+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007jmw0010 started at 13:20:58 on 05-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007jmw0010 in P2(1) CELL 0.71073 8.1461 5.9730 9.5815 90.000 100.940 90.000 ZERR 2.00 0.0003 0.0002 0.0003 0.000 0.002 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O UNIT 20 24 4 4 V = 457.73 F(000) = 204.0 Mu = 0.10 mm-1 Cell Wt = 384.43 Rho = 1.395 MERG 4 OMIT -3.00 55.00 FMAP 2 PLAN 5 ACTA SIZE 0.3 0.1 0.01 BOND $H L.S. 6 TEMP -153.00 WGHT 0.030700 0.135900 FVAR 2.65517 O1 4 0.104753 0.874664 0.425809 11.00000 0.01925 0.02432 = 0.02856 -0.00114 0.00732 -0.00257 O2 4 0.991686 1.214207 0.154501 11.00000 0.02621 0.03772 = 0.03180 0.00528 0.01333 -0.00282 N1 3 0.398826 0.814741 0.308636 11.00000 0.01929 0.01706 = 0.02303 -0.00341 0.00467 -0.00320 N2 3 0.639830 0.975521 0.257595 11.00000 0.01855 0.02082 = 0.01885 -0.00030 0.00443 0.00061 C1 1 0.253421 0.998522 0.478127 11.00000 0.02108 0.02379 = 0.02748 -0.00504 0.00768 -0.00405 AFIX 23 H1A 2 0.320009 0.918117 0.560103 11.00000 -1.20000 H1B 2 0.222745 1.146479 0.512073 11.00000 -1.20000 AFIX 0 C2 1 0.359221 1.032201 0.365883 11.00000 0.02174 0.01868 = 0.02895 -0.00338 0.00770 -0.00212 AFIX 23 H2A 2 0.297890 1.126361 0.288095 11.00000 -1.20000 H2B 2 0.464050 1.110499 0.408025 11.00000 -1.20000 AFIX 0 C3 1 0.248966 0.679217 0.260483 11.00000 0.02384 0.02236 = 0.02570 -0.00252 0.00563 -0.00624 AFIX 23 H3A 2 0.281809 0.527837 0.233862 11.00000 -1.20000 H3B 2 0.179904 0.748990 0.175443 11.00000 -1.20000 AFIX 0 C4 1 0.147906 0.660940 0.377705 11.00000 0.02426 0.02008 = 0.02929 0.00078 0.00645 -0.00475 AFIX 23 H4A 2 0.044389 0.575271 0.342105 11.00000 -1.20000 H4B 2 0.213524 0.577295 0.458697 11.00000 -1.20000 AFIX 0 C5 1 0.528445 0.808890 0.233129 11.00000 0.01716 0.02119 = 0.01662 0.00048 0.00119 0.00160 C6 1 0.768553 0.973345 0.187507 11.00000 0.01707 0.02705 = 0.01822 0.00261 0.00256 0.00099 C7 1 0.793664 0.810430 0.091678 11.00000 0.02040 0.03585 = 0.01695 -0.00061 0.00368 0.00664 AFIX 43 H7 2 0.884958 0.817736 0.043142 11.00000 -1.20000 AFIX 0 C8 1 0.679685 0.635441 0.069323 11.00000 0.02600 0.03041 = 0.02044 -0.00795 0.00102 0.00710 AFIX 43 H8 2 0.693569 0.517721 0.005906 11.00000 -1.20000 AFIX 0 C9 1 0.546235 0.632019 0.138983 11.00000 0.02150 0.02229 = 0.02458 -0.00382 0.00055 0.00042 AFIX 43 H9 2 0.467608 0.512865 0.123971 11.00000 -1.20000 AFIX 0 C10 1 0.885144 1.165107 0.221574 11.00000 0.02273 0.02609 = 0.02429 0.00228 0.00788 -0.00055 AFIX 43 H10 2 0.875481 1.255248 0.301305 11.00000 -1.20000 HKLF 4 Covalent radii and connectivity table for 2007jmw0010 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 O1 - C4 C1 O2 - C10 N1 - C5 C3 C2 N2 - C5 C6 C1 - O1 C2 C2 - N1 C1 C3 - N1 C4 C4 - O1 C3 C5 - N2 N1 C9 C6 - N2 C7 C10 C7 - C6 C8 C8 - C9 C7 C9 - C8 C5 C10 - O2 C6 Floating origin restraints generated 6441 Reflections read, of which 11 rejected -10 =< h =< 10, -7 =< k =< 6, -12 =< l =< 11, Max. 2-theta = 54.95 0 Systematic absence violations 0 Inconsistent equivalents 1152 Unique reflections, of which 0 suppressed R(int) = 0.0285 R(sigma) = 0.0237 Friedel opposites merged Maximum memory for data reduction = 1451 / 11283 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 = 1818 / 161171 wR2 = 0.0802 before cycle 1 for 1152 data and 127 / 127 parameters GooF = S = 1.125; Restrained GooF = 1.124 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0307 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.64541 0.00661 -1.476 OSF Mean shift/esd = 0.086 Maximum = -1.476 for OSF Max. shift = 0.000 A for C4 Max. dU = 0.000 for O1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1818 / 161171 wR2 = 0.0801 before cycle 2 for 1152 data and 127 / 127 parameters GooF = S = 1.124; Restrained GooF = 1.123 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0307 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.64359 0.00659 -0.277 OSF Mean shift/esd = 0.027 Maximum = -0.277 for OSF Max. shift = 0.000 A for C4 Max. dU = 0.000 for O1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1818 / 161171 wR2 = 0.0801 before cycle 3 for 1152 data and 127 / 127 parameters GooF = S = 1.124; Restrained GooF = 1.123 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0307 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.64356 0.00659 -0.004 OSF Mean shift/esd = 0.001 Maximum = -0.004 for U33 O1 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1818 / 161171 wR2 = 0.0801 before cycle 4 for 1152 data and 127 / 127 parameters GooF = S = 1.124; Restrained GooF = 1.123 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0307 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.64356 0.00659 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.002 for z C9 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C10 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1818 / 161171 wR2 = 0.0801 before cycle 5 for 1152 data and 127 / 127 parameters GooF = S = 1.124; Restrained GooF = 1.123 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0307 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.64356 0.00659 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C10 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C7 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1818 / 161171 wR2 = 0.0801 before cycle 6 for 1152 data and 127 / 127 parameters GooF = S = 1.124; Restrained GooF = 1.123 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0307 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.64356 0.00659 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C9 Max. dU = 0.000 for C10 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.3200 0.9181 0.5601 23 0.990 0.000 C1 O1 C2 H1B 0.2228 1.1465 0.5121 23 0.990 0.000 C1 O1 C2 H2A 0.2979 1.1264 0.2881 23 0.990 0.000 C2 N1 C1 H2B 0.4641 1.1105 0.4080 23 0.990 0.000 C2 N1 C1 H3A 0.2818 0.5279 0.2338 23 0.990 0.000 C3 N1 C4 H3B 0.1799 0.7490 0.1754 23 0.990 0.000 C3 N1 C4 H4A 0.0444 0.5752 0.3422 23 0.990 0.000 C4 O1 C3 H4B 0.2136 0.5773 0.4587 23 0.990 0.000 C4 O1 C3 H7 0.8849 0.8178 0.0431 43 0.950 0.000 C7 C6 C8 H8 0.6936 0.5177 0.0059 43 0.950 0.000 C8 C9 C7 H9 0.4676 0.5129 0.1239 43 0.950 0.000 C9 C8 C5 H10 0.8755 1.2553 0.3013 43 0.950 0.000 C10 O2 C6 2007jmw0010 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O1 0.10475 0.87468 0.42582 1.00000 0.01902 0.02406 0.02837 -0.00114 0.00728 -0.00256 0.02345 0.00258 0.00016 0.00026 0.00014 0.00000 0.00061 0.00075 0.00069 0.00062 0.00051 0.00057 0.00033 O2 0.99169 1.21423 0.15448 1.00000 0.02601 0.03747 0.03159 0.00522 0.01329 -0.00284 0.03066 0.00294 0.00017 0.00031 0.00015 0.00000 0.00069 0.00092 0.00075 0.00071 0.00058 0.00069 0.00037 N1 0.39883 0.81474 0.30862 1.00000 0.01910 0.01686 0.02287 -0.00341 0.00465 -0.00320 0.01952 0.00282 0.00019 0.00028 0.00017 0.00000 0.00070 0.00078 0.00072 0.00065 0.00056 0.00065 0.00033 N2 0.63982 0.97552 0.25759 1.00000 0.01834 0.02063 0.01869 -0.00029 0.00442 0.00057 0.01910 0.00286 0.00018 0.00028 0.00016 0.00000 0.00070 0.00085 0.00071 0.00066 0.00054 0.00068 0.00034 C1 0.25342 0.99853 0.47814 1.00000 0.02087 0.02361 0.02729 -0.00503 0.00763 -0.00409 0.02352 0.00356 0.00023 0.00036 0.00021 0.00000 0.00086 0.00108 0.00095 0.00085 0.00071 0.00084 0.00043 H1A 0.32001 0.91811 0.56011 1.00000 0.02823 0.00000 0.00000 H1B 0.22276 1.14648 0.51210 1.00000 0.02823 0.00000 0.00000 C2 0.35923 1.03221 0.36587 1.00000 0.02158 0.01848 0.02876 -0.00336 0.00764 -0.00211 0.02257 0.00371 0.00024 0.00035 0.00021 0.00000 0.00087 0.00096 0.00097 0.00083 0.00073 0.00079 0.00041 H2A 0.29789 1.12636 0.28808 1.00000 0.02708 0.00000 0.00000 H2B 0.46406 1.11051 0.40800 1.00000 0.02708 0.00000 0.00000 C3 0.24896 0.67923 0.26047 1.00000 0.02363 0.02219 0.02551 -0.00252 0.00558 -0.00626 0.02366 0.00358 0.00023 0.00036 0.00021 0.00000 0.00090 0.00110 0.00090 0.00082 0.00069 0.00084 0.00043 H3A 0.28179 0.52785 0.23382 1.00000 0.02839 0.00000 0.00000 H3B 0.17989 0.74903 0.17544 1.00000 0.02839 0.00000 0.00000 C4 0.14792 0.66093 0.37773 1.00000 0.02409 0.01985 0.02910 0.00072 0.00645 -0.00471 0.02416 0.00381 0.00024 0.00036 0.00021 0.00000 0.00090 0.00100 0.00097 0.00085 0.00073 0.00081 0.00042 H4A 0.04441 0.57523 0.34216 1.00000 0.02900 0.00000 0.00000 H4B 0.21357 0.57731 0.45872 1.00000 0.02900 0.00000 0.00000 C5 0.52845 0.80887 0.23314 1.00000 0.01699 0.02101 0.01647 0.00044 0.00116 0.00160 0.01842 0.00336 0.00021 0.00036 0.00018 0.00000 0.00079 0.00092 0.00077 0.00074 0.00061 0.00074 0.00037 C6 0.76856 0.97331 0.18751 1.00000 0.01690 0.02684 0.01806 0.00258 0.00255 0.00097 0.02070 0.00356 0.00022 0.00036 0.00019 0.00000 0.00079 0.00108 0.00083 0.00080 0.00061 0.00082 0.00040 C7 0.79367 0.81044 0.09166 1.00000 0.02024 0.03565 0.01678 -0.00059 0.00363 0.00663 0.02420 0.00375 0.00023 0.00040 0.00018 0.00000 0.00084 0.00117 0.00082 0.00086 0.00066 0.00088 0.00043 H7 0.88494 0.81779 0.04311 1.00000 0.02905 0.00000 0.00000 C8 0.67969 0.63542 0.06932 1.00000 0.02579 0.03026 0.02024 -0.00794 0.00097 0.00710 0.02588 0.00376 0.00024 0.00041 0.00020 0.00000 0.00093 0.00113 0.00086 0.00089 0.00070 0.00093 0.00044 H8 0.69359 0.51768 0.00592 1.00000 0.03105 0.00000 0.00000 C9 0.54623 0.63203 0.13897 1.00000 0.02134 0.02212 0.02437 -0.00384 0.00054 0.00043 0.02311 0.00355 0.00023 0.00037 0.00020 0.00000 0.00087 0.00101 0.00092 0.00084 0.00069 0.00083 0.00041 H9 0.46758 0.51290 0.12394 1.00000 0.02773 0.00000 0.00000 C10 0.88513 1.16511 0.22158 1.00000 0.02253 0.02592 0.02410 0.00226 0.00785 -0.00058 0.02373 0.00379 0.00023 0.00037 0.00020 0.00000 0.00086 0.00106 0.00088 0.00085 0.00068 0.00085 0.00042 H10 0.87546 1.25525 0.30131 1.00000 0.02848 0.00000 0.00000 Final Structure Factor Calculation for 2007jmw0010 in P2(1) Total number of l.s. parameters = 127 Maximum vector length = 511 Memory required = 1693 / 25046 wR2 = 0.0801 before cycle 7 for 1152 data and 2 / 127 parameters GooF = S = 1.124; Restrained GooF = 1.123 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0307 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0331 for 1089 Fo > 4sig(Fo) and 0.0355 for all 1152 data wR2 = 0.0801, GooF = S = 1.124, Restrained GooF = 1.123 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0292 0.0242 0.0169 O1 0.0405 0.0346 0.0169 O2 0.0248 0.0196 0.0142 N1 0.0208 0.0193 0.0172 N2 0.0320 0.0207 0.0179 C1 0.0304 0.0200 0.0172 C2 0.0299 0.0245 0.0166 C3 0.0293 0.0269 0.0163 C4 0.0217 0.0189 0.0147 C5 0.0275 0.0183 0.0163 C6 0.0383 0.0179 0.0164 C7 0.0407 0.0214 0.0155 C8 0.0297 0.0213 0.0183 C9 0.0277 0.0251 0.0184 C10 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.035 0.056 0.076 0.096 0.117 0.142 0.171 0.226 0.322 1.000 Number in group 117. 116. 116. 114. 117. 115. 111. 116. 114. 116. GooF 1.239 1.274 1.109 1.065 1.115 1.106 1.186 1.003 0.971 1.133 K 1.144 1.040 0.993 0.984 0.995 0.990 1.013 1.006 1.008 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.16 1.33 1.68 inf Number in group 117. 116. 114. 115. 116. 114. 116. 113. 117. 114. GooF 1.067 1.236 1.029 1.041 1.231 1.053 1.043 0.970 1.197 1.315 K 1.038 1.036 1.019 1.011 0.996 0.991 1.001 1.002 1.025 0.998 R1 0.075 0.067 0.061 0.051 0.044 0.031 0.026 0.023 0.025 0.023 Recommended weighting scheme: WGHT 0.0257 0.1715 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 0 6 11.92 3.05 4.67 0.044 1.25 6 4 2 16.19 25.22 4.34 0.127 0.95 0 0 7 2.85 0.65 3.69 0.020 1.34 -3 5 4 3.69 7.08 3.24 0.068 1.02 6 4 1 19.63 26.61 3.20 0.131 0.97 2 0 1 46.46 57.29 3.15 0.192 3.45 0 3 3 53.47 42.52 3.13 0.165 1.68 6 5 4 0.12 1.75 2.98 0.034 0.80 -1 3 3 118.57 102.09 2.91 0.256 1.68 -7 1 10 27.22 20.58 2.90 0.115 0.80 3 3 3 39.67 31.49 2.85 0.142 1.36 1 0 10 7.56 4.31 2.84 0.053 0.91 -1 4 7 64.89 77.56 2.80 0.223 1.01 0 6 3 3.04 1.35 2.77 0.029 0.95 5 5 0 30.85 39.08 2.76 0.159 0.96 -2 6 7 3.48 7.68 2.74 0.070 0.80 -1 0 2 1396.43 1553.34 2.74 1.000 4.44 3 5 8 1.27 4.17 2.68 0.052 0.77 -6 5 6 17.87 12.34 2.67 0.089 0.82 -2 0 2 283.67 317.54 2.64 0.452 3.38 3 3 6 48.25 39.31 2.61 0.159 1.06 4 5 1 2.30 4.35 2.54 0.053 1.01 -3 7 4 6.15 10.81 2.52 0.083 0.78 -3 2 1 87.37 75.85 2.51 0.221 2.00 -4 6 6 8.26 4.35 2.50 0.053 0.80 -5 0 2 105.19 92.11 2.47 0.244 1.61 -5 4 1 35.60 43.08 2.46 0.167 1.10 -7 5 1 27.23 20.74 2.43 0.116 0.83 -7 0 10 0.36 1.66 2.36 0.033 0.81 3 2 1 736.07 673.96 2.35 0.659 1.89 8 0 5 6.18 3.61 2.32 0.048 0.82 1 0 1 8.38 11.50 2.32 0.086 5.59 2 1 0 832.50 908.10 2.32 0.765 3.32 2 0 0 182.08 203.64 2.31 0.362 4.00 3 2 0 189.84 171.18 2.30 0.332 1.99 -2 7 2 8.23 5.35 2.30 0.059 0.83 5 0 8 1.51 0.04 2.29 0.005 0.87 3 6 5 10.30 6.87 2.28 0.066 0.81 1 0 6 74.63 64.82 2.26 0.204 1.49 4 4 5 1.98 3.69 2.24 0.049 0.96 0 0 11 1.40 0.13 2.24 0.009 0.86 0 0 10 17.52 12.90 2.21 0.091 0.94 -6 5 4 2.11 0.25 2.20 0.013 0.87 -6 1 9 11.95 15.48 2.17 0.100 0.90 -7 1 5 10.35 13.61 2.16 0.094 1.05 6 4 6 26.48 20.70 2.16 0.115 0.79 -2 5 6 1.38 2.74 2.15 0.042 0.95 -4 0 3 682.25 628.85 2.10 0.636 1.85 0 2 5 19.06 15.36 2.10 0.099 1.59 3 0 3 170.20 187.62 2.10 0.348 1.86 Bond lengths and angles O1 - Distance Angles C4 1.4239 (0.0026) C1 1.4265 (0.0023) 109.47 (0.14) O1 - C4 O2 - Distance Angles C10 1.2103 (0.0023) O2 - N1 - Distance Angles C5 1.3889 (0.0022) C3 1.4645 (0.0023) 119.52 (0.15) C2 1.4695 (0.0026) 117.33 (0.16) 112.16 (0.15) N1 - C5 C3 N2 - Distance Angles C5 1.3373 (0.0025) C6 1.3484 (0.0023) 118.12 (0.16) N2 - C5 C1 - Distance Angles O1 1.4265 (0.0023) C2 1.5141 (0.0026) 112.27 (0.16) H1A 0.9900 109.15 109.15 H1B 0.9900 109.15 109.15 107.87 C1 - O1 C2 H1A C2 - Distance Angles N1 1.4695 (0.0026) C1 1.5141 (0.0026) 110.04 (0.17) H2A 0.9900 109.65 109.65 H2B 0.9900 109.65 109.65 108.16 C2 - N1 C1 H2A C3 - Distance Angles N1 1.4645 (0.0023) C4 1.5175 (0.0026) 110.08 (0.16) H3A 0.9900 109.64 109.64 H3B 0.9900 109.64 109.64 108.15 C3 - N1 C4 H3A C4 - Distance Angles O1 1.4239 (0.0026) C3 1.5175 (0.0026) 112.15 (0.17) H4A 0.9900 109.18 109.18 H4B 0.9900 109.18 109.18 107.89 C4 - O1 C3 H4A C5 - Distance Angles N2 1.3373 (0.0025) N1 1.3889 (0.0022) 116.58 (0.16) C9 1.4143 (0.0027) 121.30 (0.16) 122.08 (0.17) C5 - N2 N1 C6 - Distance Angles N2 1.3484 (0.0023) C7 1.3794 (0.0029) 124.48 (0.19) C10 1.4843 (0.0028) 114.11 (0.17) 121.42 (0.17) C6 - N2 C7 C7 - Distance Angles C6 1.3794 (0.0029) C8 1.3876 (0.0032) 117.04 (0.17) H7 0.9500 121.48 121.48 C7 - C6 C8 C8 - Distance Angles C9 1.3796 (0.0026) C7 1.3876 (0.0032) 120.14 (0.20) H8 0.9500 119.93 119.93 C8 - C9 C7 C9 - Distance Angles C8 1.3796 (0.0026) C5 1.4143 (0.0027) 118.89 (0.19) H9 0.9500 120.55 120.55 C9 - C8 C5 C10 - Distance Angles O2 1.2103 (0.0023) C6 1.4843 (0.0028) 124.31 (0.19) H10 0.9500 117.85 117.85 C10 - O2 C6 FMAP and GRID set by program FMAP 2 2 17 GRID -3.571 -2 -2 3.571 2 2 R1 = 0.0355 for 1152 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.17 at 0.4853 0.2476 0.8348 [ 0.74 A from C5 ] Deepest hole -0.20 at 0.9379 0.2447 0.2576 [ 0.69 A from C10 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 1748 / 15407 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5147 0.7476 0.1652 1.00000 0.05 0.17 0.74 C5 0.79 C9 1.49 H9 1.83 N2 Q2 1 0.3778 0.9183 0.3357 1.00000 0.05 0.17 0.70 N1 0.77 C2 1.44 H2A 1.45 H2B Q3 1 0.8442 1.0392 0.2166 1.00000 0.05 0.16 0.74 C6 0.82 C10 1.52 H10 1.78 O2 Q4 1 0.4416 0.8222 0.2587 1.00000 0.05 0.15 0.64 N1 0.80 C5 1.79 C3 1.83 C2 Q5 1 0.2985 1.0305 0.4172 1.00000 0.05 0.14 0.76 C2 0.77 C1 1.36 H2A 1.38 H1B Shortest distances between peaks (including symmetry equivalents) 2 4 1.14 1 4 1.25 2 5 1.29 1 2 2.38 4 5 2.43 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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 0.01: Generate ISOR restraints 0.00: Generate NCSY restraints 0.03: Analyse other restraints etc. 0.62: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.03: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.46: Structure factors and derivatives 0.52: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.24: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.01: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007jmw0010 finished at 13:21:09 Total CPU time: 2.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++