+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04skc0002a started at 13:53:52 on 21-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04skc0002a in P-1 CELL 0.71073 7.5625 8.3396 9.1932 66.466 71.905 73.034 ZERR 2.00 0.0018 0.0028 0.0058 0.031 0.024 0.020 LATT 1 SFAC C H N O UNIT 16 24 4 12 V = 495.83 F(000) = 244.0 Mu = 0.13 mm-1 Cell Wt = 464.39 Rho = 1.555 MERG 2 OMIT -3.00 55.00 OMIT -1 -1 7 EXTI 0.02200 HTAB O3 O4A EQIV $1 -x, -y+1, -z+2 HTAB O2 O4B_$1 EQIV $2 -x, -y+2, -z+1 HTAB O3 O4A_$2 EQIV $3 x+1, y, z HTAB O1A O4B_$3 HTAB O1A O4A_$3 EQIV $4 -x+1, -y+2, -z+2 HTAB N21 O1B_$4 EQIV $5 -x+1, -y+2, -z+1 HTAB N23 O2_$5 HTAB N23 O1A_$5 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.02 0.08 0.15 ACTA BOND $H WGHT 0.04000 0.34790 L.S. 4 TEMP -153.00 FVAR 1.15121 MOLE 1 C1 1 0.307654 0.728312 0.935275 11.00000 0.01687 0.01637 = 0.01377 0.00090 -0.00485 -0.00533 C2 1 0.135083 0.684114 0.918686 11.00000 0.01458 0.02142 = 0.01701 -0.00754 -0.00299 -0.00733 AFIX 13 H2 2 0.061505 0.624920 1.029692 11.00000 -1.20000 AFIX 0 C3 1 0.010301 0.857661 0.835433 11.00000 0.01255 0.01832 = 0.01727 -0.00436 -0.00246 -0.00602 AFIX 13 H3 2 -0.047889 0.925236 0.912932 11.00000 -1.20000 AFIX 0 C4 1 -0.149365 0.819824 0.792212 11.00000 0.01316 0.01656 = 0.02177 -0.00514 -0.00596 -0.00037 O1A 4 0.468195 0.675300 0.849424 11.00000 0.01078 0.02959 = 0.02178 -0.01033 -0.00443 -0.00591 AFIX 147 H1 2 0.556127 0.695786 0.873200 11.00000 -1.50000 AFIX 0 O1B 4 0.284361 0.810412 1.027344 11.00000 0.01833 0.02806 = 0.02012 -0.01038 -0.00587 -0.00466 O2 4 0.184360 0.569534 0.825619 11.00000 0.01705 0.01677 = 0.01965 -0.00473 -0.00625 -0.00296 AFIX 147 H2O 2 0.224244 0.464909 0.882469 11.00000 -1.50000 AFIX 0 O3 4 0.124538 0.962136 0.696287 11.00000 0.01790 0.02593 = 0.01817 -0.00063 -0.00654 -0.01011 AFIX 147 H3O 2 0.087542 0.979810 0.612968 11.00000 -1.50000 AFIX 0 O4A 4 -0.158543 0.872864 0.648938 11.00000 0.01989 0.02958 = 0.01712 -0.00358 -0.00773 -0.00707 O4B 4 -0.266912 0.734769 0.914765 11.00000 0.01414 0.02463 = 0.01878 -0.00339 -0.00372 -0.00604 MOLE 2 C22 1 0.653625 1.294516 0.600497 11.00000 0.01950 0.01683 = 0.02095 -0.00746 -0.00354 -0.00026 C24 1 0.434511 1.203250 0.554499 11.00000 0.02009 0.02254 = 0.02592 -0.00953 -0.00650 -0.00436 AFIX 43 H24 2 0.363464 1.179866 0.498671 11.00000 -1.20000 AFIX 0 C25 1 0.405042 1.161511 0.716295 11.00000 0.02102 0.02295 = 0.02391 -0.00649 -0.00649 -0.00726 AFIX 43 H25 2 0.308783 1.102876 0.797082 11.00000 -1.20000 AFIX 0 C26 1 0.819542 1.370152 0.576198 11.00000 0.01983 0.02577 = 0.03208 -0.00841 -0.00762 -0.00440 AFIX 137 H26A 2 0.865803 1.429983 0.459726 11.00000 -1.50000 H26B 2 0.920362 1.274081 0.619732 11.00000 -1.50000 H26C 2 0.782147 1.456394 0.633073 11.00000 -1.50000 AFIX 0 N21 3 0.541760 1.220333 0.742470 11.00000 0.02192 0.02481 = 0.01885 -0.00824 -0.00640 -0.00518 AFIX 43 H21 2 0.553169 1.210314 0.838276 11.00000 -1.20000 AFIX 0 N23 3 0.588552 1.286846 0.485640 11.00000 0.02165 0.02062 = 0.01639 -0.00553 -0.00427 -0.00298 AFIX 43 H23 2 0.636616 1.328989 0.380541 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 04skc0002a in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - O2 C1 C3 C3 - O3 C4 C2 C4 - O4A O4B C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C22 - N23 N21 C26 C24 - C25 N23 C25 - C24 N21 C26 - C22 N21 - C22 C25 N23 - C22 C24 Operators for generating equivalent atoms: $1 -x, -y+1, -z+2 $2 -x, -y+2, -z+1 $3 x+1, y, z $4 -x+1, -y+2, -z+2 $5 -x+1, -y+2, -z+1 7295 Reflections read, of which 11 rejected -9 =< h =< 9, -10 =< k =< 10, -11 =< l =< 11, Max. 2-theta = 54.94 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -5 -2 5 15.51 4.97 2 26.53 0 1 7 54.08 3.16 5 19.77 2 Inconsistent equivalents 2234 Unique reflections, of which 0 suppressed R(int) = 0.0805 R(sigma) = 0.1081 Friedel opposites merged Maximum memory for data reduction = 1846 / 22371 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 = 2257 / 187920 wR2 = 0.1312 before cycle 1 for 2234 data and 150 / 150 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0400 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.15136 0.00374 0.040 OSF 2 0.02209 0.00478 0.020 EXTI Mean shift/esd = 0.025 Maximum = -0.088 for z N23 Max. shift = 0.002 A for H1 Max. dU = 0.000 for C24 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2257 / 187920 wR2 = 0.1312 before cycle 2 for 2234 data and 150 / 150 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0400 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.15130 0.00374 -0.015 OSF 2 0.02211 0.00479 0.003 EXTI Mean shift/esd = 0.009 Maximum = -0.033 for z N23 Max. shift = 0.001 A for H1 Max. dU = 0.000 for C24 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2257 / 187920 wR2 = 0.1312 before cycle 3 for 2234 data and 150 / 150 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0400 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.15129 0.00374 -0.003 OSF 2 0.02210 0.00479 -0.001 EXTI Mean shift/esd = 0.001 Maximum = -0.013 for tors H26A Max. shift = 0.000 A for H26A Max. dU = 0.000 for C25 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2257 / 187920 wR2 = 0.1312 before cycle 4 for 2234 data and 150 / 150 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0400 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.15129 0.00374 0.000 OSF 2 0.02210 0.00479 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.006 for tors H26A Max. shift = 0.000 A for H26A Max. dU = 0.000 for N21 Largest correlation matrix elements 0.512 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.0615 0.6249 1.0297 13 1.000 0.000 C2 O2 C1 C3 H3 -0.0479 0.9253 0.9129 13 1.000 0.000 C3 O3 C4 C2 H1 0.5561 0.6961 0.8730 147 0.840 0.000 O1A C1 H1 H2O 0.2245 0.4649 0.8824 147 0.840 0.000 O2 C2 H2O H3O 0.0876 0.9798 0.6130 147 0.840 0.000 O3 C3 H3O H24 0.3634 1.1799 0.4987 43 0.950 0.000 C24 C25 N23 H25 0.3088 1.1029 0.7971 43 0.950 0.000 C25 C24 N21 H26A 0.8660 1.4298 0.4597 137 0.980 0.000 C26 C22 H26A H26B 0.9203 1.2741 0.6199 137 0.980 0.000 C26 C22 H26A H26C 0.7822 1.4565 0.6330 137 0.980 0.000 C26 C22 H26A H21 0.5532 1.2103 0.8383 43 0.880 0.000 N21 C22 C25 H23 0.6366 1.3290 0.3805 43 0.880 0.000 N23 C22 C24 04skc0002a in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.30768 0.72828 0.93528 1.00000 0.01685 0.01637 0.01382 0.00085 -0.00489 -0.00536 0.01678 0.00356 0.00037 0.00036 0.00029 0.00000 0.00141 0.00149 0.00126 0.00108 0.00112 0.00117 0.00060 C2 0.13508 0.68410 0.91869 1.00000 0.01459 0.02139 0.01693 -0.00745 -0.00306 -0.00730 0.01654 0.00330 0.00035 0.00036 0.00030 0.00000 0.00136 0.00157 0.00131 0.00112 0.00109 0.00119 0.00060 H2 0.06150 0.62491 1.02969 1.00000 0.01985 0.00000 0.00000 C3 0.01032 0.85768 0.83543 1.00000 0.01259 0.01828 0.01724 -0.00438 -0.00243 -0.00599 0.01610 0.00340 0.00034 0.00035 0.00029 0.00000 0.00133 0.00155 0.00128 0.00109 0.00109 0.00116 0.00060 H3 -0.04786 0.92525 0.91293 1.00000 0.01932 0.00000 0.00000 C4 -0.14938 0.81982 0.79222 1.00000 0.01316 0.01654 0.02169 -0.00506 -0.00598 -0.00043 0.01764 0.00351 0.00036 0.00036 0.00031 0.00000 0.00134 0.00150 0.00144 0.00113 0.00115 0.00116 0.00061 O1A 0.46821 0.67531 0.84941 1.00000 0.01079 0.02953 0.02171 -0.01030 -0.00442 -0.00591 0.01947 0.00232 0.00024 0.00026 0.00020 0.00000 0.00093 0.00119 0.00101 0.00085 0.00079 0.00086 0.00046 H1 0.55611 0.69607 0.87299 1.00000 0.02921 0.00000 0.00000 O1B 0.28435 0.81041 1.02734 1.00000 0.01828 0.02801 0.02008 -0.01033 -0.00583 -0.00467 0.02097 0.00236 0.00025 0.00025 0.00020 0.00000 0.00102 0.00120 0.00097 0.00087 0.00080 0.00087 0.00047 O2 0.18437 0.56953 0.82563 1.00000 0.01703 0.01681 0.01965 -0.00474 -0.00627 -0.00297 0.01783 0.00233 0.00025 0.00024 0.00020 0.00000 0.00099 0.00107 0.00095 0.00078 0.00077 0.00085 0.00045 H2O 0.22446 0.46494 0.88243 1.00000 0.02675 0.00000 0.00000 O3 0.12453 0.96214 0.69629 1.00000 0.01789 0.02584 0.01820 -0.00059 -0.00657 -0.01005 0.02093 0.00240 0.00025 0.00025 0.00021 0.00000 0.00102 0.00119 0.00093 0.00081 0.00079 0.00087 0.00048 H3O 0.08755 0.97979 0.61298 1.00000 0.03139 0.00000 0.00000 O4A -0.15856 0.87288 0.64894 1.00000 0.01989 0.02957 0.01710 -0.00357 -0.00778 -0.00702 0.02219 0.00245 0.00025 0.00026 0.00020 0.00000 0.00101 0.00118 0.00097 0.00081 0.00079 0.00088 0.00047 O4B -0.26693 0.73478 0.91477 1.00000 0.01413 0.02466 0.01879 -0.00342 -0.00374 -0.00604 0.01994 0.00237 0.00024 0.00025 0.00020 0.00000 0.00095 0.00114 0.00096 0.00080 0.00077 0.00085 0.00047 C22 0.65360 1.29451 0.60052 1.00000 0.01946 0.01683 0.02094 -0.00742 -0.00354 -0.00030 0.01971 0.00363 0.00037 0.00036 0.00031 0.00000 0.00147 0.00152 0.00140 0.00113 0.00119 0.00121 0.00062 C24 0.43447 1.20324 0.55450 1.00000 0.02008 0.02248 0.02577 -0.00944 -0.00650 -0.00440 0.02194 0.00381 0.00039 0.00037 0.00032 0.00000 0.00147 0.00164 0.00149 0.00122 0.00121 0.00127 0.00064 H24 0.36341 1.17986 0.49868 1.00000 0.02633 0.00000 0.00000 C25 0.40503 1.16150 0.71633 1.00000 0.02100 0.02295 0.02391 -0.00651 -0.00645 -0.00722 0.02204 0.00360 0.00039 0.00038 0.00032 0.00000 0.00149 0.00165 0.00148 0.00121 0.00119 0.00126 0.00065 H25 0.30878 1.10287 0.79714 1.00000 0.02645 0.00000 0.00000 C26 0.81958 1.37013 0.57622 1.00000 0.01986 0.02573 0.03216 -0.00842 -0.00763 -0.00445 0.02590 0.00377 0.00039 0.00040 0.00034 0.00000 0.00150 0.00173 0.00162 0.00130 0.00126 0.00131 0.00069 H26A 0.86596 1.42981 0.45973 1.00000 0.03886 0.00000 0.00000 H26B 0.92032 1.27406 0.61989 1.00000 0.03886 0.00000 0.00000 H26C 0.78217 1.45649 0.63296 1.00000 0.03886 0.00000 0.00000 N21 0.54176 1.22032 0.74248 1.00000 0.02195 0.02471 0.01888 -0.00817 -0.00647 -0.00516 0.02095 0.00292 0.00030 0.00030 0.00025 0.00000 0.00128 0.00142 0.00116 0.00101 0.00101 0.00111 0.00057 H21 0.55319 1.21029 0.83829 1.00000 0.02514 0.00000 0.00000 N23 0.58856 1.28684 0.48561 1.00000 0.02163 0.02061 0.01644 -0.00559 -0.00428 -0.00294 0.02003 0.00294 0.00031 0.00030 0.00026 0.00000 0.00126 0.00134 0.00111 0.00094 0.00096 0.00105 0.00054 H23 0.63665 1.32897 0.38051 1.00000 0.02404 0.00000 0.00000 Final Structure Factor Calculation for 04skc0002a in P-1 Total number of l.s. parameters = 150 Maximum vector length = 511 Memory required = 2107 / 22995 wR2 = 0.1312 before cycle 5 for 2234 data and 0 / 150 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0400 * P )^2 + 0.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0635 for 1344 Fo > 4sig(Fo) and 0.1256 for all 2234 data wR2 = 0.1312, GooF = S = 1.021, Restrained GooF = 1.021 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 0.0243 0.0156 0.0105 C1 0.0225 0.0164 0.0107 C2 0.0204 0.0174 0.0105 C3 0.0229 0.0184 0.0116 C4 0.0295 0.0205 0.0084 O1A 0.0281 0.0201 0.0147 O1B 0.0213 0.0171 0.0151 O2 0.0339 0.0159 0.0129 O3 0.0333 0.0201 0.0132 O4A 0.0288 0.0180 0.0130 O4B 0.0237 0.0207 0.0147 C22 0.0260 0.0219 0.0179 C24 0.0266 0.0226 0.0169 C25 0.0333 0.0258 0.0187 C26 0.0248 0.0224 0.0156 N21 0.0235 0.0203 0.0164 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 0.022 0.033 0.045 0.058 0.074 0.092 0.120 0.172 1.000 Number in group 224. 238. 218. 221. 227. 221. 227. 214. 220. 224. GooF 0.920 0.979 0.976 0.990 1.043 1.180 1.031 1.085 0.991 0.997 K 22.153 2.009 1.355 1.167 0.998 0.955 1.028 1.025 1.012 1.015 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. 220. 226. 220. 224. 224. 219. 223. 222. 225. GooF 1.002 1.051 1.027 1.078 0.969 0.983 0.934 0.873 1.019 1.232 K 1.166 1.102 1.045 1.129 1.026 1.053 1.024 1.005 1.035 1.000 R1 0.318 0.334 0.256 0.223 0.148 0.108 0.065 0.052 0.055 0.034 Recommended weighting scheme: WGHT 0.0394 0.3510 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 10 910.38 99.69 4.39 0.110 0.80 4 -1 10 1.06 38.84 4.27 0.069 0.78 2 -1 10 466.82 52.57 3.77 0.080 0.80 4 8 10 11.94 42.77 3.74 0.072 0.81 2 2 3 137.56 175.80 3.47 0.147 2.64 5 8 8 544.27 0.14 3.44 0.004 0.88 1 0 3 25.12 14.37 3.37 0.042 2.77 6 8 6 73.63 30.82 3.35 0.061 0.90 1 5 1 41.19 64.41 3.29 0.089 1.62 1 2 3 88.26 65.88 3.24 0.090 2.88 1 7 8 11.62 30.30 3.23 0.061 0.95 6 6 2 -2.58 14.00 3.19 0.041 1.03 5 -2 5 242.53 18.17 3.18 0.047 1.03 -2 -2 1 124.58 155.81 3.18 0.138 2.39 -5 2 6 14.86 32.50 3.13 0.063 0.89 3 2 10 59.23 32.76 3.12 0.063 0.90 5 -5 4 256.86 179.34 3.08 0.148 0.84 0 9 6 38.38 3.04 3.01 0.019 0.85 1 2 1 73.69 95.56 2.98 0.108 4.02 3 1 10 -12.87 14.58 2.91 0.042 0.87 3 1 4 25.69 38.54 2.84 0.069 1.90 1 -3 2 346.62 284.93 2.76 0.187 1.79 -5 1 6 444.20 334.99 2.75 0.202 0.89 -3 7 7 7.16 36.67 2.74 0.067 0.80 6 4 6 73.55 100.73 2.70 0.111 1.10 8 1 7 63.14 8.91 2.69 0.033 0.83 7 4 5 39.30 59.37 2.68 0.085 1.03 -3 1 4 12.47 6.32 2.68 0.028 1.41 1 1 0 1478.43 1676.04 2.68 0.453 5.72 7 6 1 22.49 8.11 2.65 0.031 0.91 3 -4 6 22.83 0.01 2.65 0.001 0.91 -1 -1 2 412.46 474.01 2.61 0.241 2.81 3 5 10 38.67 59.83 2.56 0.086 0.91 2 -6 5 -12.46 8.78 2.55 0.033 0.84 1 8 6 108.72 146.59 2.55 0.134 0.97 4 2 9 45.76 24.70 2.54 0.055 0.97 4 1 1 282.01 325.66 2.52 0.200 1.88 1 2 2 182.24 153.81 2.47 0.137 3.62 2 9 6 -7.82 11.54 2.47 0.038 0.90 9 2 6 39.25 0.29 2.45 0.006 0.80 0 2 3 98.48 119.05 2.44 0.121 2.69 -7 -6 1 171.15 15.81 2.43 0.044 0.83 5 2 4 42.97 28.77 2.39 0.059 1.42 3 -4 8 7.27 28.27 2.38 0.059 0.77 -3 5 8 -0.25 15.14 2.37 0.043 0.84 -2 -2 4 68.60 85.01 2.34 0.102 1.40 -1 0 4 146.31 116.28 2.32 0.119 1.87 -3 5 6 26.53 12.93 2.32 0.040 0.96 -2 2 0 66.23 51.84 2.32 0.080 2.35 3 1 11 49.43 82.34 2.32 0.100 0.79 Bond lengths and angles C1 - Distance Angles O1B 1.2313 (0.0031) O1A 1.2893 (0.0031) 125.52 (0.24) C2 1.5205 (0.0036) 118.53 (0.23) 115.96 (0.22) C1 - O1B O1A C2 - Distance Angles O2 1.4250 (0.0030) C1 1.5205 (0.0036) 112.61 (0.21) C3 1.5291 (0.0037) 108.73 (0.20) 108.68 (0.21) H2 1.0000 108.92 108.92 108.92 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4156 (0.0029) C4 1.5286 (0.0036) 111.71 (0.20) C2 1.5291 (0.0037) 109.26 (0.20) 110.90 (0.21) H3 1.0000 108.29 108.29 108.29 C3 - O3 C4 C2 C4 - Distance Angles O4A 1.2285 (0.0031) O4B 1.2924 (0.0030) 125.63 (0.24) C3 1.5286 (0.0036) 119.21 (0.22) 115.15 (0.21) C4 - O4A O4B O1A - Distance Angles C1 1.2893 (0.0031) H1 0.8400 109.47 O1A - C1 O1B - Distance Angles C1 1.2313 (0.0031) O1B - O2 - Distance Angles C2 1.4250 (0.0030) H2O 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4156 (0.0029) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.2285 (0.0031) O4A - O4B - Distance Angles C4 1.2924 (0.0030) O4B - C22 - Distance Angles N23 1.3255 (0.0034) N21 1.3328 (0.0033) 106.87 (0.24) C26 1.4827 (0.0038) 126.67 (0.24) 126.46 (0.25) C22 - N23 N21 C24 - Distance Angles C25 1.3454 (0.0038) N23 1.3814 (0.0035) 106.36 (0.25) H24 0.9500 126.82 126.82 C24 - C25 N23 C25 - Distance Angles C24 1.3454 (0.0038) N21 1.3828 (0.0034) 106.84 (0.24) H25 0.9500 126.58 126.58 C25 - C24 N21 C26 - Distance Angles C22 1.4827 (0.0038) 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 1.3328 (0.0033) C25 1.3828 (0.0034) 109.65 (0.22) H21 0.8800 125.17 125.17 N21 - C22 C25 N23 - Distance Angles C22 1.3255 (0.0034) C24 1.3814 (0.0035) 110.26 (0.22) H23 0.8800 124.87 124.87 N23 - C22 C24 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.17 2.664(3) 117.2 O3-H3O...O4A 0.84 1.98 2.773(3) 156.3 O2-H2O...O4B_$1 0.84 2.19 2.871(3) 137.6 O3-H3O...O4A_$2 0.84 1.65 2.487(2) 178.3 O1A-H1...O4B_$3 0.84 2.78 3.337(3) 125.1 O1A-H1...O4A_$3 0.88 1.93 2.715(3) 148.2 N21-H21...O1B_$4 0.88 1.98 2.825(3) 159.7 N23-H23...O2_$5 0.88 2.49 3.120(3) 128.7 N23-H23...O1A_$5 FMAP and GRID set by program FMAP 2 1 22 GRID -2.632 -2 -2 2.632 2 2 R1 = 0.1255 for 2234 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.3966 0.2345 0.4368 [ 0.60 A from H24 ] Deepest hole -0.33 at 0.1887 0.9332 0.5804 [ 0.78 A from H3O ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2119 / 16607 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3966 1.2345 0.4368 1.00000 0.05 0.32 0.60 H24 1.12 C24 1.85 N23 2.03 H23 Q2 1 -0.0606 0.8475 0.8019 1.00000 0.05 0.29 0.74 C3 0.81 C4 1.45 H3 1.70 O4A Q3 1 -0.3106 0.7832 0.7398 1.00000 0.05 0.28 1.41 O4A 1.41 H1 1.58 C4 1.61 O4B Q4 1 -0.0013 0.9319 0.5946 1.00000 0.05 0.26 0.96 H3O 1.30 O4A 1.65 O3 1.85 C4 Q5 1 0.4447 0.8983 0.9336 1.00000 0.05 0.26 1.45 O1B 1.87 H1 1.90 H25 1.93 H21 Q6 1 0.3263 1.2619 0.5247 1.00000 0.05 0.25 0.76 H24 0.88 C24 1.83 C25 1.96 N23 Q7 1 -0.2683 0.7314 1.0584 1.00000 0.05 0.24 1.31 O4B 1.47 H2O 2.07 H21 2.18 H25 Q8 1 0.3005 1.1189 0.8395 1.00000 0.05 0.24 0.44 H25 1.15 C25 2.03 N21 2.25 H21 Q9 1 -0.2368 0.6282 0.9477 1.00000 0.05 0.23 0.80 O4B 1.46 H2O 1.76 H1 1.80 C4 Q10 1 0.8754 1.5634 0.4080 1.00000 0.05 0.23 1.04 H26A 1.78 C26 1.89 H26C 2.23 H26B Shortest distances between peaks (including symmetry equivalents) 1 6 0.89 7 9 1.50 4 4 1.65 2 4 1.71 7 8 1.77 5 8 1.86 6 10 1.91 3 9 1.98 1 3 2.00 2 9 2.30 2 3 2.39 2 7 2.39 3 5 2.41 5 7 2.54 6 8 2.62 10 10 2.63 3 6 2.65 1 10 2.68 3 4 2.69 5 9 2.77 5 5 2.86 3 7 2.89 8 10 3.00 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 0.03: 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. 0.34: 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 0.28: Structure factors and derivatives 0.33: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.08: 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 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04skc0002a finished at 13:53:54 Total CPU time: 1.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++