++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + s92 started at 09:19:36 on 29-May-2003 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.243 17.018 19.438 74.39 83.14 82.03 45141 Reflections read from file s92.hkl; mean (I/sigma) = 7.44 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 22562 22645 22601 22551 33904 30092 30119 45141 N (int>3sigma) = 0 12253 12471 12366 10098 18545 16400 16559 24778 Mean intensity = 0.0 50.9 66.2 65.4 33.9 60.9 66.1 65.8 65.3 Mean int/sigma = 0.0 7.3 7.5 7.5 5.7 7.4 7.5 7.5 7.5 Lattice type: P chosen Volume: 2591.17 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 8.243 17.018 19.438 74.39 83.14 82.03 Niggli form: a.a = 67.95 b.b = 289.61 c.c = 377.85 b.c = 89.04 a.c = 19.13 a.b = 19.45 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(sym) = 0.000 [ 0] Cell: 8.243 17.018 19.438 74.39 83.14 82.03 Volume: 2591.17 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 22562 22645 22601 22551 33904 30092 30119 45141 N (int>3sigma) = 0 12253 12471 12366 10098 18545 16400 16559 24778 Mean intensity = 0.0 50.9 66.2 65.4 33.9 60.9 66.1 65.8 65.3 Mean int/sigma = 0.0 7.3 7.5 7.5 5.7 7.4 7.5 7.5 7.5 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.966 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic 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] P-1 # 2 centro 1 8646 0.000 0 0.0 / 7.5 1.34 [B] P1 # 1 chiral 1 700 0.000 0 0.0 / 7.5 6.76 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 s92.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.05 608 623 97.6 8.24 209.9 47.90 0.0598 0.0145 2.05 - 1.60 704 704 100.0 6.04 126.0 32.88 0.1105 0.0230 1.60 - 1.40 639 639 100.0 5.52 80.3 26.02 0.0741 0.0269 1.40 - 1.25 826 826 100.0 5.11 59.0 19.69 0.1090 0.0361 1.25 - 1.15 769 769 100.0 4.44 47.8 15.69 0.1124 0.0475 1.15 - 1.05 1120 1120 100.0 4.04 34.6 11.13 0.1349 0.0683 1.05 - 1.00 734 736 99.7 3.72 26.8 8.34 0.1459 0.0965 1.00 - 0.95 900 906 99.3 3.37 26.1 7.45 0.1571 0.1125 0.95 - 0.90 1101 1112 99.0 3.06 20.2 5.36 0.2058 0.1648 0.90 - 0.85 1356 1388 97.7 2.80 16.2 3.93 0.2598 0.2372 0.85 - 0.80 1714 1796 95.4 2.45 11.6 2.50 0.3680 0.3929 0.80 - 0.77 1190 1335 89.1 1.93 8.4 1.50 0.6058 0.6760 ------------------------------------------------------------------------------ 0.90 - 0.77 4260 4519 94.3 2.40 12.2 2.67 0.3535 0.3815 Inf - 0.77 11661 11954 97.5 3.78 43.7 11.99 0.1033 0.0775 Merged [A], lowest resolution = 6.97 Angstroms, 5247 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 s92.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C21H21N4O2S2Ni2Cl1 Formula weight = 578.41 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.483, non-H atomic volume = 20.2 and following cell contents and analysis: C 84.00 43.60 % H 84.00 3.66 % N 16.00 9.69 % O 8.00 5.53 % S 8.00 11.09 % Cl 4.00 6.13 % Ni 8.00 20.30 % F(000) = 1184.0 Mo-K(alpha) radiation Mu (mm-1) = 1.74 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P-1 CELL 0.71073 8.2431 17.0179 19.4384 74.385 83.143 82.030 ZERR 4.00 0.0005 0.0011 0.0012 0.002 0.003 0.004 LATT 1 SFAC C H N O S CL NI UNIT 84 84 16 8 8 4 8 TREF HKLF 4 END -------------------------------------------------------------------------------