+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 11:40:24 on 03-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SOT104 in P-1 CELL 0.71073 7.9703 12.1281 14.1205 79.138 83.059 77.293 ZERR 2.00 0.0016 0.0024 0.0028 0.030 0.030 0.030 LATT 1 SFAC C H N O SI UNIT 54 72 4 12 2 V = 1303.17 F(000) = 548.0 Mu = 0.13 mm-1 Cell Wt = 1025.34 Rho = 1.307 MERG 2 FMAP 2 PLAN 10 BOND $H OMIT -3 55 EXTI OMIT -1 0 1 OMIT 4 2 1 SIZE 0.38 0.14 0.06 TEMP -153 WGHT 0.07020 0.52560 L.S. 4 FVAR 0.80189 MOLE 1 C1 1 0.191115 0.817764 0.240288 11.00000 0.01453 0.01664 = 0.01917 -0.00231 -0.00476 -0.00245 C2 1 0.317180 0.709173 0.288245 11.00000 0.01754 0.01687 = 0.02179 -0.00304 -0.00518 -0.00378 AFIX 13 H2 2 0.408374 0.732277 0.316009 11.00000 -1.20000 AFIX 0 C3 1 0.043945 0.676948 0.339045 11.00000 0.01775 0.01868 = 0.02359 -0.00252 -0.00272 -0.00493 AFIX 13 H3 2 0.028825 0.636723 0.287618 11.00000 -1.20000 AFIX 0 C4 1 0.018902 0.805953 0.301050 11.00000 0.01488 0.01817 = 0.02172 -0.00112 -0.00318 -0.00221 AFIX 23 H4A 2 0.000179 0.849274 0.353870 11.00000 -1.20000 H4B 2 -0.077947 0.831983 0.261323 11.00000 -1.20000 AFIX 0 C5 1 0.344061 0.697912 0.121612 11.00000 0.01698 0.02038 = 0.02236 -0.00492 -0.00293 -0.00422 AFIX 13 H5 2 0.438792 0.732791 0.087099 11.00000 -1.20000 AFIX 0 C6 1 0.184918 0.792055 0.137338 11.00000 0.01787 0.01676 = 0.02027 -0.00365 -0.00474 -0.00336 AFIX 23 H6A 2 0.080003 0.765855 0.132946 11.00000 -1.20000 H6B 2 0.188936 0.860217 0.089211 11.00000 -1.20000 AFIX 0 C7 1 -0.078645 0.650010 0.425902 11.00000 0.02453 0.01564 = 0.02438 -0.00199 -0.00146 -0.00524 C8 1 -0.042585 0.652569 0.519742 11.00000 0.02670 0.02047 = 0.02672 -0.00071 -0.00470 -0.00837 AFIX 43 H8 2 0.066250 0.660667 0.531102 11.00000 -1.20000 AFIX 0 C9 1 -0.168314 0.643090 0.595955 11.00000 0.03496 0.02006 = 0.02327 0.00017 -0.00486 -0.00820 AFIX 43 H9 2 -0.145311 0.645334 0.658507 11.00000 -1.20000 AFIX 0 C10 1 -0.329267 0.630179 0.577201 11.00000 0.02825 0.01849 = 0.02355 0.00260 0.00232 -0.00611 C11 1 -0.366262 0.621823 0.486063 11.00000 0.02453 0.02625 = 0.02708 0.00238 -0.00277 -0.00894 AFIX 43 H11 2 -0.473513 0.609983 0.475703 11.00000 -1.20000 AFIX 0 C12 1 -0.239373 0.631545 0.410447 11.00000 0.02521 0.02621 = 0.02178 -0.00129 -0.00286 -0.00827 AFIX 43 H12 2 -0.261531 0.625699 0.348605 11.00000 -1.20000 AFIX 0 C13 1 0.308256 0.611809 0.066004 11.00000 0.01287 0.01867 = 0.02203 -0.00537 -0.00127 -0.00182 C14 1 0.336328 0.627532 -0.034551 11.00000 0.01653 0.01896 = 0.02254 -0.00206 0.00007 -0.00451 AFIX 43 H14 2 0.384143 0.688923 -0.067169 11.00000 -1.20000 AFIX 0 C15 1 0.293701 0.552523 -0.086705 11.00000 0.01818 0.02613 = 0.01873 -0.00575 -0.00007 -0.00358 AFIX 43 H15 2 0.310174 0.563550 -0.153889 11.00000 -1.20000 AFIX 0 C16 1 0.225964 0.460920 -0.035408 11.00000 0.01273 0.02018 = 0.02848 -0.00976 -0.00326 -0.00119 C17 1 0.199201 0.441575 0.064593 11.00000 0.01581 0.01846 = 0.02816 -0.00220 -0.00157 -0.00458 AFIX 43 H17 2 0.155067 0.378582 0.097069 11.00000 -1.20000 AFIX 0 C18 1 0.239751 0.518266 0.114892 11.00000 0.01726 0.01971 = 0.01948 -0.00120 -0.00034 -0.00407 AFIX 43 H18 2 0.221194 0.507421 0.182003 11.00000 -1.20000 AFIX 0 C19 1 0.436679 0.979964 0.145239 11.00000 0.01943 0.02063 = 0.02828 -0.00505 -0.00285 -0.00743 AFIX 13 H19 2 0.404466 0.957696 0.087787 11.00000 -1.20000 AFIX 0 C20 1 0.608558 0.900329 0.170590 11.00000 0.01944 0.03003 = 0.05117 -0.00722 -0.00155 -0.00415 AFIX 137 H20A 2 0.692046 0.906566 0.115859 11.00000 -1.50000 H20B 2 0.592544 0.822639 0.187309 11.00000 -1.50000 H20C 2 0.648863 0.921845 0.224499 11.00000 -1.50000 AFIX 0 C21 1 0.464423 1.103688 0.114720 11.00000 0.03031 0.02509 = 0.03808 -0.00429 0.00282 -0.01281 AFIX 137 H21A 2 0.488437 1.131294 0.170032 11.00000 -1.50000 H21B 2 0.362160 1.151671 0.088652 11.00000 -1.50000 H21C 2 0.559990 1.105326 0.066428 11.00000 -1.50000 AFIX 0 C22 1 0.069835 1.086057 0.213553 11.00000 0.02508 0.01709 = 0.03498 -0.00105 -0.00027 -0.00058 AFIX 13 H22 2 0.120096 1.154582 0.203941 11.00000 -1.20000 AFIX 0 C23 1 0.000351 1.086920 0.116376 11.00000 0.02569 0.02607 = 0.04224 0.00438 -0.01047 0.00002 AFIX 137 H23A 2 -0.054877 1.022928 0.121831 11.00000 -1.50000 H23B 2 0.094217 1.081412 0.066896 11.00000 -1.50000 H23C 2 -0.081658 1.156959 0.099744 11.00000 -1.50000 AFIX 0 C24 1 -0.079815 1.104522 0.292126 11.00000 0.03681 0.02997 = 0.05378 -0.00528 0.01248 0.00510 AFIX 137 H24A 2 -0.157122 1.175898 0.272579 11.00000 -1.50000 H24B 2 -0.034936 1.106330 0.351796 11.00000 -1.50000 H24C 2 -0.140902 1.042876 0.301103 11.00000 -1.50000 AFIX 0 C25 1 0.341371 0.954917 0.364936 11.00000 0.04767 0.02539 = 0.02767 -0.00423 -0.00918 -0.01340 AFIX 13 H25 2 0.459248 0.909433 0.361514 11.00000 -1.20000 AFIX 0 C26 1 0.358008 1.074376 0.379174 11.00000 0.09434 0.03096 = 0.03496 -0.00509 -0.02238 -0.02713 AFIX 137 H26A 2 0.247695 1.125600 0.374518 11.00000 -1.50000 H26B 2 0.439628 1.102750 0.330091 11.00000 -1.50000 H26C 2 0.397103 1.069463 0.441815 11.00000 -1.50000 AFIX 0 C27 1 0.248332 0.898153 0.454629 11.00000 0.05093 0.04195 = 0.02675 -0.00588 -0.00576 -0.01608 AFIX 137 H27A 2 0.306529 0.897723 0.510424 11.00000 -1.50000 H27B 2 0.247848 0.820778 0.448339 11.00000 -1.50000 H27C 2 0.131683 0.940001 0.461940 11.00000 -1.50000 AFIX 0 N1 3 -0.468233 0.629338 0.656010 11.00000 0.03530 0.02612 = 0.02378 0.00493 0.00327 -0.00720 N2 3 0.179369 0.380741 -0.088655 11.00000 0.01612 0.03116 = 0.03646 -0.01663 -0.00323 -0.00303 O1 4 0.221040 0.646982 0.361942 11.00000 0.01892 0.01910 = 0.02960 0.00430 -0.00497 -0.00311 O2 4 0.390508 0.641560 0.216346 11.00000 0.02477 0.02375 = 0.02401 -0.00835 -0.01046 0.00650 O3 4 -0.446562 0.659846 0.730973 11.00000 0.04960 0.03514 = 0.02215 0.00010 0.00516 -0.01045 O4 4 -0.600612 0.600449 0.642648 11.00000 0.03423 0.06462 = 0.03639 -0.00079 0.00579 -0.02034 O5 4 0.179509 0.406021 -0.176625 11.00000 0.03268 0.05662 = 0.03355 -0.02331 0.00163 -0.01642 O6 4 0.140809 0.291971 -0.042071 11.00000 0.03927 0.02354 = 0.05687 -0.01014 -0.01603 -0.01053 SI1 5 0.255484 0.960414 0.243388 11.00000 0.01936 0.01432 = 0.01945 -0.00248 -0.00408 -0.00325 HKLF 4 Covalent radii and connectivity table for 01SOT104 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 C1 - C4 C6 C2 Si1 C2 - O2 O1 C1 C3 - O1 C7 C4 C4 - C3 C1 C5 - O2 C13 C6 C6 - C5 C1 C7 - C8 C12 C3 C8 - C9 C7 C9 - C8 C10 C10 - C11 C9 N1 C11 - C10 C12 C12 - C11 C7 C13 - C14 C18 C5 C14 - C15 C13 C15 - C16 C14 C16 - C15 C17 N2 C17 - C18 C16 C18 - C17 C13 C19 - C20 C21 Si1 C20 - C19 C21 - C19 C22 - C24 C23 Si1 C23 - C22 C24 - C22 C25 - C27 C26 Si1 C26 - C25 C27 - C25 N1 - O3 O4 C10 N2 - O5 O6 C16 O1 - C2 C3 O2 - C2 C5 O3 - N1 O4 - N1 O5 - N2 O6 - N2 Si1 - C19 C22 C25 C1 19908 Reflections read, of which 4 rejected -10 =< h =< 10, -15 =< k =< 15, -18 =< l =< 18, 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) 4 1 0 146.87 0.57 3 307.12 3 2 0 193.56 2.23 7 15.66 -6 -2 1 13.49 0.59 3 6.51 6 0 1 65.31 0.77 4 21.00 6 7 1 22.15 0.69 3 7.93 2 1 2 442.15 0.92 4 381.33 2 2 2 741.50 7.89 6 67.86 3 1 3 490.82 4.62 3 235.61 6 8 3 839.16 6.61 5 187.72 6 8 4 341.13 3.61 6 45.07 6 0 5 86.48 1.35 3 36.98 4 2 5 535.58 9.19 5 53.80 4 3 5 39.83 0.43 4 11.91 5 2 6 9.94 0.49 4 2.68 5 3 7 43.08 1.53 3 9.14 5 4 7 552.92 8.77 5 65.08 6 5 9 98.74 0.67 4 43.80 6 6 9 10.75 0.83 3 4.47 18 Inconsistent equivalents 5893 Unique reflections, of which 0 suppressed R(int) = 0.0503 R(sigma) = 0.0432 Friedel opposites merged Maximum memory for data reduction = 3477 / 59295 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 = 4451 / 419263 wR2 = 0.1286 before cycle 1 for 5893 data and 332 / 332 parameters GooF = S = 1.028; Restrained GooF = 1.028 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0702 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80530 0.00178 1.918 OSF 2 0.00532 0.00356 1.495 EXTI Mean shift/esd = 0.282 Maximum = 1.918 for OSF Max. shift = 0.006 A for H21C Max. dU = 0.001 for C27 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4451 / 419263 wR2 = 0.1278 before cycle 2 for 5893 data and 332 / 332 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0702 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80651 0.00178 0.682 OSF 2 0.00742 0.00372 0.565 EXTI Mean shift/esd = 0.108 Maximum = 0.682 for OSF Max. shift = 0.002 A for H21C Max. dU = 0.000 for C27 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4451 / 419263 wR2 = 0.1277 before cycle 3 for 5893 data and 332 / 332 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0702 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80663 0.00179 0.065 OSF 2 0.00749 0.00378 0.018 EXTI Mean shift/esd = 0.010 Maximum = 0.128 for U11 C27 Max. shift = 0.000 A for H27A Max. dU = 0.000 for C27 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4451 / 419263 wR2 = 0.1277 before cycle 4 for 5893 data and 332 / 332 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0702 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80664 0.00179 0.008 OSF 2 0.00750 0.00378 0.003 EXTI Mean shift/esd = 0.002 Maximum = 0.023 for U11 C27 Max. shift = 0.000 A for H27A Max. dU = 0.000 for C27 Largest correlation matrix elements 0.552 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.4103 0.7328 0.3165 13 1.000 0.000 C2 O2 O1 C1 H3 0.0284 0.6360 0.2865 13 1.000 0.000 C3 O1 C7 C4 H4A -0.0001 0.8502 0.3550 23 0.990 0.000 C4 C3 C1 H4B -0.0799 0.8326 0.2605 23 0.990 0.000 C4 C3 C1 H5 0.4407 0.7335 0.0864 13 1.000 0.000 C5 O2 C13 C6 H6A 0.0779 0.7654 0.1329 23 0.990 0.000 C6 C5 C1 H6B 0.1891 0.8616 0.0883 23 0.990 0.000 C6 C5 C1 H8 0.0686 0.6608 0.5314 43 0.950 0.000 C8 C9 C7 H9 -0.1450 0.6453 0.6598 43 0.950 0.000 C9 C8 C10 H11 -0.4757 0.6096 0.4754 43 0.950 0.000 C11 C10 C12 H12 -0.2618 0.6256 0.3473 43 0.950 0.000 C12 C11 C7 H14 0.3850 0.6903 -0.0678 43 0.950 0.000 C14 C15 C13 H15 0.3106 0.5638 -0.1553 43 0.950 0.000 C15 C16 C14 H17 0.1542 0.3773 0.0976 43 0.950 0.000 C17 C18 C16 H18 0.2209 0.5071 0.1834 43 0.950 0.000 C18 C17 C13 H19 0.4038 0.9572 0.0867 13 1.000 0.000 C19 C20 C21 Si1 H20A 0.6937 0.9067 0.1148 137 0.980 0.000 C20 C19 H20A H20B 0.5922 0.8210 0.1877 137 0.980 0.000 C20 C19 H20A H20C 0.6497 0.9223 0.2257 137 0.980 0.000 C20 C19 H20A H21A 0.4881 1.1320 0.1713 137 0.980 0.000 C21 C19 H21A H21B 0.3605 1.1525 0.0876 137 0.980 0.000 C21 C19 H21A H21C 0.5627 1.1051 0.0659 137 0.980 0.000 C21 C19 H21A H22 0.1213 1.1559 0.2038 13 1.000 0.000 C22 C24 C23 Si1 H23A -0.0558 1.0214 0.1220 137 0.980 0.000 C23 C22 H23A H23B 0.0960 1.0815 0.0659 137 0.980 0.000 C23 C22 H23A H23C -0.0837 1.1583 0.0996 137 0.980 0.000 C23 C22 H23A H24A -0.1589 1.1773 0.2721 137 0.980 0.000 C24 C22 H24A H24B -0.0342 1.1065 0.3531 137 0.980 0.000 C24 C22 H24A H24C -0.1421 1.0415 0.3014 137 0.980 0.000 C24 C22 H24A H25 0.4612 0.9087 0.3614 13 1.000 0.000 C25 C27 C26 Si1 H26A 0.2453 1.1268 0.3745 137 0.980 0.000 C26 C25 H26A H26B 0.4411 1.1033 0.3290 137 0.980 0.000 C26 C25 H26A H26C 0.3981 1.0693 0.4431 137 0.980 0.000 C26 C25 H26A H27A 0.3084 0.8976 0.5115 137 0.980 0.000 C27 C25 H27A H27B 0.2483 0.8191 0.4482 137 0.980 0.000 C27 C25 H27A H27C 0.1295 0.9406 0.4624 137 0.980 0.000 C27 C25 H27A 01SOT104 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.19127 0.81773 0.24030 1.00000 0.01485 0.01683 0.01918 -0.00229 -0.00468 -0.00238 0.01690 0.00207 0.00018 0.00012 0.00010 0.00000 0.00066 0.00068 0.00072 0.00054 0.00053 0.00053 0.00029 C2 0.31726 0.70920 0.28815 1.00000 0.01778 0.01694 0.02202 -0.00313 -0.00486 -0.00407 0.01857 0.00215 0.00019 0.00012 0.00011 0.00000 0.00069 0.00070 0.00075 0.00056 0.00056 0.00055 0.00031 H2 0.41034 0.73276 0.31647 1.00000 0.02229 0.00000 0.00000 C3 0.04386 0.67705 0.33902 1.00000 0.01779 0.01884 0.02441 -0.00279 -0.00340 -0.00476 0.02015 0.00223 0.00019 0.00013 0.00011 0.00000 0.00070 0.00073 0.00078 0.00058 0.00058 0.00056 0.00031 H3 0.02837 0.63604 0.28653 1.00000 0.02418 0.00000 0.00000 C4 0.01894 0.80596 0.30108 1.00000 0.01523 0.01829 0.02255 -0.00113 -0.00336 -0.00237 0.01901 0.00222 0.00018 0.00012 0.00011 0.00000 0.00068 0.00072 0.00075 0.00057 0.00055 0.00054 0.00031 H4A -0.00013 0.85015 0.35501 1.00000 0.02281 0.00000 0.00000 H4B -0.07990 0.83258 0.26053 1.00000 0.02281 0.00000 0.00000 C5 0.34403 0.69788 0.12162 1.00000 0.01745 0.02071 0.02242 -0.00482 -0.00291 -0.00424 0.01986 0.00217 0.00019 0.00013 0.00011 0.00000 0.00069 0.00074 0.00077 0.00059 0.00056 0.00056 0.00031 H5 0.44069 0.73347 0.08640 1.00000 0.02384 0.00000 0.00000 C6 0.18500 0.79205 0.13737 1.00000 0.01806 0.01669 0.02117 -0.00318 -0.00480 -0.00349 0.01837 0.00211 0.00019 0.00012 0.00011 0.00000 0.00069 0.00069 0.00074 0.00056 0.00055 0.00055 0.00030 H6A 0.07788 0.76535 0.13290 1.00000 0.02205 0.00000 0.00000 H6B 0.18914 0.86161 0.08825 1.00000 0.02205 0.00000 0.00000 C7 -0.07873 0.65004 0.42593 1.00000 0.02494 0.01502 0.02495 -0.00205 -0.00150 -0.00507 0.02169 0.00231 0.00020 0.00013 0.00011 0.00000 0.00078 0.00070 0.00080 0.00058 0.00061 0.00058 0.00032 C8 -0.04256 0.65256 0.51978 1.00000 0.02771 0.02003 0.02695 -0.00066 -0.00469 -0.00843 0.02456 0.00237 0.00022 0.00013 0.00012 0.00000 0.00082 0.00077 0.00084 0.00062 0.00064 0.00063 0.00034 H8 0.06861 0.66080 0.53143 1.00000 0.02947 0.00000 0.00000 C9 -0.16844 0.64306 0.59587 1.00000 0.03584 0.01981 0.02294 0.00029 -0.00494 -0.00837 0.02607 0.00243 0.00022 0.00013 0.00012 0.00000 0.00091 0.00077 0.00081 0.00061 0.00066 0.00066 0.00035 H9 -0.14501 0.64530 0.65979 1.00000 0.03129 0.00000 0.00000 C10 -0.32926 0.63023 0.57713 1.00000 0.02881 0.01808 0.02404 0.00265 0.00214 -0.00594 0.02465 0.00252 0.00021 0.00013 0.00012 0.00000 0.00083 0.00074 0.00082 0.00060 0.00064 0.00061 0.00034 C11 -0.36624 0.62176 0.48604 1.00000 0.02465 0.02534 0.02742 0.00235 -0.00288 -0.00862 0.02608 0.00254 0.00021 0.00014 0.00012 0.00000 0.00080 0.00082 0.00085 0.00065 0.00064 0.00064 0.00035 H11 -0.47573 0.60957 0.47545 1.00000 0.03130 0.00000 0.00000 C12 -0.23926 0.63155 0.41051 1.00000 0.02585 0.02607 0.02194 -0.00118 -0.00302 -0.00802 0.02448 0.00242 0.00021 0.00014 0.00012 0.00000 0.00081 0.00081 0.00080 0.00062 0.00062 0.00063 0.00034 H12 -0.26182 0.62558 0.34733 1.00000 0.02937 0.00000 0.00000 C13 0.30829 0.61183 0.06597 1.00000 0.01269 0.01873 0.02224 -0.00493 -0.00145 -0.00173 0.01791 0.00215 0.00018 0.00013 0.00011 0.00000 0.00064 0.00070 0.00075 0.00057 0.00053 0.00052 0.00030 C14 0.33627 0.62753 -0.03453 1.00000 0.01674 0.01845 0.02303 -0.00176 -0.00006 -0.00417 0.01967 0.00223 0.00018 0.00013 0.00011 0.00000 0.00069 0.00071 0.00077 0.00058 0.00056 0.00055 0.00031 H14 0.38504 0.69026 -0.06785 1.00000 0.02361 0.00000 0.00000 C15 0.29371 0.55254 -0.08670 1.00000 0.01760 0.02626 0.01883 -0.00546 -0.00017 -0.00312 0.02099 0.00228 0.00019 0.00014 0.00011 0.00000 0.00070 0.00079 0.00073 0.00060 0.00055 0.00059 0.00032 H15 0.31055 0.56378 -0.15533 1.00000 0.02519 0.00000 0.00000 C16 0.22599 0.46094 -0.03533 1.00000 0.01243 0.02011 0.02933 -0.00998 -0.00341 -0.00091 0.02008 0.00216 0.00018 0.00013 0.00011 0.00000 0.00064 0.00074 0.00083 0.00061 0.00056 0.00054 0.00032 C17 0.19931 0.44168 0.06449 1.00000 0.01579 0.01820 0.02824 -0.00196 -0.00150 -0.00417 0.02091 0.00227 0.00019 0.00013 0.00011 0.00000 0.00069 0.00072 0.00082 0.00060 0.00058 0.00055 0.00032 H17 0.15420 0.37734 0.09765 1.00000 0.02510 0.00000 0.00000 C18 0.23984 0.51823 0.11482 1.00000 0.01731 0.01992 0.01977 -0.00112 -0.00042 -0.00351 0.01943 0.00226 0.00019 0.00013 0.00011 0.00000 0.00069 0.00073 0.00073 0.00057 0.00055 0.00056 0.00031 H18 0.22093 0.50707 0.18338 1.00000 0.02331 0.00000 0.00000 C19 0.43667 0.97993 0.14535 1.00000 0.01974 0.02064 0.02891 -0.00504 -0.00298 -0.00739 0.02238 0.00227 0.00020 0.00013 0.00012 0.00000 0.00073 0.00075 0.00084 0.00062 0.00061 0.00059 0.00033 H19 0.40384 0.95720 0.08672 1.00000 0.02686 0.00000 0.00000 C20 0.60853 0.90035 0.17067 1.00000 0.02022 0.02964 0.05191 -0.00706 -0.00181 -0.00404 0.03415 0.00284 0.00022 0.00016 0.00015 0.00000 0.00081 0.00092 0.00116 0.00081 0.00075 0.00068 0.00041 H20A 0.69374 0.90674 0.11479 1.00000 0.05122 0.00000 0.00000 H20B 0.59223 0.82104 0.18774 1.00000 0.05122 0.00000 0.00000 H20C 0.64969 0.92233 0.22570 1.00000 0.05122 0.00000 0.00000 C21 0.46453 1.10360 0.11479 1.00000 0.03013 0.02517 0.03845 -0.00392 0.00264 -0.01246 0.03082 0.00267 0.00023 0.00015 0.00014 0.00000 0.00089 0.00085 0.00100 0.00072 0.00073 0.00069 0.00039 H21A 0.48809 1.13203 0.17135 1.00000 0.04623 0.00000 0.00000 H21B 0.36053 1.15248 0.08765 1.00000 0.04623 0.00000 0.00000 H21C 0.56272 1.10511 0.06590 1.00000 0.04623 0.00000 0.00000 C22 0.06998 1.08596 0.21359 1.00000 0.02564 0.01725 0.03513 -0.00092 -0.00003 -0.00057 0.02727 0.00263 0.00021 0.00014 0.00013 0.00000 0.00081 0.00075 0.00094 0.00065 0.00068 0.00061 0.00036 H22 0.12127 1.15588 0.20377 1.00000 0.03272 0.00000 0.00000 C23 0.00029 1.08686 0.11646 1.00000 0.02597 0.02594 0.04298 0.00450 -0.01050 0.00016 0.03320 0.00281 0.00023 0.00015 0.00014 0.00000 0.00085 0.00087 0.00106 0.00075 0.00075 0.00068 0.00041 H23A -0.05581 1.02141 0.12200 1.00000 0.04980 0.00000 0.00000 H23B 0.09597 1.08148 0.06586 1.00000 0.04980 0.00000 0.00000 H23C -0.08370 1.15827 0.09963 1.00000 0.04980 0.00000 0.00000 C24 -0.07987 1.10447 0.29217 1.00000 0.03658 0.03068 0.05463 -0.00469 0.01198 0.00555 0.04423 0.00367 0.00026 0.00017 0.00016 0.00000 0.00104 0.00100 0.00130 0.00090 0.00091 0.00080 0.00051 H24A -0.15889 1.17726 0.27212 1.00000 0.06634 0.00000 0.00000 H24B -0.03415 1.10650 0.35307 1.00000 0.06634 0.00000 0.00000 H24C -0.14208 1.04146 0.30142 1.00000 0.06634 0.00000 0.00000 C25 0.34087 0.95501 0.36494 1.00000 0.04976 0.02526 0.02822 -0.00411 -0.00944 -0.01401 0.03293 0.00251 0.00027 0.00015 0.00013 0.00000 0.00111 0.00087 0.00091 0.00069 0.00078 0.00078 0.00041 H25 0.46120 0.90866 0.36137 1.00000 0.03952 0.00000 0.00000 C26 0.35789 1.07440 0.37917 1.00000 0.09444 0.03200 0.03508 -0.00568 -0.02184 -0.02761 0.05011 0.00284 0.00036 0.00017 0.00015 0.00000 0.00183 0.00105 0.00109 0.00084 0.00110 0.00112 0.00060 H26A 0.24534 1.12678 0.37455 1.00000 0.07517 0.00000 0.00000 H26B 0.44113 1.10332 0.32899 1.00000 0.07517 0.00000 0.00000 H26C 0.39806 1.06929 0.44307 1.00000 0.07517 0.00000 0.00000 C27 0.24865 0.89806 0.45464 1.00000 0.05340 0.04248 0.02743 -0.00597 -0.00629 -0.01680 0.03972 0.00286 0.00029 0.00018 0.00013 0.00000 0.00121 0.00110 0.00095 0.00080 0.00083 0.00092 0.00046 H27A 0.30839 0.89764 0.51147 1.00000 0.05959 0.00000 0.00000 H27B 0.24833 0.81906 0.44819 1.00000 0.05959 0.00000 0.00000 H27C 0.12951 0.94060 0.46235 1.00000 0.05959 0.00000 0.00000 N1 -0.46821 0.62935 0.65594 1.00000 0.03562 0.02591 0.02431 0.00515 0.00273 -0.00733 0.03013 0.00235 0.00020 0.00012 0.00010 0.00000 0.00083 0.00074 0.00076 0.00058 0.00059 0.00061 0.00034 N2 0.17936 0.38074 -0.08868 1.00000 0.01636 0.03140 0.03677 -0.01644 -0.00330 -0.00296 0.02694 0.00200 0.00017 0.00012 0.00011 0.00000 0.00063 0.00078 0.00084 0.00064 0.00055 0.00054 0.00032 O1 0.22103 0.64699 0.36191 1.00000 0.01947 0.01925 0.02985 0.00438 -0.00510 -0.00323 0.02383 0.00167 0.00014 0.00009 0.00008 0.00000 0.00054 0.00054 0.00062 0.00044 0.00044 0.00042 0.00026 O2 0.39047 0.64166 0.21635 1.00000 0.02489 0.02391 0.02449 -0.00817 -0.01062 0.00657 0.02496 0.00163 0.00014 0.00010 0.00008 0.00000 0.00057 0.00058 0.00059 0.00045 0.00045 0.00044 0.00026 O3 -0.44662 0.65988 0.73097 1.00000 0.05011 0.03507 0.02240 -0.00009 0.00507 -0.01054 0.03687 0.00204 0.00018 0.00011 0.00009 0.00000 0.00082 0.00072 0.00064 0.00052 0.00055 0.00060 0.00032 O4 -0.60067 0.60044 0.64261 1.00000 0.03457 0.06489 0.03682 -0.00075 0.00551 -0.02039 0.04556 0.00225 0.00018 0.00014 0.00010 0.00000 0.00076 0.00100 0.00078 0.00068 0.00058 0.00069 0.00037 O5 0.17938 0.40609 -0.17666 1.00000 0.03342 0.05679 0.03364 -0.02329 0.00155 -0.01632 0.03842 0.00182 0.00017 0.00013 0.00010 0.00000 0.00069 0.00089 0.00074 0.00064 0.00054 0.00062 0.00033 O6 0.14076 0.29202 -0.04211 1.00000 0.03933 0.02365 0.05836 -0.01005 -0.01625 -0.01046 0.03834 0.00180 0.00017 0.00011 0.00011 0.00000 0.00074 0.00064 0.00089 0.00059 0.00063 0.00054 0.00033 Si1 0.25547 0.96039 0.24340 1.00000 0.01973 0.01446 0.01982 -0.00249 -0.00414 -0.00336 0.01786 0.00058 0.00005 0.00003 0.00003 0.00000 0.00022 0.00021 0.00023 0.00015 0.00015 0.00015 0.00013 Final Structure Factor Calculation for 01SOT104 in P-1 Total number of l.s. parameters = 332 Maximum vector length = 511 Memory required = 4119 / 24017 wR2 = 0.1278 before cycle 5 for 5893 data and 0 / 332 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0702 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0450 for 4879 Fo > 4sig(Fo) and 0.0576 for all 5893 data wR2 = 0.1278, GooF = S = 1.020, Restrained GooF = 1.020 for all data Occupancy sum of asymmetric unit = 36.00 for non-hydrogen and 36.00 for hydrogen atoms Principal mean square atomic displacements U 0.0207 0.0172 0.0128 C1 0.0235 0.0172 0.0150 C2 0.0249 0.0191 0.0164 C3 0.0240 0.0186 0.0144 C4 0.0231 0.0201 0.0164 C5 0.0229 0.0168 0.0154 C6 0.0259 0.0246 0.0146 C7 0.0314 0.0247 0.0176 C8 0.0364 0.0244 0.0175 C9 0.0341 0.0259 0.0140 C10 0.0347 0.0246 0.0189 C11 0.0295 0.0231 0.0209 C12 0.0226 0.0186 0.0126 C13 0.0246 0.0184 0.0160 C14 0.0269 0.0196 0.0165 C15 0.0317 0.0164 0.0121 C16 0.0292 0.0182 0.0154 C17 0.0232 0.0183 0.0168 C18 0.0289 0.0230 0.0152 C19 0.0523 0.0299 0.0202 C20 0.0417 0.0324 0.0184 C21 0.0390 0.0265 0.0163 C22 0.0499 0.0326 0.0171 C23 0.0733 0.0387 0.0206 C24 0.0517 0.0270 0.0201 C25 0.0989 0.0339 0.0176 C26 0.0560 0.0374 0.0258 C27 0.0418 0.0330 0.0156 N1 0.0440 0.0209 0.0160 N2 0.0363 0.0201 0.0152 O1 0.0416 0.0194 0.0139 O2 0.0536 0.0376 0.0195 O3 0.0687 0.0448 0.0231 O4 0.0636 0.0304 0.0213 O5 0.0634 0.0347 0.0170 O6 0.0221 0.0171 0.0144 Si1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.032 0.049 0.067 0.087 0.109 0.135 0.178 0.252 1.000 Number in group 597. 591. 594. 581. 591. 602. 583. 584. 577. 593. GooF 0.874 1.073 1.092 1.099 1.118 1.000 1.020 1.009 0.982 0.906 K 1.421 1.045 1.020 1.004 0.986 0.990 0.999 1.008 1.024 1.006 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.65 inf Number in group 613. 565. 590. 592. 591. 592. 578. 593. 587. 592. GooF 0.925 0.913 0.854 0.904 0.899 0.908 0.837 0.993 1.221 1.533 K 1.015 1.026 1.010 1.020 1.019 1.016 1.012 1.009 1.017 0.998 R1 0.119 0.108 0.074 0.069 0.058 0.049 0.040 0.039 0.043 0.046 Recommended weighting scheme: WGHT 0.0623 0.5795 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 6 0 97.40 52.16 5.66 0.082 1.94 2 -2 3 155.99 96.00 5.19 0.111 2.47 -3 -2 2 408.02 278.29 4.80 0.190 2.29 -3 -3 3 34.36 65.65 4.66 0.092 1.98 3 8 3 17.93 6.03 4.40 0.028 1.42 -4 -1 7 14.11 3.28 4.33 0.021 1.32 0 -4 4 20.49 42.14 4.29 0.074 2.06 -2 -4 3 44.73 75.55 4.08 0.099 2.09 1 1 7 88.77 57.44 3.98 0.086 2.00 2 1 3 59.89 36.91 3.95 0.069 3.22 2 -1 6 370.32 270.19 3.93 0.187 1.94 2 -2 8 20.17 8.41 3.91 0.033 1.48 0 4 5 187.31 131.14 3.90 0.130 2.20 3 -4 3 40.58 22.43 3.88 0.054 1.62 -8 2 5 52.10 25.90 3.83 0.058 0.86 1 -4 3 16.00 32.48 3.80 0.065 2.13 3 -2 4 20.32 9.26 3.79 0.035 1.86 3 4 2 24.48 43.03 3.58 0.075 2.19 3 1 14 1.82 13.58 3.57 0.042 0.96 1 3 4 176.26 243.44 3.52 0.177 2.86 1 -4 2 76.24 50.96 3.51 0.081 2.32 0 -5 5 7.50 1.16 3.50 0.012 1.65 3 -3 2 258.26 192.27 3.44 0.158 1.89 -1 -1 8 46.21 28.76 3.38 0.061 1.61 4 0 3 93.92 65.06 3.38 0.092 1.84 3 0 5 2.12 8.81 3.38 0.034 1.97 3 6 0 370.96 283.50 3.38 0.191 1.73 1 -6 3 25.70 43.52 3.33 0.075 1.61 8 5 11 555.02 396.17 3.31 0.226 0.83 -1 3 1 140.72 194.62 3.29 0.159 3.21 2 -3 4 77.24 111.98 3.28 0.120 1.98 9 5 3 175.00 119.43 3.27 0.124 0.88 -6 -5 7 45.78 27.99 3.23 0.060 0.98 3 3 0 4.23 0.06 3.22 0.003 2.39 1 -1 5 17.90 31.61 3.21 0.064 2.48 -1 1 8 91.26 128.32 3.20 0.129 1.67 4 0 4 2.75 9.21 3.19 0.034 1.75 5 3 0 21.78 36.50 3.17 0.069 1.55 -1 0 3 168.81 225.83 3.17 0.171 3.82 1 -2 7 18.47 9.32 3.15 0.035 1.74 4 -6 2 15.64 29.19 3.15 0.061 1.22 -2 0 4 98.65 136.53 3.15 0.133 2.48 0 -2 8 11.95 24.44 3.11 0.056 1.59 -3 -1 2 47.86 31.61 3.10 0.064 2.37 1 -3 6 16.42 7.71 3.09 0.032 1.79 1 5 10 14.00 5.55 3.04 0.027 1.31 5 10 8 10.16 3.27 3.02 0.021 0.98 -2 0 3 3.74 0.38 3.02 0.007 2.85 5 -1 3 29.71 47.24 3.02 0.078 1.45 -3 -1 5 77.49 107.84 3.00 0.118 1.80 Bond lengths and angles C1 - Distance Angles C4 1.5488 (0.0020) C6 1.5515 (0.0020) 109.80 (0.12) C2 1.5635 (0.0021) 101.54 (0.12) 102.77 (0.12) Si1 1.9186 (0.0015) 112.28 (0.10) 114.81 (0.10) 114.49 (0.10) C1 - C4 C6 C2 C2 - Distance Angles O2 1.4138 (0.0019) O1 1.4169 (0.0019) 110.25 (0.12) C1 1.5635 (0.0021) 108.49 (0.12) 108.19 (0.12) H2 1.0000 109.96 109.96 109.96 C2 - O2 O1 C1 C3 - Distance Angles O1 1.4391 (0.0018) C7 1.5058 (0.0022) 112.24 (0.13) C4 1.5311 (0.0021) 102.82 (0.12) 112.14 (0.13) H3 1.0000 109.81 109.82 109.81 C3 - O1 C7 C4 C4 - Distance Angles C3 1.5311 (0.0021) C1 1.5488 (0.0020) 103.18 (0.12) H4A 0.9900 111.13 111.13 H4B 0.9900 111.13 111.13 109.08 C4 - C3 C1 H4A C5 - Distance Angles O2 1.4339 (0.0019) C13 1.5105 (0.0021) 109.71 (0.12) C6 1.5334 (0.0021) 105.91 (0.12) 112.50 (0.12) H5 1.0000 109.54 109.54 109.54 C5 - O2 C13 C6 C6 - Distance Angles C5 1.5334 (0.0021) C1 1.5515 (0.0020) 105.75 (0.12) H6A 0.9900 110.59 110.59 H6B 0.9900 110.59 110.59 108.73 C6 - C5 C1 H6A C7 - Distance Angles C8 1.3970 (0.0023) C12 1.3952 (0.0023) 119.40 (0.15) C3 1.5058 (0.0022) 122.13 (0.14) 118.25 (0.14) C7 - C8 C12 C8 - Distance Angles C9 1.3849 (0.0024) C7 1.3970 (0.0023) 120.13 (0.15) H8 0.9500 119.93 119.93 C8 - C9 C7 C9 - Distance Angles C8 1.3849 (0.0024) C10 1.3866 (0.0024) 118.84 (0.15) H9 0.9500 120.58 120.58 C9 - C8 C10 C10 - Distance Angles C11 1.3807 (0.0024) C9 1.3866 (0.0024) 122.36 (0.15) N1 1.4724 (0.0022) 118.33 (0.15) 119.28 (0.15) C10 - C11 C9 C11 - Distance Angles C10 1.3807 (0.0024) C12 1.3857 (0.0023) 118.17 (0.15) H11 0.9500 120.91 120.92 C11 - C10 C12 C12 - Distance Angles C11 1.3857 (0.0023) C7 1.3952 (0.0023) 120.95 (0.15) H12 0.9500 119.53 119.53 C12 - C11 C7 C13 - Distance Angles C14 1.3929 (0.0022) C18 1.3959 (0.0021) 119.40 (0.14) C5 1.5105 (0.0021) 120.52 (0.13) 120.02 (0.13) C13 - C14 C18 C14 - Distance Angles C15 1.3905 (0.0022) C13 1.3929 (0.0022) 120.84 (0.14) H14 0.9500 119.58 119.58 C14 - C15 C13 C15 - Distance Angles C16 1.3846 (0.0022) C14 1.3905 (0.0022) 117.81 (0.14) H15 0.9500 121.10 121.10 C15 - C16 C14 C16 - Distance Angles C15 1.3846 (0.0022) C17 1.3826 (0.0023) 122.86 (0.14) N2 1.4678 (0.0020) 118.90 (0.14) 118.24 (0.14) C16 - C15 C17 C17 - Distance Angles C18 1.3811 (0.0022) C16 1.3826 (0.0023) 118.40 (0.14) H17 0.9500 120.80 120.80 C17 - C18 C16 C18 - Distance Angles C17 1.3811 (0.0022) C13 1.3959 (0.0021) 120.67 (0.14) H18 0.9500 119.67 119.67 C18 - C17 C13 C19 - Distance Angles C20 1.5305 (0.0023) C21 1.5377 (0.0022) 109.23 (0.13) Si1 1.8980 (0.0017) 112.69 (0.12) 115.11 (0.12) H19 1.0000 106.40 106.40 106.40 C19 - C20 C21 Si1 C20 - Distance Angles C19 1.5305 (0.0023) H20A 0.9800 109.47 H20B 0.9800 109.47 109.47 H20C 0.9800 109.47 109.47 109.47 C20 - C19 H20A H20B C21 - Distance Angles C19 1.5377 (0.0022) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - C19 H21A H21B C22 - Distance Angles C24 1.5375 (0.0025) C23 1.5380 (0.0025) 110.25 (0.16) Si1 1.8975 (0.0018) 117.14 (0.13) 112.24 (0.12) H22 1.0000 105.39 105.39 105.39 C22 - C24 C23 Si1 C23 - Distance Angles C22 1.5380 (0.0025) H23A 0.9800 109.47 H23B 0.9800 109.47 109.47 H23C 0.9800 109.47 109.47 109.47 C23 - C22 H23A H23B C24 - Distance Angles C22 1.5375 (0.0025) H24A 0.9800 109.47 H24B 0.9800 109.47 109.47 H24C 0.9800 109.47 109.47 109.47 C24 - C22 H24A H24B C25 - Distance Angles C27 1.5134 (0.0027) C26 1.5356 (0.0024) 109.54 (0.17) Si1 1.9061 (0.0018) 117.65 (0.13) 111.40 (0.13) H25 1.0000 105.79 105.79 105.79 C25 - C27 C26 Si1 C26 - Distance Angles C25 1.5356 (0.0024) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C25 H26A H26B C27 - Distance Angles C25 1.5134 (0.0027) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C25 H27A H27B N1 - Distance Angles O3 1.2285 (0.0020) O4 1.2283 (0.0021) 123.48 (0.15) C10 1.4724 (0.0022) 118.06 (0.15) 118.44 (0.15) N1 - O3 O4 N2 - Distance Angles O5 1.2222 (0.0020) O6 1.2309 (0.0020) 123.60 (0.15) C16 1.4678 (0.0020) 118.33 (0.14) 118.07 (0.14) N2 - O5 O6 O1 - Distance Angles C2 1.4169 (0.0019) C3 1.4391 (0.0018) 107.52 (0.11) O1 - C2 O2 - Distance Angles C2 1.4138 (0.0019) C5 1.4339 (0.0019) 112.11 (0.11) O2 - C2 O3 - Distance Angles N1 1.2285 (0.0020) O3 - O4 - Distance Angles N1 1.2283 (0.0021) O4 - O5 - Distance Angles N2 1.2222 (0.0020) O5 - O6 - Distance Angles N2 1.2309 (0.0020) O6 - Si1 - Distance Angles C19 1.8980 (0.0017) C22 1.8975 (0.0018) 106.57 (0.08) C25 1.9061 (0.0018) 107.94 (0.08) 113.16 (0.09) C1 1.9186 (0.0015) 108.20 (0.07) 111.10 (0.07) 109.67 (0.07) Si1 - C19 C22 C25 FMAP and GRID set by program FMAP 2 1 21 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.0574 for 5893 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.67 at 0.2308 0.9766 0.3786 [ 0.87 A from C25 ] Deepest hole -0.37 at 0.2696 0.0220 0.2332 [ 0.76 A from SI1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 4079 / 27333 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2308 0.9766 0.3786 1.00000 0.05 0.67 0.87 C25 1.29 C27 1.40 H27C 1.72 C26 Q2 1 0.3680 0.8719 0.4421 1.00000 0.05 0.61 0.94 C27 1.10 H27A 1.25 H27B 1.34 C25 Q3 1 0.3445 0.9728 0.1796 1.00000 0.05 0.34 0.84 C19 1.09 SI1 1.37 H19 2.04 C21 Q4 1 0.3766 0.9768 0.1973 1.00000 0.05 0.33 0.83 C19 1.13 SI1 1.61 H19 1.90 C20 Q5 1 0.1903 0.8056 0.1958 1.00000 0.05 0.32 0.67 C1 0.88 C6 1.54 H6A 1.54 H6B Q6 1 0.2742 0.9574 0.3126 1.00000 0.05 0.31 0.95 C25 1.00 SI1 1.66 H25 2.00 C27 Q7 1 -0.0219 0.6612 0.3855 1.00000 0.05 0.31 0.70 C7 0.81 C3 1.48 H3 1.83 C12 Q8 1 0.1984 0.4601 0.0176 1.00000 0.05 0.28 0.66 C17 0.75 C16 1.43 H17 1.75 C18 Q9 1 -0.3914 0.6305 0.6033 1.00000 0.05 0.28 0.58 C10 0.90 N1 1.66 C11 1.79 O4 Q10 1 0.1246 1.0248 0.2386 1.00000 0.05 0.26 0.81 C22 1.16 SI1 1.57 H22 1.86 C24 Shortest distances between peaks (including symmetry equivalents) 3 4 0.39 1 6 1.01 6 10 1.65 1 2 1.68 4 6 1.73 3 10 1.88 3 6 1.88 4 10 2.01 2 6 2.06 1 10 2.17 3 5 2.55 1 4 2.68 5 10 2.76 4 5 2.81 1 3 2.85 5 6 2.92 Time profile in seconds ----------------------- 0.20: 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. 2.59: 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 2.64: Structure factors and derivatives 4.75: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.69: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.16: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.13: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 11:40:37 Total CPU time: 11.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++