+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008skc0001 started at 09:52:33 on 13-Oct-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008skc0001 in P-1 CELL 0.71073 6.9980 8.3790 9.2500 116.302 101.825 91.149 ZERR 1.00 0.0003 0.0003 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H N O UNIT 16 20 5 8 V = 472.10 F(000) = 215.0 Mu = 0.12 mm-1 Cell Wt = 410.37 Rho = 1.443 MERG 2 OMIT -3.00 55.00 OMIT 0 1 1 OMIT -2 -1 1 SHEL 7 0.77 EQIV_$1 x+1, y, z HTAB N32 O1A_$1 HTAB N32 O1B_$1 HTAB N42 O1A_$1 HTAB N42 O1B_$1 EQIV_$2 -x+2, -y+1, -z+2 HTAB N21 O1B_$2 EQIV_$3 -x+2, -y+2, -z+3 HTAB N23 O1A_$3 EQIV_$4 -x+1, -y+1, -z+3 HTAB O3B O3B_$4 HTAB O3B O3A_$4 SIMU FMAP 2 PLAN 5 SIZE 0.07 0.09 0.19 ACTA BOND $H WGHT 0.04300 0.25670 L.S. 8 TEMP -153.00 FVAR 1.68544 MOLE 1 PART -1 C33 1 1.550114 0.865560 0.969399 10.25000 0.02951 AFIX 43 H33 2 1.603211 0.754877 0.938724 10.25000 -1.20000 AFIX 0 C35 1 1.450938 1.094314 0.949380 10.25000 0.00788 AFIX 43 H35 2 1.428604 1.186461 0.916855 10.25000 -1.20000 AFIX 0 C31 1 1.483902 1.116588 1.107463 10.25000 0.01150 AFIX 43 H31 2 1.462084 1.219168 1.200097 10.25000 -1.20000 AFIX 0 N32 3 1.550227 0.974321 1.110970 10.25000 0.00636 AFIX 43 H32 2 1.588659 0.959046 1.200227 10.25000 -1.20000 AFIX 0 N34 1 1.454732 0.932740 0.853428 10.25000 0.02362 AFIX 43 H34 2 1.408140 0.869749 0.736145 10.25000 -1.20000 AFIX 0 PART -2 C43 1 1.534500 0.836863 0.939527 10.25000 0.00670 AFIX 43 H43 2 1.554937 0.714665 0.903257 10.25000 -1.20000 AFIX 0 C44 1 1.455647 0.911055 0.844945 10.25000 0.01486 AFIX 43 H44 2 1.430556 0.856128 0.727234 10.25000 -1.20000 AFIX 0 C41 1 1.505507 1.130470 1.105703 10.25000 0.02054 AFIX 43 H41 2 1.519461 1.242203 1.202165 10.25000 -1.20000 AFIX 0 N42 3 1.580229 0.968946 1.097745 10.25000 0.01416 AFIX 43 H42 2 1.646435 0.957634 1.183776 10.25000 -1.20000 AFIX 0 N45 1 1.412802 1.092587 0.951100 10.25000 0.00561 AFIX 43 H45 2 1.335354 1.166794 0.916396 10.25000 -1.20000 AFIX 0 MOLE 2 PART 0 C1 1 0.767437 0.766770 1.317302 11.00000 0.01729 0.01640 = 0.01602 0.00805 0.00452 0.00154 C2 1 0.888103 0.693343 1.424927 11.00000 0.01900 0.02205 = 0.01861 0.01072 0.00184 0.00431 AFIX 23 H2A 2 0.994602 0.787642 1.509249 11.00000 -1.20000 H2B 2 0.950060 0.591099 1.354844 11.00000 -1.20000 AFIX 0 C3 1 0.763537 0.630962 1.512572 11.00000 0.02488 0.01537 = 0.01600 0.00800 0.00193 0.00472 C22 1 1.268515 0.712084 1.212168 11.00000 0.01869 0.01944 = 0.01817 0.00865 0.00406 0.00230 AFIX 43 H22 2 1.346244 0.656128 1.268911 11.00000 -1.20000 AFIX 0 C24 1 1.099514 0.907020 1.160149 11.00000 0.02340 0.02058 = 0.01944 0.00973 0.00307 0.00543 AFIX 43 H24 2 1.039252 1.012235 1.175914 11.00000 -1.20000 AFIX 0 C25 1 1.093785 0.763133 1.013324 11.00000 0.02228 0.02174 = 0.01766 0.01044 0.00147 0.00349 AFIX 43 H25 2 1.028679 0.747600 0.906342 11.00000 -1.20000 AFIX 0 N21 3 1.200809 0.643135 1.048868 11.00000 0.02214 0.01640 = 0.01430 0.00429 0.00351 0.00341 AFIX 43 H21 2 1.220964 0.537838 0.975175 11.00000 -1.20000 AFIX 0 N23 3 1.209028 0.872749 1.282762 11.00000 0.02249 0.01792 = 0.01307 0.00466 0.00302 0.00272 AFIX 43 H23 2 1.235267 0.945225 1.390071 11.00000 -1.20000 AFIX 0 O1A 4 0.722058 0.923818 1.388253 11.00000 0.02998 0.01718 = 0.01631 0.00567 0.00434 0.00620 O1B 4 0.715585 0.671476 1.162634 11.00000 0.03153 0.02024 = 0.01384 0.00611 0.00319 0.00660 O3A 4 0.834450 0.647369 1.651879 11.00000 0.03207 0.03199 = 0.01581 0.01249 -0.00148 0.00074 O3B 4 0.586861 0.558725 1.427375 11.00000 0.02642 0.03981 = 0.02392 0.02187 -0.00442 -0.00972 H3B 2 0.500000 0.500000 1.500000 10.50000 0.09923 HKLF 4 Covalent radii and connectivity table for 2008skc0001 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C33 - N32 N34 C35 - N34 C31 C31 - N32 C35 N32 - C33 C31 N34 - C35 C33 C43 - C44 N42 C44 - C43 N45 C41 - N45 N42 N42 - C43 C41 N45 - C41 C44 C1 - O1B O1A C2 C2 - C1 C3 C3 - O3A O3B C2 C22 - N21 N23 C24 - C25 N23 C25 - C24 N21 N21 - C22 C25 N23 - C22 C24 O1A - C1 O1B - C1 O3A - C3 O3B - C3 Operators for generating equivalent atoms: $1 x+1, y, z $2 -x+2, -y+1, -z+2 $3 -x+2, -y+2, -z+3 $4 -x+1, -y+1, -z+3 10855 Reflections read, of which 32 rejected -9 =< h =< 9, -10 =< k =< 10, -12 =< l =< 12, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 2155 Unique reflections, of which 0 suppressed R(int) = 0.0495 R(sigma) = 0.0435 Friedel opposites merged Maximum memory for data reduction = 2479 / 21658 Special position constraints for H3B x = 0.5000 y = 0.5000 z = 1.5000 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 = 2935 / 187920 wR2 = 0.1109 before cycle 1 for 2155 data and 150 / 150 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 91. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.054 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.014 for 91 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0430 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.68541 0.00407 -0.007 OSF Mean shift/su = 0.003 Maximum = -0.009 for U23 O1B Max. shift = 0.000 A for C33 Max. dU = 0.000 for C41 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2935 / 187920 wR2 = 0.1109 before cycle 2 for 2155 data and 150 / 150 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 91. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.054 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.014 for 91 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0430 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.68540 0.00407 -0.002 OSF Mean shift/su = 0.001 Maximum = -0.003 for U23 O1B Max. shift = 0.000 A for N34 Max. dU = 0.000 for C44 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2935 / 187920 wR2 = 0.1109 before cycle 3 for 2155 data and 150 / 150 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 91. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.054 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.014 for 91 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0430 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.68540 0.00407 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for x C44 Max. shift = 0.000 A for N34 Max. dU = 0.000 for H3B Least-squares cycle 4 Maximum vector length = 511 Memory required = 2935 / 187920 wR2 = 0.1109 before cycle 4 for 2155 data and 150 / 150 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 91. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.054 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.014 for 91 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0430 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.68541 0.00407 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x N34 Max. shift = 0.000 A for N34 Max. dU = 0.000 for H3B Least-squares cycle 5 Maximum vector length = 511 Memory required = 2935 / 187920 wR2 = 0.1109 before cycle 5 for 2155 data and 150 / 150 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 91. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.054 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.014 for 91 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0430 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.68540 0.00407 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for x C44 Max. shift = 0.000 A for N34 Max. dU = 0.000 for N34 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2935 / 187920 wR2 = 0.1109 before cycle 6 for 2155 data and 150 / 150 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 91. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.054 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.014 for 91 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0430 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.68541 0.00407 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for x C44 Max. shift = 0.000 A for N34 Max. dU = 0.000 for H3B Least-squares cycle 7 Maximum vector length = 511 Memory required = 2935 / 187920 wR2 = 0.1109 before cycle 7 for 2155 data and 150 / 150 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 91. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.054 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.014 for 91 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0430 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.68541 0.00407 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x C44 Max. shift = 0.000 A for C44 Max. dU = 0.000 for N34 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2935 / 187920 wR2 = 0.1109 before cycle 8 for 2155 data and 150 / 150 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 91. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.054 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.014 for 91 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0430 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.68541 0.00407 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x C44 Max. shift = 0.000 A for N34 Max. dU = 0.000 for C35 Largest correlation matrix elements -0.917 z C44 / z N34 0.746 z C43 / U11 C33 -0.696 y C41 / y C31 -0.911 x C44 / x N34 -0.737 z N42 / z N32 -0.695 z N45 / y N42 -0.893 U11 C44 / U11 N34 -0.728 z C41 / z C31 -0.679 U11 N45 / x C35 -0.843 U11 C41 / U11 C31 -0.724 y N45 / y C35 -0.677 y N32 / z C35 0.811 z N45 / y N45 -0.720 U11 N45 / U11 C35 -0.660 U11 C43 / U11 C33 0.791 z C35 / y C35 -0.713 y N42 / y N32 -0.650 y N45 / z N42 0.766 z N42 / y N42 -0.707 U11 N42 / U11 N32 -0.641 y N45 / y N42 0.753 z N32 / y N32 0.707 x N45 / U11 C35 0.637 U23 O3B / U22 O3B Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H33 1.6032 0.7549 0.9387 43 0.950 0.000 C33 N32 N34 H35 1.4286 1.1865 0.9169 43 0.950 0.000 C35 N34 C31 H31 1.4621 1.2192 1.2001 43 0.950 0.000 C31 N32 C35 H32 1.5887 0.9591 1.2002 43 0.880 0.000 N32 C33 C31 H34 1.4081 0.8697 0.7361 43 0.950 0.000 N34 C35 C33 H43 1.5549 0.7147 0.9033 43 0.950 0.000 C43 C44 N42 H44 1.4306 0.8561 0.7272 43 0.950 0.000 C44 C43 N45 H41 1.5195 1.2422 1.2022 43 0.950 0.000 C41 N45 N42 H42 1.6464 0.9576 1.1838 43 0.880 0.000 N42 C43 C41 H45 1.3353 1.1668 0.9164 43 0.950 0.000 N45 C41 C44 H2A 0.9946 0.7876 1.5092 23 0.990 0.000 C2 C1 C3 H2B 0.9501 0.5911 1.3548 23 0.990 0.000 C2 C1 C3 H22 1.3462 0.6561 1.2689 43 0.950 0.000 C22 N21 N23 H24 1.0393 1.0122 1.1759 43 0.950 0.000 C24 C25 N23 H25 1.0287 0.7476 0.9063 43 0.950 0.000 C25 C24 N21 H21 1.2210 0.5378 0.9752 43 0.880 0.000 N21 C22 C25 H23 1.2353 0.9452 1.3901 43 0.880 0.000 N23 C22 C24 2008skc0001 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C33 1.55011 0.86557 0.96941 0.25000 0.02950 0.04441 0.00234 0.00205 0.00257 0.00000 0.00405 H33 1.60322 0.75489 0.93874 0.25000 0.03540 0.00000 0.00000 C35 1.45094 1.09432 0.94938 0.25000 0.00787 0.03193 0.00156 0.00183 0.00187 0.00000 0.00253 H35 1.42862 1.18646 0.91685 0.25000 0.00945 0.00000 0.00000 C31 1.48390 1.11659 1.10746 0.25000 0.01149 0.02914 0.00186 0.00168 0.00159 0.00000 0.00325 H31 1.46207 1.21917 1.20009 0.25000 0.01379 0.00000 0.00000 N32 1.55022 0.97433 1.11097 0.25000 0.00636 0.02927 0.00127 0.00187 0.00140 0.00000 0.00217 H32 1.58865 0.95905 1.20023 0.25000 0.00763 0.00000 0.00000 N34 1.45471 0.93274 0.85343 0.25000 0.02361 0.05878 0.00303 0.00344 0.00307 0.00000 0.00570 H34 1.40810 0.86974 0.73615 0.25000 0.02833 0.00000 0.00000 C43 1.53450 0.83686 0.93952 0.25000 0.00669 0.02636 0.00152 0.00133 0.00139 0.00000 0.00215 H43 1.55493 0.71466 0.90325 0.25000 0.00802 0.00000 0.00000 C44 1.45567 0.91106 0.84495 0.25000 0.01485 0.04407 0.00266 0.00233 0.00246 0.00000 0.00466 H44 1.43060 0.85613 0.72724 0.25000 0.01783 0.00000 0.00000 C41 1.50551 1.13047 1.10571 0.25000 0.02053 0.03634 0.00225 0.00211 0.00204 0.00000 0.00405 H41 1.51946 1.24221 1.20217 0.25000 0.02463 0.00000 0.00000 N42 1.58023 0.96894 1.09774 0.25000 0.01416 0.03136 0.00166 0.00220 0.00171 0.00000 0.00281 H42 1.64643 0.95762 1.18377 0.25000 0.01699 0.00000 0.00000 N45 1.41280 1.09258 0.95110 0.25000 0.00561 0.03926 0.00161 0.00200 0.00194 0.00000 0.00236 H45 1.33535 1.16678 0.91639 0.25000 0.00673 0.00000 0.00000 C1 0.76744 0.76677 1.31730 1.00000 0.01728 0.01640 0.01602 0.00805 0.00452 0.00154 0.01624 0.00343 0.00022 0.00019 0.00018 0.00000 0.00074 0.00071 0.00070 0.00059 0.00056 0.00057 0.00031 C2 0.88810 0.69334 1.42493 1.00000 0.01900 0.02205 0.01860 0.01071 0.00184 0.00431 0.01974 0.00369 0.00023 0.00021 0.00019 0.00000 0.00078 0.00078 0.00073 0.00063 0.00059 0.00061 0.00034 H2A 0.99460 0.78764 1.50925 1.00000 0.02369 0.00000 0.00000 H2B 0.95006 0.59110 1.35484 1.00000 0.02369 0.00000 0.00000 C3 0.76354 0.63096 1.51257 1.00000 0.02487 0.01536 0.01600 0.00800 0.00193 0.00472 0.01887 0.00355 0.00024 0.00020 0.00018 0.00000 0.00081 0.00072 0.00071 0.00059 0.00059 0.00060 0.00033 C22 1.26852 0.71208 1.21217 1.00000 0.01868 0.01944 0.01817 0.00865 0.00406 0.00230 0.01880 0.00354 0.00023 0.00020 0.00019 0.00000 0.00075 0.00075 0.00072 0.00062 0.00058 0.00059 0.00033 H22 1.34625 0.65613 1.26891 1.00000 0.02256 0.00000 0.00000 C24 1.09951 0.90702 1.16015 1.00000 0.02339 0.02058 0.01944 0.00973 0.00307 0.00543 0.02120 0.00365 0.00024 0.00021 0.00019 0.00000 0.00082 0.00078 0.00077 0.00064 0.00062 0.00063 0.00035 H24 1.03925 1.01223 1.17591 1.00000 0.02544 0.00000 0.00000 C25 1.09379 0.76313 1.01333 1.00000 0.02228 0.02173 0.01766 0.01044 0.00147 0.00349 0.02053 0.00367 0.00024 0.00021 0.00019 0.00000 0.00080 0.00079 0.00073 0.00063 0.00059 0.00063 0.00034 H25 1.02868 0.74760 0.90634 1.00000 0.02463 0.00000 0.00000 N21 1.20081 0.64314 1.04887 1.00000 0.02214 0.01640 0.01430 0.00429 0.00350 0.00340 0.01877 0.00294 0.00019 0.00017 0.00015 0.00000 0.00069 0.00062 0.00061 0.00051 0.00050 0.00051 0.00029 H21 1.22096 0.53784 0.97517 1.00000 0.02253 0.00000 0.00000 N23 1.20903 0.87275 1.28276 1.00000 0.02249 0.01791 0.01307 0.00466 0.00302 0.00272 0.01894 0.00300 0.00020 0.00017 0.00015 0.00000 0.00068 0.00064 0.00059 0.00051 0.00049 0.00052 0.00029 H23 1.23527 0.94523 1.39007 1.00000 0.02273 0.00000 0.00000 O1A 0.72206 0.92382 1.38825 1.00000 0.02998 0.01718 0.01631 0.00567 0.00434 0.00620 0.02206 0.00255 0.00017 0.00014 0.00013 0.00000 0.00064 0.00055 0.00054 0.00044 0.00045 0.00046 0.00027 O1B 0.71558 0.67148 1.16263 1.00000 0.03153 0.02024 0.01384 0.00610 0.00319 0.00660 0.02282 0.00254 0.00017 0.00014 0.00013 0.00000 0.00065 0.00056 0.00052 0.00044 0.00045 0.00048 0.00027 O3A 0.83445 0.64737 1.65188 1.00000 0.03206 0.03199 0.01581 0.01249 -0.00148 0.00074 0.02724 0.00263 0.00018 0.00016 0.00013 0.00000 0.00068 0.00067 0.00056 0.00050 0.00047 0.00052 0.00030 O3B 0.58686 0.55872 1.42737 1.00000 0.02641 0.03981 0.02392 0.02187 -0.00442 -0.00972 0.02916 0.00272 0.00018 0.00017 0.00014 0.00000 0.00065 0.00072 0.00060 0.00055 0.00048 0.00053 0.00031 H3B 0.50000 0.50000 1.50000 0.50000 0.09921 0.00000 0.00000 0.00000 0.00000 0.00000 0.01494 Final Structure Factor Calculation for 2008skc0001 in P-1 Total number of l.s. parameters = 150 Maximum vector length = 511 Memory required = 2785 / 22995 wR2 = 0.1109 before cycle 9 for 2155 data and 0 / 150 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 91. 0. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.054 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.014 for 91 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0430 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0447 for 1691 Fo > 4sig(Fo) and 0.0628 for all 2155 data wR2 = 0.1109, GooF = S = 1.036, Restrained GooF = 1.014 for all data Occupancy sum of asymmetric unit = 14.50 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0177 0.0167 0.0144 C1 0.0233 0.0217 0.0142 C2 0.0277 0.0163 0.0127 C3 0.0195 0.0189 0.0180 C22 0.0268 0.0203 0.0165 C24 0.0253 0.0218 0.0145 C25 0.0239 0.0193 0.0132 N21 0.0238 0.0202 0.0128 N23 0.0323 0.0191 0.0148 O1A 0.0349 0.0197 0.0138 O1B 0.0377 0.0314 0.0126 O3A 0.0533 0.0195 0.0146 O3B Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.027 0.040 0.056 0.071 0.094 0.121 0.159 0.228 1.000 Number in group 225. 215. 214. 221. 204. 214. 214. 217. 216. 215. GooF 0.883 0.993 1.078 1.070 1.146 1.049 1.033 1.042 0.975 1.080 K 1.786 0.977 0.961 0.941 0.962 0.978 1.005 1.011 1.019 0.990 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.65 inf Number in group 221. 219. 207. 219. 216. 210. 218. 219. 210. 216. GooF 1.002 1.078 1.026 0.980 0.901 0.898 0.877 0.955 1.080 1.445 K 1.021 0.990 1.027 0.994 0.999 1.018 1.021 1.013 1.036 0.965 R1 0.169 0.148 0.129 0.082 0.063 0.052 0.039 0.041 0.035 0.035 Recommended weighting scheme: WGHT 0.0429 0.2557 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)/su Fc/Fc(max) Resolution(A) 3 1 1 37.08 23.12 4.40 0.079 1.87 6 -1 6 5.95 17.47 4.22 0.069 0.80 -1 -1 1 173.70 220.43 3.84 0.244 5.26 2 -1 4 5.80 1.78 3.83 0.022 1.69 -1 0 1 28.06 18.13 3.59 0.070 5.94 -1 2 2 8.72 3.89 3.56 0.032 2.30 -3 -1 2 118.86 93.34 3.53 0.159 2.20 1 -1 1 2805.31 3349.09 3.38 0.951 4.79 -3 -2 1 46.40 33.94 3.30 0.096 1.98 -1 7 4 -0.07 5.03 3.28 0.037 0.81 -2 4 8 0.87 7.77 3.26 0.046 0.77 1 -2 1 94.25 117.90 3.17 0.178 3.59 -1 -5 4 10.22 17.01 3.13 0.068 1.57 2 3 2 105.61 82.92 3.12 0.150 1.46 3 -3 3 55.50 41.76 3.10 0.106 1.60 -6 -2 5 1.13 4.91 2.97 0.036 1.06 1 -2 4 63.18 49.40 2.93 0.116 2.03 1 2 1 36.43 26.86 2.88 0.085 2.51 0 -1 3 5.27 2.34 2.81 0.025 3.00 -5 -7 7 40.60 54.50 2.76 0.121 0.88 0 1 2 145.25 172.67 2.74 0.216 3.01 -1 4 1 82.25 67.01 2.73 0.135 1.67 3 0 8 0.43 4.33 2.72 0.034 0.85 5 2 1 48.32 37.17 2.71 0.100 1.15 0 -1 2 390.49 452.79 2.71 0.350 4.51 -1 -1 2 121.06 145.04 2.71 0.198 4.14 -5 -2 8 2.90 7.17 2.70 0.044 0.97 -6 -4 9 77.02 55.70 2.70 0.123 0.84 8 -4 2 1.20 8.07 2.68 0.047 0.79 3 -8 4 6.34 12.92 2.65 0.059 0.96 4 7 0 19.08 10.26 2.62 0.053 0.85 -3 8 1 6.43 12.10 2.60 0.057 0.86 -7 5 0 6.88 14.43 2.60 0.062 0.86 1 -4 2 61.35 49.26 2.58 0.115 2.01 2 4 6 13.01 0.91 2.58 0.016 0.83 4 -8 4 115.66 94.96 2.56 0.160 0.90 6 -3 5 4.05 0.82 2.56 0.015 0.89 1 1 1 396.78 455.16 2.56 0.351 3.45 1 0 0 5.98 3.05 2.52 0.029 6.79 -7 -2 3 9.45 3.52 2.52 0.031 0.97 2 6 2 9.69 18.44 2.49 0.071 0.96 2 -3 6 3.14 0.67 2.43 0.013 1.29 3 1 0 7.23 11.43 2.42 0.056 2.09 -6 -6 1 7.88 17.09 2.39 0.068 0.82 0 2 0 257.28 294.83 2.38 0.282 3.73 -1 -2 2 1118.15 1257.98 2.36 0.583 3.39 0 -1 5 212.10 184.01 2.35 0.223 1.75 1 -8 8 28.43 40.08 2.35 0.104 0.91 2 -9 9 3.20 9.15 2.35 0.050 0.78 2 0 5 10.78 15.97 2.34 0.066 1.34 Bond lengths and angles C33 - Distance Angles N32 1.2195 (0.0223) N34 1.4732 (0.0272) 109.32 (1.54) H33 0.9500 125.34 125.34 C33 - N32 N34 C35 - Distance Angles N34 1.2520 (0.0299) C31 1.3581 (0.0173) 109.00 (1.16) H35 0.9500 125.50 125.50 C35 - N34 C31 C31 - Distance Angles N32 1.2991 (0.0179) C35 1.3581 (0.0173) 108.67 (0.97) H31 0.9500 125.66 125.66 C31 - N32 C35 N32 - Distance Angles C33 1.2195 (0.0223) C31 1.2991 (0.0179) 108.32 (1.07) H32 0.8800 125.84 125.84 N32 - C33 C31 N34 - Distance Angles C35 1.2520 (0.0298) C33 1.4732 (0.0272) 102.01 (1.94) H34 0.9500 129.00 129.00 N34 - C35 C33 C43 - Distance Angles C44 1.3244 (0.0218) N42 1.3519 (0.0192) 106.61 (1.26) H43 0.9500 126.69 126.69 C43 - C44 N42 C44 - Distance Angles C43 1.3244 (0.0218) N45 1.4775 (0.0236) 109.37 (1.60) H44 0.9500 125.32 125.32 C44 - C43 N45 C41 - Distance Angles N45 1.3327 (0.0194) N42 1.4376 (0.0224) 106.47 (1.06) H41 0.9500 126.77 126.77 C41 - N45 N42 N42 - Distance Angles C43 1.3519 (0.0190) C41 1.4376 (0.0224) 110.46 (0.94) H42 0.8800 124.77 124.77 N42 - C43 C41 N45 - Distance Angles C41 1.3327 (0.0194) C44 1.4775 (0.0236) 105.61 (1.08) H45 0.9500 127.19 127.19 N45 - C41 C44 C1 - Distance Angles O1B 1.2567 (0.0018) O1A 1.2649 (0.0018) 122.23 (0.14) C2 1.5171 (0.0020) 119.77 (0.13) 118.00 (0.13) C1 - O1B O1A C2 - Distance Angles C1 1.5171 (0.0020) C3 1.5288 (0.0022) 112.29 (0.13) H2A 0.9900 109.15 109.15 H2B 0.9900 109.15 109.15 107.87 C2 - C1 C3 H2A C3 - Distance Angles O3A 1.2263 (0.0018) O3B 1.2900 (0.0020) 124.79 (0.15) C2 1.5288 (0.0022) 120.26 (0.14) 114.93 (0.13) C3 - O3A O3B C22 - Distance Angles N21 1.3275 (0.0020) N23 1.3292 (0.0020) 108.37 (0.14) H22 0.9500 125.81 125.81 C22 - N21 N23 C24 - Distance Angles C25 1.3507 (0.0022) N23 1.3774 (0.0020) 107.22 (0.14) H24 0.9500 126.39 126.39 C24 - C25 N23 C25 - Distance Angles C24 1.3507 (0.0022) N21 1.3792 (0.0020) 106.68 (0.13) H25 0.9500 126.66 126.66 C25 - C24 N21 N21 - Distance Angles C22 1.3275 (0.0020) C25 1.3792 (0.0020) 109.02 (0.13) H21 0.8800 125.49 125.49 N21 - C22 C25 N23 - Distance Angles C22 1.3292 (0.0020) C24 1.3774 (0.0020) 108.71 (0.13) H23 0.8800 125.64 125.64 N23 - C22 C24 O1A - Distance Angles C1 1.2649 (0.0018) O1A - O1B - Distance Angles C1 1.2567 (0.0018) O1B - O3A - Distance Angles C3 1.2263 (0.0018) O3A - O3B - Distance Angles C3 1.2900 (0.0020) H3B 1.2293 (0.0011) 111.48 (0.11) O3B - C3 Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.95 2.815(8) 169.2 N32-H32...O1A_$1 0.88 2.49 2.995(11) 117.4 N32-H32...O1B_$1 0.88 2.00 2.859(10) 164.1 N42-H42...O1A_$1 0.88 2.39 2.942(14) 121.5 N42-H42...O1B_$1 0.88 1.78 2.6607(17) 174.7 N21-H21...O1B_$2 0.88 1.80 2.6772(16) 174.5 N23-H23...O1A_$3 1.2293(11) 1.2293(11) 2.459(2) 180.000(1) O3B-H3B...O3B_$4 1.2293(11) 2.4445(12) 3.1623(17) 114.72(6) O3B-H3B...O3A_$4 FMAP and GRID set by program FMAP 2 1 22 GRID -2.632 -2 -2 2.632 2 2 R1 = 0.0627 for 2155 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.27 at 0.1896 0.2736 0.6286 [ 0.74 A from C1 ] Deepest hole -0.26 at 0.3047 0.3817 0.4605 [ 0.61 A from C3 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2770 / 16643 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8104 0.7264 1.3714 1.00000 0.05 0.27 0.74 C1 0.80 C2 1.49 H2B 1.51 H2A Q2 1 0.8264 0.6816 1.4751 1.00000 0.05 0.21 0.73 C2 0.82 C3 1.35 H2A 1.49 H2B Q3 1 1.2704 0.6641 1.3801 1.00000 0.05 0.18 1.23 H22 1.77 C22 2.25 H2B 2.31 N23 Q4 1 0.5501 0.5990 1.0873 1.00000 0.05 0.18 1.21 O1B 1.82 H35 2.02 H21 2.12 H45 Q5 1 0.7332 0.7001 1.1003 1.00000 0.05 0.17 0.75 O1B 1.28 H45 1.52 H35 1.79 C1 Shortest distances between peaks (including symmetry equivalents) 1 2 1.16 4 5 1.48 4 4 1.72 1 5 2.36 1 4 2.61 4 5 2.79 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.48: 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 0.61: Structure factors and derivatives 0.67: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.14: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008skc0001 finished at 09:52:35 Total CPU time: 2.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++