+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0078p1 started at 12:32:10 on 06-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0078p1 in P1 CELL 0.71073 6.1782 7.5786 8.0969 100.526 91.585 107.060 ZERR 1.00 0.0003 0.0003 0.0003 0.002 0.002 0.002 LATT -1 SFAC C H N O UNIT 12 25 1 5 V = 355.00 F(000) = 144.0 Mu = 0.09 mm-1 Cell Wt = 263.33 Rho = 1.232 MERG 4 OMIT -3.00 55.00 SHEL 7 0.77 HTAB O2 O1B HTAB N25 O1B EQIV_$1 x-1, y, z HTAB O2 O4B_$1 HTAB N25 O1A_$1 EQIV_$2 x, y-1, z HTAB O4A O1A_$2 EQIV_$3 x, y+1, z HTAB N25 O2_$3 FMAP 2 PLAN 10 SIZE 0.04 0.10 0.10 ACTA BOND $H WGHT 0.02350 0.13060 L.S. 4 TEMP -153.00 FVAR 2.14862 MOLE 1 C1 1 0.887975 0.362772 0.632484 11.00000 0.02180 0.01677 = 0.01641 0.00219 0.00170 0.00612 C2 1 0.933635 0.186134 0.671539 11.00000 0.01719 0.01858 = 0.02553 0.00796 0.00212 0.00472 AFIX 13 H2 2 1.035709 0.223814 0.778263 11.00000 -1.20000 AFIX 0 C3 1 1.053374 0.098376 0.531762 11.00000 0.02688 0.01643 = 0.02437 0.00641 0.00569 0.00746 AFIX 23 H3A 2 0.953710 0.055678 0.425192 11.00000 -1.20000 H3B 2 1.194930 0.193121 0.513435 11.00000 -1.20000 AFIX 0 C4 1 1.108941 -0.067909 0.582201 11.00000 0.01794 0.01557 = 0.02486 0.00393 0.00514 0.00444 O1A 4 1.060608 0.497397 0.618810 11.00000 0.02020 0.01539 = 0.03216 0.00720 0.00212 0.00430 O1B 4 0.685853 0.361729 0.619984 11.00000 0.01964 0.01911 = 0.02744 0.00835 0.00360 0.00754 O2 4 0.729226 0.051734 0.696682 11.00000 0.01983 0.02189 = 0.04889 0.01781 0.00961 0.00699 AFIX 147 H2A 2 0.617802 0.085529 0.669002 11.00000 -1.50000 AFIX 0 O4A 4 0.973585 -0.231996 0.504340 11.00000 0.03096 0.01512 = 0.03757 0.00497 -0.00822 0.00636 AFIX 147 H4A 2 1.005628 -0.317899 0.542700 11.00000 -1.50000 AFIX 0 O4B 4 1.260217 -0.047958 0.688501 11.00000 0.02372 0.02013 = 0.03794 0.00649 -0.00577 0.00323 MOLE 2 C21 1 0.273896 0.244518 1.124578 11.00000 0.02650 0.02483 = 0.02623 0.01092 0.00706 0.00494 AFIX 137 H21A 2 0.278656 0.159963 1.018514 11.00000 -1.50000 H21B 2 0.126888 0.269332 1.125987 11.00000 -1.50000 H21C 2 0.293868 0.185344 1.219514 11.00000 -1.50000 AFIX 0 C22 1 0.465732 0.431085 1.139823 11.00000 0.02305 0.02429 = 0.01845 0.00431 0.00182 0.00671 C23 1 0.438136 0.496782 0.973001 11.00000 0.01671 0.01767 = 0.01897 0.00336 0.00151 0.00439 AFIX 23 H23A 2 0.467389 0.402011 0.882153 11.00000 -1.20000 H23B 2 0.275735 0.487548 0.954841 11.00000 -1.20000 AFIX 0 C24 1 0.575669 0.691209 0.941793 11.00000 0.01916 0.01914 = 0.01993 0.00356 0.00162 0.00550 C26 1 0.436057 0.567130 1.296664 11.00000 0.03605 0.03034 = 0.02020 0.00133 0.00250 0.01017 AFIX 137 H26A 2 0.296098 0.599571 1.278609 11.00000 -1.50000 H26B 2 0.566255 0.681885 1.316966 11.00000 -1.50000 H26C 2 0.426867 0.506816 1.394581 11.00000 -1.50000 AFIX 0 C27 1 0.692155 0.389596 1.162962 11.00000 0.02735 0.02776 = 0.02963 0.00887 -0.00201 0.01012 AFIX 137 H27A 2 0.688103 0.323078 1.256420 11.00000 -1.50000 H27B 2 0.816587 0.508302 1.188081 11.00000 -1.50000 H27C 2 0.716340 0.310918 1.059158 11.00000 -1.50000 AFIX 0 C28 1 0.486545 0.850149 1.024463 11.00000 0.02869 0.01692 = 0.02806 0.00466 0.00696 0.00788 AFIX 137 H28A 2 0.515073 0.871166 1.147222 11.00000 -1.50000 H28B 2 0.322786 0.816004 0.994094 11.00000 -1.50000 H28C 2 0.564396 0.965603 0.985295 11.00000 -1.50000 AFIX 0 C29 1 0.832404 0.744818 0.979276 11.00000 0.01768 0.02184 = 0.02882 0.00408 0.00124 0.00142 AFIX 137 H29A 2 0.906023 0.856865 0.933801 11.00000 -1.50000 H29B 2 0.886359 0.640241 0.926628 11.00000 -1.50000 H29C 2 0.869898 0.771817 1.101498 11.00000 -1.50000 AFIX 0 N25 3 0.534783 0.672919 0.751725 11.00000 0.01666 0.01568 = 0.02425 0.00526 0.00239 0.00393 AFIX 137 H25A 2 0.597805 0.586807 0.696764 11.00000 -1.50000 H25B 2 0.599499 0.786502 0.723494 11.00000 -1.50000 H25C 2 0.382680 0.634547 0.721641 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0078p1 in P1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - O2 C3 C1 C3 - C4 C2 C4 - O4B O4A C3 O1A - C1 O1B - C1 O2 - C2 O4A - C4 O4B - C4 C21 - C22 C22 - C26 C27 C21 C23 C23 - C24 C22 C24 - C28 C29 N25 C23 C26 - C22 C27 - C22 C28 - C24 C29 - C24 N25 - C24 Operators for generating equivalent atoms: $1 x-1, y, z $2 x, y-1, z $3 x, y+1, z Floating origin restraints generated 6086 Reflections read, of which 15 rejected -8 =< h =< 7, -9 =< k =< 8, -10 =< l =< 10, Max. 2-theta = 54.95 0 Systematic absence violations 0 Inconsistent equivalents 1616 Unique reflections, of which 0 suppressed R(int) = 0.0394 R(sigma) = 0.0359 Friedel opposites merged Maximum memory for data reduction = 2339 / 16137 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 = 2876 / 212805 wR2 = 0.0837 before cycle 1 for 1616 data and 171 / 171 parameters GooF = S = 1.101; Restrained GooF = 1.100 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0235 * P )^2 + 0.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.14862 0.00442 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.006 for U11 O1B Max. shift = 0.000 A for H2A Max. dU = 0.000 for O1A Least-squares cycle 2 Maximum vector length = 511 Memory required = 2876 / 212805 wR2 = 0.0837 before cycle 2 for 1616 data and 171 / 171 parameters GooF = S = 1.101; Restrained GooF = 1.100 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0235 * P )^2 + 0.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.14861 0.00442 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.002 for U11 O1B Max. shift = 0.000 A for H2A Max. dU = 0.000 for C29 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2876 / 212805 wR2 = 0.0837 before cycle 3 for 1616 data and 171 / 171 parameters GooF = S = 1.101; Restrained GooF = 1.099 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0235 * P )^2 + 0.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.14861 0.00442 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H2A Max. shift = 0.000 A for H2A Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2876 / 212805 wR2 = 0.0836 before cycle 4 for 1616 data and 171 / 171 parameters GooF = S = 1.101; Restrained GooF = 1.099 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0235 * P )^2 + 0.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.14861 0.00442 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C22 Max. shift = 0.000 A for H2A Max. dU = 0.000 for C1 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 1.0357 0.2238 0.7783 13 1.000 0.000 C2 O2 C3 C1 H3A 0.9537 0.0557 0.4252 23 0.990 0.000 C3 C4 C2 H3B 1.1949 0.1931 0.5134 23 0.990 0.000 C3 C4 C2 H2A 0.6178 0.0855 0.6690 147 0.840 0.000 O2 C2 H2A H4A 1.0056 -0.3179 0.5427 147 0.840 0.000 O4A C4 H4A H21A 0.2787 0.1600 1.0185 137 0.980 0.000 C21 C22 H21A H21B 0.1269 0.2693 1.1260 137 0.980 0.000 C21 C22 H21A H21C 0.2939 0.1853 1.2195 137 0.980 0.000 C21 C22 H21A H23A 0.4674 0.4020 0.8822 23 0.990 0.000 C23 C24 C22 H23B 0.2757 0.4875 0.9548 23 0.990 0.000 C23 C24 C22 H26A 0.2961 0.5996 1.2786 137 0.980 0.000 C26 C22 H26A H26B 0.5663 0.6819 1.3170 137 0.980 0.000 C26 C22 H26A H26C 0.4269 0.5068 1.3946 137 0.980 0.000 C26 C22 H26A H27A 0.6881 0.3231 1.2564 137 0.980 0.000 C27 C22 H27A H27B 0.8166 0.5083 1.1881 137 0.980 0.000 C27 C22 H27A H27C 0.7163 0.3109 1.0592 137 0.980 0.000 C27 C22 H27A H28A 0.5151 0.8712 1.1472 137 0.980 0.000 C28 C24 H28A H28B 0.3228 0.8160 0.9941 137 0.980 0.000 C28 C24 H28A H28C 0.5644 0.9656 0.9853 137 0.980 0.000 C28 C24 H28A H29A 0.9060 0.8569 0.9338 137 0.980 0.000 C29 C24 H29A H29B 0.8864 0.6402 0.9266 137 0.980 0.000 C29 C24 H29A H29C 0.8699 0.7718 1.1015 137 0.980 0.000 C29 C24 H29A H25A 0.5978 0.5868 0.6968 137 0.910 0.000 N25 C24 H25A H25B 0.5995 0.7865 0.7235 137 0.910 0.000 N25 C24 H25A H25C 0.3827 0.6345 0.7216 137 0.910 0.000 N25 C24 H25A 06skc0078p1 in P1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.88797 0.36277 0.63248 1.00000 0.02180 0.01677 0.01641 0.00219 0.00170 0.00612 0.01842 0.00481 0.00038 0.00032 0.00029 0.00000 0.00119 0.00112 0.00103 0.00087 0.00086 0.00095 0.00046 C2 0.93364 0.18613 0.67154 1.00000 0.01719 0.01858 0.02553 0.00796 0.00212 0.00472 0.02011 0.00520 0.00038 0.00033 0.00031 0.00000 0.00108 0.00120 0.00117 0.00095 0.00089 0.00090 0.00048 H2 1.03571 0.22381 0.77826 1.00000 0.02414 0.00000 0.00000 C3 1.05337 0.09838 0.53176 1.00000 0.02688 0.01643 0.02437 0.00641 0.00569 0.00746 0.02199 0.00551 0.00042 0.00034 0.00032 0.00000 0.00123 0.00118 0.00119 0.00093 0.00094 0.00096 0.00049 H3A 0.95371 0.05568 0.42519 1.00000 0.02639 0.00000 0.00000 H3B 1.19493 0.19312 0.51344 1.00000 0.02639 0.00000 0.00000 C4 1.10894 -0.06791 0.58220 1.00000 0.01794 0.01557 0.02486 0.00393 0.00514 0.00444 0.01955 0.00494 0.00038 0.00032 0.00030 0.00000 0.00110 0.00116 0.00120 0.00094 0.00094 0.00089 0.00048 O1A 1.06061 0.49740 0.61881 1.00000 0.02020 0.01539 0.03216 0.00720 0.00212 0.00430 0.02250 0.00344 0.00026 0.00023 0.00022 0.00000 0.00084 0.00085 0.00094 0.00071 0.00070 0.00068 0.00038 O1B 0.68585 0.36173 0.61998 1.00000 0.01963 0.01911 0.02744 0.00835 0.00360 0.00754 0.02118 0.00354 0.00027 0.00023 0.00021 0.00000 0.00080 0.00085 0.00091 0.00071 0.00067 0.00068 0.00036 O2 0.72923 0.05173 0.69668 1.00000 0.01983 0.02189 0.04889 0.01781 0.00961 0.00699 0.02850 0.00412 0.00029 0.00025 0.00026 0.00000 0.00084 0.00097 0.00118 0.00087 0.00080 0.00074 0.00043 H2A 0.61780 0.08554 0.66902 1.00000 0.04275 0.00000 0.00000 O4A 0.97358 -0.23200 0.50434 1.00000 0.03096 0.01512 0.03757 0.00497 -0.00822 0.00636 0.02828 0.00368 0.00030 0.00024 0.00024 0.00000 0.00098 0.00088 0.00107 0.00076 0.00080 0.00076 0.00043 H4A 1.00563 -0.31790 0.54270 1.00000 0.04242 0.00000 0.00000 O4B 1.26022 -0.04796 0.68850 1.00000 0.02372 0.02013 0.03794 0.00649 -0.00577 0.00323 0.02809 0.00371 0.00029 0.00025 0.00024 0.00000 0.00089 0.00090 0.00105 0.00076 0.00077 0.00072 0.00041 C21 0.27390 0.24452 1.12458 1.00000 0.02650 0.02483 0.02622 0.01092 0.00706 0.00494 0.02561 0.00563 0.00042 0.00037 0.00034 0.00000 0.00131 0.00136 0.00123 0.00103 0.00100 0.00107 0.00054 H21A 0.27866 0.15996 1.01852 1.00000 0.03841 0.00000 0.00000 H21B 0.12689 0.26933 1.12599 1.00000 0.03841 0.00000 0.00000 H21C 0.29387 0.18534 1.21952 1.00000 0.03841 0.00000 0.00000 C22 0.46573 0.43109 1.13982 1.00000 0.02304 0.02429 0.01845 0.00431 0.00182 0.00671 0.02203 0.00534 0.00042 0.00036 0.00030 0.00000 0.00114 0.00123 0.00110 0.00093 0.00089 0.00097 0.00049 C23 0.43814 0.49678 0.97300 1.00000 0.01671 0.01767 0.01896 0.00336 0.00151 0.00439 0.01800 0.00473 0.00038 0.00032 0.00028 0.00000 0.00101 0.00115 0.00108 0.00087 0.00082 0.00089 0.00045 H23A 0.46739 0.40201 0.88215 1.00000 0.02160 0.00000 0.00000 H23B 0.27574 0.48755 0.95484 1.00000 0.02160 0.00000 0.00000 C24 0.57567 0.69121 0.94179 1.00000 0.01916 0.01914 0.01993 0.00356 0.00162 0.00550 0.01953 0.00488 0.00038 0.00033 0.00029 0.00000 0.00110 0.00121 0.00113 0.00090 0.00089 0.00094 0.00048 C26 0.43606 0.56713 1.29666 1.00000 0.03605 0.03034 0.02020 0.00133 0.00250 0.01017 0.02933 0.00580 0.00048 0.00039 0.00032 0.00000 0.00145 0.00146 0.00119 0.00105 0.00103 0.00123 0.00058 H26A 0.29610 0.59957 1.27861 1.00000 0.04400 0.00000 0.00000 H26B 0.56625 0.68189 1.31697 1.00000 0.04400 0.00000 0.00000 H26C 0.42687 0.50682 1.39458 1.00000 0.04400 0.00000 0.00000 C27 0.69216 0.38960 1.16296 1.00000 0.02734 0.02776 0.02963 0.00887 -0.00201 0.01012 0.02753 0.00581 0.00045 0.00039 0.00034 0.00000 0.00130 0.00136 0.00135 0.00108 0.00106 0.00109 0.00056 H27A 0.68810 0.32308 1.25642 1.00000 0.04130 0.00000 0.00000 H27B 0.81659 0.50830 1.18808 1.00000 0.04130 0.00000 0.00000 H27C 0.71634 0.31092 1.05916 1.00000 0.04130 0.00000 0.00000 C28 0.48654 0.85015 1.02446 1.00000 0.02869 0.01692 0.02806 0.00467 0.00696 0.00788 0.02423 0.00549 0.00043 0.00035 0.00033 0.00000 0.00131 0.00117 0.00130 0.00099 0.00104 0.00103 0.00053 H28A 0.51507 0.87117 1.14722 1.00000 0.03635 0.00000 0.00000 H28B 0.32279 0.81600 0.99409 1.00000 0.03635 0.00000 0.00000 H28C 0.56440 0.96560 0.98530 1.00000 0.03635 0.00000 0.00000 C29 0.83240 0.74482 0.97928 1.00000 0.01768 0.02184 0.02881 0.00408 0.00124 0.00142 0.02393 0.00525 0.00040 0.00037 0.00033 0.00000 0.00109 0.00124 0.00128 0.00100 0.00094 0.00093 0.00051 H29A 0.90602 0.85687 0.93380 1.00000 0.03589 0.00000 0.00000 H29B 0.88636 0.64024 0.92663 1.00000 0.03589 0.00000 0.00000 H29C 0.86990 0.77181 1.10150 1.00000 0.03589 0.00000 0.00000 N25 0.53478 0.67292 0.75172 1.00000 0.01666 0.01568 0.02425 0.00526 0.00239 0.00393 0.01890 0.00409 0.00032 0.00027 0.00025 0.00000 0.00091 0.00098 0.00101 0.00077 0.00075 0.00078 0.00041 H25A 0.59781 0.58681 0.69676 1.00000 0.02834 0.00000 0.00000 H25B 0.59950 0.78650 0.72349 1.00000 0.02834 0.00000 0.00000 H25C 0.38268 0.63454 0.72164 1.00000 0.02834 0.00000 0.00000 Final Structure Factor Calculation for 06skc0078p1 in P1 Total number of l.s. parameters = 171 Maximum vector length = 511 Memory required = 2707 / 25046 wR2 = 0.0836 before cycle 5 for 1616 data and 2 / 171 parameters GooF = S = 1.101; Restrained GooF = 1.099 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0235 * P )^2 + 0.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0378 for 1540 Fo > 4sig(Fo) and 0.0407 for all 1616 data wR2 = 0.0836, GooF = S = 1.101, Restrained GooF = 1.099 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 18.00 for non-hydrogen and 25.00 for hydrogen atoms Principal mean square atomic displacements U 0.0219 0.0180 0.0154 C1 0.0266 0.0178 0.0160 C2 0.0291 0.0219 0.0150 C3 0.0265 0.0169 0.0152 C4 0.0323 0.0209 0.0143 O1A 0.0283 0.0193 0.0159 O1B 0.0512 0.0194 0.0149 O2 0.0470 0.0235 0.0143 O4A 0.0430 0.0225 0.0188 O4B 0.0308 0.0298 0.0162 C21 0.0247 0.0230 0.0184 C22 0.0192 0.0184 0.0164 C23 0.0202 0.0195 0.0189 C24 0.0362 0.0324 0.0194 C26 0.0341 0.0289 0.0196 C27 0.0330 0.0235 0.0162 C28 0.0293 0.0267 0.0158 C29 0.0243 0.0177 0.0147 N25 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.031 0.045 0.059 0.074 0.090 0.107 0.127 0.160 0.227 1.000 Number in group 168. 166. 162. 154. 166. 155. 160. 161. 161. 163. GooF 1.132 1.234 1.171 1.173 1.068 0.920 1.025 1.064 0.957 1.204 K 1.161 0.993 1.002 0.994 0.995 1.020 1.002 1.004 1.011 0.997 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.66 inf Number in group 167. 161. 162. 157. 162. 162. 162. 159. 162. 162. GooF 1.188 1.109 1.053 1.077 1.109 1.006 1.096 0.930 1.004 1.368 K 1.053 1.053 1.026 1.017 0.996 1.010 0.980 0.991 1.014 0.995 R1 0.091 0.081 0.076 0.064 0.054 0.039 0.034 0.026 0.020 0.024 Recommended weighting scheme: WGHT 0.0235 0.1306 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) -1 1 0 268.77 309.66 3.75 0.368 5.41 3 0 3 21.25 13.66 3.59 0.077 1.51 4 -6 5 24.29 34.85 3.53 0.123 0.96 0 0 7 12.65 7.29 3.51 0.056 1.13 -1 -2 7 0.67 2.81 3.35 0.035 1.12 -2 -6 6 2.76 8.02 3.20 0.059 0.88 2 7 2 8.19 2.34 3.10 0.032 0.83 -1 -3 1 349.14 304.52 3.03 0.365 2.03 0 -8 7 0.76 2.98 3.03 0.036 0.78 -4 1 0 50.54 41.83 3.00 0.135 1.54 4 -8 1 1.85 4.57 2.99 0.045 0.90 1 -1 2 12.38 8.71 2.91 0.062 3.31 0 1 1 654.86 726.41 2.90 0.563 4.83 -2 -5 2 0.69 2.65 2.84 0.034 1.17 0 -1 5 4.40 7.24 2.82 0.056 1.62 6 -6 4 8.54 4.11 2.79 0.042 0.84 0 4 0 40.53 32.22 2.75 0.119 1.77 1 2 0 220.69 196.21 2.73 0.293 2.70 -4 7 2 3.71 1.57 2.73 0.026 0.93 1 -2 2 99.63 86.93 2.72 0.195 2.87 1 0 2 413.24 455.86 2.71 0.446 3.16 -1 -8 6 0.29 2.42 2.67 0.033 0.78 -2 3 9 3.48 1.19 2.53 0.023 0.79 -2 5 7 5.42 9.73 2.53 0.065 0.83 2 -8 2 4.01 6.51 2.50 0.053 0.95 -1 2 0 105.12 118.31 2.48 0.227 3.55 -1 -7 2 2.65 1.11 2.48 0.022 0.97 0 -5 7 2.46 4.44 2.47 0.044 0.99 -3 2 1 61.60 53.52 2.44 0.153 1.92 4 -8 6 25.05 18.66 2.43 0.090 0.79 2 4 7 7.96 12.81 2.43 0.075 0.80 -3 6 2 40.97 48.54 2.42 0.146 1.09 2 5 4 4.95 8.11 2.37 0.060 0.92 1 3 3 15.95 11.95 2.37 0.072 1.46 4 -8 2 11.50 8.12 2.37 0.060 0.90 2 3 0 287.32 260.37 2.36 0.337 1.62 -3 0 9 11.01 7.18 2.34 0.056 0.83 4 -1 2 2.41 1.21 2.34 0.023 1.41 1 -2 1 103.82 117.17 2.34 0.226 3.44 -2 -3 3 122.98 109.18 2.32 0.218 1.51 -4 -4 4 12.32 16.84 2.32 0.086 0.96 0 -8 3 4.17 1.95 2.31 0.029 0.90 -1 6 6 9.27 5.88 2.29 0.051 0.83 0 2 2 52.71 45.52 2.29 0.141 2.42 -4 7 5 29.80 23.00 2.28 0.100 0.79 -1 1 2 986.60 1068.24 2.27 0.683 3.09 2 -7 2 13.49 10.35 2.25 0.067 1.08 3 0 8 2.75 1.21 2.24 0.023 0.86 1 0 8 1.03 2.42 2.23 0.033 0.96 4 4 1 13.22 17.16 2.20 0.087 0.97 Bond lengths and angles C1 - Distance Angles O1B 1.2476 (0.0028) O1A 1.2649 (0.0028) 126.31 (0.22) C2 1.5307 (0.0031) 117.31 (0.20) 116.37 (0.20) C1 - O1B O1A C2 - Distance Angles O2 1.4174 (0.0029) C3 1.5266 (0.0033) 110.06 (0.19) C1 1.5307 (0.0031) 111.02 (0.18) 111.35 (0.19) H2 1.0000 108.10 108.10 108.10 C2 - O2 C3 C1 C3 - Distance Angles C4 1.5188 (0.0031) C2 1.5266 (0.0033) 109.18 (0.19) H3A 0.9900 109.84 109.84 H3B 0.9900 109.84 109.84 108.27 C3 - C4 C2 H3A C4 - Distance Angles O4B 1.2092 (0.0030) O4A 1.3105 (0.0029) 123.95 (0.21) C3 1.5188 (0.0031) 122.26 (0.22) 113.75 (0.20) C4 - O4B O4A O1A - Distance Angles C1 1.2649 (0.0028) O1A - O1B - Distance Angles C1 1.2476 (0.0028) O1B - O2 - Distance Angles C2 1.4174 (0.0029) H2A 0.8400 109.47 O2 - C2 O4A - Distance Angles C4 1.3105 (0.0029) H4A 0.8400 109.47 O4A - C4 O4B - Distance Angles C4 1.2092 (0.0030) O4B - C21 - Distance Angles C22 1.5375 (0.0034) 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 C26 1.5345 (0.0036) C27 1.5349 (0.0035) 109.68 (0.21) C21 1.5375 (0.0034) 107.83 (0.21) 107.59 (0.21) C23 1.5441 (0.0032) 113.75 (0.21) 112.57 (0.20) 105.02 (0.19) C22 - C26 C27 C21 C23 - Distance Angles C24 1.5396 (0.0032) C22 1.5441 (0.0032) 123.06 (0.20) H23A 0.9900 106.56 106.56 H23B 0.9900 106.56 106.56 106.54 C23 - C24 C22 H23A C24 - Distance Angles C28 1.5222 (0.0033) C29 1.5242 (0.0032) 110.62 (0.20) N25 1.5269 (0.0029) 106.35 (0.18) 105.91 (0.19) C23 1.5396 (0.0032) 113.42 (0.19) 115.87 (0.19) 103.68 (0.18) C24 - C28 C29 N25 C26 - Distance Angles C22 1.5345 (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 1.5349 (0.0035) 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 1.5222 (0.0033) 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 1.5242 (0.0032) 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 1.5269 (0.0029) H25A 0.9100 109.47 H25B 0.9100 109.47 109.47 H25C 0.9100 109.47 109.47 109.47 N25 - C24 H25A H25B Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.12 2.621(2) 117.6 O2-H2A...O1B 0.91 1.94 2.828(3) 164.4 N25-H25A...O1B 0.84 2.17 2.767(2) 128.3 O2-H2A...O4B_$1 0.91 2.03 2.920(3) 166.4 N25-H25C...O1A_$1 0.84 1.74 2.582(2) 177.5 O4A-H4A...O1A_$2 0.91 1.99 2.891(3) 171.1 N25-H25B...O2_$3 FMAP and GRID set by program FMAP 2 1 31 GRID -3.571 -2 -2 3.571 2 2 R1 = 0.0407 for 1616 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.18 at 0.9146 0.2851 0.6662 [ 0.75 A from C1 ] Deepest hole -0.19 at 0.0323 0.9123 0.6552 [ 0.78 A from C4 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 2573 / 18414 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9146 0.2851 0.6662 1.00000 0.05 0.18 0.75 C1 0.80 C2 1.39 H2 1.72 O1A Q2 1 0.5303 0.7646 0.9888 1.00000 0.05 0.18 0.74 C24 0.78 C28 1.41 H28A 1.44 H28B Q3 1 0.6918 0.7139 0.9655 1.00000 0.05 0.17 0.70 C24 0.83 C29 1.45 H29C 1.48 H29B Q4 1 0.5121 0.6002 0.9658 1.00000 0.05 0.17 0.75 C24 0.80 C23 1.45 H23B 1.47 H23A Q5 1 0.9855 0.1490 0.6019 1.00000 0.05 0.16 0.71 C2 0.82 C3 1.43 H2 1.46 H3A Q6 1 0.2631 0.6615 1.4815 1.00000 0.05 0.16 1.66 H26A 1.72 H4A 1.82 H26C 2.00 O1A Q7 1 0.5719 0.4075 1.1335 1.00000 0.05 0.15 0.73 C22 0.83 C27 1.39 H27C 1.49 H27B Q8 1 1.2942 0.2636 0.7124 1.00000 0.05 0.15 1.64 H3B 1.66 H2 1.69 H23A 2.01 C3 Q9 1 1.0982 0.1554 0.6614 1.00000 0.05 0.15 1.06 C3 1.11 C2 1.13 H2 1.39 H3B Q10 1 1.1795 0.4862 0.6914 1.00000 0.05 0.15 0.96 O1A 1.40 H25C 1.77 C1 2.18 H2 Shortest distances between peaks (including symmetry equivalents) 5 9 0.82 2 3 1.18 3 4 1.19 2 4 1.20 8 9 1.25 1 5 1.27 1 9 1.70 1 10 1.86 5 8 1.96 8 10 2.04 4 7 2.26 6 10 2.32 9 10 2.37 1 8 2.42 5 10 2.44 4 10 2.81 3 7 2.83 4 8 2.91 Time profile in seconds ----------------------- 0.09: 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. 0.30: 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 0.02: Generate idealized H-atoms 0.22: Structure factors and derivatives 0.38: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0078p1 finished at 12:32:11 Total CPU time: 1.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++