++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION - Version 2014/2 + + Copyright(C) 2014 Bruker-AXS All Rights Reserved + + rudi001_0m started at 15:10:47 on 13-Feb-2026 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 13.063 10.321 20.491 90.00 89.96 90.00 37286 Reflections read from file rudi001_0m.hkl; mean (I/sigma) = 10.58 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 18626 18660 18682 18596 27984 24838 24900 37286 N (int>3sigma) = 0 15541 15154 15697 15342 23196 20828 20908 31251 Mean intensity = 0.0 17.4 15.8 17.4 17.0 16.9 16.9 17.1 16.9 Mean int/sigma = 0.0 10.6 10.3 10.7 10.6 10.5 10.6 10.6 10.6 Lattice type: P chosen Volume: 2762.71 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 Unitcell: 10.321 13.063 20.491 89.96 90.00 90.00 Niggli form: a.a = 106.53 b.b = 170.63 c.c = 419.90 b.c = 0.19 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 = 0.041 deg. ORTHORHOMBIC P-lattice R(sym) = 0.032 [ 7600] Cell: 10.321 13.063 20.491 89.96 90.00 90.00 Volume: 2762.71 Matrix: 0.0000 -1.0000 0.0000 -1.0000 0.0000 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 = 2.558 Minimum I/sigma gap between absences and rest = 2.116 ------------------------------------------------------------------------------- Current dataset is # 1 rudi001_0m.hkl ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 Unitcell: 10.321 13.063 20.491 89.96 90.00 90.00 Niggli form: a.a = 106.53 b.b = 170.63 c.c = 419.90 b.c = 0.19 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 = 0.041 deg. ORTHORHOMBIC P-lattice R(sym) = 0.032 [ 7600] Cell: 10.321 13.063 20.491 89.96 90.00 90.00 Volume: 2762.71 Matrix: 0.0000 -1.0000 0.0000 -1.0000 0.0000 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 18660 18626 18682 18596 27984 24900 24838 37286 N (int>3sigma) = 0 15154 15541 15697 15342 23196 20908 20828 31251 Mean intensity = 0.0 15.8 17.4 17.4 17.0 16.9 17.1 16.9 16.9 Mean int/sigma = 0.0 10.3 10.6 10.7 10.6 10.5 10.6 10.6 10.6 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.989 [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 1152 1162 1200 22 1059 1056 1053 25 542 537 545 55 N I>3s 557 554 7 12 931 965 918 0 89 277 272 1 26.6 26.4 0.1 0.6 30.8 35.1 28.9 0.0 0.2 18.6 18.3 0.1 7.3 7.3 0.7 4.7 12.7 12.9 11.9 0.6 1.9 7.4 7.2 0.8 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] Pna2(1) # 33 non-cen 6 903 0.032 7600 4.7 / 7.2 8.39 [B] Pnma # 62 centro 1 894 0.032 7600 4.7 / 7.2 2.03 Option [B] 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 = 2.558 Minimum I/sigma gap between absences and rest = 2.116 ------------------------------------------------------------------------------- Current dataset is # 1 rudi001_0m.hkl ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 rudi001_0m.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge Rsigma Inf - 3.73 49 49 100.0 4.12 26.02 24.27 0.0594 0.0304 3.73 - 2.36 112 112 100.0 12.99 77.22 48.42 0.0493 0.0242 2.36 - 1.82 162 162 100.0 16.81 23.79 50.69 0.0482 0.0154 1.82 - 1.57 159 159 100.0 17.21 40.36 51.69 0.0436 0.0188 1.57 - 1.41 166 166 100.0 16.27 32.60 51.44 0.0452 0.0157 1.41 - 1.30 158 158 100.0 16.68 18.63 45.54 0.0502 0.0161 1.30 - 1.22 164 164 100.0 16.01 14.10 43.07 0.0520 0.0171 1.22 - 1.15 172 172 100.0 14.14 16.63 38.70 0.0528 0.0182 1.15 - 1.10 154 154 100.0 14.63 17.08 40.69 0.0509 0.0175 1.10 - 1.05 183 183 100.0 14.36 11.83 38.65 0.0513 0.0190 1.05 - 1.02 125 125 100.0 12.25 11.85 32.43 0.0570 0.0214 1.02 - 0.98 192 192 100.0 12.64 9.24 32.01 0.0546 0.0222 0.98 - 0.95 172 172 100.0 11.95 11.31 31.31 0.0528 0.0211 0.95 - 0.93 117 117 100.0 10.68 9.79 28.79 0.0632 0.0271 0.93 - 0.90 218 218 100.0 9.67 7.23 26.53 0.0639 0.0260 0.90 - 0.88 142 142 100.0 8.99 9.03 28.03 0.0653 0.0247 0.88 - 0.86 171 171 100.0 7.71 7.56 25.14 0.0623 0.0291 0.86 - 0.84 182 182 100.0 6.48 8.29 21.88 0.0680 0.0314 0.84 - 0.83 98 98 100.0 5.86 7.52 20.11 0.0711 0.0322 0.83 - 0.81 208 209 99.5 4.19 6.69 17.39 0.0746 0.0412 0.81 - 0.80 109 114 95.6 2.64 4.26 13.20 0.0803 0.0585 ------------------------------------------------------------------------------ 0.90 - 0.80 910 916 99.3 6.03 7.34 21.20 0.0675 0.0337 Inf - 0.80 3213 3219 99.8 11.58 16.53 34.19 0.0507 0.0216 Merged [A], lowest resolution = 20.49 Angstroms ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 rudi001_0m.hkl Resolution #Data #Theory %Comp Redundancy Rrim Rpim Inf - 3.73 49 49 100.00 4.12 0.0671 0.0300 3.73 - 2.36 112 112 100.00 12.99 0.0519 0.0154 2.36 - 1.82 162 162 100.00 16.81 0.0497 0.0121 1.82 - 1.57 159 159 100.00 17.21 0.0454 0.0121 1.57 - 1.41 166 166 100.00 16.27 0.0468 0.0119 1.41 - 1.30 158 158 100.00 16.68 0.0519 0.0129 1.30 - 1.22 164 164 100.00 16.01 0.0537 0.0130 1.22 - 1.15 172 172 100.00 14.14 0.0549 0.0149 1.15 - 1.10 154 154 100.00 14.63 0.0528 0.0137 1.10 - 1.05 183 183 100.00 14.36 0.0533 0.0141 1.05 - 1.02 125 125 100.00 12.25 0.0598 0.0176 1.02 - 0.98 192 192 100.00 12.64 0.0570 0.0163 0.98 - 0.95 172 172 100.00 11.95 0.0554 0.0163 0.95 - 0.93 117 117 100.00 10.68 0.0673 0.0219 0.93 - 0.90 218 218 100.00 9.67 0.0676 0.0217 0.90 - 0.88 142 142 100.00 8.99 0.0696 0.0236 0.88 - 0.86 171 171 100.00 7.71 0.0678 0.0257 0.86 - 0.84 182 182 100.00 6.48 0.0751 0.0306 0.84 - 0.83 98 98 100.00 5.86 0.0787 0.0330 0.83 - 0.81 208 209 99.52 4.19 0.0861 0.0421 0.81 - 0.80 109 114 95.61 2.64 0.0985 0.0556 -------------------------------------------------------- 0.90 - 0.80 910 916 99.34 6.03 0.0744 0.0300 Inf - 0.80 3213 3219 99.81 11.58 0.0531 0.0150 Merged [P], lowest resolution = 20.49 Angstroms ------------------------------------------------------------------------------- Current dataset is # 1 rudi001_0m.hkl ------------------------------------------------------------------------------- Current dataset is # 1 rudi001_0m.hkl ------------------------------------------------------------------------------- Current dataset is # 1 rudi001_0m.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C14 H20 B22 Cl22 N6 Ni Formula weight = 1348.84 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.621, non-H atomic volume = 21.3 and following cell contents and analysis: C 28.00 12.47 % H 40.00 1.49 % B 44.00 17.63 % N 12.00 6.23 % Cl 44.00 57.82 % Ni 2.00 4.35 % F(000) = 1316.0 Cu-K(alpha) radiation Mu (mm-1) = 10.52 ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C14 H20 B22 Cl22 N6 Ni Formula weight = 1348.84 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.621, non-H atomic volume = 21.3 and following cell contents and analysis: C 28.00 12.47 % H 40.00 1.49 % B 44.00 17.63 % N 12.00 6.23 % Cl 44.00 57.82 % Ni 2.00 4.35 % F(000) = 1316.0 Cu-K(alpha) radiation Mu (mm-1) = 10.52 ------------------------------------------------------------------------------- File rudi001.ins set up as follows: TITL rudi001 in Pnma CELL 1.54178 10.32120 13.06270 20.49140 90.0000 90.0000 90.0000 ZERR 2.00 0.00030 0.00030 0.00050 0.0000 0.0000 0.0000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, -Z SYMM 0.5+X, 0.5-Y, 0.5-Z SFAC C H B N CL NI UNIT 28 40 44 12 44 2 TEMP -166.150 SIZE 0.132 0.149 0.259 TREF HKLF 4 END 37286 Reflections written to new reflection file rudi001.hkl -------------------------------------------------------------------------------