+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0070p212121 started at 14:36:31 on 06-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0070p212121 in P2(1)2(1)2(1) CELL 0.71073 7.0493 11.3995 16.4313 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0005 0.0009 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 S UNIT 52 64 8 12 4 V = 1320.39 F(000) = 592.0 Mu = 0.25 mm-1 Cell Wt = 1121.35 Rho = 1.410 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.01 0.17 0.18 ACTA HTAB N21 O1B EQIV_$1 -x+1/2, -y+2, z+1/2 HTAB N4 O1C_$1 HTAB N4 S1_$1 EQIV_$2 x-1/2, -y+3/2, -z+1 HTAB N4 O1A_$2 EQIV_$3 -x+1, y-1/2, -z+1/2 HTAB N21 O1A_$3 EQIV_$4 -x, y-1/2, -z+1/2 HTAB N21 O1C_$4 BOND $H WGHT 0.03510 5.33270 L.S. 4 TEMP -153.00 FVAR 0.38029 MOLE 1 C1 1 0.238049 0.887071 0.409632 11.00000 0.01392 0.00882 = 0.01269 0.00057 0.00116 -0.00248 C2 1 0.297453 0.970498 0.465088 11.00000 0.02101 0.00959 = 0.02736 -0.00203 0.00193 0.00034 AFIX 43 H2 2 0.356237 1.040692 0.446779 11.00000 -1.20000 AFIX 0 C3 1 0.270638 0.951061 0.547930 11.00000 0.01760 0.01723 = 0.01967 -0.01033 0.00331 -0.00395 AFIX 43 H3 2 0.311739 1.008400 0.586001 11.00000 -1.20000 AFIX 0 C4 1 0.184603 0.848977 0.575719 11.00000 0.01324 0.02055 = 0.01668 0.00384 0.00399 0.00156 C5 1 0.126508 0.765195 0.518280 11.00000 0.01130 0.01349 = 0.02984 0.00313 0.00352 -0.00399 AFIX 43 H5 2 0.069262 0.694274 0.536132 11.00000 -1.20000 AFIX 0 C6 1 0.151611 0.784760 0.436661 11.00000 0.01439 0.01436 = 0.02240 -0.00283 0.00022 -0.00406 AFIX 43 H6 2 0.109622 0.727986 0.398361 11.00000 -1.20000 AFIX 0 N4 3 0.152272 0.829786 0.656888 11.00000 0.04268 0.02759 = 0.01687 -0.00205 0.00446 -0.01443 AFIX 93 H4A 2 0.186260 0.882864 0.692939 11.00000 -1.20000 H4B 2 0.097525 0.764387 0.672951 11.00000 -1.20000 AFIX 0 O1A 4 0.471855 0.929426 0.291287 11.00000 0.01633 0.03104 = 0.02857 -0.00460 0.00310 -0.00008 O1B 4 0.202489 0.804424 0.264269 11.00000 0.03089 0.02190 = 0.02446 -0.00115 -0.00380 -0.00501 O1C 4 0.155585 1.012432 0.282150 11.00000 0.02906 0.02593 = 0.02272 0.00523 0.00649 0.00858 S1 5 0.268528 0.909681 0.304317 11.00000 0.01387 0.01782 = 0.01589 -0.00169 0.00031 0.00220 MOLE 2 C21 1 0.250389 0.607654 0.106874 11.00000 0.01337 0.01970 = 0.02123 0.00063 0.00257 -0.00095 C22 1 0.194285 0.522235 0.051852 11.00000 0.01719 0.00907 = 0.03413 0.00243 0.00592 -0.00146 AFIX 43 H22 2 0.141728 0.450426 0.070624 11.00000 -1.20000 AFIX 0 C23 1 0.215528 0.542527 -0.030525 11.00000 0.01681 0.01681 = 0.02913 -0.00640 0.00275 0.00114 AFIX 43 H23 2 0.179316 0.483589 -0.068334 11.00000 -1.20000 AFIX 0 C24 1 0.289474 0.648450 -0.058966 11.00000 0.00895 0.02776 = 0.01672 -0.00095 0.00299 0.00587 C25 1 0.347471 0.731031 -0.001865 11.00000 0.02018 0.01426 = 0.02634 0.00375 0.00328 0.00358 AFIX 43 H25 2 0.402681 0.802404 -0.020027 11.00000 -1.20000 AFIX 0 C26 1 0.326666 0.711696 0.080729 11.00000 0.00890 0.01072 = 0.03066 -0.00440 0.00593 0.00197 AFIX 43 H26 2 0.364722 0.769740 0.118868 11.00000 -1.20000 AFIX 0 C27 1 0.311284 0.673248 -0.148777 11.00000 0.03035 0.03536 = 0.02702 0.00588 -0.00042 -0.00927 AFIX 137 H27A 2 0.313032 0.758231 -0.157753 11.00000 -1.50000 H27B 2 0.204594 0.638576 -0.178501 11.00000 -1.50000 H27C 2 0.430377 0.639027 -0.168349 11.00000 -1.50000 AFIX 0 N21 3 0.226867 0.583458 0.194890 11.00000 0.02253 0.01783 = 0.02289 0.00376 0.00335 -0.00239 AFIX 137 H21A 2 0.325694 0.539048 0.212787 11.00000 -1.50000 H21B 2 0.116247 0.544070 0.203150 11.00000 -1.50000 H21C 2 0.224214 0.652394 0.222793 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0070p212121 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - C2 C6 S1 C2 - C1 C3 C3 - C4 C2 C4 - N4 C3 C5 C5 - C6 C4 C6 - C5 C1 N4 - C4 O1A - S1 O1B - S1 O1C - S1 S1 - O1B O1C O1A C1 C21 - C26 C22 N21 C22 - C23 C21 C23 - C22 C24 C24 - C25 C23 C27 C25 - C26 C24 C26 - C21 C25 C27 - C24 N21 - C21 Operators for generating equivalent atoms: $1 -x+1/2, -y+2, z+1/2 $2 x-1/2, -y+3/2, -z+1 $3 -x+1, y-1/2, -z+1/2 $4 -x, y-1/2, -z+1/2 h k l Fo^2 Sigma Why rejected 0 7 0 12.62 2.17 observed but should be systematically absent 13321 Reflections read, of which 78 rejected -9 =< h =< 9, -14 =< k =< 14, -21 =< l =< 21, Max. 2-theta = 54.94 1 Systematic absence violations 0 Inconsistent equivalents 3016 Unique reflections, of which 0 suppressed R(int) = 0.0957 R(sigma) = 0.0905 Friedel opposites not merged Maximum memory for data reduction = 2112 / 30162 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 = 2610 / 217418 wR2 = 0.1764 before cycle 1 for 3016 data and 174 / 174 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0351 * P )^2 + 5.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38031 0.00120 0.013 OSF Mean shift/esd = 0.003 Maximum = 0.015 for x N4 Max. shift = 0.000 A for H27A Max. dU = 0.000 for O1A Least-squares cycle 2 Maximum vector length = 511 Memory required = 2610 / 217418 wR2 = 0.1764 before cycle 2 for 3016 data and 174 / 174 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0351 * P )^2 + 5.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38031 0.00120 0.006 OSF Mean shift/esd = 0.001 Maximum = 0.006 for OSF Max. shift = 0.000 A for H27A Max. dU = 0.000 for O1A Least-squares cycle 3 Maximum vector length = 511 Memory required = 2610 / 217418 wR2 = 0.1764 before cycle 3 for 3016 data and 174 / 174 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0351 * P )^2 + 5.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38031 0.00120 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U33 C27 Max. shift = 0.000 A for H27A Max. dU = 0.000 for C27 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2610 / 217418 wR2 = 0.1764 before cycle 4 for 3016 data and 174 / 174 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0351 * P )^2 + 5.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38031 0.00120 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U33 C27 Max. shift = 0.000 A for H27A Max. dU = 0.000 for C22 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 H2 0.3562 1.0407 0.4468 43 0.950 0.000 C2 C1 C3 H3 0.3118 1.0084 0.5860 43 0.950 0.000 C3 C4 C2 H5 0.0693 0.6943 0.5361 43 0.950 0.000 C5 C6 C4 H6 0.1096 0.7280 0.3984 43 0.950 0.000 C6 C5 C1 H4A 0.1863 0.8829 0.6929 93 0.880 0.000 N4 C4 C3 H4B 0.0975 0.7644 0.6730 93 0.880 0.000 N4 C4 C3 H22 0.1417 0.4504 0.0706 43 0.950 0.000 C22 C23 C21 H23 0.1793 0.4836 -0.0683 43 0.950 0.000 C23 C22 C24 H25 0.4027 0.8024 -0.0200 43 0.950 0.000 C25 C26 C24 H26 0.3647 0.7697 0.1189 43 0.950 0.000 C26 C21 C25 H27A 0.3129 0.7582 -0.1578 137 0.980 0.000 C27 C24 H27A H27B 0.2046 0.6385 -0.1785 137 0.980 0.000 C27 C24 H27A H27C 0.4304 0.6391 -0.1684 137 0.980 0.000 C27 C24 H27A H21A 0.3257 0.5390 0.2128 137 0.910 0.000 N21 C21 H21A H21B 0.1162 0.5441 0.2031 137 0.910 0.000 N21 C21 H21A H21C 0.2242 0.6524 0.2228 137 0.910 0.000 N21 C21 H21A 06skc0070p212121 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.23805 0.88707 0.40963 1.00000 0.01391 0.00884 0.01269 0.00057 0.00116 -0.00248 0.01181 0.00766 0.00071 0.00035 0.00026 0.00000 0.00235 0.00205 0.00196 0.00155 0.00198 0.00203 0.00091 C2 0.29746 0.97050 0.46509 1.00000 0.02100 0.00959 0.02738 -0.00202 0.00194 0.00035 0.01932 0.00907 0.00080 0.00041 0.00032 0.00000 0.00290 0.00224 0.00269 0.00197 0.00226 0.00205 0.00114 H2 0.35624 1.04070 0.44678 1.00000 0.02319 0.00000 0.00000 C3 0.27065 0.95106 0.54793 1.00000 0.01758 0.01724 0.01967 -0.01033 0.00332 -0.00396 0.01816 0.00868 0.00079 0.00041 0.00029 0.00000 0.00277 0.00221 0.00222 0.00182 0.00224 0.00218 0.00106 H3 0.31177 1.00839 0.58600 1.00000 0.02180 0.00000 0.00000 C4 0.18461 0.84898 0.57572 1.00000 0.01324 0.02054 0.01669 0.00384 0.00399 0.00156 0.01682 0.00913 0.00071 0.00045 0.00030 0.00000 0.00255 0.00252 0.00242 0.00198 0.00199 0.00203 0.00109 C5 0.12651 0.76520 0.51828 1.00000 0.01129 0.01348 0.02985 0.00313 0.00352 -0.00398 0.01821 0.00914 0.00077 0.00044 0.00032 0.00000 0.00240 0.00247 0.00292 0.00216 0.00227 0.00204 0.00111 H5 0.06926 0.69428 0.53613 1.00000 0.02185 0.00000 0.00000 C6 0.15162 0.78476 0.43666 1.00000 0.01439 0.01435 0.02240 -0.00284 0.00022 -0.00404 0.01705 0.00880 0.00073 0.00044 0.00031 0.00000 0.00251 0.00243 0.00260 0.00210 0.00213 0.00210 0.00105 H6 0.10964 0.72798 0.39836 1.00000 0.02046 0.00000 0.00000 N4 0.15229 0.82979 0.65689 1.00000 0.04267 0.02759 0.01688 -0.00206 0.00447 -0.01443 0.02905 0.00856 0.00078 0.00043 0.00027 0.00000 0.00332 0.00262 0.00238 0.00191 0.00218 0.00241 0.00124 H4A 0.18629 0.88286 0.69294 1.00000 0.03486 0.00000 0.00000 H4B 0.09753 0.76439 0.67295 1.00000 0.03486 0.00000 0.00000 O1A 0.47186 0.92943 0.29129 1.00000 0.01634 0.03106 0.02858 -0.00461 0.00311 -0.00008 0.02533 0.00635 0.00050 0.00033 0.00023 0.00000 0.00183 0.00208 0.00208 0.00174 0.00161 0.00159 0.00087 O1B 0.20249 0.80442 0.26427 1.00000 0.03091 0.02190 0.02447 -0.00114 -0.00380 -0.00502 0.02576 0.00625 0.00058 0.00030 0.00022 0.00000 0.00238 0.00185 0.00193 0.00150 0.00170 0.00173 0.00092 O1C 0.15558 1.01243 0.28215 1.00000 0.02906 0.02593 0.02274 0.00524 0.00649 0.00859 0.02591 0.00693 0.00057 0.00032 0.00022 0.00000 0.00223 0.00199 0.00202 0.00156 0.00166 0.00169 0.00093 S1 0.26853 0.90968 0.30432 1.00000 0.01388 0.01783 0.01590 -0.00170 0.00031 0.00220 0.01587 0.00207 0.00017 0.00010 0.00007 0.00000 0.00060 0.00052 0.00051 0.00048 0.00050 0.00053 0.00027 C21 0.25038 0.60765 0.10687 1.00000 0.01336 0.01970 0.02124 0.00063 0.00257 -0.00094 0.01810 0.00853 0.00075 0.00041 0.00028 0.00000 0.00250 0.00241 0.00226 0.00183 0.00212 0.00243 0.00101 C22 0.19428 0.52224 0.05185 1.00000 0.01717 0.00908 0.03415 0.00244 0.00591 -0.00146 0.02013 0.00931 0.00076 0.00042 0.00034 0.00000 0.00278 0.00228 0.00288 0.00206 0.00231 0.00194 0.00116 H22 0.14173 0.45043 0.07063 1.00000 0.02416 0.00000 0.00000 C23 0.21552 0.54253 -0.03052 1.00000 0.01680 0.01681 0.02912 -0.00641 0.00274 0.00114 0.02091 0.00933 0.00082 0.00043 0.00032 0.00000 0.00262 0.00235 0.00265 0.00208 0.00235 0.00216 0.00110 H23 0.17930 0.48359 -0.06833 1.00000 0.02509 0.00000 0.00000 C24 0.28947 0.64845 -0.05897 1.00000 0.00895 0.02778 0.01672 -0.00095 0.00298 0.00589 0.01782 0.00892 0.00073 0.00045 0.00029 0.00000 0.00239 0.00265 0.00233 0.00205 0.00204 0.00221 0.00106 C25 0.34746 0.73103 -0.00187 1.00000 0.02016 0.01425 0.02635 0.00376 0.00328 0.00359 0.02026 0.00956 0.00080 0.00045 0.00032 0.00000 0.00287 0.00257 0.00280 0.00210 0.00229 0.00223 0.00117 H25 0.40267 0.80240 -0.02003 1.00000 0.02431 0.00000 0.00000 C26 0.32666 0.71169 0.08073 1.00000 0.00889 0.01073 0.03067 -0.00440 0.00594 0.00196 0.01676 0.00879 0.00066 0.00043 0.00032 0.00000 0.00241 0.00230 0.00286 0.00206 0.00204 0.00187 0.00109 H26 0.36473 0.76974 0.11886 1.00000 0.02011 0.00000 0.00000 C27 0.31127 0.67325 -0.14878 1.00000 0.03034 0.03535 0.02704 0.00588 -0.00042 -0.00925 0.03091 0.01077 0.00093 0.00055 0.00035 0.00000 0.00363 0.00327 0.00302 0.00250 0.00251 0.00271 0.00146 H27A 0.31295 0.75823 -0.15777 1.00000 0.04636 0.00000 0.00000 H27B 0.20461 0.63853 -0.17851 1.00000 0.04636 0.00000 0.00000 H27C 0.43040 0.63906 -0.16835 1.00000 0.04636 0.00000 0.00000 N21 0.22687 0.58346 0.19489 1.00000 0.02253 0.01784 0.02291 0.00375 0.00336 -0.00239 0.02109 0.00720 0.00061 0.00035 0.00024 0.00000 0.00223 0.00189 0.00194 0.00188 0.00217 0.00211 0.00087 H21A 0.32569 0.53905 0.21278 1.00000 0.03164 0.00000 0.00000 H21B 0.11624 0.54407 0.20315 1.00000 0.03164 0.00000 0.00000 H21C 0.22422 0.65239 0.22279 1.00000 0.03164 0.00000 0.00000 Final Structure Factor Calculation for 06skc0070p212121 in P2(1)2(1)2(1) Total number of l.s. parameters = 174 Maximum vector length = 511 Memory required = 2438 / 26068 wR2 = 0.1764 before cycle 5 for 3016 data and 2 / 174 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0351 * P )^2 + 5.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0809 for 2349 Fo > 4sig(Fo) and 0.1076 for all 3016 data wR2 = 0.1764, GooF = S = 1.057, Restrained GooF = 1.057 for all data Flack x parameter = 0.2428 with esd 0.1970 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 Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0152 0.0126 0.0076 C1 0.0281 0.0205 0.0093 C2 0.0308 0.0157 0.0080 C3 0.0241 0.0159 0.0105 C4 0.0308 0.0165 0.0073 C5 0.0236 0.0175 0.0100 C6 0.0521 0.0190 0.0161 N4 0.0348 0.0256 0.0155 O1A 0.0341 0.0247 0.0184 O1B 0.0402 0.0189 0.0186 O1C 0.0194 0.0156 0.0126 S1 0.0221 0.0198 0.0124 C21 0.0361 0.0160 0.0083 C22 0.0321 0.0177 0.0129 C23 0.0295 0.0177 0.0063 C24 0.0294 0.0192 0.0122 C25 0.0328 0.0120 0.0055 C26 0.0439 0.0277 0.0211 C27 0.0263 0.0228 0.0142 N21 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.025 0.033 0.039 0.047 0.057 0.066 0.082 0.107 1.000 Number in group 316. 306. 333. 256. 302. 315. 288. 316. 281. 303. GooF 1.206 1.075 1.090 1.043 1.099 0.970 0.991 1.038 0.999 1.027 K 2.875 1.359 1.175 1.064 1.078 1.036 1.000 1.002 1.003 1.012 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 315. 295. 294. 302. 306. 298. 308. 294. 303. 301. GooF 1.010 1.089 1.058 1.053 1.144 0.990 0.942 0.970 0.991 1.286 K 1.040 1.054 1.083 1.012 1.054 1.035 1.004 1.014 1.008 1.020 R1 0.209 0.211 0.170 0.155 0.141 0.108 0.073 0.060 0.057 0.051 Recommended weighting scheme: WGHT 0.0349 5.3572 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) 4 0 4 54.65 0.19 3.88 0.002 1.62 6 0 0 215.91 21.13 3.80 0.019 1.17 0 5 6 128.33 48.81 3.62 0.028 1.75 7 6 3 173.02 39.63 3.41 0.025 0.88 2 7 0 92.54 22.20 3.38 0.019 1.48 7 1 7 -40.30 70.95 3.32 0.034 0.92 6 7 12 9.77 146.26 3.28 0.049 0.78 5 0 8 107.72 15.48 3.24 0.016 1.16 0 2 2 1373.72 1755.81 3.22 0.169 4.68 -5 6 14 -38.73 64.62 3.18 0.032 0.81 -4 8 8 110.52 0.63 3.15 0.003 0.98 -3 4 2 616.14 432.11 3.14 0.084 1.77 0 12 10 594.79 374.91 3.14 0.078 0.82 1 6 0 48.53 2.40 3.13 0.006 1.83 2 0 2 591.49 412.33 3.11 0.082 3.24 -1 12 1 94.27 14.42 3.11 0.015 0.94 2 0 1 3898.88 4760.78 3.10 0.278 3.45 -9 2 2 -40.64 70.25 3.08 0.034 0.77 1 0 1 89.21 181.30 3.06 0.054 6.48 -3 13 7 90.28 226.43 3.05 0.061 0.78 -3 6 15 242.45 113.94 3.03 0.043 0.88 4 0 18 640.97 406.80 3.02 0.081 0.81 3 6 3 604.78 407.96 2.95 0.081 1.43 6 8 2 247.69 101.45 2.93 0.041 0.90 -3 9 9 666.55 432.35 2.91 0.084 0.95 0 11 7 95.89 30.50 2.88 0.022 0.95 -1 1 1 2043.89 2473.88 2.82 0.200 5.63 0 11 13 74.52 0.73 2.81 0.003 0.80 0 7 9 35.20 0.00 2.79 0.000 1.22 4 1 15 289.13 157.60 2.79 0.051 0.93 3 4 2 584.95 416.75 2.77 0.082 1.77 6 7 6 -9.88 67.07 2.77 0.033 0.90 -2 3 18 67.07 1.62 2.76 0.005 0.86 -2 3 3 87.53 33.89 2.75 0.023 2.34 2 0 12 206.80 108.24 2.73 0.042 1.28 3 3 14 223.37 112.64 2.70 0.043 1.01 -5 5 6 91.34 33.26 2.70 0.023 1.10 1 1 7 1607.23 1312.25 2.68 0.146 2.19 4 10 1 155.58 66.44 2.66 0.033 0.96 0 12 0 215.48 76.35 2.66 0.035 0.95 7 9 4 103.64 277.73 2.65 0.067 0.77 0 6 15 52.03 0.85 2.64 0.004 0.95 9 0 3 82.90 201.06 2.63 0.057 0.78 -6 7 9 135.80 248.58 2.62 0.064 0.84 2 10 3 82.89 23.37 2.61 0.019 1.06 0 8 4 90.41 39.39 2.58 0.025 1.35 3 0 11 -18.90 25.20 2.58 0.020 1.26 8 2 3 102.44 16.72 2.56 0.016 0.86 -1 4 7 262.89 384.41 2.55 0.079 1.75 0 2 13 196.74 112.62 2.55 0.043 1.23 Bond lengths and angles C1 - Distance Angles C2 1.3821 (0.0065) C6 1.3888 (0.0063) 120.00 (0.43) S1 1.7627 (0.0044) 120.64 (0.34) 119.36 (0.34) C1 - C2 C6 C2 - Distance Angles C1 1.3821 (0.0065) C3 1.3920 (0.0069) 119.61 (0.44) H2 0.9500 120.20 120.20 C2 - C1 C3 C3 - Distance Angles C4 1.3894 (0.0070) C2 1.3920 (0.0069) 120.93 (0.45) H3 0.9500 119.54 119.54 C3 - C4 C2 C4 - Distance Angles N4 1.3706 (0.0064) C3 1.3894 (0.0070) 121.74 (0.48) C5 1.4038 (0.0072) 119.81 (0.47) 118.44 (0.45) C4 - N4 C3 C5 - Distance Angles C6 1.3710 (0.0072) C4 1.4038 (0.0072) 120.62 (0.47) H5 0.9500 119.69 119.69 C5 - C6 C4 C6 - Distance Angles C5 1.3710 (0.0072) C1 1.3888 (0.0063) 120.40 (0.45) H6 0.9500 119.80 119.80 C6 - C5 C1 N4 - Distance Angles C4 1.3706 (0.0064) H4A 0.8800 120.00 H4B 0.8800 120.00 120.00 N4 - C4 H4A O1A - Distance Angles S1 1.4666 (0.0037) O1A - O1B - Distance Angles S1 1.4455 (0.0037) O1B - O1C - Distance Angles S1 1.4624 (0.0038) O1C - S1 - Distance Angles O1B 1.4455 (0.0037) O1C 1.4624 (0.0038) 112.10 (0.23) O1A 1.4666 (0.0037) 112.07 (0.23) 111.89 (0.24) C1 1.7627 (0.0044) 106.63 (0.21) 107.18 (0.21) 106.55 (0.23) S1 - O1B O1C O1A C21 - Distance Angles C26 1.3712 (0.0068) C22 1.3863 (0.0070) 121.00 (0.46) N21 1.4816 (0.0058) 120.71 (0.43) 118.29 (0.43) C21 - C26 C22 C22 - Distance Angles C23 1.3813 (0.0075) C21 1.3863 (0.0070) 119.37 (0.45) H22 0.9500 120.31 120.31 C22 - C23 C21 C23 - Distance Angles C22 1.3813 (0.0075) C24 1.3958 (0.0072) 120.89 (0.46) H23 0.9500 119.55 119.55 C23 - C22 C24 C24 - Distance Angles C25 1.3905 (0.0073) C23 1.3958 (0.0072) 118.01 (0.46) C27 1.5105 (0.0071) 120.18 (0.49) 121.80 (0.48) C24 - C25 C23 C25 - Distance Angles C26 1.3827 (0.0072) C24 1.3905 (0.0073) 121.54 (0.48) H25 0.9500 119.23 119.23 C25 - C26 C24 C26 - Distance Angles C21 1.3712 (0.0068) C25 1.3827 (0.0072) 119.14 (0.47) H26 0.9500 120.43 120.43 C26 - C21 C25 C27 - Distance Angles C24 1.5105 (0.0071) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C24 H27A H27B N21 - Distance Angles C21 1.4816 (0.0058) H21A 0.9100 109.47 H21B 0.9100 109.47 109.47 H21C 0.9100 109.47 109.47 109.47 N21 - C21 H21A H21B Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.87 2.770(5) 170.5 N21-H21C...O1B 0.88 2.19 3.050(6) 164.1 N4-H4A...O1C_$1 0.88 3.01 3.873(5) 168.3 N4-H4A...S1_$1 0.88 2.45 3.328(6) 173.6 N4-H4B...O1A_$2 0.91 1.90 2.765(6) 158.5 N21-H21A...O1A_$3 0.91 1.96 2.840(6) 160.9 N21-H21B...O1C_$4 FMAP and GRID set by program FMAP 2 1 11 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0993 for 1753 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.13 at 0.2312 0.3386 0.3012 [ 0.62 A from H27B ] Deepest hole -0.47 at 0.1177 0.0843 0.8403 [ 1.00 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 2770 / 19400 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2688 0.6614 -0.1988 1.00000 0.05 1.13 0.62 H27B 0.89 C27 1.27 H27C 1.33 H27A Q2 1 0.2212 0.8419 0.3027 1.00000 0.05 0.83 0.77 O1B 0.84 S1 1.83 C1 2.03 O1C Q3 1 0.5023 0.6800 -0.2174 1.00000 0.05 0.46 1.06 H27C 1.62 O1B 1.76 C27 1.88 H27A Q4 1 0.2554 0.8979 0.3618 1.00000 0.05 0.45 0.80 C1 0.96 S1 1.91 C2 1.93 C6 Q5 1 0.1939 0.5643 -0.2286 1.00000 0.05 0.42 1.18 H27B 1.53 H21A 1.87 O1A 1.99 C27 Q6 1 0.3532 0.9084 0.5224 1.00000 0.05 0.41 0.87 C3 1.24 C2 1.57 H3 1.63 C4 Q7 1 0.3044 0.7172 0.0396 1.00000 0.05 0.40 0.70 C26 0.76 C25 1.50 H26 1.54 H25 Q8 1 0.2780 0.4847 0.0307 1.00000 0.05 0.39 0.81 C22 1.23 H22 1.28 C23 1.77 H23 Q9 1 0.1326 0.5827 -0.0017 1.00000 0.05 0.38 0.88 C23 1.20 C22 1.61 H23 1.63 C24 Q10 1 0.2228 0.6966 0.3435 1.00000 0.05 0.38 1.26 H6 1.80 O1B 1.90 C6 2.05 H21C Shortest distances between peaks (including symmetry equivalents) 2 4 1.19 1 5 1.32 8 9 1.61 1 3 1.69 2 10 1.79 7 9 2.07 2 3 2.10 4 10 2.33 3 5 2.55 7 8 2.66 4 6 2.73 6 8 2.88 3 10 2.95 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. 0.61: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.97: Structure factors and derivatives 0.59: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0070p212121 finished at 14:36:34 Total CPU time: 2.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++