+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04src0995 started at 14:18:47 on 10-Nov-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04src0995 in P2(1)/n CELL 0.71073 10.8714 10.9150 13.5740 90.000 111.897 90.000 ZERR 4.00 0.0017 0.0008 0.0026 0.000 0.015 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H O UNIT 72 88 8 V = 1494.51 F(000) = 584.0 Mu = 0.08 mm-1 Cell Wt = 1081.42 Rho = 1.202 MERG 2 OMIT -3.00 55.00 OMIT 2 0 0 OMIT 0 2 2 OMIT 1 2 1 OMIT 1 2 0 OMIT 0 5 2 SHEL 7 0.77 EQIV $1 X-1, Y, Z EQIV $2 -X, -Y+1, -Z HTAB O5 O11_$1 HTAB O11 O5_$2 FMAP 2 PLAN 5 SIZE 0.18 0.22 0.26 ACTA BOND $H WGHT 0.03560 0.74840 L.S. 20 TEMP -153.00 FVAR 1.21995 C1 1 0.148159 0.496547 0.370848 11.00000 0.01504 0.01765 = 0.01502 0.00125 0.00643 0.00182 C2 1 0.003786 0.461909 0.304088 11.00000 0.01739 0.01911 = 0.01440 0.00150 0.00802 -0.00031 C3 1 -0.020132 0.352880 0.245720 11.00000 0.01888 0.02105 = 0.02194 -0.00130 0.00953 0.00239 AFIX 43 H3 2 0.052481 0.301062 0.251588 11.00000 -1.20000 AFIX 0 C4 1 -0.146310 0.318446 0.179811 11.00000 0.02316 0.02123 = 0.02093 -0.00440 0.01030 -0.00184 AFIX 43 H4 2 -0.159973 0.243918 0.141037 11.00000 -1.20000 AFIX 0 C5 1 -0.252843 0.393543 0.170714 11.00000 0.01741 0.02360 = 0.01582 0.00041 0.00760 -0.00331 C6 1 -0.233200 0.499849 0.230037 11.00000 0.01647 0.02214 = 0.01957 0.00131 0.00930 0.00217 AFIX 43 H6 2 -0.306603 0.549685 0.225911 11.00000 -1.20000 AFIX 0 C7 1 -0.105200 0.533562 0.295925 11.00000 0.01936 0.01774 = 0.01715 0.00027 0.00901 0.00011 AFIX 43 H7 2 -0.092240 0.607032 0.336061 11.00000 -1.20000 AFIX 0 C8 1 0.225388 0.498965 0.296590 11.00000 0.01534 0.01644 = 0.01543 -0.00096 0.00583 -0.00063 C9 1 0.347807 0.442589 0.320326 11.00000 0.01826 0.02213 = 0.01668 0.00309 0.00554 0.00384 AFIX 43 H9 2 0.384251 0.395492 0.383465 11.00000 -1.20000 AFIX 0 C10 1 0.418081 0.453728 0.253481 11.00000 0.01493 0.02853 = 0.02000 0.00155 0.00585 0.00503 AFIX 43 H10 2 0.502187 0.415540 0.271607 11.00000 -1.20000 AFIX 0 C11 1 0.365062 0.520486 0.160753 11.00000 0.01690 0.02325 = 0.01805 -0.00269 0.00873 -0.00277 C12 1 0.241514 0.574730 0.133303 11.00000 0.01777 0.02028 = 0.01642 0.00294 0.00490 0.00040 AFIX 43 H12 2 0.203727 0.618730 0.068558 11.00000 -1.20000 AFIX 0 C13 1 0.173814 0.564015 0.201394 11.00000 0.01471 0.01933 = 0.01866 0.00173 0.00574 0.00316 AFIX 43 H13 2 0.089603 0.602143 0.182726 11.00000 -1.20000 AFIX 0 C14 1 0.201535 0.399116 0.458362 11.00000 0.02309 0.02032 = 0.01818 0.00336 0.00900 0.00212 AFIX 137 H14A 2 0.198552 0.318474 0.425808 11.00000 -1.50000 H14B 2 0.146774 0.397960 0.501633 11.00000 -1.50000 H14C 2 0.293297 0.418823 0.503416 11.00000 -1.50000 AFIX 0 C15 1 0.155708 0.623584 0.423465 11.00000 0.01793 0.01925 = 0.01703 -0.00077 0.00745 0.00088 AFIX 23 H15A 2 0.115201 0.684260 0.366279 11.00000 -1.20000 H15B 2 0.099875 0.620648 0.466724 11.00000 -1.20000 AFIX 0 C16 1 0.293193 0.672009 0.494574 11.00000 0.02004 0.02029 = 0.01920 -0.00014 0.00370 -0.00020 AFIX 13 H16 2 0.347314 0.601239 0.534644 11.00000 -1.20000 AFIX 0 C17 1 0.276572 0.762007 0.574528 11.00000 0.03474 0.03312 = 0.02410 -0.00930 0.01017 -0.00797 AFIX 137 H17A 2 0.363751 0.792544 0.620876 11.00000 -1.50000 H17B 2 0.234026 0.720492 0.617483 11.00000 -1.50000 H17C 2 0.221249 0.830869 0.536646 11.00000 -1.50000 AFIX 0 C18 1 0.368839 0.734341 0.433360 11.00000 0.02343 0.02637 = 0.03012 -0.00389 0.01012 -0.00515 AFIX 137 H18A 2 0.314702 0.800605 0.389717 11.00000 -1.50000 H18B 2 0.388196 0.674190 0.387509 11.00000 -1.50000 H18C 2 0.452088 0.768167 0.483631 11.00000 -1.50000 AFIX 0 O5 3 -0.376098 0.358904 0.098803 11.00000 0.01632 0.02988 = 0.02191 -0.00418 0.00625 -0.00200 AFIX 147 H5 2 -0.433864 0.407917 0.102370 11.00000 -1.50000 AFIX 0 O11 3 0.438620 0.528441 0.097385 11.00000 0.01933 0.03796 = 0.02114 0.00570 0.01190 0.00407 AFIX 147 H11 2 0.399653 0.574387 0.045422 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 04src0995 in P2(1)/n C 0.770 H 0.320 O 0.660 C1 - C8 C14 C2 C15 C2 - C7 C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C6 O5 C4 C6 - C5 C7 C7 - C2 C6 C8 - C9 C13 C1 C9 - C8 C10 C10 - C11 C9 C11 - O11 C10 C12 C12 - C13 C11 C13 - C12 C8 C14 - C1 C15 - C16 C1 C16 - C17 C18 C15 C17 - C16 C18 - C16 O5 - C5 O11 - C11 Operators for generating equivalent atoms: $1 x-1, y, z $2 -x, -y+1, -z h k l Fo^2 Sigma Why rejected 5 0 0 19.24 4.55 observed but should be systematically absent 5 0 0 24.28 5.57 observed but should be systematically absent 7 0 0 120.68 27.53 observed but should be systematically absent 7 0 0 72.31 15.55 observed but should be systematically absent 0 5 0 51.65 9.12 observed but should be systematically absent 0 5 0 42.52 5.96 observed but should be systematically absent 0 0 7 43.57 10.86 observed but should be systematically absent 15874 Reflections read, of which 554 rejected -10 =< h =< 14, -13 =< k =< 14, -17 =< l =< 17, Max. 2-theta = 54.97 7 Systematic absence violations 0 Inconsistent equivalents 3404 Unique reflections, of which 0 suppressed R(int) = 0.0329 R(sigma) = 0.0291 Friedel opposites merged Maximum memory for data reduction = 2216 / 34468 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 = 2759 / 229828 wR2 = 0.1016 before cycle 1 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 -0.002 OSF Mean shift/esd = 0.003 Maximum = -0.009 for U33 O5 Max. shift = 0.000 A for H17C Max. dU = 0.000 for C3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1016 before cycle 2 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.003 for U33 O5 Max. shift = 0.000 A for H17C Max. dU = 0.000 for C3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1017 before cycle 3 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U33 C11 Max. shift = 0.000 A for H17C Max. dU = 0.000 for C3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1016 before cycle 4 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H17A Max. dU = 0.000 for C4 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1017 before cycle 5 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C17 Max. shift = 0.000 A for H14B Max. dU = 0.000 for O11 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1017 before cycle 6 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C17 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C11 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1017 before cycle 7 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C17 Max. shift = 0.000 A for H14A Max. dU = 0.000 for C17 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1017 before cycle 8 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C17 Max. shift = 0.000 A for H11 Max. dU = 0.000 for C4 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1017 before cycle 9 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C17 Max. shift = 0.000 A for O5 Max. dU = 0.000 for C8 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1017 before cycle 10 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C17 Max. shift = 0.000 A for H11 Max. dU = 0.000 for C18 Least-squares cycle 11 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1017 before cycle 11 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C17 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C18 Least-squares cycle 12 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1017 before cycle 12 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C17 Max. shift = 0.000 A for H14B Max. dU = 0.000 for C14 Least-squares cycle 13 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1017 before cycle 13 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C17 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C11 Least-squares cycle 14 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1017 before cycle 14 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C17 Max. shift = 0.000 A for H14B Max. dU = 0.000 for C4 Least-squares cycle 15 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1017 before cycle 15 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C17 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C9 Least-squares cycle 16 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1017 before cycle 16 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C17 Max. shift = 0.000 A for H11 Max. dU = 0.000 for C6 Least-squares cycle 17 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1017 before cycle 17 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C17 Max. shift = 0.000 A for H11 Max. dU = 0.000 for C3 Least-squares cycle 18 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1017 before cycle 18 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C17 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C18 Least-squares cycle 19 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1017 before cycle 19 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H14B Max. dU = 0.000 for C17 Least-squares cycle 20 Maximum vector length = 511 Memory required = 2759 / 229828 wR2 = 0.1017 before cycle 20 for 3404 data and 186 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.21995 0.00220 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C17 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C17 Largest correlation matrix elements 0.543 U13 O11 / U33 O11 0.503 U13 C2 / U33 C2 0.526 U13 O11 / U11 O11 0.502 U13 C5 / U33 C5 Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.0525 0.3011 0.2516 43 0.950 0.000 C3 C4 C2 H4 -0.1600 0.2439 0.1410 43 0.950 0.000 C4 C3 C5 H6 -0.3066 0.5497 0.2259 43 0.950 0.000 C6 C5 C7 H7 -0.0922 0.6070 0.3361 43 0.950 0.000 C7 C2 C6 H9 0.3843 0.3955 0.3835 43 0.950 0.000 C9 C8 C10 H10 0.5022 0.4155 0.2716 43 0.950 0.000 C10 C11 C9 H12 0.2037 0.6187 0.0686 43 0.950 0.000 C12 C13 C11 H13 0.0896 0.6021 0.1827 43 0.950 0.000 C13 C12 C8 H14A 0.1986 0.3185 0.4258 137 0.980 0.000 C14 C1 H14A H14B 0.1468 0.3980 0.5016 137 0.980 0.000 C14 C1 H14A H14C 0.2933 0.4188 0.5034 137 0.980 0.000 C14 C1 H14A H15A 0.1152 0.6843 0.3663 23 0.990 0.000 C15 C16 C1 H15B 0.0999 0.6206 0.4667 23 0.990 0.000 C15 C16 C1 H16 0.3473 0.6012 0.5346 13 1.000 0.000 C16 C17 C18 C15 H17A 0.3638 0.7925 0.6209 137 0.980 0.000 C17 C16 H17A H17B 0.2340 0.7205 0.6175 137 0.980 0.000 C17 C16 H17A H17C 0.2212 0.8309 0.5366 137 0.980 0.000 C17 C16 H17A H18A 0.3147 0.8006 0.3897 137 0.980 0.000 C18 C16 H18A H18B 0.3882 0.6742 0.3875 137 0.980 0.000 C18 C16 H18A H18C 0.4521 0.7682 0.4836 137 0.980 0.000 C18 C16 H18A H5 -0.4339 0.4079 0.1024 147 0.840 0.000 O5 C5 H5 H11 0.3997 0.5744 0.0454 147 0.840 0.000 O11 C11 H11 04src0995 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.14816 0.49655 0.37085 1.00000 0.01504 0.01765 0.01502 0.00125 0.00643 0.00182 0.01566 0.00229 0.00011 0.00010 0.00009 0.00000 0.00051 0.00054 0.00052 0.00041 0.00043 0.00042 0.00023 C2 0.00379 0.46191 0.30409 1.00000 0.01739 0.01911 0.01440 0.00150 0.00802 -0.00031 0.01636 0.00233 0.00011 0.00011 0.00009 0.00000 0.00054 0.00055 0.00052 0.00042 0.00044 0.00042 0.00023 C3 -0.02013 0.35288 0.24572 1.00000 0.01888 0.02105 0.02194 -0.00130 0.00953 0.00239 0.02007 0.00245 0.00012 0.00011 0.00009 0.00000 0.00056 0.00059 0.00058 0.00045 0.00047 0.00045 0.00025 H3 0.05248 0.30106 0.25159 1.00000 0.02409 0.00000 0.00000 C4 -0.14631 0.31845 0.17981 1.00000 0.02316 0.02123 0.02093 -0.00440 0.01030 -0.00184 0.02117 0.00246 0.00012 0.00011 0.00009 0.00000 0.00060 0.00059 0.00058 0.00046 0.00049 0.00047 0.00026 H4 -0.15997 0.24392 0.14104 1.00000 0.02541 0.00000 0.00000 C5 -0.25284 0.39354 0.17071 1.00000 0.01741 0.02360 0.01582 0.00041 0.00760 -0.00331 0.01854 0.00236 0.00011 0.00011 0.00009 0.00000 0.00055 0.00059 0.00054 0.00044 0.00045 0.00045 0.00024 C6 -0.23320 0.49985 0.23004 1.00000 0.01647 0.02214 0.01957 0.00131 0.00930 0.00217 0.01865 0.00242 0.00011 0.00011 0.00009 0.00000 0.00054 0.00058 0.00056 0.00045 0.00045 0.00044 0.00024 H6 -0.30660 0.54969 0.22591 1.00000 0.02238 0.00000 0.00000 C7 -0.10520 0.53356 0.29593 1.00000 0.01936 0.01774 0.01715 0.00027 0.00901 0.00011 0.01745 0.00239 0.00011 0.00011 0.00009 0.00000 0.00056 0.00055 0.00054 0.00042 0.00046 0.00043 0.00024 H7 -0.09224 0.60703 0.33606 1.00000 0.02094 0.00000 0.00000 C8 0.22539 0.49897 0.29659 1.00000 0.01534 0.01644 0.01543 -0.00096 0.00583 -0.00063 0.01571 0.00225 0.00011 0.00010 0.00009 0.00000 0.00052 0.00052 0.00052 0.00041 0.00043 0.00041 0.00023 C9 0.34781 0.44259 0.32033 1.00000 0.01826 0.02213 0.01668 0.00309 0.00554 0.00384 0.01930 0.00243 0.00011 0.00011 0.00009 0.00000 0.00055 0.00058 0.00054 0.00044 0.00045 0.00045 0.00024 H9 0.38425 0.39549 0.38347 1.00000 0.02316 0.00000 0.00000 C10 0.41808 0.45373 0.25348 1.00000 0.01493 0.02853 0.02000 0.00155 0.00585 0.00503 0.02134 0.00249 0.00012 0.00012 0.00009 0.00000 0.00053 0.00064 0.00058 0.00048 0.00046 0.00047 0.00026 H10 0.50219 0.41554 0.27161 1.00000 0.02561 0.00000 0.00000 C11 0.36506 0.52049 0.16075 1.00000 0.01690 0.02325 0.01805 -0.00269 0.00873 -0.00277 0.01876 0.00236 0.00011 0.00011 0.00009 0.00000 0.00055 0.00060 0.00055 0.00044 0.00046 0.00044 0.00025 C12 0.24151 0.57473 0.13330 1.00000 0.01777 0.02028 0.01642 0.00294 0.00490 0.00040 0.01858 0.00236 0.00011 0.00011 0.00009 0.00000 0.00054 0.00057 0.00054 0.00043 0.00045 0.00044 0.00024 H12 0.20373 0.61873 0.06856 1.00000 0.02230 0.00000 0.00000 C13 0.17381 0.56402 0.20139 1.00000 0.01471 0.01933 0.01866 0.00173 0.00574 0.00316 0.01771 0.00234 0.00011 0.00011 0.00009 0.00000 0.00052 0.00055 0.00055 0.00043 0.00044 0.00042 0.00024 H13 0.08960 0.60214 0.18273 1.00000 0.02125 0.00000 0.00000 C14 0.20154 0.39912 0.45836 1.00000 0.02309 0.02032 0.01818 0.00336 0.00900 0.00212 0.02015 0.00252 0.00012 0.00011 0.00009 0.00000 0.00059 0.00057 0.00056 0.00045 0.00048 0.00046 0.00025 H14A 0.19855 0.31847 0.42581 1.00000 0.03023 0.00000 0.00000 H14B 0.14677 0.39796 0.50163 1.00000 0.03023 0.00000 0.00000 H14C 0.29330 0.41882 0.50342 1.00000 0.03023 0.00000 0.00000 C15 0.15571 0.62358 0.42346 1.00000 0.01793 0.01925 0.01703 -0.00078 0.00745 0.00088 0.01780 0.00233 0.00011 0.00011 0.00009 0.00000 0.00054 0.00056 0.00054 0.00043 0.00045 0.00043 0.00024 H15A 0.11520 0.68426 0.36628 1.00000 0.02136 0.00000 0.00000 H15B 0.09987 0.62065 0.46672 1.00000 0.02136 0.00000 0.00000 C16 0.29319 0.67201 0.49457 1.00000 0.02004 0.02029 0.01920 -0.00014 0.00370 -0.00020 0.02089 0.00238 0.00012 0.00011 0.00009 0.00000 0.00058 0.00058 0.00057 0.00045 0.00047 0.00045 0.00026 H16 0.34731 0.60124 0.53464 1.00000 0.02507 0.00000 0.00000 C17 0.27657 0.76201 0.57453 1.00000 0.03474 0.03312 0.02410 -0.00930 0.01017 -0.00797 0.03089 0.00270 0.00014 0.00013 0.00011 0.00000 0.00073 0.00074 0.00065 0.00055 0.00057 0.00058 0.00031 H17A 0.36375 0.79254 0.62088 1.00000 0.04633 0.00000 0.00000 H17B 0.23403 0.72049 0.61748 1.00000 0.04633 0.00000 0.00000 H17C 0.22125 0.83087 0.53665 1.00000 0.04633 0.00000 0.00000 C18 0.36884 0.73434 0.43336 1.00000 0.02343 0.02637 0.03012 -0.00389 0.01012 -0.00515 0.02660 0.00264 0.00013 0.00012 0.00011 0.00000 0.00062 0.00066 0.00068 0.00052 0.00053 0.00050 0.00028 H18A 0.31470 0.80061 0.38972 1.00000 0.03990 0.00000 0.00000 H18B 0.38820 0.67419 0.38751 1.00000 0.03990 0.00000 0.00000 H18C 0.45209 0.76817 0.48363 1.00000 0.03990 0.00000 0.00000 O5 -0.37610 0.35890 0.09880 1.00000 0.01632 0.02988 0.02190 -0.00418 0.00625 -0.00200 0.02296 0.00170 0.00008 0.00008 0.00007 0.00000 0.00041 0.00048 0.00043 0.00036 0.00035 0.00034 0.00020 H5 -0.43386 0.40792 0.10237 1.00000 0.03443 0.00000 0.00000 O11 0.43862 0.52844 0.09738 1.00000 0.01933 0.03796 0.02114 0.00570 0.01190 0.00407 0.02489 0.00191 0.00008 0.00009 0.00007 0.00000 0.00043 0.00054 0.00044 0.00037 0.00036 0.00037 0.00021 H11 0.39965 0.57439 0.04542 1.00000 0.03733 0.00000 0.00000 Final Structure Factor Calculation for 04src0995 in P2(1)/n Total number of l.s. parameters = 186 Maximum vector length = 511 Memory required = 2573 / 21973 wR2 = 0.1017 before cycle 21 for 3404 data and 0 / 186 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0356 * P )^2 + 0.75 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0417 for 2986 Fo > 4sig(Fo) and 0.0486 for all 3404 data wR2 = 0.1017, GooF = S = 1.041, Restrained GooF = 1.041 for all data Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 22.00 for hydrogen atoms Principal mean square atomic displacements U 0.0188 0.0146 0.0136 C1 0.0195 0.0179 0.0117 C2 0.0231 0.0222 0.0150 C3 0.0264 0.0211 0.0160 C4 0.0252 0.0172 0.0133 C5 0.0234 0.0193 0.0133 C6 0.0201 0.0177 0.0145 C7 0.0171 0.0152 0.0148 C8 0.0246 0.0189 0.0144 C9 0.0302 0.0206 0.0133 C10 0.0251 0.0174 0.0138 C11 0.0224 0.0187 0.0147 C12 0.0211 0.0189 0.0131 C13 0.0247 0.0204 0.0154 C14 0.0199 0.0182 0.0154 C15 0.0254 0.0203 0.0170 C16 0.0423 0.0322 0.0181 C17 0.0327 0.0275 0.0195 C18 0.0317 0.0212 0.0160 O5 0.0402 0.0213 0.0132 O11 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.029 0.045 0.061 0.080 0.102 0.134 0.176 0.253 1.000 Number in group 342. 344. 344. 344. 337. 335. 340. 340. 338. 340. GooF 1.026 1.059 1.040 1.097 1.107 0.992 0.964 1.051 1.027 1.039 K 3.247 1.229 1.028 1.026 0.989 1.004 0.998 1.008 1.009 1.001 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 344. 343. 341. 340. 342. 335. 339. 339. 339. 342. GooF 1.002 0.927 1.005 0.874 0.889 0.954 1.070 0.952 1.194 1.420 K 1.031 1.040 1.039 1.020 1.003 0.989 0.980 0.992 1.023 1.003 R1 0.093 0.077 0.090 0.062 0.053 0.042 0.039 0.029 0.040 0.034 Recommended weighting scheme: WGHT 0.0356 0.7483 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) 0 6 6 75.55 2.11 5.57 0.017 1.37 6 0 0 81.22 0.31 5.57 0.007 1.68 3 6 0 172.83 99.67 5.37 0.118 1.60 0 7 7 83.40 34.28 4.97 0.069 1.18 -6 0 6 43.29 13.83 4.67 0.044 1.65 3 0 3 103.97 23.88 4.39 0.058 2.25 0 9 9 13.02 1.23 4.28 0.013 0.92 0 6 0 572.67 351.87 3.93 0.222 1.82 -6 3 9 428.97 335.89 3.82 0.217 1.27 3 5 2 35.15 18.15 3.81 0.050 1.67 -3 5 6 62.73 38.78 3.77 0.074 1.54 -3 7 2 35.24 18.18 3.69 0.050 1.43 -6 6 12 25.66 10.55 3.62 0.038 0.94 -3 0 9 81.39 43.97 3.62 0.078 1.51 0 4 4 48.50 28.45 3.59 0.063 2.06 5 3 0 189.20 143.70 3.56 0.142 1.76 0 6 9 5.97 0.00 3.55 0.000 1.11 -6 6 15 27.81 11.64 3.45 0.040 0.80 12 0 2 1357.59 1119.16 3.41 0.395 0.80 0 5 4 196.52 151.83 3.39 0.146 1.79 10 3 0 7.10 19.51 3.35 0.052 0.97 3 9 3 313.25 248.20 3.32 0.186 1.07 -1 7 8 392.79 479.91 3.31 0.259 1.13 6 3 0 27.72 14.61 3.27 0.045 1.53 0 3 9 6.58 1.02 3.20 0.012 1.31 -8 0 10 23.51 43.48 3.20 0.078 1.13 1 4 1 226.13 177.16 3.18 0.157 2.53 2 3 2 24.40 41.69 3.17 0.076 2.47 1 3 5 254.98 204.96 3.13 0.169 1.92 -3 1 8 100.51 73.34 3.12 0.101 1.67 0 5 5 125.64 93.21 3.11 0.114 1.65 8 3 3 278.86 344.67 3.11 0.219 1.05 9 5 3 10.28 0.43 3.03 0.008 0.90 -12 1 11 225.13 176.18 3.03 0.157 0.84 3 5 3 42.46 26.77 3.01 0.061 1.57 -1 9 8 269.41 339.60 3.01 0.218 0.98 -5 2 1 216.57 174.00 3.01 0.156 1.98 0 9 5 157.67 200.25 2.97 0.167 1.09 -8 4 2 30.22 17.49 2.93 0.049 1.20 3 1 4 758.80 653.30 2.91 0.302 1.93 -6 0 12 63.42 90.08 2.91 0.112 1.09 -7 1 10 100.08 74.44 2.88 0.102 1.19 2 6 9 16.80 31.08 2.87 0.066 1.02 4 2 2 37.16 55.74 2.85 0.088 1.95 0 7 9 7.87 17.41 2.79 0.049 1.04 -8 1 17 505.11 427.65 2.75 0.244 0.78 -7 0 13 193.09 240.83 2.73 0.183 0.99 -2 0 2 2452.45 2758.83 2.68 0.621 4.94 -11 7 5 30.38 15.95 2.67 0.047 0.83 -5 3 4 1246.59 1103.69 2.67 0.393 1.81 Bond lengths and angles C1 - Distance Angles C8 1.5339 (0.0015) C14 1.5377 (0.0016) 112.22 (0.09) C2 1.5384 (0.0016) 107.78 (0.09) 107.05 (0.09) C15 1.5478 (0.0016) 109.88 (0.09) 108.86 (0.09) 111.03 (0.09) C1 - C8 C14 C2 C2 - Distance Angles C7 1.3892 (0.0016) C3 1.3992 (0.0016) 117.44 (0.11) C1 1.5384 (0.0016) 124.13 (0.10) 118.42 (0.10) C2 - C7 C3 C3 - Distance Angles C4 1.3813 (0.0017) C2 1.3992 (0.0016) 121.88 (0.11) H3 0.9500 119.06 119.06 C3 - C4 C2 C4 - Distance Angles C3 1.3813 (0.0017) C5 1.3863 (0.0017) 119.45 (0.11) H4 0.9500 120.27 120.27 C4 - C3 C5 C5 - Distance Angles C6 1.3828 (0.0017) O5 1.3841 (0.0014) 122.58 (0.11) C4 1.3863 (0.0017) 120.12 (0.11) 117.27 (0.11) C5 - C6 O5 C6 - Distance Angles C5 1.3828 (0.0017) C7 1.3941 (0.0016) 119.70 (0.11) H6 0.9500 120.15 120.15 C6 - C5 C7 C7 - Distance Angles C2 1.3892 (0.0016) C6 1.3941 (0.0016) 121.34 (0.11) H7 0.9500 119.33 119.33 C7 - C2 C6 C8 - Distance Angles C9 1.3906 (0.0016) C13 1.3957 (0.0016) 117.32 (0.10) C1 1.5339 (0.0015) 123.45 (0.10) 119.20 (0.10) C8 - C9 C13 C9 - Distance Angles C8 1.3906 (0.0016) C10 1.3924 (0.0016) 121.38 (0.11) H9 0.9500 119.31 119.31 C9 - C8 C10 C10 - Distance Angles C11 1.3807 (0.0017) C9 1.3924 (0.0016) 119.75 (0.11) H10 0.9500 120.13 120.13 C10 - C11 C9 C11 - Distance Angles O11 1.3784 (0.0014) C10 1.3807 (0.0017) 117.39 (0.10) C12 1.3857 (0.0016) 122.35 (0.11) 120.26 (0.11) C11 - O11 C10 C12 - Distance Angles C13 1.3846 (0.0016) C11 1.3857 (0.0016) 119.19 (0.11) H12 0.9500 120.41 120.41 C12 - C13 C11 C13 - Distance Angles C12 1.3846 (0.0016) C8 1.3957 (0.0016) 122.07 (0.10) H13 0.9500 118.96 118.96 C13 - C12 C8 C14 - Distance Angles C1 1.5377 (0.0016) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - C1 H14A H14B C15 - Distance Angles C16 1.5392 (0.0016) C1 1.5478 (0.0016) 117.97 (0.09) H15A 0.9900 107.82 107.82 H15B 0.9900 107.82 107.82 107.15 C15 - C16 C1 H15A C16 - Distance Angles C17 1.5237 (0.0018) C18 1.5295 (0.0017) 109.32 (0.11) C15 1.5392 (0.0016) 108.83 (0.10) 113.90 (0.10) H16 1.0000 108.22 108.22 108.22 C16 - C17 C18 C15 C17 - Distance Angles C16 1.5237 (0.0017) H17A 0.9800 109.47 H17B 0.9800 109.47 109.47 H17C 0.9800 109.47 109.47 109.47 C17 - C16 H17A H17B C18 - Distance Angles C16 1.5295 (0.0017) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C16 H18A H18B O5 - Distance Angles C5 1.3841 (0.0014) H5 0.8400 109.47 O5 - C5 O11 - Distance Angles C11 1.3784 (0.0014) H11 0.8400 109.47 O11 - C11 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.89 2.7300(13) 173.4 O5-H5...O11_$1 0.84 2.01 2.7777(13) 150.9 O11-H11...O5_$2 FMAP and GRID set by program FMAP 2 3 20 GRID -1.471 -2 -2 1.471 2 2 R1 = 0.0485 for 3404 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.31 at 0.3055 0.0026 0.1620 [ 0.76 A from C8 ] Deepest hole -0.21 at 0.3561 0.5686 0.1152 [ 0.79 A from C11 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 2656 / 21153 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1945 0.5026 0.3380 1.00000 0.05 0.31 0.76 C8 0.79 C1 1.89 C9 1.90 C13 Q2 1 0.0727 0.4845 0.3411 1.00000 0.05 0.27 0.77 C2 0.78 C1 1.88 C7 1.90 C15 Q3 1 -0.2374 0.4654 0.1800 1.00000 0.05 0.25 0.76 C6 0.80 C5 1.47 H6 1.85 C7 Q4 1 0.1560 0.5580 0.3994 1.00000 0.05 0.25 0.76 C1 0.79 C15 1.45 H15B 1.47 H15A Q5 1 0.2271 0.6523 0.4514 1.00000 0.05 0.25 0.77 C16 0.79 C15 1.37 H15A 1.48 H16 Shortest distances between peaks (including symmetry equivalents) 1 4 1.22 2 4 1.25 4 5 1.32 1 2 1.35 1 5 2.18 2 5 2.56 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.01: Analyse other restraints etc. 0.57: 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 3.48: Structure factors and derivatives 4.02: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.52: Solve l.s. equations 0.00: Generate HTAB table 0.07: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.01: Fourier summations 0.04: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04src0995 finished at 14:18:55 Total CPU time: 8.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++