++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008sjc0003 started at 18:37:41 on 18-Mar-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 12.501 12.501 6.913 90.00 90.00 90.00 9789 Reflections read from file 2008sjc0003.hkl; mean (I/sigma) = 11.38 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4885 4856 4871 0 7306 6542 6509 9789 N (int>3sigma) = 0 4415 4376 4703 0 6747 6074 6029 9054 Mean intensity = 0.0 61.2 61.5 72.0 0.0 64.9 76.6 76.7 75.4 Mean int/sigma = 0.0 10.9 10.9 12.0 0.0 11.3 11.4 11.4 11.4 Lattice type: I chosen Volume: 1080.36 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 -1.0000 0.5000 -0.5000 -0.5000 -0.5000 -0.5000 -0.5000 Unitcell: 6.913 9.491 9.491 82.38 68.64 68.64 Niggli form: a.a = 47.79 b.b = 90.08 c.c = 90.08 b.c = 11.95 a.c = 23.90 a.b = 23.90 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TETRAGONAL I-lattice R(sym) = 0.021 [ 1791] Cell: 12.501 12.501 6.913 90.00 90.00 90.00 Volume: 1080.36 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 4885 4856 4871 0 7306 6542 6509 9789 N (int>3sigma) = 0 4415 4376 4703 0 6747 6074 6029 9054 Mean intensity = 0.0 61.2 61.5 72.0 0.0 64.9 76.6 76.7 75.4 Mean int/sigma = 0.0 10.9 10.9 12.0 0.0 11.3 11.4 11.4 11.4 Crystal system T and Lattice type I selected Mean |E*E-1| = 0.584 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: 41/43 a-- -c- --d N 7 454 449 330 N I>3s 7 342 441 275 122.8 36.0 109.9 72.7 14.4 9.2 13.4 11.0 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] I-4 # 82 non-cen 1 99 0.021 1791 0.0 / 9.2 4.40 [B] I4/m # 87 centro 1 46 0.021 1791 0.0 / 9.2 17.95 [C] I4 # 79 chiral 1 19 0.021 1791 0.0 / 9.2 8.40 [D] I-42m #121 non-cen 1 23 0.316 2075 0.0 / 9.2 67.86 [E] I4/mmm #139 centro 1 20 0.316 2075 0.0 / 9.2 80.88 [F] I-4m2 #119 non-cen 1 3 0.316 2075 0.0 / 9.2 88.69 [G] I422 # 97 chiral 1 2 0.316 2075 0.0 / 9.2 97.03 [H] I4mm #107 non-cen 1 2 0.316 2075 0.0 / 9.2 97.03 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008sjc0003.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.15 35 36 97.2 16.25 261.7 72.57 0.0334 0.0161 2.15 - 1.65 40 40 100.0 18.38 180.9 79.65 0.0392 0.0126 1.65 - 1.40 42 42 100.0 19.24 129.3 73.04 0.0371 0.0123 1.40 - 1.25 48 48 100.0 18.90 107.9 65.01 0.0440 0.0142 1.25 - 1.15 43 43 100.0 19.28 68.8 54.23 0.0530 0.0162 1.15 - 1.05 60 60 100.0 18.98 51.0 46.77 0.0551 0.0181 1.05 - 1.00 48 48 100.0 19.15 42.9 43.44 0.0648 0.0207 1.00 - 0.95 47 47 100.0 15.36 41.9 37.90 0.0588 0.0242 0.95 - 0.90 63 63 100.0 14.79 28.3 32.00 0.0737 0.0282 0.90 - 0.85 77 77 100.0 10.92 24.4 23.60 0.0810 0.0398 0.85 - 0.80 92 92 100.0 8.32 14.9 16.24 0.0947 0.0530 0.80 - 0.77 80 80 100.0 7.59 13.9 13.39 0.1042 0.0646 ------------------------------------------------------------------------------ 0.90 - 0.77 249 249 100.0 8.89 17.5 17.60 0.0900 0.0503 Inf - 0.77 675 676 99.9 14.48 64.0 40.47 0.0469 0.0195 Merged [A], lowest resolution = 6.25 Angstroms, 459 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008sjc0003.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: CC14H18Cu3N8 Formula weight = 500.99 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.540, non-H atomic volume = 20.8 and following cell contents and analysis: C 30.00 35.96 % H 36.00 3.62 % N 16.00 22.37 % Cu 6.00 38.05 % F(000) = 502.0 Mo-K(alpha) radiation Mu (mm-1) = 2.94 ------------------------------------------------------------------------------- File 2008sjc0003.ins set up as follows: TITL 2008sjc0003 in I-4 CELL 0.71073 12.5009 12.5009 6.9133 90.000 90.000 90.000 ZERR 2.00 0.0001 0.0001 0.0001 0.000 0.000 0.000 LATT -2 SYMM -X, -Y, Z SYMM Y, -X, -Z SYMM -Y, X, -Z SFAC C H N CU UNIT 30 36 16 6 TEMP 0.12 TREF HKLF 4 END -------------------------------------------------------------------------------