+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008lsh009 started at 14:56:21 on 23-Jun-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh009 in P-1 CELL 0.71073 5.0214 6.8411 12.2219 89.465 80.477 79.234 ZERR 2.00 0.0003 0.0005 0.0010 0.004 0.004 0.004 LATT 1 SFAC C H N O UNIT 18 18 2 6 V = 406.67 F(000) = 188.0 Mu = 0.11 mm-1 Cell Wt = 358.34 Rho = 1.463 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 5 ACTA DFIX 0.84 0.02 O3 H3O BOND $H L.S. 6 EQIV $1 x-1, y, z EQIV $2 -x+1, -y+1, -z+2 HTAB N1 O1_$1 HTAB O3 O2_$2 SIZE 0.12 0.08 0.02 TEMP -153.00 WGHT 0.0240 0.6324 FVAR 1.09304 C1 1 0.652989 -0.284302 0.732010 11.00000 0.02299 0.01943 = 0.02458 -0.00318 -0.00096 -0.00684 C2 1 0.826703 -0.265751 0.806924 11.00000 0.02507 0.02125 = 0.02818 -0.00056 -0.00581 -0.00301 AFIX 43 H2 2 0.967559 -0.374219 0.817927 11.00000 -1.20000 AFIX 0 C3 1 0.793853 -0.088675 0.865483 11.00000 0.02748 0.02412 = 0.02632 -0.00111 -0.00854 -0.00525 AFIX 43 H3 2 0.915163 -0.075272 0.915741 11.00000 -1.20000 AFIX 0 C4 1 0.584661 0.070750 0.851714 11.00000 0.02321 0.02029 = 0.02175 -0.00099 -0.00214 -0.00537 C5 1 0.407299 0.049904 0.777912 11.00000 0.02516 0.02225 = 0.03001 0.00076 -0.00642 -0.00279 AFIX 43 H5 2 0.262339 0.156675 0.768789 11.00000 -1.20000 AFIX 0 C6 1 0.442250 -0.126368 0.717867 11.00000 0.02556 0.02487 = 0.03012 -0.00261 -0.00907 -0.00457 AFIX 43 H6 2 0.322515 -0.139769 0.666956 11.00000 -1.20000 AFIX 0 C7 1 0.914155 -0.583342 0.626462 11.00000 0.02797 0.02009 = 0.02361 0.00090 -0.00429 -0.00385 C8 1 0.884001 -0.770111 0.568876 11.00000 0.03404 0.02196 = 0.03141 -0.00402 -0.00429 -0.00450 AFIX 137 H8A 2 1.022216 -0.796115 0.501416 11.00000 -1.50000 H8B 2 0.699774 -0.752904 0.549143 11.00000 -1.50000 H8C 2 0.910422 -0.882661 0.618656 11.00000 -1.50000 AFIX 0 C9 1 0.548402 0.260430 0.914109 11.00000 0.02561 0.01939 = 0.02422 -0.00058 -0.00433 -0.00413 N1 3 0.675349 -0.463958 0.671282 11.00000 0.02247 0.02123 = 0.03015 -0.00387 -0.00686 -0.00465 H1N 2 0.524014 -0.488750 0.657399 11.00000 -1.20000 O1 4 1.142287 -0.545729 0.631636 11.00000 0.02475 0.02812 = 0.03502 -0.00353 -0.00647 -0.00613 O2 4 0.350770 0.396813 0.908001 11.00000 0.03350 0.02058 = 0.03304 -0.00368 -0.00843 -0.00091 O3 4 0.736508 0.271887 0.974059 11.00000 0.03187 0.02418 = 0.03755 -0.00800 -0.01234 -0.00340 H3O 2 0.699362 0.384421 1.010080 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for 2008lsh009 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C6 N1 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C9 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - O2 O3 C4 N1 - C7 C1 O1 - C7 O2 - C9 O3 - C9 Operators for generating equivalent atoms: $1 x-1, y, z $2 -x+1, -y+1, -z+2 6987 Reflections read, of which 19 rejected -6 =< h =< 6, -8 =< k =< 8, -15 =< l =< 15, Max. 2-theta = 54.98 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -4 -5 1 0.46 0.39 3 2.95 1 Inconsistent equivalents 1841 Unique reflections, of which 0 suppressed R(int) = 0.0578 R(sigma) = 0.0572 Friedel opposites merged Maximum memory for data reduction = 1353 / 18182 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 = 1688 / 158870 wR2 = 0.1455 before cycle 1 for 1841 data and 125 / 125 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 0.024 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.093; Restrained GooF = 1.093 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09403 0.00360 0.274 OSF Mean shift/esd = 0.060 Maximum = 0.274 for OSF Max. shift = 0.006 A for H1N Max. dU = 0.000 for C4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1688 / 158870 wR2 = 0.1454 before cycle 2 for 1841 data and 125 / 125 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 0.026 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.094; Restrained GooF = 1.094 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09398 0.00360 -0.013 OSF Mean shift/esd = 0.021 Maximum = -0.103 for z H1N Max. shift = 0.003 A for H1N Max. dU = 0.000 for C8 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1688 / 158870 wR2 = 0.1454 before cycle 3 for 1841 data and 125 / 125 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 0.027 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.094; Restrained GooF = 1.094 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09399 0.00360 0.003 OSF Mean shift/esd = 0.002 Maximum = -0.026 for z H1N Max. shift = 0.001 A for H1N Max. dU = 0.000 for C8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1688 / 158870 wR2 = 0.1454 before cycle 4 for 1841 data and 125 / 125 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 0.027 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.093; Restrained GooF = 1.094 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09401 0.00360 0.004 OSF Mean shift/esd = 0.001 Maximum = -0.009 for z H1N Max. shift = 0.000 A for H1N Max. dU = 0.000 for C7 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1688 / 158870 wR2 = 0.1454 before cycle 5 for 1841 data and 125 / 125 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 0.027 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.094; Restrained GooF = 1.094 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09401 0.00360 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.003 for z H1N Max. shift = 0.000 A for H1N Max. dU = 0.000 for C8 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1688 / 158870 wR2 = 0.1454 before cycle 6 for 1841 data and 125 / 125 parameters Summary of restraints applied in cycle 6 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 = 1.094; Restrained GooF = 1.094 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09401 0.00360 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z H1N Max. shift = 0.000 A for H1N Max. dU = 0.000 for C5 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.9676 -0.3742 0.8178 43 0.950 0.000 C2 C3 C1 H3 0.9151 -0.0753 0.9157 43 0.950 0.000 C3 C2 C4 H5 0.2623 0.1566 0.7688 43 0.950 0.000 C5 C6 C4 H6 0.3226 -0.1398 0.6669 43 0.950 0.000 C6 C5 C1 H8A 1.0218 -0.7959 0.5013 137 0.980 0.000 C8 C7 H8A H8B 0.6996 -0.7530 0.5494 137 0.980 0.000 C8 C7 H8A H8C 0.9110 -0.8827 0.6186 137 0.980 0.000 C8 C7 H8A 2008lsh009 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.65298 -0.28425 0.73202 1.00000 0.02292 0.01936 0.02455 -0.00311 -0.00108 -0.00694 0.02220 0.00381 0.00051 0.00035 0.00021 0.00000 0.00128 0.00115 0.00138 0.00102 0.00105 0.00100 0.00055 C2 0.82670 -0.26571 0.80687 1.00000 0.02496 0.02122 0.02822 -0.00047 -0.00587 -0.00296 0.02481 0.00396 0.00053 0.00037 0.00022 0.00000 0.00133 0.00121 0.00147 0.00106 0.00112 0.00104 0.00058 H2 0.96763 -0.37416 0.81783 1.00000 0.02977 0.00000 0.00000 C3 0.79385 -0.08869 0.86547 1.00000 0.02729 0.02410 0.02626 -0.00106 -0.00861 -0.00526 0.02534 0.00410 0.00055 0.00037 0.00023 0.00000 0.00135 0.00127 0.00141 0.00107 0.00111 0.00107 0.00058 H3 0.91512 -0.07532 0.91575 1.00000 0.03040 0.00000 0.00000 C4 0.58468 0.07072 0.85170 1.00000 0.02305 0.02013 0.02174 -0.00091 -0.00212 -0.00531 0.02165 0.00388 0.00051 0.00035 0.00021 0.00000 0.00125 0.00116 0.00135 0.00101 0.00105 0.00100 0.00055 C5 0.40735 0.04985 0.77792 1.00000 0.02505 0.02223 0.02999 0.00084 -0.00652 -0.00282 0.02575 0.00409 0.00054 0.00038 0.00023 0.00000 0.00133 0.00121 0.00149 0.00108 0.00113 0.00104 0.00059 H5 0.26235 0.15661 0.76882 1.00000 0.03090 0.00000 0.00000 C6 0.44229 -0.12637 0.71786 1.00000 0.02537 0.02481 0.03008 -0.00246 -0.00908 -0.00454 0.02624 0.00408 0.00054 0.00038 0.00023 0.00000 0.00134 0.00127 0.00150 0.00109 0.00115 0.00107 0.00060 H6 0.32259 -0.13976 0.66693 1.00000 0.03149 0.00000 0.00000 C7 0.91419 -0.58339 0.62645 1.00000 0.02786 0.02001 0.02381 0.00104 -0.00430 -0.00379 0.02399 0.00406 0.00054 0.00036 0.00022 0.00000 0.00139 0.00118 0.00139 0.00102 0.00109 0.00105 0.00057 C8 0.88402 -0.77009 0.56888 1.00000 0.03430 0.02193 0.03137 -0.00396 -0.00414 -0.00446 0.02943 0.00424 0.00060 0.00038 0.00024 0.00000 0.00149 0.00125 0.00155 0.00110 0.00121 0.00112 0.00063 H8A 1.02185 -0.79587 0.50130 1.00000 0.04415 0.00000 0.00000 H8B 0.69959 -0.75303 0.54937 1.00000 0.04415 0.00000 0.00000 H8C 0.91102 -0.88273 0.61857 1.00000 0.04415 0.00000 0.00000 C9 0.54839 0.26038 0.91409 1.00000 0.02562 0.01953 0.02415 -0.00047 -0.00434 -0.00432 0.02306 0.00391 0.00052 0.00036 0.00021 0.00000 0.00133 0.00117 0.00139 0.00102 0.00108 0.00104 0.00056 N1 0.67534 -0.46392 0.67123 1.00000 0.02225 0.02125 0.03024 -0.00387 -0.00692 -0.00455 0.02420 0.00350 0.00046 0.00031 0.00019 0.00000 0.00115 0.00104 0.00128 0.00090 0.00097 0.00089 0.00051 H1N 0.52416 -0.48852 0.65658 1.00000 0.02904 0.04833 0.00630 0.00428 0.00247 0.00000 0.00000 O1 1.14227 -0.54573 0.63167 1.00000 0.02480 0.02804 0.03514 -0.00339 -0.00647 -0.00608 0.02898 0.00285 0.00037 0.00027 0.00016 0.00000 0.00099 0.00097 0.00114 0.00083 0.00084 0.00080 0.00047 O2 0.35073 0.39685 0.90799 1.00000 0.03323 0.02051 0.03316 -0.00359 -0.00845 -0.00081 0.02916 0.00288 0.00039 0.00026 0.00016 0.00000 0.00107 0.00090 0.00113 0.00078 0.00086 0.00080 0.00047 O3 0.73655 0.27182 0.97405 1.00000 0.03199 0.02407 0.03762 -0.00809 -0.01246 -0.00338 0.03065 0.00287 0.00040 0.00027 0.00017 0.00000 0.00105 0.00095 0.00120 0.00084 0.00090 0.00083 0.00048 H3O 0.70005 0.38421 1.01067 1.00000 0.04597 0.04035 0.00686 0.00342 0.00254 0.00000 0.00000 Final Structure Factor Calculation for 2008lsh009 in P-1 Total number of l.s. parameters = 125 Maximum vector length = 511 Memory required = 1563 / 22995 wR2 = 0.1454 before cycle 7 for 1841 data and 0 / 125 parameters Summary of restraints applied in cycle 7 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 = 1.094; Restrained GooF = 1.094 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.63 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0644 for 1328 Fo > 4sig(Fo) and 0.0999 for all 1841 data wR2 = 0.1454, GooF = S = 1.094, Restrained GooF = 1.094 for all data Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 9.00 for hydrogen atoms Principal mean square atomic displacements U 0.0291 0.0212 0.0163 C1 0.0290 0.0245 0.0210 C2 0.0307 0.0250 0.0204 C3 0.0249 0.0210 0.0191 C4 0.0304 0.0253 0.0215 C5 0.0335 0.0249 0.0204 C6 0.0282 0.0239 0.0199 C7 0.0351 0.0331 0.0201 C8 0.0257 0.0243 0.0192 C9 0.0326 0.0223 0.0178 N1 0.0371 0.0273 0.0225 O1 0.0385 0.0297 0.0192 O2 0.0455 0.0280 0.0184 O3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.014 0.021 0.029 0.038 0.048 0.063 0.086 0.124 1.000 Number in group 184. 203. 182. 180. 175. 183. 201. 167. 182. 184. GooF 1.195 1.181 1.167 1.217 1.013 1.065 1.024 0.913 1.076 1.025 K 8.233 1.534 1.107 1.134 1.028 0.971 0.977 0.996 1.004 0.999 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.32 1.66 inf Number in group 184. 190. 184. 181. 182. 187. 183. 182. 185. 183. GooF 1.198 1.189 1.210 1.186 1.056 1.103 1.080 0.839 0.914 1.092 K 1.056 1.103 1.083 1.036 1.000 1.018 0.991 1.000 1.016 0.987 R1 0.239 0.207 0.210 0.178 0.133 0.103 0.058 0.054 0.044 0.034 Recommended weighting scheme: WGHT 0.0212 0.6178 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) 3 -4 4 51.49 111.89 6.46 0.110 1.05 4 -4 2 51.24 80.88 3.63 0.093 0.92 -4 5 4 13.97 0.27 3.46 0.005 0.77 -4 -5 8 14.48 0.25 3.33 0.005 0.79 5 1 9 14.26 1.31 3.23 0.012 0.87 5 -2 7 -1.67 6.53 3.22 0.027 0.85 4 1 11 11.42 2.76 3.15 0.017 0.90 3 4 13 15.68 0.22 3.08 0.005 0.80 2 -5 10 -2.64 5.91 3.00 0.025 0.85 0 0 9 -1.45 3.39 2.98 0.019 1.34 -1 3 13 11.74 1.45 2.97 0.012 0.81 2 7 3 9.30 20.92 2.96 0.048 0.94 3 0 11 11.13 26.72 2.93 0.054 0.99 5 1 5 8.46 2.05 2.89 0.015 0.97 2 1 5 198.69 161.86 2.85 0.132 1.87 -3 -6 6 4.30 14.17 2.77 0.039 0.88 2 -5 12 -3.70 6.94 2.77 0.027 0.78 2 -4 7 7.93 1.47 2.73 0.013 1.08 -2 7 0 14.08 4.45 2.71 0.022 0.84 -2 -3 13 14.45 28.67 2.70 0.056 0.79 -1 -1 2 8078.35 9267.64 2.69 1.000 3.32 3 0 13 8.14 0.00 2.66 0.000 0.87 -3 -3 7 265.92 213.33 2.63 0.152 1.04 0 3 3 411.45 355.58 2.60 0.196 1.94 1 0 1 2766.03 3046.53 2.58 0.573 4.80 0 -5 10 6.24 16.52 2.55 0.042 0.91 -5 -1 5 22.02 4.36 2.54 0.022 0.87 -2 2 0 403.68 351.95 2.51 0.195 1.81 3 7 6 15.45 3.09 2.50 0.018 0.85 2 0 11 -0.92 4.12 2.47 0.021 1.07 -1 4 2 4.97 0.53 2.46 0.008 1.43 -3 -1 12 8.72 1.73 2.46 0.014 0.80 6 0 6 -3.35 3.77 2.45 0.020 0.80 4 2 8 7.92 1.95 2.45 0.015 1.03 1 -4 12 193.00 134.79 2.43 0.121 0.86 3 2 12 14.73 6.23 2.43 0.026 0.91 1 -3 2 739.86 660.85 2.43 0.267 1.86 -3 -4 8 8.71 19.53 2.41 0.046 0.93 2 3 6 20.83 32.35 2.38 0.059 1.43 6 0 0 5.21 0.09 2.36 0.003 0.81 5 0 10 -1.63 1.81 2.34 0.014 0.83 3 -4 8 28.18 15.10 2.33 0.040 0.93 1 5 13 25.07 13.03 2.30 0.037 0.78 4 0 1 18.69 10.87 2.29 0.034 1.23 2 -6 3 8.01 16.07 2.28 0.042 0.94 1 6 5 11.78 20.33 2.26 0.047 1.04 0 7 6 7.81 0.10 2.26 0.003 0.86 -1 0 10 12.89 22.32 2.26 0.049 1.13 -1 7 6 131.72 102.17 2.26 0.105 0.81 -1 7 7 18.41 6.97 2.26 0.027 0.79 Bond lengths and angles C1 - Distance Angles C2 1.3862 (0.0036) C6 1.3950 (0.0035) 120.09 (0.23) N1 1.4189 (0.0031) 121.82 (0.22) 118.05 (0.23) C1 - C2 C6 C2 - Distance Angles C3 1.3817 (0.0035) C1 1.3862 (0.0036) 119.66 (0.24) H2 0.9500 120.17 120.17 C2 - C3 C1 C3 - Distance Angles C2 1.3817 (0.0035) C4 1.3957 (0.0034) 120.81 (0.25) H3 0.9500 119.59 119.59 C3 - C2 C4 C4 - Distance Angles C5 1.3936 (0.0036) C3 1.3957 (0.0034) 119.25 (0.23) C9 1.4773 (0.0034) 119.66 (0.22) 121.09 (0.23) C4 - C5 C3 C5 - Distance Angles C6 1.3849 (0.0036) C4 1.3936 (0.0036) 120.06 (0.24) H5 0.9500 119.97 119.97 C5 - C6 C4 C6 - Distance Angles C5 1.3849 (0.0036) C1 1.3950 (0.0035) 120.10 (0.24) H6 0.9500 119.95 119.95 C6 - C5 C1 C7 - Distance Angles O1 1.2316 (0.0032) N1 1.3531 (0.0033) 123.43 (0.24) C8 1.5079 (0.0035) 121.32 (0.24) 115.25 (0.23) C7 - O1 N1 C8 - Distance Angles C7 1.5079 (0.0035) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C7 H8A H8B C9 - Distance Angles O2 1.2407 (0.0030) O3 1.3014 (0.0031) 123.65 (0.23) C4 1.4773 (0.0034) 121.06 (0.23) 115.28 (0.21) C9 - O2 O3 N1 - Distance Angles C7 1.3531 (0.0033) C1 1.4189 (0.0031) 125.24 (0.23) H1N 0.8544 (0.0306) 119.05 (2.00) 115.33 (1.99) N1 - C7 C1 O1 - Distance Angles C7 1.2316 (0.0032) O1 - O2 - Distance Angles C9 1.2407 (0.0030) O2 - O3 - Distance Angles C9 1.3014 (0.0031) H3O 0.8670 (0.0181) 110.84 (2.25) O3 - C9 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.85(3) 2.10(3) 2.950(3) 176(3) N1-H1N...O1_$1 0.867(18) 1.760(19) 2.625(3) 175(3) O3-H3O...O2_$2 FMAP and GRID set by program FMAP 2 1 15 GRID -4.167 -2 -2 4.167 2 2 R1 = 0.0998 for 1841 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.31 at 0.2003 0.2585 0.2582 [ 0.82 A from C1 ] Deepest hole -0.27 at 0.3026 0.9335 0.7151 [ 0.75 A from C6 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 1651 / 15003 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7997 -0.2585 0.7418 1.00000 0.05 0.31 0.82 C1 0.83 C2 1.48 H2 1.91 N1 Q2 1 0.8290 -0.2385 0.9855 1.00000 0.05 0.23 1.48 H3 1.80 C3 1.91 O2 2.11 C9 Q3 1 0.2194 0.1480 0.8615 1.00000 0.05 0.22 1.12 H5 1.36 C5 1.80 C4 2.05 O2 Q4 1 0.8379 0.4802 0.9589 1.00000 0.05 0.22 1.15 H3O 1.60 O3 1.86 O2 2.06 H2 Q5 1 0.5085 -0.2235 0.7454 1.00000 0.05 0.21 0.76 C1 0.78 C6 1.48 H6 1.85 C2 Shortest distances between peaks (including symmetry equivalents) 1 5 1.43 2 3 1.94 2 4 1.95 4 4 2.11 2 4 2.30 3 4 2.81 3 5 2.93 Time profile in seconds ----------------------- 0.12: 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 0.01: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.48: 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 0.46: Structure factors and derivatives 0.45: 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 0.06: Analysis of variance 0.04: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008lsh009 finished at 14:56:23 Total CPU time: 1.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++