+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 17:25:56 on 02-Dec-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02src643 in P2(1)2(1)2(1) CELL 0.71073 7.8264 13.1709 20.7532 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0006 0.0011 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 UNIT 100 124 4 12 V = 2139.26 F(000) = 848.0 Mu = 0.08 mm-1 Cell Wt = 1574.03 Rho = 1.222 MERG 4 OMIT -3.00 55.00 OMIT -1 13 3 EXTI 0.00356 FMAP 2 PLAN 10 SIZE 0.08 0.12 0.60 ACTA BOND $H WGHT 0.04160 0.08360 L.S. 4 TEMP -153.00 FVAR 0.40910 C1 1 0.090316 1.125977 0.353339 11.00000 0.02912 0.03476 = 0.02641 -0.00297 0.00420 -0.00075 AFIX 137 H1A 2 0.164362 1.146074 0.389220 11.00000 -1.50000 H1B 2 0.027198 1.064415 0.365035 11.00000 -1.50000 H1C 2 0.009423 1.180829 0.343990 11.00000 -1.50000 AFIX 0 C2 1 0.198154 1.105344 0.294417 11.00000 0.01817 0.02621 = 0.02201 -0.00459 -0.00006 -0.00150 C3 1 0.258041 1.008409 0.281602 11.00000 0.02325 0.02690 = 0.02462 0.00228 0.00196 -0.00510 AFIX 43 H3 2 0.224749 0.953808 0.308750 11.00000 -1.20000 AFIX 0 C4 1 0.365662 0.989651 0.229882 11.00000 0.02366 0.02273 = 0.02792 -0.00326 0.00042 -0.00248 AFIX 43 H4 2 0.403338 0.922218 0.222003 11.00000 -1.20000 AFIX 0 C5 1 0.419699 1.067211 0.189299 11.00000 0.01662 0.02633 = 0.02214 -0.00204 -0.00080 -0.00025 C6 1 0.353517 1.163442 0.200119 11.00000 0.01943 0.02572 = 0.02665 0.00598 -0.00001 -0.00235 AFIX 43 H6 2 0.382232 1.217401 0.171738 11.00000 -1.20000 AFIX 0 C7 1 0.245176 1.181810 0.252271 11.00000 0.02012 0.02392 = 0.03163 -0.00208 -0.00107 0.00194 AFIX 43 H7 2 0.202636 1.248527 0.258999 11.00000 -1.20000 AFIX 0 C8 1 0.548762 1.042243 0.135567 11.00000 0.02064 0.02086 = 0.02266 0.00150 0.00160 -0.00150 AFIX 13 H8 2 0.556725 0.966493 0.134274 11.00000 -1.20000 AFIX 0 C9 1 0.848555 1.010871 0.174284 11.00000 0.02202 0.02375 = 0.03123 0.00177 -0.00012 0.00153 AFIX 13 H9 2 0.954750 1.051729 0.181039 11.00000 -1.20000 AFIX 0 C10 1 0.897840 0.923222 0.130252 11.00000 0.02597 0.03154 = 0.03543 -0.00085 0.00160 0.00853 AFIX 137 H10A 2 0.799810 0.877694 0.124933 11.00000 -1.50000 H10B 2 0.993297 0.885641 0.149360 11.00000 -1.50000 H10C 2 0.932147 0.949897 0.088110 11.00000 -1.50000 AFIX 0 C11 1 0.796210 0.970641 0.240786 11.00000 0.03091 0.02608 = 0.02897 0.00459 -0.00252 0.00278 AFIX 137 H11A 2 0.760983 1.027502 0.268193 11.00000 -1.50000 H11B 2 0.893397 0.935682 0.260643 11.00000 -1.50000 H11C 2 0.700809 0.923039 0.236004 11.00000 -1.50000 AFIX 0 C12 1 0.752512 1.188392 0.152493 11.00000 0.02364 0.02081 = 0.03001 0.00277 0.00268 -0.00204 AFIX 13 H12 2 0.649976 1.224364 0.135017 11.00000 -1.20000 AFIX 0 C13 1 0.771152 1.220424 0.223302 11.00000 0.02999 0.02349 = 0.03117 0.00102 0.00076 -0.00145 AFIX 137 H13A 2 0.670337 1.198341 0.247550 11.00000 -1.50000 H13B 2 0.781414 1.294469 0.225877 11.00000 -1.50000 H13C 2 0.873599 1.188902 0.241661 11.00000 -1.50000 AFIX 0 C14 1 0.907168 1.225258 0.113694 11.00000 0.02698 0.02962 = 0.03040 0.00341 0.00206 -0.00685 AFIX 137 H14A 2 1.010993 1.192717 0.130135 11.00000 -1.50000 H14B 2 0.917653 1.299102 0.117936 11.00000 -1.50000 H14C 2 0.891744 1.207528 0.068203 11.00000 -1.50000 AFIX 0 C15 1 0.477998 1.074521 0.069270 11.00000 0.01936 0.02072 = 0.02815 0.00137 0.00051 -0.00038 AFIX 13 H15 2 0.466692 1.150115 0.067857 11.00000 -1.20000 AFIX 0 C16 1 0.597290 1.040072 0.016330 11.00000 0.02061 0.02287 = 0.02087 0.00110 -0.00356 0.00032 C17 1 0.686138 1.100112 -0.023330 11.00000 0.02317 0.02249 = 0.02417 0.00328 -0.00328 0.00019 AFIX 43 H17 2 0.667843 1.171370 -0.021694 11.00000 -1.20000 AFIX 0 C19 1 0.809884 1.059843 -0.068893 11.00000 0.02256 0.03023 = 0.02057 0.00605 -0.00292 -0.00247 C20 1 0.817701 0.948026 -0.069880 11.00000 0.01790 0.03330 = 0.01800 0.00469 -0.00268 0.00019 C21 1 0.923430 0.894601 -0.112602 11.00000 0.02117 0.03900 = 0.02116 0.00434 0.00211 0.00293 AFIX 43 H21 2 0.995983 0.931127 -0.141053 11.00000 -1.20000 AFIX 0 C22 1 0.923857 0.790601 -0.114004 11.00000 0.02713 0.04149 = 0.02127 -0.00316 -0.00026 0.01175 AFIX 43 H22 2 0.996027 0.755667 -0.143383 11.00000 -1.20000 AFIX 0 C23 1 0.818002 0.735692 -0.072166 11.00000 0.02727 0.02774 = 0.02702 -0.00106 -0.00590 0.00551 AFIX 43 H23 2 0.818277 0.663588 -0.073352 11.00000 -1.20000 AFIX 0 C24 1 0.713615 0.785925 -0.029353 11.00000 0.02250 0.02830 = 0.02350 0.00051 0.00060 -0.00128 AFIX 43 H24 2 0.642403 0.749147 -0.000553 11.00000 -1.20000 AFIX 0 C25 1 0.714321 0.891570 -0.029034 11.00000 0.01821 0.02616 = 0.01867 -0.00042 -0.00247 0.00399 C26 1 0.223488 1.063728 0.007005 11.00000 0.02386 0.04270 = 0.03183 0.00199 -0.00765 0.00212 AFIX 137 H26A 2 0.210220 1.137659 0.008833 11.00000 -1.50000 H26B 2 0.110523 1.031678 0.005854 11.00000 -1.50000 H26C 2 0.287421 1.045203 -0.031858 11.00000 -1.50000 AFIX 0 N1 3 0.724626 1.078971 0.142392 11.00000 0.01774 0.01895 = 0.02494 0.00149 0.00047 -0.00068 O1 4 0.314332 1.029667 0.062687 11.00000 0.02080 0.03340 = 0.02891 0.00254 -0.00137 -0.00289 O2 4 0.903474 1.114007 -0.102448 11.00000 0.03512 0.03824 = 0.03479 0.01275 0.00746 -0.00483 O3 4 0.605846 0.936985 0.014889 11.00000 0.02400 0.02082 = 0.02333 0.00030 0.00491 0.00020 HKLF 4 Covalent radii and connectivity table for 02src643 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C2 - C7 C3 C1 C3 - C2 C4 C4 - C3 C5 C5 - C6 C4 C8 C6 - C5 C7 C7 - C2 C6 C8 - N1 C5 C15 C9 - N1 C10 C11 C10 - C9 C11 - C9 C12 - N1 C14 C13 C13 - C12 C14 - C12 C15 - O1 C16 C8 C16 - C17 O3 C15 C17 - C16 C19 C19 - O2 C17 C20 C20 - C25 C21 C19 C21 - C22 C20 C22 - C21 C23 C23 - C24 C22 C24 - C23 C25 C25 - O3 C20 C24 C26 - O1 N1 - C8 C12 C9 O1 - C15 C26 O2 - C19 O3 - C16 C25 11833 Reflections read, of which 25 rejected -8 =< h =< 10, -17 =< k =< 13, -26 =< l =< 23, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 1 1 0 842.17 18.54 3 183.31 3 2 0 74.83 2.22 3 11.31 5 5 0 20.25 0.68 4 4.55 6 2 8 77.86 0.90 8 6.11 4 Inconsistent equivalents 2732 Unique reflections, of which 0 suppressed R(int) = 0.0486 R(sigma) = 0.0476 Friedel opposites merged Maximum memory for data reduction = 2941 / 27050 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 = 3741 / 334766 wR2 = 0.0906 before cycle 1 for 2732 data and 269 / 269 parameters GooF = S = 1.159; Restrained GooF = 1.159 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0416 * P )^2 + 0.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.40831 0.00085 -0.932 OSF 2 0.00300 0.00104 -0.537 EXTI Mean shift/su = 0.174 Maximum = -0.932 for OSF Max. shift = 0.005 A for H10C Max. dU = 0.000 for C8 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3741 / 334766 wR2 = 0.0903 before cycle 2 for 2732 data and 269 / 269 parameters GooF = S = 1.156; Restrained GooF = 1.156 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0416 * P )^2 + 0.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.40796 0.00084 -0.416 OSF 2 0.00281 0.00101 -0.187 EXTI Mean shift/su = 0.060 Maximum = -0.416 for OSF Max. shift = 0.002 A for H1A Max. dU = 0.000 for C8 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3741 / 334766 wR2 = 0.0902 before cycle 3 for 2732 data and 269 / 269 parameters GooF = S = 1.155; Restrained GooF = 1.155 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0416 * P )^2 + 0.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.40794 0.00084 -0.019 OSF 2 0.00281 0.00100 -0.005 EXTI Mean shift/su = 0.003 Maximum = 0.045 for tors H1A Max. shift = 0.001 A for H1C Max. dU = 0.000 for C13 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3741 / 334766 wR2 = 0.0902 before cycle 4 for 2732 data and 269 / 269 parameters GooF = S = 1.155; Restrained GooF = 1.155 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0416 * P )^2 + 0.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.40794 0.00084 -0.001 OSF 2 0.00281 0.00100 0.000 EXTI Mean shift/su = 0.001 Maximum = 0.018 for tors H1A Max. shift = 0.000 A for H1C Max. dU = 0.000 for N1 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 H1A 0.1643 1.1465 0.3892 137 0.980 0.000 C1 C2 H1A H1B 0.0276 1.0644 0.3652 137 0.980 0.000 C1 C2 H1A H1C 0.0091 1.1807 0.3439 137 0.980 0.000 C1 C2 H1A H3 0.2247 0.9538 0.3087 43 0.950 0.000 C3 C2 C4 H4 0.4033 0.9222 0.2220 43 0.950 0.000 C4 C3 C5 H6 0.3822 1.2174 0.1718 43 0.950 0.000 C6 C5 C7 H7 0.2026 1.2486 0.2590 43 0.950 0.000 C7 C2 C6 H8 0.5567 0.9666 0.1343 13 1.000 0.000 C8 N1 C5 C15 H9 0.9548 1.0518 0.1810 13 1.000 0.000 C9 N1 C10 C11 H10A 0.7999 0.8775 0.1252 137 0.980 0.000 C10 C9 H10A H10B 0.9937 0.8859 0.1492 137 0.980 0.000 C10 C9 H10A H10C 0.9314 0.9498 0.0880 137 0.980 0.000 C10 C9 H10A H11A 0.7610 1.0275 0.2682 137 0.980 0.000 C11 C9 H11A H11B 0.8936 0.9358 0.2607 137 0.980 0.000 C11 C9 H11A H11C 0.7010 0.9230 0.2361 137 0.980 0.000 C11 C9 H11A H12 0.6499 1.2244 0.1350 13 1.000 0.000 C12 N1 C14 C13 H13A 0.6701 1.1987 0.2476 137 0.980 0.000 C13 C12 H13A H13B 0.7821 1.2944 0.2259 137 0.980 0.000 C13 C12 H13A H13C 0.8733 1.1886 0.2418 137 0.980 0.000 C13 C12 H13A H14A 1.0110 1.1926 0.1301 137 0.980 0.000 C14 C12 H14A H14B 0.9179 1.2991 0.1181 137 0.980 0.000 C14 C12 H14A H14C 0.8917 1.2077 0.0682 137 0.980 0.000 C14 C12 H14A H15 0.4667 1.1501 0.0679 13 1.000 0.000 C15 O1 C16 C8 H17 0.6679 1.1714 -0.0217 43 0.950 0.000 C17 C16 C19 H21 0.9963 0.9312 -0.1410 43 0.950 0.000 C21 C22 C20 H22 0.9958 0.7556 -0.1435 43 0.950 0.000 C22 C21 C23 H23 0.8188 0.6636 -0.0733 43 0.950 0.000 C23 C24 C22 H24 0.6420 0.7491 -0.0006 43 0.950 0.000 C24 C23 C25 H26A 0.2105 1.1376 0.0088 137 0.980 0.000 C26 O1 H26A H26B 0.1105 1.0317 0.0059 137 0.980 0.000 C26 O1 H26A H26C 0.2875 1.0451 -0.0318 137 0.980 0.000 C26 O1 H26A 02src643 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.09033 1.12603 0.35336 1.00000 0.02906 0.03455 0.02589 -0.00278 0.00469 -0.00060 0.02983 0.00408 0.00031 0.00018 0.00010 0.00000 0.00119 0.00146 0.00121 0.00105 0.00096 0.00107 0.00055 H1A 0.16434 1.14648 0.38917 1.00000 0.04475 0.00000 0.00000 H1B 0.02764 1.06439 0.36521 1.00000 0.04475 0.00000 0.00000 H1C 0.00905 1.18065 0.34393 1.00000 0.04475 0.00000 0.00000 C2 0.19819 1.10533 0.29441 1.00000 0.01804 0.02616 0.02172 -0.00455 0.00020 -0.00152 0.02197 0.00355 0.00026 0.00017 0.00010 0.00000 0.00102 0.00121 0.00107 0.00095 0.00081 0.00094 0.00047 C3 0.25804 1.00837 0.28160 1.00000 0.02338 0.02645 0.02414 0.00259 0.00205 -0.00493 0.02466 0.00375 0.00027 0.00018 0.00010 0.00000 0.00107 0.00119 0.00105 0.00101 0.00083 0.00097 0.00048 H3 0.22472 0.95377 0.30875 1.00000 0.02959 0.00000 0.00000 C4 0.36561 0.98961 0.22991 1.00000 0.02337 0.02240 0.02746 -0.00336 0.00036 -0.00236 0.02441 0.00362 0.00025 0.00018 0.00010 0.00000 0.00109 0.00123 0.00111 0.00104 0.00085 0.00093 0.00050 H4 0.40332 0.92218 0.22204 1.00000 0.02930 0.00000 0.00000 C5 0.41966 1.06724 0.18928 1.00000 0.01715 0.02613 0.02186 -0.00199 -0.00081 -0.00098 0.02171 0.00353 0.00025 0.00017 0.00010 0.00000 0.00097 0.00127 0.00102 0.00097 0.00083 0.00093 0.00047 C6 0.35348 1.16348 0.20014 1.00000 0.01895 0.02541 0.02658 0.00607 0.00009 -0.00222 0.02365 0.00369 0.00025 0.00018 0.00010 0.00000 0.00106 0.00125 0.00113 0.00102 0.00084 0.00092 0.00049 H6 0.38221 1.21745 0.17177 1.00000 0.02838 0.00000 0.00000 C7 0.24512 1.18186 0.25230 1.00000 0.01954 0.02350 0.03134 -0.00251 -0.00097 0.00168 0.02479 0.00369 0.00026 0.00017 0.00010 0.00000 0.00104 0.00119 0.00119 0.00100 0.00087 0.00089 0.00050 H7 0.20257 1.24857 0.25905 1.00000 0.02975 0.00000 0.00000 C8 0.54874 1.04231 0.13558 1.00000 0.02043 0.01977 0.02242 0.00154 0.00177 -0.00130 0.02087 0.00364 0.00026 0.00017 0.00009 0.00000 0.00105 0.00116 0.00109 0.00093 0.00079 0.00087 0.00047 H8 0.55668 0.96656 0.13429 1.00000 0.02505 0.00000 0.00000 C9 0.84862 1.01093 0.17424 1.00000 0.02206 0.02381 0.03025 0.00170 -0.00065 0.00147 0.02537 0.00380 0.00027 0.00017 0.00010 0.00000 0.00107 0.00127 0.00119 0.00104 0.00085 0.00096 0.00050 H9 0.95483 1.05178 0.18096 1.00000 0.03045 0.00000 0.00000 C10 0.89778 0.92321 0.13023 1.00000 0.02596 0.03107 0.03502 -0.00116 0.00159 0.00854 0.03068 0.00411 0.00030 0.00018 0.00011 0.00000 0.00116 0.00139 0.00125 0.00112 0.00097 0.00107 0.00054 H10A 0.79993 0.87746 0.12517 1.00000 0.04603 0.00000 0.00000 H10B 0.99371 0.88588 0.14921 1.00000 0.04603 0.00000 0.00000 H10C 0.93135 0.94979 0.08798 1.00000 0.04603 0.00000 0.00000 C11 0.79631 0.97068 0.24082 1.00000 0.03076 0.02595 0.02852 0.00470 -0.00194 0.00272 0.02841 0.00408 0.00030 0.00017 0.00011 0.00000 0.00120 0.00125 0.00118 0.00101 0.00096 0.00098 0.00052 H11A 0.76104 1.02755 0.26821 1.00000 0.04262 0.00000 0.00000 H11B 0.89355 0.93578 0.26068 1.00000 0.04262 0.00000 0.00000 H11C 0.70096 0.92304 0.23606 1.00000 0.04262 0.00000 0.00000 C12 0.75240 1.18838 0.15249 1.00000 0.02315 0.02049 0.02974 0.00273 0.00232 -0.00217 0.02446 0.00376 0.00028 0.00016 0.00011 0.00000 0.00107 0.00116 0.00115 0.00096 0.00089 0.00093 0.00049 H12 0.64987 1.22436 0.13501 1.00000 0.02935 0.00000 0.00000 C13 0.77115 1.22042 0.22335 1.00000 0.02941 0.02351 0.03081 0.00124 0.00062 -0.00195 0.02791 0.00386 0.00030 0.00017 0.00010 0.00000 0.00126 0.00119 0.00119 0.00104 0.00095 0.00100 0.00052 H13A 0.67008 1.19867 0.24756 1.00000 0.04186 0.00000 0.00000 H13B 0.78208 1.29443 0.22591 1.00000 0.04186 0.00000 0.00000 H13C 0.87326 1.18859 0.24175 1.00000 0.04186 0.00000 0.00000 C14 0.90723 1.22527 0.11371 1.00000 0.02682 0.02967 0.02999 0.00340 0.00233 -0.00681 0.02883 0.00400 0.00029 0.00019 0.00011 0.00000 0.00116 0.00137 0.00116 0.00106 0.00095 0.00108 0.00053 H14A 1.01098 1.19256 0.13008 1.00000 0.04324 0.00000 0.00000 H14B 0.91793 1.29909 0.11807 1.00000 0.04324 0.00000 0.00000 H14C 0.89173 1.20774 0.06819 1.00000 0.04324 0.00000 0.00000 C15 0.47794 1.07451 0.06929 1.00000 0.01876 0.02016 0.02825 0.00156 0.00042 -0.00035 0.02239 0.00369 0.00025 0.00017 0.00010 0.00000 0.00104 0.00118 0.00114 0.00101 0.00084 0.00091 0.00048 H15 0.46666 1.15011 0.06786 1.00000 0.02687 0.00000 0.00000 C16 0.59734 1.04003 0.01636 1.00000 0.02040 0.02345 0.02062 0.00122 -0.00336 0.00059 0.02149 0.00357 0.00026 0.00016 0.00010 0.00000 0.00101 0.00125 0.00105 0.00093 0.00086 0.00093 0.00047 C17 0.68624 1.10014 -0.02334 1.00000 0.02323 0.02231 0.02375 0.00325 -0.00314 0.00027 0.02310 0.00361 0.00027 0.00017 0.00010 0.00000 0.00109 0.00116 0.00112 0.00097 0.00086 0.00097 0.00048 H17 0.66792 1.17139 -0.02171 1.00000 0.02772 0.00000 0.00000 C19 0.80989 1.05990 -0.06887 1.00000 0.02192 0.02991 0.02052 0.00597 -0.00289 -0.00215 0.02412 0.00375 0.00027 0.00017 0.00010 0.00000 0.00110 0.00132 0.00109 0.00100 0.00088 0.00101 0.00049 C20 0.81778 0.94799 -0.06992 1.00000 0.01752 0.03288 0.01799 0.00486 -0.00254 0.00039 0.02280 0.00367 0.00026 0.00017 0.00010 0.00000 0.00103 0.00132 0.00104 0.00096 0.00080 0.00097 0.00048 C21 0.92355 0.89463 -0.11258 1.00000 0.02171 0.03891 0.02089 0.00430 0.00207 0.00268 0.02717 0.00405 0.00028 0.00019 0.00010 0.00000 0.00113 0.00151 0.00108 0.00105 0.00089 0.00107 0.00053 H21 0.99626 0.93116 -0.14098 1.00000 0.03261 0.00000 0.00000 C22 0.92383 0.79055 -0.11403 1.00000 0.02711 0.04053 0.02115 -0.00289 -0.00012 0.01152 0.02960 0.00420 0.00029 0.00020 0.00010 0.00000 0.00120 0.00155 0.00108 0.00106 0.00092 0.00109 0.00055 H22 0.99578 0.75561 -0.14348 1.00000 0.03552 0.00000 0.00000 C23 0.81826 0.73569 -0.07217 1.00000 0.02663 0.02797 0.02691 -0.00115 -0.00570 0.00519 0.02717 0.00386 0.00029 0.00018 0.00010 0.00000 0.00121 0.00129 0.00115 0.00104 0.00095 0.00103 0.00052 H23 0.81883 0.66358 -0.07328 1.00000 0.03261 0.00000 0.00000 C24 0.71344 0.78592 -0.02933 1.00000 0.02233 0.02811 0.02339 0.00062 0.00087 -0.00166 0.02461 0.00367 0.00027 0.00017 0.00010 0.00000 0.00113 0.00127 0.00110 0.00096 0.00087 0.00096 0.00049 H24 0.64201 0.74913 -0.00061 1.00000 0.02953 0.00000 0.00000 C25 0.71436 0.89170 -0.02900 1.00000 0.01853 0.02605 0.01831 -0.00047 -0.00273 0.00420 0.02097 0.00351 0.00025 0.00016 0.00009 0.00000 0.00108 0.00122 0.00103 0.00091 0.00082 0.00091 0.00047 C26 0.22357 1.06370 0.00702 1.00000 0.02362 0.04208 0.03195 0.00184 -0.00759 0.00195 0.03255 0.00405 0.00028 0.00019 0.00011 0.00000 0.00114 0.00144 0.00125 0.00113 0.00097 0.00109 0.00056 H26A 0.21046 1.13764 0.00882 1.00000 0.04883 0.00000 0.00000 H26B 0.11054 1.03173 0.00589 1.00000 0.04883 0.00000 0.00000 H26C 0.28747 1.04508 -0.03183 1.00000 0.04883 0.00000 0.00000 N1 0.72465 1.07897 0.14236 1.00000 0.01813 0.01815 0.02477 0.00137 0.00040 -0.00043 0.02035 0.00284 0.00020 0.00013 0.00008 0.00000 0.00088 0.00093 0.00091 0.00078 0.00069 0.00075 0.00039 O1 0.31425 1.02968 0.06266 1.00000 0.02075 0.03317 0.02833 0.00253 -0.00160 -0.00255 0.02742 0.00254 0.00019 0.00012 0.00007 0.00000 0.00076 0.00094 0.00082 0.00071 0.00062 0.00068 0.00038 O2 0.90342 1.11403 -0.10249 1.00000 0.03514 0.03826 0.03425 0.01275 0.00738 -0.00506 0.03589 0.00295 0.00021 0.00013 0.00008 0.00000 0.00091 0.00107 0.00089 0.00080 0.00075 0.00083 0.00043 O3 0.60577 0.93696 0.01489 1.00000 0.02348 0.02047 0.02313 0.00013 0.00484 0.00026 0.02236 0.00242 0.00018 0.00011 0.00006 0.00000 0.00074 0.00085 0.00074 0.00067 0.00060 0.00065 0.00034 Final Structure Factor Calculation for 02src643 in P2(1)2(1)2(1) Total number of l.s. parameters = 269 Maximum vector length = 511 Memory required = 3474 / 25046 wR2 = 0.0902 before cycle 5 for 2732 data and 2 / 269 parameters GooF = S = 1.155; Restrained GooF = 1.155 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0416 * P )^2 + 0.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0403 for 2226 Fo > 4sig(Fo) and 0.0581 for all 2732 data wR2 = 0.0902, GooF = S = 1.155, Restrained GooF = 1.155 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 29.00 for non-hydrogen and 31.00 for hydrogen atoms Principal mean square atomic displacements U 0.0360 0.0312 0.0222 C1 0.0292 0.0192 0.0176 C2 0.0302 0.0257 0.0181 C3 0.0295 0.0241 0.0196 C4 0.0270 0.0214 0.0168 C5 0.0323 0.0211 0.0176 C6 0.0322 0.0232 0.0189 C7 0.0236 0.0214 0.0176 C8 0.0307 0.0244 0.0210 C9 0.0374 0.0353 0.0194 C10 0.0322 0.0319 0.0212 C11 0.0309 0.0243 0.0182 C12 0.0311 0.0299 0.0227 C13 0.0355 0.0312 0.0198 C14 0.0286 0.0200 0.0186 C15 0.0243 0.0233 0.0169 C16 0.0277 0.0231 0.0185 C17 0.0337 0.0217 0.0170 C19 0.0343 0.0196 0.0144 C20 0.0404 0.0221 0.0190 C21 0.0474 0.0220 0.0193 C22 0.0354 0.0264 0.0198 C23 0.0286 0.0239 0.0214 C24 0.0282 0.0197 0.0150 C25 0.0424 0.0364 0.0188 C26 0.0251 0.0185 0.0175 N1 0.0349 0.0273 0.0201 O1 0.0492 0.0398 0.0186 O2 0.0282 0.0205 0.0185 O3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.026 0.033 0.042 0.052 0.062 0.076 0.097 0.137 1.000 Number in group 281. 291. 248. 283. 276. 264. 268. 278. 275. 268. GooF 1.032 1.017 1.059 1.146 1.294 1.196 1.272 1.260 0.964 1.264 K 1.313 1.078 1.005 1.021 1.015 1.002 0.993 1.000 1.006 1.016 Resolution(A) 0.77 0.80 0.84 0.88 0.93 0.99 1.07 1.18 1.36 1.73 inf Number in group 286. 260. 274. 275. 274. 275. 268. 278. 268. 274. GooF 1.002 1.028 0.995 1.113 1.137 1.044 1.149 1.066 1.474 1.440 K 1.053 1.105 1.042 0.998 1.004 0.991 1.004 1.013 1.040 1.007 R1 0.158 0.129 0.120 0.095 0.073 0.043 0.034 0.029 0.036 0.027 Recommended weighting scheme: WGHT 0.0392 0.2877 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 8 5 19.39 4.45 4.03 0.012 1.53 4 4 4 747.89 621.90 3.69 0.138 1.60 5 8 15 151.27 99.54 3.61 0.055 0.88 3 0 6 5.12 18.09 3.57 0.024 2.08 1 6 16 39.07 62.20 3.41 0.044 1.11 3 6 18 34.85 62.35 3.40 0.044 0.95 1 9 3 153.84 189.47 3.39 0.076 1.41 3 3 4 132.76 108.81 3.34 0.058 2.06 1 8 3 248.70 207.67 3.25 0.080 1.57 10 2 2 19.05 131.21 3.19 0.063 0.78 0 3 7 80.64 105.84 3.16 0.057 2.46 4 0 1 121.61 151.39 3.05 0.068 1.95 1 1 1 1814.85 2215.07 3.01 0.260 6.40 3 2 6 161.19 134.91 3.00 0.064 1.99 3 7 3 16.36 7.80 2.98 0.015 1.49 0 8 4 42.23 58.77 2.96 0.042 1.57 0 8 3 191.87 244.83 2.95 0.087 1.60 1 5 21 71.65 40.60 2.90 0.035 0.92 1 9 6 103.35 126.94 2.89 0.062 1.33 1 6 8 68.06 51.57 2.89 0.040 1.64 10 2 0 -56.88 63.19 2.88 0.044 0.78 1 3 4 104.75 124.58 2.86 0.062 3.08 4 12 7 90.56 49.33 2.81 0.039 0.91 5 7 8 71.69 94.24 2.80 0.054 1.09 0 1 13 47.87 63.14 2.80 0.044 1.58 0 10 8 325.16 262.87 2.78 0.090 1.17 3 6 5 347.10 300.08 2.77 0.096 1.56 4 5 1 1432.49 1252.19 2.76 0.196 1.57 1 6 20 110.56 76.62 2.74 0.048 0.93 8 2 8 65.05 85.14 2.73 0.051 0.91 5 2 5 12.44 4.88 2.70 0.012 1.43 1 4 1 983.04 1125.33 2.70 0.186 3.00 3 1 24 129.99 89.44 2.69 0.052 0.82 3 8 22 280.45 214.79 2.69 0.081 0.78 3 4 17 150.66 122.42 2.68 0.061 1.05 0 5 12 20.35 4.51 2.68 0.012 1.45 3 0 24 113.04 65.51 2.68 0.045 0.82 8 3 8 42.65 61.12 2.64 0.043 0.90 4 1 19 11.37 23.93 2.61 0.027 0.95 7 1 11 38.80 55.23 2.58 0.041 0.96 0 11 4 82.17 58.34 2.58 0.042 1.17 3 7 13 134.08 163.07 2.58 0.071 1.10 0 2 9 81.29 99.98 2.57 0.055 2.18 5 9 16 195.73 155.68 2.55 0.069 0.82 0 0 6 329.20 283.87 2.54 0.093 3.46 1 5 3 12.94 6.13 2.52 0.014 2.35 2 1 8 580.39 509.18 2.51 0.125 2.13 4 6 3 350.35 300.94 2.51 0.096 1.43 7 4 13 27.96 43.30 2.51 0.036 0.88 0 2 26 301.26 230.87 2.50 0.084 0.79 Bond lengths and angles C1 - Distance Angles C2 1.5112 (0.0030) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - C2 H1A H1B C2 - Distance Angles C7 1.3837 (0.0032) C3 1.3860 (0.0032) 117.41 (0.19) C1 1.5112 (0.0030) 121.88 (0.20) 120.68 (0.20) C2 - C7 C3 C3 - Distance Angles C2 1.3860 (0.0032) C4 1.3859 (0.0029) 121.20 (0.21) H3 0.9500 119.40 119.40 C3 - C2 C4 C4 - Distance Angles C3 1.3859 (0.0029) C5 1.3911 (0.0031) 121.53 (0.21) H4 0.9500 119.23 119.23 C4 - C3 C5 C5 - Distance Angles C6 1.3878 (0.0032) C4 1.3911 (0.0031) 117.34 (0.19) C8 1.5396 (0.0028) 123.87 (0.19) 118.79 (0.19) C5 - C6 C4 C6 - Distance Angles C5 1.3878 (0.0032) C7 1.3963 (0.0030) 120.73 (0.20) H6 0.9500 119.64 119.64 C6 - C5 C7 C7 - Distance Angles C2 1.3837 (0.0032) C6 1.3963 (0.0030) 121.64 (0.20) H7 0.9500 119.18 119.18 C7 - C2 C6 C8 - Distance Angles N1 1.4657 (0.0027) C5 1.5396 (0.0028) 118.46 (0.17) C15 1.5425 (0.0028) 109.42 (0.17) 110.56 (0.17) H8 1.0000 105.83 105.83 105.83 C8 - N1 C5 C15 C9 - Distance Angles N1 1.4772 (0.0026) C10 1.5222 (0.0031) 110.97 (0.17) C11 1.5355 (0.0029) 115.93 (0.17) 110.20 (0.19) H9 1.0000 106.38 106.38 106.38 C9 - N1 C10 C11 C10 - Distance Angles C9 1.5222 (0.0031) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C9 H10A H10B C11 - Distance Angles C9 1.5355 (0.0029) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C9 H11A H11B C12 - Distance Angles N1 1.4724 (0.0027) C14 1.5337 (0.0030) 110.59 (0.18) C13 1.5370 (0.0030) 114.79 (0.18) 109.86 (0.18) H12 1.0000 107.07 107.07 107.07 C12 - N1 C14 C13 C13 - Distance Angles C12 1.5370 (0.0030) H13A 0.9800 109.47 H13B 0.9800 109.47 109.47 H13C 0.9800 109.47 109.47 109.47 C13 - C12 H13A H13B C14 - Distance Angles C12 1.5337 (0.0030) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - C12 H14A H14B C15 - Distance Angles O1 1.4174 (0.0025) C16 1.5119 (0.0029) 111.28 (0.17) C8 1.5425 (0.0028) 107.26 (0.17) 110.08 (0.17) H15 1.0000 109.39 109.39 109.39 C15 - O1 C16 C8 C16 - Distance Angles C17 1.3379 (0.0029) O3 1.3595 (0.0026) 123.49 (0.20) C15 1.5119 (0.0029) 126.24 (0.20) 110.26 (0.18) C16 - C17 O3 C17 - Distance Angles C16 1.3379 (0.0029) C19 1.4526 (0.0030) 122.09 (0.20) H17 0.9500 118.96 118.96 C17 - C16 C19 C19 - Distance Angles O2 1.2373 (0.0026) C17 1.4526 (0.0030) 123.41 (0.21) C20 1.4754 (0.0031) 122.86 (0.21) 113.70 (0.19) C19 - O2 C17 C20 - Distance Angles C25 1.3877 (0.0030) C21 1.4012 (0.0030) 117.60 (0.20) C19 1.4754 (0.0031) 120.02 (0.20) 122.35 (0.20) C20 - C25 C21 C21 - Distance Angles C22 1.3711 (0.0035) C20 1.4012 (0.0030) 121.08 (0.21) H21 0.9500 119.46 119.46 C21 - C22 C20 C22 - Distance Angles C21 1.3711 (0.0035) C23 1.3998 (0.0033) 120.10 (0.21) H22 0.9500 119.95 119.95 C22 - C21 C23 C23 - Distance Angles C24 1.3787 (0.0031) C22 1.3998 (0.0033) 120.25 (0.22) H23 0.9500 119.88 119.88 C23 - C24 C22 C24 - Distance Angles C23 1.3787 (0.0031) C25 1.3932 (0.0031) 118.68 (0.21) H24 0.9500 120.66 120.66 C24 - C23 C25 C25 - Distance Angles O3 1.3811 (0.0024) C20 1.3877 (0.0030) 122.13 (0.19) C24 1.3932 (0.0031) 115.58 (0.18) 122.29 (0.20) C25 - O3 C20 C26 - Distance Angles O1 1.4275 (0.0027) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - O1 H26A H26B N1 - Distance Angles C8 1.4657 (0.0027) C12 1.4724 (0.0027) 118.34 (0.17) C9 1.4772 (0.0027) 117.39 (0.17) 115.66 (0.17) N1 - C8 C12 O1 - Distance Angles C15 1.4174 (0.0026) C26 1.4275 (0.0027) 113.40 (0.16) O1 - C15 O2 - Distance Angles C19 1.2373 (0.0026) O2 - O3 - Distance Angles C16 1.3595 (0.0026) C25 1.3811 (0.0024) 118.41 (0.16) O3 - C16 FMAP and GRID set by program FMAP 2 3 25 GRID -1.136 -2 -2 1.136 2 2 R1 = 0.0581 for 2732 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.19 at 0.1629 0.0649 0.1151 [ 1.67 A from O1 ] Deepest hole -0.19 at 0.3984 0.0230 0.0083 [ 1.24 A from H26C ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 3340 / 22207 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1629 1.0649 0.1151 1.00000 0.05 0.19 1.67 O1 2.08 H14A 2.13 H9 2.29 C26 Q2 1 0.7784 0.9242 -0.0562 1.00000 0.05 0.19 0.52 C20 0.87 C25 1.68 C21 1.82 C19 Q3 1 0.3412 1.0285 0.1944 1.00000 0.05 0.19 0.81 C5 0.92 C4 1.59 H4 1.78 C6 Q4 1 0.1198 1.0808 0.3911 1.00000 0.05 0.16 0.93 H1B 0.93 H1A 1.01 C1 1.85 H1C Q5 1 0.6705 0.9040 0.2478 1.00000 0.05 0.16 0.42 H11C 1.33 C11 1.82 H11B 1.83 H11A Q6 1 0.3323 1.1554 0.0589 1.00000 0.05 0.16 1.07 H15 1.43 H26A 1.58 C15 1.66 O1 Q7 1 0.8252 1.0057 0.2136 1.00000 0.05 0.15 0.76 C11 0.84 C9 1.27 H11A 1.36 H9 Q8 1 0.7201 1.1246 0.1538 1.00000 0.05 0.15 0.65 N1 0.88 C12 1.48 H12 1.77 C8 Q9 1 0.8222 0.5986 -0.0652 1.00000 0.05 0.15 0.87 H23 1.69 O1 1.81 C23 2.48 H8 Q10 1 0.8300 1.1767 -0.0779 1.00000 0.05 0.15 1.13 O2 1.56 C19 1.72 H17 1.89 C17 Shortest distances between peaks (including symmetry equivalents) 5 7 1.94 1 6 2.13 7 8 2.16 1 3 2.21 6 10 2.25 1 9 2.69 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: 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 0.02: Analyse other restraints etc. 0.58: 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 1.06: Structure factors and derivatives 1.05: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.19: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 17:25:59 Total CPU time: 3.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++