+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04skc0013p21c started at 11:02:08 on 13-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04skc0013p21c in P2(1)/c CELL 0.71073 8.1431 9.4941 14.3618 90.000 94.415 90.000 ZERR 4.00 0.0013 0.0019 0.0031 0.000 0.015 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 32 68 4 24 V = 1107.04 F(000) = 480.0 Mu = 0.11 mm-1 Cell Wt = 892.90 Rho = 1.339 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB O3 O4B HTAB N23 O2 EQIV_$1 x, -y+1/2, z-1/2 HTAB O1B O4B_$1 EQIV_$2 -x+1, -y, -z HTAB O2 O1A_$2 EQIV_$3 -x+2, y-1/2, -z+1/2 HTAB N23 O4A_$3 FMAP 2 PLAN 10 SIZE 0.03 0.08 0.14 ACTA BOND $H WGHT 0.03420 0.60960 L.S. 4 TEMP -153.00 FVAR 0.87472 MOLE 1 C1 1 0.743545 0.074919 -0.086347 11.00000 0.02034 0.01823 = 0.01743 0.00120 0.00066 0.00200 C2 1 0.791300 0.098364 0.016916 11.00000 0.01850 0.02199 = 0.01456 0.00174 0.00188 0.00015 AFIX 13 H2 2 0.909456 0.070563 0.029063 11.00000 -1.20000 AFIX 0 C3 1 0.777713 0.254015 0.041089 11.00000 0.01826 0.02173 = 0.01474 0.00092 0.00081 0.00062 AFIX 13 H3 2 0.846874 0.309397 -0.000380 11.00000 -1.20000 AFIX 0 C4 1 0.842746 0.277924 0.142579 11.00000 0.01968 0.02089 = 0.01638 -0.00084 0.00104 -0.00204 O1A 4 0.622736 0.008616 -0.115264 11.00000 0.02438 0.02936 = 0.02054 -0.00034 -0.00212 -0.00669 O1B 4 0.847232 0.136645 -0.138406 11.00000 0.02708 0.03269 = 0.01340 0.00082 0.00100 -0.00789 AFIX 147 H1 2 0.808494 0.136321 -0.194330 11.00000 -1.50000 AFIX 0 O2 4 0.698362 0.014274 0.074074 11.00000 0.02398 0.02308 = 0.01927 0.00607 0.00276 0.00036 AFIX 147 H2O 2 0.599096 0.039010 0.067629 11.00000 -1.50000 AFIX 0 O3 4 0.611797 0.298185 0.024865 11.00000 0.02123 0.02893 = 0.01958 -0.00211 -0.00171 0.00694 AFIX 147 H3O 2 0.577650 0.328014 0.074944 11.00000 -1.50000 AFIX 0 O4A 4 0.983192 0.234464 0.166913 11.00000 0.01987 0.04619 = 0.02442 -0.00891 -0.00500 0.00434 O4B 4 0.746205 0.342808 0.192397 11.00000 0.02849 0.03046 = 0.01504 -0.00241 0.00148 0.00577 MOLE 2 C21 1 0.797689 -0.347003 0.080817 11.00000 0.04303 0.02750 = 0.02672 -0.00407 0.00067 -0.00005 AFIX 137 H21A 2 0.908802 -0.371377 0.106903 11.00000 -1.50000 H21B 2 0.803533 -0.266194 0.038745 11.00000 -1.50000 H21C 2 0.749366 -0.427612 0.045991 11.00000 -1.50000 AFIX 0 C22 1 0.691986 -0.309774 0.159071 11.00000 0.02660 0.02214 = 0.02535 -0.00010 -0.00223 -0.00344 AFIX 23 H22A 2 0.578889 -0.287652 0.132918 11.00000 -1.20000 H22B 2 0.685879 -0.391389 0.201569 11.00000 -1.20000 AFIX 0 C24 1 0.658664 -0.139689 0.288049 11.00000 0.02402 0.03018 = 0.02058 0.00292 0.00222 0.00429 AFIX 23 H24A 2 0.656692 -0.214504 0.335967 11.00000 -1.20000 H24B 2 0.544217 -0.123597 0.261779 11.00000 -1.20000 AFIX 0 C25 1 0.726249 -0.005996 0.332597 11.00000 0.04859 0.03175 = 0.02699 -0.00603 0.00475 0.00358 AFIX 137 H25A 2 0.839907 -0.021759 0.358034 11.00000 -1.50000 H25B 2 0.658642 0.021762 0.383114 11.00000 -1.50000 H25C 2 0.724167 0.068986 0.285625 11.00000 -1.50000 AFIX 0 N23 3 0.761628 -0.186209 0.212445 11.00000 0.01943 0.01972 = 0.01796 0.00235 -0.00150 -0.00076 AFIX 23 H23A 2 0.772521 -0.112489 0.171803 11.00000 -1.20000 H23B 2 0.865094 -0.208904 0.238345 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 04skc0013p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - O2 C1 C3 C3 - O3 C2 C4 C4 - O4A O4B C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C21 - C22 C22 - N23 C21 C24 - N23 C25 C25 - C24 N23 - C24 C22 Operators for generating equivalent atoms: $1 x, -y+1/2, z-1/2 $2 -x+1, -y, -z $3 -x+2, y-1/2, -z+1/2 14183 Reflections read, of which 555 rejected -10 =< h =< 10, -12 =< k =< 12, -18 =< l =< 18, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 2 9 7 24.42 6.31 2 57.15 1 Inconsistent equivalents 2539 Unique reflections, of which 0 suppressed R(int) = 0.0544 R(sigma) = 0.0448 Friedel opposites merged Maximum memory for data reduction = 1847 / 25300 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 = 2270 / 177390 wR2 = 0.1044 before cycle 1 for 2539 data and 141 / 141 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0342 * P )^2 + 0.61 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87455 0.00177 -0.096 OSF Mean shift/esd = 0.012 Maximum = -0.096 for OSF Max. shift = 0.000 A for H21B Max. dU = 0.000 for C25 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2270 / 177390 wR2 = 0.1043 before cycle 2 for 2539 data and 141 / 141 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0342 * P )^2 + 0.61 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87449 0.00177 -0.032 OSF Mean shift/esd = 0.005 Maximum = -0.032 for OSF Max. shift = 0.000 A for H2O Max. dU = 0.000 for C25 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2270 / 177390 wR2 = 0.1043 before cycle 3 for 2539 data and 141 / 141 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0342 * P )^2 + 0.61 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87449 0.00177 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for tors H2O Max. shift = 0.000 A for H2O Max. dU = 0.000 for C25 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2270 / 177390 wR2 = 0.1043 before cycle 4 for 2539 data and 141 / 141 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0342 * P )^2 + 0.61 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87449 0.00177 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H2O Max. shift = 0.000 A for H2O Max. dU = 0.000 for C21 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 0.9095 0.0706 0.0291 13 1.000 0.000 C2 O2 C1 C3 H3 0.8469 0.3094 -0.0004 13 1.000 0.000 C3 O3 C2 C4 H1 0.8085 0.1363 -0.1943 147 0.840 0.000 O1B C1 H1 H2O 0.5991 0.0390 0.0676 147 0.840 0.000 O2 C2 H2O H3O 0.5776 0.3280 0.0749 147 0.840 0.000 O3 C3 H3O H21A 0.9088 -0.3714 0.1069 137 0.980 0.000 C21 C22 H21A H21B 0.8035 -0.2662 0.0387 137 0.980 0.000 C21 C22 H21A H21C 0.7494 -0.4276 0.0460 137 0.980 0.000 C21 C22 H21A H22A 0.5789 -0.2877 0.1329 23 0.990 0.000 C22 N23 C21 H22B 0.6859 -0.3914 0.2016 23 0.990 0.000 C22 N23 C21 H24A 0.6567 -0.2145 0.3360 23 0.990 0.000 C24 N23 C25 H24B 0.5442 -0.1236 0.2618 23 0.990 0.000 C24 N23 C25 H25A 0.8399 -0.0218 0.3580 137 0.980 0.000 C25 C24 H25A H25B 0.6586 0.0218 0.3831 137 0.980 0.000 C25 C24 H25A H25C 0.7242 0.0690 0.2856 137 0.980 0.000 C25 C24 H25A H23A 0.8651 -0.2089 0.2383 23 0.920 0.000 N23 C24 C22 H23B 0.7725 -0.1125 0.1718 23 0.920 0.000 N23 C24 C22 04skc0013p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.74355 0.07492 -0.08635 1.00000 0.02033 0.01821 0.01739 0.00120 0.00066 0.00199 0.01868 0.00282 0.00019 0.00016 0.00011 0.00000 0.00077 0.00079 0.00084 0.00064 0.00063 0.00063 0.00034 C2 0.79130 0.09836 0.01692 1.00000 0.01848 0.02196 0.01453 0.00173 0.00186 0.00015 0.01829 0.00280 0.00019 0.00017 0.00011 0.00000 0.00075 0.00080 0.00080 0.00064 0.00061 0.00062 0.00034 H2 0.90946 0.07056 0.02907 1.00000 0.02195 0.00000 0.00000 C3 0.77771 0.25401 0.04109 1.00000 0.01824 0.02171 0.01471 0.00092 0.00080 0.00062 0.01825 0.00276 0.00018 0.00017 0.00011 0.00000 0.00075 0.00079 0.00080 0.00065 0.00061 0.00063 0.00034 H3 0.84687 0.30939 -0.00038 1.00000 0.02190 0.00000 0.00000 C4 0.84275 0.27793 0.14258 1.00000 0.01968 0.02088 0.01634 -0.00085 0.00103 -0.00204 0.01898 0.00279 0.00019 0.00017 0.00011 0.00000 0.00077 0.00081 0.00081 0.00065 0.00063 0.00062 0.00034 O1A 0.62273 0.00862 -0.11527 1.00000 0.02436 0.02936 0.02052 -0.00034 -0.00212 -0.00669 0.02494 0.00201 0.00014 0.00012 0.00008 0.00000 0.00061 0.00066 0.00062 0.00051 0.00049 0.00050 0.00029 O1B 0.84723 0.13664 -0.13841 1.00000 0.02707 0.03267 0.01339 0.00082 0.00100 -0.00788 0.02441 0.00199 0.00014 0.00013 0.00008 0.00000 0.00061 0.00067 0.00058 0.00051 0.00047 0.00050 0.00028 H1 0.80849 0.13634 -0.19433 1.00000 0.03661 0.00000 0.00000 O2 0.69836 0.01427 0.07407 1.00000 0.02396 0.02306 0.01924 0.00606 0.00276 0.00036 0.02203 0.00208 0.00014 0.00012 0.00008 0.00000 0.00059 0.00060 0.00060 0.00048 0.00049 0.00047 0.00027 H2O 0.59910 0.03903 0.06764 1.00000 0.03305 0.00000 0.00000 O3 0.61179 0.29819 0.02486 1.00000 0.02121 0.02891 0.01955 -0.00212 -0.00171 0.00694 0.02339 0.00204 0.00013 0.00013 0.00008 0.00000 0.00058 0.00064 0.00061 0.00050 0.00047 0.00047 0.00028 H3O 0.57764 0.32800 0.07495 1.00000 0.03509 0.00000 0.00000 O4A 0.98319 0.23446 0.16691 1.00000 0.01985 0.04618 0.02440 -0.00891 -0.00499 0.00434 0.03049 0.00213 0.00014 0.00014 0.00008 0.00000 0.00060 0.00079 0.00068 0.00059 0.00049 0.00054 0.00031 O4B 0.74620 0.34281 0.19240 1.00000 0.02846 0.03045 0.01501 -0.00241 0.00147 0.00577 0.02465 0.00206 0.00014 0.00012 0.00008 0.00000 0.00063 0.00065 0.00059 0.00050 0.00048 0.00051 0.00028 C21 0.79769 -0.34700 0.08081 1.00000 0.04301 0.02748 0.02668 -0.00407 0.00067 -0.00004 0.03250 0.00337 0.00024 0.00020 0.00013 0.00000 0.00108 0.00096 0.00101 0.00078 0.00083 0.00080 0.00044 H21A 0.90881 -0.37135 0.10690 1.00000 0.04874 0.00000 0.00000 H21B 0.80351 -0.26620 0.03874 1.00000 0.04874 0.00000 0.00000 H21C 0.74938 -0.42762 0.04600 1.00000 0.04874 0.00000 0.00000 C22 0.69198 -0.30977 0.15907 1.00000 0.02657 0.02213 0.02533 -0.00012 -0.00222 -0.00344 0.02489 0.00296 0.00021 0.00018 0.00012 0.00000 0.00085 0.00084 0.00094 0.00073 0.00071 0.00070 0.00038 H22A 0.57888 -0.28765 0.13292 1.00000 0.02987 0.00000 0.00000 H22B 0.68588 -0.39139 0.20157 1.00000 0.02987 0.00000 0.00000 C24 0.65866 -0.13969 0.28805 1.00000 0.02400 0.03016 0.02056 0.00292 0.00222 0.00427 0.02488 0.00309 0.00020 0.00018 0.00012 0.00000 0.00084 0.00093 0.00090 0.00074 0.00068 0.00070 0.00038 H24A 0.65669 -0.21451 0.33597 1.00000 0.02986 0.00000 0.00000 H24B 0.54421 -0.12360 0.26178 1.00000 0.02986 0.00000 0.00000 C25 0.72625 -0.00599 0.33260 1.00000 0.04857 0.03172 0.02695 -0.00603 0.00475 0.00357 0.03565 0.00352 0.00026 0.00020 0.00014 0.00000 0.00118 0.00103 0.00103 0.00082 0.00090 0.00088 0.00046 H25A 0.83991 -0.02176 0.35804 1.00000 0.05347 0.00000 0.00000 H25B 0.65864 0.02177 0.38311 1.00000 0.05347 0.00000 0.00000 H25C 0.72418 0.06898 0.28563 1.00000 0.05347 0.00000 0.00000 N23 0.76163 -0.18621 0.21244 1.00000 0.01941 0.01970 0.01795 0.00235 -0.00150 -0.00076 0.01917 0.00231 0.00016 0.00014 0.00009 0.00000 0.00065 0.00067 0.00070 0.00056 0.00053 0.00053 0.00030 H23A 0.86510 -0.20890 0.23834 1.00000 0.02301 0.00000 0.00000 H23B 0.77252 -0.11249 0.17180 1.00000 0.02301 0.00000 0.00000 Final Structure Factor Calculation for 04skc0013p21c in P2(1)/c Total number of l.s. parameters = 141 Maximum vector length = 511 Memory required = 2129 / 22995 wR2 = 0.1044 before cycle 5 for 2539 data and 0 / 141 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0342 * P )^2 + 0.61 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0458 for 1953 Fo > 4sig(Fo) and 0.0678 for all 2539 data wR2 = 0.1044, GooF = S = 1.043, Restrained GooF = 1.043 for all data Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.0215 0.0186 0.0159 C1 0.0224 0.0185 0.0140 C2 0.0219 0.0183 0.0146 C3 0.0224 0.0185 0.0161 C4 0.0345 0.0234 0.0170 O1A 0.0384 0.0215 0.0133 O1B 0.0276 0.0238 0.0147 O2 0.0341 0.0197 0.0163 O3 0.0511 0.0250 0.0154 O4A 0.0357 0.0238 0.0145 O4B 0.0435 0.0311 0.0230 C21 0.0314 0.0238 0.0195 C22 0.0329 0.0221 0.0197 C24 0.0493 0.0356 0.0221 C25 0.0233 0.0188 0.0154 N23 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.023 0.034 0.047 0.062 0.079 0.100 0.130 0.193 1.000 Number in group 254. 257. 260. 248. 267. 243. 257. 245. 254. 254. GooF 1.100 1.025 1.008 1.081 1.073 0.991 1.008 1.073 0.971 1.093 K 5.858 1.302 1.079 0.973 0.993 1.010 0.989 1.009 1.015 0.993 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.14 1.31 1.65 inf Number in group 264. 255. 247. 257. 250. 251. 253. 255. 252. 255. GooF 1.032 0.965 0.957 0.960 0.971 0.962 0.894 0.988 1.140 1.449 K 1.042 1.036 1.027 1.046 0.991 1.005 1.005 1.013 1.023 0.980 R1 0.169 0.173 0.130 0.112 0.083 0.061 0.040 0.037 0.036 0.031 Recommended weighting scheme: WGHT 0.0341 0.6058 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) 7 0 0 88.27 20.75 5.98 0.042 1.16 6 0 0 101.86 1.19 5.55 0.010 1.35 -3 6 6 37.52 6.36 5.24 0.023 1.21 1 1 2 1760.15 2112.53 4.26 0.419 4.54 0 1 4 73.67 46.79 3.97 0.062 3.35 -1 2 6 57.12 33.84 3.94 0.053 2.10 -8 4 11 2.00 27.64 3.79 0.048 0.79 0 9 3 9.37 0.29 3.52 0.005 1.03 1 1 1 144.03 108.70 3.50 0.095 5.55 -3 9 3 12.38 0.55 3.47 0.007 0.97 0 4 6 26.33 11.38 3.36 0.031 1.68 3 0 0 975.41 831.54 3.26 0.263 2.71 0 1 2 165.77 129.59 3.19 0.104 5.72 5 5 9 6.79 23.64 3.18 0.044 0.95 0 6 3 90.09 59.92 3.16 0.071 1.50 2 2 5 44.67 65.81 3.11 0.074 2.04 -1 2 3 -2.41 3.97 3.07 0.018 3.17 2 1 1 958.95 1102.68 3.06 0.303 3.55 4 5 12 49.32 9.75 3.06 0.028 0.88 -4 3 4 112.55 82.91 3.00 0.083 1.58 2 4 11 83.46 113.63 2.93 0.097 1.08 -2 5 6 64.86 42.75 2.93 0.060 1.42 1 2 1 2128.66 2405.03 2.93 0.447 3.90 6 1 0 202.24 161.33 2.91 0.116 1.34 1 1 3 941.90 1075.72 2.89 0.299 3.67 -4 10 6 -1.59 10.83 2.89 0.030 0.82 2 3 3 219.65 180.43 2.88 0.122 2.17 -1 0 2 3428.18 3892.07 2.86 0.568 5.59 -1 1 2 4561.53 5139.13 2.85 0.653 4.82 -4 1 14 100.15 132.41 2.85 0.105 0.94 -3 2 7 198.59 162.52 2.80 0.116 1.60 3 6 3 6.06 0.19 2.77 0.004 1.30 3 1 3 11.42 3.96 2.77 0.018 2.22 4 2 3 744.64 653.58 2.76 0.233 1.70 4 7 6 33.30 16.80 2.73 0.037 1.00 2 3 2 102.51 79.85 2.68 0.081 2.32 4 4 2 45.47 31.42 2.57 0.051 1.49 2 2 2 4.12 11.09 2.52 0.030 2.77 1 4 7 29.11 16.88 2.51 0.037 1.51 0 6 14 104.46 65.47 2.50 0.074 0.86 8 2 5 10.26 23.53 2.49 0.044 0.92 -1 4 4 85.17 65.79 2.49 0.074 1.94 0 2 16 230.74 176.54 2.49 0.121 0.88 -5 3 15 8.12 28.84 2.49 0.049 0.82 1 11 8 47.17 75.53 2.47 0.079 0.77 -1 2 14 12.88 2.80 2.46 0.015 1.00 -3 6 3 18.31 9.66 2.45 0.028 1.33 -3 0 6 483.48 416.46 2.45 0.186 1.86 0 4 3 435.72 379.03 2.45 0.177 2.13 0 2 1 4762.79 5264.50 2.44 0.661 4.51 Bond lengths and angles C1 - Distance Angles O1A 1.2139 (0.0019) O1B 1.3086 (0.0019) 125.33 (0.15) C2 1.5204 (0.0023) 123.32 (0.14) 111.34 (0.13) C1 - O1A O1B C2 - Distance Angles O2 1.4070 (0.0019) C1 1.5204 (0.0023) 112.17 (0.13) C3 1.5239 (0.0023) 111.45 (0.13) 110.27 (0.13) H2 1.0000 107.58 107.58 107.58 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4167 (0.0018) C2 1.5239 (0.0023) 109.55 (0.13) C4 1.5290 (0.0023) 111.64 (0.12) 109.58 (0.13) H3 1.0000 108.67 108.67 108.67 C3 - O3 C2 C4 C4 - Distance Angles O4A 1.2405 (0.0019) O4B 1.2633 (0.0019) 127.09 (0.15) C3 1.5290 (0.0023) 117.60 (0.14) 115.30 (0.14) C4 - O4A O4B O1A - Distance Angles C1 1.2139 (0.0019) O1A - O1B - Distance Angles C1 1.3086 (0.0019) H1 0.8400 109.47 O1B - C1 O2 - Distance Angles C2 1.4070 (0.0019) H2O 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4167 (0.0018) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.2405 (0.0019) O4A - O4B - Distance Angles C4 1.2633 (0.0019) O4B - C21 - Distance Angles C22 1.5093 (0.0025) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - C22 H21A H21B C22 - Distance Angles N23 1.4895 (0.0021) C21 1.5093 (0.0025) 110.57 (0.14) H22A 0.9900 109.54 109.54 H22B 0.9900 109.54 109.54 108.09 C22 - N23 C21 H22A C24 - Distance Angles N23 1.4891 (0.0021) C25 1.5064 (0.0025) 110.60 (0.14) H24A 0.9900 109.53 109.53 H24B 0.9900 109.53 109.53 108.09 C24 - N23 C25 H24A C25 - Distance Angles C24 1.5064 (0.0025) H25A 0.9800 109.47 H25B 0.9800 109.47 109.47 H25C 0.9800 109.47 109.47 109.47 C25 - C24 H25A H25B N23 - Distance Angles C24 1.4891 (0.0021) C22 1.4895 (0.0021) 113.29 (0.13) H23A 0.9200 108.92 108.92 H23B 0.9200 108.92 108.92 107.74 N23 - C24 C22 H23A Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.10 2.6002(17) 118.2 O3-H3O...O4B 0.92 1.91 2.7712(18) 154.8 N23-H23B...O2 0.84 1.68 2.5123(17) 171.8 O1B-H1...O4B_$1 0.84 2.03 2.7335(16) 140.7 O2-H2O...O1A_$2 0.92 1.85 2.7079(18) 155.0 N23-H23A...O4A_$3 FMAP and GRID set by program FMAP 2 2 14 GRID -2.273 -2 -2 2.273 2 2 R1 = 0.0678 for 2539 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.26 at 0.7823 0.1792 0.0224 [ 0.76 A from C3 ] Deepest hole -0.25 at 0.7708 0.1397 0.8125 [ 0.33 A from H1 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2270 / 17119 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7823 0.1792 0.0224 1.00000 0.05 0.26 0.76 C3 0.78 C2 1.39 H3 1.46 H2 Q2 1 0.7588 0.0808 -0.0337 1.00000 0.05 0.24 0.76 C1 0.77 C2 1.47 H2 1.69 O1A Q3 1 0.8094 0.2496 0.0903 1.00000 0.05 0.21 0.74 C3 0.82 C4 1.47 H3 1.73 O4A Q4 1 0.6968 -0.2015 -0.0429 1.00000 0.05 0.17 1.53 H21B 1.92 H24A 2.31 O1A 2.35 C21 Q5 1 0.6997 0.4535 0.1784 1.00000 0.05 0.17 1.13 O4B 1.52 H22B 2.09 H3O 2.12 C4 Q6 1 0.8443 -0.2642 0.0426 1.00000 0.05 0.17 0.33 H21B 1.05 C21 1.45 H21A 1.74 H21C Q7 1 0.9764 0.1563 0.2182 1.00000 0.05 0.17 1.05 O4A 1.87 C4 1.89 H23A 2.48 H25C Q8 1 0.8360 0.2287 -0.0991 1.00000 0.05 0.16 1.05 O1B 1.61 H3 1.63 H1 1.66 C1 Q9 1 0.7864 0.3778 0.2381 1.00000 0.05 0.16 0.78 O4B 0.98 H1 1.76 C4 1.81 O1B Q10 1 0.7339 -0.4500 0.2538 1.00000 0.05 0.16 0.99 H22B 1.92 C22 2.00 H1 2.16 O4B Shortest distances between peaks (including symmetry equivalents) 1 3 1.19 1 2 1.24 5 9 1.29 5 10 1.43 9 10 1.71 4 6 1.75 2 8 1.83 1 8 1.89 3 7 2.37 2 3 2.41 3 9 2.47 3 5 2.51 8 9 2.55 7 10 2.57 7 9 2.64 6 8 2.69 2 4 2.73 3 8 2.75 Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 0.64: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.42: Structure factors and derivatives 0.34: 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 0.02: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04skc0013p21c finished at 11:02:10 Total CPU time: 1.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++