Dichloridotris(trimethyl­phosphine)nickel(II)

Cao, R.; Wang, Q.; Sun, H.

doi:10.1107/S1600536808000317

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 2| February 2008| Page m335

doi:10.1107/S1600536808000317

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Dichloridotris(trimethylphosphine)nickel(II)

Ruixia Cao,^a Qibao Wang ^a and Hongjian Sun ^a ^*

^aSchool of Chemistry and Chemical Engineering, Shandong University, Shanda Nanlu 27, Jinan 250100, People's Republic of China
^*Correspondence e-mail: hjsun@sdu.edu.cn

(Received 21 November 2007; accepted 4 January 2008; online 11 January 2008)

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.

Related literature

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

Experimental

Crystal data

[NiCl₂(C₃H₉P)₃]
M_r = 357.83
Orthorhombic, P 2₁ 2₁ 2₁
a = 10.481 (2) Å
b = 11.741 (2) Å
c = 28.203 (6) Å
V = 3470.6 (12) Å³
Z = 8
Mo Kα radiation
μ = 1.68 mm⁻¹
T = 293 (2) K
0.30 × 0.25 × 0.22 mm

Data collection

Bruker P4 diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2004 ) T_min = 0.633, T_max = 0.709
26702 measured reflections
7557 independent reflections
7309 reflections with I > 2σ(I)
R_int = 0.073
4 standard reflections every 50 reflections intensity decay: 0.02%

Refinement

R[F² > 2σ(F²)] = 0.030
wR(F²) = 0.081
S = 1.06
7557 reflections
289 parameters
H-atom parameters constrained
Δρ_max = 0.63 e Å⁻³
Δρ_min = −0.84 e Å⁻³
Absolute structure: Flack (1983 ), 3276 Friedel pairs
Flack parameter: 0.006 (8)

Table 1
Selected bond lengths (Å)

Ni1—P3	2.1754 (7)
Ni1—P1	2.2051 (8)
Ni1—P2	2.2088 (8)
Ni1—Cl1	2.2901 (7)
Ni1—Cl2	2.4369 (8)

Data collection: XSCANS (Bruker, 2001 ); cell refinement: XSCANS; 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; software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808000317/br2064sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808000317/br2064Isup2.hkl

checkCIF report

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).

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

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]	F(000) = 1504
M_r = 357.83	D_x = 1.370 Mg m⁻³
Orthorhombic, P2₁2₁2₁	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2ab	Cell parameters from 6412 reflections
a = 10.481 (2) Å	θ = 1.6–24.2°
b = 11.741 (2) Å	µ = 1.68 mm⁻¹
c = 28.203 (6) Å	T = 293 K
V = 3470.6 (12) Å³	Block, blue
Z = 8	0.30 × 0.25 × 0.22 mm

Data collection top

Bruker P4 diffractometer	7309 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.073
Graphite monochromator	θ_max = 27.1°, θ_min = 1.4°
ω scans	h = −13→13
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	k = −15→14
T_min = 0.633, T_max = 0.709	l = −35→36
26702 measured reflections	4 standard reflections every 50 reflections
7557 independent reflections	intensity decay: 0.02%

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.030	H-atom parameters constrained
wR(F²) = 0.081	w = 1/[σ²(F_o²) + (0.0528P)²] where P = (F_o² + 2F_c²)/3
S = 1.06	(Δ/σ)_max = 0.002
7557 reflections	Δρ_max = 0.63 e Å⁻³
289 parameters	Δρ_min = −0.84 e Å⁻³
0 restraints	Absolute structure: Flack (1983)
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.006 (8)

Crystal data top

[NiCl₂(C₃H₉P)₃]	V = 3470.6 (12) Å³
M_r = 357.83	Z = 8
Orthorhombic, P2₁2₁2₁	Mo Kα radiation
a = 10.481 (2) Å	µ = 1.68 mm⁻¹
b = 11.741 (2) Å	T = 293 K
c = 28.203 (6) Å	0.30 × 0.25 × 0.22 mm

Data collection top

Bruker P4 diffractometer	7309 reflections with I > 2σ(I)
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	R_int = 0.073
T_min = 0.633, T_max = 0.709	4 standard reflections every 50 reflections
26702 measured reflections	intensity decay: 0.02%
7557 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.030	H-atom parameters constrained
wR(F²) = 0.081	Δρ_max = 0.63 e Å⁻³
S = 1.06	Δρ_min = −0.84 e Å⁻³
7557 reflections	Absolute structure: Flack (1983)
289 parameters	Absolute structure parameter: 0.006 (8)
0 restraints

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	0.72334 (3)	0.45758 (2)	0.757236 (10)	0.02415 (8)
Ni2	0.89293 (3)	−0.01317 (2)	0.980401 (10)	0.02370 (7)
P3	0.78376 (6)	0.52513 (5)	0.68901 (2)	0.02503 (12)
Cl1	0.59423 (6)	0.50132 (6)	0.82016 (2)	0.03563 (14)
P6	0.82135 (6)	0.04616 (5)	1.04857 (2)	0.02697 (13)
Cl4	0.83645 (6)	−0.15585 (5)	0.92899 (2)	0.03198 (13)
P5	0.77420 (6)	0.10238 (5)	0.93714 (2)	0.02798 (13)
Cl3	1.07328 (6)	0.10289 (5)	0.95390 (2)	0.03036 (12)
P2	0.88341 (7)	0.53231 (6)	0.79757 (2)	0.03072 (13)
P4	1.03877 (6)	−0.12977 (5)	1.00949 (2)	0.02620 (13)
Cl2	0.82969 (7)	0.27500 (5)	0.76850 (2)	0.03829 (15)
P1	0.56145 (7)	0.35783 (5)	0.72950 (2)	0.03075 (14)
C1	0.8573 (3)	0.6661 (2)	0.68588 (9)	0.0321 (5)
H1A	0.9325	0.6674	0.7053	0.048*
H1B	0.7980	0.7223	0.6971	0.048*
H1C	0.8799	0.6827	0.6536	0.048*
C2	0.6552 (3)	0.0922 (3)	1.05323 (11)	0.0411 (6)
H2A	0.6000	0.0318	1.0430	0.062*
H2B	0.6420	0.1579	1.0336	0.062*
H2C	0.6363	0.1111	1.0856	0.062*
C3	0.9884 (3)	−0.2639 (2)	1.03651 (11)	0.0374 (6)
H3A	1.0623	−0.3070	1.0456	0.056*
H3B	0.9390	−0.3068	1.0141	0.056*
H3C	0.9375	−0.2482	1.0640	0.056*
C4	0.6659 (3)	0.5473 (2)	0.64191 (9)	0.0343 (5)
H4A	0.7085	0.5718	0.6135	0.051*
H4B	0.6059	0.6045	0.6516	0.051*
H4C	0.6216	0.4772	0.6358	0.051*
C5	1.1530 (3)	−0.0718 (2)	1.05139 (9)	0.0343 (5)
H5A	1.2195	−0.1264	1.0568	0.051*
H5B	1.1106	−0.0552	1.0808	0.051*
H5C	1.1891	−0.0031	1.0387	0.051*
C6	0.7796 (3)	0.2542 (2)	0.95028 (10)	0.0379 (6)
H6A	0.8669	0.2787	0.9520	0.057*
H6B	0.7383	0.2683	0.9801	0.057*
H6C	0.7366	0.2956	0.9257	0.057*
C7	1.0461 (3)	0.5101 (3)	0.77589 (11)	0.0422 (6)
H7A	1.1057	0.5418	0.7981	0.063*
H7B	1.0560	0.5470	0.7457	0.063*
H7C	1.0618	0.4300	0.7724	0.063*
C8	0.8737 (4)	0.6837 (2)	0.81107 (11)	0.0452 (7)
H8A	0.7882	0.7024	0.8206	0.068*
H8B	0.8960	0.7270	0.7834	0.068*
H8C	0.9316	0.7016	0.8364	0.068*
C9	0.6053 (3)	0.0687 (2)	0.93156 (12)	0.0410 (6)
H9A	0.5664	0.1200	0.9093	0.061*
H9B	0.5647	0.0766	0.9619	0.061*
H9C	0.5958	−0.0081	0.9205	0.061*
C10	0.8988 (3)	0.4322 (2)	0.66093 (9)	0.0348 (6)
H10A	0.8632	0.3573	0.6579	0.052*
H10B	0.9747	0.4288	0.6799	0.052*
H10C	0.9196	0.4614	0.6301	0.052*
C11	1.1422 (3)	−0.1830 (2)	0.96282 (10)	0.0374 (6)
H11A	1.1893	−0.1209	0.9493	0.056*
H11B	1.0914	−0.2185	0.9387	0.056*
H11C	1.2005	−0.2378	0.9758	0.056*
C12	0.8933 (3)	0.4679 (3)	0.85625 (10)	0.0460 (7)
H12A	0.9048	0.3871	0.8531	0.069*
H12B	0.8159	0.4829	0.8734	0.069*
H12C	0.9643	0.4998	0.8732	0.069*
C13	0.8233 (3)	−0.0500 (2)	1.09934 (9)	0.0375 (6)
H13A	0.7871	−0.0123	1.1264	0.056*
H13B	0.9097	−0.0715	1.1063	0.056*
H13C	0.7743	−0.1168	1.0921	0.056*
C14	0.8227 (3)	0.1000 (3)	0.87549 (10)	0.0397 (6)
H14A	0.8126	0.0243	0.8631	0.060*
H14B	0.9105	0.1224	0.8731	0.060*
H14C	0.7706	0.1518	0.8577	0.060*
C15	0.5937 (4)	0.2620 (3)	0.67975 (11)	0.0461 (7)
H15A	0.6638	0.2130	0.6876	0.069*
H15B	0.6148	0.3060	0.6522	0.069*
H15C	0.5193	0.2168	0.6734	0.069*
C16	0.4163 (3)	0.4338 (3)	0.71333 (12)	0.0464 (7)
H16A	0.3517	0.3801	0.7043	0.070*
H16B	0.4337	0.4839	0.6872	0.070*
H16C	0.3869	0.4775	0.7400	0.070*
C17	0.9083 (3)	0.1690 (3)	1.07128 (12)	0.0450 (7)
H17A	0.8740	0.1905	1.1015	0.067*
H17B	0.8998	0.2314	1.0495	0.067*
H17C	0.9968	0.1498	1.0747	0.067*
C18	0.5033 (3)	0.2572 (3)	0.77371 (11)	0.0445 (7)
H18A	0.4602	0.2979	0.7985	0.067*
H18B	0.5740	0.2159	0.7869	0.067*
H18C	0.4451	0.2048	0.7590	0.067*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.02733 (15)	0.02569 (14)	0.01943 (13)	−0.00089 (11)	0.00117 (11)	0.00090 (10)
Ni2	0.02460 (15)	0.02604 (14)	0.02045 (13)	0.00344 (11)	−0.00030 (10)	0.00021 (10)
P3	0.0271 (3)	0.0272 (3)	0.0208 (2)	0.0007 (2)	0.0019 (2)	0.0027 (2)
Cl1	0.0369 (3)	0.0433 (3)	0.0267 (3)	0.0036 (3)	0.0070 (2)	−0.0058 (2)
P6	0.0296 (3)	0.0274 (3)	0.0238 (3)	0.0001 (2)	0.0045 (2)	−0.0017 (2)
Cl4	0.0346 (3)	0.0306 (3)	0.0308 (3)	−0.0030 (2)	−0.0036 (2)	−0.0047 (2)
P5	0.0269 (3)	0.0291 (3)	0.0279 (3)	0.0028 (3)	−0.0007 (2)	0.0050 (2)
Cl3	0.0298 (3)	0.0325 (3)	0.0288 (3)	−0.0044 (2)	0.0025 (2)	−0.0002 (2)
P2	0.0312 (3)	0.0346 (3)	0.0263 (3)	−0.0017 (3)	−0.0050 (2)	0.0017 (2)
P4	0.0255 (3)	0.0279 (3)	0.0252 (3)	0.0038 (2)	−0.0017 (2)	−0.0002 (2)
Cl2	0.0429 (4)	0.0313 (3)	0.0407 (3)	0.0099 (3)	0.0048 (3)	0.0083 (2)
P1	0.0335 (4)	0.0305 (3)	0.0283 (3)	−0.0073 (3)	0.0022 (3)	−0.0017 (2)
C1	0.0317 (14)	0.0327 (12)	0.0318 (12)	0.0001 (10)	0.0021 (10)	0.0063 (10)
C2	0.0389 (15)	0.0440 (15)	0.0403 (14)	0.0060 (13)	0.0135 (12)	0.0076 (12)
C3	0.0345 (14)	0.0347 (13)	0.0429 (15)	0.0016 (11)	−0.0011 (11)	0.0072 (11)
C4	0.0361 (14)	0.0391 (13)	0.0277 (11)	−0.0002 (11)	−0.0042 (10)	0.0042 (10)
C5	0.0309 (13)	0.0391 (13)	0.0330 (12)	0.0022 (11)	−0.0040 (10)	−0.0035 (10)
C6	0.0403 (15)	0.0314 (12)	0.0420 (14)	0.0032 (11)	0.0055 (12)	0.0074 (10)
C7	0.0335 (14)	0.0498 (16)	0.0433 (15)	−0.0002 (13)	−0.0032 (12)	0.0053 (13)
C8	0.0547 (19)	0.0398 (14)	0.0411 (15)	−0.0059 (13)	−0.0055 (14)	−0.0109 (12)
C9	0.0338 (15)	0.0399 (14)	0.0493 (16)	0.0014 (12)	−0.0068 (12)	0.0076 (12)
C10	0.0403 (15)	0.0352 (13)	0.0290 (12)	0.0045 (11)	0.0073 (11)	0.0004 (9)
C11	0.0325 (14)	0.0413 (14)	0.0383 (13)	0.0090 (11)	−0.0002 (11)	−0.0041 (11)
C12	0.0442 (17)	0.0624 (18)	0.0315 (13)	0.0027 (15)	−0.0078 (12)	0.0088 (13)
C13	0.0430 (16)	0.0403 (13)	0.0292 (12)	0.0020 (12)	0.0013 (11)	0.0028 (10)
C14	0.0417 (16)	0.0492 (15)	0.0282 (12)	0.0030 (13)	−0.0016 (11)	0.0059 (11)
C15	0.061 (2)	0.0377 (14)	0.0394 (15)	−0.0137 (14)	0.0029 (14)	−0.0092 (12)
C16	0.0386 (17)	0.0482 (16)	0.0525 (18)	−0.0079 (13)	−0.0049 (13)	0.0011 (13)
C17	0.0518 (18)	0.0394 (14)	0.0438 (15)	−0.0082 (13)	0.0086 (14)	−0.0130 (12)
C18	0.0526 (19)	0.0380 (14)	0.0429 (16)	−0.0113 (13)	0.0106 (14)	0.0021 (12)

Geometric parameters (Å, º) top

Ni1—P3	2.1754 (7)	C5—H5B	0.9600
Ni1—P1	2.2051 (8)	C5—H5C	0.9600
Ni1—P2	2.2088 (8)	C6—H6A	0.9600
Ni1—Cl1	2.2901 (7)	C6—H6B	0.9600
Ni1—Cl2	2.4369 (8)	C6—H6C	0.9600
Ni2—P6	2.1781 (7)	C7—H7A	0.9600
Ni2—P5	2.2086 (7)	C7—H7B	0.9600
Ni2—P4	2.2099 (7)	C7—H7C	0.9600
Ni2—Cl4	2.2932 (7)	C8—H8A	0.9600
Ni2—Cl3	2.4472 (7)	C8—H8B	0.9600
P3—C10	1.808 (3)	C8—H8C	0.9600
P3—C1	1.828 (3)	C9—H9A	0.9600
P3—C4	1.832 (3)	C9—H9B	0.9600
P6—C17	1.822 (3)	C9—H9C	0.9600
P6—C13	1.823 (3)	C10—H10A	0.9600
P6—C2	1.828 (3)	C10—H10B	0.9600
P5—C14	1.812 (3)	C10—H10C	0.9600
P5—C9	1.820 (3)	C11—H11A	0.9600
P5—C6	1.822 (3)	C11—H11B	0.9600
P2—C8	1.821 (3)	C11—H11C	0.9600
P2—C12	1.822 (3)	C12—H12A	0.9600
P2—C7	1.830 (3)	C12—H12B	0.9600
P4—C5	1.814 (3)	C12—H12C	0.9600
P4—C11	1.816 (3)	C13—H13A	0.9600
P4—C3	1.827 (3)	C13—H13B	0.9600
P1—C16	1.822 (4)	C13—H13C	0.9600
P1—C18	1.823 (3)	C14—H14A	0.9600
P1—C15	1.830 (3)	C14—H14B	0.9600
C1—H1A	0.9600	C14—H14C	0.9600
C1—H1B	0.9600	C15—H15A	0.9600
C1—H1C	0.9600	C15—H15B	0.9600
C2—H2A	0.9600	C15—H15C	0.9600
C2—H2B	0.9600	C16—H16A	0.9600
C2—H2C	0.9600	C16—H16B	0.9600
C3—H3A	0.9600	C16—H16C	0.9600
C3—H3B	0.9600	C17—H17A	0.9600
C3—H3C	0.9600	C17—H17B	0.9600
C4—H4A	0.9600	C17—H17C	0.9600
C4—H4B	0.9600	C18—H18A	0.9600
C4—H4C	0.9600	C18—H18B	0.9600
C5—H5A	0.9600	C18—H18C	0.9600

P3—Ni1—P1	95.96 (3)	H5A—C5—H5B	109.5
P3—Ni1—P2	95.14 (3)	P4—C5—H5C	109.5
P1—Ni1—P2	168.00 (3)	H5A—C5—H5C	109.5
P3—Ni1—Cl1	140.87 (3)	H5B—C5—H5C	109.5
P1—Ni1—Cl1	86.52 (3)	P5—C6—H6A	109.5
P2—Ni1—Cl1	87.75 (3)	P5—C6—H6B	109.5
P3—Ni1—Cl2	107.63 (3)	H6A—C6—H6B	109.5
P1—Ni1—Cl2	86.05 (3)	P5—C6—H6C	109.5
P2—Ni1—Cl2	86.26 (3)	H6A—C6—H6C	109.5
Cl1—Ni1—Cl2	111.50 (3)	H6B—C6—H6C	109.5
P6—Ni2—P5	95.57 (3)	P2—C7—H7A	109.5
P6—Ni2—P4	96.24 (3)	P2—C7—H7B	109.5
P5—Ni2—P4	167.25 (3)	H7A—C7—H7B	109.5
P6—Ni2—Cl4	134.65 (3)	P2—C7—H7C	109.5
P5—Ni2—Cl4	87.36 (3)	H7A—C7—H7C	109.5
P4—Ni2—Cl4	87.75 (3)	H7B—C7—H7C	109.5
P6—Ni2—Cl3	110.95 (3)	P2—C8—H8A	109.5
P5—Ni2—Cl3	85.67 (3)	P2—C8—H8B	109.5
P4—Ni2—Cl3	85.64 (3)	H8A—C8—H8B	109.5
Cl4—Ni2—Cl3	114.40 (3)	P2—C8—H8C	109.5
C10—P3—C1	104.12 (13)	H8A—C8—H8C	109.5
C10—P3—C4	102.56 (13)	H8B—C8—H8C	109.5
C1—P3—C4	96.91 (13)	P5—C9—H9A	109.5
C10—P3—Ni1	111.20 (9)	P5—C9—H9B	109.5
C1—P3—Ni1	119.71 (9)	H9A—C9—H9B	109.5
C4—P3—Ni1	119.79 (10)	P5—C9—H9C	109.5
C17—P6—C13	102.02 (15)	H9A—C9—H9C	109.5
C17—P6—C2	102.53 (15)	H9B—C9—H9C	109.5
C13—P6—C2	97.91 (14)	P3—C10—H10A	109.5
C17—P6—Ni2	113.03 (11)	P3—C10—H10B	109.5
C13—P6—Ni2	119.42 (10)	H10A—C10—H10B	109.5
C2—P6—Ni2	119.09 (11)	P3—C10—H10C	109.5
C14—P5—C9	100.74 (15)	H10A—C10—H10C	109.5
C14—P5—C6	101.65 (14)	H10B—C10—H10C	109.5
C9—P5—C6	105.08 (14)	P4—C11—H11A	109.5
C14—P5—Ni2	111.26 (10)	P4—C11—H11B	109.5
C9—P5—Ni2	117.54 (10)	H11A—C11—H11B	109.5
C6—P5—Ni2	118.11 (10)	P4—C11—H11C	109.5
C8—P2—C12	102.61 (16)	H11A—C11—H11C	109.5
C8—P2—C7	105.13 (16)	H11B—C11—H11C	109.5
C12—P2—C7	101.05 (15)	P2—C12—H12A	109.5
C8—P2—Ni1	116.93 (12)	P2—C12—H12B	109.5
C12—P2—Ni1	110.24 (12)	H12A—C12—H12B	109.5
C7—P2—Ni1	118.62 (10)	P2—C12—H12C	109.5
C5—P4—C11	101.98 (14)	H12A—C12—H12C	109.5
C5—P4—C3	104.01 (14)	H12B—C12—H12C	109.5
C11—P4—C3	100.25 (14)	P6—C13—H13A	109.5
C5—P4—Ni2	117.76 (9)	P6—C13—H13B	109.5
C11—P4—Ni2	110.91 (10)	H13A—C13—H13B	109.5
C3—P4—Ni2	119.26 (10)	P6—C13—H13C	109.5
C16—P1—C18	102.08 (17)	H13A—C13—H13C	109.5
C16—P1—C15	105.26 (17)	H13B—C13—H13C	109.5
C18—P1—C15	100.82 (14)	P5—C14—H14A	109.5
C16—P1—Ni1	118.12 (11)	P5—C14—H14B	109.5
C18—P1—Ni1	111.04 (12)	H14A—C14—H14B	109.5
C15—P1—Ni1	117.16 (12)	P5—C14—H14C	109.5
P3—C1—H1A	109.5	H14A—C14—H14C	109.5
P3—C1—H1B	109.5	H14B—C14—H14C	109.5
H1A—C1—H1B	109.5	P1—C15—H15A	109.5
P3—C1—H1C	109.5	P1—C15—H15B	109.5
H1A—C1—H1C	109.5	H15A—C15—H15B	109.5
H1B—C1—H1C	109.5	P1—C15—H15C	109.5
P6—C2—H2A	109.5	H15A—C15—H15C	109.5
P6—C2—H2B	109.5	H15B—C15—H15C	109.5
H2A—C2—H2B	109.5	P1—C16—H16A	109.5
P6—C2—H2C	109.5	P1—C16—H16B	109.5
H2A—C2—H2C	109.5	H16A—C16—H16B	109.5
H2B—C2—H2C	109.5	P1—C16—H16C	109.5
P4—C3—H3A	109.5	H16A—C16—H16C	109.5
P4—C3—H3B	109.5	H16B—C16—H16C	109.5
H3A—C3—H3B	109.5	P6—C17—H17A	109.5
P4—C3—H3C	109.5	P6—C17—H17B	109.5
H3A—C3—H3C	109.5	H17A—C17—H17B	109.5
H3B—C3—H3C	109.5	P6—C17—H17C	109.5
P3—C4—H4A	109.5	H17A—C17—H17C	109.5
P3—C4—H4B	109.5	H17B—C17—H17C	109.5
H4A—C4—H4B	109.5	P1—C18—H18A	109.5
P3—C4—H4C	109.5	P1—C18—H18B	109.5
H4A—C4—H4C	109.5	H18A—C18—H18B	109.5
H4B—C4—H4C	109.5	P1—C18—H18C	109.5
P4—C5—H5A	109.5	H18A—C18—H18C	109.5
P4—C5—H5B	109.5	H18B—C18—H18C	109.5

Experimental details

Crystal data
Chemical formula	[NiCl₂(C₃H₉P)₃]
M_r	357.83
Crystal system, space group	Orthorhombic, P2₁2₁2₁
Temperature (K)	293
a, b, c (Å)	10.481 (2), 11.741 (2), 28.203 (6)
V (Å³)	3470.6 (12)
Z	8
Radiation type	Mo Kα
µ (mm⁻¹)	1.68
Crystal size (mm)	0.30 × 0.25 × 0.22

Data collection
Diffractometer	Bruker P4 diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2004)
T_min, T_max	0.633, 0.709
No. of measured, independent and observed [I > 2σ(I)] reflections	26702, 7557, 7309
R_int	0.073
(sin θ/λ)_max (Å⁻¹)	0.641

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.030, 0.081, 1.06
No. of reflections	7557
No. of parameters	289
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.63, −0.84
Absolute structure	Flack (1983)
Absolute structure parameter	0.006 (8)

Computer programs: XSCANS (Bruker, 2001), SHELXTL (Sheldrick, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008).

Selected bond lengths (Å) top

Ni1—P3	2.1754 (7)	Ni1—Cl1	2.2901 (7)
Ni1—P1	2.2051 (8)	Ni1—Cl2	2.4369 (8)
Ni1—P2	2.2088 (8)

Acknowledgements

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

References

Bruker (2001). XSCANS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Doriand, Z. & Gray, H. B. (1966). J. Am. Chem. Soc. 88, 1394–1398. Google Scholar
Flack, H. D. (1983). Acta Cryst. A39, 876–881. CrossRef CAS Web of Science IUCr Journals Google Scholar
Jiao, G. L., Li, X. Y., Sun, H. J. & Xu, X. F. (2007). J. Organomet. Chem. 692, 4251–4258. Web of Science CSD CrossRef CAS Google Scholar
Sheldrick, G. M. (2001). SHELXTL. Version 5.0. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Sheldrick, G. M. (2004). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar