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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 71| Part 4| April 2015| Pages m83-m84
doi:10.1107/S2056989015004351

Crystal structure of trans-dihydrido­bis­[tris­­(di­methyl­amino)­phosphane-κP]platinum(II)

CROSSMARK_Color_square_no_text.svg
Emma L. Downs,a Lev N. Zakharova and David R. Tylera*

aDepartment of Chemistry and Biochemistry, 1253 University of Oregon, Eugene, Oregon 97403-1253, USA
*Correspondence e-mail: dtyler@uoregon.edu

Edited by S. Parkin, University of Kentucky, USA (Received 3 February 2015; accepted 2 March 2015; online 14 March 2015)

The mol­ecule of the title compound, [PtH2(C6H18N3P)2], has a centrosymmetric square-planar structure in which the PtII atom is bonded to two H and two P atoms in a mutually trans configuration. The PtII atom sits on an inversion center and thus the asymmetric unit contains only half the mol­ecule. The Pt—P and Pt—H distances are 2.2574 (10) and 1.49 (7) Å, respectively.

CCDC reference: 1051841

Similar articles

1. Related literature

For the synthesis of related compounds, see: Packett et al. (1985[Packett, D. L., Jensen, C. M., Cowan, R. L., Strouse, C. E. & Trogler, W. C. (1985). Inorg. Chem. 24, 3578-3583.]). For information on ligand-assisted hydration, see: Grotjahn (2005[Grotjahn, D. B. (2005). Chem. Eur. J. 11, 7146-7153.]); Grotjahn et al. (2008a[Grotjahn, D. B., Kragulj, E. J., Zeinalipour-Yazdi, C. D., Miranda-Soto, V., Lev, D. A. & Cooksy, A. L. (2008a). J. Am. Chem. Soc. 130, 10860-10861.],b[Grotjahn, D. B., Miranda-Soto, V., Kragulj, E. J., Lev, D. A., Erdogan, G., Zeng, X. & Cooksy, A. L. (2008b). J. Am. Chem. Soc. 130, 20-21.]). For further information on nitrile hydration, see: García-Álvarez et al. (2011[García-Álvarez, R., Díez, J., Crochet, P. & Cadierno, V. (2011). Organometallics, 30, 5442-5451.]); Knapp et al. (2012[Knapp, S. M. M., Sherbow, T. J., Juliette, J. J. & Tyler, D. R. (2012). Organometallics, 31, 2941-2944.], 2013a[Knapp, S. M. M., Sherbow, T. J., Yelle, R. B., Juliette, J. J. & Tyler, D. R. (2013a). Organometallics, 32, 3744-3752.],b[Knapp, S. M. M., Sherbow, T. J., Yelle, R. B., Zakharov, L. N., Juliette, J. J. & Tyler, D. R. (2013b). Organometallics, 32, 824-834.]). For a review of the literature on nitrile hydration, see: Ahmed et al. (2011[Ahmed, T. J., Knapp, S. M. M. & Tyler, D. R. (2011). Coord. Chem. Rev. 255, 949-974.]). For related structures, see: Packett et al. (1985[Packett, D. L., Jensen, C. M., Cowan, R. L., Strouse, C. E. & Trogler, W. C. (1985). Inorg. Chem. 24, 3578-3583.]); Robertson et al. (1986[Robertson, G. B., Tucker, P. A. & Wickramasinghe, W. A. (1986). Aust. J. Chem. 39, 1495-1507.]); Ferguson et al. (1979[Ferguson, G., Siew, P. Y. & Goel, A. B. (1979). J. Chem. Res. Synop. pp. 362-363.]).

[Scheme 1]

2. Experimental

2.1. Crystal data

  • [PtH2(C6H18N3P)2]

  • Mr = 523.51

  • Triclinic, [P \overline 1]

  • a = 7.8871 (19) Å

  • b = 7.9499 (19) Å

  • c = 9.891 (2) Å

  • α = 76.807 (4)°

  • β = 73.241 (4)°

  • γ = 60.652 (3)°

  • V = 514.8 (2) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 6.97 mm−1

  • T = 173 K

  • 0.08 × 0.06 × 0.03 mm

2.2. Data collection

  • Bruker APEXII CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1995[Sheldrick, G. M. (1995). SADABS. University of Göttingen, Germany.]) Tmin = 0.856, Tmax = 1.000

  • 5813 measured reflections

  • 2238 independent reflections

  • 2238 reflections with I > 2σ(I)

  • Rint = 0.020

2.3. Refinement

  • R[F2 > 2σ(F2)] = 0.023

  • wR(F2) = 0.059

  • S = 1.04

  • 2238 reflections

  • 101 parameters

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 0.65 e Å−3

  • Δρmin = −0.69 e Å−3

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2000[Bruker (2000). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supporting information

CCDC reference: 1051841

Crystal structure: contains datablock I. DOI: 10.1107/S2056989015004351/pk2545sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S2056989015004351/pk2545Isup2.hkl

checkCIF report


Comment top

The hydration of nitriles using homogeneous catalysts is often too slow for practical applications (Ahmed et al., 2011). Hydroxide is a much better nucleophile than water, and thus to increase the rate, many hydration reactions are carried out at high pH. When a ligand on the catalyst is capable of hydrogen bonding, the entering water nucleophile can be activated by hydrogen bonding interactions, avoiding the need for strongly basic solutions. Large rate accelerations in hydration reactions have been observed and attributed to this phenomenon, known as ligand assisted hydration or bifunctional catalysis (Grotjahn, 2005; Grotjahn et al., 2008a,b). Complexes with phosphane ligands containing hydrogen bonding moieties, in particular tris(dimethylamino)phosphane (P(NMe2)3), have achieved excellent results in nitrile hydration reactions (García-Álvarez et al., 2011; Knapp et al., 2012, 2013a,b). In particular, we reported that the [RuCl2(η6-p-cymene){P(NMe2)3}] complex is an excellent nitrile hydration catalyst (Knapp et al., 2012). Unlike related catalysts, this complex was active under acidic conditions (pH 3.5), and the improved stability of cyanohydrins in an acidic medium yielded excellent results. Glycolonitrile (1) and lactonitrile (2) were hydrated fully to their corresponding amides and acetone cyanohydrin (3) was converted to 3-hydroxy-isobutyro nitrile (HIBAM) in 15% yield. Based on this result, we hypothesized that the tris(dimethylamino)phosphane ligand could be used in other homogeneous catalysts to enhance the rates of hydration. For this purpose, two new platinum complexes, Pt(H)(Cl)(P(NMe2)3)2 and Pt(H)2(P(NMe2)3)2, were synthesized and tested for hydration activity with a variety of nitriles, including aromatic and aliphatic nitriles and cyanohydrins.

Pt(H)2(P(NMe2)3)2 was characterized by single-crystal X-ray diffraction methods. The molecule has a square planar structure (P(1)(1 - x,2 - y,1 - z)-Pt(1) (x,y,z) –P(1)(x,y,z) = 180.0 °). The Pt—P bond lengths (2.2572 (8) Å) are comparable to other Pt(H)2(phosphane)2 complexes: Pt(H)2(PMe3)2, 2.259 (3) Å; Pt(PiPr3)2(H)2, 2.252 (1) Å; Pt(H)2(PtBu3)2, 2.276 (3) Å. (Packett et al., 1985; Robertson et al., 1986; Ferguson et al., 1979). The P atom coordination environments are slightly distorted tetrahedral: N(3)—P(1)—N(1) = 110.86 (15)°; N(3)—P(1)—N(2) = 100.94 (14)°; N(1)—P(1)—N(2) = 98.70 (13)°; N(3)—P(1)—Pt(1) = 112.12 (10)°; N(1)—P(1)—Pt(1) = 113.82 (9)°; N(2)—P(1)—Pt(1) = 119.08 (9)°). The three NMe2 groups bonded to each P atom have a staggered orientation with respect to the three NMe2 groups on the other P atom. Consequently, the two Pt—P—N(2) angles, with atoms in the same plane as the Pt—H bonds, are significantly distorted (119.08 (9)°) from the tetrahedral angle.

Related literature top

For the synthesis of related compounds, see: Packett et al. (1985). For information on ligand-assisted hydration, see: Grotjahn (2005); Grotjahn et al. (2008a,b). For further information on nitrile hydration, see: García-Álvarez et al. (2011); Knapp et al. (2012, 2013a,b). For a review of the literature on nitrile hydration, see: Ahmed et al. (2011). For related structures, see: Packett et al. (1985); Robertson et al. (1986); Ferguson et al. (1979).

Experimental top

Synthesis of Pt(H)2(P(NMe2)3)2. In an inert atmosphere, PtCl2(COD) (0.1 g, 0.27 mmol) was dissolved in 10 ml dichloromethane. Two equivalents of P(NMe2)3 (0.1 ml, 0.54 mmol) were added dropwise with stirring. The solution turned from colorless to light yellow. The solution was stirred overnight. 31P NMR confirmed the formation of cis-PtCl2(P(NMe2)3)2: the free phosphane peak at 122 p.p.m. had disappeared and a peak with platinum satellites at 60 p.p.m. had appeared. The solvent and COD were removed in vacuo and the resulting light yellow powder was redissolved in acetonitrile. Two equivalents (0.02 g, 0.54 mmol) of NaBH4 were added with stirring. The solution was stirred for two hours and became bright orange; solids began to precipitate. The mixture was filtered through a celite plug to remove solids, and the solvent was removed. The brown solid was redissolved in minimal acetone and layered on top of water to precipitate brown crystals. 31P NMR: 129 p.p.m., Pt satellites at 138, 120 p.p.m.. JPt—P = 1,891 Hz. 1H NMR: t, 2.8 p.p.m. (JP—H = 5.5 Hz), tt, -3.5 (JP—H = 17.5 Hz, JPt—H = 405 Hz).

Refinement top

The structure was solved using direct methods and refined with anisotropic thermal parameters for non-H atoms. The H atom bonded to the Pt atom was found in the residual density and refined with isotropic thermal parameters. H atoms in the Me groups were positioned geometrically and refined using a rigid group model: C—H = 0.98 Å, Uiso(H) = 1.5Ueq(C).

Structure description top

The hydration of nitriles using homogeneous catalysts is often too slow for practical applications (Ahmed et al., 2011). Hydroxide is a much better nucleophile than water, and thus to increase the rate, many hydration reactions are carried out at high pH. When a ligand on the catalyst is capable of hydrogen bonding, the entering water nucleophile can be activated by hydrogen bonding interactions, avoiding the need for strongly basic solutions. Large rate accelerations in hydration reactions have been observed and attributed to this phenomenon, known as ligand assisted hydration or bifunctional catalysis (Grotjahn, 2005; Grotjahn et al., 2008a,b). Complexes with phosphane ligands containing hydrogen bonding moieties, in particular tris(dimethylamino)phosphane (P(NMe2)3), have achieved excellent results in nitrile hydration reactions (García-Álvarez et al., 2011; Knapp et al., 2012, 2013a,b). In particular, we reported that the [RuCl2(η6-p-cymene){P(NMe2)3}] complex is an excellent nitrile hydration catalyst (Knapp et al., 2012). Unlike related catalysts, this complex was active under acidic conditions (pH 3.5), and the improved stability of cyanohydrins in an acidic medium yielded excellent results. Glycolonitrile (1) and lactonitrile (2) were hydrated fully to their corresponding amides and acetone cyanohydrin (3) was converted to 3-hydroxy-isobutyro nitrile (HIBAM) in 15% yield. Based on this result, we hypothesized that the tris(dimethylamino)phosphane ligand could be used in other homogeneous catalysts to enhance the rates of hydration. For this purpose, two new platinum complexes, Pt(H)(Cl)(P(NMe2)3)2 and Pt(H)2(P(NMe2)3)2, were synthesized and tested for hydration activity with a variety of nitriles, including aromatic and aliphatic nitriles and cyanohydrins.

Pt(H)2(P(NMe2)3)2 was characterized by single-crystal X-ray diffraction methods. The molecule has a square planar structure (P(1)(1 - x,2 - y,1 - z)-Pt(1) (x,y,z) –P(1)(x,y,z) = 180.0 °). The Pt—P bond lengths (2.2572 (8) Å) are comparable to other Pt(H)2(phosphane)2 complexes: Pt(H)2(PMe3)2, 2.259 (3) Å; Pt(PiPr3)2(H)2, 2.252 (1) Å; Pt(H)2(PtBu3)2, 2.276 (3) Å. (Packett et al., 1985; Robertson et al., 1986; Ferguson et al., 1979). The P atom coordination environments are slightly distorted tetrahedral: N(3)—P(1)—N(1) = 110.86 (15)°; N(3)—P(1)—N(2) = 100.94 (14)°; N(1)—P(1)—N(2) = 98.70 (13)°; N(3)—P(1)—Pt(1) = 112.12 (10)°; N(1)—P(1)—Pt(1) = 113.82 (9)°; N(2)—P(1)—Pt(1) = 119.08 (9)°). The three NMe2 groups bonded to each P atom have a staggered orientation with respect to the three NMe2 groups on the other P atom. Consequently, the two Pt—P—N(2) angles, with atoms in the same plane as the Pt—H bonds, are significantly distorted (119.08 (9)°) from the tetrahedral angle.

For the synthesis of related compounds, see: Packett et al. (1985). For information on ligand-assisted hydration, see: Grotjahn (2005); Grotjahn et al. (2008a,b). For further information on nitrile hydration, see: García-Álvarez et al. (2011); Knapp et al. (2012, 2013a,b). For a review of the literature on nitrile hydration, see: Ahmed et al. (2011). For related structures, see: Packett et al. (1985); Robertson et al. (1986); Ferguson et al. (1979).

Computing details top

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The crystal structure of trans-dihydridobis[tris(dimethylamino)phosphane]platinum (II) with 50% probability displacement ellipsoids. H atoms in the Me groups are omitted for clarity. [Symmetry code (A): 1 - x, 2 - y, 1 - z].
trans-Dihydridobis[tris(dimethylamino)phosphane-κP]platinum(II) top
Crystal data top
[PtH2(C6H18N3P)2]Z = 1
Mr = 523.51F(000) = 260
Triclinic, P1Dx = 1.689 Mg m−3
a = 7.8871 (19) ÅMo Kα radiation, λ = 0.71073 Å
b = 7.9499 (19) ÅCell parameters from 3285 reflections
c = 9.891 (2) Åθ = 3.0–26.9°
α = 76.807 (4)°µ = 6.97 mm−1
β = 73.241 (4)°T = 173 K
γ = 60.652 (3)°Block, colorless
V = 514.8 (2) Å30.08 × 0.06 × 0.03 mm
Data collection top
Bruker APEXII CCD area-detector
diffractometer		2238 reflections with I > 2σ(I)
Radiation source: Sealed tube with triumph monochromatorRint = 0.020
φ and ω scansθmax = 27.0°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1995)		h = −10→10
Tmin = 0.856, Tmax = 1.000k = −10→10
5813 measured reflectionsl = −12→12
2238 independent reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.023H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.059 w = 1/[σ2(Fo2) + (0.0425P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max < 0.001
2238 reflectionsΔρmax = 0.65 e Å−3
101 parametersΔρmin = −0.69 e Å−3
Crystal data top
[PtH2(C6H18N3P)2]γ = 60.652 (3)°
Mr = 523.51V = 514.8 (2) Å3
Triclinic, P1Z = 1
a = 7.8871 (19) ÅMo Kα radiation
b = 7.9499 (19) ŵ = 6.97 mm−1
c = 9.891 (2) ÅT = 173 K
α = 76.807 (4)°0.08 × 0.06 × 0.03 mm
β = 73.241 (4)°
Data collection top
Bruker APEXII CCD area-detector
diffractometer		2238 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1995)		2238 reflections with I > 2σ(I)
Tmin = 0.856, Tmax = 1.000Rint = 0.020
5813 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0230 restraints
wR(F2) = 0.059H atoms treated by a mixture of independent and constrained refinement
S = 1.04Δρmax = 0.65 e Å−3
2238 reflectionsΔρmin = −0.69 e Å−3
101 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pt10.50001.00000.50000.02501 (8)
P10.58089 (14)0.80751 (13)0.70124 (10)0.02302 (18)
N10.8017 (5)0.7594 (5)0.7244 (4)0.0332 (7)
N20.6130 (5)0.5757 (4)0.7200 (3)0.0272 (6)
N30.4051 (6)0.8932 (5)0.8436 (4)0.0405 (9)
C10.8862 (7)0.8928 (6)0.6632 (5)0.0372 (9)
H1A1.01600.84040.68800.056*
H1B0.79711.01850.70070.056*
H1C0.90280.90960.55970.056*
C20.9106 (7)0.6069 (7)0.8243 (5)0.0433 (11)
H2A1.03620.60850.81770.065*
H2B0.93820.48080.80190.065*
H2C0.83080.62840.92090.065*
C30.7765 (7)0.4524 (6)0.6164 (5)0.0400 (10)
H3A0.78490.32240.63470.060*
H3B0.90160.44380.62440.060*
H3C0.75290.50830.52050.060*
C40.4314 (7)0.5651 (7)0.7249 (5)0.0433 (11)
H4A0.45920.42880.73600.065*
H4B0.38440.62980.63660.065*
H4C0.32890.62950.80550.065*
C50.2224 (7)1.0666 (8)0.8357 (6)0.0543 (14)
H5B0.14011.09080.93140.081*
H5C0.15091.05120.77690.081*
H5D0.25111.17640.79350.081*
C60.4176 (8)0.7934 (7)0.9864 (5)0.0488 (12)
H6C0.29830.86921.05390.073*
H6D0.53560.77891.01190.073*
H6A0.42740.66490.98920.073*
H10.490 (10)1.163 (10)0.557 (7)0.070 (19)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.03283 (12)0.02060 (11)0.02016 (11)−0.01088 (8)−0.01106 (8)0.00457 (7)
P10.0288 (4)0.0194 (4)0.0196 (4)−0.0097 (4)−0.0092 (3)0.0027 (3)
N10.0396 (18)0.0315 (17)0.0374 (19)−0.0219 (15)−0.0225 (15)0.0127 (14)
N20.0358 (17)0.0198 (15)0.0279 (16)−0.0138 (13)−0.0115 (13)0.0031 (12)
N30.043 (2)0.0329 (19)0.0202 (16)−0.0017 (16)−0.0033 (14)0.0009 (14)
C10.037 (2)0.034 (2)0.047 (2)−0.0233 (18)−0.0090 (18)0.0020 (18)
C20.047 (3)0.042 (2)0.048 (3)−0.024 (2)−0.030 (2)0.017 (2)
C30.050 (3)0.024 (2)0.039 (2)−0.0111 (18)−0.0111 (19)−0.0037 (17)
C40.052 (3)0.050 (3)0.042 (2)−0.035 (2)−0.023 (2)0.014 (2)
C50.040 (2)0.047 (3)0.041 (3)0.003 (2)−0.003 (2)−0.001 (2)
C60.054 (3)0.043 (3)0.024 (2)−0.008 (2)−0.0055 (19)0.0046 (18)
Geometric parameters (Å, º) top
Pt1—P12.2574 (10)C2—H2A0.9800
Pt1—P1i2.2574 (10)C2—H2B0.9800
Pt1—H11.49 (7)C2—H2C0.9800
P1—N31.660 (4)C3—H3A0.9800
P1—N11.664 (3)C3—H3B0.9800
P1—N21.705 (3)C3—H3C0.9800
N1—C11.450 (5)C4—H4A0.9800
N1—C21.451 (5)C4—H4B0.9800
N2—C31.460 (5)C4—H4C0.9800
N2—C41.462 (5)C5—H5B0.9800
N3—C51.432 (6)C5—H5C0.9800
N3—C61.458 (6)C5—H5D0.9800
C1—H1A0.9800C6—H6C0.9800
C1—H1B0.9800C6—H6D0.9800
C1—H1C0.9800C6—H6A0.9800
P1—Pt1—P1i180.0N1—C2—H2C109.5
P1—Pt1—H190 (3)H2A—C2—H2C109.5
P1i—Pt1—H190 (3)H2B—C2—H2C109.5
N3—P1—N1110.9 (2)N2—C3—H3A109.5
N3—P1—N2101.05 (19)N2—C3—H3B109.5
N1—P1—N298.82 (17)H3A—C3—H3B109.5
N3—P1—Pt1112.10 (13)N2—C3—H3C109.5
N1—P1—Pt1113.77 (12)H3A—C3—H3C109.5
N2—P1—Pt1118.93 (12)H3B—C3—H3C109.5
C1—N1—C2112.8 (3)N2—C4—H4A109.5
C1—N1—P1121.1 (3)N2—C4—H4B109.5
C2—N1—P1125.2 (3)H4A—C4—H4B109.5
C3—N2—C4110.0 (4)N2—C4—H4C109.5
C3—N2—P1114.7 (3)H4A—C4—H4C109.5
C4—N2—P1113.4 (3)H4B—C4—H4C109.5
C5—N3—C6114.0 (4)N3—C5—H5B109.5
C5—N3—P1122.7 (3)N3—C5—H5C109.5
C6—N3—P1123.1 (3)H5B—C5—H5C109.5
N1—C1—H1A109.5N3—C5—H5D109.5
N1—C1—H1B109.5H5B—C5—H5D109.5
H1A—C1—H1B109.5H5C—C5—H5D109.5
N1—C1—H1C109.5N3—C6—H6C109.5
H1A—C1—H1C109.5N3—C6—H6D109.5
H1B—C1—H1C109.5H6C—C6—H6D109.5
N1—C2—H2A109.5N3—C6—H6A109.5
N1—C2—H2B109.5H6C—C6—H6A109.5
H2A—C2—H2B109.5H6D—C6—H6A109.5
N3—P1—N1—C1−100.5 (4)N3—P1—N2—C458.6 (3)
N2—P1—N1—C1154.0 (3)N1—P1—N2—C4172.0 (3)
Pt1—P1—N1—C126.9 (4)Pt1—P1—N2—C4−64.5 (3)
N3—P1—N1—C267.7 (4)N1—P1—N3—C5130.0 (4)
N2—P1—N1—C2−37.8 (4)N2—P1—N3—C5−126.0 (5)
Pt1—P1—N1—C2−164.9 (3)Pt1—P1—N3—C51.7 (5)
N3—P1—N2—C3−174.0 (3)N1—P1—N3—C6−53.6 (5)
N1—P1—N2—C3−60.5 (3)N2—P1—N3—C650.4 (5)
Pt1—P1—N2—C362.9 (3)Pt1—P1—N3—C6178.1 (4)
Symmetry code: (i) −x+1, −y+2, −z+1.

Experimental details

Crystal data
Chemical formula[PtH2(C6H18N3P)2]
Mr523.51
Crystal system, space groupTriclinic, P1
Temperature (K)173
a, b, c (Å)7.8871 (19), 7.9499 (19), 9.891 (2)
α, β, γ (°)76.807 (4), 73.241 (4), 60.652 (3)
V (Å3)514.8 (2)
Z1
Radiation typeMo Kα
µ (mm−1)6.97
Crystal size (mm)0.08 × 0.06 × 0.03
Data collection
DiffractometerBruker APEXII CCD area-detector
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1995)
Tmin, Tmax0.856, 1.000
No. of measured, independent and
observed [I > 2σ(I)] reflections		5813, 2238, 2238
Rint0.020
(sin θ/λ)max (Å−1)0.639
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.023, 0.059, 1.04
No. of reflections2238
No. of parameters101
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3)0.65, −0.69

Computer programs: APEX2 (Bruker, 2008), SAINT (Bruker, 2000), SHELXTL (Sheldrick, 2008).

 

Acknowledgements

Acknowledgment is made to the National Science Foundation (CHE 1360347) for the support of this research.

References

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This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

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ISSN: 2056-9890
Volume 71| Part 4| April 2015| Pages m83-m84
doi:10.1107/S2056989015004351
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