+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0027p-1 started at 14:13:38 on 21-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0027p-1 in P-1 CELL 0.71073 7.5275 9.4025 9.9908 64.266 68.172 74.175 ZERR 2.00 0.0003 0.0004 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H N O UNIT 18 28 4 12 V = 586.06 F(000) = 260.0 Mu = 0.12 mm-1 Cell Wt = 492.44 Rho = 1.395 MERG 2 OMIT -3.00 55.00 OMIT 3 1 0 OMIT -3 2 0 OMIT -3 3 0 OMIT 3 2 0 OMIT 3 6 2 SHEL 7 0.77 HTAB O2 O1A EQIV_$1 -x+1, -y, -z+1 HTAB O2 O2_$1 EQIV_$2 x+1, y, z HTAB O4A O1A_$2 EQIV_$3 -x+1, -y-1, -z+1 HTAB N23 O4B_$3 HTAB N23 O3_$3 EQIV_$4 -x+1, -y, -z HTAB O3 O1B_$4 FMAP 2 PLAN 10 SIZE 0.05 0.07 0.08 ACTA BOND $H WGHT 0.11670 1.98780 L.S. 4 TEMP -153.00 FVAR 1.20941 MOLE 1 C1 1 0.394176 0.179999 0.111698 11.00000 0.02320 0.01463 = 0.02331 -0.00535 -0.00995 -0.00201 C2 1 0.562666 0.168701 0.168525 11.00000 0.01959 0.01819 = 0.02457 -0.00829 -0.00928 -0.00368 AFIX 13 H2 2 0.618214 0.271544 0.108496 11.00000 -1.20000 AFIX 0 C3 1 0.718041 0.035958 0.132959 11.00000 0.01943 0.02137 = 0.02310 -0.00964 -0.00595 -0.00249 AFIX 13 H3 2 0.763689 0.061677 0.018346 11.00000 -1.20000 AFIX 0 C4 1 0.886557 0.021921 0.188268 11.00000 0.01965 0.01917 = 0.02520 -0.01051 -0.00430 0.00081 O1A 4 0.235032 0.148233 0.212939 11.00000 0.01797 0.02731 = 0.03194 -0.00823 -0.00835 -0.00364 O1B 4 0.429361 0.218346 -0.031263 11.00000 0.02804 0.03211 = 0.02330 -0.00778 -0.00890 -0.00794 O2 4 0.505224 0.142082 0.328167 11.00000 0.02387 0.03472 = 0.02528 -0.01630 -0.00682 -0.00240 AFIX 147 H2OA 2 0.399715 0.104758 0.372151 10.50000 -1.50000 H2OB 2 0.482102 0.067757 0.418910 10.50000 -1.50000 AFIX 0 O3 4 0.642568 -0.109599 0.209403 11.00000 0.02628 0.01749 = 0.02927 -0.00680 -0.01063 -0.00456 AFIX 147 H3O 2 0.629051 -0.136291 0.144031 11.00000 -1.50000 AFIX 0 O4A 4 0.965945 0.153357 0.119835 11.00000 0.02243 0.02383 = 0.03050 -0.00363 -0.01167 -0.00720 AFIX 147 H4 2 1.060160 0.139880 0.151830 11.00000 -1.50000 AFIX 0 O4B 4 0.940753 -0.098846 0.284675 11.00000 0.03243 0.02262 = 0.04507 -0.00232 -0.02333 -0.00520 MOLE 2 C22 1 0.165754 -0.493741 0.624819 11.00000 0.02946 0.02121 = 0.02497 -0.00246 -0.00543 -0.00361 C24 1 0.297591 -0.545423 0.410625 11.00000 0.03638 0.02899 = 0.03366 -0.01501 -0.00712 0.00316 AFIX 43 H24 2 0.343802 -0.601806 0.342467 11.00000 -1.20000 AFIX 0 C25 1 0.304291 -0.389987 0.370662 11.00000 0.02726 0.03149 = 0.02622 -0.00940 -0.00560 -0.00462 AFIX 43 H25 2 0.356686 -0.316117 0.269531 11.00000 -1.20000 AFIX 0 C26 1 0.198558 -0.204825 0.517434 11.00000 0.04053 0.02593 = 0.03004 -0.00861 -0.01379 -0.00733 AFIX 137 H26A 2 0.065193 -0.178463 0.575263 11.00000 -1.50000 H26B 2 0.229657 -0.122306 0.412957 11.00000 -1.50000 H26C 2 0.286532 -0.210587 0.571900 11.00000 -1.50000 AFIX 0 C27 1 0.077664 -0.513248 0.789000 11.00000 0.04697 0.02985 = 0.02501 -0.00173 -0.00803 -0.00317 AFIX 137 H27A 2 0.030293 -0.616975 0.848614 11.00000 -1.50000 H27B 2 -0.030338 -0.428342 0.798019 11.00000 -1.50000 H27C 2 0.174301 -0.507434 0.829839 11.00000 -1.50000 AFIX 0 N21 3 0.219955 -0.359200 0.505727 11.00000 0.02480 0.02138 = 0.02238 -0.00485 -0.00624 -0.00415 N23 3 0.211853 -0.607037 0.567644 11.00000 0.03522 0.02108 = 0.03720 -0.00536 -0.00786 -0.00103 AFIX 43 H23 2 0.190546 -0.706685 0.622359 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0027p-1 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - O2 C3 C1 C3 - O3 C4 C2 C4 - O4B O4A C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C22 - N23 N21 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, -y, -z+1 $2 x+1, y, z $3 -x+1, -y-1, -z+1 $4 -x+1, -y, -z 13651 Reflections read, of which 43 rejected -9 =< h =< 9, -12 =< k =< 12, -12 =< l =< 12, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 2677 Unique reflections, of which 0 suppressed R(int) = 0.0660 R(sigma) = 0.0548 Friedel opposites merged Maximum memory for data reduction = 1935 / 26739 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 = 2373 / 198531 wR2 = 0.2858 before cycle 1 for 2677 data and 159 / 159 parameters GooF = S = 1.146; Restrained GooF = 1.146 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1167 * P )^2 + 1.99 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.20942 0.00719 0.001 OSF Mean shift/esd = 0.001 Maximum = -0.003 for U23 O4A Max. shift = 0.000 A for H2OB Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2373 / 198531 wR2 = 0.2858 before cycle 2 for 2677 data and 159 / 159 parameters GooF = S = 1.146; Restrained GooF = 1.146 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1167 * P )^2 + 1.99 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.20942 0.00719 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U23 O4A Max. shift = 0.000 A for H3O Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2373 / 198531 wR2 = 0.2858 before cycle 3 for 2677 data and 159 / 159 parameters GooF = S = 1.146; Restrained GooF = 1.146 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1167 * P )^2 + 1.99 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.20942 0.00719 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z N21 Max. shift = 0.000 A for H3O Max. dU = 0.000 for C22 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2373 / 198531 wR2 = 0.2858 before cycle 4 for 2677 data and 159 / 159 parameters GooF = S = 1.146; Restrained GooF = 1.146 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1167 * P )^2 + 1.99 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.20941 0.00719 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H3O Max. dU = 0.000 for C22 Largest correlation matrix elements -0.529 U23 O2 / U22 O2 -0.514 U13 O4B / U33 O4B Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.6182 0.2715 0.1085 13 1.000 0.000 C2 O2 C3 C1 H3 0.7637 0.0617 0.0183 13 1.000 0.000 C3 O3 C4 C2 H2OA 0.3997 0.1048 0.3722 147 0.840 0.000 O2 C2 H2OA H3O 0.6291 -0.1363 0.1440 147 0.840 0.000 O3 C3 H3O H4 1.0602 0.1399 0.1518 147 0.840 0.000 O4A C4 H4 H24 0.3438 -0.6018 0.3425 43 0.950 0.000 C24 C25 N23 H25 0.3567 -0.3161 0.2695 43 0.950 0.000 C25 C24 N21 H26A 0.0652 -0.1785 0.5753 137 0.980 0.000 C26 N21 H26A H26B 0.2297 -0.1223 0.4130 137 0.980 0.000 C26 N21 H26A H26C 0.2865 -0.2106 0.5719 137 0.980 0.000 C26 N21 H26A H27A 0.0303 -0.6170 0.8486 137 0.980 0.000 C27 C22 H27A H27B -0.0303 -0.4283 0.7980 137 0.980 0.000 C27 C22 H27A H27C 0.1743 -0.5074 0.8298 137 0.980 0.000 C27 C22 H27A H23 0.1905 -0.7067 0.6224 43 0.880 0.000 N23 C22 C24 06skc0027p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.39418 0.18000 0.11170 1.00000 0.02320 0.01463 0.02331 -0.00535 -0.00995 -0.00201 0.02016 0.00526 0.00059 0.00045 0.00046 0.00000 0.00199 0.00177 0.00201 0.00149 0.00162 0.00146 0.00083 C2 0.56267 0.16870 0.16852 1.00000 0.01959 0.01820 0.02457 -0.00829 -0.00928 -0.00368 0.01952 0.00503 0.00057 0.00046 0.00047 0.00000 0.00191 0.00182 0.00199 0.00154 0.00158 0.00147 0.00083 H2 0.61821 0.27154 0.10850 1.00000 0.02343 0.00000 0.00000 C3 0.71804 0.03596 0.13296 1.00000 0.01943 0.02137 0.02310 -0.00964 -0.00595 -0.00249 0.02092 0.00528 0.00057 0.00047 0.00048 0.00000 0.00193 0.00194 0.00197 0.00159 0.00157 0.00153 0.00085 H3 0.76369 0.06168 0.01835 1.00000 0.02511 0.00000 0.00000 C4 0.88656 0.02192 0.18827 1.00000 0.01965 0.01917 0.02520 -0.01051 -0.00430 0.00081 0.02195 0.00555 0.00059 0.00047 0.00048 0.00000 0.00192 0.00194 0.00206 0.00164 0.00160 0.00152 0.00086 O1A 0.23503 0.14823 0.21294 1.00000 0.01797 0.02731 0.03194 -0.00823 -0.00835 -0.00364 0.02633 0.00402 0.00041 0.00036 0.00035 0.00000 0.00144 0.00156 0.00167 0.00128 0.00125 0.00118 0.00071 O1B 0.42936 0.21835 -0.03126 1.00000 0.02804 0.03211 0.02330 -0.00778 -0.00890 -0.00794 0.02746 0.00399 0.00045 0.00037 0.00034 0.00000 0.00161 0.00168 0.00154 0.00128 0.00125 0.00130 0.00073 O2 0.50522 0.14208 0.32817 1.00000 0.02387 0.03472 0.02528 -0.01630 -0.00682 -0.00240 0.02648 0.00390 0.00044 0.00038 0.00035 0.00000 0.00156 0.00173 0.00156 0.00134 0.00126 0.00126 0.00071 H2OA 0.39971 0.10477 0.37215 0.50000 0.03972 0.00000 0.00000 H2OB 0.48209 0.06776 0.41891 0.50000 0.03972 0.00000 0.00000 O3 0.64257 -0.10960 0.20940 1.00000 0.02628 0.01749 0.02927 -0.00680 -0.01063 -0.00456 0.02392 0.00386 0.00043 0.00033 0.00035 0.00000 0.00154 0.00139 0.00156 0.00118 0.00127 0.00115 0.00068 H3O 0.62906 -0.13629 0.14403 1.00000 0.03588 0.00000 0.00000 O4A 0.96595 0.15336 0.11983 1.00000 0.02243 0.02383 0.03050 -0.00363 -0.01167 -0.00720 0.02588 0.00400 0.00043 0.00035 0.00036 0.00000 0.00150 0.00152 0.00162 0.00123 0.00125 0.00118 0.00071 H4 1.06016 0.13988 0.15183 1.00000 0.03883 0.00000 0.00000 O4B 0.94075 -0.09885 0.28468 1.00000 0.03243 0.02262 0.04507 -0.00232 -0.02333 -0.00520 0.03316 0.00426 0.00048 0.00036 0.00040 0.00000 0.00175 0.00157 0.00199 0.00141 0.00154 0.00131 0.00081 C22 0.16575 -0.49374 0.62482 1.00000 0.02945 0.02121 0.02497 -0.00246 -0.00543 -0.00361 0.02826 0.00642 0.00066 0.00051 0.00052 0.00000 0.00230 0.00204 0.00216 0.00167 0.00178 0.00170 0.00098 C24 0.29759 -0.54542 0.41062 1.00000 0.03638 0.02899 0.03366 -0.01501 -0.00712 0.00316 0.03439 0.00697 0.00073 0.00057 0.00058 0.00000 0.00259 0.00238 0.00249 0.00197 0.00205 0.00194 0.00110 H24 0.34380 -0.60181 0.34247 1.00000 0.04127 0.00000 0.00000 C25 0.30429 -0.38999 0.37066 1.00000 0.02726 0.03149 0.02622 -0.00940 -0.00559 -0.00462 0.02937 0.00625 0.00066 0.00055 0.00053 0.00000 0.00224 0.00233 0.00219 0.00183 0.00179 0.00182 0.00098 H25 0.35669 -0.31612 0.26953 1.00000 0.03525 0.00000 0.00000 C26 0.19856 -0.20482 0.51743 1.00000 0.04053 0.02593 0.03004 -0.00861 -0.01379 -0.00733 0.03112 0.00607 0.00074 0.00053 0.00055 0.00000 0.00265 0.00226 0.00235 0.00186 0.00202 0.00194 0.00103 H26A 0.06519 -0.17846 0.57526 1.00000 0.04669 0.00000 0.00000 H26B 0.22965 -0.12231 0.41296 1.00000 0.04669 0.00000 0.00000 H26C 0.28653 -0.21059 0.57190 1.00000 0.04669 0.00000 0.00000 C27 0.07766 -0.51325 0.78900 1.00000 0.04697 0.02985 0.02501 -0.00173 -0.00803 -0.00317 0.03835 0.00755 0.00081 0.00059 0.00054 0.00000 0.00301 0.00244 0.00233 0.00191 0.00212 0.00214 0.00119 H27A 0.03029 -0.61697 0.84861 1.00000 0.05752 0.00000 0.00000 H27B -0.03034 -0.42834 0.79802 1.00000 0.05752 0.00000 0.00000 H27C 0.17430 -0.50744 0.82984 1.00000 0.05752 0.00000 0.00000 N21 0.21995 -0.35920 0.50573 1.00000 0.02480 0.02138 0.02238 -0.00485 -0.00624 -0.00415 0.02406 0.00484 0.00052 0.00041 0.00040 0.00000 0.00180 0.00173 0.00176 0.00139 0.00144 0.00137 0.00079 N23 0.21185 -0.60704 0.56764 1.00000 0.03522 0.02108 0.03720 -0.00536 -0.00786 -0.00103 0.03469 0.00587 0.00060 0.00046 0.00048 0.00000 0.00221 0.00186 0.00221 0.00162 0.00176 0.00159 0.00096 H23 0.19055 -0.70668 0.62236 1.00000 0.04163 0.00000 0.00000 Final Structure Factor Calculation for 06skc0027p-1 in P-1 Total number of l.s. parameters = 159 Maximum vector length = 511 Memory required = 2214 / 22995 wR2 = 0.2858 before cycle 5 for 2677 data and 0 / 159 parameters GooF = S = 1.146; Restrained GooF = 1.146 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1167 * P )^2 + 1.99 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0963 for 1921 Fo > 4sig(Fo) and 0.1240 for all 2677 data wR2 = 0.2858, GooF = S = 1.146, Restrained GooF = 1.146 for all data Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0261 0.0197 0.0146 C1 0.0254 0.0194 0.0138 C2 0.0236 0.0198 0.0194 C3 0.0276 0.0232 0.0150 C4 0.0354 0.0267 0.0169 O1A 0.0354 0.0251 0.0218 O1B 0.0357 0.0240 0.0197 O2 0.0315 0.0238 0.0165 O3 0.0386 0.0221 0.0170 O4A 0.0567 0.0230 0.0198 O4B 0.0384 0.0281 0.0183 C22 0.0461 0.0345 0.0226 C24 0.0335 0.0297 0.0249 C25 0.0415 0.0275 0.0244 C26 0.0554 0.0388 0.0208 C27 0.0279 0.0250 0.0193 N21 0.0496 0.0340 0.0205 N23 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.021 0.034 0.046 0.061 0.079 0.101 0.134 0.198 1.000 Number in group 277. 259. 279. 264. 263. 268. 268. 270. 261. 268. GooF 1.501 1.199 1.059 1.225 1.216 0.934 0.956 1.023 0.971 1.240 K 32.449 2.766 1.305 1.255 1.165 1.023 1.022 1.028 1.013 1.020 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 281. 260. 269. 268. 260. 267. 269. 267. 266. 270. GooF 0.904 0.781 0.839 0.786 1.025 1.062 1.459 1.369 1.395 1.497 K 1.049 1.068 1.060 1.040 1.046 1.050 1.071 1.035 1.034 1.021 R1 0.271 0.194 0.191 0.158 0.137 0.100 0.116 0.093 0.084 0.090 Recommended weighting scheme: WGHT 0.1167 1.9879 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) -3 4 1 140.00 0.20 6.88 0.006 1.46 -3 -1 4 159.00 18.86 6.85 0.058 1.33 -3 6 1 100.59 3.45 6.56 0.025 1.15 -3 1 7 64.76 0.05 6.44 0.003 0.99 -3 0 3 232.55 64.61 6.39 0.108 1.59 3 5 9 106.97 1.18 6.36 0.015 1.09 3 4 10 119.10 6.53 6.10 0.034 1.00 -3 6 3 85.89 11.32 5.99 0.045 1.11 3 2 2 1730.48 743.24 5.97 0.366 2.42 3 -4 3 121.07 0.03 5.72 0.002 1.26 -3 3 5 125.13 25.92 5.64 0.068 1.21 3 7 7 77.94 7.19 5.64 0.036 1.16 3 9 1 73.41 1.99 5.57 0.019 0.95 -3 4 4 48.96 0.07 5.57 0.004 1.25 3 0 2 82.90 8.52 5.54 0.039 2.34 -3 1 1 78.51 15.16 5.39 0.052 2.01 -3 6 0 58.80 0.09 4.95 0.004 1.13 6 3 4 65.29 1.39 4.94 0.016 1.24 3 3 1 455.38 204.80 4.80 0.192 2.10 6 -2 3 54.99 0.45 4.75 0.009 1.07 -3 1 3 90.54 25.95 4.69 0.068 1.59 6 -2 1 44.60 1.97 4.41 0.019 1.09 6 3 3 72.00 10.69 4.38 0.044 1.24 3 0 5 58.20 13.64 4.31 0.050 1.63 3 5 2 883.72 458.04 4.22 0.288 1.65 3 -1 6 123.08 37.50 4.21 0.082 1.31 3 10 3 73.92 16.41 4.11 0.054 0.92 9 0 5 80.45 11.98 4.07 0.047 0.79 3 5 0 478.06 255.88 4.07 0.215 1.45 3 8 2 99.55 34.96 3.95 0.079 1.11 3 2 5 219.36 106.26 3.91 0.139 1.81 3 0 0 403.03 0.02 3.77 0.002 2.31 3 -1 5 96.33 38.20 3.77 0.083 1.48 -3 -7 1 21.08 0.02 3.73 0.002 1.05 3 -3 2 782.78 445.86 3.71 0.284 1.55 3 7 6 25.88 3.56 3.70 0.025 1.23 3 1 9 20.46 0.15 3.63 0.005 1.04 3 2 4 155.41 75.92 3.59 0.117 2.07 3 4 7 12.85 0.01 3.53 0.001 1.38 3 8 1 157.10 71.05 3.42 0.113 1.06 -3 -4 3 18.12 1.60 3.40 0.017 1.20 -3 -3 5 166.15 85.14 3.36 0.124 1.05 -6 1 0 42.58 0.38 3.33 0.008 1.12 3 -1 7 20.42 0.42 3.31 0.009 1.16 6 9 11 43.48 5.73 3.29 0.032 0.79 3 3 0 14.96 0.89 3.26 0.013 1.91 3 8 5 30.97 5.65 3.24 0.032 1.14 -3 3 3 18.81 2.83 3.18 0.023 1.45 -3 -8 1 19.44 0.49 3.15 0.009 0.95 -3 0 5 17.91 2.46 3.14 0.021 1.22 Bond lengths and angles C1 - Distance Angles O1B 1.2505 (0.0050) O1A 1.2566 (0.0051) 126.27 (0.38) C2 1.5336 (0.0055) 116.62 (0.36) 117.11 (0.35) C1 - O1B O1A C2 - Distance Angles O2 1.4117 (0.0049) C3 1.5271 (0.0055) 110.86 (0.32) C1 1.5336 (0.0055) 112.69 (0.33) 108.34 (0.32) H2 1.0000 108.28 108.28 108.28 C2 - O2 C3 C1 C3 - Distance Angles O3 1.4046 (0.0048) C4 1.5161 (0.0058) 109.18 (0.32) C2 1.5271 (0.0055) 110.00 (0.32) 109.47 (0.32) H3 1.0000 109.39 109.39 109.39 C3 - O3 C4 C2 C4 - Distance Angles O4B 1.2138 (0.0051) O4A 1.3104 (0.0049) 124.52 (0.40) C3 1.5161 (0.0058) 123.01 (0.38) 112.47 (0.34) C4 - O4B O4A O1A - Distance Angles C1 1.2566 (0.0051) O1A - O1B - Distance Angles C1 1.2505 (0.0050) O1B - O2 - Distance Angles C2 1.4117 (0.0049) H2OA 0.8400 109.47 H2OB 0.8599 142.18 58.05 O2 - C2 H2OA O3 - Distance Angles C3 1.4046 (0.0048) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.3104 (0.0049) H4 0.8400 109.47 O4A - C4 O4B - Distance Angles C4 1.2138 (0.0051) O4B - C22 - Distance Angles N23 1.3270 (0.0062) N21 1.3401 (0.0055) 107.30 (0.39) C27 1.4697 (0.0063) 126.39 (0.41) 126.28 (0.42) C22 - N23 N21 C24 - Distance Angles C25 1.3477 (0.0067) N23 1.3693 (0.0063) 107.33 (0.42) H24 0.9500 126.34 126.34 C24 - C25 N23 C25 - Distance Angles C24 1.3477 (0.0067) N21 1.3819 (0.0058) 106.50 (0.40) H25 0.9500 126.75 126.75 C25 - C24 N21 C26 - Distance Angles N21 1.4671 (0.0056) 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 1.4697 (0.0063) 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 1.3401 (0.0055) C25 1.3819 (0.0058) 109.17 (0.38) C26 1.4671 (0.0056) 125.46 (0.38) 125.35 (0.37) N21 - C22 C25 N23 - Distance Angles C22 1.3270 (0.0062) C24 1.3693 (0.0063) 109.71 (0.39) H23 0.8800 125.15 125.15 N23 - C22 C24 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.20 2.662(4) 114.2 O2-H2OA...O1A 0.86 2.46 3.299(6) 166.5 O2-H2OB...O2_$1 0.84 1.68 2.506(4) 169.4 O4A-H4...O1A_$2 0.88 2.00 2.841(5) 158.9 N23-H23...O4B_$3 0.88 2.29 2.886(5) 124.8 N23-H23...O3_$3 0.84 1.83 2.666(4) 169.8 O3-H3O...O1B_$4 FMAP and GRID set by program FMAP 2 1 23 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.1238 for 2677 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.81 at 0.1156 0.8344 0.7950 [ 0.88 A from O4A ] Deepest hole -0.40 at 0.1356 0.5694 0.7296 [ 0.86 A from C27 ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 2267 / 18873 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8844 0.1656 0.2050 1.00000 0.05 0.81 0.88 O4A 1.23 H4 1.43 C4 2.23 O4B Q2 1 0.3121 -0.1045 0.2476 1.00000 0.05 0.64 1.48 H26B 1.85 H25 2.19 O1A 2.21 H3O Q3 1 0.6412 0.1356 0.1314 1.00000 0.05 0.60 0.65 C2 0.95 C3 1.17 H2 1.47 H3 Q4 1 0.7150 0.1576 0.1160 1.00000 0.05 0.59 1.07 C2 1.08 C3 1.11 H2 1.49 H3 Q5 1 0.3845 -0.4585 0.5981 1.00000 0.05 0.56 1.65 N21 1.67 C22 2.17 H26C 2.20 H27C Q6 1 0.7483 0.2209 -0.0397 1.00000 0.05 0.54 1.34 H3 1.63 H2 1.84 C3 1.96 C2 Q7 1 0.2761 0.1667 0.1212 1.00000 0.05 0.54 0.80 O1A 0.90 C1 1.50 O1B 1.61 H4 Q8 1 0.1447 -0.1401 0.6783 1.00000 0.05 0.51 1.45 H26C 1.56 H26A 1.82 H4 1.83 C26 Q9 1 -0.0106 -0.4681 0.5903 1.00000 0.05 0.51 1.43 C22 1.83 N23 1.98 N21 2.13 C24 Q10 1 0.2006 0.1493 0.3441 1.00000 0.05 0.50 1.24 O1A 1.54 H2OA 1.85 H26A 2.17 C1 Shortest distances between peaks (including symmetry equivalents) 3 4 0.59 1 8 1.03 4 6 1.35 3 6 1.53 1 4 1.84 7 10 2.03 9 9 2.08 2 7 2.29 1 3 2.33 5 5 2.35 4 8 2.57 8 10 2.72 3 7 2.72 1 7 2.75 2 10 2.76 1 6 2.79 3 8 2.93 2 6 2.94 Time profile in seconds ----------------------- 0.09: 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. 0.63: 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 0.33: Structure factors and derivatives 0.52: 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 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0027p-1 finished at 14:13:39 Total CPU time: 1.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++