+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 12:03:00 on 23-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh092 in P-1 CELL 0.68890 3.8210 9.7260 22.6700 92.151 93.359 100.409 ZERR 4.00 0.0050 0.0140 0.0300 0.016 0.018 0.016 LATT 1 SFAC C H N O UNIT 32 32 8 12 V = 826.20 F(000) = 376.0 Mu = 0.11 mm-1 Cell Wt = 720.66 Rho = 1.448 MERG 2 OMIT -3.00 50.00 OMIT -1 3 4 OMIT 0 4 5 OMIT 1 1 4 OMIT 0 -3 -4 OMIT 0 3 4 OMIT -1 -3 -4 OMIT -2 -3 -4 OMIT -3 -3 -4 OMIT -3 4 4 FMAP 2 PLAN 5 ACTA BOND $H EQIV $1 x, y-1, z HTAB N1 O11 HTAB N11 O1_$1 HTAB SIZE 0.1 0.02 0.02 LIST 6 L.S. 26 TEMP -153.00 WGHT 0.0401 12.2011 EXTI 0.048257 BASF 0.22982 FVAR 0.31668 MOLE 1 C1 1 -0.423039 0.708048 -0.343382 11.00000 0.02754 0.02734 = 0.03317 -0.00288 -0.01019 0.00615 C2 1 -0.443461 0.838223 -0.369866 11.00000 0.02641 0.03871 = 0.03747 0.00462 -0.00156 0.00187 AFIX 43 H2 2 -0.507461 0.912789 -0.347117 11.00000 -1.20000 AFIX 0 C3 1 -0.371119 0.855282 -0.427722 11.00000 0.04241 0.03138 = 0.04062 0.00594 -0.00583 0.00129 AFIX 43 H3 2 -0.392647 0.940540 -0.445493 11.00000 -1.20000 AFIX 0 C4 1 -0.264603 0.746608 -0.461090 11.00000 0.02193 0.03685 = 0.03662 -0.00291 -0.00448 0.00386 C5 1 -0.243158 0.618042 -0.436071 11.00000 0.02399 0.02463 = 0.06317 -0.00964 -0.00951 0.01645 AFIX 43 H5 2 -0.176026 0.544390 -0.458969 11.00000 -1.20000 AFIX 0 C6 1 -0.320903 0.600078 -0.377766 11.00000 0.03670 0.01953 = 0.03809 0.00006 -0.00666 -0.00071 AFIX 43 H6 2 -0.305227 0.513587 -0.360612 11.00000 -1.20000 AFIX 0 C7 1 -0.603304 0.767075 -0.241657 11.00000 0.01867 0.03419 = 0.05002 -0.00780 -0.01530 0.01200 C8 1 -0.676826 0.699274 -0.182418 11.00000 0.04906 0.04389 = 0.03911 -0.00468 0.00360 0.00890 AFIX 137 H8A 2 -0.467539 0.727141 -0.154601 11.00000 -1.50000 H8B 2 -0.726635 0.597189 -0.188735 11.00000 -1.50000 H8C 2 -0.883197 0.730251 -0.166137 11.00000 -1.50000 AFIX 0 N1 3 -0.503280 0.681856 -0.284857 11.00000 0.03715 0.02876 = 0.03802 0.00307 -0.00057 0.00401 AFIX 43 H1 2 -0.487005 0.597184 -0.274012 11.00000 -1.20000 AFIX 0 N2 3 -0.173020 0.768704 -0.523471 11.00000 0.03506 0.02345 = 0.05274 -0.00076 -0.01209 0.00956 O1 4 -0.623109 0.891431 -0.249894 11.00000 0.03480 0.03622 = 0.04505 -0.00854 -0.00686 0.00371 O2 4 -0.235123 0.874805 -0.546774 11.00000 0.05673 0.02856 = 0.04465 0.00368 -0.00474 0.01171 O3 4 -0.044738 0.674776 -0.549019 11.00000 0.05953 0.04282 = 0.03881 -0.00705 -0.00167 0.02531 MOLE 2 C11 1 -0.156897 0.208081 -0.159825 11.00000 0.03185 0.03359 = 0.03252 -0.00508 0.00177 0.00375 C12 1 -0.115199 0.339197 -0.128407 11.00000 0.02750 0.03460 = 0.04363 -0.00175 0.00289 0.00400 AFIX 43 H12 2 -0.194547 0.416174 -0.146039 11.00000 -1.20000 AFIX 0 C13 1 0.046644 0.353336 -0.070346 11.00000 0.03428 0.02803 = 0.02669 -0.00300 0.00562 -0.00179 AFIX 43 H13 2 0.082462 0.440459 -0.048412 11.00000 -1.20000 AFIX 0 C14 1 0.151804 0.237876 -0.046102 11.00000 0.03533 0.02633 = 0.03321 0.00339 -0.00377 -0.00681 C15 1 0.107230 0.110850 -0.076386 11.00000 0.03199 0.02761 = 0.03888 0.00253 -0.00223 0.00313 AFIX 43 H15 2 0.183178 0.033510 -0.058495 11.00000 -1.20000 AFIX 0 C16 1 -0.048558 0.096598 -0.132922 11.00000 0.03982 0.02772 = 0.03489 0.00005 -0.00654 -0.00405 AFIX 43 H16 2 -0.082370 0.008301 -0.153905 11.00000 -1.20000 AFIX 0 C17 1 -0.421073 0.279217 -0.255623 11.00000 0.02184 0.03242 = 0.03228 -0.00705 -0.00650 0.00088 C18 1 -0.613334 0.215102 -0.314695 11.00000 0.04437 0.03219 = 0.03492 -0.00607 -0.01126 0.00695 AFIX 137 H18A 2 -0.801710 0.266943 -0.326296 11.00000 -1.50000 H18B 2 -0.718916 0.116877 -0.309967 11.00000 -1.50000 H18C 2 -0.441548 0.220745 -0.345358 11.00000 -1.50000 AFIX 0 N11 3 -0.337448 0.187384 -0.217627 11.00000 0.04448 0.02931 = 0.03191 -0.00196 -0.00636 0.00634 AFIX 43 H11 2 -0.404058 0.099184 -0.230036 11.00000 -1.20000 AFIX 0 N12 3 0.316695 0.255394 0.015689 11.00000 0.03770 0.05110 = 0.03267 -0.00341 -0.00885 -0.00595 O11 4 -0.352680 0.410650 -0.245557 11.00000 0.05458 0.02827 = 0.04753 -0.00323 -0.01068 0.01650 O12 4 0.309776 0.364337 0.044564 11.00000 0.06874 0.04402 = 0.04575 -0.01729 -0.01777 0.01836 O13 4 0.443787 0.158706 0.035552 11.00000 0.05276 0.03824 = 0.03835 0.00192 -0.01104 0.00884 HKLF 5 Covalent radii and connectivity table for 2008lsh092 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - N1 C6 C2 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 N2 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 N1 - C7 C1 N2 - O2 O3 C4 O1 - C7 O2 - N2 O3 - N2 C11 - C16 C12 N11 C12 - C13 C11 C13 - C14 C12 C14 - C15 C13 N12 C15 - C14 C16 C16 - C15 C11 C17 - O11 N11 C18 C18 - C17 N11 - C17 C11 N12 - O13 O12 C14 O11 - C17 O12 - N12 O13 - N12 Operators for generating equivalent atoms: $1 x, y-1, z ** MERG code changed to 0 for compatibility with HKLF and BASF parameters ** 6001 Reflections read, of which 17 rejected -4 =< h =< 4, -11 =< k =< 11, -25 =< l =< 26, Max. 2-theta = 48.41 0 Systematic absence violations 0 Data suppressed, R(sigma) = 0.1047 Maximum memory for data reduction = 2231 / 159 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 = 2851 / 296411 wR2 = 0.3797 before cycle 1 for 5990 data and 239 / 239 parameters GooF = S = 1.131; Restrained GooF = 1.131 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31710 0.00219 0.193 OSF 2 0.23144 0.00499 0.324 BASF 1 3 0.04993 0.00996 0.168 EXTI Mean shift/esd = 0.044 Maximum = 0.324 for BASF 1 Max. shift = 0.010 A for H18B Max. dU = 0.000 for C14 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3796 before cycle 2 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31731 0.00220 0.095 OSF 2 0.23190 0.00499 0.093 BASF 1 3 0.05090 0.01008 0.096 EXTI Mean shift/esd = 0.021 Maximum = 0.096 for EXTI Max. shift = 0.002 A for H18B Max. dU = 0.000 for C14 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 3 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31734 0.00220 0.014 OSF 2 0.23189 0.00499 -0.004 BASF 1 3 0.05113 0.01015 0.022 EXTI Mean shift/esd = 0.006 Maximum = -0.023 for tors H8A Max. shift = 0.001 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 4 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31735 0.00220 0.004 OSF 2 0.23185 0.00499 -0.006 BASF 1 3 0.05118 0.01016 0.005 EXTI Mean shift/esd = 0.003 Maximum = -0.020 for tors H8A Max. shift = 0.001 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 5 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.002 OSF 2 0.23185 0.00499 -0.002 BASF 1 3 0.05120 0.01017 0.002 EXTI Mean shift/esd = 0.002 Maximum = -0.017 for tors H8A Max. shift = 0.001 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 6 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23184 0.00499 -0.001 BASF 1 3 0.05120 0.01017 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.014 for tors H8A Max. shift = 0.001 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 7 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.001 OSF 2 0.23184 0.00499 -0.001 BASF 1 3 0.05120 0.01017 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.012 for tors H8A Max. shift = 0.001 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 8 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.001 OSF 2 0.23184 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.009 for tors H8A Max. shift = 0.001 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 9 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.008 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 10 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.001 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.006 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 11 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 11 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.005 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 12 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 12 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.004 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 13 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 13 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.003 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 14 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 14 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.003 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 15 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 15 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 16 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 16 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 17 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 17 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 18 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 18 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for O1 Least-squares cycle 19 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 19 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 20 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 20 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 21 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 21 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for C4 Least-squares cycle 22 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 22 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C8 Least-squares cycle 23 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 23 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for C8 Least-squares cycle 24 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 24 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for O3 Least-squares cycle 25 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 25 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for O1 Least-squares cycle 26 Maximum vector length = 511 Memory required = 2851 / 296411 wR2 = 0.3795 before cycle 26 for 5990 data and 239 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31736 0.00220 0.000 OSF 2 0.23183 0.00499 0.000 BASF 1 3 0.05121 0.01017 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for O13 Largest correlation matrix elements 0.660 EXTI / OSF Idealized hydrogen atom generation before cycle 27 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -0.5078 0.9128 -0.3471 43 0.950 0.000 C2 C3 C1 H3 -0.3921 0.9405 -0.4455 43 0.950 0.000 C3 C2 C4 H5 -0.1750 0.5444 -0.4590 43 0.950 0.000 C5 C6 C4 H6 -0.3055 0.5135 -0.3606 43 0.950 0.000 C6 C5 C1 H8A -0.4663 0.7262 -0.1548 137 0.980 0.000 C8 C7 H8A H8B -0.7293 0.5972 -0.1888 137 0.980 0.000 C8 C7 H8A H8C -0.8812 0.7311 -0.1659 137 0.980 0.000 C8 C7 H8A H1 -0.4873 0.5971 -0.2740 43 0.880 0.000 N1 C7 C1 H12 -0.1940 0.4161 -0.1461 43 0.950 0.000 C12 C13 C11 H13 0.0820 0.4405 -0.0484 43 0.950 0.000 C13 C14 C12 H15 0.1822 0.0335 -0.0585 43 0.950 0.000 C15 C14 C16 H16 -0.0824 0.0083 -0.1539 43 0.950 0.000 C16 C15 C11 H18A -0.8001 0.2677 -0.3265 137 0.980 0.000 C18 C17 H18A H18B -0.7216 0.1172 -0.3098 137 0.980 0.000 C18 C17 H18A H18C -0.4414 0.2197 -0.3453 137 0.980 0.000 C18 C17 H18A H11 -0.4043 0.0992 -0.2300 43 0.880 0.000 N11 C17 C11 2008lsh092 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.42289 0.70804 -0.34340 1.00000 0.02762 0.02762 0.03305 -0.00291 -0.01013 0.00568 0.02995 0.01283 0.00206 0.00072 0.00031 0.00000 0.00479 0.00370 0.00397 0.00290 0.00325 0.00328 0.00179 C2 -0.44357 0.83828 -0.36984 1.00000 0.02643 0.03900 0.03755 0.00481 -0.00157 0.00177 0.03492 0.01441 0.00214 0.00081 0.00033 0.00000 0.00480 0.00421 0.00438 0.00332 0.00343 0.00353 0.00188 H2 -0.50779 0.91281 -0.34711 1.00000 0.04191 0.00000 0.00000 C3 -0.37096 0.85524 -0.42772 1.00000 0.04277 0.03162 0.04068 0.00613 -0.00619 0.00082 0.03935 0.01444 0.00229 0.00080 0.00034 0.00000 0.00577 0.00408 0.00459 0.00334 0.00386 0.00376 0.00209 H3 -0.39207 0.94054 -0.44549 1.00000 0.04722 0.00000 0.00000 C4 -0.26503 0.74670 -0.46106 1.00000 0.02221 0.03690 0.03674 -0.00285 -0.00459 0.00392 0.03252 0.01350 0.00205 0.00078 0.00032 0.00000 0.00476 0.00416 0.00421 0.00317 0.00333 0.00344 0.00183 C5 -0.24276 0.61796 -0.43608 1.00000 0.02353 0.02478 0.06363 -0.00965 -0.00952 0.01660 0.03659 0.01403 0.00211 0.00075 0.00036 0.00000 0.00475 0.00369 0.00547 0.00341 0.00381 0.00331 0.00203 H5 -0.17499 0.54442 -0.45896 1.00000 0.04391 0.00000 0.00000 C6 -0.32087 0.60003 -0.37777 1.00000 0.03730 0.01956 0.03812 0.00021 -0.00696 -0.00097 0.03284 0.01309 0.00215 0.00071 0.00033 0.00000 0.00520 0.00339 0.00431 0.00290 0.00351 0.00324 0.00189 H6 -0.30551 0.51352 -0.36061 1.00000 0.03941 0.00000 0.00000 C7 -0.60295 0.76702 -0.24167 1.00000 0.01863 0.03444 0.05000 -0.00790 -0.01532 0.01200 0.03442 0.01338 0.00204 0.00078 0.00034 0.00000 0.00457 0.00419 0.00471 0.00334 0.00358 0.00339 0.00193 C8 -0.67658 0.69923 -0.18244 1.00000 0.04991 0.04413 0.03874 -0.00464 0.00340 0.00829 0.04446 0.01632 0.00257 0.00087 0.00034 0.00000 0.00617 0.00468 0.00461 0.00355 0.00400 0.00427 0.00219 H8A -0.46627 0.72617 -0.15477 1.00000 0.06669 0.00000 0.00000 H8B -0.72927 0.59717 -0.18884 1.00000 0.06669 0.00000 0.00000 H8C -0.88117 0.73110 -0.16594 1.00000 0.06669 0.00000 0.00000 N1 -0.50330 0.68184 -0.28484 1.00000 0.03782 0.02906 0.03772 0.00317 -0.00071 0.00356 0.03528 0.01155 0.00178 0.00064 0.00027 0.00000 0.00445 0.00325 0.00364 0.00265 0.00300 0.00298 0.00164 H1 -0.48733 0.59713 -0.27401 1.00000 0.04233 0.00000 0.00000 N2 -0.17267 0.76869 -0.52348 1.00000 0.03578 0.02315 0.05292 -0.00091 -0.01241 0.00970 0.03743 0.01153 0.00181 0.00061 0.00029 0.00000 0.00451 0.00316 0.00418 0.00282 0.00329 0.00295 0.00172 O1 -0.62340 0.89150 -0.24989 1.00000 0.03462 0.03627 0.04529 -0.00851 -0.00680 0.00387 0.03970 0.00964 0.00151 0.00054 0.00023 0.00000 0.00366 0.00310 0.00323 0.00234 0.00253 0.00255 0.00145 O2 -0.23548 0.87486 -0.54675 1.00000 0.05657 0.02863 0.04500 0.00364 -0.00452 0.01189 0.04316 0.01054 0.00168 0.00054 0.00023 0.00000 0.00424 0.00278 0.00327 0.00229 0.00279 0.00272 0.00154 O3 -0.04510 0.67484 -0.54901 1.00000 0.06023 0.04274 0.03891 -0.00692 -0.00196 0.02498 0.04579 0.01096 0.00172 0.00059 0.00023 0.00000 0.00442 0.00324 0.00317 0.00249 0.00279 0.00303 0.00159 C11 -0.15698 0.20809 -0.15983 1.00000 0.03273 0.03360 0.03228 -0.00485 0.00145 0.00335 0.03340 0.01386 0.00221 0.00075 0.00032 0.00000 0.00510 0.00394 0.00403 0.00314 0.00334 0.00349 0.00184 C12 -0.11494 0.33910 -0.12840 1.00000 0.02682 0.03465 0.04396 -0.00179 0.00335 0.00473 0.03531 0.01449 0.00217 0.00081 0.00034 0.00000 0.00495 0.00411 0.00451 0.00331 0.00357 0.00352 0.00190 H12 -0.19403 0.41610 -0.14606 1.00000 0.04237 0.00000 0.00000 C13 0.04656 0.35338 -0.07036 1.00000 0.03372 0.02829 0.02690 -0.00311 0.00586 -0.00118 0.03045 0.01364 0.00213 0.00074 0.00030 0.00000 0.00500 0.00366 0.00370 0.00284 0.00327 0.00334 0.00178 H13 0.08198 0.44049 -0.04843 1.00000 0.03654 0.00000 0.00000 C14 0.15220 0.23780 -0.04610 1.00000 0.03647 0.02630 0.03309 0.00363 -0.00408 -0.00748 0.03381 0.01352 0.00223 0.00075 0.00031 0.00000 0.00510 0.00370 0.00399 0.00296 0.00345 0.00337 0.00188 C15 0.10684 0.11094 -0.07637 1.00000 0.03132 0.02748 0.03931 0.00243 -0.00204 0.00381 0.03306 0.01363 0.00212 0.00075 0.00032 0.00000 0.00506 0.00378 0.00432 0.00314 0.00354 0.00341 0.00187 H15 0.18219 0.03351 -0.05845 1.00000 0.03967 0.00000 0.00000 C16 -0.04868 0.09662 -0.13291 1.00000 0.03902 0.02785 0.03502 -0.00021 -0.00600 -0.00350 0.03555 0.01382 0.00220 0.00078 0.00032 0.00000 0.00541 0.00378 0.00420 0.00305 0.00360 0.00352 0.00198 H16 -0.08235 0.00832 -0.15388 1.00000 0.04266 0.00000 0.00000 C17 -0.42100 0.27921 -0.25563 1.00000 0.02144 0.03255 0.03235 -0.00725 -0.00615 0.00118 0.02979 0.01291 0.00202 0.00074 0.00031 0.00000 0.00461 0.00394 0.00393 0.00295 0.00312 0.00323 0.00175 C18 -0.61358 0.21511 -0.31469 1.00000 0.04395 0.03254 0.03487 -0.00605 -0.01118 0.00709 0.03786 0.01362 0.00231 0.00078 0.00032 0.00000 0.00561 0.00409 0.00421 0.00314 0.00368 0.00378 0.00204 H18A -0.80007 0.26767 -0.32650 1.00000 0.05679 0.00000 0.00000 H18B -0.72163 0.11721 -0.30982 1.00000 0.05679 0.00000 0.00000 H18C -0.44142 0.21971 -0.34526 1.00000 0.05679 0.00000 0.00000 N11 -0.33755 0.18738 -0.21762 1.00000 0.04525 0.02949 0.03187 -0.00187 -0.00648 0.00586 0.03611 0.01160 0.00182 0.00063 0.00026 0.00000 0.00472 0.00333 0.00342 0.00258 0.00300 0.00310 0.00170 H11 -0.40434 0.09917 -0.23001 1.00000 0.04333 0.00000 0.00000 N12 0.31677 0.25533 0.01567 1.00000 0.03810 0.05110 0.03274 -0.00316 -0.00903 -0.00633 0.04305 0.01220 0.00198 0.00076 0.00028 0.00000 0.00472 0.00438 0.00368 0.00317 0.00310 0.00355 0.00184 O11 -0.35246 0.41060 -0.24556 1.00000 0.05545 0.02838 0.04759 -0.00305 -0.01105 0.01627 0.04344 0.01030 0.00164 0.00052 0.00024 0.00000 0.00422 0.00282 0.00333 0.00233 0.00282 0.00275 0.00157 O12 0.30982 0.36434 0.04457 1.00000 0.06780 0.04407 0.04610 -0.01732 -0.01763 0.01918 0.05290 0.01077 0.00180 0.00060 0.00025 0.00000 0.00485 0.00345 0.00349 0.00272 0.00310 0.00326 0.00180 O13 0.44367 0.15874 0.03556 1.00000 0.05288 0.03837 0.03836 0.00183 -0.01084 0.00893 0.04369 0.01019 0.00165 0.00056 0.00023 0.00000 0.00419 0.00316 0.00308 0.00241 0.00275 0.00289 0.00154 Final Structure Factor Calculation for 2008lsh092 in P-1 Total number of l.s. parameters = 239 Maximum vector length = 511 Memory required = 2612 / 22995 wR2 = 0.3795 before cycle 27 for 5990 data and 0 / 239 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0401 * P )^2 + 12.20 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1566 for 4248 Fo > 4sig(Fo) and 0.1847 for all 5990 data wR2 = 0.3795, GooF = S = 1.129, Restrained GooF = 1.129 for all data Occupancy sum of asymmetric unit = 26.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0441 0.0272 0.0186 C1 0.0444 0.0351 0.0253 C2 0.0553 0.0333 0.0295 C3 0.0422 0.0353 0.0200 C4 0.0721 0.0284 0.0092 C5 0.0490 0.0313 0.0182 C6 0.0630 0.0301 0.0102 C7 0.0504 0.0487 0.0343 C8 0.0424 0.0349 0.0286 N1 0.0632 0.0288 0.0203 N2 0.0546 0.0386 0.0259 O1 0.0611 0.0422 0.0261 O2 0.0702 0.0398 0.0274 O3 0.0405 0.0332 0.0265 C11 0.0456 0.0337 0.0267 C12 0.0424 0.0257 0.0233 C13 0.0515 0.0307 0.0192 C14 0.0419 0.0301 0.0272 C15 0.0503 0.0341 0.0222 C16 0.0419 0.0314 0.0160 C17 0.0553 0.0348 0.0235 C18 0.0505 0.0317 0.0261 N11 0.0640 0.0437 0.0214 N12 0.0688 0.0376 0.0239 O11 0.0880 0.0446 0.0261 O12 0.0624 0.0384 0.0303 O13 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.023 0.033 0.044 0.057 0.072 0.089 0.117 0.175 1.000 Number in group 626. 620. 591. 567. 613. 595. 593. 585. 598. 602. GooF 1.281 1.278 1.141 1.263 1.105 1.039 0.941 1.036 0.891 1.222 K 21.532 4.322 2.324 1.915 1.519 1.287 1.146 1.097 0.988 1.005 Resolution(A) 0.84 0.88 0.92 0.97 1.03 1.10 1.20 1.32 1.52 1.87 inf Number in group 621. 601. 595. 579. 599. 597. 600. 597. 601. 600. GooF 0.729 0.791 0.951 1.113 1.311 1.094 0.969 1.351 1.363 1.387 K 1.080 1.143 1.081 1.153 1.156 1.068 1.127 1.103 1.055 1.039 R1 0.316 0.316 0.270 0.249 0.223 0.157 0.184 0.194 0.128 0.108 Recommended weighting scheme: WGHT 0.0359 12.1451 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 -4 -4 171.22 1339.04 9.19 0.379 1.57 -2 -1 5 468.95 53.15 6.66 0.075 1.70 -1 7 -1 302.74 3.45 6.45 0.019 1.37 1 -7 1 287.85 3.45 6.37 0.019 1.37 -2 -1 5 461.80 53.15 6.11 0.075 1.70 0 5 17 257.40 14.40 5.82 0.039 1.07 -1 9 1 277.47 17.49 5.66 0.043 1.07 1 -9 -1 267.94 17.49 5.61 0.043 1.07 3 -7 -1 203.74 3.20 5.49 0.019 1.02 0 5 17 241.51 14.40 5.48 0.039 1.07 -3 7 1 204.34 3.20 5.33 0.019 1.02 1 -7 -1 232.12 22.36 5.16 0.049 1.36 -1 -4 -5 126.70 537.88 5.13 0.240 1.68 1 -9 2 206.76 15.81 5.01 0.041 1.07 3 -7 4 163.53 3.31 4.91 0.019 1.00 -3 3 0 155.39 2.98 4.78 0.018 1.24 -1 9 -4 153.00 2.17 4.77 0.015 1.06 -1 -2 -1 566.77 186.16 4.77 0.141 2.67 -2 8 -4 163.54 6.22 4.77 0.026 1.08 -3 7 -4 161.54 3.31 4.76 0.019 1.00 -1 1 1 128.57 0.00 4.75 0.001 3.71 1 -9 1 455.91 125.66 4.75 0.116 1.07 -3 7 6 177.44 7.67 4.72 0.029 0.99 -1 7 1 208.68 22.36 4.67 0.049 1.36 0 -3 19 381.31 100.67 4.60 0.104 1.13 2 -9 0 130.46 0.06 4.60 0.003 1.01 0 -5 -17 200.89 14.40 4.60 0.039 1.07 1 -9 4 140.49 2.17 4.58 0.015 1.06 1 -7 2 175.78 15.35 4.56 0.041 1.36 -1 9 -2 181.73 15.81 4.48 0.041 1.07 1 -7 3 302.08 69.37 4.46 0.086 1.35 -2 4 -4 123.91 1.68 4.41 0.013 1.55 -1 0 -14 243.34 43.28 4.40 0.068 1.45 0 3 -19 367.29 100.67 4.37 0.104 1.13 -2 9 0 125.30 0.06 4.36 0.003 1.01 1 -1 4 116.86 1.34 4.35 0.012 3.05 -1 1 -4 119.15 1.34 4.34 0.012 3.05 -1 7 -2 167.84 15.35 4.34 0.041 1.36 1 0 14 237.48 43.28 4.34 0.068 1.45 -3 1 -11 210.87 32.29 4.30 0.059 1.05 3 -1 11 206.50 32.29 4.27 0.059 1.05 1 -7 2 163.76 15.35 4.21 0.041 1.36 1 2 -8 103.36 0.70 4.20 0.009 2.04 -1 7 -3 287.97 69.37 4.18 0.086 1.35 1 -9 3 168.53 17.35 4.18 0.043 1.07 2 -4 -1 101.87 0.72 4.13 0.009 1.63 -2 1 -5 174.74 25.79 4.12 0.053 1.72 2 -8 4 127.79 6.22 4.10 0.026 1.08 0 -10 4 120.44 3.79 4.10 0.020 0.95 1 -2 18 101.67 0.00 4.09 0.000 1.16 Bond lengths and angles C1 - Distance Angles N1 1.4023 (0.0095) C6 1.4087 (0.0104) 117.95 (0.64) C2 1.4345 (0.0102) 123.18 (0.66) 118.86 (0.70) C1 - N1 C6 C2 - Distance Angles C3 1.3668 (0.0106) C1 1.4345 (0.0102) 120.06 (0.75) H2 0.9500 119.97 119.97 C2 - C3 C1 C3 - Distance Angles C2 1.3668 (0.0106) C4 1.4071 (0.0111) 120.18 (0.73) H3 0.9500 119.91 119.91 C3 - C2 C4 C4 - Distance Angles C5 1.4079 (0.0103) C3 1.4071 (0.0111) 120.76 (0.73) N2 1.4922 (0.0100) 119.63 (0.66) 119.61 (0.66) C4 - C5 C3 C5 - Distance Angles C6 1.3826 (0.0109) C4 1.4079 (0.0103) 119.08 (0.68) H5 0.9500 120.46 120.46 C5 - C6 C4 C6 - Distance Angles C5 1.3826 (0.0109) C1 1.4087 (0.0104) 121.03 (0.66) H6 0.9500 119.48 119.48 C6 - C5 C1 C7 - Distance Angles O1 1.2474 (0.0089) N1 1.3734 (0.0099) 121.96 (0.76) C8 1.5363 (0.0113) 122.76 (0.73) 115.26 (0.66) C7 - O1 N1 C8 - Distance Angles C7 1.5363 (0.0113) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C7 H8A H8B N1 - Distance Angles C7 1.3734 (0.0098) C1 1.4023 (0.0095) 130.43 (0.65) H1 0.8800 114.78 114.78 N1 - C7 C1 N2 - Distance Angles O2 1.2319 (0.0076) O3 1.2489 (0.0082) 124.59 (0.69) C4 1.4922 (0.0100) 118.46 (0.62) 116.91 (0.60) N2 - O2 O3 O1 - Distance Angles C7 1.2474 (0.0089) O1 - O2 - Distance Angles N2 1.2319 (0.0076) O2 - O3 - Distance Angles N2 1.2489 (0.0082) O3 - C11 - Distance Angles C16 1.3789 (0.0102) C12 1.4148 (0.0102) 119.72 (0.67) N11 1.4342 (0.0092) 119.67 (0.63) 120.41 (0.67) C11 - C16 C12 C12 - Distance Angles C13 1.4112 (0.0105) C11 1.4148 (0.0102) 118.83 (0.72) H12 0.9500 120.58 120.58 C12 - C13 C11 C13 - Distance Angles C14 1.3833 (0.0102) C12 1.4112 (0.0105) 118.57 (0.67) H13 0.9500 120.71 120.71 C13 - C14 C12 C14 - Distance Angles C15 1.3670 (0.0101) C13 1.3833 (0.0102) 122.38 (0.65) N12 1.4918 (0.0093) 120.21 (0.67) 117.41 (0.65) C14 - C15 C13 C15 - Distance Angles C14 1.3670 (0.0101) C16 1.3722 (0.0099) 119.29 (0.69) H15 0.9500 120.36 120.36 C15 - C14 C16 C16 - Distance Angles C15 1.3722 (0.0099) C11 1.3789 (0.0102) 121.19 (0.69) H16 0.9500 119.40 119.40 C16 - C15 C11 C17 - Distance Angles O11 1.2664 (0.0086) N11 1.3306 (0.0089) 124.05 (0.62) C18 1.5422 (0.0094) 120.66 (0.63) 115.29 (0.62) C17 - O11 N11 C18 - Distance Angles C17 1.5422 (0.0094) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C17 H18A H18B N11 - Distance Angles C17 1.3306 (0.0089) C11 1.4342 (0.0092) 130.79 (0.61) H11 0.8800 114.60 114.60 N11 - C17 C11 N12 - Distance Angles O13 1.2214 (0.0086) O12 1.2305 (0.0087) 123.24 (0.63) C14 1.4918 (0.0093) 118.09 (0.65) 118.64 (0.69) N12 - O13 O12 O11 - Distance Angles C17 1.2664 (0.0086) O11 - O12 - Distance Angles N12 1.2305 (0.0087) O12 - O13 - Distance Angles N12 1.2214 (0.0086) O13 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.09 2.958(9) 169.8 N1-H1...O11 0.88 2.06 2.936(9) 171.0 N11-H11...O1_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)