+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXH-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + pbca started at 14:46:27 on 04-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL pbca in Pbca CELL 0.71073 14.7295 14.7023 26.7711 90.000 90.000 90.000 ZERR 16.00 0.0004 0.0004 0.0008 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O UNIT 288 224 64 16 V = 5797.48 F(000) = 2528.0 Mu = 0.09 mm-1 Cell Wt = 4837.31 Rho = 1.386 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 5 DFIX 0.89 0.01 N4 H4A N4 H4B N24 H24A N24 H24B size 0.34 0.12 0.05 EQIV $1 -x, -y+1, -z EQIV $2 -x+1/2, y-1/2, z HTAB N1 O21_$1 HTAB N4 O1 HTAB N4 N22_$2 HTAB N21 O1_$1 HTAB N24 O21 acta BOND $H L.S. 9 TEMP -153.00 WGHT 0.010000 9.386000 EXTI 0.000714 FVAR 0.08828 MOLE 1 C1 1 0.186304 0.449788 0.048849 11.00000 0.01933 0.01473 = 0.01932 -0.00145 0.00160 0.00206 C2 1 0.252818 0.450397 0.087439 11.00000 0.01742 0.01919 = 0.01607 -0.00022 0.00002 0.00158 C3 1 0.330214 0.507221 0.086656 11.00000 0.02033 0.02096 = 0.01875 -0.00301 -0.00115 0.00044 C4 1 0.337663 0.574489 0.047857 11.00000 0.02070 0.01927 = 0.02174 0.00051 -0.00107 -0.00240 AFIX 43 H4 2 0.385887 0.617394 0.047619 11.00000 -1.20000 AFIX 0 C5 1 0.273590 0.574407 0.011785 11.00000 0.02148 0.01687 = 0.01841 -0.00111 0.00048 -0.00029 C6 1 0.265214 0.390965 0.127211 11.00000 0.01996 0.01889 = 0.01941 -0.00256 0.00093 0.00322 C7 1 0.275455 0.637616 -0.031489 11.00000 0.01474 0.02198 = 0.02091 0.00118 0.00002 0.00056 C8 1 0.301665 0.728238 -0.024873 11.00000 0.02249 0.02472 = 0.02423 0.00002 -0.00046 -0.00166 AFIX 43 H8 2 0.319920 0.748845 0.007226 11.00000 -1.20000 AFIX 0 C9 1 0.301194 0.788085 -0.064749 11.00000 0.02387 0.02106 = 0.03243 0.00449 -0.00137 -0.00198 AFIX 43 H9 2 0.318120 0.849759 -0.059716 11.00000 -1.20000 AFIX 0 C10 1 0.276226 0.758747 -0.111960 11.00000 0.02624 0.02540 = 0.02734 0.00947 0.00286 0.00354 AFIX 43 H10 2 0.275814 0.800007 -0.139268 11.00000 -1.20000 AFIX 0 C11 1 0.251838 0.668547 -0.118958 11.00000 0.02948 0.02748 = 0.01994 -0.00027 -0.00034 0.00175 AFIX 43 H11 2 0.235704 0.647850 -0.151381 11.00000 -1.20000 AFIX 0 C12 1 0.250750 0.608419 -0.079267 11.00000 0.02549 0.02037 = 0.02236 -0.00029 0.00116 0.00001 AFIX 43 H12 2 0.233134 0.546993 -0.084493 11.00000 -1.20000 AFIX 0 C13 1 0.396513 0.365223 0.184785 11.00000 0.02591 0.01982 = 0.02004 -0.00097 -0.00544 -0.00047 C14 1 0.487282 0.346677 0.176170 11.00000 0.02716 0.03481 = 0.02406 0.00335 -0.00031 0.00041 AFIX 43 H14 2 0.516460 0.368904 0.146972 11.00000 -1.20000 AFIX 0 C15 1 0.535122 0.295209 0.210723 11.00000 0.02565 0.05069 = 0.02959 0.00294 -0.00226 0.01211 AFIX 43 H15 2 0.597467 0.282068 0.205198 11.00000 -1.20000 AFIX 0 C16 1 0.492287 0.262874 0.253290 11.00000 0.04146 0.03240 = 0.02213 0.00223 -0.00551 0.01157 AFIX 43 H16 2 0.525034 0.227163 0.276743 11.00000 -1.20000 AFIX 0 C17 1 0.401585 0.282811 0.261510 11.00000 0.03803 0.02995 = 0.01867 -0.00029 -0.00170 0.00403 AFIX 43 H17 2 0.372298 0.260520 0.290660 11.00000 -1.20000 AFIX 0 C18 1 0.353221 0.334930 0.227628 11.00000 0.02494 0.03001 = 0.02047 -0.00074 -0.00116 0.00137 AFIX 43 H18 2 0.291389 0.349677 0.233653 11.00000 -1.20000 AFIX 0 N1 3 0.201290 0.512862 0.011960 11.00000 0.02002 0.01960 = 0.01606 0.00043 -0.00324 -0.00084 AFIX 43 H1 2 0.162893 0.514661 -0.013204 11.00000 -1.20000 AFIX 0 N2 3 0.389216 0.485880 0.122680 11.00000 0.02582 0.02316 = 0.02108 0.00485 -0.00464 -0.00416 N3 3 0.346447 0.414225 0.147672 11.00000 0.02167 0.02116 = 0.01971 0.00286 -0.00297 -0.00255 N4 3 0.209229 0.322811 0.144049 11.00000 0.02075 0.02265 = 0.02247 0.00331 -0.00115 0.00064 AFIX 2 0.8900 H4A 2 0.166565 0.312250 0.121393 11.00000 -1.50000 H4B 2 0.238350 0.273114 0.154349 11.00000 -1.50000 AFIX 0 O1 4 0.120931 0.395999 0.047342 11.00000 0.02056 0.02125 = 0.02263 0.00202 -0.00119 -0.00196 MOLE 2 C21 1 -0.005938 0.572338 0.069875 11.00000 0.01787 0.01741 = 0.02065 -0.00102 0.00058 0.00058 C22 1 0.057418 0.588330 0.109274 11.00000 0.02162 0.01723 = 0.01752 -0.00155 0.00090 0.00084 C23 1 0.122186 0.659331 0.107680 11.00000 0.02231 0.01696 = 0.01948 -0.00201 -0.00051 -0.00094 C24 1 0.122919 0.720425 0.066310 11.00000 0.02437 0.01795 = 0.02220 -0.00004 -0.00114 -0.00495 AFIX 43 H24 2 0.163956 0.770224 0.065081 11.00000 -1.20000 AFIX 0 C25 1 0.063410 0.705095 0.029021 11.00000 0.01954 0.01914 = 0.01929 -0.00013 0.00016 -0.00062 C26 1 0.075893 0.541068 0.153102 11.00000 0.02085 0.01837 = 0.01949 -0.00233 0.00283 0.00226 C27 1 0.058980 0.763224 -0.016311 11.00000 0.01573 0.02215 = 0.02223 0.00255 -0.00105 -0.00027 C28 1 0.074930 0.856921 -0.012507 11.00000 0.02341 0.02403 = 0.03045 0.00218 -0.00711 -0.00308 AFIX 43 H28 2 0.088268 0.883072 0.019102 11.00000 -1.20000 AFIX 0 C29 1 0.071352 0.911706 -0.054650 11.00000 0.02411 0.02258 = 0.04227 0.01049 -0.00279 -0.00138 AFIX 43 H29 2 0.082263 0.975184 -0.051840 11.00000 -1.20000 AFIX 0 C30 1 0.051849 0.873867 -0.100900 11.00000 0.02052 0.03801 = 0.02858 0.01490 0.00501 0.00238 AFIX 43 H30 2 0.048787 0.911442 -0.129720 11.00000 -1.20000 AFIX 0 C31 1 0.036870 0.781237 -0.104928 11.00000 0.02347 0.04125 = 0.01966 0.00600 0.00428 0.00272 AFIX 43 H31 2 0.023585 0.755437 -0.136631 11.00000 -1.20000 AFIX 0 C32 1 0.041072 0.725721 -0.063110 11.00000 0.01784 0.02701 = 0.02100 0.00201 0.00072 -0.00045 AFIX 43 H32 2 0.031735 0.662061 -0.066361 11.00000 -1.20000 AFIX 0 C33 1 0.193910 0.564662 0.220207 11.00000 0.02713 0.01862 = 0.01646 -0.00155 -0.00210 0.00404 C34 1 0.286593 0.581287 0.221876 11.00000 0.03013 0.02139 = 0.02111 0.00027 -0.00124 -0.00092 AFIX 43 H34 2 0.317411 0.603547 0.193201 11.00000 -1.20000 AFIX 0 C35 1 0.333854 0.565081 0.265847 11.00000 0.02964 0.02463 = 0.02637 0.00120 -0.00544 -0.00145 AFIX 43 H35 2 0.397280 0.576511 0.267277 11.00000 -1.20000 AFIX 0 C36 1 0.289146 0.532379 0.307608 11.00000 0.03634 0.02363 = 0.02042 -0.00021 -0.00615 0.00571 AFIX 43 H36 2 0.321667 0.521519 0.337667 11.00000 -1.20000 AFIX 0 C37 1 0.196971 0.515615 0.305346 11.00000 0.03450 0.03109 = 0.01850 0.00417 0.00418 0.00773 AFIX 43 H37 2 0.166419 0.492705 0.333953 11.00000 -1.20000 AFIX 0 C38 1 0.148344 0.531831 0.261758 11.00000 0.02612 0.02838 = 0.02316 0.00420 0.00027 0.00424 AFIX 43 H38 2 0.084874 0.520588 0.260465 11.00000 -1.20000 AFIX 0 N21 3 0.003328 0.632013 0.030593 11.00000 0.01985 0.01993 = 0.01720 -0.00113 -0.00390 -0.00236 AFIX 43 H21 2 -0.031547 0.623280 0.004338 11.00000 -1.20000 AFIX 0 N22 3 0.177154 0.658216 0.147083 11.00000 0.02858 0.01911 = 0.01728 0.00307 -0.00281 -0.00212 N23 3 0.146435 0.584968 0.175192 11.00000 0.02488 0.02073 = 0.01677 0.00070 -0.00152 -0.00056 N24 3 0.032304 0.466457 0.172318 11.00000 0.02549 0.02517 = 0.02589 0.00795 -0.00201 -0.00288 AFIX 2 0.8900 H24A 2 -0.006941 0.443008 0.150572 11.00000 -1.50000 H24B 2 0.066096 0.427936 0.190289 11.00000 -1.50000 AFIX 0 O21 4 -0.065387 0.511747 0.069572 11.00000 0.02132 0.01978 = 0.02803 0.00229 -0.00310 -0.00303 HKLF 4 Covalent radii and connectivity table for pbca in Pbca C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1 N1 C2 C2 - C6 C3 C1 C3 - N2 C2 C4 C4 - C5 C3 C5 - C4 N1 C7 C6 - N3 N4 C2 C7 - C12 C8 C5 C8 - C9 C7 C9 - C8 C10 C10 - C9 C11 C11 - C12 C10 C12 - C11 C7 C13 - C14 C18 N3 C14 - C13 C15 C15 - C16 C14 C16 - C17 C15 C17 - C18 C16 C18 - C17 C13 N1 - C1 C5 N2 - C3 N3 N3 - C6 N2 C13 N4 - C6 O1 - C1 C21 - O21 N21 C22 C22 - C26 C23 C21 C23 - N22 C22 C24 C24 - C25 C23 C25 - C24 N21 C27 C26 - N23 N24 C22 C27 - C32 C28 C25 C28 - C29 C27 C29 - C28 C30 C30 - C31 C29 C31 - C30 C32 C32 - C31 C27 C33 - C38 C34 N23 C34 - C33 C35 C35 - C36 C34 C36 - C37 C35 C37 - C36 C38 C38 - C33 C37 N21 - C21 C25 N22 - C23 N23 N23 - C26 N22 C33 N24 - C26 O21 - C21 Operators for generating equivalent atoms: $1 -x, -y+1, -z $2 -x+1/2, y-1/2, z h k l Fo^2 Sigma Why rejected 7 7 0 0.43 0.10 observed but should be systematically absent 19 0 3 2.70 0.62 observed but should be systematically absent 7 0 5 0.44 0.11 observed but should be systematically absent 0 0 25 2.09 0.51 observed but should be systematically absent 27831 Reflections read, of which 1676 rejected -19 =< h =< 17, -19 =< k =< 18, -34 =< l =< 34, Max. 2-theta = 54.97 4 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 7 7 3 0.22 0.01 9 0.07 1 Inconsistent equivalents 6537 Unique reflections, of which 0 suppressed R(int) = 0.0498 R(sigma) = 0.0516 Friedel opposites merged Maximum memory for data reduction = 3829 / 65959 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 = 4977 / 553073 wR2 = 0.1346 before cycle 1 for 6537 data and 428 / 428 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. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.107; Restrained GooF = 1.107 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 9.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08828 0.00016 0.011 OSF 2 0.00071 0.00013 0.002 EXTI Mean shift/esd = 0.002 Maximum = 0.011 for OSF Max. shift = 0.000 A for C13 Max. dU = 0.000 for C29 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4977 / 553073 wR2 = 0.1346 before cycle 2 for 6537 data and 428 / 428 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. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.107; Restrained GooF = 1.107 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 9.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08828 0.00016 -0.001 OSF 2 0.00071 0.00013 0.001 EXTI Mean shift/esd = 0.001 Maximum = -0.002 for z O1 Max. shift = 0.000 A for C24 Max. dU = 0.000 for C29 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4977 / 553073 wR2 = 0.1346 before cycle 3 for 6537 data and 428 / 428 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. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.107; Restrained GooF = 1.107 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 9.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08828 0.00016 0.001 OSF 2 0.00071 0.00013 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H4B Max. dU = 0.000 for C32 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4977 / 553073 wR2 = 0.1346 before cycle 4 for 6537 data and 428 / 428 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. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.107; Restrained GooF = 1.107 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 9.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08828 0.00016 0.000 OSF 2 0.00071 0.00013 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for H4B Max. dU = 0.000 for N21 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4977 / 553073 wR2 = 0.1346 before cycle 5 for 6537 data and 428 / 428 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. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.107; Restrained GooF = 1.107 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 9.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08828 0.00016 -0.001 OSF 2 0.00071 0.00013 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H24A Max. dU = 0.000 for N23 Least-squares cycle 6 Maximum vector length = 511 Memory required = 4977 / 553073 wR2 = 0.1346 before cycle 6 for 6537 data and 428 / 428 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. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.107; Restrained GooF = 1.107 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 9.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08828 0.00016 0.000 OSF 2 0.00071 0.00013 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for H24A Max. dU = 0.000 for N24 Least-squares cycle 7 Maximum vector length = 511 Memory required = 4977 / 553073 wR2 = 0.1346 before cycle 7 for 6537 data and 428 / 428 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. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.107; Restrained GooF = 1.107 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 9.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08828 0.00016 0.000 OSF 2 0.00071 0.00013 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for H24B Max. dU = 0.000 for C38 Least-squares cycle 8 Maximum vector length = 511 Memory required = 4977 / 553073 wR2 = 0.1346 before cycle 8 for 6537 data and 428 / 428 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. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.107; Restrained GooF = 1.107 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 9.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08828 0.00016 0.000 OSF 2 0.00071 0.00013 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for H24B Max. dU = 0.000 for C28 Least-squares cycle 9 Maximum vector length = 511 Memory required = 4977 / 553073 wR2 = 0.1346 before cycle 9 for 6537 data and 428 / 428 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. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.107; Restrained GooF = 1.107 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 9.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08828 0.00016 0.000 OSF 2 0.00071 0.00013 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for N1 Max. dU = 0.000 for C14 Largest correlation matrix elements -0.717 z H4A / x H4A -0.588 z H24A / x H24A 0.602 y H4B / x H4B 0.530 EXTI / OSF Idealized hydrogen atom generation before cycle 10 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H4 0.3859 0.6174 0.0476 43 0.950 0.000 C4 C5 C3 H8 0.3199 0.7488 0.0072 43 0.950 0.000 C8 C9 C7 H9 0.3181 0.8498 -0.0597 43 0.950 0.000 C9 C8 C10 H10 0.2758 0.8000 -0.1393 43 0.950 0.000 C10 C9 C11 H11 0.2357 0.6478 -0.1514 43 0.950 0.000 C11 C12 C10 H12 0.2331 0.5470 -0.0845 43 0.950 0.000 C12 C11 C7 H14 0.5165 0.3689 0.1470 43 0.950 0.000 C14 C13 C15 H15 0.5975 0.2821 0.2052 43 0.950 0.000 C15 C16 C14 H16 0.5250 0.2272 0.2767 43 0.950 0.000 C16 C17 C15 H17 0.3723 0.2605 0.2907 43 0.950 0.000 C17 C18 C16 H18 0.2914 0.3497 0.2337 43 0.950 0.000 C18 C17 C13 H1 0.1629 0.5147 -0.0132 43 0.880 0.000 N1 C1 C5 H24 0.1640 0.7702 0.0651 43 0.950 0.000 C24 C25 C23 H28 0.0883 0.8831 0.0191 43 0.950 0.000 C28 C29 C27 H29 0.0823 0.9752 -0.0518 43 0.950 0.000 C29 C28 C30 H30 0.0488 0.9114 -0.1297 43 0.950 0.000 C30 C31 C29 H31 0.0236 0.7554 -0.1366 43 0.950 0.000 C31 C30 C32 H32 0.0317 0.6621 -0.0664 43 0.950 0.000 C32 C31 C27 H34 0.3174 0.6035 0.1932 43 0.950 0.000 C34 C33 C35 H35 0.3973 0.5765 0.2673 43 0.950 0.000 C35 C36 C34 H36 0.3217 0.5215 0.3377 43 0.950 0.000 C36 C37 C35 H37 0.1664 0.4927 0.3340 43 0.950 0.000 C37 C36 C38 H38 0.0849 0.5206 0.2605 43 0.950 0.000 C38 C33 C37 H21 -0.0315 0.6233 0.0043 43 0.880 0.000 N21 C21 C25 pbca in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.18630 0.44979 0.04885 1.00000 0.01933 0.01473 0.01932 -0.00145 0.00160 0.00206 0.01779 0.00385 0.00015 0.00015 0.00008 0.00000 0.00117 0.00106 0.00106 0.00084 0.00088 0.00090 0.00046 C2 0.25282 0.45040 0.08744 1.00000 0.01742 0.01919 0.01607 -0.00022 0.00002 0.00158 0.01756 0.00380 0.00015 0.00015 0.00008 0.00000 0.00111 0.00109 0.00097 0.00085 0.00088 0.00090 0.00045 C3 0.33021 0.50722 0.08666 1.00000 0.02033 0.02096 0.01875 -0.00301 -0.00115 0.00044 0.02001 0.00385 0.00016 0.00016 0.00008 0.00000 0.00119 0.00115 0.00105 0.00089 0.00091 0.00094 0.00048 C4 0.33766 0.57449 0.04786 1.00000 0.02070 0.01927 0.02174 0.00051 -0.00107 -0.00240 0.02057 0.00396 0.00016 0.00016 0.00008 0.00000 0.00121 0.00112 0.00109 0.00091 0.00092 0.00094 0.00048 H4 0.38589 0.61739 0.04762 1.00000 0.02468 0.00000 0.00000 C5 0.27359 0.57441 0.01178 1.00000 0.02148 0.01687 0.01841 -0.00111 0.00048 -0.00029 0.01892 0.00383 0.00016 0.00015 0.00008 0.00000 0.00120 0.00107 0.00104 0.00087 0.00088 0.00091 0.00047 C6 0.26521 0.39097 0.12721 1.00000 0.01996 0.01889 0.01941 -0.00256 0.00093 0.00322 0.01942 0.00391 0.00016 0.00015 0.00008 0.00000 0.00121 0.00111 0.00105 0.00089 0.00088 0.00093 0.00047 C7 0.27546 0.63762 -0.03149 1.00000 0.01474 0.02198 0.02091 0.00118 0.00002 0.00056 0.01921 0.00394 0.00015 0.00016 0.00008 0.00000 0.00112 0.00116 0.00110 0.00091 0.00086 0.00091 0.00047 C8 0.30167 0.72824 -0.02487 1.00000 0.02249 0.02472 0.02423 0.00002 -0.00046 -0.00166 0.02381 0.00419 0.00016 0.00016 0.00009 0.00000 0.00127 0.00125 0.00118 0.00097 0.00097 0.00100 0.00052 H8 0.31992 0.74885 0.00723 1.00000 0.02858 0.00000 0.00000 C9 0.30119 0.78809 -0.06475 1.00000 0.02387 0.02106 0.03243 0.00449 -0.00137 -0.00198 0.02579 0.00438 0.00017 0.00017 0.00009 0.00000 0.00130 0.00120 0.00131 0.00102 0.00104 0.00102 0.00053 H9 0.31812 0.84976 -0.05972 1.00000 0.03094 0.00000 0.00000 C10 0.27623 0.75875 -0.11196 1.00000 0.02624 0.02540 0.02734 0.00947 0.00286 0.00354 0.02632 0.00451 0.00017 0.00017 0.00009 0.00000 0.00133 0.00127 0.00125 0.00103 0.00101 0.00104 0.00054 H10 0.27581 0.80001 -0.13927 1.00000 0.03159 0.00000 0.00000 C11 0.25184 0.66855 -0.11896 1.00000 0.02948 0.02748 0.01994 -0.00027 -0.00034 0.00175 0.02563 0.00433 0.00018 0.00017 0.00009 0.00000 0.00136 0.00127 0.00111 0.00098 0.00102 0.00110 0.00053 H11 0.23570 0.64785 -0.15138 1.00000 0.03076 0.00000 0.00000 C12 0.25075 0.60842 -0.07927 1.00000 0.02549 0.02037 0.02236 -0.00029 0.00116 0.00001 0.02274 0.00416 0.00017 0.00016 0.00008 0.00000 0.00126 0.00114 0.00113 0.00092 0.00099 0.00100 0.00050 H12 0.23313 0.54699 -0.08449 1.00000 0.02729 0.00000 0.00000 C13 0.39651 0.36522 0.18478 1.00000 0.02591 0.01982 0.02004 -0.00097 -0.00544 -0.00047 0.02193 0.00393 0.00017 0.00016 0.00008 0.00000 0.00127 0.00116 0.00109 0.00090 0.00094 0.00098 0.00050 C14 0.48728 0.34668 0.17617 1.00000 0.02716 0.03481 0.02406 0.00335 -0.00031 0.00041 0.02868 0.00447 0.00018 0.00018 0.00009 0.00000 0.00136 0.00144 0.00121 0.00106 0.00104 0.00113 0.00057 H14 0.51646 0.36890 0.14697 1.00000 0.03441 0.00000 0.00000 C15 0.53512 0.29521 0.21072 1.00000 0.02565 0.05069 0.02959 0.00294 -0.00226 0.01211 0.03531 0.00503 0.00019 0.00020 0.00010 0.00000 0.00145 0.00176 0.00133 0.00126 0.00111 0.00128 0.00065 H15 0.59747 0.28207 0.20520 1.00000 0.04237 0.00000 0.00000 C16 0.49229 0.26287 0.25329 1.00000 0.04146 0.03240 0.02213 0.00223 -0.00551 0.01157 0.03200 0.00476 0.00020 0.00018 0.00010 0.00000 0.00161 0.00139 0.00118 0.00108 0.00110 0.00125 0.00061 H16 0.52503 0.22716 0.27674 1.00000 0.03840 0.00000 0.00000 C17 0.40159 0.28281 0.26151 1.00000 0.03803 0.02995 0.01867 -0.00029 -0.00170 0.00403 0.02888 0.00440 0.00019 0.00017 0.00009 0.00000 0.00155 0.00134 0.00116 0.00100 0.00106 0.00118 0.00058 H17 0.37230 0.26052 0.29066 1.00000 0.03466 0.00000 0.00000 C18 0.35322 0.33493 0.22763 1.00000 0.02494 0.03001 0.02047 -0.00074 -0.00116 0.00137 0.02514 0.00419 0.00018 0.00017 0.00008 0.00000 0.00130 0.00131 0.00112 0.00099 0.00097 0.00107 0.00053 H18 0.29139 0.34968 0.23365 1.00000 0.03017 0.00000 0.00000 N1 0.20129 0.51286 0.01196 1.00000 0.02002 0.01960 0.01606 0.00043 -0.00324 -0.00084 0.01856 0.00315 0.00013 0.00012 0.00007 0.00000 0.00102 0.00096 0.00088 0.00075 0.00075 0.00078 0.00040 H1 0.16289 0.51466 -0.01320 1.00000 0.02227 0.00000 0.00000 N2 0.38922 0.48588 0.12268 1.00000 0.02582 0.02316 0.02108 0.00485 -0.00464 -0.00416 0.02335 0.00337 0.00014 0.00013 0.00007 0.00000 0.00113 0.00103 0.00096 0.00081 0.00082 0.00087 0.00044 N3 0.34645 0.41422 0.14767 1.00000 0.02167 0.02116 0.01971 0.00286 -0.00297 -0.00255 0.02084 0.00326 0.00013 0.00013 0.00007 0.00000 0.00104 0.00099 0.00092 0.00078 0.00079 0.00081 0.00042 N4 0.20923 0.32281 0.14405 1.00000 0.02075 0.02265 0.02247 0.00331 -0.00115 0.00064 0.02196 0.00355 0.00014 0.00014 0.00007 0.00000 0.00108 0.00103 0.00101 0.00084 0.00081 0.00085 0.00043 H4A 0.16657 0.31225 0.12139 1.00000 0.03293 0.02587 0.00141 0.00186 0.00079 0.00000 0.00000 H4B 0.23835 0.27311 0.15435 1.00000 0.03293 0.04764 0.00170 0.00122 0.00097 0.00000 0.00000 O1 0.12093 0.39600 0.04734 1.00000 0.02056 0.02125 0.02263 0.00202 -0.00119 -0.00196 0.02148 0.00272 0.00011 0.00011 0.00006 0.00000 0.00087 0.00083 0.00081 0.00066 0.00066 0.00068 0.00036 C21 -0.00594 0.57234 0.06987 1.00000 0.01787 0.01741 0.02065 -0.00102 0.00058 0.00058 0.01864 0.00387 0.00015 0.00015 0.00008 0.00000 0.00116 0.00108 0.00107 0.00088 0.00088 0.00092 0.00046 C22 0.05742 0.58833 0.10927 1.00000 0.02162 0.01723 0.01752 -0.00155 0.00090 0.00084 0.01879 0.00384 0.00016 0.00015 0.00008 0.00000 0.00121 0.00110 0.00102 0.00086 0.00089 0.00090 0.00047 C23 0.12219 0.65933 0.10768 1.00000 0.02231 0.01696 0.01948 -0.00201 -0.00051 -0.00094 0.01958 0.00384 0.00016 0.00015 0.00008 0.00000 0.00122 0.00109 0.00107 0.00087 0.00091 0.00092 0.00047 C24 0.12292 0.72042 0.06631 1.00000 0.02437 0.01795 0.02220 -0.00004 -0.00114 -0.00495 0.02151 0.00397 0.00016 0.00016 0.00008 0.00000 0.00126 0.00113 0.00112 0.00090 0.00095 0.00095 0.00049 H24 0.16396 0.77022 0.06508 1.00000 0.02581 0.00000 0.00000 C25 0.06341 0.70509 0.02902 1.00000 0.01954 0.01914 0.01929 -0.00013 0.00016 -0.00062 0.01932 0.00389 0.00016 0.00015 0.00008 0.00000 0.00118 0.00111 0.00106 0.00088 0.00090 0.00091 0.00047 C26 0.07589 0.54107 0.15310 1.00000 0.02085 0.01837 0.01949 -0.00233 0.00283 0.00226 0.01957 0.00394 0.00016 0.00015 0.00008 0.00000 0.00120 0.00110 0.00106 0.00086 0.00092 0.00091 0.00047 C27 0.05898 0.76322 -0.01631 1.00000 0.01573 0.02215 0.02223 0.00255 -0.00105 -0.00027 0.02004 0.00397 0.00015 0.00016 0.00008 0.00000 0.00113 0.00117 0.00111 0.00092 0.00089 0.00092 0.00048 C28 0.07493 0.85692 -0.01251 1.00000 0.02341 0.02403 0.03045 0.00218 -0.00711 -0.00308 0.02596 0.00423 0.00017 0.00016 0.00010 0.00000 0.00129 0.00124 0.00127 0.00102 0.00104 0.00102 0.00054 H28 0.08827 0.88307 0.01910 1.00000 0.03116 0.00000 0.00000 C29 0.07135 0.91171 -0.05465 1.00000 0.02411 0.02258 0.04227 0.01049 -0.00279 -0.00138 0.02965 0.00464 0.00017 0.00017 0.00010 0.00000 0.00135 0.00129 0.00150 0.00110 0.00114 0.00103 0.00058 H29 0.08226 0.97518 -0.05184 1.00000 0.03558 0.00000 0.00000 C30 0.05185 0.87387 -0.10090 1.00000 0.02052 0.03801 0.02858 0.01490 0.00501 0.00238 0.02904 0.00476 0.00017 0.00018 0.00009 0.00000 0.00127 0.00150 0.00129 0.00114 0.00101 0.00112 0.00058 H30 0.04879 0.91144 -0.12972 1.00000 0.03484 0.00000 0.00000 C31 0.03687 0.78124 -0.10493 1.00000 0.02347 0.04125 0.01966 0.00600 0.00428 0.00272 0.02813 0.00470 0.00017 0.00019 0.00009 0.00000 0.00133 0.00153 0.00114 0.00107 0.00097 0.00113 0.00057 H31 0.02359 0.75544 -0.13663 1.00000 0.03375 0.00000 0.00000 C32 0.04107 0.72572 -0.06311 1.00000 0.01784 0.02701 0.02100 0.00201 0.00072 -0.00045 0.02195 0.00411 0.00016 0.00017 0.00008 0.00000 0.00118 0.00126 0.00112 0.00096 0.00091 0.00098 0.00050 H32 0.03173 0.66206 -0.06636 1.00000 0.02634 0.00000 0.00000 C33 0.19391 0.56466 0.22021 1.00000 0.02713 0.01862 0.01646 -0.00155 -0.00210 0.00404 0.02073 0.00397 0.00016 0.00016 0.00008 0.00000 0.00130 0.00110 0.00105 0.00088 0.00092 0.00098 0.00049 C34 0.28659 0.58129 0.22188 1.00000 0.03013 0.02139 0.02111 0.00027 -0.00124 -0.00092 0.02421 0.00411 0.00017 0.00016 0.00009 0.00000 0.00136 0.00121 0.00114 0.00094 0.00097 0.00103 0.00052 H34 0.31741 0.60355 0.19320 1.00000 0.02905 0.00000 0.00000 C35 0.33385 0.56508 0.26585 1.00000 0.02964 0.02463 0.02637 0.00120 -0.00544 -0.00145 0.02688 0.00429 0.00018 0.00017 0.00009 0.00000 0.00140 0.00125 0.00121 0.00100 0.00105 0.00109 0.00055 H35 0.39728 0.57651 0.26728 1.00000 0.03226 0.00000 0.00000 C36 0.28915 0.53238 0.30761 1.00000 0.03634 0.02363 0.02042 -0.00021 -0.00615 0.00571 0.02680 0.00436 0.00018 0.00017 0.00009 0.00000 0.00150 0.00124 0.00115 0.00097 0.00104 0.00110 0.00055 H36 0.32167 0.52152 0.33767 1.00000 0.03215 0.00000 0.00000 C37 0.19697 0.51561 0.30535 1.00000 0.03450 0.03109 0.01850 0.00417 0.00418 0.00773 0.02803 0.00464 0.00018 0.00018 0.00009 0.00000 0.00149 0.00137 0.00112 0.00101 0.00102 0.00116 0.00057 H37 0.16642 0.49270 0.33395 1.00000 0.03363 0.00000 0.00000 C38 0.14834 0.53183 0.26176 1.00000 0.02612 0.02838 0.02316 0.00420 0.00027 0.00424 0.02589 0.00446 0.00018 0.00017 0.00009 0.00000 0.00135 0.00128 0.00119 0.00100 0.00100 0.00106 0.00054 H38 0.08487 0.52059 0.26046 1.00000 0.03107 0.00000 0.00000 N21 0.00333 0.63201 0.03059 1.00000 0.01985 0.01993 0.01720 -0.00113 -0.00390 -0.00236 0.01900 0.00317 0.00013 0.00013 0.00007 0.00000 0.00101 0.00096 0.00088 0.00076 0.00076 0.00080 0.00041 H21 -0.03155 0.62328 0.00434 1.00000 0.02280 0.00000 0.00000 N22 0.17715 0.65822 0.14708 1.00000 0.02858 0.01911 0.01728 0.00307 -0.00281 -0.00212 0.02166 0.00332 0.00014 0.00013 0.00007 0.00000 0.00113 0.00097 0.00091 0.00077 0.00081 0.00083 0.00043 N23 0.14644 0.58497 0.17519 1.00000 0.02488 0.02073 0.01676 0.00070 -0.00152 -0.00056 0.02079 0.00328 0.00014 0.00013 0.00007 0.00000 0.00107 0.00099 0.00088 0.00076 0.00079 0.00082 0.00042 N24 0.03230 0.46646 0.17232 1.00000 0.02549 0.02517 0.02589 0.00795 -0.00201 -0.00288 0.02552 0.00374 0.00015 0.00014 0.00008 0.00000 0.00118 0.00112 0.00107 0.00088 0.00088 0.00090 0.00046 H24A -0.00694 0.44301 0.15057 1.00000 0.03827 0.02041 0.00157 0.00185 0.00085 0.00000 0.00000 H24B 0.06610 0.42794 0.19029 1.00000 0.03827 0.04856 0.00168 0.00159 0.00093 0.00000 0.00000 O21 -0.06539 0.51175 0.06957 1.00000 0.02132 0.01978 0.02803 0.00229 -0.00310 -0.00303 0.02304 0.00276 0.00011 0.00011 0.00006 0.00000 0.00088 0.00084 0.00087 0.00068 0.00069 0.00069 0.00037 Final Structure Factor Calculation for pbca in Pbca Total number of l.s. parameters = 428 Maximum vector length = 511 Memory required = 4549 / 22995 wR2 = 0.1346 before cycle 10 for 6537 data and 0 / 428 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.107; Restrained GooF = 1.107 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 9.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0654 for 5012 Fo > 4sig(Fo) and 0.0912 for all 6537 data wR2 = 0.1346, GooF = S = 1.107, Restrained GooF = 1.107 for all data Occupancy sum of asymmetric unit = 46.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0210 0.0191 0.0133 C1 0.0201 0.0165 0.0160 C2 0.0234 0.0201 0.0165 C3 0.0233 0.0209 0.0175 C4 0.0216 0.0189 0.0163 C5 0.0230 0.0205 0.0147 C6 0.0228 0.0202 0.0147 C7 0.0256 0.0242 0.0215 C8 0.0344 0.0239 0.0191 C9 0.0377 0.0245 0.0168 C10 0.0305 0.0265 0.0199 C11 0.0259 0.0220 0.0203 C12 0.0292 0.0202 0.0165 C13 0.0358 0.0272 0.0231 C14 0.0557 0.0305 0.0197 C15 0.0498 0.0282 0.0180 C16 0.0398 0.0283 0.0185 C17 0.0305 0.0248 0.0202 C18 0.0222 0.0193 0.0142 N1 0.0327 0.0204 0.0170 N2 0.0265 0.0189 0.0172 N3 0.0259 0.0215 0.0185 N4 0.0251 0.0205 0.0189 O1 0.0210 0.0183 0.0167 C21 0.0219 0.0189 0.0156 C22 0.0225 0.0206 0.0157 C23 0.0273 0.0221 0.0152 C24 0.0200 0.0192 0.0187 C25 0.0231 0.0211 0.0145 C26 0.0248 0.0197 0.0156 C27 0.0359 0.0235 0.0185 C28 0.0472 0.0237 0.0180 C29 0.0497 0.0215 0.0159 C30 0.0435 0.0246 0.0163 C31 0.0276 0.0206 0.0176 C32 0.0292 0.0173 0.0156 C33 0.0304 0.0213 0.0209 C34 0.0341 0.0243 0.0223 C35 0.0403 0.0224 0.0177 C36 0.0422 0.0249 0.0170 C37 0.0330 0.0246 0.0201 C38 0.0232 0.0202 0.0136 N21 0.0300 0.0201 0.0149 N22 0.0253 0.0207 0.0164 N23 0.0348 0.0243 0.0175 N24 0.0303 0.0214 0.0174 O21 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.015 0.023 0.031 0.041 0.053 0.067 0.088 0.128 1.000 Number in group 736. 586. 654. 639. 676. 666. 636. 645. 648. 651. GooF 1.162 1.202 1.241 1.146 1.152 1.133 1.085 0.985 0.916 1.007 K 5.482 1.568 1.183 1.085 1.025 1.008 0.988 1.006 1.004 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.32 1.66 inf Number in group 674. 643. 644. 662. 646. 664. 651. 641. 657. 655. GooF 1.286 1.257 1.182 1.150 1.129 1.055 1.039 0.900 0.922 1.083 K 1.132 1.091 1.053 1.024 0.993 0.992 0.993 1.002 1.014 1.008 R1 0.226 0.208 0.176 0.140 0.121 0.081 0.062 0.050 0.049 0.030 Recommended weighting scheme: WGHT 0.0000 9.3967 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) 7 7 17 2085.79 3124.43 4.60 0.155 1.08 6 9 9 161.20 19.54 3.98 0.012 1.24 19 2 1 597.93 44.41 3.96 0.018 0.77 0 8 20 152.70 488.30 3.70 0.061 1.08 18 2 2 283.63 61.60 3.63 0.022 0.81 17 5 7 474.75 112.52 3.62 0.029 0.81 16 3 13 -30.80 189.49 3.57 0.038 0.83 10 2 18 743.60 1146.46 3.56 0.094 1.04 6 3 0 583.33 280.51 3.53 0.046 2.19 4 11 24 589.71 304.79 3.50 0.048 0.83 6 1 32 112.68 0.03 3.45 0.000 0.79 13 10 17 264.90 60.46 3.45 0.022 0.78 11 5 19 271.65 551.84 3.42 0.065 0.92 3 0 28 1015.04 624.78 3.41 0.069 0.94 1 18 9 250.20 13.86 3.40 0.010 0.79 14 2 13 5.73 171.09 3.39 0.036 0.93 6 15 4 239.97 50.33 3.39 0.020 0.90 11 0 26 38.12 248.81 3.30 0.044 0.82 10 14 6 61.59 289.09 3.30 0.047 0.84 13 8 10 1127.46 707.14 3.29 0.074 0.91 1 16 16 649.28 307.41 3.27 0.049 0.80 12 3 0 1841.77 1244.85 3.26 0.098 1.19 15 2 19 342.75 63.35 3.24 0.022 0.80 2 18 7 730.08 389.16 3.21 0.055 0.79 8 16 1 103.71 0.28 3.21 0.001 0.82 2 4 11 25588.64 22916.28 3.19 0.419 1.96 5 1 1 3932.74 4711.43 3.18 0.190 2.87 2 2 14 101.66 261.22 3.18 0.045 1.79 10 0 20 90.93 3.28 3.16 0.005 0.99 6 6 0 163.15 39.68 3.12 0.017 1.73 13 9 6 1546.26 1077.45 3.09 0.091 0.91 0 2 6 1809.44 2312.27 3.04 0.133 3.81 3 2 34 97.05 1.35 3.00 0.003 0.77 6 9 28 103.89 1.47 2.99 0.003 0.78 15 9 5 25.34 158.09 2.99 0.035 0.83 10 14 11 202.73 1.14 2.99 0.003 0.81 4 2 31 87.50 1.08 2.98 0.003 0.84 9 6 12 76.11 0.19 2.97 0.001 1.16 9 11 2 270.87 73.16 2.95 0.024 1.03 18 0 0 1192.11 615.38 2.95 0.069 0.82 4 0 28 700.51 1091.37 2.92 0.092 0.93 4 2 29 81.53 0.00 2.91 0.000 0.89 10 14 4 378.68 184.87 2.91 0.038 0.85 12 13 4 303.19 90.35 2.90 0.026 0.83 7 8 22 -30.69 71.81 2.88 0.023 0.91 5 11 17 116.25 273.13 2.88 0.046 0.96 18 2 10 205.29 0.06 2.88 0.001 0.78 1 2 34 155.80 29.63 2.88 0.015 0.78 14 11 4 193.18 33.45 2.82 0.016 0.82 1 2 13 53.46 3.52 2.82 0.005 1.97 Bond lengths and angles C1 - Distance Angles O1 1.2467 (0.0027) N1 1.3726 (0.0028) 121.97 (0.20) C2 1.4238 (0.0031) 123.98 (0.20) 114.03 (0.20) C1 - O1 N1 C2 - Distance Angles C6 1.3894 (0.0030) C3 1.4135 (0.0032) 106.09 (0.20) C1 1.4238 (0.0031) 129.98 (0.21) 123.22 (0.20) C2 - C6 C3 C3 - Distance Angles N2 1.3356 (0.0029) C2 1.4135 (0.0032) 112.04 (0.20) C4 1.4384 (0.0031) 129.29 (0.22) 118.59 (0.20) C3 - N2 C2 C4 - Distance Angles C5 1.3503 (0.0031) C3 1.4384 (0.0031) 117.55 (0.21) H4 0.9500 121.23 121.23 C4 - C5 C3 C5 - Distance Angles C4 1.3503 (0.0031) N1 1.3974 (0.0029) 122.06 (0.21) C7 1.4854 (0.0031) 122.98 (0.21) 114.95 (0.19) C5 - C4 N1 C6 - Distance Angles N3 1.3597 (0.0029) N4 1.3738 (0.0030) 125.42 (0.20) C2 1.3894 (0.0030) 105.44 (0.20) 129.14 (0.21) C6 - N3 N4 C7 - Distance Angles C12 1.3974 (0.0031) C8 1.3984 (0.0033) 118.72 (0.21) C5 1.4854 (0.0031) 121.12 (0.21) 120.16 (0.21) C7 - C12 C8 C8 - Distance Angles C9 1.3834 (0.0033) C7 1.3984 (0.0033) 120.45 (0.23) H8 0.9500 119.77 119.77 C8 - C9 C7 C9 - Distance Angles C8 1.3834 (0.0033) C10 1.3852 (0.0035) 120.49 (0.23) H9 0.9500 119.76 119.76 C9 - C8 C10 C10 - Distance Angles C9 1.3852 (0.0035) C11 1.3867 (0.0035) 119.33 (0.22) H10 0.9500 120.33 120.33 C10 - C9 C11 C11 - Distance Angles C12 1.3823 (0.0032) C10 1.3867 (0.0035) 120.71 (0.23) H11 0.9500 119.64 119.64 C11 - C12 C10 C12 - Distance Angles C11 1.3823 (0.0032) C7 1.3974 (0.0031) 120.27 (0.22) H12 0.9500 119.86 119.86 C12 - C11 C7 C13 - Distance Angles C14 1.3838 (0.0036) C18 1.3858 (0.0033) 121.28 (0.22) N3 1.4318 (0.0029) 118.76 (0.21) 119.94 (0.22) C13 - C14 C18 C14 - Distance Angles C13 1.3838 (0.0036) C15 1.3874 (0.0035) 119.15 (0.24) H14 0.9500 120.43 120.43 C14 - C13 C15 C15 - Distance Angles C16 1.3866 (0.0037) C14 1.3874 (0.0035) 120.25 (0.25) H15 0.9500 119.87 119.87 C15 - C16 C14 C16 - Distance Angles C17 1.3854 (0.0038) C15 1.3866 (0.0037) 119.79 (0.24) H16 0.9500 120.11 120.11 C16 - C17 C15 C17 - Distance Angles C18 1.3847 (0.0033) C16 1.3854 (0.0038) 120.61 (0.24) H17 0.9500 119.70 119.70 C17 - C18 C16 C18 - Distance Angles C17 1.3847 (0.0033) C13 1.3858 (0.0033) 118.90 (0.24) H18 0.9500 120.55 120.55 C18 - C17 C13 N1 - Distance Angles C1 1.3726 (0.0028) C5 1.3974 (0.0029) 124.22 (0.19) H1 0.8800 117.89 117.89 N1 - C1 C5 N2 - Distance Angles C3 1.3356 (0.0029) N3 1.3980 (0.0026) 103.26 (0.18) N2 - C3 N3 - Distance Angles C6 1.3597 (0.0029) N2 1.3980 (0.0026) 113.16 (0.18) C13 1.4318 (0.0029) 127.32 (0.19) 118.63 (0.19) N3 - C6 N2 N4 - Distance Angles C6 1.3738 (0.0030) H4A 0.8871 (0.0097) 109.18 (1.82) H4B 0.8910 (0.0098) 114.25 (1.86) 114.15 (2.53) N4 - C6 H4A O1 - Distance Angles C1 1.2467 (0.0027) O1 - C21 - Distance Angles O21 1.2492 (0.0027) N21 1.3763 (0.0028) 121.28 (0.20) C22 1.4278 (0.0031) 125.48 (0.21) 113.24 (0.19) C21 - O21 N21 C22 - Distance Angles C26 1.3905 (0.0031) C23 1.4148 (0.0031) 105.20 (0.20) C21 1.4278 (0.0031) 131.99 (0.21) 122.68 (0.20) C22 - C26 C23 C23 - Distance Angles N22 1.3299 (0.0029) C22 1.4148 (0.0031) 112.18 (0.20) C24 1.4260 (0.0031) 128.26 (0.21) 119.56 (0.21) C23 - N22 C22 C24 - Distance Angles C25 1.3475 (0.0032) C23 1.4260 (0.0031) 117.72 (0.21) H24 0.9500 121.14 121.14 C24 - C25 C23 C25 - Distance Angles C24 1.3475 (0.0032) N21 1.3926 (0.0029) 121.34 (0.21) C27 1.4858 (0.0031) 122.51 (0.21) 116.14 (0.19) C25 - C24 N21 C26 - Distance Angles N23 1.3587 (0.0030) N24 1.3712 (0.0030) 125.09 (0.21) C22 1.3905 (0.0031) 106.23 (0.20) 128.66 (0.22) C26 - N23 N24 C27 - Distance Angles C32 1.3940 (0.0032) C28 1.4012 (0.0033) 119.07 (0.22) C25 1.4858 (0.0031) 120.99 (0.21) 119.92 (0.21) C27 - C32 C28 C28 - Distance Angles C29 1.3872 (0.0034) C27 1.4012 (0.0033) 120.36 (0.24) H28 0.9500 119.82 119.82 C28 - C29 C27 C29 - Distance Angles C28 1.3872 (0.0034) C30 1.3875 (0.0037) 120.05 (0.24) H29 0.9500 119.97 119.97 C29 - C28 C30 C30 - Distance Angles C31 1.3838 (0.0038) C29 1.3875 (0.0037) 119.81 (0.23) H30 0.9500 120.09 120.09 C30 - C31 C29 C31 - Distance Angles C30 1.3838 (0.0038) C32 1.3868 (0.0032) 120.61 (0.24) H31 0.9500 119.70 119.70 C31 - C30 C32 C32 - Distance Angles C31 1.3868 (0.0032) C27 1.3940 (0.0032) 120.08 (0.23) H32 0.9500 119.96 119.96 C32 - C31 C27 C33 - Distance Angles C38 1.3859 (0.0033) C34 1.3876 (0.0035) 120.79 (0.22) N23 1.4249 (0.0028) 120.94 (0.22) 118.24 (0.21) C33 - C38 C34 C34 - Distance Angles C33 1.3876 (0.0035) C35 1.3882 (0.0033) 119.37 (0.23) H34 0.9500 120.32 120.32 C34 - C33 C35 C35 - Distance Angles C36 1.3837 (0.0035) C34 1.3882 (0.0033) 120.40 (0.25) H35 0.9500 119.80 119.80 C35 - C36 C34 C36 - Distance Angles C37 1.3812 (0.0037) C35 1.3837 (0.0035) 119.63 (0.23) H36 0.9500 120.19 120.19 C36 - C37 C35 C37 - Distance Angles C36 1.3812 (0.0037) C38 1.3898 (0.0033) 120.85 (0.24) H37 0.9500 119.57 119.57 C37 - C36 C38 C38 - Distance Angles C33 1.3859 (0.0033) C37 1.3898 (0.0033) 118.95 (0.24) H38 0.9500 120.52 120.52 C38 - C33 C37 N21 - Distance Angles C21 1.3763 (0.0028) C25 1.3926 (0.0029) 125.31 (0.19) H21 0.8800 117.35 117.35 N21 - C21 C25 N22 - Distance Angles C23 1.3299 (0.0029) N23 1.3895 (0.0026) 103.94 (0.18) N22 - C23 N23 - Distance Angles C26 1.3587 (0.0030) N22 1.3895 (0.0026) 112.43 (0.18) C33 1.4249 (0.0028) 130.08 (0.20) 117.43 (0.18) N23 - C26 N22 N24 - Distance Angles C26 1.3712 (0.0030) H24A 0.8899 (0.0098) 111.63 (1.91) H24B 0.8944 (0.0098) 116.60 (1.91) 117.91 (2.67) N24 - C26 H24A O21 - Distance Angles C21 1.2492 (0.0027) O21 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.12 2.984(2) 167.2 N1-H1...O21_$1 0.887(10) 2.43(2) 3.091(3) 132(2) N4-H4A...O1 0.891(10) 2.107(15) 2.943(3) 156(2) N4-H4B...N22_$2 0.88 1.93 2.806(2) 172.7 N21-H21...O1_$1 0.890(10) 2.54(2) 3.175(3) 129(2) N24-H24A...O21 FMAP and GRID set by program FMAP 2 1 19 GRID -1.563 -2 -1 1.563 2 1 R1 = 0.0912 for 6537 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.2476 0.9142 0.1032 [ 0.68 A from C2 ] Deepest hole -0.26 at 0.0514 0.8184 0.2198 [ 1.34 A from C15 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 5209 / 47485 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2524 0.4142 0.1032 1.00000 0.05 0.32 0.68 C2 0.75 C6 1.83 N3 1.83 C1 Q2 1 0.2481 0.6809 -0.0287 1.00000 0.05 0.31 0.76 C7 1.06 C8 1.72 C12 1.74 H8 Q3 1 0.2461 0.6179 -0.0529 1.00000 0.05 0.28 0.72 C12 0.77 C7 1.36 H12 1.89 C5 Q4 1 0.0711 0.6380 0.1122 1.00000 0.05 0.27 0.76 C22 0.82 C23 1.80 C26 1.84 N22 Q5 1 0.2274 0.4419 0.0667 1.00000 0.05 0.27 0.68 C2 0.78 C1 1.78 O1 1.84 N1 Shortest distances between peaks (including symmetry equivalents) 1 5 1.12 2 3 1.13 Time profile in seconds ----------------------- 0.05: Read and process instructions 0.00: Fit rigid groups 0.01: Interpret restraints etc. 0.00: Generate connectivity array 0.01: 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 0.02: Analyse other restraints etc. 1.59: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 9.59: Structure factors and derivatives 16.64: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 1.64: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.23: Analysis of variance 0.09: Merge reflections for Fourier and .fcf 0.14: Fourier summations 0.10: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + pbca finished at 14:47:18 Total CPU time: 30.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++