+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0003cmcm started at 15:11:19 on 21-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0003cmcm in Cmcm CELL 0.71073 6.8156 12.7537 14.1899 90.000 90.000 90.000 ZERR 8.00 0.0006 0.0012 0.0011 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 O UNIT 40 72 8 20 V = 1233.44 F(000) = 528.0 Mu = 0.11 mm-1 Cell Wt = 985.06 Rho = 1.326 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB O1A O22 HTAB N21 O1B EQIV_$1 x, y, -z+3/2 MPLA C1 O1A O1B MPLA C1_$1 O1A_$1 O1B_$1 FMAP 2 PLAN 10 SIZE 0.01 0.07 0.15 ACTA BOND $H WGHT 0.02150 2.19400 L.S. 4 TEMP -153.00 FVAR 0.64747 MOLE 1 C1 1 0.000000 0.304079 0.485150 10.50000 0.02873 0.02723 = 0.02252 0.00113 0.00000 0.00000 C2 1 0.000000 0.375014 0.569749 10.50000 0.03129 0.02432 = 0.02233 0.00133 0.00000 0.00000 AFIX 23 H2A 2 -0.117421 0.420641 0.567514 10.50000 -1.20000 H2B 2 0.117421 0.420641 0.567514 10.50000 -1.20000 AFIX 0 C3 1 0.000000 0.314082 0.661751 10.50000 0.03038 0.02169 = 0.01921 0.00113 0.00000 0.00000 AFIX 23 H3A 2 0.117237 0.268285 0.663305 10.50000 -1.20000 H3B 2 -0.117237 0.268285 0.663305 10.50000 -1.20000 AFIX 0 C4 1 0.000000 0.383054 0.750000 10.25000 0.02864 0.02505 = 0.02091 0.00000 0.00000 0.00000 AFIX 23 H4A 2 -0.117654 0.428577 0.750000 10.25000 -1.20000 H4B 2 0.117654 0.428577 0.750000 10.25000 -1.20000 AFIX 0 O1B 4 0.000000 0.209106 0.489863 10.50000 0.06095 0.02364 = 0.02395 -0.00055 0.00000 0.00000 O1A 4 0.000000 0.356541 0.404221 10.50000 0.05321 0.02476 = 0.01879 -0.00049 0.00000 0.00000 AFIX 83 H1 2 0.000000 0.313939 0.359075 10.50000 -1.50000 AFIX 0 MOLE 2 C22 1 0.000000 0.139895 0.250000 10.25000 0.02789 0.02093 = 0.02584 0.00000 0.00000 0.00000 C25 1 0.000000 -0.031460 0.304456 10.50000 0.04588 0.02217 = 0.03361 0.00063 0.00000 0.00000 AFIX 23 H25A 2 -0.118337 -0.066671 0.329662 10.50000 -1.20000 H25B 2 0.118337 -0.066671 0.329662 10.50000 -1.20000 AFIX 0 N21 3 0.000000 0.079814 0.327414 10.50000 0.04040 0.02276 = 0.02350 -0.00013 0.00000 0.00000 AFIX 43 H21 2 0.000000 0.104638 0.385277 10.50000 -1.20000 AFIX 0 O22 4 0.000000 0.239214 0.250000 10.25000 0.03748 0.02089 = 0.02024 0.00000 0.00000 0.00000 HKLF 4 Covalent radii and connectivity table for 07skc0003cmcm in Cmcm C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - C1 C3 C3 - C2 C4 C4 - C3 C3_$1 O1B - C1 O1A - C1 C22 - O22 N21_$2 N21 C25 - N21 C25_$2 N21 - C22 C25 O22 - C22 Operators for generating equivalent atoms: $1 x, y, -z+3/2 $2 x, y, -z+1/2 4648 Reflections read, of which 109 rejected -8 =< h =< 8, -16 =< k =< 11, -18 =< l =< 16, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 800 Unique reflections, of which 0 suppressed R(int) = 0.0636 R(sigma) = 0.0490 Friedel opposites merged Maximum memory for data reduction = 1413 / 9183 Special position constraints for C1 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 Special position constraints for C3 x = 0.0000 U13 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C4 x = 0.0000 z = 0.7500 U23 = 0 U13 = 0 U12 = 0 sof = 0.25000 Input constraints retained (at least in part) for sof Special position constraints for O1B x = 0.0000 U13 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O1A x = 0.0000 U13 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C22 x = 0.0000 z = 0.2500 U23 = 0 U13 = 0 U12 = 0 sof = 0.25000 Input constraints retained (at least in part) for sof Special position constraints for C25 x = 0.0000 U13 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for N21 x = 0.0000 U13 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O22 x = 0.0000 z = 0.2500 U23 = 0 U13 = 0 U12 = 0 sof = 0.25000 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 = 1648 / 80855 wR2 = 0.1284 before cycle 1 for 800 data and 55 / 55 parameters GooF = S = 1.170; Restrained GooF = 1.170 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0215 * P )^2 + 2.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64748 0.00270 0.003 OSF Mean shift/esd = 0.005 Maximum = 0.013 for y O1A Max. shift = 0.000 A for C4 Max. dU = 0.000 for C22 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1648 / 80855 wR2 = 0.1285 before cycle 2 for 800 data and 55 / 55 parameters GooF = S = 1.170; Restrained GooF = 1.170 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0215 * P )^2 + 2.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64748 0.00270 -0.001 OSF Mean shift/esd = 0.002 Maximum = 0.005 for y O1A Max. shift = 0.000 A for C4 Max. dU = 0.000 for C4 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1648 / 80855 wR2 = 0.1285 before cycle 3 for 800 data and 55 / 55 parameters GooF = S = 1.170; Restrained GooF = 1.170 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0215 * P )^2 + 2.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64748 0.00270 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U11 N21 Max. shift = 0.000 A for C4 Max. dU = 0.000 for N21 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1648 / 80855 wR2 = 0.1285 before cycle 4 for 800 data and 55 / 55 parameters GooF = S = 1.170; Restrained GooF = 1.170 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0215 * P )^2 + 2.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64748 0.00270 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C2 Max. shift = 0.000 A for C2 Max. dU = 0.000 for N21 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 -0.1174 0.4206 0.5675 23 0.990 0.000 C2 C1 C3 H2B 0.1174 0.4206 0.5675 23 0.990 0.000 C2 C1 C3 H3A 0.1172 0.2683 0.6633 23 0.990 0.000 C3 C2 C4 H3B -0.1172 0.2683 0.6633 23 0.990 0.000 C3 C2 C4 H4A -0.1177 0.4286 0.7500 23 0.990 0.000 C4 C3 C3_$1 H4B 0.1177 0.4286 0.7500 23 0.990 0.000 C4 C3 C3_$1 H1 0.0000 0.3139 0.3591 83 0.840 0.000 O1A C1 H1 H25A -0.1183 -0.0667 0.3297 23 0.990 0.000 C25 N21 C25_$2 H25B 0.1183 -0.0667 0.3297 23 0.990 0.000 C25 N21 C25_$2 H21 0.0000 0.1046 0.3853 43 0.880 0.000 N21 C22 C25 07skc0003cmcm in Cmcm ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.00000 0.30408 0.48515 0.50000 0.02872 0.02724 0.02251 0.00114 0.00000 0.00000 0.02616 0.00400 0.00000 0.00022 0.00019 0.00000 0.00155 0.00151 0.00139 0.00116 0.00000 0.00000 0.00064 C2 0.00000 0.37501 0.56975 0.50000 0.03128 0.02432 0.02233 0.00133 0.00000 0.00000 0.02598 0.00385 0.00000 0.00022 0.00018 0.00000 0.00161 0.00150 0.00134 0.00114 0.00000 0.00000 0.00065 H2A -0.11742 0.42064 0.56751 0.50000 0.03117 0.00000 0.00000 H2B 0.11742 0.42064 0.56751 0.50000 0.03117 0.00000 0.00000 C3 0.00000 0.31408 0.66175 0.50000 0.03038 0.02168 0.01921 0.00113 0.00000 0.00000 0.02376 0.00377 0.00000 0.00022 0.00017 0.00000 0.00155 0.00141 0.00134 0.00106 0.00000 0.00000 0.00064 H3A 0.11724 0.26829 0.66331 0.50000 0.02851 0.00000 0.00000 H3B -0.11724 0.26829 0.66331 0.50000 0.02851 0.00000 0.00000 C4 0.00000 0.38306 0.75000 0.25000 0.02864 0.02505 0.02093 0.00000 0.00000 0.00000 0.02487 0.00409 0.00000 0.00032 0.00000 0.00000 0.00217 0.00206 0.00185 0.00000 0.00000 0.00000 0.00087 H4A -0.11765 0.42858 0.75000 0.25000 0.02985 0.00000 0.00000 H4B 0.11765 0.42858 0.75000 0.25000 0.02985 0.00000 0.00000 O1B 0.00000 0.20911 0.48986 0.50000 0.06097 0.02363 0.02395 -0.00054 0.00000 0.00000 0.03618 0.00278 0.00000 0.00016 0.00014 0.00000 0.00159 0.00111 0.00105 0.00083 0.00000 0.00000 0.00059 O1A 0.00000 0.35654 0.40422 0.50000 0.05322 0.02475 0.01878 -0.00050 0.00000 0.00000 0.03225 0.00275 0.00000 0.00016 0.00013 0.00000 0.00143 0.00113 0.00097 0.00080 0.00000 0.00000 0.00057 H1 0.00000 0.31394 0.35907 0.50000 0.04837 0.00000 0.00000 C22 0.00000 0.13990 0.25000 0.25000 0.02790 0.02091 0.02583 0.00000 0.00000 0.00000 0.02488 0.00389 0.00000 0.00030 0.00000 0.00000 0.00219 0.00208 0.00200 0.00000 0.00000 0.00000 0.00088 C25 0.00000 -0.03146 0.30446 0.50000 0.04589 0.02219 0.03360 0.00063 0.00000 0.00000 0.03389 0.00408 0.00000 0.00023 0.00021 0.00000 0.00196 0.00146 0.00166 0.00131 0.00000 0.00000 0.00075 H25A -0.11834 -0.06667 0.32967 0.50000 0.04067 0.00000 0.00000 H25B 0.11834 -0.06667 0.32967 0.50000 0.04067 0.00000 0.00000 N21 0.00000 0.07981 0.32741 0.50000 0.04042 0.02276 0.02349 -0.00013 0.00000 0.00000 0.02889 0.00334 0.00000 0.00019 0.00016 0.00000 0.00161 0.00128 0.00121 0.00097 0.00000 0.00000 0.00063 H21 0.00000 0.10464 0.38528 0.50000 0.03466 0.00000 0.00000 O22 0.00000 0.23921 0.25000 0.25000 0.03750 0.02088 0.02023 0.00000 0.00000 0.00000 0.02621 0.00264 0.00000 0.00021 0.00000 0.00000 0.00175 0.00147 0.00135 0.00000 0.00000 0.00000 0.00068 Final Structure Factor Calculation for 07skc0003cmcm in Cmcm Total number of l.s. parameters = 55 Maximum vector length = 511 Memory required = 1593 / 22995 wR2 = 0.1285 before cycle 5 for 800 data and 0 / 55 parameters GooF = S = 1.170; Restrained GooF = 1.170 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0215 * P )^2 + 2.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0591 for 578 Fo > 4sig(Fo) and 0.0896 for all 800 data wR2 = 0.1285, GooF = S = 1.170, Restrained GooF = 1.170 for all data Occupancy sum of asymmetric unit = 4.25 for non-hydrogen and 4.50 for hydrogen atoms Principal mean square atomic displacements U 0.0287 0.0275 0.0223 C1 0.0313 0.0250 0.0217 C2 0.0304 0.0221 0.0188 C3 0.0286 0.0250 0.0209 C4 0.0610 0.0244 0.0232 O1B 0.0532 0.0248 0.0187 O1A 0.0279 0.0258 0.0209 C22 0.0459 0.0336 0.0222 C25 0.0404 0.0235 0.0227 N21 0.0375 0.0209 0.0202 O22 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.018 0.029 0.039 0.051 0.067 0.091 0.126 0.191 1.000 Number in group 85. 77. 78. 84. 76. 82. 81. 78. 79. 80. GooF 1.088 1.191 1.221 1.440 1.158 1.277 1.089 0.929 0.918 1.271 K 9.835 1.785 1.141 1.065 0.898 1.017 1.005 0.989 1.005 1.014 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.06 1.17 1.35 1.71 inf Number in group 81. 81. 80. 78. 80. 83. 78. 79. 80. 80. GooF 1.309 1.302 1.146 1.185 1.152 1.088 0.910 0.979 1.150 1.386 K 1.124 1.077 1.029 1.018 1.018 1.007 1.004 1.014 1.040 0.994 R1 0.291 0.220 0.151 0.167 0.113 0.085 0.052 0.052 0.045 0.036 Recommended weighting scheme: WGHT 0.0213 2.1920 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) 1 15 4 51.52 3.18 3.17 0.012 0.82 1 3 2 62.47 27.11 3.13 0.035 3.22 1 7 11 10.77 44.15 3.11 0.045 1.04 0 6 6 49.57 16.50 2.99 0.027 1.58 3 3 16 25.31 89.55 2.87 0.063 0.81 7 1 1 27.92 4.77 2.87 0.015 0.97 3 9 0 123.71 65.34 2.86 0.054 1.20 1 9 15 94.14 22.71 2.86 0.032 0.78 7 7 8 -12.99 22.14 2.79 0.032 0.77 3 13 2 -3.56 30.39 2.78 0.037 0.89 1 9 0 152.77 95.32 2.71 0.065 1.39 2 14 7 42.14 2.64 2.66 0.011 0.81 1 7 0 5188.65 4536.93 2.66 0.452 1.76 2 6 8 21.93 2.34 2.57 0.010 1.26 5 13 4 88.47 33.68 2.56 0.039 0.78 0 0 16 23.45 114.42 2.51 0.072 0.89 3 13 8 -13.40 13.77 2.41 0.025 0.80 0 4 3 1318.74 1524.46 2.40 0.262 2.64 0 2 1 6166.19 6886.79 2.35 0.557 5.82 3 1 1 881.70 1023.62 2.35 0.215 2.21 1 5 6 2753.66 2474.09 2.34 0.334 1.68 0 16 3 103.33 23.40 2.28 0.032 0.79 0 6 11 8.82 33.27 2.22 0.039 1.10 1 3 15 -0.91 18.97 2.22 0.029 0.92 1 1 2 5627.46 6141.88 2.21 0.526 4.59 3 3 12 56.63 99.63 2.21 0.067 1.02 3 5 12 -8.80 10.94 2.20 0.022 0.97 6 12 2 140.02 84.97 2.15 0.062 0.77 5 1 0 25.97 0.71 2.11 0.006 1.36 0 6 2 1403.60 1232.49 2.09 0.235 2.04 2 12 1 18.59 0.91 2.06 0.006 1.01 3 7 0 2843.12 2499.98 2.05 0.335 1.42 3 11 5 16.86 0.74 2.05 0.006 0.97 1 5 11 691.33 799.63 2.04 0.190 1.14 5 7 11 -2.59 22.23 2.04 0.032 0.83 0 10 13 50.26 9.89 2.03 0.021 0.83 2 10 3 13.98 0.24 2.03 0.003 1.16 4 2 16 30.79 0.66 2.02 0.005 0.78 0 2 7 887.42 773.65 1.99 0.187 1.93 0 4 7 219.72 280.27 1.96 0.112 1.71 0 4 2 141.50 102.83 1.96 0.068 2.91 2 14 0 17.21 56.99 1.95 0.051 0.88 1 1 16 144.92 85.42 1.94 0.062 0.88 0 14 5 -17.01 11.37 1.94 0.023 0.87 2 14 8 15.27 46.53 1.94 0.046 0.79 1 13 6 29.14 59.37 1.93 0.052 0.90 0 10 4 252.53 324.85 1.91 0.121 1.20 8 0 6 32.73 5.58 1.90 0.016 0.80 5 3 14 30.94 0.29 1.89 0.004 0.80 0 0 8 250.49 310.73 1.88 0.118 1.77 Bond lengths and angles C1 - Distance Angles O1B 1.2131 (0.0034) O1A 1.3291 (0.0032) 123.39 (0.26) C2 1.5031 (0.0037) 123.85 (0.25) 112.77 (0.24) C1 - O1B O1A C2 - Distance Angles C1 1.5031 (0.0037) C3 1.5193 (0.0035) 112.23 (0.23) H2A 0.9900 109.16 109.16 H2B 0.9900 109.16 109.16 107.88 C2 - C1 C3 H2A C3 - Distance Angles C2 1.5193 (0.0035) C4 1.5303 (0.0034) 114.15 (0.24) H3A 0.9900 108.72 108.72 H3B 0.9900 108.72 108.72 107.63 C3 - C2 C4 H3A C4 - Distance Angles C3 1.5303 (0.0034) C3_$1 1.5303 (0.0034) 109.82 (0.32) H4A 0.9900 109.70 109.70 H4B 0.9900 109.70 109.70 108.19 C4 - C3 C3_$1 H4A O1B - Distance Angles C1 1.2131 (0.0034) O1B - O1A - Distance Angles C1 1.3291 (0.0032) H1 0.8400 109.47 O1A - C1 C22 - Distance Angles O22 1.2667 (0.0046) N21_$2 1.3393 (0.0031) 124.90 (0.17) N21 1.3393 (0.0031) 124.90 (0.17) 110.20 (0.34) C22 - O22 N21_$2 C25 - Distance Angles N21 1.4561 (0.0037) C25_$2 1.5455 (0.0059) 102.93 (0.15) H25A 0.9900 111.18 111.18 H25B 0.9900 111.18 111.18 109.11 C25 - N21 C25_$2 H25A N21 - Distance Angles C22 1.3393 (0.0031) C25 1.4561 (0.0037) 111.97 (0.24) H21 0.8800 124.01 124.01 N21 - C22 C25 O22 - Distance Angles C22 1.2667 (0.0046) O22 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.82 2.651(2) 171.3 O1A-H1...O22 0.88 1.99 2.834(3) 159.2 N21-H21...O1B Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 6.8156 (0.0006) x + 0.0000 (0.0001) y + 0.0000 (0.0002) z = 0.0000 (0.0001) * 0.0000 (0.0000) C1 * 0.0000 (0.0000) O1A * 0.0000 (0.0000) O1B Rms deviation of fitted atoms = 0.0000 6.8156 (0.0006) x - 0.0000 (0.0002) y + 0.0000 (0.0003) z = 0.0000 (0.0002) Angle to previous plane (with approximate esd) = 0.00 ( 0.01 ) * 0.0000 (0.0000) C1_$1 * 0.0000 (0.0000) O1A_$1 * 0.0000 (0.0000) O1B_$1 Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 1 11 GRID -3.125 -1 24 3.125 1 1 R1 = 0.0895 for 800 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.31 at 0.0000 0.3393 0.2500 [ 1.28 A from O22 ] Deepest hole -0.30 at 0.0000 0.1688 0.2968 [ 0.76 A from C22 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2058 / 18783 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0000 0.3393 0.2500 0.25000 0.05 0.31 1.28 O22 1.58 H1 2.20 O1A 2.54 C22 Q2 1 0.0000 0.0130 0.4269 0.50000 0.05 0.26 1.31 H21 1.65 N21 1.83 C25 1.89 H25A Q3 1 0.0000 0.3515 0.7021 0.50000 0.05 0.25 0.75 C3 0.79 C4 1.44 H3A 1.44 H3B Q4 1 0.0000 0.1901 0.3443 0.50000 0.05 0.25 1.24 H21 1.43 N21 1.48 O22 1.48 C22 Q5 1 0.0000 -0.1075 0.3479 0.50000 0.05 0.25 0.99 H25A 0.99 H25B 0.99 H25A 0.99 H25B Q6 1 0.0000 0.0877 0.4837 0.50000 0.05 0.23 1.41 H21 1.55 O1B 2.22 N21 2.71 H2A Q7 1 0.0000 0.3446 0.6178 0.50000 0.05 0.23 0.73 C3 0.78 C2 1.41 H3A 1.41 H3B Q8 1 0.0000 0.0383 0.5272 0.50000 0.05 0.21 2.18 H21 2.21 H21 2.21 H25A 2.21 H25B Q9 1 0.0598 0.1914 0.2500 0.50000 0.05 0.19 0.73 O22 0.77 C22 1.84 N21 2.24 H1 Q10 1 0.0000 0.4619 0.5270 0.50000 0.05 0.19 1.12 H2A 1.12 H2B 1.12 H2A 1.12 H2B Shortest distances between peaks (including symmetry equivalents) 9 9 0.81 6 8 0.88 2 8 0.92 3 7 1.20 10 10 1.24 8 8 1.25 2 6 1.25 3 3 1.36 4 9 1.40 2 8 1.46 6 8 1.61 2 6 1.80 2 5 1.90 1 9 1.93 7 10 1.97 5 8 1.98 2 2 2.10 6 6 2.28 1 4 2.33 4 6 2.37 5 6 2.40 2 4 2.54 3 7 2.56 4 4 2.68 5 5 2.78 3 10 2.86 Time profile in seconds ----------------------- 0.08: 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 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.22: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.13: Structure factors and derivatives 0.02: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.03: 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 0.05: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0003cmcm finished at 15:11:20 Total CPU time: 0.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++