++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2005src1384 started at 17:11:39 on 10-NOV-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 12.319 10.927 15.390 90.00 94.96 90.00 24584 Reflections read from file 2005src1384.hkl; mean (I/sigma) = 7.17 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 12289 12279 12306 12331 18437 16375 16373 24584 N (int>3sigma) = 0 9100 9057 9205 9126 13681 12165 12026 18101 Mean intensity = 0.0 335.7 334.9 312.0 333.8 327.5 337.0 334.2 332.7 Mean int/sigma = 0.0 7.2 7.2 7.2 7.2 7.2 7.2 7.2 7.2 Lattice type: P chosen Volume: 2063.93 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 10.927 12.319 15.390 94.96 90.00 90.00 Niggli form: a.a = 119.40 b.b = 151.77 c.c = 236.85 b.c = -16.39 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.065 [ 19603] Cell: 12.319 10.927 15.390 90.00 94.96 90.00 Volume: 2063.93 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 12289 12279 12306 12331 18437 16375 16373 24584 N (int>3sigma) = 0 9100 9057 9205 9126 13681 12165 12026 18101 Mean intensity = 0.0 335.7 334.9 312.0 333.8 327.5 337.0 334.2 332.7 Mean int/sigma = 0.0 7.2 7.2 7.2 7.2 7.2 7.2 7.2 7.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.753 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 15 737 735 734 N I>3s 0 503 513 514 6.6 405.0 436.5 418.1 0.8 6.6 6.8 6.7 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1) # 4 chiral 1 3543 0.065 19603 0.8 / 6.6 1.60 [B] P2(1)/m # 11 centro 1 402 0.065 19603 0.8 / 6.6 6.44 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C44H36Br4NiP2Fe2 Formula weight = 1116.72 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.797, non-H atomic volume = 19.5 and following cell contents and analysis: C 88.00 47.32 % H 72.00 3.25 % P 4.00 5.55 % Fe 4.00 10.00 % Ni 2.00 5.26 % Br 8.00 28.62 % F(000) = 1100.0 Mo-K(alpha) radiation Mu (mm-1) = 5.13 ------------------------------------------------------------------------------- File 2005src1384.ins set up as follows: TITL 2005src1384 in P2(1) CELL 0.71073 12.3194 10.9269 15.3899 90.000 94.958 90.000 ZERR 2.00 0.0004 0.0003 0.0005 0.000 0.002 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H P FE NI BR UNIT 88 72 4 4 2 8 TEMP 0.01 TREF HKLF 4 END -------------------------------------------------------------------------------