новая папка 1 / 220880
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2013. 54, 2 |
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. 317 – 322 |
541.49:549.251:548.737
(IV)
. . 1, . . 2, . . 1, . . !2
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E-mail: ngolovnev@sfu-kras.ru |
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. . . ! " #$%, |
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13 2012 !. |
— 18 & 2012 !. |
EnrH3[SnBr3,46Cl2,54] H2O, EnrH32 — - ! " (C19H24FN3O32 ) # $ % " & ' " " ' ' .$% * &$ + & / (IV) - ! ": a = 17,1262(19), b = 10,3435(11), = 17,2582(19) Å, = 119,203(1) , V = = 2640,5(4) Å3, # . $. P21/c, Z = 4. < * " + '> '> /&- '> ?, " * " EnrH32 , [SnBr3,46Cl2,54]2– & ' * *. ' ' A +-— -& D & & % / ! EnrH32 .
" # $ % : % " ' ' , ! ", + & / (IV), * " .
<$& % " " " & ? D D % ?> . G ?J $ $
& '+ ( 93 &$/$), $"/ ( 12 &$/$) "/ ( 1,4 &$/$). / -A ' %$ & $, * " ? */ &- , # + ' ? # ! * . K$ " # ? '> '+ */ # /, # - % A '/ , % $ & ! % / # # #- */ [ 1, 2 ]. # " ? & J$*/ / +- & */ Sn(IV) [ 3 ]. < # " " # " " * - " ' ' */ + D, ! D # + +$% D$% / D. & & & '% * * +$% - *& $& , % # "& A$ % / +-— / & , " */ * +L ' '> . < # ? / * * * > # *J *D '%$ +L +$" # % &' & ? *& # &. D ? , / — A *D J$ # [ 4 ].
M & D & D ' # J D $'##* % / + " " " - ! (C19H22FN3O3 — 1-! # #-7-(4-# #-1-)-6- -4- -1,4- - $/-3-+ " , EnrH). / ' " J & # & # + ?J$ " $& ! ? */ $ A ? */ + D, >% " ' D%-
* -& *& + & ' ? & &. # ? ' " " % " ! D &- %$ , # , % / + D, # , A */ */ - ! D [ 5 ]. P ! # *& / % # & " ? " - % " & %$ */ ?$ , A */ ! D. J # & " " # #-&" & J D # !* " + ?+* # *& J % *& ! "& [ 6 ].
© Q R . ., . ., Q R . ., Q 'L Q. ., 2013
Copyright ОАО «ЦКБ «БИБКОМ» & ООО «Aгентство Kнига-Cервис»
318 |
. . Q < T<, . . KK<, . . Q < T< , Q. . Q UK |
< "L D + + & / (IV) ! " EnrH3[SnBr3,46Cl2,54] H2O # $ % " ' ' .
& ' '
< + # ? * '>L $*: ! (Fluka, A -
$ L 98 %), HBr ( X), SnCl4 5H2O ( X).
* + - C19H24FN3O3[SnBr3,46Cl2,54] H2O (1). 0,2 $ EnrH " 3 & !- D HBr. < # '% *D A *D + " 0,2 $ SnCl4 5H2O. " J EnrH:SnCl4 = 1:1. % + " +-A *D # + *D , *D #- J # # A ? & " D # % D & D +-A *D - , $ ? , # &* ! & 'J ? '/ # " D &- *. -A * & * " * " ? # # ? .
. $ $% D # & # & ? & &'/ *& & SMART APEXII # ? & & / &$ MoK -'% ", = 0,7106 Å. * # '% * # 100 K ! ?> ' % " - D * '$*/ .
* $% / # & * # & * + . 1. % #$L " $/ '% D & D - */ . M $ */ +* ' *
? DJ & # ? ? ? &* *.
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+ ! 1 |
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! ' ( 1 ) |
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& % " &' |
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C19H24FN3O3[SnBr3,46Cl2,54] H2O |
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Mr |
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864,66 |
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M " $ '## , Z |
P21/ , 4 |
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a, b, c, Å; , $ . |
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17,1262(19), 10,3435(11), 17,2582(19); 119,203(1) |
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V, Å3 |
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2668,6(5) |
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dx, $/ &3 |
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2,147 |
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, &&–1 |
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6,429 |
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* , Å |
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MoK , 0,7106 |
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' # & , K |
100(0,1) |
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X & . / . , N1 |
25384 / 7178 |
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(I ), N2 |
4030 |
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X I > 2 |
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% # $ L " |
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' ? |
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Rint |
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0,0989 |
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2 max, $ . |
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59,58 |
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h, k, l |
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–23 h 23, –14 k 14, –23 l 24 |
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R [# N1 &] |
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0,1247 |
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R [# N2 &] |
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0,0513 |
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wR(F2) [# N1 &] |
0,1036 |
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wR(F2) [# N2 &] |
0,0844 |
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S |
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1,009 |
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< " / & |
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w = 1/[ 2(F02 ) + (0,0308P)2 + 0P], $ P = max(F02 + 2Fc2)/3 |
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( / )max |
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< 0,004 |
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max / min, e/Å3 |
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1,251/ –1,143 |
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! ! (SHELX-97) |
< 0,0004 " |
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. 2013. . 54, w 2 |
319 |
M & # # & L?> #$&&* SHELXS [ 7 ] # "&*& & & . < - ' ? D * * / */ & . M '% " ' ' ' % &- & & ?J / # & L?> #$&&* SHELXL97 [ 8 ]. < % # #$?, % # +* HBr Sn(IV) + ' *D SnBr62 , *D A " 24 - "/, # */ &+ A D + ' ' */ */ ( G ) [ 9 ]. # * # & * / & Br +* & ? * , # ' % #-' '%J > ' % ". M &' +* # # A &, % 1 & & Br A &* Cl, +* # A ' ? & $'- !$ . * $' !$ (# + S4 Pioneer &* Bruker) # # ' / L , $ A '& ?J ? # A$ & " # A ? ?> 10 & A ? 4,91 (1- & ) 2,39 & .% (5- & ). P * # A > " ' % & A "
+ & 42,7 45,0 & .% ' & & + ! . " C19H24FN3O3[SnBr3,46Cl2,54] H2O *- % (& .%): Br 31,97, Cl 10,41. M-& &', # D & $ $ '% " # / +* A " ' & $+$ HCl.
% D # ! D Br/Cl # '% & ! '&&* - D Br Cl D # ! . < ' ? R- ", / #- * # * # & * # " & ? * % ". # * # & * / ? */ */ & A ' % " ? # . & +* *" * & &'&*, '>L & & & , & & , "L / "& ' *. <# * / & +* *," / / ' % " " # *D # D # & ! ?> '& ?J " % ' % " &*/ # & . < ' ? ' % ? # R = 5,13 % " 7178 ?- */ A D F2 > 2 (F2). ! ! ' % " " - $ &$ %- ".
Q % # / % / ' ' & ' # #- $&& DIAMOND [ 10 ]. ' ' # Cambridge Crystallographic Data Centre (CCDC) & & 865975. * &$' +* ? # '% * % D www.ccdc.cam.ac.uk/data_request/cif.
/ ' 0 7
< ' */ # ' */ D ! , A L / - * EnrH2 EnrH22 . < &+ A D + ' ' */ */ [ 9 ] A " - & ! " ? # &' &' > — ! ' 2-$& ,& ! / " & Enr . ‚ % " pKa " ! (pKa1 = 5,94 0,09, pKa2 = 8,70 0,44) [ 11 ] + # '% *& " ! # ! [ 12 ], #- &' & A # # A ?, % EnrH32 +' & ? # ! ! HCl *J 4—5 A ? " # / "L & & D.
& " % ? "% D " 1 A EnrH32 , SnBr3,46Cl22,54 ' & ' ' * ( . 1). * " D C—O, C—N, C—F —C - '>L * '$* & # D *& " '$/ D - ! [ 9 ]. M & 1 # A " ' & '>L D " C4—O1 1,324(7) Å # > # *& 1 ! 2-$ - & (1,241 Å) [ 13 ]. " " 1— 2 1— 3 # D +- ? D $'## ! 2-$& # & * (1,241,25 Å). < 1 d( 1— 2) = 1,236(7) d( 1— 3) = 1,317(7) Å, % # & '% ' D D " , & — D " +ƒ" " " # & #&' 3.
* [SnBr3,46Cl2,54]2– " "> " A *& & {d(Sn—Br/Cl) = 2,4901(12)2,5741(10) Å}, 12 % D '$ Br/Cl—Cd—Br/Cl / " " # 85,89(3) 93,46(3) ,
320 |
. . Q < T<, . . KK<, . . Q < T< , Q. . Q UK |
# . 1. & " % ? "% D
C19H24FN3O3[SnBr3,46Cl2,54] H2O.
ˆ / *& "& + % ** "
3 — 173,60(3) 177,66(4) . EnrH32 >% # D $& & % / !# # ?! & ! D ( &. . 1). & N3 # .+ ? &' &' 1 # & O1, *D + ' ' & '- " '> '> " ? & 2 + ? D $'##*. < ' & ' " " - " " ? C14—H14A F + ' '$D J % *D ! . & ' '- & ' " *D & S(6) [ 14, c. 501 ], # % *D " */ D / . - & '/ ' & ' " */ ' ' 1 ? 7 & A& ' " */ */ " D. - &* Br2 Br5 # & > '% " + */ " D. M & * */ " D * + . 2.
* EnrH32 '% '> & " * & [SnBr3,46Cl2,54]2 . / + ' ' '/! * * " , # % & / & A ' '$ - *& & & & & & Br4 & '> '# & ' " *D & R21 (6). < & D " N3—H3 Br6 C19—H19 Br6 &* > & % */ ! (& * R22 (7)). A *D / '$/ EnrH32 ' '> " ? & & + & , + '" ! # . ?& " " " ? % & D " O3—HO3 Ow.
% & A& ' " */ */ " D & A ' EnrH32 # + >$ $+ */ & */ ! # D ( . 2) & ' ! . G$" &' - L + '> " * & & 8,1 Å, */ & L > " * [SnBr3,46Cl2,54]2& ' * *.
' % */ & A& ' " */ # # & L #$&&* PLATON [ 15 ] # % — -& D " & A ' & % & & & */ & ' #
+ ! 2
D—H A (Å, $ .) 1
D—H |
d(D—H) |
d(H A) |
DHA |
d(D A) |
A |
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N3—H3 |
0,93 |
2,46 |
155,3 |
3,324(5) |
Br6 [x, y–1, z] |
O1—HO1 |
0,84 |
1,90 |
145,6 |
2,637(6) |
O2 |
C14—H14A |
0,99 |
2,02 |
130,5 |
2,763 |
F |
O3—HO3 |
0,84 |
1,78 |
166,2 |
2,607(6) |
Ow |
C11—H11 |
1,0 |
2,81 |
135,1 |
3,586(6) |
Br1 |
C18—H18B |
0,99 |
2,85 |
140,7 |
3,674(6) |
Br3 [1–x, y–1/2, 1/2–z] |
C14—H14B |
0,99 |
2,88 |
147,7 |
3,754(6) |
Br4 [x, y–1, z] |
C17—H17A |
0,99 |
2,87 |
148,1 |
3,747(6) |
Br4 [x, y–1, z] |
C19—H19C |
0,98 |
2,75 |
146,1 |
3,603(7) |
Br6 [1–x, y–1/2, 1/2–z] |
. 2013. . 54, w 2 |
321 |
# . 2. ‚ $ $ + * & -
* ! # EnrH32 &* -& ' * + '>L /-" /. " # * * [SnBr3,46Cl2,54]2– / # -*
+ ! 3
* — - EnrH32 1
Cgi—Cgj |
d(Cg—Cg), Å , $ . , $ . , $ . Cgi_p, Å $, Å |
Cg —Cg |
3,900 |
0 |
28,78 |
28,78 |
3,418 |
1,877 |
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1 |
1 |
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Cg —Cg |
3,736 |
3,1 |
23,15 |
21,95 |
3,465 |
1,877 |
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1 |
2 |
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Cg1 — # ? ?! C2C3C4C9C10N1; Cg2 — # ? ?!
C5C6C7C8C9C10. Cg1 Cg2 # '% * # + & [2–x, –y, 1–z].
$—/ [ 14 ], /$ " '$/ D / [ 9 ]. Q & % # & * $ & D " # * + . 3.
M # # '% D ' ' * 1 &$*& ' ' & , A L- & A * # *D ! # ! C17H22FN3O32 CuCl24 H2O [ 16 ]C17H22FN3O32 CuBr24 H2O [ 17 ], ' & ? 'L % & ' &*/ & A- & ' " */ & . Q$ $*D [SnBr3,46Cl2,54]2– '> &' - */ " D, % & &* " $ $*& & . M ? ' &' ? ' ? * & & ' * + ? " & &*/ D & A . A # # A ?, % + & ! " & */ $ $+ */ ! # D # / '% & & -*, " '$/ &$*/ */ D / [ 16, 17 ].
& + &, ' ' 1 + D *D " D — -&- D & A * & & 8,1 Å, */ & L > " * [SnBr3,46Cl2,54]2–& ' * *. < # '% */ L / + '> ", * " */ - D / , '# & ' " * & * R21 (6) R22 (7).
+ *# # D # A $ M ‰ " # A - 'L / '% */ J ‰ ( ˆ-4828.2012.2) ‰ ? D ! D #$&&* '% *'%-#$ $% * ! D 2009—2013 $* ($' * * w 02.740.11.0269 w 02.740.11.0629).
* " +#$ -#/
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322 |
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