+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0019p21 started at 16:13:56 on 07-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0019p21 in P2(1) CELL 0.71073 5.6889 8.9638 13.2457 90.000 97.112 90.000 ZERR 2.00 0.0004 0.0004 0.0011 0.000 0.003 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O S UNIT 28 34 2 6 2 V = 670.26 F(000) = 296.0 Mu = 0.24 mm-1 Cell Wt = 558.69 Rho = 1.384 MERG 2 OMIT -3.00 55.00 OMIT -3 0 11 SHEL 7 0.77 HTAB N21 O1B EQIV_$1 -x+2, y+1/2, -z+2 HTAB N21 O1A_$1 EQIV_$2 -x+1, y+1/2, -z+2 HTAB N21 O1B_$2 HTAB N21 O1C_$2 HTAB N21 S1_$2 FMAP 2 PLAN 10 SIZE 0.01 0.05 0.07 ACTA BOND $H WGHT 0.03630 0.12380 L.S. 4 TEMP -153.00 FVAR 1.51158 MOLE 1 C4 1 0.376817 0.372838 0.552419 11.00000 0.02275 0.02036 = 0.01774 -0.00055 0.00626 0.00185 C3 1 0.233412 0.269216 0.594306 11.00000 0.01285 0.02948 = 0.02100 -0.00092 0.00144 0.00030 AFIX 43 H3 2 0.078280 0.250305 0.561379 11.00000 -1.20000 AFIX 0 C2 1 0.313243 0.193792 0.682748 11.00000 0.01842 0.01886 = 0.02256 -0.00079 0.00755 0.00114 AFIX 43 H2 2 0.212731 0.124435 0.710660 11.00000 -1.20000 AFIX 0 C1 1 0.540877 0.219371 0.730982 11.00000 0.01624 0.01400 = 0.01566 0.00086 0.00269 0.00418 C6 1 0.688286 0.321520 0.689665 11.00000 0.01633 0.01846 = 0.01633 -0.00066 0.00584 0.00349 AFIX 43 H6 2 0.844320 0.339436 0.721937 11.00000 -1.20000 AFIX 0 C5 1 0.603830 0.396113 0.601179 11.00000 0.02255 0.01971 = 0.02091 -0.00003 0.00784 -0.00053 AFIX 43 H5 2 0.704217 0.465270 0.573003 11.00000 -1.20000 AFIX 0 C7 1 0.287777 0.455696 0.456301 11.00000 0.02718 0.03288 = 0.02274 -0.00033 0.00248 0.00036 AFIX 137 H7A 2 0.114184 0.454798 0.446726 11.00000 -1.50000 H7B 2 0.346951 0.407171 0.398132 11.00000 -1.50000 H7C 2 0.344274 0.559022 0.461519 11.00000 -1.50000 AFIX 0 O1A 4 0.897891 0.114688 0.847760 11.00000 0.01420 0.02908 = 0.02503 0.00838 0.00219 0.00480 O1B 4 0.573666 0.219146 0.928569 11.00000 0.02523 0.02100 = 0.01983 -0.00062 0.00660 0.00242 O1C 4 0.521996 -0.017151 0.842219 11.00000 0.02534 0.01611 = 0.02363 0.00349 0.00386 0.00172 S1 5 0.642883 0.125457 0.845884 11.00000 0.01598 0.01811 = 0.01652 0.00200 0.00342 0.00205 MOLE 2 C24 1 1.144947 0.665305 0.768419 11.00000 0.02322 0.01709 = 0.02017 -0.00517 0.00152 -0.00579 C23 1 1.217123 0.534605 0.818345 11.00000 0.01893 0.02193 = 0.02407 -0.00990 0.00360 0.00284 AFIX 43 H23 2 1.351635 0.483344 0.799922 11.00000 -1.20000 AFIX 0 C22 1 1.098055 0.476616 0.894562 11.00000 0.02343 0.01134 = 0.02321 -0.00074 0.00289 -0.00198 AFIX 43 H22 2 1.149984 0.386801 0.928304 11.00000 -1.20000 AFIX 0 C21 1 0.901944 0.551981 0.920659 11.00000 0.01747 0.02562 = 0.01091 -0.00361 0.00317 -0.00144 C26 1 0.826661 0.681914 0.872789 11.00000 0.02082 0.02070 = 0.02448 -0.00622 0.00054 0.00435 AFIX 43 H26 2 0.691061 0.732287 0.890918 11.00000 -1.20000 AFIX 0 C25 1 0.949991 0.739263 0.797682 11.00000 0.02848 0.02128 = 0.02089 0.00250 0.00032 0.00451 AFIX 43 H25 2 0.900289 0.830745 0.765671 11.00000 -1.20000 AFIX 0 C27 1 1.273993 0.726419 0.684557 11.00000 0.03140 0.02844 = 0.02150 -0.00072 0.00619 0.00039 AFIX 137 H27A 2 1.295348 0.834296 0.693536 11.00000 -1.50000 H27B 2 1.181256 0.706461 0.618557 11.00000 -1.50000 H27C 2 1.429223 0.678207 0.687090 11.00000 -1.50000 AFIX 0 N21 3 0.776527 0.491491 1.001782 11.00000 0.01937 0.02205 = 0.01794 -0.00490 0.00224 -0.00119 AFIX 137 H21A 2 0.877621 0.486094 1.060546 11.00000 -1.50000 H21B 2 0.721290 0.398649 0.984075 11.00000 -1.50000 H21C 2 0.652789 0.552169 1.011101 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0019p21 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C4 - C5 C3 C7 C3 - C2 C4 C2 - C3 C1 C1 - C2 C6 S1 C6 - C5 C1 C5 - C6 C4 C7 - C4 O1A - S1 O1B - S1 O1C - S1 S1 - O1C O1A O1B C1 C24 - C23 C25 C27 C23 - C24 C22 C22 - C21 C23 C21 - C26 C22 N21 C26 - C21 C25 C25 - C26 C24 C27 - C24 N21 - C21 Operators for generating equivalent atoms: $1 -x+2, y+1/2, -z+2 $2 -x+1, y+1/2, -z+2 Floating origin restraints generated 8560 Reflections read, of which 20 rejected -7 =< h =< 7, -11 =< k =< 11, -17 =< l =< 17, Max. 2-theta = 54.95 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -1 -3 14 557.21 96.50 2 851.05 0 2 14 290.77 56.24 2 322.72 2 Inconsistent equivalents 2844 Unique reflections, of which 0 suppressed R(int) = 0.0772 R(sigma) = 0.1010 Friedel opposites not merged Maximum memory for data reduction = 2088 / 28805 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 = 2590 / 218617 wR2 = 0.1066 before cycle 1 for 2844 data and 175 / 175 parameters GooF = S = 1.035; Restrained GooF = 1.034 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0363 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51166 0.00296 0.027 OSF Mean shift/esd = 0.007 Maximum = 0.027 for y C5 Max. shift = 0.001 A for H7A Max. dU = 0.000 for O1B Least-squares cycle 2 Maximum vector length = 511 Memory required = 2590 / 218617 wR2 = 0.1066 before cycle 2 for 2844 data and 175 / 175 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0363 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51165 0.00296 -0.002 OSF Mean shift/esd = 0.002 Maximum = 0.013 for tors H7A Max. shift = 0.000 A for H7A Max. dU = 0.000 for O1B Least-squares cycle 3 Maximum vector length = 511 Memory required = 2590 / 218617 wR2 = 0.1066 before cycle 3 for 2844 data and 175 / 175 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0363 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51165 0.00296 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.004 for tors H7A Max. shift = 0.000 A for H7C Max. dU = 0.000 for C7 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2590 / 218617 wR2 = 0.1066 before cycle 4 for 2844 data and 175 / 175 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0363 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.51165 0.00296 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for tors H7A Max. shift = 0.000 A for H7B Max. dU = 0.000 for C5 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.0783 0.2503 0.5614 43 0.950 0.000 C3 C2 C4 H2 0.2127 0.1244 0.7107 43 0.950 0.000 C2 C3 C1 H6 0.8443 0.3394 0.7219 43 0.950 0.000 C6 C5 C1 H5 0.7042 0.4653 0.5730 43 0.950 0.000 C5 C6 C4 H7A 0.1142 0.4549 0.4468 137 0.980 0.000 C7 C4 H7A H7B 0.3468 0.4071 0.3981 137 0.980 0.000 C7 C4 H7A H7C 0.3444 0.5590 0.4615 137 0.980 0.000 C7 C4 H7A H23 1.3516 0.4834 0.7999 43 0.950 0.000 C23 C24 C22 H22 1.1500 0.3868 0.9283 43 0.950 0.000 C22 C21 C23 H26 0.6911 0.7323 0.8909 43 0.950 0.000 C26 C21 C25 H25 0.9003 0.8307 0.7657 43 0.950 0.000 C25 C26 C24 H27A 1.2953 0.8343 0.6935 137 0.980 0.000 C27 C24 H27A H27B 1.1812 0.7065 0.6186 137 0.980 0.000 C27 C24 H27A H27C 1.4292 0.6782 0.6871 137 0.980 0.000 C27 C24 H27A H21A 0.8776 0.4861 1.0605 137 0.910 0.000 N21 C21 H21A H21B 0.7213 0.3987 0.9841 137 0.910 0.000 N21 C21 H21A H21C 0.6528 0.5522 1.0111 137 0.910 0.000 N21 C21 H21A 06skc0019p21 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C4 0.37681 0.37284 0.55242 1.00000 0.02275 0.02039 0.01773 -0.00055 0.00625 0.00187 0.01998 0.00641 0.00063 0.00038 0.00027 0.00000 0.00197 0.00200 0.00211 0.00153 0.00162 0.00143 0.00082 C3 0.23342 0.26922 0.59431 1.00000 0.01287 0.02948 0.02098 -0.00092 0.00143 0.00029 0.02117 0.00634 0.00060 0.00038 0.00028 0.00000 0.00184 0.00215 0.00219 0.00162 0.00156 0.00142 0.00084 H3 0.07829 0.25031 0.56138 1.00000 0.02540 0.00000 0.00000 C2 0.31324 0.19379 0.68275 1.00000 0.01843 0.01885 0.02257 -0.00080 0.00756 0.00115 0.01953 0.00627 0.00058 0.00037 0.00028 0.00000 0.00190 0.00181 0.00212 0.00153 0.00155 0.00143 0.00079 H2 0.21273 0.12443 0.71067 1.00000 0.02343 0.00000 0.00000 C1 0.54088 0.21937 0.73098 1.00000 0.01623 0.01400 0.01564 0.00086 0.00269 0.00419 0.01523 0.00586 0.00055 0.00035 0.00025 0.00000 0.00175 0.00185 0.00193 0.00141 0.00145 0.00136 0.00074 C6 0.68827 0.32151 0.68967 1.00000 0.01633 0.01844 0.01634 -0.00066 0.00581 0.00350 0.01672 0.00630 0.00060 0.00036 0.00027 0.00000 0.00183 0.00190 0.00201 0.00146 0.00148 0.00136 0.00077 H6 0.84431 0.33942 0.72194 1.00000 0.02006 0.00000 0.00000 C5 0.60382 0.39613 0.60117 1.00000 0.02256 0.01970 0.02088 -0.00006 0.00783 -0.00053 0.02062 0.00640 0.00063 0.00037 0.00027 0.00000 0.00203 0.00195 0.00219 0.00160 0.00166 0.00145 0.00083 H5 0.70421 0.46529 0.57300 1.00000 0.02474 0.00000 0.00000 C7 0.28778 0.45571 0.45630 1.00000 0.02715 0.03288 0.02276 -0.00033 0.00247 0.00038 0.02765 0.00683 0.00065 0.00042 0.00028 0.00000 0.00223 0.00226 0.00225 0.00178 0.00177 0.00172 0.00092 H7A 0.11419 0.45490 0.44676 1.00000 0.04147 0.00000 0.00000 H7B 0.34683 0.40712 0.39813 1.00000 0.04147 0.00000 0.00000 H7C 0.34442 0.55900 0.46149 1.00000 0.04147 0.00000 0.00000 O1A 0.89790 0.11469 0.84776 1.00000 0.01421 0.02906 0.02504 0.00838 0.00218 0.00478 0.02279 0.00431 0.00035 0.00031 0.00017 0.00000 0.00111 0.00127 0.00135 0.00125 0.00096 0.00119 0.00053 O1B 0.57367 0.21915 0.92857 1.00000 0.02520 0.02101 0.01981 -0.00064 0.00659 0.00241 0.02169 0.00417 0.00039 0.00025 0.00018 0.00000 0.00136 0.00131 0.00144 0.00107 0.00111 0.00106 0.00057 O1C 0.52200 -0.01715 0.84222 1.00000 0.02535 0.01612 0.02363 0.00349 0.00387 0.00174 0.02163 0.00438 0.00040 0.00025 0.00019 0.00000 0.00142 0.00128 0.00147 0.00101 0.00112 0.00104 0.00057 S1 0.64288 0.12546 0.84588 1.00000 0.01598 0.01810 0.01652 0.00201 0.00343 0.00205 0.01675 0.00147 0.00014 0.00009 0.00006 0.00000 0.00039 0.00041 0.00043 0.00040 0.00031 0.00040 0.00020 C24 1.14495 0.66530 0.76842 1.00000 0.02321 0.01710 0.02016 -0.00516 0.00151 -0.00580 0.02026 0.00594 0.00062 0.00034 0.00028 0.00000 0.00194 0.00208 0.00207 0.00142 0.00155 0.00134 0.00085 C23 1.21712 0.53461 0.81834 1.00000 0.01891 0.02196 0.02405 -0.00987 0.00361 0.00284 0.02156 0.00615 0.00062 0.00038 0.00028 0.00000 0.00201 0.00205 0.00215 0.00163 0.00167 0.00147 0.00083 H23 1.35164 0.48336 0.79992 1.00000 0.02587 0.00000 0.00000 C22 1.09806 0.47661 0.89456 1.00000 0.02341 0.01137 0.02321 -0.00077 0.00289 -0.00199 0.01933 0.00614 0.00060 0.00038 0.00027 0.00000 0.00196 0.00170 0.00210 0.00149 0.00160 0.00141 0.00078 H22 1.14997 0.38679 0.92830 1.00000 0.02319 0.00000 0.00000 C21 0.90194 0.55199 0.92065 1.00000 0.01746 0.02565 0.01090 -0.00362 0.00317 -0.00144 0.01788 0.00625 0.00063 0.00041 0.00026 0.00000 0.00200 0.00189 0.00184 0.00158 0.00157 0.00140 0.00078 C26 0.82666 0.68190 0.87279 1.00000 0.02082 0.02068 0.02449 -0.00621 0.00053 0.00436 0.02219 0.00618 0.00063 0.00036 0.00030 0.00000 0.00194 0.00195 0.00219 0.00161 0.00160 0.00143 0.00085 H26 0.69105 0.73227 0.89092 1.00000 0.02662 0.00000 0.00000 C25 0.94999 0.73926 0.79769 1.00000 0.02851 0.02129 0.02087 0.00250 0.00032 0.00450 0.02379 0.00653 0.00063 0.00041 0.00029 0.00000 0.00213 0.00198 0.00212 0.00154 0.00172 0.00155 0.00085 H25 0.90029 0.83075 0.76568 1.00000 0.02855 0.00000 0.00000 C27 1.27399 0.72642 0.68456 1.00000 0.03143 0.02841 0.02151 -0.00072 0.00621 0.00039 0.02687 0.00705 0.00066 0.00043 0.00029 0.00000 0.00217 0.00210 0.00216 0.00167 0.00171 0.00167 0.00087 H27A 1.29535 0.83430 0.69354 1.00000 0.04031 0.00000 0.00000 H27B 1.18125 0.70648 0.61856 1.00000 0.04031 0.00000 0.00000 H27C 1.42922 0.67821 0.68708 1.00000 0.04031 0.00000 0.00000 N21 0.77653 0.49149 1.00178 1.00000 0.01937 0.02204 0.01796 -0.00489 0.00225 -0.00119 0.01979 0.00508 0.00047 0.00032 0.00022 0.00000 0.00161 0.00153 0.00169 0.00128 0.00130 0.00124 0.00067 H21A 0.87764 0.48607 1.06054 1.00000 0.02969 0.00000 0.00000 H21B 0.72127 0.39865 0.98407 1.00000 0.02969 0.00000 0.00000 H21C 0.65281 0.55217 1.01111 1.00000 0.02969 0.00000 0.00000 Final Structure Factor Calculation for 06skc0019p21 in P2(1) Total number of l.s. parameters = 175 Maximum vector length = 511 Memory required = 2417 / 26068 wR2 = 0.1066 before cycle 5 for 2844 data and 2 / 175 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0363 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0579 for 2227 Fo > 4sig(Fo) and 0.0831 for all 2844 data wR2 = 0.1066, GooF = S = 1.035, Restrained GooF = 1.035 for all data Flack x parameter = -0.1384 with esd 0.1030 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.0248 0.0204 0.0148 C4 0.0296 0.0210 0.0129 C3 0.0254 0.0193 0.0139 C2 0.0196 0.0153 0.0108 C1 0.0215 0.0180 0.0107 C6 0.0264 0.0197 0.0158 C5 0.0329 0.0273 0.0227 C7 0.0359 0.0200 0.0125 O1A 0.0273 0.0213 0.0165 O1B 0.0265 0.0237 0.0147 O1C 0.0205 0.0152 0.0145 S1 0.0270 0.0225 0.0113 C24 0.0333 0.0200 0.0114 C23 0.0237 0.0232 0.0110 C22 0.0267 0.0172 0.0097 C21 0.0317 0.0202 0.0147 C26 0.0312 0.0233 0.0169 C25 0.0319 0.0285 0.0202 C27 0.0253 0.0194 0.0147 N21 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.050 0.070 0.092 0.109 0.131 0.152 0.182 0.225 0.292 1.000 Number in group 294. 281. 285. 284. 285. 284. 278. 283. 284. 286. GooF 0.944 1.051 1.048 1.002 0.964 1.102 1.071 1.144 1.009 1.003 K 1.924 1.241 1.102 1.089 1.102 1.041 1.010 1.005 0.999 1.003 Resolution(A) 0.77 0.80 0.84 0.88 0.93 1.00 1.07 1.18 1.35 1.70 inf Number in group 293. 276. 298. 277. 282. 280. 288. 282. 282. 286. GooF 1.016 1.031 0.976 1.051 1.023 0.981 1.054 1.022 1.035 1.150 K 1.091 1.078 1.095 1.159 1.049 1.004 1.007 0.990 1.004 1.002 R1 0.208 0.203 0.141 0.141 0.103 0.069 0.058 0.039 0.035 0.026 Recommended weighting scheme: WGHT 0.0371 0.1195 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) 2 -11 0 -5.83 150.65 4.18 0.183 0.78 0 -4 1 123.24 101.60 3.34 0.151 2.21 -5 1 5 346.22 423.63 3.31 0.307 1.08 -4 2 10 131.27 220.03 3.29 0.222 1.00 0 -7 9 110.03 159.66 3.25 0.189 0.96 2 11 0 63.36 152.94 3.23 0.185 0.78 -3 -4 5 60.63 91.57 3.22 0.143 1.32 5 -3 5 93.09 131.88 3.17 0.172 0.94 0 0 6 294.02 352.49 3.15 0.280 2.19 2 -6 6 20.73 4.94 3.15 0.033 1.10 4 -4 4 111.15 154.17 3.07 0.185 1.09 -6 -5 6 64.84 20.86 3.05 0.068 0.81 5 1 2 40.68 13.16 3.00 0.054 1.08 2 2 3 15.03 2.62 2.97 0.024 2.01 1 1 8 118.20 84.16 2.95 0.137 1.51 -6 2 9 5.65 36.84 2.85 0.091 0.83 1 0 4 332.17 384.28 2.82 0.293 2.70 -2 2 7 73.78 97.39 2.81 0.147 1.56 3 4 2 126.80 155.68 2.78 0.186 1.38 -2 -2 5 69.91 51.73 2.77 0.107 1.87 5 3 3 87.42 133.00 2.77 0.172 1.00 5 -2 0 43.17 16.04 2.75 0.060 1.09 4 -1 0 54.12 28.57 2.75 0.080 1.39 3 -3 11 268.40 193.78 2.73 0.208 0.91 -5 -1 13 37.02 84.13 2.72 0.137 0.80 3 0 1 2884.90 2566.54 2.71 0.757 1.83 0 9 2 580.70 451.51 2.68 0.317 0.98 2 -3 7 222.07 262.81 2.68 0.242 1.33 3 -4 6 236.28 278.67 2.67 0.249 1.15 5 -2 1 136.21 98.19 2.63 0.148 1.08 -3 7 9 314.08 246.74 2.62 0.235 0.89 2 -10 2 166.23 59.93 2.61 0.116 0.84 -1 11 1 94.52 39.80 2.56 0.094 0.81 5 1 1 152.53 92.51 2.56 0.144 1.10 -2 4 10 130.07 166.89 2.55 0.193 1.09 -1 4 11 0.98 30.33 2.55 0.082 1.06 2 0 3 135.25 109.54 2.54 0.156 2.25 -1 10 6 0.78 32.75 2.54 0.085 0.83 4 -1 2 84.08 107.33 2.52 0.155 1.33 -3 -6 11 -3.14 22.45 2.52 0.071 0.87 1 11 0 347.74 252.97 2.51 0.238 0.81 -4 0 11 63.27 13.42 2.48 0.055 0.97 -1 -3 5 1129.29 1009.45 2.47 0.475 1.92 -2 1 1 943.31 841.95 2.46 0.433 2.70 2 7 6 137.88 188.28 2.45 0.205 1.01 0 -1 16 0.97 35.92 2.45 0.090 0.82 1 -8 8 77.73 111.05 2.44 0.157 0.90 2 0 4 103.25 127.46 2.43 0.169 2.02 -3 1 1 190.07 156.78 2.42 0.187 1.85 1 3 0 224.25 254.03 2.42 0.238 2.64 Bond lengths and angles C4 - Distance Angles C5 1.3863 (0.0050) C3 1.3957 (0.0047) 118.14 (0.32) C7 1.5065 (0.0050) 121.05 (0.33) 120.81 (0.32) C4 - C5 C3 C3 - Distance Angles C2 1.3799 (0.0048) C4 1.3957 (0.0047) 121.10 (0.32) H3 0.9500 119.45 119.45 C3 - C2 C4 C2 - Distance Angles C3 1.3799 (0.0048) C1 1.3902 (0.0045) 119.95 (0.32) H2 0.9500 120.03 120.03 C2 - C3 C1 C1 - Distance Angles C2 1.3902 (0.0045) C6 1.3980 (0.0045) 119.86 (0.31) S1 1.7729 (0.0034) 120.22 (0.26) 119.90 (0.25) C1 - C2 C6 C6 - Distance Angles C5 1.3830 (0.0049) C1 1.3980 (0.0045) 119.09 (0.32) H6 0.9500 120.45 120.45 C6 - C5 C1 C5 - Distance Angles C6 1.3830 (0.0049) C4 1.3863 (0.0050) 121.86 (0.33) H5 0.9500 119.07 119.07 C5 - C6 C4 C7 - Distance Angles C4 1.5065 (0.0050) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C4 H7A H7B O1A - Distance Angles S1 1.4511 (0.0021) O1A - O1B - Distance Angles S1 1.4720 (0.0024) O1B - O1C - Distance Angles S1 1.4495 (0.0024) O1C - S1 - Distance Angles O1C 1.4495 (0.0025) O1A 1.4511 (0.0021) 114.27 (0.15) O1B 1.4720 (0.0024) 111.01 (0.14) 112.59 (0.14) C1 1.7729 (0.0034) 106.65 (0.15) 105.46 (0.14) 106.17 (0.15) S1 - O1C O1A O1B C24 - Distance Angles C23 1.3823 (0.0046) C25 1.3880 (0.0049) 118.13 (0.34) C27 1.5083 (0.0050) 121.15 (0.33) 120.71 (0.32) C24 - C23 C25 C23 - Distance Angles C24 1.3823 (0.0046) C22 1.3848 (0.0047) 121.59 (0.33) H23 0.9500 119.21 119.21 C23 - C24 C22 C22 - Distance Angles C21 1.3843 (0.0047) C23 1.3848 (0.0047) 118.74 (0.34) H22 0.9500 120.63 120.63 C22 - C21 C23 C21 - Distance Angles C26 1.3690 (0.0047) C22 1.3843 (0.0047) 121.01 (0.35) N21 1.4655 (0.0044) 120.10 (0.33) 118.88 (0.32) C21 - C26 C22 C26 - Distance Angles C21 1.3690 (0.0047) C25 1.3853 (0.0054) 119.41 (0.35) H26 0.9500 120.30 120.30 C26 - C21 C25 C25 - Distance Angles C26 1.3853 (0.0054) C24 1.3880 (0.0049) 121.10 (0.34) H25 0.9500 119.45 119.45 C25 - C26 C24 C27 - Distance Angles C24 1.5083 (0.0050) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C24 H27A H27B N21 - Distance Angles C21 1.4655 (0.0044) H21A 0.9100 109.47 H21B 0.9100 109.47 109.47 H21C 0.9100 109.47 109.47 109.47 N21 - C21 H21A H21B Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.92 2.820(4) 170.6 N21-H21B...O1B 0.91 2.01 2.776(4) 140.6 N21-H21A...O1A_$1 0.91 2.19 3.072(4) 163.4 N21-H21C...O1B_$2 0.91 2.37 2.833(4) 111.4 N21-H21C...O1C_$2 0.91 2.76 3.521(3) 141.4 N21-H21C...S1_$2 FMAP and GRID set by program FMAP 2 1 16 GRID -3.846 -2 -2 3.846 2 2 R1 = 0.0758 for 1636 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.34 at 0.0695 -0.0073 0.1293 [ 0.88 A from C21 ] Deepest hole -0.35 at 0.3101 0.5882 0.1971 [ 0.74 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2522 / 18551 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9305 0.4927 0.8707 1.00000 0.05 0.34 0.88 C21 0.98 C22 1.68 H22 1.80 C26 Q2 1 1.1052 0.1801 0.8034 1.00000 0.05 0.33 1.50 O1A 1.52 H2 2.11 C2 2.24 H6 Q3 1 0.1802 0.6349 0.4837 1.00000 0.05 0.29 1.22 H7C 1.71 H7A 1.77 C7 1.84 H3 Q4 1 1.3718 0.4032 1.0347 1.00000 0.05 0.29 1.78 H22 1.81 O1C 1.88 H26 2.14 H21C Q5 1 1.5341 0.8219 0.7205 1.00000 0.05 0.27 1.37 H27A 1.46 H27C 1.72 C27 1.94 H7B Q6 1 0.6075 0.1309 0.7744 1.00000 0.05 0.27 0.95 S1 1.02 C1 1.71 O1C 1.82 O1A Q7 1 0.9122 0.0390 0.7663 1.00000 0.05 0.27 1.29 O1A 1.87 H25 2.09 H2 2.11 S1 Q8 1 0.6563 -0.0906 0.8874 1.00000 0.05 0.26 1.12 O1C 1.60 H26 2.01 S1 2.28 C26 Q9 1 0.4962 0.2064 0.8718 1.00000 0.05 0.25 0.83 O1B 1.19 S1 1.92 C1 2.05 O1C Q10 1 0.6245 0.2861 0.5237 1.00000 0.05 0.25 1.44 C5 1.69 C4 1.77 H5 2.05 H7C Shortest distances between peaks (including symmetry equivalents) 4 8 1.06 6 9 1.65 2 7 1.71 3 10 1.76 6 7 1.93 2 9 2.31 5 8 2.37 6 8 2.48 7 8 2.57 8 9 2.81 2 6 2.84 5 6 2.88 5 7 2.91 4 9 2.94 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.39: 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 0.55: Structure factors and derivatives 0.63: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.08: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0019p21 finished at 16:13:58 Total CPU time: 1.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++