+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0073p21n started at 13:14:28 on 06-May-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0073p21n in P2(1)/n CELL 0.71073 8.6426 6.0715 18.9467 90.000 102.765 90.000 ZERR 4.00 0.0005 0.0005 0.0014 0.000 0.005 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 28 64 8 16 V = 969.63 F(000) = 416.0 Mu = 0.11 mm-1 Cell Wt = 768.87 Rho = 1.317 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB N21 O5A EQIV_$1 -x+3/2, y-1/2, -z+1/2 HTAB N21 O5A_$1 EQIV_$2 x+1/2, -y+1/2, z+1/2 HTAB N21 O1A_$2 HTAB N24 O1B_$2 EQIV_$3 x+1/2, -y-1/2, z+1/2 HTAB N24 O1A_$3 EQIV_$4 -x+1/2, y-3/2, -z+1/2 HTAB N24 O1B_$4 EQIV_$5 -x+1/2, y-1/2, -z+1/2 HTAB N24 O5B_$5 FMAP 2 PLAN 10 SIZE 0.03 0.14 0.27 ACTA CONF MPLA O1A O1B C1 MPLA O5A O5B C5 BOND $H WGHT 0.05810 0.11650 L.S. 4 TEMP -153.00 FVAR 0.92425 MOLE 1 C1 1 0.160198 0.579149 -0.021273 11.00000 0.01808 0.02075 = 0.02211 -0.00035 0.00644 -0.00305 C2 1 0.272830 0.473005 0.042345 11.00000 0.02204 0.02527 = 0.02289 -0.00169 0.00308 0.00039 AFIX 23 H2A 2 0.354449 0.582400 0.064095 11.00000 -1.20000 H2B 2 0.212637 0.434283 0.079397 11.00000 -1.20000 AFIX 0 C3 1 0.355254 0.268489 0.023712 11.00000 0.02543 0.02589 = 0.01903 0.00269 0.00564 0.00155 AFIX 23 H3A 2 0.382000 0.289691 -0.024016 11.00000 -1.20000 H3B 2 0.281094 0.142454 0.019493 11.00000 -1.20000 AFIX 0 C4 1 0.506085 0.212570 0.079280 11.00000 0.02263 0.02546 = 0.02667 0.00200 0.00627 0.00179 AFIX 23 H4A 2 0.565920 0.102651 0.057365 11.00000 -1.20000 H4B 2 0.571993 0.347332 0.088293 11.00000 -1.20000 AFIX 0 C5 1 0.488544 0.124421 0.151266 11.00000 0.02356 0.01740 = 0.02348 -0.00034 0.00587 0.00082 O1A 4 0.105020 0.466788 -0.076476 11.00000 0.02853 0.02277 = 0.02034 -0.00016 0.00093 -0.00299 O1B 4 0.128923 0.779601 -0.015139 11.00000 0.03317 0.02031 = 0.02616 -0.00036 0.00432 0.00628 O5A 4 0.617146 0.106434 0.199186 11.00000 0.02194 0.03109 = 0.02343 0.00627 0.00148 -0.00229 O5B 4 0.357333 0.070338 0.162371 11.00000 0.02146 0.04116 = 0.02954 0.01020 0.00607 -0.00389 MOLE 2 C22 1 0.473681 -0.372267 0.273065 11.00000 0.02301 0.02771 = 0.01962 -0.00057 0.00223 -0.00341 AFIX 23 H22A 2 0.476110 -0.409522 0.222451 11.00000 -1.20000 H22B 2 0.367669 -0.310685 0.273173 11.00000 -1.20000 AFIX 0 C23 1 0.497677 -0.578466 0.317782 11.00000 0.02584 0.02267 = 0.02303 -0.00331 0.00546 -0.00090 AFIX 23 H23A 2 0.432992 -0.698151 0.290499 11.00000 -1.20000 H23B 2 0.610473 -0.622924 0.326118 11.00000 -1.20000 AFIX 0 N21 3 0.596137 -0.202493 0.300087 11.00000 0.02051 0.02169 = 0.02024 0.00352 0.00276 0.00078 AFIX 137 H21A 2 0.694223 -0.264490 0.307144 11.00000 0.02864 H21B 2 0.581193 -0.146878 0.342683 11.00000 0.06254 H21C 2 0.588035 -0.092075 0.266993 11.00000 0.03672 AFIX 0 N24 3 0.453825 -0.551461 0.388474 11.00000 0.02257 0.02257 = 0.02247 0.00016 0.00669 -0.00287 AFIX 137 H24A 2 0.513266 -0.442094 0.413939 11.00000 0.05458 H24B 2 0.472042 -0.679733 0.413795 11.00000 0.05879 H24C 2 0.349192 -0.515946 0.381170 11.00000 0.04209 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0073p21n 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 - C5 C3 C5 - O5B O5A C4 O1A - C1 O1B - C1 O5A - C5 O5B - C5 C22 - N21 C23 C23 - N24 C22 N21 - C22 N24 - C23 Operators for generating equivalent atoms: $1 -x+3/2, y-1/2, -z+1/2 $2 x+1/2, -y+1/2, z+1/2 $3 x+1/2, -y-1/2, z+1/2 $4 -x+1/2, y-3/2, -z+1/2 $5 -x+1/2, y-1/2, -z+1/2 15359 Reflections read, of which 760 rejected -11 =< h =< 10, -7 =< k =< 7, -24 =< l =< 24, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 2218 Unique reflections, of which 0 suppressed R(int) = 0.1419 R(sigma) = 0.1091 Friedel opposites merged Maximum memory for data reduction = 1916 / 22001 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 = 2294 / 160020 wR2 = 0.1459 before cycle 1 for 2218 data and 126 / 126 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0581 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92422 0.00293 -0.009 OSF Mean shift/esd = 0.003 Maximum = -0.009 for OSF Max. shift = 0.000 A for H21B Max. dU = 0.000 for H21A Least-squares cycle 2 Maximum vector length = 511 Memory required = 2294 / 160020 wR2 = 0.1459 before cycle 2 for 2218 data and 126 / 126 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0581 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92421 0.00293 -0.005 OSF Mean shift/esd = 0.001 Maximum = -0.005 for OSF Max. shift = 0.000 A for H24A Max. dU = 0.000 for H24A Least-squares cycle 3 Maximum vector length = 511 Memory required = 2294 / 160020 wR2 = 0.1459 before cycle 3 for 2218 data and 126 / 126 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0581 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92421 0.00293 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H24A Max. dU = 0.000 for H24A Least-squares cycle 4 Maximum vector length = 511 Memory required = 2294 / 160020 wR2 = 0.1459 before cycle 4 for 2218 data and 126 / 126 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0581 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92421 0.00293 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C23 Max. dU = 0.000 for H24A 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 0.3544 0.5824 0.0641 23 0.990 0.000 C2 C3 C1 H2B 0.2126 0.4343 0.0794 23 0.990 0.000 C2 C3 C1 H3A 0.3820 0.2897 -0.0240 23 0.990 0.000 C3 C2 C4 H3B 0.2811 0.1425 0.0195 23 0.990 0.000 C3 C2 C4 H4A 0.5659 0.1027 0.0574 23 0.990 0.000 C4 C5 C3 H4B 0.5720 0.3473 0.0883 23 0.990 0.000 C4 C5 C3 H22A 0.4761 -0.4095 0.2225 23 0.990 0.000 C22 N21 C23 H22B 0.3677 -0.3107 0.2732 23 0.990 0.000 C22 N21 C23 H23A 0.4330 -0.6982 0.2905 23 0.990 0.000 C23 N24 C22 H23B 0.6105 -0.6229 0.3261 23 0.990 0.000 C23 N24 C22 H21A 0.6942 -0.2645 0.3071 137 0.910 0.000 N21 C22 H21A H21B 0.5812 -0.1469 0.3427 137 0.910 0.000 N21 C22 H21A H21C 0.5880 -0.0921 0.2670 137 0.910 0.000 N21 C22 H21A H24A 0.5133 -0.4421 0.4139 137 0.910 0.000 N24 C23 H24A H24B 0.4720 -0.6797 0.4138 137 0.910 0.000 N24 C23 H24A H24C 0.3492 -0.5159 0.3812 137 0.910 0.000 N24 C23 H24A 06skc0073p21n in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.16020 0.57915 -0.02127 1.00000 0.01808 0.02075 0.02211 -0.00035 0.00644 -0.00305 0.02000 0.00460 0.00026 0.00043 0.00014 0.00000 0.00124 0.00154 0.00144 0.00120 0.00106 0.00102 0.00058 C2 0.27283 0.47300 0.04235 1.00000 0.02204 0.02527 0.02288 -0.00168 0.00308 0.00039 0.02369 0.00482 0.00029 0.00044 0.00014 0.00000 0.00130 0.00155 0.00148 0.00117 0.00110 0.00106 0.00062 H2A 0.35445 0.58240 0.06410 1.00000 0.02843 0.00000 0.00000 H2B 0.21264 0.43428 0.07940 1.00000 0.02843 0.00000 0.00000 C3 0.35525 0.26849 0.02371 1.00000 0.02542 0.02589 0.01902 0.00269 0.00564 0.00155 0.02333 0.00481 0.00028 0.00044 0.00014 0.00000 0.00136 0.00156 0.00138 0.00118 0.00109 0.00108 0.00061 H3A 0.38200 0.28969 -0.02402 1.00000 0.02800 0.00000 0.00000 H3B 0.28109 0.14245 0.01949 1.00000 0.02800 0.00000 0.00000 C4 0.50608 0.21257 0.07928 1.00000 0.02263 0.02545 0.02666 0.00200 0.00627 0.00179 0.02479 0.00481 0.00028 0.00045 0.00014 0.00000 0.00133 0.00153 0.00150 0.00123 0.00110 0.00109 0.00062 H4A 0.56592 0.10265 0.05737 1.00000 0.02974 0.00000 0.00000 H4B 0.57199 0.34733 0.08829 1.00000 0.02974 0.00000 0.00000 C5 0.48854 0.12442 0.15127 1.00000 0.02356 0.01739 0.02347 -0.00034 0.00586 0.00082 0.02137 0.00468 0.00029 0.00041 0.00014 0.00000 0.00141 0.00138 0.00144 0.00115 0.00113 0.00106 0.00058 O1A 0.10502 0.46678 -0.07648 1.00000 0.02853 0.02276 0.02034 -0.00016 0.00093 -0.00299 0.02457 0.00319 0.00019 0.00029 0.00009 0.00000 0.00098 0.00105 0.00101 0.00084 0.00079 0.00075 0.00046 O1B 0.12892 0.77960 -0.01514 1.00000 0.03316 0.02030 0.02615 -0.00035 0.00432 0.00628 0.02688 0.00330 0.00020 0.00030 0.00009 0.00000 0.00101 0.00109 0.00107 0.00083 0.00081 0.00078 0.00047 O5A 0.61715 0.10643 0.19919 1.00000 0.02193 0.03108 0.02342 0.00627 0.00148 -0.00229 0.02603 0.00323 0.00019 0.00029 0.00009 0.00000 0.00090 0.00115 0.00100 0.00086 0.00077 0.00077 0.00046 O5B 0.35733 0.07034 0.16237 1.00000 0.02145 0.04115 0.02954 0.01020 0.00607 -0.00389 0.03065 0.00339 0.00020 0.00031 0.00010 0.00000 0.00097 0.00126 0.00111 0.00095 0.00079 0.00083 0.00050 C22 0.47368 -0.37227 0.27306 1.00000 0.02300 0.02771 0.01961 -0.00057 0.00223 -0.00342 0.02383 0.00454 0.00028 0.00043 0.00014 0.00000 0.00131 0.00156 0.00138 0.00119 0.00107 0.00110 0.00061 H22A 0.47611 -0.40952 0.22245 1.00000 0.02859 0.00000 0.00000 H22B 0.36767 -0.31069 0.27317 1.00000 0.02859 0.00000 0.00000 C23 0.49768 -0.57847 0.31778 1.00000 0.02584 0.02267 0.02302 -0.00331 0.00546 -0.00090 0.02383 0.00472 0.00029 0.00042 0.00014 0.00000 0.00138 0.00152 0.00143 0.00122 0.00110 0.00109 0.00061 H23A 0.43299 -0.69815 0.29050 1.00000 0.02860 0.00000 0.00000 H23B 0.61047 -0.62293 0.32612 1.00000 0.02860 0.00000 0.00000 N21 0.59614 -0.20249 0.30009 1.00000 0.02051 0.02168 0.02023 0.00352 0.00277 0.00078 0.02108 0.00371 0.00022 0.00035 0.00011 0.00000 0.00113 0.00123 0.00123 0.00101 0.00089 0.00091 0.00052 H21A 0.69422 -0.26449 0.30715 1.00000 0.02868 0.00000 0.00745 H21B 0.58119 -0.14687 0.34268 1.00000 0.06251 0.00000 0.01096 H21C 0.58804 -0.09208 0.26699 1.00000 0.03675 0.00000 0.00834 N24 0.45383 -0.55146 0.38847 1.00000 0.02256 0.02257 0.02246 0.00015 0.00669 -0.00287 0.02227 0.00396 0.00023 0.00037 0.00011 0.00000 0.00119 0.00126 0.00123 0.00106 0.00090 0.00094 0.00052 H24A 0.51327 -0.44210 0.41394 1.00000 0.05454 0.00000 0.01008 H24B 0.47204 -0.67974 0.41379 1.00000 0.05883 0.00000 0.01049 H24C 0.34919 -0.51594 0.38117 1.00000 0.04206 0.00000 0.00905 Final Structure Factor Calculation for 06skc0073p21n in P2(1)/n Total number of l.s. parameters = 126 Maximum vector length = 511 Memory required = 2168 / 22995 wR2 = 0.1459 before cycle 5 for 2218 data and 0 / 126 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0581 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0603 for 1271 Fo > 4sig(Fo) and 0.1330 for all 2218 data wR2 = 0.1459, GooF = S = 1.033, Restrained GooF = 1.033 for all data Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0235 0.0213 0.0152 C1 0.0269 0.0234 0.0208 C2 0.0276 0.0244 0.0179 C3 0.0284 0.0243 0.0217 C4 0.0241 0.0228 0.0172 C5 0.0326 0.0223 0.0188 O1A 0.0370 0.0259 0.0177 O1B 0.0366 0.0223 0.0191 O5A 0.0483 0.0251 0.0186 O5B 0.0298 0.0233 0.0184 C22 0.0264 0.0256 0.0195 C23 0.0249 0.0214 0.0169 N21 0.0256 0.0226 0.0186 N24 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.022 0.031 0.042 0.055 0.070 0.090 0.119 0.174 1.000 Number in group 228. 243. 200. 230. 211. 219. 223. 219. 228. 217. GooF 0.943 0.904 0.948 0.971 1.106 1.079 1.068 1.210 1.092 0.986 K 2.574 0.594 0.833 0.952 1.052 0.996 0.982 1.001 1.005 0.990 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 231. 223. 217. 223. 216. 226. 218. 222. 222. 220. GooF 0.903 0.891 0.906 1.016 1.068 1.009 1.109 0.965 1.036 1.357 K 0.879 1.059 1.101 0.993 1.025 0.963 1.002 1.022 1.040 0.968 R1 0.355 0.317 0.255 0.236 0.165 0.140 0.078 0.063 0.054 0.039 Recommended weighting scheme: WGHT 0.0585 0.1195 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 3 187.40 329.36 6.28 0.163 4.52 1 1 6 55.30 32.13 4.05 0.051 2.47 1 1 4 109.22 78.25 3.68 0.079 3.17 6 0 10 13.54 123.28 3.63 0.100 1.02 -1 1 4 11.25 1.72 3.54 0.012 3.61 -1 0 5 43.00 13.04 3.53 0.032 3.70 1 3 14 67.51 112.49 3.42 0.095 1.07 -8 2 19 -64.09 79.63 3.34 0.080 0.78 0 2 2 75.09 49.29 3.27 0.063 2.88 -1 3 6 12.31 0.88 3.09 0.008 1.70 3 5 4 92.73 54.36 3.05 0.066 1.06 5 0 15 -6.17 38.69 3.05 0.056 0.90 2 3 14 151.57 205.42 3.02 0.129 1.02 2 6 13 151.27 22.89 2.90 0.043 0.79 2 0 4 83.67 115.70 2.87 0.097 2.82 2 6 6 51.69 7.23 2.81 0.024 0.92 -8 3 8 60.02 30.95 2.80 0.050 0.93 4 6 6 12.90 66.80 2.80 0.073 0.85 7 4 8 562.41 417.68 2.77 0.184 0.82 -8 2 2 43.61 71.04 2.75 0.076 1.01 -1 1 3 2603.55 3093.41 2.73 0.500 4.12 -5 1 5 84.52 107.39 2.72 0.093 1.62 -1 3 15 60.98 89.78 2.72 0.085 1.07 4 2 0 138.88 111.15 2.67 0.095 1.73 1 3 3 132.12 167.85 2.64 0.116 1.85 -8 0 18 38.58 100.95 2.63 0.090 0.83 0 1 17 71.68 106.30 2.63 0.093 1.07 2 1 16 101.34 141.45 2.62 0.107 1.04 2 0 2 97.48 125.79 2.62 0.101 3.55 0 1 5 726.72 616.80 2.57 0.223 3.16 -3 1 10 249.16 201.94 2.57 0.128 1.66 0 4 0 44.40 15.36 2.56 0.035 1.52 3 6 3 199.18 268.33 2.54 0.147 0.93 -9 4 2 85.00 29.23 2.54 0.049 0.81 2 0 0 5614.95 6597.04 2.52 0.730 4.21 -8 1 19 11.71 56.23 2.48 0.067 0.80 -5 0 15 69.31 104.22 2.45 0.092 1.12 -7 1 6 0.27 20.84 2.45 0.041 1.19 -6 2 18 42.25 10.21 2.42 0.029 0.89 -2 3 19 71.48 127.60 2.40 0.101 0.89 -3 3 15 0.18 21.70 2.40 0.042 1.05 9 2 1 2.04 37.20 2.39 0.055 0.88 -5 3 4 81.09 61.23 2.39 0.070 1.31 5 2 7 24.44 8.39 2.38 0.026 1.19 -3 5 12 25.97 0.63 2.38 0.007 0.94 1 2 0 11.19 0.41 2.37 0.006 2.86 -3 5 11 351.37 278.13 2.36 0.150 0.97 -2 0 12 -8.13 7.29 2.36 0.024 1.56 1 3 0 8.44 23.49 2.36 0.044 1.97 -8 4 15 96.50 53.50 2.34 0.066 0.78 Bond lengths and angles C1 - Distance Angles O1A 1.2516 (0.0029) O1B 1.2576 (0.0030) 123.69 (0.23) C2 1.5157 (0.0034) 119.47 (0.23) 116.83 (0.22) C1 - O1A O1B C2 - Distance Angles C3 1.5117 (0.0036) C1 1.5157 (0.0034) 114.62 (0.21) H2A 0.9900 108.61 108.61 H2B 0.9900 108.61 108.61 107.57 C2 - C3 C1 H2A C3 - Distance Angles C2 1.5117 (0.0036) C4 1.5220 (0.0032) 113.42 (0.22) H3A 0.9900 108.89 108.89 H3B 0.9900 108.89 108.89 107.72 C3 - C2 C4 H3A C4 - Distance Angles C5 1.5037 (0.0035) C3 1.5220 (0.0032) 117.66 (0.21) H4A 0.9900 107.89 107.89 H4B 0.9900 107.89 107.89 107.19 C4 - C5 C3 H4A C5 - Distance Angles O5B 1.2424 (0.0028) O5A 1.2750 (0.0029) 122.78 (0.24) C4 1.5037 (0.0035) 121.76 (0.22) 115.45 (0.21) C5 - O5B O5A O1A - Distance Angles C1 1.2516 (0.0029) O1A - O1B - Distance Angles C1 1.2576 (0.0030) O1B - O5A - Distance Angles C5 1.2750 (0.0029) O5A - O5B - Distance Angles C5 1.2424 (0.0028) O5B - C22 - Distance Angles N21 1.4850 (0.0030) C23 1.5002 (0.0036) 112.67 (0.20) H22A 0.9900 109.06 109.06 H22B 0.9900 109.06 109.06 107.82 C22 - N21 C23 H22A C23 - Distance Angles N24 1.4794 (0.0032) C22 1.5002 (0.0036) 112.81 (0.21) H23A 0.9900 109.03 109.03 H23B 0.9900 109.03 109.03 107.80 C23 - N24 C22 H23A N21 - Distance Angles C22 1.4850 (0.0030) H21A 0.9100 109.47 H21B 0.9100 109.47 109.47 H21C 0.9100 109.47 109.47 109.47 N21 - C22 H21A H21B N24 - Distance Angles C23 1.4794 (0.0032) H24A 0.9100 109.47 H24B 0.9100 109.47 109.47 H24C 0.9100 109.47 109.47 109.47 N24 - C23 H24A H24B Selected torsion angles 21.65 ( 0.33) O1A - C1 - C2 - C3 -157.68 ( 0.22) O1B - C1 - C2 - C3 159.38 ( 0.21) C1 - C2 - C3 - C4 72.00 ( 0.31) C2 - C3 - C4 - C5 9.56 ( 0.37) C3 - C4 - C5 - O5B -171.42 ( 0.22) C3 - C4 - C5 - O5A 74.11 ( 0.25) N21 - C22 - C23 - N24 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.82 2.713(3) 166.7 N21-H21C...O5A 0.91 1.84 2.733(3) 168.1 N21-H21A...O5A_$1 0.91 1.86 2.728(3) 159.9 N21-H21B...O1A_$2 0.91 1.78 2.670(3) 163.6 N24-H24A...O1B_$2 0.91 2.07 2.850(3) 142.6 N24-H24B...O1A_$3 0.91 2.29 2.843(3) 118.7 N24-H24B...O1B_$4 0.91 1.87 2.750(3) 162.5 N24-H24C...O5B_$5 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 7.6828 (0.0171) x + 1.5288 (0.0132) y - 10.7910 (0.0536) z = 2.3457 (0.0080) * 0.0000 (0.0000) O1A * 0.0000 (0.0000) O1B * 0.0000 (0.0000) C1 Rms deviation of fitted atoms = 0.0000 - 1.7415 (0.0147) x + 5.6177 (0.0106) y + 6.7823 (0.0830) z = 0.8741 (0.0098) Angle to previous plane (with approximate esd) = 86.04 ( 0.19 ) * 0.0000 (0.0000) O5A * 0.0000 (0.0000) O5B * 0.0000 (0.0000) C5 Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 3 24 GRID -1.190 -2 -2 1.190 2 2 R1 = 0.1330 for 2218 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.28 at 0.6502 0.5171 0.1217 [ 1.32 A from H4B ] Deepest hole -0.32 at 0.4975 0.4239 0.2530 [ 1.16 A from H22A ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2123 / 15186 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6502 0.5171 0.1217 1.00000 0.05 0.28 1.32 H4B 2.16 H3A 2.27 C4 2.40 H21A Q2 1 0.2883 -0.3654 0.4149 1.00000 0.05 0.27 1.29 H24C 1.50 H3B 1.75 O5B 1.82 H2B Q3 1 0.2701 0.8911 0.0368 1.00000 0.05 0.26 1.54 O1B 1.57 H3B 2.04 H2A 2.12 H24C Q4 1 0.5022 -0.4536 0.1543 1.00000 0.05 0.23 1.38 H22A 1.91 H2A 1.93 H4B 2.37 C22 Q5 1 0.0244 0.4198 -0.0065 1.00000 0.05 0.22 1.59 C1 1.65 O1A 1.79 C1 1.90 O1B Q6 1 0.4800 -0.2124 0.4305 1.00000 0.05 0.22 1.47 H24A 1.52 O1B 1.81 C1 1.86 H2B Q7 1 0.6198 0.3925 0.2126 1.00000 0.05 0.22 1.75 O5A 1.77 H22A 1.97 H21A 2.17 C5 Q8 1 0.7114 -0.0356 0.3822 1.00000 0.05 0.21 1.38 H21B 1.40 O1A 1.94 N21 1.96 H4B Q9 1 0.4808 0.3669 -0.0135 1.00000 0.05 0.21 0.96 H3A 1.54 C3 1.91 H2A 1.92 H4B Q10 1 0.5788 -0.1354 0.1456 1.00000 0.05 0.21 1.77 C5 1.77 O5A 2.19 H4A 2.30 H21C Shortest distances between peaks (including symmetry equivalents) 5 5 1.11 1 8 1.26 1 4 1.55 4 7 1.62 5 6 1.65 9 9 1.70 2 6 1.87 2 3 1.87 1 7 1.95 4 10 2.06 5 6 2.13 1 9 2.23 1 10 2.27 7 8 2.59 6 8 2.61 2 5 2.72 4 9 2.76 4 8 2.76 3 9 2.78 1 9 2.81 9 10 2.82 8 9 2.89 3 10 2.99 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.80: 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 0.41: Structure factors and derivatives 0.20: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0073p21n finished at 13:14:29 Total CPU time: 1.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++