+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 17:04:10 on 21-Jan-2003 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02sot149 in P2(1)2(1)2(1) CELL 0.71073 6.8078 9.3184 17.5481 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0002 0.0003 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 52 52 4 12 V = 1113.21 F(000) = 488.0 Mu = 0.10 mm-1 Cell Wt = 924.98 Rho = 1.380 MERG 2 OMIT -3.00 55.00 OMIT 4 1 0 OMIT 3 0 6 OMIT 0 7 3 EXTI 0.10162 FMAP 2 PLAN 10 SIZE 0.14 0.18 0.30 ACTA BOND $H WGHT 0.06000 0.09120 L.S. 4 TEMP -153.00 FVAR 0.98245 C1 1 0.064154 0.039847 0.684605 11.00000 0.03136 0.03121 = 0.02151 0.00574 0.00126 0.00446 AFIX 23 H1A 2 -0.064711 0.002296 0.701513 11.00000 -1.20000 H1B 2 0.168436 -0.008645 0.714320 11.00000 -1.20000 AFIX 0 C2 1 0.074375 0.251038 0.625101 11.00000 0.01902 0.03018 = 0.01434 0.00099 -0.00100 -0.00137 C3 1 0.073664 0.393519 0.606697 11.00000 0.02968 0.02640 = 0.01939 -0.00459 -0.00044 -0.00304 AFIX 43 H3 2 0.069684 0.466300 0.644576 11.00000 -1.20000 AFIX 0 C4 1 0.079122 0.426092 0.528995 11.00000 0.02569 0.02137 = 0.02149 -0.00173 0.00029 -0.00159 AFIX 43 H4 2 0.080246 0.523957 0.513832 11.00000 -1.20000 AFIX 0 C5 1 0.082968 0.320433 0.473086 11.00000 0.01494 0.02169 = 0.01763 -0.00139 -0.00033 -0.00045 C6 1 0.086489 0.174497 0.494091 11.00000 0.02034 0.02152 = 0.01670 -0.00123 0.00097 0.00046 AFIX 43 H6 2 0.091392 0.100263 0.457033 11.00000 -1.20000 AFIX 0 C7 1 0.082510 0.144946 0.570326 11.00000 0.01781 0.02266 = 0.02196 0.00249 0.00025 0.00091 C8 1 0.083513 0.364940 0.393471 11.00000 0.01782 0.01946 = 0.02019 0.00080 0.00052 0.00052 AFIX 43 H8 2 0.105145 0.463992 0.383785 11.00000 -1.20000 AFIX 0 C9 1 0.056809 0.281065 0.332878 11.00000 0.02045 0.01945 = 0.01738 0.00120 -0.00029 -0.00004 AFIX 43 H9 2 0.031511 0.181706 0.339999 11.00000 -1.20000 AFIX 0 C10 1 0.065839 0.339743 0.255073 11.00000 0.01763 0.01942 = 0.01776 0.00010 -0.00032 0.00036 C11 1 0.060752 0.278865 0.119410 11.00000 0.03306 0.02586 = 0.01536 -0.00109 0.00324 -0.00268 AFIX 23 H11A 2 0.138724 0.204963 0.092433 11.00000 -1.20000 H11B 2 0.131093 0.371351 0.114298 11.00000 -1.20000 AFIX 0 C12 1 -0.135407 0.291786 0.081379 11.00000 0.04304 0.02052 = 0.01842 -0.00019 -0.00490 0.00114 AFIX 43 H12 2 -0.136434 0.316322 0.028835 11.00000 -1.20000 AFIX 0 C13 1 -0.306230 0.272007 0.114647 11.00000 0.03598 0.02988 = 0.02955 -0.00054 -0.00855 0.00415 AFIX 93 H13A 2 -0.311815 0.247337 0.167130 11.00000 -1.20000 H13B 2 -0.424125 0.282381 0.086213 11.00000 -1.20000 AFIX 0 N1 3 0.050670 0.241325 0.199432 11.00000 0.02791 0.01837 = 0.01617 -0.00014 -0.00021 -0.00039 O1 4 0.073148 0.191107 0.696400 11.00000 0.03778 0.03369 = 0.01639 0.00361 -0.00091 -0.00254 O2 4 0.090948 0.013095 0.604750 11.00000 0.04221 0.02471 = 0.02193 0.00535 0.00233 0.00227 O3 4 0.091131 0.469009 0.241471 11.00000 0.03716 0.01743 = 0.02072 0.00076 0.00140 -0.00116 H1N 2 0.014455 0.146655 0.212266 11.00000 0.03729 HKLF 4 Covalent radii and connectivity table for 02sot149 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1 O2 C2 - C3 O1 C7 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C8 C6 - C7 C5 C7 - C6 O2 C2 C8 - C9 C5 C9 - C8 C10 C10 - O3 N1 C9 C11 - N1 C12 C12 - C13 C11 C13 - C12 N1 - C10 C11 O1 - C2 C1 O2 - C7 C1 O3 - C10 h k l Fo^2 Sigma Why rejected 0 3 0 7.17 1.02 observed but should be systematically absent 0 7 0 5.25 1.05 observed but should be systematically absent 13519 Reflections read, of which 53 rejected -8 =< h =< 8, -12 =< k =< 11, -22 =< l =< 22, Max. 2-theta = 54.95 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 1 0 227.96 4.28 5 23.60 1 0 1 397.02 8.14 6 42.10 5 1 1 159.85 1.72 6 16.65 3 3 1 124.51 1.70 6 11.01 -7 1 2 46.35 1.69 3 14.14 6 0 5 57.30 0.97 4 13.78 6 4 5 45.00 0.85 6 4.93 7 Inconsistent equivalents 2538 Unique reflections, of which 0 suppressed R(int) = 0.0450 R(sigma) = 0.0287 Friedel opposites not merged Maximum memory for data reduction = 1655 / 25226 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 = 2087 / 198531 wR2 = 0.0875 before cycle 1 for 2538 data and 159 / 159 parameters GooF = S = 1.015; Restrained GooF = 1.015 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0600 * P )^2 + 0.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.97908 0.00247 -1.368 OSF 2 0.07382 0.00862 -3.227 EXTI Mean shift/esd = 0.236 Maximum = -3.227 for EXTI Max. shift = 0.017 A for H1N Max. dU =-0.001 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 2087 / 198531 wR2 = 0.0870 before cycle 2 for 2538 data and 159 / 159 parameters GooF = S = 1.010; Restrained GooF = 1.010 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0600 * P )^2 + 0.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.97816 0.00240 -0.381 OSF 2 0.06798 0.00754 -0.774 EXTI Mean shift/esd = 0.076 Maximum = -0.774 for EXTI Max. shift = 0.007 A for H1N Max. dU =-0.001 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 2087 / 198531 wR2 = 0.0869 before cycle 3 for 2538 data and 159 / 159 parameters GooF = S = 1.010; Restrained GooF = 1.010 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0600 * P )^2 + 0.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.97816 0.00239 -0.001 OSF 2 0.06806 0.00732 0.011 EXTI Mean shift/esd = 0.004 Maximum = -0.032 for U11 H1N Max. shift = 0.001 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 2087 / 198531 wR2 = 0.0869 before cycle 4 for 2538 data and 159 / 159 parameters GooF = S = 1.010; Restrained GooF = 1.010 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0600 * P )^2 + 0.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.97817 0.00239 0.005 OSF 2 0.06815 0.00732 0.012 EXTI Mean shift/esd = 0.001 Maximum = 0.012 for EXTI Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Largest correlation matrix elements 0.544 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A -0.0647 0.0023 0.7016 23 0.990 0.000 C1 O1 O2 H1B 0.1685 -0.0086 0.7143 23 0.990 0.000 C1 O1 O2 H3 0.0697 0.4663 0.6446 43 0.950 0.000 C3 C2 C4 H4 0.0803 0.5240 0.5139 43 0.950 0.000 C4 C5 C3 H6 0.0913 0.1002 0.4571 43 0.950 0.000 C6 C7 C5 H8 0.1051 0.4640 0.3838 43 0.950 0.000 C8 C9 C5 H9 0.0316 0.1816 0.3400 43 0.950 0.000 C9 C8 C10 H11A 0.1387 0.2051 0.0924 23 0.990 0.000 C11 N1 C12 H11B 0.1310 0.3714 0.1143 23 0.990 0.000 C11 N1 C12 H12 -0.1365 0.3163 0.0289 43 0.950 0.000 C12 C13 C11 H13A -0.3120 0.2473 0.1671 93 0.950 0.000 C13 C12 C11 H13B -0.4242 0.2824 0.0862 93 0.950 0.000 C13 C12 C11 02sot149 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.06418 0.03986 0.68464 1.00000 0.03084 0.03160 0.02107 0.00579 0.00133 0.00447 0.02784 0.00224 0.00019 0.00013 0.00007 0.00000 0.00060 0.00059 0.00055 0.00047 0.00048 0.00058 0.00027 H1A -0.06467 0.00231 0.70156 1.00000 0.03340 0.00000 0.00000 H1B 0.16849 -0.00861 0.71434 1.00000 0.03340 0.00000 0.00000 C2 0.07434 0.25104 0.62510 1.00000 0.01884 0.02959 0.01445 0.00102 -0.00102 -0.00138 0.02096 0.00187 0.00017 0.00012 0.00006 0.00000 0.00049 0.00057 0.00048 0.00041 0.00042 0.00047 0.00024 C3 0.07366 0.39351 0.60667 1.00000 0.02950 0.02603 0.01942 -0.00461 -0.00040 -0.00297 0.02498 0.00200 0.00019 0.00013 0.00007 0.00000 0.00056 0.00055 0.00053 0.00042 0.00049 0.00053 0.00025 H3 0.06968 0.46629 0.64456 1.00000 0.02998 0.00000 0.00000 C4 0.07915 0.42614 0.52902 1.00000 0.02529 0.02134 0.02138 -0.00185 0.00033 -0.00169 0.02267 0.00195 0.00018 0.00012 0.00006 0.00000 0.00054 0.00050 0.00052 0.00041 0.00048 0.00049 0.00024 H4 0.08032 0.52401 0.51387 1.00000 0.02720 0.00000 0.00000 C5 0.08296 0.32044 0.47310 1.00000 0.01479 0.02117 0.01771 -0.00145 -0.00032 -0.00041 0.01789 0.00179 0.00016 0.00011 0.00006 0.00000 0.00047 0.00052 0.00050 0.00039 0.00043 0.00043 0.00023 C6 0.08643 0.17450 0.49414 1.00000 0.02023 0.02099 0.01673 -0.00126 0.00090 0.00053 0.01932 0.00193 0.00017 0.00011 0.00006 0.00000 0.00052 0.00051 0.00049 0.00038 0.00042 0.00044 0.00023 H6 0.09127 0.10024 0.45709 1.00000 0.02318 0.00000 0.00000 C7 0.08251 0.14499 0.57029 1.00000 0.01741 0.02253 0.02188 0.00244 0.00027 0.00101 0.02061 0.00198 0.00017 0.00012 0.00006 0.00000 0.00049 0.00052 0.00054 0.00042 0.00043 0.00045 0.00023 C8 0.08352 0.36493 0.39346 1.00000 0.01738 0.01930 0.02013 0.00069 0.00050 0.00050 0.01894 0.00186 0.00015 0.00011 0.00006 0.00000 0.00048 0.00048 0.00051 0.00039 0.00043 0.00044 0.00023 H8 0.10514 0.46398 0.38375 1.00000 0.02272 0.00000 0.00000 C9 0.05682 0.28100 0.33288 1.00000 0.02020 0.01917 0.01742 0.00118 -0.00017 0.00001 0.01893 0.00188 0.00017 0.00011 0.00006 0.00000 0.00050 0.00046 0.00049 0.00039 0.00042 0.00046 0.00022 H9 0.03157 0.18164 0.34001 1.00000 0.02272 0.00000 0.00000 C10 0.06582 0.33973 0.25505 1.00000 0.01737 0.01918 0.01779 0.00015 -0.00044 0.00039 0.01811 0.00183 0.00017 0.00011 0.00006 0.00000 0.00046 0.00048 0.00049 0.00039 0.00043 0.00046 0.00022 C11 0.06070 0.27891 0.11941 1.00000 0.03294 0.02575 0.01524 -0.00101 0.00322 -0.00263 0.02464 0.00205 0.00019 0.00013 0.00006 0.00000 0.00059 0.00054 0.00049 0.00042 0.00046 0.00054 0.00025 H11A 0.13868 0.20505 0.09240 1.00000 0.02957 0.00000 0.00000 H11B 0.13097 0.37143 0.11429 1.00000 0.02957 0.00000 0.00000 C12 -0.13551 0.29178 0.08142 1.00000 0.04264 0.02029 0.01826 -0.00007 -0.00458 0.00121 0.02706 0.00211 0.00020 0.00013 0.00007 0.00000 0.00073 0.00053 0.00051 0.00041 0.00048 0.00053 0.00028 H12 -0.13652 0.31631 0.02887 1.00000 0.03247 0.00000 0.00000 C13 -0.30635 0.27201 0.11463 1.00000 0.03612 0.02966 0.02956 -0.00048 -0.00876 0.00419 0.03178 0.00232 0.00020 0.00014 0.00008 0.00000 0.00067 0.00064 0.00063 0.00052 0.00054 0.00056 0.00029 H13A -0.31204 0.24735 0.16711 1.00000 0.03814 0.00000 0.00000 H13B -0.42419 0.28238 0.08616 1.00000 0.03814 0.00000 0.00000 N1 0.05078 0.24133 0.19943 1.00000 0.02759 0.01840 0.01602 0.00001 -0.00017 -0.00031 0.02067 0.00168 0.00015 0.00010 0.00005 0.00000 0.00050 0.00044 0.00043 0.00033 0.00036 0.00042 0.00022 O1 0.07317 0.19112 0.69641 1.00000 0.03724 0.03396 0.01621 0.00358 -0.00084 -0.00253 0.02913 0.00156 0.00015 0.00009 0.00004 0.00000 0.00048 0.00047 0.00038 0.00032 0.00037 0.00044 0.00022 O2 0.09093 0.01307 0.60473 1.00000 0.04225 0.02456 0.02169 0.00528 0.00236 0.00225 0.02950 0.00156 0.00014 0.00009 0.00005 0.00000 0.00051 0.00042 0.00042 0.00032 0.00039 0.00038 0.00023 O3 0.09109 0.46900 0.24144 1.00000 0.03695 0.01730 0.02058 0.00081 0.00144 -0.00106 0.02494 0.00144 0.00014 0.00008 0.00005 0.00000 0.00047 0.00037 0.00037 0.00029 0.00035 0.00037 0.00021 H1N 0.01732 0.14819 0.21236 1.00000 0.03495 0.02673 0.00223 0.00181 0.00089 0.00000 0.00414 Final Structure Factor Calculation for 02sot149 in P2(1)2(1)2(1) Total number of l.s. parameters = 159 Maximum vector length = 511 Memory required = 1930 / 25046 wR2 = 0.0870 before cycle 5 for 2538 data and 2 / 159 parameters GooF = S = 1.010; Restrained GooF = 1.010 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0600 * P )^2 + 0.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0310 for 2414 Fo > 4sig(Fo) and 0.0337 for all 2538 data wR2 = 0.0870, GooF = S = 1.010, Restrained GooF = 1.010 for all data Flack x parameter = -0.5764 with esd 0.8078 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0374 0.0276 0.0185 C1 0.0299 0.0188 0.0142 C2 0.0316 0.0265 0.0168 C3 0.0261 0.0225 0.0193 C4 0.0217 0.0173 0.0147 C5 0.0214 0.0204 0.0161 C6 0.0248 0.0198 0.0172 C7 0.0207 0.0189 0.0172 C8 0.0202 0.0198 0.0168 C9 0.0193 0.0181 0.0170 C10 0.0344 0.0249 0.0146 C11 0.0435 0.0202 0.0174 C12 0.0432 0.0293 0.0228 C13 0.0276 0.0184 0.0160 N1 0.0389 0.0330 0.0155 O1 0.0430 0.0279 0.0176 O2 0.0371 0.0207 0.0170 O3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.030 0.045 0.059 0.073 0.088 0.106 0.131 0.166 0.237 1.000 Number in group 255. 258. 275. 232. 271. 244. 246. 248. 254. 255. GooF 1.102 1.062 1.046 0.997 0.947 1.014 1.089 0.972 0.960 0.891 K 1.004 0.991 0.995 0.998 0.987 1.009 1.007 1.007 1.010 1.011 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 267. 244. 250. 255. 257. 250. 261. 245. 254. 255. GooF 1.003 0.983 0.960 0.971 0.967 1.088 0.935 0.913 1.049 1.198 K 1.059 1.025 0.993 1.014 1.018 1.008 1.003 1.011 1.025 1.001 R1 0.066 0.069 0.046 0.041 0.034 0.031 0.025 0.022 0.027 0.026 Recommended weighting scheme: WGHT 0.0523 0.1125 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) 0 3 16 29.52 18.65 4.82 0.055 1.03 0 0 22 748.68 507.33 4.46 0.286 0.80 1 10 0 9.55 16.72 4.26 0.052 0.92 2 0 9 77.92 57.97 4.18 0.097 1.69 -2 1 22 269.07 200.38 3.82 0.180 0.77 0 4 16 61.16 81.63 3.81 0.115 0.99 -1 9 4 29.96 21.98 3.42 0.060 1.00 2 1 22 265.31 200.31 3.28 0.180 0.77 1 1 13 75.61 95.43 3.21 0.124 1.31 -3 2 6 94.60 76.16 3.18 0.111 1.67 3 0 7 2.62 5.20 3.16 0.029 1.68 0 8 12 54.97 70.76 3.14 0.107 0.91 2 0 5 10.78 7.46 3.05 0.035 2.44 1 8 13 18.55 25.74 3.04 0.064 0.87 -1 7 13 32.42 42.82 3.01 0.083 0.94 0 5 2 512.94 427.74 3.01 0.263 1.82 -1 10 4 26.68 34.99 2.99 0.075 0.90 0 1 15 41.37 52.74 2.98 0.092 1.16 3 7 3 5.07 2.86 2.95 0.021 1.13 -2 5 16 9.87 14.63 2.93 0.049 0.91 1 9 4 28.65 22.00 2.89 0.060 1.00 1 0 7 182.30 220.28 2.89 0.189 2.35 0 2 18 4.81 8.12 2.86 0.036 0.95 2 3 0 56.90 69.97 2.82 0.106 2.29 0 1 4 507.80 606.72 2.81 0.313 3.97 -1 9 3 95.44 116.41 2.80 0.137 1.01 -8 1 1 113.26 142.92 2.79 0.152 0.85 8 0 3 8.52 12.25 2.75 0.044 0.84 -3 7 1 0.92 2.59 2.72 0.020 1.15 -5 3 7 104.97 86.55 2.72 0.118 1.12 -8 1 2 83.26 106.14 2.70 0.131 0.84 1 9 3 96.44 116.75 2.69 0.137 1.01 -3 3 18 97.05 77.13 2.68 0.112 0.86 1 4 12 34.96 43.66 2.68 0.084 1.22 0 2 3 8.71 11.98 2.67 0.044 3.64 -1 6 2 40.71 49.97 2.64 0.090 1.49 1 6 2 40.90 50.15 2.63 0.090 1.49 -2 9 3 41.23 50.96 2.61 0.091 0.98 0 3 2 123.66 146.99 2.58 0.154 2.93 -2 9 1 7.54 10.95 2.56 0.042 0.99 0 7 12 37.61 46.49 2.54 0.087 0.98 0 6 0 325.22 277.11 2.54 0.211 1.55 0 8 3 82.75 99.17 2.53 0.126 1.14 2 1 4 176.85 208.70 2.52 0.183 2.58 7 3 9 17.64 23.83 2.52 0.062 0.84 0 2 16 142.14 168.94 2.51 0.165 1.07 -4 7 13 15.18 21.52 2.51 0.059 0.83 -4 4 2 218.14 185.45 2.49 0.173 1.36 2 9 12 32.33 23.32 2.48 0.061 0.82 2 0 22 136.43 110.38 2.48 0.133 0.78 Bond lengths and angles C1 - Distance Angles O1 1.4258 (0.0015) O2 1.4359 (0.0014) 107.93 (0.09) H1A 0.9900 110.12 110.12 H1B 0.9900 110.12 110.12 108.44 C1 - O1 O2 H1A C2 - Distance Angles C3 1.3665 (0.0017) O1 1.3703 (0.0013) 127.73 (0.10) C7 1.3802 (0.0016) 122.07 (0.10) 110.18 (0.10) C2 - C3 O1 C3 - Distance Angles C2 1.3665 (0.0017) C4 1.3967 (0.0016) 116.25 (0.10) H3 0.9500 121.88 121.88 C3 - C2 C4 C4 - Distance Angles C5 1.3906 (0.0015) C3 1.3967 (0.0016) 122.33 (0.10) H4 0.9500 118.83 118.83 C4 - C5 C3 C5 - Distance Angles C4 1.3906 (0.0015) C6 1.4094 (0.0015) 119.93 (0.10) C8 1.4578 (0.0014) 118.37 (0.10) 121.70 (0.10) C5 - C4 C6 C6 - Distance Angles C7 1.3645 (0.0015) C5 1.4094 (0.0015) 116.78 (0.10) H6 0.9500 121.61 121.61 C6 - C7 C5 C7 - Distance Angles C6 1.3645 (0.0015) O2 1.3710 (0.0013) 127.70 (0.10) C2 1.3802 (0.0016) 122.62 (0.10) 109.66 (0.10) C7 - C6 O2 C8 - Distance Angles C9 1.3321 (0.0015) C5 1.4578 (0.0014) 126.70 (0.10) H8 0.9500 116.65 116.65 C8 - C9 C5 C9 - Distance Angles C8 1.3321 (0.0015) C10 1.4726 (0.0014) 121.08 (0.10) H9 0.9500 119.46 119.46 C9 - C8 C10 C10 - Distance Angles O3 1.2401 (0.0013) N1 1.3431 (0.0014) 122.26 (0.10) C9 1.4726 (0.0014) 123.05 (0.10) 114.65 (0.09) C10 - O3 N1 C11 - Distance Angles N1 1.4488 (0.0014) C12 1.4976 (0.0018) 114.16 (0.10) H11A 0.9900 108.72 108.72 H11B 0.9900 108.72 108.72 107.63 C11 - N1 C12 H11A C12 - Distance Angles C13 1.3139 (0.0019) C11 1.4976 (0.0018) 125.51 (0.11) H12 0.9500 117.25 117.25 C12 - C13 C11 C13 - Distance Angles C12 1.3139 (0.0019) H13A 0.9500 120.00 H13B 0.9500 120.00 120.00 C13 - C12 H13A N1 - Distance Angles C10 1.3431 (0.0014) C11 1.4488 (0.0014) 122.40 (0.09) H1N 0.9256 (0.0168) 118.73 (0.98) 118.41 (0.97) N1 - C10 C11 O1 - Distance Angles C2 1.3703 (0.0013) C1 1.4258 (0.0015) 105.71 (0.08) O1 - C2 O2 - Distance Angles C7 1.3710 (0.0013) C1 1.4359 (0.0014) 105.62 (0.09) O2 - C7 O3 - Distance Angles C10 1.2401 (0.0013) O3 - FMAP and GRID set by program FMAP 2 1 11 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0324 for 1482 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.22 at 0.0948 0.3033 0.3003 [ 0.66 A from C9 ] Deepest hole -0.16 at 0.0875 0.4172 0.4245 [ 0.73 A from C8 ] Mean = 0.00, Rms deviation from mean = 0.03 e/A^3, Highest memory used = 2243 / 18043 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0948 0.3033 0.3003 1.00000 0.05 0.22 0.66 C9 0.89 C10 1.40 H9 1.74 C8 Q2 1 0.1201 0.1634 0.5362 1.00000 0.05 0.19 0.67 C7 0.78 C6 1.52 H6 1.79 C2 Q3 1 0.0189 0.2024 0.5953 1.00000 0.05 0.19 0.79 C2 0.82 C7 1.82 O1 1.83 C3 Q4 1 0.1257 0.3186 0.6189 1.00000 0.05 0.16 0.73 C2 0.81 C3 1.50 H3 1.84 O1 Q5 1 0.0548 0.3424 0.4405 1.00000 0.05 0.15 0.64 C5 0.87 C8 1.55 H8 1.75 C4 Q6 1 0.1103 0.3432 0.4408 1.00000 0.05 0.15 0.63 C5 0.87 C8 1.51 H8 1.74 C4 Q7 1 0.0148 0.3124 0.6151 1.00000 0.05 0.14 0.72 C2 0.87 C3 1.57 H3 1.81 C7 Q8 1 0.1343 0.3663 0.5016 1.00000 0.05 0.14 0.75 C5 0.83 C4 1.53 H4 1.82 C6 Q9 1 0.0371 0.2523 0.4829 1.00000 0.05 0.13 0.73 C5 0.82 C6 1.53 H6 1.83 C4 Q10 1 0.0864 0.3991 0.5747 1.00000 0.05 0.12 0.57 C3 0.84 C4 1.38 H3 1.58 H4 Shortest distances between peaks (including symmetry equivalents) 5 6 0.38 4 7 0.76 3 7 1.08 6 8 1.10 4 10 1.11 5 9 1.13 7 10 1.18 5 8 1.22 6 9 1.23 8 9 1.29 2 3 1.30 8 10 1.36 3 4 1.37 2 9 1.37 3 10 1.92 2 8 1.99 3 9 2.03 2 4 2.05 2 7 2.09 4 8 2.11 9 10 2.14 7 8 2.21 2 10 2.31 2 6 2.37 3 8 2.38 7 9 2.39 2 5 2.41 6 10 2.41 5 10 2.42 1 6 2.50 1 5 2.50 4 9 2.54 3 6 2.88 2 9 2.96 8 9 2.97 2 5 2.99 Time profile in seconds ----------------------- 0.11: 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 0.00: Analyse other restraints etc. 0.33: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.88: Structure factors and derivatives 0.42: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.00: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 17:04:12 Total elapsed time: 2.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++