+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0020pna21 started at 16:02:38 on 07-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0020pna21 in Pna2(1) CELL 0.71073 23.7560 7.1036 5.6944 90.000 90.000 90.000 ZERR 4.00 0.0012 0.0004 0.0002 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H N O S UNIT 32 52 4 12 4 V = 960.95 F(000) = 432.0 Mu = 0.31 mm-1 Cell Wt = 813.02 Rho = 1.405 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB N22 O1B HTAB N22 S1 EQIV_$1 -x+1/2, y+1/2, z+1/2 HTAB N22 O1B_$1 HTAB N22 O1A_$1 HTAB N22 S1_$1 EQIV_$2 x, y+1, z HTAB N22 O1A_$2 HTAB N22 S1_$2 FMAP 2 PLAN 10 SIZE 0.10 0.08 0.04 ACTA BOND $H WGHT 0.03470 0.49150 L.S. 4 TEMP -153.00 FVAR 0.55380 MOLE 1 C1 1 0.400308 0.721403 0.505292 11.00000 0.01442 0.01420 = 0.01996 0.00166 -0.00148 0.00209 C2 1 0.441759 0.669721 0.347390 11.00000 0.02081 0.01688 = 0.02218 -0.00302 -0.00079 -0.00398 AFIX 43 H2 2 0.431880 0.620103 0.198049 11.00000 -1.20000 AFIX 0 C3 1 0.498213 0.691118 0.409422 11.00000 0.01894 0.02037 = 0.02269 0.00002 0.00227 0.00109 AFIX 43 H3 2 0.526730 0.652374 0.302918 11.00000 -1.20000 AFIX 0 C4 1 0.513292 0.767815 0.623436 11.00000 0.01498 0.01693 = 0.02554 0.00462 -0.00289 -0.00228 C5 1 0.470659 0.817342 0.780412 11.00000 0.02391 0.01808 = 0.01818 -0.00024 -0.00485 -0.00061 AFIX 43 H5 2 0.480421 0.868273 0.929197 11.00000 -1.20000 AFIX 0 C6 1 0.414407 0.793721 0.723599 11.00000 0.02086 0.01595 = 0.01882 0.00144 0.00166 0.00269 AFIX 43 H6 2 0.385845 0.826672 0.832888 11.00000 -1.20000 AFIX 0 C7 1 0.574252 0.800431 0.690182 11.00000 0.01931 0.02954 = 0.03335 0.00287 -0.00708 -0.00262 AFIX 137 H7A 2 0.585414 0.928066 0.644371 11.00000 -1.50000 H7B 2 0.598133 0.708653 0.609039 11.00000 -1.50000 H7C 2 0.578641 0.785672 0.860311 11.00000 -1.50000 AFIX 0 O1A 4 0.321991 0.538004 0.278040 11.00000 0.01773 0.02123 = 0.03083 -0.00523 -0.00303 -0.00186 O1B 4 0.318144 0.876082 0.274075 11.00000 0.01896 0.01750 = 0.03527 0.00351 -0.00714 0.00151 O1C 4 0.295555 0.708102 0.633487 11.00000 0.01655 0.04527 = 0.02007 0.00074 0.00471 -0.00142 S1 5 0.328298 0.708808 0.418722 11.00000 0.01353 0.01880 = 0.01963 -0.00059 -0.00014 -0.00048 MOLE 2 C21 1 0.315193 1.212151 0.720271 11.00000 0.01811 0.03021 = 0.02524 0.00009 -0.00586 0.00219 AFIX 137 H22A 2 0.355193 1.201308 0.680430 11.00000 -1.50000 H22B 2 0.304156 1.106048 0.820166 11.00000 -1.50000 H22C 2 0.308701 1.330470 0.804528 11.00000 -1.50000 AFIX 0 N22 3 0.281064 1.210066 0.501118 11.00000 0.01763 0.02152 = 0.02066 0.00024 0.00061 0.00317 AFIX 137 H21A 2 0.243831 1.213355 0.538456 11.00000 0.04733 H21B 2 0.288609 1.103243 0.418723 11.00000 0.06845 H21C 2 0.289883 1.312327 0.412174 11.00000 0.03102 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0020pna21 in Pna2(1) C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - C2 C6 S1 C2 - C1 C3 C3 - C4 C2 C4 - C3 C5 C7 C5 - C6 C4 C6 - C5 C1 C7 - C4 O1A - S1 O1B - S1 O1C - S1 S1 - O1C O1A O1B C1 C21 - N22 N22 - C21 Operators for generating equivalent atoms: $1 -x+1/2, y+1/2, z+1/2 $2 x, y+1, z Floating origin restraints generated 8277 Reflections read, of which 488 rejected -30 =< h =< 21, -9 =< k =< 9, -6 =< l =< 7, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 18 2 -4 74.85 8.77 3 44.31 21 3 -3 70.40 15.10 2 162.55 2 Inconsistent equivalents 2114 Unique reflections, of which 0 suppressed R(int) = 0.0812 R(sigma) = 0.0873 Friedel opposites not merged Maximum memory for data reduction = 1733 / 21010 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 = 2091 / 158743 wR2 = 0.1130 before cycle 1 for 2114 data and 124 / 124 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55381 0.00138 0.005 OSF Mean shift/esd = 0.002 Maximum = 0.009 for U22 S1 Max. shift = 0.000 A for H7A Max. dU = 0.000 for H21A Least-squares cycle 2 Maximum vector length = 511 Memory required = 2091 / 158743 wR2 = 0.1130 before cycle 2 for 2114 data and 124 / 124 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55381 0.00138 0.001 OSF Mean shift/esd = 0.001 Maximum = 0.008 for tors H7A Max. shift = 0.000 A for H7A Max. dU = 0.000 for H21A Least-squares cycle 3 Maximum vector length = 511 Memory required = 2091 / 158743 wR2 = 0.1130 before cycle 3 for 2114 data and 124 / 124 parameters GooF = S = 1.032; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55381 0.00138 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.005 for tors H7A Max. shift = 0.000 A for H7A Max. dU = 0.000 for H21C Least-squares cycle 4 Maximum vector length = 511 Memory required = 2091 / 158743 wR2 = 0.1130 before cycle 4 for 2114 data and 124 / 124 parameters GooF = S = 1.032; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55381 0.00138 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.003 for tors H7A Max. shift = 0.000 A for H7A Max. dU = 0.000 for H21B 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 H2 0.4319 0.6201 0.1980 43 0.950 0.000 C2 C1 C3 H3 0.5267 0.6524 0.3029 43 0.950 0.000 C3 C4 C2 H5 0.4804 0.8683 0.9292 43 0.950 0.000 C5 C6 C4 H6 0.3858 0.8267 0.8329 43 0.950 0.000 C6 C5 C1 H7A 0.5854 0.9281 0.6445 137 0.980 0.000 C7 C4 H7A H7B 0.5981 0.7087 0.6090 137 0.980 0.000 C7 C4 H7A H7C 0.5786 0.7856 0.8603 137 0.980 0.000 C7 C4 H7A H22A 0.3552 1.2013 0.6804 137 0.980 0.000 C21 N22 H22A H22B 0.3042 1.1060 0.8202 137 0.980 0.000 C21 N22 H22A H22C 0.3087 1.3305 0.8045 137 0.980 0.000 C21 N22 H22A H21A 0.2438 1.2134 0.5385 137 0.910 0.000 N22 C21 H21A H21B 0.2886 1.1032 0.4187 137 0.910 0.000 N22 C21 H21A H21C 0.2899 1.3123 0.4122 137 0.910 0.000 N22 C21 H21A 06skc0020pna21 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.40031 0.72141 0.50530 1.00000 0.01441 0.01420 0.01997 0.00167 -0.00148 0.00209 0.01619 0.00627 0.00015 0.00051 0.00061 0.00000 0.00186 0.00177 0.00190 0.00165 0.00139 0.00157 0.00082 C2 0.44176 0.66972 0.34739 1.00000 0.02081 0.01688 0.02218 -0.00301 -0.00079 -0.00398 0.01996 0.00619 0.00015 0.00049 0.00064 0.00000 0.00203 0.00202 0.00206 0.00143 0.00151 0.00154 0.00089 H2 0.43188 0.62010 0.19805 1.00000 0.02395 0.00000 0.00000 C3 0.49821 0.69112 0.40942 1.00000 0.01893 0.02038 0.02269 0.00001 0.00227 0.00108 0.02067 0.00615 0.00013 0.00047 0.00074 0.00000 0.00172 0.00186 0.00192 0.00232 0.00207 0.00137 0.00075 H3 0.52673 0.65238 0.30292 1.00000 0.02480 0.00000 0.00000 C4 0.51329 0.76781 0.62344 1.00000 0.01498 0.01693 0.02553 0.00462 -0.00289 -0.00228 0.01914 0.00632 0.00014 0.00049 0.00070 0.00000 0.00181 0.00186 0.00202 0.00180 0.00165 0.00152 0.00079 C5 0.47066 0.81734 0.78041 1.00000 0.02391 0.01807 0.01817 -0.00024 -0.00486 -0.00062 0.02005 0.00644 0.00015 0.00050 0.00067 0.00000 0.00205 0.00205 0.00195 0.00167 0.00157 0.00157 0.00082 H5 0.48042 0.86827 0.92920 1.00000 0.02407 0.00000 0.00000 C6 0.41441 0.79372 0.72359 1.00000 0.02085 0.01595 0.01882 0.00144 0.00167 0.00269 0.01854 0.00644 0.00015 0.00052 0.00066 0.00000 0.00199 0.00188 0.00193 0.00185 0.00152 0.00163 0.00081 H6 0.38584 0.82667 0.83288 1.00000 0.02225 0.00000 0.00000 C7 0.57425 0.80043 0.69019 1.00000 0.01931 0.02954 0.03336 0.00287 -0.00708 -0.00262 0.02740 0.00674 0.00015 0.00059 0.00075 0.00000 0.00209 0.00229 0.00238 0.00207 0.00168 0.00179 0.00095 H7A 0.58541 0.92809 0.64448 1.00000 0.04110 0.00000 0.00000 H7B 0.59814 0.70871 0.60896 1.00000 0.04110 0.00000 0.00000 H7C 0.57865 0.78558 0.86030 1.00000 0.04110 0.00000 0.00000 O1A 0.32199 0.53800 0.27804 1.00000 0.01773 0.02123 0.03083 -0.00523 -0.00302 -0.00186 0.02326 0.00422 0.00010 0.00037 0.00047 0.00000 0.00137 0.00149 0.00161 0.00137 0.00120 0.00105 0.00064 O1B 0.31814 0.87608 0.27408 1.00000 0.01896 0.01750 0.03526 0.00351 -0.00714 0.00152 0.02391 0.00429 0.00010 0.00036 0.00049 0.00000 0.00145 0.00144 0.00163 0.00150 0.00117 0.00107 0.00064 O1C 0.29555 0.70810 0.63349 1.00000 0.01655 0.04527 0.02006 0.00073 0.00471 -0.00142 0.02729 0.00447 0.00010 0.00038 0.00043 0.00000 0.00141 0.00178 0.00147 0.00147 0.00114 0.00124 0.00068 S1 0.32830 0.70881 0.41872 1.00000 0.01353 0.01881 0.01963 -0.00060 -0.00014 -0.00048 0.01732 0.00143 0.00003 0.00012 0.00015 0.00000 0.00040 0.00043 0.00042 0.00073 0.00043 0.00035 0.00021 C21 0.31519 1.21215 0.72027 1.00000 0.01811 0.03022 0.02524 0.00009 -0.00587 0.00219 0.02452 0.00671 0.00016 0.00057 0.00069 0.00000 0.00201 0.00227 0.00214 0.00203 0.00160 0.00174 0.00090 H22A 0.35519 1.20133 0.68042 1.00000 0.03679 0.00000 0.00000 H22B 0.30416 1.10604 0.82015 1.00000 0.03679 0.00000 0.00000 H22C 0.30870 1.33046 0.80453 1.00000 0.03679 0.00000 0.00000 N22 0.28106 1.21007 0.50112 1.00000 0.01763 0.02152 0.02066 0.00024 0.00062 0.00317 0.01994 0.00548 0.00013 0.00048 0.00050 0.00000 0.00178 0.00176 0.00163 0.00156 0.00120 0.00145 0.00074 H21A 0.24383 1.21336 0.53846 1.00000 0.04739 0.00000 0.01494 H21B 0.28861 1.10324 0.41872 1.00000 0.06846 0.00000 0.01664 H21C 0.28988 1.31233 0.41217 1.00000 0.03098 0.00000 0.01126 Final Structure Factor Calculation for 06skc0020pna21 in Pna2(1) Total number of l.s. parameters = 124 Maximum vector length = 511 Memory required = 1969 / 26068 wR2 = 0.1130 before cycle 5 for 2114 data and 2 / 124 parameters GooF = S = 1.032; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0347 * P )^2 + 0.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0516 for 1547 Fo > 4sig(Fo) and 0.0856 for all 2114 data wR2 = 0.1130, GooF = S = 1.032, Restrained GooF = 1.031 for all data Flack x parameter = 0.2113 with esd 0.1260 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 Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0206 0.0164 0.0116 C1 0.0241 0.0224 0.0134 C2 0.0238 0.0207 0.0175 C3 0.0285 0.0155 0.0135 C4 0.0267 0.0181 0.0153 C5 0.0231 0.0179 0.0146 C6 0.0379 0.0281 0.0162 C7 0.0334 0.0212 0.0152 O1A 0.0383 0.0194 0.0140 O1B 0.0453 0.0233 0.0132 O1C 0.0199 0.0185 0.0135 S1 0.0309 0.0281 0.0146 C21 0.0234 0.0206 0.0158 N22 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 0.035 0.046 0.056 0.070 0.084 0.109 0.146 1.000 Number in group 231. 212. 196. 219. 202. 216. 209. 209. 210. 210. GooF 0.976 1.006 0.987 1.031 1.123 1.158 0.980 0.990 1.039 1.009 K 2.500 1.164 0.975 1.017 1.025 1.011 1.029 1.019 1.004 1.004 Resolution(A) 0.77 0.80 0.84 0.88 0.92 0.98 1.06 1.16 1.34 1.68 inf Number in group 217. 209. 213. 206. 211. 216. 208. 211. 211. 212. GooF 1.000 1.083 0.967 1.027 1.006 1.001 0.886 0.933 1.018 1.330 K 0.999 1.019 1.035 1.116 1.032 1.025 1.005 0.998 1.006 1.002 R1 0.200 0.200 0.144 0.137 0.101 0.083 0.046 0.038 0.035 0.031 Recommended weighting scheme: WGHT 0.0348 0.4920 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) 6 1 0 224.34 158.16 4.34 0.068 3.46 6 0 3 216.77 124.24 3.90 0.061 1.71 6 0 -3 214.38 126.76 3.68 0.061 1.71 1 2 0 1942.44 2306.11 3.68 0.261 3.51 2 2 0 125.70 81.39 3.53 0.049 3.40 1 5 4 85.91 129.98 3.49 0.062 1.00 6 3 0 411.53 318.54 3.37 0.097 2.03 22 2 4 -0.02 106.40 3.28 0.056 0.84 1 1 -1 404.75 486.91 3.22 0.120 4.37 2 1 6 324.83 229.29 3.18 0.082 0.94 8 0 6 186.37 87.27 3.13 0.051 0.90 11 7 3 90.78 179.06 3.05 0.073 0.83 13 1 -5 12.72 43.84 3.05 0.036 0.96 18 5 -2 19.13 59.78 3.03 0.042 0.92 6 4 0 137.05 87.79 3.00 0.051 1.62 22 0 -5 660.05 420.98 2.98 0.111 0.78 4 1 -3 781.84 666.78 2.97 0.140 1.75 2 7 0 126.46 73.88 2.93 0.047 1.01 8 2 0 486.75 571.82 2.86 0.130 2.28 10 1 -1 1028.67 893.41 2.84 0.162 2.09 16 6 -3 68.30 1.97 2.82 0.008 0.83 13 1 0 21.41 0.13 2.80 0.002 1.77 10 1 1 1013.42 883.97 2.77 0.161 2.09 13 1 3 12.03 30.37 2.77 0.030 1.29 16 2 -5 246.35 161.87 2.68 0.069 0.88 22 4 -3 135.75 50.49 2.66 0.039 0.83 4 1 3 797.00 681.33 2.65 0.142 1.75 1 1 1 417.33 483.55 2.65 0.119 4.37 0 6 0 180.26 74.49 2.62 0.047 1.18 13 2 -5 85.47 45.18 2.61 0.036 0.93 28 2 0 160.35 27.14 2.58 0.028 0.83 16 1 6 32.51 97.03 2.57 0.053 0.79 3 6 -5 326.63 174.41 2.56 0.072 0.82 7 3 -5 243.07 307.62 2.56 0.095 0.98 12 3 2 495.04 585.84 2.55 0.131 1.34 21 1 -2 50.41 7.54 2.53 0.015 1.04 19 2 -5 60.61 0.22 2.53 0.003 0.82 17 3 0 167.90 227.74 2.51 0.082 1.20 5 2 7 -81.32 64.48 2.50 0.044 0.78 10 0 3 839.91 708.36 2.49 0.145 1.48 15 1 -2 38.80 16.39 2.47 0.022 1.36 7 6 -2 300.61 378.75 2.47 0.106 1.04 6 3 1 456.75 533.55 2.47 0.125 1.91 3 4 6 -42.72 51.91 2.46 0.039 0.83 4 1 0 732.10 643.03 2.44 0.138 4.56 19 2 1 72.38 113.37 2.43 0.058 1.15 6 1 -2 848.93 752.80 2.42 0.149 2.20 6 0 6 1715.01 1405.68 2.42 0.204 0.92 25 2 4 -47.78 29.89 2.42 0.030 0.77 24 1 0 217.75 153.54 2.42 0.067 0.98 Bond lengths and angles C1 - Distance Angles C2 1.3831 (0.0050) C6 1.3861 (0.0051) 120.62 (0.34) S1 1.7825 (0.0038) 119.35 (0.27) 119.90 (0.27) C1 - C2 C6 C2 - Distance Angles C1 1.3831 (0.0050) C3 1.3952 (0.0048) 119.40 (0.35) H2 0.9500 120.30 120.30 C2 - C1 C3 C3 - Distance Angles C4 1.3821 (0.0057) C2 1.3952 (0.0048) 121.02 (0.34) H3 0.9500 119.49 119.49 C3 - C4 C2 C4 - Distance Angles C3 1.3821 (0.0057) C5 1.3959 (0.0052) 118.42 (0.32) C7 1.5150 (0.0049) 121.95 (0.34) 119.63 (0.36) C4 - C3 C5 C5 - Distance Angles C6 1.3852 (0.0051) C4 1.3959 (0.0052) 121.32 (0.35) H5 0.9500 119.34 119.34 C5 - C6 C4 C6 - Distance Angles C5 1.3852 (0.0051) C1 1.3861 (0.0051) 119.18 (0.34) H6 0.9500 120.41 120.41 C6 - C5 C1 C7 - Distance Angles C4 1.5150 (0.0049) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C4 H7A H7B O1A - Distance Angles S1 1.4616 (0.0028) O1A - O1B - Distance Angles S1 1.4658 (0.0028) O1B - O1C - Distance Angles S1 1.4494 (0.0026) O1C - S1 - Distance Angles O1C 1.4494 (0.0026) O1A 1.4616 (0.0028) 113.86 (0.16) O1B 1.4658 (0.0028) 112.87 (0.16) 110.37 (0.15) C1 1.7825 (0.0038) 106.37 (0.16) 106.96 (0.16) 105.82 (0.15) S1 - O1C O1A O1B C21 - Distance Angles N22 1.4883 (0.0048) H22A 0.9800 109.47 H22B 0.9800 109.47 109.47 H22C 0.9800 109.47 109.47 109.47 C21 - N22 H22A H22B N22 - Distance Angles C21 1.4883 (0.0048) H21A 0.9100 109.47 H21B 0.9100 109.47 109.47 H21C 0.9100 109.47 109.47 109.47 N22 - C21 H21A H21B Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.94 2.842(4) 169.2 N22-H21B...O1B 0.91 2.96 3.763(4) 148.6 N22-H21B...S1 0.91 2.30 3.060(4) 140.4 N22-H21A...O1B_$1 0.91 2.42 3.158(4) 138.3 N22-H21A...O1A_$1 0.91 2.76 3.522(3) 141.8 N22-H21A...S1_$1 0.91 1.93 2.826(4) 166.6 N22-H21C...O1A_$2 0.91 2.96 3.746(4) 145.4 N22-H21C...S1_$2 FMAP and GRID set by program FMAP 2 3 16 GRID -3.846 -1 -2 3.846 1 2 R1 = 0.0746 for 1207 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.49 at 0.3224 0.8734 0.4197 [ 0.84 A from O1B ] Deepest hole -0.32 at 0.0388 0.2801 0.0142 [ 1.24 A from C3 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2347 / 22425 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3224 0.8734 0.4197 1.00000 0.05 0.49 0.84 O1B 1.18 S1 1.81 O1C 1.82 H21B Q2 1 0.3976 0.8868 0.5004 1.00000 0.05 0.35 1.18 C1 1.49 C6 1.96 H6 2.06 C2 Q3 1 0.5957 0.6601 0.8428 1.00000 0.05 0.27 0.98 H7C 1.38 H7B 1.42 C7 2.23 H7A Q4 1 0.3301 0.9891 0.2756 1.00000 0.05 0.26 0.85 O1B 1.51 H21B 2.15 S1 2.22 H7A Q5 1 0.3379 0.4464 0.3123 1.00000 0.05 0.26 0.78 O1A 1.59 H21C 1.97 S1 2.21 H7B Q6 1 0.4868 0.7367 1.1166 1.00000 0.05 0.26 1.43 H5 1.54 H3 1.61 H2 1.72 C3 Q7 1 0.5286 1.0655 0.7658 1.00000 0.05 0.25 1.80 H7A 1.99 H5 2.02 C3 2.03 H5 Q8 1 0.5423 0.5270 0.1204 1.00000 0.05 0.25 1.42 H3 2.12 C2 2.18 C3 2.27 C3 Q9 1 0.3301 1.4975 0.9797 1.00000 0.05 0.24 1.63 H22C 1.73 O1A 2.36 H21A 2.37 H7B Q10 1 0.6096 0.7106 0.6799 1.00000 0.05 0.23 0.49 H7B 1.06 C7 1.37 H7C 1.66 H7A Shortest distances between peaks (including symmetry equivalents) 3 10 1.05 1 4 1.18 6 7 1.68 3 5 1.76 5 10 1.83 1 2 1.85 5 9 1.94 6 8 1.99 2 4 2.18 2 7 2.23 3 8 2.24 9 10 2.35 4 10 2.63 3 9 2.94 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. 0.41: 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 0.53: Structure factors and derivatives 0.23: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.05: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0020pna21 finished at 16:02:39 Total CPU time: 1.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++