+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010sl0004a started at 22:17:25 on 29-Mar-2011 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2010sl0004a CELL 0.71073 12.8476 3.7474 21.5262 90.000 97.291 90.000 ZERR 4.00 0.0008 0.0002 0.0014 0.000 0.003 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N F UNIT 52 0 4 12 V = 1028.00 F(000) = 448.0 Mu = 0.13 mm-1 Cell Wt = 908.56 Rho = 1.468 MERG 2 OMIT -3.00 50.00 SHEL 7 0.77 OMIT 0 0 4 FMAP 2 PLAN 20 SIZE 0.03 0.04 0.60 BOND $H WGHT 0.07990 0.18840 L.S. 20 TEMP -153.00 ACTA FVAR 0.23508 F1 4 0.839531 0.828021 0.227010 11.00000 0.03293 0.04483 = 0.02059 -0.00530 -0.00332 -0.00368 F2 4 0.891138 0.271552 0.000534 11.00000 0.03633 0.05045 = 0.02596 -0.00597 0.00677 0.00196 F3 4 0.182008 1.035993 0.159684 11.00000 0.02448 0.05396 = 0.02955 -0.00086 0.00364 0.00397 N1 3 0.578723 0.736673 0.098986 11.00000 0.02396 0.02904 = 0.02104 0.00026 -0.00124 0.00166 C1 1 0.351640 0.806363 0.190639 11.00000 0.02927 0.03299 = 0.01768 0.00009 -0.00047 -0.00292 AFIX 43 H1 2 0.332451 0.746644 0.230544 11.00000 -1.20000 AFIX 0 C2 1 0.777965 0.502336 0.068230 11.00000 0.02667 0.02541 = 0.02078 0.00265 -0.00185 0.00029 AFIX 43 H2 2 0.719940 0.468026 0.036780 11.00000 -1.20000 AFIX 0 C3 1 0.404382 0.978486 0.072802 11.00000 0.02845 0.03234 = 0.01581 0.00140 -0.00164 -0.00073 AFIX 43 H3 2 0.422084 1.033372 0.032351 11.00000 -1.20000 AFIX 0 C4 1 0.479138 0.821769 0.117128 11.00000 0.02542 0.02299 = 0.02126 -0.00237 -0.00113 -0.00110 C5 1 0.451624 0.734425 0.176109 11.00000 0.02538 0.02921 = 0.02077 0.00298 -0.00361 0.00057 AFIX 43 H5 2 0.501808 0.625053 0.206415 11.00000 -1.20000 AFIX 0 C6 1 0.851629 0.687518 0.170107 11.00000 0.03041 0.02869 = 0.01731 0.00177 -0.00010 -0.00079 C7 1 0.280804 0.966599 0.145774 11.00000 0.02234 0.03006 = 0.02333 -0.00102 0.00179 0.00041 C8 1 0.304959 1.054805 0.087012 11.00000 0.02479 0.02754 = 0.02414 0.00038 -0.00475 0.00261 AFIX 43 H8 2 0.254403 1.165337 0.057076 11.00000 -1.20000 AFIX 0 C9 1 0.877385 0.409661 0.057173 11.00000 0.03173 0.02983 = 0.02034 0.00256 0.00273 0.00149 C10 1 0.762997 0.648167 0.126442 11.00000 0.02314 0.02492 = 0.02136 0.00270 -0.00136 0.00046 C11 1 0.658876 0.758340 0.140354 11.00000 0.02938 0.02455 = 0.01857 0.00036 0.00115 -0.00199 AFIX 43 H11 2 0.651002 0.847263 0.180822 11.00000 -1.20000 AFIX 0 C12 1 0.951259 0.594203 0.159078 11.00000 0.02488 0.03660 = 0.02592 0.00684 -0.00392 -0.00226 AFIX 43 H12 2 1.009464 0.627038 0.190462 11.00000 -1.20000 AFIX 0 C13 1 0.965030 0.451212 0.101217 11.00000 0.02511 0.03613 = 0.02962 0.00662 0.00312 0.00107 AFIX 43 H13 2 1.032703 0.383649 0.092051 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2010sl0004a C 0.770 H 0.320 N 0.700 F 0.640 F1 - C6 F2 - C9 F3 - C7 N1 - C11 C4 C1 - C7 C5 C2 - C9 C10 C3 - C8 C4 C4 - C3 C5 N1 C5 - C1 C4 C6 - F1 C12 C10 C7 - F3 C1 C8 C8 - C7 C3 C9 - F2 C2 C13 C10 - C6 C2 C11 C11 - N1 C10 C12 - C6 C13 C13 - C9 C12 14663 Reflections read, of which 2854 rejected -15 =< h =< 15, -4 =< k =< 4, -25 =< l =< 25, Max. 2-theta = 49.98 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 8 1 3 3.91 0.20 10 1.17 11 2 6 2.70 0.26 7 1.56 2 Inconsistent equivalents 1815 Unique reflections, of which 0 suppressed R(int) = 0.0722 R(sigma) = 0.0532 Friedel opposites merged Maximum memory for data reduction = 1429 / 18412 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. ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 52.00 52.00 H 0.00 32.00 N 4.00 4.00 F 12.00 12.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1371 before cycle 1 for 1815 data and 154 / 154 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23671 0.00089 1.819 OSF Mean shift/su = 0.542 Maximum = 1.819 for OSF Max. shift = 0.004 A for C9 Max. dU = 0.001 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1330 before cycle 2 for 1815 data and 154 / 154 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23727 0.00087 0.641 OSF Mean shift/su = 0.205 Maximum = 0.641 for OSF Max. shift = 0.001 A for C11 Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 3 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.040 OSF Mean shift/su = 0.013 Maximum = 0.048 for U11 C2 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 4 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.001 OSF Mean shift/su = 0.002 Maximum = 0.014 for U33 C2 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C2 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 5 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.001 OSF Mean shift/su = 0.000 Maximum = 0.001 for U22 F3 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C2 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 6 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for N1 Max. dU = 0.000 for C13 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 7 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y F3 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C4 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 8 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C3 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 9 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C9 Least-squares cycle 10 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 10 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C6 Least-squares cycle 11 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 11 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for C7 Max. dU = 0.000 for N1 Least-squares cycle 12 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 12 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C12 Least-squares cycle 13 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 13 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C1 Least-squares cycle 14 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 14 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for F2 Max. dU = 0.000 for C3 Least-squares cycle 15 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 15 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for C7 Max. dU = 0.000 for F2 Least-squares cycle 16 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 16 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for F1 Least-squares cycle 17 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 17 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x F2 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C7 Least-squares cycle 18 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 18 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C4 Max. dU = 0.000 for F3 Least-squares cycle 19 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 19 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for C8 Max. dU = 0.000 for F3 Least-squares cycle 20 Maximum vector length = 511 Memory required = 1832 / 192626 wR2 = 0.1327 before cycle 20 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23730 0.00087 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C13 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.3324 0.7466 0.2303 43 0.950 0.000 C1 C7 C5 H2 0.7203 0.4671 0.0368 43 0.950 0.000 C2 C9 C10 H3 0.4220 1.0343 0.0325 43 0.950 0.000 C3 C8 C4 H5 0.5013 0.6251 0.2064 43 0.950 0.000 C5 C1 C4 H8 0.2547 1.1652 0.0573 43 0.950 0.000 C8 C7 C3 H11 0.6513 0.8467 0.1807 43 0.950 0.000 C11 N1 C10 H12 1.0091 0.6255 0.1905 43 0.950 0.000 C12 C6 C13 H13 1.0326 0.3843 0.0920 43 0.950 0.000 C13 C9 C12 2010sl0004a ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq F1 0.83948 0.82810 0.22699 1.00000 0.03336 0.04661 0.02069 -0.00473 -0.00318 -0.00366 0.03413 0.00211 0.00009 0.00034 0.00005 0.00000 0.00072 0.00082 0.00069 0.00055 0.00052 0.00056 0.00037 F2 0.89117 0.27144 0.00055 1.00000 0.03656 0.05097 0.02678 -0.00536 0.00687 0.00164 0.03786 0.00225 0.00010 0.00035 0.00006 0.00000 0.00076 0.00085 0.00077 0.00058 0.00057 0.00059 0.00039 F3 0.18205 1.03615 0.15964 1.00000 0.02536 0.05572 0.02903 -0.00063 0.00287 0.00418 0.03675 0.00228 0.00009 0.00036 0.00006 0.00000 0.00070 0.00088 0.00075 0.00059 0.00054 0.00055 0.00039 N1 0.57854 0.73653 0.09897 1.00000 0.02512 0.03052 0.02077 0.00046 -0.00102 0.00089 0.02581 0.00301 0.00013 0.00044 0.00008 0.00000 0.00095 0.00097 0.00097 0.00071 0.00075 0.00072 0.00044 C1 0.35162 0.80647 0.19042 1.00000 0.02966 0.03419 0.01806 -0.00023 -0.00060 -0.00281 0.02761 0.00361 0.00016 0.00056 0.00009 0.00000 0.00118 0.00118 0.00110 0.00086 0.00089 0.00088 0.00051 H1 0.33241 0.74657 0.23032 1.00000 0.03314 0.00000 0.00000 C2 0.77825 0.50212 0.06832 1.00000 0.02901 0.02717 0.01986 0.00345 -0.00355 -0.00026 0.02592 0.00365 0.00016 0.00051 0.00010 0.00000 0.00116 0.00114 0.00112 0.00083 0.00088 0.00085 0.00050 H2 0.72035 0.46714 0.03681 1.00000 0.03111 0.00000 0.00000 C3 0.40441 0.97885 0.07291 1.00000 0.02960 0.03178 0.01691 0.00043 -0.00079 -0.00057 0.02642 0.00363 0.00016 0.00053 0.00010 0.00000 0.00116 0.00118 0.00108 0.00084 0.00087 0.00087 0.00050 H3 0.42204 1.03429 0.03247 1.00000 0.03170 0.00000 0.00000 C4 0.47914 0.82197 0.11710 1.00000 0.02521 0.02479 0.02000 -0.00277 -0.00194 -0.00123 0.02375 0.00348 0.00015 0.00054 0.00009 0.00000 0.00110 0.00107 0.00110 0.00080 0.00086 0.00079 0.00048 C5 0.45127 0.73470 0.17602 1.00000 0.02615 0.03038 0.02057 0.00236 -0.00473 0.00086 0.02636 0.00363 0.00016 0.00055 0.00010 0.00000 0.00114 0.00114 0.00113 0.00084 0.00086 0.00085 0.00050 H5 0.50133 0.62514 0.20637 1.00000 0.03163 0.00000 0.00000 C6 0.85157 0.68731 0.17002 1.00000 0.03090 0.02885 0.01628 0.00256 -0.00133 -0.00118 0.02572 0.00367 0.00016 0.00054 0.00009 0.00000 0.00119 0.00112 0.00108 0.00082 0.00087 0.00086 0.00049 C7 0.28090 0.96648 0.14573 1.00000 0.02106 0.03162 0.02490 -0.00157 0.00251 0.00012 0.02590 0.00365 0.00015 0.00055 0.00010 0.00000 0.00108 0.00120 0.00120 0.00086 0.00088 0.00081 0.00050 C8 0.30522 1.05457 0.08719 1.00000 0.02560 0.02854 0.02254 0.00094 -0.00588 0.00222 0.02633 0.00364 0.00016 0.00054 0.00010 0.00000 0.00111 0.00111 0.00114 0.00086 0.00088 0.00084 0.00050 H8 0.25468 1.16524 0.05725 1.00000 0.03159 0.00000 0.00000 C9 0.87738 0.41048 0.05739 1.00000 0.03254 0.03021 0.02070 0.00210 0.00260 0.00154 0.02788 0.00382 0.00016 0.00057 0.00010 0.00000 0.00125 0.00113 0.00115 0.00088 0.00094 0.00092 0.00051 C10 0.76286 0.64796 0.12635 1.00000 0.02442 0.02618 0.02126 0.00276 -0.00088 -0.00090 0.02428 0.00366 0.00015 0.00054 0.00009 0.00000 0.00108 0.00107 0.00110 0.00083 0.00086 0.00081 0.00048 C11 0.65905 0.75774 0.14017 1.00000 0.03054 0.02644 0.01866 0.00115 0.00145 -0.00206 0.02535 0.00376 0.00016 0.00053 0.00010 0.00000 0.00116 0.00109 0.00107 0.00082 0.00090 0.00085 0.00049 H11 0.65133 0.84673 0.18066 1.00000 0.03043 0.00000 0.00000 C12 0.95096 0.59352 0.15900 1.00000 0.02536 0.03713 0.02619 0.00739 -0.00548 -0.00285 0.03031 0.00396 0.00016 0.00061 0.00010 0.00000 0.00117 0.00121 0.00122 0.00094 0.00090 0.00090 0.00053 H12 1.00910 0.62552 0.19045 1.00000 0.03638 0.00000 0.00000 C13 0.96491 0.45151 0.10124 1.00000 0.02551 0.03648 0.03001 0.00788 0.00385 0.00151 0.03064 0.00402 0.00016 0.00059 0.00010 0.00000 0.00115 0.00127 0.00126 0.00094 0.00095 0.00089 0.00054 H13 1.03259 0.38433 0.09204 1.00000 0.03677 0.00000 0.00000 Final Structure Factor Calculation for 2010sl0004a Total number of l.s. parameters = 154 Maximum vector length = 511 Memory required = 1678 / 22995 wR2 = 0.1327 before cycle 21 for 1815 data and 0 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 0.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0493 for 1473 Fo > 4sig(Fo) and 0.0668 for all 1815 data wR2 = 0.1327, GooF = S = 1.032, Restrained GooF = 1.032 for all data Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0478 0.0370 0.0176 F1 0.0523 0.0370 0.0243 F2 0.0563 0.0291 0.0248 F3 0.0307 0.0279 0.0188 N1 0.0358 0.0297 0.0174 C1 0.0341 0.0273 0.0163 C2 0.0322 0.0307 0.0163 C3 0.0288 0.0257 0.0167 C4 0.0329 0.0305 0.0157 C5 0.0336 0.0283 0.0152 C6 0.0320 0.0246 0.0211 C7 0.0346 0.0286 0.0157 C8 0.0333 0.0301 0.0203 C9 0.0295 0.0246 0.0187 C10 0.0320 0.0256 0.0185 C11 0.0445 0.0289 0.0175 C12 0.0418 0.0255 0.0246 C13 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.020 0.031 0.043 0.057 0.070 0.090 0.118 0.177 1.000 Number in group 189. 179. 177. 187. 182. 180. 183. 175. 180. 183. GooF 1.277 1.243 1.081 1.032 1.030 0.970 0.933 0.940 0.816 0.889 K 13.714 1.610 1.097 1.008 1.152 0.995 0.993 1.002 1.012 0.987 Resolution(A) 0.84 0.87 0.90 0.94 1.00 1.06 1.14 1.24 1.44 1.79 inf Number in group 184. 184. 176. 190. 177. 178. 181. 183. 180. 182. GooF 1.061 1.136 1.188 1.027 0.998 0.970 0.925 0.952 0.950 1.079 K 1.042 0.995 1.233 1.029 1.006 1.032 1.041 1.038 1.026 0.956 R1 0.178 0.167 0.187 0.078 0.055 0.052 0.045 0.043 0.033 0.041 Recommended weighting scheme: WGHT 0.0556 0.3608 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 2 19 20.89 1.21 4.37 0.008 0.97 0 2 19 16.38 0.68 4.10 0.006 0.96 11 1 12 21.45 64.77 3.71 0.061 0.89 -6 1 5 11.07 2.52 3.65 0.012 1.77 -3 4 3 2.64 12.59 3.31 0.027 0.91 -9 3 7 11.66 28.81 3.15 0.041 0.92 -6 1 20 15.68 0.67 3.08 0.006 0.97 9 1 2 7.73 0.08 3.04 0.002 1.30 -8 2 4 8.16 0.13 3.00 0.003 1.21 -3 1 23 27.08 10.08 2.97 0.024 0.90 -2 1 6 16.57 8.04 2.89 0.022 2.47 -11 1 5 28.13 41.99 2.86 0.049 1.10 12 1 9 262.52 178.89 2.85 0.102 0.90 8 1 13 252.21 340.68 2.84 0.141 1.04 -2 0 2 1804.91 2374.02 2.83 0.371 5.81 -2 2 14 18.80 8.07 2.82 0.022 1.18 6 3 13 37.91 5.22 2.80 0.017 0.88 -3 0 23 368.12 498.69 2.68 0.170 0.93 11 1 5 17.39 6.83 2.68 0.020 1.04 6 0 10 67.88 92.35 2.66 0.073 1.42 5 4 1 28.79 0.29 2.66 0.004 0.88 7 2 8 18.03 8.37 2.65 0.022 1.13 -10 2 4 21.01 33.27 2.64 0.044 1.06 3 3 0 4.49 0.02 2.61 0.001 1.20 5 2 4 12.15 5.55 2.61 0.018 1.42 7 0 13 66.61 92.42 2.59 0.073 1.15 13 2 2 13.68 3.00 2.52 0.013 0.86 -11 1 12 21.16 9.25 2.51 0.023 1.00 -1 4 2 1268.47 42.99 2.51 0.050 0.93 -4 3 9 64.13 86.38 2.50 0.071 1.06 -3 0 25 90.19 135.29 2.48 0.089 0.86 -12 1 6 136.37 176.50 2.48 0.101 1.02 -13 2 9 -3.64 8.91 2.44 0.023 0.85 12 1 10 220.13 162.12 2.43 0.097 0.88 1 0 23 150.44 105.33 2.43 0.078 0.92 -10 2 13 14.82 29.03 2.42 0.041 0.93 9 0 11 53.22 73.03 2.41 0.065 1.08 -6 2 5 8.58 2.53 2.38 0.012 1.37 -5 3 2 4.71 1.05 2.38 0.008 1.12 -1 3 9 8.94 17.79 2.35 0.032 1.11 -3 1 12 41.76 29.59 2.34 0.041 1.56 -10 2 17 13.20 0.90 2.34 0.007 0.85 -13 0 9 -1.95 8.18 2.33 0.022 0.95 -9 1 6 5.99 0.73 2.29 0.007 1.29 -3 2 20 -5.01 4.08 2.29 0.015 0.93 13 0 7 197.31 265.61 2.28 0.124 0.90 4 2 7 7.77 2.09 2.26 0.011 1.39 3 4 1 29.11 3.82 2.25 0.015 0.91 5 2 9 8.64 2.88 2.25 0.013 1.23 3 1 3 461.50 562.04 2.25 0.181 2.54 Bond lengths and angles F1 - Distance Angles C6 1.3620 (0.0024) F1 - F2 - Distance Angles C9 1.3620 (0.0024) F2 - F3 - Distance Angles C7 1.3664 (0.0023) F3 - N1 - Distance Angles C11 1.2766 (0.0028) C4 1.4185 (0.0026) 118.24 (0.17) N1 - C11 C1 - Distance Angles C7 1.3743 (0.0029) C5 1.3814 (0.0029) 118.49 (0.19) H1 0.9500 120.76 120.76 C1 - C7 C5 C2 - Distance Angles C9 1.3679 (0.0029) C10 1.4004 (0.0029) 119.43 (0.18) H2 0.9500 120.29 120.29 C2 - C9 C10 C3 - Distance Angles C8 1.3777 (0.0030) C4 1.3929 (0.0029) 120.77 (0.19) H3 0.9500 119.62 119.62 C3 - C8 C4 C4 - Distance Angles C3 1.3929 (0.0029) C5 1.3997 (0.0029) 118.94 (0.18) N1 1.4185 (0.0026) 118.30 (0.18) 122.63 (0.18) C4 - C3 C5 C5 - Distance Angles C1 1.3814 (0.0029) C4 1.3997 (0.0029) 120.59 (0.18) H5 0.9500 119.71 119.71 C5 - C1 C4 C6 - Distance Angles F1 1.3620 (0.0024) C12 1.3737 (0.0030) 117.99 (0.18) C10 1.3900 (0.0028) 118.20 (0.18) 123.81 (0.19) C6 - F1 C12 C7 - Distance Angles F3 1.3664 (0.0023) C1 1.3743 (0.0029) 118.70 (0.18) C8 1.3765 (0.0030) 118.69 (0.18) 122.60 (0.19) C7 - F3 C1 C8 - Distance Angles C7 1.3765 (0.0030) C3 1.3777 (0.0030) 118.59 (0.19) H8 0.9500 120.70 120.70 C8 - C7 C3 C9 - Distance Angles F2 1.3620 (0.0024) C2 1.3679 (0.0029) 118.73 (0.18) C13 1.3820 (0.0030) 117.95 (0.18) 123.32 (0.19) C9 - F2 C2 C10 - Distance Angles C6 1.3900 (0.0029) C2 1.4004 (0.0029) 116.63 (0.18) C11 1.4619 (0.0029) 121.57 (0.19) 121.80 (0.18) C10 - C6 C2 C11 - Distance Angles N1 1.2766 (0.0028) C10 1.4619 (0.0029) 121.39 (0.19) H11 0.9500 119.31 119.31 C11 - N1 C10 C12 - Distance Angles C6 1.3737 (0.0030) C13 1.3849 (0.0031) 118.84 (0.19) H12 0.9500 120.58 120.58 C12 - C6 C13 C13 - Distance Angles C9 1.3820 (0.0030) C12 1.3849 (0.0031) 117.98 (0.19) H13 0.9500 121.01 121.01 C13 - C9 C12 FMAP and GRID set by program FMAP 2 2 8 GRID -5.000 -2 -2 5.000 2 2 R1 = 0.0667 for 1815 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.17 at 0.5959 0.1474 0.1574 [ 1.39 A from H11 ] Deepest hole -0.26 at 0.2343 0.0338 0.1178 [ 0.83 A from C7 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2251 / 18006 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5959 1.1474 0.1574 1.00000 0.05 0.17 1.39 H11 1.73 C11 1.98 N1 2.04 C4 Q2 1 0.0993 1.2033 0.1348 1.00000 0.05 0.16 1.29 F3 1.36 H13 2.01 C13 2.37 H12 Q3 1 0.8046 1.0443 0.2072 1.00000 0.05 0.15 1.00 F1 1.71 C6 2.11 H11 2.30 C10 Q4 1 1.0005 0.3353 -0.0142 1.00000 0.05 0.15 1.50 F2 1.98 H13 2.02 F2 2.14 C13 Q5 1 0.9383 0.7562 0.2196 1.00000 0.05 0.15 1.27 H12 1.33 F1 1.47 C6 1.47 C12 Q6 1 1.0880 0.7370 0.1037 1.00000 0.05 0.15 1.51 H13 1.90 C13 1.95 F3 2.27 H12 Q7 1 0.0741 1.0584 0.1673 1.00000 0.05 0.15 1.42 F3 1.92 H12 2.04 H13 2.34 C12 Q8 1 0.6983 0.3344 0.0026 1.00000 0.05 0.14 0.90 H2 1.76 C2 2.14 H3 2.28 C3 Q9 1 0.4961 0.4935 0.2041 1.00000 0.05 0.14 0.50 H5 1.19 C5 2.18 C1 2.23 C4 Q10 1 1.1414 0.4767 0.1181 1.00000 0.05 0.13 1.48 H13 1.92 F3 2.25 C13 2.38 H8 Q11 1 0.2213 0.5484 0.1177 1.00000 0.05 0.13 1.81 C7 2.02 H8 2.13 F3 2.28 C8 Q12 1 0.4561 0.4978 0.0598 1.00000 0.05 0.13 1.73 C4 1.87 H3 1.91 N1 1.95 C3 Q13 1 0.5059 0.2192 0.1647 1.00000 0.05 0.13 1.77 H5 1.82 C4 1.97 C5 2.32 H11 Q14 1 1.0109 0.0964 0.1360 1.00000 0.05 0.13 1.49 H13 1.60 C13 2.10 C12 2.12 H12 Q15 1 0.1829 1.4407 0.1660 1.00000 0.05 0.13 1.52 F3 2.25 C7 2.35 H13 2.38 H1 Q16 1 0.9401 0.0511 0.1181 1.00000 0.05 0.13 1.59 C13 1.86 H13 1.92 C12 1.98 C9 Q17 1 0.5586 0.4467 0.2392 1.00000 0.05 0.13 1.16 H5 1.48 F1 2.11 C5 2.20 H12 Q18 1 0.4830 0.3171 0.2428 1.00000 0.05 0.13 1.43 H5 1.60 H12 2.13 C5 2.29 F1 Q19 1 0.2965 0.4767 0.1399 1.00000 0.05 0.13 1.74 C1 1.85 C7 1.96 C8 2.14 H8 Q20 1 0.5888 0.8042 0.0380 1.00000 0.05 0.12 1.36 N1 1.62 H3 2.11 H2 2.28 C11 Shortest distances between peaks (including symmetry equivalents) 14 16 0.96 2 7 0.97 7 14 1.00 9 17 1.05 11 19 1.06 10 11 1.06 9 18 1.09 17 18 1.10 10 15 1.11 5 17 1.14 2 14 1.21 6 10 1.21 1 13 1.22 2 10 1.23 5 18 1.23 11 15 1.27 9 13 1.35 4 4 1.38 2 15 1.49 15 19 1.63 13 18 1.78 6 11 1.84 6 7 1.85 6 14 1.86 13 17 1.87 2 6 1.87 7 16 1.90 5 9 1.96 10 19 1.99 7 15 2.00 3 17 2.01 3 5 2.02 6 15 2.02 2 11 2.10 2 16 2.11 4 6 2.13 7 10 2.14 12 20 2.16 1 9 2.16 1 17 2.19 10 14 2.27 6 16 2.29 8 12 2.34 7 18 2.34 12 20 2.40 8 20 2.43 5 16 2.45 5 7 2.47 5 14 2.48 12 13 2.50 5 13 2.51 1 18 2.56 14 15 2.57 2 19 2.72 3 16 2.75 9 19 2.75 1 5 2.77 1 3 2.79 4 10 2.79 14 18 2.80 7 17 2.83 12 19 2.84 13 19 2.84 4 16 2.85 6 19 2.86 1 20 2.87 1 12 2.90 3 18 2.93 7 11 2.93 8 11 2.94 12 12 2.94 14 17 2.99 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 0.02: Analyse other restraints etc. 2.05: 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 1.27: Structure factors and derivatives 1.70: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.08: Apply other restraints 0.94: Solve l.s. equations 0.00: Generate HTAB table 0.08: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0004a finished at 22:17:56 Total CPU time: 6.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++