+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 14:47:54 on 04-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SOT119 in Cmc2(1) CELL 0.71073 15.0935 9.0070 10.3253 90.000 90.000 90.000 ZERR 8.00 0.0024 0.0012 0.0016 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 N CL UNIT 48 88 12 4 V = 1403.70 F(000) = 528.0 Mu = 0.25 mm-1 Cell Wt = 975.10 Rho = 1.154 MERG 2 OMIT -3.00 55.00 EXTI 0.00398 EQIV $1 -X+2, Y, Z EQIV $2 -X, Y, Z FREE C7 C7_$1 FREE C7 C7_$2 FMAP 2 PLAN 10 SIZE 0.04 0.20 0.24 HTAB N1 CL1 BOND $H WGHT 0.07570 0.37710 L.S. 4 TEMP -153.00 FVAR 0.41367 H1N 2 0.598619 1.034941 0.551033 11.00000 0.05087 MOLE 1 CL1 4 0.500000 0.788500 0.971868 10.50000 0.04526 0.02486 = 0.03915 -0.00065 0.00000 0.00000 MOLE 2 C1 1 0.757655 0.825067 0.546056 11.00000 0.04422 0.03655 = 0.05086 -0.00466 0.00098 0.00913 AFIX 43 H1 2 0.809988 0.782718 0.510723 11.00000 -1.20000 AFIX 0 C2 1 0.709521 0.938832 0.494589 11.00000 0.04397 0.02808 = 0.04844 -0.00074 0.00368 -0.00024 AFIX 43 H2 2 0.722461 0.990168 0.416474 11.00000 -1.20000 AFIX 0 N1 3 0.640505 0.965715 0.573716 11.00000 0.04741 0.02659 = 0.04785 -0.00208 -0.00072 0.00586 C4 1 0.642720 0.869067 0.677191 11.00000 0.06021 0.04167 = 0.03762 0.00222 0.00533 0.00172 AFIX 43 H4 2 0.601253 0.864455 0.746291 11.00000 -1.20000 AFIX 0 C3 1 0.714906 0.782148 0.661914 11.00000 0.06256 0.04196 = 0.04439 0.01315 -0.00339 0.00977 AFIX 43 H3 2 0.733635 0.705631 0.719015 11.00000 -1.20000 AFIX 0 MOLE 3 C5 1 0.000000 0.695125 0.825654 10.50000 0.14175 0.01695 = 0.05058 -0.00148 0.00000 0.00000 AFIX 137 H5A 2 -0.011163 0.682162 0.732841 10.50000 -1.50000 H5B 2 -0.046544 0.644965 0.875300 10.50000 -1.50000 H5C 2 0.057707 0.652161 0.847742 10.50000 -1.50000 AFIX 0 C6 1 -0.077542 0.927675 0.801251 11.00000 0.04804 0.05284 = 0.18627 -0.02777 -0.00274 0.00550 AFIX 137 H6A 2 -0.075104 1.034979 0.816547 11.00000 -1.50000 H6B 2 -0.131190 0.886852 0.841130 11.00000 -1.50000 H6C 2 -0.078638 0.908467 0.707843 11.00000 -1.50000 AFIX 0 C7 1 -0.036641 0.878231 0.995716 10.50000 0.09250 0.03166 = 0.02781 -0.00260 0.00617 0.00502 AFIX 137 H7A 2 0.000586 0.823762 1.057275 10.50000 -1.50000 H7B 2 -0.097385 0.840077 0.999742 10.50000 -1.50000 H7C 2 -0.036477 0.984008 1.017946 10.50000 -1.50000 AFIX 0 N2 3 0.000000 0.857589 0.857933 10.50000 0.09051 0.02104 = 0.03007 0.00150 0.00000 0.00000 HKLF 4 1.0 0.00 1.00 0.00 1.00 0.00 0.00 0.00 0.00 -1.00 Covalent radii and connectivity table for 01SOT119 in Cmc2(1) C 0.770 H 0.320 N 0.700 CL 0.990 Cl1 - no bonds found C1 - C2 C3 C2 - N1 C1 N1 - C2 C4 C4 - C3 N1 C3 - C4 C1 C5 - N2 C6 - N2 C7 - N2 N2 - C6_$2 C6 C5 C7_$2 C7 Operators for generating equivalent atoms: $1 -x+2, y, z $2 -x, y, z Floating origin restraints generated h k l Fo^2 Sigma Why rejected 0 0 -5 8.67 1.09 observed but should be systematically absent 4017 Reflections read, of which 90 rejected -19 =< h =< 19, -10 =< k =< 11, -13 =< l =< 11, Max. 2-theta = 54.97 1 Systematic absence violations 0 Inconsistent equivalents 1465 Unique reflections, of which 0 suppressed R(int) = 0.0851 R(sigma) = 0.0928 Friedel opposites not merged Maximum memory for data reduction = 1438 / 17531 Special position constraints for Cl1 x = 0.5000 U13 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C5 x = 0.0000 U13 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for N2 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 = -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 = 1732 / 119250 wR2 = 0.1558 before cycle 1 for 1465 data and 90 / 90 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0757 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41381 0.00220 0.064 OSF 2 0.00406 0.00307 0.027 EXTI Mean shift/esd = 0.013 Maximum = 0.064 for OSF Max. shift = 0.002 A for H5B Max. dU = 0.000 for C5 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1732 / 119250 wR2 = 0.1558 before cycle 2 for 1465 data and 90 / 90 parameters GooF = S = 1.056; Restrained GooF = 1.055 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0757 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41383 0.00220 0.009 OSF 2 0.00409 0.00308 0.007 EXTI Mean shift/esd = 0.004 Maximum = 0.017 for U11 Cl1 Max. shift = 0.001 A for H5B Max. dU = 0.000 for C5 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1732 / 119250 wR2 = 0.1558 before cycle 3 for 1465 data and 90 / 90 parameters GooF = S = 1.056; Restrained GooF = 1.055 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0757 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41383 0.00220 0.000 OSF 2 0.00409 0.00308 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for U11 H1N Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1732 / 119250 wR2 = 0.1558 before cycle 4 for 1465 data and 90 / 90 parameters GooF = S = 1.056; Restrained GooF = 1.055 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0757 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41383 0.00220 0.000 OSF 2 0.00408 0.00308 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for U11 H1N Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Largest correlation matrix elements 0.527 U22 Cl1 / OSF 0.525 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.8100 0.7827 0.5107 43 0.950 0.000 C1 C2 C3 H2 0.7225 0.9902 0.4165 43 0.950 0.000 C2 N1 C1 H4 0.6012 0.8645 0.7463 43 0.950 0.000 C4 C3 N1 H3 0.7337 0.7057 0.7190 43 0.950 0.000 C3 C4 C1 H5A -0.0113 0.6822 0.7329 137 0.980 0.000 C5 N2 H5A H5B -0.0464 0.6449 0.8755 137 0.980 0.000 C5 N2 H5A H5C 0.0578 0.6522 0.8475 137 0.980 0.000 C5 N2 H5A H6A -0.0752 1.0350 0.8166 137 0.980 0.000 C6 N2 H6A H6B -0.1312 0.8868 0.8411 137 0.980 0.000 C6 N2 H6A H6C -0.0786 0.9085 0.7078 137 0.980 0.000 C6 N2 H6A H7A 0.0006 0.8237 1.0573 137 0.980 0.000 C7 N2 H7A H7B -0.0974 0.8401 0.9997 137 0.980 0.000 C7 N2 H7A H7C -0.0364 0.9840 1.0180 137 0.980 0.000 C7 N2 H7A 01SOT119 in Cmc2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq H1N 0.59862 1.03480 0.55112 1.00000 0.05083 0.07447 0.00316 0.00483 0.00442 0.00000 0.01169 Cl1 0.50000 0.78850 0.97187 0.50000 0.04531 0.02485 0.03918 -0.00065 0.00000 0.00000 0.03645 0.00142 0.00000 0.00011 0.00010 0.00000 0.00073 0.00051 0.00063 0.00051 0.00000 0.00000 0.00038 C1 0.75766 0.82506 0.54605 1.00000 0.04424 0.03654 0.05093 -0.00466 0.00092 0.00913 0.04390 0.00703 0.00026 0.00037 0.00044 0.00000 0.00241 0.00167 0.00235 0.00177 0.00200 0.00170 0.00094 H1 0.80999 0.78270 0.51071 1.00000 0.05269 0.00000 0.00000 C2 0.70953 0.93883 0.49458 1.00000 0.04400 0.02809 0.04849 -0.00074 0.00369 -0.00023 0.04019 0.00632 0.00027 0.00033 0.00037 0.00000 0.00220 0.00152 0.00276 0.00152 0.00190 0.00135 0.00099 H2 0.72247 0.99017 0.41647 1.00000 0.04823 0.00000 0.00000 N1 0.64051 0.96571 0.57372 1.00000 0.04743 0.02658 0.04789 -0.00209 -0.00069 0.00587 0.04064 0.00530 0.00023 0.00032 0.00033 0.00000 0.00205 0.00146 0.00195 0.00126 0.00162 0.00140 0.00080 C4 0.64271 0.86907 0.67720 1.00000 0.06024 0.04165 0.03761 0.00222 0.00534 0.00171 0.04650 0.00711 0.00030 0.00043 0.00037 0.00000 0.00290 0.00216 0.00224 0.00161 0.00181 0.00187 0.00108 H4 0.60123 0.86445 0.74629 1.00000 0.05580 0.00000 0.00000 C3 0.71492 0.78216 0.66191 1.00000 0.06254 0.04196 0.04429 0.01314 -0.00336 0.00978 0.04960 0.00798 0.00032 0.00044 0.00042 0.00000 0.00307 0.00215 0.00250 0.00170 0.00206 0.00204 0.00109 H3 0.73367 0.70566 0.71902 1.00000 0.05952 0.00000 0.00000 C5 0.00000 0.69514 0.82568 0.50000 0.14151 0.01690 0.05067 -0.00155 0.00000 0.00000 0.06969 0.00842 0.00000 0.00052 0.00072 0.00000 0.00749 0.00246 0.00366 0.00215 0.00000 0.00000 0.00233 H5A -0.01133 0.68216 0.73291 0.50000 0.10454 0.00000 0.00000 H5B -0.04643 0.64494 0.87551 0.50000 0.10454 0.00000 0.00000 H5C 0.05776 0.65224 0.84754 0.50000 0.10454 0.00000 0.00000 C6 -0.07755 0.92766 0.80126 1.00000 0.04802 0.05286 0.18625 -0.02789 -0.00276 0.00544 0.09571 0.01012 0.00035 0.00053 0.00080 0.00000 0.00309 0.00280 0.00770 0.00365 0.00364 0.00225 0.00246 H6A -0.07516 1.03495 0.81662 1.00000 0.14356 0.00000 0.00000 H6B -0.13120 0.88675 0.84108 1.00000 0.14356 0.00000 0.00000 H6C -0.07862 0.90853 0.70784 1.00000 0.14356 0.00000 0.00000 C7 -0.03663 0.87822 0.99571 0.50000 0.09228 0.03172 0.02780 -0.00264 0.00615 0.00506 0.05060 0.01418 0.00066 0.00077 0.00063 0.00000 0.00704 0.00308 0.00436 0.00270 0.00342 0.00314 0.00245 H7A 0.00058 0.82370 1.05725 0.50000 0.07590 0.00000 0.00000 H7B -0.09738 0.84012 0.99972 0.50000 0.07590 0.00000 0.00000 H7C -0.03643 0.98399 1.01796 0.50000 0.07590 0.00000 0.00000 N2 0.00000 0.85759 0.85794 0.50000 0.09053 0.02099 0.03007 0.00147 0.00000 0.00000 0.04720 0.00591 0.00000 0.00043 0.00043 0.00000 0.00416 0.00196 0.00239 0.00170 0.00000 0.00000 0.00130 Final Structure Factor Calculation for 01SOT119 in Cmc2(1) Total number of l.s. parameters = 90 Maximum vector length = 511 Memory required = 1644 / 25046 wR2 = 0.1558 before cycle 5 for 1465 data and 2 / 90 parameters GooF = S = 1.056; Restrained GooF = 1.055 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0757 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0617 for 1092 Fo > 4sig(Fo) and 0.0900 for all 1465 data wR2 = 0.1558, GooF = S = 1.056, Restrained GooF = 1.055 for all data Flack x parameter = -0.1371 with esd 0.1346 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 = 8.00 for non-hydrogen and 11.00 for hydrogen atoms Principal mean square atomic displacements U 0.0453 0.0392 0.0248 Cl1 0.0530 0.0491 0.0296 C1 0.0506 0.0419 0.0281 C2 0.0498 0.0472 0.0249 N1 0.0617 0.0420 0.0358 C4 0.0666 0.0548 0.0273 C3 0.1415 0.0507 0.0168 C5 0.1919 0.0524 0.0428 C6 0.0932 0.0330 0.0256 C7 0.0905 0.0303 0.0208 N2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.033 0.046 0.058 0.073 0.087 0.104 0.131 0.166 0.240 1.000 Number in group 159. 137. 148. 142. 157. 137. 149. 142. 149. 145. GooF 0.981 1.001 1.128 0.978 1.127 1.114 1.077 0.987 0.974 1.164 K 0.978 1.138 1.044 0.990 0.998 1.015 1.007 0.987 1.012 1.021 Resolution(A) 0.77 0.80 0.84 0.88 0.93 1.00 1.07 1.19 1.36 1.69 inf Number in group 149. 145. 158. 134. 148. 145. 147. 148. 146. 145. GooF 0.951 1.000 0.999 1.133 1.016 1.091 0.962 1.014 1.098 1.269 K 0.976 1.080 1.025 1.019 1.025 1.025 1.001 1.027 1.033 1.007 R1 0.270 0.223 0.168 0.136 0.093 0.081 0.055 0.048 0.048 0.048 Recommended weighting scheme: WGHT 0.0754 0.3949 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 4 0 295.21 193.16 3.83 0.109 2.16 0 0 -10 1434.17 1066.92 3.34 0.257 1.03 2 2 -12 112.92 42.80 3.26 0.051 0.84 18 2 -1 172.91 42.92 3.22 0.051 0.82 1 5 -1 234.87 170.26 3.22 0.103 1.76 8 0 -10 159.05 297.67 3.09 0.136 0.91 7 1 -8 247.96 362.86 3.09 0.150 1.10 9 1 -1 295.63 412.87 3.01 0.160 1.63 5 3 -11 72.79 19.71 2.92 0.035 0.86 3 9 1 45.68 88.50 2.91 0.074 0.98 1 5 1 236.71 170.01 2.88 0.102 1.76 0 2 -11 141.70 94.40 2.86 0.076 0.92 0 2 0 1445.58 1115.32 2.85 0.262 4.50 1 1 -8 260.88 198.21 2.73 0.111 1.27 11 3 -8 27.32 94.83 2.61 0.077 0.90 3 7 -5 53.34 25.00 2.61 0.039 1.07 3 1 -3 794.00 1010.37 2.60 0.250 2.71 7 1 1 589.77 772.82 2.59 0.219 2.06 10 2 2 95.37 134.51 2.58 0.091 1.38 6 6 6 -6.97 19.37 2.51 0.035 1.03 0 4 9 645.04 865.12 2.50 0.231 1.02 17 1 1 314.80 218.21 2.49 0.116 0.88 5 9 3 23.23 66.75 2.46 0.064 0.92 7 3 7 23.36 0.04 2.44 0.002 1.13 2 4 1 2071.81 1680.23 2.44 0.322 2.11 5 3 10 0.00 47.75 2.38 0.054 0.93 17 5 0 86.10 18.20 2.36 0.034 0.80 9 1 1 310.62 405.01 2.30 0.158 1.63 11 7 -2 172.10 113.67 2.30 0.084 0.92 10 4 -9 4.95 48.22 2.30 0.055 0.85 0 2 -2 3.96 16.14 2.29 0.032 3.39 0 4 5 139.05 198.03 2.26 0.111 1.52 17 1 -2 124.97 46.92 2.26 0.054 0.87 4 0 6 2574.31 1984.04 2.26 0.350 1.57 5 7 3 13.05 36.90 2.24 0.048 1.12 15 3 6 -38.72 35.34 2.23 0.047 0.83 3 1 5 4655.31 3779.77 2.23 0.483 1.87 16 2 1 66.31 20.16 2.22 0.035 0.92 2 2 6 655.34 808.27 2.21 0.223 1.57 3 1 -2 1814.13 2289.77 2.21 0.376 3.35 10 2 10 45.20 120.79 2.20 0.086 0.84 14 0 4 69.61 131.21 2.19 0.090 0.99 1 3 7 214.33 291.17 2.18 0.134 1.32 2 4 5 148.38 188.79 2.17 0.108 1.49 16 6 -1 154.52 72.62 2.16 0.067 0.80 9 1 2 116.24 156.37 2.15 0.098 1.57 16 2 -4 145.09 92.86 2.10 0.076 0.87 4 2 -2 1348.42 1634.34 2.10 0.318 2.52 1 5 0 4555.05 3824.97 2.09 0.486 1.79 15 7 -2 169.42 100.28 2.08 0.079 0.78 Bond lengths and angles C1 - Distance Angles C2 1.3640 (0.0049) C3 1.4130 (0.0063) 106.99 (0.36) H1 0.9500 126.51 126.51 C1 - C2 C3 C2 - Distance Angles N1 1.3459 (0.0052) C1 1.3640 (0.0049) 108.11 (0.33) H2 0.9500 125.94 125.94 C2 - N1 C1 N1 - Distance Angles C2 1.3459 (0.0053) C4 1.3785 (0.0049) 109.78 (0.32) H1N 0.9173 (0.0485) 120.07 (2.83) 129.95 (2.83) N1 - C2 C4 C4 - Distance Angles C3 1.3512 (0.0063) N1 1.3785 (0.0049) 107.14 (0.36) H4 0.9500 126.43 126.43 C4 - C3 N1 C3 - Distance Angles C4 1.3512 (0.0063) C1 1.4130 (0.0063) 107.98 (0.36) H3 0.9500 126.01 126.01 C3 - C4 C1 C5 - Distance Angles N2 1.5007 (0.0059) H5A 0.9800 109.47 H5B 0.9800 109.47 109.47 H5C 0.9800 109.47 109.47 109.47 C5 - N2 H5A H5B C6 - Distance Angles N2 1.4530 (0.0061) H6A 0.9800 109.47 H6B 0.9800 109.47 109.47 H6C 0.9800 109.47 109.47 109.47 C6 - N2 H6A H6B C7 - Distance Angles N2 1.5374 (0.0078) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - N2 H7A H7B N2 - Distance Angles C6_$2 1.4530 (0.0062) C6 1.4530 (0.0062) 107.35 (0.60) C5 1.5007 (0.0059) 109.52 (0.32) 109.52 (0.32) C7_$2 1.5374 (0.0078) 91.75 (0.48) 127.59 (0.51) 108.86 (0.46) C7 1.5374 (0.0078) 127.59 (0.51) 91.75 (0.47) 108.86 (0.46) 42.15 (0.74) N2 - C6_$2 C6 C5 C7_$2 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) ** No suitable H-bond found for N1...Cl1 = 4.893(4) A ** FMAP and GRID set by program FMAP 2 2 13 GRID -2.500 -2 -1 2.500 2 1 R1 = 0.0813 for 866 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.52 at 0.4375 0.2143 0.4718 [ 0.94 A from CL1 ] Deepest hole -0.42 at 0.0000 0.1938 0.9732 [ 0.85 A from CL1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 1999 / 19003 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5625 0.7857 0.9718 1.00000 0.05 0.52 0.94 CL1 1.89 H1N 2.06 H1 2.50 H4 Q2 1 0.0000 0.7239 0.6458 0.50000 0.05 0.32 0.99 H5A 1.80 CL1 1.88 C5 2.14 H6C Q3 1 0.0000 0.6538 0.6418 0.50000 0.05 0.26 0.99 H5A 1.83 CL1 1.94 C5 2.06 H1N Q4 1 0.5000 0.7728 0.7998 0.50000 0.05 0.26 1.78 CL1 1.82 H4 2.43 H6A 2.64 C4 Q5 1 0.5000 0.8427 0.8024 0.50000 0.05 0.22 1.65 H4 1.82 CL1 2.52 C4 2.91 H5B Q6 1 -0.0826 0.9603 0.7706 1.00000 0.05 0.22 0.44 C6 0.80 H6C 0.83 H6A 1.23 H6B Q7 1 -0.0783 0.8974 0.8690 1.00000 0.05 0.22 0.75 C6 0.85 H6B 1.24 N2 1.35 H6A Q8 1 0.5000 0.8139 1.0360 0.50000 0.05 0.21 0.70 CL1 2.02 H1N 2.04 H5A 2.93 H6C Q9 1 0.0000 0.8233 0.6781 0.50000 0.05 0.20 1.40 H5A 1.45 H6C 1.88 N2 1.91 C5 Q10 1 0.6518 0.9155 0.4842 1.00000 0.05 0.20 0.90 C2 1.04 N1 1.44 H2 1.51 H1N Shortest distances between peaks (including symmetry equivalents) 4 5 0.63 2 3 0.63 2 9 0.95 3 8 1.13 6 7 1.16 1 8 1.18 2 8 1.18 3 9 1.57 1 1 1.89 8 9 1.92 6 9 2.00 1 4 2.01 1 2 2.03 1 5 2.05 1 3 2.07 7 7 2.36 7 9 2.39 5 8 2.43 4 8 2.47 6 6 2.49 1 9 2.53 6 7 2.69 2 6 2.78 Time profile in seconds ----------------------- 0.22: 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. 0.61: 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 0.44: Structure factors and derivatives 0.17: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.11: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 14:47:56 Total CPU time: 1.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++