+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0010p212121 started at 12:45:27 on 01-Sep-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0010p212121 in P2(1)2(1)2(1) CELL 0.71073 3.8043 12.9873 14.4013 90.000 90.000 90.000 ZERR 4.00 0.0011 0.0038 0.0025 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 O UNIT 28 32 8 8 V = 711.53 F(000) = 320.0 Mu = 0.11 mm-1 Cell Wt = 608.62 Rho = 1.420 MERG 4 OMIT -3.00 55.00 SHEL 7 0.77 EQIV_$1 x-1/2, -y+1/2, -z+1 HTAB N1 N1_$1 EQIV_$2 -x, y-1/2, -z+1/2 HTAB N1 O3A_$2 DFIX 0.87 0.02 N1 H1B N1 H1A FMAP 2 PLAN 5 SIZE 0.01 0.08 0.09 ACTA BOND $H WGHT 0.00000 2.26260 L.S. 8 TEMP -153.00 FVAR 1.30075 MOLE 1 C1 1 -0.027195 0.413161 0.437115 11.00000 0.03477 0.03414 = 0.02260 0.00268 0.00168 -0.00709 C2 1 0.088599 0.476241 0.364438 11.00000 0.01819 0.03358 = 0.02002 -0.00407 -0.00563 0.00108 C3 1 0.060450 0.581695 0.378544 11.00000 0.03927 0.02601 = 0.02492 0.00915 0.00165 0.00988 C4 1 -0.054953 0.625164 0.461163 11.00000 0.03338 0.02868 = 0.02798 0.01040 -0.00290 0.00658 AFIX 43 H4 2 -0.061094 0.697778 0.468955 11.00000 -1.20000 AFIX 0 C5 1 -0.159308 0.560961 0.530875 11.00000 0.02706 0.04863 = 0.02899 -0.00901 0.00316 -0.00001 AFIX 43 H5 2 -0.241302 0.589150 0.587762 11.00000 -1.20000 AFIX 0 C6 1 -0.147092 0.455935 0.519689 11.00000 0.03254 0.03457 = 0.01179 0.01270 -0.00122 -0.00505 AFIX 43 H6 2 -0.221231 0.412216 0.568817 11.00000 -1.20000 AFIX 0 C7 1 0.241364 0.429444 0.277837 11.00000 0.02921 0.03109 = 0.02174 -0.00781 -0.00344 -0.00180 AFIX 137 H7A 2 0.354440 0.483323 0.240721 11.00000 -1.50000 H7B 2 0.053351 0.397272 0.241474 11.00000 -1.50000 H7C 2 0.415830 0.377248 0.294894 11.00000 -1.50000 AFIX 0 N1 3 -0.000996 0.306008 0.428152 11.00000 0.02703 0.03148 = 0.02398 0.00039 -0.01048 -0.00517 N3 3 0.142942 0.654597 0.304916 11.00000 0.03462 0.03334 = 0.03227 -0.00550 -0.00918 -0.00020 O3A 4 0.036947 0.634879 0.226115 11.00000 0.06011 0.03657 = 0.03277 0.00269 0.00027 0.00031 O3B 4 0.310061 0.732942 0.325438 11.00000 0.05133 0.02518 = 0.04487 0.00765 0.00893 -0.00797 H1A 2 -0.123569 0.273342 0.470200 11.00000 -1.20000 H1B 2 0.002253 0.278522 0.372315 11.00000 -1.20000 HKLF 4 Covalent radii and connectivity table for 06skc0010p212121 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 C2 N1 C2 - C3 C1 C7 C3 - C4 C2 N3 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - C2 N1 - C1 N3 - O3A O3B C3 O3A - N3 O3B - N3 Operators for generating equivalent atoms: $1 x-1/2, -y+1/2, -z+1 $2 -x, y-1/2, -z+1/2 8430 Reflections read, of which 103 rejected -4 =< h =< 4, -16 =< k =< 16, -18 =< l =< 18, 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) 4 6 0 1.32 0.55 6 18.52 0 1 2 2855.24 33.72 3 2225.76 3 4 3 82.34 28.62 7 260.69 3 5 4 156.06 36.52 7 225.81 4 8 4 11.54 24.25 2 331.20 2 10 4 22.92 4.30 12 24.43 0 14 4 519.83 63.24 3 680.33 0 16 4 116.61 47.10 2 252.13 3 6 5 75.74 35.29 6 325.00 4 6 5 54.26 21.04 4 300.27 4 8 5 52.00 31.37 2 470.13 3 9 5 44.80 20.64 10 118.18 4 8 6 1.31 23.79 3 170.25 3 7 7 133.87 42.25 5 364.27 4 6 8 113.92 27.44 2 2290.30 3 7 8 1482.15 35.18 6 553.61 16 Inconsistent equivalents 985 Unique reflections, of which 0 suppressed R(int) = 0.3099 R(sigma) = 0.2309 Friedel opposites merged Maximum memory for data reduction = 1257 / 9431 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 = 1544 / 138341 wR2 = 0.1960 before cycle 1 for 985 data and 107 / 107 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.158; Restrained GooF = 1.157 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.30074 0.00707 -0.002 OSF Mean shift/esd = 0.005 Maximum = -0.025 for U33 O3B Max. shift = 0.001 A for H1A Max. dU = 0.000 for O3B Least-squares cycle 2 Maximum vector length = 511 Memory required = 1544 / 138341 wR2 = 0.1960 before cycle 2 for 985 data and 107 / 107 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.158; Restrained GooF = 1.157 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.30071 0.00707 -0.004 OSF Mean shift/esd = 0.003 Maximum = -0.019 for U33 O3B Max. shift = 0.000 A for H1A Max. dU = 0.000 for O3B Least-squares cycle 3 Maximum vector length = 511 Memory required = 1544 / 138341 wR2 = 0.1960 before cycle 3 for 985 data and 107 / 107 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.158; Restrained GooF = 1.157 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.30070 0.00707 -0.001 OSF Mean shift/esd = 0.002 Maximum = -0.010 for U33 O3B Max. shift = 0.000 A for H1A Max. dU = 0.000 for C1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1544 / 138341 wR2 = 0.1960 before cycle 4 for 985 data and 107 / 107 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.158; Restrained GooF = 1.157 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.30070 0.00707 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.007 for U33 O3B Max. shift = 0.000 A for H1A Max. dU = 0.000 for C1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1544 / 138341 wR2 = 0.1960 before cycle 5 for 985 data and 107 / 107 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.158; Restrained GooF = 1.157 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.30070 0.00707 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.005 for U33 O3B Max. shift = 0.000 A for H7B Max. dU = 0.000 for C1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1544 / 138341 wR2 = 0.1960 before cycle 6 for 985 data and 107 / 107 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.158; Restrained GooF = 1.157 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.30070 0.00707 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.003 for U33 O3B Max. shift = 0.000 A for H1A Max. dU = 0.000 for C1 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1544 / 138341 wR2 = 0.1960 before cycle 7 for 985 data and 107 / 107 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.158; Restrained GooF = 1.157 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.30070 0.00707 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.003 for U33 O3B Max. shift = 0.000 A for H1A Max. dU = 0.000 for C1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1544 / 138341 wR2 = 0.1960 before cycle 8 for 985 data and 107 / 107 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.158; Restrained GooF = 1.157 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.30070 0.00707 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for U33 O3B Max. shift = 0.000 A for H1A Max. dU = 0.000 for C1 Largest correlation matrix elements -0.819 z H1B / y H1B 0.521 z H1A / y H1A Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H4 -0.0610 0.6978 0.4690 43 0.950 0.000 C4 C5 C3 H5 -0.2415 0.5891 0.5877 43 0.950 0.000 C5 C4 C6 H6 -0.2211 0.4122 0.5688 43 0.950 0.000 C6 C5 C1 H7A 0.3543 0.4833 0.2407 137 0.980 0.000 C7 C2 H7A H7B 0.0534 0.3972 0.2415 137 0.980 0.000 C7 C2 H7A H7C 0.4160 0.3773 0.2949 137 0.980 0.000 C7 C2 H7A 06skc0010p212121 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.02729 0.41314 0.43712 1.00000 0.03475 0.03411 0.02248 0.00273 0.00177 -0.00703 0.03045 0.01678 0.00294 0.00074 0.00060 0.00000 0.00681 0.00599 0.00536 0.00450 0.00507 0.00543 0.00260 C2 0.08858 0.47623 0.36444 1.00000 0.01820 0.03352 0.02002 -0.00406 -0.00563 0.00109 0.02391 0.01494 0.00232 0.00073 0.00056 0.00000 0.00528 0.00570 0.00482 0.00421 0.00389 0.00451 0.00222 C3 0.06051 0.58168 0.37854 1.00000 0.03913 0.02601 0.02510 0.00904 0.00155 0.00988 0.03008 0.01757 0.00277 0.00070 0.00063 0.00000 0.00687 0.00585 0.00516 0.00422 0.00507 0.00522 0.00254 C4 -0.05493 0.62516 0.46117 1.00000 0.03349 0.02868 0.02802 0.01047 -0.00286 0.00656 0.03006 0.01669 0.00260 0.00072 0.00059 0.00000 0.00610 0.00567 0.00517 0.00449 0.00499 0.00523 0.00245 H4 -0.06103 0.69777 0.46897 1.00000 0.03607 0.00000 0.00000 C5 -0.15937 0.56093 0.53085 1.00000 0.02680 0.04885 0.02895 -0.00906 0.00320 -0.00007 0.03487 0.01767 0.00262 0.00080 0.00070 0.00000 0.00623 0.00701 0.00574 0.00488 0.00485 0.00531 0.00265 H5 -0.24151 0.58911 0.58773 1.00000 0.04184 0.00000 0.00000 C6 -0.14706 0.45590 0.51968 1.00000 0.03275 0.03440 0.01184 0.01274 -0.00121 -0.00500 0.02633 0.01620 0.00247 0.00073 0.00058 0.00000 0.00628 0.00595 0.00489 0.00426 0.00437 0.00472 0.00243 H6 -0.22107 0.41218 0.56882 1.00000 0.03159 0.00000 0.00000 C7 0.24136 0.42944 0.27784 1.00000 0.02931 0.03094 0.02178 -0.00795 -0.00342 -0.00174 0.02734 0.01466 0.00238 0.00065 0.00059 0.00000 0.00556 0.00552 0.00515 0.00435 0.00433 0.00486 0.00237 H7A 0.35428 0.48333 0.24070 1.00000 0.04101 0.00000 0.00000 H7B 0.05339 0.39722 0.24150 1.00000 0.04101 0.00000 0.00000 H7C 0.41596 0.37728 0.29489 1.00000 0.04101 0.00000 0.00000 N1 -0.00096 0.30601 0.42815 1.00000 0.02711 0.03142 0.02404 0.00037 -0.01045 -0.00516 0.02752 0.01368 0.00249 0.00064 0.00049 0.00000 0.00524 0.00514 0.00476 0.00367 0.00426 0.00415 0.00208 N3 0.14291 0.65460 0.30490 1.00000 0.03449 0.03340 0.03235 -0.00554 -0.00939 -0.00021 0.03341 0.01371 0.00215 0.00064 0.00053 0.00000 0.00516 0.00520 0.00522 0.00405 0.00407 0.00475 0.00212 O3A 0.03693 0.63489 0.22611 1.00000 0.06009 0.03652 0.03288 0.00265 0.00013 0.00030 0.04316 0.01222 0.00204 0.00048 0.00043 0.00000 0.00512 0.00419 0.00386 0.00363 0.00409 0.00446 0.00198 O3B 0.31009 0.73294 0.32544 1.00000 0.05132 0.02523 0.04454 0.00759 0.00892 -0.00798 0.04036 0.01254 0.00195 0.00048 0.00046 0.00000 0.00489 0.00374 0.00447 0.00356 0.00394 0.00401 0.00200 H1A -0.12333 0.27334 0.47024 1.00000 0.04844 0.16672 0.02213 0.00705 0.00497 0.00000 0.00000 H1B 0.00216 0.27850 0.37234 1.00000 0.04844 0.13154 0.02994 0.00642 0.00294 0.00000 0.00000 Final Structure Factor Calculation for 06skc0010p212121 in P2(1)2(1)2(1) Total number of l.s. parameters = 107 Maximum vector length = 511 Memory required = 1439 / 25046 wR2 = 0.1960 before cycle 9 for 985 data and 2 / 107 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.158; Restrained GooF = 1.157 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1223 for 520 Fo > 4sig(Fo) and 0.2282 for all 985 data wR2 = 0.1960, GooF = S = 1.158, Restrained GooF = 1.157 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 11.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0415 0.0290 0.0209 C1 0.0351 0.0234 0.0132 C2 0.0461 0.0292 0.0149 C3 0.0403 0.0344 0.0154 C4 0.0524 0.0291 0.0231 C5 0.0427 0.0302 0.0061 C6 0.0355 0.0304 0.0161 C7 0.0387 0.0295 0.0144 N1 0.0441 0.0339 0.0222 N3 0.0601 0.0379 0.0315 O3A 0.0577 0.0443 0.0191 O3B Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.020 0.032 0.045 0.056 0.068 0.088 0.108 0.148 0.205 1.000 Number in group 103. 100. 97. 98. 98. 97. 99. 99. 96. 98. GooF 1.315 1.253 1.329 1.257 1.223 0.828 1.091 1.128 1.052 0.996 K 22.504 6.249 3.770 2.277 1.573 1.126 1.103 0.990 0.982 0.954 Resolution(A) 0.77 0.80 0.84 0.88 0.92 0.99 1.07 1.19 1.38 1.76 inf Number in group 100. 97. 101. 96. 101. 96. 98. 100. 98. 98. GooF 1.089 1.057 0.972 1.191 1.385 1.407 1.175 1.276 1.044 0.873 K 1.945 1.625 1.444 1.784 1.389 1.101 1.043 1.026 1.050 0.961 R1 0.577 0.466 0.382 0.409 0.327 0.244 0.147 0.165 0.092 0.042 Recommended weighting scheme: WGHT 0.0000 2.2628 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) 0 0 12 -13.88 234.36 4.34 0.203 1.20 4 8 2 0.50 48.28 4.28 0.092 0.82 2 4 12 46.98 2.11 3.33 0.019 0.97 0 11 6 117.25 15.96 3.30 0.053 1.06 3 9 1 45.83 112.65 3.23 0.140 0.95 2 7 10 70.01 9.16 3.21 0.040 0.98 3 10 0 17.94 119.10 3.21 0.144 0.91 0 2 11 146.42 375.88 3.21 0.257 1.28 3 3 8 64.34 7.38 3.01 0.036 1.01 4 9 1 2.26 56.72 3.01 0.100 0.79 4 9 2 -11.96 20.85 2.85 0.060 0.79 0 5 12 39.13 3.17 2.85 0.024 1.09 3 1 11 92.05 0.16 2.81 0.005 0.91 0 5 7 36.22 1.20 2.72 0.014 1.61 4 8 1 -3.40 15.70 2.71 0.052 0.82 3 2 7 52.89 11.31 2.64 0.045 1.06 3 3 6 60.08 16.81 2.59 0.054 1.09 3 8 9 -18.53 19.41 2.57 0.058 0.85 3 7 8 876.07 7.06 2.42 0.035 0.91 2 13 8 63.50 11.16 2.42 0.044 0.79 4 3 2 38.34 4.18 2.41 0.027 0.92 0 7 10 52.42 3.51 2.38 0.025 1.14 1 6 12 32.81 6.25 2.37 0.033 1.01 1 4 10 22.90 0.57 2.36 0.010 1.24 0 6 10 53.35 12.96 2.36 0.048 1.20 3 6 6 60.72 118.57 2.33 0.144 1.00 0 11 9 101.77 5.04 2.32 0.030 0.95 3 3 11 52.26 0.12 2.30 0.005 0.89 2 2 13 75.88 8.68 2.29 0.039 0.95 0 3 11 31.80 0.00 2.28 0.000 1.25 0 10 6 142.54 245.30 2.25 0.207 1.14 4 1 2 53.78 8.50 2.22 0.039 0.94 3 7 0 13.51 76.03 2.21 0.115 1.05 1 8 10 149.10 209.54 2.21 0.192 1.04 2 5 11 59.76 24.92 2.20 0.066 1.00 2 8 9 72.40 23.48 2.20 0.064 0.98 0 5 10 138.08 86.71 2.19 0.123 1.26 2 0 7 32.57 4.91 2.15 0.029 1.40 0 1 9 124.16 199.94 2.14 0.187 1.59 1 14 5 93.86 16.35 2.13 0.054 0.86 3 4 8 36.09 3.71 2.13 0.026 0.99 3 1 9 94.12 49.02 2.12 0.093 0.99 1 0 13 291.16 452.65 2.10 0.282 1.06 1 11 9 52.79 6.53 2.10 0.034 0.92 3 9 10 19.59 77.88 2.08 0.117 0.79 2 10 3 -2.50 36.34 2.08 0.080 1.05 0 6 6 35.45 5.28 2.06 0.030 1.61 1 9 7 32.89 3.86 2.01 0.026 1.13 4 0 7 245.42 129.30 2.00 0.151 0.86 2 5 5 40.60 14.59 2.00 0.051 1.35 Bond lengths and angles C1 - Distance Angles C6 1.3892 (0.0113) C2 1.4004 (0.0114) 120.60 (0.84) N1 1.4009 (0.0119) 119.96 (0.87) 119.32 (0.86) C1 - C6 C2 C2 - Distance Angles C3 1.3886 (0.0113) C1 1.4004 (0.0114) 116.33 (0.82) C7 1.5042 (0.0111) 123.33 (0.83) 120.32 (0.83) C2 - C3 C1 C3 - Distance Angles C4 1.3884 (0.0115) C2 1.3886 (0.0113) 123.42 (0.86) N3 1.4559 (0.0109) 115.33 (0.77) 121.23 (0.82) C3 - C4 C2 C4 - Distance Angles C5 1.3641 (0.0118) C3 1.3884 (0.0115) 118.30 (0.89) H4 0.9500 120.85 120.85 C4 - C5 C3 C5 - Distance Angles C4 1.3641 (0.0118) C6 1.3743 (0.0119) 120.72 (0.94) H5 0.9500 119.64 119.64 C5 - C4 C6 C6 - Distance Angles C5 1.3743 (0.0119) C1 1.3892 (0.0113) 120.54 (0.88) H6 0.9500 119.73 119.73 C6 - C5 C1 C7 - Distance Angles C2 1.5042 (0.0111) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C2 H7A H7B N1 - Distance Angles C1 1.4009 (0.0119) H1A 0.8741 (0.0207) 112.34 (7.11) H1B 0.8797 (0.0206) 119.25 (6.14) 116.34 (9.66) N1 - C1 H1A N3 - Distance Angles O3A 1.2311 (0.0086) O3B 1.2358 (0.0091) 124.08 (0.84) C3 1.4559 (0.0109) 117.75 (0.80) 118.16 (0.76) N3 - O3A O3B O3A - Distance Angles N3 1.2311 (0.0086) O3A - O3B - Distance Angles N3 1.2358 (0.0091) O3B - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.87(2) 2.30(3) 3.165(12) 173(9) N1-H1A...N1_$1 0.88(2) 2.35(5) 3.145(10) 151(8) N1-H1B...O3A_$2 FMAP and GRID set by program FMAP 2 1 8 GRID -5.000 -2 -2 5.000 2 2 R1 = 0.2282 for 985 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.33 at 0.2003 0.5229 0.1495 [ 1.53 A from H7A ] Deepest hole -0.47 at 0.1647 0.8620 0.0571 [ 0.85 A from C1 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 1902 / 16404 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2003 0.5229 0.1495 1.00000 0.05 0.33 1.53 H7A 1.93 O3A 2.17 H7B 2.22 C7 Q2 1 -0.1615 0.6354 0.4215 1.00000 0.05 0.31 0.71 C4 1.13 H4 1.26 C3 1.85 C5 Q3 1 -0.0403 0.6802 0.5002 1.00000 0.05 0.30 0.51 H4 0.91 C4 1.67 C5 1.89 H5 Q4 1 -0.2959 0.5555 0.5725 1.00000 0.05 0.30 0.53 H5 0.80 C5 1.60 C6 1.88 H6 Q5 1 0.0170 0.3748 0.6673 1.00000 0.05 0.30 1.75 H6 1.90 O3A 2.18 H7A 2.40 N3 Shortest distances between peaks (including symmetry equivalents) 2 3 1.35 1 5 1.73 1 4 2.15 3 4 2.16 2 4 2.46 3 3 2.63 4 5 2.96 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 0.00: 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. 0.38: 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 0.30: Structure factors and derivatives 0.22: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.08: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0010p212121 finished at 12:45:28 Total CPU time: 1.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++