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Acta Crystallographica Section E: Structure Reports Online logoLink to Acta Crystallographica Section E: Structure Reports Online
. 2008 Jan 11;64(Pt 2):m335. doi: 10.1107/S1600536808000317

Dichloridotris(trimethyl­phosphine)nickel(II)

Ruixia Cao a, Qibao Wang a, Hongjian Sun a,*
PMCID: PMC2960155  PMID: 21201300

Abstract

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 ▶).graphic file with name e-64-0m335-scheme1.jpg

Experimental

Crystal data

  • [NiCl2(C3H9P)3]

  • M r = 357.83

  • Orthorhombic, Inline graphic

  • 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[F 2 > 2σ(F 2)] = 0.030

  • wR(F 2) = 0.081

  • S = 1.06

  • 7557 reflections

  • 289 parameters

  • H-atom parameters constrained

  • Δρmax = 0.63 e Å−3

  • Δρmin = −0.84 e Å−3

  • Absolute structure: Flack (1983 ▶), 3276 Friedel pairs

  • Flack parameter: 0.006 (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.

Supplementary Material

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

e-64-0m335-sup1.cif (23.2KB, cif)

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

e-64-0m335-Isup2.hkl (369.8KB, hkl)

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

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)
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Acknowledgments

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

supplementary crystallographic information

Comment

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 °).

Experimental

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

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).

Figures

Fig. 1.

Fig. 1.

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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.)

Crystal data

[NiCl2(C3H9P)3] F000 = 1504
Mr = 357.83 Dx = 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 = 1.6–24.2º
b = 11.741 (2) Å µ = 1.68 mm−1
c = 28.203 (6) Å T = 293 (2) K
V = 3470.6 (12) Å3 Block, blue
Z = 8 0.30 × 0.25 × 0.22 mm
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Data collection

Bruker P4 diffractometer Rint = 0.073
Radiation source: fine-focus sealed tube θmax = 27.1º
Monochromator: graphite θmin = 1.4º
T = 293(2) K h = −13→13
ω scans k = −15→14
Absorption correction: multi-scan(SADABS; Sheldrick, 2004) l = −35→36
Tmin = 0.633, Tmax = 0.709 4 standard reflections
26702 measured reflections every 50 reflections
7557 independent reflections intensity decay: 0.02%
7309 reflections with I > 2σ(I)
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Refinement

Refinement on F2 Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full H-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 = 1.06 Δρmax = 0.63 e Å−3
7557 reflections Δρmin = −0.84 e Å−3
289 parameters Extinction correction: none
Primary atom site location: structure-invariant direct methods Absolute structure: Flack (1983)
Secondary atom site location: difference Fourier map Flack parameter: 0.006 (8)
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Special details

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

x y z Uiso*/Ueq
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*
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Atomic displacement parameters (Å2)

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)
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Geometric parameters (Å, °)

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
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Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BR2064).

References

  1. Bruker (2001). XSCANS Bruker AXS Inc., Madison, Wisconsin, USA.
  2. Doriand, Z. & Gray, H. B. (1966). J. Am. Chem. Soc.88, 1394–1398.
  3. Flack, H. D. (1983). Acta Cryst. A39, 876–881.
  4. Jiao, G. L., Li, X. Y., Sun, H. J. & Xu, X. F. (2007). J. Organomet. Chem.692, 4251–4258.
  5. Sheldrick, G. M. (2001). SHELXTL Version 5.0. Bruker AXS Inc., Madison, Wisconsin, USA.
  6. Sheldrick, G. M. (2004). SADABS University of Göttingen, Germany.
  7. Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [DOI] [PubMed]

Associated Data

This section collects any data citations, data availability statements, or supplementary materials included in this article.

Supplementary Materials

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

e-64-0m335-sup1.cif (23.2KB, cif)

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

e-64-0m335-Isup2.hkl (369.8KB, hkl)

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography

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