+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007may0018 started at 11:15:10 on 05-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007may0018 in Pna2(1) CELL 0.71073 9.8821 10.9251 7.1627 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0005 0.0003 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 UNIT 36 40 8 V = 773.31 F(000) = 312.0 Mu = 0.08 mm-1 Cell Wt = 584.76 Rho = 1.256 MERG 4 OMIT -3.00 55.00 OMIT 2 2 0 OMIT 1 1 1 OMIT 1 1 -1 FMAP 2 PLAN 5 DFIX 0.88 0.02 N2 H1N N2 H2N ACTA BOND $H L.S. 6 SIZE 0.3 0.1 0.1 TEMP -153.00 WGHT 0.079000 0.100800 EXTI 0.111234 FVAR 1.59540 C1 1 0.165421 1.067134 0.347815 11.00000 0.02797 0.03487 = 0.03359 0.00893 0.00546 0.00659 AFIX 43 H1 2 0.094602 1.123792 0.323806 11.00000 -1.20000 AFIX 0 C2 1 0.230613 1.053656 0.516127 11.00000 0.03831 0.03237 = 0.02840 0.00303 0.00654 0.01143 AFIX 43 H2 2 0.213175 1.098257 0.627412 11.00000 -1.20000 AFIX 0 C3 1 0.330069 0.959287 0.491488 11.00000 0.02487 0.02189 = 0.02591 0.00135 0.00298 0.00015 C4 1 0.425122 0.903674 0.610369 11.00000 0.02798 0.02341 = 0.02981 0.00064 -0.00150 -0.00143 AFIX 43 H4 2 0.432990 0.928954 0.736807 11.00000 -1.20000 AFIX 0 C5 1 0.507221 0.811474 0.540716 11.00000 0.02168 0.02005 = 0.04407 0.00313 -0.00021 -0.00313 C6 1 0.496094 0.775284 0.352536 11.00000 0.02897 0.02114 = 0.05014 -0.00400 0.00864 0.00075 AFIX 43 H6 2 0.553625 0.712427 0.306717 11.00000 -1.20000 AFIX 0 C7 1 0.403948 0.828653 0.233118 11.00000 0.03357 0.02387 = 0.03383 -0.00642 0.00582 -0.00565 AFIX 43 H7 2 0.397888 0.804055 0.106178 11.00000 -1.20000 AFIX 0 C8 1 0.319888 0.919917 0.304576 11.00000 0.02133 0.02236 = 0.02794 0.00052 0.00051 -0.00523 C9 1 0.184091 0.983565 0.022548 11.00000 0.04319 0.05208 = 0.02938 0.00136 -0.00795 -0.00638 AFIX 137 H9A 2 0.099015 1.027594 0.001754 11.00000 -1.50000 H9B 2 0.173932 0.898372 -0.017925 11.00000 -1.50000 H9C 2 0.256575 1.022652 -0.049318 11.00000 -1.50000 AFIX 0 N1 3 0.217756 0.986638 0.219546 11.00000 0.02514 0.03166 = 0.02742 0.00437 -0.00160 -0.00270 N2 3 0.597138 0.749371 0.661728 11.00000 0.02655 0.03140 = 0.06134 0.00989 -0.00458 0.00201 H1N 2 0.634298 0.801542 0.751610 11.00000 -1.20000 H2N 2 0.668417 0.716273 0.603402 11.00000 -1.20000 HKLF 4 1.0 0.00 1.00 0.00 0.00 0.00 1.00 1.00 0.00 0.00 Covalent radii and connectivity table for 2007may0018 in Pna2(1) C 0.770 H 0.320 N 0.700 C1 - N1 C2 C2 - C1 C3 C3 - C4 C8 C2 C4 - C5 C3 C5 - C4 C6 N2 C6 - C7 C5 C7 - C6 C8 C8 - N1 C7 C3 C9 - N1 N1 - C1 C8 C9 N2 - C5 Floating origin restraints generated 7817 Reflections read, of which 430 rejected -11 =< h =< 12, -14 =< k =< 14, -9 =< l =< 8, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 959 Unique reflections, of which 0 suppressed R(int) = 0.0445 R(sigma) = 0.0301 Friedel opposites merged Maximum memory for data reduction = 1252 / 9468 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 = 1543 / 138451 wR2 = 0.1032 before cycle 1 for 959 data and 108 / 108 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 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.934; Restrained GooF = 0.936 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0790 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.59249 0.00767 -0.380 OSF 2 0.11187 0.01951 0.032 EXTI Mean shift/esd = 0.183 Maximum = -0.610 for U33 C9 Max. shift = 0.013 A for H1N Max. dU = 0.000 for C9 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1543 / 138451 wR2 = 0.1028 before cycle 2 for 959 data and 108 / 108 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 0.033 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.931; Restrained GooF = 0.932 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0790 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.59117 0.00762 -0.173 OSF 2 0.11183 0.01947 -0.002 EXTI Mean shift/esd = 0.063 Maximum = 0.221 for y H2N Max. shift = 0.005 A for H2N Max. dU = 0.000 for N2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1543 / 138451 wR2 = 0.1028 before cycle 3 for 959 data and 108 / 108 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 0.031 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.931; Restrained GooF = 0.931 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0790 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.59108 0.00761 -0.012 OSF 2 0.11170 0.01947 -0.007 EXTI Mean shift/esd = 0.005 Maximum = 0.052 for y H2N Max. shift = 0.001 A for H2N Max. dU = 0.000 for C3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1543 / 138451 wR2 = 0.1028 before cycle 4 for 959 data and 108 / 108 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 0.031 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.931; Restrained GooF = 0.932 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0790 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.59107 0.00761 -0.001 OSF 2 0.11168 0.01946 -0.001 EXTI Mean shift/esd = 0.001 Maximum = 0.010 for y H2N Max. shift = 0.000 A for H2N Max. dU = 0.000 for C8 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1543 / 138451 wR2 = 0.1028 before cycle 5 for 959 data and 108 / 108 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 0.031 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.931; Restrained GooF = 0.932 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0790 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.59107 0.00761 0.000 OSF 2 0.11168 0.01946 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.003 for y H2N Max. shift = 0.000 A for H2N Max. dU = 0.000 for C9 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1543 / 138451 wR2 = 0.1028 before cycle 6 for 959 data and 108 / 108 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 0.031 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.931; Restrained GooF = 0.931 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0790 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.59107 0.00761 0.000 OSF 2 0.11168 0.01946 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for y H2N Max. shift = 0.000 A for H2N Max. dU = 0.000 for N2 Largest correlation matrix elements 0.561 EXTI / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.0945 1.1237 0.3237 43 0.950 0.000 C1 N1 C2 H2 0.2132 1.0985 0.6275 43 0.950 0.000 C2 C1 C3 H4 0.4331 0.9292 0.7367 43 0.950 0.000 C4 C5 C3 H6 0.5538 0.7125 0.3067 43 0.950 0.000 C6 C7 C5 H7 0.3980 0.8040 0.1062 43 0.950 0.000 C7 C6 C8 H9A 0.0989 1.0276 0.0017 137 0.980 0.000 C9 N1 H9A H9B 0.1740 0.8985 -0.0182 137 0.980 0.000 C9 N1 H9A H9C 0.2565 1.0229 -0.0494 137 0.980 0.000 C9 N1 H9A 2007may0018 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.16539 1.06711 0.34776 1.00000 0.02780 0.03451 0.03342 0.00877 0.00523 0.00606 0.03191 0.00390 0.00020 0.00019 0.00031 0.00000 0.00089 0.00097 0.00114 0.00086 0.00076 0.00075 0.00048 H1 0.09454 1.12372 0.32366 1.00000 0.03829 0.00000 0.00000 C2 0.23057 1.05379 0.51625 1.00000 0.03832 0.03200 0.02850 0.00316 0.00668 0.01198 0.03294 0.00394 0.00020 0.00017 0.00032 0.00000 0.00101 0.00095 0.00103 0.00084 0.00091 0.00078 0.00048 H2 0.21316 1.09847 0.62747 1.00000 0.03952 0.00000 0.00000 C3 0.33006 0.95926 0.49157 1.00000 0.02480 0.02157 0.02568 0.00110 0.00293 0.00007 0.02402 0.00324 0.00017 0.00015 0.00029 0.00000 0.00083 0.00080 0.00094 0.00069 0.00073 0.00061 0.00041 C4 0.42511 0.90376 0.61030 1.00000 0.02771 0.02322 0.02963 0.00096 -0.00142 -0.00123 0.02685 0.00335 0.00018 0.00016 0.00030 0.00000 0.00087 0.00079 0.00099 0.00072 0.00078 0.00063 0.00042 H4 0.43309 0.92919 0.73666 1.00000 0.03222 0.00000 0.00000 C5 0.50716 0.81145 0.54084 1.00000 0.02141 0.02010 0.04381 0.00325 -0.00023 -0.00329 0.02844 0.00326 0.00017 0.00016 0.00032 0.00000 0.00080 0.00082 0.00131 0.00078 0.00074 0.00063 0.00049 C6 0.49618 0.77529 0.35251 1.00000 0.02841 0.02126 0.05007 -0.00424 0.00846 0.00074 0.03325 0.00372 0.00019 0.00017 0.00035 0.00000 0.00093 0.00085 0.00135 0.00082 0.00086 0.00071 0.00051 H6 0.55380 0.71250 0.30668 1.00000 0.03990 0.00000 0.00000 C7 0.40405 0.82862 0.23312 1.00000 0.03357 0.02373 0.03367 -0.00623 0.00589 -0.00569 0.03032 0.00329 0.00018 0.00017 0.00032 0.00000 0.00091 0.00080 0.00099 0.00078 0.00088 0.00068 0.00044 H7 0.39804 0.80398 0.10620 1.00000 0.03639 0.00000 0.00000 C8 0.31982 0.91999 0.30445 1.00000 0.02134 0.02200 0.02815 0.00033 0.00035 -0.00500 0.02383 0.00299 0.00016 0.00015 0.00028 0.00000 0.00075 0.00080 0.00098 0.00071 0.00076 0.00060 0.00041 C9 0.18407 0.98365 0.02244 1.00000 0.04329 0.05187 0.02840 0.00181 -0.00798 -0.00633 0.04119 0.00384 0.00024 0.00023 0.00030 0.00000 0.00113 0.00129 0.00122 0.00103 0.00101 0.00096 0.00055 H9A 0.09895 1.02762 0.00172 1.00000 0.06178 0.00000 0.00000 H9B 0.17400 0.89848 -0.01818 1.00000 0.06178 0.00000 0.00000 H9C 0.25651 1.02285 -0.04936 1.00000 0.06178 0.00000 0.00000 N1 0.21775 0.98661 0.21957 1.00000 0.02525 0.03130 0.02732 0.00451 -0.00159 -0.00288 0.02796 0.00268 0.00014 0.00014 0.00023 0.00000 0.00074 0.00082 0.00089 0.00071 0.00071 0.00058 0.00040 N2 0.59719 0.74934 0.66176 1.00000 0.02590 0.03130 0.06100 0.01024 -0.00443 0.00184 0.03940 0.00361 0.00016 0.00016 0.00036 0.00000 0.00078 0.00085 0.00121 0.00084 0.00082 0.00064 0.00047 H1N 0.63356 0.80166 0.74958 1.00000 0.04728 0.03076 0.00252 0.00215 0.00336 0.00000 0.00000 H2N 0.66876 0.71759 0.60377 1.00000 0.04728 0.04467 0.00204 0.00206 0.00382 0.00000 0.00000 Final Structure Factor Calculation for 2007may0018 in Pna2(1) Total number of l.s. parameters = 108 Maximum vector length = 511 Memory required = 1437 / 24024 wR2 = 0.1028 before cycle 7 for 959 data and 2 / 108 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 0.031 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.931; Restrained GooF = 0.932 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0790 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0371 for 886 Fo > 4sig(Fo) and 0.0414 for all 959 data wR2 = 0.1028, GooF = S = 0.931, Restrained GooF = 0.932 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 11.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0462 0.0253 0.0242 C1 0.0500 0.0266 0.0222 C2 0.0283 0.0226 0.0211 C3 0.0307 0.0270 0.0229 C4 0.0443 0.0239 0.0172 C5 0.0534 0.0263 0.0200 C6 0.0432 0.0277 0.0201 C7 0.0282 0.0267 0.0166 C8 0.0563 0.0423 0.0249 C9 0.0353 0.0245 0.0240 N1 0.0645 0.0301 0.0235 N2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.023 0.036 0.050 0.063 0.077 0.093 0.115 0.154 0.228 1.000 Number in group 98. 103. 92. 94. 100. 91. 95. 94. 96. 96. GooF 1.029 1.225 0.937 1.000 0.918 0.924 0.850 0.730 0.627 0.910 K 1.039 1.020 0.965 0.965 1.004 1.003 1.020 1.011 1.015 1.017 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.16 1.33 1.69 inf Number in group 96. 98. 95. 96. 95. 95. 97. 95. 97. 95. GooF 0.998 0.897 1.025 0.936 0.908 0.829 0.751 0.818 0.957 1.132 K 1.037 1.045 0.993 1.040 1.022 1.017 1.011 1.015 1.036 1.006 R1 0.100 0.074 0.076 0.051 0.041 0.034 0.026 0.027 0.031 0.035 Recommended weighting scheme: WGHT 0.0442 0.1199 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) 0 1 1 1279.46 1938.78 4.08 0.669 5.99 1 3 3 55.19 41.42 3.62 0.098 1.96 2 0 8 8.56 3.38 3.52 0.028 0.88 1 1 4 7.59 4.77 3.37 0.033 1.74 3 5 3 37.84 28.85 3.23 0.082 1.45 4 8 6 5.12 10.40 3.04 0.049 0.84 1 7 8 5.42 0.30 3.03 0.008 0.77 12 1 3 5.11 10.40 2.90 0.049 0.78 2 2 3 1.87 3.43 2.86 0.028 2.00 4 4 4 14.90 10.93 2.86 0.050 1.28 7 1 7 71.78 55.01 2.81 0.113 0.83 2 0 0 426.81 531.65 2.79 0.350 4.94 4 4 5 3.03 4.93 2.78 0.034 1.13 12 4 1 2.66 5.54 2.70 0.036 0.78 6 11 1 0.75 2.53 2.57 0.024 0.84 6 7 4 4.01 2.08 2.56 0.022 0.96 5 7 6 8.36 12.03 2.56 0.053 0.85 7 5 4 11.11 15.00 2.53 0.059 0.99 3 1 7 31.56 24.85 2.52 0.076 0.97 10 2 2 -0.35 0.64 2.52 0.012 0.94 2 6 3 2.42 4.01 2.52 0.030 1.39 7 11 1 10.19 6.33 2.45 0.038 0.81 0 6 2 92.18 76.43 2.44 0.133 1.62 0 12 0 89.02 70.57 2.41 0.128 0.91 2 5 0 -0.48 0.24 2.38 0.007 2.00 1 2 7 11.56 15.16 2.35 0.059 1.00 8 9 1 1.28 2.91 2.34 0.026 0.86 7 4 5 26.18 32.78 2.32 0.087 0.94 4 7 4 18.72 23.49 2.29 0.074 1.06 12 2 3 7.39 11.70 2.29 0.052 0.77 4 8 5 3.43 5.33 2.29 0.035 0.92 5 8 6 9.34 5.35 2.27 0.035 0.82 2 12 0 -1.27 0.45 2.27 0.010 0.90 2 10 5 1.47 0.24 2.27 0.007 0.86 1 1 2 172.21 204.31 2.25 0.217 3.22 4 5 8 14.18 4.59 2.24 0.033 0.79 4 5 4 5.27 7.32 2.22 0.041 1.21 6 4 6 0.28 1.32 2.19 0.017 0.91 0 0 2 363.87 437.47 2.17 0.318 3.58 2 0 9 51.73 34.02 2.14 0.089 0.79 5 2 3 21.18 17.14 2.14 0.063 1.47 7 10 0 15.83 20.55 2.10 0.069 0.86 1 7 3 35.71 29.76 2.10 0.083 1.30 3 4 0 1.33 0.42 2.06 0.010 2.10 2 2 7 0.04 0.82 2.03 0.014 0.99 9 9 1 8.53 11.49 2.02 0.052 0.81 2 11 4 21.84 27.02 2.02 0.079 0.86 0 9 7 60.72 49.10 2.01 0.107 0.78 3 5 2 0.61 1.32 1.99 0.017 1.62 5 10 4 3.88 2.00 1.97 0.021 0.84 Bond lengths and angles C1 - Distance Angles N1 1.3727 (0.0027) C2 1.3757 (0.0032) 110.03 (0.16) H1 0.9500 124.99 124.99 C1 - N1 C2 C2 - Distance Angles C1 1.3757 (0.0032) C3 1.4368 (0.0024) 106.77 (0.19) H2 0.9500 126.62 126.62 C2 - C1 C3 C3 - Distance Angles C4 1.4047 (0.0026) C8 1.4109 (0.0030) 119.46 (0.16) C2 1.4368 (0.0024) 133.89 (0.20) 106.64 (0.17) C3 - C4 C8 C4 - Distance Angles C5 1.3864 (0.0025) C3 1.4047 (0.0026) 119.19 (0.19) H4 0.9500 120.40 120.40 C4 - C5 C3 C5 - Distance Angles C4 1.3864 (0.0025) C6 1.4098 (0.0031) 120.15 (0.18) N2 1.4150 (0.0027) 119.79 (0.21) 119.98 (0.19) C5 - C4 C6 C6 - Distance Angles C7 1.3782 (0.0030) C5 1.4098 (0.0031) 121.74 (0.18) H6 0.9500 119.13 119.13 C6 - C7 C5 C7 - Distance Angles C6 1.3782 (0.0030) C8 1.3965 (0.0024) 117.97 (0.20) H7 0.9500 121.02 121.02 C7 - C6 C8 C8 - Distance Angles N1 1.3845 (0.0023) C7 1.3965 (0.0024) 130.50 (0.19) C3 1.4109 (0.0030) 108.03 (0.15) 121.47 (0.17) C8 - N1 C7 C9 - Distance Angles N1 1.4511 (0.0028) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - N1 H9A H9B N1 - Distance Angles C1 1.3727 (0.0027) C8 1.3845 (0.0023) 108.53 (0.16) C9 1.4511 (0.0028) 125.36 (0.19) 125.64 (0.18) N1 - C1 C8 N2 - Distance Angles C5 1.4150 (0.0027) H1N 0.9227 (0.0173) 111.42 (1.70) H2N 0.8905 (0.0170) 113.62 (1.85) 104.47 (2.24) N2 - C5 H1N FMAP and GRID set by program FMAP 2 1 14 GRID -2.273 -2 -2 2.273 2 2 R1 = 0.0414 for 959 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.17 at 0.0762 0.0976 0.2610 [ 0.56 A from H1 ] Deepest hole -0.13 at 0.1525 0.2490 0.0580 [ 1.72 A from C5 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 1553 / 14314 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0762 1.0976 0.2610 1.00000 0.05 0.17 0.56 H1 1.13 C1 1.87 N1 2.02 H9A Q2 1 0.1641 1.0414 0.4463 1.00000 0.05 0.15 0.76 C1 0.84 C2 1.43 H1 1.52 H2 Q3 1 0.3466 0.8263 0.0218 1.00000 0.05 0.13 0.83 H7 1.62 C7 1.90 H9B 2.28 C8 Q4 1 0.5846 0.7370 0.8221 1.00000 0.05 0.13 1.00 H1N 1.16 N2 1.78 H2N 2.07 H9B Q5 1 0.0849 0.9286 0.1417 1.00000 0.05 0.12 1.43 C9 1.48 H9B 1.48 H9A 1.56 N1 Shortest distances between peaks (including symmetry equivalents) 1 2 1.70 1 5 2.04 1 4 2.24 2 5 2.62 2 5 2.85 4 5 2.92 3 4 2.92 3 5 2.95 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: Generate connectivity array 0.01: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.01: Analyse other restraints etc. 0.40: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.41: Structure factors and derivatives 0.38: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.05: Solve l.s. equations 0.00: Generate HTAB table 0.01: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007may0018 finished at 11:15:20 Total CPU time: 1.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++