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|
TITL p21c in P2(1)/c
created by SHELXL-2018/3 at 16:18:25 on 03-May-2018
CELL 0.71073 10.5086 20.9035 20.5072 90 94.13 90
ZERR 4 0.0003 0.0005 0.0005 0 0.001 0
LATT 1
SYMM -X, 0.5+Y, 0.5-Z
SFAC C H O F Al Ga
UNIT 1 2 3 4 5 6
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
PLAN 20
TEMP -173.18
ACTA 45
SIZE 0.12 0.23 0.33
DELU 0.04
BOND_* $H
fmap 2
REM Restraints for Fragment oc(cf3)3, Nonafluoro-tert-butoxy, [(CF3)3CO]- REM =
from: TURBOMOLE V6.0 B-P86/def-SV(P). Please cite
REM doi:10.1107/S1600576715005580
SADI_CCF3 0.02 C1 C2 C1 C3 C1 C4
SADI_CCF3 0.02 F1 C2 F2 C2 F3 C2 F4 C3 F5 C3 F6 C3 F7 C4 F8 C4 F9 C4
DEFS 0.0234 0.123 0.0123 0.0456 1.23
SADI_CCF3 0.04 C2 C3 C3 C4 C2 C4
SADI_CCF3 0.04 O1 C2 O1 C3 O1 C4
SADI_CCF3 0.04 F1 F2 F2 F3 F3 F1 F4 F5 F5 F6 F6 F4 F7 F8 F8 F9 F9 F7
DFIX_CCF3 1.44 0.02 O1 C1
SADI_CCF3 0.1 F1 C1 F2 C1 F3 C1 F4 C1 F5 C1 F6 C1 F7 C1 F8 C1 F9 C1
SIMU_CCF3 O1 > F9
RIGU_* O1 > F9
SAME_CCF3 O1 > F9
REM For further cards:
WGHT 0.049 0.0
FVAR 0.08684 0.48096 0.55764
RESI 4 CCF3
PART 2 -31
O1 3 0.074835 0.238436 0.402457 -31.00000 0.01579 0.03095 =
0.01852 -0.00468 -0.00210 0.01153
C1 1 0.028576 0.234542 0.337234 -31.00000 0.02311 0.03617 =
0.01096 -0.01000 0.00201 0.00356
C2 1 0.121540 0.194460 0.298291 -31.00000 0.02960 0.04586 =
0.01555 -0.00485 -0.00023 0.01102
F1 4 0.241900 0.211233 0.314197 -31.00000 0.02029 0.06494 =
0.02841 -0.00285 0.00512 0.01642
F2 4 0.098797 0.200975 0.234210 -31.00000 0.03990 0.07427 =
0.01638 -0.00978 0.00426 0.01510
F3 4 0.112375 0.132048 0.311380 -31.00000 0.05736 0.03839 =
0.03444 -0.00580 0.00169 0.01890
C3 1 -0.103502 0.202241 0.332346 -31.00000 0.02864 0.06150 =
0.01464 -0.00621 -0.00347 -0.00667
F4 4 -0.194239 0.242467 0.347077 -31.00000 0.01934 0.08422 =
0.03135 -0.01447 -0.00634 0.00704
F5 4 -0.106378 0.152755 0.373514 -31.00000 0.05083 0.07303 =
0.05196 0.01867 -0.01209 -0.02261
F6 4 -0.132107 0.178669 0.272635 -31.00000 0.03544 0.08301 =
0.02571 -0.02102 -0.00635 -0.01918
C4 1 0.018702 0.302508 0.307595 -31.00000 0.04608 0.04134 =
0.01911 -0.00021 -0.00914 0.00573
F7 4 -0.033689 0.340543 0.350061 -31.00000 0.06375 0.04441 =
0.03864 -0.00811 -0.01437 0.02588
F8 4 -0.057354 0.300876 0.252663 -31.00000 0.07921 0.07333 =
0.03022 0.00207 -0.02887 0.02608
F9 4 0.130286 0.325479 0.293388 -31.00000 0.06204 0.04346 =
0.03540 0.00835 -0.00140 -0.01178
PART 0
RESI 0
REM REM DSR PUT OC(CF3)3 WITH O1 C1 C4 ON O1_3A C1_3A Q6 PART 2 OCC -31
REM
GA1 6 0.639514 0.561736 0.237758 11.00000 0.02411 0.02509 =
0.02492 0.00001 -0.00158 0.00159
AL1 5 0.064280 0.260190 0.478723 11.00000 0.01606 0.01976 =
0.01375 -0.00004 -0.00222 0.00123
O1 3 0.120468 0.336570 0.494134 11.00000 0.01597 0.02185 =
0.02314 -0.00117 -0.00224 -0.00158
O2 3 -0.097347 0.260917 0.489316 11.00000 0.01699 0.02604 =
0.01664 -0.00417 0.00042 0.00073
F10 4 -0.362557 0.278255 0.447769 11.00000 0.02264 0.04202 =
0.02730 0.00098 -0.01012 0.00187
F11 4 -0.404368 0.257817 0.547035 11.00000 0.02061 0.04886 =
0.03559 -0.00164 0.00539 -0.00228
F12 4 -0.301423 0.189573 0.492527 11.00000 0.02693 0.02714 =
0.04242 -0.00400 -0.00182 -0.00533
F13 4 -0.175185 0.202425 0.610083 11.00000 0.04034 0.04367 =
0.02847 0.01315 0.00119 0.00375
F14 4 -0.031515 0.275544 0.616640 11.00000 0.02289 0.05767 =
0.02211 -0.00627 -0.00814 0.00752
F15 4 -0.222344 0.297022 0.641449 11.00000 0.03254 0.06814 =
0.01963 -0.00711 0.00369 0.01577
F16 4 -0.313279 0.377295 0.540567 11.00000 0.02355 0.03306 =
0.04461 -0.00662 -0.00018 0.00941
F17 4 -0.189445 0.376059 0.461252 11.00000 0.04568 0.02832 =
0.03495 0.00596 0.00448 0.00190
F18 4 -0.110397 0.386665 0.560069 11.00000 0.02682 0.03303 =
0.04593 -0.01526 -0.00145 -0.00434
C5 1 -0.187320 0.282849 0.527509 11.00000 0.01750 0.02237 =
0.01766 -0.00027 -0.00199 0.00127
C6 1 -0.315961 0.251666 0.503981 11.00000 0.02208 0.02832 =
0.02383 0.00048 0.00090 0.00066
C7 1 -0.154317 0.264427 0.600368 11.00000 0.02017 0.03750 =
0.02244 -0.00181 -0.00026 0.00595
C8 1 -0.201067 0.356753 0.522179 11.00000 0.02167 0.02902 =
0.02941 -0.00589 0.00037 0.00036
C1 1 0.223141 0.375178 0.503818 11.00000 0.01566 0.02218 =
0.02107 0.00104 -0.00348 -0.00053
C2 1 0.325780 0.359141 0.456111 11.00000 0.02157 0.02862 =
0.03027 -0.00071 -0.00038 -0.00059
F1 4 0.290691 0.379726 0.395764 11.00000 0.03935 0.04638 =
0.02531 0.00200 0.00756 -0.00333
F2 4 0.342782 0.296341 0.451995 11.00000 0.02510 0.03091 =
0.04948 -0.00953 0.00443 0.00466
F3 4 0.439101 0.385304 0.473512 11.00000 0.01753 0.04352 =
0.05141 -0.00541 0.00373 -0.00643
C3 1 0.178857 0.445109 0.492599 11.00000 0.02224 0.02551 =
0.02731 0.00167 -0.00198 -0.00082
F4 4 0.100281 0.449627 0.439087 11.00000 0.03711 0.03268 =
0.03461 0.00785 -0.01233 0.00734
F5 4 0.116027 0.466251 0.542724 11.00000 0.03130 0.02827 =
0.03900 -0.00871 0.00248 0.00370
F6 4 0.276150 0.485252 0.485742 11.00000 0.03305 0.02487 =
0.04651 0.00510 0.00086 -0.00680
C4 1 0.282165 0.368631 0.575532 11.00000 0.02737 0.02972 =
0.02611 0.00062 -0.00753 -0.00361
F7 4 0.358325 0.417829 0.593767 11.00000 0.03452 0.03946 =
0.03401 -0.00363 -0.01521 -0.00994
F8 4 0.351893 0.315205 0.582802 11.00000 0.03637 0.03413 =
0.04113 0.00793 -0.02042 0.00474
F9 4 0.192067 0.365522 0.617269 11.00000 0.04146 0.05393 =
0.02012 0.00219 0.00002 -0.00935
C34 1 0.369705 0.548727 0.213197 11.00000 0.01997 0.02249 =
0.03076 -0.00483 -0.00288 0.00111
AFIX 43
H34 2 0.340371 0.506496 0.203858 11.00000 -1.20000
AFIX 0
C33 1 0.380570 0.569531 0.277905 11.00000 0.01595 0.03247 =
0.02434 0.00125 -0.00203 0.00419
C32 1 0.425169 0.631358 0.290541 11.00000 0.01542 0.03211 =
0.02656 -0.00928 -0.00400 0.00558
AFIX 43
H32 2 0.435581 0.645812 0.334521 11.00000 -1.20000
AFIX 0
C35 1 0.400682 0.588146 0.161619 11.00000 0.01783 0.02846 =
0.02230 -0.00167 -0.00586 0.00291
C30 1 0.443761 0.649857 0.176365 11.00000 0.02024 0.02432 =
0.02616 0.00450 -0.00253 0.00413
AFIX 43
H30 2 0.466096 0.677175 0.141971 11.00000 -1.20000
AFIX 0
C36 1 0.383703 0.565136 0.092080 11.00000 0.04290 0.03599 =
0.02255 -0.00270 -0.00386 0.00018
AFIX 137
H36A 2 0.294850 0.571445 0.075385 11.00000 -1.50000
H36B 2 0.405081 0.519563 0.090358 11.00000 -1.50000
H36C 2 0.440111 0.589402 0.065167 11.00000 -1.50000
AFIX 0
C31 1 0.454829 0.672447 0.240679 11.00000 0.01654 0.02494 =
0.03573 -0.00430 -0.00382 0.00409
C37 1 0.341150 0.527440 0.332522 11.00000 0.02655 0.04346 =
0.02844 0.00164 0.00199 -0.00430
AFIX 137
H37A 2 0.409001 0.526870 0.367900 11.00000 -1.50000
H37B 2 0.326196 0.483861 0.316092 11.00000 -1.50000
H37C 2 0.262597 0.544192 0.349121 11.00000 -1.50000
AFIX 0
C38 1 0.494303 0.740496 0.255560 11.00000 0.03639 0.02792 =
0.04823 -0.00738 -0.00692 -0.00106
AFIX 137
H38A 2 0.530222 0.759352 0.217171 11.00000 -1.50000
H38B 2 0.558658 0.741083 0.292597 11.00000 -1.50000
H38C 2 0.419702 0.765312 0.266591 11.00000 -1.50000
AFIX 0
C21 1 0.721945 0.447951 0.167553 11.00000 0.02895 0.02285 =
0.02620 -0.00348 -0.00155 0.00708
C20 1 0.838299 0.474760 0.190372 11.00000 0.02345 0.03004 =
0.02891 0.00413 0.00469 0.00693
AFIX 43
H20 2 0.894192 0.490747 0.159810 11.00000 -1.20000
AFIX 0
C23 1 0.673436 0.429169 0.280515 11.00000 0.03009 0.01943 =
0.02962 0.00333 0.00332 0.00506
C25 1 0.874370 0.478621 0.256916 11.00000 0.01974 0.02796 =
0.03492 0.00298 -0.00733 0.00372
C22 1 0.641003 0.425688 0.213103 11.00000 0.02678 0.02173 =
0.03419 -0.00073 -0.00335 0.00181
AFIX 43
H22 2 0.561283 0.407559 0.198146 11.00000 -1.20000
AFIX 0
C28 1 0.685659 0.443539 0.095306 11.00000 0.05026 0.03684 =
0.02582 -0.00655 -0.00448 0.00290
AFIX 137
H28A 2 0.672270 0.486648 0.077319 11.00000 -1.50000
H28B 2 0.606834 0.418689 0.088044 11.00000 -1.50000
H28C 2 0.754260 0.422411 0.073537 11.00000 -1.50000
AFIX 0
C27 1 0.588439 0.401777 0.328925 11.00000 0.04256 0.04062 =
0.03932 0.00850 0.00633 -0.00200
AFIX 137
H27A 2 0.582501 0.431808 0.365277 11.00000 -1.50000
H27B 2 0.623930 0.361114 0.345619 11.00000 -1.50000
H27C 2 0.503219 0.394469 0.307585 11.00000 -1.50000
AFIX 0
C24 1 0.790626 0.456427 0.301107 11.00000 0.03211 0.02719 =
0.02314 0.00019 -0.00474 0.00905
AFIX 43
H24 2 0.813754 0.459897 0.346612 11.00000 -1.20000
AFIX 0
C26 1 1.002704 0.505424 0.281377 11.00000 0.02883 0.06245 =
0.05045 0.00721 -0.01299 -0.00249
AFIX 137
H26A 2 1.045619 0.523155 0.244543 11.00000 -1.50000
H26B 2 1.055140 0.471226 0.302028 11.00000 -1.50000
H26C 2 0.990520 0.539262 0.313413 11.00000 -1.50000
AFIX 0
RESI 1 CCF3
PART 1 21
O1 3 0.157034 0.209303 0.526987 21.00000 0.02290 0.01854 =
0.02024 -0.00272 0.00061 0.00702
C1 1 0.198924 0.149501 0.543934 21.00000 0.02042 0.01328 =
0.02551 0.00269 -0.00452 -0.00369
C2 1 0.283495 0.124820 0.490346 21.00000 0.04415 0.02527 =
0.02880 0.00167 -0.00040 0.00879
F1 4 0.356079 0.075059 0.510660 21.00000 0.04680 0.02795 =
0.02756 -0.00401 -0.00109 0.01257
F2 4 0.359587 0.170574 0.471352 21.00000 0.03966 0.03647 =
0.04562 0.00742 0.01860 0.01182
F3 4 0.212190 0.104131 0.438109 21.00000 0.07988 0.03917 =
0.02893 -0.01179 -0.02107 0.02432
C3 1 0.086376 0.103363 0.549724 21.00000 0.02202 0.03151 =
0.06369 0.01467 -0.00611 0.00072
F4 4 0.116692 0.041286 0.547341 21.00000 0.03274 0.02737 =
0.10682 0.02075 -0.00839 -0.00194
F5 4 -0.004988 0.114179 0.502041 21.00000 0.03129 0.03553 =
0.09741 0.00895 -0.03336 -0.00876
F6 4 0.032538 0.113014 0.606758 21.00000 0.04067 0.05287 =
0.08384 0.03216 0.03070 0.00247
C4 1 0.280608 0.152857 0.609877 21.00000 0.03663 0.02719 =
0.02397 0.00616 -0.00710 0.00764
F7 4 0.222275 0.187998 0.652487 21.00000 0.06647 0.04863 =
0.01636 0.00446 -0.00456 0.02286
F8 4 0.298250 0.094450 0.636824 21.00000 0.04968 0.03156 =
0.02767 0.01224 -0.00834 0.01310
F9 4 0.394933 0.177213 0.602431 21.00000 0.02826 0.03939 =
0.04497 -0.00388 -0.01890 0.00193
PART 0
RESI 0
RESI 2 CCF3
PART 2 -21
O1 3 0.142141 0.207281 0.533641 -21.00000 0.02290 0.02740 =
0.01053 0.00720 0.00036 0.00563
C1 1 0.182648 0.146456 0.545549 -21.00000 0.01893 0.02594 =
0.02031 -0.00019 -0.00484 0.00936
C2 1 0.192984 0.140449 0.621265 -21.00000 0.04315 0.02747 =
0.02385 0.00686 -0.00757 0.00126
F1 4 0.245205 0.192674 0.649231 -21.00000 0.05143 0.03826 =
0.03193 -0.00579 -0.01865 -0.00485
F2 4 0.264027 0.090306 0.642441 -21.00000 0.06073 0.04450 =
0.03972 0.01630 -0.01260 0.01460
F3 4 0.078582 0.131920 0.643529 -21.00000 0.05691 0.04955 =
0.03374 0.01040 0.01881 0.00375
C3 1 0.091542 0.095062 0.515334 -21.00000 0.02780 0.03105 =
0.03622 0.00015 -0.00420 0.00231
F4 4 0.107933 0.085470 0.452542 -21.00000 0.05359 0.03858 =
0.03371 -0.01253 -0.00959 0.00645
F5 4 -0.029902 0.112024 0.519910 -21.00000 0.02234 0.04392 =
0.06318 -0.00456 -0.00580 -0.00361
F6 4 0.109352 0.039100 0.546088 -21.00000 0.05363 0.02466 =
0.04643 -0.00160 -0.00624 -0.00337
C4 1 0.316387 0.137078 0.519902 -21.00000 0.03116 0.02615 =
0.05093 0.00984 0.00709 0.00398
F7 4 0.319119 0.157467 0.458245 -21.00000 0.04376 0.04441 =
0.04485 0.01680 0.01959 0.01340
F8 4 0.353688 0.075732 0.521565 -21.00000 0.02966 0.03601 =
0.05482 0.01221 0.00815 0.02092
F9 4 0.405819 0.168092 0.556659 -21.00000 0.02247 0.03769 =
0.09070 0.00429 -0.00681 -0.00325
PART 0
RESI 0
RESI 3 CF3
PART 1 31
O1 3 0.087763 0.232808 0.398354 31.00000 0.01707 0.02924 =
0.00692 -0.00661 0.00156 0.00658
C1 1 0.036610 0.231570 0.336510 31.00000 0.01434 0.02998 =
0.01797 0.00134 -0.00911 0.00584
C2 1 0.150502 0.233262 0.294438 31.00000 0.03946 0.03987 =
0.01789 -0.00400 -0.00262 0.00844
F1 4 0.122782 0.211275 0.232658 31.00000 0.03961 0.06075 =
0.01181 -0.00492 0.00173 0.00327
F2 4 0.246159 0.194445 0.319696 31.00000 0.02778 0.05311 =
0.02912 -0.00355 -0.00327 0.01729
F3 4 0.196682 0.292032 0.290371 31.00000 0.04403 0.04759 =
0.02854 0.00203 0.00562 -0.01235
C3 1 -0.052849 0.288661 0.318395 31.00000 0.03382 0.03990 =
0.02033 -0.00385 -0.00609 0.01178
F4 4 -0.005258 0.342945 0.346650 31.00000 0.04999 0.02714 =
0.02833 -0.00376 -0.01206 0.01276
F5 4 -0.067147 0.301053 0.253782 31.00000 0.04179 0.03970 =
0.01625 0.00060 -0.00415 0.01292
F6 4 -0.169084 0.279883 0.339273 31.00000 0.02378 0.06496 =
0.03144 0.00001 -0.00463 0.01704
C4 1 -0.039299 0.168627 0.325762 31.00000 0.03270 0.04277 =
0.02352 -0.00208 -0.01140 -0.00496
F7 4 -0.114803 0.157982 0.372858 31.00000 0.02849 0.05143 =
0.02641 -0.00326 0.00129 -0.01742
F8 4 -0.112445 0.168653 0.268184 31.00000 0.05470 0.04945 =
0.02846 0.00086 -0.02237 -0.00846
F9 4 0.041330 0.118693 0.324876 31.00000 0.05446 0.03222 =
0.03789 -0.00744 -0.01048 0.00542
RESI 0
PART 0
HKLF 4
REM p21c in P2(1)/c
REM wR2 = 0.1005, GooF = S = 1.016, Restrained GooF = 0.950 for all data
REM R1 = 0.0400 for 7085 Fo > 4sig(Fo) and 0.0794 for all 10786 data
REM 945 parameters refined using 1842 restraints
END
WGHT 0.0491 0.0000
REM Highest difference peak 0.407, deepest hole -0.691, 1-sigma level 0.073
Q1 1 0.6917 0.6019 0.2177 11.00000 0.04 0.41
Q2 1 0.7505 0.5648 0.2191 11.00000 0.04 0.36
Q3 1 0.6807 0.5284 0.2072 11.00000 0.04 0.36
Q4 1 0.7404 0.4707 0.0667 11.00000 0.04 0.34
Q5 1 0.2757 0.3719 0.4871 11.00000 0.04 0.33
Q6 1 0.6861 0.3929 0.0902 11.00000 0.04 0.33
Q7 1 0.5916 0.5882 0.2738 11.00000 0.04 0.32
Q8 1 0.6394 0.4371 0.3133 11.00000 0.04 0.31
Q9 1 -0.1805 0.3161 0.5155 11.00000 0.04 0.31
Q10 1 0.1831 0.3570 0.4989 11.00000 0.04 0.31
Q11 1 -0.1286 0.2541 0.4775 11.00000 0.04 0.30
Q12 1 0.5863 0.6686 0.2340 11.00000 0.04 0.30
Q13 1 0.5935 0.5392 0.2790 11.00000 0.04 0.30
Q14 1 0.1384 0.3035 0.4745 11.00000 0.04 0.30
Q15 1 -0.1350 0.2675 0.5111 11.00000 0.04 0.30
Q16 1 0.5875 0.5160 0.2605 11.00000 0.04 0.29
Q17 1 0.3483 0.5661 0.2460 11.00000 0.04 0.29
Q18 1 0.8796 0.5411 0.3471 11.00000 0.04 0.28
Q19 1 -0.1711 0.2796 0.5594 11.00000 0.04 0.28
Q20 1 -0.1122 0.2225 0.4997 11.00000 0.04 0.27
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