+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0018p21c started at 16:24:38 on 07-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0018p21c in P2(1)/c CELL 0.71073 13.7305 5.8676 15.4181 90.000 115.604 90.000 ZERR 4.00 0.0021 0.0006 0.0024 0.000 0.006 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S UNIT 36 60 4 16 4 V = 1120.18 F(000) = 496.0 Mu = 0.28 mm-1 Cell Wt = 933.12 Rho = 1.383 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB N24 O1B HTAB N24 S1 EQIV_$1 x, y-1, z HTAB N24 O1C_$1 HTAB N24 S1_$1 EQIV_$2 -x, y-1/2, -z+1/2 HTAB N24 O21_$2 EQIV_$3 -x, -y+1, -z HTAB O21 O1A_$3 FMAP 2 PLAN 10 SIZE 0.01 0.05 0.08 ACTA BOND $H WGHT 0.03050 2.90530 L.S. 4 TEMP -153.00 FVAR 0.48348 MOLE 1 C4 1 0.540279 0.408471 0.119423 11.00000 0.02941 0.03296 = 0.01992 0.01087 0.01003 0.00940 C3 1 0.519091 0.612784 0.153315 11.00000 0.03266 0.03146 = 0.02506 0.00316 0.00965 -0.00428 AFIX 43 H3 2 0.573641 0.726420 0.176975 11.00000 -1.20000 AFIX 0 C2 1 0.419634 0.653653 0.153192 11.00000 0.03132 0.02323 = 0.02717 -0.00189 0.01002 0.00150 AFIX 43 H2 2 0.406226 0.794152 0.176695 11.00000 -1.20000 AFIX 0 C1 1 0.340165 0.489019 0.118718 11.00000 0.03037 0.02118 = 0.02073 0.00240 0.01405 0.00209 C6 1 0.359270 0.282256 0.085265 11.00000 0.03881 0.01714 = 0.03473 0.00218 0.01919 -0.00076 AFIX 43 H6 2 0.304635 0.168759 0.061857 11.00000 -1.20000 AFIX 0 C5 1 0.459199 0.244423 0.086615 11.00000 0.04299 0.02459 = 0.03444 0.00465 0.02238 0.01224 AFIX 43 H5 2 0.472951 0.102335 0.064511 11.00000 -1.20000 AFIX 0 C7 1 0.647596 0.364139 0.118416 11.00000 0.02666 0.06056 = 0.03188 0.00987 0.00890 0.01146 AFIX 137 H7A 2 0.636279 0.319804 0.053458 11.00000 -1.50000 H7B 2 0.684827 0.240947 0.163535 11.00000 -1.50000 H7C 2 0.691656 0.502761 0.137600 11.00000 -1.50000 AFIX 0 O1A 4 0.133779 0.418232 0.032955 11.00000 0.03045 0.02537 = 0.02973 -0.00223 0.01072 -0.00098 O1B 4 0.213634 0.458047 0.205817 11.00000 0.03878 0.03169 = 0.02698 -0.00271 0.01713 -0.00657 O1C 4 0.197017 0.788834 0.106654 11.00000 0.03307 0.02062 = 0.03691 0.00071 0.01649 0.00454 S1 5 0.211407 0.542585 0.115880 11.00000 0.02761 0.01950 = 0.02598 -0.00074 0.01272 0.00019 MOLE 2 C23 1 -0.021568 0.049875 0.107152 11.00000 0.03262 0.02503 = 0.02755 -0.00064 0.01374 -0.00076 AFIX 23 H23A 2 -0.042665 -0.112329 0.093992 11.00000 -1.20000 H23B 2 -0.024001 0.118049 0.047513 11.00000 -1.20000 AFIX 0 C22 1 -0.100737 0.171796 0.134732 11.00000 0.03026 0.02810 = 0.02445 0.00084 0.00933 -0.00054 AFIX 23 H22A 2 -0.174828 0.149820 0.083579 11.00000 -1.20000 H22B 2 -0.097569 0.105096 0.194876 11.00000 -1.20000 AFIX 0 N24 3 0.090555 0.064968 0.184839 11.00000 0.03533 0.02170 = 0.02834 0.00194 0.01731 0.00439 AFIX 137 H24A 2 0.115042 0.210493 0.188816 11.00000 -1.50000 H24B 2 0.134259 -0.030735 0.171242 11.00000 -1.50000 H24C 2 0.090862 0.024366 0.241920 11.00000 -1.50000 AFIX 0 O21 4 -0.077767 0.408425 0.148331 11.00000 0.04281 0.02203 = 0.02787 -0.00145 0.01880 0.00248 H21 2 -0.083382 0.472776 0.101789 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for 06skc0018p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C4 - C3 C5 C7 C3 - C2 C4 C2 - C1 C3 C1 - C2 C6 S1 C6 - C5 C1 C5 - C6 C4 C7 - C4 O1A - S1 O1B - S1 O1C - S1 S1 - O1C O1A O1B C1 C23 - N24 C22 C22 - O21 C23 N24 - C23 O21 - C22 Operators for generating equivalent atoms: $1 x, y-1, z $2 -x, y-1/2, -z+1/2 $3 -x, -y+1, -z h k l Fo^2 Sigma Why rejected 0 0 13 46.65 11.42 observed but should be systematically absent 19254 Reflections read, of which 988 rejected -17 =< h =< 17, -7 =< k =< 7, -19 =< l =< 20, Max. 2-theta = 54.97 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 5 2 4 7.82 2.01 11 12.49 0 5 7 54.41 6.71 4 86.63 -11 3 9 34.08 3.53 7 23.80 -10 4 11 43.35 4.07 5 20.84 -12 1 13 136.47 5.99 4 33.45 5 Inconsistent equivalents 2567 Unique reflections, of which 0 suppressed R(int) = 0.1326 R(sigma) = 0.0960 Friedel opposites merged Maximum memory for data reduction = 1840 / 25986 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 = 2251 / 178412 wR2 = 0.1711 before cycle 1 for 2567 data and 141 / 141 parameters GooF = S = 1.176; Restrained GooF = 1.176 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0305 * P )^2 + 2.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48348 0.00156 -0.002 OSF Mean shift/esd = 0.001 Maximum = -0.006 for U22 S1 Max. shift = 0.000 A for H24B Max. dU = 0.000 for C6 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2251 / 178412 wR2 = 0.1711 before cycle 2 for 2567 data and 141 / 141 parameters GooF = S = 1.176; Restrained GooF = 1.176 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0305 * P )^2 + 2.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48348 0.00156 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for U22 S1 Max. shift = 0.000 A for H7C Max. dU = 0.000 for C6 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2251 / 178412 wR2 = 0.1711 before cycle 3 for 2567 data and 141 / 141 parameters GooF = S = 1.176; Restrained GooF = 1.176 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0305 * P )^2 + 2.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48348 0.00156 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U11 S1 Max. shift = 0.000 A for H21 Max. dU = 0.000 for C6 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2251 / 178412 wR2 = 0.1711 before cycle 4 for 2567 data and 141 / 141 parameters GooF = S = 1.176; Restrained GooF = 1.176 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0305 * P )^2 + 2.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48348 0.00156 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H21 Max. dU = 0.000 for C7 Largest correlation matrix elements 0.581 U13 C5 / U11 C5 0.553 U13 C6 / U11 C6 0.533 U13 C23 / U11 C23 0.575 U13 O21 / U33 O21 0.553 U13 O1B / U33 O1B 0.531 U13 C23 / U33 C23 0.569 U13 S1 / U11 S1 0.552 U13 O1B / U11 O1B 0.525 U13 C4 / U11 C4 0.568 U13 C6 / U33 C6 0.549 U13 O1C / U11 O1C 0.511 U13 C2 / U11 C2 0.567 U13 C5 / U33 C5 0.548 U13 C1 / U11 C1 0.507 U13 O1A / U33 O1A 0.566 U13 N24 / U11 N24 0.545 U13 N24 / U33 N24 0.505 U13 O1A / U11 O1A 0.561 U13 O21 / U11 O21 0.544 U13 S1 / U33 S1 0.501 U13 C3 / U11 C3 0.556 U13 C1 / U33 C1 0.540 U13 O1C / U33 O1C Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.5736 0.7264 0.1770 43 0.950 0.000 C3 C2 C4 H2 0.4062 0.7942 0.1767 43 0.950 0.000 C2 C1 C3 H6 0.3046 0.1688 0.0619 43 0.950 0.000 C6 C5 C1 H5 0.4730 0.1023 0.0645 43 0.950 0.000 C5 C6 C4 H7A 0.6363 0.3198 0.0535 137 0.980 0.000 C7 C4 H7A H7B 0.6848 0.2409 0.1635 137 0.980 0.000 C7 C4 H7A H7C 0.6917 0.5028 0.1376 137 0.980 0.000 C7 C4 H7A H23A -0.0427 -0.1123 0.0940 23 0.990 0.000 C23 N24 C22 H23B -0.0240 0.1180 0.0475 23 0.990 0.000 C23 N24 C22 H22A -0.1748 0.1498 0.0836 23 0.990 0.000 C22 O21 C23 H22B -0.0976 0.1051 0.1949 23 0.990 0.000 C22 O21 C23 H24A 0.1150 0.2105 0.1888 137 0.910 0.000 N24 C23 H24A H24B 0.1343 -0.0307 0.1712 137 0.910 0.000 N24 C23 H24A H24C 0.0909 0.0244 0.2419 137 0.910 0.000 N24 C23 H24A 06skc0018p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C4 0.54028 0.40847 0.11942 1.00000 0.02941 0.03296 0.01992 0.01087 0.01003 0.00940 0.02765 0.00961 0.00035 0.00077 0.00030 0.00000 0.00241 0.00280 0.00219 0.00192 0.00195 0.00200 0.00106 C3 0.51909 0.61278 0.15332 1.00000 0.03266 0.03146 0.02506 0.00316 0.00965 -0.00428 0.03073 0.00970 0.00037 0.00079 0.00032 0.00000 0.00259 0.00272 0.00242 0.00198 0.00209 0.00201 0.00109 H3 0.57364 0.72642 0.17697 1.00000 0.03687 0.00000 0.00000 C2 0.41963 0.65365 0.15319 1.00000 0.03132 0.02323 0.02717 -0.00189 0.01002 0.00150 0.02817 0.00917 0.00034 0.00077 0.00031 0.00000 0.00250 0.00240 0.00244 0.00196 0.00210 0.00197 0.00103 H2 0.40623 0.79415 0.17670 1.00000 0.03381 0.00000 0.00000 C1 0.34016 0.48902 0.11872 1.00000 0.03037 0.02118 0.02073 0.00240 0.01405 0.00209 0.02303 0.00879 0.00033 0.00069 0.00028 0.00000 0.00228 0.00243 0.00208 0.00180 0.00185 0.00181 0.00095 C6 0.35927 0.28226 0.08527 1.00000 0.03881 0.01714 0.03473 0.00218 0.01919 -0.00076 0.02906 0.00998 0.00038 0.00073 0.00033 0.00000 0.00268 0.00235 0.00265 0.00197 0.00228 0.00194 0.00106 H6 0.30463 0.16876 0.06186 1.00000 0.03487 0.00000 0.00000 C5 0.45920 0.24442 0.08662 1.00000 0.04299 0.02459 0.03444 0.00465 0.02238 0.01224 0.03201 0.01043 0.00039 0.00078 0.00033 0.00000 0.00285 0.00250 0.00276 0.00210 0.00237 0.00214 0.00112 H5 0.47295 0.10234 0.06451 1.00000 0.03841 0.00000 0.00000 C7 0.64760 0.36414 0.11842 1.00000 0.02666 0.06056 0.03188 0.00987 0.00890 0.01146 0.04103 0.01094 0.00037 0.00095 0.00035 0.00000 0.00250 0.00364 0.00277 0.00249 0.00221 0.00239 0.00132 H7A 0.63628 0.31980 0.05346 1.00000 0.06154 0.00000 0.00000 H7B 0.68483 0.24095 0.16353 1.00000 0.06154 0.00000 0.00000 H7C 0.69166 0.50276 0.13760 1.00000 0.06154 0.00000 0.00000 O1A 0.13378 0.41823 0.03296 1.00000 0.03045 0.02537 0.02973 -0.00223 0.01072 -0.00098 0.02933 0.00604 0.00023 0.00049 0.00021 0.00000 0.00167 0.00176 0.00170 0.00137 0.00142 0.00133 0.00074 O1B 0.21363 0.45805 0.20582 1.00000 0.03878 0.03169 0.02698 -0.00271 0.01713 -0.00657 0.03145 0.00615 0.00024 0.00053 0.00020 0.00000 0.00179 0.00176 0.00165 0.00145 0.00146 0.00149 0.00075 O1C 0.19702 0.78883 0.10665 1.00000 0.03307 0.02062 0.03691 0.00071 0.01649 0.00454 0.02972 0.00639 0.00024 0.00048 0.00022 0.00000 0.00174 0.00164 0.00184 0.00142 0.00151 0.00135 0.00075 S1 0.21141 0.54259 0.11588 1.00000 0.02761 0.01950 0.02598 -0.00074 0.01272 0.00019 0.02396 0.00229 0.00009 0.00018 0.00008 0.00000 0.00057 0.00053 0.00056 0.00049 0.00046 0.00048 0.00029 C23 -0.02157 0.04987 0.10715 1.00000 0.03262 0.02503 0.02755 -0.00064 0.01374 -0.00076 0.02814 0.00910 0.00034 0.00079 0.00030 0.00000 0.00241 0.00233 0.00232 0.00205 0.00201 0.00208 0.00099 H23A -0.04267 -0.11233 0.09399 1.00000 0.03377 0.00000 0.00000 H23B -0.02400 0.11805 0.04751 1.00000 0.03377 0.00000 0.00000 C22 -0.10074 0.17180 0.13473 1.00000 0.03026 0.02810 0.02445 0.00084 0.00933 -0.00054 0.02849 0.00943 0.00036 0.00075 0.00032 0.00000 0.00239 0.00256 0.00234 0.00198 0.00200 0.00201 0.00103 H22A -0.17483 0.14982 0.08358 1.00000 0.03418 0.00000 0.00000 H22B -0.09757 0.10510 0.19488 1.00000 0.03418 0.00000 0.00000 N24 0.09056 0.06497 0.18484 1.00000 0.03533 0.02169 0.02834 0.00194 0.01731 0.00439 0.02720 0.00744 0.00028 0.00062 0.00024 0.00000 0.00209 0.00197 0.00198 0.00164 0.00174 0.00168 0.00085 H24A 0.11504 0.21049 0.18882 1.00000 0.04079 0.00000 0.00000 H24B 0.13426 -0.03073 0.17124 1.00000 0.04079 0.00000 0.00000 H24C 0.09086 0.02437 0.24192 1.00000 0.04079 0.00000 0.00000 O21 -0.07777 0.40843 0.14833 1.00000 0.04281 0.02203 0.02787 -0.00145 0.01880 0.00248 0.02965 0.00669 0.00026 0.00051 0.00022 0.00000 0.00193 0.00181 0.00172 0.00133 0.00163 0.00140 0.00078 H21 -0.08338 0.47278 0.10179 1.00000 0.04448 0.10961 0.00413 0.00912 0.00370 0.00000 0.00000 Final Structure Factor Calculation for 06skc0018p21c in P2(1)/c Total number of l.s. parameters = 141 Maximum vector length = 511 Memory required = 2110 / 24017 wR2 = 0.1711 before cycle 5 for 2567 data and 0 / 141 parameters GooF = S = 1.176; Restrained GooF = 1.176 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0305 * P )^2 + 2.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1002 for 1818 Fo > 4sig(Fo) and 0.1504 for all 2567 data wR2 = 0.1711, GooF = S = 1.176, Restrained GooF = 1.176 for all data Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 15.00 for hydrogen atoms Principal mean square atomic displacements U 0.0416 0.0277 0.0137 C4 0.0407 0.0279 0.0236 C3 0.0353 0.0270 0.0222 C2 0.0310 0.0212 0.0169 C1 0.0397 0.0310 0.0165 C6 0.0497 0.0285 0.0179 C5 0.0647 0.0366 0.0217 C7 0.0343 0.0294 0.0243 O1A 0.0427 0.0278 0.0238 O1B 0.0371 0.0332 0.0189 O1C 0.0279 0.0247 0.0193 S1 0.0327 0.0268 0.0249 C23 0.0334 0.0280 0.0241 C22 0.0370 0.0243 0.0203 N24 0.0431 0.0260 0.0199 O21 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 0.033 0.043 0.054 0.068 0.089 0.127 1.000 Number in group 283. 243. 274. 244. 259. 242. 258. 250. 255. 259. GooF 1.469 1.469 1.319 1.131 1.083 0.933 1.078 0.990 0.966 1.130 K 35.278 5.372 2.601 1.583 1.309 1.094 1.065 1.019 0.972 1.000 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 261. 254. 259. 256. 268. 242. 263. 250. 257. 257. GooF 1.181 1.337 1.149 1.197 1.236 1.210 1.052 1.131 0.993 1.242 K 1.390 1.447 1.261 1.329 1.095 1.023 0.992 0.999 1.010 1.011 R1 0.447 0.349 0.244 0.252 0.211 0.141 0.092 0.072 0.055 0.041 Recommended weighting scheme: WGHT 0.0305 2.9053 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) -6 3 6 45.09 0.85 3.57 0.005 1.41 -9 5 13 187.51 5.79 3.37 0.012 0.81 5 0 10 606.81 911.49 3.36 0.152 1.04 1 0 4 75.50 15.68 3.28 0.020 3.02 -14 4 8 271.12 68.34 3.24 0.042 0.81 -13 0 10 463.94 698.62 3.16 0.133 1.02 -10 2 4 41.38 2.31 3.07 0.008 1.24 -16 1 1 126.71 4.03 2.97 0.010 0.78 -6 5 1 44.79 6.05 2.95 0.012 1.03 -12 2 1 83.28 11.01 2.94 0.017 1.00 -6 0 4 1188.27 948.54 2.90 0.155 2.25 3 0 6 4534.88 3871.45 2.89 0.314 1.73 8 1 4 53.52 5.92 2.88 0.012 1.20 -13 4 11 95.81 4.96 2.86 0.011 0.82 -15 2 4 126.36 37.95 2.81 0.031 0.86 2 4 13 103.33 1.30 2.81 0.006 0.82 3 2 14 105.72 4.86 2.81 0.011 0.85 -5 2 5 31.93 1.02 2.79 0.005 1.88 -2 1 3 2800.08 3258.74 2.73 0.288 3.74 0 1 10 40.19 0.04 2.71 0.001 1.35 4 0 8 55.12 0.04 2.70 0.001 1.30 -1 5 9 77.52 5.65 2.69 0.012 0.95 -6 4 13 79.25 14.17 2.65 0.019 0.92 -4 1 7 357.30 258.23 2.65 0.081 2.01 6 0 8 483.66 697.91 2.65 0.133 1.11 -2 0 2 29.44 1.16 2.63 0.005 6.12 -3 1 3 100.77 51.77 2.63 0.036 3.35 -12 4 2 94.16 15.40 2.63 0.020 0.88 12 1 2 101.75 0.07 2.62 0.001 0.95 -1 1 5 885.40 719.26 2.57 0.135 2.67 -3 3 3 34.06 5.40 2.56 0.012 1.76 -5 6 6 305.39 58.11 2.55 0.038 0.90 -7 3 17 198.68 83.27 2.54 0.046 0.82 3 4 0 28.08 0.16 2.50 0.002 1.38 -5 4 2 35.48 3.45 2.50 0.009 1.29 7 2 9 56.32 5.22 2.49 0.012 0.92 -12 4 10 58.32 0.14 2.48 0.002 0.87 1 1 3 444.90 339.83 2.48 0.093 3.21 -2 5 7 41.60 5.76 2.48 0.012 1.03 3 1 14 173.82 68.23 2.46 0.042 0.87 -10 1 16 122.25 29.05 2.46 0.027 0.91 -6 2 11 37.69 5.84 2.44 0.012 1.24 0 3 3 249.59 173.00 2.44 0.066 1.80 0 1 5 833.34 1007.12 2.43 0.160 2.51 3 4 12 163.46 48.05 2.42 0.035 0.83 9 2 9 16.89 76.40 2.41 0.044 0.82 4 4 1 21.61 0.55 2.40 0.004 1.30 -1 3 15 132.73 213.95 2.39 0.074 0.86 13 2 0 93.22 22.97 2.39 0.024 0.91 1 3 5 21.24 0.59 2.39 0.004 1.54 Bond lengths and angles C4 - Distance Angles C3 1.3879 (0.0062) C5 1.3911 (0.0065) 118.01 (0.41) C7 1.5030 (0.0061) 121.29 (0.43) 120.70 (0.42) C4 - C3 C5 C3 - Distance Angles C2 1.3857 (0.0062) C4 1.3879 (0.0062) 121.05 (0.43) H3 0.9500 119.48 119.48 C3 - C2 C4 C2 - Distance Angles C1 1.3802 (0.0058) C3 1.3857 (0.0062) 119.61 (0.42) H2 0.9500 120.20 120.20 C2 - C1 C3 C1 - Distance Angles C2 1.3802 (0.0058) C6 1.3870 (0.0058) 120.69 (0.40) S1 1.7774 (0.0042) 119.87 (0.32) 119.44 (0.33) C1 - C2 C6 C6 - Distance Angles C5 1.3812 (0.0063) C1 1.3870 (0.0058) 118.77 (0.42) H6 0.9500 120.61 120.61 C6 - C5 C1 C5 - Distance Angles C6 1.3812 (0.0063) C4 1.3911 (0.0065) 121.87 (0.42) H5 0.9500 119.07 119.07 C5 - C6 C4 C7 - Distance Angles C4 1.5030 (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 1.4578 (0.0030) O1A - O1B - Distance Angles S1 1.4605 (0.0030) O1B - O1C - Distance Angles S1 1.4569 (0.0030) O1C - S1 - Distance Angles O1C 1.4569 (0.0030) O1A 1.4578 (0.0030) 113.19 (0.18) O1B 1.4605 (0.0030) 112.07 (0.19) 111.72 (0.18) C1 1.7774 (0.0042) 105.62 (0.19) 105.99 (0.19) 107.70 (0.19) S1 - O1C O1A O1B C23 - Distance Angles N24 1.4896 (0.0053) C22 1.5079 (0.0060) 111.44 (0.35) H23A 0.9900 109.34 109.34 H23B 0.9900 109.34 109.34 107.98 C23 - N24 C22 H23A C22 - Distance Angles O21 1.4192 (0.0053) C23 1.5079 (0.0060) 111.38 (0.37) H22A 0.9900 109.35 109.35 H22B 0.9900 109.35 109.35 107.99 C22 - O21 C23 H22A N24 - Distance Angles C23 1.4896 (0.0053) H24A 0.9100 109.47 H24B 0.9100 109.47 109.47 H24C 0.9100 109.47 109.47 109.47 N24 - C23 H24A H24B O21 - Distance Angles C22 1.4192 (0.0053) H21 0.7846 (0.0513) 114.08 (3.95) O21 - C22 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.92 2.794(5) 159.2 N24-H24A...O1B 0.91 2.85 3.642(4) 146.8 N24-H24A...S1 0.91 1.90 2.782(5) 163.7 N24-H24B...O1C_$1 0.91 2.98 3.848(4) 159.2 N24-H24B...S1_$1 0.91 1.90 2.807(5) 172.2 N24-H24C...O21_$2 0.78(5) 1.99(5) 2.753(4) 164(5) O21-H21...O1A_$3 FMAP and GRID set by program FMAP 2 2 33 GRID -3.333 -1 -1 3.333 1 1 R1 = 0.1488 for 2567 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.36 at 0.1381 0.5406 0.0705 [ 0.91 A from O1A ] Deepest hole -0.41 at 0.0999 0.5029 0.0828 [ 1.17 A from O1A ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 2592 / 41649 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1381 0.5406 0.0705 1.00000 0.05 0.36 0.91 O1A 0.95 S1 1.64 O1C 1.95 O1B Q2 1 0.1328 0.2684 0.0199 1.00000 0.05 0.31 0.90 O1A 1.89 H23A 2.14 S1 2.24 H6 Q3 1 0.3720 0.5643 0.1616 1.00000 0.05 0.30 0.76 C1 0.89 C2 1.41 H2 1.99 C6 Q4 1 -0.0173 0.4984 0.1891 1.00000 0.05 0.29 0.95 O21 1.27 H21 1.76 H24C 1.91 H22B Q5 1 0.2885 0.5212 0.1117 1.00000 0.05 0.29 0.70 C1 1.10 S1 1.81 C2 1.85 C6 Q6 1 0.2858 0.5407 0.2129 1.00000 0.05 0.29 1.07 O1B 1.40 S1 1.92 C1 2.12 H7B Q7 1 0.5356 0.5090 0.1804 1.00000 0.05 0.28 0.72 C3 1.13 C4 1.39 H3 1.69 C2 Q8 1 0.2060 0.4355 0.1626 1.00000 0.05 0.28 0.64 O1B 0.98 S1 1.81 O1A 1.98 H24A Q9 1 0.2127 0.9022 0.1431 1.00000 0.05 0.28 0.84 O1C 1.38 H24B 2.15 S1 2.25 N24 Q10 1 0.0816 0.2657 0.0304 1.00000 0.05 0.27 1.14 O1A 1.80 H23B 1.97 H23A 2.31 H24A Shortest distances between peaks (including symmetry equivalents) 2 10 0.79 3 5 1.10 6 8 1.20 1 8 1.46 5 6 1.58 3 6 1.69 5 8 1.71 1 2 1.76 1 10 1.78 1 5 1.88 3 7 2.16 2 8 2.21 8 10 2.25 1 6 2.25 6 9 2.39 3 8 2.41 1 9 2.41 2 5 2.48 5 9 2.60 8 9 2.76 2 9 2.76 9 10 2.85 3 9 2.87 1 3 2.90 1 10 2.96 5 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. 0.89: 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 0.45: Structure factors and derivatives 0.38: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0018p21c finished at 16:24:40 Total CPU time: 2.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++