+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src1285 started at 17:12:26 on 13-Jan-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src1285 in P2(1) CELL 0.71073 6.2780 7.5736 13.9057 90.000 101.879 90.000 ZERR 2.00 0.0003 0.0002 0.0007 0.000 0.002 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O S UNIT 28 30 6 2 2 V = 647.02 F(000) = 288.0 Mu = 0.25 mm-1 Cell Wt = 546.70 Rho = 1.403 MERG 2 OMIT -3.00 55.00 OMIT 0 0 2 SHEL 7 0.77 FMAP 2 PLAN 20 SIZE 0.06 0.22 0.25 ACTA BOND $H WGHT 0.04900 0.06790 L.S. 4 TEMP -153.00 FVAR 1.41048 MOLE 1 C2 1 1.170009 0.731647 0.729180 11.00000 0.02773 0.02661 = 0.03002 -0.00241 0.00573 -0.00081 AFIX 43 H2 2 1.317174 0.769143 0.747645 11.00000 -1.20000 AFIX 0 C3 1 1.076799 0.655896 0.800255 11.00000 0.03461 0.03240 = 0.02938 0.00434 0.00614 0.00579 AFIX 43 H3 2 1.157026 0.638809 0.865368 11.00000 -1.20000 AFIX 0 C4 1 0.859790 0.605296 0.772720 11.00000 0.03841 0.03464 = 0.03168 0.00875 0.01507 0.00112 AFIX 43 H4 2 0.787598 0.554799 0.819803 11.00000 -1.20000 AFIX 0 C5 1 0.750303 0.628326 0.677699 11.00000 0.03009 0.02648 = 0.03195 -0.00022 0.01234 -0.00325 AFIX 43 H5 2 0.602766 0.592225 0.658334 11.00000 -1.20000 AFIX 0 C6 1 0.857889 0.705902 0.608856 11.00000 0.02625 0.02164 = 0.02522 -0.00759 0.00973 -0.00450 C8 1 0.535431 0.683391 0.468956 11.00000 0.02321 0.03329 = 0.02598 -0.00289 0.01047 -0.00708 AFIX 23 H8A 2 0.447415 0.790336 0.447977 11.00000 -1.20000 H8B 2 0.470062 0.620466 0.518198 11.00000 -1.20000 AFIX 0 C9 1 0.533644 0.565340 0.381577 11.00000 0.02176 0.02558 = 0.02425 0.00088 0.00718 -0.00643 AFIX 23 H9A 2 0.610076 0.453549 0.403553 11.00000 -1.20000 H9B 2 0.381548 0.536631 0.349871 11.00000 -1.20000 AFIX 0 C11 1 0.862525 0.712799 0.352072 11.00000 0.01687 0.02578 = 0.02055 0.00421 0.00131 -0.00505 AFIX 23 H11A 2 0.918180 0.783192 0.302526 11.00000 -1.20000 H11B 2 0.958831 0.609125 0.369384 11.00000 -1.20000 AFIX 0 C12 1 0.865785 0.823396 0.442493 11.00000 0.03131 0.03543 = 0.01980 -0.00303 0.00610 -0.01597 AFIX 23 H12A 2 1.018538 0.848909 0.474607 11.00000 -1.20000 H12B 2 0.792097 0.937298 0.422985 11.00000 -1.20000 AFIX 0 C13 1 0.525659 0.679138 0.217827 11.00000 0.01588 0.02691 = 0.02231 -0.00160 0.00410 0.00080 C14 1 0.640395 0.735864 0.139820 11.00000 0.01738 0.02461 = 0.01903 -0.00168 -0.00041 -0.00245 C15 1 0.840731 0.691274 0.123573 11.00000 0.01667 0.02968 = 0.02623 -0.00093 0.00237 -0.00018 AFIX 43 H15 2 0.942044 0.619482 0.166676 11.00000 -1.20000 AFIX 0 C16 1 0.880553 0.764810 0.034470 11.00000 0.02068 0.03496 = 0.02382 -0.00353 0.00742 -0.00238 AFIX 43 H16 2 1.011278 0.746650 0.011492 11.00000 -1.20000 AFIX 0 C17 1 0.711735 0.863453 -0.013935 11.00000 0.02755 0.03336 = 0.02174 0.00095 0.00690 -0.00353 AFIX 43 H17 2 0.711619 0.924282 -0.073692 11.00000 -1.20000 AFIX 0 N1 3 1.067579 0.756427 0.635344 11.00000 0.02865 0.03222 = 0.02449 -0.00270 0.00844 -0.00499 N7 3 0.757258 0.733918 0.512553 11.00000 0.03445 0.06476 = 0.01924 -0.00324 0.00845 -0.02962 N10 3 0.641097 0.653350 0.310685 11.00000 0.01488 0.03350 = 0.01886 0.00127 0.00185 -0.00683 O18 4 0.327291 0.651528 0.195936 11.00000 0.01448 0.04572 = 0.02752 -0.00106 0.00277 -0.00127 S1 5 0.498915 0.864959 0.045791 11.00000 0.02123 0.03170 = 0.02393 0.00219 0.00175 0.00289 HKLF 4 Covalent radii and connectivity table for 2008src1285 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C2 - N1 C3 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 - O18 N10 C14 C14 - C15 C13 S1 C15 - C14 C16 C16 - C17 C15 C17 - C16 S1 N1 - C2 C6 N7 - C6 C8 C12 N10 - C13 C11 C9 O18 - C13 S1 - C17 C14 Floating origin restraints generated 8665 Reflections read, of which 20 rejected -8 =< h =< 8, -9 =< k =< 9, -16 =< l =< 18, Max. 2-theta = 54.93 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) -7 0 6 6.79 2.79 4 14.17 1 Inconsistent equivalents 2932 Unique reflections, of which 0 suppressed R(int) = 0.0590 R(sigma) = 0.0746 Friedel opposites not merged Maximum memory for data reduction = 1831 / 29079 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 = 2318 / 215023 wR2 = 0.1111 before cycle 1 for 2932 data and 172 / 172 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0490 * P )^2 + 0.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.41063 0.00297 0.050 OSF Mean shift/su = 0.018 Maximum = 0.072 for U22 S1 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C17 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2318 / 215023 wR2 = 0.1111 before cycle 2 for 2932 data and 172 / 172 parameters GooF = S = 1.031; Restrained GooF = 1.030 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0490 * P )^2 + 0.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.41074 0.00297 0.038 OSF Mean shift/su = 0.006 Maximum = 0.038 for OSF Max. shift = 0.000 A for C9 Max. dU = 0.000 for C17 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2318 / 215023 wR2 = 0.1111 before cycle 3 for 2932 data and 172 / 172 parameters GooF = S = 1.031; Restrained GooF = 1.030 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0490 * P )^2 + 0.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.41074 0.00297 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for U13 C17 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C16 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2318 / 215023 wR2 = 0.1111 before cycle 4 for 2932 data and 172 / 172 parameters GooF = S = 1.031; Restrained GooF = 1.030 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0490 * P )^2 + 0.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.41074 0.00297 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y C13 Max. shift = 0.000 A for C13 Max. dU = 0.000 for N7 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 1.3171 0.7692 0.7477 43 0.950 0.000 C2 N1 C3 H3 1.1570 0.6388 0.8654 43 0.950 0.000 C3 C2 C4 H4 0.7876 0.5548 0.8198 43 0.950 0.000 C4 C5 C3 H5 0.6028 0.5922 0.6583 43 0.950 0.000 C5 C4 C6 H8A 0.4475 0.7904 0.4480 23 0.990 0.000 C8 N7 C9 H8B 0.4701 0.6205 0.5182 23 0.990 0.000 C8 N7 C9 H9A 0.6101 0.4535 0.4036 23 0.990 0.000 C9 N10 C8 H9B 0.3815 0.5366 0.3499 23 0.990 0.000 C9 N10 C8 H11A 0.9182 0.7832 0.3025 23 0.990 0.000 C11 N10 C12 H11B 0.9588 0.6091 0.3694 23 0.990 0.000 C11 N10 C12 H12A 1.0185 0.8489 0.4746 23 0.990 0.000 C12 N7 C11 H12B 0.7921 0.9373 0.4230 23 0.990 0.000 C12 N7 C11 H15 0.9420 0.6195 0.1667 43 0.950 0.000 C15 C14 C16 H16 1.0113 0.7467 0.0115 43 0.950 0.000 C16 C17 C15 H17 0.7116 0.9243 -0.0737 43 0.950 0.000 C17 C16 S1 2008src1285 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 1.16998 0.73166 0.72918 1.00000 0.02776 0.02659 0.03003 -0.00241 0.00574 -0.00082 0.02816 0.00555 0.00047 0.00036 0.00021 0.00000 0.00145 0.00150 0.00164 0.00117 0.00128 0.00120 0.00064 H2 1.31714 0.76919 0.74765 1.00000 0.03379 0.00000 0.00000 C3 1.07678 0.65588 0.80025 1.00000 0.03463 0.03247 0.02933 0.00431 0.00610 0.00581 0.03221 0.00612 0.00050 0.00039 0.00023 0.00000 0.00164 0.00160 0.00168 0.00131 0.00136 0.00131 0.00068 H3 1.15701 0.63878 0.86536 1.00000 0.03866 0.00000 0.00000 C4 0.85979 0.60528 0.77272 1.00000 0.03846 0.03464 0.03167 0.00875 0.01506 0.00112 0.03380 0.00621 0.00052 0.00039 0.00023 0.00000 0.00180 0.00166 0.00178 0.00130 0.00148 0.00136 0.00073 H4 0.78760 0.55478 0.81980 1.00000 0.04056 0.00000 0.00000 C5 0.75031 0.62832 0.67769 1.00000 0.03014 0.02644 0.03200 -0.00015 0.01237 -0.00322 0.02867 0.00577 0.00049 0.00036 0.00022 0.00000 0.00155 0.00154 0.00172 0.00122 0.00134 0.00119 0.00066 H5 0.60276 0.59224 0.65833 1.00000 0.03441 0.00000 0.00000 C6 0.85790 0.70589 0.60885 1.00000 0.02628 0.02166 0.02527 -0.00762 0.00980 -0.00452 0.02376 0.00498 0.00044 0.00034 0.00020 0.00000 0.00143 0.00140 0.00152 0.00108 0.00119 0.00108 0.00060 C8 0.53545 0.68340 0.46895 1.00000 0.02326 0.03340 0.02595 -0.00285 0.01050 -0.00711 0.02676 0.00521 0.00044 0.00039 0.00020 0.00000 0.00140 0.00155 0.00157 0.00123 0.00121 0.00121 0.00063 H8A 0.44745 0.79035 0.44796 1.00000 0.03211 0.00000 0.00000 H8B 0.47005 0.62050 0.51819 1.00000 0.03211 0.00000 0.00000 C9 0.53364 0.56533 0.38159 1.00000 0.02172 0.02564 0.02430 0.00091 0.00718 -0.00644 0.02354 0.00531 0.00045 0.00036 0.00021 0.00000 0.00138 0.00147 0.00153 0.00107 0.00115 0.00110 0.00060 H9A 0.61008 0.45355 0.40357 1.00000 0.02824 0.00000 0.00000 H9B 0.38154 0.53662 0.34989 1.00000 0.02824 0.00000 0.00000 C11 0.86252 0.71282 0.35208 1.00000 0.01688 0.02574 0.02061 0.00425 0.00130 -0.00507 0.02144 0.00492 0.00041 0.00035 0.00019 0.00000 0.00124 0.00145 0.00137 0.00105 0.00106 0.00102 0.00057 H11A 0.91817 0.78322 0.30253 1.00000 0.02573 0.00000 0.00000 H11B 0.95883 0.60915 0.36939 1.00000 0.02573 0.00000 0.00000 C12 0.86578 0.82340 0.44248 1.00000 0.03131 0.03544 0.01983 -0.00297 0.00610 -0.01592 0.02874 0.00506 0.00047 0.00037 0.00019 0.00000 0.00149 0.00174 0.00142 0.00110 0.00117 0.00122 0.00068 H12A 1.01853 0.84891 0.47460 1.00000 0.03449 0.00000 0.00000 H12B 0.79209 0.93730 0.42298 1.00000 0.03449 0.00000 0.00000 C13 0.52565 0.67913 0.21783 1.00000 0.01590 0.02687 0.02239 -0.00159 0.00408 0.00080 0.02170 0.00497 0.00040 0.00035 0.00019 0.00000 0.00129 0.00137 0.00146 0.00111 0.00109 0.00109 0.00056 C14 0.64040 0.73585 0.13982 1.00000 0.01745 0.02462 0.01902 -0.00170 -0.00040 -0.00246 0.02096 0.00474 0.00041 0.00034 0.00019 0.00000 0.00125 0.00140 0.00133 0.00104 0.00106 0.00104 0.00056 C15 0.84072 0.69127 0.12357 1.00000 0.01665 0.02963 0.02631 -0.00092 0.00237 -0.00018 0.02449 0.00511 0.00042 0.00038 0.00020 0.00000 0.00126 0.00145 0.00152 0.00116 0.00112 0.00108 0.00059 H15 0.94203 0.61947 0.16667 1.00000 0.02939 0.00000 0.00000 C16 0.88053 0.76483 0.03447 1.00000 0.02066 0.03502 0.02382 -0.00354 0.00742 -0.00237 0.02609 0.00519 0.00044 0.00039 0.00020 0.00000 0.00132 0.00153 0.00145 0.00127 0.00113 0.00121 0.00060 H16 1.01127 0.74668 0.01149 1.00000 0.03131 0.00000 0.00000 C17 0.71173 0.86346 -0.01394 1.00000 0.02758 0.03344 0.02177 0.00097 0.00690 -0.00356 0.02733 0.00512 0.00040 0.00044 0.00018 0.00000 0.00134 0.00140 0.00131 0.00146 0.00109 0.00147 0.00056 H17 0.71161 0.92428 -0.07369 1.00000 0.03280 0.00000 0.00000 N1 1.06760 0.75643 0.63535 1.00000 0.02866 0.03226 0.02450 -0.00270 0.00843 -0.00495 0.02805 0.00445 0.00037 0.00032 0.00017 0.00000 0.00127 0.00131 0.00128 0.00103 0.00106 0.00108 0.00054 N7 0.75724 0.73390 0.51255 1.00000 0.03444 0.06466 0.01931 -0.00325 0.00846 -0.02958 0.03905 0.00454 0.00042 0.00039 0.00017 0.00000 0.00138 0.00192 0.00127 0.00120 0.00109 0.00136 0.00070 N10 0.64110 0.65336 0.31068 1.00000 0.01491 0.03354 0.01886 0.00127 0.00186 -0.00681 0.02267 0.00410 0.00034 0.00030 0.00016 0.00000 0.00108 0.00128 0.00122 0.00097 0.00092 0.00093 0.00051 O18 0.32730 0.65153 0.19594 1.00000 0.01451 0.04571 0.02759 -0.00104 0.00278 -0.00124 0.02949 0.00366 0.00029 0.00027 0.00014 0.00000 0.00095 0.00125 0.00111 0.00090 0.00082 0.00082 0.00048 S1 0.49892 0.86496 0.04579 1.00000 0.02126 0.03173 0.02395 0.00219 0.00174 0.00289 0.02606 0.00127 0.00010 0.00010 0.00005 0.00000 0.00031 0.00035 0.00033 0.00031 0.00024 0.00030 0.00018 Final Structure Factor Calculation for 2008src1285 in P2(1) Total number of l.s. parameters = 172 Maximum vector length = 511 Memory required = 2148 / 26068 wR2 = 0.1111 before cycle 5 for 2932 data and 2 / 172 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0490 * P )^2 + 0.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0474 for 2380 Fo > 4sig(Fo) and 0.0664 for all 2932 data wR2 = 0.1111, GooF = S = 1.030, Restrained GooF = 1.030 for all data Flack x parameter = -0.1406 with su 0.0959 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 = 19.00 for non-hydrogen and 15.00 for hydrogen atoms Principal mean square atomic displacements U 0.0313 0.0279 0.0253 C2 0.0396 0.0317 0.0253 C3 0.0453 0.0356 0.0205 C4 0.0365 0.0276 0.0219 C5 0.0344 0.0213 0.0156 C6 0.0382 0.0257 0.0164 C8 0.0304 0.0249 0.0153 C9 0.0315 0.0182 0.0146 C11 0.0494 0.0195 0.0173 C12 0.0275 0.0219 0.0157 C13 0.0254 0.0235 0.0140 C14 0.0299 0.0270 0.0165 C15 0.0364 0.0237 0.0182 C16 0.0352 0.0265 0.0203 C17 0.0364 0.0256 0.0222 N1 0.0828 0.0200 0.0143 N7 0.0363 0.0190 0.0127 N10 0.0458 0.0282 0.0145 O18 0.0326 0.0266 0.0190 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.034 0.051 0.068 0.081 0.098 0.116 0.142 0.175 0.240 1.000 Number in group 296. 308. 284. 287. 295. 293. 291. 291. 293. 294. GooF 0.874 0.988 1.069 1.113 1.122 1.091 1.002 1.014 1.019 0.995 K 0.887 0.885 0.928 0.968 0.982 0.976 1.019 1.024 1.026 0.989 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.33 1.66 inf Number in group 303. 294. 285. 297. 286. 301. 288. 298. 286. 294. GooF 0.968 1.007 1.087 1.038 1.019 1.061 1.083 0.949 0.950 1.127 K 0.973 0.942 1.017 1.007 1.020 1.006 1.040 1.026 1.017 0.972 R1 0.169 0.177 0.127 0.092 0.077 0.053 0.047 0.031 0.029 0.029 Recommended weighting scheme: WGHT 0.0492 0.0672 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) 0 -1 1 316.10 443.53 4.18 0.292 6.62 1 8 7 11.33 29.27 3.99 0.075 0.83 2 0 12 10.55 28.45 3.78 0.074 1.00 -3 9 1 18.90 45.58 3.31 0.094 0.78 -3 3 10 24.57 38.44 3.25 0.086 1.13 -5 3 13 32.23 54.52 3.23 0.102 0.84 5 -2 5 22.01 36.15 3.15 0.083 1.00 -3 -9 1 15.37 45.24 3.14 0.093 0.78 4 0 3 18.02 28.56 3.14 0.074 1.37 -3 3 15 37.90 68.70 3.11 0.115 0.85 2 2 2 226.58 184.21 3.09 0.188 2.15 -2 -8 6 69.61 99.42 3.08 0.138 0.86 -7 0 12 234.22 166.84 3.03 0.179 0.78 3 -3 5 122.91 153.33 2.99 0.172 1.29 2 0 0 134.28 163.58 2.99 0.177 3.07 -2 3 5 69.49 55.20 2.99 0.103 1.69 3 -1 11 -1.98 11.41 2.87 0.047 0.97 -6 -4 4 2.60 13.46 2.85 0.051 0.91 -2 -8 4 23.49 43.86 2.85 0.092 0.89 -5 2 6 297.33 247.15 2.80 0.218 1.13 2 -2 2 217.25 181.66 2.80 0.187 2.15 -5 0 4 94.59 74.56 2.80 0.120 1.24 -1 -1 6 59.20 72.97 2.79 0.118 2.19 -4 -2 10 28.06 41.17 2.77 0.089 1.09 -7 0 8 234.40 179.50 2.75 0.186 0.85 6 -2 5 15.58 35.61 2.74 0.083 0.87 -2 2 6 255.37 216.18 2.74 0.204 1.79 0 9 4 16.73 24.92 2.70 0.069 0.82 -4 1 11 11.03 2.19 2.68 0.021 1.07 -4 3 10 63.75 85.76 2.67 0.128 1.04 6 1 0 98.05 123.65 2.63 0.154 1.01 -7 0 2 8.84 19.30 2.62 0.061 0.89 0 8 8 28.58 45.82 2.61 0.094 0.83 3 -2 11 49.31 24.95 2.61 0.069 0.94 -3 -2 6 56.04 45.19 2.61 0.093 1.55 -1 -1 16 33.59 58.51 2.61 0.106 0.86 -7 2 8 5.55 21.14 2.57 0.064 0.83 -3 -4 10 126.86 104.88 2.57 0.142 1.05 -3 -4 11 173.95 137.28 2.53 0.163 1.00 -1 -8 5 -0.12 8.29 2.52 0.040 0.89 -2 -1 16 17.37 30.41 2.51 0.077 0.86 -8 0 3 28.32 54.75 2.49 0.103 0.78 -7 -2 9 78.69 110.19 2.49 0.146 0.82 1 -1 0 2971.89 3434.18 2.49 0.813 4.77 -1 0 2 367.78 424.04 2.48 0.286 5.11 4 -1 1 124.98 102.28 2.48 0.140 1.46 0 3 11 32.10 43.62 2.48 0.092 1.11 5 1 7 50.26 67.28 2.47 0.114 0.95 -1 1 14 145.56 115.06 2.47 0.149 0.98 -1 6 4 125.37 105.91 2.45 0.143 1.18 Bond lengths and angles C2 - Distance Angles N1 1.3437 (0.0037) C3 1.3735 (0.0041) 124.58 (0.28) H2 0.9500 117.71 117.71 C2 - N1 C3 C3 - Distance Angles C2 1.3735 (0.0041) C4 1.3908 (0.0045) 117.08 (0.29) H3 0.9500 121.46 121.46 C3 - C2 C4 C4 - Distance Angles C5 1.3693 (0.0044) C3 1.3908 (0.0045) 119.94 (0.27) H4 0.9500 120.03 120.03 C4 - C5 C3 C5 - Distance Angles C4 1.3693 (0.0044) C6 1.4086 (0.0037) 119.56 (0.27) H5 0.9500 120.22 120.22 C5 - C4 C6 C6 - Distance Angles N1 1.3475 (0.0034) N7 1.3744 (0.0036) 116.74 (0.22) C5 1.4086 (0.0037) 120.71 (0.26) 122.54 (0.25) C6 - N1 N7 C8 - Distance Angles N7 1.4509 (0.0036) C9 1.5066 (0.0039) 109.92 (0.23) H8A 0.9900 109.68 109.68 H8B 0.9900 109.68 109.68 108.18 C8 - N7 C9 H8A C9 - Distance Angles N10 1.4648 (0.0032) C8 1.5066 (0.0040) 110.15 (0.21) H9A 0.9900 109.63 109.63 H9B 0.9900 109.63 109.63 108.15 C9 - N10 C8 H9A C11 - Distance Angles N10 1.4618 (0.0032) C12 1.5072 (0.0038) 110.37 (0.21) H11A 0.9900 109.58 109.58 H11B 0.9900 109.58 109.58 108.12 C11 - N10 C12 H11A C12 - Distance Angles N7 1.4650 (0.0033) C11 1.5072 (0.0038) 111.68 (0.21) H12A 0.9900 109.29 109.29 H12B 0.9900 109.29 109.29 107.95 C12 - N7 C11 H12A C13 - Distance Angles O18 1.2373 (0.0031) N10 1.3584 (0.0034) 121.51 (0.23) C14 1.4840 (0.0035) 118.98 (0.24) 119.48 (0.21) C13 - O18 N10 C14 - Distance Angles C15 1.3651 (0.0036) C13 1.4840 (0.0035) 130.67 (0.25) S1 1.7253 (0.0027) 111.28 (0.19) 117.80 (0.19) C14 - C15 C13 C15 - Distance Angles C14 1.3651 (0.0036) C16 1.4268 (0.0038) 112.28 (0.25) H15 0.9500 123.86 123.86 C15 - C14 C16 C16 - Distance Angles C17 1.3566 (0.0040) C15 1.4268 (0.0038) 112.78 (0.23) H16 0.9500 123.61 123.61 C16 - C17 C15 C17 - Distance Angles C16 1.3566 (0.0040) S1 1.7122 (0.0024) 111.77 (0.20) H17 0.9500 124.12 124.12 C17 - C16 S1 N1 - Distance Angles C2 1.3437 (0.0037) C6 1.3475 (0.0035) 118.10 (0.23) N1 - C2 N7 - Distance Angles C6 1.3744 (0.0036) C8 1.4509 (0.0036) 125.14 (0.21) C12 1.4650 (0.0033) 122.40 (0.23) 112.45 (0.23) N7 - C6 C8 N10 - Distance Angles C13 1.3584 (0.0034) C11 1.4618 (0.0033) 127.45 (0.21) C9 1.4648 (0.0032) 118.40 (0.21) 114.05 (0.21) N10 - C13 C11 O18 - Distance Angles C13 1.2373 (0.0031) O18 - S1 - Distance Angles C17 1.7122 (0.0024) C14 1.7253 (0.0027) 91.86 (0.13) S1 - C17 FMAP and GRID set by program FMAP 2 1 17 GRID -3.571 -2 -2 3.571 2 2 R1 = 0.0555 for 1590 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.22 at 0.2431 0.7537 0.2601 [ 1.37 A from O18 ] Deepest hole -0.32 at 0.4622 0.9066 0.9863 [ 0.87 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2214 / 17981 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2431 0.7537 0.2601 1.00000 0.05 0.22 1.37 O18 2.06 C13 2.14 H9B 2.25 H11A Q2 1 0.9790 0.6936 0.2198 1.00000 0.05 0.21 0.92 H15 1.44 C15 1.45 H11A 2.12 C11 Q3 1 0.9511 0.8637 -0.1156 1.00000 0.05 0.20 1.78 H17 1.94 H16 2.19 H3 2.20 C3 Q4 1 1.2481 0.6913 0.9096 1.00000 0.05 0.20 0.85 H3 1.69 C3 2.29 H16 2.45 H2 Q5 1 0.8102 0.8651 0.1614 1.00000 0.05 0.20 1.43 C14 1.44 C15 2.03 H15 2.04 H11A Q6 1 1.3296 0.5068 0.7788 1.00000 0.05 0.20 2.02 C3 2.02 C2 2.03 H2 2.04 H3 Q7 1 1.3226 0.6417 0.9750 1.00000 0.05 0.20 1.66 H3 2.15 S1 2.18 H17 2.20 C17 Q8 1 1.2210 0.8480 0.9232 1.00000 0.05 0.20 1.78 H3 2.12 H16 2.18 S1 2.28 C3 Q9 1 0.4671 0.5575 0.5243 1.00000 0.05 0.19 0.49 H8B 1.35 C8 1.90 H5 2.05 H8A Q10 1 0.3595 0.8764 0.4430 1.00000 0.05 0.19 0.85 H8A 1.82 C8 2.15 H8B 2.18 H9A Q11 1 1.3165 0.8036 0.8607 1.00000 0.05 0.19 1.59 H2 1.61 H3 1.92 C3 1.95 C2 Q12 1 0.6509 0.8652 0.5588 1.00000 0.05 0.19 1.42 N7 1.80 C6 1.86 H9B 1.88 H8A Q13 1 1.3103 0.7300 0.6801 1.00000 0.05 0.19 0.98 H2 1.22 C2 1.54 N1 2.17 H9A Q14 1 0.7065 1.0586 -0.0382 1.00000 0.05 0.18 1.13 H17 1.51 C17 2.24 H16 2.27 O18 Q15 1 1.1336 0.8489 0.5890 1.00000 0.05 0.18 1.09 N1 1.61 H12A 1.78 H9A 2.11 C6 Q16 1 0.2826 0.6391 0.5222 1.00000 0.05 0.18 1.20 H8B 1.81 H12B 1.91 C8 1.97 H8A Q17 1 1.3195 0.8540 0.7263 1.00000 0.05 0.18 0.71 H2 1.33 C2 1.96 N1 2.09 H9A Q18 1 0.6366 0.6426 0.8876 1.00000 0.05 0.18 1.61 H4 2.15 C17 2.23 H17 2.35 C4 Q19 1 0.1472 0.5068 0.3425 1.00000 0.05 0.18 1.47 H9B 1.52 H11B 2.38 C6 2.38 N1 Q20 1 1.2502 0.7873 0.4964 1.00000 0.05 0.18 1.50 H12A 1.53 H8A 1.85 H8B 1.95 H9A Shortest distances between peaks (including symmetry equivalents) 4 7 1.01 7 14 1.13 13 17 1.13 16 20 1.18 8 11 1.20 4 8 1.22 4 11 1.22 10 20 1.30 9 16 1.31 3 8 1.67 15 20 1.67 1 2 1.70 5 6 1.71 13 15 1.75 9 10 1.75 2 5 1.76 7 8 1.78 9 12 1.91 11 17 1.91 12 19 1.98 7 11 2.00 4 14 2.02 15 17 2.02 15 16 2.15 6 13 2.17 10 12 2.18 9 20 2.19 10 16 2.21 3 4 2.24 13 16 2.27 2 19 2.30 11 18 2.31 1 19 2.33 6 18 2.42 3 11 2.43 4 6 2.43 12 16 2.44 15 19 2.48 7 18 2.52 3 14 2.52 6 11 2.53 13 20 2.54 4 18 2.55 12 20 2.56 11 13 2.56 3 18 2.60 9 12 2.60 4 5 2.66 1 10 2.66 16 19 2.66 9 10 2.69 8 14 2.70 10 15 2.71 6 17 2.73 9 20 2.76 5 7 2.83 12 16 2.84 9 13 2.87 1 5 2.91 9 19 2.91 6 7 2.92 8 17 2.93 3 7 2.94 4 17 2.95 10 16 2.97 2 3 2.97 12 15 2.97 19 20 2.99 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. 0.39: 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 0.02: Generate idealized H-atoms 0.52: Structure factors and derivatives 0.61: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.08: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src1285 finished at 17:12:28 Total CPU time: 1.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++