+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0463p21c started at 13:16:56 on 15-May-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0463p21c in P2(1)/c CELL 0.71073 19.7544 7.0169 11.6931 90.000 103.210 90.000 ZERR 8.00 0.0004 0.0001 0.0002 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 64 40 24 16 V = 1577.95 F(000) = 720.0 Mu = 0.11 mm-1 Cell Wt = 1401.20 Rho = 1.475 MERG 2 OMIT -3.00 50.00 OMIT -2 2 1 OMIT 2 2 0 OMIT 2 2 1 SHEL 7 0.84 DELU C1 > O5B SIMU C1 > O5B EADP C3 C3B EQIV_$1 x, -y+1/2, z-1/2 EQIV_$2 -x+1, -y+1, -z+2 HTAB N11 N10_$1 HTAB N11 N33_$2 HTAB N31 N30_$1 HTAB N31 N13_$2 DFIX 0.89 0.02 N11 H11A N11 H11b N31 H31A N31 H31b FMAP 2 PLAN 10 SIZE 0.14 0.26 0.45 ACTA BOND $H WGHT 0.05760 0.90360 L.S. 4 TEMP -153.00 FVAR 0.24458 0.84275 PART 1 C1 1 -0.033682 0.223730 1.015465 21.00000 0.02258 0.01647 = 0.03461 0.00387 0.00481 0.00201 C2 1 -0.063859 0.203069 1.107260 21.00000 0.03650 0.03450 = 0.04246 0.00587 0.01103 -0.00060 AFIX 43 H2 2 -0.042801 0.220892 1.188099 21.00000 -1.20000 AFIX 0 C3 1 -0.133892 0.148946 1.057566 21.00000 0.02548 0.03317 = 0.06926 0.00773 0.01999 -0.00336 AFIX 43 H3 2 -0.169057 0.125061 1.099220 21.00000 -1.20000 AFIX 0 C4 1 -0.140843 0.138092 0.941661 21.00000 0.02207 0.02772 = 0.06304 -0.00410 0.00984 -0.00573 AFIX 43 H4 2 -0.182578 0.104492 0.887045 21.00000 -1.20000 AFIX 0 O5 4 -0.079797 0.181868 0.912439 21.00000 0.02068 0.03287 = 0.04307 -0.00721 0.00219 -0.00358 PART 2 SAME C1 > O5 C1B 1 -0.029628 0.203696 1.030936 -21.00000 0.01720 0.02911 = 0.02263 0.01351 -0.00647 -0.00256 C2B 1 -0.088504 0.167991 0.949232 -21.00000 0.02925 0.01756 = 0.03632 -0.01152 0.00969 -0.00669 AFIX 43 H2B 2 -0.094489 0.168607 0.866276 -21.00000 -1.20000 AFIX 0 C3B 1 -0.139723 0.129191 1.014236 -21.00000 0.02548 0.03317 = 0.06926 0.00773 0.01999 -0.00336 AFIX 43 H3B 2 -0.186545 0.091821 0.983217 -21.00000 -1.20000 AFIX 0 C4B 1 -0.108831 0.155813 1.128294 -21.00000 0.04612 0.02063 = 0.06403 0.00828 0.03267 -0.01000 AFIX 43 H4B 2 -0.130865 0.136709 1.191592 -21.00000 -1.20000 AFIX 0 O5B 4 -0.042419 0.213231 1.140541 -21.00000 0.04273 0.02892 = 0.03524 0.00453 0.02144 -0.01093 MOLE 1 PART 0 C6 1 0.036031 0.277494 1.010546 11.00000 0.02292 0.02033 = 0.02824 0.00247 0.00597 0.00160 C8 1 0.118169 0.340998 0.920136 11.00000 0.01823 0.02265 = 0.02869 -0.00061 0.00338 -0.00231 C9 1 0.141143 0.371443 1.038732 11.00000 0.01959 0.02340 = 0.02420 0.00134 0.00331 -0.00078 C12 1 0.206723 0.438835 1.099574 11.00000 0.02434 0.02940 = 0.02120 0.00098 0.00516 0.00104 C21 1 0.420208 0.168840 1.010592 11.00000 0.02038 0.02040 = 0.02539 -0.00045 0.00147 0.00161 C22 1 0.393501 0.138427 1.105187 11.00000 0.03976 0.03104 = 0.02271 -0.00085 0.01067 -0.00017 AFIX 43 H22 2 0.415893 0.156277 1.185452 11.00000 -1.20000 AFIX 0 C23 1 0.323687 0.073033 1.058167 11.00000 0.03166 0.03228 = 0.05941 0.00183 0.02592 -0.00073 AFIX 43 H23 2 0.290539 0.039399 1.102122 11.00000 -1.20000 AFIX 0 C24 1 0.314053 0.068290 0.941886 11.00000 0.01822 0.03706 = 0.05057 0.00188 0.00268 -0.00440 AFIX 43 H24 2 0.272239 0.029824 0.889160 11.00000 -1.20000 AFIX 0 C26 1 0.487640 0.238021 1.003197 11.00000 0.02188 0.02103 = 0.02144 0.00171 0.00475 0.00137 C28 1 0.567213 0.332826 0.913641 11.00000 0.01978 0.02259 = 0.02471 -0.00248 0.00367 -0.00122 C29 1 0.591594 0.344355 1.033488 11.00000 0.01952 0.02477 = 0.02097 -0.00083 0.00284 -0.00044 C32 1 0.658429 0.402616 1.096146 11.00000 0.02599 0.02752 = 0.02209 -0.00040 0.00621 -0.00106 O7 4 0.050701 0.281628 0.900655 11.00000 0.01947 0.02834 = 0.02637 -0.00289 0.00218 -0.00275 N11 3 0.145714 0.357431 0.827071 11.00000 0.02381 0.04640 = 0.02627 -0.00785 0.00479 -0.01102 N13 3 0.260280 0.495119 1.148791 11.00000 0.02422 0.04954 = 0.02895 -0.00169 0.00223 -0.00605 O27 4 0.500554 0.264793 0.893282 11.00000 0.01879 0.02799 = 0.02115 -0.00116 0.00398 -0.00309 N31 3 0.592161 0.375995 0.821328 11.00000 0.02401 0.04660 = 0.02023 -0.00317 0.00550 -0.01091 N33 3 0.713079 0.449397 1.145959 11.00000 0.02652 0.04434 = 0.02880 -0.00137 0.00372 -0.00864 N10 3 0.087101 0.328970 1.094747 11.00000 0.02134 0.02441 = 0.02694 0.00301 0.00384 0.00003 O25 4 0.372988 0.126751 0.908866 11.00000 0.02564 0.03571 = 0.03305 -0.00073 0.00146 -0.00358 N30 3 0.539212 0.282343 1.088534 11.00000 0.01962 0.02566 = 0.02352 0.00095 0.00482 -0.00031 H11A 2 0.122880 0.308322 0.757512 11.00000 -1.20000 H11B 2 0.187852 0.399018 0.836402 11.00000 -1.20000 H31A 2 0.570065 0.330130 0.750875 11.00000 -1.20000 H31B 2 0.636474 0.412035 0.834753 11.00000 -1.20000 HKLF 4 Covalent radii and connectivity table for 2009src0463p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1_a - C2_a O5_a C6 C2_a - C1_a C3_a C3_a - C4_a C2_a C4_a - C3_a O5_a O5_a - C4_a C1_a C1B_b - C2B_b O5B_b C6 C2B_b - C1B_b C3B_b C3B_b - C4B_b C2B_b C4B_b - C3B_b O5B_b O5B_b - C4B_b C1B_b C6 - N10 O7 C1_a C1B_b C8 - N11 O7 C9 C9 - C8 N10 C12 C12 - N13 C9 C21 - C22 O25 C26 C22 - C21 C23 C23 - C24 C22 C24 - C23 O25 C26 - N30 O27 C21 C28 - N31 O27 C29 C29 - C28 N30 C32 C32 - N33 C29 O7 - C8 C6 N11 - C8 N13 - C12 O27 - C28 C26 N31 - C28 N33 - C32 N10 - C6 C9 O25 - C21 C24 N30 - C26 C29 Operators for generating equivalent atoms: $1 x, -y+1/2, z-1/2 $2 -x+1, -y+1, -z+2 22985 Reflections read, of which 4047 rejected -23 =< h =< 23, -8 =< k =< 8, -13 =< l =< 13, Max. 2-theta = 49.99 0 Systematic absence violations 0 Inconsistent equivalents 2769 Unique reflections, of which 0 suppressed R(int) = 0.0559 R(sigma) = 0.0386 Friedel opposites merged Maximum memory for data reduction = 2720 / 27650 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 = 3448 / 358211 wR2 = 0.1206 before cycle 1 for 2769 data and 287 / 287 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 10. 0. 0. 0. 20. 132. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.015 0.000 0.009 0.000 0.000 0.000 0.006 0.012 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.006 for 166 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0576 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24458 0.00063 0.006 OSF 2 0.84272 0.00586 -0.005 FVAR 2 Mean shift/su = 0.007 Maximum = -0.041 for y H11A Max. shift = 0.001 A for H11A Max. dU = 0.000 for C4B_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 3448 / 358211 wR2 = 0.1206 before cycle 2 for 2769 data and 287 / 287 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 10. 0. 0. 0. 20. 132. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.015 0.000 0.009 0.000 0.000 0.000 0.006 0.012 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.006 for 166 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0576 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24459 0.00063 0.011 OSF 2 0.84270 0.00586 -0.004 FVAR 2 Mean shift/su = 0.003 Maximum = -0.024 for y H11A Max. shift = 0.000 A for H11A Max. dU = 0.000 for O5B_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 3448 / 358211 wR2 = 0.1206 before cycle 3 for 2769 data and 287 / 287 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 10. 0. 0. 0. 20. 132. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.015 0.000 0.009 0.000 0.000 0.000 0.006 0.012 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.006 for 166 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0576 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24459 0.00063 0.000 OSF 2 0.84269 0.00586 -0.001 FVAR 2 Mean shift/su = 0.000 Maximum = -0.006 for y H11A Max. shift = 0.000 A for H11A Max. dU = 0.000 for C1B_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 3448 / 358211 wR2 = 0.1206 before cycle 4 for 2769 data and 287 / 287 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 10. 0. 0. 0. 20. 132. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.015 0.000 0.009 0.000 0.000 0.000 0.006 0.012 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.006 for 166 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0576 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24459 0.00063 0.000 OSF 2 0.84269 0.00586 -0.001 FVAR 2 Mean shift/su = 0.000 Maximum = -0.002 for U13 C1B_b Max. shift = 0.000 A for C1B_b Max. dU = 0.000 for C1B_b Largest correlation matrix elements -0.967 y C1B_b / y C1_a 0.815 y C3B_b / U23 C3_a -0.760 y O5B_b / U12 C2_a -0.895 y O5B_b / y C2_a -0.784 U22 C1B_b / y C1_a 0.755 y C1B_b / U22 C1_a -0.867 y C2B_b / y O5_a -0.783 y C2B_b / U23 O5_a -0.735 z C1B_b / U33 C1_a -0.846 x C1B_b / x C1_a -0.778 y O5B_b / U23 C2_a 0.733 U23 O5_a / y O5_a -0.844 y C1B_b / U23 C1_a -0.775 y C3B_b / y C3_a -0.732 U22 C1B_b / U23 C1_a -0.840 z C1B_b / z C1_a -0.773 U12 O5B_b / y O5B_b 0.729 U23 C2_a / y C2_a 0.826 U23 C1_a / y C1_a 0.767 U23 C2B_b / y O5_a -0.728 z O5B_b / U33 C2_a 0.823 U12 O5B_b / y C2_a 0.765 U23 O5B_b / y C2_a -0.723 U23 O5B_b / y O5B_b Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -0.0428 0.2209 1.1881 43 0.950 0.000 C2_a C1_a C3_a H3 -0.1691 0.1251 1.0992 43 0.950 0.000 C3_a C4_a C2_a H4 -0.1826 0.1045 0.8870 43 0.950 0.000 C4_a C3_a O5_a H2B -0.0944 0.1685 0.8663 43 0.950 0.000 C2B_b C1B_b C3B_b H3B -0.1866 0.0920 0.9832 43 0.950 0.000 C3B_b C4B_b C2B_b H4B -0.1308 0.1366 1.1916 43 0.950 0.000 C4B_b C3B_b O5B_b H22 0.4159 0.1563 1.1854 43 0.950 0.000 C22 C21 C23 H23 0.2905 0.0394 1.1021 43 0.950 0.000 C23 C24 C22 H24 0.2722 0.0298 0.8892 43 0.950 0.000 C24 C23 O25 2009src0463p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1_a -0.03368 0.22374 1.01546 0.84269 0.02258 0.01646 0.03461 0.00389 0.00481 0.00206 0.02483 0.01308 0.00028 0.00175 0.00056 0.00586 0.00177 0.00249 0.00226 0.00260 0.00172 0.00166 0.00131 C2_a -0.06386 0.20306 1.10726 0.84269 0.03650 0.03451 0.04246 0.00584 0.01104 -0.00062 0.03750 0.00946 0.00025 0.00103 0.00046 0.00586 0.00262 0.00206 0.00262 0.00204 0.00175 0.00206 0.00104 H2_a -0.04280 0.22087 1.18810 0.84269 0.04500 0.00586 0.00000 C3_a -0.13389 0.14894 1.05757 0.84269 0.02548 0.03319 0.06925 0.00778 0.02000 -0.00334 0.04117 0.00685 0.00018 0.00067 0.00033 0.00586 0.00145 0.00190 0.00356 0.00293 0.00208 0.00123 0.00112 H3_a -0.16906 0.12506 1.09923 0.84269 0.04940 0.00586 0.00000 C4_a -0.14084 0.13809 0.94166 0.84269 0.02210 0.02774 0.06300 -0.00412 0.00985 -0.00573 0.03759 0.00533 0.00014 0.00036 0.00032 0.00586 0.00143 0.00139 0.00223 0.00135 0.00122 0.00105 0.00080 H4_a -0.18258 0.10449 0.88704 0.84269 0.04511 0.00586 0.00000 O5_a -0.07980 0.18188 0.91244 0.84269 0.02071 0.03286 0.04306 -0.00720 0.00217 -0.00358 0.03303 0.00564 0.00015 0.00059 0.00023 0.00586 0.00116 0.00127 0.00157 0.00133 0.00094 0.00090 0.00067 C1B_b -0.02961 0.20363 1.03097 0.15731 0.01722 0.02912 0.02253 0.01355 -0.00662 -0.00270 0.02475 0.06845 0.00144 0.01062 0.00254 0.00586 0.00690 0.01532 0.00796 0.00797 0.00585 0.00858 0.00645 C2B_b -0.08847 0.16795 0.94924 0.15731 0.02921 0.01756 0.03633 -0.01143 0.00966 -0.00670 0.02735 0.04327 0.00126 0.00425 0.00166 0.00586 0.00888 0.00742 0.00813 0.00817 0.00616 0.00640 0.00379 H2B_b -0.09444 0.16851 0.86629 0.15731 0.03282 0.00586 0.00000 C3B_b -0.13973 0.12927 1.01421 0.15731 0.02548 0.03319 0.06925 0.00778 0.02000 -0.00334 0.04117 0.04280 0.00110 0.00528 0.00235 0.00586 0.00145 0.00190 0.00356 0.00293 0.00208 0.00123 0.00112 H3B_b -0.18656 0.09204 0.98316 0.15731 0.04940 0.00586 0.00000 C4B_b -0.10882 0.15580 1.12831 0.15731 0.04613 0.02066 0.06407 0.00832 0.03261 -0.01000 0.04040 0.03656 0.00096 0.00222 0.00170 0.00586 0.00887 0.00667 0.00731 0.00786 0.00688 0.00711 0.00346 H4B_b -0.13084 0.13660 1.19161 0.15731 0.04848 0.00586 0.00000 O5B_b -0.04242 0.21326 1.14053 0.15731 0.04280 0.02888 0.03533 0.00449 0.02149 -0.01101 0.03365 0.02871 0.00090 0.00351 0.00138 0.00586 0.00834 0.00603 0.00733 0.00633 0.00531 0.00748 0.00353 C6 0.03603 0.27749 1.01055 1.00000 0.02294 0.02033 0.02826 0.00248 0.00599 0.00161 0.02382 0.00339 0.00009 0.00025 0.00016 0.00000 0.00094 0.00093 0.00098 0.00073 0.00075 0.00074 0.00041 C8 0.11817 0.34099 0.92014 1.00000 0.01825 0.02264 0.02870 -0.00062 0.00339 -0.00230 0.02352 0.00324 0.00009 0.00025 0.00015 0.00000 0.00090 0.00095 0.00099 0.00075 0.00071 0.00072 0.00041 C9 0.14114 0.37144 1.03873 1.00000 0.01960 0.02340 0.02420 0.00134 0.00330 -0.00078 0.02267 0.00322 0.00009 0.00025 0.00015 0.00000 0.00090 0.00097 0.00094 0.00072 0.00071 0.00073 0.00041 C12 0.20672 0.43884 1.09957 1.00000 0.02435 0.02939 0.02121 0.00098 0.00515 0.00104 0.02499 0.00346 0.00009 0.00027 0.00015 0.00000 0.00102 0.00104 0.00091 0.00074 0.00075 0.00079 0.00042 C21 0.42021 0.16884 1.01059 1.00000 0.02039 0.02039 0.02538 -0.00044 0.00145 0.00162 0.02266 0.00322 0.00009 0.00025 0.00015 0.00000 0.00091 0.00092 0.00095 0.00071 0.00072 0.00071 0.00040 C22 0.39350 0.13843 1.10518 1.00000 0.03974 0.03105 0.02269 -0.00085 0.01065 -0.00017 0.03060 0.00373 0.00010 0.00027 0.00016 0.00000 0.00116 0.00109 0.00096 0.00079 0.00082 0.00088 0.00046 H22 0.41589 0.15628 1.18545 1.00000 0.03672 0.00000 0.00000 C23 0.32369 0.07303 1.05817 1.00000 0.03168 0.03229 0.05943 0.00183 0.02593 -0.00073 0.03864 0.00419 0.00011 0.00030 0.00020 0.00000 0.00114 0.00117 0.00146 0.00098 0.00102 0.00089 0.00053 H23 0.29054 0.03939 1.10213 1.00000 0.04636 0.00000 0.00000 C24 0.31405 0.06829 0.94189 1.00000 0.01822 0.03707 0.05059 0.00188 0.00270 -0.00440 0.03613 0.00388 0.00010 0.00030 0.00019 0.00000 0.00098 0.00118 0.00133 0.00096 0.00086 0.00083 0.00051 H24 0.27224 0.02983 0.88916 1.00000 0.04335 0.00000 0.00000 C26 0.48764 0.23802 1.00320 1.00000 0.02190 0.02103 0.02145 0.00171 0.00474 0.00138 0.02149 0.00325 0.00009 0.00024 0.00015 0.00000 0.00093 0.00095 0.00090 0.00070 0.00071 0.00071 0.00040 C28 0.56721 0.33282 0.91364 1.00000 0.01979 0.02258 0.02470 -0.00248 0.00366 -0.00122 0.02259 0.00323 0.00009 0.00025 0.00015 0.00000 0.00090 0.00095 0.00094 0.00073 0.00070 0.00073 0.00040 C29 0.59159 0.34435 1.03349 1.00000 0.01953 0.02477 0.02099 -0.00084 0.00284 -0.00043 0.02205 0.00319 0.00009 0.00025 0.00015 0.00000 0.00090 0.00096 0.00091 0.00070 0.00070 0.00072 0.00040 C32 0.65843 0.40262 1.09615 1.00000 0.02599 0.02751 0.02209 -0.00040 0.00621 -0.00106 0.02508 0.00349 0.00010 0.00026 0.00015 0.00000 0.00104 0.00100 0.00092 0.00074 0.00077 0.00079 0.00042 O7 0.05070 0.28163 0.90065 1.00000 0.01948 0.02834 0.02638 -0.00289 0.00218 -0.00274 0.02522 0.00220 0.00006 0.00018 0.00010 0.00000 0.00066 0.00072 0.00068 0.00052 0.00050 0.00051 0.00032 N11 0.14571 0.35743 0.82707 1.00000 0.02381 0.04640 0.02629 -0.00786 0.00479 -0.01104 0.03232 0.00312 0.00009 0.00026 0.00014 0.00000 0.00089 0.00109 0.00089 0.00076 0.00070 0.00077 0.00041 N13 0.26028 0.49512 1.14879 1.00000 0.02426 0.04956 0.02896 -0.00169 0.00224 -0.00604 0.03488 0.00301 0.00008 0.00026 0.00014 0.00000 0.00092 0.00111 0.00089 0.00078 0.00070 0.00079 0.00043 O27 0.50055 0.26479 0.89328 1.00000 0.01880 0.02800 0.02115 -0.00117 0.00399 -0.00310 0.02274 0.00213 0.00006 0.00017 0.00010 0.00000 0.00065 0.00070 0.00065 0.00050 0.00048 0.00051 0.00031 N31 0.59216 0.37600 0.82133 1.00000 0.02402 0.04661 0.02024 -0.00317 0.00550 -0.01092 0.03022 0.00308 0.00008 0.00025 0.00013 0.00000 0.00086 0.00108 0.00084 0.00072 0.00066 0.00074 0.00040 N33 0.71308 0.44940 1.14596 1.00000 0.02654 0.04434 0.02882 -0.00137 0.00372 -0.00864 0.03365 0.00298 0.00008 0.00025 0.00014 0.00000 0.00094 0.00107 0.00088 0.00075 0.00071 0.00076 0.00042 N10 0.08710 0.32897 1.09475 1.00000 0.02135 0.02441 0.02694 0.00301 0.00383 0.00004 0.02450 0.00279 0.00008 0.00021 0.00013 0.00000 0.00079 0.00084 0.00081 0.00064 0.00062 0.00063 0.00036 O25 0.37299 0.12676 0.90887 1.00000 0.02564 0.03573 0.03308 -0.00073 0.00146 -0.00358 0.03233 0.00238 0.00007 0.00019 0.00011 0.00000 0.00071 0.00082 0.00075 0.00059 0.00056 0.00058 0.00035 N30 0.53921 0.28234 1.08853 1.00000 0.01962 0.02568 0.02352 0.00095 0.00481 -0.00031 0.02296 0.00271 0.00007 0.00021 0.00013 0.00000 0.00078 0.00082 0.00078 0.00061 0.00061 0.00061 0.00035 H11A 0.12290 0.30813 0.75754 1.00000 0.02755 0.02958 0.00095 0.00265 0.00140 0.00000 0.00000 H11B 0.18785 0.39898 0.83643 1.00000 0.02755 0.03254 0.00082 0.00277 0.00165 0.00000 0.00000 H31A 0.57008 0.33002 0.75089 1.00000 0.02755 0.02956 0.00095 0.00265 0.00139 0.00000 0.00000 H31B 0.63648 0.41202 0.83476 1.00000 0.02755 0.03243 0.00081 0.00274 0.00166 0.00000 0.00000 Final Structure Factor Calculation for 2009src0463p21c in P2(1)/c Total number of l.s. parameters = 287 Maximum vector length = 511 Memory required = 3161 / 22995 wR2 = 0.1206 before cycle 5 for 2769 data and 0 / 287 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 10. 0. 0. 0. 20. 132. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.010 0.040 0.000 0.000 rms deviation 0.000 0.015 0.000 0.009 0.000 0.000 0.000 0.006 0.012 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.006 for 166 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0576 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0436 for 2265 Fo > 4sig(Fo) and 0.0561 for all 2769 data wR2 = 0.1206, GooF = S = 1.035, Restrained GooF = 1.006 for all data Occupancy sum of asymmetric unit = 26.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0361 0.0232 0.0152 C1_a 0.0456 0.0366 0.0303 C2_a 0.0711 0.0343 0.0182 C3_a 0.0639 0.0305 0.0184 C4_a 0.0483 0.0318 0.0190 O5_a 0.0463 0.0196 0.0083 C1B_b 0.0424 0.0281 0.0115 C2B_b 0.0711 0.0343 0.0182 C3B_b 0.0734 0.0389 0.0089 C4B_b 0.0517 0.0362 0.0130 O5B_b 0.0290 0.0232 0.0192 C6 0.0297 0.0236 0.0172 C8 0.0263 0.0224 0.0193 C9 0.0297 0.0242 0.0211 C12 0.0288 0.0209 0.0183 C21 0.0399 0.0311 0.0208 C22 0.0636 0.0325 0.0199 C23 0.0538 0.0374 0.0172 C24 0.0233 0.0220 0.0192 C26 0.0266 0.0222 0.0189 C28 0.0250 0.0226 0.0186 C29 0.0281 0.0255 0.0217 C32 0.0305 0.0274 0.0179 O7 0.0518 0.0267 0.0184 N11 0.0509 0.0321 0.0216 N13 0.0290 0.0215 0.0178 O27 0.0510 0.0201 0.0195 N31 0.0480 0.0305 0.0225 N33 0.0297 0.0228 0.0210 N10 0.0384 0.0356 0.0230 O25 0.0261 0.0232 0.0196 N30 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.022 0.035 0.049 0.063 0.082 0.104 0.139 0.203 1.000 Number in group 291. 265. 275. 296. 266. 272. 276. 276. 276. 276. GooF 0.868 1.016 1.053 1.079 1.039 1.012 0.996 1.091 1.190 0.981 K 1.364 1.042 0.909 0.942 0.977 1.004 0.999 1.010 1.013 1.008 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.26 1.43 1.79 inf Number in group 279. 280. 274. 280. 276. 273. 283. 268. 277. 279. GooF 1.013 1.046 1.013 0.976 0.931 0.792 0.826 0.940 1.006 1.590 K 1.017 1.043 1.010 0.991 0.995 1.010 1.008 1.045 1.052 0.971 R1 0.133 0.106 0.088 0.073 0.051 0.037 0.037 0.042 0.037 0.044 Recommended weighting scheme: WGHT 0.0579 0.8999 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)/su Fc/Fc(max) Resolution(A) -1 1 1 93.58 242.01 7.18 0.120 5.91 0 1 2 285.67 498.36 6.81 0.173 4.42 1 1 0 277.64 619.83 6.56 0.192 6.59 2 1 1 0.98 16.25 4.69 0.031 4.82 11 0 10 24.35 65.24 4.50 0.062 0.87 3 0 0 14.04 37.70 4.01 0.047 6.41 2 1 3 229.98 314.31 3.66 0.137 2.97 5 2 3 125.46 84.21 3.54 0.071 2.00 7 3 8 3.38 19.32 3.51 0.034 1.04 -2 1 5 186.46 134.48 3.47 0.090 2.22 6 8 0 64.69 138.01 3.40 0.091 0.85 2 8 1 55.83 125.78 3.40 0.087 0.87 -22 0 6 705.78 481.89 3.39 0.170 0.87 8 7 0 11.31 37.10 3.24 0.047 0.93 6 0 6 65.20 40.11 3.18 0.049 1.49 1 0 2 254.13 332.68 3.17 0.141 5.15 3 0 2 211.72 280.50 3.16 0.129 3.84 3 3 0 -1.37 6.84 3.16 0.020 2.20 5 0 12 30.49 4.63 3.15 0.017 0.88 17 4 1 0.32 18.67 3.15 0.033 0.93 -4 3 10 8.64 23.99 3.11 0.038 1.05 -18 0 10 13.79 40.90 3.10 0.049 0.89 4 3 1 57.10 35.83 3.04 0.046 2.03 -2 3 2 132.34 178.08 2.97 0.103 2.15 6 0 2 49.15 75.53 2.96 0.067 2.55 1 2 3 15.73 6.36 2.90 0.019 2.50 -1 1 3 378.30 471.82 2.89 0.168 3.41 0 1 12 20.39 42.85 2.88 0.051 0.94 2 1 2 2696.80 3234.69 2.88 0.440 3.77 0 1 4 752.08 622.98 2.79 0.193 2.64 4 2 4 243.18 190.50 2.76 0.107 1.89 0 2 3 2025.62 2412.05 2.75 0.380 2.58 7 2 2 305.43 242.13 2.73 0.120 1.91 2 1 0 632.11 770.92 2.63 0.215 5.67 -14 0 10 84.54 52.41 2.63 0.056 1.00 -11 1 12 7.60 21.37 2.63 0.036 0.92 0 4 6 345.83 280.21 2.63 0.129 1.29 4 0 2 912.16 1097.76 2.62 0.256 3.32 9 1 1 36.90 22.65 2.61 0.037 1.94 7 1 0 135.16 103.27 2.53 0.079 2.56 -2 1 1 412.70 500.82 2.53 0.173 5.37 6 7 1 24.64 1.91 2.53 0.011 0.95 7 0 0 383.86 307.95 2.52 0.136 2.75 13 2 5 23.85 39.34 2.50 0.048 1.07 -15 3 7 14.41 28.77 2.50 0.041 1.03 -1 0 4 88.07 64.31 2.49 0.062 2.91 9 3 4 60.87 41.55 2.48 0.050 1.29 -5 3 3 383.71 463.83 2.48 0.167 1.86 -4 1 2 117.44 89.76 2.48 0.073 3.59 4 1 2 494.31 593.05 2.45 0.188 3.00 Bond lengths and angles C1_a - Distance Angles C2_a 1.3495 (0.0060) O5_a 1.3659 (0.0055) 110.58 (0.37) C6 1.4416 (0.0050) 131.26 (0.49) 118.15 (0.41) C1_a - C2_a O5_a C2_a - Distance Angles C1_a 1.3495 (0.0060) C3_a 1.4242 (0.0051) 105.58 (0.37) H2_a 0.9500 127.21 127.21 C2_a - C1_a C3_a C3_a - Distance Angles C4_a 1.3330 (0.0048) C2_a 1.4242 (0.0051) 107.14 (0.33) H3_a 0.9500 126.43 126.43 C3_a - C4_a C2_a C4_a - Distance Angles C3_a 1.3330 (0.0048) O5_a 1.3614 (0.0035) 110.55 (0.26) H4_a 0.9500 124.73 124.73 C4_a - C3_a O5_a O5_a - Distance Angles C4_a 1.3614 (0.0035) C1_a 1.3659 (0.0055) 106.12 (0.28) O5_a - C4_a C1B_b - Distance Angles C2B_b 1.3491 (0.0195) O5B_b 1.3631 (0.0208) 111.09 (1.55) C6 1.4658 (0.0248) 126.98 (2.39) 119.79 (2.29) C1B_b - C2B_b O5B_b C2B_b - Distance Angles C1B_b 1.3491 (0.0196) C3B_b 1.4238 (0.0172) 105.09 (1.48) H2B_b 0.9500 127.45 127.45 C2B_b - C1B_b C3B_b C3B_b - Distance Angles C4B_b 1.3473 (0.0180) C2B_b 1.4238 (0.0171) 106.58 (1.44) H3B_b 0.9500 126.71 126.71 C3B_b - C4B_b C2B_b C4B_b - Distance Angles C3B_b 1.3473 (0.0180) O5B_b 1.3482 (0.0154) 110.86 (1.36) H4B_b 0.9500 124.57 124.57 C4B_b - C3B_b O5B_b O5B_b - Distance Angles C4B_b 1.3482 (0.0154) C1B_b 1.3631 (0.0209) 105.70 (1.38) O5B_b - C4B_b C6 - Distance Angles N10 1.2899 (0.0023) O7 1.3807 (0.0021) 114.24 (0.15) C1_a 1.4416 (0.0050) 129.09 (0.29) 116.63 (0.28) C1B_b 1.4658 (0.0252) 122.78 (1.12) 122.73 (1.15) 9.00 (2.61) C6 - N10 O7 C1_a C8 - Distance Angles N11 1.3282 (0.0024) O7 1.3649 (0.0021) 117.19 (0.15) C9 1.3737 (0.0025) 135.31 (0.17) 107.50 (0.15) C8 - N11 O7 C9 - Distance Angles C8 1.3737 (0.0025) N10 1.4060 (0.0023) 109.06 (0.15) C12 1.4096 (0.0025) 127.97 (0.16) 122.96 (0.16) C9 - C8 N10 C12 - Distance Angles N13 1.1525 (0.0023) C9 1.4096 (0.0025) 179.49 (0.21) C12 - N13 C21 - Distance Angles C22 1.3468 (0.0025) O25 1.3657 (0.0021) 111.30 (0.16) C26 1.4388 (0.0025) 130.14 (0.17) 118.56 (0.15) C21 - C22 O25 C22 - Distance Angles C21 1.3468 (0.0025) C23 1.4381 (0.0029) 104.95 (0.17) H22 0.9500 127.52 127.52 C22 - C21 C23 C23 - Distance Angles C24 1.3296 (0.0030) C22 1.4381 (0.0029) 107.43 (0.17) H23 0.9500 126.28 126.28 C23 - C24 C22 C24 - Distance Angles C23 1.3296 (0.0030) O25 1.3704 (0.0024) 110.38 (0.17) H24 0.9500 124.81 124.81 C24 - C23 O25 C26 - Distance Angles N30 1.2907 (0.0022) O27 1.3791 (0.0020) 113.97 (0.15) C21 1.4388 (0.0025) 127.80 (0.16) 118.23 (0.15) C26 - N30 O27 C28 - Distance Angles N31 1.3202 (0.0023) O27 1.3694 (0.0021) 117.49 (0.15) C29 1.3762 (0.0024) 135.23 (0.17) 107.24 (0.15) C28 - N31 O27 C29 - Distance Angles C28 1.3762 (0.0024) N30 1.4067 (0.0023) 108.96 (0.15) C32 1.4160 (0.0025) 127.72 (0.16) 123.30 (0.15) C29 - C28 N30 C32 - Distance Angles N33 1.1511 (0.0023) C29 1.4160 (0.0025) 179.19 (0.20) C32 - N33 O7 - Distance Angles C8 1.3649 (0.0021) C6 1.3807 (0.0021) 104.82 (0.13) O7 - C8 N11 - Distance Angles C8 1.3282 (0.0024) H11A 0.9035 (0.0146) 119.37 (1.25) H11B 0.8650 (0.0147) 119.22 (1.29) 120.71 (1.78) N11 - C8 H11A N13 - Distance Angles C12 1.1525 (0.0023) N13 - O27 - Distance Angles C28 1.3694 (0.0021) C26 1.3791 (0.0020) 105.12 (0.13) O27 - C28 N31 - Distance Angles C28 1.3202 (0.0023) H31A 0.8992 (0.0145) 118.24 (1.27) H31B 0.8902 (0.0148) 117.18 (1.26) 121.00 (1.78) N31 - C28 H31A N33 - Distance Angles C32 1.1511 (0.0023) N33 - N10 - Distance Angles C6 1.2899 (0.0023) C9 1.4060 (0.0023) 104.39 (0.15) N10 - C6 O25 - Distance Angles C21 1.3657 (0.0021) C24 1.3704 (0.0024) 105.93 (0.15) O25 - C21 N30 - Distance Angles C26 1.2907 (0.0022) C29 1.4067 (0.0023) 104.72 (0.14) N30 - C26 Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.904(15) 2.106(15) 2.999(2) 169.7(17) N11-H11A...N10_$1 0.865(15) 2.195(15) 3.052(2) 170.6(18) N11-H11B...N33_$2 0.899(14) 2.017(15) 2.905(2) 168.9(18) N31-H31A...N30_$1 0.890(15) 2.107(15) 2.995(2) 175.0(18) N31-H31B...N13_$2 FMAP and GRID set by program FMAP 2 2 18 GRID 21.667 -2 -1 3.333 2 1 R1 = 0.0561 for 2769 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.25 at 0.4103 0.7172 0.0224 [ 0.78 A from C29 ] Deepest hole -0.31 at 0.3225 0.4411 0.3809 [ 0.77 A from C24 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3380 / 26343 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5897 0.2828 0.9776 1.00000 0.05 0.25 0.78 C29 0.85 C28 1.81 N30 1.82 O27 Q2 1 0.3599 0.0953 1.1161 1.00000 0.05 0.25 0.77 C22 0.88 C23 1.29 H22 1.40 H23 Q3 1 0.4133 0.1275 1.1337 1.00000 0.05 0.25 0.46 C22 0.63 H22 1.50 C21 1.83 C23 Q4 1 0.2830 0.0310 0.8522 1.00000 0.05 0.19 0.52 H24 1.12 C24 1.87 O25 2.33 N13 Q5 1 0.5693 0.4134 0.9835 1.00000 0.05 0.19 0.81 C29 0.99 C28 1.74 N30 1.84 O27 Q6 1 -0.1863 0.1104 0.8149 1.00000 0.05 0.18 0.83 H4 1.56 C4 1.82 H2B 1.97 H3B Q7 1 0.1388 0.3138 0.9895 1.00000 0.05 0.18 0.70 C9 0.84 C8 1.77 N10 1.83 O7 Q8 1 0.4487 0.2400 1.0181 1.00000 0.05 0.18 0.74 C21 0.83 C26 1.80 C22 1.81 N30 Q9 1 0.3090 0.1343 1.0075 1.00000 0.05 0.18 0.74 C23 0.92 C24 1.41 H23 1.59 H24 Q10 1 0.6823 0.4481 0.9845 1.00000 0.05 0.17 1.52 C32 1.80 H31B 1.85 N33 2.13 C29 Shortest distances between peaks (including symmetry equivalents) 1 5 1.01 2 3 1.05 2 9 1.46 3 8 1.84 4 9 1.91 1 10 2.15 5 10 2.24 3 9 2.25 5 8 2.46 2 8 2.52 5 8 2.79 8 9 2.83 9 10 2.94 1 8 2.94 Time profile in seconds ----------------------- 0.05: 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. 1.02: 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 0.72: Structure factors and derivatives 1.44: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.25: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0463p21c finished at 13:17:00 Total CPU time: 3.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++