+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2007/1 for Windows + + Copyright(C) 2007 Bruker-AXS All Rights Reserved + + 2007src1588 started at 17:59:59 on 20-Nov-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.402 15.816 26.803 90.02 89.98 90.01 58093 Reflections read from file 2007src1588.hkl; mean (I/sigma) = 5.23 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 29052 28995 29755 29035 43901 38775 38800 58093 N (int>3sigma) = 0 11739 11733 58 11586 11765 15737 15761 23569 Mean intensity = 0.0 19.9 19.9 0.3 18.3 13.2 20.0 20.1 20.0 Mean int/sigma = 0.0 5.5 5.5 0.6 5.3 3.8 5.5 5.5 5.5 Lattice type: C chosen Volume: 3137.73 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 Unitcell: 7.402 8.730 26.803 90.01 90.02 115.07 Niggli form: a.a = 54.79 b.b = 76.22 c.c = 718.42 b.c = -0.05 a.c = -0.07 a.b = -27.39 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.032 deg. ORTHORHOMBIC C-lattice R(sym) = 0.025 [ 5137] Cell: 7.402 15.815 26.803 90.02 89.98 90.01 Volume: 3137.73 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 29052 28995 29755 29035 43901 38775 38800 58093 N (int>3sigma) = 0 11739 11733 58 11586 11765 15737 15761 23569 Mean intensity = 0.0 19.9 19.9 0.3 18.3 13.2 20.0 20.1 20.0 Mean int/sigma = 0.0 5.5 5.5 0.6 5.3 3.8 5.5 5.5 5.5 Crystal system O and Lattice type C selected Mean |E*E-1| = 0.724 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: c-- n-- -c- -n- --a --b --21 N 1350 1350 564 564 255 255 117 N I>3s 1003 1003 340 340 192 192 0 54.7 54.7 25.5 25.5 52.1 52.1 0.2 10.5 10.5 8.1 8.1 9.9 9.9 0.5 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] C222(1) # 20 chiral 1 155 0.025 5137 0.5 / 5.5 2.63 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007src1588.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.18 106 113 93.8 18.58 183.3 81.23 0.0364 0.0143 2.18 - 1.71 111 111 100.0 22.74 99.0 81.74 0.0390 0.0123 1.71 - 1.47 109 111 98.2 20.60 64.5 69.87 0.0422 0.0171 1.47 - 1.33 115 115 100.0 17.63 31.5 51.79 0.0504 0.0162 1.33 - 1.23 106 106 100.0 16.96 41.5 52.91 0.0529 0.0175 1.23 - 1.15 118 120 98.3 16.29 33.6 50.20 0.0516 0.0172 1.15 - 1.08 128 130 98.5 13.69 35.3 43.47 0.0536 0.0210 1.08 - 1.03 121 121 100.0 12.67 22.0 36.10 0.0625 0.0233 1.03 - 0.98 132 132 100.0 12.72 19.0 34.05 0.0724 0.0252 0.98 - 0.94 136 137 99.3 12.03 15.3 27.51 0.0845 0.0299 0.94 - 0.91 125 125 100.0 11.30 9.7 21.93 0.1201 0.0399 0.91 - 0.88 127 127 100.0 11.02 7.4 17.83 0.1421 0.0496 0.88 - 0.86 105 105 100.0 10.70 7.5 15.99 0.1339 0.0500 0.86 - 0.84 107 107 100.0 10.56 7.9 15.80 0.1394 0.0544 0.84 - 0.82 117 117 100.0 10.17 6.0 13.48 0.1611 0.0620 0.82 - 0.80 132 132 100.0 9.79 6.0 13.13 0.1723 0.0660 0.80 - 0.78 157 157 100.0 8.76 6.1 11.89 0.1748 0.0713 0.78 - 0.76 28 66 42.4 1.23 8.5 6.55 0.1729 0.1404 ------------------------------------------------------------------------------ 0.86 - 0.76 595 633 94.0 8.92 6.7 13.43 0.1579 0.0665 Inf - 0.76 2080 2132 97.6 13.29 32.5 35.91 0.0501 0.0206 Merged [A], lowest resolution = 6.81 Angstroms, 1560 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007src1588.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C17H21NO4 Formula weight = 303.35 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.284, non-H atomic volume = 17.8 and following cell contents and analysis: C 136.00 67.31 % H 168.00 6.98 % N 8.00 4.62 % O 32.00 21.10 % F(000) = 1296.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File 2007src1588.ins set up as follows: TITL 2007src1588 in C222(1) CELL 0.71073 7.4019 15.8155 26.8034 90.000 90.000 90.000 ZERR 8.00 0.0002 0.0003 0.0004 0.000 0.000 0.000 LATT -7 SYMM -X, -Y, 0.5+Z SYMM -X, Y, 0.5-Z SYMM X, -Y, -Z SFAC C H N O UNIT 136 168 8 32 TEMP 0.2 TREF HKLF 4 END 58093 Reflections written to new reflection file 2007src1588.hkl -------------------------------------------------------------------------------