+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0002p-1 started at 16:01:12 on 06-May-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0002p-1 in P-1 CELL 0.71073 8.7148 11.4826 16.9691 81.721 81.814 77.987 ZERR 2.00 0.0003 0.0003 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H N O UNIT 60 100 8 24 V = 1632.45 F(000) = 708.0 Mu = 0.10 mm-1 Cell Wt = 1317.48 Rho = 1.340 MERG 2 OMIT -3.00 55.00 OMIT 0 2 4 OMIT 2 0 0 SHEL 7 0.77 HTAB N23 O8B HTAB N43 O31A EQIV_$1 -x+1, -y-1, -z+1 HTAB O1B O31B_$1 EQIV_$2 x+1, y, z HTAB N21 O8A_$2 EQIV_$3 -x+1, -y+1, -z HTAB O38B O8A_$3 EQIV_$4 x-1, y, z HTAB N41 O31B_$4 EQIV_$5 x, y+1, z HTAB O51A O58A_$5 EQIV_$6 x, y-1, z HTAB O58B O51B_$6 FMAP 2 CONF PLAN 5 SIZE 0.08 0.10 0.10 ACTA BOND $H WGHT 0.06040 0.53670 L.S. 4 TEMP -153.00 FVAR 0.50698 MOLE 1 C1 1 0.022180 -0.082317 0.422128 11.00000 0.01955 0.01490 = 0.01817 -0.00107 -0.00475 -0.00382 C2 1 0.107348 0.000589 0.362867 11.00000 0.01794 0.01770 = 0.01977 0.00260 -0.00178 -0.00393 AFIX 23 H2A 2 0.159422 -0.043152 0.317038 11.00000 -1.20000 H2B 2 0.191381 0.021001 0.388915 11.00000 -1.20000 AFIX 0 C3 1 0.004535 0.116312 0.330639 11.00000 0.01924 0.01797 = 0.02084 0.00318 -0.00224 -0.00443 AFIX 23 H3A 2 -0.040611 0.164612 0.375226 11.00000 -1.20000 H3B 2 -0.084041 0.097440 0.307354 11.00000 -1.20000 AFIX 0 C4 1 0.099551 0.189352 0.266449 11.00000 0.01929 0.01861 = 0.02248 0.00364 -0.00099 -0.00414 AFIX 23 H4A 2 0.182171 0.213871 0.291276 11.00000 -1.20000 H4B 2 0.153116 0.137845 0.224743 11.00000 -1.20000 AFIX 0 C5 1 -0.001838 0.300881 0.226851 11.00000 0.01895 0.01756 = 0.02034 0.00217 -0.00223 -0.00452 AFIX 23 H5A 2 -0.059311 0.350411 0.268904 11.00000 -1.20000 H5B 2 -0.081326 0.275991 0.199942 11.00000 -1.20000 AFIX 0 C6 1 0.092998 0.377291 0.165451 11.00000 0.01916 0.01703 = 0.02104 0.00196 -0.00122 -0.00397 AFIX 23 H6A 2 0.171137 0.403959 0.192286 11.00000 -1.20000 H6B 2 0.151620 0.327977 0.123516 11.00000 -1.20000 AFIX 0 C7 1 -0.012668 0.486599 0.126357 11.00000 0.01683 0.01590 = 0.01873 0.00020 -0.00173 -0.00371 AFIX 23 H7A 2 -0.083811 0.458337 0.095901 11.00000 -1.20000 H7B 2 -0.079656 0.529635 0.169366 11.00000 -1.20000 AFIX 0 C8 1 0.070582 0.575577 0.070156 11.00000 0.01829 0.01260 = 0.01708 -0.00025 -0.00298 -0.00324 O1A 4 -0.115707 -0.058847 0.448998 11.00000 0.01781 0.02165 = 0.02903 0.00284 0.00004 -0.00333 O1B 4 0.117278 -0.186108 0.441069 11.00000 0.01804 0.01644 = 0.02870 0.00637 -0.00003 -0.00368 AFIX 147 H1 2 0.065457 -0.232418 0.471323 11.00000 0.04748 AFIX 0 O8A 4 -0.018862 0.667074 0.037652 11.00000 0.01806 0.01791 = 0.02847 0.00676 -0.00271 -0.00339 O8B 4 0.217938 0.558527 0.058399 11.00000 0.01605 0.01803 = 0.03009 0.00172 -0.00257 -0.00401 MOLE 2 C22 1 0.574696 0.659498 0.031998 11.00000 0.01995 0.02136 = 0.02125 -0.00032 -0.00161 -0.00477 AFIX 43 H22 2 0.613033 0.577657 0.024509 11.00000 -1.20000 AFIX 0 C24 1 0.415288 0.831597 0.049640 11.00000 0.02108 0.01967 = 0.02320 -0.00234 -0.00117 -0.00167 AFIX 43 H24 2 0.321848 0.890605 0.056708 11.00000 -1.20000 AFIX 0 C25 1 0.565794 0.847600 0.046500 11.00000 0.02366 0.02091 = 0.02559 -0.00249 -0.00216 -0.00700 AFIX 43 H25 2 0.598007 0.920251 0.050999 11.00000 -1.20000 AFIX 0 N21 3 0.662965 0.739337 0.035612 11.00000 0.01492 0.02571 = 0.02354 -0.00138 -0.00140 -0.00436 AFIX 43 H21 2 0.766800 0.725160 0.031670 11.00000 0.03076 AFIX 0 N23 3 0.424298 0.712862 0.040567 11.00000 0.01705 0.02062 = 0.02179 0.00102 -0.00259 -0.00543 AFIX 43 H23 2 0.343262 0.678215 0.040486 11.00000 0.04899 AFIX 0 MOLE 3 C31 1 0.941416 -0.574520 0.429492 11.00000 0.01739 0.01342 = 0.01815 -0.00081 -0.00210 -0.00379 C32 1 1.028575 -0.488513 0.372771 11.00000 0.01585 0.01717 = 0.01908 0.00031 -0.00055 -0.00592 AFIX 23 H32A 2 1.101640 -0.461589 0.402786 11.00000 -1.20000 H32B 2 1.093481 -0.532787 0.329784 11.00000 -1.20000 AFIX 0 C33 1 0.924237 -0.378432 0.334057 11.00000 0.01828 0.01608 = 0.02247 0.00248 -0.00202 -0.00441 AFIX 23 H33A 2 0.866763 -0.329249 0.376294 11.00000 -1.20000 H33B 2 0.844955 -0.404349 0.307590 11.00000 -1.20000 AFIX 0 C34 1 1.017805 -0.301473 0.272220 11.00000 0.01841 0.01642 = 0.02041 0.00224 -0.00170 -0.00421 AFIX 23 H34A 2 1.099448 -0.277817 0.298274 11.00000 -1.20000 H34B 2 1.072449 -0.349887 0.229054 11.00000 -1.20000 AFIX 0 C35 1 0.913955 -0.188904 0.235306 11.00000 0.01885 0.01860 = 0.02270 0.00334 -0.00121 -0.00414 AFIX 23 H35A 2 0.862945 -0.139117 0.278355 11.00000 -1.20000 H35B 2 0.829329 -0.212713 0.211625 11.00000 -1.20000 AFIX 0 C36 1 1.003601 -0.113175 0.170638 11.00000 0.01968 0.01631 = 0.02070 0.00111 -0.00011 -0.00444 AFIX 23 H36A 2 1.091355 -0.091809 0.193197 11.00000 -1.20000 H36B 2 1.049676 -0.160744 0.125792 11.00000 -1.20000 AFIX 0 C37 1 0.895754 0.000728 0.139124 11.00000 0.01846 0.01926 = 0.02353 0.00161 -0.00179 -0.00474 AFIX 23 H37A 2 0.811387 -0.021942 0.114569 11.00000 -1.20000 H37B 2 0.844554 0.044482 0.185081 11.00000 -1.20000 AFIX 0 C38 1 0.975977 0.084344 0.078437 11.00000 0.01922 0.01479 = 0.01743 -0.00084 -0.00353 -0.00404 O31A 4 0.794369 -0.556426 0.437873 11.00000 0.01501 0.01902 = 0.03048 0.00328 -0.00276 -0.00437 O31B 4 1.027220 -0.664446 0.465848 11.00000 0.01775 0.01720 = 0.02801 0.00628 -0.00409 -0.00380 O38A 4 1.114231 0.063088 0.051005 11.00000 0.01854 0.02042 = 0.02917 0.00451 0.00081 -0.00284 O38B 4 0.878156 0.185956 0.058424 11.00000 0.01890 0.01698 = 0.02774 0.00625 0.00019 -0.00267 AFIX 147 H38 2 0.927114 0.231117 0.025380 11.00000 0.05792 AFIX 0 MOLE 4 C42 1 0.433872 -0.646307 0.467526 11.00000 0.01961 0.01905 = 0.02319 -0.00229 -0.00091 -0.00289 AFIX 43 H42 2 0.399856 -0.562594 0.469874 11.00000 -1.20000 AFIX 0 C44 1 0.585355 -0.823713 0.458870 11.00000 0.01987 0.01798 = 0.02306 -0.00246 -0.00194 -0.00285 AFIX 43 H44 2 0.676226 -0.885603 0.454217 11.00000 -1.20000 AFIX 0 C45 1 0.432831 -0.835962 0.464884 11.00000 0.02146 0.01951 = 0.02471 -0.00226 -0.00129 -0.00599 AFIX 43 H45 2 0.396363 -0.908471 0.465222 11.00000 -1.20000 AFIX 0 N41 3 0.340655 -0.724350 0.470398 11.00000 0.01391 0.02369 = 0.02241 -0.00113 -0.00112 -0.00499 AFIX 43 H41 2 0.236770 -0.707543 0.475069 11.00000 0.03912 AFIX 0 N43 3 0.582842 -0.704115 0.460822 11.00000 0.01546 0.02018 = 0.02324 0.00058 -0.00217 -0.00536 AFIX 43 H43 2 0.666384 -0.671240 0.458075 11.00000 0.03617 AFIX 0 MOLE 5 C51 1 0.508953 -0.071415 0.285704 11.00000 0.01781 0.01882 = 0.02495 -0.00590 -0.00107 -0.00281 C52 1 0.497060 -0.195189 0.325813 11.00000 0.01998 0.01822 = 0.02116 -0.00156 -0.00132 -0.00301 AFIX 23 H52A 2 0.407029 -0.188772 0.368732 11.00000 -1.20000 H52B 2 0.594247 -0.229443 0.351557 11.00000 -1.20000 AFIX 0 C53 1 0.474986 -0.281421 0.270110 11.00000 0.02417 0.01656 = 0.02417 -0.00092 -0.00182 -0.00574 AFIX 23 H53A 2 0.568546 -0.293785 0.229486 11.00000 -1.20000 H53B 2 0.381447 -0.246091 0.241663 11.00000 -1.20000 AFIX 0 C54 1 0.452800 -0.401983 0.316524 11.00000 0.02066 0.01861 = 0.02359 -0.00115 -0.00062 -0.00743 AFIX 23 H54A 2 0.359279 -0.388712 0.357092 11.00000 -1.20000 H54B 2 0.546082 -0.436025 0.345418 11.00000 -1.20000 AFIX 0 C55 1 0.430939 -0.492944 0.263716 11.00000 0.01748 0.01898 = 0.02472 -0.00115 -0.00117 -0.00545 AFIX 23 H55A 2 0.392198 -0.560440 0.298267 11.00000 -1.20000 H55B 2 0.349366 -0.454376 0.228141 11.00000 -1.20000 AFIX 0 C56 1 0.582062 -0.541907 0.212630 11.00000 0.01795 0.01784 = 0.02913 0.00048 -0.00243 -0.00502 AFIX 23 H56B 2 0.660762 -0.586151 0.248329 11.00000 -1.20000 H56A 2 0.625493 -0.473909 0.181431 11.00000 -1.20000 AFIX 0 C57 1 0.558333 -0.625240 0.154842 11.00000 0.02172 0.01855 = 0.02467 -0.00065 0.00157 -0.00631 AFIX 23 H57A 2 0.464032 -0.587408 0.127567 11.00000 -1.20000 H57B 2 0.650680 -0.633907 0.113286 11.00000 -1.20000 AFIX 0 C58 1 0.537679 -0.748013 0.193909 11.00000 0.01862 0.02002 = 0.02452 -0.00492 0.00034 -0.00270 O51A 4 0.552095 -0.005708 0.333239 11.00000 0.04352 0.01964 = 0.02740 -0.00185 -0.00939 -0.01117 AFIX 147 H51 2 0.554956 0.063147 0.309094 11.00000 0.08801 AFIX 0 O51B 4 0.478920 -0.033844 0.217434 11.00000 0.03770 0.02043 = 0.02553 -0.00085 -0.00654 -0.00957 O58B 4 0.483373 -0.809329 0.147672 11.00000 0.03278 0.01790 = 0.02651 -0.00053 -0.00565 -0.00878 AFIX 147 H58B 2 0.485419 -0.879833 0.169859 11.00000 -1.50000 AFIX 0 O58A 4 0.571741 -0.788096 0.261211 11.00000 0.05204 0.02079 = 0.02778 0.00089 -0.01249 -0.01252 HKLF 4 Covalent radii and connectivity table for 06skc0002p-1 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C1 C3 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C7 C5 C7 - C8 C6 C8 - O8B O8A C7 O1A - C1 O1B - C1 O8A - C8 O8B - C8 C22 - N23 N21 C24 - C25 N23 C25 - C24 N21 N21 - C22 C25 N23 - C22 C24 C31 - O31A O31B C32 C32 - C33 C31 C33 - C32 C34 C34 - C35 C33 C35 - C34 C36 C36 - C37 C35 C37 - C38 C36 C38 - O38A O38B C37 O31A - C31 O31B - C31 O38A - C38 O38B - C38 C42 - N41 N43 C44 - C45 N43 C45 - C44 N41 N41 - C42 C45 N43 - C42 C44 C51 - O51B O51A C52 C52 - C51 C53 C53 - C52 C54 C54 - C53 C55 C55 - C56 C54 C56 - C55 C57 C57 - C58 C56 C58 - O58A O58B C57 O51A - C51 O51B - C51 O58B - C58 O58A - C58 Operators for generating equivalent atoms: $1 -x+1, -y-1, -z+1 $2 x+1, y, z $3 -x+1, -y+1, -z $4 x-1, y, z $5 x, y+1, z $6 x, y-1, z 34105 Reflections read, of which 38 rejected -11 =< h =< 11, -14 =< k =< 14, -21 =< l =< 22, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 5 -4 13 -0.08 0.25 3 1.57 1 Inconsistent equivalents 7472 Unique reflections, of which 0 suppressed R(int) = 0.0664 R(sigma) = 0.0619 Friedel opposites merged Maximum memory for data reduction = 4966 / 74832 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 = 6238 / 550170 wR2 = 0.1430 before cycle 1 for 7472 data and 426 / 426 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0604 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50699 0.00090 0.010 OSF Mean shift/esd = 0.007 Maximum = 0.023 for U11 C51 Max. shift = 0.000 A for H38 Max. dU = 0.000 for H21 Least-squares cycle 2 Maximum vector length = 511 Memory required = 6238 / 550170 wR2 = 0.1430 before cycle 2 for 7472 data and 426 / 426 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0604 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50700 0.00090 0.017 OSF Mean shift/esd = 0.002 Maximum = 0.017 for OSF Max. shift = 0.000 A for H38 Max. dU = 0.000 for H51 Least-squares cycle 3 Maximum vector length = 511 Memory required = 6238 / 550170 wR2 = 0.1430 before cycle 3 for 7472 data and 426 / 426 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0604 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50700 0.00090 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U11 H51 Max. shift = 0.000 A for H58B Max. dU = 0.000 for H51 Least-squares cycle 4 Maximum vector length = 511 Memory required = 6238 / 550170 wR2 = 0.1430 before cycle 4 for 7472 data and 426 / 426 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0604 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50700 0.00090 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O38A Max. shift = 0.000 A for H51 Max. dU = 0.000 for H51 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 H2A 0.1594 -0.0432 0.3170 23 0.990 0.000 C2 C1 C3 H2B 0.1914 0.0210 0.3889 23 0.990 0.000 C2 C1 C3 H3A -0.0406 0.1646 0.3752 23 0.990 0.000 C3 C2 C4 H3B -0.0840 0.0974 0.3074 23 0.990 0.000 C3 C2 C4 H4A 0.1822 0.2139 0.2913 23 0.990 0.000 C4 C5 C3 H4B 0.1531 0.1378 0.2247 23 0.990 0.000 C4 C5 C3 H5A -0.0593 0.3504 0.2689 23 0.990 0.000 C5 C4 C6 H5B -0.0813 0.2760 0.1999 23 0.990 0.000 C5 C4 C6 H6A 0.1711 0.4040 0.1923 23 0.990 0.000 C6 C7 C5 H6B 0.1516 0.3280 0.1235 23 0.990 0.000 C6 C7 C5 H7A -0.0838 0.4583 0.0959 23 0.990 0.000 C7 C8 C6 H7B -0.0797 0.5296 0.1694 23 0.990 0.000 C7 C8 C6 H1 0.0655 -0.2324 0.4713 147 0.840 0.000 O1B C1 H1 H22 0.6130 0.5777 0.0245 43 0.950 0.000 C22 N23 N21 H24 0.3218 0.8906 0.0567 43 0.950 0.000 C24 C25 N23 H25 0.5980 0.9203 0.0510 43 0.950 0.000 C25 C24 N21 H21 0.7668 0.7252 0.0317 43 0.880 0.000 N21 C22 C25 H23 0.3433 0.6782 0.0405 43 0.880 0.000 N23 C22 C24 H32A 1.1016 -0.4616 0.4028 23 0.990 0.000 C32 C33 C31 H32B 1.0935 -0.5328 0.3298 23 0.990 0.000 C32 C33 C31 H33A 0.8668 -0.3292 0.3763 23 0.990 0.000 C33 C32 C34 H33B 0.8450 -0.4043 0.3076 23 0.990 0.000 C33 C32 C34 H34A 1.0995 -0.2778 0.2983 23 0.990 0.000 C34 C35 C33 H34B 1.0724 -0.3499 0.2291 23 0.990 0.000 C34 C35 C33 H35A 0.8629 -0.1391 0.2784 23 0.990 0.000 C35 C34 C36 H35B 0.8293 -0.2127 0.2116 23 0.990 0.000 C35 C34 C36 H36A 1.0914 -0.0918 0.1932 23 0.990 0.000 C36 C37 C35 H36B 1.0497 -0.1607 0.1258 23 0.990 0.000 C36 C37 C35 H37A 0.8114 -0.0219 0.1146 23 0.990 0.000 C37 C38 C36 H37B 0.8446 0.0445 0.1851 23 0.990 0.000 C37 C38 C36 H38 0.9271 0.2311 0.0254 147 0.840 0.000 O38B C38 H38 H42 0.3999 -0.5626 0.4699 43 0.950 0.000 C42 N41 N43 H44 0.6762 -0.8856 0.4542 43 0.950 0.000 C44 C45 N43 H45 0.3964 -0.9085 0.4652 43 0.950 0.000 C45 C44 N41 H41 0.2368 -0.7075 0.4751 43 0.880 0.000 N41 C42 C45 H43 0.6664 -0.6712 0.4581 43 0.880 0.000 N43 C42 C44 H52A 0.4070 -0.1888 0.3687 23 0.990 0.000 C52 C51 C53 H52B 0.5942 -0.2294 0.3516 23 0.990 0.000 C52 C51 C53 H53A 0.5686 -0.2938 0.2295 23 0.990 0.000 C53 C52 C54 H53B 0.3815 -0.2461 0.2417 23 0.990 0.000 C53 C52 C54 H54A 0.3593 -0.3887 0.3571 23 0.990 0.000 C54 C53 C55 H54B 0.5461 -0.4360 0.3454 23 0.990 0.000 C54 C53 C55 H55A 0.3922 -0.5604 0.2983 23 0.990 0.000 C55 C56 C54 H55B 0.3494 -0.4544 0.2281 23 0.990 0.000 C55 C56 C54 H56B 0.6608 -0.5861 0.2483 23 0.990 0.000 C56 C55 C57 H56A 0.6255 -0.4739 0.1814 23 0.990 0.000 C56 C55 C57 H57A 0.4640 -0.5874 0.1276 23 0.990 0.000 C57 C58 C56 H57B 0.6507 -0.6339 0.1133 23 0.990 0.000 C57 C58 C56 H51 0.5549 0.0632 0.3091 147 0.840 0.000 O51A C51 H51 H58B 0.4854 -0.8798 0.1699 147 0.840 0.000 O58B C58 H58B 06skc0002p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.02218 -0.08232 0.42213 1.00000 0.01957 0.01491 0.01818 -0.00107 -0.00475 -0.00381 0.01731 0.00255 0.00021 0.00015 0.00010 0.00000 0.00098 0.00085 0.00091 0.00071 0.00074 0.00072 0.00038 C2 0.10735 0.00059 0.36286 1.00000 0.01795 0.01771 0.01978 0.00261 -0.00178 -0.00393 0.01893 0.00275 0.00020 0.00015 0.00011 0.00000 0.00094 0.00088 0.00093 0.00073 0.00074 0.00073 0.00039 H2A 0.15942 -0.04315 0.31703 1.00000 0.02272 0.00000 0.00000 H2B 0.19139 0.02100 0.38891 1.00000 0.02272 0.00000 0.00000 C3 0.00453 0.11631 0.33064 1.00000 0.01926 0.01797 0.02085 0.00318 -0.00225 -0.00444 0.01979 0.00281 0.00021 0.00016 0.00011 0.00000 0.00096 0.00088 0.00093 0.00074 0.00074 0.00073 0.00039 H3A -0.04061 0.16461 0.37523 1.00000 0.02375 0.00000 0.00000 H3B -0.08404 0.09744 0.30736 1.00000 0.02375 0.00000 0.00000 C4 0.09955 0.18935 0.26645 1.00000 0.01929 0.01863 0.02249 0.00364 -0.00098 -0.00414 0.02081 0.00284 0.00021 0.00016 0.00011 0.00000 0.00096 0.00090 0.00097 0.00076 0.00076 0.00075 0.00040 H4A 0.18217 0.21387 0.29127 1.00000 0.02498 0.00000 0.00000 H4B 0.15312 0.13784 0.22474 1.00000 0.02498 0.00000 0.00000 C5 -0.00184 0.30088 0.22685 1.00000 0.01895 0.01757 0.02035 0.00217 -0.00224 -0.00452 0.01925 0.00274 0.00021 0.00015 0.00011 0.00000 0.00095 0.00089 0.00094 0.00075 0.00075 0.00074 0.00039 H5A -0.05931 0.35041 0.26890 1.00000 0.02310 0.00000 0.00000 H5B -0.08133 0.27599 0.19994 1.00000 0.02310 0.00000 0.00000 C6 0.09300 0.37729 0.16545 1.00000 0.01916 0.01704 0.02106 0.00196 -0.00122 -0.00397 0.01955 0.00279 0.00021 0.00015 0.00011 0.00000 0.00094 0.00087 0.00094 0.00074 0.00074 0.00073 0.00039 H6A 0.17114 0.40396 0.19229 1.00000 0.02346 0.00000 0.00000 H6B 0.15162 0.32798 0.12352 1.00000 0.02346 0.00000 0.00000 C7 -0.01267 0.48660 0.12636 1.00000 0.01685 0.01591 0.01874 0.00020 -0.00173 -0.00371 0.01734 0.00266 0.00020 0.00015 0.00010 0.00000 0.00091 0.00086 0.00091 0.00072 0.00072 0.00071 0.00038 H7A -0.08381 0.45833 0.09590 1.00000 0.02081 0.00000 0.00000 H7B -0.07966 0.52963 0.16937 1.00000 0.02081 0.00000 0.00000 C8 0.07058 0.57558 0.07016 1.00000 0.01829 0.01261 0.01710 -0.00025 -0.00298 -0.00323 0.01602 0.00256 0.00021 0.00015 0.00010 0.00000 0.00094 0.00082 0.00088 0.00070 0.00071 0.00070 0.00037 O1A -0.11570 -0.05885 0.44900 1.00000 0.01781 0.02166 0.02904 0.00284 0.00004 -0.00334 0.02376 0.00197 0.00015 0.00011 0.00008 0.00000 0.00071 0.00067 0.00074 0.00056 0.00056 0.00054 0.00030 O1B 0.11728 -0.18611 0.44107 1.00000 0.01805 0.01645 0.02871 0.00637 -0.00004 -0.00368 0.02219 0.00198 0.00014 0.00011 0.00008 0.00000 0.00066 0.00063 0.00074 0.00055 0.00055 0.00053 0.00030 H1 0.06545 -0.23242 0.47132 1.00000 0.04750 0.00000 0.00734 O8A -0.01886 0.66708 0.03765 1.00000 0.01807 0.01792 0.02848 0.00676 -0.00271 -0.00339 0.02245 0.00193 0.00014 0.00011 0.00008 0.00000 0.00067 0.00064 0.00072 0.00055 0.00054 0.00053 0.00030 O8B 0.21794 0.55853 0.05840 1.00000 0.01606 0.01804 0.03011 0.00172 -0.00258 -0.00402 0.02176 0.00187 0.00014 0.00011 0.00008 0.00000 0.00068 0.00064 0.00073 0.00055 0.00053 0.00051 0.00029 C22 0.57469 0.65950 0.03200 1.00000 0.01996 0.02138 0.02126 -0.00032 -0.00160 -0.00479 0.02105 0.00273 0.00021 0.00017 0.00011 0.00000 0.00099 0.00093 0.00096 0.00077 0.00076 0.00077 0.00040 H22 0.61303 0.57765 0.02451 1.00000 0.02526 0.00000 0.00000 C24 0.41529 0.83160 0.04964 1.00000 0.02109 0.01969 0.02320 -0.00233 -0.00118 -0.00168 0.02181 0.00277 0.00022 0.00016 0.00011 0.00000 0.00099 0.00091 0.00099 0.00077 0.00077 0.00076 0.00041 H24 0.32184 0.89060 0.05671 1.00000 0.02617 0.00000 0.00000 C25 0.56579 0.84760 0.04650 1.00000 0.02367 0.02093 0.02559 -0.00249 -0.00215 -0.00702 0.02309 0.00281 0.00022 0.00017 0.00011 0.00000 0.00103 0.00093 0.00101 0.00079 0.00080 0.00079 0.00042 H25 0.59801 0.92025 0.05100 1.00000 0.02771 0.00000 0.00000 N21 0.66297 0.73934 0.03561 1.00000 0.01493 0.02571 0.02355 -0.00138 -0.00140 -0.00436 0.02157 0.00228 0.00018 0.00013 0.00009 0.00000 0.00082 0.00084 0.00083 0.00067 0.00063 0.00065 0.00035 H21 0.76680 0.72516 0.03167 1.00000 0.03065 0.00000 0.00585 N23 0.42430 0.71286 0.04057 1.00000 0.01707 0.02062 0.02180 0.00102 -0.00260 -0.00543 0.01988 0.00228 0.00017 0.00013 0.00009 0.00000 0.00082 0.00078 0.00082 0.00064 0.00063 0.00065 0.00034 H23 0.34326 0.67822 0.04049 1.00000 0.04896 0.00000 0.00728 C31 0.94142 -0.57452 0.42949 1.00000 0.01738 0.01343 0.01816 -0.00081 -0.00210 -0.00379 0.01631 0.00257 0.00020 0.00015 0.00010 0.00000 0.00094 0.00083 0.00090 0.00071 0.00071 0.00070 0.00037 C32 1.02858 -0.48851 0.37277 1.00000 0.01586 0.01719 0.01909 0.00031 -0.00055 -0.00593 0.01737 0.00265 0.00020 0.00015 0.00010 0.00000 0.00090 0.00087 0.00091 0.00072 0.00071 0.00072 0.00038 H32A 1.10164 -0.46159 0.40278 1.00000 0.02084 0.00000 0.00000 H32B 1.09348 -0.53278 0.32978 1.00000 0.02084 0.00000 0.00000 C33 0.92424 -0.37843 0.33406 1.00000 0.01829 0.01609 0.02249 0.00248 -0.00202 -0.00441 0.01930 0.00276 0.00021 0.00015 0.00011 0.00000 0.00094 0.00086 0.00095 0.00074 0.00075 0.00072 0.00039 H33A 0.86677 -0.32925 0.37629 1.00000 0.02316 0.00000 0.00000 H33B 0.84495 -0.40435 0.30759 1.00000 0.02316 0.00000 0.00000 C34 1.01781 -0.30147 0.27222 1.00000 0.01841 0.01644 0.02042 0.00224 -0.00170 -0.00421 0.01879 0.00274 0.00020 0.00015 0.00011 0.00000 0.00094 0.00087 0.00094 0.00074 0.00074 0.00073 0.00039 H34A 1.09945 -0.27782 0.29827 1.00000 0.02255 0.00000 0.00000 H34B 1.07245 -0.34989 0.22905 1.00000 0.02255 0.00000 0.00000 C35 0.91396 -0.18890 0.23531 1.00000 0.01885 0.01861 0.02271 0.00335 -0.00121 -0.00415 0.02068 0.00285 0.00021 0.00016 0.00011 0.00000 0.00097 0.00090 0.00097 0.00076 0.00075 0.00075 0.00040 H35A 0.86294 -0.13912 0.27836 1.00000 0.02481 0.00000 0.00000 H35B 0.82933 -0.21271 0.21162 1.00000 0.02481 0.00000 0.00000 C36 1.00360 -0.11318 0.17064 1.00000 0.01971 0.01632 0.02071 0.00111 -0.00011 -0.00444 0.01932 0.00279 0.00021 0.00015 0.00011 0.00000 0.00095 0.00086 0.00092 0.00073 0.00074 0.00072 0.00039 H36A 1.09136 -0.09181 0.19320 1.00000 0.02318 0.00000 0.00000 H36B 1.04968 -0.16074 0.12579 1.00000 0.02318 0.00000 0.00000 C37 0.89575 0.00073 0.13913 1.00000 0.01847 0.01926 0.02355 0.00162 -0.00179 -0.00474 0.02074 0.00281 0.00021 0.00016 0.00011 0.00000 0.00096 0.00090 0.00098 0.00077 0.00076 0.00075 0.00040 H37A 0.81139 -0.02194 0.11457 1.00000 0.02489 0.00000 0.00000 H37B 0.84456 0.04448 0.18508 1.00000 0.02489 0.00000 0.00000 C38 0.97598 0.08435 0.07844 1.00000 0.01923 0.01480 0.01742 -0.00083 -0.00353 -0.00404 0.01700 0.00255 0.00021 0.00015 0.00010 0.00000 0.00097 0.00085 0.00090 0.00071 0.00073 0.00071 0.00038 O31A 0.79437 -0.55643 0.43787 1.00000 0.01503 0.01904 0.03048 0.00327 -0.00277 -0.00438 0.02196 0.00188 0.00014 0.00011 0.00008 0.00000 0.00068 0.00065 0.00073 0.00055 0.00053 0.00052 0.00030 O31B 1.02722 -0.66445 0.46585 1.00000 0.01776 0.01721 0.02803 0.00628 -0.00408 -0.00380 0.02169 0.00190 0.00014 0.00011 0.00008 0.00000 0.00066 0.00063 0.00071 0.00054 0.00054 0.00052 0.00029 O38A 1.11423 0.06309 0.05101 1.00000 0.01855 0.02044 0.02918 0.00451 0.00082 -0.00284 0.02396 0.00199 0.00015 0.00011 0.00008 0.00000 0.00071 0.00066 0.00074 0.00056 0.00056 0.00054 0.00031 O38B 0.87816 0.18596 0.05842 1.00000 0.01892 0.01699 0.02774 0.00625 0.00019 -0.00267 0.02251 0.00200 0.00014 0.00011 0.00008 0.00000 0.00067 0.00063 0.00074 0.00056 0.00056 0.00054 0.00030 H38 0.92711 0.23110 0.02536 1.00000 0.05792 0.00000 0.00825 C42 0.43387 -0.64631 0.46753 1.00000 0.01961 0.01907 0.02319 -0.00230 -0.00091 -0.00289 0.02092 0.00273 0.00021 0.00016 0.00011 0.00000 0.00098 0.00090 0.00098 0.00077 0.00076 0.00076 0.00040 H42 0.39986 -0.56259 0.46987 1.00000 0.02510 0.00000 0.00000 C44 0.58536 -0.82371 0.45887 1.00000 0.01989 0.01800 0.02307 -0.00245 -0.00195 -0.00285 0.02049 0.00267 0.00021 0.00016 0.00011 0.00000 0.00097 0.00089 0.00097 0.00076 0.00076 0.00074 0.00040 H44 0.67623 -0.88560 0.45422 1.00000 0.02458 0.00000 0.00000 C45 0.43283 -0.83596 0.46488 1.00000 0.02148 0.01953 0.02471 -0.00225 -0.00129 -0.00600 0.02178 0.00278 0.00021 0.00016 0.00011 0.00000 0.00100 0.00091 0.00100 0.00077 0.00079 0.00077 0.00041 H45 0.39636 -0.90847 0.46522 1.00000 0.02613 0.00000 0.00000 N41 0.34065 -0.72435 0.47040 1.00000 0.01391 0.02370 0.02243 -0.00112 -0.00113 -0.00499 0.02007 0.00224 0.00018 0.00013 0.00009 0.00000 0.00081 0.00081 0.00082 0.00066 0.00061 0.00063 0.00034 H41 0.23677 -0.70754 0.47507 1.00000 0.03904 0.00000 0.00652 N43 0.58284 -0.70412 0.46082 1.00000 0.01547 0.02019 0.02324 0.00058 -0.00216 -0.00537 0.01967 0.00224 0.00017 0.00013 0.00009 0.00000 0.00080 0.00078 0.00083 0.00065 0.00063 0.00064 0.00034 H43 0.66638 -0.67124 0.45807 1.00000 0.03622 0.00000 0.00623 C51 0.50896 -0.07141 0.28570 1.00000 0.01784 0.01882 0.02494 -0.00589 -0.00108 -0.00281 0.02044 0.00269 0.00021 0.00016 0.00011 0.00000 0.00095 0.00090 0.00100 0.00078 0.00077 0.00074 0.00040 C52 0.49706 -0.19519 0.32581 1.00000 0.02000 0.01823 0.02117 -0.00157 -0.00133 -0.00302 0.02008 0.00269 0.00022 0.00015 0.00011 0.00000 0.00096 0.00089 0.00093 0.00075 0.00075 0.00074 0.00039 H52A 0.40702 -0.18877 0.36873 1.00000 0.02409 0.00000 0.00000 H52B 0.59424 -0.22944 0.35156 1.00000 0.02409 0.00000 0.00000 C53 0.47499 -0.28142 0.27011 1.00000 0.02419 0.01656 0.02416 -0.00092 -0.00182 -0.00574 0.02161 0.00274 0.00023 0.00016 0.00011 0.00000 0.00100 0.00089 0.00099 0.00076 0.00078 0.00075 0.00041 H53A 0.56855 -0.29379 0.22949 1.00000 0.02594 0.00000 0.00000 H53B 0.38145 -0.24609 0.24166 1.00000 0.02594 0.00000 0.00000 C54 0.45280 -0.40199 0.31652 1.00000 0.02068 0.01861 0.02360 -0.00115 -0.00062 -0.00744 0.02075 0.00270 0.00022 0.00016 0.00011 0.00000 0.00096 0.00090 0.00098 0.00077 0.00076 0.00075 0.00040 H54A 0.35928 -0.38871 0.35709 1.00000 0.02490 0.00000 0.00000 H54B 0.54609 -0.43603 0.34542 1.00000 0.02490 0.00000 0.00000 C55 0.43094 -0.49295 0.26372 1.00000 0.01749 0.01899 0.02472 -0.00115 -0.00118 -0.00547 0.02038 0.00270 0.00021 0.00016 0.00011 0.00000 0.00093 0.00090 0.00099 0.00076 0.00075 0.00072 0.00040 H55A 0.39220 -0.56044 0.29827 1.00000 0.02446 0.00000 0.00000 H55B 0.34936 -0.45438 0.22814 1.00000 0.02446 0.00000 0.00000 C56 0.58207 -0.54190 0.21263 1.00000 0.01795 0.01785 0.02915 0.00047 -0.00243 -0.00502 0.02177 0.00275 0.00021 0.00016 0.00011 0.00000 0.00094 0.00088 0.00103 0.00078 0.00077 0.00073 0.00041 H56B 0.66077 -0.58615 0.24833 1.00000 0.02613 0.00000 0.00000 H56A 0.62549 -0.47390 0.18143 1.00000 0.02613 0.00000 0.00000 C57 0.55833 -0.62524 0.15484 1.00000 0.02174 0.01857 0.02467 -0.00066 0.00157 -0.00632 0.02191 0.00277 0.00022 0.00016 0.00011 0.00000 0.00098 0.00090 0.00100 0.00078 0.00078 0.00076 0.00041 H57A 0.46403 -0.58740 0.12757 1.00000 0.02629 0.00000 0.00000 H57B 0.65068 -0.63390 0.11328 1.00000 0.02629 0.00000 0.00000 C58 0.53768 -0.74801 0.19391 1.00000 0.01863 0.02001 0.02453 -0.00491 0.00034 -0.00271 0.02126 0.00277 0.00021 0.00016 0.00011 0.00000 0.00096 0.00091 0.00103 0.00079 0.00078 0.00074 0.00040 O51A 0.55210 -0.00571 0.33324 1.00000 0.04352 0.01965 0.02740 -0.00185 -0.00939 -0.01118 0.02900 0.00193 0.00017 0.00012 0.00008 0.00000 0.00089 0.00070 0.00075 0.00060 0.00064 0.00064 0.00033 H51 0.55493 0.06315 0.30910 1.00000 0.08810 0.00000 0.01120 O51B 0.47892 -0.03385 0.21743 1.00000 0.03771 0.02043 0.02554 -0.00085 -0.00653 -0.00957 0.02721 0.00195 0.00016 0.00011 0.00008 0.00000 0.00084 0.00068 0.00075 0.00058 0.00062 0.00060 0.00033 O58B 0.48337 -0.80933 0.14767 1.00000 0.03278 0.01791 0.02650 -0.00053 -0.00566 -0.00877 0.02515 0.00187 0.00016 0.00011 0.00008 0.00000 0.00079 0.00066 0.00073 0.00056 0.00060 0.00059 0.00031 H58B 0.48542 -0.87983 0.16986 1.00000 0.03772 0.00000 0.00000 O58A 0.57174 -0.78810 0.26121 1.00000 0.05205 0.02079 0.02779 0.00089 -0.01249 -0.01252 0.03232 0.00201 0.00018 0.00012 0.00008 0.00000 0.00095 0.00070 0.00078 0.00060 0.00068 0.00065 0.00035 Final Structure Factor Calculation for 06skc0002p-1 in P-1 Total number of l.s. parameters = 426 Maximum vector length = 511 Memory required = 5812 / 22995 wR2 = 0.1430 before cycle 5 for 7472 data and 0 / 426 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0604 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0524 for 4927 Fo > 4sig(Fo) and 0.0908 for all 7472 data wR2 = 0.1430, GooF = S = 1.029, Restrained GooF = 1.029 for all data Occupancy sum of asymmetric unit = 46.00 for non-hydrogen and 50.00 for hydrogen atoms Principal mean square atomic displacements U 0.0213 0.0159 0.0147 C1 0.0246 0.0180 0.0141 C2 0.0260 0.0193 0.0141 C3 0.0286 0.0194 0.0144 C4 0.0242 0.0190 0.0145 C5 0.0249 0.0192 0.0145 C6 0.0204 0.0170 0.0146 C7 0.0188 0.0170 0.0123 C8 0.0348 0.0193 0.0172 O1A 0.0364 0.0181 0.0121 O1B 0.0360 0.0181 0.0133 O8A 0.0325 0.0172 0.0156 O8B 0.0239 0.0208 0.0184 C22 0.0252 0.0219 0.0183 C24 0.0259 0.0248 0.0186 C25 0.0269 0.0231 0.0147 N21 0.0253 0.0186 0.0158 N23 0.0185 0.0174 0.0130 C31 0.0212 0.0185 0.0124 C32 0.0258 0.0184 0.0136 C33 0.0241 0.0185 0.0137 C34 0.0283 0.0190 0.0147 C35 0.0244 0.0195 0.0141 C36 0.0269 0.0191 0.0163 C37 0.0200 0.0166 0.0144 C38 0.0343 0.0172 0.0144 O31A 0.0344 0.0176 0.0131 O31B 0.0371 0.0184 0.0164 O38A 0.0363 0.0185 0.0128 O38B 0.0243 0.0199 0.0185 C42 0.0233 0.0203 0.0178 C44 0.0254 0.0222 0.0177 C45 0.0251 0.0218 0.0133 N41 0.0256 0.0191 0.0143 N43 0.0262 0.0186 0.0165 C51 0.0226 0.0195 0.0181 C52 0.0254 0.0239 0.0156 C53 0.0249 0.0226 0.0148 C54 0.0256 0.0200 0.0156 C55 0.0306 0.0189 0.0158 C56 0.0286 0.0216 0.0155 C57 0.0262 0.0207 0.0169 C58 0.0450 0.0253 0.0168 O51A 0.0385 0.0246 0.0185 O51B 0.0339 0.0256 0.0160 O58B 0.0540 0.0246 0.0184 O58A Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.006 0.012 0.018 0.025 0.034 0.045 0.059 0.081 0.121 1.000 Number in group 857. 718. 697. 720. 767. 751. 733. 752. 733. 744. GooF 0.946 0.979 0.991 0.977 1.013 1.119 1.099 1.113 1.053 0.988 K 5.099 1.476 1.028 1.006 0.980 0.984 0.990 0.999 1.017 1.010 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 784. 725. 733. 757. 752. 735. 746. 745. 742. 753. GooF 0.985 0.932 0.895 0.995 1.021 1.033 1.016 1.031 1.118 1.223 K 1.028 1.062 1.053 1.024 1.037 1.024 1.015 1.025 1.031 0.983 R1 0.224 0.189 0.171 0.145 0.107 0.078 0.061 0.050 0.044 0.039 Recommended weighting scheme: WGHT 0.0606 0.5334 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) 6 0 0 708.28 344.98 6.89 0.099 1.41 3 -3 12 85.78 29.95 5.98 0.029 1.16 5 5 10 27.74 0.93 5.87 0.005 1.23 5 0 0 239.87 134.56 5.54 0.062 1.69 3 0 12 26.15 1.97 5.43 0.007 1.31 0 -3 12 42.13 1.64 5.39 0.007 1.25 -4 3 6 30.83 4.05 4.92 0.011 1.43 6 3 6 424.27 290.43 4.83 0.091 1.35 5 1 2 205.95 135.90 4.58 0.062 1.74 5 -1 6 164.54 103.54 4.55 0.054 1.47 6 6 12 65.41 5.22 4.09 0.012 1.02 0 -4 6 10.18 0.29 3.96 0.003 1.86 6 1 0 31.93 59.18 3.94 0.041 1.43 0 6 12 838.98 598.31 3.85 0.131 1.18 4 -5 10 153.33 226.99 3.79 0.080 1.08 5 -7 6 183.12 262.34 3.79 0.086 0.99 0 -2 5 52.12 30.57 3.73 0.030 2.72 -1 -2 1 119.57 170.01 3.69 0.070 4.67 -3 3 6 196.81 140.05 3.69 0.063 1.64 6 1 2 36.82 63.40 3.61 0.042 1.45 2 8 11 37.42 75.24 3.59 0.046 1.12 -8 -7 10 32.34 91.39 3.59 0.051 0.78 1 -1 3 223.89 303.94 3.58 0.093 4.18 0 -1 2 17.69 7.81 3.55 0.015 6.33 -1 -1 1 5.09 17.27 3.47 0.022 6.40 -3 -9 6 200.68 138.60 3.47 0.063 1.06 -2 -2 4 428.85 551.33 3.40 0.125 2.56 -6 -9 4 284.28 384.74 3.39 0.105 0.96 -1 -8 16 551.91 363.48 3.39 0.102 0.79 7 1 2 91.32 132.62 3.38 0.061 1.24 1 -3 2 121.22 166.63 3.38 0.069 2.92 -3 -7 8 66.61 99.75 3.36 0.053 1.14 1 -11 3 2.85 17.46 3.35 0.022 0.95 0 4 16 210.91 153.07 3.32 0.066 1.02 -3 -7 12 19.21 41.47 3.28 0.034 0.95 2 7 20 25.24 84.03 3.27 0.049 0.79 -1 -9 4 13.73 1.53 3.26 0.007 1.16 -1 4 8 82.93 52.66 3.25 0.039 1.66 -1 3 0 20.82 37.76 3.22 0.033 3.19 -4 -10 12 139.68 80.79 3.22 0.048 0.79 -1 -1 21 48.63 109.18 3.21 0.056 0.78 3 -5 8 101.76 67.36 3.21 0.044 1.26 -6 8 6 438.18 315.20 3.20 0.095 0.86 2 4 6 421.55 328.25 3.18 0.097 2.08 -4 -7 12 63.88 115.78 3.15 0.057 0.91 -4 -11 1 -3.73 13.16 3.12 0.019 0.98 -4 -9 5 1.00 15.75 3.11 0.021 1.05 1 2 2 1607.07 1999.62 3.11 0.239 4.77 5 0 4 86.36 122.59 3.11 0.059 1.64 -6 -9 2 48.82 18.74 3.09 0.023 1.00 Bond lengths and angles C1 - Distance Angles O1A 1.2120 (0.0021) O1B 1.3285 (0.0020) 123.68 (0.16) C2 1.5081 (0.0024) 124.93 (0.15) 111.39 (0.15) C1 - O1A O1B C2 - Distance Angles C1 1.5081 (0.0024) C3 1.5173 (0.0023) 115.38 (0.15) H2A 0.9900 108.43 108.43 H2B 0.9900 108.43 108.43 107.47 C2 - C1 C3 H2A C3 - Distance Angles C2 1.5173 (0.0023) C4 1.5313 (0.0024) 111.22 (0.14) H3A 0.9900 109.39 109.39 H3B 0.9900 109.39 109.39 108.01 C3 - C2 C4 H3A C4 - Distance Angles C5 1.5240 (0.0024) C3 1.5313 (0.0023) 113.13 (0.15) H4A 0.9900 108.95 108.95 H4B 0.9900 108.95 108.95 107.76 C4 - C5 C3 H4A C5 - Distance Angles C4 1.5240 (0.0024) C6 1.5270 (0.0024) 113.48 (0.15) H5A 0.9900 108.87 108.87 H5B 0.9900 108.87 108.87 107.71 C5 - C4 C6 H5A C6 - Distance Angles C7 1.5220 (0.0023) C5 1.5270 (0.0024) 111.86 (0.15) H6A 0.9900 109.24 109.24 H6B 0.9900 109.24 109.24 107.92 C6 - C7 C5 H6A C7 - Distance Angles C8 1.5201 (0.0023) C6 1.5220 (0.0023) 116.36 (0.14) H7A 0.9900 108.20 108.20 H7B 0.9900 108.20 108.20 107.35 C7 - C8 C6 H7A C8 - Distance Angles O8B 1.2494 (0.0021) O8A 1.2768 (0.0020) 123.37 (0.15) C7 1.5201 (0.0023) 120.64 (0.15) 115.98 (0.15) C8 - O8B O8A O1A - Distance Angles C1 1.2120 (0.0021) O1A - O1B - Distance Angles C1 1.3285 (0.0020) H1 0.8400 109.47 O1B - C1 O8A - Distance Angles C8 1.2768 (0.0020) O8A - O8B - Distance Angles C8 1.2494 (0.0021) O8B - C22 - Distance Angles N23 1.3235 (0.0023) N21 1.3263 (0.0023) 108.62 (0.16) H22 0.9500 125.69 125.69 C22 - N23 N21 C24 - Distance Angles C25 1.3545 (0.0026) N23 1.3788 (0.0023) 106.54 (0.16) H24 0.9500 126.73 126.73 C24 - C25 N23 C25 - Distance Angles C24 1.3545 (0.0026) N21 1.3712 (0.0024) 107.19 (0.16) H25 0.9500 126.41 126.41 C25 - C24 N21 N21 - Distance Angles C22 1.3263 (0.0023) C25 1.3712 (0.0024) 108.77 (0.15) H21 0.8800 125.61 125.61 N21 - C22 C25 N23 - Distance Angles C22 1.3235 (0.0023) C24 1.3788 (0.0023) 108.88 (0.15) H23 0.8800 125.56 125.56 N23 - C22 C24 C31 - Distance Angles O31A 1.2455 (0.0021) O31B 1.2777 (0.0020) 123.46 (0.15) C32 1.5196 (0.0023) 120.24 (0.15) 116.29 (0.15) C31 - O31A O31B C32 - Distance Angles C33 1.5194 (0.0023) C31 1.5196 (0.0023) 115.33 (0.14) H32A 0.9900 108.44 108.44 H32B 0.9900 108.44 108.44 107.48 C32 - C33 C31 H32A C33 - Distance Angles C32 1.5194 (0.0023) C34 1.5285 (0.0023) 112.72 (0.14) H33A 0.9900 109.05 109.05 H33B 0.9900 109.05 109.05 107.81 C33 - C32 C34 H33A C34 - Distance Angles C35 1.5243 (0.0024) C33 1.5285 (0.0023) 112.77 (0.15) H34A 0.9900 109.03 109.03 H34B 0.9900 109.03 109.03 107.81 C34 - C35 C33 H34A C35 - Distance Angles C34 1.5243 (0.0024) C36 1.5279 (0.0024) 113.80 (0.15) H35A 0.9900 108.80 108.80 H35B 0.9900 108.80 108.80 107.67 C35 - C34 C36 H35A C36 - Distance Angles C37 1.5198 (0.0023) C35 1.5279 (0.0023) 111.37 (0.15) H36A 0.9900 109.35 109.35 H36B 0.9900 109.35 109.35 107.99 C36 - C37 C35 H36A C37 - Distance Angles C38 1.5036 (0.0024) C36 1.5198 (0.0023) 115.08 (0.15) H37A 0.9900 108.50 108.50 H37B 0.9900 108.50 108.50 107.51 C37 - C38 C36 H37A C38 - Distance Angles O38A 1.2159 (0.0021) O38B 1.3258 (0.0020) 123.34 (0.15) C37 1.5036 (0.0024) 124.72 (0.15) 111.94 (0.15) C38 - O38A O38B O31A - Distance Angles C31 1.2455 (0.0021) O31A - O31B - Distance Angles C31 1.2777 (0.0020) O31B - O38A - Distance Angles C38 1.2159 (0.0021) O38A - O38B - Distance Angles C38 1.3258 (0.0020) H38 0.8400 109.47 O38B - C38 C42 - Distance Angles N41 1.3208 (0.0023) N43 1.3266 (0.0023) 108.74 (0.16) H42 0.9500 125.63 125.63 C42 - N41 N43 C44 - Distance Angles C45 1.3536 (0.0025) N43 1.3740 (0.0023) 106.46 (0.16) H44 0.9500 126.77 126.77 C44 - C45 N43 C45 - Distance Angles C44 1.3536 (0.0025) N41 1.3715 (0.0023) 107.35 (0.16) H45 0.9500 126.33 126.33 C45 - C44 N41 N41 - Distance Angles C42 1.3208 (0.0023) C45 1.3715 (0.0023) 108.60 (0.15) H41 0.8800 125.70 125.70 N41 - C42 C45 N43 - Distance Angles C42 1.3266 (0.0023) C44 1.3740 (0.0023) 108.85 (0.15) H43 0.8800 125.58 125.58 N43 - C42 C44 C51 - Distance Angles O51B 1.2215 (0.0022) O51A 1.3194 (0.0022) 123.20 (0.16) C52 1.5022 (0.0024) 124.34 (0.16) 112.43 (0.16) C51 - O51B O51A C52 - Distance Angles C51 1.5022 (0.0024) C53 1.5204 (0.0025) 114.69 (0.15) H52A 0.9900 108.59 108.59 H52B 0.9900 108.59 108.59 107.56 C52 - C51 C53 H52A C53 - Distance Angles C52 1.5204 (0.0025) C54 1.5259 (0.0024) 111.21 (0.15) H53A 0.9900 109.39 109.39 H53B 0.9900 109.39 109.39 108.01 C53 - C52 C54 H53A C54 - Distance Angles C53 1.5259 (0.0024) C55 1.5268 (0.0025) 113.73 (0.15) H54A 0.9900 108.82 108.82 H54B 0.9900 108.82 108.82 107.68 C54 - C53 C55 H54A C55 - Distance Angles C56 1.5196 (0.0026) C54 1.5268 (0.0025) 113.02 (0.15) H55A 0.9900 108.98 108.98 H55B 0.9900 108.98 108.98 107.77 C55 - C56 C54 H55A C56 - Distance Angles C55 1.5196 (0.0026) C57 1.5266 (0.0026) 113.31 (0.15) H56B 0.9900 108.91 108.91 H56A 0.9900 108.91 108.91 107.74 C56 - C55 C57 H56B C57 - Distance Angles C58 1.5040 (0.0025) C56 1.5266 (0.0026) 114.33 (0.15) H57A 0.9900 108.68 108.68 H57B 0.9900 108.68 108.68 107.61 C57 - C58 C56 H57A C58 - Distance Angles O58A 1.2217 (0.0022) O58B 1.3186 (0.0022) 123.30 (0.17) C57 1.5040 (0.0025) 123.18 (0.17) 113.49 (0.16) C58 - O58A O58B O51A - Distance Angles C51 1.3194 (0.0022) H51 0.8400 109.47 O51A - C51 O51B - Distance Angles C51 1.2215 (0.0022) O51B - O58B - Distance Angles C58 1.3186 (0.0022) H58B 0.8400 109.47 O58B - C58 O58A - Distance Angles C58 1.2217 (0.0022) O58A - Selected torsion angles -5.66 ( 0.26) O1A - C1 - C2 - C3 173.73 ( 0.15) O1B - C1 - C2 - C3 -175.67 ( 0.15) C1 - C2 - C3 - C4 174.76 ( 0.16) C2 - C3 - C4 - C5 177.38 ( 0.15) C3 - C4 - C5 - C6 179.09 ( 0.15) C4 - C5 - C6 - C7 174.23 ( 0.15) C5 - C6 - C7 - C8 -0.77 ( 0.25) C6 - C7 - C8 - O8B -179.94 ( 0.15) C6 - C7 - C8 - O8A 0.04 ( 0.20) N23 - C24 - C25 - N21 -0.28 ( 0.20) N23 - C22 - N21 - C25 0.14 ( 0.20) C24 - C25 - N21 - C22 0.30 ( 0.20) N21 - C22 - N23 - C24 -0.21 ( 0.21) C25 - C24 - N23 - C22 4.37 ( 0.25) O31A - C31 - C32 - C33 -176.50 ( 0.15) O31B - C31 - C32 - C33 -174.89 ( 0.15) C31 - C32 - C33 - C34 -178.14 ( 0.15) C32 - C33 - C34 - C35 -177.49 ( 0.15) C33 - C34 - C35 - C36 -177.13 ( 0.16) C34 - C35 - C36 - C37 176.71 ( 0.15) C35 - C36 - C37 - C38 4.50 ( 0.27) C36 - C37 - C38 - O38A -174.84 ( 0.15) C36 - C37 - C38 - O38B -0.03 ( 0.20) N43 - C44 - C45 - N41 -0.36 ( 0.20) N43 - C42 - N41 - C45 0.24 ( 0.20) C44 - C45 - N41 - C42 0.34 ( 0.21) N41 - C42 - N43 - C44 -0.19 ( 0.21) C45 - C44 - N43 - C42 11.37 ( 0.26) O51B - C51 - C52 - C53 -170.20 ( 0.16) O51A - C51 - C52 - C53 -176.12 ( 0.15) C51 - C52 - C53 - C54 -179.67 ( 0.15) C52 - C53 - C54 - C55 72.10 ( 0.20) C53 - C54 - C55 - C56 -175.40 ( 0.15) C54 - C55 - C56 - C57 -75.20 ( 0.20) C55 - C56 - C57 - C58 -15.82 ( 0.26) C56 - C57 - C58 - O58A 165.92 ( 0.15) C56 - C57 - C58 - O58B Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.89 2.7356(19) 159.7 N23-H23...O8B 0.88 1.86 2.7079(19) 160.2 N43-H43...O31A 0.84 1.73 2.5647(17) 175.5 O1B-H1...O31B_$1 0.88 1.86 2.728(2) 168.2 N21-H21...O8A_$2 0.84 1.71 2.5513(17) 175.2 O38B-H38...O8A_$3 0.88 1.81 2.6838(19) 169.9 N41-H41...O31B_$4 0.84 1.81 2.6469(18) 176.0 O51A-H51...O58A_$5 0.84 1.84 2.6831(17) 176.9 O58B-H58B...O51B_$6 FMAP and GRID set by program FMAP 2 3 40 GRID -1.351 -2 -2 1.351 2 2 R1 = 0.0907 for 7472 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.31 at 0.0231 0.5316 0.0996 [ 0.73 A from C7 ] Deepest hole -0.30 at 0.4737 0.2777 0.4579 [ 0.90 A from C42 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 5328 / 29595 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0231 0.5316 0.0996 1.00000 0.05 0.31 0.73 C7 0.79 C8 1.38 H7B 1.39 H7A Q2 1 0.9841 -0.5360 0.3958 1.00000 0.05 0.28 0.76 C32 0.77 C31 1.36 H32B 1.49 H32A Q3 1 0.4253 -0.2172 0.2293 1.00000 0.05 0.28 0.56 H53B 1.01 C53 1.37 H53A 1.90 C52 Q4 1 0.9762 -0.3386 0.3064 1.00000 0.05 0.27 0.76 C34 0.77 C33 1.38 H34A 1.41 H33A Q5 1 0.0537 -0.0413 0.3802 1.00000 0.05 0.26 0.74 C2 0.84 C1 1.31 H2A 1.55 H2B Shortest distances between peaks (including symmetry equivalents) 2 4 2.53 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. 1.61: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.50: Structure factors and derivatives 8.63: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.64: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.13: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0002p-1 finished at 16:01:26 Total CPU time: 13.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++