+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0067p-1 started at 15:01:15 on 21-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0067p-1 in P-1 CELL 0.71073 8.1621 9.3259 21.3026 86.922 88.863 87.350 ZERR 8.00 0.0006 0.0005 0.0012 0.004 0.003 0.004 LATT 1 SFAC C H N O UNIT 48 88 8 40 V = 1617.22 F(000) = 752.0 Mu = 0.13 mm-1 Cell Wt = 1417.26 Rho = 1.455 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB N24 O74A HTAB O31A O1B HTAB O31A O1A HTAB O34B O51A HTAB O41 O61 HTAB N64 O74B HTAB N64 O4B HTAB O4A O74B EQIV_$1 -x+2, -y, -z HTAB N24 O31A_$1 HTAB N84 O51B_$1 HTAB N84 O34B_$1 EQIV_$2 -x+2, -y+1, -z HTAB N24 O4B_$2 HTAB N64 O31B_$2 EQIV_$3 x+1, y, z HTAB O21 O81_$3 EQIV_$4 x-1, y, z HTAB N44 O71A_$4 HTAB O61 O74A_$4 EQIV_$5 x-1, y+1, z+1 HTAB N44 O51B_$5 EQIV_$6 -x+1, -y, -z HTAB N44 O34A_$6 EQIV_$7 x, y+1, z HTAB N64 O1A_$7 EQIV_$8 x, y-2, z-1 HTAB O54A O71A_$8 HTAB O54A O71B_$8 EQIV_$9 -x+2, -y-1, -z HTAB N84 O54B_$9 EQIV_$10 x, y-1, z HTAB N84 O71B_$10 HTAB O81 O71B_$10 MPLA C71 O71A O71B MPLA C74 O74A O74B FMAP 2 PLAN 10 SIZE 0.01 0.08 0.12 ACTA BOND $H WGHT 0.04820 14.13920 L.S. 4 TEMP -153.00 FVAR 0.49067 MOLE 1 C1 1 0.840966 0.078425 -0.034686 11.00000 0.01764 0.01713 = 0.01838 -0.00358 -0.00160 -0.00259 C2 1 0.843209 0.189137 0.013003 11.00000 0.01958 0.01965 = 0.01557 -0.00529 -0.00293 -0.00320 AFIX 43 H2 2 0.845627 0.158106 0.056199 11.00000 -1.20000 AFIX 0 C3 1 0.841999 0.328653 -0.001872 11.00000 0.02042 0.01891 = 0.01480 -0.00306 0.00275 -0.00525 AFIX 43 H3 2 0.839725 0.358440 -0.045211 11.00000 -1.20000 AFIX 0 C4 1 0.843929 0.441120 0.044034 11.00000 0.00995 0.01674 = 0.00985 -0.00289 0.00157 -0.00296 O1A 4 0.793655 -0.043603 -0.019864 11.00000 0.03233 0.01213 = 0.01938 0.00089 0.00288 -0.00360 O1B 4 0.891757 0.117211 -0.090514 11.00000 0.03297 0.01628 = 0.01417 -0.00353 0.00678 -0.00334 O4A 4 0.902887 0.398463 0.098700 11.00000 0.03426 0.01209 = 0.01297 -0.00282 -0.00533 0.00219 AFIX 147 H4A 2 0.889757 0.465050 0.123607 11.00000 -1.50000 AFIX 0 O4B 4 0.794009 0.566266 0.030520 11.00000 0.03487 0.01622 = 0.01746 -0.00284 -0.00331 0.00264 MOLE 2 C22 1 1.513383 0.298100 0.155308 11.00000 0.02623 0.02924 = 0.03500 0.00602 -0.00945 -0.00181 AFIX 23 H22A 2 1.634709 0.296270 0.152883 11.00000 -1.20000 H22B 2 1.474691 0.373448 0.183820 11.00000 -1.20000 AFIX 0 C23 1 1.442028 0.327279 0.090827 11.00000 0.01388 0.03609 = 0.03268 0.00763 0.00921 0.00489 AFIX 23 H23A 2 1.471773 0.423771 0.073941 11.00000 -1.20000 H23B 2 1.488098 0.255373 0.061994 11.00000 -1.20000 AFIX 0 N24 3 1.261873 0.320009 0.094351 11.00000 0.02359 0.01875 = 0.01948 -0.00216 -0.00238 0.00586 AFIX 137 H24A 2 1.234841 0.232979 0.111915 11.00000 -1.50000 H24B 2 1.220486 0.331646 0.054960 11.00000 -1.50000 H24C 2 1.219173 0.390919 0.118351 11.00000 -1.50000 AFIX 0 O21 4 1.458849 0.163192 0.177207 11.00000 0.04041 0.02224 = 0.03507 0.00882 -0.00908 -0.00342 AFIX 147 H21 2 1.511906 0.133896 0.209135 11.00000 -1.50000 AFIX 0 MOLE 3 C31 1 1.041936 -0.108265 -0.186922 11.00000 0.02672 0.01406 = 0.01054 0.00068 -0.00274 0.00166 C32 1 1.044953 -0.222488 -0.233992 11.00000 0.02249 0.01302 = 0.01600 -0.00358 0.00464 -0.00359 AFIX 43 H32 2 1.147576 -0.266929 -0.245346 11.00000 -1.20000 AFIX 0 C33 1 0.911151 -0.263847 -0.260291 11.00000 0.02081 0.01319 = 0.01242 0.00113 0.00314 -0.00123 AFIX 43 H33 2 0.807987 -0.222709 -0.247518 11.00000 -1.20000 AFIX 0 C34 1 0.915220 -0.371827 -0.308929 11.00000 0.02250 0.01716 = 0.01233 0.00323 0.00787 -0.00139 O31A 4 0.900106 -0.079786 -0.161685 11.00000 0.02366 0.01847 = 0.02043 -0.01351 0.00063 -0.00305 AFIX 147 H31A 2 0.907572 -0.013901 -0.136650 11.00000 -1.50000 AFIX 0 O31B 4 1.168888 -0.049668 -0.176354 11.00000 0.01923 0.02531 = 0.02414 -0.00686 -0.00220 -0.00369 O34A 4 0.789042 -0.413318 -0.330044 11.00000 0.02797 0.02513 = 0.02323 -0.00596 -0.00226 -0.00419 O34B 4 1.063184 -0.415884 -0.326055 11.00000 0.02991 0.01954 = 0.01938 -0.01113 0.00335 0.00252 AFIX 147 H34B 2 1.057152 -0.481046 -0.351535 11.00000 -1.50000 AFIX 0 MOLE 4 C42 1 0.530673 0.719002 0.347476 11.00000 0.02219 0.02456 = 0.03371 -0.00061 0.00190 -0.00621 AFIX 23 H42A 2 0.465564 0.795960 0.324212 11.00000 -1.20000 H42B 2 0.643006 0.751968 0.352497 11.00000 -1.20000 AFIX 0 C43 1 0.452440 0.685556 0.410915 11.00000 0.02101 0.02606 = 0.02333 -0.00312 -0.00134 -0.00242 AFIX 23 H43A 2 0.513485 0.603380 0.432344 11.00000 -1.20000 H43B 2 0.458239 0.769629 0.437121 11.00000 -1.20000 AFIX 0 N44 3 0.278252 0.649813 0.404349 11.00000 0.02116 0.01692 = 0.01564 0.00175 0.00080 -0.00028 AFIX 137 H44A 2 0.218020 0.730566 0.391956 11.00000 -1.50000 H44B 2 0.238714 0.614157 0.441971 11.00000 -1.50000 H44C 2 0.271367 0.582831 0.375097 11.00000 -1.50000 AFIX 0 O41 4 0.535837 0.591204 0.314240 11.00000 0.05399 0.02265 = 0.02763 -0.00420 0.00786 -0.00329 AFIX 147 H41 2 0.547069 0.611813 0.275570 11.00000 -1.50000 AFIX 0 MOLE 5 C51 1 1.141001 -0.577271 -0.457557 11.00000 0.01900 0.02001 = 0.01680 -0.00348 -0.00384 0.00172 C52 1 1.151079 -0.686572 -0.504570 11.00000 0.02324 0.01548 = 0.00708 -0.00461 -0.00211 0.00134 AFIX 43 H52 2 1.152634 -0.656149 -0.547850 11.00000 -1.20000 AFIX 0 C53 1 1.158149 -0.827030 -0.488956 11.00000 0.02042 0.01458 = 0.01259 -0.00273 0.00127 0.00008 AFIX 43 H53 2 1.153179 -0.856449 -0.445595 11.00000 -1.20000 AFIX 0 C54 1 1.173244 -0.939372 -0.535142 11.00000 0.01967 0.00909 = 0.01716 0.00149 0.00456 -0.00647 O51A 4 1.078378 -0.610529 -0.403766 11.00000 0.02845 0.01760 = 0.01294 -0.00463 0.00501 -0.00631 O51B 4 1.195629 -0.454046 -0.472729 11.00000 0.02880 0.01668 = 0.01660 -0.00187 -0.00059 -0.00700 O54A 4 1.118999 -0.900860 -0.590645 11.00000 0.03239 0.01592 = 0.01365 -0.00623 -0.00096 -0.00138 AFIX 147 H54A 2 1.116762 -0.973350 -0.612322 11.00000 -1.50000 AFIX 0 O54B 4 1.232747 -1.060554 -0.521248 11.00000 0.04472 0.01410 = 0.02058 -0.00057 0.00444 0.00302 MOLE 6 C62 1 0.487159 0.827413 0.170186 11.00000 0.03278 0.01815 = 0.03767 0.00325 -0.00126 0.00069 AFIX 23 H62A 2 0.550339 0.878046 0.200696 11.00000 -1.20000 H62B 2 0.371410 0.863711 0.172571 11.00000 -1.20000 AFIX 0 C63 1 0.555930 0.857773 0.103981 11.00000 0.02559 0.03601 = 0.02296 0.00282 -0.00551 -0.00522 AFIX 23 H63A 2 0.505262 0.794277 0.074814 11.00000 -1.20000 H63B 2 0.526344 0.958511 0.090126 11.00000 -1.20000 AFIX 0 N64 3 0.736133 0.834503 0.100693 11.00000 0.02305 0.01403 = 0.02496 -0.00426 0.00188 -0.00283 AFIX 137 H64A 2 0.783355 0.894281 0.126712 11.00000 -1.50000 H64B 2 0.772234 0.853274 0.060531 11.00000 -1.50000 H64C 2 0.763789 0.741622 0.112810 11.00000 -1.50000 AFIX 0 O61 4 0.496871 0.675821 0.185905 11.00000 0.02901 0.02289 = 0.03921 0.00915 0.00080 -0.00265 AFIX 147 H61 2 0.406430 0.640753 0.178962 11.00000 -1.50000 AFIX 0 MOLE 7 C71 1 0.976566 0.885336 0.317506 11.00000 0.02113 0.01161 = 0.01204 0.00324 0.00608 -0.00354 C72 1 0.958718 0.779641 0.268160 11.00000 0.01809 0.01570 = 0.01700 0.00202 0.00195 -0.00287 AFIX 43 H72 2 0.851433 0.753291 0.258451 11.00000 -1.20000 AFIX 0 C73 1 1.084021 0.721033 0.237388 11.00000 0.02150 0.01710 = 0.01685 -0.00492 -0.00062 -0.00425 AFIX 43 H73 2 1.191131 0.746117 0.247993 11.00000 -1.20000 AFIX 0 C74 1 1.068599 0.618197 0.187148 11.00000 0.01968 0.01378 = 0.01258 -0.00156 0.00020 0.00044 O71A 4 1.121100 0.898593 0.338495 11.00000 0.02070 0.01823 = 0.01480 -0.00536 0.00246 -0.00125 O71B 4 0.853396 0.957752 0.334364 11.00000 0.02600 0.01982 = 0.01781 -0.00763 0.00139 0.00416 O74A 4 1.195454 0.560212 0.164984 11.00000 0.02482 0.01933 = 0.01649 -0.00653 0.00016 0.00679 O74B 4 0.922457 0.592268 0.171784 11.00000 0.02389 0.01555 = 0.01875 -0.00533 -0.00265 -0.00261 MOLE 8 C82 1 0.505545 0.127308 0.352452 11.00000 0.01818 0.04110 = 0.03168 -0.00559 0.00483 -0.00123 AFIX 23 H82A 2 0.515120 0.039721 0.380762 11.00000 -1.20000 H82B 2 0.387384 0.150074 0.345563 11.00000 -1.20000 AFIX 0 C83 1 0.575741 0.247064 0.383427 11.00000 0.02716 0.02692 = 0.02841 0.00032 -0.00327 0.00659 AFIX 23 H83A 2 0.504245 0.272738 0.419581 11.00000 -1.200 H83B 2 0.577277 0.331874 0.353441 11.00000 -1.2000 AFIX 0 N84 3 0.745440 0.212818 0.406133 11.00000 0.03033 0.02310 = 0.01585 -0.00212 0.00020 -0.00771 AFIX 137 H84A 2 0.741935 0.148752 0.439840 11.00000 -1.50000 H84B 2 0.790442 0.294755 0.417604 11.00000 -1.50000 H84C 2 0.807503 0.174048 0.374811 11.00000 -1.50000 AFIX 0 O81 4 0.583356 0.098241 0.293622 11.00000 0.03099 0.04410 = 0.02652 0.00087 -0.00175 0.00981 AFIX 147 H81 2 0.665168 0.041559 0.299714 11.00000 -1.50000 AFIX 0 HKLF 5 Covalent radii and connectivity table for 06skc0067p-1 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C3 C1 C3 - C2 C4 C4 - O4B O4A C3 O1A - C1 O1B - C1 O4A - C4 O4B - C4 C22 - O21 C23 C23 - N24 C22 N24 - C23 O21 - C22 C31 - O31B O31A C32 C32 - C33 C31 C33 - C32 C34 C34 - O34A O34B C33 O31A - C31 O31B - C31 O34A - C34 O34B - C34 C42 - O41 C43 C43 - N44 C42 N44 - C43 O41 - C42 C51 - O51A O51B C52 C52 - C53 C51 C53 - C52 C54 C54 - O54B O54A C53 O51A - C51 O51B - C51 O54A - C54 O54B - C54 C62 - O61 C63 C63 - N64 C62 N64 - C63 O61 - C62 C71 - O71B O71A C72 C72 - C73 C71 C73 - C72 C74 C74 - O74A O74B C73 O71A - C71 O71B - C71 O74A - C74 O74B - C74 C82 - O81 C83 C83 - C82 N84 N84 - C83 O81 - C82 Operators for generating equivalent atoms: $1 -x+2, -y, -z $2 -x+2, -y+1, -z $3 x+1, y, z $4 x-1, y, z $5 x-1, y+1, z+1 $6 -x+1, -y, -z $7 x, y+1, z $8 x, y-2, z-1 $9 -x+2, -y-1, -z $10 x, y-1, z ** MERG code changed to 0 for compatibility with HKLF and BASF parameters ** 23948 Reflections read, of which 15 rejected -10 =< h =< 10, -12 =< k =< 12, -27 =< l =< 27, Max. 2-theta = 54.95 0 Systematic absence violations 0 Data suppressed, R(sigma) = 0.1135 Maximum memory for data reduction = 5085 / 1415 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 = 6370 / 577910 wR2 = 0.3413 before cycle 1 for 23933 data and 445 / 445 parameters GooF = S = 1.191; Restrained GooF = 1.191 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0482 * P )^2 + 14.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48993 0.00100 -0.746 OSF Mean shift/esd = 0.063 Maximum = -0.746 for OSF Max. shift = 0.011 A for H41 Max. dU = 0.000 for C23 Least-squares cycle 2 Maximum vector length = 511 Memory required = 6370 / 577910 wR2 = 0.3410 before cycle 2 for 23933 data and 445 / 445 parameters GooF = S = 1.191; Restrained GooF = 1.191 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0482 * P )^2 + 14.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48967 0.00099 -0.259 OSF Mean shift/esd = 0.024 Maximum = -0.259 for OSF Max. shift = 0.008 A for H41 Max. dU = 0.000 for C23 Least-squares cycle 3 Maximum vector length = 511 Memory required = 6370 / 577910 wR2 = 0.3410 before cycle 3 for 23933 data and 445 / 445 parameters GooF = S = 1.191; Restrained GooF = 1.191 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0482 * P )^2 + 14.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48965 0.00099 -0.014 OSF Mean shift/esd = 0.004 Maximum = 0.055 for tors H41 Max. shift = 0.003 A for H41 Max. dU = 0.000 for C83 Least-squares cycle 4 Maximum vector length = 511 Memory required = 6370 / 577910 wR2 = 0.3410 before cycle 4 for 23933 data and 445 / 445 parameters GooF = S = 1.191; Restrained GooF = 1.191 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0482 * P )^2 + 14.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48965 0.00099 -0.004 OSF Mean shift/esd = 0.001 Maximum = 0.023 for tors H41 Max. shift = 0.001 A for H41 Max. dU = 0.000 for C52 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 H2 0.8458 0.1582 0.0562 43 0.950 0.000 C2 C3 C1 H3 0.8398 0.3584 -0.0452 43 0.950 0.000 C3 C2 C4 H4A 0.8890 0.4647 0.1237 147 0.840 0.000 O4A C4 H4A H22A 1.6348 0.2962 0.1529 23 0.990 0.000 C22 O21 C23 H22B 1.4748 0.3734 0.1839 23 0.990 0.000 C22 O21 C23 H23A 1.4718 0.4237 0.0739 23 0.990 0.000 C23 N24 C22 H23B 1.4881 0.2553 0.0620 23 0.990 0.000 C23 N24 C22 H24A 1.2346 0.2337 0.1126 137 0.910 0.000 N24 C23 H24A H24B 1.2205 0.3299 0.0549 137 0.910 0.000 N24 C23 H24A H24C 1.2189 0.3920 0.1177 137 0.910 0.000 N24 C23 H24A H21 1.5116 0.1340 0.2092 147 0.840 0.000 O21 C22 H21 H32 1.1476 -0.2669 -0.2454 43 0.950 0.000 C32 C33 C31 H33 0.8080 -0.2228 -0.2475 43 0.950 0.000 C33 C32 C34 H31A 0.9074 -0.0136 -0.1368 147 0.840 0.000 O31A C31 H31A H34B 1.0573 -0.4806 -0.3518 147 0.840 0.000 O34B C34 H34B H42A 0.4654 0.7959 0.3241 23 0.990 0.000 C42 O41 C43 H42B 0.6429 0.7522 0.3524 23 0.990 0.000 C42 O41 C43 H43A 0.5136 0.6035 0.4323 23 0.990 0.000 C43 N44 C42 H43B 0.4583 0.7697 0.4371 23 0.990 0.000 C43 N44 C42 H44A 0.2181 0.7305 0.3918 137 0.910 0.000 N44 C43 H44A H44B 0.2387 0.6145 0.4420 137 0.910 0.000 N44 C43 H44A H44C 0.2715 0.5826 0.3752 137 0.910 0.000 N44 C43 H44A H41 0.5499 0.6114 0.2757 147 0.840 0.000 O41 C42 H41 H52 1.1526 -0.6562 -0.5479 43 0.950 0.000 C52 C53 C51 H53 1.1530 -0.8565 -0.4456 43 0.950 0.000 C53 C52 C54 H54A 1.1169 -0.9733 -0.6124 147 0.840 0.000 O54A C54 H54A H62A 0.5504 0.8779 0.2007 23 0.990 0.000 C62 O61 C63 H62B 0.3714 0.8636 0.1726 23 0.990 0.000 C62 O61 C63 H63A 0.5052 0.7942 0.0748 23 0.990 0.000 C63 N64 C62 H63B 0.5262 0.9585 0.0901 23 0.990 0.000 C63 N64 C62 H64A 0.7833 0.8945 0.1266 137 0.910 0.000 N64 C63 H64A H64B 0.7723 0.8530 0.0605 137 0.910 0.000 N64 C63 H64A H64C 0.7639 0.7417 0.1129 137 0.910 0.000 N64 C63 H64A H61 0.4067 0.6406 0.1788 147 0.840 0.000 O61 C62 H61 H72 0.8514 0.7531 0.2585 43 0.950 0.000 C72 C73 C71 H73 1.1911 0.7463 0.2479 43 0.950 0.000 C73 C72 C74 H82A 0.5149 0.0397 0.3808 23 0.990 0.000 C82 O81 C83 H82B 0.3872 0.1501 0.3456 23 0.990 0.000 C82 O81 C83 H83A 0.5043 0.2730 0.4195 23 0.990 0.000 C83 C82 N84 H83B 0.5775 0.3318 0.3534 23 0.990 0.000 C83 C82 N84 H84A 0.7419 0.1490 0.4400 137 0.910 0.000 N84 C83 H84A H84B 0.7907 0.2948 0.4175 137 0.910 0.000 N84 C83 H84A H84C 0.8075 0.1737 0.3749 137 0.910 0.000 N84 C83 H84A H81 0.6649 0.0412 0.2997 147 0.840 0.000 O81 C82 H81 06skc0067p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.84099 0.07839 -0.03466 1.00000 0.01733 0.01717 0.01821 -0.00359 -0.00187 -0.00258 0.01740 0.00826 0.00061 0.00055 0.00022 0.00000 0.00266 0.00274 0.00254 0.00218 0.00197 0.00211 0.00108 C2 0.84331 0.18916 0.01298 1.00000 0.01950 0.01963 0.01528 -0.00533 -0.00281 -0.00326 0.01787 0.00804 0.00060 0.00055 0.00023 0.00000 0.00275 0.00278 0.00240 0.00213 0.00199 0.00213 0.00109 H2 0.84581 0.15816 0.05618 1.00000 0.02145 0.00000 0.00000 C3 0.84205 0.32861 -0.00189 1.00000 0.02024 0.01887 0.01443 -0.00309 0.00263 -0.00535 0.01767 0.00825 0.00061 0.00055 0.00022 0.00000 0.00269 0.00280 0.00242 0.00210 0.00197 0.00211 0.00109 H3 0.83982 0.35837 -0.04523 1.00000 0.02120 0.00000 0.00000 C4 0.84386 0.44115 0.04401 1.00000 0.00977 0.01683 0.00965 -0.00288 0.00138 -0.00300 0.01195 0.00767 0.00055 0.00052 0.00020 0.00000 0.00237 0.00257 0.00212 0.00191 0.00174 0.00191 0.00097 O1A 0.79373 -0.04362 -0.01985 1.00000 0.03210 0.01210 0.01918 0.00089 0.00281 -0.00371 0.02115 0.00590 0.00044 0.00036 0.00015 0.00000 0.00217 0.00188 0.00178 0.00147 0.00155 0.00158 0.00081 O1B 0.89179 0.11726 -0.09055 1.00000 0.03298 0.01612 0.01385 -0.00346 0.00694 -0.00326 0.02092 0.00592 0.00045 0.00037 0.00014 0.00000 0.00216 0.00187 0.00167 0.00145 0.00152 0.00159 0.00081 O4A 0.90295 0.39844 0.09873 1.00000 0.03426 0.01194 0.01267 -0.00297 -0.00526 0.00219 0.01958 0.00580 0.00046 0.00036 0.00014 0.00000 0.00218 0.00181 0.00161 0.00141 0.00154 0.00160 0.00079 H4A 0.88898 0.46472 0.12374 1.00000 0.02936 0.00000 0.00000 O4B 0.79404 0.56634 0.03051 1.00000 0.03461 0.01599 0.01722 -0.00293 -0.00347 0.00284 0.02262 0.00596 0.00046 0.00037 0.00015 0.00000 0.00223 0.00196 0.00176 0.00153 0.00157 0.00165 0.00083 C22 1.51347 0.29808 0.15535 1.00000 0.02563 0.02919 0.03467 0.00551 -0.00926 -0.00174 0.02996 0.00956 0.00070 0.00062 0.00026 0.00000 0.00315 0.00336 0.00303 0.00262 0.00255 0.00257 0.00135 H22A 1.63480 0.29622 0.15293 1.00000 0.03595 0.00000 0.00000 H22B 1.47478 0.37344 0.18386 1.00000 0.03595 0.00000 0.00000 C23 1.44202 0.32724 0.09079 1.00000 0.01348 0.03542 0.03237 0.00793 0.00908 0.00469 0.02775 0.00995 0.00061 0.00065 0.00025 0.00000 0.00266 0.00347 0.00295 0.00262 0.00230 0.00240 0.00133 H23A 1.47181 0.42370 0.07388 1.00000 0.03329 0.00000 0.00000 H23B 1.48805 0.25528 0.06197 1.00000 0.03329 0.00000 0.00000 N24 1.26172 0.32002 0.09433 1.00000 0.02338 0.01835 0.01928 -0.00211 -0.00237 0.00567 0.02047 0.00713 0.00050 0.00046 0.00019 0.00000 0.00240 0.00236 0.00207 0.00182 0.00181 0.00188 0.00095 H24A 1.23465 0.23366 0.11259 1.00000 0.03071 0.00000 0.00000 H24B 1.22049 0.32995 0.05488 1.00000 0.03071 0.00000 0.00000 H24C 1.21891 0.39201 0.11771 1.00000 0.03071 0.00000 0.00000 O21 1.45884 0.16318 0.17722 1.00000 0.03997 0.02230 0.03479 0.00904 -0.00905 -0.00333 0.03256 0.00654 0.00048 0.00041 0.00018 0.00000 0.00245 0.00217 0.00220 0.00180 0.00186 0.00187 0.00096 H21 1.51163 0.13397 0.20923 1.00000 0.04885 0.00000 0.00000 C31 1.04198 -0.10828 -0.18687 1.00000 0.02674 0.01400 0.01020 0.00097 -0.00276 0.00188 0.01709 0.00850 0.00064 0.00053 0.00021 0.00000 0.00292 0.00265 0.00224 0.00197 0.00200 0.00218 0.00107 C32 1.04500 -0.22246 -0.23399 1.00000 0.02212 0.01264 0.01602 -0.00353 0.00491 -0.00361 0.01681 0.00827 0.00064 0.00052 0.00021 0.00000 0.00274 0.00255 0.00233 0.00202 0.00202 0.00205 0.00105 H32 1.14763 -0.26686 -0.24537 1.00000 0.02017 0.00000 0.00000 C33 0.91112 -0.26385 -0.26030 1.00000 0.02084 0.01300 0.01209 0.00117 0.00308 -0.00125 0.01541 0.00820 0.00063 0.00051 0.00020 0.00000 0.00269 0.00250 0.00224 0.00195 0.00192 0.00205 0.00102 H33 0.80796 -0.22275 -0.24750 1.00000 0.01849 0.00000 0.00000 C34 0.91514 -0.37178 -0.30900 1.00000 0.02255 0.01699 0.01212 0.00347 0.00791 -0.00129 0.01747 0.00890 0.00063 0.00054 0.00021 0.00000 0.00275 0.00268 0.00227 0.00201 0.00202 0.00219 0.00107 O31A 0.90007 -0.07979 -0.16168 1.00000 0.02363 0.01820 0.01973 -0.01318 0.00072 -0.00302 0.02003 0.00559 0.00042 0.00038 0.00015 0.00000 0.00196 0.00194 0.00182 0.00150 0.00152 0.00155 0.00078 H31A 0.90737 -0.01359 -0.13679 1.00000 0.03005 0.00000 0.00000 O31B 1.16894 -0.04966 -0.17635 1.00000 0.01890 0.02507 0.02393 -0.00689 -0.00230 -0.00369 0.02232 0.00585 0.00042 0.00039 0.00016 0.00000 0.00190 0.00209 0.00188 0.00162 0.00149 0.00160 0.00081 O34A 0.78901 -0.41330 -0.33005 1.00000 0.02779 0.02513 0.02299 -0.00591 -0.00241 -0.00422 0.02502 0.00600 0.00044 0.00040 0.00016 0.00000 0.00216 0.00216 0.00185 0.00164 0.00164 0.00172 0.00085 O34B 1.06323 -0.41586 -0.32607 1.00000 0.03006 0.01937 0.01870 -0.01097 0.00335 0.00260 0.02252 0.00587 0.00043 0.00039 0.00015 0.00000 0.00212 0.00201 0.00183 0.00152 0.00156 0.00163 0.00081 H34B 1.05727 -0.48055 -0.35178 1.00000 0.03378 0.00000 0.00000 C42 0.53064 0.71911 0.34741 1.00000 0.02210 0.02424 0.03342 -0.00059 0.00195 -0.00622 0.02649 0.00939 0.00068 0.00059 0.00025 0.00000 0.00294 0.00306 0.00295 0.00247 0.00240 0.00239 0.00124 H42A 0.46539 0.79595 0.32413 1.00000 0.03179 0.00000 0.00000 H42B 0.64294 0.75219 0.35237 1.00000 0.03179 0.00000 0.00000 C43 0.45251 0.68564 0.41091 1.00000 0.02086 0.02570 0.02275 -0.00268 -0.00117 -0.00230 0.02300 0.00885 0.00062 0.00060 0.00023 0.00000 0.00280 0.00304 0.00258 0.00232 0.00219 0.00230 0.00117 H43A 0.51361 0.60349 0.43234 1.00000 0.02760 0.00000 0.00000 H43B 0.45830 0.76973 0.43711 1.00000 0.02760 0.00000 0.00000 N44 0.27829 0.64984 0.40434 1.00000 0.02107 0.01662 0.01528 0.00199 0.00078 -0.00032 0.01779 0.00692 0.00049 0.00044 0.00018 0.00000 0.00229 0.00228 0.00196 0.00176 0.00175 0.00182 0.00092 H44A 0.21810 0.73051 0.39182 1.00000 0.02668 0.00000 0.00000 H44B 0.23866 0.61446 0.44200 1.00000 0.02668 0.00000 0.00000 H44C 0.27148 0.58263 0.37519 1.00000 0.02668 0.00000 0.00000 O41 0.53583 0.59118 0.31427 1.00000 0.05359 0.02291 0.02746 -0.00448 0.00789 -0.00369 0.03459 0.00687 0.00053 0.00041 0.00018 0.00000 0.00277 0.00221 0.00201 0.00174 0.00204 0.00200 0.00100 H41 0.54994 0.61142 0.27570 1.00000 0.05189 0.00000 0.00000 C51 1.14102 -0.57725 -0.45760 1.00000 0.01876 0.02000 0.01671 -0.00365 -0.00413 0.00188 0.01843 0.00853 0.00062 0.00056 0.00022 0.00000 0.00275 0.00282 0.00244 0.00216 0.00203 0.00218 0.00110 C52 1.15104 -0.68660 -0.50458 1.00000 0.02290 0.01539 0.00701 -0.00479 -0.00203 0.00140 0.01500 0.00787 0.00060 0.00052 0.00021 0.00000 0.00275 0.00261 0.00215 0.00192 0.00186 0.00204 0.00104 H52 1.15259 -0.65622 -0.54786 1.00000 0.01800 0.00000 0.00000 C53 1.15806 -0.82705 -0.48895 1.00000 0.02049 0.01454 0.01216 -0.00292 0.00147 0.00009 0.01570 0.00820 0.00060 0.00052 0.00022 0.00000 0.00266 0.00257 0.00226 0.00196 0.00193 0.00204 0.00103 H53 1.15297 -0.85645 -0.44558 1.00000 0.01884 0.00000 0.00000 C54 1.17327 -0.93940 -0.53511 1.00000 0.01958 0.00919 0.01673 0.00157 0.00460 -0.00655 0.01513 0.00813 0.00060 0.00051 0.00022 0.00000 0.00266 0.00245 0.00243 0.00201 0.00197 0.00199 0.00103 O51A 1.07836 -0.61056 -0.40376 1.00000 0.02860 0.01748 0.01263 -0.00456 0.00525 -0.00614 0.01935 0.00565 0.00044 0.00037 0.00014 0.00000 0.00203 0.00189 0.00160 0.00143 0.00147 0.00156 0.00078 O51B 1.19555 -0.45404 -0.47273 1.00000 0.02851 0.01659 0.01638 -0.00182 -0.00069 -0.00701 0.02027 0.00563 0.00043 0.00037 0.00015 0.00000 0.00212 0.00196 0.00173 0.00151 0.00150 0.00158 0.00080 O54A 1.11898 -0.90082 -0.59067 1.00000 0.03210 0.01573 0.01353 -0.00623 -0.00105 -0.00130 0.02025 0.00584 0.00046 0.00036 0.00014 0.00000 0.00216 0.00189 0.00168 0.00145 0.00151 0.00163 0.00080 H54A 1.11693 -0.97327 -0.61237 1.00000 0.03037 0.00000 0.00000 O54B 1.23271 -1.06062 -0.52123 1.00000 0.04439 0.01379 0.02021 -0.00051 0.00446 0.00309 0.02635 0.00634 0.00049 0.00038 0.00016 0.00000 0.00249 0.00196 0.00184 0.00154 0.00171 0.00173 0.00089 C62 0.48717 0.82729 0.17020 1.00000 0.03315 0.01780 0.03668 0.00315 -0.00115 0.00062 0.02942 0.00995 0.00072 0.00058 0.00026 0.00000 0.00333 0.00291 0.00311 0.00251 0.00260 0.00248 0.00131 H62A 0.55037 0.87792 0.20070 1.00000 0.03531 0.00000 0.00000 H62B 0.37141 0.86355 0.17261 1.00000 0.03531 0.00000 0.00000 C63 0.55588 0.85775 0.10395 1.00000 0.02517 0.03589 0.02277 0.00318 -0.00535 -0.00521 0.02793 0.00955 0.00065 0.00066 0.00024 0.00000 0.00297 0.00350 0.00267 0.00248 0.00229 0.00255 0.00129 H63A 0.50525 0.79425 0.07478 1.00000 0.03352 0.00000 0.00000 H63B 0.52625 0.95849 0.09011 1.00000 0.03352 0.00000 0.00000 N64 0.73617 0.83452 0.10069 1.00000 0.02281 0.01394 0.02453 -0.00404 0.00176 -0.00288 0.02029 0.00706 0.00050 0.00045 0.00020 0.00000 0.00239 0.00224 0.00220 0.00185 0.00188 0.00183 0.00095 H64A 0.78335 0.89451 0.12663 1.00000 0.03043 0.00000 0.00000 H64B 0.77227 0.85303 0.06051 1.00000 0.03043 0.00000 0.00000 H64C 0.76387 0.74172 0.11293 1.00000 0.03043 0.00000 0.00000 O61 0.49695 0.67578 0.18589 1.00000 0.02891 0.02270 0.03863 0.00920 0.00090 -0.00265 0.03044 0.00686 0.00046 0.00039 0.00019 0.00000 0.00216 0.00218 0.00219 0.00184 0.00186 0.00175 0.00093 H61 0.40666 0.64062 0.17878 1.00000 0.04567 0.00000 0.00000 C71 0.97649 0.88540 0.31753 1.00000 0.02125 0.01147 0.01175 0.00326 0.00612 -0.00371 0.01495 0.00832 0.00060 0.00051 0.00020 0.00000 0.00267 0.00253 0.00224 0.00193 0.00197 0.00205 0.00103 C72 0.95868 0.77957 0.26819 1.00000 0.01776 0.01574 0.01688 0.00227 0.00196 -0.00304 0.01687 0.00845 0.00062 0.00052 0.00021 0.00000 0.00263 0.00271 0.00237 0.00208 0.00200 0.00206 0.00106 H72 0.85142 0.75307 0.25854 1.00000 0.02024 0.00000 0.00000 C73 1.08404 0.72106 0.23736 1.00000 0.02122 0.01699 0.01674 -0.00475 -0.00061 -0.00413 0.01807 0.00829 0.00064 0.00052 0.00021 0.00000 0.00278 0.00269 0.00238 0.00207 0.00204 0.00215 0.00107 H73 1.19113 0.74629 0.24792 1.00000 0.02169 0.00000 0.00000 C74 1.06867 0.61814 0.18715 1.00000 0.01938 0.01376 0.01226 -0.00144 0.00017 0.00018 0.01514 0.00810 0.00060 0.00051 0.00021 0.00000 0.00263 0.00255 0.00229 0.00194 0.00194 0.00206 0.00102 O71A 1.12114 0.89856 0.33852 1.00000 0.02073 0.01816 0.01446 -0.00514 0.00228 -0.00123 0.01765 0.00559 0.00041 0.00036 0.00014 0.00000 0.00190 0.00189 0.00164 0.00144 0.00142 0.00151 0.00076 O71B 0.85334 0.95780 0.33436 1.00000 0.02565 0.01944 0.01759 -0.00750 0.00137 0.00413 0.02084 0.00576 0.00042 0.00037 0.00015 0.00000 0.00200 0.00197 0.00171 0.00151 0.00150 0.00159 0.00079 O74A 1.19546 0.56016 0.16501 1.00000 0.02469 0.01904 0.01615 -0.00643 0.00018 0.00680 0.02001 0.00581 0.00043 0.00037 0.00015 0.00000 0.00197 0.00194 0.00169 0.00149 0.00148 0.00158 0.00079 O74B 0.92241 0.59228 0.17175 1.00000 0.02391 0.01535 0.01830 -0.00523 -0.00253 -0.00270 0.01895 0.00551 0.00042 0.00036 0.00015 0.00000 0.00195 0.00185 0.00168 0.00145 0.00149 0.00152 0.00076 C82 0.50536 0.12727 0.35250 1.00000 0.01782 0.04124 0.03165 -0.00593 0.00495 -0.00120 0.03017 0.00970 0.00067 0.00068 0.00025 0.00000 0.00282 0.00364 0.00297 0.00270 0.00235 0.00258 0.00133 H82A 0.51487 0.03971 0.38083 1.00000 0.03620 0.00000 0.00000 H82B 0.38723 0.15012 0.34559 1.00000 0.03620 0.00000 0.00000 C83 0.57582 0.24709 0.38340 1.00000 0.02684 0.02793 0.02848 -0.00097 -0.00304 0.00670 0.02798 0.00966 0.00068 0.00062 0.00026 0.00000 0.00306 0.00326 0.00280 0.00250 0.00239 0.00251 0.00128 H83A 0.50435 0.27298 0.41953 1.00000 0.03358 0.00000 0.00000 H83B 0.57747 0.33179 0.35336 1.00000 0.03358 0.00000 0.00000 N84 0.74555 0.21279 0.40615 1.00000 0.03022 0.02275 0.01573 -0.00211 0.00025 -0.00761 0.02267 0.00717 0.00053 0.00048 0.00019 0.00000 0.00261 0.00247 0.00200 0.00183 0.00186 0.00201 0.00099 H84A 0.74194 0.14900 0.43995 1.00000 0.03401 0.00000 0.00000 H84B 0.79071 0.29477 0.41748 1.00000 0.03401 0.00000 0.00000 H84C 0.80753 0.17367 0.37489 1.00000 0.03401 0.00000 0.00000 O81 0.58344 0.09821 0.29362 1.00000 0.03082 0.04397 0.02650 0.00093 -0.00185 0.00958 0.03419 0.00702 0.00047 0.00047 0.00016 0.00000 0.00235 0.00275 0.00196 0.00188 0.00173 0.00197 0.00100 H81 0.66492 0.04115 0.29972 1.00000 0.05129 0.00000 0.00000 Final Structure Factor Calculation for 06skc0067p-1 in P-1 Total number of l.s. parameters = 445 Maximum vector length = 511 Memory required = 5925 / 22995 wR2 = 0.3410 before cycle 5 for 23933 data and 0 / 445 parameters GooF = S = 1.191; Restrained GooF = 1.191 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0482 * P )^2 + 14.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1472 for 15565 Fo > 4sig(Fo) and 0.2172 for all 23933 data wR2 = 0.3410, GooF = S = 1.191, Restrained GooF = 1.191 for all data Occupancy sum of asymmetric unit = 48.00 for non-hydrogen and 44.00 for hydrogen atoms Principal mean square atomic displacements U 0.0203 0.0188 0.0132 C1 0.0224 0.0206 0.0106 C2 0.0250 0.0148 0.0132 C3 0.0181 0.0096 0.0082 C4 0.0331 0.0193 0.0111 O1A 0.0358 0.0162 0.0108 O1B 0.0359 0.0131 0.0097 O4A 0.0361 0.0174 0.0143 O4B 0.0431 0.0275 0.0193 C22 0.0484 0.0252 0.0096 C23 0.0286 0.0187 0.0141 N24 0.0487 0.0324 0.0166 O21 0.0276 0.0145 0.0091 C31 0.0260 0.0135 0.0109 C32 0.0221 0.0142 0.0099 C33 0.0278 0.0182 0.0064 C34 0.0311 0.0231 0.0060 O31A 0.0299 0.0220 0.0151 O31B 0.0298 0.0277 0.0175 O34A 0.0315 0.0285 0.0075 O34B 0.0340 0.0281 0.0174 C42 0.0263 0.0228 0.0199 C43 0.0217 0.0185 0.0131 N44 0.0564 0.0264 0.0210 O41 0.0247 0.0170 0.0136 C51 0.0241 0.0160 0.0050 C52 0.0209 0.0157 0.0104 C53 0.0240 0.0164 0.0050 C54 0.0324 0.0156 0.0101 O51A 0.0307 0.0167 0.0133 O51B 0.0321 0.0199 0.0087 O54A 0.0464 0.0193 0.0133 O54B 0.0380 0.0334 0.0168 C62 0.0394 0.0256 0.0188 C63 0.0268 0.0214 0.0127 N64 0.0448 0.0292 0.0174 O61 0.0246 0.0151 0.0051 C71 0.0199 0.0191 0.0116 C72 0.0233 0.0191 0.0118 C73 0.0196 0.0140 0.0119 C74 0.0225 0.0193 0.0111 O71A 0.0290 0.0232 0.0103 O71B 0.0309 0.0194 0.0097 O74A 0.0246 0.0210 0.0112 O74B 0.0426 0.0319 0.0160 C82 0.0359 0.0287 0.0193 C83 0.0337 0.0189 0.0154 N84 0.0513 0.0281 0.0232 O81 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.017 0.024 0.032 0.040 0.050 0.063 0.079 0.111 1.000 Number in group 2505. 2556. 2133. 2679. 2126. 2352. 2475. 2308. 2447. 2352. GooF 1.340 1.358 1.311 1.309 1.283 1.141 1.060 0.925 0.911 1.156 K 11.289 2.777 1.591 1.337 1.223 1.160 1.112 1.071 1.030 1.007 Resolution(A) 0.77 0.81 0.86 0.91 0.98 1.07 1.17 1.32 1.52 1.91 inf Number in group 2414. 2431. 2332. 2412. 2394. 2395. 2396. 2367. 2398. 2394. GooF 1.366 1.353 1.317 1.243 1.165 1.101 1.065 1.072 1.005 1.161 K 1.303 1.252 1.214 1.164 1.079 1.057 1.058 1.063 1.051 0.993 R1 0.425 0.379 0.365 0.285 0.227 0.180 0.161 0.141 0.105 0.083 Recommended weighting scheme: WGHT 0.0481 14.1127 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 0 2 11655.33 23565.69 8.38 0.775 3.78 -2 1 -7 860.65 2385.03 6.63 0.247 2.34 0 -1 9 531.78 24.37 6.03 0.025 2.26 0 -1 9 502.04 24.37 5.79 0.025 2.26 3 0 6 7341.97 4865.22 4.95 0.352 2.17 -2 0 4 2299.84 3513.74 3.84 0.299 3.21 -1 0 -2 63.73 336.69 3.81 0.093 6.52 1 -3 17 -11.72 216.64 3.80 0.074 1.13 -6 1 -11 178.97 572.76 3.77 0.121 1.10 2 5 -23 375.04 10.40 3.72 0.016 0.80 4 -5 20 199.16 3.79 3.60 0.010 0.82 -1 1 -7 1445.45 2290.40 3.56 0.242 2.69 5 -1 -1 1562.31 2423.15 3.53 0.249 1.59 2 -2 6 562.60 1090.06 3.52 0.167 2.27 0 -10 -10 263.72 13.31 3.41 0.018 0.87 0 -1 15 225.77 5.29 3.40 0.012 1.39 4 -2 4 2362.03 3409.46 3.39 0.295 1.73 5 -2 18 26.15 281.33 3.36 0.085 0.93 1 3 -13 237.49 50.18 3.35 0.036 1.40 0 -3 21 217.84 1.43 3.30 0.006 0.95 1 4 -8 2014.18 1262.57 3.28 0.179 1.68 -8 -2 15 -5.38 167.22 3.26 0.065 0.81 -2 2 0 2782.03 1933.60 3.23 0.222 3.00 -1 -3 13 226.43 50.18 3.22 0.036 1.40 1 4 -2 103.27 5.19 3.18 0.011 2.19 -3 2 -23 337.84 62.07 3.18 0.040 0.85 -4 -5 0 170.92 0.73 3.17 0.004 1.41 0 -9 -13 300.84 33.77 3.16 0.029 0.90 0 2 -4 14449.17 11611.07 3.15 0.544 3.41 -5 -10 -6 311.31 12.44 3.14 0.018 0.81 -1 1 -5 13290.22 16577.77 3.12 0.650 3.44 -2 -1 1 9401.33 11855.74 3.11 0.550 3.71 -1 1 -14 158.20 11.94 3.09 0.017 1.47 0 -8 -11 206.83 8.22 3.03 0.014 1.02 -1 -3 13 214.67 50.18 3.03 0.036 1.40 -4 -2 16 134.80 390.83 3.03 0.100 1.07 -3 -9 -16 297.42 28.34 3.02 0.027 0.81 0 5 23 -41.17 133.84 3.02 0.058 0.85 -5 9 9 -46.17 115.16 3.02 0.054 0.81 -6 2 -7 411.41 135.78 3.00 0.059 1.19 -2 0 6 114.57 7.61 3.00 0.014 2.65 4 8 17 -4.05 154.21 2.99 0.063 0.82 7 1 -3 -28.82 100.50 2.98 0.051 1.14 1 3 -13 214.67 50.18 2.98 0.036 1.40 -2 5 9 150.73 9.19 2.98 0.015 1.39 1 11 6 -48.86 113.60 2.97 0.054 0.83 5 -2 7 151.57 0.47 2.96 0.003 1.36 1 4 -2 136.09 5.19 2.95 0.011 2.19 5 2 -5 -5.63 122.01 2.93 0.056 1.45 -7 0 -19 179.43 0.38 2.92 0.003 0.81 Bond lengths and angles C1 - Distance Angles O1A 1.2411 (0.0058) O1B 1.2919 (0.0056) 123.52 (0.46) C2 1.4874 (0.0067) 120.41 (0.43) 116.07 (0.44) C1 - O1A O1B C2 - Distance Angles C3 1.3215 (0.0068) C1 1.4874 (0.0067) 123.17 (0.44) H2 0.9500 118.42 118.42 C2 - C3 C1 C3 - Distance Angles C2 1.3215 (0.0068) C4 1.4732 (0.0066) 124.60 (0.44) H3 0.9500 117.70 117.70 C3 - C2 C4 C4 - Distance Angles O4B 1.2393 (0.0057) O4A 1.3056 (0.0052) 123.63 (0.44) C3 1.4732 (0.0066) 121.58 (0.41) 114.79 (0.42) C4 - O4B O4A O1A - Distance Angles C1 1.2411 (0.0058) O1A - O1B - Distance Angles C1 1.2919 (0.0056) O1B - O4A - Distance Angles C4 1.3056 (0.0052) H4A 0.8400 109.47 O4A - C4 O4B - Distance Angles C4 1.2393 (0.0057) O4B - C22 - Distance Angles O21 1.4069 (0.0063) C23 1.5108 (0.0072) 106.06 (0.46) H22A 0.9900 110.52 110.52 H22B 0.9900 110.52 110.52 108.69 C22 - O21 C23 H22A C23 - Distance Angles N24 1.4765 (0.0063) C22 1.5108 (0.0072) 110.05 (0.42) H23A 0.9900 109.65 109.65 H23B 0.9900 109.65 109.65 108.16 C23 - N24 C22 H23A N24 - Distance Angles C23 1.4765 (0.0063) H24A 0.9100 109.47 H24B 0.9100 109.47 109.47 H24C 0.9100 109.47 109.47 109.47 N24 - C23 H24A H24B O21 - Distance Angles C22 1.4069 (0.0063) H21 0.8400 109.47 O21 - C22 C31 - Distance Angles O31B 1.2238 (0.0059) O31A 1.2892 (0.0058) 125.96 (0.46) C32 1.5013 (0.0068) 119.14 (0.46) 114.88 (0.44) C31 - O31B O31A C32 - Distance Angles C33 1.3205 (0.0069) C31 1.5013 (0.0068) 122.82 (0.48) H32 0.9500 118.59 118.59 C32 - C33 C31 C33 - Distance Angles C32 1.3205 (0.0069) C34 1.4825 (0.0068) 122.72 (0.47) H33 0.9500 118.64 118.64 C33 - C32 C34 C34 - Distance Angles O34A 1.2185 (0.0059) O34B 1.3096 (0.0057) 124.77 (0.47) C33 1.4825 (0.0068) 121.18 (0.46) 114.05 (0.45) C34 - O34A O34B O31A - Distance Angles C31 1.2892 (0.0058) H31A 0.8400 109.47 O31A - C31 O31B - Distance Angles C31 1.2238 (0.0059) O31B - O34A - Distance Angles C34 1.2185 (0.0059) O34A - O34B - Distance Angles C34 1.3096 (0.0057) H34B 0.8400 109.47 O34B - C34 C42 - Distance Angles O41 1.4170 (0.0064) C43 1.5077 (0.0070) 107.42 (0.44) H42A 0.9900 110.23 110.23 H42B 0.9900 110.23 110.23 108.51 C42 - O41 C43 H42A C43 - Distance Angles N44 1.4866 (0.0062) C42 1.5077 (0.0070) 110.74 (0.42) H43A 0.9900 109.50 109.50 H43B 0.9900 109.50 109.50 108.07 C43 - N44 C42 H43A N44 - Distance Angles C43 1.4866 (0.0063) H44A 0.9100 109.47 H44B 0.9100 109.47 109.47 H44C 0.9100 109.47 109.47 109.47 N44 - C43 H44A H44B O41 - Distance Angles C42 1.4170 (0.0064) H41 0.8400 109.47 O41 - C42 C51 - Distance Angles O51A 1.2754 (0.0057) O51B 1.2744 (0.0060) 123.55 (0.46) C52 1.4651 (0.0067) 118.23 (0.46) 118.22 (0.42) C51 - O51A O51B C52 - Distance Angles C53 1.3330 (0.0066) C51 1.4651 (0.0067) 122.57 (0.42) H52 0.9500 118.72 118.72 C52 - C53 C51 C53 - Distance Angles C52 1.3330 (0.0066) C54 1.4744 (0.0067) 123.75 (0.43) H53 0.9500 118.12 118.12 C53 - C52 C54 C54 - Distance Angles O54B 1.2329 (0.0057) O54A 1.2988 (0.0054) 123.21 (0.46) C53 1.4744 (0.0067) 121.81 (0.42) 114.98 (0.41) C54 - O54B O54A O51A - Distance Angles C51 1.2754 (0.0057) O51A - O51B - Distance Angles C51 1.2744 (0.0060) O51B - O54A - Distance Angles C54 1.2988 (0.0054) H54A 0.8400 109.47 O54A - C54 O54B - Distance Angles C54 1.2329 (0.0057) O54B - C62 - Distance Angles O61 1.4333 (0.0061) C63 1.5255 (0.0074) 110.07 (0.47) H62A 0.9900 109.65 109.65 H62B 0.9900 109.65 109.65 108.16 C62 - O61 C63 H62A C63 - Distance Angles N64 1.4782 (0.0064) C62 1.5255 (0.0073) 112.11 (0.42) H63A 0.9900 109.19 109.19 H63B 0.9900 109.19 109.19 107.89 C63 - N64 C62 H63A N64 - Distance Angles C63 1.4782 (0.0064) H64A 0.9100 109.47 H64B 0.9100 109.47 109.47 H64C 0.9100 109.47 109.47 109.47 N64 - C63 H64A H64B O61 - Distance Angles C62 1.4333 (0.0061) H61 0.8400 109.47 O61 - C62 C71 - Distance Angles O71B 1.2424 (0.0054) O71A 1.2843 (0.0056) 124.09 (0.45) C72 1.4935 (0.0068) 118.77 (0.44) 117.11 (0.43) C71 - O71B O71A C72 - Distance Angles C73 1.3177 (0.0067) C71 1.4935 (0.0068) 123.39 (0.47) H72 0.9500 118.30 118.30 C72 - C73 C71 C73 - Distance Angles C72 1.3177 (0.0067) C74 1.4859 (0.0065) 124.21 (0.48) H73 0.9500 117.90 117.90 C73 - C72 C74 C74 - Distance Angles O74A 1.2418 (0.0055) O74B 1.2813 (0.0056) 124.97 (0.45) C73 1.4859 (0.0065) 118.68 (0.44) 116.30 (0.42) C74 - O74A O74B O71A - Distance Angles C71 1.2843 (0.0056) O71A - O71B - Distance Angles C71 1.2424 (0.0055) O71B - O74A - Distance Angles C74 1.2418 (0.0055) O74A - O74B - Distance Angles C74 1.2813 (0.0056) O74B - C82 - Distance Angles O81 1.4288 (0.0061) C83 1.4718 (0.0078) 113.16 (0.47) H82A 0.9900 108.95 108.95 H82B 0.9900 108.95 108.95 107.76 C82 - O81 C83 H82A C83 - Distance Angles C82 1.4718 (0.0078) N84 1.4918 (0.0066) 113.14 (0.46) H83A 0.9900 108.95 108.95 H83B 0.9900 108.95 108.95 107.76 C83 - C82 N84 H83A N84 - Distance Angles C83 1.4918 (0.0066) H84A 0.9100 109.47 H84B 0.9100 109.47 109.47 H84C 0.9100 109.47 109.47 109.47 N84 - C83 H84A H84B O81 - Distance Angles C82 1.4288 (0.0061) H81 0.8400 109.47 O81 - C82 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.91 2.791(5) 162.8 N24-H24C...O74A 0.84 1.61 2.441(5) 171.3 O31A-H31A...O1B 0.84 2.65 3.158(5) 120.7 O31A-H31A...O1A 0.84 1.69 2.519(5) 170.8 O34B-H34B...O51A 0.84 2.02 2.825(6) 159.5 O41-H41...O61 0.91 2.21 3.019(5) 147.2 N64-H64C...O74B 0.91 2.46 2.996(5) 117.6 N64-H64C...O4B 0.84 1.65 2.460(5) 162.7 O4A-H4A...O74B 0.91 2.07 2.945(5) 159.9 N24-H24A...O31A_$1 0.91 1.95 2.788(6) 151.9 N84-H84B...O51B_$1 0.91 2.51 2.959(6) 111.1 N84-H84B...O34B_$1 0.91 2.02 2.847(5) 150.9 N24-H24B...O4B_$2 0.91 1.90 2.786(6) 165.0 N64-H64A...O31B_$2 0.84 1.91 2.726(5) 163.8 O21-H21...O81_$3 0.91 2.03 2.905(5) 162.2 N44-H44A...O71A_$4 0.84 1.95 2.785(5) 178.2 O61-H61...O74A_$4 0.91 1.92 2.823(5) 169.2 N44-H44B...O51B_$5 0.91 1.98 2.863(6) 163.3 N44-H44C...O34A_$6 0.91 1.93 2.792(5) 157.8 N64-H64B...O1A_$7 0.84 1.63 2.465(5) 173.1 O54A-H54A...O71A_$8 0.84 2.58 3.101(5) 121.8 O54A-H54A...O71B_$8 0.91 1.89 2.770(5) 162.8 N84-H84A...O54B_$9 0.91 2.25 2.985(6) 138.1 N84-H84C...O71B_$10 0.84 1.84 2.647(5) 160.6 O81-H81...O71B_$10 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 1.5888 (0.0187) x + 6.1443 (0.0556) y - 14.7989 (0.1247) z = 2.2926 (0.1024) * 0.0000 (0.0000) C71 * 0.0000 (0.0000) O71A * 0.0000 (0.0000) O71B Rms deviation of fitted atoms = 0.0000 0.3974 (0.0201) x + 6.4386 (0.0576) y - 14.5863 (0.1334) z = 1.6749 (0.0699) Angle to previous plane (with approximate esd) = 8.68 ( 1.14 ) * 0.0000 (0.0000) C74 * 0.0000 (0.0000) O74A * 0.0000 (0.0000) O74B Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 1 37 GRID -2.941 -2 -1 2.941 2 1 R1 = 0.2114 for 6777 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.84 at 0.9468 0.4411 0.3317 [ 0.29 A from O34B ] Deepest hole -0.63 at 0.3270 0.2458 0.3726 [ 1.17 A from H82B ] Mean = 0.00, Rms deviation from mean = 0.15 e/A^3, Highest memory used = 5807 / 47405 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.1717 -0.4208 -0.3113 1.00000 0.05 0.61 0.94 O34B 1.44 H34B 2.06 H32 2.12 C34 Q2 1 0.7075 0.6371 0.4091 1.00000 0.05 0.61 1.65 H42B 1.68 C51 1.69 H43A 1.76 O51A Q3 1 0.8827 -0.2996 -0.3033 1.00000 0.05 0.60 0.73 C34 1.03 C33 1.48 O34A 1.52 H33 Q4 1 0.5840 0.7512 0.2056 1.00000 0.05 0.59 1.12 O61 1.20 H62A 1.27 C62 1.93 H61 Q5 1 1.5230 0.4979 0.1574 1.00000 0.05 0.59 1.34 H22B 1.68 H61 1.80 O61 1.87 C22 Q6 1 1.7626 0.2816 0.1604 1.00000 0.05 0.59 1.06 H22A 1.96 H32 2.03 O4A 2.04 C22 Q7 1 1.0661 -0.1323 -0.1199 1.00000 0.05 0.58 1.45 C31 1.55 H2 1.63 O31B 1.68 O31A Q8 1 0.5634 0.7639 0.0717 1.00000 0.05 0.57 0.55 H63A 1.14 C63 1.72 N64 1.87 H64C Q9 1 1.0828 -0.9201 -0.4404 1.00000 0.05 0.56 0.85 H53 1.46 C53 2.15 C54 2.21 H54A Q10 1 1.2640 -0.5871 -0.4736 1.00000 0.05 0.56 1.06 C51 1.34 O51B 1.52 C52 1.99 H52 Shortest distances between peaks (including symmetry equivalents) 2 10 1.45 6 7 2.13 1 3 2.57 4 5 2.70 5 6 2.74 4 8 2.86 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.44: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 11.94: Structure factors and derivatives 29.59: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.70: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.78: Analysis of variance 0.14: Merge reflections for Fourier and .fcf 0.14: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0067p-1 finished at 15:02:00 Total CPU time: 45.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++