+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0238 started at 13:49:02 on 12-Mar-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0238 in P2(1)2(1)2(1) CELL 0.71073 7.2319 11.0720 18.1646 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0003 0.0005 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O SI UNIT 52 84 4 8 4 V = 1454.47 F(000) = 544.0 Mu = 0.15 mm-1 Cell Wt = 1005.59 Rho = 1.148 MERG 2 OMIT -3.00 55.00 EXTI 0.21166 SHEL 7 0.77 ACTA FMAP 2 PLAN 10 SIZE 0.34 0.40 0.40 BOND $H WGHT 0.06880 0.03650 L.S. 20 TEMP -153.00 FVAR 1.07954 C1 1 0.072489 0.155426 0.096567 11.00000 0.03724 0.04443 = 0.02528 -0.00742 -0.00482 -0.00327 AFIX 137 H1A 2 0.074155 0.074727 0.118719 11.00000 -1.50000 H1B 2 0.079759 0.148181 0.042875 11.00000 -1.50000 H1C 2 -0.042408 0.196772 0.110098 11.00000 -1.50000 AFIX 0 C2 1 0.272578 0.398240 0.090758 11.00000 0.04119 0.02930 = 0.02672 0.00347 0.00820 0.00633 AFIX 137 H2A 2 0.154103 0.437393 0.101543 11.00000 -1.50000 H2B 2 0.289512 0.393021 0.037324 11.00000 -1.50000 H2C 2 0.373378 0.445733 0.112256 11.00000 -1.50000 AFIX 0 C3 1 0.498851 0.171147 0.106217 11.00000 0.03340 0.03884 = 0.03418 0.00500 0.01415 0.01045 AFIX 137 H3A 2 0.600987 0.218605 0.126720 11.00000 -1.50000 H3B 2 0.510933 0.167457 0.052528 11.00000 -1.50000 H3C 2 0.502501 0.089171 0.126512 11.00000 -1.50000 AFIX 0 C4 1 0.115321 0.222855 0.268040 11.00000 0.01638 0.01994 = 0.01730 -0.00065 0.00209 -0.00161 AFIX 13 H4 2 0.060292 0.142801 0.255014 11.00000 -1.20000 AFIX 0 C5 1 -0.030761 0.322493 0.259562 11.00000 0.01842 0.02153 = 0.02024 0.00213 0.00027 -0.00195 C6 1 -0.341144 0.393883 0.282438 11.00000 0.01913 0.02516 = 0.05958 -0.00171 0.00378 0.00101 AFIX 137 H6A 2 -0.289523 0.465880 0.258722 11.00000 -1.50000 H6B 2 -0.371915 0.412506 0.333738 11.00000 -1.50000 H6C 2 -0.453193 0.368686 0.256270 11.00000 -1.50000 AFIX 0 C7 1 -0.270355 0.180346 0.308731 11.00000 0.02186 0.02391 = 0.03440 0.00243 0.00404 -0.00500 AFIX 137 H7A 2 -0.184854 0.116507 0.293311 11.00000 -1.50000 H7B 2 -0.393997 0.163262 0.289261 11.00000 -1.50000 H7C 2 -0.275357 0.183364 0.362614 11.00000 -1.50000 AFIX 0 C8 1 0.184785 0.220516 0.347366 11.00000 0.01464 0.02770 = 0.01746 -0.00166 0.00246 0.00110 C9 1 0.241798 0.326811 0.381686 11.00000 0.02000 0.03163 = 0.02845 -0.00705 0.00340 -0.00310 AFIX 43 H9 2 0.229502 0.401881 0.356836 11.00000 -1.20000 AFIX 0 C10 1 0.316298 0.323306 0.451886 11.00000 0.02357 0.05211 = 0.02910 -0.01555 -0.00021 -0.00348 AFIX 43 H10 2 0.356110 0.395859 0.474869 11.00000 -1.20000 AFIX 0 C11 1 0.332853 0.214550 0.488565 11.00000 0.02597 0.07432 = 0.02089 -0.00683 -0.00485 0.00782 AFIX 43 H11 2 0.385634 0.212220 0.536436 11.00000 -1.20000 AFIX 0 C12 1 0.272686 0.109223 0.455652 11.00000 0.03751 0.04919 = 0.02654 0.00928 -0.00161 0.01312 AFIX 43 H12 2 0.281436 0.034791 0.481434 11.00000 -1.20000 AFIX 0 C13 1 0.199188 0.111719 0.384764 11.00000 0.02856 0.02808 = 0.02404 0.00125 -0.00024 0.00329 AFIX 43 H13 2 0.159000 0.039000 0.362081 11.00000 -1.20000 AFIX 0 N1 3 -0.205849 0.296825 0.280335 11.00000 0.01636 0.01956 = 0.02949 0.00220 0.00150 -0.00066 O1 4 0.270700 0.246817 0.221913 11.00000 0.01693 0.02852 = 0.01731 0.00015 0.00305 -0.00149 O2 4 0.013728 0.422262 0.236071 11.00000 0.02471 0.02118 = 0.04704 0.01058 0.00590 -0.00122 SI1 5 0.273980 0.244039 0.130811 11.00000 0.02220 0.02289 = 0.01754 -0.00042 0.00309 0.00241 HKLF 4 Covalent radii and connectivity table for 2007src0238 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 C1 - Si1 C2 - Si1 C3 - Si1 C4 - O1 C8 C5 C5 - O2 N1 C4 C6 - N1 C7 - N1 C8 - C13 C9 C4 C9 - C10 C8 C10 - C11 C9 C11 - C12 C10 C12 - C11 C13 C13 - C8 C12 N1 - C5 C6 C7 O1 - C4 Si1 O2 - C5 Si1 - O1 C2 C1 C3 17431 Reflections read, of which 68 rejected -9 =< h =< 8, -14 =< k =< 14, -23 =< l =< 23, Max. 2-theta = 54.93 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 0 1 300.10 24.84 2 231.38 2 0 3 4538.46 51.89 4 886.82 6 0 13 96.28 3.33 4 20.14 3 Inconsistent equivalents 3314 Unique reflections, of which 0 suppressed R(int) = 0.0369 R(sigma) = 0.0292 Friedel opposites not merged Maximum memory for data reduction = 1976 / 33134 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 = 2466 / 200737 wR2 = 0.1123 before cycle 1 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07954 0.00328 -0.002 OSF 2 0.21165 0.01124 -0.001 EXTI Mean shift/esd = 0.003 Maximum = -0.021 for U12 Si1 Max. shift = 0.000 A for H6C Max. dU = 0.000 for N1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 2 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07954 0.00328 0.000 OSF 2 0.21166 0.01124 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.007 for U12 Si1 Max. shift = 0.000 A for H6C Max. dU = 0.000 for N1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 3 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07954 0.00328 0.000 OSF 2 0.21166 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for U22 Si1 Max. shift = 0.000 A for H6C Max. dU = 0.000 for C6 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 4 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07953 0.00328 0.000 OSF 2 0.21166 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H6C Max. dU = 0.000 for C13 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 5 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07954 0.00328 0.000 OSF 2 0.21166 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1C Max. dU = 0.000 for C11 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 6 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07954 0.00328 0.000 OSF 2 0.21166 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z Si1 Max. shift = 0.000 A for H6B Max. dU = 0.000 for C13 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 7 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07954 0.00328 0.000 OSF 2 0.21166 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z Si1 Max. shift = 0.000 A for H6C Max. dU = 0.000 for C11 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 8 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07954 0.00328 0.000 OSF 2 0.21166 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z Si1 Max. shift = 0.000 A for H2C Max. dU = 0.000 for C7 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 9 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07953 0.00328 0.000 OSF 2 0.21166 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z Si1 Max. shift = 0.000 A for H3C Max. dU = 0.000 for C4 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 10 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07953 0.00328 0.000 OSF 2 0.21165 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H2C Max. dU = 0.000 for C12 Least-squares cycle 11 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 11 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07953 0.00328 0.000 OSF 2 0.21165 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z Si1 Max. shift = 0.000 A for H3A Max. dU = 0.000 for C3 Least-squares cycle 12 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 12 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07953 0.00328 0.000 OSF 2 0.21166 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C12 Max. dU = 0.000 for C2 Least-squares cycle 13 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 13 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07953 0.00328 0.000 OSF 2 0.21166 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z Si1 Max. shift = 0.000 A for H3A Max. dU = 0.000 for C12 Least-squares cycle 14 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 14 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07953 0.00328 0.000 OSF 2 0.21166 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z Si1 Max. shift = 0.000 A for H3A Max. dU = 0.000 for O2 Least-squares cycle 15 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 15 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07953 0.00328 0.000 OSF 2 0.21166 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z Si1 Max. shift = 0.000 A for H2C Max. dU = 0.000 for C5 Least-squares cycle 16 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 16 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07953 0.00328 0.000 OSF 2 0.21165 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1A Max. dU = 0.000 for C11 Least-squares cycle 17 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 17 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07954 0.00328 0.000 OSF 2 0.21166 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H6C Max. dU = 0.000 for C11 Least-squares cycle 18 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 18 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07953 0.00328 0.000 OSF 2 0.21166 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z Si1 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C5 Least-squares cycle 19 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 19 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07953 0.00328 0.000 OSF 2 0.21165 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z Si1 Max. shift = 0.000 A for H6C Max. dU = 0.000 for C8 Least-squares cycle 20 Maximum vector length = 511 Memory required = 2466 / 200737 wR2 = 0.1123 before cycle 20 for 3314 data and 160 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.07954 0.00328 0.000 OSF 2 0.21166 0.01124 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z Si1 Max. shift = 0.000 A for H7A Max. dU = 0.000 for C11 Largest correlation matrix elements 0.658 EXTI / OSF 0.561 U33 Si1 / OSF 0.565 U11 Si1 / OSF 0.542 U22 Si1 / OSF Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.0742 0.0747 0.1187 137 0.980 0.000 C1 Si1 H1A H1B 0.0798 0.1482 0.0429 137 0.980 0.000 C1 Si1 H1A H1C -0.0424 0.1968 0.1101 137 0.980 0.000 C1 Si1 H1A H2A 0.1541 0.4374 0.1015 137 0.980 0.000 C2 Si1 H2A H2B 0.2895 0.3930 0.0373 137 0.980 0.000 C2 Si1 H2A H2C 0.3734 0.4457 0.1123 137 0.980 0.000 C2 Si1 H2A H3A 0.6010 0.2186 0.1267 137 0.980 0.000 C3 Si1 H3A H3B 0.5109 0.1675 0.0525 137 0.980 0.000 C3 Si1 H3A H3C 0.5025 0.0892 0.1265 137 0.980 0.000 C3 Si1 H3A H4 0.0603 0.1428 0.2550 13 1.000 0.000 C4 O1 C8 C5 H6A -0.2895 0.4659 0.2587 137 0.980 0.000 C6 N1 H6A H6B -0.3719 0.4125 0.3337 137 0.980 0.000 C6 N1 H6A H6C -0.4532 0.3687 0.2563 137 0.980 0.000 C6 N1 H6A H7A -0.1849 0.1165 0.2933 137 0.980 0.000 C7 N1 H7A H7B -0.3940 0.1633 0.2893 137 0.980 0.000 C7 N1 H7A H7C -0.2754 0.1834 0.3626 137 0.980 0.000 C7 N1 H7A H9 0.2295 0.4019 0.3568 43 0.950 0.000 C9 C10 C8 H10 0.3561 0.3959 0.4749 43 0.950 0.000 C10 C11 C9 H11 0.3856 0.2122 0.5364 43 0.950 0.000 C11 C12 C10 H12 0.2814 0.0348 0.4814 43 0.950 0.000 C12 C11 C13 H13 0.1590 0.0390 0.3621 43 0.950 0.000 C13 C8 C12 2007src0238 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.07249 0.15543 0.09657 1.00000 0.03724 0.04443 0.02528 -0.00742 -0.00482 -0.00327 0.03565 0.00336 0.00030 0.00020 0.00011 0.00000 0.00105 0.00112 0.00088 0.00080 0.00076 0.00085 0.00045 H1A 0.07416 0.07473 0.11872 1.00000 0.05347 0.00000 0.00000 H1B 0.07976 0.14818 0.04287 1.00000 0.05347 0.00000 0.00000 H1C -0.04241 0.19677 0.11010 1.00000 0.05347 0.00000 0.00000 C2 0.27258 0.39824 0.09076 1.00000 0.04119 0.02930 0.02672 0.00347 0.00820 0.00633 0.03240 0.00352 0.00029 0.00016 0.00009 0.00000 0.00106 0.00087 0.00083 0.00066 0.00075 0.00083 0.00041 H2A 0.15410 0.43739 0.10154 1.00000 0.04860 0.00000 0.00000 H2B 0.28951 0.39302 0.03732 1.00000 0.04860 0.00000 0.00000 H2C 0.37338 0.44573 0.11226 1.00000 0.04860 0.00000 0.00000 C3 0.49885 0.17115 0.10622 1.00000 0.03340 0.03884 0.03418 0.00500 0.01415 0.01045 0.03547 0.00401 0.00029 0.00018 0.00011 0.00000 0.00099 0.00103 0.00098 0.00081 0.00087 0.00083 0.00044 H3A 0.60099 0.21861 0.12672 1.00000 0.05321 0.00000 0.00000 H3B 0.51093 0.16746 0.05253 1.00000 0.05321 0.00000 0.00000 H3C 0.50250 0.08917 0.12651 1.00000 0.05321 0.00000 0.00000 C4 0.11532 0.22286 0.26804 1.00000 0.01638 0.01994 0.01730 -0.00065 0.00209 -0.00161 0.01787 0.00253 0.00021 0.00013 0.00008 0.00000 0.00069 0.00076 0.00067 0.00056 0.00053 0.00055 0.00032 H4 0.06029 0.14280 0.25501 1.00000 0.02145 0.00000 0.00000 C5 -0.03076 0.32249 0.25956 1.00000 0.01842 0.02153 0.02024 0.00213 0.00027 -0.00195 0.02006 0.00267 0.00021 0.00014 0.00009 0.00000 0.00077 0.00077 0.00076 0.00060 0.00058 0.00061 0.00034 C6 -0.34114 0.39388 0.28244 1.00000 0.01913 0.02516 0.05958 -0.00171 0.00378 0.00101 0.03462 0.00353 0.00025 0.00016 0.00012 0.00000 0.00081 0.00089 0.00125 0.00086 0.00081 0.00069 0.00044 H6A -0.28952 0.46588 0.25872 1.00000 0.05193 0.00000 0.00000 H6B -0.37192 0.41251 0.33374 1.00000 0.05193 0.00000 0.00000 H6C -0.45319 0.36869 0.25627 1.00000 0.05193 0.00000 0.00000 C7 -0.27035 0.18035 0.30873 1.00000 0.02186 0.02391 0.03440 0.00243 0.00404 -0.00500 0.02672 0.00306 0.00024 0.00015 0.00010 0.00000 0.00081 0.00078 0.00086 0.00063 0.00069 0.00068 0.00037 H7A -0.18485 0.11651 0.29331 1.00000 0.04008 0.00000 0.00000 H7B -0.39400 0.16326 0.28926 1.00000 0.04008 0.00000 0.00000 H7C -0.27536 0.18336 0.36261 1.00000 0.04008 0.00000 0.00000 C8 0.18478 0.22052 0.34737 1.00000 0.01464 0.02770 0.01746 -0.00166 0.00246 0.00110 0.01993 0.00268 0.00020 0.00015 0.00008 0.00000 0.00065 0.00079 0.00066 0.00060 0.00054 0.00055 0.00033 C9 0.24180 0.32681 0.38169 1.00000 0.02000 0.03163 0.02845 -0.00705 0.00340 -0.00310 0.02669 0.00289 0.00024 0.00015 0.00009 0.00000 0.00079 0.00084 0.00083 0.00066 0.00067 0.00064 0.00037 H9 0.22950 0.40188 0.35684 1.00000 0.03203 0.00000 0.00000 C10 0.31630 0.32331 0.45189 1.00000 0.02357 0.05211 0.02910 -0.01555 -0.00021 -0.00348 0.03493 0.00319 0.00025 0.00020 0.00011 0.00000 0.00087 0.00119 0.00091 0.00084 0.00074 0.00078 0.00045 H10 0.35611 0.39586 0.47487 1.00000 0.04191 0.00000 0.00000 C11 0.33285 0.21455 0.48856 1.00000 0.02597 0.07432 0.02089 -0.00683 -0.00485 0.00782 0.04039 0.00353 0.00028 0.00022 0.00010 0.00000 0.00089 0.00154 0.00080 0.00094 0.00069 0.00092 0.00053 H11 0.38563 0.21222 0.53644 1.00000 0.04847 0.00000 0.00000 C12 0.27269 0.10922 0.45565 1.00000 0.03751 0.04919 0.02654 0.00928 -0.00161 0.01312 0.03775 0.00378 0.00029 0.00020 0.00010 0.00000 0.00102 0.00110 0.00087 0.00082 0.00080 0.00091 0.00045 H12 0.28144 0.03479 0.48143 1.00000 0.04530 0.00000 0.00000 C13 0.19919 0.11172 0.38476 1.00000 0.02856 0.02808 0.02404 0.00125 -0.00024 0.00329 0.02689 0.00310 0.00025 0.00016 0.00009 0.00000 0.00087 0.00082 0.00078 0.00065 0.00064 0.00067 0.00036 H13 0.15900 0.03900 0.36208 1.00000 0.03227 0.00000 0.00000 N1 -0.20585 0.29683 0.28033 1.00000 0.01636 0.01956 0.02949 0.00220 0.00150 -0.00066 0.02181 0.00234 0.00018 0.00012 0.00008 0.00000 0.00064 0.00061 0.00069 0.00055 0.00052 0.00051 0.00030 O1 0.27070 0.24682 0.22191 1.00000 0.01693 0.02852 0.01731 0.00015 0.00305 -0.00149 0.02092 0.00179 0.00014 0.00010 0.00006 0.00000 0.00051 0.00055 0.00049 0.00043 0.00036 0.00052 0.00024 O2 0.01373 0.42226 0.23607 1.00000 0.02471 0.02118 0.04704 0.01058 0.00590 -0.00122 0.03098 0.00238 0.00018 0.00011 0.00007 0.00000 0.00062 0.00059 0.00076 0.00051 0.00058 0.00049 0.00031 Si1 0.27398 0.24404 0.13081 1.00000 0.02220 0.02289 0.01754 -0.00042 0.00309 0.00241 0.02088 0.00072 0.00006 0.00004 0.00002 0.00000 0.00024 0.00024 0.00023 0.00016 0.00014 0.00017 0.00015 Final Structure Factor Calculation for 2007src0238 in P2(1)2(1)2(1) Total number of l.s. parameters = 160 Maximum vector length = 511 Memory required = 2308 / 26068 wR2 = 0.1123 before cycle 21 for 3314 data and 2 / 160 parameters GooF = S = 1.261; Restrained GooF = 1.261 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0688 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0457 for 3142 Fo > 4sig(Fo) and 0.0492 for all 3314 data wR2 = 0.1123, GooF = S = 1.261, Restrained GooF = 1.261 for all data Flack x parameter = 0.0578 with esd 0.1195 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 = 17.00 for non-hydrogen and 21.00 for hydrogen atoms Principal mean square atomic displacements U 0.0472 0.0389 0.0208 C1 0.0477 0.0266 0.0229 C2 0.0553 0.0325 0.0186 C3 0.0211 0.0179 0.0146 C4 0.0235 0.0197 0.0170 C5 0.0600 0.0253 0.0186 C6 0.0357 0.0279 0.0166 C7 0.0280 0.0188 0.0130 C8 0.0384 0.0229 0.0188 C9 0.0602 0.0243 0.0203 C10 0.0766 0.0267 0.0179 C11 0.0592 0.0336 0.0205 C12 0.0317 0.0257 0.0233 C13 0.0301 0.0194 0.0159 N1 0.0287 0.0201 0.0140 O1 0.0518 0.0250 0.0161 O2 0.0254 0.0215 0.0157 Si1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.027 0.035 0.043 0.051 0.061 0.075 0.094 0.123 1.000 Number in group 332. 360. 329. 318. 323. 329. 345. 321. 325. 332. GooF 1.327 1.258 1.127 1.112 0.988 1.021 0.803 0.888 0.827 2.421 K 0.987 0.961 0.983 1.003 0.993 0.995 1.008 1.009 1.010 0.975 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.31 1.64 inf Number in group 337. 327. 331. 350. 311. 336. 329. 328. 332. 333. GooF 0.981 0.936 0.911 0.912 0.873 0.914 0.971 1.018 1.361 2.633 K 1.015 1.019 1.020 1.017 1.025 1.011 1.011 1.019 1.021 0.947 R1 0.065 0.055 0.042 0.040 0.029 0.028 0.025 0.025 0.032 0.099 Recommended weighting scheme: WGHT 0.0688 0.0365 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 0 0 1578.51 18095.59 15.34 0.731 3.62 -1 1 3 924.82 10677.32 15.12 0.561 4.28 0 2 0 3979.00 33870.88 13.99 1.000 5.54 2 2 0 3319.71 7676.70 7.18 0.476 3.03 0 0 8 15001.41 9038.98 6.12 0.517 2.27 0 0 6 10794.50 6485.56 6.08 0.438 3.03 0 2 3 8299.32 5114.00 5.85 0.389 4.09 1 0 4 9207.33 5860.63 5.21 0.416 3.85 1 0 8 7929.59 5252.48 5.04 0.394 2.17 1 0 1 434.22 2562.56 4.83 0.275 6.72 3 0 6 74.89 47.44 4.57 0.037 1.89 1 5 6 4.07 9.64 4.36 0.017 1.74 0 1 11 11.54 3.97 4.22 0.011 1.63 0 1 8 36.79 23.73 4.04 0.026 2.22 -1 5 6 4.10 9.24 4.02 0.017 1.74 4 3 4 -0.46 2.15 3.97 0.008 1.53 0 1 7 189.01 271.43 3.87 0.090 2.53 0 7 5 30.77 20.19 3.85 0.024 1.45 -2 2 3 5053.12 3704.37 3.78 0.331 2.71 0 2 9 61.69 89.87 3.75 0.052 1.90 2 7 0 25.45 16.74 3.59 0.022 1.45 0 2 16 46.32 30.80 3.57 0.030 1.11 2 2 3 4963.06 3691.35 3.55 0.330 2.71 5 0 7 16.95 8.94 3.54 0.016 1.26 0 7 4 14.84 22.62 3.41 0.026 1.49 4 0 0 9497.46 6923.09 3.34 0.452 1.81 0 3 1 90.85 123.73 3.29 0.060 3.62 3 6 3 16.02 23.36 3.21 0.026 1.42 4 8 0 11.39 6.05 3.16 0.013 1.10 -3 6 3 16.60 24.33 3.16 0.027 1.42 2 0 15 20.87 12.23 3.11 0.019 1.15 5 7 0 81.14 60.14 3.08 0.042 1.07 -3 4 6 56.42 76.65 3.07 0.048 1.56 0 4 7 152.61 202.70 3.04 0.077 1.89 3 4 6 57.23 76.99 2.99 0.048 1.56 0 5 7 2.17 5.12 2.92 0.012 1.68 1 12 8 -0.98 8.23 2.88 0.016 0.85 -2 1 2 3528.86 2774.27 2.88 0.286 3.21 2 1 2 3530.53 2774.68 2.88 0.286 3.21 5 3 0 14.80 10.43 2.87 0.018 1.35 -4 3 4 0.49 2.15 2.80 0.008 1.53 1 1 9 4390.27 3482.30 2.77 0.321 1.91 3 2 16 16.65 24.60 2.70 0.027 1.01 3 0 5 2657.32 2121.61 2.69 0.250 2.01 5 0 1 61.10 79.45 2.68 0.048 1.44 -1 1 9 4358.74 3488.92 2.67 0.321 1.91 3 2 13 35.80 49.75 2.67 0.038 1.18 0 2 5 3211.36 2570.44 2.66 0.275 3.04 3 0 4 2688.08 2152.56 2.65 0.252 2.13 4 0 20 73.02 52.48 2.65 0.039 0.81 Bond lengths and angles C1 - Distance Angles Si1 1.8636 (0.0020) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - Si1 H1A H1B C2 - Distance Angles Si1 1.8559 (0.0018) H2A 0.9800 109.47 H2B 0.9800 109.47 109.47 H2C 0.9800 109.47 109.47 109.47 C2 - Si1 H2A H2B C3 - Distance Angles Si1 1.8697 (0.0019) H3A 0.9800 109.47 H3B 0.9800 109.47 109.47 H3C 0.9800 109.47 109.47 109.47 C3 - Si1 H3A H3B C4 - Distance Angles O1 1.4266 (0.0017) C8 1.5262 (0.0020) 107.36 (0.12) C5 1.5352 (0.0021) 110.46 (0.11) 109.48 (0.12) H4 1.0000 109.84 109.84 109.84 C4 - O1 C8 C5 C5 - Distance Angles O2 1.2271 (0.0020) N1 1.3515 (0.0021) 122.14 (0.15) C4 1.5352 (0.0021) 120.09 (0.14) 117.75 (0.13) C5 - O2 N1 C6 - Distance Angles N1 1.4538 (0.0022) H6A 0.9800 109.47 H6B 0.9800 109.47 109.47 H6C 0.9800 109.47 109.47 109.47 C6 - N1 H6A H6B C7 - Distance Angles N1 1.4652 (0.0020) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - N1 H7A H7B C8 - Distance Angles C13 1.3869 (0.0023) C9 1.3942 (0.0022) 119.47 (0.14) C4 1.5262 (0.0020) 120.13 (0.14) 120.34 (0.14) C8 - C13 C9 C9 - Distance Angles C10 1.3848 (0.0026) C8 1.3942 (0.0022) 120.21 (0.16) H9 0.9500 119.90 119.90 C9 - C10 C8 C10 - Distance Angles C11 1.3814 (0.0032) C9 1.3848 (0.0026) 120.15 (0.17) H10 0.9500 119.93 119.93 C10 - C11 C9 C11 - Distance Angles C12 1.3808 (0.0032) C10 1.3814 (0.0032) 120.00 (0.16) H11 0.9500 120.00 120.00 C11 - C12 C10 C12 - Distance Angles C11 1.3808 (0.0032) C13 1.3933 (0.0025) 120.24 (0.18) H12 0.9500 119.88 119.88 C12 - C11 C13 C13 - Distance Angles C8 1.3869 (0.0023) C12 1.3933 (0.0025) 119.90 (0.16) H13 0.9500 120.05 120.05 C13 - C8 C12 N1 - Distance Angles C5 1.3515 (0.0021) C6 1.4538 (0.0022) 118.85 (0.14) C7 1.4652 (0.0020) 125.57 (0.14) 115.28 (0.14) N1 - C5 C6 O1 - Distance Angles C4 1.4266 (0.0017) Si1 1.6553 (0.0011) 126.51 (0.09) O1 - C4 O2 - Distance Angles C5 1.2271 (0.0020) O2 - Si1 - Distance Angles O1 1.6553 (0.0011) C2 1.8559 (0.0018) 112.01 (0.07) C1 1.8636 (0.0020) 109.41 (0.07) 110.44 (0.10) C3 1.8697 (0.0019) 105.03 (0.08) 107.95 (0.09) 111.91 (0.10) Si1 - O1 C2 C1 FMAP and GRID set by program FMAP 2 3 22 GRID -1.316 -2 -2 1.316 2 2 R1 = 0.0561 for 1918 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.55 at 0.0282 0.4212 0.2398 [ 0.12 A from O2 ] Deepest hole -0.98 at 0.2545 0.2670 0.0779 [ 1.00 A from SI1 ] Mean = 0.01, Rms deviation from mean = 0.24 e/A^3, Highest memory used = 2286 / 18045 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.5606 0.4304 0.2389 1.00000 0.05 0.53 1.08 H6C 1.82 C6 2.03 H6A 2.21 H6B Q2 1 -0.4069 0.0912 0.3879 1.00000 0.05 0.45 1.47 H7C 1.63 H2C 1.96 H7B 2.01 C7 Q3 1 0.5391 0.1053 0.1165 1.00000 0.05 0.44 0.37 H3C 0.81 C3 1.35 H3A 1.37 H3B Q4 1 -0.0486 0.1590 0.1139 1.00000 0.05 0.43 0.43 H1C 0.93 C1 1.29 H1A 1.59 H1B Q5 1 -0.5297 0.3320 0.2555 1.00000 0.05 0.43 0.69 H6C 1.60 C6 1.83 O1 2.03 H6B Q6 1 -0.5428 0.5164 0.2559 1.00000 0.05 0.42 1.76 H6C 1.88 H7B 1.92 H6A 2.05 C6 Q7 1 0.4693 0.5234 0.1286 1.00000 0.05 0.42 1.14 H2C 2.10 C2 2.22 H7B 2.27 H7C Q8 1 -0.4437 0.1504 0.3807 1.00000 0.05 0.41 1.31 H7C 1.71 H7B 1.84 C7 2.33 H2C Q9 1 0.5120 0.5776 0.1194 1.00000 0.05 0.40 1.78 H2C 2.09 H7B 2.10 C12 2.10 H7C Q10 1 0.0438 0.2779 0.2597 1.00000 0.05 0.40 0.73 C5 0.81 C4 1.50 H4 1.67 O2 Shortest distances between peaks (including symmetry equivalents) 7 9 0.69 2 8 0.72 2 9 0.79 2 7 0.93 8 9 0.95 1 6 1.01 1 5 1.15 7 8 1.43 5 6 2.04 1 7 2.26 6 7 2.31 3 6 2.52 6 9 2.60 1 9 2.76 2 6 2.76 6 8 2.89 1 2 2.92 Time profile in seconds ----------------------- 0.05: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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. 0.80: 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 4.41: Structure factors and derivatives 2.95: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.38: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0238 finished at 13:49:10 Total CPU time: 8.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++