+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src1307p21c started at 08:45:17 on 02-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src1307p21c in P2(1)/c CELL 0.71073 14.4770 11.2719 9.0254 90.000 102.352 90.000 ZERR 4.00 0.0005 0.0004 0.0003 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 60 96 8 8 V = 1438.70 F(000) = 576.0 Mu = 0.08 mm-1 Cell Wt = 1057.45 Rho = 1.220 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 EQIV_$1 -x, y-1/2, -z+3/2 HTAB N1 O24_$1 EQIV_$2 x, y, z+1 HTAB N1 O23_$2 EQIV_$3 -x, -y, -z+1 HTAB N9 O24_$3 HTAB N1 O23_$3 FMAP 2 PLAN 10 SIZE 0.01 0.07 0.16 ACTA BOND $H WGHT 0.00000 2.31070 L.S. 4 TEMP -153.00 FVAR 0.58940 MOLE 1 C2 1 -0.220936 0.015050 0.994539 11.00000 0.01986 0.01986 = 0.02306 -0.00102 0.00320 0.00306 AFIX 23 H2A 2 -0.215168 0.089334 0.938698 11.00000 -1.20000 H2B 2 -0.245683 0.036015 1.085259 11.00000 -1.20000 AFIX 0 C3 1 -0.292265 -0.066919 0.892622 11.00000 0.01868 0.02015 = 0.01569 0.00086 0.00437 -0.00024 C4 1 -0.390493 -0.010713 0.881092 11.00000 0.02361 0.02302 = 0.02071 -0.00074 0.00642 0.00445 AFIX 23 H4A 2 -0.402931 -0.002329 0.984260 11.00000 -1.20000 H4B 2 -0.390687 0.069692 0.836890 11.00000 -1.20000 AFIX 0 C5 1 -0.469428 -0.083915 0.784099 11.00000 0.02117 0.03686 = 0.02616 0.00190 0.00503 0.00033 AFIX 23 H5A 2 -0.458363 -0.091856 0.680039 11.00000 -1.20000 H5B 2 -0.530968 -0.043791 0.777898 11.00000 -1.20000 AFIX 0 C6 1 -0.471290 -0.206806 0.855801 11.00000 0.02502 0.03710 = 0.03555 0.00751 0.00425 -0.00671 AFIX 23 H6A 2 -0.489235 -0.198727 0.955188 11.00000 -1.20000 H6B 2 -0.519625 -0.256496 0.789770 11.00000 -1.20000 AFIX 0 C7 1 -0.375572 -0.267499 0.877850 11.00000 0.02914 0.02234 = 0.02840 0.00199 0.00602 -0.00753 AFIX 23 H7A 2 -0.363024 -0.288046 0.777337 11.00000 -1.20000 H7B 2 -0.377424 -0.342293 0.934644 11.00000 -1.20000 AFIX 0 C8 1 -0.294703 -0.190072 0.963599 11.00000 0.02309 0.02289 = 0.01889 0.00234 0.00422 -0.00201 AFIX 23 H8A 2 -0.233859 -0.230713 0.965329 11.00000 -1.20000 H8B 2 -0.301492 -0.180859 1.069836 11.00000 -1.20000 AFIX 0 C10 1 -0.258007 -0.004028 0.634526 11.00000 0.02155 0.01625 = 0.01891 -0.00141 0.00158 -0.00594 C11 1 -0.191164 -0.024166 0.545716 11.00000 0.02841 0.01779 = 0.02213 -0.00042 0.00671 0.00323 AFIX 43 H11 2 -0.148806 -0.089183 0.569237 11.00000 -1.20000 AFIX 0 C12 1 -0.185484 0.048502 0.424590 11.00000 0.03263 0.02865 = 0.02444 0.00021 0.01214 -0.00051 AFIX 43 H12 2 -0.139547 0.032531 0.366186 11.00000 -1.20000 AFIX 0 C13 1 -0.246126 0.144636 0.387163 11.00000 0.03641 0.02691 = 0.01885 0.00598 0.00392 -0.00339 AFIX 43 H13 2 -0.243015 0.194015 0.303069 11.00000 -1.20000 AFIX 0 C14 1 -0.310791 0.166063 0.475674 11.00000 0.02834 0.01918 = 0.03418 0.00489 0.00326 0.00089 AFIX 43 H14 2 -0.351819 0.232458 0.453201 11.00000 -1.20000 AFIX 0 C15 1 -0.317706 0.093498 0.596612 11.00000 0.02730 0.02303 = 0.03072 0.00452 0.01141 0.00274 AFIX 43 H15 2 -0.363728 0.110355 0.654550 11.00000 -1.20000 AFIX 0 N1 3 -0.125329 -0.038441 1.044630 11.00000 0.02194 0.01872 = 0.02244 0.00011 0.00409 -0.00173 AFIX 137 H1A 2 -0.128005 -0.098468 1.111004 11.00000 -1.50000 H1B 2 -0.084046 0.017909 1.090872 11.00000 -1.50000 H1C 2 -0.105491 -0.067465 0.962635 11.00000 -1.50000 AFIX 0 N9 3 -0.265405 -0.087481 0.745834 11.00000 0.02392 0.01547 = 0.01953 0.00239 0.00782 0.00391 H9 2 -0.222017 -0.144040 0.753470 11.00000 -1.20000 MOLE 2 C21 1 -0.053511 0.288425 0.250137 11.00000 0.02240 0.03074 = 0.03430 -0.00788 0.00471 0.00045 AFIX 137 H21A 2 -0.058655 0.265255 0.352716 11.00000 -1.50000 H21B 2 -0.111303 0.265464 0.177695 11.00000 -1.50000 H21C 2 -0.045024 0.374540 0.246238 11.00000 -1.50000 AFIX 0 C22 1 0.030275 0.226897 0.209757 11.00000 0.02379 0.02030 = 0.01737 0.00145 0.00338 0.00100 O23 4 0.016525 0.126611 0.145400 11.00000 0.02576 0.02210 = 0.02784 -0.00593 0.00533 -0.00394 O24 4 0.110023 0.276428 0.243514 11.00000 0.02130 0.02102 = 0.02954 -0.00298 0.00559 -0.00185 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 2008src1307p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C2 - N1 C3 C3 - N9 C8 C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C7 C5 C7 - C6 C8 C8 - C7 C3 C10 - C15 N9 C11 C11 - C12 C10 C12 - C11 C13 C13 - C14 C12 C14 - C13 C15 C15 - C14 C10 N1 - C2 N9 - C10 C3 C21 - C22 C22 - O24 O23 C21 O23 - C22 O24 - C22 Operators for generating equivalent atoms: $1 -x, y-1/2, -z+3/2 $2 x, y, z+1 $3 -x, -y, -z+1 h k l Fo^2 Sigma Why rejected 14 0 3 19.97 4.85 observed but should be systematically absent 16167 Reflections read, of which 501 rejected -18 =< h =< 18, -14 =< k =< 14, -11 =< l =< 11, Max. 2-theta = 54.97 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) -14 5 1 15.55 3.32 2 17.80 -10 10 2 8.87 3.52 2 23.12 -7 10 2 3.03 5.10 2 28.07 -12 7 3 6.81 2.77 2 14.42 11 9 3 7.36 2.63 2 22.65 10 11 3 2.20 2.63 2 15.64 12 1 5 -5.41 2.20 2 17.35 12 3 5 3.04 1.97 4 11.43 12 2 6 3.97 2.10 2 14.41 5 2 7 0.85 1.15 4 6.16 -2 8 7 0.18 0.29 4 1.83 3 2 10 4.18 4.49 3 23.17 3 5 10 11.98 5.18 2 27.73 -1 7 10 1.34 2.07 3 11.36 14 Inconsistent equivalents 3269 Unique reflections, of which 0 suppressed R(int) = 0.1104 R(sigma) = 0.0993 Friedel opposites merged Maximum memory for data reduction = 2336 / 32458 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 = 2885 / 219996 wR2 = 0.1525 before cycle 1 for 3269 data and 177 / 177 parameters GooF = S = 1.115; Restrained GooF = 1.115 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.58941 0.00140 0.004 OSF Mean shift/su = 0.001 Maximum = 0.005 for U12 C14 Max. shift = 0.000 A for H9 Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2885 / 219996 wR2 = 0.1525 before cycle 2 for 3269 data and 177 / 177 parameters GooF = S = 1.115; Restrained GooF = 1.115 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.58941 0.00140 0.000 OSF Mean shift/su = 0.000 Maximum = 0.002 for U12 C14 Max. shift = 0.000 A for H9 Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2885 / 219996 wR2 = 0.1525 before cycle 3 for 3269 data and 177 / 177 parameters GooF = S = 1.115; Restrained GooF = 1.115 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.58940 0.00140 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H9 Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2885 / 219996 wR2 = 0.1525 before cycle 4 for 3269 data and 177 / 177 parameters GooF = S = 1.115; Restrained GooF = 1.115 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.58941 0.00140 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z N1 Max. shift = 0.000 A for H21A Max. dU = 0.000 for C21 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 H2A -0.2152 0.0893 0.9387 23 0.990 0.000 C2 N1 C3 H2B -0.2457 0.0360 1.0853 23 0.990 0.000 C2 N1 C3 H4A -0.4029 -0.0023 0.9843 23 0.990 0.000 C4 C5 C3 H4B -0.3907 0.0697 0.8369 23 0.990 0.000 C4 C5 C3 H5A -0.4584 -0.0919 0.6800 23 0.990 0.000 C5 C4 C6 H5B -0.5310 -0.0438 0.7779 23 0.990 0.000 C5 C4 C6 H6A -0.4892 -0.1987 0.9552 23 0.990 0.000 C6 C7 C5 H6B -0.5196 -0.2565 0.7898 23 0.990 0.000 C6 C7 C5 H7A -0.3630 -0.2880 0.7773 23 0.990 0.000 C7 C6 C8 H7B -0.3774 -0.3423 0.9346 23 0.990 0.000 C7 C6 C8 H8A -0.2339 -0.2307 0.9653 23 0.990 0.000 C8 C7 C3 H8B -0.3015 -0.1809 1.0698 23 0.990 0.000 C8 C7 C3 H11 -0.1488 -0.0892 0.5692 43 0.950 0.000 C11 C12 C10 H12 -0.1395 0.0325 0.3662 43 0.950 0.000 C12 C11 C13 H13 -0.2430 0.1940 0.3031 43 0.950 0.000 C13 C14 C12 H14 -0.3518 0.2325 0.4532 43 0.950 0.000 C14 C13 C15 H15 -0.3637 0.1104 0.6545 43 0.950 0.000 C15 C14 C10 H1A -0.1280 -0.0985 1.1110 137 0.910 0.000 N1 C2 H1A H1B -0.0840 0.0179 1.0909 137 0.910 0.000 N1 C2 H1A H1C -0.1055 -0.0675 0.9626 137 0.910 0.000 N1 C2 H1A H21A -0.0587 0.2653 0.3527 137 0.980 0.000 C21 C22 H21A H21B -0.1113 0.2655 0.1777 137 0.980 0.000 C21 C22 H21A H21C -0.0450 0.3745 0.2462 137 0.980 0.000 C21 C22 H21A 2008src1307p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 -0.22094 0.01505 0.99454 1.00000 0.01986 0.01986 0.02306 -0.00102 0.00320 0.00306 0.02113 0.00518 0.00019 0.00026 0.00031 0.00000 0.00146 0.00150 0.00147 0.00113 0.00110 0.00121 0.00061 H2A -0.21517 0.08933 0.93870 1.00000 0.02536 0.00000 0.00000 H2B -0.24568 0.03602 1.08526 1.00000 0.02536 0.00000 0.00000 C3 -0.29226 -0.06692 0.89262 1.00000 0.01868 0.02016 0.01569 0.00086 0.00437 -0.00024 0.01807 0.00505 0.00019 0.00025 0.00029 0.00000 0.00137 0.00147 0.00130 0.00107 0.00103 0.00117 0.00058 C4 -0.39049 -0.01071 0.88109 1.00000 0.02361 0.02302 0.02071 -0.00074 0.00642 0.00445 0.02219 0.00532 0.00019 0.00026 0.00031 0.00000 0.00155 0.00159 0.00146 0.00114 0.00115 0.00126 0.00064 H4A -0.40293 -0.00233 0.98426 1.00000 0.02663 0.00000 0.00000 H4B -0.39069 0.06969 0.83689 1.00000 0.02663 0.00000 0.00000 C5 -0.46943 -0.08391 0.78410 1.00000 0.02117 0.03686 0.02616 0.00190 0.00503 0.00033 0.02807 0.00563 0.00021 0.00029 0.00033 0.00000 0.00154 0.00187 0.00161 0.00135 0.00119 0.00140 0.00070 H5A -0.45836 -0.09186 0.68004 1.00000 0.03368 0.00000 0.00000 H5B -0.53097 -0.04379 0.77790 1.00000 0.03368 0.00000 0.00000 C6 -0.47129 -0.20681 0.85580 1.00000 0.02502 0.03710 0.03555 0.00751 0.00425 -0.00671 0.03289 0.00627 0.00022 0.00030 0.00037 0.00000 0.00167 0.00195 0.00181 0.00146 0.00130 0.00148 0.00076 H6A -0.48923 -0.19873 0.95519 1.00000 0.03947 0.00000 0.00000 H6B -0.51962 -0.25650 0.78977 1.00000 0.03947 0.00000 0.00000 C7 -0.37557 -0.26750 0.87785 1.00000 0.02915 0.02234 0.02840 0.00199 0.00602 -0.00753 0.02665 0.00555 0.00021 0.00027 0.00034 0.00000 0.00164 0.00159 0.00164 0.00125 0.00125 0.00135 0.00067 H7A -0.36302 -0.28805 0.77734 1.00000 0.03198 0.00000 0.00000 H7B -0.37742 -0.34229 0.93464 1.00000 0.03198 0.00000 0.00000 C8 -0.29470 -0.19007 0.96360 1.00000 0.02309 0.02289 0.01888 0.00235 0.00423 -0.00201 0.02166 0.00527 0.00020 0.00025 0.00030 0.00000 0.00154 0.00154 0.00140 0.00114 0.00111 0.00126 0.00062 H8A -0.23386 -0.23071 0.96533 1.00000 0.02599 0.00000 0.00000 H8B -0.30149 -0.18086 1.06984 1.00000 0.02599 0.00000 0.00000 C10 -0.25801 -0.00403 0.63453 1.00000 0.02155 0.01625 0.01891 -0.00142 0.00158 -0.00594 0.01931 0.00496 0.00020 0.00024 0.00030 0.00000 0.00145 0.00142 0.00138 0.00106 0.00108 0.00115 0.00060 C11 -0.19116 -0.02417 0.54572 1.00000 0.02842 0.01779 0.02213 -0.00042 0.00671 0.00323 0.02258 0.00540 0.00021 0.00026 0.00030 0.00000 0.00161 0.00144 0.00146 0.00118 0.00116 0.00127 0.00062 H11 -0.14881 -0.08918 0.56924 1.00000 0.02710 0.00000 0.00000 C12 -0.18548 0.04850 0.42459 1.00000 0.03263 0.02865 0.02444 0.00021 0.01214 -0.00051 0.02767 0.00575 0.00022 0.00028 0.00032 0.00000 0.00175 0.00171 0.00154 0.00128 0.00126 0.00141 0.00069 H12 -0.13955 0.03253 0.36619 1.00000 0.03321 0.00000 0.00000 C13 -0.24613 0.14464 0.38716 1.00000 0.03641 0.02691 0.01885 0.00598 0.00392 -0.00339 0.02769 0.00574 0.00023 0.00028 0.00032 0.00000 0.00182 0.00167 0.00145 0.00124 0.00123 0.00141 0.00070 H13 -0.24301 0.19401 0.30307 1.00000 0.03322 0.00000 0.00000 C14 -0.31079 0.16606 0.47567 1.00000 0.02834 0.01918 0.03418 0.00489 0.00326 0.00090 0.02775 0.00575 0.00022 0.00027 0.00034 0.00000 0.00172 0.00157 0.00172 0.00127 0.00131 0.00129 0.00069 H14 -0.35182 0.23246 0.45320 1.00000 0.03329 0.00000 0.00000 C15 -0.31771 0.09350 0.59661 1.00000 0.02730 0.02303 0.03072 0.00452 0.01141 0.00274 0.02624 0.00576 0.00021 0.00027 0.00033 0.00000 0.00163 0.00159 0.00165 0.00126 0.00127 0.00133 0.00067 H15 -0.36373 0.11035 0.65455 1.00000 0.03149 0.00000 0.00000 N1 -0.12533 -0.03844 1.04463 1.00000 0.02194 0.01872 0.02244 0.00011 0.00409 -0.00173 0.02113 0.00431 0.00016 0.00021 0.00025 0.00000 0.00128 0.00125 0.00122 0.00099 0.00094 0.00102 0.00053 H1A -0.12801 -0.09847 1.11100 1.00000 0.03170 0.00000 0.00000 H1B -0.08405 0.01791 1.09087 1.00000 0.03170 0.00000 0.00000 H1C -0.10549 -0.06746 0.96263 1.00000 0.03170 0.00000 0.00000 N9 -0.26540 -0.08748 0.74583 1.00000 0.02392 0.01547 0.01953 0.00239 0.00782 0.00391 0.01916 0.00445 0.00017 0.00021 0.00025 0.00000 0.00129 0.00124 0.00121 0.00094 0.00095 0.00104 0.00051 H9 -0.22202 -0.14404 0.75347 1.00000 0.02300 0.05612 0.00219 0.00289 0.00321 0.00000 0.00000 C21 -0.05351 0.28842 0.25014 1.00000 0.02240 0.03074 0.03430 -0.00788 0.00471 0.00045 0.02935 0.00577 0.00021 0.00030 0.00035 0.00000 0.00160 0.00178 0.00173 0.00137 0.00126 0.00139 0.00071 H21A -0.05866 0.26525 0.35271 1.00000 0.04402 0.00000 0.00000 H21B -0.11130 0.26547 0.17769 1.00000 0.04402 0.00000 0.00000 H21C -0.04502 0.37454 0.24624 1.00000 0.04402 0.00000 0.00000 C22 0.03027 0.22690 0.20976 1.00000 0.02379 0.02030 0.01737 0.00145 0.00338 0.00100 0.02064 0.00534 0.00020 0.00026 0.00030 0.00000 0.00152 0.00148 0.00138 0.00113 0.00108 0.00128 0.00060 O23 0.01653 0.12661 0.14540 1.00000 0.02576 0.02210 0.02784 -0.00593 0.00533 -0.00394 0.02529 0.00366 0.00014 0.00018 0.00022 0.00000 0.00109 0.00110 0.00109 0.00085 0.00084 0.00092 0.00047 O24 0.11002 0.27643 0.24351 1.00000 0.02130 0.02102 0.02954 -0.00298 0.00559 -0.00185 0.02393 0.00364 0.00014 0.00018 0.00022 0.00000 0.00108 0.00107 0.00113 0.00087 0.00082 0.00091 0.00046 Final Structure Factor Calculation for 2008src1307p21c in P2(1)/c Total number of l.s. parameters = 177 Maximum vector length = 511 Memory required = 2708 / 22995 wR2 = 0.1525 before cycle 5 for 3269 data and 0 / 177 parameters GooF = S = 1.115; Restrained GooF = 1.115 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.31 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0838 for 2051 Fo > 4sig(Fo) and 0.1550 for all 3269 data wR2 = 0.1525, GooF = S = 1.115, Restrained GooF = 1.115 for all data Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0253 0.0213 0.0168 C2 0.0203 0.0187 0.0152 C3 0.0278 0.0217 0.0171 C4 0.0372 0.0259 0.0211 C5 0.0474 0.0299 0.0214 C6 0.0348 0.0284 0.0167 C7 0.0260 0.0215 0.0175 C8 0.0265 0.0195 0.0120 C10 0.0293 0.0219 0.0166 C11 0.0348 0.0287 0.0196 C12 0.0394 0.0282 0.0154 C13 0.0377 0.0279 0.0176 C14 0.0355 0.0224 0.0208 C15 0.0235 0.0220 0.0180 N1 0.0266 0.0170 0.0139 N9 0.0413 0.0244 0.0223 C21 0.0244 0.0208 0.0167 C22 0.0317 0.0266 0.0175 O23 0.0305 0.0222 0.0191 O24 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.015 0.022 0.030 0.040 0.051 0.063 0.084 0.122 1.000 Number in group 337. 360. 294. 324. 334. 332. 311. 327. 324. 326. GooF 1.181 1.144 1.172 1.208 1.241 1.137 1.037 1.048 0.972 0.969 K 25.249 3.884 1.630 1.251 1.087 0.979 0.998 0.994 1.004 1.004 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 331. 337. 318. 332. 318. 331. 323. 330. 326. 323. GooF 1.321 1.246 1.236 1.121 1.124 1.019 0.997 0.862 1.029 1.120 K 1.354 1.293 1.174 0.984 1.053 0.997 0.990 1.007 1.011 1.001 R1 0.407 0.349 0.289 0.240 0.179 0.133 0.080 0.069 0.069 0.040 Recommended weighting scheme: WGHT 0.0000 2.3125 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) 8 4 8 -50.89 209.51 4.13 0.086 0.82 -1 11 3 213.58 371.64 3.93 0.115 0.97 10 6 2 -9.01 36.87 3.90 0.036 1.05 9 7 6 111.42 0.07 3.70 0.002 0.83 1 8 2 49.50 3.59 3.50 0.011 1.33 -2 1 8 42.11 0.12 3.42 0.002 1.12 6 8 7 9.60 57.62 3.39 0.045 0.83 14 4 1 -15.60 53.76 3.38 0.044 0.93 -5 10 6 60.43 133.84 3.37 0.069 0.89 -7 3 10 65.39 6.78 3.35 0.015 0.86 -4 13 3 63.40 14.32 3.30 0.022 0.82 -11 6 7 16.77 86.29 3.21 0.055 0.89 -9 9 8 -25.35 39.35 3.21 0.037 0.79 1 11 2 93.12 40.49 3.14 0.038 0.99 3 8 7 57.01 14.70 3.13 0.023 0.89 11 8 5 95.25 16.77 3.12 0.024 0.79 -3 0 6 228.01 121.07 3.06 0.065 1.50 -17 0 6 135.35 50.14 3.04 0.042 0.80 9 11 0 27.42 0.68 3.03 0.005 0.86 -5 2 11 70.40 8.51 3.00 0.017 0.81 -3 10 7 73.70 27.74 2.97 0.031 0.85 -7 12 2 296.54 160.66 2.91 0.075 0.85 -1 2 1 7556.24 8241.85 2.90 0.540 4.67 5 7 5 -1.50 27.81 2.90 0.031 1.04 -5 4 10 16.72 61.94 2.89 0.047 0.86 10 10 4 54.85 13.93 2.85 0.022 0.78 4 1 10 42.03 0.05 2.83 0.001 0.81 -12 9 6 86.83 0.18 2.79 0.003 0.80 -6 0 6 19.48 1.22 2.79 0.007 1.39 -11 0 10 -14.13 18.44 2.75 0.026 0.81 -7 4 11 6.83 114.67 2.75 0.064 0.78 -15 1 7 36.19 5.89 2.75 0.014 0.84 -14 7 5 8.34 57.17 2.74 0.045 0.83 -13 9 5 -31.97 34.48 2.72 0.035 0.80 -1 9 6 64.73 19.56 2.70 0.026 0.96 -3 5 11 93.16 14.30 2.66 0.022 0.77 5 11 6 -17.68 23.23 2.65 0.029 0.78 2 8 1 76.86 30.98 2.64 0.033 1.36 0 6 10 63.53 7.86 2.61 0.017 0.80 0 1 9 -2.80 54.96 2.58 0.044 0.98 -18 4 3 63.35 9.19 2.56 0.018 0.77 6 0 10 92.20 5.31 2.56 0.014 0.77 -3 0 2 341.52 263.13 2.56 0.096 3.63 -9 6 7 28.02 6.09 2.54 0.015 0.95 7 2 8 -91.73 78.77 2.53 0.053 0.88 -16 5 4 243.55 34.71 2.51 0.035 0.83 4 10 7 175.07 0.19 2.51 0.003 0.79 8 6 8 275.45 1.35 2.51 0.007 0.78 10 1 4 71.08 124.64 2.49 0.066 1.08 -13 1 8 17.41 1.86 2.48 0.008 0.87 Bond lengths and angles C2 - Distance Angles N1 1.4886 (0.0034) C3 1.5361 (0.0038) 113.61 (0.23) H2A 0.9900 108.84 108.84 H2B 0.9900 108.84 108.84 107.70 C2 - N1 C3 H2A C3 - Distance Angles N9 1.4767 (0.0032) C8 1.5324 (0.0038) 105.48 (0.21) C2 1.5361 (0.0038) 111.06 (0.22) 111.54 (0.22) C4 1.5398 (0.0038) 114.87 (0.22) 107.30 (0.22) 106.61 (0.22) C3 - N9 C8 C2 C4 - Distance Angles C5 1.5248 (0.0040) C3 1.5398 (0.0038) 112.58 (0.23) H4A 0.9900 109.08 109.08 H4B 0.9900 109.08 109.08 107.83 C4 - C5 C3 H4A C5 - Distance Angles C4 1.5248 (0.0040) C6 1.5316 (0.0044) 109.00 (0.24) H5A 0.9900 109.88 109.88 H5B 0.9900 109.88 109.88 108.30 C5 - C4 C6 H5A C6 - Distance Angles C7 1.5198 (0.0043) C5 1.5316 (0.0044) 111.38 (0.25) H6A 0.9900 109.35 109.35 H6B 0.9900 109.35 109.35 107.99 C6 - C7 C5 H6A C7 - Distance Angles C6 1.5198 (0.0043) C8 1.5309 (0.0039) 112.76 (0.26) H7A 0.9900 109.04 109.04 H7B 0.9900 109.04 109.04 107.81 C7 - C6 C8 H7A C8 - Distance Angles C7 1.5309 (0.0039) C3 1.5324 (0.0038) 112.87 (0.23) H8A 0.9900 109.01 109.01 H8B 0.9900 109.01 109.01 107.79 C8 - C7 C3 H8A C10 - Distance Angles C15 1.3950 (0.0040) N9 1.3970 (0.0034) 124.63 (0.25) C11 1.4008 (0.0038) 117.06 (0.25) 118.10 (0.25) C10 - C15 N9 C11 - Distance Angles C12 1.3825 (0.0039) C10 1.4008 (0.0038) 121.45 (0.27) H11 0.9500 119.28 119.28 C11 - C12 C10 C12 - Distance Angles C11 1.3825 (0.0039) C13 1.3900 (0.0044) 120.85 (0.27) H12 0.9500 119.58 119.58 C12 - C11 C13 C13 - Distance Angles C14 1.3758 (0.0043) C12 1.3900 (0.0044) 117.94 (0.27) H13 0.9500 121.03 121.03 C13 - C14 C12 C14 - Distance Angles C13 1.3758 (0.0043) C15 1.3846 (0.0040) 121.80 (0.29) H14 0.9500 119.10 119.10 C14 - C13 C15 C15 - Distance Angles C14 1.3846 (0.0040) C10 1.3950 (0.0040) 120.89 (0.27) H15 0.9500 119.55 119.55 C15 - C14 C10 N1 - Distance Angles C2 1.4886 (0.0034) H1A 0.9100 109.47 H1B 0.9100 109.47 109.47 H1C 0.9100 109.47 109.47 109.47 N1 - C2 H1A H1B N9 - Distance Angles C10 1.3970 (0.0034) C3 1.4767 (0.0032) 127.94 (0.23) H9 0.8872 (0.0321) 112.20 (1.92) 111.16 (1.87) N9 - C10 C3 C21 - Distance Angles C22 1.5080 (0.0039) 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 O24 1.2597 (0.0034) O23 1.2670 (0.0034) 123.52 (0.26) C21 1.5080 (0.0039) 118.73 (0.25) 117.74 (0.26) C22 - O24 O23 O23 - Distance Angles C22 1.2670 (0.0034) O23 - O24 - Distance Angles C22 1.2597 (0.0034) O24 - Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.91 2.807(3) 169.9 N1-H1A...O24_$1 0.91 1.89 2.776(3) 165.4 N1-H1B...O23_$2 0.89(3) 2.20(3) 3.084(3) 175(3) N9-H9...O24_$3 0.91 1.90 2.751(3) 155.8 N1-H1C...O23_$3 FMAP and GRID set by program FMAP 2 3 14 GRID -2.273 -2 -2 2.273 2 2 R1 = 0.1549 for 3269 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.27 at 0.2960 0.1330 0.0710 [ 0.71 A from C8 ] Deepest hole -0.26 at 0.2818 0.7023 0.1272 [ 0.82 A from C13 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2907 / 20624 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.2960 -0.1330 0.9290 1.00000 0.05 0.27 0.71 C8 0.82 C3 1.40 H8B 1.42 H8A Q2 1 -0.2993 -0.1358 1.0518 1.00000 0.05 0.25 0.54 H8B 1.02 C8 1.66 C3 1.72 H8A Q3 1 0.0682 0.0560 0.2487 1.00000 0.05 0.25 1.33 O23 1.84 H11 2.01 C22 2.08 H21C Q4 1 -0.4611 -0.1400 0.8415 1.00000 0.05 0.25 0.78 C6 0.81 C5 1.36 H6A 1.51 H5B Q5 1 -0.5522 0.0273 0.8430 1.00000 0.05 0.24 1.08 H5B 1.83 H4A 1.89 C5 2.29 H4A Q6 1 -0.2407 0.2001 1.0241 1.00000 0.05 0.23 1.55 H2A 1.77 H14 1.82 C14 1.94 H2B Q7 1 -0.4436 -0.2157 0.6414 1.00000 0.05 0.23 1.47 H5A 1.71 H7A 1.93 H6A 1.96 H6B Q8 1 -0.3613 0.2305 0.6661 1.00000 0.05 0.22 1.36 H15 1.83 C15 1.86 H6B 1.96 H14 Q9 1 -0.3283 -0.2292 0.9031 1.00000 0.05 0.22 0.78 C8 0.80 C7 1.32 H7A 1.36 H8A Q10 1 -0.3762 0.0935 0.6056 1.00000 0.05 0.22 0.48 H15 0.87 C15 1.85 C14 2.00 C10 Shortest distances between peaks (including symmetry equivalents) 1 2 1.12 1 9 1.18 8 10 1.64 2 9 1.69 4 7 2.06 4 9 2.13 4 5 2.30 1 4 2.35 6 8 2.50 7 9 2.59 2 4 2.68 2 5 2.81 5 7 2.90 2 7 2.92 4 8 2.95 5 5 2.98 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 0.75: 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 0.03: Generate idealized H-atoms 0.75: Structure factors and derivatives 0.69: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src1307p21c finished at 08:45:19 Total CPU time: 2.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++