++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 07skc0026 started at 14:16:08 on 15-May-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.160 12.331 31.378 90.00 92.97 90.00 21783 Reflections read from file 07skc0026.hkl; mean (I/sigma) = 3.26 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10898 10901 10799 10898 16299 14562 14538 21783 N (int>3sigma) = 0 3490 3619 3399 3663 5254 4708 4758 7171 Mean intensity = 0.0 10.5 12.1 8.6 12.2 10.4 11.6 11.0 11.5 Mean int/sigma = 0.0 3.3 3.5 3.3 3.6 3.4 3.4 3.4 3.4 Lattice type: P chosen Volume: 2766.57 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 Unitcell: 7.160 12.331 31.378 90.00 92.97 90.00 Niggli form: a.a = 51.27 b.b = 152.05 c.c = 984.57 b.c = 0.00 a.c = -11.63 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.079 [ 4950] Cell: 7.160 12.331 31.378 90.00 92.97 90.00 Volume: 2766.57 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option A selected ------------------------------------------------------------------------------- TOLERANCES CHANGED Maximum deviation (deg.) in higher symmetry cell search = 1.000 Threshold (deg.) for terminating search = 0.050 R(int) maximum for terminating cell search = 0.120 R(int) maximum for space group determination = 0.300 Minimum number of data in group for syst. absence test = 999 Maximum mean I/sigma(I) for systematic absences = 99.000 Minimum I/sigma gap between absences and rest = 1.000 ------------------------------------------------------------------------------- Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10898 10901 10799 10898 16299 14562 14538 21783 N (int>3sigma) = 0 3490 3619 3399 3663 5254 4708 4758 7171 Mean intensity = 0.0 10.5 12.1 8.6 12.2 10.4 11.6 11.0 11.5 Mean int/sigma = 0.0 3.3 3.5 3.3 3.6 3.4 3.4 3.4 3.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 1.096 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 14 630 608 618 N I>3s 0 7 69 70 0.3 0.7 3.0 3.0 0.5 0.7 1.4 1.4 Identical indices and Friedel opposites combined before calculating R(sym) Option Space Group No. Type Axes CSD R(sym) N(eq) Syst. Abs. CFOM [A] P2 # 3 chiral 1 29 0.079 4950 0.0 / 3.4 19.21 [B] P2/m # 10 centro 1 21 0.079 4950 0.0 / 3.4 9.09 [C] Pm # 6 non-cen 1 1 0.079 4950 0.0 / 3.4 65.88 [D] P2(1) # 4 chiral 1 3543 0.079 4950 0.0 / 3.4 15.90 [E] P2(1)/m # 11 centro 1 402 0.079 4950 0.0 / 3.4 4.80 [F] P2/c # 13 centro 1 292 0.079 4950 0.0 / 3.4 4.89 [G] P2/c # 13 centro 4 292 0.079 4950 0.0 / 3.4 4.89 [H] P2/n # 13 centro 1 292 0.079 4950 0.0 / 3.4 4.89 [I] Pc # 7 non-cen 1 226 0.079 4950 0.0 / 3.4 16.32 [J] Pc # 7 non-cen 4 226 0.079 4950 0.0 / 3.4 16.32 [K] Pn # 7 non-cen 1 226 0.079 4950 0.0 / 3.4 16.32 [L] P2(1)/c # 14 centro 1 19410 0.079 4950 0.0 / 3.4 4.55 [M] P2(1)/c # 14 centro 4 19410 0.079 4950 0.0 / 3.4 4.55 [N] P2(1)/n # 14 centro 1 19410 0.079 4950 0.0 / 3.4 4.55 Option [N] chosen ------------------------------------------------------------------------------- Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10898 10901 10799 10898 16299 14562 14538 21783 N (int>3sigma) = 0 3490 3619 3399 3663 5254 4708 4758 7171 Mean intensity = 0.0 10.5 12.1 8.6 12.2 10.4 11.6 11.0 11.5 Mean int/sigma = 0.0 3.3 3.5 3.3 3.6 3.4 3.4 3.4 3.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 1.096 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 14 630 608 618 N I>3s 0 7 69 70 0.3 0.7 3.0 3.0 0.5 0.7 1.4 1.4 Identical indices and Friedel opposites combined before calculating R(sym) Option Space Group No. Type Axes CSD R(sym) N(eq) Syst. Abs. CFOM [A] P2 # 3 chiral 1 29 0.079 4950 0.0 / 3.4 19.21 [B] P2/m # 10 centro 1 21 0.079 4950 0.0 / 3.4 9.09 [C] Pm # 6 non-cen 1 1 0.079 4950 0.0 / 3.4 65.88 [D] P2(1) # 4 chiral 1 3543 0.079 4950 0.0 / 3.4 15.90 [E] P2(1)/m # 11 centro 1 402 0.079 4950 0.0 / 3.4 4.80 [F] P2/c # 13 centro 1 292 0.079 4950 0.0 / 3.4 4.89 [G] P2/c # 13 centro 4 292 0.079 4950 0.0 / 3.4 4.89 [H] P2/n # 13 centro 1 292 0.079 4950 0.0 / 3.4 4.89 [I] Pc # 7 non-cen 1 226 0.079 4950 0.0 / 3.4 16.32 [J] Pc # 7 non-cen 4 226 0.079 4950 0.0 / 3.4 16.32 [K] Pn # 7 non-cen 1 226 0.079 4950 0.0 / 3.4 16.32 [L] P2(1)/c # 14 centro 1 19410 0.079 4950 0.0 / 3.4 4.55 [M] P2(1)/c # 14 centro 4 19410 0.079 4950 0.0 / 3.4 4.55 [N] P2(1)/n # 14 centro 1 19410 0.079 4950 0.0 / 3.4 4.55 Option [M] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C7H10N2O5 Formula weight = 202.17 Tentative Z (number of formula units/cell) = 12.0 giving rho = 1.456, non-H atomic volume = 16.5 and following cell contents and analysis: C 84.00 41.58 % H 120.00 4.99 % N 24.00 13.86 % O 60.00 39.57 % F(000) = 1272.0 Mo-K(alpha) radiation Mu (mm-1) = 0.13 ------------------------------------------------------------------------------- File 07skc0026p21c.ins set up as follows: TITL 07skc0026p21c in P2(1)/c CELL 0.71073 31.3779 12.3307 7.1600 90.000 92.968 90.000 ZERR 12.00 0.0013 0.0006 0.0003 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 84 120 24 60 TEMP 0.02 TREF HKLF 4 END 21783 Reflections written to new reflection file 07skc0026p21c.hkl ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 07skc0026.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 345 355 97.2 6.37 72.4 17.09 0.0376 0.0390 2.10 - 1.65 365 366 99.7 4.55 19.7 11.84 0.0576 0.0432 1.65 - 1.40 423 426 99.3 3.98 17.1 10.21 0.0703 0.0556 1.40 - 1.25 449 452 99.3 3.87 7.9 8.11 0.0942 0.0727 1.25 - 1.15 450 456 98.7 3.41 6.5 6.68 0.1241 0.0957 1.15 - 1.05 600 605 99.2 3.21 7.6 5.96 0.1331 0.1041 1.05 - 1.00 406 418 97.1 3.07 6.2 5.12 0.1465 0.1220 1.00 - 0.95 482 491 98.2 2.98 4.4 4.03 0.2171 0.1726 0.95 - 0.90 611 617 99.0 2.88 3.0 2.97 0.2921 0.2506 0.90 - 0.85 794 800 99.3 2.73 2.3 2.38 0.3760 0.3406 0.85 - 0.80 921 942 97.8 2.56 2.0 1.98 0.4747 0.4370 0.80 - 0.77 743 825 90.1 2.18 1.8 1.52 0.5978 0.5646 ------------------------------------------------------------------------------ 0.90 - 0.77 2458 2567 95.8 2.49 2.0 1.97 0.4617 0.4348 Inf - 0.77 6589 6753 97.6 3.23 9.4 5.38 0.0914 0.0967 Merged [A], lowest resolution = 6.89 Angstroms, 173 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 07skc0026.hkl -------------------------------------------------------------------------------