+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0908 started at 11:07:22 on 29-Sep-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0908 in P2(1)/n CELL 0.71073 8.7123 14.4807 9.3751 90.000 105.322 90.000 ZERR 4.00 0.0004 0.0009 0.0005 0.000 0.003 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O SI CL UNIT 32 40 4 4 4 12 V = 1140.72 F(000) = 552.0 Mu = 0.87 mm-1 Cell Wt = 1082.44 Rho = 1.576 MERG 2 OMIT -3.00 55.00 OMIT -1 1 1 SHEL 7 0.77 FMAP 2 PLAN 20 SIZE 0.09 0.20 0.36 ACTA BOND $H WGHT 0.05260 0.55070 L.S. 4 TEMP -153.00 FVAR 0.67833 MOLE 1 C2 1 0.328295 0.066496 0.560163 11.00000 0.01842 0.02026 = 0.01599 0.00079 0.00237 0.00335 C3 1 0.348868 0.075509 0.417704 11.00000 0.02062 0.02327 = 0.01788 0.00086 0.00433 0.00352 AFIX 43 H3 2 0.279536 0.044564 0.336473 11.00000 -1.20000 AFIX 0 C4 1 0.469940 0.129380 0.396942 11.00000 0.02598 0.02473 = 0.02328 0.00598 0.01057 0.00590 AFIX 43 H4 2 0.484589 0.135193 0.300463 11.00000 -1.20000 AFIX 0 C5 1 0.573170 0.176332 0.515123 11.00000 0.02588 0.02398 = 0.02964 0.00634 0.01218 0.00179 AFIX 43 H5 2 0.656774 0.213975 0.499975 11.00000 -1.20000 AFIX 0 C6 1 0.549520 0.166142 0.652125 11.00000 0.01886 0.02127 = 0.02584 -0.00348 0.00468 -0.00069 C7 1 0.395035 0.098638 0.819965 11.00000 0.02377 0.02971 = 0.01302 -0.00300 0.00440 -0.00072 AFIX 23 H7A 2 0.383318 0.159259 0.864766 11.00000 -1.20000 H7B 2 0.484053 0.065132 0.887729 11.00000 -1.20000 AFIX 0 C8 1 0.009516 0.092442 0.722706 11.00000 0.02406 0.02963 = 0.02117 0.00044 0.00513 -0.00092 AFIX 23 H8A 2 -0.065424 0.053565 0.649221 11.00000 -1.20000 H8B 2 -0.037920 0.104133 0.806019 11.00000 -1.20000 AFIX 0 C9 1 0.187873 -0.097886 0.811921 11.00000 0.04579 0.03167 = 0.02401 0.00036 0.01092 -0.00761 AFIX 137 H9A 2 0.114621 -0.111526 0.872499 11.00000 -1.50000 H9B 2 0.293106 -0.123392 0.859654 11.00000 -1.50000 H9C 2 0.147536 -0.125769 0.713895 11.00000 -1.50000 AFIX 0 N1 3 0.429569 0.112289 0.675651 11.00000 0.01685 0.02119 = 0.01553 -0.00084 0.00380 0.00018 O2 4 0.219741 0.017221 0.593553 11.00000 0.02350 0.02602 = 0.01669 -0.00266 0.00654 -0.00637 SI1 5 0.203762 0.029561 0.792361 11.00000 0.02046 0.02510 = 0.01505 -0.00134 0.00422 -0.00333 CL2 6 0.224565 0.056975 1.037803 11.00000 0.03284 0.04520 = 0.01488 -0.00345 0.00769 -0.00492 CL4 6 0.038865 0.200182 0.638963 11.00000 0.03744 0.02706 = 0.04140 0.00471 0.01381 0.00435 CL6 6 0.666385 0.221094 0.803864 11.00000 0.02385 0.03717 = 0.03235 -0.00992 0.00585 -0.00996 HKLF 4 Covalent radii and connectivity table for 2008src0908 in P2(1)/n 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 Cl6 C7 - N1 Si1 C8 - Cl4 Si1 C9 - Si1 N1 - C6 C2 C7 O2 - C2 Si1 Si1 - C9 C8 C7 O2 Cl2 Cl2 - Si1 Cl4 - C8 Cl6 - C6 13563 Reflections read, of which 368 rejected -11 =< h =< 10, -18 =< k =< 18, -10 =< l =< 12, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) -11 2 1 -15.14 12.74 2 75.05 1 Inconsistent equivalents 2613 Unique reflections, of which 0 suppressed R(int) = 0.0661 R(sigma) = 0.0557 Friedel opposites merged Maximum memory for data reduction = 1418 / 25995 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 = 1771 / 164367 wR2 = 0.1129 before cycle 1 for 2613 data and 128 / 128 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0526 * P )^2 + 0.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.67832 0.00156 -0.003 OSF Mean shift/su = 0.002 Maximum = -0.012 for U13 Si1 Max. shift = 0.000 A for H9B Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1771 / 164367 wR2 = 0.1129 before cycle 2 for 2613 data and 128 / 128 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0526 * P )^2 + 0.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.67832 0.00156 0.000 OSF Mean shift/su = 0.001 Maximum = 0.004 for U12 Cl2 Max. shift = 0.000 A for H9B Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1771 / 164367 wR2 = 0.1129 before cycle 3 for 2613 data and 128 / 128 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0526 * P )^2 + 0.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.67832 0.00156 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for U22 Cl2 Max. shift = 0.000 A for H9A Max. dU = 0.000 for Cl2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1771 / 164367 wR2 = 0.1129 before cycle 4 for 2613 data and 128 / 128 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0526 * P )^2 + 0.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.67833 0.00156 0.001 OSF Mean shift/su = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H9A Max. dU = 0.000 for O2 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 0.2795 0.0446 0.3365 43 0.950 0.000 C3 C4 C2 H4 0.4846 0.1352 0.3005 43 0.950 0.000 C4 C3 C5 H5 0.6568 0.2140 0.5000 43 0.950 0.000 C5 C6 C4 H7A 0.3833 0.1593 0.8648 23 0.990 0.000 C7 N1 Si1 H7B 0.4841 0.0651 0.8877 23 0.990 0.000 C7 N1 Si1 H8A -0.0654 0.0536 0.6492 23 0.990 0.000 C8 Cl4 Si1 H8B -0.0379 0.1041 0.8060 23 0.990 0.000 C8 Cl4 Si1 H9A 0.1146 -0.1115 0.8725 137 0.980 0.000 C9 Si1 H9A H9B 0.2931 -0.1234 0.8597 137 0.980 0.000 C9 Si1 H9A H9C 0.1475 -0.1258 0.7139 137 0.980 0.000 C9 Si1 H9A 2008src0908 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 0.32830 0.06650 0.56016 1.00000 0.01842 0.02026 0.01599 0.00079 0.00237 0.00335 0.01864 0.00501 0.00030 0.00018 0.00028 0.00000 0.00125 0.00138 0.00129 0.00102 0.00107 0.00106 0.00055 C3 0.34887 0.07551 0.41770 1.00000 0.02062 0.02327 0.01788 0.00086 0.00433 0.00352 0.02073 0.00531 0.00030 0.00019 0.00029 0.00000 0.00130 0.00143 0.00133 0.00107 0.00110 0.00109 0.00057 H3 0.27954 0.04456 0.33647 1.00000 0.02488 0.00000 0.00000 C4 0.46994 0.12938 0.39694 1.00000 0.02598 0.02473 0.02328 0.00598 0.01057 0.00590 0.02389 0.00555 0.00031 0.00020 0.00030 0.00000 0.00139 0.00146 0.00141 0.00117 0.00117 0.00118 0.00060 H4 0.48459 0.13519 0.30046 1.00000 0.02867 0.00000 0.00000 C5 0.57317 0.17633 0.51512 1.00000 0.02588 0.02398 0.02964 0.00634 0.01218 0.00179 0.02558 0.00567 0.00033 0.00019 0.00031 0.00000 0.00138 0.00148 0.00150 0.00123 0.00123 0.00119 0.00061 H5 0.65677 0.21398 0.49998 1.00000 0.03070 0.00000 0.00000 C6 0.54952 0.16614 0.65212 1.00000 0.01886 0.02127 0.02584 -0.00348 0.00468 -0.00069 0.02222 0.00510 0.00030 0.00019 0.00030 0.00000 0.00126 0.00145 0.00145 0.00112 0.00113 0.00108 0.00059 C7 0.39503 0.09864 0.81996 1.00000 0.02377 0.02971 0.01302 -0.00300 0.00440 -0.00072 0.02225 0.00511 0.00031 0.00020 0.00028 0.00000 0.00137 0.00157 0.00122 0.00110 0.00107 0.00116 0.00058 H7A 0.38332 0.15926 0.86477 1.00000 0.02670 0.00000 0.00000 H7B 0.48405 0.06513 0.88773 1.00000 0.02670 0.00000 0.00000 C8 0.00952 0.09244 0.72271 1.00000 0.02406 0.02963 0.02117 0.00044 0.00513 -0.00092 0.02511 0.00552 0.00032 0.00020 0.00030 0.00000 0.00137 0.00158 0.00140 0.00120 0.00115 0.00121 0.00061 H8A -0.06542 0.05357 0.64922 1.00000 0.03014 0.00000 0.00000 H8B -0.03792 0.10413 0.80602 1.00000 0.03014 0.00000 0.00000 C9 0.18787 -0.09789 0.81192 1.00000 0.04579 0.03167 0.02401 0.00036 0.01092 -0.00761 0.03350 0.00601 0.00039 0.00022 0.00032 0.00000 0.00181 0.00175 0.00156 0.00128 0.00141 0.00144 0.00071 H9A 0.11462 -0.11153 0.87250 1.00000 0.05025 0.00000 0.00000 H9B 0.29311 -0.12339 0.85965 1.00000 0.05025 0.00000 0.00000 H9C 0.14754 -0.12577 0.71390 1.00000 0.05025 0.00000 0.00000 N1 0.42957 0.11229 0.67565 1.00000 0.01685 0.02119 0.01553 -0.00084 0.00380 0.00018 0.01795 0.00407 0.00024 0.00015 0.00023 0.00000 0.00102 0.00119 0.00106 0.00087 0.00086 0.00088 0.00046 O2 0.21974 0.01722 0.59355 1.00000 0.02350 0.02602 0.01669 -0.00266 0.00654 -0.00637 0.02183 0.00339 0.00021 0.00013 0.00019 0.00000 0.00095 0.00106 0.00092 0.00078 0.00077 0.00082 0.00042 Si1 0.20376 0.02956 0.79236 1.00000 0.02046 0.02510 0.01505 -0.00134 0.00422 -0.00333 0.02029 0.00141 0.00009 0.00005 0.00008 0.00000 0.00037 0.00042 0.00036 0.00030 0.00029 0.00030 0.00019 Cl2 0.22456 0.05698 1.03780 1.00000 0.03284 0.04520 0.01488 -0.00345 0.00769 -0.00492 0.03071 0.00138 0.00009 0.00006 0.00007 0.00000 0.00039 0.00047 0.00034 0.00029 0.00029 0.00032 0.00021 Cl4 0.03887 0.20018 0.63896 1.00000 0.03744 0.02706 0.04140 0.00471 0.01381 0.00435 0.03466 0.00157 0.00009 0.00005 0.00009 0.00000 0.00042 0.00041 0.00045 0.00032 0.00035 0.00031 0.00022 Cl6 0.66639 0.22109 0.80386 1.00000 0.02385 0.03717 0.03235 -0.00992 0.00585 -0.00996 0.03142 0.00130 0.00008 0.00005 0.00008 0.00000 0.00036 0.00045 0.00041 0.00032 0.00030 0.00030 0.00021 Final Structure Factor Calculation for 2008src0908 in P2(1)/n Total number of l.s. parameters = 128 Maximum vector length = 511 Memory required = 1643 / 25039 wR2 = 0.1129 before cycle 5 for 2613 data and 0 / 128 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0526 * P )^2 + 0.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0430 for 1932 Fo > 4sig(Fo) and 0.0686 for all 2613 data wR2 = 0.1129, GooF = S = 1.058, Restrained GooF = 1.058 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0233 0.0183 0.0143 C2 0.0258 0.0191 0.0173 C3 0.0340 0.0198 0.0179 C4 0.0350 0.0233 0.0184 C5 0.0282 0.0201 0.0184 C6 0.0302 0.0241 0.0124 C7 0.0299 0.0244 0.0211 C8 0.0493 0.0289 0.0224 C9 0.0214 0.0171 0.0154 N1 0.0313 0.0183 0.0159 O2 0.0268 0.0192 0.0149 Si1 0.0470 0.0313 0.0138 Cl2 0.0444 0.0344 0.0251 Cl4 0.0459 0.0309 0.0174 Cl6 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.031 0.049 0.066 0.085 0.107 0.137 0.176 0.252 1.000 Number in group 278. 250. 262. 261. 262. 261. 256. 259. 263. 261. GooF 0.927 0.933 1.001 1.226 1.215 1.164 1.080 0.988 0.988 1.013 K 1.256 0.807 0.893 0.918 0.963 0.966 0.991 1.009 1.021 1.009 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.65 inf Number in group 265. 260. 267. 258. 260. 257. 261. 265. 257. 263. GooF 0.932 1.050 1.013 1.040 1.013 1.032 0.918 0.946 1.112 1.437 K 0.963 0.990 0.995 0.997 1.016 1.029 1.034 1.037 1.008 0.989 R1 0.188 0.139 0.137 0.099 0.074 0.057 0.048 0.037 0.031 0.030 Recommended weighting scheme: WGHT 0.0526 0.5527 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) -1 3 2 23.30 4.65 5.23 0.015 3.30 -3 1 3 110.56 174.15 4.61 0.091 2.36 -5 3 2 31.51 65.58 4.49 0.056 1.63 -10 1 7 30.61 73.16 4.41 0.059 0.81 -5 3 6 126.12 62.87 4.25 0.055 1.26 -2 2 5 95.46 54.71 4.15 0.051 1.79 -4 12 8 56.49 150.83 3.96 0.085 0.82 -1 1 5 322.02 422.43 3.59 0.142 1.86 2 4 3 591.64 467.35 3.40 0.150 1.87 0 4 0 60.51 97.71 3.31 0.068 3.62 -3 0 9 1451.31 1135.65 3.28 0.233 1.04 -1 2 2 72.52 104.25 3.25 0.071 3.83 -4 1 4 20.66 38.34 3.18 0.043 1.78 -2 18 2 66.29 242.98 3.16 0.108 0.78 -4 1 3 5.27 16.38 3.12 0.028 1.97 -10 3 5 192.99 103.30 3.03 0.070 0.84 -6 14 4 85.68 147.41 3.00 0.084 0.82 -3 5 2 10.29 0.03 3.00 0.001 1.98 4 5 8 81.12 162.08 2.96 0.088 0.86 -4 5 2 80.20 51.87 2.96 0.050 1.72 3 0 3 27.86 1.77 2.89 0.009 1.83 0 5 3 157.04 114.31 2.87 0.074 2.09 -10 2 3 134.00 202.16 2.83 0.098 0.86 4 1 0 86.18 60.94 2.79 0.054 2.08 -3 0 1 1856.39 2208.08 2.79 0.325 2.90 2 2 10 284.69 166.26 2.77 0.089 0.83 4 4 3 220.90 170.20 2.74 0.090 1.42 -5 1 1 351.91 286.88 2.72 0.117 1.72 -2 1 2 4184.69 4915.31 2.71 0.485 3.48 -7 2 7 208.53 281.97 2.71 0.116 1.01 -3 6 1 3381.69 2896.44 2.69 0.372 1.86 1 2 4 13.72 0.10 2.67 0.002 1.97 3 13 6 -10.67 64.49 2.66 0.056 0.82 -10 6 5 426.89 286.54 2.65 0.117 0.80 -5 5 10 -30.41 150.14 2.64 0.085 0.86 0 4 4 230.32 171.42 2.61 0.091 1.92 -4 7 5 1141.44 966.89 2.60 0.215 1.26 3 16 2 238.05 341.30 2.58 0.128 0.83 3 9 5 1081.03 892.67 2.57 0.207 1.04 1 0 3 719.12 855.78 2.56 0.202 2.63 0 6 2 113.38 79.32 2.54 0.062 2.13 -5 12 7 297.88 388.94 2.54 0.136 0.85 0 10 0 586.09 709.13 2.53 0.184 1.45 -4 6 8 16.43 33.22 2.51 0.040 1.02 7 9 5 112.14 232.16 2.50 0.105 0.78 -4 15 1 770.45 620.24 2.49 0.172 0.88 1 7 3 12.57 27.86 2.47 0.037 1.62 2 14 2 217.02 150.67 2.46 0.085 0.97 1 5 8 101.43 134.63 2.44 0.080 1.01 2 13 6 99.14 48.95 2.43 0.048 0.85 Bond lengths and angles C2 - Distance Angles O2 1.2876 (0.0032) N1 1.3732 (0.0033) 115.86 (0.22) C3 1.3998 (0.0035) 124.82 (0.24) 119.32 (0.23) C2 - O2 N1 C3 - Distance Angles C4 1.3666 (0.0038) C2 1.3998 (0.0035) 119.17 (0.26) H3 0.9500 120.42 120.42 C3 - C4 C2 C4 - Distance Angles C3 1.3666 (0.0038) C5 1.4043 (0.0041) 121.43 (0.25) H4 0.9500 119.28 119.28 C4 - C3 C5 C5 - Distance Angles C6 1.3615 (0.0037) C4 1.4043 (0.0041) 117.83 (0.24) H5 0.9500 121.09 121.09 C5 - C6 C4 C6 - Distance Angles C5 1.3615 (0.0037) N1 1.3677 (0.0033) 121.77 (0.25) Cl6 1.7112 (0.0027) 121.92 (0.21) 116.31 (0.19) C6 - C5 N1 C7 - Distance Angles N1 1.4749 (0.0031) Si1 1.9017 (0.0027) 109.24 (0.17) H7A 0.9900 109.83 109.83 H7B 0.9900 109.83 109.83 108.27 C7 - N1 Si1 H7A C8 - Distance Angles Cl4 1.7950 (0.0029) Si1 1.8803 (0.0029) 110.71 (0.14) H8A 0.9900 109.50 109.50 H8B 0.9900 109.50 109.50 108.07 C8 - Cl4 Si1 H8A C9 - Distance Angles Si1 1.8634 (0.0032) 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 N1 - Distance Angles C6 1.3677 (0.0033) C2 1.3732 (0.0033) 120.49 (0.21) C7 1.4749 (0.0031) 125.04 (0.22) 114.47 (0.20) N1 - C6 C2 O2 - Distance Angles C2 1.2876 (0.0032) Si1 1.9137 (0.0018) 115.60 (0.16) O2 - C2 Si1 - Distance Angles C9 1.8634 (0.0032) C8 1.8803 (0.0029) 115.49 (0.14) C7 1.9017 (0.0027) 126.35 (0.14) 117.93 (0.13) O2 1.9137 (0.0018) 91.71 (0.11) 89.85 (0.10) 83.97 (0.10) Cl2 2.2945 (0.0009) 93.49 (0.09) 95.15 (0.09) 86.47 (0.08) 170.42 (0.07) Si1 - C9 C8 C7 O2 Cl2 - Distance Angles Si1 2.2945 (0.0009) Cl2 - Cl4 - Distance Angles C8 1.7950 (0.0029) Cl4 - Cl6 - Distance Angles C6 1.7112 (0.0028) Cl6 - FMAP and GRID set by program FMAP 2 2 20 GRID -1.471 -2 -2 1.471 2 2 R1 = 0.0683 for 2613 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.89 at 0.7379 0.1627 0.1837 [ 0.71 A from H9B ] Deepest hole -0.44 at 0.0958 0.1956 0.6037 [ 0.67 A from CL4 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 1737 / 16899 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2621 -0.1627 0.8163 1.00000 0.05 0.89 0.71 H9B 1.13 C9 1.30 H9C 1.68 H9A Q2 1 0.0997 -0.1146 1.0394 1.00000 0.05 0.35 1.60 H9A 1.68 H8B 2.46 C9 2.67 C8 Q3 1 0.6767 0.2505 0.5074 1.00000 0.05 0.34 0.55 H5 1.42 C5 2.31 C6 2.53 C4 Q4 1 0.3172 0.0946 0.4647 1.00000 0.05 0.33 0.64 C3 0.96 C2 1.37 H3 1.70 C4 Q5 1 0.0685 -0.1349 0.6605 1.00000 0.05 0.32 0.75 H9C 1.61 C9 1.95 H9A 2.33 H9B Q6 1 0.2255 -0.0730 0.6621 1.00000 0.05 0.30 1.21 H9C 1.45 O2 1.57 C9 1.93 H9B Q7 1 0.2354 0.0031 0.6663 1.00000 0.05 0.30 0.69 O2 1.34 SI1 1.71 C2 2.11 H9C Q8 1 0.2911 -0.0283 1.0616 1.00000 0.05 0.29 1.36 CL2 1.96 H7B 2.34 H9B 2.35 H9A Q9 1 0.3613 0.1020 0.6039 1.00000 0.05 0.29 0.67 C2 0.79 N1 1.72 O2 1.76 C3 Q10 1 0.3380 0.0430 0.8145 1.00000 0.05 0.28 0.94 C7 1.15 SI1 1.32 H7B 1.76 H7A Q11 1 0.1915 -0.0050 0.5678 1.00000 0.05 0.28 0.44 O2 1.59 C2 2.14 SI1 2.16 H8A Q12 1 0.4277 0.0750 0.8436 1.00000 0.05 0.27 0.46 C7 0.57 H7B 1.31 H7A 1.67 N1 Q13 1 0.4962 0.1325 0.6666 1.00000 0.05 0.26 0.68 N1 0.71 C6 1.81 C2 1.84 C5 Q14 1 0.1057 0.0747 0.7643 1.00000 0.05 0.26 0.86 C8 1.05 SI1 1.47 H8B 1.62 H8A Q15 1 0.3957 0.0839 0.6454 1.00000 0.05 0.26 0.54 N1 0.89 C2 1.65 C7 1.77 O2 Q16 1 0.6278 0.2952 0.4205 1.00000 0.05 0.26 1.38 H5 2.05 C5 2.13 H8B 2.45 CL2 Q17 1 0.5687 0.1936 0.8518 1.00000 0.05 0.25 1.13 CL6 1.72 H7A 1.88 C6 2.01 C7 Q18 1 0.1930 0.0423 0.3372 1.00000 0.05 0.25 0.76 H3 1.45 C3 1.80 H8A 2.14 C2 Q19 1 0.3591 0.1851 0.5941 1.00000 0.05 0.24 1.35 N1 1.63 C6 1.75 C2 2.18 C5 Q20 1 -0.1320 0.1658 0.8731 1.00000 0.05 0.24 1.46 H8B 1.88 CL6 2.36 C8 2.48 H9A Shortest distances between peaks (including symmetry equivalents) 9 15 0.50 10 12 0.89 7 11 0.91 3 16 1.04 2 20 1.09 13 15 1.10 6 7 1.11 9 19 1.21 9 13 1.25 4 9 1.26 6 11 1.30 13 19 1.43 15 19 1.55 7 10 1.55 4 18 1.58 5 6 1.63 4 15 1.66 4 19 1.76 12 15 1.81 7 15 1.87 10 15 1.88 13 17 1.90 1 6 1.91 7 14 1.93 1 5 1.96 7 9 1.98 10 14 2.01 2 8 2.05 12 13 2.08 12 17 2.10 9 11 2.11 11 15 2.16 4 13 2.18 4 11 2.18 9 12 2.20 9 10 2.21 6 10 2.25 16 20 2.26 11 18 2.27 7 12 2.28 14 16 2.36 10 11 2.43 5 11 2.44 11 14 2.45 5 7 2.46 8 12 2.47 2 16 2.48 10 13 2.55 4 7 2.56 8 20 2.59 17 20 2.59 17 19 2.62 15 17 2.64 5 18 2.65 8 10 2.66 6 14 2.67 1 19 2.67 9 18 2.69 12 14 2.71 8 17 2.71 6 15 2.74 5 17 2.74 1 7 2.76 12 19 2.76 14 20 2.86 9 17 2.86 1 2 2.90 6 9 2.91 3 20 2.92 10 17 2.92 2 14 2.94 7 13 2.94 10 19 2.96 1 8 2.97 3 13 2.98 7 19 2.99 Time profile in seconds ----------------------- 0.02: 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 0.00: Analyse other restraints etc. 0.66: 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 0.39: Structure factors and derivatives 0.31: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0908 finished at 11:07:23 Total CPU time: 1.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++