+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 15:44:27 on 06-Jan-2003 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 7.4038 7.5670 10.7531 89.924 72.445 73.549 ZERR 2.00 0.0005 0.0006 0.0011 0.004 0.004 0.006 LATT 1 SFAC C H N O UNIT 22 20 4 10 V = 548.53 F(000) = 260.0 Mu = 0.12 mm-1 Cell Wt = 500.42 Rho = 1.515 MERG 2 OMIT 1 0 1 EXTI 0.02960 SHEL 7 0.8 FMAP 2 PLAN 10 TEMP -153 SIZE 0.02 0.02 0.30 ACTA BOND $H WGHT 0.04210 0.51170 L.S. 9 FVAR 0.54595 O1 4 0.349768 0.083374 0.369648 11.00000 0.03652 0.03236 = 0.04013 0.01060 -0.01434 -0.01447 O2 4 0.138304 0.069130 0.744789 11.00000 0.01971 0.03381 = 0.02291 -0.00402 -0.00601 -0.00559 O3 4 -0.181447 0.186578 0.867826 11.00000 0.01846 0.04225 = 0.03308 0.00086 -0.00653 -0.00680 O4 4 0.143375 0.502790 1.338660 11.00000 0.03668 0.03603 = 0.02900 -0.00700 -0.00714 -0.00668 O5 4 0.445910 0.407540 1.208729 11.00000 0.02551 0.04491 = 0.03524 -0.00131 -0.01246 -0.01098 N1 3 0.236156 -0.092676 0.540687 11.00000 0.02714 0.02471 = 0.02230 0.00021 -0.00669 -0.00444 N2 3 0.268628 0.422646 1.236308 11.00000 0.02789 0.02289 = 0.02357 -0.00143 -0.00537 -0.00291 C1 1 0.357670 -0.055626 0.426625 11.00000 0.02797 0.02859 = 0.02827 0.00248 -0.01260 -0.01126 C2 1 0.492444 -0.255307 0.401209 11.00000 0.03024 0.02590 = 0.02929 -0.00182 -0.00534 -0.00995 C3 1 0.352063 -0.287837 0.533632 11.00000 0.02662 0.02668 = 0.02818 0.00130 -0.00664 -0.00571 C4 1 0.069026 0.022847 0.639300 11.00000 0.02152 0.03340 = 0.02787 -0.00374 -0.01193 -0.00410 C5 1 -0.006066 0.153842 0.854568 11.00000 0.02083 0.02248 = 0.02410 0.00284 -0.00702 -0.00509 C6 1 0.072073 0.208147 0.956570 11.00000 0.01940 0.01956 = 0.02649 0.00668 -0.01030 -0.00634 C7 1 0.276076 0.174809 0.934684 11.00000 0.01961 0.02539 = 0.02400 0.00104 -0.00446 -0.00386 C8 1 0.341755 0.243386 1.027014 11.00000 0.01989 0.02606 = 0.02524 0.00188 -0.00625 -0.00316 C9 1 0.201364 0.340796 1.140265 11.00000 0.02577 0.01958 = 0.02773 0.00253 -0.01151 -0.00468 C10 1 -0.001413 0.369897 1.166590 11.00000 0.02408 0.02816 = 0.01953 -0.00018 -0.00148 -0.00484 C11 1 -0.065350 0.304573 1.072697 11.00000 0.01969 0.02201 = 0.02733 0.00642 -0.00655 -0.00136 H2A 2 0.632092 -0.260565 0.397601 11.00000 0.05234 H2B 2 0.499238 -0.344779 0.322591 11.00000 0.05285 H3A 2 0.397784 -0.308561 0.618182 11.00000 0.04304 H3B 2 0.276618 -0.378428 0.526044 11.00000 0.02225 H4A 2 0.006054 0.138954 0.603363 11.00000 0.04324 H4B 2 -0.026964 -0.049090 0.675545 11.00000 0.02129 H7 2 0.368286 0.120012 0.856392 11.00000 0.02172 H8 2 0.475544 0.221518 1.012561 11.00000 0.04611 H10 2 -0.087630 0.442031 1.245168 11.00000 0.02760 H11 2 -0.207168 0.326744 1.086477 11.00000 0.04370 HKLF 4 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 O1 - C1 O2 - C5 C4 O3 - C5 O4 - N2 O5 - N2 N1 - C1 C4 C3 N2 - O5 O4 C9 C1 - O1 N1 C2 C2 - C1 C3 C3 - N1 C2 C4 - N1 O2 C5 - O3 O2 C6 C6 - C11 C7 C5 C7 - C8 C6 C8 - C9 C7 C9 - C8 C10 N2 C10 - C11 C9 C11 - C10 C6 9634 Reflections read, of which 481 rejected -9 =< h =< 9, -9 =< k =< 9, -13 =< l =< 13, Max. 2-theta = 52.74 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 3 0 6.07 0.69 5 7.19 4 5 0 20.32 1.22 6 7.85 4 4 1 31.30 1.21 6 6.38 -6 -2 3 0.36 0.64 7 3.42 6 -2 3 11.07 1.56 6 8.86 6 0 3 15.15 1.39 6 7.97 -5 -8 4 5.15 1.00 2 5.47 -5 -7 4 4.72 0.90 3 4.68 7 7 4 1.32 0.98 2 5.97 4 -2 5 3.97 0.85 6 4.79 0 -2 7 8.21 2.31 5 15.11 -1 -5 8 6.50 2.07 5 16.29 -2 -4 10 6.50 3.31 4 18.89 4 3 11 4.93 1.64 5 18.00 14 Inconsistent equivalents 2231 Unique reflections, of which 0 suppressed R(int) = 0.1680 R(sigma) = 0.1235 Friedel opposites merged Maximum memory for data reduction = 1550 / 22505 Least-squares cycle 1 Maximum vector length = 511 Memory required = 2027 / 252801 wR2 = 0.1693 before cycle 1 for 2231 data and 204 / 204 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54588 0.00266 -0.026 OSF 2 0.02950 0.00638 -0.016 EXTI Mean shift/esd = 0.007 Maximum = -0.029 for x C2 Max. shift = 0.002 A for H2A Max. dU = 0.000 for H2A Least-squares cycle 2 Maximum vector length = 511 Memory required = 2027 / 252801 wR2 = 0.1693 before cycle 2 for 2231 data and 204 / 204 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54586 0.00266 -0.008 OSF 2 0.02946 0.00637 -0.007 EXTI Mean shift/esd = 0.003 Maximum = -0.010 for x C2 Max. shift = 0.000 A for H2A Max. dU = 0.000 for H2A Least-squares cycle 3 Maximum vector length = 511 Memory required = 2027 / 252801 wR2 = 0.1693 before cycle 3 for 2231 data and 204 / 204 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54586 0.00266 0.000 OSF 2 0.02945 0.00637 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x H11 Max. shift = 0.000 A for H11 Max. dU = 0.000 for H11 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2027 / 252801 wR2 = 0.1693 before cycle 4 for 2231 data and 204 / 204 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54586 0.00266 0.000 OSF 2 0.02945 0.00637 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z H2A Max. shift = 0.000 A for H2A Max. dU = 0.000 for H11 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2027 / 252801 wR2 = 0.1693 before cycle 5 for 2231 data and 204 / 204 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54586 0.00266 0.000 OSF 2 0.02945 0.00637 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H11 Max. dU = 0.000 for H11 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2027 / 252801 wR2 = 0.1693 before cycle 6 for 2231 data and 204 / 204 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54586 0.00266 0.000 OSF 2 0.02945 0.00637 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O5 Max. shift = 0.000 A for H2A Max. dU = 0.000 for H2A Least-squares cycle 7 Maximum vector length = 511 Memory required = 2027 / 252801 wR2 = 0.1693 before cycle 7 for 2231 data and 204 / 204 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54586 0.00266 0.000 OSF 2 0.02945 0.00637 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z N2 Max. shift = 0.000 A for H8 Max. dU = 0.000 for H4A Least-squares cycle 8 Maximum vector length = 511 Memory required = 2027 / 252801 wR2 = 0.1694 before cycle 8 for 2231 data and 204 / 204 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54586 0.00266 0.000 OSF 2 0.02945 0.00637 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z N2 Max. shift = 0.000 A for H3A Max. dU = 0.000 for H2B Least-squares cycle 9 Maximum vector length = 511 Memory required = 2027 / 252801 wR2 = 0.1693 before cycle 9 for 2231 data and 204 / 204 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54586 0.00266 0.000 OSF 2 0.02945 0.00637 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O5 Max. shift = 0.000 A for H11 Max. dU = 0.000 for H4B Largest correlation matrix elements 0.528 EXTI / OSF -0.512 U12 O1 / U22 O1 s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O1 0.34977 0.08337 0.36964 1.00000 0.03648 0.03236 0.04011 0.01057 -0.01432 -0.01444 0.03487 0.00422 0.00042 0.00040 0.00028 0.00000 0.00163 0.00173 0.00174 0.00139 0.00135 0.00139 0.00076 O2 0.13830 0.06913 0.74479 1.00000 0.01970 0.03382 0.02290 -0.00401 -0.00602 -0.00557 0.02614 0.00371 0.00035 0.00037 0.00024 0.00000 0.00130 0.00163 0.00147 0.00118 0.00110 0.00123 0.00066 O3 -0.18145 0.18658 0.86783 1.00000 0.01846 0.04223 0.03308 0.00084 -0.00652 -0.00678 0.03210 0.00408 0.00037 0.00041 0.00027 0.00000 0.00133 0.00182 0.00160 0.00129 0.00114 0.00130 0.00072 O4 0.14338 0.50279 1.33866 1.00000 0.03667 0.03606 0.02899 -0.00699 -0.00715 -0.00668 0.03553 0.00405 0.00041 0.00040 0.00027 0.00000 0.00162 0.00177 0.00167 0.00136 0.00135 0.00144 0.00075 O5 0.44591 0.40754 1.20873 1.00000 0.02551 0.04487 0.03526 -0.00132 -0.01244 -0.01098 0.03441 0.00400 0.00039 0.00042 0.00027 0.00000 0.00151 0.00191 0.00167 0.00135 0.00125 0.00139 0.00075 N1 0.23617 -0.09268 0.54069 1.00000 0.02714 0.02469 0.02229 0.00022 -0.00670 -0.00447 0.02565 0.00462 0.00045 0.00044 0.00030 0.00000 0.00168 0.00183 0.00178 0.00137 0.00138 0.00147 0.00076 N2 0.26863 0.42265 1.23631 1.00000 0.02792 0.02290 0.02354 -0.00143 -0.00537 -0.00294 0.02641 0.00476 0.00047 0.00044 0.00031 0.00000 0.00180 0.00187 0.00183 0.00142 0.00144 0.00152 0.00077 C1 0.35767 -0.05563 0.42662 1.00000 0.02793 0.02858 0.02824 0.00247 -0.01257 -0.01126 0.02675 0.00555 0.00056 0.00056 0.00038 0.00000 0.00204 0.00231 0.00220 0.00177 0.00173 0.00181 0.00090 C2 0.49242 -0.25531 0.40122 1.00000 0.03027 0.02591 0.02925 -0.00179 -0.00535 -0.00995 0.02905 0.00637 0.00060 0.00057 0.00040 0.00000 0.00217 0.00219 0.00227 0.00176 0.00176 0.00187 0.00093 C3 0.35207 -0.28782 0.53363 1.00000 0.02665 0.02663 0.02821 0.00127 -0.00665 -0.00572 0.02809 0.00644 0.00058 0.00058 0.00041 0.00000 0.00201 0.00225 0.00222 0.00172 0.00172 0.00185 0.00091 C4 0.06902 0.02286 0.63930 1.00000 0.02151 0.03341 0.02782 -0.00373 -0.01193 -0.00416 0.02746 0.00573 0.00057 0.00062 0.00040 0.00000 0.00191 0.00241 0.00216 0.00184 0.00168 0.00188 0.00092 C5 -0.00607 0.15384 0.85458 1.00000 0.02085 0.02247 0.02407 0.00282 -0.00702 -0.00511 0.02276 0.00557 0.00052 0.00053 0.00037 0.00000 0.00190 0.00204 0.00204 0.00159 0.00158 0.00165 0.00083 C6 0.07208 0.20815 0.95657 1.00000 0.01939 0.01957 0.02649 0.00671 -0.01029 -0.00634 0.02098 0.00536 0.00050 0.00050 0.00036 0.00000 0.00180 0.00195 0.00202 0.00156 0.00154 0.00158 0.00081 C7 0.27608 0.17481 0.93469 1.00000 0.01956 0.02535 0.02402 0.00104 -0.00447 -0.00382 0.02414 0.00580 0.00055 0.00054 0.00040 0.00000 0.00184 0.00221 0.00214 0.00173 0.00167 0.00173 0.00085 C8 0.34175 0.24339 1.02701 1.00000 0.01983 0.02606 0.02520 0.00186 -0.00622 -0.00317 0.02469 0.00582 0.00057 0.00055 0.00037 0.00000 0.00190 0.00217 0.00211 0.00164 0.00161 0.00173 0.00087 C9 0.20137 0.34080 1.14026 1.00000 0.02575 0.01953 0.02768 0.00253 -0.01150 -0.00467 0.02404 0.00542 0.00054 0.00051 0.00037 0.00000 0.00197 0.00207 0.00212 0.00164 0.00164 0.00169 0.00086 C10 -0.00141 0.36990 1.16659 1.00000 0.02405 0.02814 0.01951 -0.00018 -0.00144 -0.00484 0.02578 0.00585 0.00056 0.00056 0.00038 0.00000 0.00196 0.00229 0.00207 0.00175 0.00166 0.00182 0.00089 C11 -0.06534 0.30456 1.07269 1.00000 0.01969 0.02201 0.02728 0.00640 -0.00656 -0.00136 0.02424 0.00582 0.00055 0.00052 0.00037 0.00000 0.00188 0.00213 0.00215 0.00168 0.00162 0.00170 0.00088 H2A 0.63185 -0.26062 0.39764 1.00000 0.05214 0.07461 0.00765 0.00691 0.00470 0.00000 0.01373 H2B 0.49931 -0.34483 0.32258 1.00000 0.05304 0.07722 0.00702 0.00717 0.00497 0.00000 0.01366 H3A 0.39784 -0.30859 0.61819 1.00000 0.04311 0.06880 0.00661 0.00624 0.00473 0.00000 0.01242 H3B 0.27666 -0.37839 0.52598 1.00000 0.02236 0.05988 0.00550 0.00541 0.00362 0.00000 0.00981 H4A 0.00604 0.13890 0.60339 1.00000 0.04321 0.06666 0.00670 0.00692 0.00462 0.00000 0.01247 H4B -0.02687 -0.04903 0.67552 1.00000 0.02111 0.05659 0.00568 0.00534 0.00360 0.00000 0.00961 H7 0.36828 0.12005 0.85641 1.00000 0.02174 0.05643 0.00593 0.00539 0.00405 0.00000 0.01011 H8 0.47542 0.22153 1.01254 1.00000 0.04595 0.07041 0.00738 0.00676 0.00458 0.00000 0.01319 H10 -0.08757 0.44202 1.24515 1.00000 0.02744 0.06159 0.00614 0.00596 0.00436 0.00000 0.01044 H11 -0.20729 0.32680 1.08657 1.00000 0.04381 0.06701 0.00696 0.00634 0.00436 0.00000 0.01268 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 204 Maximum vector length = 511 Memory required = 1823 / 22995 wR2 = 0.1693 before cycle 10 for 2231 data and 0 / 204 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0759 for 1260 Fo > 4sig(Fo) and 0.1517 for all 2231 data wR2 = 0.1693, GooF = S = 1.035, Restrained GooF = 1.035 for all data Occupancy sum of asymmetric unit = 18.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0440 0.0343 0.0263 O1 0.0380 0.0208 0.0196 O2 0.0440 0.0340 0.0183 O3 0.0445 0.0393 0.0228 O4 0.0477 0.0340 0.0216 O5 0.0308 0.0249 0.0213 N1 0.0331 0.0269 0.0193 N2 0.0313 0.0286 0.0203 C1 0.0368 0.0274 0.0229 C2 0.0309 0.0288 0.0245 C3 0.0406 0.0247 0.0171 C4 0.0250 0.0231 0.0202 C5 0.0284 0.0187 0.0159 C6 0.0280 0.0257 0.0187 C7 0.0295 0.0256 0.0190 C8 0.0298 0.0235 0.0188 C9 0.0320 0.0283 0.0170 C10 0.0337 0.0233 0.0157 C11 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.016 0.024 0.032 0.042 0.053 0.068 0.091 0.133 1.000 Number in group 223. 223. 231. 218. 225. 231. 219. 217. 222. 222. GooF 1.049 1.034 1.013 1.017 1.107 1.037 1.048 0.978 1.048 1.015 K 18.341 3.613 1.768 1.401 1.144 1.072 1.002 1.004 0.991 1.007 Resolution(A) 0.80 0.83 0.86 0.90 0.95 1.01 1.08 1.19 1.36 1.69 inf Number in group 225. 223. 229. 217. 224. 227. 216. 225. 224. 221. GooF 1.108 1.045 1.093 1.006 0.989 1.010 0.911 1.024 0.947 1.187 K 1.195 1.129 1.038 1.030 1.024 1.024 1.037 1.054 1.053 0.994 R1 0.396 0.346 0.298 0.213 0.167 0.119 0.083 0.105 0.070 0.057 Recommended weighting scheme: WGHT 0.0421 0.5094 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) 9 4 2 -3.29 93.70 4.76 0.093 0.80 3 2 2 37.96 14.73 3.67 0.037 2.26 4 6 10 28.05 1.99 3.58 0.014 0.82 3 8 0 -3.96 12.04 3.37 0.033 0.94 0 8 3 148.09 81.71 3.30 0.087 0.85 7 -3 3 25.05 0.08 3.23 0.003 0.85 3 2 8 19.13 0.09 3.22 0.003 1.25 -2 1 3 46.59 18.00 3.16 0.041 1.89 -3 -1 2 13.84 0.46 3.07 0.007 1.93 8 -2 6 -2.56 27.03 3.06 0.050 0.80 3 0 0 57.09 34.25 3.05 0.056 2.25 1 -3 11 16.13 38.19 2.93 0.059 0.91 -6 -5 2 25.22 2.21 2.93 0.014 0.99 8 -1 8 0.00 29.24 2.91 0.052 0.81 -7 2 1 40.67 8.80 2.91 0.028 0.84 5 3 8 38.62 16.65 2.84 0.039 1.09 -5 2 3 8.14 27.50 2.81 0.050 1.01 6 -1 10 26.30 1.47 2.70 0.012 0.89 1 0 2 321.95 391.67 2.67 0.190 4.87 -7 -5 3 53.30 0.17 2.66 0.004 0.85 -7 -3 3 63.13 2.14 2.63 0.014 0.89 -3 -2 5 51.37 29.81 2.58 0.052 1.34 -7 3 0 54.42 22.69 2.57 0.046 0.81 8 1 1 63.15 88.93 2.56 0.090 0.89 -2 2 4 409.14 334.96 2.56 0.176 1.47 4 3 7 26.09 1.16 2.56 0.010 1.24 4 -6 6 28.68 1.69 2.55 0.012 0.85 3 0 3 25.64 4.78 2.55 0.021 2.22 -4 5 4 34.56 1.43 2.53 0.011 0.84 -4 -6 7 17.34 37.21 2.49 0.059 0.85 3 7 1 78.73 56.02 2.48 0.072 1.07 0 -2 4 176.02 219.35 2.48 0.142 2.18 -2 -4 1 -4.80 7.40 2.44 0.026 1.78 1 -7 5 12.94 33.57 2.44 0.056 0.93 2 -1 11 126.56 183.08 2.42 0.130 0.97 2 6 10 -4.17 32.53 2.41 0.055 0.80 -3 5 0 73.84 36.78 2.41 0.058 1.08 -3 -8 5 43.73 10.86 2.40 0.032 0.84 -3 2 7 234.86 306.44 2.39 0.168 0.98 2 1 5 29.31 8.54 2.38 0.028 2.02 0 -5 9 19.14 5.35 2.37 0.022 0.94 0 -3 2 28.93 7.56 2.36 0.026 2.26 4 -4 4 15.24 0.69 2.36 0.008 1.10 6 -2 9 28.49 7.87 2.34 0.027 0.89 -1 -1 3 30.36 15.79 2.34 0.038 2.72 1 -2 13 29.68 3.63 2.29 0.018 0.80 5 -2 7 20.36 4.21 2.29 0.020 1.08 -1 1 7 43.26 26.25 2.28 0.049 1.29 -1 2 7 46.54 68.53 2.28 0.079 1.20 1 8 3 -2.25 16.08 2.28 0.038 0.89 Bond lengths and angles O1 - Distance Angles C1 1.2125 (0.0046) O1 - O2 - Distance Angles C5 1.3416 (0.0047) C4 1.4582 (0.0044) 114.81 (0.28) O2 - C5 O3 - Distance Angles C5 1.2140 (0.0042) O3 - O4 - Distance Angles N2 1.2274 (0.0042) O4 - O5 - Distance Angles N2 1.2264 (0.0039) O5 - N1 - Distance Angles C1 1.3670 (0.0048) C4 1.4206 (0.0051) 132.01 (0.35) C3 1.4717 (0.0052) 95.50 (0.29) 132.14 (0.33) N1 - C1 C4 N2 - Distance Angles O5 1.2264 (0.0039) O4 1.2274 (0.0042) 123.88 (0.32) C9 1.4782 (0.0047) 118.13 (0.31) 117.99 (0.32) N2 - O5 O4 C1 - Distance Angles O1 1.2125 (0.0046) N1 1.3670 (0.0048) 132.07 (0.38) C2 1.5283 (0.0057) 136.16 (0.37) 91.71 (0.30) C1 - O1 N1 C2 - Distance Angles C1 1.5283 (0.0057) C3 1.5553 (0.0055) 85.96 (0.30) H2A 1.0106 (0.0501) 110.92 (2.87) 117.36 (2.73) H2B 1.0642 (0.0525) 120.91 (2.61) 111.57 (2.61) 108.99 (3.88) C2 - C1 C3 H2A C3 - Distance Angles N1 1.4717 (0.0052) C2 1.5553 (0.0055) 86.80 (0.29) H3A 1.0590 (0.0468) 108.70 (2.51) 121.63 (2.44) H3B 1.0163 (0.0392) 113.56 (2.10) 114.56 (2.14) 109.52 (3.17) C3 - N1 C2 H3A C4 - Distance Angles N1 1.4206 (0.0051) O2 1.4582 (0.0044) 107.44 (0.28) H4A 1.0067 (0.0491) 110.80 (2.72) 110.19 (2.65) H4B 1.0015 (0.0386) 108.79 (2.25) 107.76 (2.09) 111.72 (3.21) C4 - N1 O2 H4A C5 - Distance Angles O3 1.2140 (0.0042) O2 1.3416 (0.0047) 123.39 (0.34) C6 1.4917 (0.0051) 123.82 (0.35) 112.77 (0.29) C5 - O3 O2 C6 - Distance Angles C11 1.3936 (0.0055) C7 1.4036 (0.0049) 120.38 (0.35) C5 1.4917 (0.0051) 117.66 (0.31) 121.84 (0.34) C6 - C11 C7 C7 - Distance Angles C8 1.3881 (0.0056) C6 1.4036 (0.0049) 120.01 (0.38) H7 0.9167 (0.0422) 117.91 (2.35) 121.70 (2.35) C7 - C8 C6 C8 - Distance Angles C9 1.3826 (0.0056) C7 1.3881 (0.0056) 118.11 (0.35) H8 0.9195 (0.0479) 121.96 (3.05) 119.92 (3.06) C8 - C9 C7 C9 - Distance Angles C8 1.3826 (0.0057) C10 1.3925 (0.0052) 123.04 (0.36) N2 1.4782 (0.0047) 118.64 (0.32) 118.30 (0.35) C9 - C8 C10 C10 - Distance Angles C11 1.3821 (0.0055) C9 1.3925 (0.0052) 118.32 (0.37) H10 0.9473 (0.0459) 124.01 (2.38) 117.48 (2.39) C10 - C11 C9 C11 - Distance Angles C10 1.3821 (0.0055) C6 1.3936 (0.0055) 120.08 (0.34) H11 0.9800 (0.0455) 120.46 (2.71) 119.45 (2.71) C11 - C10 C6 FMAP and GRID set by program FMAP 2 1 20 GRID -2.941 -2 -2 2.941 2 2 R1 = 0.1516 for 2231 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.29 at 0.3636 0.9606 0.6612 [ 1.61 A from O2 ] Deepest hole -0.32 at 0.4471 0.2039 0.6633 [ 0.86 A from C2 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 1838 / 16711 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3636 -0.0394 0.6612 1.00000 0.05 0.29 1.61 O2 1.92 N1 1.98 O1 2.02 H3A Q2 1 0.1715 0.0515 0.4138 1.00000 0.05 0.26 1.35 O1 1.43 C1 1.64 H4B 1.84 N1 Q3 1 0.3225 0.4636 1.3642 1.00000 0.05 0.26 1.38 O4 1.60 N2 1.63 O5 2.00 H3B Q4 1 0.6678 0.2661 1.0020 1.00000 0.05 0.26 1.53 H8 1.53 O3 1.63 H11 2.37 O5 Q5 1 -0.1760 0.1320 0.7355 1.00000 0.05 0.25 1.47 O3 1.49 H4B 1.65 H4A 1.75 C4 Q6 1 0.1068 0.2220 0.9228 1.00000 0.05 0.24 0.41 C6 1.25 C7 1.45 C5 1.71 C11 Q7 1 -0.3162 0.1813 0.7845 1.00000 0.05 0.24 1.54 O3 2.16 H2B 2.32 H4B 2.41 H7 Q8 1 0.2449 -0.0308 0.3185 1.00000 0.05 0.24 1.51 O1 1.54 H4B 1.61 C1 2.18 H4A Q9 1 -0.0937 -0.0068 0.6866 1.00000 0.05 0.23 0.49 H4B 1.24 C4 1.62 H4A 2.21 O2 Q10 1 -0.2972 0.1309 0.7808 1.00000 0.05 0.23 1.57 O3 2.06 H4B 2.39 H7 2.39 H2B Shortest distances between peaks (including symmetry equivalents) 7 10 0.36 5 10 0.88 5 7 0.97 8 9 1.09 5 9 1.09 2 8 1.10 8 10 1.20 5 8 1.26 2 9 1.45 7 8 1.45 9 10 1.60 7 9 1.86 2 5 2.11 2 10 2.29 4 7 2.38 4 10 2.50 2 7 2.52 4 5 2.81 2 2 2.96 Time profile in seconds ----------------------- 0.19: 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 0.06: Analyse other restraints etc. 0.84: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.95: Structure factors and derivatives 2.50: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.42: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 15:44:32 Total CPU time: 5.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++