+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 16:02:51 on 13-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in Pbca CELL 0.71073 10.6683 10.8869 29.9190 90.000 90.000 90.000 ZERR 8.00 0.0003 0.0003 0.0008 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O UNIT 144 160 32 16 V = 3474.93 F(000) = 1376.0 Mu = 0.08 mm-1 Cell Wt = 2595.04 Rho = 1.240 MERG 2 ACTA BOND $H SHEL 7 0.84 FMAP 2 PLAN 10 SIZE 0.10 0.15 0.20 BOND WGHT 0.05450 0.32800 L.S. 18 TEMP -153.00 FVAR 0.18402 O2 4 0.150888 0.423702 0.027777 11.00000 0.03027 0.02756 = 0.02180 -0.00103 0.00259 0.00204 N2 3 0.158239 0.386301 -0.089575 11.00000 0.02210 0.02184 = 0.02208 0.00015 -0.00088 -0.00181 O1 4 0.192573 0.569311 -0.023173 11.00000 0.04507 0.02203 = 0.02908 -0.00092 0.00136 0.00315 N1 3 0.275321 0.355350 -0.154389 11.00000 0.02256 0.02448 = 0.02105 -0.00125 -0.00075 -0.00395 C16 1 0.179743 0.463008 -0.012831 11.00000 0.02002 0.02309 = 0.02258 0.00279 -0.00141 0.00148 N3 3 0.592018 0.386767 -0.123434 11.00000 0.02710 0.04731 = 0.03738 0.00403 0.00301 -0.00012 C8 1 0.415134 0.340194 -0.008495 11.00000 0.02358 0.02186 = 0.02576 0.00209 0.00191 0.00065 C10 1 0.350829 0.322607 -0.230411 11.00000 0.02193 0.03163 = 0.02268 -0.00076 0.00471 -0.00656 C3 1 0.106666 0.281404 -0.114717 11.00000 0.02296 0.02662 = 0.02780 -0.00499 -0.00026 -0.00393 AFIX 23 H3A 2 0.014090 0.278824 -0.112630 11.00000 -1.20000 H3B 2 0.141407 0.202649 -0.103754 11.00000 -1.20000 AFIX 0 C15 1 0.291917 0.331635 -0.271555 11.00000 0.03045 0.03462 = 0.02862 -0.00248 -0.00309 0.00386 AFIX 43 H15 2 0.238810 0.399723 -0.277536 11.00000 -1.20000 AFIX 0 C17 1 0.143860 0.517371 0.062668 11.00000 0.03211 0.03314 = 0.02346 -0.00823 -0.00250 0.00381 AFIX 23 H17A 2 0.075346 0.575999 0.056116 11.00000 -1.20000 H17B 2 0.223675 0.563531 0.064347 11.00000 -1.20000 AFIX 0 C2 1 0.263699 0.436074 -0.115824 11.00000 0.02147 0.01952 = 0.02427 -0.00096 -0.00142 0.00078 AFIX 13 H2 2 0.245489 0.522109 -0.125564 11.00000 -1.20000 AFIX 0 N4 3 0.468958 0.349788 0.024312 11.00000 0.03349 0.03033 = 0.03417 0.00243 -0.00656 0.00306 C14 1 0.309395 0.242782 -0.304065 11.00000 0.03406 0.04503 = 0.02944 -0.00989 -0.00385 -0.00137 AFIX 43 H14 2 0.268355 0.249986 -0.332122 11.00000 -1.20000 AFIX 0 C5 1 0.343117 0.333318 -0.050070 11.00000 0.02424 0.01873 = 0.02150 0.00040 -0.00150 0.00075 AFIX 13 H5 2 0.356124 0.250707 -0.063926 11.00000 -1.20000 AFIX 0 C4 1 0.200520 0.356333 -0.044582 11.00000 0.02307 0.02058 = 0.02346 -0.00041 -0.00006 -0.00094 AFIX 13 H4 2 0.157530 0.280764 -0.033357 11.00000 -1.20000 AFIX 0 C7 1 0.497907 0.407032 -0.106696 11.00000 0.02726 0.02667 = 0.02526 0.00247 -0.00344 -0.00402 C6 1 0.379048 0.433113 -0.084182 11.00000 0.02162 0.02066 = 0.02376 -0.00008 -0.00061 -0.00186 AFIX 13 H6 2 0.385736 0.513854 -0.068426 11.00000 -1.20000 AFIX 0 C11 1 0.430046 0.223809 -0.222575 11.00000 0.03365 0.04323 = 0.02461 0.00142 0.00190 0.00521 AFIX 43 H11 2 0.472684 0.217315 -0.194799 11.00000 -1.20000 AFIX 0 C9 1 0.327192 0.415874 -0.194145 11.00000 0.03250 0.02872 = 0.02075 0.00238 0.00098 -0.00501 AFIX 23 H9A 2 0.406695 0.457508 -0.186287 11.00000 -1.20000 H9B 2 0.267618 0.478807 -0.205065 11.00000 -1.20000 AFIX 0 C1 1 0.148730 0.307544 -0.161722 11.00000 0.02433 0.02819 = 0.02458 -0.00346 -0.00058 -0.00293 AFIX 23 H1A 2 0.150089 0.231873 -0.180066 11.00000 -1.20000 H1B 2 0.094298 0.369362 -0.176290 11.00000 -1.20000 AFIX 0 C13 1 0.386583 0.143697 -0.295626 11.00000 0.03457 0.03572 = 0.03199 -0.00713 0.00766 -0.00290 AFIX 43 H13 2 0.397871 0.081956 -0.317700 11.00000 -1.20000 AFIX 0 C12 1 0.447320 0.134571 -0.255026 11.00000 0.03960 0.03712 = 0.03584 0.00033 0.00883 0.01090 AFIX 43 H12 2 0.501163 0.066868 -0.249308 11.00000 -1.20000 AFIX 0 C18 1 0.119467 0.452856 0.105618 11.00000 0.06459 0.04836 = 0.02276 -0.00020 0.00324 0.01082 AFIX 137 H18A 2 0.038205 0.411093 0.104081 11.00000 -1.50000 H18B 2 0.118413 0.512703 0.130083 11.00000 -1.50000 H18C 2 0.185712 0.392265 0.110988 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for s92 in Pbca C 0.770 H 0.320 N 0.700 O 0.660 O2 - C16 C17 N2 - C4 C3 C2 O1 - C16 N1 - C2 C1 C9 C16 - O1 O2 C4 N3 - C7 C8 - N4 C5 C10 - C15 C11 C9 C3 - N2 C1 C15 - C14 C10 C17 - O2 C18 C2 - N1 N2 C6 N4 - C8 C14 - C13 C15 C5 - C8 C6 C4 C4 - N2 C16 C5 C7 - N3 C6 C6 - C7 C5 C2 C11 - C12 C10 C9 - N1 C10 C1 - N1 C3 C13 - C12 C14 C12 - C13 C11 C18 - C17 14673 Reflections read, of which 2867 rejected -9 =< h =< 12, -11 =< k =< 12, -33 =< l =< 35, Max. 2-theta = 50.05 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 6 2 5 27.42 0.87 4 6.67 5 6 5 41.94 0.92 6 10.23 2 Inconsistent equivalents 3047 Unique reflections, of which 0 suppressed R(int) = 0.0560 R(sigma) = 0.0637 Friedel opposites merged Maximum memory for data reduction = 2279 / 30319 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 = 2905 / 270098 wR2 = 0.1121 before cycle 1 for 3047 data and 218 / 218 parameters GooF = S = 0.987; Restrained GooF = 0.987 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18484 0.00040 2.055 OSF Mean shift/su = 0.440 Maximum = 2.055 for OSF Max. shift = 0.002 A for H18C Max. dU = 0.001 for C16 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2905 / 270098 wR2 = 0.1104 before cycle 2 for 3047 data and 218 / 218 parameters GooF = S = 0.967; Restrained GooF = 0.967 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18532 0.00039 1.237 OSF Mean shift/su = 0.161 Maximum = 1.237 for OSF Max. shift = 0.001 A for H18C Max. dU = 0.000 for C18 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2905 / 270098 wR2 = 0.1103 before cycle 3 for 3047 data and 218 / 218 parameters GooF = S = 0.966; Restrained GooF = 0.966 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18535 0.00039 0.070 OSF Mean shift/su = 0.009 Maximum = 0.070 for OSF Max. shift = 0.000 A for H18C Max. dU = 0.000 for C18 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2905 / 270098 wR2 = 0.1103 before cycle 4 for 3047 data and 218 / 218 parameters GooF = S = 0.966; Restrained GooF = 0.966 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18535 0.00039 0.004 OSF Mean shift/su = 0.002 Maximum = 0.023 for U11 C18 Max. shift = 0.000 A for C14 Max. dU = 0.000 for C18 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2905 / 270098 wR2 = 0.1103 before cycle 5 for 3047 data and 218 / 218 parameters GooF = S = 0.966; Restrained GooF = 0.966 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18535 0.00039 0.001 OSF Mean shift/su = 0.000 Maximum = -0.001 for y C18 Max. shift = 0.000 A for H18C Max. dU = 0.000 for C18 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2905 / 270098 wR2 = 0.1103 before cycle 6 for 3047 data and 218 / 218 parameters GooF = S = 0.966; Restrained GooF = 0.966 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18535 0.00039 0.001 OSF Mean shift/su = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for C15 Max. dU = 0.000 for C18 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2905 / 270098 wR2 = 0.1103 before cycle 7 for 3047 data and 218 / 218 parameters GooF = S = 0.966; Restrained GooF = 0.966 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18535 0.00039 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C14 Max. dU = 0.000 for C2 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2905 / 270098 wR2 = 0.1103 before cycle 8 for 3047 data and 218 / 218 parameters GooF = S = 0.966; Restrained GooF = 0.966 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18535 0.00039 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C12 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2905 / 270098 wR2 = 0.1103 before cycle 9 for 3047 data and 218 / 218 parameters GooF = S = 0.966; Restrained GooF = 0.966 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18535 0.00039 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C14 Max. dU = 0.000 for C2 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2905 / 270098 wR2 = 0.1103 before cycle 10 for 3047 data and 218 / 218 parameters GooF = S = 0.966; Restrained GooF = 0.966 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18535 0.00039 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C1 Least-squares cycle 11 Maximum vector length = 511 Memory required = 2905 / 270098 wR2 = 0.1103 before cycle 11 for 3047 data and 218 / 218 parameters GooF = S = 0.966; Restrained GooF = 0.966 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18535 0.00039 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C14 Max. shift = 0.000 A for C14 Max. dU = 0.000 for C7 Least-squares cycle 12 Maximum vector length = 511 Memory required = 2905 / 270098 wR2 = 0.1103 before cycle 12 for 3047 data and 218 / 218 parameters GooF = S = 0.966; Restrained GooF = 0.966 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18535 0.00039 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x N3 Max. shift = 0.000 A for H18B Max. dU = 0.000 for C3 Least-squares cycle 13 Maximum vector length = 511 Memory required = 2905 / 270098 wR2 = 0.1103 before cycle 13 for 3047 data and 218 / 218 parameters GooF = S = 0.966; Restrained GooF = 0.966 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18535 0.00039 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C14 Max. shift = 0.000 A for C14 Max. dU = 0.000 for C13 Least-squares cycle 14 Maximum vector length = 511 Memory required = 2905 / 270098 wR2 = 0.1103 before cycle 14 for 3047 data and 218 / 218 parameters GooF = S = 0.966; Restrained GooF = 0.966 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18535 0.00039 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C6 Least-squares cycle 15 Maximum vector length = 511 Memory required = 2905 / 270098 wR2 = 0.1103 before cycle 15 for 3047 data and 218 / 218 parameters GooF = S = 0.966; Restrained GooF = 0.966 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18535 0.00039 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C14 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C12 Least-squares cycle 16 Maximum vector length = 511 Memory required = 2905 / 270098 wR2 = 0.1103 before cycle 16 for 3047 data and 218 / 218 parameters GooF = S = 0.966; Restrained GooF = 0.966 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18535 0.00039 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C14 Max. shift = 0.000 A for C14 Max. dU = 0.000 for C18 Least-squares cycle 17 Maximum vector length = 511 Memory required = 2905 / 270098 wR2 = 0.1103 before cycle 17 for 3047 data and 218 / 218 parameters GooF = S = 0.966; Restrained GooF = 0.966 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18535 0.00039 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C9 Least-squares cycle 18 Maximum vector length = 511 Memory required = 2905 / 270098 wR2 = 0.1103 before cycle 18 for 3047 data and 218 / 218 parameters GooF = S = 0.966; Restrained GooF = 0.966 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.18535 0.00039 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C14 Max. shift = 0.000 A for C14 Max. dU = 0.000 for C10 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 19 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3A 0.0141 0.2790 -0.1127 23 0.990 0.000 C3 N2 C1 H3B 0.1413 0.2027 -0.1038 23 0.990 0.000 C3 N2 C1 H15 0.2386 0.3994 -0.2775 43 0.950 0.000 C15 C14 C10 H17A 0.0752 0.5760 0.0561 23 0.990 0.000 C17 O2 C18 H17B 0.2235 0.5636 0.0643 23 0.990 0.000 C17 O2 C18 H2 0.2455 0.5221 -0.1256 13 1.000 0.000 C2 N1 N2 C6 H14 0.2687 0.2501 -0.3321 43 0.950 0.000 C14 C13 C15 H5 0.3561 0.2508 -0.0639 13 1.000 0.000 C5 C8 C6 C4 H4 0.1576 0.2809 -0.0333 13 1.000 0.000 C4 N2 C16 C5 H6 0.3859 0.5138 -0.0685 13 1.000 0.000 C6 C7 C5 C2 H11 0.4724 0.2171 -0.1948 43 0.950 0.000 C11 C12 C10 H9A 0.4070 0.4574 -0.1862 23 0.990 0.000 C9 N1 C10 H9B 0.2680 0.4790 -0.2050 23 0.990 0.000 C9 N1 C10 H1A 0.1505 0.2319 -0.1800 23 0.990 0.000 C1 N1 C3 H1B 0.0946 0.3694 -0.1763 23 0.990 0.000 C1 N1 C3 H13 0.3978 0.0820 -0.3177 43 0.950 0.000 C13 C12 C14 H12 0.5010 0.0670 -0.2493 43 0.950 0.000 C12 C13 C11 H18A 0.0380 0.4112 0.1041 137 0.980 0.000 C18 C17 H18A H18B 0.1186 0.5126 0.1301 137 0.980 0.000 C18 C17 H18A H18C 0.1855 0.3920 0.1110 137 0.980 0.000 C18 C17 H18A s92 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O2 0.15087 0.42379 0.02778 1.00000 0.03121 0.02850 0.02244 -0.00159 0.00311 0.00163 0.02738 0.00216 0.00012 0.00011 0.00004 0.00000 0.00075 0.00071 0.00075 0.00059 0.00058 0.00060 0.00033 N2 0.15828 0.38625 -0.08953 1.00000 0.02231 0.02349 0.02238 -0.00002 -0.00084 -0.00283 0.02273 0.00251 0.00014 0.00013 0.00005 0.00000 0.00082 0.00084 0.00087 0.00069 0.00066 0.00068 0.00038 O1 0.19262 0.56952 -0.02320 1.00000 0.04694 0.02237 0.03044 -0.00044 0.00190 0.00248 0.03325 0.00230 0.00013 0.00011 0.00004 0.00000 0.00090 0.00073 0.00081 0.00063 0.00067 0.00065 0.00036 N1 0.27535 0.35538 -0.15435 1.00000 0.02348 0.02492 0.02170 -0.00113 0.00002 -0.00465 0.02337 0.00255 0.00014 0.00013 0.00005 0.00000 0.00083 0.00082 0.00087 0.00070 0.00067 0.00071 0.00038 C16 0.17974 0.46304 -0.01285 1.00000 0.02032 0.02513 0.02452 0.00224 -0.00137 0.00169 0.02332 0.00314 0.00017 0.00017 0.00006 0.00000 0.00099 0.00109 0.00114 0.00086 0.00084 0.00084 0.00044 N3 0.59197 0.38690 -0.12344 1.00000 0.02897 0.04828 0.03817 0.00424 0.00250 -0.00038 0.03847 0.00315 0.00017 0.00017 0.00006 0.00000 0.00107 0.00113 0.00108 0.00086 0.00086 0.00089 0.00046 C8 0.41511 0.34014 -0.00853 1.00000 0.02457 0.02145 0.02791 0.00135 0.00216 0.00100 0.02465 0.00349 0.00018 0.00016 0.00007 0.00000 0.00103 0.00103 0.00118 0.00086 0.00096 0.00084 0.00045 C10 0.35083 0.32274 -0.23037 1.00000 0.02262 0.03160 0.02275 0.00046 0.00396 -0.00558 0.02566 0.00320 0.00017 0.00017 0.00006 0.00000 0.00103 0.00110 0.00109 0.00086 0.00086 0.00088 0.00046 C3 0.10671 0.28150 -0.11474 1.00000 0.02343 0.02688 0.02944 -0.00489 0.00036 -0.00423 0.02658 0.00310 0.00018 0.00017 0.00006 0.00000 0.00102 0.00106 0.00113 0.00088 0.00086 0.00086 0.00047 H3A 0.01412 0.27904 -0.11271 1.00000 0.03190 0.00000 0.00000 H3B 0.14128 0.20268 -0.10376 1.00000 0.03190 0.00000 0.00000 C15 0.29190 0.33148 -0.27150 1.00000 0.03140 0.03457 0.03160 -0.00306 -0.00327 0.00393 0.03252 0.00342 0.00019 0.00018 0.00007 0.00000 0.00115 0.00118 0.00126 0.00094 0.00096 0.00096 0.00051 H15 0.23856 0.39940 -0.27747 1.00000 0.03903 0.00000 0.00000 C17 0.14375 0.51738 0.06265 1.00000 0.03239 0.03403 0.02349 -0.00807 -0.00104 0.00368 0.02997 0.00333 0.00019 0.00018 0.00006 0.00000 0.00116 0.00109 0.00110 0.00092 0.00089 0.00093 0.00048 H17A 0.07518 0.57595 0.05610 1.00000 0.03596 0.00000 0.00000 H17B 0.22352 0.56361 0.06433 1.00000 0.03596 0.00000 0.00000 C2 0.26374 0.43608 -0.11583 1.00000 0.02266 0.02075 0.02426 -0.00050 -0.00094 0.00072 0.02256 0.00309 0.00017 0.00017 0.00006 0.00000 0.00097 0.00093 0.00107 0.00083 0.00082 0.00082 0.00044 H2 0.24554 0.52212 -0.12557 1.00000 0.02707 0.00000 0.00000 N4 0.46893 0.34982 0.02434 1.00000 0.03373 0.03145 0.03544 0.00316 -0.00590 0.00282 0.03354 0.00312 0.00016 0.00015 0.00006 0.00000 0.00099 0.00096 0.00111 0.00081 0.00088 0.00080 0.00043 C14 0.30952 0.24275 -0.30405 1.00000 0.03417 0.04461 0.03044 -0.00892 -0.00349 -0.00162 0.03640 0.00350 0.00020 0.00019 0.00007 0.00000 0.00123 0.00127 0.00122 0.00100 0.00095 0.00110 0.00054 H14 0.26866 0.25006 -0.33214 1.00000 0.04369 0.00000 0.00000 C5 0.34318 0.33342 -0.05005 1.00000 0.02449 0.01998 0.02173 0.00057 -0.00173 0.00046 0.02207 0.00308 0.00017 0.00016 0.00006 0.00000 0.00099 0.00094 0.00103 0.00078 0.00081 0.00082 0.00043 H5 0.35612 0.25080 -0.06390 1.00000 0.02648 0.00000 0.00000 C4 0.20059 0.35643 -0.04459 1.00000 0.02354 0.02121 0.02380 0.00010 0.00019 -0.00041 0.02285 0.00309 0.00017 0.00017 0.00006 0.00000 0.00100 0.00095 0.00109 0.00080 0.00083 0.00081 0.00044 H4 0.15764 0.28085 -0.03335 1.00000 0.02742 0.00000 0.00000 C7 0.49775 0.40694 -0.10670 1.00000 0.02733 0.02813 0.02583 0.00281 -0.00307 -0.00457 0.02710 0.00321 0.00019 0.00017 0.00007 0.00000 0.00118 0.00107 0.00112 0.00086 0.00094 0.00093 0.00047 C6 0.37913 0.43303 -0.08418 1.00000 0.02337 0.02063 0.02484 -0.00028 -0.00015 -0.00153 0.02295 0.00316 0.00017 0.00016 0.00006 0.00000 0.00100 0.00094 0.00104 0.00082 0.00083 0.00082 0.00044 H6 0.38590 0.51379 -0.06845 1.00000 0.02754 0.00000 0.00000 C11 0.42988 0.22373 -0.22261 1.00000 0.03435 0.04402 0.02525 0.00081 0.00108 0.00550 0.03454 0.00369 0.00020 0.00019 0.00007 0.00000 0.00118 0.00131 0.00114 0.00100 0.00091 0.00105 0.00052 H11 0.47244 0.21706 -0.19483 1.00000 0.04145 0.00000 0.00000 C9 0.32740 0.41593 -0.19411 1.00000 0.03440 0.02853 0.02141 0.00249 0.00160 -0.00531 0.02811 0.00334 0.00020 0.00017 0.00006 0.00000 0.00115 0.00104 0.00110 0.00085 0.00087 0.00093 0.00048 H9A 0.40700 0.45738 -0.18623 1.00000 0.03373 0.00000 0.00000 H9B 0.26797 0.47901 -0.20501 1.00000 0.03373 0.00000 0.00000 C1 0.14903 0.30759 -0.16172 1.00000 0.02541 0.02829 0.02659 -0.00317 -0.00099 -0.00304 0.02676 0.00320 0.00018 0.00018 0.00006 0.00000 0.00102 0.00103 0.00112 0.00088 0.00086 0.00088 0.00046 H1A 0.15049 0.23189 -0.18004 1.00000 0.03211 0.00000 0.00000 H1B 0.09464 0.36937 -0.17633 1.00000 0.03211 0.00000 0.00000 C13 0.38651 0.14378 -0.29559 1.00000 0.03473 0.03614 0.03379 -0.00729 0.00755 -0.00302 0.03488 0.00366 0.00019 0.00019 0.00007 0.00000 0.00122 0.00120 0.00126 0.00098 0.00102 0.00105 0.00053 H13 0.39776 0.08200 -0.31765 1.00000 0.04186 0.00000 0.00000 C12 0.44716 0.13465 -0.25504 1.00000 0.04120 0.03848 0.03614 0.00070 0.00945 0.01039 0.03861 0.00398 0.00021 0.00020 0.00007 0.00000 0.00133 0.00120 0.00136 0.00104 0.00104 0.00105 0.00056 H12 0.50102 0.06696 -0.24933 1.00000 0.04633 0.00000 0.00000 C18 0.11937 0.45277 0.10565 1.00000 0.06380 0.05099 0.02491 -0.00145 0.00331 0.01115 0.04657 0.00430 0.00025 0.00022 0.00007 0.00000 0.00161 0.00145 0.00120 0.00107 0.00113 0.00124 0.00062 H18A 0.03800 0.41120 0.10415 1.00000 0.06985 0.00000 0.00000 H18B 0.11857 0.51258 0.13013 1.00000 0.06985 0.00000 0.00000 H18C 0.18549 0.39202 0.11097 1.00000 0.06985 0.00000 0.00000 Final Structure Factor Calculation for s92 in Pbca Total number of l.s. parameters = 218 Maximum vector length = 511 Memory required = 2687 / 22995 wR2 = 0.1103 before cycle 19 for 3047 data and 0 / 218 parameters GooF = S = 0.966; Restrained GooF = 0.966 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0452 for 2027 Fo > 4sig(Fo) and 0.0844 for all 3047 data wR2 = 0.1103, GooF = S = 0.966, Restrained GooF = 0.966 for all data Occupancy sum of asymmetric unit = 24.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0325 0.0287 0.0209 O2 0.0259 0.0225 0.0198 N2 0.0474 0.0303 0.0221 O1 0.0290 0.0218 0.0193 N1 0.0271 0.0239 0.0190 C16 0.0498 0.0374 0.0282 N3 0.0293 0.0235 0.0211 C8 0.0344 0.0252 0.0173 C10 0.0341 0.0259 0.0198 C3 0.0396 0.0299 0.0281 C15 0.0402 0.0307 0.0191 C17 0.0248 0.0223 0.0205 C2 0.0406 0.0344 0.0256 N4 0.0489 0.0357 0.0246 C14 0.0253 0.0213 0.0196 C5 0.0239 0.0235 0.0211 C4 0.0343 0.0239 0.0230 C7 0.0249 0.0241 0.0199 C6 0.0466 0.0319 0.0251 C11 0.0375 0.0270 0.0198 C9 0.0314 0.0270 0.0219 C1 0.0469 0.0325 0.0253 C13 0.0538 0.0365 0.0255 C12 0.0704 0.0450 0.0244 C18 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.018 0.029 0.039 0.051 0.066 0.086 0.112 0.164 1.000 Number in group 320. 292. 337. 269. 311. 307. 307. 295. 303. 306. GooF 0.793 0.845 0.929 1.012 1.017 0.957 1.083 1.024 0.904 1.064 K 2.371 0.853 0.971 0.945 0.973 1.003 1.007 0.994 1.010 0.994 Resolution(A) 0.84 0.87 0.90 0.95 1.00 1.06 1.14 1.25 1.43 1.78 inf Number in group 307. 305. 307. 304. 299. 310. 306. 301. 304. 304. GooF 0.946 0.912 0.929 0.918 1.020 0.912 0.916 0.937 0.988 1.156 K 1.086 1.064 1.002 0.986 1.004 1.028 1.006 1.025 1.047 0.968 R1 0.270 0.199 0.166 0.126 0.083 0.061 0.056 0.053 0.043 0.036 Recommended weighting scheme: WGHT 0.0518 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)/su Fc/Fc(max) Resolution(A) 1 1 4 424.22 539.31 3.81 0.105 5.34 1 8 20 224.22 321.74 3.62 0.081 1.00 3 1 12 147.23 100.11 3.40 0.045 2.01 2 1 1 704.02 959.77 3.24 0.140 4.73 5 6 20 73.59 1.78 3.18 0.006 1.02 3 4 7 675.97 559.77 3.17 0.107 1.93 6 2 1 908.09 759.65 3.10 0.124 1.69 5 1 4 309.23 246.05 3.09 0.071 2.02 5 10 8 7.36 78.11 3.09 0.040 0.94 2 1 3 4137.96 4919.50 3.09 0.317 4.32 10 1 4 159.22 214.05 3.06 0.066 1.05 2 7 23 282.69 376.12 3.06 0.088 0.98 2 11 9 12.59 60.67 3.05 0.035 0.93 4 6 21 203.55 267.39 3.04 0.074 1.03 4 5 24 103.25 148.46 2.95 0.055 1.00 8 10 0 58.51 221.63 2.94 0.067 0.84 5 4 30 440.32 311.09 2.88 0.080 0.86 2 0 12 754.46 623.28 2.87 0.113 2.26 4 5 12 5.95 42.12 2.85 0.029 1.40 0 4 2 1222.76 1037.05 2.84 0.145 2.68 5 1 29 341.54 241.78 2.79 0.070 0.93 0 12 12 295.44 142.25 2.72 0.054 0.85 3 5 4 665.64 567.00 2.71 0.107 1.80 0 6 10 12438.43 10641.88 2.69 0.466 1.55 1 4 11 4074.31 3510.40 2.68 0.267 1.89 2 6 15 106.83 144.75 2.66 0.054 1.30 3 8 4 67.35 36.58 2.65 0.027 1.25 4 2 32 88.34 161.44 2.65 0.057 0.87 2 3 7 442.31 521.93 2.63 0.103 2.46 11 4 7 280.52 190.80 2.59 0.062 0.89 0 0 18 210.28 134.48 2.59 0.052 1.66 1 2 4 3964.38 4562.94 2.58 0.305 4.07 10 4 0 58.94 8.25 2.58 0.013 0.99 1 8 16 42.24 95.44 2.56 0.044 1.09 3 4 21 125.35 80.82 2.56 0.041 1.19 4 10 0 414.45 302.88 2.56 0.079 1.01 6 2 14 91.64 131.70 2.55 0.052 1.33 7 9 8 0.00 49.97 2.55 0.032 0.92 2 0 2 475.32 575.21 2.55 0.108 5.02 7 9 14 9.80 72.97 2.54 0.039 0.87 1 0 8 6427.35 7406.71 2.53 0.389 3.53 7 10 9 256.50 137.59 2.53 0.053 0.86 7 1 22 156.26 214.28 2.48 0.066 1.01 12 2 0 -29.40 38.80 2.48 0.028 0.88 2 1 6 228.37 280.11 2.47 0.076 3.45 1 6 21 471.37 573.62 2.47 0.108 1.11 8 7 4 19.60 59.98 2.47 0.035 1.00 6 8 8 127.98 74.25 2.46 0.039 1.04 11 6 4 124.44 76.19 2.46 0.039 0.85 0 0 6 1828.85 2160.81 2.46 0.210 4.99 Bond lengths and angles O2 - Distance Angles C16 1.3249 (0.0022) C17 1.4602 (0.0021) 116.27 (0.14) O2 - C16 N2 - Distance Angles C4 1.4551 (0.0024) C3 1.4738 (0.0023) 114.58 (0.14) C2 1.4762 (0.0023) 109.77 (0.14) 107.22 (0.14) N2 - C4 C3 O1 - Distance Angles C16 1.2077 (0.0021) O1 - N1 - Distance Angles C2 1.4544 (0.0023) C1 1.4613 (0.0024) 104.83 (0.14) C9 1.4691 (0.0024) 113.75 (0.14) 112.72 (0.15) N1 - C2 C1 C16 - Distance Angles O1 1.2077 (0.0021) O2 1.3249 (0.0022) 124.84 (0.17) C4 1.5160 (0.0026) 123.89 (0.17) 111.22 (0.15) C16 - O1 O2 N3 - Distance Angles C7 1.1441 (0.0025) N3 - C8 - Distance Angles N4 1.1436 (0.0024) C5 1.4620 (0.0028) 177.19 (0.20) C8 - N4 C10 - Distance Angles C15 1.3850 (0.0027) C11 1.3881 (0.0028) 118.53 (0.18) C9 1.5063 (0.0026) 121.22 (0.18) 120.22 (0.17) C10 - C15 C11 C3 - Distance Angles N2 1.4738 (0.0023) C1 1.5034 (0.0027) 102.72 (0.14) H3A 0.9900 111.22 111.22 H3B 0.9900 111.22 111.22 109.14 C3 - N2 C1 H3A C15 - Distance Angles C14 1.3845 (0.0027) C10 1.3850 (0.0027) 121.02 (0.19) H15 0.9500 119.49 119.49 C15 - C14 C10 C17 - Distance Angles O2 1.4602 (0.0021) C18 1.4891 (0.0029) 107.26 (0.16) H17A 0.9900 110.26 110.26 H17B 0.9900 110.26 110.26 108.53 C17 - O2 C18 H17A C2 - Distance Angles N1 1.4544 (0.0023) N2 1.4762 (0.0023) 105.38 (0.14) C6 1.5534 (0.0026) 113.74 (0.14) 105.74 (0.14) H2 1.0000 110.58 110.58 110.58 C2 - N1 N2 C6 N4 - Distance Angles C8 1.1436 (0.0024) N4 - C14 - Distance Angles C13 1.3783 (0.0029) C15 1.3845 (0.0027) 119.81 (0.19) H14 0.9500 120.09 120.09 C14 - C13 C15 C5 - Distance Angles C8 1.4620 (0.0028) C6 1.5381 (0.0025) 113.45 (0.15) C4 1.5503 (0.0025) 114.67 (0.15) 101.59 (0.14) H5 1.0000 108.94 108.94 108.94 C5 - C8 C6 C4 C4 - Distance Angles N2 1.4551 (0.0024) C16 1.5160 (0.0026) 111.25 (0.15) C5 1.5503 (0.0025) 104.06 (0.14) 109.49 (0.14) H4 1.0000 110.62 110.62 110.62 C4 - N2 C16 C5 C7 - Distance Angles N3 1.1441 (0.0025) C6 1.4614 (0.0027) 178.47 (0.21) C7 - N3 C6 - Distance Angles C7 1.4614 (0.0027) C5 1.5381 (0.0025) 112.65 (0.15) C2 1.5534 (0.0026) 114.17 (0.15) 102.83 (0.14) H6 1.0000 108.99 108.99 108.99 C6 - C7 C5 C2 C11 - Distance Angles C12 1.3841 (0.0029) C10 1.3881 (0.0028) 120.51 (0.19) H11 0.9500 119.74 119.74 C11 - C12 C10 C9 - Distance Angles N1 1.4691 (0.0024) C10 1.5063 (0.0026) 110.11 (0.15) H9A 0.9900 109.64 109.64 H9B 0.9900 109.64 109.64 108.15 C9 - N1 C10 H9A C1 - Distance Angles N1 1.4613 (0.0024) C3 1.5034 (0.0027) 101.72 (0.15) H1A 0.9900 111.43 111.43 H1B 0.9900 111.43 111.43 109.28 C1 - N1 C3 H1A C13 - Distance Angles C12 1.3785 (0.0030) C14 1.3783 (0.0029) 119.85 (0.19) H13 0.9500 120.08 120.08 C13 - C12 C14 C12 - Distance Angles C13 1.3785 (0.0030) C11 1.3841 (0.0029) 120.26 (0.20) H12 0.9500 119.87 119.87 C12 - C13 C11 C18 - Distance Angles C17 1.4891 (0.0029) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C17 H18A H18B FMAP and GRID set by program FMAP 2 1 14 GRID -2.273 -2 -1 2.273 2 1 R1 = 0.0843 for 3047 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.16 at 0.0267 0.1348 0.2281 [ 1.86 A from C11 ] Deepest hole -0.26 at 0.1475 0.5003 0.0072 [ 0.80 A from C16 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3201 / 28159 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5267 0.3652 -0.2281 1.00000 0.05 0.16 1.86 C11 1.93 C10 1.98 H11 2.05 H9A Q2 1 0.0738 0.6283 0.0202 1.00000 0.05 0.15 1.21 H17A 1.90 C17 1.93 O1 2.19 H17B Q3 1 -0.1190 0.3736 0.1002 1.00000 0.05 0.15 1.73 H18A 1.76 H5 1.92 H2 2.51 O1 Q4 1 0.4476 0.2454 0.0501 1.00000 0.05 0.15 1.39 N4 1.87 H17A 2.02 H3A 2.06 C8 Q5 1 0.1220 0.4993 -0.1441 1.00000 0.05 0.14 1.45 H2 1.74 H1B 1.86 C2 2.08 N2 Q6 1 0.4350 0.4054 -0.0980 1.00000 0.05 0.14 0.72 C7 0.79 C6 1.57 H6 1.85 N3 Q7 1 0.2355 0.6647 0.0090 1.00000 0.05 0.14 1.49 O1 1.99 H17B 2.12 H4 2.37 C16 Q8 1 0.1817 0.2986 -0.0333 1.00000 0.05 0.14 0.32 H4 0.74 C4 1.83 C5 1.89 C16 Q9 1 0.1152 0.4575 -0.0909 1.00000 0.05 0.14 0.90 N2 1.77 C2 1.87 H2 1.99 C4 Q10 1 -0.1074 0.3617 0.1400 1.00000 0.05 0.14 1.96 H18A 1.99 H2 2.04 H11 2.62 H5 Shortest distances between peaks (including symmetry equivalents) 3 10 1.20 5 10 1.53 2 4 1.57 5 9 1.66 2 7 1.80 3 9 1.86 3 5 1.91 7 8 2.12 9 10 2.46 4 7 2.47 8 9 2.54 4 8 2.59 2 8 2.87 Time profile in seconds ----------------------- 0.02: 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. 0.55: 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 3.02: Structure factors and derivatives 3.05: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.48: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 16:02:59 Total CPU time: 7.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++