+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0078y started at 15:29:51 on 05-Mar-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0078y in P2(1)/n CELL 0.71073 8.5795 8.5965 11.4708 90.000 98.957 90.000 ZERR 4.00 0.0003 0.0002 0.0003 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 40 16 12 V = 835.70 F(000) = 416.0 Mu = 0.13 mm-1 Cell Wt = 792.76 Rho = 1.575 MERG 2 OMIT -3.00 55.00 OMIT 4 0 4 EXTI 0.04402 SHEL 7 0.77 FMAP 2 PLAN 5 SIZE 0.36 0.22 0.15 ACTA EQIV $1 x-1/2, -y+1/2, z+1/2 EQIV $2 -x+2, -y, -z+2 EQIV $3 x, y-1, z HTAB N1 O11 HTAB N4 O2_$1 HTAB N4 O11_$1 HTAB O11 O1_$2 HTAB O11 N2_$3 HTAB BOND $H WGHT 0.04360 0.35830 L.S. 8 TEMP -153.00 FVAR 1.42018 MOLE 1 C1 1 0.823895 0.297165 0.934390 11.00000 0.01107 0.01516 = 0.01129 -0.00027 0.00100 -0.00099 C2 1 0.979516 0.371312 0.777352 11.00000 0.01405 0.01514 = 0.01221 -0.00058 0.00247 0.00025 C3 1 0.930433 0.540448 0.781184 11.00000 0.01853 0.01272 = 0.01430 0.00184 0.00598 0.00161 AFIX 23 H3A 2 1.026125 0.606475 0.790969 11.00000 -1.20000 H3B 2 0.865660 0.567994 0.704849 11.00000 -1.20000 AFIX 0 C4 1 0.838746 0.575510 0.878364 11.00000 0.01204 0.01334 = 0.01276 0.00041 0.00278 -0.00047 C5 1 0.788684 0.457039 0.948313 11.00000 0.01278 0.01331 = 0.01170 -0.00041 0.00336 -0.00042 C6 1 0.708788 0.534645 1.029724 11.00000 0.01167 0.01427 = 0.01138 -0.00016 0.00212 -0.00046 C7 1 0.649390 0.815609 1.062302 11.00000 0.02051 0.01451 = 0.01876 -0.00299 0.00713 0.00175 AFIX 137 H7A 2 0.534656 0.803071 1.053962 11.00000 -1.50000 H7B 2 0.674040 0.913947 1.025980 11.00000 -1.50000 H7C 2 0.694455 0.816408 1.146227 11.00000 -1.50000 AFIX 0 N1 3 0.920247 0.265364 0.849771 11.00000 0.01702 0.01123 = 0.01518 -0.00083 0.00506 0.00099 N2 3 0.796863 0.715057 0.909556 11.00000 0.01499 0.01434 = 0.01299 0.00162 0.00658 -0.00004 N3 3 0.716181 0.687123 1.004050 11.00000 0.01477 0.01309 = 0.01329 -0.00010 0.00675 0.00004 N4 3 0.640301 0.476719 1.117969 11.00000 0.02116 0.01572 = 0.01597 0.00014 0.00999 -0.00141 O1 4 0.776828 0.188507 0.990968 11.00000 0.02076 0.01341 = 0.01991 0.00355 0.00610 -0.00214 O2 4 1.068784 0.329591 0.710292 11.00000 0.02152 0.01805 = 0.01990 -0.00248 0.01016 0.00197 H1 2 0.949049 0.160927 0.841752 11.00000 0.03240 H4A 2 0.633603 0.374621 1.127512 11.00000 0.02531 H4B 2 0.593505 0.536069 1.170451 11.00000 0.04140 MOLE 2 O11 4 1.000067 -0.059388 0.829462 11.00000 0.02279 0.01515 = 0.02149 0.00373 0.00666 -0.00080 H11A 2 1.085407 -0.084119 0.883856 11.00000 0.04623 H11B 2 0.918601 -0.112453 0.853725 11.00000 0.05410 HKLF 4 Covalent radii and connectivity table for 2007src0078y in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1 N1 C5 C2 - O2 N1 C3 C3 - C4 C2 C4 - N2 C5 C3 C5 - C4 C6 C1 C6 - N4 N3 C5 C7 - N3 N1 - C2 C1 N2 - C4 N3 N3 - C6 N2 C7 N4 - C6 O1 - C1 O2 - C2 O11 - no bonds found Operators for generating equivalent atoms: $1 x-1/2, -y+1/2, z+1/2 $2 -x+2, -y, -z+2 $3 x, y-1, z h k l Fo^2 Sigma Why rejected 4 0 1 7.46 1.70 observed but should be systematically absent 10755 Reflections read, of which 454 rejected -11 =< h =< 10, -11 =< k =< 9, -14 =< l =< 13, Max. 2-theta = 54.97 1 Systematic absence violations 0 Inconsistent equivalents 1904 Unique reflections, of which 0 suppressed R(int) = 0.0366 R(sigma) = 0.0314 Friedel opposites merged Maximum memory for data reduction = 1565 / 19006 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 = 1939 / 186746 wR2 = 0.0938 before cycle 1 for 1904 data and 149 / 149 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0436 * P )^2 + 0.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.42049 0.00451 0.068 OSF 2 0.04438 0.00790 0.045 EXTI Mean shift/esd = 0.033 Maximum = -0.147 for y C6 Max. shift = 0.003 A for H1 Max. dU = 0.001 for H11A Least-squares cycle 2 Maximum vector length = 511 Memory required = 1939 / 186746 wR2 = 0.0937 before cycle 2 for 1904 data and 149 / 149 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0436 * P )^2 + 0.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.42043 0.00451 -0.013 OSF 2 0.04445 0.00791 0.009 EXTI Mean shift/esd = 0.011 Maximum = -0.051 for y C6 Max. shift = 0.001 A for H1 Max. dU = 0.000 for H11A Least-squares cycle 3 Maximum vector length = 511 Memory required = 1939 / 186746 wR2 = 0.0938 before cycle 3 for 1904 data and 149 / 149 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0436 * P )^2 + 0.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.42042 0.00451 -0.001 OSF 2 0.04444 0.00791 -0.001 EXTI Mean shift/esd = 0.001 Maximum = 0.012 for z H11A Max. shift = 0.000 A for H11A Max. dU = 0.000 for H11A Least-squares cycle 4 Maximum vector length = 511 Memory required = 1939 / 186746 wR2 = 0.0937 before cycle 4 for 1904 data and 149 / 149 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0436 * P )^2 + 0.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.42042 0.00451 -0.001 OSF 2 0.04443 0.00791 -0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for x O11 Max. shift = 0.000 A for H11A Max. dU = 0.000 for H11A Least-squares cycle 5 Maximum vector length = 511 Memory required = 1939 / 186746 wR2 = 0.0937 before cycle 5 for 1904 data and 149 / 149 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0436 * P )^2 + 0.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.42042 0.00451 0.000 OSF 2 0.04443 0.00791 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for U11 H4B Max. shift = 0.000 A for H4B Max. dU = 0.000 for H4B Least-squares cycle 6 Maximum vector length = 511 Memory required = 1939 / 186746 wR2 = 0.0937 before cycle 6 for 1904 data and 149 / 149 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0436 * P )^2 + 0.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.42042 0.00451 0.000 OSF 2 0.04443 0.00791 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C7 Max. shift = 0.000 A for H4B Max. dU = 0.000 for H4B Least-squares cycle 7 Maximum vector length = 511 Memory required = 1939 / 186746 wR2 = 0.0937 before cycle 7 for 1904 data and 149 / 149 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0436 * P )^2 + 0.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.42042 0.00451 0.000 OSF 2 0.04443 0.00791 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C7 Max. shift = 0.000 A for H4B Max. dU = 0.000 for H11A Least-squares cycle 8 Maximum vector length = 511 Memory required = 1939 / 186746 wR2 = 0.0937 before cycle 8 for 1904 data and 149 / 149 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0436 * P )^2 + 0.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.42042 0.00451 0.000 OSF 2 0.04443 0.00791 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C7 Max. shift = 0.000 A for H11B Max. dU = 0.000 for H4B Largest correlation matrix elements 0.670 EXTI / OSF Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3A 1.0261 0.6065 0.7910 23 0.990 0.000 C3 C4 C2 H3B 0.8656 0.5680 0.7049 23 0.990 0.000 C3 C4 C2 H7A 0.5347 0.8031 1.0540 137 0.980 0.000 C7 N3 H7A H7B 0.6741 0.9139 1.0260 137 0.980 0.000 C7 N3 H7A H7C 0.6944 0.8164 1.1462 137 0.980 0.000 C7 N3 H7A 2007src0078y in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.82390 0.29717 0.93439 1.00000 0.01105 0.01513 0.01130 -0.00027 0.00096 -0.00096 0.01257 0.00212 0.00014 0.00014 0.00010 0.00000 0.00057 0.00059 0.00052 0.00044 0.00042 0.00044 0.00027 C2 0.97951 0.37132 0.77735 1.00000 0.01401 0.01513 0.01221 -0.00059 0.00244 0.00024 0.01374 0.00216 0.00014 0.00014 0.00010 0.00000 0.00059 0.00061 0.00055 0.00045 0.00044 0.00046 0.00028 C3 0.93042 0.54044 0.78119 1.00000 0.01847 0.01273 0.01429 0.00185 0.00596 0.00160 0.01480 0.00230 0.00014 0.00014 0.00010 0.00000 0.00063 0.00061 0.00058 0.00045 0.00046 0.00045 0.00028 H3A 1.02612 0.60647 0.79097 1.00000 0.01776 0.00000 0.00000 H3B 0.86564 0.56799 0.70486 1.00000 0.01776 0.00000 0.00000 C4 0.83876 0.57549 0.87837 1.00000 0.01202 0.01334 0.01275 0.00041 0.00273 -0.00046 0.01262 0.00215 0.00014 0.00014 0.00010 0.00000 0.00057 0.00059 0.00054 0.00044 0.00043 0.00044 0.00027 C5 0.78868 0.45705 0.94830 1.00000 0.01275 0.01330 0.01166 -0.00039 0.00331 -0.00041 0.01242 0.00212 0.00014 0.00014 0.00010 0.00000 0.00058 0.00060 0.00054 0.00044 0.00043 0.00043 0.00027 C6 0.70879 0.53462 1.02971 1.00000 0.01164 0.01425 0.01139 -0.00016 0.00209 -0.00050 0.01239 0.00215 0.00013 0.00014 0.00010 0.00000 0.00057 0.00059 0.00054 0.00044 0.00043 0.00043 0.00027 C7 0.64939 0.81560 1.06231 1.00000 0.02047 0.01450 0.01876 -0.00306 0.00712 0.00175 0.01748 0.00240 0.00016 0.00014 0.00011 0.00000 0.00065 0.00060 0.00060 0.00049 0.00048 0.00049 0.00028 H7A 0.53466 0.80308 1.05396 1.00000 0.02622 0.00000 0.00000 H7B 0.67406 0.91394 1.02600 1.00000 0.02622 0.00000 0.00000 H7C 0.69445 0.81638 1.14624 1.00000 0.02622 0.00000 0.00000 N1 0.92025 0.26537 0.84977 1.00000 0.01701 0.01122 0.01516 -0.00081 0.00507 0.00100 0.01419 0.00188 0.00012 0.00012 0.00009 0.00000 0.00054 0.00052 0.00050 0.00041 0.00040 0.00040 0.00025 N2 0.79686 0.71506 0.90956 1.00000 0.01497 0.01428 0.01297 0.00161 0.00657 -0.00004 0.01361 0.00188 0.00012 0.00012 0.00009 0.00000 0.00052 0.00052 0.00048 0.00039 0.00038 0.00039 0.00025 N3 0.71618 0.68712 1.00405 1.00000 0.01475 0.01305 0.01331 -0.00010 0.00674 0.00006 0.01322 0.00189 0.00012 0.00012 0.00009 0.00000 0.00052 0.00052 0.00048 0.00038 0.00038 0.00038 0.00025 N4 0.64030 0.47671 1.11797 1.00000 0.02116 0.01570 0.01596 0.00015 0.00999 -0.00140 0.01685 0.00206 0.00013 0.00014 0.00009 0.00000 0.00058 0.00057 0.00052 0.00043 0.00043 0.00043 0.00026 O1 0.77682 0.18852 0.99097 1.00000 0.02070 0.01344 0.01990 0.00356 0.00611 -0.00215 0.01770 0.00167 0.00011 0.00010 0.00008 0.00000 0.00048 0.00046 0.00046 0.00034 0.00036 0.00034 0.00024 O2 1.06878 0.32958 0.71030 1.00000 0.02151 0.01805 0.01988 -0.00245 0.01016 0.00199 0.01908 0.00169 0.00011 0.00011 0.00008 0.00000 0.00050 0.00048 0.00046 0.00036 0.00037 0.00036 0.00024 H1 0.94875 0.16080 0.84188 1.00000 0.03251 0.03314 0.00208 0.00228 0.00153 0.00000 0.00455 H4A 0.63365 0.37448 1.12753 1.00000 0.02555 0.03121 0.00190 0.00217 0.00143 0.00000 0.00421 H4B 0.59375 0.53608 1.17039 1.00000 0.04116 0.03555 0.00223 0.00239 0.00169 0.00000 0.00511 O11 1.00006 -0.05938 0.82945 1.00000 0.02277 0.01513 0.02149 0.00373 0.00666 -0.00079 0.01946 0.00185 0.00012 0.00010 0.00008 0.00000 0.00053 0.00047 0.00050 0.00036 0.00040 0.00038 0.00024 H11A 1.08514 -0.08416 0.88388 1.00000 0.04703 0.03917 0.00253 0.00236 0.00183 0.00000 0.00560 H11B 0.91873 -0.11235 0.85369 1.00000 0.05384 0.04167 0.00278 0.00267 0.00189 0.00000 0.00596 Final Structure Factor Calculation for 2007src0078y in P2(1)/n Total number of l.s. parameters = 149 Maximum vector length = 511 Memory required = 1790 / 22995 wR2 = 0.0937 before cycle 9 for 1904 data and 0 / 149 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0436 * P )^2 + 0.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0349 for 1641 Fo > 4sig(Fo) and 0.0423 for all 1904 data wR2 = 0.0937, GooF = S = 1.048, Restrained GooF = 1.048 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0153 0.0120 0.0103 C1 0.0153 0.0140 0.0119 C2 0.0205 0.0127 0.0112 C3 0.0136 0.0131 0.0112 C4 0.0139 0.0129 0.0104 C5 0.0144 0.0117 0.0111 C6 0.0233 0.0184 0.0108 C7 0.0185 0.0136 0.0105 N1 0.0181 0.0144 0.0083 N2 0.0180 0.0131 0.0086 N3 0.0253 0.0158 0.0095 N4 0.0229 0.0198 0.0103 O1 0.0268 0.0197 0.0108 O2 0.0253 0.0205 0.0126 O11 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.018 0.035 0.052 0.073 0.094 0.123 0.156 0.203 0.296 1.000 Number in group 194. 191. 202. 181. 190. 184. 192. 188. 192. 190. GooF 0.839 1.114 1.132 1.114 1.097 1.078 1.044 0.983 0.969 1.080 K 0.898 0.888 0.939 0.960 0.985 0.999 1.004 1.016 1.014 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.65 inf Number in group 202. 185. 193. 190. 187. 190. 187. 191. 189. 190. GooF 0.958 1.011 0.860 1.011 1.027 1.002 1.015 0.903 1.098 1.481 K 0.997 1.031 1.019 1.011 1.010 1.005 0.997 1.010 1.015 1.006 R1 0.087 0.072 0.055 0.057 0.049 0.038 0.031 0.027 0.030 0.030 Recommended weighting scheme: WGHT 0.0424 0.3626 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 0 3 552.80 709.81 4.64 0.361 3.67 -1 4 2 275.48 216.17 4.12 0.199 1.98 -2 3 4 200.97 155.66 3.99 0.169 1.90 -5 0 5 56.86 36.49 3.91 0.082 1.47 0 1 2 60.83 85.68 3.90 0.125 4.73 -2 3 5 9.84 4.07 3.59 0.027 1.72 1 0 1 6.07 1.79 3.56 0.018 6.33 1 4 4 13.38 6.84 3.38 0.035 1.65 -4 3 2 188.32 151.06 3.26 0.167 1.69 -7 1 9 -0.59 3.79 3.25 0.026 0.94 -3 0 1 11.22 19.85 3.10 0.060 2.85 0 4 0 1181.99 1004.90 3.08 0.430 2.15 -9 5 3 4.00 15.18 3.04 0.053 0.83 1 2 2 28.34 40.63 3.03 0.086 3.08 3 0 1 84.67 108.27 3.00 0.141 2.65 -8 6 4 20.80 33.33 2.99 0.078 0.85 8 2 7 46.24 65.67 2.97 0.110 0.81 -5 6 4 27.83 40.11 2.90 0.086 1.06 0 9 1 121.23 95.17 2.86 0.132 0.95 -1 1 2 55.58 72.02 2.84 0.115 4.38 -4 4 2 70.74 55.09 2.79 0.101 1.50 -4 6 8 0.44 4.02 2.76 0.027 0.95 -1 8 3 17.78 26.87 2.74 0.070 1.03 -5 1 7 22.18 14.38 2.72 0.051 1.26 -3 6 9 25.97 38.01 2.67 0.084 0.93 -1 3 4 5.48 10.67 2.63 0.044 2.01 5 9 1 2.37 7.85 2.63 0.038 0.83 -3 7 10 22.25 10.43 2.61 0.044 0.82 -8 6 6 4.73 10.89 2.61 0.045 0.82 2 9 7 -15.02 12.95 2.53 0.049 0.80 1 3 3 27.47 19.56 2.53 0.060 2.15 4 10 3 83.76 55.72 2.51 0.101 0.77 -4 3 9 655.56 750.17 2.51 0.371 1.08 -2 2 4 78.34 63.38 2.50 0.108 2.19 -4 6 6 146.27 122.48 2.49 0.150 1.05 1 2 3 520.99 595.29 2.48 0.331 2.60 1 1 3 863.04 977.25 2.45 0.424 3.05 4 5 1 99.24 80.79 2.45 0.122 1.31 -6 8 5 16.41 8.92 2.42 0.040 0.83 -8 7 1 367.11 296.75 2.41 0.233 0.81 -2 4 4 24.93 17.79 2.39 0.057 1.64 0 8 3 11.70 18.59 2.39 0.058 1.03 8 5 6 -0.95 2.47 2.39 0.021 0.77 -5 3 10 30.34 21.69 2.39 0.063 0.96 3 2 1 316.00 363.43 2.39 0.258 2.25 3 2 7 12.45 7.59 2.37 0.037 1.26 -5 4 7 48.87 61.76 2.35 0.107 1.10 7 4 2 153.08 127.78 2.34 0.153 1.01 2 10 0 316.90 269.97 2.32 0.223 0.84 2 1 7 6.45 11.26 2.32 0.045 1.42 Bond lengths and angles C1 - Distance Angles O1 1.2403 (0.0015) N1 1.3965 (0.0015) 119.51 (0.11) C5 1.4216 (0.0017) 125.25 (0.11) 115.24 (0.10) C1 - O1 N1 C2 - Distance Angles O2 1.2208 (0.0014) N1 1.3819 (0.0015) 120.71 (0.11) C3 1.5161 (0.0017) 120.29 (0.11) 118.99 (0.10) C2 - O2 N1 C3 - Distance Angles C4 1.4916 (0.0015) C2 1.5161 (0.0017) 113.36 (0.10) H3A 0.9900 108.90 108.90 H3B 0.9900 108.90 108.90 107.73 C3 - C4 C2 H3A C4 - Distance Angles N2 1.3179 (0.0016) C5 1.4043 (0.0016) 112.60 (0.10) C3 1.4916 (0.0015) 125.78 (0.10) 121.62 (0.11) C4 - N2 C5 C5 - Distance Angles C4 1.4043 (0.0016) C6 1.4092 (0.0016) 105.02 (0.11) C1 1.4216 (0.0017) 123.20 (0.11) 131.73 (0.11) C5 - C4 C6 C6 - Distance Angles N4 1.3429 (0.0015) N3 1.3473 (0.0016) 124.50 (0.11) C5 1.4092 (0.0016) 129.74 (0.12) 105.74 (0.10) C6 - N4 N3 C7 - Distance Angles N3 1.4540 (0.0016) 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 N1 - Distance Angles C2 1.3819 (0.0016) C1 1.3965 (0.0015) 127.00 (0.10) H1 0.9396 (0.0195) 116.55 (1.07) 116.44 (1.07) N1 - C2 C1 N2 - Distance Angles C4 1.3179 (0.0016) N3 1.3948 (0.0013) 104.09 (0.09) N2 - C4 N3 - Distance Angles C6 1.3473 (0.0016) N2 1.3948 (0.0013) 112.54 (0.10) C7 1.4540 (0.0016) 127.12 (0.10) 120.34 (0.10) N3 - C6 N2 N4 - Distance Angles C6 1.3429 (0.0015) H4A 0.8886 (0.0185) 120.24 (1.06) H4B 0.9254 (0.0206) 124.70 (1.23) 115.01 (1.65) N4 - C6 H4A O1 - Distance Angles C1 1.2403 (0.0015) O1 - O2 - Distance Angles C2 1.2208 (0.0014) O2 - O11 - Distance Angles H11A 0.9089 (0.0225) H11B 0.9121 (0.0241) 104.14 (1.81) O11 - H11A Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.940(19) 1.95(2) 2.8925(14) 177.3(16) N1-H1...O11 0.889(18) 2.110(18) 2.9383(15) 154.7(15) N4-H4A...O2_$1 0.93(2) 2.11(2) 2.9574(14) 150.9(17) N4-H4B...O11_$1 0.91(2) 1.93(2) 2.8128(14) 162.2(18) O11-H11A...O1_$2 0.91(2) 1.98(2) 2.8534(14) 160(2) O11-H11B...N2_$3 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)