+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0764 started at 20:10:12 on 04-Jul-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0764 in P2(1)2(1)2(1) CELL 0.71073 9.6974 13.2347 17.3564 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0002 0.0002 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 F P UNIT 88 100 8 4 24 4 V = 2227.56 F(000) = 992.0 Mu = 0.19 mm-1 Cell Wt = 1913.64 Rho = 1.427 MERG 2 OMIT -3.00 55.00 OMIT 0 3 2 OMIT 1 0 2 FMAP 2 PLAN 20 SIZE 0.20 0.30 0.45 ACTA BOND WGHT 0.04390 0.76450 L.S. 4 TEMP -153.00 FVAR 0.86157 C1 1 -0.189303 1.122553 0.669194 11.00000 0.01257 0.01987 = 0.01556 0.00147 -0.00100 -0.00175 C2 1 -0.243035 1.187910 0.735092 11.00000 0.01958 0.02870 = 0.01982 -0.00234 0.00168 0.00223 AFIX 33 H2A 2 -0.194608 1.170155 0.782764 11.00000 -1.50000 H2B 2 -0.342129 1.176250 0.741699 11.00000 -1.50000 H2C 2 -0.226882 1.259305 0.723138 11.00000 -1.50000 AFIX 0 C3 1 -0.197333 1.010314 0.688595 11.00000 0.01687 0.02140 = 0.02223 0.00531 -0.00076 -0.00280 AFIX 33 H3A 2 -0.148822 0.997546 0.737161 11.00000 -1.50000 H3B 2 -0.154181 0.971024 0.647252 11.00000 -1.50000 H3C 2 -0.294157 0.990249 0.693837 11.00000 -1.50000 AFIX 0 C4 1 -0.407318 1.132346 0.588052 11.00000 0.01630 0.03256 = 0.02593 0.00221 -0.00596 -0.00376 AFIX 33 H4A 2 -0.446045 1.105969 0.636171 11.00000 -1.50000 H4B 2 -0.424194 1.084019 0.546324 11.00000 -1.50000 H4C 2 -0.451234 1.196985 0.575536 11.00000 -1.50000 AFIX 0 C5 1 -0.179100 1.182750 0.540152 11.00000 0.02150 0.01201 = 0.01587 -0.00118 -0.00073 0.00196 C6 1 -0.030032 1.181021 0.566508 11.00000 0.01925 0.01486 = 0.01405 0.00333 0.00025 -0.00150 AFIX 13 H6 2 0.010009 1.250436 0.562336 11.00000 -1.20000 AFIX 0 C7 1 0.057014 1.106919 0.518923 11.00000 0.01948 0.02188 = 0.01755 0.00023 0.00247 -0.00125 AFIX 23 H7A 2 0.057690 1.129955 0.464656 11.00000 -1.20000 H7B 2 0.153199 1.109236 0.537956 11.00000 -1.20000 AFIX 0 C8 1 0.007587 0.998357 0.521185 11.00000 0.02332 0.01653 = 0.01789 -0.00271 0.00372 0.00149 C9 1 0.076905 0.926592 0.564985 11.00000 0.02672 0.02741 = 0.02866 -0.00009 0.00089 0.00694 AFIX 43 H9 2 0.157986 0.945402 0.592149 11.00000 -1.20000 AFIX 0 C10 1 0.029453 0.827947 0.569616 11.00000 0.04538 0.02340 = 0.03529 0.00477 0.00451 0.01244 AFIX 43 H10 2 0.078665 0.779706 0.599394 11.00000 -1.20000 AFIX 0 C11 1 -0.089290 0.799421 0.531053 11.00000 0.05564 0.01574 = 0.03267 -0.00347 0.00788 0.00002 AFIX 43 H11 2 -0.122623 0.732129 0.535073 11.00000 -1.20000 AFIX 0 C12 1 -0.158953 0.869377 0.486722 11.00000 0.04485 0.02256 = 0.02727 -0.00354 -0.00101 -0.00847 AFIX 43 H12 2 -0.240016 0.849914 0.459809 11.00000 -1.20000 AFIX 0 C13 1 -0.111117 0.968236 0.481232 11.00000 0.03033 0.01921 = 0.01974 -0.00141 -0.00251 -0.00178 AFIX 43 H13 2 -0.159260 1.015666 0.450178 11.00000 -1.20000 AFIX 0 C14 1 0.048977 1.165265 0.701102 11.00000 0.01775 0.01818 = 0.01654 0.00229 -0.00124 0.00035 AFIX 43 H14 2 0.028556 1.139851 0.751004 11.00000 -1.20000 AFIX 0 C15 1 0.179367 1.212808 0.691061 11.00000 0.01740 0.01887 = 0.01656 0.00092 -0.00097 -0.00197 AFIX 43 H15 2 0.211967 1.232135 0.641594 11.00000 -1.20000 AFIX 0 C16 1 0.254376 1.229048 0.755400 11.00000 0.01620 0.01860 = 0.01977 0.00235 0.00085 -0.00150 AFIX 43 H16 2 0.223811 1.196125 0.800942 11.00000 -1.20000 AFIX 0 C17 1 0.377476 1.291845 0.762393 11.00000 0.01446 0.01604 = 0.01971 -0.00264 -0.00028 0.00109 C18 1 0.440637 1.299406 0.834884 11.00000 0.01913 0.02512 = 0.01866 -0.00015 -0.00215 -0.00048 AFIX 43 H18 2 0.408218 1.259288 0.876502 11.00000 -1.20000 AFIX 0 C19 1 0.550679 1.365468 0.846138 11.00000 0.02101 0.02967 = 0.02285 -0.00549 -0.00582 -0.00130 AFIX 43 H19 2 0.593479 1.370468 0.895225 11.00000 -1.20000 AFIX 0 C20 1 0.597353 1.424025 0.784932 11.00000 0.01674 0.02668 = 0.03039 -0.00694 0.00100 -0.00478 AFIX 43 H20 2 0.671874 1.469551 0.792492 11.00000 -1.20000 AFIX 0 C21 1 0.535750 1.416517 0.712560 11.00000 0.02106 0.02377 = 0.02567 -0.00004 0.00397 -0.00343 AFIX 43 H21 2 0.568775 1.456458 0.670992 11.00000 -1.20000 AFIX 0 C22 1 0.426208 1.350703 0.701262 11.00000 0.01831 0.02084 = 0.01883 -0.00106 0.00072 -0.00009 AFIX 43 H22 2 0.384272 1.345621 0.651948 11.00000 -1.20000 AFIX 0 N1 3 -0.044562 1.153399 0.648483 11.00000 0.01571 0.01424 = 0.01498 0.00123 0.00017 -0.00124 N2 3 -0.259423 1.147303 0.597156 11.00000 0.01545 0.01693 = 0.01820 0.00167 -0.00429 -0.00242 O1 4 -0.216333 1.209281 0.475952 11.00000 0.02682 0.02022 = 0.01732 0.00348 -0.00554 0.00087 F1 5 0.099473 0.972028 0.796323 11.00000 0.03671 0.03262 = 0.01994 -0.00260 0.00024 0.00980 F2 5 0.001650 1.088868 0.873995 11.00000 0.03301 0.02233 = 0.02877 0.00314 0.00533 0.00873 F3 5 0.229835 1.053513 0.884579 11.00000 0.02625 0.02487 = 0.03730 0.00580 0.00209 -0.00669 F4 5 0.083749 1.004982 0.978540 11.00000 0.04726 0.04176 = 0.01699 0.00477 0.00011 -0.01022 F5 5 0.180139 0.887110 0.900276 11.00000 0.03222 0.02091 = 0.04625 0.01060 -0.00911 0.00339 F6 5 -0.048053 0.922990 0.890437 11.00000 0.02617 0.03016 = 0.04162 0.00563 -0.00384 -0.00960 P1 6 0.091176 0.987759 0.887887 11.00000 0.02308 0.01759 = 0.01815 0.00407 -0.00087 -0.00015 HKLF 4 Covalent radii and connectivity table for 2008src0764 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 P 1.100 C1 - N2 N1 C3 C2 C2 - C1 C3 - C1 C4 - N2 C5 - O1 N2 C6 C6 - N1 C5 C7 C7 - C8 C6 C8 - C9 C13 C7 C9 - C10 C8 C10 - C11 C9 C11 - C12 C10 C12 - C11 C13 C13 - C12 C8 C14 - N1 C15 C15 - C16 C14 C16 - C15 C17 C17 - C22 C18 C16 C18 - C19 C17 C19 - C20 C18 C20 - C19 C21 C21 - C22 C20 C22 - C21 C17 N1 - C14 C6 C1 N2 - C5 C4 C1 O1 - C5 F1 - P1 F2 - P1 F3 - P1 F4 - P1 F5 - P1 F6 - P1 P1 - F4 F6 F5 F3 F1 F2 21554 Reflections read, of which 58 rejected -12 =< h =< 12, -15 =< k =< 17, -22 =< l =< 20, Max. 2-theta = 54.99 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -7 6 4 14.66 0.70 4 5.92 5 4 15 48.44 1.60 6 8.34 2 Inconsistent equivalents 5096 Unique reflections, of which 0 suppressed R(int) = 0.0376 R(sigma) = 0.0358 Friedel opposites not merged Maximum memory for data reduction = 2692 / 50757 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 = 3509 / 362880 wR2 = 0.0912 before cycle 1 for 5096 data and 289 / 289 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0439 * P )^2 + 0.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.85965 0.00119 -1.608 OSF Mean shift/esd = 0.158 Maximum = -1.608 for OSF Max. shift = 0.001 A for C11 Max. dU = 0.000 for C1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3509 / 362880 wR2 = 0.0911 before cycle 2 for 5096 data and 289 / 289 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0439 * P )^2 + 0.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.85897 0.00119 -0.578 OSF Mean shift/esd = 0.052 Maximum = -0.578 for OSF Max. shift = 0.000 A for C11 Max. dU = 0.000 for C1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3509 / 362880 wR2 = 0.0911 before cycle 3 for 5096 data and 289 / 289 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0439 * P )^2 + 0.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.85896 0.00119 -0.004 OSF Mean shift/esd = 0.001 Maximum = 0.014 for U23 C22 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3509 / 362880 wR2 = 0.0911 before cycle 4 for 5096 data and 289 / 289 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0439 * P )^2 + 0.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.85896 0.00119 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.003 for x C10 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C11 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A -0.1947 1.1702 0.7828 33 0.980 0.000 C2 C1 H2A H2B -0.3422 1.1762 0.7417 33 0.980 0.000 C2 C1 H2A H2C -0.2269 1.2593 0.7231 33 0.980 0.000 C2 C1 H2A H3A -0.1488 0.9975 0.7371 33 0.980 0.000 C3 C1 H3A H3B -0.1541 0.9710 0.6472 33 0.980 0.000 C3 C1 H3A H3C -0.2941 0.9902 0.6938 33 0.980 0.000 C3 C1 H3A H4A -0.4461 1.1060 0.6362 33 0.980 0.000 C4 N2 H4A H4B -0.4243 1.0841 0.5463 33 0.980 0.000 C4 N2 H4A H4C -0.4512 1.1971 0.5756 33 0.980 0.000 C4 N2 H4A H6 0.0100 1.2504 0.5624 13 1.000 0.000 C6 N1 C5 C7 H7A 0.0577 1.1299 0.4647 23 0.990 0.000 C7 C8 C6 H7B 0.1532 1.1092 0.5380 23 0.990 0.000 C7 C8 C6 H9 0.1581 0.9454 0.5921 43 0.950 0.000 C9 C10 C8 H10 0.0786 0.7797 0.5995 43 0.950 0.000 C10 C11 C9 H11 -0.1224 0.7321 0.5351 43 0.950 0.000 C11 C12 C10 H12 -0.2400 0.8498 0.4598 43 0.950 0.000 C12 C11 C13 H13 -0.1592 1.0157 0.4502 43 0.950 0.000 C13 C12 C8 H14 0.0286 1.1398 0.7510 43 0.950 0.000 C14 N1 C15 H15 0.2120 1.2321 0.6416 43 0.950 0.000 C15 C16 C14 H16 0.2238 1.1962 0.8010 43 0.950 0.000 C16 C15 C17 H18 0.4083 1.2593 0.8765 43 0.950 0.000 C18 C19 C17 H19 0.5935 1.3704 0.8952 43 0.950 0.000 C19 C20 C18 H20 0.6718 1.4696 0.7925 43 0.950 0.000 C20 C19 C21 H21 0.5687 1.4565 0.6710 43 0.950 0.000 C21 C22 C20 H22 0.3844 1.3457 0.6519 43 0.950 0.000 C22 C21 C17 2008src0764 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.18929 1.12255 0.66920 1.00000 0.01237 0.01945 0.01522 0.00155 -0.00099 -0.00173 0.01568 0.00298 0.00017 0.00014 0.00010 0.00000 0.00074 0.00088 0.00080 0.00069 0.00063 0.00068 0.00034 C2 -0.24307 1.18791 0.73510 1.00000 0.01945 0.02857 0.01949 -0.00236 0.00170 0.00212 0.02250 0.00335 0.00020 0.00016 0.00010 0.00000 0.00088 0.00104 0.00087 0.00079 0.00072 0.00079 0.00040 H2A -0.19465 1.17017 0.78278 1.00000 0.03375 0.00000 0.00000 H2B -0.34216 1.17624 0.74169 1.00000 0.03375 0.00000 0.00000 H2C -0.22693 1.25931 0.72314 1.00000 0.03375 0.00000 0.00000 C3 -0.19730 1.01029 0.68857 1.00000 0.01657 0.02111 0.02223 0.00539 -0.00073 -0.00282 0.01997 0.00317 0.00018 0.00014 0.00010 0.00000 0.00079 0.00092 0.00084 0.00077 0.00066 0.00074 0.00037 H3A -0.14880 0.99750 0.73713 1.00000 0.02995 0.00000 0.00000 H3B -0.15414 0.97103 0.64722 1.00000 0.02995 0.00000 0.00000 H3C -0.29413 0.99021 0.69380 1.00000 0.02995 0.00000 0.00000 C4 -0.40731 1.13242 0.58807 1.00000 0.01622 0.03233 0.02590 0.00224 -0.00589 -0.00390 0.02482 0.00332 0.00019 0.00016 0.00011 0.00000 0.00085 0.00107 0.00094 0.00082 0.00073 0.00082 0.00041 H4A -0.44606 1.10604 0.63618 1.00000 0.03723 0.00000 0.00000 H4B -0.42426 1.08413 0.54633 1.00000 0.03723 0.00000 0.00000 H4C -0.45115 1.19709 0.57558 1.00000 0.03723 0.00000 0.00000 C5 -0.17901 1.18276 0.54017 1.00000 0.02109 0.01184 0.01573 -0.00101 -0.00061 0.00190 0.01622 0.00301 0.00019 0.00013 0.00010 0.00000 0.00086 0.00078 0.00081 0.00066 0.00067 0.00068 0.00034 C6 -0.03008 1.18098 0.56652 1.00000 0.01895 0.01461 0.01381 0.00338 0.00024 -0.00148 0.01579 0.00304 0.00018 0.00013 0.00010 0.00000 0.00082 0.00082 0.00078 0.00065 0.00063 0.00067 0.00034 H6 0.00997 1.25040 0.56236 1.00000 0.01895 0.00000 0.00000 C7 0.05701 1.10691 0.51892 1.00000 0.01921 0.02164 0.01728 0.00007 0.00229 -0.00131 0.01938 0.00315 0.00019 0.00014 0.00010 0.00000 0.00084 0.00091 0.00082 0.00071 0.00068 0.00072 0.00037 H7A 0.05769 1.12994 0.46466 1.00000 0.02325 0.00000 0.00000 H7B 0.15319 1.10922 0.53796 1.00000 0.02325 0.00000 0.00000 C8 0.00752 0.99834 0.52120 1.00000 0.02316 0.01631 0.01753 -0.00265 0.00377 0.00138 0.01900 0.00315 0.00019 0.00014 0.00010 0.00000 0.00086 0.00086 0.00080 0.00072 0.00065 0.00072 0.00036 C9 0.07693 0.92661 0.56497 1.00000 0.02647 0.02700 0.02858 -0.00012 0.00086 0.00676 0.02735 0.00378 0.00022 0.00016 0.00012 0.00000 0.00098 0.00103 0.00100 0.00084 0.00081 0.00085 0.00043 H9 0.15809 0.94542 0.59207 1.00000 0.03282 0.00000 0.00000 C10 0.02942 0.82795 0.56965 1.00000 0.04505 0.02299 0.03508 0.00482 0.00445 0.01228 0.03437 0.00431 0.00026 0.00016 0.00013 0.00000 0.00131 0.00109 0.00118 0.00091 0.00100 0.00099 0.00052 H10 0.07856 0.77974 0.59950 1.00000 0.04125 0.00000 0.00000 C11 -0.08915 0.79943 0.53108 1.00000 0.05524 0.01551 0.03249 -0.00325 0.00767 -0.00002 0.03441 0.00408 0.00028 0.00015 0.00013 0.00000 0.00145 0.00095 0.00111 0.00084 0.00107 0.00098 0.00051 H11 -0.12240 0.73212 0.53509 1.00000 0.04130 0.00000 0.00000 C12 -0.15894 0.86932 0.48669 1.00000 0.04464 0.02217 0.02710 -0.00356 -0.00094 -0.00833 0.03130 0.00377 0.00025 0.00016 0.00012 0.00000 0.00126 0.00103 0.00104 0.00087 0.00091 0.00092 0.00048 H12 -0.23996 0.84981 0.45975 1.00000 0.03756 0.00000 0.00000 C13 -0.11107 0.96827 0.48125 1.00000 0.03018 0.01857 0.01982 -0.00141 -0.00247 -0.00179 0.02286 0.00330 0.00021 0.00014 0.00011 0.00000 0.00098 0.00091 0.00089 0.00071 0.00076 0.00079 0.00039 H13 -0.15921 1.01573 0.45021 1.00000 0.02743 0.00000 0.00000 C14 0.04899 1.16523 0.70111 1.00000 0.01753 0.01794 0.01624 0.00236 -0.00137 0.00040 0.01723 0.00305 0.00018 0.00013 0.00010 0.00000 0.00080 0.00087 0.00081 0.00069 0.00064 0.00070 0.00035 H14 0.02858 1.13980 0.75101 1.00000 0.02068 0.00000 0.00000 C15 0.17938 1.21276 0.69106 1.00000 0.01701 0.01867 0.01631 0.00108 -0.00096 -0.00190 0.01733 0.00308 0.00018 0.00014 0.00010 0.00000 0.00080 0.00089 0.00079 0.00071 0.00066 0.00071 0.00035 H15 0.21199 1.23206 0.64159 1.00000 0.02079 0.00000 0.00000 C16 0.25440 1.22905 0.75543 1.00000 0.01611 0.01829 0.01956 0.00230 0.00078 -0.00136 0.01799 0.00308 0.00018 0.00014 0.00010 0.00000 0.00082 0.00087 0.00086 0.00072 0.00069 0.00069 0.00036 H16 0.22382 1.19615 0.80098 1.00000 0.02159 0.00000 0.00000 C17 0.37747 1.29181 0.76241 1.00000 0.01433 0.01587 0.01935 -0.00229 -0.00020 0.00109 0.01652 0.00302 0.00017 0.00013 0.00010 0.00000 0.00078 0.00086 0.00084 0.00070 0.00065 0.00066 0.00035 C18 0.44069 1.29938 0.83490 1.00000 0.01886 0.02487 0.01849 -0.00017 -0.00211 -0.00046 0.02074 0.00318 0.00019 0.00015 0.00010 0.00000 0.00084 0.00095 0.00083 0.00074 0.00070 0.00073 0.00037 H18 0.40833 1.25925 0.87653 1.00000 0.02488 0.00000 0.00000 C19 0.55067 1.36543 0.84611 1.00000 0.02082 0.02954 0.02264 -0.00544 -0.00577 -0.00119 0.02433 0.00327 0.00020 0.00016 0.00011 0.00000 0.00089 0.00105 0.00092 0.00083 0.00074 0.00081 0.00041 H19 0.59349 1.37042 0.89519 1.00000 0.02920 0.00000 0.00000 C20 0.59734 1.42403 0.78493 1.00000 0.01659 0.02642 0.03004 -0.00660 0.00107 -0.00481 0.02435 0.00328 0.00019 0.00015 0.00011 0.00000 0.00082 0.00102 0.00100 0.00082 0.00076 0.00081 0.00041 H20 0.67185 1.46957 0.79250 1.00000 0.02922 0.00000 0.00000 C21 0.53570 1.41653 0.71258 1.00000 0.02086 0.02351 0.02542 -0.00008 0.00396 -0.00345 0.02326 0.00336 0.00019 0.00015 0.00011 0.00000 0.00087 0.00099 0.00095 0.00078 0.00074 0.00079 0.00040 H21 0.56869 1.45649 0.67102 1.00000 0.02791 0.00000 0.00000 C22 0.42627 1.35076 0.70127 1.00000 0.01812 0.02060 0.01834 -0.00103 0.00083 -0.00014 0.01902 0.00318 0.00018 0.00014 0.00010 0.00000 0.00084 0.00091 0.00082 0.00072 0.00067 0.00073 0.00036 H22 0.38435 1.34570 0.65195 1.00000 0.02282 0.00000 0.00000 N1 -0.04458 1.15338 0.64848 1.00000 0.01532 0.01419 0.01473 0.00112 0.00005 -0.00139 0.01475 0.00250 0.00015 0.00011 0.00008 0.00000 0.00067 0.00068 0.00068 0.00056 0.00053 0.00058 0.00029 N2 -0.25942 1.14727 0.59717 1.00000 0.01521 0.01675 0.01781 0.00165 -0.00425 -0.00239 0.01659 0.00249 0.00015 0.00012 0.00008 0.00000 0.00068 0.00074 0.00073 0.00059 0.00057 0.00059 0.00031 O1 -0.21634 1.20924 0.47595 1.00000 0.02652 0.02007 0.01701 0.00344 -0.00565 0.00079 0.02120 0.00225 0.00014 0.00010 0.00007 0.00000 0.00069 0.00066 0.00060 0.00052 0.00051 0.00054 0.00028 F1 0.09949 0.97201 0.79634 1.00000 0.03667 0.03231 0.01968 -0.00259 0.00036 0.00972 0.02955 0.00208 0.00013 0.00009 0.00006 0.00000 0.00065 0.00065 0.00055 0.00047 0.00048 0.00057 0.00028 F2 0.00166 1.08888 0.87397 1.00000 0.03297 0.02183 0.02840 0.00298 0.00524 0.00874 0.02773 0.00212 0.00012 0.00009 0.00007 0.00000 0.00063 0.00059 0.00062 0.00047 0.00049 0.00049 0.00027 F3 0.22984 1.05349 0.88458 1.00000 0.02611 0.02452 0.03712 0.00594 0.00214 -0.00683 0.02925 0.00213 0.00012 0.00009 0.00007 0.00000 0.00057 0.00061 0.00064 0.00052 0.00052 0.00048 0.00027 F4 0.08372 1.00500 0.97852 1.00000 0.04704 0.04144 0.01679 0.00482 0.00011 -0.01027 0.03509 0.00217 0.00014 0.00010 0.00006 0.00000 0.00075 0.00074 0.00054 0.00052 0.00050 0.00066 0.00030 F5 0.18008 0.88712 0.90030 1.00000 0.03209 0.02060 0.04590 0.01055 -0.00912 0.00330 0.03286 0.00221 0.00013 0.00009 0.00008 0.00000 0.00064 0.00058 0.00074 0.00055 0.00056 0.00052 0.00029 F6 -0.04806 0.92303 0.89041 1.00000 0.02598 0.02993 0.04125 0.00573 -0.00399 -0.00964 0.03239 0.00212 0.00012 0.00009 0.00008 0.00000 0.00058 0.00063 0.00069 0.00057 0.00055 0.00052 0.00028 P1 0.09116 0.98776 0.88789 1.00000 0.02294 0.01737 0.01800 0.00413 -0.00085 -0.00015 0.01944 0.00083 0.00005 0.00004 0.00003 0.00000 0.00023 0.00023 0.00022 0.00018 0.00017 0.00019 0.00011 Final Structure Factor Calculation for 2008src0764 in P2(1)2(1)2(1) Total number of l.s. parameters = 289 Maximum vector length = 511 Memory required = 3222 / 27090 wR2 = 0.0911 before cycle 5 for 5096 data and 2 / 289 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0439 * P )^2 + 0.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0362 for 4656 Fo > 4sig(Fo) and 0.0418 for all 5096 data wR2 = 0.0911, GooF = S = 1.058, Restrained GooF = 1.058 for all data Flack x parameter = -0.0339 with esd 0.0848 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 32.00 for non-hydrogen and 25.00 for hydrogen atoms Principal mean square atomic displacements U 0.0204 0.0148 0.0118 C1 0.0294 0.0212 0.0169 C2 0.0276 0.0177 0.0146 C3 0.0349 0.0265 0.0131 C4 0.0216 0.0158 0.0113 C5 0.0196 0.0172 0.0106 C6 0.0224 0.0201 0.0157 C7 0.0251 0.0190 0.0130 C8 0.0336 0.0286 0.0199 C9 0.0526 0.0334 0.0171 C10 0.0576 0.0308 0.0149 C11 0.0474 0.0286 0.0179 C12 0.0309 0.0206 0.0170 C13 0.0197 0.0179 0.0141 C14 0.0204 0.0160 0.0156 C15 0.0213 0.0179 0.0148 C16 0.0206 0.0154 0.0136 C17 0.0249 0.0208 0.0165 C18 0.0328 0.0257 0.0145 C19 0.0358 0.0228 0.0144 C20 0.0285 0.0242 0.0171 C21 0.0211 0.0187 0.0173 C22 0.0165 0.0150 0.0128 N1 0.0223 0.0156 0.0118 N2 0.0292 0.0216 0.0127 O1 0.0445 0.0254 0.0187 F1 0.0407 0.0254 0.0170 F2 0.0395 0.0315 0.0167 F3 0.0551 0.0344 0.0157 F4 0.0526 0.0316 0.0144 F5 0.0467 0.0324 0.0181 F6 0.0233 0.0215 0.0135 P1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.036 0.054 0.070 0.087 0.104 0.125 0.152 0.197 0.269 1.000 Number in group 525. 507. 514. 508. 516. 488. 511. 504. 512. 511. GooF 1.034 1.120 1.101 1.025 1.111 1.098 0.970 0.939 1.028 1.134 K 0.944 0.923 0.957 0.977 0.992 1.004 1.009 1.017 1.019 0.977 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 520. 505. 512. 502. 516. 502. 517. 501. 508. 513. GooF 0.970 0.906 0.925 1.006 0.939 0.872 0.874 0.944 1.284 1.614 K 0.998 1.011 1.000 0.985 0.998 1.007 1.017 1.014 1.011 0.963 R1 0.086 0.075 0.071 0.060 0.047 0.031 0.026 0.025 0.029 0.034 Recommended weighting scheme: WGHT 0.0413 0.8115 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) 1 0 7 115.85 230.26 7.43 0.122 2.40 0 8 1 60.00 22.98 5.57 0.039 1.65 0 6 5 93.57 51.55 4.72 0.058 1.86 1 7 0 436.01 326.14 4.41 0.145 1.86 -1 6 4 199.12 135.05 4.37 0.094 1.93 3 0 2 225.53 159.54 4.30 0.102 3.03 -1 6 8 114.33 70.88 4.29 0.068 1.53 3 5 0 1173.78 1474.43 4.15 0.309 2.05 1 6 8 115.14 72.57 4.02 0.069 1.53 1 6 4 195.25 133.72 3.91 0.093 1.93 0 1 9 258.24 190.12 3.88 0.111 1.91 2 0 1 12890.25 15443.13 3.69 1.000 4.67 -4 1 9 241.36 179.23 3.69 0.108 1.50 0 3 8 64.09 101.46 3.69 0.081 1.95 2 0 9 1578.45 1917.02 3.65 0.352 1.79 5 0 3 31.67 14.18 3.63 0.030 1.84 0 1 3 1192.01 1466.89 3.61 0.308 5.30 2 6 0 226.24 168.85 3.61 0.105 2.01 -8 13 3 80.78 147.77 3.60 0.098 0.77 3 3 4 93.55 134.74 3.49 0.093 2.23 -7 6 4 19.87 55.90 3.48 0.060 1.13 4 1 9 236.75 178.74 3.47 0.108 1.50 0 5 3 344.45 436.39 3.43 0.168 2.41 1 4 8 415.96 330.40 3.40 0.146 1.78 8 6 0 28.16 52.59 3.35 0.058 1.06 2 0 3 8.50 1.58 3.34 0.010 3.72 0 9 2 898.49 739.57 3.34 0.219 1.45 -1 1 2 1931.65 2401.86 3.25 0.394 5.81 -1 2 2 12981.27 15284.18 3.23 0.995 4.63 1 0 4 9.48 2.02 3.22 0.011 3.96 0 5 10 253.21 327.53 3.21 0.146 1.45 4 0 7 146.05 196.97 3.20 0.113 1.73 -10 5 4 52.15 81.12 3.18 0.072 0.89 7 2 0 216.69 160.82 3.18 0.102 1.36 10 2 13 11.66 30.61 3.18 0.045 0.78 -5 8 14 12.94 44.48 3.16 0.054 0.88 1 5 6 286.62 224.84 3.15 0.121 1.91 1 2 2 12859.10 15190.69 3.14 0.992 4.63 6 0 3 31.08 14.72 3.14 0.031 1.56 0 7 8 68.83 44.25 3.13 0.054 1.43 0 2 11 20.36 39.74 3.11 0.051 1.53 -2 5 2 365.19 295.06 3.10 0.138 2.24 2 6 5 57.25 85.02 3.09 0.074 1.74 0 10 5 316.93 249.33 3.07 0.127 1.24 0 2 1 5.78 16.36 3.06 0.033 6.18 -1 5 6 285.99 224.01 3.06 0.120 1.91 4 12 10 94.09 139.84 3.03 0.095 0.87 1 2 8 39.20 22.99 3.01 0.039 2.02 4 4 7 58.17 36.47 3.00 0.049 1.54 -1 4 8 412.73 336.37 2.99 0.148 1.78 Bond lengths and angles C1 - Distance Angles N2 1.4604 (0.0022) N1 1.5050 (0.0021) 99.72 (0.13) C3 1.5253 (0.0025) 112.53 (0.15) 111.37 (0.14) C2 1.5258 (0.0025) 110.82 (0.15) 110.13 (0.14) 111.69 (0.15) C1 - N2 N1 C3 C2 - Distance Angles C1 1.5258 (0.0025) C2 - C3 - Distance Angles C1 1.5253 (0.0025) C3 - C4 - Distance Angles N2 1.4562 (0.0022) C4 - C5 - Distance Angles O1 1.2234 (0.0021) N2 1.3443 (0.0022) 126.80 (0.17) C6 1.5151 (0.0025) 124.16 (0.16) 108.99 (0.14) C5 - O1 N2 C6 - Distance Angles N1 1.4754 (0.0021) C5 1.5151 (0.0025) 101.77 (0.13) C7 1.5352 (0.0025) 114.41 (0.15) 111.83 (0.14) C6 - N1 C5 C7 - Distance Angles C8 1.5154 (0.0025) C6 1.5352 (0.0025) 114.66 (0.14) C7 - C8 C8 - Distance Angles C9 1.3897 (0.0028) C13 1.4007 (0.0027) 118.31 (0.18) C7 1.5154 (0.0025) 120.57 (0.17) 121.10 (0.17) C8 - C9 C13 C9 - Distance Angles C10 1.3871 (0.0030) C8 1.3897 (0.0028) 120.95 (0.20) C9 - C10 C10 - Distance Angles C11 1.3830 (0.0035) C9 1.3871 (0.0030) 120.31 (0.20) C10 - C11 C11 - Distance Angles C12 1.3810 (0.0032) C10 1.3830 (0.0035) 119.65 (0.20) C11 - C12 C12 - Distance Angles C11 1.3810 (0.0032) C13 1.3927 (0.0028) 120.29 (0.21) C12 - C11 C13 - Distance Angles C12 1.3927 (0.0028) C8 1.4007 (0.0027) 120.48 (0.19) C13 - C12 C14 - Distance Angles N1 1.2970 (0.0022) C15 1.4230 (0.0024) 126.07 (0.16) C14 - N1 C15 - Distance Angles C16 1.3505 (0.0024) C14 1.4230 (0.0024) 116.60 (0.16) C15 - C16 C16 - Distance Angles C15 1.3505 (0.0024) C17 1.4591 (0.0024) 126.88 (0.16) C16 - C15 C17 - Distance Angles C22 1.3996 (0.0025) C18 1.4032 (0.0024) 119.49 (0.17) C16 1.4591 (0.0024) 122.07 (0.16) 118.20 (0.16) C17 - C22 C18 C18 - Distance Angles C19 1.3926 (0.0026) C17 1.4032 (0.0024) 120.31 (0.17) C18 - C19 C19 - Distance Angles C20 1.3906 (0.0029) C18 1.3926 (0.0026) 119.52 (0.17) C19 - C20 C20 - Distance Angles C19 1.3906 (0.0029) C21 1.3943 (0.0027) 120.56 (0.18) C20 - C19 C21 - Distance Angles C22 1.3865 (0.0026) C20 1.3943 (0.0027) 120.02 (0.18) C21 - C22 C22 - Distance Angles C21 1.3865 (0.0026) C17 1.3996 (0.0025) 120.09 (0.17) C22 - C21 N1 - Distance Angles C14 1.2970 (0.0022) C6 1.4754 (0.0021) 125.62 (0.15) C1 1.5050 (0.0021) 121.12 (0.14) 112.73 (0.13) N1 - C14 C6 N2 - Distance Angles C5 1.3443 (0.0022) C4 1.4562 (0.0022) 122.59 (0.15) C1 1.4604 (0.0022) 115.98 (0.14) 121.42 (0.14) N2 - C5 C4 O1 - Distance Angles C5 1.2234 (0.0021) O1 - F1 - Distance Angles P1 1.6045 (0.0012) F1 - F2 - Distance Angles P1 1.6133 (0.0012) F2 - F3 - Distance Angles P1 1.6027 (0.0012) F3 - F4 - Distance Angles P1 1.5912 (0.0012) F4 - F5 - Distance Angles P1 1.6012 (0.0012) F5 - F6 - Distance Angles P1 1.5995 (0.0012) F6 - P1 - Distance Angles F4 1.5912 (0.0012) F6 1.5995 (0.0012) 90.66 (0.07) F5 1.6012 (0.0012) 90.61 (0.07) 90.31 (0.07) F3 1.6027 (0.0012) 89.75 (0.07) 179.30 (0.08) 90.26 (0.07) F1 1.6045 (0.0012) 179.17 (0.08) 90.00 (0.07) 89.89 (0.07) 89.59 (0.07) F2 1.6133 (0.0012) 90.26 (0.07) 89.67 (0.07) 179.12 (0.07) 89.76 (0.07) 89.23 (0.06) P1 - F4 F6 F5 F3 F1 FMAP and GRID set by program FMAP 2 3 22 GRID -1.316 -2 -2 1.316 2 2 R1 = 0.0386 for 2881 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.34 at 0.9306 0.8576 0.0259 [ 0.85 A from H4B ] Deepest hole -0.36 at 0.9225 0.9275 0.0503 [ 0.17 A from H4B ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3158 / 23734 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.4306 1.1424 0.5259 1.00000 0.05 0.34 0.85 H4B 1.11 C4 1.14 H4C 1.98 H4A Q2 1 -0.4359 1.0595 0.6090 1.00000 0.05 0.31 0.78 H4A 1.07 C4 1.14 H4B 1.92 H4C Q3 1 -0.4541 1.1843 0.6163 1.00000 0.05 0.29 0.73 H4C 0.96 C4 1.09 H4A 1.82 H4B Q4 1 -0.5541 1.1590 0.6912 1.00000 0.05 0.18 1.58 H4A 2.25 H2B 2.25 C17 2.30 H4C Q5 1 -0.0963 1.1617 0.5522 1.00000 0.05 0.18 0.73 C6 0.87 C5 1.57 H6 1.75 N1 Q6 1 0.0237 1.0437 0.5234 1.00000 0.05 0.18 0.62 C8 0.90 C7 1.55 H7B 1.56 H7A Q7 1 -0.1743 0.8433 0.6703 1.00000 0.05 0.16 1.75 H3B 2.07 H16 2.13 C16 2.24 C3 Q8 1 -0.2344 1.0017 0.8379 1.00000 0.05 0.16 1.94 H3A 2.22 H13 2.28 F6 2.46 H2A Q9 1 -0.0436 0.9819 0.5016 1.00000 0.05 0.16 0.64 C8 0.76 C13 1.50 H13 1.76 C9 Q10 1 -0.2680 1.2683 0.6056 1.00000 0.05 0.16 1.61 N2 1.79 F5 1.82 C5 2.08 H4C Q11 1 0.2655 1.0685 0.6028 1.00000 0.05 0.16 1.66 H7B 1.94 H9 2.32 H20 2.33 H15 Q12 1 0.2790 1.3523 0.9226 1.00000 0.05 0.16 1.93 H18 1.97 C12 2.08 H12 2.13 C11 Q13 1 -0.3671 1.0103 0.7131 1.00000 0.05 0.15 0.83 H3C 1.70 C3 1.99 H4A 2.16 H3A Q14 1 -0.5617 1.0835 0.7026 1.00000 0.05 0.15 1.64 H4A 1.85 H20 2.15 C20 2.55 H2B Q15 1 0.5130 1.5190 0.7892 1.00000 0.05 0.15 1.50 C20 1.67 H20 1.85 H4A 1.91 C21 Q16 1 -0.0519 1.1319 0.9379 1.00000 0.05 0.15 1.35 F2 2.07 H12 2.08 H10 2.20 H11 Q17 1 0.2265 0.7964 0.8705 1.00000 0.05 0.15 1.38 F5 1.70 H2C 2.08 N2 2.21 C5 Q18 1 0.0205 1.1429 0.5480 1.00000 0.05 0.15 0.77 C6 0.78 C7 1.37 H7B 1.45 H6 Q19 1 0.1952 1.0499 0.5146 1.00000 0.05 0.15 0.97 H7B 1.54 C7 1.91 H7A 1.95 C8 Q20 1 0.2916 0.9202 0.8953 1.00000 0.05 0.15 1.17 F5 1.84 H21 1.87 F3 2.01 H7A Shortest distances between peaks (including symmetry equivalents) 10 17 0.69 14 15 0.98 4 14 1.02 6 9 1.11 5 18 1.16 6 18 1.38 13 15 1.42 3 4 1.66 2 3 1.66 6 19 1.67 1 3 1.68 11 19 1.69 17 20 1.81 1 2 1.81 7 12 1.91 4 15 1.92 2 15 1.99 5 6 2.01 10 20 2.02 2 13 2.03 2 14 2.06 19 20 2.11 3 10 2.13 13 14 2.13 18 19 2.17 2 4 2.25 3 14 2.26 9 18 2.36 5 10 2.37 11 14 2.42 9 19 2.49 8 13 2.52 5 17 2.56 5 9 2.59 4 11 2.62 3 17 2.67 1 10 2.68 4 13 2.70 6 11 2.74 11 18 2.74 3 15 2.79 6 20 2.89 2 11 2.90 11 15 2.93 12 16 2.93 3 13 2.97 7 13 2.99 Time profile in seconds ----------------------- 0.13: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 3.91: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.08: Structure factors and derivatives 2.28: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.50: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0764 finished at 20:10:21 Total CPU time: 9.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++