SHELXL-972006-10-102007-03-09Acta Crystallographica, Section B2007633459468FABK5044monoclinicP 2yb1374.01.525.0298.0Platecolourless0.420.270.151.44not measured532.00.119none298.0MoK\a0.71073fine-focus sealed tubegraphiteBruker SMART CCD area detector\f and \w scan8353.00.01580.01411.5325.025.00.9980.998-11.011.0-10.09.0-16.016.00.00.0Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.2162.02054.0I>2\s(I)Fsqdfull0.03580.03390.08680.08811.0641.0632162.0380.02.0mixedcalccalc w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+0.2589P] where P=(Fo^2^+2Fc^2^)/3directdifmap0.00.00.372-0.174SHELXL0.0074Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^Bruker SMARTBruker SMARTBruker SAINTSHELXS-97 (Sheldrick, 1997)SHELXL-97 (Sheldrick, 1997)Ortep-3 (Farrugia, 1997) and PyMOL (DeLano, 2002)PLATON (Spek, 2003)All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.
|C|H|N|O||C|H|N|O||0.0033|0.0|0.0061|0.0106||0.0|0.0|0.0|0.0||International Tables Vol C Tables 4.2.6.8 and 6.1.1.4|International Tables Vol C Tables 4.2.6.8 and 6.1.1.4|International Tables Vol C Tables 4.2.6.8 and 6.1.1.4|International Tables Vol C Tables 4.2.6.8 and 6.1.1.4|
organicNo _chemical_absolute_configuration info given . ?Poor Data / Parameter Ratio (Zmax .LT. 18) ..... 5.69Hirshfeld Test Diff for O11 - C11 .. 8.24 suU(iso) H8B Smaller than U(eq) N8 by ... 0.01 AngSqD-H Calc 0.83(3), Rep 0.83000 ...... Missing su O25 -H25 1.555 1.555H...A Calc 2.23(3), Rep 2.23000 ...... Missing su H25 -O1 1.555 1.555D-H..A Calc 131(3), Rep 131.00 ...... Missing su O25 -H25 -O1 1.555 1.555 1.555Centre of Gravity not Within Unit Cell: Resd. # 2 C6 H15 N4 O2Centre of Gravity not Within Unit Cell: Resd. # 3 C4 H4 O6There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C16 H34 N8 O10 Atom count from _chemical_formula_moiety:C4 H4 O6Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 25.00 From the CIF: _reflns_number_total 2162 Count of symmetry unique reflns 2167 Completeness (_total/calc) 99.77% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 0 Fraction of Friedel pairs measured 0.000 Are heavy atom types Z>Si present noConfirm the Absolute Configuration of C2 = . SConfirm the Absolute Configuration of C12 = . SConfirm the Absolute Configuration of C24 = . RConfirm the Absolute Configuration of C26 = . RNote: Number of Least-Squares Restraints ....... 2C-C = 0.0040 A1149.9(4)1149.9(4)P 21P 1 21 1P 2ybP 2yb2(C6 H15 N4 O2), C4 H4 O62(C6 H15 N4 O2) +, C4 H4 O6 2-C16 H34 N8 O10C16 H34 N8 O10498.51498.511.4401.440220.1190.119532.0532.0532.2911,10,1611,10,162167( 4045)21620.962,0.9820.9511.00(0.53)http://dynhost1.iucr.org/tmp/052907140333/platon_IIte.gif10.1107/S010876810701107X9.9078.742814.07690.0109.41290.01.0 0.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 0.0 1.0-1.0 0.0 0.0 0.0 0.0 1.0 0.0 0.5 0.0 0.0 -1.0 0.0 0.0 0.0 0.0 1.00.0475UaniN8.0.045UisoH8A.0.038UisocalcH3BR0.048UisoH1B.0.0386UaniN6.0.0437UaniC5.0.052UisocalcH5BR0.0292UaniC1.0.038UisocalcH3AR0.0343UaniC7.0.0439UaniN9.0.033UisocalcH2R0.049UisocalcH4BR0.042UisoH6.0.0319UaniC3.0.0411UaniC4.0.028UisoH1A.0.032UisoH8B.0.06UisoH9A.0.0372UaniO1.0.035UisoH1C.0.0513UaniO2.0.0281UaniN1.0.052UisocalcH5AR0.0272UaniC2.0.049UisocalcH4AR0.058UisoH9B.0.9083799553754230.96991970256100370.9368350685039590.8982292867054950.97031991851465540.97009639685178220.83706807120875980.96950650808997341.33083926042244221.31858491510440221.49252083779338051.24779610754206231.52570965472173931.2423312087663951.53378151330883731.32292318995974731.51235910169360820.96991951002656931.52201837479250070.85865818085311870.88056050610255950.88865956233573050.96960396539673031.45436410872302520.81988346522162550.9795383342775490.0435UaniC14.0.0428UaniC11.0.0413UaniC13.0.053UisoH18B.0.0445UaniN18.0.0377UaniC12.0.06UisocalcH15AR0.055UisoH11C.0.0359UaniC17.0.0351UaniN11.0.05UisocalcH13AR0.037UisoH16.0.052UisocalcH14AR0.0465UaniO11.0.082UisoH19B.0.05UisocalcH13BR0.0497UaniC15.0.0529UaniN19.0.049UisoH19A.0.06UisocalcH15BR0.045UisoH18A.0.05UisoH11A.0.0466UaniN16.0.043UisoH11B.0.0654UaniO12.0.052UisocalcH14BR0.045UisocalcH12R0.90070273987370091.22050119077326920.98878608434533570.97057879614247271.51327470693954021.51688851043462011.3199345086513971.34294633085626060.90389636148050870.83755915723322271.25942005452958060.96933878741737840.89145959324764261.49354185243285761.30927674187540230.97090043684549740.98019434378391790.90037310470765540.97086504820359580.91110651925870190.93286693567847640.96939376214682041.53239443959522941.44964755045546760.97084114443027151.54285263957174320.054UisoH27.0.0479UaniO29.0.0302UaniC26.-7.5375607294738780.035UisocalcH24R0.051UisoH25D0.029UaniC24.-7.5759046211963860.0436UaniO30.0.0305UaniC23.0.0441UaniO22.0.0322UaniC28.0.0365UaniO25D0.036UisocalcH26R0.0444UaniO21.0.0387UaniO27.1.2381088289023011.2657675800476018W0.97991164843253561.2706965512936130.86122610065201981.23425880538136321.531326496914530.82971052666177381.42394932000462121.41775208663344451.5235523923379255W0.97985272053637431.5422657029620168[H]O[C@]([H])([C@]([H])(C(=O)[O-])O[H])C(=O)[O-]InChI=1/C4H6O6/c5-1(3(7)8)2(6)4(9)10/h1-2,5-6H,(H,7,8)(H,9,10)/p-2/t1-,2-/m1/s1