+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 23:05:37 on 13-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh041 in P2(1)/n CELL 0.71073 7.0527 12.7252 9.6648 90.000 111.315 90.000 ZERR 4.00 0.0003 0.0006 0.0004 0.000 0.003 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 36 32 8 4 V = 808.05 F(000) = 336.0 Mu = 0.09 mm-1 Cell Wt = 640.70 Rho = 1.317 MERG 2 OMIT -3.00 55.00 OMIT -2 1 1 OMIT 1 3 0 OMIT -2 1 2 OMIT 1 4 0 OMIT 3 4 0 OMIT 2 0 0 OMIT 2 5 2 OMIT -3 2 8 OMIT -1 1 1 OMIT -1 3 2 DFIX 0.88 0.02 N1 H1N FMAP 2 PLAN 5 ACTA EQIV $1 x+1/2, -y+1/2, z+1/2 HTAB N1 O1_$1 HTAB SIZE 0.6 0.1 0.1 BOND $H L.S. 6 TEMP -153.00 WGHT 0.012000 0.790500 FVAR 1.75935 C1 1 0.214555 0.422258 0.479857 11.00000 0.01324 0.01559 = 0.01893 0.00005 0.00584 0.00093 C2 1 0.123251 0.456468 0.333746 11.00000 0.01664 0.01703 = 0.01770 0.00031 0.00414 0.00032 AFIX 43 H2 2 0.054680 0.408398 0.256539 11.00000 -1.20000 AFIX 0 C3 1 0.134727 0.563289 0.303114 11.00000 0.01775 0.01836 = 0.02175 0.00236 0.00793 0.00143 C4 1 0.240095 0.635067 0.412725 11.00000 0.02250 0.01634 = 0.02986 -0.00102 0.01313 -0.00037 AFIX 43 H4 2 0.248473 0.706983 0.389187 11.00000 -1.20000 AFIX 0 C5 1 0.332392 0.599064 0.556908 11.00000 0.02305 0.02081 = 0.02529 -0.00685 0.00922 -0.00423 AFIX 43 H5 2 0.405953 0.646683 0.633255 11.00000 -1.20000 AFIX 0 C6 1 0.318567 0.494280 0.590991 11.00000 0.01855 0.02255 = 0.01790 -0.00274 0.00649 -0.00119 AFIX 43 H6 2 0.380326 0.471072 0.690831 11.00000 -1.20000 AFIX 0 C7 1 0.093188 0.236973 0.444478 11.00000 0.01712 0.01828 = 0.01808 0.00009 0.00376 0.00030 C8 1 0.103478 0.136570 0.528418 11.00000 0.02271 0.01823 = 0.02385 0.00363 0.00497 -0.00240 AFIX 137 H8A 2 -0.030792 0.120987 0.531904 11.00000 -1.50000 H8B 2 0.202705 0.144139 0.629786 11.00000 -1.50000 H8C 2 0.145241 0.079032 0.478369 11.00000 -1.50000 AFIX 0 C9 1 0.029482 0.599370 0.152683 11.00000 0.02371 0.01543 = 0.02671 0.00169 0.00899 0.00186 N1 3 0.208547 0.317107 0.524242 11.00000 0.01960 0.01662 = 0.01343 0.00150 0.00132 -0.00035 N2 3 -0.058038 0.628334 0.033575 11.00000 0.03648 0.02433 = 0.03047 0.00687 0.00914 0.00608 O1 4 -0.016983 0.245218 0.312695 11.00000 0.03492 0.02162 = 0.01687 -0.00034 -0.00214 -0.00447 H1N 2 0.286469 0.304151 0.618649 11.00000 0.03476 HKLF 4 Covalent radii and connectivity table for 2008lsh041 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C6 N1 C2 - C1 C3 C3 - C4 C2 C9 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - N2 C3 N1 - C7 C1 N2 - C9 O1 - C7 Operators for generating equivalent atoms: $1 x+1/2, -y+1/2, z+1/2 h k l Fo^2 Sigma Why rejected -4 0 1 28.11 5.27 observed but should be systematically absent -3 0 2 81.06 8.28 observed but should be systematically absent -1 0 2 92.57 8.74 observed but should be systematically absent -1 0 2 90.12 12.03 observed but should be systematically absent -1 0 2 85.00 14.47 observed but should be systematically absent -1 0 4 80.04 14.64 observed but should be systematically absent -1 0 4 99.27 17.57 observed but should be systematically absent -1 0 4 91.60 13.65 observed but should be systematically absent -1 0 4 97.18 10.42 observed but should be systematically absent 1 0 4 241.07 57.28 observed but should be systematically absent 1 0 4 307.84 59.91 observed but should be systematically absent 1 0 4 263.26 23.86 observed but should be systematically absent 3 0 4 46.06 8.45 observed but should be systematically absent 3 0 4 38.93 9.26 observed but should be systematically absent -3 0 6 16.95 2.55 observed but should be systematically absent -3 0 6 21.52 4.62 observed but should be systematically absent -3 0 6 30.11 6.38 observed but should be systematically absent -5 0 8 39.04 9.66 observed but should be systematically absent -3 0 8 49.16 12.27 observed but should be systematically absent 8093 Reflections read, of which 245 rejected -9 =< h =< 8, -16 =< k =< 16, -11 =< l =< 12, Max. 2-theta = 55.00 19 Systematic absence violations 0 Inconsistent equivalents 1773 Unique reflections, of which 0 suppressed R(int) = 0.0374 R(sigma) = 0.0351 Friedel opposites merged Maximum memory for data reduction = 1265 / 17936 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 = 1541 / 146286 wR2 = 0.1137 before cycle 1 for 1773 data and 114 / 114 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.180; Restrained GooF = 1.179 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0120 * P )^2 + 0.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.75936 0.00463 0.001 OSF Mean shift/esd = 0.002 Maximum = 0.006 for U13 N1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for C4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1541 / 146286 wR2 = 0.1137 before cycle 2 for 1773 data and 114 / 114 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.179; Restrained GooF = 1.179 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0120 * P )^2 + 0.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.75936 0.00463 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.002 for U13 N1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 1541 / 146286 wR2 = 0.1137 before cycle 3 for 1773 data and 114 / 114 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.180; Restrained GooF = 1.179 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0120 * P )^2 + 0.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.75935 0.00463 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for N2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1541 / 146286 wR2 = 0.1137 before cycle 4 for 1773 data and 114 / 114 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.180; Restrained GooF = 1.179 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0120 * P )^2 + 0.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.75935 0.00463 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for N2 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1541 / 146286 wR2 = 0.1137 before cycle 5 for 1773 data and 114 / 114 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.180; Restrained GooF = 1.179 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0120 * P )^2 + 0.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.75935 0.00463 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 1541 / 146286 wR2 = 0.1137 before cycle 6 for 1773 data and 114 / 114 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.180; Restrained GooF = 1.179 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0120 * P )^2 + 0.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.75935 0.00463 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C5 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N 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 0.0547 0.4084 0.2565 43 0.950 0.000 C2 C1 C3 H4 0.2485 0.7070 0.3892 43 0.950 0.000 C4 C5 C3 H5 0.4060 0.6467 0.6333 43 0.950 0.000 C5 C4 C6 H6 0.3803 0.4711 0.6908 43 0.950 0.000 C6 C5 C1 H8A -0.0308 0.1210 0.5319 137 0.980 0.000 C8 C7 H8A H8B 0.2027 0.1441 0.6298 137 0.980 0.000 C8 C7 H8A H8C 0.1452 0.0790 0.4784 137 0.980 0.000 C8 C7 H8A 2008lsh041 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.21455 0.42226 0.47986 1.00000 0.01324 0.01559 0.01893 0.00005 0.00584 0.00093 0.01592 0.00339 0.00025 0.00013 0.00019 0.00000 0.00076 0.00082 0.00082 0.00066 0.00066 0.00062 0.00036 C2 0.12325 0.45647 0.33375 1.00000 0.01664 0.01703 0.01770 0.00031 0.00414 0.00032 0.01771 0.00351 0.00026 0.00014 0.00019 0.00000 0.00080 0.00085 0.00082 0.00067 0.00067 0.00066 0.00037 H2 0.05468 0.40840 0.25654 1.00000 0.02125 0.00000 0.00000 C3 0.13473 0.56329 0.30311 1.00000 0.01775 0.01836 0.02175 0.00236 0.00793 0.00143 0.01908 0.00364 0.00027 0.00014 0.00020 0.00000 0.00084 0.00087 0.00088 0.00069 0.00072 0.00067 0.00039 C4 0.24009 0.63507 0.41272 1.00000 0.02250 0.01634 0.02986 -0.00102 0.01313 -0.00037 0.02189 0.00379 0.00028 0.00015 0.00021 0.00000 0.00089 0.00086 0.00098 0.00074 0.00078 0.00070 0.00040 H4 0.24847 0.70698 0.38919 1.00000 0.02627 0.00000 0.00000 C5 0.33239 0.59906 0.55691 1.00000 0.02305 0.02081 0.02529 -0.00685 0.00922 -0.00423 0.02293 0.00373 0.00028 0.00015 0.00021 0.00000 0.00091 0.00090 0.00094 0.00075 0.00077 0.00073 0.00041 H5 0.40595 0.64668 0.63325 1.00000 0.02752 0.00000 0.00000 C6 0.31857 0.49428 0.59099 1.00000 0.01855 0.02255 0.01790 -0.00274 0.00649 -0.00119 0.01970 0.00352 0.00027 0.00014 0.00020 0.00000 0.00085 0.00091 0.00083 0.00070 0.00071 0.00070 0.00039 H6 0.38033 0.47107 0.69083 1.00000 0.02365 0.00000 0.00000 C7 0.09319 0.23697 0.44448 1.00000 0.01712 0.01828 0.01808 0.00009 0.00376 0.00030 0.01856 0.00345 0.00026 0.00014 0.00019 0.00000 0.00080 0.00086 0.00082 0.00069 0.00068 0.00067 0.00037 C8 0.10348 0.13657 0.52842 1.00000 0.02271 0.01823 0.02385 0.00363 0.00497 -0.00240 0.02257 0.00374 0.00029 0.00014 0.00021 0.00000 0.00090 0.00090 0.00091 0.00074 0.00074 0.00072 0.00041 H8A -0.03079 0.12099 0.53190 1.00000 0.03386 0.00000 0.00000 H8B 0.20270 0.14414 0.62979 1.00000 0.03386 0.00000 0.00000 H8C 0.14524 0.07903 0.47837 1.00000 0.03386 0.00000 0.00000 C9 0.02948 0.59937 0.15268 1.00000 0.02371 0.01543 0.02671 0.00169 0.00899 0.00186 0.02200 0.00381 0.00028 0.00014 0.00021 0.00000 0.00091 0.00085 0.00096 0.00074 0.00078 0.00070 0.00040 N1 0.20855 0.31711 0.52424 1.00000 0.01960 0.01662 0.01343 0.00150 0.00132 -0.00035 0.01786 0.00294 0.00023 0.00012 0.00016 0.00000 0.00074 0.00074 0.00068 0.00057 0.00060 0.00058 0.00034 N2 -0.05804 0.62833 0.03357 1.00000 0.03648 0.02433 0.03047 0.00687 0.00914 0.00608 0.03127 0.00368 0.00028 0.00014 0.00019 0.00000 0.00098 0.00087 0.00093 0.00074 0.00078 0.00075 0.00042 O1 -0.01698 0.24522 0.31270 1.00000 0.03492 0.02162 0.01687 -0.00034 -0.00214 -0.00447 0.02770 0.00254 0.00021 0.00010 0.00014 0.00000 0.00077 0.00069 0.00064 0.00053 0.00056 0.00059 0.00035 H1N 0.28647 0.30415 0.61865 1.00000 0.03476 0.04117 0.00329 0.00184 0.00187 0.00000 0.00632 Final Structure Factor Calculation for 2008lsh041 in P2(1)/n Total number of l.s. parameters = 114 Maximum vector length = 511 Memory required = 1427 / 22995 wR2 = 0.1137 before cycle 7 for 1773 data and 0 / 114 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.180; Restrained GooF = 1.179 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0120 * P )^2 + 0.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0498 for 1535 Fo > 4sig(Fo) and 0.0594 for all 1773 data wR2 = 0.1137, GooF = S = 1.180, Restrained GooF = 1.179 for all data Occupancy sum of asymmetric unit = 12.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0192 0.0159 0.0127 C1 0.0205 0.0171 0.0155 C2 0.0230 0.0177 0.0166 C3 0.0305 0.0189 0.0163 C4 0.0304 0.0228 0.0155 C5 0.0238 0.0187 0.0166 C6 0.0218 0.0183 0.0156 C7 0.0311 0.0207 0.0159 C8 0.0271 0.0240 0.0149 C9 0.0250 0.0167 0.0119 N1 0.0400 0.0349 0.0189 N2 0.0479 0.0213 0.0139 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.035 0.054 0.073 0.096 0.124 0.156 0.207 0.279 1.000 Number in group 178. 177. 185. 169. 184. 172. 177. 178. 175. 178. GooF 1.714 1.187 1.110 1.077 1.229 1.118 1.131 0.871 0.929 1.220 K 5.470 1.344 1.179 1.049 1.069 1.020 1.011 1.000 1.006 0.991 Resolution(A) 0.77 0.80 0.84 0.88 0.92 0.98 1.05 1.15 1.32 1.64 inf Number in group 184. 174. 177. 177. 174. 177. 178. 178. 177. 177. GooF 0.932 0.886 0.968 0.852 0.928 1.080 1.163 1.270 1.478 1.849 K 1.029 0.997 0.992 0.998 0.991 1.005 1.002 1.011 1.024 0.994 R1 0.136 0.094 0.093 0.071 0.061 0.054 0.046 0.045 0.048 0.038 Recommended weighting scheme: WGHT 0.0065 0.8184 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) -1 6 1 67.62 22.40 6.18 0.080 2.02 -4 1 1 128.06 65.24 5.92 0.137 1.71 3 1 3 20.76 0.30 5.45 0.009 1.51 -2 3 8 12.71 0.94 4.80 0.016 1.16 1 11 1 13.72 0.09 4.63 0.005 1.12 -1 6 2 64.41 33.26 4.43 0.098 1.92 3 2 0 117.70 68.86 4.33 0.141 2.07 3 3 0 10.38 0.60 4.31 0.013 1.95 2 6 4 10.34 0.45 4.19 0.011 1.28 -3 6 1 59.96 31.37 4.14 0.095 1.57 -1 2 1 1555.30 1782.77 4.09 0.718 4.57 -6 0 2 29.41 10.76 3.96 0.056 1.17 -4 8 6 10.47 1.03 3.95 0.017 1.05 -1 3 1 3107.25 3459.55 3.74 1.000 3.56 4 6 1 7.47 0.02 3.69 0.003 1.24 -2 9 3 8.37 0.17 3.66 0.007 1.26 -3 6 3 7.71 0.72 3.62 0.014 1.52 1 0 1 931.10 1109.25 3.62 0.566 4.57 3 4 2 8.47 0.83 3.56 0.015 1.52 -3 4 4 73.16 45.81 3.54 0.115 1.67 2 0 2 6.28 0.00 3.42 0.001 2.29 -5 2 9 12.49 3.15 3.40 0.030 0.98 -2 8 8 6.50 0.17 3.36 0.007 0.96 2 6 2 41.75 22.32 3.35 0.080 1.56 -2 3 3 209.94 161.61 3.34 0.216 2.32 -2 10 5 14.89 4.37 3.31 0.036 1.06 3 12 0 7.70 0.50 3.28 0.012 0.95 1 6 3 5.99 0.35 3.10 0.010 1.59 -3 10 3 5.63 0.06 3.08 0.004 1.10 -6 0 8 5.75 0.23 2.98 0.008 0.98 4 1 0 41.89 24.21 2.93 0.084 1.63 -3 3 2 24.22 11.97 2.89 0.059 2.04 0 5 4 57.32 37.30 2.87 0.104 1.69 -4 3 5 20.19 8.78 2.87 0.050 1.43 2 7 0 78.16 53.82 2.86 0.125 1.59 -2 5 2 7.97 1.03 2.84 0.017 2.01 -1 1 2 870.72 978.96 2.83 0.532 4.30 -5 0 5 19.62 38.47 2.82 0.105 1.31 -1 7 2 64.59 43.25 2.82 0.112 1.69 1 2 5 115.84 87.41 2.74 0.159 1.55 1 9 4 5.30 0.06 2.71 0.004 1.14 -3 9 3 46.55 29.24 2.71 0.092 1.19 4 9 1 10.67 3.14 2.70 0.030 1.04 -5 1 11 -2.65 5.11 2.66 0.038 0.84 0 2 2 136.97 172.17 2.64 0.223 3.67 -5 1 9 40.34 24.03 2.60 0.083 0.98 -2 8 3 27.70 15.57 2.58 0.067 1.38 -1 5 8 14.82 5.36 2.57 0.039 1.07 -1 1 5 85.22 62.17 2.57 0.134 1.90 -5 8 4 13.11 5.31 2.54 0.039 1.04 Bond lengths and angles C1 - Distance Angles C2 1.3918 (0.0024) C6 1.3996 (0.0024) 119.60 (0.16) N1 1.4105 (0.0022) 123.46 (0.15) 116.94 (0.15) C1 - C2 C6 C2 - Distance Angles C1 1.3918 (0.0024) C3 1.3998 (0.0025) 118.51 (0.16) H2 0.9500 120.74 120.74 C2 - C1 C3 C3 - Distance Angles C4 1.3916 (0.0026) C2 1.3998 (0.0025) 122.16 (0.17) C9 1.4460 (0.0025) 119.60 (0.17) 118.23 (0.16) C3 - C4 C2 C4 - Distance Angles C5 1.3842 (0.0027) C3 1.3916 (0.0026) 118.34 (0.17) H4 0.9500 120.83 120.83 C4 - C5 C3 C5 - Distance Angles C4 1.3842 (0.0027) C6 1.3854 (0.0027) 120.66 (0.17) H5 0.9500 119.67 119.67 C5 - C4 C6 C6 - Distance Angles C5 1.3854 (0.0027) C1 1.3996 (0.0024) 120.69 (0.17) H6 0.9500 119.66 119.66 C6 - C5 C1 C7 - Distance Angles O1 1.2319 (0.0021) N1 1.3565 (0.0022) 123.10 (0.16) C8 1.5010 (0.0024) 121.31 (0.16) 115.57 (0.15) C7 - O1 N1 C8 - Distance Angles C7 1.5010 (0.0024) 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 C9 - Distance Angles N2 1.1513 (0.0025) C3 1.4460 (0.0025) 178.54 (0.21) C9 - N2 N1 - Distance Angles C7 1.3565 (0.0022) C1 1.4105 (0.0022) 128.20 (0.15) H1N 0.8929 (0.0159) 117.46 (1.54) 114.24 (1.55) N1 - C7 C1 N2 - Distance Angles C9 1.1513 (0.0025) N2 - O1 - Distance Angles C7 1.2319 (0.0021) O1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.893(16) 1.986(17) 2.8679(19) 169(2) N1-H1N...O1_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)