+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 12:25:24 on 06-Jun-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 00tam081 in P2(1)2(1)2(1) CELL 0.71073 8.5829 15.5872 25.2769 90.000 90.000 90.000 ZERR 4.00 0.0017 0.0031 0.0051 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 P S CL UNIT 60 100 36 24 4 32 V = 3381.63 F(000) = 1680.0 Mu = 1.04 mm-1 Cell Wt = 3331.68 Rho = 1.636 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 10 SIZE 0.18 0.20 0.68 ACTA BOND WGHT 0.05470 L.S. 5 TEMP -153.00 FVAR 0.21168 C1 1 0.780275 -0.262163 -0.325940 11.00000 0.04838 0.02311 = 0.02769 0.00442 0.00923 0.00697 C2 1 0.672693 -0.282245 -0.364889 11.00000 0.05581 0.03133 = 0.02981 0.00916 0.00089 0.00606 C3 1 0.727092 -0.292299 -0.416395 11.00000 0.08931 0.03101 = 0.02964 0.00741 -0.00118 0.01028 AFIX 43 H3 2 0.655452 -0.307610 -0.443444 11.00000 -1.20000 AFIX 0 C4 1 0.881922 -0.280716 -0.429406 11.00000 0.10280 0.02186 = 0.04289 0.00874 0.02849 -0.00205 C5 1 0.987843 -0.262762 -0.389650 11.00000 0.06785 0.03273 = 0.07507 0.00535 0.03925 -0.00270 AFIX 43 H5 2 1.095285 -0.256661 -0.397861 11.00000 -1.20000 AFIX 0 C6 1 0.936821 -0.253563 -0.337278 11.00000 0.05743 0.03064 = 0.05347 0.00228 0.00783 -0.00445 AFIX 43 H6 2 1.009276 -0.241528 -0.309853 11.00000 -1.20000 AFIX 0 C7 1 0.502080 -0.290839 -0.354369 11.00000 0.05274 0.07619 = 0.05051 0.00643 -0.01179 0.01269 AFIX 33 H7A 2 0.447992 -0.305203 -0.387345 11.00000 -1.50000 H7B 2 0.461619 -0.236503 -0.340524 11.00000 -1.50000 H7C 2 0.484738 -0.336446 -0.328340 11.00000 -1.50000 AFIX 0 C8 1 0.935805 -0.283515 -0.486723 11.00000 0.17956 0.03889 = 0.05978 0.00314 0.06348 -0.00331 AFIX 33 H8A 2 1.048755 -0.274635 -0.488216 11.00000 -1.50000 H8B 2 0.883276 -0.238203 -0.506829 11.00000 -1.50000 H8C 2 0.910091 -0.339509 -0.502042 11.00000 -1.50000 AFIX 0 C9 1 0.500072 -0.332323 -0.162116 11.00000 0.02608 0.05868 = 0.02623 -0.00934 0.00376 -0.00054 AFIX 23 H9A 2 0.448075 -0.385306 -0.149676 11.00000 -1.20000 H9B 2 0.453580 -0.316342 -0.196578 11.00000 -1.20000 AFIX 0 C10 1 0.471421 -0.261375 -0.122835 11.00000 0.03134 0.04178 = 0.02438 -0.00429 0.00175 0.00487 AFIX 23 H10A 2 0.361092 -0.243319 -0.125397 11.00000 -1.20000 H10B 2 0.536875 -0.211475 -0.132485 11.00000 -1.20000 AFIX 0 C11 1 0.506075 -0.286104 -0.065995 11.00000 0.02496 0.02799 = 0.02812 -0.00048 0.00353 -0.00164 AFIX 23 H11A 2 0.619775 -0.294059 -0.061592 11.00000 -1.20000 H11B 2 0.454432 -0.341315 -0.057787 11.00000 -1.20000 AFIX 0 C12 1 0.449001 -0.217379 -0.027373 11.00000 0.03245 0.03050 = 0.01902 -0.00119 0.00018 0.00244 AFIX 23 H12A 2 0.494635 -0.161376 -0.037435 11.00000 -1.20000 H12B 2 0.334309 -0.212433 -0.030204 11.00000 -1.20000 AFIX 0 C13 1 0.421270 -0.314987 0.049579 11.00000 0.03533 0.02394 = 0.03233 -0.00198 0.00677 -0.00109 AFIX 23 H13A 2 0.308266 -0.305529 0.054835 11.00000 -1.20000 H13B 2 0.433837 -0.361983 0.023581 11.00000 -1.20000 AFIX 0 C14 1 0.490592 -0.340834 0.099444 11.00000 0.30465 0.05625 = 0.04567 0.02603 -0.06771 -0.08365 AFIX 23 H14A 2 0.419222 -0.383616 0.115277 11.00000 -1.20000 H14B 2 0.587822 -0.371830 0.090575 11.00000 -1.20000 AFIX 0 C15 1 0.527451 -0.284289 0.138710 11.00000 0.06312 0.03391 = 0.03663 0.01221 -0.01390 -0.00689 AFIX 23 H15A 2 0.616967 -0.308043 0.158598 11.00000 -1.20000 H15B 2 0.438179 -0.281578 0.163455 11.00000 -1.20000 AFIX 0 N1 3 0.924799 -0.388947 -0.219564 11.00000 0.02869 0.02587 = 0.02964 -0.00530 -0.00170 0.00090 N2 3 0.900275 -0.528214 -0.283929 11.00000 0.05200 0.03766 = 0.04441 -0.01767 -0.00212 0.00552 N3 3 0.646271 -0.430649 -0.263128 11.00000 0.03136 0.03518 = 0.02797 -0.00723 -0.00140 -0.00595 N4 3 0.668689 -0.349414 -0.169390 11.00000 0.03367 0.04132 = 0.01631 -0.00262 -0.00148 0.00947 N5 3 0.491039 -0.236724 0.028143 11.00000 0.04240 0.02041 = 0.02026 0.00019 0.00116 0.00117 N6 3 0.566522 -0.196784 0.123224 11.00000 0.03906 0.02851 = 0.02429 -0.00175 -0.00591 -0.00235 AFIX 43 H6N 2 0.619942 -0.165261 0.145700 11.00000 -1.20000 AFIX 0 N7 3 0.655379 -0.095503 0.042968 11.00000 0.03127 0.02192 = 0.04113 0.00001 0.00518 0.00250 N8 3 0.482849 0.050002 0.035213 11.00000 0.03552 0.02098 = 0.06090 0.00717 0.00576 0.00448 N9 3 0.359449 -0.097056 0.075181 11.00000 0.03071 0.02094 = 0.03413 0.00255 0.00353 0.00376 P1 4 0.743923 -0.364171 -0.227397 11.00000 0.02894 0.02501 = 0.02040 -0.00396 0.00173 -0.00019 P2 4 1.002770 -0.467370 -0.247727 11.00000 0.03609 0.03082 = 0.03057 -0.00476 0.00356 0.00535 P3 4 0.720606 -0.511919 -0.288527 11.00000 0.04722 0.02804 = 0.02525 -0.00604 0.00089 -0.00692 P4 4 0.517490 -0.153770 0.066954 11.00000 0.02785 0.02073 = 0.02395 -0.00163 0.00198 0.00140 P5 4 0.643611 0.001532 0.029415 11.00000 0.02915 0.02389 = 0.03876 0.00062 0.00652 -0.00068 P6 4 0.336773 -0.003313 0.054971 11.00000 0.02727 0.02254 = 0.03134 -0.00087 0.00091 0.00267 S1 5 0.720773 -0.242943 -0.259338 11.00000 0.05059 0.02629 = 0.02810 -0.00024 0.00318 0.00635 CL1 6 1.109939 -0.536975 -0.192199 11.00000 0.06874 0.04977 = 0.05262 0.00190 -0.00763 0.02506 CL2 6 1.186233 -0.429174 -0.290074 11.00000 0.04652 0.06682 = 0.06985 -0.00058 0.02718 0.00548 CL3 6 0.611297 -0.616619 -0.261770 11.00000 0.09875 0.04261 = 0.05008 -0.00158 0.00339 -0.03278 CL4 6 0.662955 -0.516666 -0.365033 11.00000 0.07797 0.04930 = 0.02679 -0.01284 -0.00559 0.00197 CL5 6 0.804172 0.066777 0.069691 11.00000 0.04190 0.04018 = 0.05755 -0.00472 0.00255 -0.01518 CL6 6 0.718293 0.020405 -0.045006 11.00000 0.05931 0.04533 = 0.04193 0.01017 0.01446 0.00464 CL7 6 0.176190 -0.001396 -0.002890 11.00000 0.04441 0.03849 = 0.03595 0.00215 -0.00971 0.00366 CL8 6 0.227754 0.064645 0.110858 11.00000 0.04544 0.03723 = 0.04136 -0.01134 0.00335 0.00995 H4N 2 0.722468 -0.371067 -0.148544 11.00000 0.01804 HKLF 4 Covalent radii and connectivity table for 00tam081 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 P 1.100 S 1.030 CL 0.990 C1 - C6 C2 S1 C2 - C1 C3 C7 C3 - C4 C2 C4 - C3 C5 C8 C5 - C4 C6 C6 - C1 C5 C7 - C2 C8 - C4 C9 - N4 C10 C10 - C9 C11 C11 - C10 C12 C12 - N5 C11 C13 - C14 N5 C14 - C15 C13 C15 - C14 N6 N1 - P2 P1 N2 - P3 P2 N3 - P3 P1 N4 - C9 P1 N5 - C13 C12 P4 N6 - C15 P4 N7 - P5 P4 N8 - P5 P6 N9 - P6 P4 P1 - N3 N1 N4 S1 P2 - N1 N2 Cl2 Cl1 P3 - N3 N2 Cl4 Cl3 P4 - N7 N6 N9 N5 P5 - N7 N8 Cl5 Cl6 P6 - N9 N8 Cl8 Cl7 S1 - C1 P1 Cl1 - P2 Cl2 - P2 Cl3 - P3 Cl4 - P3 Cl5 - P5 Cl6 - P5 Cl7 - P6 Cl8 - P6 20523 Reflections read, of which 38 rejected -11 =< h =< 11, -20 =< k =< 20, -31 =< l =< 32, Max. 2-theta = 54.95 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 6 4 0 144.19 0.74 3 85.36 8 7 0 46.95 1.32 4 13.60 -2 1 1 1974.04 27.85 4 327.10 3 1 1 158.60 0.38 5 74.64 -4 2 1 178.59 4.06 5 21.12 4 2 1 98.77 0.49 3 71.05 -5 3 1 18.65 0.49 5 3.36 -6 4 1 65.27 0.91 5 12.45 6 4 1 64.26 0.71 5 12.46 4 1 2 43.00 0.36 3 20.03 5 2 2 159.20 4.01 4 22.99 -5 3 2 35.53 0.58 4 10.24 -1 5 2 423.36 8.72 4 47.15 -4 2 3 277.68 0.48 7 80.49 1 3 3 64.10 1.62 4 9.06 6 3 3 89.73 0.73 3 57.28 -6 4 3 153.49 1.47 5 26.20 -8 7 3 33.36 0.96 6 5.16 1 9 3 261.72 6.78 4 43.67 2 1 4 227.87 4.98 4 26.64 5 1 4 86.42 0.73 3 38.06 1 2 4 726.40 18.00 3 100.18 6 2 4 196.88 5.55 3 58.20 -5 3 4 135.18 1.67 7 12.02 -1 3 4 616.86 15.20 3 76.34 -6 4 4 80.42 1.00 6 12.33 -2 5 4 371.07 7.99 4 45.42 -1 6 4 192.91 6.85 3 38.26 -9 7 4 6.06 0.76 3 4.49 4 0 5 72.98 0.49 4 22.89 -1 1 5 209.07 6.93 2 40.04 -2 2 5 515.35 12.79 3 64.17 2 3 5 483.77 9.70 4 49.94 -1 4 5 151.39 4.57 3 25.80 1 4 5 126.01 3.00 3 32.09 2 4 5 577.88 13.86 3 76.49 -9 6 6 7.28 0.95 2 6.51 0 6 6 395.71 13.84 2 104.07 1 6 6 138.56 5.20 2 26.25 8 4 7 20.77 1.09 3 8.72 -7 5 7 42.98 1.30 4 10.41 -6 2 8 47.38 1.15 5 6.73 -1 3 8 410.49 12.20 2 93.99 0 8 8 187.33 6.76 2 66.65 -6 1 9 127.77 0.87 5 38.65 -7 4 9 73.57 1.02 5 17.38 -7 2 11 30.64 1.33 3 9.81 -1 2 11 115.98 5.54 2 30.29 -8 4 11 35.81 1.21 4 7.00 3 4 12 307.18 8.00 3 47.31 ** etc. ** 52 Inconsistent equivalents 7560 Unique reflections, of which 0 suppressed R(int) = 0.0819 R(sigma) = 0.0821 Friedel opposites not merged Maximum memory for data reduction = 3031 / 76041 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 = 4005 / 453129 wR2 = 0.1127 before cycle 1 for 7560 data and 356 / 356 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0547 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21173 0.00031 0.147 OSF Mean shift/esd = 0.015 Maximum = 0.147 for OSF Max. shift = 0.001 A for H4N Max. dU = 0.000 for H4N Least-squares cycle 2 Maximum vector length = 511 Memory required = 4005 / 453129 wR2 = 0.1127 before cycle 2 for 7560 data and 356 / 356 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0547 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21173 0.00031 0.015 OSF Mean shift/esd = 0.005 Maximum = 0.022 for U11 P3 Max. shift = 0.000 A for H4N Max. dU = 0.000 for H4N Least-squares cycle 3 Maximum vector length = 511 Memory required = 4005 / 453129 wR2 = 0.1127 before cycle 3 for 7560 data and 356 / 356 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0547 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21173 0.00031 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.004 for y H4N Max. shift = 0.000 A for H4N Max. dU = 0.000 for C14 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4005 / 453129 wR2 = 0.1127 before cycle 4 for 7560 data and 356 / 356 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0547 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21173 0.00031 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.002 for U11 C14 Max. shift = 0.000 A for H4N Max. dU = 0.000 for C14 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4005 / 453129 wR2 = 0.1127 before cycle 5 for 7560 data and 356 / 356 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0547 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21173 0.00031 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U11 C14 Max. shift = 0.000 A for H4N Max. dU = 0.000 for C14 Largest correlation matrix elements -0.567 U12 C14 / U11 C14 Idealized hydrogen atom generation before cycle 6 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.6555 -0.3076 -0.4435 43 0.950 0.000 C3 C4 C2 H5 1.0953 -0.2567 -0.3978 43 0.950 0.000 C5 C4 C6 H6 1.0093 -0.2415 -0.3099 43 0.950 0.000 C6 C1 C5 H7A 0.4480 -0.3052 -0.3874 33 0.980 0.000 C7 C2 H7A H7B 0.4617 -0.2365 -0.3405 33 0.980 0.000 C7 C2 H7A H7C 0.4847 -0.3364 -0.3284 33 0.980 0.000 C7 C2 H7A H8A 1.0488 -0.2747 -0.4882 33 0.980 0.000 C8 C4 H8A H8B 0.8833 -0.2382 -0.5068 33 0.980 0.000 C8 C4 H8A H8C 0.9101 -0.3395 -0.5020 33 0.980 0.000 C8 C4 H8A H9A 0.4481 -0.3853 -0.1497 23 0.990 0.000 C9 N4 C10 H9B 0.4536 -0.3163 -0.1966 23 0.990 0.000 C9 N4 C10 H10A 0.3611 -0.2434 -0.1254 23 0.990 0.000 C10 C9 C11 H10B 0.5368 -0.2115 -0.1325 23 0.990 0.000 C10 C9 C11 H11A 0.6198 -0.2940 -0.0616 23 0.990 0.000 C11 C10 C12 H11B 0.4545 -0.3413 -0.0578 23 0.990 0.000 C11 C10 C12 H12A 0.4946 -0.1614 -0.0374 23 0.990 0.000 C12 N5 C11 H12B 0.3343 -0.2124 -0.0302 23 0.990 0.000 C12 N5 C11 H13A 0.3083 -0.3055 0.0548 23 0.990 0.000 C13 C14 N5 H13B 0.4338 -0.3620 0.0236 23 0.990 0.000 C13 C14 N5 H14A 0.4193 -0.3836 0.1153 23 0.990 0.000 C14 C15 C13 H14B 0.5879 -0.3718 0.0906 23 0.990 0.000 C14 C15 C13 H15A 0.6169 -0.3080 0.1586 23 0.990 0.000 C15 C14 N6 H15B 0.4381 -0.2816 0.1634 23 0.990 0.000 C15 C14 N6 H6N 0.6199 -0.1653 0.1457 43 0.880 0.000 N6 C15 P4 00tam081 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.78027 -0.26216 -0.32594 1.00000 0.04846 0.02306 0.02767 0.00440 0.00929 0.00699 0.03306 0.00741 0.00048 0.00024 0.00016 0.00000 0.00236 0.00197 0.00224 0.00167 0.00180 0.00169 0.00091 C2 0.67267 -0.28225 -0.36489 1.00000 0.05579 0.03134 0.02981 0.00919 0.00091 0.00601 0.03898 0.00804 0.00054 0.00027 0.00017 0.00000 0.00271 0.00228 0.00235 0.00185 0.00198 0.00187 0.00101 C3 0.72711 -0.29227 -0.41639 1.00000 0.08940 0.03101 0.02957 0.00735 -0.00127 0.01028 0.05000 0.00948 0.00068 0.00029 0.00019 0.00000 0.00386 0.00234 0.00251 0.00192 0.00251 0.00240 0.00127 H3 0.65547 -0.30755 -0.44345 1.00000 0.05999 0.00000 0.00000 C4 0.88194 -0.28072 -0.42940 1.00000 0.10268 0.02184 0.04288 0.00876 0.02848 -0.00200 0.05580 0.01077 0.00075 0.00029 0.00021 0.00000 0.00432 0.00232 0.00302 0.00214 0.00313 0.00240 0.00145 C5 0.98788 -0.26277 -0.38964 1.00000 0.06795 0.03270 0.07492 0.00537 0.03917 -0.00268 0.05852 0.01107 0.00067 0.00029 0.00025 0.00000 0.00335 0.00261 0.00396 0.00264 0.00316 0.00240 0.00149 H5 1.09532 -0.25667 -0.39784 1.00000 0.07023 0.00000 0.00000 C6 0.93682 -0.25357 -0.33728 1.00000 0.05761 0.03053 0.05343 0.00226 0.00786 -0.00447 0.04719 0.00888 0.00056 0.00029 0.00021 0.00000 0.00293 0.00241 0.00318 0.00220 0.00232 0.00204 0.00119 H6 1.00927 -0.24154 -0.30985 1.00000 0.05663 0.00000 0.00000 C7 0.50210 -0.29082 -0.35438 1.00000 0.05281 0.07614 0.05055 0.00636 -0.01169 0.01277 0.05983 0.00965 0.00059 0.00037 0.00022 0.00000 0.00307 0.00376 0.00334 0.00289 0.00258 0.00267 0.00143 H7A 0.44802 -0.30518 -0.38736 1.00000 0.08975 0.00000 0.00000 H7B 0.46165 -0.23648 -0.34054 1.00000 0.08975 0.00000 0.00000 H7C 0.48473 -0.33642 -0.32835 1.00000 0.08975 0.00000 0.00000 C8 0.93582 -0.28354 -0.48672 1.00000 0.17995 0.03877 0.05978 0.00320 0.06360 -0.00332 0.09283 0.01368 0.00099 0.00035 0.00025 0.00000 0.00753 0.00307 0.00403 0.00284 0.00470 0.00367 0.00264 H8A 1.04877 -0.27466 -0.48821 1.00000 0.13925 0.00000 0.00000 H8B 0.88329 -0.23824 -0.50683 1.00000 0.13925 0.00000 0.00000 H8C 0.91011 -0.33954 -0.50203 1.00000 0.13925 0.00000 0.00000 C9 0.50009 -0.33232 -0.16211 1.00000 0.02609 0.05874 0.02621 -0.00929 0.00379 -0.00056 0.03701 0.00718 0.00045 0.00030 0.00016 0.00000 0.00201 0.00277 0.00218 0.00197 0.00161 0.00186 0.00097 H9A 0.44811 -0.38531 -0.14967 1.00000 0.04441 0.00000 0.00000 H9B 0.45360 -0.31635 -0.19657 1.00000 0.04441 0.00000 0.00000 C10 0.47140 -0.26139 -0.12283 1.00000 0.03130 0.04172 0.02445 -0.00434 0.00166 0.00484 0.03249 0.00690 0.00045 0.00027 0.00015 0.00000 0.00203 0.00245 0.00215 0.00180 0.00158 0.00170 0.00091 H10A 0.36106 -0.24336 -0.12539 1.00000 0.03899 0.00000 0.00000 H10B 0.53681 -0.21147 -0.13249 1.00000 0.03899 0.00000 0.00000 C11 0.50609 -0.28610 -0.06600 1.00000 0.02491 0.02792 0.02820 -0.00041 0.00352 -0.00163 0.02701 0.00633 0.00040 0.00023 0.00015 0.00000 0.00179 0.00196 0.00208 0.00168 0.00160 0.00146 0.00080 H11A 0.61980 -0.29403 -0.06160 1.00000 0.03241 0.00000 0.00000 H11B 0.45448 -0.34132 -0.05778 1.00000 0.03241 0.00000 0.00000 C12 0.44900 -0.21737 -0.02737 1.00000 0.03248 0.03053 0.01897 -0.00119 0.00016 0.00244 0.02733 0.00659 0.00043 0.00025 0.00014 0.00000 0.00196 0.00210 0.00199 0.00158 0.00149 0.00151 0.00082 H12A 0.49462 -0.16137 -0.03743 1.00000 0.03279 0.00000 0.00000 H12B 0.33430 -0.21243 -0.03020 1.00000 0.03279 0.00000 0.00000 C13 0.42127 -0.31499 0.04958 1.00000 0.03534 0.02393 0.03236 -0.00204 0.00676 -0.00115 0.03055 0.00710 0.00046 0.00024 0.00016 0.00000 0.00203 0.00197 0.00231 0.00169 0.00171 0.00151 0.00087 H13A 0.30827 -0.30553 0.05484 1.00000 0.03666 0.00000 0.00000 H13B 0.43383 -0.36199 0.02358 1.00000 0.03666 0.00000 0.00000 C14 0.49061 -0.34084 0.09944 1.00000 0.30444 0.05624 0.04570 0.02595 -0.06765 -0.08353 0.13546 0.01101 0.00133 0.00041 0.00024 0.00000 0.01311 0.00379 0.00376 0.00318 0.00595 0.00628 0.00457 H14A 0.41927 -0.38364 0.11527 1.00000 0.16255 0.00000 0.00000 H14B 0.58786 -0.37182 0.09057 1.00000 0.16255 0.00000 0.00000 C15 0.52744 -0.28428 0.13871 1.00000 0.06312 0.03393 0.03669 0.01217 -0.01383 -0.00694 0.04458 0.00772 0.00059 0.00027 0.00019 0.00000 0.00290 0.00240 0.00259 0.00208 0.00222 0.00205 0.00111 H15A 0.61693 -0.30803 0.15861 1.00000 0.05350 0.00000 0.00000 H15B 0.43814 -0.28157 0.16344 1.00000 0.05350 0.00000 0.00000 N1 0.92480 -0.38895 -0.21956 1.00000 0.02876 0.02582 0.02959 -0.00531 -0.00173 0.00093 0.02806 0.00531 0.00035 0.00020 0.00013 0.00000 0.00156 0.00167 0.00182 0.00145 0.00136 0.00121 0.00070 N2 0.90029 -0.52820 -0.28393 1.00000 0.05205 0.03765 0.04441 -0.01770 -0.00211 0.00552 0.04470 0.00639 0.00044 0.00024 0.00016 0.00000 0.00221 0.00210 0.00230 0.00179 0.00176 0.00163 0.00094 N3 0.64628 -0.43065 -0.26313 1.00000 0.03133 0.03516 0.02791 -0.00722 -0.00141 -0.00599 0.03147 0.00529 0.00036 0.00021 0.00013 0.00000 0.00157 0.00184 0.00184 0.00148 0.00132 0.00137 0.00072 N4 0.66870 -0.34941 -0.16939 1.00000 0.03361 0.04139 0.01631 -0.00265 -0.00149 0.00948 0.03043 0.00594 0.00040 0.00023 0.00013 0.00000 0.00183 0.00209 0.00174 0.00150 0.00141 0.00149 0.00076 N5 0.49104 -0.23673 0.02814 1.00000 0.04241 0.02039 0.02026 0.00023 0.00114 0.00117 0.02769 0.00531 0.00036 0.00019 0.00012 0.00000 0.00177 0.00157 0.00168 0.00130 0.00136 0.00138 0.00069 N6 0.56652 -0.19678 0.12323 1.00000 0.03905 0.02854 0.02419 -0.00172 -0.00593 -0.00238 0.03060 0.00565 0.00038 0.00021 0.00013 0.00000 0.00184 0.00179 0.00181 0.00139 0.00141 0.00136 0.00076 H6N 0.61994 -0.16526 0.14570 1.00000 0.03672 0.00000 0.00000 N7 0.65538 -0.09550 0.04297 1.00000 0.03129 0.02188 0.04112 0.00002 0.00515 0.00246 0.03143 0.00571 0.00035 0.00019 0.00014 0.00000 0.00168 0.00162 0.00206 0.00148 0.00149 0.00129 0.00075 N8 0.48285 0.05000 0.03521 1.00000 0.03551 0.02098 0.06079 0.00715 0.00580 0.00445 0.03909 0.00638 0.00038 0.00020 0.00016 0.00000 0.00182 0.00166 0.00250 0.00166 0.00166 0.00141 0.00086 N9 0.35946 -0.09706 0.07518 1.00000 0.03065 0.02091 0.03415 0.00259 0.00353 0.00374 0.02857 0.00556 0.00035 0.00018 0.00013 0.00000 0.00159 0.00164 0.00192 0.00141 0.00139 0.00125 0.00071 P1 0.74392 -0.36417 -0.22740 1.00000 0.02897 0.02501 0.02041 -0.00396 0.00172 -0.00019 0.02479 0.00164 0.00011 0.00006 0.00004 0.00000 0.00049 0.00048 0.00049 0.00040 0.00036 0.00036 0.00021 P2 1.00277 -0.46737 -0.24773 1.00000 0.03611 0.03083 0.03057 -0.00476 0.00355 0.00534 0.03250 0.00187 0.00012 0.00006 0.00004 0.00000 0.00054 0.00053 0.00056 0.00045 0.00044 0.00040 0.00024 P3 0.72060 -0.51192 -0.28853 1.00000 0.04727 0.02803 0.02525 -0.00604 0.00089 -0.00692 0.03352 0.00174 0.00013 0.00007 0.00004 0.00000 0.00059 0.00054 0.00053 0.00044 0.00043 0.00046 0.00024 P4 0.51748 -0.15377 0.06695 1.00000 0.02787 0.02073 0.02397 -0.00163 0.00199 0.00141 0.02419 0.00164 0.00011 0.00006 0.00004 0.00000 0.00047 0.00046 0.00052 0.00040 0.00038 0.00035 0.00021 P5 0.64361 0.00153 0.02941 1.00000 0.02916 0.02389 0.03875 0.00061 0.00652 -0.00067 0.03060 0.00178 0.00011 0.00006 0.00004 0.00000 0.00049 0.00052 0.00060 0.00046 0.00040 0.00041 0.00023 P6 0.33677 -0.00331 0.05497 1.00000 0.02728 0.02255 0.03135 -0.00088 0.00092 0.00268 0.02706 0.00167 0.00010 0.00006 0.00004 0.00000 0.00045 0.00049 0.00053 0.00043 0.00038 0.00038 0.00021 S1 0.72077 -0.24294 -0.25934 1.00000 0.05059 0.02628 0.02810 -0.00025 0.00318 0.00634 0.03499 0.00186 0.00012 0.00006 0.00004 0.00000 0.00057 0.00049 0.00055 0.00041 0.00045 0.00042 0.00024 Cl1 1.10995 -0.53698 -0.19220 1.00000 0.06875 0.04974 0.05261 0.00189 -0.00763 0.02506 0.05704 0.00243 0.00016 0.00008 0.00005 0.00000 0.00081 0.00071 0.00077 0.00059 0.00060 0.00058 0.00034 Cl2 1.18624 -0.42918 -0.29007 1.00000 0.04656 0.06682 0.06985 -0.00059 0.02717 0.00549 0.06107 0.00260 0.00014 0.00009 0.00006 0.00000 0.00067 0.00083 0.00093 0.00071 0.00059 0.00058 0.00036 Cl3 0.61130 -0.61661 -0.26177 1.00000 0.09875 0.04258 0.05010 -0.00157 0.00340 -0.03277 0.06381 0.00220 0.00018 0.00008 0.00006 0.00000 0.00104 0.00068 0.00080 0.00059 0.00070 0.00067 0.00039 Cl4 0.66296 -0.51666 -0.36503 1.00000 0.07799 0.04930 0.02679 -0.01285 -0.00559 0.00196 0.05136 0.00202 0.00015 0.00008 0.00004 0.00000 0.00082 0.00070 0.00055 0.00050 0.00052 0.00058 0.00031 Cl5 0.80417 0.06678 0.06969 1.00000 0.04189 0.04018 0.05756 -0.00472 0.00255 -0.01517 0.04654 0.00185 0.00012 0.00007 0.00005 0.00000 0.00056 0.00059 0.00074 0.00056 0.00050 0.00045 0.00028 Cl6 0.71829 0.02040 -0.04501 1.00000 0.05933 0.04533 0.04193 0.01016 0.01446 0.00465 0.04886 0.00222 0.00014 0.00007 0.00005 0.00000 0.00067 0.00063 0.00065 0.00052 0.00053 0.00052 0.00029 Cl7 0.17619 -0.00139 -0.00289 1.00000 0.04441 0.03849 0.03596 0.00215 -0.00972 0.00366 0.03962 0.00175 0.00011 0.00007 0.00004 0.00000 0.00056 0.00059 0.00056 0.00047 0.00042 0.00043 0.00025 Cl8 0.22776 0.06464 0.11086 1.00000 0.04548 0.03723 0.04135 -0.01134 0.00335 0.00994 0.04135 0.00189 0.00012 0.00007 0.00004 0.00000 0.00057 0.00055 0.00061 0.00048 0.00045 0.00045 0.00025 H4N 0.72254 -0.37099 -0.14855 1.00000 0.01782 0.06745 0.00443 0.00241 0.00164 0.00000 0.01022 Final Structure Factor Calculation for 00tam081 in P2(1)2(1)2(1) Total number of l.s. parameters = 356 Maximum vector length = 511 Memory required = 3651 / 27090 wR2 = 0.1127 before cycle 6 for 7560 data and 2 / 356 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0547 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0453 for 6007 Fo > 4sig(Fo) and 0.0665 for all 7560 data wR2 = 0.1127, GooF = S = 1.033, Restrained GooF = 1.033 for all data Flack x parameter = 0.1197 with esd 0.0725 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 39.00 for non-hydrogen and 25.00 for hydrogen atoms Principal mean square atomic displacements U 0.0541 0.0248 0.0203 C1 0.0575 0.0384 0.0210 C2 0.0912 0.0369 0.0220 C3 0.1141 0.0368 0.0165 C4 0.1108 0.0380 0.0268 C5 0.0638 0.0485 0.0293 C6 0.0818 0.0622 0.0355 C7 0.2074 0.0409 0.0303 C8 may be split into 0.9577 -0.2837 -0.4835 and 0.9140 -0.2834 -0.4899 0.0613 0.0286 0.0212 C9 0.0442 0.0308 0.0225 C10 0.0310 0.0276 0.0224 C11 0.0341 0.0290 0.0188 C12 0.0411 0.0271 0.0234 C13 0.3473 0.0346 0.0245 C14 may be split into 0.5209 -0.3460 0.0969 and 0.4604 -0.3357 0.1020 0.0724 0.0388 0.0225 C15 0.0341 0.0281 0.0221 N1 0.0618 0.0496 0.0227 N2 0.0417 0.0314 0.0213 N3 0.0480 0.0273 0.0160 N4 0.0425 0.0204 0.0201 N5 0.0414 0.0291 0.0213 N6 0.0434 0.0297 0.0212 N7 0.0635 0.0347 0.0190 N8 0.0374 0.0288 0.0195 N9 0.0296 0.0268 0.0179 P1 0.0395 0.0351 0.0229 P2 0.0498 0.0308 0.0199 P3 0.0288 0.0243 0.0195 P4 0.0421 0.0262 0.0236 P5 0.0316 0.0284 0.0212 P6 0.0525 0.0280 0.0244 S1 0.0869 0.0534 0.0308 Cl1 0.0881 0.0671 0.0280 Cl2 0.1140 0.0499 0.0275 Cl3 0.0790 0.0544 0.0206 Cl4 0.0621 0.0518 0.0258 Cl5 0.0709 0.0453 0.0304 Cl6 0.0511 0.0396 0.0282 Cl7 0.0539 0.0468 0.0233 Cl8 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.025 0.038 0.050 0.062 0.075 0.089 0.107 0.136 0.190 1.000 Number in group 796. 775. 743. 754. 736. 764. 723. 787. 724. 758. GooF 0.878 0.978 1.168 1.046 1.026 1.168 0.999 0.981 0.992 1.073 K 0.940 0.972 1.022 1.002 1.009 0.992 0.997 1.005 1.005 0.994 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.64 inf Number in group 757. 792. 738. 739. 758. 766. 739. 758. 755. 758. GooF 0.815 0.856 0.895 0.903 0.949 1.147 1.208 1.155 0.986 1.300 K 1.019 1.041 1.011 0.996 1.013 1.004 1.006 1.013 1.002 0.982 R1 0.186 0.144 0.112 0.088 0.065 0.056 0.051 0.037 0.033 0.036 Recommended weighting scheme: WGHT 0.0545 0.0000 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 5 6 16.51 538.89 14.34 0.078 0.99 7 1 7 -16.28 194.44 10.32 0.047 1.16 7 3 6 -10.71 229.86 10.28 0.051 1.15 7 4 4 -24.76 215.82 10.17 0.049 1.15 1 2 6 10671.73 16276.35 6.17 0.430 3.40 1 0 16 7613.66 12853.25 6.16 0.382 1.55 6 5 0 208.58 91.16 5.39 0.032 1.30 -1 3 11 1394.04 2058.57 5.24 0.153 2.04 3 2 8 208.62 127.90 4.47 0.038 2.05 -2 3 9 494.91 343.73 4.24 0.062 2.14 2 0 11 14618.36 21656.05 4.22 0.496 2.03 -1 1 19 3294.90 4833.79 4.21 0.234 1.31 3 9 11 4901.60 6430.19 4.12 0.270 1.25 -1 5 7 1535.95 1192.92 4.06 0.116 2.28 4 2 5 2056.50 2711.23 4.05 0.175 1.91 7 6 16 118.93 301.03 3.93 0.058 0.91 3 1 2 561.20 767.44 3.85 0.093 2.75 0 0 8 2142.99 1614.44 3.77 0.135 3.16 6 0 15 170.23 71.20 3.66 0.028 1.09 -7 3 2 472.54 694.07 3.62 0.089 1.19 6 7 0 86.49 150.33 3.54 0.041 1.20 -3 1 2 543.06 792.69 3.51 0.095 2.75 7 4 0 145.11 204.10 3.51 0.048 1.17 0 3 6 278.10 205.33 3.47 0.048 3.27 7 6 2 166.60 247.34 3.46 0.053 1.10 -7 6 2 163.97 244.86 3.44 0.053 1.10 -3 1 5 2088.55 2610.51 3.39 0.172 2.46 3 1 0 748.72 989.98 3.35 0.106 2.81 -1 2 9 557.56 707.13 3.35 0.090 2.53 -6 6 9 334.93 440.61 3.32 0.071 1.14 0 8 3 2052.38 1671.70 3.31 0.138 1.90 7 0 6 2393.09 1868.84 3.31 0.146 1.18 -5 1 14 1496.85 1153.77 3.27 0.114 1.24 1 6 16 8931.76 11446.17 3.24 0.360 1.33 7 0 9 257.19 336.10 3.24 0.062 1.12 2 2 0 69434.80 88187.24 3.21 1.000 3.76 -8 6 1 311.71 214.77 3.21 0.049 0.99 4 1 21 1207.10 1623.04 3.18 0.136 1.05 9 4 9 351.77 202.10 3.18 0.048 0.88 0 7 5 1450.56 1188.89 3.17 0.116 2.04 1 2 12 524.79 702.70 3.12 0.089 1.98 8 1 12 167.92 226.46 3.10 0.051 0.95 -4 6 9 159.12 105.76 3.09 0.035 1.43 7 1 14 360.49 250.24 3.07 0.053 1.01 2 6 3 2763.35 3340.85 3.06 0.195 2.15 -8 3 11 523.34 340.88 3.05 0.062 0.96 2 0 0 8100.17 10451.87 3.04 0.344 4.29 -2 1 12 664.51 464.78 3.04 0.073 1.88 6 7 1 -7.05 32.04 3.03 0.019 1.20 3 2 15 576.58 416.94 3.03 0.069 1.43 Bond lengths and angles C1 - Distance Angles C6 1.3804 (0.0061) C2 1.3857 (0.0062) 121.54 (0.42) S1 1.7846 (0.0041) 117.27 (0.37) 121.16 (0.32) C1 - C6 C2 C2 - Distance Angles C1 1.3857 (0.0062) C3 1.3919 (0.0064) 117.79 (0.45) C7 1.4939 (0.0071) 123.16 (0.43) 119.03 (0.48) C2 - C1 C3 C3 - Distance Angles C4 1.3808 (0.0079) C2 1.3919 (0.0064) 122.08 (0.52) C3 - C4 C4 - Distance Angles C3 1.3808 (0.0079) C5 1.3839 (0.0086) 119.07 (0.48) C8 1.5214 (0.0074) 121.03 (0.63) 119.85 (0.57) C4 - C3 C5 C5 - Distance Angles C4 1.3839 (0.0086) C6 1.4014 (0.0074) 120.07 (0.49) C5 - C4 C6 - Distance Angles C1 1.3804 (0.0061) C5 1.4014 (0.0074) 119.38 (0.52) C6 - C1 C7 - Distance Angles C2 1.4939 (0.0070) C7 - C8 - Distance Angles C4 1.5214 (0.0075) C8 - C9 - Distance Angles N4 1.4829 (0.0051) C10 1.5063 (0.0057) 111.91 (0.33) C9 - N4 C10 - Distance Angles C9 1.5063 (0.0057) C11 1.5169 (0.0056) 113.94 (0.35) C10 - C9 C11 - Distance Angles C10 1.5169 (0.0056) C12 1.5300 (0.0052) 111.33 (0.31) C11 - C10 C12 - Distance Angles N5 1.4800 (0.0046) C11 1.5300 (0.0052) 112.59 (0.31) C12 - N5 C13 - Distance Angles C14 1.4509 (0.0074) N5 1.4630 (0.0048) 112.67 (0.41) C13 - C14 C14 - Distance Angles C15 1.3646 (0.0073) C13 1.4509 (0.0074) 123.19 (0.57) C14 - C15 C15 - Distance Angles C14 1.3646 (0.0073) N6 1.4581 (0.0053) 117.54 (0.43) C15 - C14 N1 - Distance Angles P2 1.5648 (0.0032) P1 1.6120 (0.0032) 122.90 (0.20) N1 - P2 N2 - Distance Angles P3 1.5673 (0.0040) P2 1.5843 (0.0039) 119.48 (0.23) N2 - P3 N3 - Distance Angles P3 1.5568 (0.0034) P1 1.6100 (0.0032) 122.80 (0.21) N3 - P3 N4 - Distance Angles C9 1.4829 (0.0051) P1 1.6185 (0.0033) 121.82 (0.30) N4 - C9 N5 - Distance Angles C13 1.4630 (0.0048) C12 1.4800 (0.0046) 114.92 (0.32) P4 1.6389 (0.0031) 119.53 (0.26) 116.14 (0.25) N5 - C13 C12 N6 - Distance Angles C15 1.4581 (0.0053) P4 1.6278 (0.0034) 124.07 (0.28) N6 - C15 N7 - Distance Angles P5 1.5541 (0.0032) P4 1.6103 (0.0032) 125.74 (0.19) N7 - P5 N8 - Distance Angles P5 1.5798 (0.0032) P6 1.5849 (0.0034) 118.00 (0.19) N8 - P5 N9 - Distance Angles P6 1.5600 (0.0031) P4 1.6322 (0.0030) 124.70 (0.20) N9 - P6 P1 - Distance Angles N3 1.6100 (0.0032) N1 1.6120 (0.0032) 114.58 (0.17) N4 1.6185 (0.0033) 113.08 (0.19) 107.88 (0.19) S1 2.0644 (0.0014) 108.64 (0.14) 111.10 (0.13) 100.71 (0.14) P1 - N3 N1 N4 P2 - Distance Angles N1 1.5648 (0.0032) N2 1.5843 (0.0039) 119.53 (0.19) Cl2 1.9949 (0.0016) 110.40 (0.14) 107.87 (0.16) Cl1 1.9983 (0.0016) 107.54 (0.14) 109.65 (0.16) 100.11 (0.07) P2 - N1 N2 Cl2 P3 - Distance Angles N3 1.5568 (0.0034) N2 1.5673 (0.0040) 120.29 (0.19) Cl4 1.9975 (0.0016) 109.14 (0.14) 108.03 (0.16) Cl3 2.0002 (0.0016) 109.40 (0.14) 107.72 (0.17) 100.43 (0.07) P3 - N3 N2 Cl4 P4 - Distance Angles N7 1.6103 (0.0032) N6 1.6278 (0.0034) 111.79 (0.18) N9 1.6322 (0.0030) 110.68 (0.16) 109.06 (0.18) N5 1.6389 (0.0031) 108.75 (0.17) 103.53 (0.16) 112.86 (0.17) P4 - N7 N6 N9 P5 - Distance Angles N7 1.5541 (0.0032) N8 1.5798 (0.0032) 120.11 (0.17) Cl5 1.9924 (0.0015) 109.83 (0.14) 108.22 (0.14) Cl6 2.0090 (0.0016) 109.16 (0.14) 107.18 (0.16) 100.55 (0.06) P5 - N7 N8 Cl5 P6 - Distance Angles N9 1.5600 (0.0031) N8 1.5849 (0.0034) 119.70 (0.16) Cl8 1.9982 (0.0014) 108.88 (0.13) 108.38 (0.14) Cl7 2.0099 (0.0014) 109.74 (0.13) 107.77 (0.15) 100.69 (0.06) P6 - N9 N8 Cl8 S1 - Distance Angles C1 1.7846 (0.0041) P1 2.0644 (0.0014) 100.82 (0.13) S1 - C1 Cl1 - Distance Angles P2 1.9983 (0.0016) Cl1 - Cl2 - Distance Angles P2 1.9949 (0.0016) Cl2 - Cl3 - Distance Angles P3 2.0002 (0.0016) Cl3 - Cl4 - Distance Angles P3 1.9975 (0.0016) Cl4 - Cl5 - Distance Angles P5 1.9924 (0.0015) Cl5 - Cl6 - Distance Angles P5 2.0090 (0.0016) Cl6 - Cl7 - Distance Angles P6 2.0099 (0.0014) Cl7 - Cl8 - Distance Angles P6 1.9982 (0.0014) Cl8 - FMAP and GRID set by program FMAP 2 3 30 GRID -0.926 -2 -2 0.926 2 2 R1 = 0.0570 for 4303 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.79 at 0.5209 0.6526 0.0937 [ 0.32 A from C14 ] Deepest hole -0.97 at 0.4542 0.6667 0.1031 [ 0.35 A from C14 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 3537 / 29979 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3909 -0.3185 0.1100 1.00000 0.05 0.58 0.96 C14 1.05 H14A 1.48 C15 1.52 H15B Q2 1 0.8761 -0.5441 -0.2575 1.00000 0.05 0.33 0.74 N2 1.63 P3 1.63 P2 2.54 CL3 Q3 1 0.2586 -0.2448 0.1397 1.00000 0.05 0.31 1.75 H15B 1.82 N4 1.84 H4N 2.03 H10B Q4 1 0.2060 -0.2603 -0.0320 1.00000 0.05 0.30 1.33 H12B 1.85 N5 2.19 C12 2.28 P4 Q5 1 0.3301 0.1327 0.0770 1.00000 0.05 0.29 1.62 CL8 2.12 N8 2.13 H5 2.19 P6 Q6 1 0.6259 -0.3466 0.0626 1.00000 0.05 0.29 0.87 H14B 1.49 C14 1.85 C13 1.94 H13B Q7 1 0.7822 -0.3052 -0.5105 1.00000 0.05 0.29 1.24 H8C 1.36 H8B 1.49 C8 2.02 H3 Q8 1 0.8484 -0.3359 -0.2688 1.00000 0.05 0.29 1.45 P1 1.63 N1 1.83 S1 1.94 C1 Q9 1 0.8901 -0.3151 -0.2610 1.00000 0.05 0.29 1.59 N1 1.70 P1 1.84 S1 1.97 H6 Q10 1 0.6654 -0.3382 0.0928 1.00000 0.05 0.28 0.85 H14B 1.51 C14 1.78 H15A 1.86 C15 Shortest distances between peaks (including symmetry equivalents) 8 9 0.52 6 10 0.85 1 3 1.78 4 6 1.96 5 7 2.16 4 10 2.20 1 6 2.39 1 10 2.41 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: Generate connectivity array 0.01: 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. 1.32: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 8.23: Structure factors and derivatives 10.84: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.71: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.17: Analysis of variance 0.10: Merge reflections for Fourier and .fcf 0.07: Fourier summations 0.09: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 12:25:46 Total CPU time: 21.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++