+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src1281 started at 16:24:31 on 13-Jan-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src1281 in P2(1)2(1)2(1) CELL 0.71073 8.1593 15.4230 22.8878 90.000 90.000 90.000 ZERR 8.00 0.0004 0.0008 0.0009 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O S UNIT 120 136 24 16 8 V = 2880.22 F(000) = 1280.0 Mu = 0.23 mm-1 Cell Wt = 2427.01 Rho = 1.399 MERG 2 OMIT -3.00 55.00 OMIT 0 0 4 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.10 0.15 0.20 ACTA BOND $H WGHT 0.05210 L.S. 4 TEMP -153.00 FVAR 0.44120 MOLE 1 C2 1 0.858995 0.113342 0.365400 11.00000 0.03159 0.03469 = 0.02805 0.00294 -0.00089 -0.00496 AFIX 43 H2 2 0.822941 0.122498 0.404382 11.00000 -1.20000 AFIX 0 C3 1 1.015383 0.087130 0.357524 11.00000 0.03366 0.03194 = 0.03262 -0.00042 -0.00497 0.00268 AFIX 43 H3 2 1.085819 0.075811 0.389682 11.00000 -1.20000 AFIX 0 C4 1 1.069028 0.077386 0.299621 11.00000 0.02688 0.02219 = 0.04408 0.00446 0.00312 0.00022 AFIX 43 H4 2 1.178267 0.059368 0.291950 11.00000 -1.20000 AFIX 0 C5 1 0.964952 0.093682 0.254393 11.00000 0.01979 0.03122 = 0.02861 -0.00497 0.00022 -0.00617 AFIX 43 H5 2 1.002037 0.089431 0.215153 11.00000 -1.20000 AFIX 0 C6 1 0.802011 0.116862 0.266606 11.00000 0.02088 0.01768 = 0.03069 0.00225 -0.00267 0.00199 C8 1 0.710980 0.087239 0.166987 11.00000 0.02550 0.03838 = 0.02946 -0.00808 0.00144 0.00572 AFIX 23 H8A 2 0.689575 0.024600 0.172565 11.00000 -1.20000 H8B 2 0.826452 0.094018 0.154516 11.00000 -1.20000 AFIX 0 C9 1 0.599355 0.121800 0.119763 11.00000 0.02617 0.03841 = 0.02033 -0.00200 0.00375 0.00541 AFIX 23 H9A 2 0.628635 0.182648 0.110774 11.00000 -1.20000 H9B 2 0.612999 0.087074 0.083711 11.00000 -1.20000 AFIX 0 C11 1 0.404191 0.169303 0.193040 11.00000 0.02732 0.02440 = 0.02338 0.00470 0.00240 0.00241 AFIX 23 H11A 2 0.288265 0.166041 0.205619 11.00000 -1.20000 H11B 2 0.431271 0.230797 0.185252 11.00000 -1.20000 AFIX 0 C12 1 0.514911 0.133952 0.240801 11.00000 0.02154 0.03206 = 0.02408 0.00005 0.00030 -0.00107 AFIX 23 H12A 2 0.503882 0.170414 0.276182 11.00000 -1.20000 H12B 2 0.479869 0.074384 0.250981 11.00000 -1.20000 AFIX 0 C13 1 0.278817 0.235090 0.067014 11.00000 0.02688 0.02243 = 0.02171 -0.00043 -0.00725 -0.00122 C14 1 0.377368 0.263027 0.020956 11.00000 0.02328 0.03437 = 0.02525 0.00293 0.00119 0.00282 AFIX 43 H14 2 0.448680 0.223558 0.001742 11.00000 -1.20000 AFIX 0 C15 1 0.370150 0.349673 0.003356 11.00000 0.03241 0.03950 = 0.02788 0.00934 -0.00576 -0.01399 AFIX 43 H15 2 0.434612 0.369174 -0.028614 11.00000 -1.20000 AFIX 0 C16 1 0.268543 0.407152 0.032714 11.00000 0.03618 0.02844 = 0.03433 0.00231 -0.01025 -0.00604 AFIX 43 H16 2 0.265282 0.466272 0.021121 11.00000 -1.20000 AFIX 0 C17 1 0.171964 0.379292 0.078675 11.00000 0.03039 0.02863 = 0.02942 -0.00087 -0.00929 -0.00188 AFIX 43 H17 2 0.102206 0.419158 0.098239 11.00000 -1.20000 AFIX 0 C18 1 0.176723 0.293043 0.096322 11.00000 0.02387 0.03164 = 0.01995 0.00202 -0.00565 -0.00054 AFIX 43 H18 2 0.111026 0.273812 0.128046 11.00000 -1.20000 AFIX 0 N1 3 0.749131 0.127630 0.321675 11.00000 0.02809 0.03442 = 0.02330 -0.00396 0.00073 -0.00095 N7 3 0.686388 0.132562 0.222441 11.00000 0.02812 0.03061 = 0.01905 -0.00269 0.00259 0.00126 N10 3 0.428255 0.117334 0.139487 11.00000 0.02502 0.02786 = 0.01986 -0.00179 -0.00362 0.00225 O19 4 0.338728 0.075168 0.040330 11.00000 0.04707 0.02710 = 0.02992 -0.01041 -0.00650 0.00244 O20 4 0.133488 0.106890 0.117548 11.00000 0.02580 0.03387 = 0.03419 0.00882 -0.00646 -0.00739 S1 5 0.285940 0.125803 0.089296 11.00000 0.02940 0.02313 = 0.02638 -0.00086 -0.00302 -0.00149 MOLE 2 C22 1 0.756660 0.358602 0.139842 11.00000 0.03751 0.03446 = 0.02726 0.00099 -0.00575 -0.00269 AFIX 43 H22 2 0.793512 0.348729 0.101035 11.00000 -1.20000 AFIX 0 C23 1 0.597723 0.385308 0.146857 11.00000 0.02967 0.02982 = 0.03223 0.00501 -0.00775 -0.00240 AFIX 43 H23 2 0.527121 0.393927 0.114367 11.00000 -1.20000 AFIX 0 C24 1 0.544694 0.399208 0.203934 11.00000 0.02705 0.02977 = 0.03748 0.00237 -0.00371 0.00155 AFIX 43 H24 2 0.434974 0.416834 0.211132 11.00000 -1.20000 AFIX 0 C25 1 0.651553 0.387380 0.250121 11.00000 0.02342 0.03051 = 0.03045 -0.00037 -0.00174 0.00439 AFIX 43 H25 2 0.617219 0.398089 0.289120 11.00000 -1.20000 AFIX 0 C26 1 0.812764 0.359068 0.238218 11.00000 0.02973 0.02477 = 0.02366 -0.00047 0.00110 -0.00394 C28 1 0.895083 0.381886 0.340472 11.00000 0.02656 0.03329 = 0.02119 -0.00193 0.00171 -0.00100 AFIX 23 H28A 2 0.780805 0.368924 0.352091 11.00000 -1.20000 H28B 2 0.907418 0.445685 0.338649 11.00000 -1.20000 AFIX 0 C29 1 1.010587 0.346074 0.385876 11.00000 0.02291 0.02999 = 0.02656 -0.00584 0.00918 -0.00383 AFIX 23 H29A 2 0.992981 0.376149 0.423571 11.00000 -1.20000 H29B 2 0.988880 0.283518 0.391722 11.00000 -1.20000 AFIX 0 C31 1 1.211392 0.312212 0.311429 11.00000 0.02764 0.02796 = 0.02549 -0.00332 0.00036 0.00423 AFIX 23 H31A 2 1.189139 0.249619 0.316819 11.00000 -1.20000 H31B 2 1.327392 0.319075 0.299619 11.00000 -1.20000 AFIX 0 C32 1 1.100140 0.348573 0.264455 11.00000 0.02087 0.03395 = 0.02902 -0.00287 0.00356 0.00467 AFIX 23 H32A 2 1.130535 0.409626 0.256646 11.00000 -1.20000 H32B 2 1.115883 0.315289 0.227898 11.00000 -1.20000 AFIX 0 C33 1 1.338529 0.241594 0.437350 11.00000 0.01888 0.02414 = 0.02141 -0.00182 -0.00444 -0.00242 C34 1 1.236699 0.210118 0.481853 11.00000 0.02265 0.03778 = 0.02422 -0.00276 -0.00024 0.00126 AFIX 43 H34 2 1.164644 0.248078 0.502068 11.00000 -1.20000 AFIX 0 C35 1 1.242706 0.122343 0.496005 11.00000 0.02082 0.04327 = 0.02355 0.00374 -0.00080 -0.00290 AFIX 43 H35 2 1.174526 0.099810 0.526030 11.00000 -1.20000 AFIX 0 C36 1 1.348908 0.068021 0.465970 11.00000 0.02446 0.02634 = 0.02816 0.00185 -0.00259 -0.00271 AFIX 43 H36 2 1.353128 0.008195 0.475736 11.00000 -1.20000 AFIX 0 C37 1 1.449489 0.099911 0.421686 11.00000 0.02536 0.03238 = 0.02327 0.00321 -0.00061 0.00336 AFIX 43 H37 2 1.521500 0.061921 0.401475 11.00000 -1.20000 AFIX 0 C38 1 1.444323 0.187062 0.407180 11.00000 0.02411 0.03219 = 0.02237 -0.00200 -0.00058 -0.00239 AFIX 43 H38 2 1.512282 0.209258 0.376978 11.00000 -1.20000 AFIX 0 N21 3 0.864435 0.345234 0.182998 11.00000 0.03524 0.02961 = 0.02501 0.00007 -0.00246 0.00084 N27 3 0.926958 0.344513 0.281721 11.00000 0.01750 0.02996 = 0.02216 -0.00124 0.00134 0.00234 N30 3 1.181679 0.358726 0.366367 11.00000 0.02153 0.02700 = 0.02804 -0.00254 -0.00031 0.00139 O39 4 1.267906 0.401041 0.465775 11.00000 0.04081 0.03184 = 0.02488 -0.01246 0.00255 0.00151 O40 4 1.475845 0.374635 0.387950 11.00000 0.02530 0.03005 = 0.03630 0.00035 0.00160 -0.00619 S2 5 1.324845 0.351871 0.416424 11.00000 0.02858 0.02561 = 0.02610 -0.00366 -0.00075 -0.00133 HKLF 4 Covalent radii and connectivity table for 2008src1281 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C2 - C3 N1 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - N1 N7 C5 C8 - N7 C9 C9 - N10 C8 C11 - N10 C12 C12 - N7 C11 C13 - C18 C14 S1 C14 - C13 C15 C15 - C16 C14 C16 - C17 C15 C17 - C16 C18 C18 - C17 C13 N1 - C6 C2 N7 - C6 C12 C8 N10 - C9 C11 S1 O19 - S1 O20 - S1 S1 - O20 O19 N10 C13 C22 - N21 C23 C23 - C22 C24 C24 - C25 C23 C25 - C24 C26 C26 - N21 N27 C25 C28 - N27 C29 C29 - N30 C28 C31 - N30 C32 C32 - N27 C31 C33 - C38 C34 S2 C34 - C35 C33 C35 - C36 C34 C36 - C35 C37 C37 - C38 C36 C38 - C37 C33 N21 - C22 C26 N27 - C26 C32 C28 N30 - C31 C29 S2 O39 - S2 O40 - S2 S2 - O40 O39 N30 C33 26927 Reflections read, of which 106 rejected -10 =< h =< 10, -19 =< k =< 19, -29 =< l =< 29, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 7 7 11 19.26 24.56 2 193.44 7 3 20 20.39 20.73 3 114.20 2 Inconsistent equivalents 6589 Unique reflections, of which 0 suppressed R(int) = 0.1554 R(sigma) = 0.1832 Friedel opposites not merged Maximum memory for data reduction = 3700 / 64987 Default effective X-H distances for T = -153.0 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 = 4784 / 484123 wR2 = 0.1584 before cycle 1 for 6589 data and 379 / 379 parameters GooF = S = 0.990; Restrained GooF = 0.990 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0521 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.44121 0.00088 0.011 OSF Mean shift/su = 0.001 Maximum = 0.011 for OSF Max. shift = 0.000 A for C18 Max. dU = 0.000 for C33 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4784 / 484123 wR2 = 0.1584 before cycle 2 for 6589 data and 379 / 379 parameters GooF = S = 0.990; Restrained GooF = 0.990 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0521 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.44121 0.00088 0.003 OSF Mean shift/su = 0.000 Maximum = 0.003 for OSF Max. shift = 0.000 A for H18 Max. dU = 0.000 for C33 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4784 / 484123 wR2 = 0.1584 before cycle 3 for 6589 data and 379 / 379 parameters GooF = S = 0.990; Restrained GooF = 0.990 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0521 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.44121 0.00088 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C3 Max. dU = 0.000 for C3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4784 / 484123 wR2 = 0.1584 before cycle 4 for 6589 data and 379 / 379 parameters GooF = S = 0.990; Restrained GooF = 0.990 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0521 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.44121 0.00088 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y S1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C32 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.8229 0.1225 0.4044 43 0.950 0.000 C2 C3 N1 H3 1.0858 0.0758 0.3897 43 0.950 0.000 C3 C2 C4 H4 1.1783 0.0594 0.2919 43 0.950 0.000 C4 C5 C3 H5 1.0020 0.0894 0.2152 43 0.950 0.000 C5 C4 C6 H8A 0.6896 0.0246 0.1726 23 0.990 0.000 C8 N7 C9 H8B 0.8265 0.0940 0.1545 23 0.990 0.000 C8 N7 C9 H9A 0.6286 0.1826 0.1108 23 0.990 0.000 C9 N10 C8 H9B 0.6130 0.0871 0.0837 23 0.990 0.000 C9 N10 C8 H11A 0.2883 0.1660 0.2056 23 0.990 0.000 C11 N10 C12 H11B 0.4313 0.2308 0.1853 23 0.990 0.000 C11 N10 C12 H12A 0.5039 0.1704 0.2762 23 0.990 0.000 C12 N7 C11 H12B 0.4799 0.0744 0.2510 23 0.990 0.000 C12 N7 C11 H14 0.4487 0.2236 0.0017 43 0.950 0.000 C14 C13 C15 H15 0.4346 0.3692 -0.0286 43 0.950 0.000 C15 C16 C14 H16 0.2653 0.4663 0.0211 43 0.950 0.000 C16 C17 C15 H17 0.1022 0.4192 0.0982 43 0.950 0.000 C17 C16 C18 H18 0.1110 0.2738 0.1280 43 0.950 0.000 C18 C17 C13 H22 0.7935 0.3487 0.1010 43 0.950 0.000 C22 N21 C23 H23 0.5271 0.3939 0.1144 43 0.950 0.000 C23 C22 C24 H24 0.4350 0.4168 0.2111 43 0.950 0.000 C24 C25 C23 H25 0.6172 0.3981 0.2891 43 0.950 0.000 C25 C24 C26 H28A 0.7808 0.3689 0.3521 23 0.990 0.000 C28 N27 C29 H28B 0.9074 0.4457 0.3386 23 0.990 0.000 C28 N27 C29 H29A 0.9930 0.3761 0.4236 23 0.990 0.000 C29 N30 C28 H29B 0.9889 0.2835 0.3917 23 0.990 0.000 C29 N30 C28 H31A 1.1891 0.2496 0.3168 23 0.990 0.000 C31 N30 C32 H31B 1.3274 0.3191 0.2996 23 0.990 0.000 C31 N30 C32 H32A 1.1305 0.4096 0.2566 23 0.990 0.000 C32 N27 C31 H32B 1.1159 0.3153 0.2279 23 0.990 0.000 C32 N27 C31 H34 1.1646 0.2481 0.5021 43 0.950 0.000 C34 C35 C33 H35 1.1745 0.0998 0.5260 43 0.950 0.000 C35 C36 C34 H36 1.3531 0.0082 0.4757 43 0.950 0.000 C36 C35 C37 H37 1.5215 0.0619 0.4015 43 0.950 0.000 C37 C38 C36 H38 1.5123 0.2093 0.3770 43 0.950 0.000 C38 C37 C33 2008src1281 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 0.85900 0.11334 0.36540 1.00000 0.03159 0.03469 0.02806 0.00293 -0.00089 -0.00496 0.03144 0.00823 0.00066 0.00030 0.00020 0.00000 0.00352 0.00287 0.00263 0.00239 0.00254 0.00253 0.00124 H2 0.82294 0.12250 0.40438 1.00000 0.03773 0.00000 0.00000 C3 1.01538 0.08713 0.35752 1.00000 0.03366 0.03194 0.03262 -0.00042 -0.00498 0.00268 0.03274 0.00879 0.00070 0.00031 0.00021 0.00000 0.00360 0.00285 0.00284 0.00243 0.00256 0.00246 0.00126 H3 1.08582 0.07581 0.38968 1.00000 0.03929 0.00000 0.00000 C4 1.06903 0.07739 0.29962 1.00000 0.02688 0.02220 0.04408 0.00446 0.00312 0.00022 0.03105 0.00860 0.00066 0.00029 0.00021 0.00000 0.00341 0.00253 0.00310 0.00240 0.00257 0.00218 0.00125 H4 1.17827 0.05937 0.29195 1.00000 0.03726 0.00000 0.00000 C5 0.96495 0.09368 0.25439 1.00000 0.01979 0.03122 0.02861 -0.00497 0.00022 -0.00617 0.02654 0.00795 0.00062 0.00030 0.00020 0.00000 0.00313 0.00265 0.00250 0.00231 0.00229 0.00216 0.00116 H5 1.00204 0.08943 0.21515 1.00000 0.03185 0.00000 0.00000 C6 0.80201 0.11686 0.26661 1.00000 0.02089 0.01768 0.03069 0.00225 -0.00267 0.00199 0.02308 0.00790 0.00060 0.00027 0.00019 0.00000 0.00303 0.00218 0.00257 0.00211 0.00218 0.00212 0.00108 C8 0.71098 0.08724 0.16699 1.00000 0.02550 0.03838 0.02947 -0.00808 0.00144 0.00572 0.03112 0.00832 0.00066 0.00032 0.00018 0.00000 0.00328 0.00280 0.00260 0.00229 0.00234 0.00250 0.00124 H8A 0.68958 0.02460 0.17257 1.00000 0.03734 0.00000 0.00000 H8B 0.82645 0.09402 0.15452 1.00000 0.03734 0.00000 0.00000 C9 0.59935 0.12180 0.11976 1.00000 0.02617 0.03841 0.02033 -0.00200 0.00375 0.00541 0.02831 0.00859 0.00061 0.00033 0.00019 0.00000 0.00304 0.00295 0.00224 0.00230 0.00208 0.00246 0.00118 H9A 0.62863 0.18265 0.11077 1.00000 0.03397 0.00000 0.00000 H9B 0.61300 0.08707 0.08371 1.00000 0.03397 0.00000 0.00000 C11 0.40419 0.16930 0.19304 1.00000 0.02732 0.02441 0.02338 0.00470 0.00240 0.00241 0.02504 0.00799 0.00063 0.00029 0.00018 0.00000 0.00318 0.00249 0.00250 0.00206 0.00220 0.00217 0.00116 H11A 0.28827 0.16604 0.20562 1.00000 0.03004 0.00000 0.00000 H11B 0.43127 0.23080 0.18525 1.00000 0.03004 0.00000 0.00000 C12 0.51491 0.13395 0.24080 1.00000 0.02154 0.03206 0.02408 0.00005 0.00030 -0.00107 0.02589 0.00814 0.00061 0.00031 0.00018 0.00000 0.00298 0.00275 0.00254 0.00230 0.00214 0.00226 0.00113 H12A 0.50388 0.17041 0.27618 1.00000 0.03107 0.00000 0.00000 H12B 0.47987 0.07438 0.25098 1.00000 0.03107 0.00000 0.00000 C13 0.27882 0.23509 0.06701 1.00000 0.02688 0.02243 0.02171 -0.00044 -0.00724 -0.00122 0.02367 0.00740 0.00060 0.00027 0.00018 0.00000 0.00294 0.00234 0.00236 0.00196 0.00218 0.00218 0.00109 C14 0.37737 0.26303 0.02096 1.00000 0.02329 0.03437 0.02525 0.00293 0.00120 0.00282 0.02764 0.00828 0.00062 0.00031 0.00019 0.00000 0.00309 0.00274 0.00252 0.00224 0.00226 0.00226 0.00116 H14 0.44868 0.22356 0.00174 1.00000 0.03316 0.00000 0.00000 C15 0.37015 0.34967 0.00336 1.00000 0.03241 0.03951 0.02788 0.00934 -0.00576 -0.01400 0.03327 0.00807 0.00065 0.00032 0.00020 0.00000 0.00337 0.00302 0.00261 0.00254 0.00240 0.00265 0.00127 H15 0.43461 0.36917 -0.02861 1.00000 0.03992 0.00000 0.00000 C16 0.26854 0.40715 0.03271 1.00000 0.03618 0.02844 0.03433 0.00231 -0.01025 -0.00604 0.03299 0.00823 0.00066 0.00031 0.00021 0.00000 0.00359 0.00264 0.00284 0.00236 0.00263 0.00246 0.00129 H16 0.26528 0.46627 0.02112 1.00000 0.03958 0.00000 0.00000 C17 0.17196 0.37929 0.07867 1.00000 0.03039 0.02863 0.02943 -0.00087 -0.00929 -0.00188 0.02948 0.00756 0.00061 0.00029 0.00020 0.00000 0.00312 0.00257 0.00255 0.00240 0.00236 0.00239 0.00117 H17 0.10221 0.41916 0.09824 1.00000 0.03538 0.00000 0.00000 C18 0.17672 0.29304 0.09632 1.00000 0.02387 0.03164 0.01995 0.00202 -0.00565 -0.00054 0.02515 0.00741 0.00060 0.00028 0.00018 0.00000 0.00298 0.00254 0.00231 0.00212 0.00219 0.00223 0.00111 H18 0.11103 0.27381 0.12805 1.00000 0.03018 0.00000 0.00000 N1 0.74913 0.12763 0.32168 1.00000 0.02809 0.03442 0.02330 -0.00396 0.00073 -0.00095 0.02860 0.00656 0.00052 0.00025 0.00015 0.00000 0.00268 0.00230 0.00203 0.00188 0.00188 0.00204 0.00099 N7 0.68639 0.13256 0.22244 1.00000 0.02813 0.03061 0.01905 -0.00269 0.00259 0.00126 0.02593 0.00639 0.00050 0.00024 0.00015 0.00000 0.00269 0.00214 0.00190 0.00174 0.00176 0.00198 0.00094 N10 0.42826 0.11733 0.13949 1.00000 0.02502 0.02786 0.01986 -0.00179 -0.00362 0.00225 0.02425 0.00639 0.00048 0.00024 0.00015 0.00000 0.00254 0.00215 0.00194 0.00184 0.00175 0.00186 0.00093 O19 0.33873 0.07517 0.04033 1.00000 0.04708 0.02710 0.02992 -0.01040 -0.00650 0.00243 0.03470 0.00554 0.00046 0.00019 0.00013 0.00000 0.00260 0.00177 0.00170 0.00156 0.00175 0.00171 0.00089 O20 0.13349 0.10689 0.11755 1.00000 0.02581 0.03387 0.03419 0.00882 -0.00646 -0.00739 0.03129 0.00555 0.00043 0.00020 0.00013 0.00000 0.00221 0.00194 0.00177 0.00158 0.00163 0.00167 0.00085 S1 0.28594 0.12580 0.08930 1.00000 0.02940 0.02314 0.02638 -0.00086 -0.00302 -0.00149 0.02631 0.00200 0.00016 0.00007 0.00005 0.00000 0.00076 0.00060 0.00064 0.00054 0.00057 0.00054 0.00030 C22 0.75666 0.35860 0.13984 1.00000 0.03752 0.03446 0.02726 0.00099 -0.00575 -0.00269 0.03308 0.00818 0.00067 0.00030 0.00020 0.00000 0.00360 0.00292 0.00267 0.00240 0.00248 0.00256 0.00127 H22 0.79351 0.34873 0.10104 1.00000 0.03970 0.00000 0.00000 C23 0.59772 0.38531 0.14686 1.00000 0.02967 0.02982 0.03223 0.00501 -0.00775 -0.00240 0.03057 0.00837 0.00065 0.00030 0.00021 0.00000 0.00344 0.00278 0.00278 0.00242 0.00237 0.00246 0.00123 H23 0.52712 0.39393 0.11437 1.00000 0.03669 0.00000 0.00000 C24 0.54469 0.39921 0.20393 1.00000 0.02705 0.02978 0.03748 0.00237 -0.00372 0.00155 0.03143 0.00830 0.00066 0.00031 0.00020 0.00000 0.00338 0.00278 0.00284 0.00246 0.00256 0.00232 0.00126 H24 0.43497 0.41683 0.21113 1.00000 0.03772 0.00000 0.00000 C25 0.65155 0.38738 0.25012 1.00000 0.02343 0.03051 0.03045 -0.00037 -0.00174 0.00439 0.02813 0.00815 0.00063 0.00029 0.00020 0.00000 0.00308 0.00261 0.00256 0.00238 0.00233 0.00231 0.00115 H25 0.61722 0.39809 0.28912 1.00000 0.03375 0.00000 0.00000 C26 0.81276 0.35907 0.23822 1.00000 0.02973 0.02477 0.02366 -0.00047 0.00110 -0.00394 0.02605 0.00792 0.00063 0.00029 0.00019 0.00000 0.00332 0.00244 0.00248 0.00220 0.00220 0.00232 0.00114 C28 0.89508 0.38189 0.34047 1.00000 0.02656 0.03329 0.02119 -0.00193 0.00171 -0.00100 0.02701 0.00816 0.00063 0.00031 0.00017 0.00000 0.00308 0.00274 0.00237 0.00222 0.00216 0.00241 0.00116 H28A 0.78081 0.36892 0.35209 1.00000 0.03242 0.00000 0.00000 H28B 0.90742 0.44569 0.33865 1.00000 0.03242 0.00000 0.00000 C29 1.01059 0.34607 0.38588 1.00000 0.02291 0.02999 0.02657 -0.00584 0.00919 -0.00383 0.02649 0.00811 0.00059 0.00032 0.00019 0.00000 0.00297 0.00271 0.00251 0.00220 0.00221 0.00230 0.00115 H29A 0.99298 0.37615 0.42357 1.00000 0.03179 0.00000 0.00000 H29B 0.98888 0.28352 0.39172 1.00000 0.03179 0.00000 0.00000 C31 1.21139 0.31221 0.31143 1.00000 0.02765 0.02796 0.02549 -0.00333 0.00036 0.00423 0.02703 0.00802 0.00066 0.00028 0.00018 0.00000 0.00318 0.00251 0.00254 0.00208 0.00229 0.00227 0.00116 H31A 1.18914 0.24962 0.31682 1.00000 0.03244 0.00000 0.00000 H31B 1.32739 0.31907 0.29962 1.00000 0.03244 0.00000 0.00000 C32 1.10014 0.34857 0.26446 1.00000 0.02087 0.03395 0.02902 -0.00287 0.00356 0.00467 0.02795 0.00842 0.00059 0.00032 0.00019 0.00000 0.00297 0.00271 0.00260 0.00234 0.00218 0.00228 0.00116 H32A 1.13053 0.40963 0.25665 1.00000 0.03354 0.00000 0.00000 H32B 1.11588 0.31529 0.22790 1.00000 0.03354 0.00000 0.00000 C33 1.33853 0.24159 0.43735 1.00000 0.01889 0.02415 0.02141 -0.00182 -0.00444 -0.00242 0.02148 0.00734 0.00057 0.00026 0.00018 0.00000 0.00278 0.00236 0.00233 0.00196 0.00210 0.00209 0.00105 C34 1.23670 0.21012 0.48185 1.00000 0.02265 0.03779 0.02423 -0.00276 -0.00024 0.00126 0.02822 0.00780 0.00062 0.00031 0.00019 0.00000 0.00314 0.00283 0.00246 0.00223 0.00226 0.00233 0.00118 H34 1.16464 0.24808 0.50207 1.00000 0.03387 0.00000 0.00000 C35 1.24271 0.12234 0.49601 1.00000 0.02082 0.04328 0.02355 0.00374 -0.00080 -0.00289 0.02922 0.00779 0.00059 0.00031 0.00019 0.00000 0.00296 0.00295 0.00240 0.00233 0.00213 0.00248 0.00116 H35 1.17453 0.09981 0.52603 1.00000 0.03506 0.00000 0.00000 C36 1.34891 0.06802 0.46597 1.00000 0.02447 0.02634 0.02816 0.00185 -0.00259 -0.00271 0.02632 0.00785 0.00061 0.00030 0.00019 0.00000 0.00315 0.00249 0.00254 0.00224 0.00232 0.00225 0.00113 H36 1.35313 0.00820 0.47574 1.00000 0.03159 0.00000 0.00000 C37 1.44949 0.09991 0.42169 1.00000 0.02536 0.03238 0.02328 0.00321 -0.00061 0.00335 0.02700 0.00806 0.00061 0.00030 0.00019 0.00000 0.00298 0.00276 0.00243 0.00233 0.00230 0.00216 0.00115 H37 1.52150 0.06192 0.40148 1.00000 0.03241 0.00000 0.00000 C38 1.44432 0.18706 0.40718 1.00000 0.02411 0.03219 0.02237 -0.00200 -0.00058 -0.00239 0.02622 0.00759 0.00060 0.00029 0.00019 0.00000 0.00300 0.00273 0.00254 0.00229 0.00231 0.00218 0.00115 H38 1.51228 0.20926 0.37698 1.00000 0.03147 0.00000 0.00000 N21 0.86443 0.34523 0.18300 1.00000 0.03524 0.02962 0.02501 0.00007 -0.00246 0.00084 0.02996 0.00692 0.00055 0.00025 0.00016 0.00000 0.00286 0.00217 0.00211 0.00189 0.00197 0.00209 0.00101 N27 0.92696 0.34451 0.28172 1.00000 0.01750 0.02996 0.02216 -0.00124 0.00134 0.00234 0.02321 0.00647 0.00047 0.00025 0.00015 0.00000 0.00254 0.00212 0.00204 0.00183 0.00174 0.00177 0.00092 N30 1.18168 0.35873 0.36637 1.00000 0.02154 0.02700 0.02804 -0.00254 -0.00030 0.00139 0.02553 0.00636 0.00048 0.00023 0.00015 0.00000 0.00246 0.00209 0.00204 0.00183 0.00176 0.00185 0.00093 O39 1.26791 0.40104 0.46577 1.00000 0.04081 0.03184 0.02489 -0.01246 0.00255 0.00151 0.03251 0.00546 0.00044 0.00020 0.00012 0.00000 0.00243 0.00180 0.00170 0.00149 0.00165 0.00162 0.00088 O40 1.47584 0.37463 0.38795 1.00000 0.02530 0.03005 0.03630 0.00035 0.00160 -0.00619 0.03055 0.00542 0.00042 0.00021 0.00013 0.00000 0.00214 0.00192 0.00184 0.00159 0.00159 0.00165 0.00084 S2 1.32485 0.35187 0.41642 1.00000 0.02858 0.02561 0.02610 -0.00366 -0.00074 -0.00133 0.02677 0.00201 0.00016 0.00007 0.00005 0.00000 0.00077 0.00062 0.00064 0.00057 0.00056 0.00053 0.00031 Final Structure Factor Calculation for 2008src1281 in P2(1)2(1)2(1) Total number of l.s. parameters = 379 Maximum vector length = 511 Memory required = 4407 / 26068 wR2 = 0.1584 before cycle 5 for 6589 data and 2 / 379 parameters GooF = S = 0.990; Restrained GooF = 0.990 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0521 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0724 for 3659 Fo > 4sig(Fo) and 0.1567 for all 6589 data wR2 = 0.1584, GooF = S = 0.990, Restrained GooF = 0.990 for all data Flack x parameter = -0.1934 with su 0.1128 Expected values are 0 (within 3 su'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 Occupancy sum of asymmetric unit = 42.00 for non-hydrogen and 34.00 for hydrogen atoms Principal mean square atomic displacements U 0.0391 0.0287 0.0266 C2 0.0389 0.0317 0.0276 C3 0.0455 0.0264 0.0213 C4 0.0367 0.0262 0.0168 C5 0.0316 0.0217 0.0160 C6 0.0441 0.0286 0.0206 C8 0.0405 0.0268 0.0176 C9 0.0314 0.0245 0.0192 C11 0.0322 0.0241 0.0214 C12 0.0320 0.0226 0.0164 C13 0.0360 0.0245 0.0225 C14 0.0548 0.0240 0.0210 C15 0.0475 0.0281 0.0233 C16 0.0393 0.0290 0.0202 C17 0.0323 0.0273 0.0158 C18 0.0359 0.0280 0.0220 N1 0.0314 0.0287 0.0177 N7 0.0302 0.0245 0.0180 N10 0.0508 0.0355 0.0178 O19 0.0473 0.0253 0.0212 O20 0.0314 0.0255 0.0221 S1 0.0413 0.0333 0.0247 C22 0.0413 0.0277 0.0227 C23 0.0390 0.0304 0.0248 C24 0.0331 0.0302 0.0211 C25 0.0321 0.0235 0.0226 C26 0.0338 0.0267 0.0205 C28 0.0393 0.0248 0.0153 C29 0.0327 0.0267 0.0216 C31 0.0359 0.0302 0.0177 C32 0.0251 0.0248 0.0146 C33 0.0384 0.0237 0.0225 C34 0.0443 0.0229 0.0204 C35 0.0313 0.0254 0.0223 C36 0.0344 0.0251 0.0214 C37 0.0331 0.0240 0.0215 C38 0.0359 0.0295 0.0244 N21 0.0305 0.0225 0.0166 N27 0.0303 0.0251 0.0212 N30 0.0416 0.0409 0.0151 O39 0.0366 0.0341 0.0209 O40 0.0297 0.0287 0.0219 S2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.019 0.028 0.037 0.047 0.056 0.069 0.085 0.105 0.147 1.000 Number in group 688. 665. 651. 679. 620. 697. 633. 633. 664. 659. GooF 0.879 0.928 0.928 0.967 1.023 1.022 1.078 1.055 1.012 0.999 K 2.907 1.440 1.069 1.023 1.117 1.031 1.007 1.035 1.023 0.992 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 667. 650. 672. 655. 650. 668. 659. 652. 653. 663. GooF 0.880 0.889 0.940 0.991 1.026 0.992 1.057 0.955 0.998 1.144 K 1.075 1.131 1.098 1.148 1.116 1.020 1.010 1.019 1.021 0.975 R1 0.348 0.335 0.297 0.255 0.216 0.131 0.095 0.055 0.054 0.043 Recommended weighting scheme: WGHT 0.0521 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)/su Fc/Fc(max) Resolution(A) 2 11 19 1917.09 15.41 3.97 0.017 0.89 1 0 16 81.48 184.90 3.78 0.057 1.41 9 1 4 1546.09 834.98 3.76 0.122 0.89 4 11 4 272.07 479.18 3.65 0.092 1.13 4 4 5 2505.62 1923.57 3.47 0.185 1.68 -7 6 16 510.96 81.03 3.31 0.038 0.85 5 4 17 400.91 595.32 3.26 0.103 1.00 1 1 1 745.65 946.13 3.25 0.130 6.88 -8 8 11 43.57 237.72 3.22 0.065 0.83 -2 2 13 418.37 298.38 3.21 0.073 1.58 7 8 12 264.81 55.44 3.20 0.031 0.88 -5 4 12 69.49 154.99 3.19 0.053 1.18 -1 7 8 970.32 736.37 3.19 0.115 1.71 -1 5 13 1154.59 871.90 3.18 0.125 1.50 2 8 24 397.15 58.13 3.14 0.032 0.84 -6 1 4 397.98 609.21 3.13 0.104 1.32 8 7 0 19.81 216.04 3.13 0.062 0.93 2 11 23 649.90 143.80 3.12 0.051 0.80 2 5 22 890.22 617.07 3.09 0.105 0.96 -1 16 10 241.99 709.17 3.08 0.112 0.88 -6 3 10 -18.14 131.17 3.08 0.048 1.14 8 5 6 -16.10 270.24 3.04 0.069 0.94 0 3 10 963.43 786.34 3.01 0.118 2.09 0 6 22 2350.10 1425.80 3.01 0.160 0.96 5 7 15 897.95 611.13 2.97 0.104 0.99 -2 5 19 733.38 982.32 2.94 0.132 1.08 4 6 2 281.39 146.91 2.94 0.051 1.58 -6 8 13 16.88 117.84 2.93 0.046 0.94 3 0 13 160.44 236.23 2.90 0.065 1.48 0 17 1 184.38 28.99 2.90 0.023 0.91 -7 1 11 521.02 277.59 2.89 0.070 1.01 0 4 29 -108.21 148.40 2.87 0.051 0.77 -5 11 2 753.11 515.81 2.86 0.096 1.06 0 13 7 437.26 597.06 2.86 0.103 1.12 6 4 13 279.49 427.65 2.82 0.087 1.04 -8 3 10 257.91 56.97 2.82 0.032 0.92 -1 5 8 410.00 275.77 2.81 0.070 2.03 1 0 10 494.95 378.41 2.80 0.082 2.20 6 7 13 221.40 36.76 2.79 0.026 0.97 -3 1 25 330.40 150.32 2.79 0.052 0.87 1 9 25 1111.08 568.71 2.78 0.101 0.80 -9 3 5 251.67 19.17 2.76 0.018 0.88 -2 6 26 420.46 12.47 2.75 0.015 0.82 -1 8 7 953.34 758.10 2.74 0.116 1.63 7 11 4 656.91 295.30 2.74 0.073 0.89 6 5 12 292.96 113.17 2.74 0.045 1.04 6 4 10 20.92 136.18 2.72 0.049 1.12 -5 10 6 1255.51 963.93 2.72 0.131 1.08 3 9 12 -38.00 27.72 2.70 0.022 1.15 3 0 11 435.20 299.96 2.69 0.073 1.65 Bond lengths and angles C2 - Distance Angles C3 1.3506 (0.0074) N1 1.3615 (0.0060) 124.92 (0.46) H2 0.9500 117.54 117.54 C2 - C3 N1 C3 - Distance Angles C2 1.3506 (0.0074) C4 1.4037 (0.0065) 116.91 (0.49) H3 0.9500 121.54 121.54 C3 - C2 C4 C4 - Distance Angles C5 1.3623 (0.0066) C3 1.4037 (0.0065) 120.22 (0.50) H4 0.9500 119.89 119.89 C4 - C5 C3 C5 - Distance Angles C4 1.3623 (0.0066) C6 1.4048 (0.0069) 119.06 (0.44) H5 0.9500 120.47 120.47 C5 - C4 C6 C6 - Distance Angles N1 1.3425 (0.0055) N7 1.4037 (0.0058) 116.02 (0.42) C5 1.4048 (0.0069) 121.50 (0.43) 122.46 (0.41) C6 - N1 N7 C8 - Distance Angles N7 1.4628 (0.0052) C9 1.5106 (0.0063) 111.69 (0.39) H8A 0.9900 109.28 109.28 H8B 0.9900 109.28 109.28 107.95 C8 - N7 C9 H8A C9 - Distance Angles N10 1.4688 (0.0060) C8 1.5106 (0.0063) 109.67 (0.37) H9A 0.9900 109.74 109.74 H9B 0.9900 109.74 109.74 108.21 C9 - N10 C8 H9A C11 - Distance Angles N10 1.4776 (0.0053) C12 1.5193 (0.0062) 108.85 (0.36) H11A 0.9900 109.92 109.92 H11B 0.9900 109.92 109.92 108.32 C11 - N10 C12 H11A C12 - Distance Angles N7 1.4610 (0.0061) C11 1.5193 (0.0062) 111.58 (0.36) H12A 0.9900 109.31 109.31 H12B 0.9900 109.31 109.31 107.96 C12 - N7 C11 H12A C13 - Distance Angles C18 1.3938 (0.0063) C14 1.3941 (0.0064) 120.69 (0.41) S1 1.7620 (0.0043) 119.59 (0.35) 119.70 (0.36) C13 - C18 C14 C14 - Distance Angles C13 1.3941 (0.0064) C15 1.3970 (0.0065) 119.30 (0.47) H14 0.9500 120.35 120.35 C14 - C13 C15 C15 - Distance Angles C16 1.3873 (0.0069) C14 1.3970 (0.0065) 119.79 (0.46) H15 0.9500 120.11 120.11 C15 - C16 C14 C16 - Distance Angles C17 1.3828 (0.0066) C15 1.3873 (0.0069) 120.69 (0.44) H16 0.9500 119.65 119.65 C16 - C17 C15 C17 - Distance Angles C16 1.3828 (0.0066) C18 1.3907 (0.0058) 120.15 (0.47) H17 0.9500 119.93 119.93 C17 - C16 C18 C18 - Distance Angles C17 1.3907 (0.0058) C13 1.3938 (0.0063) 119.36 (0.43) H18 0.9500 120.32 120.32 C18 - C17 C13 N1 - Distance Angles C6 1.3425 (0.0055) C2 1.3615 (0.0060) 117.29 (0.44) N1 - C6 N7 - Distance Angles C6 1.4037 (0.0059) C12 1.4610 (0.0061) 116.04 (0.35) C8 1.4628 (0.0052) 116.76 (0.37) 112.83 (0.38) N7 - C6 C12 N10 - Distance Angles C9 1.4688 (0.0060) C11 1.4776 (0.0053) 110.84 (0.37) S1 1.6386 (0.0038) 117.02 (0.29) 116.37 (0.31) N10 - C9 C11 O19 - Distance Angles S1 1.4323 (0.0032) O19 - O20 - Distance Angles S1 1.4320 (0.0036) O20 - S1 - Distance Angles O20 1.4320 (0.0036) O19 1.4323 (0.0032) 120.23 (0.21) N10 1.6386 (0.0038) 106.43 (0.19) 106.98 (0.21) C13 1.7620 (0.0043) 107.27 (0.22) 107.76 (0.20) 107.61 (0.21) S1 - O20 O19 N10 C22 - Distance Angles N21 1.3384 (0.0059) C23 1.3701 (0.0072) 125.57 (0.45) H22 0.9500 117.22 117.22 C22 - N21 C23 C23 - Distance Angles C22 1.3701 (0.0072) C24 1.3927 (0.0066) 116.76 (0.46) H23 0.9500 121.62 121.62 C23 - C22 C24 C24 - Distance Angles C25 1.3824 (0.0064) C23 1.3927 (0.0066) 120.07 (0.50) H24 0.9500 119.97 119.97 C24 - C25 C23 C25 - Distance Angles C24 1.3824 (0.0064) C26 1.4125 (0.0070) 118.73 (0.44) H25 0.9500 120.64 120.64 C25 - C24 C26 C26 - Distance Angles N21 1.3493 (0.0055) N27 1.3820 (0.0056) 116.01 (0.43) C25 1.4125 (0.0070) 121.37 (0.43) 122.62 (0.40) C26 - N21 N27 C28 - Distance Angles N27 1.4860 (0.0051) C29 1.5077 (0.0064) 111.85 (0.38) H28A 0.9900 109.24 109.24 H28B 0.9900 109.24 109.24 107.92 C28 - N27 C29 H28A C29 - Distance Angles N30 1.4786 (0.0059) C28 1.5077 (0.0064) 109.49 (0.37) H29A 0.9900 109.77 109.77 H29B 0.9900 109.77 109.77 108.23 C29 - N30 C28 H29A C31 - Distance Angles N30 1.4678 (0.0051) C32 1.5147 (0.0061) 109.15 (0.37) H31A 0.9900 109.85 109.85 H31B 0.9900 109.85 109.85 108.28 C31 - N30 C32 H31A C32 - Distance Angles N27 1.4686 (0.0058) C31 1.5147 (0.0061) 111.71 (0.38) H32A 0.9900 109.28 109.28 H32B 0.9900 109.28 109.28 107.94 C32 - N27 C31 H32A C33 - Distance Angles C38 1.3890 (0.0059) C34 1.4012 (0.0062) 121.34 (0.40) S2 1.7705 (0.0042) 119.10 (0.33) 119.48 (0.35) C33 - C38 C34 C34 - Distance Angles C35 1.3928 (0.0063) C33 1.4012 (0.0062) 119.01 (0.44) H34 0.9500 120.50 120.50 C34 - C35 C33 C35 - Distance Angles C36 1.3876 (0.0063) C34 1.3928 (0.0063) 119.58 (0.45) H35 0.9500 120.21 120.21 C35 - C36 C34 C36 - Distance Angles C35 1.3876 (0.0063) C37 1.3938 (0.0063) 120.99 (0.45) H36 0.9500 119.50 119.50 C36 - C35 C37 C37 - Distance Angles C38 1.3852 (0.0061) C36 1.3938 (0.0063) 119.92 (0.47) H37 0.9500 120.04 120.04 C37 - C38 C36 C38 - Distance Angles C37 1.3852 (0.0061) C33 1.3890 (0.0059) 119.17 (0.43) H38 0.9500 120.42 120.42 C38 - C37 C33 N21 - Distance Angles C22 1.3384 (0.0059) C26 1.3493 (0.0055) 117.49 (0.44) N21 - C22 N27 - Distance Angles C26 1.3820 (0.0056) C32 1.4686 (0.0058) 116.61 (0.37) C28 1.4860 (0.0051) 118.10 (0.37) 113.29 (0.38) N27 - C26 C32 N30 - Distance Angles C31 1.4678 (0.0051) C29 1.4786 (0.0059) 110.50 (0.37) S2 1.6396 (0.0039) 116.70 (0.31) 116.94 (0.29) N30 - C31 C29 O39 - Distance Angles S2 1.4376 (0.0031) O39 - O40 - Distance Angles S2 1.4373 (0.0035) O40 - S2 - Distance Angles O40 1.4373 (0.0035) O39 1.4376 (0.0031) 120.29 (0.21) N30 1.6396 (0.0039) 106.15 (0.19) 106.54 (0.20) C33 1.7705 (0.0042) 107.65 (0.21) 108.33 (0.20) 107.21 (0.20) S2 - O40 O39 N30 FMAP and GRID set by program FMAP 2 3 27 GRID -1.042 -2 -2 1.042 2 2 R1 = 0.1290 for 3722 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.4125 0.1234 0.0073 [ 1.22 A from O19 ] Deepest hole -0.42 at 0.2325 0.1282 0.0626 [ 0.75 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 4141 / 26691 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4125 0.1234 0.0073 1.00000 0.05 0.32 1.22 O19 1.58 H14 2.14 S1 2.20 C14 Q2 1 0.7807 0.4723 0.1111 1.00000 0.05 0.31 1.88 C22 1.92 H22 1.93 H3 2.17 C23 Q3 1 1.0446 0.1802 0.3144 1.00000 0.05 0.30 1.59 H31A 1.63 C4 1.76 C3 2.02 C5 Q4 1 1.2839 0.1814 0.3214 1.00000 0.05 0.29 1.31 H31A 2.08 H12A 2.12 C31 2.18 H4 Q5 1 0.7720 0.1824 0.4176 1.00000 0.05 0.29 1.06 H2 1.75 C2 2.30 H34 2.35 H38 Q6 1 0.2425 0.1555 0.2096 1.00000 0.05 0.29 0.42 H11A 1.39 C11 2.01 H11B 2.21 H5 Q7 1 1.1863 0.2408 0.5304 1.00000 0.05 0.28 0.68 H34 1.28 C34 2.04 C35 2.18 H35 Q8 1 1.1593 0.1846 0.3331 1.00000 0.05 0.27 1.10 H31A 1.97 C4 1.99 C3 2.07 C31 Q9 1 0.2863 0.3797 0.1352 1.00000 0.05 0.27 1.59 C17 1.83 H17 1.84 C18 2.03 H23 Q10 1 0.0812 0.4376 0.1177 1.00000 0.05 0.27 0.55 H17 1.47 C17 2.41 C18 2.50 C3 Shortest distances between peaks (including symmetry equivalents) 3 8 1.03 4 8 1.05 5 7 1.82 9 10 1.94 3 4 1.96 2 10 2.51 4 6 2.61 3 6 2.92 6 8 2.94 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.22: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 4.31: Structure factors and derivatives 5.91: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.47: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.06: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src1281 finished at 16:24:44 Total CPU time: 12.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++