++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04src1115 started at 14:37:52 on 02-DEC-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 15.431 11.575 20.502 89.92 107.67 90.01 38787 Reflections read from file 04src1115.hkl; mean (I/sigma) = 4.75 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 19314 19397 19403 19385 29057 25864 25815 38787 N (int>3sigma) = 0 11141 11160 10803 11201 16552 14736 14762 22237 Mean intensity = 0.0 164.9 162.1 153.5 164.6 160.2 161.7 156.9 158.3 Mean int/sigma = 0.0 4.9 4.8 4.7 4.9 4.8 4.8 4.8 4.8 Lattice type: P chosen Volume: 3489.21 ------------------------------------------------------------------------------- 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: 11.575 15.431 20.502 72.33 89.92 89.99 Niggli form: a.a = 133.99 b.b = 238.11 c.c = 420.32 b.c = 96.02 a.c = 0.34 a.b = 0.02 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.085 deg. MONOCLINIC P-lattice R(int) = 0.107 [ 30456] Cell: 15.431 11.575 20.502 89.92 107.67 90.01 Volume: 3489.21 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. TRICLINIC P-lattice R(int) = 0.080 [ 23889] Cell: 11.575 15.431 20.502 72.33 89.92 89.99 Volume: 3489.21 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 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 19314 19397 19403 19385 29057 25864 25815 38787 N (int>3sigma) = 0 11141 11160 10803 11201 16552 14736 14762 22237 Mean intensity = 0.0 164.9 162.1 153.5 164.6 160.2 161.7 156.9 158.3 Mean int/sigma = 0.0 4.9 4.8 4.7 4.9 4.8 4.8 4.8 4.8 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.909 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 20 1251 1225 1230 N I>3s 5 48 471 479 12.1 7.5 241.5 240.9 1.9 0.8 3.7 3.7 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2/c # 13 centro 4 292 0.107 30456 0.8 / 1.9 10.00 [B] Pc # 7 non-cen 4 226 0.107 30456 0.8 / 1.9 12.72 [C] P2(1)/c # 14 centro 4 19410 0.107 30456 1.9 / 3.7 4.79 Option [C] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C72H66N36O32Cl8Zn4 Formula weight = 2492.69 Tentative Z (number of formula units/cell) = 1.0 giving rho = 1.186, non-H atomic volume = 23.0 and following cell contents and analysis: C 72.00 34.69 % H 66.00 2.67 % N 36.00 20.23 % O 32.00 20.54 % Cl 8.00 11.38 % Zn 4.00 10.49 % F(000) = 1262.0 Mo-K(alpha) radiation Mu (mm-1) = 0.90 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL s93 in P2(1)/c CELL 0.71073 20.5017 11.5753 15.4309 90.000 107.669 90.000 ZERR 1.00 0.0043 0.0020 0.0030 0.000 0.021 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O CL ZN UNIT 72 66 36 32 8 4 TEMP 0.03 TREF HKLF 4 END 38787 Reflections written to new reflection file s93.hkl -------------------------------------------------------------------------------