Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 _publ_contact_author_name 'Prof Jun Okuda' _publ_contact_author_address ; Institut or Inorganic Chemie RWTH Aachen Professor-Pirlet-Strasse 1 Aachen D 52056 GERMANY ; _publ_contact_author_phone '049 6131 39 23737' _publ_contact_author_fax '049 6131 39 25605' _publ_contact_author_email okuda@uni-mainz.de _publ_requested_journal 'Dalton Transactions' _publ_requested_coeditor_name ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; Rare earth metal complexes supported by 1,\w-dithiaalkanediyl-bridged bis(phenolato) ligands: synthesis, characterization and ring-opening polymerization catalysis of L-lactide ; loop_ _publ_author_name _publ_author_address 'Ma, Haiyan' ; Institut fur Anorganische Chemie und Analytische Chemie Johannes Gutenberg Universitat Mainz Duesbergweg 10-14 D-55099 Mainz Germany ; 'Spaniol, Thomas P.' ; Institut fur Anorganische Chemie und Analytische Chemie Johannes Gutenberg Universitat Mainz Duesbergweg 10-14 D-55099 Mainz Germany ; 'Okuda, Jun' ; Institut fur Anorganische Chemie und Analytische Chemie Johannes Gutenberg Universitat Mainz Duesbergweg 10-14 D-55099 Mainz Germany ; #========================================================================= data_hm8 _database_code_CSD 220241 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H56 N O3 S2 Sc Si2' _chemical_formula_weight 680.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Sc Sc 0.2519 0.3716 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.951(3) _cell_length_b 11.127(4) _cell_length_c 20.548(2) _cell_angle_alpha 102.28(2) _cell_angle_beta 99.60(2) _cell_angle_gamma 95.03(3) _cell_volume 1955.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.3 _cell_measurement_theta_max 10.9 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 0.386 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.6428 _exptl_absorpt_correction_T_max 0.9248 _exptl_absorpt_process_details psi-scans _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 (Enraf nonius)' _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 -7 6 -1 -1 -14 -6 3 3 _diffrn_standards_interval_count 242 _diffrn_standards_interval_time 119 _diffrn_standards_corr_method 'STDANAL linear fit' _diffrn_standards_corr_fact_max 1.201 _diffrn_standards_corr_fact_min 1.012 _diffrn_standards_decay_% 17 _diffrn_reflns_number 15277 _diffrn_reflns_av_R_equivalents 0.0736 _diffrn_reflns_av_sigmaI/netI 0.1007 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.98 _reflns_number_total 7643 _reflns_number_gt 3913 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' #_computing_structure_solution 'SHELXS-97 (Sheldrick, 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^)+(0.1541P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7643 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1609 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.2630 _refine_ls_wR_factor_gt 0.1957 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc Sc 0.11863(12) 0.14830(9) 0.26536(5) 0.0396(3) Uani 1 1 d . . . S1 S -0.18377(18) 0.05051(14) 0.23276(9) 0.0552(4) Uani 1 1 d . . . S2 S 0.1327(2) 0.00176(15) 0.13503(8) 0.0596(5) Uani 1 1 d . . . Si1 Si 0.1452(2) 0.39257(16) 0.38355(9) 0.0576(5) Uani 1 1 d . . . H1 H 0.215(6) 0.428(5) 0.328(3) 0.057(17) Uiso 1 1 d . . . Si2 Si 0.0335(3) 0.14790(18) 0.41377(9) 0.0646(6) Uani 1 1 d . . . H2 H -0.012(5) 0.022(4) 0.376(2) 0.039(14) Uiso 1 1 d . . . O1 O 0.0090(4) 0.2489(3) 0.20721(18) 0.0415(9) Uani 1 1 d . . . O2 O 0.2060(5) -0.0076(3) 0.27692(19) 0.0495(10) Uani 1 1 d . . . O3 O 0.3441(4) 0.2325(4) 0.2601(2) 0.0521(10) Uani 1 1 d . . . N N 0.1018(6) 0.2353(4) 0.3630(2) 0.0524(13) Uani 1 1 d . . . C1 C -0.1287(6) 0.2304(5) 0.1671(3) 0.0412(13) Uani 1 1 d . . . C2 C -0.2365(6) 0.1350(5) 0.1699(3) 0.0443(13) Uani 1 1 d . . . C3 C -0.3802(7) 0.1113(6) 0.1293(3) 0.0518(16) Uani 1 1 d . . . H3 H -0.435(6) 0.058(5) 0.135(3) 0.041(17) Uiso 1 1 d . . . C4 C -0.4215(7) 0.1819(6) 0.0825(3) 0.0543(15) Uani 1 1 d . . . C5 C -0.3160(7) 0.2779(6) 0.0815(3) 0.0499(15) Uani 1 1 d . . . H5 H -0.344(6) 0.321(5) 0.050(3) 0.048(16) Uiso 1 1 d . . . C6 C -0.1702(6) 0.3081(5) 0.1213(3) 0.0396(12) Uani 1 1 d . . . C7 C -0.5775(7) 0.1553(7) 0.0356(4) 0.076(2) Uani 1 1 d . . . H7A H -0.6139 0.2321 0.0307 0.113 Uiso 1 1 calc R . . H7B H -0.6481 0.1094 0.0545 0.113 Uiso 1 1 calc R . . H7C H -0.5686 0.1076 -0.0081 0.113 Uiso 1 1 calc R . . C8 C -0.0587(7) 0.4144(5) 0.1151(3) 0.0441(13) Uani 1 1 d . . . C9 C 0.0788(7) 0.3613(6) 0.0898(4) 0.0638(18) Uani 1 1 d . . . H9A H 0.1159 0.3055 0.1167 0.096 Uiso 1 1 calc R . . H9B H 0.1582 0.4278 0.0938 0.096 Uiso 1 1 calc R . . H9C H 0.0485 0.3175 0.0432 0.096 Uiso 1 1 calc R . . C10 C -0.0055(9) 0.5066(5) 0.1849(3) 0.0667(19) Uani 1 1 d . . . H10A H 0.0393 0.4635 0.2175 0.100 Uiso 1 1 calc R . . H10B H -0.0915 0.5425 0.1994 0.100 Uiso 1 1 calc R . . H10C H 0.0689 0.5710 0.1810 0.100 Uiso 1 1 calc R . . C11 C -0.1284(8) 0.4879(6) 0.0652(4) 0.0658(19) Uani 1 1 d . . . H11A H -0.0537 0.5540 0.0635 0.099 Uiso 1 1 calc R . . H11B H -0.2153 0.5220 0.0800 0.099 Uiso 1 1 calc R . . H11C H -0.1600 0.4339 0.0209 0.099 Uiso 1 1 calc R . . C12 C -0.2296(9) -0.1095(6) 0.1868(5) 0.085(3) Uani 1 1 d . . . H12A H -0.2515 -0.1591 0.2184 0.102 Uiso 1 1 calc R . . H12B H -0.3225 -0.1168 0.1535 0.102 Uiso 1 1 calc R . . C13 C -0.1111(9) -0.1634(7) 0.1514(6) 0.103(4) Uani 1 1 d . . . H13A H -0.1520 -0.2481 0.1278 0.123 Uiso 1 1 calc R . . H13B H -0.0247 -0.1678 0.1858 0.123 Uiso 1 1 calc R . . C14 C -0.0493(9) -0.0997(8) 0.0998(4) 0.093(3) Uani 1 1 d . . . H14A H -0.1249 -0.0508 0.0829 0.112 Uiso 1 1 calc R . . H14B H -0.0353 -0.1630 0.0616 0.112 Uiso 1 1 calc R . . C15 C 0.2445(7) -0.1033(5) 0.1669(3) 0.0457(14) Uani 1 1 d . . . C16 C 0.2672(6) -0.0946(5) 0.2381(3) 0.0413(13) Uani 1 1 d . . . C17 C 0.3491(7) -0.1825(5) 0.2644(3) 0.0493(15) Uani 1 1 d . . . C18 C 0.4076(7) -0.2685(6) 0.2191(4) 0.0575(17) Uani 1 1 d . . . H18 H 0.461(6) -0.325(5) 0.241(3) 0.041(14) Uiso 1 1 d . . . C19 C 0.3910(7) -0.2768(5) 0.1495(3) 0.0522(15) Uani 1 1 d . . . C20 C 0.3080(7) -0.1921(6) 0.1248(4) 0.0525(15) Uani 1 1 d . . . H20 H 0.292(6) -0.191(5) 0.078(3) 0.039(15) Uiso 1 1 d . . . C21 C 0.4605(8) -0.3725(6) 0.1062(4) 0.072(2) Uani 1 1 d . . . H21A H 0.4006 -0.3945 0.0611 0.107 Uiso 1 1 calc R . . H21B H 0.4632 -0.4447 0.1248 0.107 Uiso 1 1 calc R . . H21C H 0.5626 -0.3400 0.1048 0.107 Uiso 1 1 calc R . . C22 C 0.3685(9) -0.1846(6) 0.3397(3) 0.067(2) Uani 1 1 d . . . C23 C 0.2096(11) -0.2105(7) 0.3564(4) 0.088(3) Uani 1 1 d . . . H23A H 0.1587 -0.2879 0.3279 0.132 Uiso 1 1 calc R . . H23B H 0.1509 -0.1450 0.3486 0.132 Uiso 1 1 calc R . . H23C H 0.2200 -0.2146 0.4031 0.132 Uiso 1 1 calc R . . C24 C 0.4550(11) -0.0601(7) 0.3849(4) 0.102(3) Uani 1 1 d . . . H24A H 0.3934 0.0053 0.3806 0.153 Uiso 1 1 calc R . . H24B H 0.5497 -0.0423 0.3706 0.153 Uiso 1 1 calc R . . H24C H 0.4753 -0.0662 0.4314 0.153 Uiso 1 1 calc R . . C25 C 0.4617(11) -0.2882(7) 0.3557(4) 0.098(3) Uani 1 1 d . . . H25A H 0.4680 -0.2899 0.4026 0.147 Uiso 1 1 calc R . . H25B H 0.5627 -0.2726 0.3468 0.147 Uiso 1 1 calc R . . H25C H 0.4125 -0.3666 0.3277 0.147 Uiso 1 1 calc R . . C26 C 0.2851(11) 0.4535(8) 0.4634(4) 0.109(3) Uani 1 1 d . . . H26A H 0.2425 0.4355 0.5006 0.164 Uiso 1 1 calc R . . H26B H 0.3090 0.5416 0.4702 0.164 Uiso 1 1 calc R . . H26C H 0.3766 0.4150 0.4608 0.164 Uiso 1 1 calc R . . C27 C -0.0173(9) 0.4815(7) 0.3860(5) 0.090(3) Uani 1 1 d . . . H27A H -0.0785 0.4663 0.3413 0.135 Uiso 1 1 calc R . . H27B H 0.0194 0.5684 0.4016 0.135 Uiso 1 1 calc R . . H27C H -0.0781 0.4565 0.4163 0.135 Uiso 1 1 calc R . . C28 C -0.1438(10) 0.1938(8) 0.4414(5) 0.095(3) Uani 1 1 d . . . H28A H -0.1201 0.2700 0.4756 0.142 Uiso 1 1 calc R . . H28B H -0.1888 0.1300 0.4597 0.142 Uiso 1 1 calc R . . H28C H -0.2144 0.2053 0.4033 0.142 Uiso 1 1 calc R . . C29 C 0.1796(12) 0.1442(10) 0.4894(5) 0.130(4) Uani 1 1 d . . . H29A H 0.2800 0.1598 0.4799 0.196 Uiso 1 1 calc R . . H29B H 0.1668 0.0642 0.4997 0.196 Uiso 1 1 calc R . . H29C H 0.1671 0.2068 0.5276 0.196 Uiso 1 1 calc R . . C30 C 0.4754(8) 0.2203(7) 0.3069(4) 0.085(3) Uani 1 1 d . . . H30A H 0.5253 0.1508 0.2878 0.101 Uiso 1 1 calc R . . H30B H 0.4474 0.2076 0.3488 0.101 Uiso 1 1 calc R . . C31 C 0.5763(10) 0.3373(10) 0.3192(5) 0.116(4) Uani 1 1 d . . . H31A H 0.5550 0.3971 0.3573 0.140 Uiso 1 1 calc R . . H31B H 0.6825 0.3239 0.3291 0.140 Uiso 1 1 calc R . . C32 C 0.5446(8) 0.3818(6) 0.2570(4) 0.074(2) Uani 1 1 d . . . H32A H 0.6143 0.3539 0.2272 0.089 Uiso 1 1 calc R . . H32B H 0.5545 0.4717 0.2672 0.089 Uiso 1 1 calc R . . C33 C 0.3850(7) 0.3279(6) 0.2251(4) 0.0600(17) Uani 1 1 d . . . H33A H 0.3173 0.3912 0.2301 0.072 Uiso 1 1 calc R . . H33B H 0.3777 0.2920 0.1772 0.072 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 Sc 0.0443(6) 0.0352(5) 0.0357(6) 0.0088(4) -0.0005(5) 0.0002(4) S1 0.0528(9) 0.0520(9) 0.0622(10) 0.0274(8) 0.0034(8) -0.0060(7) S2 0.0875(13) 0.0520(9) 0.0415(9) 0.0144(7) 0.0067(8) 0.0226(8) Si1 0.0584(11) 0.0530(10) 0.0516(11) -0.0047(8) 0.0122(9) -0.0064(8) Si2 0.0859(14) 0.0641(12) 0.0447(10) 0.0202(9) 0.0073(10) 0.0055(10) O1 0.043(2) 0.0370(19) 0.041(2) 0.0129(16) -0.0017(17) -0.0037(16) O2 0.064(3) 0.041(2) 0.044(2) 0.0143(18) 0.0035(19) 0.0107(19) O3 0.043(2) 0.052(2) 0.063(3) 0.020(2) 0.005(2) 0.0054(18) N 0.062(3) 0.045(3) 0.044(3) 0.003(2) 0.004(2) -0.001(2) C1 0.042(3) 0.034(3) 0.045(3) 0.006(2) 0.009(3) 0.000(2) C2 0.044(3) 0.041(3) 0.047(3) 0.011(2) 0.007(3) 0.001(2) C3 0.045(4) 0.057(4) 0.051(4) 0.013(3) 0.009(3) -0.007(3) C4 0.042(3) 0.069(4) 0.046(4) 0.009(3) -0.001(3) 0.005(3) C5 0.052(4) 0.057(4) 0.042(3) 0.014(3) 0.006(3) 0.009(3) C6 0.043(3) 0.040(3) 0.039(3) 0.011(2) 0.012(2) 0.011(2) C7 0.046(4) 0.106(6) 0.064(5) 0.015(4) -0.010(3) 0.003(4) C8 0.058(4) 0.042(3) 0.036(3) 0.018(2) 0.003(3) 0.009(3) C9 0.061(4) 0.072(4) 0.067(4) 0.031(4) 0.017(4) 0.008(3) C10 0.095(5) 0.042(3) 0.063(4) 0.019(3) 0.011(4) -0.002(3) C11 0.077(5) 0.060(4) 0.068(4) 0.038(3) 0.005(4) 0.011(3) C12 0.070(5) 0.047(4) 0.127(7) 0.023(4) -0.007(5) -0.015(4) C13 0.060(5) 0.043(4) 0.181(11) 0.005(5) -0.017(6) 0.003(4) C14 0.082(6) 0.094(6) 0.068(5) -0.035(5) -0.033(4) 0.042(5) C15 0.051(3) 0.042(3) 0.042(3) 0.013(2) 0.001(3) 0.002(3) C16 0.046(3) 0.036(3) 0.042(3) 0.011(2) 0.005(3) 0.002(2) C17 0.060(4) 0.041(3) 0.043(3) 0.014(3) -0.006(3) 0.001(3) C18 0.052(4) 0.038(3) 0.082(5) 0.021(3) 0.001(3) 0.007(3) C19 0.047(3) 0.045(3) 0.063(4) 0.008(3) 0.010(3) 0.003(3) C20 0.051(4) 0.050(3) 0.057(4) 0.008(3) 0.018(3) 0.005(3) C21 0.060(4) 0.061(4) 0.090(6) 0.005(4) 0.014(4) 0.016(3) C22 0.104(6) 0.045(3) 0.046(4) 0.016(3) -0.007(4) 0.011(4) C23 0.146(8) 0.070(5) 0.059(5) 0.033(4) 0.023(5) 0.019(5) C24 0.149(8) 0.061(5) 0.071(5) 0.009(4) -0.041(5) 0.015(5) C25 0.145(8) 0.068(5) 0.083(6) 0.039(4) -0.007(5) 0.034(5) C26 0.100(7) 0.103(7) 0.089(7) -0.014(5) -0.020(5) -0.024(5) C27 0.079(5) 0.056(4) 0.134(8) 0.011(5) 0.035(5) 0.001(4) C28 0.112(7) 0.096(6) 0.099(7) 0.050(5) 0.045(6) 0.023(5) C29 0.140(9) 0.158(9) 0.088(7) 0.071(7) -0.034(6) -0.009(7) C30 0.049(4) 0.096(6) 0.110(7) 0.056(5) -0.013(4) -0.008(4) C31 0.077(6) 0.145(9) 0.116(8) 0.063(7) -0.028(5) -0.039(6) C32 0.062(4) 0.060(4) 0.100(6) 0.026(4) 0.014(4) -0.002(3) C33 0.052(4) 0.067(4) 0.066(4) 0.024(3) 0.014(3) 0.006(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 Sc O1 2.004(4) . ? Sc O2 2.007(4) . ? Sc N 2.071(5) . ? Sc O3 2.179(4) . ? Sc S1 2.744(2) . ? Sc S2 2.853(2) . ? Sc Si1 3.198(2) . ? Sc Si2 3.265(2) . ? S1 C2 1.779(6) . ? S1 C12 1.805(7) . ? S2 C15 1.763(6) . ? S2 C14 1.841(9) . ? Si1 N 1.704(5) . ? Si1 C27 1.832(8) . ? Si1 C26 1.847(8) . ? Si2 N 1.717(5) . ? Si2 C28 1.849(9) . ? Si2 C29 1.868(8) . ? O1 C1 1.337(6) . ? O2 C16 1.335(6) . ? O3 C30 1.425(7) . ? O3 C33 1.456(7) . ? C1 C2 1.388(7) . ? C1 C6 1.435(7) . ? C2 C3 1.382(8) . ? C3 C4 1.390(9) . ? C4 C5 1.368(8) . ? C4 C7 1.525(8) . ? C5 C6 1.390(8) . ? C6 C8 1.519(7) . ? C8 C11 1.530(7) . ? C8 C9 1.530(9) . ? C8 C10 1.548(8) . ? C12 C13 1.483(12) . ? C13 C14 1.543(13) . ? C15 C20 1.395(8) . ? C15 C16 1.425(7) . ? C16 C17 1.416(7) . ? C17 C18 1.389(9) . ? C17 C22 1.534(8) . ? C18 C19 1.394(9) . ? C19 C20 1.377(9) . ? C19 C21 1.487(9) . ? C22 C23 1.534(11) . ? C22 C25 1.539(9) . ? C22 C24 1.551(9) . ? C30 C31 1.467(10) . ? C31 C32 1.460(11) . ? C32 C33 1.483(9) . ? 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 Sc O2 151.14(16) . . ? O1 Sc N 103.97(18) . . ? O2 Sc N 103.56(18) . . ? O1 Sc O3 93.56(15) . . ? O2 Sc O3 89.78(16) . . ? N Sc O3 100.58(18) . . ? O1 Sc S1 72.61(11) . . ? O2 Sc S1 97.54(12) . . ? N Sc S1 92.86(15) . . ? O3 Sc S1 162.78(12) . . ? O1 Sc S2 80.86(11) . . ? O2 Sc S2 71.03(12) . . ? N Sc S2 173.30(14) . . ? O3 Sc S2 83.58(12) . . ? S1 Sc S2 84.10(7) . . ? O1 Sc Si1 83.95(11) . . ? O2 Sc Si1 124.87(12) . . ? N Sc Si1 28.74(14) . . ? O3 Sc Si1 81.50(12) . . ? S1 Sc Si1 106.48(7) . . ? S2 Sc Si1 157.95(6) . . ? O1 Sc Si2 119.36(12) . . ? O2 Sc Si2 83.18(12) . . ? N Sc Si2 27.43(14) . . ? O3 Sc Si2 119.07(12) . . ? S1 Sc Si2 77.44(6) . . ? S2 Sc Si2 145.92(6) . . ? Si1 Sc Si2 56.12(5) . . ? C2 S1 C12 103.8(3) . . ? C2 S1 Sc 95.86(18) . . ? C12 S1 Sc 117.4(3) . . ? C15 S2 C14 100.2(3) . . ? C15 S2 Sc 94.9(2) . . ? C14 S2 Sc 109.4(3) . . ? N Si1 C27 116.0(3) . . ? N Si1 C26 114.1(4) . . ? C27 Si1 C26 108.2(4) . . ? N Si1 Sc 35.76(17) . . ? C27 Si1 Sc 119.0(3) . . ? C26 Si1 Sc 131.8(3) . . ? N Si2 C28 114.1(3) . . ? N Si2 C29 112.6(4) . . ? C28 Si2 C29 109.5(5) . . ? N Si2 Sc 33.76(16) . . ? C28 Si2 Sc 125.7(3) . . ? C29 Si2 Sc 122.8(4) . . ? C1 O1 Sc 133.1(3) . . ? C16 O2 Sc 135.3(3) . . ? C30 O3 C33 108.7(5) . . ? C30 O3 Sc 120.4(4) . . ? C33 O3 Sc 129.3(3) . . ? Si1 N Si2 125.5(3) . . ? Si1 N Sc 115.5(3) . . ? Si2 N Sc 118.8(2) . . ? O1 C1 C2 119.9(5) . . ? O1 C1 C6 121.7(4) . . ? C2 C1 C6 118.4(5) . . ? C3 C2 C1 122.2(6) . . ? C3 C2 S1 121.5(4) . . ? C1 C2 S1 116.2(4) . . ? C2 C3 C4 120.6(6) . . ? C5 C4 C3 116.6(6) . . ? C5 C4 C7 121.6(6) . . ? C3 C4 C7 121.7(6) . . ? C4 C5 C6 125.9(6) . . ? C5 C6 C1 116.1(5) . . ? C5 C6 C8 122.2(5) . . ? C1 C6 C8 121.6(5) . . ? C6 C8 C11 112.9(5) . . ? C6 C8 C9 108.7(5) . . ? C11 C8 C9 107.9(5) . . ? C6 C8 C10 110.1(5) . . ? C11 C8 C10 107.2(5) . . ? C9 C8 C10 110.0(5) . . ? C13 C12 S1 116.3(5) . . ? C12 C13 C14 119.5(7) . . ? C13 C14 S2 113.8(5) . . ? C20 C15 C16 120.8(6) . . ? C20 C15 S2 122.1(5) . . ? C16 C15 S2 117.1(4) . . ? O2 C16 C17 122.7(5) . . ? O2 C16 C15 119.1(5) . . ? C17 C16 C15 118.1(5) . . ? C18 C17 C16 117.4(6) . . ? C18 C17 C22 121.4(6) . . ? C16 C17 C22 121.1(6) . . ? C17 C18 C19 125.5(6) . . ? C20 C19 C18 116.0(6) . . ? C20 C19 C21 123.4(6) . . ? C18 C19 C21 120.5(6) . . ? C19 C20 C15 122.0(6) . . ? C17 C22 C23 108.5(6) . . ? C17 C22 C25 111.2(6) . . ? C23 C22 C25 108.0(6) . . ? C17 C22 C24 110.7(6) . . ? C23 C22 C24 111.1(7) . . ? C25 C22 C24 107.3(6) . . ? O3 C30 C31 105.3(6) . . ? C32 C31 C30 106.0(7) . . ? C31 C32 C33 105.1(6) . . ? O3 C33 C32 106.5(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 Sc S1 C2 11.3(2) . . . . ? O2 Sc S1 C2 -140.9(2) . . . . ? N Sc S1 C2 115.0(2) . . . . ? O3 Sc S1 C2 -26.4(5) . . . . ? S2 Sc S1 C2 -70.97(19) . . . . ? Si1 Sc S1 C2 89.3(2) . . . . ? Si2 Sc S1 C2 137.9(2) . . . . ? O1 Sc S1 C12 120.1(4) . . . . ? O2 Sc S1 C12 -32.1(4) . . . . ? N Sc S1 C12 -136.2(4) . . . . ? O3 Sc S1 C12 82.4(5) . . . . ? S2 Sc S1 C12 37.8(3) . . . . ? Si1 Sc S1 C12 -161.9(3) . . . . ? Si2 Sc S1 C12 -113.3(3) . . . . ? O1 Sc S2 C15 175.9(2) . . . . ? O2 Sc S2 C15 -10.8(2) . . . . ? N Sc S2 C15 -47.6(13) . . . . ? O3 Sc S2 C15 81.2(2) . . . . ? S1 Sc S2 C15 -110.9(2) . . . . ? Si1 Sc S2 C15 128.8(2) . . . . ? Si2 Sc S2 C15 -53.7(2) . . . . ? O1 Sc S2 C14 -81.5(3) . . . . ? O2 Sc S2 C14 91.9(3) . . . . ? N Sc S2 C14 55.1(14) . . . . ? O3 Sc S2 C14 -176.1(3) . . . . ? S1 Sc S2 C14 -8.2(3) . . . . ? Si1 Sc S2 C14 -128.5(3) . . . . ? Si2 Sc S2 C14 49.0(3) . . . . ? O1 Sc Si1 N 134.3(3) . . . . ? O2 Sc Si1 N -47.4(3) . . . . ? O3 Sc Si1 N -131.2(3) . . . . ? S1 Sc Si1 N 64.5(3) . . . . ? S2 Sc Si1 N -179.1(3) . . . . ? Si2 Sc Si1 N 2.6(3) . . . . ? O1 Sc Si1 C27 39.2(3) . . . . ? O2 Sc Si1 C27 -142.5(4) . . . . ? N Sc Si1 C27 -95.1(5) . . . . ? O3 Sc Si1 C27 133.7(3) . . . . ? S1 Sc Si1 C27 -30.6(3) . . . . ? S2 Sc Si1 C27 85.8(4) . . . . ? Si2 Sc Si1 C27 -92.5(3) . . . . ? O1 Sc Si1 C26 -153.6(5) . . . . ? O2 Sc Si1 C26 24.7(5) . . . . ? N Sc Si1 C26 72.1(5) . . . . ? O3 Sc Si1 C26 -59.1(5) . . . . ? S1 Sc Si1 C26 136.6(4) . . . . ? S2 Sc Si1 C26 -107.0(5) . . . . ? Si2 Sc Si1 C26 74.7(5) . . . . ? O1 Sc Si2 N -61.2(3) . . . . ? O2 Sc Si2 N 138.0(3) . . . . ? O3 Sc Si2 N 52.0(3) . . . . ? S1 Sc Si2 N -122.7(3) . . . . ? S2 Sc Si2 N 178.4(3) . . . . ? Si1 Sc Si2 N -2.7(3) . . . . ? O1 Sc Si2 C28 19.1(4) . . . . ? O2 Sc Si2 C28 -141.8(4) . . . . ? N Sc Si2 C28 80.2(5) . . . . ? O3 Sc Si2 C28 132.3(4) . . . . ? S1 Sc Si2 C28 -42.5(4) . . . . ? S2 Sc Si2 C28 -101.3(4) . . . . ? Si1 Sc Si2 C28 77.5(4) . . . . ? O1 Sc Si2 C29 -143.0(4) . . . . ? O2 Sc Si2 C29 56.1(4) . . . . ? N Sc Si2 C29 -81.9(5) . . . . ? O3 Sc Si2 C29 -29.8(4) . . . . ? S1 Sc Si2 C29 155.4(4) . . . . ? S2 Sc Si2 C29 96.6(4) . . . . ? Si1 Sc Si2 C29 -84.6(4) . . . . ? O2 Sc O1 C1 58.6(6) . . . . ? N Sc O1 C1 -103.6(5) . . . . ? O3 Sc O1 C1 154.6(5) . . . . ? S1 Sc O1 C1 -15.0(4) . . . . ? S2 Sc O1 C1 71.7(5) . . . . ? Si1 Sc O1 C1 -124.4(5) . . . . ? Si2 Sc O1 C1 -79.0(5) . . . . ? O1 Sc O2 C16 30.6(7) . . . . ? N Sc O2 C16 -167.3(5) . . . . ? O3 Sc O2 C16 -66.4(5) . . . . ? S1 Sc O2 C16 97.9(5) . . . . ? S2 Sc O2 C16 16.9(4) . . . . ? Si1 Sc O2 C16 -145.9(4) . . . . ? Si2 Sc O2 C16 174.3(5) . . . . ? O1 Sc O3 C30 164.0(5) . . . . ? O2 Sc O3 C30 -44.7(5) . . . . ? N Sc O3 C30 59.1(5) . . . . ? S1 Sc O3 C30 -160.2(5) . . . . ? S2 Sc O3 C30 -115.6(5) . . . . ? Si1 Sc O3 C30 80.7(5) . . . . ? Si2 Sc O3 C30 37.4(5) . . . . ? O1 Sc O3 C33 0.2(5) . . . . ? O2 Sc O3 C33 151.6(5) . . . . ? N Sc O3 C33 -104.7(5) . . . . ? S1 Sc O3 C33 36.0(7) . . . . ? S2 Sc O3 C33 80.6(5) . . . . ? Si1 Sc O3 C33 -83.1(5) . . . . ? Si2 Sc O3 C33 -126.4(5) . . . . ? C27 Si1 N Si2 -70.8(5) . . . . ? C26 Si1 N Si2 56.0(5) . . . . ? Sc Si1 N Si2 -174.9(6) . . . . ? C27 Si1 N Sc 104.2(4) . . . . ? C26 Si1 N Sc -129.1(4) . . . . ? C28 Si2 N Si1 56.1(5) . . . . ? C29 Si2 N Si1 -69.6(6) . . . . ? Sc Si2 N Si1 174.8(6) . . . . ? C28 Si2 N Sc -118.7(4) . . . . ? C29 Si2 N Sc 115.7(5) . . . . ? O1 Sc N Si1 -47.2(3) . . . . ? O2 Sc N Si1 141.6(3) . . . . ? O3 Sc N Si1 49.2(3) . . . . ? S1 Sc N Si1 -120.0(3) . . . . ? S2 Sc N Si1 177.2(11) . . . . ? Si2 Sc N Si1 -175.3(5) . . . . ? O1 Sc N Si2 128.1(3) . . . . ? O2 Sc N Si2 -43.1(3) . . . . ? O3 Sc N Si2 -135.5(3) . . . . ? S1 Sc N Si2 55.3(3) . . . . ? S2 Sc N Si2 -7.5(16) . . . . ? Si1 Sc N Si2 175.3(5) . . . . ? Sc O1 C1 C2 12.1(8) . . . . ? Sc O1 C1 C6 -168.9(4) . . . . ? O1 C1 C2 C3 -179.6(5) . . . . ? C6 C1 C2 C3 1.4(9) . . . . ? O1 C1 C2 S1 4.2(7) . . . . ? C6 C1 C2 S1 -174.8(4) . . . . ? C12 S1 C2 C3 52.5(6) . . . . ? Sc S1 C2 C3 172.5(5) . . . . ? C12 S1 C2 C1 -131.2(5) . . . . ? Sc S1 C2 C1 -11.2(4) . . . . ? C1 C2 C3 C4 1.2(10) . . . . ? S1 C2 C3 C4 177.2(5) . . . . ? C2 C3 C4 C5 -2.9(10) . . . . ? C2 C3 C4 C7 178.1(6) . . . . ? C3 C4 C5 C6 2.3(10) . . . . ? C7 C4 C5 C6 -178.7(6) . . . . ? C4 C5 C6 C1 0.1(9) . . . . ? C4 C5 C6 C8 178.1(6) . . . . ? O1 C1 C6 C5 179.0(5) . . . . ? C2 C1 C6 C5 -2.0(8) . . . . ? O1 C1 C6 C8 1.0(8) . . . . ? C2 C1 C6 C8 -180.0(5) . . . . ? C5 C6 C8 C11 4.2(8) . . . . ? C1 C6 C8 C11 -177.9(5) . . . . ? C5 C6 C8 C9 -115.5(6) . . . . ? C1 C6 C8 C9 62.3(7) . . . . ? C5 C6 C8 C10 124.0(6) . . . . ? C1 C6 C8 C10 -58.2(7) . . . . ? C2 S1 C12 C13 85.2(7) . . . . ? Sc S1 C12 C13 -19.0(8) . . . . ? S1 C12 C13 C14 -55.6(10) . . . . ? C12 C13 C14 S2 97.9(7) . . . . ? C15 S2 C14 C13 54.7(6) . . . . ? Sc S2 C14 C13 -44.3(6) . . . . ? C14 S2 C15 C20 77.9(6) . . . . ? Sc S2 C15 C20 -171.3(5) . . . . ? C14 S2 C15 C16 -101.7(5) . . . . ? Sc S2 C15 C16 9.1(4) . . . . ? Sc O2 C16 C17 166.5(4) . . . . ? Sc O2 C16 C15 -16.2(8) . . . . ? C20 C15 C16 O2 179.3(5) . . . . ? S2 C15 C16 O2 -1.0(7) . . . . ? C20 C15 C16 C17 -3.2(8) . . . . ? S2 C15 C16 C17 176.4(4) . . . . ? O2 C16 C17 C18 -180.0(5) . . . . ? C15 C16 C17 C18 2.7(8) . . . . ? O2 C16 C17 C22 1.6(8) . . . . ? C15 C16 C17 C22 -175.7(5) . . . . ? C16 C17 C18 C19 -0.8(9) . . . . ? C22 C17 C18 C19 177.5(6) . . . . ? C17 C18 C19 C20 -0.6(9) . . . . ? C17 C18 C19 C21 179.4(6) . . . . ? C18 C19 C20 C15 0.1(9) . . . . ? C21 C19 C20 C15 -179.9(6) . . . . ? C16 C15 C20 C19 1.8(9) . . . . ? S2 C15 C20 C19 -177.8(5) . . . . ? C18 C17 C22 C23 -116.9(7) . . . . ? C16 C17 C22 C23 61.4(7) . . . . ? C18 C17 C22 C25 1.8(9) . . . . ? C16 C17 C22 C25 -179.9(6) . . . . ? C18 C17 C22 C24 121.0(7) . . . . ? C16 C17 C22 C24 -60.7(9) . . . . ? C33 O3 C30 C31 21.2(9) . . . . ? Sc O3 C30 C31 -145.6(6) . . . . ? O3 C30 C31 C32 -29.7(10) . . . . ? C30 C31 C32 C33 26.4(10) . . . . ? C30 O3 C33 C32 -4.9(8) . . . . ? Sc O3 C33 C32 160.4(4) . . . . ? C31 C32 C33 O3 -13.5(9) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.775 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.099 #===END data_hm2 _database_code_CSD 220242 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H68 N O3 S2 Si2 Y' _chemical_formula_weight 808.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/C' 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 14.021(3) _cell_length_b 15.195(4) _cell_length_c 22.294(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.230(10) _cell_angle_gamma 90.00 _cell_volume 4700.8(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.2 _cell_measurement_theta_max 11.2 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 1.412 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.4846 _exptl_absorpt_correction_T_max 0.6378 _exptl_absorpt_process_details 'semi-empirical, psi-scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 (Enraf nonius)' _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 5 7 1 -5 7 5 -5 1 _diffrn_standards_interval_count 178 _diffrn_standards_interval_time 59 _diffrn_standards_corr_method 'STDANAL linear fit' _diffrn_standards_corr_fact_max 1.168 _diffrn_standards_corr_fact_min 1.006 _diffrn_standards_decay_% 14 _diffrn_reflns_number 11999 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_sigmaI/netI 0.2343 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 24.97 _reflns_number_total 8220 _reflns_number_gt 2938 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' #_computing_structure_solution 'SHELXS-97 (Sheldrick, 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^)+(0.0482P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8220 _refine_ls_number_parameters 557 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2478 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_ref 0.1470 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.942 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y Y 0.25363(5) 0.01298(4) 0.24239(3) 0.0620(3) Uani 1 1 d . . . Si1 Si 0.21754(18) 0.01303(17) 0.38716(10) 0.0924(8) Uani 1 1 d . . . Si2 Si 0.3807(2) 0.12690(18) 0.35314(12) 0.1074(10) Uani 1 1 d . . . S1 S 0.27896(16) -0.16832(12) 0.28897(8) 0.0760(6) Uani 1 1 d . . . S2 S 0.45421(14) -0.03948(12) 0.23012(8) 0.0740(6) Uani 1 1 d . . . O1 O 0.1592(3) -0.0812(3) 0.19223(19) 0.0662(14) Uani 1 1 d . . . O2 O 0.3115(4) 0.0883(3) 0.17540(19) 0.0660(13) Uani 1 1 d . . . O3 O 0.1208(4) 0.1122(3) 0.2279(3) 0.0858(16) Uani 1 1 d . . . N N 0.2873(4) 0.0561(4) 0.3392(2) 0.0704(17) Uani 1 1 d . . . C1 C 0.1591(5) -0.1669(5) 0.1822(3) 0.0563(19) Uani 1 1 d . . . C2 C 0.2122(5) -0.2206(5) 0.2253(3) 0.061(2) Uani 1 1 d . . . C3 C 0.2166(6) -0.3115(6) 0.2182(4) 0.077(3) Uani 1 1 d . . . H3 H 0.248(4) -0.339(3) 0.250(2) 0.05(2) Uiso 1 1 d . . . C4 C 0.1712(6) -0.3517(5) 0.1677(4) 0.071(2) Uani 1 1 d . A . C5 C 0.1184(6) -0.2988(6) 0.1252(4) 0.073(2) Uani 1 1 d . . . H5 H 0.088(4) -0.322(3) 0.088(2) 0.041(18) Uiso 1 1 d . . . C6 C 0.1107(5) -0.2086(5) 0.1295(3) 0.061(2) Uani 1 1 d . . . C7 C 0.1846(9) -0.4512(6) 0.1584(5) 0.095(3) Uani 1 1 d . . . C8A C 0.133(7) -0.495(3) 0.206(3) 0.28(5) Uani 0.50 1 d P A 1 H8A1 H 0.1637 -0.4782 0.2457 0.423 Uiso 0.50 1 calc PR A 1 H8A2 H 0.1369 -0.5580 0.2019 0.423 Uiso 0.50 1 calc PR A 1 H8A3 H 0.0670 -0.4773 0.2006 0.423 Uiso 0.50 1 calc PR A 1 C9A C 0.290(3) -0.470(3) 0.171(3) 0.19(3) Uani 0.50 1 d P A 1 H9A1 H 0.3180 -0.4377 0.2067 0.290 Uiso 0.50 1 calc PR A 1 H9A2 H 0.3208 -0.4519 0.1373 0.290 Uiso 0.50 1 calc PR A 1 H9A3 H 0.3004 -0.5317 0.1782 0.290 Uiso 0.50 1 calc PR A 1 C10A C 0.141(3) -0.488(2) 0.0988(12) 0.117(12) Uani 0.50 1 d P A 1 H10A H 0.1490 -0.5506 0.0990 0.175 Uiso 0.50 1 calc PR A 1 H10B H 0.1721 -0.4627 0.0672 0.175 Uiso 0.50 1 calc PR A 1 H10C H 0.0734 -0.4738 0.0917 0.175 Uiso 0.50 1 calc PR A 1 C8B C 0.196(4) -0.505(3) 0.2113(16) 0.16(2) Uani 0.50 1 d P A 2 H8B1 H 0.1902 -0.5656 0.1998 0.246 Uiso 0.50 1 calc PR A 2 H8B2 H 0.1462 -0.4904 0.2354 0.246 Uiso 0.50 1 calc PR A 2 H8B3 H 0.2577 -0.4942 0.2345 0.246 Uiso 0.50 1 calc PR A 2 C9B C 0.271(4) -0.463(3) 0.124(2) 0.19(3) Uani 0.50 1 d P A 2 H9B1 H 0.2876 -0.5240 0.1227 0.289 Uiso 0.50 1 calc PR A 2 H9B2 H 0.3255 -0.4307 0.1445 0.289 Uiso 0.50 1 calc PR A 2 H9B3 H 0.2553 -0.4407 0.0835 0.289 Uiso 0.50 1 calc PR A 2 C10B C 0.102(4) -0.486(3) 0.123(4) 0.32(5) Uani 0.50 1 d P A 2 H10D H 0.1139 -0.5454 0.1116 0.473 Uiso 0.50 1 calc PR A 2 H10E H 0.0859 -0.4509 0.0869 0.473 Uiso 0.50 1 calc PR A 2 H10F H 0.0487 -0.4850 0.1457 0.473 Uiso 0.50 1 calc PR A 2 C11 C 0.0524(6) -0.1529(5) 0.0800(3) 0.075(2) Uani 1 1 d . . . C12 C -0.0355(5) -0.1144(6) 0.1053(4) 0.114(3) Uani 1 1 d . . . H12A H -0.0145 -0.0870 0.1438 0.171 Uiso 1 1 calc R . . H12B H -0.0801 -0.1607 0.1105 0.171 Uiso 1 1 calc R . . H12C H -0.0665 -0.0714 0.0776 0.171 Uiso 1 1 calc R . . C13 C 0.1129(5) -0.0792(5) 0.0590(3) 0.092(3) Uani 1 1 d . . . H13A H 0.1311 -0.0390 0.0919 0.138 Uiso 1 1 calc R . . H13B H 0.0761 -0.0485 0.0258 0.138 Uiso 1 1 calc R . . H13C H 0.1698 -0.1035 0.0460 0.138 Uiso 1 1 calc R . . C14 C 0.0147(6) -0.2089(6) 0.0241(4) 0.121(3) Uani 1 1 d . . . H14A H -0.0110 -0.1710 -0.0087 0.181 Uiso 1 1 calc R . . H14B H -0.0349 -0.2477 0.0337 0.181 Uiso 1 1 calc R . . H14C H 0.0667 -0.2430 0.0123 0.181 Uiso 1 1 calc R . . C15 C 0.4011(7) -0.2114(7) 0.2894(5) 0.093(3) Uani 1 1 d . . . H15A H 0.442(5) -0.180(4) 0.319(3) 0.08(3) Uiso 1 1 d . . . H15B H 0.396(4) -0.264(4) 0.309(3) 0.06(2) Uiso 1 1 d . . . C16 C 0.4371(8) -0.2196(6) 0.2290(5) 0.086(3) Uani 1 1 d . . . H16A H 0.403(4) -0.275(4) 0.201(3) 0.08(2) Uiso 1 1 d . . . H16B H 0.493(5) -0.230(5) 0.242(4) 0.09(3) Uiso 1 1 d . . . C17 C 0.4199(7) -0.1405(5) 0.1876(4) 0.078(3) Uani 1 1 d . . . H17A H 0.362(4) -0.115(3) 0.168(2) 0.04(2) Uiso 1 1 d . . . H17B H 0.457(4) -0.148(3) 0.150(2) 0.061(19) Uiso 1 1 d . . . C18 C 0.4681(6) 0.0356(4) 0.1702(3) 0.065(2) Uani 1 1 d . . . C19 C 0.3926(5) 0.0936(5) 0.1523(3) 0.0538(19) Uani 1 1 d . . . C20 C 0.4088(5) 0.1578(5) 0.1089(3) 0.0530(18) Uani 1 1 d . . . C21 C 0.4926(7) 0.1523(6) 0.0839(3) 0.067(2) Uani 1 1 d . . . H21 H 0.499(3) 0.193(3) 0.056(2) 0.021(16) Uiso 1 1 d . . . C22 C 0.5648(6) 0.0906(6) 0.0978(4) 0.068(2) Uani 1 1 d . B . C23 C 0.5510(6) 0.0339(6) 0.1437(4) 0.068(2) Uani 1 1 d . . . H23 H 0.590(5) -0.012(4) 0.153(3) 0.08(3) Uiso 1 1 d . . . C24 C 0.6522(7) 0.0882(7) 0.0645(4) 0.085(3) Uani 1 1 d . . . C25A C 0.722(2) 0.018(3) 0.0923(16) 0.138(10) Uani 0.50 1 d P B 1 H25A H 0.7841 0.0281 0.0802 0.208 Uiso 0.50 1 calc PR B 1 H25B H 0.6986 -0.0388 0.0787 0.208 Uiso 0.50 1 calc PR B 1 H25C H 0.7273 0.0210 0.1357 0.208 Uiso 0.50 1 calc PR B 1 C26A C 0.705(2) 0.1709(17) 0.0708(14) 0.091(9) Uani 0.50 1 d P B 1 H26A H 0.6617 0.2190 0.0605 0.137 Uiso 0.50 1 calc PR B 1 H26B H 0.7534 0.1707 0.0441 0.137 Uiso 0.50 1 calc PR B 1 H26C H 0.7361 0.1773 0.1119 0.137 Uiso 0.50 1 calc PR B 1 C27A C 0.6200(18) 0.063(2) 0.0001(11) 0.102(10) Uani 0.50 1 d P B 1 H27A H 0.6748 0.0464 -0.0185 0.153 Uiso 0.50 1 calc PR B 1 H27B H 0.5886 0.1126 -0.0212 0.153 Uiso 0.50 1 calc PR B 1 H27C H 0.5757 0.0149 -0.0014 0.153 Uiso 0.50 1 calc PR B 1 C25B C 0.743(2) 0.109(4) 0.105(2) 0.23(3) Uani 0.50 1 d P B 2 H25D H 0.7571 0.0623 0.1340 0.345 Uiso 0.50 1 calc PR B 2 H25E H 0.7358 0.1632 0.1255 0.345 Uiso 0.50 1 calc PR B 2 H25F H 0.7946 0.1139 0.0811 0.345 Uiso 0.50 1 calc PR B 2 C26B C 0.642(3) 0.152(4) 0.008(2) 0.28(3) Uani 0.50 1 d P B 2 H26D H 0.6764 0.2062 0.0193 0.425 Uiso 0.50 1 calc PR B 2 H26E H 0.5756 0.1652 -0.0050 0.425 Uiso 0.50 1 calc PR B 2 H26F H 0.6695 0.1250 -0.0245 0.425 Uiso 0.50 1 calc PR B 2 C27B C 0.668(3) -0.004(2) 0.042(3) 0.19(2) Uani 0.50 1 d P B 2 H27D H 0.7160 -0.0023 0.0155 0.289 Uiso 0.50 1 calc PR B 2 H27E H 0.6084 -0.0255 0.0202 0.289 Uiso 0.50 1 calc PR B 2 H27F H 0.6885 -0.0414 0.0758 0.289 Uiso 0.50 1 calc PR B 2 C28 C 0.3322(6) 0.2308(5) 0.0912(3) 0.074(2) Uani 1 1 d . . . C29 C 0.3084(5) 0.2771(5) 0.1472(3) 0.093(3) Uani 1 1 d . . . H29A H 0.3624 0.3121 0.1644 0.140 Uiso 1 1 calc R . . H29B H 0.2943 0.2342 0.1763 0.140 Uiso 1 1 calc R . . H29C H 0.2533 0.3143 0.1365 0.140 Uiso 1 1 calc R . . C30 C 0.2429(6) 0.1886(5) 0.0558(3) 0.109(3) Uani 1 1 d . . . H30A H 0.2201 0.1426 0.0796 0.163 Uiso 1 1 calc R . . H30B H 0.2588 0.1642 0.0187 0.163 Uiso 1 1 calc R . . H30C H 0.1935 0.2322 0.0466 0.163 Uiso 1 1 calc R . . C31 C 0.3685(6) 0.3014(5) 0.0514(4) 0.111(3) Uani 1 1 d . . . H31A H 0.3200 0.3459 0.0424 0.166 Uiso 1 1 calc R . . H31B H 0.3821 0.2752 0.0144 0.166 Uiso 1 1 calc R . . H31C H 0.4261 0.3274 0.0724 0.166 Uiso 1 1 calc R . . C32 C 0.1533(7) 0.0954(6) 0.4284(4) 0.147(4) Uani 1 1 d . . . H32A H 0.1992 0.1274 0.4562 0.220 Uiso 1 1 calc R . . H32B H 0.1087 0.0657 0.4503 0.220 Uiso 1 1 calc R . . H32C H 0.1189 0.1355 0.3999 0.220 Uiso 1 1 calc R . . C33 C 0.2796(7) -0.0659(6) 0.4419(4) 0.159(4) Uani 1 1 d . . . H33A H 0.3330 -0.0914 0.4256 0.239 Uiso 1 1 calc R . . H33B H 0.2355 -0.1115 0.4495 0.239 Uiso 1 1 calc R . . H33C H 0.3026 -0.0360 0.4791 0.239 Uiso 1 1 calc R . . C34 C 0.3463(7) 0.2422(5) 0.3693(4) 0.151(4) Uani 1 1 d . . . H34A H 0.3177 0.2699 0.3323 0.227 Uiso 1 1 calc R . . H34B H 0.4027 0.2744 0.3862 0.227 Uiso 1 1 calc R . . H34C H 0.3008 0.2417 0.3976 0.227 Uiso 1 1 calc R . . C35 C 0.4766(6) 0.0899(8) 0.4124(4) 0.173(5) Uani 1 1 d . . . H35A H 0.4515 0.0846 0.4501 0.259 Uiso 1 1 calc R . . H35B H 0.5282 0.1319 0.4167 0.259 Uiso 1 1 calc R . . H35C H 0.5003 0.0337 0.4014 0.259 Uiso 1 1 calc R . . C36 C 0.1030(9) 0.1862(8) 0.2622(5) 0.173(5) Uani 1 1 d . . . H36A H 0.1630 0.2168 0.2754 0.207 Uiso 1 1 calc R . . H36B H 0.0762 0.1678 0.2979 0.207 Uiso 1 1 calc R . . C37 C 0.0382(9) 0.2431(7) 0.2273(7) 0.155(5) Uani 1 1 d . . . H37A H 0.0703 0.2976 0.2195 0.186 Uiso 1 1 calc R . . H37B H -0.0154 0.2568 0.2488 0.186 Uiso 1 1 calc R . . C38 C 0.0046(9) 0.1993(9) 0.1718(6) 0.183(6) Uani 1 1 d . . . H38A H 0.0208 0.2331 0.1377 0.219 Uiso 1 1 calc R . . H38B H -0.0648 0.1921 0.1671 0.219 Uiso 1 1 calc R . . C39 C 0.0519(8) 0.1143(7) 0.1746(5) 0.155(5) Uani 1 1 d . . . H39A H 0.0049 0.0678 0.1758 0.186 Uiso 1 1 calc R . . H39B H 0.0835 0.1058 0.1391 0.186 Uiso 1 1 calc R . . H1 H 0.127(3) -0.047(2) 0.3568(16) 0.026(12) Uiso 1 1 d . . . H2 H 0.420(4) 0.131(4) 0.298(3) 0.11(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y 0.0676(5) 0.0579(4) 0.0620(5) 0.0023(4) 0.0145(4) 0.0095(5) Si1 0.101(2) 0.0961(18) 0.0841(16) -0.0085(15) 0.0272(15) 0.0037(17) Si2 0.115(2) 0.114(2) 0.099(2) -0.0301(17) 0.0361(19) -0.027(2) S1 0.0965(18) 0.0675(14) 0.0613(12) 0.0107(11) 0.0016(12) 0.0124(13) S2 0.0736(15) 0.0727(14) 0.0742(13) 0.0062(11) 0.0055(11) 0.0145(11) O1 0.068(4) 0.053(3) 0.075(3) 0.011(2) 0.001(3) 0.006(3) O2 0.060(3) 0.061(3) 0.080(3) 0.010(2) 0.019(3) 0.014(3) O3 0.077(4) 0.083(4) 0.099(4) 0.002(3) 0.017(4) 0.025(3) N 0.076(4) 0.073(4) 0.065(4) -0.003(3) 0.019(3) -0.003(4) C1 0.054(5) 0.050(5) 0.069(5) 0.012(5) 0.023(4) 0.007(4) C2 0.076(6) 0.045(5) 0.065(5) 0.005(4) 0.020(4) 0.006(4) C3 0.081(7) 0.077(7) 0.070(7) 0.021(6) 0.005(5) 0.021(5) C4 0.072(6) 0.059(6) 0.083(6) -0.002(5) 0.015(5) 0.002(5) C5 0.068(6) 0.079(7) 0.068(6) -0.008(6) -0.005(5) -0.006(5) C6 0.048(5) 0.065(6) 0.069(5) 0.005(5) 0.007(4) -0.007(4) C7 0.104(9) 0.060(6) 0.115(9) -0.009(7) -0.001(8) 0.017(6) C8A 0.48(12) 0.027(19) 0.39(7) 0.00(3) 0.26(7) -0.05(4) C9A 0.10(3) 0.08(3) 0.38(8) -0.09(4) -0.01(4) 0.06(2) C10A 0.13(3) 0.10(2) 0.108(16) -0.029(15) -0.002(16) 0.04(2) C8B 0.32(8) 0.08(2) 0.11(2) 0.011(16) 0.06(3) 0.05(3) C9B 0.27(8) 0.067(17) 0.29(5) -0.03(3) 0.21(6) 0.01(3) C10B 0.14(4) 0.08(3) 0.68(13) -0.18(5) -0.07(6) 0.07(3) C11 0.063(6) 0.079(6) 0.078(6) 0.015(5) -0.008(5) -0.005(5) C12 0.050(6) 0.134(8) 0.157(8) 0.043(7) 0.010(6) 0.021(6) C13 0.101(7) 0.096(6) 0.077(5) 0.028(5) 0.009(5) -0.008(6) C14 0.107(8) 0.131(8) 0.109(7) 0.008(6) -0.034(6) -0.026(6) C15 0.097(9) 0.072(7) 0.099(9) 0.027(7) -0.027(7) -0.002(6) C16 0.075(8) 0.069(7) 0.109(9) 0.007(6) -0.010(7) 0.025(6) C17 0.091(8) 0.076(6) 0.069(6) 0.003(5) 0.016(6) 0.027(6) C18 0.069(6) 0.063(5) 0.066(5) 0.003(4) 0.024(4) 0.007(5) C19 0.046(5) 0.060(5) 0.056(5) -0.009(4) 0.009(4) 0.007(4) C20 0.055(5) 0.061(5) 0.041(4) -0.002(4) 0.001(4) -0.014(4) C21 0.085(8) 0.071(6) 0.047(5) 0.000(5) 0.016(5) -0.016(6) C22 0.063(6) 0.072(6) 0.070(6) -0.020(5) 0.008(5) 0.001(5) C23 0.068(7) 0.060(6) 0.077(6) -0.016(5) 0.013(5) 0.015(5) C24 0.060(7) 0.111(8) 0.092(7) -0.022(7) 0.033(6) -0.006(7) C25A 0.09(2) 0.18(3) 0.15(3) -0.02(3) 0.057(19) 0.02(2) C26A 0.054(19) 0.096(17) 0.13(2) -0.061(14) 0.044(16) -0.048(14) C27A 0.103(19) 0.13(2) 0.085(16) -0.058(17) 0.061(15) -0.07(2) C25B 0.06(2) 0.37(8) 0.26(6) -0.17(5) 0.03(3) -0.05(4) C26B 0.14(3) 0.50(8) 0.23(4) 0.22(5) 0.13(3) 0.08(4) C27B 0.22(5) 0.12(2) 0.28(5) -0.09(3) 0.20(4) -0.03(3) C28 0.074(6) 0.079(6) 0.071(5) 0.017(5) 0.010(5) 0.003(5) C29 0.098(7) 0.069(5) 0.113(7) 0.005(5) 0.017(6) 0.026(5) C30 0.091(7) 0.119(7) 0.104(7) 0.016(6) -0.031(6) 0.002(6) C31 0.110(7) 0.097(6) 0.128(7) 0.045(6) 0.025(6) 0.015(6) C32 0.142(9) 0.181(10) 0.124(8) -0.038(7) 0.044(7) -0.001(8) C33 0.215(12) 0.172(10) 0.096(7) 0.029(7) 0.040(8) 0.034(9) C34 0.210(11) 0.102(8) 0.153(9) -0.044(7) 0.065(8) -0.043(8) C35 0.098(8) 0.228(13) 0.182(10) -0.050(9) -0.016(8) 0.001(8) C36 0.192(13) 0.147(10) 0.168(11) -0.053(9) -0.013(9) 0.105(10) C37 0.138(11) 0.122(10) 0.212(14) 0.007(10) 0.048(10) 0.069(9) C38 0.191(14) 0.195(14) 0.152(11) -0.018(10) -0.006(10) 0.111(11) C39 0.126(10) 0.137(10) 0.183(11) -0.031(9) -0.043(9) 0.071(8) _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 Y O2 2.132(5) . ? Y O1 2.151(5) . ? Y N 2.240(5) . ? Y O3 2.382(5) . ? Y S1 2.948(2) . ? Y S2 2.973(2) . ? Y Si2 3.318(3) . ? Y Si1 3.338(2) . ? Si1 N 1.682(6) . ? Si1 C33 1.839(8) . ? Si1 C32 1.860(8) . ? Si2 N 1.688(6) . ? Si2 C35 1.833(9) . ? Si2 C34 1.866(8) . ? S1 C2 1.772(7) . ? S1 C15 1.833(10) . ? S2 C18 1.789(7) . ? S2 C17 1.831(8) . ? O1 C1 1.321(7) . ? O2 C19 1.317(7) . ? O3 C36 1.402(10) . ? O3 C39 1.421(9) . ? C1 C2 1.392(8) . ? C1 C6 1.419(9) . ? C2 C3 1.394(10) . ? C3 C4 1.356(10) . ? C4 C5 1.376(10) . ? C4 C7 1.541(10) . ? C5 C6 1.380(9) . ? C6 C11 1.531(9) . ? C7 C10B 1.41(5) . ? C7 C8B 1.42(4) . ? C7 C10A 1.49(3) . ? C7 C9A 1.50(4) . ? C7 C8A 1.52(6) . ? C7 C9B 1.54(4) . ? C11 C13 1.519(9) . ? C11 C14 1.539(9) . ? C11 C12 1.543(9) . ? C15 C16 1.509(13) . ? C16 C17 1.514(12) . ? C18 C23 1.378(9) . ? C18 C19 1.391(8) . ? C19 C20 1.416(8) . ? C20 C21 1.373(9) . ? C20 C28 1.555(9) . ? C21 C22 1.383(10) . ? C22 C23 1.372(10) . ? C22 C24 1.520(10) . ? C24 C26A 1.46(2) . ? C24 C25B 1.48(3) . ? C24 C27A 1.49(2) . ? C24 C27B 1.51(3) . ? C24 C25A 1.52(3) . ? C24 C26B 1.59(3) . ? C28 C29 1.511(9) . ? C28 C31 1.524(9) . ? C28 C30 1.525(9) . ? C36 C37 1.405(11) . ? C37 C38 1.425(13) . ? C38 C39 1.449(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Y O1 105.10(16) . . ? O2 Y N 117.96(19) . . ? O1 Y N 136.45(18) . . ? O2 Y O3 86.21(17) . . ? O1 Y O3 86.54(19) . . ? N Y O3 89.9(2) . . ? O2 Y S1 135.23(13) . . ? O1 Y S1 66.14(12) . . ? N Y S1 86.32(14) . . ? O3 Y S1 133.75(13) . . ? O2 Y S2 67.66(13) . . ? O1 Y S2 107.07(13) . . ? N Y S2 95.46(15) . . ? O3 Y S2 152.74(13) . . ? S1 Y S2 73.38(6) . . ? O2 Y Si2 91.35(13) . . ? O1 Y Si2 163.53(12) . . ? N Y Si2 27.59(15) . . ? O3 Y Si2 95.55(16) . . ? S1 Y Si2 101.58(7) . . ? S2 Y Si2 78.12(6) . . ? O2 Y Si1 143.39(13) . . ? O1 Y Si1 109.62(12) . . ? N Y Si1 26.95(15) . . ? O3 Y Si1 84.66(14) . . ? S1 Y Si1 71.75(6) . . ? S2 Y Si1 111.43(6) . . ? Si2 Y Si1 54.54(7) . . ? N Si1 C33 114.4(4) . . ? N Si1 C32 114.8(4) . . ? C33 Si1 C32 109.1(4) . . ? N Si1 Y 37.13(19) . . ? C33 Si1 Y 121.3(3) . . ? C32 Si1 Y 129.0(3) . . ? N Si2 C35 114.0(4) . . ? N Si2 C34 114.8(4) . . ? C35 Si2 C34 109.4(5) . . ? N Si2 Y 37.91(18) . . ? C35 Si2 Y 129.5(4) . . ? C34 Si2 Y 120.5(4) . . ? C2 S1 C15 103.3(4) . . ? C2 S1 Y 96.5(2) . . ? C15 S1 Y 113.7(3) . . ? C18 S2 C17 101.4(4) . . ? C18 S2 Y 95.9(3) . . ? C17 S2 Y 95.2(3) . . ? C1 O1 Y 136.8(4) . . ? C19 O2 Y 138.0(4) . . ? C36 O3 C39 106.5(7) . . ? C36 O3 Y 129.1(6) . . ? C39 O3 Y 123.6(5) . . ? Si1 N Si2 129.6(3) . . ? Si1 N Y 115.9(3) . . ? Si2 N Y 114.5(3) . . ? O1 C1 C2 118.3(7) . . ? O1 C1 C6 124.6(7) . . ? C2 C1 C6 117.1(7) . . ? C1 C2 C3 122.0(7) . . ? C1 C2 S1 117.3(6) . . ? C3 C2 S1 120.6(6) . . ? C4 C3 C2 121.3(8) . . ? C3 C4 C5 116.8(8) . . ? C3 C4 C7 120.2(9) . . ? C5 C4 C7 123.0(9) . . ? C4 C5 C6 124.9(8) . . ? C5 C6 C1 117.9(7) . . ? C5 C6 C11 122.5(7) . . ? C1 C6 C11 119.6(7) . . ? C10B C7 C8B 104(4) . . ? C10B C7 C10A 33(3) . . ? C8B C7 C10A 121(2) . . ? C10B C7 C9A 139(2) . . ? C8B C7 C9A 75(3) . . ? C10A C7 C9A 112(2) . . ? C10B C7 C8A 78(3) . . ? C8B C7 C8A 34(4) . . ? C10A C7 C8A 106(4) . . ? C9A C7 C8A 110(3) . . ? C10B C7 C9B 109(3) . . ? C8B C7 C9B 110(3) . . ? C10A C7 C9B 77(2) . . ? C9A C7 C9B 41(2) . . ? C8A C7 C9B 142(3) . . ? C10B C7 C4 109.6(19) . . ? C8B C7 C4 116.7(17) . . ? C10A C7 C4 116.4(14) . . ? C9A C7 C4 107.2(16) . . ? C8A C7 C4 104.9(19) . . ? C9B C7 C4 107.4(18) . . ? C13 C11 C6 111.4(6) . . ? C13 C11 C14 107.5(6) . . ? C6 C11 C14 111.4(7) . . ? C13 C11 C12 110.1(6) . . ? C6 C11 C12 108.5(6) . . ? C14 C11 C12 107.9(7) . . ? C16 C15 S1 117.1(7) . . ? C15 C16 C17 115.7(9) . . ? C16 C17 S2 110.0(7) . . ? C23 C18 C19 122.9(7) . . ? C23 C18 S2 119.8(7) . . ? C19 C18 S2 117.3(6) . . ? O2 C19 C18 120.9(7) . . ? O2 C19 C20 122.8(7) . . ? C18 C19 C20 116.3(7) . . ? C21 C20 C19 117.8(7) . . ? C21 C20 C28 122.7(7) . . ? C19 C20 C28 119.5(7) . . ? C20 C21 C22 126.3(8) . . ? C23 C22 C21 114.6(8) . . ? C23 C22 C24 123.9(9) . . ? C21 C22 C24 121.5(9) . . ? C22 C23 C18 121.7(8) . . ? C26A C24 C25B 51(2) . . ? C26A C24 C27A 113.0(15) . . ? C25B C24 C27A 138.8(17) . . ? C26A C24 C27B 137.1(15) . . ? C25B C24 C27B 104(2) . . ? C27A C24 C27B 58.9(18) . . ? C26A C24 C25A 105.9(16) . . ? C25B C24 C25A 56.8(18) . . ? C27A C24 C25A 107.7(16) . . ? C27B C24 C25A 51.1(18) . . ? C26A C24 C22 111.7(12) . . ? C25B C24 C22 112.4(15) . . ? C27A C24 C22 108.7(11) . . ? C27B C24 C22 110.4(12) . . ? C25A C24 C22 109.6(12) . . ? C26A C24 C26B 62(2) . . ? C25B C24 C26B 109(2) . . ? C27A C24 C26B 54(2) . . ? C27B C24 C26B 108(2) . . ? C25A C24 C26B 137.3(15) . . ? C22 C24 C26B 112.9(13) . . ? C29 C28 C31 106.6(7) . . ? C29 C28 C30 111.2(7) . . ? C31 C28 C30 108.2(7) . . ? C29 C28 C20 110.4(6) . . ? C31 C28 C20 111.9(6) . . ? C30 C28 C20 108.5(6) . . ? O3 C36 C37 110.1(9) . . ? C36 C37 C38 107.5(10) . . ? C37 C38 C39 106.6(10) . . ? O3 C39 C38 108.0(9) . . ? 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 O2 Y Si1 N -24.1(4) . . . . ? O1 Y Si1 N 175.2(3) . . . . ? O3 Y Si1 N -100.4(3) . . . . ? S1 Y Si1 N 120.0(3) . . . . ? S2 Y Si1 N 56.9(3) . . . . ? Si2 Y Si1 N 0.3(3) . . . . ? O2 Y Si1 C33 -114.0(4) . . . . ? O1 Y Si1 C33 85.3(4) . . . . ? N Y Si1 C33 -89.9(5) . . . . ? O3 Y Si1 C33 169.7(4) . . . . ? S1 Y Si1 C33 30.0(4) . . . . ? S2 Y Si1 C33 -33.0(4) . . . . ? Si2 Y Si1 C33 -89.6(4) . . . . ? O2 Y Si1 C32 55.8(5) . . . . ? O1 Y Si1 C32 -104.9(4) . . . . ? N Y Si1 C32 79.9(5) . . . . ? O3 Y Si1 C32 -20.5(4) . . . . ? S1 Y Si1 C32 -160.1(4) . . . . ? S2 Y Si1 C32 136.8(4) . . . . ? Si2 Y Si1 C32 80.2(4) . . . . ? O2 Y Si2 N 165.4(3) . . . . ? O1 Y Si2 N -17.5(6) . . . . ? O3 Y Si2 N 79.1(3) . . . . ? S1 Y Si2 N -57.8(3) . . . . ? S2 Y Si2 N -127.8(3) . . . . ? Si1 Y Si2 N -0.3(3) . . . . ? O2 Y Si2 C35 -116.3(5) . . . . ? O1 Y Si2 C35 60.8(7) . . . . ? N Y Si2 C35 78.3(5) . . . . ? O3 Y Si2 C35 157.4(5) . . . . ? S1 Y Si2 C35 20.6(4) . . . . ? S2 Y Si2 C35 -49.4(4) . . . . ? Si1 Y Si2 C35 78.0(4) . . . . ? O2 Y Si2 C34 73.4(4) . . . . ? O1 Y Si2 C34 -109.5(6) . . . . ? N Y Si2 C34 -92.0(5) . . . . ? O3 Y Si2 C34 -12.9(4) . . . . ? S1 Y Si2 C34 -149.8(3) . . . . ? S2 Y Si2 C34 140.2(4) . . . . ? Si1 Y Si2 C34 -92.3(4) . . . . ? O2 Y S1 C2 -74.2(3) . . . . ? O1 Y S1 C2 13.4(3) . . . . ? N Y S1 C2 158.8(3) . . . . ? O3 Y S1 C2 72.4(3) . . . . ? S2 Y S1 C2 -104.4(2) . . . . ? Si2 Y S1 C2 -178.1(2) . . . . ? Si1 Y S1 C2 135.6(2) . . . . ? O2 Y S1 C15 33.5(5) . . . . ? O1 Y S1 C15 121.1(4) . . . . ? N Y S1 C15 -93.6(4) . . . . ? O3 Y S1 C15 -179.9(5) . . . . ? S2 Y S1 C15 3.3(4) . . . . ? Si2 Y S1 C15 -70.5(4) . . . . ? Si1 Y S1 C15 -116.7(4) . . . . ? O2 Y S2 C18 -1.8(2) . . . . ? O1 Y S2 C18 97.9(2) . . . . ? N Y S2 C18 -119.8(3) . . . . ? O3 Y S2 C18 -19.3(4) . . . . ? S1 Y S2 C18 155.7(2) . . . . ? Si2 Y S2 C18 -98.3(2) . . . . ? Si1 Y S2 C18 -142.2(2) . . . . ? O2 Y S2 C17 -103.8(3) . . . . ? O1 Y S2 C17 -4.1(3) . . . . ? N Y S2 C17 138.2(3) . . . . ? O3 Y S2 C17 -121.4(4) . . . . ? S1 Y S2 C17 53.7(3) . . . . ? Si2 Y S2 C17 159.7(3) . . . . ? Si1 Y S2 C17 115.7(3) . . . . ? O2 Y O1 C1 108.8(6) . . . . ? N Y O1 C1 -79.9(7) . . . . ? O3 Y O1 C1 -166.1(6) . . . . ? S1 Y O1 C1 -24.4(6) . . . . ? S2 Y O1 C1 38.0(6) . . . . ? Si2 Y O1 C1 -68.2(8) . . . . ? Si1 Y O1 C1 -83.0(6) . . . . ? O1 Y O2 C19 -103.0(6) . . . . ? N Y O2 C19 83.7(6) . . . . ? O3 Y O2 C19 171.6(6) . . . . ? S1 Y O2 C19 -31.8(7) . . . . ? S2 Y O2 C19 -0.4(6) . . . . ? Si2 Y O2 C19 76.1(6) . . . . ? Si1 Y O2 C19 95.8(6) . . . . ? O2 Y O3 C36 -98.0(8) . . . . ? O1 Y O3 C36 156.6(8) . . . . ? N Y O3 C36 20.0(8) . . . . ? S1 Y O3 C36 104.8(8) . . . . ? S2 Y O3 C36 -81.8(9) . . . . ? Si2 Y O3 C36 -7.0(8) . . . . ? Si1 Y O3 C36 46.5(8) . . . . ? O2 Y O3 C39 70.3(7) . . . . ? O1 Y O3 C39 -35.1(7) . . . . ? N Y O3 C39 -171.7(7) . . . . ? S1 Y O3 C39 -86.9(7) . . . . ? S2 Y O3 C39 86.5(8) . . . . ? Si2 Y O3 C39 161.3(7) . . . . ? Si1 Y O3 C39 -145.2(7) . . . . ? C33 Si1 N Si2 -69.1(6) . . . . ? C32 Si1 N Si2 58.1(6) . . . . ? Y Si1 N Si2 -179.3(7) . . . . ? C33 Si1 N Y 110.2(4) . . . . ? C32 Si1 N Y -122.6(4) . . . . ? C35 Si2 N Si1 55.1(6) . . . . ? C34 Si2 N Si1 -72.2(6) . . . . ? Y Si2 N Si1 179.3(6) . . . . ? C35 Si2 N Y -124.2(4) . . . . ? C34 Si2 N Y 108.5(4) . . . . ? O2 Y N Si1 164.0(3) . . . . ? O1 Y N Si1 -6.5(5) . . . . ? O3 Y N Si1 78.3(3) . . . . ? S1 Y N Si1 -55.5(3) . . . . ? S2 Y N Si1 -128.4(3) . . . . ? Si2 Y N Si1 -179.4(6) . . . . ? O2 Y N Si2 -16.6(4) . . . . ? O1 Y N Si2 172.9(2) . . . . ? O3 Y N Si2 -102.2(3) . . . . ? S1 Y N Si2 123.9(3) . . . . ? S2 Y N Si2 51.0(3) . . . . ? Si1 Y N Si2 179.4(6) . . . . ? Y O1 C1 C2 25.7(9) . . . . ? Y O1 C1 C6 -152.3(5) . . . . ? O1 C1 C2 C3 -179.5(6) . . . . ? C6 C1 C2 C3 -1.3(10) . . . . ? O1 C1 C2 S1 -2.1(8) . . . . ? C6 C1 C2 S1 176.1(5) . . . . ? C15 S1 C2 C1 -126.6(6) . . . . ? Y S1 C2 C1 -10.3(5) . . . . ? C15 S1 C2 C3 51.0(7) . . . . ? Y S1 C2 C3 167.2(6) . . . . ? C1 C2 C3 C4 1.9(12) . . . . ? S1 C2 C3 C4 -175.4(6) . . . . ? C2 C3 C4 C5 -2.1(12) . . . . ? C2 C3 C4 C7 174.5(8) . . . . ? C3 C4 C5 C6 1.8(12) . . . . ? C7 C4 C5 C6 -174.7(8) . . . . ? C4 C5 C6 C1 -1.3(12) . . . . ? C4 C5 C6 C11 178.7(7) . . . . ? O1 C1 C6 C5 179.1(6) . . . . ? C2 C1 C6 C5 1.0(10) . . . . ? O1 C1 C6 C11 -0.9(10) . . . . ? C2 C1 C6 C11 -179.0(6) . . . . ? C3 C4 C7 C10B 152(4) . . . . ? C5 C4 C7 C10B -32(4) . . . . ? C3 C4 C7 C8B 34(3) . . . . ? C5 C4 C7 C8B -149(3) . . . . ? C3 C4 C7 C10A -173.5(19) . . . . ? C5 C4 C7 C10A 3(2) . . . . ? C3 C4 C7 C9A -48(3) . . . . ? C5 C4 C7 C9A 129(3) . . . . ? C3 C4 C7 C8A 69(4) . . . . ? C5 C4 C7 C8A -115(4) . . . . ? C3 C4 C7 C9B -90(2) . . . . ? C5 C4 C7 C9B 86(2) . . . . ? C5 C6 C11 C13 -126.1(8) . . . . ? C1 C6 C11 C13 53.9(9) . . . . ? C5 C6 C11 C14 -6.0(10) . . . . ? C1 C6 C11 C14 174.0(6) . . . . ? C5 C6 C11 C12 112.6(8) . . . . ? C1 C6 C11 C12 -67.4(8) . . . . ? C2 S1 C15 C16 41.3(9) . . . . ? Y S1 C15 C16 -62.1(9) . . . . ? S1 C15 C16 C17 46.4(13) . . . . ? C15 C16 C17 S2 46.5(11) . . . . ? C18 S2 C17 C16 160.7(7) . . . . ? Y S2 C17 C16 -102.1(7) . . . . ? C17 S2 C18 C23 -79.2(7) . . . . ? Y S2 C18 C23 -175.7(6) . . . . ? C17 S2 C18 C19 100.5(6) . . . . ? Y S2 C18 C19 4.0(5) . . . . ? Y O2 C19 C18 3.5(10) . . . . ? Y O2 C19 C20 -176.0(4) . . . . ? C23 C18 C19 O2 174.4(6) . . . . ? S2 C18 C19 O2 -5.2(9) . . . . ? C23 C18 C19 C20 -6.1(10) . . . . ? S2 C18 C19 C20 174.3(4) . . . . ? O2 C19 C20 C21 -174.3(6) . . . . ? C18 C19 C20 C21 6.3(9) . . . . ? O2 C19 C20 C28 5.5(9) . . . . ? C18 C19 C20 C28 -173.9(6) . . . . ? C19 C20 C21 C22 -1.4(11) . . . . ? C28 C20 C21 C22 178.9(7) . . . . ? C20 C21 C22 C23 -4.1(11) . . . . ? C20 C21 C22 C24 176.7(7) . . . . ? C21 C22 C23 C18 4.4(11) . . . . ? C24 C22 C23 C18 -176.4(7) . . . . ? C19 C18 C23 C22 0.6(11) . . . . ? S2 C18 C23 C22 -179.8(5) . . . . ? C23 C22 C24 C26A -120.2(17) . . . . ? C21 C22 C24 C26A 59.0(18) . . . . ? C23 C22 C24 C25B -64(3) . . . . ? C21 C22 C24 C25B 115(3) . . . . ? C23 C22 C24 C27A 114.4(19) . . . . ? C21 C22 C24 C27A -66.4(19) . . . . ? C23 C22 C24 C27B 52(3) . . . . ? C21 C22 C24 C27B -129(3) . . . . ? C23 C22 C24 C25A -3(2) . . . . ? C21 C22 C24 C25A 176(2) . . . . ? C23 C22 C24 C26B 172(3) . . . . ? C21 C22 C24 C26B -9(3) . . . . ? C21 C20 C28 C29 -127.4(7) . . . . ? C19 C20 C28 C29 52.9(8) . . . . ? C21 C20 C28 C31 -8.8(10) . . . . ? C19 C20 C28 C31 171.5(6) . . . . ? C21 C20 C28 C30 110.5(7) . . . . ? C19 C20 C28 C30 -69.3(8) . . . . ? C39 O3 C36 C37 -11.2(13) . . . . ? Y O3 C36 C37 158.6(7) . . . . ? O3 C36 C37 C38 7.1(15) . . . . ? C36 C37 C38 C39 -0.2(16) . . . . ? C36 O3 C39 C38 10.9(12) . . . . ? Y O3 C39 C38 -159.6(7) . . . . ? C37 C38 C39 O3 -6.7(15) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.256 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.055 #===END data_hm1 _database_code_CSD 220243 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H68 Li N2 O3 S2 Sc Si4' _chemical_formula_weight 805.30 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.2519 0.3716 '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.6130(10) _cell_length_b 18.3630(10) _cell_length_c 16.5110(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.013(5) _cell_angle_gamma 90.00 _cell_volume 4733.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.9 _cell_measurement_theta_max 10.2 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.130 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 0.377 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.7837 _exptl_absorpt_correction_T_max 0.8889 _exptl_absorpt_process_details 'semi-empirical, psi-scans' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 (Enraf nonius)' _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -2 8 1 2 -8 1 -2 8 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 7 _diffrn_standards_decay_corr_max 1.080 _diffrn_standards_decay_corr_min 0.995 _diffrn_standards_interval_count ? _diffrn_reflns_number 9589 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0798 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.97 _reflns_number_total 9233 _reflns_number_gt 4860 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' #_computing_structure_solution 'SHELXS-97 (Sheldrick, 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^)+(0.0642P)^2^+1.0199P] 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 9233 _refine_ls_number_parameters 518 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1424 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1580 _refine_ls_wR_factor_gt 0.1280 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.13507(9) 0.36759(7) 0.03125(8) 0.0678(4) Uani 1 1 d . A . Si2 Si -0.02921(8) 0.31733(7) 0.09670(8) 0.0675(4) Uani 1 1 d . . . Si3 Si 0.29477(8) 0.31698(7) 0.20491(8) 0.0666(4) Uani 1 1 d . . . Si4 Si 0.36375(10) 0.19248(11) 0.11468(13) 0.1073(7) Uani 1 1 d . . . Sc Sc 0.15335(5) 0.20932(4) 0.11526(4) 0.0477(2) Uani 1 1 d . . . S1 S 0.18624(9) 0.05607(6) 0.13107(7) 0.0695(4) Uani 1 1 d . A . S2 S -0.01040(7) 0.13961(6) 0.12405(7) 0.0600(3) Uani 1 1 d . A . O1 O 0.16360(17) 0.16624(14) 0.00527(15) 0.0562(7) Uani 1 1 d . A . O2 O 0.11066(17) 0.20846(14) 0.23446(15) 0.0511(7) Uani 1 1 d . A . O3 O 0.0437(2) 0.38351(17) 0.29505(19) 0.0753(9) Uani 1 1 d . . . N1 N 0.0807(2) 0.30923(17) 0.09471(19) 0.0524(8) Uani 1 1 d . A . N2 N 0.2787(2) 0.24051(19) 0.1484(2) 0.0593(9) Uani 1 1 d . A . Li Li 0.0879(5) 0.3132(4) 0.2245(4) 0.067(2) Uani 1 1 d . A . C1 C 0.1880(3) 0.1028(2) -0.0265(3) 0.0546(10) Uani 1 1 d . . . C2 C 0.2029(3) 0.0431(2) 0.0261(3) 0.0608(11) Uani 1 1 d . A . C3 C 0.2315(3) -0.0236(3) -0.0036(3) 0.0673(13) Uani 1 1 d . . . H3 H 0.237(3) -0.060(2) 0.036(3) 0.082(16) Uiso 1 1 d . . . C4 C 0.2460(3) -0.0337(3) -0.0841(3) 0.0691(13) Uani 1 1 d . A . C5 C 0.2300(3) 0.0249(3) -0.1352(3) 0.0653(13) Uani 1 1 d . . . H5 H 0.241(2) 0.0170(19) -0.188(2) 0.041(10) Uiso 1 1 d . . . C6 C 0.2013(3) 0.0923(2) -0.1102(3) 0.0582(11) Uani 1 1 d . A . C7 C 0.2788(4) -0.1063(3) -0.1172(3) 0.0992(19) Uani 1 1 d . . . H7A H 0.3237 -0.1244 -0.0829 0.149 Uiso 1 1 calc R A . H7B H 0.3007 -0.0993 -0.1710 0.149 Uiso 1 1 calc R . . H7C H 0.2327 -0.1409 -0.1186 0.149 Uiso 1 1 calc R . . C8 C 0.1806(3) 0.1534(3) -0.1705(3) 0.0712(13) Uani 1 1 d . . . C9 C 0.0855(3) 0.1735(3) -0.1628(3) 0.0862(16) Uani 1 1 d . A . H9A H 0.0509 0.1322 -0.1768 0.129 Uiso 1 1 calc R . . H9B H 0.0727 0.2132 -0.1986 0.129 Uiso 1 1 calc R . . H9C H 0.0736 0.1878 -0.1080 0.129 Uiso 1 1 calc R . . C10 C 0.1975(4) 0.1314(3) -0.2583(3) 0.112(2) Uani 1 1 d . A . H10A H 0.1588 0.0932 -0.2736 0.168 Uiso 1 1 calc R . . H10B H 0.2554 0.1144 -0.2635 0.168 Uiso 1 1 calc R . . H10C H 0.1891 0.1727 -0.2930 0.168 Uiso 1 1 calc R . . C11 C 0.2358(4) 0.2210(3) -0.1534(3) 0.0940(17) Uani 1 1 d . A . H11A H 0.2175 0.2604 -0.1875 0.141 Uiso 1 1 calc R . . H11B H 0.2948 0.2100 -0.1643 0.141 Uiso 1 1 calc R . . H11C H 0.2295 0.2348 -0.0976 0.141 Uiso 1 1 calc R . . C12 C 0.0828(4) 0.0120(3) 0.1431(4) 0.0829(18) Uani 1 1 d . . . H12A H 0.073(3) 0.012(3) 0.195(3) 0.077(17) Uiso 1 1 d . . . H12B H 0.088(3) -0.031(3) 0.129(3) 0.082(17) Uiso 1 1 d . . . C13 C 0.0108(4) 0.0464(3) 0.0979(4) 0.0731(15) Uani 1 1 d . A . H13A H 0.026(3) 0.049(2) 0.047(3) 0.072(16) Uiso 1 1 d . . . H13B H -0.039(3) 0.017(2) 0.108(2) 0.065(13) Uiso 1 1 d . . . C14 C -0.0129(3) 0.1343(2) 0.2308(2) 0.0554(11) Uani 1 1 d . . . C15 C 0.0549(3) 0.1658(2) 0.2737(2) 0.0533(10) Uani 1 1 d . A . C16 C 0.0618(3) 0.1499(2) 0.3573(3) 0.0634(12) Uani 1 1 d . . . C17 C -0.0051(4) 0.1126(3) 0.3914(3) 0.0863(18) Uani 1 1 d . A . H17 H -0.005(3) 0.100(2) 0.442(3) 0.062(13) Uiso 1 1 d . . . C18 C -0.0781(4) 0.0877(3) 0.3508(3) 0.0848(16) Uani 1 1 d . . . C19 C -0.0789(3) 0.0976(3) 0.2690(3) 0.0720(14) Uani 1 1 d . A . H19 H -0.123(2) 0.079(2) 0.240(2) 0.055(12) Uiso 1 1 d . . . C20 C -0.1523(5) 0.0515(4) 0.3949(4) 0.133(3) Uani 1 1 d . A . H20A H -0.1919 0.0320 0.3560 0.199 Uiso 1 1 calc R . . H20B H -0.1810 0.0868 0.4281 0.199 Uiso 1 1 calc R . . H20C H -0.1309 0.0128 0.4284 0.199 Uiso 1 1 calc R . . C21 C 0.1428(3) 0.1691(3) 0.4054(3) 0.0784(15) Uani 1 1 d . A . C22 C 0.1527(3) 0.2513(3) 0.4131(3) 0.0842(16) Uani 1 1 d . . . H22A H 0.1587 0.2723 0.3602 0.126 Uiso 1 1 calc R A . H22B H 0.2027 0.2621 0.4448 0.126 Uiso 1 1 calc R . . H22C H 0.1030 0.2712 0.4391 0.126 Uiso 1 1 calc R . . C23 C 0.2198(4) 0.1348(3) 0.3622(3) 0.0964(18) Uani 1 1 d . . . H23A H 0.2103 0.0834 0.3559 0.145 Uiso 1 1 calc R A . H23B H 0.2706 0.1425 0.3939 0.145 Uiso 1 1 calc R . . H23C H 0.2268 0.1568 0.3099 0.145 Uiso 1 1 calc R . . C24 C 0.1398(5) 0.1373(4) 0.4920(3) 0.130(3) Uani 1 1 d . . . H24A H 0.0930 0.1588 0.5212 0.196 Uiso 1 1 calc R A . H24B H 0.1926 0.1479 0.5194 0.196 Uiso 1 1 calc R . . H24C H 0.1319 0.0855 0.4892 0.196 Uiso 1 1 calc R . . C25 C 0.1521(4) 0.4603(3) 0.0748(3) 0.0941(17) Uani 1 1 d . . . H25A H 0.0981 0.4850 0.0789 0.141 Uiso 1 1 calc R A . H25B H 0.1897 0.4875 0.0402 0.141 Uiso 1 1 calc R . . H25C H 0.1772 0.4560 0.1277 0.141 Uiso 1 1 calc R . . C26 C 0.0858(4) 0.3794(3) -0.0713(3) 0.0883(16) Uani 1 1 d . . . H26A H 0.0753 0.3325 -0.0950 0.132 Uiso 1 1 calc R A . H26B H 0.1241 0.4065 -0.1054 0.132 Uiso 1 1 calc R . . H26C H 0.0326 0.4053 -0.0662 0.132 Uiso 1 1 calc R . . C27 C -0.0874(3) 0.2756(3) 0.0092(3) 0.103(2) Uani 1 1 d . . . H27A H -0.0848 0.3079 -0.0365 0.154 Uiso 1 1 calc R . . H27B H -0.1462 0.2676 0.0238 0.154 Uiso 1 1 calc R . . H27C H -0.0612 0.2300 -0.0046 0.154 Uiso 1 1 calc R . . C28 C -0.0682(4) 0.4133(3) 0.1060(3) 0.0990(18) Uani 1 1 d . . . H28A H -0.0420 0.4359 0.1522 0.148 Uiso 1 1 calc R . . H28B H -0.1293 0.4134 0.1125 0.148 Uiso 1 1 calc R . . H28C H -0.0533 0.4400 0.0580 0.148 Uiso 1 1 calc R . . C29 C 0.3568(4) 0.3917(3) 0.1538(3) 0.1033(19) Uani 1 1 d . . . H29A H 0.4163 0.3786 0.1515 0.155 Uiso 1 1 calc R . . H29B H 0.3505 0.4361 0.1841 0.155 Uiso 1 1 calc R . . H29C H 0.3354 0.3987 0.0999 0.155 Uiso 1 1 calc R . . C30 C 0.3463(3) 0.3043(3) 0.3064(3) 0.0918(17) Uani 1 1 d . . . H30A H 0.3253 0.2603 0.3308 0.138 Uiso 1 1 calc R . . H30B H 0.3327 0.3450 0.3406 0.138 Uiso 1 1 calc R . . H30C H 0.4073 0.3011 0.2999 0.138 Uiso 1 1 calc R . . C31A C 0.4027(13) 0.2391(16) 0.0086(12) 0.177(10) Uani 0.50 1 d P A 1 H31A H 0.3569 0.2372 -0.0301 0.265 Uiso 0.50 1 d PR A 1 H31B H 0.4513 0.2131 -0.0122 0.265 Uiso 0.50 1 d PR A 1 H31C H 0.4183 0.2889 0.0182 0.265 Uiso 0.50 1 d PR A 1 C32A C 0.4605(12) 0.1855(14) 0.1681(14) 0.162(10) Uani 0.50 1 d P A 1 H32A H 0.5075 0.1887 0.1308 0.242 Uiso 0.50 1 d PR A 1 H32B H 0.4626 0.1395 0.1957 0.242 Uiso 0.50 1 d PR A 1 H32C H 0.4642 0.2243 0.2068 0.242 Uiso 0.50 1 d PR A 1 C31B C 0.4461(14) 0.2396(13) 0.0667(16) 0.192(12) Uani 0.50 1 d P A 2 H31D H 0.4595 0.2828 0.0971 0.288 Uiso 0.50 1 d PR A 2 H31E H 0.4283 0.2530 0.0131 0.288 Uiso 0.50 1 d PR A 2 H31F H 0.4959 0.2092 0.0635 0.288 Uiso 0.50 1 d PR A 2 C32B C 0.4206(11) 0.1492(12) 0.2155(12) 0.151(9) Uani 0.50 1 d P A 2 H32D H 0.4697 0.1778 0.2298 0.227 Uiso 0.50 1 d PR A 2 H32E H 0.4382 0.1001 0.2044 0.227 Uiso 0.50 1 d PR A 2 H32F H 0.3805 0.1493 0.2596 0.227 Uiso 0.50 1 d PR A 2 C33A C 0.0986(7) 0.4360(6) 0.3389(7) 0.074(3) Uiso 0.50 1 d P A 1 H33A H 0.1527 0.4134 0.3533 0.088 Uiso 0.50 1 calc PR A 1 H33B H 0.1103 0.4780 0.3051 0.088 Uiso 0.50 1 calc PR A 1 C34A C 0.0536(7) 0.4577(7) 0.4105(7) 0.082(3) Uiso 0.50 1 d P A 1 H34A H 0.0676 0.5074 0.4255 0.098 Uiso 0.50 1 calc PR A 1 H34B H 0.0665 0.4256 0.4556 0.098 Uiso 0.50 1 calc PR A 1 C35A C -0.0405(9) 0.4509(8) 0.3848(9) 0.103(4) Uiso 0.50 1 d P A 1 H35A H -0.0765 0.4388 0.4307 0.124 Uiso 0.50 1 calc PR A 1 H35B H -0.0608 0.4959 0.3608 0.124 Uiso 0.50 1 calc PR A 1 C36A C -0.0406(9) 0.3935(8) 0.3269(8) 0.093(4) Uiso 0.50 1 d P A 1 H36A H -0.0798 0.4052 0.2832 0.111 Uiso 0.50 1 calc PR A 1 H36B H -0.0599 0.3488 0.3523 0.111 Uiso 0.50 1 calc PR A 1 C33B C 0.0763(8) 0.4543(7) 0.3110(8) 0.089(4) Uiso 0.50 1 d P A 2 H33C H 0.0724 0.4847 0.2630 0.107 Uiso 0.50 1 calc PR A 2 H33D H 0.1357 0.4518 0.3279 0.107 Uiso 0.50 1 calc PR A 2 C34B C 0.0215(11) 0.4839(8) 0.3774(9) 0.129(5) Uiso 0.50 1 d P A 2 H34C H -0.0184 0.5195 0.3560 0.155 Uiso 0.50 1 calc PR A 2 H34D H 0.0569 0.5075 0.4181 0.155 Uiso 0.50 1 calc PR A 2 C35B C -0.0284(9) 0.4185(7) 0.4158(8) 0.100(4) Uiso 0.50 1 d P A 2 H35C H 0.0026 0.3976 0.4611 0.120 Uiso 0.50 1 calc PR A 2 H35D H -0.0852 0.4329 0.4334 0.120 Uiso 0.50 1 calc PR A 2 C36B C -0.0323(7) 0.3658(7) 0.3434(7) 0.071(3) Uiso 0.50 1 d P A 2 H36C H -0.0304 0.3156 0.3616 0.085 Uiso 0.50 1 calc PR A 2 H36D H -0.0842 0.3732 0.3122 0.085 Uiso 0.50 1 calc PR A 2 H1A H 0.217(2) 0.339(2) 0.017(2) 0.070(12) Uiso 1 1 d . . . H1B H -0.054(2) 0.2827(18) 0.173(2) 0.055(10) Uiso 1 1 d . . . H1C H 0.2156(19) 0.3480(16) 0.2232(17) 0.034(8) Uiso 1 1 d . . . H1D H 0.346(3) 0.126(3) 0.080(3) 0.117(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0822(10) 0.0513(7) 0.0700(9) 0.0076(7) -0.0118(7) 0.0003(7) Si2 0.0661(8) 0.0627(8) 0.0736(9) 0.0071(7) -0.0213(7) 0.0094(7) Si3 0.0593(8) 0.0688(9) 0.0717(9) -0.0106(7) -0.0154(6) -0.0060(7) Si4 0.0558(9) 0.1097(14) 0.1564(17) -0.0582(13) -0.0108(10) 0.0082(9) Sc 0.0534(4) 0.0414(4) 0.0483(4) -0.0054(4) -0.0128(3) 0.0036(4) S1 0.0926(9) 0.0555(7) 0.0604(7) -0.0039(6) -0.0169(6) 0.0163(6) S2 0.0682(7) 0.0558(7) 0.0559(6) -0.0034(5) -0.0159(5) -0.0081(6) O1 0.0690(19) 0.0477(17) 0.0520(17) -0.0100(13) -0.0105(14) 0.0097(14) O2 0.0565(16) 0.0467(16) 0.0501(15) -0.0014(13) -0.0141(13) -0.0015(13) O3 0.068(2) 0.072(2) 0.086(2) -0.0264(18) 0.0019(17) -0.0025(17) N1 0.061(2) 0.0435(19) 0.052(2) -0.0003(15) -0.0160(16) 0.0028(16) N2 0.051(2) 0.063(2) 0.063(2) -0.0092(18) -0.0115(17) 0.0038(17) Li 0.088(6) 0.053(4) 0.060(5) -0.012(4) -0.013(4) 0.007(4) C1 0.052(2) 0.055(3) 0.058(3) -0.010(2) -0.010(2) 0.004(2) C2 0.066(3) 0.054(3) 0.062(3) -0.012(2) -0.012(2) 0.011(2) C3 0.072(3) 0.058(3) 0.072(3) -0.009(3) -0.014(3) 0.013(2) C4 0.062(3) 0.059(3) 0.087(4) -0.019(3) -0.010(3) 0.018(2) C5 0.057(3) 0.083(4) 0.056(3) -0.028(3) -0.005(2) 0.009(3) C6 0.054(2) 0.065(3) 0.056(3) -0.012(2) -0.005(2) 0.008(2) C7 0.098(4) 0.081(4) 0.119(5) -0.035(3) -0.010(3) 0.034(3) C8 0.081(3) 0.076(3) 0.056(3) -0.005(2) -0.003(2) 0.012(3) C9 0.088(4) 0.090(4) 0.080(4) 0.002(3) -0.021(3) 0.023(3) C10 0.159(6) 0.113(5) 0.063(3) -0.001(3) 0.005(4) 0.033(4) C11 0.095(4) 0.085(4) 0.102(4) 0.011(3) 0.009(3) 0.005(3) C12 0.122(5) 0.045(3) 0.082(4) -0.001(3) 0.013(4) -0.002(3) C13 0.093(4) 0.053(3) 0.073(4) -0.013(3) 0.001(3) -0.014(3) C14 0.067(3) 0.044(2) 0.056(3) 0.000(2) -0.008(2) 0.000(2) C15 0.058(3) 0.049(2) 0.053(2) -0.004(2) -0.011(2) 0.008(2) C16 0.089(3) 0.049(3) 0.052(3) 0.006(2) -0.003(2) 0.000(2) C17 0.134(5) 0.074(4) 0.051(3) 0.004(3) 0.001(3) -0.006(4) C18 0.109(4) 0.070(3) 0.074(4) -0.003(3) 0.022(3) -0.025(3) C19 0.078(4) 0.064(3) 0.074(4) -0.011(3) -0.004(3) -0.016(3) C20 0.175(7) 0.125(6) 0.098(5) -0.013(4) 0.039(5) -0.059(5) C21 0.097(4) 0.081(4) 0.057(3) 0.007(3) -0.028(3) 0.005(3) C22 0.090(4) 0.089(4) 0.074(3) -0.024(3) -0.025(3) 0.007(3) C23 0.105(4) 0.087(4) 0.097(4) -0.004(3) -0.044(3) 0.033(3) C24 0.168(6) 0.158(6) 0.066(4) 0.036(4) -0.044(4) -0.016(5) C25 0.122(5) 0.058(3) 0.103(4) 0.007(3) -0.021(3) -0.013(3) C26 0.117(4) 0.077(4) 0.071(3) 0.015(3) -0.015(3) 0.011(3) C27 0.092(4) 0.113(5) 0.103(4) 0.012(4) -0.057(3) -0.011(3) C28 0.105(4) 0.083(4) 0.109(4) 0.023(3) 0.000(3) 0.033(3) C29 0.102(4) 0.095(4) 0.113(5) -0.003(4) -0.011(4) -0.034(3) C30 0.084(4) 0.111(4) 0.081(4) -0.016(3) -0.029(3) -0.014(3) C31A 0.113(15) 0.28(3) 0.136(17) -0.061(18) 0.042(12) -0.032(16) C32A 0.103(15) 0.22(3) 0.17(2) -0.074(19) -0.030(13) 0.055(15) C31B 0.14(2) 0.171(19) 0.26(3) -0.06(2) 0.11(2) -0.032(16) C32B 0.121(16) 0.19(2) 0.147(18) -0.052(14) -0.053(12) 0.105(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 Si1 N1 1.723(4) . ? Si1 C25 1.866(5) . ? Si1 C26 1.873(5) . ? Si1 Sc 3.2330(15) . ? Si2 N1 1.723(3) . ? Si2 C27 1.870(5) . ? Si2 C28 1.872(5) . ? Si2 Li 2.794(7) . ? Si3 N2 1.705(4) . ? Si3 C30 1.873(5) . ? Si3 C29 1.880(5) . ? Si4 N2 1.688(4) . ? Si4 C31B 1.741(19) . ? Si4 C32A 1.753(19) . ? Si4 C31A 2.04(2) . ? Si4 C32B 2.047(18) . ? Sc O1 1.987(3) . ? Sc O2 2.078(3) . ? Sc N2 2.111(3) . ? Sc N1 2.183(3) . ? Sc Li 2.818(7) . ? Sc S2 2.8629(14) . ? Sc S1 2.8725(14) . ? S1 C2 1.768(4) . ? S1 C12 1.817(6) . ? S2 C14 1.765(4) . ? S2 C13 1.795(5) . ? O1 C1 1.333(4) . ? O2 C15 1.339(5) . ? O2 Li 1.963(8) . ? O3 C33B 1.420(12) . ? O3 C36A 1.428(13) . ? O3 C36B 1.466(11) . ? O3 C33A 1.480(11) . ? O3 Li 1.871(8) . ? N1 Li 2.148(8) . ? C1 C6 1.411(5) . ? C1 C2 1.419(6) . ? C2 C3 1.392(6) . ? C3 C4 1.361(6) . ? C4 C5 1.390(6) . ? C4 C7 1.531(6) . ? C5 C6 1.379(6) . ? C6 C8 1.534(6) . ? C8 C10 1.528(6) . ? C8 C9 1.536(6) . ? C8 C11 1.537(7) . ? C12 C13 1.490(8) . ? C14 C19 1.384(6) . ? C14 C15 1.400(5) . ? C15 C16 1.414(6) . ? C16 C17 1.371(7) . ? C16 C21 1.534(6) . ? C17 C18 1.399(7) . ? C18 C19 1.363(7) . ? C18 C20 1.521(7) . ? C21 C22 1.522(7) . ? C21 C23 1.533(7) . ? C21 C24 1.546(6) . ? C33A C34A 1.432(14) . ? C34A C35A 1.534(17) . ? C35A C36A 1.423(17) . ? C33B C34B 1.494(17) . ? C34B C35B 1.566(19) . ? C35B C36B 1.540(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C25 113.8(2) . . ? N1 Si1 C26 114.8(2) . . ? C25 Si1 C26 107.5(2) . . ? N1 Si1 Sc 39.03(11) . . ? C25 Si1 Sc 129.94(17) . . ? C26 Si1 Sc 121.89(17) . . ? N1 Si2 C27 115.7(2) . . ? N1 Si2 C28 114.0(2) . . ? C27 Si2 C28 106.9(3) . . ? N1 Si2 Li 50.2(2) . . ? C27 Si2 Li 152.9(2) . . ? C28 Si2 Li 100.2(2) . . ? N2 Si3 C30 116.8(2) . . ? N2 Si3 C29 115.6(2) . . ? C30 Si3 C29 105.7(2) . . ? N2 Si4 C31B 118.1(8) . . ? N2 Si4 C32A 123.4(7) . . ? C31B Si4 C32A 68.2(10) . . ? N2 Si4 C31A 107.3(7) . . ? C31B Si4 C31A 35.0(9) . . ? C32A Si4 C31A 101.8(9) . . ? N2 Si4 C32B 106.0(5) . . ? C31B Si4 C32B 104.1(11) . . ? C32A Si4 C32B 35.9(8) . . ? C31A Si4 C32B 137.0(8) . . ? O1 Sc O2 152.66(11) . . ? O1 Sc N2 105.66(13) . . ? O2 Sc N2 93.11(12) . . ? O1 Sc N1 103.56(11) . . ? O2 Sc N1 89.25(11) . . ? N2 Sc N1 107.09(13) . . ? O1 Sc Li 152.13(17) . . ? O2 Sc Li 44.13(17) . . ? N2 Sc Li 89.23(18) . . ? N1 Sc Li 48.87(17) . . ? O1 Sc S2 86.59(9) . . ? O2 Sc S2 70.24(8) . . ? N2 Sc S2 159.39(10) . . ? N1 Sc S2 85.39(9) . . ? Li Sc S2 86.93(17) . . ? O1 Sc S1 71.26(8) . . ? O2 Sc S1 87.92(8) . . ? N2 Sc S1 94.39(10) . . ? N1 Sc S1 158.46(9) . . ? Li Sc S1 132.06(16) . . ? S2 Sc S1 73.56(4) . . ? O1 Sc Si1 88.45(8) . . ? O2 Sc Si1 112.64(8) . . ? N2 Sc Si1 87.08(10) . . ? N1 Sc Si1 29.80(9) . . ? Li Sc Si1 68.54(16) . . ? S2 Sc Si1 110.18(4) . . ? S1 Sc Si1 159.30(5) . . ? C2 S1 C12 100.3(3) . . ? C2 S1 Sc 93.98(15) . . ? C12 S1 Sc 106.7(2) . . ? C14 S2 C13 101.1(2) . . ? C14 S2 Sc 95.48(15) . . ? C13 S2 Sc 104.4(2) . . ? C1 O1 Sc 137.0(3) . . ? C15 O2 Li 119.7(3) . . ? C15 O2 Sc 132.2(2) . . ? Li O2 Sc 88.4(2) . . ? C33B O3 C36A 98.3(8) . . ? C33B O3 C36B 113.1(7) . . ? C36A O3 C36B 23.6(7) . . ? C33B O3 C33A 26.6(6) . . ? C36A O3 C33A 105.7(7) . . ? C36B O3 C33A 110.3(7) . . ? C33B O3 Li 127.9(6) . . ? C36A O3 Li 131.2(6) . . ? C36B O3 Li 119.0(6) . . ? C33A O3 Li 122.7(5) . . ? Si2 N1 Si1 116.68(18) . . ? Si2 N1 Li 91.7(3) . . ? Si1 N1 Li 124.1(3) . . ? Si2 N1 Sc 125.95(18) . . ? Si1 N1 Sc 111.17(17) . . ? Li N1 Sc 81.2(2) . . ? Si4 N2 Si3 119.7(2) . . ? Si4 N2 Sc 120.13(19) . . ? Si3 N2 Sc 120.10(18) . . ? O3 Li O2 133.7(5) . . ? O3 Li N1 128.7(4) . . ? O2 Li N1 93.4(3) . . ? O3 Li Si2 102.1(3) . . ? O2 Li Si2 102.0(3) . . ? N1 Li Si2 38.05(15) . . ? O3 Li Sc 178.7(4) . . ? O2 Li Sc 47.50(18) . . ? N1 Li Sc 49.97(17) . . ? Si2 Li Sc 76.81(18) . . ? O1 C1 C6 123.2(4) . . ? O1 C1 C2 118.8(4) . . ? C6 C1 C2 118.0(4) . . ? C3 C2 C1 121.1(4) . . ? C3 C2 S1 120.7(4) . . ? C1 C2 S1 118.2(3) . . ? C4 C3 C2 121.2(5) . . ? C3 C4 C5 117.2(4) . . ? C3 C4 C7 121.6(5) . . ? C5 C4 C7 121.2(5) . . ? C6 C5 C4 124.8(4) . . ? C5 C6 C1 117.7(4) . . ? C5 C6 C8 122.0(4) . . ? C1 C6 C8 120.3(4) . . ? C10 C8 C6 112.7(4) . . ? C10 C8 C9 108.1(4) . . ? C6 C8 C9 109.0(4) . . ? C10 C8 C11 106.9(5) . . ? C6 C8 C11 110.7(4) . . ? C9 C8 C11 109.3(4) . . ? C13 C12 S1 115.2(4) . . ? C12 C13 S2 115.0(4) . . ? C19 C14 C15 122.2(4) . . ? C19 C14 S2 119.9(3) . . ? C15 C14 S2 117.8(3) . . ? O2 C15 C14 119.2(4) . . ? O2 C15 C16 122.9(4) . . ? C14 C15 C16 117.8(4) . . ? C17 C16 C15 116.5(5) . . ? C17 C16 C21 122.0(4) . . ? C15 C16 C21 121.4(4) . . ? C16 C17 C18 125.9(5) . . ? C19 C18 C17 116.0(5) . . ? C19 C18 C20 121.7(6) . . ? C17 C18 C20 122.3(5) . . ? C18 C19 C14 120.7(5) . . ? C22 C21 C23 111.5(5) . . ? C22 C21 C16 110.8(4) . . ? C23 C21 C16 108.1(4) . . ? C22 C21 C24 107.5(5) . . ? C23 C21 C24 107.4(5) . . ? C16 C21 C24 111.5(4) . . ? C34A C33A O3 107.5(8) . . ? C33A C34A C35A 102.6(9) . . ? C36A C35A C34A 104.3(11) . . ? C35A C36A O3 110.0(11) . . ? O3 C33B C34B 105.3(10) . . ? C33B C34B C35B 107.6(11) . . ? C36B C35B C34B 100.9(10) . . ? O3 C36B C35B 104.5(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 N1 Si1 Sc O1 121.28(18) . . . . ? C25 Si1 Sc O1 -160.1(3) . . . . ? C26 Si1 Sc O1 30.3(2) . . . . ? N1 Si1 Sc O2 -40.81(18) . . . . ? C25 Si1 Sc O2 37.8(3) . . . . ? C26 Si1 Sc O2 -131.8(2) . . . . ? N1 Si1 Sc N2 -132.96(19) . . . . ? C25 Si1 Sc N2 -54.4(3) . . . . ? C26 Si1 Sc N2 136.1(2) . . . . ? C25 Si1 Sc N1 78.6(3) . . . . ? C26 Si1 Sc N1 -91.0(3) . . . . ? N1 Si1 Sc Li -42.6(2) . . . . ? C25 Si1 Sc Li 36.0(3) . . . . ? C26 Si1 Sc Li -133.6(3) . . . . ? N1 Si1 Sc S2 35.49(17) . . . . ? C25 Si1 Sc S2 114.1(3) . . . . ? C26 Si1 Sc S2 -55.5(2) . . . . ? N1 Si1 Sc S1 132.4(2) . . . . ? C25 Si1 Sc S1 -149.0(3) . . . . ? C26 Si1 Sc S1 41.4(3) . . . . ? O1 Sc S1 C2 6.45(17) . . . . ? O2 Sc S1 C2 168.44(16) . . . . ? N2 Sc S1 C2 -98.60(18) . . . . ? N1 Sc S1 C2 85.8(3) . . . . ? Li Sc S1 C2 168.5(3) . . . . ? S2 Sc S1 C2 98.44(15) . . . . ? Si1 Sc S1 C2 -5.3(2) . . . . ? O1 Sc S1 C12 -95.5(2) . . . . ? O2 Sc S1 C12 66.5(2) . . . . ? N2 Sc S1 C12 159.4(3) . . . . ? N1 Sc S1 C12 -16.2(4) . . . . ? Li Sc S1 C12 66.5(3) . . . . ? S2 Sc S1 C12 -3.5(2) . . . . ? Si1 Sc S1 C12 -107.2(3) . . . . ? O1 Sc S2 C14 154.61(16) . . . . ? O2 Sc S2 C14 -10.62(15) . . . . ? N2 Sc S2 C14 27.1(3) . . . . ? N1 Sc S2 C14 -101.48(16) . . . . ? Li Sc S2 C14 -52.5(2) . . . . ? S1 Sc S2 C14 83.16(14) . . . . ? Si1 Sc S2 C14 -118.30(14) . . . . ? O1 Sc S2 C13 51.7(2) . . . . ? O2 Sc S2 C13 -113.5(2) . . . . ? N2 Sc S2 C13 -75.8(4) . . . . ? N1 Sc S2 C13 155.6(2) . . . . ? Li Sc S2 C13 -155.4(3) . . . . ? S1 Sc S2 C13 -19.8(2) . . . . ? Si1 Sc S2 C13 138.8(2) . . . . ? O2 Sc O1 C1 -52.5(5) . . . . ? N2 Sc O1 C1 79.2(4) . . . . ? N1 Sc O1 C1 -168.4(4) . . . . ? Li Sc O1 C1 -160.8(5) . . . . ? S2 Sc O1 C1 -84.0(4) . . . . ? S1 Sc O1 C1 -10.2(3) . . . . ? Si1 Sc O1 C1 165.7(4) . . . . ? O1 Sc O2 C15 -10.3(4) . . . . ? N2 Sc O2 C15 -144.2(3) . . . . ? N1 Sc O2 C15 108.7(3) . . . . ? Li Sc O2 C15 130.1(4) . . . . ? S2 Sc O2 C15 23.4(3) . . . . ? S1 Sc O2 C15 -49.9(3) . . . . ? Si1 Sc O2 C15 127.7(3) . . . . ? O1 Sc O2 Li -140.4(3) . . . . ? N2 Sc O2 Li 85.7(3) . . . . ? N1 Sc O2 Li -21.4(3) . . . . ? S2 Sc O2 Li -106.8(2) . . . . ? S1 Sc O2 Li 180.0(2) . . . . ? Si1 Sc O2 Li -2.4(2) . . . . ? C27 Si2 N1 Si1 77.8(3) . . . . ? C28 Si2 N1 Si1 -46.8(3) . . . . ? Li Si2 N1 Si1 -130.0(3) . . . . ? C27 Si2 N1 Li -152.3(3) . . . . ? C28 Si2 N1 Li 83.1(3) . . . . ? C27 Si2 N1 Sc -71.9(3) . . . . ? C28 Si2 N1 Sc 163.5(2) . . . . ? Li Si2 N1 Sc 80.3(3) . . . . ? C25 Si1 N1 Si2 81.2(3) . . . . ? C26 Si1 N1 Si2 -43.3(3) . . . . ? Sc Si1 N1 Si2 -154.0(3) . . . . ? C25 Si1 N1 Li -31.2(4) . . . . ? C26 Si1 N1 Li -155.7(3) . . . . ? Sc Si1 N1 Li 93.6(3) . . . . ? C25 Si1 N1 Sc -124.8(2) . . . . ? C26 Si1 N1 Sc 110.7(2) . . . . ? O1 Sc N1 Si2 89.6(2) . . . . ? O2 Sc N1 Si2 -66.0(2) . . . . ? N2 Sc N1 Si2 -159.0(2) . . . . ? Li Sc N1 Si2 -85.7(3) . . . . ? S2 Sc N1 Si2 4.25(19) . . . . ? S1 Sc N1 Si2 16.4(4) . . . . ? Si1 Sc N1 Si2 151.1(3) . . . . ? O1 Sc N1 Si1 -61.50(18) . . . . ? O2 Sc N1 Si1 142.90(16) . . . . ? N2 Sc N1 Si1 49.88(19) . . . . ? Li Sc N1 Si1 123.2(3) . . . . ? S2 Sc N1 Si1 -146.86(15) . . . . ? S1 Sc N1 Si1 -134.7(2) . . . . ? O1 Sc N1 Li 175.3(2) . . . . ? O2 Sc N1 Li 19.7(2) . . . . ? N2 Sc N1 Li -73.3(3) . . . . ? S2 Sc N1 Li 89.9(2) . . . . ? S1 Sc N1 Li 102.1(3) . . . . ? Si1 Sc N1 Li -123.2(3) . . . . ? C31B Si4 N2 Si3 -49.0(11) . . . . ? C32A Si4 N2 Si3 32.2(11) . . . . ? C31A Si4 N2 Si3 -85.4(6) . . . . ? C32B Si4 N2 Si3 67.1(7) . . . . ? C31B Si4 N2 Sc 127.6(11) . . . . ? C32A Si4 N2 Sc -151.1(11) . . . . ? C31A Si4 N2 Sc 91.3(6) . . . . ? C32B Si4 N2 Sc -116.3(7) . . . . ? C30 Si3 N2 Si4 -64.8(3) . . . . ? C29 Si3 N2 Si4 60.5(3) . . . . ? C30 Si3 N2 Sc 118.6(3) . . . . ? C29 Si3 N2 Sc -116.1(3) . . . . ? O1 Sc N2 Si4 -31.8(3) . . . . ? O2 Sc N2 Si4 128.1(2) . . . . ? N1 Sc N2 Si4 -141.7(2) . . . . ? Li Sc N2 Si4 172.1(3) . . . . ? S2 Sc N2 Si4 92.9(3) . . . . ? S1 Sc N2 Si4 40.0(2) . . . . ? Si1 Sc N2 Si4 -119.3(2) . . . . ? O1 Sc N2 Si3 144.8(2) . . . . ? O2 Sc N2 Si3 -55.3(2) . . . . ? N1 Sc N2 Si3 34.9(2) . . . . ? Li Sc N2 Si3 -11.3(3) . . . . ? S2 Sc N2 Si3 -90.5(3) . . . . ? S1 Sc N2 Si3 -143.41(19) . . . . ? Si1 Sc N2 Si3 57.3(2) . . . . ? C33B O3 Li O2 133.4(8) . . . . ? C36A O3 Li O2 -69.2(10) . . . . ? C36B O3 Li O2 -44.4(9) . . . . ? C33A O3 Li O2 101.3(8) . . . . ? C33B O3 Li N1 -76.0(9) . . . . ? C36A O3 Li N1 81.4(10) . . . . ? C36B O3 Li N1 106.2(8) . . . . ? C33A O3 Li N1 -108.1(7) . . . . ? C33B O3 Li Si2 -106.6(8) . . . . ? C36A O3 Li Si2 50.7(9) . . . . ? C36B O3 Li Si2 75.6(7) . . . . ? C33A O3 Li Si2 -138.7(6) . . . . ? C33B O3 Li Sc -71(19) . . . . ? C36A O3 Li Sc 86(19) . . . . ? C36B O3 Li Sc 111(19) . . . . ? C33A O3 Li Sc -103(19) . . . . ? C15 O2 Li O3 40.0(7) . . . . ? Sc O2 Li O3 179.2(6) . . . . ? C15 O2 Li N1 -117.5(3) . . . . ? Sc O2 Li N1 21.8(3) . . . . ? C15 O2 Li Si2 -80.0(4) . . . . ? Sc O2 Li Si2 59.3(2) . . . . ? C15 O2 Li Sc -139.3(3) . . . . ? Si2 N1 Li O3 -54.0(5) . . . . ? Si1 N1 Li O3 70.2(6) . . . . ? Sc N1 Li O3 179.8(5) . . . . ? Si2 N1 Li O2 105.2(3) . . . . ? Si1 N1 Li O2 -130.6(3) . . . . ? Sc N1 Li O2 -20.9(2) . . . . ? Si1 N1 Li Si2 124.2(3) . . . . ? Sc N1 Li Si2 -126.14(17) . . . . ? Si2 N1 Li Sc 126.14(17) . . . . ? Si1 N1 Li Sc -109.6(3) . . . . ? N1 Si2 Li O3 139.8(4) . . . . ? C27 Si2 Li O3 -153.1(5) . . . . ? C28 Si2 Li O3 26.9(4) . . . . ? N1 Si2 Li O2 -80.0(3) . . . . ? C27 Si2 Li O2 -12.9(8) . . . . ? C28 Si2 Li O2 167.1(3) . . . . ? C27 Si2 Li N1 67.2(6) . . . . ? C28 Si2 Li N1 -112.9(3) . . . . ? N1 Si2 Li Sc -39.43(16) . . . . ? C27 Si2 Li Sc 27.7(6) . . . . ? C28 Si2 Li Sc -152.3(2) . . . . ? O1 Sc Li O3 -15(19) . . . . ? O2 Sc Li O3 -156(19) . . . . ? N2 Sc Li O3 109(19) . . . . ? N1 Sc Li O3 -5(19) . . . . ? S2 Sc Li O3 -92(19) . . . . ? S1 Sc Li O3 -156(19) . . . . ? Si1 Sc Li O3 21(19) . . . . ? O1 Sc Li O2 141.2(3) . . . . ? N2 Sc Li O2 -95.3(2) . . . . ? N1 Sc Li O2 151.0(3) . . . . ? S2 Sc Li O2 64.48(19) . . . . ? S1 Sc Li O2 0.0(3) . . . . ? Si1 Sc Li O2 177.6(2) . . . . ? O1 Sc Li N1 -9.8(5) . . . . ? O2 Sc Li N1 -151.0(3) . . . . ? N2 Sc Li N1 113.7(2) . . . . ? S2 Sc Li N1 -86.56(18) . . . . ? S1 Sc Li N1 -151.09(14) . . . . ? Si1 Sc Li N1 26.54(15) . . . . ? O1 Sc Li Si2 20.9(5) . . . . ? O2 Sc Li Si2 -120.3(3) . . . . ? N2 Sc Li Si2 144.44(17) . . . . ? N1 Sc Li Si2 30.75(13) . . . . ? S2 Sc Li Si2 -55.82(13) . . . . ? S1 Sc Li Si2 -120.34(14) . . . . ? Si1 Sc Li Si2 57.29(11) . . . . ? Sc O1 C1 C6 -169.3(3) . . . . ? Sc O1 C1 C2 9.5(6) . . . . ? O1 C1 C2 C3 -177.6(4) . . . . ? C6 C1 C2 C3 1.3(6) . . . . ? O1 C1 C2 S1 1.1(5) . . . . ? C6 C1 C2 S1 180.0(3) . . . . ? C12 S1 C2 C3 -79.2(4) . . . . ? Sc S1 C2 C3 173.1(4) . . . . ? C12 S1 C2 C1 102.1(4) . . . . ? Sc S1 C2 C1 -5.7(3) . . . . ? C1 C2 C3 C4 -0.1(7) . . . . ? S1 C2 C3 C4 -178.8(4) . . . . ? C2 C3 C4 C5 -0.8(7) . . . . ? C2 C3 C4 C7 179.0(4) . . . . ? C3 C4 C5 C6 0.5(7) . . . . ? C7 C4 C5 C6 -179.3(4) . . . . ? C4 C5 C6 C1 0.7(7) . . . . ? C4 C5 C6 C8 -176.8(4) . . . . ? O1 C1 C6 C5 177.3(4) . . . . ? C2 C1 C6 C5 -1.5(6) . . . . ? O1 C1 C6 C8 -5.2(6) . . . . ? C2 C1 C6 C8 176.0(4) . . . . ? C5 C6 C8 C10 -1.5(7) . . . . ? C1 C6 C8 C10 -178.9(4) . . . . ? C5 C6 C8 C9 118.6(5) . . . . ? C1 C6 C8 C9 -58.9(5) . . . . ? C5 C6 C8 C11 -121.2(5) . . . . ? C1 C6 C8 C11 61.4(6) . . . . ? C2 S1 C12 C13 -63.3(5) . . . . ? Sc S1 C12 C13 34.0(5) . . . . ? S1 C12 C13 S2 -59.7(6) . . . . ? C14 S2 C13 C12 -48.6(5) . . . . ? Sc S2 C13 C12 50.1(5) . . . . ? C13 S2 C14 C19 -68.4(4) . . . . ? Sc S2 C14 C19 -174.3(4) . . . . ? C13 S2 C14 C15 109.3(4) . . . . ? Sc S2 C14 C15 3.4(3) . . . . ? Li O2 C15 C14 88.8(5) . . . . ? Sc O2 C15 C14 -29.5(5) . . . . ? Li O2 C15 C16 -92.2(5) . . . . ? Sc O2 C15 C16 149.5(3) . . . . ? C19 C14 C15 O2 -171.5(4) . . . . ? S2 C14 C15 O2 10.9(5) . . . . ? C19 C14 C15 C16 9.5(6) . . . . ? S2 C14 C15 C16 -168.2(3) . . . . ? O2 C15 C16 C17 172.6(4) . . . . ? C14 C15 C16 C17 -8.4(6) . . . . ? O2 C15 C16 C21 -11.3(6) . . . . ? C14 C15 C16 C21 167.7(4) . . . . ? C15 C16 C17 C18 1.5(8) . . . . ? C21 C16 C17 C18 -174.5(5) . . . . ? C16 C17 C18 C19 4.8(9) . . . . ? C16 C17 C18 C20 -175.5(6) . . . . ? C17 C18 C19 C14 -3.9(8) . . . . ? C20 C18 C19 C14 176.3(5) . . . . ? C15 C14 C19 C18 -3.1(8) . . . . ? S2 C14 C19 C18 174.5(4) . . . . ? C17 C16 C21 C22 -116.2(5) . . . . ? C15 C16 C21 C22 67.9(6) . . . . ? C17 C16 C21 C23 121.3(5) . . . . ? C15 C16 C21 C23 -54.6(6) . . . . ? C17 C16 C21 C24 3.4(7) . . . . ? C15 C16 C21 C24 -172.4(5) . . . . ? C33B O3 C33A C34A 95(2) . . . . ? C36A O3 C33A C34A 18.1(11) . . . . ? C36B O3 C33A C34A -6.3(11) . . . . ? Li O3 C33A C34A -154.5(7) . . . . ? O3 C33A C34A C35A -29.5(13) . . . . ? C33A C34A C35A C36A 30.5(16) . . . . ? C34A C35A C36A O3 -20.3(16) . . . . ? C33B O3 C36A C35A -23.7(13) . . . . ? C36B O3 C36A C35A 107(3) . . . . ? C33A O3 C36A C35A 2.4(13) . . . . ? Li O3 C36A C35A 174.2(8) . . . . ? C36A O3 C33B C34B 22.4(12) . . . . ? C36B O3 C33B C34B 3.3(13) . . . . ? C33A O3 C33B C34B -86.2(19) . . . . ? Li O3 C33B C34B -174.7(8) . . . . ? O3 C33B C34B C35B 15.6(16) . . . . ? C33B C34B C35B C36B -27.0(17) . . . . ? C33B O3 C36B C35B -20.8(12) . . . . ? C36A O3 C36B C35B -75(2) . . . . ? C33A O3 C36B C35B 7.7(11) . . . . ? Li O3 C36B C35B 157.3(7) . . . . ? C34B C35B C36B O3 27.8(14) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.302 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.049 #===END