+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0518 started at 13:41:25 on 12-May-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0518 in P2(1)/n CELL 0.71073 11.5481 8.4612 16.5109 90.000 98.323 90.000 ZERR 4.00 0.0004 0.0004 0.0008 0.000 0.003 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 64 64 24 12 V = 1596.30 F(000) = 712.0 Mu = 0.10 mm-1 Cell Wt = 1361.39 Rho = 1.416 MERG 2 OMIT -3.00 55.00 OMIT 1 1 1 EXTI 0.01429 SHEL 7 0.77 DFIX 0.88 0.02 N15 H15 FMAP 2 PLAN 10 SIZE 0.11 0.18 0.19 ACTA EQIV_$1 -x+1/2, y-1/2, -z-1/2 HTAB N15 O31_$1 HTAB O31 N17 HTAB O31 N16 BOND $H WGHT 0.07650 0.54760 L.S. 4 TEMP -153.00 FVAR 0.43605 MOLE 1 C1 1 1.024931 0.207321 -0.019590 11.00000 0.03809 0.03969 = 0.04002 0.00048 0.01186 0.00675 AFIX 137 H1A 2 0.968036 0.146685 -0.057084 11.00000 -1.50000 H1B 2 1.093486 0.141291 -0.001376 11.00000 -1.50000 H1C 2 1.049127 0.300883 -0.047861 11.00000 -1.50000 AFIX 0 C3 1 0.877391 0.353273 0.035654 11.00000 0.02449 0.02834 = 0.03137 0.00015 0.00192 0.00105 C4 1 0.826783 0.405224 -0.041742 11.00000 0.03099 0.03083 = 0.02455 -0.00122 0.00712 -0.00084 AFIX 43 H4 2 0.857652 0.372573 -0.089354 11.00000 -1.20000 AFIX 0 C5 1 0.730360 0.505639 -0.047981 11.00000 0.02665 0.03165 = 0.02458 0.00214 0.00244 0.00098 AFIX 43 H5 2 0.695520 0.541280 -0.100454 11.00000 -1.20000 AFIX 0 C6 1 0.684097 0.554736 0.020899 11.00000 0.02340 0.02436 = 0.02635 0.00166 0.00320 -0.00192 C7 1 0.735546 0.500659 0.098230 11.00000 0.02527 0.03245 = 0.02164 -0.00071 0.00349 0.00028 AFIX 43 H7 2 0.704190 0.531872 0.145887 11.00000 -1.20000 AFIX 0 C8 1 0.831686 0.402142 0.104899 11.00000 0.02633 0.03273 = 0.02371 0.00244 -0.00089 0.00265 AFIX 43 H8 2 0.867024 0.367339 0.157409 11.00000 -1.20000 AFIX 0 C9 1 0.583330 0.660373 0.013971 11.00000 0.02408 0.02628 = 0.02068 -0.00050 0.00276 -0.00308 C11 1 0.439499 0.818619 -0.019546 11.00000 0.02377 0.02543 = 0.02410 -0.00022 0.00210 -0.00195 C12 1 0.453247 0.803456 0.063214 11.00000 0.02119 0.02444 = 0.02449 0.00115 0.00022 -0.00008 C14 1 0.359596 0.910450 -0.077146 11.00000 0.02494 0.02777 = 0.02384 -0.00002 0.00198 -0.00249 C20 1 0.322898 0.982637 0.128543 11.00000 0.02989 0.03535 = 0.03187 0.00237 0.00585 0.00596 AFIX 43 H20 2 0.287791 1.040370 0.082036 11.00000 -1.20000 AFIX 0 C21 1 0.303306 1.004317 0.206642 11.00000 0.03371 0.03559 = 0.03654 -0.00597 0.01063 0.00156 AFIX 43 H21 2 0.251792 1.080058 0.224516 11.00000 -1.20000 AFIX 0 C22 1 0.373090 0.894224 0.257350 11.00000 0.03516 0.03901 = 0.02525 -0.00166 0.00771 -0.00365 AFIX 43 H22 2 0.376073 0.883062 0.314867 11.00000 -1.20000 AFIX 0 C23 1 0.434289 0.808475 0.209227 11.00000 0.03329 0.03416 = 0.02476 -0.00027 0.00505 -0.00014 AFIX 43 H23 2 0.488640 0.726969 0.227023 11.00000 -1.20000 AFIX 0 N10 3 0.524090 0.725479 -0.049911 11.00000 0.02444 0.02615 = 0.02498 -0.00054 0.00231 -0.00280 N15 3 0.359049 0.904057 -0.158181 11.00000 0.02936 0.03339 = 0.02613 -0.00106 -0.00217 0.00382 N16 3 0.275187 1.002166 -0.194449 11.00000 0.03533 0.04016 = 0.02707 0.00118 -0.00392 0.00687 N17 3 0.227638 1.065482 -0.135873 11.00000 0.03650 0.04197 = 0.02412 0.00083 -0.00235 0.00663 N18 3 0.277700 1.011876 -0.061440 11.00000 0.02775 0.03266 = 0.02883 0.00044 -0.00091 0.00317 N19 3 0.403771 0.860488 0.128600 11.00000 0.02546 0.02796 = 0.02286 0.00047 0.00235 -0.00002 O2 4 0.972584 0.255657 0.049835 11.00000 0.02964 0.04078 = 0.03340 0.00162 0.00566 0.01005 O13 4 0.544441 0.701673 0.085824 11.00000 0.02464 0.02860 = 0.02267 0.00046 0.00257 0.00158 H15 2 0.397164 0.843801 -0.191350 11.00000 0.03915 MOLE 2 O31 4 0.050140 1.249163 -0.224667 11.00000 0.03271 0.04063 = 0.03292 0.00519 -0.00129 0.00079 AFIX 147 H31 2 0.108578 1.215234 -0.193247 11.00000 -1.50000 AFIX 0 MOLE 3 C32 1 -0.030054 1.124952 -0.244907 11.00000 0.04927 0.05382 = 0.04234 0.00896 -0.00745 -0.01493 AFIX 137 H32A 2 -0.029495 1.054973 -0.197556 11.00000 -1.50000 H32B 2 -0.007697 1.064835 -0.290960 11.00000 -1.50000 H32C 2 -0.108761 1.168633 -0.260287 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2009src0518 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 C1 - O2 C3 - O2 C8 C4 C4 - C5 C3 C5 - C6 C4 C6 - C5 C7 C9 C7 - C8 C6 C8 - C7 C3 C9 - N10 O13 C6 C11 - C12 N10 C14 C12 - C11 O13 N19 C14 - N18 N15 C11 C20 - C21 N19 C21 - C20 C22 C22 - C23 C21 C23 - C22 N19 N10 - C9 C11 N15 - C14 N16 N16 - N17 N15 N17 - N16 N18 N18 - C14 N17 N19 - C12 C20 C23 O2 - C3 C1 O13 - C12 C9 O31 - C32 C32 - O31 Operators for generating equivalent atoms: $1 -x+1/2, y-1/2, -z-1/2 19788 Reflections read, of which 604 rejected -14 =< h =< 14, -10 =< k =< 10, -21 =< l =< 21, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) -7 7 7 8.12 2.50 3 13.94 1 Inconsistent equivalents 3644 Unique reflections, of which 0 suppressed R(int) = 0.0840 R(sigma) = 0.0789 Friedel opposites merged Maximum memory for data reduction = 2223 / 35923 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 = 2850 / 290106 wR2 = 0.1698 before cycle 1 for 3644 data and 234 / 234 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.027 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.031; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0765 * P )^2 + 0.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.43668 0.00149 0.419 OSF 2 0.01433 0.00267 0.014 EXTI Mean shift/su = 0.053 Maximum = 0.419 for OSF Max. shift = 0.006 A for H15 Max. dU = 0.000 for C32 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2850 / 290106 wR2 = 0.1697 before cycle 2 for 3644 data and 234 / 234 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.030 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.031; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0765 * P )^2 + 0.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.43682 0.00149 0.096 OSF 2 0.01436 0.00267 0.010 EXTI Mean shift/su = 0.019 Maximum = 0.104 for y C32 Max. shift = 0.002 A for H15 Max. dU = 0.000 for H15 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2850 / 290106 wR2 = 0.1698 before cycle 3 for 3644 data and 234 / 234 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.031 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.031; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0765 * P )^2 + 0.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.43683 0.00149 0.005 OSF 2 0.01436 0.00267 0.003 EXTI Mean shift/su = 0.001 Maximum = -0.008 for U23 C22 Max. shift = 0.000 A for H32A Max. dU = 0.000 for H15 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2850 / 290106 wR2 = 0.1697 before cycle 4 for 3644 data and 234 / 234 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.031 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.031; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0765 * P )^2 + 0.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.43683 0.00149 0.002 OSF 2 0.01437 0.00267 0.001 EXTI Mean shift/su = 0.000 Maximum = 0.003 for tors H32A Max. shift = 0.000 A for H32C Max. dU = 0.000 for H15 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 H1A 0.9679 0.1469 -0.0572 137 0.980 0.000 C1 O2 H1A H1B 1.0933 0.1410 -0.0015 137 0.980 0.000 C1 O2 H1A H1C 1.0492 0.3009 -0.0478 137 0.980 0.000 C1 O2 H1A H4 0.8576 0.3725 -0.0894 43 0.950 0.000 C4 C5 C3 H5 0.6955 0.5412 -0.1005 43 0.950 0.000 C5 C6 C4 H7 0.7042 0.5318 0.1459 43 0.950 0.000 C7 C8 C6 H8 0.8670 0.3673 0.1574 43 0.950 0.000 C8 C7 C3 H20 0.2878 1.0403 0.0820 43 0.950 0.000 C20 C21 N19 H21 0.2518 1.0801 0.2245 43 0.950 0.000 C21 C20 C22 H22 0.3761 0.8832 0.3149 43 0.950 0.000 C22 C23 C21 H23 0.4886 0.7270 0.2270 43 0.950 0.000 C23 C22 N19 H31 0.1086 1.2152 -0.1933 147 0.840 0.000 O31 C32 H31 H32A -0.0295 1.0551 -0.1975 137 0.980 0.000 C32 O31 H32A H32B -0.0077 1.0650 -0.2910 137 0.980 0.000 C32 O31 H32A H32C -0.1088 1.1688 -0.2602 137 0.980 0.000 C32 O31 H32A 2009src0518 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 1.02485 0.20730 -0.01964 1.00000 0.03816 0.03977 0.04014 0.00047 0.01185 0.00680 0.03875 0.00504 0.00023 0.00032 0.00016 0.00000 0.00137 0.00154 0.00156 0.00121 0.00116 0.00112 0.00063 H1A 0.96787 0.14691 -0.05719 1.00000 0.05812 0.00000 0.00000 H1B 1.09329 0.14104 -0.00146 1.00000 0.05812 0.00000 0.00000 H1C 1.04922 0.30085 -0.04784 1.00000 0.05812 0.00000 0.00000 C3 0.87737 0.35326 0.03563 1.00000 0.02456 0.02840 0.03145 0.00014 0.00192 0.00106 0.02835 0.00409 0.00019 0.00028 0.00015 0.00000 0.00112 0.00125 0.00131 0.00100 0.00096 0.00089 0.00054 C4 0.82677 0.40516 -0.04175 1.00000 0.03106 0.03089 0.02467 -0.00124 0.00712 -0.00081 0.02857 0.00422 0.00020 0.00028 0.00015 0.00000 0.00118 0.00133 0.00120 0.00100 0.00094 0.00097 0.00053 H4 0.85764 0.37249 -0.08935 1.00000 0.03428 0.00000 0.00000 C5 0.73037 0.50555 -0.04798 1.00000 0.02670 0.03172 0.02465 0.00211 0.00240 0.00098 0.02782 0.00416 0.00019 0.00028 0.00014 0.00000 0.00116 0.00130 0.00121 0.00098 0.00094 0.00092 0.00053 H5 0.69553 0.54118 -0.10046 1.00000 0.03338 0.00000 0.00000 C6 0.68409 0.55467 0.02089 1.00000 0.02345 0.02448 0.02645 0.00163 0.00321 -0.00195 0.02483 0.00396 0.00019 0.00026 0.00014 0.00000 0.00106 0.00122 0.00121 0.00094 0.00090 0.00086 0.00051 C7 0.73555 0.50058 0.09823 1.00000 0.02536 0.03253 0.02173 -0.00069 0.00350 0.00028 0.02653 0.00404 0.00019 0.00028 0.00014 0.00000 0.00112 0.00132 0.00115 0.00097 0.00090 0.00090 0.00052 H7 0.70420 0.53178 0.14589 1.00000 0.03184 0.00000 0.00000 C8 0.83165 0.40211 0.10489 1.00000 0.02644 0.03284 0.02378 0.00250 -0.00088 0.00265 0.02813 0.00410 0.00018 0.00029 0.00014 0.00000 0.00114 0.00134 0.00119 0.00099 0.00091 0.00094 0.00053 H8 0.86699 0.36730 0.15739 1.00000 0.03375 0.00000 0.00000 C9 0.58331 0.66035 0.01395 1.00000 0.02412 0.02641 0.02076 -0.00056 0.00276 -0.00314 0.02381 0.00381 0.00018 0.00027 0.00013 0.00000 0.00108 0.00122 0.00113 0.00092 0.00087 0.00088 0.00049 C11 0.43947 0.81861 -0.01955 1.00000 0.02383 0.02549 0.02423 -0.00020 0.00212 -0.00195 0.02465 0.00383 0.00018 0.00027 0.00013 0.00000 0.00110 0.00121 0.00119 0.00093 0.00090 0.00087 0.00051 C12 0.45322 0.80345 0.06319 1.00000 0.02126 0.02454 0.02458 0.00118 0.00025 -0.00006 0.02377 0.00386 0.00018 0.00026 0.00014 0.00000 0.00104 0.00118 0.00118 0.00094 0.00088 0.00084 0.00050 C14 0.35959 0.91040 -0.07715 1.00000 0.02500 0.02781 0.02391 -0.00001 0.00196 -0.00248 0.02573 0.00393 0.00018 0.00027 0.00014 0.00000 0.00111 0.00122 0.00119 0.00095 0.00089 0.00091 0.00051 C20 0.32289 0.98259 0.12854 1.00000 0.02997 0.03545 0.03197 0.00242 0.00589 0.00603 0.03232 0.00453 0.00020 0.00030 0.00015 0.00000 0.00120 0.00143 0.00136 0.00107 0.00101 0.00099 0.00057 H20 0.28776 1.04029 0.08203 1.00000 0.03879 0.00000 0.00000 C21 0.30330 1.00432 0.20664 1.00000 0.03379 0.03570 0.03659 -0.00589 0.01063 0.00162 0.03481 0.00450 0.00021 0.00031 0.00016 0.00000 0.00131 0.00142 0.00146 0.00114 0.00110 0.00104 0.00060 H21 0.25178 1.08007 0.22451 1.00000 0.04177 0.00000 0.00000 C22 0.37307 0.89429 0.25733 1.00000 0.03525 0.03918 0.02532 -0.00167 0.00775 -0.00358 0.03292 0.00437 0.00020 0.00031 0.00015 0.00000 0.00128 0.00147 0.00127 0.00106 0.00102 0.00105 0.00058 H22 0.37607 0.88316 0.31485 1.00000 0.03950 0.00000 0.00000 C23 0.43427 0.80850 0.20921 1.00000 0.03338 0.03429 0.02484 -0.00022 0.00506 -0.00014 0.03075 0.00421 0.00021 0.00030 0.00014 0.00000 0.00125 0.00137 0.00123 0.00104 0.00099 0.00101 0.00055 H23 0.48861 0.72699 0.22701 1.00000 0.03690 0.00000 0.00000 N10 0.52406 0.72548 -0.04992 1.00000 0.02450 0.02623 0.02510 -0.00053 0.00232 -0.00281 0.02540 0.00323 0.00015 0.00022 0.00012 0.00000 0.00096 0.00106 0.00102 0.00079 0.00079 0.00073 0.00045 N15 0.35906 0.90400 -0.15818 1.00000 0.02943 0.03341 0.02627 -0.00108 -0.00219 0.00381 0.03032 0.00351 0.00017 0.00025 0.00012 0.00000 0.00104 0.00117 0.00112 0.00089 0.00083 0.00085 0.00049 N16 0.27519 1.00211 -0.19445 1.00000 0.03537 0.04027 0.02718 0.00115 -0.00390 0.00679 0.03510 0.00380 0.00018 0.00026 0.00013 0.00000 0.00111 0.00125 0.00110 0.00095 0.00089 0.00090 0.00052 N17 0.22762 1.06545 -0.13588 1.00000 0.03660 0.04206 0.02422 0.00078 -0.00234 0.00653 0.03496 0.00372 0.00018 0.00026 0.00012 0.00000 0.00113 0.00129 0.00109 0.00094 0.00087 0.00092 0.00052 N18 0.27771 1.01180 -0.06144 1.00000 0.02785 0.03278 0.02892 0.00044 -0.00089 0.00315 0.03034 0.00350 0.00016 0.00024 0.00012 0.00000 0.00102 0.00114 0.00112 0.00088 0.00083 0.00080 0.00049 N19 0.40375 0.86049 0.12859 1.00000 0.02555 0.02804 0.02298 0.00049 0.00238 0.00000 0.02564 0.00330 0.00015 0.00022 0.00011 0.00000 0.00095 0.00105 0.00102 0.00080 0.00077 0.00077 0.00045 O2 0.97255 0.25565 0.04982 1.00000 0.02970 0.04089 0.03353 0.00161 0.00565 0.01005 0.03460 0.00316 0.00014 0.00021 0.00011 0.00000 0.00088 0.00104 0.00098 0.00077 0.00073 0.00071 0.00044 O13 0.54442 0.70166 0.08582 1.00000 0.02474 0.02872 0.02274 0.00045 0.00259 0.00156 0.02548 0.00264 0.00012 0.00018 0.00009 0.00000 0.00079 0.00088 0.00083 0.00067 0.00063 0.00063 0.00039 H15 0.39737 0.84300 -0.19122 1.00000 0.03897 0.04551 0.00208 0.00292 0.00146 0.00000 0.00759 O31 0.05012 1.24916 -0.22467 1.00000 0.03279 0.04069 0.03303 0.00520 -0.00133 0.00081 0.03610 0.00303 0.00014 0.00021 0.00010 0.00000 0.00094 0.00105 0.00103 0.00079 0.00075 0.00073 0.00045 H31 0.10857 1.21518 -0.19328 1.00000 0.05415 0.00000 0.00000 C32 -0.03005 1.12510 -0.24489 1.00000 0.04943 0.05384 0.04249 0.00895 -0.00748 -0.01491 0.04998 0.00493 0.00025 0.00037 0.00018 0.00000 0.00167 0.00188 0.00169 0.00138 0.00132 0.00136 0.00078 H32A -0.02949 1.05510 -0.19755 1.00000 0.07497 0.00000 0.00000 H32B -0.00774 1.06499 -0.29096 1.00000 0.07497 0.00000 0.00000 H32C -0.10875 1.16883 -0.26024 1.00000 0.07497 0.00000 0.00000 Final Structure Factor Calculation for 2009src0518 in P2(1)/n Total number of l.s. parameters = 234 Maximum vector length = 511 Memory required = 2616 / 22995 wR2 = 0.1698 before cycle 5 for 3644 data and 0 / 234 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.031 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.031; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0765 * P )^2 + 0.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0607 for 2346 Fo > 4sig(Fo) and 0.1033 for all 3644 data wR2 = 0.1698, GooF = S = 1.031, Restrained GooF = 1.031 for all data Occupancy sum of asymmetric unit = 25.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0477 0.0395 0.0290 C1 0.0324 0.0286 0.0240 C3 0.0327 0.0302 0.0228 C4 0.0323 0.0276 0.0236 C5 0.0281 0.0247 0.0217 C6 0.0326 0.0254 0.0216 C7 0.0338 0.0305 0.0201 C8 0.0286 0.0222 0.0206 C9 0.0271 0.0248 0.0221 C11 0.0274 0.0242 0.0198 C12 0.0295 0.0251 0.0226 C14 0.0399 0.0310 0.0260 C20 0.0427 0.0363 0.0255 C21 0.0416 0.0334 0.0237 C22 0.0343 0.0334 0.0246 C23 0.0285 0.0257 0.0221 N10 0.0385 0.0305 0.0220 N15 0.0469 0.0364 0.0220 N16 0.0475 0.0358 0.0216 N17 0.0358 0.0319 0.0233 N18 0.0281 0.0262 0.0227 N19 0.0469 0.0333 0.0237 O2 0.0293 0.0248 0.0224 O13 0.0443 0.0376 0.0264 O31 0.0775 0.0395 0.0329 C32 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.005 0.009 0.014 0.020 0.026 0.034 0.044 0.058 0.085 1.000 Number in group 391. 346. 392. 387. 345. 344. 360. 355. 358. 366. GooF 0.943 0.915 0.986 1.077 1.142 1.156 1.112 1.043 0.973 0.943 K 3.236 0.928 0.947 0.961 0.951 0.986 1.004 1.030 1.038 1.040 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.64 inf Number in group 365. 369. 371. 355. 364. 363. 363. 366. 362. 366. GooF 0.981 0.950 1.042 1.069 1.035 1.076 1.001 0.956 1.003 1.178 K 1.000 1.065 1.059 1.057 1.071 1.023 1.038 1.028 1.043 1.029 R1 0.330 0.232 0.216 0.158 0.123 0.093 0.060 0.056 0.052 0.043 Recommended weighting scheme: WGHT 0.0704 0.6303 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) -4 1 17 0.50 27.16 3.74 0.020 0.95 -9 8 2 9.65 60.35 3.72 0.030 0.82 -3 5 10 16.64 47.05 3.67 0.026 1.16 2 0 0 419.35 591.83 3.58 0.094 5.71 11 4 6 9.88 24.73 3.58 0.019 0.85 9 4 5 4.42 17.32 3.46 0.016 1.00 9 4 13 -8.55 31.57 3.44 0.022 0.78 -3 2 5 64.91 36.94 3.38 0.023 2.26 2 4 7 77.46 121.78 3.34 0.043 1.48 5 3 4 12.88 2.55 3.22 0.006 1.57 -8 5 4 19.60 44.25 3.21 0.026 1.08 7 1 13 15.24 34.55 3.19 0.023 0.93 -2 6 10 15.43 46.17 3.16 0.026 1.07 4 10 0 -4.07 36.00 3.13 0.023 0.81 1 2 7 48.22 26.73 3.10 0.020 1.97 9 7 0 41.47 85.37 3.08 0.036 0.88 10 4 1 78.84 118.85 3.04 0.042 1.00 8 7 1 67.78 109.90 3.04 0.040 0.92 -6 3 16 94.74 40.94 2.98 0.025 0.91 11 6 6 32.45 96.39 2.96 0.038 0.77 3 1 5 84.30 57.84 2.93 0.029 2.24 8 6 2 65.29 98.46 2.91 0.038 0.98 -5 3 14 107.13 62.75 2.90 0.031 1.03 -1 2 9 231.90 172.73 2.87 0.051 1.68 -1 9 9 438.34 308.74 2.83 0.068 0.84 4 2 13 26.06 48.82 2.82 0.027 1.06 -3 3 13 21.45 0.13 2.81 0.001 1.14 -10 3 9 -8.24 7.88 2.81 0.011 0.97 -4 4 18 42.47 0.49 2.78 0.003 0.83 2 3 7 184.69 135.44 2.75 0.045 1.66 -5 3 10 200.86 144.33 2.74 0.046 1.28 8 7 5 -7.37 11.91 2.73 0.013 0.87 9 5 1 -2.72 8.20 2.72 0.011 1.01 -10 5 3 68.31 104.42 2.68 0.039 0.95 -10 5 7 11.15 34.02 2.68 0.022 0.92 -1 0 9 255.70 344.30 2.68 0.072 1.83 -1 1 4 535.59 679.42 2.67 0.100 3.64 4 4 9 26.77 46.24 2.67 0.026 1.19 -5 8 4 53.93 85.66 2.66 0.036 0.95 -12 2 2 12.36 25.23 2.64 0.019 0.94 -1 0 5 1755.43 2243.06 2.64 0.183 3.27 -1 4 10 10.25 29.41 2.64 0.021 1.30 0 1 12 26.48 10.82 2.62 0.013 1.34 4 6 12 240.07 173.37 2.62 0.051 0.90 4 3 0 65.15 44.80 2.61 0.026 2.01 -12 4 3 40.24 69.32 2.61 0.032 0.88 1 3 4 129.78 95.95 2.61 0.038 2.24 -9 0 15 49.47 10.77 2.60 0.013 0.89 -1 7 15 36.27 80.62 2.59 0.035 0.81 4 1 13 46.27 72.05 2.58 0.033 1.08 Bond lengths and angles C1 - Distance Angles O2 1.4310 (0.0030) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - O2 H1A H1B C3 - Distance Angles O2 1.3677 (0.0027) C8 1.3899 (0.0033) 115.49 (0.20) C4 1.3966 (0.0033) 124.47 (0.22) 120.04 (0.21) C3 - O2 C8 C4 - Distance Angles C5 1.3923 (0.0033) C3 1.3966 (0.0033) 118.93 (0.22) H4 0.9500 120.54 120.54 C4 - C5 C3 C5 - Distance Angles C6 1.3883 (0.0032) C4 1.3923 (0.0033) 121.36 (0.21) H5 0.9500 119.32 119.32 C5 - C6 C4 C6 - Distance Angles C5 1.3883 (0.0032) C7 1.4048 (0.0032) 118.99 (0.21) C9 1.4590 (0.0031) 121.09 (0.20) 119.92 (0.21) C6 - C5 C7 C7 - Distance Angles C8 1.3793 (0.0031) C6 1.4048 (0.0032) 119.92 (0.22) H7 0.9500 120.04 120.04 C7 - C8 C6 C8 - Distance Angles C7 1.3793 (0.0031) C3 1.3899 (0.0033) 120.74 (0.21) H8 0.9500 119.63 119.63 C8 - C7 C3 C9 - Distance Angles N10 1.2943 (0.0028) O13 1.3734 (0.0026) 113.28 (0.19) C6 1.4590 (0.0031) 130.29 (0.21) 116.42 (0.18) C9 - N10 O13 C11 - Distance Angles C12 1.3584 (0.0031) N10 1.4030 (0.0029) 108.69 (0.19) C14 1.4507 (0.0030) 132.87 (0.21) 118.42 (0.20) C11 - C12 N10 C12 - Distance Angles C11 1.3584 (0.0031) O13 1.3699 (0.0026) 107.87 (0.19) N19 1.3798 (0.0029) 138.83 (0.20) 113.30 (0.18) C12 - C11 O13 C14 - Distance Angles N18 1.3298 (0.0030) N15 1.3382 (0.0030) 108.70 (0.20) C11 1.4507 (0.0030) 128.33 (0.21) 122.97 (0.21) C14 - N18 N15 C20 - Distance Angles C21 1.3536 (0.0034) N19 1.3925 (0.0030) 107.74 (0.21) H20 0.9500 126.13 126.13 C20 - C21 N19 C21 - Distance Angles C20 1.3536 (0.0034) C22 1.4217 (0.0036) 108.25 (0.22) H21 0.9500 125.87 125.87 C21 - C20 C22 C22 - Distance Angles C23 1.3491 (0.0034) C21 1.4217 (0.0036) 107.83 (0.22) H22 0.9500 126.09 126.09 C22 - C23 C21 C23 - Distance Angles C22 1.3491 (0.0034) N19 1.3978 (0.0029) 108.07 (0.22) H23 0.9500 125.97 125.97 C23 - C22 N19 N10 - Distance Angles C9 1.2943 (0.0028) C11 1.4030 (0.0029) 105.14 (0.19) N10 - C9 N15 - Distance Angles C14 1.3382 (0.0030) N16 1.3482 (0.0027) 108.56 (0.20) H15 0.9108 (0.0168) 133.58 (1.73) 117.58 (1.71) N15 - C14 N16 N16 - Distance Angles N17 1.2954 (0.0029) N15 1.3482 (0.0028) 106.15 (0.19) N16 - N17 N17 - Distance Angles N16 1.2954 (0.0029) N18 1.3584 (0.0027) 111.48 (0.19) N17 - N16 N18 - Distance Angles C14 1.3298 (0.0030) N17 1.3584 (0.0027) 105.12 (0.19) N18 - C14 N19 - Distance Angles C12 1.3798 (0.0029) C20 1.3925 (0.0030) 127.78 (0.19) C23 1.3978 (0.0029) 124.01 (0.19) 108.10 (0.19) N19 - C12 C20 O2 - Distance Angles C3 1.3677 (0.0027) C1 1.4310 (0.0030) 117.22 (0.19) O2 - C3 O13 - Distance Angles C12 1.3699 (0.0026) C9 1.3734 (0.0026) 105.01 (0.16) O13 - C12 O31 - Distance Angles C32 1.4075 (0.0031) H31 0.8400 109.47 O31 - C32 C32 - Distance Angles O31 1.4075 (0.0031) H32A 0.9800 109.47 H32B 0.9800 109.47 109.47 H32C 0.9800 109.47 109.47 109.47 C32 - O31 H32A H32B Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.911(17) 1.781(18) 2.673(3) 166(3) N15-H15...O31_$1 0.84 2.00 2.810(3) 160.6 O31-H31...N17 0.84 2.64 3.316(3) 138.7 O31-H31...N16 FMAP and GRID set by program FMAP 2 3 21 GRID -1.389 -2 -2 1.389 2 2 R1 = 0.1033 for 3644 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.29 at 0.4797 0.2627 0.1289 [ 1.30 A from N10 ] Deepest hole -0.28 at 0.5090 0.4045 0.2244 [ 0.39 A from H32B ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2559 / 19260 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5203 0.7373 -0.1289 1.00000 0.05 0.29 1.30 N10 1.86 H15 1.96 H32B 2.26 C11 Q2 1 0.6981 0.4655 -0.0011 1.00000 0.05 0.26 0.86 C6 0.97 C5 1.66 C7 1.76 H5 Q3 1 0.2778 0.9781 0.0808 1.00000 0.05 0.26 0.54 H20 0.88 C20 1.84 N19 2.07 C21 Q4 1 0.0384 1.2672 -0.1347 1.00000 0.05 0.25 1.42 H31 1.45 H1C 1.52 O31 1.91 H1A Q5 1 0.4125 0.7848 0.0143 1.00000 0.05 0.25 0.74 C11 0.89 C12 1.85 N10 1.87 C14 Q6 1 0.5252 0.6604 -0.0499 1.00000 0.05 0.25 0.55 N10 1.16 C9 1.78 C11 2.22 C6 Q7 1 0.9833 0.2629 0.1363 1.00000 0.05 0.24 1.42 O2 1.68 H8 1.99 H22 2.06 C3 Q8 1 0.2787 0.9527 0.1618 1.00000 0.05 0.24 0.84 C20 0.87 C21 1.53 H20 1.56 H21 Q9 1 0.8906 0.3015 0.1785 1.00000 0.05 0.24 0.69 H8 1.56 C8 2.04 H23 2.38 C3 Q10 1 0.5245 0.7284 0.2096 1.00000 0.05 0.24 0.54 H23 1.24 C23 2.10 O13 2.11 N19 Shortest distances between peaks (including symmetry equivalents) 3 8 1.35 7 9 1.40 1 6 1.45 9 10 2.06 5 6 2.08 2 5 2.47 7 10 2.58 3 5 2.61 2 6 2.62 1 5 2.86 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. 0.91: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.83: Structure factors and derivatives 1.33: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.16: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0518 finished at 13:41:29 Total CPU time: 3.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++