+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0007p21c started at 13:01:38 on 06-May-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0007p21c in P2(1)/c CELL 0.71073 11.5689 6.3068 16.6758 90.000 101.543 90.000 ZERR 2.00 0.0095 0.0054 0.0127 0.000 0.045 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 40 84 4 8 V = 1192.10 F(000) = 416.0 Mu = 0.07 mm-1 Cell Wt = 749.11 Rho = 1.043 MERG 2 OMIT -3.00 55.00 OMIT 2 0 0 SHEL 7 0.77 HTAB N25 O1B EQIV_$1 x, y+1, z HTAB N25 O1A_$1 EQIV_$2 -x, y+1/2, -z+3/2 HTAB N25 O1A_$2 EQIV_$3 -x, -y-1, -z+1 MPLA C1 O1A O1B MPLA C1_$3 O1A_$3 O1B_$3 FMAP 2 PLAN 10 CONF SIZE 0.01 0.10 0.17 ACTA BOND $H WGHT 0.07800 6.01800 L.S. 4 TEMP -153.00 FVAR 0.83003 C1 1 -0.013711 -0.321718 0.591244 11.00000 0.03192 0.07467 = 0.04764 0.00873 0.01755 0.00414 C2 1 0.003676 -0.397434 0.511008 11.00000 0.04117 0.07511 = 0.04346 0.00909 0.01396 -0.00028 AFIX 43 H2 2 0.020957 -0.296157 0.472906 11.00000 -1.20000 AFIX 0 O1A 4 -0.004483 -0.443184 0.650475 11.00000 0.08884 0.06823 = 0.05594 0.00827 0.03177 0.00158 O1B 4 -0.041400 -0.126407 0.594312 11.00000 0.06046 0.06855 = 0.05325 -0.00525 0.00878 0.00373 MOLE 2 C21 1 0.336568 0.152790 0.516506 11.00000 0.05380 0.11499 = 0.05456 0.00483 0.02443 -0.00061 AFIX 137 H21A 2 0.259721 0.115350 0.482932 11.00000 -1.50000 H21B 2 0.399460 0.089009 0.492921 11.00000 -1.50000 H21C 2 0.345604 0.307326 0.517883 11.00000 -1.50000 AFIX 0 C22 1 0.344169 0.070406 0.602701 11.00000 0.06184 0.08671 = 0.05524 -0.00143 0.02767 -0.00895 C23 1 0.229254 0.138892 0.627776 11.00000 0.05346 0.05861 = 0.04925 -0.00389 0.02048 -0.00450 AFIX 23 H23A 2 0.164842 0.059201 0.592392 11.00000 -1.20000 H23B 2 0.217252 0.290071 0.612367 11.00000 -1.20000 AFIX 0 C24 1 0.208438 0.119162 0.715880 11.00000 0.03471 0.06950 = 0.05373 -0.00236 0.00350 0.00316 C26 1 0.455964 0.154836 0.658292 11.00000 0.05367 0.09267 = 0.06551 0.00280 0.01188 -0.00282 AFIX 137 H26A 2 0.524595 0.120403 0.634536 11.00000 -1.50000 H26B 2 0.465011 0.089224 0.712464 11.00000 -1.50000 H26C 2 0.449970 0.309019 0.663523 11.00000 -1.50000 AFIX 0 C27 1 0.352270 -0.172575 0.597424 11.00000 0.06816 0.08733 = 0.06875 -0.01462 0.02053 0.00769 AFIX 137 H27A 2 0.275870 -0.229678 0.569775 11.00000 -1.50000 H27B 2 0.373334 -0.231968 0.652733 11.00000 -1.50000 H27C 2 0.412764 -0.210815 0.566405 11.00000 -1.50000 AFIX 0 C28 1 0.228771 -0.102486 0.754440 11.00000 0.05510 0.08522 = 0.06790 0.01763 0.01029 0.00458 AFIX 137 H28A 2 0.199116 -0.106016 0.805510 11.00000 -1.50000 H28B 2 0.313370 -0.134537 0.766034 11.00000 -1.50000 H28C 2 0.186792 -0.208229 0.716362 11.00000 -1.50000 AFIX 0 C29 1 0.268998 0.291614 0.773954 11.00000 0.08531 0.09997 = 0.05543 -0.01865 0.02424 -0.02243 AFIX 137 H29A 2 0.247855 0.431353 0.749711 11.00000 -1.50000 H29B 2 0.354727 0.272907 0.783032 11.00000 -1.50000 H29C 2 0.243209 0.281062 0.826325 11.00000 -1.50000 AFIX 0 N25 3 0.077705 0.157058 0.706171 11.00000 0.07021 0.05288 = 0.04240 -0.00295 0.02207 -0.00715 AFIX 137 H25A 2 0.060136 0.290715 0.686998 11.00000 0.07842 H25B 2 0.056426 0.141886 0.755522 11.00000 0.03989 H25C 2 0.037641 0.061448 0.670134 11.00000 0.05960 AFIX 0 HKLF 4 Covalent radii and connectivity table for 07skc0007p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C2_$3 C1 O1A - C1 O1B - C1 C21 - C22 C22 - C21 C26 C23 C27 C23 - C22 C24 C24 - N25 C29 C28 C23 C26 - C22 C27 - C22 C28 - C24 C29 - C24 N25 - C24 Operators for generating equivalent atoms: $1 x, y+1, z $2 -x, y+1/2, -z+3/2 $3 -x, -y-1, -z+1 h k l Fo^2 Sigma Why rejected 0 1 0 77.58 18.66 observed but should be systematically absent 0 1 0 125.42 17.62 observed but should be systematically absent 0 1 0 106.72 16.26 observed but should be systematically absent 0 1 0 123.02 19.96 observed but should be systematically absent -13 0 7 178.59 43.33 observed but should be systematically absent 9085 Reflections read, of which 671 rejected -15 =< h =< 15, -7 =< k =< 8, -21 =< l =< 21, Max. 2-theta = 54.95 5 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 1 2 416.00 7.51 5 557.93 1 2 3 329.98 10.21 5 314.56 4 3 4 45.34 3.59 3 35.34 5 5 4 8.18 2.54 2 47.01 6 5 4 4.00 2.12 3 23.98 4 3 5 -0.10 0.92 4 7.41 3 3 9 4.43 0.58 3 35.39 -1 6 11 8.96 4.18 3 22.75 -1 5 13 -1.67 4.11 3 23.66 -9 2 15 92.03 14.60 3 73.88 1 4 16 20.96 5.83 2 31.92 11 Inconsistent equivalents 2606 Unique reflections, of which 0 suppressed R(int) = 0.2200 R(sigma) = 0.3003 Friedel opposites merged Maximum memory for data reduction = 2034 / 26564 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 = 2440 / 161171 wR2 = 0.4237 before cycle 1 for 2606 data and 127 / 127 parameters GooF = S = 1.079; Restrained GooF = 1.079 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0780 * P )^2 + 6.02 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83006 0.00672 0.004 OSF Mean shift/esd = 0.001 Maximum = 0.004 for OSF Max. shift = 0.000 A for H29C Max. dU = 0.000 for H25C Least-squares cycle 2 Maximum vector length = 511 Memory required = 2440 / 161171 wR2 = 0.4237 before cycle 2 for 2606 data and 127 / 127 parameters GooF = S = 1.079; Restrained GooF = 1.079 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0780 * P )^2 + 6.02 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83006 0.00672 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U12 C29 Max. shift = 0.000 A for H27A Max. dU = 0.000 for H25C Least-squares cycle 3 Maximum vector length = 511 Memory required = 2440 / 161171 wR2 = 0.4237 before cycle 3 for 2606 data and 127 / 127 parameters GooF = S = 1.079; Restrained GooF = 1.079 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0780 * P )^2 + 6.02 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83006 0.00672 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U12 C29 Max. shift = 0.000 A for H27C Max. dU = 0.000 for H25C Least-squares cycle 4 Maximum vector length = 511 Memory required = 2440 / 161171 wR2 = 0.4237 before cycle 4 for 2606 data and 127 / 127 parameters GooF = S = 1.079; Restrained GooF = 1.079 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0780 * P )^2 + 6.02 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83006 0.00672 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U11 C1 Max. shift = 0.000 A for H27C Max. dU = 0.000 for H25C 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 0.0210 -0.2962 0.4729 43 0.950 0.000 C2 C2_$3 C1 H21A 0.2597 0.1153 0.4829 137 0.980 0.000 C21 C22 H21A H21B 0.3995 0.0890 0.4929 137 0.980 0.000 C21 C22 H21A H21C 0.3456 0.3073 0.5179 137 0.980 0.000 C21 C22 H21A H23A 0.1648 0.0592 0.5924 23 0.990 0.000 C23 C22 C24 H23B 0.2173 0.2901 0.6124 23 0.990 0.000 C23 C22 C24 H26A 0.5246 0.1204 0.6345 137 0.980 0.000 C26 C22 H26A H26B 0.4650 0.0892 0.7125 137 0.980 0.000 C26 C22 H26A H26C 0.4500 0.3090 0.6635 137 0.980 0.000 C26 C22 H26A H27A 0.2759 -0.2297 0.5698 137 0.980 0.000 C27 C22 H27A H27B 0.3733 -0.2320 0.6527 137 0.980 0.000 C27 C22 H27A H27C 0.4128 -0.2108 0.5664 137 0.980 0.000 C27 C22 H27A H28A 0.1991 -0.1060 0.8055 137 0.980 0.000 C28 C24 H28A H28B 0.3134 -0.1345 0.7660 137 0.980 0.000 C28 C24 H28A H28C 0.1868 -0.2082 0.7164 137 0.980 0.000 C28 C24 H28A H29A 0.2479 0.4314 0.7497 137 0.980 0.000 C29 C24 H29A H29B 0.3547 0.2729 0.7830 137 0.980 0.000 C29 C24 H29A H29C 0.2432 0.2811 0.8263 137 0.980 0.000 C29 C24 H29A H25A 0.0601 0.2907 0.6870 137 0.910 0.000 N25 C24 H25A H25B 0.0564 0.1419 0.7555 137 0.910 0.000 N25 C24 H25A H25C 0.0376 0.0615 0.6701 137 0.910 0.000 N25 C24 H25A 07skc0007p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.01371 -0.32172 0.59125 1.00000 0.03191 0.07468 0.04765 0.00873 0.01755 0.00415 0.05008 0.01905 0.00079 0.00201 0.00059 0.00000 0.00568 0.00882 0.00600 0.00655 0.00454 0.00585 0.00276 C2 0.00368 -0.39743 0.51101 1.00000 0.04118 0.07511 0.04346 0.00908 0.01396 -0.00028 0.05249 0.01702 0.00084 0.00152 0.00056 0.00000 0.00564 0.00772 0.00540 0.00641 0.00440 0.00650 0.00284 H2 0.02095 -0.29615 0.47290 1.00000 0.06298 0.00000 0.00000 O1A -0.00448 -0.44318 0.65048 1.00000 0.08885 0.06823 0.05595 0.00828 0.03178 0.00158 0.06861 0.01366 0.00065 0.00115 0.00042 0.00000 0.00596 0.00530 0.00418 0.00425 0.00393 0.00443 0.00229 O1B -0.04140 -0.12641 0.59431 1.00000 0.06046 0.06855 0.05325 -0.00525 0.00878 0.00374 0.06111 0.01233 0.00059 0.00126 0.00038 0.00000 0.00474 0.00541 0.00410 0.00404 0.00340 0.00423 0.00206 C21 0.33657 0.15279 0.51651 1.00000 0.05380 0.11501 0.05456 0.00484 0.02443 -0.00061 0.07257 0.02077 0.00093 0.00196 0.00057 0.00000 0.00685 0.01040 0.00617 0.00701 0.00517 0.00719 0.00351 H21A 0.25972 0.11534 0.48293 1.00000 0.10885 0.00000 0.00000 H21B 0.39946 0.08902 0.49292 1.00000 0.10885 0.00000 0.00000 H21C 0.34560 0.30733 0.51788 1.00000 0.10885 0.00000 0.00000 C22 0.34417 0.07041 0.60270 1.00000 0.06184 0.08672 0.05524 -0.00143 0.02767 -0.00895 0.06572 0.02127 0.00100 0.00196 0.00061 0.00000 0.00763 0.00947 0.00628 0.00662 0.00570 0.00666 0.00322 C23 0.22925 0.13889 0.62778 1.00000 0.05345 0.05862 0.04925 -0.00389 0.02048 -0.00450 0.05236 0.01783 0.00084 0.00159 0.00052 0.00000 0.00664 0.00690 0.00555 0.00544 0.00482 0.00566 0.00273 H23A 0.16484 0.05920 0.59239 1.00000 0.06283 0.00000 0.00000 H23B 0.21725 0.29007 0.61237 1.00000 0.06283 0.00000 0.00000 C24 0.20844 0.11916 0.71588 1.00000 0.03472 0.06951 0.05373 -0.00236 0.00350 0.00316 0.05340 0.01774 0.00082 0.00173 0.00056 0.00000 0.00582 0.00770 0.00574 0.00606 0.00463 0.00540 0.00275 C26 0.45596 0.15484 0.65829 1.00000 0.05366 0.09268 0.06551 0.00279 0.01189 -0.00283 0.07062 0.01979 0.00091 0.00187 0.00062 0.00000 0.00686 0.00936 0.00665 0.00666 0.00558 0.00675 0.00336 H26A 0.52459 0.12040 0.63454 1.00000 0.10593 0.00000 0.00000 H26B 0.46501 0.08923 0.71247 1.00000 0.10593 0.00000 0.00000 H26C 0.44997 0.30902 0.66352 1.00000 0.10593 0.00000 0.00000 C27 0.35227 -0.17258 0.59742 1.00000 0.06816 0.08734 0.06876 -0.01461 0.02053 0.00769 0.07380 0.02159 0.00101 0.00183 0.00068 0.00000 0.00787 0.00987 0.00706 0.00693 0.00596 0.00710 0.00349 H27A 0.27587 -0.22968 0.56978 1.00000 0.11070 0.00000 0.00000 H27B 0.37335 -0.23197 0.65273 1.00000 0.11070 0.00000 0.00000 H27C 0.41276 -0.21081 0.56640 1.00000 0.11070 0.00000 0.00000 C28 0.22877 -0.10249 0.75444 1.00000 0.05511 0.08523 0.06790 0.01763 0.01030 0.00459 0.06969 0.02055 0.00093 0.00178 0.00062 0.00000 0.00715 0.00875 0.00674 0.00679 0.00556 0.00651 0.00327 H28A 0.19912 -0.10602 0.80551 1.00000 0.10454 0.00000 0.00000 H28B 0.31337 -0.13454 0.76603 1.00000 0.10454 0.00000 0.00000 H28C 0.18679 -0.20823 0.71636 1.00000 0.10454 0.00000 0.00000 C29 0.26900 0.29162 0.77395 1.00000 0.08531 0.09998 0.05543 -0.01866 0.02425 -0.02246 0.07883 0.01962 0.00105 0.00192 0.00061 0.00000 0.00879 0.00933 0.00656 0.00697 0.00629 0.00779 0.00370 H29A 0.24786 0.43135 0.74970 1.00000 0.11824 0.00000 0.00000 H29B 0.35472 0.27290 0.78304 1.00000 0.11824 0.00000 0.00000 H29C 0.24320 0.28108 0.82632 1.00000 0.11824 0.00000 0.00000 N25 0.07770 0.15706 0.70617 1.00000 0.07022 0.05289 0.04240 -0.00296 0.02207 -0.00715 0.05367 0.01533 0.00070 0.00139 0.00046 0.00000 0.00637 0.00651 0.00469 0.00509 0.00438 0.00514 0.00240 H25A 0.06014 0.29072 0.68700 1.00000 0.07847 0.00000 0.04008 H25B 0.05642 0.14188 0.75552 1.00000 0.03986 0.00000 0.02435 H25C 0.03764 0.06146 0.67013 1.00000 0.05954 0.00000 0.03317 Final Structure Factor Calculation for 07skc0007p21c in P2(1)/c Total number of l.s. parameters = 127 Maximum vector length = 511 Memory required = 2313 / 22995 wR2 = 0.4237 before cycle 5 for 2606 data and 0 / 127 parameters GooF = S = 1.079; Restrained GooF = 1.079 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0780 * P )^2 + 6.02 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1926 for 788 Fo > 4sig(Fo) and 0.4101 for all 2606 data wR2 = 0.4237, GooF = S = 1.079, Restrained GooF = 1.079 for all data Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 21.00 for hydrogen atoms Principal mean square atomic displacements U 0.0777 0.0476 0.0250 C1 0.0775 0.0458 0.0341 C2 0.0941 0.0696 0.0421 O1A 0.0727 0.0591 0.0516 O1B 0.1154 0.0653 0.0370 C21 0.0902 0.0693 0.0377 C22 0.0648 0.0539 0.0384 C23 0.0706 0.0557 0.0340 C24 0.0933 0.0653 0.0533 C26 0.0967 0.0735 0.0512 C27 0.0962 0.0599 0.0530 C28 0.1200 0.0693 0.0472 C29 0.0746 0.0504 0.0359 N25 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.005 0.009 0.013 0.018 0.024 0.033 0.044 0.065 0.100 1.000 Number in group 311. 257. 231. 271. 236. 288. 241. 251. 264. 256. GooF 1.097 1.153 1.117 1.037 1.045 1.148 1.082 1.095 0.967 1.027 K 170.950 25.823 9.781 3.381 3.222 2.082 1.457 1.192 0.970 1.033 Resolution(A) 0.77 0.81 0.84 0.88 0.92 0.98 1.05 1.17 1.34 1.67 inf Number in group 271. 252. 260. 260. 263. 264. 256. 259. 261. 260. GooF 1.085 1.055 1.172 1.145 1.179 1.057 1.036 0.987 0.931 1.111 K 5.524 2.912 4.062 2.726 2.258 1.331 1.216 1.053 1.014 1.032 R1 0.771 0.704 0.705 0.621 0.569 0.456 0.323 0.276 0.164 0.096 Recommended weighting scheme: WGHT 0.0782 5.9951 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) -6 2 15 195.34 14.40 4.12 0.033 0.99 0 5 12 258.14 31.12 3.75 0.049 0.93 -5 2 4 14.31 108.52 3.45 0.092 1.79 1 5 12 195.89 26.29 3.38 0.045 0.91 6 2 15 109.83 10.93 3.35 0.029 0.84 1 2 15 111.93 26.60 3.26 0.046 1.01 -13 1 4 126.65 0.68 3.24 0.007 0.88 -5 7 1 121.55 10.02 3.20 0.028 0.84 10 0 2 111.79 1.66 3.20 0.011 1.09 4 5 6 169.51 46.39 3.02 0.060 1.03 11 1 3 113.20 2.25 3.01 0.013 0.97 -5 1 2 105.04 32.19 2.99 0.050 2.17 11 3 0 78.66 0.04 2.97 0.002 0.93 3 3 1 51.12 1.34 2.95 0.010 1.81 -4 4 15 155.19 41.14 2.90 0.057 0.90 -2 0 18 92.68 4.50 2.87 0.019 0.93 -1 3 16 47.77 0.01 2.82 0.001 0.93 6 6 0 85.40 6.68 2.81 0.023 0.92 -5 6 7 158.85 0.81 2.79 0.008 0.91 1 0 6 71.34 6.49 2.79 0.022 2.54 5 1 5 45.49 1.17 2.75 0.010 1.65 -10 5 5 123.00 0.06 2.71 0.002 0.85 -1 3 1 266.27 133.02 2.70 0.102 2.06 -10 2 3 74.19 1.18 2.69 0.010 1.09 -6 6 2 58.40 1.87 2.68 0.012 0.92 -3 4 16 100.07 0.01 2.66 0.001 0.87 -13 1 8 99.41 8.40 2.66 0.026 0.86 -6 3 15 75.97 2.83 2.64 0.015 0.93 8 1 9 89.39 3.85 2.64 0.017 1.01 -1 4 1 83.55 23.23 2.59 0.043 1.56 3 2 18 111.02 0.06 2.59 0.002 0.82 -15 0 4 122.49 5.67 2.57 0.021 0.77 1 4 18 69.25 0.08 2.56 0.003 0.78 -7 5 12 154.51 20.61 2.53 0.040 0.86 10 3 2 63.11 0.49 2.53 0.006 0.97 1 3 16 76.90 11.39 2.51 0.030 0.90 -6 5 13 126.41 5.12 2.51 0.020 0.85 9 4 5 230.71 11.59 2.48 0.030 0.90 -13 2 3 75.03 0.35 2.47 0.005 0.86 -5 0 4 4850.61 3795.02 2.47 0.544 2.18 -6 7 6 92.70 0.04 2.47 0.002 0.80 -10 2 12 191.73 11.44 2.46 0.030 0.93 12 3 1 106.63 0.68 2.44 0.007 0.85 -10 3 9 95.21 0.52 2.44 0.006 0.95 -2 4 18 159.77 0.30 2.44 0.005 0.80 10 4 1 82.88 0.95 2.43 0.009 0.91 2 2 2 -8.02 28.80 2.40 0.047 2.54 -11 3 15 80.94 0.27 2.40 0.005 0.78 -14 0 4 110.77 0.88 2.39 0.008 0.83 0 5 14 214.64 13.44 2.39 0.032 0.86 Bond lengths and angles C1 - Distance Angles O1A 1.2376 (0.0107) O1B 1.2764 (0.0116) 123.21 (0.93) C2 1.4719 (0.0130) 121.27 (1.06) 115.50 (0.93) C1 - O1A O1B C2 - Distance Angles C2_$3 1.3429 (0.0187) C1 1.4719 (0.0130) 123.25 (1.19) H2 0.9500 118.37 118.37 C2 - C2_$3 C1 O1A - Distance Angles C1 1.2376 (0.0107) O1A - O1B - Distance Angles C1 1.2764 (0.0116) O1B - C21 - Distance Angles C22 1.5143 (0.0133) 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 C21 1.5143 (0.0133) C26 1.5283 (0.0144) 109.73 (0.90) C23 1.5334 (0.0134) 105.86 (0.90) 114.27 (0.85) C27 1.5389 (0.0149) 106.26 (0.93) 109.14 (0.99) 111.23 (0.91) C22 - C21 C26 C23 C23 - Distance Angles C22 1.5334 (0.0134) C24 1.5407 (0.0121) 123.15 (0.83) H23A 0.9900 106.54 106.54 H23B 0.9900 106.54 106.54 106.53 C23 - C22 C24 H23A C24 - Distance Angles N25 1.5076 (0.0115) C29 1.5297 (0.0135) 106.13 (0.83) C28 1.5370 (0.0138) 104.80 (0.81) 111.68 (0.82) C23 1.5407 (0.0121) 103.28 (0.72) 114.02 (0.86) 115.62 (0.85) C24 - N25 C29 C28 C26 - Distance Angles C22 1.5283 (0.0144) 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 C27 - Distance Angles C22 1.5389 (0.0149) 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 C28 - Distance Angles C24 1.5370 (0.0138) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C24 H28A H28B C29 - Distance Angles C24 1.5297 (0.0135) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 - C24 H29A H29B N25 - Distance Angles C24 1.5076 (0.0116) H25A 0.9100 109.47 H25B 0.9100 109.47 109.47 H25C 0.9100 109.47 109.47 109.47 N25 - C24 H25A H25B Selected torsion angles 19.88 ( 1.77) O1A - C1 - C2 - C2_$3 -158.44 ( 1.18) O1B - C1 - C2 - C2_$3 -169.92 ( 0.94) C21 - C22 - C23 - C24 -49.05 ( 1.37) C26 - C22 - C23 - C24 75.08 ( 1.23) C27 - C22 - C23 - C24 -167.54 ( 0.92) C22 - C23 - C24 - N25 77.78 ( 1.25) C22 - C23 - C24 - C29 -53.70 ( 1.31) C22 - C23 - C24 - C28 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.84 2.747(11) 177.9 N25-H25C...O1B 0.91 1.89 2.787(12) 169.4 N25-H25A...O1A_$1 0.91 1.87 2.764(10) 168.7 N25-H25B...O1A_$2 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 10.7705 (0.0735) x + 1.5048 (0.0477) y + 1.4078 (0.2771) z = 0.2006 (0.1610) * 0.0000 (0.0001) C1 * 0.0000 (0.0001) O1A * 0.0000 (0.0000) O1B Rms deviation of fitted atoms = 0.0000 - 10.7705 (0.0731) x - 1.5048 (0.0477) y - 1.4078 (0.2773) z = 0.2975 (0.0820) Angle to previous plane (with approximate esd) = 0.00 ( 1.54 ) * 0.0000 (0.0000) C1_$3 * 0.0000 (0.0000) O1A_$3 * 0.0000 (0.0000) O1B_$3 Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 2 11 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.4099 for 2606 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.35 at 0.0035 0.1294 0.5151 [ 1.12 A from H2 ] Deepest hole -0.25 at 0.8672 0.1556 0.4412 [ 1.48 A from H23A ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2732 / 19441 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0035 -0.1294 0.4849 1.00000 0.05 0.35 1.12 H2 1.74 C2 1.96 O1B 2.09 H23A Q2 1 0.3829 0.4777 0.5953 1.00000 0.05 0.28 1.64 H26C 1.67 H21C 2.07 H27C 2.08 H27B Q3 1 0.2188 0.4344 0.7376 1.00000 0.05 0.27 0.36 H29A 1.17 C29 1.74 H29C 1.90 H29B Q4 1 0.4467 -0.4280 0.6761 1.00000 0.05 0.26 1.51 H27B 1.67 H26C 1.94 H26B 2.22 C27 Q5 1 -0.0197 0.1437 0.6605 1.00000 0.05 0.26 0.83 H25C 1.23 N25 1.32 H25A 1.65 H25B Q6 1 -0.0205 -0.5692 0.5989 1.00000 0.05 0.25 1.16 O1A 1.47 H2 1.57 C1 1.81 H25A Q7 1 -0.0015 0.0870 0.5981 1.00000 0.05 0.25 1.21 H25C 1.42 O1B 1.76 H2 1.90 N25 Q8 1 0.2184 0.5611 0.6344 1.00000 0.05 0.25 1.75 H23B 1.91 H27A 2.05 H29A 2.08 H28C Q9 1 0.3433 -0.4462 0.5994 1.00000 0.05 0.24 1.60 H27A 1.62 H27B 1.73 C27 1.82 H27C Q10 1 -0.0423 -0.2500 0.6542 1.00000 0.05 0.22 1.25 C1 1.27 O1B 1.30 O1A 1.69 H25B Shortest distances between peaks (including symmetry equivalents) 2 9 0.68 5 7 1.16 1 7 1.42 2 4 1.52 4 9 1.57 8 9 1.66 1 1 1.70 3 8 1.90 5 6 2.08 6 7 2.18 2 8 2.20 6 10 2.25 1 7 2.32 7 10 2.41 1 6 2.41 1 5 2.49 5 10 2.50 4 8 2.59 6 8 2.83 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 0.00: 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. 0.41: 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 0.44: Structure factors and derivatives 0.34: 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 0.03: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0007p21c finished at 13:01:40 Total CPU time: 1.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++