+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 02sot051 started at 13:29:00 on 30-Jul-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02SOT051 in P-1 CELL 0.71073 8.9559 9.0489 24.0779 85.016 88.263 87.538 ZERR 4.00 0.0004 0.0004 0.0013 0.002 0.001 0.002 LATT 1 SFAC C H N O SI S UNIT 72 112 8 8 4 4 V = 1941.43 F(000) = 784.0 Mu = 0.24 mm-1 Cell Wt = 1458.30 Rho = 1.247 MERG 2 OMIT 1 2 2 OMIT 2 4 7 OMIT 2 2 8 OMIT -2 -5 2 OMIT -1 2 3 OMIT 0 1 5 OMIT 0 1 4 OMIT -3 -2 6 OMIT 0 2 0 OMIT 3 0 1 OMIT -2 -4 1 OMIT -5 -5 7 OMIT -1 6 5 OMIT -1 1 5 OMIT 6 1 4 OMIT -1 0 4 ISOR C28 C31 C32 FMAP 2 OMIT -3 55 EXTI SIZE 0.3 0.14 0.1 TEMP -153 PLAN 10 BOND $H WGHT 0.09020 8.29620 L.S. 4 FVAR 0.52015 MOLE 1 C1 1 0.095589 0.210991 0.213115 11.00000 0.06217 0.05232 = 0.04154 -0.00144 0.01142 -0.01745 AFIX 137 H1A 2 0.009005 0.223216 0.190359 11.00000 -1.50000 H1B 2 0.084139 0.274392 0.243053 11.00000 -1.50000 H1C 2 0.106355 0.109471 0.228196 11.00000 -1.50000 AFIX 0 C2 1 0.232442 0.251597 0.178202 11.00000 0.04551 0.02960 = 0.04106 -0.00017 0.00771 -0.00819 C3 1 0.369582 0.269362 0.202448 11.00000 0.06224 0.05488 = 0.03351 0.01068 -0.00512 -0.01342 AFIX 43 H3 2 0.377531 0.253529 0.240947 11.00000 -1.20000 AFIX 0 C4 1 0.493037 0.309926 0.170225 11.00000 0.04481 0.05460 = 0.04270 0.01434 -0.01175 -0.01108 AFIX 43 H4 2 0.583229 0.322650 0.187009 11.00000 -1.20000 AFIX 0 C5 1 0.482999 0.331840 0.112723 11.00000 0.03540 0.02426 = 0.03483 -0.00143 -0.00104 -0.00104 C6 1 0.347825 0.315111 0.087731 11.00000 0.03328 0.02779 = 0.03470 -0.00428 -0.00185 -0.00799 AFIX 43 H6 2 0.340265 0.332217 0.049253 11.00000 -1.20000 AFIX 0 C7 1 0.224091 0.272797 0.120347 11.00000 0.03880 0.03469 = 0.03498 -0.00414 0.00214 -0.00949 AFIX 43 H7 2 0.134509 0.258403 0.103414 11.00000 -1.20000 AFIX 0 C8 1 0.456727 0.693260 0.134659 11.00000 0.03619 0.04535 = 0.04816 -0.01601 0.00795 -0.00663 AFIX 13 H8 2 0.384680 0.620373 0.126222 11.00000 -1.20000 AFIX 0 C9 1 0.443038 0.727055 0.194635 11.00000 0.09147 0.06472 = 0.04370 -0.01534 0.01730 -0.00263 AFIX 23 H9A 2 0.339779 0.755442 0.203194 11.00000 -1.20000 H9B 2 0.468921 0.637736 0.218191 11.00000 -1.20000 AFIX 0 C10 1 0.538497 0.845615 0.207861 11.00000 0.07504 0.07877 = 0.04880 -0.01909 0.00727 0.00582 AFIX 23 H10A 2 0.543671 0.847201 0.247986 11.00000 -1.20000 H10B 2 0.496861 0.940875 0.192729 11.00000 -1.20000 AFIX 0 C11 1 0.692369 0.819153 0.183192 11.00000 0.05596 0.03648 = 0.04267 -0.00542 0.00136 0.00294 AFIX 23 H11A 2 0.742372 0.739225 0.205900 11.00000 -1.20000 H11B 2 0.748316 0.907765 0.185479 11.00000 -1.20000 AFIX 0 C12 1 0.698926 0.779240 0.121616 11.00000 0.03742 0.02532 = 0.03400 -0.00700 -0.00322 -0.00300 C13 1 0.604770 0.893145 0.086392 11.00000 0.04667 0.02948 = 0.04002 -0.00830 -0.00882 -0.00016 C14 1 0.439745 0.838994 0.094989 11.00000 0.05267 0.07163 = 0.04727 -0.01954 -0.01204 0.02743 AFIX 23 H14A 2 0.375722 0.912588 0.112025 11.00000 -1.20000 H14B 2 0.398308 0.819208 0.059750 11.00000 -1.20000 AFIX 0 C15 1 0.642132 1.008469 0.056042 11.00000 0.07085 0.05043 = 0.06210 -0.00399 -0.01127 0.00954 AFIX 93 H15A 2 0.741798 1.033723 0.053059 11.00000 -1.20000 H15B 2 0.569786 1.067540 0.036834 11.00000 -1.20000 AFIX 0 C16 1 0.991725 0.595636 0.142133 11.00000 0.03849 0.04616 = 0.07927 -0.01023 -0.01979 -0.00248 AFIX 137 H16A 2 0.936896 0.508076 0.138876 11.00000 -1.50000 H16B 2 0.989517 0.618316 0.180372 11.00000 -1.50000 H16C 2 1.093461 0.578780 0.129767 11.00000 -1.50000 AFIX 0 C17 1 1.002453 0.927193 0.112233 11.00000 0.04847 0.04828 = 0.08949 -0.02177 -0.00536 -0.02067 AFIX 137 H17A 2 1.027371 0.921906 0.150873 11.00000 -1.50000 H17B 2 0.937655 1.012822 0.103530 11.00000 -1.50000 H17C 2 1.092194 0.934761 0.089508 11.00000 -1.50000 AFIX 0 C18 1 0.932044 0.727863 0.022884 11.00000 0.03641 0.07870 = 0.05196 -0.01975 0.01249 -0.02310 AFIX 137 H18A 2 1.036082 0.734829 0.012620 11.00000 -1.50000 H18B 2 0.874942 0.803099 0.001223 11.00000 -1.50000 H18C 2 0.899267 0.631724 0.015901 11.00000 -1.50000 AFIX 0 C19 1 0.736433 0.131939 0.285008 11.00000 0.05331 0.10643 = 0.06749 -0.02662 -0.00213 0.00933 AFIX 137 H19A 2 0.738973 0.041757 0.309170 11.00000 -1.50000 H19B 2 0.830429 0.141451 0.265046 11.00000 -1.50000 H19C 2 0.657684 0.129443 0.258970 11.00000 -1.50000 AFIX 0 C20 1 0.708764 0.261309 0.318981 11.00000 0.01990 0.08148 = 0.05941 -0.01173 -0.00585 0.00648 C21 1 0.713604 0.407372 0.296087 11.00000 0.03447 0.10177 = 0.04405 -0.01332 -0.00285 -0.00868 AFIX 43 H21 2 0.740545 0.425807 0.258599 11.00000 -1.20000 AFIX 0 C22 1 0.679482 0.526711 0.327417 11.00000 0.03220 0.08934 = 0.03853 0.00692 -0.00858 -0.00734 AFIX 43 H22 2 0.683866 0.623948 0.311580 11.00000 -1.20000 AFIX 0 C23 1 0.638778 0.496182 0.382930 11.00000 0.02145 0.06882 = 0.04154 0.00281 -0.00568 0.00138 C24 1 0.635910 0.353584 0.407155 11.00000 0.03430 0.07785 = 0.04569 0.00957 -0.00245 0.01315 AFIX 43 H24 2 0.611055 0.335694 0.444851 11.00000 -1.20000 AFIX 0 C25 1 0.670478 0.235698 0.374917 11.00000 0.03300 0.06857 = 0.05955 -0.00119 -0.00431 0.01437 AFIX 43 H25 2 0.667784 0.138758 0.391176 11.00000 -1.20000 AFIX 0 C26 1 0.266199 0.513937 0.362642 11.00000 0.05224 0.05017 = 0.12276 0.00473 -0.03181 -0.00818 AFIX 13 H26 2 0.353620 0.455407 0.350237 11.00000 -1.20000 AFIX 0 C27 1 0.180410 0.421370 0.397808 11.00000 0.08348 0.20296 = 0.11796 0.05167 -0.05044 -0.03294 AFIX 23 H27A 2 0.143306 0.343019 0.377560 11.00000 -1.20000 H27B 2 0.240211 0.376067 0.428135 11.00000 -1.20000 AFIX 0 C28 1 0.062949 0.504152 0.418545 11.00000 0.19639 0.09514 = 0.06328 0.01883 0.03817 0.06946 AFIX 23 H28A 2 0.033182 0.453435 0.454047 11.00000 -1.20000 H28B 2 -0.019392 0.497888 0.393708 11.00000 -1.20000 AFIX 0 C29 1 0.072846 0.662678 0.427908 11.00000 0.03261 0.09154 = 0.05398 -0.00899 -0.01422 -0.00769 AFIX 23 H29A 2 0.107442 0.669712 0.465339 11.00000 -1.20000 H29B 2 -0.026529 0.709497 0.425733 11.00000 -1.20000 AFIX 0 C30 1 0.178919 0.750335 0.385730 11.00000 0.02627 0.08012 = 0.03731 -0.00628 -0.00754 0.01405 C31 1 0.114889 0.737452 0.326606 11.00000 0.04478 0.19421 = 0.04382 -0.01217 -0.01769 0.05066 C32 1 0.173640 0.570888 0.308861 11.00000 0.15561 0.16968 = 0.04353 -0.05120 0.02796 -0.09883 AFIX 23 H32A 2 0.090883 0.508094 0.303783 11.00000 -1.20000 H32B 2 0.236665 0.577595 0.275330 11.00000 -1.20000 AFIX 0 C33 1 0.004254 0.803825 0.307072 11.00000 0.17519 0.19561 = 0.10063 0.03237 -0.01979 0.01019 AFIX 93 H33A 2 -0.050970 0.869793 0.327933 11.00000 -1.20000 H33B 2 -0.024764 0.788395 0.271337 11.00000 -1.20000 AFIX 0 C34 1 0.344193 1.028400 0.345851 11.00000 0.08138 0.07504 = 0.05919 0.01408 0.01153 0.01562 AFIX 137 H34A 2 0.299499 1.025992 0.310219 11.00000 -1.50000 H34B 2 0.437575 0.972159 0.346217 11.00000 -1.50000 H34C 2 0.361422 1.129338 0.352405 11.00000 -1.50000 AFIX 0 C35 1 0.034188 1.056647 0.401651 11.00000 0.07446 0.10879 = 0.08692 -0.01466 -0.01766 0.04668 AFIX 137 H35A 2 0.006792 1.085648 0.363906 11.00000 -1.50000 H35B 2 0.044721 1.143659 0.421113 11.00000 -1.50000 H35C 2 -0.042102 0.997231 0.419919 11.00000 -1.50000 AFIX 0 C36 1 0.298217 0.955768 0.471250 11.00000 0.04831 0.07723 = 0.05101 -0.00018 -0.00871 0.01014 AFIX 137 H36A 2 0.290179 1.056233 0.481291 11.00000 -1.50000 H36B 2 0.401619 0.923294 0.469805 11.00000 -1.50000 H36C 2 0.245269 0.892732 0.498553 11.00000 -1.50000 AFIX 0 N1 3 0.623083 0.580168 0.069747 11.00000 0.03785 0.02652 = 0.03388 -0.00265 0.00752 -0.00599 AFIX 43 H1 2 0.621992 0.635150 0.038767 11.00000 -1.20000 AFIX 0 N2 3 0.612965 0.639665 0.123090 11.00000 0.02971 0.03321 = 0.03392 -0.00632 0.00103 0.00000 N3 3 0.399046 0.637333 0.430514 11.00000 0.02546 0.08435 = 0.03156 0.00358 -0.00574 0.00347 AFIX 43 H3A 2 0.355018 0.624755 0.462716 11.00000 -1.20000 AFIX 0 N4 3 0.319313 0.654091 0.380102 11.00000 0.02891 0.06106 = 0.03126 0.00074 -0.00595 0.00485 O1 4 0.768943 0.347744 0.101483 11.00000 0.03153 0.03707 = 0.06559 -0.01017 -0.00817 0.00308 O2 4 0.620825 0.366208 0.015906 11.00000 0.03738 0.02915 = 0.04092 -0.01004 0.00700 -0.00306 O3 4 0.632097 0.611130 0.478857 11.00000 0.03263 0.07846 = 0.03734 0.00117 -0.00965 0.00339 O4 4 0.619559 0.781459 0.392512 11.00000 0.03839 0.06845 = 0.05319 0.00952 -0.00879 -0.00427 SI1 5 0.904676 0.754805 0.098092 11.00000 0.02801 0.03743 = 0.04273 -0.00823 -0.00304 -0.00542 SI2 5 0.216022 0.946168 0.401683 11.00000 0.04611 0.07467 = 0.03709 0.00559 -0.00028 0.02270 S1 6 0.636983 0.397391 0.072874 11.00000 0.02805 0.02694 = 0.04365 -0.00610 0.00119 -0.00192 S2 6 0.580899 0.643730 0.422782 11.00000 0.02677 0.06852 = 0.03906 0.00550 -0.00666 0.00191 HKLF 4 Covalent radii and connectivity table for 02SOT051 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 S 1.030 C1 - C2 C2 - C7 C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C4 C6 S1 C6 - C7 C5 C7 - C6 C2 C8 - N2 C9 C14 C9 - C10 C8 C10 - C9 C11 C11 - C10 C12 C12 - N2 C13 C11 Si1 C13 - C15 C12 C14 C14 - C8 C13 C15 - C13 C16 - Si1 C17 - Si1 C18 - Si1 C19 - C20 C20 - C25 C21 C19 C21 - C22 C20 C22 - C23 C21 C23 - C24 C22 S2 C24 - C23 C25 C25 - C20 C24 C26 - C27 N4 C32 C27 - C28 C26 C28 - C27 C29 C29 - C28 C30 C30 - N4 C29 C31 Si2 C31 - C33 C30 C32 C32 - C26 C31 C33 - C31 C34 - Si2 C35 - Si2 C36 - Si2 N1 - N2 S1 N2 - N1 C8 C12 N3 - N4 S2 N4 - N3 C26 C30 O1 - S1 O2 - S1 O3 - S2 O4 - S2 Si1 - C18 C16 C17 C12 Si2 - C36 C34 C35 C30 S1 - O1 O2 N1 C5 S2 - O4 O3 N3 C23 13804 Reflections read, of which 54 rejected -11 =< h =< 11, -8 =< k =< 10, -31 =< l =< 31, Max. 2-theta = 54.89 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 1 0 720.82 21.06 3 180.75 0 3 0 1749.86 72.38 2 872.27 0 4 0 23.88 0.95 2 15.85 -5 -6 1 44.62 0.90 3 14.80 0 -5 1 24.93 0.71 3 6.56 -3 -4 1 103.66 3.07 3 26.73 -1 -3 1 685.61 27.13 2 236.49 -1 -1 1 408.80 19.82 2 149.26 1 1 1 1084.68 34.25 3 238.24 -1 -4 2 766.51 21.28 3 200.87 -1 -5 3 811.09 16.82 3 256.51 3 4 3 45.80 0.95 3 16.97 0 5 3 148.61 1.04 3 90.56 4 5 3 24.05 0.85 3 8.43 0 6 3 46.54 1.76 2 23.70 0 -7 4 121.07 7.90 2 45.25 -4 -6 4 33.74 1.01 2 25.37 -1 -5 4 14.79 0.75 2 5.78 4 5 4 43.08 0.94 3 14.84 -3 -6 5 95.55 1.91 3 36.16 1 4 5 25.91 0.86 3 8.05 0 6 5 50.53 0.87 4 9.53 0 7 8 20.23 0.95 2 6.88 4 6 9 13.17 0.75 2 5.26 2 -4 14 46.08 2.24 2 11.94 1 -4 15 406.56 15.23 2 99.66 26 Inconsistent equivalents 6515 Unique reflections, of which 0 suppressed R(int) = 0.0484 R(sigma) = 0.0608 Friedel opposites merged Maximum memory for data reduction = 4914 / 67382 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 = 6220 / 575550 wR2 = 0.2571 before cycle 1 for 6515 data and 442 / 442 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.056 0.000 GooF = S = 1.065; Restrained GooF = 1.064 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0902 * P )^2 + 8.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52555 0.00206 2.628 OSF 2 0.00911 0.00265 3.442 EXTI Mean shift/esd = 0.179 Maximum = 3.442 for EXTI Max. shift = 0.027 A for H35C Max. dU = 0.002 for C32 Least-squares cycle 2 Maximum vector length = 511 Memory required = 6220 / 575550 wR2 = 0.2556 before cycle 2 for 6515 data and 442 / 442 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.056 0.000 GooF = S = 1.055; Restrained GooF = 1.054 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0902 * P )^2 + 8.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52803 0.00211 1.171 OSF 2 0.01462 0.00310 1.777 EXTI Mean shift/esd = 0.086 Maximum = 1.777 for EXTI Max. shift = 0.028 A for H35C Max. dU =-0.001 for C27 Least-squares cycle 3 Maximum vector length = 511 Memory required = 6220 / 575550 wR2 = 0.2551 before cycle 3 for 6515 data and 442 / 442 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.056 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0902 * P )^2 + 8.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52836 0.00215 0.153 OSF 2 0.01541 0.00336 0.237 EXTI Mean shift/esd = 0.021 Maximum = 0.298 for tors H35A Max. shift = 0.021 A for H35C Max. dU =-0.001 for C33 Least-squares cycle 4 Maximum vector length = 511 Memory required = 6220 / 575550 wR2 = 0.2550 before cycle 4 for 6515 data and 442 / 442 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.056 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0902 * P )^2 + 8.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52842 0.00215 0.031 OSF 2 0.01554 0.00339 0.037 EXTI Mean shift/esd = 0.011 Maximum = 0.230 for tors H35A Max. shift = 0.017 A for H35A Max. dU = 0.000 for C33 Largest correlation matrix elements 0.629 EXTI / OSF -0.514 U13 C32 / U23 C32 -0.586 U12 C32 / U11 C32 -0.513 U12 C32 / U22 C32 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.0072 0.2231 0.1899 137 0.980 0.000 C1 C2 H1A H1B 0.0833 0.2769 0.2436 137 0.980 0.000 C1 C2 H1A H1C 0.1067 0.1082 0.2290 137 0.980 0.000 C1 C2 H1A H3 0.3773 0.2527 0.2418 43 0.950 0.000 C3 C4 C2 H4 0.5851 0.3226 0.1875 43 0.950 0.000 C4 C3 C5 H6 0.3399 0.3321 0.0484 43 0.950 0.000 C6 C7 C5 H7 0.1327 0.2580 0.1031 43 0.950 0.000 C7 C6 C2 H8 0.3832 0.6190 0.1260 13 1.000 0.000 C8 N2 C9 C14 H9A 0.3373 0.7556 0.2033 23 0.990 0.000 C9 C10 C8 H9B 0.4691 0.6354 0.2186 23 0.990 0.000 C9 C10 C8 H10A 0.5439 0.8471 0.2489 23 0.990 0.000 C10 C9 C11 H10B 0.4960 0.9429 0.1925 23 0.990 0.000 C10 C9 C11 H11A 0.7435 0.7376 0.2063 23 0.990 0.000 C11 C10 C12 H11B 0.7495 0.9096 0.1855 23 0.990 0.000 C11 C10 C12 H14A 0.3743 0.9140 0.1123 23 0.990 0.000 C14 C8 C13 H14B 0.3973 0.8185 0.0590 23 0.990 0.000 C14 C8 C13 H15A 0.7443 1.0337 0.0528 93 0.950 0.000 C15 C13 C12 H15B 0.5686 1.0688 0.0362 93 0.950 0.000 C15 C13 C12 H16A 0.9398 0.5053 0.1371 137 0.980 0.000 C16 Si1 H16A H16B 0.9830 0.6168 0.1816 137 0.980 0.000 C16 Si1 H16A H16C 1.0973 0.5833 0.1314 137 0.980 0.000 C16 Si1 H16A H17A 1.0261 0.9220 0.1518 137 0.980 0.000 C17 Si1 H17A H17B 0.9359 1.0142 0.1029 137 0.980 0.000 C17 Si1 H17A H17C 1.0940 0.9341 0.0894 137 0.980 0.000 C17 Si1 H17A H18A 1.0383 0.7359 0.0123 137 0.980 0.000 C18 Si1 H18A H18B 0.8732 0.8039 0.0008 137 0.980 0.000 C18 Si1 H18A H18C 0.8998 0.6292 0.0158 137 0.980 0.000 C18 Si1 H18A H19A 0.7340 0.0398 0.3091 137 0.980 0.000 C19 C20 H19A H19B 0.8349 0.1394 0.2660 137 0.980 0.000 C19 C20 H19A H19C 0.6591 0.1328 0.2569 137 0.980 0.000 C19 C20 H19A H21 0.7406 0.4261 0.2578 43 0.950 0.000 C21 C22 C20 H22 0.6837 0.6263 0.3113 43 0.950 0.000 C22 C23 C21 H24 0.6103 0.3352 0.4457 43 0.950 0.000 C24 C23 C25 H25 0.6674 0.1369 0.3916 43 0.950 0.000 C25 C20 C24 H26 0.3553 0.4540 0.3502 13 1.000 0.000 C26 C27 N4 C32 H27A 0.1429 0.3412 0.3777 23 0.990 0.000 C27 C28 C26 H27B 0.2414 0.3763 0.4293 23 0.990 0.000 C27 C28 C26 H28A 0.0322 0.4528 0.4546 23 0.990 0.000 C28 C27 C29 H28B -0.0203 0.4980 0.3929 23 0.990 0.000 C28 C27 C29 H29A 0.1085 0.6697 0.4659 23 0.990 0.000 C29 C28 C30 H29B -0.0282 0.7102 0.4255 23 0.990 0.000 C29 C28 C30 H32A 0.0896 0.5075 0.3034 23 0.990 0.000 C32 C26 C31 H32B 0.2387 0.5788 0.2747 23 0.990 0.000 C32 C26 C31 H33A -0.0531 0.8719 0.3291 93 0.950 0.001 C33 C31 C30 H33B -0.0270 0.7901 0.2710 93 0.950 0.000 C33 C31 C30 H34A 0.2978 1.0248 0.3094 137 0.980 0.000 C34 Si2 H34A H34B 0.4390 0.9700 0.3460 137 0.980 0.000 C34 Si2 H34A H34C 0.3615 1.1307 0.3522 137 0.980 0.000 C34 Si2 H34A H35A 0.0015 1.0794 0.3635 137 0.980 0.000 C35 Si2 H35A H35B 0.0482 1.1507 0.4186 137 0.980 0.000 C35 Si2 H35A H35C -0.0414 1.0006 0.4236 137 0.980 0.000 C35 Si2 H35A H36A 0.2912 1.0586 0.4814 137 0.980 0.000 C36 Si2 H36A H36B 0.4032 0.9212 0.4702 137 0.980 0.000 C36 Si2 H36A H36C 0.2430 0.8927 0.4994 137 0.980 0.000 C36 Si2 H36A H1 0.6221 0.6366 0.0380 43 0.880 0.000 N1 N2 S1 H3A 0.3542 0.6243 0.4634 43 0.880 0.000 N3 N4 S2 02SOT051 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.09546 0.21147 0.21324 1.00000 0.06367 0.05313 0.04186 -0.00144 0.01069 -0.01707 0.05286 0.01112 0.00076 0.00077 0.00024 0.00000 0.00436 0.00433 0.00316 0.00264 0.00277 0.00331 0.00164 H1A 0.00723 0.22311 0.18991 1.00000 0.07929 0.00000 0.00000 H1B 0.08333 0.27695 0.24355 1.00000 0.07929 0.00000 0.00000 H1C 0.10668 0.10816 0.22897 1.00000 0.07929 0.00000 0.00000 C2 0.23265 0.25179 0.17827 1.00000 0.04622 0.03079 0.04165 -0.00019 0.00724 -0.00848 0.03969 0.00974 0.00066 0.00063 0.00022 0.00000 0.00344 0.00339 0.00287 0.00216 0.00233 0.00258 0.00130 C3 0.36928 0.26913 0.20246 1.00000 0.06347 0.05563 0.03450 0.01079 -0.00517 -0.01258 0.05169 0.01082 0.00075 0.00075 0.00024 0.00000 0.00428 0.00436 0.00283 0.00254 0.00262 0.00330 0.00163 H3 0.37732 0.25272 0.24178 1.00000 0.06202 0.00000 0.00000 C4 0.49297 0.30971 0.17029 1.00000 0.04536 0.05646 0.04332 0.01493 -0.01119 -0.01032 0.04906 0.01054 0.00070 0.00073 0.00024 0.00000 0.00362 0.00428 0.00313 0.00265 0.00250 0.00298 0.00157 H4 0.58508 0.32258 0.18747 1.00000 0.05887 0.00000 0.00000 C5 0.48300 0.33181 0.11270 1.00000 0.03615 0.02635 0.03509 -0.00186 -0.00134 -0.00070 0.03258 0.00857 0.00059 0.00058 0.00020 0.00000 0.00291 0.00305 0.00252 0.00192 0.00199 0.00227 0.00114 C6 0.34766 0.31485 0.08773 1.00000 0.03332 0.02818 0.03592 -0.00420 -0.00140 -0.00801 0.03219 0.00819 0.00057 0.00058 0.00021 0.00000 0.00285 0.00310 0.00254 0.00194 0.00199 0.00224 0.00113 H6 0.33989 0.33208 0.04842 1.00000 0.03862 0.00000 0.00000 C7 0.22425 0.27277 0.12033 1.00000 0.03966 0.03602 0.03578 -0.00406 0.00236 -0.00907 0.03695 0.00913 0.00063 0.00062 0.00021 0.00000 0.00312 0.00339 0.00264 0.00208 0.00210 0.00248 0.00123 H7 0.13272 0.25798 0.10306 1.00000 0.04434 0.00000 0.00000 C8 0.45669 0.69337 0.13467 1.00000 0.03749 0.04414 0.04919 -0.01610 0.00801 -0.00763 0.04291 0.00975 0.00065 0.00069 0.00023 0.00000 0.00321 0.00386 0.00320 0.00250 0.00238 0.00270 0.00138 H8 0.38320 0.61900 0.12602 1.00000 0.05150 0.00000 0.00000 C9 0.44274 0.72670 0.19461 1.00000 0.09347 0.06438 0.04439 -0.01456 0.01776 -0.00308 0.06724 0.01296 0.00096 0.00089 0.00027 0.00000 0.00584 0.00515 0.00357 0.00310 0.00347 0.00432 0.00208 H9A 0.33734 0.75563 0.20333 1.00000 0.08068 0.00000 0.00000 H9B 0.46914 0.63544 0.21861 1.00000 0.08068 0.00000 0.00000 C10 0.53852 0.84559 0.20793 1.00000 0.07484 0.07677 0.04957 -0.01851 0.00787 0.00399 0.06669 0.01280 0.00087 0.00094 0.00029 0.00000 0.00524 0.00567 0.00373 0.00337 0.00335 0.00424 0.00205 H10A 0.54389 0.84705 0.24888 1.00000 0.08003 0.00000 0.00000 H10B 0.49601 0.94286 0.19254 1.00000 0.08003 0.00000 0.00000 C11 0.69242 0.81913 0.18318 1.00000 0.05734 0.03640 0.04368 -0.00559 0.00068 0.00251 0.04585 0.01048 0.00072 0.00070 0.00023 0.00000 0.00394 0.00360 0.00307 0.00233 0.00258 0.00290 0.00144 H11A 0.74352 0.73758 0.20634 1.00000 0.05502 0.00000 0.00000 H11B 0.74951 0.90958 0.18549 1.00000 0.05502 0.00000 0.00000 C12 0.69890 0.77917 0.12156 1.00000 0.03822 0.02486 0.03508 -0.00674 -0.00286 -0.00382 0.03237 0.00829 0.00060 0.00058 0.00020 0.00000 0.00299 0.00304 0.00254 0.00190 0.00202 0.00228 0.00114 C13 0.60469 0.89294 0.08636 1.00000 0.04758 0.03145 0.04029 -0.00864 -0.00913 0.00022 0.03934 0.00910 0.00067 0.00064 0.00022 0.00000 0.00343 0.00339 0.00284 0.00221 0.00231 0.00261 0.00129 C14 0.43960 0.83885 0.09497 1.00000 0.05455 0.07247 0.04808 -0.02003 -0.01252 0.02799 0.05815 0.01151 0.00076 0.00082 0.00026 0.00000 0.00407 0.00498 0.00343 0.00304 0.00284 0.00359 0.00188 H14A 0.37426 0.91402 0.11233 1.00000 0.06978 0.00000 0.00000 H14B 0.39730 0.81852 0.05902 1.00000 0.06978 0.00000 0.00000 C15 0.64242 1.00827 0.05586 1.00000 0.07159 0.05100 0.06208 -0.00417 -0.01109 0.01067 0.06179 0.01261 0.00090 0.00080 0.00028 0.00000 0.00496 0.00461 0.00416 0.00320 0.00342 0.00371 0.00188 H15A 0.74432 1.03375 0.05276 1.00000 0.07414 0.00000 0.00000 H15B 0.56864 1.06875 0.03623 1.00000 0.07414 0.00000 0.00000 C16 0.99150 0.59622 0.14228 1.00000 0.03926 0.04783 0.07981 -0.01145 -0.02039 -0.00146 0.05491 0.01047 0.00072 0.00076 0.00030 0.00000 0.00356 0.00429 0.00454 0.00314 0.00304 0.00298 0.00169 H16A 0.93981 0.50534 0.13707 1.00000 0.08237 0.00000 0.00000 H16B 0.98301 0.61681 0.18156 1.00000 0.08237 0.00000 0.00000 H16C 1.09725 0.58326 0.13138 1.00000 0.08237 0.00000 0.00000 C17 1.00176 0.92680 0.11222 1.00000 0.04815 0.05153 0.08933 -0.02224 -0.00445 -0.02044 0.06148 0.01043 0.00078 0.00082 0.00032 0.00000 0.00405 0.00480 0.00513 0.00354 0.00340 0.00331 0.00188 H17A 1.02611 0.92199 0.15176 1.00000 0.09221 0.00000 0.00000 H17B 0.93590 1.01417 0.10292 1.00000 0.09221 0.00000 0.00000 H17C 1.09399 0.93409 0.08936 1.00000 0.09221 0.00000 0.00000 C18 0.93225 0.72773 0.02288 1.00000 0.03683 0.07889 0.05292 -0.02054 0.01185 -0.02240 0.05503 0.01014 0.00069 0.00086 0.00025 0.00000 0.00344 0.00531 0.00353 0.00318 0.00261 0.00326 0.00176 H18A 1.03833 0.73586 0.01235 1.00000 0.08255 0.00000 0.00000 H18B 0.87318 0.80387 0.00076 1.00000 0.08255 0.00000 0.00000 H18C 0.89980 0.62916 0.01582 1.00000 0.08255 0.00000 0.00000 C19 0.73658 0.13223 0.28478 1.00000 0.05552 0.10557 0.06811 -0.02643 -0.00168 0.01041 0.07568 0.01335 0.00087 0.00104 0.00033 0.00000 0.00466 0.00710 0.00470 0.00437 0.00354 0.00445 0.00237 H19A 0.73397 0.03976 0.30914 1.00000 0.11353 0.00000 0.00000 H19B 0.83489 0.13938 0.26596 1.00000 0.11353 0.00000 0.00000 H19C 0.65910 0.13282 0.25688 1.00000 0.11353 0.00000 0.00000 C20 0.70881 0.26150 0.31891 1.00000 0.02076 0.08038 0.06091 -0.01180 -0.00585 0.00584 0.05381 0.01096 0.00063 0.00089 0.00027 0.00000 0.00290 0.00540 0.00388 0.00341 0.00246 0.00304 0.00172 C21 0.71332 0.40726 0.29613 1.00000 0.03553 0.10187 0.04474 -0.01293 -0.00280 -0.01001 0.06008 0.01113 0.00069 0.00098 0.00027 0.00000 0.00354 0.00648 0.00339 0.00357 0.00255 0.00362 0.00195 H21 0.74058 0.42611 0.25781 1.00000 0.07210 0.00000 0.00000 C22 0.67925 0.52699 0.32750 1.00000 0.03332 0.09135 0.03896 0.00693 -0.00831 -0.00712 0.05500 0.01088 0.00065 0.00090 0.00024 0.00000 0.00332 0.00558 0.00307 0.00309 0.00235 0.00325 0.00179 H22 0.68373 0.62634 0.31135 1.00000 0.06600 0.00000 0.00000 C23 0.63869 0.49617 0.38296 1.00000 0.02306 0.06945 0.04216 0.00206 -0.00618 0.00146 0.04528 0.01000 0.00060 0.00076 0.00023 0.00000 0.00278 0.00458 0.00294 0.00268 0.00210 0.00270 0.00149 C24 0.63575 0.35350 0.40718 1.00000 0.03550 0.07639 0.04650 0.00885 -0.00225 0.01343 0.05406 0.01192 0.00067 0.00082 0.00026 0.00000 0.00336 0.00506 0.00328 0.00305 0.00248 0.00322 0.00173 H24 0.61030 0.33523 0.44568 1.00000 0.06487 0.00000 0.00000 C25 0.67024 0.23587 0.37503 1.00000 0.03455 0.06988 0.06038 -0.00099 -0.00446 0.01498 0.05563 0.01189 0.00069 0.00085 0.00028 0.00000 0.00335 0.00495 0.00388 0.00323 0.00271 0.00319 0.00173 H25 0.66739 0.13685 0.39164 1.00000 0.06676 0.00000 0.00000 C26 0.26612 0.51384 0.36281 1.00000 0.05364 0.05178 0.12268 0.00382 -0.03348 -0.00781 0.07590 0.01293 0.00091 0.00092 0.00040 0.00000 0.00466 0.00521 0.00724 0.00436 0.00456 0.00378 0.00244 H26 0.35532 0.45398 0.35022 1.00000 0.09107 0.00000 0.00000 C27 0.18047 0.42176 0.39815 1.00000 0.08346 0.19398 0.11630 0.04585 -0.04948 -0.03391 0.13294 0.02171 0.00127 0.00178 0.00051 0.00000 0.00769 0.01458 0.00905 0.00925 0.00666 0.00864 0.00519 H27A 0.14295 0.34118 0.37772 1.00000 0.15952 0.00000 0.00000 H27B 0.24143 0.37634 0.42926 1.00000 0.15952 0.00000 0.00000 C28 0.06330 0.50438 0.41843 1.00000 0.19647 0.09505 0.06177 0.01633 0.03601 0.06801 0.12204 0.02446 0.00165 0.00116 0.00038 0.00000 0.01311 0.00786 0.00533 0.00475 0.00654 0.00840 0.00494 H28A 0.03220 0.45284 0.45462 1.00000 0.14645 0.00000 0.00000 H28B -0.02026 0.49799 0.39286 1.00000 0.14645 0.00000 0.00000 C29 0.07322 0.66248 0.42768 1.00000 0.03266 0.09328 0.05468 -0.00873 -0.01386 -0.00733 0.05967 0.01091 0.00071 0.00093 0.00027 0.00000 0.00337 0.00612 0.00376 0.00345 0.00265 0.00341 0.00191 H29A 0.10848 0.66969 0.46589 1.00000 0.07161 0.00000 0.00000 H29B -0.02824 0.71019 0.42547 1.00000 0.07161 0.00000 0.00000 C30 0.17889 0.75025 0.38568 1.00000 0.02691 0.08328 0.03784 -0.00683 -0.00770 0.01540 0.04962 0.01050 0.00063 0.00080 0.00023 0.00000 0.00291 0.00498 0.00284 0.00276 0.00214 0.00296 0.00163 C31 0.11473 0.73814 0.32673 1.00000 0.04607 0.19135 0.04468 -0.01444 -0.01774 0.05012 0.09502 0.01648 0.00087 0.00136 0.00030 0.00000 0.00431 0.01063 0.00383 0.00489 0.00312 0.00548 0.00350 C32 0.17394 0.57154 0.30880 1.00000 0.15766 0.17393 0.04477 -0.05088 0.02827 -0.10232 0.12090 0.01353 0.00129 0.00137 0.00032 0.00000 0.00996 0.01159 0.00425 0.00550 0.00509 0.00871 0.00473 H32A 0.08959 0.50752 0.30337 1.00000 0.14508 0.00000 0.00000 H32B 0.23865 0.57876 0.27469 1.00000 0.14508 0.00000 0.00000 C33 0.00309 0.80510 0.30748 1.00000 0.17987 0.18615 0.09979 0.02642 -0.01856 0.02887 0.15828 0.02763 0.00176 0.00180 0.00054 0.00000 0.01487 0.01540 0.00894 0.00896 0.00895 0.01164 0.00591 H33A -0.05311 0.87189 0.32911 1.00000 0.18993 0.00000 0.00000 H33B -0.02704 0.79009 0.27096 1.00000 0.18993 0.00000 0.00000 C34 0.34374 1.02753 0.34567 1.00000 0.08072 0.07182 0.06062 0.01233 0.01164 0.01265 0.07283 0.01567 0.00093 0.00094 0.00031 0.00000 0.00565 0.00549 0.00432 0.00358 0.00375 0.00436 0.00226 H34A 0.29785 1.02476 0.30936 1.00000 0.10925 0.00000 0.00000 H34B 0.43901 0.97001 0.34603 1.00000 0.10925 0.00000 0.00000 H34C 0.36152 1.13065 0.35219 1.00000 0.10925 0.00000 0.00000 C35 0.03436 1.05747 0.40185 1.00000 0.07534 0.11074 0.08777 -0.01485 -0.01859 0.04697 0.09204 0.01706 0.00100 0.00115 0.00038 0.00000 0.00597 0.00772 0.00599 0.00511 0.00462 0.00552 0.00303 H35A 0.00147 1.07936 0.36345 1.00000 0.13806 0.00000 0.00000 H35B 0.04817 1.15065 0.41862 1.00000 0.13806 0.00000 0.00000 H35C -0.04141 1.00060 0.42357 1.00000 0.13806 0.00000 0.00000 C36 0.29806 0.95580 0.47144 1.00000 0.04958 0.08061 0.05078 0.00026 -0.00899 0.01064 0.06090 0.01220 0.00078 0.00090 0.00027 0.00000 0.00403 0.00546 0.00362 0.00324 0.00288 0.00361 0.00188 H36A 0.29118 1.05864 0.48141 1.00000 0.09135 0.00000 0.00000 H36B 0.40322 0.92122 0.47018 1.00000 0.09135 0.00000 0.00000 H36C 0.24295 0.89267 0.49940 1.00000 0.09135 0.00000 0.00000 N1 0.62313 0.58026 0.06972 1.00000 0.03809 0.02713 0.03509 -0.00255 0.00754 -0.00653 0.03347 0.00711 0.00048 0.00048 0.00017 0.00000 0.00252 0.00261 0.00216 0.00166 0.00174 0.00195 0.00099 H1 0.62208 0.63658 0.03803 1.00000 0.04016 0.00000 0.00000 N2 0.61298 0.63948 0.12308 1.00000 0.03026 0.03417 0.03464 -0.00643 0.00096 -0.00040 0.03289 0.00703 0.00047 0.00050 0.00017 0.00000 0.00235 0.00274 0.00216 0.00171 0.00166 0.00193 0.00099 N3 0.39914 0.63726 0.43048 1.00000 0.02646 0.08429 0.03230 0.00347 -0.00581 0.00351 0.04824 0.00831 0.00050 0.00064 0.00018 0.00000 0.00247 0.00412 0.00231 0.00224 0.00177 0.00245 0.00134 H3A 0.35417 0.62433 0.46344 1.00000 0.05789 0.00000 0.00000 N4 0.31913 0.65395 0.38012 1.00000 0.03004 0.06094 0.03215 0.00051 -0.00580 0.00498 0.04140 0.00796 0.00050 0.00059 0.00017 0.00000 0.00246 0.00349 0.00221 0.00196 0.00172 0.00224 0.00117 O1 0.76864 0.34750 0.10151 1.00000 0.03299 0.03791 0.06699 -0.00993 -0.00824 0.00313 0.04564 0.00652 0.00043 0.00045 0.00017 0.00000 0.00218 0.00253 0.00264 0.00183 0.00179 0.00179 0.00100 O2 0.62083 0.36603 0.01594 1.00000 0.03841 0.02921 0.04224 -0.01015 0.00716 -0.00310 0.03633 0.00601 0.00041 0.00040 0.00014 0.00000 0.00214 0.00223 0.00197 0.00146 0.00152 0.00165 0.00086 O3 0.63191 0.61138 0.47892 1.00000 0.03349 0.07961 0.03829 0.00088 -0.00966 0.00366 0.05080 0.00694 0.00043 0.00053 0.00015 0.00000 0.00224 0.00332 0.00208 0.00192 0.00161 0.00207 0.00111 O4 0.61938 0.78120 0.39250 1.00000 0.03870 0.07159 0.05391 0.01042 -0.00862 -0.00420 0.05545 0.00748 0.00046 0.00054 0.00018 0.00000 0.00242 0.00334 0.00249 0.00211 0.00184 0.00216 0.00118 Si1 0.90468 0.75478 0.09812 1.00000 0.02870 0.03861 0.04343 -0.00825 -0.00306 -0.00543 0.03647 0.00243 0.00017 0.00018 0.00006 0.00000 0.00082 0.00099 0.00081 0.00061 0.00058 0.00065 0.00040 Si2 0.21595 0.94602 0.40169 1.00000 0.04699 0.07580 0.03781 0.00543 -0.00037 0.02291 0.05488 0.00353 0.00021 0.00023 0.00007 0.00000 0.00107 0.00140 0.00086 0.00078 0.00070 0.00095 0.00055 S1 0.63694 0.39732 0.07288 1.00000 0.02862 0.02792 0.04438 -0.00613 0.00113 -0.00211 0.03348 0.00218 0.00014 0.00015 0.00005 0.00000 0.00071 0.00081 0.00072 0.00050 0.00050 0.00055 0.00036 S2 0.58087 0.64380 0.42277 1.00000 0.02770 0.06981 0.03987 0.00545 -0.00678 0.00221 0.04639 0.00263 0.00016 0.00020 0.00006 0.00000 0.00075 0.00117 0.00074 0.00065 0.00053 0.00069 0.00044 Final Structure Factor Calculation for 02SOT051 in P-1 Total number of l.s. parameters = 442 Maximum vector length = 511 Memory required = 5778 / 25039 wR2 = 0.2550 before cycle 5 for 6515 data and 0 / 442 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.056 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0902 * P )^2 + 8.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0985 for 5161 Fo > 4sig(Fo) and 0.1175 for all 6515 data wR2 = 0.2550, GooF = S = 1.050, Restrained GooF = 1.049 for all data Occupancy sum of asymmetric unit = 48.00 for non-hydrogen and 56.00 for hydrogen atoms Principal mean square atomic displacements U 0.0753 0.0502 0.0330 C1 0.0532 0.0398 0.0261 C2 0.0743 0.0526 0.0281 C3 0.0764 0.0406 0.0301 C4 0.0363 0.0352 0.0263 C5 0.0378 0.0360 0.0228 C6 0.0461 0.0351 0.0297 C7 0.0624 0.0340 0.0324 C8 0.1009 0.0664 0.0344 C9 0.0834 0.0769 0.0397 C10 0.0587 0.0441 0.0348 C11 0.0391 0.0359 0.0221 C12 0.0533 0.0370 0.0278 C13 0.1011 0.0406 0.0328 C14 0.0811 0.0600 0.0442 C15 0.0872 0.0470 0.0306 C16 0.0943 0.0641 0.0259 C17 0.0932 0.0451 0.0268 C18 0.1150 0.0617 0.0503 C19 0.0830 0.0589 0.0196 C20 0.1027 0.0442 0.0334 C21 0.0958 0.0412 0.0281 C22 0.0719 0.0426 0.0213 C23 0.0883 0.0446 0.0293 C24 0.0786 0.0604 0.0278 C25 0.1366 0.0512 0.0399 C26 0.2438 0.1061 0.0489 C27 0.2553 0.0594 0.0514 C28 may be split into 0.0833 0.5152 0.4211 and 0.0433 0.4936 0.4158 0.0935 0.0601 0.0254 C29 0.0891 0.0391 0.0207 C30 0.2121 0.0506 0.0223 C31 may be split into 0.1205 0.7594 0.3267 and 0.1089 0.7169 0.3268 0.2666 0.0678 0.0283 C32 may be split into 0.1566 0.5896 0.3070 and 0.1913 0.5535 0.3106 0.2272 0.1665 0.0812 C33 0.1072 0.0626 0.0486 C34 0.1506 0.0855 0.0399 C35 0.0868 0.0570 0.0390 C36 0.0459 0.0307 0.0239 N1 0.0377 0.0324 0.0286 N2 0.0871 0.0349 0.0227 N3 0.0635 0.0360 0.0247 N4 0.0690 0.0378 0.0302 O1 0.0504 0.0334 0.0252 O2 0.0817 0.0447 0.0260 O3 0.0828 0.0483 0.0353 O4 0.0460 0.0376 0.0259 Si1 0.0946 0.0390 0.0310 Si2 0.0450 0.0286 0.0268 S1 0.0742 0.0407 0.0244 S2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.023 0.033 0.046 0.061 0.078 0.103 0.138 0.207 1.000 Number in group 690. 645. 628. 662. 656. 637. 643. 648. 650. 656. GooF 1.301 1.167 1.139 0.977 0.910 0.895 0.961 0.958 1.057 1.045 K 9.727 2.202 1.592 1.230 1.128 1.069 1.005 0.995 1.005 1.008 Resolution(A) 0.77 0.81 0.85 0.90 0.96 1.03 1.12 1.25 1.43 1.78 inf Number in group 654. 664. 644. 644. 652. 652. 659. 643. 646. 657. GooF 0.749 0.799 0.837 0.809 0.919 1.000 1.092 1.082 1.218 1.662 K 1.058 1.055 1.053 1.034 1.033 1.028 1.013 1.005 1.008 1.021 R1 0.246 0.218 0.179 0.156 0.134 0.116 0.102 0.083 0.085 0.089 Recommended weighting scheme: WGHT 0.0949 7.2205 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) 0 1 6 799.27 382.04 4.94 0.152 3.77 5 0 8 143.16 19.15 4.76 0.034 1.55 4 5 1 123.74 15.81 4.72 0.031 1.44 1 2 0 215.61 57.84 4.60 0.059 4.09 -5 0 8 142.04 13.98 4.55 0.029 1.52 3 -3 2 111.09 15.89 4.52 0.031 2.03 -1 -2 2 169.57 42.30 4.48 0.051 3.77 2 3 0 1133.03 589.76 4.45 0.189 2.54 -2 -6 5 11.33 150.74 4.42 0.096 1.35 -1 4 9 294.41 106.86 4.31 0.081 1.75 -2 0 3 160.13 429.06 4.29 0.161 3.86 0 -3 1 98.88 14.97 4.25 0.030 2.95 -4 2 17 74.89 0.08 4.25 0.002 1.15 -4 0 9 64.44 0.52 4.21 0.006 1.69 -1 9 0 56.62 0.26 4.19 0.004 0.99 4 4 19 70.66 0.35 4.08 0.005 1.04 2 -2 1 80.25 10.32 4.04 0.025 3.07 7 0 4 75.86 4.47 4.03 0.016 1.26 -1 -2 1 342.69 707.14 4.02 0.207 3.97 0 -3 15 66.07 2.51 4.01 0.012 1.36 1 1 5 760.99 1343.23 4.00 0.285 4.01 0 -2 2 3029.21 1974.62 3.96 0.346 4.10 1 3 5 87.98 14.18 3.96 0.029 2.58 3 2 4 91.68 15.71 3.95 0.031 2.40 1 3 9 93.11 16.77 3.85 0.032 2.05 5 3 11 54.33 1.42 3.81 0.009 1.31 1 4 7 44.55 0.55 3.78 0.006 1.94 6 4 6 46.99 1.55 3.70 0.010 1.23 1 -1 2 678.88 380.09 3.69 0.152 5.43 2 0 10 599.59 330.45 3.69 0.142 2.14 3 0 5 57.83 5.44 3.67 0.018 2.56 -2 8 3 94.48 17.53 3.66 0.033 1.08 -2 -6 9 50.90 2.77 3.66 0.013 1.22 1 -4 2 45.15 1.40 3.62 0.009 2.10 -2 6 11 63.14 6.90 3.60 0.020 1.22 6 5 10 60.02 0.95 3.59 0.008 1.09 2 5 6 41.61 0.79 3.59 0.007 1.61 -3 2 5 903.24 548.93 3.57 0.182 2.20 0 7 7 67.54 9.32 3.56 0.024 1.24 3 4 13 93.33 21.31 3.50 0.036 1.36 -2 -3 4 220.63 88.69 3.50 0.073 2.27 -1 5 0 55.81 6.20 3.49 0.019 1.75 -1 8 1 45.34 1.76 3.49 0.010 1.11 -2 1 9 93.14 21.64 3.49 0.036 2.22 -2 0 2 1752.18 2661.69 3.49 0.402 4.15 -1 -4 9 39.86 0.80 3.48 0.007 1.63 5 4 14 81.00 14.89 3.48 0.030 1.14 1 3 7 50.25 3.44 3.48 0.014 2.31 1 -2 1 1119.46 711.51 3.47 0.208 3.87 2 -3 1 262.23 119.60 3.46 0.085 2.42 Bond lengths and angles C1 - Distance Angles C2 1.5079 (0.0079) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - C2 H1A H1B C2 - Distance Angles C7 1.3954 (0.0071) C3 1.3916 (0.0085) 118.54 (0.52) C1 1.5079 (0.0079) 120.00 (0.54) 121.46 (0.51) C2 - C7 C3 C3 - Distance Angles C4 1.3768 (0.0085) C2 1.3916 (0.0085) 121.03 (0.52) H3 0.9500 119.48 119.49 C3 - C4 C2 C4 - Distance Angles C3 1.3768 (0.0085) C5 1.3887 (0.0071) 119.95 (0.56) H4 0.9500 120.03 120.02 C4 - C3 C5 C5 - Distance Angles C4 1.3887 (0.0071) C6 1.3893 (0.0071) 119.91 (0.51) S1 1.7501 (0.0054) 119.34 (0.43) 120.49 (0.38) C5 - C4 C6 C6 - Distance Angles C7 1.3835 (0.0072) C5 1.3893 (0.0071) 119.76 (0.47) H6 0.9500 120.12 120.12 C6 - C7 C5 C7 - Distance Angles C6 1.3835 (0.0072) C2 1.3954 (0.0071) 120.78 (0.52) H7 0.9500 119.61 119.61 C7 - C6 C2 C8 - Distance Angles N2 1.4887 (0.0070) C9 1.5004 (0.0078) 108.53 (0.52) C14 1.5630 (0.0091) 103.36 (0.45) 110.87 (0.53) H8 1.0000 111.26 111.26 111.26 C8 - N2 C9 C14 C9 - Distance Angles C10 1.4669 (0.0109) C8 1.5004 (0.0078) 113.14 (0.59) H9A 0.9900 108.94 108.95 H9B 0.9900 108.96 108.95 107.76 C9 - C10 C8 H9A C10 - Distance Angles C9 1.4669 (0.0109) C11 1.5029 (0.0092) 109.17 (0.59) H10A 0.9900 109.85 109.84 H10B 0.9900 109.85 109.84 108.28 C10 - C9 C11 H10A C11 - Distance Angles C10 1.5029 (0.0092) C12 1.5562 (0.0071) 115.73 (0.52) H11A 0.9900 108.34 108.34 H11B 0.9900 108.36 108.35 107.43 C11 - C10 C12 H11A C12 - Distance Angles N2 1.5050 (0.0070) C13 1.5189 (0.0073) 104.08 (0.41) C11 1.5562 (0.0071) 103.92 (0.42) 109.32 (0.43) Si1 1.9203 (0.0055) 114.01 (0.34) 116.06 (0.38) 108.69 (0.37) C12 - N2 C13 C11 C13 - Distance Angles C15 1.2747 (0.0090) C12 1.5189 (0.0073) 130.46 (0.61) C14 1.5794 (0.0095) 124.87 (0.59) 104.67 (0.48) C13 - C15 C12 C14 - Distance Angles C8 1.5630 (0.0091) C13 1.5794 (0.0095) 103.84 (0.46) H14A 0.9900 110.99 110.99 H14B 0.9900 110.99 110.99 108.99 C14 - C8 C13 H14A C15 - Distance Angles C13 1.2747 (0.0090) H15A 0.9500 120.00 H15B 0.9500 120.00 120.00 C15 - C13 H15A C16 - Distance Angles Si1 1.8662 (0.0067) H16A 0.9800 109.47 H16B 0.9800 109.48 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - Si1 H16A H16B C17 - Distance Angles Si1 1.8763 (0.0066) H17A 0.9800 109.47 H17B 0.9800 109.48 109.47 H17C 0.9800 109.47 109.47 109.47 C17 - Si1 H17A H17B C18 - Distance Angles Si1 1.8567 (0.0060) H18A 0.9800 109.48 H18B 0.9800 109.48 109.47 H18C 0.9800 109.46 109.47 109.47 C18 - Si1 H18A H18B C19 - Distance Angles C20 1.4951 (0.0104) H19A 0.9800 109.47 H19B 0.9800 109.47 109.47 H19C 0.9800 109.47 109.47 109.47 C19 - C20 H19A H19B C20 - Distance Angles C25 1.3866 (0.0089) C21 1.3856 (0.0105) 118.20 (0.65) C19 1.4951 (0.0104) 119.22 (0.73) 122.51 (0.66) C20 - C25 C21 C21 - Distance Angles C22 1.3919 (0.0103) C20 1.3856 (0.0104) 122.20 (0.63) H21 0.9500 118.90 118.90 C21 - C22 C20 C22 - Distance Angles C23 1.3811 (0.0077) C21 1.3919 (0.0103) 117.61 (0.69) H22 0.9500 121.20 121.19 C22 - C23 C21 C23 - Distance Angles C24 1.3706 (0.0091) C22 1.3811 (0.0078) 121.80 (0.65) S2 1.7620 (0.0068) 119.10 (0.47) 119.04 (0.54) C23 - C24 C22 C24 - Distance Angles C23 1.3706 (0.0091) C25 1.3886 (0.0098) 119.51 (0.60) H24 0.9500 120.24 120.25 C24 - C23 C25 C25 - Distance Angles C20 1.3866 (0.0089) C24 1.3886 (0.0098) 120.65 (0.68) H25 0.9500 119.68 119.67 C25 - C20 C24 C26 - Distance Angles C27 1.3781 (0.0133) N4 1.4704 (0.0094) 121.49 (1.02) C32 1.5984 (0.0128) 110.02 (0.70) 101.28 (0.60) H26 1.0000 107.76 107.76 107.78 C26 - C27 N4 C32 C27 - Distance Angles C28 1.3651 (0.0153) C26 1.3781 (0.0133) 108.34 (1.28) H27A 0.9900 110.04 110.02 H27B 0.9900 110.01 110.04 108.38 C27 - C28 C26 H27A C28 - Distance Angles C27 1.3651 (0.0154) C29 1.4737 (0.0130) 122.91 (1.32) H28A 0.9900 106.61 106.62 H28B 0.9900 106.59 106.59 106.56 C28 - C27 C29 H28A C29 - Distance Angles C28 1.4737 (0.0130) C30 1.5544 (0.0094) 114.49 (0.67) H29A 0.9900 108.63 108.64 H29B 0.9900 108.66 108.63 107.59 C29 - C28 C30 H29A C30 - Distance Angles N4 1.5069 (0.0073) C29 1.5544 (0.0094) 106.48 (0.53) C31 1.5617 (0.0086) 98.89 (0.48) 106.01 (0.59) Si2 1.8905 (0.0076) 113.41 (0.42) 115.96 (0.45) 114.41 (0.58) C30 - N4 C29 C31 C31 - Distance Angles C33 1.2283 (0.0142) C30 1.5617 (0.0086) 126.33 (1.02) C32 1.6645 (0.0156) 123.26 (1.12) 105.22 (0.64) C31 - C33 C30 C32 - Distance Angles C26 1.5984 (0.0128) C31 1.6645 (0.0156) 99.91 (0.55) H32A 0.9900 111.78 111.80 H32B 0.9900 111.79 111.79 109.53 C32 - C26 C31 H32A C33 - Distance Angles C31 1.2283 (0.0142) H33A 0.9500 120.02 H33B 0.9500 119.98 120.00 C33 - C31 H33A C34 - Distance Angles Si2 1.8652 (0.0074) H34A 0.9800 109.48 H34B 0.9800 109.47 109.47 H34C 0.9800 109.46 109.47 109.47 C34 - Si2 H34A H34B C35 - Distance Angles Si2 1.8766 (0.0077) H35A 0.9800 109.47 H35B 0.9800 109.47 109.47 H35C 0.9800 109.48 109.47 109.47 C35 - Si2 H35A H35B C36 - Distance Angles Si2 1.8644 (0.0065) H36A 0.9800 109.47 H36B 0.9800 109.47 109.47 H36C 0.9800 109.47 109.47 109.47 C36 - Si2 H36A H36B N1 - Distance Angles N2 1.4333 (0.0056) S1 1.6500 (0.0045) 114.16 (0.32) H1 0.8800 122.92 122.92 N1 - N2 S1 N2 - Distance Angles N1 1.4333 (0.0056) C8 1.4887 (0.0070) 109.86 (0.38) C12 1.5050 (0.0070) 110.13 (0.37) 102.73 (0.41) N2 - N1 C8 N3 - Distance Angles N4 1.4205 (0.0056) S2 1.6355 (0.0048) 115.17 (0.35) H3A 0.8800 122.41 122.42 N3 - N4 S2 N4 - Distance Angles N3 1.4205 (0.0056) C26 1.4704 (0.0094) 113.85 (0.50) C30 1.5069 (0.0073) 111.59 (0.42) 104.27 (0.51) N4 - N3 C26 O1 - Distance Angles S1 1.4210 (0.0039) O1 - O2 - Distance Angles S1 1.4365 (0.0037) O2 - O3 - Distance Angles S2 1.4421 (0.0038) O3 - O4 - Distance Angles S2 1.4353 (0.0047) O4 - Si1 - Distance Angles C18 1.8567 (0.0060) C16 1.8662 (0.0067) 110.93 (0.34) C17 1.8763 (0.0066) 107.92 (0.33) 107.63 (0.32) C12 1.9203 (0.0055) 114.02 (0.25) 108.29 (0.28) 107.83 (0.29) Si1 - C18 C16 C17 Si2 - Distance Angles C36 1.8644 (0.0066) C34 1.8652 (0.0074) 110.28 (0.38) C35 1.8766 (0.0077) 106.78 (0.36) 109.63 (0.42) C30 1.8905 (0.0076) 113.27 (0.31) 107.86 (0.34) 108.99 (0.40) Si2 - C36 C34 C35 S1 - Distance Angles O1 1.4210 (0.0039) O2 1.4365 (0.0037) 119.80 (0.24) N1 1.6500 (0.0045) 108.96 (0.24) 103.30 (0.22) C5 1.7501 (0.0054) 108.01 (0.25) 109.21 (0.24) 106.85 (0.23) S1 - O1 O2 N1 S2 - Distance Angles O4 1.4353 (0.0047) O3 1.4421 (0.0038) 119.01 (0.28) N3 1.6355 (0.0048) 109.82 (0.27) 103.04 (0.24) C23 1.7620 (0.0068) 108.83 (0.29) 108.94 (0.27) 106.45 (0.29) S2 - O4 O3 N3 FMAP and GRID set by program FMAP 2 1 41 GRID -2.632 -2 -1 2.632 2 1 R1 = 0.1168 for 6515 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.85 at 0.9632 0.7365 0.4518 [ 0.70 A from H29B ] Deepest hole -0.50 at 0.2228 0.3618 0.3809 [ 0.75 A from H27A ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 5562 / 53511 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0368 0.7365 0.4518 1.00000 0.05 1.85 0.70 H29B 1.32 C29 1.45 H29A 2.43 H35C Q2 1 0.0552 0.6389 0.3053 1.00000 0.05 1.11 1.20 C32 1.22 H32A 1.22 C31 1.56 C33 Q3 1 0.4676 0.9532 0.0953 1.00000 0.05 0.70 0.99 H14A 1.08 C14 1.34 C13 1.71 H14B Q4 1 0.7413 0.8947 0.2087 1.00000 0.05 0.65 0.57 H11B 1.07 C11 1.43 H11A 1.89 C10 Q5 1 0.2054 0.5874 0.3035 1.00000 0.05 0.58 0.34 C32 0.76 H32B 1.29 H32A 1.62 C26 Q6 1 0.1906 0.4798 0.3221 1.00000 0.05 0.55 0.87 C32 1.03 H32A 1.27 C26 1.45 H32B Q7 1 0.3605 0.7839 0.1104 1.00000 0.05 0.52 0.93 C14 1.19 H14A 1.28 C8 1.29 H14B Q8 1 0.6339 0.8856 0.0574 1.00000 0.05 0.39 0.75 C13 1.11 C15 1.69 H15A 1.77 H15B Q9 1 0.5272 0.6000 0.0468 1.00000 0.05 0.38 0.94 H1 1.04 N1 2.03 O2 2.08 N2 Q10 1 0.1387 0.8250 0.3187 1.00000 0.05 0.35 0.83 C31 1.28 C33 1.74 C30 1.77 H33A Shortest distances between peaks (including symmetry equivalents) 5 6 1.05 2 5 1.41 3 8 1.83 3 7 1.85 2 6 1.87 2 10 1.93 5 10 2.26 7 9 2.73 8 9 2.83 7 8 2.88 Time profile in seconds ----------------------- 0.22: 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. 2.05: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 4.11: Structure factors and derivatives 8.98: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 1.30: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.28: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 02sot051 finished at 13:29:18 Total CPU time: 17.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++