+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0030p21n started at 16:13:03 on 29-Jan-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0030p21n in P2(1)/n CELL 0.71073 7.9081 5.6870 24.1173 90.000 98.322 90.000 ZERR 4.00 0.0008 0.0006 0.0024 0.000 0.007 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O S UNIT 40 48 8 12 4 V = 1073.22 F(000) = 504.0 Mu = 0.29 mm-1 Cell Wt = 961.10 Rho = 1.487 MERG 2 OMIT -3.00 55.00 OMIT 1 3 1 OMIT -3 4 3 SHEL 7 0.77 EQIV_$1 -x+3/2, y-1/2, -z+1/2 HTAB N21 O1A_$1 EQIV_$2 -x+3/2, y+1/2, -z+1/2 HTAB N21 O1C_$2 EQIV_$3 -x+5/2, y+1/2, -z+1/2 HTAB N23 O1B_$3 EQIV_$4 x+1/2, -y+3/2, z+1/2 HTAB N23 O1B_$4 FMAP 2 PLAN 10 SIZE 0.01 0.07 0.10 ACTA BOND $H WGHT 0.01260 3.86030 L.S. 4 TEMP -153.00 FVAR 0.66051 MOLE 1 C4 1 0.993373 0.664822 0.254213 11.00000 0.01946 0.04165 = 0.02894 0.00027 0.00579 -0.00535 C3 1 1.038151 0.451481 0.232002 11.00000 0.02307 0.04226 = 0.03409 0.00555 0.00286 0.00717 AFIX 43 H3 2 1.121919 0.355187 0.253222 11.00000 -1.20000 AFIX 0 C2 1 0.962157 0.376734 0.179148 11.00000 0.02513 0.02763 = 0.03629 -0.00172 0.00371 0.00552 AFIX 43 H2 2 0.994464 0.230700 0.164682 11.00000 -1.20000 AFIX 0 C1 1 0.839474 0.515178 0.147644 11.00000 0.01921 0.02872 = 0.02821 0.00192 0.00225 0.00233 C6 1 0.796149 0.731999 0.169485 11.00000 0.02903 0.02771 = 0.03291 0.00188 0.00173 0.00372 AFIX 43 H6 2 0.714999 0.831567 0.148107 11.00000 -1.20000 AFIX 0 C5 1 0.872114 0.799962 0.222245 11.00000 0.02556 0.02689 = 0.03364 -0.00255 0.00795 -0.00118 AFIX 43 H5 2 0.839408 0.945273 0.236970 11.00000 -1.20000 AFIX 0 C7 1 1.069804 0.741488 0.312225 11.00000 0.03200 0.04115 = 0.03300 -0.00107 0.00456 -0.00070 AFIX 137 H7A 2 1.096408 0.909746 0.311915 11.00000 -1.50000 H7B 2 1.174819 0.652402 0.324208 11.00000 -1.50000 H7C 2 0.987922 0.712204 0.338300 11.00000 -1.50000 AFIX 0 O1A 4 0.593718 0.565524 0.065451 11.00000 0.01748 0.02868 = 0.03501 0.00089 0.00138 0.00383 O1B 4 0.876957 0.483047 0.043216 11.00000 0.02229 0.03104 = 0.03096 0.00316 0.00766 -0.00014 O1C 4 0.716592 0.175262 0.082142 11.00000 0.02422 0.02533 = 0.03506 0.00283 0.00446 0.00080 S1 5 0.749100 0.427016 0.079338 11.00000 0.01914 0.02579 = 0.02759 0.00133 0.00260 0.00177 MOLE 2 C22 1 1.188140 0.642175 0.457293 11.00000 0.02672 0.03740 = 0.02743 -0.00317 -0.00134 0.00756 AFIX 43 H22 2 1.121478 0.758990 0.472159 11.00000 -1.20000 AFIX 0 C24 1 1.403439 0.456053 0.428928 11.00000 0.02718 0.03214 = 0.03564 0.00612 0.00635 0.00577 AFIX 43 H24 2 1.514566 0.422777 0.420414 11.00000 -1.20000 AFIX 0 C25 1 1.267251 0.313020 0.420553 11.00000 0.03920 0.02689 = 0.03309 0.00011 0.00243 0.00037 AFIX 43 H25 2 1.263848 0.158557 0.405433 11.00000 -1.20000 AFIX 0 N21 3 1.134405 0.432123 0.437942 11.00000 0.02513 0.04471 = 0.03140 0.00494 0.00069 -0.00890 AFIX 43 H21 2 1.029567 0.378219 0.436554 11.00000 0.08336 AFIX 0 N23 3 1.352358 0.657922 0.451932 11.00000 0.02334 0.03269 = 0.03240 0.00065 -0.00113 -0.00317 AFIX 43 H23 2 1.418197 0.780127 0.461742 11.00000 0.10132 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0030p21n in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C4 - C5 C3 C7 C3 - C4 C2 C2 - C1 C3 C1 - C2 C6 S1 C6 - C5 C1 C5 - C4 C6 C7 - C4 O1A - S1 O1B - S1 O1C - S1 S1 - O1A O1C O1B C1 C22 - N23 N21 C24 - C25 N23 C25 - C24 N21 N21 - C22 C25 N23 - C22 C24 Operators for generating equivalent atoms: $1 -x+3/2, y-1/2, -z+1/2 $2 -x+3/2, y+1/2, -z+1/2 $3 -x+5/2, y+1/2, -z+1/2 $4 x+1/2, -y+3/2, z+1/2 h k l Fo^2 Sigma Why rejected 0 3 0 404.91 54.95 observed but should be systematically absent 0 3 0 724.83 166.37 observed but should be systematically absent 0 3 0 433.96 99.94 observed but should be systematically absent 0 3 0 404.95 98.91 observed but should be systematically absent -6 0 1 24.73 5.37 observed but should be systematically absent -2 0 1 21.92 5.18 observed but should be systematically absent -2 0 1 26.46 6.33 observed but should be systematically absent -7 0 2 21.79 4.92 observed but should be systematically absent -5 0 2 65.05 14.76 observed but should be systematically absent -5 0 2 63.06 13.43 observed but should be systematically absent -5 0 2 57.33 11.98 observed but should be systematically absent -5 0 2 42.51 8.02 observed but should be systematically absent 1 0 2 32.74 6.93 observed but should be systematically absent 1 0 2 37.35 6.22 observed but should be systematically absent 1 0 2 30.79 7.06 observed but should be systematically absent -6 0 3 29.15 7.19 observed but should be systematically absent -6 0 3 46.50 10.27 observed but should be systematically absent -7 0 4 33.91 7.05 observed but should be systematically absent -5 0 4 264.47 44.54 observed but should be systematically absent -7 0 6 48.99 11.44 observed but should be systematically absent -8 0 7 54.45 12.30 observed but should be systematically absent -4 0 11 36.59 8.81 observed but should be systematically absent 21749 Reflections read, of which 1260 rejected -10 =< h =< 10, -7 =< k =< 7, -31 =< l =< 31, Max. 2-theta = 54.94 22 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 4 2 4 28.12 3.88 7 51.20 -4 1 5 41.52 1.13 12 8.90 -6 2 5 98.98 2.48 10 39.92 -8 0 14 37.91 2.46 4 18.91 4 Inconsistent equivalents 2459 Unique reflections, of which 0 suppressed R(int) = 0.1427 R(sigma) = 0.0751 Friedel opposites merged Maximum memory for data reduction = 1731 / 24890 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 = 2137 / 186595 wR2 = 0.1697 before cycle 1 for 2459 data and 148 / 148 parameters GooF = S = 1.195; Restrained GooF = 1.195 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0126 * P )^2 + 3.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.66068 0.00210 0.079 OSF Mean shift/esd = 0.006 Maximum = 0.079 for OSF Max. shift = 0.000 A for H7B Max. dU = 0.000 for H21 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2137 / 186595 wR2 = 0.1697 before cycle 2 for 2459 data and 148 / 148 parameters GooF = S = 1.195; Restrained GooF = 1.195 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0126 * P )^2 + 3.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.66071 0.00210 0.016 OSF Mean shift/esd = 0.002 Maximum = 0.016 for OSF Max. shift = 0.000 A for H7B Max. dU = 0.000 for H21 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2137 / 186595 wR2 = 0.1697 before cycle 3 for 2459 data and 148 / 148 parameters GooF = S = 1.195; Restrained GooF = 1.195 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0126 * P )^2 + 3.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.66071 0.00210 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for U11 H21 Max. shift = 0.000 A for H7B Max. dU = 0.000 for H21 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2137 / 186595 wR2 = 0.1697 before cycle 4 for 2459 data and 148 / 148 parameters GooF = S = 1.195; Restrained GooF = 1.195 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0126 * P )^2 + 3.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.66071 0.00210 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U11 H21 Max. shift = 0.000 A for H7B Max. dU = 0.000 for H21 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 1.1219 0.3552 0.2532 43 0.950 0.000 C3 C4 C2 H2 0.9945 0.2307 0.1647 43 0.950 0.000 C2 C1 C3 H6 0.7150 0.8316 0.1481 43 0.950 0.000 C6 C5 C1 H5 0.8394 0.9453 0.2370 43 0.950 0.000 C5 C4 C6 H7A 1.0964 0.9098 0.3119 137 0.980 0.000 C7 C4 H7A H7B 1.1748 0.6524 0.3242 137 0.980 0.000 C7 C4 H7A H7C 0.9879 0.7122 0.3383 137 0.980 0.000 C7 C4 H7A H22 1.1215 0.7590 0.4722 43 0.950 0.000 C22 N23 N21 H24 1.5146 0.4228 0.4204 43 0.950 0.000 C24 C25 N23 H25 1.2639 0.1586 0.4054 43 0.950 0.000 C25 C24 N21 H21 1.0296 0.3782 0.4366 43 0.880 0.000 N21 C22 C25 H23 1.4182 0.7801 0.4617 43 0.880 0.000 N23 C22 C24 06skc0030p21n in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C4 0.99337 0.66483 0.25421 1.00000 0.01948 0.04167 0.02896 0.00027 0.00581 -0.00534 0.02981 0.00831 0.00053 0.00094 0.00018 0.00000 0.00210 0.00304 0.00230 0.00210 0.00174 0.00203 0.00108 C3 1.03815 0.45147 0.23200 1.00000 0.02310 0.04227 0.03410 0.00555 0.00285 0.00718 0.03328 0.00902 0.00056 0.00097 0.00019 0.00000 0.00220 0.00304 0.00246 0.00227 0.00182 0.00218 0.00111 H3 1.12193 0.35518 0.25322 1.00000 0.03994 0.00000 0.00000 C2 0.96216 0.37673 0.17915 1.00000 0.02515 0.02765 0.03631 -0.00172 0.00372 0.00553 0.02978 0.00836 0.00054 0.00086 0.00019 0.00000 0.00222 0.00263 0.00249 0.00200 0.00186 0.00195 0.00104 H2 0.99445 0.23068 0.16469 1.00000 0.03573 0.00000 0.00000 C1 0.83948 0.51518 0.14764 1.00000 0.01922 0.02874 0.02826 0.00192 0.00226 0.00233 0.02552 0.00795 0.00051 0.00082 0.00018 0.00000 0.00202 0.00254 0.00219 0.00186 0.00166 0.00184 0.00097 C6 0.79615 0.73200 0.16949 1.00000 0.02907 0.02771 0.03293 0.00189 0.00174 0.00372 0.03017 0.00850 0.00058 0.00085 0.00019 0.00000 0.00240 0.00263 0.00242 0.00202 0.00186 0.00204 0.00104 H6 0.71499 0.83157 0.14811 1.00000 0.03621 0.00000 0.00000 C5 0.87212 0.79996 0.22224 1.00000 0.02557 0.02691 0.03366 -0.00255 0.00795 -0.00118 0.02835 0.00819 0.00054 0.00086 0.00018 0.00000 0.00225 0.00244 0.00237 0.00205 0.00184 0.00201 0.00099 H5 0.83942 0.94528 0.23697 1.00000 0.03402 0.00000 0.00000 C7 1.06980 0.74149 0.31222 1.00000 0.03204 0.04116 0.03300 -0.00107 0.00456 -0.00069 0.03541 0.00877 0.00061 0.00097 0.00019 0.00000 0.00254 0.00316 0.00243 0.00218 0.00195 0.00226 0.00116 H7A 1.09638 0.90976 0.31192 1.00000 0.05312 0.00000 0.00000 H7B 1.17483 0.65243 0.32420 1.00000 0.05312 0.00000 0.00000 H7C 0.98793 0.71217 0.33830 1.00000 0.05312 0.00000 0.00000 O1A 0.59372 0.56553 0.06545 1.00000 0.01750 0.02870 0.03502 0.00088 0.00137 0.00383 0.02732 0.00551 0.00034 0.00059 0.00012 0.00000 0.00139 0.00176 0.00164 0.00144 0.00118 0.00136 0.00070 O1B 0.87696 0.48305 0.04322 1.00000 0.02233 0.03107 0.03097 0.00316 0.00765 -0.00014 0.02775 0.00554 0.00036 0.00057 0.00012 0.00000 0.00150 0.00185 0.00160 0.00136 0.00121 0.00135 0.00073 O1C 0.71659 0.17527 0.08214 1.00000 0.02425 0.02535 0.03507 0.00282 0.00446 0.00079 0.02821 0.00564 0.00037 0.00056 0.00012 0.00000 0.00160 0.00170 0.00168 0.00143 0.00127 0.00134 0.00072 S1 0.74910 0.42702 0.07934 1.00000 0.01916 0.02581 0.02760 0.00134 0.00260 0.00177 0.02427 0.00203 0.00013 0.00020 0.00005 0.00000 0.00050 0.00058 0.00054 0.00049 0.00038 0.00048 0.00028 C22 1.18814 0.64217 0.45729 1.00000 0.02675 0.03741 0.02744 -0.00316 -0.00134 0.00756 0.03105 0.00842 0.00057 0.00090 0.00018 0.00000 0.00235 0.00293 0.00226 0.00205 0.00179 0.00210 0.00108 H22 1.12148 0.75898 0.47216 1.00000 0.03726 0.00000 0.00000 C24 1.40343 0.45606 0.42893 1.00000 0.02721 0.03213 0.03565 0.00614 0.00635 0.00576 0.03148 0.00888 0.00058 0.00090 0.00019 0.00000 0.00229 0.00280 0.00252 0.00217 0.00188 0.00213 0.00107 H24 1.51456 0.42278 0.42041 1.00000 0.03778 0.00000 0.00000 C25 1.26725 0.31303 0.42055 1.00000 0.03921 0.02692 0.03309 0.00012 0.00242 0.00038 0.03335 0.00896 0.00062 0.00090 0.00019 0.00000 0.00265 0.00250 0.00238 0.00220 0.00196 0.00228 0.00105 H25 1.26385 0.15857 0.40544 1.00000 0.04002 0.00000 0.00000 N21 1.13440 0.43212 0.43794 1.00000 0.02517 0.04471 0.03141 0.00494 0.00069 -0.00890 0.03410 0.00720 0.00048 0.00080 0.00015 0.00000 0.00202 0.00262 0.00203 0.00200 0.00157 0.00200 0.00095 H21 1.02957 0.37822 0.43655 1.00000 0.08302 0.00000 0.02329 N23 1.35235 0.65792 0.45193 1.00000 0.02337 0.03271 0.03240 0.00066 -0.00112 -0.00316 0.03000 0.00716 0.00047 0.00074 0.00015 0.00000 0.00191 0.00238 0.00205 0.00176 0.00152 0.00175 0.00090 H23 1.41819 0.78013 0.46174 1.00000 0.10126 0.00000 0.02785 Final Structure Factor Calculation for 06skc0030p21n in P2(1)/n Total number of l.s. parameters = 148 Maximum vector length = 511 Memory required = 1989 / 24017 wR2 = 0.1697 before cycle 5 for 2459 data and 0 / 148 parameters GooF = S = 1.195; Restrained GooF = 1.195 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0126 * P )^2 + 3.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0889 for 1842 Fo > 4sig(Fo) and 0.1235 for all 2459 data wR2 = 0.1697, GooF = S = 1.195, Restrained GooF = 1.195 for all data Occupancy sum of asymmetric unit = 16.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0429 0.0292 0.0173 C4 0.0462 0.0333 0.0204 C3 0.0374 0.0314 0.0206 C2 0.0304 0.0275 0.0186 C1 0.0348 0.0318 0.0239 C6 0.0355 0.0261 0.0235 C5 0.0413 0.0330 0.0320 C7 0.0358 0.0299 0.0162 O1A 0.0345 0.0288 0.0200 O1B 0.0358 0.0250 0.0238 O1C 0.0283 0.0258 0.0187 S1 0.0440 0.0277 0.0215 C22 0.0414 0.0298 0.0233 C24 0.0408 0.0324 0.0269 C25 0.0508 0.0298 0.0217 N21 0.0369 0.0320 0.0211 N23 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.020 0.031 0.041 0.055 0.070 0.088 0.113 0.169 1.000 Number in group 253. 246. 262. 235. 241. 250. 233. 247. 247. 245. GooF 1.742 1.589 1.212 0.978 1.043 1.032 0.916 1.020 0.958 1.119 K 28.318 4.961 2.072 1.399 1.164 1.072 1.005 1.010 0.988 0.987 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.14 1.32 1.64 inf Number in group 251. 241. 247. 251. 241. 249. 243. 245. 243. 248. GooF 0.980 0.953 1.021 1.056 1.145 1.137 1.170 1.095 1.432 1.743 K 1.101 1.178 1.151 1.084 1.062 1.009 1.024 1.004 1.031 0.997 R1 0.311 0.239 0.201 0.200 0.146 0.112 0.100 0.070 0.078 0.061 Recommended weighting scheme: WGHT 0.0128 3.8590 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 4 0 166.54 0.28 6.39 0.003 1.42 1 3 0 254.74 0.00 6.22 0.000 1.84 -3 1 3 213.82 2.55 5.88 0.010 2.36 -2 3 3 179.82 1.00 5.20 0.007 1.69 -3 3 2 62.72 0.99 4.69 0.006 1.54 2 3 0 412.70 196.44 4.22 0.092 1.71 -4 5 3 82.13 4.88 4.21 0.014 0.98 -7 3 3 80.49 8.69 3.99 0.019 0.97 -1 4 1 61.93 3.07 3.69 0.011 1.40 -5 3 2 62.89 6.93 3.67 0.017 1.21 -7 1 5 346.39 199.64 3.64 0.092 1.10 -4 5 1 301.95 122.40 3.57 0.072 0.99 -2 4 4 54.74 0.00 3.56 0.000 1.32 -2 4 2 104.33 5.60 3.51 0.015 1.34 1 1 20 79.52 0.15 3.49 0.003 1.13 -3 2 1 79.02 0.83 3.42 0.006 1.93 2 1 2 119.68 40.26 3.41 0.041 3.02 -5 4 3 127.83 16.10 3.36 0.026 1.06 -3 4 1 232.82 107.20 3.35 0.068 1.25 4 3 0 57.88 0.48 3.32 0.005 1.36 -5 4 2 89.51 25.28 3.31 0.033 1.06 -2 2 2 92.88 5.07 3.25 0.015 2.30 -3 1 4 63.15 1.12 3.24 0.007 2.31 -1 2 1 90.20 8.80 3.24 0.019 2.67 -4 3 3 300.43 166.92 3.15 0.084 1.36 0 4 4 53.75 2.80 3.15 0.011 1.38 -4 3 1 94.86 7.80 3.14 0.018 1.37 -6 2 4 94.41 20.34 3.07 0.029 1.19 0 1 5 30.34 0.59 3.07 0.005 3.66 0 4 2 204.77 111.50 3.02 0.069 1.41 -1 1 8 41.67 7.84 2.99 0.018 2.61 -5 0 3 6293.77 5467.39 2.99 0.483 1.58 -5 4 5 175.09 86.77 2.99 0.061 1.05 1 1 3 335.99 216.31 2.93 0.096 3.84 1 0 5 94.77 39.20 2.91 0.041 3.84 4 5 0 157.87 66.45 2.91 0.053 0.98 -6 1 2 136.27 51.93 2.89 0.047 1.28 -4 1 3 40.14 2.39 2.89 0.010 1.86 -2 6 1 55.52 0.13 2.82 0.002 0.92 -1 6 2 59.75 0.25 2.81 0.003 0.94 1 2 2 351.15 229.51 2.81 0.099 2.58 -4 2 2 69.62 22.38 2.79 0.031 1.62 2 0 0 3567.64 3007.25 2.76 0.358 3.91 -1 3 2 255.39 93.06 2.74 0.063 1.83 0 0 6 16236.46 18143.36 2.72 0.880 3.98 2 2 0 154.86 40.95 2.62 0.042 2.30 -5 2 6 39.36 4.02 2.62 0.013 1.35 4 2 1 45.66 0.02 2.60 0.001 1.60 2 3 1 919.41 722.36 2.59 0.176 1.69 -6 4 2 51.66 11.06 2.59 0.022 0.97 Bond lengths and angles C4 - Distance Angles C5 1.3749 (0.0064) C3 1.3927 (0.0071) 117.83 (0.42) C7 1.5060 (0.0061) 120.84 (0.46) 121.29 (0.44) C4 - C5 C3 C3 - Distance Angles C4 1.3927 (0.0071) C2 1.3946 (0.0063) 121.14 (0.43) H3 0.9500 119.43 119.43 C3 - C4 C2 C2 - Distance Angles C1 1.3874 (0.0060) C3 1.3946 (0.0063) 120.15 (0.44) H2 0.9500 119.93 119.93 C2 - C1 C3 C1 - Distance Angles C2 1.3874 (0.0060) C6 1.4028 (0.0064) 118.86 (0.41) S1 1.7707 (0.0044) 120.33 (0.35) 120.71 (0.34) C1 - C2 C6 C6 - Distance Angles C5 1.3812 (0.0062) C1 1.4028 (0.0064) 119.64 (0.43) H6 0.9500 120.18 120.18 C6 - C5 C1 C5 - Distance Angles C4 1.3749 (0.0065) C6 1.3812 (0.0062) 122.36 (0.45) H5 0.9500 118.82 118.82 C5 - C4 C6 C7 - Distance Angles C4 1.5060 (0.0061) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C4 H7A H7B O1A - Distance Angles S1 1.4572 (0.0030) O1A - O1B - Distance Angles S1 1.4621 (0.0029) O1B - O1C - Distance Angles S1 1.4579 (0.0034) O1C - S1 - Distance Angles O1A 1.4572 (0.0030) O1C 1.4579 (0.0034) 113.14 (0.19) O1B 1.4621 (0.0029) 112.22 (0.18) 112.55 (0.19) C1 1.7707 (0.0044) 105.91 (0.19) 106.56 (0.20) 105.77 (0.19) S1 - O1A O1C O1B C22 - Distance Angles N23 1.3265 (0.0057) N21 1.3296 (0.0064) 107.11 (0.41) H22 0.9500 126.45 126.45 C22 - N23 N21 C24 - Distance Angles C25 1.3413 (0.0068) N23 1.3615 (0.0062) 107.07 (0.41) H24 0.9500 126.47 126.46 C24 - C25 N23 C25 - Distance Angles C24 1.3413 (0.0068) N21 1.3659 (0.0062) 106.83 (0.44) H25 0.9500 126.58 126.58 C25 - C24 N21 N21 - Distance Angles C22 1.3296 (0.0064) C25 1.3659 (0.0062) 109.40 (0.39) H21 0.8800 125.30 125.30 N21 - C22 C25 N23 - Distance Angles C22 1.3265 (0.0057) C24 1.3615 (0.0062) 109.58 (0.41) H23 0.8800 125.21 125.21 N23 - C22 C24 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.03 2.750(5) 139.0 N21-H21...O1A_$1 0.88 2.57 3.076(5) 117.6 N21-H21...O1C_$2 0.88 2.01 2.818(5) 152.8 N23-H23...O1B_$3 0.88 2.44 2.988(5) 120.6 N23-H23...O1B_$4 FMAP and GRID set by program FMAP 2 3 29 GRID -0.962 -2 -2 0.962 2 2 R1 = 0.1223 for 2459 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.53 at 0.7762 0.4370 0.1222 [ 0.86 A from C1 ] Deepest hole -0.48 at 0.6561 0.3555 0.0805 [ 0.84 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 1917 / 15471 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7762 0.4370 0.1222 1.00000 0.05 0.53 0.86 C1 1.03 S1 1.80 O1C 1.89 C2 Q2 1 0.7346 0.4191 0.0326 1.00000 0.05 0.40 1.12 S1 1.18 O1B 1.68 O1A 1.85 O1C Q3 1 0.9195 0.6871 0.2509 1.00000 0.05 0.35 0.59 C4 0.98 C5 1.61 H5 1.73 C3 Q4 1 1.2805 0.3022 0.4688 1.00000 0.05 0.31 1.16 C25 1.48 N21 1.71 C24 1.72 H25 Q5 1 0.7163 0.1099 0.0499 1.00000 0.05 0.31 0.86 O1C 1.94 S1 2.39 H24 2.41 H21 Q6 1 1.0431 0.7656 0.2583 1.00000 0.05 0.30 0.69 C4 1.29 C7 1.51 C5 1.54 H7A Q7 1 0.7322 0.1673 0.1274 1.00000 0.05 0.30 1.08 O1C 1.89 S1 1.98 H6 2.05 H7C Q8 1 1.4090 0.0852 0.3759 1.00000 0.05 0.30 1.49 H25 2.11 C25 2.14 C2 2.18 C1 Q9 1 0.7842 0.1140 0.1034 1.00000 0.05 0.29 0.77 O1C 1.88 S1 2.05 H6 2.08 H24 Q10 1 1.0259 0.5585 0.2522 1.00000 0.05 0.28 0.66 C4 0.79 C3 1.38 H3 1.78 C7 Shortest distances between peaks (including symmetry equivalents) 7 9 0.82 3 6 1.07 3 10 1.11 6 10 1.19 5 9 1.32 1 7 1.58 2 5 1.82 5 7 1.88 1 9 1.90 2 4 2.06 1 2 2.14 4 5 2.15 2 9 2.42 1 5 2.55 1 8 2.62 2 7 2.70 4 8 2.87 Time profile in seconds ----------------------- 0.04: 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 0.01: Analyse other restraints etc. 0.98: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.46: Structure factors and derivatives 0.52: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.01: Other dependent quantities, CIF, tables 0.07: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0030p21n finished at 16:13:06 Total CPU time: 2.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++