+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0138 started at 15:55:22 on 26-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0138 in Pbca CELL 0.71073 11.8719 15.0801 15.5429 90.000 90.000 90.000 ZERR 8.00 0.0003 0.0003 0.0003 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O SI CL UNIT 104 120 16 16 8 8 V = 2782.64 F(000) = 1232.0 Mu = 0.36 mm-1 Cell Wt = 2358.48 Rho = 1.407 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.14 0.23 0.34 ACTA BOND $H WGHT 0.05660 1.18730 L.S. 4 TEMP -153.00 FVAR 0.40693 MOLE 1 C2 1 0.279738 -0.074689 0.675591 11.00000 0.02127 0.01834 = 0.02075 0.00128 0.00150 -0.00111 C3 1 0.268860 -0.128107 0.599419 11.00000 0.02672 0.01936 = 0.02529 0.00059 -0.00338 -0.00207 AFIX 43 H3 2 0.198892 -0.156099 0.587499 11.00000 -1.20000 AFIX 0 C4 1 0.355836 -0.139452 0.544345 11.00000 0.03478 0.01494 = 0.01951 -0.00100 -0.00164 0.00396 AFIX 43 H4 2 0.345081 -0.173392 0.493513 11.00000 -1.20000 AFIX 0 C5 1 0.462145 -0.101746 0.561145 11.00000 0.03037 0.02153 = 0.02166 0.00124 0.00606 0.00248 AFIX 43 H5 2 0.523112 -0.110471 0.522472 11.00000 -1.20000 AFIX 0 C6 1 0.475782 -0.052899 0.633354 11.00000 0.02214 0.02315 = 0.02200 0.00103 0.00624 0.00084 AFIX 43 H6 2 0.547176 -0.027403 0.645606 11.00000 -1.20000 AFIX 0 C7 1 0.403581 0.017763 0.764201 11.00000 0.01624 0.02123 = 0.01570 -0.00041 0.00107 -0.00375 AFIX 13 H7 2 0.483797 0.037983 0.763463 11.00000 -1.20000 AFIX 0 C9 1 0.450623 -0.109170 0.860600 11.00000 0.01955 0.02140 = 0.02389 -0.00148 0.00203 0.00257 AFIX 43 H9 2 0.509660 -0.126180 0.822783 11.00000 -1.20000 AFIX 0 C10 1 0.428571 -0.158239 0.932266 11.00000 0.02807 0.02258 = 0.02574 0.00404 0.00259 0.00471 AFIX 43 H10 2 0.472240 -0.209277 0.945346 11.00000 -1.20000 AFIX 0 C11 1 0.339652 -0.131744 0.986607 11.00000 0.03169 0.02371 = 0.02135 0.00128 0.00525 -0.00192 AFIX 43 H11 2 0.322687 -0.166029 1.036219 11.00000 -1.20000 AFIX 0 C12 1 0.277762 -0.058059 0.969323 11.00000 0.02593 0.02270 = 0.01937 -0.00124 0.00626 -0.00017 AFIX 43 H12 2 0.217998 -0.040992 1.006442 11.00000 -1.20000 AFIX 0 C13 1 0.303239 -0.007091 0.895552 11.00000 0.01981 0.02009 = 0.01853 -0.00267 0.00267 -0.00187 C15 1 0.381665 0.211940 0.839527 11.00000 0.03003 0.02571 = 0.02730 -0.00470 0.00308 -0.00234 AFIX 137 H15A 2 0.384810 0.266457 0.805293 11.00000 -1.50000 H15B 2 0.458335 0.193021 0.853985 11.00000 -1.50000 H15C 2 0.339306 0.223015 0.892567 11.00000 -1.50000 AFIX 0 C16 1 0.168050 0.151648 0.734747 11.00000 0.02100 0.02499 = 0.02670 0.00396 0.00365 -0.00006 AFIX 137 H16A 2 0.113655 0.150065 0.782148 11.00000 -1.50000 H16B 2 0.145760 0.108784 0.690520 11.00000 -1.50000 H16C 2 0.169723 0.211310 0.709786 11.00000 -1.50000 AFIX 0 N1 3 0.387443 -0.039638 0.689383 11.00000 0.01964 0.01794 = 0.01593 -0.00067 0.00177 -0.00036 N8 3 0.387732 -0.035526 0.843240 11.00000 0.01856 0.02007 = 0.01603 0.00022 0.00153 0.00010 O2 4 0.203249 -0.057723 0.727695 11.00000 0.01939 0.03088 = 0.02603 -0.00427 0.00390 -0.00432 O13 4 0.252014 0.064735 0.873741 11.00000 0.02380 0.02219 = 0.02137 0.00145 0.00563 0.00426 SI14 5 0.310146 0.122826 0.776017 11.00000 0.01701 0.01883 = 0.01866 -0.00087 0.00153 -0.00049 CL17 6 0.390420 0.166149 0.643508 11.00000 0.01940 0.02423 = 0.02087 0.00331 0.00170 -0.00057 HKLF 4 Covalent radii and connectivity table for 2009src0138 in Pbca C 0.770 H 0.320 N 0.700 O 0.660 SI 1.170 CL 0.990 C2 - O2 N1 C3 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 C6 - C5 N1 C7 - N1 N8 Si14 C9 - C10 N8 C10 - C9 C11 C11 - C12 C10 C12 - C11 C13 C13 - O13 N8 C12 C15 - Si14 C16 - Si14 N1 - C6 C2 C7 N8 - C13 C9 C7 O2 - C2 O13 - C13 Si14 Si14 - C16 C15 O13 C7 Cl17 Cl17 - Si14 34250 Reflections read, of which 2246 rejected -13 =< h =< 15, -16 =< k =< 19, -20 =< l =< 20, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 2 3 17 0.00 0.52 10 2.61 1 Inconsistent equivalents 3187 Unique reflections, of which 0 suppressed R(int) = 0.0758 R(sigma) = 0.0426 Friedel opposites merged Maximum memory for data reduction = 1878 / 31930 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 = 2370 / 218440 wR2 = 0.1106 before cycle 1 for 3187 data and 174 / 174 parameters GooF = S = 1.051; Restrained GooF = 1.051 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0566 * P )^2 + 1.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.40678 0.00085 -0.177 OSF Mean shift/su = 0.048 Maximum = -0.233 for U22 Si14 Max. shift = 0.001 A for H15A Max. dU = 0.000 for C6 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2370 / 218440 wR2 = 0.1105 before cycle 2 for 3187 data and 174 / 174 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0566 * P )^2 + 1.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.40666 0.00085 -0.138 OSF Mean shift/su = 0.016 Maximum = -0.138 for OSF Max. shift = 0.001 A for H15A Max. dU = 0.000 for C6 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2370 / 218440 wR2 = 0.1105 before cycle 3 for 3187 data and 174 / 174 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0566 * P )^2 + 1.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.40666 0.00085 -0.001 OSF Mean shift/su = 0.001 Maximum = 0.018 for tors H15A Max. shift = 0.000 A for H15A Max. dU = 0.000 for C4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2370 / 218440 wR2 = 0.1105 before cycle 4 for 3187 data and 174 / 174 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0566 * P )^2 + 1.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.40666 0.00085 0.000 OSF Mean shift/su = 0.000 Maximum = 0.009 for tors H15A Max. shift = 0.000 A for H15B Max. dU = 0.000 for C7 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.1989 -0.1561 0.5875 43 0.950 0.000 C3 C4 C2 H4 0.3451 -0.1734 0.4935 43 0.950 0.000 C4 C3 C5 H5 0.5231 -0.1104 0.5225 43 0.950 0.000 C5 C6 C4 H6 0.5472 -0.0274 0.6456 43 0.950 0.000 C6 C5 N1 H7 0.4838 0.0380 0.7635 13 1.000 0.000 C7 N1 N8 Si14 H9 0.5097 -0.1262 0.8228 43 0.950 0.000 C9 C10 N8 H10 0.4722 -0.2093 0.9453 43 0.950 0.000 C10 C9 C11 H11 0.3227 -0.1661 1.0362 43 0.950 0.000 C11 C12 C10 H12 0.2180 -0.0410 1.0065 43 0.950 0.000 C12 C11 C13 H15A 0.3847 0.2665 0.8053 137 0.980 0.000 C15 Si14 H15A H15B 0.4584 0.1931 0.8539 137 0.980 0.000 C15 Si14 H15A H15C 0.3394 0.2229 0.8926 137 0.980 0.000 C15 Si14 H15A H16A 0.1137 0.1501 0.7822 137 0.980 0.000 C16 Si14 H16A H16B 0.1458 0.1088 0.6905 137 0.980 0.000 C16 Si14 H16A H16C 0.1697 0.2113 0.7098 137 0.980 0.000 C16 Si14 H16A 2009src0138 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 0.27974 -0.07469 0.67558 1.00000 0.02118 0.01833 0.02064 0.00129 0.00144 -0.00112 0.02005 0.00334 0.00017 0.00013 0.00012 0.00000 0.00100 0.00097 0.00091 0.00073 0.00077 0.00083 0.00041 C3 0.26888 -0.12810 0.59942 1.00000 0.02659 0.01926 0.02521 0.00058 -0.00330 -0.00215 0.02369 0.00350 0.00018 0.00013 0.00013 0.00000 0.00108 0.00103 0.00098 0.00078 0.00084 0.00085 0.00044 H3 0.19891 -0.15610 0.58750 1.00000 0.02842 0.00000 0.00000 C4 0.35585 -0.13946 0.54435 1.00000 0.03473 0.01487 0.01938 -0.00099 -0.00161 0.00400 0.02299 0.00353 0.00019 0.00013 0.00012 0.00000 0.00120 0.00094 0.00093 0.00072 0.00086 0.00085 0.00044 H4 0.34510 -0.17341 0.49352 1.00000 0.02759 0.00000 0.00000 C5 0.46215 -0.10174 0.56113 1.00000 0.03020 0.02154 0.02152 0.00122 0.00610 0.00249 0.02442 0.00359 0.00018 0.00013 0.00012 0.00000 0.00114 0.00102 0.00094 0.00077 0.00083 0.00088 0.00044 H5 0.52311 -0.11045 0.52245 1.00000 0.02930 0.00000 0.00000 C6 0.47578 -0.05291 0.63336 1.00000 0.02202 0.02299 0.02195 0.00100 0.00623 0.00085 0.02232 0.00357 0.00017 0.00013 0.00012 0.00000 0.00104 0.00106 0.00094 0.00077 0.00078 0.00085 0.00043 H6 0.54718 -0.02743 0.64563 1.00000 0.02678 0.00000 0.00000 C7 0.40358 0.01776 0.76421 1.00000 0.01615 0.02112 0.01558 -0.00043 0.00106 -0.00375 0.01762 0.00315 0.00016 0.00012 0.00011 0.00000 0.00095 0.00096 0.00087 0.00070 0.00070 0.00078 0.00040 H7 0.48379 0.03799 0.76347 1.00000 0.02114 0.00000 0.00000 C9 0.45063 -0.10917 0.86060 1.00000 0.01944 0.02133 0.02385 -0.00143 0.00203 0.00259 0.02154 0.00337 0.00017 0.00013 0.00012 0.00000 0.00101 0.00102 0.00094 0.00077 0.00078 0.00083 0.00042 H9 0.50966 -0.12618 0.82279 1.00000 0.02585 0.00000 0.00000 C10 0.42857 -0.15823 0.93226 1.00000 0.02799 0.02250 0.02563 0.00405 0.00260 0.00467 0.02537 0.00372 0.00019 0.00014 0.00013 0.00000 0.00111 0.00104 0.00101 0.00080 0.00085 0.00089 0.00045 H10 0.47224 -0.20927 0.94533 1.00000 0.03045 0.00000 0.00000 C11 0.33966 -0.13176 0.98660 1.00000 0.03163 0.02353 0.02132 0.00129 0.00524 -0.00194 0.02549 0.00362 0.00019 0.00013 0.00013 0.00000 0.00117 0.00104 0.00096 0.00079 0.00085 0.00091 0.00045 H11 0.32269 -0.16605 1.03621 1.00000 0.03059 0.00000 0.00000 C12 0.27775 -0.05805 0.96932 1.00000 0.02583 0.02263 0.01929 -0.00120 0.00627 -0.00015 0.02258 0.00346 0.00018 0.00013 0.00012 0.00000 0.00105 0.00103 0.00090 0.00074 0.00079 0.00087 0.00043 H12 0.21800 -0.04098 1.00645 1.00000 0.02710 0.00000 0.00000 C13 0.30322 -0.00709 0.89554 1.00000 0.01966 0.02004 0.01844 -0.00267 0.00261 -0.00181 0.01938 0.00321 0.00016 0.00012 0.00012 0.00000 0.00097 0.00099 0.00089 0.00072 0.00074 0.00081 0.00041 C15 0.38165 0.21194 0.83952 1.00000 0.02994 0.02568 0.02724 -0.00470 0.00308 -0.00234 0.02762 0.00357 0.00019 0.00014 0.00013 0.00000 0.00116 0.00110 0.00104 0.00086 0.00086 0.00093 0.00047 H15A 0.38468 0.26648 0.80533 1.00000 0.04143 0.00000 0.00000 H15B 0.45836 0.19306 0.85390 1.00000 0.04143 0.00000 0.00000 H15C 0.33935 0.22294 0.89261 1.00000 0.04143 0.00000 0.00000 C16 0.16806 0.15164 0.73475 1.00000 0.02095 0.02491 0.02671 0.00392 0.00362 -0.00008 0.02419 0.00364 0.00017 0.00014 0.00013 0.00000 0.00105 0.00103 0.00102 0.00080 0.00081 0.00086 0.00044 H16A 0.11367 0.15008 0.78216 1.00000 0.03629 0.00000 0.00000 H16B 0.14576 0.10876 0.69055 1.00000 0.03629 0.00000 0.00000 H16C 0.16974 0.21129 0.70977 1.00000 0.03629 0.00000 0.00000 N1 0.38745 -0.03964 0.68938 1.00000 0.01950 0.01788 0.01585 -0.00072 0.00177 -0.00042 0.01774 0.00266 0.00013 0.00010 0.00009 0.00000 0.00083 0.00080 0.00075 0.00060 0.00062 0.00066 0.00035 N8 0.38774 -0.03551 0.84324 1.00000 0.01843 0.02002 0.01597 0.00020 0.00152 0.00010 0.01814 0.00271 0.00013 0.00011 0.00010 0.00000 0.00083 0.00083 0.00074 0.00060 0.00061 0.00067 0.00035 O2 0.20325 -0.05772 0.72769 1.00000 0.01930 0.03078 0.02594 -0.00428 0.00390 -0.00432 0.02534 0.00237 0.00012 0.00010 0.00008 0.00000 0.00074 0.00080 0.00074 0.00057 0.00058 0.00062 0.00033 O13 0.25201 0.06473 0.87374 1.00000 0.02372 0.02210 0.02130 0.00147 0.00562 0.00427 0.02237 0.00241 0.00012 0.00009 0.00008 0.00000 0.00075 0.00074 0.00065 0.00054 0.00056 0.00060 0.00031 Si14 0.31014 0.12283 0.77602 1.00000 0.01694 0.01874 0.01858 -0.00086 0.00153 -0.00051 0.01809 0.00089 0.00004 0.00003 0.00003 0.00000 0.00028 0.00029 0.00026 0.00019 0.00020 0.00021 0.00015 Cl17 0.39042 0.16615 0.64351 1.00000 0.01934 0.02415 0.02082 0.00330 0.00170 -0.00057 0.02143 0.00081 0.00004 0.00003 0.00003 0.00000 0.00026 0.00027 0.00024 0.00018 0.00017 0.00019 0.00014 Final Structure Factor Calculation for 2009src0138 in Pbca Total number of l.s. parameters = 174 Maximum vector length = 511 Memory required = 2196 / 25039 wR2 = 0.1105 before cycle 5 for 3187 data and 0 / 174 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0566 * P )^2 + 1.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0414 for 2496 Fo > 4sig(Fo) and 0.0598 for all 3187 data wR2 = 0.1105, GooF = S = 1.052, Restrained GooF = 1.052 for all data Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 15.00 for hydrogen atoms Principal mean square atomic displacements U 0.0224 0.0207 0.0171 C2 0.0297 0.0227 0.0187 C3 0.0357 0.0193 0.0140 C4 0.0340 0.0209 0.0184 C5 0.0285 0.0227 0.0157 C6 0.0232 0.0158 0.0138 C7 0.0247 0.0231 0.0168 C9 0.0332 0.0240 0.0189 C10 0.0340 0.0241 0.0184 C11 0.0297 0.0227 0.0154 C12 0.0241 0.0180 0.0160 C13 0.0345 0.0267 0.0217 C15 0.0307 0.0233 0.0186 C16 0.0204 0.0178 0.0150 N1 0.0201 0.0191 0.0152 N8 0.0353 0.0236 0.0171 O2 0.0305 0.0204 0.0162 O13 0.0202 0.0181 0.0160 Si14 0.0262 0.0208 0.0173 Cl17 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.024 0.036 0.050 0.064 0.082 0.103 0.134 0.190 1.000 Number in group 325. 335. 314. 319. 307. 323. 315. 319. 310. 320. GooF 0.939 0.939 1.112 1.180 1.154 1.150 1.060 0.966 0.999 0.993 K 2.083 0.985 0.928 0.928 0.954 0.979 0.992 1.016 1.030 0.999 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 329. 323. 306. 320. 327. 313. 312. 320. 320. 317. GooF 0.988 0.966 0.980 1.052 1.046 1.033 0.982 0.957 1.131 1.330 K 0.985 1.029 1.015 1.010 1.032 1.025 1.037 1.039 1.015 0.969 R1 0.144 0.123 0.098 0.083 0.062 0.055 0.043 0.035 0.036 0.031 Recommended weighting scheme: WGHT 0.0554 1.2225 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) 5 3 6 525.51 347.78 4.83 0.075 1.65 3 4 7 60.77 23.04 4.18 0.019 1.72 2 7 3 276.90 183.65 3.91 0.054 1.89 11 0 14 2056.97 1329.63 3.88 0.147 0.77 1 6 5 104.21 58.54 3.79 0.031 1.93 6 12 9 78.96 164.46 3.78 0.052 0.90 4 1 7 145.25 85.06 3.74 0.037 1.77 5 12 14 185.21 360.11 3.72 0.076 0.79 1 7 14 164.33 260.43 3.57 0.065 0.98 0 2 4 262.89 187.86 3.39 0.055 3.45 1 7 1 24.53 2.85 3.31 0.007 2.10 12 0 6 367.25 607.66 3.30 0.099 0.92 6 5 2 1175.01 928.20 3.24 0.122 1.62 8 15 4 451.70 248.63 3.21 0.063 0.81 2 2 8 75.73 122.14 3.18 0.044 1.79 3 5 15 91.29 153.67 3.14 0.050 0.95 4 8 2 235.06 159.79 3.14 0.051 1.56 7 12 1 3.09 56.03 3.13 0.030 1.01 6 1 3 3069.78 2508.68 3.09 0.201 1.83 6 3 0 979.09 1269.78 3.09 0.143 1.84 10 3 2 299.78 408.55 3.08 0.081 1.14 10 7 9 82.10 20.55 3.07 0.018 0.89 12 1 5 238.45 351.30 3.06 0.075 0.94 1 0 2 47.90 80.97 3.02 0.036 6.50 6 11 10 155.09 230.80 2.99 0.061 0.91 2 4 18 220.58 338.73 2.98 0.074 0.83 9 8 14 252.00 388.81 2.91 0.079 0.77 2 2 10 199.03 140.90 2.88 0.048 1.47 5 3 1 790.79 982.18 2.86 0.126 2.13 2 7 6 327.43 423.80 2.84 0.083 1.60 3 11 1 69.19 124.36 2.80 0.045 1.29 2 8 0 3.91 21.98 2.77 0.019 1.80 5 9 13 61.87 114.09 2.73 0.043 0.90 9 6 7 30.93 56.74 2.73 0.030 1.03 2 17 6 1160.77 838.78 2.73 0.116 0.83 4 1 4 266.11 345.54 2.71 0.075 2.33 0 4 6 1761.84 1468.28 2.69 0.154 2.14 0 6 5 447.81 568.14 2.69 0.096 1.95 9 1 6 40.32 87.23 2.68 0.038 1.17 3 6 2 1231.09 1483.88 2.68 0.155 2.05 1 11 4 57.33 96.55 2.66 0.039 1.29 4 12 7 44.79 88.71 2.65 0.038 1.03 4 6 5 2817.04 2386.09 2.63 0.196 1.63 8 1 2 113.20 163.06 2.62 0.051 1.45 7 5 9 -2.61 20.56 2.60 0.018 1.12 7 11 9 38.96 88.25 2.59 0.038 0.91 6 11 4 16.70 58.07 2.58 0.031 1.08 6 12 3 230.89 310.80 2.57 0.071 1.04 2 7 4 2276.18 2689.76 2.55 0.208 1.80 1 7 5 49.24 80.10 2.53 0.036 1.75 Bond lengths and angles C2 - Distance Angles O2 1.2434 (0.0023) N1 1.4002 (0.0025) 119.30 (0.17) C3 1.4376 (0.0027) 125.89 (0.19) 114.80 (0.17) C2 - O2 N1 C3 - Distance Angles C4 1.3522 (0.0030) C2 1.4376 (0.0027) 121.58 (0.20) H3 0.9500 119.21 119.21 C3 - C4 C2 C4 - Distance Angles C3 1.3522 (0.0030) C5 1.4085 (0.0030) 121.05 (0.18) H4 0.9500 119.48 119.48 C4 - C3 C5 C5 - Distance Angles C6 1.3523 (0.0028) C4 1.4085 (0.0030) 118.74 (0.19) H5 0.9500 120.63 120.63 C5 - C6 C4 C6 - Distance Angles C5 1.3523 (0.0028) N1 1.3775 (0.0024) 120.85 (0.19) H6 0.9500 119.58 119.58 C6 - C5 N1 C7 - Distance Angles N1 1.4624 (0.0023) N8 1.4798 (0.0023) 108.80 (0.15) Si14 1.9428 (0.0020) 118.89 (0.13) 106.97 (0.12) H7 1.0000 107.22 107.22 107.22 C7 - N1 N8 Si14 C9 - Distance Angles C10 1.3625 (0.0028) N8 1.3653 (0.0026) 119.89 (0.18) H9 0.9500 120.06 120.06 C9 - C10 N8 C10 - Distance Angles C9 1.3625 (0.0028) C11 1.4096 (0.0029) 118.68 (0.19) H10 0.9500 120.66 120.66 C10 - C9 C11 C11 - Distance Angles C12 1.3593 (0.0029) C10 1.4096 (0.0029) 121.21 (0.18) H11 0.9500 119.40 119.40 C11 - C12 C10 C12 - Distance Angles C11 1.3593 (0.0029) C13 1.4131 (0.0026) 119.30 (0.18) H12 0.9500 120.35 120.35 C12 - C11 C13 C13 - Distance Angles O13 1.2875 (0.0023) N8 1.3607 (0.0024) 117.13 (0.16) C12 1.4131 (0.0026) 124.76 (0.17) 118.12 (0.17) C13 - O13 N8 C15 - Distance Angles Si14 1.8710 (0.0021) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 - Si14 H15A H15B C16 - Distance Angles Si14 1.8561 (0.0021) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - Si14 H16A H16B N1 - Distance Angles C6 1.3775 (0.0024) C2 1.4002 (0.0025) 122.93 (0.16) C7 1.4624 (0.0023) 119.28 (0.16) 117.70 (0.15) N1 - C6 C2 N8 - Distance Angles C13 1.3607 (0.0024) C9 1.3653 (0.0026) 122.78 (0.16) C7 1.4798 (0.0023) 114.75 (0.15) 122.43 (0.15) N8 - C13 C9 O2 - Distance Angles C2 1.2434 (0.0023) O2 - O13 - Distance Angles C13 1.2875 (0.0023) Si14 1.8844 (0.0014) 115.49 (0.12) O13 - C13 Si14 - Distance Angles C16 1.8561 (0.0021) C15 1.8710 (0.0021) 115.25 (0.10) O13 1.8844 (0.0014) 93.13 (0.08) 94.29 (0.08) C7 1.9428 (0.0020) 132.62 (0.09) 112.12 (0.09) 84.61 (0.07) Cl17 2.3615 (0.0007) 90.04 (0.07) 94.49 (0.07) 168.35 (0.05) 85.00 (0.06) Si14 - C16 C15 O13 C7 Cl17 - Distance Angles Si14 2.3615 (0.0007) Cl17 - FMAP and GRID set by program FMAP 2 2 19 GRID -1.563 24 -2 1.563 1 2 R1 = 0.0593 for 3187 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.28 at 0.8985 0.1631 0.5936 [ 1.16 A from H15C ] Deepest hole -0.40 at 0.3207 0.1270 0.7312 [ 0.71 A from SI14 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2548 / 26921 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3985 0.1631 0.9064 1.00000 0.05 0.28 1.16 H15C 1.17 H15B 1.29 C15 2.22 H15A Q2 1 0.3865 0.1701 0.8113 1.00000 0.05 0.27 0.77 C15 1.13 H15B 1.28 SI14 1.46 H15A Q3 1 0.4007 0.0737 0.7719 1.00000 0.05 0.27 0.85 C7 1.13 H7 1.31 SI14 1.99 N8 Q4 1 0.2806 -0.1174 0.6394 1.00000 0.05 0.25 0.66 C3 0.86 C2 1.39 H3 1.76 C4 Q5 1 0.3969 0.1192 0.7142 1.00000 0.05 0.25 1.31 CL17 1.41 SI14 1.72 C7 1.77 H7 Q6 1 0.1351 0.0077 0.6891 1.00000 0.05 0.24 1.41 O2 1.53 H16B 1.99 H7 2.13 C2 Q7 1 0.3179 0.1258 0.9437 1.00000 0.05 0.23 1.63 O13 1.69 H15C 2.15 C13 2.20 H4 Q8 1 0.3087 0.1264 0.6837 1.00000 0.05 0.23 1.30 CL17 1.44 SI14 1.89 C16 1.96 H16B Q9 1 0.2026 0.1298 0.7697 1.00000 0.05 0.22 0.76 C16 1.12 H16A 1.28 SI14 1.44 H16B Q10 1 0.2932 0.2567 0.8910 1.00000 0.05 0.22 0.75 H15C 1.48 C15 1.73 H15A 2.26 H15B Shortest distances between peaks (including symmetry equivalents) 3 5 1.13 5 8 1.15 1 7 1.25 1 2 1.49 2 3 1.59 2 5 1.70 8 9 1.84 1 10 1.90 3 8 1.92 2 10 2.11 7 10 2.16 2 8 2.28 2 7 2.31 2 9 2.36 6 9 2.37 5 9 2.47 1 3 2.49 3 9 2.50 4 6 2.67 6 8 2.73 9 10 2.89 3 7 2.95 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.02: 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 0.00: Analyse other restraints etc. 1.58: 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 1.00: Structure factors and derivatives 0.73: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0138 finished at 15:55:26 Total CPU time: 3.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++