++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION - Version 2014/2 + + Copyright(C) 2014 Bruker-AXS All Rights Reserved + + rudi002_0m started at 16:34:29 on 12-Mar-2026 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 14.186 14.278 21.341 89.74 72.20 74.79 130012 Reflections read from file rudi002_0m.hkl; mean (I/sigma) = 9.28 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 64948 65063 65033 64908 97522 86698 86581 130012 N (int>3sigma) = 0 57153 57186 56995 57075 85667 76069 76082 114265 Mean intensity = 0.0 23.3 23.2 23.2 23.3 23.2 23.0 22.6 22.9 Mean int/sigma = 0.0 9.3 9.3 9.3 9.3 9.3 9.3 9.3 9.3 Lattice type: P chosen Volume: 3957.99 ------------------------------------------------------------------------------- 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: 14.186 14.278 21.341 89.74 72.20 74.79 Niggli form: a.a = 201.24 b.b = 203.87 c.c = 455.43 b.c = 1.39 a.c = 92.55 a.b = 53.13 ------------------------------------------------------------------------------- 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: 14.186 14.278 21.341 89.74 72.20 74.79 Volume: 3957.99 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 = 2.428 Minimum I/sigma gap between absences and rest = 1.857 ------------------------------------------------------------------------------- Current dataset is # 1 rudi002_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: 14.186 14.278 21.341 89.74 72.20 74.79 Niggli form: a.a = 201.24 b.b = 203.87 c.c = 455.43 b.c = 1.39 a.c = 92.55 a.b = 53.13 ------------------------------------------------------------------------------- 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: 14.186 14.278 21.341 89.74 72.20 74.79 Volume: 3957.99 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 64948 65063 65033 64908 97522 86698 86581 130012 N (int>3sigma) = 0 57153 57186 56995 57075 85667 76069 76082 114265 Mean intensity = 0.0 23.3 23.2 23.2 23.3 23.2 23.0 22.6 22.9 Mean int/sigma = 0.0 9.3 9.3 9.3 9.3 9.3 9.3 9.3 9.3 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.896 [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 1.61 [B] P1 # 1 chiral 1 700 0.000 0 0.0 / 9.3 3.77 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 = 2.428 Minimum I/sigma gap between absences and rest = 1.857 ------------------------------------------------------------------------------- Current dataset is # 1 rudi002_0m.hkl ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 rudi002_0m.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge Rsigma Inf - 3.27 239 240 99.6 9.14 58.50 42.12 0.0478 0.0228 3.27 - 2.18 560 560 100.0 12.80 76.15 46.88 0.0485 0.0192 2.18 - 1.73 790 790 100.0 13.81 37.53 46.16 0.0489 0.0187 1.73 - 1.51 827 827 100.0 13.21 36.78 41.85 0.0476 0.0195 1.51 - 1.37 818 818 100.0 12.77 33.10 39.54 0.0500 0.0204 1.37 - 1.27 808 808 100.0 11.97 19.52 33.72 0.0586 0.0233 1.27 - 1.20 754 754 100.0 11.44 18.62 32.05 0.0607 0.0244 1.20 - 1.14 810 810 100.0 10.95 18.74 30.21 0.0631 0.0253 1.14 - 1.09 774 774 100.0 9.98 18.66 27.92 0.0684 0.0274 1.09 - 1.05 803 803 100.0 10.03 16.15 27.69 0.0676 0.0279 1.05 - 1.01 859 859 100.0 8.91 11.53 22.80 0.0773 0.0337 1.01 - 0.98 778 778 100.0 8.58 12.19 22.20 0.0774 0.0337 0.98 - 0.95 832 832 100.0 8.00 11.08 20.57 0.0789 0.0361 0.95 - 0.92 998 998 100.0 7.03 10.67 18.88 0.0858 0.0403 0.92 - 0.90 712 712 100.0 6.23 9.54 16.71 0.0985 0.0458 0.90 - 0.88 800 800 100.0 5.20 8.68 14.86 0.1035 0.0519 0.88 - 0.86 870 889 97.9 3.10 8.82 12.59 0.0842 0.0630 0.86 - 0.84 903 928 97.3 2.59 8.52 11.56 0.0802 0.0688 0.84 - 0.83 480 494 97.2 2.24 8.15 10.74 0.0823 0.0720 0.83 - 0.81 1044 1132 92.2 1.73 6.53 8.82 0.0860 0.0900 0.81 - 0.80 417 616 67.7 0.99 5.23 7.16 0.0992 0.1125 ------------------------------------------------------------------------------ 0.90 - 0.80 4514 4859 92.9 2.67 7.80 11.22 0.0909 0.0714 Inf - 0.80 15876 16222 97.9 8.01 18.74 24.87 0.0576 0.0300 Merged [A], lowest resolution = 13.73 Angstroms ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 rudi002_0m.hkl Resolution #Data #Theory %Comp Redundancy Rrim Rpim Inf - 3.27 239 240 99.58 9.14 0.0508 0.0167 3.27 - 2.18 560 560 100.00 12.80 0.0506 0.0143 2.18 - 1.73 790 790 100.00 13.81 0.0508 0.0138 1.73 - 1.51 827 827 100.00 13.21 0.0496 0.0137 1.51 - 1.37 818 818 100.00 12.77 0.0521 0.0147 1.37 - 1.27 808 808 100.00 11.97 0.0613 0.0180 1.27 - 1.20 754 754 100.00 11.44 0.0636 0.0189 1.20 - 1.14 810 810 100.00 10.95 0.0663 0.0202 1.14 - 1.09 774 774 100.00 9.98 0.0723 0.0233 1.09 - 1.05 803 803 100.00 10.03 0.0714 0.0227 1.05 - 1.01 859 859 100.00 8.91 0.0822 0.0279 1.01 - 0.98 778 778 100.00 8.58 0.0825 0.0283 0.98 - 0.95 832 832 100.00 8.00 0.0845 0.0301 0.95 - 0.92 998 998 100.00 7.03 0.0929 0.0353 0.92 - 0.90 712 712 100.00 6.23 0.1079 0.0436 0.90 - 0.88 800 800 100.00 5.20 0.1156 0.0507 0.88 - 0.86 870 889 97.86 3.10 0.1009 0.0546 0.86 - 0.84 903 928 97.31 2.59 0.0996 0.0580 0.84 - 0.83 480 494 97.17 2.24 0.1045 0.0635 0.83 - 0.81 1044 1132 92.23 1.73 0.1134 0.0730 0.81 - 0.80 417 616 67.69 0.99 0.1348 0.0907 -------------------------------------------------------- 0.90 - 0.80 4514 4859 92.90 2.67 0.1083 0.0570 Inf - 0.80 15876 16222 97.87 8.01 0.0609 0.0193 Merged [P], lowest resolution = 13.73 Angstroms ------------------------------------------------------------------------------- Current dataset is # 1 rudi002_0m.hkl ------------------------------------------------------------------------------- Current dataset is # 1 rudi002_0m.hkl ------------------------------------------------------------------------------- Current dataset is # 1 rudi002_0m.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C21 H31 B33 Cl33 F6 Gd O8 Formula weight = 2209.41 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.854, non-H atomic volume = 19.4 and following cell contents and analysis: C 42.00 11.42 % H 62.00 1.41 % B 66.00 16.15 % O 16.00 5.79 % F 12.00 5.16 % Cl 66.00 52.95 % Gd 2.00 7.12 % F(000) = 2130.0 Cu-K(alpha) radiation Mu (mm-1) = 16.15 ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C21 H31 B33 Cl33 F6 Gd O8 Formula weight = 2209.41 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.854, non-H atomic volume = 19.4 and following cell contents and analysis: C 42.00 11.42 % H 62.00 1.41 % B 66.00 16.15 % O 16.00 5.79 % F 12.00 5.16 % Cl 66.00 52.95 % Gd 2.00 7.12 % F(000) = 2130.0 Cu-K(alpha) radiation Mu (mm-1) = 16.15 ------------------------------------------------------------------------------- File rudi002.ins set up as follows: TITL rudi002 in P-1 CELL 1.54178 14.18590 14.27820 21.34070 89.7393 72.1991 74.7922 ZERR 2.00 0.00050 0.00050 0.00080 0.0017 0.0017 0.0017 LATT 1 SFAC C H B O F CL GD UNIT 42 62 66 16 12 66 2 TEMP -166.150 SIZE 0.163 0.189 0.262 TREF HKLF 4 END 130012 Reflections written to new reflection file rudi002.hkl -------------------------------------------------------------------------------