+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0671 started at 17:58:27 on 14-Jul-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0671 in C2 CELL 0.71073 18.9488 5.6024 20.7934 90.000 90.355 90.000 ZERR 4.00 0.0006 0.0001 0.0006 0.000 0.002 0.000 LATT -7 SYMM - X, Y, - Z SFAC C H O S UNIT 84 104 36 4 V = 2207.36 F(000) = 960.0 Mu = 0.20 mm-1 Cell Wt = 1817.91 Rho = 1.368 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 20 SIZE 0.02 0.02 0.15 ACTA BOND $H WGHT 0.00000 4.98390 L.S. 10 TEMP -153.00 FVAR 0.49973 MOLE 1 C1 1 0.260987 0.917743 0.182550 11.00000 0.02153 0.02270 = 0.01635 0.00032 -0.00063 -0.00231 AFIX 13 H1 2 0.286803 1.063899 0.197144 11.00000 -1.20000 AFIX 0 C2 1 0.309556 0.762440 0.142225 11.00000 0.02292 0.02129 = 0.01577 -0.00010 0.00067 -0.00430 AFIX 13 H2 2 0.284399 0.615795 0.127042 11.00000 -1.20000 AFIX 0 C3 1 0.374551 0.696532 0.182422 11.00000 0.02113 0.01697 = 0.01567 -0.00540 0.00274 0.00115 AFIX 13 H3 2 0.404833 0.840164 0.189924 11.00000 -1.20000 AFIX 0 C4 1 0.352333 0.586954 0.246140 11.00000 0.01826 0.01766 = 0.01972 -0.00072 -0.00010 -0.00094 AFIX 13 H4 2 0.333986 0.421988 0.238433 11.00000 -1.20000 AFIX 0 C5 1 0.296075 0.734249 0.279894 11.00000 0.01760 0.02446 = 0.01600 0.00348 -0.00329 -0.00220 AFIX 13 H5 2 0.316706 0.886375 0.296727 11.00000 -1.20000 AFIX 0 C6 1 0.194992 0.988705 0.145821 11.00000 0.02613 0.02629 = 0.01900 -0.00254 -0.00112 0.00656 AFIX 23 H6A 2 0.206806 1.020144 0.100290 11.00000 -1.20000 H6B 2 0.160235 0.856883 0.147096 11.00000 -1.20000 AFIX 0 C7 1 0.108287 1.173005 0.213436 11.00000 0.02651 0.02431 = 0.01911 0.00164 -0.00626 0.00131 C8 1 0.084716 1.406970 0.239453 11.00000 0.02730 0.02417 = 0.02689 -0.00106 0.00137 0.00352 AFIX 137 H8A 2 0.067868 1.508037 0.204086 11.00000 -1.50000 H8B 2 0.124367 1.485570 0.261290 11.00000 -1.50000 H8C 2 0.046384 1.381423 0.270119 11.00000 -1.50000 AFIX 0 C9 1 0.332732 0.802465 0.028883 11.00000 0.01864 0.02705 = 0.01697 -0.00171 -0.00185 0.00366 C10 1 0.359864 0.972974 -0.020138 11.00000 0.03437 0.02823 = 0.01994 0.00206 0.00776 0.00061 AFIX 137 H10A 2 0.410868 0.950940 -0.024932 11.00000 -1.50000 H10B 2 0.350245 1.136871 -0.006249 11.00000 -1.50000 H10C 2 0.336316 0.943203 -0.061459 11.00000 -1.50000 AFIX 0 C11 1 0.471696 0.575887 0.115585 11.00000 0.01968 0.03070 = 0.01796 -0.00286 -0.00114 0.00581 C12 1 0.505239 0.359195 0.087088 11.00000 0.02799 0.03871 = 0.02682 -0.00792 0.00198 0.00789 AFIX 137 H12A 2 0.544686 0.407523 0.059751 11.00000 -1.50000 H12B 2 0.470299 0.272426 0.061182 11.00000 -1.50000 H12C 2 0.522728 0.255543 0.121645 11.00000 -1.50000 AFIX 0 C13 1 0.437285 0.356647 0.305308 11.00000 0.02201 0.02589 = 0.02287 0.00317 0.00335 0.00235 C14 1 0.495506 0.376613 0.353872 11.00000 0.02590 0.03053 = 0.02748 0.00136 -0.00274 0.00400 AFIX 137 H14A 2 0.476014 0.427838 0.395178 11.00000 -1.50000 H14B 2 0.530186 0.494066 0.339198 11.00000 -1.50000 H14C 2 0.518478 0.221024 0.359072 11.00000 -1.50000 AFIX 0 C15 1 0.198443 0.759328 0.379998 11.00000 0.02325 0.02793 = 0.02303 0.00131 0.00360 0.00114 AFIX 23 H15A 2 0.222063 0.908679 0.393708 11.00000 -1.20000 H15B 2 0.161357 0.799706 0.348067 11.00000 -1.20000 AFIX 0 C16 1 0.166329 0.634962 0.437275 11.00000 0.01713 0.02838 = 0.02107 0.00163 0.00263 0.00314 C17 1 0.126081 0.428756 0.429324 11.00000 0.03149 0.03069 = 0.02118 -0.00142 -0.00243 0.00017 AFIX 43 H17 2 0.117708 0.367408 0.387372 11.00000 -1.20000 AFIX 0 C18 1 0.098191 0.312630 0.482258 11.00000 0.02210 0.03448 = 0.03738 0.00359 -0.00087 -0.00795 AFIX 43 H18 2 0.071185 0.171381 0.476331 11.00000 -1.20000 AFIX 0 C19 1 0.109350 0.400691 0.543682 11.00000 0.02991 0.03561 = 0.02707 0.00943 0.00653 -0.00145 AFIX 43 H19 2 0.090081 0.320960 0.579871 11.00000 -1.20000 AFIX 0 C20 1 0.148979 0.606617 0.551750 11.00000 0.03284 0.03647 = 0.02025 -0.00464 0.00378 0.00225 AFIX 43 H20 2 0.156487 0.668638 0.593760 11.00000 -1.20000 AFIX 0 C21 1 0.177757 0.723058 0.499366 11.00000 0.02622 0.02472 = 0.02736 -0.00202 0.00290 -0.00077 AFIX 43 H21 2 0.205293 0.862942 0.505625 11.00000 -1.20000 AFIX 0 O1 3 0.238838 0.783002 0.236928 11.00000 0.01934 0.02688 = 0.01646 0.00181 0.00035 0.00286 O2 3 0.164846 1.201419 0.174442 11.00000 0.02835 0.02161 = 0.02513 0.00210 0.00558 0.00488 O3 3 0.081467 0.981250 0.223901 11.00000 0.03134 0.02175 = 0.03654 0.00070 0.00666 -0.00068 O4 3 0.332984 0.904648 0.088222 11.00000 0.02650 0.02001 = 0.01478 0.00156 0.00169 -0.00366 O5 3 0.314550 0.600260 0.018948 11.00000 0.06533 0.02635 = 0.02122 -0.00635 0.00722 -0.01083 O6 3 0.413997 0.512077 0.149992 11.00000 0.02088 0.01968 = 0.02485 -0.00239 0.00390 0.00104 O7 3 0.491073 0.778710 0.109705 11.00000 0.03009 0.02555 = 0.03598 0.00260 0.01082 -0.00423 O8 3 0.413361 0.575325 0.288132 11.00000 0.01873 0.02053 = 0.01849 -0.00211 -0.00508 0.00286 O9 3 0.413184 0.172217 0.285347 11.00000 0.03319 0.01827 = 0.03875 0.00268 -0.00526 0.00375 S1 4 0.262106 0.555512 0.345103 11.00000 0.02319 0.02917 = 0.02100 0.00691 0.00457 0.00379 HKLF 4 Covalent radii and connectivity table for 2009src0671 in C2 C 0.770 H 0.320 O 0.660 S 1.030 C1 - O1 C6 C2 C2 - O4 C1 C3 C3 - O6 C4 C2 C4 - O8 C3 C5 C5 - O1 C4 S1 C6 - O2 C1 C7 - O3 O2 C8 C8 - C7 C9 - O5 O4 C10 C10 - C9 C11 - O7 O6 C12 C12 - C11 C13 - O9 O8 C14 C14 - C13 C15 - C16 S1 C16 - C17 C21 C15 C17 - C18 C16 C18 - C19 C17 C19 - C18 C20 C20 - C21 C19 C21 - C20 C16 O1 - C1 C5 O2 - C7 C6 O3 - C7 O4 - C9 C2 O5 - C9 O6 - C11 C3 O7 - C11 O8 - C13 C4 O9 - C13 S1 - C5 C15 Floating origin restraints generated 10903 Reflections read, of which 5 rejected -24 =< h =< 24, -7 =< k =< 7, -25 =< l =< 27, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 4782 Unique reflections, of which 0 suppressed R(int) = 0.0523 R(sigma) = 0.0802 Friedel opposites not merged Maximum memory for data reduction = 2800 / 58469 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 = 3612 / 354281 wR2 = 0.1233 before cycle 1 for 4782 data and 284 / 284 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.49973 0.00082 0.002 OSF Mean shift/su = 0.002 Maximum = 0.008 for U12 S1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for C8 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3612 / 354281 wR2 = 0.1233 before cycle 2 for 4782 data and 284 / 284 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.49973 0.00081 0.000 OSF Mean shift/su = 0.001 Maximum = 0.003 for U12 S1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for C8 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3612 / 354281 wR2 = 0.1233 before cycle 3 for 4782 data and 284 / 284 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.49973 0.00082 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for tors H14A Max. shift = 0.000 A for H14A Max. dU = 0.000 for C16 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3612 / 354281 wR2 = 0.1233 before cycle 4 for 4782 data and 284 / 284 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.49973 0.00082 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for tors H14A Max. shift = 0.000 A for H14B Max. dU = 0.000 for C1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3612 / 354281 wR2 = 0.1233 before cycle 5 for 4782 data and 284 / 284 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.49973 0.00082 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for tors H14A Max. shift = 0.000 A for H14B Max. dU = 0.000 for C4 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3612 / 354281 wR2 = 0.1233 before cycle 6 for 4782 data and 284 / 284 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.49973 0.00082 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for tors H14A Max. shift = 0.000 A for H14C Max. dU = 0.000 for C10 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3612 / 354281 wR2 = 0.1233 before cycle 7 for 4782 data and 284 / 284 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.49973 0.00082 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z S1 Max. shift = 0.000 A for H14B Max. dU = 0.000 for C18 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3612 / 354281 wR2 = 0.1233 before cycle 8 for 4782 data and 284 / 284 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.49973 0.00081 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H14C Max. dU = 0.000 for O5 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3612 / 354281 wR2 = 0.1233 before cycle 9 for 4782 data and 284 / 284 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.49973 0.00081 -0.001 OSF Mean shift/su = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H14A Max. dU = 0.000 for O5 Least-squares cycle 10 Maximum vector length = 511 Memory required = 3612 / 354281 wR2 = 0.1233 before cycle 10 for 4782 data and 284 / 284 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.49973 0.00081 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z S1 Max. shift = 0.000 A for H14A Max. dU = 0.000 for O7 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.2868 1.0639 0.1971 13 1.000 0.000 C1 O1 C6 C2 H2 0.2844 0.6158 0.1270 13 1.000 0.000 C2 O4 C1 C3 H3 0.4048 0.8402 0.1899 13 1.000 0.000 C3 O6 C4 C2 H4 0.3340 0.4220 0.2384 13 1.000 0.000 C4 O8 C3 C5 H5 0.3167 0.8864 0.2967 13 1.000 0.000 C5 O1 C4 S1 H6A 0.2068 1.0201 0.1003 23 0.990 0.000 C6 O2 C1 H6B 0.1602 0.8569 0.1471 23 0.990 0.000 C6 O2 C1 H8A 0.0679 1.5080 0.2041 137 0.980 0.000 C8 C7 H8A H8B 0.1244 1.4856 0.2613 137 0.980 0.000 C8 C7 H8A H8C 0.0464 1.3814 0.2701 137 0.980 0.000 C8 C7 H8A H10A 0.4109 0.9509 -0.0249 137 0.980 0.000 C10 C9 H10A H10B 0.3502 1.1369 -0.0062 137 0.980 0.000 C10 C9 H10A H10C 0.3363 0.9432 -0.0615 137 0.980 0.000 C10 C9 H10A H12A 0.5447 0.4075 0.0597 137 0.980 0.000 C12 C11 H12A H12B 0.4703 0.2724 0.0612 137 0.980 0.000 C12 C11 H12A H12C 0.5227 0.2555 0.1216 137 0.980 0.000 C12 C11 H12A H14A 0.4760 0.4279 0.3952 137 0.980 0.000 C14 C13 H14A H14B 0.5302 0.4940 0.3392 137 0.980 0.000 C14 C13 H14A H14C 0.5185 0.2210 0.3591 137 0.980 0.000 C14 C13 H14A H15A 0.2221 0.9087 0.3937 23 0.990 0.000 C15 C16 S1 H15B 0.1614 0.7997 0.3481 23 0.990 0.000 C15 C16 S1 H17 0.1177 0.3674 0.3874 43 0.950 0.000 C17 C18 C16 H18 0.0712 0.1714 0.4763 43 0.950 0.000 C18 C19 C17 H19 0.0901 0.3210 0.5799 43 0.950 0.000 C19 C18 C20 H20 0.1565 0.6686 0.5938 43 0.950 0.000 C20 C21 C19 H21 0.2053 0.8629 0.5056 43 0.950 0.000 C21 C20 C16 2009src0671 in C2 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.26099 0.91774 0.18255 1.00000 0.02153 0.02270 0.01635 0.00032 -0.00063 -0.00230 0.02019 0.00626 0.00019 0.00067 0.00016 0.00000 0.00188 0.00197 0.00165 0.00152 0.00137 0.00156 0.00077 H1 0.28680 1.06390 0.19714 1.00000 0.02423 0.00000 0.00000 C2 0.30956 0.76244 0.14222 1.00000 0.02292 0.02128 0.01577 -0.00010 0.00067 -0.00430 0.01999 0.00623 0.00019 0.00067 0.00016 0.00000 0.00192 0.00192 0.00173 0.00149 0.00141 0.00151 0.00078 H2 0.28440 0.61579 0.12704 1.00000 0.02399 0.00000 0.00000 C3 0.37455 0.69653 0.18242 1.00000 0.02113 0.01697 0.01567 -0.00540 0.00274 0.00115 0.01791 0.00595 0.00018 0.00063 0.00015 0.00000 0.00183 0.00174 0.00162 0.00147 0.00137 0.00150 0.00072 H3 0.40483 0.84016 0.18992 1.00000 0.02149 0.00000 0.00000 C4 0.35233 0.58695 0.24614 1.00000 0.01826 0.01765 0.01972 -0.00071 -0.00011 -0.00094 0.01855 0.00582 0.00017 0.00068 0.00015 0.00000 0.00172 0.00180 0.00167 0.00154 0.00129 0.00155 0.00072 H4 0.33399 0.42199 0.23843 1.00000 0.02226 0.00000 0.00000 C5 0.29608 0.73425 0.27989 1.00000 0.01761 0.02446 0.01601 0.00348 -0.00329 -0.00220 0.01937 0.00616 0.00018 0.00067 0.00016 0.00000 0.00181 0.00200 0.00165 0.00150 0.00134 0.00151 0.00076 H5 0.31671 0.88638 0.29673 1.00000 0.02325 0.00000 0.00000 C6 0.19499 0.98870 0.14582 1.00000 0.02613 0.02629 0.01900 -0.00254 -0.00112 0.00655 0.02381 0.00651 0.00020 0.00068 0.00017 0.00000 0.00205 0.00204 0.00174 0.00150 0.00150 0.00157 0.00084 H6A 0.20681 1.02014 0.10029 1.00000 0.02858 0.00000 0.00000 H6B 0.16024 0.85688 0.14710 1.00000 0.02858 0.00000 0.00000 C7 0.10829 1.17300 0.21344 1.00000 0.02651 0.02431 0.01911 0.00164 -0.00626 0.00131 0.02334 0.00654 0.00020 0.00071 0.00017 0.00000 0.00210 0.00207 0.00182 0.00163 0.00152 0.00173 0.00083 C8 0.08472 1.40697 0.23945 1.00000 0.02730 0.02418 0.02689 -0.00107 0.00137 0.00352 0.02612 0.00669 0.00020 0.00070 0.00018 0.00000 0.00211 0.00203 0.00196 0.00171 0.00158 0.00171 0.00084 H8A 0.06787 1.50804 0.20409 1.00000 0.03918 0.00000 0.00000 H8B 0.12437 1.48556 0.26130 1.00000 0.03918 0.00000 0.00000 H8C 0.04638 1.38142 0.27012 1.00000 0.03918 0.00000 0.00000 C9 0.33273 0.80247 0.02888 1.00000 0.01864 0.02705 0.01697 -0.00171 -0.00185 0.00366 0.02089 0.00629 0.00019 0.00069 0.00016 0.00000 0.00186 0.00208 0.00174 0.00155 0.00139 0.00159 0.00079 C10 0.35986 0.97297 -0.02014 1.00000 0.03437 0.02823 0.01994 0.00206 0.00776 0.00060 0.02748 0.00692 0.00021 0.00071 0.00017 0.00000 0.00227 0.00205 0.00184 0.00159 0.00158 0.00172 0.00089 H10A 0.41087 0.95093 -0.02493 1.00000 0.04123 0.00000 0.00000 H10B 0.35025 1.13687 -0.00625 1.00000 0.04123 0.00000 0.00000 H10C 0.33631 0.94321 -0.06146 1.00000 0.04123 0.00000 0.00000 C11 0.47170 0.57588 0.11559 1.00000 0.01969 0.03070 0.01795 -0.00286 -0.00115 0.00581 0.02278 0.00636 0.00018 0.00077 0.00016 0.00000 0.00173 0.00211 0.00163 0.00179 0.00129 0.00186 0.00076 C12 0.50524 0.35920 0.08709 1.00000 0.02799 0.03871 0.02681 -0.00792 0.00198 0.00788 0.03116 0.00727 0.00021 0.00080 0.00019 0.00000 0.00224 0.00252 0.00205 0.00190 0.00166 0.00195 0.00097 H12A 0.54468 0.40753 0.05975 1.00000 0.04674 0.00000 0.00000 H12B 0.47030 0.27242 0.06118 1.00000 0.04674 0.00000 0.00000 H12C 0.52273 0.25555 0.12165 1.00000 0.04674 0.00000 0.00000 C13 0.43729 0.35665 0.30531 1.00000 0.02200 0.02589 0.02287 0.00317 0.00336 0.00235 0.02358 0.00676 0.00019 0.00071 0.00017 0.00000 0.00199 0.00218 0.00186 0.00163 0.00148 0.00162 0.00082 C14 0.49551 0.37661 0.35387 1.00000 0.02591 0.03054 0.02747 0.00137 -0.00275 0.00400 0.02798 0.00684 0.00020 0.00079 0.00018 0.00000 0.00212 0.00213 0.00199 0.00179 0.00159 0.00179 0.00086 H14A 0.47602 0.42786 0.39518 1.00000 0.04198 0.00000 0.00000 H14B 0.53019 0.49405 0.33919 1.00000 0.04198 0.00000 0.00000 H14C 0.51847 0.22102 0.35908 1.00000 0.04198 0.00000 0.00000 C15 0.19844 0.75933 0.38000 1.00000 0.02325 0.02794 0.02304 0.00131 0.00361 0.00114 0.02473 0.00682 0.00020 0.00069 0.00017 0.00000 0.00200 0.00215 0.00193 0.00165 0.00151 0.00165 0.00084 H15A 0.22206 0.90868 0.39371 1.00000 0.02967 0.00000 0.00000 H15B 0.16136 0.79970 0.34807 1.00000 0.02967 0.00000 0.00000 C16 0.16633 0.63496 0.43727 1.00000 0.01713 0.02838 0.02106 0.00163 0.00263 0.00313 0.02218 0.00641 0.00019 0.00066 0.00017 0.00000 0.00184 0.00214 0.00181 0.00152 0.00141 0.00150 0.00082 C17 0.12608 0.42876 0.42932 1.00000 0.03150 0.03069 0.02118 -0.00142 -0.00243 0.00017 0.02780 0.00683 0.00021 0.00073 0.00018 0.00000 0.00223 0.00234 0.00188 0.00171 0.00158 0.00178 0.00089 H17 0.11771 0.36741 0.38737 1.00000 0.03336 0.00000 0.00000 C18 0.09819 0.31263 0.48226 1.00000 0.02209 0.03448 0.03739 0.00359 -0.00087 -0.00794 0.03132 0.00717 0.00021 0.00077 0.00019 0.00000 0.00210 0.00238 0.00234 0.00187 0.00169 0.00176 0.00095 H18 0.07119 0.17138 0.47633 1.00000 0.03759 0.00000 0.00000 C19 0.10935 0.40069 0.54368 1.00000 0.02991 0.03561 0.02708 0.00944 0.00653 -0.00145 0.03084 0.00734 0.00021 0.00079 0.00018 0.00000 0.00222 0.00235 0.00204 0.00192 0.00165 0.00193 0.00092 H19 0.09008 0.32096 0.57987 1.00000 0.03700 0.00000 0.00000 C20 0.14898 0.60661 0.55175 1.00000 0.03284 0.03647 0.02025 -0.00464 0.00379 0.00225 0.02984 0.00693 0.00021 0.00076 0.00018 0.00000 0.00220 0.00250 0.00186 0.00172 0.00155 0.00187 0.00094 H20 0.15649 0.66864 0.59376 1.00000 0.03580 0.00000 0.00000 C21 0.17776 0.72306 0.49937 1.00000 0.02622 0.02472 0.02737 -0.00202 0.00290 -0.00077 0.02609 0.00675 0.00020 0.00071 0.00018 0.00000 0.00209 0.00207 0.00199 0.00169 0.00159 0.00167 0.00086 H21 0.20529 0.86294 0.50562 1.00000 0.03131 0.00000 0.00000 O1 0.23884 0.78300 0.23693 1.00000 0.01933 0.02688 0.01646 0.00181 0.00035 0.00286 0.02089 0.00438 0.00013 0.00046 0.00011 0.00000 0.00131 0.00138 0.00120 0.00105 0.00096 0.00109 0.00055 O2 0.16485 1.20142 0.17444 1.00000 0.02835 0.02161 0.02514 0.00211 0.00558 0.00488 0.02501 0.00454 0.00013 0.00047 0.00012 0.00000 0.00148 0.00138 0.00138 0.00115 0.00111 0.00119 0.00059 O3 0.08147 0.98125 0.22390 1.00000 0.03134 0.02175 0.03654 0.00070 0.00666 -0.00068 0.02985 0.00485 0.00015 0.00047 0.00013 0.00000 0.00156 0.00143 0.00158 0.00120 0.00123 0.00117 0.00065 O4 0.33298 0.90465 0.08822 1.00000 0.02650 0.02001 0.01477 0.00156 0.00169 -0.00365 0.02042 0.00409 0.00013 0.00044 0.00011 0.00000 0.00140 0.00131 0.00116 0.00106 0.00098 0.00112 0.00055 O5 0.31455 0.60026 0.01895 1.00000 0.06533 0.02635 0.02122 -0.00636 0.00722 -0.01082 0.03760 0.00475 0.00016 0.00051 0.00012 0.00000 0.00203 0.00164 0.00137 0.00122 0.00129 0.00151 0.00073 O6 0.41400 0.51208 0.14999 1.00000 0.02088 0.01968 0.02485 -0.00239 0.00389 0.00104 0.02179 0.00409 0.00012 0.00042 0.00011 0.00000 0.00129 0.00140 0.00130 0.00108 0.00101 0.00105 0.00057 O7 0.49107 0.77871 0.10971 1.00000 0.03009 0.02555 0.03599 0.00260 0.01082 -0.00422 0.03050 0.00494 0.00015 0.00049 0.00013 0.00000 0.00160 0.00154 0.00164 0.00129 0.00125 0.00122 0.00067 O8 0.41336 0.57532 0.28813 1.00000 0.01874 0.02053 0.01849 -0.00210 -0.00508 0.00286 0.01927 0.00397 0.00011 0.00047 0.00010 0.00000 0.00120 0.00127 0.00115 0.00114 0.00089 0.00119 0.00051 O9 0.41318 0.17222 0.28535 1.00000 0.03319 0.01827 0.03875 0.00268 -0.00525 0.00375 0.03009 0.00463 0.00014 0.00046 0.00013 0.00000 0.00161 0.00143 0.00162 0.00125 0.00125 0.00120 0.00065 S1 0.26211 0.55551 0.34510 1.00000 0.02319 0.02917 0.02100 0.00691 0.00457 0.00379 0.02444 0.00163 0.00005 0.00017 0.00004 0.00000 0.00046 0.00051 0.00044 0.00044 0.00034 0.00045 0.00021 Final Structure Factor Calculation for 2009src0671 in C2 Total number of l.s. parameters = 284 Maximum vector length = 511 Memory required = 3330 / 25046 wR2 = 0.1233 before cycle 11 for 4782 data and 2 / 284 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 4.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0617 for 3858 Fo > 4sig(Fo) and 0.0869 for all 4782 data wR2 = 0.1233, GooF = S = 1.102, Restrained GooF = 1.102 for all data Flack x parameter = 0.0788 with su 0.1154 Expected values are 0 (within 3 su'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 = 31.00 for non-hydrogen and 26.00 for hydrogen atoms Principal mean square atomic displacements U 0.0246 0.0198 0.0162 C1 0.0265 0.0178 0.0157 C2 0.0226 0.0209 0.0102 C3 0.0199 0.0189 0.0168 C4 0.0269 0.0181 0.0131 C5 0.0333 0.0201 0.0180 C6 0.0303 0.0248 0.0150 C7 0.0297 0.0273 0.0214 C8 0.0289 0.0182 0.0156 C9 0.0378 0.0283 0.0164 C10 0.0338 0.0173 0.0172 C11 0.0451 0.0292 0.0191 C12 0.0297 0.0219 0.0191 C13 0.0329 0.0293 0.0218 C14 0.0291 0.0254 0.0197 C15 0.0298 0.0213 0.0155 C16 0.0323 0.0307 0.0204 C17 0.0416 0.0342 0.0182 C18 0.0421 0.0326 0.0178 C19 0.0381 0.0336 0.0179 C20 0.0303 0.0246 0.0233 C21 0.0281 0.0184 0.0161 O1 0.0344 0.0217 0.0189 O2 0.0409 0.0271 0.0216 O3 0.0282 0.0193 0.0138 O4 0.0695 0.0264 0.0169 O5 0.0274 0.0211 0.0169 O6 0.0440 0.0290 0.0185 O7 0.0261 0.0183 0.0134 O8 0.0422 0.0315 0.0167 O9 0.0356 0.0215 0.0163 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.033 0.048 0.062 0.075 0.090 0.109 0.131 0.162 0.222 1.000 Number in group 499. 483. 458. 502. 457. 480. 473. 480. 470. 480. GooF 1.147 1.163 1.158 1.151 1.190 1.072 1.112 1.073 0.949 0.976 K 1.787 1.086 1.067 1.056 1.015 0.992 1.006 1.014 1.003 1.002 Resolution(A) 0.77 0.80 0.83 0.88 0.92 0.98 1.06 1.17 1.34 1.67 inf Number in group 486. 488. 461. 484. 477. 480. 469. 491. 470. 476. GooF 1.212 1.156 1.225 1.165 1.212 1.032 0.993 0.896 1.010 1.071 K 1.071 1.073 1.053 1.045 1.028 1.003 0.996 1.002 1.002 0.999 R1 0.200 0.188 0.173 0.132 0.122 0.076 0.056 0.044 0.038 0.026 Recommended weighting scheme: WGHT 0.0000 4.9871 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) -4 0 19 -41.11 181.98 3.84 0.067 1.07 10 2 0 947.08 1395.41 3.61 0.187 1.57 -4 6 11 11.37 242.63 3.42 0.078 0.82 7 -1 20 308.19 550.85 3.39 0.117 0.95 -16 2 11 92.91 244.53 3.34 0.078 0.95 -6 0 22 207.00 472.18 3.28 0.109 0.91 8 0 19 49.33 219.13 3.25 0.074 0.99 17 -1 8 581.71 336.24 3.24 0.092 1.01 -12 4 15 38.88 154.29 3.20 0.062 0.84 7 -3 22 437.87 124.44 3.18 0.056 0.80 -21 1 13 -52.79 97.14 3.18 0.049 0.78 -20 -4 4 514.79 285.82 3.11 0.084 0.78 -10 2 18 234.19 473.13 3.09 0.109 0.93 -7 -1 19 63.53 193.48 3.04 0.070 1.00 19 -3 8 -24.34 90.96 3.03 0.048 0.83 21 1 2 -58.94 160.65 3.03 0.063 0.89 -1 -7 2 481.69 267.39 3.03 0.082 0.80 10 -2 20 396.35 640.71 3.02 0.127 0.86 10 6 5 10.41 94.38 3.02 0.049 0.82 19 -1 10 218.67 487.80 3.00 0.110 0.89 -22 0 5 145.24 9.33 2.99 0.015 0.84 11 -5 15 259.88 57.43 2.95 0.038 0.78 1 -1 26 435.82 213.70 2.92 0.073 0.79 3 -7 0 318.62 87.33 2.91 0.047 0.79 -6 2 13 385.75 595.44 2.89 0.122 1.27 -16 -4 13 -18.14 170.31 2.88 0.065 0.79 -8 6 11 -68.53 79.92 2.86 0.045 0.79 -9 -5 6 -36.48 47.19 2.85 0.034 0.95 13 -5 12 -62.71 131.06 2.84 0.057 0.79 2 -2 19 614.09 397.22 2.83 0.100 1.01 15 -1 11 269.48 94.19 2.82 0.049 1.03 0 -4 16 247.46 471.17 2.78 0.108 0.95 -8 0 19 -33.22 97.63 2.78 0.049 1.00 -2 -4 7 275.84 424.19 2.75 0.103 1.26 -21 3 8 455.49 176.75 2.75 0.066 0.78 17 3 3 1173.30 746.73 2.74 0.137 0.95 -6 0 23 219.07 0.25 2.74 0.002 0.87 -19 -1 15 242.01 33.83 2.74 0.029 0.80 0 -4 20 824.39 520.31 2.74 0.114 0.83 1 -5 13 936.75 649.68 2.73 0.127 0.92 -11 -1 18 -42.93 157.78 2.71 0.063 0.95 20 0 7 769.71 506.17 2.71 0.112 0.90 20 0 6 282.70 17.22 2.70 0.021 0.91 -19 1 15 344.21 35.56 2.69 0.030 0.80 10 -4 1 120.89 243.69 2.66 0.078 1.12 4 -6 7 328.13 175.00 2.64 0.066 0.88 12 4 6 328.77 186.99 2.63 0.068 1.00 -13 1 12 113.14 222.58 2.63 0.075 1.10 -8 -2 2 3035.41 2586.53 2.62 0.254 1.78 17 -3 12 109.25 266.29 2.62 0.082 0.84 Bond lengths and angles C1 - Distance Angles O1 1.4249 (0.0041) C6 1.5144 (0.0049) 107.03 (0.29) C2 1.5221 (0.0048) 108.44 (0.28) 111.87 (0.28) H1 1.0000 109.81 109.81 109.81 C1 - O1 C6 C2 C2 - Distance Angles O4 1.4488 (0.0040) C1 1.5221 (0.0048) 107.57 (0.29) C3 1.5294 (0.0048) 107.87 (0.28) 108.94 (0.26) H2 1.0000 110.79 110.79 110.79 C2 - O4 C1 C3 C3 - Distance Angles O6 1.4448 (0.0040) C4 1.5220 (0.0046) 105.34 (0.27) C2 1.5294 (0.0048) 109.56 (0.26) 110.30 (0.27) H3 1.0000 110.51 110.51 110.51 C3 - O6 C4 C2 C4 - Distance Angles O8 1.4462 (0.0037) C3 1.5220 (0.0046) 108.62 (0.26) C5 1.5229 (0.0047) 107.79 (0.26) 112.38 (0.28) H4 1.0000 109.33 109.33 109.33 C4 - O8 C3 C5 C5 - Distance Angles O1 1.4273 (0.0039) C4 1.5229 (0.0047) 110.28 (0.26) S1 1.8073 (0.0034) 107.63 (0.23) 107.40 (0.24) H5 1.0000 110.48 110.48 110.48 C5 - O1 C4 S1 C6 - Distance Angles O2 1.4508 (0.0043) C1 1.5144 (0.0049) 109.56 (0.29) H6A 0.9900 109.76 109.76 H6B 0.9900 109.76 109.76 108.22 C6 - O2 C1 H6A C7 - Distance Angles O3 1.2088 (0.0045) O2 1.3572 (0.0044) 123.11 (0.36) C8 1.4877 (0.0053) 126.16 (0.35) 110.72 (0.33) C7 - O3 O2 C8 - Distance Angles C7 1.4877 (0.0053) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C7 H8A H8B C9 - Distance Angles O5 1.2016 (0.0046) O4 1.3602 (0.0041) 123.51 (0.33) C10 1.4907 (0.0051) 125.90 (0.34) 110.57 (0.32) C9 - O5 O4 C10 - Distance Angles C9 1.4907 (0.0051) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C9 H10A H10B C11 - Distance Angles O7 1.2006 (0.0048) O6 1.3582 (0.0040) 123.40 (0.34) C12 1.4945 (0.0055) 126.68 (0.34) 109.92 (0.35) C11 - O7 O6 C12 - Distance Angles C11 1.4945 (0.0055) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C11 H12A H12B C13 - Distance Angles O9 1.2025 (0.0046) O8 1.3535 (0.0046) 124.11 (0.33) C14 1.4952 (0.0051) 125.06 (0.36) 110.79 (0.33) C13 - O9 O8 C14 - Distance Angles C13 1.4952 (0.0051) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - C13 H14A H14B C15 - Distance Angles C16 1.5110 (0.0049) S1 1.8156 (0.0037) 107.27 (0.26) H15A 0.9900 110.26 110.26 H15B 0.9900 110.26 110.26 108.53 C15 - C16 S1 H15A C16 - Distance Angles C17 1.3936 (0.0052) C21 1.3978 (0.0049) 118.93 (0.33) C15 1.5110 (0.0049) 120.77 (0.33) 120.29 (0.34) C16 - C17 C21 C17 - Distance Angles C18 1.3861 (0.0053) C16 1.3936 (0.0052) 120.40 (0.35) H17 0.9500 119.80 119.80 C17 - C18 C16 C18 - Distance Angles C19 1.3842 (0.0055) C17 1.3861 (0.0053) 120.57 (0.38) H18 0.9500 119.71 119.71 C18 - C19 C17 C19 - Distance Angles C18 1.3842 (0.0055) C20 1.3861 (0.0059) 119.20 (0.36) H19 0.9500 120.40 120.40 C19 - C18 C20 C20 - Distance Angles C21 1.3845 (0.0053) C19 1.3861 (0.0059) 120.84 (0.36) H20 0.9500 119.58 119.58 C20 - C21 C19 C21 - Distance Angles C20 1.3845 (0.0053) C16 1.3978 (0.0049) 120.05 (0.37) H21 0.9500 119.97 119.97 C21 - C20 C16 O1 - Distance Angles C1 1.4249 (0.0041) C5 1.4273 (0.0039) 111.82 (0.26) O1 - C1 O2 - Distance Angles C7 1.3572 (0.0044) C6 1.4508 (0.0043) 117.59 (0.30) O2 - C7 O3 - Distance Angles C7 1.2088 (0.0045) O3 - O4 - Distance Angles C9 1.3602 (0.0041) C2 1.4488 (0.0040) 118.18 (0.28) O4 - C9 O5 - Distance Angles C9 1.2016 (0.0046) O5 - O6 - Distance Angles C11 1.3582 (0.0040) C3 1.4448 (0.0040) 118.56 (0.28) O6 - C11 O7 - Distance Angles C11 1.2006 (0.0048) O7 - O8 - Distance Angles C13 1.3535 (0.0046) C4 1.4462 (0.0037) 117.73 (0.29) O8 - C13 O9 - Distance Angles C13 1.2025 (0.0046) O9 - S1 - Distance Angles C5 1.8073 (0.0035) C15 1.8156 (0.0037) 101.07 (0.17) S1 - C5 FMAP and GRID set by program FMAP 2 2 27 GRID -4.167 -1 -1 4.167 1 1 R1 = 0.0792 for 2771 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.3277 0.0493 0.1204 [ 1.06 A from O4 ] Deepest hole -0.31 at 0.2902 0.5470 0.3235 [ 0.70 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 4182 / 64434 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3277 1.0493 0.1204 1.00000 0.05 0.32 1.06 O4 1.71 C2 1.78 H1 1.96 C1 Q2 1 0.1687 0.5824 0.5188 1.00000 0.05 0.31 0.79 C20 0.90 C21 1.61 C19 1.65 H20 Q3 1 0.6106 0.5626 0.3024 1.00000 0.05 0.30 1.75 H14B 1.78 O3 1.95 C7 2.00 H15B Q4 1 0.3411 0.3828 0.0308 1.00000 0.05 0.28 1.34 O5 1.59 H10B 2.36 C9 2.55 C10 Q5 1 0.0036 0.0039 0.4766 1.00000 0.05 0.28 1.59 H18 1.82 H14A 1.97 H18 2.49 C18 Q6 1 0.5194 0.4123 0.1618 1.00000 0.05 0.28 1.21 H12C 1.60 C12 1.60 C11 1.78 O3 Q7 1 0.5098 0.7236 0.1619 1.00000 0.05 0.28 1.18 O7 1.46 C11 2.12 H8A 2.16 C7 Q8 1 0.4221 0.0680 0.0797 1.00000 0.05 0.28 1.52 H12B 1.93 O4 2.17 O7 2.27 H10B Q9 1 0.2083 1.0798 0.4027 1.00000 0.05 0.27 1.01 H15A 1.87 C15 2.13 H15B 2.38 H17 Q10 1 0.2706 0.5526 0.2986 1.00000 0.05 0.27 0.98 S1 1.19 C5 1.89 H4 1.91 C4 Q11 1 0.3368 0.4742 0.0740 1.00000 0.05 0.27 1.41 O5 1.69 H2 2.07 C9 2.16 O6 Q12 1 0.0219 1.0514 0.1939 1.00000 0.05 0.26 1.34 O3 1.82 C7 1.89 C11 2.24 H12C Q13 1 0.0961 1.4080 0.2799 1.00000 0.05 0.26 0.79 H8B 0.87 C8 0.97 H8C 1.75 H8A Q14 1 0.2496 0.9158 0.5697 1.00000 0.05 0.26 1.60 H21 1.95 S1 2.02 C16 2.27 C21 Q15 1 0.1460 0.9136 0.0774 1.00000 0.05 0.26 1.38 H6A 1.51 H6B 1.75 C6 1.95 H12A Q16 1 0.3013 0.2095 0.2799 1.00000 0.05 0.26 1.60 H4 1.87 H5 1.92 H1 2.13 O9 Q17 1 0.0897 0.1919 0.6076 1.00000 0.05 0.25 0.92 H19 1.81 C19 1.93 H14A 2.27 O8 Q18 1 0.0686 0.3792 0.6002 1.00000 0.05 0.25 0.67 H19 1.41 C19 2.23 C20 2.33 H20 Q19 1 0.4919 -0.0143 0.3234 1.00000 0.05 0.25 1.59 H14C 1.63 H8C 1.98 O9 2.28 C14 Q20 1 0.4074 0.8486 0.0925 1.00000 0.05 0.25 1.45 O4 1.67 O7 1.95 C9 2.01 C11 Shortest distances between peaks (including symmetry equivalents) 5 5 0.98 6 12 1.03 4 11 1.04 17 18 1.13 7 12 1.19 8 20 1.29 6 7 1.75 1 20 1.97 1 8 1.98 3 13 2.01 10 16 2.05 18 19 2.05 9 14 2.12 13 19 2.22 4 15 2.27 7 20 2.51 11 20 2.52 4 8 2.55 1 11 2.57 2 14 2.58 2 14 2.63 1 4 2.65 17 19 2.68 5 17 2.70 3 9 2.78 2 18 2.79 8 11 2.79 3 12 2.81 2 9 2.84 10 14 2.87 5 18 2.97 6 15 2.98 Time profile in seconds ----------------------- 0.05: 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. 0.44: 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 2.11: Structure factors and derivatives 4.14: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.44: Solve l.s. equations 0.00: Generate HTAB table 0.09: 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 +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0671 finished at 17:58:35 Total CPU time: 7.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++