++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION - Version 2014/2 + + Copyright(C) 2014 Bruker-AXS All Rights Reserved + + rudi004_0m started at 12:39:57 on 09-Apr-2026 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.932 13.030 19.217 93.96 98.56 97.14 93369 Reflections read from file rudi004_0m.hkl; mean (I/sigma) = 9.30 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 46717 46775 46662 46731 70077 62291 62210 93369 N (int>3sigma) = 0 36736 37069 36691 36988 55248 49027 49115 73657 Mean intensity = 0.0 25.4 25.2 25.5 25.8 25.4 25.1 25.2 25.2 Mean int/sigma = 0.0 9.3 9.3 9.4 9.4 9.4 9.3 9.3 9.3 Lattice type: P chosen Volume: 2919.90 ------------------------------------------------------------------------------- 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: 11.932 13.030 19.217 93.96 98.56 97.14 Niggli form: a.a = 142.37 b.b = 169.79 c.c = 369.30 b.c = -17.31 a.c = -34.13 a.b = -19.32 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(sym) = 0.000 [ 0] Cell: 11.932 13.030 19.217 93.96 98.56 97.14 Volume: 2919.90 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 = 2.430 Minimum I/sigma gap between absences and rest = 1.859 ------------------------------------------------------------------------------- Current dataset is # 1 rudi004_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: 11.932 13.030 19.217 93.96 98.56 97.14 Niggli form: a.a = 142.37 b.b = 169.79 c.c = 369.30 b.c = -17.31 a.c = -34.13 a.b = -19.32 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(sym) = 0.000 [ 0] Cell: 11.932 13.030 19.217 93.96 98.56 97.14 Volume: 2919.90 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 46717 46775 46662 46731 70077 62291 62210 93369 N (int>3sigma) = 0 36736 37069 36691 36988 55248 49027 49115 73657 Mean intensity = 0.0 25.4 25.2 25.5 25.8 25.4 25.1 25.2 25.2 Mean int/sigma = 0.0 9.3 9.3 9.4 9.4 9.4 9.3 9.3 9.3 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.980 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic 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] P-1 # 2 centro 1 8646 0.000 0 0.0 / 9.3 1.10 [B] P1 # 1 chiral 1 700 0.000 0 0.0 / 9.3 7.19 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 = 2.430 Minimum I/sigma gap between absences and rest = 1.859 ------------------------------------------------------------------------------- Current dataset is # 1 rudi004_0m.hkl ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 rudi004_0m.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge Rsigma Inf - 3.22 177 177 100.0 10.25 52.47 47.31 0.0460 0.0198 3.22 - 2.18 413 413 100.0 14.13 82.97 52.16 0.0444 0.0175 2.18 - 1.72 602 602 100.0 14.80 39.92 47.47 0.0444 0.0164 1.72 - 1.51 578 578 100.0 13.82 39.16 42.73 0.0462 0.0172 1.51 - 1.37 606 606 100.0 12.22 36.36 40.30 0.0461 0.0189 1.37 - 1.27 615 615 100.0 11.02 22.66 32.31 0.0503 0.0219 1.27 - 1.20 535 535 100.0 10.51 18.73 29.23 0.0577 0.0239 1.20 - 1.14 613 613 100.0 10.08 22.54 29.35 0.0556 0.0237 1.14 - 1.09 569 569 100.0 9.20 21.57 27.42 0.0601 0.0256 1.09 - 1.05 571 571 100.0 9.24 19.22 25.36 0.0605 0.0261 1.05 - 1.01 644 644 100.0 8.16 12.37 20.59 0.0773 0.0335 1.01 - 0.98 567 567 100.0 7.90 12.03 19.44 0.0816 0.0345 0.98 - 0.95 659 659 100.0 7.43 13.23 19.71 0.0757 0.0341 0.95 - 0.92 679 679 100.0 6.66 12.03 17.73 0.0863 0.0387 0.92 - 0.90 578 578 100.0 5.88 12.18 16.10 0.0946 0.0430 0.90 - 0.88 571 571 100.0 5.01 11.47 14.99 0.0959 0.0477 0.88 - 0.86 609 623 97.8 3.25 10.79 13.87 0.0674 0.0529 0.86 - 0.84 719 738 97.4 2.70 10.16 11.87 0.0725 0.0632 0.84 - 0.83 345 360 95.8 2.41 10.11 11.46 0.0726 0.0657 0.83 - 0.81 763 805 94.8 1.90 7.26 9.12 0.0782 0.0843 0.81 - 0.80 326 435 74.9 1.13 6.80 7.14 0.0767 0.1030 ------------------------------------------------------------------------------ 0.90 - 0.80 3333 3532 94.4 2.76 9.50 11.64 0.0804 0.0646 Inf - 0.80 11739 11938 98.3 7.82 20.76 24.58 0.0535 0.0284 Merged [A], lowest resolution = 18.93 Angstroms ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 rudi004_0m.hkl Resolution #Data #Theory %Comp Redundancy Rrim Rpim Inf - 3.22 177 177 100.00 10.25 0.0486 0.0154 3.22 - 2.18 413 413 100.00 14.13 0.0464 0.0132 2.18 - 1.72 602 602 100.00 14.80 0.0461 0.0121 1.72 - 1.51 578 578 100.00 13.82 0.0480 0.0130 1.51 - 1.37 606 606 100.00 12.22 0.0482 0.0139 1.37 - 1.27 615 615 100.00 11.02 0.0528 0.0159 1.27 - 1.20 535 535 100.00 10.51 0.0607 0.0188 1.20 - 1.14 613 613 100.00 10.08 0.0587 0.0185 1.14 - 1.09 569 569 100.00 9.20 0.0638 0.0213 1.09 - 1.05 571 571 100.00 9.24 0.0641 0.0213 1.05 - 1.01 644 644 100.00 8.16 0.0827 0.0290 1.01 - 0.98 567 567 100.00 7.90 0.0876 0.0317 0.98 - 0.95 659 659 100.00 7.43 0.0816 0.0303 0.95 - 0.92 679 679 100.00 6.66 0.0941 0.0370 0.92 - 0.90 578 578 100.00 5.88 0.1044 0.0437 0.90 - 0.88 571 571 100.00 5.01 0.1080 0.0489 0.88 - 0.86 609 623 97.75 3.25 0.0798 0.0420 0.86 - 0.84 719 738 97.43 2.70 0.0891 0.0509 0.84 - 0.83 345 360 95.83 2.41 0.0902 0.0526 0.83 - 0.81 763 805 94.78 1.90 0.1015 0.0638 0.81 - 0.80 326 435 74.94 1.13 0.1049 0.0711 -------------------------------------------------------- 0.90 - 0.80 3333 3532 94.37 2.76 0.0955 0.0500 Inf - 0.80 11739 11938 98.33 7.82 0.0567 0.0183 Merged [P], lowest resolution = 18.93 Angstroms ------------------------------------------------------------------------------- Current dataset is # 1 rudi004_0m.hkl ------------------------------------------------------------------------------- Current dataset is # 1 rudi004_0m.hkl ------------------------------------------------------------------------------- Current dataset is # 1 rudi004_0m.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C16 H18 B22 Cl22 Ni Formula weight = 1286.81 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.464, non-H atomic volume = 23.9 and following cell contents and analysis: C 32.00 14.93 % H 36.00 1.41 % B 44.00 18.48 % Cl 44.00 60.61 % Ni 2.00 4.56 % F(000) = 1252.0 Cu-K(alpha) radiation Mu (mm-1) = 9.89 ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C16 H18 B22 Cl22 Ni Formula weight = 1286.81 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.464, non-H atomic volume = 23.9 and following cell contents and analysis: C 32.00 14.93 % H 36.00 1.41 % B 44.00 18.48 % Cl 44.00 60.61 % Ni 2.00 4.56 % F(000) = 1252.0 Cu-K(alpha) radiation Mu (mm-1) = 9.89 ------------------------------------------------------------------------------- File rudi004.ins set up as follows: TITL rudi004 in P-1 CELL 1.54178 11.93190 13.03020 19.21730 93.9636 98.5598 97.1401 ZERR 2.00 0.00040 0.00040 0.00060 0.0015 0.0014 0.0014 LATT 1 SFAC C H B CL NI UNIT 32 36 44 44 2 TEMP -164.150 SIZE 0.146 0.233 0.276 TREF HKLF 4 END 93369 Reflections written to new reflection file rudi004.hkl -------------------------------------------------------------------------------