++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2005src1566 started at 09:43:19 on 21-DEC-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 24.596 24.596 48.278 90.00 90.00 120.00 74398 Reflections read from file 2005src1566.hkl; mean (I/sigma) = 5.48 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 37191 37193 37248 37176 55816 0 49634 74398 N (int>3sigma) = 0 18463 18402 18577 18579 27721 0 24979 37138 Mean intensity = 0.0 149.3 148.1 148.0 149.2 148.5 0.0 147.8 147.2 Mean int/sigma = 0.0 5.6 5.5 5.5 5.6 5.5 0.0 5.6 5.6 Lattice type: O chosen Volume: 25292.57 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.3333 0.3333 0.3333 -0.3333 -0.6667 0.3333 0.6667 0.3333 0.3333 Unitcell: 21.462 21.462 21.462 69.92 69.92 69.92 Niggli form: a.a = 460.62 b.b = 460.62 c.c = 460.62 b.c = 158.15 a.c = 158.15 a.b = 158.15 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. RHOMBOHEDRAL O-lattice R(int) = 0.102 [ 61342] Cell: 24.596 24.595 48.278 90.00 90.00 120.00 Volume: 25292.57 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. RHOMBOHEDRAL P-lattice R(int) = 0.102 [ 61342] Cell: 21.462 21.462 21.462 69.92 69.92 69.92 Volume: 8430.86 Matrix: 0.6667 0.3333 0.3333 -0.3333 0.3333 0.3333 -0.3333 -0.6667 0.3333 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 37161 37248 37249 37206 55829 49582 49676 74398 N (int>3sigma) = 0 18401 18577 18518 18464 27748 24746 24817 37138 Mean intensity = 0.0 147.3 148.0 146.9 146.0 147.4 148.3 147.4 147.2 Mean int/sigma = 0.0 5.5 5.5 5.5 5.5 5.5 5.6 5.6 5.6 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.859 [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 0.068 39357 0.0 / 5.6 3.00 [B] P1 # 1 chiral 1 700 0.068 39357 0.0 / 5.6 3.46 Option [B] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C92H100O4B1Cl1F24Fe2Ga2 Formula weight = 2023.12 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.594, non-H atomic volume = 16.7 and following cell contents and analysis: C 368.00 54.61 % H 400.00 4.98 % B 4.00 0.53 % O 16.00 3.16 % F 96.00 22.54 % Cl 4.00 1.75 % Fe 8.00 5.52 % Ga 8.00 6.89 % F(000) = 4144.0 Mo-K(alpha) radiation Mu (mm-1) = 1.11 ------------------------------------------------------------------------------- File p1.ins set up as follows: TITL p1 in P1 CELL 0.71073 21.4621 21.4621 21.4621 69.919 69.919 69.919 ZERR 4.00 0.0030 0.0025 0.0030 0.000 0.000 0.000 LATT -1 SFAC C H B O F CL FE GA UNIT 368 400 4 16 96 4 8 8 TEMP 0.06 TREF HKLF 4 END 74398 Reflections written to new reflection file p1.hkl -------------------------------------------------------------------------------