+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src1284p21c started at 20:40:57 on 12-Jan-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src1284p21c in P2(1)/c CELL 0.71073 13.2331 11.7105 10.2193 90.000 99.664 90.000 ZERR 4.00 0.0006 0.0006 0.0005 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S UNIT 40 80 16 24 8 V = 1561.17 F(000) = 752.0 Mu = 0.38 mm-1 Cell Wt = 1425.68 Rho = 1.516 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 DFIX 0.84 0.02 o1w h1w o1w h2w DANG 1.35 0.02 h1w h2w FMAP 2 PLAN 10 SIZE 0.01 0.02 0.07 ACTA HTAB O1W O22 HTAB O1W S2 EQIV_$1 -x, y-1/2, -z+1/2 HTAB N5 O1W_$1 EQIV_$2 -x, y+1/2, -z+1/2 HTAB O1w O21_$2 HTAB O1w S2_$2 BOND $H WGHT 0.00000 6.57210 L.S. 4 TEMP -153.00 FVAR 0.44258 MOLE 1 C2 1 -0.253477 0.622605 0.281469 11.00000 0.02230 0.02214 = 0.02939 -0.00246 0.00564 -0.00188 AFIX 43 H2 2 -0.276822 0.699304 0.281779 11.00000 -1.20000 AFIX 0 C3 1 -0.188305 0.583682 0.393542 11.00000 0.02740 0.02565 = 0.02586 -0.00603 0.00478 -0.00350 AFIX 43 H3 2 -0.170429 0.629887 0.470349 11.00000 -1.20000 AFIX 0 C4 1 -0.151763 0.476326 0.387115 11.00000 0.02355 0.02841 = 0.01733 0.00093 -0.00109 -0.00626 AFIX 43 H4 2 -0.103909 0.446842 0.458907 11.00000 -1.20000 AFIX 0 C6 1 -0.251873 0.451935 0.175152 11.00000 0.01693 0.01754 = 0.01916 0.00167 0.00814 -0.00347 C8 1 -0.258668 0.264047 0.059873 11.00000 0.02461 0.01932 = 0.03149 -0.00359 0.00069 0.00567 AFIX 23 H8A 2 -0.218069 0.237856 0.144844 11.00000 -1.20000 H8B 2 -0.215853 0.255411 -0.010191 11.00000 -1.20000 AFIX 0 C9 1 -0.354336 0.191083 0.026040 11.00000 0.02569 0.01767 = 0.01605 -0.00399 -0.00238 0.00178 AFIX 23 H9A 2 -0.334988 0.110932 0.011828 11.00000 -1.20000 H9B 2 -0.393771 0.192814 0.100213 11.00000 -1.20000 AFIX 0 C11 1 -0.448767 0.356216 -0.079179 11.00000 0.02357 0.01878 = 0.01799 0.00191 0.00424 0.00580 AFIX 23 H11A 2 -0.489100 0.361521 -0.006110 11.00000 -1.20000 H11B 2 -0.491968 0.383692 -0.161729 11.00000 -1.20000 AFIX 0 C12 1 -0.353132 0.428689 -0.047661 11.00000 0.02588 0.01761 = 0.01883 0.00248 0.00029 -0.00216 AFIX 23 H12A 2 -0.315865 0.427731 -0.123943 11.00000 -1.20000 H12B 2 -0.372434 0.508653 -0.032331 11.00000 -1.20000 AFIX 0 C13 1 -0.603462 0.144685 -0.067966 11.00000 0.02402 0.02388 = 0.02154 -0.00124 0.00264 -0.00690 AFIX 137 H13A 2 -0.659265 0.094760 -0.109232 11.00000 -1.20000 H13B 2 -0.630469 0.221356 -0.056852 11.00000 -1.20000 H13C 2 -0.573292 0.113861 0.019000 11.00000 -1.20000 AFIX 0 N1 3 -0.285323 0.560412 0.174352 11.00000 0.02115 0.02073 = 0.02431 0.00137 0.00481 -0.00164 N5 3 -0.183236 0.410349 0.278268 11.00000 0.01631 0.01935 = 0.02088 0.00106 -0.00025 -0.00005 AFIX 43 H55 2 -0.159128 0.340601 0.274570 11.00000 -1.20000 AFIX 0 N7 3 -0.286167 0.384826 0.071159 11.00000 0.02396 0.01899 = 0.01799 -0.00361 -0.00060 -0.00098 N10 3 -0.417680 0.236391 -0.095865 11.00000 0.01976 0.01578 = 0.01953 -0.00072 -0.00270 0.00404 O1 4 -0.463801 0.040909 -0.175256 11.00000 0.03009 0.02174 = 0.02621 -0.00889 -0.00118 0.00381 O2 4 -0.552775 0.206417 -0.292400 11.00000 0.02983 0.02628 = 0.01563 0.00266 0.00109 0.00225 S1 5 -0.509144 0.151991 -0.169762 11.00000 0.02359 0.01850 = 0.01617 -0.00144 0.00210 0.00080 MOLE 2 C21 1 0.122518 0.415057 0.064369 11.00000 0.03007 0.04261 = 0.02409 -0.00181 0.00354 -0.00246 AFIX 137 H21A 2 0.067371 0.360735 0.033266 11.00000 -1.20000 H21B 2 0.188554 0.381431 0.054121 11.00000 -1.20000 H21C 2 0.111450 0.485381 0.011936 11.00000 -1.20000 AFIX 0 O21 4 0.131389 0.336435 0.300228 11.00000 0.02912 0.02176 = 0.02568 0.00258 -0.00031 -0.00007 O22 4 0.025618 0.503579 0.239142 11.00000 0.02138 0.02810 = 0.04654 0.00572 0.00789 0.00601 O23 4 0.210308 0.520326 0.276505 11.00000 0.02736 0.02399 = 0.02801 -0.00389 0.00426 -0.00416 S2 5 0.122841 0.446748 0.232990 11.00000 0.02146 0.01933 = 0.02218 0.00052 0.00313 0.00065 MOLE 3 O1W 4 0.053171 0.735830 0.185257 11.00000 0.02407 0.01955 = 0.05105 -0.00170 -0.00288 0.00250 H1W 2 -0.005967 0.764055 0.185121 11.00000 0.04007 H2W 2 0.050577 0.669417 0.215765 11.00000 0.06013 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 2008src1284p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C2 - N1 C3 C3 - C4 C2 C4 - C3 N5 C6 - N7 N1 N5 C8 - N7 C9 C9 - N10 C8 C11 - N10 C12 C12 - N7 C11 C13 - S1 N1 - C2 C6 N5 - C6 C4 N7 - C6 C8 C12 N10 - C9 C11 S1 O1 - S1 O2 - S1 S1 - O1 O2 N10 C13 C21 - S2 O21 - S2 O22 - S2 O23 - S2 S2 - O23 O21 O22 C21 O1W - no bonds found Operators for generating equivalent atoms: $1 -x, y-1/2, -z+1/2 $2 -x, y+1/2, -z+1/2 16239 Reflections read, of which 462 rejected -17 =< h =< 17, -15 =< k =< 15, -11 =< l =< 13, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 3546 Unique reflections, of which 0 suppressed R(int) = 0.0994 R(sigma) = 0.0988 Friedel opposites merged Maximum memory for data reduction = 2332 / 35557 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 = 2925 / 259978 wR2 = 0.1625 before cycle 1 for 3546 data and 209 / 209 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.007 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.182; Restrained GooF = 1.182 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.44258 0.00110 0.000 OSF Mean shift/su = 0.001 Maximum = 0.007 for U13 S1 Max. shift = 0.000 A for H2W Max. dU = 0.000 for C13 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2925 / 259978 wR2 = 0.1625 before cycle 2 for 3546 data and 209 / 209 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.007 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.182; Restrained GooF = 1.182 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.44258 0.00110 -0.001 OSF Mean shift/su = 0.000 Maximum = 0.003 for U13 S1 Max. shift = 0.000 A for S1 Max. dU = 0.000 for H1W Least-squares cycle 3 Maximum vector length = 511 Memory required = 2925 / 259978 wR2 = 0.1625 before cycle 3 for 3546 data and 209 / 209 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.007 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.182; Restrained GooF = 1.182 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.44258 0.00110 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H2W Max. dU = 0.000 for H2W Least-squares cycle 4 Maximum vector length = 511 Memory required = 2925 / 259978 wR2 = 0.1625 before cycle 4 for 3546 data and 209 / 209 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.007 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.182; Restrained GooF = 1.182 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.44258 0.00110 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x S1 Max. shift = 0.000 A for H2W Max. dU = 0.000 for H2W Largest correlation matrix elements 0.750 z H2W / y H2W 0.673 y H1W / x H1W -0.582 x H2W / y H1W Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -0.2768 0.6993 0.2818 43 0.950 0.000 C2 N1 C3 H3 -0.1704 0.6299 0.4703 43 0.950 0.000 C3 C4 C2 H4 -0.1039 0.4468 0.4589 43 0.950 0.000 C4 C3 N5 H8A -0.2181 0.2379 0.1448 23 0.990 0.000 C8 N7 C9 H8B -0.2159 0.2554 -0.0102 23 0.990 0.000 C8 N7 C9 H9A -0.3350 0.1109 0.0118 23 0.990 0.000 C9 N10 C8 H9B -0.3938 0.1928 0.1002 23 0.990 0.000 C9 N10 C8 H11A -0.4891 0.3615 -0.0061 23 0.990 0.000 C11 N10 C12 H11B -0.4920 0.3837 -0.1617 23 0.990 0.000 C11 N10 C12 H12A -0.3159 0.4277 -0.1239 23 0.990 0.000 C12 N7 C11 H12B -0.3724 0.5087 -0.0323 23 0.990 0.000 C12 N7 C11 H13A -0.6593 0.0948 -0.1092 137 0.980 0.000 C13 S1 H13A H13B -0.6305 0.2214 -0.0569 137 0.980 0.000 C13 S1 H13A H13C -0.5733 0.1139 0.0190 137 0.980 0.000 C13 S1 H13A H55 -0.1591 0.3406 0.2746 43 0.880 0.000 N5 C6 C4 H21A 0.0674 0.3607 0.0333 137 0.980 0.000 C21 S2 H21A H21B 0.1886 0.3814 0.0541 137 0.980 0.000 C21 S2 H21A H21C 0.1114 0.4854 0.0119 137 0.980 0.000 C21 S2 H21A 2008src1284p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 -0.25348 0.62261 0.28147 1.00000 0.02230 0.02214 0.02939 -0.00246 0.00564 -0.00188 0.02446 0.00906 0.00038 0.00044 0.00051 0.00000 0.00266 0.00275 0.00280 0.00222 0.00229 0.00209 0.00115 H2 -0.27682 0.69930 0.28178 1.00000 0.02935 0.00000 0.00000 C3 -0.18831 0.58368 0.39354 1.00000 0.02740 0.02565 0.02586 -0.00603 0.00478 -0.00350 0.02627 0.00932 0.00039 0.00044 0.00052 0.00000 0.00285 0.00291 0.00276 0.00227 0.00233 0.00223 0.00119 H3 -0.17043 0.62989 0.47035 1.00000 0.03152 0.00000 0.00000 C4 -0.15176 0.47633 0.38712 1.00000 0.02355 0.02841 0.01733 0.00093 -0.00109 -0.00626 0.02362 0.00880 0.00038 0.00044 0.00048 0.00000 0.00261 0.00289 0.00239 0.00212 0.00206 0.00219 0.00112 H4 -0.10391 0.44684 0.45891 1.00000 0.02834 0.00000 0.00000 C6 -0.25187 0.45193 0.17515 1.00000 0.01693 0.01754 0.01916 0.00167 0.00814 -0.00347 0.01729 0.00849 0.00034 0.00041 0.00045 0.00000 0.00230 0.00242 0.00233 0.00201 0.00193 0.00195 0.00098 C8 -0.25867 0.26405 0.05987 1.00000 0.02461 0.01932 0.03149 -0.00359 0.00069 0.00567 0.02560 0.00910 0.00038 0.00041 0.00054 0.00000 0.00268 0.00262 0.00289 0.00226 0.00231 0.00212 0.00116 H8A -0.21807 0.23786 0.14484 1.00000 0.03073 0.00000 0.00000 H8B -0.21585 0.25541 -0.01019 1.00000 0.03073 0.00000 0.00000 C9 -0.35434 0.19108 0.02604 1.00000 0.02569 0.01767 0.01605 -0.00399 -0.00238 0.00178 0.02048 0.00833 0.00036 0.00042 0.00046 0.00000 0.00267 0.00250 0.00229 0.00196 0.00205 0.00204 0.00107 H9A -0.33499 0.11093 0.01183 1.00000 0.02458 0.00000 0.00000 H9B -0.39377 0.19281 0.10021 1.00000 0.02458 0.00000 0.00000 C11 -0.44877 0.35622 -0.07918 1.00000 0.02357 0.01878 0.01799 0.00191 0.00424 0.00580 0.02003 0.00882 0.00037 0.00040 0.00047 0.00000 0.00257 0.00252 0.00233 0.00203 0.00204 0.00202 0.00103 H11A -0.48910 0.36152 -0.00611 1.00000 0.02403 0.00000 0.00000 H11B -0.49197 0.38369 -0.16173 1.00000 0.02403 0.00000 0.00000 C12 -0.35313 0.42869 -0.04766 1.00000 0.02588 0.01761 0.01883 0.00248 0.00029 -0.00216 0.02117 0.00851 0.00037 0.00041 0.00047 0.00000 0.00264 0.00253 0.00239 0.00202 0.00205 0.00204 0.00106 H12A -0.31586 0.42773 -0.12394 1.00000 0.02540 0.00000 0.00000 H12B -0.37243 0.50865 -0.03233 1.00000 0.02540 0.00000 0.00000 C13 -0.60346 0.14468 -0.06797 1.00000 0.02402 0.02388 0.02154 -0.00124 0.00264 -0.00690 0.02328 0.00884 0.00037 0.00044 0.00048 0.00000 0.00266 0.00270 0.00247 0.00219 0.00214 0.00216 0.00110 H13A -0.65927 0.09476 -0.10923 1.00000 0.02793 0.00000 0.00000 H13B -0.63047 0.22136 -0.05685 1.00000 0.02793 0.00000 0.00000 H13C -0.57329 0.11386 0.01900 1.00000 0.02793 0.00000 0.00000 N1 -0.28532 0.56041 0.17435 1.00000 0.02115 0.02073 0.02431 0.00137 0.00481 -0.00164 0.02195 0.00736 0.00030 0.00035 0.00040 0.00000 0.00213 0.00222 0.00217 0.00185 0.00177 0.00176 0.00091 N5 -0.18324 0.41035 0.27827 1.00000 0.01631 0.01935 0.02088 0.00106 -0.00025 -0.00005 0.01923 0.00697 0.00029 0.00034 0.00039 0.00000 0.00203 0.00213 0.00205 0.00173 0.00169 0.00162 0.00088 H55 -0.15913 0.34060 0.27457 1.00000 0.02308 0.00000 0.00000 N7 -0.28617 0.38483 0.07116 1.00000 0.02396 0.01899 0.01799 -0.00361 -0.00060 -0.00098 0.02079 0.00706 0.00031 0.00034 0.00039 0.00000 0.00223 0.00214 0.00203 0.00167 0.00179 0.00173 0.00092 N10 -0.41768 0.23639 -0.09587 1.00000 0.01976 0.01578 0.01953 -0.00072 -0.00270 0.00404 0.01905 0.00694 0.00029 0.00033 0.00038 0.00000 0.00206 0.00211 0.00204 0.00167 0.00170 0.00165 0.00089 O1 -0.46380 0.04091 -0.17526 1.00000 0.03009 0.02174 0.02621 -0.00889 -0.00118 0.00381 0.02669 0.00607 0.00026 0.00029 0.00034 0.00000 0.00196 0.00193 0.00187 0.00158 0.00157 0.00155 0.00083 O2 -0.55278 0.20642 -0.29240 1.00000 0.02983 0.02628 0.01563 0.00266 0.00109 0.00225 0.02423 0.00613 0.00026 0.00030 0.00031 0.00000 0.00196 0.00198 0.00167 0.00149 0.00148 0.00154 0.00079 S1 -0.50914 0.15199 -0.16976 1.00000 0.02359 0.01850 0.01617 -0.00144 0.00210 0.00080 0.01956 0.00221 0.00010 0.00010 0.00012 0.00000 0.00064 0.00062 0.00056 0.00050 0.00049 0.00051 0.00028 C21 0.12252 0.41506 0.06437 1.00000 0.03007 0.04261 0.02409 -0.00181 0.00354 -0.00246 0.03237 0.00998 0.00043 0.00050 0.00052 0.00000 0.00298 0.00358 0.00276 0.00255 0.00239 0.00254 0.00132 H21A 0.06737 0.36073 0.03327 1.00000 0.03885 0.00000 0.00000 H21B 0.18855 0.38143 0.05412 1.00000 0.03885 0.00000 0.00000 H21C 0.11145 0.48538 0.01194 1.00000 0.03885 0.00000 0.00000 O21 0.13139 0.33643 0.30023 1.00000 0.02912 0.02176 0.02568 0.00258 -0.00031 -0.00007 0.02608 0.00621 0.00026 0.00029 0.00034 0.00000 0.00196 0.00191 0.00189 0.00154 0.00159 0.00153 0.00083 O22 0.02562 0.50358 0.23914 1.00000 0.02138 0.02810 0.04654 0.00572 0.00789 0.00601 0.03176 0.00703 0.00026 0.00032 0.00039 0.00000 0.00189 0.00212 0.00236 0.00180 0.00172 0.00157 0.00091 O23 0.21031 0.52033 0.27650 1.00000 0.02736 0.02399 0.02801 -0.00389 0.00426 -0.00416 0.02650 0.00613 0.00026 0.00029 0.00035 0.00000 0.00190 0.00195 0.00195 0.00156 0.00158 0.00152 0.00082 S2 0.12284 0.44675 0.23299 1.00000 0.02146 0.01933 0.02218 0.00052 0.00313 0.00065 0.02105 0.00226 0.00009 0.00011 0.00012 0.00000 0.00063 0.00062 0.00061 0.00053 0.00050 0.00051 0.00029 O1W 0.05317 0.73583 0.18526 1.00000 0.02407 0.01955 0.05105 -0.00170 -0.00288 0.00250 0.03261 0.00691 0.00028 0.00033 0.00043 0.00000 0.00210 0.00212 0.00262 0.00190 0.00187 0.00164 0.00094 H1W -0.00597 0.76405 0.18512 1.00000 0.04007 0.10336 0.00235 0.00401 0.00587 0.00000 0.01819 H2W 0.05058 0.66942 0.21577 1.00000 0.06013 0.11920 0.00415 0.00265 0.00662 0.00000 0.02340 Final Structure Factor Calculation for 2008src1284p21c in P2(1)/c Total number of l.s. parameters = 209 Maximum vector length = 511 Memory required = 2716 / 24017 wR2 = 0.1625 before cycle 5 for 3546 data and 0 / 209 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.007 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.182; Restrained GooF = 1.182 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.57 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0893 for 2282 Fo > 4sig(Fo) and 0.1496 for all 3546 data wR2 = 0.1625, GooF = S = 1.182, Restrained GooF = 1.182 for all data Occupancy sum of asymmetric unit = 22.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0303 0.0228 0.0203 C2 0.0326 0.0267 0.0194 C3 0.0341 0.0214 0.0153 C4 0.0227 0.0195 0.0096 C6 0.0366 0.0248 0.0154 C8 0.0308 0.0184 0.0123 C9 0.0275 0.0178 0.0148 C11 0.0289 0.0189 0.0157 C12 0.0310 0.0221 0.0168 C13 0.0248 0.0226 0.0185 N1 0.0236 0.0191 0.0150 N5 0.0271 0.0213 0.0140 N7 0.0280 0.0166 0.0125 N10 0.0404 0.0249 0.0148 O1 0.0314 0.0265 0.0148 O2 0.0243 0.0189 0.0155 S1 0.0431 0.0301 0.0238 C21 0.0339 0.0243 0.0201 O21 0.0483 0.0292 0.0178 O22 0.0312 0.0282 0.0201 O23 0.0226 0.0215 0.0191 S2 0.0560 0.0235 0.0184 O1W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.019 0.030 0.041 0.053 0.068 0.087 0.110 0.157 1.000 Number in group 386. 325. 361. 376. 347. 340. 354. 349. 352. 356. GooF 1.150 1.235 1.298 1.339 1.272 1.229 1.202 1.133 0.966 0.929 K 13.567 2.906 1.434 1.279 1.059 1.046 1.019 0.990 1.003 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 364. 349. 352. 362. 346. 355. 355. 352. 358. 353. GooF 1.307 1.361 1.259 1.218 1.186 1.207 1.093 1.063 0.982 1.096 K 1.222 1.214 1.126 1.058 1.057 1.019 1.000 0.991 1.008 1.003 R1 0.342 0.329 0.246 0.238 0.184 0.152 0.096 0.070 0.063 0.040 Recommended weighting scheme: WGHT 0.0000 6.5721 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) -5 10 5 253.49 10.42 3.77 0.014 0.97 -10 11 6 65.60 379.28 3.61 0.087 0.77 14 8 0 328.80 0.01 3.45 0.000 0.79 4 1 12 262.30 0.73 3.38 0.004 0.78 0 14 3 808.57 372.98 3.34 0.086 0.81 -3 5 10 188.34 417.93 3.30 0.091 0.94 12 8 3 275.16 21.86 3.29 0.021 0.82 -7 6 6 257.61 73.35 3.20 0.038 1.12 -8 13 2 143.10 8.09 3.17 0.013 0.79 -4 12 5 176.14 440.49 3.15 0.093 0.86 7 7 0 60.85 194.28 3.06 0.062 1.24 -2 7 11 356.95 91.77 3.00 0.043 0.81 -14 2 3 88.15 311.45 2.97 0.078 0.93 6 11 2 248.25 21.74 2.93 0.021 0.93 8 0 6 200.63 457.49 2.92 0.095 1.08 3 6 10 462.72 149.82 2.92 0.054 0.85 1 9 6 91.61 288.90 2.90 0.076 1.02 -4 3 1 -19.52 69.18 2.88 0.037 2.51 -14 6 4 694.62 88.27 2.82 0.042 0.84 -11 1 11 633.05 36.36 2.81 0.027 0.79 -14 4 2 262.31 67.27 2.81 0.036 0.90 10 10 3 194.04 17.61 2.79 0.019 0.82 6 9 3 184.73 9.64 2.76 0.014 1.03 11 7 5 589.65 261.37 2.75 0.072 0.83 -4 7 7 414.67 653.02 2.74 0.114 1.08 -6 5 4 113.53 5.17 2.74 0.010 1.43 7 13 3 375.75 130.02 2.73 0.051 0.78 -15 4 7 457.41 154.65 2.73 0.055 0.78 14 5 2 216.05 0.08 2.73 0.001 0.83 7 11 1 151.75 20.45 2.73 0.020 0.91 -12 8 4 322.81 45.90 2.72 0.030 0.86 4 12 2 409.74 218.21 2.71 0.066 0.91 -13 6 6 643.77 166.93 2.71 0.057 0.84 -8 1 11 712.43 429.09 2.67 0.092 0.86 -8 6 8 102.11 3.20 2.67 0.008 0.95 8 13 0 307.48 63.56 2.65 0.035 0.79 -16 1 6 232.11 61.30 2.64 0.035 0.79 -10 1 8 351.30 84.27 2.64 0.041 0.99 2 2 11 188.51 358.25 2.62 0.084 0.88 -2 5 11 206.22 16.36 2.62 0.018 0.86 -4 12 1 165.40 16.97 2.61 0.018 0.94 6 5 10 188.61 0.19 2.61 0.002 0.81 9 1 8 249.45 28.51 2.60 0.024 0.88 1 1 12 200.79 52.09 2.60 0.032 0.83 -12 3 6 280.41 92.25 2.58 0.043 0.96 0 12 7 133.05 4.46 2.58 0.009 0.81 -14 5 5 349.81 4.38 2.56 0.009 0.84 5 2 7 114.99 3.58 2.55 0.008 1.16 -9 12 2 148.08 6.05 2.55 0.011 0.81 0 1 5 -14.13 84.88 2.54 0.041 1.99 Bond lengths and angles C2 - Distance Angles N1 1.3234 (0.0063) C3 1.3898 (0.0071) 124.65 (0.48) H2 0.9500 117.68 117.68 C2 - N1 C3 C3 - Distance Angles C4 1.3525 (0.0071) C2 1.3898 (0.0071) 116.25 (0.48) H3 0.9500 121.88 121.88 C3 - C4 C2 C4 - Distance Angles C3 1.3525 (0.0071) N5 1.3609 (0.0062) 120.30 (0.47) H4 0.9500 119.85 119.85 C4 - C3 N5 C6 - Distance Angles N7 1.3383 (0.0060) N1 1.3448 (0.0061) 118.85 (0.42) N5 1.3606 (0.0059) 119.88 (0.43) 121.27 (0.42) C6 - N7 N1 C8 - Distance Angles N7 1.4698 (0.0061) C9 1.5184 (0.0068) 110.58 (0.40) H8A 0.9900 109.53 109.53 H8B 0.9900 109.53 109.53 108.09 C8 - N7 C9 H8A C9 - Distance Angles N10 1.4784 (0.0057) C8 1.5184 (0.0068) 108.85 (0.40) H9A 0.9900 109.92 109.92 H9B 0.9900 109.92 109.92 108.32 C9 - N10 C8 H9A C11 - Distance Angles N10 1.4802 (0.0059) C12 1.5129 (0.0065) 108.52 (0.38) H11A 0.9900 109.99 109.99 H11B 0.9900 109.99 109.99 108.36 C11 - N10 C12 H11A C12 - Distance Angles N7 1.4705 (0.0059) C11 1.5129 (0.0065) 110.27 (0.38) H12A 0.9900 109.60 109.60 H12B 0.9900 109.60 109.60 108.13 C12 - N7 C11 H12A C13 - Distance Angles S1 1.7559 (0.0050) H13A 0.9800 109.47 H13B 0.9800 109.47 109.47 H13C 0.9800 109.47 109.47 109.47 C13 - S1 H13A H13B N1 - Distance Angles C2 1.3234 (0.0063) C6 1.3448 (0.0061) 117.13 (0.42) N1 - C2 N5 - Distance Angles C6 1.3606 (0.0059) C4 1.3609 (0.0062) 120.18 (0.42) H55 0.8800 119.91 119.91 N5 - C6 C4 N7 - Distance Angles C6 1.3383 (0.0060) C8 1.4698 (0.0061) 124.89 (0.41) C12 1.4705 (0.0059) 121.85 (0.40) 113.21 (0.38) N7 - C6 C8 N10 - Distance Angles C9 1.4784 (0.0058) C11 1.4802 (0.0059) 111.86 (0.36) S1 1.6448 (0.0039) 116.15 (0.31) 115.17 (0.30) N10 - C9 C11 O1 - Distance Angles S1 1.4376 (0.0035) O1 - O2 - Distance Angles S1 1.4378 (0.0034) O2 - S1 - Distance Angles O1 1.4376 (0.0035) O2 1.4378 (0.0034) 118.44 (0.21) N10 1.6448 (0.0039) 106.37 (0.20) 106.90 (0.20) C13 1.7559 (0.0050) 108.78 (0.24) 108.46 (0.23) 107.38 (0.22) S1 - O1 O2 N10 C21 - Distance Angles S2 1.7620 (0.0054) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - S2 H21A H21B O21 - Distance Angles S2 1.4586 (0.0036) O21 - O22 - Distance Angles S2 1.4592 (0.0035) O22 - O23 - Distance Angles S2 1.4516 (0.0035) O23 - S2 - Distance Angles O23 1.4516 (0.0036) O21 1.4586 (0.0036) 112.74 (0.21) O22 1.4592 (0.0035) 112.31 (0.22) 112.51 (0.22) C21 1.7620 (0.0054) 107.19 (0.24) 105.15 (0.25) 106.31 (0.25) S2 - O23 O21 O22 O1W - Distance Angles H1W 0.8493 (0.0191) H2W 0.8407 (0.0193) 105.41 (2.98) O1W - H1W Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.841(19) 1.99(3) 2.811(5) 165(7) O1W-H2W...O22 0.841(19) 2.77(3) 3.521(4) 149(5) O1W-H2W...S2 0.88 1.86 2.658(5) 150.4 N5-H55...O1W_$1 0.849(19) 1.89(2) 2.738(5) 174(6) O1W-H1W...O21_$2 0.849(19) 2.85(3) 3.588(4) 147(5) O1W-H1W...S2_$2 FMAP and GRID set by program FMAP 2 3 15 GRID -2.083 -2 -2 2.083 2 2 R1 = 0.1481 for 3546 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.46 at 0.5472 0.8391 0.0951 [ 0.86 A from C13 ] Deepest hole -0.44 at 0.4780 0.7637 0.0169 [ 1.23 A from N10 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 2909 / 20823 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.5472 0.1609 -0.0951 1.00000 0.05 0.46 0.86 C13 0.99 S1 1.38 H13C 1.42 H13B Q2 1 -0.3590 0.4259 -0.2250 1.00000 0.05 0.44 1.09 H12A 1.80 C12 2.04 H11B 2.21 O23 Q3 1 -0.5805 0.3028 -0.2429 1.00000 0.05 0.43 1.31 O2 1.62 H11B 1.86 H2 2.08 S1 Q4 1 -0.3430 0.6949 0.3765 1.00000 0.05 0.41 1.41 H2 1.86 C2 1.89 O2 1.91 H13C Q5 1 0.1021 0.3344 0.4076 1.00000 0.05 0.41 1.22 O21 1.47 H3 1.67 H1W 2.27 S2 Q6 1 -0.1997 0.6817 0.1661 1.00000 0.05 0.41 1.63 C2 1.70 H2 1.83 N1 2.03 O21 Q7 1 -0.2532 0.3337 -0.1679 1.00000 0.05 0.40 1.49 H12A 1.85 H8B 2.17 O23 2.21 H8A Q8 1 -0.4405 0.4815 -0.2272 1.00000 0.05 0.40 1.54 H11B 1.63 O1 1.91 H12A 2.07 H12B Q9 1 -0.1527 0.7072 0.3712 1.00000 0.05 0.40 1.41 H3 1.55 C3 1.74 H2 1.79 C2 Q10 1 0.0196 0.6590 0.1212 1.00000 0.05 0.40 0.99 H2W 1.16 O1W 1.46 H1W 1.81 H21A Shortest distances between peaks (including symmetry equivalents) 2 8 1.26 3 4 1.56 2 7 1.79 6 9 2.10 1 3 2.24 5 9 2.30 5 6 2.40 4 9 2.53 5 10 2.60 1 8 2.76 3 8 2.78 1 4 2.89 Time profile in seconds ----------------------- 0.02: 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. 0.73: 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 0.78: Structure factors and derivatives 1.05: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.13: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.13: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src1284p21c finished at 20:41:00 Total CPU time: 3.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++