+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src1140 started at 14:09:53 on 04-Dec-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src1140 in P2(1)2(1)2(1) CELL 0.71073 5.2557 10.3241 24.6007 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0004 0.0009 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H O UNIT 60 88 12 V = 1334.84 F(000) = 544.0 Mu = 0.09 mm-1 Cell Wt = 1001.30 Rho = 1.246 MERG 4 OMIT -3.00 55.00 OMIT 1 0 2 SHEL 7 0.77 FMAP 2 PLAN 20 SIZE 0.06 0.22 0.62 ACTA BOND $H WGHT 0.03980 0.24890 L.S. 4 TEMP -153.00 FVAR 1.12786 MOLE 1 C1 1 0.479009 0.534057 0.159790 11.00000 0.02164 0.01901 = 0.01900 -0.00357 -0.00341 0.00313 AFIX 13 H1 2 0.631594 0.584353 0.171799 11.00000 -1.20000 AFIX 0 C2 1 0.379913 0.459061 0.207996 11.00000 0.03397 0.02089 = 0.02158 0.00057 -0.00466 -0.00427 AFIX 23 H2A 2 0.519761 0.407666 0.224170 11.00000 -1.20000 H2B 2 0.316853 0.520126 0.235946 11.00000 -1.20000 AFIX 0 C4 1 0.207675 0.245524 0.200979 11.00000 0.02776 0.02117 = 0.02016 0.00294 0.00510 0.00296 C5 1 -0.011197 0.165989 0.180467 11.00000 0.02588 0.01961 = 0.03956 0.00099 0.00527 -0.00210 AFIX 23 H5A 2 -0.163314 0.185825 0.202694 11.00000 -1.20000 H5B 2 0.029467 0.073198 0.185719 11.00000 -1.20000 AFIX 0 C6 1 -0.076386 0.188420 0.120462 11.00000 0.02322 0.01784 = 0.04329 -0.00330 -0.00570 0.00053 AFIX 23 H6A 2 -0.217312 0.130008 0.109874 11.00000 -1.20000 H6B 2 -0.135508 0.278729 0.115610 11.00000 -1.20000 AFIX 0 C7 1 0.146655 0.164603 0.084033 11.00000 0.03323 0.01938 = 0.02919 -0.00547 -0.00577 0.00585 AFIX 43 H7 2 0.203957 0.077612 0.081100 11.00000 -1.20000 AFIX 0 C8 1 0.272521 0.252626 0.055413 11.00000 0.03388 0.02467 = 0.02268 -0.00711 -0.00392 0.00705 AFIX 43 H8 2 0.411873 0.222265 0.034375 11.00000 -1.20000 AFIX 0 C9 1 0.217885 0.395076 0.052785 11.00000 0.03192 0.02217 = 0.02267 -0.00253 -0.00872 0.00338 AFIX 23 H9A 2 0.077929 0.415593 0.078306 11.00000 -1.20000 H9B 2 0.159390 0.417128 0.015668 11.00000 -1.20000 AFIX 0 C10 1 0.447899 0.478615 0.066799 11.00000 0.02510 0.02500 = 0.01758 -0.00083 -0.00155 0.00488 AFIX 13 H10 2 0.579247 0.468421 0.037702 11.00000 -1.20000 AFIX 0 C11 1 0.382072 0.621979 0.072656 11.00000 0.02168 0.02078 = 0.01763 -0.00034 -0.00272 0.00061 AFIX 13 H11 2 0.239822 0.646102 0.047630 11.00000 -1.20000 AFIX 0 C12 1 0.615569 0.707307 0.062250 11.00000 0.02561 0.02739 = 0.02453 0.00311 0.00414 0.00067 AFIX 23 H12A 2 0.764904 0.668560 0.080613 11.00000 -1.20000 H12B 2 0.651165 0.709146 0.022740 11.00000 -1.20000 AFIX 0 C13 1 0.580097 0.845423 0.082491 11.00000 0.03020 0.02361 = 0.03108 0.00441 0.00094 -0.00183 AFIX 23 H13A 2 0.439323 0.887110 0.062269 11.00000 -1.20000 H13B 2 0.737250 0.895759 0.075707 11.00000 -1.20000 AFIX 0 C14 1 0.519944 0.846282 0.143265 11.00000 0.02973 0.01999 = 0.02886 -0.00075 -0.00197 -0.00145 AFIX 23 H14A 2 0.667295 0.811423 0.163624 11.00000 -1.20000 H14B 2 0.491434 0.936576 0.155368 11.00000 -1.20000 AFIX 0 C15 1 0.284774 0.765426 0.156032 11.00000 0.02390 0.02211 = 0.02280 -0.00291 0.00030 0.00401 AFIX 23 H15A 2 0.132930 0.810384 0.141501 11.00000 -1.20000 H15B 2 0.265230 0.759506 0.195981 11.00000 -1.20000 AFIX 0 C16 1 0.294119 0.627880 0.132373 11.00000 0.01588 0.02196 = 0.02031 -0.00013 -0.00020 0.00164 AFIX 13 H16 2 0.119332 0.589974 0.134585 11.00000 -1.20000 AFIX 0 O3 3 0.174939 0.373012 0.191523 11.00000 0.02730 0.01763 = 0.03372 0.00171 -0.00277 -0.00129 O4 3 0.389335 0.201284 0.224386 11.00000 0.03753 0.02661 = 0.04248 0.00778 -0.01068 0.00201 O17 3 0.558607 0.443936 0.118461 11.00000 0.02727 0.02380 = 0.02123 -0.00521 -0.00583 0.01056 HKLF 4 Covalent radii and connectivity table for 2008src1140 in P2(1)2(1)2(1) C 0.770 H 0.320 O 0.660 C1 - O17 C2 C16 C2 - O3 C1 C4 - O4 O3 C5 C5 - C4 C6 C6 - C7 C5 C7 - C8 C6 C8 - C7 C9 C9 - C8 C10 C10 - O17 C9 C11 C11 - C10 C12 C16 C12 - C13 C11 C13 - C12 C14 C14 - C15 C13 C15 - C14 C16 C16 - C1 C15 C11 O3 - C4 C2 O4 - C4 O17 - C1 C10 10785 Reflections read, of which 63 rejected -6 =< h =< 6, -12 =< k =< 13, -30 =< l =< 31, Max. 2-theta = 54.93 0 Systematic absence violations 0 Inconsistent equivalents 1796 Unique reflections, of which 0 suppressed R(int) = 0.0467 R(sigma) = 0.0371 Friedel opposites merged Maximum memory for data reduction = 2074 / 17428 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 = 2582 / 202251 wR2 = 0.0887 before cycle 1 for 1796 data and 163 / 163 parameters GooF = S = 1.054; Restrained GooF = 1.054 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0398 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.12787 0.00244 0.004 OSF Mean shift/su = 0.002 Maximum = 0.009 for U23 O4 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C15 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2582 / 202251 wR2 = 0.0887 before cycle 2 for 1796 data and 163 / 163 parameters GooF = S = 1.054; Restrained GooF = 1.054 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0398 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.12787 0.00244 0.001 OSF Mean shift/su = 0.001 Maximum = 0.003 for U23 O4 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C15 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2582 / 202251 wR2 = 0.0887 before cycle 3 for 1796 data and 163 / 163 parameters GooF = S = 1.054; Restrained GooF = 1.054 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0398 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.12787 0.00244 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C16 Max. dU = 0.000 for C14 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2582 / 202251 wR2 = 0.0887 before cycle 4 for 1796 data and 163 / 163 parameters GooF = S = 1.054; Restrained GooF = 1.054 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0398 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.12787 0.00244 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y C13 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C5 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.6316 0.5844 0.1718 13 1.000 0.000 C1 O17 C2 C16 H2A 0.5198 0.4077 0.2242 23 0.990 0.000 C2 O3 C1 H2B 0.3169 0.5201 0.2359 23 0.990 0.000 C2 O3 C1 H5A -0.1633 0.1858 0.2027 23 0.990 0.000 C5 C4 C6 H5B 0.0295 0.0732 0.1857 23 0.990 0.000 C5 C4 C6 H6A -0.2173 0.1300 0.1099 23 0.990 0.000 C6 C7 C5 H6B -0.1355 0.2787 0.1156 23 0.990 0.000 C6 C7 C5 H7 0.2040 0.0776 0.0811 43 0.950 0.000 C7 C8 C6 H8 0.4119 0.2223 0.0344 43 0.950 0.000 C8 C7 C9 H9A 0.0779 0.4156 0.0783 23 0.990 0.000 C9 C8 C10 H9B 0.1594 0.4171 0.0157 23 0.990 0.000 C9 C8 C10 H10 0.5792 0.4684 0.0377 13 1.000 0.000 C10 O17 C9 C11 H11 0.2398 0.6461 0.0476 13 1.000 0.000 C11 C10 C12 C16 H12A 0.7649 0.6686 0.0806 23 0.990 0.000 C12 C13 C11 H12B 0.6512 0.7091 0.0227 23 0.990 0.000 C12 C13 C11 H13A 0.4393 0.8871 0.0623 23 0.990 0.000 C13 C12 C14 H13B 0.7372 0.8958 0.0757 23 0.990 0.000 C13 C12 C14 H14A 0.6673 0.8114 0.1636 23 0.990 0.000 C14 C15 C13 H14B 0.4914 0.9366 0.1554 23 0.990 0.000 C14 C15 C13 H15A 0.1329 0.8104 0.1415 23 0.990 0.000 C15 C14 C16 H15B 0.2652 0.7595 0.1960 23 0.990 0.000 C15 C14 C16 H16 0.1193 0.5900 0.1346 13 1.000 0.000 C16 C1 C15 C11 2008src1140 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.47901 0.53406 0.15979 1.00000 0.02164 0.01901 0.01900 -0.00357 -0.00341 0.00313 0.01988 0.00315 0.00036 0.00018 0.00007 0.00000 0.00089 0.00098 0.00086 0.00074 0.00072 0.00076 0.00040 H1 0.63159 0.58435 0.17180 1.00000 0.02386 0.00000 0.00000 C2 0.37991 0.45906 0.20800 1.00000 0.03398 0.02089 0.02158 0.00057 -0.00466 -0.00427 0.02548 0.00330 0.00041 0.00019 0.00007 0.00000 0.00106 0.00103 0.00088 0.00078 0.00083 0.00089 0.00044 H2A 0.51976 0.40767 0.22417 1.00000 0.03058 0.00000 0.00000 H2B 0.31685 0.52013 0.23595 1.00000 0.03058 0.00000 0.00000 C4 0.20768 0.24552 0.20098 1.00000 0.02776 0.02118 0.02015 0.00294 0.00510 0.00296 0.02303 0.00340 0.00037 0.00019 0.00007 0.00000 0.00097 0.00101 0.00085 0.00078 0.00079 0.00084 0.00041 C5 -0.01120 0.16599 0.18047 1.00000 0.02588 0.01961 0.03956 0.00099 0.00528 -0.00210 0.02835 0.00356 0.00038 0.00020 0.00009 0.00000 0.00100 0.00105 0.00113 0.00091 0.00086 0.00082 0.00047 H5A -0.16331 0.18583 0.20269 1.00000 0.03402 0.00000 0.00000 H5B 0.02947 0.07320 0.18572 1.00000 0.03402 0.00000 0.00000 C6 -0.07638 0.18842 0.12046 1.00000 0.02322 0.01784 0.04329 -0.00330 -0.00570 0.00053 0.02812 0.00338 0.00036 0.00019 0.00008 0.00000 0.00095 0.00102 0.00117 0.00094 0.00094 0.00084 0.00046 H6A -0.21731 0.13001 0.10987 1.00000 0.03374 0.00000 0.00000 H6B -0.13551 0.27873 0.11561 1.00000 0.03374 0.00000 0.00000 C7 0.14665 0.16460 0.08403 1.00000 0.03323 0.01938 0.02919 -0.00547 -0.00578 0.00585 0.02727 0.00336 0.00039 0.00019 0.00008 0.00000 0.00105 0.00103 0.00100 0.00084 0.00089 0.00086 0.00045 H7 0.20395 0.07761 0.08110 1.00000 0.03272 0.00000 0.00000 C8 0.27252 0.25263 0.05541 1.00000 0.03388 0.02467 0.02268 -0.00711 -0.00392 0.00705 0.02708 0.00341 0.00041 0.00020 0.00007 0.00000 0.00108 0.00108 0.00093 0.00083 0.00081 0.00093 0.00046 H8 0.41187 0.22226 0.03438 1.00000 0.03249 0.00000 0.00000 C9 0.21789 0.39508 0.05278 1.00000 0.03192 0.02217 0.02267 -0.00252 -0.00872 0.00338 0.02559 0.00333 0.00041 0.00019 0.00008 0.00000 0.00104 0.00106 0.00090 0.00079 0.00083 0.00089 0.00045 H9A 0.07793 0.41559 0.07831 1.00000 0.03071 0.00000 0.00000 H9B 0.15939 0.41713 0.01567 1.00000 0.03071 0.00000 0.00000 C10 0.44790 0.47861 0.06680 1.00000 0.02510 0.02499 0.01758 -0.00083 -0.00155 0.00488 0.02256 0.00327 0.00037 0.00019 0.00007 0.00000 0.00091 0.00106 0.00082 0.00079 0.00076 0.00084 0.00041 H10 0.57924 0.46842 0.03770 1.00000 0.02707 0.00000 0.00000 C11 0.38207 0.62198 0.07266 1.00000 0.02168 0.02078 0.01763 -0.00034 -0.00272 0.00061 0.02003 0.00310 0.00035 0.00018 0.00007 0.00000 0.00084 0.00096 0.00081 0.00074 0.00074 0.00079 0.00038 H11 0.23982 0.64610 0.04763 1.00000 0.02404 0.00000 0.00000 C12 0.61557 0.70731 0.06225 1.00000 0.02561 0.02739 0.02453 0.00312 0.00414 0.00067 0.02584 0.00340 0.00036 0.00019 0.00008 0.00000 0.00096 0.00109 0.00093 0.00082 0.00083 0.00090 0.00044 H12A 0.76490 0.66856 0.08061 1.00000 0.03101 0.00000 0.00000 H12B 0.65116 0.70915 0.02274 1.00000 0.03101 0.00000 0.00000 C13 0.58010 0.84542 0.08249 1.00000 0.03020 0.02361 0.03108 0.00441 0.00094 -0.00183 0.02830 0.00357 0.00042 0.00019 0.00008 0.00000 0.00101 0.00108 0.00105 0.00085 0.00090 0.00088 0.00045 H13A 0.43932 0.88711 0.06227 1.00000 0.03396 0.00000 0.00000 H13B 0.73725 0.89576 0.07571 1.00000 0.03396 0.00000 0.00000 C14 0.51994 0.84628 0.14327 1.00000 0.02973 0.01999 0.02886 -0.00075 -0.00197 -0.00145 0.02619 0.00346 0.00039 0.00020 0.00008 0.00000 0.00106 0.00104 0.00100 0.00082 0.00083 0.00088 0.00046 H14A 0.66730 0.81142 0.16362 1.00000 0.03143 0.00000 0.00000 H14B 0.49143 0.93658 0.15537 1.00000 0.03143 0.00000 0.00000 C15 0.28478 0.76543 0.15603 1.00000 0.02390 0.02212 0.02280 -0.00291 0.00029 0.00401 0.02294 0.00322 0.00036 0.00018 0.00007 0.00000 0.00091 0.00102 0.00090 0.00080 0.00077 0.00081 0.00041 H15A 0.13293 0.81038 0.14150 1.00000 0.02753 0.00000 0.00000 H15B 0.26523 0.75951 0.19598 1.00000 0.02753 0.00000 0.00000 C16 0.29412 0.62788 0.13237 1.00000 0.01588 0.02196 0.02031 -0.00013 -0.00020 0.00164 0.01938 0.00311 0.00035 0.00019 0.00007 0.00000 0.00078 0.00100 0.00087 0.00076 0.00069 0.00078 0.00040 H16 0.11933 0.58997 0.13459 1.00000 0.02326 0.00000 0.00000 O3 0.17494 0.37301 0.19152 1.00000 0.02730 0.01763 0.03372 0.00171 -0.00277 -0.00129 0.02622 0.00229 0.00026 0.00013 0.00005 0.00000 0.00070 0.00070 0.00075 0.00060 0.00061 0.00060 0.00033 O4 0.38933 0.20128 0.22439 1.00000 0.03753 0.02661 0.04248 0.00779 -0.01068 0.00201 0.03554 0.00257 0.00029 0.00014 0.00006 0.00000 0.00086 0.00083 0.00086 0.00067 0.00074 0.00073 0.00039 O17 0.55861 0.44394 0.11846 1.00000 0.02727 0.02380 0.02123 -0.00521 -0.00583 0.01057 0.02410 0.00220 0.00025 0.00013 0.00005 0.00000 0.00071 0.00073 0.00064 0.00056 0.00057 0.00063 0.00032 Final Structure Factor Calculation for 2008src1140 in P2(1)2(1)2(1) Total number of l.s. parameters = 163 Maximum vector length = 511 Memory required = 2421 / 24024 wR2 = 0.0887 before cycle 5 for 1796 data and 2 / 163 parameters GooF = S = 1.054; Restrained GooF = 1.054 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0398 * P )^2 + 0.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0392 for 1592 Fo > 4sig(Fo) and 0.0479 for all 1796 data wR2 = 0.0887, GooF = S = 1.054, Restrained GooF = 1.054 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 18.00 for non-hydrogen and 22.00 for hydrogen atoms Principal mean square atomic displacements U 0.0268 0.0175 0.0154 C1 0.0367 0.0207 0.0191 C2 0.0318 0.0203 0.0170 C4 0.0414 0.0251 0.0186 C5 0.0452 0.0217 0.0174 C6 0.0403 0.0252 0.0163 C7 0.0405 0.0245 0.0163 C8 0.0383 0.0211 0.0174 C9 0.0302 0.0202 0.0173 C10 0.0232 0.0206 0.0163 C11 0.0312 0.0260 0.0203 C12 0.0331 0.0307 0.0211 C13 0.0314 0.0276 0.0197 C14 0.0277 0.0234 0.0177 C15 0.0224 0.0203 0.0155 C16 0.0350 0.0263 0.0173 O3 0.0520 0.0338 0.0208 O4 0.0396 0.0179 0.0148 O17 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.021 0.034 0.045 0.057 0.070 0.083 0.105 0.134 0.192 1.000 Number in group 181. 182. 179. 185. 177. 174. 180. 183. 174. 181. GooF 0.960 1.056 1.057 1.050 1.087 1.018 1.098 1.069 0.957 1.170 K 1.197 1.015 1.005 1.013 1.016 0.998 1.007 0.998 1.007 0.973 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.06 1.18 1.36 1.72 inf Number in group 185. 178. 178. 181. 177. 182. 176. 179. 179. 181. GooF 0.983 1.010 0.923 1.091 1.073 1.029 0.950 0.974 1.053 1.382 K 1.012 1.043 1.036 1.024 1.011 0.995 0.986 0.992 1.020 0.963 R1 0.096 0.098 0.083 0.082 0.057 0.042 0.032 0.028 0.025 0.033 Recommended weighting scheme: WGHT 0.0396 0.2510 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)/su Fc/Fc(max) Resolution(A) 0 0 4 6331.40 10696.29 6.32 1.000 6.15 1 8 16 19.45 52.64 4.76 0.070 0.97 0 5 3 200.21 163.70 3.45 0.124 2.00 6 0 2 72.20 103.69 3.19 0.098 0.87 5 0 3 62.97 42.44 3.15 0.063 1.04 0 6 14 15.60 29.57 3.12 0.053 1.23 2 1 2 8.50 4.43 2.93 0.020 2.49 2 5 0 86.86 70.06 2.80 0.081 1.62 2 9 13 6.37 16.17 2.78 0.039 0.92 0 13 1 192.69 141.23 2.77 0.115 0.79 3 3 6 3.91 8.00 2.70 0.027 1.46 2 2 1 26.21 19.21 2.64 0.042 2.33 0 5 9 633.12 552.90 2.62 0.227 1.65 1 3 25 24.33 13.01 2.62 0.035 0.93 2 0 5 239.07 275.01 2.57 0.160 2.32 5 2 15 30.75 20.13 2.56 0.043 0.87 2 0 29 142.56 102.54 2.56 0.098 0.81 4 4 14 36.18 26.00 2.54 0.049 0.97 1 9 8 13.96 24.83 2.54 0.048 1.05 4 6 4 120.12 143.29 2.52 0.116 1.03 1 6 28 5.61 17.71 2.52 0.041 0.77 3 2 4 93.90 78.94 2.51 0.086 1.60 1 1 0 3719.87 4147.67 2.42 0.623 4.68 6 4 1 120.54 99.21 2.41 0.096 0.83 1 0 22 163.72 136.47 2.38 0.113 1.09 2 4 2 130.15 112.28 2.36 0.102 1.82 1 7 9 28.28 19.31 2.35 0.042 1.26 3 2 8 109.51 127.96 2.35 0.109 1.46 0 6 8 10.26 5.03 2.34 0.022 1.50 1 9 10 9.46 1.69 2.34 0.013 1.02 5 8 10 24.48 37.23 2.34 0.059 0.77 0 2 18 30.42 21.87 2.32 0.045 1.32 2 1 3 589.60 529.10 2.32 0.222 2.43 0 1 6 1019.07 1138.45 2.32 0.326 3.81 0 3 18 16.34 23.33 2.30 0.047 1.27 4 3 22 220.09 185.87 2.29 0.132 0.83 1 10 10 33.85 22.22 2.27 0.046 0.94 4 2 18 31.80 22.84 2.27 0.046 0.93 1 0 8 50.87 41.16 2.27 0.062 2.65 5 7 0 40.07 27.99 2.26 0.051 0.86 3 3 2 69.76 83.34 2.26 0.088 1.55 0 2 15 104.43 87.49 2.26 0.090 1.56 6 4 8 0.97 8.69 2.24 0.029 0.80 5 5 0 227.08 195.06 2.24 0.135 0.94 5 4 10 246.12 214.15 2.23 0.141 0.91 2 8 1 124.72 107.54 2.23 0.100 1.16 0 2 0 4285.02 4752.35 2.23 0.667 5.16 2 2 28 182.15 153.23 2.21 0.120 0.82 1 10 19 57.86 42.34 2.21 0.063 0.80 2 7 11 109.67 133.62 2.19 0.112 1.11 Bond lengths and angles C1 - Distance Angles O17 1.4403 (0.0021) C2 1.5090 (0.0026) 108.88 (0.15) C16 1.5289 (0.0025) 106.41 (0.13) 116.90 (0.16) H1 1.0000 108.12 108.12 108.12 C1 - O17 C2 C16 C2 - Distance Angles O3 1.4540 (0.0023) C1 1.5090 (0.0026) 110.50 (0.15) H2A 0.9900 109.55 109.55 H2B 0.9900 109.55 109.55 108.10 C2 - O3 C1 H2A C4 - Distance Angles O4 1.2049 (0.0023) O3 1.3476 (0.0023) 123.63 (0.19) C5 1.5007 (0.0027) 124.10 (0.19) 112.24 (0.17) C4 - O4 O3 C5 - Distance Angles C4 1.5007 (0.0027) C6 1.5330 (0.0028) 114.36 (0.17) H5A 0.9900 108.67 108.67 H5B 0.9900 108.67 108.67 107.60 C5 - C4 C6 H5A C6 - Distance Angles C7 1.4959 (0.0028) C5 1.5330 (0.0028) 112.14 (0.16) H6A 0.9900 109.18 109.18 H6B 0.9900 109.18 109.18 107.89 C6 - C7 C5 H6A C7 - Distance Angles C8 1.3263 (0.0029) C6 1.4959 (0.0028) 126.60 (0.19) H7 0.9500 116.70 116.70 C7 - C8 C6 C8 - Distance Angles C7 1.3263 (0.0029) C9 1.4998 (0.0028) 126.82 (0.19) H8 0.9500 116.59 116.59 C8 - C7 C9 C9 - Distance Angles C8 1.4998 (0.0028) C10 1.5245 (0.0027) 113.15 (0.17) H9A 0.9900 108.95 108.95 H9B 0.9900 108.95 108.95 107.76 C9 - C8 C10 H9A C10 - Distance Angles O17 1.4429 (0.0021) C9 1.5245 (0.0027) 112.25 (0.16) C11 1.5268 (0.0026) 104.41 (0.14) 112.96 (0.16) H10 1.0000 109.03 109.03 109.03 C10 - O17 C9 C11 C11 - Distance Angles C10 1.5268 (0.0026) C12 1.5322 (0.0026) 111.11 (0.15) C16 1.5413 (0.0023) 101.32 (0.14) 112.13 (0.15) H11 1.0000 110.65 110.65 110.65 C11 - C10 C12 C16 C12 - Distance Angles C13 1.5218 (0.0027) C11 1.5322 (0.0026) 112.70 (0.16) H12A 0.9900 109.05 109.05 H12B 0.9900 109.05 109.05 107.81 C12 - C13 C11 H12A C13 - Distance Angles C12 1.5218 (0.0027) C14 1.5282 (0.0027) 110.54 (0.16) H13A 0.9900 109.54 109.54 H13B 0.9900 109.54 109.54 108.10 C13 - C12 C14 H13A C14 - Distance Angles C15 1.5242 (0.0027) C13 1.5282 (0.0027) 111.48 (0.17) H14A 0.9900 109.33 109.33 H14B 0.9900 109.33 109.33 107.97 C14 - C15 C13 H14A C15 - Distance Angles C14 1.5242 (0.0027) C16 1.5355 (0.0026) 113.73 (0.16) H15A 0.9900 108.81 108.81 H15B 0.9900 108.81 108.81 107.68 C15 - C14 C16 H15A C16 - Distance Angles C1 1.5289 (0.0025) C15 1.5355 (0.0026) 116.04 (0.15) C11 1.5413 (0.0023) 101.82 (0.14) 114.04 (0.16) H16 1.0000 108.17 108.17 108.17 C16 - C1 C15 C11 O3 - Distance Angles C4 1.3476 (0.0023) C2 1.4540 (0.0023) 117.00 (0.16) O3 - C4 O4 - Distance Angles C4 1.2049 (0.0023) O4 - O17 - Distance Angles C1 1.4403 (0.0021) C10 1.4429 (0.0021) 110.14 (0.13) O17 - C1 FMAP and GRID set by program FMAP 2 3 29 GRID -0.962 -2 -2 0.962 2 2 R1 = 0.0479 for 1796 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.20 at 0.6718 0.4163 -0.0003 [ 1.18 A from H10 ] Deepest hole -0.21 at 0.4702 0.7442 0.1247 [ 1.18 A from C14 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2281 / 16899 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6718 0.4163 -0.0003 1.00000 0.05 0.20 1.18 H10 2.00 H7 2.08 H8 2.13 C10 Q2 1 0.3107 0.4017 0.0016 1.00000 0.05 0.19 0.88 H9B 1.35 C9 1.80 H10 1.93 C10 Q3 1 0.3743 0.1792 0.2619 1.00000 0.05 0.18 0.95 O4 1.87 C4 1.90 H1 2.30 H14A Q4 1 0.0883 0.5188 0.2476 1.00000 0.05 0.18 1.24 H2B 1.84 H5B 1.92 C2 2.09 O3 Q5 1 0.2317 0.3839 -0.0016 1.00000 0.05 0.18 0.66 H9B 1.34 C9 1.96 C8 2.11 H8 Q6 1 0.2563 0.7192 0.2431 1.00000 0.05 0.18 1.23 H15B 1.46 H5A 2.04 O4 2.09 H2B Q7 1 0.5463 0.2694 0.0084 1.00000 0.05 0.17 1.07 H8 1.85 C8 1.98 C8 2.10 H9B Q8 1 0.2442 0.8068 0.2429 1.00000 0.05 0.17 1.26 H15B 1.81 H2A 1.88 H5A 2.19 C15 Q9 1 0.7415 0.5640 -0.0091 1.00000 0.05 0.17 1.74 H10 1.75 H13A 1.76 H12B 2.30 H7 Q10 1 0.4116 0.5153 -0.0010 1.00000 0.05 0.17 1.39 H10 1.72 H9B 1.72 C10 2.02 H11 Q11 1 0.2131 0.1835 0.0086 1.00000 0.05 0.17 1.29 H8 1.39 C8 1.90 C7 2.06 H10 Q12 1 0.5049 0.4393 -0.0113 1.00000 0.05 0.16 1.30 H10 1.95 H9B 1.99 C10 2.02 H7 Q13 1 -0.0617 0.2283 0.2528 1.00000 0.05 0.16 1.41 H5A 1.68 H15B 1.91 C5 1.91 C4 Q14 1 0.0250 0.3467 -0.0065 1.00000 0.05 0.16 1.15 H9B 1.15 H8 1.85 C9 2.06 C8 Q15 1 0.6708 0.6567 0.0065 1.00000 0.05 0.16 0.68 H12B 1.50 C12 1.89 H12A 2.14 H10 Q16 1 0.4894 0.6519 -0.0091 1.00000 0.05 0.16 1.30 H12B 1.92 H11 1.96 C12 2.11 C11 Q17 1 0.6713 0.5979 -0.0107 1.00000 0.05 0.16 1.42 H12B 1.85 H10 1.90 H13A 2.14 C12 Q18 1 0.1651 0.5628 -0.0068 1.00000 0.05 0.16 1.60 H9B 1.64 H11 1.79 H13B 1.88 H13A Q19 1 0.2097 0.1313 0.2492 1.00000 0.05 0.16 1.34 O4 1.67 C4 1.92 H5B 2.08 C5 Q20 1 0.1586 0.6170 0.2479 1.00000 0.05 0.16 1.33 H2B 1.41 H5A 1.96 H5B 1.99 C5 Shortest distances between peaks (including symmetry equivalents) 2 5 0.46 9 17 0.51 15 17 0.74 6 8 0.91 1 12 0.95 10 12 0.96 15 16 1.03 6 13 1.03 3 19 1.04 1 11 1.07 4 20 1.08 7 11 1.09 9 15 1.10 16 17 1.11 2 12 1.14 5 14 1.16 6 20 1.18 7 14 1.20 13 20 1.26 8 13 1.26 2 10 1.29 10 18 1.39 10 16 1.48 5 12 1.56 1 9 1.58 9 16 1.61 2 14 1.62 10 17 1.63 5 10 1.65 1 7 1.67 11 14 1.67 11 12 1.68 1 10 1.71 13 19 1.75 9 12 1.79 9 10 1.82 7 12 1.83 2 18 1.84 2 7 1.85 12 17 1.86 5 7 1.87 5 18 1.88 1 17 1.89 1 2 1.90 16 18 1.94 19 20 1.94 4 19 1.95 7 11 1.96 3 6 1.99 11 14 1.99 1 14 2.00 10 15 2.01 8 20 2.01 5 7 2.05 5 11 2.09 4 13 2.17 12 16 2.20 12 18 2.20 9 18 2.23 4 6 2.25 2 7 2.26 2 11 2.30 2 11 2.32 1 5 2.34 14 18 2.35 3 13 2.36 3 8 2.40 12 15 2.45 1 15 2.49 3 20 2.55 9 11 2.56 15 16 2.59 10 11 2.60 6 19 2.62 17 18 2.62 1 16 2.62 5 11 2.63 7 10 2.65 7 14 2.66 10 14 2.68 7 7 2.69 9 14 2.69 12 14 2.70 1 7 2.75 2 16 2.76 2 17 2.79 15 18 2.79 2 14 2.80 4 8 2.81 1 14 2.83 2 9 2.83 5 14 2.84 15 18 2.90 11 17 2.91 3 4 2.95 12 14 2.99 11 11 3.00 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.55: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.61: Structure factors and derivatives 0.33: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src1140 finished at 14:09:55 Total CPU time: 1.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++