+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 14:53:36 on 04-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in Pna2(1) CELL 0.71073 10.9732 12.7636 20.7212 90.000 90.000 90.000 ZERR 8.00 0.0022 0.0026 0.0041 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H O F UNIT 120 152 32 8 V = 2902.16 F(000) = 1200.0 Mu = 0.10 mm-1 Cell Wt = 2258.42 Rho = 1.292 SHEL 7 0.84 TEMP -123 SIZE 0.1 0.1 0.1 HTAB FMAP 2 PLAN 20 BOND L.S. 4 WGHT 0.0452 0.0000 EXTI 0.009994 FVAR 1.17737 MOLE 1 F1 4 0.905028 0.671179 0.359315 11.00000 0.10895 0.13139 = 0.12350 0.00823 0.00666 -0.05149 O1 3 0.070155 0.422881 0.357455 11.00000 0.06261 0.15613 = 0.08732 -0.00837 0.00699 0.00135 AFIX 147 H1 2 -0.001300 0.437117 0.345853 11.00000 -1.50000 AFIX 0 O2 3 0.323849 0.434825 0.370025 11.00000 0.07066 0.05916 = 0.07090 0.00504 -0.00944 -0.00284 O3 3 0.332533 0.402453 0.509607 11.00000 0.06961 0.09844 = 0.07059 0.00152 0.01580 0.00394 AFIX 147 H3 2 0.281594 0.450025 0.502055 11.00000 -1.50000 AFIX 0 O4 3 0.390694 0.593804 0.481472 11.00000 0.09082 0.08451 = 0.10487 -0.01714 0.01513 0.01930 C1 1 0.082233 0.364427 0.249838 11.00000 0.08565 0.11644 = 0.08067 -0.01756 -0.01122 -0.00601 AFIX 33 H1A 2 0.005201 0.399450 0.239479 11.00000 -1.50000 H1B 2 0.065619 0.293080 0.264937 11.00000 -1.50000 H1C 2 0.133534 0.361569 0.211165 11.00000 -1.50000 AFIX 0 C2 1 0.171205 0.537555 0.282238 11.00000 0.12295 0.08425 = 0.10385 0.01283 -0.03406 0.00217 AFIX 33 H2A 2 0.093388 0.571080 0.271648 11.00000 -1.50000 H2B 2 0.224140 0.538044 0.244148 11.00000 -1.50000 H2C 2 0.210734 0.576036 0.317406 11.00000 -1.50000 AFIX 0 C3 1 0.148642 0.425877 0.303055 11.00000 0.06738 0.08967 = 0.05578 -0.00194 0.00206 -0.00147 C4 1 0.267173 0.373982 0.320161 11.00000 0.06469 0.07498 = 0.06529 -0.00774 -0.00031 -0.00947 AFIX 13 H4 2 0.321181 0.374104 0.281290 11.00000 -1.20000 AFIX 0 C5 1 0.262938 0.263232 0.347865 11.00000 0.11405 0.06592 = 0.13065 0.00078 -0.03179 -0.00836 AFIX 23 H5A 2 0.180937 0.247898 0.365407 11.00000 -1.20000 H5B 2 0.281947 0.211113 0.313944 11.00000 -1.20000 AFIX 0 C6 1 0.355990 0.259181 0.400182 11.00000 0.08125 0.06133 = 0.08859 0.00347 0.00380 0.00803 AFIX 23 H6A 2 0.419132 0.206070 0.390471 11.00000 -1.20000 H6B 2 0.317694 0.241972 0.442122 11.00000 -1.20000 AFIX 0 C7 1 0.410900 0.368696 0.401542 11.00000 0.05936 0.06692 = 0.06546 -0.00357 0.00537 0.00553 AFIX 13 H7 2 0.488304 0.368666 0.376071 11.00000 -1.20000 AFIX 0 C8 1 0.435687 0.415073 0.468141 11.00000 0.05580 0.07509 = 0.05919 0.00550 0.00674 0.00970 AFIX 13 H8 2 0.506585 0.377430 0.487679 11.00000 -1.20000 AFIX 0 C9 1 0.467017 0.530532 0.463088 11.00000 0.06802 0.06986 = 0.06827 -0.00593 -0.00144 0.01087 C10 1 0.583204 0.564689 0.435734 11.00000 0.07101 0.06208 = 0.05964 -0.00110 -0.00950 0.00286 C11 1 0.679703 0.496465 0.423577 11.00000 0.06606 0.06430 = 0.07082 -0.00215 -0.00779 -0.00182 AFIX 43 H11 2 0.670918 0.424156 0.433398 11.00000 -1.20000 AFIX 0 C12 1 0.787899 0.532133 0.397500 11.00000 0.06606 0.08455 = 0.07643 -0.00423 -0.00297 -0.01179 AFIX 43 H12 2 0.852853 0.485085 0.388616 11.00000 -1.20000 AFIX 0 C13 1 0.799029 0.635220 0.384982 11.00000 0.07936 0.08996 = 0.08064 0.00443 -0.00617 -0.02591 C14 1 0.710044 0.706324 0.397555 11.00000 0.11998 0.07154 = 0.09456 0.01277 -0.01438 -0.01912 AFIX 43 H14 2 0.722480 0.778707 0.389145 11.00000 -1.20000 AFIX 0 C15 1 0.599633 0.670543 0.423175 11.00000 0.09630 0.07034 = 0.08109 0.00223 -0.00963 0.00932 AFIX 43 H15 2 0.535838 0.718786 0.431981 11.00000 -1.20000 AFIX 0 MOLE 2 F2 4 0.876365 1.192674 0.098789 11.00000 0.10232 0.10340 = 0.15008 -0.00220 -0.01099 -0.03384 O5 3 0.077781 0.928188 0.138212 11.00000 0.06609 0.10140 = 0.07118 -0.00904 -0.00966 0.00243 AFIX 147 H5 2 0.116570 0.929609 0.103274 11.00000 -1.50000 AFIX 0 O6 3 0.340707 0.933054 0.142651 11.00000 0.06765 0.06042 = 0.06475 0.00491 0.00495 0.00465 O7 3 0.374448 0.766443 0.044801 11.00000 0.07886 0.07966 = 0.09601 -0.02074 -0.01373 -0.00475 AFIX 147 H7A 2 0.325288 0.806256 0.025717 11.00000 -1.50000 AFIX 0 O8 3 0.416857 0.956758 -0.002248 11.00000 0.07566 0.11498 = 0.06932 0.00963 -0.01205 -0.00471 C16 1 0.069175 0.975474 0.248383 11.00000 0.07770 0.13037 = 0.07533 -0.02134 0.00791 0.01721 AFIX 33 H16A 2 0.052615 0.902232 0.259544 11.00000 -1.50000 H16B 2 -0.007967 1.012148 0.240792 11.00000 -1.50000 H16C 2 0.112903 1.009291 0.283973 11.00000 -1.50000 AFIX 0 C17 1 0.172458 1.092438 0.167576 11.00000 0.11174 0.06631 = 0.11900 -0.00588 -0.00402 0.01897 AFIX 33 H17A 2 0.221337 1.093114 0.127995 11.00000 -1.50000 H17B 2 0.217211 1.128015 0.202143 11.00000 -1.50000 H17C 2 0.095152 1.128796 0.159876 11.00000 -1.50000 AFIX 0 C18 1 0.147124 0.979764 0.187303 11.00000 0.06301 0.07970 = 0.06427 -0.01719 -0.00272 0.00922 C19 1 0.266192 0.921164 0.198686 11.00000 0.06420 0.06306 = 0.06439 -0.00166 0.00086 0.00016 AFIX 13 H19 2 0.309009 0.952602 0.236632 11.00000 -1.20000 AFIX 0 C20 1 0.258626 0.804079 0.207565 11.00000 0.08146 0.07424 = 0.07139 0.00736 0.00606 -0.00070 AFIX 23 H20A 2 0.193597 0.773659 0.180258 11.00000 -1.20000 H20B 2 0.242525 0.785904 0.253223 11.00000 -1.20000 AFIX 0 C21 1 0.383276 0.765482 0.186582 11.00000 0.07500 0.06995 = 0.08532 0.00973 0.00355 0.00843 AFIX 23 H21A 2 0.376318 0.699963 0.161277 11.00000 -1.20000 H21B 2 0.436264 0.752575 0.224424 11.00000 -1.20000 AFIX 0 C22 1 0.434032 0.854669 0.144876 11.00000 0.05984 0.06207 = 0.07019 -0.00012 -0.00381 0.00578 AFIX 13 H22 2 0.507891 0.884571 0.166322 11.00000 -1.20000 AFIX 0 C23 1 0.465353 0.826809 0.075000 11.00000 0.05757 0.07168 = 0.07261 -0.01351 -0.00249 0.00705 AFIX 13 H23 2 0.542627 0.785278 0.075099 11.00000 -1.20000 AFIX 0 C24 1 0.488820 0.929331 0.038851 11.00000 0.05872 0.08176 = 0.05679 -0.00644 -0.00094 0.01132 C25 1 0.592278 0.996272 0.057059 11.00000 0.05873 0.06562 = 0.06116 0.00103 0.00173 0.00706 C26 1 0.699986 0.956821 0.082239 11.00000 0.06098 0.07211 = 0.06940 0.00704 0.00101 0.00180 AFIX 43 H26 2 0.707589 0.883753 0.089988 11.00000 -1.20000 AFIX 0 C27 1 0.796452 1.022766 0.096188 11.00000 0.06117 0.08569 = 0.07596 0.00629 0.00032 0.00299 AFIX 43 H27 2 0.870788 0.996052 0.112965 11.00000 -1.20000 AFIX 0 C28 1 0.781583 1.127497 0.085104 11.00000 0.07252 0.08119 = 0.08167 -0.00273 0.00151 -0.01221 C29 1 0.677518 1.169937 0.061427 11.00000 0.08873 0.07401 = 0.08102 0.00487 0.00181 0.00539 AFIX 43 H29 2 0.670151 1.243428 0.055303 11.00000 -1.20000 AFIX 0 C30 1 0.582622 1.103295 0.046484 11.00000 0.07080 0.08421 = 0.07042 -0.00175 -0.00447 0.01008 AFIX 43 H30 2 0.509655 1.131073 0.028706 11.00000 -1.20000 HKLF 4 Covalent radii and connectivity table for s92 in Pna2(1) C 0.770 H 0.320 O 0.660 F 0.640 F1 - C13 O1 - C3 O2 - C7 C4 O3 - C8 O4 - C9 C1 - C3 C2 - C3 C3 - O1 C4 C2 C1 C4 - O2 C3 C5 C5 - C6 C4 C6 - C5 C7 C7 - O2 C6 C8 C8 - O3 C9 C7 C9 - O4 C10 C8 C10 - C15 C11 C9 C11 - C12 C10 C12 - C13 C11 C13 - C12 C14 F1 C14 - C13 C15 C15 - C10 C14 F2 - C28 O5 - C18 O6 - C19 C22 O7 - C23 O8 - C24 C16 - C18 C17 - C18 C18 - O5 C17 C19 C16 C19 - O6 C20 C18 C20 - C19 C21 C21 - C20 C22 C22 - O6 C23 C21 C23 - O7 C24 C22 C24 - O8 C25 C23 C25 - C26 C30 C24 C26 - C27 C25 C27 - C28 C26 C28 - C29 F2 C27 C29 - C28 C30 C30 - C29 C25 Floating origin restraints generated 26699 Reflections read, of which 4088 rejected -11 =< h =< 13, -13 =< k =< 15, -22 =< l =< 24, Max. 2-theta = 50.05 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 1 2 1633.50 44.45 4 234.90 1 Inconsistent equivalents 5008 Unique reflections, of which 0 suppressed R(int) = 0.0812 R(sigma) = 0.0760 Friedel opposites not merged Maximum memory for data reduction = 3453 / 50412 Default effective X-H distances for T = -123.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 4527 / 464940 wR2 = 0.1126 before cycle 1 for 5008 data and 366 / 366 parameters GooF = S = 0.951; Restrained GooF = 0.951 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0452 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.17622 0.00254 -0.451 OSF 2 0.00977 0.00096 -0.231 EXTI Mean shift/esd = 0.171 Maximum = 0.742 for x O1 Max. shift = 0.018 A for H3 Max. dU =-0.001 for C6 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4527 / 464940 wR2 = 0.1123 before cycle 2 for 5008 data and 366 / 366 parameters GooF = S = 0.950; Restrained GooF = 0.950 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0452 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.17553 0.00253 -0.274 OSF 2 0.00966 0.00095 -0.118 EXTI Mean shift/esd = 0.054 Maximum = -0.274 for OSF Max. shift = 0.011 A for H1 Max. dU = 0.000 for C6 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4527 / 464940 wR2 = 0.1122 before cycle 3 for 5008 data and 366 / 366 parameters GooF = S = 0.950; Restrained GooF = 0.950 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0452 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.17551 0.00252 -0.010 OSF 2 0.00964 0.00095 -0.016 EXTI Mean shift/esd = 0.008 Maximum = 0.233 for tors H1 Max. shift = 0.012 A for H1 Max. dU = 0.000 for O1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4527 / 464940 wR2 = 0.1122 before cycle 4 for 5008 data and 366 / 366 parameters GooF = S = 0.950; Restrained GooF = 0.950 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0452 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.17548 0.00252 -0.012 OSF 2 0.00964 0.00095 -0.004 EXTI Mean shift/esd = 0.008 Maximum = 0.262 for tors H1 Max. shift = 0.014 A for H1 Max. dU = 0.000 for C1 Largest correlation matrix elements 0.564 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 -0.0017 0.4337 0.3457 147 0.840 0.000 O1 C3 H1 H3 0.2809 0.4491 0.5014 147 0.840 0.000 O3 C8 H3 H1A 0.0053 0.3994 0.2394 33 0.980 0.000 C1 C3 H1A H1B 0.0658 0.2930 0.2648 33 0.980 0.000 C1 C3 H1A H1C 0.1338 0.3616 0.2112 33 0.980 0.000 C1 C3 H1A H2A 0.0933 0.5711 0.2717 33 0.980 0.000 C2 C3 H2A H2B 0.2241 0.5381 0.2442 33 0.980 0.000 C2 C3 H2A H2C 0.2107 0.5761 0.3174 33 0.980 0.000 C2 C3 H2A H4 0.3211 0.3741 0.2813 13 1.000 0.000 C4 O2 C3 C5 H5A 0.1808 0.2481 0.3656 23 0.990 0.000 C5 C6 C4 H5B 0.2815 0.2110 0.3140 23 0.990 0.000 C5 C6 C4 H6A 0.4192 0.2060 0.3904 23 0.990 0.000 C6 C5 C7 H6B 0.3179 0.2417 0.4421 23 0.990 0.000 C6 C5 C7 H7 0.4884 0.3687 0.3761 13 1.000 0.000 C7 O2 C6 C8 H8 0.5067 0.3775 0.4877 13 1.000 0.000 C8 O3 C9 C7 H11 0.6710 0.4240 0.4334 43 0.950 0.000 C11 C12 C10 H12 0.8530 0.4852 0.3886 43 0.950 0.000 C12 C13 C11 H14 0.7220 0.7788 0.3893 43 0.950 0.000 C14 C13 C15 H15 0.5357 0.7186 0.4320 43 0.950 0.000 C15 C10 C14 H5 0.1177 0.9279 0.1035 147 0.840 0.000 O5 C18 H5 H7A 0.3244 0.8065 0.0265 147 0.840 0.000 O7 C23 H7A H16A 0.0527 0.9020 0.2595 33 0.980 0.000 C16 C18 H16A H16B -0.0080 1.0120 0.2408 33 0.980 0.000 C16 C18 H16A H16C 0.1129 1.0091 0.2840 33 0.980 0.000 C16 C18 H16A H17A 0.2215 1.0931 0.1280 33 0.980 0.000 C17 C18 H17A H17B 0.2174 1.1281 0.2021 33 0.980 0.000 C17 C18 H17A H17C 0.0953 1.1289 0.1599 33 0.980 0.000 C17 C18 H17A H19 0.3090 0.9526 0.2367 13 1.000 0.000 C19 O6 C20 C18 H20A 0.1937 0.7738 0.1801 23 0.990 0.000 C20 C19 C21 H20B 0.2425 0.7858 0.2531 23 0.990 0.000 C20 C19 C21 H21A 0.3763 0.6999 0.1612 23 0.990 0.000 C21 C20 C22 H21B 0.4362 0.7524 0.2244 23 0.990 0.000 C21 C20 C22 H22 0.5078 0.8845 0.1664 13 1.000 0.000 C22 O6 C23 C21 H23 0.5426 0.7852 0.0751 13 1.000 0.000 C23 O7 C24 C22 H26 0.7075 0.8838 0.0900 43 0.950 0.000 C26 C27 C25 H27 0.8710 0.9960 0.1128 43 0.950 0.000 C27 C28 C26 H29 0.6702 1.2432 0.0552 43 0.950 0.000 C29 C28 C30 H30 0.5095 1.1310 0.0288 43 0.950 0.000 C30 C29 C25 s92 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq F1 0.90481 0.67137 0.35938 1.00000 0.10778 0.13208 0.12345 0.00864 0.00638 -0.05190 0.12110 0.00452 0.00026 0.00021 0.00014 0.00000 0.00208 0.00206 0.00232 0.00181 0.00178 0.00163 0.00098 O1 0.07042 0.42294 0.35758 1.00000 0.06189 0.15687 0.08645 -0.00802 0.00677 0.00177 0.10174 0.00563 0.00026 0.00027 0.00015 0.00000 0.00179 0.00265 0.00226 0.00193 0.00171 0.00183 0.00093 H1 -0.00171 0.43371 0.34573 1.00000 0.15261 0.00000 0.00000 O2 0.32378 0.43484 0.36998 1.00000 0.07054 0.05914 0.07121 0.00528 -0.00991 -0.00286 0.06697 0.00410 0.00023 0.00016 0.00012 0.00000 0.00157 0.00130 0.00168 0.00124 0.00130 0.00114 0.00066 O3 0.33255 0.40241 0.50958 1.00000 0.06922 0.09831 0.07013 0.00105 0.01552 0.00395 0.07922 0.00510 0.00023 0.00021 0.00014 0.00000 0.00177 0.00197 0.00178 0.00141 0.00151 0.00129 0.00074 H3 0.28090 0.44913 0.50141 1.00000 0.11882 0.00000 0.00000 O4 0.39072 0.59392 0.48144 1.00000 0.08992 0.08459 0.10430 -0.01735 0.01500 0.01887 0.09294 0.00486 0.00025 0.00021 0.00014 0.00000 0.00207 0.00176 0.00257 0.00157 0.00176 0.00156 0.00092 C1 0.08237 0.36439 0.24980 1.00000 0.08593 0.11667 0.08039 -0.01763 -0.01100 -0.00587 0.09433 0.00684 0.00040 0.00034 0.00022 0.00000 0.00319 0.00357 0.00330 0.00260 0.00264 0.00222 0.00140 H1A 0.00533 0.39937 0.23942 1.00000 0.14149 0.00000 0.00000 H1B 0.06579 0.29301 0.26485 1.00000 0.14149 0.00000 0.00000 H1C 0.13375 0.36163 0.21115 1.00000 0.14149 0.00000 0.00000 C2 0.17114 0.53763 0.28226 1.00000 0.12372 0.08272 0.10310 0.01284 -0.03357 0.00164 0.10318 0.00800 0.00046 0.00033 0.00025 0.00000 0.00378 0.00308 0.00386 0.00249 0.00311 0.00241 0.00151 H2A 0.09330 0.57112 0.27167 1.00000 0.15477 0.00000 0.00000 H2B 0.22407 0.53814 0.24416 1.00000 0.15477 0.00000 0.00000 H2C 0.21066 0.57612 0.31742 1.00000 0.15477 0.00000 0.00000 C3 0.14863 0.42582 0.30310 1.00000 0.06685 0.08969 0.05527 -0.00157 0.00168 -0.00091 0.07060 0.00671 0.00034 0.00030 0.00020 0.00000 0.00252 0.00279 0.00251 0.00195 0.00206 0.00192 0.00101 C4 0.26716 0.37401 0.32016 1.00000 0.06471 0.07428 0.06506 -0.00784 -0.00066 -0.00942 0.06802 0.00608 0.00033 0.00025 0.00019 0.00000 0.00243 0.00238 0.00263 0.00200 0.00206 0.00179 0.00098 H4 0.32114 0.37408 0.28128 1.00000 0.08162 0.00000 0.00000 C5 0.26277 0.26322 0.34795 1.00000 0.11426 0.06615 0.13059 0.00055 -0.03178 -0.00813 0.10367 0.00763 0.00046 0.00029 0.00027 0.00000 0.00357 0.00270 0.00442 0.00240 0.00330 0.00226 0.00154 H5A 0.18080 0.24805 0.36558 1.00000 0.12440 0.00000 0.00000 H5B 0.28152 0.21102 0.31403 1.00000 0.12440 0.00000 0.00000 C6 0.35605 0.25904 0.40019 1.00000 0.08044 0.06042 0.08710 0.00296 0.00380 0.00736 0.07599 0.00696 0.00034 0.00027 0.00022 0.00000 0.00268 0.00237 0.00304 0.00188 0.00246 0.00170 0.00110 H6A 0.41917 0.20597 0.39036 1.00000 0.09118 0.00000 0.00000 H6B 0.31791 0.24172 0.44215 1.00000 0.09118 0.00000 0.00000 C7 0.41097 0.36869 0.40160 1.00000 0.05895 0.06649 0.06540 -0.00362 0.00582 0.00511 0.06361 0.00595 0.00032 0.00026 0.00018 0.00000 0.00219 0.00217 0.00257 0.00177 0.00197 0.00170 0.00093 H7 0.48836 0.36867 0.37612 1.00000 0.07634 0.00000 0.00000 C8 0.43584 0.41507 0.46816 1.00000 0.05608 0.07430 0.05877 0.00503 0.00649 0.00973 0.06305 0.00623 0.00031 0.00026 0.00018 0.00000 0.00219 0.00231 0.00240 0.00182 0.00190 0.00167 0.00092 H8 0.50675 0.37747 0.48771 1.00000 0.07566 0.00000 0.00000 C9 0.46705 0.53052 0.46302 1.00000 0.06870 0.07050 0.06731 -0.00610 -0.00192 0.01131 0.06883 0.00656 0.00036 0.00027 0.00019 0.00000 0.00263 0.00246 0.00271 0.00189 0.00205 0.00197 0.00099 C10 0.58332 0.56483 0.43571 1.00000 0.07027 0.06140 0.05938 -0.00114 -0.00848 0.00269 0.06369 0.00613 0.00034 0.00028 0.00018 0.00000 0.00244 0.00233 0.00241 0.00165 0.00205 0.00175 0.00091 C11 0.67979 0.49632 0.42356 1.00000 0.06606 0.06443 0.07157 -0.00198 -0.00835 -0.00229 0.06736 0.00598 0.00033 0.00027 0.00018 0.00000 0.00240 0.00216 0.00278 0.00179 0.00205 0.00183 0.00098 H11 0.67098 0.42400 0.43335 1.00000 0.08083 0.00000 0.00000 C12 0.78796 0.53220 0.39747 1.00000 0.06539 0.08333 0.07642 -0.00406 -0.00286 -0.01177 0.07505 0.00648 0.00036 0.00032 0.00020 0.00000 0.00269 0.00278 0.00295 0.00200 0.00225 0.00185 0.00110 H12 0.85297 0.48522 0.38856 1.00000 0.09005 0.00000 0.00000 C13 0.79903 0.63514 0.38499 1.00000 0.08074 0.09046 0.07902 0.00352 -0.00589 -0.02633 0.08341 0.00694 0.00043 0.00037 0.00021 0.00000 0.00309 0.00320 0.00317 0.00233 0.00235 0.00258 0.00119 C14 0.70971 0.70639 0.39764 1.00000 0.12008 0.06963 0.09424 0.01226 -0.01436 -0.01792 0.09465 0.00756 0.00052 0.00034 0.00023 0.00000 0.00422 0.00286 0.00363 0.00237 0.00313 0.00284 0.00141 H14 0.72202 0.77880 0.38926 1.00000 0.11358 0.00000 0.00000 C15 0.59962 0.67042 0.42320 1.00000 0.09510 0.07102 0.08166 0.00307 -0.00959 0.00914 0.08259 0.00750 0.00044 0.00031 0.00021 0.00000 0.00323 0.00275 0.00301 0.00216 0.00259 0.00208 0.00116 H15 0.53575 0.71858 0.43203 1.00000 0.09911 0.00000 0.00000 F2 0.87637 1.19264 0.09882 1.00000 0.10133 0.10347 0.15016 -0.00227 -0.01050 -0.03381 0.11832 0.00426 0.00024 0.00020 0.00014 0.00000 0.00194 0.00174 0.00271 0.00165 0.00187 0.00143 0.00099 O5 0.07778 0.92824 0.13812 1.00000 0.06563 0.10101 0.07071 -0.00928 -0.00924 0.00260 0.07912 0.00443 0.00022 0.00021 0.00014 0.00000 0.00159 0.00185 0.00177 0.00163 0.00139 0.00134 0.00072 H5 0.11770 0.92787 0.10353 1.00000 0.11868 0.00000 0.00000 O6 0.34076 0.93306 0.14264 1.00000 0.06702 0.06009 0.06437 0.00506 0.00478 0.00537 0.06383 0.00399 0.00020 0.00016 0.00012 0.00000 0.00150 0.00138 0.00171 0.00108 0.00139 0.00103 0.00063 O7 0.37440 0.76651 0.04477 1.00000 0.07822 0.08004 0.09627 -0.02157 -0.01443 -0.00536 0.08485 0.00412 0.00023 0.00018 0.00015 0.00000 0.00193 0.00163 0.00237 0.00157 0.00166 0.00131 0.00084 H7A 0.32438 0.80648 0.02646 1.00000 0.12727 0.00000 0.00000 O8 0.41663 0.95685 -0.00223 1.00000 0.07491 0.11499 0.06888 0.01021 -0.01312 -0.00417 0.08626 0.00472 0.00025 0.00020 0.00014 0.00000 0.00193 0.00215 0.00195 0.00160 0.00163 0.00151 0.00081 C16 0.06917 0.97531 0.24838 1.00000 0.07703 0.13048 0.07528 -0.02168 0.00868 0.01779 0.09426 0.00802 0.00038 0.00037 0.00022 0.00000 0.00282 0.00360 0.00309 0.00253 0.00254 0.00234 0.00131 H16A 0.05265 0.90204 0.25951 1.00000 0.14139 0.00000 0.00000 H16B -0.00799 1.01195 0.24079 1.00000 0.14139 0.00000 0.00000 H16C 0.11287 1.00910 0.28399 1.00000 0.14139 0.00000 0.00000 C17 0.17259 1.09253 0.16756 1.00000 0.11255 0.06700 0.11825 -0.00531 -0.00313 0.02030 0.09927 0.00807 0.00043 0.00029 0.00026 0.00000 0.00359 0.00276 0.00401 0.00223 0.00294 0.00233 0.00144 H17A 0.22147 1.09315 0.12798 1.00000 0.14890 0.00000 0.00000 H17B 0.21739 1.12809 0.20212 1.00000 0.14890 0.00000 0.00000 H17C 0.09533 1.12894 0.15986 1.00000 0.14890 0.00000 0.00000 C18 0.14710 0.97969 0.18734 1.00000 0.06235 0.07877 0.06326 -0.01661 -0.00229 0.00836 0.06813 0.00623 0.00033 0.00029 0.00019 0.00000 0.00239 0.00250 0.00272 0.00198 0.00206 0.00178 0.00099 C19 0.26623 0.92118 0.19873 1.00000 0.06413 0.06300 0.06307 -0.00179 0.00079 0.00058 0.06340 0.00625 0.00032 0.00024 0.00019 0.00000 0.00232 0.00206 0.00252 0.00182 0.00205 0.00159 0.00091 H19 0.30904 0.95257 0.23670 1.00000 0.07608 0.00000 0.00000 C20 0.25868 0.80408 0.20747 1.00000 0.08066 0.07499 0.07195 0.00760 0.00506 -0.00033 0.07587 0.00690 0.00037 0.00025 0.00020 0.00000 0.00280 0.00247 0.00284 0.00208 0.00218 0.00193 0.00109 H20A 0.19367 0.77376 0.18011 1.00000 0.09104 0.00000 0.00000 H20B 0.24249 0.78579 0.25311 1.00000 0.09104 0.00000 0.00000 C21 0.38328 0.76541 0.18652 1.00000 0.07430 0.06932 0.08477 0.00858 0.00374 0.00804 0.07613 0.00726 0.00033 0.00028 0.00021 0.00000 0.00273 0.00242 0.00314 0.00206 0.00231 0.00175 0.00112 H21A 0.37631 0.69994 0.16117 1.00000 0.09136 0.00000 0.00000 H21B 0.43625 0.75243 0.22436 1.00000 0.09136 0.00000 0.00000 C22 0.43397 0.85466 0.14491 1.00000 0.05877 0.06203 0.07031 -0.00045 -0.00349 0.00538 0.06370 0.00628 0.00030 0.00024 0.00019 0.00000 0.00217 0.00219 0.00264 0.00189 0.00195 0.00164 0.00092 H22 0.50784 0.88452 0.16637 1.00000 0.07644 0.00000 0.00000 C23 0.46537 0.82668 0.07502 1.00000 0.05741 0.07162 0.07168 -0.01316 -0.00219 0.00717 0.06690 0.00615 0.00033 0.00026 0.00019 0.00000 0.00213 0.00225 0.00275 0.00198 0.00190 0.00168 0.00097 H23 0.54265 0.78515 0.07509 1.00000 0.08028 0.00000 0.00000 C24 0.48858 0.92928 0.03875 1.00000 0.05924 0.08083 0.05705 -0.00635 0.00079 0.01113 0.06570 0.00673 0.00034 0.00028 0.00020 0.00000 0.00242 0.00256 0.00262 0.00192 0.00209 0.00180 0.00098 C25 0.59224 0.99638 0.05710 1.00000 0.05797 0.06525 0.06099 0.00081 0.00133 0.00676 0.06140 0.00612 0.00030 0.00027 0.00018 0.00000 0.00219 0.00220 0.00235 0.00173 0.00197 0.00160 0.00087 C26 0.69995 0.95692 0.08222 1.00000 0.06113 0.07111 0.06898 0.00626 0.00074 0.00117 0.06707 0.00649 0.00033 0.00028 0.00018 0.00000 0.00247 0.00228 0.00258 0.00182 0.00192 0.00175 0.00099 H26 0.70750 0.88384 0.08995 1.00000 0.08049 0.00000 0.00000 C27 0.79658 1.02278 0.09615 1.00000 0.06142 0.08472 0.07552 0.00613 0.00048 0.00326 0.07389 0.00684 0.00034 0.00031 0.00019 0.00000 0.00248 0.00289 0.00288 0.00204 0.00216 0.00195 0.00107 H27 0.87097 0.99600 0.11282 1.00000 0.08866 0.00000 0.00000 C28 0.78166 1.12747 0.08518 1.00000 0.07280 0.08242 0.08019 -0.00309 0.00196 -0.01238 0.07847 0.00684 0.00038 0.00031 0.00021 0.00000 0.00299 0.00302 0.00312 0.00217 0.00231 0.00224 0.00115 C29 0.67755 1.16976 0.06142 1.00000 0.08830 0.07346 0.08101 0.00410 0.00198 0.00593 0.08092 0.00774 0.00040 0.00032 0.00021 0.00000 0.00317 0.00256 0.00307 0.00217 0.00264 0.00219 0.00114 H29 0.67023 1.24323 0.05518 1.00000 0.09711 0.00000 0.00000 C30 0.58251 1.10320 0.04653 1.00000 0.06994 0.08380 0.06953 -0.00222 -0.00441 0.00989 0.07442 0.00686 0.00035 0.00029 0.00020 0.00000 0.00256 0.00286 0.00266 0.00216 0.00221 0.00206 0.00105 H30 0.50950 1.13100 0.02881 1.00000 0.08931 0.00000 0.00000 Final Structure Factor Calculation for s92 in Pna2(1) Total number of l.s. parameters = 366 Maximum vector length = 511 Memory required = 4163 / 25046 wR2 = 0.1122 before cycle 5 for 5008 data and 2 / 366 parameters GooF = S = 0.950; Restrained GooF = 0.949 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0452 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0448 for 2794 Fo > 4sig(Fo) and 0.1088 for all 5008 data wR2 = 0.1122, GooF = S = 0.950, Restrained GooF = 0.949 for all data Flack x parameter = 0.1032 with esd 1.0417 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 40.00 for non-hydrogen and 38.00 for hydrogen atoms Principal mean square atomic displacements U 0.1734 0.1251 0.0648 F1 0.1578 0.0874 0.0600 O1 0.0823 0.0616 0.0571 O2 0.0993 0.0843 0.0540 O3 0.1154 0.1063 0.0571 O4 0.1239 0.0935 0.0656 C1 0.1491 0.0916 0.0688 C2 0.0898 0.0670 0.0550 C3 0.0825 0.0656 0.0560 C4 0.1556 0.0911 0.0644 C5 0.0900 0.0800 0.0579 C6 0.0696 0.0685 0.0527 C7 0.0809 0.0585 0.0497 C8 0.0831 0.0660 0.0574 C9 0.0755 0.0608 0.0547 C10 0.0776 0.0660 0.0585 C11 0.0896 0.0770 0.0585 C12 0.1136 0.0781 0.0586 C13 0.1336 0.0883 0.0620 C14 0.1016 0.0807 0.0654 C15 0.1531 0.1343 0.0676 F2 0.1043 0.0748 0.0583 O5 0.0744 0.0608 0.0562 O6 0.1136 0.0839 0.0570 O7 0.1183 0.0826 0.0579 O8 0.1412 0.0849 0.0568 C16 0.1243 0.1145 0.0590 C17 0.0917 0.0608 0.0519 C18 0.0649 0.0644 0.0609 C19 0.0844 0.0786 0.0646 C20 0.0914 0.0747 0.0622 C21 0.0717 0.0650 0.0544 C22 0.0863 0.0608 0.0535 C23 0.0866 0.0585 0.0520 C24 0.0695 0.0608 0.0539 C25 0.0765 0.0637 0.0610 C26 0.0882 0.0725 0.0610 C27 0.0920 0.0791 0.0643 C28 0.0914 0.0810 0.0704 C29 0.0898 0.0702 0.0633 C30 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.013 0.017 0.023 0.030 0.038 0.051 0.072 0.109 1.000 Number in group 504. 578. 425. 554. 489. 469. 488. 517. 481. 503. GooF 0.816 0.818 0.808 0.921 0.993 1.060 1.004 0.985 0.945 1.105 K 1.713 1.029 0.870 0.984 0.959 0.969 0.988 0.988 1.012 1.014 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.15 1.26 1.44 1.80 inf Number in group 509. 502. 498. 495. 503. 502. 499. 498. 497. 505. GooF 0.841 0.827 0.847 0.936 0.993 0.963 1.017 0.959 0.973 1.104 K 1.150 0.951 0.906 1.002 0.991 0.988 1.002 1.005 1.033 1.010 R1 0.525 0.430 0.325 0.254 0.161 0.086 0.066 0.063 0.039 0.027 Recommended weighting scheme: WGHT 0.0421 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 2 0 1 1187.92 1597.92 5.57 0.201 5.30 4 2 15 5.77 51.07 4.38 0.036 1.21 2 0 -1 1292.03 1591.30 4.01 0.201 5.30 4 0 0 14734.75 11929.99 3.92 0.549 2.74 3 4 7 932.91 766.98 3.81 0.139 1.87 7 5 -10 -2.77 25.30 3.79 0.025 1.12 9 2 -5 0.00 28.77 3.56 0.027 1.15 5 11 -8 67.21 44.08 3.49 0.033 0.95 9 3 12 84.52 48.73 3.41 0.035 0.97 5 1 -7 889.94 750.71 3.40 0.138 1.75 1 12 -9 122.38 73.76 3.29 0.043 0.96 3 4 15 68.44 115.14 3.22 0.054 1.20 5 11 14 59.55 1.33 3.13 0.006 0.84 1 6 -20 -5.71 37.89 3.11 0.031 0.93 2 3 1 268.26 314.85 3.10 0.089 3.32 1 2 3 2556.08 2956.78 3.10 0.273 4.31 4 2 -13 159.29 208.38 3.09 0.073 1.35 6 2 -7 80.45 109.90 3.06 0.053 1.51 4 5 13 14.50 47.61 3.06 0.035 1.21 5 8 6 86.16 52.43 3.05 0.036 1.21 4 9 16 2.09 26.70 3.00 0.026 0.90 2 2 2 1469.69 1687.71 3.00 0.207 3.86 2 6 12 8.38 34.08 2.98 0.029 1.30 5 5 -2 434.85 373.99 2.95 0.097 1.64 4 9 8 75.36 110.68 2.93 0.053 1.13 5 10 -4 132.03 160.21 2.92 0.064 1.08 9 7 -5 11.35 36.28 2.90 0.030 0.98 6 10 -3 33.41 15.42 2.89 0.020 1.03 0 8 -2 56.59 100.14 2.89 0.050 1.58 2 8 1 364.06 313.53 2.88 0.089 1.53 3 4 -5 416.28 475.62 2.85 0.110 2.08 2 1 -3 2242.02 2557.81 2.85 0.254 4.07 6 1 9 113.64 56.50 2.82 0.038 1.42 11 6 2 30.23 1.43 2.81 0.006 0.90 6 6 -6 70.11 50.06 2.81 0.036 1.29 4 1 -9 1015.41 887.71 2.79 0.150 1.75 8 5 11 28.61 62.67 2.78 0.040 1.02 4 3 9 591.67 482.85 2.78 0.111 1.63 5 11 -7 103.00 79.33 2.77 0.045 0.97 0 1 -17 144.96 220.55 2.75 0.075 1.21 9 3 1 -4.96 20.24 2.75 0.023 1.17 8 6 -5 134.77 168.07 2.75 0.065 1.11 11 4 -5 51.15 16.04 2.75 0.020 0.93 8 10 -2 -3.43 12.56 2.74 0.018 0.93 8 7 -5 113.11 81.05 2.74 0.045 1.06 7 7 1 139.76 170.59 2.73 0.066 1.19 7 3 -12 61.40 40.45 2.69 0.032 1.12 8 4 2 13.74 34.56 2.68 0.030 1.25 2 4 -18 -5.37 20.15 2.67 0.023 1.06 8 9 5 -5.85 11.67 2.67 0.017 0.96 Bond lengths and angles F1 - Distance Angles C13 1.3575 (0.0048) F1 - O1 - Distance Angles C3 1.4185 (0.0048) O1 - O2 - Distance Angles C7 1.4344 (0.0040) C4 1.4334 (0.0042) 107.41 (0.24) O2 - C7 O3 - Distance Angles C8 1.4308 (0.0042) O3 - O4 - Distance Angles C9 1.2256 (0.0039) O4 - C1 - Distance Angles C3 1.5372 (0.0055) C1 - C2 - Distance Angles C3 1.5113 (0.0053) C2 - C3 - Distance Angles O1 1.4185 (0.0048) C4 1.5013 (0.0050) 108.99 (0.32) C2 1.5113 (0.0053) 110.53 (0.36) 109.97 (0.31) C1 1.5372 (0.0054) 105.81 (0.32) 110.75 (0.33) 110.71 (0.35) C3 - O1 C4 C2 C4 - Distance Angles O2 1.4334 (0.0042) C3 1.5013 (0.0050) 107.85 (0.29) C5 1.5276 (0.0048) 104.10 (0.31) 117.98 (0.33) C4 - O2 C3 C5 - Distance Angles C6 1.4907 (0.0055) C4 1.5276 (0.0048) 106.57 (0.32) C5 - C6 C6 - Distance Angles C5 1.4907 (0.0055) C7 1.5240 (0.0046) 104.63 (0.31) C6 - C5 C7 - Distance Angles O2 1.4344 (0.0040) C6 1.5240 (0.0046) 105.55 (0.28) C8 1.5257 (0.0050) 107.68 (0.27) 116.39 (0.33) C7 - O2 C6 C8 - Distance Angles O3 1.4308 (0.0042) C9 1.5165 (0.0048) 109.32 (0.27) C7 1.5257 (0.0050) 110.90 (0.28) 110.73 (0.30) C8 - O3 C9 C9 - Distance Angles O4 1.2256 (0.0039) C10 1.4628 (0.0052) 121.25 (0.33) C8 1.5165 (0.0048) 117.73 (0.34) 121.00 (0.30) C9 - O4 C10 C10 - Distance Angles C15 1.3841 (0.0048) C11 1.3960 (0.0048) 118.57 (0.37) C9 1.4628 (0.0052) 118.47 (0.34) 122.93 (0.33) C10 - C15 C11 C11 - Distance Angles C12 1.3823 (0.0051) C10 1.3960 (0.0048) 120.94 (0.35) C11 - C12 C12 - Distance Angles C13 1.3446 (0.0053) C11 1.3823 (0.0051) 118.46 (0.40) C12 - C13 C13 - Distance Angles C12 1.3446 (0.0053) C14 1.3624 (0.0062) 123.38 (0.42) F1 1.3575 (0.0047) 119.03 (0.45) 117.58 (0.42) C13 - C12 C14 C14 - Distance Angles C13 1.3624 (0.0062) C15 1.3967 (0.0061) 118.41 (0.39) C14 - C13 C15 - Distance Angles C10 1.3841 (0.0048) C14 1.3967 (0.0061) 120.19 (0.40) C15 - C10 F2 - Distance Angles C28 1.3608 (0.0043) F2 - O5 - Distance Angles C18 1.4318 (0.0043) O5 - O6 - Distance Angles C19 1.4293 (0.0042) C22 1.4317 (0.0036) 107.93 (0.25) O6 - C19 O7 - Distance Angles C23 1.4069 (0.0040) O7 - O8 - Distance Angles C24 1.2118 (0.0041) O8 - C16 - Distance Angles C18 1.5277 (0.0055) C16 - C17 - Distance Angles C18 1.5233 (0.0054) C17 - C18 - Distance Angles O5 1.4318 (0.0043) C17 1.5233 (0.0054) 109.85 (0.35) C19 1.5240 (0.0049) 109.95 (0.28) 110.33 (0.31) C16 1.5277 (0.0055) 106.00 (0.31) 111.11 (0.32) 109.51 (0.32) C18 - O5 C17 C19 C19 - Distance Angles O6 1.4293 (0.0042) C20 1.5079 (0.0044) 103.55 (0.26) C18 1.5240 (0.0049) 108.24 (0.29) 117.21 (0.30) C19 - O6 C20 C20 - Distance Angles C19 1.5079 (0.0044) C21 1.5172 (0.0050) 103.80 (0.30) C20 - C19 C21 - Distance Angles C20 1.5172 (0.0050) C22 1.5331 (0.0049) 104.25 (0.28) C21 - C20 C22 - Distance Angles O6 1.4317 (0.0036) C23 1.5308 (0.0052) 107.02 (0.28) C21 1.5331 (0.0049) 106.18 (0.27) 116.13 (0.29) C22 - O6 C23 C23 - Distance Angles O7 1.4069 (0.0040) C24 1.5313 (0.0052) 111.48 (0.31) C22 1.5308 (0.0052) 112.90 (0.30) 107.60 (0.26) C23 - O7 C24 C24 - Distance Angles O8 1.2118 (0.0041) C25 1.4737 (0.0049) 121.00 (0.35) C23 1.5313 (0.0052) 118.94 (0.34) 119.91 (0.34) C24 - O8 C25 C25 - Distance Angles C26 1.3862 (0.0046) C30 1.3851 (0.0048) 118.87 (0.33) C24 1.4737 (0.0049) 122.95 (0.33) 118.15 (0.32) C25 - C26 C30 C26 - Distance Angles C27 1.3837 (0.0050) C25 1.3862 (0.0046) 120.73 (0.35) C26 - C27 C27 - Distance Angles C28 1.3653 (0.0050) C26 1.3837 (0.0050) 117.90 (0.36) C27 - C28 C28 - Distance Angles C29 1.3561 (0.0053) F2 1.3608 (0.0042) 118.40 (0.39) C27 1.3653 (0.0050) 123.44 (0.36) 118.17 (0.38) C28 - C29 F2 C29 - Distance Angles C28 1.3561 (0.0053) C30 1.3800 (0.0052) 118.22 (0.38) C29 - C28 C30 - Distance Angles C29 1.3800 (0.0052) C25 1.3851 (0.0048) 120.82 (0.36) C30 - C29 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)