+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 16:32:26 on 03-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01sot025 in P2(1)/c CELL 0.71073 16.4380 7.8238 18.1280 90 109.970 90 ZERR 2 0.0003 0.0001 0.0003 0 0.003 0 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O S UNIT 104 88 8 12 4 V = 2191.22 F(000) = 928.0 Mu = 0.18 mm-1 Cell Wt = 1770.06 Rho = 1.341 SHEL 7 0.84 OMIT -2 0 12 OMIT 0 0 16 TEMP -123 SIZE 0.15 0.1 0.08 EQIV $1 x, y+1, z HTAB N2 O3_$1 HTAB N2 S1_$1 HTAB L.S. 5 WGHT 0.041300 EXTI 0.003232 FVAR 0.13655 C1 1 0.047380 1.014376 -0.087896 11.00000 0.03705 0.03307 = 0.04306 0.00276 0.02159 0.00436 AFIX 43 H1 2 0.029746 1.012420 -0.043160 11.00000 -1.20000 AFIX 0 C2 1 0.037361 1.161801 -0.131285 11.00000 0.04055 0.02952 = 0.05155 0.00425 0.01971 0.00534 AFIX 43 H2 2 0.012184 1.259773 -0.116766 11.00000 -1.20000 AFIX 0 C3 1 0.063632 1.168370 -0.195770 11.00000 0.02850 0.03500 = 0.04090 0.01104 0.00830 -0.00172 AFIX 43 H3 2 0.057236 1.270539 -0.225540 11.00000 -1.20000 AFIX 0 C4 1 0.098923 1.026154 -0.216211 11.00000 0.03248 0.04816 = 0.03266 0.00839 0.01220 -0.00203 AFIX 43 H4 2 0.116404 1.029034 -0.261025 11.00000 -1.20000 AFIX 0 C5 1 0.109594 0.877470 -0.172394 11.00000 0.02745 0.03898 = 0.03678 0.00125 0.00973 0.00450 AFIX 43 H5 2 0.135666 0.780320 -0.186558 11.00000 -1.20000 AFIX 0 C6 1 0.082419 0.869692 -0.107964 11.00000 0.01590 0.02377 = 0.02929 -0.00028 0.00349 -0.00386 C7 1 0.099158 0.713422 -0.059117 11.00000 0.02469 0.02386 = 0.02798 0.00086 0.00672 -0.00123 C8 1 0.181542 0.629637 -0.026307 11.00000 0.02168 0.02577 = 0.03142 -0.00174 0.00939 -0.00030 C9 1 0.264092 0.689984 -0.034010 11.00000 0.02066 0.03073 = 0.03378 0.00340 0.00633 -0.00002 C10 1 0.287590 0.860521 -0.022356 11.00000 0.02279 0.03637 = 0.03455 -0.00020 0.00863 -0.00276 AFIX 43 H10 2 0.250740 0.938825 -0.008911 11.00000 -1.20000 AFIX 0 C11 1 0.363756 0.918780 -0.029951 11.00000 0.03244 0.04409 = 0.04346 -0.00267 0.00995 -0.01323 AFIX 43 H11 2 0.379206 1.036004 -0.021514 11.00000 -1.20000 AFIX 0 C12 1 0.417279 0.805187 -0.049917 11.00000 0.02367 0.06198 = 0.04503 0.00226 0.01302 -0.00664 AFIX 43 H12 2 0.469499 0.844768 -0.055511 11.00000 -1.20000 AFIX 0 C13 1 0.395502 0.636630 -0.061621 11.00000 0.03180 0.05120 = 0.05003 -0.00317 0.01803 0.00947 AFIX 43 H13 2 0.432578 0.559475 -0.075418 11.00000 -1.20000 AFIX 0 C14 1 0.319226 0.577074 -0.053453 11.00000 0.02929 0.03694 = 0.03850 -0.00311 0.00942 0.00152 AFIX 43 H14 2 0.304715 0.459311 -0.061139 11.00000 -1.20000 AFIX 0 C15 1 0.172427 0.493237 0.016754 11.00000 0.01826 0.02384 = 0.03373 -0.00055 0.00619 -0.00058 C16 1 0.242696 0.375556 0.065908 11.00000 0.01978 0.02293 = 0.03791 0.00475 0.00836 -0.00219 C17 1 0.350128 0.354311 0.199276 11.00000 0.01775 0.02345 = 0.03470 0.00033 0.00250 0.00110 C18 1 0.353532 0.362335 0.276729 11.00000 0.03059 0.03401 = 0.03938 0.00021 0.01251 0.00354 AFIX 43 H18 2 0.308620 0.417973 0.289366 11.00000 -1.20000 AFIX 0 C19 1 0.422433 0.289234 0.335844 11.00000 0.03857 0.04352 = 0.03683 0.00450 0.00687 0.00430 AFIX 43 H19 2 0.424680 0.295628 0.388837 11.00000 -1.20000 AFIX 0 C20 1 0.487563 0.207438 0.317872 11.00000 0.03078 0.04318 = 0.04682 0.00485 -0.00295 0.00894 AFIX 43 H20 2 0.534217 0.155944 0.358233 11.00000 -1.20000 AFIX 0 C21 1 0.484632 0.200762 0.240999 11.00000 0.02417 0.03994 = 0.05342 0.00216 0.00731 0.00671 AFIX 43 H21 2 0.529780 0.145081 0.228746 11.00000 -1.20000 AFIX 0 C22 1 0.416817 0.274068 0.181459 11.00000 0.02812 0.03481 = 0.04034 -0.00064 0.01288 0.00158 AFIX 43 H22 2 0.415728 0.269722 0.128759 11.00000 -1.20000 AFIX 0 C23 1 0.041931 0.619792 -0.033760 11.00000 0.01831 0.01909 = 0.03173 0.00234 0.00307 0.00182 C24 1 0.051280 0.363566 0.051096 11.00000 0.02312 0.02318 = 0.03061 0.00159 0.00508 -0.00143 C25 1 0.182057 0.002110 0.228072 11.00000 0.05016 0.03762 = 0.04166 0.00117 0.01118 0.00463 AFIX 33 H25A 2 0.121284 0.006368 0.224630 11.00000 -1.50000 H25B 2 0.202022 0.117705 0.222254 11.00000 -1.50000 H25C 2 0.217297 -0.044456 0.279193 11.00000 -1.50000 AFIX 0 C26 1 0.305163 -0.108971 0.174904 11.00000 0.04329 0.05619 = 0.09488 -0.01165 0.03903 -0.01381 AFIX 33 H26A 2 0.323630 -0.176552 0.137914 11.00000 -1.50000 H26B 2 0.335165 -0.149773 0.228452 11.00000 -1.50000 H26C 2 0.319330 0.011607 0.171011 11.00000 -1.50000 AFIX 0 N1 3 0.086779 0.484491 0.013270 11.00000 0.01718 0.02560 = 0.03063 0.00440 0.00187 0.00369 N2 3 0.278930 0.431484 0.140847 11.00000 0.01984 0.02567 = 0.03528 -0.00142 0.00516 0.00555 AFIX 43 H2A 2 0.256382 0.523262 0.154315 11.00000 -1.20000 AFIX 0 O1 4 0.266759 0.253519 0.036940 11.00000 0.03328 0.03360 = 0.04373 -0.00784 0.00247 0.01030 O2 4 0.096904 0.254632 0.093095 11.00000 0.02113 0.03294 = 0.04638 0.01481 0.00460 0.00413 O3 4 0.179302 -0.310437 0.174517 11.00000 0.03895 0.03216 = 0.06997 -0.00181 0.02976 0.00340 S1 5 0.192169 -0.130975 0.152059 11.00000 0.03790 0.03574 = 0.04094 0.00042 0.01249 0.00611 HKLF 4 Covalent radii and connectivity table for 01sot025 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - C2 C6 C2 - C1 C3 C3 - C4 C2 C4 - C3 C5 C5 - C4 C6 C6 - C1 C5 C7 C7 - C23 C8 C6 C8 - C15 C7 C9 C9 - C10 C14 C8 C10 - C11 C9 C11 - C10 C12 C12 - C13 C11 C13 - C12 C14 C14 - C13 C9 C15 - C8 N1 C16 C16 - O1 N2 C15 C17 - C18 C22 N2 C18 - C17 C19 C19 - C20 C18 C20 - C19 C21 C21 - C20 C22 C22 - C21 C17 C23 - C7 N1 C24_$2 C24 - O2 N1 C23_$2 C25 - S1 C26 - S1 N1 - C15 C23 C24 N2 - C16 C17 O1 - C16 O2 - C24 O3 - S1 S1 - O3 C26 C25 Operators for generating equivalent atoms: $1 x, y+1, z $2 -x, -y+1, -z 13796 Reflections read, of which 1321 rejected -19 =< h =< 19, -9 =< k =< 9, -20 =< l =< 21, 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 3 41.51 0.12 4 100.27 -3 1 6 13.16 0.21 3 6.54 -2 2 6 21.91 0.23 4 10.03 -4 1 8 8.82 0.20 3 4.85 -5 2 9 15.75 0.40 4 3.87 -5 1 10 5.83 0.33 4 1.82 -6 2 11 8.21 0.37 4 1.95 -6 1 12 6.10 0.36 4 2.14 -7 3 12 8.96 0.45 3 8.88 9 Inconsistent equivalents 3848 Unique reflections, of which 0 suppressed R(int) = 0.1479 R(sigma) = 0.1541 Friedel opposites merged Maximum memory for data reduction = 2323 / 38855 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 = 3123 / 363172 wR2 = 0.1363 before cycle 1 for 3848 data and 290 / 290 parameters GooF = S = 0.947; Restrained GooF = 0.947 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0413 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13655 0.00034 0.015 OSF 2 0.00323 0.00084 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.015 for OSF Max. shift = 0.000 A for C18 Max. dU = 0.000 for C16 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3123 / 363172 wR2 = 0.1363 before cycle 2 for 3848 data and 290 / 290 parameters GooF = S = 0.947; Restrained GooF = 0.947 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0413 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13655 0.00034 0.000 OSF 2 0.00323 0.00084 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for U23 S1 Max. shift = 0.000 A for C18 Max. dU = 0.000 for C16 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3123 / 363172 wR2 = 0.1363 before cycle 3 for 3848 data and 290 / 290 parameters GooF = S = 0.947; Restrained GooF = 0.947 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0413 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13655 0.00034 0.000 OSF 2 0.00323 0.00084 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x N2 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3123 / 363172 wR2 = 0.1363 before cycle 4 for 3848 data and 290 / 290 parameters GooF = S = 0.947; Restrained GooF = 0.947 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0413 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13655 0.00034 0.000 OSF 2 0.00323 0.00084 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y C1 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C20 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3123 / 363172 wR2 = 0.1363 before cycle 5 for 3848 data and 290 / 290 parameters GooF = S = 0.947; Restrained GooF = 0.947 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0413 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13655 0.00034 0.000 OSF 2 0.00323 0.00084 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y C1 Max. shift = 0.000 A for O3 Max. dU = 0.000 for C20 Largest correlation matrix elements 0.537 U13 C26 / U11 C26 0.526 U13 C26 / U33 C26 0.530 EXTI / OSF 0.501 U13 O3 / U11 O3 Idealized hydrogen atom generation before cycle 6 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.0297 1.0124 -0.0432 43 0.950 0.000 C1 C2 C6 H2 0.0122 1.2598 -0.1168 43 0.950 0.000 C2 C1 C3 H3 0.0572 1.2705 -0.2255 43 0.950 0.000 C3 C4 C2 H4 0.1164 1.0290 -0.2610 43 0.950 0.000 C4 C3 C5 H5 0.1357 0.7803 -0.1866 43 0.950 0.000 C5 C4 C6 H10 0.2507 0.9388 -0.0089 43 0.950 0.000 C10 C11 C9 H11 0.3792 1.0360 -0.0215 43 0.950 0.000 C11 C10 C12 H12 0.4695 0.8448 -0.0555 43 0.950 0.000 C12 C13 C11 H13 0.4326 0.5595 -0.0754 43 0.950 0.000 C13 C12 C14 H14 0.3047 0.4593 -0.0611 43 0.950 0.000 C14 C13 C9 H18 0.3086 0.4180 0.2894 43 0.950 0.000 C18 C17 C19 H19 0.4247 0.2956 0.3888 43 0.950 0.000 C19 C20 C18 H20 0.5342 0.1559 0.3582 43 0.950 0.000 C20 C19 C21 H21 0.5298 0.1451 0.2287 43 0.950 0.000 C21 C20 C22 H22 0.4157 0.2697 0.1288 43 0.950 0.000 C22 C21 C17 H25A 0.1213 0.0064 0.2246 33 0.980 0.000 C25 S1 H25A H25B 0.2020 0.1177 0.2223 33 0.980 0.000 C25 S1 H25A H25C 0.2173 -0.0445 0.2792 33 0.980 0.000 C25 S1 H25A H26A 0.3236 -0.1766 0.1379 33 0.980 0.000 C26 S1 H26A H26B 0.3352 -0.1498 0.2285 33 0.980 0.000 C26 S1 H26A H26C 0.3193 0.0116 0.1710 33 0.980 0.000 C26 S1 H26A H2A 0.2564 0.5233 0.1543 43 0.880 0.000 N2 C16 C17 01sot025 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.04738 1.01438 -0.08790 1.00000 0.03705 0.03307 0.04306 0.00276 0.02159 0.00436 0.03569 0.00751 0.00024 0.00049 0.00022 0.00000 0.00264 0.00253 0.00246 0.00200 0.00200 0.00206 0.00100 H1 0.02975 1.01242 -0.04316 1.00000 0.04283 0.00000 0.00000 C2 0.03736 1.16180 -0.13129 1.00000 0.04055 0.02952 0.05155 0.00425 0.01971 0.00534 0.03951 0.00785 0.00025 0.00049 0.00023 0.00000 0.00278 0.00252 0.00266 0.00204 0.00214 0.00202 0.00107 H2 0.01218 1.25977 -0.11677 1.00000 0.04741 0.00000 0.00000 C3 0.06363 1.16837 -0.19577 1.00000 0.02850 0.03500 0.04090 0.01104 0.00830 -0.00172 0.03571 0.00737 0.00024 0.00049 0.00022 0.00000 0.00252 0.00264 0.00248 0.00196 0.00194 0.00200 0.00103 H3 0.05724 1.27054 -0.22554 1.00000 0.04285 0.00000 0.00000 C4 0.09892 1.02615 -0.21621 1.00000 0.03248 0.04816 0.03266 0.00839 0.01220 -0.00203 0.03749 0.00743 0.00024 0.00052 0.00021 0.00000 0.00264 0.00282 0.00232 0.00215 0.00190 0.00221 0.00104 H4 0.11640 1.02903 -0.26102 1.00000 0.04499 0.00000 0.00000 C5 0.10959 0.87747 -0.17239 1.00000 0.02745 0.03898 0.03678 0.00125 0.00973 0.00450 0.03472 0.00729 0.00023 0.00051 0.00021 0.00000 0.00244 0.00253 0.00229 0.00206 0.00183 0.00198 0.00099 H5 0.13567 0.78032 -0.18656 1.00000 0.04166 0.00000 0.00000 C6 0.08242 0.86969 -0.10796 1.00000 0.01590 0.02377 0.02929 -0.00028 0.00349 -0.00386 0.02407 0.00648 0.00021 0.00045 0.00019 0.00000 0.00210 0.00213 0.00209 0.00177 0.00160 0.00176 0.00085 C7 0.09916 0.71342 -0.05912 1.00000 0.02469 0.02386 0.02798 0.00086 0.00672 -0.00123 0.02610 0.00696 0.00023 0.00044 0.00020 0.00000 0.00235 0.00213 0.00205 0.00169 0.00171 0.00183 0.00089 C8 0.18154 0.62964 -0.02631 1.00000 0.02168 0.02577 0.03142 -0.00174 0.00939 -0.00030 0.02621 0.00685 0.00022 0.00045 0.00020 0.00000 0.00226 0.00214 0.00211 0.00181 0.00171 0.00190 0.00087 C9 0.26409 0.68998 -0.03401 1.00000 0.02066 0.03073 0.03378 0.00340 0.00633 -0.00002 0.02916 0.00728 0.00023 0.00047 0.00021 0.00000 0.00231 0.00246 0.00227 0.00174 0.00178 0.00187 0.00095 C10 0.28759 0.86052 -0.02236 1.00000 0.02279 0.03637 0.03455 -0.00020 0.00863 -0.00276 0.03153 0.00715 0.00023 0.00049 0.00020 0.00000 0.00235 0.00250 0.00220 0.00193 0.00176 0.00198 0.00094 H10 0.25074 0.93883 -0.00891 1.00000 0.03784 0.00000 0.00000 C11 0.36376 0.91878 -0.02995 1.00000 0.03244 0.04409 0.04346 -0.00267 0.00995 -0.01323 0.04077 0.00770 0.00026 0.00054 0.00022 0.00000 0.00272 0.00272 0.00249 0.00207 0.00204 0.00223 0.00109 H11 0.37921 1.03600 -0.02151 1.00000 0.04893 0.00000 0.00000 C12 0.41728 0.80519 -0.04992 1.00000 0.02367 0.06198 0.04503 0.00226 0.01302 -0.00664 0.04323 0.00838 0.00026 0.00059 0.00023 0.00000 0.00252 0.00331 0.00264 0.00226 0.00202 0.00238 0.00114 H12 0.46950 0.84477 -0.05551 1.00000 0.05187 0.00000 0.00000 C13 0.39550 0.63663 -0.06162 1.00000 0.03180 0.05120 0.05003 -0.00317 0.01803 0.00947 0.04329 0.00855 0.00026 0.00058 0.00022 0.00000 0.00277 0.00303 0.00270 0.00230 0.00210 0.00236 0.00110 H13 0.43258 0.55948 -0.07542 1.00000 0.05195 0.00000 0.00000 C14 0.31923 0.57707 -0.05345 1.00000 0.02929 0.03694 0.03850 -0.00311 0.00942 0.00152 0.03547 0.00755 0.00025 0.00050 0.00020 0.00000 0.00258 0.00250 0.00238 0.00194 0.00195 0.00207 0.00101 H14 0.30471 0.45931 -0.06114 1.00000 0.04256 0.00000 0.00000 C15 0.17243 0.49324 0.01675 1.00000 0.01826 0.02384 0.03373 -0.00055 0.00619 -0.00058 0.02597 0.00679 0.00023 0.00044 0.00020 0.00000 0.00226 0.00217 0.00218 0.00177 0.00169 0.00178 0.00088 C16 0.24270 0.37556 0.06591 1.00000 0.01978 0.02293 0.03791 0.00475 0.00836 -0.00219 0.02725 0.00732 0.00023 0.00048 0.00021 0.00000 0.00220 0.00223 0.00235 0.00198 0.00177 0.00190 0.00088 C17 0.35013 0.35431 0.19928 1.00000 0.01775 0.02345 0.03470 0.00033 0.00250 0.00110 0.02696 0.00675 0.00022 0.00044 0.00020 0.00000 0.00218 0.00215 0.00221 0.00177 0.00168 0.00181 0.00089 C18 0.35353 0.36234 0.27673 1.00000 0.03059 0.03401 0.03938 0.00021 0.01251 0.00354 0.03452 0.00726 0.00024 0.00046 0.00021 0.00000 0.00256 0.00240 0.00241 0.00200 0.00192 0.00202 0.00099 H18 0.30862 0.41797 0.28937 1.00000 0.04142 0.00000 0.00000 C19 0.42243 0.28923 0.33584 1.00000 0.03857 0.04352 0.03683 0.00450 0.00687 0.00430 0.04119 0.00797 0.00027 0.00050 0.00024 0.00000 0.00279 0.00267 0.00245 0.00204 0.00212 0.00225 0.00108 H19 0.42468 0.29563 0.38884 1.00000 0.04943 0.00000 0.00000 C20 0.48756 0.20744 0.31787 1.00000 0.03078 0.04318 0.04682 0.00485 -0.00295 0.00894 0.04443 0.00801 0.00027 0.00051 0.00025 0.00000 0.00274 0.00274 0.00292 0.00215 0.00213 0.00222 0.00115 H20 0.53422 0.15594 0.35823 1.00000 0.05332 0.00000 0.00000 C21 0.48463 0.20076 0.24100 1.00000 0.02417 0.03994 0.05342 0.00216 0.00731 0.00671 0.04071 0.00799 0.00025 0.00050 0.00025 0.00000 0.00251 0.00269 0.00288 0.00211 0.00210 0.00204 0.00109 H21 0.52978 0.14508 0.22875 1.00000 0.04885 0.00000 0.00000 C22 0.41682 0.27407 0.18146 1.00000 0.02812 0.03481 0.04034 -0.00064 0.01288 0.00158 0.03412 0.00748 0.00024 0.00047 0.00022 0.00000 0.00250 0.00241 0.00249 0.00193 0.00200 0.00204 0.00100 H22 0.41573 0.26972 0.12876 1.00000 0.04094 0.00000 0.00000 C23 0.04193 0.61979 -0.03376 1.00000 0.01831 0.01909 0.03173 0.00234 0.00308 0.00182 0.02445 0.00683 0.00022 0.00043 0.00020 0.00000 0.00220 0.00203 0.00201 0.00176 0.00162 0.00176 0.00085 C24 0.05128 0.36357 0.05110 1.00000 0.02312 0.02318 0.03061 0.00159 0.00508 -0.00143 0.02669 0.00681 0.00023 0.00046 0.00020 0.00000 0.00234 0.00215 0.00215 0.00187 0.00173 0.00195 0.00088 C25 0.18206 0.00211 0.22807 1.00000 0.05016 0.03762 0.04166 0.00117 0.01118 0.00463 0.04431 0.00774 0.00027 0.00048 0.00022 0.00000 0.00301 0.00256 0.00248 0.00204 0.00207 0.00228 0.00111 H25A 0.12128 0.00637 0.22463 1.00000 0.06646 0.00000 0.00000 H25B 0.20202 0.11771 0.22225 1.00000 0.06646 0.00000 0.00000 H25C 0.21730 -0.04446 0.27919 1.00000 0.06646 0.00000 0.00000 C26 0.30516 -0.10897 0.17490 1.00000 0.04329 0.05619 0.09488 -0.01165 0.03903 -0.01381 0.06081 0.00880 0.00027 0.00057 0.00028 0.00000 0.00306 0.00318 0.00376 0.00276 0.00274 0.00252 0.00137 H26A 0.32363 -0.17655 0.13791 1.00000 0.09121 0.00000 0.00000 H26B 0.33516 -0.14977 0.22845 1.00000 0.09121 0.00000 0.00000 H26C 0.31933 0.01161 0.17101 1.00000 0.09121 0.00000 0.00000 N1 0.08678 0.48449 0.01327 1.00000 0.01718 0.02560 0.03063 0.00440 0.00187 0.00369 0.02609 0.00544 0.00018 0.00036 0.00015 0.00000 0.00186 0.00181 0.00179 0.00144 0.00135 0.00148 0.00074 N2 0.27893 0.43148 0.14085 1.00000 0.01984 0.02567 0.03528 -0.00142 0.00516 0.00555 0.02803 0.00559 0.00018 0.00036 0.00016 0.00000 0.00189 0.00179 0.00189 0.00147 0.00147 0.00140 0.00077 H2A 0.25638 0.52326 0.15432 1.00000 0.03363 0.00000 0.00000 O1 0.26676 0.25352 0.03694 1.00000 0.03328 0.03360 0.04373 -0.00784 0.00247 0.01030 0.03962 0.00504 0.00017 0.00033 0.00015 0.00000 0.00176 0.00171 0.00169 0.00137 0.00130 0.00137 0.00072 O2 0.09690 0.25463 0.09309 1.00000 0.02113 0.03294 0.04638 0.01481 0.00460 0.00413 0.03527 0.00489 0.00015 0.00032 0.00015 0.00000 0.00158 0.00163 0.00171 0.00135 0.00128 0.00128 0.00069 O3 0.17930 -0.31044 0.17452 1.00000 0.03895 0.03216 0.06997 -0.00181 0.02976 0.00340 0.04415 0.00552 0.00017 0.00031 0.00017 0.00000 0.00186 0.00169 0.00202 0.00139 0.00152 0.00135 0.00076 S1 0.19217 -0.13097 0.15206 1.00000 0.03790 0.03574 0.04094 0.00042 0.01249 0.00611 0.03845 0.00211 0.00007 0.00013 0.00006 0.00000 0.00070 0.00065 0.00061 0.00053 0.00049 0.00055 0.00032 Final Structure Factor Calculation for 01sot025 in P2(1)/c Total number of l.s. parameters = 290 Maximum vector length = 511 Memory required = 2833 / 24017 wR2 = 0.1363 before cycle 6 for 3848 data and 0 / 290 parameters GooF = S = 0.947; Restrained GooF = 0.947 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0413 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0580 for 1938 Fo > 4sig(Fo) and 0.1481 for all 3848 data wR2 = 0.1363, GooF = S = 0.947, Restrained GooF = 0.947 for all data Occupancy sum of asymmetric unit = 32.00 for non-hydrogen and 22.00 for hydrogen atoms Principal mean square atomic displacements U 0.0476 0.0327 0.0267 C1 0.0529 0.0382 0.0274 C2 0.0526 0.0284 0.0261 C3 0.0527 0.0330 0.0267 C4 0.0405 0.0377 0.0259 C5 0.0331 0.0249 0.0142 C6 0.0307 0.0246 0.0230 C7 0.0321 0.0253 0.0212 C8 0.0379 0.0289 0.0206 C9 0.0371 0.0353 0.0222 C10 0.0534 0.0451 0.0238 C11 0.0639 0.0448 0.0210 C12 0.0568 0.0492 0.0238 C13 0.0429 0.0345 0.0290 C14 0.0358 0.0239 0.0182 C15 0.0410 0.0231 0.0177 C16 0.0403 0.0236 0.0169 C17 0.0395 0.0362 0.0278 C18 0.0469 0.0458 0.0309 C19 0.0654 0.0467 0.0212 C20 0.0580 0.0424 0.0217 C21 0.0405 0.0351 0.0267 C22 0.0367 0.0205 0.0161 C23 0.0351 0.0233 0.0217 C24 0.0554 0.0418 0.0358 C25 0.0995 0.0555 0.0274 C26 0.0370 0.0268 0.0145 N1 0.0400 0.0276 0.0165 N2 0.0637 0.0322 0.0230 O1 0.0594 0.0286 0.0178 O2 0.0710 0.0354 0.0260 O3 0.0440 0.0408 0.0305 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.016 0.024 0.033 0.043 0.055 0.071 0.092 0.136 1.000 Number in group 407. 393. 383. 385. 370. 369. 387. 382. 391. 381. GooF 0.743 0.830 0.842 0.916 0.917 0.952 1.002 1.025 0.912 1.256 K 0.744 1.702 0.807 0.973 0.967 1.010 0.974 0.985 1.003 1.009 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.26 1.44 1.80 inf Number in group 386. 391. 383. 390. 379. 378. 394. 377. 385. 385. GooF 0.813 0.817 0.830 0.910 0.909 0.908 0.889 0.883 0.991 1.385 K 1.005 1.005 1.007 0.987 0.999 1.012 0.982 1.013 1.029 0.998 R1 0.414 0.333 0.296 0.217 0.171 0.125 0.098 0.074 0.062 0.050 Recommended weighting scheme: WGHT 0.0408 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 2 5 558.05 385.97 4.40 0.085 2.27 -1 1 5 2075.21 2636.88 4.37 0.221 3.27 -1 1 2 2134.62 2620.89 4.31 0.220 5.86 1 2 1 2462.39 2961.52 4.03 0.234 3.64 4 2 4 439.77 321.93 3.95 0.077 2.09 -1 1 6 1924.67 2337.52 3.79 0.208 2.78 0 2 1 11172.10 13227.16 3.76 0.495 3.81 15 2 2 61.87 280.83 3.66 0.072 0.95 -2 2 1 2566.95 3042.15 3.61 0.238 3.53 -2 3 7 167.05 104.73 3.35 0.044 1.84 -1 2 3 6620.13 7642.46 3.25 0.376 3.28 -7 2 13 71.51 24.31 3.22 0.021 1.27 -16 4 4 197.60 439.32 3.22 0.090 0.90 -5 1 11 22.11 48.22 3.11 0.030 1.59 9 1 5 -28.55 52.36 3.11 0.031 1.34 -1 2 1 1337.61 1552.13 3.11 0.170 3.77 -4 3 14 550.78 839.88 3.09 0.125 1.16 -2 0 16 735.10 530.64 3.09 0.099 1.11 0 1 17 159.34 60.96 3.08 0.034 0.99 6 2 1 158.50 99.44 3.07 0.043 2.06 0 4 2 -3.46 54.41 3.03 0.032 1.91 -5 2 18 -25.37 81.97 3.01 0.039 0.97 -1 3 6 1387.14 1610.48 3.00 0.173 1.96 -9 4 18 76.03 286.00 2.94 0.073 0.88 -11 5 13 48.93 147.58 2.92 0.052 0.94 -7 1 10 64.90 20.62 2.91 0.020 1.61 -3 1 11 187.26 270.42 2.91 0.071 1.61 0 2 3 3247.69 3709.80 2.91 0.262 3.22 -6 0 10 2487.57 2080.37 2.91 0.196 1.72 3 1 2 1305.44 1122.73 2.91 0.144 3.46 -4 1 9 145.61 211.66 2.90 0.063 1.93 -7 1 5 301.17 229.66 2.87 0.065 2.15 -5 5 11 61.50 2.18 2.84 0.006 1.13 1 2 0 4265.36 4863.87 2.83 0.300 3.79 3 2 6 609.81 515.66 2.82 0.098 1.91 -4 9 4 305.29 26.66 2.80 0.022 0.84 -6 5 7 163.72 260.66 2.78 0.070 1.27 2 3 4 471.12 386.57 2.77 0.085 2.04 1 1 2 1281.13 1455.87 2.77 0.164 5.03 -8 1 7 114.03 58.38 2.76 0.033 1.80 6 2 0 2193.07 1907.39 2.75 0.188 2.15 -2 3 3 163.33 230.96 2.73 0.065 2.36 -2 0 4 3023.33 3473.15 2.72 0.254 4.42 -1 3 15 1862.68 1426.31 2.71 0.163 1.06 5 1 4 1178.43 1010.13 2.70 0.137 2.09 -14 2 5 621.48 809.90 2.70 0.123 1.12 12 1 10 362.36 157.70 2.69 0.054 0.89 -6 0 6 4004.50 3427.05 2.69 0.252 2.35 0 1 5 15.70 31.23 2.68 0.024 3.12 8 0 4 4116.70 3558.70 2.67 0.257 1.57 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.94 2.795(4) 164.9 N2-H2A...O3_$1 0.88 2.90 3.741(3) 160.6 N2-H2A...S1_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)