+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008lsh032 started at 16:50:02 on 08-Jul-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh032 in P2(1)/c CELL 0.71073 13.2432 9.5856 7.4783 90.000 103.345 90.000 ZERR 4.00 0.0003 0.0003 0.0002 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 40 52 4 8 V = 923.69 F(000) = 384.0 Mu = 0.09 mm-1 Cell Wt = 716.86 Rho = 1.289 MERG 2 OMIT -3.00 55.00 OMIT -1 2 1 OMIT -12 0 2 FMAP 2 PLAN 5 EQIV $1 -x, y+1/2, -z-1/2 HTAB N1 O1_$1 HTAB SIZE 0.10 0.10 0.40 ACTA BOND $H L.S. 6 TEMP -153.00 WGHT 0.0295 0.4879 FVAR 1.45898 C1 1 0.153451 0.422349 -0.080800 11.00000 0.01669 0.01672 = 0.01806 -0.00228 0.00271 0.00100 C2 1 0.180010 0.326072 0.060838 11.00000 0.01862 0.02084 = 0.02212 0.00235 0.00570 -0.00197 AFIX 43 H2 2 0.128175 0.267014 0.088946 11.00000 -1.20000 AFIX 0 C3 1 0.282383 0.315377 0.162349 11.00000 0.02126 0.02168 = 0.02057 0.00524 0.00448 0.00075 AFIX 43 H3 2 0.300001 0.249476 0.259444 11.00000 -1.20000 AFIX 0 C4 1 0.358411 0.401214 0.121171 11.00000 0.01617 0.02003 = 0.01936 -0.00112 0.00215 0.00029 C5 1 0.332470 0.496530 -0.022463 11.00000 0.01944 0.01825 = 0.02359 0.00207 0.00432 -0.00359 AFIX 43 H5 2 0.384587 0.554039 -0.052536 11.00000 -1.20000 AFIX 0 C6 1 0.230721 0.507491 -0.121450 11.00000 0.02172 0.01690 = 0.02053 0.00306 0.00316 -0.00035 AFIX 43 H6 2 0.213235 0.573708 -0.218185 11.00000 -1.20000 AFIX 0 C7 1 -0.025718 0.345335 -0.223197 11.00000 0.02009 0.02039 = 0.01940 -0.00377 0.00599 -0.00032 C8 1 -0.127518 0.395346 -0.340571 11.00000 0.01932 0.02708 = 0.02757 -0.00412 0.00117 -0.00031 AFIX 137 H8A 2 -0.149589 0.332590 -0.445802 11.00000 -1.50000 H8B 2 -0.118999 0.489898 -0.384722 11.00000 -1.50000 H8C 2 -0.180158 0.396067 -0.267508 11.00000 -1.50000 AFIX 0 C9 1 0.490987 0.314230 0.372471 11.00000 0.02104 0.02421 = 0.02180 0.00392 0.00127 0.00179 AFIX 23 H9A 2 0.483905 0.214327 0.338297 11.00000 -1.20000 H9B 2 0.446299 0.334046 0.458852 11.00000 -1.20000 AFIX 0 C10 1 0.602880 0.348602 0.460378 11.00000 0.02368 0.02540 = 0.02684 0.00088 -0.00194 -0.00004 AFIX 137 H10A 2 0.647564 0.314161 0.382224 11.00000 -1.50000 H10B 2 0.622726 0.304001 0.581341 11.00000 -1.50000 H10C 2 0.610864 0.449918 0.474536 11.00000 -1.50000 AFIX 0 N1 3 0.050449 0.442064 -0.186097 11.00000 0.01726 0.01697 = 0.02203 0.00093 0.00216 0.00095 O1 4 -0.014388 0.224386 -0.165663 11.00000 0.02598 0.01879 = 0.02950 -0.00027 0.00290 -0.00363 O2 4 0.461492 0.400073 0.211966 11.00000 0.01648 0.02748 = 0.02384 0.00688 0.00145 -0.00163 H1N 2 0.036216 0.527900 -0.237951 11.00000 0.03342 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 2008lsh032 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C6 N1 C2 - C1 C3 C3 - C4 C2 C4 - O2 C3 C5 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - O2 C10 C10 - C9 N1 - C7 C1 O1 - C7 O2 - C4 C9 Operators for generating equivalent atoms: $1 -x, y+1/2, -z-1/2 h k l Fo^2 Sigma Why rejected -7 0 7 33.81 7.78 observed but should be systematically absent 10123 Reflections read, of which 374 rejected -17 =< h =< 16, -12 =< k =< 12, -9 =< l =< 9, Max. 2-theta = 54.97 1 Systematic absence violations 0 Inconsistent equivalents 2106 Unique reflections, of which 0 suppressed R(int) = 0.0259 R(sigma) = 0.0251 Friedel opposites merged Maximum memory for data reduction = 1483 / 20979 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 = 1835 / 157721 wR2 = 0.0939 before cycle 1 for 2106 data and 124 / 124 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0295 * P )^2 + 0.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45922 0.00307 0.078 OSF Mean shift/esd = 0.021 Maximum = -0.090 for x C4 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 1835 / 157721 wR2 = 0.0940 before cycle 2 for 2106 data and 124 / 124 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0295 * P )^2 + 0.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45922 0.00307 0.001 OSF Mean shift/esd = 0.007 Maximum = -0.031 for x C4 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 1835 / 157721 wR2 = 0.0940 before cycle 3 for 2106 data and 124 / 124 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0295 * P )^2 + 0.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45923 0.00307 0.002 OSF Mean shift/esd = 0.000 Maximum = 0.002 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1835 / 157721 wR2 = 0.0939 before cycle 4 for 2106 data and 124 / 124 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0295 * P )^2 + 0.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45923 0.00307 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U22 C1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 1835 / 157721 wR2 = 0.0939 before cycle 5 for 2106 data and 124 / 124 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0295 * P )^2 + 0.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45923 0.00307 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C10 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 1835 / 157721 wR2 = 0.0939 before cycle 6 for 2106 data and 124 / 124 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0295 * P )^2 + 0.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45923 0.00307 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C6 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 0.1282 0.2670 0.0889 43 0.950 0.000 C2 C1 C3 H3 0.3000 0.2495 0.2594 43 0.950 0.000 C3 C4 C2 H5 0.3846 0.5540 -0.0525 43 0.950 0.000 C5 C6 C4 H6 0.2132 0.5737 -0.2182 43 0.950 0.000 C6 C5 C1 H8A -0.1496 0.3326 -0.4458 137 0.980 0.000 C8 C7 H8A H8B -0.1190 0.4899 -0.3848 137 0.980 0.000 C8 C7 H8A H8C -0.1802 0.3961 -0.2675 137 0.980 0.000 C8 C7 H8A H9A 0.4839 0.2143 0.3383 23 0.990 0.000 C9 O2 C10 H9B 0.4463 0.3341 0.4588 23 0.990 0.000 C9 O2 C10 H10A 0.6476 0.3142 0.3822 137 0.980 0.000 C10 C9 H10A H10B 0.6227 0.3040 0.5813 137 0.980 0.000 C10 C9 H10A H10C 0.6109 0.4499 0.4745 137 0.980 0.000 C10 C9 H10A 2008lsh032 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.15346 0.42235 -0.08079 1.00000 0.01667 0.01671 0.01806 -0.00229 0.00271 0.00100 0.01735 0.00206 0.00008 0.00012 0.00015 0.00000 0.00052 0.00052 0.00052 0.00042 0.00042 0.00042 0.00024 C2 0.18001 0.32608 0.06084 1.00000 0.01866 0.02083 0.02211 0.00234 0.00573 -0.00199 0.02037 0.00222 0.00009 0.00012 0.00016 0.00000 0.00055 0.00056 0.00057 0.00045 0.00045 0.00043 0.00025 H2 0.12818 0.26702 0.08895 1.00000 0.02444 0.00000 0.00000 C3 0.28239 0.31539 0.16234 1.00000 0.02128 0.02165 0.02055 0.00523 0.00448 0.00076 0.02122 0.00229 0.00009 0.00013 0.00016 0.00000 0.00057 0.00058 0.00056 0.00045 0.00045 0.00045 0.00026 H3 0.30001 0.24949 0.25944 1.00000 0.02546 0.00000 0.00000 C4 0.35840 0.40121 0.12116 1.00000 0.01617 0.02001 0.01936 -0.00113 0.00216 0.00030 0.01883 0.00212 0.00009 0.00012 0.00016 0.00000 0.00052 0.00056 0.00054 0.00043 0.00042 0.00042 0.00025 C5 0.33246 0.49652 -0.02246 1.00000 0.01944 0.01824 0.02359 0.00207 0.00432 -0.00361 0.02053 0.00220 0.00009 0.00012 0.00016 0.00000 0.00054 0.00055 0.00059 0.00044 0.00046 0.00043 0.00025 H5 0.38458 0.55403 -0.05254 1.00000 0.02463 0.00000 0.00000 C6 0.23072 0.50748 -0.12145 1.00000 0.02177 0.01689 0.02050 0.00307 0.00317 -0.00035 0.02000 0.00219 0.00009 0.00012 0.00016 0.00000 0.00057 0.00053 0.00056 0.00043 0.00045 0.00044 0.00025 H6 0.21323 0.57370 -0.21818 1.00000 0.02400 0.00000 0.00000 C7 -0.02571 0.34534 -0.22319 1.00000 0.02012 0.02041 0.01941 -0.00379 0.00603 -0.00033 0.01974 0.00217 0.00009 0.00012 0.00016 0.00000 0.00055 0.00056 0.00055 0.00044 0.00044 0.00044 0.00025 C8 -0.12752 0.39534 -0.34057 1.00000 0.01933 0.02710 0.02756 -0.00415 0.00119 -0.00033 0.02535 0.00230 0.00009 0.00014 0.00018 0.00000 0.00056 0.00064 0.00063 0.00050 0.00047 0.00048 0.00028 H8A -0.14959 0.33257 -0.44578 1.00000 0.03803 0.00000 0.00000 H8B -0.11900 0.48988 -0.38475 1.00000 0.03803 0.00000 0.00000 H8C -0.18015 0.39608 -0.26750 1.00000 0.03803 0.00000 0.00000 C9 0.49098 0.31424 0.37247 1.00000 0.02105 0.02422 0.02179 0.00394 0.00128 0.00179 0.02295 0.00232 0.00009 0.00013 0.00017 0.00000 0.00057 0.00060 0.00057 0.00047 0.00046 0.00046 0.00026 H9A 0.48390 0.21433 0.33829 1.00000 0.02754 0.00000 0.00000 H9B 0.44630 0.33405 0.45885 1.00000 0.02754 0.00000 0.00000 C10 0.60289 0.34861 0.46037 1.00000 0.02371 0.02539 0.02684 0.00089 -0.00192 -0.00004 0.02657 0.00234 0.00010 0.00014 0.00018 0.00000 0.00061 0.00063 0.00062 0.00050 0.00049 0.00049 0.00028 H10A 0.64757 0.31416 0.38222 1.00000 0.03986 0.00000 0.00000 H10B 0.62273 0.30401 0.58134 1.00000 0.03986 0.00000 0.00000 H10C 0.61087 0.44992 0.47452 1.00000 0.03986 0.00000 0.00000 N1 0.05045 0.44206 -0.18609 1.00000 0.01727 0.01694 0.02204 0.00093 0.00216 0.00095 0.01913 0.00185 0.00007 0.00011 0.00014 0.00000 0.00047 0.00048 0.00049 0.00038 0.00038 0.00037 0.00022 O1 -0.01439 0.22438 -0.16566 1.00000 0.02600 0.01879 0.02950 -0.00027 0.00292 -0.00364 0.02533 0.00161 0.00007 0.00009 0.00012 0.00000 0.00046 0.00043 0.00048 0.00035 0.00037 0.00034 0.00022 O2 0.46149 0.40008 0.21197 1.00000 0.01649 0.02748 0.02383 0.00688 0.00145 -0.00163 0.02312 0.00159 0.00006 0.00009 0.00012 0.00000 0.00040 0.00046 0.00044 0.00035 0.00033 0.00033 0.00021 H1N 0.03623 0.52785 -0.23795 1.00000 0.03326 0.02957 0.00117 0.00181 0.00216 0.00000 0.00417 Final Structure Factor Calculation for 2008lsh032 in P2(1)/c Total number of l.s. parameters = 124 Maximum vector length = 511 Memory required = 1711 / 22995 wR2 = 0.0939 before cycle 7 for 2106 data and 0 / 124 parameters GooF = S = 1.058; Restrained GooF = 1.058 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0295 * P )^2 + 0.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0396 for 1910 Fo > 4sig(Fo) and 0.0443 for all 2106 data wR2 = 0.0939, GooF = S = 1.058, Restrained GooF = 1.058 for all data Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0210 0.0162 0.0149 C1 0.0241 0.0209 0.0160 C2 0.0264 0.0214 0.0158 C3 0.0218 0.0191 0.0156 C4 0.0257 0.0213 0.0146 C5 0.0244 0.0205 0.0151 C6 0.0238 0.0199 0.0155 C7 0.0332 0.0248 0.0180 C8 0.0278 0.0244 0.0167 C9 0.0356 0.0254 0.0188 C10 0.0238 0.0179 0.0157 N1 0.0330 0.0257 0.0172 O1 0.0344 0.0191 0.0159 O2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.031 0.047 0.064 0.086 0.110 0.141 0.187 0.272 1.000 Number in group 212. 213. 220. 203. 204. 214. 209. 209. 210. 212. GooF 1.201 1.062 1.065 1.024 0.972 0.978 1.100 1.120 1.043 0.989 K 2.281 1.095 1.007 0.997 0.981 1.002 1.008 1.006 1.003 1.006 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.65 inf Number in group 215. 218. 200. 212. 209. 211. 209. 210. 213. 209. GooF 1.070 1.184 0.999 0.931 0.845 1.008 0.970 0.871 1.194 1.380 K 1.039 1.052 1.036 1.012 0.993 0.995 0.990 0.997 1.009 1.006 R1 0.091 0.096 0.066 0.061 0.043 0.045 0.035 0.025 0.035 0.028 Recommended weighting scheme: WGHT 0.0289 0.4918 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 3 13.04 0.38 6.28 0.009 1.59 0 3 3 25.78 10.43 4.75 0.049 1.93 1 2 0 16.42 7.04 3.99 0.040 4.49 10 1 3 152.05 198.92 3.91 0.215 1.04 1 4 2 68.38 47.48 3.71 0.105 1.94 -3 4 2 25.38 14.08 3.60 0.057 1.91 12 1 1 47.86 68.77 3.43 0.126 1.02 -5 9 6 0.68 8.53 3.38 0.044 0.80 -5 4 1 137.84 108.39 3.30 0.158 1.77 1 2 1 279.41 333.43 3.30 0.278 3.69 -9 9 5 14.06 5.96 3.08 0.037 0.79 12 5 3 136.28 103.83 3.06 0.155 0.82 5 0 2 97.22 75.49 3.05 0.132 1.91 11 1 2 112.77 141.69 3.01 0.181 1.04 6 0 2 41.05 57.11 2.91 0.115 1.69 10 0 2 355.73 414.95 2.88 0.310 1.13 -1 7 7 5.83 1.67 2.87 0.020 0.84 -7 2 3 68.76 51.90 2.82 0.110 1.57 5 10 4 4.40 0.37 2.77 0.009 0.78 -10 10 1 63.39 86.03 2.73 0.141 0.78 -10 5 6 73.55 55.11 2.71 0.113 0.89 15 3 1 64.79 43.79 2.71 0.101 0.80 2 0 0 1926.74 2164.88 2.69 0.708 6.44 1 8 5 13.92 23.09 2.69 0.073 0.91 14 1 2 35.34 23.54 2.68 0.074 0.84 -3 6 3 110.55 84.21 2.68 0.140 1.32 11 3 2 6.95 13.47 2.65 0.056 0.99 -9 8 1 48.85 35.52 2.62 0.091 0.93 8 0 2 81.72 101.71 2.57 0.154 1.36 5 3 2 561.36 500.48 2.57 0.341 1.64 1 7 6 18.36 28.03 2.56 0.081 0.89 -8 0 2 54.15 70.39 2.56 0.128 1.62 -11 8 3 120.89 97.36 2.56 0.150 0.84 -4 11 1 4.32 0.30 2.52 0.008 0.84 12 8 0 -0.93 1.48 2.52 0.018 0.80 16 1 0 206.51 169.33 2.50 0.198 0.80 0 5 2 326.55 286.50 2.49 0.258 1.70 2 10 4 31.12 21.11 2.49 0.070 0.83 -5 2 4 84.28 103.72 2.48 0.155 1.59 4 5 1 71.06 88.95 2.47 0.144 1.57 -3 6 6 4.08 1.09 2.44 0.016 0.98 2 6 5 5.72 2.24 2.43 0.023 1.03 -3 1 5 12.31 6.97 2.42 0.040 1.47 2 6 4 6.00 2.51 2.41 0.024 1.15 1 2 3 187.48 161.10 2.41 0.193 2.07 14 0 2 84.58 64.40 2.41 0.122 0.85 -2 5 2 113.16 94.01 2.39 0.148 1.69 -2 7 3 2.50 0.46 2.38 0.010 1.20 3 6 6 5.33 1.92 2.38 0.021 0.91 -1 1 1 110.86 132.41 2.38 0.175 5.69 Bond lengths and angles C1 - Distance Angles C2 1.3875 (0.0016) C6 1.3960 (0.0016) 119.06 (0.10) N1 1.4216 (0.0014) 123.57 (0.10) 117.36 (0.10) C1 - C2 C6 C2 - Distance Angles C1 1.3875 (0.0016) C3 1.3963 (0.0016) 120.47 (0.11) H2 0.9500 119.77 119.77 C2 - C1 C3 C3 - Distance Angles C4 1.3886 (0.0016) C2 1.3963 (0.0016) 119.91 (0.11) H3 0.9500 120.05 120.05 C3 - C4 C2 C4 - Distance Angles O2 1.3774 (0.0013) C3 1.3886 (0.0016) 124.94 (0.10) C5 1.3914 (0.0016) 115.20 (0.10) 119.85 (0.11) C4 - O2 C3 C5 - Distance Angles C6 1.3835 (0.0016) C4 1.3914 (0.0016) 119.95 (0.11) H5 0.9500 120.02 120.02 C5 - C6 C4 C6 - Distance Angles C5 1.3835 (0.0016) C1 1.3960 (0.0016) 120.75 (0.11) H6 0.9500 119.62 119.62 C6 - C5 C1 C7 - Distance Angles O1 1.2337 (0.0015) N1 1.3508 (0.0015) 123.26 (0.11) C8 1.5072 (0.0016) 121.49 (0.11) 115.24 (0.10) C7 - O1 N1 C8 - Distance Angles C7 1.5072 (0.0016) 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 O2 1.4331 (0.0014) C10 1.5123 (0.0016) 106.81 (0.10) H9A 0.9900 110.36 110.36 H9B 0.9900 110.36 110.36 108.59 C9 - O2 C10 H9A C10 - Distance Angles C9 1.5123 (0.0016) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C9 H10A H10B N1 - Distance Angles C7 1.3508 (0.0015) C1 1.4216 (0.0014) 126.74 (0.10) H1N 0.9102 (0.0171) 117.48 (0.97) 115.71 (0.97) N1 - C7 C1 O1 - Distance Angles C7 1.2337 (0.0015) O1 - O2 - Distance Angles C4 1.3774 (0.0013) C9 1.4331 (0.0014) 117.71 (0.09) O2 - C4 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.910(17) 2.014(17) 2.9217(13) 175.0(14) 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)