+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0664 started at 01:45:14 on 07-Jul-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0664 in C2/c CELL 0.71073 13.3991 8.2341 22.8014 90.000 96.356 90.000 ZERR 8.00 0.0005 0.0003 0.0008 0.000 0.002 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H O UNIT 136 112 8 V = 2500.20 F(000) = 992.0 Mu = 0.08 mm-1 Cell Wt = 1874.26 Rho = 1.245 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 20 SIZE 0.10 0.30 0.30 ACTA BOND $H WGHT 0.09250 1.05720 L.S. 10 TEMP -153.00 FVAR 0.41830 MOLE 1 C1 1 0.631228 0.343402 0.661145 11.00000 0.02839 0.02445 = 0.02180 0.00339 0.00426 0.00033 C2 1 0.591226 0.463304 0.693357 11.00000 0.03398 0.03214 = 0.02524 0.00365 0.00886 0.00726 AFIX 43 H2 2 0.521009 0.464432 0.696139 11.00000 -1.20000 AFIX 0 C3 1 0.651947 0.583762 0.722136 11.00000 0.04674 0.02959 = 0.02444 -0.00262 0.00826 0.00683 AFIX 43 H3 2 0.622846 0.665136 0.744398 11.00000 -1.20000 AFIX 0 C4 1 0.753000 0.584632 0.718296 11.00000 0.04489 0.02605 = 0.02339 -0.00280 0.00238 -0.00254 AFIX 43 H4 2 0.793991 0.665904 0.738323 11.00000 -1.20000 AFIX 0 C5 1 0.902186 0.467883 0.680990 11.00000 0.03327 0.03005 = 0.02639 0.00318 0.00019 -0.00932 AFIX 43 H5 2 0.941829 0.552357 0.699978 11.00000 -1.20000 AFIX 0 C6 1 0.946948 0.350989 0.650619 11.00000 0.02310 0.03960 = 0.03084 0.00554 0.00304 -0.00502 AFIX 43 H6 2 1.017407 0.353684 0.648756 11.00000 -1.20000 AFIX 0 C7 1 0.888214 0.225784 0.621912 11.00000 0.02569 0.02971 = 0.02949 0.00350 0.00675 0.00303 AFIX 43 H7 2 0.920343 0.143938 0.601414 11.00000 -1.20000 AFIX 0 C8 1 0.785693 0.219084 0.622815 11.00000 0.02571 0.02128 = 0.02188 0.00213 0.00400 -0.00005 C9 1 0.737082 0.339714 0.654671 11.00000 0.02688 0.01900 = 0.01920 0.00268 0.00300 -0.00043 C10 1 0.796968 0.465083 0.684635 11.00000 0.03354 0.02329 = 0.01880 0.00330 0.00096 -0.00296 C11 1 0.731904 0.080480 0.590711 11.00000 0.02452 0.02248 = 0.02373 -0.00114 0.00609 0.00141 C12 1 0.739464 -0.076023 0.614437 11.00000 0.03513 0.02539 = 0.02271 0.00229 0.00298 -0.00078 AFIX 43 H12 2 0.776622 -0.093047 0.651885 11.00000 -1.20000 AFIX 0 C13 1 0.693520 -0.206964 0.584130 11.00000 0.03728 0.02103 = 0.02905 0.00013 0.00742 -0.00027 AFIX 43 H13 2 0.699232 -0.312032 0.601388 11.00000 -1.20000 AFIX 0 C14 1 0.639069 -0.187281 0.528773 11.00000 0.02601 0.02622 = 0.02936 -0.00636 0.00948 -0.00136 C15 1 0.631743 -0.031478 0.504688 11.00000 0.02820 0.03321 = 0.02506 -0.00043 0.00254 -0.00109 AFIX 43 H15 2 0.595222 -0.015083 0.467014 11.00000 -1.20000 AFIX 0 C16 1 0.677116 0.099923 0.535044 11.00000 0.03117 0.02448 = 0.02782 0.00314 0.00341 0.00282 AFIX 43 H16 2 0.670969 0.204998 0.517816 11.00000 -1.20000 AFIX 0 C17 1 0.589130 -0.330768 0.497139 11.00000 0.03534 0.03179 = 0.03933 -0.01062 0.00694 -0.00806 AFIX 137 H17A 2 0.635641 -0.422994 0.499795 11.00000 -1.50000 H17B 2 0.570430 -0.302997 0.455581 11.00000 -1.50000 H17C 2 0.528742 -0.359910 0.515406 11.00000 -1.50000 AFIX 0 O1 3 0.564829 0.229545 0.637590 11.00000 0.02654 0.03576 = 0.04207 -0.00822 0.00974 -0.00397 AFIX 147 H1 2 0.595240 0.160105 0.619248 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2009src0664 in C2/c C 0.770 H 0.320 O 0.660 C1 - O1 C2 C9 C2 - C1 C3 C3 - C4 C2 C4 - C3 C10 C5 - C6 C10 C6 - C5 C7 C7 - C8 C6 C8 - C7 C9 C11 C9 - C8 C10 C1 C10 - C4 C5 C9 C11 - C12 C16 C8 C12 - C13 C11 C13 - C12 C14 C14 - C15 C13 C17 C15 - C16 C14 C16 - C15 C11 C17 - C14 O1 - C1 18358 Reflections read, of which 796 rejected -17 =< h =< 17, -10 =< k =< 10, -29 =< l =< 29, Max. 2-theta = 54.95 0 Systematic absence violations 0 Inconsistent equivalents 2874 Unique reflections, of which 0 suppressed R(int) = 0.0602 R(sigma) = 0.0440 Friedel opposites merged Maximum memory for data reduction = 1715 / 34243 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 = 2180 / 204628 wR2 = 0.1650 before cycle 1 for 2874 data and 165 / 165 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0925 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41961 0.00143 0.915 OSF Mean shift/su = 0.286 Maximum = 0.915 for OSF Max. shift = 0.006 A for H1 Max. dU = 0.000 for C17 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2180 / 204628 wR2 = 0.1640 before cycle 2 for 2874 data and 165 / 165 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0925 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.42001 0.00142 0.285 OSF Mean shift/su = 0.105 Maximum = -0.322 for x C4 Max. shift = 0.003 A for H1 Max. dU = 0.000 for C17 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2180 / 204628 wR2 = 0.1638 before cycle 3 for 2874 data and 165 / 165 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0925 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.42009 0.00142 0.053 OSF Mean shift/su = 0.010 Maximum = 0.078 for tors H17A Max. shift = 0.001 A for H17C Max. dU = 0.000 for C4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2180 / 204628 wR2 = 0.1638 before cycle 4 for 2874 data and 165 / 165 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0925 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.42009 0.00142 0.005 OSF Mean shift/su = 0.002 Maximum = 0.045 for tors H17A Max. shift = 0.001 A for H17C Max. dU = 0.000 for C13 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2180 / 204628 wR2 = 0.1638 before cycle 5 for 2874 data and 165 / 165 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0925 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.42010 0.00142 0.001 OSF Mean shift/su = 0.001 Maximum = 0.026 for tors H17A Max. shift = 0.000 A for H17C Max. dU = 0.000 for C5 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2180 / 204628 wR2 = 0.1638 before cycle 6 for 2874 data and 165 / 165 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0925 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.42010 0.00142 0.000 OSF Mean shift/su = 0.000 Maximum = 0.015 for tors H17A Max. shift = 0.000 A for H17C Max. dU = 0.000 for C5 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2180 / 204628 wR2 = 0.1638 before cycle 7 for 2874 data and 165 / 165 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0925 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.42010 0.00142 0.001 OSF Mean shift/su = 0.000 Maximum = 0.009 for tors H17A Max. shift = 0.000 A for H17C Max. dU = 0.000 for C5 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2180 / 204628 wR2 = 0.1638 before cycle 8 for 2874 data and 165 / 165 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0925 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.42010 0.00142 0.000 OSF Mean shift/su = 0.000 Maximum = 0.005 for tors H17A Max. shift = 0.000 A for H17B Max. dU = 0.000 for C17 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2180 / 204628 wR2 = 0.1638 before cycle 9 for 2874 data and 165 / 165 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0925 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.42010 0.00142 0.000 OSF Mean shift/su = 0.000 Maximum = 0.003 for tors H17A Max. shift = 0.000 A for H17B Max. dU = 0.000 for C13 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2180 / 204628 wR2 = 0.1638 before cycle 10 for 2874 data and 165 / 165 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0925 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.42010 0.00142 0.000 OSF Mean shift/su = 0.000 Maximum = 0.002 for tors H17A Max. shift = 0.000 A for H17A Max. dU = 0.000 for C10 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.5211 0.4641 0.6961 43 0.950 0.000 C2 C1 C3 H3 0.6228 0.6652 0.7443 43 0.950 0.000 C3 C4 C2 H4 0.7938 0.6657 0.7383 43 0.950 0.000 C4 C3 C10 H5 0.9419 0.5521 0.7000 43 0.950 0.000 C5 C6 C10 H6 1.0174 0.3536 0.6488 43 0.950 0.000 C6 C5 C7 H7 0.9202 0.1440 0.6014 43 0.950 0.000 C7 C8 C6 H12 0.7763 -0.0930 0.6519 43 0.950 0.000 C12 C13 C11 H13 0.6995 -0.3118 0.6013 43 0.950 0.000 C13 C12 C14 H15 0.5954 -0.0151 0.4671 43 0.950 0.000 C15 C16 C14 H16 0.6711 0.2048 0.5178 43 0.950 0.000 C16 C15 C11 H17A 0.6355 -0.4231 0.4999 137 0.980 0.000 C17 C14 H17A H17B 0.5708 -0.3031 0.4555 137 0.980 0.000 C17 C14 H17A H17C 0.5285 -0.3595 0.5152 137 0.980 0.000 C17 C14 H17A H1 0.5954 0.1596 0.6196 147 0.840 0.000 O1 C1 H1 2009src0664 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.63120 0.34360 0.66115 1.00000 0.02874 0.02478 0.02218 0.00346 0.00381 0.00010 0.02516 0.00293 0.00012 0.00020 0.00007 0.00000 0.00089 0.00084 0.00077 0.00067 0.00066 0.00069 0.00038 C2 0.59131 0.46311 0.69332 1.00000 0.03414 0.03288 0.02465 0.00383 0.00882 0.00724 0.03014 0.00325 0.00013 0.00021 0.00007 0.00000 0.00095 0.00096 0.00083 0.00073 0.00073 0.00075 0.00041 H2 0.52111 0.46409 0.69614 1.00000 0.03617 0.00000 0.00000 C3 0.65196 0.58376 0.72209 1.00000 0.04624 0.03040 0.02418 -0.00233 0.00772 0.00684 0.03332 0.00329 0.00014 0.00022 0.00007 0.00000 0.00114 0.00097 0.00083 0.00073 0.00076 0.00081 0.00044 H3 0.62285 0.66521 0.74431 1.00000 0.03999 0.00000 0.00000 C4 0.75283 0.58447 0.71825 1.00000 0.04573 0.02660 0.02344 -0.00250 0.00218 -0.00243 0.03205 0.00318 0.00014 0.00021 0.00007 0.00000 0.00112 0.00090 0.00083 0.00070 0.00075 0.00079 0.00043 H4 0.79382 0.66573 0.73828 1.00000 0.03846 0.00000 0.00000 C5 0.90222 0.46769 0.68100 1.00000 0.03308 0.02996 0.02703 0.00372 -0.00025 -0.00880 0.03029 0.00314 0.00013 0.00022 0.00007 0.00000 0.00095 0.00095 0.00084 0.00073 0.00071 0.00075 0.00041 H5 0.94190 0.55210 0.70001 1.00000 0.03635 0.00000 0.00000 C6 0.94690 0.35097 0.65066 1.00000 0.02309 0.03976 0.03064 0.00572 0.00268 -0.00502 0.03118 0.00317 0.00013 0.00023 0.00007 0.00000 0.00085 0.00103 0.00089 0.00079 0.00069 0.00075 0.00042 H6 1.01737 0.35359 0.64882 1.00000 0.03742 0.00000 0.00000 C7 0.88810 0.22582 0.62192 1.00000 0.02620 0.03027 0.02949 0.00405 0.00691 0.00305 0.02837 0.00316 0.00013 0.00021 0.00007 0.00000 0.00088 0.00091 0.00086 0.00071 0.00069 0.00071 0.00040 H7 0.92021 0.14398 0.60141 1.00000 0.03404 0.00000 0.00000 C8 0.78569 0.21914 0.62281 1.00000 0.02644 0.02153 0.02164 0.00274 0.00415 0.00000 0.02309 0.00291 0.00012 0.00019 0.00007 0.00000 0.00085 0.00083 0.00075 0.00063 0.00064 0.00064 0.00037 C9 0.73710 0.33973 0.65469 1.00000 0.02739 0.01929 0.01868 0.00327 0.00298 -0.00042 0.02175 0.00279 0.00012 0.00019 0.00006 0.00000 0.00085 0.00077 0.00072 0.00061 0.00062 0.00064 0.00036 C10 0.79686 0.46508 0.68464 1.00000 0.03381 0.02318 0.01893 0.00399 0.00083 -0.00271 0.02546 0.00289 0.00013 0.00020 0.00006 0.00000 0.00093 0.00083 0.00074 0.00065 0.00065 0.00069 0.00039 C11 0.73182 0.08046 0.59069 1.00000 0.02484 0.02274 0.02364 -0.00091 0.00635 0.00112 0.02346 0.00289 0.00012 0.00019 0.00007 0.00000 0.00084 0.00085 0.00078 0.00064 0.00064 0.00065 0.00038 C12 0.73932 -0.07597 0.61442 1.00000 0.03572 0.02614 0.02271 0.00184 0.00307 -0.00095 0.02820 0.00307 0.00013 0.00020 0.00007 0.00000 0.00097 0.00091 0.00079 0.00067 0.00069 0.00073 0.00040 H12 0.77632 -0.09296 0.65192 1.00000 0.03384 0.00000 0.00000 C13 0.69361 -0.20675 0.58410 1.00000 0.03702 0.02075 0.02929 0.00017 0.00728 -0.00016 0.02875 0.00309 0.00013 0.00020 0.00007 0.00000 0.00098 0.00085 0.00088 0.00068 0.00074 0.00069 0.00041 H13 0.69951 -0.31184 0.60133 1.00000 0.03450 0.00000 0.00000 C14 0.63907 -0.18726 0.52877 1.00000 0.02539 0.02683 0.02909 -0.00575 0.00927 -0.00104 0.02664 0.00302 0.00013 0.00020 0.00007 0.00000 0.00085 0.00088 0.00084 0.00069 0.00068 0.00068 0.00039 C15 0.63186 -0.03153 0.50476 1.00000 0.02784 0.03362 0.02533 -0.00065 0.00243 -0.00115 0.02897 0.00304 0.00013 0.00021 0.00007 0.00000 0.00089 0.00097 0.00081 0.00073 0.00068 0.00072 0.00041 H15 0.59536 -0.01509 0.46708 1.00000 0.03476 0.00000 0.00000 C16 0.67718 0.09978 0.53505 1.00000 0.03144 0.02456 0.02744 0.00347 0.00364 0.00287 0.02778 0.00309 0.00013 0.00021 0.00007 0.00000 0.00092 0.00086 0.00083 0.00068 0.00070 0.00069 0.00040 H16 0.67110 0.20480 0.51778 1.00000 0.03334 0.00000 0.00000 C17 0.58913 -0.33072 0.49711 1.00000 0.03589 0.03261 0.04000 -0.01035 0.00740 -0.00775 0.03593 0.00319 0.00014 0.00023 0.00008 0.00000 0.00101 0.00100 0.00101 0.00083 0.00081 0.00080 0.00045 H17A 0.63550 -0.42314 0.49995 1.00000 0.05389 0.00000 0.00000 H17B 0.57079 -0.30311 0.45550 1.00000 0.05389 0.00000 0.00000 H17C 0.52852 -0.35950 0.51522 1.00000 0.05389 0.00000 0.00000 O1 0.56484 0.22958 0.63758 1.00000 0.02669 0.03607 0.04258 -0.00851 0.00971 -0.00413 0.03467 0.00214 0.00009 0.00015 0.00006 0.00000 0.00067 0.00074 0.00076 0.00058 0.00056 0.00054 0.00035 H1 0.59542 0.15958 0.61959 1.00000 0.05201 0.00000 0.00000 Final Structure Factor Calculation for 2009src0664 in C2/c Total number of l.s. parameters = 165 Maximum vector length = 511 Memory required = 2015 / 21973 wR2 = 0.1638 before cycle 11 for 2874 data and 0 / 165 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0925 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0553 for 2077 Fo > 4sig(Fo) and 0.0821 for all 2874 data wR2 = 0.1638, GooF = S = 1.046, Restrained GooF = 1.046 for all data Occupancy sum of asymmetric unit = 18.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0289 0.0270 0.0196 C1 0.0425 0.0265 0.0214 C2 0.0489 0.0300 0.0211 C3 0.0463 0.0278 0.0220 C4 0.0429 0.0257 0.0223 C5 0.0439 0.0283 0.0213 C6 0.0358 0.0261 0.0232 C7 0.0268 0.0239 0.0186 C8 0.0274 0.0223 0.0156 C9 0.0354 0.0244 0.0165 C10 0.0276 0.0234 0.0194 C11 0.0359 0.0269 0.0218 C12 0.0381 0.0274 0.0207 C13 0.0360 0.0252 0.0187 C14 0.0339 0.0278 0.0252 C15 0.0328 0.0286 0.0219 C16 0.0500 0.0339 0.0239 C17 0.0499 0.0302 0.0239 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.016 0.024 0.034 0.043 0.055 0.073 0.100 0.148 1.000 Number in group 329. 279. 276. 294. 267. 284. 283. 286. 290. 286. GooF 0.935 0.988 1.041 1.093 1.156 1.080 1.087 1.023 0.921 1.136 K 3.620 1.302 0.979 1.011 0.982 0.986 0.995 1.000 1.026 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.65 inf Number in group 292. 289. 286. 286. 287. 287. 289. 281. 288. 289. GooF 0.906 1.022 0.975 0.926 1.011 1.000 1.033 0.816 1.059 1.545 K 1.078 1.065 1.062 1.025 1.021 1.027 1.030 1.046 1.050 0.979 R1 0.214 0.179 0.160 0.118 0.103 0.076 0.055 0.041 0.050 0.046 Recommended weighting scheme: WGHT 0.0865 1.2204 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 3925.54 10848.29 7.82 0.438 5.67 -1 1 1 951.86 2705.73 7.39 0.219 6.80 -1 1 2 629.67 1335.62 5.81 0.154 6.12 -4 2 8 33.04 5.59 4.98 0.010 2.00 3 1 11 70.51 24.71 4.96 0.021 1.75 7 5 9 18.26 75.02 4.61 0.036 1.09 0 4 3 116.39 60.02 4.14 0.033 1.99 -3 1 10 41.39 13.91 4.12 0.016 2.05 0 2 9 128.97 65.83 4.11 0.034 2.15 -1 3 6 386.45 247.75 3.97 0.066 2.21 6 0 8 98.77 49.44 3.48 0.030 1.66 -6 6 10 28.37 64.98 3.36 0.034 1.06 6 2 0 16.44 1.08 3.30 0.004 1.95 10 0 6 -3.60 29.91 3.28 0.023 1.21 -12 0 8 226.45 362.73 3.26 0.080 1.07 3 3 8 25.61 53.20 3.06 0.031 1.75 -6 2 2 36.59 15.78 2.99 0.017 1.96 -12 0 4 668.63 938.84 2.98 0.129 1.11 5 1 9 114.23 71.19 2.95 0.035 1.70 -8 0 2 216.86 145.06 2.92 0.051 1.67 2 4 21 122.43 202.31 2.89 0.060 0.93 1 1 1 301.13 445.06 2.87 0.089 6.58 -14 2 16 34.40 104.45 2.84 0.043 0.82 0 0 16 251.18 175.14 2.83 0.056 1.42 5 1 2 110.38 164.10 2.79 0.054 2.42 5 7 11 139.91 69.48 2.78 0.035 0.94 -2 6 7 14.40 45.52 2.77 0.028 1.25 8 2 1 39.19 18.03 2.76 0.018 1.53 2 4 1 9.59 25.89 2.74 0.021 1.95 -2 2 7 39.51 18.14 2.71 0.018 2.45 7 3 20 227.29 346.88 2.71 0.078 0.88 5 1 15 18.81 1.12 2.69 0.004 1.24 3 5 15 168.98 242.05 2.67 0.065 1.06 -5 1 9 945.66 726.21 2.64 0.113 1.89 -2 8 16 48.19 119.41 2.59 0.046 0.83 11 5 1 94.18 157.30 2.59 0.053 0.97 -1 9 11 162.72 80.88 2.58 0.038 0.84 7 3 3 293.29 215.40 2.56 0.062 1.50 -11 1 23 10.20 69.96 2.56 0.035 0.81 3 9 9 319.28 206.94 2.54 0.060 0.84 2 4 2 67.62 41.43 2.52 0.027 1.93 -10 4 4 6.66 29.41 2.51 0.023 1.12 4 10 5 644.71 448.85 2.48 0.089 0.78 2 8 14 144.52 62.67 2.47 0.033 0.85 15 1 5 716.67 511.15 2.47 0.095 0.85 -16 2 9 153.97 88.57 2.47 0.040 0.80 9 5 15 70.53 11.31 2.46 0.014 0.86 4 4 7 90.93 134.25 2.46 0.049 1.50 12 2 13 32.90 90.76 2.44 0.040 0.87 -5 3 3 423.95 324.68 2.44 0.076 1.89 Bond lengths and angles C1 - Distance Angles O1 1.3620 (0.0020) C2 1.3706 (0.0023) 115.46 (0.15) C9 1.4431 (0.0023) 123.42 (0.14) 121.10 (0.16) C1 - O1 C2 C2 - Distance Angles C1 1.3706 (0.0023) C3 1.3999 (0.0025) 121.31 (0.16) H2 0.9500 119.34 119.34 C2 - C1 C3 C3 - Distance Angles C4 1.3640 (0.0026) C2 1.3999 (0.0025) 120.06 (0.16) H3 0.9500 119.97 119.97 C3 - C4 C2 C4 - Distance Angles C3 1.3640 (0.0026) C10 1.4148 (0.0023) 120.49 (0.16) H4 0.9500 119.75 119.75 C4 - C3 C10 C5 - Distance Angles C6 1.3610 (0.0025) C10 1.4234 (0.0024) 120.92 (0.16) H5 0.9500 119.54 119.54 C5 - C6 C10 C6 - Distance Angles C5 1.3610 (0.0025) C7 1.4135 (0.0025) 119.77 (0.16) H6 0.9500 120.12 120.12 C6 - C5 C7 C7 - Distance Angles C8 1.3756 (0.0023) C6 1.4135 (0.0025) 121.87 (0.16) H7 0.9500 119.06 119.06 C7 - C8 C6 C8 - Distance Angles C7 1.3756 (0.0023) C9 1.4294 (0.0022) 119.41 (0.15) C11 1.4981 (0.0022) 116.79 (0.14) 123.79 (0.14) C8 - C7 C9 C9 - Distance Angles C8 1.4294 (0.0022) C10 1.4325 (0.0022) 118.75 (0.14) C1 1.4431 (0.0023) 125.15 (0.15) 116.07 (0.14) C9 - C8 C10 C10 - Distance Angles C4 1.4148 (0.0023) C5 1.4234 (0.0024) 119.79 (0.16) C9 1.4325 (0.0022) 120.95 (0.15) 119.26 (0.15) C10 - C4 C5 C11 - Distance Angles C12 1.3965 (0.0022) C16 1.4018 (0.0023) 117.60 (0.15) C8 1.4981 (0.0022) 120.24 (0.14) 122.07 (0.14) C11 - C12 C16 C12 - Distance Angles C13 1.3852 (0.0024) C11 1.3965 (0.0022) 120.98 (0.15) H12 0.9500 119.51 119.51 C12 - C13 C11 C13 - Distance Angles C12 1.3852 (0.0024) C14 1.3955 (0.0025) 121.34 (0.15) H13 0.9500 119.33 119.33 C13 - C12 C14 C14 - Distance Angles C15 1.3934 (0.0024) C13 1.3955 (0.0025) 117.88 (0.15) C17 1.5025 (0.0024) 121.80 (0.16) 120.32 (0.16) C14 - C15 C13 C15 - Distance Angles C16 1.3863 (0.0024) C14 1.3934 (0.0024) 120.96 (0.15) H15 0.9500 119.52 119.52 C15 - C16 C14 C16 - Distance Angles C15 1.3863 (0.0024) C11 1.4018 (0.0023) 121.23 (0.16) H16 0.9500 119.39 119.39 C16 - C15 C11 C17 - Distance Angles C14 1.5025 (0.0024) H17A 0.9800 109.47 H17B 0.9800 109.47 109.47 H17C 0.9800 109.47 109.47 109.47 C17 - C14 H17A H17B O1 - Distance Angles C1 1.3620 (0.0020) H1 0.8400 109.47 O1 - C1 FMAP and GRID set by program FMAP 2 2 12 GRID -2.778 24 -2 2.778 1 2 R1 = 0.0821 for 2874 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.27 at 0.0791 0.0721 0.5295 [ 0.91 A from H17C ] Deepest hole -0.28 at 0.7345 0.1990 0.6330 [ 0.77 A from C8 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2782 / 27651 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5791 -0.4279 0.5295 1.00000 0.05 0.27 0.91 H17C 1.07 H17A 1.11 C17 1.97 H17B Q2 1 0.5007 -0.2898 0.4822 1.00000 0.05 0.26 0.99 H17C 1.18 H17B 1.24 C17 2.11 H17A Q3 1 0.6653 0.0873 0.5883 1.00000 0.05 0.24 0.89 C11 1.25 C16 1.37 H1 1.74 C12 Q4 1 0.6352 -0.3914 0.4689 1.00000 0.05 0.23 0.75 H17A 1.06 C17 1.14 H17B 1.89 H17C Q5 1 0.9584 0.5645 0.7634 1.00000 0.05 0.20 1.44 H5 1.50 H5 2.10 C5 2.28 C5 Q6 1 0.7793 0.4979 0.7095 1.00000 0.05 0.19 0.69 C10 0.83 C4 1.53 H4 1.85 C9 Q7 1 0.8394 0.6391 0.7303 1.00000 0.05 0.17 0.69 H4 1.25 C4 1.76 H5 1.82 C10 Q8 1 0.6147 0.3742 0.6931 1.00000 0.05 0.17 0.80 C2 0.82 C1 1.46 H2 1.81 O1 Q9 1 0.8995 0.6828 0.7461 1.00000 0.05 0.16 1.41 H4 1.65 H5 2.16 C4 2.31 C5 Q10 1 0.6176 -0.0981 0.5225 1.00000 0.05 0.16 0.72 C15 0.80 C14 1.44 H15 1.82 C16 Q11 1 0.8623 0.5462 0.7177 1.00000 0.05 0.16 1.18 H5 1.23 C5 1.28 C10 1.46 H4 Q12 1 0.4803 0.4228 0.7060 1.00000 0.05 0.15 0.70 H2 1.58 C2 2.26 H2 2.45 C1 Q13 1 0.6266 -0.0471 0.4497 1.00000 0.05 0.15 0.66 H15 1.26 C15 2.13 C14 2.25 H17B Q14 1 0.9536 0.6070 0.7160 1.00000 0.05 0.15 0.59 H5 1.52 C5 2.29 H5 2.31 H4 Q15 1 0.6724 0.2411 0.6278 1.00000 0.05 0.15 1.23 H1 1.29 C9 1.30 C1 1.49 O1 Q16 1 1.0000 0.6876 0.7500 0.50000 0.05 0.15 1.72 H5 2.62 H2 2.65 C5 2.75 H4 Q17 1 0.7592 0.4143 0.6632 1.00000 0.05 0.15 0.70 C9 0.78 C10 1.81 C1 1.89 C4 Q18 1 0.5917 0.7227 0.7598 1.00000 0.05 0.14 0.74 H3 1.69 C3 2.41 C6 2.42 C5 Q19 1 0.8435 0.6042 0.7815 1.00000 0.05 0.14 1.24 H4 1.79 C4 2.34 O1 2.36 H1 Q20 1 1.0172 0.6609 0.7380 1.00000 0.05 0.14 1.54 H5 1.71 H5 2.48 C5 2.51 O1 Shortest distances between peaks (including symmetry equivalents) 16 20 0.44 20 20 0.75 5 20 0.86 7 11 0.88 7 9 0.92 14 20 1.04 5 14 1.13 9 20 1.15 14 16 1.15 14 20 1.16 6 11 1.18 7 19 1.20 5 16 1.21 9 14 1.22 6 17 1.26 5 14 1.27 5 9 1.29 5 20 1.30 11 14 1.33 9 19 1.33 5 5 1.33 9 16 1.34 9 11 1.36 6 7 1.46 3 15 1.55 5 11 1.57 11 19 1.58 9 20 1.62 7 14 1.62 5 19 1.67 1 4 1.67 10 13 1.73 5 7 1.80 1 2 1.82 14 14 1.87 8 12 1.90 15 17 1.96 6 19 1.97 7 20 1.98 12 12 2.02 19 20 2.02 2 4 2.04 11 20 2.04 11 17 2.06 8 15 2.07 8 9 2.12 8 17 2.15 9 14 2.15 5 9 2.17 12 16 2.18 7 16 2.19 3 10 2.19 14 19 2.21 11 16 2.24 11 20 2.28 6 9 2.30 12 20 2.31 2 10 2.34 8 19 2.35 7 20 2.38 15 19 2.39 16 19 2.39 5 11 2.40 6 8 2.42 18 18 2.45 8 20 2.48 9 12 2.48 6 14 2.49 12 20 2.51 7 17 2.56 1 2 2.56 8 16 2.62 5 6 2.63 7 8 2.63 12 14 2.64 1 1 2.66 19 20 2.67 9 9 2.68 9 12 2.70 14 19 2.71 4 10 2.73 5 7 2.77 2 13 2.77 11 18 2.77 1 10 2.77 8 12 2.78 11 14 2.79 12 18 2.79 4 13 2.87 6 18 2.89 7 14 2.92 5 18 2.93 5 8 2.94 17 18 2.96 5 19 2.97 3 19 2.99 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 0.02: 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. 0.67: 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 0.75: Structure factors and derivatives 0.91: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.16: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0664 finished at 01:45:17 Total CPU time: 2.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++