Di-μ-diphenylphosphido-bis{chlorido[(mesitylmethyl)diphenylphosphine-κP]palladium(II)}

(1)

Institut de Chimie, Universite´ de Neuchaˆtel, Case Postale 158, CH-2009 Neuchaˆtel, Switzerland Correspondence e-mail: georg.suess-fink@unine.ch

In the title dinuclear palladium complex, [Pd2(C12H10P)2- Cl2(C22H23P)2], the terminal ligands adopt a trans conﬁgura- tion with a Pd Pd distance of 3.6111 (4) A˚ . A crystal- lographic twofold rotation axis runs perpendicular to the Pd2P2ring. The Cl atom lies slightly out of the plane of the Pd and three P atoms in each half of the molecule.

Related literature

For similar dinuclear palladium complexes, see: Brandon &

Dixon (1981); Carty et al. (1982); Gebauer et al. (1992);

Zhuravel et al. (2000). For the synthesis of PPh2CH2(2,4,6- Me3C6H2), see: Chahenet al.(2006).

Experimental Crystal data

[Pd2(C12H10P)2Cl2(C22H23P)2] M_r= 1290.83

Orthorhombic,Pccn a= 12.0793 (7) A˚ b= 22.6156 (14) A˚ c= 22.5499 (14) A˚

V= 6160.2 (6) A˚³ Z= 4

MoKradiation = 0.81 mm ¹ T= 173 (2) K 0.310.240.17 mm

Data collection Stoe IPDS diffractometer Absorption correction: none 46413 measured reﬂections

6011 independent reﬂections 3498 reﬂections withI> 2(I) R_int= 0.089

Reﬁnement

R[F²> 2(F²)] = 0.031 wR(F²) = 0.064 S= 0.78 6011 reﬂections

346 parameters

H-atom parameters constrained max= 0.53 e A˚ ³

min= 0.98 e A˚ ³

Data collection:EXPOSEinIPDS Software(Stoe & Cie, 2000);

cell reﬁnement: CELL in IPDS Software; data reduction: INTE- GRATE in IPDS Software; program(s) used to solve structure:

SHELXS97 (Sheldrick, 1997); program(s) used to reﬁne structure:

SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and Mercury (Version 1.4.1; Bruno et al., 2002);

software used to prepare material for publication:SHELXL97.

This work was supported by the Swiss National Science Foundation (grant No 20-61227-00).

References

Brandon, J. B. & Dixon, K. R. (1981).Can. J. Chem.59, 1188–1200.

Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. & Taylor, R. (2002).Acta Cryst.B58, 389–397.

Carty, A. J., Hartstock, F. & Taylor, N. J. (1982).Inorg. Chem.21, 1349–1354.

Chahen, L., Therrien, B. & Su¨ss-Fink, G. (2006).J. Organomet. Chem.691, 4257–4264.

Farrugia, L. J. (1997).J. Appl. Cryst.30, 565.

Gebauer, T., Frenzen, G. & Dehnicke, K. (1992).Z. Naturforsch. Teil B,47, 1505–1512.

Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Go¨ttingen, Germany.

Stoe & Cie (2000).IPDS Software. Stoe & Cie GmbH, Darmstadt, Germany.

Zhuravel, M. A., Moncarz, J. R., Glueck, D. S., Lam, K.-C. & Rheingold, A. L.

(2000).Organometallics,19, 3447–3454.

Di- -diphenylphosphido-bis chlorido[(mesitylmethyl)diphenyl- phosphine-

P ]palladium(II)

Ludovic Chahen, Bruno Therrien and Georg S ¨uss-Fink

(2)

electronic reprint

(3)

!" #"#$ %&& '"!(($)

*+&,-. &/01 2

!

"

#

$%&

_' _%

#

(

) +,+,,+,+,**+

,+,,- !

_'

.+,/0- +123+, 2111 1 * ,%

^'

"

#(4&5+36+7

+,8,9$%+613,,+7,::;..;1.+,/0- ,+++<) 7*,,,2++2172+33,, +,,

#

$%&

_' _%

#

3,-,**1+,*+**

7,6<,+-,++,21,+1,3+,17<+,,-**=3,*

,+,31+>,+,,+3+1,<+21,,+,+,

*,1,,+7,,-6,<+,,<$ ?<+2+33,#76+

,3277*>,+,,+**%' @363+,312<+,<++*

=3A+72,,,3,+,+< !

#

,+1 !

#

B2,+ ,)!

#

C+,6

*1** < !

"

#

$%&

_' _%

#

(

* , *1** < !

_'

.+, / 0- 17 + * +< 21 +,3+,1 *, 3 +,D,D

#4&5 0

_'

D%E%$$# %$# 8*# '$%#

^'

4&5 0

_'

D8,9$%

&FF)G DH

_%

#

_%%

_$

,<+

_%

#

_%%

_$

D %'H#88=D %H#8 !

"

#

$%&

_' _%

#

(

**6+<+,+1,,2<+I+,1<<+,,, 1,+2,2176,+,<+<+*

#,*7+,,**,+<*3,+37 J#K'E%?,7

_*

# K8<+13+* *

_>

(4)

=3,+++<0,**,++,7, 8L+2,216#,*,62<+,+1

=3.<+,,21

! " 3#!$$"#%

# #_' K%$

K' _-K'&3^9'

A++2 &M+,,

NK'?

#,*12D,2, ,+,+*<++<*

K' ? OKE8P

K%8%$ ? !K⁹

K8$$ ? K' Q

K%%% ?^' ,17

K$ 'R$R

F)0F

<<+,+ %+<*

5,,*+D<<**,2 '$+<*7ST

&+,+D3+, K 0++*D-* O_,-K%P

K' Q OKP

U*,*,* !K9$V$

:2*+++D "K9V

$%$',*++<* K9V

#$

5< F,+1,*,D<<+=++, W,**>,+*,+-D< #1+3*,D<++<+32+3

**

ST K' #,,+,+**+,

(5)

% K%$ %KGT X$

7+KX G'

&K YGT _,-K

%+<* YZ_,-K8'?^9' '$%,+,+* YZK9?^9' +,+1,*,D*++6,+,+

* -++D

&'

45 "#&:+1*,7,*,'Q,F),3,0<<+,F1*F *3&M3+, +,+,,),3,*,U*,*,*9@*YUK@'*+<+,

/"#:*;*-*+,,3277*,* ,+*,*3<6,+,, +-*;*,+,[,6,1*,<*;**,*,3*,+*,3*H++,*

27*;*,+,+*,+1*71,+<21+1*,*1+1:,+-,*+ +,<

*;***<+*,3*;*663*,*

67 "#5<<=,3,*:WW+<*73 <,+% ,3**<<F,+2,*=6

, <,+* ,+2,*=7=*\+<+3,6=+*-+**<=S*3,= **1<+,, 3 <,+*3 ,*+6,<+<*<++< <,+*2,*=,+*,*,1,27 ,*,+3,**2,*=,5E<,+*2,*:WW,,726,+3+

$'()*''$'$+,^-.

/ _*]G_>

''$ %8 $%'8

#: '''' $ '8]

#. % % ' '8]

'$% %%'8 8% '' ' %' %8''% 88 '$

$ '' 8 ' $$%

#$ % 8$' ' 8$]

8 '' %8' '8 $%

% $' %%% ' $$

#% $% % '' 8']

$$' %88 8'% '' '' 8''% '% $88

#: 8'8% %]

#. % 8% ' %]

# %8$ 8%8 %$ %]

$$$ 8 '$ 8$

#: '' 88 '% $]

#. $ 8 $$ $]

# $%8 8$'' '% $]

$$' 8'8 $$8% $'$

#: '8 $ %8]

#. $ 88 %8]

# $ %' %8]

(6)

$ 88' $'$8 8

$' 8$%8 $8 ''8

# $' 88' '$ $]

' 8'' $8%8 8 '

#' $ $8 % $8]

$ 88$$' $%% $% $

#$ 8 $'$ 8$ $]

8 8''' 8%% 8 '%$

#8 %% 8'8 ' $$]

% 8$ 88 %$ '$

#% 88$8 % 88 '%]

$ %$ 8

$' %8% 9% '

# 8%% %% 9 $8]

$%' %% 9 $$'

# 8%' % 9' 8']

'8'' %' 9 8

# '' % 9'% %]

$'' %%8 98' %$'

# % 9%$% $]

'' %8 8$ $8

# $% % '$ 8]

' $ %'$8$ $8 8%

$ $' 8$88 88%8% '$

#$ 8 8%8 ']

8 8'' 8'% $%%

#8 $$ $% ' 8%]

% $' 88 9$8 8$

#% 8'$ 9 %8]

%' %8 98% 8

# $' % 9$ %']

' %88 98%% '

# %$ 9 $8]

$ %8$$ $8% %

' %'%' %8 88 '8

#' 8'$ 8% $']

' $' 8'' $ 8

#' '88 88' $8 %]

' '' %' 88

#' $$ 88 ' %%]

'' 8'$ %$% $$ 8'

#'' %%' '' %]

'$ ''' %'% 88% '8

#'$ % 8 $8]

$%'% $ $ '%

' %$% %' $

8 $%'% %%$ %%$ $

%''% $$ ''$ $

(7)

$'$'$+,^-.

^'' ^' ^'

8 '' '' $ 8'$ 98

'8 ' $88 8

' '$ ' ' % % 9

$ ' $ 8' 9

8 $ 88' '' %

% $8 88' ''' ' 9$

% '% '$ ' 98$

$ $%' $' 98' $% 8

8$ $ 8' 9' 9' $'

$% $8 '% 9' 8% 9

'8 $$ ' $$ '%

'8' '' '' 9%8 9'% ''

' $ 8 $'' 98$% 98$

$ $% $' '%% '

8 '' ' '' '8 $% '

% % ' ' 8$ ''8 '

$ 98 9$8 98

' $ ' 9$% '

%' $ 9' $ 9'

' 8' ' % 9%

$%' $ $' 9$ 9%'

''8 ' '' 9' 9

' 8 ' % $'' 9$' 98%

$ 8 ' '% 9$8 '% 9

8 $% $ 8' 9$% 9

% 8 %' $' 9 9

%'' %' 98

$ $ % $ 9 98

' $ % 9%$ 9%$ 8%

' '% '% '8 '8 9$% 8

' 88 $' 8' 9 $

' %$' %' '' 9% 9'

'' 8 ' 8 9' 8

'$ $ ' ' %% 9% '$

'$$ %8 % $8' 9$$ 8$

' $ $ '$8 %' '$ $

8 $ '$$ 8 9%' $$ $

' $ 8%' 98 '

0$'$+,12.

J 8$8 J '8

J8 %' J# '

J#: J '%8

J#. J# '

(8)

J $8 J '%%

J ' $8 J# '

'J $ '8 J '%

'J 88 J# '

$J 8 '88 J# '

$J#$ ' 'J $ '%$

8J % '8 'J $8

8J 8% 'J' '

%J '%8 $J 8 '8

%J#% ' $J#$ '

J 88 8J % '%%

J#: % 8J#8 '

J#. % %J ''%

J# % %J#% '

J#: % J '88

J#. % J# '

J# % J# '

J#: % J '$ '8

J#. % J ' '$

J# % J' '

J % '8 'J ' ''8

J '8 'J#' '

J8 ' 'J ' '%

J ' '8 'J#' '

J# ' 'J '' ''%

'J $ '8 'J#' '

'J#' ' ''J '$ ''8

$J 8 ''8 ''J#'' '

$J#$ ' '$J#'$ '

8J % '88 J '

8J#8 ' 'J %

%J#% ' 'J '

J ''8 8J '%

J ''$ J' '

J8 '

J J8 '8 J J $$

J J#: J J#

8J J#: J J#

J J#. J J $

8J J#. J J# 8

#:J J#. J J# 8

J J ' ' J J 8$

J J ' J J#

'J J '' J J#

$J 'J '$ J J $

$J 'J $' J J#

J 'J '' J J#

8J $J ' $ $J 'J '

(9)

8J $J#$ % $J 'J' ''

'J $J#$ % J 'J' '

$J 8J % $ 8J $J ' $

$J 8J $ 8J $J#$ 8

%J 8J $ 'J $J#$ 8

8J %J %$ %J 8J $ '$

8J %J#% %J 8J#8

J %J#% $J 8J#8

%J J $' 8J %J $

%J J %' 8J %J#%

J J ' J %J#%

'J J#: 8 %J J $

'J J#. 8 %J J# 8

#:J J#. 8 J J# 8

'J J# 8 J J ' $

#:J J# 8 J J#

#.J J# 8 'J J#

8J J#: 8 '$J J ' '

8J J#. 8 '$J J' '

#:J J#. 8 'J J' '

8J J# 8 'J 'J $$

#:J J# 8 'J 'J#' '

#.J J# 8 J 'J#' '

J J#: 8 'J 'J ' $

J J#. 8 'J 'J#' 8

#:J J#. 8 'J 'J#' 8

J J# 8 'J 'J '' $

#:J J# 8 'J 'J#'

#.J J# 8 ''J 'J#'

%J J %' 'J ''J '$ $$

%J J8 ' 'J ''J#'' '

J J8 '8' '$J ''J#'' '

'J J ' ''J '$J $

'J J# ''J '$J#'$ 8

J J# J '$J#'$ 8

$J 'J 8' 'J'J %

$J 'J#' 'J'J '

J 'J#' J'J 8$

'J $J 8 $ 'J'J 8

'J $J#$ J'J $

8J $J#$ J'J $'

$J 8J % $ J8J 8'%8

$J 8J#8 J8J 8'88

%J 8J#8 J8J '8

8J %J ' J8J $

8J %J#% 8 J8J 88

J %J#% 8 J8J %

J J ' 'JJ' 888'

(10)

J J8 $ 'JJ8 $%'

J J8 $8' 'JJ8 '$

J J ' 'JJ %8'

J J# 8 'JJ '''

J J# 8 8JJ %'

8J J J 8'' 'J 'J ''J '$ % 8J J J ' 9' 'J ''J '$J 9%

J J 'J $ 9$8 'J J '$J '' 9'8 J J 'J $ %' 'J J '$J '' 9$%' J J 'J 8%' $J 'J'J '' J J 'J 9%8 J 'J'J 988 J 'J $J 8 8 $J 'J'J 98' J 'J $J 8 8' J 'J'J

'J $J 8J % $'% $J 'J'J $8 'J $J 8J 98%$ J 'J'J 9'%%' $J 8J %J 9'% '$J J'J ' 9$$' J 8J %J %$ 'J J'J ' '%8' 8J %J J 98 '$J J'J 9' 8J %J J %' 'J J'J %8 'J J J % 888 '$J J'J %' J J J % 9' 'J J'J 98' 'J J J 9$' %J J8J '8

J J J '8 J J8J 98'

%J J J ' 98 %J J8J 9'$'

8J J J ' % J J8J '

J J 'J $ 98 %J J8J 88' J 'J $J 8 88 J J8J 9' 'J $J 8J % 98 J J8J 9'' $J 8J %J 9'8 J J8J ' J J %J 8 8$ J J8J %$8'

8J J %J 8 9 J J8J 9'

J J J 9%8 J J8J $$'

8J J J 9' J J8J 9''

J J J % J J8J $8'

J J J 98% J J8J 8'

J J J 9 J J8J 9'

J J J 8 'J'JJ' 9%8$

J J J 9% J'JJ'

8J J J %' J'JJ' 9%8'8 J 'J $J 8 8 'J'JJ8 8$'

'J 'J $J 8 '' J'JJ8 9

'J $J 8J % 9$% J'JJ8 $' $J 8J %J 8% 'J'JJ 9$

8J %J J 9% J'JJ '8

%J J J ' 9'% J'JJ %

$J 'J J $8 J8JJ' $$

(11)

'J 'J J 9' J8JJ' 9%8 '$J J 'J ' 88 J8JJ' '%

'J J 'J ' 8%' J8JJ 9'$

J 'J 'J ' 9$% J8JJ %$

'J 'J 'J '' % J8JJ 9$%

F1+1*D 9/X'G9X'G

(12)

&'

(13)

&(

Di-μ-diphenylphosphido-bis{chlorido[(mesitylmethyl)diphenylphosphine-κP]palladium(II)}

Di- -diphenylphosphido-bis chlorido[(mesitylmethyl)diphenyl- phosphine-

P ]palladium(II)

Ludovic Chahen, Bruno Therrien and Georg S ¨uss-Fink

electronic reprint

!" #"#$ %&& '"!(($)

*+&,-. &/01 2

!

"

#

$%&

#

(

) *+,+,*,+,+,**+

,+,,- !

.+,/0- +1*23+, 21*11 1 * ,%

"

#(4&5*+36*+*7*

+,8,9$%+*61*3,*,+**7,::;..;**1*.+,/0- ,+*++<) *7*,,,*2*++217*2+33,*, +,,

#

$%&

#

3,-,**1+,*+**

7,6*<,+-,++,21,+1*,3+,17<+,,-**=3,*

,+,*31*+*>,+,,+3+1,<+21,,+,+,*

*,1,,+7,,-6,<+,,<$ ?<+2+33,#76+

,3277*>,+,,+**%' @363+*,*312<+,<++*

=3A+7*2*,*,,3*,+*,+*< !

#

,+1 !

#

B2,+ ,)!

#

C+,6

*1** < !

"

#

$%&

#

(

* , *1** < !

.+, / 0- 17 + * +< 21 +,3+,1 *, 3 +,D,D

#4&5 0

D%E%$$# %$# 8*# '$%#

4&5 0

D8,9$%

&FF)G DH

#

,<+

#

D %'H#88=D %H#8 !

"

#

$%&

#

(

**6+<+,+1*,**,2<+I+,1<<+,,, 1**,+2,21*76,+,<+<+*

#,*7+,,**,+<*3,+37 J#K'E%?,7

# K8<+13+* *

=3,+*++<0*,**,++,7, 8L+2,216#,*,62<+,+1

=3.<+,,21

) +,+,,+,+,**+

.+,/0- +123+, 2111 1 * ,%

#(4&5+36+7

+,8,9$%+613,,+7,::;..;1.+,/0- ,+++<) 7*,,,2++2172+33,, +,,

7,6<,+-,++,21,+1,3+,17<+,,-**=3,*

,+,31+>,+,,+3+1,<+21,,+,+,

,3277*>,+,,+**%' @363+,312<+,<++*

=3A+72,,,3,+,+< !

**6+<+,+1,,2<+I+,1<<+,,, 1,+2,2176,+,<+<+*

=3,+++<0,**,++,7, 8L+2,216#,*,62<+,+1