++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXTL XT - CRYSTAL STRUCTURE SOLUTION VERSION 2014/5 + + Copyright(c) Bruker AXS 2010-2014 All Rights Reserved + + Started at 16:28:02 on 18 Oct 2021 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ XT should be started by: xt name to read name.ins and name.hkl, followed by any of the following switches on the same line (default settings in square brackets). The cell, types of element present and Laue group (but not space group or numbers of atoms) are taken from the .ins file. Only CELL, LATT, SYMM, SFAC and HKLF are read from this file. If -l is not set, the SYMM instructions set the Laue group. General: -l Laue group N (SADABS code). N=15 all hexagonal and trigonal N=16 monoclinic with a unique, N=17 monoclinic with c unique -tN use N threads, otherwise use 5 or max available, if less. -d highest resolution to be employed [-d0.8] -e fill out missing data to specified resolution [-eX] where X is max(0.9,d-0.1) and d is the observed resolution Phasing: -q structure factors Go=E^q*Fo^(1-q) [-q0.5] -iN NGo-(N-1)Gc map in dual space recycling [-i3] -o switch OFF Patterson superpostion (not recommended) -kN apply random omit every kth cycle [-k3] -fX randomly omit fraction X of atoms [-f0.3] -z sigma threshold for P1 peak-search [-z2.5] -uX tangent expansion for E>X after random omit [off] -v atomic volume threshold for P1 peak-search [-v13] -m initial number of P1 dual space iterations [-m100] -b spread factor for atom masks [-b3] -jX CFOM = 0.01*CC - X*R(weak) [-j1] -y CFOM = CHEM*CC (alternative to default -j1) [off] -xX accept if CFOM > X+0.01*max(20-m,0) where m is try number [-x0.65] CHEM is a 'chemical' figure of merit that should be between 1.0 (most reasonable) and 0.0 (awful). Currently the only option (-y or -y1) is the fraction of bond angles between 95 and 135 degrees ignoring the 20% highest and 10% lowest peaks. This is only useful for organic compounds and ligands, not for inorganics, but can be invaluable when CC and R(weak) fail to distinguish between correct and incorrect P1 solutions. Space group determination: -s"Name" space group (replace "/" by "_" e.g. -s"P2(1)_c") [off] -c space group restricted to the Sohncke space groups [off] -n space group restricted to non-centrosymmetric [off] -w worst alpha gap for a possible solution [-w0.15] -p maximum number of atoms in full matrix, rest are blocked [-p20] -g smallest gap in R1 to best cent. for non-cent. SG [-g0.02] -h halt if R1 is less that this [-h0.08] -r radius around peak for density integration [-r0.7] -aX search ALL space groups in given Laue group with alpha < X [off] -a overrides -g, -h and -w, but not -c or -n; -a without a number is equivalent to -a0.3. If the default settings fail, try -y and -a if the CC is good but the solution is a mess, -q1 or -m1000 if all the CC values are less than 0.87. Also worth trying is truncating noisy outer data with -d. Command line parameters: neal054 4 threads running in parallel Unit-cell: 6.252 11.741 13.037 90.00 96.74 90.00 -a set to extend space group search because atom heavier than Sc expected Laue group identified as number 2: 2/m 3177 reflections read from file neal054.hkl R(sym) = 0.0495, R(rim) = 0.0638, R(pim) = 0.0397 Highest resln. = 0.860 A. For 1.2>d>1.1, = 34.0 and %(F>4sig) = 98.9 1558 unique reflections converted to 2950 with d > 0.860 A in P1 79 data added to fill out missing data to 0.900A in P1 Fourier grid: 24 x 40 x 45: 0.261 x 0.294 x 0.290 A Mean |E^2-1| 0kl 0.672 h0l 0.867 hk0 0.641 Rest 0.638 321 Reflections with E < 0.330 employed for R(weak) Unique Patterson peaks (origin + d>1.7A) for superposition: N X Y Z Height Distance 1 0.0000 0.0000 0.0000 999.00 0.000 2 0.8578 0.5000 0.0602 394.82 6.003 3 0.0004 0.5549 0.5000 84.51 8.355 4 0.4018 0.6557 0.2029 67.70 5.299 5 0.5002 0.8683 0.4200 56.91 6.793 6 0.0000 0.6267 0.0000 52.62 4.383 7 0.0781 0.8773 0.4081 51.55 5.478 8 0.1684 0.9482 0.4443 51.43 5.796 9 0.4797 0.2188 0.4149 49.54 6.406 10 0.0858 0.6221 0.5300 48.95 7.635 11 0.8146 0.1268 0.0715 48.94 2.164 12 0.6653 0.2765 0.5307 48.85 7.024 13 0.6159 0.2271 0.3120 48.14 5.632 14 0.3754 0.3849 0.6329 43.40 7.175 15 0.3732 0.6528 0.4680 42.51 7.480 16 0.7447 0.7521 0.2224 42.49 4.529 17 0.4443 0.1509 0.8653 42.18 3.884 18 0.4265 0.3157 0.5613 40.46 7.559 19 0.5898 0.1201 0.2464 39.63 4.563 20 0.5772 0.1827 0.5100 36.18 6.959 21 0.3742 0.2747 0.9835 34.71 4.005 22 0.0130 0.0836 0.5000 34.15 6.583 23 0.2950 0.4646 0.7952 33.82 6.437 24 0.8813 0.5000 0.1588 32.58 6.298 25 0.5247 0.7758 0.9292 32.14 3.996 26 0.7344 0.5491 0.6871 32.03 6.770 27 0.5394 0.2624 0.1601 31.56 4.853 28 0.5946 0.9527 0.7429 31.28 3.997 29 0.4440 0.9677 0.7313 30.88 4.733 30 0.4532 0.6213 0.3058 30.74 6.406 31 0.7830 0.4234 0.5485 30.55 7.702 32 0.5424 0.6984 0.6226 30.28 6.452 33 0.0059 0.5000 0.8627 30.11 6.139 34 0.4826 0.8564 0.3098 29.99 5.039 35 0.0000 0.4716 0.0000 29.88 5.537 36 0.5678 0.9529 0.6109 29.84 5.489 37 0.7674 0.8484 0.7332 29.83 4.025 38 0.8917 0.7403 0.1497 29.74 3.724 39 0.2529 0.5000 0.0272 29.41 6.079 40 0.0613 0.5000 0.0974 28.51 6.009 40 unique Patterson peaks with heights greater than 28 selected as superposition vectors Setup: 0.427 secs Try N(iter) CC R(weak) CHEM CFOM best Sig(min) N(P1) Vol/N 1 100 85.57 0.0958 0.3125 0.7599 0.7599 2.389 57 16.67 2 100 86.87 0.0806 0.8333 0.7881 0.7881 2.790 48 19.80 3 100 85.20 0.0691 0.5000 0.7830 0.7881 2.798 50 19.01 4 100 86.76 0.0861 0.3684 0.7815 0.7881 2.800 48 19.80 5 146 88.63 0.1092 0.2857 0.7772 0.7881 2.439 59 16.11 6 146 90.58 0.1319 0.6000 0.7739 0.7881 2.460 38 25.01 7 146 85.49 0.1469 1.0000 0.7080 0.7881 2.485 37 25.69 8 146 78.68 0.1999 0.3333 0.5869 0.7881 2.398 64 14.85 8 attempts, solution 2 selected with best CFOM = 0.7881, Alpha0 = 0.170 Structure solution: 0.332 secs 8 Centrosymmetric and 6 non-centrosymmetric space groups evaluated Space group determination: 0.020 secs R1 Rweak Alpha Orientation Space group Flack_x File Formula 0.253 0.124 0.136 as input P2/m neal054_a C56 N26 O12 I3 0.105 0.049 0.094 as input Pm 0.45 neal054_b C51 N29 O7 I2 0.217 0.103 0.144 as input P2 0.38 neal054_c C47 N33 O11 I3 0.098 0.039 0.221 as input P2(1) 0.13 neal054_d C18 N4 O6 I Assign elements and isotropic refinement 0.704 secs ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XT finished at 16:28:04 Total time: 1.483 secs + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++