+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0047p-1 started at 15:25:04 on 16-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0047p-1 in P-1 CELL 0.71073 8.1285 9.1297 13.7387 89.781 89.170 79.782 ZERR 2.00 0.0006 0.0007 0.0011 0.004 0.004 0.005 LATT 1 SFAC C H N O UNIT 36 56 8 16 V = 1003.28 F(000) = 456.0 Mu = 0.11 mm-1 Cell Wt = 856.89 Rho = 1.418 MERG 2 OMIT -3.00 55.00 OMIT 1 -4 3 OMIT -1 2 3 OMIT 0 2 6 OMIT 1 -1 11 SHEL 7 0.77 HTAB O1A O31A HTAB N43 O35B EQIV_$1 x+1, y-1, z HTAB N23 O31B_$1 EQIV_$2 x, y, z-1 HTAB O5B O35A_$2 FMAP 2 PLAN 10 SIZE 0.04 0.06 0.10 ACTA MPLA O1A O1B C1 MPLA O5A O5B C5 BOND $H WGHT 0.06950 9.75720 L.S. 4 TEMP -153.00 FVAR 0.77012 MOLE 1 C1 1 0.678375 0.555376 0.804645 11.00000 0.03448 0.02156 = 0.02152 -0.00612 0.00137 0.00030 C2 1 0.600008 0.630781 0.714166 11.00000 0.03045 0.02661 = 0.02640 -0.00399 -0.00071 -0.00364 AFIX 23 H2A 2 0.600160 0.738837 0.719739 11.00000 -1.20000 H2B 2 0.481821 0.617457 0.712760 11.00000 -1.20000 AFIX 0 C3 1 0.682173 0.577414 0.617526 11.00000 0.02710 0.01317 = 0.01932 -0.00101 -0.00225 0.00474 AFIX 23 H3A 2 0.676074 0.471099 0.607956 11.00000 -1.20000 H3B 2 0.801475 0.587392 0.617672 11.00000 -1.20000 AFIX 0 C4 1 0.592797 0.670153 0.534517 11.00000 0.03088 0.02293 = 0.02204 0.00564 -0.00678 -0.00329 AFIX 23 H4A 2 0.471641 0.668035 0.539744 11.00000 -1.20000 H4B 2 0.607544 0.774783 0.542308 11.00000 -1.20000 AFIX 0 C5 1 0.654804 0.616989 0.433879 11.00000 0.02757 0.02507 = 0.01944 -0.00330 -0.00611 -0.00181 O1A 4 0.609930 0.609282 0.888261 11.00000 0.03955 0.03764 = 0.01589 -0.00622 0.00141 0.00134 AFIX 147 H1 2 0.535180 0.683373 0.877271 11.00000 -1.50000 AFIX 0 O1B 4 0.790326 0.449405 0.801316 11.00000 0.03202 0.02918 = 0.01880 -0.00296 0.00157 0.00091 O5A 4 0.765619 0.503431 0.420823 11.00000 0.03198 0.03181 = 0.02163 -0.00537 -0.00006 0.00668 O5B 4 0.586383 0.690874 0.360374 11.00000 0.03747 0.02916 = 0.01953 0.00096 -0.00144 0.00804 AFIX 147 H5 2 0.519474 0.766023 0.380219 11.00000 -1.50000 AFIX 0 MOLE 2 C22 1 1.048388 0.186500 0.695773 11.00000 0.02780 0.02359 = 0.02431 -0.00875 0.00075 -0.00351 AFIX 43 H22 2 0.975874 0.265617 0.727451 11.00000 -1.20000 AFIX 0 C24 1 1.237577 -0.015255 0.668919 11.00000 0.03296 0.03666 = 0.03912 0.00402 0.00336 -0.00493 AFIX 43 H24 2 1.319810 -0.101313 0.679890 11.00000 -1.20000 AFIX 0 C25 1 1.184221 0.039027 0.585551 11.00000 0.03024 0.02946 = 0.04423 0.00574 -0.00971 -0.00354 AFIX 43 H25 2 1.222336 -0.003114 0.524399 11.00000 -1.20000 AFIX 0 C26 1 0.973229 0.257891 0.525199 11.00000 0.02810 0.03190 = 0.05363 0.00629 -0.01090 0.00804 AFIX 137 H26A 2 0.853625 0.256955 0.534332 11.00000 -1.50000 H26B 2 1.008992 0.220319 0.460146 11.00000 -1.50000 H26C 2 0.993754 0.359935 0.531868 11.00000 -1.50000 AFIX 0 N21 3 1.065433 0.165367 0.596924 11.00000 0.02584 0.02825 = 0.03182 0.00564 -0.00597 -0.00414 N23 3 1.149990 0.078076 0.738995 11.00000 0.03950 0.04033 = 0.02687 -0.00929 0.00370 -0.01015 AFIX 43 H23 2 1.160736 0.066533 0.802342 11.00000 0.03892 AFIX 0 MOLE 3 C31 1 0.317309 0.912413 0.933173 11.00000 0.02158 0.02791 = 0.01075 -0.00726 0.00263 -0.00820 C32 1 0.376013 0.860416 1.034877 11.00000 0.03027 0.02572 = 0.01266 -0.00285 0.00256 -0.00307 AFIX 23 H32A 2 0.359797 0.756088 1.042914 11.00000 -1.20000 H32B 2 0.497657 0.860271 1.037875 11.00000 -1.20000 AFIX 0 C33 1 0.292992 0.948790 1.120664 11.00000 0.02663 0.01313 = 0.01477 0.00006 -0.00056 0.00464 AFIX 23 H33A 2 0.172088 0.944686 1.121779 11.00000 -1.20000 H33B 2 0.305348 1.054241 1.113437 11.00000 -1.20000 AFIX 0 C34 1 0.370007 0.887793 1.215872 11.00000 0.03038 0.01963 = 0.01185 0.00401 0.00063 -0.00109 AFIX 23 H34A 2 0.360031 0.781478 1.220539 11.00000 -1.20000 H34B 2 0.490745 0.892441 1.213137 11.00000 -1.20000 AFIX 0 C35 1 0.297069 0.964356 1.307689 11.00000 0.03140 0.02755 = 0.01624 0.00462 0.00080 -0.01209 O31A 4 0.382100 0.830737 0.862782 11.00000 0.03465 0.03125 = 0.01805 -0.00151 0.00286 -0.00228 O31B 4 0.212779 1.027174 0.925242 11.00000 0.03735 0.03274 = 0.01760 0.00568 -0.00357 -0.00054 O35A 4 0.358687 0.907065 1.387339 11.00000 0.03793 0.04048 = 0.00819 -0.00244 0.00225 0.00268 O35B 4 0.183371 1.076570 1.306353 11.00000 0.03294 0.02799 = 0.01887 -0.00010 0.00105 0.00189 MOLE 4 C42 1 -0.100689 1.376325 1.207811 11.00000 0.03062 0.03749 = 0.01756 0.01044 -0.00423 -0.01257 AFIX 43 H42 2 -0.123094 1.402919 1.274091 11.00000 -1.20000 AFIX 0 C44 1 -0.001166 1.255806 1.072792 11.00000 0.02764 0.02769 = 0.04060 0.00946 -0.00432 0.00181 AFIX 43 H44 2 0.058353 1.183234 1.029825 11.00000 -1.20000 AFIX 0 C45 1 -0.106055 1.379289 1.050513 11.00000 0.03252 0.02649 = 0.04271 -0.00361 0.00250 -0.00117 AFIX 43 H45 2 -0.133833 1.410920 0.985925 11.00000 -1.20000 AFIX 0 C46 1 -0.286638 1.595949 1.134331 11.00000 0.04230 0.04112 = 0.03998 -0.00141 0.00357 0.00083 AFIX 137 H46A 2 -0.232821 1.675686 1.107811 11.00000 -1.50000 H46B 2 -0.320768 1.618607 1.202106 11.00000 -1.50000 H46C 2 -0.385250 1.588044 1.095844 11.00000 -1.50000 AFIX 0 N41 3 -0.167705 1.453560 1.130160 11.00000 0.03171 0.03002 = 0.03330 0.00750 -0.00471 -0.00625 N43 3 0.001211 1.257631 1.176014 11.00000 0.03584 0.02871 = 0.02498 0.00569 -0.00133 0.00102 AFIX 43 H43 2 0.061373 1.190013 1.212876 11.00000 -1.20000 AFIX 0 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 Covalent radii and connectivity table for 06skc0047p-1 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - C1 C3 C3 - C2 C4 C4 - C5 C3 C5 - O5A O5B C4 O1A - C1 O1B - C1 O5A - C5 O5B - C5 C22 - N23 N21 C24 - C25 N23 C25 - C24 N21 C26 - N21 N21 - C22 C25 C26 N23 - C22 C24 C31 - O31B O31A C32 C32 - C33 C31 C33 - C32 C34 C34 - C35 C33 C35 - O35B O35A C34 O31A - C31 O31B - C31 O35A - C35 O35B - C35 C42 - N43 N41 C44 - C45 N43 C45 - C44 N41 C46 - N41 N41 - C45 C42 C46 N43 - C42 C44 Operators for generating equivalent atoms: $1 x+1, y-1, z $2 x, y, z-1 18864 Reflections read, of which 117 rejected -10 =< h =< 10, -11 =< k =< 11, -17 =< l =< 17, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 6 4 7 12.77 1.25 6 7.04 1 Inconsistent equivalents 4591 Unique reflections, of which 0 suppressed R(int) = 0.1239 R(sigma) = 0.1191 Friedel opposites merged Maximum memory for data reduction = 2963 / 45246 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 = 3755 / 343845 wR2 = 0.3389 before cycle 1 for 4591 data and 276 / 276 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0695 * P )^2 + 9.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.77012 0.00386 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.002 for U13 O5A Max. shift = 0.000 A for H26C Max. dU = 0.000 for C5 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3755 / 343845 wR2 = 0.3389 before cycle 2 for 4591 data and 276 / 276 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0695 * P )^2 + 9.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.77012 0.00386 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U13 O35A Max. shift = 0.000 A for N41 Max. dU = 0.000 for H23 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3755 / 343845 wR2 = 0.3389 before cycle 3 for 4591 data and 276 / 276 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0695 * P )^2 + 9.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.77012 0.00386 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C44 Max. shift = 0.000 A for H44 Max. dU = 0.000 for H23 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3755 / 343845 wR2 = 0.3389 before cycle 4 for 4591 data and 276 / 276 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0695 * P )^2 + 9.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.77012 0.00386 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O35B Max. shift = 0.000 A for C44 Max. dU = 0.000 for H23 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 H2A 0.6002 0.7388 0.7197 23 0.990 0.000 C2 C1 C3 H2B 0.4818 0.6175 0.7128 23 0.990 0.000 C2 C1 C3 H3A 0.6761 0.4711 0.6080 23 0.990 0.000 C3 C2 C4 H3B 0.8015 0.5874 0.6177 23 0.990 0.000 C3 C2 C4 H4A 0.4716 0.6680 0.5397 23 0.990 0.000 C4 C5 C3 H4B 0.6075 0.7748 0.5423 23 0.990 0.000 C4 C5 C3 H1 0.5352 0.6834 0.8773 147 0.840 0.000 O1A C1 H1 H5 0.5195 0.7660 0.3802 147 0.840 0.000 O5B C5 H5 H22 0.9759 0.2656 0.7275 43 0.950 0.000 C22 N23 N21 H24 1.3198 -0.1013 0.6799 43 0.950 0.000 C24 C25 N23 H25 1.2223 -0.0031 0.5244 43 0.950 0.000 C25 C24 N21 H26A 0.8536 0.2570 0.5343 137 0.980 0.000 C26 N21 H26A H26B 1.0090 0.2203 0.4601 137 0.980 0.000 C26 N21 H26A H26C 0.9938 0.3599 0.5319 137 0.980 0.000 C26 N21 H26A H23 1.1607 0.0665 0.8023 43 0.880 0.000 N23 C22 C24 H32A 0.3598 0.7561 1.0429 23 0.990 0.000 C32 C33 C31 H32B 0.4977 0.8603 1.0379 23 0.990 0.000 C32 C33 C31 H33A 0.1721 0.9447 1.1218 23 0.990 0.000 C33 C32 C34 H33B 0.3053 1.0542 1.1134 23 0.990 0.000 C33 C32 C34 H34A 0.3600 0.7815 1.2205 23 0.990 0.000 C34 C35 C33 H34B 0.4907 0.8924 1.2131 23 0.990 0.000 C34 C35 C33 H42 -0.1231 1.4029 1.2741 43 0.950 0.000 C42 N43 N41 H44 0.0584 1.1832 1.0298 43 0.950 0.000 C44 C45 N43 H45 -0.1338 1.4109 0.9859 43 0.950 0.000 C45 C44 N41 H46A -0.2328 1.6757 1.1078 137 0.980 0.000 C46 N41 H46A H46B -0.3208 1.6186 1.2021 137 0.980 0.000 C46 N41 H46A H46C -0.3852 1.5880 1.0958 137 0.980 0.000 C46 N41 H46A H43 0.0614 1.1900 1.2129 43 0.880 0.000 N43 C42 C44 06skc0047p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.67837 0.55538 0.80464 1.00000 0.03448 0.02156 0.02152 -0.00612 0.00137 0.00030 0.02650 0.01080 0.00085 0.00071 0.00047 0.00000 0.00363 0.00323 0.00335 0.00256 0.00270 0.00281 0.00144 C2 0.60001 0.63078 0.71417 1.00000 0.03045 0.02661 0.02640 -0.00399 -0.00071 -0.00364 0.02798 0.01109 0.00085 0.00076 0.00048 0.00000 0.00349 0.00340 0.00352 0.00269 0.00272 0.00278 0.00145 H2A 0.60016 0.73884 0.71974 1.00000 0.03358 0.00000 0.00000 H2B 0.48182 0.61746 0.71276 1.00000 0.03358 0.00000 0.00000 C3 0.68217 0.57741 0.61753 1.00000 0.02710 0.01318 0.01932 -0.00101 -0.00224 0.00474 0.02086 0.01016 0.00078 0.00064 0.00043 0.00000 0.00317 0.00271 0.00305 0.00228 0.00244 0.00237 0.00129 H3A 0.67607 0.47110 0.60796 1.00000 0.02503 0.00000 0.00000 H3B 0.80147 0.58739 0.61767 1.00000 0.02503 0.00000 0.00000 C4 0.59280 0.67015 0.53452 1.00000 0.03088 0.02293 0.02204 0.00564 -0.00678 -0.00329 0.02542 0.01079 0.00083 0.00072 0.00045 0.00000 0.00343 0.00320 0.00333 0.00258 0.00266 0.00273 0.00141 H4A 0.47164 0.66803 0.53974 1.00000 0.03050 0.00000 0.00000 H4B 0.60754 0.77478 0.54231 1.00000 0.03050 0.00000 0.00000 C5 0.65480 0.61699 0.43388 1.00000 0.02757 0.02507 0.01944 -0.00330 -0.00611 -0.00181 0.02431 0.01002 0.00080 0.00071 0.00045 0.00000 0.00326 0.00329 0.00318 0.00256 0.00254 0.00271 0.00138 O1A 0.60993 0.60928 0.88826 1.00000 0.03955 0.03764 0.01589 -0.00622 0.00141 0.00134 0.03203 0.00802 0.00062 0.00056 0.00032 0.00000 0.00284 0.00286 0.00226 0.00196 0.00194 0.00220 0.00114 H1 0.53518 0.68337 0.87727 1.00000 0.04804 0.00000 0.00000 O1B 0.79033 0.44940 0.80132 1.00000 0.03202 0.02918 0.01880 -0.00296 0.00157 0.00091 0.02745 0.00743 0.00056 0.00050 0.00031 0.00000 0.00253 0.00250 0.00231 0.00188 0.00189 0.00207 0.00106 O5A 0.76562 0.50343 0.42082 1.00000 0.03198 0.03181 0.02163 -0.00537 -0.00006 0.00668 0.02997 0.00774 0.00058 0.00052 0.00033 0.00000 0.00250 0.00257 0.00238 0.00194 0.00190 0.00206 0.00110 O5B 0.58638 0.69087 0.36037 1.00000 0.03747 0.02916 0.01953 0.00096 -0.00144 0.00804 0.03042 0.00803 0.00060 0.00053 0.00032 0.00000 0.00275 0.00256 0.00232 0.00190 0.00195 0.00209 0.00112 H5 0.51947 0.76602 0.38022 1.00000 0.04562 0.00000 0.00000 C22 1.04839 0.18650 0.69577 1.00000 0.02780 0.02359 0.02431 -0.00876 0.00075 -0.00352 0.02535 0.01023 0.00081 0.00072 0.00047 0.00000 0.00334 0.00324 0.00335 0.00263 0.00262 0.00270 0.00140 H22 0.97587 0.26562 0.72745 1.00000 0.03042 0.00000 0.00000 C24 1.23758 -0.01526 0.66892 1.00000 0.03296 0.03666 0.03912 0.00402 0.00336 -0.00493 0.03645 0.01275 0.00093 0.00086 0.00056 0.00000 0.00383 0.00405 0.00435 0.00332 0.00318 0.00320 0.00171 H24 1.31981 -0.10131 0.67989 1.00000 0.04374 0.00000 0.00000 C25 1.18422 0.03903 0.58555 1.00000 0.03024 0.02946 0.04423 0.00574 -0.00971 -0.00354 0.03478 0.01215 0.00089 0.00079 0.00059 0.00000 0.00366 0.00372 0.00443 0.00321 0.00317 0.00302 0.00167 H25 1.22234 -0.00311 0.52440 1.00000 0.04174 0.00000 0.00000 C26 0.97323 0.25789 0.52520 1.00000 0.02810 0.03190 0.05363 0.00629 -0.01090 0.00804 0.03942 0.01329 0.00090 0.00083 0.00061 0.00000 0.00367 0.00391 0.00501 0.00351 0.00337 0.00310 0.00186 H26A 0.85362 0.25695 0.53433 1.00000 0.05914 0.00000 0.00000 H26B 1.00899 0.22032 0.46015 1.00000 0.05914 0.00000 0.00000 H26C 0.99375 0.35993 0.53187 1.00000 0.05914 0.00000 0.00000 N21 1.06543 0.16537 0.59692 1.00000 0.02584 0.02825 0.03182 0.00564 -0.00597 -0.00414 0.02868 0.00932 0.00069 0.00063 0.00042 0.00000 0.00283 0.00295 0.00316 0.00242 0.00234 0.00235 0.00127 N23 1.14999 0.07808 0.73899 1.00000 0.03950 0.04033 0.02687 -0.00929 0.00370 -0.01015 0.03521 0.00972 0.00076 0.00069 0.00045 0.00000 0.00346 0.00359 0.00338 0.00267 0.00260 0.00285 0.00144 H23 1.16074 0.06653 0.80234 1.00000 0.03893 0.00000 0.02264 C31 0.31731 0.91241 0.93317 1.00000 0.02158 0.02791 0.01075 -0.00726 0.00263 -0.00820 0.01962 0.00934 0.00074 0.00069 0.00041 0.00000 0.00293 0.00330 0.00275 0.00238 0.00222 0.00261 0.00126 C32 0.37601 0.86042 1.03488 1.00000 0.03027 0.02572 0.01266 -0.00285 0.00256 -0.00307 0.02313 0.01030 0.00081 0.00071 0.00042 0.00000 0.00333 0.00328 0.00289 0.00244 0.00243 0.00268 0.00134 H32A 0.35980 0.75609 1.04291 1.00000 0.02776 0.00000 0.00000 H32B 0.49766 0.86027 1.03787 1.00000 0.02776 0.00000 0.00000 C33 0.29299 0.94879 1.12066 1.00000 0.02663 0.01313 0.01477 0.00006 -0.00056 0.00464 0.01917 0.01000 0.00077 0.00063 0.00041 0.00000 0.00307 0.00269 0.00286 0.00218 0.00231 0.00231 0.00124 H33A 0.17209 0.94469 1.12178 1.00000 0.02301 0.00000 0.00000 H33B 0.30535 1.05424 1.11344 1.00000 0.02301 0.00000 0.00000 C34 0.37001 0.88779 1.21587 1.00000 0.03038 0.01963 0.01185 0.00401 0.00063 -0.00109 0.02105 0.01034 0.00080 0.00067 0.00041 0.00000 0.00328 0.00298 0.00280 0.00226 0.00237 0.00255 0.00129 H34A 0.36003 0.78148 1.22054 1.00000 0.02526 0.00000 0.00000 H34B 0.49075 0.89244 1.21314 1.00000 0.02526 0.00000 0.00000 C35 0.29707 0.96436 1.30769 1.00000 0.03140 0.02755 0.01624 0.00462 0.00080 -0.01209 0.02425 0.01035 0.00081 0.00072 0.00044 0.00000 0.00349 0.00341 0.00306 0.00253 0.00255 0.00286 0.00138 O31A 0.38210 0.83074 0.86278 1.00000 0.03465 0.03125 0.01805 -0.00151 0.00286 -0.00228 0.02845 0.00757 0.00058 0.00052 0.00031 0.00000 0.00256 0.00253 0.00228 0.00191 0.00189 0.00205 0.00107 O31B 0.21278 1.02717 0.92524 1.00000 0.03736 0.03274 0.01760 0.00568 -0.00357 -0.00054 0.02991 0.00779 0.00059 0.00052 0.00032 0.00000 0.00267 0.00262 0.00229 0.00191 0.00193 0.00218 0.00110 O35A 0.35869 0.90706 1.38734 1.00000 0.03793 0.04048 0.00819 -0.00244 0.00225 0.00268 0.03006 0.00774 0.00059 0.00054 0.00030 0.00000 0.00265 0.00278 0.00207 0.00188 0.00181 0.00218 0.00112 O35B 0.18337 1.07657 1.30635 1.00000 0.03294 0.02799 0.01887 -0.00010 0.00105 0.00189 0.02751 0.00749 0.00057 0.00050 0.00031 0.00000 0.00253 0.00244 0.00233 0.00186 0.00188 0.00205 0.00106 C42 -0.10069 1.37632 1.20781 1.00000 0.03062 0.03749 0.01756 0.01045 -0.00423 -0.01257 0.02775 0.01102 0.00083 0.00078 0.00047 0.00000 0.00348 0.00384 0.00315 0.00278 0.00261 0.00299 0.00148 H42 -0.12309 1.40292 1.27409 1.00000 0.03330 0.00000 0.00000 C44 -0.00117 1.25581 1.07279 1.00000 0.02764 0.02769 0.04060 0.00946 -0.00432 0.00181 0.03278 0.01226 0.00085 0.00079 0.00055 0.00000 0.00349 0.00358 0.00428 0.00307 0.00301 0.00289 0.00162 H44 0.05835 1.18323 1.02982 1.00000 0.03934 0.00000 0.00000 C45 -0.10605 1.37929 1.05051 1.00000 0.03252 0.02649 0.04272 -0.00361 0.00250 -0.00117 0.03443 0.01225 0.00089 0.00078 0.00059 0.00000 0.00373 0.00357 0.00439 0.00312 0.00317 0.00295 0.00165 H45 -0.13383 1.41092 0.98592 1.00000 0.04131 0.00000 0.00000 C46 -0.28664 1.59595 1.13433 1.00000 0.04230 0.04112 0.03998 -0.00141 0.00357 0.00083 0.04218 0.01404 0.00101 0.00089 0.00060 0.00000 0.00440 0.00445 0.00448 0.00352 0.00351 0.00357 0.00189 H46A -0.23282 1.67569 1.10781 1.00000 0.06326 0.00000 0.00000 H46B -0.32077 1.61861 1.20211 1.00000 0.06326 0.00000 0.00000 H46C -0.38525 1.58804 1.09584 1.00000 0.06326 0.00000 0.00000 N41 -0.16771 1.45356 1.13016 1.00000 0.03171 0.03002 0.03330 0.00750 -0.00471 -0.00624 0.03156 0.00966 0.00072 0.00064 0.00044 0.00000 0.00312 0.00314 0.00330 0.00253 0.00252 0.00255 0.00134 N43 0.00121 1.25763 1.17601 1.00000 0.03584 0.02871 0.02498 0.00569 -0.00133 0.00102 0.03067 0.00972 0.00073 0.00064 0.00041 0.00000 0.00318 0.00303 0.00297 0.00236 0.00242 0.00252 0.00132 H43 0.06137 1.19001 1.21288 1.00000 0.03681 0.00000 0.00000 Final Structure Factor Calculation for 06skc0047p-1 in P-1 Total number of l.s. parameters = 276 Maximum vector length = 511 Memory required = 3479 / 22995 wR2 = 0.3389 before cycle 5 for 4591 data and 0 / 276 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0695 * P )^2 + 9.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1381 for 2970 Fo > 4sig(Fo) and 0.1929 for all 4591 data wR2 = 0.3389, GooF = S = 1.094, Restrained GooF = 1.094 for all data Occupancy sum of asymmetric unit = 30.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0375 0.0270 0.0149 C1 0.0322 0.0292 0.0225 C2 0.0331 0.0189 0.0105 C3 0.0342 0.0267 0.0154 C4 0.0336 0.0236 0.0157 C5 0.0489 0.0332 0.0140 O1A 0.0385 0.0264 0.0175 O1B 0.0474 0.0249 0.0176 O5A 0.0509 0.0217 0.0187 O5B 0.0328 0.0281 0.0152 C22 0.0443 0.0343 0.0308 C24 0.0491 0.0317 0.0235 C25 0.0571 0.0459 0.0152 C26 0.0370 0.0279 0.0211 N21 0.0469 0.0366 0.0221 N23 0.0317 0.0190 0.0081 C31 0.0315 0.0261 0.0117 C32 0.0322 0.0148 0.0105 C33 0.0324 0.0206 0.0101 C34 0.0357 0.0238 0.0132 C35 0.0379 0.0301 0.0173 O31A 0.0424 0.0323 0.0150 O31B 0.0510 0.0314 0.0078 O35A 0.0398 0.0240 0.0187 O35B 0.0444 0.0258 0.0131 C42 0.0458 0.0343 0.0183 C44 0.0438 0.0354 0.0241 C45 0.0522 0.0413 0.0330 C46 0.0403 0.0306 0.0237 N41 0.0419 0.0301 0.0200 N43 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.018 0.027 0.037 0.049 0.064 0.081 0.108 0.154 1.000 Number in group 490. 464. 441. 456. 470. 460. 433. 462. 453. 462. GooF 1.347 1.161 1.096 1.089 0.969 1.110 0.979 1.035 0.962 1.113 K 34.804 5.464 2.540 1.858 1.351 1.241 1.079 1.095 0.997 0.989 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.64 inf Number in group 468. 454. 456. 473. 448. 461. 458. 460. 455. 458. GooF 0.908 0.839 0.863 0.876 1.029 0.991 1.071 1.089 1.390 1.627 K 1.060 1.248 1.206 1.244 1.108 1.084 1.059 1.014 1.020 1.026 R1 0.400 0.373 0.295 0.284 0.239 0.161 0.153 0.132 0.139 0.105 Recommended weighting scheme: WGHT 0.0695 9.7573 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 4 5 451.48 113.35 5.99 0.092 1.65 3 -3 5 258.51 15.23 5.95 0.034 1.53 0 4 1 300.71 50.37 5.90 0.062 2.22 3 -2 3 182.92 0.62 5.61 0.007 1.94 1 -8 7 221.55 11.90 5.58 0.030 0.95 3 -6 7 319.83 39.32 5.58 0.054 1.04 1 4 3 158.46 5.83 5.45 0.021 2.04 1 -5 5 291.03 52.94 5.25 0.063 1.44 -1 1 12 126.42 3.23 5.11 0.016 1.12 1 5 7 115.70 0.70 5.06 0.007 1.34 -1 -6 3 180.32 0.01 5.04 0.001 1.44 2 -5 1 224.68 35.27 4.99 0.052 1.53 1 -1 2 545.47 220.11 4.83 0.129 4.32 2 -5 6 216.09 41.18 4.82 0.056 1.28 1 -7 9 166.46 17.25 4.72 0.036 0.96 -1 7 6 363.96 118.46 4.63 0.094 1.09 -1 3 7 289.97 80.83 4.56 0.078 1.58 -1 -3 11 153.28 7.87 4.49 0.024 1.15 -1 -9 5 113.15 0.08 4.37 0.002 0.95 -2 1 5 2157.40 1292.26 4.31 0.312 2.13 -2 0 6 127.05 2.51 4.28 0.014 1.98 0 2 8 90.12 4.40 4.15 0.018 1.60 -3 0 3 341.78 122.32 4.09 0.096 2.29 2 -1 2 71.22 1.33 4.04 0.010 3.09 1 -7 5 224.50 63.13 4.03 0.069 1.13 -3 7 6 73.40 0.56 4.01 0.007 0.98 0 -7 6 87.48 1.01 4.01 0.009 1.12 -1 4 1 556.68 266.68 3.99 0.142 2.05 -1 1 7 289.07 100.81 3.95 0.087 1.84 2 -4 3 187.98 46.62 3.93 0.059 1.70 -1 3 3 113.16 14.28 3.88 0.033 2.29 -2 8 1 94.97 6.77 3.84 0.023 1.03 0 -4 2 84.41 5.08 3.83 0.020 2.13 0 3 1 58.99 0.01 3.82 0.001 2.93 0 5 5 141.12 31.58 3.76 0.049 1.50 2 -2 6 62.44 0.99 3.69 0.009 1.77 -3 6 3 62.51 0.74 3.66 0.007 1.17 -1 -3 4 66.41 0.73 3.66 0.007 2.25 -2 5 4 240.36 84.08 3.60 0.080 1.40 0 1 4 79.95 9.14 3.52 0.026 3.21 0 -2 3 78.89 4.93 3.51 0.019 3.20 1 -1 6 4772.02 3347.06 3.51 0.502 2.12 2 -3 1 744.15 391.41 3.48 0.172 2.19 -1 7 8 73.23 0.10 3.47 0.003 1.00 2 -7 5 56.38 0.43 3.46 0.006 1.07 -1 4 4 60.02 3.32 3.41 0.016 1.77 -2 5 3 158.44 44.33 3.41 0.058 1.46 -2 -1 1 482.25 246.45 3.39 0.136 3.76 1 -1 4 91.67 15.47 3.33 0.034 2.93 0 -7 1 126.52 30.12 3.33 0.048 1.28 Bond lengths and angles C1 - Distance Angles O1B 1.2054 (0.0075) O1A 1.3267 (0.0076) 122.06 (0.60) C2 1.5119 (0.0092) 122.53 (0.58) 115.33 (0.55) C1 - O1B O1A C2 - Distance Angles C1 1.5119 (0.0093) C3 1.5199 (0.0086) 116.50 (0.54) H2A 0.9900 108.17 108.17 H2B 0.9900 108.17 108.17 107.33 C2 - C1 C3 H2A C3 - Distance Angles C2 1.5199 (0.0086) C4 1.5309 (0.0080) 109.59 (0.50) H3A 0.9900 109.75 109.75 H3B 0.9900 109.75 109.75 108.22 C3 - C2 C4 H3A C4 - Distance Angles C5 1.5164 (0.0088) C3 1.5309 (0.0080) 113.94 (0.52) H4A 0.9900 108.77 108.77 H4B 0.9900 108.77 108.77 107.66 C4 - C5 C3 H4A C5 - Distance Angles O5A 1.2585 (0.0076) O5B 1.2892 (0.0075) 120.25 (0.58) C4 1.5164 (0.0088) 122.36 (0.56) 117.37 (0.54) C5 - O5A O5B O1A - Distance Angles C1 1.3267 (0.0076) H1 0.8400 109.47 O1A - C1 O1B - Distance Angles C1 1.2054 (0.0075) O1B - O5A - Distance Angles C5 1.2585 (0.0075) O5A - O5B - Distance Angles C5 1.2892 (0.0075) H5 0.8400 109.47 O5B - C5 C22 - Distance Angles N23 1.3169 (0.0089) N21 1.3740 (0.0086) 108.16 (0.56) H22 0.9500 125.92 125.92 C22 - N23 N21 C24 - Distance Angles C25 1.2959 (0.0105) N23 1.3896 (0.0096) 105.99 (0.69) H24 0.9500 127.01 127.01 C24 - C25 N23 C25 - Distance Angles C24 1.2959 (0.0105) N21 1.3744 (0.0090) 111.34 (0.74) H25 0.9500 124.33 124.33 C25 - C24 N21 C26 - Distance Angles N21 1.4271 (0.0087) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - N21 H26A H26B N21 - Distance Angles C22 1.3740 (0.0086) C25 1.3744 (0.0090) 105.16 (0.58) C26 1.4271 (0.0087) 125.08 (0.61) 129.75 (0.66) N21 - C22 C25 N23 - Distance Angles C22 1.3169 (0.0089) C24 1.3896 (0.0096) 109.35 (0.61) H23 0.8800 125.33 125.33 N23 - C22 C24 C31 - Distance Angles O31B 1.2319 (0.0076) O31A 1.2728 (0.0071) 125.28 (0.56) C32 1.5295 (0.0082) 118.78 (0.50) 115.94 (0.53) C31 - O31B O31A C32 - Distance Angles C33 1.5121 (0.0079) C31 1.5295 (0.0082) 117.38 (0.51) H32A 0.9900 107.96 107.96 H32B 0.9900 107.96 107.96 107.22 C32 - C33 C31 H32A C33 - Distance Angles C32 1.5121 (0.0079) C34 1.5190 (0.0078) 111.06 (0.48) H33A 0.9900 109.42 109.42 H33B 0.9900 109.42 109.42 108.03 C33 - C32 C34 H33A C34 - Distance Angles C35 1.5064 (0.0085) C33 1.5190 (0.0077) 116.66 (0.51) H34A 0.9900 108.13 108.13 H34B 0.9900 108.13 108.13 107.31 C34 - C35 C33 H34A C35 - Distance Angles O35B 1.2524 (0.0077) O35A 1.2808 (0.0075) 122.11 (0.58) C34 1.5064 (0.0085) 122.25 (0.54) 115.65 (0.56) C35 - O35B O35A O31A - Distance Angles C31 1.2728 (0.0071) O31A - O31B - Distance Angles C31 1.2319 (0.0076) O31B - O35A - Distance Angles C35 1.2808 (0.0075) O35A - O35B - Distance Angles C35 1.2524 (0.0078) O35B - C42 - Distance Angles N43 1.3137 (0.0089) N41 1.3442 (0.0084) 108.05 (0.60) H42 0.9500 125.98 125.98 C42 - N43 N41 C44 - Distance Angles C45 1.3249 (0.0095) N43 1.4188 (0.0094) 103.60 (0.65) H44 0.9500 128.20 128.20 C44 - C45 N43 C45 - Distance Angles C44 1.3249 (0.0095) N41 1.3332 (0.0094) 111.47 (0.72) H45 0.9500 124.26 124.26 C45 - C44 N41 C46 - Distance Angles N41 1.4768 (0.0093) H46A 0.9800 109.47 H46B 0.9800 109.47 109.47 H46C 0.9800 109.47 109.47 109.47 C46 - N41 H46A H46B N41 - Distance Angles C45 1.3332 (0.0094) C42 1.3442 (0.0084) 107.71 (0.61) C46 1.4768 (0.0093) 127.06 (0.63) 125.22 (0.64) N41 - C45 C42 N43 - Distance Angles C42 1.3137 (0.0089) C44 1.4188 (0.0094) 109.16 (0.55) H43 0.8800 125.42 125.42 N43 - C42 C44 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.68 2.515(7) 176.3 O1A-H1...O31A 0.88 1.84 2.705(7) 169.4 N43-H43...O35B 0.88 1.77 2.640(8) 171.2 N23-H23...O31B_$1 0.84 1.67 2.480(6) 162.3 O5B-H5...O35A_$2 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 6.4266 (0.0336) x + 6.7609 (0.0491) y + 0.9019 (0.1519) z = 8.8402 (0.1233) * 0.0000 (0.0001) O1A * 0.0000 (0.0001) O1B * 0.0000 (0.0000) C1 Rms deviation of fitted atoms = 0.0000 6.6654 (0.0259) x + 6.4700 (0.0347) y + 0.2990 (0.1551) z = 8.4862 (0.0647) Angle to previous plane (with approximate esd) = 3.73 ( 0.81 ) * 0.0000 (0.0000) O5A * 0.0000 (0.0000) O5B * 0.0000 (0.0000) C5 Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 1 21 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.1928 for 4591 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.17 at 0.1811 0.5514 0.7553 [ 0.70 A from H42 ] Deepest hole -0.61 at 0.0334 0.1674 0.2056 [ 0.35 A from H43 ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 3388 / 22503 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.1811 1.4486 1.2447 1.00000 0.05 1.17 0.70 H42 0.98 C42 1.58 N41 1.85 H46B Q2 1 0.9898 0.2504 0.6660 1.00000 0.05 0.69 0.80 C22 0.86 H22 1.30 N21 1.94 C26 Q3 1 0.8310 0.4472 0.4474 1.00000 0.05 0.67 0.77 O5A 1.84 H26C 1.93 C5 2.09 H26A Q4 1 0.4620 0.8402 0.3954 1.00000 0.05 0.66 0.78 H5 0.95 O35A 1.62 O5B 2.01 C35 Q5 1 1.1184 0.1450 0.5188 1.00000 0.05 0.64 1.15 N21 1.31 H26B 1.37 C25 1.42 C26 Q6 1 0.6730 0.6171 0.3596 1.00000 0.05 0.62 0.88 O5B 1.03 C5 1.44 O5A 1.70 H5 Q7 1 1.1580 0.0660 0.6558 1.00000 0.05 0.60 0.91 C24 1.01 C25 1.15 N23 1.35 N21 Q8 1 0.5038 0.7744 0.8633 1.00000 0.05 0.55 0.85 H1 1.03 O31A 1.64 O1A 2.02 C31 Q9 1 0.5447 0.7243 0.7255 1.00000 0.05 0.54 0.50 H2A 0.90 C2 1.19 H2B 2.04 C1 Q10 1 -0.0791 1.3596 1.1007 1.00000 0.05 0.52 0.74 C45 1.09 N41 1.11 C44 1.47 N43 Shortest distances between peaks (including symmetry equivalents) 8 9 1.96 2 7 1.98 5 7 2.02 3 6 2.20 1 10 2.23 1 6 2.36 2 5 2.39 4 6 2.47 1 3 2.79 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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. 0.83: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.92: Structure factors and derivatives 2.23: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.23: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.13: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0047p-1 finished at 15:25:09 Total CPU time: 4.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++