++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 94SRC104 started at 16:13:15 on 03-Nov-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 13.114 13.235 22.903 96.18 96.19 113.35 8790 Reflections read from file 94SRC104.hkl; mean (I/sigma) = 28.62 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4425 4374 4391 4384 6595 5872 5847 8790 N (int>3sigma) = 0 2662 2804 2758 2779 4112 3719 3715 5581 Mean intensity = 0.0 221.2 265.1 259.5 263.8 248.5 264.9 263.3 263.9 Mean int/sigma = 0.0 12.0 37.2 38.1 23.1 29.1 32.4 27.8 28.6 Lattice type: P chosen Volume: 3578.71 ------------------------------------------------------------------------------- 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: 13.114 13.235 22.903 96.18 96.19 113.35 Niggli form: a.a = 171.98 b.b = 175.17 c.c = 524.55 b.c = -32.63 a.c = -32.39 a.b = -68.79 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.580 deg. MONOCLINIC C-lattice R(sym) = 0.414 [ 3191] Cell: 14.476 22.016 22.903 90.03 101.31 89.43 Volume: 7157.41 Matrix: 1.0000 1.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. TRICLINIC P-lattice R(sym) = 0.000 [ 0] Cell: 13.114 13.235 22.903 96.18 96.19 113.35 Volume: 3578.71 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4425 4374 4391 4384 6595 5872 5847 8790 N (int>3sigma) = 0 2662 2804 2758 2779 4112 3719 3715 5581 Mean intensity = 0.0 221.2 265.1 259.5 263.8 248.5 264.9 263.3 263.9 Mean int/sigma = 0.0 12.0 37.2 38.1 23.1 29.1 32.4 27.8 28.6 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.000 [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 / 28.6 94.06 [B] P1 # 1 chiral 1 700 0.000 0 0.0 / 28.6 54.66 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 94SRC104.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.50 437 473 92.4 0.93 611.8 209.79 0.5804 0.0341 2.50 - 1.95 486 545 89.2 0.91 419.3 75.97 0.5972 0.0541 1.95 - 1.70 457 521 87.7 0.89 369.3 24.38 0.4085 0.0689 1.70 - 1.50 570 684 83.3 0.85 319.4 19.60 0.4973 0.0903 1.50 - 1.40 446 515 86.6 0.88 278.9 15.17 0.7847 0.1208 1.40 - 1.30 567 665 85.3 0.86 283.3 15.41 0.4171 0.1157 1.30 - 1.20 775 923 84.0 0.85 249.9 64.83 0.2893 0.1515 1.20 - 1.15 502 610 82.3 0.82 246.5 10.46 0.1685 1.15 - 1.10 554 670 82.7 0.84 229.9 9.51 0.6316 0.1856 1.10 - 1.05 698 874 79.9 0.80 222.3 8.14 0.2673 0.2115 1.05 - 1.00 807 1016 79.4 0.80 211.7 7.16 0.4253 0.2401 1.00 - 0.95 915 1237 74.0 0.75 191.2 5.59 0.5878 0.2851 0.95 - 0.90 974 1556 62.6 0.63 169.1 4.43 0.8878 0.3377 0.90 - 0.25 443 469359 0.1 0.00 150.9 3.98 0.2432 0.3753 0.25 - 0.11 835903565 0.0 0.00 242.3 9.54 0.1867 ------------------------------------------------------------------------------ 0.20 - 0.11 575446276 0.0 0.00 231.4 8.63 0.2093 Inf - 0.11 87146383213 0.1 0.00 264.4 28.76 0.5305 0.1579 Merged [A], lowest resolution = 11.38 Angstroms, 68 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 94SRC104.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C74H81B2Cl6CoN12 Formula weight = 1431.76 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.329, non-H atomic volume = 18.8 and following cell contents and analysis: C 148.00 62.07 % H 162.00 5.70 % B 4.00 1.51 % N 24.00 11.74 % Cl 12.00 14.86 % Co 2.00 4.12 % F(000) = 1496.0 Mo-K(alpha) radiation Mu (mm-1) = 0.52 ------------------------------------------------------------------------------- File 94SRC104.ins set up as follows: TITL 94SRC104 in P-1 CELL 0.71073 13.1140 13.2350 22.9030 96.180 96.190 113.350 ZERR 2.00 0.0026 0.0026 0.0046 0.030 0.030 0.030 LATT 1 SFAC C H B N CL CO UNIT 148 162 4 24 12 2 TREF HKLF 4 END -------------------------------------------------------------------------------