+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007may0020 started at 11:48:47 on 05-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007may0020 in P2(1)/c CELL 0.71073 5.1078 5.8535 16.0142 90.000 90.624 90.000 ZERR 4.00 0.0004 0.0005 0.0014 0.000 0.005 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O UNIT 20 16 12 V = 478.77 F(000) = 232.0 Mu = 0.13 mm-1 Cell Wt = 448.33 Rho = 1.555 MERG 2 OMIT -3.00 55.00 OMIT 1 0 2 OMIT 1 0 4 OMIT 0 2 0 EXTI 0.07414 EQIV $1 -x + 1, -y + 2, -z HTAB O1 O2_$1 DFIX 0.84 0.02 O1 H1O FMAP 2 PLAN 5 SIZE 0.02 0.12 0.22 ACTA BOND $H WGHT 0.04510 0.24200 L.S. 6 TEMP -153.00 FVAR 1.48537 MOLE 1 C1 1 0.224453 0.877349 0.067209 11.00000 0.02191 0.02084 = 0.02282 0.00009 0.00061 0.00088 C2 1 0.018770 0.778542 0.118843 11.00000 0.02103 0.02225 = 0.02151 0.00015 0.00188 0.00102 C3 1 -0.049902 0.555384 0.122706 11.00000 0.02373 0.02344 = 0.02687 0.00013 0.00529 -0.00016 AFIX 43 H3 2 0.031305 0.436141 0.092188 11.00000 -1.20000 AFIX 0 C4 1 -0.308716 0.739048 0.208064 11.00000 0.02538 0.02599 = 0.03009 -0.00162 0.00785 0.00217 AFIX 43 H4 2 -0.440529 0.768821 0.248021 11.00000 -1.20000 AFIX 0 C5 1 -0.152640 0.898353 0.174644 11.00000 0.02277 0.02147 = 0.03111 -0.00193 0.00549 0.00172 AFIX 43 H5 2 -0.154787 1.057853 0.185579 11.00000 -1.20000 AFIX 0 O1 3 0.355575 0.724641 0.024093 11.00000 0.02724 0.02026 = 0.03200 -0.00280 0.01217 -0.00005 O2 3 0.268012 1.084201 0.065046 11.00000 0.02728 0.01879 = 0.03217 -0.00025 0.00764 0.00035 O3 3 -0.251118 0.526088 0.176328 11.00000 0.02734 0.02192 = 0.03317 0.00236 0.00733 -0.00199 H1O 2 0.476621 0.787723 -0.006214 11.00000 0.05521 HKLF 4 Covalent radii and connectivity table for 2007may0020 in P2(1)/c C 0.770 H 0.320 O 0.660 C1 - O2 O1 C2 C2 - C3 C5 C1 C3 - C2 O3 C4 - C5 O3 C5 - C4 C2 O1 - C1 O2 - C1 O3 - C3 C4 Operators for generating equivalent atoms: $1 -x+1, -y+2, -z 6845 Reflections read, of which 421 rejected -6 =< h =< 6, -7 =< k =< 7, -20 =< l =< 20, 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) 3 3 0 37.35 2.15 8 12.33 4 1 1 14.90 4.26 3 42.48 3 3 3 10.79 2.43 6 24.16 -2 4 3 16.65 8.61 2 200.60 2 4 3 15.92 4.72 3 59.44 2 1 4 12.91 3.76 3 50.27 1 3 4 8.73 1.87 7 22.29 3 3 4 3.65 0.84 9 13.10 5 1 5 8.02 2.07 8 14.98 -4 4 5 0.56 1.71 7 15.04 4 2 6 13.18 0.96 9 8.38 1 3 6 0.80 2.41 5 40.15 2 2 7 5.16 1.46 7 25.39 3 2 7 130.18 4.03 8 22.16 5 2 9 15.35 1.85 6 18.73 15 Inconsistent equivalents 1100 Unique reflections, of which 0 suppressed R(int) = 0.0579 R(sigma) = 0.0879 Friedel opposites merged Maximum memory for data reduction = 884 / 10913 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 = 1073 / 104926 wR2 = 0.1050 before cycle 1 for 1100 data and 78 / 78 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.038 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0451 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.48490 0.00645 -0.074 OSF 2 0.07371 0.01487 -0.029 EXTI Mean shift/esd = 0.094 Maximum = -0.366 for U22 C5 Max. shift = 0.003 A for H1O Max. dU = 0.001 for H1O Least-squares cycle 2 Maximum vector length = 511 Memory required = 1073 / 104926 wR2 = 0.1048 before cycle 2 for 1100 data and 78 / 78 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.035 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.038 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0451 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.48452 0.00644 -0.058 OSF 2 0.07347 0.01483 -0.016 EXTI Mean shift/esd = 0.034 Maximum = -0.129 for U22 C5 Max. shift = 0.001 A for H1O Max. dU = 0.001 for H1O Least-squares cycle 3 Maximum vector length = 511 Memory required = 1073 / 104926 wR2 = 0.1048 before cycle 3 for 1100 data and 78 / 78 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.038 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0451 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.48452 0.00644 0.000 OSF 2 0.07344 0.01482 -0.002 EXTI Mean shift/esd = 0.003 Maximum = 0.016 for U11 H1O Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 4 Maximum vector length = 511 Memory required = 1073 / 104926 wR2 = 0.1048 before cycle 4 for 1100 data and 78 / 78 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.038 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0451 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.48453 0.00644 0.001 OSF 2 0.07345 0.01482 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.005 for U11 C2 Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 5 Maximum vector length = 511 Memory required = 1073 / 104926 wR2 = 0.1048 before cycle 5 for 1100 data and 78 / 78 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.038 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0451 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.48453 0.00644 0.000 OSF 2 0.07345 0.01482 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for U11 O3 Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 6 Maximum vector length = 511 Memory required = 1073 / 104926 wR2 = 0.1048 before cycle 6 for 1100 data and 78 / 78 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.038 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0451 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.48453 0.00644 0.000 OSF 2 0.07345 0.01482 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for U11 O2 Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Largest correlation matrix elements 0.610 EXTI / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.0313 0.4363 0.0922 43 0.950 0.000 C3 C2 O3 H4 -0.4406 0.7689 0.2480 43 0.950 0.000 C4 C5 O3 H5 -0.1547 1.0578 0.1856 43 0.950 0.000 C5 C4 C2 2007may0020 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.22442 0.87731 0.06723 1.00000 0.02176 0.02069 0.02271 0.00003 0.00048 0.00094 0.02172 0.00285 0.00031 0.00029 0.00010 0.00000 0.00079 0.00086 0.00081 0.00062 0.00063 0.00063 0.00038 C2 0.01881 0.77857 0.11883 1.00000 0.02097 0.02211 0.02143 0.00013 0.00173 0.00103 0.02149 0.00283 0.00031 0.00028 0.00010 0.00000 0.00078 0.00085 0.00079 0.00064 0.00062 0.00064 0.00039 C3 -0.04992 0.55547 0.12270 1.00000 0.02365 0.02349 0.02660 0.00002 0.00527 -0.00012 0.02455 0.00305 0.00034 0.00030 0.00010 0.00000 0.00081 0.00087 0.00088 0.00068 0.00066 0.00070 0.00040 H3 0.03126 0.43626 0.09216 1.00000 0.02946 0.00000 0.00000 C4 -0.30876 0.73910 0.20807 1.00000 0.02531 0.02575 0.03017 -0.00180 0.00771 0.00224 0.02702 0.00312 0.00034 0.00030 0.00011 0.00000 0.00082 0.00091 0.00091 0.00069 0.00072 0.00071 0.00042 H4 -0.44062 0.76892 0.24800 1.00000 0.03243 0.00000 0.00000 C5 -0.15260 0.89830 0.17464 1.00000 0.02286 0.02102 0.03108 -0.00190 0.00527 0.00174 0.02495 0.00302 0.00032 0.00029 0.00011 0.00000 0.00083 0.00089 0.00091 0.00070 0.00067 0.00068 0.00041 H5 -0.15469 1.05780 0.18559 1.00000 0.02994 0.00000 0.00000 O1 0.35557 0.72461 0.02408 1.00000 0.02733 0.02027 0.03202 -0.00280 0.01223 -0.00002 0.02645 0.00213 0.00023 0.00020 0.00007 0.00000 0.00067 0.00066 0.00070 0.00049 0.00054 0.00049 0.00035 O2 0.26801 1.08416 0.06504 1.00000 0.02719 0.01857 0.03212 -0.00016 0.00760 0.00024 0.02591 0.00212 0.00023 0.00020 0.00007 0.00000 0.00064 0.00065 0.00068 0.00048 0.00049 0.00049 0.00034 O3 -0.25108 0.52602 0.17633 1.00000 0.02725 0.02185 0.03312 0.00232 0.00735 -0.00188 0.02735 0.00216 0.00024 0.00020 0.00008 0.00000 0.00067 0.00067 0.00070 0.00048 0.00052 0.00049 0.00035 H1O 0.47725 0.78825 -0.00625 1.00000 0.05739 0.04464 0.00428 0.00443 0.00146 0.00000 0.00764 Final Structure Factor Calculation for 2007may0020 in P2(1)/c Total number of l.s. parameters = 78 Maximum vector length = 511 Memory required = 995 / 21973 wR2 = 0.1048 before cycle 7 for 1100 data and 0 / 78 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.038 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0451 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0407 for 836 Fo > 4sig(Fo) and 0.0689 for all 1100 data wR2 = 0.1048, GooF = S = 1.037, Restrained GooF = 1.038 for all data Occupancy sum of asymmetric unit = 8.00 for non-hydrogen and 4.00 for hydrogen atoms Principal mean square atomic displacements U 0.0228 0.0222 0.0201 C1 0.0233 0.0217 0.0195 C2 0.0303 0.0235 0.0199 C3 0.0355 0.0269 0.0187 C4 0.0334 0.0231 0.0183 C5 0.0419 0.0209 0.0165 O1 0.0373 0.0219 0.0185 O2 0.0378 0.0250 0.0193 O3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.023 0.036 0.049 0.067 0.094 0.123 0.165 0.225 1.000 Number in group 120. 108. 103. 110. 109. 113. 107. 112. 108. 110. GooF 0.896 0.985 1.017 1.105 1.089 1.124 1.052 0.973 0.948 1.155 K 16.429 2.541 1.532 1.108 0.984 0.997 0.979 1.006 1.007 1.017 Resolution(A) 0.77 0.80 0.83 0.86 0.91 0.96 1.04 1.14 1.30 1.63 inf Number in group 110. 112. 110. 109. 110. 109. 110. 110. 111. 109. GooF 1.015 1.076 0.964 1.055 0.901 1.004 0.891 0.864 1.231 1.284 K 1.009 1.037 1.023 0.990 1.020 1.001 1.022 1.015 1.087 0.992 R1 0.199 0.138 0.113 0.102 0.082 0.054 0.038 0.035 0.063 0.041 Recommended weighting scheme: WGHT 0.0432 0.2412 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) 1 4 1 63.86 45.75 3.96 0.103 1.40 -4 5 7 2.25 11.65 3.78 0.052 0.81 -1 2 1 275.24 228.87 3.29 0.231 2.51 2 0 8 5021.48 4284.05 3.07 1.000 1.57 5 1 11 0.48 9.45 3.07 0.047 0.82 -1 4 3 23.27 33.02 3.06 0.088 1.36 -1 4 1 35.83 26.26 3.05 0.078 1.40 -1 1 2 325.97 384.61 2.99 0.300 3.48 -5 0 8 0.10 6.09 2.88 0.038 0.91 0 2 5 104.77 86.60 2.76 0.142 2.16 2 1 2 158.96 188.01 2.72 0.209 2.24 1 4 0 47.74 37.39 2.71 0.093 1.41 -3 0 4 820.03 711.14 2.70 0.407 1.57 -3 4 11 81.08 62.47 2.70 0.121 0.89 1 2 0 385.57 457.50 2.68 0.327 2.54 -2 1 3 71.59 87.47 2.68 0.143 2.15 0 4 4 37.57 28.83 2.60 0.082 1.37 0 4 3 209.73 179.94 2.59 0.205 1.41 -3 2 8 9.22 4.97 2.57 0.034 1.19 -4 3 6 -0.77 1.99 2.55 0.022 1.00 4 1 2 27.79 37.84 2.51 0.094 1.23 0 1 6 147.71 173.64 2.50 0.201 2.43 5 3 10 13.35 23.28 2.49 0.074 0.78 1 2 4 7.19 3.82 2.48 0.030 2.14 -2 5 14 70.22 53.96 2.46 0.112 0.78 -1 4 16 8.28 2.40 2.46 0.024 0.82 -5 2 5 -0.16 1.46 2.41 0.018 0.93 3 0 12 851.90 742.85 2.39 0.416 1.04 2 2 5 23.47 17.20 2.38 0.063 1.64 -1 2 2 101.94 86.95 2.28 0.142 2.42 -5 0 4 2.35 0.16 2.27 0.006 0.99 -2 0 8 933.20 821.42 2.26 0.438 1.58 -5 4 7 4.43 0.17 2.22 0.006 0.79 2 5 0 18.26 12.54 2.19 0.054 1.06 -4 1 9 2.40 5.10 2.19 0.034 1.03 -1 3 15 9.12 15.15 2.18 0.059 0.92 4 1 13 11.09 17.85 2.18 0.065 0.87 -3 4 8 -1.53 1.65 2.18 0.020 0.97 -1 2 5 60.53 50.80 2.15 0.109 2.00 0 4 7 51.05 61.22 2.13 0.120 1.23 3 0 18 4.91 13.11 2.13 0.055 0.78 -2 2 6 13.01 9.07 2.13 0.046 1.57 5 4 0 -0.57 2.94 2.12 0.026 0.84 -2 2 2 67.87 57.55 2.12 0.116 1.87 -5 1 12 6.89 2.12 2.11 0.022 0.81 3 6 7 1.17 7.18 2.11 0.041 0.79 0 5 9 289.65 255.02 2.10 0.244 0.98 -5 1 5 5.78 9.18 2.10 0.046 0.96 -1 3 8 3.83 1.81 2.07 0.021 1.35 -3 1 5 135.55 154.71 2.07 0.190 1.46 Bond lengths and angles C1 - Distance Angles O2 1.2316 (0.0021) O1 1.3172 (0.0019) 123.99 (0.14) C2 1.4625 (0.0022) 122.40 (0.14) 113.62 (0.14) C1 - O2 O1 C2 - Distance Angles C3 1.3538 (0.0024) C5 1.4401 (0.0022) 106.34 (0.14) C1 1.4625 (0.0022) 126.53 (0.15) 127.12 (0.15) C2 - C3 C5 C3 - Distance Angles C2 1.3538 (0.0024) O3 1.3573 (0.0020) 110.48 (0.14) H3 0.9500 124.76 124.76 C3 - C2 O3 C4 - Distance Angles C5 1.3418 (0.0025) O3 1.3798 (0.0021) 110.53 (0.15) H4 0.9500 124.74 124.74 C4 - C5 O3 C5 - Distance Angles C4 1.3418 (0.0025) C2 1.4401 (0.0022) 106.12 (0.15) H5 0.9500 126.94 126.94 C5 - C4 C2 O1 - Distance Angles C1 1.3172 (0.0019) H1O 0.8762 (0.0168) 111.73 (1.79) O1 - C1 O2 - Distance Angles C1 1.2316 (0.0021) O2 - O3 - Distance Angles C3 1.3573 (0.0020) C4 1.3798 (0.0021) 106.52 (0.13) O3 - C3 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.876(17) 1.779(17) 2.6545(17) 178(3) O1-H1O...O2_$1 FMAP and GRID set by program FMAP 2 1 14 GRID -4.545 -2 -1 4.545 2 1 R1 = 0.0689 for 1100 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.27 at 0.0489 0.3490 0.3614 [ 0.63 A from C2 ] Deepest hole -0.26 at 0.0566 0.4737 0.0880 [ 0.26 A from H3 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 1217 / 15183 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0489 0.8490 0.1386 1.00000 0.05 0.27 0.63 C2 0.84 C5 1.54 H5 1.74 C3 Q2 1 0.1192 0.8167 0.1017 1.00000 0.05 0.27 0.63 C2 0.85 C1 1.79 C3 1.82 O1 Q3 1 -0.0278 0.3780 0.1124 1.00000 0.05 0.25 0.56 H3 1.06 C3 1.77 O3 2.31 H5 Q4 1 -0.4882 0.7019 0.2531 1.00000 0.05 0.22 0.47 H4 1.19 C4 2.02 O3 2.25 H5 Q5 1 -0.6353 0.6508 0.2794 1.00000 0.05 0.18 1.32 H4 1.33 H5 1.98 C5 2.10 C4 Shortest distances between peaks (including symmetry equivalents) 4 5 0.91 1 2 1.06 2 3 2.68 1 5 2.74 4 5 2.75 1 3 2.79 3 5 2.79 4 4 2.93 Time profile in seconds ----------------------- 0.07: Read and process instructions 0.00: Fit rigid groups 0.01: 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. 0.29: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.19: Structure factors and derivatives 0.23: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.13: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007may0020 finished at 11:48:56 Total CPU time: 1.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++