+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0068p21c started at 11:33:01 on 13-Jun-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0068p21c in P2(1)/c CELL 0.71073 8.3220 11.2030 11.9150 90.000 97.786 90.000 ZERR 4.00 0.0038 0.0053 0.0052 0.000 0.034 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 32 56 16 24 V = 1100.61 F(000) = 552.0 Mu = 0.14 mm-1 Cell Wt = 1048.93 Rho = 1.583 MERG 2 OMIT -3.00 50.00 SHEL 7 0.84 EQIV_$1 -x, -y, -z+1 HTAB O1B O22_$1 HTAB N23 O1A_$1 EQIV_$2 x, -y-1/2, z+1/2 HTAB O2A O32_$2 HTAB N21 O1A_$2 EQIV_$3 -x-1, -y, -z+1 HTAB N31 O2B_$3 EQIV_$4 x, -y-1/2, z-1/2 HTAB N33 O2B_$4 EADP C24 C25 EADP C1 C2 FMAP 2 PLAN 10 SIZE 0.01 0.08 0.10 ACTA BOND $H WGHT 0.00000 9.02670 L.S. 4 TEMP -153.00 FVAR 0.27487 MOLE 1 C1 1 -0.202596 -0.112955 0.468660 11.00000 0.01259 0.02253 = 0.01898 -0.00652 -0.00378 0.00109 C2 1 -0.293749 -0.153400 0.564357 11.00000 0.01259 0.02253 = 0.01898 -0.00652 -0.00378 0.00109 O1A 4 -0.141259 -0.185244 0.410540 11.00000 0.02693 0.01888 = 0.02375 -0.00394 0.01316 0.00383 O1B 4 -0.200309 0.002199 0.457043 11.00000 0.02123 0.01443 = 0.02859 -0.00081 0.01579 -0.00106 AFIX 147 H1 2 -0.143781 0.020209 0.406238 11.00000 -1.50000 AFIX 0 O2A 4 -0.294529 -0.268307 0.577505 11.00000 0.02233 0.01766 = 0.02282 -0.00080 0.00391 -0.00993 AFIX 147 H2 2 -0.341447 -0.285444 0.633534 11.00000 -1.50000 AFIX 0 O2B 4 -0.359258 -0.084022 0.619893 11.00000 0.02326 0.02162 = 0.02140 -0.00389 0.01065 -0.00274 MOLE 2 C22 1 -0.025334 -0.024221 0.759586 11.00000 0.02146 0.02531 = 0.02540 0.00578 0.00030 -0.00039 C24 1 -0.098066 0.135417 0.861716 11.00000 0.02110 0.01350 = 0.02490 -0.00370 0.00168 0.00323 AFIX 23 H24A 2 -0.175801 0.201841 0.843902 11.00000 -1.20000 H24B 2 -0.009371 0.161525 0.920447 11.00000 -1.20000 AFIX 0 C25 1 -0.182816 0.022037 0.898328 11.00000 0.02110 0.01350 = 0.02490 -0.00370 0.00168 0.00323 AFIX 23 H25A 2 -0.170146 0.013857 0.981793 11.00000 -1.20000 H25B 2 -0.299550 0.020975 0.867861 11.00000 -1.20000 AFIX 0 N21 3 -0.093212 -0.069858 0.846515 11.00000 0.02486 0.02035 = 0.02181 0.00790 0.00767 0.00739 AFIX 43 H21 2 -0.084656 -0.144716 0.868906 11.00000 -1.20000 AFIX 0 N23 3 -0.035713 0.091838 0.760329 11.00000 0.04195 0.01941 = 0.02074 0.00370 0.00994 -0.00005 AFIX 43 H23 2 -0.008514 0.138289 0.706396 11.00000 -1.20000 AFIX 0 O22 4 0.039527 -0.088376 0.689991 11.00000 0.03388 0.01980 = 0.01712 -0.00355 0.00903 0.00643 MOLE 3 C32 1 -0.520472 -0.210802 0.290724 11.00000 0.00923 0.01695 = 0.02433 -0.00987 -0.00269 0.00436 C34 1 -0.609788 -0.373254 0.382998 11.00000 0.01819 0.03295 = 0.02079 -0.00130 0.00568 0.00520 AFIX 23 H34A 2 -0.525101 -0.412089 0.437228 11.00000 -1.20000 H34B 2 -0.699469 -0.430349 0.361458 11.00000 -1.20000 AFIX 0 C35 1 -0.670361 -0.259135 0.431521 11.00000 0.02117 0.02875 = 0.02601 0.00257 0.00518 0.00086 AFIX 23 H35A 2 -0.788941 -0.250033 0.410458 11.00000 -1.20000 H35B 2 -0.644348 -0.257365 0.515080 11.00000 -1.20000 AFIX 0 N31 3 -0.582748 -0.167430 0.379638 11.00000 0.02300 0.01426 = 0.02220 -0.00044 0.00527 0.00117 AFIX 43 H31 2 -0.572027 -0.093156 0.403514 11.00000 -1.20000 AFIX 0 N33 3 -0.544436 -0.329313 0.285146 11.00000 0.02435 0.01978 = 0.01853 -0.00727 0.00621 -0.00479 AFIX 43 H33 2 -0.522842 -0.374486 0.228644 11.00000 -1.20000 AFIX 0 O32 4 -0.455172 -0.150954 0.221006 11.00000 0.02491 0.02085 = 0.02101 0.00347 -0.00008 -0.00134 HKLF 4 Covalent radii and connectivity table for 06skc0068p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - O2B O2A C1 O1A - C1 O1B - C1 O2A - C2 O2B - C2 C22 - O22 N23 N21 C24 - N23 C25 C25 - N21 C24 N21 - C22 C25 N23 - C22 C24 O22 - C22 C32 - O32 N31 N33 C34 - N33 C35 C35 - N31 C34 N31 - C32 C35 N33 - C32 C34 O32 - C32 Operators for generating equivalent atoms: $1 -x, -y, -z+1 $2 x, -y-1/2, z+1/2 $3 -x-1, -y, -z+1 $4 x, -y-1/2, z-1/2 h k l Fo^2 Sigma Why rejected 8 0 3 23.29 5.37 observed but should be systematically absent 19764 Reflections read, of which 3810 rejected -9 =< h =< 9, -13 =< k =< 13, -14 =< l =< 14, Max. 2-theta = 50.00 1 Systematic absence violations 0 Inconsistent equivalents 1934 Unique reflections, of which 0 suppressed R(int) = 0.1842 R(sigma) = 0.1022 Friedel opposites merged Maximum memory for data reduction = 1965 / 19243 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 = 2418 / 191448 wR2 = 0.2344 before cycle 1 for 1934 data and 153 / 153 parameters GooF = S = 1.243; Restrained GooF = 1.243 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 9.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27487 0.00135 -0.001 OSF Mean shift/esd = 0.003 Maximum = 0.011 for U11 N33 Max. shift = 0.000 A for H2 Max. dU = 0.000 for N33 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2418 / 191448 wR2 = 0.2344 before cycle 2 for 1934 data and 153 / 153 parameters GooF = S = 1.243; Restrained GooF = 1.243 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 9.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27487 0.00135 0.003 OSF Mean shift/esd = 0.002 Maximum = 0.009 for U11 O32 Max. shift = 0.000 A for H2 Max. dU = 0.000 for N33 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2418 / 191448 wR2 = 0.2344 before cycle 3 for 1934 data and 153 / 153 parameters GooF = S = 1.243; Restrained GooF = 1.243 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 9.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27487 0.00135 0.001 OSF Mean shift/esd = 0.001 Maximum = -0.005 for U11 O1B Max. shift = 0.000 A for H2 Max. dU = 0.000 for N33 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2418 / 191448 wR2 = 0.2343 before cycle 4 for 1934 data and 153 / 153 parameters GooF = S = 1.243; Restrained GooF = 1.243 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 9.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27487 0.00135 0.001 OSF Mean shift/esd = 0.001 Maximum = -0.003 for U11 O1B Max. shift = 0.000 A for H2 Max. dU = 0.000 for N33 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 H1 -0.1438 0.0202 0.4062 147 0.840 0.000 O1B C1 H1 H2 -0.3415 -0.2854 0.6335 147 0.840 0.000 O2A C2 H2 H24A -0.1758 0.2018 0.8439 23 0.990 0.000 C24 N23 C25 H24B -0.0094 0.1615 0.9204 23 0.990 0.000 C24 N23 C25 H25A -0.1701 0.0139 0.9818 23 0.990 0.000 C25 N21 C24 H25B -0.2995 0.0210 0.8679 23 0.990 0.000 C25 N21 C24 H21 -0.0847 -0.1447 0.8689 43 0.880 0.000 N21 C22 C25 H23 -0.0085 0.1383 0.7064 43 0.880 0.000 N23 C22 C24 H34A -0.5251 -0.4121 0.4372 23 0.990 0.000 C34 N33 C35 H34B -0.6995 -0.4304 0.3615 23 0.990 0.000 C34 N33 C35 H35A -0.7889 -0.2500 0.4105 23 0.990 0.000 C35 N31 C34 H35B -0.6443 -0.2574 0.5151 23 0.990 0.000 C35 N31 C34 H31 -0.5720 -0.0932 0.4035 43 0.880 0.000 N31 C32 C35 H33 -0.5229 -0.3745 0.2286 43 0.880 0.000 N33 C32 C34 06skc0068p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.20260 -0.11296 0.46866 1.00000 0.01259 0.02255 0.01900 -0.00652 -0.00377 0.00109 0.01859 0.01328 0.00089 0.00072 0.00063 0.00000 0.00279 0.00326 0.00288 0.00255 0.00227 0.00244 0.00124 C2 -0.29376 -0.15340 0.56435 1.00000 0.01259 0.02255 0.01900 -0.00652 -0.00377 0.00109 0.01859 0.01325 0.00088 0.00072 0.00063 0.00000 0.00279 0.00326 0.00288 0.00255 0.00227 0.00244 0.00124 O1A -0.14125 -0.18524 0.41054 1.00000 0.02696 0.01889 0.02377 -0.00395 0.01319 0.00386 0.02231 0.00977 0.00063 0.00047 0.00044 0.00000 0.00311 0.00300 0.00294 0.00244 0.00246 0.00257 0.00130 O1B -0.20032 0.00220 0.45705 1.00000 0.02116 0.01444 0.02863 -0.00080 0.01578 -0.00102 0.02026 0.00997 0.00064 0.00047 0.00045 0.00000 0.00319 0.00303 0.00322 0.00234 0.00250 0.00242 0.00131 H1 -0.14378 0.02021 0.40625 1.00000 0.03040 0.00000 0.00000 O2A -0.29452 -0.26831 0.57751 1.00000 0.02236 0.01768 0.02282 -0.00079 0.00395 -0.00993 0.02087 0.00933 0.00066 0.00045 0.00044 0.00000 0.00319 0.00315 0.00302 0.00248 0.00244 0.00248 0.00131 H2 -0.34150 -0.28545 0.63351 1.00000 0.03131 0.00000 0.00000 O2B -0.35925 -0.08402 0.61990 1.00000 0.02321 0.02161 0.02144 -0.00390 0.01062 -0.00276 0.02139 0.00937 0.00063 0.00048 0.00042 0.00000 0.00310 0.00322 0.00296 0.00247 0.00252 0.00251 0.00134 C22 -0.02535 -0.02421 0.75958 1.00000 0.02140 0.02536 0.02539 0.00579 0.00032 -0.00040 0.02431 0.01557 0.00098 0.00078 0.00070 0.00000 0.00478 0.00518 0.00451 0.00389 0.00376 0.00387 0.00197 C24 -0.09805 0.13541 0.86172 1.00000 0.02104 0.01353 0.02490 -0.00371 0.00170 0.00317 0.01995 0.01388 0.00094 0.00068 0.00063 0.00000 0.00319 0.00309 0.00310 0.00252 0.00251 0.00260 0.00133 H24A -0.17579 0.20184 0.84391 1.00000 0.02395 0.00000 0.00000 H24B -0.00935 0.16151 0.92045 1.00000 0.02395 0.00000 0.00000 C25 -0.18280 0.02203 0.89833 1.00000 0.02104 0.01353 0.02490 -0.00371 0.00170 0.00317 0.01995 0.01408 0.00095 0.00065 0.00066 0.00000 0.00319 0.00309 0.00310 0.00252 0.00251 0.00260 0.00133 H25A -0.17012 0.01385 0.98180 1.00000 0.02395 0.00000 0.00000 H25B -0.29953 0.02097 0.86787 1.00000 0.02395 0.00000 0.00000 N21 -0.09321 -0.06987 0.84651 1.00000 0.02491 0.02029 0.02181 0.00788 0.00765 0.00738 0.02193 0.01182 0.00076 0.00059 0.00051 0.00000 0.00390 0.00398 0.00373 0.00309 0.00307 0.00320 0.00162 H21 -0.08465 -0.14473 0.86890 1.00000 0.02631 0.00000 0.00000 N23 -0.03572 0.09184 0.76033 1.00000 0.04196 0.01936 0.02077 0.00371 0.00991 -0.00004 0.02684 0.01256 0.00084 0.00062 0.00056 0.00000 0.00476 0.00414 0.00362 0.00304 0.00332 0.00336 0.00175 H23 -0.00852 0.13830 0.70639 1.00000 0.03221 0.00000 0.00000 O22 0.03953 -0.08838 0.68999 1.00000 0.03388 0.01981 0.01713 -0.00354 0.00905 0.00644 0.02309 0.00977 0.00068 0.00048 0.00043 0.00000 0.00338 0.00326 0.00286 0.00250 0.00253 0.00265 0.00136 C32 -0.52047 -0.21080 0.29073 1.00000 0.00914 0.01695 0.02432 -0.00987 -0.00268 0.00434 0.01726 0.01313 0.00085 0.00070 0.00064 0.00000 0.00404 0.00470 0.00454 0.00353 0.00356 0.00338 0.00186 C34 -0.60979 -0.37326 0.38300 1.00000 0.01818 0.03288 0.02082 -0.00130 0.00567 0.00518 0.02368 0.01509 0.00096 0.00076 0.00065 0.00000 0.00448 0.00527 0.00430 0.00386 0.00351 0.00391 0.00196 H34A -0.52510 -0.41209 0.43723 1.00000 0.02842 0.00000 0.00000 H34B -0.69947 -0.43035 0.36146 1.00000 0.02842 0.00000 0.00000 C35 -0.67036 -0.25914 0.43152 1.00000 0.02126 0.02872 0.02600 0.00254 0.00521 0.00084 0.02514 0.01541 0.00101 0.00073 0.00069 0.00000 0.00470 0.00504 0.00451 0.00401 0.00381 0.00389 0.00200 H35A -0.78894 -0.25004 0.41046 1.00000 0.03017 0.00000 0.00000 H35B -0.64434 -0.25737 0.51508 1.00000 0.03017 0.00000 0.00000 N31 -0.58276 -0.16743 0.37964 1.00000 0.02309 0.01423 0.02216 -0.00046 0.00527 0.00118 0.01962 0.01156 0.00075 0.00057 0.00051 0.00000 0.00366 0.00369 0.00353 0.00293 0.00292 0.00296 0.00152 H31 -0.57205 -0.09316 0.40352 1.00000 0.02355 0.00000 0.00000 N33 -0.54444 -0.32931 0.28514 1.00000 0.02445 0.01983 0.01851 -0.00727 0.00620 -0.00478 0.02063 0.01128 0.00075 0.00059 0.00051 0.00000 0.00380 0.00401 0.00364 0.00288 0.00295 0.00300 0.00159 H33 -0.52285 -0.37448 0.22864 1.00000 0.02475 0.00000 0.00000 O32 -0.45516 -0.15095 0.22100 1.00000 0.02499 0.02085 0.02099 0.00347 -0.00009 -0.00134 0.02257 0.00965 0.00064 0.00050 0.00043 0.00000 0.00313 0.00338 0.00302 0.00246 0.00251 0.00254 0.00135 Final Structure Factor Calculation for 06skc0068p21c in P2(1)/c Total number of l.s. parameters = 153 Maximum vector length = 511 Memory required = 2265 / 22995 wR2 = 0.2343 before cycle 5 for 1934 data and 0 / 153 parameters GooF = S = 1.243; Restrained GooF = 1.243 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 9.03 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1421 for 1265 Fo > 4sig(Fo) and 0.2012 for all 1934 data wR2 = 0.2343, GooF = S = 1.243, Restrained GooF = 1.243 for all data Occupancy sum of asymmetric unit = 18.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0296 0.0168 0.0093 C1 0.0296 0.0168 0.0093 C2 0.0341 0.0228 0.0100 O1A 0.0364 0.0144 0.0100 O1B 0.0302 0.0226 0.0097 O2A 0.0311 0.0198 0.0133 O2B 0.0321 0.0220 0.0188 C22 0.0274 0.0211 0.0114 C24 0.0274 0.0211 0.0114 C25 0.0346 0.0184 0.0128 N21 0.0427 0.0226 0.0152 N23 0.0367 0.0221 0.0105 O22 0.0340 0.0106 0.0071 C32 0.0346 0.0223 0.0142 C34 0.0304 0.0248 0.0202 C35 0.0246 0.0203 0.0140 N31 0.0305 0.0195 0.0119 N33 0.0286 0.0217 0.0174 O32 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.004 0.009 0.013 0.018 0.023 0.030 0.037 0.050 0.072 1.000 Number in group 194. 228. 180. 213. 166. 205. 172. 193. 188. 195. GooF 1.632 1.545 1.357 1.375 1.187 1.117 1.019 0.945 0.927 0.990 K 61.613 8.297 3.066 1.810 1.418 1.183 1.047 1.052 1.001 0.996 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.25 1.44 1.81 inf Number in group 195. 198. 191. 196. 189. 193. 193. 191. 195. 193. GooF 1.421 1.311 1.192 1.288 1.243 1.229 1.232 1.156 1.156 1.173 K 1.521 1.264 1.265 1.099 1.116 1.087 1.047 1.071 1.037 1.004 R1 0.443 0.375 0.333 0.255 0.238 0.173 0.162 0.158 0.088 0.064 Recommended weighting scheme: WGHT 0.0000 9.0244 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) -9 4 5 334.50 4.77 3.87 0.006 0.85 0 13 1 321.50 0.54 3.69 0.002 0.86 -8 7 5 222.76 3.01 3.39 0.005 0.85 -8 6 6 266.95 2.78 3.28 0.005 0.86 -6 1 6 184.63 19.39 3.12 0.012 1.20 3 12 2 184.34 1.08 3.08 0.003 0.87 -5 7 7 159.77 1.41 2.99 0.003 0.99 -6 1 1 73.09 0.25 2.92 0.001 1.38 7 8 0 252.09 68.02 2.82 0.023 0.90 -5 6 4 115.25 5.39 2.80 0.007 1.18 -3 3 10 155.89 0.23 2.78 0.001 1.09 4 8 8 185.91 5.66 2.77 0.007 0.88 -1 8 1 257.91 109.37 2.69 0.030 1.37 2 1 1 217.49 98.90 2.69 0.028 3.55 -8 1 2 93.15 2.63 2.68 0.005 1.03 -7 8 4 161.48 5.18 2.65 0.006 0.89 -3 4 1 169.11 59.97 2.61 0.022 1.97 -1 3 5 466.28 280.69 2.60 0.047 1.99 3 4 0 151.61 53.72 2.60 0.021 1.96 4 5 7 320.18 142.81 2.57 0.034 1.08 -6 4 4 158.66 54.23 2.57 0.021 1.19 -1 6 5 129.86 37.34 2.56 0.017 1.46 3 3 2 127.33 38.86 2.56 0.018 2.00 -1 3 12 115.42 0.58 2.55 0.002 0.96 -8 3 1 106.25 0.05 2.53 0.001 1.00 -5 5 9 189.50 22.11 2.53 0.013 0.99 1 7 1 70.19 0.01 2.53 0.000 1.55 -3 5 5 64.03 0.39 2.51 0.002 1.46 -6 7 9 189.79 30.85 2.51 0.016 0.86 9 2 2 479.91 249.49 2.49 0.045 0.88 5 3 7 112.27 19.45 2.48 0.012 1.06 8 5 3 152.62 1.49 2.46 0.003 0.89 5 1 3 67.95 10.02 2.40 0.009 1.44 5 8 6 151.56 0.35 2.38 0.002 0.91 0 1 11 195.52 81.13 2.38 0.025 1.07 1 5 2 100.55 23.63 2.38 0.014 2.01 2 9 9 140.86 8.27 2.36 0.008 0.87 -7 4 1 102.01 1.77 2.34 0.004 1.09 9 2 1 136.99 9.99 2.34 0.009 0.89 9 4 1 137.99 0.83 2.32 0.003 0.86 -5 1 12 134.01 25.79 2.32 0.014 0.90 4 9 1 102.04 3.41 2.32 0.005 1.05 1 11 4 365.09 179.23 2.31 0.038 0.95 6 2 0 53.81 0.01 2.29 0.000 1.33 3 8 3 90.98 9.29 2.28 0.009 1.17 -1 11 7 191.15 49.76 2.28 0.020 0.87 -6 1 11 110.74 10.61 2.28 0.009 0.90 -3 7 6 194.67 72.16 2.28 0.024 1.17 3 1 7 75.53 2.21 2.26 0.004 1.35 2 4 11 150.87 24.58 2.25 0.014 0.95 Bond lengths and angles C1 - Distance Angles O1A 1.2213 (0.0087) O1B 1.2979 (0.0092) 125.83 (0.74) C2 1.5216 (0.0104) 121.11 (0.72) 113.06 (0.65) C1 - O1A O1B C2 - Distance Angles O2B 1.1987 (0.0087) O2A 1.2970 (0.0093) 124.53 (0.74) C1 1.5216 (0.0104) 122.06 (0.72) 113.40 (0.65) C2 - O2B O2A O1A - Distance Angles C1 1.2213 (0.0088) O1A - O1B - Distance Angles C1 1.2979 (0.0092) H1 0.8400 109.47 O1B - C1 O2A - Distance Angles C2 1.2970 (0.0093) H2 0.8400 109.47 O2A - C2 O2B - Distance Angles C2 1.1987 (0.0087) O2B - C22 - Distance Angles O22 1.2716 (0.0097) N23 1.3032 (0.0106) 127.07 (0.78) N21 1.3461 (0.0098) 123.12 (0.81) 109.80 (0.78) C22 - O22 N23 C24 - Distance Angles N23 1.4617 (0.0093) C25 1.5441 (0.0103) 100.70 (0.59) H24A 0.9900 111.63 111.63 H24B 0.9900 111.63 111.63 109.42 C24 - N23 C25 H24A C25 - Distance Angles N21 1.4566 (0.0094) C24 1.5441 (0.0103) 100.49 (0.59) H25A 0.9900 111.67 111.67 H25B 0.9900 111.67 111.67 109.45 C25 - N21 C24 H25A N21 - Distance Angles C22 1.3461 (0.0098) C25 1.4566 (0.0094) 110.48 (0.68) H21 0.8800 124.76 124.76 N21 - C22 C25 N23 - Distance Angles C22 1.3032 (0.0106) C24 1.4617 (0.0093) 111.72 (0.69) H23 0.8800 124.14 124.14 N23 - C22 C24 O22 - Distance Angles C22 1.2716 (0.0097) O22 - C32 - Distance Angles O32 1.2479 (0.0090) N31 1.3326 (0.0093) 125.78 (0.74) N33 1.3429 (0.0097) 124.99 (0.69) 109.19 (0.70) C32 - O32 N31 C34 - Distance Angles N33 1.4385 (0.0095) C35 1.5171 (0.0109) 101.66 (0.65) H34A 0.9900 111.44 111.44 H34B 0.9900 111.44 111.44 109.29 C34 - N33 C35 H34A C35 - Distance Angles N31 1.4461 (0.0098) C34 1.5171 (0.0109) 102.89 (0.62) H35A 0.9900 111.19 111.19 H35B 0.9900 111.19 111.19 109.12 C35 - N31 C34 H35A N31 - Distance Angles C32 1.3326 (0.0093) C35 1.4461 (0.0098) 110.72 (0.67) H31 0.8800 124.64 124.64 N31 - C32 C35 N33 - Distance Angles C32 1.3429 (0.0097) C34 1.4385 (0.0095) 111.60 (0.64) H33 0.8800 124.20 124.20 N33 - C32 C34 O32 - Distance Angles C32 1.2479 (0.0090) O32 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.71 2.535(8) 167.3 O1B-H1...O22_$1 0.88 2.06 2.867(8) 152.1 N23-H23...O1A_$1 0.84 1.66 2.480(8) 164.4 O2A-H2...O32_$2 0.88 2.04 2.890(8) 162.2 N21-H21...O1A_$2 0.88 2.07 2.858(8) 147.9 N31-H31...O2B_$3 0.88 2.06 2.831(8) 146.5 N33-H33...O2B_$4 FMAP and GRID set by program FMAP 2 2 15 GRID -2.083 -2 -2 2.083 2 2 R1 = 0.2012 for 1934 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.36 at 0.3832 0.0570 0.8773 [ 1.58 A from H34B ] Deepest hole -0.35 at 0.7733 0.0361 0.3871 [ 0.72 A from H1 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 2275 / 15063 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.6168 -0.5570 0.3773 1.00000 0.05 0.36 1.58 H34B 1.74 O32 1.80 H2 1.89 H34A Q2 1 -0.5305 -0.5008 0.3318 1.00000 0.05 0.35 1.60 H34A 1.69 H34B 1.72 C34 1.79 O32 Q3 1 -0.8126 -0.5222 0.2938 1.00000 0.05 0.33 1.55 H34B 1.84 C22 2.00 N23 2.04 O22 Q4 1 -0.3521 -0.1245 0.2027 1.00000 0.05 0.33 0.96 O32 1.31 H2 2.02 O2A 2.10 C32 Q5 1 0.0951 0.0850 0.6892 1.00000 0.05 0.31 1.09 H23 1.47 N23 1.72 O1A 1.72 H1 Q6 1 -0.2429 0.1092 0.3757 1.00000 0.05 0.31 1.31 H1 1.55 O1B 1.97 O22 2.17 H33 Q7 1 -0.4264 -0.0780 0.6862 1.00000 0.05 0.31 1.03 O2B 1.14 H33 1.94 N33 2.12 C2 Q8 1 -0.2010 0.0018 0.9627 1.00000 0.05 0.31 0.35 H25A 0.83 C25 1.32 H25B 1.92 N21 Q9 1 -0.1457 0.0921 0.6017 1.00000 0.05 0.30 1.66 H23 1.85 H35A 1.98 N23 2.00 O1B Q10 1 -0.7174 -0.1945 0.5116 1.00000 0.05 0.30 0.93 H35B 1.30 C35 1.41 H35A 2.07 N31 Shortest distances between peaks (including symmetry equivalents) 1 2 1.14 1 4 1.22 3 5 1.54 2 4 1.71 6 10 1.72 3 4 1.78 1 3 1.83 9 10 2.00 5 9 2.13 2 7 2.22 2 3 2.34 4 5 2.38 3 6 2.59 5 6 2.66 1 8 2.67 6 9 2.71 6 7 2.77 3 8 2.90 2 8 2.96 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 0.02: 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. 0.92: 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 0.36: Structure factors and derivatives 0.31: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0068p21c finished at 11:33:03 Total CPU time: 2.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++