+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0032p21c started at 12:20:15 on 06-May-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0032p21c in P2(1)/c CELL 0.71073 13.5580 9.1910 25.2770 90.000 105.232 90.000 ZERR 4.00 0.0005 0.0003 0.0009 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 96 208 8 36 V = 3039.15 F(000) = 1128.0 Mu = 0.08 mm-1 Cell Wt = 2050.70 Rho = 1.120 MERG 2 OMIT -3.00 55.00 OMIT 1 1 1 DFIX 0.84 0.02 O1W H1W O1W H2W DANG 1.35 0.02 H1W H2W SHEL 7 0.77 HTAB O1A O31A HTAB N25 O1W EQIV_$1 x, y+1, z HTAB N25 O1B_$1 HTAB O1W O31B_$1 EQIV_$2 -x+2, y+1/2, -z+1/2 HTAB N25 O4B_$2 HTAB O1W O4A_$2 EQIV_$3 x-1, y, z HTAB O34A O4A_$3 EQIV_$4 -x+1, y-1/2, -z+1/2 HTAB N45 O31B_$4 HTAB N45 O34B_$4 EQIV_$5 x, y-1, z HTAB N45 O1W_$5 HTAB N45 O34B_$5 MPLA C31 O31A O31B MPLA C34 O34A O34B FMAP 2 CONF PLAN 10 SIZE 0.01 0.05 0.15 ACTA BOND $H WGHT 0.00000 7.57040 L.S. 4 TEMP -153.00 FVAR 0.40269 C1 1 0.928704 0.700003 0.120041 11.00000 0.01755 0.03275 = 0.01840 -0.00711 0.00060 -0.00349 C2 1 0.987455 0.776093 0.085432 11.00000 0.02387 0.03564 = 0.02073 0.00044 0.00723 0.00064 AFIX 23 H2A 2 0.971323 0.881294 0.084177 11.00000 -1.20000 H2B 2 0.965327 0.737988 0.047517 11.00000 -1.20000 AFIX 0 C3 1 1.101674 0.756112 0.106977 11.00000 0.02114 0.03244 = 0.02270 -0.00013 0.00827 0.00000 AFIX 23 H3A 2 1.136302 0.807915 0.082564 11.00000 -1.20000 H3B 2 1.118150 0.651368 0.106025 11.00000 -1.20000 AFIX 0 C4 1 1.142840 0.812153 0.165051 11.00000 0.02736 0.01863 = 0.02042 0.00458 0.01124 -0.00325 O1A 4 0.841737 0.764120 0.119034 11.00000 0.02292 0.03378 = 0.04469 0.01127 0.01498 0.00485 AFIX 147 H1 2 0.811730 0.717627 0.138835 11.00000 -1.50000 AFIX 0 O1B 4 0.958899 0.589061 0.145484 11.00000 0.02458 0.02330 = 0.03817 0.00607 0.00988 0.00318 O4A 4 1.237749 0.788911 0.187220 11.00000 0.01803 0.03813 = 0.02623 -0.00418 0.00414 -0.00197 O4B 4 1.084156 0.875529 0.187584 11.00000 0.02435 0.02861 = 0.02416 -0.00198 0.00992 0.00080 MOLE 2 C21 1 0.732720 1.378058 0.076240 11.00000 0.04841 0.03235 = 0.02424 -0.00336 -0.00336 0.00045 AFIX 137 H21A 2 0.677140 1.384047 0.042504 11.00000 -1.50000 H21B 2 0.778430 1.461675 0.078311 11.00000 -1.50000 H21C 2 0.704073 1.378623 0.108026 11.00000 -1.50000 AFIX 0 C22 1 0.792538 1.238018 0.076052 11.00000 0.03591 0.02215 = 0.02520 -0.00350 0.00852 -0.00208 C23 1 0.895113 1.231696 0.121088 11.00000 0.03135 0.02014 = 0.02560 0.00147 0.00927 0.00368 AFIX 23 H23A 2 0.929693 1.141681 0.114028 11.00000 -1.20000 H23B 2 0.936678 1.313687 0.113439 11.00000 -1.20000 AFIX 0 C24 1 0.906541 1.234948 0.183271 11.00000 0.02961 0.01786 = 0.02186 -0.00190 0.00986 0.00224 C26 1 0.822714 1.230639 0.021573 11.00000 0.06484 0.04509 = 0.02387 -0.00232 0.01281 -0.00609 AFIX 137 H26A 2 0.761200 1.237867 -0.009067 11.00000 -1.50000 H26B 2 0.857220 1.138033 0.019337 11.00000 -1.50000 H26C 2 0.868955 1.311315 0.019727 11.00000 -1.50000 AFIX 0 C27 1 0.722493 1.108533 0.078082 11.00000 0.04780 0.03364 = 0.03598 0.00122 0.00316 -0.01044 AFIX 137 H27A 2 0.693307 1.119438 0.109455 11.00000 -1.50000 H27B 2 0.762118 1.018167 0.081947 11.00000 -1.50000 H27C 2 0.667242 1.105153 0.044142 11.00000 -1.50000 AFIX 0 C28 1 0.856714 1.108341 0.205227 11.00000 0.04846 0.02122 = 0.02748 0.00167 0.01130 0.00257 AFIX 137 H28A 2 0.877186 1.110095 0.245401 11.00000 -1.50000 H28B 2 0.878665 1.016504 0.192227 11.00000 -1.50000 H28C 2 0.782202 1.116885 0.192193 11.00000 -1.50000 AFIX 0 C29 1 1.020883 1.238114 0.212044 11.00000 0.03317 0.03452 = 0.03610 -0.00097 0.01094 0.01247 AFIX 137 H29A 2 1.052296 1.322864 0.199464 11.00000 -1.50000 H29B 2 1.053125 1.149052 0.203321 11.00000 -1.50000 H29C 2 1.030471 1.244453 0.251778 11.00000 -1.50000 AFIX 0 N25 3 0.863630 1.374250 0.199425 11.00000 0.02284 0.02369 = 0.02197 0.00059 0.00667 0.00282 AFIX 137 H25A 2 0.888415 1.451113 0.184198 11.00000 -1.50000 H25B 2 0.882324 1.383128 0.236586 11.00000 -1.50000 H25C 2 0.794230 1.372660 0.187250 11.00000 -1.50000 AFIX 0 MOLE 3 C31 1 0.645819 0.672492 0.162726 11.00000 0.02323 0.01915 = 0.02486 -0.00035 0.01108 0.00224 C32 1 0.610843 0.800484 0.124967 11.00000 0.02421 0.03117 = 0.03083 0.00604 0.01292 0.00241 AFIX 23 H32A 2 0.648609 0.800255 0.096349 11.00000 -1.20000 H32B 2 0.628342 0.891511 0.146314 11.00000 -1.20000 AFIX 0 C33 1 0.497239 0.799760 0.097448 11.00000 0.02401 0.03749 = 0.02504 0.00469 0.00706 0.00283 AFIX 23 H33A 2 0.481214 0.880188 0.070493 11.00000 -1.20000 H33B 2 0.479119 0.707224 0.077177 11.00000 -1.20000 AFIX 0 C34 1 0.433106 0.816276 0.137372 11.00000 0.01790 0.02230 = 0.02707 0.00387 0.00325 0.00580 O31A 4 0.739254 0.638395 0.174529 11.00000 0.01710 0.03188 = 0.03845 0.00726 0.01022 0.00574 O31B 4 0.580766 0.607156 0.181338 11.00000 0.02614 0.02367 = 0.02995 0.00537 0.01359 0.00249 O34A 4 0.346465 0.745993 0.123150 11.00000 0.01947 0.03493 = 0.03003 -0.00845 0.00835 -0.00274 AFIX 147 H34 2 0.312420 0.763497 0.145800 11.00000 -1.50000 AFIX 0 O34B 4 0.459532 0.892519 0.178590 11.00000 0.02526 0.02508 = 0.03213 -0.00677 0.00750 -0.00102 MOLE 4 C41 1 0.253433 0.135655 0.049065 11.00000 0.08240 0.03259 = 0.04499 -0.01129 -0.02424 0.01516 AFIX 137 H41A 2 0.207521 0.122410 0.072849 11.00000 -1.50000 H41B 2 0.298816 0.051223 0.052458 11.00000 -1.50000 H41C 2 0.212985 0.145221 0.010917 11.00000 -1.50000 AFIX 0 C42 1 0.317462 0.273326 0.066204 11.00000 0.05142 0.02989 = 0.02981 -0.00240 -0.00410 0.01070 C43 1 0.397470 0.253849 0.121871 11.00000 0.03128 0.02913 = 0.01935 -0.00221 0.00439 0.00508 AFIX 23 H43A 2 0.449106 0.331385 0.124149 11.00000 -1.20000 H43B 2 0.432607 0.160384 0.119869 11.00000 -1.20000 AFIX 0 C44 1 0.369039 0.254271 0.177249 11.00000 0.02061 0.02092 = 0.02398 0.00165 0.00166 -0.00123 C46 1 0.379952 0.301160 0.024156 11.00000 0.09947 0.07285 = 0.02132 0.00779 0.01209 0.02538 AFIX 137 H46A 2 0.333431 0.309510 -0.012637 11.00000 -1.50000 H46B 2 0.427187 0.219983 0.024954 11.00000 -1.50000 H46C 2 0.418884 0.391646 0.033473 11.00000 -1.50000 AFIX 0 C47 1 0.246386 0.402956 0.064414 11.00000 0.06071 0.02859 = 0.03139 -0.00058 -0.00792 0.01343 AFIX 137 H47A 2 0.203954 0.416484 0.026864 11.00000 -1.50000 H47B 2 0.287154 0.490787 0.076330 11.00000 -1.50000 H47C 2 0.202392 0.384871 0.088898 11.00000 -1.50000 AFIX 0 C48 1 0.277207 0.161471 0.179695 11.00000 0.02654 0.03047 = 0.04009 0.00249 0.00401 -0.00104 AFIX 137 H48A 2 0.287172 0.061879 0.168247 11.00000 -1.50000 H48B 2 0.215189 0.202424 0.155105 11.00000 -1.50000 H48C 2 0.270200 0.160428 0.217306 11.00000 -1.50000 AFIX 0 C49 1 0.358614 0.408251 0.198463 11.00000 0.03194 0.02779 = 0.02844 -0.00175 0.00398 0.00438 AFIX 137 H49A 2 0.356226 0.403294 0.236836 11.00000 -1.50000 H49B 2 0.295551 0.452843 0.176345 11.00000 -1.50000 H49C 2 0.417399 0.467046 0.195770 11.00000 -1.50000 AFIX 0 N45 3 0.460943 0.186733 0.216827 11.00000 0.02241 0.02281 = 0.02045 0.00088 0.00728 -0.00080 AFIX 137 H45A 2 0.452345 0.189180 0.251329 11.00000 -1.50000 H45B 2 0.518124 0.237566 0.216014 11.00000 -1.50000 H45C 2 0.467701 0.092783 0.206969 11.00000 -1.50000 AFIX 0 MOLE 5 O1W 4 0.641729 1.328296 0.209362 11.00000 0.02339 0.02909 = 0.02812 0.00209 0.00415 0.00189 H1W 2 0.681827 1.326609 0.241119 11.00000 0.03997 H2W 2 0.620963 1.415154 0.203612 11.00000 0.06423 HKLF 4 Covalent radii and connectivity table for 07skc0032p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - C1 C3 C3 - C2 C4 C4 - O4B O4A C3 O1A - C1 O1B - C1 O4A - C4 O4B - C4 C21 - C22 C22 - C21 C27 C26 C23 C23 - C24 C22 C24 - N25 C28 C29 C23 C26 - C22 C27 - C22 C28 - C24 C29 - C24 N25 - C24 C31 - O31B O31A C32 C32 - C31 C33 C33 - C34 C32 C34 - O34B O34A C33 O31A - C31 O31B - C31 O34A - C34 O34B - C34 C41 - C42 C42 - C47 C41 C46 C43 C43 - C42 C44 C44 - N45 C48 C49 C43 C46 - C42 C47 - C42 C48 - C44 C49 - C44 N45 - C44 O1W - no bonds found Operators for generating equivalent atoms: $1 x, y+1, z $2 -x+2, y+1/2, -z+1/2 $3 x-1, y, z $4 -x+1, y-1/2, -z+1/2 $5 x, y-1, z 31753 Reflections read, of which 1166 rejected -17 =< h =< 17, -11 =< k =< 11, -32 =< l =< 32, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 6913 Unique reflections, of which 0 suppressed R(int) = 0.1068 R(sigma) = 0.1221 Friedel opposites merged Maximum memory for data reduction = 4612 / 68443 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 = 5679 / 426398 wR2 = 0.1958 before cycle 1 for 6913 data and 338 / 338 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.005 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.172; Restrained GooF = 1.172 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 7.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40270 0.00081 0.015 OSF Mean shift/esd = 0.002 Maximum = 0.015 for OSF Max. shift = 0.000 A for H34 Max. dU = 0.000 for H1W Least-squares cycle 2 Maximum vector length = 511 Memory required = 5679 / 426398 wR2 = 0.1958 before cycle 2 for 6913 data and 338 / 338 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.005 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.172; Restrained GooF = 1.172 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 7.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40270 0.00081 0.001 OSF Mean shift/esd = 0.001 Maximum = 0.003 for U33 C21 Max. shift = 0.000 A for H34 Max. dU = 0.000 for H1W Least-squares cycle 3 Maximum vector length = 511 Memory required = 5679 / 426398 wR2 = 0.1958 before cycle 3 for 6913 data and 338 / 338 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.005 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.172; Restrained GooF = 1.172 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 7.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40270 0.00081 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H41C Max. dU = 0.000 for H1W Least-squares cycle 4 Maximum vector length = 511 Memory required = 5679 / 426398 wR2 = 0.1958 before cycle 4 for 6913 data and 338 / 338 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.005 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.172; Restrained GooF = 1.172 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 7.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40270 0.00081 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H46A Max. dU = 0.000 for H1W Largest correlation matrix elements 0.580 y H2W / x H2W Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.9713 0.8813 0.0842 23 0.990 0.000 C2 C1 C3 H2B 0.9653 0.7380 0.0475 23 0.990 0.000 C2 C1 C3 H3A 1.1363 0.8079 0.0826 23 0.990 0.000 C3 C2 C4 H3B 1.1181 0.6514 0.1060 23 0.990 0.000 C3 C2 C4 H1 0.8117 0.7176 0.1388 147 0.840 0.000 O1A C1 H1 H21A 0.6771 1.3840 0.0425 137 0.980 0.000 C21 C22 H21A H21B 0.7784 1.4617 0.0783 137 0.980 0.000 C21 C22 H21A H21C 0.7041 1.3786 0.1080 137 0.980 0.000 C21 C22 H21A H23A 0.9297 1.1417 0.1140 23 0.990 0.000 C23 C24 C22 H23B 0.9367 1.3137 0.1134 23 0.990 0.000 C23 C24 C22 H26A 0.7612 1.2379 -0.0091 137 0.980 0.000 C26 C22 H26A H26B 0.8572 1.1380 0.0193 137 0.980 0.000 C26 C22 H26A H26C 0.8690 1.3113 0.0197 137 0.980 0.000 C26 C22 H26A H27A 0.6933 1.1194 0.1095 137 0.980 0.000 C27 C22 H27A H27B 0.7621 1.0182 0.0819 137 0.980 0.000 C27 C22 H27A H27C 0.6672 1.1052 0.0441 137 0.980 0.000 C27 C22 H27A H28A 0.8772 1.1101 0.2454 137 0.980 0.000 C28 C24 H28A H28B 0.8787 1.0165 0.1922 137 0.980 0.000 C28 C24 H28A H28C 0.7822 1.1169 0.1922 137 0.980 0.000 C28 C24 H28A H29A 1.0523 1.3229 0.1995 137 0.980 0.000 C29 C24 H29A H29B 1.0531 1.1491 0.2033 137 0.980 0.000 C29 C24 H29A H29C 1.0305 1.2445 0.2518 137 0.980 0.000 C29 C24 H29A H25A 0.8884 1.4511 0.1842 137 0.910 0.000 N25 C24 H25A H25B 0.8823 1.3831 0.2366 137 0.910 0.000 N25 C24 H25A H25C 0.7942 1.3727 0.1872 137 0.910 0.000 N25 C24 H25A H32A 0.6486 0.8003 0.0963 23 0.990 0.000 C32 C31 C33 H32B 0.6283 0.8915 0.1463 23 0.990 0.000 C32 C31 C33 H33A 0.4812 0.8802 0.0705 23 0.990 0.000 C33 C34 C32 H33B 0.4791 0.7072 0.0772 23 0.990 0.000 C33 C34 C32 H34 0.3124 0.7635 0.1458 147 0.840 0.000 O34A C34 H34 H41A 0.2075 0.1224 0.0728 137 0.980 0.000 C41 C42 H41A H41B 0.2988 0.0512 0.0525 137 0.980 0.000 C41 C42 H41A H41C 0.2130 0.1452 0.0109 137 0.980 0.000 C41 C42 H41A H43A 0.4491 0.3314 0.1241 23 0.990 0.000 C43 C42 C44 H43B 0.4326 0.1604 0.1199 23 0.990 0.000 C43 C42 C44 H46A 0.3334 0.3095 -0.0126 137 0.980 0.000 C46 C42 H46A H46B 0.4272 0.2200 0.0250 137 0.980 0.000 C46 C42 H46A H46C 0.4189 0.3916 0.0335 137 0.980 0.000 C46 C42 H46A H47A 0.2040 0.4165 0.0269 137 0.980 0.000 C47 C42 H47A H47B 0.2872 0.4908 0.0763 137 0.980 0.000 C47 C42 H47A H47C 0.2024 0.3849 0.0889 137 0.980 0.000 C47 C42 H47A H48A 0.2872 0.0619 0.1682 137 0.980 0.000 C48 C44 H48A H48B 0.2152 0.2024 0.1551 137 0.980 0.000 C48 C44 H48A H48C 0.2702 0.1604 0.2173 137 0.980 0.000 C48 C44 H48A H49A 0.3562 0.4033 0.2368 137 0.980 0.000 C49 C44 H49A H49B 0.2956 0.4528 0.1763 137 0.980 0.000 C49 C44 H49A H49C 0.4174 0.4670 0.1958 137 0.980 0.000 C49 C44 H49A H45A 0.4523 0.1892 0.2513 137 0.910 0.000 N45 C44 H45A H45B 0.5181 0.2376 0.2160 137 0.910 0.000 N45 C44 H45A H45C 0.4677 0.0928 0.2070 137 0.910 0.000 N45 C44 H45A 07skc0032p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.92870 0.70000 0.12004 1.00000 0.01755 0.03275 0.01840 -0.00712 0.00060 -0.00349 0.02368 0.00750 0.00031 0.00047 0.00016 0.00000 0.00220 0.00251 0.00201 0.00189 0.00172 0.00179 0.00093 C2 0.98746 0.77609 0.08543 1.00000 0.02386 0.03565 0.02074 0.00044 0.00723 0.00064 0.02649 0.00807 0.00030 0.00048 0.00016 0.00000 0.00227 0.00257 0.00210 0.00190 0.00183 0.00189 0.00097 H2A 0.97132 0.88129 0.08418 1.00000 0.03179 0.00000 0.00000 H2B 0.96533 0.73799 0.04752 1.00000 0.03179 0.00000 0.00000 C3 1.10167 0.75611 0.10698 1.00000 0.02114 0.03244 0.02269 -0.00013 0.00827 0.00000 0.02495 0.00772 0.00030 0.00048 0.00016 0.00000 0.00218 0.00239 0.00209 0.00193 0.00177 0.00189 0.00091 H3A 1.13630 0.80791 0.08257 1.00000 0.02994 0.00000 0.00000 H3B 1.11815 0.65137 0.10603 1.00000 0.02994 0.00000 0.00000 C4 1.14284 0.81215 0.16505 1.00000 0.02735 0.01862 0.02043 0.00458 0.01124 -0.00324 0.02120 0.00787 0.00032 0.00042 0.00016 0.00000 0.00240 0.00210 0.00207 0.00171 0.00189 0.00175 0.00089 O1A 0.84174 0.76412 0.11903 1.00000 0.02292 0.03378 0.04469 0.01127 0.01498 0.00484 0.03265 0.00617 0.00022 0.00032 0.00013 0.00000 0.00167 0.00179 0.00196 0.00152 0.00146 0.00138 0.00074 H1 0.81173 0.71763 0.13884 1.00000 0.04897 0.00000 0.00000 O1B 0.95890 0.58906 0.14548 1.00000 0.02458 0.02330 0.03817 0.00607 0.00988 0.00318 0.02838 0.00562 0.00021 0.00031 0.00012 0.00000 0.00167 0.00163 0.00178 0.00140 0.00141 0.00127 0.00070 O4A 1.23775 0.78891 0.18722 1.00000 0.01803 0.03813 0.02624 -0.00418 0.00413 -0.00197 0.02778 0.00532 0.00021 0.00031 0.00011 0.00000 0.00156 0.00180 0.00158 0.00135 0.00130 0.00128 0.00069 O4B 1.08416 0.87553 0.18758 1.00000 0.02436 0.02861 0.02417 -0.00198 0.00993 0.00080 0.02505 0.00534 0.00021 0.00030 0.00011 0.00000 0.00162 0.00164 0.00152 0.00129 0.00131 0.00127 0.00066 C21 0.73272 1.37806 0.07624 1.00000 0.04841 0.03236 0.02426 -0.00336 -0.00336 0.00045 0.03744 0.00881 0.00037 0.00049 0.00018 0.00000 0.00321 0.00271 0.00238 0.00207 0.00222 0.00226 0.00117 H21A 0.67714 1.38404 0.04250 1.00000 0.05616 0.00000 0.00000 H21B 0.77843 1.46168 0.07831 1.00000 0.05616 0.00000 0.00000 H21C 0.70407 1.37863 0.10803 1.00000 0.05616 0.00000 0.00000 C22 0.79254 1.23802 0.07605 1.00000 0.03591 0.02215 0.02520 -0.00349 0.00852 -0.00207 0.02766 0.00810 0.00033 0.00045 0.00017 0.00000 0.00260 0.00223 0.00223 0.00187 0.00199 0.00196 0.00097 C23 0.89511 1.23169 0.12109 1.00000 0.03135 0.02014 0.02560 0.00146 0.00928 0.00367 0.02536 0.00796 0.00031 0.00045 0.00016 0.00000 0.00251 0.00218 0.00220 0.00181 0.00194 0.00181 0.00095 H23A 0.92969 1.14168 0.11403 1.00000 0.03043 0.00000 0.00000 H23B 0.93668 1.31368 0.11344 1.00000 0.03043 0.00000 0.00000 C24 0.90654 1.23495 0.18327 1.00000 0.02961 0.01786 0.02186 -0.00189 0.00986 0.00224 0.02253 0.00778 0.00031 0.00042 0.00016 0.00000 0.00235 0.00209 0.00206 0.00174 0.00184 0.00174 0.00089 C26 0.82271 1.23064 0.02157 1.00000 0.06484 0.04509 0.02387 -0.00232 0.01281 -0.00610 0.04438 0.00954 0.00041 0.00056 0.00018 0.00000 0.00364 0.00315 0.00242 0.00230 0.00245 0.00268 0.00130 H26A 0.76120 1.23787 -0.00907 1.00000 0.06657 0.00000 0.00000 H26B 0.85722 1.13803 0.01934 1.00000 0.06657 0.00000 0.00000 H26C 0.86896 1.31131 0.01973 1.00000 0.06657 0.00000 0.00000 C27 0.72249 1.10853 0.07808 1.00000 0.04780 0.03364 0.03597 0.00122 0.00315 -0.01043 0.04061 0.00895 0.00038 0.00051 0.00020 0.00000 0.00328 0.00281 0.00275 0.00228 0.00242 0.00235 0.00123 H27A 0.69331 1.11944 0.10945 1.00000 0.06092 0.00000 0.00000 H27B 0.76212 1.01817 0.08195 1.00000 0.06092 0.00000 0.00000 H27C 0.66724 1.10515 0.04414 1.00000 0.06092 0.00000 0.00000 C28 0.85671 1.10834 0.20523 1.00000 0.04847 0.02121 0.02748 0.00168 0.01130 0.00258 0.03214 0.00879 0.00037 0.00045 0.00017 0.00000 0.00310 0.00231 0.00243 0.00194 0.00223 0.00207 0.00108 H28A 0.87719 1.11009 0.24540 1.00000 0.04821 0.00000 0.00000 H28B 0.87866 1.01650 0.19223 1.00000 0.04821 0.00000 0.00000 H28C 0.78220 1.11689 0.19219 1.00000 0.04821 0.00000 0.00000 C29 1.02088 1.23812 0.21204 1.00000 0.03317 0.03452 0.03610 -0.00098 0.01094 0.01246 0.03425 0.00884 0.00033 0.00050 0.00018 0.00000 0.00263 0.00263 0.00256 0.00221 0.00216 0.00214 0.00108 H29A 1.05229 1.32287 0.19947 1.00000 0.05138 0.00000 0.00000 H29B 1.05313 1.14906 0.20332 1.00000 0.05138 0.00000 0.00000 H29C 1.03047 1.24445 0.25178 1.00000 0.05138 0.00000 0.00000 N25 0.86363 1.37425 0.19943 1.00000 0.02284 0.02370 0.02197 0.00059 0.00667 0.00282 0.02269 0.00642 0.00025 0.00034 0.00013 0.00000 0.00194 0.00186 0.00178 0.00150 0.00152 0.00147 0.00077 H25A 0.88842 1.45111 0.18420 1.00000 0.03403 0.00000 0.00000 H25B 0.88232 1.38312 0.23659 1.00000 0.03403 0.00000 0.00000 H25C 0.79423 1.37266 0.18725 1.00000 0.03403 0.00000 0.00000 C31 0.64582 0.67249 0.16273 1.00000 0.02323 0.01916 0.02485 -0.00037 0.01107 0.00223 0.02152 0.00793 0.00031 0.00042 0.00016 0.00000 0.00232 0.00213 0.00219 0.00175 0.00188 0.00172 0.00089 C32 0.61084 0.80048 0.12497 1.00000 0.02421 0.03117 0.03084 0.00604 0.01293 0.00241 0.02767 0.00855 0.00031 0.00046 0.00017 0.00000 0.00236 0.00244 0.00238 0.00198 0.00200 0.00187 0.00099 H32A 0.64861 0.80026 0.09635 1.00000 0.03320 0.00000 0.00000 H32B 0.62834 0.89151 0.14631 1.00000 0.03320 0.00000 0.00000 C33 0.49724 0.79976 0.09745 1.00000 0.02401 0.03749 0.02504 0.00469 0.00706 0.00284 0.02873 0.00847 0.00031 0.00050 0.00017 0.00000 0.00240 0.00265 0.00227 0.00198 0.00194 0.00192 0.00101 H33A 0.48121 0.88019 0.07049 1.00000 0.03448 0.00000 0.00000 H33B 0.47912 0.70722 0.07718 1.00000 0.03448 0.00000 0.00000 C34 0.43311 0.81628 0.13737 1.00000 0.01791 0.02230 0.02708 0.00388 0.00325 0.00580 0.02293 0.00816 0.00030 0.00044 0.00017 0.00000 0.00221 0.00219 0.00228 0.00189 0.00182 0.00171 0.00091 O31A 0.73925 0.63839 0.17453 1.00000 0.01710 0.03188 0.03845 0.00726 0.01022 0.00574 0.02859 0.00570 0.00021 0.00031 0.00012 0.00000 0.00158 0.00169 0.00179 0.00140 0.00138 0.00126 0.00070 O31B 0.58077 0.60716 0.18134 1.00000 0.02613 0.02367 0.02996 0.00538 0.01359 0.00249 0.02542 0.00550 0.00021 0.00029 0.00011 0.00000 0.00164 0.00156 0.00160 0.00130 0.00136 0.00125 0.00066 O34A 0.34647 0.74599 0.12315 1.00000 0.01947 0.03493 0.03004 -0.00844 0.00835 -0.00274 0.02780 0.00519 0.00021 0.00032 0.00011 0.00000 0.00156 0.00173 0.00163 0.00142 0.00129 0.00135 0.00067 H34 0.31241 0.76351 0.14580 1.00000 0.04170 0.00000 0.00000 O34B 0.45953 0.89252 0.17859 1.00000 0.02526 0.02508 0.03214 -0.00677 0.00751 -0.00103 0.02750 0.00542 0.00021 0.00030 0.00012 0.00000 0.00168 0.00160 0.00169 0.00139 0.00137 0.00127 0.00068 C41 0.25343 0.13566 0.04906 1.00000 0.08239 0.03259 0.04499 -0.01129 -0.02423 0.01516 0.06103 0.00974 0.00046 0.00055 0.00022 0.00000 0.00456 0.00302 0.00328 0.00257 0.00307 0.00286 0.00176 H41A 0.20752 0.12241 0.07285 1.00000 0.09155 0.00000 0.00000 H41B 0.29881 0.05122 0.05246 1.00000 0.09155 0.00000 0.00000 H41C 0.21298 0.14523 0.01092 1.00000 0.09155 0.00000 0.00000 C42 0.31746 0.27333 0.06621 1.00000 0.05141 0.02989 0.02982 -0.00240 -0.00409 0.01069 0.03982 0.00918 0.00039 0.00051 0.00019 0.00000 0.00322 0.00264 0.00254 0.00214 0.00232 0.00229 0.00121 C43 0.39747 0.25385 0.12187 1.00000 0.03128 0.02912 0.01937 -0.00220 0.00440 0.00508 0.02701 0.00803 0.00032 0.00048 0.00015 0.00000 0.00252 0.00237 0.00206 0.00188 0.00186 0.00196 0.00096 H43A 0.44911 0.33138 0.12415 1.00000 0.03242 0.00000 0.00000 H43B 0.43260 0.16038 0.11987 1.00000 0.03242 0.00000 0.00000 C44 0.36904 0.25427 0.17725 1.00000 0.02061 0.02092 0.02398 0.00166 0.00166 -0.00123 0.02263 0.00754 0.00030 0.00044 0.00016 0.00000 0.00215 0.00212 0.00210 0.00181 0.00175 0.00174 0.00088 C46 0.37995 0.30116 0.02416 1.00000 0.09947 0.07285 0.02132 0.00778 0.01208 0.02539 0.06526 0.01207 0.00049 0.00068 0.00020 0.00000 0.00516 0.00436 0.00263 0.00274 0.00303 0.00369 0.00186 H46A 0.33343 0.30952 -0.01264 1.00000 0.09789 0.00000 0.00000 H46B 0.42718 0.21997 0.02495 1.00000 0.09789 0.00000 0.00000 H46C 0.41889 0.39164 0.03348 1.00000 0.09789 0.00000 0.00000 C47 0.24639 0.40296 0.06441 1.00000 0.06069 0.02859 0.03140 -0.00058 -0.00793 0.01342 0.04400 0.00948 0.00040 0.00050 0.00019 0.00000 0.00364 0.00275 0.00271 0.00220 0.00249 0.00241 0.00134 H47A 0.20395 0.41648 0.02686 1.00000 0.06599 0.00000 0.00000 H47B 0.28715 0.49079 0.07633 1.00000 0.06599 0.00000 0.00000 H47C 0.20240 0.38488 0.08890 1.00000 0.06599 0.00000 0.00000 C48 0.27721 0.16147 0.17970 1.00000 0.02654 0.03048 0.04011 0.00249 0.00402 -0.00104 0.03327 0.00854 0.00033 0.00047 0.00019 0.00000 0.00257 0.00251 0.00273 0.00216 0.00215 0.00197 0.00108 H48A 0.28717 0.06188 0.16825 1.00000 0.04990 0.00000 0.00000 H48B 0.21519 0.20243 0.15511 1.00000 0.04990 0.00000 0.00000 H48C 0.27020 0.16043 0.21731 1.00000 0.04990 0.00000 0.00000 C49 0.35861 0.40825 0.19846 1.00000 0.03194 0.02780 0.02845 -0.00174 0.00399 0.00438 0.03014 0.00835 0.00034 0.00045 0.00017 0.00000 0.00264 0.00243 0.00238 0.00198 0.00204 0.00194 0.00102 H49A 0.35622 0.40329 0.23683 1.00000 0.04520 0.00000 0.00000 H49B 0.29555 0.45285 0.17634 1.00000 0.04520 0.00000 0.00000 H49C 0.41740 0.46704 0.19577 1.00000 0.04520 0.00000 0.00000 N45 0.46094 0.18673 0.21683 1.00000 0.02241 0.02280 0.02046 0.00088 0.00729 -0.00080 0.02158 0.00622 0.00024 0.00035 0.00013 0.00000 0.00191 0.00184 0.00174 0.00145 0.00150 0.00144 0.00075 H45A 0.45235 0.18918 0.25133 1.00000 0.03237 0.00000 0.00000 H45B 0.51812 0.23757 0.21601 1.00000 0.03237 0.00000 0.00000 H45C 0.46770 0.09278 0.20697 1.00000 0.03237 0.00000 0.00000 O1W 0.64173 1.32830 0.20936 1.00000 0.02339 0.02909 0.02813 0.00209 0.00415 0.00189 0.02737 0.00586 0.00024 0.00033 0.00013 0.00000 0.00175 0.00186 0.00182 0.00141 0.00147 0.00136 0.00069 H1W 0.68184 1.32661 0.24112 1.00000 0.04004 0.05918 0.00284 0.00445 0.00103 0.00000 0.01506 H2W 0.62097 1.41516 0.20361 1.00000 0.06423 0.08639 0.00364 0.00282 0.00179 0.00000 0.01920 Final Structure Factor Calculation for 07skc0032p21c in P2(1)/c Total number of l.s. parameters = 338 Maximum vector length = 511 Memory required = 5341 / 22995 wR2 = 0.1958 before cycle 5 for 6913 data and 0 / 338 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.005 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.172; Restrained GooF = 1.172 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 7.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1087 for 3706 Fo > 4sig(Fo) and 0.2073 for all 6913 data wR2 = 0.1958, GooF = S = 1.172, Restrained GooF = 1.172 for all data Occupancy sum of asymmetric unit = 35.00 for non-hydrogen and 52.00 for hydrogen atoms Principal mean square atomic displacements U 0.0357 0.0229 0.0125 C1 0.0357 0.0241 0.0197 C2 0.0324 0.0240 0.0184 C3 0.0291 0.0237 0.0108 C4 0.0522 0.0267 0.0190 O1A 0.0403 0.0244 0.0204 O1B 0.0394 0.0262 0.0177 O4A 0.0294 0.0269 0.0189 O4B 0.0588 0.0329 0.0206 C21 0.0362 0.0269 0.0199 C22 0.0326 0.0244 0.0190 C23 0.0303 0.0218 0.0155 C24 0.0669 0.0435 0.0227 C26 0.0592 0.0346 0.0280 C27 0.0488 0.0269 0.0207 C28 0.0466 0.0363 0.0199 C29 0.0261 0.0218 0.0201 N25 0.0280 0.0206 0.0159 C31 0.0381 0.0263 0.0187 C32 0.0393 0.0235 0.0234 C33 0.0295 0.0259 0.0134 C34 0.0433 0.0280 0.0144 O31A 0.0356 0.0222 0.0185 O31B 0.0413 0.0237 0.0184 O34A 0.0364 0.0251 0.0210 O34B 0.1283 0.0294 0.0253 C41 0.0679 0.0275 0.0241 C42 0.0372 0.0250 0.0189 C43 0.0290 0.0202 0.0186 C44 0.1164 0.0594 0.0200 C46 0.0815 0.0294 0.0212 C47 0.0440 0.0299 0.0259 C48 0.0385 0.0269 0.0250 C49 0.0234 0.0228 0.0185 N45 0.0310 0.0290 0.0220 O1W 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 0.019 0.026 0.034 0.044 0.056 0.074 0.109 1.000 Number in group 822. 629. 627. 720. 675. 712. 652. 691. 698. 687. GooF 1.145 1.208 1.277 1.255 1.237 1.248 1.260 1.138 0.985 0.934 K 13.490 3.075 1.930 1.346 1.106 1.069 1.058 1.017 0.999 1.001 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 699. 684. 719. 681. 688. 676. 689. 694. 691. 692. GooF 1.331 1.310 1.287 1.266 1.252 1.122 1.110 0.964 1.002 0.998 K 1.405 1.298 1.223 1.084 1.098 1.016 0.991 0.982 1.002 1.000 R1 0.434 0.409 0.383 0.352 0.267 0.209 0.145 0.109 0.087 0.040 Recommended weighting scheme: WGHT 0.0000 7.5677 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) -14 2 14 443.66 162.28 3.69 0.050 0.91 -14 1 16 642.73 294.52 3.66 0.068 0.91 -14 5 15 251.41 26.49 3.56 0.020 0.82 -12 3 27 568.08 171.04 3.48 0.052 0.78 -8 5 22 188.82 24.89 3.34 0.020 0.92 -8 9 18 571.62 213.66 3.33 0.058 0.78 -13 1 7 243.77 7.00 3.31 0.010 1.04 -11 3 23 226.80 10.60 3.28 0.013 0.88 -10 7 12 391.32 129.69 3.25 0.045 0.91 0 1 24 358.30 138.26 3.24 0.047 1.01 0 10 15 265.18 1.30 3.24 0.005 0.80 3 5 25 358.67 108.81 3.24 0.041 0.81 -13 4 24 420.50 12.39 3.22 0.014 0.78 -2 7 22 264.15 7.46 3.22 0.011 0.86 16 1 4 239.25 14.09 3.20 0.015 0.78 2 8 7 107.93 10.48 3.19 0.013 1.06 3 3 27 392.55 52.11 3.17 0.029 0.81 5 3 24 301.57 70.27 3.17 0.033 0.84 1 5 28 384.29 13.32 3.16 0.014 0.77 -14 7 9 337.83 67.12 3.15 0.032 0.78 -13 5 17 232.55 35.92 3.13 0.024 0.84 3 1 14 1.70 141.24 3.12 0.047 1.47 10 3 18 49.34 247.63 3.12 0.062 0.81 13 2 4 291.54 18.96 3.11 0.017 0.93 2 10 10 320.72 40.13 3.10 0.025 0.84 4 7 15 391.72 96.49 3.10 0.039 0.93 -7 8 14 310.56 54.00 3.08 0.029 0.91 5 2 14 83.96 359.59 3.07 0.075 1.25 2 1 0 32460.85 35345.34 3.07 0.745 5.33 2 10 12 193.07 7.90 3.06 0.011 0.82 14 4 7 243.74 22.09 3.03 0.019 0.80 2 4 15 22.48 148.39 3.02 0.048 1.25 2 7 18 342.81 38.71 3.00 0.025 0.91 10 1 8 503.11 233.33 3.00 0.060 1.09 4 10 12 201.00 2.81 2.99 0.007 0.79 -13 3 23 747.85 366.78 2.99 0.076 0.82 8 1 18 243.43 1.31 2.98 0.005 0.93 4 4 14 -26.43 56.43 2.97 0.030 1.19 -8 5 28 210.59 12.60 2.96 0.014 0.79 -11 7 11 294.45 97.78 2.95 0.039 0.88 -4 3 31 185.69 26.92 2.94 0.021 0.79 10 2 17 15.59 165.11 2.92 0.051 0.85 4 4 23 380.51 170.33 2.86 0.052 0.87 3 3 23 193.44 2.81 2.86 0.007 0.93 -4 7 24 300.94 10.06 2.82 0.013 0.82 0 1 6 59591.73 63766.08 2.82 1.000 3.72 4 1 0 151.18 39.31 2.82 0.025 3.08 11 4 1 1127.48 1567.77 2.82 0.157 1.04 10 5 11 235.05 55.57 2.82 0.030 0.89 4 0 26 192.76 1.04 2.81 0.004 0.84 Bond lengths and angles C1 - Distance Angles O1B 1.2176 (0.0048) O1A 1.3124 (0.0047) 124.19 (0.38) C2 1.5017 (0.0055) 122.79 (0.38) 113.01 (0.37) C1 - O1B O1A C2 - Distance Angles C1 1.5017 (0.0055) C3 1.5117 (0.0054) 112.55 (0.34) H2A 0.9900 109.09 109.09 H2B 0.9900 109.09 109.09 107.83 C2 - C1 C3 H2A C3 - Distance Angles C2 1.5117 (0.0054) C4 1.5169 (0.0054) 112.89 (0.33) H3A 0.9900 109.01 109.01 H3B 0.9900 109.01 109.01 107.79 C3 - C2 C4 H3A C4 - Distance Angles O4B 1.2389 (0.0045) O4A 1.2793 (0.0047) 124.80 (0.37) C3 1.5169 (0.0054) 119.15 (0.37) 116.05 (0.34) C4 - O4B O4A O1A - Distance Angles C1 1.3124 (0.0047) H1 0.8400 109.47 O1A - C1 O1B - Distance Angles C1 1.2176 (0.0048) O1B - O4A - Distance Angles C4 1.2793 (0.0047) O4A - O4B - Distance Angles C4 1.2389 (0.0045) O4B - C21 - Distance Angles C22 1.5220 (0.0060) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - C22 H21A H21B C22 - Distance Angles C21 1.5220 (0.0060) C27 1.5318 (0.0059) 108.74 (0.37) C26 1.5376 (0.0056) 107.91 (0.37) 107.99 (0.37) C23 1.5497 (0.0057) 113.92 (0.35) 113.01 (0.36) 104.93 (0.35) C22 - C21 C27 C26 C23 - Distance Angles C24 1.5387 (0.0052) C22 1.5497 (0.0057) 125.44 (0.34) H23A 0.9900 105.96 105.96 H23B 0.9900 105.96 105.96 106.26 C23 - C24 C22 H23A C24 - Distance Angles N25 1.5064 (0.0048) C28 1.5217 (0.0055) 108.12 (0.31) C29 1.5299 (0.0057) 105.68 (0.32) 109.43 (0.35) C23 1.5387 (0.0052) 110.55 (0.32) 114.99 (0.34) 107.67 (0.33) C24 - N25 C28 C29 C26 - Distance Angles C22 1.5376 (0.0056) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C22 H26A H26B C27 - Distance Angles C22 1.5318 (0.0059) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C22 H27A H27B C28 - Distance Angles C24 1.5217 (0.0055) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C24 H28A H28B C29 - Distance Angles C24 1.5299 (0.0057) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 - C24 H29A H29B N25 - Distance Angles C24 1.5064 (0.0048) H25A 0.9100 109.47 H25B 0.9100 109.47 109.47 H25C 0.9100 109.47 109.47 109.47 N25 - C24 H25A H25B C31 - Distance Angles O31B 1.2561 (0.0044) O31A 1.2623 (0.0045) 123.55 (0.37) C32 1.5106 (0.0055) 118.31 (0.35) 118.14 (0.34) C31 - O31B O31A C32 - Distance Angles C31 1.5106 (0.0055) C33 1.5144 (0.0056) 113.54 (0.35) H32A 0.9900 108.86 108.86 H32B 0.9900 108.86 108.86 107.71 C32 - C31 C33 H32A C33 - Distance Angles C34 1.5029 (0.0054) C32 1.5144 (0.0056) 112.90 (0.35) H33A 0.9900 109.01 109.01 H33B 0.9900 109.01 109.01 107.79 C33 - C34 C32 H33A C34 - Distance Angles O34B 1.2283 (0.0047) O34A 1.3056 (0.0047) 123.83 (0.37) C33 1.5029 (0.0054) 122.41 (0.38) 113.74 (0.36) C34 - O34B O34A O31A - Distance Angles C31 1.2623 (0.0046) O31A - O31B - Distance Angles C31 1.2561 (0.0044) O31B - O34A - Distance Angles C34 1.3056 (0.0047) H34 0.8400 109.47 O34A - C34 O34B - Distance Angles C34 1.2283 (0.0047) O34B - C41 - Distance Angles C42 1.5313 (0.0070) H41A 0.9800 109.47 H41B 0.9800 109.47 109.47 H41C 0.9800 109.47 109.47 109.47 C41 - C42 H41A H41B C42 - Distance Angles C47 1.5255 (0.0063) C41 1.5313 (0.0070) 109.28 (0.43) C46 1.5447 (0.0070) 107.86 (0.42) 108.35 (0.43) C43 1.5448 (0.0058) 113.86 (0.37) 111.85 (0.39) 105.37 (0.40) C42 - C47 C41 C46 C43 - Distance Angles C42 1.5448 (0.0058) C44 1.5465 (0.0053) 122.81 (0.36) H43A 0.9900 106.63 106.63 H43B 0.9900 106.63 106.63 106.57 C43 - C42 C44 H43A C44 - Distance Angles N45 1.5112 (0.0048) C48 1.5238 (0.0055) 106.47 (0.32) C49 1.5330 (0.0056) 106.46 (0.31) 110.56 (0.34) C43 1.5465 (0.0053) 103.88 (0.31) 115.85 (0.35) 112.75 (0.34) C44 - N45 C48 C49 C46 - Distance Angles C42 1.5447 (0.0070) H46A 0.9800 109.47 H46B 0.9800 109.47 109.47 H46C 0.9800 109.47 109.47 109.47 C46 - C42 H46A H46B C47 - Distance Angles C42 1.5255 (0.0063) H47A 0.9800 109.47 H47B 0.9800 109.47 109.47 H47C 0.9800 109.47 109.47 109.47 C47 - C42 H47A H47B C48 - Distance Angles C44 1.5238 (0.0055) H48A 0.9800 109.47 H48B 0.9800 109.47 109.47 H48C 0.9800 109.47 109.47 109.47 C48 - C44 H48A H48B C49 - Distance Angles C44 1.5330 (0.0056) H49A 0.9800 109.47 H49B 0.9800 109.47 109.47 H49C 0.9800 109.47 109.47 109.47 C49 - C44 H49A H49B N45 - Distance Angles C44 1.5112 (0.0048) H45A 0.9100 109.47 H45B 0.9100 109.47 109.47 H45C 0.9100 109.47 109.47 109.47 N45 - C44 H45A H45B O1W - Distance Angles H1W 0.8431 (0.0182) H2W 0.8463 (0.0185) 106.44 (2.78) O1W - H1W Selected torsion angles -30.33 ( 0.56) O1B - C1 - C2 - C3 150.75 ( 0.36) O1A - C1 - C2 - C3 -59.00 ( 0.48) C1 - C2 - C3 - C4 -4.76 ( 0.53) C2 - C3 - C4 - O4B 175.05 ( 0.34) C2 - C3 - C4 - O4A 62.49 ( 0.53) C21 - C22 - C23 - C24 -62.28 ( 0.53) C27 - C22 - C23 - C24 -179.71 ( 0.39) C26 - C22 - C23 - C24 -60.80 ( 0.50) C22 - C23 - C24 - N25 61.96 ( 0.53) C22 - C23 - C24 - C28 -175.78 ( 0.38) C22 - C23 - C24 - C29 -21.90 ( 0.54) O31B - C31 - C32 - C33 159.17 ( 0.37) O31A - C31 - C32 - C33 64.76 ( 0.48) C31 - C32 - C33 - C34 35.20 ( 0.56) C32 - C33 - C34 - O34B -146.72 ( 0.37) C32 - C33 - C34 - O34A 49.43 ( 0.60) C47 - C42 - C43 - C44 -75.07 ( 0.55) C41 - C42 - C43 - C44 167.42 ( 0.41) C46 - C42 - C43 - C44 162.95 ( 0.37) C42 - C43 - C44 - N45 46.57 ( 0.56) C42 - C43 - C44 - C48 -82.20 ( 0.49) C42 - C43 - C44 - C49 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.67 2.502(4) 172.7 O1A-H1...O31A 0.91 2.32 3.113(4) 146.2 N25-H25C...O1W 0.91 1.99 2.890(4) 168.5 N25-H25A...O1B_$1 0.846(19) 1.889(19) 2.729(4) 172(5) O1W-H2W...O31B_$1 0.91 1.85 2.756(4) 172.4 N25-H25B...O4B_$2 0.843(18) 1.885(19) 2.718(4) 170(4) O1W-H1W...O4A_$2 0.84 1.65 2.491(4) 175.1 O34A-H34...O4A_$3 0.91 2.02 2.872(4) 155.8 N45-H45A...O31B_$4 0.91 2.64 3.199(4) 120.8 N45-H45A...O34B_$4 0.91 1.92 2.825(4) 173.8 N45-H45B...O1W_$5 0.91 1.97 2.870(4) 170.8 N45-H45C...O34B_$5 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) - 0.3140 (0.0287) x + 5.7651 (0.0530) y + 19.1399 (0.1072) z = 6.7888 (0.0155) * 0.0000 (0.0000) C31 * 0.0000 (0.0000) O31A * 0.0000 (0.0000) O31B Rms deviation of fitted atoms = 0.0000 - 4.1350 (0.0816) x + 7.2895 (0.0119) y - 10.8330 (0.1491) z = 2.6712 (0.0181) Angle to previous plane (with approximate esd) = 84.60 ( 0.41 ) * 0.0000 (0.0000) C34 * 0.0000 (0.0000) O34A * 0.0000 (0.0000) O34B Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 1 34 GRID -1.613 -2 -1 1.613 2 1 R1 = 0.2071 for 6913 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.3406 0.3344 0.3392 [ 0.71 A from H32B ] Deepest hole -0.36 at 0.2223 0.3013 0.0614 [ 0.99 A from C47 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 5391 / 48944 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6594 0.8344 0.1608 1.00000 0.05 0.32 0.71 H32B 1.02 C32 1.50 C31 1.63 H32A Q2 1 0.4018 0.1986 0.0213 1.00000 0.05 0.30 0.39 H46B 1.00 C46 1.49 H46A 1.81 H46C Q3 1 0.2717 0.2266 0.0586 1.00000 0.05 0.30 0.74 C42 0.89 C41 1.40 H41A 1.46 H41C Q4 1 0.9496 0.7064 0.0856 1.00000 0.05 0.29 0.82 C2 0.99 C1 1.08 H2B 1.64 H2A Q5 1 0.3201 0.7136 0.0908 1.00000 0.05 0.29 0.85 O34A 1.49 H34 1.92 C34 2.11 H47B Q6 1 0.7420 1.1807 0.2427 1.00000 0.05 0.29 1.56 H1W 1.62 H28C 1.93 H28A 1.95 O1W Q7 1 0.8900 1.0627 0.0507 1.00000 0.05 0.28 1.06 H26B 1.71 H23A 1.85 C26 2.05 H2A Q8 1 0.8326 1.3810 0.2611 1.00000 0.05 0.28 1.03 H25B 1.48 O4B 1.72 N25 1.80 H25C Q9 1 0.9337 0.8759 0.0211 1.00000 0.05 0.27 1.44 H2B 1.54 H2A 1.84 C2 1.95 H41C Q10 1 0.3555 0.2757 0.0485 1.00000 0.05 0.27 0.77 C42 0.81 C46 1.37 H46B 1.48 H46C Shortest distances between peaks (including symmetry equivalents) 2 10 1.26 3 10 1.31 7 9 2.02 6 8 2.19 2 3 2.22 4 9 2.22 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 1.44: 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 2.97: Structure factors and derivatives 4.97: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.38: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.19: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.13: Fourier summations 0.06: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0032p21c finished at 12:20:25 Total CPU time: 10.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++