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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 64| Part 1| January 2008| Page m239
https://doi.org/10.1107/S1600536807066949

Bis(pyridinium) trans-tetra­chlorido­dioxidouranate(VI) dioxane solvate

Izabela Pospieszna,a Wanda Radecka-Paryzeka and Maciej Kubickia*

aDepartment of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznań, Poland
*Correspondence e-mail: mkubicki@amu.edu.pl

(Received 16 November 2007; accepted 14 December 2007; online 21 December 2007)

In the crystal structure of the title compound, (C5H6N)2[UCl4O2]·C4H8O2, the pyridinium cations occupy general positions and the anions and the solvent dioxane mol­ecule are located on centres of inversion. The dioxane mol­ecules are connected to two symmetry-related pyridinium cations via O—H⋯O hydrogen bonding. There are additional inter­molecular C—H⋯Cl contacts, which are indicative of weak C—H⋯Cl inter­actions.

Related literature

For related literature, see Kaczmarek et al. (2004[Kaczmarek, M. T., Pospieszna-Markiewicz, I. & Radecka-Paryzek, W. (2004). J. Inclus. Phenom. Macrocyclic Chem. 49, 115-119.]); Pospieszna-Markiewicz & Radecka-Paryzek (2004[Pospieszna-Markiewicz, I. & Radecka-Paryzek, W. (2004). J. Alloys Compd, 374, 253-257.]); Sessler et al. (2006[Sessler, J., Melfi, P. J. & Pantos, G. D. (2006). Coord. Chem. Rev. 250, 816-843.]); Allen (2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.]).

[Scheme 1]

Experimental

Crystal data

  • (C5H6N)2[UCl4O2]·C4H8O2

  • Mr = 660.15

  • Triclinic, [P \overline 1]

  • a = 7.766 (2) Å

  • b = 8.666 (2) Å

  • c = 9.202 (2) Å

  • α = 63.57 (3)°

  • β = 67.08 (2)°

  • γ = 81.96 (2)°

  • V = 510.4 (3) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 8.49 mm−1

  • T = 100 (1) K

  • 0.2 × 0.1 × 0.1 mm
Data collection

  • Kuma KM-4-CCD four-circle diffractometer

  • Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2006[Oxford Diffraction (2006). CrysAlis CCD (Version 1.171.29.9) and CrysAlis RED (Version 1.171.29.9). Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.]) Tmin = 0.29, Tmax = 0.43

  • 3821 measured reflections

  • 1770 independent reflections

  • 1142 reflections with I > 2σ(I)

  • Rint = 0.097
Refinement

  • R[F2 > 2σ(F2)] = 0.056

  • wR(F2) = 0.090

  • S = 0.89

  • 1770 reflections

  • 115 parameters

  • 54 restraints

  • H-atom parameters constrained

  • Δρmax = 1.80 e Å−3

  • Δρmin = −2.38 e Å−3

Table 1
Selected geometric parameters (Å, °)

U1—O1 1.789 (7)
U1—Cl2 2.679 (3)
U1—Cl1 2.684 (3)
O1—U1—Cl2 91.5 (2)
O1i—U1—Cl2 88.5 (2)
Cl2i—U1—Cl2 180
O1—U1—Cl1 88.4 (2)
O1i—U1—Cl1 91.6 (2)
Cl2—U1—Cl1 89.43 (8)
Cl2—U1—Cl1i 90.57 (8)
Cl1—U1—Cl1i 180
Symmetry code: (i) -x+2, -y+2, -z.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
C6B—H6B⋯Cl1 0.95 2.87 3.525 (12) 127
C2A—H2A2⋯Cl2ii 0.99 2.88 3.754 (12) 147
N1B—H1B⋯O1Aiii 0.88 1.92 2.725 (11) 151
C4B—H4B⋯Cl1iv 0.95 2.85 3.803 (13) 177
Symmetry codes: (ii) -x+1, -y+2, -z+1; (iii) x+1, y, z; (iv) x-1, y, z+1.

Data collection: CrysAlis CCD (Oxford Diffraction, 2006[Oxford Diffraction (2006). CrysAlis CCD (Version 1.171.29.9) and CrysAlis RED (Version 1.171.29.9). Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.]); cell refinement: CrysAlis RED (Oxford Diffraction, 2006[Oxford Diffraction (2006). CrysAlis CCD (Version 1.171.29.9) and CrysAlis RED (Version 1.171.29.9). Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.]); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997[Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997[Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.]); molecular graphics: XP (Siemens, 1989[Siemens (1989). XP. Release 3.4. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.]); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536807066949/nc2081sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536807066949/nc2081Isup2.hkl

checkCIF report


Comment top

The use of uranium as a source of energy has caused increasing attention which is focused on the problem of fuel reprocessing and waste storage. Much effort has been devoted, in recent years, to the preparation and characterization of specific complexing agents for the uranyl ion (UO22+), so-called "uranophiles" with the objective of a possible application for the separation of uranium species in waste liquids from the nuclear fuel cycle and for the recovery and utilization of uranium from the sea water (Sessler et al. 2006). The title compound was isolated during our study on the synthesis and characterization of uranyl complexes containing macrocyclic and acyclic polyaza and polyoxaaza Schiff bases derived from biogenic amines and their analogs to evaluate their potential as uranyl sequestering agents (Pospieszna-Markiewicz & Radecka-Paryzek, 2004; Kaczmarek et al., 2004).

The asymmetric unit of the title compound (I) consists of one uranyl tetrachloride dianion and one dioxane molecule which are located on centres of inversion and one pyridinium cation which occupy a general position. This is quite common for similar complexes. In the Cambridge Structural Database (Allen, 2002; Version August 2007) there are 34 structures containing tetrachloro-uranyl dianions and a total of 144 structures which contain tetra-coordinated uranyl cations. Of those, 25 tetrachloro (79 for all) crystallizes with Z'<1, of which 22 (71 for all) have Z'=1/2.

In the crystal structure of the title compound the uranium atoms are coordinated by two oxygen and four chlorine atoms within slightly distorted octahedra (Fig. 1 and Tab.1). The U—O bond lengths of 1.789 (7)Å and the U—Cl bond lengths of 2.679 (3)Å and 2,684 (3)Å are close to the average CSD values (U—O = 1.77 (2)Å and U—Cl = 2.6791) Å, respectively).

Each two symmetry related pyridinium cations are connected by strong N—H···O hydrogen bonding to the dioxane molecule, forming hydrogen-bonded (pyridine···dioxane···pyridine)2+ cations (Tab. 2). These building units are connected by weak C—H···Cl interactions to the dications into a three-dimensional network (Tab. 2 and Fig. 2).

Related literature top

For related literature, see Kaczmarek et al. (2004); Pospieszna-Markiewicz & Radecka-Paryzek (2004); Sessler et al. (2006); Allen (2002).

Experimental top

The title compound was isolated during the slow diffusion of dioxane into pyridine hydrochloride solution of the uranyl(VI) Schiff base complex prepared through one-step template reaction of 2,6-diacetylpyridine with spermidine in the presence of uranyl(VI) acetateunder following conditions: to a mixture of uranyl acetate (42.5 mg, 0.1 mmol) in methanol (10 cm3) and 2,6-diacetylpyridine (16,3 mg, 0.1 mmol) in methanol (10 cm3), spermidine (0.016 cm3, 0.1 mmol) in methanol (10 cm3) was added dropwise with stirring; the reaction wascarried out for 4 h, the solution volume was then reduced to 10 cm3 by roto-evaporation and a yellow precipitate formed on addition of a small amount of diethyl ether was filtered off, washed with ether, and dried in vacuo.

Refinement top

The H atoms were positioned with idealized geometry and were refined isotropic using a riding model with Uiso(H) = 1.2. Ueq(C,N) of the parent atom. Weak restraints (ISOR) were applied to the displacement parameters of C, N and O atoms.

Structure description top

The use of uranium as a source of energy has caused increasing attention which is focused on the problem of fuel reprocessing and waste storage. Much effort has been devoted, in recent years, to the preparation and characterization of specific complexing agents for the uranyl ion (UO22+), so-called "uranophiles" with the objective of a possible application for the separation of uranium species in waste liquids from the nuclear fuel cycle and for the recovery and utilization of uranium from the sea water (Sessler et al. 2006). The title compound was isolated during our study on the synthesis and characterization of uranyl complexes containing macrocyclic and acyclic polyaza and polyoxaaza Schiff bases derived from biogenic amines and their analogs to evaluate their potential as uranyl sequestering agents (Pospieszna-Markiewicz & Radecka-Paryzek, 2004; Kaczmarek et al., 2004).

The asymmetric unit of the title compound (I) consists of one uranyl tetrachloride dianion and one dioxane molecule which are located on centres of inversion and one pyridinium cation which occupy a general position. This is quite common for similar complexes. In the Cambridge Structural Database (Allen, 2002; Version August 2007) there are 34 structures containing tetrachloro-uranyl dianions and a total of 144 structures which contain tetra-coordinated uranyl cations. Of those, 25 tetrachloro (79 for all) crystallizes with Z'<1, of which 22 (71 for all) have Z'=1/2.

In the crystal structure of the title compound the uranium atoms are coordinated by two oxygen and four chlorine atoms within slightly distorted octahedra (Fig. 1 and Tab.1). The U—O bond lengths of 1.789 (7)Å and the U—Cl bond lengths of 2.679 (3)Å and 2,684 (3)Å are close to the average CSD values (U—O = 1.77 (2)Å and U—Cl = 2.6791) Å, respectively).

Each two symmetry related pyridinium cations are connected by strong N—H···O hydrogen bonding to the dioxane molecule, forming hydrogen-bonded (pyridine···dioxane···pyridine)2+ cations (Tab. 2). These building units are connected by weak C—H···Cl interactions to the dications into a three-dimensional network (Tab. 2 and Fig. 2).

For related literature, see Kaczmarek et al. (2004); Pospieszna-Markiewicz & Radecka-Paryzek (2004); Sessler et al. (2006); Allen (2002).

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis RED (Oxford Diffraction, 2006); data reduction: CrysAlis RED (Oxford Diffraction, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1989); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1] Fig. 1. Crystal structure of the title compound with labeling and displacement ellipsoids drawn at the 50% propability level, H atoms are drawn as spheres with arbitrary radii. Symmetry codes: (i) 2 - x,2 - y,-z, (ii) 1 - x,1 - y,1 - z.
[Figure 2] Fig. 2. Crystal structure of (I) with view along the a axis. O—H···O hydrogen bonding and C—H···Cl interactions are shown as dashed lines.
bis(pyridinium) uranyl tetrachloridodioxidouranium(VI) dioxane solvate] top
Crystal data top
(C5H6N)2[UCl4O2]·C4H8O2Z = 1
Mr = 660.15F(000) = 310
Triclinic, P1Dx = 2.148 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.766 (2) ÅCell parameters from 2368 reflections
b = 8.666 (2) Åθ = 4–25°
c = 9.202 (2) ŵ = 8.50 mm−1
α = 63.57 (3)°T = 100 K
β = 67.08 (2)°Block, colourless
γ = 81.96 (2)°0.2 × 0.1 × 0.1 mm
V = 510.4 (3) Å3
Data collection top
Kuma KM-4-CCD four-circle
diffractometer		1770 independent reflections
Radiation source: fine-focus sealed tube1142 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.097
ω scansθmax = 25.0°, θmin = 2.6°
Absorption correction: multi-scan
(CrysAlis RED; Oxford Diffraction, 2006)		h = −9→8
Tmin = 0.29, Tmax = 0.43k = −10→9
3821 measured reflectionsl = −10→5
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.056Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.090H-atom parameters constrained
S = 0.89 w = 1/[σ2(Fo2) + (0.02P)2]
where P = (Fo2 + 2Fc2)/3
1770 reflections(Δ/σ)max < 0.001
115 parametersΔρmax = 1.80 e Å−3
54 restraintsΔρmin = −2.38 e Å−3
Crystal data top
(C5H6N)2[UCl4O2]·C4H8O2γ = 81.96 (2)°
Mr = 660.15V = 510.4 (3) Å3
Triclinic, P1Z = 1
a = 7.766 (2) ÅMo Kα radiation
b = 8.666 (2) ŵ = 8.50 mm−1
c = 9.202 (2) ÅT = 100 K
α = 63.57 (3)°0.2 × 0.1 × 0.1 mm
β = 67.08 (2)°
Data collection top
Kuma KM-4-CCD four-circle
diffractometer		1770 independent reflections
Absorption correction: multi-scan
(CrysAlis RED; Oxford Diffraction, 2006)		1142 reflections with I > 2σ(I)
Tmin = 0.29, Tmax = 0.43Rint = 0.097
3821 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.05654 restraints
wR(F2) = 0.090H-atom parameters constrained
S = 0.89Δρmax = 1.80 e Å−3
1770 reflectionsΔρmin = −2.38 e Å−3
115 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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
U11.00001.00000.00000.0190 (3)
O10.8449 (10)0.8196 (8)0.0864 (8)0.0147 (18)
Cl11.1731 (4)0.8012 (3)0.2188 (3)0.0233 (9)
Cl20.7746 (4)1.1044 (3)0.2426 (3)0.0220 (9)
O1A0.3181 (10)0.5610 (8)0.5613 (8)0.013 (2)
C2A0.4823 (16)0.6717 (13)0.4704 (13)0.017 (3)
H2A20.46320.76240.51220.022*
H2A10.50580.72870.34390.022*
C3A0.6456 (17)0.5718 (14)0.4994 (13)0.018 (3)
H3A20.75730.65080.43750.023*
H3A10.62300.51830.62560.023*
N1B0.9618 (13)0.6611 (10)0.6810 (10)0.016 (2)
H1B1.06810.64350.60870.019*
C2B0.9005 (17)0.5495 (14)0.8497 (13)0.022 (3)
H2B0.97330.45480.89230.027*
C3B0.7294 (17)0.5742 (14)0.9614 (13)0.020 (3)
H3B0.68100.49111.07960.024*
C4B0.6257 (18)0.7202 (14)0.9030 (13)0.023 (3)
H4B0.51070.74120.97920.028*
C5B0.7038 (17)0.8332 (14)0.7241 (12)0.018 (3)
H5B0.64090.93470.67770.022*
C6B0.8639 (17)0.8001 (14)0.6192 (14)0.021 (3)
H6B0.91030.87590.49830.026*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
U10.0264 (6)0.0098 (4)0.0142 (4)0.0037 (4)−0.0084 (3)0.0003 (3)
O10.015 (2)0.015 (2)0.015 (2)0.0000 (10)−0.0054 (11)−0.0072 (11)
Cl10.031 (2)0.0219 (17)0.0137 (15)0.0129 (17)−0.0104 (16)−0.0067 (13)
Cl20.026 (2)0.0193 (17)0.0173 (15)0.0095 (16)−0.0073 (15)−0.0077 (13)
O1A0.005 (5)0.014 (4)0.020 (4)0.001 (4)−0.004 (4)−0.008 (3)
C2A0.017 (3)0.017 (3)0.017 (3)0.0005 (10)−0.0060 (14)−0.0072 (15)
C3A0.018 (3)0.018 (3)0.018 (3)0.0004 (10)−0.0066 (14)−0.0075 (15)
N1B0.016 (2)0.016 (2)0.016 (2)0.0006 (10)−0.0053 (13)−0.0073 (13)
C2B0.022 (3)0.022 (3)0.022 (3)0.0011 (10)−0.0083 (15)−0.0093 (15)
C3B0.020 (3)0.020 (3)0.020 (3)0.0009 (10)−0.0076 (14)−0.0082 (15)
C4B0.023 (3)0.023 (3)0.023 (3)0.0006 (10)−0.0086 (15)−0.0100 (16)
C5B0.018 (3)0.018 (3)0.018 (3)0.0008 (10)−0.0067 (14)−0.0078 (15)
C6B0.021 (3)0.021 (3)0.021 (3)0.0007 (10)−0.0081 (14)−0.0088 (15)
Geometric parameters (Å, º) top
U1—O11.789 (7)C3A—H3A10.9900
U1—O1i1.789 (7)N1B—C2B1.337 (11)
U1—Cl2i2.679 (3)N1B—C6B1.350 (12)
U1—Cl22.679 (3)N1B—H1B0.8800
U1—Cl12.684 (3)C2B—C3B1.386 (15)
U1—Cl1i2.684 (3)C2B—H2B0.9500
O1A—C2A1.430 (13)C3B—C4B1.409 (13)
O1A—C3Aii1.440 (12)C3B—H3B0.9500
C2A—C3A1.477 (13)C4B—C5B1.411 (12)
C2A—H2A20.9900C4B—H4B0.9500
C2A—H2A10.9900C5B—C6B1.331 (14)
C3A—O1Aii1.440 (12)C5B—H5B0.9500
C3A—H3A20.9900C6B—H6B0.9500
O1—U1—O1i180.000 (1)O1Aii—C3A—H3A2109.2
O1—U1—Cl2i88.5 (2)C2A—C3A—H3A2109.2
O1i—U1—Cl2i91.5 (2)O1Aii—C3A—H3A1109.2
O1—U1—Cl291.5 (2)C2A—C3A—H3A1109.2
O1i—U1—Cl288.5 (2)H3A2—C3A—H3A1107.9
Cl2i—U1—Cl2180.000 (1)C2B—N1B—C6B121.4 (10)
O1—U1—Cl188.4 (2)C2B—N1B—H1B119.3
O1i—U1—Cl191.6 (2)C6B—N1B—H1B119.3
Cl2i—U1—Cl190.57 (8)N1B—C2B—C3B119.0 (10)
Cl2—U1—Cl189.43 (8)N1B—C2B—H2B120.5
O1—U1—Cl1i91.6 (2)C3B—C2B—H2B120.5
O1i—U1—Cl1i88.4 (2)C2B—C3B—C4B121.2 (10)
Cl2i—U1—Cl1i89.43 (8)C2B—C3B—H3B119.4
Cl2—U1—Cl1i90.57 (8)C4B—C3B—H3B119.4
Cl1—U1—Cl1i180.000 (1)C3B—C4B—C5B115.7 (11)
C2A—O1A—C3Aii107.7 (8)C3B—C4B—H4B122.2
O1A—C2A—C3A110.4 (8)C5B—C4B—H4B122.2
O1A—C2A—H2A2109.6C6B—C5B—C4B121.2 (10)
C3A—C2A—H2A2109.6C6B—C5B—H5B119.4
O1A—C2A—H2A1109.6C4B—C5B—H5B119.4
C3A—C2A—H2A1109.6C5B—C6B—N1B121.4 (10)
H2A2—C2A—H2A1108.1C5B—C6B—H6B119.3
O1Aii—C3A—C2A112.1 (10)N1B—C6B—H6B119.3
Symmetry codes: (i) −x+2, −y+2, −z; (ii) −x+1, −y+1, −z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C6B—H6B···Cl10.952.873.525 (12)127
C2A—H2A2···Cl2iii0.992.883.754 (12)147
N1B—H1B···O1Aiv0.881.922.725 (11)151
C4B—H4B···Cl1v0.952.853.803 (13)177
Symmetry codes: (iii) −x+1, −y+2, −z+1; (iv) x+1, y, z; (v) x−1, y, z+1.

Experimental details

Crystal data
Chemical formula(C5H6N)2[UCl4O2]·C4H8O2
Mr660.15
Crystal system, space groupTriclinic, P1
Temperature (K)100
a, b, c (Å)7.766 (2), 8.666 (2), 9.202 (2)
α, β, γ (°)63.57 (3), 67.08 (2), 81.96 (2)
V (Å3)510.4 (3)
Z1
Radiation typeMo Kα
µ (mm−1)8.50
Crystal size (mm)0.2 × 0.1 × 0.1
Data collection
DiffractometerKuma KM-4-CCD four-circle
Absorption correctionMulti-scan
(CrysAlis RED; Oxford Diffraction, 2006)
Tmin, Tmax0.29, 0.43
No. of measured, independent and
observed [I > 2σ(I)] reflections		3821, 1770, 1142
Rint0.097
(sin θ/λ)max (Å−1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.056, 0.090, 0.89
No. of reflections1770
No. of parameters115
No. of restraints54
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)1.80, −2.38

Computer programs: CrysAlis CCD (Oxford Diffraction, 2006), CrysAlis RED (Oxford Diffraction, 2006), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), XP (Siemens, 1989).

Selected geometric parameters (Å, º) top
U1—O11.789 (7)U1—Cl12.684 (3)
U1—Cl22.679 (3)
O1—U1—Cl291.5 (2)O1i—U1—Cl191.6 (2)
O1i—U1—Cl288.5 (2)Cl2—U1—Cl189.43 (8)
Cl2i—U1—Cl2180.000 (1)Cl2—U1—Cl1i90.57 (8)
O1—U1—Cl188.4 (2)Cl1—U1—Cl1i180.000 (1)
Symmetry code: (i) −x+2, −y+2, −z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C6B—H6B···Cl10.952.873.525 (12)127.3
C2A—H2A2···Cl2ii0.992.883.754 (12)147.3
N1B—H1B···O1Aiii0.881.922.725 (11)150.7
C4B—H4B···Cl1iv0.952.853.803 (13)177.4
Symmetry codes: (ii) −x+1, −y+2, −z+1; (iii) x+1, y, z; (iv) x−1, y, z+1.
 

Acknowledgements

This work was supported by the Ministry of Science and Higher Education (grant No. N204 0317 33).

References

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ISSN: 2056-9890
Volume 64| Part 1| January 2008| Page m239
https://doi.org/10.1107/S1600536807066949
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