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|
TITL p1_b.res in P1
p1_b.res
created by SHELXL-2018/3 at 17:47:42 on 28-Feb-2022
REM Old TITL p1 in P1
REM SHELXT solution in P1: R1 0.202, Rweak 0.015, Alpha 0.000
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Flack x = 0.474 ( 0.071 ) from 4327 Parsons' quotients
REM Formula found by SHELXT: C41 O12 F41 Al5
CELL 0.71073 10.3518 10.3854 12.5305 89.044 85.654 81.199
ZERR 14.000 0.0027 0.0024 0.0034 0.006 0.007 0.007
LATT -1
SFAC C O F AL Fe H
UNIT 1 2 3 4 5 6
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 https://doi.org/10.1107/S1600576718004508
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
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
SADI_CCF3 0.02 O1 C1
SADI_CCF3 0.04 F1 C1 F2 C1 F3 C1 F4 C1 F5 C1 F6 C1 F7 C1 F8 C1 F9 C1
SIMU_CCF3 O1 > F9
RIGU_CCF3 O1 > F9
SAME_CCF3 O1 > F9
EADP F3_7 F3_5
SIMU 0.01 0.02 2 O1_5 C1_5 C2_5 F1_5 F2_5 F3_5 C3_5 F4_5 F5_5 F6_5 =
C4_5 F7_5 F8_5 F9_5 O1_7 C1_7 C2_7 F1_7 F2_7 F3_7 C3_7 F4_7 F5_7 F6_7 =
C4_7 F7_7 F8_7 F9_7
SIMU 0.04 0.08 1
TEMP -173.150
L.S. 20
BOND
LIST 4
ACTA
FMAP 2
TWIN
PLAN 20
WGHT 0.179700 4.024700
BASF 0.50152
FVAR 0.64025 0.78287 0.85076 0.01243 0.18094
PART 0
AL1 4 0.676255 0.540147 0.498296 11.00000 0.01195 0.01806 =
0.02057 0.00338 -0.00313 -0.00399
AL2 4 0.606252 0.666314 0.242627 11.00000 0.01634 0.02009 =
0.01179 0.00735 -0.00168 -0.00368
F1 3 0.641362 0.604279 0.368332 11.00000 0.03217 0.02335 =
0.01623 0.00563 -0.00314 -0.00294
RESI CCF3 1
O1 2 0.714063 0.664285 0.572068 11.00000 0.01636 0.03374 =
0.04322 0.00410 -0.01087 -0.00888
C1 1 0.810406 0.717922 0.613915 11.00000 0.01762 0.02126 =
0.01907 -0.00190 -0.00037 -0.00486
C2 1 0.745847 0.836164 0.684140 11.00000 0.01435 0.03314 =
0.03575 -0.00275 0.00351 0.00140
F1 3 0.686334 0.795396 0.773975 11.00000 0.04429 0.04072 =
0.02424 -0.00532 0.00479 -0.01121
F2 3 0.831866 0.910433 0.710607 11.00000 0.03747 0.02638 =
0.03843 -0.01127 -0.00922 -0.00534
F3 3 0.655269 0.911032 0.632681 11.00000 0.03474 0.04136 =
0.03992 -0.00959 -0.01706 0.00320
C3 1 0.902719 0.766021 0.523710 11.00000 0.02962 0.03175 =
0.02646 0.00278 0.00048 -0.00823
F4 3 0.933272 0.673019 0.447579 11.00000 0.05039 0.03740 =
0.02327 -0.00301 0.00550 -0.01784
F5 3 0.847288 0.874713 0.477057 11.00000 0.06125 0.02522 =
0.02807 0.00638 -0.00829 -0.01176
F6 3 1.014785 0.787169 0.560550 11.00000 0.02897 0.04875 =
0.04290 -0.00064 0.00575 -0.01723
C4 1 0.891448 0.614724 0.683499 11.00000 0.01643 0.03595 =
0.02572 0.00411 -0.00485 -0.00305
F7 3 0.979437 0.531433 0.627626 11.00000 0.02018 0.03826 =
0.04391 -0.00542 -0.00528 -0.00032
F8 3 0.954658 0.669427 0.755414 11.00000 0.04208 0.04375 =
0.03556 -0.00878 -0.01477 -0.00615
F9 3 0.813668 0.543864 0.742184 11.00000 0.03719 0.04247 =
0.03033 0.01845 -0.00615 -0.00921
RESI 0
RESI CCF3 2
O1 2 0.528199 0.494925 0.537472 11.00000 0.01913 0.07063 =
0.02097 0.00042 -0.00050 -0.02812
C1 1 0.444943 0.465878 0.619736 11.00000 0.01476 0.05438 =
0.02531 0.00323 0.00034 -0.01835
C2 1 0.397005 0.588470 0.691748 11.00000 0.05611 0.06533 =
0.02159 0.00316 0.00579 -0.03277
F1 3 0.494068 0.596296 0.756560 11.00000 0.06752 0.13183 =
0.01891 -0.01261 0.00372 -0.06941
F2 3 0.286433 0.576693 0.752057 11.00000 0.04434 0.04992 =
0.08185 0.00054 0.02934 -0.00841
F3 3 0.374803 0.695716 0.633318 11.00000 0.06379 0.04997 =
0.04666 0.00779 -0.00043 -0.02466
C3 1 0.323979 0.425270 0.570986 11.00000 0.02829 0.06358 =
0.01549 0.00989 -0.00148 -0.02561
F4 3 0.364390 0.343820 0.489952 11.00000 0.02681 0.06394 =
0.02636 0.00124 -0.00002 -0.02006
F5 3 0.248737 0.528075 0.531481 11.00000 0.03001 0.05400 =
0.03283 0.00907 -0.00435 -0.01900
F6 3 0.257227 0.359743 0.644732 11.00000 0.03946 0.08574 =
0.02124 0.01211 -0.00264 -0.04725
C4 1 0.511513 0.355100 0.689825 11.00000 0.03899 0.07056 =
0.03245 0.00991 -0.00611 -0.02696
F7 3 0.523824 0.241845 0.636195 11.00000 0.03520 0.05314 =
0.03900 0.01801 -0.00411 -0.00760
F8 3 0.441561 0.345685 0.782963 11.00000 0.04269 0.06685 =
0.02693 0.01671 -0.00969 -0.02333
F9 3 0.632911 0.369842 0.708940 11.00000 0.03358 0.07692 =
0.04730 0.00638 -0.01629 -0.01483
RESI 0
RESI CCF3 3
O1 2 0.570768 0.538504 0.169724 11.00000 0.02067 0.01956 =
0.01763 -0.00381 -0.00344 0.00364
C1 1 0.473279 0.488924 0.126829 11.00000 0.02238 0.02668 =
0.02103 0.00311 -0.00596 -0.00294
C2 1 0.540394 0.369293 0.058120 11.00000 0.04065 0.02770 =
0.02188 -0.00578 -0.01328 -0.00823
F1 3 0.598007 0.410739 -0.032117 11.00000 0.02664 0.05880 =
0.03861 -0.01428 0.00719 -0.01015
F2 3 0.453268 0.293929 0.029909 11.00000 0.03523 0.04142 =
0.03451 -0.00574 -0.00529 -0.01413
F3 3 0.630908 0.294801 0.110639 11.00000 0.03488 0.02550 =
0.05465 -0.01129 -0.01541 0.01049
C3 1 0.377322 0.442824 0.216428 11.00000 0.03026 0.02491 =
0.02395 -0.00216 -0.00073 -0.01024
F4 3 0.350217 0.530393 0.292331 11.00000 0.04536 0.03415 =
0.02802 -0.00370 0.01060 -0.00648
F5 3 0.434595 0.333458 0.260669 11.00000 0.05480 0.03310 =
0.03212 0.00919 -0.00284 -0.00984
F6 3 0.266428 0.416278 0.179906 11.00000 0.03083 0.05165 =
0.03797 -0.00137 -0.00013 -0.02121
C4 1 0.394090 0.588765 0.052049 11.00000 0.03102 0.02821 =
0.02351 0.00360 -0.01011 -0.00555
F7 3 0.309150 0.672419 0.112745 11.00000 0.02715 0.02929 =
0.03532 0.00297 -0.01241 0.00600
F8 3 0.326446 0.530487 -0.015933 11.00000 0.03194 0.04427 =
0.02911 0.00636 -0.02014 -0.00749
F9 3 0.475593 0.655396 -0.002519 11.00000 0.03794 0.04003 =
0.03984 0.01519 -0.00554 -0.01364
RESI 0
RESI CCF3 4
O1 2 0.755408 0.704147 0.199544 11.00000 0.02953 0.03512 =
0.01737 0.00394 0.00733 -0.01083
C1 1 0.840210 0.735341 0.118531 11.00000 0.02642 0.03077 =
0.01355 0.00573 0.00417 -0.01106
C2 1 0.959368 0.778136 0.169010 11.00000 0.02188 0.02863 =
0.04271 -0.00063 0.00210 -0.00497
F1 3 1.035642 0.673184 0.205143 11.00000 0.02855 0.04831 =
0.04437 0.00953 -0.00880 0.00668
F2 3 1.036441 0.837272 0.098168 11.00000 0.02254 0.04716 =
0.04838 0.01183 0.00089 -0.01368
F3 3 0.920853 0.862591 0.248429 11.00000 0.04279 0.04677 =
0.03493 -0.00569 -0.00644 -0.02309
C3 1 0.772752 0.846481 0.050322 11.00000 0.02550 0.03800 =
0.02935 0.01215 0.00165 -0.00183
F4 3 0.652782 0.827834 0.033002 11.00000 0.02177 0.06727 =
0.03654 0.01738 -0.00737 -0.00987
F5 3 0.771138 0.963008 0.100550 11.00000 0.06399 0.03112 =
0.07836 0.00466 0.01237 0.00494
F6 3 0.836629 0.857067 -0.048273 11.00000 0.04174 0.07697 =
0.02435 0.02172 0.00071 -0.02263
C4 1 0.887406 0.614116 0.044509 11.00000 0.03775 0.03396 =
0.03314 -0.00698 0.00305 -0.00592
F7 3 0.794442 0.593535 -0.020602 11.00000 0.05047 0.05477 =
0.03753 -0.01834 -0.00015 -0.02082
F8 3 0.995108 0.628501 -0.015540 11.00000 0.04620 0.07226 =
0.01759 -0.00836 0.00919 -0.01621
F9 3 0.916011 0.508565 0.106900 11.00000 0.08447 0.02987 =
0.05338 0.00286 -0.00120 -0.00643
RESI 0
RESI CCF3 5
PART 1 21
O1 2 0.805436 0.417680 0.480282 21.00000 0.01617 0.02902 =
0.04051 -0.00057 -0.00501 -0.00848
C1 1 0.870172 0.306241 0.436705 21.00000 0.01678 0.02486 =
0.03688 0.00444 -0.00942 -0.00222
C2 1 0.790938 0.256558 0.349535 21.00000 0.02979 0.02843 =
0.05540 -0.00613 -0.01510 0.00133
F1 3 0.797993 0.329485 0.260670 21.00000 0.06129 0.05459 =
0.04375 -0.00258 -0.03103 0.01225
F2 3 0.821993 0.131073 0.325923 21.00000 0.04138 0.02714 =
0.07519 -0.02006 -0.01817 -0.00718
F3 3 0.661389 0.277839 0.378488 21.00000 0.02263 0.04305 =
0.08012 -0.01751 -0.02562 -0.00805
C3 1 0.882669 0.201572 0.526042 21.00000 0.03472 0.03163 =
0.04527 0.00788 -0.00133 -0.00286
F4 3 0.919357 0.249828 0.615100 21.00000 0.06367 0.04503 =
0.02856 0.01515 -0.00419 0.00006
F5 3 0.770299 0.159049 0.551924 21.00000 0.05043 0.03533 =
0.07223 0.00581 0.02180 -0.01786
F6 3 0.978429 0.105115 0.498319 21.00000 0.05100 0.03230 =
0.05691 0.01481 -0.00367 0.01870
C4 1 1.004311 0.329250 0.382702 21.00000 0.02759 0.03875 =
0.03505 -0.00563 -0.00004 -0.01116
F7 3 1.089889 0.335783 0.456585 21.00000 0.01492 0.07692 =
0.05578 -0.02069 -0.00518 -0.01932
F8 3 1.060765 0.233506 0.317207 21.00000 0.03107 0.05020 =
0.04384 -0.01155 0.01194 -0.00103
F9 3 0.991010 0.439753 0.327872 21.00000 0.07451 0.03912 =
0.03552 -0.00384 0.00686 -0.03119
PART 0
RESI 0
RESI CCF3 6
O1 2 0.476540 0.786614 0.257463 11.00000 0.03170 0.01009 =
0.04463 -0.00467 -0.01666 0.00958
C1 1 0.417349 0.901172 0.303270 11.00000 0.01726 0.01379 =
0.02951 -0.00094 -0.00333 0.00185
C2 1 0.499010 0.948120 0.389634 11.00000 0.03041 0.04236 =
0.07488 -0.02665 -0.02058 -0.00096
F1 3 0.486501 0.876362 0.477801 11.00000 0.10170 0.07032 =
0.05904 -0.00705 -0.05338 0.00807
F2 3 0.454218 1.073233 0.415258 11.00000 0.04660 0.04268 =
0.07138 -0.02762 -0.01119 0.00013
F3 3 0.623132 0.939045 0.351835 11.00000 0.02965 0.07688 =
0.15616 -0.05442 -0.00657 -0.01142
C3 1 0.389439 1.004653 0.214251 11.00000 0.07947 0.02205 =
0.03803 0.01021 0.00580 0.01839
F4 3 0.353204 0.950470 0.129757 11.00000 0.14387 0.05378 =
0.03706 -0.00128 -0.03061 0.03923
F5 3 0.503259 1.051389 0.188526 11.00000 0.11029 0.02970 =
0.11413 0.01241 0.06240 -0.00070
F6 3 0.302324 1.107305 0.243172 11.00000 0.06208 0.02729 =
0.06038 -0.00443 -0.02116 0.01853
C4 1 0.279929 0.879289 0.355081 11.00000 0.02494 0.04587 =
0.05070 -0.00317 -0.00366 -0.01185
F7 3 0.198046 0.880415 0.278166 11.00000 0.03240 0.09050 =
0.08510 -0.03422 -0.02351 0.00610
F8 3 0.231486 0.975516 0.423724 11.00000 0.04219 0.05950 =
0.06647 -0.01872 0.01073 -0.00651
F9 3 0.287583 0.767147 0.406567 11.00000 0.07779 0.04593 =
0.08252 0.01115 0.02988 -0.02030
RESI 0
RESI CCF3 7
PART 2 -21
O1 2 0.805115 0.418797 0.492874 -21.00000 0.01768 0.02593 =
0.03175 0.00304 -0.00586 -0.00741
C1 1 0.868606 0.307101 0.447791 -21.00000 0.02180 0.02887 =
0.03897 0.00035 -0.00851 -0.00398
C2 1 0.768174 0.234538 0.396331 -21.00000 0.02738 0.03172 =
0.05128 -0.00952 -0.01324 -0.00207
F1 3 0.702671 0.171807 0.468862 -21.00000 0.03069 0.03488 =
0.06874 -0.01113 -0.00950 -0.01269
F2 3 0.827752 0.154540 0.319507 -21.00000 0.04393 0.04193 =
0.05448 -0.01225 -0.00878 -0.00233
F3 3 0.679528 0.319016 0.350050 -21.00000 0.02263 0.04305 =
0.08012 -0.01751 -0.02562 -0.00805
C3 1 0.973187 0.340534 0.360799 -21.00000 0.03370 0.03754 =
0.04239 -0.00149 0.00449 -0.00401
F4 3 1.051481 0.416179 0.401818 -21.00000 0.04443 0.04295 =
0.05596 -0.00354 0.01973 -0.02347
F5 3 0.911201 0.401769 0.280243 -21.00000 0.06783 0.05722 =
0.05220 0.01167 0.00051 -0.00126
F6 3 1.048991 0.233952 0.321762 -21.00000 0.04148 0.04264 =
0.04118 -0.00462 0.01069 -0.00642
C4 1 0.936685 0.219156 0.534633 -21.00000 0.02751 0.02588 =
0.04262 0.00358 -0.01216 -0.00390
F7 3 1.042535 0.261525 0.563373 -21.00000 0.02895 0.02457 =
0.05360 -0.00320 -0.02541 0.00263
F8 3 0.966592 0.095537 0.501521 -21.00000 0.02782 0.01680 =
0.05441 0.01257 -0.00126 -0.01017
F9 3 0.853353 0.214230 0.620853 -21.00000 0.05268 0.03630 =
0.04653 0.01990 -0.00184 0.00571
PART 0
RESI 0
RESI NBZ2 8
PART 1 11
C1 1 -0.071342 0.270732 0.883709 11.00000 0.02547 0.03813 =
0.05318 -0.00140 0.00432 0.00902
AFIX 43
H1 6 -0.141587 0.285368 0.838244 11.00000 -1.20000
AFIX 0
C2 1 0.047475 0.317251 0.854354 11.00000 0.02097 0.05775 =
0.07194 0.03956 0.01160 0.01284
AFIX 43
H2 6 0.054367 0.369965 0.792105 11.00000 -1.20000
AFIX 0
C3 1 0.153956 0.286933 0.915215 11.00000 0.05011 0.04476 =
0.07111 0.01368 -0.02208 -0.02752
AFIX 43
H3 6 0.237024 0.308462 0.890334 11.00000 -1.20000
AFIX 0
C4 1 0.138090 0.224555 1.013285 11.00000 0.07170 0.04904 =
0.04531 -0.00870 -0.02278 -0.00584
AFIX 43
H4 6 0.207164 0.214218 1.059949 11.00000 -1.20000
AFIX 0
C5 1 0.021955 0.177030 1.043874 11.00000 0.09705 0.04407 =
0.01886 -0.00007 0.02011 -0.00458
AFIX 43
H5 6 0.015152 0.127162 1.107745 11.00000 -1.20000
AFIX 0
C6 1 -0.084971 0.202937 0.980187 11.00000 0.03233 0.04518 =
0.07464 0.00516 0.03721 0.00861
AFIX 43
H6 6 -0.165863 0.174649 1.002455 11.00000 -1.20000
AFIX 0
C7 1 0.351198 -0.049084 0.861454 11.00000 0.04865 0.08204 =
0.06725 0.00597 -0.02245 -0.00360
AFIX 43
H7 6 0.419024 -0.054287 0.909058 11.00000 -1.20000
AFIX 0
C8 1 0.238555 -0.103626 0.887886 11.00000 0.06707 0.04665 =
0.02400 0.00553 0.00201 -0.00047
AFIX 43
H8 6 0.232902 -0.151581 0.952861 11.00000 -1.20000
AFIX 0
C9 1 0.135447 -0.091406 0.824601 11.00000 0.03184 0.03164 =
0.05167 -0.00204 0.00497 -0.00750
AFIX 43
H9 6 0.061869 -0.134198 0.842549 11.00000 -1.20000
AFIX 0
C10 1 0.141747 -0.013543 0.732163 11.00000 0.07610 0.05129 =
0.06388 0.02139 -0.04473 -0.02790
AFIX 43
H10 6 0.065816 0.010607 0.693965 11.00000 -1.20000
AFIX 0
C11 1 0.258444 0.028023 0.696679 11.00000 0.08409 0.02815 =
0.04145 0.00748 0.00941 0.00864
AFIX 43
H11 6 0.268296 0.066253 0.627710 11.00000 -1.20000
AFIX 0
C12 1 0.361158 0.012971 0.763561 11.00000 0.06017 0.03458 =
0.07969 0.00270 0.00407 -0.01922
AFIX 43
H12 6 0.439613 0.046035 0.741418 11.00000 -1.20000
PART 0
AFIX 0
HKLF 4
REM p1_b.res in P1
REM wR2 = 0.3334, GooF = S = 1.084, Restrained GooF = 1.030 for all data
REM R1 = 0.1174 for 15498 Fo > 4sig(Fo) and 0.1485 for all 20895 data
REM 1026 parameters refined using 8499 restraints
END
WGHT 0.1804 3.9470
REM Highest difference peak 7.753, deepest hole -2.943, 1-sigma level 0.180
Q1 1 0.0187 0.1371 0.8809 11.00000 0.05 7.75
Q2 1 0.2631 0.0729 0.8602 11.00000 0.05 7.41
Q3 1 0.1371 0.0424 0.8332 11.00000 0.05 3.17
Q4 1 0.1490 0.1651 0.9108 11.00000 0.05 3.02
Q5 1 0.4379 0.0900 0.8950 11.00000 0.05 1.52
Q6 1 -0.1508 0.1184 0.8452 11.00000 0.05 1.52
Q7 1 -0.0433 0.2739 1.0345 11.00000 0.05 1.23
Q8 1 0.3247 -0.1452 0.8020 11.00000 0.05 1.23
Q9 1 -0.0439 0.3555 0.9377 11.00000 0.05 1.19
Q10 1 0.3920 0.3194 0.5872 11.00000 0.05 1.11
Q11 1 0.3249 -0.0589 0.7046 11.00000 0.05 1.05
Q12 1 0.8902 0.8855 0.1540 11.00000 0.05 1.04
Q13 1 0.4029 0.6589 0.5859 11.00000 0.05 1.01
Q14 1 0.7768 0.7737 0.0136 11.00000 0.05 0.99
Q15 1 0.1946 0.1594 0.9724 11.00000 0.05 0.98
Q16 1 1.0210 0.6461 0.0514 11.00000 0.05 0.98
Q17 1 0.0927 0.0440 0.7657 11.00000 0.05 0.95
Q18 1 0.8813 0.5480 0.1563 11.00000 0.05 0.94
Q19 1 -0.2555 0.1251 0.8443 11.00000 0.05 0.89
Q20 1 0.5393 0.0853 0.8951 11.00000 0.05 0.88
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