9(4) . . . . ? Lu S2 C13 C12 -52.8(3) . . . . ? C13 S2 C14 C19 74.9(4) . . . . ? Lu S2 C14 C19 -180.0(3) . . . . ? C13 S2 C14 C15 -106.6(3) . . . . ? Lu S2 C14 C15 -1.5(3) . . . . ? Lu O2 C15 C14 4.3(6) . . . . ? Lu O2 C15 C16 -177.6(3) . . . . ? C19 C14 C15 O2 177.7(4) . . . . ? S2 C14 C15 O2 -0.7(5) . . . . ? C19 C14 C15 C16 -0.4(6) . . . . ? S2 C14 C15 C16 -178.9(3) . . . . ? O2 C15 C16 C17 -178.4(4) . . . . ? C14 C15 C16 C17 -0.3(6) . . . . ? O2 C15 C16 C21 0.1(6) . . . . ? C14 C15 C16 C21 178.3(4) . . . . ? C15 C16 C17 C18 0.3(6) . . . . ? C21 C16 C17 C18 -178.2(4) . . . . ? C16 C17 C18 C19 0.5(7) . . . . ? C16 C17 C18 C20 178.3(4) . . . . ? C17 C18 C19 C14 -1.2(7) . . . . ? C20 C18 C19 C14 -179.0(4) . . . . ? C15 C14 C19 C18 1.2(7) . . . . ? S2 C14 C19 C18 179.7(3) . . . . ? C17 C16 C21 C23 118.3(4) . . . . ? C15 C16 C21 C23 -60.2(5) . . . . ? C17 C16 C21 C24 -1.2(5) . . . . ? C15 C16 C21 C24 -179.7(4) . . . . ? C17 C16 C21 C22 -119.9(4) . . . . ? C15 C16 C21 C22 61.6(5) . . . . ? C26 Si C25 Lu -46.7(4) . . . . ? C28 Si C25 Lu 73.7(3) . . . . ? C27 Si C25 Lu -166.3(3) . . . . ? O1 Lu C25 Si -30.5(3) . . . . ? O2 Lu C25 Si 137.5(3) . . . . ? O3 Lu C25 Si -126.0(3) . . . . ? S2 Lu C25 Si 64.8(3) . . . . ? S1 Lu C25 Si 26.9(15) . . . . ? C32 O3 C29 C30 7.6(7) . . . . ? Lu O3 C29 C30 -162.0(3) . . . . ? O3 C29 C30 C31 -20.2(6) . . . . ? C29 C30 C31 C32 25.6(7) . . . . ? C30 C31 C32 O3 -21.8(8) . . . . ? C29 O3 C32 C31 9.0(8) . . . . ? Lu O3 C32 C31 178.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.379 _refine_diff_density_min -1.011 _refine_diff_density_rms 0.125 #===END #============================================================================== data_mk5 _database_code_depnum_ccdc_archive 'CCDC 643867' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(tetrahydrofurane)-thiobis(6-tert-butyl-4-methylphenolato)- triphenylmethoxy-lutetium(III) ; _chemical_name_common ; Bis(tetrahydrofurane)-thiobis(6-tert-butyl-4-methylphenolato)- triphenylmethoxy-lutetium(iii) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55.75 H74 Lu O5.75 S' _chemical_formula_weight 1043.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.017(5) _cell_length_b 18.291(3) _cell_length_c 20.635(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.832(3) _cell_angle_gamma 90.00 _cell_volume 11794(3) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 925 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 18.54 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4332 _exptl_absorpt_coefficient_mu 1.750 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3868 _exptl_absorpt_correction_T_max 0.8044 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 80196 _diffrn_reflns_av_R_equivalents 0.0954 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.40 _reflns_number_total 14774 _reflns_number_gt 9713 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SIR-97 (Altomare et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0723P)^2^+10.7922P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14774 _refine_ls_number_parameters 573 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0936 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1488 _refine_ls_wR_factor_gt 0.1294 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.076 _refine_ls_shift/su_mean 0.001 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 0.680768(7) 0.059132(12) 0.197726(11) 0.03248(8) Uani 1 1 d . . . S S 0.73786(5) 0.13079(8) 0.13673(8) 0.0460(4) Uani 1 1 d . . . O1 O 0.72717(12) 0.1191(2) 0.2742(2) 0.0428(9) Uani 1 1 d . . . O2 O 0.64849(12) 0.1485(2) 0.1393(2) 0.0440(9) Uani 1 1 d . . . O3 O 0.65939(13) -0.0111(2) 0.09985(19) 0.0498(10) Uani 1 1 d . . . O4 O 0.72992(13) -0.0359(2) 0.2250(2) 0.0491(10) Uani 1 1 d . . . O5 O 0.63951(11) 0.0245(2) 0.24497(18) 0.0375(8) Uani 1 1 d . . . C1 C 0.76281(18) 0.1535(3) 0.2761(3) 0.0444(14) Uani 1 1 d . . . C2 C 0.77277(18) 0.1643(3) 0.2158(3) 0.0485(15) Uani 1 1 d . . . C3 C 0.8102(2) 0.2008(4) 0.2164(4) 0.064(2) Uani 1 1 d . . . H3 H 0.8162 0.2078 0.1748 0.077 Uiso 1 1 calc R . . C4 C 0.8383(2) 0.2267(4) 0.2769(5) 0.074(2) Uani 1 1 d . . . C5 C 0.8283(2) 0.2152(4) 0.3370(4) 0.066(2) Uani 1 1 d . . . H5 H 0.8479 0.2325 0.3788 0.079 Uiso 1 1 calc R . . C6 C 0.79132(19) 0.1796(3) 0.3393(3) 0.0513(16) Uani 1 1 d . . . C7 C 0.8783(3) 0.2670(6) 0.2777(5) 0.112(4) Uani 1 1 d . . . H7A H 0.8771 0.3172 0.2934 0.168 Uiso 1 1 calc R . . H7B H 0.8804 0.2677 0.2314 0.168 Uiso 1 1 calc R . . H7C H 0.9034 0.2422 0.3088 0.168 Uiso 1 1 calc R . . C8 C 0.7821(2) 0.1701(4) 0.4062(4) 0.0614(18) Uani 1 1 d . . . C9 C 0.7414(2) 0.2146(5) 0.4003(4) 0.089(3) Uani 1 1 d . . . H9A H 0.7456 0.2654 0.3889 0.134 Uiso 1 1 calc R . . H9B H 0.7357 0.2129 0.4440 0.134 Uiso 1 1 calc R . . H9C H 0.7171 0.1936 0.3642 0.134 Uiso 1 1 calc R . . C10 C 0.8182(3) 0.2006(5) 0.4681(4) 0.090(3) Uani 1 1 d . . . H10A H 0.8449 0.1746 0.4724 0.135 Uiso 1 1 calc R . . H10B H 0.8107 0.1936 0.5099 0.135 Uiso 1 1 calc R . . H10C H 0.8220 0.2528 0.4613 0.135 Uiso 1 1 calc R . . C11 C 0.7748(3) 0.0902(5) 0.4199(4) 0.077(2) Uani 1 1 d . . . H11A H 0.7497 0.0718 0.3836 0.115 Uiso 1 1 calc R . . H11B H 0.7700 0.0858 0.4642 0.115 Uiso 1 1 calc R . . H11C H 0.8000 0.0615 0.4207 0.115 Uiso 1 1 calc R . . C12 C 0.70215(19) 0.2057(3) 0.1036(3) 0.0416(13) Uani 1 1 d . . . C13 C 0.66164(19) 0.2050(3) 0.1104(3) 0.0412(13) Uani 1 1 d . . . C14 C 0.6346(2) 0.2659(3) 0.0858(3) 0.0443(14) Uani 1 1 d . . . C15 C 0.6496(2) 0.3204(3) 0.0535(3) 0.0528(16) Uani 1 1 d . . . H15 H 0.6314 0.3612 0.0367 0.063 Uiso 1 1 calc R . . C16 C 0.6892(2) 0.3201(3) 0.0435(3) 0.0527(16) Uani 1 1 d . . . C17 C 0.7155(2) 0.2613(3) 0.0699(3) 0.0503(15) Uani 1 1 d . . . H17 H 0.7431 0.2590 0.0649 0.060 Uiso 1 1 calc R . . C18 C 0.7030(3) 0.3826(4) 0.0067(4) 0.081(2) Uani 1 1 d . . . H18A H 0.6777 0.4075 -0.0235 0.121 Uiso 1 1 calc R . . H18B H 0.7200 0.3632 -0.0205 0.121 Uiso 1 1 calc R . . H18C H 0.7203 0.4174 0.0405 0.121 Uiso 1 1 calc R . . C19 C 0.5904(2) 0.2687(4) 0.0944(3) 0.0560(17) Uani 1 1 d . . . C20 C 0.5672(3) 0.3435(4) 0.0687(5) 0.084(3) Uani 1 1 d . . . H20A H 0.5849 0.3838 0.0941 0.126 Uiso 1 1 calc R . . H20B H 0.5394 0.3441 0.0764 0.126 Uiso 1 1 calc R . . H20C H 0.5629 0.3493 0.0198 0.126 Uiso 1 1 calc R . . C21 C 0.5619(2) 0.2070(4) 0.0550(4) 0.0604(18) Uani 1 1 d . . . H21A H 0.5572 0.2130 0.0059 0.091 Uiso 1 1 calc R . . H21B H 0.5344 0.2083 0.0634 0.091 Uiso 1 1 calc R . . H21C H 0.5759 0.1599 0.0702 0.091 Uiso 1 1 calc R . . C22 C 0.5945(2) 0.2630(4) 0.1713(3) 0.0643(19) Uani 1 1 d . . . H22A H 0.6094 0.2176 0.1903 0.096 Uiso 1 1 calc R . . H22B H 0.5659 0.2629 0.1760 0.096 Uiso 1 1 calc R . . H22C H 0.6108 0.3049 0.1961 0.096 Uiso 1 1 calc R . . C23 C 0.60530(16) 0.0146(3) 0.2698(3) 0.0331(11) Uani 1 1 d . . . C24 C 0.59682(17) 0.0855(3) 0.3030(3) 0.0351(11) Uani 1 1 d . . . C25 C 0.62806(19) 0.1376(3) 0.3256(3) 0.0449(14) Uani 1 1 d . . . H25 H 0.6552 0.1298 0.3200 0.054 Uiso 1 1 calc R . . C26 C 0.6209(2) 0.2014(3) 0.3564(3) 0.0537(16) Uani 1 1 d . . . H26 H 0.6434 0.2360 0.3725 0.064 Uiso 1 1 calc R . . C27 C 0.5819(2) 0.2154(4) 0.3639(3) 0.0584(17) Uani 1 1 d . . . H27 H 0.5771 0.2596 0.3844 0.070 Uiso 1 1 calc R . . C28 C 0.5501(2) 0.1642(4) 0.3412(3) 0.0577(17) Uani 1 1 d . . . H28 H 0.5229 0.1728 0.3461 0.069 Uiso 1 1 calc R . . C29 C 0.5574(2) 0.1001(3) 0.3110(3) 0.0454(14) Uani 1 1 d . . . H29 H 0.5349 0.0653 0.2955 0.055 Uiso 1 1 calc R . . C30 C 0.56654(16) -0.0069(3) 0.2070(3) 0.0354(12) Uani 1 1 d . . . C31 C 0.54684(19) 0.0468(3) 0.1600(3) 0.0440(14) Uani 1 1 d . . . H31 H 0.5553 0.0964 0.1693 0.053 Uiso 1 1 calc R . . C32 C 0.5149(2) 0.0291(4) 0.0996(3) 0.0521(16) Uani 1 1 d . . . H32 H 0.5016 0.0667 0.0681 0.062 Uiso 1 1 calc R . . C33 C 0.50242(19) -0.0418(4) 0.0849(3) 0.0511(16) Uani 1 1 d . . . H33 H 0.4806 -0.0539 0.0434 0.061 Uiso 1 1 calc R . . C34 C 0.5215(2) -0.0948(4) 0.1303(4) 0.0594(18) Uani 1 1 d . . . H34 H 0.5130 -0.1442 0.1203 0.071 Uiso 1 1 calc R . . C35 C 0.55336(19) -0.0778(3) 0.1914(3) 0.0502(15) Uani 1 1 d . . . H35 H 0.5662 -0.1158 0.2227 0.060 Uiso 1 1 calc R . . C36 C 0.61636(18) -0.0446(3) 0.3255(3) 0.0377(12) Uani 1 1 d . . . C37 C 0.65797(19) -0.0700(3) 0.3529(3) 0.0446(14) Uani 1 1 d . . . H37 H 0.6797 -0.0501 0.3371 0.054 Uiso 1 1 calc R . . C38 C 0.6684(2) -0.1241(4) 0.4032(3) 0.0589(18) Uani 1 1 d . . . H38 H 0.6971 -0.1410 0.4213 0.071 Uiso 1 1 calc R . . C39 C 0.6373(3) -0.1531(4) 0.4265(3) 0.0629(19) Uani 1 1 d . . . H39 H 0.6441 -0.1908 0.4599 0.075 Uiso 1 1 calc R . . C40 C 0.5963(2) -0.1267(4) 0.4009(4) 0.069(2) Uani 1 1 d . . . H40 H 0.5748 -0.1459 0.4176 0.082 Uiso 1 1 calc R . . C41 C 0.5857(2) -0.0729(4) 0.3517(3) 0.0542(17) Uani 1 1 d . . . H41 H 0.5572 -0.0549 0.3354 0.065 Uiso 1 1 calc R . . C42 C 0.6827(3) -0.0277(6) 0.0531(5) 0.108(3) Uani 1 1 d . . . H42A H 0.6907 0.0182 0.0348 0.129 Uiso 1 1 calc R . . H42B H 0.7093 -0.0545 0.0775 0.129 Uiso 1 1 calc R . . C43 C 0.6565(4) -0.0713(5) -0.0020(5) 0.105(3) Uani 1 1 d . . . H43A H 0.6690 -0.1207 -0.0012 0.126 Uiso 1 1 calc R . . H43B H 0.6536 -0.0481 -0.0466 0.126 Uiso 1 1 calc R . . C44 C 0.6138(3) -0.0761(6) 0.0091(5) 0.108(4) Uani 1 1 d . . . H44A H 0.5904 -0.0629 -0.0331 0.129 Uiso 1 1 calc R . . H44B H 0.6087 -0.1260 0.0232 0.129 Uiso 1 1 calc R . . C45 C 0.6166(3) -0.0234(7) 0.0638(5) 0.113(4) Uani 1 1 d . . . H45A H 0.6026 0.0230 0.0440 0.135 Uiso 1 1 calc R . . H45B H 0.6018 -0.0429 0.0950 0.135 Uiso 1 1 calc R . . C46 C 0.7756(3) -0.0289(4) 0.2560(5) 0.085(3) Uani 1 1 d . . . H46A H 0.7826 -0.0002 0.2988 0.102 Uiso 1 1 calc R . . H46B H 0.7882 -0.0040 0.2243 0.102 Uiso 1 1 calc R . . C47 C 0.7926(3) -0.1043(5) 0.2704(6) 0.109(4) Uani 1 1 d . . . H47A H 0.8090 -0.1175 0.2395 0.131 Uiso 1 1 calc R . . H47B H 0.8119 -0.1081 0.3183 0.131 Uiso 1 1 calc R . . C48 C 0.7575(4) -0.1510(6) 0.2597(9) 0.233(11) Uani 1 1 d . . . H48A H 0.7559 -0.1685 0.3043 0.280 Uiso 1 1 calc R . . H48B H 0.7606 -0.1940 0.2326 0.280 Uiso 1 1 calc R . . C49 C 0.7190(3) -0.1116(4) 0.2236(5) 0.078(2) Uani 1 1 d . . . H49A H 0.7075 -0.1290 0.1757 0.093 Uiso 1 1 calc R . . H49B H 0.6970 -0.1192 0.2460 0.093 Uiso 1 1 calc R . . C50 C 0.1086(13) -0.043(2) 0.367(2) 0.30(2) Uiso 0.40 1 d PD A 1 H50A H 0.0841 -0.0675 0.3331 0.365 Uiso 0.40 1 calc PR A 1 H50B H 0.1037 -0.0358 0.4117 0.365 Uiso 0.40 1 calc PR A 1 C51 C 0.1525(12) -0.073(2) 0.3717(19) 0.261(19) Uiso 0.40 1 d PD A 1 H51A H 0.1581 -0.1197 0.3965 0.313 Uiso 0.40 1 calc PR A 1 H51B H 0.1752 -0.0374 0.3956 0.313 Uiso 0.40 1 calc PR A 1 C52 C 0.151(2) -0.083(3) 0.294(3) 0.61(6) Uiso 0.40 1 d PD A 1 H52A H 0.1339 -0.1264 0.2723 0.732 Uiso 0.40 1 calc PR A 1 H52B H 0.1795 -0.0843 0.2890 0.732 Uiso 0.40 1 calc PR A 1 C53 C 0.1260(18) -0.007(3) 0.2688(17) 0.37(3) Uiso 0.40 1 d PD A 1 H53A H 0.1417 0.0251 0.2468 0.440 Uiso 0.40 1 calc PR A 1 H53B H 0.0965 -0.0152 0.2376 0.440 Uiso 0.40 1 calc PR A 1 C54 C 0.1269(13) 0.0217(17) 0.341(2) 0.253(17) Uiso 0.40 1 d PD A 1 H54A H 0.1564 0.0328 0.3707 0.304 Uiso 0.40 1 calc PR A 1 H54B H 0.1088 0.0657 0.3370 0.304 Uiso 0.40 1 calc PR A 1 O6A O 0.1086(13) -0.043(2) 0.367(2) 0.30(2) Uiso 0.10 1 d P B 2 O6B O 0.1525(12) -0.073(2) 0.3717(19) 0.261(19) Uiso 0.10 1 d P B 2 O6C O 0.151(2) -0.083(3) 0.294(3) 0.61(6) Uiso 0.10 1 d P B 2 O6D O 0.1260(18) -0.007(3) 0.2688(17) 0.37(3) Uiso 0.10 1 d P B 2 O6E O 0.1269(13) 0.0217(17) 0.341(2) 0.253(17) Uiso 0.10 1 d P B 2 C55 C 0.0000 0.8453(18) 0.2500 0.203(18) Uiso 0.40 2 d SPD . 1 H55A H -0.0257 0.8136 0.2385 0.244 Uiso 0.20 1 calc PR . 1 H55B H 0.0257 0.8136 0.2615 0.244 Uiso 0.20 1 calc PR . 1 C56 C -0.0018(12) 0.8944(17) 0.1896(7) 0.241(16) Uiso 0.40 1 d PD C 1 H56A H -0.0305 0.8927 0.1546 0.289 Uiso 0.40 1 calc PR C 1 H56B H 0.0197 0.8789 0.1682 0.289 Uiso 0.40 1 calc PR C 1 C57 C 0.008(3) 0.9717(19) 0.219(3) 0.60(6) Uiso 0.40 1 d PD . 1 H57A H 0.0393 0.9816 0.2339 0.723 Uiso 0.40 1 calc PR . 1 H57B H -0.0069 1.0090 0.1853 0.723 Uiso 0.40 1 calc PR . 1 O7A O 0.0000 0.8453(18) 0.2500 0.203(18) Uiso 0.10 2 d SP . 2 O7B O -0.0018(12) 0.8944(17) 0.1896(7) 0.241(16) Uiso 0.10 1 d P D 2 O7C O 0.008(3) 0.9717(19) 0.219(3) 0.60(6) Uiso 0.10 1 d P . 2 C58 C 0.0574(12) 0.2015(16) 0.0101(17) 0.26(2) Uiso 0.50 1 d PD . . H58A H 0.0802 0.2259 0.0462 0.387 Uiso 0.50 1 calc PR . . H58B H 0.0295 0.2195 0.0106 0.387 Uiso 0.50 1 calc PR . . H58C H 0.0607 0.2119 -0.0345 0.387 Uiso 0.50 1 calc PR . . C59 C 0.0601(12) 0.1184(16) 0.0228(13) 0.225(16) Uiso 0.50 1 d PD . . H59A H 0.0390 0.0932 -0.0161 0.270 Uiso 0.50 1 calc PR . . H59B H 0.0890 0.1007 0.0258 0.270 Uiso 0.50 1 calc PR . . C60 C 0.0514(8) 0.1003(15) 0.0870(15) 0.186(13) Uiso 0.50 1 d PD . . H60A H 0.0229 0.0771 0.0758 0.223 Uiso 0.50 1 calc PR . . H60B H 0.0509 0.1459 0.1126 0.223 Uiso 0.50 1 calc PR . . C61 C 0.0855(10) 0.0481(17) 0.1327(14) 0.207(16) Uiso 0.50 1 d PD . . H61A H 0.0725 0.0033 0.1443 0.248 Uiso 0.50 1 calc PR . . H61B H 0.1033 0.0724 0.1753 0.248 Uiso 0.50 1 calc PR . . C62 C 0.1115(8) 0.0319(16) 0.0842(15) 0.174(12) Uiso 0.50 1 d PD . . H62A H 0.0948 -0.0002 0.0471 0.260 Uiso 0.50 1 calc PR . . H62B H 0.1383 0.0076 0.1098 0.260 Uiso 0.50 1 calc PR . . H62C H 0.1177 0.0778 0.0648 0.260 Uiso 0.50 1 calc PR . . C63 C 0.0000 0.1832(19) 0.2500 0.183(18) Uiso 0.50 2 d SPD . . H63A H -0.0210 0.1509 0.2608 0.220 Uiso 0.25 1 calc PR . . H63B H 0.0210 0.1509 0.2392 0.220 Uiso 0.25 1 calc PR . . C64 C 0.0230(9) 0.2209(15) 0.3129(7) 0.210(15) Uiso 0.50 1 d PD . . H64A H 0.0026 0.2340 0.3372 0.253 Uiso 0.50 1 calc PR . . H64B H 0.0350 0.2668 0.3015 0.253 Uiso 0.50 1 calc PR . . C65 C 0.0590(7) 0.1757(16) 0.3604(11) 0.185(13) Uiso 0.50 1 d PD . . H65A H 0.0477 0.1288 0.3697 0.277 Uiso 0.50 1 calc PR . . H65B H 0.0718 0.2021 0.4034 0.277 Uiso 0.50 1 calc PR . . H65C H 0.0809 0.1669 0.3385 0.277 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 Lu 0.03549(13) 0.03376(12) 0.03184(12) -0.00109(10) 0.01593(9) -0.00223(10) S 0.0493(9) 0.0440(8) 0.0536(9) 0.0096(7) 0.0290(7) 0.0029(7) O1 0.038(2) 0.047(2) 0.047(2) -0.0078(18) 0.0172(18) -0.0109(18) O2 0.044(2) 0.045(2) 0.047(2) 0.0097(18) 0.0209(19) 0.0030(18) O3 0.053(3) 0.061(3) 0.036(2) -0.0131(19) 0.0164(19) 0.000(2) O4 0.046(2) 0.037(2) 0.066(3) 0.003(2) 0.021(2) 0.0050(18) O5 0.035(2) 0.044(2) 0.037(2) -0.0014(17) 0.0176(16) -0.0057(17) C1 0.037(3) 0.036(3) 0.059(4) 0.002(3) 0.014(3) -0.001(2) C2 0.036(3) 0.046(3) 0.064(4) 0.012(3) 0.017(3) 0.000(3) C3 0.043(4) 0.067(5) 0.084(5) 0.033(4) 0.021(4) 0.002(3) C4 0.042(4) 0.061(5) 0.110(7) 0.033(4) 0.011(4) -0.013(3) C5 0.045(4) 0.051(4) 0.088(6) 0.009(4) 0.003(4) -0.009(3) C6 0.043(3) 0.034(3) 0.068(4) 0.001(3) 0.006(3) 0.000(3) C7 0.053(5) 0.127(8) 0.136(9) 0.044(7) 0.004(5) -0.038(5) C8 0.055(4) 0.065(4) 0.058(4) -0.021(4) 0.009(3) -0.019(3) C9 0.063(5) 0.113(7) 0.091(6) -0.049(6) 0.023(4) -0.011(5) C10 0.076(6) 0.096(7) 0.084(6) -0.033(5) 0.006(5) -0.015(5) C11 0.096(6) 0.083(5) 0.048(4) -0.008(4) 0.019(4) -0.023(5) C12 0.053(4) 0.036(3) 0.039(3) 0.005(2) 0.021(3) -0.003(3) C13 0.052(4) 0.040(3) 0.034(3) 0.004(2) 0.018(3) 0.003(3) C14 0.059(4) 0.041(3) 0.035(3) -0.001(2) 0.018(3) 0.001(3) C15 0.069(4) 0.041(3) 0.047(3) 0.003(3) 0.017(3) 0.008(3) C16 0.072(4) 0.040(3) 0.047(3) 0.009(3) 0.020(3) -0.007(3) C17 0.066(4) 0.046(4) 0.047(3) 0.000(3) 0.029(3) -0.006(3) C18 0.100(6) 0.063(5) 0.085(6) 0.028(4) 0.037(5) -0.002(4) C19 0.073(5) 0.050(4) 0.053(4) 0.008(3) 0.031(4) 0.020(3) C20 0.088(6) 0.071(5) 0.104(7) 0.020(5) 0.045(5) 0.039(5) C21 0.053(4) 0.066(5) 0.060(4) 0.003(4) 0.015(3) 0.010(3) C22 0.075(5) 0.077(5) 0.049(4) -0.002(3) 0.031(4) 0.012(4) C23 0.033(3) 0.036(3) 0.033(3) 0.004(2) 0.015(2) -0.003(2) C24 0.036(3) 0.043(3) 0.026(2) 0.002(2) 0.010(2) -0.001(2) C25 0.048(3) 0.052(4) 0.035(3) -0.003(3) 0.014(3) -0.001(3) C26 0.068(5) 0.047(4) 0.046(4) -0.010(3) 0.018(3) -0.011(3) C27 0.079(5) 0.054(4) 0.047(4) -0.004(3) 0.026(4) 0.009(4) C28 0.061(4) 0.065(4) 0.054(4) -0.006(3) 0.028(3) 0.013(4) C29 0.050(4) 0.050(4) 0.038(3) -0.003(3) 0.016(3) -0.001(3) C30 0.029(3) 0.051(3) 0.030(3) 0.003(2) 0.015(2) 0.002(2) C31 0.049(3) 0.051(4) 0.031(3) -0.003(2) 0.011(2) -0.005(3) C32 0.048(4) 0.070(4) 0.036(3) 0.007(3) 0.011(3) 0.001(3) C33 0.036(3) 0.080(5) 0.038(3) -0.013(3) 0.012(3) -0.007(3) C34 0.047(4) 0.055(4) 0.071(5) -0.022(4) 0.012(3) -0.011(3) C35 0.037(3) 0.047(4) 0.061(4) -0.005(3) 0.009(3) 0.001(3) C36 0.040(3) 0.039(3) 0.034(3) 0.002(2) 0.014(2) 0.000(2) C37 0.042(3) 0.045(3) 0.045(3) 0.006(3) 0.012(3) 0.004(3) C38 0.054(4) 0.060(4) 0.053(4) 0.011(3) 0.004(3) 0.015(3) C39 0.086(5) 0.053(4) 0.051(4) 0.015(3) 0.023(4) 0.008(4) C40 0.073(5) 0.076(5) 0.068(5) 0.034(4) 0.038(4) 0.011(4) C41 0.048(4) 0.059(4) 0.059(4) 0.026(3) 0.022(3) 0.009(3) C42 0.112(8) 0.148(9) 0.081(6) -0.055(6) 0.056(6) -0.026(7) C43 0.152(10) 0.099(7) 0.063(5) -0.027(5) 0.034(6) 0.012(7) C44 0.095(7) 0.134(9) 0.080(6) -0.061(6) 0.008(6) -0.006(6) C45 0.065(6) 0.180(11) 0.088(7) -0.077(7) 0.017(5) -0.026(6) C46 0.065(5) 0.058(5) 0.126(8) 0.011(5) 0.021(5) 0.011(4) C47 0.086(7) 0.087(7) 0.139(9) 0.028(7) 0.016(7) 0.041(6) C48 0.153(12) 0.047(6) 0.35(2) 0.014(9) -0.129(14) 0.005(7) C49 0.094(6) 0.037(4) 0.112(7) -0.003(4) 0.046(5) -0.005(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 Lu O5 2.016(3) . ? Lu O2 2.105(4) . ? Lu O1 2.116(4) . ? Lu O3 2.303(4) . ? Lu O4 2.319(4) . ? Lu S 2.8961(14) . ? S C2 1.776(7) . ? S C12 1.793(6) . ? O1 C1 1.324(6) . ? O2 C13 1.334(6) . ? O3 C45 1.386(9) . ? O3 C42 1.448(9) . ? O4 C49 1.429(8) . ? O4 C46 1.442(8) . ? O5 C23 1.394(6) . ? C1 C2 1.399(8) . ? C1 C6 1.422(8) . ? C2 C3 1.402(8) . ? C3 C4 1.376(11) . ? C3 H3 0.9500 . ? C4 C5 1.398(12) . ? C4 C7 1.507(10) . ? C5 C6 1.399(9) . ? C5 H5 0.9500 . ? C6 C8 1.517(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C11 1.523(10) . ? C8 C9 1.541(10) . ? C8 C10 1.543(9) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C17 1.382(8) . ? C12 C13 1.389(8) . ? C13 C14 1.414(8) . ? C14 C15 1.377(8) . ? C14 C19 1.529(9) . ? C15 C16 1.387(9) . ? C15 H15 0.9500 . ? C16 C17 1.381(9) . ? C16 C18 1.522(9) . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C21 1.525(10) . ? C19 C22 1.551(9) . ? C19 C20 1.573(9) . ? 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 C24 1.533(7) . ? C23 C36 1.534(7) . ? C23 C30 1.549(7) . ? C24 C25 1.371(8) . ? C24 C29 1.391(8) . ? C25 C26 1.385(8) . ? C25 H25 0.9500 . ? C26 C27 1.368(9) . ? C26 H26 0.9500 . ? C27 C28 1.372(10) . ? C27 H27 0.9500 . ? C28 C29 1.385(8) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C35 1.374(8) . ? C30 C31 1.386(8) . ? C31 C32 1.387(8) . ? C31 H31 0.9500 . ? C32 C33 1.366(9) . ? C32 H32 0.9500 . ? C33 C34 1.353(10) . ? C33 H33 0.9500 . ? C34 C35 1.391(9) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.386(8) . ? C36 C41 1.393(8) . ? C37 C38 1.395(8) . ? C37 H37 0.9500 . ? C38 C39 1.374(10) . ? C38 H38 0.9500 . ? C39 C40 1.374(10) . ? C39 H39 0.9500 . ? C40 C41 1.376(8) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.429(12) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.502(14) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.464(11) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.482(11) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.400(15) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.441(12) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C54 1.508(19) . ? C50 C51 1.521(19) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.592(19) . ? C51 C54 1.93(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.607(19) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.574(19) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.523(13) 2 ? C55 C56 1.523(13) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.534(19) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C57 1.53(2) 2 ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.540(18) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.481(18) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.544(17) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.542(18) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.448(13) . ? C63 C64 1.448(13) 2 ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.520(17) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Lu O2 103.01(15) . . ? O5 Lu O1 104.02(14) . . ? O2 Lu O1 97.77(16) . . ? O5 Lu O3 100.66(15) . . ? O2 Lu O3 88.58(15) . . ? O1 Lu O3 152.34(15) . . ? O5 Lu O4 100.14(15) . . ? O2 Lu O4 154.92(15) . . ? O1 Lu O4 85.76(15) . . ? O3 Lu O4 77.73(15) . . ? O5 Lu S 171.34(11) . . ? O2 Lu S 71.33(11) . . ? O1 Lu S 70.92(11) . . ? O3 Lu S 85.95(11) . . ? O4 Lu S 86.66(11) . . ? C2 S C12 103.8(3) . . ? C2 S Lu 94.4(2) . . ? C12 S Lu 94.09(19) . . ? C1 O1 Lu 133.7(4) . . ? C13 O2 Lu 132.8(4) . . ? C45 O3 C42 106.1(6) . . ? C45 O3 Lu 122.1(4) . . ? C42 O3 Lu 128.6(5) . . ? C49 O4 C46 108.3(5) . . ? C49 O4 Lu 124.7(4) . . ? C46 O4 Lu 126.3(4) . . ? C23 O5 Lu 166.4(3) . . ? O1 C1 C2 120.1(5) . . ? O1 C1 C6 120.3(6) . . ? C2 C1 C6 119.5(6) . . ? C1 C2 C3 121.3(6) . . ? C1 C2 S 120.0(4) . . ? C3 C2 S 118.8(5) . . ? C4 C3 C2 120.4(7) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 118.0(6) . . ? C3 C4 C7 120.7(8) . . ? C5 C4 C7 121.3(8) . . ? C4 C5 C6 124.0(7) . . ? C4 C5 H5 118.0 . . ? C6 C5 H5 118.0 . . ? C5 C6 C1 116.8(7) . . ? C5 C6 C8 121.2(6) . . ? C1 C6 C8 122.0(6) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 C11 111.6(6) . . ? C6 C8 C9 107.1(6) . . ? C11 C8 C9 109.6(7) . . ? C6 C8 C10 112.5(6) . . ? C11 C8 C10 108.6(7) . . ? C9 C8 C10 107.3(6) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 122.2(6) . . ? C17 C12 S 118.4(5) . . ? C13 C12 S 119.4(4) . . ? O2 C13 C12 121.0(5) . . ? O2 C13 C14 120.8(5) . . ? C12 C13 C14 118.2(5) . . ? C15 C14 C13 117.4(6) . . ? C15 C14 C19 122.5(6) . . ? C13 C14 C19 120.0(5) . . ? C14 C15 C16 124.9(6) . . ? C14 C15 H15 117.5 . . ? C16 C15 H15 117.5 . . ? C17 C16 C15 116.6(6) . . ? C17 C16 C18 122.0(6) . . ? C15 C16 C18 121.4(6) . . ? C16 C17 C12 120.5(6) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C19 C14 111.1(5) . . ? C21 C19 C22 109.4(6) . . ? C14 C19 C22 110.2(6) . . ? C21 C19 C20 108.4(6) . . ? C14 C19 C20 111.6(6) . . ? C22 C19 C20 106.0(6) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 C24 110.0(4) . . ? O5 C23 C36 109.9(4) . . ? C24 C23 C36 107.2(4) . . ? O5 C23 C30 105.9(4) . . ? C24 C23 C30 111.5(4) . . ? C36 C23 C30 112.3(4) . . ? C25 C24 C29 117.2(5) . . ? C25 C24 C23 120.9(5) . . ? C29 C24 C23 121.9(5) . . ? C24 C25 C26 121.4(6) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C27 C26 C25 121.0(6) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 118.6(6) . . ? C26 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? C27 C28 C29 120.4(6) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C24 121.4(6) . . ? C28 C29 H29 119.3 . . ? C24 C29 H29 119.3 . . ? C35 C30 C31 117.6(5) . . ? C35 C30 C23 123.3(5) . . ? C31 C30 C23 118.7(5) . . ? C30 C31 C32 120.8(6) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? C33 C32 C31 120.6(6) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C32 119.1(6) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C35 121.0(6) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C30 C35 C34 120.8(6) . . ? C30 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C37 C36 C41 117.8(5) . . ? C37 C36 C23 120.4(5) . . ? C41 C36 C23 121.7(5) . . ? C36 C37 C38 121.1(6) . . ? C36 C37 H37 119.5 . . ? C38 C37 H37 119.5 . . ? C39 C38 C37 120.0(6) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C40 C39 C38 119.1(6) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C39 C40 C41 121.3(7) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C40 C41 C36 120.6(6) . . ? C40 C41 H41 119.7 . . ? C36 C41 H41 119.7 . . ? C43 C42 O3 109.4(8) . . ? C43 C42 H42A 109.8 . . ? O3 C42 H42A 109.8 . . ? C43 C42 H42B 109.8 . . ? O3 C42 H42B 109.8 . . ? H42A C42 H42B 108.2 . . ? C42 C43 C44 105.5(7) . . ? C42 C43 H43A 110.6 . . ? C44 C43 H43A 110.6 . . ? C42 C43 H43B 110.6 . . ? C44 C43 H43B 110.6 . . ? H43A C43 H43B 108.8 . . ? C45 C44 C43 104.6(8) . . ? C45 C44 H44A 110.8 . . ? C43 C44 H44A 110.8 . . ? C45 C44 H44B 110.8 . . ? C43 C44 H44B 110.8 . . ? H44A C44 H44B 108.9 . . ? O3 C45 C44 108.6(8) . . ? O3 C45 H45A 110.0 . . ? C44 C45 H45A 110.0 . . ? O3 C45 H45B 110.0 . . ? C44 C45 H45B 110.0 . . ? H45A C45 H45B 108.3 . . ? O4 C46 C47 106.3(7) . . ? O4 C46 H46A 110.5 . . ? C47 C46 H46A 110.5 . . ? O4 C46 H46B 110.5 . . ? C47 C46 H46B 110.5 . . ? H46A C46 H46B 108.7 . . ? C48 C47 C46 107.2(8) . . ? C48 C47 H47A 110.3 . . ? C46 C47 H47A 110.3 . . ? C48 C47 H47B 110.3 . . ? C46 C47 H47B 110.3 . . ? H47A C47 H47B 108.5 . . ? C47 C48 C49 108.8(9) . . ? C47 C48 H48A 109.9 . . ? C49 C48 H48A 109.9 . . ? C47 C48 H48B 109.9 . . ? C49 C48 H48B 109.9 . . ? H48A C48 H48B 108.3 . . ? O4 C49 C48 107.5(7) . . ? O4 C49 H49A 110.2 . . ? C48 C49 H49A 110.2 . . ? O4 C49 H49B 110.2 . . ? C48 C49 H49B 110.2 . . ? H49A C49 H49B 108.5 . . ? C54 C50 C51 79(2) . . ? C54 C50 H50A 115.3 . . ? C51 C50 H50A 115.4 . . ? C54 C50 H50B 115.3 . . ? C51 C50 H50B 115.4 . . ? H50A C50 H50B 112.4 . . ? C50 C51 C52 104.9(16) . . ? C50 C51 C54 50.0(12) . . ? C52 C51 C54 84.8(12) . . ? C50 C51 H51A 110.7 . . ? C52 C51 H51A 110.8 . . ? C54 C51 H51A 159.2 . . ? C50 C51 H51B 110.8 . . ? C52 C51 H51B 110.8 . . ? C54 C51 H51B 76.5 . . ? H51A C51 H51B 108.8 . . ? C51 C52 C53 94.3(12) . . ? C51 C52 H52A 112.9 . . ? C53 C52 H52A 112.9 . . ? C51 C52 H52B 112.8 . . ? C53 C52 H52B 112.9 . . ? H52A C52 H52B 110.3 . . ? C54 C53 C52 97.4(13) . . ? C54 C53 H53A 112.3 . . ? C52 C53 H53A 112.3 . . ? C54 C53 H53B 112.2 . . ? C52 C53 H53B 112.2 . . ? H53A C53 H53B 109.9 . . ? C50 C54 C53 101(3) . . ? C50 C54 C51 50.6(12) . . ? C53 C54 C51 83.2(12) . . ? C50 C54 H54A 111.6 . . ? C53 C54 H54A 111.6 . . ? C51 C54 H54A 75.0 . . ? C50 C54 H54B 111.7 . . ? C53 C54 H54B 111.6 . . ? C51 C54 H54B 160.1 . . ? H54A C54 H54B 109.4 . . ? C56 C55 C56 107.7(16) 2 . ? C56 C55 H55A 110.2 2 . ? C56 C55 H55A 110.2 . . ? C56 C55 H55B 110.2 2 . ? C56 C55 H55B 110.2 . . ? H55A C55 H55B 108.5 . . ? C55 C56 C57 105.6(14) . . ? C55 C56 H56A 110.6 . . ? C57 C56 H56A 110.6 . . ? C55 C56 H56B 110.6 . . ? C57 C56 H56B 110.6 . . ? H56A C56 H56B 108.7 . . ? C57 C57 C56 104(2) 2 . ? C57 C57 H57A 110.9 2 . ? C56 C57 H57A 110.9 . . ? C57 C57 H57B 110.9 2 . ? C56 C57 H57B 110.9 . . ? H57A C57 H57B 108.9 . . ? C59 C58 H58A 109.5 . . ? C59 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C59 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 C58 110.8(18) . . ? C60 C59 H59A 109.5 . . ? C58 C59 H59A 109.5 . . ? C60 C59 H59B 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 108.1 . . ? C59 C60 C61 111.7(15) . . ? C59 C60 H60A 109.2 . . ? C61 C60 H60A 109.3 . . ? C59 C60 H60B 109.3 . . ? C61 C60 H60B 109.3 . . ? H60A C60 H60B 107.9 . . ? C60 C61 C62 99.9(12) . . ? C60 C61 H61A 111.7 . . ? C62 C61 H61A 111.8 . . ? C60 C61 H61B 111.8 . . ? C62 C61 H61B 111.9 . . ? H61A C61 H61B 109.5 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.4 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 C64 123(2) . 2 ? C64 C63 H63A 106.5 . . ? C64 C63 H63A 106.5 2 . ? C64 C63 H63B 106.5 . . ? C64 C63 H63B 106.5 2 . ? H63A C63 H63B 106.5 . . ? C63 C64 C65 113.2(16) . . ? C63 C64 H64A 108.9 . . ? C65 C64 H64A 108.9 . . ? C63 C64 H64B 108.9 . . ? C65 C64 H64B 108.9 . . ? H64A C64 H64B 107.8 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Lu S C2 61.0(8) . . . . ? O2 Lu S C2 111.2(2) . . . . ? O1 Lu S C2 5.7(2) . . . . ? O3 Lu S C2 -158.9(2) . . . . ? O4 Lu S C2 -81.0(2) . . . . ? O5 Lu S C12 -43.2(8) . . . . ? O2 Lu S C12 7.0(2) . . . . ? O1 Lu S C12 -98.5(2) . . . . ? O3 Lu S C12 96.9(2) . . . . ? O4 Lu S C12 174.8(2) . . . . ? O5 Lu O1 C1 177.8(5) . . . . ? O2 Lu O1 C1 -76.7(5) . . . . ? O3 Lu O1 C1 25.2(7) . . . . ? O4 Lu O1 C1 78.4(5) . . . . ? S Lu O1 C1 -9.6(5) . . . . ? O5 Lu O2 C13 160.9(5) . . . . ? O1 Lu O2 C13 54.5(5) . . . . ? O3 Lu O2 C13 -98.5(5) . . . . ? O4 Lu O2 C13 -42.2(7) . . . . ? S Lu O2 C13 -12.3(4) . . . . ? O5 Lu O3 C45 41.7(7) . . . . ? O2 Lu O3 C45 -61.2(7) . . . . ? O1 Lu O3 C45 -165.4(7) . . . . ? O4 Lu O3 C45 139.9(7) . . . . ? S Lu O3 C45 -132.6(7) . . . . ? O5 Lu O3 C42 -161.4(7) . . . . ? O2 Lu O3 C42 95.6(7) . . . . ? O1 Lu O3 C42 -8.5(9) . . . . ? O4 Lu O3 C42 -63.2(7) . . . . ? S Lu O3 C42 24.3(7) . . . . ? O5 Lu O4 C49 42.1(5) . . . . ? O2 Lu O4 C49 -115.1(6) . . . . ? O1 Lu O4 C49 145.6(5) . . . . ? O3 Lu O4 C49 -56.7(5) . . . . ? S Lu O4 C49 -143.3(5) . . . . ? O5 Lu O4 C46 -127.5(6) . . . . ? O2 Lu O4 C46 75.3(7) . . . . ? O1 Lu O4 C46 -24.0(6) . . . . ? O3 Lu O4 C46 133.7(6) . . . . ? S Lu O4 C46 47.1(6) . . . . ? O2 Lu O5 C23 -2.8(14) . . . . ? O1 Lu O5 C23 98.8(14) . . . . ? O3 Lu O5 C23 -93.8(14) . . . . ? O4 Lu O5 C23 -173.1(14) . . . . ? S Lu O5 C23 45.5(18) . . . . ? Lu O1 C1 C2 9.9(8) . . . . ? Lu O1 C1 C6 -169.8(4) . . . . ? O1 C1 C2 C3 179.7(6) . . . . ? C6 C1 C2 C3 -0.6(9) . . . . ? O1 C1 C2 S -0.7(8) . . . . ? C6 C1 C2 S 179.0(4) . . . . ? C12 S C2 C1 90.8(5) . . . . ? Lu S C2 C1 -4.5(5) . . . . ? C12 S C2 C3 -89.6(5) . . . . ? Lu S C2 C3 175.1(5) . . . . ? C1 C2 C3 C4 0.4(10) . . . . ? S C2 C3 C4 -179.2(6) . . . . ? C2 C3 C4 C5 0.3(11) . . . . ? C2 C3 C4 C7 -179.2(7) . . . . ? C3 C4 C5 C6 -0.8(11) . . . . ? C7 C4 C5 C6 178.6(7) . . . . ? C4 C5 C6 C1 0.6(10) . . . . ? C4 C5 C6 C8 -178.8(7) . . . . ? O1 C1 C6 C5 179.8(5) . . . . ? C2 C1 C6 C5 0.1(9) . . . . ? O1 C1 C6 C8 -0.8(9) . . . . ? C2 C1 C6 C8 179.5(6) . . . . ? C5 C6 C8 C11 -124.8(7) . . . . ? C1 C6 C8 C11 55.8(9) . . . . ? C5 C6 C8 C9 115.2(7) . . . . ? C1 C6 C8 C9 -64.1(8) . . . . ? C5 C6 C8 C10 -2.4(10) . . . . ? C1 C6 C8 C10 178.2(6) . . . . ? C2 S C12 C17 81.7(5) . . . . ? Lu S C12 C17 177.3(5) . . . . ? C2 S C12 C13 -100.5(5) . . . . ? Lu S C12 C13 -4.9(5) . . . . ? Lu O2 C13 C12 13.4(8) . . . . ? Lu O2 C13 C14 -166.5(4) . . . . ? C17 C12 C13 O2 175.7(5) . . . . ? S C12 C13 O2 -2.0(8) . . . . ? C17 C12 C13 C14 -4.4(9) . . . . ? S C12 C13 C14 178.0(4) . . . . ? O2 C13 C14 C15 -176.7(5) . . . . ? C12 C13 C14 C15 3.3(8) . . . . ? O2 C13 C14 C19 2.1(8) . . . . ? C12 C13 C14 C19 -177.9(5) . . . . ? C13 C14 C15 C16 -0.3(9) . . . . ? C19 C14 C15 C16 -179.1(6) . . . . ? C14 C15 C16 C17 -1.7(10) . . . . ? C14 C15 C16 C18 179.7(6) . . . . ? C15 C16 C17 C12 0.8(9) . . . . ? C18 C16 C17 C12 179.4(6) . . . . ? C13 C12 C17 C16 2.3(9) . . . . ? S C12 C17 C16 180.0(5) . . . . ? C15 C14 C19 C21 115.5(6) . . . . ? C13 C14 C19 C21 -63.3(7) . . . . ? C15 C14 C19 C22 -123.1(6) . . . . ? C13 C14 C19 C22 58.1(8) . . . . ? C15 C14 C19 C20 -5.7(9) . . . . ? C13 C14 C19 C20 175.6(6) . . . . ? Lu O5 C23 C24 -53.0(15) . . . . ? Lu O5 C23 C36 -170.9(12) . . . . ? Lu O5 C23 C30 67.6(15) . . . . ? O5 C23 C24 C25 -21.6(7) . . . . ? C36 C23 C24 C25 97.9(6) . . . . ? C30 C23 C24 C25 -138.7(5) . . . . ? O5 C23 C24 C29 157.9(5) . . . . ? C36 C23 C24 C29 -82.6(6) . . . . ? C30 C23 C24 C29 40.7(7) . . . . ? C29 C24 C25 C26 1.3(8) . . . . ? C23 C24 C25 C26 -179.2(5) . . . . ? C24 C25 C26 C27 -1.5(9) . . . . ? C25 C26 C27 C28 1.0(10) . . . . ? C26 C27 C28 C29 -0.3(10) . . . . ? C27 C28 C29 C24 0.1(10) . . . . ? C25 C24 C29 C28 -0.6(8) . . . . ? C23 C24 C29 C28 179.9(5) . . . . ? O5 C23 C30 C35 98.4(6) . . . . ? C24 C23 C30 C35 -142.0(5) . . . . ? C36 C23 C30 C35 -21.6(7) . . . . ? O5 C23 C30 C31 -74.4(6) . . . . ? C24 C23 C30 C31 45.2(6) . . . . ? C36 C23 C30 C31 165.6(5) . . . . ? C35 C30 C31 C32 0.2(8) . . . . ? C23 C30 C31 C32 173.4(5) . . . . ? C30 C31 C32 C33 -0.4(9) . . . . ? C31 C32 C33 C34 0.2(10) . . . . ? C32 C33 C34 C35 0.2(10) . . . . ? C31 C30 C35 C34 0.2(9) . . . . ? C23 C30 C35 C34 -172.6(5) . . . . ? C33 C34 C35 C30 -0.5(10) . . . . ? O5 C23 C36 C37 11.8(7) . . . . ? C24 C23 C36 C37 -107.7(6) . . . . ? C30 C23 C36 C37 129.4(5) . . . . ? O5 C23 C36 C41 -170.3(5) . . . . ? C24 C23 C36 C41 70.2(7) . . . . ? C30 C23 C36 C41 -52.7(7) . . . . ? C41 C36 C37 C38 2.5(9) . . . . ? C23 C36 C37 C38 -179.6(5) . . . . ? C36 C37 C38 C39 -0.2(10) . . . . ? C37 C38 C39 C40 -1.6(11) . . . . ? C38 C39 C40 C41 1.2(12) . . . . ? C39 C40 C41 C36 1.2(12) . . . . ? C37 C36 C41 C40 -2.9(10) . . . . ? C23 C36 C41 C40 179.1(6) . . . . ? C45 O3 C42 C43 -18.4(12) . . . . ? Lu O3 C42 C43 -178.1(6) . . . . ? O3 C42 C43 C44 4.8(13) . . . . ? C42 C43 C44 C45 9.7(13) . . . . ? C42 O3 C45 C44 24.8(12) . . . . ? Lu O3 C45 C44 -173.9(7) . . . . ? C43 C44 C45 O3 -21.6(13) . . . . ? C49 O4 C46 C47 2.7(10) . . . . ? Lu O4 C46 C47 173.7(6) . . . . ? O4 C46 C47 C48 -10.2(14) . . . . ? C46 C47 C48 C49 13.8(18) . . . . ? C46 O4 C49 C48 5.5(13) . . . . ? Lu O4 C49 C48 -165.7(10) . . . . ? C47 C48 C49 O4 -12.2(18) . . . . ? C54 C50 C51 C52 -70(3) . . . . ? C50 C51 C52 C53 42(5) . . . . ? C54 C51 C52 C53 -4(4) . . . . ? C51 C52 C53 C54 5(5) . . . . ? C51 C50 C54 C53 72(3) . . . . ? C52 C53 C54 C50 -52(5) . . . . ? C52 C53 C54 C51 -4(4) . . . . ? C52 C51 C54 C50 114(3) . . . . ? C50 C51 C54 C53 -110(4) . . . . ? C52 C51 C54 C53 4(4) . . . . ? C56 C55 C56 C57 11(3) 2 . . . ? C55 C56 C57 C57 -29(8) . . . 2 ? C58 C59 C60 C61 -131(3) . . . . ? C59 C60 C61 C62 -6(4) . . . . ? C64 C63 C64 C65 -155(3) 2 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.116 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.129 #===END #============================================================================== data_mk6 _database_code_depnum_ccdc_archive 'CCDC 643868' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tris(tetrahydrofurane)-thiobis(6-tert-butyl-4-methylphenolato)- diphenylmethoxy-lutetium(III) ; _chemical_name_common ; Tris(tetrahydrofurane)-thiobis(6-tert-butyl-4- methylphenolato)-diphenylmethoxy-lutetium(iii) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H63 Lu O6 S' _chemical_formula_weight 931.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.710(3) _cell_length_b 13.582(3) _cell_length_c 22.910(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.290(4) _cell_angle_gamma 90.00 _cell_volume 4346.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 828 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 19.41 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 2.366 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5571 _exptl_absorpt_correction_T_max 0.8333 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57519 _diffrn_reflns_av_R_equivalents 0.0947 _diffrn_reflns_av_sigmaI/netI 0.0760 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.38 _reflns_number_total 10862 _reflns_number_gt 7876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10862 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Lu1 Lu 0.558999(12) 0.231233(12) 0.819927(8) 0.02458(6) Uani 1 1 d . . . S1 S 0.46296(7) 0.04437(7) 0.79966(5) 0.0251(2) Uani 1 1 d . . . O1 O 0.64689(19) 0.12549(19) 0.88255(13) 0.0282(6) Uani 1 1 d . . . O2 O 0.5691(2) 0.16132(19) 0.73669(13) 0.0281(6) Uani 1 1 d . . . O3 O 0.4511(2) 0.3268(2) 0.77734(13) 0.0337(7) Uani 1 1 d . . . O4 O 0.6133(2) 0.3503(2) 0.90010(14) 0.0387(8) Uani 1 1 d . . . O5 O 0.4616(2) 0.2147(2) 0.88839(13) 0.0313(7) Uani 1 1 d . . . O6 O 0.6898(2) 0.3139(2) 0.80461(15) 0.0381(7) Uani 1 1 d . . . C1 C 0.6428(3) 0.0282(3) 0.88544(19) 0.0261(9) Uani 1 1 d . . . C2 C 0.7167(3) -0.0287(3) 0.92712(19) 0.0268(9) Uani 1 1 d . . . C3 C 0.8047(3) 0.0208(3) 0.9708(2) 0.0334(10) Uani 1 1 d . . . C4 C 0.8768(3) -0.0522(3) 1.0104(2) 0.0395(11) Uani 1 1 d . . . H4A H 0.9318 -0.0162 1.0374 0.059 Uiso 1 1 calc R . . H4B H 0.8987 -0.0966 0.9839 0.059 Uiso 1 1 calc R . . H4C H 0.8465 -0.0905 1.0354 0.059 Uiso 1 1 calc R . . C5 C 0.8557(3) 0.0819(4) 0.9345(2) 0.0458(13) Uani 1 1 d . . . H5A H 0.9124 0.1132 0.9630 0.069 Uiso 1 1 calc R . . H5B H 0.8122 0.1327 0.9109 0.069 Uiso 1 1 calc R . . H5C H 0.8754 0.0389 0.9062 0.069 Uiso 1 1 calc R . . C6 C 0.7728(3) 0.0871(3) 1.0151(2) 0.0388(11) Uani 1 1 d . . . H6A H 0.8289 0.1193 1.0435 0.058 Uiso 1 1 calc R . . H6B H 0.7408 0.0470 1.0384 0.058 Uiso 1 1 calc R . . H6C H 0.7282 0.1371 0.9915 0.058 Uiso 1 1 calc R . . C7 C 0.7054(3) -0.1306(3) 0.9271(2) 0.0305(10) Uani 1 1 d . . . H7 H 0.7550 -0.1686 0.9544 0.037 Uiso 1 1 calc R . . C8 C 0.6248(3) -0.1805(3) 0.8890(2) 0.0335(10) Uani 1 1 d . . . C9 C 0.6140(4) -0.2907(3) 0.8934(3) 0.0494(14) Uani 1 1 d . . . H9A H 0.6711 -0.3176 0.9240 0.074 Uiso 1 1 calc R . . H9B H 0.6066 -0.3208 0.8533 0.074 Uiso 1 1 calc R . . H9C H 0.5574 -0.3051 0.9058 0.074 Uiso 1 1 calc R . . C10 C 0.5545(3) -0.1253(3) 0.8497(2) 0.0306(9) Uani 1 1 d . . . H10 H 0.4995 -0.1569 0.8231 0.037 Uiso 1 1 calc R . . C11 C 0.5620(3) -0.0239(3) 0.84805(19) 0.0242(8) Uani 1 1 d . . . C12 C 0.5177(3) 0.0923(3) 0.70094(19) 0.0276(9) Uani 1 1 d . . . C13 C 0.5090(3) 0.0855(3) 0.6372(2) 0.0333(10) Uani 1 1 d . . . C14 C 0.5541(4) 0.1628(3) 0.6071(2) 0.0406(11) Uani 1 1 d . . . C15 C 0.5279(6) 0.1485(4) 0.5383(3) 0.084(2) Uani 1 1 d . . . H15A H 0.5587 0.1997 0.5209 0.126 Uiso 1 1 calc R . . H15B H 0.4582 0.1531 0.5197 0.126 Uiso 1 1 calc R . . H15C H 0.5497 0.0836 0.5296 0.126 Uiso 1 1 calc R . . C16 C 0.6635(4) 0.1579(4) 0.6349(3) 0.0672(18) Uani 1 1 d . . . H16A H 0.6927 0.2082 0.6157 0.101 Uiso 1 1 calc R . . H16B H 0.6859 0.0926 0.6274 0.101 Uiso 1 1 calc R . . H16C H 0.6817 0.1699 0.6792 0.101 Uiso 1 1 calc R . . C17 C 0.5207(4) 0.2653(3) 0.6173(2) 0.0442(12) Uani 1 1 d . . . H17A H 0.5513 0.3141 0.5980 0.066 Uiso 1 1 calc R . . H17B H 0.5384 0.2785 0.6615 0.066 Uiso 1 1 calc R . . H17C H 0.4510 0.2696 0.5990 0.066 Uiso 1 1 calc R . . C18 C 0.4552(4) 0.0076(3) 0.6041(2) 0.0389(11) Uani 1 1 d . . . H18 H 0.4511 0.0012 0.5621 0.047 Uiso 1 1 calc R . . C19 C 0.4068(3) -0.0619(3) 0.6286(2) 0.0376(11) Uani 1 1 d . . . C20 C 0.3496(4) -0.1430(4) 0.5884(2) 0.0522(14) Uani 1 1 d . . . H20A H 0.3552 -0.1374 0.5470 0.078 Uiso 1 1 calc R . . H20B H 0.2822 -0.1372 0.5861 0.078 Uiso 1 1 calc R . . H20C H 0.3743 -0.2071 0.6060 0.078 Uiso 1 1 calc R . . C21 C 0.4116(3) -0.0509(3) 0.6888(2) 0.0309(10) Uani 1 1 d . . . H21 H 0.3773 -0.0948 0.7066 0.037 Uiso 1 1 calc R . . C22 C 0.4661(3) 0.0239(3) 0.72422(19) 0.0264(9) Uani 1 1 d . . . C23 C 0.3684(3) 0.3809(3) 0.7522(2) 0.0309(10) Uani 1 1 d . . . H23 H 0.3363 0.3866 0.7847 0.037 Uiso 1 1 calc R . . C24 C 0.3911(3) 0.4851(3) 0.73661(19) 0.0300(9) Uani 1 1 d . . . C25 C 0.4431(3) 0.5000(3) 0.6962(2) 0.0408(12) Uani 1 1 d . . . H25 H 0.4608 0.4453 0.6762 0.049 Uiso 1 1 calc R . . C26 C 0.4692(4) 0.5938(4) 0.6850(2) 0.0442(12) Uani 1 1 d . . . H26 H 0.5057 0.6035 0.6578 0.053 Uiso 1 1 calc R . . C27 C 0.4428(4) 0.6731(3) 0.7130(2) 0.0432(12) Uani 1 1 d . . . H27 H 0.4629 0.7374 0.7062 0.052 Uiso 1 1 calc R . . C28 C 0.3878(4) 0.6600(3) 0.7503(2) 0.0449(12) Uani 1 1 d . . . H28 H 0.3665 0.7154 0.7678 0.054 Uiso 1 1 calc R . . C29 C 0.3627(3) 0.5653(3) 0.7629(2) 0.0393(11) Uani 1 1 d . . . H29 H 0.3257 0.5562 0.7899 0.047 Uiso 1 1 calc R . . C30 C 0.2980(3) 0.3288(3) 0.6973(2) 0.0296(9) Uani 1 1 d . . . C31 C 0.3169(3) 0.2364(3) 0.6796(2) 0.0356(10) Uani 1 1 d . . . H31 H 0.3757 0.2053 0.7012 0.043 Uiso 1 1 calc R . . C32 C 0.2523(4) 0.1877(4) 0.6309(2) 0.0444(12) Uani 1 1 d . . . H32 H 0.2666 0.1236 0.6197 0.053 Uiso 1 1 calc R . . C33 C 0.1672(4) 0.2324(4) 0.5989(2) 0.0420(11) Uani 1 1 d . . . H33 H 0.1227 0.1993 0.5655 0.050 Uiso 1 1 calc R . . C34 C 0.1469(3) 0.3249(3) 0.6155(2) 0.0387(11) Uani 1 1 d . . . H34 H 0.0884 0.3561 0.5934 0.046 Uiso 1 1 calc R . . C35 C 0.2118(3) 0.3727(3) 0.6644(2) 0.0348(10) Uani 1 1 d . . . H35 H 0.1972 0.4367 0.6756 0.042 Uiso 1 1 calc R . . C36 C 0.5556(4) 0.4305(3) 0.9087(2) 0.0483(13) Uani 1 1 d . . . H36A H 0.4915 0.4069 0.9078 0.058 Uiso 1 1 calc R . . H36B H 0.5478 0.4805 0.8760 0.058 Uiso 1 1 calc R . . C37 C 0.6086(4) 0.4731(4) 0.9706(2) 0.0513(14) Uani 1 1 d . . . H37A H 0.5956 0.5444 0.9723 0.062 Uiso 1 1 calc R . . H37B H 0.5912 0.4390 1.0038 0.062 Uiso 1 1 calc R . . C38 C 0.7111(4) 0.4546(3) 0.9752(2) 0.0499(14) Uani 1 1 d . . . H38A H 0.7523 0.4525 1.0186 0.060 Uiso 1 1 calc R . . H38B H 0.7353 0.5059 0.9532 0.060 Uiso 1 1 calc R . . C39 C 0.7072(4) 0.3557(4) 0.9449(2) 0.0463(13) Uani 1 1 d . . . H39A H 0.7575 0.3505 0.9248 0.056 Uiso 1 1 calc R . . H39B H 0.7163 0.3021 0.9755 0.056 Uiso 1 1 calc R . . C40 C 0.4919(3) 0.1747(4) 0.9496(2) 0.0405(11) Uani 1 1 d . . . H40A H 0.4969 0.2273 0.9804 0.049 Uiso 1 1 calc R . . H40B H 0.5550 0.1421 0.9584 0.049 Uiso 1 1 calc R . . C41 C 0.4173(4) 0.1023(4) 0.9510(3) 0.0567(15) Uani 1 1 d . . . H41A H 0.4141 0.0943 0.9933 0.068 Uiso 1 1 calc R . . H41B H 0.4300 0.0374 0.9355 0.068 Uiso 1 1 calc R . . C42 C 0.3253(3) 0.1469(4) 0.9090(2) 0.0431(12) Uani 1 1 d . . . H42A H 0.2911 0.1837 0.9330 0.052 Uiso 1 1 calc R . . H42B H 0.2825 0.0950 0.8848 0.052 Uiso 1 1 calc R . . C43 C 0.3577(3) 0.2160(3) 0.8669(2) 0.0358(11) Uani 1 1 d . . . H43A H 0.3333 0.1930 0.8237 0.043 Uiso 1 1 calc R . . H43B H 0.3336 0.2835 0.8691 0.043 Uiso 1 1 calc R . . C44 C 0.7757(4) 0.2709(4) 0.7979(3) 0.0535(14) Uani 1 1 d . . . H44A H 0.7600 0.2113 0.7717 0.064 Uiso 1 1 calc R . . H44B H 0.8205 0.2522 0.8385 0.064 Uiso 1 1 calc R . . C45 C 0.8199(4) 0.3478(5) 0.7684(3) 0.0654(17) Uani 1 1 d . . . H45A H 0.8766 0.3774 0.7989 0.079 Uiso 1 1 calc R . . H45B H 0.8397 0.3191 0.7345 0.079 Uiso 1 1 calc R . . C46 C 0.7443(5) 0.4223(5) 0.7445(3) 0.0724(19) Uani 1 1 d . . . H46A H 0.7042 0.4062 0.7021 0.087 Uiso 1 1 calc R . . H46B H 0.7722 0.4887 0.7448 0.087 Uiso 1 1 calc R . . C47 C 0.6871(4) 0.4166(4) 0.7885(3) 0.0560(15) Uani 1 1 d . . . H47A H 0.7165 0.4576 0.8254 0.067 Uiso 1 1 calc R . . H47B H 0.6205 0.4388 0.7686 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.02389(9) 0.01648(9) 0.03260(10) 0.00117(7) 0.00775(7) -0.00079(7) S1 0.0226(5) 0.0193(5) 0.0333(6) 0.0010(4) 0.0085(4) -0.0006(4) O1 0.0246(15) 0.0183(14) 0.0380(17) 0.0009(12) 0.0045(13) -0.0021(11) O2 0.0294(16) 0.0216(14) 0.0339(16) 0.0004(12) 0.0108(13) -0.0046(12) O3 0.0338(17) 0.0243(16) 0.0402(18) 0.0054(13) 0.0076(14) 0.0078(12) O4 0.0367(18) 0.0295(17) 0.048(2) -0.0113(14) 0.0103(15) -0.0051(13) O5 0.0292(16) 0.0341(18) 0.0313(16) 0.0005(12) 0.0105(13) -0.0013(12) O6 0.0330(17) 0.0289(17) 0.055(2) 0.0012(15) 0.0170(15) -0.0092(13) C1 0.028(2) 0.021(2) 0.034(2) 0.0003(17) 0.0162(18) 0.0002(16) C2 0.027(2) 0.024(2) 0.031(2) 0.0045(17) 0.0116(18) 0.0024(17) C3 0.026(2) 0.033(2) 0.039(3) 0.0051(19) 0.008(2) 0.0054(18) C4 0.031(2) 0.043(3) 0.041(3) 0.001(2) 0.007(2) 0.009(2) C5 0.022(2) 0.056(3) 0.056(3) 0.017(2) 0.009(2) -0.006(2) C6 0.030(2) 0.039(3) 0.040(3) -0.008(2) 0.000(2) 0.002(2) C7 0.028(2) 0.026(2) 0.040(3) 0.0062(18) 0.013(2) 0.0073(17) C8 0.035(2) 0.021(2) 0.049(3) 0.0030(19) 0.020(2) 0.0045(18) C9 0.043(3) 0.024(3) 0.077(4) 0.013(2) 0.012(3) 0.003(2) C10 0.031(2) 0.022(2) 0.039(3) 0.0010(18) 0.012(2) -0.0020(17) C11 0.025(2) 0.0171(19) 0.032(2) 0.0027(16) 0.0113(17) 0.0004(15) C12 0.030(2) 0.018(2) 0.035(2) 0.0000(17) 0.0107(19) 0.0013(16) C13 0.045(3) 0.018(2) 0.041(3) -0.0032(18) 0.021(2) 0.0003(18) C14 0.058(3) 0.028(2) 0.045(3) -0.003(2) 0.030(3) -0.006(2) C15 0.170(8) 0.045(3) 0.058(4) -0.014(3) 0.065(5) -0.044(4) C16 0.061(4) 0.048(3) 0.114(5) 0.018(3) 0.058(4) 0.004(3) C17 0.058(3) 0.028(2) 0.050(3) 0.010(2) 0.022(3) 0.001(2) C18 0.054(3) 0.029(2) 0.038(3) -0.0046(19) 0.020(2) 0.000(2) C19 0.048(3) 0.022(2) 0.041(3) -0.0013(19) 0.010(2) -0.0033(19) C20 0.071(4) 0.036(3) 0.048(3) -0.013(2) 0.017(3) -0.020(3) C21 0.032(2) 0.024(2) 0.036(3) 0.0010(18) 0.010(2) -0.0032(18) C22 0.029(2) 0.019(2) 0.031(2) 0.0028(16) 0.0094(18) 0.0059(16) C23 0.039(3) 0.024(2) 0.035(2) 0.0051(17) 0.019(2) 0.0096(18) C24 0.033(2) 0.022(2) 0.031(2) 0.0008(17) 0.0060(19) 0.0047(17) C25 0.056(3) 0.027(2) 0.043(3) -0.0050(19) 0.021(3) 0.002(2) C26 0.053(3) 0.037(3) 0.045(3) 0.004(2) 0.019(3) 0.001(2) C27 0.052(3) 0.023(2) 0.048(3) 0.001(2) 0.006(2) -0.002(2) C28 0.052(3) 0.024(2) 0.055(3) -0.012(2) 0.010(3) 0.004(2) C29 0.040(3) 0.033(3) 0.042(3) -0.005(2) 0.009(2) 0.008(2) C30 0.030(2) 0.027(2) 0.035(2) 0.0055(17) 0.0140(19) 0.0049(17) C31 0.032(2) 0.033(2) 0.040(3) 0.004(2) 0.009(2) 0.0089(19) C32 0.056(3) 0.034(3) 0.044(3) -0.004(2) 0.018(3) 0.002(2) C33 0.042(3) 0.042(3) 0.040(3) 0.000(2) 0.010(2) -0.002(2) C34 0.030(2) 0.043(3) 0.044(3) 0.009(2) 0.012(2) 0.007(2) C35 0.033(2) 0.025(2) 0.048(3) 0.0052(19) 0.016(2) 0.0065(18) C36 0.054(3) 0.028(3) 0.066(4) -0.012(2) 0.023(3) 0.001(2) C37 0.085(4) 0.025(3) 0.048(3) 0.002(2) 0.027(3) 0.002(3) C38 0.066(4) 0.030(3) 0.045(3) -0.003(2) 0.005(3) -0.017(2) C39 0.041(3) 0.042(3) 0.046(3) -0.003(2) -0.001(2) -0.006(2) C40 0.035(3) 0.058(3) 0.027(2) 0.004(2) 0.007(2) 0.000(2) C41 0.041(3) 0.070(4) 0.060(4) 0.018(3) 0.017(3) 0.006(3) C42 0.032(3) 0.040(3) 0.058(3) 0.015(2) 0.015(2) -0.001(2) C43 0.029(2) 0.036(3) 0.043(3) 0.010(2) 0.013(2) 0.0109(19) C44 0.036(3) 0.054(3) 0.077(4) 0.007(3) 0.029(3) 0.000(2) C45 0.059(4) 0.074(4) 0.076(4) 0.005(3) 0.039(3) -0.013(3) C46 0.092(5) 0.065(4) 0.065(4) 0.018(3) 0.031(4) -0.023(4) C47 0.053(3) 0.033(3) 0.081(4) 0.015(3) 0.018(3) -0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 O3 2.045(3) . ? Lu1 O1 2.151(3) . ? Lu1 O2 2.176(3) . ? Lu1 O6 2.347(3) . ? Lu1 O4 2.389(3) . ? Lu1 O5 2.445(3) . ? Lu1 S1 2.8707(11) . ? S1 C22 1.765(4) . ? S1 C11 1.788(4) . ? O1 C1 1.326(4) . ? O2 C12 1.316(5) . ? O3 C23 1.383(5) . ? O4 C36 1.431(5) . ? O4 C39 1.442(5) . ? O5 C40 1.438(5) . ? O5 C43 1.450(5) . ? O6 C47 1.440(5) . ? O6 C44 1.444(6) . ? C1 C11 1.417(5) . ? C1 C2 1.427(6) . ? C2 C7 1.395(6) . ? C2 C3 1.522(6) . ? C3 C4 1.526(6) . ? C3 C5 1.528(6) . ? C3 C6 1.535(6) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.406(6) . ? C7 H7 0.9500 . ? C8 C10 1.363(6) . ? C8 C9 1.512(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.383(5) . ? C10 H10 0.9500 . ? C12 C22 1.406(6) . ? C12 C13 1.428(6) . ? C13 C18 1.394(6) . ? C13 C14 1.520(6) . ? C14 C15 1.513(7) . ? C14 C17 1.519(6) . ? C14 C16 1.534(7) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.402(6) . ? C18 H18 0.9500 . ? C19 C21 1.367(6) . ? C19 C20 1.511(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.388(6) . ? C21 H21 0.9500 . ? C23 C24 1.523(6) . ? C23 C30 1.528(6) . ? C23 H23 1.0000 . ? C24 C29 1.372(6) . ? C24 C25 1.389(6) . ? C25 C26 1.378(7) . ? C25 H25 0.9500 . ? C26 C27 1.370(7) . ? C26 H26 0.9500 . ? C27 C28 1.362(7) . ? C27 H27 0.9500 . ? C28 C29 1.393(6) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.373(6) . ? C30 C35 1.391(6) . ? C31 C32 1.386(7) . ? C31 H31 0.9500 . ? C32 C33 1.378(7) . ? C32 H32 0.9500 . ? C33 C34 1.372(7) . ? C33 H33 0.9500 . ? C34 C35 1.385(6) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.504(7) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.500(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.505(7) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.482(7) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.519(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.525(6) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.499(7) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.475(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.504(8) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 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 O3 Lu1 O1 162.89(12) . . ? O3 Lu1 O2 96.59(11) . . ? O1 Lu1 O2 95.81(11) . . ? O3 Lu1 O6 100.07(11) . . ? O1 Lu1 O6 94.00(11) . . ? O2 Lu1 O6 78.08(10) . . ? O3 Lu1 O4 87.67(11) . . ? O1 Lu1 O4 87.33(11) . . ? O2 Lu1 O4 150.56(11) . . ? O6 Lu1 O4 72.50(11) . . ? O3 Lu1 O5 80.85(11) . . ? O1 Lu1 O5 82.04(10) . . ? O2 Lu1 O5 137.47(10) . . ? O6 Lu1 O5 144.39(10) . . ? O4 Lu1 O5 71.97(10) . . ? O3 Lu1 S1 102.42(9) . . ? O1 Lu1 S1 71.33(7) . . ? O2 Lu1 S1 68.77(7) . . ? O6 Lu1 S1 141.59(8) . . ? O4 Lu1 S1 138.74(8) . . ? O5 Lu1 S1 70.41(7) . . ? C22 S1 C11 105.01(19) . . ? C22 S1 Lu1 97.73(14) . . ? C11 S1 Lu1 95.41(13) . . ? C1 O1 Lu1 132.2(2) . . ? C12 O2 Lu1 132.3(3) . . ? C23 O3 Lu1 170.2(3) . . ? C36 O4 C39 109.9(4) . . ? C36 O4 Lu1 123.5(3) . . ? C39 O4 Lu1 126.6(3) . . ? C40 O5 C43 107.9(3) . . ? C40 O5 Lu1 126.5(3) . . ? C43 O5 Lu1 123.2(2) . . ? C47 O6 C44 108.6(4) . . ? C47 O6 Lu1 123.0(3) . . ? C44 O6 Lu1 127.5(3) . . ? O1 C1 C11 120.6(4) . . ? O1 C1 C2 122.4(4) . . ? C11 C1 C2 116.9(4) . . ? C7 C2 C1 118.1(4) . . ? C7 C2 C3 121.0(4) . . ? C1 C2 C3 120.8(4) . . ? C2 C3 C4 113.2(4) . . ? C2 C3 C5 110.1(4) . . ? C4 C3 C5 107.9(4) . . ? C2 C3 C6 108.7(3) . . ? C4 C3 C6 106.7(4) . . ? C5 C3 C6 110.2(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 C8 123.7(4) . . ? C2 C7 H7 118.1 . . ? C8 C7 H7 118.1 . . ? C10 C8 C7 117.6(4) . . ? C10 C8 C9 121.0(4) . . ? C7 C8 C9 121.4(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 C11 121.0(4) . . ? C8 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C10 C11 C1 122.6(4) . . ? C10 C11 S1 118.5(3) . . ? C1 C11 S1 118.8(3) . . ? O2 C12 C22 120.5(4) . . ? O2 C12 C13 122.2(4) . . ? C22 C12 C13 117.3(4) . . ? C18 C13 C12 117.3(4) . . ? C18 C13 C14 122.2(4) . . ? C12 C13 C14 120.5(4) . . ? C15 C14 C17 106.8(4) . . ? C15 C14 C13 112.3(4) . . ? C17 C14 C13 110.8(4) . . ? C15 C14 C16 108.6(5) . . ? C17 C14 C16 108.9(4) . . ? C13 C14 C16 109.4(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 C19 124.5(4) . . ? C13 C18 H18 117.7 . . ? C19 C18 H18 117.7 . . ? C21 C19 C18 117.3(4) . . ? C21 C19 C20 122.5(4) . . ? C18 C19 C20 120.2(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 C22 120.4(4) . . ? C19 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C12 123.0(4) . . ? C21 C22 S1 119.9(3) . . ? C12 C22 S1 116.8(3) . . ? O3 C23 C24 111.2(4) . . ? O3 C23 C30 112.1(3) . . ? C24 C23 C30 112.2(3) . . ? O3 C23 H23 107.0 . . ? C24 C23 H23 107.0 . . ? C30 C23 H23 107.0 . . ? C29 C24 C25 119.0(4) . . ? C29 C24 C23 121.0(4) . . ? C25 C24 C23 120.0(4) . . ? C26 C25 C24 120.2(4) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C25 120.2(5) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 C26 120.3(5) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 119.9(4) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C24 C29 C28 120.3(5) . . ? C24 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C35 117.8(4) . . ? C31 C30 C23 121.2(4) . . ? C35 C30 C23 121.0(4) . . ? C30 C31 C32 121.5(4) . . ? C30 C31 H31 119.2 . . ? C32 C31 H31 119.2 . . ? C33 C32 C31 119.8(5) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C34 C33 C32 119.8(5) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 119.9(4) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C34 C35 C30 121.2(4) . . ? C34 C35 H35 119.4 . . ? C30 C35 H35 119.4 . . ? O4 C36 C37 105.6(4) . . ? O4 C36 H36A 110.6 . . ? C37 C36 H36A 110.6 . . ? O4 C36 H36B 110.6 . . ? C37 C36 H36B 110.6 . . ? H36A C36 H36B 108.7 . . ? C38 C37 C36 102.3(4) . . ? C38 C37 H37A 111.3 . . ? C36 C37 H37A 111.3 . . ? C38 C37 H37B 111.3 . . ? C36 C37 H37B 111.3 . . ? H37A C37 H37B 109.2 . . ? C37 C38 C39 103.1(4) . . ? C37 C38 H38A 111.2 . . ? C39 C38 H38A 111.2 . . ? C37 C38 H38B 111.2 . . ? C39 C38 H38B 111.2 . . ? H38A C38 H38B 109.1 . . ? O4 C39 C38 105.2(4) . . ? O4 C39 H39A 110.7 . . ? C38 C39 H39A 110.7 . . ? O4 C39 H39B 110.7 . . ? C38 C39 H39B 110.7 . . ? H39A C39 H39B 108.8 . . ? O5 C40 C41 105.5(4) . . ? O5 C40 H40A 110.6 . . ? C41 C40 H40A 110.6 . . ? O5 C40 H40B 110.6 . . ? C41 C40 H40B 110.6 . . ? H40A C40 H40B 108.8 . . ? C40 C41 C42 103.9(4) . . ? C40 C41 H41A 111.0 . . ? C42 C41 H41A 111.0 . . ? C40 C41 H41B 111.0 . . ? C42 C41 H41B 111.0 . . ? H41A C41 H41B 109.0 . . ? C41 C42 C43 104.7(4) . . ? C41 C42 H42A 110.8 . . ? C43 C42 H42A 110.8 . . ? C41 C42 H42B 110.8 . . ? C43 C42 H42B 110.8 . . ? H42A C42 H42B 108.9 . . ? O5 C43 C42 106.4(3) . . ? O5 C43 H43A 110.4 . . ? C42 C43 H43A 110.4 . . ? O5 C43 H43B 110.4 . . ? C42 C43 H43B 110.4 . . ? H43A C43 H43B 108.6 . . ? O6 C44 C45 106.5(4) . . ? O6 C44 H44A 110.4 . . ? C45 C44 H44A 110.4 . . ? O6 C44 H44B 110.4 . . ? C45 C44 H44B 110.4 . . ? H44A C44 H44B 108.6 . . ? C46 C45 C44 105.2(5) . . ? C46 C45 H45A 110.7 . . ? C44 C45 H45A 110.7 . . ? C46 C45 H45B 110.7 . . ? C44 C45 H45B 110.7 . . ? H45A C45 H45B 108.8 . . ? C45 C46 C47 103.4(5) . . ? C45 C46 H46A 111.1 . . ? C47 C46 H46A 111.1 . . ? C45 C46 H46B 111.1 . . ? C47 C46 H46B 111.1 . . ? H46A C46 H46B 109.0 . . ? O6 C47 C46 104.2(5) . . ? O6 C47 H47A 110.9 . . ? C46 C47 H47A 110.9 . . ? O6 C47 H47B 110.9 . . ? C46 C47 H47B 110.9 . . ? H47A C47 H47B 108.9 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.488 _refine_diff_density_min -0.812 _refine_diff_density_rms 0.117 #===END #============================================================================== data_mk7 _database_code_depnum_ccdc_archive 'CCDC 643869' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(tetrahydrofurane)-\m-hydrido-thiobis(6-tert-butyl-4-methylphenolato)- lutetium(III) dimer ; _chemical_name_common ; Bis(tetrahydrofurane)-mu-hydrido-thiobis(6-tert-butyl-4- methylphenolato)-lutetium(iii) dimer ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H65 Lu O5 S' _chemical_formula_weight 820.98 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' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1250 0.1230 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.835(9) _cell_length_b 17.805(6) _cell_length_c 18.098(6) _cell_angle_alpha 90.00 _cell_angle_beta 121.466(5) _cell_angle_gamma 90.00 _cell_volume 8200(5) _cell_formula_units_Z 8 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 982 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.19 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3407 _exptl_absorpt_coefficient_mu 2.496 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3159 _exptl_absorpt_correction_T_max 0.5214 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42018 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 28.36 _reflns_number_total 10147 _reflns_number_gt 8778 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+23.6656P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10147 _refine_ls_number_parameters 414 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0682 _refine_ls_wR_factor_gt 0.0633 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu Lu 0.480016(4) 0.235468(6) 0.138753(6) 0.01481(4) Uani 1 1 d . . . H1 H 0.4552(13) 0.2383(17) 0.227(2) 0.026(9) Uiso 1 1 d . . . S S 0.44373(2) 0.23982(4) -0.04542(4) 0.01843(12) Uani 1 1 d . . . O1 O 0.43179(7) 0.33136(10) 0.08109(11) 0.0199(4) Uani 1 1 d . . . O2 O 0.42286(7) 0.15043(11) 0.07161(11) 0.0207(4) Uani 1 1 d . . . O3 O 0.54441(7) 0.31177(11) 0.13550(12) 0.0241(4) Uani 1 1 d . . . O4 O 0.53689(7) 0.14627(11) 0.13571(12) 0.0267(4) Uani 1 1 d . . . C1 C 0.40596(9) 0.36038(14) 0.00219(15) 0.0176(5) Uani 1 1 d . . . C2 C 0.40772(9) 0.32508(15) -0.06653(15) 0.0184(5) Uani 1 1 d . . . C3 C 0.38275(10) 0.35525(16) -0.14973(16) 0.0216(5) Uani 1 1 d . . . H3 H 0.3855 0.3308 -0.1939 0.026 Uiso 1 1 calc R . . C4 C 0.35382(10) 0.42102(16) -0.16817(16) 0.0231(5) Uani 1 1 d . . . C5 C 0.35077(10) 0.45485(15) -0.10168(17) 0.0220(5) Uani 1 1 d . . . H5 H 0.3307 0.4996 -0.1144 0.026 Uiso 1 1 calc R . . C6 C 0.37545(10) 0.42688(15) -0.01733(16) 0.0189(5) Uani 1 1 d . . . C7 C 0.32543(13) 0.4540(2) -0.25858(19) 0.0363(7) Uani 1 1 d . . . H7A H 0.2902 0.4322 -0.2924 0.054 Uiso 1 1 calc R . . H7B H 0.3451 0.4425 -0.2868 0.054 Uiso 1 1 calc R . . H7C H 0.3226 0.5085 -0.2551 0.054 Uiso 1 1 calc R . . C8 C 0.36754(10) 0.46403(15) 0.05195(17) 0.0220(5) Uani 1 1 d . . . C9 C 0.34112(11) 0.40638(17) 0.08093(18) 0.0272(6) Uani 1 1 d . . . H9A H 0.3077 0.3900 0.0306 0.041 Uiso 1 1 calc R . . H9B H 0.3345 0.4296 0.1235 0.041 Uiso 1 1 calc R . . H9C H 0.3643 0.3629 0.1072 0.041 Uiso 1 1 calc R . . C10 C 0.42036(11) 0.48971(17) 0.12979(18) 0.0275(6) Uani 1 1 d . . . H10A H 0.4439 0.4464 0.1545 0.041 Uiso 1 1 calc R . . H10B H 0.4146 0.5118 0.1737 0.041 Uiso 1 1 calc R . . H10C H 0.4362 0.5273 0.1108 0.041 Uiso 1 1 calc R . . C11 C 0.33126(13) 0.53294(18) 0.0165(2) 0.0340(7) Uani 1 1 d . . . H11A H 0.3472 0.5710 -0.0019 0.051 Uiso 1 1 calc R . . H11B H 0.3264 0.5538 0.0619 0.051 Uiso 1 1 calc R . . H11C H 0.2971 0.5179 -0.0331 0.051 Uiso 1 1 calc R . . C12 C 0.39486(10) 0.16924(15) -0.07654(16) 0.0195(5) Uani 1 1 d . . . C13 C 0.39073(9) 0.13207(14) -0.01105(15) 0.0185(5) Uani 1 1 d . . . C14 C 0.35171(10) 0.07525(15) -0.03737(16) 0.0209(5) Uani 1 1 d . . . C15 C 0.31990(10) 0.05993(16) -0.12553(17) 0.0241(6) Uani 1 1 d . . . H15 H 0.2938 0.0221 -0.1429 0.029 Uiso 1 1 calc R . . C16 C 0.32397(10) 0.09681(17) -0.19001(17) 0.0248(6) Uani 1 1 d . . . C17 C 0.36226(10) 0.15125(16) -0.16437(16) 0.0237(6) Uani 1 1 d . . . H17 H 0.3665 0.1766 -0.2065 0.028 Uiso 1 1 calc R . . C18 C 0.28677(12) 0.0784(2) -0.28487(18) 0.0348(7) Uani 1 1 d . . . H18A H 0.2541 0.1069 -0.3069 0.052 Uiso 1 1 calc R . . H18B H 0.2789 0.0245 -0.2912 0.052 Uiso 1 1 calc R . . H18C H 0.3032 0.0919 -0.3178 0.052 Uiso 1 1 calc R . . C19 C 0.34357(11) 0.03475(17) 0.02950(18) 0.0263(6) Uani 1 1 d . . . C20 C 0.30110(13) -0.0263(2) -0.0118(2) 0.0399(8) Uani 1 1 d . . . H20A H 0.2675 -0.0033 -0.0545 0.060 Uiso 1 1 calc R . . H20B H 0.2976 -0.0510 0.0333 0.060 Uiso 1 1 calc R . . H20C H 0.3111 -0.0634 -0.0406 0.060 Uiso 1 1 calc R . . C21 C 0.39481(13) -0.00366(19) 0.0990(2) 0.0380(7) Uani 1 1 d . . . H21A H 0.4058 -0.0405 0.0713 0.057 Uiso 1 1 calc R . . H21B H 0.3888 -0.0292 0.1411 0.057 Uiso 1 1 calc R . . H21C H 0.4224 0.0343 0.1288 0.057 Uiso 1 1 calc R . . C22 C 0.32577(12) 0.0924(2) 0.0718(2) 0.0342(7) Uani 1 1 d . . . H22A H 0.3517 0.1330 0.0971 0.051 Uiso 1 1 calc R . . H22B H 0.3226 0.0679 0.1173 0.051 Uiso 1 1 calc R . . H22C H 0.2916 0.1132 0.0279 0.051 Uiso 1 1 calc R . . C23 C 0.56526(11) 0.3151(2) 0.07905(19) 0.0327(7) Uani 1 1 d . . . H23A H 0.5510 0.2738 0.0362 0.039 Uiso 1 1 calc R . . H23B H 0.6041 0.3117 0.1129 0.039 Uiso 1 1 calc R . . C24 C 0.54741(16) 0.3911(2) 0.0342(2) 0.0509(10) Uani 1 1 d . . . H24A H 0.5154 0.3857 -0.0239 0.061 Uiso 1 1 calc R . . H24B H 0.5753 0.4146 0.0280 0.061 Uiso 1 1 calc R . . C25 C 0.53620(14) 0.4379(2) 0.0937(2) 0.0445(9) Uani 1 1 d . . . H25A H 0.5577 0.4843 0.1126 0.053 Uiso 1 1 calc R . . H25B H 0.4986 0.4518 0.0641 0.053 Uiso 1 1 calc R . . C26 C 0.55122(12) 0.38671(17) 0.1699(2) 0.0308(6) Uani 1 1 d . . . H26A H 0.5881 0.3953 0.2167 0.037 Uiso 1 1 calc R . . H26B H 0.5281 0.3953 0.1933 0.037 Uiso 1 1 calc R . . C27 C 0.59332(12) 0.1445(2) 0.1957(2) 0.0415(8) Uani 1 1 d . . . H27A H 0.6015 0.1351 0.2554 0.050 Uiso 1 1 calc R . . H27B H 0.6093 0.1930 0.1947 0.050 Uiso 1 1 calc R . . C28 C 0.61367(16) 0.0837(3) 0.1672(4) 0.091(2) Uani 1 1 d . . . H28A H 0.6329 0.1045 0.1409 0.110 Uiso 1 1 calc R . . H28B H 0.6382 0.0521 0.2172 0.110 Uiso 1 1 calc R . . C29 C 0.57018(16) 0.0397(3) 0.1050(4) 0.089(2) Uani 1 1 d . . . H29A H 0.5693 -0.0088 0.1308 0.107 Uiso 1 1 calc R . . H29B H 0.5735 0.0294 0.0542 0.107 Uiso 1 1 calc R . . C30 C 0.52199(12) 0.08205(19) 0.0781(2) 0.0385(8) Uani 1 1 d . . . H30A H 0.5059 0.0989 0.0173 0.046 Uiso 1 1 calc R . . H30B H 0.4963 0.0504 0.0827 0.046 Uiso 1 1 calc R . . O5 O 0.19990(11) 0.77316(19) 0.22158(19) 0.0617(8) Uani 1 1 d . . . C31 C 0.23902(16) 0.7166(2) 0.2477(3) 0.0507(10) Uani 1 1 d . . . H31A H 0.2707 0.7371 0.2503 0.061 Uiso 1 1 calc R . . H31B H 0.2255 0.6740 0.2063 0.061 Uiso 1 1 calc R . . C32 C 0.25174(18) 0.6916(3) 0.3347(3) 0.0610(12) Uani 1 1 d . . . H32A H 0.2881 0.6720 0.3691 0.073 Uiso 1 1 calc R . . H32B H 0.2270 0.6523 0.3304 0.073 Uiso 1 1 calc R . . C33 C 0.2457(2) 0.7618(2) 0.3732(3) 0.0598(12) Uani 1 1 d . . . H33A H 0.2789 0.7908 0.4026 0.072 Uiso 1 1 calc R . . H33B H 0.2351 0.7505 0.4155 0.072 Uiso 1 1 calc R . . C34 C 0.20319(15) 0.8043(2) 0.2966(3) 0.0478(9) Uani 1 1 d . . . H34A H 0.1692 0.7988 0.2934 0.057 Uiso 1 1 calc R . . H34B H 0.2121 0.8584 0.3016 0.057 Uiso 1 1 calc R . . C35 C 0.1457(6) 0.7430(8) 0.9872(11) 0.118(2) Uiso 0.50 1 d PD . . H35A H 0.1500 0.6967 1.0196 0.176 Uiso 0.50 1 calc PR . . H35B H 0.1104 0.7442 0.9352 0.176 Uiso 0.50 1 calc PR . . H35C H 0.1504 0.7865 1.0237 0.176 Uiso 0.50 1 calc PR . . C36 C 0.1850(5) 0.7452(12) 0.9621(11) 0.118(2) Uiso 0.50 1 d PD . . H36A H 0.1794 0.7916 0.9281 0.141 Uiso 0.50 1 calc PR . . H36B H 0.1788 0.7020 0.9234 0.141 Uiso 0.50 1 calc PR . . C37 C 0.2434(5) 0.7431(10) 1.0381(11) 0.118(2) Uiso 0.50 1 d PD . . H37A H 0.2513 0.7871 1.0763 0.141 Uiso 0.50 1 calc PR . . H37B H 0.2502 0.6969 1.0729 0.141 Uiso 0.50 1 calc PR . . C38 C 0.2770(5) 0.7441(11) 0.9989(12) 0.118(2) Uiso 0.50 1 d PD . . H38A H 0.2664 0.7870 0.9583 0.141 Uiso 0.50 1 calc PR . . H38B H 0.2710 0.6974 0.9653 0.141 Uiso 0.50 1 calc PR . . C39 C 0.3349(5) 0.7508(11) 1.0666(12) 0.118(2) Uiso 0.50 1 d PD . . H39A H 0.3514 0.7011 1.0779 0.176 Uiso 0.50 1 calc PR . . H39B H 0.3392 0.7710 1.1203 0.176 Uiso 0.50 1 calc PR . . H39C H 0.3517 0.7847 1.0456 0.176 Uiso 0.50 1 calc PR . . C40 C 0.0210(9) 0.3804(12) 0.1938(14) 0.193(5) Uiso 0.50 1 d PD . . H40A H -0.0026 0.4147 0.1471 0.289 Uiso 0.50 1 calc PR . . H40B H 0.0426 0.3529 0.1766 0.289 Uiso 0.50 1 calc PR . . H40C H 0.0439 0.4093 0.2465 0.289 Uiso 0.50 1 calc PR . . C41 C -0.0066(10) 0.3331(11) 0.2087(13) 0.193(5) Uiso 0.50 1 d PD . . H41A H -0.0143 0.2970 0.1618 0.231 Uiso 0.50 1 calc PR . . H41B H -0.0391 0.3635 0.1842 0.231 Uiso 0.50 1 calc PR . . C42 C -0.0160(9) 0.2878(11) 0.2566(18) 0.193(5) Uiso 0.50 1 d PD . . H42A H -0.0526 0.2699 0.2189 0.231 Uiso 0.50 1 calc PR . . H42B H -0.0159 0.3196 0.3016 0.231 Uiso 0.50 1 calc PR . . C43 C 0.0160(10) 0.2204(11) 0.3022(13) 0.193(5) Uiso 0.50 1 d PD . . H43A H -0.0004 0.1924 0.3293 0.231 Uiso 0.50 1 calc PR . . H43B H 0.0517 0.2359 0.3484 0.231 Uiso 0.50 1 calc PR . . C44 C 0.0195(9) 0.1709(11) 0.2378(16) 0.193(5) Uiso 0.50 1 d PD . . H44A H 0.0363 0.1985 0.2120 0.289 Uiso 0.50 1 calc PR . . H44B H -0.0160 0.1557 0.1922 0.289 Uiso 0.50 1 calc PR . . H44C H 0.0402 0.1261 0.2674 0.289 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 Lu 0.01594(6) 0.01514(6) 0.00965(5) 0.00006(4) 0.00409(4) 0.00127(4) S 0.0172(3) 0.0203(3) 0.0147(3) -0.0007(2) 0.0061(2) 0.0014(2) O1 0.0226(9) 0.0222(10) 0.0112(8) 0.0029(7) 0.0064(7) 0.0051(7) O2 0.0231(9) 0.0221(10) 0.0124(8) -0.0020(7) 0.0060(7) -0.0018(7) O3 0.0286(10) 0.0231(10) 0.0224(9) 0.0012(7) 0.0145(8) -0.0017(8) O4 0.0205(9) 0.0255(11) 0.0223(9) -0.0082(8) 0.0031(8) 0.0049(8) C1 0.0176(11) 0.0190(12) 0.0132(11) 0.0020(9) 0.0059(9) -0.0009(9) C2 0.0182(11) 0.0178(12) 0.0162(11) 0.0013(9) 0.0069(9) 0.0007(9) C3 0.0235(12) 0.0258(14) 0.0151(11) 0.0009(10) 0.0099(10) -0.0010(10) C4 0.0232(13) 0.0265(14) 0.0152(11) 0.0057(10) 0.0070(10) 0.0006(10) C5 0.0215(12) 0.0207(13) 0.0214(12) 0.0070(10) 0.0096(10) 0.0032(10) C6 0.0192(11) 0.0199(13) 0.0168(11) 0.0017(9) 0.0088(10) 0.0002(9) C7 0.0448(18) 0.0405(19) 0.0205(14) 0.0128(12) 0.0149(13) 0.0117(15) C8 0.0262(13) 0.0209(13) 0.0198(12) 0.0035(10) 0.0125(10) 0.0066(10) C9 0.0291(14) 0.0319(16) 0.0257(13) 0.0019(11) 0.0178(12) 0.0013(12) C10 0.0336(15) 0.0249(15) 0.0239(13) -0.0029(11) 0.0149(12) 0.0001(12) C11 0.0426(17) 0.0324(17) 0.0289(15) 0.0064(12) 0.0200(14) 0.0167(14) C12 0.0190(11) 0.0189(13) 0.0153(11) -0.0028(9) 0.0054(9) 0.0006(10) C13 0.0161(11) 0.0183(12) 0.0158(11) -0.0030(9) 0.0047(9) 0.0035(9) C14 0.0200(12) 0.0215(13) 0.0196(12) -0.0030(10) 0.0092(10) 0.0019(10) C15 0.0198(12) 0.0237(14) 0.0233(13) -0.0072(10) 0.0075(10) -0.0004(10) C16 0.0228(13) 0.0279(15) 0.0160(12) -0.0059(10) 0.0047(10) 0.0026(11) C17 0.0262(13) 0.0258(14) 0.0148(11) -0.0015(10) 0.0076(10) 0.0043(11) C18 0.0352(16) 0.0413(19) 0.0180(13) -0.0089(12) 0.0070(12) -0.0069(14) C19 0.0255(13) 0.0286(15) 0.0223(13) -0.0035(11) 0.0108(11) -0.0069(11) C20 0.0408(18) 0.044(2) 0.0323(16) -0.0075(14) 0.0171(14) -0.0204(15) C21 0.0372(17) 0.0330(18) 0.0351(17) 0.0109(13) 0.0129(14) 0.0007(14) C22 0.0323(15) 0.047(2) 0.0269(15) -0.0073(13) 0.0177(13) -0.0062(14) C23 0.0253(14) 0.050(2) 0.0244(14) -0.0009(13) 0.0140(12) -0.0055(13) C24 0.052(2) 0.059(3) 0.0396(19) 0.0132(17) 0.0227(17) -0.0133(19) C25 0.0384(18) 0.0335(19) 0.055(2) 0.0118(16) 0.0194(16) -0.0060(15) C26 0.0307(15) 0.0237(15) 0.0339(15) -0.0060(12) 0.0139(13) -0.0065(12) C27 0.0219(14) 0.0399(19) 0.0378(17) -0.0131(14) -0.0017(12) 0.0102(13) C28 0.0296(19) 0.098(4) 0.104(4) -0.072(3) 0.005(2) 0.010(2) C29 0.037(2) 0.073(3) 0.116(4) -0.065(3) 0.011(2) 0.010(2) C30 0.0308(15) 0.0336(18) 0.0379(17) -0.0204(14) 0.0089(13) 0.0020(13) O5 0.0441(16) 0.089(2) 0.0391(15) 0.0068(14) 0.0127(13) 0.0211(15) C31 0.046(2) 0.052(2) 0.062(3) -0.0095(19) 0.034(2) -0.0006(18) C32 0.062(3) 0.051(3) 0.082(3) 0.016(2) 0.046(2) 0.016(2) C33 0.079(3) 0.051(3) 0.037(2) -0.0028(17) 0.022(2) -0.007(2) C34 0.048(2) 0.037(2) 0.058(2) -0.0038(17) 0.0273(18) 0.0069(16) _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 O1 2.1229(18) . ? Lu O2 2.1245(19) . ? Lu O4 2.3456(19) . ? Lu O3 2.379(2) . ? Lu S 2.9191(12) . ? Lu Lu 3.5530(13) 2_655 ? Lu H1 2.09(3) . ? S C12 1.779(3) . ? S C2 1.782(3) . ? O1 C1 1.323(3) . ? O2 C13 1.329(3) . ? O3 C26 1.441(3) . ? O3 C23 1.448(3) . ? O4 C27 1.451(3) . ? O4 C30 1.452(3) . ? C1 C2 1.419(3) . ? C1 C6 1.421(4) . ? C2 C3 1.393(3) . ? C3 C4 1.388(4) . ? C3 H3 0.9500 . ? C4 C5 1.391(4) . ? C4 C7 1.514(4) . ? C5 C6 1.395(3) . ? C5 H5 0.9500 . ? C6 C8 1.541(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C10 1.536(4) . ? C8 C11 1.537(4) . ? C8 C9 1.543(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C17 1.400(3) . ? C12 C13 1.418(4) . ? C13 C14 1.423(4) . ? C14 C15 1.393(4) . ? C14 C19 1.533(4) . ? C15 C16 1.399(4) . ? C15 H15 0.9500 . ? C16 C17 1.381(4) . ? C16 C18 1.516(4) . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C22 1.531(4) . ? C19 C20 1.535(4) . ? C19 C21 1.543(4) . ? 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 C24 1.524(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.530(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.514(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.461(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.427(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.463(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? O5 C34 1.422(5) . ? O5 C31 1.423(5) . ? C31 C32 1.482(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.487(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.506(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.461(15) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.558(15) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.500(13) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.515(14) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.301(15) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.318(14) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.487(16) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.506(16) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Lu O2 99.00(8) . . ? O1 Lu O4 147.77(7) . . ? O2 Lu O4 83.02(7) . . ? O1 Lu O3 82.96(7) . . ? O2 Lu O3 144.13(7) . . ? O4 Lu O3 77.45(8) . . ? O1 Lu S 70.43(5) . . ? O2 Lu S 69.95(5) . . ? O4 Lu S 80.38(5) . . ? O3 Lu S 77.26(5) . . ? O1 Lu Lu 107.31(5) . 2_655 ? O2 Lu Lu 110.03(5) . 2_655 ? O4 Lu Lu 101.99(5) . 2_655 ? O3 Lu Lu 103.32(5) . 2_655 ? S Lu Lu 177.633(13) . 2_655 ? O1 Lu H1 86.4(9) . . ? O2 Lu H1 87.4(9) . . ? O4 Lu H1 125.8(9) . . ? O3 Lu H1 128.3(9) . . ? S Lu H1 143.8(9) . . ? Lu Lu H1 34.3(9) 2_655 . ? C12 S C2 103.36(12) . . ? C12 S Lu 95.56(8) . . ? C2 S Lu 95.17(8) . . ? C1 O1 Lu 135.07(16) . . ? C13 O2 Lu 135.32(17) . . ? C26 O3 C23 104.6(2) . . ? C26 O3 Lu 116.82(17) . . ? C23 O3 Lu 133.70(17) . . ? C27 O4 C30 108.7(2) . . ? C27 O4 Lu 124.62(17) . . ? C30 O4 Lu 126.59(16) . . ? O1 C1 C2 120.4(2) . . ? O1 C1 C6 122.0(2) . . ? C2 C1 C6 117.6(2) . . ? C3 C2 C1 122.2(2) . . ? C3 C2 S 118.9(2) . . ? C1 C2 S 118.91(18) . . ? C4 C3 C2 120.0(2) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 118.1(2) . . ? C3 C4 C7 120.9(3) . . ? C5 C4 C7 121.0(3) . . ? C4 C5 C6 123.8(3) . . ? C4 C5 H5 118.1 . . ? C6 C5 H5 118.1 . . ? C5 C6 C1 118.2(2) . . ? C5 C6 C8 121.3(2) . . ? C1 C6 C8 120.4(2) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C10 C8 C11 107.9(2) . . ? C10 C8 C6 110.8(2) . . ? C11 C8 C6 112.1(2) . . ? C10 C8 C9 110.3(2) . . ? C11 C8 C9 107.4(2) . . ? C6 C8 C9 108.3(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 122.0(2) . . ? C17 C12 S 119.3(2) . . ? C13 C12 S 118.66(18) . . ? O2 C13 C12 120.0(2) . . ? O2 C13 C14 122.3(2) . . ? C12 C13 C14 117.7(2) . . ? C15 C14 C13 118.2(2) . . ? C15 C14 C19 121.2(2) . . ? C13 C14 C19 120.6(2) . . ? C14 C15 C16 124.0(3) . . ? C14 C15 H15 118.0 . . ? C16 C15 H15 118.0 . . ? C17 C16 C15 117.8(2) . . ? C17 C16 C18 121.4(3) . . ? C15 C16 C18 120.8(3) . . ? C16 C17 C12 120.3(3) . . ? C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22 C19 C14 108.5(2) . . ? C22 C19 C20 107.7(3) . . ? C14 C19 C20 112.3(2) . . ? C22 C19 C21 110.1(2) . . ? C14 C19 C21 110.8(2) . . ? C20 C19 C21 107.3(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O3 C23 C24 104.7(3) . . ? O3 C23 H23A 110.8 . . ? C24 C23 H23A 110.8 . . ? O3 C23 H23B 110.8 . . ? C24 C23 H23B 110.8 . . ? H23A C23 H23B 108.9 . . ? C23 C24 C25 104.7(3) . . ? C23 C24 H24A 110.8 . . ? C25 C24 H24A 110.8 . . ? C23 C24 H24B 110.8 . . ? C25 C24 H24B 110.8 . . ? H24A C24 H24B 108.9 . . ? C26 C25 C24 104.1(3) . . ? C26 C25 H25A 110.9 . . ? C24 C25 H25A 110.9 . . ? C26 C25 H25B 110.9 . . ? C24 C25 H25B 110.9 . . ? H25A C25 H25B 109.0 . . ? O3 C26 C25 104.8(3) . . ? O3 C26 H26A 110.8 . . ? C25 C26 H26A 110.8 . . ? O3 C26 H26B 110.8 . . ? C25 C26 H26B 110.8 . . ? H26A C26 H26B 108.9 . . ? O4 C27 C28 106.6(3) . . ? O4 C27 H27A 110.4 . . ? C28 C27 H27A 110.4 . . ? O4 C27 H27B 110.4 . . ? C28 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? C29 C28 C27 108.1(3) . . ? C29 C28 H28A 110.1 . . ? C27 C28 H28A 110.1 . . ? C29 C28 H28B 110.1 . . ? C27 C28 H28B 110.1 . . ? H28A C28 H28B 108.4 . . ? C28 C29 C30 108.1(3) . . ? C28 C29 H29A 110.1 . . ? C30 C29 H29A 110.1 . . ? C28 C29 H29B 110.1 . . ? C30 C29 H29B 110.1 . . ? H29A C29 H29B 108.4 . . ? O4 C30 C29 106.7(3) . . ? O4 C30 H30A 110.4 . . ? C29 C30 H30A 110.4 . . ? O4 C30 H30B 110.4 . . ? C29 C30 H30B 110.4 . . ? H30A C30 H30B 108.6 . . ? C34 O5 C31 108.9(3) . . ? O5 C31 C32 106.0(3) . . ? O5 C31 H31A 110.5 . . ? C32 C31 H31A 110.5 . . ? O5 C31 H31B 110.5 . . ? C32 C31 H31B 110.5 . . ? H31A C31 H31B 108.7 . . ? C31 C32 C33 102.7(3) . . ? C31 C32 H32A 111.2 . . ? C33 C32 H32A 111.2 . . ? C31 C32 H32B 111.2 . . ? C33 C32 H32B 111.2 . . ? H32A C32 H32B 109.1 . . ? C32 C33 C34 103.9(3) . . ? C32 C33 H33A 111.0 . . ? C34 C33 H33A 111.0 . . ? C32 C33 H33B 111.0 . . ? C34 C33 H33B 111.0 . . ? H33A C33 H33B 109.0 . . ? O5 C34 C33 106.8(3) . . ? O5 C34 H34A 110.4 . . ? C33 C34 H34A 110.4 . . ? O5 C34 H34B 110.4 . . ? C33 C34 H34B 110.4 . . ? H34A C34 H34B 108.6 . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C35 C36 C37 115.7(13) . . ? C35 C36 H36A 108.4 . . ? C37 C36 H36A 108.4 . . ? C35 C36 H36B 108.4 . . ? C37 C36 H36B 108.4 . . ? H36A C36 H36B 107.4 . . ? C38 C37 C36 107.3(12) . . ? C38 C37 H37A 110.2 . . ? C36 C37 H37A 110.2 . . ? C38 C37 H37B 110.2 . . ? C36 C37 H37B 110.2 . . ? H37A C37 H37B 108.5 . . ? C37 C38 C39 112.4(13) . . ? C37 C38 H38A 109.1 . . ? C39 C38 H38A 109.1 . . ? C37 C38 H38B 109.1 . . ? C39 C38 H38B 109.1 . . ? H38A C38 H38B 107.9 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C40 C41 C42 155(3) . . ? C40 C41 H41A 97.6 . . ? C42 C41 H41A 97.6 . . ? C40 C41 H41B 97.6 . . ? C42 C41 H41B 97.6 . . ? H41A C41 H41B 103.6 . . ? C41 C42 C43 124.3(16) . . ? C41 C42 H42A 106.3 . . ? C43 C42 H42A 106.3 . . ? C41 C42 H42B 106.3 . . ? C43 C42 H42B 106.3 . . ? H42A C42 H42B 106.4 . . ? C42 C43 C44 109.1(15) . . ? C42 C43 H43A 109.9 . . ? C44 C43 H43A 109.9 . . ? C42 C43 H43B 109.9 . . ? C44 C43 H43B 109.9 . . ? H43A C43 H43B 108.3 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Lu S C12 -103.06(10) . . . . ? O2 Lu S C12 4.78(10) . . . . ? O4 Lu S C12 90.81(10) . . . . ? O3 Lu S C12 169.99(10) . . . . ? Lu Lu S C12 -85.4(3) 2_655 . . . ? O1 Lu S C2 0.95(10) . . . . ? O2 Lu S C2 108.78(10) . . . . ? O4 Lu S C2 -165.19(10) . . . . ? O3 Lu S C2 -86.01(10) . . . . ? Lu Lu S C2 18.6(4) 2_655 . . . ? O2 Lu O1 C1 -65.3(2) . . . . ? O4 Lu O1 C1 25.8(3) . . . . ? O3 Lu O1 C1 78.5(2) . . . . ? S Lu O1 C1 -0.4(2) . . . . ? Lu Lu O1 C1 -179.7(2) 2_655 . . . ? O1 Lu O2 C13 57.6(2) . . . . ? O4 Lu O2 C13 -89.9(2) . . . . ? O3 Lu O2 C13 -32.8(3) . . . . ? S Lu O2 C13 -7.7(2) . . . . ? Lu Lu O2 C13 169.8(2) 2_655 . . . ? O1 Lu O3 C26 49.93(18) . . . . ? O2 Lu O3 C26 145.55(17) . . . . ? O4 Lu O3 C26 -155.81(19) . . . . ? S Lu O3 C26 121.38(18) . . . . ? Lu Lu O3 C26 -56.26(18) 2_655 . . . ? O1 Lu O3 C23 -100.9(2) . . . . ? O2 Lu O3 C23 -5.2(3) . . . . ? O4 Lu O3 C23 53.4(2) . . . . ? S Lu O3 C23 -29.4(2) . . . . ? Lu Lu O3 C23 153.0(2) 2_655 . . . ? O1 Lu O4 C27 107.0(3) . . . . ? O2 Lu O4 C27 -157.2(3) . . . . ? O3 Lu O4 C27 53.1(3) . . . . ? S Lu O4 C27 132.0(3) . . . . ? Lu Lu O4 C27 -48.1(3) 2_655 . . . ? O1 Lu O4 C30 -76.6(3) . . . . ? O2 Lu O4 C30 19.2(2) . . . . ? O3 Lu O4 C30 -130.6(3) . . . . ? S Lu O4 C30 -51.6(2) . . . . ? Lu Lu O4 C30 128.2(2) 2_655 . . . ? Lu O1 C1 C2 -0.5(4) . . . . ? Lu O1 C1 C6 179.06(17) . . . . ? O1 C1 C2 C3 -177.5(2) . . . . ? C6 C1 C2 C3 2.9(4) . . . . ? O1 C1 C2 S 1.7(3) . . . . ? C6 C1 C2 S -177.88(19) . . . . ? C12 S C2 C3 -85.4(2) . . . . ? Lu S C2 C3 177.6(2) . . . . ? C12 S C2 C1 95.4(2) . . . . ? Lu S C2 C1 -1.6(2) . . . . ? C1 C2 C3 C4 -1.7(4) . . . . ? S C2 C3 C4 179.1(2) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C2 C3 C4 C7 -178.7(3) . . . . ? C3 C4 C5 C6 0.6(4) . . . . ? C7 C4 C5 C6 179.2(3) . . . . ? C4 C5 C6 C1 0.7(4) . . . . ? C4 C5 C6 C8 -175.9(3) . . . . ? O1 C1 C6 C5 178.1(2) . . . . ? C2 C1 C6 C5 -2.3(4) . . . . ? O1 C1 C6 C8 -5.3(4) . . . . ? C2 C1 C6 C8 174.3(2) . . . . ? C5 C6 C8 C10 -121.4(3) . . . . ? C1 C6 C8 C10 62.2(3) . . . . ? C5 C6 C8 C11 -0.8(4) . . . . ? C1 C6 C8 C11 -177.3(2) . . . . ? C5 C6 C8 C9 117.5(3) . . . . ? C1 C6 C8 C9 -59.0(3) . . . . ? C2 S C12 C17 80.1(2) . . . . ? Lu S C12 C17 176.8(2) . . . . ? C2 S C12 C13 -100.8(2) . . . . ? Lu S C12 C13 -4.1(2) . . . . ? Lu O2 C13 C12 7.5(4) . . . . ? Lu O2 C13 C14 -172.89(18) . . . . ? C17 C12 C13 O2 179.3(2) . . . . ? S C12 C13 O2 0.3(3) . . . . ? C17 C12 C13 C14 -0.3(4) . . . . ? S C12 C13 C14 -179.36(19) . . . . ? O2 C13 C14 C15 -179.9(2) . . . . ? C12 C13 C14 C15 -0.3(4) . . . . ? O2 C13 C14 C19 2.7(4) . . . . ? C12 C13 C14 C19 -177.7(2) . . . . ? C13 C14 C15 C16 0.2(4) . . . . ? C19 C14 C15 C16 177.5(3) . . . . ? C14 C15 C16 C17 0.6(4) . . . . ? C14 C15 C16 C18 -178.2(3) . . . . ? C15 C16 C17 C12 -1.2(4) . . . . ? C18 C16 C17 C12 177.6(3) . . . . ? C13 C12 C17 C16 1.1(4) . . . . ? S C12 C17 C16 -179.8(2) . . . . ? C15 C14 C19 C22 -114.2(3) . . . . ? C13 C14 C19 C22 63.1(3) . . . . ? C15 C14 C19 C20 4.8(4) . . . . ? C13 C14 C19 C20 -177.9(3) . . . . ? C15 C14 C19 C21 124.8(3) . . . . ? C13 C14 C19 C21 -57.9(3) . . . . ? C26 O3 C23 C24 -39.4(3) . . . . ? Lu O3 C23 C24 113.9(3) . . . . ? O3 C23 C24 C25 21.7(3) . . . . ? C23 C24 C25 C26 2.9(4) . . . . ? C23 O3 C26 C25 41.5(3) . . . . ? Lu O3 C26 C25 -117.1(2) . . . . ? C24 C25 C26 O3 -26.7(3) . . . . ? C30 O4 C27 C28 6.9(5) . . . . ? Lu O4 C27 C28 -176.2(3) . . . . ? O4 C27 C28 C29 -12.6(7) . . . . ? C27 C28 C29 C30 13.6(8) . . . . ? C27 O4 C30 C29 1.3(5) . . . . ? Lu O4 C30 C29 -175.6(3) . . . . ? C28 C29 C30 O4 -9.2(7) . . . . ? C34 O5 C31 C32 22.8(5) . . . . ? O5 C31 C32 C33 -33.8(5) . . . . ? C31 C32 C33 C34 31.5(5) . . . . ? C31 O5 C34 C33 -2.3(5) . . . . ? C32 C33 C34 O5 -18.8(5) . . . . ? C35 C36 C37 C38 178.8(13) . . . . ? C36 C37 C38 C39 173.7(18) . . . . ? C40 C41 C42 C43 -61(6) . . . . ? C41 C42 C43 C44 -54(3) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.783 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.107