+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 19:14:24 on 23-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh068 in Pna2(1) CELL 0.71073 10.0265 4.5597 29.0659 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0002 0.0011 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H N O UNIT 60 64 8 12 V = 1328.83 F(000) = 576.0 Mu = 0.10 mm-1 Cell Wt = 1089.19 Rho = 1.361 MERG 2 OMIT -3.00 55.00 OMIT 2 1 0 OMIT 2 0 2 DFIX 0.88 0.02 N1 H1N N2 H2N EQIV $1 x, y+1, z HTAB N1 O1_$1 HTAB N2 O1_$1 FMAP 2 PLAN 5 SIZE 0.08 0.40 0.50 ACTA HTAB 2.00000 BOND $H WGHT 0.06860 0.10580 L.S. 6 TEMP -153.00 FVAR 0.79983 O2 4 0.487671 0.603828 0.128412 11.00000 0.04273 0.05751 = 0.01469 -0.00334 -0.00076 -0.01318 O3 4 0.750546 0.608992 0.524573 11.00000 0.04638 0.04893 = 0.01504 0.00321 -0.00218 0.01356 C15 1 0.643801 0.801389 0.535671 11.00000 0.04838 0.04813 = 0.01296 -0.00108 0.00357 0.00671 AFIX 137 H15A 2 0.663079 0.997490 0.523580 11.00000 -1.50000 H15B 2 0.633626 0.811628 0.569166 11.00000 -1.50000 H15C 2 0.561080 0.727741 0.521922 11.00000 -1.50000 AFIX 0 C14 1 0.595936 0.794978 0.117510 11.00000 0.04123 0.05566 = 0.02260 0.00621 0.00631 -0.00977 AFIX 137 H14A 2 0.576592 0.992222 0.129122 11.00000 -1.50000 H14B 2 0.607728 0.802520 0.084061 11.00000 -1.50000 H14C 2 0.677802 0.721397 0.131864 11.00000 -1.50000 AFIX 0 C1 1 0.489650 0.627559 0.255305 11.00000 0.01955 0.01311 = 0.01759 -0.00080 -0.00494 0.00396 C2 1 0.526996 0.691584 0.210300 11.00000 0.02170 0.02085 = 0.01929 0.00212 -0.00032 0.00034 AFIX 43 H2 2 0.597671 0.825114 0.204377 11.00000 -1.20000 AFIX 0 C3 1 0.459698 0.557901 0.174080 11.00000 0.02783 0.02762 = 0.01678 -0.00405 -0.00366 0.00404 C4 1 0.357183 0.359486 0.182871 11.00000 0.02796 0.02517 = 0.02536 -0.00561 -0.00974 0.00115 AFIX 43 H4 2 0.312822 0.264951 0.158088 11.00000 -1.20000 AFIX 0 C5 1 0.320082 0.300348 0.227807 11.00000 0.02294 0.02258 = 0.02981 -0.00097 -0.00261 -0.00363 AFIX 43 H5 2 0.250021 0.165279 0.233741 11.00000 -1.20000 AFIX 0 C6 1 0.384594 0.437164 0.264323 11.00000 0.02328 0.02074 = 0.02022 0.00029 -0.00050 -0.00010 AFIX 43 H6 2 0.357167 0.400897 0.295086 11.00000 -1.20000 AFIX 0 C7 1 0.616684 0.604648 0.326720 11.00000 0.01742 0.01482 = 0.01577 0.00097 -0.00116 -0.00048 C8 1 0.745006 0.628826 0.397577 11.00000 0.02056 0.01336 = 0.01769 0.00174 -0.00347 -0.00525 C9 1 0.708892 0.694626 0.442633 11.00000 0.02129 0.01911 = 0.01815 0.00162 -0.00249 0.00055 AFIX 43 H9 2 0.638701 0.829119 0.448705 11.00000 -1.20000 AFIX 0 C10 1 0.776986 0.560750 0.478675 11.00000 0.02666 0.02636 = 0.01627 0.00178 -0.00009 -0.00310 C11 1 0.878356 0.358975 0.469932 11.00000 0.02492 0.02661 = 0.02314 0.00481 -0.00612 0.00183 AFIX 43 H11 2 0.922353 0.263222 0.494676 11.00000 -1.20000 AFIX 0 C12 1 0.914240 0.299497 0.425131 11.00000 0.02010 0.02231 = 0.02925 -0.00161 -0.00536 -0.00020 AFIX 43 H12 2 0.984255 0.164550 0.419066 11.00000 -1.20000 AFIX 0 C13 1 0.848555 0.435914 0.388564 11.00000 0.02186 0.01756 = 0.01974 -0.00247 -0.00085 -0.00151 AFIX 43 H13 2 0.874657 0.396767 0.357751 11.00000 -1.20000 AFIX 0 N1 3 0.559213 0.764216 0.292360 11.00000 0.02652 0.01101 = 0.01793 0.00062 -0.00479 -0.00167 N2 3 0.675157 0.763836 0.360803 11.00000 0.02957 0.00913 = 0.01427 -0.00043 -0.00309 0.00098 O1 4 0.616684 0.332995 0.326429 11.00000 0.03125 0.01288 = 0.02360 0.00047 -0.00777 0.00014 H1N 2 0.573167 0.946952 0.292742 11.00000 -1.20000 H2N 2 0.663353 0.944882 0.362726 11.00000 -1.20000 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 2008lsh068 in Pna2(1) C 0.770 H 0.320 N 0.700 O 0.660 O2 - C3 C14 O3 - C10 C15 C15 - O3 C14 - O2 C1 - C6 C2 N1 C2 - C3 C1 C3 - O2 C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C1 C5 C7 - O1 N2 N1 C8 - C13 C9 N2 C9 - C8 C10 C10 - O3 C9 C11 C11 - C12 C10 C12 - C11 C13 C13 - C8 C12 N1 - C7 C1 N2 - C7 C8 O1 - C7 Operators for generating equivalent atoms: $1 x, y+1, z Floating origin restraints generated 8707 Reflections read, of which 966 rejected -12 =< h =< 12, -5 =< k =< 5, -37 =< l =< 20, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 2273 Unique reflections, of which 0 suppressed R(int) = 0.0453 R(sigma) = 0.0485 Friedel opposites not merged Maximum memory for data reduction = 1984 / 22648 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 = 2503 / 234486 wR2 = 0.1156 before cycle 1 for 2273 data and 189 / 189 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 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.055; Restrained GooF = 1.056 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 0.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.79752 0.00213 -1.084 OSF Mean shift/esd = 0.073 Maximum = -1.084 for OSF Max. shift = 0.003 A for H2N Max. dU = 0.000 for O3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2503 / 234486 wR2 = 0.1155 before cycle 2 for 2273 data and 189 / 189 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 0.038 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.055 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 0.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.79696 0.00213 -0.263 OSF Mean shift/esd = 0.024 Maximum = -0.263 for OSF Max. shift = 0.001 A for H2N Max. dU = 0.000 for C14 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2503 / 234486 wR2 = 0.1155 before cycle 3 for 2273 data and 189 / 189 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 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.055 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 0.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.79694 0.00213 -0.007 OSF Mean shift/esd = 0.002 Maximum = -0.011 for U33 C14 Max. shift = 0.000 A for H2N Max. dU = 0.000 for C14 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2503 / 234486 wR2 = 0.1155 before cycle 4 for 2273 data and 189 / 189 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 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.055 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 0.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.79694 0.00213 -0.001 OSF Mean shift/esd = 0.001 Maximum = 0.005 for U33 C15 Max. shift = 0.000 A for H2N Max. dU = 0.000 for C15 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2503 / 234486 wR2 = 0.1155 before cycle 5 for 2273 data and 189 / 189 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 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.055 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 0.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.79694 0.00213 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for y C14 Max. shift = 0.000 A for H2N Max. dU = 0.000 for C14 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2503 / 234486 wR2 = 0.1155 before cycle 6 for 2273 data and 189 / 189 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 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.055 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 0.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.79694 0.00213 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y C15 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C14 Largest correlation matrix elements 0.746 z N2 / z N1 0.594 U23 C9 / U23 C2 -0.546 U22 C8 / U22 C1 -0.693 U22 N2 / U22 N1 0.587 U23 C12 / U23 C5 -0.540 y C12 / y C5 -0.683 U33 N2 / U33 N1 -0.567 U33 C12 / U33 C5 0.505 U23 C14 / U23 C15 -0.672 U33 C14 / U33 C15 -0.561 y C9 / y C2 0.502 U12 C9 / U12 C2 0.619 z C14 / z C15 0.556 z C12 / z C5 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H15A 0.6629 0.9974 0.5235 137 0.980 0.000 C15 O3 H15A H15B 0.6338 0.8122 0.5692 137 0.980 0.000 C15 O3 H15A H15C 0.5610 0.7275 0.5220 137 0.980 0.000 C15 O3 H15A H14A 0.5766 0.9921 0.1292 137 0.980 0.000 C14 O2 H14A H14B 0.6077 0.8026 0.0841 137 0.980 0.000 C14 O2 H14A H14C 0.6778 0.7212 0.1319 137 0.980 0.000 C14 O2 H14A H2 0.5977 0.8252 0.2044 43 0.950 0.000 C2 C3 C1 H4 0.3128 0.2649 0.1581 43 0.950 0.000 C4 C5 C3 H5 0.2501 0.1651 0.2338 43 0.950 0.000 C5 C4 C6 H6 0.3571 0.4010 0.2951 43 0.950 0.000 C6 C1 C5 H9 0.6387 0.8292 0.4487 43 0.950 0.000 C9 C8 C10 H11 0.9224 0.2633 0.4947 43 0.950 0.000 C11 C12 C10 H12 0.9842 0.1645 0.4191 43 0.950 0.000 C12 C11 C13 H13 0.8747 0.3968 0.3577 43 0.950 0.000 C13 C8 C12 2008lsh068 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O2 0.48765 0.60384 0.12840 1.00000 0.04259 0.05723 0.01458 -0.00326 -0.00071 -0.01313 0.03813 0.00346 0.00019 0.00048 0.00007 0.00000 0.00114 0.00147 0.00095 0.00098 0.00092 0.00101 0.00053 O3 0.75056 0.60894 0.52457 1.00000 0.04614 0.04872 0.01481 0.00319 -0.00204 0.01369 0.03655 0.00381 0.00020 0.00048 0.00007 0.00000 0.00112 0.00138 0.00097 0.00100 0.00091 0.00095 0.00052 C15 0.64378 0.80145 0.53567 1.00000 0.04815 0.04812 0.01298 -0.00110 0.00371 0.00671 0.03642 0.00588 0.00030 0.00078 0.00011 0.00000 0.00163 0.00174 0.00163 0.00145 0.00132 0.00152 0.00074 H15A 0.66292 0.99738 0.52349 1.00000 0.05462 0.00000 0.00000 H15B 0.63383 0.81223 0.56917 1.00000 0.05462 0.00000 0.00000 H15C 0.56099 0.72745 0.52202 1.00000 0.05462 0.00000 0.00000 C14 0.59595 0.79493 0.11752 1.00000 0.04104 0.05547 0.02223 0.00629 0.00619 -0.00977 0.03958 0.00607 0.00031 0.00079 0.00013 0.00000 0.00176 0.00206 0.00189 0.00162 0.00138 0.00162 0.00082 H14A 0.57665 0.99213 0.12916 1.00000 0.05937 0.00000 0.00000 H14B 0.60773 0.80264 0.08407 1.00000 0.05937 0.00000 0.00000 H14C 0.67780 0.72118 0.13186 1.00000 0.05937 0.00000 0.00000 C1 0.48964 0.62759 0.25530 1.00000 0.01930 0.01289 0.01751 -0.00084 -0.00499 0.00390 0.01657 0.00397 0.00022 0.00047 0.00009 0.00000 0.00106 0.00116 0.00126 0.00100 0.00095 0.00085 0.00050 C2 0.52702 0.69162 0.21030 1.00000 0.02148 0.02065 0.01915 0.00208 -0.00035 0.00035 0.02043 0.00480 0.00024 0.00062 0.00010 0.00000 0.00113 0.00106 0.00138 0.00125 0.00106 0.00109 0.00053 H2 0.59769 0.82516 0.20438 1.00000 0.02451 0.00000 0.00000 C3 0.45972 0.55787 0.17408 1.00000 0.02767 0.02733 0.01659 -0.00405 -0.00364 0.00397 0.02386 0.00447 0.00024 0.00056 0.00009 0.00000 0.00131 0.00126 0.00118 0.00111 0.00110 0.00107 0.00054 C4 0.35716 0.35938 0.18286 1.00000 0.02789 0.02490 0.02523 -0.00555 -0.00967 0.00114 0.02601 0.00438 0.00025 0.00058 0.00009 0.00000 0.00130 0.00146 0.00155 0.00119 0.00116 0.00109 0.00061 H4 0.31279 0.26486 0.15808 1.00000 0.03121 0.00000 0.00000 C5 0.32009 0.30027 0.22781 1.00000 0.02275 0.02241 0.02953 -0.00102 -0.00255 -0.00370 0.02489 0.00508 0.00025 0.00066 0.00012 0.00000 0.00127 0.00125 0.00166 0.00136 0.00113 0.00108 0.00062 H5 0.25007 0.16513 0.23375 1.00000 0.02987 0.00000 0.00000 C6 0.38457 0.43720 0.26433 1.00000 0.02307 0.02060 0.01997 0.00032 -0.00052 -0.00012 0.02121 0.00427 0.00024 0.00054 0.00009 0.00000 0.00114 0.00116 0.00131 0.00103 0.00099 0.00097 0.00053 H6 0.35712 0.40102 0.29509 1.00000 0.02545 0.00000 0.00000 C7 0.61670 0.60463 0.32672 1.00000 0.01720 0.01467 0.01557 0.00098 -0.00120 -0.00049 0.01581 0.00423 0.00025 0.00037 0.00010 0.00000 0.00089 0.00085 0.00090 0.00114 0.00076 0.00092 0.00039 C8 0.74496 0.62883 0.39758 1.00000 0.02037 0.01319 0.01751 0.00169 -0.00350 -0.00521 0.01702 0.00386 0.00022 0.00047 0.00009 0.00000 0.00114 0.00119 0.00124 0.00097 0.00096 0.00084 0.00050 C9 0.70887 0.69469 0.44263 1.00000 0.02107 0.01891 0.01795 0.00150 -0.00245 0.00063 0.01931 0.00458 0.00024 0.00061 0.00009 0.00000 0.00112 0.00098 0.00133 0.00118 0.00102 0.00107 0.00051 H9 0.63870 0.82922 0.44871 1.00000 0.02317 0.00000 0.00000 C10 0.77699 0.56077 0.47867 1.00000 0.02645 0.02613 0.01611 0.00177 -0.00018 -0.00310 0.02289 0.00434 0.00024 0.00057 0.00009 0.00000 0.00122 0.00131 0.00122 0.00109 0.00103 0.00108 0.00055 C11 0.87836 0.35899 0.46993 1.00000 0.02458 0.02638 0.02305 0.00488 -0.00614 0.00177 0.02467 0.00452 0.00024 0.00058 0.00010 0.00000 0.00119 0.00151 0.00147 0.00122 0.00110 0.00105 0.00058 H11 0.92237 0.26325 0.49468 1.00000 0.02961 0.00000 0.00000 C12 0.91423 0.29949 0.42513 1.00000 0.01991 0.02207 0.02930 -0.00167 -0.00539 -0.00024 0.02376 0.00466 0.00023 0.00063 0.00011 0.00000 0.00115 0.00125 0.00172 0.00133 0.00117 0.00111 0.00061 H12 0.98423 0.16450 0.41907 1.00000 0.02851 0.00000 0.00000 C13 0.84857 0.43588 0.38856 1.00000 0.02166 0.01738 0.01957 -0.00249 -0.00082 -0.00142 0.01954 0.00409 0.00023 0.00052 0.00009 0.00000 0.00117 0.00109 0.00124 0.00099 0.00102 0.00092 0.00050 H13 0.87469 0.39675 0.35775 1.00000 0.02344 0.00000 0.00000 N1 0.55921 0.76424 0.29237 1.00000 0.02630 0.01097 0.01768 0.00063 -0.00475 -0.00164 0.01832 0.00400 0.00021 0.00041 0.00010 0.00000 0.00103 0.00121 0.00137 0.00081 0.00098 0.00078 0.00054 N2 0.67513 0.76391 0.36082 1.00000 0.02926 0.00911 0.01394 -0.00049 -0.00309 0.00091 0.01744 0.00410 0.00022 0.00041 0.00010 0.00000 0.00108 0.00116 0.00128 0.00073 0.00091 0.00079 0.00052 O1 0.61666 0.33296 0.32643 1.00000 0.03106 0.01264 0.02341 0.00049 -0.00781 0.00012 0.02237 0.00313 0.00019 0.00026 0.00008 0.00000 0.00077 0.00065 0.00074 0.00109 0.00063 0.00085 0.00034 H1N 0.57313 0.94759 0.29276 1.00000 0.02684 0.04649 0.00276 0.00381 0.00114 0.00000 0.00000 H2N 0.66325 0.94585 0.36270 1.00000 0.02684 0.04641 0.00260 0.00388 0.00119 0.00000 0.00000 Final Structure Factor Calculation for 2008lsh068 in Pna2(1) Total number of l.s. parameters = 189 Maximum vector length = 511 Memory required = 2316 / 25046 wR2 = 0.1155 before cycle 7 for 2273 data and 2 / 189 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 0.036 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.055 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0686 * P )^2 + 0.11 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0433 for 1910 Fo > 4sig(Fo) and 0.0548 for all 2273 data wR2 = 0.1155, GooF = S = 1.054, Restrained GooF = 1.055 for all data Flack x parameter = -0.5171 with esd 1.5865 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 Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0651 0.0351 0.0142 O2 0.0612 0.0344 0.0141 O3 0.0549 0.0418 0.0125 C15 0.0606 0.0400 0.0181 C14 0.0246 0.0145 0.0106 C1 0.0221 0.0215 0.0176 C2 0.0332 0.0235 0.0148 C3 0.0379 0.0247 0.0154 C4 0.0304 0.0260 0.0183 C5 0.0232 0.0207 0.0198 C6 0.0181 0.0153 0.0140 C7 0.0251 0.0155 0.0105 C8 0.0224 0.0197 0.0158 C9 0.0295 0.0234 0.0158 C10 0.0312 0.0274 0.0154 C11 0.0320 0.0220 0.0173 C12 0.0221 0.0212 0.0153 C13 0.0286 0.0156 0.0108 N1 0.0299 0.0134 0.0090 N2 0.0359 0.0186 0.0126 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.019 0.031 0.042 0.053 0.068 0.083 0.100 0.136 0.199 1.000 Number in group 228. 242. 224. 225. 229. 222. 224. 224. 226. 229. GooF 0.907 0.946 1.166 1.202 1.151 1.033 1.027 1.035 0.963 1.075 K 0.912 0.937 0.958 0.997 0.964 1.008 1.004 1.008 1.018 1.003 Resolution(A) 0.77 0.81 0.84 0.89 0.94 1.01 1.10 1.24 1.43 1.81 inf Number in group 230. 231. 234. 217. 229. 225. 224. 230. 229. 224. GooF 1.062 1.059 1.138 1.017 0.955 0.978 0.930 0.931 1.181 1.238 K 1.028 1.021 1.011 1.024 1.025 1.010 1.008 1.003 1.042 0.989 R1 0.142 0.117 0.099 0.072 0.056 0.047 0.035 0.034 0.037 0.035 Recommended weighting scheme: WGHT 0.0677 0.1104 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 -22 924.63 1396.33 4.38 0.295 1.17 5 2 13 140.25 226.87 4.13 0.119 1.25 2 4 -20 34.43 71.28 3.47 0.067 0.88 0 3 -29 34.14 62.27 3.41 0.062 0.84 0 2 4 40.06 28.28 3.39 0.042 2.18 1 1 -1 5142.97 6571.00 3.32 0.641 4.11 2 2 9 81.42 57.03 3.28 0.060 1.75 1 1 0 2493.10 3165.23 3.23 0.445 4.15 4 4 2 52.01 33.76 3.18 0.046 1.04 0 2 -22 3.19 22.97 3.13 0.038 1.14 6 1 4 28.74 20.57 3.10 0.036 1.53 12 0 -14 24.61 45.97 3.08 0.054 0.78 2 2 -9 74.35 56.99 3.04 0.060 1.75 7 3 -19 -4.45 5.86 2.95 0.019 0.86 1 1 2 5410.37 6790.05 2.94 0.652 3.99 5 4 -12 43.40 66.76 2.93 0.065 0.92 1 1 1 5252.18 6571.85 2.87 0.641 4.11 3 1 -14 122.34 91.04 2.87 0.075 1.64 0 3 -31 78.45 43.62 2.86 0.052 0.80 1 1 3 1940.37 2391.57 2.80 0.387 3.82 2 1 -35 130.69 92.30 2.79 0.076 0.81 1 1 18 35.21 50.76 2.77 0.056 1.50 4 2 7 31.28 19.19 2.75 0.035 1.56 1 2 -32 54.56 38.15 2.74 0.049 0.84 2 2 8 40.34 27.59 2.74 0.042 1.80 2 0 -15 68.93 92.51 2.74 0.076 1.81 3 1 16 12.91 25.16 2.71 0.040 1.51 6 2 -25 114.61 87.25 2.71 0.074 0.88 3 5 -10 -3.73 9.38 2.70 0.024 0.84 2 0 -22 -0.63 4.91 2.70 0.018 1.28 1 3 -28 -10.44 8.54 2.68 0.023 0.85 6 1 -29 17.98 5.10 2.68 0.018 0.84 1 1 5 164.67 202.86 2.66 0.113 3.38 1 5 -14 14.82 36.90 2.65 0.048 0.83 9 4 -9 124.69 93.62 2.64 0.077 0.77 1 1 -2 5586.59 6788.23 2.63 0.651 3.99 3 5 7 26.00 55.00 2.63 0.059 0.86 9 3 14 -0.34 21.98 2.62 0.037 0.82 8 1 -23 5.91 36.30 2.62 0.048 0.87 2 2 -3 361.31 298.44 2.61 0.137 2.03 2 2 3 361.08 298.44 2.58 0.137 2.03 7 1 -20 70.92 94.04 2.58 0.077 1.00 6 1 -4 29.69 20.62 2.55 0.036 1.53 11 1 -5 18.29 31.63 2.54 0.044 0.88 2 2 -25 188.91 153.85 2.53 0.098 1.01 0 2 2 567.24 470.77 2.52 0.172 2.25 1 3 11 197.34 262.57 2.50 0.128 1.31 1 3 10 170.40 219.53 2.50 0.117 1.33 7 3 -8 11.27 18.87 2.45 0.034 1.00 0 2 -2 565.73 470.68 2.45 0.172 2.25 Bond lengths and angles O2 - Distance Angles C3 1.3731 (0.0032) C14 1.4277 (0.0035) 117.54 (0.24) O2 - C3 O3 - Distance Angles C10 1.3776 (0.0031) C15 1.4216 (0.0036) 117.60 (0.22) O3 - C10 C15 - Distance Angles O3 1.4216 (0.0036) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 - O3 H15A H15B C14 - Distance Angles O2 1.4277 (0.0035) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - O2 H14A H14B C1 - Distance Angles C6 1.3901 (0.0034) C2 1.3916 (0.0037) 120.83 (0.23) N1 1.4267 (0.0037) 120.05 (0.24) 119.11 (0.23) C1 - C6 C2 C2 - Distance Angles C3 1.3911 (0.0038) C1 1.3916 (0.0037) 119.25 (0.24) H2 0.9500 120.38 120.38 C2 - C3 C1 C3 - Distance Angles O2 1.3731 (0.0032) C2 1.3911 (0.0038) 124.46 (0.24) C4 1.3934 (0.0038) 115.25 (0.23) 120.28 (0.26) C3 - O2 C2 C4 - Distance Angles C5 1.3849 (0.0043) C3 1.3934 (0.0038) 119.81 (0.25) H4 0.9500 120.09 120.09 C4 - C5 C3 C5 - Distance Angles C4 1.3849 (0.0043) C6 1.3907 (0.0039) 120.52 (0.25) H5 0.9500 119.74 119.74 C5 - C4 C6 C6 - Distance Angles C1 1.3901 (0.0034) C5 1.3907 (0.0039) 119.25 (0.25) H6 0.9500 120.38 120.38 C6 - C1 C5 C7 - Distance Angles O1 1.2388 (0.0021) N2 1.3613 (0.0038) 122.58 (0.25) N1 1.3634 (0.0038) 121.92 (0.25) 115.49 (0.16) C7 - O1 N2 C8 - Distance Angles C13 1.3863 (0.0032) C9 1.3914 (0.0037) 120.65 (0.22) N2 1.4182 (0.0037) 120.21 (0.24) 119.14 (0.23) C8 - C13 C9 C9 - Distance Angles C8 1.3914 (0.0037) C10 1.3917 (0.0036) 119.09 (0.23) H9 0.9500 120.46 120.46 C9 - C8 C10 C10 - Distance Angles O3 1.3776 (0.0031) C9 1.3917 (0.0036) 124.36 (0.23) C11 1.3943 (0.0036) 114.96 (0.22) 120.67 (0.24) C10 - O3 C9 C11 - Distance Angles C12 1.3779 (0.0043) C10 1.3943 (0.0036) 119.50 (0.24) H11 0.9500 120.25 120.25 C11 - C12 C10 C12 - Distance Angles C11 1.3779 (0.0043) C13 1.3964 (0.0038) 120.57 (0.24) H12 0.9500 119.71 119.71 C12 - C11 C13 C13 - Distance Angles C8 1.3863 (0.0032) C12 1.3964 (0.0038) 119.48 (0.24) H13 0.9500 120.26 120.26 C13 - C8 C12 N1 - Distance Angles C7 1.3634 (0.0038) C1 1.4267 (0.0037) 121.78 (0.18) H1N 0.8477 (0.0168) 116.55 (2.26) 121.42 (2.29) N1 - C7 C1 N2 - Distance Angles C7 1.3613 (0.0037) C8 1.4182 (0.0037) 121.96 (0.18) H2N 0.8399 (0.0168) 120.89 (2.22) 116.73 (2.29) N2 - C7 C8 O1 - Distance Angles C7 1.2388 (0.0021) O1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.848(17) 2.06(2) 2.835(3) 152(3) N1-H1N...O1_$1 0.840(17) 2.11(2) 2.842(2) 146(3) N2-H2N...O1_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)