+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0193 started at 17:06:53 on 19-Feb-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0193 in C2/m CELL 0.71073 20.9041 14.5008 5.9078 90.000 102.021 90.000 ZERR 1.00 0.0007 0.0005 0.0002 0.000 0.002 0.000 LATT 7 SYMM - X, Y, - Z SFAC C H N O F P CL UNIT 24 16 12 8 32 12 16 V = 1751.54 F(000) = 1048.0 Mu = 1.04 mm-1 Cell Wt = 2147.33 Rho = 2.036 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 20 SIZE 0.10 0.10 0.45 ACTA BOND WGHT 0.08380 63.83500 L.S. 4 TEMP -153.00 FVAR 0.29317 C1 1 0.133435 0.186176 -0.109974 11.00000 0.01521 0.02241 = 0.03142 -0.00142 -0.00213 0.00358 AFIX 23 H1A 2 0.128216 0.248820 -0.049687 11.00000 -1.20000 H1B 2 0.117701 0.140691 -0.009086 11.00000 -1.20000 AFIX 0 C2 1 0.095209 0.177288 -0.357456 11.00000 0.01935 0.02057 = 0.02798 0.00320 0.00669 0.00082 C3 1 0.021374 0.188633 -0.375091 11.00000 0.01840 0.02459 = 0.02357 -0.00305 0.00347 -0.00253 N1 3 0.312065 0.093896 -0.007018 11.00000 0.01535 0.02099 = 0.02782 0.00121 0.00726 -0.00217 N2 3 0.202249 0.000000 0.024444 10.50000 0.01212 0.02117 = 0.02736 0.00000 0.00744 0.00000 O1 4 0.200878 0.169026 -0.115664 11.00000 0.01394 0.02260 = 0.02706 0.00519 0.00064 0.00044 F1 5 0.106922 0.094745 -0.444502 11.00000 0.02608 0.03327 = 0.03797 -0.01384 -0.00390 0.00824 F2 5 0.114544 0.242107 -0.495129 11.00000 0.02078 0.04798 = 0.03392 0.01949 0.00227 -0.00409 F3 5 0.001706 0.119255 -0.254646 11.00000 0.02172 0.05308 = 0.02963 0.01586 -0.00331 -0.01122 F4 5 0.010874 0.267880 -0.271932 11.00000 0.02615 0.04296 = 0.04970 -0.02278 -0.00561 0.01206 P1 6 0.348161 0.000000 -0.031009 10.50000 0.01311 0.02296 = 0.01724 0.00000 0.00372 0.00000 P2 6 0.240833 0.094221 0.047227 11.00000 0.01347 0.01756 = 0.01884 0.00024 0.00274 0.00028 CL1 7 0.378333 0.000000 -0.330297 10.50000 0.02348 0.04440 = 0.01903 0.00000 0.00780 0.00000 CL2 7 0.434861 0.000000 0.190306 10.50000 0.01363 0.04116 = 0.02082 0.00000 0.00114 0.00000 CL3 7 0.244765 0.145458 0.363466 11.00000 0.02651 0.02608 = 0.02231 -0.00374 0.00621 0.00009 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 Covalent radii and connectivity table for 2007src0193 in C2/m C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 P 1.100 CL 0.990 C1 - O1 C2 C2 - F1 F2 C1 C3 C3 - F4 F3 C2 C3_$1 N1 - P1 P2 N2 - P2 P2_$2 O1 - C1 P2 F1 - C2 F2 - C2 F3 - C3 F4 - C3 P1 - N1_$2 N1 Cl1 Cl2 P2 - O1 N2 N1 Cl3 Cl1 - P1 Cl2 - P1 Cl3 - P2 Operators for generating equivalent atoms: $1 -x, y, -z-1 $2 x, -y, z 9089 Reflections read, of which 3 rejected -27 =< h =< 27, -18 =< k =< 18, -7 =< l =< 7, Max. 2-theta = 54.99 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -6 0 1 108.78 2.33 6 45.58 -4 0 1 30.02 0.65 7 10.16 9 1 1 140.39 3.78 10 27.18 -17 3 1 31.86 2.04 6 12.35 -9 11 1 4.48 0.93 2 8.10 1 1 3 81.13 1.78 9 20.76 8 2 3 241.73 11.43 7 57.95 -1 3 3 41.16 1.39 7 12.49 -10 4 3 84.93 2.88 5 55.73 5 5 3 185.04 7.39 5 57.41 -12 6 3 116.84 5.42 4 31.60 2 6 3 25.87 1.54 6 9.22 -6 8 3 206.66 3.88 7 29.09 -7 11 3 105.61 6.00 3 66.22 14 Inconsistent equivalents 2099 Unique reflections, of which 0 suppressed R(int) = 0.0447 R(sigma) = 0.0356 Friedel opposites merged Maximum memory for data reduction = 1206 / 24379 Special position constraints for N2 y = 0.0000 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for P1 y = 0.0000 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Cl1 y = 0.0000 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Cl2 y = 0.0000 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 1522 / 160787 wR2 = 0.2484 before cycle 1 for 2099 data and 124 / 124 parameters GooF = S = 1.156; Restrained GooF = 1.156 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0838 * P )^2 + 63.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29316 0.00166 -0.005 OSF Mean shift/esd = 0.002 Maximum = 0.006 for U13 P2 Max. shift = 0.000 A for C2 Max. dU = 0.000 for C1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1522 / 160787 wR2 = 0.2484 before cycle 2 for 2099 data and 124 / 124 parameters GooF = S = 1.156; Restrained GooF = 1.156 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0838 * P )^2 + 63.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29316 0.00166 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.002 for U13 P2 Max. shift = 0.000 A for C2 Max. dU = 0.000 for F1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1522 / 160787 wR2 = 0.2484 before cycle 3 for 2099 data and 124 / 124 parameters GooF = S = 1.156; Restrained GooF = 1.156 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0838 * P )^2 + 63.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29316 0.00166 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U23 Cl3 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1522 / 160787 wR2 = 0.2484 before cycle 4 for 2099 data and 124 / 124 parameters GooF = S = 1.156; Restrained GooF = 1.156 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0838 * P )^2 + 63.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29316 0.00166 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C1 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 H1A 0.1282 0.2488 -0.0497 23 0.990 0.000 C1 O1 C2 H1B 0.1177 0.1407 -0.0091 23 0.990 0.000 C1 O1 C2 2007src0193 in C2/m ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.13343 0.18618 -0.10997 1.00000 0.01522 0.02240 0.03143 -0.00142 -0.00214 0.00357 0.02403 0.01377 0.00034 0.00053 0.00137 0.00000 0.00308 0.00347 0.00386 0.00298 0.00277 0.00266 0.00150 H1A 0.12821 0.24882 -0.04969 1.00000 0.02884 0.00000 0.00000 H1B 0.11770 0.14069 -0.00909 1.00000 0.02884 0.00000 0.00000 C2 0.09521 0.17729 -0.35745 1.00000 0.01936 0.02056 0.02800 0.00321 0.00669 0.00082 0.02238 0.01436 0.00035 0.00051 0.00134 0.00000 0.00321 0.00331 0.00366 0.00287 0.00275 0.00262 0.00143 C3 0.02137 0.18863 -0.37509 1.00000 0.01840 0.02459 0.02358 -0.00304 0.00348 -0.00253 0.02232 0.01322 0.00034 0.00053 0.00125 0.00000 0.00323 0.00360 0.00362 0.00282 0.00277 0.00270 0.00146 N1 0.31206 0.09390 -0.00702 1.00000 0.01536 0.02099 0.02782 0.00122 0.00726 -0.00217 0.02099 0.01161 0.00028 0.00043 0.00111 0.00000 0.00263 0.00291 0.00307 0.00245 0.00234 0.00219 0.00123 N2 0.20225 0.00000 0.02444 0.50000 0.01212 0.02116 0.02736 0.00000 0.00744 0.00000 0.01973 0.01377 0.00039 0.00000 0.00157 0.00000 0.00351 0.00415 0.00436 0.00000 0.00319 0.00000 0.00169 O1 0.20088 0.16903 -0.11566 1.00000 0.01394 0.02259 0.02706 0.00519 0.00063 0.00043 0.02173 0.00954 0.00023 0.00036 0.00091 0.00000 0.00221 0.00254 0.00263 0.00208 0.00194 0.00187 0.00107 F1 0.10692 0.09475 -0.44450 1.00000 0.02608 0.03327 0.03798 -0.01384 -0.00390 0.00824 0.03398 0.00875 0.00023 0.00035 0.00089 0.00000 0.00227 0.00260 0.00270 0.00216 0.00201 0.00196 0.00117 F2 0.11454 0.24211 -0.49513 1.00000 0.02078 0.04798 0.03392 0.01948 0.00228 -0.00409 0.03472 0.00971 0.00022 0.00038 0.00087 0.00000 0.00219 0.00304 0.00257 0.00231 0.00190 0.00204 0.00120 F3 0.00171 0.11926 -0.25464 1.00000 0.02172 0.05306 0.02963 0.01586 -0.00331 -0.01122 0.03606 0.00943 0.00023 0.00040 0.00085 0.00000 0.00219 0.00323 0.00250 0.00229 0.00184 0.00215 0.00124 F4 0.01087 0.26788 -0.27193 1.00000 0.02615 0.04294 0.04972 -0.02278 -0.00561 0.01205 0.04156 0.00944 0.00024 0.00039 0.00100 0.00000 0.00241 0.00308 0.00317 0.00259 0.00222 0.00219 0.00139 P1 0.34816 0.00000 -0.03101 0.50000 0.01311 0.02296 0.01725 0.00000 0.00373 0.00000 0.01769 0.00391 0.00012 0.00000 0.00043 0.00000 0.00106 0.00125 0.00114 0.00000 0.00088 0.00000 0.00054 P2 0.24083 0.09422 0.04723 1.00000 0.01347 0.01756 0.01884 0.00024 0.00275 0.00028 0.01672 0.00324 0.00008 0.00012 0.00030 0.00000 0.00077 0.00082 0.00082 0.00065 0.00061 0.00061 0.00041 Cl1 0.37833 0.00000 -0.33030 0.50000 0.02349 0.04439 0.01903 0.00000 0.00780 0.00000 0.02848 0.00416 0.00013 0.00000 0.00044 0.00000 0.00121 0.00159 0.00115 0.00000 0.00095 0.00000 0.00061 Cl2 0.43486 0.00000 0.19031 0.50000 0.01363 0.04116 0.02082 0.00000 0.00114 0.00000 0.02556 0.00380 0.00011 0.00000 0.00044 0.00000 0.00103 0.00148 0.00113 0.00000 0.00085 0.00000 0.00058 Cl3 0.24477 0.14546 0.36347 1.00000 0.02651 0.02608 0.02231 -0.00374 0.00621 0.00008 0.02480 0.00337 0.00009 0.00013 0.00030 0.00000 0.00087 0.00087 0.00085 0.00068 0.00066 0.00068 0.00044 Final Structure Factor Calculation for 2007src0193 in C2/m Total number of l.s. parameters = 124 Maximum vector length = 511 Memory required = 1398 / 26061 wR2 = 0.2484 before cycle 5 for 2099 data and 0 / 124 parameters GooF = S = 1.156; Restrained GooF = 1.156 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0838 * P )^2 + 63.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0840 for 1966 Fo > 4sig(Fo) and 0.0870 for all 2099 data wR2 = 0.2484, GooF = S = 1.156, Restrained GooF = 1.156 for all data Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 2.00 for hydrogen atoms Principal mean square atomic displacements U 0.0366 0.0226 0.0129 C1 0.0293 0.0194 0.0185 C2 0.0272 0.0225 0.0173 C3 0.0281 0.0217 0.0131 N1 0.0275 0.0212 0.0105 N2 0.0318 0.0200 0.0134 O1 0.0593 0.0222 0.0205 F1 0.0639 0.0209 0.0194 F2 0.0683 0.0224 0.0174 F3 0.0808 0.0244 0.0195 F4 0.0230 0.0173 0.0129 P1 0.0191 0.0176 0.0135 P2 0.0444 0.0247 0.0163 Cl1 0.0412 0.0222 0.0133 Cl2 0.0284 0.0265 0.0195 Cl3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.034 0.051 0.069 0.089 0.113 0.141 0.182 0.251 1.000 Number in group 210. 218. 205. 210. 206. 214. 209. 209. 208. 210. GooF 1.476 1.380 1.403 0.871 1.004 1.182 0.973 0.955 1.005 1.119 K 13.679 2.662 1.643 1.132 1.111 1.095 1.040 1.019 1.018 0.998 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.33 1.68 inf Number in group 218. 204. 213. 206. 208. 210. 209. 210. 210. 211. GooF 0.792 1.034 0.823 0.956 0.904 1.294 1.211 1.581 1.561 1.094 K 1.047 1.081 1.013 1.038 1.013 1.046 1.009 1.038 1.024 1.021 R1 0.109 0.117 0.087 0.090 0.079 0.091 0.090 0.099 0.090 0.060 Recommended weighting scheme: WGHT 0.0838 63.8587 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) -8 10 4 6084.51 26.23 9.42 0.017 1.00 -8 2 4 7914.56 1120.21 9.23 0.111 1.36 -4 0 4 7625.88 197.11 8.36 0.047 1.47 -5 5 4 9253.47 2121.47 7.54 0.153 1.30 -6 6 4 6963.20 1325.25 7.35 0.121 1.24 -11 1 4 1482.97 0.68 6.90 0.003 1.27 -4 8 4 3440.64 153.22 6.25 0.041 1.14 -8 12 4 1396.22 7.25 6.06 0.009 0.91 -9 1 4 10496.40 4443.48 5.91 0.221 1.35 3 5 4 1283.90 10.69 5.82 0.011 1.23 -14 6 4 3387.97 504.06 5.75 0.074 1.04 18 0 4 2691.28 97.54 5.60 0.033 0.81 4 4 4 1397.63 100.58 5.39 0.033 1.24 -22 6 4 1932.66 79.70 5.37 0.030 0.82 8 4 4 1162.27 27.12 5.27 0.017 1.10 -2 0 1 40063.42 76490.84 5.09 0.917 5.55 0 0 4 1771.07 224.09 4.94 0.050 1.44 -7 3 4 1586.44 228.96 4.93 0.050 1.36 -15 3 4 1920.97 413.62 4.70 0.067 1.09 -9 7 4 1599.49 166.98 4.60 0.043 1.13 5 5 4 671.60 1.54 4.57 0.004 1.17 5 7 4 1256.46 190.21 4.44 0.046 1.09 7 11 4 1193.33 206.42 4.19 0.048 0.89 -15 9 4 621.94 16.64 4.13 0.014 0.92 -18 10 4 1293.72 148.18 4.00 0.040 0.82 -9 11 4 2198.84 762.19 3.88 0.091 0.94 -2 10 4 1826.42 606.37 3.85 0.082 1.03 4 0 4 2270.04 583.95 3.81 0.080 1.32 -12 0 4 4528.99 2125.52 3.74 0.153 1.24 1 11 4 2022.16 761.82 3.73 0.091 0.97 -11 13 4 512.36 2.46 3.73 0.005 0.84 -17 5 4 457.37 0.72 3.67 0.003 0.98 -5 15 4 510.10 0.78 3.66 0.003 0.81 -1 1 4 869.05 177.91 3.59 0.044 1.46 -6 2 4 551.20 59.41 3.51 0.026 1.41 -13 5 4 6459.48 3577.18 3.34 0.198 1.10 14 4 4 2193.39 781.53 3.27 0.093 0.90 -13 3 4 1965.95 850.98 3.26 0.097 1.16 -16 2 4 917.93 238.05 3.26 0.051 1.06 14 2 4 895.86 213.76 3.21 0.048 0.93 -16 10 4 656.52 14.72 3.20 0.013 0.86 4 8 4 1701.91 690.59 3.19 0.087 1.07 2 4 0 51322.19 37313.38 3.17 0.640 3.42 9 11 4 546.54 54.14 3.16 0.024 0.85 12 0 4 6709.49 3896.43 3.12 0.207 1.00 2 14 4 383.93 9.73 3.11 0.010 0.83 -4 6 4 2000.72 887.40 3.10 0.099 1.26 -20 6 4 2859.71 1423.88 3.06 0.125 0.87 -12 8 4 2188.48 967.25 3.03 0.103 1.02 -5 3 4 300.65 7.48 3.00 0.009 1.40 Bond lengths and angles C1 - Distance Angles O1 1.4389 (0.0082) C2 1.5186 (0.0104) 106.53 (0.61) C1 - O1 C2 - Distance Angles F1 1.3452 (0.0087) F2 1.3584 (0.0085) 106.63 (0.62) C1 1.5186 (0.0104) 110.02 (0.60) 110.81 (0.62) C3 1.5340 (0.0097) 109.28 (0.60) 107.80 (0.59) 112.12 (0.61) C2 - F1 F2 C1 C3 - Distance Angles F4 1.3401 (0.0089) F3 1.3451 (0.0089) 107.68 (0.63) C2 1.5340 (0.0097) 108.59 (0.59) 107.33 (0.60) C3_$1 1.5580 (0.0142) 108.35 (0.47) 108.84 (0.52) 115.77 (0.76) C3 - F4 F3 C2 N1 - Distance Angles P1 1.5773 (0.0063) P2 1.5870 (0.0059) 120.48 (0.39) N1 - P1 N2 - Distance Angles P2 1.5780 (0.0043) P2_$2 1.5780 (0.0043) 119.95 (0.51) N2 - P2 O1 - Distance Angles C1 1.4389 (0.0082) P2 1.5702 (0.0052) 120.25 (0.47) O1 - C1 F1 - Distance Angles C2 1.3452 (0.0087) F1 - F2 - Distance Angles C2 1.3584 (0.0086) F2 - F3 - Distance Angles C3 1.3451 (0.0088) F3 - F4 - Distance Angles C3 1.3401 (0.0089) F4 - P1 - Distance Angles N1_$2 1.5773 (0.0063) N1 1.5773 (0.0063) 119.36 (0.44) Cl1 1.9971 (0.0036) 108.95 (0.25) 108.95 (0.25) Cl2 2.0018 (0.0034) 109.04 (0.25) 109.04 (0.25) 99.69 (0.15) P1 - N1_$2 N1 Cl1 P2 - Distance Angles O1 1.5702 (0.0052) N2 1.5780 (0.0043) 110.41 (0.35) N1 1.5870 (0.0059) 106.26 (0.31) 117.68 (0.36) Cl3 1.9963 (0.0025) 103.26 (0.22) 108.83 (0.34) 109.43 (0.25) P2 - O1 N2 N1 Cl1 - Distance Angles P1 1.9971 (0.0036) Cl1 - Cl2 - Distance Angles P1 2.0018 (0.0034) Cl2 - Cl3 - Distance Angles P2 1.9963 (0.0025) Cl3 - FMAP and GRID set by program FMAP 2 3 17 GRID -3.571 -1 -1 3.571 1 1 R1 = 0.0867 for 2099 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.75 at 0.1510 0.5000 0.2449 [ 0.87 A from CL1 ] Deepest hole -0.84 at 0.3565 0.5000 0.1152 [ 1.33 A from N2 ] Mean = 0.00, Rms deviation from mean = 0.22 e/A^3, Highest memory used = 2258 / 22180 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3490 0.0000 -0.2449 0.50000 0.05 1.75 0.87 CL1 1.27 P1 2.21 N1 2.81 CL2 Q2 1 0.4355 0.0000 0.4690 0.50000 0.05 1.69 1.64 CL2 1.85 CL1 3.02 CL2 3.66 N1 Q3 1 0.2413 0.0965 0.2966 1.00000 0.05 1.67 0.81 CL3 1.47 P2 2.16 N2 2.55 N1 Q4 1 0.2417 0.0957 -0.2176 1.00000 0.05 1.66 1.56 O1 1.57 P2 1.72 N1 2.27 N2 Q5 1 0.3483 0.0000 0.2632 0.50000 0.05 1.61 1.74 P1 1.95 CL2 2.11 N1 2.35 CL1 Q6 1 0.4336 0.0000 -0.0548 0.50000 0.05 1.51 1.44 CL2 1.79 CL1 1.82 P1 2.95 N1 Q7 1 0.3493 0.0000 -0.4852 0.50000 0.05 1.50 0.99 CL1 2.69 P1 2.88 CL2 3.04 CL3 Q8 1 0.3792 0.0000 -0.6118 0.50000 0.05 1.49 1.67 CL1 1.81 CL2 2.43 P1 2.81 N1 Q9 1 0.3766 0.0000 -0.1275 0.50000 0.05 1.45 0.91 P1 1.21 CL1 2.01 CL2 2.14 N1 Q10 1 0.2417 0.0929 0.5395 1.00000 0.05 1.40 1.30 CL3 2.61 O1 2.78 N1 2.84 F1 Q11 1 0.3757 0.0000 0.1151 0.50000 0.05 1.34 0.93 P1 1.22 CL2 1.93 N1 2.64 CL1 Q12 1 0.4341 0.0000 -0.2923 0.50000 0.05 1.28 1.14 CL1 2.60 P1 2.68 CL2 2.85 CL2 Q13 1 0.0000 0.1281 0.0000 0.50000 0.05 1.23 1.52 F3 2.48 H1B 2.51 C3 2.63 F4 Q14 1 0.2495 0.1450 0.6360 1.00000 0.05 1.19 1.59 CL3 1.98 O1 2.36 N1 2.58 P2 Q15 1 0.2464 0.1467 0.1170 1.00000 0.05 1.01 0.86 P2 1.46 CL3 1.53 O1 1.85 N1 Q16 1 0.2473 0.1472 -0.1545 1.00000 0.05 0.95 1.09 O1 1.45 P2 1.64 N1 2.51 C1 Q17 1 0.0000 0.2685 0.0000 0.50000 0.05 0.95 1.67 F4 2.62 C3 2.64 F3 2.77 H1A Q18 1 0.0000 0.1279 -0.5000 0.50000 0.05 0.94 1.18 C3 1.45 F3 2.12 C2 2.24 F1 Q19 1 0.1095 0.2351 -0.7725 1.00000 0.05 0.85 1.62 F2 1.77 H1A 1.99 H1B 2.27 C1 Q20 1 0.1992 0.1703 -0.3620 1.00000 0.05 0.71 1.45 O1 2.06 F2 2.08 CL3 2.18 C2 Shortest distances between peaks (including symmetry equivalents) 1 9 0.80 4 16 0.83 5 8 0.87 10 14 0.94 7 8 1.07 14 20 1.11 5 11 1.14 4 14 1.16 2 8 1.17 6 9 1.18 14 16 1.25 3 15 1.31 6 12 1.41 2 12 1.42 1 7 1.42 3 10 1.43 4 10 1.44 9 11 1.44 16 20 1.45 5 7 1.48 4 20 1.54 8 11 1.60 15 16 1.61 10 20 1.61 9 12 1.70 6 11 1.73 1 12 1.86 2 7 1.88 1 6 1.89 7 12 1.90 10 16 1.95 2 5 1.97 8 12 1.99 13 17 2.04 7 9 2.07 1 11 2.08 4 15 2.09 3 14 2.10 2 11 2.20 1 8 2.38 17 19 2.45 5 9 2.50 7 11 2.53 3 20 2.59 10 15 2.64 2 2 2.64 7 10 2.65 1 4 2.67 3 5 2.68 10 10 2.69 1 10 2.70 6 6 2.72 1 2 2.72 3 7 2.74 6 7 2.78 4 4 2.78 3 16 2.79 3 3 2.80 15 20 2.82 2 6 2.82 5 6 2.85 5 12 2.86 14 15 2.86 13 19 2.86 3 4 2.87 8 9 2.87 19 20 2.90 2 9 2.90 1 5 2.90 11 12 2.92 1 14 2.94 13 18 2.95 15 16 3.00 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.01: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.01: 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. 2.49: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.52: Structure factors and derivatives 0.60: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.27: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.10: Analysis of variance 0.04: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.02: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0193 finished at 17:06:58 Total CPU time: 4.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++