+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0078 started at 14:50:26 on 05-Mar-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0078 in P2(1)/n CELL 0.71073 7.8088 7.3343 13.4110 90.000 104.984 90.000 ZERR 4.00 0.0004 0.0002 0.0007 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 28 32 16 8 V = 741.96 F(000) = 376.0 Mu = 0.12 mm-1 Cell Wt = 720.70 Rho = 1.613 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 5 eqiv $1 -x+1, -y, -z+1 eqiv $2 x+1/2, -y+1/2, z+1/2 eqiv $3 x-1/2, -y+1/2, z+1/2 htab N1 O1_$1 htab N4 N2_$2 htab N4 O2_$3 size 0.52 0.08 0.03 ACTA HTAB BOND $H WGHT 0.005000 1.39500 L.S. 15 TEMP -153.00 FVAR 0.74807 O1 4 0.353586 0.114896 0.561249 11.00000 0.01514 0.02471 = 0.01972 -0.00276 0.00219 0.00119 O2 4 0.267708 -0.010280 0.221763 11.00000 0.02667 0.03049 = 0.01954 0.00021 0.00981 0.00414 N1 3 0.299770 0.053373 0.389623 11.00000 0.01336 0.02084 = 0.01849 -0.00063 0.00375 0.00221 N4 3 0.014182 0.294449 0.618100 11.00000 0.01928 0.02493 = 0.01853 -0.00147 0.00627 0.00411 C4 1 -0.040875 0.192688 0.352172 11.00000 0.01748 0.01661 = 0.01732 0.00280 0.00656 0.00021 N3 3 -0.185558 0.306935 0.451364 11.00000 0.01557 0.01988 = 0.01753 0.00048 0.00525 0.00214 C6 1 -0.025996 0.268126 0.515115 11.00000 0.01301 0.01490 = 0.02015 0.00144 0.00418 -0.00104 C1 1 0.247696 0.119966 0.474827 11.00000 0.01760 0.01357 = 0.01739 -0.00010 0.00487 -0.00118 N2 3 -0.197807 0.262405 0.348613 11.00000 0.01935 0.02149 = 0.01718 0.00148 0.00554 0.00124 C5 1 0.073143 0.192518 0.451784 11.00000 0.01758 0.01448 = 0.01866 -0.00056 0.00578 -0.00108 C7 1 -0.337519 0.385215 0.478231 11.00000 0.01690 0.02147 = 0.02540 0.00259 0.00832 0.00400 AFIX 137 H7A 2 -0.340041 0.344359 0.547411 11.00000 -1.50000 H7B 2 -0.446207 0.345853 0.428118 11.00000 -1.50000 H7C 2 -0.329352 0.518515 0.477382 11.00000 -1.50000 AFIX 0 C2 1 0.201447 0.049128 0.287968 11.00000 0.01872 0.01578 = 0.01969 0.00112 0.00670 -0.00049 C3 1 0.012463 0.115609 0.261893 11.00000 0.02125 0.01921 = 0.01562 -0.00035 0.00471 -0.00078 AFIX 23 H3A 2 -0.003032 0.210306 0.207681 11.00000 -1.20000 H3B 2 -0.067309 0.012811 0.233283 11.00000 -1.20000 AFIX 0 H1N 2 0.410590 0.014250 0.402270 11.00000 0.02697 H4A 2 0.122183 0.271752 0.655619 11.00000 0.02483 H4B 2 -0.049780 0.373578 0.643642 11.00000 0.03771 HKLF 4 Covalent radii and connectivity table for 2007src0078 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 O1 - C1 O2 - C2 N1 - C2 C1 N4 - C6 C4 - N2 C5 C3 N3 - C6 N2 C7 C6 - N3 N4 C5 C1 - O1 N1 C5 N2 - C4 N3 C5 - C4 C6 C1 C7 - N3 C2 - O2 N1 C3 C3 - C4 C2 Operators for generating equivalent atoms: $1 -x+1, -y, -z+1 $2 x+1/2, -y+1/2, z+1/2 $3 x-1/2, -y+1/2, z+1/2 7138 Reflections read, of which 349 rejected -10 =< h =< 10, -9 =< k =< 9, -17 =< l =< 17, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 1689 Unique reflections, of which 0 suppressed R(int) = 0.0549 R(sigma) = 0.0511 Friedel opposites merged Maximum memory for data reduction = 1383 / 16960 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 = 1718 / 165785 wR2 = 0.1287 before cycle 1 for 1689 data and 131 / 131 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74816 0.00231 0.039 OSF Mean shift/esd = 0.015 Maximum = -0.066 for U12 C1 Max. shift = 0.001 A for H4A Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 1718 / 165785 wR2 = 0.1287 before cycle 2 for 1689 data and 131 / 131 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74820 0.00231 0.017 OSF Mean shift/esd = 0.006 Maximum = -0.027 for U12 C1 Max. shift = 0.000 A for H4A Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 1718 / 165785 wR2 = 0.1287 before cycle 3 for 1689 data and 131 / 131 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74820 0.00231 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.004 for tors H7A Max. shift = 0.000 A for H7C Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1718 / 165785 wR2 = 0.1287 before cycle 4 for 1689 data and 131 / 131 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74820 0.00231 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for tors H7A Max. shift = 0.000 A for H7A Max. dU = 0.000 for H4B Least-squares cycle 5 Maximum vector length = 511 Memory required = 1718 / 165785 wR2 = 0.1287 before cycle 5 for 1689 data and 131 / 131 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74820 0.00231 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H7A Max. shift = 0.000 A for H7A Max. dU = 0.000 for H4A Least-squares cycle 6 Maximum vector length = 511 Memory required = 1718 / 165785 wR2 = 0.1287 before cycle 6 for 1689 data and 131 / 131 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74820 0.00231 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H7A Max. dU = 0.000 for H4B Least-squares cycle 7 Maximum vector length = 511 Memory required = 1718 / 165785 wR2 = 0.1287 before cycle 7 for 1689 data and 131 / 131 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74820 0.00231 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H4A Max. dU = 0.000 for H4B Least-squares cycle 8 Maximum vector length = 511 Memory required = 1718 / 165785 wR2 = 0.1287 before cycle 8 for 1689 data and 131 / 131 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74820 0.00231 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H4B Max. dU = 0.000 for H4A Least-squares cycle 9 Maximum vector length = 511 Memory required = 1718 / 165785 wR2 = 0.1287 before cycle 9 for 1689 data and 131 / 131 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74820 0.00231 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H4A Max. dU = 0.000 for H4A Least-squares cycle 10 Maximum vector length = 511 Memory required = 1718 / 165785 wR2 = 0.1287 before cycle 10 for 1689 data and 131 / 131 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74820 0.00231 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H4B Max. dU = 0.000 for H4A Least-squares cycle 11 Maximum vector length = 511 Memory required = 1718 / 165785 wR2 = 0.1287 before cycle 11 for 1689 data and 131 / 131 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74820 0.00231 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H4B Max. dU = 0.000 for H1N Least-squares cycle 12 Maximum vector length = 511 Memory required = 1718 / 165785 wR2 = 0.1287 before cycle 12 for 1689 data and 131 / 131 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74820 0.00231 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H4B Max. dU = 0.000 for H4B Least-squares cycle 13 Maximum vector length = 511 Memory required = 1718 / 165785 wR2 = 0.1287 before cycle 13 for 1689 data and 131 / 131 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74820 0.00231 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H4A Max. dU = 0.000 for H4A Least-squares cycle 14 Maximum vector length = 511 Memory required = 1718 / 165785 wR2 = 0.1287 before cycle 14 for 1689 data and 131 / 131 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74820 0.00231 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H4A Max. dU = 0.000 for H1N Least-squares cycle 15 Maximum vector length = 511 Memory required = 1718 / 165785 wR2 = 0.1287 before cycle 15 for 1689 data and 131 / 131 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74820 0.00231 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1 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 16 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H7A -0.3401 0.3443 0.5474 137 0.980 0.000 C7 N3 H7A H7B -0.4462 0.3459 0.4281 137 0.980 0.000 C7 N3 H7A H7C -0.3293 0.5185 0.4774 137 0.980 0.000 C7 N3 H7A H3A -0.0030 0.2103 0.2077 23 0.990 0.000 C3 C4 C2 H3B -0.0673 0.0128 0.2333 23 0.990 0.000 C3 C4 C2 2007src0078 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O1 0.35358 0.11488 0.56125 1.00000 0.01518 0.02472 0.01971 -0.00276 0.00221 0.00117 0.02030 0.00314 0.00021 0.00023 0.00013 0.00000 0.00084 0.00091 0.00086 0.00072 0.00067 0.00069 0.00040 O2 0.26770 -0.01028 0.22176 1.00000 0.02669 0.03053 0.01954 0.00020 0.00984 0.00414 0.02487 0.00356 0.00023 0.00026 0.00013 0.00000 0.00098 0.00103 0.00090 0.00075 0.00076 0.00077 0.00044 N1 0.29976 0.05338 0.38962 1.00000 0.01335 0.02087 0.01848 -0.00064 0.00377 0.00221 0.01763 0.00389 0.00027 0.00028 0.00015 0.00000 0.00099 0.00104 0.00102 0.00083 0.00080 0.00081 0.00044 N4 0.01418 0.29445 0.61810 1.00000 0.01927 0.02498 0.01855 -0.00145 0.00625 0.00409 0.02068 0.00423 0.00030 0.00030 0.00016 0.00000 0.00108 0.00115 0.00104 0.00089 0.00089 0.00091 0.00046 C4 -0.04087 0.19268 0.35217 1.00000 0.01747 0.01657 0.01739 0.00276 0.00655 0.00016 0.01676 0.00451 0.00030 0.00032 0.00018 0.00000 0.00113 0.00115 0.00114 0.00093 0.00093 0.00092 0.00049 N3 -0.18556 0.30694 0.45137 1.00000 0.01560 0.01991 0.01753 0.00048 0.00524 0.00211 0.01750 0.00383 0.00025 0.00028 0.00015 0.00000 0.00096 0.00103 0.00098 0.00080 0.00079 0.00080 0.00044 C6 -0.02600 0.26812 0.51511 1.00000 0.01304 0.01490 0.02016 0.00143 0.00420 -0.00107 0.01605 0.00438 0.00029 0.00031 0.00018 0.00000 0.00107 0.00108 0.00116 0.00092 0.00090 0.00086 0.00048 C1 0.24768 0.11997 0.47483 1.00000 0.01766 0.01353 0.01743 -0.00011 0.00487 -0.00127 0.01615 0.00445 0.00030 0.00031 0.00018 0.00000 0.00111 0.00108 0.00112 0.00092 0.00091 0.00089 0.00047 N2 -0.19781 0.26240 0.34861 1.00000 0.01936 0.02149 0.01720 0.00147 0.00554 0.00124 0.01920 0.00393 0.00026 0.00028 0.00015 0.00000 0.00104 0.00105 0.00098 0.00083 0.00081 0.00082 0.00045 C5 0.07315 0.19251 0.45179 1.00000 0.01761 0.01447 0.01867 -0.00053 0.00578 -0.00105 0.01672 0.00442 0.00030 0.00031 0.00018 0.00000 0.00115 0.00108 0.00115 0.00091 0.00093 0.00090 0.00049 C7 -0.33751 0.38521 0.47824 1.00000 0.01694 0.02148 0.02537 0.00260 0.00833 0.00395 0.02073 0.00492 0.00031 0.00035 0.00019 0.00000 0.00118 0.00123 0.00126 0.00103 0.00099 0.00097 0.00053 H7A -0.34008 0.34429 0.54740 1.00000 0.03110 0.00000 0.00000 H7B -0.44620 0.34590 0.42810 1.00000 0.03110 0.00000 0.00000 H7C -0.32932 0.51851 0.47743 1.00000 0.03110 0.00000 0.00000 C2 0.20144 0.04913 0.28797 1.00000 0.01878 0.01578 0.01973 0.00116 0.00671 -0.00050 0.01777 0.00460 0.00031 0.00032 0.00018 0.00000 0.00116 0.00114 0.00118 0.00094 0.00094 0.00092 0.00050 C3 0.01247 0.11561 0.26190 1.00000 0.02126 0.01919 0.01566 -0.00032 0.00471 -0.00082 0.01872 0.00464 0.00031 0.00034 0.00018 0.00000 0.00121 0.00118 0.00112 0.00095 0.00093 0.00096 0.00051 H3A -0.00302 0.21031 0.20769 1.00000 0.02246 0.00000 0.00000 H3B -0.06730 0.01281 0.23328 1.00000 0.02246 0.00000 0.00000 H1N 0.41059 0.01434 0.40221 1.00000 0.02654 0.05637 0.00413 0.00402 0.00219 0.00000 0.00759 H4A 0.12213 0.27159 0.65559 1.00000 0.02492 0.05763 0.00408 0.00399 0.00225 0.00000 0.00759 H4B -0.04978 0.37354 0.64368 1.00000 0.03754 0.06114 0.00429 0.00454 0.00248 0.00000 0.00886 Final Structure Factor Calculation for 2007src0078 in P2(1)/n Total number of l.s. parameters = 131 Maximum vector length = 511 Memory required = 1587 / 22995 wR2 = 0.1287 before cycle 16 for 1689 data and 0 / 131 parameters GooF = S = 1.105; Restrained GooF = 1.105 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 1.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0608 for 1357 Fo > 4sig(Fo) and 0.0799 for all 1689 data wR2 = 0.1287, GooF = S = 1.105, Restrained GooF = 1.105 for all data Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0269 0.0194 0.0147 O1 0.0332 0.0252 0.0162 O2 0.0219 0.0183 0.0127 N1 0.0274 0.0196 0.0150 N4 0.0202 0.0170 0.0131 C4 0.0208 0.0175 0.0142 N3 0.0208 0.0151 0.0122 C6 0.0181 0.0172 0.0132 C1 0.0224 0.0188 0.0164 N2 0.0193 0.0167 0.0141 C5 0.0275 0.0209 0.0138 C7 0.0208 0.0177 0.0149 C2 0.0216 0.0189 0.0156 C3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.017 0.027 0.036 0.048 0.062 0.079 0.103 0.149 1.000 Number in group 193. 145. 176. 168. 165. 173. 165. 167. 167. 170. GooF 1.271 1.147 1.085 1.225 1.081 1.024 1.026 1.063 0.901 1.157 K 5.927 1.693 1.147 1.089 1.020 1.033 1.004 0.988 0.999 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 171. 170. 175. 159. 169. 169. 170. 167. 169. 170. GooF 1.082 1.202 1.212 1.198 1.099 1.039 1.032 0.951 0.909 1.264 K 1.115 1.067 1.072 1.023 1.021 0.992 0.994 0.976 1.007 1.007 R1 0.168 0.215 0.145 0.127 0.105 0.073 0.048 0.054 0.038 0.035 Recommended weighting scheme: WGHT 0.0000 1.3910 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) -3 6 6 31.31 0.58 4.10 0.006 1.03 3 6 0 58.36 24.85 3.84 0.038 1.10 0 3 3 15.02 0.33 3.25 0.004 2.13 3 3 11 -7.66 12.79 3.13 0.027 0.90 6 4 7 0.97 18.89 3.07 0.033 0.83 -1 1 3 13.67 2.99 3.06 0.013 3.68 -5 7 1 17.00 0.87 2.89 0.007 0.87 3 4 11 138.97 87.04 2.89 0.071 0.86 5 7 4 46.19 4.86 2.88 0.017 0.80 -2 2 14 57.34 29.71 2.87 0.041 0.93 3 3 3 17.95 5.75 2.86 0.018 1.53 -10 1 6 33.24 11.89 2.75 0.026 0.77 -1 1 2 1929.31 2129.51 2.73 0.351 4.50 1 1 5 668.37 570.19 2.66 0.182 2.17 -4 4 13 11.34 0.00 2.66 0.000 0.87 8 3 3 15.29 0.91 2.60 0.007 0.82 -6 7 3 1.66 16.38 2.57 0.031 0.82 2 0 2 98.82 138.78 2.57 0.090 2.95 -1 1 16 55.88 19.55 2.53 0.034 0.82 2 1 5 1244.21 1101.69 2.50 0.252 1.85 -3 3 13 527.08 436.40 2.49 0.159 0.94 3 3 7 13.28 34.52 2.48 0.045 1.17 -8 1 1 0.95 13.69 2.46 0.028 0.95 2 8 7 -6.45 8.19 2.43 0.022 0.78 -5 7 8 20.89 3.44 2.43 0.014 0.81 -7 5 5 42.85 15.25 2.43 0.030 0.88 -5 4 13 15.47 36.23 2.43 0.046 0.85 6 3 7 43.21 19.56 2.40 0.034 0.87 7 1 7 -2.87 5.59 2.39 0.018 0.84 8 3 0 0.58 13.37 2.39 0.028 0.88 -6 6 11 250.64 183.71 2.39 0.103 0.77 1 2 11 65.92 97.26 2.39 0.075 1.07 -1 2 6 64.43 41.81 2.38 0.049 1.91 -4 0 4 230.05 182.90 2.38 0.103 1.85 -7 5 10 12.79 2.52 2.36 0.012 0.80 -7 0 11 95.03 139.98 2.35 0.090 0.92 -2 1 7 659.81 575.32 2.34 0.182 1.81 -6 2 12 468.21 391.59 2.33 0.150 0.92 6 6 3 16.31 1.57 2.32 0.010 0.83 -3 6 3 542.37 445.92 2.32 0.161 1.10 4 2 6 1080.45 1216.67 2.28 0.265 1.20 3 7 7 28.88 0.00 2.28 0.000 0.82 8 0 4 415.91 325.26 2.27 0.137 0.85 -2 1 16 5.23 18.68 2.26 0.033 0.83 4 7 5 24.06 0.73 2.25 0.006 0.83 0 1 6 513.47 444.26 2.21 0.160 2.07 0 1 16 -3.24 9.53 2.20 0.023 0.80 -5 0 7 690.82 786.90 2.20 0.213 1.35 5 1 8 11.67 0.00 2.20 0.000 0.98 -2 1 11 7.50 0.54 2.20 0.006 1.20 Bond lengths and angles O1 - Distance Angles C1 1.2381 (0.0028) O1 - O2 - Distance Angles C2 1.2180 (0.0028) O2 - N1 - Distance Angles C2 1.3812 (0.0031) C1 1.3964 (0.0029) 127.62 (0.20) H1N 0.8854 (0.0308) 116.57 (1.86) 115.74 (1.86) N1 - C2 C1 N4 - Distance Angles C6 1.3488 (0.0031) H4A 0.8789 (0.0307) 119.56 (1.88) H4B 0.8901 (0.0341) 118.87 (2.09) 117.04 (2.79) N4 - C6 H4A C4 - Distance Angles N2 1.3173 (0.0029) C5 1.4009 (0.0033) 113.01 (0.20) C3 1.4898 (0.0031) 124.81 (0.21) 122.16 (0.21) C4 - N2 C5 N3 - Distance Angles C6 1.3467 (0.0030) N2 1.3953 (0.0027) 113.16 (0.18) C7 1.4451 (0.0029) 127.61 (0.20) 119.22 (0.19) N3 - C6 N2 C6 - Distance Angles N3 1.3467 (0.0029) N4 1.3488 (0.0031) 123.49 (0.21) C5 1.4030 (0.0032) 105.32 (0.20) 131.13 (0.22) C6 - N3 N4 C1 - Distance Angles O1 1.2381 (0.0028) N1 1.3964 (0.0029) 119.35 (0.21) C5 1.4206 (0.0032) 125.86 (0.21) 114.77 (0.20) C1 - O1 N1 N2 - Distance Angles C4 1.3173 (0.0029) N3 1.3953 (0.0027) 103.27 (0.18) N2 - C4 C5 - Distance Angles C4 1.4009 (0.0033) C6 1.4030 (0.0032) 105.24 (0.20) C1 1.4206 (0.0032) 123.04 (0.21) 131.67 (0.22) C5 - C4 C6 C7 - Distance Angles N3 1.4451 (0.0029) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - N3 H7A H7B C2 - Distance Angles O2 1.2180 (0.0028) N1 1.3812 (0.0031) 119.68 (0.21) C3 1.5068 (0.0033) 121.45 (0.21) 118.87 (0.20) C2 - O2 N1 C3 - Distance Angles C4 1.4898 (0.0031) C2 1.5068 (0.0033) 113.39 (0.20) H3A 0.9900 108.89 108.89 H3B 0.9900 108.89 108.89 107.73 C3 - C4 C2 H3A Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.89(3) 2.02(3) 2.892(3) 170(3) N1-H1N...O1_$1 0.88(3) 2.62(3) 3.346(3) 141(2) N4-H4A...N2_$2 0.89(3) 2.21(3) 3.086(3) 166(3) N4-H4B...O2_$3 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)