+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005slh1128 started at 11:39:08 on 23-Oct-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005slh1128 in P1 P-1 CELL 0.71073 8.1800 9.8839 10.4172 90.737 101.898 100.785 ZERR 1.00 0.0002 0.0002 0.0002 0.001 0.001 0.001 LATT 1 SFAC C H CD N O P S UNIT 28 32 1 2 4 2 4 V = 808.42 F(000) = 388.0 Mu = 1.07 mm-1 Cell Wt = 763.14 Rho = 1.568 MERG 2 OMIT -3.00 55.00 OMIT -1 2 1 OMIT -1 1 0 OMIT 0 1 1 FMAP 2 PLAN 5 SIZE 0.20 0.20 0.30 ACTA BOND $H L.S. 8 TEMP -153.00 WGHT 0.032600 1.171500 EXTI 0.010448 FVAR 0.95427 C1 1 1.019870 0.772784 0.544901 11.00000 0.01816 0.02842 = 0.01734 0.00643 -0.00177 0.00146 AFIX 23 H1A 2 1.024378 0.674639 0.559420 11.00000 -1.20000 H1B 2 0.955065 0.804714 0.605859 11.00000 -1.20000 AFIX 0 C2 1 1.196816 0.857544 0.569963 11.00000 0.01771 0.02238 = 0.02814 -0.00411 0.00193 0.00087 AFIX 137 H2A 2 1.260010 0.825263 0.509247 11.00000 -1.50000 H2B 2 1.254925 0.848122 0.660630 11.00000 -1.50000 H2C 2 1.191124 0.954626 0.556386 11.00000 -1.50000 C3 1 0.698138 0.776326 0.197247 11.00000 0.01964 0.03788 = 0.01316 0.00594 0.00527 0.01561 C4 1 0.799142 0.892823 0.161232 11.00000 0.05504 0.01700 = 0.01404 0.00021 -0.00194 0.01318 AFIX 43 H4 2 0.897549 0.939312 0.221863 11.00000 -1.20000 AFIX 7 C5 1 0.756161 0.941299 0.036503 11.00000 0.07085 0.01933 = 0.01590 0.00372 0.00293 0.01827 AFIX 43 H5 2 0.825191 1.020920 0.011889 11.00000 -1.20000 AFIX 7 C6 1 0.612178 0.873277 -0.052211 11.00000 0.03539 0.05933 = 0.01310 0.01067 0.00756 0.03384 C7 1 0.511173 0.756782 -0.016198 11.00000 0.01462 0.13994 = 0.01915 0.03020 -0.00066 0.00253 AFIX 43 H7 2 0.412766 0.710294 -0.076830 11.00000 -1.20000 AFIX 7 C8 1 0.554151 0.708305 0.108529 11.00000 0.01653 0.11673 = 0.02008 0.02633 0.00168 -0.00425 AFIX 43 H8 2 0.485118 0.628684 0.133142 11.00000 -1.20000 AFIX 7 C9 1 0.661648 1.022817 -0.224346 11.00000 0.11429 0.03536 = 0.01819 0.01264 0.00132 0.03106 H9A 2 0.666047 1.106511 -0.171250 11.00000 -1.50000 H9B 2 0.611129 1.034784 -0.316305 11.00000 -1.50000 H9C 2 0.777264 1.005805 -0.217736 11.00000 -1.50000 AFIX 0 C10 1 0.183849 0.581281 0.285315 11.00000 0.02705 0.05069 = 0.01152 -0.00907 -0.00311 0.02239 AFIX 43 H10 2 0.191190 0.646868 0.354750 11.00000 -1.20000 AFIX 0 C11 1 0.072462 0.589506 0.167358 11.00000 0.02748 0.04942 = 0.01586 -0.00908 -0.00516 0.02662 AFIX 43 H11 2 0.005757 0.659221 0.157649 11.00000 -1.20000 AFIX 0 C12 1 0.058289 0.496848 0.064224 11.00000 0.01562 0.01369 = 0.01260 0.00106 -0.00249 0.00070 C13 1 0.156644 0.397564 0.087959 11.00000 0.08970 0.03306 = 0.03244 -0.02369 -0.04001 0.04174 AFIX 43 H13 2 0.151285 0.329884 0.020849 11.00000 -1.20000 AFIX 0 C14 1 0.263396 0.396131 0.209469 11.00000 0.07763 0.02836 = 0.03184 -0.01593 -0.03521 0.03456 AFIX 43 H14 2 0.328162 0.325253 0.223600 11.00000 -1.20000 AFIX 0 CD1 3 0.500000 0.500000 0.500000 10.50000 0.01736 0.01331 = 0.01244 0.00245 -0.00550 0.00015 N1 4 0.280121 0.487728 0.306660 11.00000 0.01506 0.01640 = 0.01328 0.00236 -0.00299 -0.00129 O1 5 0.936799 0.787884 0.409598 11.00000 0.01468 0.02245 = 0.01586 0.00527 0.00235 0.00348 O2 5 0.561041 0.909171 -0.177783 11.00000 0.04339 0.07753 = 0.01605 0.01856 0.00686 0.03521 P1 6 0.743441 0.709849 0.359332 11.00000 0.01396 0.01876 = 0.01160 0.00163 0.00135 0.00625 S1 7 0.595195 0.768146 0.471833 11.00000 0.01496 0.01219 = 0.01463 0.00084 0.00407 0.00292 S2 7 0.725682 0.505681 0.345362 11.00000 0.02069 0.01998 = 0.02219 -0.00522 -0.00068 0.00991 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 Covalent radii and connectivity table for 2005slh1128 in P1 P-1 C 0.770 H 0.320 CD 1.490 N 0.700 O 0.660 P 1.100 S 1.030 C1 - O1 C2 C2 - C1 C3 - C4 C8 P1 C4 - C3 C5 C5 - C6 C4 C6 - O2 C7 C5 C7 - C6 C8 C8 - C7 C3 C9 - O2 C10 - N1 C11 C11 - C12 C10 C12 - C11 C13 C12_$1 C13 - C12 C14 C14 - N1 C13 Cd1 - N1 N1_$2 S1 S1_$2 S2_$2 S2 N1 - C10 C14 Cd1 O1 - C1 P1 O2 - C6 C9 P1 - O1 C3 S2 S1 S1 - P1 Cd1 S2 - P1 Cd1 Operators for generating equivalent atoms: $1 -x, -y+1, -z $2 -x+1, -y+1, -z+1 16306 Reflections read, of which 5 rejected -10 =< h =< 10, -12 =< k =< 12, -13 =< l =< 13, Max. 2-theta = 54.99 0 Systematic absence violations 0 Inconsistent equivalents 3694 Unique reflections, of which 0 suppressed R(int) = 0.0422 R(sigma) = 0.0317 Friedel opposites merged Maximum memory for data reduction = 2113 / 36701 Special position constraints for Cd1 x = 0.5000 y = 0.5000 z = 0.5000 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 2620 / 212289 wR2 = 0.0760 before cycle 1 for 3694 data and 168 / 172 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0326 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.95428 0.00177 0.004 OSF 2 0.01045 0.00168 0.000 EXTI Mean shift/esd = 0.003 Maximum = 0.044 for U13 Cd1 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2620 / 212289 wR2 = 0.0759 before cycle 2 for 3694 data and 168 / 172 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0326 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.95427 0.00177 -0.001 OSF 2 0.01045 0.00168 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.015 for U13 Cd1 Max. shift = 0.000 A for C14 Max. dU = 0.000 for C1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2620 / 212289 wR2 = 0.0759 before cycle 3 for 3694 data and 168 / 172 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0326 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.95427 0.00177 -0.001 OSF 2 0.01045 0.00168 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C5 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2620 / 212289 wR2 = 0.0759 before cycle 4 for 3694 data and 168 / 172 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0326 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.95427 0.00177 0.000 OSF 2 0.01045 0.00168 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y S2 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C10 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2620 / 212289 wR2 = 0.0759 before cycle 5 for 3694 data and 168 / 172 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0326 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.95427 0.00177 0.000 OSF 2 0.01045 0.00168 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y S2 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C7 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2620 / 212289 wR2 = 0.0759 before cycle 6 for 3694 data and 168 / 172 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0326 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.95427 0.00177 0.000 OSF 2 0.01045 0.00168 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y S2 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C8 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2620 / 212289 wR2 = 0.0759 before cycle 7 for 3694 data and 168 / 172 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0326 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.95427 0.00177 0.000 OSF 2 0.01045 0.00168 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y S2 Max. shift = 0.000 A for H9C Max. dU = 0.000 for C6 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2620 / 212289 wR2 = 0.0759 before cycle 8 for 3694 data and 168 / 172 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0326 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.95427 0.00177 -0.001 OSF 2 0.01045 0.00168 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for C3 Max. dU = 0.000 for C9 Largest correlation matrix elements -0.844 tors H2A / y C2 0.645 U11 Cd1 / OSF 0.542 U12 C6 / U22 C6 0.682 EXTI / OSF 0.605 z C2 / y C2 0.531 U12 C14 / U11 C14 -0.664 tors H2A / z C2 0.598 tors H2A / x C2 0.522 U12 C6 / U11 C6 0.653 U22 Cd1 / OSF 0.577 U12 C13 / U11 C13 0.516 U13 C13 / U23 C13 0.650 U33 Cd1 / OSF 0.546 U12 C13 / U22 C13 0.507 U12 C14 / U22 C14 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 1.0244 0.6746 0.5594 23 0.990 0.000 C1 O1 C2 H1B 0.9551 0.8047 0.6059 23 0.990 0.000 C1 O1 C2 H2A 1.2600 0.8253 0.5092 137 0.980 0.000 C2 C1 H2A H2B 1.2549 0.8481 0.6606 137 0.980 0.000 C2 C1 H2A H2C 1.1911 0.9546 0.5564 137 0.980 0.000 C2 C1 H2A H4 0.8975 0.9393 0.2219 43 0.950 0.000 C4 C3 C5 H5 0.8252 1.0209 0.0119 43 0.950 0.000 C5 C6 C4 H7 0.4128 0.7103 -0.0768 43 0.950 0.000 C7 C6 C8 H8 0.4851 0.6287 0.1331 43 0.950 0.000 C8 C7 C3 H10 0.1912 0.6469 0.3548 43 0.950 0.000 C10 N1 C11 H11 0.0058 0.6592 0.1576 43 0.950 0.000 C11 C12 C10 H13 0.1513 0.3299 0.0208 43 0.950 0.000 C13 C12 C14 H14 0.3282 0.3253 0.2236 43 0.950 0.000 C14 N1 C13 2005slh1128 in P1 P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 1.01987 0.77278 0.54490 1.00000 0.01816 0.02842 0.01734 0.00643 -0.00177 0.00146 0.02247 0.00454 0.00028 0.00025 0.00022 0.00000 0.00105 0.00119 0.00104 0.00087 0.00082 0.00088 0.00046 H1A 1.02438 0.67464 0.55942 1.00000 0.02697 0.00000 0.00000 H1B 0.95507 0.80471 0.60586 1.00000 0.02697 0.00000 0.00000 C2 1.19682 0.85754 0.56996 1.00000 0.01771 0.02238 0.02814 -0.00411 0.00193 0.00087 0.02362 0.00259 0.00015 0.00019 0.00012 0.00000 0.00105 0.00110 0.00119 0.00090 0.00089 0.00085 0.00047 H2A 1.26001 0.82526 0.50925 1.00000 0.03544 0.00000 0.00000 H2B 1.25492 0.84812 0.66063 1.00000 0.03544 0.00000 0.00000 H2C 1.19112 0.95463 0.55639 1.00000 0.03544 0.00000 0.00000 C3 0.69814 0.77633 0.19725 1.00000 0.01964 0.03788 0.01316 0.00594 0.00527 0.01561 0.02193 0.00203 0.00012 0.00011 0.00009 0.00000 0.00104 0.00130 0.00097 0.00089 0.00081 0.00094 0.00046 C4 0.79914 0.89282 0.16123 1.00000 0.05504 0.01700 0.01404 0.00021 -0.00194 0.01318 0.02924 0.00207 0.00012 0.00011 0.00009 0.00000 0.00164 0.00108 0.00103 0.00083 0.00102 0.00104 0.00056 H4 0.89755 0.93931 0.22186 1.00000 0.03508 0.00000 0.00000 C5 0.75616 0.94130 0.03650 1.00000 0.07085 0.01933 0.01590 0.00372 0.00293 0.01827 0.03499 0.00206 0.00012 0.00011 0.00009 0.00000 0.00201 0.00115 0.00111 0.00089 0.00117 0.00120 0.00065 H5 0.82519 1.02092 0.01189 1.00000 0.04199 0.00000 0.00000 C6 0.61218 0.87328 -0.05221 1.00000 0.03539 0.05933 0.01310 0.01067 0.00756 0.03384 0.03224 0.00204 0.00012 0.00011 0.00009 0.00000 0.00136 0.00176 0.00106 0.00106 0.00097 0.00129 0.00061 C7 0.51117 0.75678 -0.01620 1.00000 0.01462 0.13994 0.01915 0.03020 -0.00066 0.00253 0.05994 0.00202 0.00012 0.00011 0.00009 0.00000 0.00119 0.00370 0.00130 0.00175 0.00100 0.00163 0.00119 H7 0.41277 0.71029 -0.07683 1.00000 0.07193 0.00000 0.00000 C8 0.55415 0.70830 0.10853 1.00000 0.01653 0.11673 0.02008 0.02633 0.00168 -0.00425 0.05351 0.00201 0.00013 0.00011 0.00009 0.00000 0.00120 0.00314 0.00130 0.00161 0.00100 0.00150 0.00104 H8 0.48512 0.62868 0.13314 1.00000 0.06421 0.00000 0.00000 C9 0.66165 1.02282 -0.22435 1.00000 0.11429 0.03536 0.01819 0.01264 0.00132 0.03106 0.05552 0.00205 0.00012 0.00011 0.00009 0.00000 0.00324 0.00160 0.00127 0.00115 0.00158 0.00182 0.00103 H9A 0.66605 1.10651 -0.17125 1.00000 0.08329 0.00000 0.00000 H9B 0.61113 1.03478 -0.31631 1.00000 0.08329 0.00000 0.00000 H9C 0.77726 1.00580 -0.21774 1.00000 0.08329 0.00000 0.00000 C10 0.18385 0.58128 0.28531 1.00000 0.02705 0.05069 0.01152 -0.00907 -0.00311 0.02239 0.02894 0.00516 0.00032 0.00030 0.00022 0.00000 0.00120 0.00158 0.00100 0.00097 0.00088 0.00111 0.00056 H10 0.19119 0.64687 0.35475 1.00000 0.03472 0.00000 0.00000 C11 0.07246 0.58951 0.16736 1.00000 0.02748 0.04942 0.01586 -0.00908 -0.00516 0.02662 0.02991 0.00520 0.00032 0.00030 0.00023 0.00000 0.00123 0.00158 0.00108 0.00102 0.00092 0.00114 0.00058 H11 0.00576 0.65922 0.15765 1.00000 0.03589 0.00000 0.00000 C12 0.05829 0.49685 0.06422 1.00000 0.01562 0.01369 0.01260 0.00106 -0.00249 0.00070 0.01506 0.00390 0.00026 0.00021 0.00019 0.00000 0.00094 0.00092 0.00096 0.00072 0.00078 0.00073 0.00039 C13 0.15664 0.39756 0.08796 1.00000 0.08970 0.03306 0.03244 -0.02369 -0.04001 0.04174 0.05577 0.00593 0.00050 0.00031 0.00030 0.00000 0.00260 0.00152 0.00151 0.00123 0.00163 0.00168 0.00112 H13 0.15128 0.32988 0.02085 1.00000 0.06693 0.00000 0.00000 C14 0.26340 0.39613 0.20947 1.00000 0.07763 0.02836 0.03184 -0.01593 -0.03521 0.03456 0.04975 0.00573 0.00047 0.00030 0.00029 0.00000 0.00230 0.00139 0.00146 0.00115 0.00150 0.00148 0.00097 H14 0.32816 0.32525 0.22360 1.00000 0.05970 0.00000 0.00000 Cd1 0.50000 0.50000 0.50000 0.50000 0.01736 0.01331 0.01244 0.00245 -0.00550 0.00015 0.01600 0.00000 0.00000 0.00000 0.00000 0.00000 0.00013 0.00013 0.00012 0.00007 0.00008 0.00008 0.00009 N1 0.28012 0.48773 0.30666 1.00000 0.01506 0.01640 0.01328 0.00236 -0.00299 -0.00129 0.01635 0.00342 0.00022 0.00018 0.00017 0.00000 0.00083 0.00084 0.00081 0.00065 0.00065 0.00065 0.00035 O1 0.93680 0.78788 0.40960 1.00000 0.01468 0.02245 0.01586 0.00527 0.00235 0.00348 0.01777 0.00307 0.00019 0.00016 0.00015 0.00000 0.00070 0.00077 0.00072 0.00058 0.00056 0.00057 0.00031 O2 0.56104 0.90917 -0.17778 1.00000 0.04339 0.07753 0.01605 0.01856 0.00686 0.03521 0.04232 0.00484 0.00027 0.00026 0.00018 0.00000 0.00114 0.00157 0.00086 0.00092 0.00079 0.00111 0.00053 P1 0.74344 0.70985 0.35933 1.00000 0.01396 0.01876 0.01160 0.00163 0.00135 0.00625 0.01456 0.00107 0.00007 0.00006 0.00005 0.00000 0.00025 0.00026 0.00024 0.00019 0.00019 0.00020 0.00013 S1 0.59519 0.76815 0.47183 1.00000 0.01496 0.01219 0.01463 0.00084 0.00407 0.00292 0.01375 0.00099 0.00006 0.00005 0.00005 0.00000 0.00024 0.00023 0.00024 0.00017 0.00018 0.00017 0.00012 S2 0.72568 0.50568 0.34536 1.00000 0.02069 0.01998 0.02219 -0.00522 -0.00068 0.00991 0.02099 0.00110 0.00007 0.00006 0.00006 0.00000 0.00027 0.00027 0.00027 0.00020 0.00021 0.00021 0.00013 Final Structure Factor Calculation for 2005slh1128 in P1 P-1 Total number of l.s. parameters = 172 Maximum vector length = 511 Memory required = 2452 / 26061 wR2 = 0.0759 before cycle 9 for 3694 data and 0 / 172 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0326 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0298 for 3527 Fo > 4sig(Fo) and 0.0313 for all 3694 data wR2 = 0.0759, GooF = S = 1.042, Restrained GooF = 1.042 for all data Occupancy sum of asymmetric unit = 20.50 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0347 0.0204 0.0124 C1 0.0319 0.0231 0.0158 C2 0.0409 0.0128 0.0121 C3 0.0599 0.0147 0.0131 C4 0.0739 0.0186 0.0125 C5 0.0708 0.0153 0.0106 C6 0.1517 0.0178 0.0103 C7 0.1309 0.0160 0.0136 C8 0.1205 0.0365 0.0096 C9 0.0611 0.0164 0.0093 C10 0.0647 0.0140 0.0111 C11 0.0224 0.0134 0.0094 C12 0.1450 0.0139 0.0084 C13 0.1254 0.0137 0.0102 C14 0.0282 0.0125 0.0073 Cd1 0.0259 0.0140 0.0091 N1 0.0249 0.0153 0.0131 O1 0.0866 0.0302 0.0102 O2 0.0198 0.0136 0.0103 P1 0.0156 0.0136 0.0121 S1 0.0335 0.0172 0.0123 S2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.037 0.070 0.099 0.133 0.168 0.203 0.244 0.300 0.379 1.000 Number in group 373. 374. 362. 370. 373. 372. 360. 372. 366. 372. GooF 1.018 1.137 1.025 1.037 1.044 0.956 1.046 0.992 0.995 1.153 K 1.162 0.981 0.992 0.981 0.993 1.005 1.001 1.007 1.010 1.004 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 377. 363. 373. 372. 369. 363. 376. 362. 369. 370. GooF 1.102 0.947 0.967 0.988 0.919 0.908 0.874 0.939 1.121 1.504 K 0.974 1.005 1.006 1.012 1.012 1.019 1.014 1.016 1.004 0.992 R1 0.055 0.042 0.039 0.036 0.030 0.027 0.023 0.024 0.025 0.029 Recommended weighting scheme: WGHT 0.0326 1.1711 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 -4 1 68.55 24.08 6.21 0.046 1.92 0 4 3 55.80 24.90 4.52 0.047 1.92 -4 0 4 5.36 25.89 4.13 0.048 1.74 -1 3 3 1171.08 1445.44 4.11 0.358 2.37 -2 -4 2 3317.30 2808.71 3.99 0.499 1.87 0 0 2 2408.29 2852.57 3.64 0.503 5.09 -1 12 4 332.34 489.78 3.63 0.208 0.77 0 3 3 13.88 3.15 3.56 0.017 2.28 4 -1 1 519.85 645.94 3.54 0.239 1.89 0 -1 4 28.48 11.45 3.51 0.032 2.49 -9 -4 2 112.42 171.18 3.46 0.123 0.79 -7 -6 8 40.92 77.51 3.45 0.083 0.78 0 10 4 137.92 195.54 3.43 0.132 0.89 -7 -5 7 250.00 335.30 3.37 0.172 0.84 -1 -3 2 207.38 274.09 3.37 0.156 2.59 2 -1 2 5289.60 6088.42 3.33 0.735 2.85 -3 4 0 114.08 163.22 3.31 0.120 1.98 -1 10 4 53.85 28.98 3.28 0.051 0.91 0 6 0 300.19 379.29 3.24 0.183 1.62 2 0 4 1485.91 1739.57 3.21 0.393 1.95 -2 2 5 433.04 530.74 3.16 0.217 1.87 -1 2 0 564.50 683.43 3.15 0.246 4.54 -2 -1 3 625.21 753.45 3.09 0.258 2.70 4 1 2 124.13 87.71 3.08 0.088 1.64 -2 5 2 240.98 307.91 3.03 0.165 1.80 2 -3 5 58.90 90.38 3.03 0.090 1.57 3 2 3 388.32 475.82 3.03 0.205 1.67 -6 -3 4 265.01 207.16 3.01 0.136 1.13 5 6 7 219.39 288.40 3.01 0.160 0.78 6 0 0 273.34 213.97 2.96 0.138 1.31 1 -1 5 244.91 191.50 2.95 0.130 1.88 -1 -5 3 394.79 321.89 2.86 0.169 1.66 -3 4 3 234.50 183.49 2.86 0.128 1.80 -4 0 6 628.74 525.44 2.85 0.216 1.44 2 10 5 278.75 351.54 2.84 0.177 0.80 -5 -5 4 1340.11 1162.07 2.84 0.321 1.10 -2 10 4 945.97 794.73 2.83 0.265 0.92 -1 10 3 83.09 54.34 2.83 0.069 0.94 0 11 4 304.72 387.74 2.82 0.185 0.82 -5 -1 3 921.16 787.60 2.82 0.264 1.50 -3 12 4 185.10 250.51 2.77 0.149 0.78 -8 -6 1 25.95 49.18 2.76 0.066 0.78 -5 3 2 60.63 38.55 2.76 0.058 1.55 -2 4 1 1859.78 2112.74 2.75 0.433 2.25 7 -5 3 884.04 752.29 2.68 0.258 0.97 6 -11 2 100.50 142.32 2.67 0.112 0.79 1 -3 3 1095.15 1251.22 2.63 0.333 2.30 5 2 8 124.03 165.48 2.63 0.121 0.86 -2 4 5 246.96 304.18 2.61 0.164 1.57 -2 10 5 118.72 158.03 2.60 0.118 0.89 Bond lengths and angles C1 - Distance Angles O1 1.4557 (0.0025) C2 1.4999 (0.0024) 108.38 (0.16) H1A 0.9900 110.02 110.02 H1B 0.9900 110.02 110.02 108.38 C1 - O1 C2 H1A C2 - Distance Angles C1 1.4999 (0.0024) H2A 0.9800 109.47 H2B 0.9800 109.47 109.47 H2C 0.9800 109.47 109.47 109.47 C2 - C1 H2A H2B C3 - Distance Angles C4 1.3900 C8 1.3900 120.00 P1 1.8115 (0.0010) 122.40 117.58 C3 - C4 C8 C4 - Distance Angles C3 1.3900 C5 1.3900 120.00 H4 0.9500 120.00 120.00 C4 - C3 C5 C5 - Distance Angles C6 1.3900 C4 1.3900 120.00 H5 0.9500 120.00 120.00 C5 - C6 C4 C6 - Distance Angles O2 1.3616 (0.0019) C7 1.3900 115.02 (0.11) C5 1.3900 124.95 (0.11) 120.00 C6 - O2 C7 C7 - Distance Angles C6 1.3900 C8 1.3900 120.00 H7 0.9500 120.00 120.00 C7 - C6 C8 C8 - Distance Angles C7 1.3900 C3 1.3900 120.00 H8 0.9500 120.00 120.00 C8 - C7 C3 C9 - Distance Angles O2 1.4167 (0.0025) H9A 0.9800 109.46 H9B 0.9800 109.43 109.47 H9C 0.9800 109.52 109.47 109.47 C9 - O2 H9A H9B C10 - Distance Angles N1 1.3154 (0.0031) C11 1.3840 (0.0031) 123.67 (0.22) H10 0.9500 118.17 118.17 C10 - N1 C11 C11 - Distance Angles C12 1.3748 (0.0030) C10 1.3840 (0.0031) 120.04 (0.22) H11 0.9500 119.98 119.98 C11 - C12 C10 C12 - Distance Angles C11 1.3748 (0.0030) C13 1.3752 (0.0033) 116.04 (0.20) C12_$1 1.4839 (0.0038) 121.66 (0.24) 122.29 (0.24) C12 - C11 C13 C13 - Distance Angles C12 1.3752 (0.0033) C14 1.3836 (0.0034) 120.07 (0.24) H13 0.9500 119.96 119.96 C13 - C12 C14 C14 - Distance Angles N1 1.3177 (0.0032) C13 1.3836 (0.0034) 123.57 (0.24) H14 0.9500 118.22 118.22 C14 - N1 C13 Cd1 - Distance Angles N1 2.3926 (0.0017) N1_$2 2.3926 (0.0017) 180.00 S1 2.6568 (0.0005) 89.45 (0.04) 90.55 (0.04) S1_$2 2.6568 (0.0005) 90.55 (0.04) 89.45 (0.04) 180.00 S2_$2 2.6825 (0.0006) 91.31 (0.05) 88.69 (0.05) 102.65 (0.02) 77.35 (0.02) S2 2.6825 (0.0006) 88.69 (0.05) 91.31 (0.05) 77.35 (0.02) 102.65 (0.02) 180.00 Cd1 - N1 N1_$2 S1 S1_$2 S2_$2 N1 - Distance Angles C10 1.3154 (0.0031) C14 1.3177 (0.0032) 116.57 (0.20) Cd1 2.3926 (0.0017) 121.82 (0.15) 121.13 (0.16) N1 - C10 C14 O1 - Distance Angles C1 1.4557 (0.0025) P1 1.6007 (0.0015) 118.11 (0.13) O1 - C1 O2 - Distance Angles C6 1.3616 (0.0019) C9 1.4167 (0.0025) 118.60 (0.18) O2 - C6 P1 - Distance Angles O1 1.6007 (0.0016) C3 1.8115 (0.0010) 99.96 (0.07) S2 1.9971 (0.0008) 111.39 (0.06) 110.26 (0.05) S1 2.0015 (0.0007) 110.50 (0.06) 110.87 (0.04) 113.11 (0.03) P1 - O1 C3 S2 S1 - Distance Angles P1 2.0015 (0.0007) Cd1 2.6568 (0.0005) 85.07 (0.02) S1 - P1 S2 - Distance Angles P1 1.9971 (0.0008) Cd1 2.6825 (0.0006) 84.46 (0.02) S2 - P1 FMAP and GRID set by program FMAP 2 1 21 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.0308 for 3694 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.66 at 0.4675 0.1854 0.0166 [ 0.57 A from C7 ] Deepest hole -0.69 at 0.4926 0.3405 0.0343 [ 0.97 A from C7 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 2476 / 19962 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5325 0.8146 -0.0166 1.00000 0.05 0.66 0.57 C7 0.93 C6 1.33 H7 1.69 C8 Q2 1 0.5760 0.7644 0.1334 1.00000 0.05 0.54 0.59 C8 1.07 C3 1.41 H8 1.54 C7 Q3 1 0.5972 0.6769 0.0926 1.00000 0.05 0.49 0.56 C8 1.12 H8 1.46 C3 1.52 C7 Q4 1 0.7568 0.8650 0.1631 1.00000 0.05 0.48 0.40 C4 1.02 C3 1.27 H4 1.53 C5 Q5 1 0.1976 0.4386 0.0577 1.00000 0.05 0.46 0.61 C13 1.11 H13 1.38 C12 1.65 C14 Shortest distances between peaks (including symmetry equivalents) 2 3 1.02 2 4 1.59 1 2 1.63 1 3 1.87 3 4 2.09 1 4 2.31 3 5 2.89 Time profile in seconds ----------------------- 0.04: 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 0.00: Analyse other restraints etc. 0.76: 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 1.49: Structure factors and derivatives 1.73: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.20: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.07: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005slh1128 finished at 11:39:13 Total CPU time: 4.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++