+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007may0014 started at 16:22:24 on 02-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007may0014 in P2(1)/c New: Pbca CELL 0.71073 14.2845 5.4226 22.7593 90.000 90.000 90.000 ZERR 8.00 0.0008 0.0002 0.0014 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S UNIT 80 72 8 8 8 V = 1762.92 F(000) = 800.0 Mu = 0.32 mm-1 Cell Wt = 1529.94 Rho = 1.441 MERG 2 OMIT -3.00 55.00 DFIX 0.84 0.02 O1 H1O EQIV $1 -x + 3/2, y - 1/2, z HTAB O1 O1_$1 FMAP 2 PLAN 5 SIZE 0.01 0.02 0.22 ACTA BOND $H WGHT 0.00000 10.09390 L.S. 6 TEMP -153.00 FVAR 0.39220 C1 1 0.623779 1.012435 -0.095319 11.00000 0.02253 0.05255 = 0.02251 0.00152 -0.00096 -0.00290 AFIX 23 H1A 2 0.589286 0.880088 -0.116035 11.00000 -1.20000 H1B 2 0.591406 1.170315 -0.103340 11.00000 -1.20000 AFIX 0 C2 1 0.621623 0.962383 -0.030225 11.00000 0.02340 0.03033 = 0.02865 0.00286 0.00006 0.00427 C3 1 0.661632 1.127931 0.009337 11.00000 0.01991 0.03456 = 0.03000 -0.00186 0.00245 -0.00063 AFIX 43 H3 2 0.690271 1.274942 -0.004533 11.00000 -1.20000 AFIX 0 C4 1 0.659433 1.077025 0.069034 11.00000 0.02103 0.02307 = 0.03379 -0.00696 -0.00064 -0.00213 AFIX 43 H4 2 0.685710 1.188908 0.096597 11.00000 -1.20000 AFIX 0 C5 1 0.617816 0.858059 0.087721 11.00000 0.02516 0.02618 = 0.02470 0.00027 0.00226 0.00297 C6 1 0.580670 0.754893 -0.007180 11.00000 0.02833 0.03152 = 0.02952 -0.00395 -0.00116 0.00225 AFIX 43 H6 2 0.552558 0.642097 -0.033803 11.00000 -1.20000 AFIX 0 C7 1 0.616588 0.789191 0.150201 11.00000 0.02458 0.02674 = 0.03136 0.00059 0.00032 0.00405 C8 1 0.659945 0.900796 0.197418 11.00000 0.03164 0.03353 = 0.02627 -0.00046 0.00090 0.00414 AFIX 43 H8 2 0.696484 1.046570 0.194241 11.00000 -1.20000 AFIX 0 C9 1 0.644381 0.776130 0.250756 11.00000 0.03343 0.04367 = 0.02282 -0.00790 -0.00512 0.00477 AFIX 43 H9 2 0.669318 0.827647 0.287454 11.00000 -1.20000 AFIX 0 C10 1 0.589401 0.572967 0.243670 11.00000 0.04763 0.03750 = 0.02363 0.00466 -0.00003 0.00097 AFIX 43 H10 2 0.571150 0.467670 0.275002 11.00000 -1.20000 AFIX 0 N1 3 0.577470 0.699431 0.050819 11.00000 0.03423 0.02541 = 0.02506 -0.00144 -0.00204 -0.00365 O1 4 0.716572 1.025029 -0.117766 11.00000 0.03659 0.06385 = 0.03066 -0.00258 0.00487 -0.00012 H1O 2 0.739139 0.880321 -0.120588 11.00000 -1.50000 S1 5 0.556987 0.528630 0.172369 11.00000 0.04481 0.03583 = 0.02663 0.00181 0.00243 -0.00694 HKLF 4 1.0 0.00 1.00 0.00 -1.00 0.00 0.00 0.00 0.00 1.00 Covalent radii and connectivity table for 2007may0014 in P2(1)/c New: Pbca C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - O1 C2 C2 - C6 C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - N1 C4 C7 C6 - N1 C2 C7 - C8 C5 S1 C8 - C7 C9 C9 - C10 C8 C10 - C9 S1 N1 - C5 C6 O1 - C1 S1 - C10 C7 Operators for generating equivalent atoms: $1 -x+3/2, y-1/2, z 13049 Reflections read, of which 1264 rejected -18 =< h =< 17, -6 =< k =< 6, -29 =< l =< 28, 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) 4 5 4 6.37 1.02 6 5.44 1 Inconsistent equivalents 1999 Unique reflections, of which 0 suppressed R(int) = 0.1290 R(sigma) = 0.1226 Friedel opposites merged Maximum memory for data reduction = 1372 / 19871 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 = 1703 / 155302 wR2 = 0.1999 before cycle 1 for 1999 data and 121 / 121 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.181; Restrained GooF = 1.181 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 10.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39172 0.00152 -0.314 OSF Mean shift/esd = 0.061 Maximum = 0.844 for y O1 Max. shift = 0.024 A for H1O Max. dU = 0.000 for O1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1703 / 155302 wR2 = 0.1995 before cycle 2 for 1999 data and 121 / 121 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.179; Restrained GooF = 1.179 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 10.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39163 0.00151 -0.060 OSF Mean shift/esd = 0.023 Maximum = -0.331 for U22 O1 Max. shift = 0.012 A for H1O Max. dU = 0.000 for O1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1703 / 155302 wR2 = 0.1995 before cycle 3 for 1999 data and 121 / 121 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 0.014 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.179; Restrained GooF = 1.179 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 10.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39163 0.00151 -0.003 OSF Mean shift/esd = 0.003 Maximum = -0.027 for U22 O1 Max. shift = 0.002 A for H1O Max. dU = 0.000 for C10 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1703 / 155302 wR2 = 0.1995 before cycle 4 for 1999 data and 121 / 121 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 0.014 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.179; Restrained GooF = 1.179 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 10.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39163 0.00151 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.004 for U22 O1 Max. shift = 0.000 A for H1O Max. dU = 0.000 for C3 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1703 / 155302 wR2 = 0.1995 before cycle 5 for 1999 data and 121 / 121 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 0.014 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.179; Restrained GooF = 1.179 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 10.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39163 0.00151 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for x H1O Max. shift = 0.000 A for H1O Max. dU = 0.000 for C8 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1703 / 155302 wR2 = 0.1995 before cycle 6 for 1999 data and 121 / 121 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 0.014 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.179; Restrained GooF = 1.179 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 10.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39163 0.00151 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U22 O1 Max. shift = 0.000 A for H1O Max. dU = 0.000 for C10 Largest correlation matrix elements 0.763 y H1O / x H1O Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.5896 0.8794 -0.1160 23 0.990 0.000 C1 O1 C2 H1B 0.5911 1.1697 -0.1034 23 0.990 0.000 C1 O1 C2 H3 0.6903 1.2749 -0.0045 43 0.950 0.000 C3 C4 C2 H4 0.6857 1.1890 0.0966 43 0.950 0.000 C4 C3 C5 H6 0.5526 0.6421 -0.0338 43 0.950 0.000 C6 N1 C2 H8 0.6965 1.0466 0.1943 43 0.950 0.000 C8 C7 C9 H9 0.6693 0.8275 0.2875 43 0.950 0.000 C9 C10 C8 H10 0.5712 0.4676 0.2750 43 0.950 0.000 C10 C9 S1 2007may0014 in P2(1)/c New: Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.62379 1.01230 -0.09532 1.00000 0.02241 0.05239 0.02249 0.00146 -0.00084 -0.00306 0.03243 0.01051 0.00039 0.00130 0.00024 0.00000 0.00311 0.00400 0.00306 0.00314 0.00239 0.00307 0.00145 H1A 0.58956 0.87943 -0.11601 1.00000 0.03892 0.00000 0.00000 H1B 0.59111 1.16970 -0.10338 1.00000 0.03892 0.00000 0.00000 C2 0.62161 0.96248 -0.03022 1.00000 0.02342 0.03022 0.02857 0.00268 0.00006 0.00421 0.02740 0.01024 0.00039 0.00110 0.00025 0.00000 0.00299 0.00310 0.00315 0.00282 0.00244 0.00274 0.00130 C3 0.66166 1.12796 0.00934 1.00000 0.01986 0.03441 0.02998 -0.00183 0.00244 -0.00076 0.02809 0.01014 0.00039 0.00113 0.00025 0.00000 0.00309 0.00320 0.00353 0.00281 0.00257 0.00262 0.00139 H3 0.69033 1.27492 -0.00453 1.00000 0.03370 0.00000 0.00000 C4 0.65945 1.07708 0.06902 1.00000 0.02089 0.02310 0.03350 -0.00707 -0.00065 -0.00216 0.02583 0.00974 0.00038 0.00101 0.00026 0.00000 0.00305 0.00304 0.00342 0.00261 0.00259 0.00245 0.00134 H4 0.68570 1.18899 0.09659 1.00000 0.03100 0.00000 0.00000 C5 0.61784 0.85806 0.08771 1.00000 0.02520 0.02612 0.02446 0.00018 0.00227 0.00315 0.02526 0.01005 0.00040 0.00102 0.00025 0.00000 0.00322 0.00296 0.00321 0.00256 0.00259 0.00263 0.00131 C6 0.58066 0.75488 -0.00718 1.00000 0.02812 0.03148 0.02930 -0.00379 -0.00117 0.00202 0.02963 0.01062 0.00039 0.00118 0.00026 0.00000 0.00344 0.00316 0.00351 0.00287 0.00259 0.00276 0.00140 H6 0.55256 0.64208 -0.03381 1.00000 0.03556 0.00000 0.00000 C7 0.61657 0.78912 0.15019 1.00000 0.02452 0.02649 0.03121 0.00039 0.00051 0.00395 0.02741 0.01030 0.00041 0.00106 0.00026 0.00000 0.00316 0.00298 0.00332 0.00274 0.00264 0.00264 0.00133 C8 0.65996 0.90084 0.19743 1.00000 0.03144 0.03364 0.02610 -0.00065 0.00110 0.00414 0.03039 0.01076 0.00043 0.00114 0.00025 0.00000 0.00353 0.00332 0.00330 0.00281 0.00273 0.00277 0.00142 H8 0.69649 1.04664 0.19427 1.00000 0.03647 0.00000 0.00000 C9 0.64438 0.77604 0.25076 1.00000 0.03347 0.04354 0.02283 -0.00786 -0.00513 0.00491 0.03328 0.01073 0.00041 0.00116 0.00028 0.00000 0.00358 0.00361 0.00313 0.00306 0.00268 0.00299 0.00147 H9 0.66933 0.82750 0.28746 1.00000 0.03994 0.00000 0.00000 C10 0.58940 0.57292 0.24368 1.00000 0.04745 0.03738 0.02367 0.00483 -0.00006 0.00091 0.03617 0.01076 0.00044 0.00114 0.00027 0.00000 0.00402 0.00355 0.00331 0.00293 0.00283 0.00305 0.00156 H10 0.57115 0.46762 0.27501 1.00000 0.04340 0.00000 0.00000 N1 0.57747 0.69941 0.05081 1.00000 0.03411 0.02514 0.02494 -0.00126 -0.00196 -0.00357 0.02807 0.00805 0.00033 0.00087 0.00021 0.00000 0.00305 0.00264 0.00282 0.00219 0.00223 0.00222 0.00120 O1 0.71635 1.02609 -0.11779 1.00000 0.03744 0.05991 0.03252 -0.00252 0.00500 0.00156 0.04329 0.00849 0.00031 0.00097 0.00021 0.00000 0.00271 0.00324 0.00248 0.00264 0.00200 0.00251 0.00120 H1O 0.73758 0.87901 -0.11925 1.00000 0.06493 0.12835 0.00535 0.00644 0.00329 0.00000 0.00000 S1 0.55699 0.52864 0.17237 1.00000 0.04467 0.03573 0.02652 0.00182 0.00242 -0.00695 0.03564 0.00283 0.00012 0.00029 0.00007 0.00000 0.00092 0.00085 0.00076 0.00075 0.00074 0.00081 0.00044 Final Structure Factor Calculation for 2007may0014 in P2(1)/c New: Pbca Total number of l.s. parameters = 121 Maximum vector length = 511 Memory required = 1582 / 24017 wR2 = 0.1995 before cycle 7 for 1999 data and 0 / 121 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 0.014 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.179; Restrained GooF = 1.179 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 10.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1062 for 1065 Fo > 4sig(Fo) and 0.2077 for all 1999 data wR2 = 0.1995, GooF = S = 1.179, Restrained GooF = 1.179 for all data Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 9.00 for hydrogen atoms Principal mean square atomic displacements U 0.0528 0.0230 0.0216 C1 0.0335 0.0275 0.0212 C2 0.0352 0.0297 0.0193 C3 0.0371 0.0225 0.0179 C4 0.0294 0.0249 0.0215 C5 0.0351 0.0274 0.0264 C6 0.0314 0.0294 0.0214 C7 0.0368 0.0288 0.0255 C8 0.0488 0.0317 0.0193 C9 0.0475 0.0388 0.0221 C10 0.0356 0.0262 0.0224 N1 0.0602 0.0406 0.0291 O1 0.0485 0.0331 0.0253 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.015 0.022 0.030 0.040 0.051 0.066 0.087 0.129 1.000 Number in group 216. 206. 183. 195. 220. 186. 197. 200. 196. 200. GooF 1.184 1.232 1.195 1.165 1.183 1.337 1.360 1.144 0.988 0.946 K 17.462 4.004 1.885 1.337 1.099 1.066 1.017 1.049 1.017 1.015 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.65 inf Number in group 206. 196. 209. 191. 197. 203. 199. 197. 200. 201. GooF 1.243 1.344 1.328 1.321 1.210 1.045 1.054 0.994 0.986 1.189 K 1.313 1.506 1.241 1.088 1.145 1.026 0.986 0.995 0.995 1.020 R1 0.497 0.432 0.370 0.325 0.245 0.184 0.129 0.098 0.081 0.050 Recommended weighting scheme: WGHT 0.0000 10.5269 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) 2 6 1 738.26 269.80 4.19 0.069 0.90 15 3 8 373.14 2.15 3.60 0.006 0.81 2 4 22 369.53 53.19 3.39 0.030 0.82 7 4 17 -115.57 206.44 3.29 0.060 0.86 2 6 10 243.09 13.03 3.19 0.015 0.83 8 1 23 229.18 44.80 3.15 0.028 0.85 2 3 22 267.55 6.14 3.15 0.010 0.89 4 3 18 229.98 12.77 3.15 0.015 1.00 15 4 3 -53.08 190.86 3.12 0.058 0.78 4 0 0 63934.93 57324.64 3.01 1.000 3.57 13 4 8 660.97 181.56 2.91 0.056 0.82 0 2 12 21.41 222.62 2.91 0.062 1.55 11 3 16 543.78 143.69 2.90 0.050 0.85 10 5 10 609.44 241.32 2.89 0.065 0.81 2 6 3 108.47 9.15 2.87 0.013 0.89 16 1 2 469.43 95.12 2.80 0.041 0.88 11 4 16 811.42 414.65 2.78 0.085 0.78 13 1 6 6.32 174.90 2.77 0.055 1.04 3 4 5 24.74 170.68 2.74 0.055 1.25 0 6 14 -121.18 169.79 2.71 0.054 0.79 14 1 14 285.89 26.04 2.64 0.021 0.85 14 1 0 -48.14 100.73 2.61 0.042 1.00 11 1 20 268.45 49.98 2.61 0.030 0.85 11 1 8 93.16 2.22 2.57 0.006 1.15 11 2 19 208.61 0.57 2.54 0.003 0.84 2 3 4 178.72 59.80 2.53 0.032 1.67 0 2 26 -101.71 326.99 2.52 0.076 0.83 7 4 7 82.92 2.46 2.49 0.007 1.07 9 2 23 315.35 4.07 2.47 0.008 0.80 2 0 24 519.63 228.60 2.47 0.063 0.94 7 4 19 259.26 20.19 2.46 0.019 0.82 12 1 9 254.15 85.84 2.46 0.039 1.06 0 4 8 114.91 27.24 2.45 0.022 1.22 1 1 2 6878.41 6107.02 2.43 0.326 4.63 12 0 22 375.04 14.45 2.43 0.016 0.78 11 3 11 157.70 25.55 2.43 0.021 0.94 11 3 14 123.76 4.14 2.43 0.008 0.88 2 4 13 364.60 592.38 2.42 0.102 1.06 14 3 11 504.46 100.82 2.39 0.042 0.82 5 4 17 385.26 137.01 2.38 0.049 0.90 1 2 8 -29.94 54.21 2.38 0.031 1.94 7 2 16 28.32 128.57 2.37 0.047 1.07 16 0 14 684.82 290.62 2.36 0.071 0.78 10 5 9 239.74 2.08 2.36 0.006 0.82 10 4 7 284.75 131.78 2.35 0.048 0.94 3 6 7 360.10 165.00 2.35 0.054 0.86 16 3 2 534.65 0.01 2.34 0.000 0.80 11 1 21 19.47 180.17 2.34 0.056 0.82 6 3 18 331.88 107.94 2.32 0.043 0.95 8 6 6 378.23 75.71 2.31 0.036 0.79 Bond lengths and angles C1 - Distance Angles O1 1.4195 (0.0068) C2 1.5065 (0.0079) 112.52 (0.46) H1A 0.9900 109.09 109.09 H1B 0.9900 109.09 109.09 107.84 C1 - O1 C2 H1A C2 - Distance Angles C6 1.3727 (0.0084) C3 1.3939 (0.0080) 117.14 (0.55) C1 1.5065 (0.0079) 122.11 (0.56) 120.75 (0.55) C2 - C6 C3 C3 - Distance Angles C4 1.3865 (0.0079) C2 1.3939 (0.0080) 119.69 (0.56) H3 0.9500 120.16 120.16 C3 - C4 C2 C4 - Distance Angles C3 1.3865 (0.0079) C5 1.3945 (0.0076) 118.56 (0.54) H4 0.9500 120.72 120.72 C4 - C3 C5 C5 - Distance Angles N1 1.3334 (0.0071) C4 1.3945 (0.0077) 122.80 (0.54) C7 1.4704 (0.0081) 116.09 (0.51) 121.12 (0.54) C5 - N1 C4 C6 - Distance Angles N1 1.3546 (0.0073) C2 1.3727 (0.0084) 124.65 (0.56) H6 0.9500 117.67 117.67 C6 - N1 C2 C7 - Distance Angles C8 1.3810 (0.0080) C5 1.4704 (0.0081) 129.48 (0.55) S1 1.7246 (0.0060) 110.67 (0.45) 119.82 (0.45) C7 - C8 C5 C8 - Distance Angles C7 1.3810 (0.0080) C9 1.4074 (0.0084) 112.92 (0.57) H8 0.9500 123.54 123.54 C8 - C7 C9 C9 - Distance Angles C10 1.3623 (0.0085) C8 1.4074 (0.0084) 112.21 (0.57) H9 0.9500 123.90 123.90 C9 - C10 C8 C10 - Distance Angles C9 1.3623 (0.0085) S1 1.7048 (0.0063) 112.53 (0.49) H10 0.9500 123.74 123.74 C10 - C9 S1 N1 - Distance Angles C5 1.3334 (0.0071) C6 1.3546 (0.0073) 117.12 (0.50) N1 - C5 O1 - Distance Angles C1 1.4195 (0.0068) H1O 0.8539 (0.0200) 107.20 (5.58) O1 - C1 S1 - Distance Angles C10 1.7048 (0.0063) C7 1.7246 (0.0061) 91.67 (0.30) S1 - C10 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.85(2) 2.02(2) 2.877(3) 176(8) O1-H1O...O1_$1 FMAP and GRID set by program FMAP 2 2 10 GRID -3.571 24 -2 3.571 1 2 R1 = 0.2071 for 1999 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.54 at 0.6370 0.2251 0.3976 [ 0.87 A from H1B ] Deepest hole -0.40 at 0.3084 0.0785 0.3726 [ 1.65 A from C7 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 2498 / 25293 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6370 1.2749 -0.1024 1.00000 0.05 0.54 0.87 H1B 1.45 C1 1.80 O1 1.92 H1O Q2 1 0.6624 1.0904 0.2017 1.00000 0.05 0.40 0.57 H8 1.03 C8 2.05 C9 2.12 C7 Q3 1 0.4555 0.7896 -0.1082 1.00000 0.05 0.39 1.98 H1A 2.00 C4 2.04 H4 2.23 C5 Q4 1 0.5536 0.5447 -0.0419 1.00000 0.05 0.39 0.56 H6 1.44 C6 2.30 N1 2.30 N1 Q5 1 0.6198 1.0935 -0.0144 1.00000 0.05 0.39 0.80 C2 0.83 C3 1.43 H3 1.89 C1 Shortest distances between peaks (including symmetry equivalents) 1 5 2.24 1 4 2.34 3 4 2.45 4 4 2.49 4 5 2.70 2 3 2.79 Time profile in seconds ----------------------- 0.13: 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 0.02: Analyse other restraints etc. 0.84: 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 0.22: Structure factors and derivatives 0.01: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.15: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.01: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007may0014 finished at 16:22:30 Total CPU time: 1.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++