++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 10:51:06 on 31-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.945 7.789 12.333 97.75 94.54 106.50 3524 Reflections read from file s92.hkl; mean (I/sigma) = 10.00 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1775 1763 1774 1755 2656 2354 2353 3524 N (int>3sigma) = 0 1352 1360 1326 1323 2019 1762 1766 2657 Mean intensity = 0.0 196.0 203.7 174.9 189.1 191.5 192.5 190.0 188.5 Mean int/sigma = 0.0 10.3 10.4 10.0 10.1 10.2 9.9 10.0 10.1 Lattice type: P chosen Volume: 538.39 ------------------------------------------------------------------------------- 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: 5.945 7.789 12.333 97.75 94.54 106.50 Niggli form: a.a = 35.34 b.b = 60.67 c.c = 152.12 b.c = -12.95 a.c = -5.80 a.b = -13.15 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.021 [ 1360] Cell: 5.945 7.789 12.333 97.75 94.54 106.50 Volume: 538.39 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1775 1763 1774 1755 2656 2354 2353 3524 N (int>3sigma) = 0 1352 1360 1326 1323 2019 1762 1766 2657 Mean intensity = 0.0 196.0 203.7 174.9 189.1 191.5 192.5 190.0 188.5 Mean int/sigma = 0.0 10.3 10.4 10.0 10.1 10.2 9.9 10.0 10.1 Crystal system A and Lattice type P selected Mean |E*E-1| = 1.017 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.021 1360 0.0 / 10.1 1.24 [B] P1 # 1 chiral 1 700 0.021 1360 0.0 / 10.1 9.02 Option [A] chosen ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1775 1763 1774 1755 2656 2354 2353 3524 N (int>3sigma) = 0 1352 1360 1326 1323 2019 1762 1766 2657 Mean intensity = 0.0 196.0 203.7 174.9 189.1 191.5 192.5 190.0 188.5 Mean int/sigma = 0.0 10.3 10.4 10.0 10.1 10.2 9.9 10.0 10.1 Crystal system A and Lattice type P selected Mean |E*E-1| = 1.017 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.021 1360 0.0 / 10.1 1.24 [B] P1 # 1 chiral 1 700 0.021 1360 0.0 / 10.1 9.02 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C13 H12 N2 O1 Formula weight = 212.25 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.309, non-H atomic volume = 16.8 and following cell contents and analysis: C 26.00 73.56 % H 24.00 5.70 % N 4.00 13.20 % O 2.00 7.54 % F(000) = 224.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P-1 CELL 0.71073 5.9447 7.7890 12.3335 97.747 94.537 106.505 ZERR 2.00 0.0012 0.0016 0.0025 0.030 0.030 0.030 LATT 1 SFAC C H N O UNIT 26 24 4 2 TREF HKLF 4 END -------------------------------------------------------------------------------