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The crystal and molecular structure of [bis­(di­cyclo­hexyl­phosphino)­ethane-κ2P,P′]­bromo­(phenyl)­nickel(II) chloro­ben­zene solvate, [NiBr(C6H5)(dcpe)]·C6H5Cl [dcpe is bis­(di­cyclo­hexyl­phosphino)­ethane, (C6H11)2PCH2CH2P(C6H11)2 or C26H48P2], is reported. The complex is square planar and the Ni—P bond trans to the phenyl group is longer than the bond trans to Br, reflecting the stronger trans influence of the aromatic ring.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680201509X/wn6116sup1.cif
Contains datablocks global, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680201509X/wn6116IIsup2.hkl
Contains datablock II

CCDC reference: 197455

Key indicators

  • Single-crystal X-ray study
  • T = 200 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.030
  • wR factor = 0.031
  • Data-to-parameter ratio = 10.7

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
DENSD_01 Alert C The ratio of the submitted crystal density and that calculated from the formula is outside the range 0.99 <> 1.01 Crystal density given = 1.280 Calculated crystal density = 1.335 PLAT_732 Alert C Angle Calc 119.7(4), Rep 119.69(19) .... 2.11 s.u-Ratio C4 -C3 -H31 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 120.3(4), Rep 120.31(19) .... 2.11 s.u-Ratio C3 -C4 -H41 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 120.8(4), Rep 120.77(19) .... 2.11 s.u-Ratio C5 -C4 -H41 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 119.9(4), Rep 119.90(19) .... 2.11 s.u-Ratio C4 -C5 -H51 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.1(3), Rep 109.07(9) .... 3.33 s.u-Ratio P1 -C7 -H71 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.3(3), Rep 109.29(9) .... 3.33 s.u-Ratio P1 -C7 -H72 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.4(3), Rep 109.39(14) .... 2.14 s.u-Ratio C8 -C7 -H72 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 108.7(3), Rep 108.75(9) .... 3.33 s.u-Ratio P2 -C8 -H81 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.1(3), Rep 109.10(9) .... 3.33 s.u-Ratio P2 -C8 -H82 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.5(4), Rep 109.45(18) .... 2.22 s.u-Ratio C12 -C11 -H112 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.9(4), Rep 109.94(17) .... 2.35 s.u-Ratio C11 -C12 -H121 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.8(4), Rep 109.81(18) .... 2.22 s.u-Ratio C13 -C12 -H121 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.5(4), Rep 109.45(18) .... 2.22 s.u-Ratio C14 -C13 -H132 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.4(4), Rep 109.38(16) .... 2.50 s.u-Ratio C9 -C14 -H141 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 106.0(2), Rep 106.04(9) .... 2.22 s.u-Ratio P1 -C15 -H151 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.8(4), Rep 109.80(19) .... 2.11 s.u-Ratio C16 -C17 -H171 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.7(4), Rep 109.76(18) .... 2.22 s.u-Ratio C17 -C18 -H182 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.4(4), Rep 109.28(18) .... 2.22 s.u-Ratio C19 -C18 -H182 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.4(4), Rep 109.41(18) .... 2.22 s.u-Ratio C18 -C19 -H191 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.1(4), Rep 109.14(17) .... 2.35 s.u-Ratio C20 -C19 -H191 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 108.4(4), Rep 108.40(19) .... 2.11 s.u-Ratio C20 -C19 -H192 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 107.2(2), Rep 107.18(8) .... 2.50 s.u-Ratio P2 -C21 -H211 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 108.6(4), Rep 108.65(17) .... 2.35 s.u-Ratio C22 -C23 -H231 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 108.7(4), Rep 108.72(16) .... 2.50 s.u-Ratio C26 -C25 -H251 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.5(4), Rep 109.43(17) .... 2.35 s.u-Ratio C24 -C25 -H252 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.0(4), Rep 109.08(16) .... 2.50 s.u-Ratio C25 -C26 -H262 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 106.5(2), Rep 106.56(9) .... 2.22 s.u-Ratio P2 -C27 -H271 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 108.8(4), Rep 108.84(18) .... 2.22 s.u-Ratio C29 -C28 -H281 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.6(4), Rep 109.70(18) .... 2.22 s.u-Ratio C28 -C29 -H291 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.2(4), Rep 109.26(19) .... 2.11 s.u-Ratio C30 -C29 -H291 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 108.6(4), Rep 108.63(18) .... 2.22 s.u-Ratio C28 -C29 -H292 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.7(4), Rep 109.70(18) .... 2.22 s.u-Ratio C29 -C30 -H302 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 109.7(4), Rep 109.68(18) .... 2.22 s.u-Ratio C30 -C31 -H311 1.555 1.555 1.555 PLAT_732 Alert C Angle Calc 110.1(4), Rep 110.04(17) .... 2.35 s.u-Ratio C32 -C31 -H311 1.555 1.555 1.555 PLAT_741 Alert C Bond Calc 1.001(5), Rep 1.00000 .... Missing s.u. C2 -H21 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(5), Rep 1.00000 .... Missing s.u. C3 -H31 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(4), Rep 1.00000 .... Missing s.u. C4 -H41 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(5), Rep 1.00000 .... Missing s.u. C5 -H51 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(5), Rep 1.00000 .... Missing s.u. C6 -H61 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(5), Rep 1.00000 .... Missing s.u. C7 -H71 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(4), Rep 1.00000 .... Missing s.u. C7 -H72 1.555 1.555 PLAT_741 Alert C Bond Calc 0.999(4), Rep 1.00000 .... Missing s.u. C8 -H81 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(4), Rep 1.00000 .... Missing s.u. C8 -H82 1.555 1.555 PLAT_741 Alert C Bond Calc 1.001(4), Rep 1.00000 .... Missing s.u. C9 -H91 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(4), Rep 1.00000 .... Missing s.u. C10 -H101 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(4), Rep 1.00000 .... Missing s.u. C10 -H102 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(6), Rep 1.00000 .... Missing s.u. C11 -H111 1.555 1.555 PLAT_741 Alert C Bond Calc 0.999(4), Rep 1.00000 .... Missing s.u. C11 -H112 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(5), Rep 1.00000 .... Missing s.u. C12 -H121 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(6), Rep 1.00000 .... Missing s.u. C12 -H122 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(6), Rep 1.00000 .... Missing s.u. C13 -H131 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(5), Rep 1.00000 .... Missing s.u. C13 -H132 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(5), Rep 1.00000 .... Missing s.u. C14 -H141 1.555 1.555 PLAT_741 Alert C Bond Calc 1.001(6), Rep 1.00000 .... Missing s.u. C14 -H142 1.555 1.555 PLAT_741 Alert C Bond Calc 1.001(4), Rep 1.00000 .... Missing s.u. C15 -H151 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(4), Rep 1.00000 .... Missing s.u. C16 -H161 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(5), Rep 1.00000 .... Missing s.u. C16 -H162 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(6), Rep 1.00000 .... Missing s.u. C17 -H171 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(5), Rep 1.00000 .... Missing s.u. C17 -H172 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(6), Rep 1.00000 .... Missing s.u. C18 -H181 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(5), Rep 1.00000 .... Missing s.u. C18 -H182 1.555 1.555 PLAT_741 Alert C Bond Calc 0.999(5), Rep 1.00000 .... Missing s.u. C19 -H191 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(6), Rep 1.00000 .... Missing s.u. C19 -H192 1.555 1.555 PLAT_741 Alert C Bond Calc 1.001(4), Rep 1.00000 .... Missing s.u. C20 -H201 1.555 1.555 PLAT_741 Alert C Bond Calc 0.999(4), Rep 1.00000 .... Missing s.u. C20 -H202 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(4), Rep 1.00000 .... Missing s.u. C21 -H211 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(4), Rep 1.00000 .... Missing s.u. C22 -H221 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(4), Rep 1.00000 .... Missing s.u. C22 -H222 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(4), Rep 1.00000 .... Missing s.u. C23 -H231 1.555 1.555 PLAT_741 Alert C Bond Calc 0.999(5), Rep 1.00000 .... Missing s.u. C23 -H232 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(5), Rep 1.00000 .... Missing s.u. C24 -H241 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(4), Rep 1.00000 .... Missing s.u. C24 -H242 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(4), Rep 1.00000 .... Missing s.u. C25 -H251 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(4), Rep 1.00000 .... Missing s.u. C25 -H252 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(5), Rep 1.00000 .... Missing s.u. C26 -H261 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(4), Rep 1.00000 .... Missing s.u. C26 -H262 1.555 1.555 PLAT_741 Alert C Bond Calc 0.999(4), Rep 1.00000 .... Missing s.u. C27 -H271 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(4), Rep 1.00000 .... Missing s.u. C28 -H281 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(5), Rep 1.00000 .... Missing s.u. C28 -H282 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(5), Rep 1.00000 .... Missing s.u. C29 -H291 1.555 1.555 PLAT_741 Alert C Bond Calc 0.999(6), Rep 1.00000 .... Missing s.u. C29 -H292 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(6), Rep 1.00000 .... Missing s.u. C30 -H301 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(5), Rep 1.00000 .... Missing s.u. C30 -H302 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(5), Rep 1.00000 .... Missing s.u. C31 -H311 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(6), Rep 1.00000 .... Missing s.u. C31 -H312 1.555 1.555 PLAT_741 Alert C Bond Calc 0.999(4), Rep 1.00000 .... Missing s.u. C32 -H321 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(4), Rep 1.00000 .... Missing s.u. C32 -H322 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(7), Rep 1.00000 .... Missing s.u. C34 -H341 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(7), Rep 1.00000 .... Missing s.u. C35 -H351 1.555 1.555 PLAT_741 Alert C Bond Calc 1.001(6), Rep 1.00000 .... Missing s.u. C36 -H361 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(7), Rep 1.00000 .... Missing s.u. C37 -H371 1.555 1.555 PLAT_741 Alert C Bond Calc 1.000(7), Rep 1.00000 .... Missing s.u. C38 -H381 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(4), Rep 109.47 .... Missing s.u. H71 -C7 -H72 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(3), Rep 109.47 .... Missing s.u. H81 -C8 -H82 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(4), Rep 109.47 .... Missing s.u. H101 -C10 -H102 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(4), Rep 109.47 .... Missing s.u. H111 -C11 -H112 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.4(5), Rep 109.47 .... Missing s.u. H121 -C12 -H122 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(4), Rep 109.47 .... Missing s.u. H131 -C13 -H132 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(5), Rep 109.47 .... Missing s.u. H141 -C14 -H142 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(4), Rep 109.47 .... Missing s.u. H161 -C16 -H162 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(4), Rep 109.47 .... Missing s.u. H171 -C17 -H172 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.4(5), Rep 109.47 .... Missing s.u. H181 -C18 -H182 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(5), Rep 109.47 .... Missing s.u. H191 -C19 -H192 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(4), Rep 109.47 .... Missing s.u. H201 -C20 -H202 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(4), Rep 109.47 .... Missing s.u. H221 -C22 -H222 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(4), Rep 109.47 .... Missing s.u. H231 -C23 -H232 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.4(4), Rep 109.47 .... Missing s.u. H241 -C24 -H242 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(4), Rep 109.47 .... Missing s.u. H251 -C25 -H252 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(4), Rep 109.47 .... Missing s.u. H261 -C26 -H262 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(4), Rep 109.47 .... Missing s.u. H281 -C28 -H282 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(4), Rep 109.47 .... Missing s.u. H291 -C29 -H292 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(5), Rep 109.47 .... Missing s.u. H301 -C30 -H302 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(5), Rep 109.47 .... Missing s.u. H311 -C31 -H312 1.555 1.555 1.555 PLAT_742 Alert C Angle Calc 109.5(4), Rep 109.47 .... Missing s.u. H321 -C32 -H322 1.555 1.555 1.555
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
115 Alert Level C = Please check

Comment top

Arylnickel(II) complexes are usually prepared by oxidative addition of aryl halides to a nickel(0) centre. Compound (II) and related species have been obtained by reaction of bromobenzene with [Ni(η2-C2H4)(dcpe)] (Bennett et al., 1985) or with [NiBr2(PPh3)2] in the presence of activated zinc, followed by ligand exchange with dcpe (Bennett & Wenger, 1995). The present sample, however, was isolated after hydrolysis of the arylnickel(II) complex (I) bearing a boronic ester group in the ortho position. The latter complex, which has been studied as a precursor to the benzynenickel(0) complex [Ni(η2-C6H4)(dcpe)] (Bennett et al., 2002), is highly reactive towards moisture, due to the large steric interaction between the boronic ester substituent and the cyclohexyl groups on the diphosphine ligand. Cleavage of the C—B bond in (I) occurs readily and compound (II) was obtained from attempted crystallizations of (I).

Complex (II) crystallized as a chlorobenzene solvate, and the solvent molecule was clearly defined. The nickel centre of (II) is in a square-planar environment, with C1—Ni—P1 and Br1—Ni—P2 angles of 170.47 (8) and 173.61 (3)°, respectively. The Ni—P distances are not equivalent, the bond trans to atom C1 being longer than the bond trans to Br, as expected from the larger trans influence of the phenyl group. Similarly, the Ni—C1 distance [1.981 (3) Å] is longer than that in complexes having trans phosphines and a halide trans to Ni—C; see for example [NiCl(o-C6H4Me)(PPh3)2] (1.900 Å; Spek et al., 2000) and [NiCl(o-C6H4CF3)(PPh3)2] (1.890%A; Lutz et al., 1998). The other geometric data of complex (II) are unexceptional.

Experimental top

A solution of the boronic ester complex (I) (50 mg) was prepared with chlorobenzene (3 ml) and pentane was diffused into it at room temperature. Crystallization was very slow, but after 72 h, orange crystals of the title compound formed. Attempted recrystallizations of the title compound from CH2Cl2/hexane or THF/hexane had similar outcomes. The NMR data are analogous to those of the iodo analogue [NiI(Ph)(dcpe)] (Bennett et al., 1985). 1H NMR (300 MHz, CD2Cl2, p.p.m.): δ 1.15–1.95 (m, 42H, dcpe), 2.04–2.18 (m, 4H, dcpe), 2.34–2.46 (m, 2H, dcpe), 6.77 (t, 1H, J = 7.2 Hz, p-Ph), 6.95 (t, 2H, J = 7.2 Hz, m-Ph), 7.45 (br t, 2H, J = 6.0 Hz, o-Ph); 13C NMR (75.4 MHz, CD2Cl2, p.p.m.): δ 19.24 (dd, J = 19.9, 11.7 Hz, PCH2), 24.90 (t, J = 23.1 Hz, PCH2), 26.17–30.68 (m, CH2), 34.50 (d, J = 18.7 Hz, PCH), 34.75 (br d, J = 25.3 Hz, PCH), 121.88 (s, p-CH), 126.04 (d, J = 6.0 Hz, o-CH), 137.68 (s, m-CH), 159.10 (dd, J = 85.7, 37.5, Ni—C); 31P{1H} NMR (80.96 MHz, CD2Cl2, p.p.m.): δ 63.3 (d), 67.6 (d, JPP = 19.5 Hz)

Refinement top

H atoms were included at calculated positions riding on the attached C atom and individual isotropic displacement parameters were refined.

Computing details top

Data collection: COLLECT (Nonius, 1997); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: CRYSTALS (Watkin et al., 2001) and maXus (Mackay et al., 1999); molecular graphics: CAMERON (Watkin et al., 1996); software used to prepare material for publication: CRYSTALS and maXus.

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound, with the atom-labelling scheme. Dispacement ellipsoids are drawn at the 50% probability level and H atoms have been omitted for clarity.
[bis(dicyclohexylphosphino)ethane-κ2P,P']bromo(phenyl)nickel(II) chlorobenzene solvate top
Crystal data top
[NiBr(C6H5)(C26H48P2)]·C6H5ClF(000) = 1584
Mr = 750.89Dx = 1.280 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 11.8308 (1) ÅCell parameters from 89742 reflections
b = 22.7790 (3) Åθ = 2.9–27.5°
c = 14.5238 (2) ŵ = 1.77 mm1
β = 107.4072 (5)°T = 200 K
V = 3734.82 (8) Å3Prism, yellow
Z = 40.20 × 0.16 × 0.15 mm
Data collection top
Nonius KappaCCD
diffractometer
4771 reflections with I > 3σ(I)
Radiation source: fine-focus sealed tubeRint = 0.044
ϕ and ω scansθmax = 27.5°, θmin = 2.9°
Absorption correction: integration
(Coppens, 1970)
h = 1515
Tmin = 0.662, Tmax = 0.808k = 2929
94198 measured reflectionsl = 1818
8553 independent reflections
Refinement top
Refinement on FSecondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.030Only H-atom displacement parameters refined
wR(F2) = 0.031 Chebychev polynomial with 4 parameters 0.522, -.637, 0.215, -.339 (Carruthers & Watkin , 1979)
S = 1.05(Δ/σ)max = 0.001
4771 reflectionsΔρmax = 0.56 e Å3
446 parametersΔρmin = 0.51 e Å3
Primary atom site location: structure-invariant direct methods
Crystal data top
[NiBr(C6H5)(C26H48P2)]·C6H5ClV = 3734.82 (8) Å3
Mr = 750.89Z = 4
Monoclinic, P21/nMo Kα radiation
a = 11.8308 (1) ŵ = 1.77 mm1
b = 22.7790 (3) ÅT = 200 K
c = 14.5238 (2) Å0.20 × 0.16 × 0.15 mm
β = 107.4072 (5)°
Data collection top
Nonius KappaCCD
diffractometer
8553 independent reflections
Absorption correction: integration
(Coppens, 1970)
4771 reflections with I > 3σ(I)
Tmin = 0.662, Tmax = 0.808Rint = 0.044
94198 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.030446 parameters
wR(F2) = 0.031Only H-atom displacement parameters refined
S = 1.05Δρmax = 0.56 e Å3
4771 reflectionsΔρmin = 0.51 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.46259 (3)0.280369 (14)0.76672 (2)0.0320
Br10.50019 (3)0.237201 (14)0.91905 (2)0.0479
Cl10.12559 (17)0.45200 (6)0.91951 (11)0.1250
P10.43070 (6)0.19424 (3)0.69151 (5)0.0341
P20.41007 (6)0.32327 (3)0.62946 (5)0.0331
C10.5164 (2)0.35707 (11)0.82877 (19)0.0346
C20.6396 (3)0.36330 (13)0.8622 (2)0.0464
C30.6881 (3)0.41487 (14)0.9088 (2)0.0522
C40.6166 (3)0.45927 (14)0.9227 (2)0.0579
C50.4953 (3)0.45158 (14)0.8913 (2)0.0543
C60.4465 (3)0.39970 (13)0.8444 (2)0.0462
C70.4077 (3)0.20758 (12)0.5624 (2)0.0415
C80.3512 (2)0.26822 (12)0.5332 (2)0.0384
C90.5612 (2)0.14528 (11)0.7269 (2)0.0387
C100.6748 (2)0.17813 (13)0.7289 (2)0.0450
C110.7839 (2)0.13823 (14)0.7623 (3)0.0507
C120.7689 (3)0.08257 (15)0.7015 (3)0.0601
C130.6565 (3)0.05017 (14)0.7002 (3)0.0615
C140.5472 (3)0.08941 (13)0.6649 (3)0.0517
C150.3056 (2)0.14549 (12)0.6914 (2)0.0391
C160.3216 (3)0.11250 (14)0.7864 (2)0.0502
C170.2187 (3)0.06967 (15)0.7773 (3)0.0592
C180.1001 (3)0.10106 (16)0.7466 (3)0.0616
C190.0837 (3)0.13651 (16)0.6551 (3)0.0578
C200.1872 (2)0.17861 (13)0.6627 (2)0.0455
C210.2859 (2)0.37508 (12)0.6137 (2)0.0369
C220.1879 (2)0.34906 (13)0.6516 (2)0.0427
C230.0915 (3)0.39504 (14)0.6456 (2)0.0512
C240.0406 (3)0.41700 (14)0.5431 (2)0.0511
C250.1357 (3)0.44119 (13)0.5029 (2)0.0461
C260.2343 (3)0.39626 (12)0.5102 (2)0.0414
C270.5197 (2)0.36377 (12)0.5862 (2)0.0385
C280.5440 (3)0.42697 (12)0.6240 (2)0.0445
C290.6324 (3)0.45680 (14)0.5813 (3)0.0547
C300.7479 (3)0.42215 (15)0.6046 (3)0.0642
C310.7253 (3)0.35961 (15)0.5663 (3)0.0619
C320.6350 (2)0.32872 (13)0.6060 (2)0.0453
C330.0998 (4)0.37829 (18)0.8979 (3)0.0677
C340.1933 (4)0.3385 (2)0.9245 (3)0.0744
C350.1682 (4)0.2797 (2)0.9050 (3)0.0761
C360.0554 (5)0.2615 (2)0.8595 (3)0.0834
C370.0367 (4)0.2994 (2)0.8329 (3)0.0834
C380.0136 (4)0.3598 (2)0.8543 (3)0.0730
H210.6920 (3)0.33094 (13)0.8523 (2)0.049 (9)*
H310.7761 (3)0.41972 (14)0.9318 (2)0.067 (11)*
H410.6521 (3)0.49642 (14)0.9555 (2)0.06 (1)*
H510.4420 (3)0.48313 (14)0.9023 (2)0.067 (11)*
H610.3586 (3)0.39431 (13)0.8217 (2)0.068 (11)*
H710.4859 (3)0.20609 (12)0.5492 (2)0.035 (7)*
H720.3544 (3)0.17652 (12)0.5239 (2)0.044 (8)*
H810.3687 (2)0.28158 (12)0.4734 (2)0.034 (7)*
H820.2635 (2)0.26493 (12)0.5203 (2)0.043 (8)*
H910.5694 (2)0.13146 (11)0.7940 (2)0.045 (8)*
H1010.6848 (2)0.21262 (13)0.7732 (2)0.053 (9)*
H1020.6669 (2)0.19213 (13)0.6620 (2)0.051 (9)*
H1110.7950 (2)0.12656 (14)0.8308 (3)0.06 (1)*
H1120.8553 (2)0.16017 (14)0.7580 (3)0.075 (12)*
H1210.8390 (3)0.05629 (15)0.7273 (3)0.074 (11)*
H1220.7628 (3)0.09403 (15)0.6337 (3)0.072 (12)*
H1310.6639 (3)0.03752 (14)0.7677 (3)0.06 (1)*
H1320.6467 (3)0.01483 (14)0.6577 (3)0.079 (12)*
H1410.4750 (3)0.06755 (13)0.6677 (3)0.069 (11)*
H1420.5380 (3)0.10126 (13)0.5967 (3)0.063 (11)*
H1510.3030 (2)0.11455 (12)0.6419 (2)0.055 (9)*
H1610.3214 (3)0.14192 (14)0.8375 (2)0.06 (1)*
H1620.3988 (3)0.09101 (14)0.8049 (2)0.054 (9)*
H1710.2293 (3)0.04915 (15)0.8402 (3)0.074 (12)*
H1720.2194 (3)0.04017 (15)0.7265 (3)0.06 (1)*
H1810.0974 (3)0.12853 (16)0.7996 (3)0.071 (12)*
H1820.0345 (3)0.07179 (16)0.7361 (3)0.075 (12)*
H1910.0086 (3)0.15959 (16)0.6410 (3)0.074 (11)*
H1920.0786 (3)0.10850 (16)0.6010 (3)0.082 (13)*
H2010.1893 (2)0.20875 (13)0.7133 (2)0.044 (8)*
H2020.1761 (2)0.19851 (13)0.5993 (2)0.044 (8)*
H2110.3181 (2)0.41070 (12)0.6531 (2)0.034 (7)*
H2210.2232 (2)0.33592 (13)0.7199 (2)0.055 (9)*
H2220.1517 (2)0.31463 (13)0.6106 (2)0.039 (8)*
H2310.1277 (3)0.42907 (14)0.6876 (2)0.06 (1)*
H2320.0270 (3)0.37772 (14)0.6684 (2)0.06 (1)*
H2410.0198 (3)0.44815 (14)0.5406 (2)0.054 (9)*
H2420.0019 (3)0.38304 (14)0.5020 (2)0.046 (8)*
H2510.1709 (3)0.47673 (13)0.5412 (2)0.040 (8)*
H2520.0993 (3)0.45245 (13)0.4338 (2)0.051 (9)*
H2610.2986 (3)0.41464 (12)0.4883 (2)0.034 (7)*
H2620.2007 (3)0.36189 (12)0.4681 (2)0.048 (9)*
H2710.4840 (2)0.36861 (12)0.5150 (2)0.043 (8)*
H2810.5783 (3)0.42575 (12)0.6958 (2)0.051 (9)*
H2820.4682 (3)0.44964 (12)0.6064 (2)0.051 (9)*
H2910.6494 (3)0.49741 (14)0.6081 (3)0.051 (9)*
H2920.5970 (3)0.45887 (14)0.5097 (3)0.072 (12)*
H3010.7834 (3)0.42029 (15)0.6763 (3)0.073 (12)*
H3020.8043 (3)0.44215 (15)0.5755 (3)0.086 (13)*
H3110.8014 (3)0.33716 (15)0.5842 (3)0.07 (1)*
H3120.6922 (3)0.36139 (15)0.4944 (3)0.063 (11)*
H3210.6704 (2)0.32440 (13)0.6773 (2)0.049 (9)*
H3220.6168 (2)0.28901 (13)0.5758 (2)0.033 (7)*
H3410.2755 (4)0.3525 (2)0.9579 (3)0.068 (11)*
H3510.2329 (4)0.2498 (2)0.9240 (3)0.100 (15)*
H3610.0404 (5)0.2188 (2)0.8444 (3)0.19 (3)*
H3710.1188 (4)0.2854 (2)0.7991 (3)0.070 (11)*
H3810.0792 (4)0.3893 (2)0.8380 (3)0.127 (19)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.02780 (15)0.02679 (16)0.03603 (19)0.00113 (13)0.00120 (13)0.00099 (13)
Br10.05188 (17)0.03917 (15)0.04293 (16)0.00306 (13)0.00057 (13)0.00557 (13)
Cl10.1838 (16)0.0630 (7)0.104 (1)0.0126 (8)0.006 (1)0.0053 (7)
P10.0284 (3)0.0271 (3)0.0415 (4)0.0008 (3)0.0026 (3)0.0011 (3)
P20.0282 (3)0.0278 (3)0.0384 (4)0.0001 (2)0.0025 (3)0.0001 (3)
C10.0351 (13)0.0326 (14)0.0308 (13)0.006 (1)0.0015 (11)0.008 (1)
C20.0410 (15)0.0433 (16)0.0490 (18)0.0022 (13)0.0042 (13)0.0030 (13)
C30.0519 (19)0.0463 (18)0.0521 (19)0.0141 (15)0.0059 (15)0.0012 (14)
C40.075 (2)0.0376 (17)0.055 (2)0.0140 (16)0.0095 (17)0.0064 (14)
C50.068 (2)0.0407 (17)0.0506 (19)0.0060 (15)0.0117 (16)0.0066 (14)
C60.0467 (17)0.0475 (17)0.0392 (17)0.0064 (13)0.0049 (13)0.0043 (13)
C70.0368 (14)0.0338 (15)0.0482 (17)0.0002 (11)0.0042 (12)0.0055 (12)
C80.0345 (13)0.0385 (15)0.0366 (14)0.0004 (11)0.0024 (11)0.0004 (12)
C90.0292 (13)0.0312 (13)0.0510 (18)0.002 (1)0.0048 (12)0.0016 (12)
C100.0332 (14)0.0386 (15)0.060 (2)0.0007 (11)0.0089 (13)0.0000 (14)
C110.0286 (14)0.0568 (19)0.065 (2)0.0037 (13)0.0110 (14)0.0009 (16)
C120.0402 (17)0.0534 (19)0.089 (3)0.0105 (14)0.0226 (17)0.0006 (18)
C130.0468 (18)0.0384 (17)0.098 (3)0.0089 (14)0.0205 (18)0.0063 (17)
C140.0379 (16)0.0334 (15)0.079 (3)0.0036 (12)0.0106 (15)0.0091 (15)
C150.0285 (13)0.0322 (14)0.0527 (18)0.001 (1)0.0064 (12)0.0030 (12)
C160.0347 (15)0.0439 (17)0.067 (2)0.0034 (12)0.0070 (14)0.0118 (15)
C170.0438 (17)0.0456 (18)0.084 (3)0.0072 (14)0.0133 (17)0.0086 (18)
C180.0432 (18)0.058 (2)0.086 (3)0.0068 (15)0.0234 (18)0.0021 (19)
C190.0299 (15)0.062 (2)0.076 (2)0.0014 (14)0.0079 (15)0.0051 (18)
C200.0321 (14)0.0435 (16)0.0566 (19)0.0038 (12)0.0069 (13)0.0039 (14)
C210.0314 (13)0.0306 (13)0.0438 (16)0.001 (1)0.0038 (11)0.0015 (11)
C220.0367 (15)0.0392 (15)0.0505 (18)0.0016 (12)0.0103 (13)0.0038 (13)
C230.0433 (17)0.0494 (18)0.063 (2)0.0057 (14)0.0195 (15)0.0009 (15)
C240.0405 (16)0.0426 (17)0.068 (2)0.0104 (13)0.0134 (15)0.0021 (15)
C250.0435 (15)0.0350 (15)0.0543 (19)0.0066 (12)0.0063 (14)0.0028 (13)
C260.0380 (14)0.0365 (14)0.0459 (17)0.0033 (11)0.0066 (12)0.0024 (12)
C270.0331 (13)0.0367 (14)0.0412 (16)0.0002 (11)0.0045 (11)0.0037 (12)
C280.0387 (15)0.0331 (15)0.057 (2)0.0027 (12)0.0073 (13)0.0068 (13)
C290.0458 (17)0.0408 (17)0.073 (2)0.0056 (13)0.0107 (16)0.0098 (15)
C300.0400 (18)0.053 (2)0.097 (3)0.0058 (15)0.0172 (19)0.0113 (19)
C310.0429 (18)0.056 (2)0.090 (3)0.0035 (15)0.0248 (18)0.0093 (19)
C320.0365 (15)0.0381 (15)0.061 (2)0.0002 (12)0.0137 (14)0.0064 (14)
C330.085 (3)0.064 (2)0.052 (2)0.003 (2)0.0155 (19)0.0069 (17)
C340.066 (3)0.091 (3)0.070 (3)0.001 (2)0.025 (2)0.015 (2)
C350.078 (3)0.075 (3)0.085 (3)0.014 (2)0.038 (2)0.005 (2)
C360.093 (3)0.079 (3)0.088 (3)0.004 (3)0.042 (3)0.008 (2)
C370.077 (3)0.107 (4)0.075 (3)0.002 (3)0.035 (2)0.012 (3)
C380.073 (3)0.085 (3)0.063 (3)0.014 (2)0.023 (2)0.011 (2)
Geometric parameters (Å, º) top
Ni1—Br12.3390 (5)C18—C191.518 (5)
Ni1—P12.2223 (7)C18—H1811.000
Ni1—P22.1387 (8)C18—H1821.000
Ni1—C11.981 (3)C19—C201.533 (4)
Cl1—C331.719 (4)C19—H1911.000
P1—C71.838 (3)C19—H1921.000
P1—C91.848 (3)C20—H2011.000
P1—C151.850 (3)C20—H2021.000
P2—C81.851 (3)C21—C221.543 (4)
P2—C211.844 (3)C21—C261.522 (4)
P2—C271.848 (3)C21—H2111.000
C1—C21.400 (4)C22—C231.532 (4)
C1—C61.338 (4)C22—H2211.000
C2—C31.391 (4)C22—H2221.000
C2—H211.000C23—C241.514 (5)
C3—C41.372 (5)C23—H2311.000
C3—H311.000C23—H2321.000
C4—C51.381 (5)C24—C251.518 (4)
C4—H411.000C24—H2411.000
C5—C61.399 (4)C24—H2421.000
C5—H511.000C25—C261.531 (4)
C6—H611.000C25—H2511.000
C7—C81.538 (4)C25—H2521.000
C7—H711.000C26—H2611.000
C7—H721.000C26—H2621.000
C8—H811.000C27—C281.537 (4)
C8—H821.000C27—C321.532 (4)
C9—C101.531 (4)C27—H2711.000
C9—C141.539 (4)C28—C291.526 (4)
C9—H911.000C28—H2811.000
C10—C111.534 (4)C28—H2821.000
C10—H1011.000C29—C301.526 (4)
C10—H1021.000C29—H2911.000
C11—C121.525 (5)C29—H2921.000
C11—H1111.000C30—C311.524 (5)
C11—H1121.000C30—H3011.000
C12—C131.516 (5)C30—H3021.000
C12—H1211.000C31—C321.528 (4)
C12—H1221.000C31—H3111.000
C13—C141.529 (4)C31—H3121.000
C13—H1311.000C32—H3211.000
C13—H1321.000C32—H3221.000
C14—H1411.000C33—C341.393 (6)
C14—H1421.000C33—C381.367 (6)
C15—C161.533 (4)C34—C351.382 (6)
C15—C201.535 (4)C34—H3411.000
C15—H1511.000C35—C361.365 (6)
C16—C171.535 (4)C35—H3511.000
C16—H1611.000C36—C371.353 (6)
C16—H1621.000C36—H3611.000
C17—C181.517 (5)C37—C381.420 (6)
C17—H1711.000C37—H3711.000
C17—H1721.000C38—H3811.000
Br1—Ni1—P192.87 (2)C17—C18—H182109.76 (18)
Br1—Ni1—P2173.61 (3)C19—C18—H182109.28 (18)
P1—Ni1—P289.19 (3)H181—C18—H182109.467
Br1—Ni1—C189.78 (7)C18—C19—C20112.3 (3)
P1—Ni1—C1170.47 (8)C18—C19—H191109.41 (18)
P2—Ni1—C189.16 (7)C20—C19—H191109.14 (17)
Ni1—P1—C7107.89 (9)C18—C19—H192108.1 (2)
Ni1—P1—C9113.02 (9)C20—C19—H192108.40 (19)
C7—P1—C9103.90 (13)H191—C19—H192109.467
Ni1—P1—C15123.3 (1)C15—C20—C19110.9 (2)
C7—P1—C15102.94 (13)C15—C20—H201108.56 (16)
C9—P1—C15103.85 (12)C19—C20—H201109.07 (19)
Ni1—P2—C8109.45 (9)C15—C20—H202109.29 (17)
Ni1—P2—C21113.97 (9)C19—C20—H202109.55 (18)
C8—P2—C21103.53 (12)H201—C20—H202109.467
Ni1—P2—C27120.48 (9)P2—C21—C22111.44 (18)
C8—P2—C27103.03 (13)P2—C21—C26113.26 (19)
C21—P2—C27104.61 (12)C22—C21—C26110.6 (2)
Ni1—C1—C2114.0 (2)P2—C21—H211107.18 (8)
Ni1—C1—C6125.9 (2)C22—C21—H211107.86 (15)
C2—C1—C6120.0 (3)C26—C21—H211106.20 (15)
C1—C2—C3119.3 (3)C21—C22—C23110.1 (2)
C1—C2—H21120.07 (17)C21—C22—H221109.47 (15)
C3—C2—H21120.6 (2)C23—C22—H221110.13 (17)
C2—C3—C4120.8 (3)C21—C22—H222108.84 (15)
C2—C3—H31119.5 (2)C23—C22—H222108.85 (17)
C4—C3—H31119.69 (19)H221—C22—H222109.467
C3—C4—C5118.9 (3)C22—C23—C24110.7 (3)
C3—C4—H41120.31 (19)C22—C23—H231108.65 (17)
C5—C4—H41120.77 (19)C24—C23—H231108.41 (18)
C4—C5—C6120.3 (3)C22—C23—H232109.91 (17)
C4—C5—H51119.90 (19)C24—C23—H232109.72 (17)
C6—C5—H51119.8 (2)H231—C23—H232109.467
C1—C6—C5120.7 (3)C23—C24—C25112.0 (3)
C1—C6—H61119.28 (16)C23—C24—H241109.84 (16)
C5—C6—H61120.0 (2)C25—C24—H241109.44 (15)
P1—C7—C8110.43 (19)C23—C24—H242107.88 (18)
P1—C7—H71109.07 (9)C25—C24—H242108.15 (18)
C8—C7—H71109.17 (16)H241—C24—H242109.467
P1—C7—H72109.29 (9)C24—C25—C26111.6 (2)
C8—C7—H72109.39 (14)C24—C25—H251108.26 (18)
H71—C7—H72109.467C26—C25—H251108.72 (16)
P2—C8—C7111.46 (18)C24—C25—H252109.43 (17)
P2—C8—H81108.75 (9)C26—C25—H252109.36 (16)
C7—C8—H81109.06 (16)H251—C25—H252109.467
P2—C8—H82109.10 (9)C21—C26—C25110.7 (2)
C7—C8—H82108.98 (15)C21—C26—H261109.12 (15)
H81—C8—H82109.467C25—C26—H261109.53 (16)
P1—C9—C10111.44 (18)C21—C26—H262108.96 (15)
P1—C9—C14113.66 (19)C25—C26—H262109.08 (16)
C10—C9—C14110.8 (2)H261—C26—H262109.466
P1—C9—H91106.9 (1)P2—C27—C28115.0 (2)
C10—C9—H91107.86 (17)P2—C27—C32110.65 (19)
C14—C9—H91105.77 (18)C28—C27—C32111.1 (2)
C9—C10—C11111.5 (2)P2—C27—H271106.56 (9)
C9—C10—H101109.29 (16)C28—C27—H271104.02 (16)
C11—C10—H101109.58 (17)C32—C27—H271109.11 (17)
C9—C10—H102108.18 (17)C27—C28—C29110.5 (3)
C11—C10—H102108.76 (18)C27—C28—H281108.71 (16)
H101—C10—H102109.467C29—C28—H281108.84 (18)
C10—C11—C12111.6 (3)C27—C28—H282109.55 (15)
C10—C11—H111108.69 (18)C29—C28—H282109.75 (16)
C12—C11—H111108.2 (2)H281—C28—H282109.467
C10—C11—H112109.34 (17)C28—C29—C30110.9 (3)
C12—C11—H112109.45 (18)C28—C29—H291109.70 (18)
H111—C11—H112109.467C30—C29—H291109.26 (19)
C11—C12—C13111.2 (3)C28—C29—H292108.63 (18)
C11—C12—H121109.94 (17)C30—C29—H292108.8 (2)
C13—C12—H121109.81 (18)H291—C29—H292109.467
C11—C12—H122108.3 (2)C29—C30—C31110.8 (3)
C13—C12—H122108.1 (2)C29—C30—H301108.8 (2)
H121—C12—H122109.467C31—C30—H301108.3 (2)
C12—C13—C14111.7 (3)C29—C30—H302109.70 (18)
C12—C13—H131108.0 (2)C31—C30—H302109.7 (2)
C14—C13—H131108.4 (2)H301—C30—H302109.467
C12—C13—H132109.8 (2)C30—C31—C32111.0 (3)
C14—C13—H132109.45 (18)C30—C31—H311109.68 (18)
H131—C13—H132109.467C32—C31—H311110.04 (17)
C9—C14—C13110.8 (3)C30—C31—H312108.3 (2)
C9—C14—H141109.38 (16)C32—C31—H312108.3 (2)
C13—C14—H141110.01 (18)H311—C31—H312109.467
C9—C14—H142108.48 (18)C27—C32—C31111.9 (2)
C13—C14—H142108.7 (2)C27—C32—H321108.54 (17)
H141—C14—H142109.467C31—C32—H321108.3 (2)
P1—C15—C16114.22 (19)C27—C32—H322109.02 (15)
P1—C15—C20111.73 (19)C31—C32—H322109.58 (19)
C16—C15—C20110.0 (2)H321—C32—H322109.467
P1—C15—H151106.04 (9)Cl1—C33—C34120.2 (3)
C16—C15—H151105.67 (17)Cl1—C33—C38118.7 (3)
C20—C15—H151108.82 (16)C34—C33—C38121.1 (4)
C15—C16—C17110.7 (3)C33—C34—C35118.0 (4)
C15—C16—H161108.18 (17)C33—C34—H341120.2 (3)
C17—C16—H161108.2 (2)C35—C34—H341121.8 (3)
C15—C16—H162109.79 (15)C34—C35—C36120.9 (4)
C17—C16—H162110.47 (17)C34—C35—H351120.2 (3)
H161—C16—H162109.467C36—C35—H351118.9 (3)
C16—C17—C18111.4 (3)C35—C36—C37122.1 (5)
C16—C17—H171109.80 (19)C35—C36—H361119.1 (3)
C18—C17—H171110.0 (2)C37—C36—H361118.9 (3)
C16—C17—H172108.0 (2)C36—C37—C38118.1 (5)
C18—C17—H172108.2 (2)C36—C37—H371121.1 (3)
H171—C17—H172109.467C38—C37—H371120.8 (3)
C17—C18—C19111.9 (3)C33—C38—C37119.8 (4)
C17—C18—H181108.0 (2)C33—C38—H381119.2 (3)
C19—C18—H181108.4 (2)C37—C38—H381120.9 (3)

Experimental details

Crystal data
Chemical formula[NiBr(C6H5)(C26H48P2)]·C6H5Cl
Mr750.89
Crystal system, space groupMonoclinic, P21/n
Temperature (K)200
a, b, c (Å)11.8308 (1), 22.7790 (3), 14.5238 (2)
β (°) 107.4072 (5)
V3)3734.82 (8)
Z4
Radiation typeMo Kα
µ (mm1)1.77
Crystal size (mm)0.20 × 0.16 × 0.15
Data collection
DiffractometerNonius KappaCCD
diffractometer
Absorption correctionIntegration
(Coppens, 1970)
Tmin, Tmax0.662, 0.808
No. of measured, independent and
observed [I > 3σ(I)] reflections
94198, 8553, 4771
Rint0.044
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.030, 0.031, 1.05
No. of reflections4771
No. of parameters446
No. of restraints?
H-atom treatmentOnly H-atom displacement parameters refined
Δρmax, Δρmin (e Å3)0.56, 0.51

Computer programs: COLLECT (Nonius, 1997), HKL SCALEPACK (Otwinowski & Minor, 1997), DENZO and SCALEPACK (Otwinowski & Minor, 1997), SIR92 (Altomare et al., 1994), CRYSTALS (Watkin et al., 2001) and maXus (Mackay et al., 1999), CAMERON (Watkin et al., 1996), CRYSTALS and maXus.

Selected geometric parameters (Å, º) top
Ni1—Br12.3390 (5)P2—C271.848 (3)
Ni1—P12.2223 (7)C1—C21.400 (4)
Ni1—P22.1387 (8)C1—C61.338 (4)
Ni1—C11.981 (3)C2—C31.391 (4)
P1—C71.838 (3)C3—C41.372 (5)
P1—C91.848 (3)C4—C51.381 (5)
P1—C151.850 (3)C5—C61.399 (4)
P2—C81.851 (3)C7—C81.538 (4)
P2—C211.844 (3)
Br1—Ni1—P192.87 (2)Ni1—P1—C15123.3 (1)
Br1—Ni1—P2173.61 (3)Ni1—P2—C8109.45 (9)
P1—Ni1—P289.19 (3)Ni1—P2—C21113.97 (9)
Br1—Ni1—C189.78 (7)Ni1—P2—C27120.48 (9)
P1—Ni1—C1170.47 (8)Ni1—C1—C2114.0 (2)
P2—Ni1—C189.16 (7)Ni1—C1—C6125.9 (2)
Ni1—P1—C7107.89 (9)P1—C7—C8110.43 (19)
Ni1—P1—C9113.02 (9)P2—C8—C7111.46 (18)
 

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