++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + s92 started at 15:20:46 on 23-Oct-2002 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 17.978 22.113 18.998 90.00 91.57 90.00 46693 Reflections read from file s92.hkl; mean (I/sigma) = 4.26 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 23383 23329 23328 23400 35020 31110 31081 46693 N (int>3sigma) = 0 8645 8223 8430 8698 12649 11443 11450 17283 Mean intensity = 0.0 21.6 14.9 20.4 21.2 19.0 20.1 21.5 21.1 Mean int/sigma = 0.0 4.5 4.2 4.3 4.5 4.3 4.4 4.4 4.4 Lattice type: P chosen Volume: 7549.81 ------------------------------------------------------------------------------- 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: 17.978 18.998 22.113 90.00 90.00 91.57 Niggli form: a.a = 323.22 b.b = 360.92 c.c = 488.98 b.c = 0.00 a.c = 0.00 a.b = -9.36 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.079 [ 8442] Cell: 17.978 22.113 18.998 90.00 91.57 90.00 Volume: 7549.81 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 23383 23329 23328 23400 35020 31110 31081 46693 N (int>3sigma) = 0 8645 8223 8430 8698 12649 11443 11450 17283 Mean intensity = 0.0 21.6 14.9 20.4 21.2 19.0 20.1 21.5 21.1 Mean int/sigma = 0.0 4.5 4.2 4.3 4.5 4.3 4.4 4.4 4.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.879 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 23 570 606 618 N I>3s 0 10 233 237 0.4 0.7 22.8 22.3 0.3 0.6 5.4 5.3 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)/c # 14 centro 4 19410 0.079 8442 0.6 / 4.4 3.37 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 - 2.95 2432 627 387.9 3.88 187.7 14.69 0.0576 2.95 - 2.35 2605 600 434.2 4.34 44.1 10.78 0.0638 2.35 - 2.05 2682 618 434.0 4.34 41.2 10.45 0.0740 2.05 - 1.85 2914 669 435.6 4.36 31.9 8.85 0.0808 1.85 - 1.70 2672 709 376.9 3.77 17.1 6.41 0.1142 1.70 - 1.55 3345 1038 322.3 3.22 11.7 5.14 0.1498 1.55 - 1.45 2778 953 291.5 2.92 7.9 3.98 0.2154 1.45 - 1.35 3161 1233 256.4 2.56 5.4 2.86 0.3243 1.35 - 1.25 3766 1668 225.8 2.26 4.5 2.27 0.4109 1.25 - 1.15 3773 2304 163.8 1.64 4.8 2.04 0.4511 1.15 - 1.05 4039 3249 124.3 1.24 3.7 1.41 0.6895 1.05 - 1.00 2405 2138 112.5 1.12 2.2 0.77 1.3114 1.00 - 0.95 2800 2637 106.2 1.06 1.5 0.46 2.1496 0.95 - 0.90 3167 3272 96.8 0.97 1.1 0.29 3.3504 0.90 - 0.85 3550 4063 87.4 0.87 0.8 0.20 4.8643 0.85 - 0.84 604 1024 59.0 0.59 0.6 0.14 7.0675 ------------------------------------------------------------------------------ 0.95 - 0.84 7321 8359 87.6 0.88 0.9 0.24 4.2008 Inf - 0.84 46693 26802 174.2 1.74 20.7 4.26 0.1461 Merged [N], lowest resolution = 6.97 Angstroms, 0 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 s92.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C36H48N7O10F1 Formula weight = 757.81 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.333, non-H atomic volume = 17.5 and following cell contents and analysis: C 288.00 57.05 % H 384.00 6.38 % N 56.00 12.94 % O 80.00 21.11 % F 8.00 2.51 % F(000) = 3216.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL s93 in P2(1)/c CELL 0.71073 18.9979 22.1130 17.9782 90.000 91.571 90.000 ZERR 8.00 0.0013 0.0011 0.0010 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O F UNIT 288 384 56 80 8 TREF HKLF 4 END -------------------------------------------------------------------------------