+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 16:23:43 on 08-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02src629 in P-1 New: Ccca CELL 0.71073 13.0370 19.1366 10.0187 90.000 90.000 90.000 ZERR 8.00 0.0005 0.0006 0.0004 0.000 0.000 0.000 LATT 7 SYMM - X, 1/2 - Y, Z SYMM X, 1/2 - Y, 1/2 - Z SYMM - X, Y, 1/2 - Z SFAC C 2.31000 20.84392 1.02000 10.20751 1.58860 0.56870 = 0.86500 51.65125 0.21560 0.003 0.002 11.500 0.680 12.010 SFAC H 0.49300 10.51091 0.32291 26.12573 0.14019 3.14236 = 0.04081 57.79977 0.00304 0.000 0.000 0.624 0.350 1.000 SFAC N 12.21261 0.00570 3.13220 9.89331 2.01250 28.99754 = 1.16630 0.58260 -11.52901 0.006 0.003 19.600 0.680 14.010 SFAC O 3.04850 13.27711 2.28680 5.70111 1.54630 0.32390 = 0.86700 32.90894 0.25080 0.011 0.006 32.500 0.680 16.000 UNIT 80 208 16 8 V = 2499.50 F(000) = 863.8 Mu = 0.06 mm-1 Cell Wt = 1520.96 Rho = 1.010 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H TEMP -153 CONF WGHT 0.04350 2.45710 L.S. 5 FVAR 0.20052 N1 3 0.381802 0.194484 0.019783 11.00000 0.01282 0.01523 = 0.02057 0.00174 -0.00232 -0.00174 AFIX 3 H1N 2 0.354062 0.215594 -0.047517 11.00000 -1.20000 AFIX 0 C1 1 0.354602 0.119004 0.006773 11.00000 0.01604 0.01380 = 0.01348 -0.00117 -0.00057 -0.00246 C2 1 0.397642 0.086234 -0.120797 11.00000 0.03010 0.02357 = 0.02189 -0.00498 0.00189 -0.00169 AFIX 137 H2A 2 0.376434 0.113339 -0.196557 11.00000 -1.50000 H2B 2 0.372305 0.039356 -0.129579 11.00000 -1.50000 H2C 2 0.471188 0.085448 -0.116286 11.00000 -1.50000 AFIX 0 C3 1 0.238069 0.116251 0.003697 11.00000 0.01813 0.01970 = 0.02543 0.00247 -0.00249 -0.00381 AFIX 137 H3A 2 0.211259 0.135418 0.085086 11.00000 -1.50000 H3B 2 0.216069 0.068605 -0.005242 11.00000 -1.50000 H3C 2 0.213302 0.142990 -0.070696 11.00000 -1.50000 AFIX 0 C4 1 0.394785 0.079436 0.128162 11.00000 0.03033 0.02052 = 0.02211 0.00230 -0.00525 -0.00019 AFIX 137 H4A 2 0.468385 0.078455 0.125803 11.00000 -1.50000 H4B 2 0.368856 0.032488 0.126925 11.00000 -1.50000 H4C 2 0.372402 0.102463 0.208155 11.00000 -1.50000 AFIX 0 C5 1 0.491942 0.210886 0.019561 11.00000 0.01512 0.01899 = 0.03266 0.00082 -0.00063 -0.00065 AFIX 23 H5A 2 0.523871 0.190671 -0.058904 11.00000 -1.20000 H5B 2 0.524064 0.190652 0.097875 11.00000 -1.20000 AFIX 0 O1 4 0.264161 0.250000 0.250000 10.50000 0.02220 0.02784 = 0.02266 -0.00468 0.00000 0.00000 AFIX 3 H3O 2 0.303591 0.233270 0.179770 11.00000 -1.50000 AFIX 0 HKLF 4 1.0 0.00 -1.00 1.00 0.00 -1.00 -1.00 1.00 0.00 0.00 Covalent radii and connectivity table for 02src629 in P-1 New: Ccca C 0.680 H 0.350 N 0.680 O 0.680 N1 - C5 C1 C1 - N1 C3 C4 C2 C2 - C1 C3 - C1 C4 - C1 C5 - N1 C5_$1 O1 - no bonds found Operators for generating equivalent atoms: $1 -x+1, -y+1/2, z h k l Fo^2 Sigma Why rejected 6 0 3 6.02 1.00 observed but should be systematically absent 1 23 0 195.62 46.16 observed but should be systematically absent 15547 Reflections read, of which 1123 rejected -16 =< h =< 16, -24 =< k =< 24, -12 =< l =< 12, Max. 2-theta = 54.87 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 12 12 1 4.32 0.80 9 4.50 0 14 2 9.60 0.86 8 4.55 5 21 3 1.93 1.09 8 6.19 8 0 4 163.30 0.98 5 43.83 7 15 4 3.26 0.52 12 5.92 6 20 4 17.01 1.34 7 12.78 1 15 8 7.65 0.85 9 4.57 1 17 8 3.30 1.11 6 14.47 0 6 10 1.08 0.74 6 7.56 3 3 11 8.94 0.81 8 5.73 10 Inconsistent equivalents 1421 Unique reflections, of which 0 suppressed R(int) = 0.1033 R(sigma) = 0.0488 Friedel opposites merged Maximum memory for data reduction = 1222 / 16623 Special position constraints for O1 y = 0.2500 z = 0.2500 U13 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 1447 / 89523 wR2 = 0.1272 before cycle 1 for 1421 data and 63 / 63 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0435 * P )^2 + 2.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.20014 0.00068 -0.560 OSF Mean shift/su = 0.603 Maximum = -1.734 for U33 C4 Max. shift = 0.006 A for H2B Max. dU =-0.001 for C4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1447 / 89523 wR2 = 0.1243 before cycle 2 for 1421 data and 63 / 63 parameters GooF = S = 1.019; Restrained GooF = 1.019 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0435 * P )^2 + 2.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19978 0.00067 -0.530 OSF Mean shift/su = 0.243 Maximum = -0.740 for U11 C3 Max. shift = 0.002 A for H4A Max. dU = 0.000 for C4 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1447 / 89523 wR2 = 0.1240 before cycle 3 for 1421 data and 63 / 63 parameters GooF = S = 1.017; Restrained GooF = 1.017 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0435 * P )^2 + 2.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19974 0.00066 -0.068 OSF Mean shift/su = 0.018 Maximum = -0.072 for U11 C3 Max. shift = 0.000 A for H4A Max. dU = 0.000 for C4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1447 / 89523 wR2 = 0.1240 before cycle 4 for 1421 data and 63 / 63 parameters GooF = S = 1.017; Restrained GooF = 1.017 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0435 * P )^2 + 2.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19974 0.00066 -0.005 OSF Mean shift/su = 0.003 Maximum = -0.010 for U22 C1 Max. shift = 0.000 A for H2B Max. dU = 0.000 for C1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1447 / 89523 wR2 = 0.1240 before cycle 5 for 1421 data and 63 / 63 parameters GooF = S = 1.017; Restrained GooF = 1.017 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0435 * P )^2 + 2.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19974 0.00066 -0.001 OSF Mean shift/su = 0.000 Maximum = -0.001 for x C3 Max. shift = 0.000 A for H4A Max. dU = 0.000 for C4 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 6 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.3762 0.1140 -0.1985 137 0.980 0.000 C2 C1 H2A H2B 0.3714 0.0384 -0.1303 137 0.980 0.000 C2 C1 H2A H2C 0.4727 0.0851 -0.1165 137 0.980 0.000 C2 C1 H2A H3A 0.2103 0.1358 0.0865 137 0.980 0.000 C3 C1 H3A H3B 0.2154 0.0676 -0.0056 137 0.980 0.000 C3 C1 H3A H3C 0.2125 0.1435 -0.0725 137 0.980 0.000 C3 C1 H3A H4A 0.4699 0.0786 0.1263 137 0.980 0.000 C4 C1 H4A H4B 0.3685 0.0315 0.1270 137 0.980 0.000 C4 C1 H4A H4C 0.3717 0.1029 0.2100 137 0.980 0.000 C4 C1 H4A H5A 0.5246 0.1901 -0.0606 23 0.990 0.000 C5 N1 C5_$1 H5B 0.5248 0.1901 0.0994 23 0.990 0.000 C5 N1 C5_$1 02src629 in P-1 New: Ccca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq N1 0.38167 0.19452 0.01963 1.00000 0.01228 0.01492 0.01978 0.00097 -0.00203 -0.00147 0.01566 0.00200 0.00009 0.00006 0.00012 0.00000 0.00061 0.00061 0.00066 0.00052 0.00053 0.00048 0.00032 H1N 0.35393 0.21563 -0.04767 1.00000 0.01879 0.00000 0.00000 C1 0.35465 0.11906 0.00668 1.00000 0.01547 0.01399 0.01439 -0.00140 -0.00053 -0.00230 0.01462 0.00247 0.00011 0.00007 0.00015 0.00000 0.00067 0.00067 0.00069 0.00060 0.00062 0.00057 0.00033 C2 0.39761 0.08616 -0.12116 1.00000 0.02941 0.02409 0.02032 -0.00579 0.00222 -0.00231 0.02461 0.00278 0.00013 0.00009 0.00016 0.00000 0.00092 0.00093 0.00081 0.00070 0.00074 0.00075 0.00041 H2A 0.37625 0.11396 -0.19846 1.00000 0.03691 0.00000 0.00000 H2B 0.37137 0.03841 -0.13028 1.00000 0.03691 0.00000 0.00000 H2C 0.47268 0.08507 -0.11646 1.00000 0.03691 0.00000 0.00000 C3 0.23778 0.11623 0.00350 1.00000 0.01622 0.02056 0.02536 0.00188 -0.00276 -0.00391 0.02071 0.00266 0.00011 0.00008 0.00017 0.00000 0.00075 0.00077 0.00078 0.00072 0.00071 0.00062 0.00036 H3A 0.21035 0.13583 0.08653 1.00000 0.03107 0.00000 0.00000 H3B 0.21539 0.06758 -0.00555 1.00000 0.03107 0.00000 0.00000 H3C 0.21250 0.14348 -0.07251 1.00000 0.03107 0.00000 0.00000 C4 0.39480 0.07944 0.12844 1.00000 0.02899 0.02033 0.02010 0.00326 -0.00625 -0.00051 0.02314 0.00276 0.00013 0.00008 0.00016 0.00000 0.00089 0.00089 0.00078 0.00068 0.00073 0.00072 0.00039 H4A 0.46994 0.07857 0.12633 1.00000 0.03471 0.00000 0.00000 H4B 0.36852 0.03146 0.12702 1.00000 0.03471 0.00000 0.00000 H4C 0.37167 0.10288 0.21004 1.00000 0.03471 0.00000 0.00000 C5 0.49205 0.21073 0.01947 1.00000 0.01409 0.01751 0.03364 0.00065 -0.00046 -0.00123 0.02175 0.00260 0.00012 0.00008 0.00017 0.00000 0.00076 0.00080 0.00093 0.00069 0.00072 0.00063 0.00039 H5A 0.52464 0.19010 -0.06061 1.00000 0.02610 0.00000 0.00000 H5B 0.52478 0.19009 0.09944 1.00000 0.02610 0.00000 0.00000 O1 0.26427 0.25000 0.25000 0.50000 0.02169 0.02721 0.02216 -0.00443 0.00000 0.00000 0.02369 0.00147 0.00011 0.00000 0.00000 0.00000 0.00083 0.00085 0.00081 0.00072 0.00000 0.00000 0.00040 H3O 0.30370 0.23327 0.17977 1.00000 0.03553 0.00000 0.00000 Final Structure Factor Calculation for 02src629 in P-1 New: Ccca Total number of l.s. parameters = 63 Maximum vector length = 511 Memory required = 1384 / 22995 wR2 = 0.1240 before cycle 6 for 1421 data and 0 / 63 parameters GooF = S = 1.017; Restrained GooF = 1.017 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0435 * P )^2 + 2.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0561 for 1022 Fo > 4sig(Fo) and 0.0907 for all 1421 data wR2 = 0.1240, GooF = S = 1.017, Restrained GooF = 1.017 for all data Occupancy sum of asymmetric unit = 6.50 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0206 0.0150 0.0114 N1 0.0172 0.0151 0.0116 C1 0.0321 0.0256 0.0161 C2 0.0275 0.0209 0.0137 C3 0.0325 0.0215 0.0154 C4 0.0337 0.0179 0.0137 C5 0.0298 0.0217 0.0196 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.014 0.021 0.028 0.036 0.044 0.057 0.079 0.122 1.000 Number in group 164. 123. 151. 132. 156. 126. 142. 142. 144. 141. GooF 1.058 1.093 1.006 1.087 0.992 0.941 0.938 1.025 1.056 0.963 K 10.672 2.337 1.545 1.256 1.123 1.014 1.039 1.014 1.001 0.984 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.33 1.65 inf Number in group 147. 142. 139. 140. 142. 146. 139. 142. 142. 142. GooF 0.922 0.990 0.927 0.950 0.961 1.026 0.998 1.015 1.162 1.184 K 1.153 1.168 1.135 1.048 0.992 0.978 0.993 1.000 1.014 0.976 R1 0.193 0.186 0.179 0.147 0.109 0.089 0.059 0.051 0.058 0.032 Recommended weighting scheme: WGHT 0.0428 2.0285 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) 12 4 0 92.21 7.89 4.05 0.009 1.06 2 6 5 113.01 53.45 3.70 0.025 1.64 4 6 1 205.99 135.49 3.03 0.039 2.22 12 0 4 100.82 179.83 2.99 0.045 1.00 2 18 1 54.05 140.99 2.80 0.040 1.04 2 12 1 2579.97 2214.34 2.78 0.158 1.53 4 20 5 -13.97 42.78 2.69 0.022 0.83 4 2 9 78.39 140.34 2.65 0.040 1.05 4 0 2 807.83 664.97 2.64 0.087 2.73 10 2 1 497.41 385.40 2.62 0.066 1.28 12 4 4 27.19 0.38 2.56 0.002 0.98 6 10 5 548.20 693.98 2.55 0.088 1.17 1 9 1 112.49 67.70 2.53 0.028 2.05 6 10 1 40.49 12.73 2.49 0.012 1.42 5 1 5 54.97 22.43 2.47 0.016 1.58 0 22 4 3238.58 2760.38 2.46 0.176 0.82 3 7 2 221.64 162.44 2.46 0.043 2.10 12 6 8 229.66 113.87 2.46 0.036 0.79 4 14 7 148.95 95.94 2.46 0.033 0.95 3 3 12 197.08 107.73 2.45 0.035 0.81 6 8 2 248.40 183.09 2.45 0.045 1.53 5 17 5 47.81 1.54 2.44 0.004 0.92 2 8 7 917.77 1086.16 2.43 0.111 1.21 7 11 8 269.63 177.06 2.40 0.045 0.89 7 11 2 55.34 10.45 2.39 0.011 1.23 6 2 8 76.61 32.36 2.39 0.019 1.08 7 11 5 691.17 830.50 2.38 0.097 1.07 4 4 4 485.51 393.22 2.37 0.067 1.83 3 11 9 44.39 8.28 2.36 0.010 0.92 1 7 5 53.00 18.74 2.35 0.015 1.60 0 0 2 78866.06 88813.72 2.33 1.000 5.01 4 16 1 634.16 520.07 2.31 0.077 1.12 7 1 4 24.08 3.28 2.30 0.006 1.49 2 4 8 117.12 67.71 2.29 0.028 1.19 3 17 7 52.83 112.48 2.27 0.036 0.87 11 11 6 146.05 54.14 2.27 0.025 0.84 4 4 2 1857.59 2118.14 2.25 0.154 2.37 4 0 6 1180.41 1374.71 2.25 0.124 1.49 1 3 4 507.54 418.33 2.24 0.069 2.29 5 1 4 46.59 19.80 2.23 0.015 1.80 4 6 3 755.48 640.76 2.21 0.085 1.88 10 10 2 30.91 2.28 2.20 0.005 1.05 0 2 8 28.94 3.21 2.20 0.006 1.24 6 4 1 100.65 66.17 2.17 0.027 1.94 9 1 3 26.13 5.54 2.17 0.008 1.33 3 19 5 34.78 87.45 2.17 0.031 0.88 0 2 2 5167.13 5770.36 2.16 0.255 4.44 3 17 3 39.35 83.35 2.15 0.031 1.04 3 11 11 144.00 28.22 2.15 0.018 0.79 6 2 11 253.95 37.94 2.13 0.021 0.84 Bond lengths and angles N1 - Distance Angles C5 1.4721 (0.0019) C1 1.4919 (0.0017) 115.77 (0.11) H1N 0.8652 108.02 106.59 N1 - C5 C1 C1 - Distance Angles N1 1.4919 (0.0017) C3 1.5250 (0.0020) 105.79 (0.11) C4 1.5287 (0.0021) 109.26 (0.12) 109.95 (0.13) C2 1.5332 (0.0021) 112.57 (0.13) 109.45 (0.13) 109.75 (0.13) C1 - N1 C3 C4 C2 - Distance Angles C1 1.5332 (0.0021) H2A 0.9800 109.47 H2B 0.9800 109.47 109.47 H2C 0.9800 109.47 109.47 109.47 C2 - C1 H2A H2B C3 - Distance Angles C1 1.5250 (0.0020) H3A 0.9800 109.47 H3B 0.9800 109.47 109.47 H3C 0.9800 109.47 109.47 109.47 C3 - C1 H3A H3B C4 - Distance Angles C1 1.5287 (0.0021) H4A 0.9800 109.47 H4B 0.9800 109.47 109.47 H4C 0.9800 109.47 109.47 109.47 C4 - C1 H4A H4B C5 - Distance Angles N1 1.4721 (0.0019) C5_$1 1.5172 (0.0029) 110.02 (0.16) H5A 0.9900 109.66 109.66 H5B 0.9900 109.66 109.66 108.16 C5 - N1 C5_$1 H5A O1 - Distance Angles H3O 0.9283 O1 - Selected torsion angles -177.68 ( 0.13) C5 - N1 - C1 - C3 64.00 ( 0.16) C5 - N1 - C1 - C4 -58.19 ( 0.17) C5 - N1 - C1 - C2 174.45 ( 0.09) C1 - N1 - C5 - C5_$1 FMAP and GRID set by program FMAP 2 3 14 GRID -2.273 -2 -1 2.273 2 1 R1 = 0.0906 for 1421 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.18 at 0.5000 0.2500 0.0134 [ 0.76 A from C5 ] Deepest hole -0.20 at 0.9849 0.1764 0.0332 [ 0.64 A from H5A ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2065 / 17587 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5000 0.2500 0.0134 0.50000 0.05 0.18 0.76 C5 1.40 H5A 1.47 H5B 1.87 N1 Q2 1 0.3014 0.1142 0.0153 1.00000 0.05 0.17 0.71 C1 0.84 C3 1.45 H3A 1.45 H3B Q3 1 0.3313 0.1886 0.3023 1.00000 0.05 0.16 1.54 H3O 1.55 H3O 1.56 O1 1.63 H3C Q4 1 0.4387 0.2006 0.0192 1.00000 0.05 0.15 0.72 C5 0.75 N1 1.32 H1N 1.39 H5A Q5 1 0.3724 0.1004 0.0585 1.00000 0.05 0.15 0.67 C1 0.86 C4 1.49 H4B 1.50 H4A Q6 1 0.2584 0.1264 -0.1620 1.00000 0.05 0.14 1.13 H3C 1.60 H2A 1.69 C3 2.01 H3B Q7 1 0.5514 0.1844 -0.0033 1.00000 0.05 0.14 0.68 H5A 0.95 C5 1.09 H5B 2.10 C5 Q8 1 0.3137 0.0661 0.2439 1.00000 0.05 0.14 1.09 H4C 1.52 H4B 1.59 C4 2.37 H4A Q9 1 0.3055 0.1187 -0.2228 1.00000 0.05 0.13 0.96 H2A 1.69 C2 1.95 H3A 1.99 H2B Q10 1 0.2977 0.0938 -0.2473 1.00000 0.05 0.13 1.20 H2A 1.82 C2 1.85 H2B 1.85 H3A Q11 1 0.3670 0.0981 -0.0607 1.00000 0.05 0.13 0.76 C2 0.80 C1 1.34 H2B 1.42 H2A Q12 1 0.3667 0.1576 0.0222 1.00000 0.05 0.12 0.73 N1 0.77 C1 1.32 H1N 1.87 C3 Q13 1 0.5355 0.2139 0.2070 1.00000 0.05 0.12 1.18 H5B 1.96 C5 2.14 H5B 2.27 H5B Q14 1 0.2345 0.1882 -0.1623 1.00000 0.05 0.12 1.27 H3C 1.47 O1 1.59 H3O 1.87 H3O Q15 1 0.5946 0.2022 0.2319 1.00000 0.05 0.12 1.63 H5B 1.70 H3O 1.89 H3O 2.04 H4C Q16 1 0.4014 0.1921 -0.2204 1.00000 0.05 0.12 1.55 H2A 1.89 H1N 2.26 C2 2.27 H5A Q17 1 0.5000 0.0478 0.2500 0.50000 0.05 0.12 1.43 H4A 1.93 C4 2.02 H4C 2.13 H4B Q18 1 0.3071 0.0409 -0.2462 1.00000 0.05 0.11 1.43 H2B 1.73 H2A 1.93 C2 2.04 H4B Q19 1 0.3561 0.2999 0.1548 1.00000 0.05 0.11 1.47 H3O 1.63 H3C 1.66 H5B 1.80 O1 Q20 1 0.3788 0.2257 0.0973 1.00000 0.05 0.11 0.98 N1 1.29 H3O 1.50 H1N 1.69 C5 Shortest distances between peaks (including symmetry equivalents) 9 10 0.54 3 19 0.58 13 15 0.84 6 9 0.88 3 14 0.93 15 19 1.01 10 18 1.02 2 5 1.05 3 15 1.06 5 12 1.16 6 10 1.17 2 11 1.19 2 12 1.19 5 11 1.20 4 20 1.20 14 19 1.20 6 14 1.22 1 4 1.24 4 12 1.25 13 13 1.27 11 12 1.41 1 7 1.43 9 18 1.51 12 20 1.51 4 7 1.52 13 19 1.53 8 10 1.55 19 20 1.56 13 13 1.63 8 18 1.65 13 13 1.66 3 6 1.71 9 14 1.73 6 8 1.76 15 20 1.80 3 13 1.80 13 15 1.82 6 11 1.82 1 20 1.85 9 11 1.85 15 15 1.86 2 6 1.88 8 9 1.88 9 16 1.88 13 15 1.88 6 18 1.95 13 20 1.95 15 20 1.96 14 15 1.97 7 19 2.01 3 20 2.02 8 18 2.05 6 19 2.05 10 11 2.08 1 13 2.11 5 8 2.11 4 5 2.14 10 14 2.16 18 18 2.16 7 13 2.19 7 20 2.19 4 7 2.22 3 9 2.24 14 16 2.25 3 20 2.26 13 20 2.27 4 13 2.28 15 19 2.28 16 16 2.29 11 18 2.29 14 20 2.31 4 11 2.31 6 16 2.32 13 20 2.33 10 16 2.33 13 15 2.35 2 9 2.39 6 12 2.40 3 15 2.41 3 8 2.43 5 20 2.43 2 14 2.44 2 4 2.44 7 15 2.45 11 16 2.45 4 16 2.45 8 17 2.45 2 8 2.47 7 12 2.47 4 4 2.48 1 12 2.48 15 15 2.49 2 20 2.50 4 13 2.51 3 10 2.52 3 7 2.53 4 15 2.53 1 19 2.54 19 20 2.55 12 16 2.56 4 19 2.57 3 3 2.57 13 19 2.57 7 20 2.59 12 14 2.59 8 14 2.59 3 19 2.61 16 16 2.64 11 14 2.64 12 15 2.66 2 10 2.66 1 15 2.67 6 15 2.68 13 14 2.68 9 12 2.69 19 19 2.70 9 19 2.71 5 6 2.71 3 13 2.72 5 17 2.73 13 19 2.73 2 10 2.74 4 13 2.78 8 19 2.81 7 16 2.84 7 7 2.85 4 15 2.86 3 13 2.87 3 14 2.87 4 20 2.88 8 15 2.88 1 16 2.89 5 15 2.90 5 7 2.90 3 12 2.91 7 14 2.91 13 19 2.91 8 12 2.91 11 20 2.91 14 20 2.91 10 18 2.92 1 13 2.92 7 16 2.93 4 15 2.94 14 14 2.95 5 10 2.95 5 9 2.97 2 18 2.97 7 11 2.97 2 9 2.97 14 15 2.97 1 15 2.98 Time profile in seconds ----------------------- 0.00: 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. 0.69: 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 0.23: Structure factors and derivatives 0.06: 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 0.02: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.02: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 16:23:44 Total CPU time: 1.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++