+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 16:13:12 on 08-Aug-2000 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P2(1)/c CELL 0.71073 7.1328 20.6990 7.1455 90.000 116.173 90.000 ZERR 2.00 0.0014 0.0041 0.0014 0.000 0.030 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O CL PD UNIT 24 36 12 12 4 2 V = 946.80 F(000) = 520.0 Mu = 1.30 mm-1 Cell Wt = 1039.25 Rho = 1.823 MERG 2 ACTA FMAP 2 PLAN 20 BOND L.S. 1 WGHT 0.023900 1.105200 EXTI 0.004848 FVAR 0.40217 C6 1 0.461188 0.570075 0.838750 11.00000 0.01562 0.03264 = 0.03066 -0.00872 0.00863 -0.00207 H4A 2 0.538900 0.669425 1.078359 11.00000 0.01816 H6C 2 0.560058 0.564418 0.981144 11.00000 0.04177 H5A 2 0.574669 0.681734 1.419088 11.00000 0.01653 H6B 2 0.437178 0.530467 0.773934 11.00000 0.03926 H5B 2 0.340356 0.675072 1.342332 11.00000 0.02647 H4B 2 0.400297 0.724392 1.079591 11.00000 0.02086 H3 2 -0.210589 0.602496 0.654231 11.00000 0.02468 H6A 2 0.523288 0.599673 0.779254 11.00000 0.04685 H3O 2 0.384700 0.579318 1.332293 11.00000 0.02480 MOLE 1 PD1 6 0.000000 0.500000 0.500000 10.50000 0.01185 0.01505 = 0.01120 -0.00148 0.00443 -0.00235 CL1 5 0.010349 0.568566 0.251758 11.00000 0.02916 0.02919 = 0.01928 0.00591 0.00948 -0.00747 N2 3 0.246966 0.647718 0.935168 11.00000 0.01756 0.01719 = 0.01273 -0.00107 0.00415 -0.00340 O3 4 0.482196 0.592504 1.346376 11.00000 0.02101 0.02477 = 0.02717 0.00305 0.00477 -0.00313 N3 3 0.074495 0.573460 0.703214 11.00000 0.01583 0.01634 = 0.01470 -0.00072 0.00494 -0.00188 O1 4 -0.245072 0.707736 0.867426 11.00000 0.03128 0.03355 = 0.04210 -0.00019 0.01827 0.01278 N1 3 -0.053659 0.707238 0.939365 11.00000 0.03357 0.01954 = 0.02232 -0.00017 0.01111 0.00655 C2 1 0.263713 0.596267 0.827835 11.00000 0.01668 0.01890 = 0.01405 -0.00096 0.00555 -0.00351 C1 1 0.035796 0.656297 0.873096 11.00000 0.02066 0.01521 = 0.01563 0.00189 0.00847 0.00260 C3 1 -0.068462 0.610418 0.729869 11.00000 0.01353 0.01996 = 0.01580 0.00114 0.00573 0.00098 C5 1 0.451004 0.660262 1.316993 11.00000 0.02275 0.02325 = 0.01886 -0.00497 0.00466 -0.00493 C4 1 0.425781 0.680443 1.103149 11.00000 0.02281 0.02083 = 0.02143 -0.00512 0.00673 -0.00997 O2 4 0.061257 0.747798 1.060895 11.00000 0.04750 0.03079 = 0.04247 -0.01901 0.00911 0.00574 HKLF 4 Covalent radii and connectivity table for s92 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 PD 1.380 C6 - C2 Pd1 - N3 N3_$1 Cl1 Cl1_$1 Cl1 - Pd1 N2 - C2 C1 C4 O3 - C5 N3 - C2 C3 Pd1 O1 - N1 N1 - O2 O1 C1 C2 - N3 N2 C6 C1 - C3 N2 N1 C3 - C1 N3 C5 - O3 C4 C4 - N2 C5 O2 - N1 Operators for generating equivalent atoms: $1 -x, -y+1, -z+1 h k l Fo^2 Sigma Why rejected 0 7 0 1.92 0.48 observed but should be systematically absent 0 0 1 1.59 0.37 observed but should be systematically absent 10271 Reflections read, of which 180 rejected -9 =< h =< 9, -26 =< k =< 26, -9 =< l =< 8, Max. 2-theta = 55.02 2 Systematic absence violations 0 Inconsistent equivalents 2165 Unique reflections, of which 0 suppressed R(int) = 0.0487 R(sigma) = 0.0324 Friedel opposites merged Maximum memory for data reduction = 1346 / 21791 Special position constraints for Pd1 x = 0.0000 y = 0.5000 z = 0.5000 sof = 0.50000 Input constraints retained (at least in part) for sof Least-squares cycle 1 Maximum vector length = 511 Memory required = 1729 / 202944 wR2 = 0.0573 before cycle 1 for 2165 data and 161 / 161 parameters GooF = S = 0.961; Restrained GooF = 0.961 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0239 * P )^2 + 1.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40221 0.00071 0.059 OSF 2 0.00484 0.00073 -0.008 EXTI Mean shift/esd = 0.150 Maximum = -0.561 for U23 Cl1 Max. shift = 0.010 A for H6B Max. dU =-0.002 for H5B Largest correlation matrix elements 0.659 U22 Pd1 / OSF 0.591 U13 Pd1 / U33 Pd1 0.504 U13 C1 / U11 C1 0.646 U11 Pd1 / OSF 0.583 U13 Pd1 / U11 Pd1 0.503 U13 Cl1 / U33 Cl1 0.643 U33 Pd1 / OSF 0.544 U13 O1 / U11 O1 0.501 U13 Cl1 / U11 Cl1 0.614 EXTI / OSF 0.540 U13 O1 / U33 O1 s92 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C6 0.46120 0.57005 0.83874 1.00000 0.01561 0.03256 0.03082 -0.00880 0.00835 -0.00194 0.02702 0.00513 0.00036 0.00013 0.00040 0.00000 0.00106 0.00132 0.00127 0.00106 0.00095 0.00095 0.00050 H4A 0.53951 0.66939 1.07864 1.00000 0.01981 0.05275 0.00392 0.00116 0.00390 0.00000 0.00582 H6C 0.56070 0.56428 0.98100 1.00000 0.04234 0.06524 0.00492 0.00141 0.00480 0.00000 0.00811 H5A 0.57549 0.68170 1.41870 1.00000 0.01687 0.05249 0.00380 0.00110 0.00370 0.00000 0.00563 H6B 0.43704 0.53089 0.77467 1.00000 0.03883 0.06853 0.00471 0.00153 0.00481 0.00000 0.00773 H5B 0.34087 0.67483 1.34206 1.00000 0.02476 0.05504 0.00428 0.00121 0.00400 0.00000 0.00663 H4B 0.39944 0.72445 1.07903 1.00000 0.02197 0.05243 0.00385 0.00121 0.00380 0.00000 0.00613 H3 -0.21048 0.60275 0.65424 1.00000 0.02436 0.05611 0.00417 0.00117 0.00404 0.00000 0.00640 H6A 0.52344 0.59991 0.77953 1.00000 0.04659 0.06779 0.00499 0.00151 0.00506 0.00000 0.00874 H3O 0.38481 0.57930 1.33131 1.00000 0.02588 0.06146 0.00461 0.00130 0.00440 0.00000 0.00787 Pd1 0.00000 0.50000 0.50000 0.50000 0.01186 0.01506 0.01121 -0.00149 0.00443 -0.00234 0.01295 0.00000 0.00000 0.00000 0.00000 0.00000 0.00012 0.00013 0.00012 0.00007 0.00008 0.00008 0.00009 Cl1 0.01034 0.56856 0.25178 1.00000 0.02922 0.02918 0.01931 0.00579 0.00948 -0.00739 0.02635 0.00117 0.00009 0.00003 0.00008 0.00000 0.00029 0.00029 0.00024 0.00021 0.00021 0.00023 0.00014 N2 0.24693 0.64771 0.93512 1.00000 0.01756 0.01727 0.01292 -0.00111 0.00422 -0.00325 0.01683 0.00344 0.00027 0.00008 0.00025 0.00000 0.00085 0.00083 0.00077 0.00063 0.00066 0.00066 0.00035 O3 0.48217 0.59252 1.34643 1.00000 0.02102 0.02485 0.02746 0.00294 0.00483 -0.00329 0.02659 0.00370 0.00029 0.00008 0.00026 0.00000 0.00087 0.00085 0.00087 0.00066 0.00070 0.00070 0.00037 N3 0.07451 0.57347 0.70316 1.00000 0.01569 0.01653 0.01458 -0.00083 0.00487 -0.00207 0.01626 0.00349 0.00027 0.00008 0.00025 0.00000 0.00082 0.00082 0.00078 0.00064 0.00066 0.00066 0.00035 O1 -0.24501 0.70772 0.86736 1.00000 0.03143 0.03365 0.04216 -0.00047 0.01866 0.01264 0.03486 0.00398 0.00028 0.00008 0.00029 0.00000 0.00099 0.00094 0.00103 0.00078 0.00084 0.00076 0.00041 N1 -0.05371 0.70726 0.93931 1.00000 0.03373 0.01950 0.02235 -0.00017 0.01129 0.00647 0.02558 0.00437 0.00033 0.00009 0.00030 0.00000 0.00112 0.00095 0.00091 0.00075 0.00083 0.00080 0.00042 C2 0.26373 0.59626 0.82776 1.00000 0.01681 0.01887 0.01425 -0.00075 0.00595 -0.00312 0.01697 0.00418 0.00032 0.00010 0.00031 0.00000 0.00096 0.00096 0.00090 0.00075 0.00077 0.00078 0.00040 C1 0.03585 0.65631 0.87309 1.00000 0.02065 0.01524 0.01562 0.00185 0.00867 0.00289 0.01693 0.00432 0.00032 0.00009 0.00030 0.00000 0.00102 0.00093 0.00091 0.00073 0.00080 0.00078 0.00041 C3 -0.06852 0.61044 0.72986 1.00000 0.01376 0.01979 0.01568 0.00118 0.00551 0.00112 0.01677 0.00440 0.00032 0.00010 0.00031 0.00000 0.00095 0.00101 0.00091 0.00077 0.00078 0.00078 0.00040 C5 0.45107 0.66030 1.31689 1.00000 0.02284 0.02359 0.01869 -0.00492 0.00445 -0.00477 0.02342 0.00455 0.00037 0.00011 0.00034 0.00000 0.00115 0.00110 0.00102 0.00085 0.00090 0.00091 0.00046 C4 0.42578 0.68046 1.10309 1.00000 0.02258 0.02116 0.02121 -0.00505 0.00640 -0.00970 0.02284 0.00444 0.00037 0.00011 0.00034 0.00000 0.00114 0.00113 0.00104 0.00085 0.00089 0.00090 0.00046 O2 0.06130 0.74779 1.06097 1.00000 0.04741 0.03075 0.04285 -0.01915 0.00916 0.00590 0.04426 0.00407 0.00032 0.00009 0.00032 0.00000 0.00117 0.00100 0.00108 0.00084 0.00093 0.00087 0.00051 Final Structure Factor Calculation for s92 in P2(1)/c Total number of l.s. parameters = 161 Maximum vector length = 511 Memory required = 1568 / 25039 wR2 = 0.0572 before cycle 2 for 2165 data and 0 / 161 parameters GooF = S = 0.959; Restrained GooF = 0.959 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0239 * P )^2 + 1.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0229 for 1872 Fo > 4sig(Fo) and 0.0298 for all 2165 data wR2 = 0.0572, GooF = S = 0.959, Restrained GooF = 0.959 for all data Occupancy sum of asymmetric unit = 13.50 for non-hydrogen and 9.00 for hydrogen atoms Principal mean square atomic displacements U 0.0418 0.0239 0.0154 C6 0.0163 0.0125 0.0101 Pd1 0.0414 0.0237 0.0139 Cl1 0.0223 0.0163 0.0119 N2 0.0381 0.0229 0.0188 O3 0.0193 0.0164 0.0130 N3 0.0458 0.0421 0.0167 O1 0.0379 0.0223 0.0165 N1 0.0215 0.0156 0.0138 C2 0.0219 0.0153 0.0135 C1 0.0201 0.0168 0.0134 C3 0.0299 0.0266 0.0138 C5 0.0324 0.0249 0.0113 C4 0.0767 0.0406 0.0155 O2 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 0.053 0.079 0.105 0.133 0.160 0.194 0.249 1.000 Number in group 229. 209. 216. 216. 214. 217. 215. 219. 212. 218. GooF 0.911 0.972 0.879 1.109 0.937 0.920 0.882 0.836 1.056 1.056 K 0.873 0.906 0.971 0.964 0.971 0.986 0.997 1.009 1.013 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.66 inf Number in group 217. 224. 209. 219. 214. 216. 219. 215. 215. 217. GooF 0.939 0.834 0.817 0.885 0.945 0.857 0.886 0.799 0.999 1.457 K 0.961 0.982 1.012 1.005 1.013 1.021 1.019 1.019 1.009 0.994 R1 0.064 0.048 0.044 0.034 0.029 0.023 0.022 0.019 0.018 0.022 Recommended weighting scheme: WGHT 0.0211 0.7089 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) 3 2 1 74.69 34.89 4.82 0.029 1.77 -1 2 2 656.39 520.84 4.59 0.111 3.37 0 2 2 306.61 227.04 4.33 0.074 3.06 0 6 0 204.70 142.72 4.14 0.058 3.45 -3 7 1 1684.79 1951.79 3.74 0.216 1.84 -4 2 1 160.24 218.08 3.68 0.072 1.72 2 1 2 364.43 296.58 3.25 0.084 1.88 -3 19 5 216.71 283.51 3.22 0.082 0.86 0 7 1 6202.38 6787.62 3.14 0.402 2.69 4 4 0 680.34 782.26 2.99 0.136 1.53 3 1 1 3781.21 4171.24 2.98 0.315 1.79 -1 9 2 1080.65 959.13 2.95 0.151 1.93 1 7 2 1802.73 1613.06 2.94 0.196 1.89 -1 0 2 1789.13 2051.09 2.93 0.221 3.56 -1 4 3 223.83 181.48 2.83 0.066 2.15 -1 6 4 70.70 48.81 2.80 0.034 1.56 -2 3 1 2352.54 2596.40 2.80 0.249 3.16 -1 6 7 145.97 198.17 2.80 0.069 0.93 -1 5 1 743.03 846.43 2.79 0.142 3.42 -6 7 6 14.91 41.14 2.79 0.031 0.96 -1 10 1 53.57 76.75 2.76 0.043 1.96 1 10 0 931.47 1040.74 2.72 0.157 1.97 -8 1 4 38.94 1.25 2.70 0.005 0.89 -6 6 6 3719.29 3359.81 2.70 0.283 0.97 4 1 0 53.68 26.96 2.69 0.025 1.60 2 17 5 671.94 786.45 2.69 0.137 0.79 -2 0 2 978.27 1111.57 2.68 0.163 3.03 3 6 1 1768.25 1593.65 2.66 0.195 1.60 -4 5 2 230.30 181.56 2.65 0.066 1.63 1 22 2 2228.94 1972.62 2.61 0.217 0.88 1 7 1 2579.37 2820.27 2.61 0.259 2.33 -6 13 2 423.69 498.06 2.60 0.109 0.95 1 2 1 268.26 222.61 2.58 0.073 3.55 -4 15 2 51.36 74.11 2.53 0.042 1.09 0 10 0 3534.96 3836.59 2.53 0.302 2.07 0 5 1 412.88 472.78 2.52 0.106 3.48 -4 4 9 194.87 276.95 2.52 0.081 0.78 -6 10 8 260.84 369.04 2.52 0.094 0.78 2 0 2 74.46 51.39 2.48 0.035 1.89 -5 10 8 348.37 450.96 2.48 0.104 0.81 -6 1 7 1851.16 1680.38 2.42 0.200 0.92 -8 2 4 1378.67 1222.55 2.42 0.171 0.89 3 1 2 26.12 14.42 2.39 0.019 1.49 -4 15 7 501.86 584.83 2.39 0.118 0.82 0 5 2 685.01 609.40 2.38 0.120 2.53 -8 1 3 1806.68 1624.24 2.38 0.197 0.89 -4 1 8 26.15 53.87 2.38 0.036 0.89 0 20 1 -3.03 4.76 2.37 0.011 1.02 3 23 2 -0.81 25.39 2.36 0.025 0.77 2 8 0 137.06 168.80 2.35 0.063 2.01 Bond lengths and angles C6 - Distance Angles C2 1.4788 (0.0031) C6 - Pd1 - Distance Angles N3 2.0054 (0.0017) N3_$1 2.0054 (0.0017) 180.00 (0.06) Cl1 2.2980 (0.0006) 90.11 (0.05) 89.89 (0.05) Cl1_$1 2.2980 (0.0006) 89.89 (0.05) 90.11 (0.05) 180.00 (0.02) Pd1 - N3 N3_$1 Cl1 Cl1 - Distance Angles Pd1 2.2980 (0.0006) Cl1 - N2 - Distance Angles C2 1.3484 (0.0027) C1 1.3807 (0.0027) 106.09 (0.16) C4 1.4754 (0.0026) 124.32 (0.18) 129.13 (0.18) N2 - C2 C1 O3 - Distance Angles C5 1.4215 (0.0028) O3 - N3 - Distance Angles C2 1.3329 (0.0026) C3 1.3545 (0.0027) 108.04 (0.17) Pd1 2.0054 (0.0017) 128.23 (0.14) 123.70 (0.14) N3 - C2 C3 O1 - Distance Angles N1 1.2278 (0.0027) O1 - N1 - Distance Angles O2 1.2262 (0.0028) O1 1.2278 (0.0027) 124.33 (0.20) C1 1.4181 (0.0027) 119.11 (0.21) 116.56 (0.19) N1 - O2 O1 C2 - Distance Angles N3 1.3329 (0.0026) N2 1.3484 (0.0027) 109.98 (0.18) C6 1.4788 (0.0031) 124.46 (0.19) 125.53 (0.19) C2 - N3 N2 C1 - Distance Angles C3 1.3531 (0.0029) N2 1.3807 (0.0027) 108.10 (0.18) N1 1.4181 (0.0027) 126.56 (0.20) 125.22 (0.18) C1 - C3 N2 C3 - Distance Angles C1 1.3531 (0.0029) N3 1.3545 (0.0027) 107.80 (0.18) C3 - C1 C5 - Distance Angles O3 1.4215 (0.0028) C4 1.5157 (0.0032) 111.27 (0.19) C5 - O3 C4 - Distance Angles N2 1.4754 (0.0026) C5 1.5157 (0.0031) 111.67 (0.18) C4 - N2 O2 - Distance Angles N1 1.2262 (0.0028) O2 - FMAP and GRID set by program FMAP 2 1 22 GRID -2.632 24 -2 2.632 1 2 R1 = 0.0297 for 2165 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.79 at -0.0017 0.5707 0.7550 [ 0.78 A from N3 ] Deepest hole -0.72 at 0.0464 0.5017 0.6366 [ 0.88 A from PD1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 1884 / 25524 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0017 0.5707 0.7550 1.00000 0.05 0.79 0.78 N3 0.93 C3 1.49 H3 1.81 C2 Q2 1 0.0560 0.5501 0.6571 1.00000 0.05 0.52 0.57 N3 1.45 PD1 1.73 C2 1.74 C3 Q3 1 0.1068 0.5426 0.4393 1.00000 0.05 0.39 1.32 CL1 1.36 PD1 2.10 N3 2.52 H6B Q4 1 0.0008 0.6774 0.8966 1.00000 0.05 0.32 0.56 C1 0.85 N1 1.75 C3 1.76 N2 Q5 1 0.1575 0.5793 0.7671 1.00000 0.05 0.32 0.58 N3 0.77 C2 1.65 C3 1.78 N2 Q6 1 0.1569 0.4512 0.5215 1.00000 0.05 0.32 1.46 PD1 1.80 N3 1.84 H3 2.06 C3 Q7 1 -0.0687 0.5380 0.5912 1.00000 0.05 0.31 1.23 N3 1.25 PD1 1.80 C3 1.85 H3 Q8 1 0.3154 0.6598 1.0015 1.00000 0.05 0.31 0.57 N2 0.91 C4 1.46 H4A 1.47 H4B Q9 1 0.2585 0.6255 0.8815 1.00000 0.05 0.31 0.63 N2 0.73 C2 1.69 C1 1.74 N3 Q10 1 -0.0256 0.6287 0.8166 1.00000 0.05 0.30 0.67 C3 0.72 C1 1.42 H3 1.73 N3 Q11 1 -0.0782 0.5309 0.3134 1.00000 0.05 0.29 1.20 CL1 1.36 PD1 2.16 N3 2.65 N3 Q12 1 0.1448 0.6504 0.9272 1.00000 0.05 0.27 0.71 N2 0.71 C1 1.74 C2 1.76 C3 Q13 1 0.1619 0.7520 1.0022 1.00000 0.05 0.27 0.98 O2 1.64 H4B 1.68 N1 2.20 C1 Q14 1 0.7665 0.5968 1.1654 1.00000 0.05 0.26 1.62 H6C 1.67 CL1 2.09 H4A 2.45 C6 Q15 1 0.1633 0.4792 0.6622 1.00000 0.05 0.26 1.30 PD1 1.89 CL1 2.05 H6B 2.11 N3 Q16 1 0.7373 0.6509 1.0605 1.00000 0.05 0.25 1.52 H4A 1.86 O1 2.12 H6C 2.18 H6A Q17 1 0.0097 0.7418 0.9360 1.00000 0.05 0.24 0.81 O2 0.85 N1 1.80 O1 1.86 C1 Q18 1 0.5020 0.5914 0.6459 1.00000 0.05 0.24 0.92 H6A 1.59 C6 1.73 H6B 2.04 H3 Q19 1 0.4420 0.4940 0.7656 1.00000 0.05 0.24 0.77 H6B 1.65 C6 2.01 H6C 2.13 O3 Q20 1 -0.0992 0.5734 0.2599 1.00000 0.05 0.23 0.81 CL1 2.16 PD1 2.37 H6C 2.85 N3 Shortest distances between peaks (including symmetry equivalents) 11 15 0.73 6 7 0.80 2 7 0.84 11 20 0.94 13 17 1.00 2 5 1.00 14 20 1.02 1 2 1.05 8 9 1.05 4 12 1.10 8 12 1.11 1 5 1.11 9 12 1.12 4 10 1.13 6 15 1.14 10 12 1.21 3 11 1.25 1 7 1.25 5 9 1.26 14 16 1.31 1 10 1.32 4 17 1.36 15 20 1.39 2 6 1.49 6 11 1.56 3 20 1.60 2 15 1.65 7 15 1.67 3 7 1.69 2 11 1.69 7 11 1.72 2 3 1.75 5 7 1.77 11 14 1.78 3 15 1.79 5 10 1.81 15 19 1.82 1 6 1.85 6 20 1.85 9 10 1.87 4 13 1.87 5 12 1.89 14 15 1.92 7 15 1.93 7 11 1.96 3 15 1.96 3 6 1.97 3 7 1.99 1 9 2.02 3 6 2.02 1 12 2.05 4 8 2.06 16 20 2.12 12 17 2.14 12 13 2.16 4 9 2.17 2 3 2.19 6 19 2.20 8 13 2.20 2 15 2.21 2 10 2.21 5 15 2.21 2 11 2.24 2 9 2.25 5 8 2.28 6 14 2.28 1 11 2.29 8 10 2.29 18 19 2.30 3 5 2.33 6 11 2.36 5 11 2.36 5 6 2.37 7 20 2.40 7 10 2.40 3 11 2.41 1 4 2.43 11 19 2.45 10 17 2.47 1 15 2.47 7 7 2.50 2 6 2.50 6 15 2.52 11 15 2.56 2 7 2.57 14 19 2.58 2 20 2.60 7 20 2.60 6 7 2.60 15 15 2.60 3 14 2.61 2 20 2.61 8 17 2.64 1 3 2.66 4 16 2.67 4 5 2.67 3 19 2.69 5 19 2.69 3 3 2.71 2 12 2.71 11 11 2.71 6 10 2.73 3 18 2.73 19 20 2.75 1 3 2.75 2 19 2.77 7 19 2.84 1 8 2.85 8 16 2.85 1 15 2.87 2 2 2.90 10 13 2.91 6 6 2.93 9 13 2.93 10 16 2.95 16 18 2.95 5 18 2.95 7 9 2.96 9 18 2.99 7 14 2.99 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.06: 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. 5.05: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.11: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.29: Structure factors and derivatives 1.14: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.22: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.33: Analysis of variance 0.22: Merge reflections for Fourier and .fcf 0.25: Fourier summations 0.23: Peaksearch 0.06: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 16:13:21 Total CPU time: 9.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++