+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0022p21n started at 22:07:37 on 31-Jul-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0022p21n in P2(1)/n CELL 0.71073 7.6480 11.6730 11.2040 90.000 93.547 90.000 ZERR 4.00 0.0007 0.0009 0.0011 0.000 0.004 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 36 48 8 16 V = 998.32 F(000) = 448.0 Mu = 0.11 mm-1 Cell Wt = 848.82 Rho = 1.412 MERG 2 OMIT -3.00 55.00 OMIT 0 2 0 SHEL 7 0.77 EQIV_$1 x+1/2, -y+1/2, z+1/2 HTAB O4A O1B_$1 EQIV_$2 -x+1/2, y+1/2, -z-3/2 HTAB N23 O1A_$2 HTAB N23 O1B_$2 FMAP 2 PLAN 10 SIZE 0.01 0.05 0.08 ACTA BOND $H WGHT 0.00000 3.22200 L.S. 4 TEMP -153.00 FVAR 0.34683 MOLE 1 C1 1 0.081914 0.045046 -0.656591 11.00000 0.02473 0.01695 = 0.03073 -0.00076 0.00311 -0.00052 C2 1 0.122253 0.161212 -0.605184 11.00000 0.03204 0.02044 = 0.02283 0.00256 -0.00070 0.00289 AFIX 43 H2 2 0.066604 0.226408 -0.641273 11.00000 -1.20000 AFIX 0 C3 1 0.232613 0.175616 -0.511418 11.00000 0.02745 0.02111 = 0.02691 0.00433 -0.00093 -0.00151 AFIX 43 H3 2 0.287905 0.109704 -0.476605 11.00000 -1.20000 AFIX 0 C4 1 0.275549 0.288779 -0.457042 11.00000 0.01947 0.02503 = 0.02470 -0.00171 0.00249 -0.00429 O1A 4 0.159740 -0.040653 -0.609725 11.00000 0.03158 0.01759 = 0.02760 0.00066 -0.00571 0.00159 O1B 4 -0.027479 0.039036 -0.746188 11.00000 0.03283 0.02179 = 0.02959 0.00045 -0.01061 -0.00222 O4A 4 0.385099 0.279539 -0.360649 11.00000 0.03397 0.02092 = 0.03090 -0.00483 -0.00917 -0.00015 AFIX 147 H4 2 0.409873 0.345147 -0.333840 11.00000 0.07199 AFIX 0 O4B 4 0.215809 0.379614 -0.494942 11.00000 0.03706 0.02269 = 0.03430 0.00336 -0.00604 0.00112 MOLE 2 C22 1 0.428843 0.171627 -0.804203 11.00000 0.02329 0.02181 = 0.02465 0.00078 0.00264 0.00365 C24 1 0.568423 0.274875 -0.665221 11.00000 0.02840 0.02535 = 0.02028 -0.00071 -0.00355 -0.00346 AFIX 43 H24 2 0.609802 0.339028 -0.619572 11.00000 -1.20000 AFIX 0 C25 1 0.608554 0.164951 -0.642492 11.00000 0.02541 0.02769 = 0.02169 0.00038 -0.00276 0.00388 AFIX 43 H25 2 0.682333 0.136473 -0.577874 11.00000 -1.20000 AFIX 0 C26 1 0.530748 -0.024157 -0.745645 11.00000 0.03372 0.01909 = 0.02720 -0.00064 -0.00453 0.00099 AFIX 137 H26A 2 0.472051 -0.046289 -0.822420 11.00000 -1.50000 H26B 2 0.472647 -0.061387 -0.680428 11.00000 -1.50000 H26C 2 0.653702 -0.048142 -0.743461 11.00000 -1.50000 AFIX 0 C27 1 0.316532 0.141289 -0.912021 11.00000 0.03082 0.02419 = 0.02499 0.00347 -0.00441 0.00410 AFIX 137 H27A 2 0.390404 0.118392 -0.976345 11.00000 -1.50000 H27B 2 0.245589 0.207766 -0.937771 11.00000 -1.50000 H27C 2 0.239297 0.077638 -0.893282 11.00000 -1.50000 AFIX 0 N21 3 0.521496 0.101110 -0.731558 11.00000 0.02762 0.01931 = 0.02740 -0.00017 -0.00158 0.00095 N23 3 0.457282 0.278502 -0.765811 11.00000 0.02410 0.02153 = 0.02578 0.00251 -0.00239 0.00056 AFIX 43 H23 2 0.412242 0.340866 -0.799428 11.00000 0.02995 AFIX 0 HKLF 4 Covalent radii and connectivity table for 07skc0022p21n in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C3 C1 C3 - C2 C4 C4 - O4B O4A C3 O1A - C1 O1B - C1 O4A - C4 O4B - C4 C22 - N21 N23 C27 C24 - C25 N23 C25 - C24 N21 C26 - N21 C27 - C22 N21 - C22 C25 C26 N23 - C22 C24 Operators for generating equivalent atoms: $1 x+1/2, -y+1/2, z+1/2 $2 -x+1/2, y+1/2, -z-3/2 15730 Reflections read, of which 512 rejected -9 =< h =< 9, -15 =< k =< 14, -14 =< l =< 14, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 2279 Unique reflections, of which 0 suppressed R(int) = 0.1219 R(sigma) = 0.0854 Friedel opposites merged Maximum memory for data reduction = 1606 / 22574 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 = 1996 / 177390 wR2 = 0.1889 before cycle 1 for 2279 data and 141 / 141 parameters GooF = S = 1.167; Restrained GooF = 1.167 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34683 0.00122 0.002 OSF Mean shift/esd = 0.001 Maximum = 0.002 for U12 O4A Max. shift = 0.000 A for H27B Max. dU = 0.000 for C4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1996 / 177390 wR2 = 0.1889 before cycle 2 for 2279 data and 141 / 141 parameters GooF = S = 1.167; Restrained GooF = 1.167 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34683 0.00122 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U12 O4A Max. shift = 0.000 A for H4 Max. dU = 0.000 for C4 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1996 / 177390 wR2 = 0.1889 before cycle 3 for 2279 data and 141 / 141 parameters GooF = S = 1.167; Restrained GooF = 1.167 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34683 0.00122 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C22 Max. shift = 0.000 A for H27A Max. dU = 0.000 for H4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1996 / 177390 wR2 = 0.1889 before cycle 4 for 2279 data and 141 / 141 parameters GooF = S = 1.167; Restrained GooF = 1.167 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34683 0.00122 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1B Max. shift = 0.000 A for H27A Max. dU = 0.000 for H4 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 0.0666 0.2264 -0.6413 43 0.950 0.000 C2 C3 C1 H3 0.2879 0.1097 -0.4766 43 0.950 0.000 C3 C2 C4 H4 0.4099 0.3451 -0.3338 147 0.840 0.000 O4A C4 H4 H24 0.6098 0.3390 -0.6196 43 0.950 0.000 C24 C25 N23 H25 0.6823 0.1365 -0.5779 43 0.950 0.000 C25 C24 N21 H26A 0.4721 -0.0463 -0.8224 137 0.980 0.000 C26 N21 H26A H26B 0.4726 -0.0614 -0.6804 137 0.980 0.000 C26 N21 H26A H26C 0.6537 -0.0481 -0.7435 137 0.980 0.000 C26 N21 H26A H27A 0.3904 0.1184 -0.9763 137 0.980 0.000 C27 C22 H27A H27B 0.2456 0.2078 -0.9378 137 0.980 0.000 C27 C22 H27A H27C 0.2393 0.0776 -0.8933 137 0.980 0.000 C27 C22 H27A H23 0.4122 0.3409 -0.7994 43 0.880 0.000 N23 C22 C24 07skc0022p21n in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.08191 0.04505 -0.65659 1.00000 0.02473 0.01695 0.03073 -0.00076 0.00311 -0.00052 0.02408 0.00725 0.00055 0.00034 0.00038 0.00000 0.00224 0.00201 0.00244 0.00183 0.00194 0.00178 0.00094 C2 0.12225 0.16121 -0.60518 1.00000 0.03204 0.02044 0.02283 0.00256 -0.00070 0.00289 0.02520 0.00746 0.00057 0.00035 0.00037 0.00000 0.00254 0.00203 0.00238 0.00172 0.00198 0.00182 0.00099 H2 0.06660 0.22641 -0.64127 1.00000 0.03024 0.00000 0.00000 C3 0.23261 0.17562 -0.51142 1.00000 0.02745 0.02111 0.02691 0.00433 -0.00093 -0.00151 0.02527 0.00728 0.00055 0.00035 0.00038 0.00000 0.00241 0.00208 0.00249 0.00179 0.00200 0.00180 0.00100 H3 0.28791 0.10970 -0.47661 1.00000 0.03032 0.00000 0.00000 C4 0.27555 0.28878 -0.45704 1.00000 0.01947 0.02503 0.02470 -0.00171 0.00249 -0.00429 0.02302 0.00705 0.00053 0.00035 0.00038 0.00000 0.00211 0.00221 0.00224 0.00187 0.00178 0.00179 0.00092 O1A 0.15974 -0.04065 -0.60973 1.00000 0.03158 0.01759 0.02760 0.00066 -0.00571 0.00159 0.02590 0.00479 0.00038 0.00023 0.00025 0.00000 0.00168 0.00142 0.00167 0.00128 0.00133 0.00131 0.00070 O1B -0.02748 0.03904 -0.74619 1.00000 0.03283 0.02179 0.02959 0.00045 -0.01061 -0.00222 0.02859 0.00489 0.00039 0.00024 0.00026 0.00000 0.00175 0.00152 0.00171 0.00128 0.00141 0.00133 0.00074 O4A 0.38510 0.27954 -0.36065 1.00000 0.03397 0.02092 0.03090 -0.00483 -0.00917 -0.00015 0.02906 0.00503 0.00040 0.00025 0.00027 0.00000 0.00184 0.00160 0.00177 0.00141 0.00148 0.00144 0.00076 H4 0.40987 0.34515 -0.33384 1.00000 0.07199 0.00000 0.02097 O4B 0.21581 0.37961 -0.49494 1.00000 0.03706 0.02269 0.03430 0.00336 -0.00604 0.00112 0.03169 0.00521 0.00041 0.00024 0.00028 0.00000 0.00184 0.00157 0.00182 0.00139 0.00148 0.00139 0.00077 C22 0.42884 0.17163 -0.80420 1.00000 0.02329 0.02181 0.02465 0.00078 0.00264 0.00365 0.02320 0.00736 0.00054 0.00035 0.00038 0.00000 0.00227 0.00207 0.00237 0.00174 0.00182 0.00175 0.00094 C24 0.56842 0.27487 -0.66522 1.00000 0.02840 0.02535 0.02028 -0.00071 -0.00355 -0.00346 0.02489 0.00729 0.00055 0.00036 0.00036 0.00000 0.00235 0.00223 0.00224 0.00181 0.00189 0.00185 0.00097 H24 0.60980 0.33903 -0.61957 1.00000 0.02986 0.00000 0.00000 C25 0.60855 0.16495 -0.64249 1.00000 0.02541 0.02769 0.02169 0.00038 -0.00276 0.00388 0.02510 0.00745 0.00056 0.00035 0.00039 0.00000 0.00233 0.00223 0.00227 0.00184 0.00186 0.00187 0.00096 H25 0.68233 0.13647 -0.57787 1.00000 0.03012 0.00000 0.00000 C26 0.53075 -0.02416 -0.74565 1.00000 0.03372 0.01909 0.02720 -0.00064 -0.00453 0.00099 0.02694 0.00740 0.00059 0.00034 0.00039 0.00000 0.00249 0.00214 0.00238 0.00178 0.00196 0.00184 0.00100 H26A 0.47205 -0.04629 -0.82242 1.00000 0.04041 0.00000 0.00000 H26B 0.47265 -0.06139 -0.68043 1.00000 0.04041 0.00000 0.00000 H26C 0.65370 -0.04814 -0.74346 1.00000 0.04041 0.00000 0.00000 C27 0.31653 0.14129 -0.91202 1.00000 0.03082 0.02419 0.02499 0.00347 -0.00441 0.00410 0.02692 0.00732 0.00057 0.00036 0.00038 0.00000 0.00249 0.00219 0.00241 0.00178 0.00200 0.00184 0.00102 H27A 0.39040 0.11839 -0.97635 1.00000 0.04038 0.00000 0.00000 H27B 0.24559 0.20777 -0.93777 1.00000 0.04038 0.00000 0.00000 H27C 0.23930 0.07764 -0.89328 1.00000 0.04038 0.00000 0.00000 N21 0.52150 0.10111 -0.73156 1.00000 0.02762 0.01931 0.02740 -0.00017 -0.00158 0.00095 0.02491 0.00608 0.00046 0.00029 0.00032 0.00000 0.00195 0.00176 0.00197 0.00151 0.00160 0.00153 0.00082 N23 0.45728 0.27850 -0.76581 1.00000 0.02410 0.02153 0.02578 0.00251 -0.00239 0.00056 0.02397 0.00586 0.00044 0.00029 0.00031 0.00000 0.00192 0.00185 0.00198 0.00154 0.00158 0.00153 0.00082 H23 0.41224 0.34087 -0.79943 1.00000 0.02995 0.00000 0.01278 Final Structure Factor Calculation for 07skc0022p21n in P2(1)/n Total number of l.s. parameters = 141 Maximum vector length = 511 Memory required = 1855 / 22995 wR2 = 0.1889 before cycle 5 for 2279 data and 0 / 141 parameters GooF = S = 1.167; Restrained GooF = 1.167 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1020 for 1382 Fo > 4sig(Fo) and 0.1724 for all 2279 data wR2 = 0.1889, GooF = S = 1.167, Restrained GooF = 1.167 for all data Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0310 0.0243 0.0169 C1 0.0332 0.0244 0.0180 C2 0.0317 0.0253 0.0188 C3 0.0283 0.0236 0.0171 C4 0.0379 0.0226 0.0171 O1A 0.0449 0.0220 0.0189 O1B 0.0449 0.0248 0.0175 O4A 0.0447 0.0293 0.0211 O4B 0.0270 0.0238 0.0188 C22 0.0324 0.0247 0.0176 C24 0.0314 0.0254 0.0185 C25 0.0382 0.0236 0.0190 C26 0.0354 0.0278 0.0176 C27 0.0311 0.0245 0.0192 N21 0.0296 0.0231 0.0193 N23 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.004 0.008 0.011 0.015 0.019 0.026 0.033 0.043 0.063 1.000 Number in group 242. 263. 206. 227. 209. 254. 210. 222. 217. 229. GooF 1.293 1.326 1.267 1.236 1.210 1.104 1.121 1.090 0.911 1.013 K 20.781 3.957 1.951 1.341 1.127 1.054 1.047 0.982 0.989 0.991 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.65 inf Number in group 229. 230. 231. 226. 228. 225. 226. 227. 228. 229. GooF 1.323 1.223 1.216 1.298 1.212 1.082 1.036 1.048 1.088 1.098 K 1.331 1.154 1.198 1.135 1.064 1.042 1.021 0.980 1.044 0.971 R1 0.414 0.328 0.324 0.285 0.246 0.152 0.107 0.110 0.072 0.044 Recommended weighting scheme: WGHT 0.0000 3.2220 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 6 3 173.32 62.14 5.09 0.027 1.56 -1 0 1 22.92 107.65 4.27 0.036 6.49 -7 5 3 67.34 4.74 3.64 0.008 0.97 3 2 12 118.04 1.35 3.56 0.004 0.85 4 12 5 75.83 7.21 3.47 0.009 0.80 0 8 10 61.33 0.45 3.44 0.002 0.89 -7 7 2 53.62 0.88 3.17 0.003 0.91 3 4 2 32.78 4.79 3.12 0.008 1.79 -1 1 13 168.77 12.21 3.06 0.012 0.86 -4 0 4 16247.36 14438.36 3.05 0.415 1.62 6 8 1 66.53 153.62 3.00 0.043 0.95 6 6 2 70.71 9.62 2.97 0.011 1.04 -4 1 12 89.59 3.05 2.94 0.006 0.86 1 1 12 128.35 52.81 2.92 0.025 0.92 -4 13 5 91.15 26.22 2.91 0.018 0.77 1 14 4 79.40 1.63 2.88 0.004 0.79 4 13 1 -21.58 32.58 2.88 0.020 0.81 4 6 1 69.20 26.20 2.81 0.018 1.35 8 4 6 83.66 19.00 2.80 0.015 0.80 4 3 4 168.23 258.76 2.75 0.056 1.43 6 8 7 86.24 24.42 2.74 0.017 0.81 1 1 0 110.90 60.74 2.72 0.027 6.39 -8 1 3 44.53 0.46 2.69 0.002 0.94 -1 3 14 -23.56 29.04 2.65 0.019 0.78 -8 1 6 49.38 0.44 2.62 0.002 0.87 -2 14 3 52.11 2.46 2.61 0.005 0.80 3 11 5 47.20 8.19 2.58 0.010 0.89 5 12 3 44.46 1.64 2.57 0.004 0.80 4 6 9 49.95 5.83 2.57 0.008 0.90 -7 2 6 38.35 1.96 2.56 0.005 0.95 -2 8 9 37.38 0.20 2.51 0.002 0.93 7 0 1 49.59 6.09 2.48 0.009 1.08 -5 10 5 32.48 1.76 2.40 0.005 0.87 -2 0 2 76971.67 83896.17 2.38 1.000 3.25 -5 12 3 35.19 1.21 2.37 0.004 0.81 -6 10 5 59.64 122.22 2.36 0.038 0.81 2 7 12 70.67 3.55 2.36 0.007 0.79 3 6 3 37.35 11.25 2.34 0.012 1.41 -4 4 11 53.03 0.00 2.33 0.000 0.88 0 5 12 46.31 0.08 2.33 0.001 0.87 2 5 3 14.25 0.53 2.33 0.003 1.73 5 5 9 -3.88 38.53 2.32 0.021 0.87 7 4 7 35.85 1.30 2.31 0.004 0.84 -9 2 4 64.93 8.65 2.31 0.010 0.82 4 0 2 108.92 61.88 2.30 0.027 1.77 9 1 5 70.95 14.56 2.30 0.013 0.78 0 14 0 35.12 110.02 2.30 0.036 0.83 7 2 8 59.22 16.29 2.29 0.014 0.83 -3 14 3 -19.18 21.15 2.28 0.016 0.78 0 8 12 94.46 32.21 2.28 0.020 0.79 Bond lengths and angles C1 - Distance Angles O1A 1.2618 (0.0046) O1B 1.2683 (0.0049) 123.82 (0.37) C2 1.4979 (0.0055) 118.50 (0.37) 117.68 (0.36) C1 - O1A O1B C2 - Distance Angles C3 1.3171 (0.0059) C1 1.4979 (0.0055) 121.93 (0.39) H2 0.9500 119.04 119.04 C2 - C3 C1 C3 - Distance Angles C2 1.3171 (0.0059) C4 1.4830 (0.0056) 123.79 (0.39) H3 0.9500 118.11 118.11 C3 - C2 C4 C4 - Distance Angles O4B 1.2204 (0.0048) O4A 1.3297 (0.0048) 123.82 (0.38) C3 1.4830 (0.0056) 124.22 (0.37) 111.95 (0.36) C4 - O4B O4A O1A - Distance Angles C1 1.2618 (0.0046) O1A - O1B - Distance Angles C1 1.2683 (0.0049) O1B - O4A - Distance Angles C4 1.3297 (0.0048) H4 0.8400 109.47 O4A - C4 O4B - Distance Angles C4 1.2204 (0.0048) O4B - C22 - Distance Angles N21 1.3307 (0.0051) N23 1.3331 (0.0052) 108.15 (0.36) C27 1.4812 (0.0057) 127.66 (0.37) 124.17 (0.37) C22 - N21 N23 C24 - Distance Angles C25 1.3401 (0.0058) N23 1.3696 (0.0050) 108.01 (0.38) H24 0.9500 126.00 126.00 C24 - C25 N23 C25 - Distance Angles C24 1.3401 (0.0058) N21 1.3828 (0.0052) 106.53 (0.37) H25 0.9500 126.74 126.74 C25 - C24 N21 C26 - Distance Angles N21 1.4729 (0.0050) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - N21 H26A H26B C27 - Distance Angles C22 1.4812 (0.0057) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C22 H27A H27B N21 - Distance Angles C22 1.3307 (0.0051) C25 1.3828 (0.0052) 108.81 (0.33) C26 1.4729 (0.0050) 125.16 (0.36) 126.03 (0.35) N21 - C22 C25 N23 - Distance Angles C22 1.3331 (0.0052) C24 1.3696 (0.0050) 108.49 (0.35) H23 0.8800 125.76 125.76 N23 - C22 C24 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.72 2.544(4) 165.6 O4A-H4...O1B_$1 0.88 1.78 2.655(4) 169.8 N23-H23...O1A_$2 0.88 2.52 3.090(4) 123.4 N23-H23...O1B_$2 FMAP and GRID set by program FMAP 2 1 12 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.1724 for 2279 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.28 at 0.0305 0.7779 0.9200 [ 0.96 A from O4A ] Deepest hole -0.32 at 0.0300 0.6966 0.2317 [ 0.90 A from C22 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 2087 / 16812 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4695 0.2779 -0.4200 1.00000 0.05 0.28 0.96 O4A 1.35 H4 1.52 C4 2.14 H27B Q2 1 0.1151 0.1204 -0.8913 1.00000 0.05 0.28 1.07 H27C 1.54 H27B 1.59 C27 1.78 H4 Q3 1 0.5176 0.3451 -0.5656 1.00000 0.05 0.27 0.96 H24 1.46 C24 2.27 H27B 2.37 C4 Q4 1 0.6633 0.4487 -0.5714 1.00000 0.05 0.27 1.44 H24 2.07 H27C 2.13 H27A 2.31 O4B Q5 1 0.1118 0.2127 -0.9266 1.00000 0.05 0.26 1.04 H27B 1.77 C27 1.88 H27C 1.93 O4A Q6 1 -0.0627 0.0336 -0.5370 1.00000 0.05 0.25 1.79 C1 1.85 O1A 2.12 O1A 2.22 C2 Q7 1 0.2248 -0.0270 -0.6777 1.00000 0.05 0.25 0.95 O1A 1.41 C1 1.87 H23 1.94 H26B Q8 1 0.6170 0.3660 -0.6420 1.00000 0.05 0.25 0.41 H24 1.15 C24 2.06 N23 2.30 H23 Q9 1 0.3372 0.2728 -1.0234 1.00000 0.05 0.24 1.44 H27B 1.68 H25 1.91 H27A 1.99 C27 Q10 1 -0.0574 0.0598 -0.8162 1.00000 0.05 0.24 0.84 O1B 1.15 H4 1.98 O4A 2.03 C1 Shortest distances between peaks (including symmetry equivalents) 1 5 1.10 2 5 1.15 3 8 1.20 4 8 1.28 6 6 1.46 1 2 1.65 3 4 1.65 2 10 1.76 3 5 1.81 1 3 1.87 4 10 1.95 2 3 2.09 5 9 2.21 2 4 2.23 1 10 2.24 8 10 2.35 6 9 2.39 4 5 2.53 5 10 2.57 5 8 2.58 8 9 2.64 7 10 2.77 6 7 2.77 2 8 2.81 3 9 2.82 3 10 2.86 6 7 2.87 2 9 2.92 2 4 2.93 4 9 2.94 1 8 2.98 Time profile in seconds ----------------------- 0.06: 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. 0.72: 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 0.34: Structure factors and derivatives 0.34: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0022p21n finished at 22:07:39 Total CPU time: 1.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++