+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 22:27:34 on 13-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh038 in Pna2(1) CELL 0.71073 10.5129 17.0435 4.0675 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0004 0.0001 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 32 36 4 8 V = 728.80 F(000) = 320.0 Mu = 0.10 mm-1 Cell Wt = 604.65 Rho = 1.378 MERG 2 OMIT -3.00 55.00 DFIX 0.88 0.02 N1 H1N DFIX 0.84 0.02 O2 H2O EQIV $1 -x+2, -y+1, z+1/2 EQIV $2 -x+3/2, y+1/2, z-1/2 HTAB N1 O2_$1 HTAB O2 O1_$2 FMAP 2 PLAN 5 SIZE 0.06 0.14 0.40 ACTA HTAB 2.00000 BOND $H WGHT 0.02380 0.21750 L.S. 6 TEMP -153.00 FVAR 2.11394 C1 1 0.809608 0.404651 0.266886 11.00000 0.01815 0.01657 = 0.01889 0.00146 0.00405 0.00128 C2 1 0.861028 0.480100 0.274794 11.00000 0.01638 0.01776 = 0.01960 0.00085 0.00110 -0.00026 AFIX 43 H2 2 0.939079 0.489137 0.386240 11.00000 -1.20000 AFIX 0 C3 1 0.799558 0.541789 0.122161 11.00000 0.01829 0.01532 = 0.02297 0.00095 0.00457 0.00021 C4 1 0.684361 0.529106 -0.041086 11.00000 0.02038 0.01885 = 0.02318 0.00253 0.00155 0.00349 AFIX 43 H4 2 0.641221 0.571195 -0.146033 11.00000 -1.20000 AFIX 0 C5 1 0.634364 0.453846 -0.046687 11.00000 0.01729 0.02324 = 0.02296 -0.00078 -0.00170 0.00001 AFIX 43 H5 2 0.556062 0.444970 -0.157183 11.00000 -1.20000 AFIX 0 C6 1 0.694996 0.391007 0.103939 11.00000 0.02056 0.01633 = 0.02258 -0.00182 0.00099 -0.00295 AFIX 43 H6 2 0.659196 0.339861 0.096155 11.00000 -1.20000 AFIX 0 C7 1 0.849882 0.271460 0.499075 11.00000 0.01957 0.01606 = 0.02253 0.00133 0.00469 0.00084 C8 1 0.946214 0.227074 0.700642 11.00000 0.02648 0.01729 = 0.02732 0.00385 0.00079 0.00073 AFIX 137 H8A 2 0.902043 0.191866 0.853126 11.00000 -1.50000 H8B 2 0.998383 0.264266 0.825472 11.00000 -1.50000 H8C 2 1.000873 0.196219 0.554435 11.00000 -1.50000 AFIX 0 N1 3 0.881000 0.346579 0.434060 11.00000 0.01732 0.01515 = 0.02172 0.00164 -0.00052 -0.00097 O1 4 0.751533 0.240047 0.397527 11.00000 0.02339 0.01696 = 0.03963 0.00545 -0.00236 -0.00408 O2 4 0.857207 0.613489 0.137313 11.00000 0.02037 0.01369 = 0.04154 0.00496 -0.00160 -0.00001 H1N 2 0.955176 0.361646 0.515944 11.00000 0.02227 H2O 2 0.810689 0.650496 0.054280 11.00000 0.04453 HKLF 4 Covalent radii and connectivity table for 2008lsh038 in Pna2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 C2 N1 C2 - C3 C1 C3 - O2 C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 N1 - C7 C1 O1 - C7 O2 - C3 Operators for generating equivalent atoms: $1 -x+2, -y+1, z+1/2 $2 -x+3/2, y+1/2, z-1/2 Floating origin restraints generated 6471 Reflections read, of which 310 rejected -13 =< h =< 10, -21 =< k =< 22, -5 =< l =< 4, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 1555 Unique reflections, of which 0 suppressed R(int) = 0.0246 R(sigma) = 0.0282 Friedel opposites not merged Maximum memory for data reduction = 1298 / 15537 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 = 1593 / 140606 wR2 = 0.0708 before cycle 1 for 1555 data and 109 / 109 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.061 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0238 * P )^2 + 0.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.11406 0.00404 0.029 OSF Mean shift/esd = 0.012 Maximum = -0.036 for y C3 Max. shift = 0.000 A for H2O Max. dU = 0.000 for H2O Least-squares cycle 2 Maximum vector length = 511 Memory required = 1593 / 140606 wR2 = 0.0708 before cycle 2 for 1555 data and 109 / 109 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.062; Restrained GooF = 1.061 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0238 * P )^2 + 0.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.11406 0.00404 0.000 OSF Mean shift/esd = 0.004 Maximum = -0.013 for y C3 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H2O Least-squares cycle 3 Maximum vector length = 511 Memory required = 1593 / 140606 wR2 = 0.0708 before cycle 3 for 1555 data and 109 / 109 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.060 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0238 * P )^2 + 0.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.11406 0.00404 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.002 for U11 H1N Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1593 / 140606 wR2 = 0.0708 before cycle 4 for 1555 data and 109 / 109 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.060 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0238 * P )^2 + 0.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.11406 0.00404 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y H2O Max. shift = 0.000 A for H2O Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 1593 / 140606 wR2 = 0.0708 before cycle 5 for 1555 data and 109 / 109 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.060 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0238 * P )^2 + 0.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.11406 0.00404 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H2O Max. dU = 0.000 for H2O Least-squares cycle 6 Maximum vector length = 511 Memory required = 1593 / 140606 wR2 = 0.0708 before cycle 6 for 1555 data and 109 / 109 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.060 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0238 * P )^2 + 0.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.11406 0.00404 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H2O 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 0.9391 0.4891 0.3862 43 0.950 0.000 C2 C3 C1 H4 0.6412 0.5712 -0.1460 43 0.950 0.000 C4 C5 C3 H5 0.5561 0.4450 -0.1572 43 0.950 0.000 C5 C4 C6 H6 0.6592 0.3399 0.0962 43 0.950 0.000 C6 C5 C1 H8A 0.9020 0.1919 0.8531 137 0.980 0.000 C8 C7 H8A H8B 0.9984 0.2643 0.8255 137 0.980 0.000 C8 C7 H8A H8C 1.0009 0.1962 0.5544 137 0.980 0.000 C8 C7 H8A 2008lsh038 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.80960 0.40465 0.26688 1.00000 0.01814 0.01659 0.01888 0.00146 0.00405 0.00130 0.01787 0.00234 0.00012 0.00007 0.00037 0.00000 0.00057 0.00054 0.00066 0.00054 0.00056 0.00046 0.00027 C2 0.86103 0.48010 0.27478 1.00000 0.01637 0.01777 0.01960 0.00084 0.00110 -0.00026 0.01791 0.00230 0.00011 0.00007 0.00037 0.00000 0.00057 0.00055 0.00069 0.00052 0.00054 0.00044 0.00027 H2 0.93908 0.48914 0.38621 1.00000 0.02150 0.00000 0.00000 C3 0.79956 0.54179 0.12217 1.00000 0.01829 0.01533 0.02296 0.00096 0.00457 0.00020 0.01886 0.00237 0.00012 0.00007 0.00037 0.00000 0.00058 0.00051 0.00072 0.00056 0.00056 0.00045 0.00028 C4 0.68436 0.52911 -0.04107 1.00000 0.02036 0.01886 0.02316 0.00254 0.00156 0.00351 0.02079 0.00244 0.00012 0.00007 0.00038 0.00000 0.00061 0.00056 0.00075 0.00057 0.00064 0.00046 0.00029 H4 0.64122 0.57120 -0.14602 1.00000 0.02495 0.00000 0.00000 C5 0.63436 0.45385 -0.04668 1.00000 0.01728 0.02327 0.02296 -0.00078 -0.00169 0.00001 0.02117 0.00243 0.00012 0.00007 0.00041 0.00000 0.00057 0.00061 0.00074 0.00061 0.00059 0.00047 0.00029 H5 0.55606 0.44497 -0.15719 1.00000 0.02540 0.00000 0.00000 C6 0.69500 0.39101 0.10394 1.00000 0.02055 0.01633 0.02260 -0.00181 0.00101 -0.00296 0.01982 0.00236 0.00012 0.00007 0.00038 0.00000 0.00060 0.00053 0.00074 0.00057 0.00058 0.00046 0.00028 H6 0.65920 0.33986 0.09616 1.00000 0.02379 0.00000 0.00000 C7 0.84988 0.27146 0.49908 1.00000 0.01958 0.01608 0.02253 0.00132 0.00470 0.00084 0.01940 0.00238 0.00013 0.00007 0.00036 0.00000 0.00062 0.00054 0.00076 0.00050 0.00055 0.00047 0.00029 C8 0.94621 0.22707 0.70064 1.00000 0.02649 0.01728 0.02731 0.00384 0.00079 0.00072 0.02369 0.00255 0.00014 0.00008 0.00039 0.00000 0.00068 0.00055 0.00083 0.00055 0.00057 0.00049 0.00032 H8A 0.90204 0.19186 0.85308 1.00000 0.03554 0.00000 0.00000 H8B 0.99836 0.26427 0.82551 1.00000 0.03554 0.00000 0.00000 H8C 1.00089 0.19623 0.55443 1.00000 0.03554 0.00000 0.00000 N1 0.88100 0.34658 0.43406 1.00000 0.01733 0.01513 0.02173 0.00165 -0.00052 -0.00097 0.01806 0.00213 0.00010 0.00006 0.00036 0.00000 0.00048 0.00046 0.00059 0.00048 0.00048 0.00038 0.00023 O1 0.75153 0.24005 0.39752 1.00000 0.02338 0.01697 0.03962 0.00545 -0.00236 -0.00408 0.02666 0.00186 0.00009 0.00005 0.00034 0.00000 0.00046 0.00041 0.00061 0.00049 0.00045 0.00036 0.00024 O2 0.85721 0.61349 0.13731 1.00000 0.02038 0.01369 0.04154 0.00496 -0.00161 -0.00001 0.02520 0.00177 0.00009 0.00005 0.00031 0.00000 0.00046 0.00040 0.00069 0.00044 0.00046 0.00035 0.00026 H1N 0.95524 0.36165 0.51598 1.00000 0.02227 0.02424 0.00131 0.00085 0.00429 0.00000 0.00418 H2O 0.81065 0.65047 0.05431 1.00000 0.04468 0.03344 0.00170 0.00097 0.00528 0.00000 0.00583 Final Structure Factor Calculation for 2008lsh038 in Pna2(1) Total number of l.s. parameters = 109 Maximum vector length = 511 Memory required = 1486 / 25046 wR2 = 0.0708 before cycle 7 for 1555 data and 2 / 109 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.061 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0238 * P )^2 + 0.22 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0306 for 1497 Fo > 4sig(Fo) and 0.0322 for all 1555 data wR2 = 0.0708, GooF = S = 1.061, Restrained GooF = 1.061 for all data Flack x parameter = 0.1815 with esd 1.1386 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 = 11.00 for non-hydrogen and 9.00 for hydrogen atoms Principal mean square atomic displacements U 0.0232 0.0160 0.0144 C1 0.0202 0.0177 0.0159 C2 0.0258 0.0157 0.0150 C3 0.0260 0.0205 0.0159 C4 0.0241 0.0226 0.0168 C5 0.0242 0.0207 0.0146 C6 0.0262 0.0162 0.0158 C7 0.0290 0.0261 0.0160 C8 0.0222 0.0175 0.0145 N1 0.0414 0.0242 0.0143 O1 0.0425 0.0203 0.0128 O2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.047 0.069 0.087 0.109 0.131 0.161 0.198 0.248 0.359 1.000 Number in group 157. 164. 151. 159. 147. 162. 151. 155. 153. 156. GooF 1.114 1.061 1.035 1.048 1.052 1.037 1.049 0.992 0.934 1.257 K 0.978 0.965 0.996 1.004 0.996 1.002 1.008 1.002 1.010 1.003 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.16 1.32 1.67 inf Number in group 164. 157. 150. 154. 157. 152. 157. 152. 158. 154. GooF 1.155 1.072 1.064 0.880 0.860 0.988 0.969 0.887 1.103 1.485 K 1.048 1.036 1.024 0.985 1.002 0.997 0.993 1.001 1.011 1.003 R1 0.075 0.057 0.057 0.038 0.032 0.028 0.025 0.019 0.024 0.023 Recommended weighting scheme: WGHT 0.0236 0.2174 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 1 0 807.57 930.26 3.90 0.626 5.02 5 2 0 56.11 41.16 3.86 0.132 2.04 8 17 1 27.53 15.28 3.67 0.080 0.78 5 8 0 5.10 10.19 3.49 0.065 1.50 4 3 0 16.10 23.90 3.36 0.100 2.39 2 2 0 490.67 553.33 3.35 0.482 4.47 3 6 0 1104.72 993.48 3.35 0.646 2.21 1 3 0 287.54 325.06 3.14 0.370 5.00 2 10 0 22.60 30.92 3.11 0.114 1.62 1 2 0 525.63 597.46 3.10 0.501 6.62 8 5 4 4.68 1.15 3.10 0.022 0.78 4 17 0 78.75 95.66 3.09 0.201 0.94 12 8 1 49.66 34.99 3.06 0.121 0.79 4 14 0 10.33 6.12 3.03 0.051 1.10 1 8 0 2.40 0.76 2.83 0.018 2.09 3 8 0 1560.37 1428.76 2.83 0.775 1.82 0 12 0 95.53 112.00 2.79 0.217 1.42 5 19 0 2.10 0.10 2.78 0.007 0.83 3 2 0 36.07 45.94 2.76 0.139 3.24 6 2 0 953.91 867.50 2.74 0.604 1.72 10 0 -1 36.20 46.86 2.73 0.140 1.02 7 4 0 -0.39 1.22 2.71 0.023 1.42 4 15 0 175.70 199.28 2.71 0.290 1.04 2 3 0 2179.36 2377.43 2.70 1.000 3.86 5 3 -1 212.41 188.09 2.69 0.281 1.77 1 17 3 115.33 90.14 2.64 0.195 0.80 7 9 3 3.87 7.67 2.57 0.057 0.89 5 3 1 210.74 188.41 2.56 0.282 1.77 8 3 0 83.67 97.01 2.46 0.202 1.28 1 4 0 3.46 6.19 2.44 0.051 3.95 7 17 -1 106.50 91.15 2.43 0.196 0.82 7 2 -2 77.16 89.89 2.41 0.194 1.20 4 2 1 36.65 29.75 2.39 0.112 2.14 6 0 -1 322.18 360.68 2.37 0.389 1.61 6 16 0 68.28 80.84 2.35 0.184 0.91 5 19 1 52.83 42.82 2.32 0.134 0.81 4 2 -1 36.45 29.74 2.31 0.112 2.14 9 10 2 28.97 19.65 2.30 0.091 0.87 11 9 2 59.42 44.66 2.28 0.137 0.79 2 7 -1 678.20 628.65 2.27 0.514 1.94 7 13 -1 23.25 29.48 2.27 0.111 0.96 1 4 -2 396.86 364.64 2.26 0.392 1.81 4 16 0 77.67 89.37 2.25 0.194 0.99 8 3 -4 26.02 34.79 2.25 0.121 0.80 8 15 -1 36.37 28.17 2.24 0.109 0.84 1 10 0 274.70 251.05 2.24 0.325 1.68 8 0 -1 81.18 68.88 2.23 0.170 1.25 2 13 4 29.02 39.43 2.23 0.129 0.79 8 17 -1 23.40 15.26 2.21 0.080 0.78 8 15 0 32.20 40.39 2.20 0.130 0.86 Bond lengths and angles C1 - Distance Angles C6 1.3946 (0.0019) C2 1.3953 (0.0017) 119.96 (0.12) N1 1.4162 (0.0018) 124.72 (0.11) 115.32 (0.12) C1 - C6 C2 C2 - Distance Angles C3 1.3814 (0.0018) C1 1.3953 (0.0017) 120.65 (0.12) H2 0.9500 119.68 119.68 C2 - C3 C1 C3 - Distance Angles O2 1.3655 (0.0015) C2 1.3814 (0.0018) 116.95 (0.12) C4 1.3979 (0.0019) 122.98 (0.12) 120.07 (0.11) C3 - O2 C2 C4 - Distance Angles C5 1.3864 (0.0017) C3 1.3979 (0.0019) 118.64 (0.12) H4 0.9500 120.68 120.68 C4 - C5 C3 C5 - Distance Angles C4 1.3864 (0.0017) C6 1.3888 (0.0019) 122.15 (0.13) H5 0.9500 118.92 118.92 C5 - C4 C6 C6 - Distance Angles C5 1.3888 (0.0019) C1 1.3946 (0.0019) 118.53 (0.11) H6 0.9500 120.73 120.73 C6 - C5 C1 C7 - Distance Angles O1 1.2354 (0.0016) N1 1.3476 (0.0016) 123.32 (0.13) C8 1.5066 (0.0019) 121.80 (0.11) 114.87 (0.12) C7 - O1 N1 C8 - Distance Angles C7 1.5066 (0.0019) 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 1.3476 (0.0016) C1 1.4162 (0.0018) 129.02 (0.12) H1N 0.8866 (0.0131) 114.53 (1.01) 116.39 (1.00) N1 - C7 C1 O1 - Distance Angles C7 1.2354 (0.0017) O1 - O2 - Distance Angles C3 1.3655 (0.0015) H2O 0.8666 (0.0147) 112.50 (1.25) O2 - C3 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.887(13) 2.076(13) 2.9531(15) 169.9(15) N1-H1N...O2_$1 0.867(15) 1.779(15) 2.6288(13) 166.3(18) O2-H2O...O1_$2 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)