Chlorido(ethyl­diphenyl­phosphine-κP)(1-pyrrolidinecarbodithio­ato-κ2S,S′)nickel(II)

Kropidłowska, A.; Turowska-Tyrk, I.; Becker, B.

doi:10.1107/S1600536808011860

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 5| May 2008| Page m748

doi:10.1107/S1600536808011860

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Chlorido(ethyldiphenylphosphine-κP)(1-pyrrolidinecarbodithioato-κ²S,S′)nickel(II)

Anna Kropidłowska,^a ^* Ilona Turowska-Tyrk ^b and Barbara Becker ^a

^aDepartment of Inorganic Chemistry, Chemical Faculty, Gdańsk University of Technology, 11/12 G. Narutowicza St., 80-952 PL Gdańsk, Poland, and ^bInstitute of Physical and Theoretical Chemistry, Chemical Faculty, Wrocław University of Technology, 27 Wybrzeże Wyspiańskiego, 50-370 PL Wrocław, Poland
^*Correspondence e-mail: anna@urethan.chem.pg.gda.pl

(Received 23 April 2008; accepted 24 April 2008; online 30 April 2008)

In the crystal structure of the title complex, [Ni(C₅H₈NS₂)Cl(C₁₄H₁₅P)], the Ni atom is coordinated by an S,S′-chelating dithiocarbamate, a chloride and a diphenylethylphosphine ligand in a distorted square-planar arrangement.

Related literature

For related literature, see: Allen (2002 ); Darkwa et al. (1999 ); Kropidłowska, Chojnacki et al. (2007 ); Kropidłowska, Janczak et al. (2007 ); Pastorek et al. (1996 , 1999 ); Reger & Collins (1995 ).

Experimental

Crystal data

[Ni(C₅H₈NS₂)Cl(C₁₄H₁₅P)]
M_r = 454.63
Monoclinic, P 2₁ /c
a = 6.5218 (5) Å
b = 19.1695 (15) Å
c = 16.6178 (14) Å
β = 90.786 (6)°
V = 2077.4 (3) Å³
Z = 4
Mo Kα radiation
μ = 1.34 mm⁻¹
T = 299 (2) K
0.50 × 0.21 × 0.17 mm

Data collection

Kuma KM-4-CCD diffractometer
Absorption correction: refined from ΔF (Walker & Stuart, 1983 ) T_min = 0.553, T_max = 0.804
10912 measured reflections
3637 independent reflections
2989 reflections with I > 2σ(I)
R_int = 0.042

Refinement

R[F² > 2σ(F²)] = 0.040
wR(F²) = 0.113
S = 1.08
3637 reflections
226 parameters
H-atom parameters constrained
Δρ_max = 0.57 e Å⁻³
Δρ_min = −0.35 e Å⁻³

Data collection: CrysAlis CCD (Oxford Diffraction, 2003 $[Oxford Diffraction (2003). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Poland, Wrocław, Poland.]$ ); cell refinement: CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2003 $[Oxford Diffraction (2003). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Poland, Wrocław, Poland.]$ ); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997 ) and Mercury (Macrae et al., 2006 ); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808011860/at2563sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808011860/at2563Isup2.hkl

checkCIF report

Comment top

Metal (Ni, Pd) complexes in which the atom is coordinated by a S,S-chelating dithiocarbamate, one halogenide and one phosphine have been investigated and used to obtain compounds with a sulfur rich kernel arising from the presence of two different S-donor ligands (Darkwa et al., 1999; Pastorek et al., 1999; Reger & Collins, 1995). Several structures of such species are stored in the Cambridge Structural Database (CSD-2007, Allen 2002).

Recently, we reported the synthesis of [Ni{S₂CN(CH₂)₄}(Cl)(PPh₃)] (Kropidłowska, Janczak et al., 2007) solvated by a chloroform molecule, which interacts with the complex by a weak C—H···S hydrogen bond. The structure of homologous hemisolvated [Ni{S₂CN(CH₂)₄}(Br)(PPh₃)] has also been reported (Pastorek et al., 1996). In the present paper we describe the structure of another nickel(II) complex - (1-pyrrolidinylcarbodithioato-S,S') -chlorido-(diphenylethylphosphine)nickel(II), [Ni{S₂CN(CH₂)₄}(Cl)(PPh₂Et)] (I) obtained by essentially quantitative metathesis of trans-dichloro-bis(diphenylethylphosphine)-nickel(II) and bis(1-pyrrolidinylcarbodithioato-S,S')nickel(II). The molecular structure of (I) with the atom numbering scheme is shown in Figure 1.

In this compound the metal(II) ion is four-coordinated within a typical square planar [NiClS₂P] heterogeneous coordination sphere. The dithiocarbamate ligand acts as a bidentate chelate, coordinating to Ni via both S atoms and thus introducing a deformation of the coordination geometry. Atom S1 is located trans to the Cl ligand and atom S2 is trans to the diphenylethylphosphine ligand. Although (I) was obtained in the same manner as previously mentioned [Ni{S₂CN(CH₂)₄}(Cl)(PPh₃)] it did not retain the solvent within its crystal structure, similarily to previously described [Ni{S₂CN(C₄H₈O)}(Cl)(PPh₃)] (Kropidłowska, Chojnacki et al., 2007). The schematic drawing of the crystal packing in (I) is presented in Figure 2.

Related literature top

For related literature, see: Allen (2002); Darkwa et al. (1999); Kropidłowska, Chojnacki et al. (2007); Kropidłowska, Janczak et al. (2007); Pastorek et al. (1996, 1999); Reger & Collins (1995).

Experimental top

Nickel chloride, NiCl₂^.6H₂O (0.594 g, 0.0025 mol, purchased from POCh) was dissolved in 50 ml of methanol/water (10/1, v/v) and this solution was added dropwise to the ammonium salt of pyrrolidinylcarbodithioic acid C₄H₈NCS₂NH₄ (0.82 g, 0.005 mol, Fluka) dissolved in methanol/water. This mixture was stirred vigorously under argon atmosphere for ca 20 minutes, then filtered and the filtrate left for crystallization at 278 K. After a week the green crystalline product, namely Ni(S₂CNC₄H₈)₂ was collected. It was further dissolved (0.199 g, 0.00057 mol) in 10 ml of chloroform and mixed with solution of equimolar amount of NiCl₂(PPh₂Et)₂ (0.315 g). The mixture which turned into deep violet colour, was stirred for 10 minutes and then filtered. To the filtrate 10 ml of Et₂O was added. After two days violet crystals were collected and washed with several portions of ether.

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2003); cell refinement: CrysAlis CCD (Oxford Diffraction, 2003); data reduction: CrysAlis RED (Oxford Diffraction, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997) and Mercury (Macrae et al., 2006); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. Molecular structure and atom-numbering scheme for the title complex (I) with displacement ellipsoids drawn at 50% probability level. H atoms are represented as circles of arbitrary size.
	Fig. 2. Schematic drawing of the crystal packing down the a axis.

Chlorido(ethyldiphenylphosphine-κP)(1-pyrrolidinecarbodithioato- κ²S,S')nickel(II) top

Crystal data top

[Ni(C₅H₈NS₂)Cl(C₁₄H₁₅P)]	F(000) = 944
M_r = 454.63	D_x = 1.454 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 3645 reflections
a = 6.5218 (5) Å	θ = 3.5–23.0°
b = 19.1695 (15) Å	µ = 1.34 mm⁻¹
c = 16.6178 (14) Å	T = 299 K
β = 90.786 (6)°	Block, violet
V = 2077.4 (3) Å³	0.50 × 0.21 × 0.17 mm
Z = 4

Data collection top

Kuma KM-4-CCD diffractometer	3637 independent reflections
Radiation source: fine-focus sealed tube	2989 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.042
ω scans	θ_max = 25.0°, θ_min = 3.1°
Absorption correction: part of the refinement model (ΔF) (Walker & Stuart, 1983)	h = −6→7
T_min = 0.553, T_max = 0.804	k = −22→22
10912 measured reflections	l = −19→18

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.040	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.113	H-atom parameters constrained
S = 1.08	w = 1/[σ²(F_o²) + (0.0634P)² + 0.6647P] where P = (F_o² + 2F_c²)/3
3637 reflections	(Δ/σ)_max = 0.001
226 parameters	Δρ_max = 0.57 e Å⁻³
0 restraints	Δρ_min = −0.35 e Å⁻³

Crystal data top

[Ni(C₅H₈NS₂)Cl(C₁₄H₁₅P)]	V = 2077.4 (3) Å³
M_r = 454.63	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 6.5218 (5) Å	µ = 1.34 mm⁻¹
b = 19.1695 (15) Å	T = 299 K
c = 16.6178 (14) Å	0.50 × 0.21 × 0.17 mm
β = 90.786 (6)°

Data collection top

Kuma KM-4-CCD diffractometer	3637 independent reflections
Absorption correction: part of the refinement model (ΔF) (Walker & Stuart, 1983)	2989 reflections with I > 2σ(I)
T_min = 0.553, T_max = 0.804	R_int = 0.042
10912 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.040	0 restraints
wR(F²) = 0.113	H-atom parameters constrained
S = 1.08	Δρ_max = 0.57 e Å⁻³
3637 reflections	Δρ_min = −0.35 e Å⁻³
226 parameters

Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ni1	0.41398 (6)	0.542285 (19)	0.69879 (2)	0.04145 (15)
Cl1	0.45930 (14)	0.44894 (4)	0.77213 (6)	0.0630 (3)
P1	0.19702 (11)	0.59106 (4)	0.78208 (5)	0.0397 (2)
S1	0.38209 (13)	0.62417 (5)	0.60835 (5)	0.0544 (2)
S2	0.64891 (13)	0.50962 (4)	0.60948 (5)	0.0508 (2)
N1	0.6761 (4)	0.61076 (14)	0.49827 (16)	0.0524 (7)
C1	0.0929 (4)	0.67350 (15)	0.74538 (17)	0.0421 (7)
C2	0.2112 (5)	0.73347 (17)	0.7499 (2)	0.0534 (8)
H2	0.3426	0.7314	0.7722	0.064*
C3	0.1353 (7)	0.79645 (19)	0.7214 (2)	0.0658 (10)
H3	0.2148	0.8366	0.7255	0.079*
C4	−0.0576 (7)	0.7995 (2)	0.6872 (3)	0.0732 (11)
H4	−0.1092	0.8418	0.6686	0.088*
C5	−0.1733 (7)	0.7405 (2)	0.6805 (3)	0.0743 (11)
H5	−0.3029	0.7426	0.6566	0.089*
C6	−0.0994 (5)	0.67784 (19)	0.7092 (2)	0.0571 (9)
H6	−0.1796	0.6379	0.7041	0.069*
C7	0.2986 (5)	0.61533 (16)	0.88112 (18)	0.0447 (7)
C8	0.1922 (6)	0.6611 (2)	0.9294 (2)	0.0651 (10)
H8	0.0725	0.6817	0.9097	0.078*
C9	0.2601 (8)	0.6766 (2)	1.0060 (2)	0.0790 (12)
H9	0.1865	0.7076	1.0376	0.095*
C10	0.4359 (8)	0.6466 (2)	1.0358 (2)	0.0769 (12)
H10	0.4819	0.6569	1.0876	0.092*
C11	0.5419 (7)	0.6020 (3)	0.9890 (3)	0.0833 (13)
H11	0.6618	0.5818	1.0090	0.100*
C12	0.4748 (5)	0.5858 (2)	0.9115 (2)	0.0637 (10)
H12	0.5495	0.5549	0.8802	0.076*
C13	−0.0307 (5)	0.53894 (19)	0.8047 (2)	0.0614 (9)
H13A	−0.1441	0.5706	0.8141	0.074*
H13B	−0.0657	0.5114	0.7575	0.074*
C14	−0.0117 (6)	0.4907 (2)	0.8755 (3)	0.0737 (11)
H14A	−0.1381	0.4659	0.8821	0.111*
H14B	0.0179	0.5174	0.9232	0.111*
H14C	0.0973	0.4581	0.8666	0.111*
C15	0.5834 (5)	0.58493 (17)	0.55992 (19)	0.0468 (7)
C16	0.6134 (7)	0.6751 (2)	0.4568 (2)	0.0740 (11)
H16A	0.4787	0.6699	0.4321	0.089*
H16B	0.6106	0.7141	0.4940	0.089*
C17	0.7689 (10)	0.6853 (3)	0.3962 (4)	0.125 (2)
H17A	0.7055	0.6832	0.3431	0.151*
H17B	0.8298	0.7312	0.4028	0.151*
C18	0.9245 (7)	0.6337 (3)	0.4024 (3)	0.1021 (17)
H18A	1.0527	0.6550	0.4198	0.123*
H18B	0.9453	0.6122	0.3503	0.123*
C19	0.8606 (5)	0.5801 (2)	0.4617 (2)	0.0609 (9)
H19A	0.8285	0.5362	0.4353	0.073*
H19B	0.9673	0.5722	0.5020	0.073*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.0434 (2)	0.0415 (2)	0.0394 (2)	0.00158 (16)	−0.00237 (16)	−0.00039 (16)
Cl1	0.0697 (6)	0.0521 (5)	0.0672 (6)	0.0089 (4)	0.0010 (4)	0.0144 (4)
P1	0.0380 (4)	0.0437 (4)	0.0373 (4)	−0.0021 (3)	−0.0015 (3)	0.0024 (3)
S1	0.0597 (5)	0.0577 (5)	0.0459 (5)	0.0158 (4)	0.0092 (4)	0.0086 (4)
S2	0.0543 (5)	0.0506 (5)	0.0475 (5)	0.0093 (4)	0.0022 (4)	−0.0024 (4)
N1	0.0547 (16)	0.0542 (16)	0.0486 (15)	0.0051 (13)	0.0081 (13)	0.0023 (13)
C1	0.0450 (16)	0.0463 (17)	0.0351 (15)	0.0027 (13)	0.0054 (12)	0.0009 (13)
C2	0.0593 (19)	0.0530 (19)	0.0481 (18)	−0.0062 (16)	0.0068 (15)	0.0000 (15)
C3	0.085 (3)	0.050 (2)	0.063 (2)	−0.0068 (19)	0.019 (2)	0.0035 (17)
C4	0.091 (3)	0.054 (2)	0.074 (3)	0.022 (2)	0.010 (2)	0.0109 (19)
C5	0.073 (2)	0.067 (3)	0.082 (3)	0.018 (2)	−0.008 (2)	0.013 (2)
C6	0.056 (2)	0.057 (2)	0.058 (2)	0.0034 (16)	−0.0081 (16)	0.0028 (16)
C7	0.0473 (17)	0.0488 (17)	0.0381 (16)	−0.0055 (13)	−0.0004 (13)	0.0008 (13)
C8	0.077 (2)	0.070 (2)	0.048 (2)	0.0109 (19)	−0.0018 (17)	−0.0049 (18)
C9	0.116 (4)	0.074 (3)	0.047 (2)	0.000 (3)	0.008 (2)	−0.008 (2)
C10	0.105 (3)	0.078 (3)	0.048 (2)	−0.025 (3)	−0.014 (2)	0.001 (2)
C11	0.074 (3)	0.111 (4)	0.064 (3)	0.001 (2)	−0.029 (2)	−0.002 (3)
C12	0.0516 (19)	0.086 (3)	0.054 (2)	0.0034 (18)	−0.0077 (16)	−0.0089 (19)
C13	0.0479 (19)	0.070 (2)	0.066 (2)	−0.0158 (16)	−0.0042 (16)	0.0143 (18)
C14	0.061 (2)	0.066 (2)	0.094 (3)	−0.0119 (18)	0.002 (2)	0.027 (2)
C15	0.0475 (17)	0.0486 (18)	0.0443 (17)	0.0054 (14)	−0.0042 (13)	−0.0050 (14)
C16	0.090 (3)	0.069 (2)	0.064 (2)	0.011 (2)	0.020 (2)	0.015 (2)
C17	0.145 (5)	0.091 (4)	0.142 (5)	0.014 (4)	0.076 (4)	0.045 (4)
C18	0.081 (3)	0.127 (4)	0.100 (4)	0.016 (3)	0.043 (3)	0.042 (3)
C19	0.0510 (19)	0.070 (2)	0.062 (2)	−0.0008 (17)	0.0124 (16)	−0.0050 (18)

Geometric parameters (Å, º) top

Ni1—S1	2.1812 (9)	C8—H8	0.9300
Ni1—Cl1	2.1828 (9)	C9—C10	1.369 (6)
Ni1—P1	2.2014 (8)	C9—H9	0.9300
Ni1—S2	2.2371 (9)	C10—C11	1.353 (6)
P1—C1	1.822 (3)	C10—H10	0.9300
P1—C7	1.826 (3)	C11—C12	1.389 (5)
P1—C13	1.833 (3)	C11—H11	0.9300
S1—C15	1.722 (3)	C12—H12	0.9300
S2—C15	1.713 (3)	C13—C14	1.501 (5)
N1—C15	1.295 (4)	C13—H13A	0.9700
N1—C16	1.468 (5)	C13—H13B	0.9700
N1—C19	1.477 (4)	C14—H14A	0.9600
C1—C2	1.386 (4)	C14—H14B	0.9600
C1—C6	1.386 (4)	C14—H14C	0.9600
C2—C3	1.385 (5)	C16—C17	1.453 (6)
C2—H2	0.9300	C16—H16A	0.9700
C3—C4	1.375 (6)	C16—H16B	0.9700
C3—H3	0.9300	C17—C18	1.420 (7)
C4—C5	1.362 (6)	C17—H17A	0.9700
C4—H4	0.9300	C17—H17B	0.9700
C5—C6	1.377 (5)	C18—C19	1.488 (5)
C5—H5	0.9300	C18—H18A	0.9700
C6—H6	0.9300	C18—H18B	0.9700
C7—C12	1.371 (5)	C19—H19A	0.9700
C7—C8	1.382 (5)	C19—H19B	0.9700
C8—C9	1.375 (5)

S1—Ni1—Cl1	170.25 (4)	C9—C10—H10	120.3
S1—Ni1—P1	94.10 (3)	C10—C11—C12	121.1 (4)
Cl1—Ni1—P1	94.62 (3)	C10—C11—H11	119.5
S1—Ni1—S2	78.70 (3)	C12—C11—H11	119.5
Cl1—Ni1—S2	92.99 (4)	C7—C12—C11	120.1 (4)
P1—Ni1—S2	171.11 (4)	C7—C12—H12	120.0
C1—P1—C7	102.11 (14)	C11—C12—H12	120.0
C1—P1—C13	104.01 (16)	C14—C13—P1	116.0 (3)
C7—P1—C13	103.83 (16)	C14—C13—H13A	108.3
C1—P1—Ni1	113.44 (9)	P1—C13—H13A	108.3
C7—P1—Ni1	116.52 (10)	C14—C13—H13B	108.3
C13—P1—Ni1	115.28 (14)	P1—C13—H13B	108.3
C15—S1—Ni1	86.65 (11)	H13A—C13—H13B	107.4
C15—S2—Ni1	85.09 (11)	C13—C14—H14A	109.5
C15—N1—C16	124.2 (3)	C13—C14—H14B	109.5
C15—N1—C19	124.4 (3)	H14A—C14—H14B	109.5
C16—N1—C19	111.4 (3)	C13—C14—H14C	109.5
C2—C1—C6	118.3 (3)	H14A—C14—H14C	109.5
C2—C1—P1	119.8 (2)	H14B—C14—H14C	109.5
C6—C1—P1	121.9 (2)	N1—C15—S2	125.9 (2)
C3—C2—C1	120.6 (3)	N1—C15—S1	124.7 (2)
C3—C2—H2	119.7	S2—C15—S1	109.28 (18)
C1—C2—H2	119.7	C17—C16—N1	104.2 (3)
C4—C3—C2	119.9 (4)	C17—C16—H16A	110.9
C4—C3—H3	120.1	N1—C16—H16A	110.9
C2—C3—H3	120.1	C17—C16—H16B	110.9
C5—C4—C3	120.1 (4)	N1—C16—H16B	110.9
C5—C4—H4	119.9	H16A—C16—H16B	108.9
C3—C4—H4	119.9	C18—C17—C16	111.2 (4)
C4—C5—C6	120.3 (4)	C18—C17—H17A	109.4
C4—C5—H5	119.8	C16—C17—H17A	109.4
C6—C5—H5	119.8	C18—C17—H17B	109.4
C5—C6—C1	120.8 (4)	C16—C17—H17B	109.4
C5—C6—H6	119.6	H17A—C17—H17B	108.0
C1—C6—H6	119.6	C17—C18—C19	108.8 (4)
C12—C7—C8	118.2 (3)	C17—C18—H18A	109.9
C12—C7—P1	121.3 (3)	C19—C18—H18A	109.9
C8—C7—P1	120.4 (3)	C17—C18—H18B	109.9
C9—C8—C7	121.1 (4)	C19—C18—H18B	109.9
C9—C8—H8	119.4	H18A—C18—H18B	108.3
C7—C8—H8	119.4	N1—C19—C18	103.6 (3)
C10—C9—C8	120.1 (4)	N1—C19—H19A	111.0
C10—C9—H9	120.0	C18—C19—H19A	111.0
C8—C9—H9	120.0	N1—C19—H19B	111.0
C11—C10—C9	119.4 (4)	C18—C19—H19B	111.0
C11—C10—H10	120.3	H19A—C19—H19B	109.0

Experimental details

Crystal data
Chemical formula	[Ni(C₅H₈NS₂)Cl(C₁₄H₁₅P)]
M_r	454.63
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	299
a, b, c (Å)	6.5218 (5), 19.1695 (15), 16.6178 (14)
β (°)	90.786 (6)
V (Å³)	2077.4 (3)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.34
Crystal size (mm)	0.50 × 0.21 × 0.17

Data collection
Diffractometer	Kuma KM-4-CCD diffractometer
Absorption correction	Part of the refinement model (ΔF) (Walker & Stuart, 1983)
T_min, T_max	0.553, 0.804
No. of measured, independent and observed [I > 2σ(I)] reflections	10912, 3637, 2989
R_int	0.042
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.040, 0.113, 1.08
No. of reflections	3637
No. of parameters	226
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.57, −0.35

Computer programs: CrysAlis CCD (Oxford Diffraction, 2003), CrysAlis RED (Oxford Diffraction, 2003), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997) and Mercury (Macrae et al., 2006).

Acknowledgements

The authors acknowledge Professor J. Pikies for his donation of the sample of NiCl₂(PPh₂Et)₂ and J. Gołaszewska for her help during the crystallization. This work was supported by the Ministry of Science and Higher Education (Poland), grant No. 1 T09A 117 30. A. Kropidłowska thanks the Foundation for Polish Science for a fellowship.

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