+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0004p21c started at 15:14:53 on 21-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0004p21c in P2(1)/c CELL 0.71073 5.7683 13.7020 14.4419 90.000 97.458 90.000 ZERR 4.00 0.0009 0.0027 0.0026 0.000 0.011 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 40 68 4 20 V = 1131.79 F(000) = 496.0 Mu = 0.11 mm-1 Cell Wt = 924.98 Rho = 1.357 MERG 2 OMIT -3.00 55.00 OMIT -3 0 4 OMIT -3 1 4 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.01 0.02 0.18 ACTA BOND $H WGHT 0.04250 9.22550 L.S. 4 TEMP -153.00 FVAR 0.54054 MOLE 1 C1 1 -0.248546 1.064977 0.098846 11.00000 0.01932 0.04106 = 0.02488 -0.00053 -0.00308 0.00485 C2 1 -0.217765 0.955095 0.098712 11.00000 0.03371 0.02216 = 0.02939 0.00234 -0.00571 0.00401 AFIX 23 H2A 2 -0.339652 0.924207 0.131254 11.00000 -1.2000 H2B 2 -0.237020 0.931019 0.033532 11.00000 -1.2000 AFIX 0 C3 1 0.019660 0.926828 0.146429 11.00000 0.02366 0.02122 = 0.02949 -0.00196 0.00659 0.00117 AFIX 13 H3 2 0.139265 0.967134 0.119637 11.00000 -1.2000 AFIX 0 C4 1 0.067244 0.819629 0.127631 11.00000 0.02492 0.03005 = 0.02787 0.00177 0.00376 -0.00129 C5 1 -0.523293 1.190526 0.104726 11.00000 0.02738 0.03502 = 0.04227 0.00450 0.00399 -0.00261 AFIX 137 H5A 2 -0.408879 1.227550 0.146958 11.00000 -1.50000 H5B 2 -0.679914 1.200756 0.122357 11.00000 -1.50000 H5C 2 -0.519983 1.212883 0.040453 11.00000 -1.50000 AFIX 0 C6 1 0.359123 0.699216 0.136887 11.00000 0.03889 0.02240 = 0.04222 -0.00721 -0.00245 0.00918 AFIX 137 H6A 2 0.290777 0.660047 0.183254 11.00000 -1.50000 H6B 2 0.529555 0.691879 0.146392 11.00000 -1.50000 H6C 2 0.297686 0.676911 0.073995 11.00000 -1.50000 AFIX 0 C22 1 0.270587 0.975264 0.290170 11.00000 0.02599 0.03078 = 0.02973 0.00675 -0.00544 -0.00363 AFIX 23 H22A 2 0.330384 1.030262 0.255647 11.00000 -1.20000 H22B 2 0.377029 0.918953 0.287450 11.00000 -1.20000 AFIX 0 C23 1 0.261413 1.004348 0.391149 11.00000 0.03665 0.02654 = 0.02619 0.00255 -0.00124 0.00298 AFIX 23 H23A 2 0.420556 1.021897 0.420605 11.00000 -1.20000 H23B 2 0.160572 1.062605 0.392934 11.00000 -1.20000 AFIX 0 C25 1 -0.057915 0.903611 0.402150 11.00000 0.03012 0.03847 = 0.02995 0.00523 0.00752 -0.00559 AFIX 23 H25A 2 -0.161678 0.960850 0.404601 11.00000 -1.20000 H25B 2 -0.117537 0.850431 0.439007 11.00000 -1.20000 AFIX 0 C26 1 -0.062193 0.870963 0.301818 11.00000 0.02148 0.03900 = 0.03512 -0.00599 0.00525 -0.00081 AFIX 23 H26A 2 0.032109 0.810867 0.299402 11.00000 -1.20000 H26B 2 -0.224799 0.856261 0.274479 11.00000 -1.20000 AFIX 0 N21 3 0.034105 0.949149 0.247743 11.00000 0.02256 0.02567 = 0.02900 0.00037 0.00482 -0.00257 O1A 4 -0.102873 1.123562 0.085750 11.00000 0.02762 0.03509 = 0.06162 0.00342 0.00759 -0.00458 O1B 4 -0.466850 1.089522 0.111126 11.00000 0.02564 0.02972 = 0.03761 -0.00063 0.00776 0.00592 O4A 4 0.299193 0.800671 0.147237 11.00000 0.02658 0.02858 = 0.04295 -0.00818 0.00316 0.00672 O4B 4 -0.076434 0.759830 0.101970 11.00000 0.02619 0.03588 = 0.04130 -0.00237 0.00373 -0.00207 O24 4 0.174222 0.928778 0.442031 11.00000 0.04108 0.03784 = 0.02559 0.00280 -0.00184 -0.00818 HKLF 4 Covalent radii and connectivity table for 07skc0004p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C3 C1 C3 - N21 C2 C4 C4 - O4B O4A C3 C5 - O1B C6 - O4A C22 - N21 C23 C23 - O24 C22 C25 - O24 C26 C26 - N21 C25 N21 - C22 C26 C3 O1A - C1 O1B - C1 C5 O4A - C4 C6 O4B - C4 O24 - C23 C25 h k l Fo^2 Sigma Why rejected -4 0 5 18.75 3.67 observed but should be systematically absent 12702 Reflections read, of which 431 rejected -7 =< h =< 7, -17 =< k =< 17, -18 =< l =< 18, Max. 2-theta = 54.97 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -5 5 5 2.64 0.76 5 5.76 2 5 10 47.35 3.54 4 30.09 -4 11 10 14.67 9.34 2 47.73 3 Inconsistent equivalents 2590 Unique reflections, of which 0 suppressed R(int) = 0.1974 R(sigma) = 0.1928 Friedel opposites merged Maximum memory for data reduction = 1745 / 25648 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 = 2180 / 184401 wR2 = 0.3148 before cycle 1 for 2590 data and 147 / 147 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0425 * P )^2 + 9.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54051 0.00302 -0.010 OSF Mean shift/esd = 0.014 Maximum = -0.107 for U33 C2 Max. shift = 0.001 A for H5A Max. dU = 0.000 for C3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2180 / 184401 wR2 = 0.3147 before cycle 2 for 2590 data and 147 / 147 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0425 * P )^2 + 9.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54050 0.00302 -0.002 OSF Mean shift/esd = 0.007 Maximum = -0.047 for U33 C2 Max. shift = 0.001 A for H5A Max. dU = 0.000 for C3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2180 / 184401 wR2 = 0.3147 before cycle 3 for 2590 data and 147 / 147 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0425 * P )^2 + 9.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54050 0.00301 0.000 OSF Mean shift/esd = 0.002 Maximum = 0.009 for U11 C3 Max. shift = 0.000 A for H5A Max. dU = 0.000 for C3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2180 / 184401 wR2 = 0.3147 before cycle 4 for 2590 data and 147 / 147 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0425 * P )^2 + 9.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54050 0.00301 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.003 for tors H5A Max. shift = 0.000 A for H5A Max. dU = 0.000 for C3 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 -0.3396 0.9242 0.1313 23 0.990 0.000 C2 C3 C1 H2B -0.2370 0.9310 0.0335 23 0.990 0.000 C2 C3 C1 H3 0.1393 0.9671 0.1196 13 1.000 0.000 C3 N21 C2 C4 H5A -0.4086 1.2276 0.1468 137 0.980 0.000 C5 O1B H5A H5B -0.6797 1.2008 0.1225 137 0.980 0.000 C5 O1B H5A H5C -0.5203 1.2128 0.0404 137 0.980 0.000 C5 O1B H5A H6A 0.2909 0.6600 0.1833 137 0.980 0.000 C6 O4A H6A H6B 0.5296 0.6919 0.1464 137 0.980 0.000 C6 O4A H6A H6C 0.2976 0.6769 0.0740 137 0.980 0.000 C6 O4A H6A H22A 0.3303 1.0303 0.2556 23 0.990 0.000 C22 N21 C23 H22B 0.3770 0.9190 0.2875 23 0.990 0.000 C22 N21 C23 H23A 0.4206 1.0219 0.4206 23 0.990 0.000 C23 O24 C22 H23B 0.1606 1.0626 0.3930 23 0.990 0.000 C23 O24 C22 H25A -0.1617 0.9608 0.4046 23 0.990 0.000 C25 O24 C26 H25B -0.1175 0.8504 0.4390 23 0.990 0.000 C25 O24 C26 H26A 0.0321 0.8109 0.2994 23 0.990 0.000 C26 N21 C25 H26B -0.2248 0.8562 0.2745 23 0.990 0.000 C26 N21 C25 07skc0004p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.24854 1.06498 0.09884 1.00000 0.01920 0.04111 0.02487 -0.00052 -0.00293 0.00496 0.02890 0.01417 0.00122 0.00064 0.00051 0.00000 0.00373 0.00529 0.00398 0.00377 0.00315 0.00379 0.00184 C2 -0.21775 0.95512 0.09872 1.00000 0.03386 0.02238 0.02872 0.00227 -0.00563 0.00388 0.02917 0.01395 0.00130 0.00056 0.00055 0.00000 0.00416 0.00438 0.00416 0.00352 0.00341 0.00354 0.00181 H2A -0.33963 0.92424 0.13127 1.00000 0.03501 0.00000 0.00000 H2B -0.23703 0.93104 0.03354 1.00000 0.03501 0.00000 0.00000 C3 0.01965 0.92683 0.14642 1.00000 0.02421 0.02111 0.02939 -0.00226 0.00618 0.00147 0.02466 0.01332 0.00122 0.00054 0.00051 0.00000 0.00368 0.00437 0.00402 0.00337 0.00320 0.00324 0.00170 H3 0.13927 0.96714 0.11964 1.00000 0.02960 0.00000 0.00000 C4 0.06722 0.81962 0.12762 1.00000 0.02490 0.03006 0.02774 0.00166 0.00364 -0.00138 0.02755 0.01438 0.00129 0.00059 0.00052 0.00000 0.00401 0.00479 0.00429 0.00362 0.00332 0.00366 0.00179 C5 -0.52325 1.19053 0.10471 1.00000 0.02709 0.03506 0.04235 0.00445 0.00397 -0.00253 0.03488 0.01518 0.00134 0.00061 0.00060 0.00000 0.00417 0.00522 0.00492 0.00412 0.00372 0.00368 0.00201 H5A -0.40858 1.22756 0.14682 1.00000 0.05232 0.00000 0.00000 H5B -0.67970 1.20080 0.12250 1.00000 0.05232 0.00000 0.00000 H5C -0.52032 1.21284 0.04040 1.00000 0.05232 0.00000 0.00000 C6 0.35914 0.69919 0.13690 1.00000 0.03874 0.02239 0.04218 -0.00723 -0.00238 0.00928 0.03511 0.01489 0.00144 0.00057 0.00059 0.00000 0.00461 0.00460 0.00495 0.00389 0.00386 0.00378 0.00201 H6A 0.29090 0.66004 0.18331 1.00000 0.05267 0.00000 0.00000 H6B 0.52957 0.69186 0.14636 1.00000 0.05267 0.00000 0.00000 H6C 0.29759 0.67686 0.07403 1.00000 0.05267 0.00000 0.00000 C22 0.27056 0.97526 0.29018 1.00000 0.02590 0.03069 0.02966 0.00662 -0.00525 -0.00370 0.02953 0.01327 0.00125 0.00060 0.00052 0.00000 0.00389 0.00474 0.00425 0.00359 0.00331 0.00347 0.00185 H22A 0.33032 1.03027 0.25565 1.00000 0.03543 0.00000 0.00000 H22B 0.37704 0.91897 0.28745 1.00000 0.03543 0.00000 0.00000 C23 0.26144 1.00435 0.39116 1.00000 0.03667 0.02646 0.02630 0.00250 -0.00117 0.00301 0.03027 0.01438 0.00138 0.00060 0.00051 0.00000 0.00454 0.00459 0.00403 0.00367 0.00352 0.00365 0.00186 H23A 0.42060 1.02188 0.42061 1.00000 0.03633 0.00000 0.00000 H23B 0.16064 1.06262 0.39295 1.00000 0.03633 0.00000 0.00000 C25 -0.05792 0.90361 0.40214 1.00000 0.03026 0.03846 0.02990 0.00524 0.00761 -0.00559 0.03255 0.01407 0.00134 0.00063 0.00052 0.00000 0.00416 0.00512 0.00434 0.00386 0.00356 0.00371 0.00196 H25A -0.16168 0.96085 0.40458 1.00000 0.03906 0.00000 0.00000 H25B -0.11755 0.85043 0.43900 1.00000 0.03906 0.00000 0.00000 C26 -0.06218 0.87095 0.30184 1.00000 0.02148 0.03896 0.03517 -0.00612 0.00533 -0.00094 0.03172 0.01406 0.00128 0.00062 0.00054 0.00000 0.00380 0.00515 0.00449 0.00402 0.00354 0.00364 0.00192 H26A 0.03213 0.81086 0.29944 1.00000 0.03807 0.00000 0.00000 H26B -0.22478 0.85624 0.27451 1.00000 0.03807 0.00000 0.00000 N21 0.03411 0.94912 0.24775 1.00000 0.02254 0.02570 0.02900 0.00044 0.00474 -0.00266 0.02562 0.01089 0.00098 0.00046 0.00042 0.00000 0.00310 0.00359 0.00344 0.00295 0.00266 0.00284 0.00145 O1A -0.10287 1.12357 0.08574 1.00000 0.02754 0.03512 0.06171 0.00336 0.00759 -0.00467 0.04130 0.01061 0.00094 0.00043 0.00043 0.00000 0.00306 0.00361 0.00416 0.00311 0.00289 0.00282 0.00156 O1B -0.46687 1.08953 0.11112 1.00000 0.02575 0.02972 0.03756 -0.00074 0.00772 0.00594 0.03069 0.00956 0.00087 0.00038 0.00037 0.00000 0.00271 0.00325 0.00310 0.00262 0.00242 0.00240 0.00132 O4A 0.29920 0.80068 0.14724 1.00000 0.02658 0.02864 0.04300 -0.00820 0.00320 0.00674 0.03286 0.00959 0.00088 0.00039 0.00037 0.00000 0.00280 0.00327 0.00334 0.00268 0.00252 0.00248 0.00139 O4B -0.07644 0.75982 0.10197 1.00000 0.02615 0.03590 0.04138 -0.00241 0.00369 -0.00195 0.03454 0.00999 0.00088 0.00042 0.00038 0.00000 0.00288 0.00354 0.00335 0.00281 0.00254 0.00272 0.00141 O24 0.17419 0.92878 0.44203 1.00000 0.04088 0.03799 0.02554 0.00276 -0.00184 -0.00812 0.03534 0.00963 0.00094 0.00042 0.00036 0.00000 0.00319 0.00360 0.00281 0.00265 0.00244 0.00277 0.00141 Final Structure Factor Calculation for 07skc0004p21c in P2(1)/c Total number of l.s. parameters = 147 Maximum vector length = 511 Memory required = 2033 / 22995 wR2 = 0.3147 before cycle 5 for 2590 data and 0 / 147 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0425 * P )^2 + 9.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1456 for 1150 Fo > 4sig(Fo) and 0.2800 for all 2590 data wR2 = 0.3147, GooF = S = 1.121, Restrained GooF = 1.121 for all data Occupancy sum of asymmetric unit = 16.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.0425 0.0285 0.0157 C1 0.0429 0.0262 0.0184 C2 0.0305 0.0243 0.0192 C3 0.0312 0.0271 0.0243 C4 0.0449 0.0336 0.0261 C5 0.0542 0.0339 0.0172 C6 0.0432 0.0258 0.0196 C22 0.0399 0.0288 0.0221 C23 0.0425 0.0334 0.0218 C25 0.0435 0.0307 0.0210 C26 0.0291 0.0272 0.0205 N21 0.0622 0.0372 0.0245 O1A 0.0382 0.0336 0.0202 O1B 0.0482 0.0312 0.0192 O4A 0.0423 0.0355 0.0258 O4B 0.0505 0.0315 0.0241 O24 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.012 0.018 0.025 0.033 0.042 0.055 0.074 0.111 1.000 Number in group 310. 219. 265. 255. 260. 257. 257. 256. 254. 257. GooF 1.359 1.075 1.080 1.057 1.232 1.149 1.057 1.082 0.931 1.066 K 50.316 6.075 2.474 2.062 1.658 1.171 1.057 1.031 1.002 1.004 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.14 1.32 1.65 inf Number in group 265. 257. 260. 258. 257. 263. 255. 256. 258. 261. GooF 1.157 1.166 1.157 1.107 1.070 1.057 1.064 1.095 1.066 1.248 K 1.695 1.894 1.425 1.433 1.123 1.080 1.033 1.011 1.033 1.009 R1 0.586 0.545 0.491 0.451 0.346 0.287 0.183 0.166 0.122 0.073 Recommended weighting scheme: WGHT 0.0425 9.2691 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 9 0 335.01 21.14 6.23 0.027 1.19 -3 2 3 894.43 387.73 5.61 0.117 1.79 3 1 0 421.82 133.66 5.16 0.068 1.89 1 0 0 4469.40 7256.45 5.08 0.505 5.72 -3 4 5 126.39 1.14 5.05 0.006 1.52 -3 2 9 135.27 20.86 3.69 0.027 1.28 -5 2 12 279.52 19.71 3.52 0.026 0.88 -1 9 1 105.00 7.42 3.51 0.016 1.47 -3 3 2 88.53 6.69 3.45 0.015 1.76 0 8 15 173.69 22.42 3.43 0.028 0.83 -4 0 10 -29.88 187.51 3.31 0.081 1.08 3 0 0 303.58 135.59 3.24 0.069 1.91 -2 11 3 88.92 0.24 3.14 0.003 1.12 -4 11 4 20.53 177.46 3.13 0.079 0.93 6 9 2 135.85 0.35 3.12 0.004 0.79 -3 2 4 1276.17 880.76 3.11 0.176 1.72 0 8 13 119.36 1.31 3.08 0.007 0.93 2 16 3 216.45 0.18 3.08 0.003 0.80 -6 6 10 154.30 32.23 3.01 0.034 0.79 3 6 6 163.49 38.41 2.93 0.037 1.20 -1 11 7 98.83 1.31 2.92 0.007 1.06 0 1 13 126.23 27.35 2.92 0.031 1.10 -4 12 5 254.89 98.56 2.89 0.059 0.87 -6 3 9 330.06 71.97 2.86 0.050 0.85 2 14 8 133.13 0.99 2.83 0.006 0.81 -3 2 10 61.38 6.21 2.80 0.015 1.20 3 3 4 66.37 0.46 2.80 0.004 1.51 -3 8 6 86.16 11.75 2.79 0.020 1.17 5 8 8 151.61 20.22 2.78 0.027 0.80 0 0 6 9434.96 7864.60 2.78 0.525 2.39 -3 10 6 102.66 13.50 2.77 0.022 1.04 3 7 7 134.37 20.78 2.77 0.027 1.09 0 11 12 190.89 38.93 2.72 0.037 0.86 -7 5 6 372.42 0.17 2.71 0.002 0.77 -4 5 5 47.25 1.60 2.70 0.007 1.21 3 9 5 116.84 0.87 2.66 0.006 1.07 3 6 3 115.48 30.82 2.65 0.033 1.36 -5 0 14 181.25 1.35 2.60 0.007 0.82 0 7 2 2265.82 1777.26 2.60 0.250 1.89 3 0 4 284.28 141.87 2.57 0.071 1.60 3 10 8 125.19 1.06 2.57 0.006 0.91 3 11 0 75.59 1.16 2.55 0.006 1.04 4 14 2 123.87 0.00 2.55 0.000 0.80 -3 15 5 123.36 7.54 2.54 0.016 0.80 -7 1 3 70.99 0.42 2.53 0.004 0.82 -5 8 8 344.11 12.11 2.51 0.021 0.88 -1 5 17 116.78 0.18 2.50 0.002 0.81 -3 9 5 132.07 39.77 2.50 0.037 1.13 -4 5 11 113.80 2.22 2.45 0.009 0.97 -3 4 3 116.55 42.57 2.42 0.039 1.63 Bond lengths and angles C1 - Distance Angles O1A 1.1948 (0.0091) O1B 1.3374 (0.0084) 123.07 (0.77) C2 1.5158 (0.0114) 125.60 (0.70) 111.25 (0.68) C1 - O1A O1B C2 - Distance Angles C3 1.5017 (0.0098) C1 1.5158 (0.0113) 110.84 (0.64) H2A 0.9900 109.47 109.47 H2B 0.9900 109.47 109.47 108.06 C2 - C3 C1 H2A C3 - Distance Angles N21 1.4866 (0.0093) C2 1.5017 (0.0098) 109.26 (0.58) C4 1.5252 (0.0106) 112.62 (0.61) 109.96 (0.63) H3 1.0000 108.30 108.30 108.30 C3 - N21 C2 C4 C4 - Distance Angles O4B 1.1898 (0.0088) O4A 1.3564 (0.0086) 124.17 (0.73) C3 1.5252 (0.0106) 125.77 (0.69) 110.03 (0.64) C4 - O4B O4A C5 - Distance Angles O1B 1.4219 (0.0094) H5A 0.9800 109.47 H5B 0.9800 109.47 109.47 H5C 0.9800 109.47 109.47 109.47 C5 - O1B H5A H5B C6 - Distance Angles O4A 1.4453 (0.0090) H6A 0.9800 109.47 H6B 0.9800 109.47 109.47 H6C 0.9800 109.47 109.47 109.47 C6 - O4A H6A H6B C22 - Distance Angles N21 1.4653 (0.0089) C23 1.5194 (0.0106) 108.61 (0.62) H22A 0.9900 109.97 109.97 H22B 0.9900 109.97 109.97 108.35 C22 - N21 C23 H22A C23 - Distance Angles O24 1.4005 (0.0091) C22 1.5194 (0.0106) 111.66 (0.66) H23A 0.9900 109.29 109.29 H23B 0.9900 109.29 109.29 107.95 C23 - O24 C22 H23A C25 - Distance Angles O24 1.4294 (0.0089) C26 1.5132 (0.0105) 110.80 (0.62) H25A 0.9900 109.48 109.48 H25B 0.9900 109.48 109.48 108.06 C25 - O24 C26 H25A C26 - Distance Angles N21 1.4760 (0.0096) C25 1.5132 (0.0105) 109.37 (0.65) H26A 0.9900 109.80 109.80 H26B 0.9900 109.80 109.80 108.25 C26 - N21 C25 H26A N21 - Distance Angles C22 1.4653 (0.0089) C26 1.4760 (0.0096) 110.48 (0.58) C3 1.4866 (0.0093) 113.08 (0.56) 113.27 (0.58) N21 - C22 C26 O1A - Distance Angles C1 1.1948 (0.0091) O1A - O1B - Distance Angles C1 1.3374 (0.0084) C5 1.4219 (0.0094) 116.58 (0.62) O1B - C1 O4A - Distance Angles C4 1.3564 (0.0086) C6 1.4453 (0.0090) 113.91 (0.62) O4A - C4 O4B - Distance Angles C4 1.1898 (0.0088) O4B - O24 - Distance Angles C23 1.4005 (0.0091) C25 1.4294 (0.0090) 110.40 (0.59) O24 - C23 FMAP and GRID set by program FMAP 2 1 16 GRID -3.846 -2 -1 3.846 2 1 R1 = 0.2800 for 2590 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.48 at 0.2357 0.0887 0.1139 [ 1.61 A from H5B ] Deepest hole -0.43 at 0.0172 0.8584 0.2170 [ 1.32 A from N21 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 2421 / 24942 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.7643 1.0887 0.1139 1.00000 0.05 0.48 1.61 H5B 1.72 O1B 1.76 H3 1.99 C5 Q2 1 0.4175 0.9456 0.2486 1.00000 0.05 0.48 0.73 H22B 1.17 C22 1.27 H22A 2.21 N21 Q3 1 -0.3332 0.8575 0.1204 1.00000 0.05 0.44 0.93 H2A 1.54 C2 1.75 H2B 2.04 O4B Q4 1 0.6067 0.7800 0.1138 1.00000 0.05 0.43 1.39 H6B 1.87 C6 1.88 O4B 1.92 O4A Q5 1 -0.4131 0.9024 0.3876 1.00000 0.05 0.35 1.65 H25A 1.78 H22B 1.91 H25B 1.99 H23A Q6 1 0.5810 0.9735 0.2983 1.00000 0.05 0.35 1.39 H22B 1.69 H22A 1.78 C22 2.00 H25A Q7 1 -0.3854 0.9558 0.2296 1.00000 0.05 0.35 1.54 H2A 1.73 H26B 1.77 H22B 2.01 H22A Q8 1 0.3328 0.9574 0.0878 1.00000 0.05 0.34 1.27 H3 1.97 H2A 2.13 C3 2.15 O1B Q9 1 0.3015 0.8885 0.2927 1.00000 0.05 0.34 0.62 H22B 1.20 C22 1.80 N21 1.90 H26A Q10 1 0.3605 0.8440 0.4324 1.00000 0.05 0.32 1.60 O24 2.00 H5A 2.03 H5C 2.14 H6C Shortest distances between peaks (including symmetry equivalents) 6 7 1.06 3 4 1.12 2 6 1.17 2 7 1.21 2 9 1.26 5 6 1.61 5 10 1.73 1 8 1.94 6 9 1.98 5 9 2.01 9 10 2.09 3 7 2.12 2 5 2.20 2 8 2.31 7 9 2.32 3 8 2.36 5 7 2.42 7 8 2.44 2 3 2.76 1 2 2.86 4 8 2.90 4 7 2.93 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 0.00: Analyse other restraints etc. 0.58: 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 0.55: 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 0.00: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0004p21c finished at 15:14:54 Total CPU time: 1.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++