++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION - Version 2014/2 + + COPYRIGHT(c) 2014 Bruker-AXS All Rights Reserved + + neal054_0m started at 15:01:00 on 27-Oct-2021 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.257 11.763 13.039 90.00 96.66 90.00 18124 Reflections read from file neal054_0m.hkl; mean (I/sigma) = 11.23 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9149 9080 9069 9076 13649 12117 12102 18124 N (int>3sigma) = 0 8736 8628 8568 8591 12966 11513 11449 17212 Mean intensity = 0.0 33.6 35.7 35.4 35.5 34.9 35.8 36.0 35.5 Mean int/sigma = 0.0 11.4 11.3 11.2 11.2 11.3 11.3 11.2 11.2 Lattice type: P chosen Volume: 953.22 ------------------------------------------------------------------------------- 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: 6.257 11.763 13.039 90.00 96.66 90.00 Niggli form: a.a = 39.15 b.b = 138.37 c.c = 170.01 b.c = 0.00 a.c = -9.46 a.b = 0.00 ------------------------------------------------------------------------------- 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) = 0.036 [ 1402] Cell: 6.257 11.763 13.039 90.00 96.66 90.00 Volume: 953.22 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option A selected ------------------------------------------------------------------------------- TOLERANCES CHANGED Maximum deviation (deg.) in higher symmetry cell search = 1.000 Threshold (deg.) for terminating search = 0.050 R(int) maximum for terminating cell search = 0.120 R(int) maximum for space group determination = 0.300 Minimum number of data in group for syst. absence test = 5 Maximum mean I/sigma(I) for systematic absences = 2.623 Minimum I/sigma gap between absences and rest = 2.245 ------------------------------------------------------------------------------- Current dataset is # 1 neal054_0m.hkl ------------------------------------------------------------------------------- Original cell in Angstroms and degrees: 6.257 11.763 13.039 90.00 96.66 90.00 18124 Reflections read from file neal054_0m.hkl; mean (I/sigma) = 11.23 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9149 9080 9069 9076 13649 12117 12102 18124 N (int>3sigma) = 0 8736 8628 8568 8591 12966 11513 11449 17212 Mean intensity = 0.0 33.6 35.7 35.4 35.5 34.9 35.8 36.0 35.5 Mean int/sigma = 0.0 11.4 11.3 11.2 11.2 11.3 11.3 11.2 11.2 Lattice type: C chosen Volume: 953.22 ------------------------------------------------------------------------------- TOLERANCES CHANGED Maximum deviation (deg.) in higher symmetry cell search = 1.000 Threshold (deg.) for terminating search = 0.050 R(int) maximum for terminating cell search = 0.120 R(int) maximum for space group determination = 0.300 Minimum number of data in group for syst. absence test = 5 Maximum mean I/sigma(I) for systematic absences = 2.623 Minimum I/sigma gap between absences and rest = 2.245 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 Unitcell: 6.257 6.662 13.039 86.88 83.34 61.99 Niggli form: a.a = 39.15 b.b = 44.38 c.c = 170.01 b.c = 4.73 a.c = 9.46 a.b = 19.58 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(sym) = 0.036 [ 700] Cell: 6.257 11.763 13.039 90.00 96.66 90.00 Volume: 953.22 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 9149 9080 9069 9076 13649 12117 12102 18124 N (int>3sigma) = 0 8736 8628 8568 8591 12966 11513 11449 17212 Mean intensity = 0.0 33.6 35.7 35.4 35.5 34.9 35.8 36.0 35.5 Mean int/sigma = 0.0 11.4 11.3 11.2 11.2 11.3 11.3 11.2 11.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.652 [expected .968 centrosym and .736 non-centrosym] Chiral flag set Systematic absence exceptions: -21- -a- -c- -n- N 46 540 550 560 N I>3s 9 499 526 521 0.2 52.9 39.4 55.1 1.9 11.1 11.3 11.3 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) # 4 chiral 1 3543 0.036 1402 1.9 / 11.1 1.80 Option [A] chosen ------------------------------------------------------------------------------- TOLERANCES CHANGED Maximum deviation (deg.) in higher symmetry cell search = 1.000 Threshold (deg.) for terminating search = 0.050 R(int) maximum for terminating cell search = 0.120 R(int) maximum for space group determination = 0.300 Minimum number of data in group for syst. absence test = 5 Maximum mean I/sigma(I) for systematic absences = 2.623 Minimum I/sigma gap between absences and rest = 2.245 ------------------------------------------------------------------------------- Current dataset is # 1 neal054_0m.hkl ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 neal054_0m.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge Rsigma Inf - 3.44 48 51 94.1 5.59 189.12 33.27 0.0591 0.0405 3.44 - 2.35 111 112 99.1 8.11 121.97 39.30 0.0641 0.0268 2.35 - 1.86 154 154 100.0 8.40 74.56 37.80 0.0589 0.0245 1.86 - 1.62 157 157 100.0 8.45 63.74 37.47 0.0554 0.0245 1.62 - 1.47 159 159 100.0 8.03 40.56 35.78 0.0493 0.0262 1.47 - 1.37 154 154 100.0 7.93 40.09 35.43 0.0414 0.0267 1.37 - 1.28 162 162 100.0 7.53 30.32 32.88 0.0445 0.0283 1.28 - 1.22 155 155 100.0 7.05 27.40 30.18 0.0494 0.0299 1.22 - 1.17 157 158 99.4 6.63 20.53 27.09 0.0529 0.0320 1.17 - 1.12 171 171 100.0 6.52 22.47 27.98 0.0548 0.0324 1.12 - 1.08 153 153 100.0 6.19 16.98 25.66 0.0599 0.0350 1.08 - 1.05 149 149 100.0 5.83 15.10 23.14 0.0584 0.0363 1.05 - 1.02 152 152 100.0 5.41 14.47 22.00 0.0611 0.0392 1.02 - 0.99 192 192 100.0 5.05 12.09 21.58 0.0658 0.0411 0.99 - 0.97 127 128 99.2 4.62 12.74 20.71 0.0698 0.0436 0.97 - 0.95 141 142 99.3 4.35 10.03 20.35 0.0710 0.0450 0.95 - 0.93 155 155 100.0 4.18 9.77 19.37 0.0736 0.0462 0.93 - 0.90 235 235 100.0 3.55 7.85 16.74 0.0638 0.0533 0.90 - 0.89 92 94 97.9 3.27 9.33 17.77 0.0651 0.0511 0.89 - 0.87 205 208 98.6 2.59 5.51 13.30 0.0673 0.0641 0.87 - 0.86 101 117 86.3 1.67 5.37 11.61 0.0714 0.0766 ------------------------------------------------------------------------------ 0.96 - 0.86 865 886 97.6 3.21 7.69 16.17 0.0683 0.0543 Inf - 0.86 3130 3158 99.1 5.74 29.15 25.78 0.0562 0.0318 Merged [S], lowest resolution = 12.95 Angstroms ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 neal054_0m.hkl Resolution #Data #Theory %Comp %F-comp Redund Ranom Rrim Rpim Inf - 3.75 26 26 100.0 82.4 9.15 6.85 0.2942 0.1189 0.0385 3.75 - 2.43 59 59 100.0 97.9 13.93 5.60 0.1625 0.0965 0.0253 2.43 - 1.89 80 80 100.0 100.0 15.49 5.27 0.1521 0.0933 0.0224 1.89 - 1.65 84 84 100.0 100.0 16.01 5.06 0.1539 0.0905 0.0220 1.65 - 1.49 84 84 100.0 100.0 15.05 4.86 0.1421 0.0808 0.0202 1.49 - 1.38 84 84 100.0 100.0 14.89 4.57 0.1490 0.0799 0.0203 1.38 - 1.29 89 89 100.0 100.0 14.36 3.88 0.1425 0.0802 0.0207 1.29 - 1.23 75 75 100.0 100.0 13.40 4.53 0.1556 0.0875 0.0234 1.23 - 1.18 79 79 100.0 98.6 12.62 3.59 0.1512 0.0866 0.0244 1.18 - 1.13 89 89 100.0 100.0 12.75 3.90 0.1559 0.0933 0.0257 1.13 - 1.09 81 81 100.0 100.0 12.02 4.97 0.2442 0.1274 0.0362 1.09 - 1.05 94 94 100.0 100.0 11.20 4.45 0.2328 0.1184 0.0344 1.05 - 1.02 81 81 100.0 100.0 10.15 3.41 0.2005 0.1082 0.0336 1.02 - 0.99 100 100 100.0 100.0 9.70 3.33 0.1782 0.1110 0.0352 0.99 - 0.97 67 67 100.0 98.4 8.82 3.84 0.2357 0.1380 0.0465 0.97 - 0.95 73 73 100.0 98.6 8.45 3.34 0.2195 0.1290 0.0434 0.95 - 0.93 80 80 100.0 100.0 8.10 3.15 0.1970 0.1245 0.0436 0.93 - 0.90 121 121 100.0 100.0 6.89 2.76 0.2066 0.1257 0.0458 0.90 - 0.89 50 51 98.0 97.7 6.02 2.68 0.1745 0.1108 0.0451 0.89 - 0.87 107 107 100.0 97.0 5.04 2.45 0.2350 0.1370 0.0588 0.87 - 0.86 56 62 90.3 81.8 3.15 2.20 0.2680 0.1498 0.0772 ------------------------------------------------------------------------------ 0.96 - 0.86 454 461 98.5 96.7 6.18 2.75 0.2137 0.1275 0.0483 Inf - 0.86 1659 1666 99.6 98.6 10.88 3.88 0.1732 0.0953 0.0258 Merged [P], lowest resolution = 12.95 Angstroms ------------------------------------------------------------------------------- Current dataset is # 1 neal054_0m.hkl ------------------------------------------------------------------------------- Current dataset is # 1 neal054_0m.hkl ------------------------------------------------------------------------------- Current dataset is # 1 neal054_0m.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C17H23IN2O4 Formula weight = 446.28 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.555, non-H atomic volume = 19.9 and following cell contents and analysis: C 34.00 45.75 % H 46.00 5.19 % N 4.00 6.28 % O 8.00 14.34 % I 2.00 28.44 % F(000) = 448.0 Cu-K(alpha) radiation Mu (mm-1) = 13.39 ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C17H23IN2O4 Formula weight = 446.28 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.555, non-H atomic volume = 19.9 and following cell contents and analysis: C 34.00 45.75 % H 46.00 5.19 % N 4.00 6.28 % O 8.00 14.34 % I 2.00 28.44 % F(000) = 448.0 Cu-K(alpha) radiation Mu (mm-1) = 13.39 ------------------------------------------------------------------------------- File neal054.ins set up as follows: TITL neal054 in P2(1) CELL 1.54178 6.25720 11.76300 13.03870 90.0000 96.6572 90.0000 ZERR 2.00 0.00050 0.00090 0.00100 0.0000 0.0000 0.0000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O I UNIT 34 46 4 8 2 TEMP -173.150 SIZE 0.028 0.099 0.172 TREF HKLF 4 END 18124 Reflections written to new reflection file neal054.hkl ------------------------------------------------------------------------------- File neal054.ins set up as follows: TITL neal054 in P2(1) CELL 1.54178 6.25720 11.76300 13.03870 90.0000 96.6572 90.0000 ZERR 2.00 0.00050 0.00090 0.00100 0.0000 0.0000 0.0000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O I UNIT 34 46 4 8 2 TEMP -173.150 SIZE 0.028 0.099 0.172 TREF HKLF 4 END 18124 Reflections written to new reflection file neal054.hkl -------------------------------------------------------------------------------