++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 93SRC031 started at 16:33:07 on 25-Nov-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.532 13.132 26.226 90.00 90.00 96.29 8293 Reflections read from file 93SRC031.hkl; mean (I/sigma) = 6.72 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4145 4118 4147 4109 6205 5517 5529 8293 N (int>3sigma) = 0 3495 3438 3485 3432 5209 4633 4630 6946 Mean intensity = 0.0 953.7 944.3 943.4 944.8 947.1 937.4 936.8 936.2 Mean int/sigma = 0.0 6.7 6.7 6.7 6.7 6.7 6.8 6.8 6.7 Lattice type: P chosen Volume: 2920.70 ------------------------------------------------------------------------------- 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: 8.532 13.132 26.226 90.00 90.00 96.29 Niggli form: a.a = 72.80 b.b = 172.45 c.c = 687.80 b.c = 0.00 a.c = 0.00 a.b = -12.29 ------------------------------------------------------------------------------- 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) = 0.024 [ 3144] Cell: 8.532 26.226 13.132 90.00 96.29 90.00 Volume: 2920.70 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4145 4147 4118 4109 6205 5517 5524 8293 N (int>3sigma) = 0 3495 3485 3438 3432 5209 4633 4627 6946 Mean intensity = 0.0 953.7 943.4 944.3 944.8 947.1 937.4 934.4 936.2 Mean int/sigma = 0.0 6.7 6.7 6.7 6.7 6.7 6.8 6.6 6.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.566 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 7 89 62 89 N I>3s 0 56 4 58 194.01142.1 139.81136.7 2.0 7.3 1.5 7.3 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 # 3 chiral 1 29 0.024 3144 0.0 / 1.5 12.79 [B] P2/m # 10 centro 1 21 0.024 3144 0.0 / 1.5 27.28 [C] Pm # 6 non-cen 1 1 0.024 3144 0.0 / 1.5 59.45 [D] P2(1)/c # 14 centro 1 19410 0.024 3144 2.0 / 6.7 18.05 Option [D] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 93SRC031.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.45 215 230 93.5 2.29 1500.8 18.16 0.0283 0.0519 2.45 - 1.90 241 248 97.2 2.17 1367.1 14.35 0.0260 0.0630 1.90 - 1.65 224 231 97.0 2.13 1071.3 11.60 0.0260 0.0777 1.65 - 1.50 242 244 99.2 2.16 1031.5 11.11 0.0287 0.0813 1.50 - 1.40 214 219 97.7 2.16 966.7 10.52 0.0309 0.0874 1.40 - 1.30 282 289 97.6 2.10 980.2 10.09 0.0276 0.0903 1.30 - 1.20 363 375 96.8 2.07 890.8 9.29 0.0292 0.0991 1.20 - 1.15 234 249 94.0 1.92 884.4 8.63 0.0303 0.1075 1.15 - 1.10 272 293 92.8 1.90 786.3 7.98 0.0290 0.1169 1.10 - 1.05 323 358 90.2 1.68 692.7 6.91 0.0287 0.1378 1.05 - 1.00 383 428 89.5 1.73 695.8 6.95 0.0290 0.1378 1.00 - 0.95 443 501 88.4 1.64 663.1 6.35 0.0339 0.1499 0.95 - 0.90 484 670 72.2 1.21 674.6 7.40 0.0332 0.1598 0.90 - 0.85 257 785 32.7 0.43 660.6 5.22 0.0263 0.1827 0.85 - 0.85 4 50 8.0 0.08 807.6 5.51 0.1770 ------------------------------------------------------------------------------ 0.95 - 0.85 745 1505 49.5 0.77 670.5 6.64 0.0319 0.1677 Inf - 0.85 4181 5170 80.9 1.60 873.6 9.08 0.0290 0.1079 Merged [A], lowest resolution = 11.69 Angstroms, 28 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 93SRC031.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C26 H24 N1 O3 I2 Sb W Formula weight = 957.86 Tentative Z (number of formula units/cell) = 4.0 giving rho = 2.178, non-H atomic volume = 21.5 and following cell contents and analysis: C 104.00 32.60 % H 96.00 2.53 % N 4.00 1.46 % O 12.00 5.01 % Sb 4.00 12.71 % I 8.00 26.50 % W 4.00 19.19 % F(000) = 1768.0 Mo-K(alpha) radiation Mu (mm-1) = 7.00 ------------------------------------------------------------------------------- File Solution.ins set up as follows: TITL Solution in P2(1)/c CELL 0.71073 8.5320 26.2260 13.1320 90.000 96.295 90.000 ZERR 4.00 0.0017 0.0052 0.0026 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O SB I W UNIT 104 96 4 12 4 8 4 TREF HKLF 4 END 8293 Reflections written to new reflection file Solution.hkl -------------------------------------------------------------------------------