+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007jmw0002 started at 14:54:42 on 27-Feb-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007jmw0002 in P2(1)/c CELL 0.71073 10.0118 4.3353 16.6170 90.000 106.290 90.000 ZERR 4.00 0.0008 0.0003 0.0014 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O S UNIT 28 24 12 4 V = 692.29 F(000) = 352.0 Mu = 0.41 mm-1 Cell Wt = 680.71 Rho = 1.633 MERG 0 OMIT -3.00 50.00 OMIT 1 2 -2 FMAP 2 PLAN 5 SIZE 0.01 0.06 0.25 ACTA BOND $H L.S. 10 TEMP -153.00 WGHT 0.0578 3.0732 EXTI 0.023596 BASF 0.28940 FVAR 1.01044 C1 1 0.226288 0.889562 0.255384 11.00000 0.02216 0.02813 = 0.01371 -0.00103 0.00221 -0.00156 C2 1 0.227883 0.926809 0.337930 11.00000 0.01860 0.02178 = 0.01599 -0.00157 0.00352 -0.00594 C3 1 0.139056 1.035471 0.450911 11.00000 0.02594 0.03563 = 0.00961 -0.00095 0.00464 -0.00341 AFIX 23 H3A 2 0.091195 0.838114 0.454321 11.00000 -1.20000 H3B 2 0.089697 1.201434 0.471893 11.00000 -1.20000 AFIX 0 C4 1 0.286755 1.017799 0.504541 11.00000 0.03164 0.02870 = 0.01387 -0.00250 0.00232 -0.00069 AFIX 23 H4A 2 0.334513 1.214768 0.500533 11.00000 -1.20000 H4B 2 0.287702 0.988297 0.563777 11.00000 -1.20000 AFIX 0 C5 1 0.338783 0.765223 0.393953 11.00000 0.02117 0.02636 = 0.01016 0.00232 -0.00241 -0.00506 C6 1 0.419745 0.608577 0.353718 11.00000 0.02025 0.02878 = 0.01921 0.00259 0.00062 0.00201 AFIX 43 H6 2 0.498467 0.487994 0.381377 11.00000 -1.20000 AFIX 0 C7 1 0.131750 1.028699 0.182818 11.00000 0.02300 0.03903 = 0.01631 -0.00077 0.00256 -0.00310 AFIX 43 H7 2 0.059464 1.155468 0.191266 11.00000 -1.20000 AFIX 0 O1 3 0.134260 1.097727 0.363595 11.00000 0.02250 0.03310 = 0.01309 0.00169 0.00397 0.00357 O2 3 0.361600 0.765972 0.479102 11.00000 0.02823 0.02794 = 0.01245 0.00304 0.00296 0.00415 O3 3 0.138504 0.994169 0.110871 11.00000 0.03594 0.04034 = 0.01139 0.00125 0.00140 -0.00238 S1 4 0.361470 0.656829 0.246927 11.00000 0.02214 0.03273 = 0.01289 -0.00091 0.00323 -0.00027 HKLF 5 Covalent radii and connectivity table for 2007jmw0002 in P2(1)/c C 0.770 H 0.320 O 0.660 S 1.030 C1 - C2 C7 S1 C2 - O1 C1 C5 C3 - O1 C4 C4 - O2 C3 C5 - C6 O2 C2 C6 - C5 S1 C7 - O3 C1 O1 - C2 C3 O2 - C5 C4 O3 - C7 S1 - C6 C1 5642 Reflections read, of which 1236 rejected -11 =< h =< 11, -5 =< k =< 5, -19 =< l =< 18, Max. 2-theta = 49.99 0 Systematic absence violations 0 Data suppressed, R(sigma) = 0.0667 Maximum memory for data reduction = 1080 / 9 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 = 1347 / 132696 wR2 = 0.1854 before cycle 1 for 4407 data and 102 / 102 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0578 * P )^2 + 3.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01043 0.00411 -0.004 OSF 2 0.28929 0.00361 -0.030 BASF 1 3 0.02369 0.00376 0.024 EXTI Mean shift/esd = 0.013 Maximum = 0.062 for U22 S1 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1347 / 132696 wR2 = 0.1854 before cycle 2 for 4407 data and 102 / 102 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0578 * P )^2 + 3.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01044 0.00411 0.003 OSF 2 0.28925 0.00361 -0.011 BASF 1 3 0.02372 0.00377 0.010 EXTI Mean shift/esd = 0.005 Maximum = 0.019 for U22 S1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C4 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1347 / 132696 wR2 = 0.1854 before cycle 3 for 4407 data and 102 / 102 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0578 * P )^2 + 3.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01044 0.00411 0.000 OSF 2 0.28925 0.00361 0.000 BASF 1 3 0.02373 0.00377 0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for U11 C6 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C6 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1347 / 132696 wR2 = 0.1854 before cycle 4 for 4407 data and 102 / 102 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0578 * P )^2 + 3.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01044 0.00411 0.000 OSF 2 0.28925 0.00361 0.000 BASF 1 3 0.02373 0.00377 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for U11 S1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1347 / 132696 wR2 = 0.1854 before cycle 5 for 4407 data and 102 / 102 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0578 * P )^2 + 3.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01044 0.00411 0.000 OSF 2 0.28925 0.00361 0.000 BASF 1 3 0.02373 0.00377 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for O2 Max. dU = 0.000 for O2 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1347 / 132696 wR2 = 0.1854 before cycle 6 for 4407 data and 102 / 102 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0578 * P )^2 + 3.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01044 0.00411 0.000 OSF 2 0.28925 0.00361 0.000 BASF 1 3 0.02373 0.00377 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for BASF 1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C2 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1347 / 132696 wR2 = 0.1854 before cycle 7 for 4407 data and 102 / 102 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0578 * P )^2 + 3.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01044 0.00411 0.000 OSF 2 0.28925 0.00361 0.000 BASF 1 3 0.02373 0.00377 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y S1 Max. shift = 0.000 A for O2 Max. dU = 0.000 for C1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1347 / 132696 wR2 = 0.1854 before cycle 8 for 4407 data and 102 / 102 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0578 * P )^2 + 3.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01044 0.00411 0.000 OSF 2 0.28925 0.00361 0.000 BASF 1 3 0.02373 0.00377 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y S1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C2 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1347 / 132696 wR2 = 0.1854 before cycle 9 for 4407 data and 102 / 102 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0578 * P )^2 + 3.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01044 0.00411 0.000 OSF 2 0.28925 0.00361 0.000 BASF 1 3 0.02373 0.00377 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y S1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C1 Least-squares cycle 10 Maximum vector length = 511 Memory required = 1347 / 132696 wR2 = 0.1854 before cycle 10 for 4407 data and 102 / 102 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0578 * P )^2 + 3.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01044 0.00411 0.000 OSF 2 0.28925 0.00361 0.000 BASF 1 3 0.02373 0.00377 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y S1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for O3 Largest correlation matrix elements 0.581 EXTI / OSF Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3A 0.0912 0.8381 0.4543 23 0.990 0.000 C3 O1 C4 H3B 0.0897 1.2014 0.4719 23 0.990 0.000 C3 O1 C4 H4A 0.3345 1.2147 0.5005 23 0.990 0.000 C4 O2 C3 H4B 0.2877 0.9882 0.5638 23 0.990 0.000 C4 O2 C3 H6 0.4984 0.4880 0.3814 43 0.950 0.000 C6 C5 S1 H7 0.0595 1.1555 0.1913 43 0.950 0.000 C7 O3 C1 2007jmw0002 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.22629 0.88958 0.25538 1.00000 0.02212 0.02816 0.01370 -0.00104 0.00223 -0.00159 0.02189 0.00552 0.00031 0.00068 0.00017 0.00000 0.00174 0.00180 0.00146 0.00127 0.00119 0.00136 0.00072 C2 0.22788 0.92681 0.33793 1.00000 0.01862 0.02179 0.01600 -0.00157 0.00353 -0.00591 0.01907 0.00526 0.00030 0.00066 0.00017 0.00000 0.00170 0.00165 0.00147 0.00126 0.00120 0.00132 0.00069 C3 0.13905 1.03544 0.45091 1.00000 0.02590 0.03569 0.00963 -0.00097 0.00464 -0.00341 0.02381 0.00555 0.00032 0.00074 0.00017 0.00000 0.00181 0.00187 0.00146 0.00133 0.00122 0.00150 0.00073 H3A 0.09119 0.83808 0.45432 1.00000 0.02858 0.00000 0.00000 H3B 0.08969 1.20140 0.47190 1.00000 0.02858 0.00000 0.00000 C4 0.28676 1.01776 0.50455 1.00000 0.03167 0.02873 0.01388 -0.00249 0.00229 -0.00070 0.02559 0.00565 0.00032 0.00073 0.00018 0.00000 0.00193 0.00189 0.00148 0.00134 0.00131 0.00150 0.00078 H4A 0.33451 1.21473 0.50054 1.00000 0.03071 0.00000 0.00000 H4B 0.28770 0.98825 0.56378 1.00000 0.03071 0.00000 0.00000 C5 0.33878 0.76520 0.39396 1.00000 0.02115 0.02641 0.01013 0.00233 -0.00243 -0.00506 0.02061 0.00521 0.00029 0.00070 0.00016 0.00000 0.00162 0.00173 0.00133 0.00132 0.00113 0.00141 0.00070 C6 0.41973 0.60856 0.35371 1.00000 0.02025 0.02882 0.01923 0.00257 0.00064 0.00199 0.02376 0.00561 0.00032 0.00070 0.00018 0.00000 0.00173 0.00182 0.00162 0.00133 0.00128 0.00137 0.00074 H6 0.49845 0.48796 0.38137 1.00000 0.02851 0.00000 0.00000 C7 0.13175 1.02873 0.18282 1.00000 0.02295 0.03910 0.01633 -0.00078 0.00254 -0.00307 0.02673 0.00570 0.00033 0.00077 0.00018 0.00000 0.00184 0.00205 0.00167 0.00143 0.00125 0.00152 0.00076 H7 0.05946 1.15551 0.19126 1.00000 0.03207 0.00000 0.00000 O1 0.13426 1.09772 0.36360 1.00000 0.02246 0.03314 0.01309 0.00168 0.00397 0.00355 0.02310 0.00375 0.00021 0.00046 0.00012 0.00000 0.00121 0.00128 0.00104 0.00091 0.00085 0.00096 0.00053 O2 0.36160 0.76596 0.47910 1.00000 0.02817 0.02798 0.01249 0.00305 0.00297 0.00414 0.02343 0.00381 0.00021 0.00047 0.00011 0.00000 0.00121 0.00120 0.00098 0.00093 0.00082 0.00102 0.00052 O3 0.13851 0.99418 0.11087 1.00000 0.03591 0.04040 0.01139 0.00127 0.00140 -0.00239 0.03030 0.00395 0.00023 0.00050 0.00012 0.00000 0.00140 0.00146 0.00108 0.00099 0.00091 0.00109 0.00060 S1 0.36147 0.65683 0.24693 1.00000 0.02214 0.03277 0.01289 -0.00091 0.00323 -0.00028 0.02294 0.00143 0.00008 0.00018 0.00004 0.00000 0.00046 0.00052 0.00040 0.00032 0.00029 0.00034 0.00028 Final Structure Factor Calculation for 2007jmw0002 in P2(1)/c Total number of l.s. parameters = 102 Maximum vector length = 511 Memory required = 1245 / 22995 wR2 = 0.1854 before cycle 11 for 4407 data and 0 / 102 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0578 * P )^2 + 3.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0727 for 3616 Fo > 4sig(Fo) and 0.0913 for all 4407 data wR2 = 0.1854, GooF = S = 1.094, Restrained GooF = 1.094 for all data Occupancy sum of asymmetric unit = 11.00 for non-hydrogen and 6.00 for hydrogen atoms Principal mean square atomic displacements U 0.0286 0.0238 0.0133 C1 0.0265 0.0172 0.0135 C2 0.0368 0.0253 0.0094 C3 0.0343 0.0291 0.0133 C4 0.0331 0.0204 0.0083 C5 0.0295 0.0265 0.0153 C6 0.0397 0.0248 0.0157 C7 0.0342 0.0221 0.0129 O1 0.0326 0.0259 0.0118 O2 0.0428 0.0368 0.0112 O3 0.0328 0.0232 0.0128 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.035 0.052 0.072 0.092 0.116 0.139 0.178 0.235 1.000 Number in group 450. 464. 416. 434. 446. 446. 431. 450. 428. 442. GooF 1.177 1.206 1.085 0.947 1.154 1.085 1.087 1.055 0.958 1.135 K 3.012 1.293 1.148 1.071 1.057 1.036 1.036 1.030 0.997 1.005 Resolution(A) 0.84 0.89 0.94 1.00 1.06 1.15 1.25 1.39 1.62 2.00 inf Number in group 458. 434. 430. 441. 441. 442. 446. 442. 430. 443. GooF 1.442 1.120 1.129 1.163 1.070 1.001 0.931 0.959 0.977 1.038 K 1.064 1.058 1.075 1.025 1.010 1.009 1.007 1.008 1.022 1.003 R1 0.225 0.154 0.137 0.123 0.096 0.075 0.074 0.063 0.060 0.042 Recommended weighting scheme: WGHT 0.0579 3.0661 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) 5 -1 -7 126.69 6.62 5.39 0.025 1.60 5 1 -7 127.01 6.62 5.30 0.025 1.60 0 2 2 7.15 90.53 5.27 0.091 2.09 -1 -1 2 4678.85 3288.55 5.23 0.550 3.72 7 4 -1 19.40 176.53 5.20 0.127 0.86 1 1 -2 4519.83 3288.55 4.67 0.550 3.72 2 5 2 4.80 73.50 4.21 0.082 0.84 1 5 3 3.04 103.02 4.14 0.097 0.85 2 5 -4 12.65 102.12 4.03 0.097 0.84 -1 5 -1 15.01 109.15 4.02 0.100 0.86 -2 5 2 65.46 230.54 3.98 0.146 0.85 -3 2 3 3303.33 2500.92 3.77 0.480 1.79 2 5 -4 10.83 102.12 3.58 0.097 0.84 6 4 4 7.80 60.81 3.58 0.075 0.85 4 4 7 55.72 156.20 3.57 0.120 0.87 2 4 2 193.23 361.35 3.54 0.182 1.04 -1 5 4 38.75 192.39 3.54 0.133 0.85 0 4 2 333.79 646.79 3.51 0.244 1.07 -1 5 -2 17.00 81.81 3.50 0.087 0.86 6 3 1 69.93 9.74 3.40 0.030 1.06 1 5 -4 64.05 192.39 3.36 0.133 0.85 1 -1 -2 4142.97 3288.54 3.36 0.550 3.72 4 4 -2 138.13 281.42 3.33 0.161 0.99 0 5 -3 4.11 69.42 3.28 0.080 0.86 1 5 2 -3.18 81.81 3.25 0.087 0.86 -2 -2 -12 -7.52 20.91 3.18 0.044 1.05 1 4 -1 67.97 163.90 3.17 0.123 1.08 3 4 -2 147.53 281.70 3.16 0.161 1.03 -4 -3 -11 47.68 1.82 3.11 0.013 0.88 0 4 10 350.38 559.32 3.07 0.227 0.90 -5 3 -7 329.57 180.60 3.02 0.129 0.97 2 4 3 -8.90 21.68 3.01 0.045 1.02 1 4 -4 -7.10 23.11 2.98 0.046 1.05 -5 0 -14 -4.62 27.60 2.97 0.050 0.88 -3 4 3 74.33 16.63 2.96 0.039 1.03 -2 1 -1 1842.92 2438.28 2.91 0.474 3.05 3 4 3 71.08 151.53 2.84 0.118 0.99 8 -3 3 316.36 184.40 2.83 0.130 0.88 7 1 -18 -2.16 25.55 2.82 0.048 0.85 6 -2 -9 133.59 57.05 2.80 0.072 1.18 -2 2 4 931.80 700.21 2.79 0.254 1.86 -4 1 0 351.77 508.94 2.76 0.216 2.10 2 2 -4 917.80 700.21 2.75 0.254 1.86 -1 -3 -11 332.11 210.80 2.72 0.139 1.00 8 1 5 55.50 126.21 2.72 0.108 1.00 -2 5 4 34.81 102.12 2.69 0.097 0.84 10 -1 -9 52.59 9.76 2.67 0.030 0.94 7 -3 -12 84.44 24.64 2.67 0.048 0.89 8 -2 -6 42.01 0.13 2.66 0.003 1.07 2 4 5 -5.59 17.77 2.62 0.040 0.99 Bond lengths and angles C1 - Distance Angles C2 1.3768 (0.0039) C7 1.4400 (0.0040) 127.33 (0.29) S1 1.7253 (0.0032) 111.08 (0.22) 121.55 (0.23) C1 - C2 C7 C2 - Distance Angles O1 1.3541 (0.0035) C1 1.3768 (0.0039) 124.22 (0.25) C5 1.4180 (0.0039) 123.18 (0.25) 112.60 (0.27) C2 - O1 C1 C3 - Distance Angles O1 1.4633 (0.0032) C4 1.4992 (0.0041) 110.57 (0.25) H3A 0.9900 109.53 109.53 H3B 0.9900 109.53 109.53 108.09 C3 - O1 C4 H3A C4 - Distance Angles O2 1.4524 (0.0036) C3 1.4992 (0.0041) 111.64 (0.24) H4A 0.9900 109.29 109.29 H4B 0.9900 109.29 109.29 107.95 C4 - O2 C3 H4A C5 - Distance Angles C6 1.3672 (0.0042) O2 1.3684 (0.0032) 123.85 (0.25) C2 1.4180 (0.0039) 112.75 (0.25) 123.40 (0.27) C5 - C6 O2 C6 - Distance Angles C5 1.3672 (0.0042) S1 1.7181 (0.0029) 111.63 (0.21) H6 0.9500 124.18 124.18 C6 - C5 S1 C7 - Distance Angles O3 1.2254 (0.0036) C1 1.4400 (0.0041) 124.23 (0.31) H7 0.9500 117.88 117.88 C7 - O3 C1 O1 - Distance Angles C2 1.3541 (0.0035) C3 1.4633 (0.0032) 112.23 (0.21) O1 - C2 O2 - Distance Angles C5 1.3684 (0.0032) C4 1.4524 (0.0036) 110.65 (0.21) O2 - C5 O3 - Distance Angles C7 1.2254 (0.0036) O3 - S1 - Distance Angles C6 1.7181 (0.0029) C1 1.7253 (0.0032) 91.94 (0.14) S1 - C6 FMAP and GRID set by program FMAP 2 2 8 GRID -5.000 -2 -2 5.000 2 2 R1 = 0.0778 for 1201 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.53 at 0.3607 0.1760 0.7383 [ 1.45 A from S1 ] Deepest hole -1.03 at 0.6322 0.1461 0.7489 [ 0.86 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 1560 / 14046 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3607 0.3240 0.2383 1.00000 0.05 0.53 1.45 S1 2.22 C6 2.38 C1 2.49 H6 Q2 1 0.2768 0.7746 0.2446 1.00000 0.05 0.51 0.77 C1 0.98 S1 1.87 C2 1.88 C7 Q3 1 0.2194 1.2617 0.3579 1.00000 0.05 0.50 1.13 O1 1.50 C2 2.17 C3 2.34 H4A Q4 1 0.2786 0.5379 0.2433 1.00000 0.05 0.46 0.96 S1 1.64 C1 2.00 C6 2.45 C2 Q5 1 0.0466 1.0926 0.1980 1.00000 0.05 0.44 0.33 H7 0.99 C7 1.97 O3 1.99 C1 Shortest distances between peaks (including symmetry equivalents) 2 4 1.03 1 4 1.26 1 2 2.14 3 4 2.46 2 5 2.61 1 3 2.76 3 5 2.83 3 5 2.94 4 5 2.95 2 3 2.99 Time profile in seconds ----------------------- 0.12: 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. 0.40: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.25: Structure factors and derivatives 0.64: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.08: Solve l.s. equations 0.00: Generate HTAB table 0.04: Other dependent quantities, CIF, tables 0.07: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007jmw0002 finished at 14:54:44 Total CPU time: 2.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++