+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0001pbca started at 12:49:50 on 14-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0001pbca in Pbca CELL 0.71073 13.3732 8.5025 27.6932 90.000 90.000 90.000 ZERR 8.00 0.0016 0.0009 0.0034 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O UNIT 96 224 16 48 V = 3148.87 F(000) = 1296.0 Mu = 0.10 mm-1 Cell Wt = 2370.91 Rho = 1.250 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB N25 O1A HTAB N25 O2 HTAB N35 O3 HTAB N35 O4B EQIV_$1 -x+3/2, y+1/2, z HTAB O2 O4B_$1 HTAB N25 O2_$1 EQIV_$2 -x+1, -y, -z+1 HTAB O3 O1B_$2 EQIV_$3 x, y+1, z HTAB N25 O4A_$3 EQIV_$4 x+1/2, -y+1/2, -z+1 HTAB N35 O1B_$4 EQIV_$5 -x+3/2, y-1/2, z HTAB N35 O1A_$5 FMAP 2 PLAN 10 SIZE 0.02 0.09 0.11 ACTA 50 BOND $H WGHT 0.00000 19.30320 L.S. 4 TEMP -153.00 FVAR 0.50784 MOLE 1 C1 1 0.505249 0.237191 0.432441 11.00000 0.03200 0.02786 = 0.01717 0.00410 -0.00834 0.00100 C2 1 0.560169 0.097061 0.408753 11.00000 0.03049 0.03251 = 0.02310 -0.00623 0.00052 0.00253 AFIX 13 H2 2 0.515104 0.054976 0.382997 11.00000 -1.20000 AFIX 0 C3 1 0.578026 -0.036082 0.444495 11.00000 0.02501 0.03201 = 0.02364 0.00152 -0.00973 -0.00734 AFIX 13 H3 2 0.511450 -0.078870 0.454381 11.00000 -1.20000 AFIX 0 C4 1 0.637140 -0.168865 0.421141 11.00000 0.03499 0.02298 = 0.02746 0.00608 0.00249 -0.00483 O1A 4 0.543431 0.371031 0.427957 11.00000 0.02951 0.02761 = 0.03301 0.00048 0.00224 0.00161 O1B 4 0.424250 0.208460 0.453876 11.00000 0.03095 0.03542 = 0.03001 0.00019 0.00599 -0.00056 O2 4 0.650250 0.143540 0.385814 11.00000 0.02233 0.03715 = 0.02718 -0.00036 0.00113 -0.00165 AFIX 147 H20 2 0.691286 0.174446 0.406726 11.00000 -1.5 AFIX 0 O3 4 0.625859 0.025748 0.486590 11.00000 0.03359 0.02964 = 0.02231 0.00305 -0.00337 0.00203 AFIX 147 H3O 2 0.624211 -0.041635 0.508758 11.00000 -1.50000 AFIX 0 O4A 4 0.599932 -0.224759 0.383022 11.00000 0.03922 0.03469 = 0.03367 -0.01243 -0.00717 0.00770 O4B 4 0.717110 -0.212414 0.440958 11.00000 0.02319 0.04005 = 0.03616 -0.00149 -0.00252 0.00913 MOLE 2 C21 1 0.408647 0.431168 0.229512 11.00000 0.04157 0.08494 = 0.03387 -0.00435 -0.00513 -0.00241 AFIX 137 H21A 2 0.373408 0.349856 0.247937 11.00000 -1.50000 H21B 2 0.399551 0.412149 0.194887 11.00000 -1.50000 H21C 2 0.381556 0.534750 0.237864 11.00000 -1.50000 AFIX 0 C22 1 0.518351 0.426175 0.241567 11.00000 0.03656 0.05612 = 0.03253 -0.00180 0.00239 0.00342 AFIX 23 H22A 2 0.553549 0.506711 0.222133 11.00000 -1.20000 H22B 2 0.545360 0.322048 0.232303 11.00000 -1.20000 AFIX 0 C23 1 0.540346 0.454776 0.294650 11.00000 0.03479 0.04453 = 0.02534 -0.00106 -0.00129 -0.00268 AFIX 23 H23A 2 0.511429 0.557288 0.304262 11.00000 -1.20000 H23B 2 0.507295 0.371993 0.314072 11.00000 -1.20000 AFIX 0 C24 1 0.651099 0.455003 0.305935 11.00000 0.03365 0.03699 = 0.02400 -0.00187 0.00305 0.00599 AFIX 23 H24A 2 0.679553 0.350317 0.298443 11.00000 -1.20000 H24B 2 0.685144 0.533573 0.285301 11.00000 -1.20000 AFIX 0 N25 3 0.669464 0.492239 0.356700 11.00000 0.02615 0.03050 = 0.02885 -0.00283 -0.00226 0.00428 AFIX 137 H25A 2 0.640075 0.418135 0.375693 11.00000 -1.5 H25B 2 0.643259 0.588380 0.363653 11.00000 -1.5 H25C 2 0.736491 0.493382 0.362356 11.00000 -1.5 AFIX 0 MOLE 3 C31 1 0.761255 -0.178300 0.669058 11.00000 0.05405 0.07496 = 0.03894 0.00979 0.00248 -0.00670 AFIX 137 H31A 2 0.769011 -0.071177 0.681571 11.00000 -1.50000 H31B 2 0.780449 -0.254062 0.694064 11.00000 -1.50000 H31C 2 0.691352 -0.195759 0.659891 11.00000 -1.50000 AFIX 0 C32 1 0.827856 -0.199853 0.625099 11.00000 0.04335 0.04685 = 0.03571 0.00539 -0.00376 -0.00760 AFIX 23 H32A 2 0.816794 -0.306102 0.611487 11.00000 -1.20000 H32B 2 0.898727 -0.192708 0.635194 11.00000 -1.20000 AFIX 0 C33 1 0.807645 -0.077134 0.586057 11.00000 0.03368 0.04262 = 0.02373 -0.00257 -0.00207 -0.00514 AFIX 23 H33A 2 0.734880 -0.072405 0.579641 11.00000 -1.20000 H33B 2 0.829076 0.027473 0.597863 11.00000 -1.20000 AFIX 0 C34 1 0.861930 -0.114064 0.539696 11.00000 0.02776 0.03570 = 0.03127 -0.00117 -0.00609 -0.00365 AFIX 23 H34A 2 0.934424 -0.124077 0.546252 11.00000 -1.20000 H34B 2 0.837841 -0.215790 0.526766 11.00000 -1.20000 AFIX 0 N35 3 0.845111 0.012670 0.502911 11.00000 0.02823 0.03986 = 0.02862 -0.00554 -0.00086 -0.00102 AFIX 137 H35A 2 0.880468 -0.009853 0.475700 11.00000 -1.5 H35B 2 0.865813 0.106601 0.515083 11.00000 -1.5 H35C 2 0.778847 0.018156 0.495632 11.00000 -1.5 AFIX 0 HKLF 4 Covalent radii and connectivity table for 07skc0001pbca in Pbca C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - O2 C3 C1 C3 - O3 C4 C2 C4 - O4B O4A C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C21 - C22 C22 - C21 C23 C23 - C24 C22 C24 - N25 C23 N25 - C24 C31 - C32 C32 - C31 C33 C33 - C34 C32 C34 - N35 C33 N35 - C34 Operators for generating equivalent atoms: $1 -x+3/2, y+1/2, z $2 -x+1, -y, -z+1 $3 x, y+1, z $4 x+1/2, -y+1/2, -z+1 $5 -x+3/2, y-1/2, z h k l Fo^2 Sigma Why rejected 0 1 13 64.10 15.30 observed but should be systematically absent 8 0 27 193.39 48.20 observed but should be systematically absent 14749 Reflections read, of which 1209 rejected -15 =< h =< 17, -10 =< k =< 10, -24 =< l =< 35, Max. 2-theta = 54.96 2 Systematic absence violations 0 Inconsistent equivalents 3058 Unique reflections, of which 0 suppressed R(int) = 0.0955 R(sigma) = 0.1238 Friedel opposites merged Maximum memory for data reduction = 2717 / 31433 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 = 3312 / 232061 wR2 = 0.2355 before cycle 1 for 3058 data and 187 / 187 parameters GooF = S = 1.146; Restrained GooF = 1.146 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 19.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50782 0.00182 -0.008 OSF Mean shift/esd = 0.061 Maximum = -0.662 for U13 N35 Max. shift = 0.011 A for H25C Max. dU = 0.000 for C31 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3312 / 232061 wR2 = 0.2354 before cycle 2 for 3058 data and 187 / 187 parameters GooF = S = 1.145; Restrained GooF = 1.145 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 19.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50782 0.00182 -0.004 OSF Mean shift/esd = 0.025 Maximum = -0.298 for U13 N35 Max. shift = 0.005 A for H3O Max. dU = 0.000 for N25 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3312 / 232061 wR2 = 0.2353 before cycle 3 for 3058 data and 187 / 187 parameters GooF = S = 1.145; Restrained GooF = 1.145 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 19.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50782 0.00182 -0.001 OSF Mean shift/esd = 0.005 Maximum = -0.038 for U13 N35 Max. shift = 0.002 A for H3O Max. dU = 0.000 for O4B Least-squares cycle 4 Maximum vector length = 511 Memory required = 3312 / 232061 wR2 = 0.2353 before cycle 4 for 3058 data and 187 / 187 parameters GooF = S = 1.145; Restrained GooF = 1.145 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 19.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50782 0.00182 0.001 OSF Mean shift/esd = 0.001 Maximum = -0.011 for tors H3O Max. shift = 0.001 A for H3O Max. dU = 0.000 for C3 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 H2 0.5151 0.0550 0.3830 13 1.000 0.000 C2 O2 C3 C1 H3 0.5115 -0.0788 0.4544 13 1.000 0.000 C3 O3 C4 C2 H20 0.6915 0.1737 0.4068 147 0.840 0.000 O2 C2 H20 H3O 0.6232 -0.0410 0.5089 147 0.840 0.000 O3 C3 H3O H21A 0.3734 0.3500 0.2479 137 0.980 0.000 C21 C22 H21A H21B 0.3996 0.4123 0.1949 137 0.980 0.000 C21 C22 H21A H21C 0.3816 0.5349 0.2379 137 0.980 0.000 C21 C22 H21A H22A 0.5536 0.5066 0.2221 23 0.990 0.000 C22 C21 C23 H22B 0.5453 0.3219 0.2323 23 0.990 0.000 C22 C21 C23 H23A 0.5114 0.5573 0.3042 23 0.990 0.000 C23 C24 C22 H23B 0.5073 0.3721 0.3141 23 0.990 0.000 C23 C24 C22 H24A 0.6795 0.3502 0.2985 23 0.990 0.000 C24 N25 C23 H24B 0.6852 0.5334 0.2853 23 0.990 0.000 C24 N25 C23 H25A 0.6408 0.4177 0.3757 137 0.910 0.000 N25 C24 H25A H25B 0.6425 0.5880 0.3637 137 0.910 0.000 N25 C24 H25A H25C 0.7365 0.4950 0.3622 137 0.910 0.000 N25 C24 H25A H31A 0.7691 -0.0712 0.6816 137 0.980 0.000 C31 C32 H31A H31B 0.7803 -0.2542 0.6940 137 0.980 0.000 C31 C32 H31A H31C 0.6913 -0.1955 0.6599 137 0.980 0.000 C31 C32 H31A H32A 0.8168 -0.3061 0.6115 23 0.990 0.000 C32 C31 C33 H32B 0.8987 -0.1926 0.6352 23 0.990 0.000 C32 C31 C33 H33A 0.7349 -0.0725 0.5796 23 0.990 0.000 C33 C34 C32 H33B 0.8291 0.0275 0.5979 23 0.990 0.000 C33 C34 C32 H34A 0.9344 -0.1241 0.5463 23 0.990 0.000 C34 N35 C33 H34B 0.8379 -0.2159 0.5268 23 0.990 0.000 C34 N35 C33 H35A 0.8811 -0.0100 0.4757 137 0.910 0.000 N35 C34 H35A H35B 0.8656 0.1065 0.5150 137 0.910 0.000 N35 C34 H35A H35C 0.7791 0.0174 0.4953 137 0.910 0.000 N35 C34 H35A 07skc0001pbca in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.50526 0.23720 0.43245 1.00000 0.03192 0.02782 0.01720 0.00403 -0.00844 0.00118 0.02565 0.01010 0.00046 0.00071 0.00020 0.00000 0.00379 0.00370 0.00291 0.00246 0.00274 0.00305 0.00140 C2 0.56015 0.09709 0.40875 1.00000 0.03075 0.03275 0.02277 -0.00640 0.00053 0.00253 0.02876 0.01038 0.00045 0.00069 0.00021 0.00000 0.00372 0.00371 0.00306 0.00267 0.00275 0.00294 0.00147 H2 0.51513 0.05504 0.38297 1.00000 0.03451 0.00000 0.00000 C3 0.57803 -0.03606 0.44448 1.00000 0.02476 0.03199 0.02367 0.00172 -0.00965 -0.00716 0.02681 0.00955 0.00045 0.00068 0.00020 0.00000 0.00335 0.00357 0.00305 0.00268 0.00258 0.00283 0.00142 H3 0.51146 -0.07884 0.45437 1.00000 0.03217 0.00000 0.00000 C4 0.63712 -0.16888 0.42112 1.00000 0.03475 0.02314 0.02742 0.00579 0.00252 -0.00496 0.02843 0.01076 0.00048 0.00068 0.00022 0.00000 0.00386 0.00344 0.00328 0.00263 0.00296 0.00296 0.00144 O1A 0.54344 0.37105 0.42796 1.00000 0.02951 0.02747 0.03323 0.00040 0.00227 0.00167 0.03007 0.00706 0.00030 0.00047 0.00014 0.00000 0.00242 0.00251 0.00245 0.00193 0.00196 0.00206 0.00102 O1B 0.42425 0.20847 0.45386 1.00000 0.03098 0.03545 0.03007 0.00013 0.00607 -0.00042 0.03217 0.00707 0.00031 0.00047 0.00015 0.00000 0.00259 0.00255 0.00237 0.00198 0.00206 0.00202 0.00105 O2 0.65034 0.14367 0.38586 1.00000 0.02261 0.03674 0.02741 0.00024 0.00176 -0.00112 0.02892 0.00690 0.00028 0.00050 0.00014 0.00000 0.00240 0.00253 0.00222 0.00196 0.00184 0.00200 0.00100 H20 0.69153 0.17369 0.40682 1.00000 0.04338 0.00000 0.00000 O3 0.62588 0.02574 0.48657 1.00000 0.03340 0.02972 0.02218 0.00309 -0.00304 0.00202 0.02844 0.00663 0.00031 0.00046 0.00013 0.00000 0.00251 0.00238 0.00206 0.00177 0.00192 0.00202 0.00100 H3O 0.62321 -0.04095 0.50891 1.00000 0.04265 0.00000 0.00000 O4A 0.59993 -0.22477 0.38302 1.00000 0.03924 0.03448 0.03371 -0.01242 -0.00720 0.00774 0.03581 0.00708 0.00031 0.00049 0.00015 0.00000 0.00275 0.00255 0.00249 0.00207 0.00212 0.00213 0.00112 O4B 0.71708 -0.21241 0.44096 1.00000 0.02320 0.04008 0.03642 -0.00129 -0.00249 0.00911 0.03323 0.00715 0.00030 0.00049 0.00015 0.00000 0.00247 0.00269 0.00249 0.00214 0.00197 0.00206 0.00108 C21 0.40865 0.43126 0.22951 1.00000 0.04158 0.08529 0.03366 -0.00430 -0.00517 -0.00222 0.05351 0.01238 0.00052 0.00097 0.00025 0.00000 0.00453 0.00604 0.00387 0.00400 0.00348 0.00427 0.00211 H21A 0.37337 0.34996 0.24792 1.00000 0.08026 0.00000 0.00000 H21B 0.39956 0.41231 0.19488 1.00000 0.08026 0.00000 0.00000 H21C 0.38161 0.53486 0.23788 1.00000 0.08026 0.00000 0.00000 C22 0.51837 0.42611 0.24158 1.00000 0.03637 0.05654 0.03276 -0.00184 0.00259 0.00360 0.04189 0.01182 0.00049 0.00086 0.00023 0.00000 0.00434 0.00470 0.00386 0.00333 0.00313 0.00357 0.00180 H22A 0.55363 0.50655 0.22213 1.00000 0.05026 0.00000 0.00000 H22B 0.54532 0.32192 0.23234 1.00000 0.05026 0.00000 0.00000 C23 0.54033 0.45480 0.29465 1.00000 0.03503 0.04454 0.02541 -0.00118 -0.00137 -0.00266 0.03499 0.01078 0.00048 0.00081 0.00022 0.00000 0.00390 0.00403 0.00326 0.00298 0.00290 0.00327 0.00158 H23A 0.51143 0.55734 0.30424 1.00000 0.04199 0.00000 0.00000 H23B 0.50725 0.37206 0.31408 1.00000 0.04199 0.00000 0.00000 C24 0.65108 0.45499 0.30593 1.00000 0.03350 0.03727 0.02380 -0.00199 0.00317 0.00615 0.03152 0.01065 0.00045 0.00077 0.00021 0.00000 0.00386 0.00375 0.00306 0.00277 0.00277 0.00314 0.00151 H24A 0.67950 0.35024 0.29850 1.00000 0.03783 0.00000 0.00000 H24B 0.68516 0.53342 0.28526 1.00000 0.03783 0.00000 0.00000 N25 0.66945 0.49248 0.35667 1.00000 0.02528 0.03143 0.02829 -0.00175 -0.00208 0.00332 0.02833 0.00811 0.00036 0.00057 0.00017 0.00000 0.00280 0.00301 0.00264 0.00226 0.00224 0.00238 0.00120 H25A 0.64081 0.41772 0.37569 1.00000 0.04250 0.00000 0.00000 H25B 0.64248 0.58804 0.36368 1.00000 0.04250 0.00000 0.00000 H25C 0.73650 0.49500 0.36223 1.00000 0.04250 0.00000 0.00000 C31 0.76124 -0.17826 0.66906 1.00000 0.05392 0.07451 0.03902 0.00984 0.00285 -0.00665 0.05582 0.01349 0.00057 0.00095 0.00025 0.00000 0.00501 0.00584 0.00412 0.00405 0.00394 0.00437 0.00217 H31A 0.76910 -0.07121 0.68161 1.00000 0.08373 0.00000 0.00000 H31B 0.78031 -0.25417 0.69404 1.00000 0.08373 0.00000 0.00000 H31C 0.69133 -0.19549 0.65986 1.00000 0.08373 0.00000 0.00000 C32 0.82788 -0.19983 0.62510 1.00000 0.04346 0.04713 0.03523 0.00519 -0.00381 -0.00754 0.04194 0.01197 0.00053 0.00082 0.00023 0.00000 0.00418 0.00448 0.00386 0.00329 0.00324 0.00348 0.00177 H32A 0.81684 -0.30610 0.61150 1.00000 0.05033 0.00000 0.00000 H32B 0.89874 -0.19264 0.63521 1.00000 0.05033 0.00000 0.00000 C33 0.80764 -0.07714 0.58605 1.00000 0.03382 0.04257 0.02355 -0.00219 -0.00186 -0.00483 0.03332 0.01070 0.00047 0.00075 0.00021 0.00000 0.00387 0.00419 0.00319 0.00289 0.00283 0.00315 0.00160 H33A 0.73488 -0.07245 0.57963 1.00000 0.03998 0.00000 0.00000 H33B 0.82905 0.02749 0.59785 1.00000 0.03998 0.00000 0.00000 C34 0.86195 -0.11410 0.53970 1.00000 0.02811 0.03584 0.03089 -0.00128 -0.00600 -0.00370 0.03162 0.01030 0.00046 0.00071 0.00021 0.00000 0.00364 0.00373 0.00338 0.00292 0.00293 0.00302 0.00150 H34A 0.93444 -0.12413 0.54628 1.00000 0.03794 0.00000 0.00000 H34B 0.83789 -0.21589 0.52680 1.00000 0.03794 0.00000 0.00000 N35 0.84529 0.01237 0.50280 1.00000 0.02781 0.03766 0.03104 -0.00551 -0.00320 -0.00195 0.03217 0.00839 0.00037 0.00059 0.00018 0.00000 0.00301 0.00310 0.00278 0.00240 0.00234 0.00253 0.00126 H35A 0.88108 -0.01004 0.47571 1.00000 0.04825 0.00000 0.00000 H35B 0.86557 0.10649 0.51500 1.00000 0.04825 0.00000 0.00000 H35C 0.77911 0.01738 0.49531 1.00000 0.04825 0.00000 0.00000 Final Structure Factor Calculation for 07skc0001pbca in Pbca Total number of l.s. parameters = 187 Maximum vector length = 511 Memory required = 3125 / 22995 wR2 = 0.2353 before cycle 5 for 3058 data and 0 / 187 parameters GooF = S = 1.145; Restrained GooF = 1.145 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 19.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1244 for 1695 Fo > 4sig(Fo) and 0.2187 for all 3058 data wR2 = 0.2353, GooF = S = 1.145, Restrained GooF = 1.145 for all data Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0358 0.0289 0.0123 C1 0.0366 0.0303 0.0194 C2 0.0396 0.0271 0.0137 C3 0.0366 0.0313 0.0174 C4 0.0345 0.0293 0.0264 O1A 0.0367 0.0354 0.0244 O1B 0.0368 0.0280 0.0220 O2 0.0345 0.0306 0.0201 O3 0.0541 0.0317 0.0217 O4A 0.0446 0.0360 0.0190 O4B 0.0857 0.0441 0.0307 C21 0.0572 0.0375 0.0310 C22 0.0453 0.0346 0.0251 C23 0.0418 0.0309 0.0218 C24 0.0340 0.0276 0.0235 N25 0.0784 0.0537 0.0354 C31 0.0551 0.0375 0.0331 C32 0.0448 0.0324 0.0227 C33 0.0376 0.0349 0.0223 C34 0.0408 0.0316 0.0241 N35 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.018 0.027 0.038 0.050 0.065 0.086 0.117 0.169 1.000 Number in group 313. 322. 285. 320. 292. 307. 309. 296. 308. 306. GooF 1.197 1.199 1.181 1.148 1.168 1.122 1.231 1.262 0.940 0.964 K 43.342 5.967 2.493 1.768 1.230 1.150 1.069 1.057 1.002 1.008 Resolution(A) 0.77 0.81 0.85 0.90 0.95 1.02 1.10 1.21 1.39 1.74 inf Number in group 311. 307. 304. 306. 300. 308. 310. 300. 306. 306. GooF 1.343 1.338 1.181 1.175 1.276 1.177 1.044 0.982 0.931 0.897 K 2.081 1.651 1.424 1.182 1.102 1.037 1.003 0.999 0.995 1.010 R1 0.549 0.482 0.391 0.359 0.290 0.213 0.135 0.128 0.085 0.038 Recommended weighting scheme: WGHT 0.0000 19.2434 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) 5 8 6 -0.22 435.15 5.22 0.107 0.97 10 8 11 1171.98 18.54 4.66 0.022 0.79 6 6 8 528.30 1246.28 4.25 0.181 1.13 11 5 19 688.15 129.37 3.78 0.058 0.82 8 7 12 -12.80 348.71 3.65 0.096 0.90 1 9 18 1437.21 493.96 3.48 0.114 0.80 6 0 22 33.85 404.32 3.45 0.103 1.10 1 7 17 -9.87 230.18 3.31 0.078 0.97 4 3 30 351.24 4.93 3.29 0.011 0.85 2 0 0 562.78 1143.24 3.25 0.174 6.69 5 8 13 190.75 0.66 3.21 0.004 0.90 7 4 26 345.35 14.09 3.06 0.019 0.85 10 1 13 161.37 14.83 3.02 0.020 1.12 1 5 20 208.86 22.09 2.98 0.024 1.07 9 6 22 653.33 0.15 2.97 0.002 0.80 6 8 2 7.02 172.26 2.96 0.067 0.96 2 4 30 249.33 9.00 2.91 0.015 0.84 7 5 24 246.10 13.26 2.90 0.019 0.85 4 7 23 736.54 119.60 2.90 0.056 0.83 11 5 4 -37.58 136.04 2.90 0.060 0.98 12 5 19 493.03 83.79 2.89 0.047 0.79 11 4 23 1269.73 497.73 2.88 0.115 0.79 3 4 22 294.81 74.23 2.84 0.044 1.05 15 1 1 87.56 382.46 2.81 0.100 0.89 4 8 7 -1.20 231.02 2.80 0.078 0.98 13 5 15 232.77 6.75 2.78 0.013 0.79 5 8 21 558.98 19.94 2.78 0.023 0.79 2 0 26 276.52 38.48 2.73 0.032 1.05 6 6 12 318.56 48.27 2.70 0.036 1.06 3 5 14 212.92 495.71 2.69 0.114 1.24 12 2 22 948.08 257.94 2.68 0.082 0.82 12 4 18 290.17 38.15 2.67 0.032 0.83 11 2 25 267.40 0.01 2.67 0.001 0.80 2 9 12 556.03 68.47 2.67 0.043 0.87 5 5 11 321.02 667.27 2.64 0.133 1.25 12 2 21 850.59 10.71 2.63 0.017 0.83 10 1 25 311.49 40.73 2.62 0.033 0.85 9 5 7 186.96 464.88 2.62 0.111 1.08 2 8 22 439.85 94.94 2.62 0.050 0.81 9 2 26 258.59 17.70 2.61 0.022 0.85 12 4 10 798.82 262.91 2.60 0.083 0.93 8 0 8 934.50 1477.48 2.59 0.197 1.51 1 5 23 162.39 0.80 2.57 0.005 0.98 6 7 12 -130.47 146.46 2.57 0.062 0.97 7 5 25 228.98 1.27 2.56 0.006 0.83 10 2 23 471.54 38.33 2.56 0.032 0.88 5 2 30 293.23 52.29 2.54 0.037 0.85 13 5 10 1160.96 480.13 2.53 0.113 0.84 2 3 34 215.01 0.33 2.53 0.003 0.78 11 4 10 422.58 177.02 2.52 0.068 0.99 Bond lengths and angles C1 - Distance Angles O1A 1.2535 (0.0069) O1B 1.2590 (0.0068) 124.99 (0.56) C2 1.5455 (0.0081) 117.66 (0.53) 117.33 (0.53) C1 - O1A O1B C2 - Distance Angles O2 1.4190 (0.0068) C3 1.5224 (0.0079) 111.37 (0.48) C1 1.5455 (0.0081) 112.23 (0.49) 111.83 (0.47) H2 1.0000 107.02 107.02 107.02 C2 - O2 C3 C1 C3 - Distance Angles O3 1.4298 (0.0063) C4 1.5225 (0.0083) 112.75 (0.48) C2 1.5224 (0.0079) 109.07 (0.46) 110.92 (0.46) H3 1.0000 107.98 107.98 107.98 C3 - O3 C4 C2 C4 - Distance Angles O4B 1.2579 (0.0070) O4A 1.2595 (0.0070) 126.20 (0.58) C3 1.5225 (0.0083) 118.29 (0.53) 115.52 (0.54) C4 - O4B O4A O1A - Distance Angles C1 1.2535 (0.0069) O1A - O1B - Distance Angles C1 1.2590 (0.0069) O1B - O2 - Distance Angles C2 1.4190 (0.0068) H20 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4298 (0.0063) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.2595 (0.0070) O4A - O4B - Distance Angles C4 1.2579 (0.0070) O4B - C21 - Distance Angles C22 1.5055 (0.0091) 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 C21 1.5055 (0.0091) C23 1.5185 (0.0083) 113.49 (0.55) H22A 0.9900 108.87 108.87 H22B 0.9900 108.87 108.87 107.71 C22 - C21 C23 H22A C23 - Distance Angles C24 1.5138 (0.0085) C22 1.5185 (0.0083) 112.90 (0.52) H23A 0.9900 109.01 109.01 H23B 0.9900 109.01 109.01 107.79 C23 - C24 C22 H23A C24 - Distance Angles N25 1.4615 (0.0069) C23 1.5138 (0.0085) 111.29 (0.48) H24A 0.9900 109.37 109.37 H24B 0.9900 109.37 109.37 108.00 C24 - N25 C23 H24A N25 - Distance Angles C24 1.4615 (0.0069) H25A 0.9100 109.47 H25B 0.9100 109.47 109.47 H25C 0.9100 109.47 109.47 109.47 N25 - C24 H25A H25B C31 - Distance Angles C32 1.5197 (0.0091) H31A 0.9800 109.47 H31B 0.9800 109.47 109.47 H31C 0.9800 109.47 109.47 109.47 C31 - C32 H31A H31B C32 - Distance Angles C31 1.5197 (0.0090) C33 1.5268 (0.0085) 112.39 (0.59) H32A 0.9900 109.12 109.12 H32B 0.9900 109.12 109.12 107.85 C32 - C31 C33 H32A C33 - Distance Angles C34 1.5080 (0.0080) C32 1.5268 (0.0085) 112.04 (0.54) H33A 0.9900 109.20 109.20 H33B 0.9900 109.20 109.20 107.90 C33 - C34 C32 H33A C34 - Distance Angles N35 1.5000 (0.0074) C33 1.5080 (0.0080) 111.03 (0.49) H34A 0.9900 109.43 109.43 H34B 0.9900 109.43 109.43 108.03 C34 - N35 C33 H34A N35 - Distance Angles C34 1.5000 (0.0074) H35A 0.9100 109.47 H35B 0.9100 109.47 109.47 H35C 0.9100 109.47 109.47 109.47 N35 - C34 H35A H35B Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.99 2.793(6) 146.8 N25-H25A...O1A 0.91 2.35 3.084(6) 137.6 N25-H25A...O2 0.91 2.06 2.971(6) 173.5 N35-H35C...O3 0.91 2.60 3.086(6) 114.0 N35-H35C...O4B 0.84 1.82 2.640(6) 163.6 O2-H20...O4B_$1 0.91 2.08 2.848(6) 141.8 N25-H25C...O2_$1 0.84 1.87 2.671(6) 159.2 O3-H3O...O1B_$2 0.91 1.77 2.679(6) 173.3 N25-H25B...O4A_$3 0.91 1.96 2.862(6) 171.7 N35-H35B...O1B_$4 0.91 1.95 2.820(6) 160.3 N35-H35A...O1A_$5 FMAP and GRID set by program FMAP 2 2 13 GRID -2.500 24 -2 2.500 1 2 R1 = 0.2185 for 3058 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.45 at 0.3992 0.1533 0.4815 [ 0.96 A from O1B ] Deepest hole -0.35 at 0.6603 0.0016 0.5795 [ 1.18 A from H33A ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 3994 / 32699 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3992 0.1533 0.4815 1.00000 0.05 0.45 0.96 O1B 1.04 H3O 1.79 O3 2.09 C1 Q2 1 0.3456 0.1798 0.4599 1.00000 0.05 0.41 1.09 O1B 1.52 H3O 1.79 H33A 1.96 H35B Q3 1 0.6798 0.2798 0.3185 1.00000 0.05 0.35 0.82 H24A 1.58 C24 2.04 H25A 2.10 N25 Q4 1 0.7663 0.4275 0.2969 1.00000 0.05 0.34 1.33 H24A 1.45 H24B 1.58 C24 1.80 H21B Q5 1 0.3608 0.4989 0.1924 1.00000 0.05 0.32 0.90 H21B 1.32 H21C 1.34 C21 2.00 H21A Q6 1 0.5418 0.3051 0.4503 1.00000 0.05 0.32 0.84 O1A 0.90 C1 1.78 O1B 2.01 H35A Q7 1 0.4359 0.2063 0.4078 1.00000 0.05 0.32 1.18 C1 1.29 O1B 1.80 H2 1.90 C2 Q8 1 0.6581 0.4992 0.4129 1.00000 0.05 0.32 1.26 H25A 1.57 N25 1.57 H25B 1.75 H25C Q9 1 0.4652 -0.0947 0.3716 1.00000 0.05 0.31 1.47 H2 2.02 H32B 2.14 O4A 2.21 H32A Q10 1 0.6427 0.0264 0.4417 1.00000 0.05 0.31 1.02 C3 1.26 O3 1.55 C2 1.71 H20 Shortest distances between peaks (including symmetry equivalents) 1 2 0.96 4 5 1.43 3 4 1.81 2 7 1.90 6 7 2.02 1 7 2.15 1 6 2.46 3 5 2.47 6 8 2.49 1 10 2.68 6 10 2.74 7 9 2.78 8 10 2.79 2 6 2.84 Time profile in seconds ----------------------- 0.11: 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. 0.81: 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 1.16: Structure factors and derivatives 0.75: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.03: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0001pbca finished at 12:49:53 Total CPU time: 3.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++