+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0046c2c started at 13:15:49 on 23-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0046c2c in C2/c CELL 0.71073 16.6403 14.4382 7.6872 90.000 117.299 90.000 ZERR 4.00 0.0010 0.0005 0.0005 0.000 0.002 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O UNIT 48 88 24 28 V = 1641.20 F(000) = 768.0 Mu = 0.12 mm-1 Cell Wt = 1449.42 Rho = 1.467 MERG 2 OMIT -3.00 55.00 OMIT -4 0 2 OMIT 1 3 4 OMIT -8 0 4 OMIT 6 0 4 OMIT 4 10 2 OMIT -8 0 6 EXTI 0.01705 SHEL 7 0.77 HTAB O1B O22 HTAB N21 O32 HTAB N23 O1A EQIV_$1 -x, y, -z+3/2 MPLA C1 O1A O1B MPLA C1_$1 O1A_$1 O1B_$1 HTAB N31 O22 FMAP 2 PLAN 10 SIZE 0.10 0.16 0.18 ACTA BOND $H WGHT 0.01490 32.20900 L.S. 4 TEMP -153.00 FVAR 0.54585 MOLE 1 C2 1 0.000000 0.257754 0.750000 10.50000 0.01775 0.01797 = 0.03000 0.00000 0.01143 0.00000 AFIX 23 H2A 2 0.018964 0.298285 0.866090 10.50000 -1.20000 H2B 2 -0.018963 0.298285 0.633910 10.50000 -1.20000 AFIX 0 C1 1 0.081044 0.201207 0.771992 11.00000 0.01901 0.02379 = 0.02812 0.00092 0.01020 0.00074 O1A 4 0.098851 0.124335 0.840342 11.00000 0.02749 0.02316 = 0.05086 0.00970 0.02416 0.00481 O1B 4 0.131388 0.249914 0.712514 11.00000 0.02557 0.02553 = 0.04674 0.00776 0.02303 0.00237 AFIX 147 H1 2 0.183873 0.227708 0.761709 11.00000 -1.50000 AFIX 0 MOLE 2 C22 1 0.300534 0.098270 0.798156 11.00000 0.02151 0.01783 = 0.03121 0.00024 0.01292 0.00001 C24 1 0.275053 -0.059074 0.800351 11.00000 0.02556 0.02066 = 0.02791 -0.00276 0.00968 -0.00425 AFIX 23 H24A 2 0.237093 -0.100093 0.689739 11.00000 -1.20000 H24B 2 0.280596 -0.086232 0.923625 11.00000 -1.20000 AFIX 0 C25 1 0.368989 -0.043516 0.810329 11.00000 0.02776 0.01985 = 0.03416 0.00077 0.01475 0.00411 AFIX 23 H25A 2 0.417004 -0.076191 0.923486 11.00000 -1.20000 H25B 2 0.370015 -0.064239 0.688601 11.00000 -1.20000 AFIX 0 N21 3 0.379117 0.057616 0.833682 11.00000 0.02204 0.01959 = 0.03547 -0.00273 0.01200 -0.00164 AFIX 43 H21 2 0.430122 0.087583 0.866687 11.00000 -1.20000 AFIX 0 N23 3 0.238077 0.033825 0.771032 11.00000 0.01854 0.02440 = 0.04440 0.00181 0.01367 0.00034 AFIX 43 H23 2 0.181252 0.046363 0.739151 11.00000 -1.20000 AFIX 0 O22 4 0.288465 0.184615 0.791191 11.00000 0.02448 0.01946 = 0.05132 -0.00111 0.01854 0.00199 MOLE 3 C32 1 0.500000 0.247978 0.750000 10.50000 0.01962 0.02007 = 0.02163 0.00000 0.00852 0.00000 C35 1 0.452447 0.399676 0.747307 11.00000 0.02967 0.01931 = 0.03520 0.00373 0.01422 0.00288 AFIX 23 H35A 2 0.451874 0.438987 0.852251 11.00000 -1.20000 H35B 2 0.404701 0.420969 0.618967 11.00000 -1.20000 AFIX 0 N31 3 0.441571 0.301112 0.780291 11.00000 0.02611 0.02358 = 0.03425 -0.00009 0.01796 0.00098 AFIX 43 H31 2 0.401675 0.279717 0.815518 11.00000 -1.20000 AFIX 0 O32 4 0.500000 0.161956 0.750000 10.50000 0.02436 0.02060 = 0.04008 0.00000 0.01751 0.00000 HKLF 4 Covalent radii and connectivity table for 06skc0046c2c in C2/c C 0.770 H 0.320 N 0.700 O 0.660 C2 - C1_$1 C1 C1 - O1A O1B C2 O1A - C1 O1B - C1 C22 - O22 N23 N21 C24 - N23 C25 C25 - N21 C24 N21 - C22 C25 N23 - C22 C24 O22 - C22 C32 - O32 N31 N31_$2 C35 - N31 C35_$2 N31 - C32 C35 O32 - C32 Operators for generating equivalent atoms: $1 -x, y, -z+3/2 $2 -x+1, y, -z+3/2 h k l Fo^2 Sigma Why rejected 0 0 1 16.44 2.98 observed but should be systematically absent 10980 Reflections read, of which 261 rejected -21 =< h =< 20, -17 =< k =< 18, -9 =< l =< 9, Max. 2-theta = 54.96 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 6 16 0 3.76 2.82 3 14.26 1 Inconsistent equivalents 1868 Unique reflections, of which 0 suppressed R(int) = 0.0559 R(sigma) = 0.0481 Friedel opposites merged Maximum memory for data reduction = 1699 / 22297 Special position constraints for C2 x = 0.0000 z = 0.7500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C32 x = 0.5000 z = 0.7500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O32 x = 0.5000 z = 0.7500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 2038 / 149706 wR2 = 0.2731 before cycle 1 for 1868 data and 117 / 117 parameters GooF = S = 1.168; Restrained GooF = 1.168 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0149 * P )^2 + 32.21 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54583 0.00492 -0.003 OSF 2 0.01703 0.00301 -0.007 EXTI Mean shift/esd = 0.001 Maximum = -0.010 for tors H1 Max. shift = 0.001 A for H1 Max. dU = 0.000 for O22 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2038 / 149706 wR2 = 0.2731 before cycle 2 for 1868 data and 117 / 117 parameters GooF = S = 1.168; Restrained GooF = 1.168 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0149 * P )^2 + 32.21 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54582 0.00492 -0.003 OSF 2 0.01702 0.00301 -0.004 EXTI Mean shift/esd = 0.001 Maximum = -0.012 for tors H1 Max. shift = 0.001 A for H1 Max. dU = 0.000 for O22 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2038 / 149706 wR2 = 0.2731 before cycle 3 for 1868 data and 117 / 117 parameters GooF = S = 1.168; Restrained GooF = 1.168 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0149 * P )^2 + 32.21 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54582 0.00492 0.000 OSF 2 0.01702 0.00301 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.010 for tors H1 Max. shift = 0.001 A for H1 Max. dU = 0.000 for O22 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2038 / 149706 wR2 = 0.2731 before cycle 4 for 1868 data and 117 / 117 parameters GooF = S = 1.168; Restrained GooF = 1.168 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0149 * P )^2 + 32.21 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54582 0.00492 0.000 OSF 2 0.01701 0.00301 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.009 for tors H1 Max. shift = 0.001 A for H1 Max. dU = 0.000 for O22 Largest correlation matrix elements 0.782 EXTI / OSF 0.576 U13 O32 / U11 O32 0.547 U13 O22 / U11 O22 0.645 U13 O1B / U33 O1B 0.571 U13 C2 / U33 C2 0.547 U13 C2 / U11 C2 0.624 U13 O1A / U33 O1A 0.570 U13 O22 / U33 O22 0.546 U13 N21 / U33 N21 0.613 U13 O1B / U11 O1B 0.565 U13 C22 / U33 C22 0.541 U13 C35 / U33 C35 0.608 U13 O1A / U11 O1A 0.561 U13 C25 / U33 C25 0.541 U13 C1 / U33 C1 0.602 U13 N31 / U33 N31 0.558 U13 C32 / U33 C32 0.537 U13 N23 / U33 N23 0.588 U13 O32 / U33 O32 0.557 U13 C22 / U11 C22 0.534 U13 N21 / U11 N21 0.584 U13 N31 / U11 N31 0.547 z O1B / x O1B 0.533 U13 C25 / U11 C25 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.0190 0.2983 0.8661 23 0.990 0.000 C2 C1_$1 C1 H2B -0.0190 0.2983 0.6339 23 0.990 0.000 C2 C1_$1 C1 H1 0.1839 0.2278 0.7621 147 0.840 0.000 O1B C1 H1 H24A 0.2371 -0.1001 0.6897 23 0.990 0.000 C24 N23 C25 H24B 0.2806 -0.0862 0.9236 23 0.990 0.000 C24 N23 C25 H25A 0.4170 -0.0762 0.9235 23 0.990 0.000 C25 N21 C24 H25B 0.3700 -0.0642 0.6886 23 0.990 0.000 C25 N21 C24 H21 0.4301 0.0876 0.8667 43 0.880 0.000 N21 C22 C25 H23 0.1813 0.0464 0.7391 43 0.880 0.000 N23 C22 C24 H35A 0.4519 0.4390 0.8522 23 0.990 0.000 C35 N31 C35_$2 H35B 0.4047 0.4210 0.6190 23 0.990 0.000 C35 N31 C35_$2 H31 0.4017 0.2797 0.8155 43 0.880 0.000 N31 C32 C35 06skc0046c2c in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 0.00000 0.25776 0.75000 0.50000 0.01775 0.01797 0.02999 0.00000 0.01143 0.00000 0.02172 0.00767 0.00000 0.00053 0.00000 0.00000 0.00360 0.00368 0.00422 0.00000 0.00327 0.00000 0.00163 H2A 0.01896 0.29829 0.86609 0.50000 0.02606 0.00000 0.00000 H2B -0.01896 0.29829 0.63391 0.50000 0.02606 0.00000 0.00000 C1 0.08104 0.20121 0.77199 1.00000 0.01901 0.02378 0.02811 0.00092 0.01020 0.00074 0.02387 0.01220 0.00037 0.00039 0.00085 0.00000 0.00269 0.00297 0.00300 0.00227 0.00235 0.00215 0.00125 O1A 0.09885 0.12434 0.84034 1.00000 0.02749 0.02316 0.05086 0.00970 0.02416 0.00481 0.03144 0.01013 0.00028 0.00028 0.00071 0.00000 0.00223 0.00220 0.00282 0.00195 0.00210 0.00171 0.00110 O1B 0.13139 0.24991 0.71251 1.00000 0.02556 0.02554 0.04672 0.00776 0.02301 0.00236 0.03011 0.01011 0.00028 0.00030 0.00069 0.00000 0.00212 0.00215 0.00273 0.00189 0.00207 0.00170 0.00109 H1 0.18393 0.22784 0.76207 1.00000 0.04517 0.00000 0.00000 C22 0.30053 0.09827 0.79816 1.00000 0.02152 0.01782 0.03122 0.00023 0.01292 0.00001 0.02320 0.01229 0.00037 0.00038 0.00086 0.00000 0.00271 0.00268 0.00312 0.00225 0.00242 0.00210 0.00122 C24 0.27505 -0.05907 0.80035 1.00000 0.02555 0.02065 0.02791 -0.00276 0.00968 -0.00425 0.02571 0.01232 0.00039 0.00039 0.00088 0.00000 0.00291 0.00279 0.00297 0.00231 0.00242 0.00223 0.00129 H24A 0.23709 -0.10009 0.68974 1.00000 0.03085 0.00000 0.00000 H24B 0.28060 -0.08623 0.92363 1.00000 0.03085 0.00000 0.00000 C25 0.36899 -0.04352 0.81033 1.00000 0.02776 0.01984 0.03416 0.00077 0.01475 0.00412 0.02704 0.01328 0.00040 0.00039 0.00094 0.00000 0.00298 0.00282 0.00326 0.00236 0.00260 0.00231 0.00132 H25A 0.41700 -0.07619 0.92349 1.00000 0.03245 0.00000 0.00000 H25B 0.37002 -0.06424 0.68860 1.00000 0.03245 0.00000 0.00000 N21 0.37912 0.05762 0.83368 1.00000 0.02203 0.01959 0.03546 -0.00273 0.01200 -0.00164 0.02615 0.01058 0.00033 0.00033 0.00075 0.00000 0.00244 0.00241 0.00283 0.00206 0.00218 0.00189 0.00116 H21 0.43012 0.08758 0.86668 1.00000 0.03138 0.00000 0.00000 N23 0.23808 0.03382 0.77103 1.00000 0.01854 0.02440 0.04440 0.00181 0.01367 0.00034 0.02941 0.01122 0.00033 0.00034 0.00083 0.00000 0.00239 0.00262 0.00315 0.00222 0.00224 0.00195 0.00124 H23 0.18125 0.04636 0.73915 1.00000 0.03529 0.00000 0.00000 O22 0.28846 0.18462 0.79119 1.00000 0.02447 0.01945 0.05131 -0.00111 0.01854 0.00199 0.03129 0.00949 0.00028 0.00028 0.00070 0.00000 0.00213 0.00210 0.00292 0.00190 0.00204 0.00166 0.00111 C32 0.50000 0.24798 0.75000 0.50000 0.01961 0.02007 0.02162 0.00000 0.00852 0.00000 0.02080 0.00777 0.00000 0.00054 0.00000 0.00000 0.00362 0.00379 0.00381 0.00000 0.00313 0.00000 0.00158 C35 0.45245 0.39968 0.74730 1.00000 0.02966 0.01931 0.03520 0.00373 0.01422 0.00289 0.02831 0.01354 0.00040 0.00040 0.00095 0.00000 0.00322 0.00278 0.00340 0.00246 0.00269 0.00237 0.00137 H35A 0.45187 0.43899 0.85225 1.00000 0.03397 0.00000 0.00000 H35B 0.40470 0.42097 0.61896 1.00000 0.03397 0.00000 0.00000 N31 0.44157 0.30111 0.78029 1.00000 0.02610 0.02358 0.03425 -0.00010 0.01796 0.00098 0.02638 0.01098 0.00034 0.00033 0.00076 0.00000 0.00254 0.00259 0.00277 0.00209 0.00223 0.00200 0.00116 H31 0.40167 0.27972 0.81552 1.00000 0.03166 0.00000 0.00000 O32 0.50000 0.16196 0.75000 0.50000 0.02436 0.02060 0.04008 0.00000 0.01751 0.00000 0.02729 0.00557 0.00000 0.00039 0.00000 0.00000 0.00293 0.00297 0.00356 0.00000 0.00271 0.00000 0.00136 Final Structure Factor Calculation for 06skc0046c2c in C2/c Total number of l.s. parameters = 117 Maximum vector length = 511 Memory required = 1921 / 22995 wR2 = 0.2731 before cycle 5 for 1868 data and 0 / 117 parameters GooF = S = 1.168; Restrained GooF = 1.168 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0149 * P )^2 + 32.21 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1115 for 1411 Fo > 4sig(Fo) and 0.1392 for all 1868 data wR2 = 0.2731, GooF = S = 1.168, Restrained GooF = 1.168 for all data Occupancy sum of asymmetric unit = 12.50 for non-hydrogen and 11.00 for hydrogen atoms Principal mean square atomic displacements U 0.0305 0.0180 0.0167 C2 0.0292 0.0237 0.0187 C1 0.0539 0.0203 0.0201 O1A 0.0493 0.0236 0.0174 O1B 0.0314 0.0203 0.0178 C22 0.0318 0.0274 0.0179 C24 0.0343 0.0290 0.0178 C25 0.0375 0.0223 0.0187 N21 0.0467 0.0242 0.0173 N23 0.0525 0.0236 0.0178 O22 0.0228 0.0201 0.0195 C32 0.0366 0.0301 0.0182 C35 0.0347 0.0240 0.0204 N31 0.0401 0.0211 0.0206 O32 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.026 0.040 0.055 0.071 0.089 0.114 0.157 0.224 1.000 Number in group 188. 205. 170. 188. 188. 189. 180. 186. 186. 188. GooF 1.507 1.368 1.204 0.985 1.010 1.332 0.916 1.099 0.874 1.184 K 23.219 3.209 1.979 1.268 1.165 1.211 1.031 1.062 1.014 0.992 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.66 inf Number in group 193. 182. 188. 191. 184. 184. 185. 186. 188. 187. GooF 0.740 0.707 0.720 0.780 0.743 0.878 1.100 1.372 1.640 2.086 K 1.008 0.982 1.024 1.010 1.046 1.032 1.057 1.033 1.037 1.016 R1 0.273 0.234 0.213 0.184 0.129 0.112 0.110 0.115 0.121 0.095 Recommended weighting scheme: WGHT 0.0148 32.2064 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 1 2 2119.96 519.68 7.42 0.149 2.32 -5 9 2 646.32 15.85 6.37 0.026 1.42 2 10 2 909.00 137.83 5.93 0.077 1.27 -3 3 6 483.45 0.25 5.68 0.003 1.20 -2 4 1 439.21 1.40 5.59 0.008 3.19 4 4 2 896.91 165.04 5.51 0.084 1.80 -6 0 4 453.32 0.02 5.45 0.001 1.86 1 3 2 2929.10 1395.52 5.35 0.243 2.57 -1 1 5 415.18 6.54 5.16 0.017 1.41 -6 2 4 377.83 8.61 4.93 0.019 1.80 0 6 1 670.59 116.67 4.93 0.070 2.27 -4 2 1 743.53 147.77 4.90 0.079 3.59 -6 2 5 676.68 130.99 4.73 0.075 1.50 -12 2 1 883.34 233.47 4.69 0.100 1.30 -3 3 2 326.11 6.62 4.64 0.017 2.94 -6 8 1 613.16 111.59 4.61 0.069 1.51 -2 2 3 1375.70 525.89 4.58 0.149 2.38 -8 2 4 417.53 34.79 4.56 0.038 1.66 -9 1 1 293.46 0.03 4.52 0.001 1.78 -4 2 2 566.61 102.83 4.46 0.066 3.08 -11 1 3 726.85 173.66 4.39 0.086 1.49 5 9 3 444.05 65.08 4.16 0.053 1.10 -12 10 2 734.19 169.70 4.14 0.085 1.00 -8 2 3 243.28 1.49 4.06 0.008 1.87 8 2 1 1590.63 748.73 4.00 0.178 1.57 7 5 1 216.60 0.04 3.89 0.001 1.53 4 2 5 244.27 3.74 3.82 0.013 1.11 4 10 1 335.88 42.00 3.80 0.042 1.28 -5 9 1 322.59 49.63 3.55 0.046 1.44 -2 10 4 1554.33 802.76 3.55 0.185 1.14 5 5 3 271.38 28.89 3.49 0.035 1.33 -2 0 6 502.95 130.64 3.47 0.074 1.21 10 0 2 2986.55 1886.73 3.44 0.283 1.17 -7 1 1 4268.88 3006.08 3.28 0.357 2.31 4 0 2 526.18 165.79 3.27 0.084 2.08 -6 2 2 950.05 430.43 3.26 0.135 2.50 -1 5 2 583.08 201.28 3.26 0.092 2.28 -7 7 4 549.32 189.58 3.14 0.090 1.35 -12 4 2 152.63 1.20 3.10 0.007 1.29 -11 5 5 461.24 144.20 3.07 0.078 1.19 -5 1 2 3603.42 2535.64 3.04 0.328 2.96 -7 11 3 139.45 2.77 2.97 0.011 1.11 17 1 1 208.16 17.80 2.93 0.027 0.82 -6 4 5 153.92 9.08 2.93 0.020 1.41 0 10 4 289.00 63.98 2.92 0.052 1.10 -9 1 6 156.19 4.59 2.90 0.014 1.23 -1 5 4 249.25 49.00 2.86 0.046 1.52 7 5 3 156.35 10.90 2.81 0.022 1.17 5 3 0 26677.32 23549.69 2.80 1.000 2.52 -7 7 2 587.04 244.96 2.78 0.102 1.55 Bond lengths and angles C2 - Distance Angles C1_$1 1.5181 (0.0067) C1 1.5181 (0.0067) 114.93 (0.65) H2A 0.9900 108.54 108.54 H2B 0.9900 108.54 108.54 107.53 C2 - C1_$1 C1 H2A C1 - Distance Angles O1A 1.2054 (0.0069) O1B 1.3254 (0.0069) 124.82 (0.53) C2 1.5181 (0.0067) 124.89 (0.53) 110.24 (0.47) C1 - O1A O1B O1A - Distance Angles C1 1.2054 (0.0069) O1A - O1B - Distance Angles C1 1.3254 (0.0069) H1 0.8400 109.47 O1B - C1 C22 - Distance Angles O22 1.2600 (0.0069) N23 1.3381 (0.0072) 125.74 (0.52) N21 1.3422 (0.0072) 124.25 (0.52) 110.01 (0.48) C22 - O22 N23 C24 - Distance Angles N23 1.4496 (0.0074) C25 1.5459 (0.0081) 102.75 (0.45) H24A 0.9900 111.22 111.22 H24B 0.9900 111.22 111.22 109.14 C24 - N23 C25 H24A C25 - Distance Angles N21 1.4714 (0.0071) C24 1.5459 (0.0081) 101.94 (0.45) H25A 0.9900 111.38 111.38 H25B 0.9900 111.38 111.38 109.25 C25 - N21 C24 H25A N21 - Distance Angles C22 1.3422 (0.0072) C25 1.4714 (0.0071) 111.27 (0.47) H21 0.8800 124.36 124.36 N21 - C22 C25 N23 - Distance Angles C22 1.3381 (0.0072) C24 1.4496 (0.0074) 112.04 (0.46) H23 0.8800 123.98 123.98 N23 - C22 C24 O22 - Distance Angles C22 1.2600 (0.0069) O22 - C32 - Distance Angles O32 1.2420 (0.0097) N31 1.3401 (0.0065) 124.92 (0.35) N31_$2 1.3401 (0.0065) 124.92 (0.35) 110.15 (0.70) C32 - O32 N31 C35 - Distance Angles N31 1.4712 (0.0073) C35_$2 1.5641 (0.0119) 101.44 (0.31) H35A 0.9900 111.48 111.48 H35B 0.9900 111.48 111.48 109.31 C35 - N31 C35_$2 H35A N31 - Distance Angles C32 1.3401 (0.0065) C35 1.4712 (0.0073) 111.56 (0.50) H31 0.8800 124.22 124.22 N31 - C32 C35 O32 - Distance Angles C32 1.2420 (0.0097) O32 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.76 2.576(6) 162.4 O1B-H1...O22 0.88 2.07 2.814(6) 142.3 N21-H21...O32 0.88 2.18 2.914(7) 141.3 N23-H23...O1A 0.88 2.27 3.086(6) 154.5 N31-H31...O22 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 1.5564 (0.1727) x + 5.6312 (0.0824) y + 5.9278 (0.0314) z = 5.8354 (0.0184) * 0.0000 (0.0000) C1 * 0.0000 (0.0000) O1A * 0.0000 (0.0000) O1B Rms deviation of fitted atoms = 0.0000 1.5564 (0.1725) x - 5.6312 (0.0823) y + 5.9278 (0.0312) z = 3.0563 (0.0310) Angle to previous plane (with approximate esd) = 45.91 ( 0.51 ) * 0.0000 (0.0000) C1_$1 * 0.0000 (0.0000) O1A_$1 * 0.0000 (0.0000) O1B_$1 Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 2 23 GRID -1.250 -2 -1 1.250 2 1 R1 = 0.1392 for 1868 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.48 at 0.1340 0.2447 0.5508 [ 1.27 A from O1B ] Deepest hole -0.46 at 0.0667 0.0111 0.3805 [ 1.09 A from H35B ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 2124 / 22213 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1340 0.2447 0.5508 1.00000 0.05 0.48 1.27 O1B 1.47 H1 2.33 C1 2.36 N31 Q2 1 0.4224 0.2949 0.6004 1.00000 0.05 0.41 1.27 N31 1.44 C32 1.82 C35 1.85 H31 Q3 1 0.3074 -0.1480 0.7623 1.00000 0.05 0.40 1.25 H24A 1.47 C24 1.74 H24B 1.75 O1B Q4 1 0.4908 0.5467 0.8397 1.00000 0.05 0.39 1.70 H35A 1.87 O1A 2.12 O1A 2.12 H35A Q5 1 0.1850 0.3021 0.8613 1.00000 0.05 0.38 1.31 H1 1.32 O1B 2.07 H24A 2.09 H25B Q6 1 0.5000 -0.0381 0.7500 0.50000 0.05 0.37 2.03 H25B 2.38 H25A 2.43 C25 2.49 H2A Q7 1 0.0000 0.1225 0.7500 0.50000 0.05 0.37 1.46 O1A 1.71 C1 1.95 C2 2.66 H2A Q8 1 0.1513 0.1214 0.7006 1.00000 0.05 0.37 1.17 H23 1.63 H1 1.67 O1A 1.81 N23 Q9 1 0.4851 0.1398 0.5698 1.00000 0.05 0.36 1.33 O32 1.47 H21 1.49 H25A 2.03 C32 Q10 1 0.3694 -0.0359 0.9554 1.00000 0.05 0.35 1.10 H25A 1.12 C25 1.51 C24 1.56 H24B Shortest distances between peaks (including symmetry equivalents) 3 5 1.24 1 2 1.25 4 7 1.34 4 4 1.54 1 3 2.03 1 8 2.07 3 10 2.12 9 10 2.28 1 5 2.29 2 8 2.39 1 9 2.43 4 8 2.48 2 9 2.53 6 10 2.55 2 2 2.55 9 9 2.58 5 5 2.69 4 4 2.70 7 8 2.71 3 9 2.82 5 8 2.83 6 9 2.87 6 9 2.97 Time profile in seconds ----------------------- 0.05: 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. 0.52: 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 0.28: Structure factors and derivatives 0.19: 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 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0046c2c finished at 13:15:50 Total CPU time: 1.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++