+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 293 started at 13:54:51 on 26-Feb-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 293 in Cmc2(1) CELL 0.71073 10.6657 13.4889 8.8593 90.000 90.000 90.000 ZERR 4.00 0.0021 0.0027 0.0018 0.000 0.000 0.000 LATT -7 SYMM - X, - Y, 1/2 + Z SYMM X, - Y, 1/2 + Z SYMM - X, Y, Z SFAC C H O P CL N UNIT 12 24 8 12 16 12 V = 1274.57 F(000) = 696.0 Mu = 1.29 mm-1 Cell Wt = 1403.27 Rho = 1.828 MERG 2 OMIT -3.00 55.00 FMAP 2 SIZE 0.3 0.04 0.04 PLAN 20 ACTA BOND WGHT 0.03840 1.06590 L.S. 4 FVAR 0.44454 CL2 5 0.142774 0.158770 1.025195 11.00000 0.09578 0.08232 = 0.08618 0.00924 -0.02150 0.02655 N2 6 0.000000 0.130285 0.749194 10.50000 0.17378 0.03340 = 0.05126 0.00204 0.00000 0.00000 N3 6 0.000000 0.313160 0.873797 10.50000 0.08073 0.04148 = 0.03721 -0.00214 0.00000 0.00000 N1 6 0.000000 0.292028 0.571202 10.50000 0.10645 0.03836 = 0.03581 -0.00311 0.00000 0.00000 P1 4 0.000000 0.364070 0.711240 10.50000 0.05992 0.03603 = 0.03439 0.00049 0.00000 0.00000 P2 4 0.000000 0.176348 0.587869 10.50000 0.10075 0.03978 = 0.03981 -0.00845 0.00000 0.00000 P3 4 0.000000 0.198182 0.894593 10.50000 0.07401 0.03927 = 0.03802 0.00251 0.00000 0.00000 CL1 5 0.143536 0.121131 0.471018 11.00000 0.13299 0.08766 = 0.08892 -0.01916 0.02166 0.02977 O1 3 0.115959 0.433474 0.695958 11.00000 0.08009 0.05601 = 0.06199 -0.00789 0.01902 -0.01831 C2 1 0.000000 0.585139 0.741167 10.50000 0.25785 0.03886 = 0.03435 0.00151 0.00000 0.00000 AFIX 23 H2A 2 0.000000 0.646775 0.797568 10.50000 -1.20000 H2B 2 0.000000 0.601323 0.634486 10.50000 -1.20000 AFIX 0 C1 1 0.114961 0.527918 0.778139 11.00000 0.14281 0.06622 = 0.05617 -0.01365 0.02227 -0.05027 AFIX 23 H1A 2 0.188481 0.566330 0.751061 11.00000 -1.20000 H1B 2 0.117918 0.515267 0.885862 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 293 in Cmc2(1) C 0.770 H 0.320 O 0.660 P 1.100 CL 0.990 N 0.700 Cl2 - P3 N2 - P2 P3 N3 - P3 P1 N1 - P2 P1 P1 - O1_$1 O1 N1 N3 P2 - N2 N1 Cl1_$1 Cl1 P3 - N3 N2 Cl2 Cl2_$1 Cl1 - P2 O1 - C1 P1 C2 - C1_$1 C1 C1 - O1 C2 Operators for generating equivalent atoms: $1 -x, y, z Floating origin restraints generated h k l Fo^2 Sigma Why rejected 2 0 1 1.40 0.30 observed but should be systematically absent 4706 Reflections read, of which 114 rejected -12 =< h =< 13, -17 =< k =< 17, -11 =< l =< 10, Max. 2-theta = 54.75 1 Systematic absence violations 0 Inconsistent equivalents 1496 Unique reflections, of which 0 suppressed R(int) = 0.0464 R(sigma) = 0.0378 Friedel opposites not merged Maximum memory for data reduction = 1124 / 17375 Special position constraints for N2 x = 0.0000 U13 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for N3 x = 0.0000 U13 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for N1 x = 0.0000 U13 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for P1 x = 0.0000 U13 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for P2 x = 0.0000 U13 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for P3 x = 0.0000 U13 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C2 x = 0.0000 U13 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Default effective X-H distances for T = 20.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 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 = 1359 / 109095 wR2 = 0.0933 before cycle 1 for 1496 data and 79 / 79 parameters GooF = S = 1.048; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 1.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44452 0.00112 -0.015 OSF Mean shift/esd = 0.070 Maximum = 0.252 for U33 N3 Max. shift = 0.001 A for C1 Max. dU = 0.000 for N2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1359 / 109095 wR2 = 0.0933 before cycle 2 for 1496 data and 79 / 79 parameters GooF = S = 1.047; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 1.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44455 0.00112 0.024 OSF Mean shift/esd = 0.022 Maximum = -0.077 for U13 Cl1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for N2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1359 / 109095 wR2 = 0.0933 before cycle 3 for 1496 data and 79 / 79 parameters GooF = S = 1.047; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 1.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44455 0.00112 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.006 for x Cl1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for Cl2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1359 / 109095 wR2 = 0.0933 before cycle 4 for 1496 data and 79 / 79 parameters GooF = S = 1.047; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 1.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44455 0.00112 -0.002 OSF Mean shift/esd = 0.000 Maximum = -0.002 for U12 Cl1 Max. shift = 0.000 A for N3 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 H2A 0.0000 0.6468 0.7976 23 0.970 0.000 C2 C1_$1 C1 H2B 0.0000 0.6013 0.6345 23 0.970 0.000 C2 C1_$1 C1 H1A 0.1884 0.5664 0.7511 23 0.970 0.000 C1 O1 C2 H1B 0.1178 0.5153 0.8859 23 0.970 0.000 C1 O1 C2 293 in Cmc2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Cl2 0.14278 0.15874 1.02523 1.00000 0.09592 0.08232 0.08616 0.00929 -0.02143 0.02645 0.08813 0.00254 0.00014 0.00010 0.00016 0.00000 0.00090 0.00074 0.00082 0.00065 0.00072 0.00069 0.00042 N2 0.00000 0.13028 0.74914 0.50000 0.17489 0.03358 0.05123 0.00223 0.00000 0.00000 0.08656 0.00717 0.00000 0.00034 0.00060 0.00000 0.00541 0.00225 0.00313 0.00198 0.00000 0.00000 0.00176 N3 0.00000 0.31316 0.87382 0.50000 0.08097 0.04139 0.03801 -0.00204 0.00000 0.00000 0.05346 0.00573 0.00000 0.00029 0.00046 0.00000 0.00314 0.00207 0.00250 0.00179 0.00000 0.00000 0.00113 N1 0.00000 0.29198 0.57123 0.50000 0.10728 0.03844 0.03598 -0.00313 0.00000 0.00000 0.06057 0.00584 0.00000 0.00031 0.00048 0.00000 0.00395 0.00195 0.00225 0.00180 0.00000 0.00000 0.00128 P1 0.00000 0.36407 0.71124 0.50000 0.05993 0.03601 0.03440 0.00043 0.00000 0.00000 0.04345 0.00157 0.00000 0.00008 0.00013 0.00000 0.00069 0.00056 0.00060 0.00049 0.00000 0.00000 0.00029 P2 0.00000 0.17634 0.58785 0.50000 0.10091 0.03981 0.03971 -0.00844 0.00000 0.00000 0.06014 0.00174 0.00000 0.00009 0.00015 0.00000 0.00118 0.00061 0.00065 0.00059 0.00000 0.00000 0.00041 P3 0.00000 0.19817 0.89461 0.50000 0.07411 0.03919 0.03799 0.00254 0.00000 0.00000 0.05043 0.00182 0.00000 0.00009 0.00015 0.00000 0.00088 0.00058 0.00062 0.00053 0.00000 0.00000 0.00033 Cl1 0.14354 0.12113 0.47099 1.00000 0.13319 0.08780 0.08871 -0.01919 0.02138 0.02983 0.10323 0.00304 0.00018 0.00010 0.00017 0.00000 0.00128 0.00082 0.00091 0.00076 0.00086 0.00078 0.00053 O1 0.11589 0.43348 0.69593 1.00000 0.08029 0.05580 0.06202 -0.00771 0.01917 -0.01827 0.06603 0.00465 0.00026 0.00019 0.00032 0.00000 0.00165 0.00149 0.00170 0.00132 0.00143 0.00128 0.00075 C2 0.00000 0.58515 0.74119 0.50000 0.25813 0.03898 0.03457 0.00163 0.00000 0.00000 0.11056 0.00879 0.00000 0.00045 0.00072 0.00000 0.01022 0.00304 0.00293 0.00242 0.00000 0.00000 0.00308 H2A 0.00000 0.64679 0.79760 0.50000 0.13268 0.00000 0.00000 H2B 0.00000 0.60134 0.63451 0.50000 0.13268 0.00000 0.00000 C1 0.11487 0.52796 0.77814 1.00000 0.14326 0.06654 0.05590 -0.01385 0.02201 -0.05027 0.08857 0.00805 0.00056 0.00033 0.00054 0.00000 0.00454 0.00298 0.00246 0.00214 0.00287 0.00300 0.00169 H1A 0.18839 0.56637 0.75109 1.00000 0.10628 0.00000 0.00000 H1B 0.11781 0.51530 0.88586 1.00000 0.10628 0.00000 0.00000 Final Structure Factor Calculation for 293 in Cmc2(1) Total number of l.s. parameters = 79 Maximum vector length = 511 Memory required = 1282 / 27090 wR2 = 0.0933 before cycle 5 for 1496 data and 2 / 79 parameters GooF = S = 1.047; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 1.07 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0366 for 1252 Fo > 4sig(Fo) and 0.0479 for all 1496 data wR2 = 0.0933, GooF = S = 1.047, Restrained GooF = 1.046 for all data Flack x parameter = -0.0176 with esd 0.1633 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 7.50 for non-hydrogen and 3.00 for hydrogen atoms Principal mean square atomic displacements U 0.1210 0.0937 0.0497 Cl2 0.1749 0.0515 0.0333 N2 0.0810 0.0424 0.0371 N3 0.1073 0.0406 0.0338 N1 0.0599 0.0361 0.0343 P1 0.1009 0.0482 0.0313 P2 0.0741 0.0412 0.0360 P3 0.1501 0.1069 0.0526 Cl1 0.1009 0.0518 0.0454 O1 0.2581 0.0395 0.0340 C2 may be split into 0.0219 0.5852 0.7412 and -0.0219 0.5852 0.7412 0.1738 0.0509 0.0409 C1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.018 0.030 0.042 0.053 0.064 0.079 0.100 0.134 0.217 1.000 Number in group 151. 148. 155. 147. 153. 143. 150. 154. 147. 148. GooF 0.896 0.963 0.979 1.118 1.005 1.089 1.177 1.154 0.981 1.073 K 1.048 1.048 0.949 0.975 1.011 1.034 1.004 1.001 1.008 1.001 Resolution(A) 0.77 0.80 0.84 0.88 0.93 0.98 1.06 1.17 1.35 1.69 inf Number in group 154. 146. 153. 145. 152. 147. 152. 149. 149. 149. GooF 0.887 0.976 1.108 1.069 0.992 1.057 1.083 0.984 0.962 1.298 K 1.008 1.014 1.039 0.987 1.035 1.007 0.997 1.003 1.008 0.999 R1 0.165 0.150 0.106 0.091 0.062 0.053 0.041 0.025 0.022 0.021 Recommended weighting scheme: WGHT 0.0400 1.0154 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) 2 2 3 1790.72 2299.94 5.02 0.238 2.41 3 9 -8 652.70 464.45 4.39 0.107 0.86 2 2 -3 1872.49 2317.50 4.30 0.239 2.41 2 6 -1 459.32 596.92 4.01 0.121 2.02 3 9 -7 481.61 356.93 3.99 0.094 0.93 9 3 4 457.79 334.81 3.50 0.091 1.02 2 4 0 834.88 685.35 3.43 0.130 2.85 9 9 0 44.20 13.72 3.18 0.018 0.93 6 6 -6 70.37 117.01 3.02 0.054 1.01 0 16 1 427.08 292.51 3.01 0.085 0.84 9 3 0 26.33 2.08 2.98 0.007 1.15 11 5 -1 80.06 129.71 2.87 0.057 0.91 11 1 -3 45.82 84.26 2.87 0.046 0.92 5 1 2 301.54 239.77 2.85 0.077 1.90 7 1 1 1383.36 1170.65 2.80 0.170 1.49 7 3 0 2922.31 2559.07 2.71 0.251 1.44 9 7 0 159.97 107.04 2.69 0.051 1.01 8 0 -4 55.62 88.29 2.67 0.047 1.14 10 10 1 69.31 115.94 2.65 0.054 0.83 2 6 1 499.71 608.97 2.63 0.123 2.02 3 3 1 1917.02 1693.57 2.61 0.205 2.66 3 9 0 219.87 170.14 2.60 0.065 1.38 6 4 -8 281.82 213.78 2.60 0.073 0.91 4 6 7 681.62 551.24 2.59 0.117 1.02 3 9 8 583.00 458.76 2.56 0.106 0.86 5 3 -5 224.95 281.12 2.54 0.083 1.30 7 9 -4 214.36 272.54 2.53 0.082 0.96 1 5 10 138.14 236.34 2.52 0.076 0.84 3 11 -7 59.55 99.24 2.49 0.050 0.85 4 0 -10 295.34 225.12 2.49 0.075 0.84 11 1 5 38.74 79.62 2.49 0.044 0.85 0 2 -10 44.78 84.03 2.48 0.046 0.88 5 1 6 52.20 81.81 2.47 0.045 1.21 7 1 -8 36.48 68.93 2.47 0.041 0.89 3 9 7 438.41 355.70 2.43 0.094 0.93 3 1 -6 723.17 841.36 2.43 0.144 1.36 4 4 -7 381.26 455.32 2.43 0.106 1.08 2 6 -9 255.10 191.55 2.41 0.069 0.89 0 4 -5 922.28 1062.13 2.38 0.162 1.57 7 9 4 214.43 272.50 2.31 0.082 0.96 6 6 5 255.06 314.43 2.29 0.088 1.10 0 4 -10 122.98 78.76 2.29 0.044 0.86 6 2 0 4646.20 4190.08 2.27 0.322 1.72 7 7 2 995.64 853.42 2.25 0.145 1.15 3 3 -1 1863.43 1657.56 2.25 0.202 2.66 3 5 -7 592.60 511.12 2.22 0.112 1.09 5 1 0 146.22 113.27 2.21 0.053 2.11 4 6 -7 648.84 562.80 2.19 0.118 1.02 10 4 -5 9.46 37.91 2.17 0.031 0.88 12 4 1 27.99 1.85 2.16 0.007 0.86 Bond lengths and angles Cl2 - Distance Angles P3 1.9852 (0.0015) Cl2 - N2 - Distance Angles P2 1.5581 (0.0054) P3 1.5810 (0.0054) 121.10 (0.30) N2 - P2 N3 - Distance Angles P3 1.5620 (0.0042) P1 1.5957 (0.0042) 122.26 (0.27) N3 - P3 N1 - Distance Angles P2 1.5668 (0.0043) P1 1.5761 (0.0043) 122.70 (0.28) N1 - P2 P1 - Distance Angles O1_$1 1.5566 (0.0026) O1 1.5566 (0.0026) 105.14 (0.23) N1 1.5761 (0.0043) 107.61 (0.14) 107.61 (0.14) N3 1.5957 (0.0042) 109.72 (0.15) 109.72 (0.15) 116.42 (0.21) P1 - O1_$1 O1 N1 P2 - Distance Angles N2 1.5581 (0.0054) N1 1.5668 (0.0043) 118.89 (0.25) Cl1_$1 1.9925 (0.0017) 109.12 (0.12) 108.86 (0.11) Cl1 1.9925 (0.0017) 109.12 (0.12) 108.86 (0.11) 100.41 (0.12) P2 - N2 N1 Cl1_$1 P3 - Distance Angles N3 1.5620 (0.0042) N2 1.5810 (0.0054) 118.63 (0.24) Cl2 1.9852 (0.0015) 109.56 (0.11) 108.66 (0.12) Cl2_$1 1.9852 (0.0015) 109.56 (0.11) 108.66 (0.12) 100.19 (0.11) P3 - N3 N2 Cl2 Cl1 - Distance Angles P2 1.9925 (0.0017) Cl1 - O1 - Distance Angles C1 1.4679 (0.0050) P1 1.5566 (0.0026) 118.24 (0.27) O1 - C1 C2 - Distance Angles C1_$1 1.4843 (0.0065) C1 1.4843 (0.0065) 111.25 (0.51) C2 - C1_$1 C1 - Distance Angles O1 1.4679 (0.0050) C2 1.4843 (0.0065) 110.36 (0.46) C1 - O1 FMAP and GRID set by program FMAP 2 1 15 GRID -2.083 -1 -2 2.083 1 2 R1 = 0.0418 for 807 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.28 at 0.1502 0.1649 0.9219 [ 0.92 A from CL2 ] Deepest hole -0.25 at 0.2141 0.1633 0.4400 [ 0.98 A from CL1 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 1561 / 17682 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1502 0.1649 0.9219 1.00000 0.05 0.28 0.92 CL2 1.68 P3 2.26 N2 2.60 N3 Q2 1 0.1418 0.1063 0.5790 1.00000 0.05 0.23 0.98 CL1 1.79 P2 2.16 N2 2.43 H1A Q3 1 0.1849 0.1136 0.4605 1.00000 0.05 0.21 0.46 CL1 2.42 P2 2.81 H1B 2.98 H1A Q4 1 0.0000 0.6270 0.5115 0.50000 0.05 0.21 1.14 H2B 1.46 N3 2.11 C2 2.55 H2A Q5 1 0.0000 0.3293 0.7930 0.50000 0.05 0.20 0.75 N3 0.86 P1 1.99 P3 2.03 N1 Q6 1 0.1514 0.1752 0.5291 1.00000 0.05 0.20 0.90 CL1 1.70 P2 2.29 N1 2.60 N2 Q7 1 0.0000 0.3289 0.6184 0.50000 0.05 0.20 0.65 N1 0.95 P1 2.00 O1 2.08 P2 Q8 1 0.0000 0.0684 1.2012 0.50000 0.05 0.17 2.50 CL2 2.71 N2 2.93 CL1 3.23 P3 Q9 1 0.0000 0.1676 0.7099 0.50000 0.05 0.17 0.61 N2 1.09 P2 1.69 P3 2.08 N1 Q10 1 0.0000 0.0900 1.0281 0.50000 0.05 0.17 1.78 CL2 1.88 P3 2.53 N2 3.27 CL1 Q11 1 0.0000 0.1763 0.8195 0.50000 0.05 0.16 0.73 P3 0.88 N2 1.91 N3 2.05 P2 Q12 1 0.1450 0.0330 0.9069 1.00000 0.05 0.16 1.99 CL2 2.16 CL1 2.29 H1A 2.46 N2 Q13 1 0.0000 0.2487 0.5819 0.50000 0.05 0.16 0.59 N1 0.98 P2 1.93 P1 2.18 N2 Q14 1 0.0000 0.1594 0.4542 0.50000 0.05 0.16 1.21 P2 1.62 CL1 2.07 N1 2.64 N2 Q15 1 0.0000 0.0773 0.7183 0.50000 0.05 0.15 0.77 N2 1.77 P2 2.26 P3 2.74 CL1 Q16 1 0.0000 0.0420 0.6986 0.50000 0.05 0.15 1.27 N2 2.06 P2 2.73 P3 2.75 CL1 Q17 1 0.1744 0.1745 0.6370 1.00000 0.05 0.15 1.67 CL1 1.91 P2 2.19 N2 2.30 H1A Q18 1 0.0000 0.1962 1.0209 0.50000 0.05 0.15 1.12 P3 1.60 CL2 2.05 N3 2.57 N2 Q19 1 0.2688 0.5012 0.7215 1.00000 0.05 0.15 1.26 H1A 1.75 C1 1.88 O1 2.18 H1B Q20 1 0.1630 0.5106 0.6586 1.00000 0.05 0.15 1.15 H1A 1.20 C1 1.20 O1 2.07 H1B Shortest distances between peaks (including symmetry equivalents) 15 16 0.51 9 11 0.98 6 17 0.99 2 6 1.03 3 6 1.09 2 17 1.11 7 13 1.13 2 3 1.15 9 15 1.22 19 20 1.26 10 18 1.43 8 16 1.49 5 7 1.55 8 10 1.56 9 13 1.58 11 15 1.61 13 14 1.65 9 16 1.70 6 14 1.76 3 17 1.77 1 12 1.78 11 18 1.80 1 11 1.85 1 18 1.87 12 19 1.93 6 13 1.95 8 15 1.97 9 17 1.97 2 15 1.99 2 14 2.01 4 5 2.02 10 12 2.03 2 16 2.04 3 14 2.07 2 9 2.08 5 11 2.08 3 12 2.08 11 16 2.10 1 10 2.12 2 19 2.12 5 13 2.16 13 17 2.17 10 11 2.18 9 14 2.27 6 9 2.28 5 9 2.30 11 13 2.32 7 9 2.32 10 16 2.33 8 18 2.35 12 15 2.35 4 18 2.39 15 17 2.39 12 16 2.41 2 12 2.42 2 13 2.45 11 17 2.46 1 9 2.47 14 17 2.47 17 19 2.53 16 19 2.53 1 17 2.54 2 20 2.55 8 14 2.56 14 15 2.59 11 12 2.59 13 15 2.61 16 17 2.64 8 19 2.64 3 19 2.67 15 19 2.67 6 15 2.68 4 20 2.68 14 16 2.68 1 15 2.69 5 18 2.70 7 14 2.71 7 11 2.72 6 7 2.74 10 15 2.75 8 12 2.75 3 20 2.76 2 11 2.78 9 18 2.78 7 17 2.80 3 19 2.81 10 15 2.82 17 20 2.82 6 16 2.84 12 18 2.87 3 13 2.89 9 12 2.95 1 19 2.96 1 5 2.96 12 19 2.97 13 16 2.97 10 16 2.99 Time profile in seconds ----------------------- 0.07: 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. 0.75: 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 0.34: Structure factors and derivatives 0.20: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.12: Solve l.s. equations 0.00: Generate HTAB table 0.01: Other dependent quantities, CIF, tables 0.04: Analysis of variance 0.01: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 293 finished at 13:55:26 Total CPU time: 1.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++