+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src1375 started at 14:06:53 on 17-Nov-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src1375 in Pnma CELL 0.71073 8.3358 26.3096 5.6923 90.000 90.000 90.000 ZERR 4.00 0.0006 0.0017 0.0003 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, - Z SYMM 1/2 + X, 1/2 - Y, 1/2 - Z SFAC C H S UNIT 72 48 4 V = 1248.39 F(000) = 544.0 Mu = 0.24 mm-1 Cell Wt = 1041.34 Rho = 1.385 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 10 BOND $H CONF SIZE 0.01 0.15 0.26 ACTA WGHT 0.05230 2.48810 L.S. 5 TEMP -153.00 FVAR 0.67165 C1 1 0.366215 0.296226 0.079876 11.00000 0.02169 0.03011 = 0.02476 0.00038 0.00252 0.00124 C2 1 0.280447 0.276798 -0.106288 11.00000 0.02163 0.02892 = 0.02216 0.00123 0.00197 0.00048 C3 1 0.210451 0.318954 -0.249807 11.00000 0.02630 0.03228 = 0.02041 0.00169 -0.00298 0.00128 AFIX 23 H3A 2 0.091741 0.317811 -0.249202 11.00000 -1.20000 H3B 2 0.249405 0.317824 -0.414022 11.00000 -1.20000 AFIX 0 C4 1 0.273316 0.365870 -0.120771 11.00000 0.02242 0.03168 = 0.02574 -0.00273 0.00353 -0.00001 C5 1 0.250150 0.416768 -0.171525 11.00000 0.03405 0.03378 = 0.02774 0.00342 0.00356 0.00347 AFIX 43 H5 2 0.188863 0.426749 -0.304453 11.00000 -1.20000 AFIX 0 C6 1 0.318221 0.453076 -0.024395 11.00000 0.03830 0.02610 = 0.03772 0.00039 0.00675 0.00220 AFIX 43 H6 2 0.303370 0.488171 -0.057077 11.00000 -1.20000 AFIX 0 C7 1 0.407333 0.438456 0.169057 11.00000 0.03485 0.03084 = 0.03746 -0.00537 0.00469 -0.00184 AFIX 43 H7 2 0.452423 0.463897 0.267371 11.00000 -1.20000 AFIX 0 C8 1 0.432698 0.387863 0.223512 11.00000 0.02594 0.03410 = 0.02926 -0.00196 0.00028 -0.00040 AFIX 43 H8 2 0.494575 0.378316 0.356535 11.00000 -1.20000 AFIX 0 C9 1 0.364959 0.351554 0.077817 11.00000 0.02023 0.03090 = 0.02428 0.00083 0.00511 0.00167 S1 3 0.450760 0.250000 0.255797 10.50000 0.02781 0.02913 = 0.02542 0.00000 -0.00653 0.00000 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 2007src1375 in Pnma C 0.770 H 0.320 S 1.030 C1 - C2 C9 S1 C2 - C1 C2_$1 C3 C3 - C2 C4 C4 - C5 C9 C3 C5 - C4 C6 C6 - C7 C5 C7 - C6 C8 C8 - C7 C9 C9 - C8 C4 C1 S1 - C1_$1 C1 Operators for generating equivalent atoms: $1 x, -y+1/2, z h k l Fo^2 Sigma Why rejected 0 7 0 11.19 2.77 observed but should be systematically absent 0 8 3 8.53 2.13 observed but should be systematically absent 8764 Reflections read, of which 879 rejected -10 =< h =< 10, -34 =< k =< 33, -7 =< l =< 7, Max. 2-theta = 54.99 2 Systematic absence violations 0 Inconsistent equivalents 1461 Unique reflections, of which 0 suppressed R(int) = 0.0643 R(sigma) = 0.0476 Friedel opposites merged Maximum memory for data reduction = 1266 / 14495 Special position constraints for S1 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 1510 / 116001 wR2 = 0.1586 before cycle 1 for 1461 data and 88 / 88 parameters GooF = S = 1.069; Restrained GooF = 1.069 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0523 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.67169 0.00285 0.013 OSF Mean shift/esd = 0.005 Maximum = 0.017 for U22 S1 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C7 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1510 / 116001 wR2 = 0.1586 before cycle 2 for 1461 data and 88 / 88 parameters GooF = S = 1.069; Restrained GooF = 1.069 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0523 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.67170 0.00285 0.004 OSF Mean shift/esd = 0.002 Maximum = 0.007 for U22 S1 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C7 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1510 / 116001 wR2 = 0.1586 before cycle 3 for 1461 data and 88 / 88 parameters GooF = S = 1.069; Restrained GooF = 1.069 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0523 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.67170 0.00285 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z C1 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C7 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1510 / 116001 wR2 = 0.1586 before cycle 4 for 1461 data and 88 / 88 parameters GooF = S = 1.069; Restrained GooF = 1.069 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0523 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.67170 0.00285 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C5 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1510 / 116001 wR2 = 0.1586 before cycle 5 for 1461 data and 88 / 88 parameters GooF = S = 1.069; Restrained GooF = 1.069 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0523 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.67170 0.00285 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C2 Max. dU = 0.000 for C9 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 6 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3A 0.0917 0.3178 -0.2492 23 0.990 0.000 C3 C2 C4 H3B 0.2494 0.3178 -0.4140 23 0.990 0.000 C3 C2 C4 H5 0.1889 0.4267 -0.3045 43 0.950 0.000 C5 C4 C6 H6 0.3034 0.4882 -0.0571 43 0.950 0.000 C6 C7 C5 H7 0.4524 0.4639 0.2674 43 0.950 0.000 C7 C6 C8 H8 0.4946 0.3783 0.3565 43 0.950 0.000 C8 C7 C9 2007src1375 in Pnma ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.36622 0.29623 0.07988 1.00000 0.02168 0.03014 0.02475 0.00038 0.00252 0.00124 0.02552 0.00439 0.00030 0.00009 0.00044 0.00000 0.00122 0.00124 0.00120 0.00099 0.00098 0.00099 0.00055 C2 0.28045 0.27680 -0.10629 1.00000 0.02162 0.02895 0.02215 0.00124 0.00198 0.00048 0.02424 0.00428 0.00030 0.00009 0.00042 0.00000 0.00118 0.00127 0.00115 0.00095 0.00097 0.00099 0.00053 C3 0.21045 0.31895 -0.24981 1.00000 0.02629 0.03229 0.02041 0.00169 -0.00298 0.00129 0.02633 0.00433 0.00033 0.00009 0.00043 0.00000 0.00127 0.00124 0.00111 0.00101 0.00102 0.00105 0.00055 H3A 0.09174 0.31781 -0.24920 1.00000 0.03160 0.00000 0.00000 H3B 0.24941 0.31782 -0.41402 1.00000 0.03160 0.00000 0.00000 C4 0.27332 0.36587 -0.12077 1.00000 0.02241 0.03170 0.02573 -0.00274 0.00354 -0.00001 0.02662 0.00442 0.00031 0.00010 0.00044 0.00000 0.00123 0.00130 0.00120 0.00099 0.00101 0.00102 0.00056 C5 0.25015 0.41677 -0.17152 1.00000 0.03404 0.03380 0.02774 0.00343 0.00356 0.00348 0.03186 0.00505 0.00035 0.00010 0.00049 0.00000 0.00152 0.00134 0.00126 0.00106 0.00111 0.00115 0.00062 H5 0.18887 0.42675 -0.30445 1.00000 0.03823 0.00000 0.00000 C6 0.31822 0.45307 -0.02439 1.00000 0.03830 0.02609 0.03772 0.00039 0.00675 0.00220 0.03404 0.00508 0.00036 0.00010 0.00050 0.00000 0.00160 0.00123 0.00146 0.00108 0.00125 0.00115 0.00065 H6 0.30337 0.48817 -0.05707 1.00000 0.04084 0.00000 0.00000 C7 0.40733 0.43846 0.16905 1.00000 0.03484 0.03086 0.03746 -0.00537 0.00470 -0.00184 0.03439 0.00505 0.00036 0.00010 0.00050 0.00000 0.00156 0.00134 0.00147 0.00113 0.00127 0.00115 0.00065 H7 0.45242 0.46390 0.26736 1.00000 0.04127 0.00000 0.00000 C8 0.43269 0.38786 0.22351 1.00000 0.02593 0.03411 0.02925 -0.00195 0.00028 -0.00040 0.02976 0.00459 0.00033 0.00010 0.00047 0.00000 0.00135 0.00129 0.00127 0.00107 0.00107 0.00106 0.00058 H8 0.49457 0.37832 0.35653 1.00000 0.03572 0.00000 0.00000 C9 0.36496 0.35156 0.07782 1.00000 0.02023 0.03092 0.02427 0.00083 0.00512 0.00167 0.02514 0.00444 0.00030 0.00009 0.00043 0.00000 0.00119 0.00123 0.00115 0.00099 0.00097 0.00097 0.00054 S1 0.45076 0.25000 0.25580 0.50000 0.02781 0.02914 0.02542 0.00000 -0.00653 0.00000 0.02746 0.00127 0.00012 0.00000 0.00016 0.00000 0.00050 0.00045 0.00046 0.00000 0.00036 0.00000 0.00028 Final Structure Factor Calculation for 2007src1375 in Pnma Total number of l.s. parameters = 88 Maximum vector length = 511 Memory required = 1422 / 21973 wR2 = 0.1586 before cycle 6 for 1461 data and 0 / 88 parameters GooF = S = 1.069; Restrained GooF = 1.069 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0523 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0629 for 1201 Fo > 4sig(Fo) and 0.0780 for all 1461 data wR2 = 0.1586, GooF = S = 1.069, Restrained GooF = 1.069 for all data Occupancy sum of asymmetric unit = 9.50 for non-hydrogen and 6.00 for hydrogen atoms Principal mean square atomic displacements U 0.0304 0.0260 0.0202 C1 0.0293 0.0236 0.0199 C2 0.0327 0.0275 0.0189 C3 0.0329 0.0269 0.0200 C4 0.0395 0.0304 0.0257 C5 0.0450 0.0315 0.0256 C6 0.0434 0.0320 0.0278 C7 0.0348 0.0286 0.0259 C8 0.0317 0.0271 0.0167 C9 0.0333 0.0291 0.0200 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.021 0.032 0.043 0.055 0.072 0.092 0.124 0.176 1.000 Number in group 158. 142. 147. 145. 139. 149. 142. 147. 146. 146. GooF 1.224 1.070 1.126 1.011 1.086 0.981 1.076 0.966 0.995 1.116 K 3.627 1.373 1.078 1.034 0.988 1.045 0.989 0.994 1.012 1.036 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.33 1.67 inf Number in group 155. 140. 143. 151. 141. 147. 146. 145. 146. 147. GooF 1.164 1.172 1.015 0.935 1.024 0.910 0.961 0.966 0.999 1.433 K 1.070 1.046 1.041 1.036 1.005 1.003 0.997 0.985 1.006 1.052 R1 0.162 0.176 0.116 0.089 0.087 0.071 0.058 0.056 0.052 0.052 Recommended weighting scheme: WGHT 0.0520 2.4940 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 10 2 21.81 1.47 4.01 0.009 1.93 1 0 6 47.94 117.46 3.76 0.079 0.94 6 3 3 51.72 7.61 3.70 0.020 1.11 8 18 3 -1.58 39.78 3.68 0.046 0.77 4 1 1 2683.02 2117.93 3.35 0.334 1.95 3 0 3 47.68 14.51 3.34 0.028 1.57 4 9 0 29.07 3.81 3.08 0.014 1.70 7 2 5 5.63 34.46 2.99 0.043 0.82 10 2 1 41.03 11.79 2.87 0.025 0.82 8 7 4 42.38 11.13 2.84 0.024 0.82 0 14 0 17.23 47.53 2.83 0.050 1.88 8 1 2 222.78 149.70 2.77 0.089 0.98 3 4 2 630.40 495.13 2.68 0.162 1.90 4 2 2 477.33 366.12 2.66 0.139 1.67 0 30 0 933.64 699.59 2.66 0.192 0.88 2 0 0 10429.00 8531.58 2.66 0.670 4.17 7 8 3 18.73 1.87 2.64 0.010 0.96 0 8 0 122.53 77.82 2.60 0.064 3.29 2 1 2 97.26 59.30 2.59 0.056 2.34 4 0 4 19.29 1.69 2.59 0.009 1.18 3 0 1 9926.46 8281.48 2.54 0.661 2.50 0 12 0 114.57 72.76 2.52 0.062 2.19 7 22 3 21.99 1.22 2.49 0.008 0.77 2 0 6 13.25 42.30 2.46 0.047 0.93 0 3 3 63.17 103.58 2.43 0.074 1.85 2 13 0 1989.19 1653.06 2.41 0.295 1.82 2 29 3 314.61 233.49 2.36 0.111 0.80 8 6 2 57.73 23.50 2.34 0.035 0.95 9 6 1 18.09 0.42 2.31 0.005 0.89 5 10 6 25.08 2.56 2.31 0.012 0.79 0 28 4 336.55 249.01 2.30 0.115 0.78 4 5 3 9.93 0.19 2.30 0.003 1.36 0 10 6 55.08 24.03 2.30 0.036 0.89 6 8 5 173.42 121.28 2.29 0.080 0.85 10 12 0 63.10 112.04 2.28 0.077 0.78 3 2 7 27.88 55.62 2.27 0.054 0.78 3 0 2 10050.37 8513.36 2.24 0.670 1.99 5 26 1 10.40 0.01 2.24 0.001 0.86 0 30 2 269.40 202.22 2.21 0.103 0.84 2 2 2 104.66 149.88 2.21 0.089 2.31 8 15 2 70.18 115.95 2.20 0.078 0.85 8 4 4 17.59 2.68 2.19 0.012 0.83 2 6 0 1693.89 1986.86 2.19 0.324 3.02 4 22 2 14.73 3.57 2.17 0.014 0.97 4 6 2 8.27 0.41 2.16 0.005 1.57 1 13 1 2674.80 2311.95 2.16 0.349 1.86 2 8 1 73.87 46.58 2.14 0.050 2.35 8 21 0 153.84 107.08 2.12 0.075 0.80 3 30 2 9.88 0.40 2.11 0.005 0.80 2 23 1 78.56 50.08 2.09 0.051 1.08 Bond lengths and angles C1 - Distance Angles C2 1.3767 (0.0035) C9 1.4558 (0.0034) 111.18 (0.22) S1 1.7259 (0.0026) 113.39 (0.19) 135.42 (0.20) C1 - C2 C9 C2 - Distance Angles C1 1.3767 (0.0035) C2_$1 1.4101 (0.0048) 111.79 (0.15) C3 1.4960 (0.0032) 110.34 (0.21) 137.85 (0.13) C2 - C1 C2_$1 C3 - Distance Angles C2 1.4960 (0.0032) C4 1.5290 (0.0034) 101.68 (0.20) H3A 0.9900 111.43 111.43 H3B 0.9900 111.43 111.43 109.28 C3 - C2 C4 H3A C4 - Distance Angles C5 1.3834 (0.0036) C9 1.4154 (0.0036) 119.98 (0.24) C3 1.5290 (0.0034) 129.29 (0.24) 110.72 (0.21) C4 - C5 C9 C5 - Distance Angles C4 1.3834 (0.0036) C6 1.3913 (0.0039) 118.81 (0.26) H5 0.9500 120.59 120.59 C5 - C4 C6 C6 - Distance Angles C7 1.3828 (0.0042) C5 1.3913 (0.0039) 120.49 (0.25) H6 0.9500 119.75 119.75 C6 - C7 C5 C7 - Distance Angles C6 1.3828 (0.0042) C8 1.3829 (0.0038) 121.89 (0.26) H7 0.9500 119.05 119.05 C7 - C6 C8 C8 - Distance Angles C7 1.3829 (0.0038) C9 1.3853 (0.0036) 117.85 (0.26) H8 0.9500 121.07 121.07 C8 - C7 C9 C9 - Distance Angles C8 1.3853 (0.0036) C4 1.4154 (0.0036) 120.97 (0.23) C1 1.4558 (0.0034) 132.98 (0.24) 106.04 (0.22) C9 - C8 C4 S1 - Distance Angles C1_$1 1.7259 (0.0026) C1 1.7259 (0.0026) 89.61 (0.17) S1 - C1_$1 Selected torsion angles -179.91 ( 0.15) C9 - C1 - C2 - C2_$1 0.87 ( 0.20) S1 - C1 - C2 - C2_$1 -1.01 ( 0.30) C9 - C1 - C2 - C3 179.78 ( 0.18) S1 - C1 - C2 - C3 1.50 ( 0.27) C1 - C2 - C3 - C4 179.98 ( 0.13) C2_$1 - C2 - C3 - C4 179.41 ( 0.27) C2 - C3 - C4 - C5 -1.52 ( 0.27) C2 - C3 - C4 - C9 -0.03 ( 0.39) C9 - C4 - C5 - C6 178.97 ( 0.25) C3 - C4 - C5 - C6 -0.02 ( 0.42) C4 - C5 - C6 - C7 0.19 ( 0.44) C5 - C6 - C7 - C8 -0.29 ( 0.42) C6 - C7 - C8 - C9 0.24 ( 0.39) C7 - C8 - C9 - C4 179.90 ( 0.27) C7 - C8 - C9 - C1 -0.08 ( 0.38) C5 - C4 - C9 - C8 -179.25 ( 0.23) C3 - C4 - C9 - C8 -179.83 ( 0.24) C5 - C4 - C9 - C1 1.00 ( 0.27) C3 - C4 - C9 - C1 -179.71 ( 0.27) C2 - C1 - C9 - C8 -0.74 ( 0.48) S1 - C1 - C9 - C8 -0.01 ( 0.29) C2 - C1 - C9 - C4 178.96 ( 0.22) S1 - C1 - C9 - C4 -1.14 ( 0.26) C2 - C1 - S1 - C1_$1 179.90 ( 0.20) C9 - C1 - S1 - C1_$1 FMAP and GRID set by program FMAP 2 3 10 GRID -3.571 -2 24 3.571 2 1 R1 = 0.0779 for 1461 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.91 at 0.2915 0.7500 0.2629 [ 1.19 A from C2 ] Deepest hole -0.34 at 0.9505 0.2653 0.1806 [ 0.54 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 2025 / 19975 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2085 0.2500 -0.2371 0.50000 0.05 0.91 1.19 C2 1.82 C3 2.03 H3A 2.08 H3B Q2 1 0.2187 0.2879 -0.2379 1.00000 0.05 0.46 0.82 C3 0.95 C2 1.30 H3B 1.32 H3A Q3 1 0.4429 0.2829 0.2007 1.00000 0.05 0.45 0.92 S1 1.00 C1 2.04 C9 2.22 C2 Q4 1 0.4595 0.3183 0.2797 1.00000 0.05 0.38 1.49 C1 1.65 C9 1.66 H8 1.80 S1 Q5 1 0.2600 0.3424 -0.1790 1.00000 0.05 0.37 0.71 C4 0.84 C3 1.49 H3B 1.60 H3A Q6 1 0.3774 0.4335 0.0492 1.00000 0.05 0.36 0.74 C7 0.83 C6 1.60 H7 1.62 C8 Q7 1 0.4198 0.4139 0.1795 1.00000 0.05 0.36 0.66 C7 0.74 C8 1.43 H7 1.51 H8 Q8 1 0.3752 0.3246 0.1023 1.00000 0.05 0.35 0.73 C9 0.76 C1 1.87 C8 1.87 C4 Q9 1 0.3900 0.3717 0.1428 1.00000 0.05 0.33 0.68 C9 0.72 C8 1.51 H8 1.77 C7 Q10 1 0.2907 0.4255 -0.0797 1.00000 0.05 0.32 0.66 C5 0.82 C6 1.54 H5 1.59 C4 Shortest distances between peaks (including symmetry equivalents) 6 7 0.97 1 2 1.00 3 4 1.04 6 10 1.05 7 9 1.16 4 8 1.24 8 9 1.27 3 8 1.35 2 5 1.51 4 9 1.71 6 9 1.71 3 3 1.73 7 10 1.85 5 8 1.92 2 2 2.00 9 10 2.07 5 9 2.26 5 10 2.27 3 9 2.40 7 8 2.42 1 5 2.49 2 8 2.53 4 7 2.60 3 4 2.70 6 8 2.88 5 6 2.90 8 10 2.93 3 8 2.94 Time profile in seconds ----------------------- 0.06: 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. 0.57: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.47: Structure factors and derivatives 0.16: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.05: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.04: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src1375 finished at 14:06:55 Total CPU time: 1.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++