+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 11:43:46 on 14-May-2003 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in Cc CELL 0.71073 13.4334 14.3903 13.7137 90.000 90.407 90.000 ZERR 4.00 0.0002 0.0002 0.0003 0.000 0.001 0.000 LATT -7 SYMM X, - Y, 1/2 + Z SFAC C H N O P UNIT 128 104 4 16 4 V = 2650.94 F(000) = 1088.0 Mu = 0.14 mm-1 Cell Wt = 2078.03 Rho = 1.302 MERG 2 OMIT -3.00 55.00 OMIT 0 0 2 OMIT 0 0 -2 OMIT 2 0 0 EXTI 0.00664 ACTA HTAB O1 O2 FMAP 2 PLAN 10 SIZE 0.14 0.18 0.25 BOND $H WGHT 0.02570 1.38200 L.S. 19 TEMP -153.00 FVAR 0.33153 C1 1 0.922085 0.576386 0.149538 11.00000 0.02389 0.01473 = 0.01965 0.00056 0.00220 -0.00560 C2 1 0.967622 0.524600 0.076092 11.00000 0.03248 0.02339 = 0.02148 -0.00463 0.00357 -0.00853 AFIX 43 H2 2 0.940172 0.524384 0.012058 11.00000 -1.20000 AFIX 0 C3 1 1.052263 0.473844 0.096356 11.00000 0.03505 0.02246 = 0.02742 -0.00878 0.01315 -0.00577 AFIX 43 H3 2 1.083371 0.439502 0.045859 11.00000 -1.20000 AFIX 0 C4 1 1.092517 0.472423 0.189909 11.00000 0.02640 0.01831 = 0.03784 -0.00342 0.01026 0.00118 AFIX 43 H4 2 1.149019 0.434954 0.204084 11.00000 -1.20000 AFIX 0 C5 1 1.049703 0.526108 0.262684 11.00000 0.02413 0.01856 = 0.02393 0.00101 0.00423 0.00019 AFIX 43 H5 2 1.077495 0.525246 0.326572 11.00000 -1.20000 AFIX 0 C6 1 0.966142 0.581469 0.243136 11.00000 0.01976 0.01514 = 0.01793 -0.00009 0.00291 -0.00349 C7 1 0.921727 0.645447 0.316476 11.00000 0.01993 0.01838 = 0.01549 0.00368 0.00236 0.00064 C8 1 0.981252 0.690369 0.391087 11.00000 0.01759 0.01781 = 0.01655 0.00069 0.00166 -0.00150 C9 1 1.087572 0.687250 0.390968 11.00000 0.02190 0.02074 = 0.01409 -0.00104 0.00272 -0.00116 C10 1 0.930569 0.733841 0.468032 11.00000 0.01929 0.01462 = 0.01665 0.00202 0.00037 -0.00206 AFIX 43 H10 2 0.862573 0.716849 0.474252 11.00000 -1.20000 AFIX 0 C11 1 0.964831 0.797943 0.536436 11.00000 0.01955 0.01683 = 0.01513 -0.00033 0.00441 -0.00230 C12 1 1.049229 0.861959 0.525847 11.00000 0.01959 0.01806 = 0.01928 -0.00013 0.00423 -0.00161 C13 1 1.168499 0.927834 0.418014 11.00000 0.02495 0.03170 = 0.02662 0.00485 0.00442 -0.00817 AFIX 23 H13A 2 1.210474 0.900240 0.366513 11.00000 -1.20000 H13B 2 1.208772 0.931884 0.478603 11.00000 -1.20000 AFIX 0 C14 1 1.135617 1.023744 0.387496 11.00000 0.03820 0.02864 = 0.04059 0.00527 0.00045 -0.01103 AFIX 137 H14A 2 1.094983 1.019426 0.328036 11.00000 -1.50000 H14B 2 1.194251 1.062336 0.374939 11.00000 -1.50000 H14C 2 1.096241 1.051819 0.439674 11.00000 -1.50000 AFIX 0 C15 1 0.967906 0.777082 0.753371 11.00000 0.02020 0.01370 = 0.01770 -0.00082 0.00144 -0.00149 C16 1 1.069914 0.761560 0.752512 11.00000 0.02062 0.02248 = 0.02257 0.00146 0.00175 0.00056 AFIX 43 H16 2 1.107386 0.775533 0.695882 11.00000 -1.20000 AFIX 0 C17 1 1.117032 0.725511 0.834779 11.00000 0.02034 0.02641 = 0.03044 0.00008 -0.00355 0.00124 AFIX 43 H17 2 1.186833 0.714924 0.834466 11.00000 -1.20000 AFIX 0 C18 1 1.062211 0.705019 0.917225 11.00000 0.03307 0.02734 = 0.02222 -0.00038 -0.00578 0.00332 AFIX 43 H18 2 1.094466 0.679212 0.972833 11.00000 -1.20000 AFIX 0 C19 1 0.960822 0.721860 0.919184 11.00000 0.03352 0.03728 = 0.01817 0.00494 0.00369 0.00385 AFIX 43 H19 2 0.924079 0.708821 0.976516 11.00000 -1.20000 AFIX 0 C20 1 0.912605 0.757800 0.837495 11.00000 0.02357 0.02807 = 0.01887 -0.00039 0.00422 0.00348 AFIX 43 H20 2 0.842965 0.769202 0.838558 11.00000 -1.20000 AFIX 0 C21 1 0.870074 0.938240 0.658036 11.00000 0.01926 0.01479 = 0.02121 -0.00034 0.00306 -0.00161 C22 1 0.882908 0.985953 0.746323 11.00000 0.02269 0.02028 = 0.02714 -0.00498 0.00039 -0.00101 AFIX 43 H22 2 0.901458 0.953176 0.803774 11.00000 -1.20000 AFIX 0 C23 1 0.868321 1.081559 0.749297 11.00000 0.02572 0.02082 = 0.04368 -0.01405 0.00059 -0.00309 AFIX 43 H23 2 0.877104 1.114373 0.808850 11.00000 -1.20000 AFIX 0 C24 1 0.840977 1.128915 0.665371 11.00000 0.02489 0.01567 = 0.05374 -0.00099 0.00543 -0.00216 AFIX 43 H24 2 0.832111 1.194369 0.667756 11.00000 -1.20000 AFIX 0 C25 1 0.826348 1.082408 0.578027 11.00000 0.02555 0.02047 = 0.04100 0.01046 0.00415 0.00160 AFIX 43 H25 2 0.806133 1.115398 0.521244 11.00000 -1.20000 AFIX 0 C26 1 0.841589 0.986784 0.574347 11.00000 0.02512 0.02274 = 0.02567 0.00354 0.00086 -0.00190 AFIX 43 H26 2 0.832544 0.954441 0.514547 11.00000 -1.20000 AFIX 0 C27 1 0.788349 0.746931 0.646383 11.00000 0.01863 0.01660 = 0.01107 -0.00151 0.00155 -0.00112 C28 1 0.693224 0.785308 0.649194 11.00000 0.02296 0.01676 = 0.01761 -0.00202 -0.00105 0.00250 AFIX 43 H28 2 0.684732 0.850842 0.649994 11.00000 -1.20000 AFIX 0 C29 1 0.610801 0.726902 0.650819 11.00000 0.01627 0.02492 = 0.02377 -0.00228 0.00029 0.00140 AFIX 43 H29 2 0.545892 0.752996 0.652949 11.00000 -1.20000 AFIX 0 C30 1 0.621919 0.631559 0.649383 11.00000 0.01919 0.02386 = 0.02074 -0.00132 0.00333 -0.00532 AFIX 43 H30 2 0.564889 0.592525 0.649626 11.00000 -1.20000 AFIX 0 C31 1 0.716959 0.592557 0.647575 11.00000 0.02507 0.01464 = 0.02651 -0.00036 0.00094 -0.00029 AFIX 43 H31 2 0.724724 0.526949 0.646436 11.00000 -1.20000 AFIX 0 C32 1 0.799830 0.649524 0.647442 11.00000 0.01794 0.01740 = 0.02597 -0.00078 0.00395 0.00222 AFIX 43 H32 2 0.864599 0.623015 0.648065 11.00000 -1.20000 AFIX 0 N1 3 1.173156 0.681511 0.395230 11.00000 0.02193 0.03873 = 0.02515 0.00257 0.00067 -0.00012 O1 4 0.836752 0.621654 0.127131 11.00000 0.02663 0.02507 = 0.02463 -0.00165 -0.00507 -0.00138 AFIX 147 H1 2 0.807591 0.636804 0.178728 11.00000 -1.50000 AFIX 0 O2 4 0.831135 0.664193 0.309381 11.00000 0.01774 0.02837 = 0.02319 -0.00397 -0.00054 0.00156 O3 4 1.081437 0.908456 0.593544 11.00000 0.02744 0.02278 = 0.02193 -0.00319 0.00263 -0.00825 O4 4 1.081785 0.868898 0.434466 11.00000 0.03246 0.02620 = 0.01921 0.00100 0.00711 -0.01329 P1 5 0.899645 0.816363 0.647205 11.00000 0.01713 0.01367 = 0.01462 -0.00096 0.00179 -0.00133 HKLF 4 Covalent radii and connectivity table for s92 in Cc C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 C1 - O1 C2 C6 C2 - C3 C1 C3 - C2 C4 C4 - C3 C5 C5 - C4 C6 C6 - C5 C1 C7 C7 - O2 C8 C6 C8 - C10 C9 C7 C9 - N1 C8 C10 - C11 C8 C11 - C10 C12 P1 C12 - O3 O4 C11 C13 - O4 C14 C14 - C13 C15 - C16 C20 P1 C16 - C15 C17 C17 - C18 C16 C18 - C19 C17 C19 - C18 C20 C20 - C19 C15 C21 - C26 C22 P1 C22 - C23 C21 C23 - C24 C22 C24 - C25 C23 C25 - C24 C26 C26 - C25 C21 C27 - C28 C32 P1 C28 - C29 C27 C29 - C30 C28 C30 - C29 C31 C31 - C32 C30 C32 - C31 C27 N1 - C9 O1 - C1 O2 - C7 O3 - C12 O4 - C12 C13 P1 - C11 C27 C21 C15 Floating origin restraints generated 23499 Reflections read, of which 543 rejected -17 =< h =< 17, -18 =< k =< 18, -17 =< l =< 17, 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) 10 8 -8 59.65 1.71 5 10.29 11 5 -6 87.84 4.57 3 33.96 7 9 -5 198.81 4.93 5 29.88 7 11 -5 10.37 0.90 3 6.28 7 13 -5 46.80 1.82 3 17.57 8 4 -4 124.16 3.59 4 39.86 6 8 -3 167.28 8.13 2 83.11 4 4 -2 917.63 22.04 4 143.40 6 10 -2 21.08 1.02 2 28.70 0 2 -1 724.29 22.29 4 178.88 4 6 -1 249.92 7.26 3 70.67 5 3 1 296.34 4.31 5 42.09 6 10 1 43.83 1.00 3 25.44 11 3 2 21.10 0.93 5 5.59 7 13 2 47.66 1.02 3 49.56 8 10 4 60.65 1.02 4 33.31 16 Inconsistent equivalents 6014 Unique reflections, of which 0 suppressed R(int) = 0.0463 R(sigma) = 0.0484 Friedel opposites not merged Maximum memory for data reduction = 3179 / 70914 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 = 4128 / 438352 wR2 = 0.0766 before cycle 1 for 6014 data and 346 / 346 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33071 0.00042 -1.940 OSF 2 0.00642 0.00048 -0.458 EXTI Mean shift/esd = 0.340 Maximum = -1.940 for OSF Max. shift = 0.007 A for H1 Max. dU =-0.001 for C7 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0759 before cycle 2 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33035 0.00042 -0.876 OSF 2 0.00632 0.00047 -0.215 EXTI Mean shift/esd = 0.114 Maximum = -0.876 for OSF Max. shift = 0.002 A for H1 Max. dU = 0.000 for C7 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0758 before cycle 3 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33034 0.00041 -0.019 OSF 2 0.00631 0.00047 -0.027 EXTI Mean shift/esd = 0.004 Maximum = -0.027 for EXTI Max. shift = 0.000 A for H14C Max. dU = 0.000 for C14 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0758 before cycle 4 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33034 0.00041 0.000 OSF 2 0.00631 0.00047 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.009 for U13 C23 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C25 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0758 before cycle 5 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33034 0.00041 0.002 OSF 2 0.00631 0.00047 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for OSF Max. shift = 0.000 A for H1 Max. dU = 0.000 for C1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0758 before cycle 6 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33034 0.00041 0.001 OSF 2 0.00631 0.00047 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H14C Max. dU = 0.000 for C5 Least-squares cycle 7 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0758 before cycle 7 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33034 0.00041 0.000 OSF 2 0.00631 0.00047 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x O3 Max. shift = 0.000 A for C12 Max. dU = 0.000 for C24 Least-squares cycle 8 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0758 before cycle 8 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33034 0.00041 0.000 OSF 2 0.00631 0.00047 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x O3 Max. shift = 0.000 A for H14A Max. dU = 0.000 for C23 Least-squares cycle 9 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0758 before cycle 9 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33034 0.00041 0.000 OSF 2 0.00631 0.00047 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x O3 Max. shift = 0.000 A for H14C Max. dU = 0.000 for C24 Least-squares cycle 10 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0758 before cycle 10 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33034 0.00041 0.000 OSF 2 0.00631 0.00047 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x C9 Max. shift = 0.000 A for H14C Max. dU = 0.000 for C8 Least-squares cycle 11 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0758 before cycle 11 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33034 0.00041 0.000 OSF 2 0.00631 0.00047 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x O3 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C14 Least-squares cycle 12 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0758 before cycle 12 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33034 0.00041 0.000 OSF 2 0.00631 0.00047 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x O3 Max. shift = 0.000 A for H1 Max. dU = 0.000 for N1 Least-squares cycle 13 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0758 before cycle 13 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33034 0.00041 0.000 OSF 2 0.00631 0.00047 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x O3 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C19 Least-squares cycle 14 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0758 before cycle 14 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33034 0.00041 0.000 OSF 2 0.00631 0.00047 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x O3 Max. shift = 0.000 A for C15 Max. dU = 0.000 for O3 Least-squares cycle 15 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0758 before cycle 15 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33034 0.00041 0.000 OSF 2 0.00631 0.00047 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x O3 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C4 Least-squares cycle 16 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0758 before cycle 16 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33034 0.00041 0.000 OSF 2 0.00631 0.00047 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x O3 Max. shift = 0.000 A for C15 Max. dU = 0.000 for C14 Least-squares cycle 17 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0758 before cycle 17 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33034 0.00041 0.000 OSF 2 0.00631 0.00047 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x O3 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C20 Least-squares cycle 18 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0758 before cycle 18 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33034 0.00041 0.000 OSF 2 0.00631 0.00047 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x O3 Max. shift = 0.000 A for C15 Max. dU = 0.000 for C3 Least-squares cycle 19 Maximum vector length = 511 Memory required = 4128 / 438352 wR2 = 0.0758 before cycle 19 for 6014 data and 346 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33034 0.00041 -0.001 OSF 2 0.00631 0.00047 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H17 Max. dU = 0.000 for C13 Largest correlation matrix elements 0.603 EXTI / OSF Idealized hydrogen atom generation before cycle 20 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.9401 0.5243 0.0121 43 0.950 0.000 C2 C3 C1 H3 1.0833 0.4395 0.0459 43 0.950 0.000 C3 C2 C4 H4 1.1490 0.4351 0.2040 43 0.950 0.000 C4 C3 C5 H5 1.0777 0.5252 0.3263 43 0.950 0.000 C5 C4 C6 H10 0.8625 0.7170 0.4743 43 0.950 0.000 C10 C11 C8 H13A 1.2107 0.9004 0.3666 23 0.990 0.000 C13 O4 C14 H13B 1.2088 0.9320 0.4787 23 0.990 0.000 C13 O4 C14 H14A 1.0949 1.0192 0.3282 137 0.980 0.000 C14 C13 H14A H14B 1.1942 1.0622 0.3749 137 0.980 0.000 C14 C13 H14A H14C 1.0964 1.0517 0.4398 137 0.980 0.000 C14 C13 H14A H16 1.1075 0.7756 0.6960 43 0.950 0.000 C16 C15 C17 H17 1.1868 0.7147 0.8345 43 0.950 0.000 C17 C18 C16 H18 1.0945 0.6792 0.9728 43 0.950 0.000 C18 C19 C17 H19 0.9241 0.7089 0.9765 43 0.950 0.000 C19 C18 C20 H20 0.8431 0.7693 0.8385 43 0.950 0.000 C20 C19 C15 H22 0.9014 0.9532 0.8037 43 0.950 0.000 C22 C23 C21 H23 0.8772 1.1143 0.8089 43 0.950 0.000 C23 C24 C22 H24 0.8319 1.1944 0.6677 43 0.950 0.000 C24 C25 C23 H25 0.8064 1.1153 0.5213 43 0.950 0.000 C25 C24 C26 H26 0.8325 0.9546 0.5146 43 0.950 0.000 C26 C25 C21 H28 0.6848 0.8508 0.6499 43 0.950 0.000 C28 C29 C27 H29 0.5459 0.7531 0.6529 43 0.950 0.000 C29 C30 C28 H30 0.5651 0.5924 0.6496 43 0.950 0.000 C30 C29 C31 H31 0.7246 0.5270 0.6463 43 0.950 0.000 C31 C32 C30 H32 0.8647 0.6231 0.6481 43 0.950 0.000 C32 C31 C27 H1 0.8072 0.6362 0.1789 147 0.840 0.000 O1 C1 H1 s92 in Cc ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.92211 0.57630 0.14950 1.00000 0.02300 0.01386 0.01990 0.00059 0.00212 -0.00540 0.01891 0.00272 0.00012 0.00011 0.00012 0.00000 0.00090 0.00071 0.00079 0.00061 0.00066 0.00061 0.00034 C2 0.96756 0.52458 0.07613 1.00000 0.03269 0.02301 0.02033 -0.00469 0.00354 -0.00824 0.02533 0.00302 0.00014 0.00012 0.00013 0.00000 0.00095 0.00087 0.00084 0.00066 0.00069 0.00074 0.00037 H2 0.94008 0.52435 0.01211 1.00000 0.03039 0.00000 0.00000 C3 1.05221 0.47385 0.09638 1.00000 0.03466 0.02192 0.02714 -0.00877 0.01312 -0.00618 0.02785 0.00315 0.00014 0.00013 0.00013 0.00000 0.00102 0.00087 0.00094 0.00070 0.00076 0.00077 0.00040 H3 1.08330 0.43947 0.04590 1.00000 0.03342 0.00000 0.00000 C4 1.09247 0.47252 0.18986 1.00000 0.02555 0.01856 0.03690 -0.00336 0.00953 0.00115 0.02696 0.00327 0.00014 0.00012 0.00014 0.00000 0.00089 0.00085 0.00099 0.00071 0.00073 0.00071 0.00038 H4 1.14901 0.43510 0.20402 1.00000 0.03235 0.00000 0.00000 C5 1.04975 0.52608 0.26250 1.00000 0.02360 0.01805 0.02366 0.00103 0.00438 0.00016 0.02175 0.00300 0.00013 0.00011 0.00012 0.00000 0.00083 0.00080 0.00084 0.00063 0.00066 0.00067 0.00035 H5 1.07768 0.52525 0.32633 1.00000 0.02610 0.00000 0.00000 C6 0.96601 0.58143 0.24319 1.00000 0.01964 0.01485 0.01743 0.00051 0.00308 -0.00347 0.01729 0.00273 0.00012 0.00011 0.00011 0.00000 0.00079 0.00076 0.00077 0.00058 0.00062 0.00062 0.00032 C7 0.92171 0.64539 0.31644 1.00000 0.01914 0.01722 0.01519 0.00365 0.00255 0.00029 0.01717 0.00279 0.00012 0.00011 0.00011 0.00000 0.00079 0.00077 0.00074 0.00059 0.00058 0.00064 0.00032 C8 0.98120 0.69039 0.39111 1.00000 0.01694 0.01747 0.01637 0.00074 0.00147 -0.00136 0.01692 0.00270 0.00012 0.00011 0.00011 0.00000 0.00077 0.00076 0.00076 0.00057 0.00060 0.00062 0.00032 C9 1.08760 0.68724 0.39090 1.00000 0.02176 0.02016 0.01342 -0.00080 0.00280 -0.00111 0.01843 0.00279 0.00012 0.00011 0.00012 0.00000 0.00088 0.00081 0.00072 0.00060 0.00059 0.00065 0.00033 C10 0.93053 0.73388 0.46809 1.00000 0.01875 0.01486 0.01655 0.00198 0.00011 -0.00201 0.01672 0.00273 0.00012 0.00011 0.00011 0.00000 0.00079 0.00074 0.00075 0.00057 0.00059 0.00061 0.00031 H10 0.86251 0.71696 0.47430 1.00000 0.02006 0.00000 0.00000 C11 0.96490 0.79794 0.53654 1.00000 0.01892 0.01638 0.01515 -0.00027 0.00429 -0.00202 0.01679 0.00276 0.00012 0.00011 0.00011 0.00000 0.00076 0.00074 0.00073 0.00057 0.00058 0.00062 0.00031 C12 1.04919 0.86190 0.52593 1.00000 0.01942 0.01793 0.01885 -0.00013 0.00441 -0.00210 0.01871 0.00278 0.00012 0.00011 0.00012 0.00000 0.00081 0.00079 0.00078 0.00062 0.00063 0.00064 0.00033 C13 1.16862 0.92794 0.41807 1.00000 0.02548 0.03173 0.02603 0.00486 0.00429 -0.00857 0.02773 0.00323 0.00014 0.00013 0.00013 0.00000 0.00092 0.00099 0.00092 0.00073 0.00072 0.00077 0.00040 H13A 1.21067 0.90039 0.36661 1.00000 0.03327 0.00000 0.00000 H13B 1.20881 0.93201 0.47871 1.00000 0.03327 0.00000 0.00000 C14 1.13567 1.02359 0.38761 1.00000 0.03769 0.02877 0.04050 0.00584 0.00080 -0.01031 0.03565 0.00364 0.00016 0.00014 0.00016 0.00000 0.00113 0.00101 0.00113 0.00084 0.00087 0.00088 0.00046 H14A 1.09493 1.01919 0.32822 1.00000 0.05347 0.00000 0.00000 H14B 1.19424 1.06222 0.37491 1.00000 0.05347 0.00000 0.00000 H14C 1.09637 1.05167 0.43983 1.00000 0.05347 0.00000 0.00000 C15 0.96783 0.77703 0.75340 1.00000 0.01981 0.01362 0.01765 -0.00106 0.00133 -0.00101 0.01702 0.00273 0.00012 0.00011 0.00011 0.00000 0.00078 0.00072 0.00077 0.00058 0.00059 0.00061 0.00031 C16 1.06995 0.76156 0.75258 1.00000 0.02004 0.02200 0.02218 0.00123 0.00220 0.00005 0.02140 0.00296 0.00013 0.00012 0.00012 0.00000 0.00081 0.00083 0.00084 0.00063 0.00064 0.00067 0.00034 H16 1.10746 0.77565 0.69601 1.00000 0.02568 0.00000 0.00000 C17 1.11701 0.72539 0.83484 1.00000 0.01930 0.02568 0.03093 -0.00039 -0.00357 0.00106 0.02532 0.00307 0.00013 0.00013 0.00013 0.00000 0.00083 0.00091 0.00094 0.00071 0.00070 0.00071 0.00037 H17 1.18678 0.71465 0.83448 1.00000 0.03039 0.00000 0.00000 C18 1.06227 0.70501 0.91722 1.00000 0.03246 0.02752 0.02173 -0.00048 -0.00614 0.00393 0.02727 0.00320 0.00014 0.00013 0.00013 0.00000 0.00100 0.00094 0.00088 0.00069 0.00072 0.00078 0.00039 H18 1.09453 0.67924 0.97285 1.00000 0.03272 0.00000 0.00000 C19 0.96083 0.72189 0.91920 1.00000 0.03323 0.03760 0.01767 0.00481 0.00368 0.00389 0.02949 0.00345 0.00014 0.00014 0.00013 0.00000 0.00101 0.00109 0.00086 0.00074 0.00072 0.00083 0.00041 H19 0.92406 0.70888 0.97652 1.00000 0.03538 0.00000 0.00000 C20 0.91271 0.75785 0.83743 1.00000 0.02314 0.02779 0.01871 -0.00049 0.00384 0.00361 0.02319 0.00309 0.00013 0.00012 0.00012 0.00000 0.00085 0.00090 0.00082 0.00068 0.00067 0.00074 0.00036 H20 0.84308 0.76932 0.83849 1.00000 0.02783 0.00000 0.00000 C21 0.86998 0.93819 0.65812 1.00000 0.01884 0.01435 0.02094 -0.00055 0.00276 -0.00160 0.01803 0.00274 0.00012 0.00011 0.00012 0.00000 0.00079 0.00074 0.00080 0.00060 0.00063 0.00060 0.00033 C22 0.88282 0.98597 0.74623 1.00000 0.02209 0.02080 0.02658 -0.00501 0.00042 -0.00078 0.02316 0.00295 0.00013 0.00012 0.00013 0.00000 0.00084 0.00084 0.00087 0.00067 0.00069 0.00070 0.00036 H22 0.90135 0.95319 0.80368 1.00000 0.02779 0.00000 0.00000 C23 0.86834 1.08157 0.74935 1.00000 0.02447 0.02151 0.04224 -0.01385 0.00115 -0.00294 0.02940 0.00310 0.00014 0.00013 0.00015 0.00000 0.00090 0.00090 0.00110 0.00080 0.00079 0.00072 0.00041 H23 0.87722 1.11434 0.80891 1.00000 0.03528 0.00000 0.00000 C24 0.84092 1.12898 0.66535 1.00000 0.02400 0.01589 0.05366 -0.00061 0.00602 -0.00146 0.03116 0.00343 0.00014 0.00013 0.00016 0.00000 0.00090 0.00082 0.00122 0.00078 0.00084 0.00072 0.00042 H24 0.83192 1.19442 0.66768 1.00000 0.03739 0.00000 0.00000 C25 0.82647 1.08231 0.57814 1.00000 0.02538 0.02025 0.04054 0.01032 0.00424 0.00125 0.02870 0.00343 0.00014 0.00012 0.00014 0.00000 0.00092 0.00089 0.00109 0.00076 0.00078 0.00073 0.00040 H25 0.80640 1.11528 0.52130 1.00000 0.03445 0.00000 0.00000 C26 0.84155 0.98689 0.57440 1.00000 0.02412 0.02246 0.02502 0.00378 0.00135 -0.00131 0.02387 0.00314 0.00013 0.00012 0.00013 0.00000 0.00085 0.00087 0.00087 0.00068 0.00067 0.00070 0.00036 H26 0.83247 0.95461 0.51457 1.00000 0.02864 0.00000 0.00000 C27 0.78839 0.74703 0.64638 1.00000 0.01809 0.01617 0.01091 -0.00158 0.00139 -0.00150 0.01505 0.00266 0.00012 0.00011 0.00011 0.00000 0.00072 0.00077 0.00068 0.00055 0.00054 0.00059 0.00030 C28 0.69327 0.78530 0.64916 1.00000 0.02269 0.01599 0.01756 -0.00179 -0.00059 0.00234 0.01875 0.00279 0.00012 0.00011 0.00011 0.00000 0.00082 0.00079 0.00078 0.00060 0.00062 0.00066 0.00033 H28 0.68480 0.85084 0.64993 1.00000 0.02250 0.00000 0.00000 C29 0.61077 0.72703 0.65080 1.00000 0.01588 0.02428 0.02363 -0.00233 0.00017 0.00122 0.02127 0.00299 0.00013 0.00012 0.00013 0.00000 0.00075 0.00087 0.00082 0.00066 0.00061 0.00066 0.00034 H29 0.54585 0.75312 0.65293 1.00000 0.02552 0.00000 0.00000 C30 0.62211 0.63149 0.64935 1.00000 0.01910 0.02316 0.02067 -0.00142 0.00315 -0.00572 0.02096 0.00294 0.00013 0.00012 0.00012 0.00000 0.00076 0.00085 0.00080 0.00064 0.00062 0.00067 0.00034 H30 0.56513 0.59240 0.64961 1.00000 0.02515 0.00000 0.00000 C31 0.71686 0.59264 0.64753 1.00000 0.02513 0.01422 0.02590 -0.00059 0.00108 -0.00061 0.02175 0.00291 0.00013 0.00011 0.00012 0.00000 0.00086 0.00080 0.00087 0.00063 0.00067 0.00065 0.00035 H31 0.72461 0.52703 0.64635 1.00000 0.02610 0.00000 0.00000 C32 0.79990 0.64960 0.64744 1.00000 0.01741 0.01731 0.02522 -0.00074 0.00319 0.00193 0.01996 0.00295 0.00012 0.00012 0.00012 0.00000 0.00077 0.00081 0.00083 0.00063 0.00062 0.00064 0.00033 H32 0.86465 0.62307 0.64810 1.00000 0.02396 0.00000 0.00000 N1 1.17315 0.68153 0.39525 1.00000 0.02168 0.03755 0.02494 0.00238 0.00073 0.00012 0.02805 0.00274 0.00011 0.00012 0.00011 0.00000 0.00079 0.00091 0.00081 0.00065 0.00060 0.00066 0.00035 O1 0.83673 0.62178 0.12722 1.00000 0.02628 0.02490 0.02400 -0.00163 -0.00521 -0.00096 0.02508 0.00210 0.00009 0.00009 0.00009 0.00000 0.00063 0.00064 0.00060 0.00050 0.00050 0.00052 0.00027 H1 0.80723 0.63623 0.17885 1.00000 0.03762 0.00000 0.00000 O2 0.83112 0.66421 0.30933 1.00000 0.01752 0.02776 0.02313 -0.00418 -0.00051 0.00135 0.02281 0.00198 0.00008 0.00009 0.00008 0.00000 0.00057 0.00065 0.00063 0.00049 0.00047 0.00050 0.00026 O3 1.08144 0.90847 0.59356 1.00000 0.02671 0.02261 0.02174 -0.00303 0.00224 -0.00845 0.02368 0.00199 0.00009 0.00008 0.00008 0.00000 0.00062 0.00062 0.00060 0.00048 0.00048 0.00051 0.00026 O4 1.08177 0.86896 0.43440 1.00000 0.03195 0.02651 0.01853 0.00102 0.00701 -0.01357 0.02563 0.00206 0.00009 0.00009 0.00008 0.00000 0.00067 0.00065 0.00059 0.00047 0.00050 0.00053 0.00028 P1 0.89965 0.81637 0.64719 1.00000 0.01694 0.01349 0.01430 -0.00094 0.00182 -0.00118 0.01490 0.00065 0.00003 0.00003 0.00003 0.00000 0.00018 0.00018 0.00018 0.00015 0.00013 0.00016 0.00009 Final Structure Factor Calculation for s92 in Cc Total number of l.s. parameters = 346 Maximum vector length = 511 Memory required = 3784 / 26068 wR2 = 0.0758 before cycle 20 for 6014 data and 2 / 346 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0257 * P )^2 + 1.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0333 for 5700 Fo > 4sig(Fo) and 0.0369 for all 6014 data wR2 = 0.0758, GooF = S = 1.014, Restrained GooF = 1.014 for all data Flack x parameter = 0.0178 with esd 0.0577 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 = 38.00 for non-hydrogen and 26.00 for hydrogen atoms Principal mean square atomic displacements U 0.0259 0.0197 0.0111 C1 0.0389 0.0209 0.0162 C2 0.0482 0.0208 0.0146 C3 0.0423 0.0221 0.0165 C4 0.0279 0.0196 0.0177 C5 0.0226 0.0170 0.0123 C6 0.0214 0.0181 0.0119 C7 0.0186 0.0176 0.0145 C8 0.0231 0.0196 0.0126 C9 0.0198 0.0173 0.0130 C10 0.0222 0.0160 0.0122 C11 0.0238 0.0180 0.0143 C12 0.0380 0.0295 0.0157 C13 0.0462 0.0402 0.0206 C14 0.0206 0.0172 0.0133 C15 0.0240 0.0215 0.0187 C16 0.0321 0.0257 0.0181 C17 0.0370 0.0262 0.0187 C18 0.0413 0.0310 0.0162 C19 0.0299 0.0235 0.0161 C20 0.0229 0.0174 0.0138 C21 0.0295 0.0221 0.0178 C22 0.0493 0.0247 0.0141 C23 0.0547 0.0231 0.0156 C24 0.0457 0.0245 0.0159 C25 0.0277 0.0247 0.0191 C26 0.0193 0.0155 0.0104 C27 0.0237 0.0181 0.0145 C28 0.0264 0.0217 0.0157 C29 0.0283 0.0200 0.0145 C30 0.0265 0.0245 0.0142 C31 0.0262 0.0189 0.0147 C32 0.0380 0.0246 0.0216 N1 0.0307 0.0255 0.0191 O1 0.0304 0.0207 0.0173 O2 0.0343 0.0210 0.0158 O3 0.0439 0.0217 0.0113 O4 0.0182 0.0136 0.0129 P1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.035 0.051 0.065 0.079 0.094 0.111 0.131 0.160 0.212 1.000 Number in group 607. 648. 564. 598. 612. 585. 615. 589. 591. 605. GooF 1.015 1.117 1.076 1.006 1.038 1.045 0.975 0.925 0.916 1.005 K 1.047 0.985 0.979 1.000 0.991 1.004 1.011 1.014 1.011 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.64 inf Number in group 608. 615. 581. 602. 617. 599. 586. 615. 586. 605. GooF 1.063 0.960 0.999 1.007 0.957 0.939 0.933 0.880 1.101 1.253 K 0.999 1.030 1.024 1.015 1.012 1.005 1.013 1.005 1.003 1.006 R1 0.083 0.076 0.059 0.051 0.038 0.034 0.027 0.022 0.025 0.021 Recommended weighting scheme: WGHT 0.0144 1.4892 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) 2 6 -5 654.27 489.58 4.45 0.100 1.75 9 13 -3 0.00 81.11 3.97 0.041 0.87 17 1 0 75.53 163.78 3.81 0.058 0.79 -7 3 -1 3519.87 2995.31 3.77 0.248 1.77 2 2 0 1419.56 1718.70 3.74 0.188 4.91 -9 3 -11 -3.79 26.49 3.54 0.023 0.94 -3 3 4 271.70 200.18 3.53 0.064 2.37 -2 6 5 641.15 506.10 3.52 0.102 1.75 -3 3 7 513.80 406.41 3.51 0.091 1.68 -2 2 -3 3818.20 4336.75 3.49 0.298 3.34 5 3 3 585.51 461.11 3.48 0.097 2.08 -2 4 -7 147.95 96.19 3.45 0.044 1.66 4 2 8 580.77 456.22 3.43 0.097 1.49 3 3 -4 250.84 184.71 3.40 0.062 2.37 -4 16 0 399.21 572.05 3.36 0.108 0.87 11 7 1 221.96 143.27 3.36 0.054 1.05 2 4 7 161.39 108.68 3.33 0.047 1.66 -7 5 15 56.87 134.29 3.32 0.052 0.80 -10 0 0 721.54 877.52 3.32 0.134 1.34 -4 16 -8 342.60 495.20 3.28 0.101 0.77 -4 6 4 114.91 72.55 3.26 0.039 1.70 7 15 0 59.63 106.09 3.24 0.047 0.86 -9 9 -1 251.33 347.77 3.24 0.084 1.09 10 8 10 396.47 231.64 3.23 0.069 0.84 -3 1 -3 1915.05 2194.38 3.20 0.212 3.11 3 3 -7 502.87 405.63 3.17 0.091 1.68 -15 1 2 34.56 69.09 3.17 0.038 0.89 0 4 -7 387.60 483.69 3.17 0.100 1.72 2 4 -8 1247.91 1063.26 3.16 0.148 1.51 -11 9 -1 34.58 75.74 3.15 0.039 0.97 -3 13 -12 122.76 200.74 3.14 0.064 0.78 12 6 1 218.89 293.36 3.07 0.078 1.01 -6 16 2 -9.35 51.22 3.07 0.032 0.83 -4 18 -1 -28.32 60.29 3.07 0.035 0.78 -2 6 -3 150.12 106.03 3.04 0.047 2.02 -3 1 -2 2770.91 3116.77 2.97 0.253 3.62 6 4 6 296.85 227.44 2.97 0.068 1.46 -10 10 -10 186.07 289.71 2.96 0.077 0.80 -9 1 13 581.16 757.60 2.96 0.125 0.86 -10 6 -4 384.04 299.12 2.95 0.078 1.11 6 4 4 814.99 671.32 2.95 0.117 1.66 3 5 6 444.19 356.37 2.94 0.086 1.66 0 4 2 3347.74 3761.66 2.92 0.278 3.19 -15 3 8 45.95 118.46 2.89 0.049 0.79 7 5 3 697.36 572.08 2.87 0.108 1.50 -16 6 -2 124.18 187.46 2.83 0.062 0.79 -1 9 1 455.44 369.05 2.83 0.087 1.58 -17 3 0 80.84 164.97 2.81 0.058 0.78 2 2 3 3882.54 4325.43 2.81 0.298 3.34 8 0 8 343.76 257.62 2.79 0.073 1.20 Bond lengths and angles C1 - Distance Angles O1 1.3537 (0.0020) C2 1.3957 (0.0024) 117.99 (0.15) C6 1.4117 (0.0022) 121.87 (0.14) 120.13 (0.15) C1 - O1 C2 C2 - Distance Angles C3 1.3779 (0.0028) C1 1.3957 (0.0024) 120.12 (0.16) H2 0.9500 119.94 119.94 C2 - C3 C1 C3 - Distance Angles C2 1.3779 (0.0028) C4 1.3879 (0.0027) 120.60 (0.16) H3 0.9500 119.70 119.70 C3 - C2 C4 C4 - Distance Angles C3 1.3879 (0.0027) C5 1.3870 (0.0023) 119.69 (0.17) H4 0.9500 120.16 120.16 C4 - C3 C5 C5 - Distance Angles C4 1.3870 (0.0023) C6 1.4022 (0.0023) 121.03 (0.16) H5 0.9500 119.48 119.48 C5 - C4 C6 C6 - Distance Angles C5 1.4022 (0.0023) C1 1.4117 (0.0022) 118.13 (0.14) C7 1.4896 (0.0021) 123.19 (0.15) 118.67 (0.14) C6 - C5 C1 C7 - Distance Angles O2 1.2498 (0.0020) C8 1.4474 (0.0022) 119.38 (0.14) C6 1.4896 (0.0021) 118.34 (0.14) 122.17 (0.14) C7 - O2 C8 C8 - Distance Angles C10 1.4071 (0.0021) C9 1.4300 (0.0022) 120.30 (0.14) C7 1.4474 (0.0022) 117.53 (0.14) 122.09 (0.14) C8 - C10 C9 C9 - Distance Angles N1 1.1533 (0.0022) C8 1.4300 (0.0022) 176.18 (0.18) C9 - N1 C10 - Distance Angles C11 1.3920 (0.0022) C8 1.4071 (0.0021) 129.83 (0.15) H10 0.9500 115.08 115.08 C10 - C11 C8 C11 - Distance Angles C10 1.3920 (0.0022) C12 1.4672 (0.0022) 126.94 (0.14) P1 1.7777 (0.0015) 120.75 (0.12) 112.12 (0.11) C11 - C10 C12 C12 - Distance Angles O3 1.2212 (0.0020) O4 1.3362 (0.0019) 123.70 (0.15) C11 1.4672 (0.0022) 122.61 (0.14) 113.52 (0.13) C12 - O3 O4 C13 - Distance Angles O4 1.4613 (0.0021) C14 1.5041 (0.0027) 109.90 (0.15) H13A 0.9900 109.68 109.68 H13B 0.9900 109.68 109.68 108.18 C13 - O4 C14 H13A C14 - Distance Angles C13 1.5041 (0.0027) 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 1.3898 (0.0023) C20 1.4015 (0.0022) 120.16 (0.15) P1 1.8061 (0.0016) 122.59 (0.12) 117.19 (0.12) C15 - C16 C20 C16 - Distance Angles C15 1.3898 (0.0023) C17 1.3903 (0.0025) 119.77 (0.15) H16 0.9500 120.11 120.11 C16 - C15 C17 C17 - Distance Angles C18 1.3839 (0.0027) C16 1.3903 (0.0025) 120.04 (0.17) H17 0.9500 119.98 119.98 C17 - C18 C16 C18 - Distance Angles C19 1.3846 (0.0027) C17 1.3839 (0.0027) 120.50 (0.17) H18 0.9500 119.75 119.75 C18 - C19 C17 C19 - Distance Angles C18 1.3846 (0.0027) C20 1.3903 (0.0025) 120.10 (0.16) H19 0.9500 119.95 119.95 C19 - C18 C20 C20 - Distance Angles C19 1.3903 (0.0025) C15 1.4015 (0.0022) 119.41 (0.16) H20 0.9500 120.29 120.29 C20 - C19 C15 C21 - Distance Angles C26 1.3960 (0.0023) C22 1.3999 (0.0023) 119.64 (0.16) P1 1.8042 (0.0016) 118.61 (0.13) 121.54 (0.13) C21 - C26 C22 C22 - Distance Angles C23 1.3900 (0.0026) C21 1.3999 (0.0023) 119.76 (0.17) H22 0.9500 120.12 120.12 C22 - C23 C21 C23 - Distance Angles C24 1.3864 (0.0029) C22 1.3900 (0.0026) 119.85 (0.17) H23 0.9500 120.07 120.07 C23 - C24 C22 C24 - Distance Angles C25 1.3841 (0.0029) C23 1.3864 (0.0030) 120.93 (0.17) H24 0.9500 119.53 119.53 C24 - C25 C23 C25 - Distance Angles C24 1.3841 (0.0029) C26 1.3890 (0.0025) 119.47 (0.17) H25 0.9500 120.27 120.27 C25 - C24 C26 C26 - Distance Angles C25 1.3890 (0.0025) C21 1.3960 (0.0023) 120.34 (0.17) H26 0.9500 119.83 119.83 C26 - C25 C21 C27 - Distance Angles C28 1.3923 (0.0023) C32 1.4106 (0.0022) 119.56 (0.15) P1 1.7970 (0.0016) 122.93 (0.12) 117.44 (0.12) C27 - C28 C32 C28 - Distance Angles C29 1.3900 (0.0024) C27 1.3923 (0.0023) 119.60 (0.15) H28 0.9500 120.20 120.20 C28 - C29 C27 C29 - Distance Angles C30 1.3834 (0.0024) C28 1.3900 (0.0024) 120.75 (0.16) H29 0.9500 119.62 119.62 C29 - C30 C28 C30 - Distance Angles C29 1.3834 (0.0024) C31 1.3907 (0.0025) 120.05 (0.16) H30 0.9500 119.98 119.98 C30 - C29 C31 C31 - Distance Angles C32 1.3842 (0.0024) C30 1.3907 (0.0025) 119.97 (0.15) H31 0.9500 120.01 120.01 C31 - C32 C30 C32 - Distance Angles C31 1.3842 (0.0024) C27 1.4106 (0.0022) 120.03 (0.15) H32 0.9500 119.99 119.99 C32 - C31 C27 N1 - Distance Angles C9 1.1533 (0.0022) N1 - O1 - Distance Angles C1 1.3537 (0.0020) H1 0.8400 109.47 O1 - C1 O2 - Distance Angles C7 1.2498 (0.0020) O2 - O3 - Distance Angles C12 1.2212 (0.0020) O3 - O4 - Distance Angles C12 1.3362 (0.0019) C13 1.4613 (0.0021) 117.09 (0.13) O4 - C12 P1 - Distance Angles C11 1.7777 (0.0015) C27 1.7970 (0.0016) 109.08 (0.07) C21 1.8042 (0.0016) 109.05 (0.07) 110.84 (0.07) C15 1.8061 (0.0016) 113.04 (0.08) 104.35 (0.07) 110.40 (0.07) P1 - C11 C27 C21 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.86 2.5726(17) 141.8 O1-H1...O2 FMAP and GRID set by program FMAP 2 2 19 GRID -1.563 -2 -2 1.563 2 2 R1 = 0.0299 for 3036 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.19 at 0.1100 0.0315 0.8982 [ 0.88 A from C14 ] Deepest hole -0.19 at 0.8812 0.1743 0.1889 [ 0.64 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 3817 / 27011 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.1100 0.9685 0.3982 1.00000 0.05 0.19 0.88 C14 1.01 C13 1.22 H14A 1.34 H14C Q2 1 1.0328 0.9096 0.4065 1.00000 0.05 0.19 0.96 O4 1.79 C12 1.85 C13 2.09 H14A Q3 1 0.8461 0.7714 0.6576 1.00000 0.05 0.19 0.86 C27 0.98 P1 1.86 C32 2.07 C28 Q4 1 0.8867 0.8868 0.6526 1.00000 0.05 0.18 0.78 C21 1.03 P1 1.89 C26 1.92 C22 Q5 1 0.8001 0.7015 0.6437 1.00000 0.05 0.17 0.67 C27 0.75 C32 1.42 H32 1.88 C28 Q6 1 0.8225 1.1072 0.6227 1.00000 0.05 0.16 0.71 C24 0.71 C25 1.40 H24 1.41 H25 Q7 1 0.8603 0.9678 0.6203 1.00000 0.05 0.15 0.68 C21 0.73 C26 1.51 H26 1.77 C22 Q8 1 0.9048 0.5420 0.6592 1.00000 0.05 0.15 1.29 H32 1.71 C2 1.72 C1 2.10 C32 Q9 1 1.2372 0.9361 0.4041 1.00000 0.05 0.15 0.81 H13A 0.95 C13 1.10 H13B 1.87 C14 Q10 1 0.5920 0.6561 0.7321 1.00000 0.05 0.14 1.26 C30 1.50 H30 1.53 C29 1.87 H29 Shortest distances between peaks (including symmetry equivalents) 3 5 1.19 4 7 1.30 1 2 1.34 3 4 1.75 1 9 1.77 6 7 2.07 2 10 2.70 5 8 2.70 2 9 2.77 3 7 2.88 1 10 2.91 4 5 2.91 Time profile in seconds ----------------------- 0.14: 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. 1.89: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 14.25: Structure factors and derivatives 30.88: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.27: Apply other restraints 2.81: Solve l.s. equations 0.00: Generate HTAB table 0.19: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.08: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.08: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 11:44:37 Total CPU time: 50.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++