++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION - Version 2014/2 + + Copyright(C) 2014 Bruker-AXS All Rights Reserved + + rudi005_0m started at 16:00:28 on 29-Apr-2026 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.201 16.694 22.176 90.00 90.00 90.00 32863 Reflections read from file rudi005_0m.hkl; mean (I/sigma) = 10.62 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 16627 16417 16414 16466 24729 21911 21903 32863 N (int>3sigma) = 0 15051 15266 15209 15156 22763 20335 20350 30450 Mean intensity = 0.0 31.6 47.9 48.3 46.7 42.5 47.6 47.8 47.5 Mean int/sigma = 0.0 9.8 10.7 10.7 10.5 10.4 10.6 10.6 10.6 Lattice type: P chosen Volume: 4146.82 ------------------------------------------------------------------------------- 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: 11.201 16.694 22.176 90.00 90.00 90.00 Niggli form: a.a = 125.47 b.b = 278.70 c.c = 491.77 b.c = 0.00 a.c = 0.00 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. ORTHORHOMBIC P-lattice R(sym) = 0.050 [ 10883] Cell: 11.201 16.694 22.176 90.00 90.00 90.00 Volume: 4146.82 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Current cell not changed ------------------------------------------------------------------------------- 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 = 2.562 Minimum I/sigma gap between absences and rest = 2.124 ------------------------------------------------------------------------------- Current dataset is # 1 rudi005_0m.hkl ------------------------------------------------------------------------------- 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: 11.201 16.694 22.176 90.00 90.00 90.00 Niggli form: a.a = 125.47 b.b = 278.70 c.c = 491.77 b.c = 0.00 a.c = 0.00 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. ORTHORHOMBIC P-lattice R(sym) = 0.050 [ 10883] Cell: 11.201 16.694 22.176 90.00 90.00 90.00 Volume: 4146.82 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 16627 16417 16414 16466 24729 21911 21903 32863 N (int>3sigma) = 0 15051 15266 15209 15156 22763 20335 20350 30450 Mean intensity = 0.0 31.6 47.9 48.3 46.7 42.5 47.6 47.8 47.5 Mean int/sigma = 0.0 9.8 10.7 10.7 10.5 10.4 10.6 10.6 10.6 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.754 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 1036 1044 1064 9 554 545 553 25 473 473 468 28 N I>3s 844 833 813 3 460 466 464 3 401 396 377 2 40.1 40.1 24.1 0.4 38.4 41.8 54.1 0.3 40.7 40.3 38.1 0.4 9.1 9.0 8.1 1.8 9.1 9.5 9.8 1.6 9.5 9.5 9.1 1.2 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)2(1)2(1) # 19 chiral 1 5917 0.050 10883 1.8 / 8.1 1.51 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 = 2.562 Minimum I/sigma gap between absences and rest = 2.124 ------------------------------------------------------------------------------- Current dataset is # 1 rudi005_0m.hkl ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 rudi005_0m.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge Rsigma Inf - 3.31 126 127 99.2 2.09 154.40 21.16 0.0439 0.0443 3.31 - 2.20 291 291 100.0 5.65 111.96 32.42 0.0461 0.0284 2.20 - 1.74 418 418 100.0 5.99 116.94 33.75 0.0450 0.0278 1.74 - 1.52 423 423 100.0 5.90 56.21 29.87 0.0486 0.0300 1.52 - 1.38 409 409 100.0 5.57 59.82 29.11 0.0484 0.0311 1.38 - 1.28 424 424 100.0 5.34 65.01 27.36 0.0476 0.0322 1.28 - 1.20 447 448 99.8 5.04 53.87 25.94 0.0495 0.0340 1.20 - 1.14 413 413 100.0 4.96 43.40 24.05 0.0517 0.0354 1.14 - 1.09 428 428 100.0 4.62 41.08 22.27 0.0584 0.0380 1.09 - 1.05 402 402 100.0 4.64 36.73 22.06 0.0573 0.0379 1.05 - 1.01 452 452 100.0 4.16 34.01 20.21 0.0599 0.0423 1.01 - 0.98 417 417 100.0 4.09 27.28 18.84 0.0609 0.0439 0.98 - 0.95 443 443 100.0 3.88 25.33 17.65 0.0661 0.0452 0.95 - 0.93 318 318 100.0 3.58 22.28 16.93 0.0682 0.0486 0.93 - 0.91 386 387 99.7 3.25 19.96 15.02 0.0746 0.0553 0.91 - 0.88 593 594 99.8 3.00 21.51 15.35 0.0753 0.0552 0.88 - 0.86 456 461 98.9 2.39 22.77 14.41 0.0721 0.0595 0.86 - 0.85 229 247 92.7 2.01 19.74 12.85 0.0743 0.0681 0.85 - 0.83 491 515 95.3 1.90 19.96 12.41 0.0771 0.0681 0.83 - 0.81 513 575 89.2 1.58 17.64 11.54 0.0819 0.0761 0.81 - 0.80 212 313 67.7 0.95 15.57 10.04 0.0884 0.0885 ------------------------------------------------------------------------------ 0.90 - 0.80 2309 2520 91.6 1.98 19.91 12.92 0.0757 0.0668 Inf - 0.80 8291 8505 97.5 3.86 42.65 20.63 0.0521 0.0393 Merged [S], lowest resolution = 22.18 Angstroms ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 rudi005_0m.hkl Resolution #Data #Theory %Comp %F-comp Redund Ranom Rrim Rpim Inf - 3.68 71 71 100.0 96.0 2.48 2.66 0.1627 0.0854 0.0483 3.68 - 2.32 165 165 100.0 100.0 8.12 3.68 0.1064 0.0677 0.0231 2.32 - 1.81 235 235 100.0 100.0 10.08 2.89 0.0807 0.0614 0.0187 1.81 - 1.56 237 237 100.0 100.0 10.38 2.71 0.0865 0.0639 0.0194 1.56 - 1.40 251 251 100.0 100.0 9.86 2.62 0.0925 0.0693 0.0220 1.40 - 1.30 226 226 100.0 100.0 9.31 2.48 0.0864 0.0632 0.0205 1.30 - 1.22 233 234 99.6 100.0 9.44 2.46 0.0811 0.0667 0.0215 1.22 - 1.15 262 262 100.0 100.0 8.61 2.39 0.1084 0.0754 0.0255 1.15 - 1.10 230 230 100.0 100.0 8.39 2.25 0.1050 0.0821 0.0286 1.10 - 1.06 207 207 100.0 100.0 8.61 2.35 0.1136 0.0837 0.0283 1.06 - 1.02 241 241 100.0 100.0 7.76 2.17 0.1162 0.0856 0.0305 1.02 - 0.98 296 296 100.0 100.0 7.49 2.02 0.1137 0.0864 0.0310 0.98 - 0.95 244 244 100.0 100.0 7.05 1.72 0.1017 0.0870 0.0325 0.95 - 0.93 170 170 100.0 100.0 6.71 1.61 0.1070 0.0920 0.0352 0.93 - 0.90 314 314 100.0 99.6 5.82 1.86 0.1407 0.1062 0.0436 0.90 - 0.88 221 221 100.0 99.5 5.48 1.78 0.1300 0.1031 0.0446 0.88 - 0.86 248 251 98.8 99.0 4.39 1.57 0.1272 0.1019 0.0475 0.86 - 0.84 267 277 96.4 92.4 3.63 1.57 0.1626 0.1145 0.0583 0.84 - 0.83 134 136 98.5 89.3 3.43 1.57 0.1582 0.1196 0.0635 0.83 - 0.81 307 310 99.0 77.7 2.92 1.54 0.1725 0.1241 0.0688 0.81 - 0.80 143 167 85.6 47.3 1.78 1.68 0.2503 0.1628 0.1004 ------------------------------------------------------------------------------ 0.90 - 0.80 1320 1362 96.9 85.4 3.66 1.61 0.1538 0.1119 0.0555 Inf - 0.80 4702 4745 99.1 95.5 6.93 2.11 0.1068 0.0737 0.0259 Merged [P], lowest resolution = 22.18 Angstroms ------------------------------------------------------------------------------- Current dataset is # 1 rudi005_0m.hkl ------------------------------------------------------------------------------- Current dataset is # 1 rudi005_0m.hkl ------------------------------------------------------------------------------- Current dataset is # 1 rudi005_0m.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C37 H53 B11 Cl11 I In N Formula weight = 1262.45 Tentative Z (number of formula units/cell) = 4.0 giving rho = 2.022, non-H atomic volume = 16.7 and following cell contents and analysis: C 148.00 35.20 % H 212.00 4.23 % B 44.00 9.42 % N 4.00 1.11 % Cl 44.00 30.89 % In 4.00 9.09 % I 4.00 10.05 % F(000) = 2504.0 Cu-K(alpha) radiation Mu (mm-1) = 17.20 ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C37 H53 B11 Cl11 I In N Formula weight = 1262.45 Tentative Z (number of formula units/cell) = 4.0 giving rho = 2.022, non-H atomic volume = 16.7 and following cell contents and analysis: C 148.00 35.20 % H 212.00 4.23 % B 44.00 9.42 % N 4.00 1.11 % Cl 44.00 30.89 % In 4.00 9.09 % I 4.00 10.05 % F(000) = 2504.0 Cu-K(alpha) radiation Mu (mm-1) = 17.20 ------------------------------------------------------------------------------- File rudi005.ins set up as follows: TITL rudi005 in P2(1)2(1)2(1) CELL 1.54178 11.20130 16.69420 22.17590 90.0000 90.0000 90.0000 ZERR 4.00 0.00030 0.00040 0.00060 0.0000 0.0000 0.0000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H B N CL IN I UNIT 148 212 44 4 44 4 4 TEMP -170.150 SIZE 0.065 0.126 0.131 TREF HKLF 4 END 32863 Reflections written to new reflection file rudi005.hkl -------------------------------------------------------------------------------