+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 17:20:54 on 08-Oct-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0940 in P-1 CELL 0.71073 7.2306 9.4023 9.5351 119.096 96.715 98.833 ZERR 2.00 0.0005 0.0008 0.0008 0.004 0.005 0.005 LATT 1 SFAC C H N O SI CL F UNIT 16 24 2 4 2 2 2 V = 545.76 F(000) = 246.0 Mu = 0.45 mm-1 Cell Wt = 473.45 Rho = 1.441 MERG 2 OMIT -3.00 55.00 OMIT 1 -3 1 OMIT 0 -3 2 SIZE 0.08 0.26 0.36 ACTA BOND $H WGHT 0.12120 1.85670 L.S. 4 TEMP -153.00 FVAR 1.06395 SI1 5 0.309122 0.205287 0.709893 11.00000 0.04084 0.02538 = 0.01853 0.01273 0.00310 0.00727 CL1 6 0.591824 0.380058 0.595029 11.00000 0.05035 0.03558 = 0.04097 0.02245 0.01935 0.00892 O1 4 0.397709 0.265200 0.940753 11.00000 0.03455 0.02233 = 0.01854 0.01030 0.00136 0.00463 N1 3 0.232207 -0.002092 0.837966 11.00000 0.02516 0.02474 = 0.01714 0.01188 0.00420 0.00933 C1 1 0.214173 -0.007746 0.680107 11.00000 0.03198 0.02728 = 0.01587 0.01049 0.00246 0.00574 AFIX 23 H1A 2 0.077410 -0.050116 0.621931 11.00000 -1.20000 H1B 2 0.285919 -0.086692 0.610523 11.00000 -1.20000 AFIX 0 C5 1 0.184459 -0.118676 1.004605 11.00000 0.02668 0.03391 = 0.03497 0.02366 0.01206 0.01360 AFIX 43 H5 2 0.133822 -0.210242 1.017091 11.00000 -1.20000 AFIX 0 C6 1 0.155021 -0.136315 0.851915 11.00000 0.02338 0.02703 = 0.02824 0.01557 0.00943 0.01167 C2 1 0.335124 0.149508 0.969715 11.00000 0.02205 0.02816 = 0.01811 0.01260 0.00616 0.01102 C4 1 0.289677 0.034982 1.143162 11.00000 0.02789 0.04177 = 0.02423 0.02072 0.01038 0.01857 AFIX 43 H4 2 0.308378 0.046481 1.248811 11.00000 -1.20000 AFIX 0 C3 1 0.365171 0.167635 1.127766 11.00000 0.02616 0.03187 = 0.01721 0.01157 0.00423 0.01121 AFIX 43 H3 2 0.436854 0.270679 1.221657 11.00000 -1.20000 AFIX 0 C8 1 0.567742 0.292997 0.726687 11.00000 0.04101 0.03924 = 0.02925 0.02069 0.00309 -0.00249 AFIX 23 H8B 2 0.626954 0.381664 0.842327 11.00000 -1.20000 H8A 2 0.637337 0.202911 0.695571 11.00000 -1.20000 AFIX 0 F1 7 0.242560 0.122745 0.505628 11.00000 0.05065 0.04047 = 0.02032 0.01751 0.00157 0.00384 C7 1 0.045805 -0.294846 0.697611 11.00000 0.03497 0.02591 = 0.03108 0.01303 0.00922 0.00895 AFIX 137 H7A 2 -0.060630 -0.271944 0.644551 11.00000 -1.20000 H7C 2 -0.005033 -0.378889 0.724902 11.00000 -1.20000 H7B 2 0.131629 -0.337417 0.622434 11.00000 -1.20000 AFIX 0 C9 1 0.152798 0.359731 0.777009 11.00000 0.06458 0.03874 = 0.04009 0.02406 0.00018 0.01890 AFIX 137 H9A 2 0.077916 0.352016 0.679948 11.00000 -1.50000 H9B 2 0.233856 0.473704 0.848843 11.00000 -1.50000 H9C 2 0.065487 0.333630 0.837070 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2008src0940 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 CL 0.990 F 0.640 Si1 - F1 C8 C1 C9 O1 Cl1 - C8 O1 - C2 Si1 N1 - C2 C6 C1 C1 - N1 Si1 C5 - C6 C4 C6 - C5 N1 C7 C2 - O1 N1 C3 C4 - C3 C5 C3 - C4 C2 C8 - Cl1 Si1 F1 - Si1 C7 - C6 C9 - Si1 12298 Reflections read, of which 21 rejected -9 =< h =< 9, -12 =< k =< 12, -12 =< l =< 12, Max. 2-theta = 55.00 0 Systematic absence violations 0 Inconsistent equivalents 2511 Unique reflections, of which 0 suppressed R(int) = 0.0571 R(sigma) = 0.0445 Friedel opposites merged Maximum memory for data reduction = 1545 / 25494 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. ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 16.00 18.00 H 24.00 26.00 N 2.00 2.00 O 4.00 2.00 SI 2.00 2.00 CL 2.00 2.00 F 2.00 2.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 1914 / 166542 wR2 = 0.2356 before cycle 1 for 2511 data and 129 / 129 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1212 * P )^2 + 1.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06348 0.00546 -0.086 OSF Mean shift/esd = 0.037 Maximum = 0.240 for y C7 Max. shift = 0.008 A for H7B Max. dU = 0.000 for O1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1914 / 166542 wR2 = 0.2356 before cycle 2 for 2511 data and 129 / 129 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1212 * P )^2 + 1.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06336 0.00545 -0.021 OSF Mean shift/esd = 0.015 Maximum = -0.090 for y F1 Max. shift = 0.002 A for H7B Max. dU = 0.000 for O1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1914 / 166542 wR2 = 0.2356 before cycle 3 for 2511 data and 129 / 129 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1212 * P )^2 + 1.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06336 0.00545 -0.001 OSF Mean shift/esd = 0.002 Maximum = -0.011 for y F1 Max. shift = 0.000 A for H9A Max. dU = 0.000 for C8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1914 / 166542 wR2 = 0.2356 before cycle 4 for 2511 data and 129 / 129 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1212 * P )^2 + 1.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06336 0.00545 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.004 for tors H9A Max. shift = 0.000 A for H9A Max. dU = 0.000 for C2 Largest correlation matrix elements 0.674 U23 C5 / U22 C5 0.652 U23 C9 / U33 C9 0.625 U23 C6 / U22 C6 0.671 U23 C5 / U33 C5 0.650 U23 C9 / U22 C9 0.618 U23 C2 / U22 C2 0.666 U23 Cl1 / U22 Cl1 0.642 U23 C8 / U22 C8 0.612 U23 C2 / U33 C2 0.662 U23 Cl1 / U33 Cl1 0.639 U23 C8 / U33 C8 0.608 U23 N1 / U33 N1 0.661 U23 C4 / U22 C4 0.636 U23 F1 / U22 F1 0.605 U23 C7 / U22 C7 0.660 U23 Si1 / U33 Si1 0.636 U23 F1 / U33 F1 0.605 U23 O1 / U33 O1 0.658 U23 Si1 / U22 Si1 0.626 U23 N1 / U22 N1 0.603 U23 O1 / U22 O1 0.656 U23 C4 / U33 C4 0.626 U23 C6 / U33 C6 0.598 U23 C1 / U22 C1 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.0774 -0.0500 0.6219 23 0.990 0.000 C1 N1 Si1 H1B 0.2859 -0.0866 0.6105 23 0.990 0.000 C1 N1 Si1 H5 0.1339 -0.2101 1.0171 43 0.950 0.000 C5 C6 C4 H4 0.3084 0.0467 1.2488 43 0.950 0.000 C4 C3 C5 H3 0.4369 0.2705 1.2217 43 0.950 0.000 C3 C4 C2 H8B 0.6270 0.3815 0.8423 23 0.990 0.000 C8 Cl1 Si1 H8A 0.6373 0.2027 0.6955 23 0.990 0.000 C8 Cl1 Si1 H7A -0.0613 -0.2719 0.6451 137 0.980 0.000 C7 C6 H7A H7C -0.0040 -0.3791 0.7247 137 0.980 0.000 C7 C6 H7A H7B 0.1313 -0.3366 0.6219 137 0.980 0.000 C7 C6 H7A H9A 0.0783 0.3523 0.6800 137 0.980 0.000 C9 Si1 H9A H9B 0.2339 0.4737 0.8491 137 0.980 0.000 C9 Si1 H9A H9C 0.0653 0.3336 0.8368 137 0.980 0.000 C9 Si1 H9A 2008src0940 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Si1 0.30912 0.20526 0.70990 1.00000 0.04082 0.02535 0.01851 0.01272 0.00310 0.00727 0.02800 0.00289 0.00018 0.00014 0.00013 0.00000 0.00070 0.00061 0.00055 0.00047 0.00046 0.00049 0.00035 Cl1 0.59182 0.38007 0.59502 1.00000 0.05035 0.03551 0.04096 0.02246 0.01935 0.00892 0.04032 0.00319 0.00018 0.00015 0.00015 0.00000 0.00072 0.00065 0.00066 0.00053 0.00053 0.00051 0.00037 O1 0.39772 0.26524 0.94075 1.00000 0.03456 0.02218 0.01857 0.01035 0.00136 0.00460 0.02587 0.00697 0.00043 0.00035 0.00033 0.00000 0.00151 0.00139 0.00129 0.00112 0.00110 0.00115 0.00062 N1 0.23218 -0.00220 0.83797 1.00000 0.02507 0.02478 0.01708 0.01180 0.00417 0.00930 0.02148 0.00825 0.00046 0.00041 0.00038 0.00000 0.00158 0.00165 0.00145 0.00130 0.00121 0.00130 0.00068 C1 0.21419 -0.00764 0.68011 1.00000 0.03189 0.02734 0.01581 0.01038 0.00243 0.00578 0.02577 0.00999 0.00060 0.00051 0.00046 0.00000 0.00208 0.00202 0.00171 0.00156 0.00148 0.00163 0.00083 H1A 0.07743 -0.04997 0.62194 1.00000 0.03093 0.00000 0.00000 H1B 0.28591 -0.08658 0.61047 1.00000 0.03093 0.00000 0.00000 C5 0.18448 -0.11858 1.00458 1.00000 0.02664 0.03399 0.03487 0.02358 0.01203 0.01363 0.02791 0.01150 0.00059 0.00056 0.00054 0.00000 0.00196 0.00221 0.00220 0.00190 0.00168 0.00170 0.00087 H5 0.13386 -0.21013 1.01709 1.00000 0.03349 0.00000 0.00000 C6 0.15504 -0.13622 0.85190 1.00000 0.02339 0.02689 0.02829 0.01561 0.00942 0.01167 0.02450 0.01053 0.00056 0.00051 0.00050 0.00000 0.00185 0.00200 0.00199 0.00170 0.00155 0.00156 0.00082 C2 0.33512 0.14952 0.96972 1.00000 0.02196 0.02825 0.01799 0.01244 0.00610 0.01104 0.02170 0.00996 0.00054 0.00050 0.00046 0.00000 0.00176 0.00195 0.00169 0.00154 0.00138 0.00150 0.00077 C4 0.28973 0.03516 1.14315 1.00000 0.02792 0.04166 0.02422 0.02072 0.01035 0.01854 0.02786 0.01123 0.00058 0.00057 0.00050 0.00000 0.00201 0.00242 0.00192 0.00187 0.00158 0.00180 0.00089 H4 0.30838 0.04670 1.24882 1.00000 0.03343 0.00000 0.00000 C3 0.36512 0.16747 1.12777 1.00000 0.02614 0.03186 0.01713 0.01152 0.00420 0.01121 0.02506 0.01038 0.00057 0.00053 0.00047 0.00000 0.00191 0.00210 0.00174 0.00160 0.00144 0.00162 0.00083 H3 0.43688 0.27046 1.22168 1.00000 0.03007 0.00000 0.00000 C8 0.56775 0.29287 0.72669 1.00000 0.04086 0.03940 0.02914 0.02056 0.00306 -0.00254 0.03713 0.01210 0.00071 0.00064 0.00058 0.00000 0.00248 0.00255 0.00219 0.00203 0.00186 0.00199 0.00104 H8B 0.62701 0.38148 0.84234 1.00000 0.04456 0.00000 0.00000 H8A 0.63728 0.20273 0.69549 1.00000 0.04456 0.00000 0.00000 F1 0.24254 0.12264 0.50563 1.00000 0.05054 0.04059 0.02025 0.01748 0.00155 0.00383 0.03780 0.00666 0.00042 0.00035 0.00030 0.00000 0.00163 0.00152 0.00118 0.00113 0.00110 0.00124 0.00066 C7 0.04583 -0.29467 0.69756 1.00000 0.03497 0.02587 0.03102 0.01300 0.00921 0.00895 0.03097 0.01109 0.00065 0.00054 0.00054 0.00000 0.00224 0.00209 0.00217 0.00182 0.00179 0.00174 0.00092 H7A -0.06133 -0.27194 0.64510 1.00000 0.03716 0.00000 0.00000 H7C -0.00399 -0.37912 0.72465 1.00000 0.03716 0.00000 0.00000 H7B 0.13134 -0.33662 0.62194 1.00000 0.03716 0.00000 0.00000 C9 0.15284 0.35982 0.77700 1.00000 0.06452 0.03891 0.03991 0.02387 0.00011 0.01902 0.04643 0.01416 0.00087 0.00067 0.00066 0.00000 0.00345 0.00270 0.00268 0.00233 0.00242 0.00250 0.00129 H9A 0.07825 0.35232 0.67995 1.00000 0.06965 0.00000 0.00000 H9B 0.23393 0.47375 0.84907 1.00000 0.06965 0.00000 0.00000 H9C 0.06527 0.33358 0.83682 1.00000 0.06965 0.00000 0.00000 Final Structure Factor Calculation for 2008src0940 in P-1 Total number of l.s. parameters = 129 Maximum vector length = 511 Memory required = 1785 / 26061 wR2 = 0.2356 before cycle 5 for 2511 data and 0 / 129 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1212 * P )^2 + 1.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0826 for 2001 Fo > 4sig(Fo) and 0.1003 for all 2511 data wR2 = 0.2356, GooF = S = 1.064, Restrained GooF = 1.064 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0425 0.0253 0.0162 Si1 0.0565 0.0374 0.0270 Cl1 0.0372 0.0226 0.0178 O1 0.0284 0.0210 0.0150 N1 0.0333 0.0288 0.0151 C1 0.0397 0.0235 0.0206 C5 0.0307 0.0253 0.0175 C6 0.0308 0.0177 0.0167 C2 0.0452 0.0199 0.0184 C4 0.0361 0.0227 0.0164 C3 0.0564 0.0305 0.0245 C8 0.0571 0.0394 0.0168 F1 0.0357 0.0323 0.0249 C7 0.0744 0.0418 0.0231 C9 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.026 0.039 0.053 0.070 0.089 0.111 0.146 0.208 1.000 Number in group 260. 250. 252. 249. 256. 243. 248. 256. 246. 251. GooF 1.185 0.950 0.933 1.133 1.088 1.020 1.009 1.055 1.260 0.953 K 3.765 1.210 1.034 0.990 0.970 0.994 1.017 1.027 1.022 1.029 Resolution(A) 0.77 0.79 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.64 inf Number in group 253. 255. 248. 250. 251. 251. 252. 249. 249. 253. GooF 0.827 0.840 0.894 0.862 0.913 0.922 0.932 1.068 1.195 1.803 K 1.005 1.028 1.008 1.044 1.037 1.028 1.037 1.056 1.030 1.012 R1 0.175 0.152 0.140 0.105 0.103 0.092 0.087 0.075 0.077 0.086 Recommended weighting scheme: WGHT 0.1204 1.7593 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) -1 2 1 22.55 0.06 5.49 0.003 3.08 -3 -2 3 73.84 20.80 5.16 0.052 1.92 -4 1 2 21.41 0.90 4.82 0.011 1.71 -4 3 0 367.36 181.94 4.82 0.154 1.65 0 -4 3 87.32 32.86 4.41 0.065 2.25 2 -2 1 14.00 0.33 4.21 0.007 3.02 1 1 0 485.75 270.74 4.13 0.188 4.71 0 -2 3 45.51 13.70 4.11 0.042 3.10 -1 3 0 104.23 227.04 4.04 0.172 2.71 -1 1 0 860.69 1948.77 3.96 0.504 6.02 -1 4 0 242.58 131.77 3.86 0.131 2.05 0 1 2 127.76 258.79 3.82 0.184 3.04 0 -2 2 388.61 227.60 3.63 0.172 4.08 1 3 1 180.35 98.48 3.56 0.113 1.96 2 -2 2 8.61 37.44 3.48 0.070 2.68 -2 0 2 22.71 63.85 3.47 0.091 2.99 0 -5 6 13.83 1.29 3.43 0.013 1.47 0 -1 4 157.46 86.99 3.39 0.106 2.27 0 -5 3 21.44 60.34 3.39 0.089 1.85 -1 -7 5 18.66 3.69 3.28 0.022 1.25 2 -3 2 35.36 12.70 3.26 0.041 2.44 2 -1 2 20.17 55.41 3.25 0.085 2.66 -2 4 2 18.70 4.22 3.20 0.023 1.54 -3 2 0 288.93 178.68 3.17 0.153 2.26 4 -7 6 46.88 97.96 3.11 0.113 1.04 2 -7 3 8.85 0.32 3.07 0.006 1.31 1 -4 1 9.66 0.83 3.07 0.010 2.25 -8 -1 2 38.46 14.07 2.98 0.043 0.87 -4 1 1 48.16 96.42 2.96 0.112 1.80 -8 -2 4 185.24 111.03 2.92 0.120 0.85 -3 -3 6 10.63 1.16 2.92 0.012 1.38 -1 -6 4 121.79 208.17 2.91 0.165 1.46 -3 -1 3 145.76 243.92 2.91 0.178 2.02 1 -3 3 81.99 44.08 2.90 0.076 2.56 -4 -4 8 9.99 0.18 2.90 0.005 1.04 3 0 0 406.60 267.71 2.90 0.187 2.32 -7 1 1 72.91 37.96 2.89 0.070 1.03 0 -1 3 203.23 329.24 2.89 0.207 3.09 0 -3 4 31.36 12.14 2.88 0.040 2.27 -1 -3 1 33.55 70.82 2.84 0.096 2.60 -6 -5 3 82.77 44.56 2.83 0.076 0.93 -3 1 2 113.35 66.75 2.79 0.093 2.13 0 -4 6 79.15 43.54 2.77 0.075 1.55 1 0 5 23.12 7.73 2.73 0.032 1.51 -6 0 7 15.05 2.32 2.72 0.017 0.93 -3 3 3 99.05 166.60 2.71 0.147 1.48 -2 -3 5 162.83 259.26 2.69 0.184 1.72 4 -6 2 186.87 119.67 2.69 0.125 1.27 2 2 1 6.90 0.46 2.69 0.008 2.03 -2 -2 3 70.41 122.87 2.66 0.127 2.39 Bond lengths and angles Si1 - Distance Angles F1 1.6803 (0.0026) C8 1.8788 (0.0050) 95.31 (0.18) C1 1.8810 (0.0043) 89.40 (0.16) 123.91 (0.22) C9 1.8887 (0.0055) 98.37 (0.19) 116.37 (0.26) 118.07 (0.23) O1 1.9814 (0.0029) 170.17 (0.15) 84.56 (0.17) 82.58 (0.14) 90.45 (0.19) Si1 - F1 C8 C1 C9 Cl1 - Distance Angles C8 1.8130 (0.0047) Cl1 - O1 - Distance Angles C2 1.2788 (0.0049) Si1 1.9814 (0.0029) 114.12 (0.25) O1 - C2 N1 - Distance Angles C2 1.3709 (0.0052) C6 1.3714 (0.0052) 123.28 (0.33) C1 1.4705 (0.0046) 113.41 (0.32) 123.31 (0.34) N1 - C2 C6 C1 - Distance Angles N1 1.4705 (0.0046) Si1 1.8810 (0.0042) 111.72 (0.27) H1A 0.9900 109.28 109.28 H1B 0.9900 109.28 109.28 107.94 C1 - N1 Si1 H1A C5 - Distance Angles C6 1.3691 (0.0057) C4 1.4085 (0.0064) 120.08 (0.39) H5 0.9500 119.96 119.96 C5 - C6 C4 C6 - Distance Angles C5 1.3691 (0.0057) N1 1.3714 (0.0052) 118.43 (0.38) C7 1.4978 (0.0059) 123.92 (0.39) 117.63 (0.36) C6 - C5 N1 C2 - Distance Angles O1 1.2788 (0.0049) N1 1.3709 (0.0051) 117.26 (0.33) C3 1.4183 (0.0051) 124.60 (0.37) 118.14 (0.36) C2 - O1 N1 C4 - Distance Angles C3 1.3617 (0.0061) C5 1.4085 (0.0064) 120.92 (0.37) H4 0.9500 119.54 119.54 C4 - C3 C5 C3 - Distance Angles C4 1.3617 (0.0061) C2 1.4183 (0.0051) 119.14 (0.38) H3 0.9500 120.43 120.43 C3 - C4 C2 C8 - Distance Angles Cl1 1.8130 (0.0046) Si1 1.8788 (0.0049) 111.58 (0.26) H8B 0.9900 109.31 109.31 H8A 0.9900 109.31 109.31 107.96 C8 - Cl1 Si1 H8B F1 - Distance Angles Si1 1.6803 (0.0026) F1 - C7 - Distance Angles C6 1.4978 (0.0058) H7A 0.9800 109.47 H7C 0.9800 109.47 109.47 H7B 0.9800 109.47 109.47 109.47 C7 - C6 H7A H7C C9 - Distance Angles Si1 1.8887 (0.0055) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - Si1 H9A H9B FMAP and GRID set by program FMAP 2 1 23 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.0998 for 2511 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 2.75 at 0.0429 0.3802 0.8380 [ 0.49 A from H9C ] Deepest hole -0.71 at 0.2039 0.1728 0.7068 [ 0.77 A from SI1 ] Mean = 0.00, Rms deviation from mean = 0.13 e/A^3, Highest memory used = 1886 / 18214 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4207 0.2353 0.7156 1.00000 0.05 1.23 0.80 SI1 1.08 C8 1.66 H8A 1.71 H8B Q2 1 0.2767 0.4058 0.7597 1.00000 0.05 0.77 0.91 H9B 1.00 C9 1.43 H9A 1.77 SI1 Q3 1 0.3594 0.1500 0.5052 1.00000 0.05 0.57 0.85 F1 1.86 SI1 2.10 C8 2.10 H4 Q4 1 0.2413 -0.0466 1.0661 1.00000 0.05 0.38 0.67 C5 0.75 C4 1.43 H5 1.49 H4 Q5 1 0.1971 -0.1207 0.9245 1.00000 0.05 0.34 0.66 C6 0.77 C5 1.55 H5 1.69 N1 Q6 1 -0.1097 -0.4385 0.4773 1.00000 0.05 0.33 1.55 H7A 1.82 H7B 1.87 H7B 1.93 C7 Q7 1 0.2475 0.0800 0.7209 1.00000 0.05 0.31 0.70 C1 1.25 SI1 1.43 H1A 1.50 H1B Q8 1 0.0284 0.0287 0.8346 1.00000 0.05 0.30 1.54 N1 1.89 H1A 1.98 C6 2.05 C1 Q9 1 0.0948 -0.2362 0.7546 1.00000 0.05 0.29 0.57 C7 0.93 C6 1.25 H7B 1.30 H7C Q10 1 0.5545 0.1266 0.8752 1.00000 0.05 0.28 1.79 O1 1.90 C2 1.98 C4 1.98 H4 Q11 1 0.2205 -0.2095 1.0656 1.00000 0.05 0.28 0.73 H5 1.29 C5 2.00 C4 2.11 H4 Q12 1 0.1021 0.0731 1.0493 1.00000 0.05 0.27 1.72 C4 1.85 C5 1.86 C3 2.09 C6 Q13 1 0.6439 0.2581 1.2826 1.00000 0.05 0.27 1.58 H3 1.63 H7B 2.13 C3 2.14 C6 Q14 1 0.3485 0.0768 1.1186 1.00000 0.05 0.26 0.67 C4 0.80 C3 1.45 H4 1.56 H3 Q15 1 -0.0470 -0.4223 0.9224 1.00000 0.05 0.26 1.92 H5 2.06 H9C 2.16 H7C 2.35 H9C Q16 1 0.7605 0.1947 0.7007 1.00000 0.05 0.26 0.90 H8A 1.76 C8 2.09 H8B 2.25 H9C Q17 1 0.2715 0.2777 0.7444 1.00000 0.05 0.26 0.71 SI1 1.21 C9 1.70 H9B 1.83 H9A Q18 1 0.1243 -0.2225 0.5221 1.00000 0.05 0.25 1.40 H1B 1.55 H1A 1.75 H7B 1.78 C1 Q19 1 0.2899 -0.0786 0.4559 1.00000 0.05 0.24 1.52 H1B 1.57 H8A 1.81 F1 2.08 C1 Q20 1 0.2241 -0.3244 0.9628 1.00000 0.05 0.23 1.27 H5 1.69 H9B 1.85 C5 2.36 H8B Shortest distances between peaks (including symmetry equivalents) 11 20 1.06 4 14 1.12 2 17 1.13 4 5 1.15 1 17 1.22 16 19 1.31 5 9 1.45 4 11 1.51 10 11 1.59 12 12 1.66 4 12 1.67 1 3 1.73 7 17 1.74 1 7 1.80 12 14 1.81 8 12 1.87 4 10 1.90 5 11 1.90 5 14 1.91 5 12 1.92 3 19 1.93 15 20 1.94 1 2 1.95 9 13 1.99 8 12 2.01 10 20 2.03 18 19 2.04 7 8 2.14 5 20 2.15 11 16 2.15 10 14 2.16 6 6 2.22 3 17 2.23 6 18 2.26 4 8 2.26 11 15 2.27 4 20 2.28 5 12 2.29 9 18 2.31 7 19 2.32 5 13 2.32 13 14 2.33 7 10 2.37 8 9 2.37 5 8 2.38 1 10 2.40 2 20 2.45 7 18 2.46 6 9 2.48 11 14 2.48 16 18 2.48 5 10 2.49 4 12 2.52 9 12 2.53 13 18 2.54 1 16 2.55 4 9 2.58 10 16 2.59 8 11 2.61 2 6 2.61 3 7 2.62 9 20 2.63 15 15 2.64 2 3 2.67 1 19 2.69 6 13 2.70 3 19 2.75 3 16 2.77 6 9 2.80 16 20 2.80 5 8 2.84 2 7 2.87 9 11 2.87 9 12 2.89 8 14 2.91 13 20 2.92 1 19 2.94 4 8 2.97 11 12 2.98 19 19 2.99 Time profile in seconds ----------------------- 0.14: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.03: 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 0.02: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.03: Analyse other restraints etc. 16.75: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.14: Structure factors and derivatives 1.81: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.11: Apply other restraints 1.42: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.41: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxl finished at 17:21:16 Total CPU time: 22.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++