+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0048pna21 started at 14:38:05 on 21-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0048pna21 in Pna2(1) CELL 0.71073 10.4056 22.8884 4.6392 90.000 90.000 90.000 ZERR 4.00 0.0016 0.0040 0.0009 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H N O UNIT 40 64 8 16 V = 1104.91 F(000) = 488.0 Mu = 0.11 mm-1 Cell Wt = 912.99 Rho = 1.372 MERG 4 OMIT -3.00 55.00 OMIT 0 4 0 SHEL 7 0.77 EQIV_$1 x-1/2, -y+3/2, z-1 HTAB O5B O1B_$1 EQIV_$2 -x+1, -y+1, z-1/2 HTAB N23 O1A_$2 FMAP 2 PLAN 10 SIZE 0.06 0.10 0.12 ACTA BOND $H WGHT 0.11940 L.S. 4 TEMP -153.00 FVAR 0.69189 MOLE 1 C1 1 0.472665 0.673292 0.261380 11.00000 0.02561 0.02332 = 0.03669 -0.00605 -0.00421 -0.00222 C2 1 0.375458 0.700657 0.062566 11.00000 0.04235 0.02456 = 0.02928 0.00410 0.00146 0.00021 AFIX 23 H2A 2 0.422237 0.720561 -0.095188 11.00000 -1.20000 H2B 2 0.328071 0.730992 0.171389 11.00000 -1.20000 AFIX 0 C3 1 0.277784 0.659013 -0.071347 11.00000 0.03462 0.02821 = 0.03607 0.00396 -0.00010 -0.00008 AFIX 23 H3A 2 0.322625 0.630607 -0.196970 11.00000 -1.20000 H3B 2 0.233219 0.636995 0.082750 11.00000 -1.20000 AFIX 0 C4 1 0.180069 0.693098 -0.247423 11.00000 0.04162 0.02247 = 0.03700 -0.00289 0.00724 -0.00628 AFIX 23 H4A 2 0.133740 0.720183 -0.117486 11.00000 -1.20000 H4B 2 0.226533 0.717025 -0.391443 11.00000 -1.20000 AFIX 0 C5 1 0.082441 0.655458 -0.403224 11.00000 0.02114 0.03526 = 0.03001 0.00097 0.00346 0.00724 O1A 4 0.477521 0.619057 0.282785 11.00000 0.04615 0.01941 = 0.04314 0.00148 -0.00375 0.00257 O1B 4 0.543744 0.707538 0.405924 11.00000 0.04398 0.02541 = 0.04249 -0.00113 -0.01144 0.00313 O5A 4 0.072838 0.603450 -0.368458 11.00000 0.05009 0.01657 = 0.04823 -0.00107 -0.00548 0.00184 O5B 4 0.003381 0.683172 -0.577947 11.00000 0.04582 0.02219 = 0.04355 -0.00187 -0.01060 0.00059 AFIX 147 H5 2 0.019638 0.719112 -0.574306 11.00000 -1.50000 AFIX 0 MOLE 2 C22 1 0.277862 0.412519 0.330685 11.00000 0.02303 0.02536 = 0.03755 -0.00005 -0.01046 -0.00036 C24 1 0.363479 0.494418 0.166181 11.00000 0.02252 0.02316 = 0.04644 -0.00316 -0.00241 0.00301 AFIX 43 H24 2 0.415973 0.520646 0.059756 11.00000 -1.20000 AFIX 0 C25 1 0.273221 0.509052 0.355592 11.00000 0.05663 0.01171 = 0.03379 0.00105 -0.00336 0.00303 AFIX 43 H25 2 0.250243 0.547609 0.411183 11.00000 -1.20000 AFIX 0 C26 1 0.112994 0.453683 0.663068 11.00000 0.04208 0.02636 = 0.03416 -0.00255 -0.00345 -0.00052 AFIX 137 H26A 2 0.036236 0.438848 0.564957 11.00000 -1.50000 H26B 2 0.094899 0.492427 0.743300 11.00000 -1.50000 H26C 2 0.136875 0.426941 0.819105 11.00000 -1.50000 AFIX 0 C27 1 0.251390 0.350658 0.378615 11.00000 0.04402 0.02366 = 0.04344 0.00124 0.00044 -0.00020 AFIX 137 H27A 2 0.318563 0.327088 0.286962 11.00000 -1.50000 H27B 2 0.167744 0.340681 0.294939 11.00000 -1.50000 H27C 2 0.250087 0.342667 0.586126 11.00000 -1.50000 AFIX 0 N21 3 0.218898 0.457909 0.456905 11.00000 0.03732 0.02508 = 0.03558 -0.00588 0.00043 0.00191 N23 3 0.367102 0.434398 0.152186 11.00000 0.04017 0.02352 = 0.03305 -0.00825 -0.00008 0.00279 AFIX 43 H23 2 0.419480 0.413717 0.043704 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0048pna21 in Pna2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C1 C3 C3 - C4 C2 C4 - C5 C3 C5 - O5A O5B C4 O1A - C1 O1B - C1 O5A - C5 O5B - C5 C22 - N21 N23 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-1/2, -y+3/2, z-1 $2 -x+1, -y+1, z-1/2 Floating origin restraints generated 7004 Reflections read, of which 353 rejected -13 =< h =< 11, -27 =< k =< 29, -6 =< l =< 5, Max. 2-theta = 54.94 0 Systematic absence violations 0 Inconsistent equivalents 1362 Unique reflections, of which 0 suppressed R(int) = 0.1474 R(sigma) = 0.1371 Friedel opposites merged Maximum memory for data reduction = 1792 / 13445 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 = 2225 / 185573 wR2 = 0.2227 before cycle 1 for 1362 data and 148 / 148 parameters GooF = S = 1.039; Restrained GooF = 1.038 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1194 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69140 0.00481 -0.103 OSF Mean shift/esd = 0.038 Maximum = 0.164 for x O1A Max. shift = 0.005 A for H27B Max. dU = 0.000 for O5B Least-squares cycle 2 Maximum vector length = 511 Memory required = 2225 / 185573 wR2 = 0.2226 before cycle 2 for 1362 data and 148 / 148 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1194 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69128 0.00480 -0.025 OSF Mean shift/esd = 0.016 Maximum = 0.063 for x O1A Max. shift = 0.002 A for H26B Max. dU = 0.000 for O5B Least-squares cycle 3 Maximum vector length = 511 Memory required = 2225 / 185573 wR2 = 0.2225 before cycle 3 for 1362 data and 148 / 148 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1194 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69126 0.00480 -0.003 OSF Mean shift/esd = 0.003 Maximum = 0.017 for tors H26A Max. shift = 0.001 A for H26B Max. dU = 0.000 for O5B Least-squares cycle 4 Maximum vector length = 511 Memory required = 2225 / 185573 wR2 = 0.2225 before cycle 4 for 1362 data and 148 / 148 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1194 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.69126 0.00480 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.008 for tors H26A Max. shift = 0.000 A for H26B Max. dU = 0.000 for C22 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 0.4224 0.7205 -0.0953 23 0.990 0.000 C2 C1 C3 H2B 0.3282 0.7310 0.1712 23 0.990 0.000 C2 C1 C3 H3A 0.3226 0.6306 -0.1969 23 0.990 0.000 C3 C4 C2 H3B 0.2333 0.6370 0.0829 23 0.990 0.000 C3 C4 C2 H4A 0.1337 0.7202 -0.1174 23 0.990 0.000 C4 C5 C3 H4B 0.2265 0.7171 -0.3913 23 0.990 0.000 C4 C5 C3 H5 0.0199 0.7191 -0.5752 147 0.840 0.000 O5B C5 H5 H24 0.4160 0.5206 0.0593 43 0.950 0.000 C24 C25 N23 H25 0.2504 0.5476 0.4111 43 0.950 0.000 C25 C24 N21 H26A 0.0364 0.4386 0.5651 137 0.980 0.000 C26 N21 H26A H26B 0.0946 0.4925 0.7424 137 0.980 0.000 C26 N21 H26A H26C 0.1370 0.4271 0.8197 137 0.980 0.000 C26 N21 H26A H27A 0.3190 0.3271 0.2878 137 0.980 0.000 C27 C22 H27A H27B 0.1681 0.3406 0.2938 137 0.980 0.000 C27 C22 H27A H27C 0.2497 0.3427 0.5860 137 0.980 0.000 C27 C22 H27A H23 0.4195 0.4137 0.0438 43 0.880 0.000 N23 C22 C24 06skc0048pna21 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.47270 0.67329 0.26134 1.00000 0.02576 0.02303 0.03646 -0.00610 -0.00410 -0.00247 0.02841 0.01165 0.00056 0.00026 0.00176 0.00000 0.00307 0.00322 0.00405 0.00321 0.00336 0.00261 0.00155 C2 0.37555 0.70066 0.06249 1.00000 0.04268 0.02450 0.02902 0.00426 0.00133 0.00021 0.03206 0.01142 0.00065 0.00026 0.00156 0.00000 0.00376 0.00327 0.00428 0.00287 0.00353 0.00284 0.00175 H2A 0.42235 0.72053 -0.09534 1.00000 0.03848 0.00000 0.00000 H2B 0.32820 0.73102 0.17121 1.00000 0.03848 0.00000 0.00000 C3 0.27782 0.65901 -0.07126 1.00000 0.03473 0.02839 0.03571 0.00393 -0.00010 -0.00002 0.03294 0.01213 0.00060 0.00028 0.00185 0.00000 0.00323 0.00342 0.00425 0.00339 0.00386 0.00277 0.00164 H3A 0.32263 0.63059 -0.19691 1.00000 0.03953 0.00000 0.00000 H3B 0.23329 0.63700 0.08292 1.00000 0.03953 0.00000 0.00000 C4 0.18002 0.69312 -0.24736 1.00000 0.04166 0.02236 0.03701 -0.00269 0.00707 -0.00605 0.03368 0.01172 0.00063 0.00026 0.00181 0.00000 0.00337 0.00324 0.00438 0.00323 0.00362 0.00280 0.00168 H4A 0.13369 0.72019 -0.11735 1.00000 0.04041 0.00000 0.00000 H4B 0.22646 0.71706 -0.39135 1.00000 0.04041 0.00000 0.00000 C5 0.08242 0.65550 -0.40314 1.00000 0.02131 0.03447 0.03036 0.00064 0.00346 0.00699 0.02872 0.01183 0.00056 0.00029 0.00161 0.00000 0.00302 0.00370 0.00416 0.00360 0.00343 0.00283 0.00159 O1A 0.47762 0.61906 0.28283 1.00000 0.04563 0.01953 0.04340 0.00164 -0.00369 0.00261 0.03618 0.00804 0.00041 0.00018 0.00119 0.00000 0.00259 0.00222 0.00324 0.00225 0.00263 0.00185 0.00128 O1B 0.54376 0.70754 0.40593 1.00000 0.04373 0.02555 0.04245 -0.00090 -0.01152 0.00312 0.03724 0.00790 0.00042 0.00017 0.00118 0.00000 0.00248 0.00240 0.00317 0.00250 0.00284 0.00192 0.00128 O5A 0.07281 0.60345 -0.36840 1.00000 0.04970 0.01699 0.04801 -0.00112 -0.00537 0.00180 0.03823 0.00852 0.00045 0.00017 0.00129 0.00000 0.00263 0.00239 0.00339 0.00222 0.00275 0.00194 0.00131 O5B 0.00338 0.68318 -0.57789 1.00000 0.04547 0.02213 0.04331 -0.00191 -0.01074 0.00083 0.03697 0.00825 0.00042 0.00018 0.00132 0.00000 0.00251 0.00222 0.00320 0.00248 0.00279 0.00210 0.00124 H5 0.01993 0.71909 -0.57517 1.00000 0.05546 0.00000 0.00000 C22 0.27788 0.41253 0.33064 1.00000 0.02320 0.02523 0.03739 -0.00030 -0.01031 -0.00034 0.02861 0.01136 0.00057 0.00027 0.00166 0.00000 0.00284 0.00328 0.00457 0.00309 0.00361 0.00251 0.00168 C24 0.36353 0.49441 0.16591 1.00000 0.02267 0.02303 0.04623 -0.00335 -0.00248 0.00308 0.03064 0.01148 0.00055 0.00026 0.00185 0.00000 0.00284 0.00321 0.00459 0.00329 0.00366 0.00256 0.00164 H24 0.41600 0.52061 0.05928 1.00000 0.03677 0.00000 0.00000 C25 0.27329 0.50908 0.35551 1.00000 0.05655 0.01148 0.03389 0.00099 -0.00376 0.00314 0.03397 0.01142 0.00065 0.00025 0.00160 0.00000 0.00405 0.00293 0.00469 0.00287 0.00410 0.00279 0.00179 H25 0.25037 0.54765 0.41113 1.00000 0.04077 0.00000 0.00000 C26 0.11298 0.45368 0.66302 1.00000 0.04206 0.02624 0.03405 -0.00254 -0.00378 -0.00015 0.03412 0.01202 0.00060 0.00028 0.00176 0.00000 0.00370 0.00346 0.00460 0.00335 0.00403 0.00275 0.00178 H26A 0.03637 0.43864 0.56514 1.00000 0.05117 0.00000 0.00000 H26B 0.09456 0.49247 0.74241 1.00000 0.05117 0.00000 0.00000 H26C 0.13704 0.42712 0.81966 1.00000 0.05117 0.00000 0.00000 C27 0.25149 0.35065 0.37851 1.00000 0.04439 0.02351 0.04352 0.00150 0.00046 -0.00033 0.03714 0.01237 0.00062 0.00027 0.00190 0.00000 0.00398 0.00331 0.00497 0.00314 0.00415 0.00277 0.00181 H27A 0.31896 0.32711 0.28781 1.00000 0.05571 0.00000 0.00000 H27B 0.16808 0.34060 0.29383 1.00000 0.05571 0.00000 0.00000 H27C 0.24969 0.34269 0.58604 1.00000 0.05571 0.00000 0.00000 N21 0.21888 0.45790 0.45695 1.00000 0.03764 0.02473 0.03557 -0.00609 0.00039 0.00215 0.03264 0.00985 0.00052 0.00022 0.00141 0.00000 0.00283 0.00289 0.00374 0.00284 0.00317 0.00228 0.00144 N23 0.36709 0.43439 0.15221 1.00000 0.03975 0.02361 0.03354 -0.00853 -0.00016 0.00296 0.03230 0.00902 0.00050 0.00021 0.00136 0.00000 0.00300 0.00281 0.00371 0.00288 0.00320 0.00240 0.00144 H23 0.41948 0.41370 0.04382 1.00000 0.03876 0.00000 0.00000 Final Structure Factor Calculation for 06skc0048pna21 in Pna2(1) Total number of l.s. parameters = 148 Maximum vector length = 511 Memory required = 2079 / 25046 wR2 = 0.2225 before cycle 5 for 1362 data and 2 / 148 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1194 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0793 for 785 Fo > 4sig(Fo) and 0.1527 for all 1362 data wR2 = 0.2225, GooF = S = 1.037, Restrained GooF = 1.037 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 16.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0395 0.0272 0.0186 C1 0.0428 0.0314 0.0219 C2 0.0374 0.0347 0.0267 C3 0.0484 0.0320 0.0206 C4 0.0380 0.0305 0.0176 C5 0.0484 0.0410 0.0191 O1A 0.0549 0.0319 0.0249 O1B 0.0544 0.0434 0.0169 O5A 0.0553 0.0337 0.0220 O5B 0.0428 0.0253 0.0178 C22 0.0470 0.0251 0.0198 C24 0.0574 0.0334 0.0112 C25 0.0436 0.0334 0.0254 C26 0.0446 0.0434 0.0234 C27 0.0387 0.0376 0.0217 N21 0.0410 0.0375 0.0184 N23 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.024 0.031 0.037 0.048 0.059 0.075 0.098 0.139 1.000 Number in group 143. 141. 135. 126. 142. 131. 137. 135. 135. 137. GooF 0.890 1.050 1.050 1.013 1.079 1.038 1.021 1.097 0.981 1.137 K 4.346 2.165 1.427 1.223 1.041 1.061 0.976 1.027 1.016 1.001 Resolution(A) 0.77 0.81 0.84 0.88 0.93 0.99 1.07 1.18 1.37 1.73 inf Number in group 140. 133. 139. 133. 136. 137. 135. 137. 136. 136. GooF 0.841 0.923 0.982 0.981 0.999 0.981 1.069 0.988 1.098 1.413 K 1.225 1.199 1.312 1.145 1.121 0.985 1.001 0.977 1.026 1.001 R1 0.417 0.362 0.316 0.240 0.171 0.116 0.086 0.070 0.061 0.064 Recommended weighting scheme: WGHT 0.1211 0.0000 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 4 0 4182.32 9522.71 5.57 0.710 5.01 1 9 0 670.35 1500.92 5.24 0.282 2.47 7 5 0 65.03 142.30 4.92 0.087 1.41 2 0 0 34.47 7.36 4.92 0.020 5.20 6 3 3 74.41 15.30 4.82 0.028 1.14 3 6 1 336.86 672.34 4.66 0.189 2.25 6 3 0 297.90 502.79 3.40 0.163 1.69 9 18 0 211.63 59.45 3.36 0.056 0.86 6 6 0 84.84 46.17 3.28 0.049 1.58 3 6 3 158.69 91.61 3.22 0.070 1.32 2 9 1 208.83 348.33 3.10 0.136 2.05 2 4 1 32.90 15.26 3.04 0.028 2.96 11 3 1 215.98 107.13 2.99 0.075 0.92 9 3 2 82.42 39.80 2.98 0.046 1.03 9 8 0 20.63 2.94 2.96 0.012 1.07 1 4 3 46.59 14.62 2.96 0.028 1.48 2 26 1 156.03 27.68 2.73 0.038 0.85 1 3 0 34.32 20.16 2.72 0.033 6.15 4 7 0 17.17 0.56 2.71 0.005 2.04 9 6 0 19.26 3.42 2.71 0.013 1.11 4 9 0 203.77 129.36 2.64 0.083 1.82 3 19 0 38.35 9.78 2.60 0.023 1.14 6 2 0 299.16 435.14 2.59 0.152 1.71 6 1 2 37.18 58.13 2.51 0.055 1.39 6 24 1 86.06 5.50 2.48 0.017 0.82 2 6 0 211.73 151.47 2.46 0.090 3.08 4 25 2 -11.06 43.49 2.44 0.048 0.81 7 13 1 3.93 38.53 2.41 0.045 1.10 10 10 3 -90.22 52.43 2.38 0.053 0.81 6 4 4 110.40 64.96 2.37 0.059 0.95 5 11 4 -4.68 24.55 2.34 0.036 0.91 5 9 0 232.41 168.71 2.28 0.094 1.61 11 4 1 49.77 18.63 2.28 0.031 0.91 6 17 1 92.52 154.49 2.23 0.090 1.04 8 17 3 -4.53 59.82 2.23 0.056 0.80 8 16 0 228.91 149.73 2.22 0.089 0.96 11 2 2 13.30 75.51 2.19 0.063 0.87 2 11 5 -15.23 27.87 2.18 0.038 0.84 2 20 0 224.89 312.76 2.16 0.129 1.12 1 22 1 57.90 89.43 2.13 0.069 1.01 2 16 3 9.50 25.10 2.13 0.036 1.03 9 4 1 438.92 328.65 2.12 0.132 1.10 8 8 0 12.02 30.41 2.12 0.040 1.18 7 3 4 151.46 233.01 2.11 0.111 0.91 5 15 3 39.28 17.17 2.10 0.030 0.96 6 14 2 328.76 251.70 2.09 0.115 1.06 3 20 3 85.89 43.40 2.09 0.048 0.89 6 16 1 119.84 186.06 2.09 0.099 1.07 1 7 0 70.02 35.15 2.08 0.043 3.12 1 10 4 47.56 87.33 2.07 0.068 1.03 Bond lengths and angles C1 - Distance Angles O1A 1.2464 (0.0071) O1B 1.2692 (0.0077) 123.29 (0.64) C2 1.5051 (0.0097) 119.41 (0.58) 117.27 (0.51) C1 - O1A O1B C2 - Distance Angles C1 1.5051 (0.0097) C3 1.5258 (0.0092) 115.90 (0.53) H2A 0.9900 108.31 108.31 H2B 0.9900 108.31 108.31 107.41 C2 - C1 C3 H2A C3 - Distance Angles C4 1.5208 (0.0097) C2 1.5258 (0.0092) 110.10 (0.53) H3A 0.9900 109.64 109.64 H3B 0.9900 109.64 109.64 108.15 C3 - C4 C2 H3A C4 - Distance Angles C5 1.5149 (0.0093) C3 1.5208 (0.0098) 114.40 (0.53) H4A 0.9900 108.66 108.66 H4B 0.9900 108.66 108.66 107.60 C4 - C5 C3 H4A C5 - Distance Angles O5A 1.2064 (0.0076) O5B 1.3172 (0.0080) 120.35 (0.61) C4 1.5149 (0.0093) 123.58 (0.62) 116.03 (0.55) C5 - O5A O5B O1A - Distance Angles C1 1.2464 (0.0071) O1A - O1B - Distance Angles C1 1.2692 (0.0077) O1B - O5A - Distance Angles C5 1.2064 (0.0076) O5A - O5B - Distance Angles C5 1.3172 (0.0080) H5 0.8400 109.47 O5B - C5 C22 - Distance Angles N21 1.3413 (0.0085) N23 1.3407 (0.0090) 107.31 (0.55) C27 1.4596 (0.0084) 126.78 (0.65) 125.91 (0.61) C22 - N21 N23 C24 - Distance Angles C25 1.3297 (0.0097) N23 1.3757 (0.0076) 107.57 (0.59) H24 0.9500 126.22 126.22 C24 - C25 N23 C25 - Distance Angles C24 1.3297 (0.0097) N21 1.3836 (0.0084) 107.46 (0.54) H25 0.9500 126.27 126.27 C25 - C24 N21 C26 - Distance Angles N21 1.4620 (0.0089) 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 1.4596 (0.0084) 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 1.3413 (0.0085) C25 1.3836 (0.0084) 108.65 (0.58) C26 1.4620 (0.0089) 125.42 (0.57) 125.92 (0.54) N21 - C22 C25 N23 - Distance Angles C22 1.3407 (0.0090) C24 1.3757 (0.0076) 109.00 (0.55) H23 0.8800 125.50 125.50 N23 - C22 C24 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.70 2.538(6) 174.9 O5B-H5...O1B_$1 0.88 1.78 2.654(7) 170.8 N23-H23...O1A_$2 FMAP and GRID set by program FMAP 2 3 13 GRID -5.000 -2 24 5.000 2 1 R1 = 0.1527 for 1362 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.34 at 0.6155 0.4304 0.1075 [ 1.74 A from H25 ] Deepest hole -0.34 at 0.2354 0.6955 0.0069 [ 1.01 A from C3 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 2620 / 24643 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3845 0.5696 0.6075 1.00000 0.05 0.34 1.74 H25 1.78 H3A 2.10 H23 2.12 O1A Q2 1 0.3581 0.3350 0.4373 1.00000 0.05 0.34 0.82 H27A 1.20 C27 1.33 H27C 2.02 C22 Q3 1 0.2032 0.3085 0.7880 1.00000 0.05 0.34 1.31 H27C 1.88 H2B 2.19 C27 2.25 O5B Q4 1 0.1898 0.3500 0.4126 1.00000 0.05 0.32 0.63 H27B 0.66 C27 1.03 H27C 1.55 H27A Q5 1 0.1984 0.5501 0.4595 1.00000 0.05 0.32 0.59 H25 1.31 C25 1.96 O5A 2.12 N21 Q6 1 0.2948 0.7818 -0.5255 1.00000 0.05 0.31 1.76 H4B 1.86 H2B 2.04 H27B 2.14 H27A Q7 1 0.5932 0.6905 0.5430 1.00000 0.05 0.30 0.91 O1B 1.51 H27A 1.85 C1 2.27 H5 Q8 1 0.2107 0.5871 0.3156 1.00000 0.05 0.29 1.09 H25 1.59 H3B 1.91 C25 2.09 O5A Q9 1 0.0116 0.4978 0.6454 1.00000 0.05 0.28 0.98 H26B 1.43 H26A 1.46 C26 2.18 H26B Q10 1 0.3805 0.5602 0.3948 1.00000 0.05 0.27 1.39 H25 1.63 C25 1.76 O1A 1.84 H24 Shortest distances between peaks (including symmetry equivalents) 1 10 1.01 3 6 1.06 5 8 1.09 2 4 1.79 8 10 1.91 5 10 1.93 2 7 1.99 3 4 1.99 1 5 2.10 6 7 2.21 1 8 2.29 9 9 2.33 2 3 2.37 3 7 2.43 5 9 2.44 4 6 2.57 5 9 2.85 2 6 2.94 4 7 2.98 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. 0.33: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.38: Structure factors and derivatives 0.22: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.08: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0048pna21 finished at 14:38:07 Total CPU time: 1.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++