+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 17:34:31 on 30-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh121 in I2 CELL 0.71073 6.7095 4.7163 20.0338 90.000 92.902 90.000 ZERR 2.00 0.0003 0.0003 0.0013 0.000 0.004 0.000 LATT -2 SYMM - X, Y, - Z SFAC C H N O UNIT 26 20 8 10 V = 633.14 F(000) = 312.0 Mu = 0.13 mm-1 Cell Wt = 604.50 Rho = 1.585 MERG 2 OMIT -3.00 55.00 DFIX 0.88 0.02 N1 H1N FMAP 2 PLAN 5 SIZE 0.01 0.02 0.44 ACTA EQIV $1 x, y+1, z HTAB N1 O1_$1 HTAB BOND $H L.S. 6 TEMP -153.00 WGHT 0.000000 0.921700 EXTI 0.007345 FVAR 0.76593 C1 1 -0.260984 1.490323 0.596627 11.00000 0.01807 0.01994 = 0.02082 0.00347 -0.00148 -0.00225 C2 1 -0.125812 1.278452 0.583117 11.00000 0.01909 0.01882 = 0.01881 0.00016 -0.00157 0.00188 AFIX 43 H2 2 -0.137362 1.174155 0.542538 11.00000 -1.20000 AFIX 0 C3 1 0.026871 1.223121 0.630590 11.00000 0.01834 0.01991 = 0.02242 0.00267 0.00101 0.00039 C4 1 0.048627 1.362700 0.691130 11.00000 0.02206 0.02335 = 0.02159 0.00248 -0.00393 0.00038 AFIX 43 H4 2 0.154871 1.318282 0.722536 11.00000 -1.20000 AFIX 0 C5 1 -0.090380 1.569985 0.704329 11.00000 0.02558 0.02584 = 0.01919 -0.00133 -0.00104 -0.00021 AFIX 43 H5 2 -0.080734 1.668643 0.745709 11.00000 -1.20000 AFIX 0 C6 1 -0.243431 1.634765 0.657706 11.00000 0.01959 0.02237 = 0.02189 -0.00048 -0.00058 -0.00014 AFIX 43 H6 2 -0.337126 1.778300 0.667284 11.00000 -1.20000 AFIX 0 C7 1 -0.500000 1.422238 0.500000 10.50000 0.01596 0.01650 = 0.02105 0.00000 -0.00011 0.00000 N1 3 -0.407236 1.584016 0.548973 11.00000 0.02148 0.01742 = 0.02114 -0.00022 -0.00666 0.00103 N2 3 0.174899 1.005692 0.614928 11.00000 0.01973 0.02673 = 0.02385 0.00246 -0.00005 0.00444 O1 4 -0.500000 1.164226 0.500000 10.50000 0.02683 0.01762 = 0.02927 0.00000 -0.00925 0.00000 O2 4 0.144862 0.861275 0.564650 11.00000 0.02987 0.02970 = 0.02328 -0.00254 -0.00093 0.00609 O3 4 0.323830 0.982982 0.653250 11.00000 0.02465 0.05216 = 0.03211 -0.00325 -0.00992 0.01453 H1N 2 -0.436338 1.760478 0.548191 11.00000 0.02449 HKLF 4 1 0 0 -1 0 1 0 1 0 1 Covalent radii and connectivity table for 2008lsh121 in I2 C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C6 N1 C2 - C1 C3 C3 - C4 C2 N2 C4 - C3 C5 C5 - C4 C6 C6 - C5 C1 C7 - O1 N1 N1_$2 N1 - C7 C1 N2 - O2 O3 C3 O1 - C7 O2 - N2 O3 - N2 Operators for generating equivalent atoms: $1 x, y+1, z $2 -x-1, y, -z+1 Floating origin restraints generated 3631 Reflections read, of which 2 rejected -8 =< h =< 8, -6 =< k =< 5, -23 =< l =< 25, Max. 2-theta = 54.98 0 Systematic absence violations 0 Inconsistent equivalents 1282 Unique reflections, of which 0 suppressed R(int) = 0.0386 R(sigma) = 0.0478 Friedel opposites not merged Maximum memory for data reduction = 1143 / 15484 Special position constraints for C7 x = -0.5000 z = 0.5000 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O1 x = -0.5000 z = 0.5000 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 1423 / 137210 wR2 = 0.0927 before cycle 1 for 1282 data and 106 / 106 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 0.025 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.125 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.76593 0.00231 0.001 OSF 2 0.00735 0.00182 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.004 for z O2 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 1423 / 137210 wR2 = 0.0927 before cycle 2 for 1282 data and 106 / 106 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 0.025 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.125 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.76593 0.00231 0.000 OSF 2 0.00735 0.00182 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for z O2 Max. shift = 0.000 A for O2 Max. dU = 0.000 for C1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1423 / 137210 wR2 = 0.0927 before cycle 3 for 1282 data and 106 / 106 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 0.025 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.125 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.76593 0.00231 0.000 OSF 2 0.00735 0.00182 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C3 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1423 / 137210 wR2 = 0.0927 before cycle 4 for 1282 data and 106 / 106 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 0.025 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.125 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.76593 0.00231 0.000 OSF 2 0.00735 0.00182 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O2 Max. shift = 0.000 A for H1N Max. dU = 0.000 for O3 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1423 / 137210 wR2 = 0.0927 before cycle 5 for 1282 data and 106 / 106 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 0.025 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.125 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.76593 0.00231 0.000 OSF 2 0.00735 0.00182 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z N2 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C3 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1423 / 137210 wR2 = 0.0927 before cycle 6 for 1282 data and 106 / 106 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 0.025 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.125 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.76593 0.00231 0.000 OSF 2 0.00735 0.00182 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O2 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C2 Largest correlation matrix elements 0.558 EXTI / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -0.1374 1.1742 0.5425 43 0.950 0.000 C2 C1 C3 H4 0.1549 1.3183 0.7225 43 0.950 0.000 C4 C3 C5 H5 -0.0807 1.6686 0.7457 43 0.950 0.000 C5 C4 C6 H6 -0.3371 1.7783 0.6673 43 0.950 0.000 C6 C5 C1 2008lsh121 in I2 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.26098 1.49032 0.59663 1.00000 0.01807 0.01994 0.02082 0.00347 -0.00148 -0.00225 0.01969 0.00433 0.00034 0.00056 0.00012 0.00000 0.00107 0.00139 0.00122 0.00111 0.00096 0.00110 0.00055 C2 -0.12581 1.27845 0.58312 1.00000 0.01909 0.01882 0.01881 0.00016 -0.00157 0.00188 0.01899 0.00439 0.00033 0.00058 0.00012 0.00000 0.00115 0.00131 0.00116 0.00098 0.00094 0.00105 0.00054 H2 -0.13736 1.17415 0.54254 1.00000 0.02279 0.00000 0.00000 C3 0.02687 1.22312 0.63059 1.00000 0.01834 0.01991 0.02242 0.00267 0.00101 0.00039 0.02023 0.00460 0.00037 0.00056 0.00013 0.00000 0.00115 0.00148 0.00125 0.00098 0.00098 0.00094 0.00057 C4 0.04863 1.36270 0.69113 1.00000 0.02206 0.02335 0.02159 0.00248 -0.00393 0.00038 0.02250 0.00436 0.00035 0.00057 0.00012 0.00000 0.00117 0.00147 0.00122 0.00115 0.00095 0.00114 0.00057 H4 0.15487 1.31828 0.72254 1.00000 0.02701 0.00000 0.00000 C5 -0.09038 1.56999 0.70433 1.00000 0.02558 0.02584 0.01919 -0.00133 -0.00104 -0.00021 0.02361 0.00449 0.00036 0.00062 0.00012 0.00000 0.00127 0.00153 0.00119 0.00112 0.00100 0.00117 0.00059 H5 -0.08073 1.66864 0.74571 1.00000 0.02833 0.00000 0.00000 C6 -0.24343 1.63477 0.65771 1.00000 0.01959 0.02237 0.02189 -0.00048 -0.00058 -0.00014 0.02134 0.00434 0.00036 0.00058 0.00012 0.00000 0.00114 0.00156 0.00121 0.00117 0.00095 0.00111 0.00057 H6 -0.33713 1.77830 0.66728 1.00000 0.02560 0.00000 0.00000 C7 -0.50000 1.42224 0.50000 0.50000 0.01596 0.01650 0.02105 0.00000 -0.00011 0.00000 0.01787 0.00355 0.00000 0.00075 0.00000 0.00000 0.00151 0.00207 0.00172 0.00000 0.00131 0.00000 0.00076 N1 -0.40724 1.58402 0.54897 1.00000 0.02148 0.01742 0.02114 -0.00022 -0.00666 0.00103 0.02027 0.00363 0.00032 0.00049 0.00010 0.00000 0.00102 0.00128 0.00107 0.00090 0.00083 0.00090 0.00050 N2 0.17490 1.00569 0.61493 1.00000 0.01973 0.02673 0.02385 0.00246 -0.00005 0.00444 0.02348 0.00390 0.00030 0.00051 0.00011 0.00000 0.00100 0.00129 0.00106 0.00102 0.00086 0.00099 0.00051 O1 -0.50000 1.16423 0.50000 0.50000 0.02683 0.01762 0.02927 0.00000 -0.00925 0.00000 0.02494 0.00256 0.00000 0.00054 0.00000 0.00000 0.00136 0.00145 0.00139 0.00000 0.00108 0.00000 0.00061 O2 0.14486 0.86127 0.56465 1.00000 0.02987 0.02970 0.02328 -0.00254 -0.00093 0.00609 0.02770 0.00330 0.00026 0.00044 0.00009 0.00000 0.00095 0.00117 0.00096 0.00091 0.00076 0.00091 0.00048 O3 0.32383 0.98298 0.65325 1.00000 0.02465 0.05216 0.03211 -0.00325 -0.00992 0.01453 0.03669 0.00371 0.00027 0.00051 0.00010 0.00000 0.00092 0.00150 0.00108 0.00102 0.00081 0.00100 0.00058 H1N -0.43634 1.76048 0.54819 1.00000 0.02449 0.04646 0.00393 0.00413 0.00137 0.00000 0.00777 Final Structure Factor Calculation for 2008lsh121 in I2 Total number of l.s. parameters = 106 Maximum vector length = 511 Memory required = 1319 / 25046 wR2 = 0.0927 before cycle 7 for 1282 data and 2 / 106 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 0.025 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.125; Restrained GooF = 1.125 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0444 for 1132 Fo > 4sig(Fo) and 0.0567 for all 1282 data wR2 = 0.0927, GooF = S = 1.125, Restrained GooF = 1.125 for all data Flack x parameter = -0.5593 with esd 1.9434 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 5.00 for hydrogen atoms Principal mean square atomic displacements U 0.0256 0.0169 0.0166 C1 0.0222 0.0190 0.0158 C2 0.0241 0.0186 0.0180 C3 0.0277 0.0234 0.0164 C4 0.0265 0.0260 0.0184 C5 0.0230 0.0222 0.0188 C6 0.0213 0.0165 0.0158 C7 0.0295 0.0174 0.0139 N1 0.0294 0.0240 0.0170 N2 0.0394 0.0178 0.0176 O1 0.0369 0.0238 0.0224 O2 0.0609 0.0350 0.0141 O3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.025 0.038 0.047 0.059 0.069 0.082 0.103 0.127 0.189 1.000 Number in group 133. 139. 119. 135. 118. 131. 125. 128. 125. 129. GooF 1.289 1.203 1.158 1.103 1.294 0.991 1.043 0.968 0.906 1.217 K 1.013 0.984 0.946 0.967 0.947 0.976 1.006 1.014 1.017 1.014 Resolution(A) 0.77 0.81 0.84 0.88 0.94 1.00 1.08 1.18 1.36 1.72 inf Number in group 129. 128. 129. 131. 125. 127. 128. 129. 128. 128. GooF 1.155 1.237 1.182 1.120 1.226 1.189 0.942 0.890 1.014 1.235 K 1.036 1.060 0.988 0.998 0.995 0.997 1.010 1.001 1.020 1.009 R1 0.134 0.126 0.121 0.079 0.073 0.046 0.038 0.030 0.028 0.024 Recommended weighting scheme: WGHT 0.0000 0.9096 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 -2 6 43.61 79.77 3.67 0.067 1.28 -2 0 2 811.64 941.41 3.59 0.231 3.23 -1 0 19 38.49 5.40 3.36 0.017 1.05 3 2 15 140.82 187.43 3.13 0.103 1.01 3 0 7 863.54 746.01 3.01 0.205 1.72 3 2 7 36.06 63.63 2.99 0.060 1.39 -6 -4 6 -15.07 18.08 2.74 0.032 0.79 -2 -5 11 74.27 39.14 2.64 0.047 0.82 4 -3 11 25.72 2.49 2.62 0.012 0.96 -2 -2 4 3551.65 3323.63 2.61 0.433 1.82 0 2 2 17.85 36.88 2.61 0.046 2.30 -4 4 4 -10.94 21.27 2.57 0.035 0.95 0 -5 9 24.37 5.37 2.54 0.017 0.87 -7 0 11 -1.58 11.61 2.52 0.026 0.87 -6 -2 10 74.96 105.30 2.51 0.077 0.92 1 -4 7 4.76 17.39 2.48 0.031 1.07 1 3 16 54.14 80.79 2.47 0.068 0.96 -1 0 13 1167.40 1050.58 2.47 0.244 1.52 0 -4 10 27.43 47.84 2.39 0.052 1.02 2 4 14 18.22 41.68 2.39 0.049 0.87 0 -2 18 133.95 171.05 2.33 0.098 1.01 4 5 5 -10.93 10.54 2.32 0.024 0.80 -2 -4 12 56.64 81.93 2.32 0.068 0.93 4 2 18 -6.81 5.90 2.31 0.018 0.85 2 1 9 603.90 538.50 2.29 0.174 1.69 -1 -3 2 224.87 185.09 2.25 0.102 1.52 5 -1 12 39.09 64.26 2.25 0.060 1.00 3 -2 15 152.54 187.48 2.25 0.103 1.01 -8 -2 4 93.90 65.91 2.23 0.061 0.79 -3 -3 20 43.03 66.44 2.21 0.061 0.80 1 -2 15 39.38 58.26 2.18 0.057 1.14 -6 -2 12 37.02 57.87 2.17 0.057 0.88 1 -2 7 1469.20 1361.39 2.17 0.277 1.74 5 -4 9 47.36 24.04 2.16 0.037 0.81 0 -1 5 1036.90 1125.70 2.16 0.252 3.05 4 -4 14 114.61 76.83 2.14 0.066 0.79 -7 3 2 362.31 284.95 2.14 0.127 0.82 5 -5 0 5.35 29.92 2.13 0.041 0.77 0 -4 14 13.62 31.38 2.13 0.042 0.91 4 -5 3 1.03 14.02 2.13 0.028 0.81 5 -2 9 85.51 118.84 2.12 0.082 1.01 3 4 13 182.52 136.80 2.11 0.088 0.85 -8 1 1 69.04 96.03 2.10 0.074 0.83 -7 2 9 28.71 51.84 2.10 0.054 0.84 1 -4 19 20.02 6.11 2.10 0.019 0.78 -4 -3 5 41.00 57.02 2.07 0.057 1.11 -3 -5 6 14.20 44.30 2.07 0.050 0.84 -5 0 15 35.49 55.81 2.06 0.056 0.97 -4 -4 4 10.85 21.30 2.05 0.035 0.95 -3 0 19 22.58 10.26 2.04 0.024 0.97 Bond lengths and angles C1 - Distance Angles C2 1.3853 (0.0035) C6 1.4002 (0.0034) 119.65 (0.21) N1 1.4053 (0.0031) 122.39 (0.22) 117.75 (0.23) C1 - C2 C6 C2 - Distance Angles C1 1.3853 (0.0035) C3 1.3869 (0.0032) 118.03 (0.22) H2 0.9500 120.99 120.99 C2 - C1 C3 C3 - Distance Angles C4 1.3812 (0.0035) C2 1.3869 (0.0032) 123.64 (0.23) N2 1.4724 (0.0033) 118.47 (0.21) 117.89 (0.22) C3 - C4 C2 C4 - Distance Angles C3 1.3812 (0.0035) C5 1.3858 (0.0037) 117.49 (0.22) H4 0.9500 121.26 121.26 C4 - C3 C5 C5 - Distance Angles C4 1.3858 (0.0037) C6 1.3868 (0.0033) 120.63 (0.24) H5 0.9500 119.69 119.69 C5 - C4 C6 C6 - Distance Angles C5 1.3868 (0.0033) C1 1.4002 (0.0034) 120.53 (0.24) H6 0.9500 119.73 119.73 C6 - C5 C1 C7 - Distance Angles O1 1.2169 (0.0043) N1 1.3676 (0.0028) 123.91 (0.16) N1_$2 1.3676 (0.0028) 123.91 (0.16) 112.18 (0.31) C7 - O1 N1 N1 - Distance Angles C7 1.3676 (0.0028) C1 1.4053 (0.0031) 126.07 (0.24) H1N 0.8548 (0.0181) 115.77 (1.92) 118.01 (1.91) N1 - C7 C1 N2 - Distance Angles O2 1.2242 (0.0028) O3 1.2336 (0.0028) 123.93 (0.22) C3 1.4724 (0.0033) 118.56 (0.20) 117.50 (0.21) N2 - O2 O3 O1 - Distance Angles C7 1.2169 (0.0043) O1 - O2 - Distance Angles N2 1.2242 (0.0028) O2 - O3 - Distance Angles N2 1.2336 (0.0028) O3 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.855(18) 2.17(2) 2.962(3) 155(3) 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)