+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04sjc0831 started at 09:34:31 on 07-Oct-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04sjc0831 in Pbca CELL 0.71073 16.4963 8.3249 20.0608 90.000 90.000 90.000 ZERR 8.00 0.0018 0.0030 0.0063 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 O UNIT 112 160 40 V = 2754.95 F(000) = 1152.0 Mu = 0.10 mm-1 Cell Wt = 2146.40 Rho = 1.294 MERG 2 OMIT -3 55 OMIT 6 6 3 OMIT 12 0 6 FMAP 2 EXTI TEMP -153 SIZE 0.25 0.17 0.02 ACTA PLAN 10 BOND $H WGHT 0.04580 0.97680 L.S. 4 FVAR 0.42527 MOLE 1 C1 1 0.106605 0.603054 0.156030 11.00000 0.02782 0.02314 = 0.02611 0.00011 0.00372 -0.00165 C2 1 0.076719 0.615742 0.091750 11.00000 0.03696 0.03317 = 0.03017 0.00456 -0.00095 -0.00124 AFIX 43 H2 2 0.028482 0.670261 0.083753 11.00000 -1.20000 AFIX 0 C3 1 0.119194 0.546557 0.039212 11.00000 0.04724 0.04770 = 0.02897 0.00078 0.00357 -0.00876 AFIX 43 H3 2 0.099000 0.554136 -0.003956 11.00000 -1.20000 AFIX 0 C4 1 0.190396 0.467541 0.050648 11.00000 0.03996 0.03970 = 0.03489 -0.00761 0.01435 -0.00760 AFIX 43 H4 2 0.218300 0.422099 0.015053 11.00000 -1.20000 AFIX 0 C5 1 0.221898 0.453986 0.114961 11.00000 0.02705 0.02605 = 0.04318 -0.00392 0.00911 -0.00402 AFIX 43 H5 2 0.270324 0.399631 0.122353 11.00000 -1.20000 AFIX 0 C6 1 0.180187 0.522394 0.167515 11.00000 0.02681 0.01708 = 0.03058 0.00100 0.00143 -0.00478 C7 1 -0.013852 0.707283 0.206017 11.00000 0.02890 0.02549 = 0.03202 0.00250 -0.00466 0.00651 AFIX 23 H7A 2 -0.045459 0.622903 0.185128 11.00000 -1.20000 H7B 2 -0.018211 0.803539 0.179006 11.00000 -1.20000 AFIX 0 C8 1 -0.044362 0.738831 0.274497 11.00000 0.02973 0.02625 = 0.03794 0.00124 -0.00108 0.00638 AFIX 23 H8A 2 -0.007048 0.808920 0.297961 11.00000 -1.20000 H8B 2 -0.096699 0.791684 0.272319 11.00000 -1.20000 AFIX 0 C9 1 -0.063046 0.609171 0.378873 11.00000 0.02870 0.03915 = 0.03054 -0.00362 0.00373 0.00413 AFIX 23 H9A 2 -0.091617 0.516260 0.396177 11.00000 -1.20000 H9B 2 -0.096535 0.702998 0.386846 11.00000 -1.20000 AFIX 0 C10 1 0.016068 0.628092 0.415889 11.00000 0.03232 0.03076 = 0.02807 -0.00528 0.00145 0.00135 AFIX 23 H10A 2 0.047218 0.715658 0.396879 11.00000 -1.20000 H10B 2 0.005730 0.652246 0.462422 11.00000 -1.20000 AFIX 0 C11 1 0.140508 0.494341 0.432774 11.00000 0.03055 0.03463 = 0.03014 -0.00510 -0.00395 -0.00279 AFIX 23 H11A 2 0.141352 0.511670 0.480585 11.00000 -1.20000 H11B 2 0.167004 0.584776 0.411447 11.00000 -1.20000 AFIX 0 C12 1 0.184499 0.341532 0.415985 11.00000 0.03445 0.03131 = 0.03475 0.00286 -0.00612 -0.00140 AFIX 23 H12A 2 0.235693 0.339971 0.439763 11.00000 -1.20000 H12B 2 0.152580 0.251218 0.431619 11.00000 -1.20000 AFIX 0 C13 1 0.270409 0.403582 0.324049 11.00000 0.02348 0.02406 = 0.04972 0.00698 -0.00445 0.00015 AFIX 23 H13A 2 0.318792 0.347758 0.338828 11.00000 -1.20000 H13B 2 0.271620 0.511755 0.341991 11.00000 -1.20000 AFIX 0 C14 1 0.268239 0.409423 0.250024 11.00000 0.02101 0.02345 = 0.04490 0.00403 0.00259 0.00243 AFIX 23 H14A 2 0.319468 0.448379 0.232643 11.00000 -1.20000 H14B 2 0.258129 0.303287 0.231887 11.00000 -1.20000 AFIX 0 O1 3 0.069345 0.659095 0.211544 11.00000 0.02564 0.02963 = 0.02831 -0.00137 -0.00169 0.00630 O2 3 -0.051749 0.590116 0.309177 11.00000 0.03048 0.02800 = 0.02856 -0.00151 -0.00073 0.00088 O3 3 0.059876 0.482142 0.410323 11.00000 0.02661 0.03015 = 0.03443 -0.00435 -0.00625 0.00031 O4 3 0.199936 0.321388 0.347256 11.00000 0.03173 0.02388 = 0.03597 0.00033 0.00052 -0.00267 O5 3 0.203751 0.517006 0.232471 11.00000 0.02445 0.02065 = 0.03348 -0.00219 -0.00266 0.00438 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 04sjc0831 in Pbca C 0.770 H 0.320 O 0.660 C1 - O1 C2 C6 C2 - C1 C3 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 C6 - O5 C5 C1 C7 - O1 C8 C8 - O2 C7 C9 - O2 C10 C10 - O3 C9 C11 - O3 C12 C12 - O4 C11 C13 - O4 C14 C14 - O5 C13 O1 - C1 C7 O2 - C9 C8 O3 - C11 C10 O4 - C12 C13 O5 - C6 C14 h k l Fo^2 Sigma Why rejected 13 0 0 19.91 4.41 observed but should be systematically absent 0 3 7 72.90 16.39 observed but should be systematically absent 0 3 7 72.13 10.91 observed but should be systematically absent 0 3 7 50.03 9.08 observed but should be systematically absent 0 3 14 47.03 8.39 observed but should be systematically absent 0 3 14 36.21 6.58 observed but should be systematically absent 0 3 14 33.77 7.32 observed but should be systematically absent 21771 Reflections read, of which 1669 rejected -19 =< h =< 21, -9 =< k =< 10, -26 =< l =< 24, Max. 2-theta = 55.00 7 Systematic absence violations 0 Inconsistent equivalents 3155 Unique reflections, of which 0 suppressed R(int) = 0.0905 R(sigma) = 0.0670 Friedel opposites merged Maximum memory for data reduction = 2020 / 31534 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 = 2535 / 214176 wR2 = 0.1216 before cycle 1 for 3155 data and 173 / 173 parameters GooF = S = 1.001; Restrained GooF = 1.001 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0458 * P )^2 + 0.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.42817 0.00104 2.774 OSF 2 0.00281 0.00058 4.839 EXTI Mean shift/esd = 0.511 Maximum = 4.839 for EXTI Max. shift = 0.003 A for H5 Max. dU = 0.001 for C10 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2535 / 214176 wR2 = 0.1194 before cycle 2 for 3155 data and 173 / 173 parameters GooF = S = 0.977; Restrained GooF = 0.977 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0458 * P )^2 + 0.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43003 0.00105 1.765 OSF 2 0.00462 0.00070 2.599 EXTI Mean shift/esd = 0.213 Maximum = 2.599 for EXTI Max. shift = 0.001 A for C5 Max. dU = 0.000 for C10 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2535 / 214176 wR2 = 0.1192 before cycle 3 for 3155 data and 173 / 173 parameters GooF = S = 0.975; Restrained GooF = 0.975 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0458 * P )^2 + 0.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43022 0.00107 0.180 OSF 2 0.00487 0.00077 0.321 EXTI Mean shift/esd = 0.018 Maximum = 0.321 for EXTI Max. shift = 0.000 A for C3 Max. dU = 0.000 for C10 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2535 / 214176 wR2 = 0.1192 before cycle 4 for 3155 data and 173 / 173 parameters GooF = S = 0.974; Restrained GooF = 0.974 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0458 * P )^2 + 0.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43024 0.00107 0.017 OSF 2 0.00489 0.00078 0.024 EXTI Mean shift/esd = 0.003 Maximum = 0.024 for EXTI Max. shift = 0.000 A for C14 Max. dU = 0.000 for C12 Largest correlation matrix elements 0.505 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.0274 0.6713 0.0837 43 0.950 0.000 C2 C1 C3 H3 0.0986 0.5546 -0.0049 43 0.950 0.000 C3 C4 C2 H4 0.2188 0.4203 0.0144 43 0.950 0.000 C4 C3 C5 H5 0.2715 0.3992 0.1223 43 0.950 0.000 C5 C6 C4 H7A -0.0461 0.6209 0.1847 23 0.990 0.000 C7 O1 C8 H7B -0.0184 0.8053 0.1784 23 0.990 0.000 C7 O1 C8 H8A -0.0061 0.8102 0.2984 23 0.990 0.000 C8 O2 C7 H8B -0.0977 0.7928 0.2723 23 0.990 0.000 C8 O2 C7 H9A -0.0920 0.5139 0.3965 23 0.990 0.000 C9 O2 C10 H9B -0.0973 0.7045 0.3870 23 0.990 0.000 C9 O2 C10 H10A 0.0478 0.7175 0.3963 23 0.990 0.000 C10 O3 C9 H10B 0.0055 0.6532 0.4633 23 0.990 0.000 C10 O3 C9 H11A 0.1414 0.5122 0.4815 23 0.990 0.000 C11 O3 C12 H11B 0.1675 0.5867 0.4109 23 0.990 0.000 C11 O3 C12 H12A 0.2370 0.3404 0.4402 23 0.990 0.000 C12 O4 C11 H12B 0.1522 0.2494 0.4321 23 0.990 0.000 C12 O4 C11 H13A 0.3198 0.3469 0.3392 23 0.990 0.000 C13 O4 C14 H13B 0.2715 0.5141 0.3423 23 0.990 0.000 C13 O4 C14 H14A 0.3207 0.4495 0.2323 23 0.990 0.000 C14 O5 C13 H14B 0.2582 0.3011 0.2315 23 0.990 0.000 C14 O5 C13 04sjc0831 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.10650 0.60276 0.15602 1.00000 0.02880 0.02317 0.02748 -0.00006 0.00390 -0.00149 0.02648 0.00311 0.00011 0.00022 0.00009 0.00000 0.00096 0.00097 0.00106 0.00078 0.00076 0.00083 0.00043 C2 0.07667 0.61560 0.09181 1.00000 0.03764 0.03455 0.03173 0.00510 -0.00151 -0.00142 0.03464 0.00345 0.00012 0.00025 0.00010 0.00000 0.00113 0.00118 0.00116 0.00088 0.00086 0.00092 0.00049 H2 0.02740 0.67131 0.08366 1.00000 0.04157 0.00000 0.00000 C3 0.11916 0.54657 0.03925 1.00000 0.04767 0.04840 0.02825 0.00083 0.00337 -0.00843 0.04144 0.00366 0.00013 0.00027 0.00010 0.00000 0.00136 0.00138 0.00116 0.00097 0.00091 0.00111 0.00055 H3 0.09858 0.55458 -0.00486 1.00000 0.04973 0.00000 0.00000 C4 0.19043 0.46720 0.05067 1.00000 0.04144 0.04096 0.03461 -0.00740 0.01399 -0.00867 0.03900 0.00357 0.00012 0.00026 0.00010 0.00000 0.00122 0.00129 0.00122 0.00094 0.00091 0.00105 0.00053 H4 0.21882 0.42032 0.01435 1.00000 0.04680 0.00000 0.00000 C5 0.22184 0.45428 0.11478 1.00000 0.02777 0.02697 0.04314 -0.00369 0.00927 -0.00489 0.03263 0.00330 0.00011 0.00023 0.00010 0.00000 0.00098 0.00108 0.00127 0.00088 0.00082 0.00085 0.00048 H5 0.27146 0.39922 0.12228 1.00000 0.03916 0.00000 0.00000 C6 0.18018 0.52231 0.16750 1.00000 0.02721 0.01815 0.03063 0.00080 0.00207 -0.00518 0.02533 0.00303 0.00010 0.00021 0.00009 0.00000 0.00097 0.00093 0.00108 0.00076 0.00075 0.00079 0.00042 C7 -0.01388 0.70714 0.20599 1.00000 0.02814 0.02658 0.03514 0.00188 -0.00441 0.00699 0.02995 0.00332 0.00011 0.00023 0.00009 0.00000 0.00099 0.00105 0.00113 0.00085 0.00081 0.00084 0.00045 H7A -0.04611 0.62092 0.18471 1.00000 0.03595 0.00000 0.00000 H7B -0.01837 0.80533 0.17840 1.00000 0.03595 0.00000 0.00000 C8 -0.04430 0.73872 0.27450 1.00000 0.03007 0.02711 0.03877 0.00025 -0.00064 0.00642 0.03198 0.00346 0.00011 0.00024 0.00009 0.00000 0.00103 0.00105 0.00120 0.00086 0.00082 0.00086 0.00047 H8A -0.00615 0.81016 0.29843 1.00000 0.03838 0.00000 0.00000 H8B -0.09768 0.79279 0.27232 1.00000 0.03838 0.00000 0.00000 C9 -0.06303 0.60894 0.37886 1.00000 0.02904 0.03955 0.03182 -0.00337 0.00427 0.00404 0.03347 0.00339 0.00011 0.00026 0.00009 0.00000 0.00101 0.00120 0.00114 0.00090 0.00081 0.00090 0.00047 H9A -0.09204 0.51393 0.39652 1.00000 0.04016 0.00000 0.00000 H9B -0.09734 0.70451 0.38703 1.00000 0.04016 0.00000 0.00000 C10 0.01605 0.62825 0.41580 1.00000 0.03355 0.03097 0.03057 -0.00542 0.00155 0.00278 0.03170 0.00329 0.00011 0.00023 0.00009 0.00000 0.00107 0.00113 0.00110 0.00083 0.00081 0.00087 0.00047 H10A 0.04784 0.71746 0.39626 1.00000 0.03804 0.00000 0.00000 H10B 0.00554 0.65323 0.46327 1.00000 0.03804 0.00000 0.00000 C11 0.14053 0.49438 0.43276 1.00000 0.03050 0.03579 0.03262 -0.00446 -0.00471 -0.00251 0.03297 0.00322 0.00011 0.00024 0.00010 0.00000 0.00100 0.00118 0.00109 0.00090 0.00080 0.00091 0.00046 H11A 0.14142 0.51220 0.48155 1.00000 0.03957 0.00000 0.00000 H11B 0.16752 0.58667 0.41095 1.00000 0.03957 0.00000 0.00000 C12 0.18465 0.34160 0.41604 1.00000 0.03622 0.03325 0.03400 0.00366 -0.00595 -0.00122 0.03449 0.00344 0.00012 0.00024 0.00010 0.00000 0.00112 0.00117 0.00119 0.00088 0.00084 0.00092 0.00049 H12A 0.23699 0.34037 0.44019 1.00000 0.04139 0.00000 0.00000 H12B 0.15223 0.24936 0.43215 1.00000 0.04139 0.00000 0.00000 C13 0.27036 0.40367 0.32405 1.00000 0.02391 0.02605 0.05061 0.00720 -0.00423 -0.00005 0.03352 0.00345 0.00011 0.00024 0.00010 0.00000 0.00100 0.00108 0.00132 0.00091 0.00083 0.00084 0.00049 H13A 0.31975 0.34688 0.33922 1.00000 0.04023 0.00000 0.00000 H13B 0.27148 0.51412 0.34232 1.00000 0.04023 0.00000 0.00000 C14 0.26840 0.40942 0.24999 1.00000 0.02225 0.02431 0.04669 0.00427 0.00257 0.00376 0.03108 0.00345 0.00010 0.00023 0.00010 0.00000 0.00095 0.00100 0.00123 0.00088 0.00081 0.00081 0.00046 H14A 0.32067 0.44945 0.23232 1.00000 0.03730 0.00000 0.00000 H14B 0.25823 0.30107 0.23146 1.00000 0.03730 0.00000 0.00000 O1 0.06936 0.65908 0.21157 1.00000 0.02666 0.03017 0.03033 -0.00221 -0.00166 0.00667 0.02906 0.00212 0.00007 0.00015 0.00006 0.00000 0.00067 0.00074 0.00075 0.00057 0.00054 0.00057 0.00033 O2 -0.05174 0.59002 0.30918 1.00000 0.03164 0.02860 0.02946 -0.00137 -0.00073 0.00012 0.02990 0.00213 0.00007 0.00015 0.00006 0.00000 0.00071 0.00075 0.00075 0.00057 0.00054 0.00059 0.00033 O3 0.05977 0.48216 0.41035 1.00000 0.02758 0.03098 0.03595 -0.00404 -0.00575 0.00035 0.03150 0.00209 0.00007 0.00016 0.00006 0.00000 0.00069 0.00077 0.00079 0.00059 0.00054 0.00059 0.00034 O4 0.19986 0.32128 0.34725 1.00000 0.03216 0.02486 0.03766 0.00056 0.00132 -0.00283 0.03156 0.00217 0.00007 0.00015 0.00006 0.00000 0.00071 0.00073 0.00082 0.00056 0.00057 0.00059 0.00034 O5 0.20375 0.51684 0.23245 1.00000 0.02539 0.02104 0.03462 -0.00197 -0.00224 0.00373 0.02702 0.00205 0.00007 0.00014 0.00006 0.00000 0.00065 0.00068 0.00077 0.00053 0.00051 0.00055 0.00032 Final Structure Factor Calculation for 04sjc0831 in Pbca Total number of l.s. parameters = 173 Maximum vector length = 511 Memory required = 2362 / 21973 wR2 = 0.1192 before cycle 5 for 3155 data and 0 / 173 parameters GooF = S = 0.974; Restrained GooF = 0.974 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0458 * P )^2 + 0.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0487 for 1990 Fo > 4sig(Fo) and 0.0977 for all 3155 data wR2 = 0.1192, GooF = S = 0.974, Restrained GooF = 0.974 for all data Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0323 0.0247 0.0225 C1 0.0401 0.0360 0.0278 C2 0.0566 0.0403 0.0274 C3 0.0594 0.0340 0.0236 C4 0.0489 0.0275 0.0215 C5 0.0318 0.0285 0.0156 C6 0.0375 0.0332 0.0191 C7 0.0388 0.0351 0.0220 C8 0.0414 0.0349 0.0241 C9 0.0366 0.0342 0.0243 C10 0.0390 0.0352 0.0247 C11 0.0424 0.0330 0.0281 C12 0.0531 0.0248 0.0226 C13 0.0479 0.0260 0.0194 C14 0.0365 0.0291 0.0215 O1 0.0320 0.0302 0.0276 O2 0.0404 0.0299 0.0242 O3 0.0380 0.0329 0.0238 O4 0.0357 0.0265 0.0189 O5 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.013 0.020 0.027 0.035 0.045 0.059 0.080 0.123 1.000 Number in group 344. 299. 343. 290. 311. 331. 304. 307. 313. 313. GooF 0.924 0.903 0.998 1.019 0.992 1.114 1.049 0.869 0.895 0.948 K 3.772 1.756 1.155 0.970 1.000 0.998 0.988 0.995 1.002 1.017 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.64 inf Number in group 323. 312. 316. 316. 309. 319. 317. 315. 310. 318. GooF 0.847 0.863 0.894 0.953 0.959 1.012 0.983 0.901 1.141 1.142 K 0.972 1.043 1.021 1.032 1.002 1.001 1.023 1.013 1.029 1.011 R1 0.314 0.284 0.231 0.185 0.119 0.101 0.060 0.041 0.042 0.030 Recommended weighting scheme: WGHT 0.0420 0.4765 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) 6 3 9 126.39 27.08 7.38 0.021 1.47 9 3 6 35.50 0.45 5.13 0.003 1.39 9 3 3 53.85 11.16 5.03 0.014 1.49 4 0 12 43.25 117.40 4.93 0.045 1.55 2 1 2 15.42 0.17 3.71 0.002 5.06 4 2 10 121.01 76.26 3.61 0.036 1.66 3 6 9 109.95 62.93 3.58 0.033 1.15 0 4 3 366.45 484.79 3.57 0.091 1.99 2 1 0 429.98 557.13 3.55 0.097 5.86 3 6 6 162.84 108.69 3.21 0.043 1.25 3 1 9 145.44 100.12 3.20 0.041 2.00 9 0 12 163.70 99.05 3.19 0.041 1.24 6 8 4 25.24 73.27 3.09 0.035 0.96 15 0 6 1734.49 1446.11 3.04 0.157 1.04 9 7 1 63.95 121.83 3.03 0.046 1.00 1 1 9 203.77 152.89 2.97 0.051 2.14 3 6 5 141.79 198.55 2.97 0.058 1.28 1 1 1 1741.91 2056.51 2.96 0.187 6.97 4 2 6 256.67 198.01 2.96 0.058 2.20 0 10 6 7.28 107.66 2.93 0.043 0.81 10 2 14 49.18 88.02 2.91 0.039 1.05 11 5 13 65.12 114.70 2.89 0.044 0.90 0 0 14 61.67 8.66 2.87 0.012 1.43 3 8 4 49.33 9.22 2.86 0.013 1.00 18 4 10 53.82 159.01 2.85 0.052 0.77 1 5 2 10.74 37.30 2.82 0.025 1.63 4 4 4 16.11 0.00 2.82 0.000 1.74 17 3 4 192.58 115.55 2.80 0.044 0.90 6 2 0 1007.53 1216.54 2.78 0.144 2.29 8 4 15 44.87 9.63 2.67 0.013 0.99 3 1 4 666.80 781.82 2.66 0.115 3.39 5 8 1 86.20 141.24 2.64 0.049 0.99 2 4 2 20.91 0.30 2.63 0.002 1.98 11 4 3 111.71 64.37 2.62 0.033 1.20 14 3 7 71.21 118.24 2.62 0.045 1.01 13 5 3 -22.50 22.88 2.56 0.020 1.00 1 1 13 34.13 12.31 2.56 0.014 1.51 3 7 7 28.19 0.23 2.56 0.002 1.08 6 10 4 -32.01 70.32 2.54 0.035 0.79 9 1 16 0.13 30.82 2.54 0.023 1.03 0 0 12 2420.27 1981.01 2.53 0.184 1.67 14 6 6 -44.59 27.36 2.53 0.022 0.87 6 3 19 86.38 133.81 2.53 0.048 0.93 3 1 17 320.77 397.88 2.52 0.082 1.14 8 1 15 31.68 6.66 2.50 0.011 1.11 6 6 6 127.69 90.18 2.50 0.039 1.16 4 1 18 19.75 49.44 2.49 0.029 1.07 1 0 4 2042.84 2363.28 2.49 0.201 4.80 8 2 7 140.80 181.00 2.48 0.056 1.55 0 4 19 73.47 140.57 2.48 0.049 0.94 Bond lengths and angles C1 - Distance Angles O1 1.3552 (0.0021) C2 1.3830 (0.0027) 125.33 (0.17) C6 1.4068 (0.0025) 114.87 (0.16) 119.78 (0.17) C1 - O1 C2 C2 - Distance Angles C1 1.3830 (0.0027) C3 1.3906 (0.0029) 119.67 (0.19) H2 0.9500 120.17 120.17 C2 - C1 C3 C3 - Distance Angles C4 1.3679 (0.0030) C2 1.3906 (0.0029) 120.39 (0.20) H3 0.9500 119.81 119.81 C3 - C4 C2 C4 - Distance Angles C3 1.3679 (0.0030) C5 1.3907 (0.0029) 120.83 (0.19) H4 0.9500 119.58 119.58 C4 - C3 C5 C5 - Distance Angles C6 1.3827 (0.0026) C4 1.3907 (0.0029) 119.37 (0.19) H5 0.9500 120.31 120.32 C5 - C6 C4 C6 - Distance Angles O5 1.3605 (0.0021) C5 1.3827 (0.0026) 125.22 (0.17) C1 1.4068 (0.0025) 114.81 (0.15) 119.95 (0.17) C6 - O5 C5 C7 - Distance Angles O1 1.4346 (0.0021) C8 1.4866 (0.0026) 107.48 (0.14) H7A 0.9900 110.22 110.22 H7B 0.9900 110.22 110.22 108.50 C7 - O1 C8 H7A C8 - Distance Angles O2 1.4253 (0.0023) C7 1.4866 (0.0026) 109.07 (0.15) H8A 0.9900 109.87 109.87 H8B 0.9900 109.87 109.87 108.29 C8 - O2 C7 H8A C9 - Distance Angles O2 1.4191 (0.0023) C10 1.5088 (0.0026) 112.47 (0.15) H9A 0.9900 109.11 109.11 H9B 0.9900 109.11 109.11 107.85 C9 - O2 C10 H9A C10 - Distance Angles O3 1.4182 (0.0022) C9 1.5088 (0.0026) 108.09 (0.15) H10A 0.9900 110.08 110.08 H10B 0.9900 110.08 110.08 108.42 C10 - O3 C9 H10A C11 - Distance Angles O3 1.4097 (0.0021) C12 1.5033 (0.0028) 108.99 (0.15) H11A 0.9900 109.89 109.89 H11B 0.9900 109.89 109.89 108.30 C11 - O3 C12 H11A C12 - Distance Angles O4 1.4128 (0.0023) C11 1.5033 (0.0028) 113.91 (0.16) H12A 0.9900 108.77 108.77 H12B 0.9900 108.77 108.77 107.66 C12 - O4 C11 H12A C13 - Distance Angles O4 1.4282 (0.0022) C14 1.4868 (0.0029) 108.87 (0.15) H13A 0.9900 109.91 109.91 H13B 0.9900 109.91 109.91 108.31 C13 - O4 C14 H13A C14 - Distance Angles O5 1.4356 (0.0021) C13 1.4868 (0.0029) 106.33 (0.15) H14A 0.9900 110.46 110.46 H14B 0.9900 110.46 110.47 108.65 C14 - O5 C13 H14A O1 - Distance Angles C1 1.3552 (0.0021) C7 1.4346 (0.0021) 117.71 (0.14) O1 - C1 O2 - Distance Angles C9 1.4191 (0.0023) C8 1.4253 (0.0023) 113.31 (0.14) O2 - C9 O3 - Distance Angles C11 1.4097 (0.0021) C10 1.4182 (0.0022) 113.21 (0.14) O3 - C11 O4 - Distance Angles C12 1.4128 (0.0023) C13 1.4282 (0.0022) 113.92 (0.14) O4 - C12 O5 - Distance Angles C6 1.3605 (0.0021) C14 1.4356 (0.0021) 117.90 (0.14) O5 - C6 FMAP and GRID set by program FMAP 2 1 21 GRID -1.389 -2 -1 1.389 2 1 R1 = 0.0976 for 3155 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.21 at 0.2204 0.3228 0.2205 [ 0.69 A from H14B ] Deepest hole -0.19 at 0.0431 0.3498 0.2491 [ 1.04 A from C8 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2605 / 26520 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2204 0.3228 0.2205 1.00000 0.05 0.21 0.69 H14B 1.22 C14 1.66 O5 1.98 H14A Q2 1 0.0041 0.5653 0.2958 1.00000 0.05 0.20 0.98 O2 1.70 C8 2.03 C9 2.05 H8A Q3 1 -0.0857 0.5090 0.2679 1.00000 0.05 0.20 1.21 O2 1.62 H14A 2.02 H7A 2.03 C8 Q4 1 0.1386 0.2562 0.4196 1.00000 0.05 0.17 0.34 H12B 1.04 C12 1.82 H12A 1.85 O4 Q5 1 0.0338 0.5981 0.3328 1.00000 0.05 0.17 1.49 O2 1.63 H10A 1.71 C10 1.85 C9 Q6 1 0.0449 0.6772 0.2882 1.00000 0.05 0.17 1.41 H8A 1.58 C8 1.60 O1 1.80 O2 Q7 1 -0.1109 0.6397 0.3988 1.00000 0.05 0.17 0.63 H9B 0.92 C9 1.09 H9A 2.09 O2 Q8 1 0.0528 0.5140 0.2406 1.00000 0.05 0.16 1.37 O1 2.00 H8B 2.02 H8A 2.05 C1 Q9 1 0.0633 0.4925 0.3598 1.00000 0.05 0.16 1.02 O3 1.77 C10 1.89 H7B 1.94 C11 Q10 1 0.1237 0.1442 0.4384 1.00000 0.05 0.16 1.00 H12B 1.98 C12 2.05 H3 2.25 H4 Shortest distances between peaks (including symmetry equivalents) 2 5 0.93 4 10 1.03 5 6 1.13 5 9 1.14 2 6 1.16 2 8 1.43 2 3 1.65 6 8 1.67 2 9 1.72 5 8 2.00 6 9 2.13 3 8 2.35 8 9 2.40 3 5 2.48 3 6 2.60 4 9 2.62 5 7 2.75 2 7 2.87 3 7 2.87 Time profile in seconds ----------------------- 0.05: 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. 0.91: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.92: Structure factors and derivatives 0.50: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.03: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.05: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04sjc0831 finished at 09:34:34 Total CPU time: 2.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++