+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 15:58:08 on 29-Jul-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 00SOT002 in C2/c CELL 0.71073 20.4261 5.5841 25.5362 90.000 93.049 90.000 ZERR 8.00 0.0041 0.0011 0.0051 0.000 0.030 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H O F UNIT 120 136 24 24 V = 2908.57 F(000) = 1264.0 Mu = 0.12 mm-1 Cell Wt = 2418.29 Rho = 1.381 L.S. 4 BOND FMAP 2 PLAN 10 OMIT 0 0 2 WGHT 0.100000 EXTI 0.002510 FVAR 0.16740 F1 4 0.165055 0.105205 0.037367 11.00000 0.10732 0.09790 = 0.08084 0.01527 0.04807 0.05269 F2 4 0.076661 0.150611 -0.010329 11.00000 0.13325 0.10566 = 0.04452 -0.02504 0.01094 -0.04100 F3 4 0.148313 0.425540 -0.007186 11.00000 0.09556 0.08910 = 0.05267 0.01177 0.02518 -0.01717 O1 3 0.092866 0.582196 0.075388 11.00000 0.06998 0.03795 = 0.07777 -0.00110 0.01897 -0.00453 O2 3 0.050385 0.422272 0.182040 11.00000 0.03327 0.04905 = 0.04235 -0.01420 -0.00293 0.00741 O3 3 0.196357 0.011660 0.387761 11.00000 0.05123 0.07213 = 0.03940 0.00843 -0.00015 -0.00977 C1 1 0.119471 0.262177 0.021002 11.00000 0.06707 0.05900 = 0.03852 0.00091 0.00788 -0.00072 C2 1 0.086293 0.371019 0.067969 11.00000 0.04073 0.03858 = 0.04014 0.00026 -0.00192 0.00261 C3 1 0.046893 0.201015 0.099215 11.00000 0.03952 0.03232 = 0.03760 -0.00533 0.00445 0.00058 AFIX 13 H3 2 0.053755 0.038754 0.085951 11.00000 -1.20000 AFIX 0 C4 1 -0.026860 0.260251 0.091503 11.00000 0.03890 0.05323 = 0.03894 -0.00817 -0.00308 -0.00255 AFIX 23 H4A 2 -0.038033 0.285323 0.054515 11.00000 -1.20000 H4B 2 -0.052419 0.125980 0.103222 11.00000 -1.20000 AFIX 0 C5 1 -0.043973 0.482521 0.121930 11.00000 0.03539 0.06618 = 0.04741 -0.01376 -0.00533 0.01095 AFIX 23 H5A 2 -0.024675 0.621798 0.106086 11.00000 -1.20000 H5B 2 -0.091175 0.503583 0.120282 11.00000 -1.20000 AFIX 0 C6 1 -0.019099 0.463217 0.178567 11.00000 0.03707 0.06854 = 0.04573 -0.01527 -0.00218 0.01545 AFIX 23 H6A 2 -0.028947 0.609890 0.196917 11.00000 -1.20000 H6B 2 -0.041194 0.332291 0.195283 11.00000 -1.20000 AFIX 0 C7 1 0.066861 0.203289 0.158095 11.00000 0.03482 0.03588 = 0.03838 -0.00427 0.00293 0.00249 AFIX 13 H7 2 0.042676 0.075130 0.174792 11.00000 -1.20000 AFIX 0 C8 1 0.139719 0.160218 0.170223 11.00000 0.03560 0.04343 = 0.04103 0.00044 0.00396 0.00651 AFIX 23 H8A 2 0.153164 0.019065 0.151435 11.00000 -1.20000 H8B 2 0.164275 0.295587 0.157781 11.00000 -1.20000 AFIX 0 C9 1 0.156154 0.126058 0.227995 11.00000 0.02689 0.03331 = 0.03990 -0.00134 0.00547 0.00576 C10 1 0.189851 0.297609 0.257371 11.00000 0.03016 0.03098 = 0.04604 0.00385 0.00632 0.00068 AFIX 43 H10 2 0.203118 0.436932 0.241028 11.00000 -1.20000 AFIX 0 C11 1 0.204587 0.268068 0.310868 11.00000 0.03260 0.03310 = 0.04857 -0.00567 0.00407 -0.00026 AFIX 43 H11 2 0.227454 0.386260 0.329860 11.00000 -1.20000 AFIX 0 C12 1 0.185021 0.062338 0.335445 11.00000 0.03085 0.04694 = 0.03603 0.00147 0.00205 0.00186 C13 1 0.151578 -0.112931 0.306093 11.00000 0.03648 0.03787 = 0.05145 0.01057 0.00200 -0.00599 AFIX 43 H13 2 0.138608 -0.252938 0.322324 11.00000 -1.20000 AFIX 0 C14 1 0.137517 -0.081429 0.253423 11.00000 0.03327 0.03403 = 0.04788 -0.00341 -0.00136 -0.00352 AFIX 43 H14 2 0.115157 -0.200738 0.234398 11.00000 -1.20000 AFIX 0 C15 1 0.231352 0.185748 0.418806 11.00000 0.05532 0.08947 = 0.04248 -0.00715 -0.00513 0.00332 AFIX 137 H15A 2 0.274894 0.201922 0.406833 11.00000 -1.50000 H15B 2 0.233664 0.135854 0.454833 11.00000 -1.50000 H15C 2 0.209110 0.336935 0.415701 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for 00SOT002 in C2/c C 0.770 H 0.320 O 0.660 F 0.640 F1 - C1 F2 - C1 F3 - C1 O1 - C2 O2 - C7 C6 O3 - C12 C15 C1 - F2 F3 F1 C2 C2 - O1 C3 C1 C3 - C2 C7 C4 C4 - C5 C3 C5 - C6 C4 C6 - O2 C5 C7 - O2 C8 C3 C8 - C9 C7 C9 - C10 C14 C8 C10 - C9 C11 C11 - C12 C10 C12 - O3 C11 C13 C13 - C14 C12 C14 - C13 C9 C15 - O3 16416 Reflections read, of which 1108 rejected -25 =< h =< 26, -7 =< k =< 6, -32 =< l =< 33, Max. 2-theta = 54.94 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 2 0 0 40.32 1.70 3 9.43 -5 1 1 73.52 0.46 5 266.20 -5 1 2 32.66 0.11 4 68.51 -16 2 4 0.94 0.11 5 0.97 -14 2 5 22.23 0.10 6 19.77 -13 5 14 8.82 2.11 2 19.68 6 Inconsistent equivalents 3306 Unique reflections, of which 0 suppressed R(int) = 0.0734 R(sigma) = 0.0768 Friedel opposites merged Maximum memory for data reduction = 1864 / 39841 Default effective X-H distances for T = 20.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 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 = 2407 / 238131 wR2 = 0.1587 before cycle 1 for 3306 data and 192 / 192 parameters GooF = S = 0.895; Restrained GooF = 0.895 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16740 0.00058 -0.008 OSF 2 0.00251 0.00067 0.000 EXTI Mean shift/esd = 0.002 Maximum = -0.008 for OSF Max. shift = 0.000 A for F3 Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2407 / 238131 wR2 = 0.1587 before cycle 2 for 3306 data and 192 / 192 parameters GooF = S = 0.895; Restrained GooF = 0.895 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16740 0.00058 0.000 OSF 2 0.00251 0.00067 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.002 for z F3 Max. shift = 0.000 A for H15C Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2407 / 238131 wR2 = 0.1587 before cycle 3 for 3306 data and 192 / 192 parameters GooF = S = 0.895; Restrained GooF = 0.895 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16740 0.00058 0.000 OSF 2 0.00251 0.00067 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H15A Max. dU = 0.000 for O1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2407 / 238131 wR2 = 0.1587 before cycle 4 for 3306 data and 192 / 192 parameters GooF = S = 0.895; Restrained GooF = 0.895 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.16740 0.00058 0.000 OSF 2 0.00251 0.00067 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C10 Max. shift = 0.000 A for H5A Max. dU = 0.000 for C2 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 H3 0.0538 0.0388 0.0860 13 0.980 0.000 C3 C2 C7 C4 H4A -0.0380 0.2853 0.0545 23 0.970 0.000 C4 C5 C3 H4B -0.0524 0.1260 0.1032 23 0.970 0.000 C4 C5 C3 H5A -0.0247 0.6218 0.1061 23 0.970 0.000 C5 C6 C4 H5B -0.0912 0.5036 0.1203 23 0.970 0.000 C5 C6 C4 H6A -0.0289 0.6099 0.1969 23 0.970 0.000 C6 O2 C5 H6B -0.0412 0.3323 0.1953 23 0.970 0.000 C6 O2 C5 H7 0.0427 0.0751 0.1748 13 0.980 0.000 C7 O2 C8 C3 H8A 0.1532 0.0191 0.1514 23 0.970 0.000 C8 C9 C7 H8B 0.1643 0.2956 0.1578 23 0.970 0.000 C8 C9 C7 H10 0.2031 0.4369 0.2410 43 0.930 0.000 C10 C9 C11 H11 0.2275 0.3863 0.3299 43 0.930 0.000 C11 C12 C10 H13 0.1386 -0.2529 0.3223 43 0.930 0.000 C13 C14 C12 H14 0.1152 -0.2007 0.2344 43 0.930 0.000 C14 C13 C9 H15A 0.2749 0.2019 0.4068 137 0.960 0.000 C15 O3 H15A H15B 0.2337 0.1359 0.4548 137 0.960 0.000 C15 O3 H15A H15C 0.2091 0.3369 0.4157 137 0.960 0.000 C15 O3 H15A 00SOT002 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq F1 0.16505 0.10520 0.03737 1.00000 0.10732 0.09790 0.08084 0.01527 0.04807 0.05269 0.09382 0.00354 0.00009 0.00031 0.00006 0.00000 0.00130 0.00124 0.00109 0.00092 0.00095 0.00108 0.00060 F2 0.07666 0.15061 -0.01033 1.00000 0.13325 0.10566 0.04452 -0.02504 0.01094 -0.04100 0.09425 0.00261 0.00009 0.00031 0.00005 0.00000 0.00147 0.00137 0.00083 0.00087 0.00087 0.00115 0.00061 F3 0.14831 0.42554 -0.00719 1.00000 0.09556 0.08910 0.05267 0.01177 0.02518 -0.01717 0.07836 0.00268 0.00008 0.00029 0.00005 0.00000 0.00113 0.00119 0.00086 0.00076 0.00080 0.00087 0.00051 O1 0.09287 0.58220 0.07539 1.00000 0.06998 0.03795 0.07777 -0.00110 0.01897 -0.00453 0.06137 0.00290 0.00008 0.00028 0.00007 0.00000 0.00108 0.00096 0.00115 0.00078 0.00088 0.00077 0.00048 O2 0.05038 0.42227 0.18204 1.00000 0.03327 0.04905 0.04235 -0.01420 -0.00293 0.00741 0.04174 0.00213 0.00006 0.00024 0.00005 0.00000 0.00070 0.00089 0.00080 0.00065 0.00058 0.00062 0.00040 O3 0.19636 0.01166 0.38776 1.00000 0.05123 0.07213 0.03940 0.00843 -0.00015 -0.00977 0.05434 0.00256 0.00007 0.00029 0.00005 0.00000 0.00086 0.00110 0.00088 0.00075 0.00068 0.00080 0.00045 C1 0.11947 0.26218 0.02100 1.00000 0.06707 0.05900 0.03852 0.00091 0.00788 -0.00072 0.05468 0.00423 0.00012 0.00046 0.00008 0.00000 0.00152 0.00146 0.00123 0.00112 0.00116 0.00129 0.00062 C2 0.08629 0.37102 0.06797 1.00000 0.04073 0.03858 0.04015 0.00026 -0.00192 0.00261 0.03997 0.00349 0.00010 0.00037 0.00008 0.00000 0.00108 0.00122 0.00112 0.00092 0.00087 0.00089 0.00049 C3 0.04689 0.20101 0.09921 1.00000 0.03952 0.03232 0.03760 -0.00533 0.00445 0.00058 0.03640 0.00325 0.00009 0.00034 0.00007 0.00000 0.00103 0.00102 0.00106 0.00085 0.00084 0.00085 0.00047 H3 0.05376 0.03875 0.08595 1.00000 0.04368 0.00000 0.00000 C4 -0.02686 0.26025 0.09150 1.00000 0.03890 0.05323 0.03894 -0.00817 -0.00308 -0.00255 0.04387 0.00333 0.00009 0.00040 0.00008 0.00000 0.00105 0.00136 0.00114 0.00098 0.00088 0.00097 0.00054 H4A -0.03803 0.28532 0.05452 1.00000 0.05265 0.00000 0.00000 H4B -0.05242 0.12598 0.10322 1.00000 0.05265 0.00000 0.00000 C5 -0.04397 0.48252 0.12193 1.00000 0.03539 0.06618 0.04741 -0.01376 -0.00533 0.01095 0.04993 0.00364 0.00010 0.00044 0.00008 0.00000 0.00104 0.00150 0.00130 0.00108 0.00094 0.00101 0.00059 H5A -0.02467 0.62180 0.10609 1.00000 0.05991 0.00000 0.00000 H5B -0.09118 0.50358 0.12028 1.00000 0.05991 0.00000 0.00000 C6 -0.01910 0.46322 0.17857 1.00000 0.03707 0.06854 0.04573 -0.01527 -0.00218 0.01545 0.05060 0.00371 0.00009 0.00044 0.00008 0.00000 0.00108 0.00156 0.00129 0.00109 0.00096 0.00104 0.00060 H6A -0.02895 0.60989 0.19692 1.00000 0.06073 0.00000 0.00000 H6B -0.04119 0.33229 0.19528 1.00000 0.06073 0.00000 0.00000 C7 0.06686 0.20329 0.15810 1.00000 0.03482 0.03588 0.03838 -0.00427 0.00293 0.00249 0.03633 0.00321 0.00009 0.00035 0.00007 0.00000 0.00098 0.00111 0.00110 0.00088 0.00083 0.00085 0.00048 H7 0.04268 0.07513 0.17479 1.00000 0.04359 0.00000 0.00000 C8 0.13972 0.16022 0.17022 1.00000 0.03560 0.04343 0.04103 0.00044 0.00396 0.00651 0.03995 0.00341 0.00009 0.00038 0.00008 0.00000 0.00103 0.00117 0.00112 0.00090 0.00085 0.00088 0.00049 H8A 0.15316 0.01907 0.15144 1.00000 0.04794 0.00000 0.00000 H8B 0.16427 0.29559 0.15778 1.00000 0.04794 0.00000 0.00000 C9 0.15615 0.12606 0.22799 1.00000 0.02689 0.03331 0.03990 -0.00134 0.00547 0.00576 0.03323 0.00315 0.00008 0.00034 0.00007 0.00000 0.00090 0.00103 0.00107 0.00084 0.00079 0.00078 0.00046 C10 0.18985 0.29761 0.25737 1.00000 0.03016 0.03098 0.04604 0.00385 0.00632 0.00068 0.03557 0.00325 0.00008 0.00034 0.00007 0.00000 0.00094 0.00104 0.00119 0.00087 0.00084 0.00081 0.00047 H10 0.20312 0.43693 0.24103 1.00000 0.04269 0.00000 0.00000 C11 0.20459 0.26807 0.31087 1.00000 0.03260 0.03310 0.04857 -0.00567 0.00407 -0.00026 0.03802 0.00334 0.00009 0.00035 0.00008 0.00000 0.00099 0.00107 0.00122 0.00088 0.00088 0.00082 0.00049 H11 0.22745 0.38626 0.32986 1.00000 0.04563 0.00000 0.00000 C12 0.18502 0.06234 0.33544 1.00000 0.03085 0.04694 0.03603 0.00147 0.00205 0.00186 0.03793 0.00333 0.00009 0.00036 0.00007 0.00000 0.00094 0.00122 0.00111 0.00091 0.00083 0.00089 0.00049 C13 0.15158 -0.11293 0.30609 1.00000 0.03648 0.03787 0.05145 0.01057 0.00200 -0.00599 0.04194 0.00352 0.00009 0.00036 0.00008 0.00000 0.00103 0.00115 0.00128 0.00097 0.00092 0.00088 0.00052 H13 0.13861 -0.25294 0.32232 1.00000 0.05033 0.00000 0.00000 C14 0.13752 -0.08143 0.25342 1.00000 0.03327 0.03403 0.04788 -0.00341 -0.00136 -0.00352 0.03852 0.00327 0.00009 0.00034 0.00008 0.00000 0.00096 0.00108 0.00124 0.00090 0.00089 0.00084 0.00049 H14 0.11516 -0.20074 0.23440 1.00000 0.04622 0.00000 0.00000 C15 0.23135 0.18575 0.41881 1.00000 0.05532 0.08947 0.04248 -0.00715 -0.00513 0.00332 0.06270 0.00398 0.00011 0.00051 0.00008 0.00000 0.00138 0.00199 0.00128 0.00129 0.00109 0.00133 0.00070 H15A 0.27489 0.20192 0.40683 1.00000 0.09405 0.00000 0.00000 H15B 0.23366 0.13585 0.45483 1.00000 0.09405 0.00000 0.00000 H15C 0.20911 0.33694 0.41570 1.00000 0.09405 0.00000 0.00000 Final Structure Factor Calculation for 00SOT002 in C2/c Total number of l.s. parameters = 192 Maximum vector length = 511 Memory required = 2215 / 22995 wR2 = 0.1587 before cycle 5 for 3306 data and 0 / 192 parameters GooF = S = 0.895; Restrained GooF = 0.895 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0491 for 1816 Fo > 4sig(Fo) and 0.1169 for all 3306 data wR2 = 0.1587, GooF = S = 0.895, Restrained GooF = 0.895 for all data Occupancy sum of asymmetric unit = 21.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.1725 0.0732 0.0359 F1 0.1650 0.0825 0.0352 F2 0.1110 0.0877 0.0364 F3 0.0889 0.0579 0.0373 O1 0.0634 0.0319 0.0299 O2 0.0783 0.0474 0.0374 O3 0.0677 0.0590 0.0373 C1 0.0453 0.0393 0.0353 C2 0.0420 0.0386 0.0286 C3 0.0569 0.0433 0.0314 C4 0.0781 0.0404 0.0313 C5 0.0824 0.0392 0.0302 C6 0.0417 0.0365 0.0308 C7 0.0473 0.0410 0.0316 C8 0.0407 0.0366 0.0224 C9 0.0478 0.0302 0.0287 C10 0.0505 0.0325 0.0310 C11 0.0473 0.0358 0.0306 C12 0.0579 0.0396 0.0283 C13 0.0493 0.0372 0.0291 C14 0.0912 0.0582 0.0387 C15 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.006 0.011 0.017 0.022 0.030 0.040 0.055 0.078 0.121 1.000 Number in group 398. 298. 352. 274. 338. 329. 331. 334. 323. 329. GooF 0.747 0.851 0.890 0.927 0.914 1.060 1.019 0.926 0.783 0.815 K 0.189 1.264 0.800 0.900 1.043 1.014 0.999 0.997 1.029 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.67 inf Number in group 334. 335. 329. 327. 330. 338. 324. 330. 328. 331. GooF 0.824 0.792 0.820 0.864 0.903 1.001 0.947 0.914 0.950 0.916 K 1.124 1.027 1.061 1.019 1.006 1.026 1.054 1.051 1.044 0.986 R1 0.446 0.370 0.288 0.213 0.168 0.097 0.070 0.060 0.046 0.039 Recommended weighting scheme: WGHT 0.0739 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 10 2 8 43.62 85.07 3.67 0.031 1.44 19 3 9 61.43 202.17 3.49 0.047 0.87 6 2 5 6.51 28.67 3.47 0.018 1.96 9 1 22 129.05 227.28 3.42 0.050 0.99 -9 1 6 73.28 37.99 3.42 0.021 1.92 2 0 26 57.96 166.34 3.39 0.043 0.97 7 1 13 -4.94 21.86 3.37 0.016 1.53 -20 0 6 -22.48 43.86 3.37 0.022 1.00 1 1 25 269.44 382.54 3.33 0.065 1.00 -3 5 18 93.81 188.42 3.31 0.046 0.87 -1 3 22 48.42 103.19 3.26 0.034 0.98 22 0 10 -6.13 68.63 3.24 0.028 0.86 -7 3 20 17.60 64.04 3.04 0.027 1.00 2 0 14 681.39 506.61 3.03 0.075 1.78 -4 4 13 286.68 204.59 3.03 0.048 1.12 -2 2 9 73.56 41.78 2.98 0.022 1.97 -16 2 4 33.69 126.88 2.97 0.038 1.15 15 1 1 6.99 28.10 2.94 0.018 1.32 7 3 20 15.96 89.75 2.89 0.032 0.98 4 0 22 124.36 70.83 2.87 0.028 1.12 2 0 28 476.85 223.92 2.86 0.050 0.90 -5 1 1 2773.73 28094.00 2.85 0.558 3.28 -9 5 14 -20.00 54.40 2.84 0.025 0.89 -15 1 14 150.18 213.93 2.81 0.049 1.10 13 5 13 -0.32 185.26 2.80 0.045 0.82 9 5 3 3.15 29.73 2.79 0.018 0.99 -5 5 8 400.35 291.56 2.78 0.057 1.02 -1 1 27 37.15 81.42 2.78 0.030 0.93 5 1 12 468.87 365.05 2.77 0.064 1.75 5 1 22 285.01 396.43 2.76 0.066 1.08 -4 2 10 1579.99 1242.31 2.76 0.117 1.79 -11 1 8 955.74 747.61 2.76 0.091 1.57 10 0 28 416.00 218.17 2.75 0.049 0.82 -19 3 6 109.00 194.55 2.74 0.046 0.92 12 2 6 13.01 30.93 2.73 0.019 1.36 -23 3 8 151.34 310.46 2.73 0.059 0.79 -1 5 5 59.36 118.93 2.72 0.036 1.09 13 1 6 126.05 90.46 2.72 0.032 1.40 7 1 12 196.01 149.98 2.71 0.041 1.60 16 4 10 92.83 209.10 2.68 0.048 0.87 -5 1 2 1182.41 7056.31 2.67 0.280 3.22 -3 1 22 5.88 38.51 2.66 0.021 1.13 -13 1 1 16.92 0.04 2.64 0.001 1.51 14 4 18 206.78 5.02 2.57 0.007 0.81 11 1 3 11.81 29.82 2.57 0.018 1.71 -6 0 20 18.09 59.67 2.57 0.026 1.22 -5 1 17 68.30 100.47 2.56 0.033 1.39 -17 1 21 1022.48 703.68 2.56 0.088 0.87 21 3 4 124.80 215.10 2.53 0.049 0.85 -7 5 13 258.51 352.79 2.52 0.063 0.93 Bond lengths and angles F1 - Distance Angles C1 1.3299 (0.0027) F1 - F2 - Distance Angles C1 1.3109 (0.0027) F2 - F3 - Distance Angles C1 1.3200 (0.0027) F3 - O1 - Distance Angles C2 1.2008 (0.0024) O1 - O2 - Distance Angles C7 1.4157 (0.0022) C6 1.4357 (0.0023) 111.58 (0.15) O2 - C7 O3 - Distance Angles C12 1.3732 (0.0023) C15 1.4227 (0.0028) 117.07 (0.17) O3 - C12 C1 - Distance Angles F2 1.3109 (0.0027) F3 1.3200 (0.0027) 107.35 (0.19) F1 1.3299 (0.0027) 108.16 (0.22) 107.55 (0.20) C2 1.5341 (0.0031) 110.94 (0.19) 112.40 (0.20) 110.27 (0.18) C1 - F2 F3 F1 C2 - Distance Angles O1 1.2008 (0.0024) C3 1.5013 (0.0028) 126.57 (0.19) C1 1.5341 (0.0031) 117.52 (0.20) 115.89 (0.18) C2 - O1 C3 C3 - Distance Angles C2 1.5013 (0.0028) C7 1.5369 (0.0025) 113.13 (0.15) C4 1.5447 (0.0026) 110.09 (0.16) 109.22 (0.15) C3 - C2 C7 C4 - Distance Angles C5 1.5150 (0.0030) C3 1.5447 (0.0026) 111.11 (0.15) C4 - C5 C5 - Distance Angles C6 1.5111 (0.0029) C4 1.5150 (0.0030) 110.94 (0.17) C5 - C6 C6 - Distance Angles O2 1.4357 (0.0023) C5 1.5111 (0.0029) 110.58 (0.17) C6 - O2 C7 - Distance Angles O2 1.4157 (0.0022) C8 1.5230 (0.0025) 107.50 (0.15) C3 1.5369 (0.0025) 111.89 (0.15) 113.78 (0.15) C7 - O2 C8 C8 - Distance Angles C9 1.5076 (0.0027) C7 1.5230 (0.0025) 112.54 (0.16) C8 - C9 C9 - Distance Angles C10 1.3781 (0.0026) C14 1.3911 (0.0027) 117.78 (0.17) C8 1.5076 (0.0027) 121.57 (0.18) 120.66 (0.17) C9 - C10 C14 C10 - Distance Angles C9 1.3781 (0.0026) C11 1.3929 (0.0026) 121.81 (0.18) C10 - C9 C11 - Distance Angles C12 1.3784 (0.0028) C10 1.3929 (0.0026) 119.50 (0.18) C11 - C12 C12 - Distance Angles O3 1.3732 (0.0023) C11 1.3784 (0.0028) 125.22 (0.18) C13 1.3899 (0.0028) 115.60 (0.18) 119.17 (0.18) C12 - O3 C11 C13 - Distance Angles C14 1.3716 (0.0027) C12 1.3899 (0.0028) 120.65 (0.18) C13 - C14 C14 - Distance Angles C13 1.3716 (0.0027) C9 1.3911 (0.0028) 121.08 (0.18) C14 - C13 C15 - Distance Angles O3 1.4227 (0.0028) C15 - FMAP and GRID set by program FMAP 2 1 25 GRID -1.136 -2 -1 1.136 2 1 R1 = 0.1167 for 3306 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.27 at 0.0556 0.4172 0.1826 [ 0.11 A from O2 ] Deepest hole -0.32 at 0.1963 0.1407 0.0596 [ 0.85 A from F1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2383 / 26741 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1214 0.0354 0.0193 1.00000 0.05 0.25 1.06 F1 1.27 C1 1.32 F2 2.25 H3 Q2 1 0.1047 0.3079 0.2510 1.00000 0.05 0.24 1.60 C9 1.74 C10 1.94 H6B 2.13 O2 Q3 1 0.2254 -0.1839 0.3732 1.00000 0.05 0.24 1.31 O3 1.85 C12 2.17 H13 2.26 C13 Q4 1 0.1984 -0.0990 0.3100 1.00000 0.05 0.21 0.96 C13 1.15 C12 1.54 H13 1.86 C14 Q5 1 0.0842 0.3721 0.2107 1.00000 0.05 0.21 1.02 O2 1.66 C7 1.97 C8 2.04 C9 Q6 1 -0.0062 0.7108 0.1798 1.00000 0.05 0.21 0.86 H6A 1.41 C6 1.96 H5A 1.98 O2 Q7 1 0.2521 -0.2030 0.4383 1.00000 0.05 0.21 1.98 H15B 2.06 O3 2.07 F1 2.26 C15 Q8 1 -0.0455 0.7491 0.0834 1.00000 0.05 0.21 1.00 H5A 1.78 C5 1.93 H5B 2.02 F2 Q9 1 0.2248 -0.1521 0.4132 1.00000 0.05 0.20 1.25 O3 1.90 C15 1.93 H15B 2.24 H15A Q10 1 0.0581 0.2813 0.0923 1.00000 0.05 0.20 0.54 C3 1.00 C2 1.37 H3 1.74 C7 Shortest distances between peaks (including symmetry equivalents) 7 9 0.87 3 9 1.04 2 5 1.15 3 7 1.72 3 4 1.74 6 8 2.56 4 9 2.68 1 10 2.70 5 6 2.73 Time profile in seconds ----------------------- 0.23: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 2.33: 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 1.13: Structure factors and derivatives 1.36: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.25: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.14: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 15:58:14 Total CPU time: 5.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++