+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0169 started at 15:33:09 on 26-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0169 in P2(1) CELL 0.71073 8.4340 7.2540 9.6610 90.000 103.079 90.000 ZERR 2.00 0.0003 0.0002 0.0003 0.000 0.002 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O SI I UNIT 16 28 2 4 2 2 V = 575.73 F(000) = 304.0 Mu = 2.86 mm-1 Cell Wt = 622.38 Rho = 1.795 MERG 2 OMIT -3.00 55.00 TWIN BASF 0.48208 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.04 0.16 0.18 ACTA WGHT 0.00000 0.71040 L.S. 8 TEMP -153.00 FVAR 0.56754 C2 1 1.065810 0.282754 0.368246 11.00000 0.01448 0.01525 = 0.01712 -0.00258 0.00346 -0.00197 C3 1 1.148218 0.263633 0.519405 11.00000 0.02479 0.02810 = 0.01327 0.00277 0.00088 -0.00068 AFIX 23 H3A 2 1.156641 0.131448 0.545537 11.00000 -1.20000 H3B 2 1.083119 0.325847 0.579031 11.00000 -1.20000 AFIX 0 C4 1 1.317363 0.347976 0.547580 11.00000 0.01752 0.02862 = 0.01806 -0.00540 -0.00475 -0.00161 AFIX 23 H4A 2 1.308802 0.483625 0.537288 11.00000 -1.20000 H4B 2 1.376663 0.319573 0.645917 11.00000 -1.20000 AFIX 0 C5 1 1.409350 0.270840 0.443429 11.00000 0.01204 0.02976 = 0.01962 -0.00152 -0.00444 0.00318 AFIX 23 H5A 2 1.515912 0.333905 0.457577 11.00000 -1.20000 H5B 2 1.430488 0.138226 0.463817 11.00000 -1.20000 AFIX 0 C6 1 1.320433 0.292414 0.291224 11.00000 0.01216 0.01242 = 0.02405 -0.00111 0.00376 -0.00548 C7 1 1.046123 0.305695 0.118380 11.00000 0.01664 0.01654 = 0.01115 0.00150 0.00043 -0.00598 AFIX 23 H7A 2 1.068775 0.201019 0.059987 11.00000 -1.20000 H7B 2 1.066795 0.422660 0.072676 11.00000 -1.20000 AFIX 0 C8 1 0.713266 0.082978 0.101346 11.00000 0.01137 0.02306 = 0.01828 -0.00274 0.00655 -0.00398 AFIX 137 H8A 2 0.784021 -0.023383 0.132410 11.00000 -1.50000 H8B 2 0.669078 0.075673 -0.001447 11.00000 -1.50000 H8C 2 0.623622 0.082762 0.150561 11.00000 -1.50000 AFIX 0 C9 1 0.721819 0.515349 0.120040 11.00000 0.02243 0.01946 = 0.02470 0.00212 -0.00037 -0.00165 AFIX 137 H9A 2 0.631143 0.509944 0.167914 11.00000 -1.50000 H9B 2 0.679514 0.538614 0.018459 11.00000 -1.50000 H9C 2 0.796050 0.615058 0.161168 11.00000 -1.50000 AFIX 0 N1 3 1.145861 0.293460 0.265884 11.00000 0.01310 0.01379 = 0.01496 -0.00526 0.00151 0.00157 O2 4 0.908502 0.283387 0.330482 11.00000 0.01177 0.03642 = 0.01650 0.00475 0.00404 -0.00011 O6 4 1.382040 0.301035 0.191022 11.00000 0.01472 0.02472 = 0.02549 -0.00282 0.00631 0.00819 SI1 5 0.831347 0.296165 0.143490 11.00000 0.01189 0.01667 = 0.01642 0.00279 0.00201 0.00241 I1 6 1.189852 -0.197324 0.248342 11.00000 0.02034 0.01553 = 0.01994 -0.00105 0.00094 -0.00057 HKLF 4 Covalent radii and connectivity table for 2009src0169 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 I 1.330 C2 - O2 N1 C3 C3 - C2 C4 C4 - C5 C3 C5 - C6 C4 C6 - O6 N1 C5 C7 - N1 Si1 C8 - Si1 C9 - Si1 N1 - C2 C6 C7 O2 - C2 Si1 O6 - C6 Si1 - O2 C9 C8 C7 I1 - no bonds found Floating origin restraints generated 6965 Reflections read, of which 9 rejected -10 =< h =< 10, -9 =< k =< 9, -12 =< l =< 12, Max. 2-theta = 54.94 0 Systematic absence violations 0 Inconsistent equivalents 2582 Unique reflections, of which 0 suppressed R(int) = 0.0328 R(sigma) = 0.0398 Friedel opposites not merged Maximum memory for data reduction = 1407 / 25685 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 = 1768 / 156324 wR2 = 0.0497 before cycle 1 for 2582 data and 121 / 121 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56702 0.00053 -0.977 OSF 2 0.48166 0.03651 -0.012 BASF 1 Mean shift/su = 0.197 Maximum = 1.132 for U11 I1 Max. shift = 0.006 A for H9A Max. dU = 0.000 for C4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1768 / 156324 wR2 = 0.0495 before cycle 2 for 2582 data and 121 / 121 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56723 0.00053 0.401 OSF 2 0.48132 0.03665 -0.009 BASF 1 Mean shift/su = 0.068 Maximum = 0.401 for OSF Max. shift = 0.004 A for H9B Max. dU = 0.000 for C4 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1768 / 156324 wR2 = 0.0495 before cycle 3 for 2582 data and 121 / 121 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56723 0.00053 0.003 OSF 2 0.48139 0.03673 0.002 BASF 1 Mean shift/su = 0.008 Maximum = 0.036 for U23 O6 Max. shift = 0.002 A for H9B Max. dU = 0.000 for C9 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1768 / 156324 wR2 = 0.0495 before cycle 4 for 2582 data and 121 / 121 parameters GooF = S = 1.031; Restrained GooF = 1.030 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56723 0.00053 0.000 OSF 2 0.48156 0.03676 0.005 BASF 1 Mean shift/su = 0.002 Maximum = 0.013 for x C9 Max. shift = 0.000 A for H8B Max. dU = 0.000 for C9 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1768 / 156324 wR2 = 0.0495 before cycle 5 for 2582 data and 121 / 121 parameters GooF = S = 1.030; Restrained GooF = 1.029 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56724 0.00053 0.002 OSF 2 0.48157 0.03672 0.000 BASF 1 Mean shift/su = 0.001 Maximum = 0.003 for U22 C9 Max. shift = 0.000 A for H9A Max. dU = 0.000 for C2 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1768 / 156324 wR2 = 0.0495 before cycle 6 for 2582 data and 121 / 121 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56724 0.00053 0.001 OSF 2 0.48157 0.03676 0.000 BASF 1 Mean shift/su = 0.000 Maximum = -0.002 for x I1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for C5 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1768 / 156324 wR2 = 0.0495 before cycle 7 for 2582 data and 121 / 121 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56724 0.00053 0.000 OSF 2 0.48158 0.03675 0.000 BASF 1 Mean shift/su = 0.000 Maximum = -0.002 for x I1 Max. shift = 0.000 A for H9B Max. dU = 0.000 for C5 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1768 / 156324 wR2 = 0.0495 before cycle 8 for 2582 data and 121 / 121 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56724 0.00053 0.001 OSF 2 0.48158 0.03675 0.000 BASF 1 Mean shift/su = 0.000 Maximum = -0.002 for x I1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for C3 Largest correlation matrix elements -0.892 x C9 / x C8 -0.769 U11 C9 / U11 C8 0.534 U33 I1 / OSF 0.890 U22 C2 / y C2 0.762 U22 N1 / y N1 -0.524 U13 C9 / U13 C8 0.885 U22 O2 / y O2 0.734 tors H9A / tors H8A -0.522 U23 C6 / z C6 0.828 y C9 / y C8 0.719 U22 C5 / y C5 -0.515 U12 O2 / x O2 0.817 U22 C6 / y C6 0.689 U22 Si1 / y Si1 0.507 U22 I1 / OSF -0.798 z C9 / z C8 0.652 U33 C9 / z C8 0.503 U11 I1 / OSF 0.780 U12 C9 / U12 C8 0.615 U23 C9 / U23 C8 -0.770 U22 C9 / U22 C8 -0.553 z C9 / U33 C8 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3A 1.1565 0.1315 0.5458 23 0.990 0.000 C3 C2 C4 H3B 1.0831 0.3261 0.5791 23 0.990 0.000 C3 C2 C4 H4A 1.3088 0.4836 0.5372 23 0.990 0.000 C4 C5 C3 H4B 1.3767 0.3197 0.6459 23 0.990 0.000 C4 C5 C3 H5A 1.5162 0.3338 0.4578 23 0.990 0.000 C5 C6 C4 H5B 1.4305 0.1382 0.4638 23 0.990 0.000 C5 C6 C4 H7A 1.0686 0.2002 0.0603 23 0.990 0.000 C7 N1 Si1 H7B 1.0668 0.4220 0.0723 23 0.990 0.000 C7 N1 Si1 H8A 0.7839 -0.0234 0.1323 137 0.980 0.000 C8 Si1 H8A H8B 0.6679 0.0759 -0.0009 137 0.980 0.000 C8 Si1 H8A H8C 0.6239 0.0827 0.1517 137 0.980 0.000 C8 Si1 H8A H9A 0.6308 0.5098 0.1666 137 0.980 0.000 C9 Si1 H9A H9B 0.6806 0.5387 0.0178 137 0.980 0.000 C9 Si1 H9A H9C 0.7961 0.6149 0.1612 137 0.980 0.000 C9 Si1 H9A 2009src0169 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 1.06582 0.28276 0.36827 1.00000 0.01539 0.01499 0.01692 -0.00242 0.00380 -0.00301 0.01574 0.01181 0.00040 0.00144 0.00034 0.00000 0.00144 0.00397 0.00140 0.00204 0.00112 0.00209 0.00131 C3 1.14813 0.26368 0.51958 1.00000 0.02426 0.02839 0.01295 0.00287 0.00104 -0.00010 0.02237 0.00696 0.00046 0.00059 0.00036 0.00000 0.00185 0.00388 0.00148 0.00147 0.00134 0.00160 0.00127 H3A 1.15646 0.13152 0.54580 1.00000 0.02684 0.00000 0.00000 H3B 1.08307 0.32608 0.57915 1.00000 0.02684 0.00000 0.00000 C4 1.31740 0.34795 0.54757 1.00000 0.01760 0.02799 0.01748 -0.00530 -0.00454 -0.00095 0.02238 0.00655 0.00045 0.00053 0.00037 0.00000 0.00178 0.00331 0.00165 0.00141 0.00138 0.00143 0.00113 H4A 1.30883 0.48359 0.53721 1.00000 0.02686 0.00000 0.00000 H4B 1.37671 0.31967 0.64592 1.00000 0.02686 0.00000 0.00000 C5 1.40954 0.27085 0.44356 1.00000 0.01316 0.02810 0.01938 -0.00164 -0.00482 0.00296 0.02156 0.00802 0.00043 0.00085 0.00035 0.00000 0.00157 0.00453 0.00154 0.00170 0.00125 0.00162 0.00148 H5A 1.51616 0.33381 0.45783 1.00000 0.02588 0.00000 0.00000 H5B 1.43052 0.13818 0.46380 1.00000 0.02588 0.00000 0.00000 C6 1.32046 0.29290 0.29123 1.00000 0.01204 0.01261 0.02406 -0.00032 0.00376 -0.00582 0.01629 0.01383 0.00037 0.00176 0.00035 0.00000 0.00136 0.00252 0.00143 0.00358 0.00113 0.00343 0.00089 C7 1.04600 0.30532 0.11835 1.00000 0.01701 0.01618 0.01090 0.00006 0.00063 -0.00491 0.01510 0.01383 0.00033 0.00191 0.00026 0.00000 0.00138 0.00136 0.00119 0.00468 0.00103 0.00462 0.00057 H7A 1.06855 0.20025 0.06029 1.00000 0.01812 0.00000 0.00000 H7B 1.06676 0.42196 0.07227 1.00000 0.01812 0.00000 0.00000 C8 0.71297 0.08306 0.10178 1.00000 0.01254 0.02117 0.01944 -0.00192 0.00674 -0.00436 0.01722 0.01696 0.00125 0.00110 0.00102 0.00000 0.00350 0.00323 0.00305 0.00242 0.00250 0.00255 0.00157 H8A 0.78385 -0.02336 0.13230 1.00000 0.02583 0.00000 0.00000 H8B 0.66794 0.07594 -0.00090 1.00000 0.02583 0.00000 0.00000 H8C 0.62392 0.08273 0.15169 1.00000 0.02583 0.00000 0.00000 C9 0.72209 0.51527 0.11950 1.00000 0.02055 0.02045 0.02540 0.00244 -0.00056 -0.00222 0.02305 0.01819 0.00134 0.00112 0.00106 0.00000 0.00418 0.00347 0.00379 0.00254 0.00288 0.00291 0.00198 H9A 0.63081 0.50980 0.16665 1.00000 0.03457 0.00000 0.00000 H9B 0.68064 0.53866 0.01783 1.00000 0.03457 0.00000 0.00000 H9C 0.79608 0.61494 0.16115 1.00000 0.03457 0.00000 0.00000 N1 1.14575 0.29374 0.26583 1.00000 0.01234 0.01381 0.01476 -0.00377 0.00134 0.00236 0.01391 0.01046 0.00031 0.00137 0.00025 0.00000 0.00113 0.00184 0.00108 0.00297 0.00088 0.00311 0.00067 O2 0.90841 0.28342 0.33052 1.00000 0.01214 0.03615 0.01613 0.00500 0.00392 0.00069 0.02136 0.00944 0.00028 0.00121 0.00023 0.00000 0.00102 0.00335 0.00098 0.00192 0.00081 0.00187 0.00108 O6 1.38200 0.30130 0.19093 1.00000 0.01416 0.02471 0.02531 -0.00223 0.00619 0.00617 0.02112 0.00867 0.00023 0.00108 0.00021 0.00000 0.00102 0.00118 0.00105 0.00411 0.00085 0.00441 0.00047 Si1 0.83140 0.29642 0.14348 1.00000 0.01194 0.01702 0.01618 0.00319 0.00196 0.00236 0.01524 0.00374 0.00010 0.00048 0.00008 0.00000 0.00037 0.00055 0.00035 0.00110 0.00029 0.00114 0.00020 I1 1.18985 -0.19733 0.24833 1.00000 0.02050 0.01563 0.02004 -0.00104 0.00093 -0.00046 0.01931 0.00036 0.00002 0.00003 0.00002 0.00000 0.00011 0.00010 0.00010 0.00025 0.00007 0.00026 0.00007 Final Structure Factor Calculation for 2009src0169 in P2(1) Total number of l.s. parameters = 121 Maximum vector length = 511 Memory required = 1649 / 27090 wR2 = 0.0495 before cycle 9 for 2582 data and 2 / 121 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0242 for 2426 Fo > 4sig(Fo) and 0.0271 for all 2582 data wR2 = 0.0495, GooF = S = 1.030, Restrained GooF = 1.030 for all data Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0192 0.0161 0.0119 C2 0.0293 0.0256 0.0122 C3 0.0321 0.0253 0.0097 C4 0.0315 0.0245 0.0087 C5 0.0243 0.0181 0.0064 C6 0.0226 0.0127 0.0101 C7 0.0241 0.0182 0.0094 C8 0.0321 0.0195 0.0176 C9 0.0201 0.0119 0.0098 N1 0.0373 0.0150 0.0118 O2 0.0289 0.0245 0.0100 O6 0.0198 0.0154 0.0105 Si1 0.0250 0.0177 0.0152 I1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.037 0.069 0.092 0.120 0.141 0.166 0.192 0.226 0.288 1.000 Number in group 264. 257. 255. 268. 260. 251. 254. 256. 258. 259. GooF 0.989 1.111 1.156 1.130 1.049 1.025 0.937 0.903 0.917 1.046 K 1.121 1.004 1.008 0.986 0.998 1.006 1.008 1.004 1.003 1.002 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.32 1.67 inf Number in group 267. 254. 258. 260. 252. 257. 260. 263. 252. 259. GooF 1.055 1.016 1.140 1.039 1.030 0.952 0.910 0.899 1.028 1.196 K 1.000 0.991 1.016 1.012 1.005 1.009 1.006 1.000 1.001 1.000 R1 0.054 0.052 0.050 0.037 0.033 0.025 0.019 0.017 0.015 0.013 Recommended weighting scheme: WGHT 0.0000 0.5116 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)/su Fc/Fc(max) Resolution(A) -9 1 1 17.04 51.02 4.23 0.041 0.92 -5 0 3 205.43 265.96 3.68 0.093 1.61 1 1 4 374.26 441.15 3.38 0.119 2.05 1 -1 4 364.34 439.31 3.37 0.119 2.05 4 -7 2 1486.31 1679.03 3.27 0.232 0.89 4 2 4 -0.70 11.73 3.18 0.019 1.30 -6 -6 6 79.25 148.14 3.10 0.069 0.84 -6 1 7 310.55 388.21 3.07 0.112 1.08 -9 -2 5 996.16 1208.84 3.06 0.197 0.88 -10 -2 1 170.00 260.72 2.99 0.092 0.81 2 5 8 601.45 496.89 2.97 0.126 0.86 -3 -1 2 656.26 580.04 2.97 0.137 2.48 -7 3 9 264.80 163.97 2.96 0.073 0.83 -6 0 7 274.38 213.81 2.90 0.083 1.09 -8 -4 8 683.31 922.18 2.88 0.172 0.79 4 0 0 901.24 809.82 2.82 0.161 2.05 2 -2 10 682.50 847.12 2.80 0.165 0.85 -9 2 8 135.88 68.60 2.77 0.047 0.80 -8 0 9 95.79 152.28 2.77 0.070 0.83 1 3 0 2692.87 2883.92 2.76 0.305 2.32 5 1 0 369.85 429.90 2.75 0.118 1.60 -3 0 1 138.08 174.17 2.72 0.075 2.81 3 -5 8 23.70 55.34 2.71 0.042 0.82 0 8 4 514.85 614.02 2.70 0.141 0.85 -7 0 11 109.43 182.46 2.69 0.077 0.78 6 -3 1 387.96 490.39 2.65 0.126 1.15 -7 0 7 738.47 626.59 2.61 0.142 1.00 1 -3 0 2659.32 2883.48 2.59 0.305 2.32 -10 1 6 106.80 154.42 2.56 0.070 0.80 8 1 0 13.67 50.99 2.56 0.041 1.02 2 -7 7 613.03 723.03 2.52 0.153 0.78 5 -1 0 380.50 429.98 2.51 0.118 1.60 1 0 10 212.58 162.33 2.47 0.072 0.91 6 -1 6 570.71 472.12 2.46 0.123 0.92 -3 1 5 2725.41 2888.16 2.45 0.305 1.70 4 0 8 32.70 63.06 2.44 0.045 0.93 6 -1 7 112.28 151.29 2.44 0.070 0.86 6 0 5 1088.63 957.83 2.43 0.176 1.00 -2 1 4 812.51 887.00 2.43 0.169 2.17 2 -1 8 1005.19 908.52 2.43 0.171 1.06 7 -5 0 1199.64 1070.45 2.42 0.186 0.91 -1 8 4 77.69 50.12 2.42 0.040 0.85 5 8 1 64.15 101.71 2.40 0.057 0.78 2 -4 8 587.35 512.93 2.40 0.128 0.92 0 6 8 1302.48 1152.30 2.40 0.193 0.84 5 0 3 2706.53 2906.75 2.40 0.306 1.34 1 -1 1 2123.05 2262.97 2.38 0.270 4.43 -2 -4 3 1221.48 1126.31 2.37 0.190 1.53 5 7 4 46.34 84.40 2.36 0.052 0.79 5 -1 4 517.79 580.75 2.35 0.137 1.21 Bond lengths and angles C2 - Distance Angles O2 1.2948 (0.0039) N1 1.3199 (0.0041) 116.98 (0.29) C3 1.4760 (0.0045) 120.12 (0.31) 122.87 (0.31) C2 - O2 N1 C3 - Distance Angles C2 1.4760 (0.0045) C4 1.5200 (0.0052) 110.53 (0.36) C3 - C2 C4 - Distance Angles C5 1.5099 (0.0053) C3 1.5200 (0.0052) 109.68 (0.31) C4 - C5 C5 - Distance Angles C6 1.5018 (0.0046) C4 1.5099 (0.0053) 113.20 (0.39) C5 - C6 C6 - Distance Angles O6 1.1998 (0.0037) N1 1.4380 (0.0037) 118.41 (0.28) C5 1.5018 (0.0046) 125.79 (0.30) 115.70 (0.29) C6 - O6 N1 C7 - Distance Angles N1 1.4840 (0.0035) Si1 1.8810 (0.0029) 103.13 (0.18) C7 - N1 C8 - Distance Angles Si1 1.8367 (0.0089) C8 - C9 - Distance Angles Si1 1.8241 (0.0095) C9 - N1 - Distance Angles C2 1.3199 (0.0041) C6 1.4380 (0.0037) 123.32 (0.27) C7 1.4840 (0.0035) 116.65 (0.25) 120.03 (0.24) N1 - C2 C6 O2 - Distance Angles C2 1.2948 (0.0039) Si1 1.7790 (0.0024) 113.69 (0.21) O2 - C2 O6 - Distance Angles C6 1.1998 (0.0037) O6 - Si1 - Distance Angles O2 1.7790 (0.0024) C9 1.8241 (0.0095) 103.47 (0.43) C8 1.8367 (0.0089) 103.51 (0.43) 118.13 (0.16) C7 1.8810 (0.0029) 89.55 (0.11) 115.29 (0.60) 119.47 (0.56) Si1 - O2 C9 C8 FMAP and GRID set by program FMAP 2 2 20 GRID -2.941 -2 -2 2.941 2 2 R1 = 0.0230 for 1429 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.51 at 0.2291 0.3015 0.2824 [ 0.69 A from N1 ] Deepest hole -0.42 at 0.2585 0.3013 0.3659 [ 0.98 A from C6 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 1704 / 16868 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.2291 0.3015 0.2824 1.00000 0.05 0.51 0.69 N1 0.76 C6 1.72 O6 1.77 C2 Q2 1 1.1145 0.2889 0.2082 1.00000 0.05 0.40 0.56 N1 0.93 C7 1.53 H7A 1.61 H7B Q3 1 0.8384 0.3051 0.3662 1.00000 0.05 0.39 0.76 O2 1.92 C2 2.14 SI1 2.51 H3A Q4 1 1.5598 0.3006 0.3456 1.00000 0.05 0.38 1.25 H5A 1.76 C5 1.86 O6 1.97 C6 Q5 1 1.2375 0.2962 0.5203 1.00000 0.05 0.35 0.76 C4 0.79 C3 1.42 H3A 1.48 H4A Q6 1 1.3427 0.2733 0.3785 1.00000 0.05 0.35 0.74 C5 0.83 C6 1.38 H5B 1.55 H5A Q7 1 1.1033 0.3093 0.3067 1.00000 0.05 0.35 0.60 N1 0.76 C2 1.72 O2 1.77 C7 Q8 1 1.4789 0.2978 0.2276 1.00000 0.05 0.34 0.81 O6 1.59 C6 2.17 H9A 2.19 H5A Q9 1 1.2372 -0.2038 0.4063 1.00000 0.05 0.32 1.49 I1 2.21 H5A 2.60 H4A 2.74 H3B Q10 1 1.0308 -0.1903 0.2299 1.00000 0.05 0.32 1.31 I1 2.27 H3B 2.40 H9C 2.41 H8A Shortest distances between peaks (including symmetry equivalents) 2 7 0.99 1 2 1.07 1 7 1.14 4 8 1.19 1 6 1.19 5 6 1.80 4 6 1.94 6 7 2.00 6 8 2.06 5 7 2.12 9 10 2.14 2 6 2.23 1 5 2.28 1 8 2.29 3 4 2.31 3 9 2.42 3 7 2.43 4 9 2.61 1 4 2.72 2 5 2.96 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.02: Analyse other restraints etc. 0.39: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.55: Structure factors and derivatives 0.64: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.11: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0169 finished at 15:33:13 Total CPU time: 2.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++