+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007may0004 started at 14:24:12 on 29-Sep-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007may0004 in C2/c CELL 0.71073 22.2448 5.1191 15.6074 90.000 95.838 90.000 ZERR 8.00 0.0016 0.0002 0.0010 0.000 0.003 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H O UNIT 88 64 24 V = 1768.05 F(000) = 784.0 Mu = 0.10 mm-1 Cell Wt = 1505.39 Rho = 1.414 MERG 2 OMIT -3.00 55.00 DFIX 0.84 0.02 O2 H1O FMAP 2 PLAN 5 SIZE 0.02 0.06 0.30 ACTA EQIV $1 -x, -y + 2, -z HTAB O2 O3_$1 BOND $H L.S. 6 TEMP -153.00 WGHT 0.054800 0.859500 EXTI 0.002704 FVAR 0.39374 C1 1 0.235917 0.243460 0.130713 11.00000 0.02437 0.02499 = 0.01950 -0.00078 0.00257 -0.00036 C2 1 0.275670 0.052913 0.155331 11.00000 0.02927 0.02602 = 0.02807 0.00466 -0.00049 0.00104 AFIX 43 H2 2 0.267920 -0.099293 0.187253 11.00000 -1.20000 AFIX 0 C3 1 0.331608 0.122910 0.124400 11.00000 0.02539 0.03938 = 0.03754 -0.00731 0.00094 0.00908 AFIX 43 H3 2 0.368207 0.026015 0.131136 11.00000 -1.20000 AFIX 0 C4 1 0.322380 0.351447 0.084118 11.00000 0.02096 0.04569 = 0.03382 -0.00711 0.00942 -0.00391 AFIX 43 H4 2 0.352187 0.445285 0.057270 11.00000 -1.20000 AFIX 0 C5 1 0.172234 0.280321 0.142271 11.00000 0.02394 0.02204 = 0.02141 -0.00393 -0.00024 -0.00004 C6 1 0.138415 0.478335 0.098668 11.00000 0.02481 0.02246 = 0.01929 -0.00179 0.00377 -0.00361 AFIX 43 H6 2 0.157235 0.592068 0.061380 11.00000 -1.20000 AFIX 0 C7 1 0.077651 0.510870 0.109176 11.00000 0.02253 0.02255 = 0.01923 -0.00252 0.00025 0.00082 C8 1 0.049691 0.347069 0.164355 11.00000 0.02096 0.02805 = 0.02606 -0.00172 0.00382 0.00059 AFIX 43 H8 2 0.008122 0.369078 0.171708 11.00000 -1.20000 AFIX 0 C9 1 0.083243 0.150695 0.208657 11.00000 0.02927 0.02606 = 0.02295 0.00252 0.00487 -0.00379 AFIX 43 H9 2 0.064569 0.039041 0.246727 11.00000 -1.20000 AFIX 0 C10 1 0.143543 0.117792 0.197422 11.00000 0.02745 0.02246 = 0.02109 -0.00049 -0.00154 0.00197 AFIX 43 H10 2 0.165891 -0.017559 0.227683 11.00000 -1.20000 AFIX 0 C11 1 0.043648 0.720913 0.060068 11.00000 0.01864 0.02451 = 0.02330 -0.00340 0.00324 -0.00284 O1 3 0.263651 0.432036 0.086936 11.00000 0.02958 0.03359 = 0.03512 0.00266 0.00545 -0.00012 O2 3 -0.012640 0.749893 0.078383 11.00000 0.02094 0.02991 = 0.03504 0.00800 0.00575 0.00379 H1O 2 -0.029283 0.877813 0.049678 11.00000 0.06359 O3 3 0.066115 0.855707 0.006319 11.00000 0.02336 0.03011 = 0.02794 0.00650 0.00486 0.00274 HKLF 4 Covalent radii and connectivity table for 2007may0004 in C2/c C 0.770 H 0.320 O 0.660 C1 - C2 O1 C5 C2 - C1 C3 C3 - C4 C2 C4 - C3 O1 C5 - C10 C6 C1 C6 - C7 C5 C7 - C6 C8 C11 C8 - C7 C9 C9 - C10 C8 C10 - C9 C5 C11 - O3 O2 C7 O1 - C1 C4 O2 - C11 O3 - C11 Operators for generating equivalent atoms: $1 -x, -y+2, -z 11102 Reflections read, of which 751 rejected -28 =< h =< 28, -6 =< k =< 6, -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 5 11 74.27 8.50 3 54.12 1 Inconsistent equivalents 2030 Unique reflections, of which 0 suppressed R(int) = 0.0791 R(sigma) = 0.0741 Friedel opposites merged Maximum memory for data reduction = 1329 / 24305 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 = 1677 / 165919 wR2 = 0.1359 before cycle 1 for 2030 data and 132 / 132 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 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39374 0.00137 -0.001 OSF 2 0.00270 0.00079 0.000 EXTI Mean shift/esd = 0.002 Maximum = -0.004 for U12 C7 Max. shift = 0.000 A for H6 Max. dU = 0.000 for C5 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1677 / 165919 wR2 = 0.1359 before cycle 2 for 2030 data and 132 / 132 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 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39374 0.00137 0.000 OSF 2 0.00270 0.00079 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.002 for U12 O3 Max. shift = 0.000 A for H6 Max. dU = 0.000 for C5 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1677 / 165919 wR2 = 0.1359 before cycle 3 for 2030 data and 132 / 132 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 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39374 0.00137 -0.001 OSF 2 0.00270 0.00079 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 4 Maximum vector length = 511 Memory required = 1677 / 165919 wR2 = 0.1359 before cycle 4 for 2030 data and 132 / 132 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 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39374 0.00137 0.000 OSF 2 0.00270 0.00079 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 5 Maximum vector length = 511 Memory required = 1677 / 165919 wR2 = 0.1359 before cycle 5 for 2030 data and 132 / 132 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 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39374 0.00137 0.000 OSF 2 0.00270 0.00079 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 6 Maximum vector length = 511 Memory required = 1677 / 165919 wR2 = 0.1359 before cycle 6 for 2030 data and 132 / 132 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 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39374 0.00137 0.000 OSF 2 0.00270 0.00079 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.2679 -0.0993 0.1873 43 0.950 0.000 C2 C1 C3 H3 0.3682 0.0260 0.1311 43 0.950 0.000 C3 C4 C2 H4 0.3522 0.4453 0.0573 43 0.950 0.000 C4 C3 O1 H6 0.1572 0.5921 0.0614 43 0.950 0.000 C6 C7 C5 H8 0.0081 0.3691 0.1717 43 0.950 0.000 C8 C7 C9 H9 0.0646 0.0390 0.2467 43 0.950 0.000 C9 C10 C8 H10 0.1659 -0.0176 0.2277 43 0.950 0.000 C10 C9 C5 2007may0004 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.23592 0.24346 0.13071 1.00000 0.02437 0.02499 0.01950 -0.00078 0.00257 -0.00036 0.02293 0.00366 0.00010 0.00038 0.00013 0.00000 0.00123 0.00115 0.00104 0.00089 0.00090 0.00093 0.00050 C2 0.27567 0.05291 0.15533 1.00000 0.02927 0.02602 0.02807 0.00466 -0.00048 0.00104 0.02802 0.00388 0.00010 0.00042 0.00014 0.00000 0.00134 0.00120 0.00124 0.00096 0.00100 0.00101 0.00055 H2 0.26792 -0.09929 0.18725 1.00000 0.03363 0.00000 0.00000 C3 0.33161 0.12291 0.12440 1.00000 0.02539 0.03938 0.03754 -0.00731 0.00094 0.00908 0.03426 0.00409 0.00010 0.00046 0.00015 0.00000 0.00137 0.00143 0.00138 0.00113 0.00107 0.00106 0.00061 H3 0.36821 0.02602 0.13114 1.00000 0.04111 0.00000 0.00000 C4 0.32238 0.35145 0.08412 1.00000 0.02096 0.04569 0.03382 -0.00711 0.00942 -0.00391 0.03303 0.00411 0.00010 0.00049 0.00015 0.00000 0.00130 0.00150 0.00131 0.00113 0.00101 0.00109 0.00058 H4 0.35219 0.44528 0.05727 1.00000 0.03964 0.00000 0.00000 C5 0.17223 0.28032 0.14227 1.00000 0.02394 0.02204 0.02141 -0.00393 -0.00024 -0.00004 0.02264 0.00354 0.00010 0.00038 0.00013 0.00000 0.00120 0.00109 0.00108 0.00087 0.00090 0.00090 0.00049 C6 0.13841 0.47833 0.09867 1.00000 0.02481 0.02246 0.01929 -0.00179 0.00377 -0.00361 0.02208 0.00358 0.00010 0.00040 0.00013 0.00000 0.00124 0.00109 0.00105 0.00085 0.00088 0.00089 0.00050 H6 0.15724 0.59207 0.06138 1.00000 0.02650 0.00000 0.00000 C7 0.07765 0.51087 0.10918 1.00000 0.02253 0.02255 0.01923 -0.00252 0.00025 0.00082 0.02157 0.00355 0.00009 0.00039 0.00013 0.00000 0.00120 0.00109 0.00108 0.00086 0.00088 0.00088 0.00049 C8 0.04969 0.34707 0.16436 1.00000 0.02096 0.02805 0.02606 -0.00172 0.00382 0.00059 0.02492 0.00375 0.00010 0.00041 0.00013 0.00000 0.00119 0.00113 0.00116 0.00096 0.00093 0.00096 0.00051 H8 0.00812 0.36908 0.17171 1.00000 0.02991 0.00000 0.00000 C9 0.08324 0.15069 0.20866 1.00000 0.02927 0.02606 0.02295 0.00252 0.00487 -0.00379 0.02594 0.00382 0.00010 0.00041 0.00014 0.00000 0.00129 0.00113 0.00112 0.00093 0.00093 0.00099 0.00052 H9 0.06457 0.03904 0.24673 1.00000 0.03113 0.00000 0.00000 C10 0.14354 0.11779 0.19742 1.00000 0.02745 0.02246 0.02109 -0.00049 -0.00154 0.00197 0.02394 0.00362 0.00010 0.00040 0.00013 0.00000 0.00128 0.00110 0.00112 0.00086 0.00093 0.00091 0.00051 H10 0.16589 -0.01756 0.22768 1.00000 0.02873 0.00000 0.00000 C11 0.04365 0.72091 0.06007 1.00000 0.01864 0.02451 0.02330 -0.00340 0.00324 -0.00284 0.02207 0.00353 0.00009 0.00038 0.00013 0.00000 0.00116 0.00111 0.00110 0.00091 0.00091 0.00090 0.00049 O1 0.26365 0.43204 0.08694 1.00000 0.02958 0.03359 0.03512 0.00266 0.00545 -0.00012 0.03262 0.00276 0.00007 0.00029 0.00010 0.00000 0.00097 0.00088 0.00094 0.00070 0.00072 0.00072 0.00043 O2 -0.01264 0.74989 0.07838 1.00000 0.02094 0.02991 0.03504 0.00800 0.00575 0.00379 0.02843 0.00275 0.00007 0.00029 0.00010 0.00000 0.00088 0.00091 0.00091 0.00071 0.00070 0.00067 0.00041 H1O -0.02928 0.87781 0.04968 1.00000 0.06359 0.05190 0.00123 0.00455 0.00171 0.00000 0.00961 O3 0.06612 0.85571 0.00632 1.00000 0.02336 0.03011 0.02794 0.00650 0.00486 0.00274 0.02698 0.00261 0.00006 0.00028 0.00009 0.00000 0.00088 0.00085 0.00083 0.00069 0.00067 0.00067 0.00041 Final Structure Factor Calculation for 2007may0004 in C2/c Total number of l.s. parameters = 132 Maximum vector length = 511 Memory required = 1545 / 21973 wR2 = 0.1359 before cycle 7 for 2030 data and 0 / 132 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 0.016 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0581 for 1292 Fo > 4sig(Fo) and 0.1063 for all 2030 data wR2 = 0.1359, GooF = S = 1.056, Restrained GooF = 1.056 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0252 0.0242 0.0193 C1 0.0335 0.0291 0.0215 C2 0.0496 0.0325 0.0206 C3 0.0500 0.0317 0.0174 C4 0.0272 0.0233 0.0174 C5 0.0278 0.0200 0.0185 C6 0.0253 0.0217 0.0177 C7 0.0290 0.0255 0.0203 C8 0.0318 0.0266 0.0195 C9 0.0304 0.0220 0.0195 C10 0.0280 0.0207 0.0175 C11 0.0373 0.0322 0.0283 O1 0.0415 0.0243 0.0195 O2 0.0362 0.0226 0.0221 O3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.016 0.023 0.031 0.040 0.052 0.067 0.095 0.140 1.000 Number in group 219. 219. 183. 203. 201. 193. 209. 202. 198. 203. GooF 0.967 1.176 0.906 1.021 1.115 1.098 1.096 1.063 0.970 1.100 K 7.209 1.825 1.161 1.057 1.046 0.989 0.987 1.004 1.011 1.012 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.63 inf Number in group 205. 208. 196. 213. 193. 202. 205. 204. 200. 204. GooF 1.011 0.940 1.084 1.007 0.936 1.067 1.101 0.919 0.967 1.429 K 1.051 1.051 1.114 1.053 1.059 1.008 0.997 1.003 1.021 1.006 R1 0.323 0.261 0.212 0.198 0.132 0.097 0.064 0.052 0.043 0.035 Recommended weighting scheme: WGHT 0.0548 0.8326 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) 4 0 0 1378.38 2362.19 6.33 0.188 5.53 -1 1 3 80.03 16.04 5.48 0.015 3.63 2 2 1 621.84 456.58 4.01 0.083 2.45 16 2 11 408.87 235.26 3.52 0.059 0.88 -6 2 14 99.51 13.59 3.34 0.014 1.01 0 0 6 1528.40 1980.90 3.30 0.172 2.59 3 1 10 49.33 13.29 3.25 0.014 1.43 11 3 8 623.00 827.55 3.07 0.111 1.05 -17 3 10 148.86 50.60 3.07 0.027 0.90 -7 1 18 241.72 77.57 2.95 0.034 0.84 18 0 10 7880.01 6405.25 2.95 0.309 0.92 -4 2 2 161.77 112.44 2.94 0.041 2.25 -6 4 7 57.71 119.14 2.90 0.042 1.08 -10 0 4 1151.72 927.91 2.85 0.118 2.01 4 6 3 124.67 1.05 2.85 0.004 0.83 -20 2 10 -48.49 43.99 2.76 0.026 0.89 -9 5 12 126.31 3.70 2.75 0.007 0.78 4 4 6 45.84 93.95 2.73 0.037 1.11 -1 5 9 150.93 250.62 2.73 0.061 0.88 0 2 1 473.14 382.77 2.70 0.076 2.53 -9 1 3 145.60 98.02 2.70 0.038 2.11 2 2 3 41.10 70.90 2.67 0.033 2.23 20 4 3 13.41 95.60 2.66 0.038 0.82 25 1 7 125.89 12.20 2.65 0.013 0.79 0 4 8 65.91 116.86 2.65 0.042 1.07 11 3 7 310.31 430.09 2.61 0.080 1.09 -19 3 13 213.63 10.46 2.60 0.012 0.78 14 2 7 -1.35 35.91 2.58 0.023 1.11 2 2 14 354.45 479.91 2.56 0.085 1.00 25 1 3 126.95 29.65 2.56 0.021 0.85 22 0 0 1077.69 1369.94 2.54 0.143 1.01 23 1 8 305.47 180.30 2.54 0.052 0.82 -24 2 11 140.33 16.21 2.54 0.016 0.77 -7 1 6 6.93 38.75 2.53 0.024 1.95 7 1 18 81.54 0.00 2.52 0.000 0.80 -20 2 3 108.92 2.06 2.51 0.006 1.01 1 1 6 -1.01 16.95 2.51 0.016 2.28 -23 3 8 273.91 128.97 2.50 0.044 0.80 -4 4 8 209.10 272.23 2.42 0.064 1.06 -12 0 2 2342.84 2004.28 2.41 0.173 1.84 -16 2 14 139.12 12.02 2.40 0.013 0.86 -13 3 15 148.01 14.27 2.39 0.015 0.81 17 1 12 807.36 633.64 2.38 0.097 0.86 -9 1 2 105.53 149.52 2.36 0.047 2.18 12 0 8 16.21 69.31 2.35 0.032 1.27 1 3 13 51.63 0.76 2.34 0.003 0.97 -8 2 16 85.33 0.03 2.34 0.001 0.89 20 2 11 92.32 2.65 2.33 0.006 0.79 -17 3 1 121.50 40.57 2.32 0.025 1.04 26 2 0 -8.45 57.46 2.28 0.029 0.81 Bond lengths and angles C1 - Distance Angles C2 1.3461 (0.0029) O1 1.3657 (0.0025) 109.75 (0.19) C5 1.4584 (0.0030) 132.58 (0.20) 117.67 (0.17) C1 - C2 O1 C2 - Distance Angles C1 1.3461 (0.0029) C3 1.4255 (0.0032) 106.97 (0.19) H2 0.9500 126.51 126.51 C2 - C1 C3 C3 - Distance Angles C4 1.3341 (0.0035) C2 1.4255 (0.0032) 106.39 (0.20) H3 0.9500 126.80 126.80 C3 - C4 C2 C4 - Distance Angles C3 1.3341 (0.0035) O1 1.3750 (0.0027) 110.44 (0.20) H4 0.9500 124.78 124.78 C4 - C3 O1 C5 - Distance Angles C10 1.3972 (0.0029) C6 1.3973 (0.0029) 118.36 (0.20) C1 1.4584 (0.0030) 120.63 (0.18) 121.01 (0.19) C5 - C10 C6 C6 - Distance Angles C7 1.3881 (0.0029) C5 1.3973 (0.0029) 120.80 (0.20) H6 0.9500 119.60 119.60 C6 - C7 C5 C7 - Distance Angles C6 1.3881 (0.0029) C8 1.3931 (0.0029) 120.14 (0.19) C11 1.4825 (0.0028) 118.54 (0.19) 121.32 (0.19) C7 - C6 C8 C8 - Distance Angles C7 1.3931 (0.0029) C9 1.3931 (0.0030) 119.40 (0.19) H8 0.9500 120.30 120.30 C8 - C7 C9 C9 - Distance Angles C10 1.3807 (0.0030) C8 1.3931 (0.0030) 120.22 (0.20) H9 0.9500 119.89 119.89 C9 - C10 C8 C10 - Distance Angles C9 1.3807 (0.0030) C5 1.3972 (0.0029) 121.07 (0.19) H10 0.9500 119.46 119.46 C10 - C9 C5 C11 - Distance Angles O3 1.2308 (0.0023) O2 1.3207 (0.0025) 122.97 (0.18) C7 1.4825 (0.0028) 122.53 (0.19) 114.50 (0.18) C11 - O3 O2 O1 - Distance Angles C1 1.3657 (0.0025) C4 1.3750 (0.0027) 106.44 (0.17) O1 - C1 O2 - Distance Angles C11 1.3207 (0.0025) H1O 0.8561 (0.0174) 109.98 (1.98) O2 - C11 O3 - Distance Angles C11 1.2308 (0.0023) O3 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.856(17) 1.775(18) 2.630(2) 177(3) O2-H1O...O3_$1 FMAP and GRID set by program FMAP 2 2 9 GRID -4.167 -2 -1 4.167 2 1 R1 = 0.1063 for 2030 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.24 at 0.1596 0.0362 0.4415 [ 0.54 A from H4 ] Deepest hole -0.24 at 0.2240 0.1335 0.8856 [ 0.59 A from O1 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2532 / 24423 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3404 0.5362 0.0585 1.00000 0.05 0.24 0.54 H4 1.12 C4 1.89 O1 2.37 C3 Q2 1 0.0695 0.6514 0.0985 1.00000 0.05 0.22 0.76 C7 0.86 C11 1.77 C6 1.77 O3 Q3 1 0.1637 0.5882 0.0360 1.00000 0.05 0.22 0.43 H6 1.30 C6 2.28 C5 2.36 C7 Q4 1 0.2499 0.0864 0.1164 1.00000 0.05 0.21 0.81 C2 0.90 C1 1.48 H2 1.82 C3 Q5 1 0.2629 0.1803 0.1770 1.00000 0.05 0.20 0.80 C2 0.95 C1 1.44 H2 1.83 C3 Shortest distances between peaks (including symmetry equivalents) 4 5 1.07 1 3 2.42 2 3 2.42 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 0.02: 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 0.01: Analyse other restraints etc. 0.31: 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 0.54: Structure factors and derivatives 0.95: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.18: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.04: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.04: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007may0004 finished at 14:24:27 Total CPU time: 2.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++