+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0022p21c started at 15:44:17 on 07-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0022p21c in P2(1)/c CELL 0.71073 13.7465 8.6976 10.3290 90.000 97.361 90.000 ZERR 4.00 0.0012 0.0008 0.0006 0.000 0.005 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S UNIT 48 60 4 16 4 V = 1224.77 F(000) = 568.0 Mu = 0.27 mm-1 Cell Wt = 1077.24 Rho = 1.461 MERG 2 OMIT -3.00 55.00 OMIT 2 0 10 SHEL 7 0.77 EQIV_$1 x+1, -y+1/2, z+1/2 HTAB N24 O2A_$1 HTAB N24 S2_$1 EQIV_$2 -x+2, y+1/2, -z+1/2 HTAB N24 O2B_$2 HTAB N24 S2_$2 HTAB O21 O2A_$2 HTAB O21 S2_$2 EQIV_$3 x+1, y, z HTAB N24 O2C_$3 HTAB N24 S2_$3 FMAP 2 PLAN 10 SIZE 0.01 0.04 0.06 ACTA BOND $H WGHT 0.03480 0.95720 L.S. 8 TEMP -153.00 FVAR 0.80319 MOLE 1 C1 1 0.861744 0.075684 0.153799 11.00000 0.02365 0.01322 = 0.01253 -0.00205 0.00063 -0.00271 AFIX 43 H1 2 0.846272 -0.003834 0.210817 11.00000 -1.20000 AFIX 0 C2 1 0.788260 0.162781 0.088739 11.00000 0.01645 0.01504 = 0.01230 -0.00395 0.00340 -0.00004 C3 1 0.808904 0.280014 0.000928 11.00000 0.02380 0.01677 = 0.01755 -0.00156 0.00376 0.00378 AFIX 43 H3 2 0.757169 0.338041 -0.045429 11.00000 -1.20000 AFIX 0 C4 1 0.904306 0.308546 -0.016222 11.00000 0.02638 0.01670 = 0.01575 0.00242 0.00422 0.00127 AFIX 43 H4 2 0.918119 0.387159 -0.075061 11.00000 -1.20000 AFIX 0 C5 1 0.982785 0.224205 0.051243 11.00000 0.02024 0.01645 = 0.01730 -0.00448 0.00358 -0.00061 C6 1 1.082087 0.254983 0.039224 11.00000 0.02479 0.02281 = 0.02227 -0.00334 0.00779 -0.00382 AFIX 43 H6 2 1.097705 0.334328 -0.017865 11.00000 -1.20000 AFIX 0 C7 1 1.156093 0.172954 0.108038 11.00000 0.01891 0.02859 = 0.02676 -0.00990 0.00398 -0.00334 AFIX 43 H7 2 1.222462 0.197815 0.100721 11.00000 -1.20000 AFIX 0 C8 1 1.134230 0.051274 0.190041 11.00000 0.02352 0.02287 = 0.02309 -0.00211 -0.00009 0.00333 AFIX 43 H8 2 1.185917 -0.007333 0.235864 11.00000 -1.20000 AFIX 0 C9 1 1.039003 0.017461 0.203764 11.00000 0.02312 0.02192 = 0.01700 0.00218 0.00177 0.00116 AFIX 43 H9 2 1.024945 -0.064719 0.259041 11.00000 -1.20000 AFIX 0 C10 1 0.961246 0.103664 0.136449 11.00000 0.02169 0.01546 = 0.01086 -0.00358 0.00119 -0.00086 O2A 4 0.618320 0.056764 -0.007221 11.00000 0.02327 0.02266 = 0.02138 -0.00131 -0.00416 -0.00215 O2B 4 0.665021 0.031034 0.225789 11.00000 0.02416 0.02396 = 0.02460 0.00487 0.00352 -0.00692 O2C 4 0.623494 0.282002 0.130193 11.00000 0.02215 0.01761 = 0.04153 -0.00041 0.01330 0.00171 S2 5 0.665154 0.130674 0.112685 11.00000 0.01674 0.01720 = 0.02065 0.00012 0.00262 -0.00031 MOLE 2 C22 1 1.357602 0.162604 0.426823 11.00000 0.02153 0.01828 = 0.02024 -0.00278 0.00086 -0.00207 AFIX 23 H22A 2 1.303496 0.221093 0.376845 11.00000 -1.20000 H22B 2 1.331545 0.061066 0.448712 11.00000 -1.20000 AFIX 0 C23 1 1.438923 0.139862 0.342987 11.00000 0.02428 0.01581 = 0.02121 0.00018 0.00216 0.00198 AFIX 23 H23A 2 1.491373 0.076004 0.390692 11.00000 -1.20000 H23B 2 1.412890 0.084703 0.262072 11.00000 -1.20000 AFIX 0 N24 3 1.480935 0.291222 0.308405 11.00000 0.01920 0.01855 = 0.01921 -0.00161 0.00302 0.00130 AFIX 137 H24A 2 1.518620 0.330434 0.379618 11.00000 -1.50000 H24B 2 1.431279 0.357733 0.281779 11.00000 -1.50000 H24C 2 1.518408 0.277385 0.242824 11.00000 -1.50000 AFIX 0 O21 4 1.390779 0.242764 0.543897 11.00000 0.02627 0.02180 = 0.01846 0.00055 0.00123 0.00102 AFIX 147 H21 2 1.389606 0.337792 0.529266 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0022p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - C2 C10 C2 - C1 C3 S2 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 C10 C6 - C7 C5 C7 - C6 C8 C8 - C9 C7 C9 - C8 C10 C10 - C9 C1 C5 O2A - S2 O2B - S2 O2C - S2 S2 - O2B O2C O2A C2 C22 - O21 C23 C23 - N24 C22 N24 - C23 O21 - C22 Operators for generating equivalent atoms: $1 x+1, -y+1/2, z+1/2 $2 -x+2, y+1/2, -z+1/2 $3 x+1, y, z h k l Fo^2 Sigma Why rejected 0 0 5 59.44 13.97 observed but should be systematically absent 15465 Reflections read, of which 565 rejected -17 =< h =< 17, -10 =< k =< 11, -12 =< l =< 13, 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) 11 5 0 76.45 28.76 3 147.91 -12 5 5 77.72 29.06 3 197.86 2 Inconsistent equivalents 2804 Unique reflections, of which 0 suppressed R(int) = 0.1299 R(sigma) = 0.1129 Friedel opposites merged Maximum memory for data reduction = 2102 / 27980 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 = 2570 / 206672 wR2 = 0.1261 before cycle 1 for 2804 data and 165 / 165 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80319 0.00185 0.002 OSF Mean shift/esd = 0.001 Maximum = -0.007 for U11 S2 Max. shift = 0.000 A for H24C Max. dU = 0.000 for C7 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2570 / 206672 wR2 = 0.1261 before cycle 2 for 2804 data and 165 / 165 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80320 0.00185 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.003 for U11 S2 Max. shift = 0.000 A for H24C Max. dU = 0.000 for C7 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2570 / 206672 wR2 = 0.1261 before cycle 3 for 2804 data and 165 / 165 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80319 0.00185 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U11 S2 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C23 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2570 / 206672 wR2 = 0.1261 before cycle 4 for 2804 data and 165 / 165 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80319 0.00185 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O21 Max. shift = 0.000 A for H21 Max. dU = 0.000 for C9 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2570 / 206672 wR2 = 0.1261 before cycle 5 for 2804 data and 165 / 165 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80319 0.00185 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x S2 Max. shift = 0.000 A for C6 Max. dU = 0.000 for O21 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2570 / 206672 wR2 = 0.1261 before cycle 6 for 2804 data and 165 / 165 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80319 0.00185 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x S2 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C2 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2570 / 206672 wR2 = 0.1261 before cycle 7 for 2804 data and 165 / 165 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80320 0.00185 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x S2 Max. shift = 0.000 A for C22 Max. dU = 0.000 for O2A Least-squares cycle 8 Maximum vector length = 511 Memory required = 2570 / 206672 wR2 = 0.1261 before cycle 8 for 2804 data and 165 / 165 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.80319 0.00185 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x S2 Max. shift = 0.000 A for C6 Max. dU = 0.000 for O21 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.8463 -0.0038 0.2108 43 0.950 0.000 C1 C2 C10 H3 0.7572 0.3380 -0.0454 43 0.950 0.000 C3 C4 C2 H4 0.9181 0.3872 -0.0751 43 0.950 0.000 C4 C3 C5 H6 1.0977 0.3343 -0.0179 43 0.950 0.000 C6 C7 C5 H7 1.2225 0.1978 0.1007 43 0.950 0.000 C7 C6 C8 H8 1.1859 -0.0073 0.2359 43 0.950 0.000 C8 C9 C7 H9 1.0249 -0.0647 0.2590 43 0.950 0.000 C9 C8 C10 H22A 1.3035 0.2211 0.3768 23 0.990 0.000 C22 O21 C23 H22B 1.3315 0.0611 0.4487 23 0.990 0.000 C22 O21 C23 H23A 1.4914 0.0760 0.3907 23 0.990 0.000 C23 N24 C22 H23B 1.4129 0.0847 0.2621 23 0.990 0.000 C23 N24 C22 H24A 1.5186 0.3304 0.3796 137 0.910 0.000 N24 C23 H24A H24B 1.4313 0.3577 0.2818 137 0.910 0.000 N24 C23 H24A H24C 1.5184 0.2774 0.2428 137 0.910 0.000 N24 C23 H24A H21 1.3896 0.3378 0.5293 147 0.840 0.000 O21 C22 H21 06skc0022p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.86174 0.07568 0.15380 1.00000 0.02365 0.01322 0.01253 -0.00205 0.00063 -0.00271 0.01661 0.00534 0.00023 0.00035 0.00028 0.00000 0.00186 0.00164 0.00151 0.00128 0.00128 0.00135 0.00070 H1 0.84627 -0.00383 0.21082 1.00000 0.01993 0.00000 0.00000 C2 0.78826 0.16278 0.08874 1.00000 0.01645 0.01504 0.01230 -0.00395 0.00340 -0.00004 0.01446 0.00530 0.00022 0.00034 0.00027 0.00000 0.00170 0.00169 0.00152 0.00126 0.00122 0.00132 0.00068 C3 0.80890 0.28001 0.00093 1.00000 0.02380 0.01677 0.01755 -0.00156 0.00376 0.00378 0.01928 0.00574 0.00024 0.00036 0.00029 0.00000 0.00194 0.00181 0.00161 0.00136 0.00133 0.00142 0.00073 H3 0.75717 0.33804 -0.04543 1.00000 0.02313 0.00000 0.00000 C4 0.90431 0.30855 -0.01622 1.00000 0.02638 0.01670 0.01575 0.00242 0.00422 0.00127 0.01948 0.00577 0.00024 0.00036 0.00029 0.00000 0.00199 0.00174 0.00161 0.00133 0.00136 0.00142 0.00073 H4 0.91812 0.38716 -0.07506 1.00000 0.02337 0.00000 0.00000 C5 0.98278 0.22421 0.05124 1.00000 0.02024 0.01645 0.01730 -0.00448 0.00358 -0.00061 0.01789 0.00551 0.00023 0.00036 0.00028 0.00000 0.00185 0.00177 0.00161 0.00132 0.00130 0.00137 0.00071 C6 1.08209 0.25498 0.03922 1.00000 0.02479 0.02281 0.02227 -0.00334 0.00779 -0.00382 0.02288 0.00581 0.00024 0.00039 0.00030 0.00000 0.00203 0.00187 0.00173 0.00149 0.00143 0.00156 0.00077 H6 1.09770 0.33433 -0.01787 1.00000 0.02745 0.00000 0.00000 C7 1.15609 0.17295 0.10804 1.00000 0.01891 0.02859 0.02676 -0.00990 0.00398 -0.00334 0.02466 0.00597 0.00026 0.00038 0.00031 0.00000 0.00189 0.00202 0.00181 0.00160 0.00142 0.00158 0.00079 H7 1.22246 0.19781 0.10072 1.00000 0.02959 0.00000 0.00000 C8 1.13423 0.05127 0.19004 1.00000 0.02352 0.02287 0.02309 -0.00211 -0.00009 0.00333 0.02343 0.00588 0.00025 0.00038 0.00031 0.00000 0.00203 0.00195 0.00178 0.00148 0.00141 0.00149 0.00078 H8 1.18592 -0.00733 0.23586 1.00000 0.02812 0.00000 0.00000 C9 1.03900 0.01746 0.20376 1.00000 0.02312 0.02192 0.01700 0.00218 0.00177 0.00116 0.02075 0.00577 0.00024 0.00039 0.00029 0.00000 0.00193 0.00188 0.00170 0.00137 0.00135 0.00148 0.00075 H9 1.02495 -0.06472 0.25904 1.00000 0.02490 0.00000 0.00000 C10 0.96125 0.10366 0.13645 1.00000 0.02169 0.01546 0.01086 -0.00358 0.00119 -0.00086 0.01608 0.00537 0.00023 0.00035 0.00027 0.00000 0.00180 0.00173 0.00149 0.00126 0.00124 0.00137 0.00069 O2A 0.61832 0.05676 -0.00722 1.00000 0.02327 0.02266 0.02138 -0.00131 -0.00416 -0.00215 0.02305 0.00388 0.00016 0.00025 0.00020 0.00000 0.00134 0.00132 0.00120 0.00096 0.00094 0.00101 0.00055 O2B 0.66502 0.03103 0.22579 1.00000 0.02416 0.02396 0.02460 0.00487 0.00352 -0.00692 0.02421 0.00400 0.00016 0.00025 0.00020 0.00000 0.00135 0.00136 0.00124 0.00101 0.00097 0.00104 0.00056 O2C 0.62349 0.28200 0.13019 1.00000 0.02215 0.01761 0.04153 -0.00041 0.01330 0.00171 0.02629 0.00420 0.00016 0.00025 0.00022 0.00000 0.00138 0.00131 0.00140 0.00104 0.00107 0.00100 0.00057 S2 0.66515 0.13067 0.11268 1.00000 0.01674 0.01720 0.02065 0.00012 0.00262 -0.00031 0.01818 0.00146 0.00006 0.00009 0.00007 0.00000 0.00043 0.00043 0.00042 0.00036 0.00030 0.00035 0.00021 C22 1.35760 0.16260 0.42682 1.00000 0.02153 0.01828 0.02024 -0.00278 0.00086 -0.00207 0.02018 0.00563 0.00024 0.00038 0.00029 0.00000 0.00187 0.00187 0.00167 0.00135 0.00133 0.00139 0.00075 H22A 1.30350 0.22109 0.37684 1.00000 0.02421 0.00000 0.00000 H22B 1.33155 0.06107 0.44871 1.00000 0.02421 0.00000 0.00000 C23 1.43892 0.13986 0.34299 1.00000 0.02428 0.01581 0.02121 0.00018 0.00216 0.00198 0.02050 0.00590 0.00024 0.00036 0.00030 0.00000 0.00188 0.00174 0.00167 0.00144 0.00136 0.00146 0.00073 H23A 1.49137 0.07600 0.39069 1.00000 0.02460 0.00000 0.00000 H23B 1.41289 0.08470 0.26207 1.00000 0.02460 0.00000 0.00000 N24 1.48093 0.29122 0.30840 1.00000 0.01920 0.01855 0.01921 -0.00161 0.00302 0.00130 0.01894 0.00465 0.00019 0.00029 0.00024 0.00000 0.00156 0.00152 0.00139 0.00111 0.00109 0.00115 0.00062 H24A 1.51862 0.33043 0.37962 1.00000 0.02841 0.00000 0.00000 H24B 1.43128 0.35773 0.28178 1.00000 0.02841 0.00000 0.00000 H24C 1.51841 0.27738 0.24282 1.00000 0.02841 0.00000 0.00000 O21 1.39078 0.24276 0.54390 1.00000 0.02627 0.02180 0.01846 0.00055 0.00123 0.00102 0.02232 0.00388 0.00017 0.00026 0.00019 0.00000 0.00136 0.00130 0.00114 0.00099 0.00093 0.00109 0.00054 H21 1.38961 0.33779 0.52927 1.00000 0.03348 0.00000 0.00000 Final Structure Factor Calculation for 06skc0022p21c in P2(1)/c Total number of l.s. parameters = 165 Maximum vector length = 511 Memory required = 2405 / 24017 wR2 = 0.1261 before cycle 9 for 2804 data and 0 / 165 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.96 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0661 for 1790 Fo > 4sig(Fo) and 0.1242 for all 2804 data wR2 = 0.1261, GooF = S = 1.043, Restrained GooF = 1.043 for all data Occupancy sum of asymmetric unit = 18.00 for non-hydrogen and 15.00 for hydrogen atoms Principal mean square atomic displacements U 0.0246 0.0148 0.0104 C1 0.0181 0.0162 0.0090 C2 0.0254 0.0186 0.0138 C3 0.0267 0.0181 0.0137 C4 0.0219 0.0195 0.0123 C5 0.0308 0.0200 0.0179 C6 0.0378 0.0191 0.0170 C7 0.0295 0.0210 0.0198 C8 0.0238 0.0223 0.0161 C9 0.0220 0.0174 0.0089 C10 0.0305 0.0233 0.0153 O2A 0.0330 0.0248 0.0149 O2B 0.0442 0.0192 0.0155 O2C 0.0207 0.0174 0.0165 S2 0.0231 0.0220 0.0154 C22 0.0250 0.0212 0.0154 C23 0.0208 0.0197 0.0163 N24 0.0270 0.0218 0.0182 O21 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.028 0.045 0.062 0.080 0.101 0.127 0.163 0.223 1.000 Number in group 292. 271. 286. 273. 283. 281. 280. 276. 282. 280. GooF 1.120 1.084 1.073 0.934 0.994 1.062 1.021 1.091 1.039 0.996 K 20.814 2.765 1.732 1.222 1.074 1.033 1.016 1.017 1.001 0.997 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.66 inf Number in group 283. 280. 287. 272. 284. 277. 279. 280. 283. 279. GooF 0.982 0.979 1.002 0.976 0.987 1.024 1.040 1.035 1.132 1.243 K 1.056 1.184 1.113 1.072 1.046 1.037 1.015 1.003 1.010 0.998 R1 0.363 0.287 0.234 0.186 0.142 0.120 0.074 0.060 0.060 0.035 Recommended weighting scheme: WGHT 0.0348 0.9572 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) 1 2 3 522.84 396.43 3.94 0.157 2.59 2 2 8 470.68 644.32 3.22 0.200 1.18 8 2 10 223.14 0.08 3.16 0.002 0.82 12 3 4 84.49 183.82 3.14 0.107 0.94 5 4 1 52.22 3.11 3.13 0.014 1.66 -5 2 1 618.24 750.86 3.11 0.216 2.31 2 4 12 139.62 3.80 3.11 0.015 0.78 -11 1 11 312.92 164.08 3.06 0.101 0.79 12 5 4 122.98 0.06 3.02 0.002 0.86 -2 3 6 28.48 4.14 2.95 0.016 1.47 9 1 1 51.63 1.19 2.95 0.009 1.45 -1 3 1 70.10 27.06 2.92 0.041 2.75 7 9 2 485.53 697.97 2.91 0.208 0.85 -3 4 8 89.96 15.09 2.89 0.031 1.10 -15 1 5 -40.26 46.00 2.89 0.054 0.87 6 1 0 2786.47 2439.66 2.87 0.390 2.20 10 8 3 181.28 5.81 2.85 0.019 0.81 4 7 3 200.82 282.70 2.82 0.133 1.09 10 1 7 284.60 390.13 2.81 0.156 0.93 -10 0 2 140.05 49.54 2.76 0.056 1.36 3 6 0 63.36 12.12 2.74 0.027 1.38 -9 4 4 417.12 322.32 2.73 0.142 1.17 -4 3 1 433.87 348.60 2.73 0.147 2.20 5 1 3 2634.62 2324.34 2.72 0.380 1.96 -15 0 6 369.81 560.56 2.69 0.187 0.85 -12 1 4 376.97 483.17 2.68 0.173 1.08 6 2 5 58.46 14.71 2.64 0.030 1.36 0 3 1 211.52 131.65 2.64 0.091 2.79 5 1 2 226.60 163.25 2.64 0.101 2.21 -3 1 6 46.68 25.13 2.63 0.040 1.64 5 3 3 41.40 6.51 2.61 0.020 1.65 -2 8 1 535.24 401.28 2.61 0.158 1.07 10 9 0 -7.29 131.71 2.60 0.091 0.79 2 5 3 357.99 274.57 2.59 0.131 1.49 4 7 1 76.59 18.61 2.58 0.034 1.15 9 7 3 78.13 2.30 2.57 0.012 0.91 4 2 3 182.10 128.13 2.56 0.089 2.01 -6 7 4 -27.86 27.53 2.54 0.041 1.03 -3 4 4 795.74 925.15 2.52 0.240 1.60 -5 3 4 36.90 9.21 2.52 0.024 1.65 -9 1 9 43.72 0.37 2.51 0.005 0.97 -4 6 1 154.36 91.09 2.51 0.075 1.33 -2 3 5 105.35 63.00 2.50 0.063 1.67 12 1 2 85.72 28.95 2.50 0.042 1.07 3 8 2 61.99 1.78 2.47 0.011 1.03 -12 4 8 232.34 328.91 2.47 0.143 0.84 1 2 8 42.27 89.53 2.47 0.075 1.21 4 6 10 212.39 0.12 2.47 0.003 0.79 -5 1 10 94.60 55.17 2.47 0.059 1.00 -7 3 1 226.76 156.90 2.46 0.099 1.62 Bond lengths and angles C1 - Distance Angles C2 1.3682 (0.0043) C10 1.4230 (0.0043) 120.30 (0.28) H1 0.9500 119.85 119.85 C1 - C2 C10 C2 - Distance Angles C1 1.3682 (0.0043) C3 1.4173 (0.0042) 121.12 (0.29) S2 1.7636 (0.0031) 120.32 (0.23) 118.56 (0.23) C2 - C1 C3 C3 - Distance Angles C4 1.3683 (0.0044) C2 1.4173 (0.0042) 119.15 (0.30) H3 0.9500 120.42 120.42 C3 - C4 C2 C4 - Distance Angles C3 1.3683 (0.0044) C5 1.4124 (0.0045) 121.74 (0.29) H4 0.9500 119.13 119.13 C4 - C3 C5 C5 - Distance Angles C6 1.4120 (0.0044) C4 1.4124 (0.0045) 122.96 (0.30) C10 1.4241 (0.0042) 118.28 (0.29) 118.76 (0.29) C5 - C6 C4 C6 - Distance Angles C7 1.3652 (0.0047) C5 1.4120 (0.0044) 121.29 (0.31) H6 0.9500 119.35 119.35 C6 - C7 C5 C7 - Distance Angles C6 1.3652 (0.0047) C8 1.4117 (0.0046) 120.16 (0.32) H7 0.9500 119.92 119.92 C7 - C6 C8 C8 - Distance Angles C9 1.3666 (0.0045) C7 1.4117 (0.0046) 120.26 (0.32) H8 0.9500 119.87 119.87 C8 - C9 C7 C9 - Distance Angles C8 1.3666 (0.0045) C10 1.4134 (0.0044) 120.59 (0.30) H9 0.9500 119.71 119.71 C9 - C8 C10 C10 - Distance Angles C9 1.4134 (0.0044) C1 1.4230 (0.0043) 121.73 (0.28) C5 1.4241 (0.0042) 119.37 (0.29) 118.88 (0.28) C10 - C9 C1 O2A - Distance Angles S2 1.4688 (0.0022) O2A - O2B - Distance Angles S2 1.4548 (0.0022) O2B - O2C - Distance Angles S2 1.4559 (0.0023) O2C - S2 - Distance Angles O2B 1.4548 (0.0022) O2C 1.4559 (0.0023) 113.44 (0.14) O2A 1.4688 (0.0022) 111.77 (0.14) 111.32 (0.14) C2 1.7636 (0.0031) 107.87 (0.14) 105.91 (0.14) 106.01 (0.13) S2 - O2B O2C O2A C22 - Distance Angles O21 1.4195 (0.0036) C23 1.5122 (0.0042) 111.82 (0.26) H22A 0.9900 109.25 109.25 H22B 0.9900 109.25 109.25 107.93 C22 - O21 C23 H22A C23 - Distance Angles N24 1.4990 (0.0039) C22 1.5122 (0.0042) 110.93 (0.26) H23A 0.9900 109.45 109.45 H23B 0.9900 109.45 109.45 108.04 C23 - N24 C22 H23A N24 - Distance Angles C23 1.4990 (0.0039) 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 1.4195 (0.0036) H21 0.8400 109.47 O21 - C22 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.95 2.832(3) 163.2 N24-H24A...O2A_$1 0.91 2.95 3.836(3) 163.7 N24-H24A...S2_$1 0.91 2.00 2.884(3) 163.2 N24-H24B...O2B_$2 0.91 2.99 3.719(3) 138.1 N24-H24B...S2_$2 0.84 1.92 2.758(3) 175.6 O21-H21...O2A_$2 0.84 2.99 3.778(2) 157.7 O21-H21...S2_$2 0.91 1.97 2.856(3) 165.0 N24-H24C...O2C_$3 0.91 2.86 3.710(3) 155.3 N24-H24C...S2_$3 FMAP and GRID set by program FMAP 2 2 13 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.1226 for 2804 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.41 at 0.7386 0.1312 0.0989 [ 0.76 A from C2 ] Deepest hole -0.40 at 0.6774 0.0533 0.0977 [ 0.72 A from S2 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 2606 / 18172 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7386 0.1312 0.0989 1.00000 0.05 0.41 0.76 C2 1.04 S2 1.78 C1 1.96 O2B Q2 1 1.4526 0.1250 0.5685 1.00000 0.05 0.39 1.33 O21 1.86 C22 1.94 H23A 2.02 H22B Q3 1 0.6172 0.0190 0.2676 1.00000 0.05 0.29 0.84 O2B 1.61 H24B 2.05 S2 2.33 H23A Q4 1 0.6348 0.0213 -0.0743 1.00000 0.05 0.29 0.82 O2A 1.71 H21 2.06 H24A 2.15 S2 Q5 1 1.1263 0.3591 0.1533 1.00000 0.05 0.29 1.55 C6 1.75 C7 1.77 H6 1.84 H1 Q6 1 0.9177 -0.1509 0.3045 1.00000 0.05 0.28 1.77 H9 1.81 C6 1.81 H1 2.10 C7 Q7 1 1.0340 0.2601 0.0736 1.00000 0.05 0.27 0.78 C5 0.79 C6 1.51 H6 1.83 C7 Q8 1 1.3960 0.2483 0.3476 1.00000 0.05 0.27 1.12 C23 1.27 C22 1.30 H24B 1.34 N24 Q9 1 1.4128 0.1244 0.3866 1.00000 0.05 0.27 0.63 C23 0.97 C22 1.15 H23A 1.33 H23B Q10 1 0.9231 0.3646 -0.0374 1.00000 0.05 0.27 0.43 H4 0.61 C4 1.68 C5 1.82 C3 Shortest distances between peaks (including symmetry equivalents) 5 6 0.79 8 9 1.16 6 7 1.55 5 7 1.66 2 9 1.89 7 10 2.00 1 4 2.34 2 3 2.40 2 8 2.55 3 8 2.63 5 10 2.73 1 3 2.74 2 9 2.85 6 10 2.97 2 2 2.98 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. 0.73: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.92: Structure factors and derivatives 1.09: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.16: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0022p21c finished at 15:44:20 Total CPU time: 3.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++