+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0012p212121 started at 15:22:41 on 04-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0012p212121 in P2(1)2(1)2(1) CELL 0.71073 8.1972 14.3404 14.6661 90.000 90.000 90.000 ZERR 12.00 0.0010 0.0020 0.0015 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O UNIT 60 84 12 36 V = 1724.02 F(000) = 816.0 Mu = 0.12 mm-1 Cell Wt = 1549.39 Rho = 1.492 MERG 2 OMIT -3.00 55.00 OMIT 0 1 1 SHEL 7 0.77 HTAB N1 O26B EQIV_$1 x-1/2, -y+1/2, -z+1 HTAB O6A O22_$1 HTAB N21 O36B_$1 EQIV_$2 x+1/2, -y+1/2, -z HTAB O26A O2_$2 EQIV_$3 -x+1/2, -y, z-1/2 HTAB O36A O32_$3 EQIV_$4 x+1/2, -y+1/2, -z+1 HTAB N31 O26B_$4 EQIV_$5 -x+1/2, -y, z+1/2 HTAB N31 O6A_$5 FMAP 2 PLAN 5 SIZE 0.06 0.10 0.22 ACTA BOND $H WGHT 0.05340 L.S. 4 TEMP -153.00 FVAR 0.45983 MOLE 1 C2 1 -0.181168 0.213315 0.032946 11.00000 0.03646 0.04827 = 0.03076 -0.00769 -0.00444 0.00233 C3 1 -0.281642 0.126625 0.021456 11.00000 0.03951 0.04740 = 0.03324 -0.00329 -0.00298 -0.00092 AFIX 23 H3A 2 -0.226101 0.081307 -0.018911 11.00000 -1.20000 H3B 2 -0.390198 0.141432 -0.004345 11.00000 -1.20000 AFIX 0 C4 1 -0.296951 0.088408 0.118393 11.00000 0.04382 0.04793 = 0.03485 -0.00024 -0.00352 -0.00500 AFIX 23 H4A 2 -0.297617 0.019374 0.118351 11.00000 -1.20000 H4B 2 -0.397910 0.111176 0.148006 11.00000 -1.20000 AFIX 0 C5 1 -0.144957 0.126243 0.166996 11.00000 0.03778 0.04794 = 0.03599 0.00119 0.00177 0.00097 AFIX 13 H5 2 -0.052678 0.081125 0.160463 11.00000 -1.20000 AFIX 0 C6 1 -0.174768 0.146876 0.267002 11.00000 0.03560 0.04167 = 0.04034 0.00743 0.00259 0.00143 N1 3 -0.110753 0.210452 0.114995 11.00000 0.04823 0.04510 = 0.03160 -0.00161 -0.00425 -0.00795 AFIX 43 H1 2 -0.048759 0.255754 0.135911 11.00000 -1.20000 AFIX 0 O2 4 -0.161486 0.278433 -0.021925 11.00000 0.06261 0.04721 = 0.03264 0.00484 -0.00530 -0.00800 O6A 4 -0.201047 0.069334 0.312876 11.00000 0.05616 0.04423 = 0.03099 0.00120 0.00345 -0.00147 AFIX 147 H6A 2 -0.212590 0.081870 0.368451 11.00000 -1.50000 AFIX 0 O6B 4 -0.172705 0.223845 0.299516 11.00000 0.06751 0.04195 = 0.03798 -0.00185 0.00038 -0.00297 MOLE 2 C22 1 0.228810 0.342820 0.468698 11.00000 0.02982 0.04683 = 0.03291 0.01157 0.00034 -0.00668 C23 1 0.365452 0.273238 0.478770 11.00000 0.04035 0.04383 = 0.04173 0.00210 -0.00195 0.00034 AFIX 23 H23A 2 0.335022 0.223087 0.521928 11.00000 -1.20000 H23B 2 0.466080 0.303995 0.500881 11.00000 -1.20000 AFIX 0 C24 1 0.389871 0.234033 0.382182 11.00000 0.03420 0.04917 = 0.03114 0.00212 -0.00478 0.00766 AFIX 23 H24A 2 0.475292 0.268948 0.348840 11.00000 -1.20000 H24B 2 0.419704 0.167161 0.383950 11.00000 -1.20000 AFIX 0 C25 1 0.222024 0.248281 0.338658 11.00000 0.04661 0.04088 = 0.03066 -0.00043 0.00027 -0.00256 AFIX 13 H25 2 0.152739 0.192375 0.351354 11.00000 -1.20000 AFIX 0 C26 1 0.224376 0.265909 0.237818 11.00000 0.03269 0.04876 = 0.03669 -0.00294 -0.00532 -0.01184 N21 3 0.156901 0.327681 0.388410 11.00000 0.03993 0.04822 = 0.03198 0.00370 -0.00451 0.00208 AFIX 43 H21 2 0.077099 0.362674 0.367431 11.00000 -1.20000 AFIX 0 O22 4 0.187705 0.403417 0.524357 11.00000 0.04437 0.04368 = 0.03349 -0.00415 0.00066 0.00343 O26A 4 0.301863 0.199089 0.194056 11.00000 0.07040 0.06189 = 0.03113 0.00018 0.00513 0.01891 AFIX 147 H26A 2 0.300232 0.210164 0.137821 11.00000 -1.50000 AFIX 0 O26B 4 0.157389 0.331279 0.201001 11.00000 0.04441 0.05058 = 0.03320 0.00550 -0.00391 0.00741 MOLE 3 C32 1 0.321144 0.009360 0.921867 11.00000 0.04071 0.04934 = 0.03199 -0.00565 0.00452 -0.00220 C33 1 0.142040 0.028495 0.934311 11.00000 0.03366 0.05247 = 0.03563 0.00259 -0.00026 -0.00140 AFIX 23 H33A 2 0.124431 0.084660 0.972309 11.00000 -1.20000 H33B 2 0.086455 -0.025242 0.963131 11.00000 -1.20000 AFIX 0 C34 1 0.080255 0.043984 0.836845 11.00000 0.03392 0.05335 = 0.04184 0.00243 -0.00015 0.00046 AFIX 23 H34A 2 -0.010969 0.089209 0.835645 11.00000 -1.20000 H34B 2 0.043796 -0.015312 0.808920 11.00000 -1.20000 AFIX 0 C35 1 0.230878 0.082907 0.787730 11.00000 0.03912 0.04617 = 0.03028 -0.00062 -0.00154 -0.00025 AFIX 13 H35 2 0.234266 0.152051 0.796370 11.00000 -1.20000 AFIX 0 C36 1 0.246780 0.061406 0.687268 11.00000 0.04558 0.03006 = 0.04057 0.00530 -0.00682 -0.00148 N31 3 0.363045 0.040983 0.839428 11.00000 0.02878 0.05974 = 0.03152 -0.00134 0.00295 0.00349 AFIX 43 H31 2 0.463097 0.036735 0.818078 11.00000 -1.20000 AFIX 0 O32 4 0.415519 -0.028825 0.975369 11.00000 0.04334 0.06290 = 0.03148 0.00600 -0.00251 0.00788 O36A 4 0.103464 0.064989 0.645713 11.00000 0.04338 0.06746 = 0.03193 -0.00403 -0.00165 0.00250 AFIX 147 H36A 2 0.116344 0.055881 0.589594 11.00000 -1.50000 AFIX 0 O36B 4 0.375006 0.046671 0.649878 11.00000 0.03598 0.05751 = 0.03681 -0.00154 0.00470 0.00332 HKLF 4 Covalent radii and connectivity table for 06skc0012p212121 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 C2 - O2 N1 C3 C3 - C2 C4 C4 - C3 C5 C5 - N1 C6 C4 C6 - O6B O6A C5 N1 - C2 C5 O2 - C2 O6A - C6 O6B - C6 C22 - O22 N21 C23 C23 - C22 C24 C24 - C25 C23 C25 - N21 C26 C24 C26 - O26B O26A C25 N21 - C22 C25 O22 - C22 O26A - C26 O26B - C26 C32 - O32 N31 C33 C33 - C32 C34 C34 - C33 C35 C35 - N31 C36 C34 C36 - O36B O36A C35 N31 - C32 C35 O32 - C32 O36A - C36 O36B - C36 Operators for generating equivalent atoms: $1 x-1/2, -y+1/2, -z+1 $2 x+1/2, -y+1/2, -z $3 -x+1/2, -y, z-1/2 $4 x+1/2, -y+1/2, -z+1 $5 -x+1/2, -y, z+1/2 23268 Reflections read, of which 127 rejected -9 =< h =< 8, -15 =< k =< 15, -16 =< l =< 16, Max. 2-theta = 46.74 0 Systematic absence violations 0 Inconsistent equivalents 2495 Unique reflections, of which 0 suppressed R(int) = 0.1562 R(sigma) = 0.0869 Friedel opposites not merged Maximum memory for data reduction = 2722 / 24891 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 = 3416 / 306551 wR2 = 0.1118 before cycle 1 for 2495 data and 247 / 247 parameters GooF = S = 1.012; Restrained GooF = 1.012 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0534 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45993 0.00120 0.084 OSF Mean shift/esd = 0.033 Maximum = 0.118 for y C26 Max. shift = 0.002 A for H6A Max. dU = 0.000 for C33 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3416 / 306551 wR2 = 0.1118 before cycle 2 for 2495 data and 247 / 247 parameters GooF = S = 1.013; Restrained GooF = 1.013 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0534 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45990 0.00120 -0.022 OSF Mean shift/esd = 0.010 Maximum = 0.037 for y C26 Max. shift = 0.000 A for H6A Max. dU = 0.000 for C33 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3416 / 306551 wR2 = 0.1118 before cycle 3 for 2495 data and 247 / 247 parameters GooF = S = 1.013; Restrained GooF = 1.013 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0534 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45990 0.00120 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.004 for U23 N1 Max. shift = 0.000 A for H26A Max. dU = 0.000 for C32 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3416 / 306551 wR2 = 0.1118 before cycle 4 for 2495 data and 247 / 247 parameters GooF = S = 1.012; Restrained GooF = 1.012 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0534 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45990 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U33 N1 Max. shift = 0.000 A for H6A Max. dU = 0.000 for C4 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 H3A -0.2261 0.0813 -0.0190 23 0.990 0.000 C3 C2 C4 H3B -0.3902 0.1415 -0.0044 23 0.990 0.000 C3 C2 C4 H4A -0.2976 0.0194 0.1183 23 0.990 0.000 C4 C3 C5 H4B -0.3979 0.1112 0.1480 23 0.990 0.000 C4 C3 C5 H5 -0.0526 0.0811 0.1605 13 1.000 0.000 C5 N1 C6 C4 H1 -0.0488 0.2557 0.1359 43 0.880 0.000 N1 C2 C5 H6A -0.2123 0.0818 0.3685 147 0.840 0.000 O6A C6 H6A H23A 0.3349 0.2231 0.5219 23 0.990 0.000 C23 C22 C24 H23B 0.4660 0.3040 0.5009 23 0.990 0.000 C23 C22 C24 H24A 0.4753 0.2690 0.3488 23 0.990 0.000 C24 C25 C23 H24B 0.4198 0.1672 0.3839 23 0.990 0.000 C24 C25 C23 H25 0.1527 0.1924 0.3513 13 1.000 0.000 C25 N21 C26 C24 H21 0.0771 0.3627 0.3674 43 0.880 0.000 N21 C22 C25 H26A 0.3001 0.2101 0.1378 147 0.840 0.000 O26A C26 H26A H33A 0.1245 0.0847 0.9723 23 0.990 0.000 C33 C32 C34 H33B 0.0865 -0.0252 0.9632 23 0.990 0.000 C33 C32 C34 H34A -0.0110 0.0892 0.8356 23 0.990 0.000 C34 C33 C35 H34B 0.0438 -0.0153 0.8089 23 0.990 0.000 C34 C33 C35 H35 0.2343 0.1521 0.7964 13 1.000 0.000 C35 N31 C36 C34 H31 0.4631 0.0367 0.8181 43 0.880 0.000 N31 C32 C35 H36A 0.1163 0.0560 0.5896 147 0.840 0.000 O36A C36 H36A 06skc0012p212121 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 -0.18116 0.21334 0.03292 1.00000 0.03645 0.04836 0.03061 -0.00778 -0.00445 0.00230 0.03847 0.00773 0.00055 0.00033 0.00032 0.00000 0.00305 0.00340 0.00310 0.00268 0.00247 0.00283 0.00120 C3 -0.28166 0.12664 0.02143 1.00000 0.03944 0.04746 0.03308 -0.00328 -0.00304 -0.00102 0.03999 0.00725 0.00056 0.00029 0.00027 0.00000 0.00313 0.00320 0.00274 0.00244 0.00246 0.00251 0.00128 H3A -0.22613 0.08133 -0.01895 1.00000 0.04799 0.00000 0.00000 H3B -0.39022 0.14145 -0.00436 1.00000 0.04799 0.00000 0.00000 C4 -0.29696 0.08839 0.11839 1.00000 0.04373 0.04779 0.03496 -0.00023 -0.00366 -0.00494 0.04216 0.00747 0.00057 0.00035 0.00026 0.00000 0.00328 0.00318 0.00291 0.00235 0.00235 0.00271 0.00129 H4A -0.29763 0.01935 0.11833 1.00000 0.05059 0.00000 0.00000 H4B -0.39791 0.11115 0.14801 1.00000 0.05059 0.00000 0.00000 C5 -0.14492 0.12622 0.16699 1.00000 0.03777 0.04786 0.03579 0.00118 0.00187 0.00080 0.04047 0.00759 0.00055 0.00032 0.00029 0.00000 0.00308 0.00327 0.00301 0.00252 0.00247 0.00242 0.00127 H5 -0.05264 0.08111 0.16046 1.00000 0.04857 0.00000 0.00000 C6 -0.17473 0.14692 0.26701 1.00000 0.03540 0.04196 0.04029 0.00772 0.00273 0.00157 0.03922 0.00865 0.00053 0.00038 0.00030 0.00000 0.00289 0.00344 0.00352 0.00274 0.00245 0.00273 0.00124 N1 -0.11077 0.21044 0.11499 1.00000 0.04839 0.04501 0.03132 -0.00162 -0.00419 -0.00806 0.04158 0.00619 0.00047 0.00025 0.00023 0.00000 0.00287 0.00269 0.00243 0.00200 0.00198 0.00223 0.00107 H1 -0.04880 0.25575 0.13592 1.00000 0.04989 0.00000 0.00000 O2 -0.16146 0.27843 -0.02192 1.00000 0.06256 0.04713 0.03270 0.00500 -0.00517 -0.00805 0.04746 0.00523 0.00041 0.00022 0.00020 0.00000 0.00233 0.00212 0.00192 0.00171 0.00170 0.00195 0.00089 O6A -0.20106 0.06933 0.31287 1.00000 0.05625 0.04427 0.03103 0.00114 0.00343 -0.00156 0.04385 0.00494 0.00039 0.00020 0.00018 0.00000 0.00210 0.00203 0.00172 0.00160 0.00173 0.00170 0.00082 H6A -0.21234 0.08182 0.36847 1.00000 0.06578 0.00000 0.00000 O6B -0.17273 0.22387 0.29952 1.00000 0.06772 0.04173 0.03802 -0.00200 0.00038 -0.00304 0.04916 0.00546 0.00037 0.00023 0.00020 0.00000 0.00246 0.00210 0.00200 0.00169 0.00188 0.00188 0.00091 C22 0.22882 0.34282 0.46870 1.00000 0.02985 0.04694 0.03282 0.01157 0.00047 -0.00664 0.03654 0.00850 0.00053 0.00033 0.00032 0.00000 0.00287 0.00326 0.00319 0.00258 0.00257 0.00269 0.00117 C23 0.36540 0.27324 0.47878 1.00000 0.04024 0.04391 0.04170 0.00211 -0.00180 0.00032 0.04195 0.00785 0.00054 0.00031 0.00029 0.00000 0.00325 0.00311 0.00304 0.00253 0.00248 0.00259 0.00128 H23A 0.33493 0.22309 0.52193 1.00000 0.05034 0.00000 0.00000 H23B 0.46602 0.30399 0.50092 1.00000 0.05034 0.00000 0.00000 C24 0.38989 0.23404 0.38217 1.00000 0.03412 0.04907 0.03114 0.00201 -0.00477 0.00768 0.03811 0.00752 0.00054 0.00033 0.00026 0.00000 0.00302 0.00325 0.00279 0.00242 0.00222 0.00248 0.00126 H24A 0.47529 0.26898 0.34884 1.00000 0.04574 0.00000 0.00000 H24B 0.41977 0.16718 0.38394 1.00000 0.04574 0.00000 0.00000 C25 0.22196 0.24828 0.33865 1.00000 0.04673 0.04067 0.03051 -0.00062 0.00020 -0.00237 0.03930 0.00776 0.00058 0.00031 0.00027 0.00000 0.00310 0.00309 0.00282 0.00246 0.00239 0.00250 0.00123 H25 0.15267 0.19237 0.35133 1.00000 0.04716 0.00000 0.00000 C26 0.22432 0.26597 0.23782 1.00000 0.03281 0.04894 0.03649 -0.00321 -0.00508 -0.01204 0.03941 0.00739 0.00059 0.00038 0.00029 0.00000 0.00292 0.00352 0.00330 0.00281 0.00258 0.00265 0.00124 N21 0.15689 0.32768 0.38841 1.00000 0.03992 0.04825 0.03185 0.00366 -0.00463 0.00213 0.04001 0.00640 0.00047 0.00025 0.00024 0.00000 0.00243 0.00277 0.00238 0.00194 0.00202 0.00219 0.00102 H21 0.07710 0.36268 0.36744 1.00000 0.04801 0.00000 0.00000 O22 0.18770 0.40343 0.52437 1.00000 0.04434 0.04363 0.03347 -0.00416 0.00059 0.00354 0.04048 0.00518 0.00038 0.00020 0.00020 0.00000 0.00207 0.00195 0.00179 0.00161 0.00155 0.00172 0.00082 O26A 0.30185 0.19908 0.19406 1.00000 0.07053 0.06182 0.03109 0.00023 0.00492 0.01872 0.05448 0.00596 0.00043 0.00023 0.00021 0.00000 0.00241 0.00229 0.00194 0.00181 0.00201 0.00198 0.00092 H26A 0.30014 0.21010 0.13782 1.00000 0.08172 0.00000 0.00000 O26B 0.15735 0.33130 0.20098 1.00000 0.04456 0.05032 0.03323 0.00561 -0.00397 0.00755 0.04270 0.00485 0.00035 0.00022 0.00020 0.00000 0.00199 0.00216 0.00191 0.00167 0.00169 0.00172 0.00083 C32 0.32120 0.00936 0.92189 1.00000 0.04071 0.04925 0.03184 -0.00593 0.00478 -0.00226 0.04060 0.00782 0.00060 0.00033 0.00032 0.00000 0.00326 0.00349 0.00305 0.00255 0.00254 0.00287 0.00127 C33 0.14209 0.02853 0.93433 1.00000 0.03357 0.05240 0.03541 0.00258 -0.00015 -0.00139 0.04046 0.00757 0.00049 0.00034 0.00028 0.00000 0.00310 0.00330 0.00278 0.00236 0.00226 0.00260 0.00124 H33A 0.12451 0.08471 0.97231 1.00000 0.04855 0.00000 0.00000 H33B 0.08649 -0.02519 0.96318 1.00000 0.04855 0.00000 0.00000 C34 0.08024 0.04399 0.83683 1.00000 0.03405 0.05342 0.04180 0.00244 0.00001 0.00042 0.04309 0.00792 0.00054 0.00033 0.00027 0.00000 0.00278 0.00334 0.00283 0.00266 0.00237 0.00256 0.00124 H34A -0.01099 0.08921 0.83562 1.00000 0.05171 0.00000 0.00000 H34B 0.04380 -0.01531 0.80891 1.00000 0.05171 0.00000 0.00000 C35 0.23093 0.08292 0.78773 1.00000 0.03904 0.04610 0.03030 -0.00061 -0.00156 -0.00031 0.03848 0.00753 0.00052 0.00032 0.00028 0.00000 0.00298 0.00293 0.00253 0.00227 0.00236 0.00249 0.00116 H35 0.23432 0.15207 0.79637 1.00000 0.04618 0.00000 0.00000 C36 0.24681 0.06140 0.68725 1.00000 0.04557 0.02978 0.04052 0.00536 -0.00703 -0.00142 0.03862 0.00757 0.00064 0.00029 0.00029 0.00000 0.00355 0.00293 0.00301 0.00238 0.00288 0.00255 0.00117 N31 0.36306 0.04100 0.83942 1.00000 0.02886 0.05981 0.03133 -0.00134 0.00282 0.00362 0.04000 0.00569 0.00040 0.00025 0.00023 0.00000 0.00232 0.00278 0.00219 0.00218 0.00188 0.00206 0.00102 H31 0.46310 0.03674 0.81805 1.00000 0.04800 0.00000 0.00000 O32 0.41552 -0.02884 0.97539 1.00000 0.04332 0.06268 0.03151 0.00618 -0.00265 0.00800 0.04584 0.00528 0.00038 0.00021 0.00020 0.00000 0.00209 0.00240 0.00179 0.00179 0.00160 0.00191 0.00089 O36A 0.10347 0.06500 0.64571 1.00000 0.04336 0.06742 0.03195 -0.00416 -0.00158 0.00252 0.04758 0.00545 0.00037 0.00025 0.00019 0.00000 0.00214 0.00254 0.00177 0.00202 0.00159 0.00186 0.00091 H36A 0.11635 0.05599 0.58957 1.00000 0.07136 0.00000 0.00000 O36B 0.37504 0.04667 0.64987 1.00000 0.03588 0.05736 0.03692 -0.00154 0.00476 0.00319 0.04339 0.00499 0.00037 0.00022 0.00019 0.00000 0.00212 0.00237 0.00192 0.00165 0.00153 0.00172 0.00089 Final Structure Factor Calculation for 06skc0012p212121 in P2(1)2(1)2(1) Total number of l.s. parameters = 247 Maximum vector length = 511 Memory required = 3171 / 25046 wR2 = 0.1118 before cycle 5 for 2495 data and 2 / 247 parameters GooF = S = 1.012; Restrained GooF = 1.012 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0534 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0518 for 1581 Fo > 4sig(Fo) and 0.1088 for all 2495 data wR2 = 0.1118, GooF = S = 1.012, Restrained GooF = 1.012 for all data Flack x parameter = 0.1523 with esd 1.9909 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 27.00 for non-hydrogen and 21.00 for hydrogen atoms Principal mean square atomic displacements U 0.0522 0.0367 0.0265 C2 0.0482 0.0406 0.0311 C3 0.0513 0.0418 0.0333 C4 0.0481 0.0387 0.0346 C5 0.0495 0.0353 0.0329 C6 0.0552 0.0401 0.0294 N1 0.0673 0.0442 0.0309 O2 0.0569 0.0442 0.0304 O6A 0.0681 0.0423 0.0371 O6B 0.0547 0.0312 0.0237 C22 0.0453 0.0420 0.0386 C23 0.0523 0.0362 0.0258 C24 0.0476 0.0399 0.0305 C25 0.0554 0.0393 0.0236 C26 0.0492 0.0420 0.0288 N21 0.0480 0.0417 0.0317 O22 0.0857 0.0474 0.0303 O26A 0.0558 0.0433 0.0290 O26B 0.0523 0.0409 0.0287 C32 0.0529 0.0350 0.0335 C33 0.0539 0.0413 0.0340 C34 0.0461 0.0393 0.0300 C35 0.0514 0.0371 0.0274 C36 0.0603 0.0331 0.0266 N31 0.0663 0.0422 0.0290 O32 0.0682 0.0432 0.0313 O36A 0.0579 0.0411 0.0312 O36B Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.021 0.028 0.037 0.045 0.054 0.066 0.085 0.112 1.000 Number in group 279. 236. 240. 279. 221. 241. 256. 248. 244. 251. GooF 0.892 0.968 0.896 0.993 1.003 1.106 1.071 1.040 0.950 1.179 K 0.374 0.830 0.979 0.956 0.945 0.957 0.989 0.991 1.010 0.994 Resolution(A) 0.89 0.93 0.97 1.01 1.07 1.13 1.22 1.34 1.53 1.92 inf Number in group 250. 256. 249. 248. 244. 249. 252. 250. 247. 250. GooF 0.970 0.946 0.967 1.065 1.026 0.987 1.043 0.952 1.064 1.096 K 1.059 0.969 1.014 1.017 1.000 0.997 0.967 0.998 1.044 0.970 R1 0.363 0.266 0.220 0.138 0.114 0.095 0.082 0.044 0.035 0.028 Recommended weighting scheme: WGHT 0.0527 0.0000 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 0 2 2989.45 3811.79 4.25 0.273 5.47 0 2 1 41.93 94.92 4.07 0.043 6.44 -6 9 6 481.88 318.31 4.02 0.079 0.95 2 7 11 121.46 231.07 3.96 0.067 1.08 0 2 2 56.18 40.72 3.77 0.028 5.13 6 5 8 596.43 430.03 3.72 0.092 1.02 0 2 8 1160.56 954.49 3.63 0.137 1.78 7 0 6 468.69 352.86 3.42 0.083 1.06 -5 4 9 64.63 147.66 3.36 0.054 1.10 0 10 11 1035.30 797.62 3.15 0.125 0.98 3 10 0 80.46 126.85 3.08 0.050 1.27 8 5 4 150.78 11.77 2.96 0.015 0.93 3 15 0 -11.98 118.65 2.89 0.048 0.90 2 12 6 -4.96 44.85 2.88 0.030 1.04 2 13 0 1203.21 976.88 2.83 0.138 1.07 -6 2 4 220.08 278.60 2.72 0.074 1.26 3 9 3 139.90 204.09 2.71 0.063 1.32 -2 15 4 174.45 40.18 2.70 0.028 0.90 0 8 3 2124.54 1833.47 2.69 0.189 1.68 7 7 1 299.98 208.39 2.67 0.064 1.01 3 5 6 336.70 406.64 2.66 0.089 1.54 -1 3 3 213.85 183.36 2.64 0.060 3.15 -7 7 5 24.27 114.73 2.62 0.047 0.96 1 8 2 2088.20 1803.19 2.61 0.188 1.70 4 9 8 18.43 135.57 2.59 0.051 1.04 -4 6 11 720.04 592.69 2.58 0.108 1.01 1 8 5 3388.53 2932.00 2.57 0.239 1.50 -5 3 5 84.05 120.01 2.55 0.048 1.37 8 0 4 269.73 179.63 2.52 0.059 0.99 4 7 5 95.08 140.13 2.49 0.052 1.30 2 2 13 33.17 125.92 2.48 0.050 1.08 -1 10 7 50.70 109.32 2.48 0.046 1.17 4 4 11 375.07 284.71 2.48 0.075 1.07 -4 7 3 42.79 77.72 2.47 0.039 1.39 -3 5 5 3781.32 3302.74 2.46 0.254 1.64 -1 13 5 77.79 142.74 2.45 0.053 1.02 -3 8 10 254.76 182.55 2.45 0.060 1.05 7 9 4 105.15 35.00 2.43 0.026 0.91 2 1 0 4718.40 5375.28 2.43 0.324 3.94 -2 5 12 390.87 312.32 2.43 0.078 1.08 -5 8 11 231.85 4.72 2.41 0.010 0.90 -4 5 12 51.45 129.92 2.41 0.050 0.99 3 11 9 540.26 384.84 2.39 0.087 0.95 2 0 0 45011.98 51224.54 2.36 1.000 4.10 1 2 9 218.13 260.23 2.36 0.071 1.56 1 7 9 42.66 89.25 2.36 0.042 1.26 3 0 10 54.01 21.31 2.34 0.020 1.29 0 8 1 4262.28 3757.50 2.34 0.271 1.78 1 7 10 27.86 79.32 2.33 0.039 1.18 1 8 4 1455.79 1263.12 2.33 0.157 1.58 Bond lengths and angles C2 - Distance Angles O2 1.2427 (0.0047) N1 1.3354 (0.0052) 123.41 (0.42) C3 1.5010 (0.0058) 128.37 (0.39) 108.21 (0.39) C2 - O2 N1 C3 - Distance Angles C2 1.5010 (0.0058) C4 1.5293 (0.0055) 103.75 (0.33) H3A 0.9900 111.01 111.01 H3B 0.9900 111.01 111.01 109.00 C3 - C2 C4 H3A C4 - Distance Angles C3 1.5293 (0.0055) C5 1.5348 (0.0058) 103.80 (0.36) H4A 0.9900 111.00 111.00 H4B 0.9900 111.00 111.00 108.99 C4 - C3 C5 H4A C5 - Distance Angles N1 1.4556 (0.0051) C6 1.5165 (0.0058) 112.05 (0.39) C4 1.5348 (0.0058) 101.90 (0.34) 112.81 (0.38) H5 1.0000 109.95 109.95 109.95 C5 - N1 C6 C4 C6 - Distance Angles O6B 1.2021 (0.0051) O6A 1.3180 (0.0050) 125.09 (0.42) C5 1.5165 (0.0058) 124.13 (0.43) 110.78 (0.42) C6 - O6B O6A N1 - Distance Angles C2 1.3354 (0.0052) C5 1.4556 (0.0051) 114.52 (0.37) H1 0.8800 122.74 122.74 N1 - C2 C5 O2 - Distance Angles C2 1.2427 (0.0047) O2 - O6A - Distance Angles C6 1.3180 (0.0050) H6A 0.8400 109.47 O6A - C6 O6B - Distance Angles C6 1.2021 (0.0051) O6B - C22 - Distance Angles O22 1.2392 (0.0050) N21 1.3347 (0.0054) 125.11 (0.42) C23 1.5069 (0.0059) 127.00 (0.41) 107.89 (0.40) C22 - O22 N21 C23 - Distance Angles C22 1.5069 (0.0059) C24 1.5375 (0.0054) 104.40 (0.35) H23A 0.9900 110.87 110.87 H23B 0.9900 110.87 110.87 108.91 C23 - C22 C24 H23A C24 - Distance Angles C25 1.5311 (0.0060) C23 1.5375 (0.0055) 102.60 (0.34) H24A 0.9900 111.25 111.25 H24B 0.9900 111.25 111.25 109.16 C24 - C25 C23 H24A C25 - Distance Angles N21 1.4538 (0.0052) C26 1.5005 (0.0054) 111.53 (0.40) C24 1.5311 (0.0060) 103.00 (0.35) 114.95 (0.39) H25 1.0000 109.04 109.04 109.04 C25 - N21 C26 C24 C26 - Distance Angles O26B 1.2128 (0.0051) O26A 1.3175 (0.0053) 124.31 (0.41) C25 1.5005 (0.0054) 124.32 (0.47) 111.30 (0.45) C26 - O26B O26A N21 - Distance Angles C22 1.3347 (0.0054) C25 1.4538 (0.0052) 114.09 (0.38) H21 0.8800 122.95 122.95 N21 - C22 C25 O22 - Distance Angles C22 1.2392 (0.0050) O22 - O26A - Distance Angles C26 1.3175 (0.0053) H26A 0.8400 109.47 O26A - C26 O26B - Distance Angles C26 1.2128 (0.0052) O26B - C32 - Distance Angles O32 1.2302 (0.0051) N31 1.3366 (0.0052) 124.54 (0.44) C33 1.5048 (0.0064) 128.11 (0.43) 107.35 (0.40) C32 - O32 N31 C33 - Distance Angles C32 1.5048 (0.0064) C34 1.5333 (0.0055) 103.65 (0.35) H33A 0.9900 111.03 111.03 H33B 0.9900 111.03 111.03 109.01 C33 - C32 C34 H33A C34 - Distance Angles C33 1.5333 (0.0055) C35 1.5349 (0.0060) 102.94 (0.35) H34A 0.9900 111.18 111.18 H34B 0.9900 111.18 111.18 109.11 C34 - C33 C35 H34A C35 - Distance Angles N31 1.4523 (0.0050) C36 1.5113 (0.0059) 111.11 (0.37) C34 1.5349 (0.0060) 101.82 (0.32) 116.90 (0.39) H35 1.0000 108.88 108.88 108.88 C35 - N31 C36 C34 C36 - Distance Angles O36B 1.2042 (0.0050) O36A 1.3245 (0.0051) 124.88 (0.38) C35 1.5113 (0.0059) 123.70 (0.42) 111.36 (0.41) C36 - O36B O36A N31 - Distance Angles C32 1.3366 (0.0052) C35 1.4523 (0.0050) 114.92 (0.35) H31 0.8800 122.54 122.54 N31 - C32 C35 O32 - Distance Angles C32 1.2302 (0.0051) O32 - O36A - Distance Angles C36 1.3245 (0.0051) H36A 0.8400 109.47 O36A - C36 O36B - Distance Angles C36 1.2042 (0.0051) O36B - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.22 3.070(5) 161.5 N1-H1...O26B 0.84 1.79 2.585(4) 158.5 O6A-H6A...O22_$1 0.88 2.12 2.983(5) 166.4 N21-H21...O36B_$1 0.84 1.74 2.563(4) 167.4 O26A-H26A...O2_$2 0.84 1.74 2.556(4) 163.6 O36A-H36A...O32_$3 0.88 2.49 3.086(5) 125.7 N31-H31...O26B_$4 0.88 2.47 3.214(5) 142.0 N31-H31...O6A_$5 FMAP and GRID set by program FMAP 2 1 11 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0867 for 1453 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.22 at 0.0364 0.1967 0.0171 [ 1.81 A from C2 ] Deepest hole -0.27 at 0.2501 0.2831 0.4040 [ 1.02 A from N21 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 3265 / 17547 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0364 0.1967 0.0171 1.00000 0.05 0.22 1.81 C2 1.88 H33A 1.89 N1 2.06 H1 Q2 1 0.0290 0.3392 0.3777 1.00000 0.05 0.20 0.54 H21 1.07 N21 2.11 O36B 2.11 C22 Q3 1 0.4732 0.0632 0.8249 1.00000 0.05 0.19 0.40 H31 0.98 N31 2.04 C32 2.08 C35 Q4 1 -0.0567 -0.0750 0.8192 1.00000 0.05 0.18 1.20 H34B 1.98 H24B 1.99 O6A 2.03 H6A Q5 1 -0.4395 0.2154 -0.0421 1.00000 0.05 0.18 1.26 H3B 1.69 H1 2.04 C3 2.05 O2 Shortest distances between peaks (including symmetry equivalents) 1 5 1.33 Time profile in seconds ----------------------- 0.09: 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. 1.05: 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 0.98: Structure factors and derivatives 1.06: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.19: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0012p212121 finished at 15:22:44 Total CPU time: 3.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++