+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0081p21n started at 15:35:51 on 06-May-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0081p21n in P2(1)/n CELL 0.71073 11.6287 5.1904 11.9417 90.000 108.971 90.000 ZERR 2.00 0.0003 0.0002 0.0003 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 24 36 4 12 V = 681.62 F(000) = 304.0 Mu = 0.11 mm-1 Cell Wt = 572.57 Rho = 1.395 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 EQIV_$1 x-1/2, -y+1/2, z+1/2 HTAB O1B O22_$1 EQIV_$2 -x+1, -y, -z-1 HTAB N21 O22_$2 EQIV_$3 -x+1, -y, -z MPLA C1 O1A O1B MPLA C1_$3 O1A_$3 O1B_$3 FMAP 2 PLAN 10 SIZE 0.08 0.13 0.16 ACTA CONF BOND $H WGHT 0.00610 0.80400 L.S. 4 TEMP -153.00 FVAR 0.87262 MOLE 1 C1 1 0.356143 0.118345 0.029180 11.00000 0.01996 0.02757 = 0.01864 -0.00330 0.00230 0.00258 C2 1 0.457806 -0.046672 0.019398 11.00000 0.02328 0.02380 = 0.02026 -0.00119 0.00304 -0.00049 AFIX 43 H2 2 0.461135 -0.222834 0.041821 11.00000 -1.20000 AFIX 0 O1A 4 0.332536 0.331599 -0.015444 11.00000 0.02621 0.02983 = 0.03123 0.00205 0.01330 0.00066 O1B 4 0.295607 0.003827 0.090373 11.00000 0.02667 0.02647 = 0.03177 0.00414 0.01231 0.00636 AFIX 147 H1 2 0.234443 0.092667 0.087873 11.00000 0.08306 AFIX 0 MOLE 2 C22 1 0.529245 0.293199 -0.378278 11.00000 0.02415 0.01998 = 0.02084 0.00012 0.00870 -0.00019 C23 1 0.547289 0.496511 -0.285037 11.00000 0.02475 0.02161 = 0.02239 -0.00371 0.00865 -0.00132 AFIX 23 H23A 2 0.571858 0.662243 -0.311494 11.00000 -1.20000 H23B 2 0.609720 0.443545 -0.210160 11.00000 -1.20000 AFIX 0 C24 1 0.421261 0.517900 -0.269754 11.00000 0.02794 0.02035 = 0.02210 -0.00123 0.00867 0.00242 AFIX 23 H24A 2 0.428779 0.543328 -0.185503 11.00000 -1.20000 H24B 2 0.374444 0.663070 -0.316713 11.00000 -1.20000 AFIX 0 C25 1 0.360018 0.259250 -0.315710 11.00000 0.02303 0.02332 = 0.02031 0.00149 0.00969 -0.00030 AFIX 23 H25A 2 0.369480 0.136293 -0.249939 11.00000 -1.20000 H25B 2 0.272380 0.282375 -0.359531 11.00000 -1.20000 AFIX 0 N21 3 0.425435 0.171517 -0.394019 11.00000 0.02380 0.02177 = 0.02239 -0.00457 0.00923 -0.00538 AFIX 43 H21 2 0.398284 0.048822 -0.446901 11.00000 0.02572 AFIX 0 O22 4 0.602044 0.241105 -0.432829 11.00000 0.02890 0.03034 = 0.03341 -0.01018 0.01699 -0.00761 HKLF 4 Covalent radii and connectivity table for 06skc0081p21n in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C2_$3 C1 O1A - C1 O1B - C1 C22 - O22 N21 C23 C23 - C22 C24 C24 - C25 C23 C25 - N21 C24 N21 - C22 C25 O22 - C22 Operators for generating equivalent atoms: $1 x-1/2, -y+1/2, z+1/2 $2 -x+1, -y, -z-1 $3 -x+1, -y, -z h k l Fo^2 Sigma Why rejected 7 0 0 6.00 1.45 observed but should be systematically absent 8013 Reflections read, of which 620 rejected -14 =< h =< 15, -6 =< k =< 6, -15 =< l =< 15, Max. 2-theta = 54.95 1 Systematic absence violations 0 Inconsistent equivalents 1553 Unique reflections, of which 0 suppressed R(int) = 0.0483 R(sigma) = 0.0413 Friedel opposites merged Maximum memory for data reduction = 1402 / 15511 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 = 1670 / 123716 wR2 = 0.1111 before cycle 1 for 1553 data and 94 / 94 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87262 0.00225 0.001 OSF Mean shift/esd = 0.002 Maximum = 0.006 for U33 N21 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H21 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1670 / 123716 wR2 = 0.1111 before cycle 2 for 1553 data and 94 / 94 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87263 0.00225 0.001 OSF Mean shift/esd = 0.001 Maximum = -0.002 for U13 O22 Max. shift = 0.000 A for N21 Max. dU = 0.000 for H21 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1670 / 123716 wR2 = 0.1111 before cycle 3 for 1553 data and 94 / 94 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87263 0.00225 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 H21 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1670 / 123716 wR2 = 0.1111 before cycle 4 for 1553 data and 94 / 94 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.87263 0.00225 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C23 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 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 H2 0.4611 -0.2228 0.0418 43 0.950 0.000 C2 C2_$3 C1 H1 0.2344 0.0927 0.0879 147 0.840 0.000 O1B C1 H1 H23A 0.5719 0.6622 -0.3115 23 0.990 0.000 C23 C22 C24 H23B 0.6097 0.4435 -0.2102 23 0.990 0.000 C23 C22 C24 H24A 0.4288 0.5433 -0.1855 23 0.990 0.000 C24 C25 C23 H24B 0.3744 0.6631 -0.3167 23 0.990 0.000 C24 C25 C23 H25A 0.3695 0.1363 -0.2499 23 0.990 0.000 C25 N21 C24 H25B 0.2724 0.2824 -0.3595 23 0.990 0.000 C25 N21 C24 H21 0.3983 0.0488 -0.4469 43 0.880 0.000 N21 C22 C25 06skc0081p21n in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.35614 0.11834 0.02918 1.00000 0.01996 0.02757 0.01864 -0.00330 0.00230 0.00258 0.02302 0.00367 0.00017 0.00040 0.00016 0.00000 0.00093 0.00105 0.00089 0.00081 0.00073 0.00080 0.00043 C2 0.45781 -0.04667 0.01940 1.00000 0.02328 0.02380 0.02026 -0.00119 0.00304 -0.00049 0.02343 0.00369 0.00017 0.00040 0.00016 0.00000 0.00094 0.00099 0.00090 0.00078 0.00073 0.00078 0.00042 H2 0.46113 -0.22283 0.04182 1.00000 0.02811 0.00000 0.00000 O1A 0.33254 0.33160 -0.01544 1.00000 0.02622 0.02983 0.03124 0.00205 0.01330 0.00066 0.02813 0.00285 0.00012 0.00028 0.00013 0.00000 0.00074 0.00080 0.00077 0.00065 0.00060 0.00061 0.00035 O1B 0.29561 0.00383 0.09037 1.00000 0.02667 0.02647 0.03177 0.00414 0.01231 0.00636 0.02762 0.00291 0.00013 0.00028 0.00012 0.00000 0.00077 0.00077 0.00079 0.00065 0.00062 0.00063 0.00035 H1 0.23444 0.09267 0.08787 1.00000 0.08306 0.00000 0.01148 C22 0.52924 0.29320 -0.37828 1.00000 0.02415 0.01998 0.02084 0.00012 0.00870 -0.00019 0.02132 0.00375 0.00017 0.00037 0.00016 0.00000 0.00095 0.00095 0.00091 0.00076 0.00075 0.00077 0.00041 C23 0.54729 0.49651 -0.28504 1.00000 0.02476 0.02161 0.02239 -0.00371 0.00865 -0.00132 0.02268 0.00371 0.00017 0.00038 0.00017 0.00000 0.00097 0.00097 0.00091 0.00078 0.00076 0.00080 0.00042 H23A 0.57186 0.66224 -0.31149 1.00000 0.02721 0.00000 0.00000 H23B 0.60972 0.44354 -0.21016 1.00000 0.02721 0.00000 0.00000 C24 0.42126 0.51790 -0.26975 1.00000 0.02794 0.02035 0.02210 -0.00123 0.00867 0.00242 0.02333 0.00385 0.00018 0.00038 0.00017 0.00000 0.00100 0.00096 0.00092 0.00079 0.00077 0.00080 0.00042 H24A 0.42878 0.54333 -0.18550 1.00000 0.02800 0.00000 0.00000 H24B 0.37444 0.66307 -0.31671 1.00000 0.02800 0.00000 0.00000 C25 0.36002 0.25925 -0.31571 1.00000 0.02303 0.02332 0.02031 0.00149 0.00969 -0.00030 0.02158 0.00381 0.00017 0.00037 0.00017 0.00000 0.00095 0.00098 0.00089 0.00077 0.00075 0.00077 0.00041 H25A 0.36948 0.13629 -0.24994 1.00000 0.02590 0.00000 0.00000 H25B 0.27238 0.28238 -0.35953 1.00000 0.02590 0.00000 0.00000 N21 0.42543 0.17152 -0.39402 1.00000 0.02380 0.02177 0.02240 -0.00457 0.00923 -0.00538 0.02224 0.00311 0.00014 0.00032 0.00014 0.00000 0.00084 0.00083 0.00081 0.00069 0.00066 0.00068 0.00037 H21 0.39828 0.04882 -0.44690 1.00000 0.02573 0.00000 0.00575 O22 0.60204 0.24111 -0.43283 1.00000 0.02890 0.03034 0.03341 -0.01018 0.01699 -0.00761 0.02922 0.00276 0.00013 0.00028 0.00013 0.00000 0.00076 0.00081 0.00079 0.00065 0.00063 0.00062 0.00036 Final Structure Factor Calculation for 06skc0081p21n in P2(1)/n Total number of l.s. parameters = 94 Maximum vector length = 511 Memory required = 1576 / 22995 wR2 = 0.1111 before cycle 5 for 1553 data and 0 / 94 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0531 for 1239 Fo > 4sig(Fo) and 0.0717 for all 1553 data wR2 = 0.1111, GooF = S = 1.086, Restrained GooF = 1.086 for all data Occupancy sum of asymmetric unit = 10.00 for non-hydrogen and 9.00 for hydrogen atoms Principal mean square atomic displacements U 0.0316 0.0213 0.0162 C1 0.0281 0.0240 0.0182 C2 0.0335 0.0289 0.0221 O1A 0.0359 0.0269 0.0200 O1B 0.0243 0.0201 0.0195 C22 0.0263 0.0236 0.0181 C23 0.0288 0.0227 0.0185 C24 0.0242 0.0235 0.0170 C25 0.0294 0.0204 0.0168 N21 0.0451 0.0221 0.0205 O22 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.016 0.024 0.034 0.044 0.056 0.073 0.101 0.147 1.000 Number in group 171. 151. 151. 159. 154. 151. 159. 147. 157. 153. GooF 1.066 1.198 1.130 1.072 1.084 1.115 1.138 0.949 0.974 1.110 K 4.403 1.694 1.135 1.035 1.010 0.979 1.016 1.007 1.003 1.000 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 160. 155. 151. 155. 159. 152. 157. 157. 151. 156. GooF 1.251 1.247 0.950 1.098 1.037 0.863 0.991 0.855 1.149 1.301 K 1.104 1.053 1.049 1.012 1.005 0.997 0.997 0.983 1.027 0.997 R1 0.234 0.186 0.131 0.112 0.091 0.058 0.052 0.039 0.040 0.027 Recommended weighting scheme: WGHT 0.0062 0.8037 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 1 1 1636.47 1862.00 4.05 0.378 4.72 3 3 3 16.68 4.04 3.69 0.018 1.38 -14 2 2 47.68 3.26 3.67 0.016 0.78 -2 0 2 2500.24 2807.78 3.51 0.464 4.79 4 5 7 6.43 20.89 2.98 0.040 0.79 -8 3 2 32.48 52.80 2.89 0.064 1.11 3 1 2 217.34 176.81 2.87 0.116 2.40 -11 4 5 15.61 0.24 2.86 0.004 0.82 -7 5 4 15.23 34.80 2.86 0.052 0.87 -1 4 12 5.65 18.66 2.82 0.038 0.77 3 3 9 10.12 1.66 2.79 0.011 0.92 -3 1 3 15.29 6.68 2.76 0.023 2.72 2 0 0 1665.93 1832.01 2.68 0.375 5.50 6 2 8 13.92 2.69 2.66 0.014 0.91 -2 6 4 20.61 40.47 2.61 0.056 0.83 3 1 0 306.98 356.49 2.59 0.165 2.99 -3 0 9 1205.28 1080.27 2.58 0.288 1.33 -8 1 10 4.03 12.49 2.58 0.031 1.04 -9 5 4 107.71 78.05 2.58 0.077 0.81 -11 3 8 -1.42 6.74 2.53 0.023 0.85 4 5 4 21.72 10.19 2.52 0.028 0.89 7 3 1 1.94 8.49 2.45 0.025 1.13 -6 2 3 75.45 55.85 2.44 0.065 1.54 0 2 2 531.84 470.65 2.43 0.190 2.36 -1 1 1 79.33 101.95 2.42 0.088 4.56 -7 5 3 87.05 61.40 2.41 0.069 0.88 -4 2 7 200.87 168.10 2.39 0.113 1.39 -12 3 1 7.76 0.20 2.39 0.004 0.82 -4 1 15 4.38 15.86 2.38 0.035 0.79 -1 4 8 11.70 5.10 2.37 0.020 0.97 10 3 4 34.48 19.93 2.37 0.039 0.82 9 5 1 47.78 30.25 2.34 0.048 0.78 5 3 0 865.54 949.15 2.34 0.270 1.36 -11 1 8 0.42 7.16 2.31 0.023 0.96 -6 1 1 30.47 19.54 2.30 0.039 1.79 -13 2 7 18.09 4.49 2.29 0.019 0.83 -8 4 5 11.90 22.84 2.25 0.042 0.95 -11 4 8 0.70 9.31 2.23 0.027 0.78 -13 3 7 80.88 55.87 2.22 0.065 0.78 7 3 5 11.63 5.02 2.22 0.020 0.95 -5 2 6 4.55 0.92 2.22 0.008 1.44 -8 5 3 18.45 4.08 2.22 0.018 0.84 13 2 0 6.98 16.26 2.21 0.035 0.80 0 6 6 51.05 32.04 2.18 0.050 0.79 3 5 5 20.27 33.16 2.18 0.050 0.88 -12 2 11 40.63 9.40 2.18 0.027 0.79 -10 4 3 12.50 5.08 2.18 0.020 0.87 -5 0 3 260.81 225.52 2.17 0.131 2.24 -9 4 10 63.23 41.33 2.17 0.056 0.80 -7 2 10 5.49 1.00 2.17 0.009 1.01 Bond lengths and angles C1 - Distance Angles O1A 1.2204 (0.0024) O1B 1.3105 (0.0024) 124.72 (0.18) C2 1.4949 (0.0027) 123.84 (0.18) 111.44 (0.17) C1 - O1A O1B C2 - Distance Angles C2_$3 1.3069 (0.0038) C1 1.4949 (0.0027) 121.29 (0.25) H2 0.9500 119.36 119.36 C2 - C2_$3 C1 O1A - Distance Angles C1 1.2204 (0.0024) O1A - O1B - Distance Angles C1 1.3105 (0.0024) H1 0.8400 109.47 O1B - C1 C22 - Distance Angles O22 1.2541 (0.0023) N21 1.3206 (0.0024) 124.27 (0.18) C23 1.4985 (0.0026) 125.64 (0.17) 110.08 (0.16) C22 - O22 N21 C23 - Distance Angles C22 1.4985 (0.0026) C24 1.5386 (0.0026) 103.31 (0.15) H23A 0.9900 111.10 111.10 H23B 0.9900 111.10 111.10 109.06 C23 - C22 C24 H23A C24 - Distance Angles C25 1.5351 (0.0027) C23 1.5386 (0.0026) 104.10 (0.15) H24A 0.9900 110.94 110.94 H24B 0.9900 110.94 110.94 108.95 C24 - C25 C23 H24A C25 - Distance Angles N21 1.4571 (0.0023) C24 1.5351 (0.0027) 102.97 (0.14) H25A 0.9900 111.17 111.17 H25B 0.9900 111.17 111.17 109.11 C25 - N21 C24 H25A N21 - Distance Angles C22 1.3206 (0.0024) C25 1.4571 (0.0023) 113.77 (0.16) H21 0.8800 123.12 123.12 N21 - C22 C25 O22 - Distance Angles C22 1.2541 (0.0023) O22 - Selected torsion angles 12.86 ( 0.35) O1A - C1 - C2 - C2_$3 -167.77 ( 0.22) O1B - C1 - C2 - C2_$3 167.76 ( 0.19) O22 - C22 - C23 - C24 -13.29 ( 0.21) N21 - C22 - C23 - C24 22.14 ( 0.19) C22 - C23 - C24 - C25 -23.08 ( 0.18) C23 - C24 - C25 - N21 177.02 ( 0.18) O22 - C22 - N21 - C25 -1.95 ( 0.22) C23 - C22 - N21 - C25 16.31 ( 0.21) C24 - C25 - N21 - C22 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.71 2.5476(19) 173.5 O1B-H1...O22_$1 0.88 2.08 2.921(2) 159.9 N21-H21...O22_$2 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 4.1167 (0.0354) x + 2.1497 (0.0098) y + 8.0954 (0.0177) z = 1.9567 (0.0096) * 0.0000 (0.0000) C1 * 0.0000 (0.0000) O1A * 0.0000 (0.0000) O1B Rms deviation of fitted atoms = 0.0000 4.1167 (0.0354) x + 2.1497 (0.0098) y + 8.0954 (0.0177) z = 2.1599 (0.0259) Angle to previous plane (with approximate esd) = 0.00 ( 0.37 ) * 0.0000 (0.0000) C1_$3 * 0.0000 (0.0000) O1A_$3 * 0.0000 (0.0000) O1B_$3 Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 2 10 GRID -3.571 -2 -2 3.571 2 2 R1 = 0.0717 for 1553 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.35 at 0.4804 0.1289 -0.0080 [ 0.88 A from C2 ] Deepest hole -0.25 at 0.9737 0.1694 0.1611 [ 0.93 A from C22 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 1886 / 15324 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5196 -0.1289 0.0080 1.00000 0.05 0.35 0.88 C2 1.02 H2 1.03 C2 1.64 C1 Q2 1 0.3970 0.3879 -0.2817 1.00000 0.05 0.28 0.73 C24 0.83 C25 1.35 H24A 1.43 H25A Q3 1 0.2960 0.4630 0.0863 1.00000 0.05 0.22 1.57 O1A 1.60 H23B 2.05 H1 2.11 C1 Q4 1 0.4560 -0.2917 0.0153 1.00000 0.05 0.20 0.47 H2 1.27 C2 2.13 C2 2.38 O1A Q5 1 0.4014 0.5722 -0.2158 1.00000 0.05 0.19 0.42 H24A 0.80 C24 1.24 H24B 1.98 C25 Q6 1 0.3331 -0.1044 -0.4773 1.00000 0.05 0.19 1.08 H21 1.66 O22 1.87 N21 1.93 O1A Q7 1 0.2348 0.0609 -0.3153 1.00000 0.05 0.19 1.39 H25B 1.56 H25A 1.78 C25 1.91 H24A Q8 1 0.4794 0.5152 -0.2689 1.00000 0.05 0.19 0.67 C24 0.88 C23 1.32 H24A 1.40 H24B Q9 1 0.6435 0.1786 -0.3634 1.00000 0.05 0.18 0.88 O22 1.41 C22 1.81 H1 2.35 C23 Q10 1 0.3192 0.4932 0.0008 1.00000 0.05 0.18 0.89 O1A 2.00 C1 2.15 H2 2.25 H25B Shortest distances between peaks (including symmetry equivalents) 2 8 1.13 1 4 1.14 3 10 1.15 2 5 1.23 5 8 1.30 1 1 1.41 3 6 1.67 5 7 1.74 6 10 1.77 4 10 1.90 6 9 2.04 7 10 2.13 3 9 2.18 1 4 2.23 2 7 2.38 4 4 2.47 2 7 2.47 3 4 2.61 6 7 2.69 1 10 2.69 4 5 2.72 4 7 2.79 3 8 2.81 4 5 2.83 4 10 2.88 7 8 2.98 7 7 2.99 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 0.00: 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 0.02: Analyse other restraints etc. 0.47: 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 0.20: Structure factors and derivatives 0.09: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.05: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0081p21n finished at 15:35:52 Total CPU time: 1.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++