+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0079p21c started at 16:01:00 on 04-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0079p21c in P2(1)/c CELL 0.71073 5.7944 7.4316 15.9213 90.000 96.289 90.000 ZERR 4.00 0.0002 0.0005 0.0010 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S UNIT 24 28 4 12 4 V = 681.47 F(000) = 360.0 Mu = 0.42 mm-1 Cell Wt = 692.74 Rho = 1.688 MERG 2 OMIT -3.00 55.00 OMIT -1 0 2 SHEL 7 0.77 EQIV_$1 x, -y+3/2, z-1/2 HTAB N4 O1B_$1 EQIV_$2 -x, -y+2, -z HTAB N4 O1A_$2 EQIV_$3 -x, -y+1, -z HTAB N4 O1C_$3 HTAB N4 S1_$3 EQIV_$4 x-1, -y+3/2, z-1/2 HTAB N4 O1A_$4 FMAP 2 PLAN 10 SIZE 0.03 0.06 0.20 ACTA BOND $H WGHT 0.02610 1.17130 L.S. 4 TEMP -153.00 FVAR 0.23962 MOLE 1 C1 1 0.127805 0.719109 0.055318 11.00000 0.01259 0.00944 = 0.01307 0.00054 -0.00027 -0.00252 C2 1 -0.092880 0.796140 0.048189 11.00000 0.01470 0.01139 = 0.01428 -0.00021 0.00272 0.00019 AFIX 43 H2 2 -0.161753 0.829736 0.097343 11.00000 -1.20000 AFIX 0 C3 1 -0.211075 0.823273 -0.031574 11.00000 0.01020 0.01103 = 0.01707 0.00057 0.00001 0.00083 AFIX 43 H3 2 -0.360756 0.876978 -0.037578 11.00000 -1.20000 AFIX 0 C4 1 -0.107833 0.770978 -0.102338 11.00000 0.01522 0.00921 = 0.01127 0.00085 -0.00205 -0.00128 C5 1 0.110034 0.693358 -0.096195 11.00000 0.01645 0.01242 = 0.01211 0.00051 0.00246 -0.00003 AFIX 43 H5 2 0.177088 0.657875 -0.145461 11.00000 -1.20000 AFIX 0 C6 1 0.229399 0.668208 -0.016154 11.00000 0.01306 0.01125 = 0.01666 0.00128 0.00036 0.00139 AFIX 43 H6 2 0.380126 0.616293 -0.010480 11.00000 -1.20000 AFIX 0 N4 3 -0.236976 0.793217 -0.186594 11.00000 0.01655 0.01242 = 0.01207 0.00070 -0.00306 -0.00010 AFIX 137 H4A 2 -0.135855 0.792475 -0.226478 11.00000 0.03525 H4B 2 -0.314942 0.899703 -0.188791 11.00000 0.02530 H4C 2 -0.339968 0.701221 -0.196600 11.00000 0.03745 AFIX 0 O1A 4 0.411471 0.859623 0.174747 11.00000 0.03276 0.01244 = 0.03228 -0.00551 -0.01758 0.00120 O1B 4 0.118679 0.650211 0.214220 11.00000 0.02593 0.04719 = 0.01303 0.00297 0.00439 0.00740 O1C 4 0.449389 0.542601 0.148480 11.00000 0.01753 0.01182 = 0.01740 0.00032 -0.00234 0.00412 S1 5 0.288499 0.690096 0.155893 11.00000 0.01701 0.01311 = 0.01240 -0.00199 -0.00305 0.00223 HKLF 4 Covalent radii and connectivity table for 06skc0079p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - C6 C2 S1 C2 - C3 C1 C3 - C4 C2 C4 - C5 C3 N4 C5 - C4 C6 C6 - C1 C5 N4 - C4 O1A - S1 O1B - S1 O1C - S1 S1 - O1C O1B O1A C1 Operators for generating equivalent atoms: $1 x, -y+3/2, z-1/2 $2 -x, -y+2, -z $3 -x, -y+1, -z $4 x-1, -y+3/2, z-1/2 h k l Fo^2 Sigma Why rejected -5 0 7 2.21 0.35 observed but should be systematically absent -5 0 7 3.24 0.64 observed but should be systematically absent 8603 Reflections read, of which 333 rejected -6 =< h =< 7, -9 =< k =< 9, -20 =< l =< 20, Max. 2-theta = 54.95 2 Systematic absence violations 0 Inconsistent equivalents 1567 Unique reflections, of which 0 suppressed R(int) = 0.0505 R(sigma) = 0.0430 Friedel opposites merged Maximum memory for data reduction = 1348 / 15574 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 = 1623 / 135973 wR2 = 0.1022 before cycle 1 for 1567 data and 104 / 104 parameters GooF = S = 1.101; Restrained GooF = 1.101 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0261 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23952 0.00064 -0.150 OSF Mean shift/esd = 0.020 Maximum = -0.150 for OSF Max. shift = 0.000 A for H4A Max. dU = 0.000 for H4B Least-squares cycle 2 Maximum vector length = 511 Memory required = 1623 / 135973 wR2 = 0.1022 before cycle 2 for 1567 data and 104 / 104 parameters GooF = S = 1.101; Restrained GooF = 1.101 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0261 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23949 0.00064 -0.051 OSF Mean shift/esd = 0.007 Maximum = -0.051 for OSF Max. shift = 0.000 A for H4A Max. dU = 0.000 for H4B Least-squares cycle 3 Maximum vector length = 511 Memory required = 1623 / 135973 wR2 = 0.1022 before cycle 3 for 1567 data and 104 / 104 parameters GooF = S = 1.101; Restrained GooF = 1.101 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0261 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23949 0.00064 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for x C6 Max. shift = 0.000 A for H4C Max. dU = 0.000 for H4C Least-squares cycle 4 Maximum vector length = 511 Memory required = 1623 / 135973 wR2 = 0.1022 before cycle 4 for 1567 data and 104 / 104 parameters GooF = S = 1.101; Restrained GooF = 1.101 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0261 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23949 0.00064 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U11 N4 Max. shift = 0.000 A for H4A Max. dU = 0.000 for H4A 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 -0.1617 0.8297 0.0973 43 0.950 0.000 C2 C3 C1 H3 -0.3607 0.8770 -0.0376 43 0.950 0.000 C3 C4 C2 H5 0.1771 0.6579 -0.1455 43 0.950 0.000 C5 C4 C6 H6 0.3801 0.6163 -0.0105 43 0.950 0.000 C6 C1 C5 H4A -0.1359 0.7924 -0.2265 137 0.910 0.000 N4 C4 H4A H4B -0.3149 0.8997 -0.1888 137 0.910 0.000 N4 C4 H4A H4C -0.3400 0.7012 -0.1966 137 0.910 0.000 N4 C4 H4A 06skc0079p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.12781 0.71911 0.05532 1.00000 0.01254 0.00940 0.01303 0.00053 -0.00027 -0.00251 0.01178 0.00389 0.00039 0.00030 0.00014 0.00000 0.00112 0.00104 0.00106 0.00082 0.00082 0.00081 0.00045 C2 -0.09287 0.79614 0.04819 1.00000 0.01465 0.01134 0.01425 -0.00022 0.00272 0.00018 0.01333 0.00409 0.00040 0.00030 0.00014 0.00000 0.00116 0.00105 0.00109 0.00086 0.00085 0.00086 0.00046 H2 -0.16175 0.82974 0.09734 1.00000 0.01599 0.00000 0.00000 C3 -0.21106 0.82327 -0.03158 1.00000 0.01016 0.01100 0.01701 0.00058 0.00001 0.00084 0.01283 0.00404 0.00039 0.00030 0.00014 0.00000 0.00108 0.00105 0.00113 0.00087 0.00084 0.00085 0.00045 H3 -0.36075 0.87697 -0.03758 1.00000 0.01540 0.00000 0.00000 C4 -0.10782 0.77099 -0.10233 1.00000 0.01517 0.00918 0.01121 0.00085 -0.00206 -0.00129 0.01211 0.00391 0.00040 0.00029 0.00014 0.00000 0.00114 0.00102 0.00107 0.00080 0.00082 0.00084 0.00046 C5 0.11002 0.69336 -0.09619 1.00000 0.01640 0.01238 0.01207 0.00052 0.00244 -0.00002 0.01355 0.00411 0.00040 0.00030 0.00014 0.00000 0.00117 0.00110 0.00106 0.00086 0.00085 0.00088 0.00047 H5 0.17706 0.65787 -0.14546 1.00000 0.01626 0.00000 0.00000 C6 0.22940 0.66821 -0.01615 1.00000 0.01301 0.01121 0.01660 0.00127 0.00036 0.00139 0.01370 0.00412 0.00040 0.00030 0.00015 0.00000 0.00113 0.00107 0.00113 0.00087 0.00087 0.00085 0.00047 H6 0.38013 0.61631 -0.01048 1.00000 0.01644 0.00000 0.00000 N4 -0.23698 0.79322 -0.18659 1.00000 0.01651 0.01239 0.01201 0.00070 -0.00306 -0.00010 0.01398 0.00338 0.00034 0.00026 0.00012 0.00000 0.00102 0.00096 0.00094 0.00074 0.00075 0.00078 0.00042 H4A -0.13587 0.79243 -0.22648 1.00000 0.03525 0.00000 0.00893 H4B -0.31490 0.89972 -0.18880 1.00000 0.02554 0.00000 0.00770 H4C -0.34001 0.70124 -0.19659 1.00000 0.03756 0.00000 0.00916 O1A 0.41149 0.85963 0.17474 1.00000 0.03273 0.01238 0.03225 -0.00550 -0.01759 0.00117 0.02735 0.00307 0.00033 0.00023 0.00012 0.00000 0.00110 0.00090 0.00109 0.00074 0.00084 0.00075 0.00048 O1B 0.11867 0.65021 0.21422 1.00000 0.02588 0.04715 0.01298 0.00297 0.00440 0.00740 0.02850 0.00362 0.00033 0.00029 0.00011 0.00000 0.00103 0.00129 0.00087 0.00081 0.00073 0.00089 0.00048 O1C 0.44940 0.54260 0.14848 1.00000 0.01749 0.01177 0.01737 0.00034 -0.00234 0.00413 0.01586 0.00292 0.00028 0.00021 0.00010 0.00000 0.00087 0.00080 0.00085 0.00064 0.00064 0.00065 0.00037 S1 0.28850 0.69010 0.15589 1.00000 0.01697 0.01307 0.01236 -0.00199 -0.00305 0.00223 0.01448 0.00100 0.00010 0.00008 0.00003 0.00000 0.00032 0.00029 0.00029 0.00022 0.00021 0.00022 0.00018 Final Structure Factor Calculation for 06skc0079p21c in P2(1)/c Total number of l.s. parameters = 104 Maximum vector length = 511 Memory required = 1519 / 24017 wR2 = 0.1022 before cycle 5 for 1567 data and 0 / 104 parameters GooF = S = 1.101; Restrained GooF = 1.101 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0261 * P )^2 + 1.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0434 for 1298 Fo > 4sig(Fo) and 0.0589 for all 1567 data wR2 = 0.1022, GooF = S = 1.101, Restrained GooF = 1.101 for all data Occupancy sum of asymmetric unit = 11.00 for non-hydrogen and 7.00 for hydrogen atoms Principal mean square atomic displacements U 0.0155 0.0118 0.0080 C1 0.0155 0.0132 0.0113 C2 0.0175 0.0115 0.0095 C3 0.0180 0.0095 0.0089 C4 0.0165 0.0127 0.0115 C5 0.0173 0.0137 0.0101 C6 0.0200 0.0125 0.0095 N4 0.0568 0.0156 0.0096 O1A 0.0496 0.0236 0.0122 O1B 0.0230 0.0154 0.0091 O1C 0.0216 0.0121 0.0098 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.027 0.040 0.057 0.073 0.089 0.112 0.140 0.192 1.000 Number in group 168. 153. 149. 168. 159. 146. 154. 162. 151. 157. GooF 1.277 1.094 1.237 1.071 1.105 1.044 0.980 0.963 0.970 1.208 K 3.062 1.298 0.935 0.963 0.968 0.977 0.992 1.010 1.014 0.990 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.66 inf Number in group 160. 160. 151. 157. 158. 159. 156. 152. 156. 158. GooF 0.996 0.902 0.929 1.024 0.951 1.080 1.125 1.005 1.219 1.602 K 0.990 0.971 0.977 1.000 1.012 1.020 1.016 1.024 1.030 0.963 R1 0.127 0.098 0.084 0.074 0.063 0.046 0.043 0.032 0.041 0.041 Recommended weighting scheme: WGHT 0.0264 1.1675 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) 5 1 5 85.88 28.80 5.18 0.039 1.04 3 4 1 23.06 1.73 4.89 0.010 1.32 0 1 6 77.36 37.05 4.49 0.045 2.49 -5 2 2 26.45 0.39 4.16 0.005 1.11 -5 4 8 33.56 1.64 4.15 0.009 0.91 1 0 4 10968.89 12845.73 3.96 0.833 3.11 2 4 4 40.42 6.28 3.94 0.018 1.42 -1 1 6 120.73 77.90 3.49 0.065 2.37 2 4 0 254.20 4.15 3.47 0.015 1.56 4 0 14 -5.06 85.22 3.45 0.068 0.85 2 0 0 2255.92 2690.23 3.42 0.381 2.88 2 5 0 55.25 26.85 3.38 0.038 1.32 -5 2 8 19.77 1.31 3.37 0.008 1.01 -1 0 4 2096.47 2480.03 3.34 0.366 3.44 0 1 1 449.93 584.93 3.31 0.178 6.73 -2 6 4 13.63 0.16 3.13 0.003 1.11 1 0 2 2879.05 3353.88 3.07 0.425 4.43 2 0 2 1089.58 1276.16 3.05 0.262 2.62 -5 3 6 35.67 16.07 3.03 0.029 1.01 -1 2 3 203.88 153.29 2.99 0.091 2.76 3 5 0 9.14 0.01 2.98 0.001 1.18 -3 4 9 98.83 62.98 2.97 0.058 1.10 2 2 2 102.28 142.14 2.88 0.088 2.14 3 0 2 171.29 124.46 2.88 0.082 1.82 2 1 5 606.56 451.68 2.87 0.156 1.95 -3 4 8 15.81 3.30 2.86 0.013 1.15 3 2 0 55.57 14.66 2.84 0.028 1.71 -5 3 2 85.13 53.75 2.82 0.054 1.05 0 3 6 129.65 92.52 2.77 0.071 1.81 0 2 2 380.56 313.52 2.74 0.130 3.36 -3 4 5 28.22 8.29 2.74 0.021 1.27 -3 1 12 220.93 281.42 2.72 0.123 1.13 -4 1 14 183.03 239.93 2.68 0.114 0.93 -1 1 4 2031.18 2279.66 2.65 0.351 3.12 3 4 2 7.39 0.03 2.65 0.001 1.30 -4 4 1 8.44 0.27 2.65 0.004 1.14 5 3 5 32.63 14.93 2.62 0.028 0.96 1 2 3 1626.38 1822.01 2.61 0.314 2.62 0 2 0 16933.43 18527.81 2.59 1.000 3.72 2 1 12 127.19 176.80 2.55 0.098 1.14 2 5 16 32.44 64.61 2.53 0.059 0.77 -1 3 6 62.32 40.31 2.53 0.047 1.76 -3 4 7 1634.58 1465.81 2.51 0.281 1.19 3 8 5 30.84 71.49 2.50 0.062 0.80 -3 3 8 198.55 155.88 2.50 0.092 1.26 0 2 8 684.84 594.92 2.47 0.179 1.75 2 1 0 524.49 605.51 2.43 0.181 2.69 -1 2 1 2938.83 3225.65 2.43 0.417 3.10 -3 3 7 1148.97 1023.92 2.42 0.235 1.31 6 1 1 232.23 172.92 2.39 0.097 0.94 Bond lengths and angles C1 - Distance Angles C6 1.3897 (0.0032) C2 1.3943 (0.0032) 120.80 (0.21) S1 1.7750 (0.0023) 118.57 (0.18) 120.60 (0.17) C1 - C6 C2 C2 - Distance Angles C3 1.3899 (0.0031) C1 1.3943 (0.0032) 119.32 (0.21) H2 0.9500 120.34 120.34 C2 - C3 C1 C3 - Distance Angles C4 1.3877 (0.0032) C2 1.3899 (0.0031) 119.21 (0.21) H3 0.9500 120.39 120.39 C3 - C4 C2 C4 - Distance Angles C5 1.3815 (0.0032) C3 1.3877 (0.0032) 122.09 (0.21) N4 1.4721 (0.0028) 118.73 (0.20) 119.15 (0.20) C4 - C5 C3 C5 - Distance Angles C4 1.3815 (0.0032) C6 1.3944 (0.0032) 118.59 (0.21) H5 0.9500 120.70 120.70 C5 - C4 C6 C6 - Distance Angles C1 1.3897 (0.0032) C5 1.3944 (0.0032) 119.98 (0.21) H6 0.9500 120.01 120.01 C6 - C1 C5 N4 - Distance Angles C4 1.4721 (0.0028) H4A 0.9100 109.47 H4B 0.9100 109.47 109.47 H4C 0.9100 109.47 109.47 109.47 N4 - C4 H4A H4B O1A - Distance Angles S1 1.4623 (0.0018) O1A - O1B - Distance Angles S1 1.4556 (0.0019) O1B - O1C - Distance Angles S1 1.4522 (0.0017) O1C - S1 - Distance Angles O1C 1.4522 (0.0017) O1B 1.4556 (0.0019) 112.52 (0.11) O1A 1.4623 (0.0018) 111.36 (0.11) 113.13 (0.12) C1 1.7750 (0.0023) 107.24 (0.10) 106.01 (0.11) 106.03 (0.11) S1 - O1C O1B O1A Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.89 2.762(3) 161.3 N4-H4A...O1B_$1 0.91 1.89 2.785(3) 165.5 N4-H4B...O1A_$2 0.91 2.09 2.877(3) 143.7 N4-H4C...O1C_$3 0.91 2.99 3.642(2) 130.2 N4-H4C...S1_$3 0.91 2.41 3.054(3) 127.4 N4-H4C...O1A_$4 FMAP and GRID set by program FMAP 2 1 16 GRID -3.846 -2 -1 3.846 2 1 R1 = 0.0584 for 1567 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.33 at 0.0177 0.7354 0.0503 [ 0.65 A from C1 ] Deepest hole -0.53 at 0.3904 0.7042 0.1316 [ 0.75 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 1769 / 18209 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0177 0.7354 0.0503 1.00000 0.05 0.33 0.65 C1 0.78 C2 1.52 H2 1.78 C6 Q2 1 -0.0199 0.6871 -0.2825 1.00000 0.05 0.29 1.41 H4A 1.46 O1B 2.00 H2 2.23 N4 Q3 1 0.3913 0.4930 0.2424 1.00000 0.05 0.28 1.61 O1C 1.63 H4C 1.92 O1A 1.98 O1B Q4 1 0.0046 0.7454 -0.0923 1.00000 0.05 0.27 0.68 C4 0.73 C5 1.52 H5 1.76 C3 Q5 1 0.0356 0.4884 -0.1230 1.00000 0.05 0.26 1.56 H5 1.63 C5 1.92 O1B 2.16 C1 Q6 1 0.5494 0.9445 0.1262 1.00000 0.05 0.26 1.33 O1A 1.98 H2 2.12 H4B 2.15 H3 Q7 1 0.1790 0.7224 0.0886 1.00000 0.05 0.26 0.58 C1 1.21 S1 1.72 C2 1.77 C6 Q8 1 0.1815 0.7137 -0.0521 1.00000 0.05 0.25 0.70 C6 0.79 C5 1.46 H6 1.54 H5 Q9 1 0.4349 0.9231 0.2417 1.00000 0.05 0.24 1.16 O1A 1.67 H4B 1.80 H4C 2.01 O1C Q10 1 -0.1623 0.7785 -0.1303 1.00000 0.05 0.24 0.52 C4 0.96 N4 1.51 H4C 1.51 H4B Shortest distances between peaks (including symmetry equivalents) 1 7 1.06 4 10 1.11 3 9 1.14 4 8 1.17 1 8 1.98 4 5 1.98 6 9 2.03 1 5 2.07 5 7 2.11 3 6 2.11 5 8 2.14 7 8 2.24 1 4 2.26 8 10 2.28 5 10 2.44 2 7 2.55 2 3 2.67 2 5 2.69 6 7 2.72 2 10 2.73 2 9 2.75 1 2 2.75 3 10 2.92 2 6 2.92 2 5 2.92 4 7 2.95 3 5 2.95 1 10 2.97 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 0.00: Analyse other restraints etc. 0.39: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.14: Structure factors and derivatives 0.16: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.05: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0079p21c finished at 16:01:00 Total CPU time: 0.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++