Supplementary Material for Organic & Biomolecular Chemistry This journal is © The Royal Society of Chemistry 2004 Supplementary data data_global _publ_contact_author_email haz@chem.au.dk _publ_contact_author_name 'Rita Hazell' _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Direct catalytic asymmetric aldol reactions of pyruvates: scope and mechanism ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name 'Nicholas Gathergood' 'Thomas B. Poulsen' 'Karsten Juhl' 'Karl Thordrup' 'Karl Anker Jorgensen' _publ_contact_author_address ; Department of Chemistry Aarhus University Langelandsgade 140 DK-8000 Aarhus C DENMARK ; #============================================================================== # 4. TEXT _publ_section_references ; Altomare,A., Cascarano,G., Giacovazzo,C., Guagliardi,A., Moliterni,.A,G,G., Burla,M.C., Polidori,G., Camalli,M. & Spagna,R. (1997). SIR97. University of Bari, Italy. Becker,P.J. & Coppens, P. (1974). Acta Cryst. A30, 129-153. Burnett,M.N. & Johnson,C.K. (1996). ORTEP-III. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA. Busing,W.R., Martin,K.O. & Levy,H.A. (1962). ORFLS. Report ORNL-TM-305. Oak Ridge National Laboratory, Tennessee, USA. Hazell,A. (1995). KRYSTAL, An integrated system of crystallographic programs. Aarhus University, Denmark. Rogers,D. (1981). Acta Cryst. A37, 734-741. Siemens (1995) SMART, SAINT and XPREP Area-Detector Control and Integration Software. Siemens Analytical X-ray Instruments Inc. Madison, Wisconsin, USA. ; #============================================================================== data_cpd_4ab _database_code_depnum_ccdc_archive 'CCDC 225814' #=================================== # 5. CHEMICAL DATA _chemical_name_systematic ; 4-(Di-tert-butyl-hydroxy-silanyloxy)-2-methyl-5-oxo-2,5-dihydro-furan- -2-carboxylic acid ethyl ester ; _chemical_formula_sum 'C16 H28 O6 Si' _chemical_formula_moiety 'C16 H28 O6 Si' _chemical_formula_weight 344.49 #=================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,-z _cell_length_a 12.626(1) _cell_length_b 14.332(2) _cell_length_c 20.971(2) _cell_angle_alpha 90.000 _cell_angle_beta 95.257(2) _cell_angle_gamma 90.000 _cell_volume 3778.9(7) _cell_formula_units_Z 8 _cell_measurement_temperature 120 _cell_measurement_reflns_used 7054 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 27.51 _exptl_crystal_description slab _exptl_crystal_colour colourless _exptl_crystal_size_max .58 _exptl_crystal_size_mid .33 _exptl_crystal_size_min .14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.149 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'XPREP, 1995 ' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.98 #=================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation scans with narrow frames' _diffrn_standards_decay_% 0 _diffrn_reflns_number 74525 _diffrn_reflns_av_R_equivalents 0.122 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process 74525 _reflns_number_total 17356 _diffrn_measured_fraction_theta_max 100.0 _diffrn_measured_fraction_theta_full 100.0 _diffrn_reflns_theta_full 27.51 _reflns_number_gt 13270 _reflns_threshold_expression I>3\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Altomare et al., 1997 ), KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #=================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement was done with standard least squares procedures and no special treatment was used in spite of the fact, that the structure contains a near halving of the a-axis and a near c-glide. The main deviations from the extra symmetry occur at the ethyl groups. The residual density is found in these areas, and reflects that the ordering of these 'tails' is not perfect. The crystal used in this investigation was much larger and better quality than several earlier attempts, some of which didn't show the weak layers, possibly because the crystals were too small to give strong enough reflections -possibly because the disorder was more pronounced. The hydrogen atoms on carbon were kept 'riding', those on the hydroxy groups were refined isotropically. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w= 1/{[\s~cs~(F^2^)+B+(1+A)F^2^]^1/2^- |F|}^2^ where A = 0.04 and B = 0.5 ; _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method ; Type 1 Lorentzian isotropic ( Becker and Coppens, 1974) ; _refine_ls_extinction_coef 140(25) _refine_ls_abs_structure_details ; The least squares refinement included a parameter according to Rogers (1981) refined against all 13270 significant reflections including 5967 Bijvoet pairs. The result is convincing although Si is not usually used for the determination of absolute configurations. ; _refine_ls_abs_structure_Rogers 0.86(16) _refine_ls_number_reflns 13270 _refine_ls_number_parameters 846 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_gt 0.055 _refine_ls_wR_factor_ref 0.065 _refine_ls_goodness_of_fit_ref 1.45 _refine_ls_shift/su_max 0.0028 _refine_ls_shift/su_mean 0.0003 _refine_diff_density_max 1.5(1) _refine_diff_density_min -1.1(1) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Si1 0.98331(7) 0.64556(9) 0.34027(4) 0.0123(5) Uij Si2 0.48134(7) 0.66233(9) 0.34309(4) 0.0130(5) Uij Si3 0.23481(7) 0.17992(9) 0.29407(4) 0.0116(4) Uij Si4 0.73803(7) 0.18088(9) 0.29407(4) 0.0118(4) Uij O1 0.7035(2) 0.7695(2) 0.2347(1) 0.017(1) Uij O2 0.8792(2) 0.6530(2) 0.2842(1) 0.016(1) Uij O3 1.0931(2) 0.6308(2) 0.3069(1) 0.018(1) Uij O4 0.7952(2) 0.7904(2) 0.1493(1) 0.016(1) Uij O5 0.7805(2) 0.6838(2) 0.0443(1) 0.023(1) Uij O6 0.9582(2) 0.6808(2) 0.0417(1) 0.019(1) Uij O21 0.1865(2) 0.7520(2) 0.2213(1) 0.018(1) Uij O22 0.3798(2) 0.6812(2) 0.2871(1) 0.022(1) Uij O23 0.5916(2) 0.6467(2) 0.3111(1) 0.016(1) Uij O24 0.2858(2) 0.7907(2) 0.1420(1) 0.017(1) Uij O25 0.3292(2) 0.6630(2) 0.0545(1) 0.021(1) Uij O26 0.5000(2) 0.7096(2) 0.0572(1) 0.023(1) Uij O41 -0.0560(2) 0.3122(2) 0.1955(1) 0.019(1) Uij O42 0.1371(2) 0.2512(2) 0.2649(1) 0.018(1) Uij O43 0.3491(2) 0.2317(2) 0.2990(1) 0.018(1) Uij O44 0.0449(2) 0.4138(2) 0.1470(1) 0.016(1) Uij O45 0.1320(2) 0.3585(2) 0.0419(1) 0.020(1) Uij O46 0.2900(2) 0.4221(2) 0.0764(1) 0.016(1) Uij O61 0.4428(2) 0.3017(2) 0.1943(1) 0.023(1) Uij O62 0.6382(2) 0.2460(2) 0.2610(1) 0.028(1) Uij O63 0.8493(2) 0.2370(2) 0.2988(1) 0.018(1) Uij O64 0.5342(2) 0.4157(2) 0.1520(1) 0.018(1) Uij O65 0.6240(2) 0.3994(2) 0.0420(1) 0.026(1) Uij O66 0.7830(2) 0.4456(2) 0.0883(1) 0.020(1) Uij C1 0.7817(2) 0.7538(2) 0.2072(2) 0.014(2) Uij C2 0.8750(2) 0.6958(2) 0.2277(2) 0.015(2) Uij C3 0.9396(2) 0.6962(2) 0.1813(2) 0.015(2) Uij C4 0.8952(2) 0.7578(2) 0.1285(2) 0.016(2) Uij C5 0.9649(3) 0.8424(2) 0.1185(2) 0.018(2) Uij C6 0.8680(3) 0.7037(2) 0.0665(2) 0.015(2) Uij C7 0.9479(3) 0.6409(3) -0.0225(2) 0.021(2) Uij C8 1.0472(3) 0.5862(3) -0.0299(2) 0.025(2) Uij C9 0.9853(3) 0.7591(2) 0.3855(2) 0.018(2) Uij C10 1.0261(4) 0.8352(3) 0.3426(2) 0.035(2) Uij C11 1.0593(4) 0.7545(3) 0.4467(2) 0.036(2) Uij C12 0.8742(3) 0.7870(3) 0.4016(2) 0.035(2) Uij C13 0.9558(3) 0.5323(2) 0.3806(2) 0.018(2) Uij C14 1.0408(3) 0.5095(3) 0.4352(2) 0.028(2) Uij C15 0.8464(3) 0.5340(3) 0.4065(2) 0.036(2) Uij C16 0.9593(4) 0.4571(3) 0.3297(2) 0.032(2) Uij C21 0.2723(3) 0.7534(2) 0.2002(2) 0.014(2) Uij C22 0.3765(3) 0.7206(2) 0.2296(2) 0.016(2) Uij C23 0.4490(3) 0.7382(3) 0.1895(2) 0.016(2) Uij C24 0.3961(3) 0.7814(2) 0.1299(2) 0.016(2) Uij C25 0.4392(3) 0.8764(3) 0.1144(2) 0.022(2) Uij C26 0.4009(3) 0.7118(3) 0.0750(2) 0.018(2) Uij C27 0.5226(3) 0.6389(3) 0.0099(2) 0.026(2) Uij C28 0.4873(3) 0.6694(3) -0.0561(2) 0.033(2) Uij C29 0.4864(3) 0.7704(2) 0.3944(2) 0.018(2) Uij C30 0.5322(3) 0.8491(3) 0.3560(2) 0.031(2) Uij C31 0.5579(3) 0.7572(3) 0.4560(2) 0.032(2) Uij C32 0.3752(3) 0.7991(3) 0.4102(2) 0.035(2) Uij C33 0.4476(3) 0.5456(3) 0.3767(2) 0.018(2) Uij C34 0.5343(3) 0.5131(3) 0.4275(2) 0.030(2) Uij C35 0.3412(3) 0.5475(3) 0.4059(2) 0.033(2) Uij C36 0.4414(4) 0.4762(3) 0.3212(2) 0.044(3) Uij C41 0.0306(3) 0.3435(2) 0.1882(2) 0.014(2) Uij C42 0.1351(2) 0.3171(2) 0.2201(2) 0.014(2) Uij C43 0.2089(3) 0.3690(2) 0.1972(2) 0.014(2) Uij C44 0.1571(2) 0.4320(2) 0.1466(2) 0.013(2) Uij C45 0.1783(3) 0.5345(2) 0.1586(2) 0.019(2) Uij C46 0.1892(2) 0.3989(2) 0.0810(2) 0.013(2) Uij C47 0.3358(3) 0.3929(2) 0.0181(2) 0.016(2) Uij C48 0.3022(3) 0.4576(3) -0.0359(2) 0.020(2) Uij C49 0.2029(3) 0.1629(3) 0.3786(2) 0.019(2) Uij C50 0.2095(4) 0.2589(3) 0.4103(2) 0.037(3) Uij C51 0.2842(3) 0.0997(3) 0.4160(2) 0.032(2) Uij C52 0.0912(3) 0.1230(4) 0.3825(2) 0.041(3) Uij C53 0.2325(3) 0.0782(2) 0.2378(2) 0.021(2) Uij C54 0.3079(5) 0.0016(3) 0.2646(2) 0.054(3) Uij C55 0.1211(4) 0.0380(5) 0.2229(3) 0.075(4) Uij C56 0.2714(4) 0.1114(3) 0.1743(2) 0.036(3) Uij C61 0.5261(3) 0.3405(2) 0.1892(2) 0.016(2) Uij C62 0.6317(3) 0.3172(2) 0.2206(2) 0.015(2) Uij C63 0.7019(3) 0.3761(2) 0.2009(2) 0.015(2) Uij C64 0.6448(2) 0.4428(2) 0.1542(2) 0.014(2) Uij C65 0.6557(3) 0.5436(3) 0.1732(2) 0.025(2) Uij C66 0.6800(3) 0.4258(2) 0.0873(2) 0.015(2) Uij C67 0.8333(3) 0.4206(3) 0.0309(2) 0.025(2) Uij C68 0.8509(3) 0.3180(3) 0.0278(2) 0.031(2) Uij C69 0.7037(3) 0.1673(3) 0.3783(2) 0.022(2) Uij C70 0.7089(6) 0.2635(4) 0.4084(3) 0.073(4) Uij C71 0.7850(4) 0.1049(5) 0.4171(2) 0.062(4) Uij C72 0.5937(3) 0.1262(3) 0.3826(2) 0.031(2) Uij C73 0.7428(3) 0.0770(3) 0.2406(2) 0.022(2) Uij C74 0.8212(4) 0.0045(3) 0.2688(3) 0.048(3) Uij C75 0.6345(3) 0.0301(3) 0.2255(2) 0.035(2) Uij C76 0.7819(4) 0.1123(4) 0.1776(2) 0.046(3) Uij H3o 1.1278(30) 0.6805(31) 0.2938(18) 0.027(11) Uiso H23o 0.6295(32) 0.6891(31) 0.2977(19) 0.029(12) Uiso H43o 0.3708(29) 0.2339(27) 0.2677(18) 0.012(11) Uiso H63o 0.8676(37) 0.2399(35) 0.2708(21) 0.035(16) Uiso H3 1.0044 0.6623 0.1818 0.018 Uiso H5a 1.0304 0.8210 0.1049 0.021 Uiso H5b 0.9777 0.8758 0.1576 0.021 Uiso H5c 0.9304 0.8820 0.0868 0.021 Uiso H7a 0.9404 0.6892 -0.0536 0.025 Uiso H7b 0.8876 0.6010 -0.0276 0.025 Uiso H8a 1.0404 0.5601 -0.0717 0.030 Uiso H8b 1.0546 0.5378 0.0012 0.030 Uiso H8c 1.1075 0.6260 -0.0248 0.030 Uiso H10a 1.0271 0.8925 0.3654 0.042 Uiso H10b 0.9802 0.8403 0.3042 0.042 Uiso H10c 1.0959 0.8202 0.3324 0.042 Uiso H11a 1.0603 0.8118 0.4695 0.044 Uiso H11b 1.1292 0.7409 0.4362 0.044 Uiso H11c 1.0358 0.7063 0.4732 0.044 Uiso H12a 0.8752 0.8443 0.4244 0.042 Uiso H12b 0.8470 0.7395 0.4272 0.042 Uiso H12c 0.8293 0.7935 0.3630 0.042 Uiso H14a 1.0268 0.4522 0.4556 0.033 Uiso H14b 1.0425 0.5583 0.4660 0.033 Uiso H14c 1.1079 0.5054 0.4183 0.033 Uiso H15a 0.8325 0.4767 0.4269 0.044 Uiso H15b 0.7935 0.5439 0.3720 0.044 Uiso H15c 0.8443 0.5834 0.4366 0.044 Uiso H16a 0.9454 0.3999 0.3501 0.039 Uiso H16b 1.0275 0.4556 0.3139 0.039 Uiso H16c 0.9066 0.4687 0.2953 0.039 Uiso H23 0.5229 0.7255 0.1972 0.019 Uiso H25a 0.5118 0.8703 0.1064 0.026 Uiso H25b 0.4336 0.9173 0.1495 0.026 Uiso H25c 0.3996 0.9009 0.0774 0.026 Uiso H27a 0.4864 0.5829 0.0188 0.031 Uiso H27b 0.5970 0.6276 0.0130 0.031 Uiso H28a 0.5019 0.6235 -0.0868 0.040 Uiso H28b 0.5234 0.7254 -0.0650 0.040 Uiso H28c 0.4128 0.6807 -0.0591 0.040 Uiso H30a 0.5348 0.9036 0.3818 0.038 Uiso H30b 0.4879 0.8596 0.3175 0.038 Uiso H30c 0.6018 0.8332 0.3459 0.038 Uiso H31a 0.5605 0.8117 0.4819 0.038 Uiso H31b 0.6278 0.7429 0.4456 0.038 Uiso H31c 0.5314 0.7069 0.4794 0.038 Uiso H32a 0.3777 0.8536 0.4361 0.042 Uiso H32b 0.3448 0.7496 0.4325 0.042 Uiso H32c 0.3323 0.8111 0.3714 0.042 Uiso H34a 0.5172 0.4541 0.4444 0.036 Uiso H34b 0.5413 0.5575 0.4612 0.036 Uiso H34c 0.5997 0.5082 0.4086 0.036 Uiso H35a 0.3241 0.4884 0.4228 0.040 Uiso H35b 0.2869 0.5646 0.3736 0.040 Uiso H35c 0.3447 0.5923 0.4393 0.040 Uiso H36a 0.4243 0.4172 0.3382 0.053 Uiso H36b 0.5079 0.4730 0.3035 0.053 Uiso H36c 0.3877 0.4947 0.2889 0.053 Uiso H43 0.2828 0.3669 0.2106 0.017 Uiso H45a 0.2522 0.5465 0.1583 0.023 Uiso H45b 0.1559 0.5513 0.1990 0.023 Uiso H45c 0.1400 0.5702 0.1260 0.023 Uiso H47a 0.3122 0.3316 0.0071 0.020 Uiso H47b 0.4112 0.3934 0.0255 0.020 Uiso H48a 0.3320 0.4386 -0.0738 0.024 Uiso H48b 0.3258 0.5190 -0.0249 0.024 Uiso H48c 0.2268 0.4571 -0.0433 0.024 Uiso H50a 0.1933 0.2503 0.4532 0.044 Uiso H50b 0.1596 0.3002 0.3885 0.044 Uiso H50c 0.2792 0.2838 0.4095 0.044 Uiso H51a 0.2680 0.0911 0.4590 0.038 Uiso H51b 0.3527 0.1274 0.4163 0.038 Uiso H51c 0.2845 0.0407 0.3955 0.038 Uiso H52a 0.0749 0.1143 0.4254 0.049 Uiso H52b 0.0866 0.0645 0.3611 0.049 Uiso H52c 0.0408 0.1649 0.3618 0.049 Uiso H54a 0.3067 -0.0499 0.2360 0.065 Uiso H54b 0.2866 -0.0187 0.3046 0.065 Uiso H54c 0.3781 0.0259 0.2705 0.065 Uiso H55a 0.1200 -0.0136 0.1945 0.090 Uiso H55b 0.0760 0.0854 0.2041 0.090 Uiso H55c 0.0954 0.0180 0.2619 0.090 Uiso H56a 0.2702 0.0598 0.1457 0.043 Uiso H56b 0.3418 0.1348 0.1816 0.043 Uiso H56c 0.2258 0.1592 0.1563 0.043 Uiso H63 0.7760 0.3764 0.2140 0.018 Uiso H65a 0.7283 0.5614 0.1746 0.030 Uiso H65b 0.6309 0.5522 0.2142 0.030 Uiso H65c 0.6148 0.5810 0.1427 0.030 Uiso H67a 0.8999 0.4517 0.0315 0.030 Uiso H67b 0.7887 0.4397 -0.0057 0.030 Uiso H68a 0.8837 0.3018 -0.0097 0.037 Uiso H68b 0.7843 0.2870 0.0272 0.037 Uiso H68c 0.8955 0.2990 0.0644 0.037 Uiso H70a 0.6914 0.2566 0.4513 0.087 Uiso H70b 0.6593 0.3039 0.3855 0.087 Uiso H70c 0.7785 0.2885 0.4080 0.087 Uiso H71a 0.7675 0.0980 0.4599 0.074 Uiso H71b 0.8535 0.1323 0.4174 0.074 Uiso H71c 0.7855 0.0452 0.3975 0.074 Uiso H72a 0.5762 0.1193 0.4254 0.037 Uiso H72b 0.5910 0.0666 0.3627 0.037 Uiso H72c 0.5427 0.1662 0.3605 0.037 Uiso H74a 0.8236 -0.0483 0.2416 0.058 Uiso H74b 0.8003 -0.0151 0.3091 0.058 Uiso H74c 0.8900 0.0318 0.2746 0.058 Uiso H75a 0.6369 -0.0227 0.1983 0.042 Uiso H75b 0.5867 0.0744 0.2052 0.042 Uiso H75c 0.6090 0.0107 0.2647 0.042 Uiso H76a 0.7843 0.0595 0.1504 0.055 Uiso H76b 0.8507 0.1390 0.1854 0.055 Uiso H76c 0.7340 0.1576 0.1585 0.055 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Si1 0.0111(4) 0.0132(5) 0.0128(4) -0.0005(3) 0.0020(4) 0.0014(4) Si2 0.0131(4) 0.0137(5) 0.0124(4) -0.0006(3) 0.0019(4) 0.0016(3) Si3 0.0102(4) 0.0103(4) 0.0143(4) 0.0001(4) 0.0014(3) 0.0027(4) Si4 0.0110(4) 0.0108(4) 0.0139(4) -0.0003(4) 0.0022(3) 0.0025(4) O1 0.011(1) 0.019(1) 0.021(1) 0.000(1) 0.004(1) -0.002(1) O2 0.012(1) 0.020(1) 0.015(1) 0.000(1) 0.001(1) 0.003(1) O3 0.016(1) 0.017(1) 0.021(1) -0.001(1) 0.006(1) 0.002(1) O4 0.013(1) 0.019(1) 0.017(1) 0.005(1) 0.005(1) 0.003(1) O5 0.012(1) 0.027(1) 0.029(1) -0.002(1) -0.001(1) -0.003(1) O6 0.014(1) 0.024(1) 0.019(1) 0.000(1) 0.005(1) -0.003(1) O21 0.011(1) 0.022(1) 0.022(1) -0.001(1) 0.004(1) 0.002(1) O22 0.016(1) 0.033(1) 0.015(1) -0.003(1) 0.001(1) 0.009(1) O23 0.016(1) 0.016(1) 0.018(1) 0.000(1) 0.006(1) 0.001(1) O24 0.013(1) 0.022(1) 0.016(1) 0.002(1) 0.002(1) 0.005(1) O25 0.015(1) 0.025(1) 0.024(1) -0.006(1) 0.002(1) -0.008(1) O26 0.012(1) 0.035(2) 0.021(1) -0.010(1) 0.004(1) -0.011(1) O41 0.010(1) 0.028(1) 0.021(1) -0.005(1) 0.002(1) 0.008(1) O42 0.016(1) 0.017(1) 0.020(1) 0.003(1) 0.003(1) 0.010(1) O43 0.013(1) 0.019(1) 0.020(1) -0.006(1) 0.001(1) 0.002(1) O44 0.011(1) 0.021(1) 0.017(1) 0.003(1) 0.003(1) 0.009(1) O45 0.016(1) 0.018(1) 0.026(1) -0.002(1) 0.004(1) -0.005(1) O46 0.011(1) 0.021(1) 0.016(1) 0.000(1) 0.003(1) -0.001(1) O61 0.013(1) 0.027(1) 0.030(1) -0.002(1) 0.007(1) 0.007(1) O62 0.019(1) 0.024(1) 0.041(2) 0.004(1) 0.008(1) 0.022(1) O63 0.016(1) 0.020(1) 0.018(1) -0.006(1) 0.005(1) 0.000(1) O64 0.014(1) 0.023(1) 0.017(1) 0.002(1) 0.004(1) 0.007(1) O65 0.017(1) 0.044(2) 0.018(1) -0.004(1) 0.001(1) -0.001(1) O66 0.015(1) 0.019(1) 0.026(1) -0.007(1) 0.006(1) 0.001(1) C1 0.010(2) 0.017(2) 0.016(2) -0.004(1) 0.002(1) -0.001(1) C2 0.013(2) 0.020(2) 0.013(2) -0.003(1) 0.001(1) 0.001(1) C3 0.013(2) 0.017(2) 0.015(2) -0.001(1) -0.001(1) 0.002(1) C4 0.008(2) 0.018(2) 0.020(2) 0.003(1) 0.003(1) 0.000(1) C5 0.015(2) 0.017(2) 0.020(2) -0.004(1) 0.002(1) 0.001(1) C6 0.014(2) 0.017(2) 0.014(2) 0.000(1) 0.000(1) 0.007(1) C7 0.028(2) 0.018(2) 0.017(2) 0.004(2) 0.004(2) 0.000(1) C8 0.030(2) 0.015(2) 0.031(2) 0.006(2) 0.010(2) 0.001(2) C9 0.025(2) 0.009(2) 0.021(2) -0.001(1) 0.005(1) -0.001(1) C10 0.052(3) 0.013(2) 0.043(3) 0.000(2) 0.018(2) 0.000(2) C11 0.051(3) 0.019(2) 0.038(2) -0.005(2) -0.006(2) -0.005(2) C12 0.035(2) 0.029(2) 0.041(2) 0.004(2) 0.012(2) -0.014(2) C13 0.018(2) 0.019(2) 0.017(2) -0.005(1) 0.001(1) 0.004(1) C14 0.027(2) 0.024(2) 0.032(2) -0.004(2) -0.003(2) 0.015(2) C15 0.023(2) 0.036(2) 0.053(3) 0.000(2) 0.012(2) 0.019(2) C16 0.048(3) 0.013(2) 0.035(2) -0.011(2) 0.003(2) -0.001(2) C21 0.014(2) 0.014(2) 0.014(2) -0.004(1) -0.001(1) 0.000(1) C22 0.016(2) 0.019(2) 0.014(2) -0.003(1) -0.001(1) 0.002(1) C23 0.013(2) 0.023(2) 0.012(2) -0.004(1) -0.001(1) -0.001(1) C24 0.016(2) 0.018(2) 0.015(2) -0.003(1) 0.000(1) -0.001(1) C25 0.026(2) 0.024(2) 0.018(2) -0.011(2) 0.006(2) -0.001(1) C26 0.013(2) 0.028(2) 0.013(2) -0.002(1) 0.001(1) 0.005(1) C27 0.015(2) 0.037(2) 0.028(2) -0.006(2) 0.006(2) -0.007(2) C28 0.033(2) 0.040(2) 0.029(2) -0.010(2) 0.009(2) -0.008(2) C29 0.026(2) 0.011(2) 0.019(2) 0.001(1) 0.004(1) -0.001(1) C30 0.045(3) 0.019(2) 0.033(2) -0.004(2) 0.013(2) -0.003(2) C31 0.046(3) 0.020(2) 0.028(2) -0.001(2) -0.007(2) -0.003(2) C32 0.037(2) 0.027(2) 0.044(3) 0.009(2) 0.018(2) -0.006(2) C33 0.018(2) 0.023(2) 0.015(2) -0.006(1) 0.005(1) 0.004(1) C34 0.026(2) 0.019(2) 0.045(3) 0.001(2) 0.000(2) 0.016(2) C35 0.024(2) 0.032(2) 0.045(3) 0.001(2) 0.011(2) 0.021(2) C36 0.075(4) 0.024(2) 0.034(3) -0.021(2) 0.013(2) -0.004(2) C41 0.017(2) 0.011(2) 0.014(2) 0.000(1) 0.003(1) 0.001(1) C42 0.007(2) 0.019(2) 0.015(2) 0.000(1) 0.000(1) 0.003(1) C43 0.013(2) 0.009(1) 0.019(2) 0.000(1) 0.001(1) 0.002(1) C44 0.010(2) 0.011(2) 0.017(2) -0.001(1) 0.001(1) 0.003(1) C45 0.019(2) 0.017(2) 0.022(2) 0.001(1) 0.008(2) -0.005(1) C46 0.010(2) 0.011(2) 0.019(2) 0.000(1) 0.002(1) -0.001(1) C47 0.014(2) 0.019(2) 0.018(2) -0.001(1) 0.007(1) -0.001(1) C48 0.018(2) 0.022(2) 0.019(2) 0.002(1) 0.003(1) -0.001(1) C49 0.017(2) 0.023(2) 0.017(2) -0.001(1) 0.001(1) 0.005(1) C50 0.053(3) 0.043(3) 0.015(2) 0.007(2) 0.008(2) -0.002(2) C51 0.032(2) 0.041(2) 0.021(2) 0.008(2) 0.000(2) 0.014(2) C52 0.019(2) 0.075(3) 0.028(2) -0.014(2) 0.001(2) 0.025(2) C53 0.017(2) 0.016(2) 0.031(2) -0.004(1) 0.004(2) -0.008(2) C54 0.098(4) 0.026(2) 0.041(3) 0.023(3) 0.022(3) -0.002(2) C55 0.043(3) 0.087(4) 0.098(5) -0.038(3) 0.025(3) -0.069(4) C56 0.068(3) 0.023(2) 0.017(2) 0.005(2) 0.003(2) -0.003(2) C61 0.017(2) 0.016(2) 0.016(2) 0.002(1) 0.007(1) -0.002(1) C62 0.009(2) 0.013(2) 0.023(2) 0.001(1) 0.004(1) 0.004(1) C63 0.015(2) 0.013(2) 0.017(2) -0.001(1) 0.000(1) 0.004(1) C64 0.012(2) 0.012(2) 0.019(2) 0.001(1) 0.000(1) 0.002(1) C65 0.040(2) 0.013(2) 0.023(2) -0.002(2) 0.011(2) -0.003(2) C66 0.012(2) 0.010(2) 0.023(2) 0.001(1) 0.002(1) 0.005(1) C67 0.015(2) 0.037(2) 0.026(2) -0.005(2) 0.010(2) 0.004(2) C68 0.020(2) 0.046(3) 0.026(2) 0.005(2) 0.008(2) -0.012(2) C69 0.019(2) 0.032(2) 0.016(2) -0.010(2) 0.004(1) -0.002(2) C70 0.125(5) 0.058(4) 0.043(3) -0.033(4) 0.052(3) -0.027(3) C71 0.035(3) 0.127(5) 0.024(3) 0.012(3) 0.004(2) 0.035(3) C72 0.025(2) 0.045(3) 0.024(2) -0.008(2) 0.007(2) 0.007(2) C73 0.018(2) 0.021(2) 0.028(2) -0.008(1) 0.007(2) -0.011(2) C74 0.039(3) 0.021(2) 0.086(4) 0.005(2) 0.006(3) -0.021(2) C75 0.034(2) 0.037(2) 0.035(2) -0.020(2) 0.003(2) -0.017(2) C76 0.050(3) 0.060(3) 0.031(2) -0.028(2) 0.018(2) -0.024(2) #================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Si1 O3 1.623(2) Si1 O2 1.685(2) Si1 C13 1.878(4) Si1 C9 1.883(4) Si2 O23 1.616(2) Si2 O22 1.679(2) Si2 C33 1.879(4) Si2 C29 1.884(4) Si3 O43 1.618(2) Si3 O42 1.674(2) Si3 C49 1.870(3) Si3 C53 1.875(4) Si4 O63 1.615(3) Si4 O62 1.667(3) Si4 C69 1.868(4) Si4 C73 1.868(4) O1 C1 1.210(4) O2 C2 1.330(4) O4 C1 1.348(4) O4 C4 1.450(4) O5 C6 1.194(4) O6 C6 1.335(4) O6 C7 1.458(4) O21 C21 1.207(4) O22 C22 1.329(4) O24 C21 1.358(4) O24 C24 1.444(4) O25 C26 1.192(4) O26 C26 1.338(4) O26 C27 1.464(4) O41 C41 1.205(4) O42 C42 1.331(4) O44 C41 1.352(4) O44 C44 1.441(4) O45 C46 1.192(4) O46 C46 1.327(4) O46 C47 1.460(4) O61 C61 1.203(4) O62 C62 1.325(4) O64 C61 1.340(4) O64 C64 1.446(4) O65 C66 1.193(4) O66 C66 1.330(4) O66 C67 1.456(4) C1 C2 1.473(4) C2 C3 1.326(4) C3 C4 1.486(4) C4 C6 1.526(5) C4 C5 1.523(5) C7 C8 1.499(5) C9 C11 1.519(5) C9 C12 1.526(5) C9 C10 1.533(5) C13 C16 1.521(5) C13 C14 1.530(5) C13 C15 1.530(5) C21 C22 1.477(5) C22 C23 1.324(5) C23 C24 1.495(5) C24 C25 1.513(5) C24 C26 1.530(5) C27 C28 1.481(6) C29 C31 1.519(5) C29 C32 1.529(5) C29 C30 1.531(5) C33 C34 1.529(5) C33 C36 1.528(5) C33 C35 1.526(5) C41 C42 1.472(4) C42 C43 1.317(4) C43 C44 1.498(4) C44 C45 1.510(5) C44 C46 1.543(5) C47 C48 1.495(5) C49 C50 1.527(6) C49 C52 1.530(5) C49 C51 1.531(5) C53 C54 1.526(6) C53 C55 1.526(6) C53 C56 1.537(6) C61 C62 1.470(5) C62 C63 1.318(4) C63 C64 1.504(4) C64 C65 1.502(5) C64 C66 1.529(5) C67 C68 1.490(6) C69 C70 1.515(6) C69 C72 1.520(5) C69 C71 1.536(6) C73 C74 1.518(6) C73 C75 1.531(5) C73 C76 1.537(6) C3 H3 0.95 C5 H5b 0.95 C5 H5a 0.95 C5 H5c 0.95 C7 H7a 0.95 C7 H7b 0.95 C8 H8c 0.95 C8 H8a 0.95 C8 H8b 0.95 C10 H10a 0.95 C10 H10c 0.95 C10 H10b 0.95 C11 H11c 0.95 C11 H11b 0.95 C11 H11a 0.95 C12 H12c 0.95 C12 H12b 0.95 C12 H12a 0.95 C14 H14a 0.95 C14 H14c 0.95 C14 H14b 0.95 C15 H15c 0.95 C15 H15a 0.95 C15 H15b 0.95 C16 H16b 0.95 C16 H16a 0.95 C16 H16c 0.95 C23 H23 0.95 C25 H25c 0.95 C25 H25a 0.95 C25 H25b 0.95 C27 H27a 0.95 C27 H27b 0.95 C28 H28a 0.95 C28 H28b 0.95 C28 H28c 0.95 C30 H30c 0.95 C30 H30a 0.95 C30 H30b 0.95 C31 H31a 0.95 C31 H31c 0.95 C31 H31b 0.95 C32 H32c 0.95 C32 H32a 0.95 C32 H32b 0.95 C34 H34c 0.95 C34 H34b 0.95 C34 H34a 0.95 C35 H35c 0.95 C35 H35a 0.95 C35 H35b 0.95 C36 H36a 0.95 C36 H36b 0.95 C36 H36c 0.95 C43 H43 0.95 C45 H45a 0.95 C45 H45b 0.95 C45 H45c 0.95 C47 H47b 0.95 C47 H47a 0.95 C48 H48a 0.95 C48 H48b 0.95 C48 H48c 0.95 C50 H50b 0.95 C50 H50c 0.95 C50 H50a 0.95 C51 H51c 0.95 C51 H51a 0.95 C51 H51b 0.95 C52 H52c 0.95 C52 H52b 0.95 C52 H52a 0.95 C54 H54b 0.95 C54 H54a 0.95 C54 H54c 0.95 C55 H55c 0.95 C55 H55a 0.95 C55 H55b 0.95 C56 H56c 0.95 C56 H56b 0.95 C56 H56a 0.95 C63 H63 0.95 C65 H65a 0.95 C65 H65b 0.95 C65 H65c 0.95 C67 H67b 0.95 C67 H67a 0.95 C68 H68c 0.95 C68 H68a 0.95 C68 H68b 0.95 C70 H70b 0.95 C70 H70c 0.95 C70 H70a 0.95 C71 H71c 0.95 C71 H71b 0.95 C71 H71a 0.95 C72 H72c 0.95 C72 H72b 0.95 C72 H72a 0.95 C74 H74a 0.95 C74 H74b 0.95 C74 H74c 0.95 C75 H75a 0.95 C75 H75c 0.95 C75 H75b 0.95 C76 H76c 0.95 C76 H76a 0.95 C76 H76b 0.95 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O2 Si1 O3 110.5(1) O3 Si1 C13 106.4(1) O3 Si1 C9 110.9(1) O2 Si1 C13 101.8(1) O2 Si1 C9 105.7(1) C9 Si1 C13 121.0(2) O22 Si2 O23 111.3(1) O23 Si2 C33 105.4(1) O23 Si2 C29 111.5(1) O22 Si2 C33 102.8(1) O22 Si2 C29 104.5(2) C29 Si2 C33 121.0(2) O42 Si3 O43 111.5(1) O43 Si3 C49 105.5(2) O43 Si3 C53 111.1(2) O42 Si3 C49 102.1(1) O42 Si3 C53 106.1(2) C49 Si3 C53 120.2(2) O62 Si4 O63 111.5(1) O63 Si4 C69 105.6(2) O63 Si4 C73 111.0(2) O62 Si4 C69 102.7(2) O62 Si4 C73 105.1(2) C69 Si4 C73 120.5(2) Si1 O2 C2 128.0(2) C1 O4 C4 109.3(2) C6 O6 C7 116.7(3) Si2 O22 C22 131.5(2) C21 O24 C24 108.9(2) C26 O26 C27 116.7(3) Si3 O42 C42 131.1(2) C41 O44 C44 109.1(2) C46 O46 C47 116.4(3) Si4 O62 C62 134.3(2) C61 O64 C64 108.8(3) C66 O66 C67 115.8(3) O1 C1 O4 122.2(3) O1 C1 C2 129.2(3) O4 C1 C2 108.6(3) O2 C2 C3 132.7(3) C1 C2 C3 108.2(3) O2 C2 C1 119.0(3) C2 C3 C4 109.5(3) O4 C4 C3 104.3(3) O4 C4 C6 106.6(3) O4 C4 C5 108.3(3) C3 C4 C6 111.9(3) C3 C4 C5 113.1(3) C5 C4 C6 112.0(3) O5 C6 O6 125.5(3) O5 C6 C4 125.6(3) O6 C6 C4 108.9(3) O6 C7 C8 107.2(3) C11 C9 C12 109.3(3) C10 C9 C11 108.3(3) Si1 C9 C11 111.5(2) C10 C9 C12 108.0(3) Si1 C9 C12 111.6(3) Si1 C9 C10 108.0(3) C14 C13 C16 108.1(3) C15 C13 C16 110.3(3) Si1 C13 C16 106.0(2) C14 C13 C15 109.4(3) Si1 C13 C14 112.1(2) Si1 C13 C15 110.9(3) O21 C21 O24 121.8(3) O21 C21 C22 129.5(3) O24 C21 C22 108.7(3) O22 C22 C23 133.8(3) O22 C22 C21 117.9(3) C21 C22 C23 108.3(3) C22 C23 C24 109.1(3) O24 C24 C23 104.9(3) O24 C24 C25 109.1(3) O24 C24 C26 107.4(3) C23 C24 C25 114.2(3) C23 C24 C26 108.3(3) C25 C24 C26 112.6(3) O25 C26 O26 125.8(3) O25 C26 C24 124.9(3) O26 C26 C24 109.2(3) O26 C27 C28 111.6(3) C31 C29 C32 109.6(3) C30 C29 C31 108.4(3) Si2 C29 C31 111.7(2) C30 C29 C32 108.4(3) Si2 C29 C32 111.2(3) Si2 C29 C30 107.5(2) C34 C33 C36 108.4(3) C34 C33 C35 109.0(3) Si2 C33 C34 111.1(2) C35 C33 C36 109.3(3) Si2 C33 C36 107.0(2) Si2 C33 C35 111.9(3) O41 C41 O44 122.3(3) O41 C41 C42 129.3(3) O44 C41 C42 108.4(3) O42 C42 C43 133.7(3) C41 C42 C43 108.9(3) O42 C42 C41 117.5(3) C42 C43 C44 108.8(3) O44 C44 C43 104.6(2) O44 C44 C45 109.5(3) O44 C44 C46 106.8(3) C43 C44 C45 114.1(3) C43 C44 C46 108.2(3) C45 C44 C46 113.0(3) O45 C46 O46 126.5(3) O45 C46 C44 124.8(3) O46 C46 C44 108.6(3) O46 C47 C48 110.5(3) C50 C49 C52 109.2(3) C50 C49 C51 107.6(3) Si3 C49 C50 106.6(2) C51 C49 C52 109.3(3) Si3 C49 C52 112.2(2) Si3 C49 C51 111.7(3) C54 C53 C55 109.7(4) C54 C53 C56 107.7(3) Si3 C53 C54 110.7(3) C55 C53 C56 107.6(4) Si3 C53 C55 112.5(3) Si3 C53 C56 108.5(2) O61 C61 O64 122.5(3) O61 C61 C62 128.3(3) O64 C61 C62 109.2(3) O62 C62 C63 133.6(3) C61 C62 C63 108.8(3) O62 C62 C61 117.5(3) C62 C63 C64 108.3(3) O64 C64 C65 109.3(3) O64 C64 C63 104.8(3) O64 C64 C66 106.8(3) C63 C64 C65 114.3(3) C65 C64 C66 111.7(3) C63 C64 C66 109.5(3) O65 C66 O66 126.0(3) O65 C66 C64 125.5(3) O66 C66 C64 108.5(3) O66 C67 C68 110.9(3) C70 C69 C72 109.5(4) C70 C69 C71 108.0(4) Si4 C69 C70 107.1(3) C71 C69 C72 108.3(4) Si4 C69 C72 112.8(2) Si4 C69 C71 111.1(3) C74 C73 C75 108.6(3) C74 C73 C76 108.1(4) Si4 C73 C74 111.5(3) C75 C73 C76 108.5(3) Si4 C73 C75 113.4(3) Si4 C73 C76 106.5(3) Si1 O3 H3o 119.4(26) Si2 O23 H23o 125.4(28) Si3 O43 H43o 111.4(30) Si4 O63 H63o 111.3(40) C2 C3 H3 125.2 C4 C3 H3 125.2 H5a C5 H5b 109.8 H5b C5 H5c 109.5 C4 C5 H5b 109.7 H5a C5 H5c 109.8 C4 C5 H5a 108.3 C4 C5 H5c 109.7 H7a C7 H7b 109.5 O6 C7 H7a 110.0 C8 C7 H7a 110.0 O6 C7 H7b 110.0 C8 C7 H7b 110.1 H8a C8 H8c 110.1 H8b C8 H8c 109.5 C7 C8 H8c 110.1 H8a C8 H8b 110.0 C7 C8 H8a 107.2 C7 C8 H8b 110.0 H10a C10 H10c 109.8 H10a C10 H10b 109.9 C9 C10 H10a 108.0 H10b C10 H10c 109.5 C9 C10 H10c 109.8 C9 C10 H10b 109.8 H11b C11 H11c 109.5 H11a C11 H11c 109.0 C9 C11 H11c 109.0 H11a C11 H11b 109.0 C9 C11 H11b 109.0 C9 C11 H11a 111.5 H12b C12 H12c 109.5 H12a C12 H12c 108.9 C9 C12 H12c 108.9 H12a C12 H12b 108.9 C9 C12 H12b 109.0 C9 C12 H12a 111.6 H14a C14 H14c 108.8 H14a C14 H14b 108.8 C13 C14 H14a 112.1 H14b C14 H14c 109.5 C13 C14 H14c 108.8 C13 C14 H14b 108.8 H15a C15 H15c 109.2 H15b C15 H15c 109.5 C13 C15 H15c 109.1 H15a C15 H15b 109.1 C13 C15 H15a 110.9 C13 C15 H15b 109.1 H16a C16 H16b 110.3 H16b C16 H16c 109.5 C13 C16 H16b 110.3 H16a C16 H16c 110.3 C13 C16 H16a 106.0 C13 C16 H16c 110.3 C22 C23 H23 125.4 C24 C23 H23 125.4 H25a C25 H25c 109.6 H25b C25 H25c 109.5 C24 C25 H25c 109.6 H25a C25 H25b 109.6 C24 C25 H25a 109.1 C24 C25 H25b 109.6 H27a C27 H27b 109.5 O26 C27 H27a 108.9 C28 C27 H27a 108.9 O26 C27 H27b 108.9 C28 C27 H27b 108.9 H28a C28 H28b 108.9 H28a C28 H28c 108.9 C27 C28 H28a 111.6 H28b C28 H28c 109.5 C27 C28 H28b 108.9 C27 C28 H28c 108.9 H30a C30 H30c 110.0 H30b C30 H30c 109.5 C29 C30 H30c 110.0 H30a C30 H30b 110.0 C29 C30 H30a 107.5 C29 C30 H30b 110.0 H31a C31 H31c 108.9 H31a C31 H31b 108.9 C29 C31 H31a 111.7 H31b C31 H31c 109.5 C29 C31 H31c 108.9 C29 C31 H31b 108.9 H32a C32 H32c 109.0 H32b C32 H32c 109.5 C29 C32 H32c 109.0 H32a C32 H32b 109.0 C29 C32 H32a 111.2 C29 C32 H32b 109.0 H34b C34 H34c 109.5 H34a C34 H34c 109.1 C33 C34 H34c 109.0 H34a C34 H34b 109.1 C33 C34 H34b 109.1 C33 C34 H34a 111.1 H35a C35 H35c 108.9 H35b C35 H35c 109.5 C33 C35 H35c 108.9 H35a C35 H35b 108.8 C33 C35 H35a 111.9 C33 C35 H35b 108.8 H36a C36 H36b 110.1 H36a C36 H36c 110.1 C33 C36 H36a 107.0 H36b C36 H36c 109.5 C33 C36 H36b 110.1 C33 C36 H36c 110.1 C42 C43 H43 125.6 C44 C43 H43 125.6 H45a C45 H45b 109.5 H45a C45 H45c 109.5 C44 C45 H45a 109.5 H45b C45 H45c 109.5 C44 C45 H45b 109.5 C44 C45 H45c 109.5 H47a C47 H47b 109.5 O46 C47 H47b 109.2 C48 C47 H47b 109.2 O46 C47 H47a 109.2 C48 C47 H47a 109.2 H48a C48 H48b 109.2 H48a C48 H48c 109.2 C47 C48 H48a 110.5 H48b C48 H48c 109.4 C47 C48 H48b 109.2 C47 C48 H48c 109.2 H50b C50 H50c 109.5 H50a C50 H50b 110.2 C49 C50 H50b 110.2 H50a C50 H50c 110.2 C49 C50 H50c 110.2 C49 C50 H50a 106.6 H51a C51 H51c 108.9 H51b C51 H51c 109.5 C49 C51 H51c 108.9 H51a C51 H51b 108.9 C49 C51 H51a 111.7 C49 C51 H51b 108.9 H52b C52 H52c 109.5 H52a C52 H52c 108.8 C49 C52 H52c 108.8 H52a C52 H52b 108.8 C49 C52 H52b 108.8 C49 C52 H52a 112.2 H54a C54 H54b 109.1 H54b C54 H54c 109.5 C53 C54 H54b 109.1 H54a C54 H54c 109.2 C53 C54 H54a 110.7 C53 C54 H54c 109.1 H55a C55 H55c 108.6 H55b C55 H55c 109.5 C53 C55 H55c 108.6 H55a C55 H55b 108.8 C53 C55 H55a 112.5 C53 C55 H55b 108.8 H56b C56 H56c 109.5 H56a C56 H56c 109.7 C53 C56 H56c 109.7 H56a C56 H56b 109.7 C53 C56 H56b 109.7 C53 C56 H56a 108.5 C62 C63 H63 125.8 C64 C63 H63 125.8 H65a C65 H65b 109.5 H65a C65 H65c 109.5 C64 C65 H65a 109.3 H65b C65 H65c 109.5 C64 C65 H65b 109.5 C64 C65 H65c 109.5 H67a C67 H67b 109.5 O66 C67 H67b 109.1 C68 C67 H67b 109.1 O66 C67 H67a 109.1 C68 C67 H67a 109.1 H68a C68 H68c 109.1 H68b C68 H68c 109.5 C67 C68 H68c 109.1 H68a C68 H68b 109.1 C67 C68 H68a 110.9 C67 C68 H68b 109.1 H70b C70 H70c 109.4 H70a C70 H70b 110.0 C69 C70 H70b 110.1 H70a C70 H70c 110.0 C69 C70 H70c 110.1 C69 C70 H70a 107.2 H71b C71 H71c 109.5 H71a C71 H71c 109.1 C69 C71 H71c 109.1 H71a C71 H71b 109.1 C69 C71 H71b 109.1 C69 C71 H71a 111.1 H72b C72 H72c 109.5 H72a C72 H72c 108.6 C69 C72 H72c 108.6 H72a C72 H72b 108.6 C69 C72 H72b 108.6 C69 C72 H72a 112.8 H74a C74 H74b 109.0 H74a C74 H74c 109.0 C73 C74 H74a 111.5 H74b C74 H74c 109.5 C73 C74 H74b 108.9 C73 C74 H74c 108.9 H75a C75 H75c 108.5 H75a C75 H75b 108.5 C73 C75 H75a 113.4 H75b C75 H75c 109.5 C73 C75 H75c 108.5 C73 C75 H75b 108.5 H76a C76 H76c 110.2 H76b C76 H76c 109.5 C73 C76 H76c 110.2 H76a C76 H76b 110.2 C73 C76 H76a 106.5 C73 C76 H76b 110.2 #loop_ #_publ_manuscript_incl_extra_item #'_geom_bond_atom_site_label_D' #'_geom_bond_atom_site_label_H' #'_geom_contact_atom_site_label_A' #'_geom_bond_distance_DH' #'_geom_contact_distance_HA' #'_geom_contact_distance_DA' #'_geom_angle_DHA' #'_geom_contact_site_symmetry_A' loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A O3 H3o O21 0.893(43) 2.030(42) 2.833(3) 149(4) 1_655 O23 H23o O1 0.837(43) 2.043(43) 2.841(3) 159(4) . O43 H43o O61 0.734(37) 2.097(39) 2.775(4) 154(4) . O63 H63o O41 0.651(45) 2.187(47) 2.786(4) 154(6) 1_655