+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0049p-1 started at 14:15:46 on 11-Jul-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0049p-1 in P-1 CELL 0.71073 5.3800 8.1542 12.6592 78.350 82.962 84.496 ZERR 2.00 0.0003 0.0006 0.0010 0.004 0.004 0.004 LATT 1 SFAC C H N O UNIT 18 28 4 8 V = 538.37 F(000) = 228.0 Mu = 0.10 mm-1 Cell Wt = 428.44 Rho = 1.321 MERG 2 OMIT -3.00 55.00 OMIT 3 0 6 SHEL 7 0.77 HTAB N23 O5A EQIV_$1 -x-1, -y+1, -z+1 HTAB O1A O1A_$1 HTAB O1A O1B_$1 EQIV_$2 -x+1, -y, -z HTAB O5A O5A_$2 HTAB N23 O5B_$2 EQIV_$3 x+2, y-1, z HTAB N21 O1B_$3 EQIV_$4 -x+1, -y, -z+1 HTAB N21 O1A_$4 FMAP 2 PLAN 10 SIZE 0.02 0.06 0.14 ACTA BOND $H WGHT 0.02850 0.61550 L.S. 4 TEMP -153.00 FVAR 0.89580 MOLE 1 C1 1 -0.335849 0.333235 0.402806 11.00000 0.02321 0.02825 = 0.02609 -0.00701 -0.00599 0.00307 C2 1 -0.115498 0.212007 0.378430 11.00000 0.02717 0.03177 = 0.02680 -0.00815 -0.00179 0.00684 AFIX 23 H2A 2 -0.150276 0.098361 0.419650 11.00000 -1.20000 H2B 2 0.035269 0.245193 0.404194 11.00000 -1.20000 AFIX 0 C3 1 -0.058710 0.204376 0.258947 11.00000 0.02268 0.02704 = 0.02365 -0.00654 -0.00679 0.00370 AFIX 23 H3A 2 -0.195498 0.150884 0.236105 11.00000 -1.20000 H3B 2 -0.053590 0.320013 0.215958 11.00000 -1.20000 AFIX 0 C4 1 0.189386 0.106440 0.235183 11.00000 0.02271 0.02819 = 0.02474 -0.00673 -0.00366 0.00369 AFIX 23 H4A 2 0.323836 0.157128 0.261737 11.00000 -1.20000 H4B 2 0.180508 -0.010101 0.276418 11.00000 -1.20000 AFIX 0 C5 1 0.260399 0.101149 0.116911 11.00000 0.02254 0.02728 = 0.02739 -0.00941 -0.00410 0.00121 O1A 4 -0.341700 0.382393 0.493878 11.00000 0.02957 0.04009 = 0.02190 -0.01332 -0.00524 0.01458 AFIX 147 H1 2 -0.450948 0.462791 0.496133 10.50000 0.04312 AFIX 0 O1B 4 -0.492091 0.379753 0.338361 11.00000 0.03030 0.04260 = 0.03777 -0.02226 -0.01408 0.01557 O5A 4 0.442011 -0.007221 0.097097 11.00000 0.03609 0.03943 = 0.02318 -0.00972 -0.00221 0.01746 AFIX 147 H5 2 0.476878 0.002207 0.029724 10.50000 0.08402 AFIX 0 O5B 4 0.152381 0.197618 0.046500 11.00000 0.03877 0.04227 = 0.02326 -0.00574 -0.00537 0.01955 MOLE 2 C22 1 1.117476 -0.346536 0.181921 11.00000 0.02390 0.02842 = 0.02760 -0.00465 -0.00471 0.00044 C24 1 0.783485 -0.225664 0.263175 11.00000 0.02360 0.03110 = 0.02556 -0.00563 -0.00044 0.00040 AFIX 43 H24 2 0.627540 -0.162935 0.274107 11.00000 -1.20000 AFIX 0 C25 1 0.926991 -0.305779 0.340589 11.00000 0.02954 0.02893 = 0.02494 -0.00454 -0.00193 0.00323 AFIX 43 H25 2 0.892528 -0.310691 0.416536 11.00000 -1.20000 AFIX 0 C26 1 1.299612 -0.404651 0.097518 11.00000 0.02882 0.04041 = 0.03131 -0.01205 0.00146 0.00335 AFIX 137 H26A 2 1.451013 -0.457476 0.129913 11.00000 -1.50000 H26B 2 1.344225 -0.308596 0.040277 11.00000 -1.50000 H26C 2 1.224344 -0.486409 0.066410 11.00000 -1.50000 AFIX 0 N21 3 1.134695 -0.379508 0.287357 11.00000 0.02554 0.02825 = 0.02840 -0.00466 -0.00664 0.00323 AFIX 43 H21 2 1.259545 -0.439395 0.319030 11.00000 0.09542 AFIX 0 N23 3 0.905214 -0.251789 0.165396 11.00000 0.02577 0.03333 = 0.02148 -0.00301 -0.00623 0.00283 AFIX 43 H23 2 0.851100 -0.211983 0.101680 11.00000 0.07921 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0049p-1 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - C1 C3 C3 - C4 C2 C4 - C5 C3 C5 - O5B O5A C4 O1A - C1 O1B - C1 O5A - C5 O5B - C5 C22 - N21 N23 C26 C24 - C25 N23 C25 - C24 N21 C26 - C22 N21 - C22 C25 N23 - C22 C24 Operators for generating equivalent atoms: $1 -x-1, -y+1, -z+1 $2 -x+1, -y, -z $3 x+2, y-1, z $4 -x+1, -y, -z+1 12525 Reflections read, of which 82 rejected -6 =< h =< 6, -10 =< k =< 10, -16 =< l =< 16, Max. 2-theta = 54.95 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 4 0 42.09 9.82 2 189.87 -2 5 1 31.85 2.69 7 14.15 -1 -7 3 42.78 16.74 2 165.56 3 3 4 13.66 4.60 4 26.86 4 Inconsistent equivalents 2457 Unique reflections, of which 0 suppressed R(int) = 0.1573 R(sigma) = 0.1376 Friedel opposites merged Maximum memory for data reduction = 1876 / 24214 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 = 2286 / 179723 wR2 = 0.1758 before cycle 1 for 2457 data and 143 / 143 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0285 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.89581 0.00315 0.002 OSF Mean shift/esd = 0.001 Maximum = 0.003 for U11 O1A Max. shift = 0.000 A for H5 Max. dU = 0.000 for H1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2286 / 179723 wR2 = 0.1758 before cycle 2 for 2457 data and 143 / 143 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0285 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.89581 0.00315 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U11 O1A Max. shift = 0.000 A for H1 Max. dU = 0.000 for H5 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2286 / 179723 wR2 = 0.1758 before cycle 3 for 2457 data and 143 / 143 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0285 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.89581 0.00315 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H5 Max. dU = 0.000 for H23 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2286 / 179723 wR2 = 0.1758 before cycle 4 for 2457 data and 143 / 143 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0285 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.89581 0.00315 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U22 C26 Max. shift = 0.000 A for H5 Max. dU = 0.000 for H5 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 H2A -0.1503 0.0984 0.4197 23 0.990 0.000 C2 C1 C3 H2B 0.0353 0.2452 0.4042 23 0.990 0.000 C2 C1 C3 H3A -0.1955 0.1509 0.2361 23 0.990 0.000 C3 C4 C2 H3B -0.0536 0.3200 0.2160 23 0.990 0.000 C3 C4 C2 H4A 0.3238 0.1571 0.2617 23 0.990 0.000 C4 C5 C3 H4B 0.1805 -0.0101 0.2764 23 0.990 0.000 C4 C5 C3 H1 -0.4510 0.4628 0.4961 147 0.840 0.000 O1A C1 H1 H5 0.4769 0.0022 0.0297 147 0.840 0.000 O5A C5 H5 H24 0.6275 -0.1629 0.2741 43 0.950 0.000 C24 C25 N23 H25 0.8925 -0.3107 0.4165 43 0.950 0.000 C25 C24 N21 H26A 1.4510 -0.4575 0.1299 137 0.980 0.000 C26 C22 H26A H26B 1.3442 -0.3086 0.0403 137 0.980 0.000 C26 C22 H26A H26C 1.2243 -0.4864 0.0664 137 0.980 0.000 C26 C22 H26A H21 1.2595 -0.4394 0.3190 43 0.880 0.000 N21 C22 C25 H23 0.8511 -0.2120 0.1017 43 0.880 0.000 N23 C22 C24 06skc0049p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.33585 0.33324 0.40281 1.00000 0.02321 0.02825 0.02609 -0.00701 -0.00599 0.00307 0.02564 0.00502 0.00057 0.00040 0.00028 0.00000 0.00165 0.00177 0.00199 0.00148 0.00141 0.00135 0.00076 C2 -0.11550 0.21201 0.37843 1.00000 0.02717 0.03177 0.02680 -0.00815 -0.00179 0.00684 0.02891 0.00539 0.00059 0.00042 0.00028 0.00000 0.00172 0.00184 0.00198 0.00152 0.00142 0.00143 0.00080 H2A -0.15027 0.09836 0.41965 1.00000 0.03469 0.00000 0.00000 H2B 0.03527 0.24519 0.40419 1.00000 0.03469 0.00000 0.00000 C3 -0.05871 0.20438 0.25895 1.00000 0.02268 0.02704 0.02365 -0.00654 -0.00679 0.00370 0.02422 0.00493 0.00055 0.00040 0.00027 0.00000 0.00159 0.00173 0.00184 0.00140 0.00133 0.00132 0.00073 H3A -0.19550 0.15088 0.23611 1.00000 0.02906 0.00000 0.00000 H3B -0.05359 0.32001 0.21596 1.00000 0.02906 0.00000 0.00000 C4 0.18939 0.10644 0.23518 1.00000 0.02271 0.02819 0.02475 -0.00674 -0.00366 0.00369 0.02525 0.00500 0.00055 0.00040 0.00027 0.00000 0.00162 0.00175 0.00190 0.00143 0.00136 0.00135 0.00075 H4A 0.32384 0.15713 0.26174 1.00000 0.03030 0.00000 0.00000 H4B 0.18051 -0.01010 0.27642 1.00000 0.03030 0.00000 0.00000 C5 0.26040 0.10115 0.11691 1.00000 0.02254 0.02728 0.02739 -0.00941 -0.00410 0.00121 0.02523 0.00481 0.00056 0.00040 0.00028 0.00000 0.00162 0.00175 0.00196 0.00151 0.00138 0.00137 0.00075 O1A -0.34170 0.38239 0.49388 1.00000 0.02958 0.04009 0.02190 -0.01332 -0.00524 0.01458 0.03040 0.00359 0.00040 0.00030 0.00019 0.00000 0.00129 0.00146 0.00136 0.00108 0.00099 0.00108 0.00060 H1 -0.45095 0.46279 0.49613 0.50000 0.04313 0.00000 0.02327 O1B -0.49209 0.37975 0.33836 1.00000 0.03030 0.04260 0.03777 -0.02226 -0.01408 0.01557 0.03515 0.00351 0.00040 0.00030 0.00020 0.00000 0.00127 0.00145 0.00157 0.00120 0.00113 0.00108 0.00064 O5A 0.44201 -0.00722 0.09710 1.00000 0.03610 0.03944 0.02318 -0.00972 -0.00221 0.01746 0.03380 0.00423 0.00045 0.00031 0.00020 0.00000 0.00137 0.00142 0.00147 0.00116 0.00113 0.00111 0.00062 H5 0.47688 0.00221 0.02972 0.50000 0.08401 0.00000 0.03259 O5B 0.15238 0.19762 0.04650 1.00000 0.03877 0.04227 0.02326 -0.00574 -0.00537 0.01955 0.03616 0.00391 0.00043 0.00030 0.00019 0.00000 0.00138 0.00143 0.00142 0.00113 0.00109 0.00114 0.00065 C22 1.11748 -0.34654 0.18192 1.00000 0.02390 0.02841 0.02760 -0.00465 -0.00471 0.00044 0.02673 0.00497 0.00057 0.00040 0.00028 0.00000 0.00167 0.00179 0.00201 0.00148 0.00139 0.00140 0.00077 C24 0.78349 -0.22566 0.26317 1.00000 0.02360 0.03110 0.02556 -0.00563 -0.00044 0.00040 0.02707 0.00504 0.00058 0.00040 0.00027 0.00000 0.00165 0.00183 0.00196 0.00149 0.00140 0.00138 0.00077 H24 0.62754 -0.16294 0.27411 1.00000 0.03249 0.00000 0.00000 C25 0.92699 -0.30578 0.34059 1.00000 0.02954 0.02893 0.02494 -0.00454 -0.00193 0.00323 0.02833 0.00523 0.00058 0.00040 0.00029 0.00000 0.00175 0.00179 0.00193 0.00147 0.00144 0.00142 0.00078 H25 0.89253 -0.31069 0.41654 1.00000 0.03400 0.00000 0.00000 C26 1.29961 -0.40465 0.09752 1.00000 0.02882 0.04041 0.03131 -0.01205 0.00145 0.00335 0.03357 0.00561 0.00061 0.00045 0.00030 0.00000 0.00178 0.00208 0.00215 0.00168 0.00152 0.00153 0.00086 H26A 1.45101 -0.45748 0.12991 1.00000 0.05035 0.00000 0.00000 H26B 1.34423 -0.30860 0.04028 1.00000 0.05035 0.00000 0.00000 H26C 1.22434 -0.48641 0.06641 1.00000 0.05035 0.00000 0.00000 N21 1.13469 -0.37951 0.28736 1.00000 0.02554 0.02825 0.02840 -0.00466 -0.00664 0.00323 0.02753 0.00412 0.00048 0.00033 0.00023 0.00000 0.00145 0.00151 0.00173 0.00126 0.00123 0.00121 0.00067 H21 1.25955 -0.43939 0.31903 1.00000 0.09541 0.00000 0.01856 N23 0.90521 -0.25179 0.16540 1.00000 0.02577 0.03333 0.02149 -0.00301 -0.00623 0.00283 0.02720 0.00423 0.00047 0.00033 0.00024 0.00000 0.00144 0.00156 0.00165 0.00126 0.00118 0.00120 0.00066 H23 0.85110 -0.21198 0.10168 1.00000 0.07922 0.00000 0.01655 Final Structure Factor Calculation for 06skc0049p-1 in P-1 Total number of l.s. parameters = 143 Maximum vector length = 511 Memory required = 2143 / 22995 wR2 = 0.1758 before cycle 5 for 2457 data and 0 / 143 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0285 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0941 for 1441 Fo > 4sig(Fo) and 0.1675 for all 2457 data wR2 = 0.1758, GooF = S = 1.046, Restrained GooF = 1.046 for all data Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0324 0.0247 0.0198 C1 0.0396 0.0275 0.0196 C2 0.0319 0.0229 0.0178 C3 0.0321 0.0240 0.0196 C4 0.0317 0.0229 0.0211 C5 0.0542 0.0215 0.0154 O1A 0.0636 0.0235 0.0183 O1B 0.0602 0.0249 0.0163 O5A 0.0659 0.0234 0.0192 O5B 0.0297 0.0283 0.0223 C22 0.0324 0.0270 0.0218 C24 0.0359 0.0250 0.0241 C25 0.0434 0.0354 0.0219 C26 0.0328 0.0292 0.0205 N21 0.0367 0.0266 0.0183 N23 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.015 0.022 0.029 0.038 0.049 0.064 0.086 0.123 1.000 Number in group 268. 254. 237. 224. 256. 239. 250. 240. 242. 247. GooF 1.117 1.067 1.104 0.951 0.981 1.068 1.036 1.101 1.017 0.997 K 39.733 4.914 3.339 1.974 1.725 1.075 1.128 1.076 1.011 0.995 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.66 inf Number in group 248. 243. 253. 238. 251. 249. 237. 245. 250. 243. GooF 1.058 0.996 1.028 1.051 1.133 1.099 1.015 0.922 1.049 1.093 K 1.230 1.232 1.235 1.158 1.235 1.547 1.030 0.998 1.037 0.992 R1 0.449 0.413 0.311 0.257 0.215 0.225 0.090 0.077 0.072 0.040 Recommended weighting scheme: WGHT 0.0284 0.6171 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) 0 3 3 45.80 16.06 4.65 0.039 2.46 3 6 0 112.27 63.10 4.45 0.077 1.10 -6 -3 1 153.24 72.44 3.53 0.083 0.85 -3 3 3 13.34 1.86 3.48 0.013 1.36 -3 6 6 22.66 4.02 3.42 0.020 0.95 2 -4 11 32.67 4.92 3.38 0.022 0.87 -3 -7 2 22.68 4.01 3.37 0.019 0.95 -5 3 2 42.32 73.12 3.28 0.083 0.95 -1 -10 1 56.04 2.55 3.27 0.016 0.78 3 2 11 922.66 73.67 3.22 0.084 1.02 -3 -3 3 18.63 3.54 3.19 0.018 1.35 -2 -8 2 1171.37 0.00 3.16 0.001 0.91 -2 -3 9 1044.22 14.27 3.14 0.037 1.02 -2 -7 6 22.50 0.03 3.02 0.002 0.88 4 3 10 37.05 15.75 3.00 0.039 0.96 -5 5 6 18.95 1.72 2.97 0.013 0.80 -1 -5 12 -7.15 18.32 2.95 0.042 0.78 1 -4 6 13.85 2.35 2.89 0.015 1.28 -1 -3 14 27.32 58.03 2.87 0.074 0.77 1 -1 7 236.35 167.48 2.86 0.126 1.62 3 6 3 151.11 113.46 2.77 0.104 1.13 5 1 9 126.16 89.87 2.77 0.092 0.90 -1 5 9 827.85 675.67 2.76 0.253 1.10 0 -5 8 1370.62 2.85 2.74 0.016 1.01 -2 6 7 21.84 0.19 2.72 0.004 1.02 4 6 12 -14.86 13.12 2.71 0.035 0.80 4 7 10 1.30 27.17 2.65 0.051 0.82 1 -1 3 24.10 12.15 2.65 0.034 2.94 5 1 12 532.88 2.10 2.61 0.014 0.79 -3 -6 3 846.25 10.60 2.61 0.032 1.01 5 6 5 51.01 19.84 2.60 0.043 0.87 -3 -7 5 -8.84 8.36 2.57 0.028 0.86 5 2 3 8.92 0.58 2.56 0.007 1.06 -2 -2 5 87.20 114.78 2.54 0.104 1.53 -2 5 9 54.88 34.29 2.54 0.057 1.01 -1 -6 3 11.98 0.06 2.53 0.002 1.18 6 4 2 9.47 26.84 2.50 0.050 0.85 0 -2 1 1898.16 2148.72 2.50 0.452 3.59 -5 -2 7 29.62 3.01 2.48 0.017 0.85 0 -4 10 25.91 9.48 2.48 0.030 0.97 2 5 2 78.55 103.28 2.47 0.099 1.45 -3 2 12 110.48 63.77 2.46 0.078 0.85 -4 3 9 24.54 3.48 2.44 0.018 0.88 -2 1 1 8.81 19.01 2.44 0.042 2.41 6 0 8 15.49 0.56 2.43 0.007 0.81 2 10 6 -3.91 18.11 2.42 0.041 0.79 1 7 6 26.92 43.36 2.42 0.064 1.09 0 6 0 6.18 0.07 2.40 0.003 1.33 0 -3 3 164.34 134.13 2.39 0.113 2.06 -4 -1 9 26.47 48.01 2.38 0.068 0.89 Bond lengths and angles C1 - Distance Angles O1B 1.2239 (0.0036) O1A 1.2908 (0.0039) 124.24 (0.29) C2 1.5121 (0.0042) 120.68 (0.30) 115.08 (0.27) C1 - O1B O1A C2 - Distance Angles C1 1.5121 (0.0042) C3 1.5186 (0.0045) 113.86 (0.27) H2A 0.9900 108.78 108.78 H2B 0.9900 108.78 108.78 107.67 C2 - C1 C3 H2A C3 - Distance Angles C4 1.5179 (0.0040) C2 1.5186 (0.0045) 112.18 (0.26) H3A 0.9900 109.17 109.17 H3B 0.9900 109.17 109.17 107.88 C3 - C4 C2 H3A C4 - Distance Angles C5 1.5074 (0.0045) C3 1.5179 (0.0040) 114.40 (0.26) H4A 0.9900 108.66 108.66 H4B 0.9900 108.66 108.66 107.60 C4 - C5 C3 H4A C5 - Distance Angles O5B 1.2276 (0.0037) O5A 1.2893 (0.0036) 124.04 (0.31) C4 1.5074 (0.0045) 120.70 (0.27) 115.25 (0.28) C5 - O5B O5A O1A - Distance Angles C1 1.2908 (0.0039) H1 0.8400 109.47 O1A - C1 O1B - Distance Angles C1 1.2239 (0.0037) O1B - O5A - Distance Angles C5 1.2893 (0.0036) H5 0.8400 109.47 O5A - C5 O5B - Distance Angles C5 1.2276 (0.0037) O5B - C22 - Distance Angles N21 1.3202 (0.0043) N23 1.3299 (0.0039) 107.43 (0.29) C26 1.4783 (0.0045) 126.43 (0.29) 126.14 (0.31) C22 - N21 N23 C24 - Distance Angles C25 1.3466 (0.0045) N23 1.3739 (0.0042) 107.05 (0.28) H24 0.9500 126.48 126.48 C24 - C25 N23 C25 - Distance Angles C24 1.3466 (0.0045) N21 1.3836 (0.0041) 106.23 (0.30) H25 0.9500 126.88 126.88 C25 - C24 N21 C26 - Distance Angles C22 1.4783 (0.0045) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C22 H26A H26B N21 - Distance Angles C22 1.3202 (0.0043) C25 1.3836 (0.0041) 109.80 (0.27) H21 0.8800 125.10 125.10 N21 - C22 C25 N23 - Distance Angles C22 1.3299 (0.0039) C24 1.3739 (0.0042) 109.48 (0.28) H23 0.8800 125.26 125.26 N23 - C22 C24 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.63 3.133(3) 117.2 N23-H23...O5A 0.84 1.62 2.456(4) 177.3 O1A-H1...O1A_$1 0.84 2.64 3.152(3) 120.4 O1A-H1...O1B_$1 0.84 1.60 2.443(5) 175.5 O5A-H5...O5A_$2 0.88 1.86 2.681(4) 154.8 N23-H23...O5B_$2 0.88 1.89 2.711(3) 154.4 N21-H21...O1B_$3 0.88 2.60 3.104(4) 117.3 N21-H21...O1A_$4 FMAP and GRID set by program FMAP 2 1 15 GRID -4.167 -2 -2 4.167 2 2 R1 = 0.1674 for 2457 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.26 at 0.4439 0.6625 0.0731 [ 0.71 A from H26B ] Deepest hole -0.27 at 0.1236 0.5657 0.3613 [ 0.85 A from H21 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2254 / 16647 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.4439 -0.3375 0.0731 1.00000 0.05 0.26 0.71 H26B 0.98 C26 1.09 H26A 1.79 H26C Q2 1 0.2632 0.0523 0.3627 1.00000 0.05 0.23 1.41 H4A 1.43 H4B 1.67 C4 2.01 H2B Q3 1 -0.0352 0.2250 0.0082 1.00000 0.05 0.23 1.16 O5B 1.62 H23 1.86 H26B 2.20 N23 Q4 1 -0.3882 0.0717 0.3990 1.00000 0.05 0.23 1.38 H2A 1.91 C2 2.19 C1 2.19 H3A Q5 1 1.2676 -0.2978 0.2472 1.00000 0.05 0.22 1.04 N21 1.32 H21 1.36 C22 2.05 C25 Q6 1 0.2810 0.2552 0.2411 1.00000 0.05 0.22 0.81 H4A 1.37 C4 1.87 H3B 1.89 C3 Q7 1 1.4349 -0.5504 0.1593 1.00000 0.05 0.22 0.78 H26A 1.47 C26 1.70 H26C 2.28 H26B Q8 1 1.2080 -0.4413 0.4051 1.00000 0.05 0.21 1.09 H21 1.56 N21 1.71 O1A 1.89 H1 Q9 1 0.0047 -0.0484 0.2005 1.00000 0.05 0.21 1.52 H4B 1.83 C4 1.94 N23 1.94 C24 Q10 1 0.3597 0.1580 0.1836 1.00000 0.05 0.20 0.98 H4A 1.12 C4 1.24 C5 1.87 H4B Shortest distances between peaks (including symmetry equivalents) 6 10 1.20 1 7 1.86 6 7 1.91 2 4 2.01 2 6 2.02 5 8 2.11 2 10 2.27 1 5 2.36 5 9 2.38 7 10 2.40 1 3 2.55 5 7 2.57 9 10 2.63 4 4 2.77 2 9 2.90 4 6 2.93 3 9 2.96 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 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.58: 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 0.02: Generate idealized H-atoms 0.33: 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 0.08: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0049p-1 finished at 14:15:48 Total CPU time: 1.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++