+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007may0011 started at 15:28:09 on 01-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007may0011 in P2(1)/c CELL 0.71073 6.2391 13.8231 6.4019 90.000 96.887 90.000 ZERR 4.00 0.0002 0.0005 0.0002 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 20 20 4 12 V = 548.14 F(000) = 264.0 Mu = 0.13 mm-1 Cell Wt = 508.40 Rho = 1.540 MERG 2 OMIT -3.00 55.00 OMIT 0 0 4 EQIV $1 -x + 2, y + 1/2, -z + 1/2 HTAB O1 N1_$1 DFIX 0.84 0.02 O1 H1O FMAP 2 PLAN 5 SIZE 0.04 0.08 0.08 ACTA BOND $H L.S. 6 TEMP -153.00 WGHT 0.0423 0.2963 FVAR 1.75017 C1 1 1.029481 0.605871 0.236569 11.00000 0.02121 0.01732 = 0.01799 -0.00090 0.00144 0.00101 C2 1 0.903828 0.514721 0.241415 11.00000 0.02153 0.01620 = 0.01804 0.00081 0.00167 0.00291 C3 1 0.693582 0.493831 0.246239 11.00000 0.02080 0.01770 = 0.02036 -0.00065 0.00147 0.00269 AFIX 43 H3 2 0.576153 0.537746 0.243478 11.00000 -1.20000 AFIX 0 C4 1 0.687321 0.391057 0.256409 11.00000 0.02140 0.01882 = 0.01789 -0.00008 0.00137 0.00129 C5 1 0.497708 0.326432 0.267093 11.00000 0.02378 0.02098 = 0.03316 0.00109 0.00349 -0.00166 AFIX 137 H5A 2 0.546487 0.259079 0.280264 11.00000 -1.50000 H5B 2 0.396628 0.333833 0.138604 11.00000 -1.50000 H5C 2 0.425339 0.343895 0.389437 11.00000 -1.50000 AFIX 0 N1 3 0.881646 0.354732 0.257338 11.00000 0.02200 0.01483 = 0.02511 0.00082 0.00278 -0.00176 O1 4 0.902248 0.682286 0.228224 11.00000 0.02108 0.01449 = 0.03782 -0.00049 0.00247 0.00106 O2 4 1.223803 0.607013 0.241013 11.00000 0.02017 0.02160 = 0.02983 -0.00064 0.00283 0.00026 O3 4 1.023898 0.432759 0.247369 11.00000 0.01886 0.01499 = 0.02737 -0.00015 0.00251 0.00094 H1O 2 0.980199 0.735085 0.228395 11.00000 0.05169 HKLF 4 Covalent radii and connectivity table for 2007may0011 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O2 O1 C2 C2 - C3 O3 C1 C3 - C2 C4 C4 - N1 C3 C5 C5 - C4 N1 - C4 O3 O1 - C1 O2 - C1 O3 - C2 N1 Operators for generating equivalent atoms: $1 -x+2, y+1/2, -z+1/2 h k l Fo^2 Sigma Why rejected 0 7 0 8.88 2.07 observed but should be systematically absent 0 13 0 15.78 3.86 observed but should be systematically absent 0 0 5 19.26 3.79 observed but should be systematically absent 0 0 5 18.63 4.26 observed but should be systematically absent 0 0 7 26.45 5.01 observed but should be systematically absent 6963 Reflections read, of which 210 rejected -8 =< h =< 6, -17 =< k =< 17, -7 =< l =< 8, Max. 2-theta = 54.95 5 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 3 4 44.59 1.56 6 8.80 -1 4 4 29.79 1.72 3 13.23 2 Inconsistent equivalents 1247 Unique reflections, of which 0 suppressed R(int) = 0.0430 R(sigma) = 0.0297 Friedel opposites merged Maximum memory for data reduction = 981 / 12501 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 = 1203 / 115911 wR2 = 0.1153 before cycle 1 for 1247 data and 87 / 87 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.203; Restrained GooF = 1.204 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0423 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.74699 0.00614 -0.517 OSF Mean shift/esd = 0.055 Maximum = -0.517 for OSF Max. shift = 0.001 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 2 Maximum vector length = 511 Memory required = 1203 / 115911 wR2 = 0.1153 before cycle 2 for 1247 data and 87 / 87 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.202; Restrained GooF = 1.203 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0423 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.74635 0.00614 -0.105 OSF Mean shift/esd = 0.018 Maximum = -0.105 for OSF Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 3 Maximum vector length = 511 Memory required = 1203 / 115911 wR2 = 0.1153 before cycle 3 for 1247 data and 87 / 87 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.203; Restrained GooF = 1.204 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0423 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.74634 0.00614 -0.001 OSF Mean shift/esd = 0.001 Maximum = -0.004 for y N1 Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 4 Maximum vector length = 511 Memory required = 1203 / 115911 wR2 = 0.1153 before cycle 4 for 1247 data and 87 / 87 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.203; Restrained GooF = 1.204 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0423 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.74634 0.00614 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.003 for U22 C2 Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 5 Maximum vector length = 511 Memory required = 1203 / 115911 wR2 = 0.1153 before cycle 5 for 1247 data and 87 / 87 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.203; Restrained GooF = 1.204 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0423 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.74634 0.00614 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y H1O Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 6 Maximum vector length = 511 Memory required = 1203 / 115911 wR2 = 0.1153 before cycle 6 for 1247 data and 87 / 87 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.203; Restrained GooF = 1.204 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0423 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.74634 0.00614 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O2 Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O 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 H3 0.5762 0.5377 0.2435 43 0.950 0.000 C3 C2 C4 H5A 0.5465 0.2591 0.2802 137 0.980 0.000 C5 C4 H5A H5B 0.3966 0.3338 0.1386 137 0.980 0.000 C5 C4 H5A H5C 0.4253 0.3439 0.3894 137 0.980 0.000 C5 C4 H5A 2007may0011 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 1.02948 0.60587 0.23656 1.00000 0.02117 0.01725 0.01785 -0.00090 0.00141 0.00108 0.01883 0.00264 0.00024 0.00010 0.00022 0.00000 0.00073 0.00075 0.00064 0.00050 0.00054 0.00053 0.00033 C2 0.90384 0.51472 0.24142 1.00000 0.02145 0.01614 0.01791 0.00080 0.00165 0.00295 0.01856 0.00262 0.00024 0.00010 0.00022 0.00000 0.00072 0.00074 0.00064 0.00051 0.00053 0.00053 0.00033 C3 0.69359 0.49382 0.24624 1.00000 0.02071 0.01760 0.02025 -0.00064 0.00145 0.00271 0.01960 0.00262 0.00024 0.00011 0.00022 0.00000 0.00073 0.00070 0.00068 0.00052 0.00055 0.00054 0.00033 H3 0.57615 0.53774 0.24347 1.00000 0.02352 0.00000 0.00000 C4 0.68733 0.39106 0.25641 1.00000 0.02131 0.01879 0.01774 -0.00009 0.00135 0.00129 0.01936 0.00263 0.00024 0.00011 0.00022 0.00000 0.00073 0.00073 0.00066 0.00051 0.00055 0.00055 0.00033 C5 0.49771 0.32643 0.26709 1.00000 0.02368 0.02090 0.03305 0.00109 0.00350 -0.00167 0.02587 0.00295 0.00026 0.00012 0.00027 0.00000 0.00079 0.00076 0.00082 0.00060 0.00064 0.00059 0.00037 H5A 0.54649 0.25908 0.28024 1.00000 0.03880 0.00000 0.00000 H5B 0.39663 0.33384 0.13861 1.00000 0.03880 0.00000 0.00000 H5C 0.42535 0.34388 0.38944 1.00000 0.03880 0.00000 0.00000 N1 0.88164 0.35472 0.25734 1.00000 0.02194 0.01473 0.02501 0.00082 0.00274 -0.00178 0.02056 0.00225 0.00020 0.00009 0.00019 0.00000 0.00064 0.00062 0.00062 0.00047 0.00049 0.00047 0.00031 O1 0.90225 0.68229 0.22822 1.00000 0.02099 0.01438 0.03771 -0.00049 0.00246 0.00105 0.02445 0.00204 0.00018 0.00008 0.00019 0.00000 0.00058 0.00055 0.00064 0.00043 0.00047 0.00040 0.00030 O2 1.22380 0.60701 0.24101 1.00000 0.02005 0.02150 0.02972 -0.00065 0.00279 0.00027 0.02377 0.00200 0.00017 0.00008 0.00018 0.00000 0.00058 0.00057 0.00059 0.00042 0.00044 0.00042 0.00029 O3 1.02390 0.43276 0.24737 1.00000 0.01878 0.01489 0.02727 -0.00015 0.00248 0.00095 0.02033 0.00191 0.00017 0.00007 0.00017 0.00000 0.00055 0.00053 0.00055 0.00040 0.00042 0.00039 0.00028 H1O 0.98003 0.73518 0.22829 1.00000 0.05130 0.03748 0.00358 0.00139 0.00402 0.00000 0.00698 Final Structure Factor Calculation for 2007may0011 in P2(1)/c Total number of l.s. parameters = 87 Maximum vector length = 511 Memory required = 1116 / 22995 wR2 = 0.1153 before cycle 7 for 1247 data and 0 / 87 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.203; Restrained GooF = 1.204 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0423 * P )^2 + 0.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0424 for 1152 Fo > 4sig(Fo) and 0.0461 for all 1247 data wR2 = 0.1153, GooF = S = 1.203, Restrained GooF = 1.204 for all data Occupancy sum of asymmetric unit = 9.00 for non-hydrogen and 5.00 for hydrogen atoms Principal mean square atomic displacements U 0.0219 0.0180 0.0165 C1 0.0229 0.0182 0.0146 C2 0.0230 0.0198 0.0160 C3 0.0222 0.0183 0.0176 C4 0.0332 0.0245 0.0200 C5 0.0251 0.0223 0.0142 N1 0.0380 0.0211 0.0142 O1 0.0298 0.0215 0.0200 O2 0.0274 0.0190 0.0147 O3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.029 0.045 0.063 0.082 0.108 0.142 0.190 0.275 1.000 Number in group 127. 124. 125. 125. 124. 124. 129. 119. 125. 125. GooF 1.820 1.612 1.035 0.905 1.114 0.884 1.103 1.014 1.041 1.127 K 4.820 1.443 0.982 1.008 1.003 1.001 1.006 1.011 1.005 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.98 1.04 1.15 1.32 1.64 inf Number in group 127. 127. 121. 124. 130. 120. 129. 120. 125. 124. GooF 1.074 0.963 1.115 1.056 1.097 0.964 1.509 1.182 1.556 1.327 K 0.997 1.020 1.035 1.010 1.005 1.003 0.996 0.996 1.037 0.998 R1 0.080 0.079 0.063 0.063 0.050 0.037 0.042 0.040 0.040 0.031 Recommended weighting scheme: WGHT 0.0422 0.2989 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) -2 3 4 18.32 0.78 7.38 0.015 1.42 1 8 4 24.52 0.20 7.27 0.008 1.13 -3 8 4 15.42 0.76 6.28 0.015 1.06 2 2 4 11.89 0.50 6.22 0.012 1.32 -1 10 4 14.30 0.00 5.49 0.000 1.04 -6 0 4 6.42 0.54 3.84 0.013 0.92 0 7 4 13.68 2.30 3.41 0.026 1.24 2 4 1 16.69 27.18 3.15 0.090 2.11 -6 6 4 40.41 21.66 3.11 0.081 0.85 -4 2 4 25.26 15.40 3.10 0.068 1.17 -3 12 3 2.90 0.45 3.01 0.012 0.93 -4 7 1 182.06 226.80 3.00 0.261 1.22 1 8 0 79.32 60.66 2.91 0.135 1.66 -2 7 4 60.80 43.32 2.88 0.114 1.19 3 8 0 8.74 15.68 2.84 0.069 1.33 6 0 0 5.29 1.45 2.76 0.021 1.03 -2 1 4 2.20 0.26 2.70 0.009 1.48 0 6 0 435.39 366.41 2.70 0.331 2.30 -2 4 1 95.78 118.76 2.60 0.189 2.23 5 11 0 85.50 65.93 2.54 0.141 0.88 -1 15 4 4.68 1.31 2.54 0.020 0.80 7 0 0 10.30 4.55 2.52 0.037 0.88 7 5 0 -0.29 1.84 2.49 0.023 0.84 -5 14 1 2.72 7.03 2.47 0.046 0.77 -3 12 4 2.86 0.60 2.47 0.013 0.87 1 13 4 1.65 0.03 2.43 0.003 0.87 3 3 0 258.10 219.36 2.43 0.256 1.88 1 10 4 2.22 0.31 2.41 0.010 1.02 3 7 4 2.95 0.14 2.41 0.007 1.02 2 3 0 42.35 54.82 2.39 0.128 2.57 -6 1 2 1.23 0.00 2.37 0.000 1.02 0 14 1 1.78 0.27 2.36 0.009 0.98 1 2 3 87.19 71.14 2.35 0.146 1.86 -3 5 7 3.96 7.98 2.31 0.049 0.83 1 10 0 4.87 2.22 2.21 0.026 1.35 -3 12 1 8.21 4.64 2.20 0.037 1.00 2 8 1 1.74 0.32 2.20 0.010 1.45 0 16 0 105.51 78.97 2.15 0.154 0.86 2 0 0 839.45 963.90 2.15 0.537 3.10 -4 12 1 5.29 2.48 2.12 0.027 0.92 -1 2 1 850.83 960.63 2.12 0.536 3.90 2 8 0 1108.57 984.43 2.09 0.543 1.51 -3 10 2 88.80 106.21 2.07 0.178 1.10 4 12 1 10.35 6.39 2.05 0.044 0.91 3 2 0 988.48 880.37 2.04 0.513 1.98 -1 15 2 2.60 0.65 2.03 0.014 0.88 -1 1 1 621.65 698.95 2.01 0.457 4.47 1 15 0 0.97 0.02 2.01 0.003 0.91 3 0 4 13.09 8.22 2.00 0.050 1.19 6 2 4 7.18 3.61 2.00 0.033 0.82 Bond lengths and angles C1 - Distance Angles O2 1.2094 (0.0018) O1 1.3186 (0.0018) 125.97 (0.14) C2 1.4862 (0.0020) 122.71 (0.13) 111.32 (0.13) C1 - O2 O1 C2 - Distance Angles C3 1.3472 (0.0021) O3 1.3562 (0.0017) 110.87 (0.13) C1 1.4862 (0.0020) 134.41 (0.14) 114.70 (0.13) C2 - C3 O3 C3 - Distance Angles C2 1.3472 (0.0021) C4 1.4227 (0.0021) 104.32 (0.13) H3 0.9500 127.84 127.84 C3 - C2 C4 C4 - Distance Angles N1 1.3116 (0.0019) C3 1.4227 (0.0021) 110.62 (0.13) C5 1.4906 (0.0021) 120.57 (0.13) 128.81 (0.14) C4 - N1 C3 C5 - Distance Angles C4 1.4906 (0.0021) H5A 0.9800 109.47 H5B 0.9800 109.47 109.47 H5C 0.9800 109.47 109.47 109.47 C5 - C4 H5A H5B N1 - Distance Angles C4 1.3116 (0.0019) O3 1.4032 (0.0016) 107.14 (0.12) N1 - C4 O1 - Distance Angles C1 1.3186 (0.0018) H1O 0.8775 (0.0163) 109.71 (1.62) O1 - C1 O2 - Distance Angles C1 1.2094 (0.0018) O2 - O3 - Distance Angles C2 1.3562 (0.0017) N1 1.4032 (0.0016) 107.05 (0.11) O3 - C2 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.878(16) 1.861(17) 2.7346(17) 173(2) O1-H1O...N1_$1 FMAP and GRID set by program FMAP 2 3 11 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0461 for 1247 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.35 at 0.9671 0.5611 0.2345 [ 0.73 A from C1 ] Deepest hole -0.19 at 0.9845 0.1099 0.1354 [ 0.84 A from C1 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 1310 / 13529 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9671 0.5611 0.2345 1.00000 0.05 0.35 0.73 C1 0.76 C2 1.72 O2 1.72 O1 Q2 1 0.6779 0.4405 0.2752 1.00000 0.05 0.26 0.70 C4 0.77 C3 1.49 H3 1.75 N1 Q3 1 0.8202 0.5125 0.2978 1.00000 0.05 0.22 0.67 C2 0.86 C3 1.56 H3 1.74 O3 Q4 1 0.7682 0.3792 0.1960 1.00000 0.05 0.19 0.69 C4 0.84 N1 1.69 C3 1.75 O3 Q5 1 1.0710 0.3345 0.2379 1.00000 0.05 0.18 1.23 N1 1.39 O3 1.43 H1O 2.12 O1 Shortest distances between peaks (including symmetry equivalents) 2 4 1.17 1 3 1.24 2 3 1.33 3 4 1.97 4 5 1.97 1 2 2.49 1 4 2.80 2 5 2.89 3 5 2.96 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.01: Fit rigid groups 0.00: Interpret restraints etc. 0.01: Generate connectivity array 0.02: 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. 0.64: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.27: Structure factors and derivatives 0.45: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.10: Solve l.s. equations 0.00: Generate HTAB table 0.04: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007may0011 finished at 15:28:19 Total CPU time: 1.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++