# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_glu14ges _database_code_depnum_ccdc_archive 'CCDC 837993' #TrackingRef 'analogues_of_ec23.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H22 O2' _chemical_formula_sum 'C22 H22 O2' _chemical_formula_weight 318.40 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' _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 6.6502(19) _cell_length_b 8.0811(19) _cell_length_c 18.466(5) _cell_angle_alpha 80.28(3) _cell_angle_beta 84.36(3) _cell_angle_gamma 66.24(3) _cell_volume 894.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2258 _cell_measurement_theta_min 4.75 _cell_measurement_theta_max 23.65 _exptl_crystal_description ultra_thin_plate _exptl_crystal_colour colorless _exptl_crystal_size_max .50 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 340 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate_Stoe-IPDS _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12799 _diffrn_reflns_av_R_equivalents 0.0927 _diffrn_reflns_av_sigmaI/netI 0.0931 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 29.17 _reflns_number_total 4485 _reflns_number_gt 2531 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. C02 apparantly partly disordered and likewise all the nearby hydrogens. But this was not fully incorporated in the model. Therefore some unrealistic short H ... H contacts. TITL glu14g solved by Sir2004 CELL 0.71073 6.6502 8.0811 18.4657 80.283 84.356 66.240 ZERR 2. 0.0019 0.0019 0.0049 0.030 0.033 0.029 LATT 1 SFAC C H O UNIT 44 44 4 L.S. 12 TEMP -100 ACTA CONF HTAB 2.5 FMAP 2 PLAN 25 WGHT 0.100500 FVAR 0.38139 0.89610 PART 1 C1 1 0.402166 0.373044 0.625589 11.00000 0.05683 0.04138 = 0.05953 -0.00096 -0.02787 -0.00591 AFIX 137 H1A 2 0.322256 0.359748 0.672228 11.00000 -1.50000 H1B 2 0.300580 0.414852 0.585075 11.00000 -1.50000 H1C 2 0.466176 0.462610 0.626684 11.00000 -1.50000 AFIX 0 C2 1 0.724477 0.211848 0.546185 11.00000 0.07233 0.07969 = 0.03620 0.00778 -0.00848 -0.03183 AFIX 137 H2A 2 0.787725 0.299425 0.551662 11.00000 -1.50000 H2B 2 0.632729 0.256903 0.502967 11.00000 -1.50000 H2C 2 0.843085 0.093600 0.539957 11.00000 -1.50000 AFIX 0 C3 1 0.477358 -0.225360 0.699405 11.00000 0.04350 0.05087 = 0.06177 -0.02067 0.00044 -0.02743 AFIX 137 H3A 2 0.570369 -0.344952 0.724913 11.00000 -1.50000 H3B 2 0.384641 -0.241246 0.665312 11.00000 -1.50000 H3C 2 0.384050 -0.148747 0.735479 11.00000 -1.50000 AFIX 0 C4 1 0.791853 -0.268285 0.609893 11.00000 0.05228 0.05048 = 0.05268 -0.02633 0.00671 -0.02210 AFIX 137 H4A 2 0.886848 -0.211695 0.582174 11.00000 -1.50000 H4B 2 0.715828 -0.301712 0.575598 11.00000 -1.50000 H4C 2 0.881416 -0.378104 0.642035 11.00000 -1.50000 AFIX 0 C5 1 0.739036 -0.071532 0.706565 11.00000 0.02494 0.02446 = 0.03074 -0.00527 -0.00250 -0.00887 C6 1 0.726337 0.104140 0.681490 11.00000 0.02998 0.02625 = 0.02829 -0.00373 -0.00440 -0.00941 C7 1 0.836647 0.180757 0.716262 11.00000 0.03206 0.02417 = 0.03551 -0.00493 -0.00438 -0.01272 AFIX 43 H7 2 0.827934 0.300766 0.698506 11.00000 -1.20000 AFIX 0 C8 1 0.960963 0.080044 0.777722 11.00000 0.02635 0.03295 = 0.03099 -0.00970 -0.00147 -0.01251 C9 1 0.963218 -0.092897 0.804839 11.00000 0.03077 0.03502 = 0.02971 -0.00094 -0.00739 -0.01246 AFIX 43 H9 2 1.040578 -0.159150 0.848047 11.00000 -1.20000 AFIX 0 C10 1 0.853744 -0.169118 0.769394 11.00000 0.03223 0.02533 = 0.03476 0.00028 -0.00554 -0.01147 AFIX 43 H10 2 0.857273 -0.287236 0.787994 11.00000 -1.20000 AFIX 0 C11 1 1.094315 0.147787 0.810744 11.00000 0.02895 0.03640 = 0.03516 -0.01045 -0.00129 -0.01342 C12 1 1.219710 0.193929 0.836046 11.00000 0.02842 0.03758 = 0.03494 -0.00910 -0.00252 -0.01412 C13 1 1.368530 0.249775 0.867119 11.00000 0.02592 0.03741 = 0.02966 -0.00954 -0.00049 -0.01433 C14 1 1.358552 0.427071 0.848967 11.00000 0.03083 0.03468 = 0.04015 -0.00596 -0.01101 -0.01136 AFIX 43 H14 2 1.252924 0.512308 0.815457 11.00000 -1.20000 AFIX 0 C15 1 1.501599 0.480370 0.879405 11.00000 0.03309 0.03172 = 0.03635 -0.00436 -0.00820 -0.01324 AFIX 43 H15 2 1.492787 0.602025 0.867040 11.00000 -1.20000 AFIX 0 C16 1 1.658087 0.355790 0.928059 11.00000 0.02472 0.03352 = 0.02582 -0.00555 -0.00108 -0.01473 C17 1 1.670323 0.179300 0.946069 11.00000 0.03152 0.03453 = 0.03067 -0.00120 -0.00572 -0.01537 AFIX 43 H17 2 1.777030 0.094353 0.979311 11.00000 -1.20000 AFIX 0 C18 1 1.527454 0.125333 0.915841 11.00000 0.03424 0.03147 = 0.03395 -0.00301 -0.00351 -0.01812 AFIX 43 H18 2 1.537440 0.003357 0.928245 11.00000 -1.20000 AFIX 0 C19 1 1.811302 0.416542 0.958740 11.00000 0.02707 0.03326 = 0.02484 -0.00255 -0.00332 -0.01351 SADI C01 C02 C01B C02B C03 C02 C03B C02B EXYZ C01 C01B EADP C01 C01B EXYZ C03 C03B EADP C03 C03B C01 1 0.584746 0.189543 0.614370 21.00000 0.04618 0.02971 = 0.03411 -0.00087 -0.01459 -0.01439 C02 1 0.476721 0.050888 0.613060 21.00000 0.04024 0.03364 = 0.03890 -0.00604 -0.01270 -0.01398 AFIX 23 H10A 2 0.326987 0.096002 0.635970 21.00000 -1.20000 H10B 2 0.465435 0.035618 0.561733 21.00000 -1.20000 AFIX 0 C03 1 0.622802 -0.133312 0.656421 21.00000 0.03449 0.02679 = 0.03643 -0.00767 -0.00584 -0.01232 PART 2 C01B 1 0.584746 0.189543 0.614370 -21.00000 0.04618 0.02971 = 0.03411 -0.00087 -0.01459 -0.01439 ISOR .005 C02B C02B 1 0.605762 0.015616 0.583737 -21.00000 0.02768 0.02615 = 0.03001 -0.00353 -0.00597 -0.00817 AFIX 23 H02A 2 0.739036 -0.027594 0.551439 -21.00000 -1.20000 H02B 2 0.475348 0.039737 0.555517 -21.00000 -1.20000 AFIX 0 C03B 1 0.622802 -0.133312 0.656421 -21.00000 0.03449 0.02679 = 0.03643 -0.00767 -0.00584 -0.01232 PART 1 O1 3 1.803194 0.574804 0.939175 11.00000 0.04345 0.03585 = 0.04014 0.00294 -0.01280 -0.02249 O2 3 1.949026 0.298556 1.005645 11.00000 0.03618 0.04053 = 0.03550 0.00121 -0.01359 -0.02002 AFIX 147 H2 2 2.028419 0.345322 1.019395 11.00000 -1.50000 HKLF 4 REM glu14g solved by Sir2004 REM R1 = 0.0579 for 2531 Fo > 4sig(Fo) and 0.1034 for all 4485 data REM 232 parameters refined using 12 restraints END WGHT 0.1004 0.0000 REM Highest difference peak 0.368, deepest hole -0.261, 1-sigma level 0.056 Q1 1 0.4254 -0.1137 0.6695 11.00000 0.05 0.37 Q2 1 1.9507 0.5638 0.9372 11.00000 0.05 0.29 Q3 1 1.7438 0.3854 0.9408 11.00000 0.05 0.29 Q4 1 1.4535 0.4350 0.8572 11.00000 0.05 0.28 Q5 1 1.9558 0.5647 0.8807 11.00000 0.05 0.23 Q6 1 1.9326 0.4757 0.9834 11.00000 0.05 0.22 Q7 1 1.5973 0.1440 0.9372 11.00000 0.05 0.20 Q8 1 1.0397 0.1059 0.7881 11.00000 0.05 0.20 Q9 1 1.4931 0.3642 0.9382 11.00000 0.05 0.19 Q10 1 1.0076 0.1235 0.7978 11.00000 0.05 0.19 Q11 1 2.0635 0.4860 0.9048 11.00000 0.05 0.19 Q12 1 2.1484 0.2805 0.9768 11.00000 0.05 0.19 Q13 1 0.8052 0.1256 0.6991 11.00000 0.05 0.19 Q14 1 1.5219 0.3859 0.7926 11.00000 0.05 0.18 Q15 1 0.3099 -0.0897 0.6916 11.00000 0.05 0.18 Q16 1 0.3875 0.2526 0.6351 11.00000 0.05 0.18 Q17 1 0.7988 -0.3029 0.7925 11.00000 0.05 0.18 Q18 1 0.8602 0.2357 0.5477 11.00000 0.05 0.18 Q19 1 0.6899 -0.0976 0.6883 11.00000 0.05 0.18 Q20 1 1.7979 0.3142 0.8598 11.00000 0.05 0.18 Q21 1 1.2634 0.1199 0.8018 11.00000 0.05 0.18 Q22 1 2.1573 0.2198 1.0109 11.00000 0.05 0.18 Q23 1 1.2244 0.0335 0.8552 11.00000 0.05 0.17 Q24 1 1.1278 -0.2190 0.8018 11.00000 0.05 0.17 Q25 1 1.6528 0.5957 0.9257 11.00000 0.05 0.17 ; _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^)+(0.1005P)^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 4485 _refine_ls_number_parameters 232 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1034 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1664 _refine_ls_wR_factor_gt 0.1443 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.903 _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 C1 C 0.4022(4) 0.3730(3) 0.62559(12) 0.0558(6) Uani 1 1 d . A 1 H1A H 0.3223 0.3597 0.6722 0.084 Uiso 1 1 calc R A 1 H1B H 0.3006 0.4149 0.5851 0.084 Uiso 1 1 calc R A 1 H1C H 0.4662 0.4626 0.6267 0.084 Uiso 1 1 calc R A 1 C2 C 0.7245(4) 0.2118(4) 0.54619(11) 0.0637(7) Uani 1 1 d . A 1 H2A H 0.7877 0.2994 0.5517 0.095 Uiso 1 1 calc R A 1 H2B H 0.6327 0.2569 0.5030 0.095 Uiso 1 1 calc R A 1 H2C H 0.8431 0.0936 0.5400 0.095 Uiso 1 1 calc R A 1 C3 C 0.4774(3) -0.2254(3) 0.69941(12) 0.0477(5) Uani 1 1 d . A 1 H3A H 0.5704 -0.3450 0.7249 0.072 Uiso 1 1 calc R A 1 H3B H 0.3846 -0.2412 0.6653 0.072 Uiso 1 1 calc R A 1 H3C H 0.3841 -0.1487 0.7355 0.072 Uiso 1 1 calc R A 1 C4 C 0.7919(4) -0.2683(3) 0.60989(11) 0.0494(5) Uani 1 1 d . A 1 H4A H 0.8868 -0.2117 0.5822 0.074 Uiso 1 1 calc R A 1 H4B H 0.7158 -0.3017 0.5756 0.074 Uiso 1 1 calc R A 1 H4C H 0.8814 -0.3781 0.6420 0.074 Uiso 1 1 calc R A 1 C5 C 0.7390(3) -0.0715(2) 0.70657(8) 0.0267(4) Uani 1 1 d . A 1 C6 C 0.7263(3) 0.1041(2) 0.68149(8) 0.0285(4) Uani 1 1 d . A 1 C7 C 0.8366(3) 0.1808(2) 0.71626(8) 0.0297(4) Uani 1 1 d . A 1 H7 H 0.8279 0.3008 0.6985 0.036 Uiso 1 1 calc R A 1 C8 C 0.9610(3) 0.0800(2) 0.77772(8) 0.0291(4) Uani 1 1 d . A 1 C9 C 0.9632(3) -0.0929(3) 0.80484(8) 0.0320(4) Uani 1 1 d . A 1 H9 H 1.0406 -0.1591 0.8480 0.038 Uiso 1 1 calc R A 1 C10 C 0.8537(3) -0.1691(2) 0.76939(8) 0.0310(4) Uani 1 1 d . A 1 H10 H 0.8573 -0.2872 0.7880 0.037 Uiso 1 1 calc R A 1 C11 C 1.0943(3) 0.1478(3) 0.81074(9) 0.0326(4) Uani 1 1 d . A 1 C12 C 1.2197(3) 0.1939(3) 0.83605(9) 0.0327(4) Uani 1 1 d . A 1 C13 C 1.3685(3) 0.2498(3) 0.86712(8) 0.0298(4) Uani 1 1 d . A 1 C14 C 1.3586(3) 0.4271(3) 0.84897(9) 0.0349(4) Uani 1 1 d . A 1 H14 H 1.2529 0.5123 0.8155 0.042 Uiso 1 1 calc R A 1 C15 C 1.5016(3) 0.4804(3) 0.87941(9) 0.0331(4) Uani 1 1 d . A 1 H15 H 1.4928 0.6020 0.8670 0.040 Uiso 1 1 calc R A 1 C16 C 1.6581(3) 0.3558(2) 0.92806(8) 0.0268(4) Uani 1 1 d . A 1 C17 C 1.6703(3) 0.1793(3) 0.94607(8) 0.0316(4) Uani 1 1 d . A 1 H17 H 1.7770 0.0944 0.9793 0.038 Uiso 1 1 calc R A 1 C18 C 1.5275(3) 0.1253(3) 0.91584(8) 0.0316(4) Uani 1 1 d . A 1 H18 H 1.5374 0.0034 0.9282 0.038 Uiso 1 1 calc R A 1 C19 C 1.8113(3) 0.4165(2) 0.95874(8) 0.0279(4) Uani 1 1 d . A 1 C01 C 0.5847(3) 0.1895(3) 0.61437(9) 0.0363(4) Uani 0.896(6) 1 d PD A 1 C02 C 0.4767(4) 0.0509(3) 0.61306(12) 0.0368(7) Uani 0.896(6) 1 d PD A 1 H10A H 0.3270 0.0960 0.6360 0.044 Uiso 0.896(6) 1 calc PR A 1 H10B H 0.4654 0.0356 0.5617 0.044 Uiso 0.896(6) 1 calc PR A 1 C03 C 0.6228(3) -0.1333(2) 0.65642(9) 0.0317(4) Uani 0.896(6) 1 d PD A 1 C01B C 0.5847(3) 0.1895(3) 0.61437(9) 0.0363(4) Uani 0.104(6) 1 d PD A 2 C02B C 0.606(3) 0.0156(15) 0.5837(7) 0.028(5) Uani 0.104(6) 1 d PDU A 2 H02A H 0.7390 -0.0276 0.5514 0.034 Uiso 0.104(6) 1 calc PR A 2 H02B H 0.4753 0.0397 0.5555 0.034 Uiso 0.104(6) 1 calc PR A 2 C03B C 0.6228(3) -0.1333(2) 0.65642(9) 0.0317(4) Uani 0.104(6) 1 d PD A 2 O1 O 1.8032(2) 0.57480(18) 0.93917(6) 0.0378(3) Uani 1 1 d . A 1 O2 O 1.9490(2) 0.29856(18) 1.00564(6) 0.0357(3) Uani 1 1 d . A 1 H2 H 2.0284 0.3453 1.0194 0.054 Uiso 1 1 calc R A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0568(13) 0.0414(12) 0.0595(12) -0.0010(10) -0.0279(10) -0.0059(10) C2 0.0723(16) 0.0797(18) 0.0362(10) 0.0078(10) -0.0085(10) -0.0318(14) C3 0.0435(11) 0.0509(13) 0.0618(12) -0.0207(10) 0.0004(9) -0.0274(10) C4 0.0523(12) 0.0505(13) 0.0527(11) -0.0263(10) 0.0067(9) -0.0221(10) C5 0.0249(8) 0.0245(9) 0.0307(7) -0.0053(6) -0.0025(6) -0.0089(6) C6 0.0300(8) 0.0262(9) 0.0283(7) -0.0037(6) -0.0044(6) -0.0094(7) C7 0.0321(8) 0.0242(9) 0.0355(8) -0.0049(6) -0.0044(6) -0.0127(7) C8 0.0263(8) 0.0330(10) 0.0310(8) -0.0097(6) -0.0015(6) -0.0125(7) C9 0.0308(8) 0.0350(10) 0.0297(8) -0.0009(7) -0.0074(6) -0.0125(7) C10 0.0322(8) 0.0253(9) 0.0348(8) 0.0003(6) -0.0055(6) -0.0115(7) C11 0.0290(8) 0.0364(10) 0.0352(8) -0.0104(7) -0.0013(6) -0.0134(7) C12 0.0284(8) 0.0376(10) 0.0349(8) -0.0091(7) -0.0025(6) -0.0141(7) C13 0.0259(8) 0.0374(10) 0.0297(7) -0.0095(7) -0.0005(6) -0.0143(7) C14 0.0308(9) 0.0347(10) 0.0401(9) -0.0060(7) -0.0110(7) -0.0114(8) C15 0.0331(9) 0.0317(10) 0.0363(8) -0.0044(7) -0.0082(7) -0.0132(7) C16 0.0247(7) 0.0335(9) 0.0258(7) -0.0055(6) -0.0011(6) -0.0147(7) C17 0.0315(8) 0.0345(10) 0.0307(7) -0.0012(7) -0.0057(6) -0.0154(7) C18 0.0342(9) 0.0315(10) 0.0340(8) -0.0030(7) -0.0035(7) -0.0181(7) C19 0.0271(8) 0.0333(10) 0.0248(7) -0.0025(6) -0.0033(6) -0.0135(7) C01 0.0462(10) 0.0297(10) 0.0341(8) -0.0009(7) -0.0146(7) -0.0144(8) C02 0.0402(14) 0.0336(12) 0.0389(11) -0.0060(8) -0.0127(9) -0.0140(9) C03 0.0345(9) 0.0268(9) 0.0364(8) -0.0077(7) -0.0058(7) -0.0123(7) C01B 0.0462(10) 0.0297(10) 0.0341(8) -0.0009(7) -0.0146(7) -0.0144(8) C02B 0.028(6) 0.026(6) 0.030(6) -0.004(4) -0.006(4) -0.008(4) C03B 0.0345(9) 0.0268(9) 0.0364(8) -0.0077(7) -0.0058(7) -0.0123(7) O1 0.0435(7) 0.0358(8) 0.0401(6) 0.0029(5) -0.0128(5) -0.0225(6) O2 0.0362(7) 0.0405(8) 0.0355(6) 0.0012(5) -0.0136(5) -0.0200(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C01 1.523(3) . ? C2 C01 1.520(3) . ? C3 C03 1.532(3) . ? C4 C03 1.526(3) . ? C5 C6 1.388(2) . ? C5 C10 1.389(2) . ? C5 C03 1.521(2) . ? C6 C7 1.388(2) . ? C6 C01 1.522(2) . ? C7 C8 1.402(2) . ? C8 C9 1.397(3) . ? C8 C11 1.438(2) . ? C9 C10 1.389(2) . ? C11 C12 1.199(2) . ? C12 C13 1.439(2) . ? C13 C14 1.391(3) . ? C13 C18 1.401(2) . ? C14 C15 1.387(2) . ? C15 C16 1.392(2) . ? C16 C17 1.380(3) . ? C16 C19 1.487(2) . ? C17 C18 1.387(2) . ? C19 O1 1.250(2) . ? C19 O2 1.2929(19) . ? C01 C02 1.560(3) . ? C02 C03 1.545(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C5 C10 119.95(16) . . ? C6 C5 C03 111.69(14) . . ? C10 C5 C03 128.33(16) . . ? C5 C6 C7 120.75(14) . . ? C5 C6 C01 111.48(15) . . ? C7 C6 C01 127.77(16) . . ? C6 C7 C8 119.62(16) . . ? C9 C8 C7 119.14(16) . . ? C9 C8 C11 119.70(15) . . ? C7 C8 C11 121.09(16) . . ? C10 C9 C8 120.81(14) . . ? C9 C10 C5 119.58(16) . . ? C12 C11 C8 174.84(18) . . ? C11 C12 C13 179.35(18) . . ? C14 C13 C18 118.90(16) . . ? C14 C13 C12 120.78(15) . . ? C18 C13 C12 120.32(17) . . ? C15 C14 C13 120.52(16) . . ? C14 C15 C16 120.07(17) . . ? C17 C16 C15 119.88(16) . . ? C17 C16 C19 121.42(14) . . ? C15 C16 C19 118.70(16) . . ? C16 C17 C18 120.28(15) . . ? C17 C18 C13 120.35(17) . . ? O1 C19 O2 123.05(15) . . ? O1 C19 C16 120.24(14) . . ? O2 C19 C16 116.71(15) . . ? C2 C01 C6 110.74(16) . . ? C2 C01 C1 110.07(18) . . ? C6 C01 C1 111.58(15) . . ? C2 C01 C02 114.59(18) . . ? C6 C01 C02 101.66(14) . . ? C1 C01 C02 107.95(18) . . ? C03 C02 C01 107.85(16) . . ? C5 C03 C4 109.91(15) . . ? C5 C03 C3 112.39(14) . . ? C4 C03 C3 108.41(17) . . ? C5 C03 C02 101.42(15) . . ? C4 C03 C02 115.14(16) . . ? C3 C03 C02 109.54(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 C5 C6 C7 3.4(2) . . . . ? C03 C5 C6 C7 -174.93(14) . . . . ? C10 C5 C6 C01 -177.30(15) . . . . ? C03 C5 C6 C01 4.40(19) . . . . ? C5 C6 C7 C8 -0.5(2) . . . . ? C01 C6 C7 C8 -179.68(15) . . . . ? C6 C7 C8 C9 -2.9(2) . . . . ? C6 C7 C8 C11 173.91(15) . . . . ? C7 C8 C9 C10 3.4(2) . . . . ? C11 C8 C9 C10 -173.43(15) . . . . ? C8 C9 C10 C5 -0.6(2) . . . . ? C6 C5 C10 C9 -2.8(2) . . . . ? C03 C5 C10 C9 175.15(15) . . . . ? C9 C8 C11 C12 68(2) . . . . ? C7 C8 C11 C12 -108(2) . . . . ? C8 C11 C12 C13 -145(18) . . . . ? C11 C12 C13 C14 -94(19) . . . . ? C11 C12 C13 C18 87(19) . . . . ? C18 C13 C14 C15 -0.9(2) . . . . ? C12 C13 C14 C15 179.64(15) . . . . ? C13 C14 C15 C16 0.6(3) . . . . ? C14 C15 C16 C17 -0.1(2) . . . . ? C14 C15 C16 C19 179.01(14) . . . . ? C15 C16 C17 C18 0.1(2) . . . . ? C19 C16 C17 C18 -179.06(14) . . . . ? C16 C17 C18 C13 -0.4(2) . . . . ? C14 C13 C18 C17 0.8(2) . . . . ? C12 C13 C18 C17 -179.71(14) . . . . ? C17 C16 C19 O1 176.92(15) . . . . ? C15 C16 C19 O1 -2.2(2) . . . . ? C17 C16 C19 O2 -3.2(2) . . . . ? C15 C16 C19 O2 177.69(14) . . . . ? C5 C6 C01 C2 -111.23(19) . . . . ? C7 C6 C01 C2 68.0(2) . . . . ? C5 C6 C01 C1 125.79(18) . . . . ? C7 C6 C01 C1 -54.9(3) . . . . ? C5 C6 C01 C02 10.9(2) . . . . ? C7 C6 C01 C02 -169.78(17) . . . . ? C2 C01 C02 C03 97.6(2) . . . . ? C6 C01 C02 C03 -21.9(2) . . . . ? C1 C01 C02 C03 -139.41(17) . . . . ? C6 C5 C03 C4 104.50(18) . . . . ? C10 C5 C03 C4 -73.6(2) . . . . ? C6 C5 C03 C3 -134.67(17) . . . . ? C10 C5 C03 C3 47.2(2) . . . . ? C6 C5 C03 C02 -17.78(19) . . . . ? C10 C5 C03 C02 164.10(18) . . . . ? C01 C02 C03 C5 24.2(2) . . . . ? C01 C02 C03 C4 -94.4(2) . . . . ? C01 C02 C03 C3 143.11(17) . . . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 29.17 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.368 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.056 data_glu17abs _database_code_depnum_ccdc_archive 'CCDC 837994' #TrackingRef 'analogues_of_ec23.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H22 O2 Si2' _chemical_formula_sum 'C20 H22 O2 Si2' _chemical_formula_weight 350.56 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.7328(10) _cell_length_b 11.2756(8) _cell_length_c 35.715(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3919.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3000 _cell_measurement_theta_min 7.35 _cell_measurement_theta_max 25.3 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max .5 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.190 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9187 _exptl_absorpt_correction_T_max 0.9878 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate_Stoe-IPDs _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19094 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 26.92 _reflns_number_total 3971 _reflns_number_gt 2736 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. TITL glu17c in Pbca CELL 0.71073 9.7328 11.2756 35.7155 90.000 90.000 90.000 ZERR 8.00 0.0010 0.0008 0.0038 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H O Si UNIT 160 176 16 16 L.S. 8 ACTA BOND FMAP 2 PLAN 20 HTAB 2.5 CONF TEMP -100 WGHT 0.066500 0.220000 FVAR 0.53061 0.47695 MOLE 1 C2 1 0.677755 0.438191 0.189277 11.00000 0.06070 0.05229 = 0.07690 0.00898 0.02195 -0.00693 AFIX 137 H2A 2 0.637306 0.399849 0.211297 11.00000 -1.50000 H2B 2 0.662800 0.388302 0.167181 11.00000 -1.50000 H2C 2 0.634313 0.515628 0.185392 11.00000 -1.50000 AFIX 0 C1 1 0.893697 0.569795 0.234648 11.00000 0.11312 0.04463 = 0.03932 -0.00186 0.00506 0.00100 AFIX 137 H1A 2 0.854840 0.646300 0.227071 11.00000 -1.50000 H1B 2 0.992529 0.578687 0.239080 11.00000 -1.50000 H1C 2 0.848846 0.542803 0.257689 11.00000 -1.50000 AFIX 0 C4 1 1.080619 0.162126 0.140768 11.00000 0.09700 0.03259 = 0.04906 0.00037 0.00125 0.00660 AFIX 137 H4A 2 1.142490 0.166556 0.119166 11.00000 -1.50000 H4B 2 0.986042 0.150929 0.132041 11.00000 -1.50000 H4C 2 1.107229 0.095140 0.156676 11.00000 -1.50000 AFIX 0 C3 1 1.268700 0.314609 0.187095 11.00000 0.06573 0.07048 = 0.08943 0.02751 -0.03256 -0.01226 AFIX 137 H3A 2 1.289125 0.245396 0.202730 11.00000 -1.50000 H3B 2 1.275583 0.386835 0.202243 11.00000 -1.50000 H3C 2 1.334672 0.318600 0.166405 11.00000 -1.50000 AFIX 0 C5 1 1.052716 0.434752 0.138019 11.00000 0.03579 0.02410 = 0.03388 0.00244 0.00078 0.00089 C6 1 0.950159 0.511364 0.152492 11.00000 0.03607 0.02235 = 0.03246 0.00194 0.00136 -0.00025 C7 1 0.923491 0.618745 0.134356 11.00000 0.03503 0.02384 = 0.03576 0.00246 0.00281 0.00146 AFIX 43 H7 2 0.854350 0.669863 0.143951 11.00000 -1.20000 AFIX 0 C8 1 0.996637 0.652495 0.102326 11.00000 0.03018 0.02577 = 0.03415 0.00471 -0.00338 -0.00208 C9 1 1.093572 0.573795 0.087387 11.00000 0.04058 0.03614 = 0.03615 0.00968 0.00785 0.00241 AFIX 43 H9 2 1.140877 0.593676 0.064983 11.00000 -1.20000 AFIX 0 C10 1 1.120754 0.467146 0.105130 11.00000 0.04268 0.03425 = 0.04111 0.00716 0.01013 0.00875 AFIX 43 H10 2 1.187093 0.414888 0.094713 11.00000 -1.20000 AFIX 0 C11 1 0.979152 0.767523 0.085974 11.00000 0.03111 0.02921 = 0.03481 0.00362 -0.00150 -0.00317 C12 1 0.971520 0.866078 0.073216 11.00000 0.03092 0.02876 = 0.03220 0.00282 -0.00178 -0.00298 C13 1 0.972303 0.984216 0.058867 11.00000 0.03108 0.02416 = 0.02684 0.00209 -0.00395 -0.00243 C14 1 0.860327 1.060804 0.063847 11.00000 0.02872 0.02861 = 0.03655 0.00441 0.00297 -0.00316 AFIX 43 H14 2 0.780246 1.033342 0.076341 11.00000 -1.20000 AFIX 0 C15 1 0.865629 1.175634 0.050743 11.00000 0.02556 0.02973 = 0.03889 0.00349 0.00067 0.00205 AFIX 43 H15 2 0.789026 1.226727 0.054144 11.00000 -1.20000 AFIX 0 C16 1 0.983063 1.217399 0.032473 11.00000 0.02508 0.02348 = 0.03265 0.00290 -0.00432 -0.00056 C17 1 1.093615 1.140783 0.026831 11.00000 0.02494 0.02655 = 0.03197 0.00405 -0.00081 -0.00025 AFIX 43 H17 2 1.173147 1.168172 0.014063 11.00000 -1.20000 AFIX 0 C18 1 1.088276 1.025924 0.039617 11.00000 0.02648 0.02742 = 0.03066 0.00228 -0.00245 0.00292 AFIX 43 H18 2 1.163822 0.974289 0.035380 11.00000 -1.20000 AFIX 0 C19 1 0.989732 1.340298 0.018598 11.00000 0.02651 0.02507 = 0.03367 0.00284 -0.00179 -0.00184 C03 1 0.956255 0.315080 0.205046 11.00000 0.07638 0.03722 = 0.05081 0.01450 0.01988 0.01499 AFIX 23 H31 2 0.890946 0.247976 0.203373 11.00000 -1.20000 H32 2 0.998652 0.314570 0.230242 11.00000 -1.20000 AFIX 0 O1 3 0.884437 1.405531 0.020244 11.00000 0.02852 0.02547 = 0.06636 0.00903 -0.00336 0.00247 AFIX 147 H2O1 2 0.903073 1.472790 0.011499 21.00000 -1.50000 AFIX 0 O2 3 1.104522 1.376762 0.005235 11.00000 0.03226 0.02783 = 0.05308 0.00965 0.00465 -0.00269 AFIX 147 REM H2 2 1.143689 1.322479 -0.006111 11.00000 -1.50000 H2O2 2 1.098634 1.449315 0.000144 -21.00000 -1.50000 AFIX 0 SI1 4 0.864910 0.458629 0.196776 11.00000 0.05231 0.02412 = 0.03298 0.00330 0.01150 0.00339 SI2 4 1.092123 0.301351 0.167991 11.00000 0.04036 0.02437 = 0.03280 0.00347 -0.00233 0.00358 HKLF 4 REM glu17c in Pbca REM R1 = 0.0402 for 2736 Fo > 4sig(Fo) and 0.0639 for all 3971 data REM 224 parameters refined using 0 restraints END WGHT 0.0665 0.2137 REM Highest difference peak 0.232, deepest hole -0.284, 1-sigma level 0.046 Q1 1 1.0796 0.3633 0.1417 11.00000 0.05 0.23 Q2 1 0.9147 0.4929 0.1679 11.00000 0.05 0.23 Q3 1 0.9784 0.4660 0.1413 11.00000 0.05 0.21 Q4 1 1.0176 1.1726 0.0229 11.00000 0.05 0.20 Q5 1 0.9288 0.3805 0.2058 11.00000 0.05 0.19 Q6 1 0.8689 0.5461 0.2132 11.00000 0.05 0.19 Q7 1 1.1289 0.9602 0.0257 11.00000 0.05 0.19 Q8 1 0.9011 0.3553 0.1947 11.00000 0.05 0.18 Q9 1 1.1151 0.2079 0.1632 11.00000 0.05 0.18 Q10 1 0.9158 1.1932 0.0394 11.00000 0.05 0.18 Q11 1 1.0918 0.4609 0.1330 11.00000 0.05 0.17 Q12 1 0.9475 1.0401 0.0700 11.00000 0.05 0.17 Q13 1 1.1675 0.6458 0.0704 11.00000 0.05 0.17 Q14 1 0.9468 0.5196 0.1795 11.00000 0.05 0.17 Q15 1 1.0168 1.0056 0.0504 11.00000 0.05 0.17 Q16 1 0.9570 0.2439 0.2208 11.00000 0.05 0.17 Q17 1 0.9516 0.5695 0.1485 11.00000 0.05 0.16 Q18 1 0.9538 0.5257 0.2124 11.00000 0.05 0.16 Q19 1 0.9295 0.9997 0.0517 11.00000 0.05 0.15 Q20 1 0.9176 1.0215 0.0572 11.00000 0.05 0.15 ; _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^)+(0.0665P)^2^+0.2200P] 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 3971 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 C2 C 0.6778(2) 0.4382(2) 0.18928(9) 0.0633(7) Uani 1 1 d . . . H2A H 0.6373 0.3998 0.2113 0.095 Uiso 1 1 calc R . . H2B H 0.6628 0.3883 0.1672 0.095 Uiso 1 1 calc R . . H2C H 0.6343 0.5156 0.1854 0.095 Uiso 1 1 calc R . . C1 C 0.8937(3) 0.5698(2) 0.23465(8) 0.0657(7) Uani 1 1 d . . . H1A H 0.8548 0.6463 0.2271 0.099 Uiso 1 1 calc R . . H1B H 0.9925 0.5787 0.2391 0.099 Uiso 1 1 calc R . . H1C H 0.8488 0.5428 0.2577 0.099 Uiso 1 1 calc R . . C4 C 1.0806(3) 0.1621(2) 0.14077(8) 0.0595(6) Uani 1 1 d . . . H4A H 1.1425 0.1666 0.1192 0.089 Uiso 1 1 calc R . . H4B H 0.9860 0.1509 0.1320 0.089 Uiso 1 1 calc R . . H4C H 1.1072 0.0951 0.1567 0.089 Uiso 1 1 calc R . . C3 C 1.2687(3) 0.3146(3) 0.18710(10) 0.0752(9) Uani 1 1 d . . . H3A H 1.2891 0.2454 0.2027 0.113 Uiso 1 1 calc R . . H3B H 1.2756 0.3868 0.2022 0.113 Uiso 1 1 calc R . . H3C H 1.3347 0.3186 0.1664 0.113 Uiso 1 1 calc R . . C5 C 1.05272(17) 0.43475(17) 0.13802(6) 0.0313(4) Uani 1 1 d . . . C6 C 0.95016(17) 0.51136(16) 0.15249(5) 0.0303(4) Uani 1 1 d . . . C7 C 0.92349(17) 0.61875(17) 0.13436(6) 0.0315(4) Uani 1 1 d . . . H7 H 0.8543 0.6699 0.1440 0.038 Uiso 1 1 calc R . . C8 C 0.99664(16) 0.65249(17) 0.10233(5) 0.0300(4) Uani 1 1 d . . . C9 C 1.09357(18) 0.57380(19) 0.08739(6) 0.0376(5) Uani 1 1 d . . . H9 H 1.1409 0.5937 0.0650 0.045 Uiso 1 1 calc R . . C10 C 1.12075(18) 0.46715(19) 0.10513(6) 0.0393(5) Uani 1 1 d . . . H10 H 1.1871 0.4149 0.0947 0.047 Uiso 1 1 calc R . . C11 C 0.97915(17) 0.76752(17) 0.08597(6) 0.0317(4) Uani 1 1 d . . . C12 C 0.97152(16) 0.86608(17) 0.07322(5) 0.0306(4) Uani 1 1 d . . . C13 C 0.97230(16) 0.98422(16) 0.05887(5) 0.0274(4) Uani 1 1 d . . . C14 C 0.86033(16) 1.06080(17) 0.06385(6) 0.0313(4) Uani 1 1 d . . . H14 H 0.7802 1.0333 0.0763 0.038 Uiso 1 1 calc R . . C15 C 0.86563(16) 1.17563(17) 0.05074(6) 0.0314(4) Uani 1 1 d . . . H15 H 0.7890 1.2267 0.0541 0.038 Uiso 1 1 calc R . . C16 C 0.98306(15) 1.21740(15) 0.03247(5) 0.0271(4) Uani 1 1 d . . . C17 C 1.09361(15) 1.14078(16) 0.02683(5) 0.0278(4) Uani 1 1 d . . . H17 H 1.1731 1.1682 0.0141 0.033 Uiso 1 1 calc R . . C18 C 1.08828(16) 1.02592(16) 0.03962(5) 0.0282(4) Uani 1 1 d . . . H18 H 1.1638 0.9743 0.0354 0.034 Uiso 1 1 calc R . . C19 C 0.98973(15) 1.34030(16) 0.01860(5) 0.0284(4) Uani 1 1 d . . . C03 C 0.9563(3) 0.3151(2) 0.20505(7) 0.0548(6) Uani 1 1 d . . . H31 H 0.8909 0.2480 0.2034 0.066 Uiso 1 1 calc R . . H32 H 0.9987 0.3146 0.2302 0.066 Uiso 1 1 calc R . . O1 O 0.88444(11) 1.40553(13) 0.02024(5) 0.0401(4) Uani 1 1 d . . . H2O1 H 0.9031 1.4728 0.0115 0.060 Uiso 0.48(4) 1 calc PR . . O2 O 1.10452(12) 1.37676(13) 0.00524(4) 0.0377(3) Uani 1 1 d . . . H2O2 H 1.0986 1.4493 0.0001 0.057 Uiso 0.52(4) 1 calc PR . . Si1 Si 0.86491(6) 0.45863(5) 0.196776(17) 0.03647(16) Uani 1 1 d . . . Si2 Si 1.09212(5) 0.30135(5) 0.167991(16) 0.03251(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2 0.0607(14) 0.0523(17) 0.077(2) 0.0090(14) 0.0220(12) -0.0069(11) C1 0.113(2) 0.0446(16) 0.0393(16) -0.0019(11) 0.0051(13) 0.0010(13) C4 0.0970(18) 0.0326(14) 0.0491(16) 0.0004(11) 0.0012(12) 0.0066(12) C3 0.0657(15) 0.070(2) 0.089(2) 0.0275(17) -0.0326(15) -0.0123(13) C5 0.0358(9) 0.0241(11) 0.0339(11) 0.0024(8) 0.0008(7) 0.0009(7) C6 0.0361(8) 0.0224(10) 0.0325(10) 0.0019(8) 0.0014(7) -0.0003(7) C7 0.0350(8) 0.0238(11) 0.0358(11) 0.0025(8) 0.0028(7) 0.0015(7) C8 0.0302(8) 0.0258(10) 0.0342(10) 0.0047(8) -0.0034(7) -0.0021(7) C9 0.0406(9) 0.0361(12) 0.0361(12) 0.0097(9) 0.0078(8) 0.0024(8) C10 0.0427(10) 0.0342(12) 0.0411(12) 0.0072(9) 0.0101(8) 0.0088(8) C11 0.0311(8) 0.0292(11) 0.0348(11) 0.0036(8) -0.0015(7) -0.0032(7) C12 0.0309(8) 0.0288(11) 0.0322(10) 0.0028(8) -0.0018(7) -0.0030(7) C13 0.0311(8) 0.0242(10) 0.0268(10) 0.0021(7) -0.0039(6) -0.0024(6) C14 0.0287(8) 0.0286(11) 0.0365(11) 0.0044(8) 0.0030(7) -0.0032(7) C15 0.0256(8) 0.0297(11) 0.0389(11) 0.0035(8) 0.0007(7) 0.0021(7) C16 0.0251(7) 0.0235(10) 0.0327(10) 0.0029(7) -0.0043(6) -0.0006(6) C17 0.0249(7) 0.0266(10) 0.0320(10) 0.0040(8) -0.0008(6) -0.0003(6) C18 0.0265(7) 0.0274(10) 0.0307(10) 0.0023(7) -0.0024(6) 0.0029(6) C19 0.0265(8) 0.0251(10) 0.0337(10) 0.0028(7) -0.0018(6) -0.0018(6) C03 0.0764(15) 0.0372(14) 0.0508(15) 0.0145(11) 0.0199(11) 0.0150(11) O1 0.0285(6) 0.0255(8) 0.0664(11) 0.0090(7) -0.0034(6) 0.0025(5) O2 0.0323(6) 0.0278(8) 0.0531(10) 0.0096(6) 0.0047(5) -0.0027(5) Si1 0.0523(3) 0.0241(3) 0.0330(3) 0.0033(2) 0.0115(2) 0.0034(2) Si2 0.0404(3) 0.0244(3) 0.0328(3) 0.0035(2) -0.0023(2) 0.00358(19) _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 C2 Si1 1.855(2) . ? C1 Si1 1.865(3) . ? C4 Si2 1.850(3) . ? C3 Si2 1.855(2) . ? C5 C10 1.397(3) . ? C5 C6 1.418(3) . ? C5 Si2 1.8856(19) . ? C6 C7 1.397(3) . ? C6 Si1 1.8824(19) . ? C7 C8 1.400(3) . ? C8 C9 1.401(3) . ? C8 C11 1.433(3) . ? C9 C10 1.385(3) . ? C11 C12 1.203(3) . ? C12 C13 1.427(3) . ? C13 C14 1.402(2) . ? C13 C18 1.403(2) . ? C14 C15 1.378(3) . ? C15 C16 1.398(2) . ? C16 C17 1.395(2) . ? C16 C19 1.473(3) . ? C17 C18 1.374(3) . ? C19 O1 1.263(2) . ? C19 O2 1.283(2) . ? C03 Si1 1.870(2) . ? C03 Si2 1.877(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 C5 C6 118.75(17) . . ? C10 C5 Si2 126.12(14) . . ? C6 C5 Si2 114.98(14) . . ? C7 C6 C5 119.32(17) . . ? C7 C6 Si1 125.54(14) . . ? C5 C6 Si1 115.10(14) . . ? C6 C7 C8 121.32(17) . . ? C7 C8 C9 118.78(17) . . ? C7 C8 C11 121.25(17) . . ? C9 C8 C11 119.89(17) . . ? C10 C9 C8 120.30(18) . . ? C9 C10 C5 121.42(18) . . ? C12 C11 C8 176.19(18) . . ? C11 C12 C13 175.96(17) . . ? C14 C13 C18 118.76(16) . . ? C14 C13 C12 121.69(15) . . ? C18 C13 C12 119.55(16) . . ? C15 C14 C13 120.45(16) . . ? C14 C15 C16 120.39(16) . . ? C17 C16 C15 119.32(16) . . ? C17 C16 C19 120.01(15) . . ? C15 C16 C19 120.66(15) . . ? C18 C17 C16 120.44(15) . . ? C17 C18 C13 120.61(16) . . ? O1 C19 O2 122.51(17) . . ? O1 C19 C16 119.77(15) . . ? O2 C19 C16 117.72(15) . . ? Si1 C03 Si2 107.15(11) . . ? C2 Si1 C1 109.61(13) . . ? C2 Si1 C03 112.46(12) . . ? C1 Si1 C03 113.31(13) . . ? C2 Si1 C6 110.53(11) . . ? C1 Si1 C6 109.32(11) . . ? C03 Si1 C6 101.34(9) . . ? C4 Si2 C3 108.53(14) . . ? C4 Si2 C03 113.44(12) . . ? C3 Si2 C03 112.75(15) . . ? C4 Si2 C5 111.48(11) . . ? C3 Si2 C5 109.45(11) . . ? C03 Si2 C5 101.02(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 C10 C5 C6 C7 -2.3(3) . . . . ? Si2 C5 C6 C7 173.50(14) . . . . ? C10 C5 C6 Si1 179.79(15) . . . . ? Si2 C5 C6 Si1 -4.37(19) . . . . ? C5 C6 C7 C8 -0.4(3) . . . . ? Si1 C6 C7 C8 177.22(14) . . . . ? C6 C7 C8 C9 3.1(3) . . . . ? C6 C7 C8 C11 -173.59(17) . . . . ? C7 C8 C9 C10 -3.0(3) . . . . ? C11 C8 C9 C10 173.70(18) . . . . ? C8 C9 C10 C5 0.3(3) . . . . ? C6 C5 C10 C9 2.4(3) . . . . ? Si2 C5 C10 C9 -172.91(16) . . . . ? C7 C8 C11 C12 102(3) . . . . ? C9 C8 C11 C12 -75(3) . . . . ? C8 C11 C12 C13 12(6) . . . . ? C11 C12 C13 C14 -138(3) . . . . ? C11 C12 C13 C18 41(3) . . . . ? C18 C13 C14 C15 -1.4(3) . . . . ? C12 C13 C14 C15 177.91(18) . . . . ? C13 C14 C15 C16 -0.3(3) . . . . ? C14 C15 C16 C17 1.5(3) . . . . ? C14 C15 C16 C19 -179.62(18) . . . . ? C15 C16 C17 C18 -1.1(3) . . . . ? C19 C16 C17 C18 -179.90(17) . . . . ? C16 C17 C18 C13 -0.7(3) . . . . ? C14 C13 C18 C17 1.9(3) . . . . ? C12 C13 C18 C17 -177.43(17) . . . . ? C17 C16 C19 O1 172.59(17) . . . . ? C15 C16 C19 O1 -6.2(3) . . . . ? C17 C16 C19 O2 -7.6(3) . . . . ? C15 C16 C19 O2 173.61(18) . . . . ? Si2 C03 Si1 C2 121.92(15) . . . . ? Si2 C03 Si1 C1 -113.09(16) . . . . ? Si2 C03 Si1 C6 3.89(16) . . . . ? C7 C6 Si1 C2 63.0(2) . . . . ? C5 C6 Si1 C2 -119.23(16) . . . . ? C7 C6 Si1 C1 -57.7(2) . . . . ? C5 C6 Si1 C1 120.04(17) . . . . ? C7 C6 Si1 C03 -177.55(18) . . . . ? C5 C6 Si1 C03 0.18(18) . . . . ? Si1 C03 Si2 C4 -125.20(15) . . . . ? Si1 C03 Si2 C3 110.93(16) . . . . ? Si1 C03 Si2 C5 -5.78(16) . . . . ? C10 C5 Si2 C4 -57.2(2) . . . . ? C6 C5 Si2 C4 127.33(16) . . . . ? C10 C5 Si2 C3 62.9(2) . . . . ? C6 C5 Si2 C3 -112.60(19) . . . . ? C10 C5 Si2 C03 -178.01(19) . . . . ? C6 C5 Si2 C03 6.51(18) . . . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 26.92 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 0.232 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.046 data_glu11k _database_code_depnum_ccdc_archive 'CCDC 837995' #TrackingRef 'analogues_of_ec23.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H24 O2' _chemical_formula_sum 'C23 H24 O2' _chemical_formula_weight 332.42 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 20.5765(9) _cell_length_b 11.1441(5) _cell_length_c 8.1245(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.9270(10) _cell_angle_gamma 90.00 _cell_volume 1840.43(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9862 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 33.18 _exptl_crystal_description flat_plate _exptl_crystal_colour colorless _exptl_crystal_size_max .30 _exptl_crystal_size_mid .22 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min .6280 _exptl_absorpt_correction_T_max .7465 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source rotating_anode _diffrn_radiation_monochromator MONTEL_multi_layer_optics _diffrn_measurement_device_type Bruker-Kappa_Apex2_CCD _diffrn_measurement_method omega_and_phi_scans _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 38468 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 33.14 _reflns_number_total 6772 _reflns_number_gt 5507 _reflns_threshold_expression >2sigma(I) _computing_data_collection Bruker-SAINT _computing_cell_refinement Bruker-SAINT' _computing_data_reduction Bruker-SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. TITL glu11c in P2(1)/c CELL 0.71073 20.5765 11.1441 8.1245 90.000 98.927 90.000 ZERR 4.00 0.0009 0.0005 0.0004 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O UNIT 92 96 8 L.S. 12 ACTA BOND $H FMAP 2 PLAN 20 CONF TEMP -172.970 WGHT 0.056500 0.535600 FVAR 0.14479 MOLE 1 C1 1 0.624202 -0.060377 0.475943 11.00000 0.02790 0.02081 = 0.01590 -0.00380 0.00175 -0.00220 AFIX 137 H1A 2 0.611973 0.019391 0.430616 11.00000 -1.50000 H1B 2 0.588854 -0.117397 0.437332 11.00000 -1.50000 H1C 2 0.664847 -0.086551 0.437881 11.00000 -1.50000 AFIX 0 C2 1 0.656442 -0.179387 0.736399 11.00000 0.02486 0.01384 = 0.02737 0.00274 0.00312 -0.00189 AFIX 137 H2A 2 0.697899 -0.201996 0.699494 11.00000 -1.50000 H2B 2 0.622447 -0.238444 0.695592 11.00000 -1.50000 H2C 2 0.662636 -0.177138 0.858416 11.00000 -1.50000 AFIX 0 C3 1 0.545863 0.196672 0.848533 11.00000 0.02037 0.01968 = 0.02241 0.00156 0.00584 0.00287 AFIX 137 H3A 2 0.562159 0.258101 0.931015 11.00000 -1.50000 H3B 2 0.502160 0.169980 0.866758 11.00000 -1.50000 H3C 2 0.543015 0.230401 0.736244 11.00000 -1.50000 AFIX 0 C4 1 0.598860 0.039488 1.044868 11.00000 0.02161 0.02306 = 0.01765 0.00413 0.00574 -0.00102 AFIX 137 H4A 2 0.625724 -0.033528 1.054225 11.00000 -1.50000 H4B 2 0.554872 0.020578 1.069591 11.00000 -1.50000 H4C 2 0.619584 0.099539 1.124262 11.00000 -1.50000 AFIX 0 C5 1 0.661483 0.122687 0.833777 11.00000 0.01683 0.01401 = 0.01241 0.00014 0.00298 -0.00083 C6 1 0.686039 0.039482 0.730827 11.00000 0.01694 0.01211 = 0.01261 0.00058 0.00267 -0.00078 C7 1 0.750430 0.047955 0.698576 11.00000 0.01737 0.01528 = 0.01461 0.00069 0.00421 -0.00001 AFIX 43 H7 2 0.767544 -0.010480 0.631715 11.00000 -1.20000 AFIX 0 C8 1 0.789560 0.144314 0.766585 11.00000 0.01701 0.01794 = 0.01449 0.00186 0.00294 -0.00158 C9 1 0.763896 0.229624 0.866817 11.00000 0.01972 0.01763 = 0.01692 -0.00136 0.00282 -0.00470 AFIX 43 H9 2 0.790285 0.295639 0.910564 11.00000 -1.20000 AFIX 0 C10 1 0.700260 0.218141 0.902375 11.00000 0.02074 0.01566 = 0.01646 -0.00299 0.00446 -0.00194 AFIX 43 H10 2 0.683429 0.274638 0.972532 11.00000 -1.20000 AFIX 0 C11 1 0.855036 0.161101 0.731217 11.00000 0.01877 0.02028 = 0.01738 0.00144 0.00256 -0.00245 C12 1 0.908885 0.183867 0.698329 11.00000 0.01928 0.02109 = 0.01822 0.00042 0.00273 -0.00290 C13 1 0.971254 0.214840 0.652320 11.00000 0.01652 0.01924 = 0.01600 -0.00006 0.00240 -0.00291 C14 1 1.015601 0.125575 0.621426 11.00000 0.02050 0.01705 = 0.02326 0.00211 0.00468 -0.00233 AFIX 43 H14 2 1.005477 0.043610 0.637214 11.00000 -1.20000 AFIX 0 C15 1 1.074386 0.156023 0.567773 11.00000 0.01911 0.01852 = 0.02278 0.00120 0.00506 0.00048 AFIX 43 H15 2 1.103881 0.094826 0.545006 11.00000 -1.20000 AFIX 0 C16 1 1.090111 0.276026 0.547347 11.00000 0.01569 0.01945 = 0.01631 0.00002 0.00217 -0.00168 C17 1 1.046961 0.365818 0.583089 11.00000 0.01951 0.01640 = 0.02528 -0.00081 0.00594 -0.00302 AFIX 43 H17 2 1.058196 0.447844 0.572558 11.00000 -1.20000 AFIX 0 C18 1 0.987708 0.335404 0.633953 11.00000 0.01916 0.01833 = 0.02502 -0.00159 0.00676 -0.00073 AFIX 43 H18 2 0.958221 0.396717 0.656374 11.00000 -1.20000 AFIX 0 C19 1 1.152140 0.304181 0.481733 11.00000 0.01681 0.02314 = 0.01794 -0.00062 0.00245 -0.00313 C20 1 1.212141 0.453762 0.365575 11.00000 0.02528 0.03413 = 0.02551 -0.00058 0.00880 -0.01225 AFIX 137 H20A 2 1.251844 0.439794 0.446869 11.00000 -1.50000 H20B 2 1.209306 0.538962 0.335443 11.00000 -1.50000 H20C 2 1.214141 0.405498 0.265652 11.00000 -1.50000 AFIX 0 C01 1 0.635060 -0.055013 0.667011 11.00000 0.01729 0.01300 = 0.01531 -0.00124 0.00298 -0.00144 C02 1 0.593204 0.089548 0.866655 11.00000 0.01679 0.01517 = 0.01471 -0.00070 0.00418 -0.00084 C03 1 0.572311 -0.007779 0.731636 11.00000 0.01656 0.02093 = 0.02192 -0.00606 0.00375 -0.00281 AFIX 23 H22A 2 0.541421 0.027048 0.638297 11.00000 -1.20000 H22B 2 0.549829 -0.074706 0.779868 11.00000 -1.20000 AFIX 0 O1 3 1.194587 0.231463 0.467193 11.00000 0.02102 0.03070 = 0.03546 0.00255 0.01061 0.00270 O2 3 1.154813 0.419886 0.437490 11.00000 0.02125 0.02315 = 0.02505 -0.00010 0.00725 -0.00688 HKLF 4 REM glu11c in P2(1)/c REM R1 = 0.0422 for 5507 Fo > 4sig(Fo) and 0.0553 for all 6772 data REM 231 parameters refined using 0 restraints END WGHT 0.0565 0.5357 REM Highest difference peak 0.558, deepest hole -0.184, 1-sigma level 0.051 Q1 1 0.7307 0.2241 0.8815 11.00000 0.05 0.56 Q2 1 0.7190 0.0412 0.7180 11.00000 0.05 0.55 Q3 1 0.6759 0.0815 0.7876 11.00000 0.05 0.51 Q4 1 1.0191 0.3455 0.6161 11.00000 0.05 0.49 Q5 1 1.0463 0.1401 0.6018 11.00000 0.05 0.48 Q6 1 1.0818 0.2187 0.5659 11.00000 0.05 0.45 Q7 1 0.9785 0.2729 0.6444 11.00000 0.05 0.45 Q8 1 1.1209 0.2893 0.5180 11.00000 0.05 0.44 Q9 1 0.7760 0.1863 0.8147 11.00000 0.05 0.42 Q10 1 0.6291 0.1050 0.8594 11.00000 0.05 0.41 Q11 1 0.9414 0.2040 0.6681 11.00000 0.05 0.40 Q12 1 0.6852 0.1582 0.8768 11.00000 0.05 0.40 Q13 1 1.0722 0.3164 0.5718 11.00000 0.05 0.39 Q14 1 0.6436 -0.1206 0.6960 11.00000 0.05 0.39 Q15 1 0.6019 -0.0354 0.6939 11.00000 0.05 0.38 Q16 1 0.8182 0.1537 0.7428 11.00000 0.05 0.38 Q17 1 0.5825 0.0415 0.8032 11.00000 0.05 0.37 Q18 1 0.9886 0.1724 0.6295 11.00000 0.05 0.37 Q19 1 0.7710 0.0914 0.7358 11.00000 0.05 0.35 Q20 1 0.6663 -0.0198 0.7108 11.00000 0.05 0.34 ; _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^)+(0.0565P)^2^+0.5356P] 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 6772 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1216 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 C1 C 0.62420(5) -0.06038(9) 0.47594(11) 0.02171(17) Uani 1 1 d . . . H1A H 0.6120 0.0194 0.4306 0.033 Uiso 1 1 calc R . . H1B H 0.5889 -0.1174 0.4373 0.033 Uiso 1 1 calc R . . H1C H 0.6648 -0.0866 0.4379 0.033 Uiso 1 1 calc R . . C2 C 0.65644(5) -0.17939(8) 0.73640(12) 0.02212(17) Uani 1 1 d . . . H2A H 0.6979 -0.2020 0.6995 0.033 Uiso 1 1 calc R . . H2B H 0.6224 -0.2384 0.6956 0.033 Uiso 1 1 calc R . . H2C H 0.6626 -0.1771 0.8584 0.033 Uiso 1 1 calc R . . C3 C 0.54586(5) 0.19667(8) 0.84853(11) 0.02055(17) Uani 1 1 d . . . H3A H 0.5622 0.2581 0.9310 0.031 Uiso 1 1 calc R . . H3B H 0.5022 0.1700 0.8668 0.031 Uiso 1 1 calc R . . H3C H 0.5430 0.2304 0.7362 0.031 Uiso 1 1 calc R . . C4 C 0.59886(5) 0.03949(9) 1.04487(11) 0.02049(17) Uani 1 1 d . . . H4A H 0.6257 -0.0335 1.0542 0.031 Uiso 1 1 calc R . . H4B H 0.5549 0.0206 1.0696 0.031 Uiso 1 1 calc R . . H4C H 0.6196 0.0995 1.1243 0.031 Uiso 1 1 calc R . . C5 C 0.66148(4) 0.12269(7) 0.83378(10) 0.01434(14) Uani 1 1 d . . . C6 C 0.68604(4) 0.03948(7) 0.73083(9) 0.01385(14) Uani 1 1 d . . . C7 C 0.75043(4) 0.04795(8) 0.69858(10) 0.01557(15) Uani 1 1 d . . . H7 H 0.7675 -0.0105 0.6317 0.019 Uiso 1 1 calc R . . C8 C 0.78956(4) 0.14431(8) 0.76659(10) 0.01643(15) Uani 1 1 d . . . C9 C 0.76390(4) 0.22962(8) 0.86682(11) 0.01809(16) Uani 1 1 d . . . H9 H 0.7903 0.2956 0.9106 0.022 Uiso 1 1 calc R . . C10 C 0.70026(4) 0.21814(8) 0.90238(10) 0.01745(16) Uani 1 1 d . . . H10 H 0.6834 0.2746 0.9725 0.021 Uiso 1 1 calc R . . C11 C 0.85504(4) 0.16110(8) 0.73122(11) 0.01884(16) Uani 1 1 d . . . C12 C 0.90889(4) 0.18387(8) 0.69833(11) 0.01955(16) Uani 1 1 d . . . C13 C 0.97125(4) 0.21484(8) 0.65232(10) 0.01727(16) Uani 1 1 d . . . C14 C 1.01560(4) 0.12558(8) 0.62143(11) 0.02013(17) Uani 1 1 d . . . H14 H 1.0055 0.0436 0.6372 0.024 Uiso 1 1 calc R . . C15 C 1.07439(4) 0.15602(9) 0.56777(11) 0.01994(16) Uani 1 1 d . . . H15 H 1.1039 0.0948 0.5450 0.024 Uiso 1 1 calc R . . C16 C 1.09011(4) 0.27603(8) 0.54735(10) 0.01718(15) Uani 1 1 d . . . C17 C 1.04696(4) 0.36582(8) 0.58309(12) 0.02014(17) Uani 1 1 d . . . H17 H 1.0582 0.4478 0.5726 0.024 Uiso 1 1 calc R . . C18 C 0.98771(4) 0.33540(8) 0.63395(12) 0.02048(17) Uani 1 1 d . . . H18 H 0.9582 0.3967 0.6564 0.025 Uiso 1 1 calc R . . C19 C 1.15214(4) 0.30418(9) 0.48173(11) 0.01932(16) Uani 1 1 d . . . C20 C 1.21214(5) 0.45376(10) 0.36557(13) 0.0278(2) Uani 1 1 d . . . H20A H 1.2518 0.4398 0.4469 0.042 Uiso 1 1 calc R . . H20B H 1.2093 0.5390 0.3354 0.042 Uiso 1 1 calc R . . H20C H 1.2141 0.4055 0.2657 0.042 Uiso 1 1 calc R . . C01 C 0.63506(4) -0.05501(7) 0.66701(10) 0.01515(15) Uani 1 1 d . . . C02 C 0.59320(4) 0.08955(8) 0.86666(10) 0.01537(15) Uani 1 1 d . . . C03 C 0.57231(4) -0.00778(8) 0.73164(11) 0.01972(16) Uani 1 1 d . . . H22A H 0.5414 0.0270 0.6383 0.024 Uiso 1 1 calc R . . H22B H 0.5498 -0.0747 0.7799 0.024 Uiso 1 1 calc R . . O1 O 1.19459(4) 0.23146(7) 0.46719(10) 0.02840(16) Uani 1 1 d . . . O2 O 1.15481(3) 0.41989(7) 0.43749(9) 0.02276(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0279(4) 0.0208(4) 0.0159(3) -0.0038(3) 0.0017(3) -0.0022(3) C2 0.0249(4) 0.0138(4) 0.0274(4) 0.0027(3) 0.0031(3) -0.0019(3) C3 0.0204(4) 0.0197(4) 0.0224(4) 0.0016(3) 0.0058(3) 0.0029(3) C4 0.0216(4) 0.0231(4) 0.0177(4) 0.0041(3) 0.0057(3) -0.0010(3) C5 0.0168(3) 0.0140(3) 0.0124(3) 0.0001(3) 0.0030(3) -0.0008(3) C6 0.0169(3) 0.0121(3) 0.0126(3) 0.0006(2) 0.0027(3) -0.0008(3) C7 0.0174(3) 0.0153(4) 0.0146(3) 0.0007(3) 0.0042(3) 0.0000(3) C8 0.0170(3) 0.0179(4) 0.0145(3) 0.0019(3) 0.0029(3) -0.0016(3) C9 0.0197(4) 0.0176(4) 0.0169(3) -0.0014(3) 0.0028(3) -0.0047(3) C10 0.0207(4) 0.0157(4) 0.0165(3) -0.0030(3) 0.0045(3) -0.0019(3) C11 0.0188(4) 0.0203(4) 0.0174(3) 0.0014(3) 0.0026(3) -0.0025(3) C12 0.0193(4) 0.0211(4) 0.0182(4) 0.0004(3) 0.0027(3) -0.0029(3) C13 0.0165(3) 0.0192(4) 0.0160(3) -0.0001(3) 0.0024(3) -0.0029(3) C14 0.0205(4) 0.0170(4) 0.0233(4) 0.0021(3) 0.0047(3) -0.0023(3) C15 0.0191(4) 0.0185(4) 0.0228(4) 0.0012(3) 0.0051(3) 0.0005(3) C16 0.0157(3) 0.0195(4) 0.0163(3) 0.0000(3) 0.0022(3) -0.0017(3) C17 0.0195(4) 0.0164(4) 0.0253(4) -0.0008(3) 0.0059(3) -0.0030(3) C18 0.0192(4) 0.0183(4) 0.0250(4) -0.0016(3) 0.0068(3) -0.0007(3) C19 0.0168(4) 0.0231(4) 0.0179(3) -0.0006(3) 0.0025(3) -0.0031(3) C20 0.0253(4) 0.0341(5) 0.0255(4) -0.0006(4) 0.0088(4) -0.0123(4) C01 0.0173(3) 0.0130(3) 0.0153(3) -0.0012(3) 0.0030(3) -0.0014(3) C02 0.0168(3) 0.0152(4) 0.0147(3) -0.0007(3) 0.0042(3) -0.0008(3) C03 0.0166(3) 0.0209(4) 0.0219(4) -0.0061(3) 0.0037(3) -0.0028(3) O1 0.0210(3) 0.0307(4) 0.0355(4) 0.0025(3) 0.0106(3) 0.0027(3) O2 0.0212(3) 0.0231(3) 0.0251(3) -0.0001(3) 0.0072(2) -0.0069(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 C1 C01 1.5348(12) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C01 1.5348(12) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C02 1.5334(12) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C02 1.5391(12) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C10 1.3931(12) . ? C5 C6 1.3949(11) . ? C5 C02 1.5159(11) . ? C6 C7 1.3931(11) . ? C6 C01 1.5196(11) . ? C7 C8 1.4031(12) . ? C7 H7 0.9500 . ? C8 C9 1.4069(12) . ? C8 C11 1.4328(12) . ? C9 C10 1.3899(12) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.2064(12) . ? C12 C13 1.4334(12) . ? C13 C14 1.3987(13) . ? C13 C18 1.3992(13) . ? C14 C15 1.3899(12) . ? C14 H14 0.9500 . ? C15 C16 1.3919(13) . ? C15 H15 0.9500 . ? C16 C17 1.3979(13) . ? C16 C19 1.4909(12) . ? C17 C18 1.3887(12) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 O1 1.2106(12) . ? C19 O2 1.3420(12) . ? C20 O2 1.4454(11) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C01 C03 1.5589(12) . ? C02 C03 1.5551(12) . ? C03 H22A 0.9900 . ? C03 H22B 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 C01 C1 H1A 109.5 . . ? C01 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C01 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C01 C2 H2A 109.5 . . ? C01 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C01 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C02 C3 H3A 109.5 . . ? C02 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C02 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C02 C4 H4A 109.5 . . ? C02 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C02 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 120.61(8) . . ? C10 C5 C02 127.19(7) . . ? C6 C5 C02 112.06(7) . . ? C7 C6 C5 120.75(7) . . ? C7 C6 C01 127.52(7) . . ? C5 C6 C01 111.72(7) . . ? C6 C7 C8 118.83(8) . . ? C6 C7 H7 120.6 . . ? C8 C7 H7 120.6 . . ? C7 C8 C9 120.07(8) . . ? C7 C8 C11 121.40(8) . . ? C9 C8 C11 118.49(8) . . ? C10 C9 C8 120.56(8) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C5 119.12(8) . . ? C9 C10 H10 120.4 . . ? C5 C10 H10 120.4 . . ? C12 C11 C8 175.16(10) . . ? C11 C12 C13 177.01(10) . . ? C14 C13 C18 119.24(8) . . ? C14 C13 C12 120.73(8) . . ? C18 C13 C12 120.02(8) . . ? C15 C14 C13 120.42(8) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 120.11(8) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 119.74(8) . . ? C15 C16 C19 118.20(8) . . ? C17 C16 C19 122.02(8) . . ? C18 C17 C16 120.16(8) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C13 120.28(8) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? O1 C19 O2 123.84(8) . . ? O1 C19 C16 124.38(9) . . ? O2 C19 C16 111.77(8) . . ? O2 C20 H20A 109.5 . . ? O2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C6 C01 C2 110.92(7) . . ? C6 C01 C1 110.89(7) . . ? C2 C01 C1 108.95(7) . . ? C6 C01 C03 102.42(6) . . ? C2 C01 C03 112.73(7) . . ? C1 C01 C03 110.83(7) . . ? C5 C02 C3 112.69(7) . . ? C5 C02 C4 108.49(7) . . ? C3 C02 C4 109.07(7) . . ? C5 C02 C03 102.00(6) . . ? C3 C02 C03 111.92(7) . . ? C4 C02 C03 112.52(7) . . ? C02 C03 C01 108.68(7) . . ? C02 C03 H22A 110.0 . . ? C01 C03 H22A 110.0 . . ? C02 C03 H22B 110.0 . . ? C01 C03 H22B 110.0 . . ? H22A C03 H22B 108.3 . . ? C19 O2 C20 115.41(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 C10 C5 C6 C7 1.98(12) . . . . ? C02 C5 C6 C7 -173.98(7) . . . . ? C10 C5 C6 C01 -178.70(7) . . . . ? C02 C5 C6 C01 5.34(10) . . . . ? C5 C6 C7 C8 -2.30(12) . . . . ? C01 C6 C7 C8 178.49(8) . . . . ? C6 C7 C8 C9 0.65(12) . . . . ? C6 C7 C8 C11 -176.92(8) . . . . ? C7 C8 C9 C10 1.36(13) . . . . ? C11 C8 C9 C10 179.00(8) . . . . ? C8 C9 C10 C5 -1.71(13) . . . . ? C6 C5 C10 C9 0.06(12) . . . . ? C02 C5 C10 C9 175.35(8) . . . . ? C7 C8 C11 C12 129.0(11) . . . . ? C9 C8 C11 C12 -48.6(11) . . . . ? C8 C11 C12 C13 -36(3) . . . . ? C11 C12 C13 C14 -127.2(19) . . . . ? C11 C12 C13 C18 51(2) . . . . ? C18 C13 C14 C15 -2.11(13) . . . . ? C12 C13 C14 C15 176.36(8) . . . . ? C13 C14 C15 C16 1.20(14) . . . . ? C14 C15 C16 C17 0.84(13) . . . . ? C14 C15 C16 C19 -177.09(8) . . . . ? C15 C16 C17 C18 -1.94(13) . . . . ? C19 C16 C17 C18 175.91(8) . . . . ? C16 C17 C18 C13 1.01(14) . . . . ? C14 C13 C18 C17 1.00(13) . . . . ? C12 C13 C18 C17 -177.48(8) . . . . ? C15 C16 C19 O1 -11.09(13) . . . . ? C17 C16 C19 O1 171.04(9) . . . . ? C15 C16 C19 O2 167.74(8) . . . . ? C17 C16 C19 O2 -10.14(12) . . . . ? C7 C6 C01 C2 64.92(11) . . . . ? C5 C6 C01 C2 -114.35(8) . . . . ? C7 C6 C01 C1 -56.28(11) . . . . ? C5 C6 C01 C1 124.45(8) . . . . ? C7 C6 C01 C03 -174.56(8) . . . . ? C5 C6 C01 C03 6.17(9) . . . . ? C10 C5 C02 C3 49.91(11) . . . . ? C6 C5 C02 C3 -134.46(8) . . . . ? C10 C5 C02 C4 -70.97(11) . . . . ? C6 C5 C02 C4 104.66(8) . . . . ? C10 C5 C02 C03 170.08(8) . . . . ? C6 C5 C02 C03 -14.29(9) . . . . ? C5 C02 C03 C01 17.77(9) . . . . ? C3 C02 C03 C01 138.48(7) . . . . ? C4 C02 C03 C01 -98.28(8) . . . . ? C6 C01 C03 C02 -15.02(9) . . . . ? C2 C01 C03 C02 104.24(8) . . . . ? C1 C01 C03 C02 -133.34(8) . . . . ? O1 C19 O2 C20 1.44(13) . . . . ? C16 C19 O2 C20 -177.40(7) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 33.14 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.558 _refine_diff_density_min -0.184 _refine_diff_density_rms 0.051 data_glu09k _database_code_depnum_ccdc_archive 'CCDC 837996' #TrackingRef 'analogues_of_ec23.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H22 O3 Si2' _chemical_formula_sum 'C20 H22 O3 Si2' _chemical_formula_weight 366.56 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' 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 C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 60.024(5) _cell_length_b 11.4478(8) _cell_length_c 8.7407(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.534(4) _cell_angle_gamma 90.00 _cell_volume 5978.1(7) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9546 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 26.37 _exptl_crystal_description flat_plate _exptl_crystal_colour colorless _exptl_crystal_size_max .47 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 0.193 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min .6117 _exptl_absorpt_correction_T_max .7454 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source rotation_anode _diffrn_radiation_monochromator Montel_multi_layer_optics _diffrn_measurement_device_type Bruker_Kappa_CCD_Apex2 _diffrn_measurement_method omega_and_phi_scans _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39207 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -72 _diffrn_reflns_limit_h_max 74 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 26.37 _reflns_number_total 12031 _reflns_number_gt 10105 _reflns_threshold_expression >2sigma(I) _computing_data_collection Bruker-SAINT _computing_cell_refinement Bruker-SAINT _computing_data_reduction Bruker-SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. TITL glu09g in C2 CELL 0.71073 60.0240 11.4478 8.7407 90.000 95.534 90.000 ZERR 12.00 0.0045 0.0008 0.0006 0.000 0.004 0.000 LATT -7 SYMM -X, Y, -Z SFAC C H O Si UNIT 240 264 36 24 L.S. 8 ACTA LIST 3 BOND FMAP 2 PLAN 20 TWIN -1 0 0 0 -1 0 0 0 -1 CONF HTAB 2.5 TEMP -173.000 WGHT 0.090900 2.787900 BASF 0.17835 FVAR 0.04900 MOLE 1 SI1 4 0.249865 0.882772 0.377896 11.00000 0.02289 0.02305 = 0.02387 -0.00223 0.00262 -0.00323 SI2 4 0.242283 0.723729 0.128744 11.00000 0.02790 0.02439 = 0.02352 -0.00529 0.00582 -0.00251 O1 3 0.256758 0.833679 0.210576 11.00000 0.02524 0.03669 = 0.03290 -0.00991 0.01050 -0.00645 O2 3 0.087907 0.685758 1.189226 11.00000 0.02543 0.03848 = 0.02973 -0.00226 0.00621 -0.00252 O3 3 0.116930 0.757063 1.343545 11.00000 0.03572 0.03452 = 0.01909 0.00006 0.00320 -0.00343 C1 1 0.243658 1.041576 0.364564 11.00000 0.03329 0.02122 = 0.04194 0.00084 0.00888 -0.00492 AFIX 137 H1A 2 0.257590 1.085004 0.357452 11.00000 -1.50000 H1B 2 0.236768 1.066651 0.456304 11.00000 -1.50000 H1C 2 0.233340 1.056871 0.272901 11.00000 -1.50000 AFIX 0 C2 1 0.272511 0.856817 0.533335 11.00000 0.02916 0.03131 = 0.04710 0.00068 -0.00862 -0.00560 AFIX 137 H2A 2 0.276814 0.774226 0.533937 11.00000 -1.50000 H2B 2 0.267220 0.877257 0.632524 11.00000 -1.50000 H2C 2 0.285491 0.905224 0.515844 11.00000 -1.50000 AFIX 0 C3 1 0.229573 0.764763 -0.065686 11.00000 0.04884 0.03116 = 0.02664 0.00062 0.00642 -0.00610 AFIX 137 H3A 2 0.220207 0.834278 -0.058326 11.00000 -1.50000 H3B 2 0.220351 0.700073 -0.109474 11.00000 -1.50000 H3C 2 0.241444 0.781617 -0.131981 11.00000 -1.50000 AFIX 0 C4 1 0.259792 0.592162 0.118937 11.00000 0.04160 0.04037 = 0.03291 -0.00644 0.00402 0.00718 AFIX 137 H4A 2 0.272281 0.609075 0.057982 11.00000 -1.50000 H4B 2 0.250750 0.528483 0.070577 11.00000 -1.50000 H4C 2 0.265653 0.568980 0.223037 11.00000 -1.50000 AFIX 0 C5 1 0.220692 0.708705 0.270741 11.00000 0.02875 0.01658 = 0.02036 0.00211 0.00117 -0.00013 C6 1 0.224809 0.787318 0.396040 11.00000 0.02365 0.01878 = 0.02214 0.00154 -0.00037 0.00046 C7 1 0.210316 0.785995 0.513454 11.00000 0.02775 0.01850 = 0.02010 0.00278 -0.00109 0.00111 AFIX 43 H7 2 0.213025 0.837376 0.598563 11.00000 -1.20000 AFIX 0 C8 1 0.192008 0.710171 0.506546 11.00000 0.02491 0.02199 = 0.02300 0.00678 0.00102 0.00115 C9 1 0.187888 0.634950 0.381489 11.00000 0.02492 0.02514 = 0.02767 -0.00059 0.00137 -0.00504 AFIX 43 H9 2 0.175315 0.584173 0.375264 11.00000 -1.20000 AFIX 0 C10 1 0.202361 0.634650 0.265281 11.00000 0.03198 0.02116 = 0.02379 -0.00475 0.00227 -0.00402 AFIX 43 H10 2 0.199572 0.582643 0.180913 11.00000 -1.20000 AFIX 0 C11 1 0.177454 0.709006 0.627255 11.00000 0.02723 0.02166 = 0.02530 0.00341 -0.00014 0.00293 C12 1 0.165866 0.707111 0.730895 11.00000 0.02734 0.02283 = 0.02478 0.00241 0.00279 -0.00041 C13 1 0.151258 0.708005 0.853218 11.00000 0.03352 0.02193 = 0.02080 -0.00053 0.00353 0.00102 C14 1 0.158575 0.759556 0.994890 11.00000 0.02171 0.03127 = 0.02752 -0.00145 0.00368 -0.00243 AFIX 43 H14 2 0.173194 0.791782 1.011390 11.00000 -1.20000 AFIX 0 C15 1 0.144294 0.763167 1.110942 11.00000 0.02765 0.02546 = 0.02060 -0.00181 0.00045 -0.00115 AFIX 43 H15 2 0.149255 0.797421 1.207236 11.00000 -1.20000 AFIX 0 C16 1 0.122826 0.717077 1.087200 11.00000 0.02791 0.01939 = 0.02313 0.00144 0.00385 0.00301 C17 1 0.115547 0.664197 0.946555 11.00000 0.02223 0.02310 = 0.02567 -0.00026 -0.00129 -0.00359 AFIX 43 H17 2 0.100931 0.631884 0.930508 11.00000 -1.20000 AFIX 0 C18 1 0.129668 0.659377 0.832115 11.00000 0.04017 0.01938 = 0.01921 0.00094 0.00039 -0.00130 AFIX 43 H18 2 0.124780 0.622658 0.737314 11.00000 -1.20000 AFIX 0 C19 1 0.107228 0.718351 1.208287 11.00000 0.02598 0.02181 = 0.02548 0.00032 0.00072 -0.00056 C20 1 0.103007 0.752739 1.468206 11.00000 0.04848 0.03566 = 0.02072 -0.00029 0.00650 -0.00171 AFIX 137 H20A 2 0.091436 0.813183 1.453553 11.00000 -1.50000 H20B 2 0.112183 0.766318 1.565500 11.00000 -1.50000 H20C 2 0.095903 0.675767 1.470605 11.00000 -1.50000 AFIX 0 SI21 4 0.034160 -0.093011 0.372788 11.00000 0.02585 0.03310 = 0.01774 -0.00743 0.00522 -0.01277 SI22 4 0.045552 0.065863 0.617395 11.00000 0.02707 0.03239 = 0.01502 -0.00532 0.00360 -0.00859 O21 3 0.028614 -0.036026 0.539050 11.00000 0.02791 0.04714 = 0.02191 -0.01263 0.01033 -0.01676 O22 3 0.195203 0.088920 -0.467981 11.00000 0.02279 0.04573 = 0.03028 0.00440 0.00317 -0.00312 O23 3 0.167321 -0.002096 -0.613696 11.00000 0.02909 0.03256 = 0.02281 -0.00093 0.00909 0.00092 C21 1 0.011946 -0.058108 0.215589 11.00000 0.02553 0.04531 = 0.02300 -0.00880 0.00317 -0.00799 AFIX 137 H21A 2 -0.001782 -0.100455 0.232777 11.00000 -1.50000 H21B 2 0.016951 -0.081601 0.116661 11.00000 -1.50000 H21C 2 0.008985 0.026088 0.214655 11.00000 -1.50000 AFIX 0 C22 1 0.037991 -0.252513 0.393948 11.00000 0.04963 0.03249 = 0.02994 -0.00173 0.00785 -0.01477 AFIX 137 H22A 2 0.049765 -0.268565 0.476926 11.00000 -1.50000 H22B 2 0.042300 -0.285323 0.297521 11.00000 -1.50000 H22C 2 0.023939 -0.288261 0.418622 11.00000 -1.50000 AFIX 0 C23 1 0.030901 0.208317 0.623639 11.00000 0.03337 0.04548 = 0.03308 -0.00334 0.01136 0.00502 AFIX 137 H23A 2 0.025216 0.231440 0.519160 11.00000 -1.50000 H23B 2 0.041376 0.267698 0.667940 11.00000 -1.50000 H23C 2 0.018377 0.201027 0.687114 11.00000 -1.50000 AFIX 0 C24 1 0.057269 0.024041 0.814275 11.00000 0.03874 0.04155 = 0.01841 -0.00628 0.00253 -0.00967 AFIX 137 H24A 2 0.045042 0.013988 0.879755 11.00000 -1.50000 H24B 2 0.067390 0.085533 0.857013 11.00000 -1.50000 H24C 2 0.065554 -0.049459 0.809905 11.00000 -1.50000 AFIX 0 C25 1 0.066700 0.064114 0.473918 11.00000 0.02558 0.02029 = 0.01734 -0.00138 0.00361 -0.00376 C26 1 0.060855 -0.014023 0.349608 11.00000 0.02379 0.02428 = 0.01688 0.00023 0.00222 -0.00312 C27 1 0.074643 -0.021362 0.230486 11.00000 0.02418 0.02105 = 0.01618 -0.00027 0.00042 0.00036 AFIX 43 H27 2 0.070721 -0.072325 0.146409 11.00000 -1.20000 AFIX 0 C28 1 0.094178 0.045408 0.233299 11.00000 0.02448 0.02074 = 0.01689 0.00542 0.00168 -0.00022 C29 1 0.100110 0.120679 0.356718 11.00000 0.02046 0.02393 = 0.02570 0.00301 0.00544 -0.00119 AFIX 43 H29 2 0.113475 0.165374 0.359204 11.00000 -1.20000 AFIX 0 C30 1 0.086427 0.129934 0.475565 11.00000 0.02786 0.02373 = 0.02055 -0.00272 0.00237 -0.00435 AFIX 43 H30 2 0.090476 0.181416 0.558874 11.00000 -1.20000 AFIX 0 C31 1 0.108312 0.040301 0.108861 11.00000 0.02473 0.01797 = 0.01918 -0.00006 0.00243 -0.00344 C32 1 0.119862 0.040004 0.004233 11.00000 0.02012 0.02029 = 0.02176 -0.00117 0.00003 -0.00049 C33 1 0.133978 0.041618 -0.119332 11.00000 0.02525 0.01882 = 0.02080 0.00277 0.00638 0.00386 C34 1 0.127108 -0.011399 -0.258802 11.00000 0.02235 0.02710 = 0.02529 -0.00218 0.00345 -0.00281 AFIX 43 H34 2 0.112898 -0.048477 -0.272769 11.00000 -1.20000 AFIX 0 C35 1 0.140797 -0.010754 -0.378012 11.00000 0.02488 0.02841 = 0.02383 -0.00262 0.00283 0.00353 AFIX 43 H35 2 0.135906 -0.046828 -0.473246 11.00000 -1.20000 AFIX 0 C36 1 0.161594 0.042508 -0.358074 11.00000 0.02536 0.02417 = 0.01910 0.00494 0.00584 0.00788 C37 1 0.168571 0.096781 -0.218506 11.00000 0.02105 0.02866 = 0.02366 0.00701 0.00042 0.00010 AFIX 43 H37 2 0.182791 0.133805 -0.205267 11.00000 -1.20000 AFIX 0 C38 1 0.154999 0.097154 -0.099530 11.00000 0.02771 0.02084 = 0.02012 0.00170 0.00184 0.00081 AFIX 43 H38 2 0.159807 0.134582 -0.005077 11.00000 -1.20000 AFIX 0 C39 1 0.176808 0.046444 -0.481928 11.00000 0.02202 0.02967 = 0.02767 0.00844 0.00617 0.00996 C40 1 0.181263 -0.002000 -0.739884 11.00000 0.03918 0.03461 = 0.02199 0.00116 0.00643 0.00633 AFIX 137 H40A 2 0.187478 0.076311 -0.751478 11.00000 -1.50000 H40B 2 0.172250 -0.024130 -0.834933 11.00000 -1.50000 H40C 2 0.193502 -0.058115 -0.718679 11.00000 -1.50000 AFIX 0 SI41 4 0.035872 0.554188 0.876472 11.00000 0.02570 0.03080 = 0.01681 0.00626 0.00469 0.01031 SI42 4 0.046503 0.397081 1.123284 11.00000 0.02404 0.02845 = 0.01632 0.00643 0.00497 0.00487 O41 3 0.030012 0.500135 1.043640 11.00000 0.02823 0.04448 = 0.02073 0.00960 0.00802 0.01565 O42 3 0.197378 0.285960 0.061254 11.00000 0.02839 0.03882 = 0.03603 -0.00414 0.00889 0.00905 O43 3 0.176998 0.424492 -0.071726 11.00000 0.03900 0.02671 = 0.03885 0.00402 0.02158 0.00677 C41 1 0.041201 0.714113 0.892702 11.00000 0.05214 0.02695 = 0.03331 0.00207 0.00475 0.01471 AFIX 137 H41A 2 0.027949 0.753224 0.925661 11.00000 -1.50000 H41B 2 0.044416 0.744945 0.792571 11.00000 -1.50000 H41C 2 0.054043 0.728362 0.968417 11.00000 -1.50000 AFIX 0 C42 1 0.013048 0.523156 0.723713 11.00000 0.02343 0.04651 = 0.02969 0.01343 0.00474 0.00590 AFIX 137 H42A 2 0.011417 0.438483 0.710460 11.00000 -1.50000 H42B 2 0.016656 0.558421 0.626959 11.00000 -1.50000 H42C 2 -0.001000 0.556149 0.752923 11.00000 -1.50000 AFIX 0 C43 1 0.058342 0.438771 1.319275 11.00000 0.03771 0.03707 = 0.01614 0.00389 0.00231 0.00723 AFIX 137 H43A 2 0.066373 0.513045 1.314858 11.00000 -1.50000 H43B 2 0.068716 0.377985 1.360855 11.00000 -1.50000 H43C 2 0.046200 0.447334 1.385779 11.00000 -1.50000 AFIX 0 C44 1 0.031119 0.257084 1.127502 11.00000 0.03324 0.04039 = 0.02759 0.00848 0.00740 0.00132 AFIX 137 H44A 2 0.018477 0.266176 1.189577 11.00000 -1.50000 H44B 2 0.041196 0.196259 1.172646 11.00000 -1.50000 H44C 2 0.025541 0.234730 1.022516 11.00000 -1.50000 AFIX 0 C45 1 0.067673 0.392368 0.978776 11.00000 0.02413 0.02087 = 0.01963 -0.00044 0.00265 0.00091 C46 1 0.062070 0.468330 0.852742 11.00000 0.02004 0.02007 = 0.01478 0.00083 0.00208 0.00295 C47 1 0.075821 0.471866 0.732435 11.00000 0.02210 0.01944 = 0.01681 0.00090 0.00274 0.00056 AFIX 43 H47 2 0.072103 0.522341 0.647531 11.00000 -1.20000 AFIX 0 C48 1 0.094913 0.402262 0.735546 11.00000 0.01940 0.01904 = 0.01881 -0.00441 0.00551 -0.00254 C49 1 0.100422 0.327866 0.860769 11.00000 0.02242 0.01844 = 0.02293 0.00161 0.00057 0.00573 AFIX 43 H49 2 0.113472 0.280632 0.864015 11.00000 -1.20000 AFIX 0 C50 1 0.086762 0.323328 0.980145 11.00000 0.02999 0.01784 = 0.01825 0.00471 0.00147 0.00223 AFIX 43 H50 2 0.090521 0.272155 1.064247 11.00000 -1.20000 AFIX 0 C51 1 0.109185 0.403927 0.612541 11.00000 0.02347 0.01798 = 0.02428 -0.00224 0.00204 -0.00406 C52 1 0.121380 0.400885 0.512501 11.00000 0.02385 0.01891 = 0.02117 -0.00337 0.00198 0.00020 C53 1 0.136318 0.390211 0.393917 11.00000 0.02010 0.01671 = 0.02343 -0.00430 0.00623 -0.00427 C54 1 0.130916 0.439356 0.248732 11.00000 0.02436 0.01932 = 0.02675 0.00012 0.00424 0.00037 AFIX 43 H54 2 0.117134 0.479638 0.227116 11.00000 -1.20000 AFIX 0 C55 1 0.145522 0.429660 0.136392 11.00000 0.03095 0.02351 = 0.02304 0.00106 0.00779 -0.00359 AFIX 43 H55 2 0.141985 0.465188 0.038849 11.00000 -1.20000 AFIX 0 C56 1 0.165428 0.367724 0.166482 11.00000 0.02165 0.01744 = 0.02444 -0.00636 0.00536 -0.00491 C57 1 0.170848 0.316745 0.309779 11.00000 0.01953 0.02131 = 0.02909 -0.00543 0.00401 -0.00066 AFIX 43 H57 2 0.184390 0.274029 0.329501 11.00000 -1.20000 AFIX 0 C58 1 0.156415 0.328435 0.423998 11.00000 0.02246 0.02100 = 0.02360 -0.00045 0.00356 -0.00119 AFIX 43 H58 2 0.160171 0.294581 0.522338 11.00000 -1.20000 AFIX 0 C59 1 0.182025 0.352596 0.048526 11.00000 0.02663 0.02204 = 0.02539 -0.00576 0.00169 -0.00263 C60 1 0.192530 0.419166 -0.188430 11.00000 0.04813 0.03919 = 0.03614 0.00673 0.02486 0.00671 AFIX 137 H60A 2 0.207522 0.441056 -0.143169 11.00000 -1.50000 H60B 2 0.187694 0.473330 -0.271918 11.00000 -1.50000 H60C 2 0.192886 0.339508 -0.229187 11.00000 -1.50000 HKLF 4 REM glu09g in C2 REM R1 = 0.0549 for 10105 Fo > 4sig(Fo) and 0.0688 for all 12031 data REM 692 parameters refined using 1 restraints END WGHT 0.0909 2.7873 REM Highest difference peak 1.103, deepest hole -0.295, 1-sigma level 0.075 these two peaks could not be explained Q1 1 0.2493 0.5523 -0.1204 11.00000 0.05 1.10 Q2 1 0.2579 1.2118 0.3674 11.00000 0.05 1.09 Q3 1 0.0408 0.3354 1.1038 11.00000 0.05 0.66 Q4 1 0.0882 0.7491 1.6939 11.00000 0.05 0.59 Q5 1 0.1152 0.6835 0.8537 11.00000 0.05 0.57 Q6 1 0.0380 -0.1604 0.3822 11.00000 0.05 0.50 Q7 1 0.0285 0.4981 0.8672 11.00000 0.05 0.48 Q8 1 0.1947 0.3619 0.0253 11.00000 0.05 0.48 Q9 1 0.1321 0.7745 1.3367 11.00000 0.05 0.46 Q10 1 0.1654 0.4421 -0.1093 11.00000 0.05 0.46 Q11 1 0.1509 0.7249 1.3594 11.00000 0.05 0.45 Q12 1 0.1058 0.7071 0.7176 11.00000 0.05 0.45 Q13 1 0.1455 0.6718 0.6204 11.00000 0.05 0.45 Q14 1 0.1222 0.7232 1.5892 11.00000 0.05 0.45 Q15 1 0.2428 1.0974 0.2922 11.00000 0.05 0.44 Q16 1 0.1580 0.6816 0.5051 11.00000 0.05 0.43 Q17 1 0.1640 0.7259 1.2346 11.00000 0.05 0.42 Q18 1 0.2209 0.7214 -0.2249 11.00000 0.05 0.41 Q19 1 0.2291 0.6691 0.4384 11.00000 0.05 0.41 Q20 1 0.0344 -0.0793 0.4813 11.00000 0.05 0.40 ; _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^)+(0.0909P)^2^+2.7879P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(15) _refine_ls_number_reflns 12031 _refine_ls_number_parameters 692 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1458 _refine_ls_wR_factor_gt 0.1359 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 0.249865(16) 0.88277(8) 0.37790(10) 0.0232(2) Uani 1 1 d . . . Si2 Si 0.242283(17) 0.72373(8) 0.12874(10) 0.0251(2) Uani 1 1 d . . . O1 O 0.25676(4) 0.8337(2) 0.2106(3) 0.0311(6) Uani 1 1 d . . . O2 O 0.08791(4) 0.6858(2) 1.1892(3) 0.0310(6) Uani 1 1 d . . . O3 O 0.11693(4) 0.7571(2) 1.3435(2) 0.0297(6) Uani 1 1 d . . . C1 C 0.24366(6) 1.0416(3) 0.3646(4) 0.0318(8) Uani 1 1 d . . . H1A H 0.2576 1.0850 0.3575 0.048 Uiso 1 1 calc R . . H1B H 0.2368 1.0667 0.4563 0.048 Uiso 1 1 calc R . . H1C H 0.2333 1.0569 0.2729 0.048 Uiso 1 1 calc R . . C2 C 0.27251(6) 0.8568(3) 0.5333(4) 0.0367(9) Uani 1 1 d . . . H2A H 0.2768 0.7742 0.5339 0.055 Uiso 1 1 calc R . . H2B H 0.2672 0.8773 0.6325 0.055 Uiso 1 1 calc R . . H2C H 0.2855 0.9052 0.5158 0.055 Uiso 1 1 calc R . . C3 C 0.22957(7) 0.7648(3) -0.0657(4) 0.0354(9) Uani 1 1 d . . . H3A H 0.2202 0.8343 -0.0583 0.053 Uiso 1 1 calc R . . H3B H 0.2204 0.7001 -0.1095 0.053 Uiso 1 1 calc R . . H3C H 0.2414 0.7816 -0.1320 0.053 Uiso 1 1 calc R . . C4 C 0.25979(7) 0.5922(4) 0.1189(4) 0.0383(9) Uani 1 1 d . . . H4A H 0.2723 0.6091 0.0580 0.057 Uiso 1 1 calc R . . H4B H 0.2508 0.5285 0.0706 0.057 Uiso 1 1 calc R . . H4C H 0.2657 0.5690 0.2230 0.057 Uiso 1 1 calc R . . C5 C 0.22069(6) 0.7087(3) 0.2707(3) 0.0220(7) Uani 1 1 d . . . C6 C 0.22481(6) 0.7873(3) 0.3960(3) 0.0217(7) Uani 1 1 d . . . C7 C 0.21032(6) 0.7860(3) 0.5135(3) 0.0223(7) Uani 1 1 d . . . H7 H 0.2130 0.8374 0.5986 0.027 Uiso 1 1 calc R . . C8 C 0.19201(6) 0.7102(3) 0.5065(4) 0.0234(7) Uani 1 1 d . . . C9 C 0.18789(6) 0.6350(3) 0.3815(4) 0.0260(7) Uani 1 1 d . . . H9 H 0.1753 0.5842 0.3753 0.031 Uiso 1 1 calc R . . C10 C 0.20236(6) 0.6347(3) 0.2653(4) 0.0257(7) Uani 1 1 d . . . H10 H 0.1996 0.5826 0.1809 0.031 Uiso 1 1 calc R . . C11 C 0.17745(6) 0.7090(3) 0.6273(4) 0.0249(7) Uani 1 1 d . . . C12 C 0.16587(6) 0.7071(3) 0.7309(4) 0.0250(7) Uani 1 1 d . . . C13 C 0.15126(6) 0.7080(3) 0.8532(3) 0.0254(7) Uani 1 1 d . . . C14 C 0.15857(6) 0.7596(3) 0.9949(4) 0.0268(7) Uani 1 1 d . . . H14 H 0.1732 0.7918 1.0114 0.032 Uiso 1 1 calc R . . C15 C 0.14429(6) 0.7632(3) 1.1109(4) 0.0247(7) Uani 1 1 d . . . H15 H 0.1493 0.7974 1.2072 0.030 Uiso 1 1 calc R . . C16 C 0.12283(6) 0.7171(3) 1.0872(3) 0.0234(7) Uani 1 1 d . . . C17 C 0.11555(6) 0.6642(3) 0.9466(4) 0.0239(7) Uani 1 1 d . . . H17 H 0.1009 0.6319 0.9305 0.029 Uiso 1 1 calc R . . C18 C 0.12967(6) 0.6594(3) 0.8321(4) 0.0264(8) Uani 1 1 d . . . H18 H 0.1248 0.6227 0.7373 0.032 Uiso 1 1 calc R . . C19 C 0.10723(6) 0.7184(3) 1.2083(4) 0.0245(7) Uani 1 1 d . . . C20 C 0.10301(7) 0.7527(4) 1.4682(4) 0.0347(9) Uani 1 1 d . . . H20A H 0.0914 0.8132 1.4536 0.052 Uiso 1 1 calc R . . H20B H 0.1122 0.7663 1.5655 0.052 Uiso 1 1 calc R . . H20C H 0.0959 0.6758 1.4706 0.052 Uiso 1 1 calc R . . Si21 Si 0.034160(16) -0.09301(9) 0.37279(10) 0.0254(2) Uani 1 1 d . . . Si22 Si 0.045552(16) 0.06586(9) 0.61739(9) 0.0247(2) Uani 1 1 d . . . O21 O 0.02861(4) -0.0360(2) 0.5391(3) 0.0318(6) Uani 1 1 d . . . O22 O 0.19520(4) 0.0889(2) -0.4680(3) 0.0329(6) Uani 1 1 d . . . O23 O 0.16732(4) -0.0021(2) -0.6137(2) 0.0277(5) Uani 1 1 d . . . C21 C 0.01195(6) -0.0581(4) 0.2156(4) 0.0312(9) Uani 1 1 d . . . H21A H -0.0018 -0.1005 0.2328 0.047 Uiso 1 1 calc R . . H21B H 0.0170 -0.0816 0.1167 0.047 Uiso 1 1 calc R . . H21C H 0.0090 0.0261 0.2147 0.047 Uiso 1 1 calc R . . C22 C 0.03799(7) -0.2525(3) 0.3939(4) 0.0371(9) Uani 1 1 d . . . H22A H 0.0498 -0.2686 0.4769 0.056 Uiso 1 1 calc R . . H22B H 0.0423 -0.2853 0.2975 0.056 Uiso 1 1 calc R . . H22C H 0.0239 -0.2883 0.4186 0.056 Uiso 1 1 calc R . . C23 C 0.03090(7) 0.2083(4) 0.6236(4) 0.0368(9) Uani 1 1 d . . . H23A H 0.0252 0.2314 0.5192 0.055 Uiso 1 1 calc R . . H23B H 0.0414 0.2677 0.6679 0.055 Uiso 1 1 calc R . . H23C H 0.0184 0.2010 0.6871 0.055 Uiso 1 1 calc R . . C24 C 0.05727(7) 0.0240(4) 0.8143(4) 0.0329(9) Uani 1 1 d . . . H24A H 0.0450 0.0140 0.8798 0.049 Uiso 1 1 calc R . . H24B H 0.0674 0.0855 0.8570 0.049 Uiso 1 1 calc R . . H24C H 0.0656 -0.0495 0.8099 0.049 Uiso 1 1 calc R . . C25 C 0.06670(6) 0.0641(3) 0.4739(3) 0.0210(7) Uani 1 1 d . . . C26 C 0.06086(6) -0.0140(3) 0.3496(3) 0.0216(7) Uani 1 1 d . . . C27 C 0.07464(6) -0.0214(3) 0.2305(3) 0.0206(7) Uani 1 1 d . . . H27 H 0.0707 -0.0723 0.1464 0.025 Uiso 1 1 calc R . . C28 C 0.09418(6) 0.0454(3) 0.2333(3) 0.0207(7) Uani 1 1 d . . . C29 C 0.10011(6) 0.1207(3) 0.3567(4) 0.0232(7) Uani 1 1 d . . . H29 H 0.1135 0.1654 0.3592 0.028 Uiso 1 1 calc R . . C30 C 0.08643(6) 0.1299(3) 0.4756(4) 0.0240(7) Uani 1 1 d . . . H30 H 0.0905 0.1814 0.5589 0.029 Uiso 1 1 calc R . . C31 C 0.10831(6) 0.0403(3) 0.1089(3) 0.0206(7) Uani 1 1 d . . . C32 C 0.11986(5) 0.0400(3) 0.0042(3) 0.0209(7) Uani 1 1 d . . . C33 C 0.13398(6) 0.0416(3) -0.1193(3) 0.0214(7) Uani 1 1 d . . . C34 C 0.12711(6) -0.0114(3) -0.2588(4) 0.0248(7) Uani 1 1 d . . . H34 H 0.1129 -0.0485 -0.2728 0.030 Uiso 1 1 calc R . . C35 C 0.14080(6) -0.0108(3) -0.3780(4) 0.0257(7) Uani 1 1 d . . . H35 H 0.1359 -0.0468 -0.4732 0.031 Uiso 1 1 calc R . . C36 C 0.16159(6) 0.0425(3) -0.3581(3) 0.0226(7) Uani 1 1 d . . . C37 C 0.16857(6) 0.0968(3) -0.2185(4) 0.0246(7) Uani 1 1 d . . . H37 H 0.1828 0.1338 -0.2053 0.029 Uiso 1 1 calc R . . C38 C 0.15500(6) 0.0972(3) -0.0995(4) 0.0229(7) Uani 1 1 d . . . H38 H 0.1598 0.1346 -0.0051 0.028 Uiso 1 1 calc R . . C39 C 0.17681(6) 0.0464(3) -0.4819(4) 0.0262(7) Uani 1 1 d . . . C40 C 0.18126(6) -0.0020(3) -0.7399(4) 0.0317(8) Uani 1 1 d . . . H40A H 0.1875 0.0763 -0.7515 0.048 Uiso 1 1 calc R . . H40B H 0.1723 -0.0241 -0.8349 0.048 Uiso 1 1 calc R . . H40C H 0.1935 -0.0581 -0.7187 0.048 Uiso 1 1 calc R . . Si41 Si 0.035872(16) 0.55419(9) 0.87647(9) 0.0243(2) Uani 1 1 d . . . Si42 Si 0.046503(16) 0.39708(8) 1.12328(9) 0.0227(2) Uani 1 1 d . . . O41 O 0.03001(4) 0.5001(2) 1.0436(2) 0.0308(6) Uani 1 1 d . . . O42 O 0.19738(4) 0.2860(2) 0.0613(3) 0.0340(6) Uani 1 1 d . . . O43 O 0.17700(4) 0.4245(2) -0.0717(3) 0.0337(6) Uani 1 1 d . . . C41 C 0.04120(7) 0.7141(3) 0.8927(4) 0.0374(10) Uani 1 1 d . . . H41A H 0.0279 0.7532 0.9257 0.056 Uiso 1 1 calc R . . H41B H 0.0444 0.7449 0.7926 0.056 Uiso 1 1 calc R . . H41C H 0.0540 0.7284 0.9684 0.056 Uiso 1 1 calc R . . C42 C 0.01305(6) 0.5232(4) 0.7237(4) 0.0331(9) Uani 1 1 d . . . H42A H 0.0114 0.4385 0.7105 0.050 Uiso 1 1 calc R . . H42B H 0.0167 0.5584 0.6270 0.050 Uiso 1 1 calc R . . H42C H -0.0010 0.5561 0.7529 0.050 Uiso 1 1 calc R . . C43 C 0.05834(7) 0.4388(3) 1.3193(3) 0.0303(8) Uani 1 1 d . . . H43A H 0.0664 0.5130 1.3149 0.045 Uiso 1 1 calc R . . H43B H 0.0687 0.3780 1.3609 0.045 Uiso 1 1 calc R . . H43C H 0.0462 0.4473 1.3858 0.045 Uiso 1 1 calc R . . C44 C 0.03112(7) 0.2571(4) 1.1275(4) 0.0334(9) Uani 1 1 d . . . H44A H 0.0185 0.2662 1.1896 0.050 Uiso 1 1 calc R . . H44B H 0.0412 0.1963 1.1726 0.050 Uiso 1 1 calc R . . H44C H 0.0255 0.2347 1.0225 0.050 Uiso 1 1 calc R . . C45 C 0.06767(5) 0.3924(3) 0.9788(3) 0.0215(7) Uani 1 1 d . . . C46 C 0.06207(5) 0.4683(3) 0.8527(3) 0.0183(7) Uani 1 1 d . . . C47 C 0.07582(5) 0.4719(3) 0.7324(3) 0.0194(7) Uani 1 1 d . . . H47 H 0.0721 0.5223 0.6475 0.023 Uiso 1 1 calc R . . C48 C 0.09491(5) 0.4023(3) 0.7355(3) 0.0188(6) Uani 1 1 d . . . C49 C 0.10042(6) 0.3279(3) 0.8608(3) 0.0214(7) Uani 1 1 d . . . H49 H 0.1135 0.2806 0.8640 0.026 Uiso 1 1 calc R . . C50 C 0.08676(6) 0.3233(3) 0.9801(3) 0.0221(7) Uani 1 1 d . . . H50 H 0.0905 0.2722 1.0642 0.026 Uiso 1 1 calc R . . C51 C 0.10919(6) 0.4039(3) 0.6125(3) 0.0219(7) Uani 1 1 d . . . C52 C 0.12138(5) 0.4009(3) 0.5125(3) 0.0213(7) Uani 1 1 d . . . C53 C 0.13632(5) 0.3902(3) 0.3939(3) 0.0198(6) Uani 1 1 d . . . C54 C 0.13092(6) 0.4394(3) 0.2487(4) 0.0234(7) Uani 1 1 d . . . H54 H 0.1171 0.4796 0.2271 0.028 Uiso 1 1 calc R . . C55 C 0.14552(6) 0.4297(3) 0.1364(4) 0.0255(7) Uani 1 1 d . . . H55 H 0.1420 0.4652 0.0388 0.031 Uiso 1 1 calc R . . C56 C 0.16543(5) 0.3677(3) 0.1665(3) 0.0210(7) Uani 1 1 d . . . C57 C 0.17085(6) 0.3167(3) 0.3098(4) 0.0232(7) Uani 1 1 d . . . H57 H 0.1844 0.2740 0.3295 0.028 Uiso 1 1 calc R . . C58 C 0.15641(6) 0.3284(3) 0.4240(4) 0.0223(7) Uani 1 1 d . . . H58 H 0.1602 0.2946 0.5223 0.027 Uiso 1 1 calc R . . C59 C 0.18202(6) 0.3526(3) 0.0485(4) 0.0247(7) Uani 1 1 d . . . C60 C 0.19253(7) 0.4192(4) -0.1884(4) 0.0398(10) Uani 1 1 d . . . H60A H 0.2075 0.4411 -0.1432 0.060 Uiso 1 1 calc R . . H60B H 0.1877 0.4733 -0.2719 0.060 Uiso 1 1 calc R . . H60C H 0.1929 0.3395 -0.2292 0.060 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 Si1 0.0229(5) 0.0231(5) 0.0239(4) -0.0022(4) 0.0026(3) -0.0032(4) Si2 0.0279(5) 0.0244(5) 0.0235(4) -0.0053(4) 0.0058(4) -0.0025(4) O1 0.0252(14) 0.0367(14) 0.0329(13) -0.0099(11) 0.0105(10) -0.0064(11) O2 0.0254(14) 0.0385(15) 0.0297(12) -0.0023(11) 0.0062(10) -0.0025(11) O3 0.0357(15) 0.0345(14) 0.0191(11) 0.0001(10) 0.0032(10) -0.0034(11) C1 0.033(2) 0.0212(18) 0.042(2) 0.0008(15) 0.0089(16) -0.0049(16) C2 0.029(2) 0.031(2) 0.047(2) 0.0007(17) -0.0086(17) -0.0056(16) C3 0.049(3) 0.031(2) 0.0266(17) 0.0006(15) 0.0064(16) -0.0061(18) C4 0.042(2) 0.040(2) 0.0329(18) -0.0064(17) 0.0040(17) 0.0072(19) C5 0.0287(19) 0.0166(16) 0.0204(14) 0.0021(12) 0.0012(12) -0.0001(14) C6 0.0237(19) 0.0188(16) 0.0221(15) 0.0015(13) -0.0004(13) 0.0005(13) C7 0.0277(19) 0.0185(16) 0.0201(15) 0.0028(13) -0.0011(13) 0.0011(14) C8 0.0249(18) 0.0220(17) 0.0230(15) 0.0068(13) 0.0010(13) 0.0012(14) C9 0.0249(19) 0.0251(18) 0.0277(16) -0.0006(13) 0.0014(14) -0.0050(14) C10 0.032(2) 0.0212(17) 0.0238(16) -0.0048(13) 0.0023(14) -0.0040(14) C11 0.0272(19) 0.0217(17) 0.0253(16) 0.0034(13) -0.0001(14) 0.0029(14) C12 0.0273(19) 0.0228(18) 0.0248(15) 0.0024(13) 0.0028(14) -0.0004(14) C13 0.034(2) 0.0219(17) 0.0208(15) -0.0005(13) 0.0035(13) 0.0010(15) C14 0.0217(19) 0.0313(19) 0.0275(16) -0.0014(14) 0.0037(13) -0.0024(15) C15 0.0277(19) 0.0255(18) 0.0206(15) -0.0018(13) 0.0004(13) -0.0011(14) C16 0.0279(19) 0.0194(16) 0.0231(15) 0.0014(13) 0.0039(13) 0.0030(14) C17 0.0222(18) 0.0231(17) 0.0257(16) -0.0003(13) -0.0013(13) -0.0036(14) C18 0.040(2) 0.0194(17) 0.0192(15) 0.0009(13) 0.0004(14) -0.0013(15) C19 0.0260(19) 0.0218(17) 0.0255(16) 0.0003(13) 0.0007(13) -0.0006(15) C20 0.048(3) 0.036(2) 0.0207(16) -0.0003(15) 0.0065(15) -0.0017(18) Si21 0.0259(5) 0.0331(5) 0.0177(4) -0.0074(4) 0.0052(3) -0.0128(4) Si22 0.0271(5) 0.0324(5) 0.0150(4) -0.0053(4) 0.0036(3) -0.0086(4) O21 0.0279(14) 0.0471(16) 0.0219(11) -0.0126(11) 0.0103(10) -0.0168(12) O22 0.0228(14) 0.0457(16) 0.0303(12) 0.0044(12) 0.0032(10) -0.0031(12) O23 0.0291(14) 0.0326(14) 0.0228(11) -0.0009(10) 0.0091(10) 0.0009(11) C21 0.026(2) 0.045(2) 0.0230(16) -0.0088(16) 0.0032(14) -0.0080(17) C22 0.050(3) 0.032(2) 0.0299(19) -0.0017(16) 0.0079(17) -0.0148(19) C23 0.033(2) 0.045(2) 0.0331(19) -0.0033(18) 0.0114(16) 0.0050(19) C24 0.039(2) 0.042(2) 0.0184(16) -0.0063(15) 0.0025(15) -0.0097(18) C25 0.0256(18) 0.0203(16) 0.0173(14) -0.0014(13) 0.0036(12) -0.0038(14) C26 0.0238(19) 0.0243(17) 0.0169(14) 0.0002(13) 0.0022(13) -0.0031(14) C27 0.0242(19) 0.0210(17) 0.0162(14) -0.0003(12) 0.0004(12) 0.0004(14) C28 0.0245(18) 0.0207(16) 0.0169(14) 0.0054(12) 0.0017(12) -0.0002(14) C29 0.0205(18) 0.0239(17) 0.0257(16) 0.0030(14) 0.0054(13) -0.0012(14) C30 0.028(2) 0.0237(17) 0.0205(15) -0.0027(13) 0.0024(13) -0.0044(15) C31 0.0247(18) 0.0180(16) 0.0192(14) -0.0001(12) 0.0024(13) -0.0034(14) C32 0.0201(18) 0.0203(16) 0.0218(15) -0.0012(13) 0.0000(13) -0.0005(13) C33 0.0252(18) 0.0188(16) 0.0208(14) 0.0028(12) 0.0064(12) 0.0039(14) C34 0.0224(19) 0.0271(18) 0.0253(16) -0.0022(14) 0.0034(13) -0.0028(15) C35 0.025(2) 0.0284(19) 0.0238(15) -0.0026(14) 0.0028(13) 0.0035(15) C36 0.0254(19) 0.0242(17) 0.0191(14) 0.0049(13) 0.0058(12) 0.0079(15) C37 0.0210(18) 0.0287(19) 0.0237(15) 0.0070(14) 0.0004(13) 0.0001(14) C38 0.0277(19) 0.0208(17) 0.0201(15) 0.0017(13) 0.0018(13) 0.0008(14) C39 0.0220(19) 0.0297(19) 0.0277(16) 0.0084(14) 0.0062(13) 0.0100(16) C40 0.039(2) 0.035(2) 0.0220(16) 0.0012(15) 0.0064(15) 0.0063(17) Si41 0.0257(5) 0.0308(5) 0.0168(4) 0.0063(4) 0.0047(3) 0.0103(4) Si42 0.0240(5) 0.0285(5) 0.0163(4) 0.0064(4) 0.0050(3) 0.0049(4) O41 0.0282(15) 0.0445(16) 0.0207(11) 0.0096(11) 0.0080(10) 0.0156(12) O42 0.0284(15) 0.0388(15) 0.0360(13) -0.0041(12) 0.0089(11) 0.0090(12) O43 0.0390(16) 0.0267(14) 0.0388(14) 0.0040(11) 0.0216(12) 0.0068(11) C41 0.052(3) 0.027(2) 0.0333(19) 0.0021(16) 0.0047(17) 0.0147(19) C42 0.023(2) 0.047(2) 0.0297(17) 0.0134(17) 0.0047(15) 0.0059(17) C43 0.038(2) 0.037(2) 0.0161(15) 0.0039(14) 0.0023(14) 0.0072(17) C44 0.033(2) 0.040(2) 0.0276(17) 0.0085(16) 0.0074(15) 0.0013(17) C45 0.0241(17) 0.0209(16) 0.0196(14) -0.0004(13) 0.0027(12) 0.0009(15) C46 0.0200(18) 0.0201(16) 0.0148(13) 0.0008(12) 0.0021(12) 0.0030(13) C47 0.0221(18) 0.0194(16) 0.0168(14) 0.0009(12) 0.0027(12) 0.0006(13) C48 0.0194(17) 0.0190(16) 0.0188(14) -0.0044(12) 0.0055(12) -0.0025(14) C49 0.0224(19) 0.0184(16) 0.0229(16) 0.0016(13) 0.0006(13) 0.0057(14) C50 0.030(2) 0.0178(16) 0.0182(15) 0.0047(12) 0.0015(13) 0.0022(14) C51 0.0235(18) 0.0180(16) 0.0243(15) -0.0022(13) 0.0020(13) -0.0041(14) C52 0.0239(18) 0.0189(16) 0.0212(14) -0.0034(13) 0.0020(12) 0.0002(14) C53 0.0201(17) 0.0167(15) 0.0234(14) -0.0043(12) 0.0062(12) -0.0043(13) C54 0.0244(19) 0.0193(17) 0.0267(16) 0.0001(13) 0.0042(14) 0.0004(14) C55 0.031(2) 0.0235(17) 0.0230(15) 0.0011(13) 0.0078(14) -0.0036(15) C56 0.0217(17) 0.0174(16) 0.0244(15) -0.0064(12) 0.0054(13) -0.0049(13) C57 0.0195(18) 0.0213(17) 0.0291(16) -0.0054(13) 0.0040(13) -0.0007(13) C58 0.0225(18) 0.0210(16) 0.0236(15) -0.0005(13) 0.0036(13) -0.0012(14) C59 0.027(2) 0.0220(17) 0.0254(16) -0.0058(13) 0.0017(14) -0.0026(15) C60 0.048(3) 0.039(2) 0.0361(19) 0.0067(17) 0.0249(18) 0.0067(19) _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 O1 1.656(2) . ? Si1 C2 1.851(4) . ? Si1 C1 1.857(4) . ? Si1 C6 1.878(3) . ? Si2 O1 1.653(3) . ? Si2 C4 1.843(4) . ? Si2 C3 1.855(4) . ? Si2 C5 1.887(3) . ? O2 C19 1.214(4) . ? O3 C19 1.342(4) . ? O3 C20 1.437(4) . ? C5 C10 1.386(5) . ? C5 C6 1.421(4) . ? C6 C7 1.408(4) . ? C7 C8 1.397(5) . ? C8 C9 1.395(5) . ? C8 C11 1.433(4) . ? C9 C10 1.399(5) . ? C11 C12 1.194(5) . ? C12 C13 1.447(4) . ? C13 C14 1.403(4) . ? C13 C18 1.406(5) . ? C14 C15 1.390(4) . ? C15 C16 1.389(5) . ? C16 C17 1.402(4) . ? C16 C19 1.479(4) . ? C17 C18 1.373(5) . ? Si21 O21 1.656(2) . ? Si21 C22 1.847(4) . ? Si21 C21 1.863(4) . ? Si21 C26 1.868(4) . ? Si21 Si22 2.8398(12) . ? Si22 O21 1.652(3) . ? Si22 C23 1.856(4) . ? Si22 C24 1.858(3) . ? Si22 C25 1.869(3) . ? O22 C39 1.202(4) . ? O23 C39 1.354(4) . ? O23 C40 1.447(4) . ? C25 C30 1.402(5) . ? C25 C26 1.425(4) . ? C26 C27 1.394(4) . ? C27 C28 1.398(5) . ? C28 C29 1.400(5) . ? C28 C31 1.444(4) . ? C29 C30 1.389(4) . ? C31 C32 1.200(4) . ? C32 C33 1.436(4) . ? C33 C34 1.388(4) . ? C33 C38 1.409(5) . ? C34 C35 1.388(4) . ? C35 C36 1.385(5) . ? C36 C37 1.397(5) . ? C36 C39 1.483(4) . ? C37 C38 1.381(4) . ? Si41 O41 1.656(2) . ? Si41 C42 1.853(4) . ? Si41 C41 1.862(4) . ? Si41 C46 1.883(3) . ? Si41 Si42 2.8338(12) . ? Si42 O41 1.650(3) . ? Si42 C44 1.852(4) . ? Si42 C43 1.853(3) . ? Si42 C45 1.877(3) . ? O42 C59 1.193(4) . ? O43 C59 1.346(4) . ? O43 C60 1.448(4) . ? C45 C50 1.391(5) . ? C45 C46 1.418(4) . ? C46 C47 1.399(4) . ? C47 C48 1.394(4) . ? C48 C49 1.401(4) . ? C48 C51 1.438(4) . ? C49 C50 1.389(4) . ? C51 C52 1.194(4) . ? C52 C53 1.440(4) . ? C53 C54 1.397(4) . ? C53 C58 1.401(5) . ? C54 C55 1.382(4) . ? C55 C56 1.392(5) . ? C56 C57 1.392(4) . ? C56 C59 1.511(4) . ? C57 C58 1.390(4) . ? 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 Si1 C2 111.43(17) . . ? O1 Si1 C1 110.03(16) . . ? C2 Si1 C1 109.38(18) . . ? O1 Si1 C6 98.48(14) . . ? C2 Si1 C6 112.46(16) . . ? C1 Si1 C6 114.67(16) . . ? O1 Si2 C4 111.35(17) . . ? O1 Si2 C3 110.87(16) . . ? C4 Si2 C3 110.50(18) . . ? O1 Si2 C5 98.66(13) . . ? C4 Si2 C5 112.77(17) . . ? C3 Si2 C5 112.20(17) . . ? Si2 O1 Si1 118.36(15) . . ? C19 O3 C20 115.0(3) . . ? C10 C5 C6 119.5(3) . . ? C10 C5 Si2 128.8(2) . . ? C6 C5 Si2 111.7(2) . . ? C7 C6 C5 118.8(3) . . ? C7 C6 Si1 128.6(2) . . ? C5 C6 Si1 112.6(2) . . ? C8 C7 C6 120.9(3) . . ? C9 C8 C7 119.8(3) . . ? C9 C8 C11 119.8(3) . . ? C7 C8 C11 120.4(3) . . ? C8 C9 C10 119.7(3) . . ? C5 C10 C9 121.3(3) . . ? C12 C11 C8 178.0(4) . . ? C11 C12 C13 177.8(4) . . ? C14 C13 C18 119.2(3) . . ? C14 C13 C12 119.6(3) . . ? C18 C13 C12 121.1(3) . . ? C15 C14 C13 119.6(3) . . ? C16 C15 C14 120.5(3) . . ? C15 C16 C17 120.1(3) . . ? C15 C16 C19 122.1(3) . . ? C17 C16 C19 117.8(3) . . ? C18 C17 C16 119.6(3) . . ? C17 C18 C13 121.0(3) . . ? O2 C19 O3 123.4(3) . . ? O2 C19 C16 124.1(3) . . ? O3 C19 C16 112.5(3) . . ? O21 Si21 C22 109.58(16) . . ? O21 Si21 C21 111.87(15) . . ? C22 Si21 C21 111.04(18) . . ? O21 Si21 C26 98.72(13) . . ? C22 Si21 C26 112.93(18) . . ? C21 Si21 C26 112.12(16) . . ? O21 Si21 Si22 30.81(9) . . ? C22 Si21 Si22 122.62(13) . . ? C21 Si21 Si22 121.40(13) . . ? C26 Si21 Si22 67.96(10) . . ? O21 Si22 C23 110.99(17) . . ? O21 Si22 C24 111.40(16) . . ? C23 Si22 C24 109.71(18) . . ? O21 Si22 C25 98.34(13) . . ? C23 Si22 C25 112.56(16) . . ? C24 Si22 C25 113.45(16) . . ? O21 Si22 Si21 30.89(8) . . ? C23 Si22 Si21 120.30(13) . . ? C24 Si22 Si21 125.06(13) . . ? C25 Si22 Si21 67.52(10) . . ? Si22 O21 Si21 118.31(15) . . ? C39 O23 C40 114.9(3) . . ? C30 C25 C26 119.4(3) . . ? C30 C25 Si22 127.9(2) . . ? C26 C25 Si22 112.7(2) . . ? C27 C26 C25 119.2(3) . . ? C27 C26 Si21 129.0(2) . . ? C25 C26 Si21 111.8(2) . . ? C26 C27 C28 120.8(3) . . ? C27 C28 C29 120.1(3) . . ? C27 C28 C31 121.2(3) . . ? C29 C28 C31 118.8(3) . . ? C30 C29 C28 119.9(3) . . ? C29 C30 C25 120.7(3) . . ? C32 C31 C28 177.7(4) . . ? C31 C32 C33 178.8(4) . . ? C34 C33 C38 119.5(3) . . ? C34 C33 C32 120.5(3) . . ? C38 C33 C32 120.0(3) . . ? C35 C34 C33 120.6(3) . . ? C36 C35 C34 120.0(3) . . ? C35 C36 C37 119.8(3) . . ? C35 C36 C39 122.2(3) . . ? C37 C36 C39 118.0(3) . . ? C38 C37 C36 120.7(3) . . ? C37 C38 C33 119.5(3) . . ? O22 C39 O23 124.0(3) . . ? O22 C39 C36 124.2(3) . . ? O23 C39 C36 111.7(3) . . ? O41 Si41 C42 111.05(15) . . ? O41 Si41 C41 110.48(16) . . ? C42 Si41 C41 110.68(18) . . ? O41 Si41 C46 98.79(13) . . ? C42 Si41 C46 112.82(16) . . ? C41 Si41 C46 112.50(17) . . ? O41 Si41 Si42 30.94(9) . . ? C42 Si41 Si42 121.57(13) . . ? C41 Si41 Si42 122.80(12) . . ? C46 Si41 Si42 67.88(9) . . ? O41 Si42 C44 110.31(16) . . ? O41 Si42 C43 111.52(15) . . ? C44 Si42 C43 110.61(17) . . ? O41 Si42 C45 98.87(13) . . ? C44 Si42 C45 111.09(16) . . ? C43 Si42 C45 113.92(16) . . ? O41 Si42 Si41 31.05(8) . . ? C44 Si42 Si41 119.23(12) . . ? C43 Si42 Si41 125.35(13) . . ? C45 Si42 Si41 67.87(10) . . ? Si42 O41 Si41 118.01(14) . . ? C59 O43 C60 114.4(3) . . ? C50 C45 C46 119.2(3) . . ? C50 C45 Si42 128.4(2) . . ? C46 C45 Si42 112.3(2) . . ? C47 C46 C45 119.3(3) . . ? C47 C46 Si41 128.9(2) . . ? C45 C46 Si41 111.9(2) . . ? C48 C47 C46 120.8(3) . . ? C47 C48 C49 119.6(3) . . ? C47 C48 C51 121.7(3) . . ? C49 C48 C51 118.6(3) . . ? C50 C49 C48 119.9(3) . . ? C49 C50 C45 121.2(3) . . ? C52 C51 C48 177.3(4) . . ? C51 C52 C53 176.7(4) . . ? C54 C53 C58 119.6(3) . . ? C54 C53 C52 120.9(3) . . ? C58 C53 C52 119.5(3) . . ? C55 C54 C53 120.3(3) . . ? C54 C55 C56 119.9(3) . . ? C57 C56 C55 120.4(3) . . ? C57 C56 C59 117.0(3) . . ? C55 C56 C59 122.7(3) . . ? C58 C57 C56 119.9(3) . . ? C57 C58 C53 119.9(3) . . ? O42 C59 O43 125.2(3) . . ? O42 C59 C56 124.3(3) . . ? O43 C59 C56 110.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Si2 O1 Si1 -114.3(2) . . . . ? C3 Si2 O1 Si1 122.2(2) . . . . ? C5 Si2 O1 Si1 4.4(2) . . . . ? C2 Si1 O1 Si2 114.5(2) . . . . ? C1 Si1 O1 Si2 -124.0(2) . . . . ? C6 Si1 O1 Si2 -3.7(2) . . . . ? O1 Si2 C5 C10 176.1(3) . . . . ? C4 Si2 C5 C10 -66.2(4) . . . . ? C3 Si2 C5 C10 59.3(4) . . . . ? O1 Si2 C5 C6 -3.3(3) . . . . ? C4 Si2 C5 C6 114.3(3) . . . . ? C3 Si2 C5 C6 -120.1(2) . . . . ? C10 C5 C6 C7 1.3(5) . . . . ? Si2 C5 C6 C7 -179.2(2) . . . . ? C10 C5 C6 Si1 -178.2(3) . . . . ? Si2 C5 C6 Si1 1.3(3) . . . . ? O1 Si1 C6 C7 -178.2(3) . . . . ? C2 Si1 C6 C7 64.3(3) . . . . ? C1 Si1 C6 C7 -61.5(3) . . . . ? O1 Si1 C6 C5 1.2(3) . . . . ? C2 Si1 C6 C5 -116.3(3) . . . . ? C1 Si1 C6 C5 117.9(3) . . . . ? C5 C6 C7 C8 -0.9(5) . . . . ? Si1 C6 C7 C8 178.5(3) . . . . ? C6 C7 C8 C9 -0.3(5) . . . . ? C6 C7 C8 C11 179.6(3) . . . . ? C7 C8 C9 C10 1.1(5) . . . . ? C11 C8 C9 C10 -178.8(3) . . . . ? C6 C5 C10 C9 -0.5(5) . . . . ? Si2 C5 C10 C9 -179.9(3) . . . . ? C8 C9 C10 C5 -0.7(5) . . . . ? C9 C8 C11 C12 119(11) . . . . ? C7 C8 C11 C12 -60(11) . . . . ? C8 C11 C12 C13 154(9) . . . . ? C11 C12 C13 C14 -110(11) . . . . ? C11 C12 C13 C18 69(11) . . . . ? C18 C13 C14 C15 -0.9(5) . . . . ? C12 C13 C14 C15 178.3(3) . . . . ? C13 C14 C15 C16 -0.5(5) . . . . ? C14 C15 C16 C17 1.3(5) . . . . ? C14 C15 C16 C19 179.4(3) . . . . ? C15 C16 C17 C18 -0.7(5) . . . . ? C19 C16 C17 C18 -178.9(3) . . . . ? C16 C17 C18 C13 -0.8(5) . . . . ? C14 C13 C18 C17 1.6(5) . . . . ? C12 C13 C18 C17 -177.6(3) . . . . ? C20 O3 C19 O2 2.6(5) . . . . ? C20 O3 C19 C16 -176.0(3) . . . . ? C15 C16 C19 O2 175.2(3) . . . . ? C17 C16 C19 O2 -6.7(5) . . . . ? C15 C16 C19 O3 -6.3(5) . . . . ? C17 C16 C19 O3 171.8(3) . . . . ? C22 Si21 Si22 O21 -72.8(3) . . . . ? C21 Si21 Si22 O21 80.1(2) . . . . ? C26 Si21 Si22 O21 -176.6(2) . . . . ? O21 Si21 Si22 C23 -80.3(2) . . . . ? C22 Si21 Si22 C23 -153.1(2) . . . . ? C21 Si21 Si22 C23 -0.2(2) . . . . ? C26 Si21 Si22 C23 103.07(19) . . . . ? O21 Si21 Si22 C24 72.2(2) . . . . ? C22 Si21 Si22 C24 -0.5(2) . . . . ? C21 Si21 Si22 C24 152.4(2) . . . . ? C26 Si21 Si22 C24 -104.40(19) . . . . ? O21 Si21 Si22 C25 175.9(2) . . . . ? C22 Si21 Si22 C25 103.1(2) . . . . ? C21 Si21 Si22 C25 -104.00(18) . . . . ? C26 Si21 Si22 C25 -0.77(16) . . . . ? C23 Si22 O21 Si21 114.3(2) . . . . ? C24 Si22 O21 Si21 -123.1(2) . . . . ? C25 Si22 O21 Si21 -3.8(2) . . . . ? C22 Si21 O21 Si22 121.4(2) . . . . ? C21 Si21 O21 Si22 -115.0(2) . . . . ? C26 Si21 O21 Si22 3.1(2) . . . . ? O21 Si22 C25 C30 -177.9(3) . . . . ? C23 Si22 C25 C30 65.1(4) . . . . ? C24 Si22 C25 C30 -60.2(4) . . . . ? Si21 Si22 C25 C30 179.9(3) . . . . ? O21 Si22 C25 C26 3.1(3) . . . . ? C23 Si22 C25 C26 -113.8(3) . . . . ? C24 Si22 C25 C26 120.9(3) . . . . ? Si21 Si22 C25 C26 1.0(2) . . . . ? C30 C25 C26 C27 -1.4(5) . . . . ? Si22 C25 C26 C27 177.6(2) . . . . ? C30 C25 C26 Si21 179.5(3) . . . . ? Si22 C25 C26 Si21 -1.5(3) . . . . ? O21 Si21 C26 C27 -179.7(3) . . . . ? C22 Si21 C26 C27 64.6(3) . . . . ? C21 Si21 C26 C27 -61.8(3) . . . . ? Si22 Si21 C26 C27 -178.0(3) . . . . ? O21 Si21 C26 C25 -0.7(3) . . . . ? C22 Si21 C26 C25 -116.4(3) . . . . ? C21 Si21 C26 C25 117.2(3) . . . . ? Si22 Si21 C26 C25 1.0(2) . . . . ? C25 C26 C27 C28 1.0(5) . . . . ? Si21 C26 C27 C28 180.0(3) . . . . ? C26 C27 C28 C29 0.1(5) . . . . ? C26 C27 C28 C31 -178.6(3) . . . . ? C27 C28 C29 C30 -0.7(5) . . . . ? C31 C28 C29 C30 178.0(3) . . . . ? C28 C29 C30 C25 0.3(5) . . . . ? C26 C25 C30 C29 0.8(5) . . . . ? Si22 C25 C30 C29 -178.1(3) . . . . ? C27 C28 C31 C32 113(9) . . . . ? C29 C28 C31 C32 -65(9) . . . . ? C28 C31 C32 C33 62(24) . . . . ? C31 C32 C33 C34 -165(76) . . . . ? C31 C32 C33 C38 15(19) . . . . ? C38 C33 C34 C35 0.4(5) . . . . ? C32 C33 C34 C35 -179.5(3) . . . . ? C33 C34 C35 C36 0.4(5) . . . . ? C34 C35 C36 C37 -0.9(5) . . . . ? C34 C35 C36 C39 -179.6(3) . . . . ? C35 C36 C37 C38 0.5(5) . . . . ? C39 C36 C37 C38 179.2(3) . . . . ? C36 C37 C38 C33 0.3(5) . . . . ? C34 C33 C38 C37 -0.8(5) . . . . ? C32 C33 C38 C37 179.1(3) . . . . ? C40 O23 C39 O22 1.3(5) . . . . ? C40 O23 C39 C36 -179.7(3) . . . . ? C35 C36 C39 O22 -177.9(3) . . . . ? C37 C36 C39 O22 3.4(5) . . . . ? C35 C36 C39 O23 3.1(4) . . . . ? C37 C36 C39 O23 -175.7(3) . . . . ? C42 Si41 Si42 O41 -78.2(2) . . . . ? C41 Si41 Si42 O41 74.6(2) . . . . ? C46 Si41 Si42 O41 177.9(2) . . . . ? O41 Si41 Si42 C44 80.9(2) . . . . ? C42 Si41 Si42 C44 2.7(2) . . . . ? C41 Si41 Si42 C44 155.5(2) . . . . ? C46 Si41 Si42 C44 -101.25(18) . . . . ? O41 Si41 Si42 C43 -72.2(2) . . . . ? C42 Si41 Si42 C43 -150.3(2) . . . . ? C41 Si41 Si42 C43 2.4(2) . . . . ? C46 Si41 Si42 C43 105.68(19) . . . . ? O41 Si41 Si42 C45 -176.5(2) . . . . ? C42 Si41 Si42 C45 105.30(18) . . . . ? C41 Si41 Si42 C45 -101.9(2) . . . . ? C46 Si41 Si42 C45 1.32(15) . . . . ? C44 Si42 O41 Si41 -113.2(2) . . . . ? C43 Si42 O41 Si41 123.42(19) . . . . ? C45 Si42 O41 Si41 3.2(2) . . . . ? C42 Si41 O41 Si42 116.7(2) . . . . ? C41 Si41 O41 Si42 -120.1(2) . . . . ? C46 Si41 O41 Si42 -2.0(2) . . . . ? O41 Si42 C45 C50 178.6(3) . . . . ? C44 Si42 C45 C50 -65.5(3) . . . . ? C43 Si42 C45 C50 60.2(4) . . . . ? Si41 Si42 C45 C50 -179.6(3) . . . . ? O41 Si42 C45 C46 -3.6(3) . . . . ? C44 Si42 C45 C46 112.3(3) . . . . ? C43 Si42 C45 C46 -121.9(3) . . . . ? Si41 Si42 C45 C46 -1.7(2) . . . . ? C50 C45 C46 C47 0.2(5) . . . . ? Si42 C45 C46 C47 -177.8(2) . . . . ? C50 C45 C46 Si41 -179.3(3) . . . . ? Si42 C45 C46 Si41 2.6(3) . . . . ? O41 Si41 C46 C47 179.9(3) . . . . ? C42 Si41 C46 C47 62.6(3) . . . . ? C41 Si41 C46 C47 -63.5(3) . . . . ? Si42 Si41 C46 C47 178.8(3) . . . . ? O41 Si41 C46 C45 -0.6(3) . . . . ? C42 Si41 C46 C45 -118.0(2) . . . . ? C41 Si41 C46 C45 115.9(3) . . . . ? Si42 Si41 C46 C45 -1.7(2) . . . . ? C45 C46 C47 C48 -0.3(5) . . . . ? Si41 C46 C47 C48 179.1(2) . . . . ? C46 C47 C48 C49 -0.1(5) . . . . ? C46 C47 C48 C51 179.5(3) . . . . ? C47 C48 C49 C50 0.5(5) . . . . ? C51 C48 C49 C50 -179.1(3) . . . . ? C48 C49 C50 C45 -0.6(5) . . . . ? C46 C45 C50 C49 0.2(5) . . . . ? Si42 C45 C50 C49 177.9(3) . . . . ? C47 C48 C51 C52 -160(7) . . . . ? C49 C48 C51 C52 19(8) . . . . ? C48 C51 C52 C53 13(12) . . . . ? C51 C52 C53 C54 136(6) . . . . ? C51 C52 C53 C58 -43(6) . . . . ? C58 C53 C54 C55 -1.6(5) . . . . ? C52 C53 C54 C55 179.2(3) . . . . ? C53 C54 C55 C56 1.9(5) . . . . ? C54 C55 C56 C57 -0.8(5) . . . . ? C54 C55 C56 C59 179.3(3) . . . . ? C55 C56 C57 C58 -0.5(5) . . . . ? C59 C56 C57 C58 179.3(3) . . . . ? C56 C57 C58 C53 0.8(5) . . . . ? C54 C53 C58 C57 0.2(5) . . . . ? C52 C53 C58 C57 179.4(3) . . . . ? C60 O43 C59 O42 -2.2(5) . . . . ? C60 O43 C59 C56 177.8(3) . . . . ? C57 C56 C59 O42 12.3(5) . . . . ? C55 C56 C59 O42 -167.9(3) . . . . ? C57 C56 C59 O43 -167.7(3) . . . . ? C55 C56 C59 O43 12.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.103 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.075 data_glu08k _database_code_depnum_ccdc_archive 'CCDC 837997' #TrackingRef 'analogues_of_ec23.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H26 Si3' _chemical_formula_sum 'C14 H26 Si3' _chemical_formula_weight 278.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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/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 14.635(4) _cell_length_b 10.5599(16) _cell_length_c 11.643(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.50(3) _cell_angle_gamma 90.00 _cell_volume 1793.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4730 _cell_measurement_theta_min 3.9 _cell_measurement_theta_max 26.05 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max .5 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.032 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.247 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8432 _exptl_absorpt_correction_T_max 1.0011 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate_Stoe-IPDS _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21879 _diffrn_reflns_av_R_equivalents 0.0949 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3958 _reflns_number_gt 2555 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. INTENSITY STATISTICS FOR DATASET # 1 GLU08c.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.06 242 252 96.0 4.90 64.2 41.62 0.0468 0.0164 2.06 - 1.62 249 250 99.6 5.29 30.6 32.13 0.0689 0.0235 1.62 - 1.41 255 258 98.8 5.32 24.7 30.25 0.0716 0.0283 1.41 - 1.28 247 251 98.4 5.32 20.3 26.59 0.0812 0.0340 1.28 - 1.18 261 262 99.6 5.42 13.2 17.83 0.1148 0.0471 1.18 - 1.11 248 257 96.5 5.19 10.6 16.23 0.1136 0.0531 1.11 - 1.05 261 268 97.4 5.31 6.3 10.09 0.1601 0.0876 1.05 - 1.00 267 276 96.7 5.25 7.0 10.66 0.1581 0.0894 1.00 - 0.96 257 263 97.7 5.30 7.0 11.29 0.1391 0.0818 0.96 - 0.92 305 324 94.1 5.14 6.8 10.45 0.1591 0.0872 0.92 - 0.89 272 275 98.9 5.36 4.7 7.20 0.1929 0.1267 0.89 - 0.86 287 313 91.7 4.98 4.0 6.22 0.1828 0.1559 0.86 - 0.83 341 355 96.1 5.20 2.8 4.44 0.2346 0.2256 0.83 - 0.81 272 289 94.1 5.03 2.5 3.81 0.2445 0.2560 0.81 - 0.79 268 289 92.7 5.07 2.1 2.90 0.2833 0.3494 0.79 - 0.77 317 338 93.8 5.06 1.3 1.80 0.3988 0.5485 following data have been cut off by SHEL command: 0.77 - 0.75 341 368 92.7 5.01 0.9 1.25 0.5059 0.8429 0.75 - 0.73 115 153 75.2 3.08 0.5 0.52 0.7606 1.9506 #----------------------------------------------------------------------------- 0.83 - 0.73 1434 1562 91.8 4.86 1.6 2.33 0.3326 0.4570 Inf - 0.73 4805 5041 95.3 5.11 11.1 12.64 0.1008 0.0613 Merged [A], lowest resolution = 8.55 Angstroms, 2061 outliers downweighted TITL glu08b in P2(1)/c CELL 0.71073 14.6354 10.5599 11.6434 90.000 94.501 90.000 ZERR 4.0 0.0038 0.0016 0.0029 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H Si UNIT 56 104 12 SHEL .77 12. L.S. 12 ACTA BOND FMAP 2 PLAN 20 HTAB 2.5 CONF TEMP -100 WGHT 0.058800 FVAR 0.64363 MOLE 1 C1 1 0.554335 0.083414 0.630485 11.00000 0.04428 0.04741 = 0.05098 0.00167 -0.01179 -0.00347 AFIX 137 H1A 2 0.517122 0.053013 0.691231 11.00000 -1.50000 H1B 2 0.577414 0.010914 0.588894 11.00000 -1.50000 H1C 2 0.516691 0.136937 0.576743 11.00000 -1.50000 AFIX 0 C2 1 0.607322 0.311974 0.779738 11.00000 0.05928 0.04314 = 0.04883 -0.00363 -0.00112 0.01514 AFIX 137 H2A 2 0.658067 0.366921 0.808351 11.00000 -1.50000 H2B 2 0.576441 0.278496 0.844992 11.00000 -1.50000 H2C 2 0.563557 0.360875 0.729491 11.00000 -1.50000 AFIX 0 C03 1 0.734005 0.237027 0.590767 11.00000 0.04922 0.03529 = 0.02708 0.00979 -0.00344 -0.00109 AFIX 23 H03A 2 0.730411 0.183680 0.520639 11.00000 -1.20000 H03B 2 0.719294 0.325545 0.568231 11.00000 -1.20000 AFIX 0 C3 1 0.941447 0.167987 0.576945 11.00000 0.05648 0.05396 = 0.03729 0.00686 0.01596 -0.00201 AFIX 137 H3A 2 0.946011 0.225320 0.511457 11.00000 -1.50000 H3B 2 0.925227 0.082914 0.548550 11.00000 -1.50000 H3C 2 1.000490 0.164914 0.622800 11.00000 -1.50000 AFIX 0 C4 1 0.886347 0.381725 0.735618 11.00000 0.05697 0.03167 = 0.04386 0.00575 -0.00078 -0.01081 AFIX 137 H4A 2 0.945810 0.372102 0.779640 11.00000 -1.50000 H4B 2 0.840421 0.409100 0.787264 11.00000 -1.50000 H4C 2 0.891384 0.445251 0.675082 11.00000 -1.50000 AFIX 0 C5 1 0.828107 0.105764 0.782544 11.00000 0.03400 0.02128 = 0.02067 -0.00003 0.00183 -0.00003 C6 1 0.734289 0.076866 0.792431 11.00000 0.03396 0.02459 = 0.02141 -0.00122 0.00082 0.00019 C7 1 0.711536 -0.017322 0.869969 11.00000 0.03598 0.02366 = 0.02531 0.00276 0.00343 -0.00151 AFIX 43 H7 2 0.648680 -0.036499 0.876050 11.00000 -1.20000 AFIX 0 C8 1 0.778080 -0.084704 0.939249 11.00000 0.03700 0.02219 = 0.01974 -0.00051 0.00252 0.00068 C9 1 0.870055 -0.051667 0.929452 11.00000 0.03798 0.02508 = 0.02312 0.00168 -0.00346 0.00267 AFIX 43 H9 2 0.916592 -0.093787 0.976435 11.00000 -1.20000 AFIX 0 C10 1 0.894925 0.040609 0.853228 11.00000 0.03327 0.02709 = 0.02420 0.00038 0.00145 -0.00087 AFIX 43 H10 2 0.957895 0.060142 0.848627 11.00000 -1.20000 AFIX 0 C11 1 0.638548 -0.179835 1.102331 11.00000 0.06662 0.05464 = 0.04856 0.01160 0.02384 -0.00131 AFIX 137 H11A 2 0.621265 -0.250578 1.150613 11.00000 -1.50000 H11B 2 0.589398 -0.164053 1.041930 11.00000 -1.50000 H11C 2 0.648374 -0.103778 1.149931 11.00000 -1.50000 AFIX 0 C12 1 0.729422 -0.365882 0.944006 11.00000 0.09362 0.03335 = 0.04616 -0.00558 0.01377 -0.01438 AFIX 137 H12A 2 0.712357 -0.436788 0.992238 11.00000 -1.50000 H12B 2 0.786500 -0.386169 0.909264 11.00000 -1.50000 H12C 2 0.680555 -0.350995 0.883040 11.00000 -1.50000 AFIX 0 C13 1 0.840912 -0.250894 1.148380 11.00000 0.06675 0.04504 = 0.03872 0.02013 -0.00116 -0.00177 AFIX 137 H13A 2 0.854210 -0.173322 1.192784 11.00000 -1.50000 H13B 2 0.895917 -0.277723 1.112078 11.00000 -1.50000 H13C 2 0.822256 -0.317852 1.199925 11.00000 -1.50000 AFIX 0 SI1 3 0.652995 0.177504 0.696387 11.00000 0.03507 0.02558 = 0.02804 0.00289 -0.00363 0.00168 SI2 3 0.850953 0.226833 0.668664 11.00000 0.03907 0.02733 = 0.02373 0.00524 0.00311 -0.00344 SI3 3 0.746344 -0.220009 1.034765 11.00000 0.04880 0.02529 = 0.02415 0.00432 0.00613 -0.00211 HKLF 4 REM glu08b in P2(1)/c REM R1 = 0.0425 for 2555 Fo > 4sig(Fo) and 0.0719 for all 3958 data REM 161 parameters refined using 0 restraints END WGHT 0.0588 0.0000 REM Highest difference peak 0.357, deepest hole -0.278, 1-sigma level 0.055 Q1 1 0.7526 -0.1329 0.9767 11.00000 0.05 0.36 Q2 1 0.6980 0.0990 0.7576 11.00000 0.05 0.32 Q3 1 0.8546 0.1454 0.7447 11.00000 0.05 0.30 Q4 1 0.7325 -0.3050 0.9786 11.00000 0.05 0.29 Q5 1 0.8920 0.2961 0.7232 11.00000 0.05 0.28 Q6 1 0.6610 0.2710 0.7534 11.00000 0.05 0.26 Q7 1 0.7432 -0.0780 0.8982 11.00000 0.05 0.25 Q8 1 0.8632 0.0945 0.8170 11.00000 0.05 0.23 Q9 1 0.7561 -0.4408 1.0054 11.00000 0.05 0.22 Q10 1 0.8003 -0.2903 1.0852 11.00000 0.05 0.22 Q11 1 0.5835 0.1262 0.6621 11.00000 0.05 0.21 Q12 1 0.8074 0.3081 0.6083 11.00000 0.05 0.21 Q13 1 0.7959 -0.2938 0.9772 11.00000 0.05 0.20 Q14 1 0.5860 -0.1032 1.1184 11.00000 0.05 0.20 Q15 1 0.6021 0.2440 0.7405 11.00000 0.05 0.20 Q16 1 0.6446 0.4180 0.8769 11.00000 0.05 0.20 Q17 1 0.8051 -0.1192 1.0331 11.00000 0.05 0.20 Q18 1 0.9626 0.1437 0.8775 11.00000 0.05 0.20 Q19 1 0.9182 0.1687 0.6250 11.00000 0.05 0.19 Q20 1 0.7276 0.2524 0.6877 11.00000 0.05 0.19 ; _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^)+(0.0588P)^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 3958 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1084 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _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 C1 C 0.55433(17) 0.0834(3) 0.6305(2) 0.0484(6) Uani 1 1 d . . . H1A H 0.5171 0.0530 0.6912 0.073 Uiso 1 1 calc R . . H1B H 0.5774 0.0109 0.5889 0.073 Uiso 1 1 calc R . . H1C H 0.5167 0.1369 0.5767 0.073 Uiso 1 1 calc R . . C2 C 0.60732(19) 0.3120(3) 0.7797(2) 0.0507(7) Uani 1 1 d . . . H2A H 0.6581 0.3669 0.8084 0.076 Uiso 1 1 calc R . . H2B H 0.5764 0.2785 0.8450 0.076 Uiso 1 1 calc R . . H2C H 0.5636 0.3609 0.7295 0.076 Uiso 1 1 calc R . . C03 C 0.73400(16) 0.2370(2) 0.59077(17) 0.0375(5) Uani 1 1 d . . . H03A H 0.7304 0.1837 0.5206 0.045 Uiso 1 1 calc R . . H03B H 0.7193 0.3255 0.5682 0.045 Uiso 1 1 calc R . . C3 C 0.94145(19) 0.1680(3) 0.5769(2) 0.0486(6) Uani 1 1 d . . . H3A H 0.9460 0.2253 0.5115 0.073 Uiso 1 1 calc R . . H3B H 0.9252 0.0829 0.5485 0.073 Uiso 1 1 calc R . . H3C H 1.0005 0.1649 0.6228 0.073 Uiso 1 1 calc R . . C4 C 0.88635(18) 0.3817(2) 0.7356(2) 0.0444(6) Uani 1 1 d . . . H4A H 0.9458 0.3721 0.7796 0.067 Uiso 1 1 calc R . . H4B H 0.8404 0.4091 0.7873 0.067 Uiso 1 1 calc R . . H4C H 0.8914 0.4453 0.6751 0.067 Uiso 1 1 calc R . . C5 C 0.82811(14) 0.10576(19) 0.78254(14) 0.0253(4) Uani 1 1 d . . . C6 C 0.73429(14) 0.0769(2) 0.79243(15) 0.0267(4) Uani 1 1 d . . . C7 C 0.71154(14) -0.0173(2) 0.86997(16) 0.0283(4) Uani 1 1 d . . . H7 H 0.6487 -0.0365 0.8760 0.034 Uiso 1 1 calc R . . C8 C 0.77808(14) -0.0847(2) 0.93925(14) 0.0263(4) Uani 1 1 d . . . C9 C 0.87005(15) -0.0517(2) 0.92945(16) 0.0290(5) Uani 1 1 d . . . H9 H 0.9166 -0.0938 0.9764 0.035 Uiso 1 1 calc R . . C10 C 0.89492(14) 0.0406(2) 0.85323(15) 0.0282(4) Uani 1 1 d . . . H10 H 0.9579 0.0601 0.8486 0.034 Uiso 1 1 calc R . . C11 C 0.6385(2) -0.1798(3) 1.1023(2) 0.0556(7) Uani 1 1 d . . . H11A H 0.6213 -0.2506 1.1506 0.083 Uiso 1 1 calc R . . H11B H 0.5894 -0.1641 1.0419 0.083 Uiso 1 1 calc R . . H11C H 0.6484 -0.1038 1.1499 0.083 Uiso 1 1 calc R . . C12 C 0.7294(2) -0.3659(3) 0.9440(2) 0.0573(8) Uani 1 1 d . . . H12A H 0.7124 -0.4368 0.9922 0.086 Uiso 1 1 calc R . . H12B H 0.7865 -0.3862 0.9093 0.086 Uiso 1 1 calc R . . H12C H 0.6806 -0.3510 0.8830 0.086 Uiso 1 1 calc R . . C13 C 0.84091(19) -0.2509(3) 1.1484(2) 0.0504(7) Uani 1 1 d . . . H13A H 0.8542 -0.1733 1.1928 0.076 Uiso 1 1 calc R . . H13B H 0.8959 -0.2777 1.1121 0.076 Uiso 1 1 calc R . . H13C H 0.8223 -0.3179 1.1999 0.076 Uiso 1 1 calc R . . Si1 Si 0.65299(4) 0.17750(6) 0.69639(5) 0.02988(15) Uani 1 1 d . . . Si2 Si 0.85095(4) 0.22683(6) 0.66866(4) 0.03001(15) Uani 1 1 d . . . Si3 Si 0.74634(4) -0.22001(6) 1.03477(4) 0.03257(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0443(14) 0.0474(18) 0.0510(14) 0.0017(12) -0.0118(11) -0.0035(11) C2 0.0593(17) 0.0431(18) 0.0488(13) -0.0036(11) -0.0011(12) 0.0151(12) C03 0.0492(14) 0.0353(15) 0.0271(9) 0.0098(9) -0.0034(9) -0.0011(10) C3 0.0565(16) 0.0540(18) 0.0373(11) 0.0069(11) 0.0160(11) -0.0020(12) C4 0.0570(16) 0.0317(15) 0.0439(12) 0.0058(10) -0.0008(11) -0.0108(11) C5 0.0340(11) 0.0213(12) 0.0207(8) 0.0000(7) 0.0018(7) 0.0000(8) C6 0.0340(11) 0.0246(12) 0.0214(8) -0.0012(7) 0.0008(7) 0.0002(8) C7 0.0360(11) 0.0237(12) 0.0253(8) 0.0028(7) 0.0034(8) -0.0015(8) C8 0.0370(11) 0.0222(12) 0.0197(8) -0.0005(7) 0.0025(7) 0.0007(8) C9 0.0380(12) 0.0251(12) 0.0231(9) 0.0017(7) -0.0035(8) 0.0027(8) C10 0.0333(11) 0.0271(13) 0.0242(9) 0.0004(7) 0.0015(8) -0.0009(8) C11 0.0666(18) 0.055(2) 0.0486(14) 0.0116(12) 0.0238(13) -0.0013(13) C12 0.094(2) 0.0333(17) 0.0462(13) -0.0056(11) 0.0138(14) -0.0144(14) C13 0.0668(18) 0.0450(18) 0.0387(12) 0.0201(11) -0.0012(12) -0.0018(12) Si1 0.0351(3) 0.0256(3) 0.0280(3) 0.0029(2) -0.0036(2) 0.0017(2) Si2 0.0391(3) 0.0273(4) 0.0237(2) 0.0052(2) 0.0031(2) -0.0034(2) Si3 0.0488(4) 0.0253(4) 0.0242(2) 0.0043(2) 0.0061(2) -0.0021(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 C1 Si1 1.867(2) . ? C2 Si1 1.873(3) . ? C03 Si2 1.876(2) . ? C03 Si1 1.882(2) . ? C3 Si2 1.872(3) . ? C4 Si2 1.868(3) . ? C5 C10 1.407(3) . ? C5 C6 1.420(3) . ? C5 Si2 1.891(2) . ? C6 C7 1.401(3) . ? C6 Si1 1.894(2) . ? C7 C8 1.408(3) . ? C8 C9 1.404(3) . ? C8 Si3 1.891(2) . ? C9 C10 1.386(3) . ? C11 Si3 1.866(3) . ? C12 Si3 1.873(3) . ? C13 Si3 1.867(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si2 C03 Si1 105.22(10) . . ? C10 C5 C6 118.65(18) . . ? C10 C5 Si2 126.00(16) . . ? C6 C5 Si2 115.31(14) . . ? C7 C6 C5 119.02(18) . . ? C7 C6 Si1 127.51(16) . . ? C5 C6 Si1 113.46(15) . . ? C6 C7 C8 122.64(19) . . ? C9 C8 C7 116.90(18) . . ? C9 C8 Si3 121.13(15) . . ? C7 C8 Si3 121.88(16) . . ? C10 C9 C8 121.90(18) . . ? C9 C10 C5 120.86(19) . . ? C1 Si1 C2 108.69(13) . . ? C1 Si1 C03 114.56(11) . . ? C2 Si1 C03 110.74(13) . . ? C1 Si1 C6 111.95(11) . . ? C2 Si1 C6 110.65(10) . . ? C03 Si1 C6 100.05(10) . . ? C4 Si2 C3 110.09(13) . . ? C4 Si2 C03 111.36(12) . . ? C3 Si2 C03 113.75(11) . . ? C4 Si2 C5 110.98(10) . . ? C3 Si2 C5 110.35(11) . . ? C03 Si2 C5 99.96(10) . . ? C11 Si3 C13 110.20(12) . . ? C11 Si3 C12 110.24(15) . . ? C13 Si3 C12 108.30(14) . . ? C11 Si3 C8 109.33(12) . . ? C13 Si3 C8 110.25(11) . . ? C12 Si3 C8 108.50(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 C5 C6 C7 -1.5(3) . . . . ? Si2 C5 C6 C7 176.27(15) . . . . ? C10 C5 C6 Si1 177.47(15) . . . . ? Si2 C5 C6 Si1 -4.76(19) . . . . ? C5 C6 C7 C8 0.2(3) . . . . ? Si1 C6 C7 C8 -178.58(15) . . . . ? C6 C7 C8 C9 1.3(3) . . . . ? C6 C7 C8 Si3 -175.18(15) . . . . ? C7 C8 C9 C10 -1.6(3) . . . . ? Si3 C8 C9 C10 174.91(15) . . . . ? C8 C9 C10 C5 0.4(3) . . . . ? C6 C5 C10 C9 1.2(3) . . . . ? Si2 C5 C10 C9 -176.27(15) . . . . ? Si2 C03 Si1 C1 -143.52(12) . . . . ? Si2 C03 Si1 C2 93.12(14) . . . . ? Si2 C03 Si1 C6 -23.63(13) . . . . ? C7 C6 Si1 C1 -40.9(2) . . . . ? C5 C6 Si1 C1 140.19(16) . . . . ? C7 C6 Si1 C2 80.5(2) . . . . ? C5 C6 Si1 C2 -98.40(17) . . . . ? C7 C6 Si1 C03 -162.71(19) . . . . ? C5 C6 Si1 C03 18.42(16) . . . . ? Si1 C03 Si2 C4 -95.91(14) . . . . ? Si1 C03 Si2 C3 139.00(13) . . . . ? Si1 C03 Si2 C5 21.42(13) . . . . ? C10 C5 Si2 C4 -75.9(2) . . . . ? C6 C5 Si2 C4 106.49(17) . . . . ? C10 C5 Si2 C3 46.4(2) . . . . ? C6 C5 Si2 C3 -131.20(16) . . . . ? C10 C5 Si2 C03 166.46(18) . . . . ? C6 C5 Si2 C03 -11.11(17) . . . . ? C9 C8 Si3 C11 144.11(18) . . . . ? C7 C8 Si3 C11 -39.6(2) . . . . ? C9 C8 Si3 C13 22.8(2) . . . . ? C7 C8 Si3 C13 -160.85(17) . . . . ? C9 C8 Si3 C12 -95.63(19) . . . . ? C7 C8 Si3 C12 80.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.357 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.055 data_glu07f _database_code_depnum_ccdc_archive 'CCDC 837998' #TrackingRef 'analogues_of_ec23.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H24 O Si3' _chemical_formula_sum 'C13 H24 O Si3' _chemical_formula_weight 280.59 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.2270(8) _cell_length_b 10.0764(18) _cell_length_c 14.0512(19) _cell_angle_alpha 90.00 _cell_angle_beta 91.347(16) _cell_angle_gamma 90.00 _cell_volume 881.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3052 _cell_measurement_theta_min 7.2 _cell_measurement_theta_max 27.05 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max .5 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.057 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 304 _exptl_absorpt_coefficient_mu 0.256 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate_Stoe-IPDS _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11609 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 29.52 _reflns_number_total 4562 _reflns_number_gt 3705 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. TITL glu07b in P2(1) CELL 0.71073 6.2270 10.0764 14.0512 90.000 91.347 90.000 ZERR 2. 0.0008 0.0018 0.0019 0.000 0.016 0.000 REM CELL 0.71073 6.2273 10.0783 14.0507 90.000 91.385 90.000 REM ZERR 4.00 0.0012 0.0020 0.0028 0.000 0.030 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H O Si UNIT 26 48 2 6 L.S. 12 TEMP -100 ACTA CONF HTAB 2.5 BOND FMAP 2 PLAN 20 WGHT 0.077770 FVAR 0.54989 0.42934 0.06738 MOLE 1 C1 1 0.527965 0.088930 0.298808 11.00000 0.06192 0.04775 = 0.05043 0.00660 -0.00122 0.01917 AFIX 137 H1A 2 0.585140 -0.000317 0.288153 11.00000 -1.50000 H1B 2 0.459564 0.092146 0.360871 11.00000 -1.50000 H1C 2 0.645452 0.153577 0.297627 11.00000 -1.50000 AFIX 0 C2 1 0.116050 0.000598 0.201383 11.00000 0.05891 0.04012 = 0.06529 -0.01059 0.02145 -0.01186 AFIX 137 H2A 2 0.010520 0.022086 0.150878 11.00000 -1.50000 H2B 2 0.044753 -0.001887 0.262796 11.00000 -1.50000 H2C 2 0.180088 -0.086245 0.188596 11.00000 -1.50000 AFIX 0 C3 1 0.740490 0.357447 0.046122 11.00000 0.04133 0.04468 = 0.04534 0.00270 0.00007 -0.00649 AFIX 137 H3A 2 0.805208 0.357234 0.110374 11.00000 -1.50000 H3B 2 0.738930 0.448217 0.021070 11.00000 -1.50000 H3C 2 0.824792 0.300500 0.004555 11.00000 -1.50000 AFIX 0 C4 1 0.343807 0.291608 -0.070506 11.00000 0.03710 0.05341 = 0.03818 -0.00540 -0.00414 0.00557 AFIX 137 H4A 2 0.441908 0.246510 -0.113408 11.00000 -1.50000 H4B 2 0.320003 0.382860 -0.092456 11.00000 -1.50000 H4C 2 0.206428 0.244179 -0.070204 11.00000 -1.50000 AFIX 0 C5 1 0.288074 0.385057 0.140267 11.00000 0.02729 0.02726 = 0.03203 -0.00022 -0.00139 -0.00134 C6 1 0.220320 0.302154 0.217071 11.00000 0.03040 0.02590 = 0.02886 -0.00203 -0.00120 0.00174 C7 1 0.083602 0.355178 0.289091 11.00000 0.03960 0.02639 = 0.02927 -0.00108 0.00116 0.00581 AFIX 43 H7 2 0.037453 0.298344 0.338529 11.00000 -1.20000 AFIX 0 C8 1 0.016716 0.487498 0.288556 11.00000 0.04055 0.02850 = 0.03152 -0.00382 -0.00327 0.00627 C9 1 0.087404 0.567151 0.211737 11.00000 0.04603 0.02366 = 0.03840 -0.00179 -0.00171 0.00484 AFIX 43 H9 2 0.044680 0.657614 0.209206 11.00000 -1.20000 AFIX 0 C10 1 0.218464 0.517513 0.139010 11.00000 0.04055 0.02456 = 0.03611 0.00337 0.00386 -0.00169 AFIX 43 H10 2 0.259828 0.574447 0.088763 11.00000 -1.20000 AFIX 0 PART 1 ISOR .005 C11 C11B C12 C12B C13 C13B SAME Si3B C11B C12B C13B SAME Si3 C11 C13 C12 EADP Si3 Si3B EXYZ Si3 Si3B SI3 4 -0.159250 0.554316 0.388879 21.00000 0.05150 0.03278 = 0.03460 -0.00709 0.00384 0.01054 C11 1 -0.395624 0.451567 0.405531 21.00000 0.06105 0.07607 = 0.06098 -0.02214 -0.00056 0.00010 AFIX 137 H11A 2 -0.353539 0.357853 0.406527 21.00000 -1.50000 H11B 2 -0.499108 0.466879 0.353054 21.00000 -1.50000 H11C 2 -0.461562 0.474618 0.465980 21.00000 -1.50000 AFIX 0 C12 1 -0.217050 0.733111 0.367085 21.00000 0.08240 0.06333 = 0.07512 -0.00600 0.02117 0.02667 AFIX 137 H12A 2 -0.321084 0.764645 0.413208 21.00000 -1.50000 H12B 2 -0.276646 0.744489 0.302428 21.00000 -1.50000 H12C 2 -0.083853 0.784344 0.374143 21.00000 -1.50000 AFIX 0 C13 1 0.015829 0.547845 0.501261 21.00000 0.05670 0.05807 = 0.03714 -0.01293 -0.00201 -0.00256 AFIX 137 H13A 2 0.152575 0.592632 0.489944 21.00000 -1.50000 H13B 2 0.043144 0.455091 0.518679 21.00000 -1.50000 H13C 2 -0.057872 0.592472 0.553162 21.00000 -1.50000 PART 2 AFIX 0 SI3B 4 -0.159250 0.554316 0.388879 -21.00000 0.05150 0.03278 = 0.03460 -0.00709 0.00384 0.01054 C11B 1 -0.357562 0.421259 0.430917 -21.00000 0.05452 0.05843 = 0.06829 -0.01382 0.02122 0.00169 AFIX 137 H11D 2 -0.277365 0.344441 0.455570 -21.00000 -1.50000 H11E 2 -0.450379 0.393540 0.377241 -21.00000 -1.50000 H11F 2 -0.445900 0.458058 0.481340 -21.00000 -1.50000 AFIX 0 C12B 1 -0.332373 0.695770 0.346299 -21.00000 0.07739 0.06744 = 0.07545 0.01074 0.02042 0.03356 AFIX 137 H12D 2 -0.401967 0.736872 0.400754 -21.00000 -1.50000 H12E 2 -0.442301 0.662513 0.301294 -21.00000 -1.50000 H12F 2 -0.243261 0.761795 0.314611 -21.00000 -1.50000 AFIX 0 C13B 1 0.009807 0.605350 0.487430 -21.00000 0.08013 0.08197 = 0.06696 -0.02368 0.00503 -0.00457 AFIX 137 H13D 2 0.127085 0.660518 0.464168 -21.00000 -1.50000 H13E 2 0.069627 0.526817 0.519522 -21.00000 -1.50000 H13F 2 -0.074987 0.656580 0.532409 -21.00000 -1.50000 PART 0 AFIX 0 O1 3 0.454199 0.143716 0.099861 11.00000 0.04200 0.02798 = 0.03924 -0.00419 0.00739 0.00263 SI1 4 0.329363 0.128899 0.204935 11.00000 0.03744 0.02300 = 0.03599 -0.00086 0.00567 0.00236 SI2 4 0.462142 0.294005 0.050589 11.00000 0.02810 0.02983 = 0.02973 -0.00156 0.00147 -0.00041 HKLF 4 1 1 0 0 0 -1 0 0 0 -1 REM glu07b in P2(1) REM R1 = 0.0433 for 3705 Fo > 4sig(Fo) and 0.0585 for all 4562 data REM 193 parameters refined using 51 restraints END WGHT 0.0777 0.0000 REM Highest difference peak 0.365, deepest hole -0.381, 1-sigma level 0.061 Q1 1 0.6382 0.3096 0.0785 11.00000 0.05 0.37 Q2 1 0.3065 0.2941 -0.0008 11.00000 0.05 0.30 Q3 1 0.3658 0.3579 0.0995 11.00000 0.05 0.29 Q4 1 -0.3182 0.5432 0.3449 11.00000 0.05 0.27 Q5 1 0.6050 0.3129 0.0069 11.00000 0.05 0.27 Q6 1 0.3111 0.2918 0.1059 11.00000 0.05 0.26 Q7 1 0.1628 0.1106 0.1670 11.00000 0.05 0.25 Q8 1 0.5497 0.1073 0.0825 11.00000 0.05 0.25 Q9 1 0.0110 0.5735 0.4242 11.00000 0.05 0.24 Q10 1 -0.0651 0.5372 0.3031 11.00000 0.05 0.24 Q11 1 -0.3183 0.5325 0.4263 11.00000 0.05 0.24 Q12 1 -0.0121 0.5565 0.3479 11.00000 0.05 0.24 Q13 1 0.1671 0.1365 0.2572 11.00000 0.05 0.24 Q14 1 0.2388 0.0483 0.2256 11.00000 0.05 0.24 Q15 1 -0.0103 0.5440 0.4356 11.00000 0.05 0.23 Q16 1 -0.0732 0.5095 0.3235 11.00000 0.05 0.23 Q17 1 -0.1364 0.7511 0.3941 11.00000 0.05 0.22 Q18 1 0.2582 0.3386 0.1756 11.00000 0.05 0.22 Q19 1 0.9960 0.1270 0.0194 11.00000 0.05 0.22 Q20 1 0.5441 0.3925 0.0387 11.00000 0.05 0.21 ; _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^)+(0.0778P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(13) _refine_ls_number_reflns 4562 _refine_ls_number_parameters 193 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1232 _refine_ls_wR_factor_gt 0.1094 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.083 _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 C1 C 0.5280(6) 0.0889(3) 0.2988(2) 0.0534(8) Uani 1 1 d . . . H1A H 0.5851 -0.0003 0.2882 0.080 Uiso 1 1 calc R . . H1B H 0.4596 0.0921 0.3609 0.080 Uiso 1 1 calc R . . H1C H 0.6455 0.1536 0.2976 0.080 Uiso 1 1 calc R . . C2 C 0.1161(6) 0.0006(3) 0.2014(3) 0.0545(8) Uani 1 1 d . . . H2A H 0.0105 0.0221 0.1509 0.082 Uiso 1 1 calc R . . H2B H 0.0448 -0.0019 0.2628 0.082 Uiso 1 1 calc R . . H2C H 0.1801 -0.0862 0.1886 0.082 Uiso 1 1 calc R . . C3 C 0.7405(5) 0.3574(3) 0.0461(2) 0.0438(6) Uani 1 1 d . A . H3A H 0.8052 0.3572 0.1104 0.066 Uiso 1 1 calc R . . H3B H 0.7389 0.4482 0.0211 0.066 Uiso 1 1 calc R . . H3C H 0.8248 0.3005 0.0046 0.066 Uiso 1 1 calc R . . C4 C 0.3438(5) 0.2916(3) -0.07051(18) 0.0430(6) Uani 1 1 d . A . H4A H 0.4419 0.2465 -0.1134 0.064 Uiso 1 1 calc R . . H4B H 0.3200 0.3829 -0.0925 0.064 Uiso 1 1 calc R . . H4C H 0.2064 0.2442 -0.0702 0.064 Uiso 1 1 calc R . . C5 C 0.2881(4) 0.3851(2) 0.14027(15) 0.0289(5) Uani 1 1 d . A . C6 C 0.2203(4) 0.3022(2) 0.21707(15) 0.0284(4) Uani 1 1 d . . . C7 C 0.0836(5) 0.3552(2) 0.28909(16) 0.0317(5) Uani 1 1 d . A . H7 H 0.0375 0.2983 0.3385 0.038 Uiso 1 1 calc R . . C8 C 0.0167(5) 0.4875(2) 0.28856(17) 0.0336(5) Uani 1 1 d . . . C9 C 0.0874(5) 0.5672(3) 0.21174(17) 0.0361(6) Uani 1 1 d . A . H9 H 0.0447 0.6576 0.2092 0.043 Uiso 1 1 calc R . . C10 C 0.2185(4) 0.5175(2) 0.13901(18) 0.0337(5) Uani 1 1 d . . . H10 H 0.2598 0.5744 0.0888 0.040 Uiso 1 1 calc R A . Si3 Si -0.15925(14) 0.55432(7) 0.38888(5) 0.0396(2) Uani 0.429(18) 1 d PD A 1 C11 C -0.396(2) 0.4516(15) 0.4055(10) 0.066(3) Uani 0.429(18) 1 d PDU A 1 H11A H -0.3535 0.3579 0.4065 0.099 Uiso 0.429(18) 1 calc PR A 1 H11B H -0.4991 0.4669 0.3531 0.099 Uiso 0.429(18) 1 calc PR A 1 H11C H -0.4616 0.4746 0.4660 0.099 Uiso 0.429(18) 1 calc PR A 1 C12 C -0.217(3) 0.7331(10) 0.3671(9) 0.073(3) Uani 0.429(18) 1 d PDU A 1 H12A H -0.3211 0.7646 0.4132 0.110 Uiso 0.429(18) 1 calc PR A 1 H12B H -0.2766 0.7445 0.3024 0.110 Uiso 0.429(18) 1 calc PR A 1 H12C H -0.0839 0.7843 0.3741 0.110 Uiso 0.429(18) 1 calc PR A 1 C13 C 0.0158(17) 0.5478(14) 0.5013(6) 0.051(2) Uani 0.429(18) 1 d PDU A 1 H13A H 0.1526 0.5926 0.4899 0.076 Uiso 0.429(18) 1 calc PR A 1 H13B H 0.0431 0.4551 0.5187 0.076 Uiso 0.429(18) 1 calc PR A 1 H13C H -0.0579 0.5925 0.5532 0.076 Uiso 0.429(18) 1 calc PR A 1 Si3B Si -0.15925(14) 0.55432(7) 0.38888(5) 0.0396(2) Uani 0.571(18) 1 d PD A 2 C11B C -0.3576(15) 0.4213(9) 0.4309(8) 0.060(2) Uani 0.571(18) 1 d PDU A 2 H11D H -0.2774 0.3444 0.4556 0.090 Uiso 0.571(18) 1 calc PR A 2 H11E H -0.4504 0.3935 0.3772 0.090 Uiso 0.571(18) 1 calc PR A 2 H11F H -0.4459 0.4581 0.4813 0.090 Uiso 0.571(18) 1 calc PR A 2 C12B C -0.332(2) 0.6958(10) 0.3463(6) 0.073(3) Uani 0.571(18) 1 d PDU A 2 H12D H -0.4020 0.7369 0.4008 0.110 Uiso 0.571(18) 1 calc PR A 2 H12E H -0.4423 0.6625 0.3013 0.110 Uiso 0.571(18) 1 calc PR A 2 H12F H -0.2433 0.7618 0.3146 0.110 Uiso 0.571(18) 1 calc PR A 2 C13B C 0.0098(17) 0.6054(15) 0.4874(7) 0.076(3) Uani 0.571(18) 1 d PDU A 2 H13D H 0.1271 0.6605 0.4642 0.114 Uiso 0.571(18) 1 calc PR A 2 H13E H 0.0696 0.5268 0.5195 0.114 Uiso 0.571(18) 1 calc PR A 2 H13F H -0.0750 0.6566 0.5324 0.114 Uiso 0.571(18) 1 calc PR A 2 O1 O 0.4542(3) 0.14372(17) 0.09986(12) 0.0363(4) Uani 1 1 d . A . Si1 Si 0.32936(12) 0.12890(6) 0.20494(4) 0.03207(16) Uani 1 1 d . . . Si2 Si 0.46214(11) 0.29401(6) 0.05059(4) 0.02921(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.062(2) 0.0478(17) 0.0504(15) 0.0066(12) -0.0012(14) 0.0192(15) C2 0.059(2) 0.0401(15) 0.0653(19) -0.0106(13) 0.0214(16) -0.0119(15) C3 0.0413(17) 0.0447(15) 0.0453(14) 0.0027(11) 0.0001(12) -0.0065(12) C4 0.0371(15) 0.0534(15) 0.0382(12) -0.0054(12) -0.0041(10) 0.0056(14) C5 0.0273(13) 0.0273(11) 0.0320(11) -0.0002(8) -0.0014(9) -0.0013(9) C6 0.0304(12) 0.0259(10) 0.0289(9) -0.0020(8) -0.0012(8) 0.0017(10) C7 0.0396(15) 0.0264(11) 0.0293(10) -0.0011(8) 0.0012(9) 0.0058(10) C8 0.0405(15) 0.0285(11) 0.0315(11) -0.0038(8) -0.0033(9) 0.0063(10) C9 0.0460(16) 0.0237(11) 0.0384(12) -0.0018(9) -0.0017(10) 0.0048(11) C10 0.0405(15) 0.0246(11) 0.0361(12) 0.0034(8) 0.0039(10) -0.0017(10) Si3 0.0515(5) 0.0328(3) 0.0346(3) -0.0071(3) 0.0038(3) 0.0105(3) C11 0.061(5) 0.076(5) 0.061(5) -0.022(4) -0.001(4) 0.000(4) C12 0.082(6) 0.063(4) 0.075(5) -0.006(3) 0.021(4) 0.027(4) C13 0.057(4) 0.058(4) 0.037(3) -0.013(3) -0.002(3) -0.003(3) Si3B 0.0515(5) 0.0328(3) 0.0346(3) -0.0071(3) 0.0038(3) 0.0105(3) C11B 0.055(4) 0.058(4) 0.068(4) -0.014(3) 0.021(3) 0.002(3) C12B 0.077(5) 0.067(4) 0.075(4) 0.011(3) 0.020(3) 0.034(3) C13B 0.080(4) 0.082(5) 0.067(4) -0.024(4) 0.005(3) -0.005(4) O1 0.0420(11) 0.0280(8) 0.0392(8) -0.0042(7) 0.0074(7) 0.0026(8) Si1 0.0374(4) 0.0230(3) 0.0360(3) -0.0009(2) 0.0057(3) 0.0024(3) Si2 0.0281(3) 0.0298(3) 0.0297(3) -0.0016(2) 0.0015(2) -0.0004(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 C1 Si1 1.832(3) . ? C2 Si1 1.853(3) . ? C3 Si2 1.850(3) . ? C4 Si2 1.838(3) . ? C5 C10 1.403(3) . ? C5 C6 1.436(3) . ? C5 Si2 1.915(2) . ? C6 C7 1.440(3) . ? C6 Si1 1.882(3) . ? C7 C8 1.397(3) . ? C8 C9 1.423(4) . ? C8 Si3 1.927(3) . ? C9 C10 1.414(4) . ? Si3 C11 1.819(11) . ? Si3 C12 1.861(9) . ? Si3 C13 1.899(8) . ? O1 Si2 1.6664(19) . ? O1 Si1 1.6913(18) . ? 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 C10 C5 C6 117.8(2) . . ? C10 C5 Si2 128.81(18) . . ? C6 C5 Si2 113.37(17) . . ? C5 C6 C7 120.1(2) . . ? C5 C6 Si1 111.01(17) . . ? C7 C6 Si1 128.91(18) . . ? C8 C7 C6 122.1(2) . . ? C7 C8 C9 116.4(2) . . ? C7 C8 Si3 120.28(19) . . ? C9 C8 Si3 123.30(19) . . ? C10 C9 C8 122.9(2) . . ? C5 C10 C9 120.7(2) . . ? C11 Si3 C12 114.7(6) . . ? C11 Si3 C13 108.9(5) . . ? C12 Si3 C13 106.0(6) . . ? C11 Si3 C8 111.8(4) . . ? C12 Si3 C8 109.2(4) . . ? C13 Si3 C8 105.7(4) . . ? Si2 O1 Si1 117.50(10) . . ? O1 Si1 C1 109.37(13) . . ? O1 Si1 C2 112.45(12) . . ? C1 Si1 C2 109.72(17) . . ? O1 Si1 C6 99.87(9) . . ? C1 Si1 C6 112.18(12) . . ? C2 Si1 C6 112.93(15) . . ? O1 Si2 C4 110.94(13) . . ? O1 Si2 C3 111.42(12) . . ? C4 Si2 C3 109.19(13) . . ? O1 Si2 C5 98.00(9) . . ? C4 Si2 C5 113.23(12) . . ? C3 Si2 C5 113.70(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 C5 C6 C7 0.6(3) . . . . ? Si2 C5 C6 C7 -178.36(18) . . . . ? C10 C5 C6 Si1 179.64(18) . . . . ? Si2 C5 C6 Si1 0.7(2) . . . . ? C5 C6 C7 C8 -1.5(4) . . . . ? Si1 C6 C7 C8 179.6(2) . . . . ? C6 C7 C8 C9 1.2(4) . . . . ? C6 C7 C8 Si3 -178.15(19) . . . . ? C7 C8 C9 C10 0.0(4) . . . . ? Si3 C8 C9 C10 179.3(2) . . . . ? C6 C5 C10 C9 0.5(4) . . . . ? Si2 C5 C10 C9 179.30(18) . . . . ? C8 C9 C10 C5 -0.8(4) . . . . ? C7 C8 Si3 C11 -52.4(6) . . . . ? C9 C8 Si3 C11 128.2(6) . . . . ? C7 C8 Si3 C12 179.5(7) . . . . ? C9 C8 Si3 C12 0.2(7) . . . . ? C7 C8 Si3 C13 65.9(5) . . . . ? C9 C8 Si3 C13 -113.4(5) . . . . ? Si2 O1 Si1 C1 -112.47(15) . . . . ? Si2 O1 Si1 C2 125.38(17) . . . . ? Si2 O1 Si1 C6 5.40(14) . . . . ? C5 C6 Si1 O1 -3.42(18) . . . . ? C7 C6 Si1 O1 175.5(2) . . . . ? C5 C6 Si1 C1 112.3(2) . . . . ? C7 C6 Si1 C1 -68.7(3) . . . . ? C5 C6 Si1 C2 -123.05(19) . . . . ? C7 C6 Si1 C2 55.9(3) . . . . ? Si1 O1 Si2 C4 -123.67(14) . . . . ? Si1 O1 Si2 C3 114.45(15) . . . . ? Si1 O1 Si2 C5 -4.97(14) . . . . ? C10 C5 Si2 O1 -176.5(2) . . . . ? C6 C5 Si2 O1 2.37(19) . . . . ? C10 C5 Si2 C4 -59.5(3) . . . . ? C6 C5 Si2 C4 119.32(19) . . . . ? C10 C5 Si2 C3 65.9(3) . . . . ? C6 C5 Si2 C3 -115.30(19) . . . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 29.52 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.365 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.061 data_glu12ad _database_code_depnum_ccdc_archive 'CCDC 837999' #TrackingRef 'analogues_of_ec23.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H20 O2 Si2' _chemical_formula_sum 'C13 H20 O2 Si2' _chemical_formula_weight 264.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 12.8871(17) _cell_length_b 8.8099(11) _cell_length_c 14.4156(14) _cell_angle_alpha 90.00 _cell_angle_beta 116.374(12) _cell_angle_gamma 90.00 _cell_volume 1466.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4504 _cell_measurement_theta_min 7.15 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max .4 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 0.231 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate_Stoe_IPDS _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18328 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 29.25 _reflns_number_total 3938 _reflns_number_gt 3195 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. TITL glu12ac in P2(1)/c CELL 0.71073 12.8871 8.8099 14.4156 90.000 116.374 90.000 ZERR 4.0 0.0017 0.0011 0.0014 0.000 0.012 0.000 REM CELL 0.71073 12.9142 8.8097 14.4381 90.000 116.486 90.000 REM ZERR 4.00 0.0026 0.0018 0.0029 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O Si UNIT 52 80 8 8 ACTA TEMP -100 CONF HTAB 2.5 L.S. 12 BOND $H FMAP 2 PLAN 20 WGHT 0.076900 0.347400 FVAR 0.32093 C2A 1 0.285674 0.424760 0.948460 11.00000 0.06316 0.03262 = 0.04363 0.00152 0.01778 -0.00435 AFIX 137 H2A 2 0.331836 0.506917 0.993878 11.00000 0.08044 H2B 2 0.205325 0.433308 0.937834 11.00000 0.07877 H2C 2 0.288021 0.432144 0.881586 11.00000 0.10337 AFIX 0 C1A 1 0.491119 0.213785 1.010768 11.00000 0.04263 0.05593 = 0.05974 -0.01154 0.02776 -0.01433 AFIX 137 H1A 2 0.481051 0.203499 0.939561 11.00000 0.07024 H1B 2 0.528749 0.122506 1.050234 11.00000 0.06318 H1C 2 0.539423 0.302668 1.043149 11.00000 0.07209 AFIX 0 C4A 1 0.140356 -0.015335 1.146271 11.00000 0.04044 0.04487 = 0.03773 -0.00397 0.02117 -0.00150 AFIX 137 H4A 2 0.073170 -0.076066 1.100921 11.00000 0.05448 H4B 2 0.122396 0.092724 1.131828 11.00000 0.06461 H4C 2 0.159004 -0.036398 1.218736 11.00000 0.05979 AFIX 0 C3A 1 0.313855 -0.265166 1.163374 11.00000 0.03855 0.03757 = 0.03764 0.00672 0.01403 0.00086 AFIX 137 H3A 2 0.382407 -0.288339 1.153096 11.00000 0.05707 H3B 2 0.251010 -0.334877 1.121892 11.00000 0.06405 H3C 2 0.332691 -0.276983 1.236747 11.00000 0.05789 AFIX 0 C5A 1 0.218517 -0.045993 0.978353 11.00000 0.02685 0.03065 = 0.02538 -0.00071 0.01022 -0.00031 C6A 1 0.246213 0.079265 0.932098 11.00000 0.02989 0.02785 = 0.02560 -0.00206 0.01103 -0.00181 C7A 1 0.197252 0.086292 0.823725 11.00000 0.03316 0.02960 = 0.02608 -0.00125 0.01236 -0.00263 AFIX 43 H7 2 0.215191 0.169729 0.791652 11.00000 0.04287 AFIX 0 C8A 1 0.122683 -0.026866 0.762032 11.00000 0.02865 0.03043 = 0.02527 -0.00323 0.00972 0.00022 C9A 1 0.096665 -0.150922 0.807565 11.00000 0.03364 0.03269 = 0.02845 -0.00453 0.01030 -0.00526 AFIX 43 H9 2 0.046752 -0.228866 0.765931 11.00000 0.04358 AFIX 0 C10A 1 0.144632 -0.159161 0.914581 11.00000 0.03626 0.03192 = 0.02779 -0.00067 0.01232 -0.00698 AFIX 43 H10 2 0.126953 -0.243993 0.945700 11.00000 0.04180 AFIX 0 C11A 1 0.070342 -0.014517 0.647570 11.00000 0.02924 0.02917 = 0.02706 -0.00240 0.01013 0.00090 C03A 1 0.362069 0.230917 1.145053 11.00000 0.04009 0.03611 = 0.02889 -0.00628 0.01198 -0.00769 AFIX 23 H03A 2 0.424727 0.300912 1.189123 11.00000 0.04788 H03B 2 0.289210 0.266212 1.145203 11.00000 0.05428 AFIX 0 C04A 1 0.390176 0.069332 1.191498 11.00000 0.03703 0.04096 = 0.02622 -0.00020 0.00681 -0.00825 AFIX 23 H04A 2 0.407380 0.073534 1.265560 11.00000 0.06817 H04B 2 0.460102 0.031165 1.187085 11.00000 0.04824 AFIX 0 O1A 3 0.089493 0.101138 0.606439 11.00000 0.05258 0.03902 = 0.02721 0.00107 0.01272 -0.00396 O2A 3 0.006204 -0.125025 0.595398 11.00000 0.04893 0.04408 = 0.02632 -0.00617 0.00722 -0.00947 H2O 2 -0.028769 -0.110948 0.519922 11.00000 -1.50000 SI1A 4 0.346299 0.237995 1.009544 11.00000 0.03433 0.02979 = 0.02781 -0.00334 0.01212 -0.00698 SI2A 4 0.267018 -0.065368 1.122131 11.00000 0.02910 0.03208 = 0.02392 0.00037 0.00967 -0.00234 HKLF 4 REM glu12ac in P2(1)/c REM R1 = 0.0446 for 3195 Fo > 4sig(Fo) and 0.0541 for all 3938 data REM 180 parameters refined using 0 restraints END WGHT 0.0769 0.3474 REM Highest difference peak 0.382, deepest hole -0.403, 1-sigma level 0.055 Q1 1 0.2765 0.1489 0.9606 11.00000 0.05 0.38 Q2 1 0.3444 0.0172 1.1596 11.00000 0.05 0.32 Q3 1 0.2274 -0.0478 1.0321 11.00000 0.05 0.32 Q4 1 0.4401 0.2405 1.0143 11.00000 0.05 0.30 Q5 1 0.3101 -0.1786 1.1631 11.00000 0.05 0.30 Q6 1 0.1577 0.0257 0.7896 11.00000 0.05 0.27 Q7 1 0.3026 0.3326 0.9530 11.00000 0.05 0.26 Q8 1 0.1875 -0.0458 1.1455 11.00000 0.05 0.25 Q9 1 0.0675 0.0869 0.5569 11.00000 0.05 0.25 Q10 1 0.3422 0.2412 1.0915 11.00000 0.05 0.24 Q11 1 0.2183 -0.1310 1.0427 11.00000 0.05 0.24 Q12 1 0.2841 -0.0485 1.0490 11.00000 0.05 0.22 Q13 1 0.1011 -0.0689 0.7781 11.00000 0.05 0.21 Q14 1 0.4303 0.2275 1.0889 11.00000 0.05 0.20 Q15 1 0.1901 -0.1026 0.9566 11.00000 0.05 0.19 Q16 1 0.1017 -0.1461 0.8633 11.00000 0.05 0.18 Q17 1 0.2228 0.0955 0.8900 11.00000 0.05 0.18 Q18 1 0.1419 0.0868 0.9422 11.00000 0.05 0.18 Q19 1 0.3081 0.3584 1.0207 11.00000 0.05 0.18 Q20 1 0.3050 0.1876 1.0667 11.00000 0.05 0.18 ; _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^)+(0.0769P)^2^+0.3474P] 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 3938 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1252 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 C2A C 0.2857(2) 0.4248(2) 0.94846(16) 0.0487(4) Uani 1 1 d . . . H2A H 0.3318 0.5069 0.9939 0.080(10) Uiso 1 1 calc R . . H2B H 0.2053 0.4333 0.9378 0.079(10) Uiso 1 1 calc R . . H2C H 0.2880 0.4321 0.8816 0.103(12) Uiso 1 1 calc R . . C1A C 0.49112(18) 0.2138(3) 1.01077(18) 0.0509(5) Uani 1 1 d . . . H1A H 0.4811 0.2035 0.9396 0.070(8) Uiso 1 1 calc R . . H1B H 0.5287 0.1225 1.0502 0.063(8) Uiso 1 1 calc R . . H1C H 0.5394 0.3027 1.0431 0.072(8) Uiso 1 1 calc R . . C4A C 0.14036(15) -0.0153(2) 1.14627(14) 0.0396(4) Uani 1 1 d . . . H4A H 0.0732 -0.0761 1.1009 0.054(7) Uiso 1 1 calc R . . H4B H 0.1224 0.0927 1.1318 0.065(8) Uiso 1 1 calc R . . H4C H 0.1590 -0.0364 1.2187 0.060(7) Uiso 1 1 calc R . . C3A C 0.31385(15) -0.2652(2) 1.16337(14) 0.0390(4) Uani 1 1 d . . . H3A H 0.3824 -0.2883 1.1531 0.057(7) Uiso 1 1 calc R . . H3B H 0.2510 -0.3349 1.1219 0.064(8) Uiso 1 1 calc R . . H3C H 0.3327 -0.2770 1.2367 0.058(7) Uiso 1 1 calc R . . C5A C 0.21852(12) -0.04599(17) 0.97835(11) 0.0281(3) Uani 1 1 d . . . C6A C 0.24621(12) 0.07926(17) 0.93210(11) 0.0283(3) Uani 1 1 d . . . C7A C 0.19725(13) 0.08629(17) 0.82372(11) 0.0299(3) Uani 1 1 d . . . H7 H 0.2152 0.1697 0.7917 0.043(6) Uiso 1 1 calc R . . C8A C 0.12268(12) -0.02687(17) 0.76203(11) 0.0289(3) Uani 1 1 d . . . C9A C 0.09667(13) -0.15092(19) 0.80757(12) 0.0329(3) Uani 1 1 d . . . H9 H 0.0468 -0.2289 0.7659 0.044(6) Uiso 1 1 calc R . . C10A C 0.14463(13) -0.15916(18) 0.91458(12) 0.0327(3) Uani 1 1 d . . . H10 H 0.1270 -0.2440 0.9457 0.042(6) Uiso 1 1 calc R . . C11A C 0.07034(12) -0.01452(17) 0.64757(11) 0.0294(3) Uani 1 1 d . . . C03A C 0.36207(15) 0.23092(19) 1.14505(12) 0.0363(3) Uani 1 1 d . . . H03A H 0.4247 0.3009 1.1891 0.048(6) Uiso 1 1 calc R . . H03B H 0.2892 0.2662 1.1452 0.054(7) Uiso 1 1 calc R . . C04A C 0.39018(15) 0.0693(2) 1.19150(12) 0.0374(3) Uani 1 1 d . . . H04A H 0.4074 0.0735 1.2656 0.068(8) Uiso 1 1 calc R . . H04B H 0.4601 0.0312 1.1871 0.048(6) Uiso 1 1 calc R . . O1A O 0.08949(12) 0.10114(15) 0.60644(9) 0.0414(3) Uani 1 1 d . . . O2A O 0.00620(11) -0.12503(16) 0.59540(9) 0.0433(3) Uani 1 1 d . . . H2O H -0.029(2) -0.111(3) 0.520(2) 0.065 Uiso 1 1 d . . . Si1A Si 0.34630(4) 0.23799(5) 1.00954(3) 0.03126(13) Uani 1 1 d . . . Si2A Si 0.26702(3) -0.06537(5) 1.12213(3) 0.02914(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2A 0.0632(12) 0.0326(9) 0.0436(10) 0.0015(7) 0.0178(9) -0.0044(8) C1A 0.0426(9) 0.0559(12) 0.0597(12) -0.0115(10) 0.0278(9) -0.0143(9) C4A 0.0404(8) 0.0449(9) 0.0377(8) -0.0040(7) 0.0212(7) -0.0015(7) C3A 0.0385(8) 0.0376(8) 0.0376(8) 0.0067(7) 0.0140(7) 0.0009(6) C5A 0.0268(6) 0.0307(7) 0.0254(6) -0.0007(5) 0.0102(5) -0.0003(5) C6A 0.0299(6) 0.0279(7) 0.0256(6) -0.0021(5) 0.0110(5) -0.0018(5) C7A 0.0332(7) 0.0296(7) 0.0261(6) -0.0012(5) 0.0124(5) -0.0026(5) C8A 0.0286(6) 0.0304(7) 0.0253(6) -0.0032(5) 0.0097(5) 0.0002(5) C9A 0.0336(7) 0.0327(7) 0.0284(7) -0.0045(6) 0.0103(5) -0.0053(6) C10A 0.0363(7) 0.0319(7) 0.0278(7) -0.0007(5) 0.0123(6) -0.0070(6) C11A 0.0292(6) 0.0292(7) 0.0271(6) -0.0024(5) 0.0101(5) 0.0009(5) C03A 0.0401(8) 0.0361(8) 0.0289(7) -0.0063(6) 0.0120(6) -0.0077(6) C04A 0.0370(8) 0.0410(9) 0.0262(7) -0.0002(6) 0.0068(6) -0.0082(6) O1A 0.0526(7) 0.0390(6) 0.0272(5) 0.0011(5) 0.0127(5) -0.0040(5) O2A 0.0489(7) 0.0441(7) 0.0263(5) -0.0062(5) 0.0072(5) -0.0095(5) Si1A 0.0343(2) 0.0298(2) 0.0278(2) -0.00334(15) 0.01212(16) -0.00698(15) Si2A 0.0291(2) 0.0321(2) 0.02392(19) 0.00037(14) 0.00967(15) -0.00234(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 C2A Si1A 1.866(2) . ? C2A H2A 0.9800 . ? C2A H2B 0.9800 . ? C2A H2C 0.9800 . ? C1A Si1A 1.871(2) . ? C1A H1A 0.9800 . ? C1A H1B 0.9800 . ? C1A H1C 0.9800 . ? C4A Si2A 1.8667(18) . ? C4A H4A 0.9800 . ? C4A H4B 0.9800 . ? C4A H4C 0.9800 . ? C3A Si2A 1.8701(18) . ? C3A H3A 0.9800 . ? C3A H3B 0.9800 . ? C3A H3C 0.9800 . ? C5A C10A 1.403(2) . ? C5A C6A 1.415(2) . ? C5A Si2A 1.8880(15) . ? C6A C7A 1.402(2) . ? C6A Si1A 1.8937(15) . ? C7A C8A 1.396(2) . ? C7A H7 0.9500 . ? C8A C9A 1.390(2) . ? C8A C11A 1.483(2) . ? C9A C10A 1.386(2) . ? C9A H9 0.9500 . ? C10A H10 0.9500 . ? C11A O1A 1.257(2) . ? C11A O2A 1.2823(19) . ? C03A C04A 1.546(2) . ? C03A Si1A 1.8731(17) . ? C03A H03A 0.9900 . ? C03A H03B 0.9900 . ? C04A Si2A 1.8754(17) . ? C04A H04A 0.9900 . ? C04A H04B 0.9900 . ? O2A H2O 0.98(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si1A C2A H2A 109.5 . . ? Si1A C2A H2B 109.5 . . ? H2A C2A H2B 109.5 . . ? Si1A C2A H2C 109.5 . . ? H2A C2A H2C 109.5 . . ? H2B C2A H2C 109.5 . . ? Si1A C1A H1A 109.5 . . ? Si1A C1A H1B 109.5 . . ? H1A C1A H1B 109.5 . . ? Si1A C1A H1C 109.5 . . ? H1A C1A H1C 109.5 . . ? H1B C1A H1C 109.5 . . ? Si2A C4A H4A 109.5 . . ? Si2A C4A H4B 109.5 . . ? H4A C4A H4B 109.5 . . ? Si2A C4A H4C 109.5 . . ? H4A C4A H4C 109.5 . . ? H4B C4A H4C 109.5 . . ? Si2A C3A H3A 109.5 . . ? Si2A C3A H3B 109.5 . . ? H3A C3A H3B 109.5 . . ? Si2A C3A H3C 109.5 . . ? H3A C3A H3C 109.5 . . ? H3B C3A H3C 109.5 . . ? C10A C5A C6A 119.04(13) . . ? C10A C5A Si2A 116.90(11) . . ? C6A C5A Si2A 123.93(11) . . ? C7A C6A C5A 118.47(13) . . ? C7A C6A Si1A 118.40(11) . . ? C5A C6A Si1A 123.13(11) . . ? C8A C7A C6A 121.32(14) . . ? C8A C7A H7 119.3 . . ? C6A C7A H7 119.3 . . ? C9A C8A C7A 120.18(13) . . ? C9A C8A C11A 119.79(13) . . ? C7A C8A C11A 120.03(14) . . ? C10A C9A C8A 119.00(14) . . ? C10A C9A H9 120.5 . . ? C8A C9A H9 120.5 . . ? C9A C10A C5A 121.98(15) . . ? C9A C10A H10 119.0 . . ? C5A C10A H10 119.0 . . ? O1A C11A O2A 123.31(14) . . ? O1A C11A C8A 119.77(13) . . ? O2A C11A C8A 116.92(14) . . ? C04A C03A Si1A 112.23(11) . . ? C04A C03A H03A 109.2 . . ? Si1A C03A H03A 109.2 . . ? C04A C03A H03B 109.2 . . ? Si1A C03A H03B 109.2 . . ? H03A C03A H03B 107.9 . . ? C03A C04A Si2A 111.82(11) . . ? C03A C04A H04A 109.3 . . ? Si2A C04A H04A 109.3 . . ? C03A C04A H04B 109.3 . . ? Si2A C04A H04B 109.3 . . ? H04A C04A H04B 107.9 . . ? C11A O2A H2O 114.4(17) . . ? C2A Si1A C1A 108.17(11) . . ? C2A Si1A C03A 110.50(9) . . ? C1A Si1A C03A 109.92(9) . . ? C2A Si1A C6A 109.89(8) . . ? C1A Si1A C6A 109.68(8) . . ? C03A Si1A C6A 108.67(7) . . ? C4A Si2A C3A 110.39(9) . . ? C4A Si2A C04A 110.74(9) . . ? C3A Si2A C04A 110.42(8) . . ? C4A Si2A C5A 107.03(7) . . ? C3A Si2A C5A 109.68(8) . . ? C04A Si2A C5A 108.49(7) . . ? 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 C10A C5A C6A C7A 0.8(2) . . . . ? Si2A C5A C6A C7A -174.92(11) . . . . ? C10A C5A C6A Si1A -179.19(12) . . . . ? Si2A C5A C6A Si1A 5.09(19) . . . . ? C5A C6A C7A C8A 0.1(2) . . . . ? Si1A C6A C7A C8A -179.93(12) . . . . ? C6A C7A C8A C9A -0.9(2) . . . . ? C6A C7A C8A C11A 178.71(14) . . . . ? C7A C8A C9A C10A 0.8(2) . . . . ? C11A C8A C9A C10A -178.80(14) . . . . ? C8A C9A C10A C5A 0.1(2) . . . . ? C6A C5A C10A C9A -0.9(2) . . . . ? Si2A C5A C10A C9A 175.12(13) . . . . ? C9A C8A C11A O1A 176.62(15) . . . . ? C7A C8A C11A O1A -3.0(2) . . . . ? C9A C8A C11A O2A -3.0(2) . . . . ? C7A C8A C11A O2A 177.38(15) . . . . ? Si1A C03A C04A Si2A -65.99(15) . . . . ? C04A C03A Si1A C2A 169.37(12) . . . . ? C04A C03A Si1A C1A -71.32(14) . . . . ? C04A C03A Si1A C6A 48.72(13) . . . . ? C7A C6A Si1A C2A 42.14(15) . . . . ? C5A C6A Si1A C2A -137.86(14) . . . . ? C7A C6A Si1A C1A -76.64(15) . . . . ? C5A C6A Si1A C1A 103.35(15) . . . . ? C7A C6A Si1A C03A 163.17(12) . . . . ? C5A C6A Si1A C03A -16.84(15) . . . . ? C03A C04A Si2A C4A -68.06(14) . . . . ? C03A C04A Si2A C3A 169.35(12) . . . . ? C03A C04A Si2A C5A 49.13(14) . . . . ? C10A C5A Si2A C4A -73.81(14) . . . . ? C6A C5A Si2A C4A 101.99(14) . . . . ? C10A C5A Si2A C3A 45.96(14) . . . . ? C6A C5A Si2A C3A -138.23(13) . . . . ? C10A C5A Si2A C04A 166.65(13) . . . . ? C6A C5A Si2A C04A -17.55(15) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 29.25 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.382 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.055 data_glu10g _database_code_depnum_ccdc_archive 'CCDC 838000' #TrackingRef 'analogues_of_ec23.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H18 O2 Si2' _chemical_formula_sum 'C12 H18 O2 Si2' _chemical_formula_weight 250.44 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' 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 '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 17.973(4) _cell_length_b 5.5806(8) _cell_length_c 27.605(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.75(3) _cell_angle_gamma 90.00 _cell_volume 2768.5(9) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 7.2 _cell_measurement_theta_max 26.65 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max .5 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.241 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8526 _exptl_absorpt_correction_T_max 0.9419 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate_Stoe-IPDS _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19009 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 29.16 _reflns_number_total 3545 _reflns_number_gt 3091 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDs _computing_cell_refinement Stoe-IPDs _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+1.4934P] 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 3545 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.1054 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 C1 C 0.11095(9) 0.3057(3) 0.22383(5) 0.0359(3) Uani 1 1 d . . . H1A H 0.0696 0.4186 0.2197 0.054 Uiso 1 1 calc R . . H1B H 0.1578 0.3948 0.2268 0.054 Uiso 1 1 calc R . . H1C H 0.1035 0.2104 0.2532 0.054 Uiso 1 1 calc R . . C2 C 0.02381(8) -0.0573(3) 0.16524(6) 0.0356(3) Uani 1 1 d . . . H2A H 0.0166 -0.1547 0.1943 0.053 Uiso 1 1 calc R . . H2B H 0.0235 -0.1611 0.1366 0.053 Uiso 1 1 calc R . . H2C H -0.0165 0.0604 0.1623 0.053 Uiso 1 1 calc R . . C03 C 0.19996(7) -0.0928(2) 0.17232(5) 0.0258(3) Uani 1 1 d . . . H03A H 0.2154 -0.1253 0.2062 0.031 Uiso 1 1 calc R . . H03B H 0.1908 -0.2471 0.1556 0.031 Uiso 1 1 calc R . . C3 C 0.31969(8) 0.3036(3) 0.18224(5) 0.0340(3) Uani 1 1 d . . . H3A H 0.3495 0.2153 0.2063 0.051 Uiso 1 1 calc R . . H3B H 0.2822 0.3998 0.1988 0.051 Uiso 1 1 calc R . . H3C H 0.3522 0.4093 0.1636 0.051 Uiso 1 1 calc R . . C4 C 0.34563(8) -0.0868(3) 0.10866(6) 0.0352(3) Uani 1 1 d . . . H4A H 0.3788 -0.1621 0.1327 0.053 Uiso 1 1 calc R . . H4B H 0.3744 0.0213 0.0882 0.053 Uiso 1 1 calc R . . H4C H 0.3222 -0.2109 0.0885 0.053 Uiso 1 1 calc R . . C5 C 0.20992(6) 0.2640(2) 0.09812(4) 0.0221(2) Uani 1 1 d . . . C6 C 0.13517(6) 0.2794(2) 0.11334(4) 0.0217(2) Uani 1 1 d . . . C7 C 0.08545(7) 0.4286(2) 0.08819(5) 0.0239(3) Uani 1 1 d . . . H7 H 0.0349 0.4367 0.0978 0.029 Uiso 1 1 calc R . . C8 C 0.10968(7) 0.5658(2) 0.04908(4) 0.0246(3) Uani 1 1 d . . . C9 C 0.18268(7) 0.5434(3) 0.03314(5) 0.0283(3) Uani 1 1 d . . . H9 H 0.1985 0.6316 0.0057 0.034 Uiso 1 1 calc R . . C10 C 0.23231(7) 0.3927(3) 0.05717(5) 0.0265(3) Uani 1 1 d . . . H10 H 0.2817 0.3766 0.0458 0.032 Uiso 1 1 calc R . . C11 C 0.05996(7) 0.7461(3) 0.02581(5) 0.0274(3) Uani 1 1 d . . . O2 O -0.00747(6) 0.7541(2) 0.03926(4) 0.0387(3) Uani 1 1 d . . . H2O H -0.0280 0.8773 0.0278 0.058 Uiso 1 1 calc R . . O1 O 0.08704(6) 0.8866(2) -0.00528(4) 0.0399(3) Uani 1 1 d . . . Si1 Si 0.114798(18) 0.10189(6) 0.169945(12) 0.02261(11) Uani 1 1 d . . . Si2 Si 0.272421(17) 0.08668(6) 0.140277(12) 0.02252(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0435(8) 0.0347(8) 0.0296(6) 0.0003(6) 0.0057(5) 0.0027(6) C2 0.0244(6) 0.0339(8) 0.0485(8) 0.0050(6) 0.0041(5) -0.0025(5) C03 0.0237(5) 0.0225(7) 0.0312(6) 0.0062(5) -0.0003(4) 0.0014(4) C3 0.0320(6) 0.0341(8) 0.0356(7) 0.0039(6) -0.0080(5) -0.0055(5) C4 0.0282(6) 0.0348(9) 0.0429(8) 0.0045(6) 0.0059(5) 0.0080(5) C5 0.0212(5) 0.0222(6) 0.0228(5) 0.0020(4) -0.0008(4) 0.0006(4) C6 0.0213(5) 0.0219(6) 0.0220(5) 0.0026(4) -0.0004(4) 0.0010(4) C7 0.0209(5) 0.0255(7) 0.0254(6) 0.0033(4) 0.0004(4) 0.0022(4) C8 0.0243(5) 0.0252(7) 0.0241(5) 0.0041(4) -0.0017(4) 0.0022(4) C9 0.0268(6) 0.0328(8) 0.0254(6) 0.0073(5) 0.0029(4) 0.0016(5) C10 0.0223(5) 0.0310(7) 0.0263(6) 0.0056(5) 0.0029(4) 0.0020(5) C11 0.0274(6) 0.0296(7) 0.0252(6) 0.0063(5) -0.0007(4) 0.0034(5) O2 0.0280(5) 0.0455(7) 0.0427(6) 0.0181(5) 0.0012(4) 0.0104(4) O1 0.0385(5) 0.0418(7) 0.0396(6) 0.0203(5) 0.0068(4) 0.0099(5) Si1 0.02137(17) 0.0217(2) 0.02484(18) 0.00442(12) 0.00200(12) 0.00072(11) Si2 0.01884(17) 0.0229(2) 0.02584(18) 0.00408(12) -0.00122(12) 0.00142(11) _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. TITL glu10c in C2/c CELL 0.71073 17.9727 5.5806 27.6046 90.000 90.752 90.000 ZERR 8. 0.0037 0.0008 0.0064 0.000 0.026 0.000 REM CELL 0.71073 18.0083 5.5801 27.6005 90.000 90.666 90.000 REM ZERR 8.00 0.0036 0.0011 0.0055 0.000 0.030 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H O Si UNIT 96 144 16 16 L.S. 18 ACTA BOND $H FMAP 2 PLAN 20 HTAB 2.5 CONF TEMP -100 WGHT 0.061900 1.493400 FVAR 0.60210 MOLE 1 C1 1 0.110946 0.305749 0.223834 11.00000 0.04351 0.03467 = 0.02962 0.00027 0.00569 0.00267 AFIX 137 H1A 2 0.069571 0.418600 0.219696 11.00000 -1.50000 H1B 2 0.157778 0.394819 0.226795 11.00000 -1.50000 H1C 2 0.103475 0.210390 0.253182 11.00000 -1.50000 AFIX 0 C2 1 0.023813 -0.057251 0.165243 11.00000 0.02436 0.03391 = 0.04850 0.00498 0.00406 -0.00247 AFIX 137 H2A 2 0.016571 -0.154748 0.194330 11.00000 -1.50000 H2B 2 0.023514 -0.161054 0.136606 11.00000 -1.50000 H2C 2 -0.016485 0.060374 0.162322 11.00000 -1.50000 AFIX 0 C03 1 0.199959 -0.092789 0.172319 11.00000 0.02366 0.02250 = 0.03120 0.00618 -0.00026 0.00145 AFIX 23 H03A 2 0.215371 -0.125301 0.206248 11.00000 -1.20000 H03B 2 0.190816 -0.247127 0.155589 11.00000 -1.20000 AFIX 0 C3 1 0.319693 0.303599 0.182242 11.00000 0.03202 0.03407 = 0.03558 0.00386 -0.00801 -0.00548 AFIX 137 H3A 2 0.349505 0.215300 0.206267 11.00000 -1.50000 H3B 2 0.282157 0.399794 0.198803 11.00000 -1.50000 H3C 2 0.352169 0.409278 0.163627 11.00000 -1.50000 AFIX 0 C4 1 0.345626 -0.086757 0.108662 11.00000 0.02818 0.03477 = 0.04293 0.00450 0.00592 0.00796 AFIX 137 H4A 2 0.378775 -0.162062 0.132670 11.00000 -1.50000 H4B 2 0.374450 0.021325 0.088153 11.00000 -1.50000 H4C 2 0.322224 -0.210914 0.088506 11.00000 -1.50000 AFIX 0 C5 1 0.209923 0.263987 0.098121 11.00000 0.02116 0.02218 = 0.02282 0.00203 -0.00077 0.00058 C6 1 0.135170 0.279408 0.113336 11.00000 0.02128 0.02192 = 0.02199 0.00261 -0.00041 0.00098 C7 1 0.085451 0.428607 0.088190 11.00000 0.02091 0.02546 = 0.02541 0.00328 0.00041 0.00216 AFIX 43 H7 2 0.034929 0.436724 0.097752 11.00000 -1.20000 AFIX 0 C8 1 0.109680 0.565788 0.049081 11.00000 0.02426 0.02522 = 0.02415 0.00412 -0.00173 0.00222 C9 1 0.182676 0.543378 0.033143 11.00000 0.02677 0.03284 = 0.02544 0.00732 0.00294 0.00159 AFIX 43 H9 2 0.198503 0.631647 0.005715 11.00000 -1.20000 AFIX 0 C10 1 0.232311 0.392686 0.057173 11.00000 0.02234 0.03104 = 0.02627 0.00564 0.00292 0.00198 AFIX 43 H10 2 0.281730 0.376646 0.045815 11.00000 -1.20000 AFIX 0 C11 1 0.059959 0.746121 0.025808 11.00000 0.02737 0.02960 = 0.02518 0.00625 -0.00069 0.00340 O2 3 -0.007471 0.754110 0.039258 11.00000 0.02802 0.04547 = 0.04270 0.01814 0.00124 0.01043 AFIX 87 H2O 2 -0.027966 0.877343 0.027801 11.00000 -1.50000 AFIX 0 O1 3 0.087043 0.886618 -0.005283 11.00000 0.03849 0.04179 = 0.03960 0.02025 0.00675 0.00985 SI1 4 0.114798 0.101893 0.169945 11.00000 0.02137 0.02167 = 0.02484 0.00442 0.00200 0.00072 SI2 4 0.272421 0.086678 0.140277 11.00000 0.01884 0.02286 = 0.02584 0.00408 -0.00122 0.00142 HKLF 4 REM glu10c in C2/c REM R1 = 0.0370 for 3091 Fo > 4sig(Fo) and 0.0417 for all 3545 data REM 150 parameters refined using 0 restraints END WGHT 0.0619 1.4932 REM Highest difference peak 0.364, deepest hole -0.242, 1-sigma level 0.054 Q1 1 0.1216 0.2157 0.1368 11.00000 0.05 0.36 Q2 1 0.2353 0.1738 0.1142 11.00000 0.05 0.35 Q3 1 0.1720 0.2690 0.1099 11.00000 0.05 0.34 Q4 1 0.2237 0.3221 0.0797 11.00000 0.05 0.34 Q5 1 0.0971 0.4999 0.0682 11.00000 0.05 0.33 Q6 1 0.1109 0.2136 0.1996 11.00000 0.05 0.33 Q7 1 0.0873 0.6450 0.0392 11.00000 0.05 0.31 Q8 1 0.2299 -0.0265 0.1565 11.00000 0.05 0.31 Q9 1 0.1111 0.3675 0.1036 11.00000 0.05 0.30 Q10 1 0.1396 0.5813 0.0465 11.00000 0.05 0.30 Q11 1 0.0652 -0.0018 0.1700 11.00000 0.05 0.29 Q12 1 0.3072 0.0017 0.1229 11.00000 0.05 0.29 Q13 1 0.1658 -0.0195 0.1721 11.00000 0.05 0.28 Q14 1 0.0672 1.0028 -0.0100 11.00000 0.05 0.27 Q15 1 0.0727 0.8211 -0.0014 11.00000 0.05 0.25 Q16 1 0.3002 0.2244 0.1618 11.00000 0.05 0.25 Q17 1 0.2045 0.4333 0.0418 11.00000 0.05 0.25 Q18 1 0.1133 -0.2968 0.1711 11.00000 0.05 0.23 Q19 1 0.0873 0.9031 0.0120 11.00000 0.05 0.22 Q20 1 0.0149 0.8542 0.0528 11.00000 0.05 0.17 ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 Si1 1.8747(16) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 Si1 1.8639(15) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C03 Si2 1.8739(13) . ? C03 Si1 1.8774(13) . ? C03 H03A 0.9900 . ? C03 H03B 0.9900 . ? C3 Si2 1.8717(16) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 Si2 1.8600(15) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C10 1.4026(17) . ? C5 C6 1.4155(16) . ? C5 Si2 1.8870(13) . ? C6 C7 1.3990(16) . ? C6 Si1 1.8901(13) . ? C7 C8 1.3977(17) . ? C7 H7 0.9500 . ? C8 C9 1.3948(17) . ? C8 C11 1.4863(17) . ? C9 C10 1.3883(18) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 O1 1.2646(16) . ? C11 O2 1.2729(16) . ? O2 H2O 0.8400 . ? 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 Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si2 C03 Si1 104.21(7) . . ? Si2 C03 H03A 110.9 . . ? Si1 C03 H03A 110.9 . . ? Si2 C03 H03B 110.9 . . ? Si1 C03 H03B 110.9 . . ? H03A C03 H03B 108.9 . . ? Si2 C3 H3A 109.5 . . ? Si2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 119.43(11) . . ? C10 C5 Si2 126.21(9) . . ? C6 C5 Si2 114.11(9) . . ? C7 C6 C5 119.44(11) . . ? C7 C6 Si1 126.35(9) . . ? C5 C6 Si1 114.10(9) . . ? C8 C7 C6 120.38(11) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C9 C8 C7 119.89(12) . . ? C9 C8 C11 119.15(11) . . ? C7 C8 C11 120.87(11) . . ? C10 C9 C8 120.31(12) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C5 120.39(11) . . ? C9 C10 H10 119.8 . . ? C5 C10 H10 119.8 . . ? O1 C11 O2 123.55(12) . . ? O1 C11 C8 118.59(12) . . ? O2 C11 C8 117.84(11) . . ? C11 O2 H2O 109.5 . . ? C2 Si1 C1 107.63(7) . . ? C2 Si1 C03 116.15(7) . . ? C1 Si1 C03 111.23(7) . . ? C2 Si1 C6 111.81(7) . . ? C1 Si1 C6 110.34(7) . . ? C03 Si1 C6 99.53(6) . . ? C4 Si2 C3 107.99(7) . . ? C4 Si2 C03 116.33(7) . . ? C3 Si2 C03 111.48(7) . . ? C4 Si2 C5 113.73(6) . . ? C3 Si2 C5 107.71(7) . . ? C03 Si2 C5 99.18(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 C5 C6 C7 -2.00(19) . . . . ? Si2 C5 C6 C7 172.69(10) . . . . ? C10 C5 C6 Si1 -178.48(10) . . . . ? Si2 C5 C6 Si1 -3.80(12) . . . . ? C5 C6 C7 C8 -1.51(19) . . . . ? Si1 C6 C7 C8 174.50(10) . . . . ? C6 C7 C8 C9 3.8(2) . . . . ? C6 C7 C8 C11 -172.68(12) . . . . ? C7 C8 C9 C10 -2.6(2) . . . . ? C11 C8 C9 C10 173.95(13) . . . . ? C8 C9 C10 C5 -0.9(2) . . . . ? C6 C5 C10 C9 3.2(2) . . . . ? Si2 C5 C10 C9 -170.77(11) . . . . ? C9 C8 C11 O1 -5.3(2) . . . . ? C7 C8 C11 O1 171.23(14) . . . . ? C9 C8 C11 O2 176.34(13) . . . . ? C7 C8 C11 O2 -7.1(2) . . . . ? Si2 C03 Si1 C2 146.80(7) . . . . ? Si2 C03 Si1 C1 -89.65(8) . . . . ? Si2 C03 Si1 C6 26.66(8) . . . . ? C7 C6 Si1 C2 45.38(14) . . . . ? C5 C6 Si1 C2 -138.42(10) . . . . ? C7 C6 Si1 C1 -74.37(13) . . . . ? C5 C6 Si1 C1 101.83(11) . . . . ? C7 C6 Si1 C03 168.65(12) . . . . ? C5 C6 Si1 C03 -15.15(11) . . . . ? Si1 C03 Si2 C4 -150.64(7) . . . . ? Si1 C03 Si2 C3 84.95(8) . . . . ? Si1 C03 Si2 C5 -28.30(7) . . . . ? C10 C5 Si2 C4 -40.50(14) . . . . ? C6 C5 Si2 C4 145.24(10) . . . . ? C10 C5 Si2 C3 79.14(13) . . . . ? C6 C5 Si2 C3 -95.12(11) . . . . ? C10 C5 Si2 C03 -164.69(12) . . . . ? C6 C5 Si2 C03 21.04(11) . . . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 29.16 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.364 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.054 data_glu23d _database_code_depnum_ccdc_archive 'CCDC 872960' #TrackingRef 'glu23d_.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H24 O2 Si2' _chemical_formula_sum 'C22 H24 O2 Si2' _chemical_formula_weight 376.59 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.3734(6) _cell_length_b 11.1736(7) _cell_length_c 36.103(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4184.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5.35 _cell_measurement_theta_max 26.8 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max .4 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.182 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate_Stoe-IPDS _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30629 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 26.86 _reflns_number_total 4474 _reflns_number_gt 3404 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+2.6001P] 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 4474 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1229 _refine_ls_wR_factor_gt 0.1125 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 C1 C 0.3113(3) 0.5340(2) 0.30444(8) 0.0623(7) Uani 1 1 d . . . H1A H 0.3495 0.4551 0.3088 0.093 Uiso 1 1 calc R . . H1B H 0.3330 0.5874 0.3251 0.093 Uiso 1 1 calc R . . H1C H 0.3452 0.5674 0.2813 0.093 Uiso 1 1 calc R . . C2 C 0.0923(4) 0.4111(2) 0.26317(7) 0.0693(8) Uani 1 1 d . . . H2A H 0.1226 0.4429 0.2394 0.104 Uiso 1 1 calc R . . H2B H -0.0012 0.3993 0.2621 0.104 Uiso 1 1 calc R . . H2C H 0.1347 0.3343 0.2681 0.104 Uiso 1 1 calc R . . C3 C -0.0647(4) 0.8212(2) 0.36030(8) 0.0706(9) Uani 1 1 d . . . H3A H -0.0896 0.8886 0.3445 0.106 Uiso 1 1 calc R . . H3B H 0.0237 0.8329 0.3691 0.106 Uiso 1 1 calc R . . H3C H -0.1233 0.8165 0.3815 0.106 Uiso 1 1 calc R . . C4 C -0.2406(4) 0.6616(3) 0.31478(10) 0.0857(10) Uani 1 1 d . . . H4A H -0.3020 0.6599 0.3354 0.129 Uiso 1 1 calc R . . H4B H -0.2464 0.5865 0.3009 0.129 Uiso 1 1 calc R . . H4C H -0.2610 0.7288 0.2984 0.129 Uiso 1 1 calc R . . C5 C -0.0317(2) 0.54389(17) 0.36200(6) 0.0387(4) Uani 1 1 d . . . C6 C 0.0593(2) 0.46540(16) 0.34599(5) 0.0359(4) Uani 1 1 d . . . C7 C 0.0854(2) 0.35494(16) 0.36307(5) 0.0351(4) Uani 1 1 d . . . H7 H 0.1463 0.3024 0.3520 0.042 Uiso 1 1 calc R . . C8 C 0.0240(2) 0.32050(16) 0.39590(5) 0.0332(4) Uani 1 1 d . . . C9 C -0.0617(2) 0.40159(17) 0.41227(6) 0.0389(5) Uani 1 1 d . . . H9 H -0.1015 0.3816 0.4352 0.047 Uiso 1 1 calc R . . C10 C -0.0895(2) 0.51077(18) 0.39562(6) 0.0415(5) Uani 1 1 d . . . H10 H -0.1487 0.5639 0.4072 0.050 Uiso 1 1 calc R . . C11 C 0.04456(19) 0.19913(16) 0.41228(5) 0.0316(4) Uani 1 1 d . . . C12 C 0.1632(2) 0.13690(17) 0.40800(5) 0.0339(4) Uani 1 1 d . . . H12 H 0.2324 0.1748 0.3954 0.041 Uiso 1 1 calc R . . C13 C 0.18013(19) 0.02330(16) 0.42174(5) 0.0331(4) Uani 1 1 d . . . H13 H 0.2606 -0.0159 0.4186 0.040 Uiso 1 1 calc R . . C14 C 0.07828(18) -0.03630(16) 0.44068(5) 0.0298(4) Uani 1 1 d . . . C15 C 0.08958(18) -0.15524(16) 0.45405(5) 0.0302(4) Uani 1 1 d . . . H15 H 0.1683 -0.1976 0.4509 0.036 Uiso 1 1 calc R . . C16 C -0.01293(18) -0.20979(15) 0.47157(5) 0.0299(4) Uani 1 1 d . . . C17 C -0.12999(19) -0.14683(17) 0.47733(5) 0.0345(4) Uani 1 1 d . . . H17 H -0.1995 -0.1844 0.4899 0.041 Uiso 1 1 calc R . . C18 C -0.14255(19) -0.03178(16) 0.46475(6) 0.0347(4) Uani 1 1 d . . . H18 H -0.2210 0.0101 0.4688 0.042 Uiso 1 1 calc R . . C19 C -0.04009(19) 0.02579(16) 0.44579(5) 0.0305(4) Uani 1 1 d . . . C20 C -0.05405(19) 0.14304(16) 0.43128(5) 0.0322(4) Uani 1 1 d . . . H20 H -0.1333 0.1841 0.4347 0.039 Uiso 1 1 calc R . . C21 C -0.00566(18) -0.33563(16) 0.48459(5) 0.0309(4) Uani 1 1 d . . . C03 C 0.0505(3) 0.6684(2) 0.29561(7) 0.0616(7) Uani 1 1 d . . . H03A H 0.1141 0.7340 0.2980 0.074 Uiso 1 1 calc R . . H03B H 0.0091 0.6742 0.2710 0.074 Uiso 1 1 calc R . . O1 O 0.10131(14) -0.39162(12) 0.47840(5) 0.0426(4) Uani 1 1 d . . . H1 H 0.0942 -0.4631 0.4853 0.064 Uiso 1 1 calc R . . O2 O -0.10004(14) -0.38325(12) 0.50041(4) 0.0424(4) Uani 1 1 d . . . Si1 Si 0.13223(7) 0.51926(5) 0.300965(15) 0.04297(18) Uani 1 1 d . . . Si2 Si -0.07418(7) 0.67970(5) 0.333233(16) 0.04204(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0789(19) 0.0491(14) 0.0588(15) 0.0058(11) 0.0188(13) -0.0055(13) C2 0.120(3) 0.0465(13) 0.0417(12) -0.0024(11) -0.0062(14) -0.0105(16) C3 0.124(3) 0.0316(12) 0.0558(15) 0.0020(10) -0.0026(16) 0.0049(14) C4 0.085(2) 0.076(2) 0.096(2) 0.0282(18) -0.033(2) -0.0087(18) C5 0.0506(12) 0.0256(9) 0.0398(10) 0.0028(7) -0.0051(9) -0.0012(8) C6 0.0500(12) 0.0234(8) 0.0343(9) 0.0023(7) -0.0039(8) -0.0034(8) C7 0.0451(11) 0.0242(8) 0.0359(9) 0.0010(7) -0.0010(8) -0.0013(8) C8 0.0387(10) 0.0238(8) 0.0371(9) 0.0024(7) -0.0053(8) -0.0018(8) C9 0.0466(12) 0.0306(9) 0.0397(10) 0.0059(8) 0.0032(9) 0.0019(9) C10 0.0524(13) 0.0278(9) 0.0444(11) 0.0038(8) 0.0039(9) 0.0059(9) C11 0.0378(10) 0.0237(8) 0.0333(9) 0.0015(7) -0.0034(7) -0.0020(8) C12 0.0375(10) 0.0275(9) 0.0367(9) 0.0028(7) 0.0014(8) -0.0034(8) C13 0.0327(10) 0.0279(9) 0.0386(9) 0.0017(7) 0.0009(8) 0.0008(8) C14 0.0329(10) 0.0247(8) 0.0318(9) 0.0005(7) -0.0029(7) -0.0009(7) C15 0.0300(9) 0.0249(8) 0.0356(9) 0.0008(7) -0.0028(7) 0.0019(7) C16 0.0311(10) 0.0229(8) 0.0357(9) 0.0025(7) -0.0053(7) -0.0015(7) C17 0.0330(10) 0.0278(9) 0.0428(10) 0.0060(8) 0.0008(8) -0.0006(8) C18 0.0302(10) 0.0287(9) 0.0451(10) 0.0056(8) 0.0012(8) 0.0031(8) C19 0.0343(10) 0.0235(8) 0.0338(9) 0.0015(7) -0.0029(7) -0.0007(7) C20 0.0340(10) 0.0245(8) 0.0383(9) 0.0021(7) -0.0025(8) 0.0027(7) C21 0.0305(10) 0.0260(9) 0.0363(9) 0.0028(7) -0.0053(7) -0.0024(7) C03 0.094(2) 0.0343(12) 0.0565(14) 0.0153(10) 0.0116(13) 0.0108(13) O1 0.0352(8) 0.0252(6) 0.0674(10) 0.0102(6) 0.0016(7) 0.0040(6) O2 0.0355(8) 0.0284(7) 0.0632(9) 0.0123(6) 0.0015(7) -0.0022(6) Si1 0.0707(4) 0.0240(3) 0.0341(3) 0.0031(2) 0.0042(3) -0.0008(3) Si2 0.0601(4) 0.0248(3) 0.0413(3) 0.0050(2) -0.0075(3) 0.0028(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 C1 Si1 1.869(3) . ? C2 Si1 1.869(3) . ? C3 Si2 1.861(3) . ? C4 Si2 1.862(3) . ? C5 C10 1.404(3) . ? C5 C6 1.412(3) . ? C5 Si2 1.891(2) . ? C6 C7 1.406(3) . ? C6 Si1 1.891(2) . ? C7 C8 1.399(3) . ? C8 C9 1.401(3) . ? C8 C11 1.495(2) . ? C9 C10 1.390(3) . ? C11 C20 1.382(3) . ? C11 C12 1.422(3) . ? C12 C13 1.374(3) . ? C13 C14 1.424(3) . ? C14 C15 1.419(2) . ? C14 C19 1.422(3) . ? C15 C16 1.379(3) . ? C16 C17 1.419(3) . ? C16 C21 1.484(2) . ? C17 C18 1.370(3) . ? C18 C19 1.419(3) . ? C19 C20 1.418(2) . ? C21 O2 1.252(2) . ? C21 O1 1.293(2) . ? C03 Si2 1.880(3) . ? C03 Si1 1.880(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 C5 C6 118.42(18) . . ? C10 C5 Si2 125.93(16) . . ? C6 C5 Si2 115.44(15) . . ? C7 C6 C5 119.64(18) . . ? C7 C6 Si1 125.39(16) . . ? C5 C6 Si1 114.93(14) . . ? C8 C7 C6 121.68(19) . . ? C7 C8 C9 117.94(17) . . ? C7 C8 C11 121.33(17) . . ? C9 C8 C11 120.68(17) . . ? C10 C9 C8 121.12(19) . . ? C9 C10 C5 121.1(2) . . ? C20 C11 C12 118.22(17) . . ? C20 C11 C8 120.16(18) . . ? C12 C11 C8 121.59(17) . . ? C13 C12 C11 121.53(18) . . ? C12 C13 C14 120.71(18) . . ? C15 C14 C19 118.96(17) . . ? C15 C14 C13 122.70(17) . . ? C19 C14 C13 118.34(16) . . ? C16 C15 C14 120.41(17) . . ? C15 C16 C17 120.53(16) . . ? C15 C16 C21 121.64(17) . . ? C17 C16 C21 117.82(17) . . ? C18 C17 C16 119.89(18) . . ? C17 C18 C19 120.96(18) . . ? C20 C19 C18 121.37(17) . . ? C20 C19 C14 119.40(17) . . ? C18 C19 C14 119.22(16) . . ? C11 C20 C19 121.78(18) . . ? O2 C21 O1 122.96(17) . . ? O2 C21 C16 120.48(17) . . ? O1 C21 C16 116.56(16) . . ? Si2 C03 Si1 107.20(11) . . ? C1 Si1 C2 109.02(15) . . ? C1 Si1 C03 112.15(13) . . ? C2 Si1 C03 113.48(14) . . ? C1 Si1 C6 111.60(11) . . ? C2 Si1 C6 109.46(11) . . ? C03 Si1 C6 100.95(10) . . ? C3 Si2 C4 109.22(17) . . ? C3 Si2 C03 113.59(14) . . ? C4 Si2 C03 111.85(16) . . ? C3 Si2 C5 112.40(10) . . ? C4 Si2 C5 108.99(12) . . ? C03 Si2 C5 100.51(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 C5 C6 C7 2.7(3) . . . . ? Si2 C5 C6 C7 -172.30(15) . . . . ? C10 C5 C6 Si1 -179.52(16) . . . . ? Si2 C5 C6 Si1 5.5(2) . . . . ? C5 C6 C7 C8 -0.4(3) . . . . ? Si1 C6 C7 C8 -178.00(15) . . . . ? C6 C7 C8 C9 -2.3(3) . . . . ? C6 C7 C8 C11 175.15(18) . . . . ? C7 C8 C9 C10 2.8(3) . . . . ? C11 C8 C9 C10 -174.66(19) . . . . ? C8 C9 C10 C5 -0.6(3) . . . . ? C6 C5 C10 C9 -2.2(3) . . . . ? Si2 C5 C10 C9 172.20(17) . . . . ? C7 C8 C11 C20 -147.18(19) . . . . ? C9 C8 C11 C20 30.2(3) . . . . ? C7 C8 C11 C12 31.0(3) . . . . ? C9 C8 C11 C12 -151.6(2) . . . . ? C20 C11 C12 C13 1.0(3) . . . . ? C8 C11 C12 C13 -177.22(17) . . . . ? C11 C12 C13 C14 0.3(3) . . . . ? C12 C13 C14 C15 177.46(18) . . . . ? C12 C13 C14 C19 -1.5(3) . . . . ? C19 C14 C15 C16 0.3(3) . . . . ? C13 C14 C15 C16 -178.67(17) . . . . ? C14 C15 C16 C17 -1.6(3) . . . . ? C14 C15 C16 C21 177.66(16) . . . . ? C15 C16 C17 C18 1.4(3) . . . . ? C21 C16 C17 C18 -177.96(17) . . . . ? C16 C17 C18 C19 0.3(3) . . . . ? C17 C18 C19 C20 177.29(18) . . . . ? C17 C18 C19 C14 -1.6(3) . . . . ? C15 C14 C19 C20 -177.61(16) . . . . ? C13 C14 C19 C20 1.4(3) . . . . ? C15 C14 C19 C18 1.3(3) . . . . ? C13 C14 C19 C18 -179.68(17) . . . . ? C12 C11 C20 C19 -1.1(3) . . . . ? C8 C11 C20 C19 177.16(17) . . . . ? C18 C19 C20 C11 -179.01(18) . . . . ? C14 C19 C20 C11 -0.1(3) . . . . ? C15 C16 C21 O2 -179.98(18) . . . . ? C17 C16 C21 O2 -0.7(3) . . . . ? C15 C16 C21 O1 -0.5(3) . . . . ? C17 C16 C21 O1 178.82(17) . . . . ? Si2 C03 Si1 C1 -125.83(15) . . . . ? Si2 C03 Si1 C2 110.08(17) . . . . ? Si2 C03 Si1 C6 -6.91(17) . . . . ? C7 C6 Si1 C1 -61.9(2) . . . . ? C5 C6 Si1 C1 120.40(18) . . . . ? C7 C6 Si1 C2 58.9(2) . . . . ? C5 C6 Si1 C2 -118.82(19) . . . . ? C7 C6 Si1 C03 178.76(19) . . . . ? C5 C6 Si1 C03 1.09(19) . . . . ? Si1 C03 Si2 C3 129.51(15) . . . . ? Si1 C03 Si2 C4 -106.29(18) . . . . ? Si1 C03 Si2 C5 9.25(17) . . . . ? C10 C5 Si2 C3 54.8(2) . . . . ? C6 C5 Si2 C3 -130.64(19) . . . . ? C10 C5 Si2 C4 -66.4(2) . . . . ? C6 C5 Si2 C4 108.1(2) . . . . ? C10 C5 Si2 C03 175.9(2) . . . . ? C6 C5 Si2 C03 -9.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.86 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.271 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.048