+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src1282 started at 16:46:43 on 13-Jan-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src1282 in P2(1)/c CELL 0.71073 9.2292 5.7759 19.7467 90.000 102.396 90.000 ZERR 4.00 0.0005 0.0003 0.0012 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 44 60 12 4 V = 1028.10 F(000) = 440.0 Mu = 0.09 mm-1 Cell Wt = 821.04 Rho = 1.326 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.11 0.07 0.01 ACTA BOND $H WGHT 0.00000 2.06970 L.S. 4 TEMP -153.00 FVAR 0.51778 MOLE 1 C2 1 0.099768 0.413378 0.136412 11.00000 0.02702 0.03474 = 0.03106 -0.00607 0.00577 -0.00133 AFIX 43 H2 2 0.098239 0.281439 0.107542 11.00000 -1.20000 AFIX 0 C3 1 -0.010784 0.576605 0.116590 11.00000 0.02391 0.03647 = 0.02825 0.00570 0.00570 -0.00229 AFIX 43 H3 2 -0.085753 0.559448 0.075629 11.00000 -1.20000 AFIX 0 C4 1 -0.006045 0.767000 0.159927 11.00000 0.02474 0.02806 = 0.03730 0.01043 0.00980 0.00446 AFIX 43 H4 2 -0.080094 0.883404 0.148943 11.00000 -1.20000 AFIX 0 C5 1 0.104224 0.789072 0.218394 11.00000 0.02535 0.02441 = 0.03263 0.00326 0.01168 0.00137 AFIX 43 H5 2 0.106888 0.919072 0.248108 11.00000 -1.20000 AFIX 0 C6 1 0.213105 0.615855 0.233495 11.00000 0.02236 0.02226 = 0.02490 0.00201 0.01024 -0.00090 C8 1 0.331772 0.795993 0.344752 11.00000 0.02394 0.02122 = 0.03073 -0.00452 0.00691 0.00044 AFIX 23 H8A 2 0.273353 0.729524 0.376631 11.00000 -1.20000 H8B 2 0.282636 0.940856 0.325159 11.00000 -1.20000 AFIX 0 C9 1 0.488149 0.850140 0.384895 11.00000 0.02800 0.02030 = 0.03512 -0.00369 0.00823 0.00080 AFIX 23 H9A 2 0.540587 0.941427 0.355120 11.00000 -1.20000 H9B 2 0.482510 0.945486 0.425912 11.00000 -1.20000 AFIX 0 C11 1 0.572577 0.475821 0.351455 11.00000 0.02768 0.02009 = 0.02318 -0.00339 0.00523 0.00461 AFIX 23 H11A 2 0.623587 0.331735 0.370541 11.00000 -1.20000 H11B 2 0.627757 0.542831 0.318328 11.00000 -1.20000 AFIX 0 C12 1 0.415720 0.419872 0.313928 11.00000 0.02807 0.01661 = 0.02709 -0.00356 0.00558 0.00208 AFIX 23 H12A 2 0.418175 0.316203 0.274265 11.00000 -1.20000 H12B 2 0.363648 0.338039 0.345792 11.00000 -1.20000 AFIX 0 C13 1 0.663059 0.628355 0.471210 11.00000 0.02514 0.03187 = 0.02793 -0.00424 0.00674 -0.00580 C14 1 0.761149 0.416236 0.487069 11.00000 0.03444 0.03674 = 0.02697 0.00073 0.00101 0.00473 AFIX 137 H14A 2 0.828347 0.434766 0.532446 11.00000 -1.50000 H14B 2 0.819323 0.398007 0.451319 11.00000 -1.50000 H14C 2 0.699205 0.278775 0.487695 11.00000 -1.50000 AFIX 0 N1 3 0.208565 0.427139 0.193083 11.00000 0.02305 0.02622 = 0.03232 -0.00447 0.00530 0.00087 N7 3 0.335070 0.632450 0.288778 11.00000 0.02395 0.01737 = 0.02825 -0.00016 0.00388 0.00359 N10 3 0.572423 0.639538 0.407616 11.00000 0.02708 0.02115 = 0.02811 -0.00255 0.00582 0.00030 O15 4 0.666715 0.780691 0.514762 11.00000 0.03740 0.04782 = 0.03425 -0.01932 0.00303 0.00216 HKLF 4 Covalent radii and connectivity table for 2008src1282 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C2 - N1 C3 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - N1 N7 C5 C8 - N7 C9 C9 - N10 C8 C11 - N10 C12 C12 - N7 C11 C13 - O15 N10 C14 C14 - C13 N1 - C2 C6 N7 - C6 C8 C12 N10 - C13 C11 C9 O15 - C13 10725 Reflections read, of which 664 rejected -11 =< h =< 11, -7 =< k =< 7, -22 =< l =< 25, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 2349 Unique reflections, of which 0 suppressed R(int) = 0.0687 R(sigma) = 0.0694 Friedel opposites merged Maximum memory for data reduction = 1622 / 23426 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 = 2029 / 172736 wR2 = 0.1620 before cycle 1 for 2349 data and 137 / 137 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.51790 0.00151 0.081 OSF Mean shift/su = 0.031 Maximum = 0.108 for U33 C13 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C14 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2029 / 172736 wR2 = 0.1620 before cycle 2 for 2349 data and 137 / 137 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.51794 0.00151 0.028 OSF Mean shift/su = 0.012 Maximum = 0.044 for U33 C13 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C13 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2029 / 172736 wR2 = 0.1620 before cycle 3 for 2349 data and 137 / 137 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.51795 0.00151 0.003 OSF Mean shift/su = 0.001 Maximum = 0.005 for U33 C14 Max. shift = 0.000 A for H14B Max. dU = 0.000 for C14 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2029 / 172736 wR2 = 0.1620 before cycle 4 for 2349 data and 137 / 137 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.51795 0.00151 0.001 OSF Mean shift/su = 0.000 Maximum = 0.001 for U12 C3 Max. shift = 0.000 A for H14B Max. dU = 0.000 for C2 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.0982 0.2814 0.1075 43 0.950 0.000 C2 N1 C3 H3 -0.0857 0.5595 0.0756 43 0.950 0.000 C3 C2 C4 H4 -0.0801 0.8833 0.1489 43 0.950 0.000 C4 C5 C3 H5 0.1069 0.9191 0.2481 43 0.950 0.000 C5 C4 C6 H8A 0.2734 0.7295 0.3766 23 0.990 0.000 C8 N7 C9 H8B 0.2827 0.9408 0.3252 23 0.990 0.000 C8 N7 C9 H9A 0.5406 0.9414 0.3551 23 0.990 0.000 C9 N10 C8 H9B 0.4825 0.9455 0.4259 23 0.990 0.000 C9 N10 C8 H11A 0.6236 0.3317 0.3705 23 0.990 0.000 C11 N10 C12 H11B 0.6277 0.5429 0.3183 23 0.990 0.000 C11 N10 C12 H12A 0.4182 0.3162 0.2743 23 0.990 0.000 C12 N7 C11 H12B 0.3636 0.3380 0.3458 23 0.990 0.000 C12 N7 C11 H14A 0.8283 0.4348 0.5325 137 0.980 0.000 C14 C13 H14A H14B 0.8193 0.3980 0.4513 137 0.980 0.000 C14 C13 H14A H14C 0.6992 0.2788 0.4877 137 0.980 0.000 C14 C13 H14A 2008src1282 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 0.09974 0.41340 0.13641 1.00000 0.02708 0.03470 0.03126 -0.00610 0.00581 -0.00129 0.03108 0.00591 0.00032 0.00058 0.00017 0.00000 0.00158 0.00180 0.00183 0.00147 0.00135 0.00137 0.00074 H2 0.09819 0.28144 0.10755 1.00000 0.03729 0.00000 0.00000 C3 -0.01079 0.57662 0.11659 1.00000 0.02386 0.03660 0.02827 0.00571 0.00567 -0.00235 0.02957 0.00609 0.00033 0.00056 0.00017 0.00000 0.00151 0.00181 0.00176 0.00145 0.00127 0.00134 0.00072 H3 -0.08574 0.55949 0.07562 1.00000 0.03548 0.00000 0.00000 C4 -0.00605 0.76694 0.15992 1.00000 0.02469 0.02805 0.03721 0.01039 0.00976 0.00456 0.02952 0.00614 0.00033 0.00056 0.00017 0.00000 0.00154 0.00171 0.00192 0.00146 0.00134 0.00127 0.00073 H4 -0.08011 0.88332 0.14895 1.00000 0.03542 0.00000 0.00000 C5 0.10422 0.78907 0.21839 1.00000 0.02546 0.02423 0.03277 0.00327 0.01162 0.00146 0.02668 0.00599 0.00031 0.00053 0.00017 0.00000 0.00151 0.00158 0.00181 0.00134 0.00131 0.00123 0.00069 H5 0.10688 0.91909 0.24810 1.00000 0.03201 0.00000 0.00000 C6 0.21309 0.61586 0.23349 1.00000 0.02230 0.02225 0.02513 0.00214 0.01029 -0.00100 0.02245 0.00548 0.00030 0.00050 0.00015 0.00000 0.00139 0.00150 0.00162 0.00125 0.00118 0.00115 0.00063 C8 0.33179 0.79598 0.34475 1.00000 0.02403 0.02125 0.03074 -0.00449 0.00705 0.00044 0.02517 0.00531 0.00031 0.00051 0.00016 0.00000 0.00148 0.00154 0.00177 0.00127 0.00125 0.00118 0.00068 H8A 0.27338 0.72951 0.37663 1.00000 0.03020 0.00000 0.00000 H8B 0.28265 0.94084 0.32516 1.00000 0.03020 0.00000 0.00000 C9 0.48816 0.85014 0.38489 1.00000 0.02803 0.02031 0.03508 -0.00380 0.00820 0.00082 0.02759 0.00570 0.00032 0.00051 0.00017 0.00000 0.00155 0.00149 0.00186 0.00134 0.00134 0.00123 0.00070 H9A 0.54060 0.94139 0.35511 1.00000 0.03311 0.00000 0.00000 H9B 0.48252 0.94551 0.42590 1.00000 0.03311 0.00000 0.00000 C11 0.57254 0.47582 0.35144 1.00000 0.02780 0.02013 0.02308 -0.00323 0.00524 0.00464 0.02370 0.00531 0.00031 0.00050 0.00015 0.00000 0.00151 0.00149 0.00158 0.00125 0.00121 0.00119 0.00064 H11A 0.62357 0.33174 0.37051 1.00000 0.02844 0.00000 0.00000 H11B 0.62770 0.54287 0.31831 1.00000 0.02844 0.00000 0.00000 C12 0.41571 0.41986 0.31393 1.00000 0.02823 0.01664 0.02699 -0.00345 0.00556 0.00205 0.02401 0.00543 0.00031 0.00049 0.00016 0.00000 0.00151 0.00143 0.00167 0.00123 0.00124 0.00116 0.00065 H12A 0.41816 0.31617 0.27427 1.00000 0.02881 0.00000 0.00000 H12B 0.36364 0.33804 0.34580 1.00000 0.02881 0.00000 0.00000 C13 0.66305 0.62834 0.47121 1.00000 0.02507 0.03193 0.02821 -0.00423 0.00684 -0.00582 0.02823 0.00568 0.00032 0.00056 0.00016 0.00000 0.00152 0.00176 0.00176 0.00144 0.00127 0.00129 0.00070 C14 0.76114 0.41623 0.48707 1.00000 0.03456 0.03689 0.02698 0.00060 0.00114 0.00464 0.03363 0.00616 0.00035 0.00058 0.00017 0.00000 0.00173 0.00189 0.00179 0.00149 0.00139 0.00146 0.00077 H14A 0.82833 0.43477 0.53245 1.00000 0.05045 0.00000 0.00000 H14B 0.81932 0.39799 0.45133 1.00000 0.05045 0.00000 0.00000 H14C 0.69919 0.27877 0.48770 1.00000 0.05045 0.00000 0.00000 N1 0.20858 0.42714 0.19309 1.00000 0.02311 0.02628 0.03218 -0.00452 0.00524 0.00079 0.02730 0.00469 0.00026 0.00044 0.00014 0.00000 0.00126 0.00138 0.00150 0.00115 0.00108 0.00107 0.00060 N7 0.33507 0.63246 0.28877 1.00000 0.02397 0.01742 0.02831 -0.00019 0.00396 0.00358 0.02348 0.00452 0.00025 0.00040 0.00013 0.00000 0.00124 0.00124 0.00144 0.00107 0.00104 0.00098 0.00056 N10 0.57241 0.63950 0.40762 1.00000 0.02705 0.02115 0.02807 -0.00260 0.00574 0.00037 0.02545 0.00455 0.00026 0.00042 0.00013 0.00000 0.00128 0.00129 0.00148 0.00110 0.00108 0.00104 0.00058 O15 0.66673 0.78070 0.51476 1.00000 0.03756 0.04769 0.03425 -0.01934 0.00308 0.00207 0.04053 0.00416 0.00025 0.00043 0.00012 0.00000 0.00133 0.00150 0.00141 0.00120 0.00106 0.00111 0.00064 Final Structure Factor Calculation for 2008src1282 in P2(1)/c Total number of l.s. parameters = 137 Maximum vector length = 511 Memory required = 1892 / 22995 wR2 = 0.1620 before cycle 5 for 2349 data and 0 / 137 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0827 for 1518 Fo > 4sig(Fo) and 0.1355 for all 2349 data wR2 = 0.1620, GooF = S = 1.107, Restrained GooF = 1.107 for all data Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 15.00 for hydrogen atoms Principal mean square atomic displacements U 0.0393 0.0277 0.0262 C2 0.0402 0.0259 0.0225 C3 0.0444 0.0234 0.0208 C4 0.0356 0.0234 0.0210 C5 0.0284 0.0230 0.0160 C6 0.0325 0.0240 0.0190 C8 0.0360 0.0278 0.0190 C9 0.0309 0.0242 0.0160 C11 0.0296 0.0273 0.0151 C12 0.0365 0.0264 0.0217 C13 0.0422 0.0341 0.0246 C14 0.0351 0.0243 0.0225 N1 0.0296 0.0250 0.0158 N7 0.0291 0.0270 0.0202 N10 0.0639 0.0372 0.0205 O15 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.005 0.010 0.014 0.020 0.025 0.032 0.042 0.056 0.083 1.000 Number in group 270. 243. 204. 254. 212. 248. 216. 233. 233. 236. GooF 1.255 1.087 1.157 1.204 1.186 1.034 1.137 1.024 0.973 0.956 K 12.185 1.867 1.345 1.212 1.120 1.050 1.013 0.999 0.991 0.992 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.14 1.32 1.65 inf Number in group 238. 233. 238. 231. 237. 233. 235. 237. 230. 237. GooF 1.306 1.217 1.224 1.134 1.117 1.140 1.067 0.907 0.927 0.950 K 1.216 1.162 1.105 1.031 1.041 1.001 0.981 1.003 1.018 0.984 R1 0.337 0.298 0.254 0.186 0.196 0.133 0.090 0.073 0.071 0.035 Recommended weighting scheme: WGHT 0.0000 2.0505 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)/su Fc/Fc(max) Resolution(A) -2 5 8 39.23 0.66 4.24 0.004 1.04 -6 0 12 35.72 0.08 3.75 0.001 1.24 -9 4 2 55.72 8.12 3.55 0.014 0.83 6 4 1 70.93 135.46 3.51 0.059 1.03 -3 6 15 81.56 9.73 3.34 0.016 0.77 -8 4 3 28.59 84.17 3.34 0.047 0.90 -4 3 17 42.27 0.00 3.32 0.000 0.96 2 6 8 80.73 26.33 3.19 0.026 0.86 -3 3 9 24.96 1.04 3.04 0.005 1.37 2 6 6 15.73 0.01 2.87 0.000 0.89 -11 2 3 37.84 0.20 2.85 0.002 0.80 -5 6 9 57.55 0.93 2.84 0.005 0.82 5 2 13 30.04 2.01 2.83 0.007 0.98 9 1 7 52.51 15.86 2.82 0.020 0.87 -6 3 20 31.02 0.32 2.81 0.003 0.82 1 4 18 59.78 118.74 2.80 0.055 0.84 -4 3 21 0.41 42.90 2.77 0.033 0.83 0 4 15 29.67 5.12 2.74 0.011 0.96 2 2 16 77.47 35.55 2.72 0.030 1.03 -6 3 21 28.89 0.00 2.70 0.000 0.79 5 0 12 145.80 237.68 2.69 0.078 1.09 3 4 18 42.79 3.99 2.67 0.010 0.79 -3 5 15 56.06 21.28 2.65 0.023 0.86 -5 3 13 53.23 93.91 2.64 0.049 1.07 1 0 22 -8.78 25.89 2.61 0.026 0.86 -7 2 15 20.34 0.00 2.61 0.000 0.97 -4 5 17 35.52 0.15 2.61 0.002 0.80 3 6 12 6.12 40.00 2.60 0.032 0.77 -2 4 19 29.80 0.75 2.56 0.004 0.84 -10 3 14 5.44 41.15 2.54 0.033 0.77 -9 3 14 26.19 0.07 2.50 0.001 0.82 0 4 21 30.12 0.01 2.50 0.000 0.77 -7 5 4 60.45 19.63 2.50 0.022 0.87 -10 1 5 -11.02 10.92 2.46 0.017 0.91 7 5 7 15.79 45.55 2.44 0.034 0.79 -9 4 13 37.63 12.13 2.44 0.018 0.78 6 4 0 10.79 0.03 2.44 0.001 1.04 7 3 8 29.36 5.22 2.43 0.012 0.92 4 6 8 20.08 0.01 2.42 0.000 0.81 6 6 3 78.80 6.67 2.41 0.013 0.79 -1 3 22 24.65 0.67 2.40 0.004 0.81 -6 0 14 181.42 111.26 2.40 0.053 1.15 1 7 8 -15.51 13.16 2.39 0.018 0.77 -11 2 10 63.03 24.07 2.38 0.025 0.79 5 3 15 25.43 5.00 2.38 0.011 0.86 -7 1 22 47.32 14.79 2.36 0.019 0.80 1 1 24 29.60 2.79 2.35 0.008 0.78 1 6 13 21.23 0.63 2.35 0.004 0.80 -8 3 13 15.08 44.56 2.35 0.034 0.89 -1 0 4 139.16 194.80 2.35 0.071 4.69 Bond lengths and angles C2 - Distance Angles N1 1.3361 (0.0038) C3 1.3824 (0.0043) 124.96 (0.31) H2 0.9500 117.52 117.52 C2 - N1 C3 C3 - Distance Angles C2 1.3824 (0.0043) C4 1.3881 (0.0046) 116.22 (0.30) H3 0.9500 121.89 121.89 C3 - C2 C4 C4 - Distance Angles C5 1.3712 (0.0043) C3 1.3881 (0.0046) 120.82 (0.29) H4 0.9500 119.59 119.59 C4 - C5 C3 C5 - Distance Angles C4 1.3712 (0.0043) C6 1.4039 (0.0040) 118.71 (0.30) H5 0.9500 120.64 120.64 C5 - C4 C6 C6 - Distance Angles N1 1.3461 (0.0038) N7 1.3930 (0.0036) 115.92 (0.25) C5 1.4039 (0.0040) 121.43 (0.27) 122.59 (0.27) C6 - N1 N7 C8 - Distance Angles N7 1.4591 (0.0036) C9 1.5224 (0.0040) 110.85 (0.23) H8A 0.9900 109.47 109.47 H8B 0.9900 109.47 109.47 108.05 C8 - N7 C9 H8A C9 - Distance Angles N10 1.4617 (0.0037) C8 1.5224 (0.0040) 111.79 (0.24) H9A 0.9900 109.26 109.26 H9B 0.9900 109.26 109.26 107.93 C9 - N10 C8 H9A C11 - Distance Angles N10 1.4577 (0.0036) C12 1.5126 (0.0038) 110.75 (0.23) H11A 0.9900 109.49 109.49 H11B 0.9900 109.49 109.49 108.07 C11 - N10 C12 H11A C12 - Distance Angles N7 1.4662 (0.0035) C11 1.5126 (0.0038) 110.47 (0.23) H12A 0.9900 109.56 109.56 H12B 0.9900 109.56 109.56 108.10 C12 - N7 C11 H12A C13 - Distance Angles O15 1.2259 (0.0037) N10 1.3527 (0.0039) 122.38 (0.30) C14 1.5155 (0.0043) 120.66 (0.29) 116.96 (0.27) C13 - O15 N10 C14 - Distance Angles C13 1.5155 (0.0043) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - C13 H14A H14B N1 - Distance Angles C2 1.3361 (0.0038) C6 1.3461 (0.0038) 117.81 (0.26) N1 - C2 N7 - Distance Angles C6 1.3930 (0.0036) C8 1.4591 (0.0036) 119.57 (0.23) C12 1.4662 (0.0035) 118.29 (0.23) 112.15 (0.23) N7 - C6 C8 N10 - Distance Angles C13 1.3527 (0.0039) C11 1.4577 (0.0036) 125.04 (0.25) C9 1.4617 (0.0037) 120.46 (0.26) 113.17 (0.24) N10 - C13 C11 O15 - Distance Angles C13 1.2259 (0.0037) O15 - FMAP and GRID set by program FMAP 2 1 24 GRID -2.381 -2 -1 2.381 2 1 R1 = 0.1353 for 2349 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.28 at 0.4770 0.7991 0.0256 [ 1.60 A from H14C ] Deepest hole -0.26 at 0.1684 0.3360 0.1512 [ 0.78 A from C2 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2039 / 22533 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5230 0.2991 0.4744 1.00000 0.05 0.28 1.60 H14C 1.87 O15 2.25 C13 2.25 H9B Q2 1 0.5214 0.7401 0.4010 1.00000 0.05 0.25 0.74 N10 0.75 C9 1.36 H9B 1.51 H9A Q3 1 0.5505 0.4024 0.2393 1.00000 0.05 0.24 1.61 H12A 1.77 H11B 1.89 H9A 2.03 N7 Q4 1 0.0744 0.7807 0.1788 1.00000 0.05 0.24 0.76 C4 0.77 C5 1.54 H4 1.56 H5 Q5 1 0.3040 0.6486 0.4315 1.00000 0.05 0.23 1.16 H8A 1.61 H14A 1.66 H14C 1.87 C14 Q6 1 0.5245 1.0632 0.3096 1.00000 0.05 0.22 1.13 H9A 1.81 H12A 2.01 C9 2.05 H11A Q7 1 0.4735 0.4626 0.4498 1.00000 0.05 0.22 1.70 N10 1.96 C13 2.13 O15 2.21 H12B Q8 1 0.0981 1.0716 0.1724 1.00000 0.05 0.22 1.72 H5 1.76 H2 1.86 C5 1.94 H4 Q9 1 0.5919 0.1085 0.4782 1.00000 0.05 0.21 1.38 H14C 1.59 H9B 2.09 O15 2.17 H9B Q10 1 -0.0005 0.6101 0.0585 1.00000 0.05 0.21 0.97 H3 1.19 C3 1.98 C2 2.21 C4 Shortest distances between peaks (including symmetry equivalents) 1 7 1.11 1 9 1.27 3 6 1.41 4 8 1.70 5 7 1.87 2 7 1.97 7 7 1.99 1 7 2.03 1 5 2.20 2 5 2.28 5 9 2.31 7 9 2.33 9 9 2.41 3 6 2.44 4 10 2.53 1 2 2.59 2 6 2.60 1 1 2.60 2 9 2.62 10 10 2.64 1 9 2.82 5 7 2.84 1 5 2.85 2 3 2.86 1 2 2.93 2 9 2.94 7 9 2.98 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: 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 0.00: Analyse other restraints etc. 0.52: Read intensity data, sort/merge etc. 0.02: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.42: Structure factors and derivatives 0.30: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src1282 finished at 16:46:44 Total CPU time: 1.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++