++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04src0422 started at 16:31:14 on 27-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 23.507 18.121 21.007 90.03 118.69 89.96 33556 Reflections read from file 04src0422.hkl; mean (I/sigma) = 5.95 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 16781 16781 0 16763 16781 22382 22368 33556 N (int>3sigma) = 0 9364 9364 0 9391 9364 12444 12505 18718 Mean intensity = 0.0 212.5 212.5 0.0 212.4 212.5 204.2 209.5 207.1 Mean int/sigma = 0.0 6.0 6.0 0.0 6.0 6.0 6.0 6.0 6.0 Lattice type: C chosen Volume: 7849.88 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 -1.0000 Unitcell: 14.835 14.846 20.602 109.44 101.78 104.74 Niggli form: a.a = 220.08 b.b = 220.40 c.c = 424.44 b.c = -101.78 a.c = -62.37 a.b = -56.05 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.044 deg. MONOCLINIC C-lattice R(int) = 0.064 [ 24329] Cell: 23.507 18.121 21.007 90.03 118.69 89.96 Volume: 7849.88 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.044 deg. MONOCLINIC I-lattice R(int) = 0.064 [ 24329] Cell: 21.007 18.121 22.799 89.98 115.24 89.97 Volume: 7849.88 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 16781 16781 0 16763 16781 22382 22368 33556 N (int>3sigma) = 0 9364 9364 0 9391 9364 12444 12505 18718 Mean intensity = 0.0 212.5 212.5 0.0 212.4 212.5 204.2 209.5 207.1 Mean int/sigma = 0.0 6.0 6.0 0.0 6.0 6.0 6.0 6.0 6.0 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.941 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 720 N I>3s 149 19.3 2.0 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2 # 5 chiral 1 552 0.064 24329 0.0 / 2.0 9.51 [B] C2/m # 12 centro 1 310 0.064 24329 0.0 / 2.0 5.50 [C] Cm # 8 non-cen 1 32 0.064 24329 0.0 / 2.0 12.36 [D] C2/c # 15 centro 1 3696 0.064 24329 2.0 / 6.0 2.55 [E] Cc # 9 non-cen 1 566 0.064 24329 2.0 / 6.0 6.85 Option [D] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C87H75N39O24Cl6Zn3 Formula weight = 2459.67 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.041, non-H atomic volume = 24.7 and following cell contents and analysis: C 174.00 42.48 % H 150.00 3.07 % N 78.00 22.21 % O 48.00 15.61 % Cl 12.00 8.65 % Zn 6.00 7.97 % F(000) = 2508.0 Mo-K(alpha) radiation Mu (mm-1) = 0.62 ------------------------------------------------------------------------------- File 04src0422.ins set up as follows: TITL 04src0422 in C2/c CELL 0.71073 23.5068 18.1213 21.0066 90.000 118.687 90.000 ZERR 2.00 0.0047 0.0036 0.0042 0.000 0.030 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O CL ZN UNIT 174 150 78 48 12 6 TEMP 0.07 TREF HKLF 4 END -------------------------------------------------------------------------------