+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + ssg0302 started at 12:36:37 on 06-May-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL ssg0302 in C2 CELL 0.69110 23.0890 6.4030 18.4960 90.000 94.025 90.000 ZERR 2.00 0.0070 0.0020 0.0060 0.000 0.003 0.000 LATT -7 SYMM - X, Y, - Z SFAC C H N O UNIT 94 200 8 24 V = 2727.68 F(000) = 1012.0 Mu = 0.08 mm-1 Cell Wt = 1826.62 Rho = 1.112 MERG 4 SHEL 7 0.77 HTAB N25 O1B HTAB N45 O5B EQIV_$1 x, y-1, z HTAB N25 O1A_$1 HTAB N45 O5A_$1 EQIV_$2 -x+1/2, y-1/2, -z HTAB N25 O1A_$2 EQIV_$3 x-1/2, y-1/2, z HTAB O31B O5B_$3 EQIV_$4 -x+1/2, y-1/2, -z+1 HTAB N45 O5A_$4 EQIV_$5 -x, y, -z+1 MPLA O31A O31B C31 MPLA O31A_$5 O31B_$5 C31_$5 FMAP 2 PLAN 10 SIZE 0.02 0.02 0.20 ACTA CONF BOND $H WGHT 0.07050 0.64760 L.S. 4 TEMP -153.00 FVAR 0.27506 MOLE 1 C1 1 0.265833 0.666599 0.144818 11.00000 0.01769 0.02493 = 0.01963 -0.00101 -0.00102 0.00124 C2 1 0.279051 0.767791 0.218354 11.00000 0.02253 0.02567 = 0.01945 -0.00289 -0.00068 0.00072 AFIX 23 H2A 2 0.247458 0.735329 0.250096 11.00000 -1.20000 H2B 2 0.280661 0.921305 0.212442 11.00000 -1.20000 AFIX 0 C3 1 0.336762 0.690361 0.254116 11.00000 0.02142 0.03336 = 0.01877 -0.00092 0.00182 0.00000 AFIX 23 H3A 2 0.368825 0.737855 0.225295 11.00000 -1.20000 H3B 2 0.336915 0.535750 0.254421 11.00000 -1.20000 AFIX 0 C4 1 0.347188 0.770815 0.332234 11.00000 0.02414 0.03138 = 0.02174 0.00010 -0.00086 -0.00694 AFIX 23 H4A 2 0.388221 0.746629 0.349392 11.00000 -1.20000 H4B 2 0.339848 0.923084 0.333246 11.00000 -1.20000 AFIX 0 C5 1 0.307901 0.661685 0.382469 11.00000 0.01928 0.02916 = 0.01658 -0.00101 -0.00250 -0.00222 O1A 4 0.265660 0.782440 0.088576 11.00000 0.03508 0.02509 = 0.02112 0.00150 -0.00435 -0.00391 O1B 4 0.256394 0.475822 0.143130 11.00000 0.03283 0.02329 = 0.02351 -0.00100 0.00111 -0.00159 O5A 4 0.273576 0.767375 0.417704 11.00000 0.02661 0.02507 = 0.02251 0.00035 0.00068 0.00317 O5B 4 0.312223 0.465077 0.387459 11.00000 0.02115 0.02313 = 0.02906 -0.00080 0.00065 -0.00051 MOLE 2 C21 1 0.453739 0.160775 0.222046 11.00000 0.02686 0.05523 = 0.02547 -0.00015 -0.00616 0.00197 AFIX 137 H21A 2 0.494329 0.132974 0.238252 11.00000 -1.50000 H21B 2 0.428705 0.056654 0.243011 11.00000 -1.50000 H21C 2 0.442902 0.300621 0.237874 11.00000 -1.50000 AFIX 0 C22 1 0.446310 0.148297 0.138597 11.00000 0.02018 0.02818 = 0.02423 0.00092 -0.00288 -0.00143 C23 1 0.380481 0.176776 0.118174 11.00000 0.02173 0.02689 = 0.01950 -0.00075 -0.00241 0.00024 AFIX 23 H23A 2 0.360900 0.052937 0.137255 11.00000 -1.20000 H23B 2 0.367896 0.298211 0.146262 11.00000 -1.20000 AFIX 0 C24 1 0.354562 0.208168 0.039464 11.00000 0.01895 0.02472 = 0.02011 0.00109 -0.00057 0.00096 C26 1 0.483942 0.319316 0.108306 11.00000 0.02621 0.03843 = 0.04069 0.00525 -0.00204 -0.00733 AFIX 137 H26A 2 0.524206 0.302243 0.127913 11.00000 -1.50000 H26B 2 0.469533 0.456467 0.122246 11.00000 -1.50000 H26C 2 0.482214 0.308887 0.055337 11.00000 -1.50000 AFIX 0 C27 1 0.467663 -0.065324 0.115944 11.00000 0.03178 0.03337 = 0.04204 -0.00381 -0.01000 0.00931 AFIX 137 H27A 2 0.467120 -0.072118 0.062969 11.00000 -1.50000 H27B 2 0.442227 -0.173940 0.133471 11.00000 -1.50000 H27C 2 0.507384 -0.087402 0.136813 11.00000 -1.50000 AFIX 0 C28 1 0.370912 0.042857 -0.014590 11.00000 0.02859 0.03067 = 0.02380 -0.00368 -0.00122 0.00519 AFIX 137 H28A 2 0.364845 -0.096299 0.005605 11.00000 -1.50000 H28B 2 0.411833 0.059288 -0.024360 11.00000 -1.50000 H28C 2 0.346587 0.059117 -0.059828 11.00000 -1.50000 AFIX 0 C29 1 0.364153 0.427237 0.010072 11.00000 0.02605 0.02719 = 0.02822 0.00659 -0.00074 -0.00078 AFIX 137 H29A 2 0.405332 0.446006 0.002033 11.00000 -1.50000 H29B 2 0.352431 0.530976 0.045164 11.00000 -1.50000 H29C 2 0.340853 0.445404 -0.035856 11.00000 -1.50000 AFIX 0 N25 3 0.289624 0.188177 0.045658 11.00000 0.02182 0.02199 = 0.02043 0.00218 -0.00285 -0.00140 AFIX 147 H25A 2 0.282973 0.082634 0.063229 11.00000 0.04209 H25B 2 0.267183 0.204306 0.002558 11.00000 0.04709 H25C 2 0.274214 0.292302 0.079600 11.00000 0.03952 AFIX 0 MOLE 3 C31 1 -0.042785 -0.195874 0.415048 11.00000 0.03091 0.04078 = 0.03217 -0.00429 0.00001 0.00198 C32 1 0.004525 -0.352025 0.431592 11.00000 0.02903 0.04541 = 0.03700 -0.00435 0.00141 0.00472 AFIX 23 H32A 2 0.042030 -0.276550 0.435885 11.00000 -1.20000 H32B 2 0.005514 -0.448133 0.389768 11.00000 -1.20000 AFIX 0 C33 1 0.000000 -0.483169 0.500000 10.50000 0.02155 0.03461 = 0.04347 0.00000 -0.00138 0.00000 AFIX 23 H33A 2 -0.034600 -0.574341 0.493440 10.50000 -1.20000 H33B 2 0.034600 -0.574341 0.506560 10.50000 -1.20000 AFIX 0 O31A 4 -0.034141 -0.012187 0.403416 11.00000 0.03529 0.04747 = 0.08814 0.01614 0.00001 -0.00327 O31B 4 -0.094728 -0.278921 0.414144 11.00000 0.02873 0.03539 = 0.05899 -0.00428 -0.00127 0.00149 AFIX 147 H31 2 -0.119617 -0.183783 0.416116 11.00000 0.17942 AFIX 0 MOLE 4 C41 1 0.144958 0.113222 0.187649 11.00000 0.03529 0.04942 = 0.02172 -0.00278 -0.00395 0.00182 AFIX 137 H41A 2 0.144754 -0.038492 0.194620 11.00000 -1.50000 H41B 2 0.183738 0.158139 0.175763 11.00000 -1.50000 H41C 2 0.116560 0.150869 0.147919 11.00000 -1.50000 AFIX 0 C42 1 0.128949 0.221994 0.257877 11.00000 0.02263 0.02981 = 0.02074 0.00196 -0.00341 -0.00050 C43 1 0.178249 0.167865 0.316155 11.00000 0.02048 0.02594 = 0.02056 0.00016 -0.00156 0.00254 AFIX 23 H43A 2 0.186952 0.017570 0.310561 11.00000 -1.20000 H43B 2 0.213144 0.245262 0.303122 11.00000 -1.20000 AFIX 0 C44 1 0.172241 0.206064 0.397641 11.00000 0.01697 0.02169 = 0.02151 0.00206 -0.00206 -0.00091 C46 1 0.125752 0.457975 0.242578 11.00000 0.02727 0.03401 = 0.03333 0.00928 -0.00559 0.00057 AFIX 137 H46A 2 0.098316 0.484135 0.200701 11.00000 -1.50000 H46B 2 0.164283 0.509365 0.232216 11.00000 -1.50000 H46C 2 0.112620 0.530783 0.285070 11.00000 -1.50000 AFIX 0 C47 1 0.068985 0.142309 0.276066 11.00000 0.02480 0.04033 = 0.03025 0.00701 -0.00445 -0.00620 AFIX 137 H47A 2 0.056227 0.218767 0.318011 11.00000 -1.50000 H47B 2 0.071376 -0.007068 0.287429 11.00000 -1.50000 H47C 2 0.041064 0.164348 0.234373 11.00000 -1.50000 AFIX 0 C48 1 0.134206 0.044067 0.431820 11.00000 0.02647 0.03263 = 0.02712 0.00508 -0.00133 -0.00704 AFIX 137 H48A 2 0.148976 -0.096192 0.422559 11.00000 -1.50000 H48B 2 0.094236 0.056368 0.410654 11.00000 -1.50000 H48C 2 0.134957 0.067902 0.484215 11.00000 -1.50000 AFIX 0 C49 1 0.154133 0.426235 0.417036 11.00000 0.02242 0.02960 = 0.02900 -0.00435 -0.00118 0.00408 AFIX 137 H49A 2 0.156312 0.441718 0.469870 11.00000 -1.50000 H49B 2 0.114216 0.451593 0.397430 11.00000 -1.50000 H49C 2 0.180202 0.527300 0.396309 11.00000 -1.50000 AFIX 0 N45 3 0.233088 0.175849 0.433064 11.00000 0.02013 0.01956 = 0.01983 -0.00003 -0.00123 0.00052 AFIX 137 H45A 2 0.246217 0.046330 0.422258 11.00000 0.01884 H45B 2 0.232259 0.189019 0.481969 11.00000 0.04411 H45C 2 0.257208 0.274111 0.416169 11.00000 0.03177 AFIX 0 HKLF 4 Covalent radii and connectivity table for ssg0302 in C2 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - C1 C3 C3 - C2 C4 C4 - C5 C3 C5 - O5A O5B C4 O1A - C1 O1B - C1 O5A - C5 O5B - C5 C21 - C22 C22 - C27 C26 C21 C23 C23 - C24 C22 C24 - N25 C28 C29 C23 C26 - C22 C27 - C22 C28 - C24 C29 - C24 N25 - C24 C31 - O31A O31B C32 C32 - C31 C33 C33 - C32_$5 C32 O31A - C31 O31B - C31 C41 - C42 C42 - C47 C46 C41 C43 C43 - C44 C42 C44 - N45 C49 C48 C43 C46 - C42 C47 - C42 C48 - C44 C49 - C44 N45 - C44 Operators for generating equivalent atoms: $1 x, y-1, z $2 -x+1/2, y-1/2, -z $3 x-1/2, y-1/2, z $4 -x+1/2, y-1/2, -z+1 $5 -x, y, -z+1 Floating origin restraints generated 12632 Reflections read, of which 614 rejected -29 =< h =< 29, -8 =< k =< 8, -24 =< l =< 23, Max. 2-theta = 53.33 0 Systematic absence violations 0 Inconsistent equivalents 3392 Unique reflections, of which 0 suppressed R(int) = 0.0565 R(sigma) = 0.0552 Friedel opposites merged Maximum memory for data reduction = 4339 / 39908 Special position constraints for C33 x = 0.0000 z = 0.5000 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 5334 / 381980 wR2 = 0.1217 before cycle 1 for 3392 data and 305 / 305 parameters GooF = S = 1.038; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0705 * P )^2 + 0.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27506 0.00065 -0.002 OSF Mean shift/esd = 0.003 Maximum = -0.021 for tors H31 Max. shift = 0.002 A for H31 Max. dU = 0.000 for H31 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5334 / 381980 wR2 = 0.1217 before cycle 2 for 3392 data and 305 / 305 parameters GooF = S = 1.038; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0705 * P )^2 + 0.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27506 0.00065 0.001 OSF Mean shift/esd = 0.001 Maximum = 0.019 for U11 H31 Max. shift = 0.001 A for H31 Max. dU = 0.001 for H31 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5334 / 381980 wR2 = 0.1217 before cycle 3 for 3392 data and 305 / 305 parameters GooF = S = 1.038; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0705 * P )^2 + 0.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27506 0.00065 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.012 for U11 H31 Max. shift = 0.001 A for H31 Max. dU = 0.000 for H31 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5334 / 381980 wR2 = 0.1217 before cycle 4 for 3392 data and 305 / 305 parameters GooF = S = 1.038; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0705 * P )^2 + 0.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27506 0.00065 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.008 for U11 H31 Max. shift = 0.000 A for H31 Max. dU = 0.000 for H31 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 0.2475 0.7353 0.2501 23 0.990 0.000 C2 C1 C3 H2B 0.2807 0.9213 0.2124 23 0.990 0.000 C2 C1 C3 H3A 0.3688 0.7379 0.2253 23 0.990 0.000 C3 C2 C4 H3B 0.3369 0.5358 0.2544 23 0.990 0.000 C3 C2 C4 H4A 0.3882 0.7466 0.3494 23 0.990 0.000 C4 C5 C3 H4B 0.3398 0.9231 0.3332 23 0.990 0.000 C4 C5 C3 H21A 0.4943 0.1330 0.2383 137 0.980 0.000 C21 C22 H21A H21B 0.4287 0.0566 0.2430 137 0.980 0.000 C21 C22 H21A H21C 0.4429 0.3006 0.2379 137 0.980 0.000 C21 C22 H21A H23A 0.3609 0.0529 0.1373 23 0.990 0.000 C23 C24 C22 H23B 0.3679 0.2982 0.1463 23 0.990 0.000 C23 C24 C22 H26A 0.5242 0.3022 0.1279 137 0.980 0.000 C26 C22 H26A H26B 0.4695 0.4565 0.1223 137 0.980 0.000 C26 C22 H26A H26C 0.4822 0.3089 0.0553 137 0.980 0.000 C26 C22 H26A H27A 0.4671 -0.0721 0.0630 137 0.980 0.000 C27 C22 H27A H27B 0.4422 -0.1739 0.1335 137 0.980 0.000 C27 C22 H27A H27C 0.5074 -0.0874 0.1368 137 0.980 0.000 C27 C22 H27A H28A 0.3648 -0.0963 0.0056 137 0.980 0.000 C28 C24 H28A H28B 0.4118 0.0593 -0.0244 137 0.980 0.000 C28 C24 H28A H28C 0.3466 0.0591 -0.0598 137 0.980 0.000 C28 C24 H28A H29A 0.4053 0.4460 0.0020 137 0.980 0.000 C29 C24 H29A H29B 0.3524 0.5310 0.0452 137 0.980 0.000 C29 C24 H29A H29C 0.3409 0.4454 -0.0359 137 0.980 0.000 C29 C24 H29A H25A 0.2830 0.0826 0.0632 147 0.770 0.000 N25 C24 H25A H32A 0.0420 -0.2766 0.4359 23 0.990 0.000 C32 C31 C33 H32B 0.0055 -0.4481 0.3898 23 0.990 0.000 C32 C31 C33 H33A -0.0346 -0.5743 0.4934 23 0.990 0.000 C33 C32_$5 C32 H33B 0.0346 -0.5743 0.5066 23 0.990 0.000 C33 C32_$5 C32 H31 -0.1196 -0.1838 0.4163 147 0.840 0.000 O31B C31 H31 H41A 0.1447 -0.0385 0.1946 137 0.980 0.000 C41 C42 H41A H41B 0.1837 0.1581 0.1758 137 0.980 0.000 C41 C42 H41A H41C 0.1166 0.1509 0.1479 137 0.980 0.000 C41 C42 H41A H43A 0.1870 0.0176 0.3106 23 0.990 0.000 C43 C44 C42 H43B 0.2131 0.2453 0.3031 23 0.990 0.000 C43 C44 C42 H46A 0.0983 0.4841 0.2007 137 0.980 0.000 C46 C42 H46A H46B 0.1643 0.5094 0.2322 137 0.980 0.000 C46 C42 H46A H46C 0.1126 0.5308 0.2851 137 0.980 0.000 C46 C42 H46A H47A 0.0562 0.2188 0.3180 137 0.980 0.000 C47 C42 H47A H47B 0.0714 -0.0071 0.2874 137 0.980 0.000 C47 C42 H47A H47C 0.0411 0.1644 0.2344 137 0.980 0.000 C47 C42 H47A H48A 0.1490 -0.0962 0.4226 137 0.980 0.000 C48 C44 H48A H48B 0.0942 0.0563 0.4106 137 0.980 0.000 C48 C44 H48A H48C 0.1350 0.0679 0.4842 137 0.980 0.000 C48 C44 H48A H49A 0.1563 0.4417 0.4699 137 0.980 0.000 C49 C44 H49A H49B 0.1142 0.4516 0.3974 137 0.980 0.000 C49 C44 H49A H49C 0.1802 0.5273 0.3963 137 0.980 0.000 C49 C44 H49A H45A 0.2462 0.0463 0.4223 137 0.910 0.000 N45 C44 H45A H45B 0.2323 0.1890 0.4820 137 0.910 0.000 N45 C44 H45A H45C 0.2572 0.2741 0.4162 137 0.910 0.000 N45 C44 H45A ssg0302 in C2 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.26583 0.66660 0.14482 1.00000 0.01770 0.02493 0.01963 -0.00101 -0.00102 0.00124 0.02086 0.00389 0.00009 0.00039 0.00011 0.00000 0.00092 0.00118 0.00096 0.00089 0.00073 0.00088 0.00043 C2 0.27905 0.76779 0.21835 1.00000 0.02253 0.02567 0.01945 -0.00289 -0.00068 0.00072 0.02265 0.00398 0.00010 0.00040 0.00011 0.00000 0.00100 0.00116 0.00096 0.00086 0.00075 0.00090 0.00045 H2A 0.24746 0.73533 0.25010 1.00000 0.02718 0.00000 0.00000 H2B 0.28066 0.92131 0.21244 1.00000 0.02718 0.00000 0.00000 C3 0.33676 0.69036 0.25412 1.00000 0.02142 0.03336 0.01877 -0.00092 0.00182 0.00000 0.02450 0.00412 0.00009 0.00043 0.00011 0.00000 0.00100 0.00130 0.00095 0.00095 0.00076 0.00097 0.00047 H3A 0.36882 0.73786 0.22529 1.00000 0.02940 0.00000 0.00000 H3B 0.33691 0.53575 0.25442 1.00000 0.02940 0.00000 0.00000 C4 0.34719 0.77082 0.33223 1.00000 0.02414 0.03139 0.02174 0.00010 -0.00086 -0.00694 0.02587 0.00408 0.00010 0.00043 0.00012 0.00000 0.00106 0.00128 0.00103 0.00095 0.00081 0.00098 0.00048 H4A 0.38822 0.74663 0.34939 1.00000 0.03104 0.00000 0.00000 H4B 0.33985 0.92308 0.33325 1.00000 0.03104 0.00000 0.00000 C5 0.30790 0.66168 0.38247 1.00000 0.01928 0.02916 0.01658 -0.00100 -0.00250 -0.00222 0.02185 0.00388 0.00009 0.00040 0.00011 0.00000 0.00096 0.00124 0.00091 0.00087 0.00073 0.00093 0.00045 O1A 0.26566 0.78244 0.08858 1.00000 0.03508 0.02509 0.02111 0.00150 -0.00435 -0.00391 0.02739 0.00291 0.00007 0.00029 0.00008 0.00000 0.00091 0.00090 0.00077 0.00067 0.00064 0.00075 0.00038 O1B 0.25639 0.47582 0.14313 1.00000 0.03283 0.02330 0.02351 -0.00100 0.00111 -0.00159 0.02658 0.00300 0.00007 0.00029 0.00009 0.00000 0.00085 0.00087 0.00077 0.00065 0.00063 0.00073 0.00036 O5A 0.27358 0.76737 0.41770 1.00000 0.02661 0.02507 0.02251 0.00035 0.00068 0.00316 0.02478 0.00295 0.00007 0.00028 0.00008 0.00000 0.00079 0.00087 0.00075 0.00065 0.00059 0.00068 0.00035 O5B 0.31222 0.46508 0.38746 1.00000 0.02115 0.02313 0.02906 -0.00080 0.00064 -0.00051 0.02450 0.00287 0.00007 0.00028 0.00009 0.00000 0.00074 0.00087 0.00080 0.00068 0.00059 0.00066 0.00035 C21 0.45374 0.16077 0.22205 1.00000 0.02686 0.05523 0.02548 -0.00014 -0.00615 0.00197 0.03623 0.00503 0.00011 0.00057 0.00013 0.00000 0.00115 0.00183 0.00114 0.00121 0.00090 0.00124 0.00062 H21A 0.49433 0.13298 0.23825 1.00000 0.05435 0.00000 0.00000 H21B 0.42871 0.05665 0.24301 1.00000 0.05435 0.00000 0.00000 H21C 0.44290 0.30062 0.23787 1.00000 0.05435 0.00000 0.00000 C22 0.44631 0.14830 0.13860 1.00000 0.02018 0.02818 0.02423 0.00092 -0.00288 -0.00143 0.02440 0.00414 0.00010 0.00041 0.00012 0.00000 0.00099 0.00126 0.00104 0.00091 0.00080 0.00092 0.00047 C23 0.38048 0.17678 0.11817 1.00000 0.02173 0.02690 0.01949 -0.00075 -0.00241 0.00024 0.02289 0.00398 0.00009 0.00041 0.00011 0.00000 0.00097 0.00120 0.00094 0.00091 0.00074 0.00093 0.00044 H23A 0.36090 0.05294 0.13726 1.00000 0.02747 0.00000 0.00000 H23B 0.36790 0.29821 0.14626 1.00000 0.02747 0.00000 0.00000 C24 0.35456 0.20817 0.03946 1.00000 0.01895 0.02472 0.02011 0.00108 -0.00057 0.00096 0.02135 0.00392 0.00009 0.00038 0.00011 0.00000 0.00093 0.00117 0.00095 0.00084 0.00073 0.00086 0.00044 C26 0.48394 0.31932 0.10831 1.00000 0.02620 0.03842 0.04069 0.00525 -0.00204 -0.00733 0.03531 0.00495 0.00011 0.00049 0.00015 0.00000 0.00121 0.00155 0.00142 0.00118 0.00101 0.00110 0.00060 H26A 0.52421 0.30223 0.12791 1.00000 0.05297 0.00000 0.00000 H26B 0.46954 0.45647 0.12225 1.00000 0.05297 0.00000 0.00000 H26C 0.48221 0.30890 0.05534 1.00000 0.05297 0.00000 0.00000 C27 0.46766 -0.06533 0.11595 1.00000 0.03178 0.03336 0.04205 -0.00381 -0.01000 0.00932 0.03632 0.00485 0.00012 0.00046 0.00016 0.00000 0.00126 0.00155 0.00146 0.00121 0.00107 0.00116 0.00062 H27A 0.46712 -0.07212 0.06297 1.00000 0.05448 0.00000 0.00000 H27B 0.44223 -0.17394 0.13347 1.00000 0.05448 0.00000 0.00000 H27C 0.50738 -0.08740 0.13681 1.00000 0.05448 0.00000 0.00000 C28 0.37091 0.04285 -0.01459 1.00000 0.02859 0.03068 0.02380 -0.00368 -0.00122 0.00519 0.02783 0.00438 0.00011 0.00042 0.00012 0.00000 0.00114 0.00136 0.00107 0.00097 0.00087 0.00101 0.00051 H28A 0.36484 -0.09630 0.00560 1.00000 0.04175 0.00000 0.00000 H28B 0.41184 0.05927 -0.02435 1.00000 0.04175 0.00000 0.00000 H28C 0.34659 0.05913 -0.05983 1.00000 0.04175 0.00000 0.00000 C29 0.36415 0.42724 0.01007 1.00000 0.02606 0.02719 0.02822 0.00659 -0.00074 -0.00077 0.02728 0.00450 0.00011 0.00041 0.00013 0.00000 0.00109 0.00132 0.00114 0.00096 0.00089 0.00095 0.00050 H29A 0.40533 0.44601 0.00204 1.00000 0.04092 0.00000 0.00000 H29B 0.35243 0.53098 0.04516 1.00000 0.04092 0.00000 0.00000 H29C 0.34086 0.44540 -0.03586 1.00000 0.04092 0.00000 0.00000 N25 0.28962 0.18818 0.04566 1.00000 0.02181 0.02200 0.02043 0.00218 -0.00285 -0.00140 0.02162 0.00327 0.00008 0.00033 0.00010 0.00000 0.00087 0.00099 0.00083 0.00075 0.00066 0.00078 0.00038 H25A 0.28297 0.08264 0.06323 1.00000 0.04214 0.00000 0.00966 H25B 0.26718 0.20429 0.00256 1.00000 0.04707 0.00000 0.00950 H25C 0.27421 0.29231 0.07960 1.00000 0.03953 0.00000 0.00853 C31 -0.04278 -0.19587 0.41505 1.00000 0.03091 0.04078 0.03218 -0.00429 0.00001 0.00199 0.03473 0.00491 0.00012 0.00049 0.00014 0.00000 0.00129 0.00165 0.00129 0.00117 0.00099 0.00117 0.00060 C32 0.00452 -0.35203 0.43159 1.00000 0.02903 0.04542 0.03701 -0.00435 0.00141 0.00472 0.03720 0.00533 0.00011 0.00053 0.00015 0.00000 0.00124 0.00169 0.00133 0.00123 0.00102 0.00122 0.00062 H32A 0.04203 -0.27655 0.43588 1.00000 0.04463 0.00000 0.00000 H32B 0.00551 -0.44813 0.38977 1.00000 0.04463 0.00000 0.00000 C33 0.00000 -0.48317 0.50000 0.50000 0.02155 0.03461 0.04346 0.00000 -0.00139 0.00000 0.03338 0.00417 0.00000 0.00065 0.00000 0.00000 0.00153 0.00208 0.00198 0.00000 0.00136 0.00000 0.00080 H33A -0.03460 -0.57434 0.49344 0.50000 0.04006 0.00000 0.00000 H33B 0.03460 -0.57434 0.50656 0.50000 0.04006 0.00000 0.00000 O31A -0.03414 -0.01219 0.40342 1.00000 0.03529 0.04746 0.08813 0.01613 0.00001 -0.00327 0.05717 0.00467 0.00010 0.00042 0.00015 0.00000 0.00111 0.00148 0.00179 0.00133 0.00108 0.00105 0.00065 O31B -0.09473 -0.27892 0.41414 1.00000 0.02874 0.03539 0.05896 -0.00427 -0.00126 0.00148 0.04123 0.00360 0.00008 0.00034 0.00012 0.00000 0.00090 0.00118 0.00128 0.00095 0.00085 0.00085 0.00050 H31 -0.11960 -0.18381 0.41632 1.00000 0.18116 0.00000 0.03396 C41 0.14496 0.11322 0.18765 1.00000 0.03529 0.04943 0.02172 -0.00278 -0.00395 0.00182 0.03576 0.00495 0.00012 0.00051 0.00013 0.00000 0.00131 0.00177 0.00109 0.00108 0.00095 0.00120 0.00063 H41A 0.14474 -0.03849 0.19462 1.00000 0.05364 0.00000 0.00000 H41B 0.18374 0.15811 0.17577 1.00000 0.05364 0.00000 0.00000 H41C 0.11656 0.15089 0.14792 1.00000 0.05364 0.00000 0.00000 C42 0.12895 0.22199 0.25788 1.00000 0.02262 0.02981 0.02074 0.00196 -0.00341 -0.00050 0.02462 0.00405 0.00010 0.00041 0.00012 0.00000 0.00100 0.00130 0.00099 0.00087 0.00079 0.00093 0.00048 C43 0.17825 0.16787 0.31615 1.00000 0.02048 0.02594 0.02056 0.00016 -0.00156 0.00255 0.02247 0.00401 0.00009 0.00040 0.00011 0.00000 0.00098 0.00117 0.00096 0.00091 0.00075 0.00092 0.00044 H43A 0.18695 0.01757 0.31056 1.00000 0.02696 0.00000 0.00000 H43B 0.21314 0.24526 0.30312 1.00000 0.02696 0.00000 0.00000 C44 0.17224 0.20606 0.39764 1.00000 0.01697 0.02168 0.02151 0.00206 -0.00206 -0.00090 0.02022 0.00377 0.00009 0.00037 0.00011 0.00000 0.00091 0.00113 0.00097 0.00082 0.00073 0.00082 0.00043 C46 0.12575 0.45798 0.24258 1.00000 0.02727 0.03401 0.03333 0.00928 -0.00558 0.00057 0.03190 0.00482 0.00011 0.00046 0.00014 0.00000 0.00114 0.00143 0.00121 0.00111 0.00092 0.00108 0.00054 H46A 0.09832 0.48414 0.20070 1.00000 0.04785 0.00000 0.00000 H46B 0.16428 0.50937 0.23221 1.00000 0.04785 0.00000 0.00000 H46C 0.11262 0.53079 0.28507 1.00000 0.04785 0.00000 0.00000 C47 0.06898 0.14231 0.27607 1.00000 0.02480 0.04033 0.03025 0.00701 -0.00445 -0.00620 0.03209 0.00465 0.00010 0.00047 0.00014 0.00000 0.00112 0.00154 0.00118 0.00110 0.00091 0.00109 0.00057 H47A 0.05623 0.21875 0.31802 1.00000 0.04814 0.00000 0.00000 H47B 0.07137 -0.00707 0.28742 1.00000 0.04814 0.00000 0.00000 H47C 0.04106 0.16438 0.23438 1.00000 0.04814 0.00000 0.00000 C48 0.13421 0.04407 0.43182 1.00000 0.02647 0.03263 0.02712 0.00508 -0.00133 -0.00705 0.02889 0.00444 0.00011 0.00044 0.00013 0.00000 0.00114 0.00137 0.00111 0.00102 0.00087 0.00101 0.00052 H48A 0.14898 -0.09619 0.42257 1.00000 0.04334 0.00000 0.00000 H48B 0.09424 0.05635 0.41065 1.00000 0.04334 0.00000 0.00000 H48C 0.13495 0.06792 0.48421 1.00000 0.04334 0.00000 0.00000 C49 0.15413 0.42624 0.41704 1.00000 0.02242 0.02960 0.02900 -0.00435 -0.00119 0.00408 0.02715 0.00434 0.00010 0.00042 0.00013 0.00000 0.00105 0.00131 0.00114 0.00097 0.00086 0.00096 0.00050 H49A 0.15631 0.44171 0.46987 1.00000 0.04072 0.00000 0.00000 H49B 0.11422 0.45160 0.39742 1.00000 0.04072 0.00000 0.00000 H49C 0.18021 0.52730 0.39632 1.00000 0.04072 0.00000 0.00000 N45 0.23309 0.17585 0.43306 1.00000 0.02012 0.01955 0.01984 -0.00003 -0.00123 0.00052 0.01996 0.00322 0.00007 0.00032 0.00009 0.00000 0.00083 0.00092 0.00081 0.00074 0.00065 0.00075 0.00036 H45A 0.24621 0.04632 0.42227 1.00000 0.01884 0.00000 0.00633 H45B 0.23226 0.18904 0.48197 1.00000 0.04409 0.00000 0.00906 H45C 0.25721 0.27410 0.41616 1.00000 0.03182 0.00000 0.00773 Final Structure Factor Calculation for ssg0302 in C2 Total number of l.s. parameters = 305 Maximum vector length = 511 Memory required = 5031 / 25046 wR2 = 0.1217 before cycle 5 for 3392 data and 2 / 305 parameters GooF = S = 1.038; Restrained GooF = 1.037 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0705 * P )^2 + 0.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0446 for 3048 Fo > 4sig(Fo) and 0.0508 for all 3392 data wR2 = 0.1217, GooF = S = 1.038, Restrained GooF = 1.037 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 31.50 for non-hydrogen and 50.00 for hydrogen atoms Principal mean square atomic displacements U 0.0255 0.0208 0.0163 C1 0.0274 0.0227 0.0178 C2 0.0334 0.0215 0.0186 C3 0.0358 0.0230 0.0188 C4 0.0296 0.0220 0.0139 C5 0.0393 0.0238 0.0191 O1A 0.0332 0.0244 0.0222 O1B 0.0292 0.0234 0.0217 O5A 0.0294 0.0232 0.0209 O5B 0.0554 0.0347 0.0186 C21 0.0295 0.0262 0.0176 C22 0.0271 0.0247 0.0168 C23 0.0250 0.0217 0.0174 C24 0.0485 0.0347 0.0227 C26 0.0551 0.0328 0.0210 C27 0.0370 0.0243 0.0221 C28 0.0352 0.0257 0.0209 C29 0.0271 0.0208 0.0169 N25 0.0433 0.0316 0.0293 C31 0.0486 0.0353 0.0277 C32 0.0444 0.0346 0.0212 C33 0.0947 0.0424 0.0344 O31A 0.0607 0.0347 0.0282 O31B 0.0502 0.0373 0.0197 C41 0.0307 0.0263 0.0169 C42 0.0272 0.0229 0.0173 C43 0.0251 0.0201 0.0154 C44 0.0450 0.0308 0.0199 C46 0.0477 0.0278 0.0209 C47 0.0404 0.0244 0.0218 C48 0.0359 0.0250 0.0205 C49 0.0229 0.0196 0.0175 N45 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.040 0.063 0.081 0.099 0.118 0.144 0.178 0.230 0.323 1.000 Number in group 340. 344. 348. 339. 325. 342. 335. 342. 336. 341. GooF 0.929 1.141 1.110 1.049 1.086 0.976 1.017 1.034 0.997 1.019 K 0.944 1.056 1.029 1.032 1.023 1.021 1.018 1.001 0.993 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.32 1.66 inf Number in group 353. 331. 335. 347. 336. 334. 340. 335. 341. 340. GooF 0.981 0.996 0.984 0.847 0.917 0.927 0.992 1.067 1.133 1.422 K 1.029 1.028 1.029 1.022 1.006 1.005 0.990 0.983 1.001 1.013 R1 0.093 0.084 0.076 0.059 0.055 0.049 0.040 0.041 0.038 0.038 Recommended weighting scheme: WGHT 0.0705 0.6477 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) -9 1 1 61.29 22.68 5.47 0.042 2.38 4 2 3 139.37 75.86 5.02 0.077 2.51 -9 1 2 220.82 136.42 4.65 0.104 2.34 20 0 2 437.23 735.36 4.63 0.241 1.13 -12 0 6 113.93 58.74 4.16 0.068 1.68 -2 0 9 182.41 108.45 4.03 0.093 2.04 4 2 5 209.96 137.83 4.02 0.104 2.19 -2 0 4 78.70 130.08 3.84 0.101 4.39 11 1 11 94.93 52.50 3.82 0.064 1.24 26 2 5 81.95 37.33 3.76 0.054 0.82 4 4 6 109.21 170.19 3.68 0.116 1.37 -15 3 10 110.41 64.43 3.57 0.071 1.06 22 0 13 338.23 526.45 3.54 0.204 0.82 8 0 6 1252.83 925.11 3.46 0.270 2.03 -12 6 3 110.44 180.42 3.45 0.119 0.93 -1 1 1 3089.50 4218.59 3.45 0.577 5.88 0 4 1 477.65 646.05 3.39 0.226 1.59 2 0 9 4926.33 3763.27 3.34 0.545 1.99 1 3 0 69.73 116.04 3.32 0.096 2.13 -4 0 1 390.68 564.91 3.27 0.211 5.61 3 3 5 478.58 358.95 3.25 0.168 1.78 -4 2 7 507.68 385.17 3.17 0.174 1.95 4 0 8 730.63 546.56 3.15 0.208 2.09 -5 3 2 1037.46 808.77 3.08 0.253 1.91 14 0 6 68.88 38.84 3.06 0.055 1.41 -3 5 16 56.83 24.24 3.06 0.044 0.86 -19 3 14 -4.96 24.14 3.00 0.044 0.85 -2 0 8 2305.10 1793.26 3.00 0.376 2.29 -16 0 3 66.77 36.39 2.99 0.054 1.42 0 2 7 1282.26 1003.29 2.98 0.281 2.03 13 3 9 1612.80 2059.67 2.95 0.403 1.11 4 4 1 80.85 51.08 2.95 0.063 1.53 -12 2 15 41.15 73.41 2.91 0.076 1.02 6 4 4 52.14 83.18 2.89 0.081 1.40 12 0 5 240.54 328.86 2.87 0.161 1.66 2 2 2 477.96 615.17 2.86 0.220 2.91 9 5 14 158.63 102.15 2.86 0.090 0.85 3 1 3 894.55 1128.92 2.83 0.298 3.76 23 5 1 80.45 39.99 2.82 0.056 0.79 25 3 1 268.55 190.31 2.78 0.123 0.84 15 3 3 53.93 28.86 2.77 0.048 1.21 -3 1 11 349.73 268.99 2.76 0.146 1.61 2 4 4 243.51 180.25 2.75 0.119 1.49 15 3 0 119.35 73.52 2.73 0.076 1.25 -2 4 2 1508.53 1914.55 2.73 0.389 1.57 28 2 3 178.98 248.83 2.71 0.140 0.78 8 6 12 -7.44 13.35 2.68 0.032 0.83 -4 0 16 -3.19 18.31 2.67 0.038 1.15 -6 2 2 8084.01 10336.10 2.67 0.903 2.40 6 2 7 96.97 133.47 2.66 0.103 1.76 Bond lengths and angles C1 - Distance Angles O1B 1.2408 (0.0031) O1A 1.2774 (0.0028) 124.10 (0.21) C2 1.5181 (0.0030) 117.82 (0.20) 118.08 (0.22) C1 - O1B O1A C2 - Distance Angles C1 1.5181 (0.0030) C3 1.5281 (0.0031) 111.33 (0.19) H2A 0.9900 109.36 109.36 H2B 0.9900 109.36 109.36 107.99 C2 - C1 C3 H2A C3 - Distance Angles C2 1.5281 (0.0031) C4 1.5369 (0.0030) 111.87 (0.19) H3A 0.9900 109.24 109.24 H3B 0.9900 109.24 109.24 107.92 C3 - C2 C4 H3A C4 - Distance Angles C5 1.5142 (0.0031) C3 1.5369 (0.0030) 111.17 (0.19) H4A 0.9900 109.40 109.40 H4B 0.9900 109.40 109.40 108.01 C4 - C5 C3 H4A C5 - Distance Angles O5A 1.2583 (0.0028) O5B 1.2657 (0.0032) 123.13 (0.21) C4 1.5142 (0.0031) 119.73 (0.23) 117.14 (0.21) C5 - O5A O5B O1A - Distance Angles C1 1.2774 (0.0028) O1A - O1B - Distance Angles C1 1.2408 (0.0031) O1B - O5A - Distance Angles C5 1.2583 (0.0028) O5A - O5B - Distance Angles C5 1.2657 (0.0032) O5B - C21 - Distance Angles C22 1.5430 (0.0032) 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 C27 1.5227 (0.0038) C26 1.5285 (0.0036) 109.84 (0.21) C21 1.5430 (0.0032) 107.84 (0.23) 107.66 (0.22) C23 1.5510 (0.0031) 111.67 (0.20) 113.52 (0.21) 106.01 (0.18) C22 - C27 C26 C21 C23 - Distance Angles C24 1.5478 (0.0029) C22 1.5510 (0.0031) 123.50 (0.18) H23A 0.9900 106.45 106.45 H23B 0.9900 106.45 106.45 106.49 C23 - C24 C22 H23A C24 - Distance Angles N25 1.5172 (0.0027) C28 1.5217 (0.0032) 106.44 (0.18) C29 1.5261 (0.0035) 105.86 (0.18) 110.88 (0.19) C23 1.5478 (0.0029) 103.71 (0.16) 115.49 (0.19) 113.47 (0.19) C24 - N25 C28 C29 C26 - Distance Angles C22 1.5285 (0.0036) 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 1.5227 (0.0038) 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 (0.0032) 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 1.5261 (0.0035) 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 1.5172 (0.0027) H25A 0.7700 109.47 H25B 0.9255 114.96 110.20 H25C 0.9983 112.89 103.31 105.33 N25 - C24 H25A H25B C31 - Distance Angles O31A 1.2147 (0.0040) O31B 1.3110 (0.0034) 123.50 (0.27) C32 1.4965 (0.0041) 123.81 (0.26) 112.68 (0.26) C31 - O31A O31B C32 - Distance Angles C31 1.4965 (0.0041) C33 1.5282 (0.0037) 116.43 (0.22) H32A 0.9900 108.18 108.18 H32B 0.9900 108.18 108.18 107.34 C32 - C31 C33 H32A C33 - Distance Angles C32_$5 1.5282 (0.0037) C32 1.5282 (0.0037) 113.34 (0.36) H33A 0.9900 108.90 108.90 H33B 0.9900 108.90 108.90 107.73 C33 - C32_$5 C32 H33A O31A - Distance Angles C31 1.2147 (0.0040) O31A - O31B - Distance Angles C31 1.3110 (0.0034) H31 0.8400 109.47 O31B - C31 C41 - Distance Angles C42 1.5415 (0.0035) 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 1.5348 (0.0033) C46 1.5381 (0.0039) 109.54 (0.22) C41 1.5415 (0.0035) 107.93 (0.21) 107.46 (0.22) C43 1.5510 (0.0029) 113.75 (0.19) 111.76 (0.20) 106.08 (0.19) C42 - C47 C46 C41 C43 - Distance Angles C44 1.5427 (0.0029) C42 1.5510 (0.0029) 122.11 (0.18) H43A 0.9900 106.80 106.80 H43B 0.9900 106.80 106.80 106.65 C43 - C44 C42 H43A C44 - Distance Angles N45 1.5203 (0.0026) C49 1.5205 (0.0035) 106.10 (0.18) C48 1.5247 (0.0032) 106.05 (0.18) 110.92 (0.19) C43 1.5427 (0.0029) 104.90 (0.16) 115.00 (0.19) 113.02 (0.19) C44 - N45 C49 C48 C46 - Distance Angles C42 1.5381 (0.0039) 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 1.5348 (0.0033) 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 1.5247 (0.0032) 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 1.5205 (0.0035) 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 1.5203 (0.0026) 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 Selected torsion angles 66.24 ( 0.27) O1B - C1 - C2 - C3 -113.10 ( 0.23) O1A - C1 - C2 - C3 -173.10 ( 0.20) C1 - C2 - C3 - C4 72.45 ( 0.27) C2 - C3 - C4 - C5 -121.68 ( 0.22) C3 - C4 - C5 - O5A 59.33 ( 0.27) C3 - C4 - C5 - O5B -72.37 ( 0.30) C27 - C22 - C23 - C24 52.46 ( 0.32) C26 - C22 - C23 - C24 170.44 ( 0.24) C21 - C22 - C23 - C24 169.95 ( 0.22) C22 - C23 - C24 - N25 53.92 ( 0.31) C22 - C23 - C24 - C28 -75.68 ( 0.29) C22 - C23 - C24 - C29 127.47 ( 0.33) O31A - C31 - C32 - C33 -52.80 ( 0.34) O31B - C31 - C32 - C33 -55.52 ( 0.21) C31 - C32 - C33 - C32_$5 -47.89 ( 0.33) C47 - C42 - C43 - C44 76.80 ( 0.28) C46 - C42 - C43 - C44 -166.37 ( 0.22) C41 - C42 - C43 - C44 -168.55 ( 0.21) C42 - C43 - C44 - N45 -52.40 ( 0.29) C42 - C43 - C44 - C49 76.37 ( 0.28) C42 - C43 - C44 - C48 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 1.00 1.73 2.725(3) 172.8 N25-H25C...O1B 0.91 1.87 2.774(3) 174.6 N45-H45C...O5B 0.77 2.02 2.783(3) 168.3 N25-H25A...O1A_$1 0.91 1.90 2.799(3) 169.8 N45-H45A...O5A_$1 0.93 1.87 2.777(2) 167.1 N25-H25B...O1A_$2 0.84 1.89 2.674(3) 156.0 O31B-H31...O5B_$3 0.91 1.94 2.836(3) 169.9 N45-H45B...O5A_$4 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) - 2.3258 (0.0948) x + 1.2572 (0.0244) y + 18.1263 (0.0175) z = 7.3765 (0.0073) * 0.0000 (0.0000) O31A * 0.0000 (0.0000) O31B * 0.0000 (0.0000) C31 Rms deviation of fitted atoms = 0.0000 - 2.3258 (0.0949) x - 1.2572 (0.0245) y + 18.1263 (0.0172) z = 10.7498 (0.0114) Angle to previous plane (with approximate esd) = 22.65 ( 0.19 ) * 0.0000 (0.0000) O31A_$5 * 0.0000 (0.0000) O31B_$5 * 0.0000 (0.0000) C31_$5 Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 2 30 GRID -3.704 -1 -1 3.704 1 1 R1 = 0.0508 for 3392 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.53 at 0.3892 0.1125 0.4543 [ 1.10 A from O31B ] Deepest hole -0.21 at 0.4716 0.4881 0.3619 [ 0.79 A from O31A ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 5819 / 75756 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.1108 -0.3875 0.4543 1.00000 0.05 0.53 1.10 O31B 1.49 H31 2.11 H49A 2.16 C31 Q2 1 -0.0772 -0.1340 0.3787 1.00000 0.05 0.49 1.08 C31 1.22 O31B 1.28 H31 1.32 O31A Q3 1 0.2722 0.7327 0.1826 1.00000 0.05 0.22 0.71 C2 0.82 C1 1.34 H2B 1.41 H2A Q4 1 0.3686 0.1967 0.0766 1.00000 0.05 0.21 0.74 C24 0.81 C23 1.44 H23B 1.47 H23A Q5 1 0.4491 0.0400 0.1201 1.00000 0.05 0.19 0.78 C22 0.81 C27 1.37 H27A 1.40 H27B Q6 1 0.1825 0.0565 0.5239 1.00000 0.05 0.18 1.28 H48C 1.66 H45B 1.74 O5B 1.86 C5 Q7 1 0.0434 0.2341 0.2088 1.00000 0.05 0.18 0.66 H47C 1.46 C47 1.90 H27C 2.02 H47A Q8 1 0.3347 0.7077 0.3559 1.00000 0.05 0.17 0.68 C4 0.87 C5 1.27 H4A 1.45 H4B Q9 1 0.3232 0.2029 0.0435 1.00000 0.05 0.16 0.73 C24 0.79 N25 1.28 H25A 1.45 H25B Q10 1 0.0105 -0.3801 0.3730 1.00000 0.05 0.16 0.55 H32B 1.12 C32 1.48 H32A 1.91 C31 Shortest distances between peaks (including symmetry equivalents) 4 9 1.18 4 5 2.21 1 2 2.31 6 8 2.48 2 10 2.57 2 8 3.00 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.00: Generate connectivity array 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.63: 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 1.41: Structure factors and derivatives 2.00: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.28: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.13: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + ssg0302 finished at 12:36:42 Total CPU time: 4.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++