+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0076p21c started at 11:20:39 on 15-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0076p21c in P2(1)/c CELL 0.71073 14.0939 4.9227 11.3731 90.000 97.321 90.000 ZERR 4.00 0.0006 0.0002 0.0005 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S NA UNIT 24 24 4 12 4 4 V = 782.63 F(000) = 400.0 Mu = 0.43 mm-1 Cell Wt = 780.67 Rho = 1.656 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB N2 O1C EQIV_$1 x, -y-1/2, z-1/2 HTAB N2 O1A_$1 HTAB N2 S1_$1 FMAP 2 PLAN 10 SIZE 0.02 0.09 0.13 ACTA BOND $H WGHT 0.02810 2.00310 L.S. 4 TEMP -153.00 FVAR 0.74441 NA1 6 0.553677 -0.016714 0.133630 11.00000 0.02446 0.01754 = 0.01422 0.00055 0.00190 -0.00132 MOLE 1 C1 1 0.739421 0.001962 0.391527 11.00000 0.01887 0.01664 = 0.01875 0.00200 0.00026 0.00344 C2 1 0.754931 -0.170456 0.297161 11.00000 0.02414 0.01649 = 0.01940 0.00094 0.00330 0.00322 C3 1 0.845174 -0.164897 0.257881 11.00000 0.02748 0.02741 = 0.03385 -0.00099 0.00843 0.00342 AFIX 43 H3 2 0.857176 -0.276565 0.193267 11.00000 -1.20000 AFIX 0 C4 1 0.916649 0.000284 0.311720 11.00000 0.02176 0.03431 = 0.05889 -0.00354 0.01247 -0.00022 AFIX 43 H4 2 0.977185 0.002290 0.283329 11.00000 -1.20000 AFIX 0 C5 1 0.901476 0.164386 0.407158 11.00000 0.02536 0.03107 = 0.05398 -0.00666 -0.00140 -0.00694 AFIX 43 H5 2 0.951841 0.273674 0.445235 11.00000 -1.20000 AFIX 0 C6 1 0.812649 0.167054 0.446038 11.00000 0.02651 0.02021 = 0.03070 -0.00329 -0.00264 -0.00167 AFIX 43 H6 2 0.801330 0.281521 0.510045 11.00000 -1.20000 AFIX 0 N2 3 0.681713 -0.328946 0.240981 11.00000 0.02122 0.02278 = 0.01709 -0.00716 0.00349 0.00010 AFIX 93 H1 2 0.691393 -0.428668 0.179403 11.00000 -1.20000 H2 2 0.625458 -0.330042 0.266821 11.00000 -1.20000 AFIX 0 O1A 4 0.634353 0.194058 0.540690 11.00000 0.03579 0.01539 = 0.01208 -0.00180 0.00271 0.00216 O1B 4 0.565809 0.165227 0.333391 11.00000 0.02330 0.01640 = 0.01334 0.00113 0.00141 0.00328 O1C 4 0.588758 -0.244234 0.451875 11.00000 0.02745 0.01410 = 0.01774 0.00160 0.00633 -0.00152 S1 5 0.623417 0.030620 0.433438 11.00000 0.02266 0.01297 = 0.01210 0.00024 0.00219 0.00107 HKLF 4 Covalent radii and connectivity table for 06skc0076p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 NA 1.860 Na1 - O1A_$7 O1B_$3 O1B O1C_$1 O1C_$4 N2 Na1_$2 S1_$3 Na1_$4 Na1_$3 C1 - C6 C2 S1 C2 - N2 C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 C6 - C5 C1 N2 - C2 Na1 O1A - S1 Na1_$6 O1B - S1 Na1_$4 Na1 O1C - S1 Na1_$5 Na1_$3 S1 - O1A O1C O1B C1 Na1_$4 Operators for generating equivalent atoms: $1 x, -y-1/2, z-1/2 $2 -x+1, -y, -z $3 -x+1, y-1/2, -z+1/2 $4 -x+1, y+1/2, -z+1/2 $5 x, -y-1/2, z+1/2 $6 x, -y+1/2, z+1/2 $7 x, -y+1/2, z-1/2 12224 Reflections read, of which 772 rejected -18 =< h =< 18, -6 =< k =< 6, -14 =< l =< 14, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 11 1 5 270.71 8.07 5 57.34 -7 2 9 -0.85 0.34 9 2.02 2 Inconsistent equivalents 1804 Unique reflections, of which 0 suppressed R(int) = 0.0716 R(sigma) = 0.0478 Friedel opposites merged Maximum memory for data reduction = 1630 / 18149 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 = 1919 / 142650 wR2 = 0.1150 before cycle 1 for 1804 data and 109 / 109 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0281 * P )^2 + 2.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74442 0.00203 0.003 OSF Mean shift/esd = 0.002 Maximum = -0.011 for U22 S1 Max. shift = 0.000 A for Na1 Max. dU = 0.000 for S1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1919 / 142650 wR2 = 0.1150 before cycle 2 for 1804 data and 109 / 109 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0281 * P )^2 + 2.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74441 0.00203 -0.003 OSF Mean shift/esd = 0.001 Maximum = -0.004 for U22 S1 Max. shift = 0.000 A for C6 Max. dU = 0.000 for S1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1919 / 142650 wR2 = 0.1150 before cycle 3 for 1804 data and 109 / 109 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0281 * P )^2 + 2.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74441 0.00203 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U11 C4 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1919 / 142650 wR2 = 0.1150 before cycle 4 for 1804 data and 109 / 109 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0281 * P )^2 + 2.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.74441 0.00203 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x S1 Max. shift = 0.000 A for O1B 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 H3 0.8572 -0.2766 0.1933 43 0.950 0.000 C3 C4 C2 H4 0.9772 0.0023 0.2833 43 0.950 0.000 C4 C3 C5 H5 0.9518 0.2737 0.4452 43 0.950 0.000 C5 C6 C4 H6 0.8013 0.2815 0.5100 43 0.950 0.000 C6 C5 C1 ** Bond(s) to Na1 ignored in idealizing H-atoms attached to N2 ** H1 0.6914 -0.4287 0.1794 93 0.880 0.000 N2 C2 C3 H2 0.6255 -0.3300 0.2668 93 0.880 0.000 N2 C2 C3 06skc0076p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Na1 0.55368 -0.01671 0.13363 1.00000 0.02446 0.01754 0.01422 0.00055 0.00190 -0.00132 0.01879 0.00199 0.00008 0.00023 0.00009 0.00000 0.00063 0.00060 0.00055 0.00046 0.00045 0.00047 0.00029 C1 0.73942 0.00196 0.39153 1.00000 0.01887 0.01664 0.01875 0.00200 0.00026 0.00344 0.01827 0.00524 0.00020 0.00059 0.00025 0.00000 0.00137 0.00144 0.00135 0.00117 0.00109 0.00115 0.00059 C2 0.75493 -0.17046 0.29716 1.00000 0.02414 0.01649 0.01940 0.00094 0.00330 0.00322 0.01997 0.00545 0.00021 0.00061 0.00026 0.00000 0.00152 0.00147 0.00141 0.00118 0.00119 0.00119 0.00062 C3 0.84517 -0.16490 0.25788 1.00000 0.02748 0.02741 0.03385 -0.00099 0.00843 0.00342 0.02919 0.00636 0.00023 0.00071 0.00031 0.00000 0.00168 0.00179 0.00175 0.00149 0.00143 0.00143 0.00074 H3 0.85718 -0.27657 0.19327 1.00000 0.03503 0.00000 0.00000 C4 0.91665 0.00028 0.31172 1.00000 0.02176 0.03431 0.05889 -0.00354 0.01247 -0.00022 0.03769 0.00697 0.00025 0.00078 0.00037 0.00000 0.00166 0.00207 0.00243 0.00183 0.00163 0.00150 0.00088 H4 0.97719 0.00229 0.28333 1.00000 0.04522 0.00000 0.00000 C5 0.90148 0.16439 0.40716 1.00000 0.02536 0.03107 0.05398 -0.00666 -0.00140 -0.00694 0.03736 0.00651 0.00025 0.00076 0.00036 0.00000 0.00174 0.00198 0.00235 0.00179 0.00165 0.00150 0.00088 H5 0.95184 0.27367 0.44523 1.00000 0.04483 0.00000 0.00000 C6 0.81265 0.16705 0.44604 1.00000 0.02651 0.02021 0.03070 -0.00329 -0.00264 -0.00167 0.02635 0.00565 0.00023 0.00066 0.00029 0.00000 0.00165 0.00161 0.00170 0.00137 0.00135 0.00130 0.00070 H6 0.80133 0.28152 0.51005 1.00000 0.03162 0.00000 0.00000 N2 0.68171 -0.32895 0.24098 1.00000 0.02122 0.02278 0.01709 -0.00716 0.00349 0.00010 0.02027 0.00432 0.00017 0.00052 0.00021 0.00000 0.00129 0.00136 0.00117 0.00106 0.00099 0.00106 0.00055 H1 0.69139 -0.42867 0.17940 1.00000 0.02433 0.00000 0.00000 H2 0.62546 -0.33004 0.26682 1.00000 0.02433 0.00000 0.00000 O1A 0.63435 0.19406 0.54069 1.00000 0.03579 0.01539 0.01208 -0.00180 0.00271 0.00216 0.02111 0.00367 0.00016 0.00041 0.00017 0.00000 0.00122 0.00105 0.00095 0.00080 0.00085 0.00089 0.00048 O1B 0.56581 0.16523 0.33339 1.00000 0.02330 0.01640 0.01334 0.00113 0.00141 0.00328 0.01776 0.00356 0.00014 0.00040 0.00016 0.00000 0.00104 0.00104 0.00092 0.00081 0.00079 0.00083 0.00045 O1C 0.58876 -0.24423 0.45187 1.00000 0.02745 0.01410 0.01774 0.00160 0.00633 -0.00152 0.01946 0.00367 0.00015 0.00041 0.00017 0.00000 0.00112 0.00102 0.00099 0.00082 0.00085 0.00084 0.00046 S1 0.62342 0.03062 0.43344 1.00000 0.02266 0.01297 0.01210 0.00024 0.00219 0.00107 0.01591 0.00126 0.00005 0.00014 0.00006 0.00000 0.00037 0.00034 0.00033 0.00027 0.00025 0.00028 0.00019 Final Structure Factor Calculation for 06skc0076p21c in P2(1)/c Total number of l.s. parameters = 109 Maximum vector length = 511 Memory required = 1810 / 25039 wR2 = 0.1150 before cycle 5 for 1804 data and 0 / 109 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0281 * P )^2 + 2.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0520 for 1450 Fo > 4sig(Fo) and 0.0716 for all 1804 data wR2 = 0.1150, GooF = S = 1.078, Restrained GooF = 1.078 for all data Occupancy sum of asymmetric unit = 12.00 for non-hydrogen and 6.00 for hydrogen atoms Principal mean square atomic displacements U 0.0249 0.0174 0.0141 Na1 0.0218 0.0199 0.0131 C1 0.0253 0.0193 0.0153 C2 0.0357 0.0299 0.0220 C3 0.0600 0.0339 0.0192 C4 0.0573 0.0355 0.0193 C5 0.0363 0.0247 0.0180 C6 0.0276 0.0213 0.0119 N2 0.0362 0.0160 0.0111 O1A 0.0247 0.0158 0.0128 O1B 0.0282 0.0174 0.0127 O1C 0.0228 0.0129 0.0120 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.030 0.045 0.060 0.079 0.101 0.128 0.163 0.224 1.000 Number in group 188. 174. 184. 176. 187. 175. 186. 176. 176. 182. GooF 1.172 1.190 1.084 1.043 1.034 1.182 0.971 0.972 1.023 1.085 K 4.638 1.479 1.040 1.060 1.024 1.013 0.994 1.013 1.005 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.04 1.14 1.32 1.64 inf Number in group 181. 182. 179. 185. 177. 178. 181. 179. 181. 181. GooF 1.161 1.132 1.096 1.002 0.897 1.022 0.868 0.908 1.082 1.478 K 1.064 1.060 1.049 1.021 1.001 1.005 1.000 0.986 1.009 1.009 R1 0.187 0.138 0.124 0.109 0.077 0.070 0.039 0.040 0.041 0.036 Recommended weighting scheme: WGHT 0.0281 2.0031 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) 4 1 3 53.35 16.59 4.18 0.032 2.17 1 1 4 706.33 531.00 4.12 0.182 2.37 -6 0 2 667.91 861.60 3.69 0.231 2.26 6 1 3 29.90 5.04 3.67 0.018 1.75 -7 4 9 56.15 119.63 3.33 0.086 0.83 -1 1 4 6935.81 6071.71 3.26 0.614 2.46 -9 0 12 259.68 115.10 3.21 0.085 0.85 3 1 3 828.59 1008.18 3.20 0.250 2.41 4 1 1 73.60 126.61 3.19 0.089 2.70 -17 1 3 69.13 18.98 3.07 0.034 0.81 -9 4 9 58.36 12.45 3.04 0.028 0.80 -2 0 6 183.01 122.92 2.87 0.087 1.88 -1 2 2 19.13 3.29 2.86 0.014 2.25 5 2 0 69.48 37.03 2.81 0.048 1.85 -6 3 1 23.39 4.91 2.77 0.017 1.34 -12 0 6 50.71 102.46 2.75 0.080 1.05 -4 6 2 32.58 0.27 2.74 0.004 0.79 9 4 1 81.37 41.25 2.70 0.051 0.95 -6 2 10 49.70 88.91 2.69 0.074 0.98 16 2 0 293.90 210.16 2.69 0.114 0.82 5 1 1 352.84 277.50 2.63 0.131 2.32 5 2 5 20.60 4.43 2.63 0.017 1.37 -9 0 10 28.05 0.18 2.62 0.003 0.97 -4 3 1 166.43 117.27 2.58 0.085 1.48 -5 1 9 18.00 2.57 2.55 0.013 1.17 7 5 3 31.14 1.59 2.54 0.010 0.85 -18 0 4 407.27 292.46 2.53 0.135 0.77 16 1 5 31.78 0.07 2.50 0.002 0.77 1 3 11 23.91 0.86 2.50 0.007 0.86 -3 2 4 30.65 58.15 2.49 0.060 1.77 0 1 4 407.62 329.06 2.48 0.143 2.45 11 0 10 48.00 5.61 2.44 0.019 0.79 -13 2 9 100.05 54.24 2.43 0.058 0.82 -4 0 6 244.18 184.31 2.42 0.107 1.75 8 0 12 -7.86 26.26 2.39 0.040 0.79 -9 5 2 302.63 232.99 2.39 0.120 0.83 -2 1 5 895.67 770.33 2.39 0.219 2.03 -7 4 6 24.08 2.45 2.38 0.012 0.94 -16 1 1 533.21 433.64 2.38 0.164 0.87 7 0 12 156.71 88.79 2.38 0.074 0.81 7 1 1 377.33 458.95 2.37 0.169 1.79 13 0 8 127.53 34.74 2.34 0.046 0.81 1 2 0 249.00 314.12 2.32 0.140 2.42 -7 1 5 217.72 278.35 2.31 0.132 1.52 -3 2 2 174.82 130.19 2.30 0.090 2.07 2 6 0 56.09 23.15 2.29 0.038 0.81 -8 2 2 396.61 478.65 2.28 0.173 1.42 -8 1 5 196.89 252.90 2.28 0.125 1.41 -9 1 11 -21.38 19.27 2.28 0.035 0.90 8 2 11 24.35 0.01 2.27 0.001 0.79 Bond lengths and angles Na1 - Distance Angles O1A_$7 2.2889 (0.0023) O1B_$3 2.3641 (0.0022) 159.82 (0.09) O1B 2.4277 (0.0022) 101.32 (0.08) 93.58 (0.06) O1C_$1 2.4825 (0.0022) 77.35 (0.08) 92.27 (0.08) 163.01 (0.08) O1C_$4 2.5054 (0.0023) 82.52 (0.08) 82.21 (0.08) 97.07 (0.08) 99.52 (0.07) N2 2.5589 (0.0027) 105.99 (0.09) 89.99 (0.08) 79.27 (0.08) 84.80 (0.08) 171.19 (0.09) Na1_$2 3.2223 (0.0021) 74.34 (0.06) 85.71 (0.06) 146.36 (0.08) 50.07 (0.06) 49.45 (0.05) 134.31 (0.08) S1_$3 3.3603 (0.0013) 138.91 (0.07) 22.08 (0.05) 114.76 (0.06) 73.60 (0.06) 74.44 (0.06) 99.68 (0.07) 64.78 (0.04) Na1_$4 4.0466 (0.0017) 97.42 (0.05) 88.04 (0.06) 31.91 (0.05) 164.53 (0.07) 65.19 (0.05) 110.67 (0.07) 114.60 (0.05) Na1_$3 4.0466 (0.0017) 166.73 (0.07) 32.87 (0.05) 66.41 (0.06) 112.77 (0.05) 103.39 (0.07) 67.81 (0.06) 118.58 (0.06) Na1 - O1A_$7 O1B_$3 O1B O1C_$1 O1C_$4 N2 Na1_$2 C1 - Distance Angles C6 1.3953 (0.0042) C2 1.4071 (0.0041) 120.81 (0.28) S1 1.7660 (0.0030) 119.43 (0.23) 119.55 (0.23) C1 - C6 C2 C2 - Distance Angles N2 1.3834 (0.0038) C3 1.4010 (0.0043) 121.19 (0.28) C1 1.4071 (0.0041) 120.88 (0.27) 117.84 (0.28) C2 - N2 C3 C3 - Distance Angles C4 1.3761 (0.0050) C2 1.4010 (0.0043) 120.83 (0.32) H3 0.9500 119.58 119.58 C3 - C4 C2 C4 - Distance Angles C3 1.3761 (0.0050) C5 1.3913 (0.0053) 120.91 (0.32) H4 0.9500 119.55 119.55 C4 - C3 C5 C5 - Distance Angles C6 1.3799 (0.0048) C4 1.3913 (0.0053) 119.44 (0.32) H5 0.9500 120.28 120.28 C5 - C6 C4 C6 - Distance Angles C5 1.3799 (0.0048) C1 1.3953 (0.0042) 120.13 (0.31) H6 0.9500 119.93 119.93 C6 - C5 C1 N2 - Distance Angles C2 1.3834 (0.0038) Na1 2.5589 (0.0027) 108.71 (0.18) H1 0.8800 120.00 97.28 H2 0.8800 120.00 63.41 120.00 N2 - C2 Na1 H1 O1A - Distance Angles S1 1.4529 (0.0020) Na1_$6 2.2889 (0.0023) 140.01 (0.13) O1A - S1 O1B - Distance Angles S1 1.4689 (0.0020) Na1_$4 2.3641 (0.0022) 120.70 (0.11) Na1 2.4277 (0.0022) 121.64 (0.11) 115.22 (0.08) O1B - S1 Na1_$4 O1C - Distance Angles S1 1.4627 (0.0021) Na1_$5 2.4825 (0.0022) 131.56 (0.12) Na1_$3 2.5054 (0.0023) 134.85 (0.12) 80.48 (0.07) O1C - S1 Na1_$5 S1 - Distance Angles O1A 1.4529 (0.0020) O1C 1.4627 (0.0021) 113.17 (0.12) O1B 1.4689 (0.0020) 112.93 (0.12) 111.51 (0.12) C1 1.7660 (0.0030) 105.55 (0.13) 107.60 (0.13) 105.44 (0.12) Na1_$4 3.3603 (0.0013) 79.61 (0.09) 113.20 (0.09) 37.23 (0.08) 132.70 (0.10) S1 - O1A O1C O1B C1 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.27 2.906(3) 129.0 N2-H2...O1C 0.88 2.13 2.912(3) 148.3 N2-H1...O1A_$1 0.88 2.88 3.628(2) 143.4 N2-H1...S1_$1 FMAP and GRID set by program FMAP 2 2 9 GRID -4.167 -2 -2 4.167 2 2 R1 = 0.0709 for 1804 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.56 at 0.3170 0.0021 0.5785 [ 0.88 A from S1 ] Deepest hole -0.44 at 0.3899 0.1802 0.2458 [ 0.25 A from H2 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 2201 / 15987 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6830 -0.0021 0.4215 1.00000 0.05 0.56 0.88 S1 0.90 C1 1.85 O1C 1.86 O1A Q2 1 0.6317 -0.4423 0.2866 1.00000 0.05 0.43 0.60 H2 1.08 N2 1.57 H1 2.18 C2 Q3 1 0.5021 0.0846 0.3183 1.00000 0.05 0.38 0.98 O1B 1.98 H2 2.03 S1 2.21 NA1 Q4 1 0.5262 -0.3022 0.4491 1.00000 0.05 0.30 0.92 O1C 1.73 NA1 2.16 S1 2.27 NA1 Q5 1 0.9391 -0.3804 0.3239 1.00000 0.05 0.30 1.79 C3 1.83 H3 1.89 H4 1.90 C4 Q6 1 0.5736 -0.0995 0.4409 1.00000 0.05 0.29 0.75 O1C 0.96 S1 1.78 O1B 1.97 O1A Q7 1 0.6443 -0.2474 0.2161 1.00000 0.05 0.28 0.69 N2 0.78 H2 1.22 H1 1.75 C2 Q8 1 0.7962 -0.0991 0.2732 1.00000 0.05 0.28 0.76 C2 0.80 C3 1.59 H3 1.72 C1 Q9 1 0.5568 -0.0482 0.4278 1.00000 0.05 0.28 1.01 S1 1.09 O1C 1.52 O1B 1.98 O1A Q10 1 0.8231 -0.1997 0.3141 1.00000 0.05 0.27 0.77 C3 0.97 C2 1.56 H3 1.65 C4 Shortest distances between peaks (including symmetry equivalents) 6 9 0.36 8 10 0.75 4 6 1.21 2 7 1.28 4 9 1.35 3 9 1.53 1 6 1.66 1 9 1.80 3 6 1.85 5 10 1.85 2 3 2.10 3 7 2.21 7 8 2.28 3 4 2.41 4 4 2.43 5 8 2.45 9 9 2.48 1 8 2.51 4 9 2.59 2 4 2.61 6 9 2.61 1 7 2.62 7 10 2.63 1 10 2.64 2 6 2.64 1 2 2.70 1 3 2.70 1 4 2.71 6 6 2.79 2 9 2.81 4 6 2.81 2 8 2.89 3 3 2.91 3 4 2.93 2 10 2.93 3 7 2.94 6 7 2.95 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.56: 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 0.19: Structure factors and derivatives 0.20: 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 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0076p21c finished at 11:20:40 Total CPU time: 1.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++