+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 05skc0002p1 started at 12:37:04 on 14-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 05skc0002p1 in P1 CELL 0.71073 5.1580 5.3261 7.5218 78.735 83.330 79.077 ZERR 1.00 0.0005 0.0007 0.0006 0.008 0.010 0.011 LATT -1 SFAC C H N O UNIT 5 11 1 6 V = 198.31 F(000) = 96.0 Mu = 0.14 mm-1 Cell Wt = 181.15 Rho = 1.517 MERG 4 OMIT -3.00 55.00 EXTI 0.19495 SHEL 7 0.77 HTAB O2 O1A HTAB N22 O1A EQIV_$1 x, y, z-1 HTAB O1B O4A_$1 HTAB N22 O2_$1 EQIV_$2 x, y-1, z HTAB O2 O3_$2 EQIV_$3 x-1, y, z HTAB O3 O4B_$3 EQIV_$4 x-1, y, z-1 HTAB N22 O4B_$4 EQIV_$5 x, y-1, z-1 HTAB N22 O4A_$5 FMAP 2 PLAN 10 SIZE 0.02 0.12 0.20 ACTA BOND $H WGHT 0.04100 0.04220 L.S. 8 TEMP -153.00 FVAR 2.91796 0.01000 MOLE 1 C1 1 0.445164 -0.076192 0.140261 11.00000 0.01830 0.01494 = 0.01313 -0.00389 -0.00002 -0.00181 C2 1 0.535268 -0.105024 0.329867 11.00000 0.02009 0.01214 = 0.01224 -0.00217 -0.00173 -0.00333 AFIX 13 H2 2 0.729524 -0.174994 0.327293 11.00000 -1.20000 AFIX 0 C3 1 0.483991 0.160812 0.389383 11.00000 0.01553 0.01627 = 0.01014 -0.00267 -0.00098 -0.00387 AFIX 13 H3 2 0.598100 0.272860 0.305559 11.00000 -1.20000 AFIX 0 C4 1 0.576576 0.121796 0.580328 11.00000 0.01739 0.01124 = 0.01277 -0.00138 -0.00135 -0.00458 O1A 4 0.276088 -0.195604 0.115660 11.00000 0.03402 0.02562 = 0.01578 -0.00289 -0.00376 -0.01572 O1B 4 0.564534 0.077374 0.016488 11.00000 0.02655 0.02602 = 0.01019 -0.00260 -0.00100 -0.01229 AFIX 147 H1 2 0.515390 0.075398 -0.085783 11.00000 -1.50000 AFIX 0 O2 4 0.398395 -0.278958 0.455537 11.00000 0.02923 0.01469 = 0.01296 -0.00196 0.00001 -0.00935 AFIX 147 H2O 2 0.312086 -0.352320 0.399111 11.00000 -1.50000 AFIX 0 O3 4 0.218033 0.284140 0.373909 11.00000 0.01533 0.01663 = 0.01499 -0.00112 -0.00233 -0.00244 AFIX 147 H3O 2 0.120436 0.210271 0.457118 11.00000 -1.50000 AFIX 0 O4A 4 0.399766 0.144993 0.710862 11.00000 0.01856 0.02348 = 0.01061 -0.00403 -0.00052 -0.00369 O4B 4 0.819431 0.064518 0.595510 11.00000 0.01511 0.02648 = 0.01705 -0.00288 -0.00218 -0.00527 MOLE 2 C21 1 -0.076430 -0.525100 -0.104180 11.00000 0.02177 0.02129 = 0.03300 -0.00645 0.00366 -0.00750 AFIX 137 H21B 2 -0.124818 -0.601387 -0.201506 11.00000 -1.50000 H21C 2 -0.236606 -0.433301 -0.045888 11.00000 -1.50000 H21A 2 0.011785 -0.663206 -0.013744 11.00000 -1.50000 AFIX 0 N22 3 0.105452 -0.339821 -0.181863 11.00000 0.01683 0.02480 = 0.01752 -0.00341 -0.00177 -0.00708 AFIX 137 H22B 2 0.171811 -0.289341 -0.090101 11.00000 -1.50000 H22C 2 0.015416 -0.198199 -0.251456 11.00000 -1.50000 H22A 2 0.240880 -0.418084 -0.251763 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 05skc0002p1 in P1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - O2 C1 C3 C3 - O3 C4 C2 C4 - O4B O4A C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C21 - N22 N22 - C21 Operators for generating equivalent atoms: $1 x, y, z-1 $2 x, y-1, z $3 x-1, y, z $4 x-1, y, z-1 $5 x, y-1, z-1 Floating origin restraints generated 4317 Reflections read, of which 6 rejected -6 =< h =< 6, -6 =< k =< 6, -9 =< l =< 9, Max. 2-theta = 54.91 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 -4 1 22.97 1.52 9 13.64 1 Inconsistent equivalents 905 Unique reflections, of which 0 suppressed R(int) = 0.0369 R(sigma) = 0.0319 Friedel opposites merged Maximum memory for data reduction = 1586 / 8887 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 = 1912 / 148565 wR2 = 0.0779 before cycle 1 for 905 data and 116 / 116 parameters GooF = S = 1.078; Restrained GooF = 1.076 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0410 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.91779 0.01091 -0.016 OSF 2 0.01000 9.99999 0.000 FVAR 2 3 0.19506 0.03456 0.003 EXTI Mean shift/esd = 0.023 Maximum = -0.085 for y C3 Max. shift = 0.001 A for H22A Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1912 / 148565 wR2 = 0.0779 before cycle 2 for 905 data and 116 / 116 parameters GooF = S = 1.079; Restrained GooF = 1.077 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0410 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.91738 0.01091 -0.038 OSF 2 0.01000 9.99999 0.000 FVAR 2 3 0.19502 0.03458 -0.001 EXTI Mean shift/esd = 0.008 Maximum = -0.038 for OSF Max. shift = 0.000 A for H1 Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1912 / 148565 wR2 = 0.0779 before cycle 3 for 905 data and 116 / 116 parameters GooF = S = 1.079; Restrained GooF = 1.077 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0410 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.91737 0.01091 -0.001 OSF 2 0.01000 9.99999 0.000 FVAR 2 3 0.19496 0.03458 -0.002 EXTI Mean shift/esd = 0.000 Maximum = -0.004 for tors H1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for N22 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1912 / 148565 wR2 = 0.0779 before cycle 4 for 905 data and 116 / 116 parameters GooF = S = 1.079; Restrained GooF = 1.077 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0410 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.91737 0.01091 0.000 OSF 2 0.01000 9.99999 0.000 FVAR 2 3 0.19496 0.03457 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for tors H1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for O1B Least-squares cycle 5 Maximum vector length = 511 Memory required = 1912 / 148565 wR2 = 0.0779 before cycle 5 for 905 data and 116 / 116 parameters GooF = S = 1.079; Restrained GooF = 1.077 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0410 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.91738 0.01091 0.000 OSF 2 0.01000 9.99999 0.000 FVAR 2 3 0.19497 0.03458 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1 Max. dU = 0.000 for O4A Least-squares cycle 6 Maximum vector length = 511 Memory required = 1912 / 148565 wR2 = 0.0779 before cycle 6 for 905 data and 116 / 116 parameters GooF = S = 1.079; Restrained GooF = 1.077 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0410 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.91738 0.01091 0.000 OSF 2 0.01000 9.99999 0.000 FVAR 2 3 0.19497 0.03458 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O4B Max. shift = 0.000 A for H1 Max. dU = 0.000 for O4A Least-squares cycle 7 Maximum vector length = 511 Memory required = 1912 / 148565 wR2 = 0.0779 before cycle 7 for 905 data and 116 / 116 parameters GooF = S = 1.079; Restrained GooF = 1.077 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0410 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.91738 0.01091 0.000 OSF 2 0.01000 9.99999 0.000 FVAR 2 3 0.19497 0.03458 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O4B Max. shift = 0.000 A for H1 Max. dU = 0.000 for O1A Least-squares cycle 8 Maximum vector length = 511 Memory required = 1912 / 148565 wR2 = 0.0779 before cycle 8 for 905 data and 116 / 116 parameters GooF = S = 1.079; Restrained GooF = 1.077 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0410 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.91737 0.01091 0.000 OSF 2 0.01000 9.99999 0.000 FVAR 2 3 0.19496 0.03458 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H21C Max. dU = 0.000 for O4B Largest correlation matrix elements 0.653 EXTI / OSF Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.7295 -0.1750 0.3273 13 1.000 0.000 C2 O2 C1 C3 H3 0.5981 0.2728 0.3056 13 1.000 0.000 C3 O3 C4 C2 H1 0.5156 0.0752 -0.0858 147 0.840 0.000 O1B C1 H1 H2O 0.3120 -0.3523 0.3991 147 0.840 0.000 O2 C2 H2O H3O 0.1204 0.2101 0.4570 147 0.840 0.000 O3 C3 H3O H21B -0.1246 -0.6015 -0.2015 137 0.980 0.000 C21 N22 H21B H21C -0.2367 -0.4332 -0.0460 137 0.980 0.000 C21 N22 H21B H21A 0.0117 -0.6631 -0.0136 137 0.980 0.000 C21 N22 H21B H22B 0.1716 -0.2892 -0.0901 137 0.910 0.000 N22 C21 H22B H22C 0.0155 -0.1983 -0.2516 137 0.910 0.000 N22 C21 H22B H22A 0.2410 -0.4182 -0.2516 137 0.910 0.000 N22 C21 H22B 05skc0002p1 in P1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.44515 -0.07617 0.14027 1.00000 0.01829 0.01489 0.01308 -0.00386 -0.00001 -0.00181 0.01547 0.00351 0.00046 0.00043 0.00031 0.00000 0.00114 0.00114 0.00110 0.00091 0.00090 0.00090 0.00049 C2 0.53529 -0.10500 0.32986 1.00000 0.02001 0.01212 0.01215 -0.00215 -0.00172 -0.00333 0.01465 0.00357 0.00047 0.00044 0.00031 0.00000 0.00119 0.00112 0.00110 0.00087 0.00091 0.00087 0.00050 H2 0.72955 -0.17498 0.32728 1.00000 0.01758 0.00000 0.00000 C3 0.48402 0.16076 0.38939 1.00000 0.01543 0.01626 0.01012 -0.00268 -0.00098 -0.00386 0.01374 0.00339 0.00045 0.00044 0.00031 0.00000 0.00109 0.00114 0.00109 0.00087 0.00088 0.00087 0.00049 H3 0.59814 0.27281 0.30558 1.00000 0.01649 0.00000 0.00000 C4 0.57656 0.12181 0.58031 1.00000 0.01735 0.01122 0.01271 -0.00139 -0.00135 -0.00457 0.01357 0.00350 0.00047 0.00044 0.00032 0.00000 0.00114 0.00103 0.00107 0.00083 0.00086 0.00084 0.00047 O1A 0.27607 -0.19560 0.11566 1.00000 0.03397 0.02561 0.01577 -0.00289 -0.00378 -0.01574 0.02366 0.00267 0.00037 0.00036 0.00024 0.00000 0.00112 0.00097 0.00091 0.00072 0.00075 0.00082 0.00045 O1B 0.56454 0.07737 0.01649 1.00000 0.02652 0.02595 0.01015 -0.00258 -0.00101 -0.01226 0.01996 0.00260 0.00034 0.00033 0.00022 0.00000 0.00098 0.00096 0.00081 0.00070 0.00072 0.00074 0.00041 H1 0.51559 0.07520 -0.08580 1.00000 0.02994 0.00000 0.00000 O2 0.39839 -0.27896 0.45555 1.00000 0.02921 0.01465 0.01294 -0.00195 0.00000 -0.00939 0.01839 0.00250 0.00034 0.00031 0.00021 0.00000 0.00097 0.00082 0.00090 0.00069 0.00074 0.00070 0.00041 H2O 0.31203 -0.35228 0.39912 1.00000 0.02758 0.00000 0.00000 O3 0.21803 0.28415 0.37390 1.00000 0.01527 0.01657 0.01501 -0.00109 -0.00234 -0.00242 0.01580 0.00246 0.00031 0.00030 0.00023 0.00000 0.00081 0.00087 0.00084 0.00066 0.00064 0.00064 0.00038 H3O 0.12038 0.21014 0.45700 1.00000 0.02370 0.00000 0.00000 O4A 0.39975 0.14501 0.71086 1.00000 0.01851 0.02349 0.01057 -0.00402 -0.00051 -0.00371 0.01742 0.00259 0.00033 0.00032 0.00023 0.00000 0.00085 0.00097 0.00081 0.00069 0.00064 0.00069 0.00040 O4B 0.81945 0.06449 0.59551 1.00000 0.01506 0.02647 0.01702 -0.00287 -0.00216 -0.00524 0.01936 0.00270 0.00034 0.00035 0.00024 0.00000 0.00080 0.00093 0.00087 0.00072 0.00065 0.00070 0.00041 C21 -0.07645 -0.52509 -0.10419 1.00000 0.02174 0.02124 0.03293 -0.00647 0.00371 -0.00747 0.02505 0.00442 0.00056 0.00052 0.00041 0.00000 0.00125 0.00135 0.00157 0.00115 0.00114 0.00104 0.00060 H21B -0.12465 -0.60154 -0.20149 1.00000 0.03758 0.00000 0.00000 H21C -0.23672 -0.43323 -0.04604 1.00000 0.03758 0.00000 0.00000 H21A 0.01167 -0.66308 -0.01363 1.00000 0.03758 0.00000 0.00000 N22 0.10547 -0.33982 -0.18187 1.00000 0.01679 0.02475 0.01743 -0.00339 -0.00176 -0.00704 0.01921 0.00327 0.00041 0.00042 0.00029 0.00000 0.00100 0.00116 0.00103 0.00088 0.00080 0.00083 0.00047 H22B 0.17165 -0.28917 -0.09010 1.00000 0.02882 0.00000 0.00000 H22C 0.01550 -0.19830 -0.25159 1.00000 0.02882 0.00000 0.00000 H22A 0.24102 -0.41817 -0.25163 1.00000 0.02882 0.00000 0.00000 Final Structure Factor Calculation for 05skc0002p1 in P1 Total number of l.s. parameters = 116 Maximum vector length = 511 Memory required = 1798 / 25046 wR2 = 0.0779 before cycle 9 for 905 data and 2 / 116 parameters GooF = S = 1.079; Restrained GooF = 1.077 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0410 * P )^2 + 0.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0330 for 840 Fo > 4sig(Fo) and 0.0381 for all 905 data wR2 = 0.0779, GooF = S = 1.079, Restrained GooF = 1.077 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 12.00 for non-hydrogen and 11.00 for hydrogen atoms Principal mean square atomic displacements U 0.0191 0.0154 0.0119 C1 0.0200 0.0121 0.0118 C2 0.0169 0.0144 0.0099 C3 0.0177 0.0129 0.0101 C4 0.0399 0.0173 0.0138 O1A 0.0329 0.0169 0.0101 O1B 0.0305 0.0133 0.0114 O2 0.0180 0.0158 0.0136 O3 0.0235 0.0186 0.0102 O4A 0.0269 0.0172 0.0140 O4B 0.0361 0.0223 0.0168 C21 0.0257 0.0175 0.0145 N22 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.045 0.063 0.081 0.101 0.118 0.138 0.173 0.218 0.294 1.000 Number in group 94. 88. 94. 89. 93. 89. 89. 88. 90. 91. GooF 1.097 1.230 1.064 1.000 1.077 1.154 0.895 1.037 1.093 1.110 K 1.023 0.922 0.950 0.964 0.979 0.996 1.018 1.026 1.027 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.04 1.16 1.31 1.64 inf Number in group 93. 90. 93. 87. 90. 90. 91. 90. 91. 90. GooF 1.205 1.059 1.169 1.107 0.915 1.031 1.061 0.924 1.025 1.239 K 1.021 1.035 1.006 1.027 1.009 1.017 1.013 1.022 1.015 1.000 R1 0.110 0.075 0.082 0.053 0.033 0.033 0.027 0.022 0.021 0.022 Recommended weighting scheme: WGHT 0.0402 0.0437 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) 0 0 2 61.12 74.13 3.77 0.248 3.68 1 1 7 2.18 3.71 3.20 0.055 1.07 1 5 1 2.13 0.43 3.05 0.019 1.06 -2 5 3 50.26 40.33 2.99 0.183 0.88 2 6 0 -0.20 1.16 2.64 0.031 0.86 -3 0 1 12.83 15.52 2.51 0.113 1.61 -1 -5 3 3.75 5.40 2.51 0.067 0.90 -2 1 8 8.05 12.01 2.44 0.100 0.84 -1 0 2 117.92 132.15 2.38 0.331 2.86 -1 3 1 15.71 13.24 2.38 0.105 1.56 1 0 1 219.37 244.93 2.38 0.451 4.33 3 6 0 1.06 3.18 2.36 0.051 0.82 2 1 9 13.74 17.89 2.35 0.122 0.82 2 0 8 12.24 15.79 2.31 0.114 0.89 4 -2 5 28.87 22.51 2.30 0.137 0.86 6 3 3 6.71 10.05 2.28 0.091 0.81 2 -4 4 116.26 100.98 2.27 0.289 0.88 1 4 6 2.35 3.63 2.27 0.055 1.00 -3 2 7 65.91 55.45 2.25 0.214 0.83 4 5 6 4.64 7.01 2.22 0.076 0.79 2 1 8 14.78 17.89 2.21 0.122 0.91 -4 -3 4 23.20 27.93 2.19 0.152 0.88 -1 4 8 6.36 10.19 2.16 0.092 0.79 3 6 1 9.07 11.96 2.15 0.100 0.84 -1 6 5 10.17 5.06 2.11 0.065 0.77 1 6 1 41.59 35.14 2.11 0.171 0.88 -4 0 5 67.21 58.74 2.09 0.221 0.92 0 3 8 -0.26 0.58 2.08 0.022 0.88 -5 -4 1 19.26 22.93 2.07 0.138 0.85 -1 6 4 11.62 7.66 2.07 0.080 0.80 0 5 2 9.51 12.04 2.07 0.100 1.04 1 0 5 12.35 14.48 2.05 0.110 1.44 -5 -2 5 1.91 4.51 2.05 0.061 0.77 -6 -3 1 1.12 2.73 2.04 0.048 0.79 5 1 7 56.67 48.37 2.04 0.200 0.78 0 5 1 17.56 20.61 2.02 0.131 1.05 4 0 8 43.46 32.72 2.02 0.165 0.77 5 0 2 4.75 6.19 2.01 0.072 0.99 -5 -4 3 7.79 3.08 2.00 0.050 0.77 -1 -6 1 1.76 3.36 1.99 0.053 0.85 4 1 8 0.13 1.71 1.97 0.038 0.80 2 -4 1 4.00 5.48 1.95 0.067 1.05 -4 4 1 9.82 12.53 1.93 0.102 0.83 -1 -5 1 16.25 18.78 1.93 0.125 1.01 5 5 0 3.88 5.56 1.92 0.068 0.79 -4 3 0 13.37 16.22 1.92 0.116 0.94 -2 -1 2 243.16 223.19 1.91 0.430 1.89 1 1 0 341.07 371.69 1.91 0.555 3.96 2 -2 8 11.35 14.38 1.90 0.109 0.78 -3 5 4 22.28 18.43 1.89 0.124 0.78 Bond lengths and angles C1 - Distance Angles O1A 1.2220 (0.0030) O1B 1.2942 (0.0028) 125.89 (0.22) C2 1.5215 (0.0032) 119.96 (0.20) 114.14 (0.19) C1 - O1A O1B C2 - Distance Angles O2 1.4147 (0.0028) C1 1.5215 (0.0032) 110.35 (0.18) C3 1.5337 (0.0030) 109.65 (0.18) 109.84 (0.18) H2 1.0000 108.99 108.99 108.99 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4119 (0.0028) C4 1.5291 (0.0031) 114.39 (0.19) C2 1.5337 (0.0030) 111.61 (0.18) 107.91 (0.18) H3 1.0000 107.55 107.55 107.55 C3 - O3 C4 C2 C4 - Distance Angles O4B 1.2452 (0.0030) O4A 1.2681 (0.0030) 125.23 (0.22) C3 1.5291 (0.0031) 117.31 (0.21) 117.44 (0.21) C4 - O4B O4A O1A - Distance Angles C1 1.2220 (0.0030) O1A - O1B - Distance Angles C1 1.2942 (0.0028) H1 0.8400 109.47 O1B - C1 O2 - Distance Angles C2 1.4147 (0.0028) H2O 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4119 (0.0028) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.2681 (0.0030) O4A - O4B - Distance Angles C4 1.2452 (0.0030) O4B - C21 - Distance Angles N22 1.4811 (0.0031) H21B 0.9800 109.47 H21C 0.9800 109.47 109.47 H21A 0.9800 109.47 109.47 109.47 C21 - N22 H21B H21C N22 - Distance Angles C21 1.4811 (0.0031) H22B 0.9100 109.47 H22C 0.9100 109.47 109.47 H22A 0.9100 109.47 109.47 109.47 N22 - C21 H22B H22C Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.15 2.637(2) 117.0 O2-H2O...O1A 0.91 1.88 2.785(3) 173.7 N22-H22B...O1A 0.84 1.66 2.480(2) 166.6 O1B-H1...O4A_$1 0.91 2.29 2.951(3) 129.5 N22-H22A...O2_$1 0.84 2.13 2.858(2) 144.7 O2-H2O...O3_$2 0.84 1.97 2.780(2) 163.2 O3-H3O...O4B_$3 0.91 1.85 2.753(3) 173.9 N22-H22C...O4B_$4 0.91 2.38 3.080(3) 134.2 N22-H22A...O4A_$5 FMAP and GRID set by program FMAP 2 1 26 GRID -4.348 -2 -2 4.348 2 2 R1 = 0.0381 for 905 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.23 at 0.4710 0.0928 0.8258 [ 0.71 A from H1 ] Deepest hole -0.19 at 0.4827 0.0358 0.9272 [ 0.29 A from H1 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 1744 / 13800 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4710 0.0928 -0.1742 1.00000 0.05 0.23 0.71 H1 0.95 O4A 1.55 O1B 1.85 C4 Q2 1 0.5238 0.0219 0.3475 1.00000 0.05 0.19 0.70 C2 0.84 C3 1.36 H2 1.43 H3 Q3 1 0.4780 -0.0635 0.2369 1.00000 0.05 0.19 0.77 C2 0.78 C1 1.50 H2 1.73 O1B Q4 1 0.2759 0.0136 0.7968 1.00000 0.05 0.18 1.10 O4A 1.71 H1 1.82 H22B 2.01 H22C Q5 1 0.1720 -0.0853 0.4816 1.00000 0.05 0.18 1.43 O2 1.52 H3O 1.67 H2O 2.01 O4B Q6 1 0.1795 -0.4272 0.1722 1.00000 0.05 0.17 1.39 O1A 1.94 O3 1.97 H22B 2.04 H2O Q7 1 0.0955 -0.0701 -0.1913 1.00000 0.05 0.16 1.06 H22C 1.28 H22B 1.42 N22 1.98 H22A Q8 1 0.4199 -0.0416 0.7071 1.00000 0.05 0.16 0.99 O4A 1.44 C4 1.93 H1 2.26 H22B Q9 1 0.1563 -0.1389 0.0402 1.00000 0.05 0.16 0.86 O1A 1.37 H22B 1.86 C1 2.22 N22 Q10 1 0.2700 -0.1517 -0.2760 1.00000 0.05 0.15 1.37 H22C 1.43 H22A 1.46 N22 1.52 H22B Shortest distances between peaks (including symmetry equivalents) 4 8 0.99 8 10 1.04 2 3 1.09 4 7 1.09 7 10 1.11 4 10 1.13 1 4 1.22 1 8 1.32 6 9 1.65 7 9 1.76 7 8 1.78 5 10 1.90 4 9 1.93 2 5 2.09 1 10 2.11 3 5 2.28 1 7 2.29 5 8 2.31 9 10 2.39 5 7 2.46 1 9 2.48 3 9 2.48 4 5 2.66 2 8 2.66 8 9 2.71 3 6 2.83 Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.20: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.14: Structure factors and derivatives 0.20: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.11: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 05skc0002p1 finished at 12:37:05 Total CPU time: 0.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++