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Acta Cryst. (2008). E64, m335    [ doi:10.1107/S1600536808000317 ]

Dichloridotris(trimethylphosphine)nickel(II)

R. Cao, Q. Wang and H. Sun

Abstract top

The title compound, [NiCl2(C3H9P)3], was obtained as a product of the reaction of [NiCl2(PMe3)2] with an equivalent trimethylphosphine in diethyl ether. It easily loses trimethylphosphine at room temperature to give NiCl2(PMe3)2. There are two independent molecules in the asymmetric unit, and their bond lengths and angles are similar. The Ni environment is trigonal bipyramidal. One Ni, one P and two Cl atoms lie in the equatorial plane, with the remaining two P atoms occupying axial positions. The equatorial Ni-P bond length is shorter than the axial bond lengths.

Comment top

The title molecular (Fig.1) contains two molecules in an asymmetric unit. Bond lengths and angles in the two molecules are approximately the same. The nickel atom lies in the center of a trigonal bipyramid in which two chlorine atoms and one P atom form an equatorial plane, two other phosphorus are arranged in axial positions. The equatorial Ni—P bond lengh is shorter than the axial ones. The nickel atoms do not lie on a straight line joining the apical phosphorus atoms. This is due to the apical groups experiencing greater repulsion from the equatorial PMe3 groups. Similar crystal structures have been reported in the literature e.g. tris(trimethylphosphine)diiodocobalt(II) (Jiao et al.(2007)). The lengths of Co—I (2.6) is longer than the range of Ni—Cl bond lengths, angle in the axial position of this compound (169.8 °) is a little bigger than that in the title compound (167.3–168.0 °).

Related literature top

The crystal structure of the related cobalt compound has been reported by Jiao et al. (2007). For related literature, see: Doriand & Gray (1966).

Experimental top

Standard vacuum techniques were used in manipulations of volatile and air sensitive material. Literature procedure was followed in the preparation of dichlorodi(trimethylphosphine)nickel (Doriand et al.(1966)). Other chemicals were used by purchased. To the solution of NiCl2(PMe3)2(1.0 g, 3.55 mmol) in 50 ml of diethyl ether was added trimethylphosphine (0.27 g, 3.55 mmol) at 193 K. This mixture was allowed to warm to 293 K and stirred for 6 h to form a dark blue solution, which was filtered. Crystallization from ether at 277 K afforded dark blue crystals suitable for X-ray diffraction analysis. (yield: 1.14 g, 89.8%, m. p: 397.15 K).

Refinement top

All H atoms were positioned geometrically. All the H atoms are refined using a riding model with C—H = 0.96 Å and with Uiso(H) = 1.5 times Ueq(C).

Computing details top

Data collection: XSCANS (Bruker, 2001); cell refinement: XSCANS (Bruker, 2001); data reduction: SHELXTL (Sheldrick, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2001); software used to prepare material for publication: SHELXTL (Sheldrick, 2001).

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), with atom labels and 30% probability displacement ellipsoids for non-H atoms. (Only one of the two molecules is shown.)
Dichloridotris(trimethylphosphine)nickel(II) top
Crystal data top
[NiCl2(C3H9P)3]F000 = 1504
Mr = 357.83Dx = 1.370 Mg m−3
Orthorhombic, P212121Mo Kα radiation
λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 6412 reflections
a = 10.481 (2) Åθ = 1.6–24.2º
b = 11.741 (2) ŵ = 1.68 mm−1
c = 28.203 (6) ÅT = 293 (2) K
V = 3470.6 (12) Å3Block, blue
Z = 80.30 × 0.25 × 0.22 mm
Data collection top
Bruker P4
diffractometer		Rint = 0.073
Radiation source: fine-focus sealed tubeθmax = 27.1º
Monochromator: graphiteθmin = 1.4º
T = 293(2) Kh = −13→13
ω scansk = −15→14
Absorption correction: multi-scan
(SADABS; Sheldrick, 2004)		l = −35→36
Tmin = 0.633, Tmax = 0.7094 standard reflections
26702 measured reflections every 50 reflections
7557 independent reflections intensity decay: 0.02%
7309 reflections with I > 2σ(I)
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.030  w = 1/[σ2(Fo2) + (0.0528P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.081(Δ/σ)max = 0.002
S = 1.06Δρmax = 0.63 e Å−3
7557 reflectionsΔρmin = −0.84 e Å−3
289 parametersExtinction correction: none
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack (1983)
Secondary atom site location: difference Fourier mapFlack parameter: 0.006 (8)
Crystal data top
[NiCl2(C3H9P)3]V = 3470.6 (12) Å3
Mr = 357.83Z = 8
Orthorhombic, P212121Mo Kα
a = 10.481 (2) ŵ = 1.68 mm−1
b = 11.741 (2) ÅT = 293 (2) K
c = 28.203 (6) Å0.30 × 0.25 × 0.22 mm
Data collection top
Bruker P4
diffractometer		7309 reflections with I > 2σ(I)
Absorption correction: multi-scan
(SADABS; Sheldrick, 2004)		Rint = 0.073
Tmin = 0.633, Tmax = 0.7094 standard reflections
26702 measured reflections every 50 reflections
7557 independent reflections intensity decay: 0.02%
Refinement top
R[F2 > 2σ(F2)] = 0.030H-atom parameters constrained
wR(F2) = 0.081Δρmax = 0.63 e Å−3
S = 1.06Δρmin = −0.84 e Å−3
7557 reflectionsAbsolute structure: Flack (1983)
289 parametersFlack parameter: 0.006 (8)
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
xyzUiso*/Ueq
Ni10.72334 (3)0.45758 (2)0.757236 (10)0.02415 (8)
Ni20.89293 (3)−0.01317 (2)0.980401 (10)0.02370 (7)
P30.78376 (6)0.52513 (5)0.68901 (2)0.02503 (12)
Cl10.59423 (6)0.50132 (6)0.82016 (2)0.03563 (14)
P60.82135 (6)0.04616 (5)1.04857 (2)0.02697 (13)
Cl40.83645 (6)−0.15585 (5)0.92899 (2)0.03198 (13)
P50.77420 (6)0.10238 (5)0.93714 (2)0.02798 (13)
Cl31.07328 (6)0.10289 (5)0.95390 (2)0.03036 (12)
P20.88341 (7)0.53231 (6)0.79757 (2)0.03072 (13)
P41.03877 (6)−0.12977 (5)1.00949 (2)0.02620 (13)
Cl20.82969 (7)0.27500 (5)0.76850 (2)0.03829 (15)
P10.56145 (7)0.35783 (5)0.72950 (2)0.03075 (14)
C10.8573 (3)0.6661 (2)0.68588 (9)0.0321 (5)
H1A0.93250.66740.70530.048*
H1B0.79800.72230.69710.048*
H1C0.87990.68270.65360.048*
C20.6552 (3)0.0922 (3)1.05323 (11)0.0411 (6)
H2A0.60000.03181.04300.062*
H2B0.64200.15791.03360.062*
H2C0.63630.11111.08560.062*
C30.9884 (3)−0.2639 (2)1.03651 (11)0.0374 (6)
H3A1.0623−0.30701.04560.056*
H3B0.9390−0.30681.01410.056*
H3C0.9375−0.24821.06400.056*
C40.6659 (3)0.5473 (2)0.64191 (9)0.0343 (5)
H4A0.70850.57180.61350.051*
H4B0.60590.60450.65160.051*
H4C0.62160.47720.63580.051*
C51.1530 (3)−0.0718 (2)1.05139 (9)0.0343 (5)
H5A1.2195−0.12641.05680.051*
H5B1.1106−0.05521.08080.051*
H5C1.1891−0.00311.03870.051*
C60.7796 (3)0.2542 (2)0.95028 (10)0.0379 (6)
H6A0.86690.27870.95200.057*
H6B0.73830.26830.98010.057*
H6C0.73660.29560.92570.057*
C71.0461 (3)0.5101 (3)0.77589 (11)0.0422 (6)
H7A1.10570.54180.79810.063*
H7B1.05600.54700.74570.063*
H7C1.06180.43000.77240.063*
C80.8737 (4)0.6837 (2)0.81107 (11)0.0452 (7)
H8A0.78820.70240.82060.068*
H8B0.89600.72700.78340.068*
H8C0.93160.70160.83640.068*
C90.6053 (3)0.0687 (2)0.93156 (12)0.0410 (6)
H9A0.56640.12000.90930.061*
H9B0.56470.07660.96190.061*
H9C0.5958−0.00810.92050.061*
C100.8988 (3)0.4322 (2)0.66093 (9)0.0348 (6)
H10A0.86320.35730.65790.052*
H10B0.97470.42880.67990.052*
H10C0.91960.46140.63010.052*
C111.1422 (3)−0.1830 (2)0.96282 (10)0.0374 (6)
H11A1.1893−0.12090.94930.056*
H11B1.0914−0.21850.93870.056*
H11C1.2005−0.23780.97580.056*
C120.8933 (3)0.4679 (3)0.85625 (10)0.0460 (7)
H12A0.90480.38710.85310.069*
H12B0.81590.48290.87340.069*
H12C0.96430.49980.87320.069*
C130.8233 (3)−0.0500 (2)1.09934 (9)0.0375 (6)
H13A0.7871−0.01231.12640.056*
H13B0.9097−0.07151.10630.056*
H13C0.7743−0.11681.09210.056*
C140.8227 (3)0.1000 (3)0.87549 (10)0.0397 (6)
H14A0.81260.02430.86310.060*
H14B0.91050.12240.87310.060*
H14C0.77060.15180.85770.060*
C150.5937 (4)0.2620 (3)0.67975 (11)0.0461 (7)
H15A0.66380.21300.68760.069*
H15B0.61480.30600.65220.069*
H15C0.51930.21680.67340.069*
C160.4163 (3)0.4338 (3)0.71333 (12)0.0464 (7)
H16A0.35170.38010.70430.070*
H16B0.43370.48390.68720.070*
H16C0.38690.47750.74000.070*
C170.9083 (3)0.1690 (3)1.07128 (12)0.0450 (7)
H17A0.87400.19051.10150.067*
H17B0.89980.23141.04950.067*
H17C0.99680.14981.07470.067*
C180.5033 (3)0.2572 (3)0.77371 (11)0.0445 (7)
H18A0.46020.29790.79850.067*
H18B0.57400.21590.78690.067*
H18C0.44510.20480.75900.067*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.02733 (15)0.02569 (14)0.01943 (13)−0.00089 (11)0.00117 (11)0.00090 (10)
Ni20.02460 (15)0.02604 (14)0.02045 (13)0.00344 (11)−0.00030 (10)0.00021 (10)
P30.0271 (3)0.0272 (3)0.0208 (2)0.0007 (2)0.0019 (2)0.0027 (2)
Cl10.0369 (3)0.0433 (3)0.0267 (3)0.0036 (3)0.0070 (2)−0.0058 (2)
P60.0296 (3)0.0274 (3)0.0238 (3)0.0001 (2)0.0045 (2)−0.0017 (2)
Cl40.0346 (3)0.0306 (3)0.0308 (3)−0.0030 (2)−0.0036 (2)−0.0047 (2)
P50.0269 (3)0.0291 (3)0.0279 (3)0.0028 (3)−0.0007 (2)0.0050 (2)
Cl30.0298 (3)0.0325 (3)0.0288 (3)−0.0044 (2)0.0025 (2)−0.0002 (2)
P20.0312 (3)0.0346 (3)0.0263 (3)−0.0017 (3)−0.0050 (2)0.0017 (2)
P40.0255 (3)0.0279 (3)0.0252 (3)0.0038 (2)−0.0017 (2)−0.0002 (2)
Cl20.0429 (4)0.0313 (3)0.0407 (3)0.0099 (3)0.0048 (3)0.0083 (2)
P10.0335 (4)0.0305 (3)0.0283 (3)−0.0073 (3)0.0022 (3)−0.0017 (2)
C10.0317 (14)0.0327 (12)0.0318 (12)0.0001 (10)0.0021 (10)0.0063 (10)
C20.0389 (15)0.0440 (15)0.0403 (14)0.0060 (13)0.0135 (12)0.0076 (12)
C30.0345 (14)0.0347 (13)0.0429 (15)0.0016 (11)−0.0011 (11)0.0072 (11)
C40.0361 (14)0.0391 (13)0.0277 (11)−0.0002 (11)−0.0042 (10)0.0042 (10)
C50.0309 (13)0.0391 (13)0.0330 (12)0.0022 (11)−0.0040 (10)−0.0035 (10)
C60.0403 (15)0.0314 (12)0.0420 (14)0.0032 (11)0.0055 (12)0.0074 (10)
C70.0335 (14)0.0498 (16)0.0433 (15)−0.0002 (13)−0.0032 (12)0.0053 (13)
C80.0547 (19)0.0398 (14)0.0411 (15)−0.0059 (13)−0.0055 (14)−0.0109 (12)
C90.0338 (15)0.0399 (14)0.0493 (16)0.0014 (12)−0.0068 (12)0.0076 (12)
C100.0403 (15)0.0352 (13)0.0290 (12)0.0045 (11)0.0073 (11)0.0004 (9)
C110.0325 (14)0.0413 (14)0.0383 (13)0.0090 (11)−0.0002 (11)−0.0041 (11)
C120.0442 (17)0.0624 (18)0.0315 (13)0.0027 (15)−0.0078 (12)0.0088 (13)
C130.0430 (16)0.0403 (13)0.0292 (12)0.0020 (12)0.0013 (11)0.0028 (10)
C140.0417 (16)0.0492 (15)0.0282 (12)0.0030 (13)−0.0016 (11)0.0059 (11)
C150.061 (2)0.0377 (14)0.0394 (15)−0.0137 (14)0.0029 (14)−0.0092 (12)
C160.0386 (17)0.0482 (16)0.0525 (18)−0.0079 (13)−0.0049 (13)0.0011 (13)
C170.0518 (18)0.0394 (14)0.0438 (15)−0.0082 (13)0.0086 (14)−0.0130 (12)
C180.0526 (19)0.0380 (14)0.0429 (16)−0.0113 (13)0.0106 (14)0.0021 (12)
Geometric parameters (Å, °) top
Ni1—P32.1754 (7)C5—H5B0.9600
Ni1—P12.2051 (8)C5—H5C0.9600
Ni1—P22.2088 (8)C6—H6A0.9600
Ni1—Cl12.2901 (7)C6—H6B0.9600
Ni1—Cl22.4369 (8)C6—H6C0.9600
Ni2—P62.1781 (7)C7—H7A0.9600
Ni2—P52.2086 (7)C7—H7B0.9600
Ni2—P42.2099 (7)C7—H7C0.9600
Ni2—Cl42.2932 (7)C8—H8A0.9600
Ni2—Cl32.4472 (7)C8—H8B0.9600
P3—C101.808 (3)C8—H8C0.9600
P3—C11.828 (3)C9—H9A0.9600
P3—C41.832 (3)C9—H9B0.9600
P6—C171.822 (3)C9—H9C0.9600
P6—C131.823 (3)C10—H10A0.9600
P6—C21.828 (3)C10—H10B0.9600
P5—C141.812 (3)C10—H10C0.9600
P5—C91.820 (3)C11—H11A0.9600
P5—C61.822 (3)C11—H11B0.9600
P2—C81.821 (3)C11—H11C0.9600
P2—C121.822 (3)C12—H12A0.9600
P2—C71.830 (3)C12—H12B0.9600
P4—C51.814 (3)C12—H12C0.9600
P4—C111.816 (3)C13—H13A0.9600
P4—C31.827 (3)C13—H13B0.9600
P1—C161.822 (4)C13—H13C0.9600
P1—C181.823 (3)C14—H14A0.9600
P1—C151.830 (3)C14—H14B0.9600
C1—H1A0.9600C14—H14C0.9600
C1—H1B0.9600C15—H15A0.9600
C1—H1C0.9600C15—H15B0.9600
C2—H2A0.9600C15—H15C0.9600
C2—H2B0.9600C16—H16A0.9600
C2—H2C0.9600C16—H16B0.9600
C3—H3A0.9600C16—H16C0.9600
C3—H3B0.9600C17—H17A0.9600
C3—H3C0.9600C17—H17B0.9600
C4—H4A0.9600C17—H17C0.9600
C4—H4B0.9600C18—H18A0.9600
C4—H4C0.9600C18—H18B0.9600
C5—H5A0.9600C18—H18C0.9600
P3—Ni1—P195.96 (3)H5A—C5—H5B109.5
P3—Ni1—P295.14 (3)P4—C5—H5C109.5
P1—Ni1—P2168.00 (3)H5A—C5—H5C109.5
P3—Ni1—Cl1140.87 (3)H5B—C5—H5C109.5
P1—Ni1—Cl186.52 (3)P5—C6—H6A109.5
P2—Ni1—Cl187.75 (3)P5—C6—H6B109.5
P3—Ni1—Cl2107.63 (3)H6A—C6—H6B109.5
P1—Ni1—Cl286.05 (3)P5—C6—H6C109.5
P2—Ni1—Cl286.26 (3)H6A—C6—H6C109.5
Cl1—Ni1—Cl2111.50 (3)H6B—C6—H6C109.5
P6—Ni2—P595.57 (3)P2—C7—H7A109.5
P6—Ni2—P496.24 (3)P2—C7—H7B109.5
P5—Ni2—P4167.25 (3)H7A—C7—H7B109.5
P6—Ni2—Cl4134.65 (3)P2—C7—H7C109.5
P5—Ni2—Cl487.36 (3)H7A—C7—H7C109.5
P4—Ni2—Cl487.75 (3)H7B—C7—H7C109.5
P6—Ni2—Cl3110.95 (3)P2—C8—H8A109.5
P5—Ni2—Cl385.67 (3)P2—C8—H8B109.5
P4—Ni2—Cl385.64 (3)H8A—C8—H8B109.5
Cl4—Ni2—Cl3114.40 (3)P2—C8—H8C109.5
C10—P3—C1104.12 (13)H8A—C8—H8C109.5
C10—P3—C4102.56 (13)H8B—C8—H8C109.5
C1—P3—C496.91 (13)P5—C9—H9A109.5
C10—P3—Ni1111.20 (9)P5—C9—H9B109.5
C1—P3—Ni1119.71 (9)H9A—C9—H9B109.5
C4—P3—Ni1119.79 (10)P5—C9—H9C109.5
C17—P6—C13102.02 (15)H9A—C9—H9C109.5
C17—P6—C2102.53 (15)H9B—C9—H9C109.5
C13—P6—C297.91 (14)P3—C10—H10A109.5
C17—P6—Ni2113.03 (11)P3—C10—H10B109.5
C13—P6—Ni2119.42 (10)H10A—C10—H10B109.5
C2—P6—Ni2119.09 (11)P3—C10—H10C109.5
C14—P5—C9100.74 (15)H10A—C10—H10C109.5
C14—P5—C6101.65 (14)H10B—C10—H10C109.5
C9—P5—C6105.08 (14)P4—C11—H11A109.5
C14—P5—Ni2111.26 (10)P4—C11—H11B109.5
C9—P5—Ni2117.54 (10)H11A—C11—H11B109.5
C6—P5—Ni2118.11 (10)P4—C11—H11C109.5
C8—P2—C12102.61 (16)H11A—C11—H11C109.5
C8—P2—C7105.13 (16)H11B—C11—H11C109.5
C12—P2—C7101.05 (15)P2—C12—H12A109.5
C8—P2—Ni1116.93 (12)P2—C12—H12B109.5
C12—P2—Ni1110.24 (12)H12A—C12—H12B109.5
C7—P2—Ni1118.62 (10)P2—C12—H12C109.5
C5—P4—C11101.98 (14)H12A—C12—H12C109.5
C5—P4—C3104.01 (14)H12B—C12—H12C109.5
C11—P4—C3100.25 (14)P6—C13—H13A109.5
C5—P4—Ni2117.76 (9)P6—C13—H13B109.5
C11—P4—Ni2110.91 (10)H13A—C13—H13B109.5
C3—P4—Ni2119.26 (10)P6—C13—H13C109.5
C16—P1—C18102.08 (17)H13A—C13—H13C109.5
C16—P1—C15105.26 (17)H13B—C13—H13C109.5
C18—P1—C15100.82 (14)P5—C14—H14A109.5
C16—P1—Ni1118.12 (11)P5—C14—H14B109.5
C18—P1—Ni1111.04 (12)H14A—C14—H14B109.5
C15—P1—Ni1117.16 (12)P5—C14—H14C109.5
P3—C1—H1A109.5H14A—C14—H14C109.5
P3—C1—H1B109.5H14B—C14—H14C109.5
H1A—C1—H1B109.5P1—C15—H15A109.5
P3—C1—H1C109.5P1—C15—H15B109.5
H1A—C1—H1C109.5H15A—C15—H15B109.5
H1B—C1—H1C109.5P1—C15—H15C109.5
P6—C2—H2A109.5H15A—C15—H15C109.5
P6—C2—H2B109.5H15B—C15—H15C109.5
H2A—C2—H2B109.5P1—C16—H16A109.5
P6—C2—H2C109.5P1—C16—H16B109.5
H2A—C2—H2C109.5H16A—C16—H16B109.5
H2B—C2—H2C109.5P1—C16—H16C109.5
P4—C3—H3A109.5H16A—C16—H16C109.5
P4—C3—H3B109.5H16B—C16—H16C109.5
H3A—C3—H3B109.5P6—C17—H17A109.5
P4—C3—H3C109.5P6—C17—H17B109.5
H3A—C3—H3C109.5H17A—C17—H17B109.5
H3B—C3—H3C109.5P6—C17—H17C109.5
P3—C4—H4A109.5H17A—C17—H17C109.5
P3—C4—H4B109.5H17B—C17—H17C109.5
H4A—C4—H4B109.5P1—C18—H18A109.5
P3—C4—H4C109.5P1—C18—H18B109.5
H4A—C4—H4C109.5H18A—C18—H18B109.5
H4B—C4—H4C109.5P1—C18—H18C109.5
P4—C5—H5A109.5H18A—C18—H18C109.5
P4—C5—H5B109.5H18B—C18—H18C109.5
Table 1
Selected geometric parameters (Å) top
Ni1—P32.1754 (7)Ni1—Cl12.2901 (7)
Ni1—P12.2051 (8)Ni1—Cl22.4369 (8)
Ni1—P22.2088 (8)
Acknowledgements top

This work was supported by the NSFC (grant Nos. 20572062 and 20372042).

references
References top

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