# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012
data_General
_journal_name_full 'Dalton Trans.'
_journal_coden_cambridge 0222
#TrackingRef '- wt1945w-shelxl-revised.cif'
_audit_creation_date 2012-May-10
_audit_creation_method SHELXL97
_audit_update_record
;
2012-May-10 # Formatted by publCIF
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#==============================================================================
# PROCESSING SUMMARY (IUCr Office Use Only)
_journal_date_recd_electronic ?
_journal_date_from_coeditor ?
_journal_date_accepted ?
_journal_coeditor_code ?
#==============================================================================
# SUBMISSION DETAILS
_publ_contact_author_name 'Professor V.W.W. YAM'
_publ_contact_author_email wwyam@hku.hk
_publ_contact_author_fax '(852)2915 5176'
_publ_contact_author_phone '(852)2859 2153'
_publ_contact_author_address
;
Department of Chemistry
The University of Hong Kong
Pokfulam Road, Pokfulam,
Hong Kong SAR,
P. R. CHINA
;
_publ_contact_letter
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ENTER TEXT OF LETTER
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_publ_requested_category ? #'CHOOSE FI FM FO CI CM CO or AD'
_publ_requested_coeditor_name ?
#==============================================================================
# TITLE AND AUTHOR LIST
_publ_section_title
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Directory Reference: COM648 wt1945w-YAM-AT315_Anthony Tam_20-Oct-2009
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_publ_section_title_footnote .
loop_
_publ_author_name
_publ_author_footnote
_publ_author_address
E.S.-H.Lam .
;
Department of Chemistry
The University of Hong Kong
Pokfulam Road, Pokfulam,
Hong Kong SAR,
P. R. CHINA
;
A.Y.-Y.Tam .
;
Department of Chemistry
The University of Hong Kong
Pokfulam Road, Pokfulam,
Hong Kong SAR,
P. R. CHINA
;
V.W.-W.Yam .
;
Department of Chemistry
The University of Hong Kong
Pokfulam Road, Pokfulam,
Hong Kong SAR,
P. R. CHINA
;
_publ_section_synopsis .
#==============================================================================
# TEXT
_publ_section_abstract
;
(type here to add abstract)
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_publ_section_comment
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The compound, [C~96~H~82~AgN~10~O~3~Pt~2~]^+^ [CF~3~O~3~S]^-^, was
recrystallized in centrosymmetric primitive triclinic space group,
P-1 (#2). There are two molecules in the unit cell.
In the compound, .
;
_publ_section_references
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Bruker AXS Inc. (1998). SMART version 5.059, Madison, Wisconsin, USA.
Bruker AXS Inc. (2006). SAINT, version 7.34A, Madison, Wisconsin, USA.
Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P.,
Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A.
(2008). Mercury J. Appl. Cryst, 41, 466--470.
Sheldrick, G. M. (2004). SADABS, G\"ottingen University, G\"ottingen,
Germany.
Sheldrick, G. M. (2008). SHELX programs:SHELXL97 &
SHELXS97. Acta Cryst. E64, 112-122.
;
_publ_section_acknowledgements
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_publ_section_figure_captions
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Fig. 1. The compound was shown at 20% probability thermal ellipsoids with the
atom numbering scheme. (Only major components were shown)
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_publ_section_exptl_prep
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A yellow block crystal of, [C~96~H~82~Ag N~10~Pt~2~]^+^ [CF~3~O~3~S]^-^,
having approximate dimensions of 0.39 x 0.42 x 0.49 mm was mounted
in glass capillary. All measurements were made on a Bruker SMART 1000 CCD
detector with graphite monochromated Mo---K\a radiation. The
crystal-to-detector distance was 50.00 mm.
Indexing was performed from 60 images that were exposed for 10 s for a
preliminary unit cell determination. Of which, 196 out of total of 264
reflections were successfully indexed. The crystal-to-detector distance was
50.00 mm.
Cell constants and an orientation matrix for data collection corresponded to a
primitive triclinic cell with dimensions: a = 14.002(2)\%A, b = 14.255(4)
\%A, c = 24.591(4) \%A, V = 4716.2(12) \%A^3^ \a = 102.52(2)\%
\b = 96.09(2)\% \g = 96.61(2)\%.
For Z = 2 and F.W. = 2022.84, the calculated density is 1.424 g/cm^3^.
Based on a statistical analysis of intensity distribution, and the successful
solution and refinement of the structure, the space group was determined to
be: P -1 (#2)
The data were collected at a temperature of 28(2)\%C to a maximum 2\q value of
50.05\%. A total of 1421 oscillation images were collected in 4 runs. A sweep
of data was done using \w scans from 330.0 to 148.2\% in -0.3\% step, at \c =
54.7\% and \f = 0.0\%. The exposure rate was 80.0 [sec./\%]. The detector
swing angle was -30.00\%. A second sweep was performed using \w scans from
330.0 to 199.5\% in -0.3\% step, at \c = 54.7\% and \f = 90.0\%. The exposure
rate was 80.0 [sec./\%]. The detector swing angle was -30.00\%. A third sweep
was performed using \w scans from 330.0 to 261.0\% in -0.3\% step, at \c =
54.7\% and \f = 180.0\%. The exposure rate was 80.0 [sec./\%]. The detector
swing angle was -30.00\%. A last sweep was performed using \w scans from 330.0
to 285.0\% in -0.3\% step, at \c = 54.7\% and \f = 270.0\%. The exposure
rate was 80.0 [sec./\%]. The detector swing angle was -30.00\%. The
crystal-to-detector distance was 50.00 mm.
Of the 44341 reflections that were collected, 16587 reflections were unique.
(R~int~ = 0.0321); equivalent reflections were merged.
;
_publ_section_exptl_refinement
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The structure was solved by Direct methods (SHELXS, (Sheldrick, 2008))
and expanded using Fourier techniques. Most of the non-H atoms
were refined anisotropically.
Due to the data quality problem, some of the C-bound H atoms were refined
using riding model with U~iso~(H) = 1.2U~eq~(Carrier) for phenyl
and methylene H-atoms and U~iso~(H) = 1.5U~eq~(Carrier)
for methyl H-atoms. Some phenyl H atoms were fixed.
Highest peak is 1.38 at (0.1666, 0.6778, 0.2421) [0.14\%A from Pt2]
Deepest hole is -0.86 at (0.7986, 0.5710, 0.4313) [0.65\%A from S1]
;
#==============================================================================
data_wt1945w-shelxl
_database_code_depnum_ccdc_archive 'CCDC 767390'
#TrackingRef '- wt1945w-shelxl-revised.cif'
# wt1945w-YAM-AT315
_iucr_refine_instructions_details
;
TITL wt1945w-YAM-AT315
CELL 0.71073 14.00200 14.25500 24.59100 102.520 96.090 96.610
ZERR 2 0.00200 0.00200 0.00400 0.020 0.020 0.020
LATT 1
SFAC C H AG F N O PT S
UNIT 194 164 2 6 20 6 4 2
SHEL 8.000000 0.84
OMIT 0 -2 1
OMIT -1 1 5
OMIT 1 1 7
OMIT 2 -1 2
OMIT 1 3 3
OMIT 1 -1 1
OMIT 2 -5 3
OMIT -1 1 4
OMIT -1 3 2
OMIT 2 -2 4
OMIT 0 -1 4
OMIT 0 0 4
OMIT -1 1 2
OMIT 1 -2 5
OMIT -2 1 6
L.S. 20
FMAP 2
PLAN -20
BOND $H
HTAB
MERG 3
TEMP 28.0
EADP C53 C53'
EXYZ C53 C53'
DFIX 1.73 0.01 S1 C97
DFIX 1.33 0.01 C97 F1
DFIX 1.43 0.01 S1 O1
DFIX 1.53 0.01 C22 C23
DANG 2.56 0.02 C22 C24
SADI 0.01 C23 C24 C22 C23
SADI 0.02 C54 C55 C55 C56 C54' C55' C55' C56'
ISOR 0.01 0.02 C12 C17 C23 C24 C28 C46 C47 C52 C67 C69 C73 C76
ISOR 0.01 0.02 C80 C80' C81 C81' C82' C83 C83' C84 C84' C85 C87 C88 C89 C90
ACTA
SIZE 0.490 0.420 0.390
LIST 4
WGHT 0.114400
FVAR 1.73296 0.53602 0.54462 0.72790
PT1 7 0.679532 0.080934 0.628846 11.00000 0.06888 0.10115 =
0.07036 0.01629 0.00954 0.00735
PT2 7 0.837065 0.318702 0.762399 11.00000 0.07120 0.09704 =
0.07145 0.01868 0.01129 0.00786
AG1 3 0.766478 0.111324 0.754436 11.00000 0.09240 0.10337 =
0.07841 0.01705 0.00873 0.01096
N1 5 0.533129 0.047059 0.620786 11.00000 0.07342 0.10340 =
0.08420 0.01195 0.01227 -0.00255
N2 5 0.385607 0.067532 0.584379 11.00000 0.06321 0.21120 =
0.14671 0.06443 -0.00707 -0.00564
N3 5 0.810431 0.143466 0.616583 11.00000 0.06769 0.10007 =
0.07442 0.01593 0.01945 0.01213
N4 5 0.895592 0.242411 0.575241 11.00000 0.08082 0.09262 =
0.08214 0.01042 0.01488 -0.00116
N5 5 0.699189 0.327143 0.729044 11.00000 0.07227 0.08851 =
0.08047 0.02455 0.01620 0.01393
N6 5 0.600098 0.376333 0.668182 11.00000 0.08449 0.10015 =
0.08573 0.03380 0.00847 0.01407
N7 5 0.984524 0.341006 0.773611 11.00000 0.06459 0.11498 =
0.08690 0.00739 0.00587 0.00401
N8 5 1.122285 0.405122 0.750994 11.00000 0.07205 0.15539 =
0.09430 -0.01237 0.02300 -0.00347
N9 5 0.785041 -0.369648 0.819916 11.00000 0.17076 0.12693 =
0.10869 0.03022 0.00713 0.05671
N10 5 0.777388 0.075975 1.061685 11.00000 0.14355 0.12874 =
0.10014 0.05662 -0.03075 0.00093
C1 1 0.465964 -0.009132 0.643095 11.00000 0.07387 0.12181 =
0.09234 0.01406 0.00986 -0.01685
C2 1 0.476701 -0.066173 0.679720 11.00000 0.11619 0.16931 =
0.09486 0.05345 0.02440 -0.00487
AFIX 43
H2 2 0.537275 -0.075767 0.695273 11.00000 -1.20000
AFIX 0
C3 1 0.389836 -0.110071 0.692700 11.00000 0.11113 0.22885 =
0.18689 0.10883 0.05067 -0.00403
AFIX 43
H3 2 0.393104 -0.148813 0.718601 11.00000 -1.20000
AFIX 0
C4 1 0.299922 -0.098244 0.668725 11.00000 0.11811 0.22418 =
0.14078 0.04450 0.02532 -0.05139
AFIX 43
H4 2 0.245225 -0.129560 0.679186 11.00000 -1.20000
AFIX 0
C5 1 0.286594 -0.041385 0.629334 11.00000 0.10946 0.26315 =
0.14121 0.07462 -0.00410 -0.05641
AFIX 43
H5 2 0.226517 -0.034519 0.611717 11.00000 -1.20000
AFIX 0
C6 1 0.373056 0.002353 0.620304 11.00000 0.10285 0.14880 =
0.11175 0.02665 0.02562 -0.02999
C7 1 0.485034 0.092046 0.584386 11.00000 0.07330 0.13855 =
0.10162 0.03479 -0.00785 -0.01241
C8 1 0.539470 0.152223 0.556024 11.00000 0.06097 0.13257 =
0.11174 0.03176 -0.00274 -0.02045
C9 1 0.639020 0.157612 0.575384 11.00000 0.08116 0.10130 =
0.07483 0.00796 0.01728 0.00633
C10 1 0.710199 0.210680 0.553669 11.00000 0.07350 0.10107 =
0.10106 0.02753 0.01547 0.01319
C11 1 0.681749 0.260317 0.514399 11.00000 0.09582 0.13808 =
0.14777 0.07935 0.01183 0.01465
AFIX 43
H11 2 0.727340 0.298950 0.500876 11.00000 -1.20000
AFIX 0
C12 1 0.582237 0.251879 0.494823 11.00000 0.12457 0.16493 =
0.14201 0.08134 0.00169 0.01325
AFIX 43
H12 2 0.564597 0.281327 0.465749 11.00000 -1.20000
AFIX 0
C13 1 0.510064 0.203675 0.515446 11.00000 0.10914 0.21471 =
0.14061 0.11915 0.02144 0.04688
AFIX 43
H13 2 0.444934 0.204488 0.503526 11.00000 -1.20000
AFIX 0
C14 1 0.805184 0.201433 0.580031 11.00000 0.05591 0.08977 =
0.08426 0.00881 0.01168 0.00843
C15 1 0.908694 0.145883 0.636671 11.00000 0.06053 0.11768 =
0.07910 0.01520 0.01891 0.01265
C16 1 0.951818 0.102227 0.671001 11.00000 0.08094 0.19026 =
0.06881 0.03480 0.01495 0.03748
AFIX 43
H16 2 0.915317 0.061203 0.688151 11.00000 -1.20000
AFIX 0
C17 1 1.053380 0.116419 0.682516 11.00000 0.09092 0.15691 =
0.09088 0.02844 0.01325 0.02496
AFIX 43
H17 2 1.084922 0.082410 0.705508 11.00000 -1.20000
AFIX 0
C18 1 1.105321 0.181595 0.659133 11.00000 0.07989 0.17702 =
0.08348 0.00064 -0.01363 0.02917
AFIX 43
H18 2 1.172201 0.194846 0.669418 11.00000 -1.20000
AFIX 0
C19 1 1.064063 0.227749 0.621735 11.00000 0.07765 0.13211 =
0.09424 -0.01262 0.02244 -0.00619
AFIX 43
H19 2 1.099985 0.269532 0.604775 11.00000 -1.20000
AFIX 0
C20 1 0.962595 0.206789 0.610999 11.00000 0.06510 0.11761 =
0.07150 -0.00031 0.00334 0.01481
SAME C25 > C28
SAME C53 > C56
SAME C53' > C56'
C21 1 0.299386 0.119390 0.557394 11.00000 0.14553 0.15344 =
0.13929 -0.01645 0.05763 -0.00503
AFIX 23
H21A 2 0.245022 0.120397 0.578796 11.00000 -1.20000
H21B 2 0.323261 0.185212 0.555748 11.00000 -1.20000
AFIX 0
C22 1 0.272181 0.056042 0.500715 11.00000 0.31600 0.15025 =
0.26020 -0.09809 0.10299 -0.02415
AFIX 23
H22A 2 0.253188 -0.010632 0.502684 11.00000 -1.20000
H22B 2 0.325735 0.058393 0.478824 11.00000 -1.20000
AFIX 0
C23 1 0.184003 0.098117 0.474068 11.00000 0.14858 0.19958 =
0.20217 0.05179 -0.03566 0.04037
AFIX 23
H23A 2 0.187186 0.166782 0.490808 11.00000 -1.20000
H23B 2 0.183758 0.089304 0.433814 11.00000 -1.20000
AFIX 0
C24 1 0.091719 0.039177 0.487201 11.00000 0.25404 0.25492 =
0.26743 0.02847 0.03497 0.08029
AFIX 137
H24A 2 0.035491 0.049163 0.464385 11.00000 -1.50000
H24B 2 0.084879 0.060742 0.526194 11.00000 -1.50000
H24C 2 0.098027 -0.028627 0.479100 11.00000 -1.50000
AFIX 0
C25 1 0.922205 0.303677 0.535644 11.00000 0.08641 0.09365 =
0.12810 0.02682 0.01391 -0.00473
AFIX 23
H25A 2 0.984636 0.342933 0.550384 11.00000 -1.20000
H25B 2 0.874465 0.347248 0.532968 11.00000 -1.20000
AFIX 0
C26 1 0.927400 0.244221 0.478479 11.00000 0.10784 0.12315 =
0.10233 0.02630 0.03358 -0.00891
AFIX 23
H26A 2 0.865265 0.203970 0.464422 11.00000 -1.20000
H26B 2 0.975724 0.201339 0.481444 11.00000 -1.20000
AFIX 0
C27 1 0.952472 0.303075 0.436368 11.00000 0.11964 0.14617 =
0.13111 0.04467 0.02163 -0.00730
AFIX 23
H27A 2 1.011533 0.348042 0.451272 11.00000 -1.20000
H27B 2 0.900654 0.340343 0.429299 11.00000 -1.20000
AFIX 0
C28 1 0.966796 0.233407 0.380640 11.00000 0.18973 0.23184 =
0.13060 0.07182 0.02430 -0.01677
AFIX 137
H28A 2 0.979596 0.270311 0.353211 11.00000 -1.50000
H28B 2 0.909049 0.187439 0.366861 11.00000 -1.50000
H28C 2 1.020584 0.199465 0.387447 11.00000 -1.50000
AFIX 0
C29 1 0.605417 0.287541 0.733549 11.00000 0.06137 0.07871 =
0.08441 0.01393 0.00573 0.00485
C30 1 0.568509 0.230534 0.766222 11.00000 0.07779 0.09650 =
0.09319 0.02818 0.01350 0.00490
AFIX 43
H30 2 0.608748 0.210919 0.792947 11.00000 -1.20000
AFIX 0
C31 1 0.468328 0.202414 0.758362 11.00000 0.09721 0.12415 =
0.11358 0.02734 0.03145 0.00588
AFIX 43
H31 2 0.441904 0.160959 0.779051 11.00000 -1.20000
AFIX 0
C32 1 0.407541 0.234549 0.720694 11.00000 0.08104 0.13890 =
0.12043 0.02346 0.02801 -0.00180
AFIX 43
H32 2 0.341007 0.215284 0.717287 11.00000 -1.20000
AFIX 0
C33 1 0.441855 0.293586 0.688338 11.00000 0.07647 0.11593 =
0.11261 0.01848 0.00747 0.01803
AFIX 43
H33 2 0.400429 0.315444 0.663194 11.00000 -1.20000
AFIX 0
C34 1 0.544850 0.320418 0.694889 11.00000 0.07360 0.09065 =
0.08574 0.01051 0.00514 0.00048
C35 1 0.694656 0.378566 0.689966 11.00000 0.08060 0.07229 =
0.08501 0.02680 0.01595 0.02028
C36 1 0.786760 0.424262 0.677319 11.00000 0.08042 0.09530 =
0.08027 0.02820 0.01973 0.00631
C37 1 0.863001 0.400233 0.709005 11.00000 0.08357 0.07683 =
0.07292 0.00504 0.01436 0.00168
C38 1 0.959021 0.435303 0.705273 11.00000 0.08352 0.09602 =
0.07949 0.00014 0.02212 -0.00014
C39 1 0.977126 0.494922 0.667595 11.00000 0.10147 0.11222 =
0.12089 0.02375 0.03629 -0.01549
AFIX 43
H39 2 1.040217 0.519271 0.664244 11.00000 -1.20000
AFIX 0
C40 1 0.899602 0.515985 0.636147 11.00000 0.14415 0.11023 =
0.11805 0.04221 0.04863 0.00547
AFIX 43
H40 2 0.910837 0.554161 0.610604 11.00000 -1.20000
AFIX 0
C41 1 0.806489 0.483002 0.640924 11.00000 0.11043 0.12586 =
0.11458 0.06169 0.02286 0.01436
AFIX 43
H41 2 0.755576 0.500240 0.619420 11.00000 -1.20000
AFIX 0
C42 1 1.024349 0.397628 0.741513 11.00000 0.07070 0.10512 =
0.08732 -0.00344 0.01414 -0.00836
AFIX 66
C43 1 1.059170 0.308632 0.802085 11.00000 0.08626 0.13644 =
0.06930 -0.00373 -0.00876 0.01431
C44 1 1.059677 0.244321 0.837248 11.00000 0.09238 0.18473 =
0.09514 0.00711 -0.00335 0.04244
AFIX 43
H44 2 1.001520 0.217079 0.846212 11.00000 -1.20000
AFIX 65
C45 1 1.147107 0.220725 0.859013 11.00000 0.11327 0.23108 =
0.12046 0.00304 -0.00489 0.06907
AFIX 43
H45 2 1.147447 0.177696 0.882540 11.00000 -1.20000
AFIX 65
C46 1 1.234030 0.261441 0.845616 11.00000 0.12451 0.17476 =
0.14571 0.00654 0.00132 0.04314
AFIX 43
H46 2 1.292526 0.245654 0.860179 11.00000 -1.20000
AFIX 65
C47 1 1.233524 0.325752 0.810453 11.00000 0.10121 0.15460 =
0.13253 -0.00595 0.01130 0.00708
AFIX 43
H47 2 1.291682 0.352993 0.801489 11.00000 -1.20000
AFIX 65
C48 1 1.146095 0.349349 0.788687 11.00000 0.06853 0.17545 =
0.10517 -0.02722 -0.00758 0.01994
AFIX 0
C49 1 0.562958 0.428445 0.626780 11.00000 0.10270 0.16029 =
0.11727 0.07492 0.00610 0.01739
AFIX 23
H49A 2 0.497945 0.398120 0.609754 11.00000 -1.20000
H49B 2 0.604124 0.425192 0.597281 11.00000 -1.20000
AFIX 0
C50 1 0.561237 0.532796 0.655185 11.00000 0.16489 0.15150 =
0.20434 0.10712 -0.02101 0.04658
AFIX 23
H50A 2 0.619484 0.554548 0.682230 11.00000 -1.20000
H50B 2 0.506402 0.535127 0.676220 11.00000 -1.20000
AFIX 0
C51 1 0.554715 0.606952 0.617588 11.00000 0.22779 0.17389 =
0.22159 0.02096 -0.03851 0.03800
AFIX 23
H51A 2 0.612922 0.612043 0.599639 11.00000 -1.20000
H51B 2 0.499579 0.584398 0.588360 11.00000 -1.20000
AFIX 0
C52 1 0.544296 0.700433 0.650455 11.00000 0.33543 0.21034 =
0.32371 0.02122 -0.04385 0.09153
AFIX 33
H52A 2 0.527533 0.741717 0.625907 11.00000 -1.50000
H52B 2 0.604379 0.728734 0.673929 11.00000 -1.50000
H52C 2 0.493995 0.693479 0.673549 11.00000 -1.50000
AFIX 0
PART 1
C53 1 1.190413 0.455351 0.722209 21.00000 0.13111
AFIX 23
H53A 2 1.170629 0.431824 0.682063 21.00000 -1.20000
H53B 2 1.253720 0.436508 0.730646 21.00000 -1.20000
AFIX 0
C54 1 1.201881 0.565684 0.735590 21.00000 0.18944
AFIX 23
H54A 2 1.138760 0.587305 0.736637 21.00000 -1.20000
H54B 2 1.232719 0.589747 0.706812 21.00000 -1.20000
AFIX 0
C55 1 1.264882 0.604905 0.793285 21.00000 0.46346
AFIX 23
H55A 2 1.309796 0.560123 0.799518 21.00000 -1.20000
H55B 2 1.223920 0.611096 0.822936 21.00000 -1.20000
AFIX 0
C56 1 1.321771 0.705091 0.794477 21.00000 0.27140
AFIX 33
H56A 2 1.370623 0.723782 0.826802 21.00000 -1.50000
H56B 2 1.277968 0.752440 0.796399 21.00000 -1.50000
H56C 2 1.352049 0.701264 0.760970 21.00000 -1.50000
AFIX 0
PART 2
C53' 1 1.190413 0.455351 0.722209 -21.00000 0.13111
AFIX 23
H53C 2 1.157496 0.473543 0.690134 -21.00000 -1.20000
H53D 2 1.239869 0.416237 0.710008 -21.00000 -1.20000
AFIX 0
C54' 1 1.232334 0.542873 0.768245 -21.00000 0.14772
AFIX 23
H54C 2 1.258072 0.521560 0.801005 -21.00000 -1.20000
H54D 2 1.180997 0.580627 0.778717 -21.00000 -1.20000
AFIX 0
C55' 1 1.313596 0.607980 0.750752 -21.00000 10.30000
AFIX 23
H55C 2 1.346141 0.569940 0.722636 -21.00000 -1.20000
H55D 2 1.361119 0.640075 0.782977 -21.00000 -1.20000
AFIX 0
C56' 1 1.261765 0.683809 0.726171 -21.00000 10.48383
AFIX 33
H56D 2 1.308622 0.725863 0.713465 -21.00000 -1.50000
H56E 2 1.231158 0.721604 0.754777 -21.00000 -1.50000
H56F 2 1.213607 0.650646 0.695137 -21.00000 -1.50000
AFIX 0
PART 0
C57 1 0.719374 -0.007748 0.680311 11.00000 0.08043 0.11604 =
0.06875 -0.01038 0.00972 -0.00408
C58 1 0.738794 -0.064233 0.711043 11.00000 0.10278 0.11500 =
0.06613 0.02372 0.00258 0.00922
C59 1 0.751419 -0.141017 0.738120 11.00000 0.08676 0.10270 =
0.07590 0.01453 0.00158 0.00787
C60 1 0.709079 -0.146131 0.786321 11.00000 0.11572 0.11462 =
0.08960 0.02734 0.01764 0.02766
AFIX 43
H60 2 0.672931 -0.098018 0.800742 11.00000 -1.20000
AFIX 0
C61 1 0.719044 -0.219572 0.812999 11.00000 0.15014 0.11206 =
0.08089 0.02612 0.02750 0.03692
AFIX 43
H61 2 0.687323 -0.222058 0.844131 11.00000 -1.20000
AFIX 0
C62 1 0.775912 -0.290968 0.794444 11.00000 0.12769 0.11502 =
0.09186 0.01931 0.00742 0.01645
C63 1 0.819410 -0.287750 0.744850 11.00000 0.14015 0.12620 =
0.10308 0.01930 0.01972 0.05019
AFIX 43
H63 2 0.854775 -0.336169 0.729838 11.00000 -1.20000
AFIX 0
C64 1 0.807997 -0.210928 0.719347 11.00000 0.11256 0.12314 =
0.09671 0.01837 0.02319 0.01662
AFIX 43
H64 2 0.839796 -0.206652 0.688449 11.00000 -1.20000
AFIX 66
C65 1 0.704744 -0.428782 0.832516 11.00000 0.21187 0.10826 =
0.09474 0.03015 0.02959 0.01467
C66 1 0.604802 -0.431639 0.822056 11.00000 0.17486 0.17168 =
0.14382 0.03318 0.02360 -0.01837
AFIX 43
H66 2 0.579113 -0.389200 0.802544 11.00000 -1.20000
AFIX 65
C67 1 0.543253 -0.497924 0.840758 11.00000 0.20690 0.18752 =
0.18257 0.05501 0.04012 0.00576
AFIX 43
H67 2 0.476385 -0.499835 0.833759 11.00000 -1.20000
AFIX 65
C68 1 0.581646 -0.561355 0.869920 11.00000 0.24963 0.12672 =
0.15868 0.05023 0.05240 0.02075
AFIX 43
H68 2 0.540466 -0.605704 0.882433 11.00000 -1.20000
AFIX 65
C69 1 0.681588 -0.558499 0.880381 11.00000 0.19480 0.13302 =
0.13108 0.03762 0.01529 0.02780
AFIX 43
H69 2 0.707276 -0.600938 0.899893 11.00000 -1.20000
AFIX 65
C70 1 0.743138 -0.492214 0.861679 11.00000 0.22222 0.10182 =
0.10817 -0.01475 0.03124 0.02840
AFIX 66
C71 1 0.844028 -0.471353 0.867466 11.00000 0.27193 0.14085 =
0.08765 0.01408 -0.01510 0.11295
C72 1 0.865692 -0.396489 0.840797 11.00000 0.20619 0.14973 =
0.08163 -0.00249 0.01517 0.08449
C73 1 0.961796 -0.358835 0.840834 11.00000 0.16152 0.15172 =
0.13808 0.01223 0.01205 0.04232
AFIX 43
H73 2 0.976290 -0.308746 0.822991 11.00000 -1.20000
AFIX 65
C74 1 1.036235 -0.396045 0.867540 11.00000 0.21505 0.20593 =
0.14730 -0.03983 0.00273 0.10863
AFIX 43
H74 2 1.100534 -0.370851 0.867565 11.00000 -1.20000
AFIX 65
C75 1 1.014573 -0.470908 0.894208 11.00000 0.21891
AFIX 43
H75 2 1.064378 -0.495804 0.912076 11.00000 -1.20000
AFIX 65
C76 1 0.918470 -0.508563 0.894172 11.00000 0.21219 0.15003 =
0.15787 0.02913 0.01777 0.03480
AFIX 43
H76 2 0.903976 -0.558652 0.912015 11.00000 -1.20000
AFIX 0
C77 1 0.812363 0.242816 0.821771 11.00000 0.08838 0.08923 =
0.06550 0.01700 -0.00017 0.00961
C78 1 0.799366 0.199619 0.858892 11.00000 0.08145 0.11630 =
0.09615 0.02342 0.00567 0.03630
PART 1
SAME C79' > C84'
AFIX 66
C79 1 0.797284 0.168008 0.908606 31.00000 0.07189 0.09044 =
0.05329 0.02859 -0.01209 0.02244
C80 1 0.856045 0.222292 0.956863 31.00000 0.13481 0.11933 =
0.10044 0.04533 -0.00241 -0.00222
AFIX 43
H80 2 0.895298 0.278850 0.955648 31.00000 -1.20000
AFIX 65
C81 1 0.856140 0.192043 1.006935 31.00000 0.12009 0.10527 =
0.08601 0.04408 -0.00885 0.00445
AFIX 43
H81 2 0.895455 0.228362 1.039222 31.00000 -1.20000
AFIX 65
C82 1 0.797473 0.107510 1.008751 31.00000 0.08792 0.21769 =
0.06323 0.03396 -0.00261 0.01524
C83 1 0.738711 0.053225 0.960495 31.00000 0.12982 0.12062 =
0.11505 0.03558 0.02017 0.00393
AFIX 43
H83 2 0.699459 -0.003334 0.961710 31.00000 -1.20000
AFIX 65
C84 1 0.738616 0.083473 0.910422 31.00000 0.10072 0.11285 =
0.08876 0.02603 0.00329 -0.01209
AFIX 43
H84 2 0.699300 0.047153 0.878136 31.00000 -1.20000
AFIX 66
PART 2
C79' 1 0.778156 0.157915 0.912298 -31.00000 0.14560 0.09316 =
0.11236 0.02126 0.06731 0.03198
C80' 1 0.741677 0.216272 0.955948 -31.00000 0.13867 0.13457 =
0.11676 0.03738 0.03164 0.01583
AFIX 43
H80' 2 0.718900 0.273017 0.950983 -31.00000 -1.20000
AFIX 65
C81' 1 0.739242 0.189816 1.007019 -31.00000 0.15132 0.13902 =
0.14279 0.03916 0.03014 0.04460
AFIX 43
H81' 2 0.714835 0.228861 1.036224 -31.00000 -1.20000
AFIX 65
C82' 1 0.773284 0.105003 1.014440 -31.00000 0.08150 0.06651 =
0.08544 0.03010 -0.00094 0.00934
C83' 1 0.809763 0.046646 0.970790 -31.00000 0.13916 0.12927 =
0.13217 0.03208 0.02657 0.02680
AFIX 43
H83' 2 0.832539 -0.010100 0.975756 -31.00000 -1.20000
AFIX 65
C84' 1 0.812199 0.073100 0.919720 -31.00000 0.12544 0.11488 =
0.10366 0.03693 0.01363 0.02237
AFIX 43
H84' 2 0.836605 0.034055 0.890515 -31.00000 -1.20000
AFIX 66
PART 0
C85 1 0.848679 0.065591 1.099505 11.00000 0.15019 0.11847 =
0.12632 0.04376 -0.02017 0.00618
C86 1 0.946876 0.076590 1.094023 11.00000 0.21670 0.18387 =
0.18409 0.11757 -0.06572 -0.00413
AFIX 43
H86 2 0.967200 0.091377 1.061680 11.00000 -1.20000
AFIX 65
C87 1 1.014694 0.065490 1.136881 11.00000 0.24562 0.26163 =
0.24325 0.09199 -0.00191 0.01016
AFIX 43
H87 2 1.080394 0.072850 1.133213 11.00000 -1.20000
AFIX 65
C88 1 0.984317 0.043389 1.185222 11.00000 0.20556 0.22636 =
0.19159 0.09734 -0.01572 0.01907
AFIX 43
H88 2 1.029693 0.035962 1.213897 11.00000 -1.20000
AFIX 65
C89 1 0.886121 0.032389 1.190705 11.00000 0.19713 0.18094 =
0.16460 0.08715 -0.02092 0.00953
AFIX 43
H89 2 0.865798 0.017602 1.223048 11.00000 -1.20000
AFIX 65
C90 1 0.818302 0.043490 1.147847 11.00000 0.16028 0.12221 =
0.11938 0.06653 -0.03077 -0.00476
AFIX 66
C91 1 0.719121 0.033599 1.137029 11.00000 0.20719 0.14226 =
0.08917 0.06442 -0.00635 0.01228
C92 1 0.694768 0.057111 1.085828 11.00000 0.20202 0.12114 =
0.09951 0.03799 0.00673 0.00985
C93 1 0.598225 0.059099 1.066519 11.00000 0.17162 0.28799 =
0.11194 0.07216 -0.00265 0.02352
AFIX 43
H93 2 0.581932 0.074830 1.032262 11.00000 -1.20000
AFIX 65
C94 1 0.526034 0.037576 1.098411 11.00000 0.16983 0.37531 =
0.17249 0.14921 0.04258 0.05143
AFIX 43
H94 2 0.461440 0.038906 1.085491 11.00000 -1.20000
AFIX 65
C95 1 0.550385 0.014064 1.149612 11.00000 0.18925 0.37150 =
0.17844 0.12942 0.05696 0.00919
AFIX 43
H95 2 0.502084 -0.000337 1.170950 11.00000 -1.20000
AFIX 65
C96 1 0.646928 0.012075 1.168922 11.00000 0.29037 0.19562 =
0.12105 0.09484 0.00947 0.00650
AFIX 43
H96 2 0.663220 -0.003655 1.203179 11.00000 -1.20000
AFIX 0
PART 1
SAME S1 O2 O3 O1 C97 F3 F1 F2
SAME S1' > F3'
S1 8 0.248515 0.433912 0.572647 41.00000 0.14105
O1 6 0.147224 0.429370 0.570491 41.00000 0.21937
O2 6 0.290970 0.525870 0.607774 41.00000 0.29865
O3 6 0.284643 0.360538 0.589699 41.00000 0.22374
C97 1 0.281814 0.434858 0.507577 41.00000 10.32785
F1 4 0.373014 0.424271 0.515415 41.00000 0.27896
F2 4 0.267479 0.513510 0.495300 41.00000 0.38098
F3 4 0.238715 0.363929 0.469751 41.00000 0.33786
PART 2
S1' 8 0.321430 0.443110 0.616292 -41.00000 0.21352
O1' 6 0.269386 0.387167 0.646725 -41.00000 10.30136
O2' 6 0.393529 0.511124 0.651908 -41.00000 0.45031
O3' 6 0.360297 0.383093 0.573637 -41.00000 10.30136
C97' 1 0.243839 0.504324 0.584912 -41.00000 0.07548
F1' 4 0.289815 0.585644 0.581263 -41.00000 0.16948
F2' 4 0.178070 0.525139 0.615464 -41.00000 0.33558
F3' 4 0.199691 0.472801 0.536976 -41.00000 10.21541
PART 0
HKLF 4
REM wt1945w-YAM-AT315
REM R1 = 0.0559 for 10781 Fo > 4sig(Fo) and 0.0818 for all 16587 data
REM 1002 parameters refined using 311 restraints
END
WGHT 0.1094 0.0000
REM Highest difference peak 1.378, deepest hole -0.863, 1-sigma level 0.103
Q1 1 0.7511 0.2863 0.6366 11.00000 0.05 1.30
Q2 1 0.6594 0.1042 0.6036 11.00000 0.05 1.14
Q3 1 0.2552 0.3878 0.5482 11.00000 0.05 1.01
Q4 1 0.9183 -0.6462 0.8861 11.00000 0.05 1.01
Q5 1 0.6662 0.1266 0.6577 11.00000 0.05 0.97
Q6 1 0.1852 0.5191 0.5030 11.00000 0.05 0.95
Q7 1 0.6943 0.1378 0.6593 11.00000 0.05 0.94
Q8 1 0.3578 0.5046 0.5094 11.00000 0.05 0.93
Q9 1 0.3876 0.1280 0.3763 11.00000 0.05 0.93
Q10 1 0.9933 -0.4423 0.8939 11.00000 0.05 0.89
Q11 1 0.8025 0.2632 0.7330 11.00000 0.05 0.87
Q12 1 0.1745 0.3514 0.5601 11.00000 0.05 0.83
Q13 1 0.2217 0.4886 0.5536 11.00000 0.05 0.81
Q14 1 0.8743 0.3719 0.7928 11.00000 0.05 0.78
Q15 1 0.4781 0.1596 0.5023 11.00000 0.05 0.72
Q16 1 0.3223 0.0402 0.5300 11.00000 0.05 0.67
Q17 1 0.6414 0.0243 0.5998 11.00000 0.05 0.63
Q18 1 0.4829 0.5461 0.6788 11.00000 0.05 0.57
Q19 1 0.2030 0.1627 0.4459 11.00000 0.05 0.56
Q20 1 1.2106 0.4262 0.7411 11.00000 0.05 0.56
;
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C96 H82 Ag N10 Pt2, C F3 O3 S'
_chemical_formula_sum 'C97 H82 Ag F3 N10 O3 Pt2 S'
_chemical_formula_weight 2022.84
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 14.002(2)
_cell_length_b 14.255(2)
_cell_length_c 24.591(4)
_cell_angle_alpha 102.52(2)
_cell_angle_beta 96.09(2)
_cell_angle_gamma 96.61(2)
_cell_volume 4716.1(12)
_cell_formula_units_Z 2
_cell_measurement_temperature 301(2)
_cell_measurement_reflns_used 44341
_cell_measurement_theta_min 2.57
_cell_measurement_theta_max 25.03
_exptl_crystal_description block
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.49
_exptl_crystal_size_mid 0.42
_exptl_crystal_size_min 0.39
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.424
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2008
_exptl_absorpt_coefficient_mu 3.244
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.2993
_exptl_absorpt_correction_T_max 0.3643
_exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 301(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker SMART 1000 CCD'
_diffrn_measurement_method '\w and \f scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time .
_diffrn_standards_decay_% ?
_diffrn_reflns_number 44341
_diffrn_reflns_av_R_equivalents 0.0321
_diffrn_reflns_av_sigmaI/netI 0.0399
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_theta_min 2.57
_diffrn_reflns_theta_max 25.03
_reflns_number_total 16587
_reflns_number_gt 10781
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'SMART (Bruker AXS Inc, 1998)'
_computing_cell_refinement 'SAINT (Bruker AXS Inc, 2006)'
_computing_data_reduction 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'MERCURY (Macrae et al., 2008)'
_computing_publication_material 'SHELXL97 (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The data set was collected at ambient temperature, 28(2)\% Celsius.
A total of 311 restraints have been used in the refinement.
156 restraints were related to the anisotropic refinement of the 26 atoms:
C12 C17 C23 C24 C28 C46 C47 C52 C67 C69 C73 C76 C80 C80' C81 C81' C82'
C83 C83' C84 C84' C85 C87 C88 C89 & C90 using isotropic restraints with
standard uncertainty of 0.01, 6 restraints for each atoms.
149 restraints were related to the similar distance restraints for the
butyl groups and the CF~3~SO~3~ ion. 5 restraints were used to fix the
S1--C97 to be 1.73(1)\%A, C97--F1 to be 1.33(1)\%A, S1--O1 to be 1.43\%A,
C22--C23 to be 1.53(1)\%A and C22-C23-C24 angle to be 109.5(2)\%.
Details of the command used could be found under
_iucr_refine_instructions_details of this CIF.
A total of seven phenyl rings were refined as rigid groups, i.e. C43-C48,
C65-C70, C71-C76, C79-C84, C79'-C84', C85-C90, C91-C96' using AFIX 66.
Due to the high thermal parameter of the CF~3~SO~3~ ion, the atoms were only
refined isotropically, and the atoms C97, O1', O2', O3' and F3' could only be
refined with fixed thermal parameters.
One of the n-butyl group (C53-C56), the phenyl ring (C79-C84) and the triflate
ion (S1/O1-O3/C97/F1-F3) were found to be disordered, The occupancies ratio
were refined to be 0.54(2):0.48(2); 0.545(11):0.455(11) and 0.728(7):0.272(7)
respectively.
There is a large void in the lattice, which amount to about 598\%A^3^. Attempts
to locate the solvent molecules in the void as dichloromethane
were unsuccessful. Attempts to model the void as two diethyl ether molecules
originally give some positive results, however, the refinement could not be
converged even with lots of restraints/constraints. Thus at the end, the
PLATON SQUEEZE routine was run and the .hkp file obtained containing
the solvent free reflection data was renamed to .hkl file. the SHELXL
refinement was continued with the disordered solvent free .ins file.
After least-square convergence, PLATON was run again with the new .hkl
and .res files with the instruction 'CALC FCF' in order to produce
a proper final FoFc-CIF on a file with extension .hkp which was then
renamed to extension .fcf.
The .sqf file produced by PLATON which details the SQUEEZE results was
appended to the CIF here.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1144P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 16587
_refine_ls_number_parameters 1002
_refine_ls_number_restraints 311
_refine_ls_R_factor_all 0.0818
_refine_ls_R_factor_gt 0.0559
_refine_ls_wR_factor_ref 0.1802
_refine_ls_wR_factor_gt 0.1652
_refine_ls_goodness_of_fit_ref 1.009
_refine_ls_restrained_S_all 1.031
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.67953(2) 0.08093(2) 0.628846(13) 0.08106(14) Uani 1 1 d . . .
Pt2 Pt 0.83707(2) 0.31870(2) 0.762399(13) 0.08024(14) Uani 1 1 d . . .
Ag1 Ag 0.76648(5) 0.11132(5) 0.75444(3) 0.0925(2) Uani 1 1 d . B .
N1 N 0.5331(5) 0.0471(5) 0.6208(3) 0.0896(19) Uani 1 1 d . . .
N2 N 0.3856(6) 0.0675(9) 0.5844(5) 0.140(4) Uani 1 1 d . . .
N3 N 0.8104(4) 0.1435(5) 0.6166(3) 0.0806(17) Uani 1 1 d . . .
N4 N 0.8956(5) 0.2424(5) 0.5752(3) 0.0875(18) Uani 1 1 d . . .
N5 N 0.6992(4) 0.3271(5) 0.7290(3) 0.0790(16) Uani 1 1 d . . .
N6 N 0.6001(5) 0.3763(5) 0.6682(3) 0.0884(18) Uani 1 1 d . . .
N7 N 0.9845(5) 0.3410(6) 0.7736(3) 0.092(2) Uani 1 1 d . A .
N8 N 1.1223(5) 0.4051(7) 0.7510(4) 0.114(3) Uani 1 1 d . . .
N9 N 0.7850(9) -0.3696(7) 0.8199(4) 0.133(3) Uani 1 1 d . . .
N10 N 0.7774(7) 0.0760(7) 1.0617(4) 0.124(3) Uani 1 1 d . . .
C1 C 0.4660(7) -0.0091(8) 0.6431(4) 0.100(3) Uani 1 1 d . . .
C2 C 0.4767(8) -0.0662(9) 0.6797(4) 0.125(4) Uani 1 1 d . . .
H2 H 0.5373 -0.0758 0.6953 0.149 Uiso 1 1 calc R . .
C3 C 0.3898(10) -0.1101(12) 0.6927(7) 0.166(6) Uani 1 1 d . . .
H3 H 0.3931 -0.1488 0.7186 0.200 Uiso 1 1 calc R . .
C4 C 0.2999(10) -0.0982(12) 0.6687(6) 0.166(6) Uani 1 1 d . . .
H4 H 0.2452 -0.1296 0.6792 0.199 Uiso 1 1 calc R . .
C5 C 0.2866(9) -0.0414(13) 0.6293(6) 0.175(7) Uani 1 1 d . . .
H5 H 0.2265 -0.0345 0.6117 0.210 Uiso 1 1 calc R . .
C6 C 0.3731(8) 0.0024(9) 0.6203(5) 0.125(4) Uani 1 1 d . . .
C7 C 0.4850(7) 0.0920(8) 0.5844(4) 0.107(3) Uani 1 1 d . . .
C8 C 0.5395(6) 0.1522(8) 0.5560(4) 0.105(3) Uani 1 1 d . . .
C9 C 0.6390(6) 0.1576(6) 0.5754(3) 0.088(2) Uani 1 1 d . . .
C10 C 0.7102(6) 0.2107(7) 0.5537(4) 0.091(2) Uani 1 1 d . . .
C11 C 0.6817(8) 0.2603(8) 0.5144(5) 0.121(4) Uani 1 1 d . . .
H11 H 0.7273 0.2990 0.5009 0.145 Uiso 1 1 calc R . .
C12 C 0.5822(9) 0.2519(9) 0.4948(5) 0.139(4) Uani 1 1 d U . .
H12 H 0.5646 0.2813 0.4657 0.166 Uiso 1 1 calc R . .
C13 C 0.5101(8) 0.2037(10) 0.5154(5) 0.141(5) Uani 1 1 d . . .
H13 H 0.4449 0.2045 0.5035 0.169 Uiso 1 1 calc R . .
C14 C 0.8052(5) 0.2014(6) 0.5800(4) 0.078(2) Uani 1 1 d . . .
C15 C 0.9087(6) 0.1459(7) 0.6367(4) 0.086(2) Uani 1 1 d . . .
C16 C 0.9518(7) 0.1022(9) 0.6710(4) 0.111(3) Uani 1 1 d . . .
H16 H 0.9153 0.0612 0.6882 0.133 Uiso 1 1 calc R . .
C17 C 1.0534(7) 0.1164(9) 0.6825(4) 0.112(3) Uani 1 1 d U . .
H17 H 1.0849 0.0824 0.7055 0.135 Uiso 1 1 calc R . .
C18 C 1.1053(7) 0.1816(10) 0.6591(4) 0.119(4) Uani 1 1 d . . .
H18 H 1.1722 0.1948 0.6694 0.143 Uiso 1 1 calc R . .
C19 C 1.0641(7) 0.2277(8) 0.6217(4) 0.108(3) Uani 1 1 d . . .
H19 H 1.1000 0.2695 0.6048 0.130 Uiso 1 1 calc R . .
C20 C 0.9626(6) 0.2068(7) 0.6110(3) 0.088(2) Uani 1 1 d . . .
C21 C 0.2994(9) 0.1194(10) 0.5574(5) 0.153(5) Uani 1 1 d D . .
H21A H 0.2450 0.1204 0.5788 0.184 Uiso 1 1 calc R . .
H21B H 0.3233 0.1852 0.5557 0.184 Uiso 1 1 calc R . .
C22 C 0.2722(11) 0.0560(11) 0.5007(7) 0.265(12) Uani 1 1 d D . .
H22A H 0.2532 -0.0106 0.5027 0.317 Uiso 1 1 calc R . .
H22B H 0.3257 0.0584 0.4788 0.317 Uiso 1 1 calc R . .
C23 C 0.1840(12) 0.0981(12) 0.4741(7) 0.186(6) Uani 1 1 d DU . .
H23A H 0.1872 0.1668 0.4908 0.223 Uiso 1 1 calc R . .
H23B H 0.1838 0.0893 0.4338 0.223 Uiso 1 1 calc R . .
C24 C 0.0917(12) 0.0392(15) 0.4872(10) 0.260(10) Uani 1 1 d DU . .
H24A H 0.0355 0.0492 0.4644 0.390 Uiso 1 1 calc R . .
H24B H 0.0849 0.0607 0.5262 0.390 Uiso 1 1 calc R . .
H24C H 0.0980 -0.0286 0.4791 0.390 Uiso 1 1 calc R . .
C25 C 0.9222(7) 0.3037(7) 0.5356(4) 0.104(3) Uani 1 1 d D . .
H25A H 0.9846 0.3429 0.5504 0.125 Uiso 1 1 calc R . .
H25B H 0.8745 0.3472 0.5330 0.125 Uiso 1 1 calc R . .
C26 C 0.9274(7) 0.2442(7) 0.4785(4) 0.112(3) Uani 1 1 d D . .
H26A H 0.8653 0.2040 0.4644 0.134 Uiso 1 1 calc R . .
H26B H 0.9757 0.2013 0.4814 0.134 Uiso 1 1 calc R . .
C27 C 0.9525(8) 0.3031(9) 0.4364(5) 0.132(4) Uani 1 1 d D . .
H27A H 1.0115 0.3480 0.4513 0.159 Uiso 1 1 calc R . .
H27B H 0.9007 0.3403 0.4293 0.159 Uiso 1 1 calc R . .
C28 C 0.9668(11) 0.2334(11) 0.3806(5) 0.183(6) Uani 1 1 d DU . .
H28A H 0.9796 0.2703 0.3532 0.275 Uiso 1 1 calc R . .
H28B H 0.9090 0.1874 0.3669 0.275 Uiso 1 1 calc R . .
H28C H 1.0206 0.1995 0.3874 0.275 Uiso 1 1 calc R . .
C29 C 0.6054(5) 0.2875(6) 0.7335(3) 0.076(2) Uani 1 1 d . . .
C30 C 0.5685(6) 0.2305(6) 0.7662(4) 0.089(2) Uani 1 1 d . . .
H30 H 0.6087 0.2109 0.7929 0.106 Uiso 1 1 calc R . .
C31 C 0.4683(8) 0.2024(8) 0.7584(5) 0.111(3) Uani 1 1 d . . .
H31 H 0.4419 0.1610 0.7791 0.133 Uiso 1 1 calc R . .
C32 C 0.4075(7) 0.2345(9) 0.7207(5) 0.115(3) Uani 1 1 d . . .
H32 H 0.3410 0.2153 0.7173 0.138 Uiso 1 1 calc R . .
C33 C 0.4419(7) 0.2936(8) 0.6883(4) 0.103(3) Uani 1 1 d . . .
H33 H 0.4004 0.3154 0.6632 0.124 Uiso 1 1 calc R . .
C34 C 0.5448(6) 0.3204(6) 0.6949(4) 0.086(2) Uani 1 1 d . . .
C35 C 0.6947(6) 0.3786(6) 0.6900(4) 0.077(2) Uani 1 1 d . . .
C36 C 0.7868(6) 0.4243(6) 0.6773(4) 0.084(2) Uani 1 1 d . . .
C37 C 0.8630(6) 0.4002(6) 0.7090(3) 0.080(2) Uani 1 1 d . A .
C38 C 0.9590(6) 0.4353(7) 0.7053(4) 0.090(2) Uani 1 1 d . . .
C39 C 0.9771(8) 0.4949(8) 0.6676(5) 0.113(3) Uani 1 1 d . A .
H39 H 1.0402 0.5193 0.6642 0.136 Uiso 1 1 calc R . .
C40 C 0.8996(10) 0.5160(8) 0.6361(5) 0.120(3) Uani 1 1 d . . .
H40 H 0.9108 0.5542 0.6106 0.145 Uiso 1 1 calc R A .
C41 C 0.8065(8) 0.4830(8) 0.6409(5) 0.111(3) Uani 1 1 d . A .
H41 H 0.7556 0.5002 0.6194 0.134 Uiso 1 1 calc R . .
C42 C 1.0243(6) 0.3976(7) 0.7415(4) 0.093(3) Uani 1 1 d . A .
C43 C 1.0592(4) 0.3086(6) 0.8021(3) 0.103(3) Uani 1 1 d G . .
C44 C 1.0597(5) 0.2443(6) 0.8372(3) 0.127(4) Uani 1 1 d G A .
H44 H 1.0015 0.2171 0.8462 0.153 Uiso 1 1 calc R . .
C45 C 1.1471(6) 0.2207(6) 0.8590(3) 0.159(5) Uani 1 1 d G A .
H45 H 1.1474 0.1777 0.8825 0.190 Uiso 1 1 calc R . .
C46 C 1.2340(5) 0.2614(7) 0.8456(4) 0.153(4) Uani 1 1 d GU A .
H46 H 1.2925 0.2457 0.8602 0.183 Uiso 1 1 calc R . .
C47 C 1.2335(4) 0.3258(6) 0.8105(4) 0.137(4) Uani 1 1 d GU A .
H47 H 1.2917 0.3530 0.8015 0.164 Uiso 1 1 calc R . .
C48 C 1.1461(5) 0.3493(5) 0.7887(3) 0.127(4) Uani 1 1 d G A .
C49 C 0.5630(8) 0.4284(9) 0.6268(5) 0.121(3) Uani 1 1 d . . .
H49A H 0.4979 0.3981 0.6098 0.145 Uiso 1 1 calc R . .
H49B H 0.6041 0.4252 0.5973 0.145 Uiso 1 1 calc R . .
C50 C 0.5612(11) 0.5328(10) 0.6552(7) 0.165(6) Uani 1 1 d . . .
H50A H 0.6195 0.5545 0.6822 0.198 Uiso 1 1 calc R . .
H50B H 0.5064 0.5351 0.6762 0.198 Uiso 1 1 calc R . .
C51 C 0.5547(14) 0.6070(13) 0.6176(9) 0.216(8) Uani 1 1 d . . .
H51A H 0.6129 0.6120 0.5996 0.259 Uiso 1 1 calc R . .
H51B H 0.4996 0.5844 0.5884 0.259 Uiso 1 1 calc R . .
C52 C 0.5443(19) 0.7004(17) 0.6505(12) 0.298(12) Uani 1 1 d U . .
H52A H 0.5275 0.7417 0.6259 0.448 Uiso 1 1 calc R . .
H52B H 0.6044 0.7287 0.6739 0.448 Uiso 1 1 calc R . .
H52C H 0.4940 0.6935 0.6735 0.448 Uiso 1 1 calc R . .
C53 C 1.1904(9) 0.4554(8) 0.7222(5) 0.131(4) Uiso 0.54(2) 1 d PD A 1
H53A H 1.1706 0.4318 0.6821 0.157 Uiso 0.54(2) 1 calc PR A 1
H53B H 1.2537 0.4365 0.7306 0.157 Uiso 0.54(2) 1 calc PR A 1
C54 C 1.202(2) 0.5657(13) 0.7356(13) 0.189(14) Uiso 0.54(2) 1 d PD A 1
H54A H 1.1388 0.5873 0.7366 0.227 Uiso 0.54(2) 1 calc PR A 1
H54B H 1.2327 0.5897 0.7068 0.227 Uiso 0.54(2) 1 calc PR A 1
C55 C 1.265(5) 0.605(3) 0.7933(17) 0.46(5) Uiso 0.54(2) 1 d PD A 1
H55A H 1.3098 0.5601 0.7995 0.556 Uiso 0.54(2) 1 calc PR A 1
H55B H 1.2239 0.6111 0.8229 0.556 Uiso 0.54(2) 1 calc PR A 1
C56 C 1.322(3) 0.705(3) 0.7945(19) 0.27(2) Uiso 0.54(2) 1 d PD A 1
H56A H 1.3706 0.7238 0.8268 0.407 Uiso 0.54(2) 1 calc PR A 1
H56B H 1.2780 0.7524 0.7964 0.407 Uiso 0.54(2) 1 calc PR A 1
H56C H 1.3520 0.7013 0.7610 0.407 Uiso 0.54(2) 1 calc PR A 1
C53' C 1.1904(9) 0.4554(8) 0.7222(5) 0.131(4) Uiso 0.46(2) 1 d PD A 2
H53C H 1.1575 0.4735 0.6901 0.157 Uiso 0.46(2) 1 calc PR A 2
H53D H 1.2399 0.4162 0.7100 0.157 Uiso 0.46(2) 1 calc PR A 2
C54' C 1.232(2) 0.5429(17) 0.7682(10) 0.148(11) Uiso 0.46(2) 1 d PD A 2
H54C H 1.2581 0.5216 0.8010 0.177 Uiso 0.46(2) 1 calc PR A 2
H54D H 1.1810 0.5806 0.7787 0.177 Uiso 0.46(2) 1 calc PR A 2
C55' C 1.314(3) 0.608(3) 0.751(2) 0.300 Uiso 0.46(2) 1 d PD A 2
H55C H 1.3461 0.5699 0.7226 0.360 Uiso 0.46(2) 1 calc PR A 2
H55D H 1.3611 0.6401 0.7830 0.360 Uiso 0.46(2) 1 calc PR A 2
C56' C 1.262(6) 0.684(5) 0.726(4) 0.484 Uiso 0.46(2) 1 d PD A 2
H56D H 1.3086 0.7259 0.7135 0.726 Uiso 0.46(2) 1 calc PR A 2
H56E H 1.2312 0.7216 0.7548 0.726 Uiso 0.46(2) 1 calc PR A 2
H56F H 1.2136 0.6506 0.6951 0.726 Uiso 0.46(2) 1 calc PR A 2
C57 C 0.7194(6) -0.0077(7) 0.6803(4) 0.095(3) Uani 1 1 d . . .
C58 C 0.7388(7) -0.0642(7) 0.7110(4) 0.095(3) Uani 1 1 d . . .
C59 C 0.7514(6) -0.1410(7) 0.7381(4) 0.091(2) Uani 1 1 d . . .
C60 C 0.7091(7) -0.1461(8) 0.7863(4) 0.105(3) Uani 1 1 d . . .
H60 H 0.6729 -0.0980 0.8007 0.126 Uiso 1 1 calc R . .
C61 C 0.7190(8) -0.2196(8) 0.8130(4) 0.111(3) Uani 1 1 d . . .
H61 H 0.6873 -0.2221 0.8441 0.134 Uiso 1 1 calc R . .
C62 C 0.7759(8) -0.2910(8) 0.7944(4) 0.113(3) Uani 1 1 d . . .
C63 C 0.8194(8) -0.2877(9) 0.7449(5) 0.122(3) Uani 1 1 d . . .
H63 H 0.8548 -0.3362 0.7298 0.146 Uiso 1 1 calc R . .
C64 C 0.8080(7) -0.2109(8) 0.7193(4) 0.111(3) Uani 1 1 d . . .
H64 H 0.8398 -0.2067 0.6884 0.133 Uiso 1 1 calc R . .
C65 C 0.7047(9) -0.4288(6) 0.8325(4) 0.137(5) Uani 1 1 d G . .
C66 C 0.6048(10) -0.4316(7) 0.8221(4) 0.167(6) Uani 1 1 d G . .
H66 H 0.5791 -0.3892 0.8025 0.201 Uiso 1 1 calc R . .
C67 C 0.5433(7) -0.4979(9) 0.8408(5) 0.191(6) Uani 1 1 d GU . .
H67 H 0.4764 -0.4998 0.8338 0.229 Uiso 1 1 calc R . .
C68 C 0.5816(10) -0.5614(7) 0.8699(5) 0.174(6) Uani 1 1 d G . .
H68 H 0.5405 -0.6057 0.8824 0.209 Uiso 1 1 calc R . .
C69 C 0.6816(10) -0.5585(6) 0.8804(4) 0.152(5) Uani 1 1 d GU . .
H69 H 0.7073 -0.6009 0.8999 0.182 Uiso 1 1 calc R . .
C70 C 0.7431(7) -0.4922(8) 0.8617(4) 0.149(5) Uani 1 1 d G . .
C71 C 0.8440(7) -0.4714(7) 0.8675(4) 0.165(7) Uani 1 1 d G . .
C72 C 0.8657(9) -0.3965(7) 0.8408(3) 0.146(5) Uani 1 1 d G . .
C73 C 0.9618(10) -0.3588(6) 0.8408(4) 0.153(5) Uani 1 1 d GU . .
H73 H 0.9763 -0.3087 0.8230 0.183 Uiso 1 1 calc R . .
C74 C 1.0362(7) -0.3960(8) 0.8675(5) 0.197(8) Uani 1 1 d G . .
H74 H 1.1005 -0.3709 0.8676 0.237 Uiso 1 1 calc R . .
C75 C 1.0146(8) -0.4709(9) 0.8942(4) 0.219(9) Uiso 1 1 d G . .
H75 H 1.0644 -0.4958 0.9121 0.263 Uiso 1 1 calc R . .
C76 C 0.9185(9) -0.5086(7) 0.8942(4) 0.174(5) Uani 1 1 d GU . .
H76 H 0.9040 -0.5587 0.9120 0.209 Uiso 1 1 calc R . .
C77 C 0.8124(6) 0.2428(6) 0.8218(3) 0.082(2) Uani 1 1 d . B .
C78 C 0.7994(6) 0.1996(7) 0.8589(4) 0.097(3) Uani 1 1 d . . .
C79 C 0.7973(9) 0.1680(10) 0.9086(4) 0.071(6) Uani 0.545(11) 1 d PGD B 1
C80 C 0.8560(9) 0.2223(8) 0.9569(5) 0.118(6) Uani 0.545(11) 1 d PGDU B 1
H80 H 0.8953 0.2789 0.9556 0.142 Uiso 0.545(11) 1 calc PR B 1
C81 C 0.8561(10) 0.1920(9) 1.0069(4) 0.103(5) Uani 0.545(11) 1 d PGDU B 1
H81 H 0.8955 0.2284 1.0392 0.124 Uiso 0.545(11) 1 calc PR B 1
C82 C 0.7975(11) 0.1075(10) 1.0088(4) 0.124(11) Uani 0.545(11) 1 d PGD B 1
C83 C 0.7387(10) 0.0532(9) 0.9605(6) 0.121(7) Uani 0.545(11) 1 d PGDU B 1
H83 H 0.6995 -0.0033 0.9617 0.146 Uiso 0.545(11) 1 calc PR B 1
C84 C 0.7386(8) 0.0835(10) 0.9104(4) 0.103(5) Uani 0.545(11) 1 d PGDU B 1
H84 H 0.6993 0.0472 0.8781 0.124 Uiso 0.545(11) 1 calc PR B 1
C79' C 0.7782(13) 0.1579(12) 0.9123(6) 0.113(12) Uani 0.455(11) 1 d PGD B 2
C80' C 0.7417(13) 0.2163(10) 0.9559(7) 0.128(8) Uani 0.455(11) 1 d PGDU B 2
H80' H 0.7189 0.2730 0.9510 0.154 Uiso 0.455(11) 1 calc PR B 2
C81' C 0.7392(13) 0.1898(11) 1.0070(6) 0.141(9) Uani 0.455(11) 1 d PGDU B 2
H81' H 0.7148 0.2289 1.0362 0.169 Uiso 0.455(11) 1 calc PR B 2
C82' C 0.7733(13) 0.1050(11) 1.0144(6) 0.077(7) Uani 0.455(11) 1 d PGDU B 2
C83' C 0.8098(13) 0.0466(10) 0.9708(8) 0.132(9) Uani 0.455(11) 1 d PGDU B 2
H83' H 0.8325 -0.0101 0.9758 0.158 Uiso 0.455(11) 1 calc PR B 2
C84' C 0.8122(13) 0.0731(11) 0.9197(7) 0.113(7) Uani 0.455(11) 1 d PGDU B 2
H84' H 0.8366 0.0341 0.8905 0.135 Uiso 0.455(11) 1 calc PR B 2
C85 C 0.8487(7) 0.0656(6) 1.0995(3) 0.133(4) Uani 1 1 d GU B .
C86 C 0.9469(8) 0.0766(8) 1.0940(4) 0.193(7) Uani 1 1 d G . .
H86 H 0.9672 0.0914 1.0617 0.231 Uiso 1 1 calc R B .
C87 C 1.0147(6) 0.0655(9) 1.1369(5) 0.250(9) Uani 1 1 d GU B .
H87 H 1.0804 0.0728 1.1332 0.300 Uiso 1 1 calc R . .
C88 C 0.9843(7) 0.0434(8) 1.1852(4) 0.204(7) Uani 1 1 d GU . .
H88 H 1.0297 0.0360 1.2139 0.245 Uiso 1 1 calc R B .
C89 C 0.8861(8) 0.0324(7) 1.1907(3) 0.178(5) Uani 1 1 d GU B .
H89 H 0.8658 0.0176 1.2230 0.214 Uiso 1 1 calc R . .
C90 C 0.8183(6) 0.0435(6) 1.1478(4) 0.134(4) Uani 1 1 d GU . .
C91 C 0.7191(7) 0.0336(7) 1.1370(4) 0.143(4) Uani 1 1 d G B .
C92 C 0.6948(8) 0.0571(7) 1.0858(3) 0.141(4) Uani 1 1 d G B .
C93 C 0.5982(9) 0.0591(9) 1.0665(4) 0.189(7) Uani 1 1 d G . .
H93 H 0.5819 0.0748 1.0323 0.227 Uiso 1 1 calc R B .
C94 C 0.5260(7) 0.0376(10) 1.0984(6) 0.223(9) Uani 1 1 d G B .
H94 H 0.4614 0.0389 1.0855 0.268 Uiso 1 1 calc R . .
C95 C 0.5504(9) 0.0141(10) 1.1496(5) 0.236(10) Uani 1 1 d G . .
H95 H 0.5021 -0.0003 1.1709 0.284 Uiso 1 1 calc R B .
C96 C 0.6469(10) 0.0121(8) 1.1689(3) 0.197(7) Uani 1 1 d G B .
H96 H 0.6632 -0.0037 1.2032 0.236 Uiso 1 1 calc R . .
S1 S 0.2485(4) 0.4339(4) 0.5726(2) 0.1410(19) Uiso 0.728(7) 1 d PD C 1
O1 O 0.1472(7) 0.4294(13) 0.5705(8) 0.219(7) Uiso 0.728(7) 1 d PD C 1
O2 O 0.2910(17) 0.5259(14) 0.6078(9) 0.299(11) Uiso 0.728(7) 1 d PD C 1
O3 O 0.2846(14) 0.3605(12) 0.5897(8) 0.224(7) Uiso 0.728(7) 1 d PD C 1
C97 C 0.2818(13) 0.4349(15) 0.5076(5) 0.328 Uiso 0.728(7) 1 d PD C 1
F1 F 0.3730(12) 0.4243(14) 0.5154(8) 0.279(8) Uiso 0.728(7) 1 d PD C 1
F2 F 0.2675(19) 0.5135(17) 0.4953(11) 0.381(13) Uiso 0.728(7) 1 d PD C 1
F3 F 0.2387(16) 0.3639(16) 0.4698(8) 0.338(11) Uiso 0.728(7) 1 d PD C 1
S1' S 0.3214(14) 0.4431(16) 0.6163(9) 0.214(9) Uiso 0.272(7) 1 d PD C 2
O1' O 0.269(3) 0.387(4) 0.647(2) 0.301 Uiso 0.272(7) 1 d PD C 2
O2' O 0.394(3) 0.511(3) 0.652(2) 0.45(6) Uiso 0.272(7) 1 d PD C 2
O3' O 0.360(4) 0.383(4) 0.5736(17) 0.301 Uiso 0.272(7) 1 d PD C 2
C97' C 0.2438(15) 0.5043(16) 0.5849(10) 0.075(7) Uiso 0.272(7) 1 d PD C 2
F1' F 0.2898(19) 0.5856(17) 0.5813(12) 0.169(11) Uiso 0.272(7) 1 d PD C 2
F2' F 0.178(3) 0.525(3) 0.6155(17) 0.34(3) Uiso 0.272(7) 1 d PD C 2
F3' F 0.200(2) 0.473(2) 0.5370(12) 0.215 Uiso 0.272(7) 1 d PD C 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.0689(2) 0.1012(3) 0.0704(2) 0.01629(17) 0.00954(14) 0.00735(16)
Pt2 0.0712(2) 0.0970(3) 0.0715(2) 0.01868(17) 0.01129(14) 0.00786(16)
Ag1 0.0924(4) 0.1034(5) 0.0784(4) 0.0170(3) 0.0087(3) 0.0110(3)
N1 0.073(4) 0.103(5) 0.084(5) 0.012(4) 0.012(4) -0.003(4)
N2 0.063(5) 0.211(11) 0.147(8) 0.064(8) -0.007(5) -0.006(6)
N3 0.068(4) 0.100(5) 0.074(4) 0.016(4) 0.019(3) 0.012(3)
N4 0.081(4) 0.093(5) 0.082(4) 0.010(4) 0.015(3) -0.001(3)
N5 0.072(4) 0.089(4) 0.080(4) 0.025(4) 0.016(3) 0.014(3)
N6 0.084(5) 0.100(5) 0.086(5) 0.034(4) 0.008(4) 0.014(4)
N7 0.065(4) 0.115(5) 0.087(5) 0.007(4) 0.006(3) 0.004(4)
N8 0.072(5) 0.155(8) 0.094(6) -0.012(5) 0.023(4) -0.003(5)
N9 0.171(9) 0.127(8) 0.109(7) 0.030(6) 0.007(6) 0.057(7)
N10 0.144(8) 0.129(7) 0.100(6) 0.057(5) -0.031(5) 0.001(6)
C1 0.074(6) 0.122(7) 0.092(6) 0.014(6) 0.010(5) -0.017(5)
C2 0.116(8) 0.169(10) 0.095(7) 0.053(7) 0.024(6) -0.005(7)
C3 0.111(9) 0.229(15) 0.187(13) 0.109(12) 0.051(9) -0.004(9)
C4 0.118(10) 0.224(16) 0.141(11) 0.044(11) 0.025(8) -0.051(10)
C5 0.109(9) 0.263(18) 0.141(12) 0.075(12) -0.004(8) -0.056(10)
C6 0.103(8) 0.149(10) 0.112(8) 0.027(7) 0.026(6) -0.030(7)
C7 0.073(6) 0.139(8) 0.102(7) 0.035(6) -0.008(5) -0.012(5)
C8 0.061(5) 0.133(8) 0.112(7) 0.032(6) -0.003(5) -0.020(5)
C9 0.081(5) 0.101(6) 0.075(5) 0.008(4) 0.017(4) 0.006(4)
C10 0.074(5) 0.101(6) 0.101(6) 0.028(5) 0.015(5) 0.013(4)
C11 0.096(7) 0.138(9) 0.148(10) 0.079(8) 0.012(6) 0.015(6)
C12 0.125(7) 0.165(8) 0.142(7) 0.081(7) 0.002(6) 0.013(6)
C13 0.109(8) 0.215(13) 0.141(10) 0.119(10) 0.021(7) 0.047(8)
C14 0.056(4) 0.090(5) 0.084(5) 0.009(4) 0.012(4) 0.008(4)
C15 0.061(4) 0.118(7) 0.079(5) 0.015(5) 0.019(4) 0.013(4)
C16 0.081(6) 0.190(11) 0.069(5) 0.035(6) 0.015(4) 0.037(6)
C17 0.091(6) 0.157(7) 0.091(6) 0.028(5) 0.013(5) 0.025(5)
C18 0.080(6) 0.177(11) 0.083(7) 0.001(7) -0.014(5) 0.029(7)
C19 0.078(6) 0.132(8) 0.094(7) -0.013(6) 0.022(5) -0.006(5)
C20 0.065(5) 0.118(7) 0.071(5) 0.000(5) 0.003(4) 0.015(5)
C21 0.146(11) 0.153(11) 0.139(10) -0.016(9) 0.058(9) -0.005(8)
C22 0.32(3) 0.150(14) 0.26(2) -0.098(16) 0.10(2) -0.024(15)
C23 0.149(9) 0.200(10) 0.202(10) 0.052(8) -0.036(7) 0.040(8)
C24 0.254(17) 0.255(17) 0.267(18) 0.028(14) 0.035(14) 0.080(14)
C25 0.086(6) 0.094(6) 0.128(8) 0.027(6) 0.014(5) -0.005(5)
C26 0.108(7) 0.123(7) 0.102(7) 0.026(6) 0.034(6) -0.009(6)
C27 0.120(8) 0.146(9) 0.131(9) 0.045(8) 0.022(7) -0.007(7)
C28 0.190(12) 0.232(13) 0.131(10) 0.072(10) 0.024(9) -0.017(10)
C29 0.061(4) 0.079(5) 0.084(5) 0.014(4) 0.006(4) 0.005(4)
C30 0.078(5) 0.096(6) 0.093(6) 0.028(5) 0.014(4) 0.005(4)
C31 0.097(7) 0.124(8) 0.114(8) 0.027(6) 0.031(6) 0.006(6)
C32 0.081(6) 0.139(9) 0.120(8) 0.023(7) 0.028(6) -0.002(6)
C33 0.076(6) 0.116(7) 0.113(7) 0.018(6) 0.007(5) 0.018(5)
C34 0.074(5) 0.091(5) 0.086(6) 0.011(5) 0.005(4) 0.000(4)
C35 0.081(5) 0.072(5) 0.085(5) 0.027(4) 0.016(4) 0.020(4)
C36 0.080(5) 0.095(6) 0.080(5) 0.028(5) 0.020(4) 0.006(4)
C37 0.084(5) 0.077(5) 0.073(5) 0.005(4) 0.014(4) 0.002(4)
C38 0.084(6) 0.096(6) 0.079(5) 0.000(5) 0.022(4) 0.000(5)
C39 0.101(7) 0.112(7) 0.121(8) 0.024(6) 0.036(6) -0.015(6)
C40 0.144(10) 0.110(8) 0.118(8) 0.042(6) 0.049(8) 0.005(7)
C41 0.110(7) 0.126(8) 0.115(8) 0.062(7) 0.023(6) 0.014(6)
C42 0.071(5) 0.105(6) 0.087(6) -0.003(5) 0.014(4) -0.008(5)
C43 0.086(6) 0.136(8) 0.069(5) -0.004(5) -0.009(5) 0.014(6)
C44 0.092(7) 0.185(11) 0.095(7) 0.007(7) -0.003(5) 0.042(7)
C45 0.113(9) 0.231(15) 0.120(9) 0.003(9) -0.005(7) 0.069(10)
C46 0.125(7) 0.175(8) 0.146(8) 0.007(7) 0.001(6) 0.043(7)
C47 0.101(7) 0.155(8) 0.133(7) -0.006(6) 0.011(6) 0.007(6)
C48 0.069(6) 0.175(11) 0.105(8) -0.027(8) -0.008(5) 0.020(6)
C49 0.103(7) 0.160(11) 0.117(8) 0.075(8) 0.006(6) 0.017(7)
C50 0.165(12) 0.151(11) 0.204(15) 0.107(11) -0.021(10) 0.047(9)
C51 0.228(19) 0.174(16) 0.22(2) 0.021(14) -0.039(15) 0.038(13)
C52 0.34(2) 0.210(16) 0.32(2) 0.021(15) -0.044(15) 0.092(15)
C57 0.080(5) 0.116(7) 0.069(5) -0.010(5) 0.010(4) -0.004(5)
C58 0.103(7) 0.115(7) 0.066(5) 0.024(5) 0.003(4) 0.009(5)
C59 0.087(6) 0.103(6) 0.076(5) 0.015(5) 0.002(4) 0.008(5)
C60 0.116(7) 0.115(7) 0.090(6) 0.027(6) 0.018(5) 0.028(6)
C61 0.150(9) 0.112(7) 0.081(6) 0.026(6) 0.028(6) 0.037(7)
C62 0.128(8) 0.115(8) 0.092(7) 0.019(6) 0.007(6) 0.016(6)
C63 0.140(9) 0.126(9) 0.103(8) 0.019(7) 0.020(7) 0.050(7)
C64 0.113(7) 0.123(8) 0.097(7) 0.018(6) 0.023(6) 0.017(6)
C65 0.212(16) 0.108(9) 0.095(8) 0.030(7) 0.030(9) 0.015(10)
C66 0.175(14) 0.172(13) 0.144(12) 0.033(10) 0.024(10) -0.018(11)
C67 0.207(10) 0.188(10) 0.183(10) 0.055(8) 0.040(8) 0.006(8)
C68 0.25(2) 0.127(11) 0.159(13) 0.050(9) 0.052(13) 0.021(11)
C69 0.195(9) 0.133(8) 0.131(8) 0.038(7) 0.015(7) 0.028(7)
C70 0.222(16) 0.102(9) 0.108(10) -0.015(7) 0.031(11) 0.028(10)
C71 0.272(19) 0.141(11) 0.088(8) 0.014(7) -0.015(10) 0.113(13)
C72 0.206(16) 0.150(11) 0.082(7) -0.002(7) 0.015(8) 0.084(11)
C73 0.162(8) 0.152(8) 0.138(8) 0.012(7) 0.012(7) 0.042(7)
C74 0.215(17) 0.206(17) 0.147(13) -0.040(12) 0.003(12) 0.109(14)
C76 0.212(10) 0.150(8) 0.158(9) 0.029(7) 0.018(8) 0.035(8)
C77 0.088(5) 0.089(5) 0.066(5) 0.017(4) 0.000(4) 0.010(4)
C78 0.081(6) 0.116(7) 0.096(7) 0.023(6) 0.006(5) 0.036(5)
C79 0.072(9) 0.090(15) 0.053(10) 0.029(10) -0.012(7) 0.022(9)
C80 0.135(10) 0.119(10) 0.100(9) 0.045(8) -0.002(8) -0.002(8)
C81 0.120(9) 0.105(9) 0.086(8) 0.044(7) -0.009(7) 0.004(7)
C82 0.088(14) 0.22(3) 0.063(12) 0.034(15) -0.003(10) 0.015(15)
C83 0.130(10) 0.121(10) 0.115(10) 0.036(8) 0.020(8) 0.004(8)
C84 0.101(9) 0.113(9) 0.089(8) 0.026(7) 0.003(7) -0.012(7)
C79' 0.15(2) 0.09(2) 0.11(2) 0.021(18) 0.067(19) 0.032(19)
C80' 0.139(12) 0.135(12) 0.117(11) 0.037(9) 0.032(9) 0.016(9)
C81' 0.151(13) 0.139(12) 0.143(12) 0.039(9) 0.030(9) 0.045(9)
C82' 0.081(9) 0.067(9) 0.085(11) 0.030(8) -0.001(7) 0.009(7)
C83' 0.139(12) 0.129(12) 0.132(12) 0.032(9) 0.027(9) 0.027(9)
C84' 0.125(11) 0.115(10) 0.104(10) 0.037(8) 0.014(8) 0.022(8)
C85 0.150(8) 0.118(7) 0.126(7) 0.044(6) -0.020(6) 0.006(6)
C86 0.217(17) 0.184(14) 0.184(14) 0.118(12) -0.066(12) -0.004(12)
C87 0.246(12) 0.262(12) 0.243(12) 0.092(9) -0.002(9) 0.010(9)
C88 0.206(10) 0.226(10) 0.192(10) 0.097(8) -0.016(8) 0.019(8)
C89 0.197(10) 0.181(9) 0.165(9) 0.087(7) -0.021(7) 0.010(7)
C90 0.160(8) 0.122(7) 0.119(7) 0.067(6) -0.031(6) -0.005(6)
C91 0.207(14) 0.142(10) 0.089(7) 0.064(7) -0.006(8) 0.012(9)
C92 0.202(14) 0.121(9) 0.100(8) 0.038(7) 0.007(9) 0.010(9)
C93 0.172(14) 0.29(2) 0.112(10) 0.072(11) -0.003(10) 0.024(14)
C94 0.170(15) 0.38(3) 0.172(16) 0.149(18) 0.043(12) 0.051(16)
C95 0.189(18) 0.37(3) 0.178(18) 0.129(19) 0.057(14) 0.009(18)
C96 0.29(2) 0.196(15) 0.121(11) 0.095(11) 0.009(14) 0.006(15)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 C9 1.963(9) . ?
Pt1 N3 2.025(6) . ?
Pt1 N1 2.030(7) . ?
Pt1 C57 2.054(12) . ?
Pt1 Ag1 3.1159(10) . ?
Pt2 C37 1.968(8) . ?
Pt2 C77 2.032(9) . ?
Pt2 N7 2.032(6) . ?
Pt2 N5 2.043(6) . ?
Pt2 Ag1 2.9647(9) . ?
Ag1 C57 2.187(8) . ?
Ag1 C77 2.195(8) . ?
Ag1 C58 2.466(10) . ?
Ag1 C78 2.571(10) . ?
N1 C7 1.373(12) . ?
N1 C1 1.398(11) . ?
N2 C7 1.396(12) . ?
N2 C6 1.423(15) . ?
N2 C21 1.641(16) . ?
N3 C14 1.348(10) . ?
N3 C15 1.406(10) . ?
N4 C14 1.360(9) . ?
N4 C20 1.428(11) . ?
N4 C25 1.490(11) . ?
N5 C35 1.330(10) . ?
N5 C29 1.394(10) . ?
N6 C34 1.363(11) . ?
N6 C35 1.369(10) . ?
N6 C49 1.471(11) . ?
N7 C42 1.361(11) . ?
N7 C43 1.375(9) . ?
N8 C42 1.354(11) . ?
N8 C48 1.385(12) . ?
N8 C53 1.459(14) . ?
N9 C72 1.322(12) . ?
N9 C62 1.410(14) . ?
N9 C65 1.428(14) . ?
N10 C82' 1.313(14) . ?
N10 C85 1.334(10) . ?
N10 C92 1.381(12) . ?
N10 C82 1.509(13) . ?
C1 C2 1.346(14) . ?
C1 C6 1.403(15) . ?
C2 C3 1.402(14) . ?
C2 H2 0.9300 . ?
C3 C4 1.377(18) . ?
C3 H3 0.9300 . ?
C4 C5 1.402(19) . ?
C4 H4 0.9300 . ?
C5 C6 1.359(15) . ?
C5 H5 0.9300 . ?
C7 C8 1.423(13) . ?
C8 C9 1.412(12) . ?
C8 C13 1.415(13) . ?
C9 C10 1.402(12) . ?
C10 C11 1.368(13) . ?
C10 C14 1.449(11) . ?
C11 C12 1.408(14) . ?
C11 H11 0.9300 . ?
C12 C13 1.360(15) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C15 C16 1.293(13) . ?
C15 C20 1.382(12) . ?
C16 C17 1.402(13) . ?
C16 H16 0.9300 . ?
C17 C18 1.374(15) . ?
C17 H17 0.9300 . ?
C18 C19 1.360(15) . ?
C18 H18 0.9300 . ?
C19 C20 1.402(12) . ?
C19 H19 0.9300 . ?
C21 C22 1.472(14) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.576(8) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.561(10) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.490(11) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.512(11) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.555(12) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.359(11) . ?
C29 C34 1.399(12) . ?
C30 C31 1.395(13) . ?
C30 H30 0.9300 . ?
C31 C32 1.378(15) . ?
C31 H31 0.9300 . ?
C32 C33 1.360(14) . ?
C32 H32 0.9300 . ?
C33 C34 1.431(12) . ?
C33 H33 0.9300 . ?
C35 C36 1.471(11) . ?
C36 C37 1.374(12) . ?
C36 C41 1.379(12) . ?
C37 C38 1.399(11) . ?
C38 C39 1.409(14) . ?
C38 C42 1.438(13) . ?
C39 C40 1.365(15) . ?
C39 H39 0.9300 . ?
C40 C41 1.360(14) . ?
C40 H40 0.9300 . ?
C41 H41 0.9300 . ?
C43 C44 1.3900 . ?
C43 C48 1.3900 . ?
C44 C45 1.3900 . ?
C44 H44 0.9300 . ?
C45 C46 1.3900 . ?
C45 H45 0.9300 . ?
C46 C47 1.3900 . ?
C46 H46 0.9300 . ?
C47 C48 1.3900 . ?
C47 H47 0.9300 . ?
C49 C50 1.504(17) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C50 C51 1.55(2) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C51 C52 1.43(2) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 C54 1.521(17) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 C55 1.543(17) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C55 C56 1.546(17) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C54' C55' 1.541(17) . ?
C54' H54C 0.9700 . ?
C54' H54D 0.9700 . ?
C55' C56' 1.559(17) . ?
C55' H55C 0.9700 . ?
C55' H55D 0.9700 . ?
C56' H56D 0.9600 . ?
C56' H56E 0.9600 . ?
C56' H56F 0.9600 . ?
C57 C58 1.251(13) . ?
C58 C59 1.417(13) . ?
C59 C64 1.376(13) . ?
C59 C60 1.392(13) . ?
C60 C61 1.363(13) . ?
C60 H60 0.9300 . ?
C61 C62 1.393(14) . ?
C61 H61 0.9300 . ?
C62 C63 1.427(14) . ?
C63 C64 1.391(14) . ?
C63 H63 0.9300 . ?
C64 H64 0.9300 . ?
C65 C66 1.3900 . ?
C65 C70 1.3900 . ?
C66 C67 1.3900 . ?
C66 H66 0.9300 . ?
C67 C68 1.3900 . ?
C67 H67 0.9300 . ?
C68 C69 1.3900 . ?
C68 H68 0.9300 . ?
C69 C70 1.3900 . ?
C69 H69 0.9300 . ?
C70 C71 1.395(12) . ?
C71 C72 1.3900 . ?
C71 C76 1.3900 . ?
C72 C73 1.3900 . ?
C73 C74 1.3900 . ?
C73 H73 0.9300 . ?
C74 C75 1.3900 . ?
C74 H74 0.9300 . ?
C75 C76 1.3900 . ?
C75 H75 0.9300 . ?
C76 H76 0.9300 . ?
C77 C78 1.224(12) . ?
C78 C79 1.393(14) . ?
C78 C79' 1.596(16) . ?
C79 C80 1.3900 . ?
C79 C84 1.3900 . ?
C80 C81 1.3900 . ?
C80 H80 0.9300 . ?
C81 C82 1.3900 . ?
C81 H81 0.9300 . ?
C82 C83 1.3900 . ?
C83 C84 1.3900 . ?
C83 H83 0.9300 . ?
C84 H84 0.9300 . ?
C79' C80' 1.3900 . ?
C79' C84' 1.3900 . ?
C80' C81' 1.3900 . ?
C80' H80' 0.9300 . ?
C81' C82' 1.3900 . ?
C81' H81' 0.9300 . ?
C82' C83' 1.3900 . ?
C83' C84' 1.3900 . ?
C83' H83' 0.9300 . ?
C84' H84' 0.9300 . ?
C85 C86 1.3900 . ?
C85 C90 1.3900 . ?
C86 C87 1.3900 . ?
C86 H86 0.9300 . ?
C87 C88 1.3900 . ?
C87 H87 0.9300 . ?
C88 C89 1.3900 . ?
C88 H88 0.9300 . ?
C89 C90 1.3900 . ?
C89 H89 0.9300 . ?
C90 C91 1.371(12) . ?
C91 C92 1.3900 . ?
C91 C96 1.3900 . ?
C92 C93 1.3900 . ?
C93 C94 1.3900 . ?
C93 H93 0.9300 . ?
C94 C95 1.3900 . ?
C94 H94 0.9300 . ?
C95 C96 1.3900 . ?
C95 H95 0.9300 . ?
C96 H96 0.9300 . ?
S1 O3 1.339(13) . ?
S1 O1 1.407(8) . ?
S1 O2 1.428(15) . ?
S1 C97 1.716(10) . ?
C97 F2 1.255(16) . ?
C97 F3 1.259(16) . ?
C97 F1 1.302(9) . ?
S1' O2' 1.395(17) . ?
S1' O3' 1.403(17) . ?
S1' O1' 1.403(17) . ?
S1' C97' 1.694(19) . ?
C97' F3' 1.235(17) . ?
C97' F2' 1.270(17) . ?
C97' F1' 1.285(17) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 Pt1 N3 79.5(3) . . ?
C9 Pt1 N1 79.4(3) . . ?
N3 Pt1 N1 158.9(3) . . ?
C9 Pt1 C57 176.0(3) . . ?
N3 Pt1 C57 101.5(3) . . ?
N1 Pt1 C57 99.5(3) . . ?
C9 Pt1 Ag1 139.6(2) . . ?
N3 Pt1 Ag1 86.91(19) . . ?
N1 Pt1 Ag1 109.5(2) . . ?
C57 Pt1 Ag1 44.4(2) . . ?
C37 Pt2 C77 176.1(3) . . ?
C37 Pt2 N7 79.0(3) . . ?
C77 Pt2 N7 100.2(3) . . ?
C37 Pt2 N5 78.9(3) . . ?
C77 Pt2 N5 101.9(3) . . ?
N7 Pt2 N5 157.9(3) . . ?
C37 Pt2 Ag1 136.1(2) . . ?
C77 Pt2 Ag1 47.8(2) . . ?
N7 Pt2 Ag1 109.7(2) . . ?
N5 Pt2 Ag1 85.99(19) . . ?
C57 Ag1 C77 173.0(4) . . ?
C57 Ag1 C58 30.4(3) . . ?
C77 Ag1 C58 156.5(3) . . ?
C57 Ag1 C78 158.3(4) . . ?
C77 Ag1 C78 28.4(3) . . ?
C58 Ag1 C78 129.6(3) . . ?
C57 Ag1 Pt2 129.9(3) . . ?
C77 Ag1 Pt2 43.2(2) . . ?
C58 Ag1 Pt2 155.7(2) . . ?
C78 Ag1 Pt2 71.6(2) . . ?
C57 Ag1 Pt1 41.1(3) . . ?
C77 Ag1 Pt1 132.0(2) . . ?
C58 Ag1 Pt1 71.5(2) . . ?
C78 Ag1 Pt1 155.2(2) . . ?
Pt2 Ag1 Pt1 91.73(3) . . ?
C7 N1 C1 109.7(8) . . ?
C7 N1 Pt1 113.0(6) . . ?
C1 N1 Pt1 137.4(7) . . ?
C7 N2 C6 107.9(9) . . ?
C7 N2 C21 125.9(10) . . ?
C6 N2 C21 125.3(9) . . ?
C14 N3 C15 108.3(6) . . ?
C14 N3 Pt1 113.9(5) . . ?
C15 N3 Pt1 137.8(6) . . ?
C14 N4 C20 107.0(7) . . ?
C14 N4 C25 127.2(8) . . ?
C20 N4 C25 125.4(7) . . ?
C35 N5 C29 108.8(7) . . ?
C35 N5 Pt2 114.2(5) . . ?
C29 N5 Pt2 136.7(6) . . ?
C34 N6 C35 106.6(7) . . ?
C34 N6 C49 125.7(8) . . ?
C35 N6 C49 127.6(7) . . ?
C42 N7 C43 107.6(7) . . ?
C42 N7 Pt2 114.4(6) . . ?
C43 N7 Pt2 137.8(6) . . ?
C42 N8 C48 108.2(8) . . ?
C42 N8 C53 125.7(11) . . ?
C48 N8 C53 125.8(9) . . ?
C72 N9 C62 127.8(12) . . ?
C72 N9 C65 108.0(10) . . ?
C62 N9 C65 123.9(10) . . ?
C82' N10 C85 135.0(12) . . ?
C82' N10 C92 121.3(11) . . ?
C85 N10 C92 103.4(8) . . ?
C85 N10 C82 122.0(10) . . ?
C92 N10 C82 134.5(9) . . ?
C2 C1 N1 132.2(9) . . ?
C2 C1 C6 120.4(9) . . ?
N1 C1 C6 107.4(10) . . ?
C1 C2 C3 115.1(11) . . ?
C1 C2 H2 122.5 . . ?
C3 C2 H2 122.5 . . ?
C4 C3 C2 122.8(13) . . ?
C4 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
C3 C4 C5 123.4(12) . . ?
C3 C4 H4 118.3 . . ?
C5 C4 H4 118.3 . . ?
C6 C5 C4 111.1(13) . . ?
C6 C5 H5 124.5 . . ?
C4 C5 H5 124.5 . . ?
C5 C6 C1 127.2(13) . . ?
C5 C6 N2 125.7(13) . . ?
C1 C6 N2 107.1(9) . . ?
N1 C7 N2 107.9(9) . . ?
N1 C7 C8 119.3(8) . . ?
N2 C7 C8 132.8(10) . . ?
C9 C8 C13 119.9(9) . . ?
C9 C8 C7 108.6(9) . . ?
C13 C8 C7 131.5(9) . . ?
C10 C9 C8 121.1(9) . . ?
C10 C9 Pt1 119.1(7) . . ?
C8 C9 Pt1 119.6(6) . . ?
C11 C10 C9 118.9(9) . . ?
C11 C10 C14 132.0(9) . . ?
C9 C10 C14 109.1(8) . . ?
C10 C11 C12 118.8(10) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
C13 C12 C11 124.6(11) . . ?
C13 C12 H12 117.7 . . ?
C11 C12 H12 117.7 . . ?
C12 C13 C8 116.4(10) . . ?
C12 C13 H13 121.8 . . ?
C8 C13 H13 121.8 . . ?
N3 C14 N4 110.3(7) . . ?
N3 C14 C10 118.3(7) . . ?
N4 C14 C10 131.4(8) . . ?
C16 C15 C20 120.1(8) . . ?
C16 C15 N3 132.5(9) . . ?
C20 C15 N3 107.4(8) . . ?
C15 C16 C17 120.3(10) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C18 C17 C16 118.6(10) . . ?
C18 C17 H17 120.7 . . ?
C16 C17 H17 120.7 . . ?
C19 C18 C17 123.4(10) . . ?
C19 C18 H18 118.3 . . ?
C17 C18 H18 118.3 . . ?
C18 C19 C20 114.1(10) . . ?
C18 C19 H19 123.0 . . ?
C20 C19 H19 123.0 . . ?
C15 C20 C19 123.2(9) . . ?
C15 C20 N4 107.1(7) . . ?
C19 C20 N4 129.6(9) . . ?
C22 C21 N2 102.2(10) . . ?
C22 C21 H21A 111.3 . . ?
N2 C21 H21A 111.3 . . ?
C22 C21 H21B 111.3 . . ?
N2 C21 H21B 111.3 . . ?
H21A C21 H21B 109.2 . . ?
C21 C22 C23 104.6(11) . . ?
C21 C22 H22A 110.8 . . ?
C23 C22 H22A 110.8 . . ?
C21 C22 H22B 110.8 . . ?
C23 C22 H22B 110.8 . . ?
H22A C22 H22B 108.9 . . ?
C24 C23 C22 105.1(11) . . ?
C24 C23 H23A 110.7 . . ?
C22 C23 H23A 110.7 . . ?
C24 C23 H23B 110.7 . . ?
C22 C23 H23B 110.7 . . ?
H23A C23 H23B 108.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N4 C25 C26 112.1(7) . . ?
N4 C25 H25A 109.2 . . ?
C26 C25 H25A 109.2 . . ?
N4 C25 H25B 109.2 . . ?
C26 C25 H25B 109.2 . . ?
H25A C25 H25B 107.9 . . ?
C25 C26 C27 114.2(9) . . ?
C25 C26 H26A 108.7 . . ?
C27 C26 H26A 108.7 . . ?
C25 C26 H26B 108.7 . . ?
C27 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
C26 C27 C28 109.3(10) . . ?
C26 C27 H27A 109.8 . . ?
C28 C27 H27A 109.8 . . ?
C26 C27 H27B 109.8 . . ?
C28 C27 H27B 109.8 . . ?
H27A C27 H27B 108.3 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 N5 133.6(8) . . ?
C30 C29 C34 121.3(8) . . ?
N5 C29 C34 105.1(7) . . ?
C29 C30 C31 117.8(9) . . ?
C29 C30 H30 121.1 . . ?
C31 C30 H30 121.1 . . ?
C32 C31 C30 121.6(10) . . ?
C32 C31 H31 119.2 . . ?
C30 C31 H31 119.2 . . ?
C33 C32 C31 122.0(10) . . ?
C33 C32 H32 119.0 . . ?
C31 C32 H32 119.0 . . ?
C32 C33 C34 116.7(10) . . ?
C32 C33 H33 121.6 . . ?
C34 C33 H33 121.6 . . ?
N6 C34 C29 109.2(7) . . ?
N6 C34 C33 130.3(9) . . ?
C29 C34 C33 120.5(9) . . ?
N5 C35 N6 110.1(7) . . ?
N5 C35 C36 117.6(7) . . ?
N6 C35 C36 132.3(8) . . ?
C37 C36 C41 118.7(8) . . ?
C37 C36 C35 109.6(7) . . ?
C41 C36 C35 131.7(9) . . ?
C36 C37 C38 121.1(8) . . ?
C36 C37 Pt2 119.6(6) . . ?
C38 C37 Pt2 119.3(7) . . ?
C37 C38 C39 119.0(9) . . ?
C37 C38 C42 109.9(8) . . ?
C39 C38 C42 131.0(9) . . ?
C40 C39 C38 118.2(9) . . ?
C40 C39 H39 120.9 . . ?
C38 C39 H39 120.9 . . ?
C41 C40 C39 122.2(10) . . ?
C41 C40 H40 118.9 . . ?
C39 C40 H40 118.9 . . ?
C40 C41 C36 120.7(10) . . ?
C40 C41 H41 119.6 . . ?
C36 C41 H41 119.6 . . ?
N8 C42 N7 109.4(9) . . ?
N8 C42 C38 133.2(9) . . ?
N7 C42 C38 117.4(8) . . ?
N7 C43 C44 131.9(6) . . ?
N7 C43 C48 108.1(6) . . ?
C44 C43 C48 120.0 . . ?
C43 C44 C45 120.0 . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C46 C45 C44 120.0 . . ?
C46 C45 H45 120.0 . . ?
C44 C45 H45 120.0 . . ?
C45 C46 C47 120.0 . . ?
C45 C46 H46 120.0 . . ?
C47 C46 H46 120.0 . . ?
C48 C47 C46 120.0 . . ?
C48 C47 H47 120.0 . . ?
C46 C47 H47 120.0 . . ?
C47 C48 C43 120.0 . . ?
C47 C48 N8 133.2(6) . . ?
C43 C48 N8 106.7(6) . . ?
N6 C49 C50 109.8(9) . . ?
N6 C49 H49A 109.7 . . ?
C50 C49 H49A 109.7 . . ?
N6 C49 H49B 109.7 . . ?
C50 C49 H49B 109.7 . . ?
H49A C49 H49B 108.2 . . ?
C49 C50 C51 117.8(14) . . ?
C49 C50 H50A 107.8 . . ?
C51 C50 H50A 107.8 . . ?
C49 C50 H50B 107.8 . . ?
C51 C50 H50B 107.8 . . ?
H50A C50 H50B 107.2 . . ?
C52 C51 C50 111(2) . . ?
C52 C51 H51A 109.5 . . ?
C50 C51 H51A 109.5 . . ?
C52 C51 H51B 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 108.1 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N8 C53 C54 117.6(16) . . ?
N8 C53 H53A 107.9 . . ?
C54 C53 H53A 107.9 . . ?
N8 C53 H53B 107.9 . . ?
C54 C53 H53B 107.9 . . ?
H53A C53 H53B 107.2 . . ?
C53 C54 C55 108(2) . . ?
C53 C54 H54A 110.0 . . ?
C55 C54 H54A 110.0 . . ?
C53 C54 H54B 110.0 . . ?
C55 C54 H54B 110.0 . . ?
H54A C54 H54B 108.4 . . ?
C54 C55 C56 109(2) . . ?
C54 C55 H55A 109.8 . . ?
C56 C55 H55A 109.8 . . ?
C54 C55 H55B 109.9 . . ?
C56 C55 H55B 109.9 . . ?
H55A C55 H55B 108.3 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55' C54' H54C 109.1 . . ?
C55' C54' H54D 109.1 . . ?
H54C C54' H54D 107.8 . . ?
C54' C55' C56' 105(2) . . ?
C54' C55' H55C 110.7 . . ?
C56' C55' H55C 110.7 . . ?
C54' C55' H55D 110.7 . . ?
C56' C55' H55D 110.7 . . ?
H55C C55' H55D 108.8 . . ?
C55' C56' H56D 109.5 . . ?
C55' C56' H56E 109.5 . . ?
H56D C56' H56E 109.5 . . ?
C55' C56' H56F 109.5 . . ?
H56D C56' H56F 109.5 . . ?
H56E C56' H56F 109.5 . . ?
C58 C57 Pt1 176.7(8) . . ?
C58 C57 Ag1 87.2(6) . . ?
Pt1 C57 Ag1 94.5(4) . . ?
C57 C58 C59 170.0(9) . . ?
C57 C58 Ag1 62.4(6) . . ?
C59 C58 Ag1 127.3(6) . . ?
C64 C59 C60 117.5(10) . . ?
C64 C59 C58 121.9(9) . . ?
C60 C59 C58 120.5(9) . . ?
C61 C60 C59 121.9(10) . . ?
C61 C60 H60 119.0 . . ?
C59 C60 H60 119.0 . . ?
C60 C61 C62 121.1(10) . . ?
C60 C61 H61 119.4 . . ?
C62 C61 H61 119.4 . . ?
C61 C62 N9 122.5(10) . . ?
C61 C62 C63 117.9(10) . . ?
N9 C62 C63 119.4(10) . . ?
C64 C63 C62 118.8(10) . . ?
C64 C63 H63 120.6 . . ?
C62 C63 H63 120.6 . . ?
C59 C64 C63 122.5(10) . . ?
C59 C64 H64 118.8 . . ?
C63 C64 H64 118.8 . . ?
C66 C65 C70 120.0 . . ?
C66 C65 N9 133.2(10) . . ?
C70 C65 N9 106.8(10) . . ?
C65 C66 C67 120.0 . . ?
C65 C66 H66 120.0 . . ?
C67 C66 H66 120.0 . . ?
C66 C67 C68 120.0 . . ?
C66 C67 H67 120.0 . . ?
C68 C67 H67 120.0 . . ?
C69 C68 C67 120.0 . . ?
C69 C68 H68 120.0 . . ?
C67 C68 H68 120.0 . . ?
C70 C69 C68 120.0 . . ?
C70 C69 H69 120.0 . . ?
C68 C69 H69 120.0 . . ?
C69 C70 C65 120.0 . . ?
C69 C70 C71 132.3(10) . . ?
C65 C70 C71 107.6(10) . . ?
C72 C71 C76 120.0 . . ?
C72 C71 C70 107.1(10) . . ?
C76 C71 C70 132.8(10) . . ?
N9 C72 C71 110.4(10) . . ?
N9 C72 C73 129.6(10) . . ?
C71 C72 C73 120.0 . . ?
C74 C73 C72 120.0 . . ?
C74 C73 H73 120.0 . . ?
C72 C73 H73 120.0 . . ?
C75 C74 C73 120.0 . . ?
C75 C74 H74 120.0 . . ?
C73 C74 H74 120.0 . . ?
C76 C75 C74 120.0 . . ?
C76 C75 H75 120.0 . . ?
C74 C75 H75 120.0 . . ?
C75 C76 C71 120.0 . . ?
C75 C76 H76 120.0 . . ?
C71 C76 H76 120.0 . . ?
C78 C77 Pt2 177.8(8) . . ?
C78 C77 Ag1 93.1(7) . . ?
Pt2 C77 Ag1 89.0(3) . . ?
C77 C78 C79 167.6(11) . . ?
C77 C78 C79' 171.5(11) . . ?
C79 C78 C79' 9.6(9) . . ?
C77 C78 Ag1 58.5(6) . . ?
C79 C78 Ag1 133.2(8) . . ?
C79' C78 Ag1 128.5(8) . . ?
C80 C79 C84 120.0 . . ?
C80 C79 C78 118.7(9) . . ?
C84 C79 C78 121.3(9) . . ?
C81 C80 C79 120.0 . . ?
C81 C80 H80 120.0 . . ?
C79 C80 H80 120.0 . . ?
C80 C81 C82 120.0 . . ?
C80 C81 H81 120.0 . . ?
C82 C81 H81 120.0 . . ?
C83 C82 C81 120.0 . . ?
C83 C82 N10 114.0(9) . . ?
C81 C82 N10 125.2(9) . . ?
C84 C83 C82 120.0 . . ?
C84 C83 H83 120.0 . . ?
C82 C83 H83 120.0 . . ?
C83 C84 C79 120.0 . . ?
C83 C84 H84 120.0 . . ?
C79 C84 H84 120.0 . . ?
C80' C79' C84' 120.0 . . ?
C80' C79' C78 118.7(11) . . ?
C84' C79' C78 120.2(11) . . ?
C79' C80' C81' 120.0 . . ?
C79' C80' H80' 120.0 . . ?
C81' C80' H80' 120.0 . . ?
C80' C81' C82' 120.0 . . ?
C80' C81' H81' 120.0 . . ?
C82' C81' H81' 120.0 . . ?
N10 C82' C83' 115.5(12) . . ?
N10 C82' C81' 124.4(12) . . ?
C83' C82' C81' 120.0 . . ?
C82' C83' C84' 120.0 . . ?
C82' C83' H83' 120.0 . . ?
C84' C83' H83' 120.0 . . ?
C83' C84' C79' 120.0 . . ?
C83' C84' H84' 120.0 . . ?
C79' C84' H84' 120.0 . . ?
N10 C85 C86 125.3(9) . . ?
N10 C85 C90 114.7(9) . . ?
C86 C85 C90 120.0 . . ?
C85 C86 C87 120.0 . . ?
C85 C86 H86 120.0 . . ?
C87 C86 H86 120.0 . . ?
C86 C87 C88 120.0 . . ?
C86 C87 H87 120.0 . . ?
C88 C87 H87 120.0 . . ?
C87 C88 C89 120.0 . . ?
C87 C88 H88 120.0 . . ?
C89 C88 H88 120.0 . . ?
C90 C89 C88 120.0 . . ?
C90 C89 H89 120.0 . . ?
C88 C89 H89 120.0 . . ?
C91 C90 C89 136.5(8) . . ?
C91 C90 C85 103.4(8) . . ?
C89 C90 C85 120.0 . . ?
C90 C91 C92 108.2(8) . . ?
C90 C91 C96 131.6(8) . . ?
C92 C91 C96 120.0 . . ?
N10 C92 C91 110.1(8) . . ?
N10 C92 C93 129.9(8) . . ?
C91 C92 C93 120.0 . . ?
C92 C93 C94 120.0 . . ?
C92 C93 H93 120.0 . . ?
C94 C93 H93 120.0 . . ?
C95 C94 C93 120.0 . . ?
C95 C94 H94 120.0 . . ?
C93 C94 H94 120.0 . . ?
C96 C95 C94 120.0 . . ?
C96 C95 H95 120.0 . . ?
C94 C95 H95 120.0 . . ?
C95 C96 C91 120.0 . . ?
C95 C96 H96 120.0 . . ?
C91 C96 H96 120.0 . . ?
O3 S1 O1 114.4(11) . . ?
O3 S1 O2 111.8(12) . . ?
O1 S1 O2 107.2(11) . . ?
O3 S1 C97 107.6(10) . . ?
O1 S1 C97 110.2(10) . . ?
O2 S1 C97 105.3(11) . . ?
F2 C97 F3 110.6(17) . . ?
F2 C97 F1 114.0(18) . . ?
F3 C97 F1 108.1(16) . . ?
F2 C97 S1 109.4(15) . . ?
F3 C97 S1 113.0(15) . . ?
F1 C97 S1 101.5(12) . . ?
O2' S1' O3' 111(2) . . ?
O2' S1' O1' 111(2) . . ?
O3' S1' O1' 110(2) . . ?
O2' S1' C97' 108(2) . . ?
O3' S1' C97' 107.4(19) . . ?
O1' S1' C97' 108.6(18) . . ?
F3' C97' F2' 105(2) . . ?
F3' C97' F1' 102(2) . . ?
F2' C97' F1' 106(2) . . ?
F3' C97' S1' 124(2) . . ?
F2' C97' S1' 110(2) . . ?
F1' C97' S1' 109.2(17) . . ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 25.03
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 1.378
_refine_diff_density_min -0.863
_refine_diff_density_rms 0.103
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 1.000 598 105 ' '
_platon_squeeze_details
;
There is about 598 cubic Angstroms of solvent accessible void volume in
the crystal lattice.
Attempts to model the void with dichloromethane or diethyl ether
(the recrystallization solvent) were not successful. As a result, the
PLATON-SQUEEZE routine was run and the .hkp file obtained containing
the solvent free reflection data was renamed to .hkl file. the SHELXL
refinement was continued with the disordered solvent free .ins file.
After least-square convergence, PLATON was run again with the new .hkl
and .res files with the instruction 'CALC FCF' in order to produce
a proper final FoFc-CIF on a file with extension .hkp which was then
renamed to extension .fcf.
The .sqf file produced by PLATON which details the SQUEEZE results was
appended to the CIF here.
;
# start Validation Reply Form
_vrf_PLAT234_wt1945w-shelxl
;
PROBLEM: Large Hirshfeld Difference N9 -- C65 .. 0.19 Ang.
Large Hirshfeld Difference C1 -- C6 .. 0.21 Ang.
Large Hirshfeld Difference C8 -- C13 .. 0.23 Ang.
Large Hirshfeld Difference C18 -- C19 .. 0.20 Ang.
Large Hirshfeld Difference C27 -- C28 .. 0.22 Ang.
Large Hirshfeld Difference C43 -- C44 .. 0.18 Ang.
Large Hirshfeld Difference C47 -- C48 .. 0.20 Ang.
Large Hirshfeld Difference C65 -- C70 .. 0.20 Ang.
Large Hirshfeld Difference C67 -- C68 .. 0.21 Ang.
Large Hirshfeld Difference C68 -- C69 .. 0.25 Ang.
Large Hirshfeld Difference C72 -- C73 .. 0.24 Ang.
Large Hirshfeld Difference C77 -- C78 .. 0.18 Ang.
Large Hirshfeld Difference C78 -- C79 .. 0.23 Ang.
Large Hirshfeld Difference C79 -- C80 .. 0.21 Ang.
Large Hirshfeld Difference C87 -- C88 .. 0.22 Ang.
Large Hirshfeld Difference C89 -- C90 .. 0.20 Ang.
Large Hirshfeld Difference C90 -- C91 .. 0.22 Ang.
Large Hirshfeld Difference C91 -- C92 .. 0.18 Ang.
Large Hirshfeld Difference C91 -- C96 .. 0.20 Ang.
RESPONSE: Due to the data quality collected at ambient temperature of
301 K and also the disorder of the butyl groups and some phenyl rings,
large Hirshfeld difference was found for various atom pairs.
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_vrf_PLAT241_wt1945w-shelxl
;
PROBLEM: Check High Ueq as Compared to Neighbors for C3
Check High Ueq as Compared to Neighbors for C5
Check High Ueq as Compared to Neighbors for C13
Check High Ueq as Compared to Neighbors for C45
Check High Ueq as Compared to Neighbors for C67
Check High Ueq as Compared to Neighbors for C95
RESPONSE: Due to the data quality collected at ambient temperature of
301 K and also the disorder of the butyl groups and some phenyl rings,
large Hirshfeld difference was found for various atom pairs.
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_vrf_PLAT920_wt1945w-shelxl
;
PROBLEM: Theta(Max) in CIF and FCF Differ by ........... 2.46 Deg.
RESPONSE:
Due to the data quality, the solvent in the lattice could not be
successfully located, thus the PLATON-SQUEEZE routine was used.
Following the procedure suggested, the FCF file was generated from the
RES and HKL file. May be due to this reason, that there is a discrepancies
in the theta(max) values in CIF and FCF files.
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_vrf_PLAT201_wt1945w-shelxl
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PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 5
RESPONSE: The atoms in the butyl group, C53, C54, C55, C56 and C75 were only
refined isotropically.
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_vrf_PLAT202_wt1945w-shelxl
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PROBLEM: Isotropic non-H Atoms in Anion/Solvent ......... 8
RESPONSE: The atoms in the triflate anion, S1, C97, O1-O3, F1-F3 were only
refined isotropically (some with fixed thermal parameters) because the
anion was seriously disordered.
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_vrf_PLAT220_wt1945w-shelxl
;
PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.9 Ratio
RESPONSE:
;
_vrf_PLAT230_wt1945w-shelxl
;
PROBLEM: Hirshfeld Test Diff for C17 -- C18 .. 5.1 su
Hirshfeld Test Diff for N2 -- C21 .. 8.4 su
Hirshfeld Test Diff for C22 -- C23 .. 16.5 su
Hirshfeld Test Diff for C50 -- C51 .. 7.0 su
Hirshfeld Test Diff for C57 -- C58 .. 6.3 su
Hirshfeld Test Diff for C85 -- C86 .. 5.4 su
Hirshfeld Test Diff for C86 -- C87 .. 6.4 su
RESPONSE: Due to the data quality collected at ambient temperature of
301 K and also the disorder of the butyl groups and some phenyl rings,
large Hirshfeld difference was found for various atom pairs.
;
_vrf_PLAT242_wt1945w-shelxl
;
PROBLEM: Check Low Ueq as Compared to Neighbors for C27
Check Low Ueq as Compared to Neighbors for C51
Check Low Ueq as Compared to Neighbors for C53
Check Low Ueq as Compared to Neighbors for C54
Check Low Ueq as Compared to Neighbors for C54'
Check Low Ueq as Compared to Neighbors for C55'
Check Low Ueq as Compared to Neighbors for C73
Check Low Ueq as Compared to Neighbors for C76
Check Low Ueq as Compared to Neighbors for C79
Check Low Ueq as Compared to Neighbors for C81
Check Low Ueq as Compared to Neighbors for C82'
Check Low Ueq as Compared to Neighbors for C85
Check Low Ueq as Compared to Neighbors for C90
Check Low Ueq as Compared to Neighbors for C23
RESPONSE: Due to the data quality collected at ambient temperature of
301 K and also the disorder of the butyl groups and some phenyl rings,
large Hirshfeld difference was found for various atom pairs.
;
_vrf_PLAT366_wt1945w-shelxl
;
PROBLEM: Short? C(sp?)-C(sp?) Bond C77 - C78 ... 1.22 Ang.
RESPONSE: C-77-C78 is a triple, C(sp)-C(sp), bond.
;
_vrf_PLAT413_wt1945w-shelxl
;
PROBLEM: Short Inter XH3 .. XHn H3 .. H56A .. 2.00 Ang.
RESPONSE: The H56 was disordered, so the short contact may not
actually exist.
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_vrf_PLAT934_wt1945w-shelxl
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW .gt. 10 Outliers . 6
RESPONSE:
;
_vrf_PLAT919_wt1945w-shelxl
;
PROBLEM: Reflection # Likely Affected by the Beamstop ... 1
RESPONSE:
;
_vrf_PLAT953_wt1945w-shelxl
;
PROBLEM: Reported and Actual Hmax Values in FCF Differ by 2
RESPONSE: Due to the data quality, the solvent in the lattice could not be
successfully located, thus the PLATON-SQUEEZE routine was used.
Following the procedure suggested, the FCF file was generated from the
RES and HKL file. May be due to this reason, that there is a discrepancies
of 2 in the Reported and Actual Hmax Values in FCF.
;
_vrf_PLAT954_wt1945w-shelxl
;
PROBLEM: Reported and Actual Kmax Values in FCF Differ by 2
RESPONSE: Due to the data quality, the solvent in the lattice could not be
successfully located, thus the PLATON-SQUEEZE routine was used.
Following the procedure suggested, the FCF file was generated from the
RES and HKL file. May be due to this reason, that there is a discrepancies
of 2 in the Reported and Actual Kmax Values in FCF.
;
_vrf_PLAT955_wt1945w-shelxl
;
PROBLEM: Reported and Actual Lmax Values in FCF Differ by 2
RESPONSE: Due to the data quality, the solvent in the lattice could not be
successfully located, thus the PLATON-SQUEEZE routine was used.
Following the procedure suggested, the FCF file was generated from the
RES and HKL file.
May be due to this reason, that there is a discrepancies
of 2 in the Reported and Actual Lmax Values in FCF.
;
_vrf_PLAT072_wt1945w-shelxl
;
PROBLEM: SHELXL First Parameter in WGHT Unusually Large. 0.11
RESPONSE:
The p4p file (with 264 reflections) has been submitted for Cell_now check,
however, 248 reflections were assigned to the same domain. This seems to
suggest no significant twinning detected.
;
_vrf_PLAT432_wt1945w-shelxl
;
PROBLEM: Short Inter X...Y Contact C24 .. C24 .. 3.00 Ang.
RESPONSE:
;
_vrf_PLAT606_wt1945w-shelxl
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure !
RESPONSE: Due to the data quality, the solvent in the lattice could not be
successfully located, thus the PLATON-SQUEEZE routine was used to remove
the structure factor effect from the disordered solvents.
;
_vrf_PLAT860_wt1945w-shelxl
;
PROBLEM: Note: Number of Least-Squares Restraints ....... 311
RESPONSE: Due to the data quality at room temperature, or the large mosacity
of the crystal, most of the phenyl rings seems to have some rocking or
swinging motion, and the butyl group tends to be disordered.
As a result, in order to stabilize the refinement, a lot of restraints
(311 in total) have been used.
;
_vrf_PLAT002_wt1945w-shelxl
;
PROBLEM: Number of Distance or Angle Restraints on AtSite 44
RESPONSE: The 44 atoms are C21-C28 (8), C53-C56 (4), C53'-C56' (4),
C79-C84 (6), C79'-C84' (6), the triflate ion, S1/O1-O3/C97/F1-F3 (8),
S1'/O1'-O3'/C97'/F1'-F3'(8).
These atoms have to be restrained for better modeling.
;
_vrf_PLAT003_wt1945w-shelxl
;
PROBLEM: Number of Uiso or Uij Restrained Atom Sites .... 26
RESPONSE:
The 26 atoms: C12 C17 C23 C24 C28 C46 C47 C52 C67 C69 C73 C76 C80 C80' C81
C81' C82' C83 C83' C84 C84' C85 C87 C88 C89 & C90, were refined with
isotropic restraints with standard uncertainty of 0.01, 6 restraints
for each atoms (i.e. 156 restraints in total.)
;
_vrf_PLAT_wt1945w-shelxl
;
PROBLEM:
RESPONSE:
;