+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0082p21n started at 14:42:48 on 11-Jul-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0082p21n in P2(1)/n CELL 0.71073 7.5192 7.0534 18.9307 90.000 100.552 90.000 ZERR 4.00 0.0003 0.0003 0.0008 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 32 48 8 24 V = 987.03 F(000) = 488.0 Mu = 0.14 mm-1 Cell Wt = 928.78 Rho = 1.563 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB N23 O1B HTAB N23 O2 HTAB O3 O4B EQIV_$1 x-1, y, z HTAB O4A O1B_$1 EQIV_$2 -x+1, -y, -z HTAB O3 O4B_$2 EQIV_$3 -x+3/2, y+1/2, -z+1/2 HTAB O2 O1A_$3 FMAP 2 PLAN 10 SIZE 0.05 0.08 0.10 ACTA BOND $H WGHT 0.02240 1.43410 L.S. 4 TEMP -153.00 FVAR 0.88353 MOLE 1 C1 1 0.926094 0.084522 0.204245 11.00000 0.01493 0.02128 = 0.01615 -0.00366 0.00390 -0.00299 C2 1 0.722428 0.127538 0.190070 11.00000 0.01485 0.02587 = 0.01485 0.00006 0.00559 0.00089 AFIX 13 H2 2 0.681400 0.136778 0.237304 11.00000 -1.20000 AFIX 0 C3 1 0.619202 -0.036372 0.146653 11.00000 0.01182 0.02748 = 0.01729 0.00001 0.00398 0.00125 AFIX 13 H3 2 0.624999 -0.149809 0.178680 11.00000 -1.20000 AFIX 0 C4 1 0.422209 0.022501 0.124912 11.00000 0.01471 0.02158 = 0.01965 -0.00336 0.00305 -0.00310 O1A 4 0.989732 -0.007830 0.259057 11.00000 0.01443 0.02960 = 0.01888 0.00494 0.00192 0.00066 O1B 4 1.016388 0.143679 0.158076 11.00000 0.01333 0.03170 = 0.01931 0.00373 0.00603 0.00091 O2 4 0.684428 0.301602 0.153135 11.00000 0.01925 0.02446 = 0.01980 0.00036 0.00560 0.00424 AFIX 147 H2A 2 0.638822 0.377649 0.178954 11.00000 -1.50000 AFIX 0 O3 4 0.696008 -0.085235 0.086588 11.00000 0.01648 0.03521 = 0.01735 -0.00453 0.00424 0.00302 AFIX 147 H3A 2 0.628743 -0.046685 0.048943 11.00000 -1.50000 AFIX 0 O4A 4 0.343827 0.037373 0.180620 11.00000 0.01212 0.03945 = 0.01657 0.00146 0.00393 0.00234 AFIX 147 H4A 2 0.234970 0.068016 0.167066 11.00000 0.06062 AFIX 0 O4B 4 0.353685 0.054115 0.062835 11.00000 0.01644 0.04027 = 0.01700 -0.00083 0.00184 0.00157 MOLE 2 C22 1 0.963203 0.265334 -0.028150 11.00000 0.02052 0.02497 = 0.02329 0.00082 0.00535 -0.00026 AFIX 43 H22 2 1.075645 0.201700 -0.025303 11.00000 -1.20000 AFIX 0 C24 1 0.715642 0.380916 -0.000188 11.00000 0.02448 0.04838 = 0.02785 0.00652 0.01066 0.01111 AFIX 43 H24 2 0.624060 0.412355 0.026351 11.00000 -1.20000 AFIX 0 C25 1 0.716396 0.425567 -0.069290 11.00000 0.02203 0.04595 = 0.02627 0.00682 0.00352 0.01008 AFIX 43 H25 2 0.625947 0.494635 -0.100541 11.00000 -1.20000 AFIX 0 C26 1 0.929398 0.369632 -0.155654 11.00000 0.03754 0.03479 = 0.01823 0.00186 0.01305 -0.00095 AFIX 137 H26A 2 1.057633 0.336005 -0.150274 11.00000 -1.50000 H26B 2 0.911700 0.500427 -0.172981 11.00000 -1.50000 H26C 2 0.857277 0.283763 -0.190280 11.00000 -1.50000 AFIX 0 N21 3 0.871864 0.352712 -0.085908 11.00000 0.02177 0.02811 = 0.01888 0.00106 0.00583 -0.00150 N23 3 0.870477 0.282266 0.024727 11.00000 0.02144 0.03177 = 0.01906 0.00254 0.00331 0.00263 AFIX 43 H23 2 0.903313 0.237386 0.068551 11.00000 0.05239 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0082p21n in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - O2 C1 C3 C3 - O3 C4 C2 C4 - O4B O4A C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C22 - N23 N21 C24 - C25 N23 C25 - C24 N21 C26 - N21 N21 - C22 C25 C26 N23 - C22 C24 Operators for generating equivalent atoms: $1 x-1, y, z $2 -x+1, -y, -z $3 -x+3/2, y+1/2, -z+1/2 h k l Fo^2 Sigma Why rejected 3 0 0 15.26 3.48 observed but should be systematically absent 3 0 0 11.81 2.60 observed but should be systematically absent 3 0 0 20.45 4.86 observed but should be systematically absent 3 0 2 21.07 3.52 observed but should be systematically absent 3 0 2 14.56 2.23 observed but should be systematically absent 3 0 2 15.82 3.77 observed but should be systematically absent 28732 Reflections read, of which 1240 rejected -9 =< h =< 9, -9 =< k =< 9, -24 =< l =< 24, Max. 2-theta = 54.97 6 Systematic absence violations 0 Inconsistent equivalents 2266 Unique reflections, of which 0 suppressed R(int) = 0.0660 R(sigma) = 0.0328 Friedel opposites merged Maximum memory for data reduction = 1725 / 22717 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 = 2140 / 189095 wR2 = 0.1134 before cycle 1 for 2266 data and 151 / 151 parameters GooF = S = 1.124; Restrained GooF = 1.124 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0224 * P )^2 + 1.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.88352 0.00194 -0.003 OSF Mean shift/esd = 0.002 Maximum = -0.005 for U23 O1A Max. shift = 0.000 A for O4B Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2140 / 189095 wR2 = 0.1134 before cycle 2 for 2266 data and 151 / 151 parameters GooF = S = 1.124; Restrained GooF = 1.124 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0224 * P )^2 + 1.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.88353 0.00194 0.001 OSF Mean shift/esd = 0.001 Maximum = -0.002 for U23 O1A Max. shift = 0.000 A for O4B Max. dU = 0.000 for H23 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2140 / 189095 wR2 = 0.1134 before cycle 3 for 2266 data and 151 / 151 parameters GooF = S = 1.124; Restrained GooF = 1.124 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0224 * P )^2 + 1.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.88353 0.00194 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H3A Max. dU = 0.000 for H23 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2140 / 189095 wR2 = 0.1134 before cycle 4 for 2266 data and 151 / 151 parameters GooF = S = 1.124; Restrained GooF = 1.124 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0224 * P )^2 + 1.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.88353 0.00194 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1B Max. shift = 0.000 A for H4A Max. dU = 0.000 for H4A 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 0.6814 0.1368 0.2373 13 1.000 0.000 C2 O2 C1 C3 H3 0.6250 -0.1498 0.1787 13 1.000 0.000 C3 O3 C4 C2 H2A 0.6388 0.3776 0.1790 147 0.840 0.000 O2 C2 H2A H3A 0.6287 -0.0467 0.0489 147 0.840 0.000 O3 C3 H3A H4A 0.2350 0.0680 0.1671 147 0.840 0.000 O4A C4 H4A H22 1.0756 0.2017 -0.0253 43 0.950 0.000 C22 N23 N21 H24 0.6241 0.4124 0.0264 43 0.950 0.000 C24 C25 N23 H25 0.6259 0.4946 -0.1005 43 0.950 0.000 C25 C24 N21 H26A 1.0576 0.3360 -0.1503 137 0.980 0.000 C26 N21 H26A H26B 0.9117 0.5004 -0.1730 137 0.980 0.000 C26 N21 H26A H26C 0.8573 0.2838 -0.1903 137 0.980 0.000 C26 N21 H26A H23 0.9033 0.2374 0.0686 43 0.880 0.000 N23 C22 C24 06skc0082p21n in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.92609 0.08452 0.20425 1.00000 0.01493 0.02128 0.01615 -0.00366 0.00390 -0.00299 0.01732 0.00374 0.00027 0.00031 0.00011 0.00000 0.00095 0.00109 0.00098 0.00085 0.00076 0.00081 0.00043 C2 0.72243 0.12754 0.19007 1.00000 0.01485 0.02587 0.01485 0.00006 0.00559 0.00089 0.01816 0.00390 0.00027 0.00032 0.00011 0.00000 0.00096 0.00116 0.00097 0.00087 0.00076 0.00086 0.00044 H2 0.68140 0.13678 0.23730 1.00000 0.02180 0.00000 0.00000 C3 0.61920 -0.03637 0.14665 1.00000 0.01182 0.02748 0.01729 0.00001 0.00398 0.00125 0.01870 0.00390 0.00026 0.00033 0.00011 0.00000 0.00092 0.00121 0.00103 0.00089 0.00076 0.00085 0.00045 H3 0.62500 -0.14981 0.17868 1.00000 0.02244 0.00000 0.00000 C4 0.42221 0.02250 0.12491 1.00000 0.01471 0.02158 0.01965 -0.00336 0.00305 -0.00310 0.01866 0.00378 0.00027 0.00031 0.00011 0.00000 0.00095 0.00113 0.00107 0.00087 0.00079 0.00083 0.00044 O1A 0.98973 -0.00783 0.25906 1.00000 0.01443 0.02960 0.01888 0.00494 0.00192 0.00066 0.02111 0.00280 0.00019 0.00023 0.00008 0.00000 0.00070 0.00088 0.00076 0.00065 0.00056 0.00063 0.00035 O1B 1.01639 0.14368 0.15808 1.00000 0.01333 0.03170 0.01931 0.00373 0.00603 0.00091 0.02106 0.00283 0.00019 0.00023 0.00008 0.00000 0.00069 0.00091 0.00074 0.00067 0.00056 0.00064 0.00035 O2 0.68443 0.30160 0.15313 1.00000 0.01925 0.02446 0.01980 0.00036 0.00560 0.00424 0.02091 0.00290 0.00020 0.00023 0.00008 0.00000 0.00075 0.00085 0.00077 0.00065 0.00059 0.00064 0.00035 H2A 0.63882 0.37765 0.17895 1.00000 0.03137 0.00000 0.00000 O3 0.69601 -0.08524 0.08659 1.00000 0.01648 0.03521 0.01735 -0.00453 0.00424 0.00302 0.02287 0.00286 0.00020 0.00024 0.00008 0.00000 0.00073 0.00096 0.00075 0.00069 0.00058 0.00066 0.00036 H3A 0.62874 -0.04669 0.04894 1.00000 0.03430 0.00000 0.00000 O4A 0.34383 0.03737 0.18062 1.00000 0.01212 0.03945 0.01657 0.00146 0.00393 0.00234 0.02255 0.00288 0.00019 0.00025 0.00008 0.00000 0.00072 0.00099 0.00074 0.00068 0.00056 0.00067 0.00036 H4A 0.23497 0.06802 0.16707 1.00000 0.06062 0.00000 0.01061 O4B 0.35369 0.05412 0.06283 1.00000 0.01644 0.04027 0.01700 -0.00083 0.00184 0.00157 0.02472 0.00290 0.00020 0.00025 0.00008 0.00000 0.00074 0.00101 0.00076 0.00070 0.00059 0.00069 0.00038 C22 0.96320 0.26533 -0.02815 1.00000 0.02052 0.02497 0.02329 0.00082 0.00535 -0.00026 0.02276 0.00415 0.00030 0.00033 0.00012 0.00000 0.00107 0.00125 0.00110 0.00093 0.00086 0.00091 0.00048 H22 1.07564 0.20170 -0.02530 1.00000 0.02731 0.00000 0.00000 C24 0.71564 0.38092 -0.00019 1.00000 0.02448 0.04838 0.02785 0.00652 0.01066 0.01111 0.03283 0.00505 0.00033 0.00041 0.00013 0.00000 0.00117 0.00165 0.00128 0.00118 0.00098 0.00115 0.00060 H24 0.62406 0.41235 0.02635 1.00000 0.03939 0.00000 0.00000 C25 0.71640 0.42557 -0.06929 1.00000 0.02203 0.04595 0.02627 0.00682 0.00352 0.01008 0.03153 0.00492 0.00032 0.00041 0.00013 0.00000 0.00116 0.00160 0.00125 0.00114 0.00095 0.00109 0.00059 H25 0.62595 0.49463 -0.10054 1.00000 0.03783 0.00000 0.00000 C26 0.92940 0.36963 -0.15565 1.00000 0.03754 0.03479 0.01823 0.00186 0.01305 -0.00095 0.02918 0.00477 0.00034 0.00038 0.00012 0.00000 0.00135 0.00141 0.00112 0.00102 0.00099 0.00112 0.00055 H26A 1.05763 0.33600 -0.15027 1.00000 0.04377 0.00000 0.00000 H26B 0.91170 0.50043 -0.17298 1.00000 0.04377 0.00000 0.00000 H26C 0.85728 0.28376 -0.19028 1.00000 0.04377 0.00000 0.00000 N21 0.87186 0.35271 -0.08591 1.00000 0.02177 0.02811 0.01888 0.00106 0.00583 -0.00150 0.02266 0.00349 0.00025 0.00029 0.00010 0.00000 0.00092 0.00107 0.00091 0.00081 0.00072 0.00080 0.00042 N23 0.87048 0.28227 0.02473 1.00000 0.02144 0.03177 0.01906 0.00254 0.00331 0.00263 0.02414 0.00358 0.00025 0.00030 0.00010 0.00000 0.00094 0.00112 0.00097 0.00084 0.00074 0.00083 0.00043 H23 0.90331 0.23739 0.06855 1.00000 0.05239 0.00000 0.00952 Final Structure Factor Calculation for 06skc0082p21n in P2(1)/n Total number of l.s. parameters = 151 Maximum vector length = 511 Memory required = 1989 / 22995 wR2 = 0.1134 before cycle 5 for 2266 data and 0 / 151 parameters GooF = S = 1.124; Restrained GooF = 1.124 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0224 * P )^2 + 1.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0572 for 1903 Fo > 4sig(Fo) and 0.0717 for all 2266 data wR2 = 0.1134, GooF = S = 1.124, Restrained GooF = 1.124 for all data Occupancy sum of asymmetric unit = 16.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0239 0.0144 0.0137 C1 0.0259 0.0172 0.0113 C2 0.0276 0.0174 0.0111 C3 0.0244 0.0181 0.0134 C4 0.0316 0.0176 0.0142 O1A 0.0328 0.0191 0.0113 O1B 0.0269 0.0202 0.0156 O2 0.0369 0.0178 0.0139 O3 0.0397 0.0166 0.0113 O4A 0.0404 0.0181 0.0156 O4B 0.0253 0.0234 0.0196 C22 0.0543 0.0267 0.0176 C24 0.0505 0.0263 0.0177 C25 0.0392 0.0350 0.0133 C26 0.0285 0.0224 0.0170 N21 0.0327 0.0213 0.0184 N23 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.026 0.037 0.051 0.067 0.085 0.106 0.142 0.206 1.000 Number in group 246. 218. 220. 232. 227. 222. 220. 229. 228. 224. GooF 1.398 1.311 1.199 1.183 1.034 0.952 0.982 0.978 1.018 1.065 K 5.622 1.934 1.285 1.109 1.051 1.004 0.998 0.989 0.992 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.66 inf Number in group 227. 227. 228. 224. 229. 225. 227. 225. 228. 226. GooF 1.127 1.142 1.113 1.100 1.170 1.064 1.029 1.055 1.067 1.339 K 1.036 1.058 1.070 1.045 1.024 1.003 0.990 0.984 1.010 1.007 R1 0.172 0.158 0.133 0.117 0.102 0.069 0.048 0.052 0.037 0.029 Recommended weighting scheme: WGHT 0.0224 1.4341 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) -1 0 7 393.20 292.52 3.87 0.159 2.66 3 6 0 41.24 12.74 3.79 0.033 1.06 -1 1 21 66.42 22.60 3.67 0.044 0.89 -6 6 6 27.53 2.40 3.57 0.014 0.85 2 2 0 11.42 1.10 3.42 0.010 2.55 4 1 1 9.23 0.13 3.41 0.003 1.75 -2 7 14 26.66 2.22 3.20 0.014 0.80 -1 7 11 36.44 4.85 3.08 0.021 0.87 1 1 0 894.94 1039.37 2.98 0.300 5.10 5 2 12 14.39 0.18 2.95 0.004 0.95 7 3 7 74.82 38.81 2.92 0.058 0.86 -2 1 9 335.38 266.99 2.85 0.152 1.89 -2 2 19 28.13 5.79 2.84 0.022 0.96 -2 1 1 901.29 1039.22 2.82 0.300 3.32 -7 3 7 14.88 0.72 2.82 0.008 0.96 -7 0 19 32.62 6.16 2.78 0.023 0.79 0 9 3 33.19 7.99 2.76 0.026 0.78 3 2 18 44.48 20.42 2.73 0.042 0.87 -3 7 13 43.39 16.02 2.70 0.037 0.81 -2 2 3 35.80 18.26 2.67 0.040 2.47 0 5 13 17.86 1.17 2.66 0.010 1.00 6 3 8 25.73 5.15 2.65 0.021 0.93 -5 1 2 178.30 232.31 2.65 0.142 1.47 -6 1 5 85.26 129.32 2.64 0.106 1.22 5 5 6 16.90 3.12 2.62 0.016 0.94 1 4 0 303.74 371.87 2.59 0.180 1.72 0 4 18 42.66 18.79 2.58 0.040 0.89 2 5 4 10.41 1.02 2.57 0.009 1.25 1 1 1 3569.79 3897.53 2.57 0.582 4.77 1 7 13 29.25 7.58 2.56 0.026 0.81 -8 1 12 -3.70 10.54 2.53 0.030 0.86 6 2 0 17.18 3.66 2.51 0.018 1.16 1 3 7 87.12 59.06 2.51 0.072 1.67 4 2 19 -5.09 9.09 2.51 0.028 0.79 0 8 4 55.96 24.64 2.48 0.046 0.87 5 6 9 19.12 0.43 2.48 0.006 0.81 -8 0 8 34.13 11.88 2.45 0.032 0.92 1 0 5 77.15 110.24 2.44 0.098 3.10 -7 2 10 12.93 0.03 2.44 0.002 0.96 -1 1 5 894.77 1011.76 2.43 0.296 3.21 0 6 3 13.35 3.12 2.43 0.016 1.16 2 3 5 5.73 0.01 2.42 0.001 1.68 -1 2 11 9.09 1.77 2.41 0.012 1.55 -3 6 11 10.68 0.23 2.39 0.004 0.93 -3 6 5 20.01 5.89 2.39 0.023 1.04 1 0 11 756.93 657.57 2.36 0.239 1.59 -7 2 15 87.81 53.82 2.35 0.068 0.86 -6 1 7 22.25 8.56 2.35 0.027 1.19 -3 3 6 47.63 28.49 2.35 0.050 1.58 3 3 13 10.42 0.05 2.35 0.002 1.03 Bond lengths and angles C1 - Distance Angles O1A 1.2442 (0.0026) O1B 1.2713 (0.0025) 124.95 (0.19) C2 1.5358 (0.0028) 117.91 (0.18) 117.13 (0.18) C1 - O1A O1B C2 - Distance Angles O2 1.4159 (0.0027) C1 1.5358 (0.0028) 111.23 (0.17) C3 1.5430 (0.0030) 110.51 (0.16) 109.47 (0.17) H2 1.0000 108.52 108.52 108.52 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4092 (0.0024) C4 1.5207 (0.0028) 111.79 (0.17) C2 1.5430 (0.0030) 111.87 (0.17) 108.03 (0.17) H3 1.0000 108.34 108.34 108.34 C3 - O3 C4 C2 C4 - Distance Angles O4B 1.2143 (0.0025) O4A 1.3031 (0.0025) 126.43 (0.19) C3 1.5207 (0.0028) 122.12 (0.19) 111.43 (0.17) C4 - O4B O4A O1A - Distance Angles C1 1.2442 (0.0026) O1A - O1B - Distance Angles C1 1.2713 (0.0025) O1B - O2 - Distance Angles C2 1.4159 (0.0027) H2A 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4092 (0.0024) H3A 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.3031 (0.0025) H4A 0.8400 109.47 O4A - C4 O4B - Distance Angles C4 1.2143 (0.0025) O4B - C22 - Distance Angles N23 1.3259 (0.0029) N21 1.3312 (0.0029) 108.35 (0.20) H22 0.9500 125.82 125.82 C22 - N23 N21 C24 - Distance Angles C25 1.3465 (0.0034) N23 1.3642 (0.0030) 107.46 (0.21) H24 0.9500 126.27 126.27 C24 - C25 N23 C25 - Distance Angles C24 1.3465 (0.0034) N21 1.3654 (0.0030) 106.97 (0.21) H25 0.9500 126.51 126.51 C25 - C24 N21 C26 - Distance Angles N21 1.4676 (0.0027) 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 N21 - Distance Angles C22 1.3312 (0.0029) C25 1.3654 (0.0030) 108.65 (0.19) C26 1.4676 (0.0027) 125.72 (0.20) 125.63 (0.20) N21 - C22 C25 N23 - Distance Angles C22 1.3259 (0.0029) C24 1.3642 (0.0030) 108.57 (0.19) H23 0.8800 125.72 125.72 N23 - C22 C24 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.87 2.742(2) 169.4 N23-H23...O1B 0.88 2.54 3.022(2) 115.3 N23-H23...O2 0.84 2.25 2.715(2) 115.3 O3-H3A...O4B 0.84 1.71 2.534(2) 167.9 O4A-H4A...O1B_$1 0.84 2.14 2.793(2) 133.9 O3-H3A...O4B_$2 0.84 1.84 2.661(2) 166.0 O2-H2A...O1A_$3 FMAP and GRID set by program FMAP 2 3 24 GRID -1.190 -2 -2 1.190 2 2 R1 = 0.0716 for 2266 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.31 at 0.8188 0.1002 0.1900 [ 0.75 A from C2 ] Deepest hole -0.25 at 0.9212 0.2236 0.2241 [ 1.05 A from C1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 1940 / 15279 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8188 0.1002 0.1900 1.00000 0.05 0.31 0.75 C2 0.81 C1 1.51 H2 1.73 O1B Q2 1 0.6997 0.5654 -0.0868 1.00000 0.05 0.30 0.76 H25 1.04 C25 1.98 N21 2.08 C24 Q3 1 0.6766 0.0460 0.1713 1.00000 0.05 0.26 0.73 C2 0.82 C3 1.40 H2 1.45 H3 Q4 1 0.8171 0.4031 -0.2132 1.00000 0.05 0.25 0.97 H26C 1.17 H26B 1.27 C26 2.03 H26A Q5 1 0.6768 0.5247 -0.0214 1.00000 0.05 0.22 1.11 C24 1.22 C25 1.32 H24 1.49 H25 Q6 1 0.6643 -0.2039 0.1544 1.00000 0.05 0.21 0.70 H3 1.23 C3 1.59 O3 2.26 H3A Q7 1 1.0042 0.5036 -0.1555 1.00000 0.05 0.20 0.71 H26B 1.10 C26 1.25 H26A 1.95 H26C Q8 1 0.5143 -0.0112 0.1405 1.00000 0.05 0.20 0.74 C4 0.80 C3 1.40 H3 1.64 O4A Q9 1 0.3954 0.3957 -0.1189 1.00000 0.05 0.20 1.84 H25 1.95 H2A 2.06 H3 2.24 H24 Q10 1 1.1394 0.2191 0.1549 1.00000 0.05 0.20 1.08 O1B 1.28 H4A 1.99 O4A 2.06 H26B Shortest distances between peaks (including symmetry equivalents) 1 3 1.13 2 5 1.31 3 8 1.32 6 9 1.54 6 8 1.75 4 7 1.76 3 6 1.79 7 10 2.23 1 8 2.44 2 10 2.45 1 6 2.47 2 9 2.56 5 9 2.70 4 10 2.75 1 10 2.75 8 9 2.84 5 9 2.86 2 7 2.87 4 10 2.88 2 4 2.93 5 5 2.94 7 9 2.99 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 0.02: Analyse other restraints etc. 1.31: 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 0.39: Structure factors and derivatives 0.36: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0082p21n finished at 14:42:51 Total CPU time: 2.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++