+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04skc0003p1 started at 12:22:26 on 14-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04skc0003p1 in P-1 CELL 0.71073 9.3454 9.3736 17.6236 78.408 78.446 89.855 ZERR 2.00 0.0019 0.0019 0.0035 0.030 0.030 0.030 LATT 1 SFAC C H N O UNIT 48 102 2 28 V = 1480.55 F(000) = 628.0 Mu = 0.11 mm-1 Cell Wt = 1155.32 Rho = 1.296 MERG 2 OMIT -3.00 55.00 EXTI 0.03952 SHEL 7 0.77 DFIX 0.84 0.02 O1W H11W O1W H12W O2W H21W O2W H22W DANG 1.35 0.02 H11W H12W H21W H22W HTAB O24A O1W HTAB O2W O1B EQIV_$1 -x+1, -y, -z HTAB O2 O4B_$1 EQIV_$2 -x+1, -y+1, -z HTAB O4A O2W_$2 EQIV_$3 -x, -y+2, -z+1 HTAB O21A O21A_$3 EQIV_$4 -x, -y+1, -z+1 HTAB O22 O24B_$4 HTAB O23 O22_$4 EQIV_$5 x, y-1, z HTAB O1W O21B_$5 EQIV_$6 -x+1, -y+1, -z+1 HTAB O1W O21B_$6 EQIV_$7 -x, -y+1, -z HTAB O2W O1B_$7 FMAP 2 PLAN 15 SIZE 0.03 0.12 0.20 ACTA 50.00 BOND $H WGHT 0.12780 L.S. 8 TEMP -153.00 FVAR 0.15795 0.68918 MOLE 1 C1 1 0.162688 0.176623 -0.011551 11.00000 0.02553 0.01738 = 0.02445 -0.00212 -0.00967 0.00058 C2 1 0.325872 0.210359 -0.029431 11.00000 0.02322 0.01888 = 0.02157 0.00055 -0.00109 0.00297 AFIX 13 H2 2 0.345990 0.309790 -0.063847 11.00000 -1.20000 AFIX 0 C3 1 0.379459 0.209704 0.047754 11.00000 0.01734 0.01920 = 0.02890 -0.00428 -0.00124 0.00008 AFIX 13 H3 2 0.325170 0.286436 0.072468 11.00000 -1.20000 AFIX 0 C4 1 0.538291 0.252208 0.033046 11.00000 0.02771 0.02533 = 0.02913 -0.00943 -0.01071 0.00071 O1A 4 0.127883 0.049042 -0.021787 11.00000 0.02074 0.03050 = 0.03421 -0.01122 -0.00776 -0.00467 AFIX 87 H1 2 0.036645 0.035429 -0.009521 10.50000 0.03044 AFIX 0 O1B 4 0.078837 0.266092 0.011934 11.00000 0.02582 0.02230 = 0.03269 -0.00767 -0.00674 0.00133 O2 4 0.408169 0.108080 -0.069337 11.00000 0.02573 0.03286 = 0.02798 -0.01692 -0.00709 0.00432 AFIX 147 H2A 2 0.363211 0.085304 -0.102218 11.00000 -1.50000 AFIX 0 O3 4 0.342008 0.078038 0.101454 11.00000 0.02329 0.02827 = 0.02930 -0.00274 -0.00337 0.00199 AFIX 147 H3A 2 0.408901 0.019313 0.093972 11.00000 -1.50000 AFIX 0 O4A 4 0.579249 0.368572 -0.022818 11.00000 0.02254 0.03358 = 0.04338 0.00199 -0.00865 -0.00789 AFIX 147 H4 2 0.663544 0.397065 -0.021224 11.00000 -1.50000 AFIX 0 O4B 4 0.621009 0.186503 0.072241 11.00000 0.02293 0.03283 = 0.04855 -0.00330 -0.01754 0.00032 MOLE 2 C21 1 0.174768 0.843890 0.489228 11.00000 0.02113 0.02088 = 0.02208 -0.00462 -0.01052 0.00122 O21A 4 0.048574 0.887661 0.479955 11.00000 0.02723 0.02472 = 0.03413 -0.00835 -0.00724 0.00134 AFIX 147 H21 2 0.032726 0.965198 0.496709 10.50000 -1.50000 AFIX 0 O21B 4 0.266089 0.908605 0.513222 11.00000 0.02973 0.02336 = 0.03132 -0.00397 -0.00976 -0.00439 C22 1 0.208076 0.692983 0.471596 11.00000 0.01945 0.02322 = 0.02732 -0.00405 0.00057 0.00317 AFIX 13 H22 2 0.307974 0.698053 0.437422 11.00000 -1.20000 AFIX 0 O22 4 0.107844 0.643630 0.431628 11.00000 0.02776 0.02342 = 0.03319 -0.00998 -0.01136 0.00425 AFIX 147 H22O 2 0.034667 0.696008 0.434249 11.00000 -1.50000 AFIX 0 C23 1 0.208374 0.583920 0.550013 11.00000 0.02217 0.02404 = 0.02582 -0.00559 -0.00258 -0.00044 AFIX 13 H23 2 0.284890 0.619878 0.574745 11.00000 -1.20000 AFIX 0 O23 4 0.075948 0.578036 0.603042 11.00000 0.03586 0.02451 = 0.02558 -0.00748 -0.00216 0.00003 AFIX 147 H23O 2 0.021586 0.511092 0.597669 11.00000 -1.50000 AFIX 0 C24 1 0.251567 0.431543 0.534680 11.00000 0.02163 0.02716 = 0.03245 -0.00708 -0.01290 0.00315 O24A 4 0.368257 0.438274 0.477108 11.00000 0.03664 0.02075 = 0.04654 -0.00658 -0.00303 0.00820 AFIX 147 H24O 2 0.410873 0.359030 0.483271 11.00000 -1.50000 AFIX 0 O24B 4 0.187112 0.323204 0.573539 11.00000 0.03786 0.02243 = 0.04318 0.00461 -0.00029 0.00081 MOLE 3 C32A 1 0.764174 0.009745 0.303474 11.00000 0.01976 0.01920 = 0.02119 0.00169 0.00474 -0.00769 AFIX 23 H32G 2 0.720456 0.071510 0.340841 11.00000 -1.20000 H32H 2 0.792475 -0.081700 0.335022 11.00000 -1.20000 AFIX 0 C32B 1 0.975852 -0.005780 0.193894 11.00000 0.01622 0.01740 = 0.02097 -0.01027 -0.00208 0.00162 AFIX 23 H32A 2 1.063630 0.049258 0.159810 11.00000 -1.20000 H32B 2 0.909034 -0.022237 0.159156 11.00000 -1.20000 AFIX 0 C32C 1 0.998790 0.118226 0.304465 11.00000 0.01763 0.02467 = 0.02629 -0.00463 -0.00324 0.00015 AFIX 23 H32C 2 1.020916 0.024076 0.336106 11.00000 -1.20000 H32D 2 0.944271 0.174979 0.341780 11.00000 -1.20000 AFIX 0 C32D 1 0.863586 0.228144 0.197831 11.00000 0.02482 0.02202 = 0.01897 -0.00318 -0.00658 0.00250 AFIX 23 H32E 2 0.954873 0.272772 0.162096 11.00000 -1.20000 H32F 2 0.797668 0.203154 0.164511 11.00000 -1.20000 AFIX 0 C33A 1 0.649141 -0.026974 0.259941 11.00000 0.02248 0.01808 = 0.02456 -0.00421 -0.00546 0.00050 AFIX 23 H33G 2 0.691839 -0.087791 0.221856 11.00000 -1.20000 H33H 2 0.617019 0.063977 0.229775 11.00000 -1.20000 AFIX 0 C33B 1 1.022256 -0.153481 0.234013 11.00000 0.02484 0.02469 = 0.02740 -0.00154 -0.00079 0.00249 AFIX 23 H33A 2 1.092588 -0.138790 0.267209 11.00000 -1.20000 H33B 2 0.935742 -0.209547 0.268823 11.00000 -1.20000 AFIX 0 C33C 1 1.142554 0.200468 0.263443 11.00000 0.02189 0.02272 = 0.02757 -0.00409 -0.00702 -0.00398 AFIX 23 H33C 2 1.197275 0.146183 0.224909 11.00000 -1.20000 H33D 2 1.122093 0.297235 0.233867 11.00000 -1.20000 AFIX 0 C33D 1 0.792735 0.337840 0.242600 11.00000 0.02372 0.02271 = 0.02344 -0.00404 -0.00400 -0.00166 AFIX 23 H33E 2 0.859322 0.365656 0.274843 11.00000 -1.20000 H33F 2 0.702058 0.293525 0.279075 11.00000 -1.20000 AFIX 0 C34A 1 0.517457 -0.108953 0.317973 11.00000 0.02504 0.03074 = 0.02313 0.00063 -0.00595 -0.00815 AFIX 23 H34C 2 0.549302 -0.201235 0.346977 11.00000 -1.20000 H34D 2 0.476903 -0.049336 0.357081 11.00000 -1.20000 AFIX 0 C34B 1 1.092324 -0.238374 0.172648 11.00000 0.03447 0.02271 = 0.02806 -0.01034 -0.00084 0.00318 AFIX 23 H34E 2 1.177873 -0.181364 0.137427 11.00000 -1.20000 H34F 2 1.021442 -0.253642 0.139864 11.00000 -1.20000 AFIX 0 C34C 1 1.235490 0.220334 0.321815 11.00000 0.01745 0.03729 = 0.03946 -0.01455 -0.00908 0.00255 AFIX 23 H34A 2 1.180768 0.274485 0.360416 11.00000 -1.20000 H34B 2 1.256222 0.123592 0.351307 11.00000 -1.20000 AFIX 0 C34D 1 0.755969 0.473166 0.187865 11.00000 0.02787 0.02022 = 0.02978 -0.00381 -0.00926 -0.00010 AFIX 23 H34G 2 0.846373 0.516137 0.150625 11.00000 -1.20000 H34H 2 0.687788 0.445498 0.156432 11.00000 -1.20000 AFIX 0 C35A 1 0.400310 -0.142078 0.275686 11.00000 0.02214 0.03384 = 0.03506 -0.00652 -0.00532 -0.00050 AFIX 137 H35D 2 0.369415 -0.050901 0.246472 11.00000 -1.20000 H35E 2 0.316359 -0.192110 0.314439 11.00000 -1.20000 H35F 2 0.438987 -0.204759 0.238654 11.00000 -1.20000 AFIX 0 C35B 1 1.141565 -0.386739 0.211742 11.00000 0.03731 0.02659 = 0.04290 -0.01260 -0.00389 0.00327 AFIX 137 H35J 2 1.209652 -0.371901 0.245382 11.00000 -1.20000 H35K 2 1.190328 -0.437350 0.170712 11.00000 -1.20000 H35L 2 1.056130 -0.445626 0.244074 11.00000 -1.20000 AFIX 0 C35C 1 1.377531 0.302056 0.280988 11.00000 0.03077 0.03409 = 0.04203 -0.00627 -0.01241 0.00203 AFIX 137 H35G 2 1.435807 0.244502 0.246239 11.00000 -1.20000 H35H 2 1.431861 0.319106 0.320685 11.00000 -1.20000 H35I 2 1.357365 0.395745 0.249471 11.00000 -1.20000 AFIX 0 C35D 1 0.687061 0.586107 0.232720 11.00000 0.04688 0.02297 = 0.03751 -0.00704 -0.00886 0.00848 AFIX 137 H35A 2 0.592087 0.547860 0.265275 11.00000 -1.20000 H35B 2 0.673371 0.674904 0.195103 11.00000 -1.20000 H35C 2 0.751096 0.608709 0.266835 11.00000 -1.20000 AFIX 0 N31 3 0.899999 0.087664 0.250516 11.00000 0.02259 0.01967 = 0.01943 -0.00167 -0.00241 0.00120 MOLE 4 O1W 4 0.453744 0.176224 0.464942 11.00000 0.02422 0.02127 = 0.04870 -0.00617 -0.01186 0.00332 H11W 2 0.381401 0.118262 0.483982 11.00000 0.00896 H12W 2 0.528942 0.144413 0.477409 11.00000 -1.20000 MOLE 5 O2W 4 0.153367 0.545862 0.029243 11.00000 0.02739 0.02940 = 0.05080 -0.01143 -0.01516 0.00026 H21W 2 0.125509 0.478124 0.010088 11.00000 0.06146 H22W 2 0.110983 0.621527 0.013649 11.00000 0.03077 HKLF 4 Covalent radii and connectivity table for 04skc0003p1 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - O2 C1 C3 C3 - O3 C4 C2 C4 - O4B O4A C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C21 - O21B O21A C22 O21A - C21 O21B - C21 C22 - O22 C21 C23 O22 - C22 C23 - O23 C24 C22 O23 - C23 C24 - O24B O24A C23 O24A - C24 O24B - C24 C32A - N31 C33A C32B - N31 C33B C32C - N31 C33C C32D - C33D N31 C33A - C32A C34A C33B - C34B C32B C33C - C34C C32C C33D - C32D C34D C34A - C35A C33A C34B - C33B C35B C34C - C35C C33C C34D - C35D C33D C35A - C34A C35B - C34B C35C - C34C C35D - C34D N31 - C32A C32C C32B C32D O1W - no bonds found O2W - no bonds found Operators for generating equivalent atoms: $1 -x+1, -y, -z $2 -x+1, -y+1, -z $3 -x, -y+2, -z+1 $4 -x, -y+1, -z+1 $5 x, y-1, z $6 -x+1, -y+1, -z+1 $7 -x, -y+1, -z 12222 Reflections read, of which 34 rejected -11 =< h =< 11, -12 =< k =< 10, -22 =< l =< 22, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 1 5 63.76 5.15 2 27.58 1 Inconsistent equivalents 5375 Unique reflections, of which 0 suppressed R(int) = 0.1272 R(sigma) = 0.2821 Friedel opposites merged Maximum memory for data reduction = 4541 / 55528 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 = 5703 / 487316 wR2 = 0.2993 before cycle 1 for 5375 data and 382 / 382 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. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.022 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.982; Restrained GooF = 0.981 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1278 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15795 0.00091 -0.002 OSF 2 0.68918 9.99999 0.000 FVAR 2 3 0.03951 0.00766 -0.001 EXTI Mean shift/esd = 0.001 Maximum = -0.003 for U22 O24B Max. shift = 0.000 A for H12W Max. dU = 0.000 for H11W Least-squares cycle 2 Maximum vector length = 511 Memory required = 5703 / 487316 wR2 = 0.2993 before cycle 2 for 5375 data and 382 / 382 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. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.022 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.982; Restrained GooF = 0.981 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1278 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15795 0.00091 -0.002 OSF 2 0.68918 9.99999 0.000 FVAR 2 3 0.03951 0.00766 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for OSF Max. shift = 0.000 A for H21 Max. dU = 0.000 for H11W Least-squares cycle 3 Maximum vector length = 511 Memory required = 5703 / 487316 wR2 = 0.2993 before cycle 3 for 5375 data and 382 / 382 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. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.022 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.982; Restrained GooF = 0.981 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1278 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15795 0.00091 -0.001 OSF 2 0.68918 9.99999 0.000 FVAR 2 3 0.03950 0.00766 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for EXTI Max. shift = 0.000 A for H21 Max. dU = 0.000 for H1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5703 / 487316 wR2 = 0.2993 before cycle 4 for 5375 data and 382 / 382 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. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.022 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.982; Restrained GooF = 0.981 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1278 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15795 0.00091 0.000 OSF 2 0.68918 9.99999 0.000 FVAR 2 3 0.03950 0.00766 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for EXTI Max. shift = 0.000 A for H21 Max. dU = 0.000 for H1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 5703 / 487316 wR2 = 0.2993 before cycle 5 for 5375 data and 382 / 382 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. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.022 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.982; Restrained GooF = 0.981 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1278 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15795 0.00091 0.000 OSF 2 0.68918 9.99999 0.000 FVAR 2 3 0.03950 0.00766 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for EXTI Max. shift = 0.000 A for H23O Max. dU = 0.000 for H1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 5703 / 487316 wR2 = 0.2993 before cycle 6 for 5375 data and 382 / 382 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.022 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.982; Restrained GooF = 0.981 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1278 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15795 0.00091 0.000 OSF 2 0.68918 9.99999 0.000 FVAR 2 3 0.03950 0.00766 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H4 Max. dU = 0.000 for H1 Least-squares cycle 7 Maximum vector length = 511 Memory required = 5703 / 487316 wR2 = 0.2993 before cycle 7 for 5375 data and 382 / 382 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.022 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.982; Restrained GooF = 0.981 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1278 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15795 0.00091 0.000 OSF 2 0.68918 9.99999 0.000 FVAR 2 3 0.03950 0.00766 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O23 Max. shift = 0.000 A for H2A Max. dU = 0.000 for H1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 5703 / 487316 wR2 = 0.2993 before cycle 8 for 5375 data and 382 / 382 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.022 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.982; Restrained GooF = 0.981 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1278 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15795 0.00091 0.000 OSF 2 0.68918 9.99999 0.000 FVAR 2 3 0.03950 0.00766 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O23 Max. shift = 0.000 A for H23O Max. dU = 0.000 for H1 Largest correlation matrix elements -0.746 z H21W / y H21W -0.629 z H12W / x H12W 0.587 EXTI / OSF 0.713 y H22W / x H22W -0.615 y H11W / x H11W -0.566 z H22W / x H22W -0.636 z H21W / x H21W 0.604 x H12W / x H11W 0.554 y H22W / y H21W Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.3460 0.3098 -0.0638 13 1.000 0.000 C2 O2 C1 C3 H3 0.3252 0.2864 0.0725 13 1.000 0.000 C3 O3 C4 C2 H1 0.0366 0.0354 -0.0095 87 0.840 0.000 O1A C1 H1 H2A 0.3632 0.0853 -0.1022 147 0.840 0.000 O2 C2 H2A H3A 0.4089 0.0193 0.0940 147 0.840 0.000 O3 C3 H3A H4 0.6635 0.3971 -0.0212 147 0.840 0.000 O4A C4 H4 H21 0.0327 0.9652 0.4967 147 0.840 0.000 O21A C21 H21 H22 0.3080 0.6981 0.4374 13 1.000 0.000 C22 O22 C21 C23 H22O 0.0347 0.6960 0.4343 147 0.840 0.000 O22 C22 H22O H23 0.2849 0.6199 0.5747 13 1.000 0.000 C23 O23 C24 C22 H23O 0.0216 0.5111 0.5977 147 0.840 0.000 O23 C23 H23O H24O 0.4109 0.3590 0.4833 147 0.840 0.000 O24A C24 H24O H32G 0.7205 0.0715 0.3408 23 0.990 0.000 C32A N31 C33A H32H 0.7925 -0.0817 0.3350 23 0.990 0.000 C32A N31 C33A H32A 1.0636 0.0493 0.1598 23 0.990 0.000 C32B N31 C33B H32B 0.9090 -0.0222 0.1592 23 0.990 0.000 C32B N31 C33B H32C 1.0209 0.0241 0.3361 23 0.990 0.000 C32C N31 C33C H32D 0.9443 0.1750 0.3418 23 0.990 0.000 C32C N31 C33C H32E 0.9549 0.2728 0.1621 23 0.990 0.000 C32D C33D N31 H32F 0.7977 0.2032 0.1645 23 0.990 0.000 C32D C33D N31 H33G 0.6918 -0.0878 0.2219 23 0.990 0.000 C33A C32A C34A H33H 0.6170 0.0640 0.2298 23 0.990 0.000 C33A C32A C34A H33A 1.0926 -0.1388 0.2672 23 0.990 0.000 C33B C34B C32B H33B 0.9357 -0.2096 0.2688 23 0.990 0.000 C33B C34B C32B H33C 1.1973 0.1462 0.2249 23 0.990 0.000 C33C C34C C32C H33D 1.1221 0.2972 0.2339 23 0.990 0.000 C33C C34C C32C H33E 0.8593 0.3657 0.2748 23 0.990 0.000 C33D C32D C34D H33F 0.7021 0.2935 0.2791 23 0.990 0.000 C33D C32D C34D H34C 0.5493 -0.2012 0.3470 23 0.990 0.000 C34A C35A C33A H34D 0.4769 -0.0493 0.3571 23 0.990 0.000 C34A C35A C33A H34E 1.1779 -0.1814 0.1374 23 0.990 0.000 C34B C33B C35B H34F 1.0214 -0.2536 0.1399 23 0.990 0.000 C34B C33B C35B H34A 1.1808 0.2745 0.3604 23 0.990 0.000 C34C C35C C33C H34B 1.2562 0.1236 0.3513 23 0.990 0.000 C34C C35C C33C H34G 0.8464 0.5161 0.1506 23 0.990 0.000 C34D C35D C33D H34H 0.6878 0.4455 0.1564 23 0.990 0.000 C34D C35D C33D H35D 0.3694 -0.0509 0.2465 137 0.980 0.000 C35A C34A H35D H35E 0.3164 -0.1921 0.3144 137 0.980 0.000 C35A C34A H35D H35F 0.4390 -0.2048 0.2387 137 0.980 0.000 C35A C34A H35D H35J 1.2096 -0.3719 0.2454 137 0.980 0.000 C35B C34B H35J H35K 1.1903 -0.4374 0.1707 137 0.980 0.000 C35B C34B H35J H35L 1.0561 -0.4456 0.2441 137 0.980 0.000 C35B C34B H35J H35G 1.4358 0.2445 0.2462 137 0.980 0.000 C35C C34C H35G H35H 1.4319 0.3191 0.3207 137 0.980 0.000 C35C C34C H35G H35I 1.3574 0.3957 0.2495 137 0.980 0.000 C35C C34C H35G H35A 0.5921 0.5479 0.2653 137 0.980 0.000 C35D C34D H35A H35B 0.6734 0.6749 0.1951 137 0.980 0.000 C35D C34D H35A H35C 0.7511 0.6087 0.2668 137 0.980 0.000 C35D C34D H35A 04skc0003p1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.16269 0.17662 -0.01155 1.00000 0.02553 0.01737 0.02445 -0.00212 -0.00967 0.00058 0.02211 0.00883 0.00067 0.00058 0.00032 0.00000 0.00330 0.00280 0.00288 0.00235 0.00250 0.00252 0.00128 C2 0.32587 0.21036 -0.02943 1.00000 0.02322 0.01888 0.02157 0.00055 -0.00110 0.00297 0.02239 0.00924 0.00064 0.00059 0.00032 0.00000 0.00326 0.00274 0.00275 0.00227 0.00239 0.00246 0.00127 H2 0.34599 0.30979 -0.06385 1.00000 0.02687 0.00000 0.00000 C3 0.37946 0.20970 0.04775 1.00000 0.01735 0.01920 0.02889 -0.00428 -0.00123 0.00008 0.02240 0.00889 0.00063 0.00059 0.00033 0.00000 0.00308 0.00278 0.00301 0.00239 0.00246 0.00236 0.00126 H3 0.32517 0.28644 0.07247 1.00000 0.02688 0.00000 0.00000 C4 0.53829 0.25221 0.03305 1.00000 0.02772 0.02533 0.02913 -0.00943 -0.01071 0.00071 0.02614 0.00890 0.00068 0.00062 0.00034 0.00000 0.00353 0.00310 0.00310 0.00267 0.00275 0.00268 0.00138 O1A 0.12788 0.04904 -0.02179 1.00000 0.02074 0.03050 0.03421 -0.01122 -0.00776 -0.00467 0.02751 0.00609 0.00046 0.00043 0.00025 0.00000 0.00253 0.00231 0.00229 0.00188 0.00191 0.00183 0.00097 H1 0.03665 0.03543 -0.00952 0.50000 0.03044 0.00000 0.03754 O1B 0.07884 0.26609 0.01193 1.00000 0.02582 0.02230 0.03268 -0.00767 -0.00674 0.00133 0.02653 0.00622 0.00046 0.00041 0.00024 0.00000 0.00235 0.00203 0.00218 0.00179 0.00180 0.00186 0.00096 O2 0.40817 0.10808 -0.06934 1.00000 0.02574 0.03285 0.02797 -0.01692 -0.00709 0.00432 0.02710 0.00639 0.00046 0.00043 0.00023 0.00000 0.00238 0.00228 0.00214 0.00182 0.00176 0.00190 0.00098 H2A 0.36321 0.08530 -0.10222 1.00000 0.04066 0.00000 0.00000 O3 0.34201 0.07804 0.10145 1.00000 0.02330 0.02826 0.02929 -0.00274 -0.00337 0.00199 0.02768 0.00657 0.00044 0.00042 0.00023 0.00000 0.00239 0.00221 0.00215 0.00180 0.00183 0.00183 0.00099 H3A 0.40890 0.01931 0.09398 1.00000 0.04153 0.00000 0.00000 O4A 0.57925 0.36857 -0.02282 1.00000 0.02254 0.03358 0.04337 0.00199 -0.00865 -0.00789 0.03428 0.00699 0.00049 0.00046 0.00026 0.00000 0.00242 0.00243 0.00256 0.00211 0.00200 0.00195 0.00108 H4 0.66354 0.39706 -0.02123 1.00000 0.05142 0.00000 0.00000 O4B 0.62101 0.18650 0.07224 1.00000 0.02293 0.03283 0.04855 -0.00330 -0.01754 0.00032 0.03403 0.00667 0.00048 0.00045 0.00027 0.00000 0.00236 0.00236 0.00259 0.00204 0.00207 0.00192 0.00106 C21 0.17477 0.84389 0.48923 1.00000 0.02113 0.02087 0.02208 -0.00462 -0.01052 0.00122 0.02046 0.00873 0.00065 0.00058 0.00032 0.00000 0.00318 0.00273 0.00272 0.00231 0.00239 0.00241 0.00122 O21A 0.04857 0.88766 0.47995 1.00000 0.02723 0.02471 0.03413 -0.00834 -0.00724 0.00134 0.02822 0.00630 0.00046 0.00041 0.00024 0.00000 0.00255 0.00217 0.00232 0.00183 0.00192 0.00182 0.00100 H21 0.03272 0.96520 0.49671 0.50000 0.04233 0.00000 0.00000 O21B 0.26609 0.90860 0.51322 1.00000 0.02973 0.02335 0.03131 -0.00396 -0.00976 -0.00439 0.02785 0.00634 0.00047 0.00041 0.00024 0.00000 0.00248 0.00206 0.00219 0.00177 0.00188 0.00181 0.00098 C22 0.20808 0.69298 0.47160 1.00000 0.01945 0.02322 0.02732 -0.00404 0.00057 0.00317 0.02425 0.00948 0.00066 0.00060 0.00034 0.00000 0.00321 0.00288 0.00298 0.00244 0.00250 0.00246 0.00130 H22 0.30797 0.69805 0.43742 1.00000 0.02910 0.00000 0.00000 O22 0.10784 0.64363 0.43163 1.00000 0.02776 0.02342 0.03318 -0.00998 -0.01136 0.00425 0.02680 0.00611 0.00047 0.00041 0.00024 0.00000 0.00246 0.00207 0.00216 0.00179 0.00188 0.00178 0.00097 H22O 0.03467 0.69601 0.43425 1.00000 0.04020 0.00000 0.00000 C23 0.20837 0.58392 0.55001 1.00000 0.02217 0.02403 0.02582 -0.00559 -0.00258 -0.00044 0.02426 0.00946 0.00065 0.00059 0.00033 0.00000 0.00333 0.00298 0.00288 0.00244 0.00250 0.00252 0.00130 H23 0.28488 0.61988 0.57475 1.00000 0.02912 0.00000 0.00000 O23 0.07595 0.57804 0.60304 1.00000 0.03587 0.02450 0.02558 -0.00748 -0.00216 0.00003 0.02890 0.00655 0.00048 0.00042 0.00023 0.00000 0.00268 0.00223 0.00207 0.00177 0.00192 0.00189 0.00102 H23O 0.02159 0.51109 0.59767 1.00000 0.04334 0.00000 0.00000 C24 0.25157 0.43154 0.53468 1.00000 0.02163 0.02715 0.03245 -0.00708 -0.01290 0.00315 0.02589 0.00904 0.00066 0.00064 0.00035 0.00000 0.00342 0.00339 0.00329 0.00283 0.00280 0.00277 0.00140 O24A 0.36826 0.43827 0.47711 1.00000 0.03664 0.02074 0.04654 -0.00658 -0.00303 0.00820 0.03547 0.00732 0.00051 0.00043 0.00027 0.00000 0.00284 0.00216 0.00262 0.00197 0.00227 0.00199 0.00113 H24O 0.41087 0.35903 0.48327 1.00000 0.05321 0.00000 0.00000 O24B 0.18711 0.32320 0.57354 1.00000 0.03786 0.02242 0.04318 0.00461 -0.00029 0.00081 0.03724 0.00755 0.00052 0.00046 0.00027 0.00000 0.00281 0.00230 0.00260 0.00205 0.00222 0.00210 0.00114 C32A 0.76417 0.00974 0.30347 1.00000 0.01976 0.01920 0.02119 0.00169 0.00475 -0.00769 0.02213 0.00894 0.00062 0.00059 0.00032 0.00000 0.00316 0.00273 0.00275 0.00222 0.00236 0.00236 0.00123 H32G 0.72046 0.07151 0.34084 1.00000 0.02656 0.00000 0.00000 H32H 0.79247 -0.08170 0.33502 1.00000 0.02656 0.00000 0.00000 C32B 0.97585 -0.00578 0.19389 1.00000 0.01622 0.01740 0.02097 -0.01027 -0.00208 0.00162 0.01754 0.00816 0.00060 0.00053 0.00030 0.00000 0.00296 0.00260 0.00264 0.00220 0.00224 0.00225 0.00116 H32A 1.06363 0.04926 0.15981 1.00000 0.02104 0.00000 0.00000 H32B 0.90904 -0.02224 0.15915 1.00000 0.02104 0.00000 0.00000 C32C 0.99879 0.11823 0.30447 1.00000 0.01764 0.02467 0.02629 -0.00463 -0.00324 0.00015 0.02312 0.00881 0.00061 0.00060 0.00032 0.00000 0.00314 0.00293 0.00293 0.00241 0.00244 0.00247 0.00128 H32C 1.02091 0.02407 0.33611 1.00000 0.02774 0.00000 0.00000 H32D 0.94428 0.17498 0.34178 1.00000 0.02774 0.00000 0.00000 C32D 0.86359 0.22814 0.19783 1.00000 0.02482 0.02201 0.01897 -0.00318 -0.00658 0.00250 0.02178 0.00888 0.00065 0.00056 0.00031 0.00000 0.00324 0.00282 0.00265 0.00230 0.00240 0.00247 0.00124 H32E 0.95487 0.27278 0.16210 1.00000 0.02614 0.00000 0.00000 H32F 0.79767 0.20315 0.16451 1.00000 0.02614 0.00000 0.00000 C33A 0.64914 -0.02697 0.25994 1.00000 0.02249 0.01808 0.02456 -0.00421 -0.00546 0.00050 0.02163 0.00853 0.00062 0.00057 0.00032 0.00000 0.00320 0.00276 0.00280 0.00228 0.00241 0.00241 0.00124 H33G 0.69183 -0.08780 0.22186 1.00000 0.02596 0.00000 0.00000 H33H 0.61702 0.06398 0.22977 1.00000 0.02596 0.00000 0.00000 C33B 1.02226 -0.15348 0.23401 1.00000 0.02484 0.02469 0.02740 -0.00154 -0.00079 0.00249 0.02683 0.00976 0.00068 0.00060 0.00034 0.00000 0.00344 0.00303 0.00301 0.00250 0.00259 0.00260 0.00136 H33A 1.09258 -0.13879 0.26721 1.00000 0.03219 0.00000 0.00000 H33B 0.93575 -0.20955 0.26882 1.00000 0.03219 0.00000 0.00000 C33C 1.14255 0.20047 0.26344 1.00000 0.02190 0.02272 0.02757 -0.00409 -0.00702 -0.00398 0.02392 0.00873 0.00064 0.00060 0.00034 0.00000 0.00327 0.00291 0.00297 0.00241 0.00249 0.00251 0.00128 H33C 1.19727 0.14618 0.22491 1.00000 0.02871 0.00000 0.00000 H33D 1.12210 0.29724 0.23387 1.00000 0.02871 0.00000 0.00000 C33D 0.79273 0.33784 0.24260 1.00000 0.02372 0.02271 0.02344 -0.00404 -0.00400 -0.00166 0.02350 0.00891 0.00066 0.00057 0.00032 0.00000 0.00327 0.00296 0.00282 0.00240 0.00246 0.00253 0.00128 H33E 0.85932 0.36566 0.27484 1.00000 0.02820 0.00000 0.00000 H33F 0.70206 0.29352 0.27908 1.00000 0.02820 0.00000 0.00000 C34A 0.51746 -0.10895 0.31797 1.00000 0.02504 0.03073 0.02313 0.00063 -0.00595 -0.00815 0.02701 0.00936 0.00067 0.00067 0.00034 0.00000 0.00333 0.00318 0.00290 0.00248 0.00250 0.00263 0.00134 H34C 0.54930 -0.20124 0.34698 1.00000 0.03241 0.00000 0.00000 H34D 0.47691 -0.04933 0.35708 1.00000 0.03241 0.00000 0.00000 C34B 1.09232 -0.23837 0.17265 1.00000 0.03448 0.02270 0.02806 -0.01034 -0.00084 0.00318 0.02847 0.00976 0.00073 0.00060 0.00034 0.00000 0.00371 0.00302 0.00308 0.00253 0.00275 0.00270 0.00140 H34E 1.17787 -0.18136 0.13743 1.00000 0.03416 0.00000 0.00000 H34F 1.02145 -0.25365 0.13986 1.00000 0.03416 0.00000 0.00000 C34C 1.23549 0.22033 0.32182 1.00000 0.01745 0.03728 0.03945 -0.01455 -0.00908 0.00255 0.02997 0.00944 0.00068 0.00069 0.00038 0.00000 0.00316 0.00343 0.00346 0.00287 0.00264 0.00271 0.00141 H34A 1.18077 0.27449 0.36042 1.00000 0.03597 0.00000 0.00000 H34B 1.25622 0.12359 0.35131 1.00000 0.03597 0.00000 0.00000 C34D 0.75597 0.47317 0.18787 1.00000 0.02788 0.02021 0.02978 -0.00381 -0.00926 -0.00010 0.02566 0.00933 0.00069 0.00058 0.00035 0.00000 0.00348 0.00286 0.00305 0.00243 0.00262 0.00251 0.00133 H34G 0.84637 0.51614 0.15062 1.00000 0.03079 0.00000 0.00000 H34H 0.68779 0.44549 0.15643 1.00000 0.03079 0.00000 0.00000 C35A 0.40031 -0.14208 0.27569 1.00000 0.02214 0.03383 0.03505 -0.00652 -0.00532 -0.00049 0.03049 0.00947 0.00067 0.00067 0.00037 0.00000 0.00348 0.00339 0.00330 0.00279 0.00270 0.00276 0.00142 H35D 0.36942 -0.05090 0.24647 1.00000 0.03659 0.00000 0.00000 H35E 0.31636 -0.19211 0.31444 1.00000 0.03659 0.00000 0.00000 H35F 0.43898 -0.20476 0.23865 1.00000 0.03659 0.00000 0.00000 C35B 1.14156 -0.38674 0.21174 1.00000 0.03732 0.02658 0.04289 -0.01260 -0.00389 0.00328 0.03543 0.01055 0.00079 0.00064 0.00040 0.00000 0.00411 0.00330 0.00372 0.00291 0.00309 0.00289 0.00157 H35J 1.20965 -0.37190 0.24538 1.00000 0.04251 0.00000 0.00000 H35K 1.19033 -0.43735 0.17071 1.00000 0.04251 0.00000 0.00000 H35L 1.05614 -0.44563 0.24407 1.00000 0.04251 0.00000 0.00000 C35C 1.37753 0.30206 0.28099 1.00000 0.03078 0.03409 0.04202 -0.00628 -0.01241 0.00203 0.03514 0.01051 0.00075 0.00070 0.00041 0.00000 0.00379 0.00355 0.00361 0.00295 0.00301 0.00295 0.00154 H35G 1.43580 0.24450 0.24624 1.00000 0.04216 0.00000 0.00000 H35H 1.43186 0.31911 0.32069 1.00000 0.04216 0.00000 0.00000 H35I 1.35737 0.39575 0.24947 1.00000 0.04216 0.00000 0.00000 C35D 0.68706 0.58611 0.23272 1.00000 0.04689 0.02296 0.03751 -0.00703 -0.00886 0.00848 0.03564 0.01086 0.00082 0.00065 0.00039 0.00000 0.00434 0.00312 0.00348 0.00274 0.00313 0.00296 0.00159 H35A 0.59209 0.54786 0.26528 1.00000 0.04277 0.00000 0.00000 H35B 0.67337 0.67491 0.19510 1.00000 0.04277 0.00000 0.00000 H35C 0.75109 0.60871 0.26684 1.00000 0.04277 0.00000 0.00000 N31 0.90000 0.08766 0.25052 1.00000 0.02259 0.01967 0.01942 -0.00167 -0.00241 0.00120 0.02116 0.00731 0.00053 0.00047 0.00026 0.00000 0.00270 0.00236 0.00224 0.00190 0.00199 0.00202 0.00106 O1W 0.45374 0.17622 0.46494 1.00000 0.02422 0.02126 0.04869 -0.00617 -0.01186 0.00332 0.03091 0.00712 0.00052 0.00044 0.00027 0.00000 0.00254 0.00220 0.00273 0.00201 0.00219 0.00203 0.00104 H11W 0.38140 0.11826 0.48398 1.00000 0.00895 0.06213 0.00304 0.00430 0.00289 0.00000 0.01433 H12W 0.52894 0.14441 0.47741 1.00000 0.01074 0.06619 0.00286 0.00483 0.00293 0.00000 0.00000 O2W 0.15337 0.54586 0.02924 1.00000 0.02740 0.02939 0.05079 -0.01143 -0.01516 0.00026 0.03437 0.00684 0.00050 0.00048 0.00028 0.00000 0.00265 0.00248 0.00276 0.00222 0.00213 0.00206 0.00108 H21W 0.12551 0.47812 0.01009 1.00000 0.06145 0.04689 0.00829 0.00456 0.00458 0.00000 0.02667 H22W 0.11098 0.62153 0.01365 1.00000 0.03078 0.08375 0.00677 0.00371 0.00373 0.00000 0.01798 Final Structure Factor Calculation for 04skc0003p1 in P-1 Total number of l.s. parameters = 382 Maximum vector length = 511 Memory required = 5321 / 22995 wR2 = 0.2993 before cycle 9 for 5375 data and 0 / 382 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.012 0.022 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.982; Restrained GooF = 0.981 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1278 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1106 for 2266 Fo > 4sig(Fo) and 0.2391 for all 5375 data wR2 = 0.2993, GooF = S = 0.982, Restrained GooF = 0.981 for all data Occupancy sum of asymmetric unit = 39.00 for non-hydrogen and 51.00 for hydrogen atoms Principal mean square atomic displacements U 0.0295 0.0200 0.0169 C1 0.0308 0.0203 0.0161 C2 0.0310 0.0193 0.0169 C3 0.0329 0.0266 0.0189 C4 0.0371 0.0302 0.0152 O1A 0.0328 0.0255 0.0213 O1B 0.0397 0.0249 0.0167 O2 0.0339 0.0262 0.0229 O3 0.0527 0.0324 0.0177 O4A 0.0532 0.0323 0.0167 O4B 0.0267 0.0208 0.0138 C21 0.0343 0.0269 0.0235 O21A 0.0362 0.0276 0.0197 O21B 0.0327 0.0233 0.0168 C22 0.0363 0.0233 0.0208 O22 0.0277 0.0238 0.0212 C23 0.0385 0.0262 0.0219 O23 0.0350 0.0267 0.0160 C24 0.0520 0.0369 0.0174 O24A 0.0568 0.0356 0.0193 O24B 0.0317 0.0268 0.0079 C32A 0.0251 0.0167 0.0107 C32B 0.0270 0.0247 0.0176 C32C 0.0255 0.0224 0.0174 C32D 0.0248 0.0221 0.0180 C33A 0.0352 0.0232 0.0221 C33B 0.0296 0.0254 0.0167 C33C 0.0260 0.0239 0.0207 C33D 0.0402 0.0224 0.0184 C34A 0.0391 0.0290 0.0173 C34B 0.0440 0.0299 0.0160 C34C 0.0324 0.0244 0.0201 C34D 0.0355 0.0341 0.0219 C35A 0.0465 0.0368 0.0229 C35B 0.0437 0.0342 0.0275 C35C 0.0489 0.0375 0.0206 C35D 0.0250 0.0209 0.0176 N31 0.0493 0.0238 0.0196 O1W 0.0517 0.0297 0.0217 O2W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.013 0.020 0.027 0.035 0.044 0.054 0.069 0.096 1.000 Number in group 577. 520. 569. 534. 534. 538. 506. 522. 540. 535. GooF 0.891 0.867 0.921 0.940 1.015 0.959 1.022 0.966 1.025 1.182 K 24.999 3.907 1.750 1.573 1.228 1.145 1.087 1.043 1.034 1.091 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.95 1.01 1.10 1.23 1.51 inf Number in group 557. 526. 539. 535. 544. 526. 540. 529. 537. 542. GooF 0.761 0.746 0.787 0.787 0.814 0.873 0.932 1.043 1.109 1.625 K 1.164 1.127 1.139 1.088 1.108 1.050 1.080 1.049 1.068 1.137 R1 0.473 0.388 0.392 0.315 0.259 0.233 0.177 0.129 0.130 0.117 Recommended weighting scheme: WGHT 0.1279 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 1 -2 2 786.41 139.86 6.50 0.062 3.61 0 0 4 77893.54 36570.09 6.13 1.000 4.23 4 0 4 1708.24 773.27 6.13 0.145 2.21 2 -4 1 86.99 13.38 6.07 0.019 2.04 -4 2 0 120.00 378.50 5.92 0.102 2.08 1 0 2 405.05 1032.01 5.81 0.168 6.95 -3 0 3 927.92 293.05 5.46 0.090 2.48 0 4 0 2252.81 1143.00 5.37 0.177 2.29 -3 4 1 209.71 105.28 5.04 0.054 1.87 4 -1 9 236.22 98.66 4.98 0.052 1.56 2 -3 3 199.29 68.96 4.76 0.043 2.30 0 -4 4 179.48 61.53 4.75 0.041 1.86 2 -4 7 125.40 23.93 4.69 0.026 1.51 5 -2 5 118.70 33.37 4.66 0.030 1.61 0 4 6 1639.04 913.01 4.64 0.158 1.99 4 -5 8 150.20 12.70 4.59 0.019 1.18 -4 -2 5 288.35 52.52 4.58 0.038 1.56 -4 0 2 646.10 289.76 4.39 0.089 2.10 4 1 2 708.18 41.53 4.34 0.034 2.27 -1 4 2 826.44 476.26 4.28 0.114 2.26 4 -2 3 197.03 101.02 4.27 0.053 2.01 4 2 8 241.13 5.04 4.23 0.012 1.71 3 2 6 144.99 42.28 3.99 0.034 2.20 1 -1 1 670.22 1196.66 3.96 0.181 6.16 -4 -4 2 162.02 44.29 3.96 0.035 1.49 -3 -5 3 97.70 3.82 3.94 0.010 1.40 4 4 0 79.77 0.86 3.90 0.005 1.59 4 5 5 246.68 92.04 3.88 0.050 1.45 5 0 4 281.96 107.44 3.85 0.054 1.82 -4 0 6 876.35 526.05 3.81 0.120 1.62 -1 2 1 126.78 21.79 3.78 0.024 4.14 -3 7 1 86.02 15.15 3.76 0.020 1.23 4 1 10 230.03 127.62 3.70 0.059 1.53 -4 0 9 91.76 29.68 3.58 0.028 1.32 -4 -1 7 526.75 299.92 3.56 0.091 1.46 2 2 6 51.66 5.98 3.54 0.013 2.49 -4 -4 1 77.58 8.48 3.54 0.015 1.54 0 -4 1 4553.76 2913.47 3.54 0.282 2.21 4 0 2 2465.43 1513.66 3.52 0.203 2.33 8 -4 7 261.20 113.72 3.52 0.056 0.99 1 0 9 138.29 0.08 3.44 0.002 1.92 0 -3 5 194.28 18.04 3.40 0.022 2.07 4 1 14 187.19 63.86 3.40 0.042 1.19 4 0 10 96.37 4.60 3.37 0.011 1.51 -1 -4 3 127.49 8.47 3.36 0.015 1.90 8 1 4 94.97 9.43 3.34 0.016 1.16 -1 -3 5 130.83 62.56 3.31 0.041 1.95 4 -1 7 389.71 184.78 3.30 0.071 1.78 1 -4 2 1417.67 759.98 3.29 0.144 2.09 -3 -5 8 271.03 96.15 3.28 0.051 1.11 Bond lengths and angles C1 - Distance Angles O1B 1.2227 (0.0066) O1A 1.2964 (0.0069) 126.80 (0.58) C2 1.5149 (0.0086) 119.38 (0.51) 113.80 (0.48) C1 - O1B O1A C2 - Distance Angles O2 1.4338 (0.0067) C1 1.5149 (0.0086) 112.78 (0.47) C3 1.5397 (0.0079) 108.19 (0.41) 110.17 (0.45) H2 1.0000 108.54 108.54 108.54 C2 - O2 C1 C3 C3 - Distance Angles O3 1.3934 (0.0068) C4 1.4955 (0.0085) 113.23 (0.43) C2 1.5397 (0.0078) 111.29 (0.47) 112.37 (0.47) H3 1.0000 106.47 106.47 106.47 C3 - O3 C4 C2 C4 - Distance Angles O4B 1.2225 (0.0066) O4A 1.3134 (0.0073) 123.26 (0.58) C3 1.4955 (0.0085) 122.19 (0.55) 114.49 (0.46) C4 - O4B O4A O1A - Distance Angles C1 1.2964 (0.0069) H1 0.8400 109.47 O1A - C1 O1B - Distance Angles C1 1.2227 (0.0066) O1B - O2 - Distance Angles C2 1.4338 (0.0067) H2A 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.3934 (0.0068) H3A 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.3134 (0.0073) H4 0.8400 109.47 O4A - C4 O4B - Distance Angles C4 1.2225 (0.0066) O4B - C21 - Distance Angles O21B 1.2351 (0.0070) O21A 1.2782 (0.0069) 126.57 (0.48) C22 1.5265 (0.0077) 118.90 (0.47) 114.47 (0.49) C21 - O21B O21A O21A - Distance Angles C21 1.2782 (0.0069) H21 0.8400 109.47 O21A - C21 O21B - Distance Angles C21 1.2351 (0.0070) O21B - C22 - Distance Angles O22 1.4089 (0.0072) C21 1.5265 (0.0077) 112.65 (0.42) C23 1.5456 (0.0078) 109.98 (0.49) 109.15 (0.44) H22 1.0000 108.32 108.32 108.32 C22 - O22 C21 C23 O22 - Distance Angles C22 1.4089 (0.0073) H22O 0.8400 109.47 O22 - C22 C23 - Distance Angles O23 1.3872 (0.0072) C24 1.5442 (0.0079) 111.69 (0.49) C22 1.5456 (0.0078) 111.86 (0.43) 111.05 (0.46) H23 1.0000 107.32 107.32 107.32 C23 - O23 C24 C22 O23 - Distance Angles C23 1.3872 (0.0072) H23O 0.8400 109.47 O23 - C23 C24 - Distance Angles O24B 1.1922 (0.0074) O24A 1.3244 (0.0076) 126.13 (0.51) C23 1.5442 (0.0079) 121.79 (0.54) 112.03 (0.52) C24 - O24B O24A O24A - Distance Angles C24 1.3244 (0.0076) H24O 0.8400 109.47 O24A - C24 O24B - Distance Angles C24 1.1922 (0.0074) O24B - C32A - Distance Angles N31 1.5073 (0.0073) C33A 1.5170 (0.0080) 114.42 (0.43) H32G 0.9900 108.66 108.66 H32H 0.9900 108.66 108.66 107.60 C32A - N31 C33A H32G C32B - Distance Angles N31 1.5265 (0.0064) C33B 1.5268 (0.0071) 114.81 (0.41) H32A 0.9900 108.56 108.56 H32B 0.9900 108.56 108.56 107.55 C32B - N31 C33B H32A C32C - Distance Angles N31 1.5169 (0.0071) C33C 1.5212 (0.0083) 115.80 (0.44) H32C 0.9900 108.33 108.33 H32D 0.9900 108.33 108.33 107.42 C32C - N31 C33C H32C C32D - Distance Angles C33D 1.4938 (0.0074) N31 1.5313 (0.0065) 113.99 (0.42) H32E 0.9900 108.76 108.76 H32F 0.9900 108.76 108.76 107.65 C32D - C33D N31 H32E C33A - Distance Angles C32A 1.5170 (0.0080) C34A 1.5283 (0.0085) 110.78 (0.44) H33G 0.9900 109.49 109.49 H33H 0.9900 109.49 109.49 108.06 C33A - C32A C34A H33G C33B - Distance Angles C34B 1.5137 (0.0077) C32B 1.5268 (0.0071) 110.37 (0.44) H33A 0.9900 109.58 109.58 H33B 0.9900 109.58 109.58 108.12 C33B - C34B C32B H33A C33C - Distance Angles C34C 1.5110 (0.0080) C32C 1.5212 (0.0083) 111.77 (0.48) H33C 0.9900 109.26 109.26 H33D 0.9900 109.26 109.26 107.94 C33C - C34C C32C H33C C33D - Distance Angles C32D 1.4938 (0.0074) C34D 1.5154 (0.0073) 111.87 (0.45) H33E 0.9900 109.24 109.24 H33F 0.9900 109.24 109.24 107.92 C33D - C32D C34D H33E C34A - Distance Angles C35A 1.5073 (0.0084) C33A 1.5283 (0.0085) 111.32 (0.47) H34C 0.9900 109.37 109.37 H34D 0.9900 109.37 109.37 107.99 C34A - C35A C33A H34C C34B - Distance Angles C33B 1.5137 (0.0077) C35B 1.5360 (0.0081) 111.24 (0.47) H34E 0.9900 109.38 109.38 H34F 0.9900 109.38 109.38 108.00 C34B - C33B C35B H34E C34C - Distance Angles C35C 1.5059 (0.0095) C33C 1.5110 (0.0080) 111.60 (0.52) H34A 0.9900 109.30 109.30 H34B 0.9900 109.30 109.30 107.96 C34C - C35C C33C H34A C34D - Distance Angles C35D 1.5131 (0.0080) C33D 1.5154 (0.0073) 112.16 (0.48) H34G 0.9900 109.17 109.17 H34H 0.9900 109.17 109.17 107.88 C34D - C35D C33D H34G C35A - Distance Angles C34A 1.5073 (0.0084) H35D 0.9800 109.47 H35E 0.9800 109.47 109.47 H35F 0.9800 109.47 109.47 109.47 C35A - C34A H35D H35E C35B - Distance Angles C34B 1.5360 (0.0081) H35J 0.9800 109.47 H35K 0.9800 109.47 109.47 H35L 0.9800 109.47 109.47 109.47 C35B - C34B H35J H35K C35C - Distance Angles C34C 1.5059 (0.0095) H35G 0.9800 109.47 H35H 0.9800 109.47 109.47 H35I 0.9800 109.47 109.47 109.47 C35C - C34C H35G H35H C35D - Distance Angles C34D 1.5131 (0.0080) H35A 0.9800 109.47 H35B 0.9800 109.47 109.47 H35C 0.9800 109.47 109.47 109.47 C35D - C34D H35A H35B N31 - Distance Angles C32A 1.5073 (0.0073) C32C 1.5169 (0.0071) 106.55 (0.40) C32B 1.5265 (0.0064) 110.92 (0.42) 110.77 (0.39) C32D 1.5313 (0.0065) 111.46 (0.43) 111.61 (0.42) 105.62 (0.37) N31 - C32A C32C C32B O1W - Distance Angles H11W 0.8382 (0.0187) H12W 0.8158 (0.0186) 112.93 (3.09) O1W - H11W O2W - Distance Angles H21W 0.8409 (0.0195) H22W 0.8363 (0.0192) 108.77 (3.19) O2W - H21W Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.84 2.617(5) 154.3 O24A-H24O...O1W 0.84(2) 2.03(3) 2.806(6) 153(6) O2W-H21W...O1B 0.84 2.51 2.787(6) 100.7 O2-H2A...O4B_$1 0.84 1.76 2.600(6) 173.4 O4A-H4...O2W_$2 0.84 1.66 2.468(7) 161.4 O21A-H21...O21A_$3 0.84 2.11 2.791(6) 137.3 O22-H22O...O24B_$4 0.84 2.10 2.931(6) 172.5 O23-H23O...O22_$4 0.838(19) 2.16(3) 2.943(6) 155(5) O1W-H11W...O21B_$5 0.816(19) 2.01(2) 2.812(6) 168(5) O1W-H12W...O21B_$6 0.836(19) 2.14(4) 2.905(6) 152(6) O2W-H22W...O1B_$7 FMAP and GRID set by program FMAP 2 3 41 GRID -1.316 -2 -2 1.316 2 2 R1 = 0.2390 for 5375 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.55 at 0.5837 0.3966 0.4289 [ 1.23 A from H23 ] Deepest hole -0.39 at 0.7304 0.2432 0.3681 [ 1.62 A from H33F ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 4863 / 27560 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4163 0.6034 0.5711 1.00000 0.05 0.55 1.23 H23 1.70 H24O 2.07 C23 2.09 O24A Q2 1 -0.0957 0.9142 0.4912 1.00000 0.05 0.49 1.32 H21 1.35 H21 1.35 O21A 2.09 O21A Q3 1 0.1953 0.1514 0.4864 1.00000 0.05 0.46 1.76 H11W 2.25 O21A 2.27 H21 2.32 H34A Q4 1 0.1320 -0.0612 -0.0022 1.00000 0.05 0.45 1.02 O1A 1.27 H1 1.57 H1 2.22 C1 Q5 1 1.1440 0.3266 0.2659 1.00000 0.05 0.44 0.74 H33D 1.19 C33C 1.62 C34C 1.74 H34A Q6 1 0.1242 0.3772 0.5490 1.00000 0.05 0.39 0.89 O24B 1.25 C24 1.58 H22O 1.82 H23O Q7 1 1.5470 0.3354 0.2366 1.00000 0.05 0.39 1.31 H35G 1.62 C35C 1.63 H35H 1.77 H33F Q8 1 0.1868 0.3339 0.4748 1.00000 0.05 0.39 1.72 C24 1.72 O24B 1.97 O24A 2.15 H24O Q9 1 0.0927 0.4323 -0.0324 1.00000 0.05 0.38 1.03 H21W 1.59 O1B 1.83 O2W 1.92 H22W Q10 1 0.1006 0.6814 -0.0220 1.00000 0.05 0.37 0.78 H22W 1.55 O2W 1.73 O1B 1.90 H21W Q11 1 0.8318 0.5822 0.2334 1.00000 0.05 0.37 0.93 H35C 1.36 C35D 1.66 C34D 1.68 H34G Q12 1 1.4136 0.3937 0.2458 1.00000 0.05 0.37 0.52 H35I 0.97 C35C 1.41 H35H 1.41 H35G Q13 1 -0.0426 0.8359 0.4721 1.00000 0.05 0.36 1.03 O21A 1.58 H21 1.69 H22O 2.05 H21 Q14 1 0.1316 0.4231 0.0177 1.00000 0.05 0.36 0.51 H21W 1.23 O2W 1.58 O1B 1.86 H22W Q15 1 1.4560 0.4028 0.2104 1.00000 0.05 0.36 1.03 H35I 1.46 C35C 1.49 H35G 1.91 H35H Shortest distances between peaks (including symmetry equivalents) 12 15 0.66 2 13 0.96 9 14 1.01 2 3 1.08 7 15 1.17 7 12 1.35 6 8 1.46 3 13 1.48 3 8 1.69 8 13 2.03 9 10 2.05 6 13 2.27 10 14 2.36 9 10 2.38 9 9 2.39 2 8 2.40 10 14 2.42 9 14 2.49 2 2 2.51 4 10 2.53 5 12 2.54 3 6 2.60 4 4 2.71 2 13 2.92 5 15 2.93 14 14 2.96 2 6 2.98 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.56: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.11: Structure factors and derivatives 9.81: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.94: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.02: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04skc0003p1 finished at 12:22:41 Total CPU time: 14.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++