+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007jmw0003 started at 11:24:30 on 27-Feb-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007jmw0003 in Pnn2 CELL 0.71073 12.7013 16.5159 4.3164 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0006 0.0001 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, 1/2 + Z SFAC C H N O UNIT 40 44 12 4 V = 905.47 F(000) = 400.0 Mu = 0.09 mm-1 Cell Wt = 756.87 Rho = 1.388 MERG 4 OMIT -3.00 55.00 FMAP 2 PLAN 5 SIZE 0.05 0.05 0.30 ACTA BOND $H L.S. 6 TEMP -153.00 WGHT 0.0424 0.1000 EXTI 0.009036 FVAR 1.18703 C1 1 0.240524 0.058138 0.412668 11.00000 0.02406 0.02048 = 0.02767 -0.00167 -0.00164 0.00465 AFIX 43 H1 2 0.291891 0.033717 0.282815 11.00000 -1.20000 AFIX 0 C2 1 0.098206 0.079347 0.640228 11.00000 0.02182 0.01883 = 0.02761 0.00275 -0.00109 -0.00152 AFIX 43 H2 2 0.027671 0.076153 0.712424 11.00000 -1.20000 AFIX 0 C3 1 0.150685 0.208517 0.917664 11.00000 0.02698 0.01994 = 0.01848 -0.00373 0.00183 -0.00238 AFIX 23 H3A 2 0.212735 0.216466 1.053097 11.00000 -1.20000 H3B 2 0.088430 0.200011 1.051780 11.00000 -1.20000 AFIX 0 C4 1 0.134204 0.283224 0.721942 11.00000 0.02152 0.01826 = 0.01883 -0.00458 -0.00005 0.00167 C5 1 0.217857 0.333278 0.627343 11.00000 0.01928 0.01847 = 0.01667 -0.00421 0.00062 0.00137 C6 1 0.195885 0.398181 0.430453 11.00000 0.02395 0.01940 = 0.02260 -0.00180 0.00446 -0.00127 AFIX 43 H6 2 0.251909 0.431728 0.361263 11.00000 -1.20000 AFIX 0 C7 1 0.094154 0.414691 0.333887 11.00000 0.02757 0.02167 = 0.02513 -0.00168 -0.00291 0.00655 AFIX 43 H7 2 0.081134 0.459091 0.199315 11.00000 -1.20000 AFIX 0 C8 1 0.011540 0.366793 0.432640 11.00000 0.01956 0.02751 = 0.03309 -0.00362 -0.00756 0.00363 AFIX 43 H8 2 -0.058471 0.378526 0.369534 11.00000 -1.20000 AFIX 0 C9 1 0.031935 0.301519 0.624559 11.00000 0.01862 0.02503 = 0.02666 -0.00546 0.00092 -0.00305 AFIX 43 H9 2 -0.024816 0.268404 0.691630 11.00000 -1.20000 AFIX 0 C10 1 0.329746 0.318494 0.738526 11.00000 0.02002 0.01986 = 0.02669 -0.00202 0.00056 0.00035 AFIX 23 H10A 2 0.330326 0.319377 0.967853 11.00000 -1.20000 H10B 2 0.351878 0.263734 0.671730 11.00000 -1.20000 AFIX 0 N1 3 0.166978 0.136787 0.723512 11.00000 0.01986 0.01856 = 0.02018 0.00277 -0.00002 0.00012 N2 3 0.260281 0.124280 0.575850 11.00000 0.01994 0.02151 = 0.02647 -0.00074 0.00076 0.00160 N3 3 0.141635 0.027518 0.443602 11.00000 0.02743 0.01868 = 0.03093 0.00062 -0.00540 0.00112 O1 4 0.404446 0.375725 0.628151 11.00000 0.01846 0.02512 = 0.03788 -0.00520 0.00426 -0.00154 AFIX 3 H1A 2 0.397186 0.419535 0.724661 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for 2007jmw0003 in Pnn2 C 0.770 H 0.320 N 0.700 O 0.660 C1 - N2 N3 C2 - N3 N1 C3 - N1 C4 C4 - C9 C5 C3 C5 - C6 C4 C10 C6 - C7 C5 C7 - C8 C6 C8 - C7 C9 C9 - C8 C4 C10 - O1 C5 N1 - C2 N2 C3 N2 - C1 N1 N3 - C2 C1 O1 - C10 Floating origin restraints generated 10824 Reflections read, of which 540 rejected -16 =< h =< 16, -21 =< k =< 21, -5 =< l =< 5, Max. 2-theta = 54.98 0 Systematic absence violations 0 Inconsistent equivalents 1180 Unique reflections, of which 0 suppressed R(int) = 0.0516 R(sigma) = 0.0312 Friedel opposites merged Maximum memory for data reduction = 1429 / 11466 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 = 1791 / 162323 wR2 = 0.0832 before cycle 1 for 1180 data and 128 / 128 parameters GooF = S = 1.108; Restrained GooF = 1.108 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0424 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18759 0.00353 0.159 OSF 2 0.01058 0.00385 0.401 EXTI Mean shift/esd = 0.154 Maximum = 0.527 for U33 C4 Max. shift = 0.001 A for C8 Max. dU = 0.000 for C9 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1791 / 162323 wR2 = 0.0830 before cycle 2 for 1180 data and 128 / 128 parameters GooF = S = 1.106; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0424 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18748 0.00352 -0.033 OSF 2 0.01108 0.00391 0.127 EXTI Mean shift/esd = 0.051 Maximum = 0.169 for U33 C4 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C9 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1791 / 162323 wR2 = 0.0829 before cycle 3 for 1180 data and 128 / 128 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0424 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18746 0.00352 -0.005 OSF 2 0.01107 0.00394 -0.002 EXTI Mean shift/esd = 0.003 Maximum = -0.023 for x N3 Max. shift = 0.000 A for N3 Max. dU = 0.000 for C7 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1791 / 162323 wR2 = 0.0829 before cycle 4 for 1180 data and 128 / 128 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0424 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18746 0.00352 0.000 OSF 2 0.01106 0.00394 -0.002 EXTI Mean shift/esd = 0.001 Maximum = 0.004 for U11 C10 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C3 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1791 / 162323 wR2 = 0.0829 before cycle 5 for 1180 data and 128 / 128 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0424 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18746 0.00352 0.000 OSF 2 0.01106 0.00394 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for U11 C8 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C8 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1791 / 162323 wR2 = 0.0829 before cycle 6 for 1180 data and 128 / 128 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0424 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.18746 0.00352 0.000 OSF 2 0.01106 0.00394 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for N2 Max. dU = 0.000 for C6 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.2920 0.0338 0.2827 43 0.950 0.000 C1 N2 N3 H2 0.0277 0.0761 0.7123 43 0.950 0.000 C2 N3 N1 H3A 0.2128 0.2165 1.0530 23 0.990 0.000 C3 N1 C4 H3B 0.0885 0.2000 1.0521 23 0.990 0.000 C3 N1 C4 H6 0.2520 0.4317 0.3612 43 0.950 0.000 C6 C7 C5 H7 0.0811 0.4591 0.1991 43 0.950 0.000 C7 C8 C6 H8 -0.0586 0.3784 0.3693 43 0.950 0.000 C8 C7 C9 H9 -0.0248 0.2685 0.6917 43 0.950 0.000 C9 C8 C4 H10A 0.3303 0.3194 0.9679 23 0.990 0.000 C10 O1 C5 H10B 0.3518 0.2637 0.6718 23 0.990 0.000 C10 O1 C5 2007jmw0003 in Pnn2 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.24060 0.05816 0.41264 1.00000 0.02374 0.02054 0.02766 -0.00154 -0.00201 0.00454 0.02398 0.00357 0.00015 0.00012 0.00054 0.00000 0.00103 0.00097 0.00107 0.00087 0.00099 0.00080 0.00044 H1 0.29198 0.03377 0.28275 1.00000 0.02878 0.00000 0.00000 C2 0.09821 0.07933 0.64018 1.00000 0.02187 0.01863 0.02760 0.00242 -0.00120 -0.00156 0.02270 0.00346 0.00015 0.00011 0.00053 0.00000 0.00100 0.00093 0.00111 0.00090 0.00092 0.00074 0.00044 H2 0.02766 0.07614 0.71230 1.00000 0.02724 0.00000 0.00000 C3 0.15073 0.20850 0.91781 1.00000 0.02713 0.01999 0.01820 -0.00341 0.00190 -0.00229 0.02177 0.00339 0.00015 0.00011 0.00050 0.00000 0.00104 0.00095 0.00094 0.00085 0.00097 0.00075 0.00043 H3A 0.21284 0.21646 1.05299 1.00000 0.02613 0.00000 0.00000 H3B 0.08854 0.20000 1.05215 1.00000 0.02613 0.00000 0.00000 C4 0.13415 0.28324 0.72186 1.00000 0.02136 0.01799 0.01948 -0.00446 0.00026 0.00144 0.01961 0.00330 0.00015 0.00011 0.00048 0.00000 0.00097 0.00091 0.00095 0.00079 0.00082 0.00075 0.00042 C5 0.21787 0.33325 0.62750 1.00000 0.01912 0.01821 0.01699 -0.00441 0.00066 0.00133 0.01811 0.00316 0.00015 0.00011 0.00045 0.00000 0.00090 0.00090 0.00089 0.00076 0.00077 0.00072 0.00039 C6 0.19594 0.39818 0.43039 1.00000 0.02405 0.01920 0.02257 -0.00166 0.00412 -0.00121 0.02194 0.00344 0.00015 0.00011 0.00049 0.00000 0.00102 0.00094 0.00096 0.00088 0.00092 0.00081 0.00042 H6 0.25198 0.43171 0.36117 1.00000 0.02632 0.00000 0.00000 C7 0.09408 0.41471 0.33368 1.00000 0.02755 0.02174 0.02514 -0.00154 -0.00262 0.00650 0.02481 0.00357 0.00015 0.00012 0.00053 0.00000 0.00115 0.00106 0.00107 0.00087 0.00085 0.00083 0.00048 H7 0.08105 0.45911 0.19912 1.00000 0.02977 0.00000 0.00000 C8 0.01146 0.36676 0.43248 1.00000 0.01962 0.02725 0.03330 -0.00368 -0.00725 0.00335 0.02672 0.00361 0.00015 0.00012 0.00058 0.00000 0.00103 0.00102 0.00108 0.00099 0.00103 0.00080 0.00046 H8 -0.05857 0.37843 0.36934 1.00000 0.03207 0.00000 0.00000 C9 0.03199 0.30157 0.62445 1.00000 0.01872 0.02470 0.02636 -0.00490 0.00086 -0.00320 0.02326 0.00339 0.00015 0.00011 0.00051 0.00000 0.00094 0.00100 0.00107 0.00090 0.00085 0.00079 0.00045 H9 -0.02476 0.26847 0.69168 1.00000 0.02791 0.00000 0.00000 C10 0.32973 0.31848 0.73859 1.00000 0.01996 0.02004 0.02700 -0.00178 0.00068 0.00028 0.02233 0.00334 0.00014 0.00011 0.00052 0.00000 0.00101 0.00096 0.00107 0.00086 0.00090 0.00075 0.00045 H10A 0.33032 0.31937 0.96791 1.00000 0.02680 0.00000 0.00000 H10B 0.35185 0.26372 0.67182 1.00000 0.02680 0.00000 0.00000 N1 0.16695 0.13680 0.72353 1.00000 0.02023 0.01822 0.02026 0.00282 -0.00029 0.00002 0.01957 0.00272 0.00012 0.00009 0.00039 0.00000 0.00084 0.00079 0.00082 0.00070 0.00074 0.00061 0.00038 N2 0.26025 0.12427 0.57587 1.00000 0.01966 0.02145 0.02658 -0.00085 0.00090 0.00161 0.02256 0.00279 0.00013 0.00009 0.00040 0.00000 0.00083 0.00086 0.00093 0.00071 0.00076 0.00066 0.00040 N3 0.14163 0.02750 0.44371 1.00000 0.02711 0.01875 0.03079 0.00043 -0.00515 0.00114 0.02555 0.00301 0.00013 0.00010 0.00046 0.00000 0.00090 0.00078 0.00095 0.00080 0.00089 0.00069 0.00039 O1 0.40444 0.37569 0.62817 1.00000 0.01815 0.02489 0.03803 -0.00492 0.00434 -0.00150 0.02703 0.00248 0.00010 0.00008 0.00040 0.00000 0.00069 0.00074 0.00090 0.00071 0.00068 0.00055 0.00038 H1A 0.39718 0.41950 0.72468 1.00000 0.04054 0.00000 0.00000 Final Structure Factor Calculation for 2007jmw0003 in Pnn2 Total number of l.s. parameters = 128 Maximum vector length = 511 Memory required = 1665 / 25046 wR2 = 0.0829 before cycle 7 for 1180 data and 2 / 128 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0424 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0329 for 1023 Fo > 4sig(Fo) and 0.0424 for all 1180 data wR2 = 0.0829, GooF = S = 1.105, Restrained GooF = 1.105 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 11.00 for hydrogen atoms Principal mean square atomic displacements U 0.0299 0.0248 0.0173 C1 0.0286 0.0219 0.0176 C2 0.0286 0.0211 0.0156 C3 0.0235 0.0213 0.0140 C4 0.0222 0.0193 0.0128 C5 0.0279 0.0194 0.0184 C6 0.0329 0.0240 0.0175 C7 0.0384 0.0255 0.0162 C8 0.0311 0.0215 0.0171 C9 0.0275 0.0202 0.0193 C10 0.0223 0.0202 0.0162 N1 0.0268 0.0224 0.0185 N2 0.0344 0.0238 0.0185 N3 0.0406 0.0233 0.0172 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.026 0.041 0.053 0.067 0.083 0.104 0.123 0.156 0.219 1.000 Number in group 125. 115. 119. 118. 114. 125. 113. 117. 115. 119. GooF 0.820 1.054 1.220 1.309 1.226 1.145 1.047 1.031 1.080 1.056 K 1.019 0.915 0.913 0.970 0.994 0.998 0.998 1.009 1.016 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.06 1.17 1.36 1.73 inf Number in group 123. 116. 117. 118. 116. 119. 118. 118. 117. 118. GooF 1.167 1.116 1.076 1.016 0.943 0.948 1.051 1.024 1.265 1.368 K 1.006 1.018 1.017 0.999 0.998 1.002 1.010 0.992 1.023 1.003 R1 0.110 0.104 0.075 0.062 0.035 0.038 0.029 0.027 0.029 0.022 Recommended weighting scheme: WGHT 0.0420 0.1623 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) 1 2 0 10.93 20.75 4.75 0.055 6.92 1 13 0 1.42 14.43 3.95 0.046 1.26 7 5 1 26.74 17.98 3.88 0.051 1.49 8 13 1 54.51 37.37 3.42 0.074 0.97 0 6 0 49.68 63.96 3.37 0.096 2.75 3 3 1 20.40 27.26 3.30 0.063 2.65 5 8 0 289.41 239.06 3.21 0.186 1.60 1 11 3 22.58 32.85 3.20 0.069 1.04 12 13 1 46.86 28.90 3.19 0.065 0.80 13 10 2 131.75 100.92 3.18 0.121 0.78 1 11 4 30.78 41.63 2.86 0.078 0.87 2 8 0 29.74 22.45 2.84 0.057 1.96 5 1 5 290.36 244.90 2.82 0.188 0.82 10 13 2 33.30 46.31 2.82 0.082 0.83 10 1 2 42.65 53.92 2.72 0.088 1.09 2 13 3 117.93 141.16 2.71 0.143 0.94 13 2 2 42.10 55.99 2.70 0.090 0.88 2 14 1 10.20 17.21 2.66 0.050 1.12 4 4 0 670.82 593.02 2.63 0.293 2.52 3 18 2 25.12 39.02 2.63 0.075 0.83 7 1 0 450.06 394.28 2.61 0.239 1.80 3 11 0 245.19 212.33 2.56 0.175 1.42 9 8 4 4.90 13.30 2.49 0.044 0.79 11 7 1 16.45 26.48 2.48 0.062 1.01 15 4 2 50.91 33.82 2.48 0.070 0.77 0 19 1 153.86 126.68 2.47 0.135 0.85 0 21 1 29.85 48.12 2.44 0.083 0.77 11 14 1 45.33 31.66 2.42 0.068 0.81 3 8 0 162.76 141.67 2.37 0.143 1.86 1 13 2 39.43 47.94 2.33 0.083 1.09 3 2 2 52.76 61.66 2.31 0.095 1.87 3 4 5 7.20 0.26 2.28 0.006 0.83 8 3 1 47.37 56.03 2.27 0.090 1.44 14 11 0 105.50 82.84 2.23 0.110 0.78 10 11 2 11.86 5.91 2.22 0.029 0.88 3 12 4 49.88 61.69 2.22 0.095 0.83 4 1 1 11.33 8.71 2.21 0.036 2.53 1 0 3 292.91 260.61 2.20 0.194 1.43 16 1 0 114.43 92.18 2.20 0.116 0.79 6 13 0 5.54 10.87 2.15 0.040 1.09 4 3 0 176.54 197.89 2.14 0.169 2.75 1 3 5 124.19 108.06 2.14 0.125 0.85 10 6 0 127.18 146.07 2.13 0.145 1.15 0 3 5 304.55 266.14 2.12 0.196 0.85 7 13 0 13.63 22.27 2.11 0.057 1.04 1 6 1 3.50 1.93 2.11 0.017 2.28 3 16 0 -1.26 4.96 2.10 0.027 1.00 8 1 2 18.02 23.12 2.10 0.058 1.28 6 10 0 12.91 18.58 2.09 0.052 1.30 0 6 2 257.09 230.72 2.08 0.183 1.70 Bond lengths and angles C1 - Distance Angles N2 1.3232 (0.0025) N3 1.3618 (0.0026) 115.37 (0.19) H1 0.9500 122.32 122.32 C1 - N2 N3 C2 - Distance Angles N3 1.3252 (0.0027) N1 1.3388 (0.0024) 111.01 (0.17) H2 0.9500 124.50 124.50 C2 - N3 N1 C3 - Distance Angles N1 1.4656 (0.0024) C4 1.5110 (0.0026) 111.06 (0.16) H3A 0.9900 109.42 109.42 H3B 0.9900 109.42 109.42 108.03 C3 - N1 C4 H3A C4 - Distance Angles C9 1.3972 (0.0027) C5 1.4068 (0.0026) 119.18 (0.18) C3 1.5110 (0.0026) 118.36 (0.17) 122.44 (0.17) C4 - C9 C5 C5 - Distance Angles C6 1.3969 (0.0027) C4 1.4068 (0.0026) 118.45 (0.17) C10 1.5192 (0.0026) 120.13 (0.17) 121.41 (0.17) C5 - C6 C4 C6 - Distance Angles C7 1.3865 (0.0027) C5 1.3969 (0.0027) 121.37 (0.18) H6 0.9500 119.32 119.32 C6 - C7 C5 C7 - Distance Angles C8 1.3821 (0.0028) C6 1.3865 (0.0027) 120.19 (0.19) H7 0.9500 119.91 119.91 C7 - C8 C6 C8 - Distance Angles C7 1.3821 (0.0028) C9 1.3834 (0.0029) 119.18 (0.18) H8 0.9500 120.41 120.41 C8 - C7 C9 C9 - Distance Angles C8 1.3834 (0.0029) C4 1.3972 (0.0027) 121.60 (0.18) H9 0.9500 119.20 119.20 C9 - C8 C4 C10 - Distance Angles O1 1.4215 (0.0022) C5 1.5192 (0.0026) 114.32 (0.16) H10A 0.9900 108.68 108.68 H10B 0.9900 108.68 108.68 107.61 C10 - O1 C5 H10A N1 - Distance Angles C2 1.3388 (0.0024) N2 1.3614 (0.0022) 109.52 (0.16) C3 1.4656 (0.0024) 129.42 (0.16) 120.86 (0.14) N1 - C2 N2 N2 - Distance Angles C1 1.3232 (0.0025) N1 1.3614 (0.0022) 102.15 (0.15) N2 - C1 N3 - Distance Angles C2 1.3252 (0.0027) C1 1.3618 (0.0026) 101.95 (0.17) N3 - C2 O1 - Distance Angles C10 1.4215 (0.0022) H1A 0.8400 109.45 O1 - C10 FMAP and GRID set by program FMAP 2 3 13 GRID -5.000 -2 -1 5.000 2 1 R1 = 0.0424 for 1180 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.17 at 0.8748 0.2305 0.2175 [ 0.36 A from H10B ] Deepest hole -0.17 at 0.6236 0.2680 0.1115 [ 0.98 A from C4 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 2173 / 22958 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3748 0.2695 0.7175 1.00000 0.05 0.17 0.36 H10B 1.00 C10 1.47 H10A 1.84 O1 Q2 1 0.1802 0.3025 0.6635 1.00000 0.05 0.16 0.71 C4 0.71 C5 1.88 C6 1.89 C9 Q3 1 0.0520 0.3912 0.4471 1.00000 0.05 0.16 0.66 C8 0.82 C7 1.46 H8 1.59 H7 Q4 1 0.1017 0.0655 0.4494 1.00000 0.05 0.14 0.81 N3 0.86 C2 1.48 H2 1.78 C1 Q5 1 0.3620 0.4627 0.2235 1.00000 0.05 0.14 1.60 H6 1.61 N3 2.02 C2 2.20 H2 Shortest distances between peaks (including symmetry equivalents) 4 5 2.12 2 3 2.38 1 2 2.54 Time profile in seconds ----------------------- 0.08: 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 0.01: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.43: 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 0.42: Structure factors and derivatives 0.20: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.01: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007jmw0003 finished at 11:24:31 Total CPU time: 1.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++