++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2007src0178 started at 12:46:58 on 08-Mar-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.149 18.610 8.865 90.00 113.22 90.00 16491 Reflections read from file 2007src0178.hkl; mean (I/sigma) = 8.35 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8261 8224 8257 8236 12371 11002 10999 16491 N (int>3sigma) = 0 6661 6542 6707 6525 9955 8912 8972 13345 Mean intensity = 0.0 471.7 474.2 453.5 462.5 466.4 468.3 471.0 469.7 Mean int/sigma = 0.0 8.4 8.3 8.4 8.3 8.4 8.4 8.5 8.4 Lattice type: P chosen Volume: 1083.91 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.149 8.865 18.610 90.00 90.00 113.22 Niggli form: a.a = 51.11 b.b = 78.59 c.c = 346.33 b.c = 0.00 a.c = 0.00 a.b = -24.99 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.560 deg. ORTHORHOMBIC C-lattice R(sym) = 0.552 [ 3483] Cell: 7.149 16.295 18.610 90.00 90.00 89.44 Volume: 2167.82 Matrix: 1.0000 0.0000 0.0000 1.0000 0.0000 2.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.028 [ 2356] Cell: 7.149 18.610 8.865 90.00 113.22 90.00 Volume: 1083.91 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.560 deg. MONOCLINIC C-lattice R(sym) = 0.607 [ 2232] Cell: 16.295 7.149 18.610 90.00 90.00 90.56 Volume: 2167.82 Matrix:-1.0000 0.0000 -2.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.560 deg. MONOCLINIC C-lattice R(sym) = 0.569 [ 2333] Cell: 7.149 16.295 18.610 90.00 90.00 89.44 Volume: 2167.82 Matrix:-1.0000 0.0000 0.0000 -1.0000 0.0000 -2.0000 0.0000 -1.0000 0.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8261 8224 8257 8236 12371 11002 10999 16491 N (int>3sigma) = 0 6661 6542 6707 6525 9955 8912 8972 13345 Mean intensity = 0.0 471.7 474.2 453.5 462.5 466.4 468.3 471.0 469.7 Mean int/sigma = 0.0 8.4 8.3 8.4 8.3 8.4 8.4 8.5 8.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.935 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 39 211 211 218 N I>3s 4 91 93 2 3.8 315.7 315.6 3.4 0.9 4.5 4.4 0.7 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] P2(1)/n # 14 centro 1 19410 0.028 2356 0.9 / 4.4 2.79 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007src0178.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 131 140 93.6 7.19 1438.6 33.07 0.0453 0.0286 2.10 - 1.65 135 135 100.0 8.41 997.7 35.29 0.0429 0.0271 1.65 - 1.40 172 172 100.0 8.61 827.2 34.34 0.0397 0.0275 1.40 - 1.25 171 171 100.0 8.55 564.0 31.74 0.0494 0.0293 1.25 - 1.15 169 169 100.0 8.63 513.9 28.18 0.0493 0.0287 1.15 - 1.05 246 246 100.0 8.45 362.1 23.34 0.0521 0.0336 1.05 - 1.00 151 151 100.0 8.25 362.5 22.63 0.0587 0.0334 1.00 - 0.95 205 205 100.0 6.94 223.6 17.51 0.0690 0.0423 0.95 - 0.90 223 223 100.0 6.39 212.4 16.39 0.0710 0.0471 0.90 - 0.85 316 316 100.0 4.79 184.2 12.10 0.0761 0.0616 0.85 - 0.80 364 365 99.7 3.72 157.5 10.33 0.0842 0.0721 0.80 - 0.77 288 320 90.0 2.82 110.7 7.61 0.0996 0.0947 ------------------------------------------------------------------------------ 0.90 - 0.77 968 1001 96.7 3.77 152.3 10.10 0.0830 0.0728 Inf - 0.77 2571 2613 98.4 6.31 401.8 19.98 0.0512 0.0368 Merged [A], lowest resolution = 6.57 Angstroms, 677 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007src0178.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C16 H24 Cl1 N2 O3 Si2 Formula weight = 384.00 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.177, non-H atomic volume = 22.6 and following cell contents and analysis: C 32.00 50.04 % H 48.00 6.30 % N 4.00 7.30 % O 6.00 12.50 % Si 4.00 14.63 % Cl 2.00 9.23 % F(000) = 406.0 Mo-K(alpha) radiation Mu (mm-1) = 0.30 ------------------------------------------------------------------------------- File 2007src0178.ins set up as follows: TITL 2007src0178 in P2(1)/n CELL 0.71073 7.1492 18.6099 8.8649 90.000 113.219 90.000 ZERR 2.00 0.0001 0.0006 0.0002 0.000 0.002 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O SI CL UNIT 32 48 4 6 4 2 TEMP 0.06 TREF HKLF 4 END -------------------------------------------------------------------------------