Crystal structure of tetra­guanidinium [hexa­hydrogen hexa­arsenato(V)tetra­vanadate(V)] tetra­hydrate

Harrison, W.T.A.

doi:10.1107/S1600536814011349

metal-organic compounds

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ISSN: 2056-9890

Volume 70| Part 9| September 2014| Pages m305-m306

doi:10.1107/S1600536814011349

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Crystal structure of tetraguanidinium [hexahydrogen hexaarsenato(V)tetravanadate(V)] tetrahydrate

William T. A. Harrison ^a ^*

^aDepartment of Chemistry, University of Aberdeen, Meston Walk, Aberdeen AB24 3UE, Scotland
^*Correspondence e-mail: w.harrison@abdn.ac.uk

Edited by M. Weil, Vienna University of Technology, Austria (Received 15 April 2014; accepted 16 May 2014; online 1 August 2014)

The complete polyoxidometallate anion in the title compound, (CH₆N₃)₄[H₆V₄As₆O₃₀]·4H₂O, is generated by crystallographic inversion symmetry. The polyhedral building units are distorted VO₆ octahedra and AsO₃OH tetrahedra. The VO₆ units feature a short formal V=O double bond and are linked by a common edge. Two such V₂O₆ double octahedral units are linked by four isolated AsO₃OH tetrahedra to complete the anion, which features two internal O—H⋯O hydrogen bonds. In the crystal, O—H⋯O hydrogen bonds between the polyoxidometallate anions generate (01-1) sheets. The sheets are connected by cation-to-cluster N—H⋯O hydrogen bonds, and cation-to-water N—H⋯O links also occur. The O atom of one of the water molecules is disordered over two sites in a 0.703 (17):0.297 (17) ratio.

Keywords: crystal structure; polyoxidometallate anion; vanadium; arsenic.

CCDC reference: 1004306

1. Related literature

For crystal structures containing the same type of anion accompanied by different counter-cations, see: Durif & Averbuch-Pouchot (1979 ); Nenoff et al. (1994 ); Bremner & Harrison (2002 ). The site symmetries of these anions include $[\overline{1}]$ (as seen for the title compound) as well as 2/m and mmm.

2. Experimental

2.1. Crystal data

(CH₆N₃)₄[H₆V₄As₆O₃₀]·4H₂O
M_r = 1447.71
Triclinic, $[P \overline 1]$
a = 10.0403 (5) Å
b = 11.0199 (6) Å
c = 11.9806 (6) Å
α = 114.892 (1)°
β = 94.696 (1)°
γ = 111.751 (1)°
V = 1071.39 (10) Å³
Z = 1
Mo Kα radiation
μ = 5.56 mm⁻¹
T = 293 K
0.30 × 0.20 × 0.20 mm

2.2. Data collection

Bruker SMART CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 1999 ) T_min = 0.287, T_max = 0.403
8711 measured reflections
4909 independent reflections
3655 reflections with I > 2σ(I)
R_int = 0.035

2.3. Refinement

R[F² > 2σ(F²)] = 0.047
wR(F²) = 0.129
S = 0.99
4909 reflections
271 parameters
H-atom parameters constrained
Δρ_max = 1.79 e Å⁻³
Δρ_min = −1.25 e Å⁻³

Table 1
Selected bond lengths (Å)

V1—O1	1.591 (4)
V1—O2	1.723 (4)
V1—O5	1.963 (4)
V1—O4	1.992 (4)
V1—O6	2.029 (4)
V1—O3	2.376 (4)
V2—O8	1.603 (5)
V2—O2	1.934 (4)
V2—O9	2.006 (4)
V2—O7	2.015 (4)
V2—O10	2.027 (4)
V2—O3	2.260 (4)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O12—H12⋯O4ⁱ	0.98	1.72	2.678 (5)	165
O14—H14⋯O13ⁱⁱ	0.96	1.66	2.579 (6)	158
O15—H15⋯O13ⁱⁱⁱ	0.96	1.67	2.619 (6)	170
N1—H1B⋯O13^iv	0.86	2.26	3.056 (8)	154
N1—H1A⋯O6^iv	0.86	2.18	3.007 (7)	160
N2—H2A⋯O15^v	0.86	2.20	3.042 (8)	167
N2—H2B⋯O11^iv	0.86	2.44	3.210 (8)	150
N2—H2B⋯O1^vi	0.86	2.47	3.040 (8)	125
N3—H3A⋯O9^v	0.86	2.05	2.895 (7)	169
N3—H3B⋯O1W	0.86	2.20	2.984 (10)	152
N4—H4A⋯O12^vi	0.86	2.30	3.089 (9)	152
N4—H4B⋯O10^vii	0.86	2.48	3.230 (9)	146
N5—H5A⋯O2WA^v	0.86	2.14	2.959 (13)	160
N5—H5B⋯O7^vii	0.86	2.19	2.963 (8)	150
N6—H6B⋯O12^vi	0.86	2.37	3.140 (9)	150
N6—H6B⋯O5^vi	0.86	2.45	3.022 (7)	125
N6—H6A⋯O2WB^v	0.86	2.01	2.78 (5)	148
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) -x+1, -y+2, -z+2; (iii) -x, -y+1, -z+1; (iv) x, y-1, z; (v) x+1, y, z; (vi) -x+1, -y, -z+1; (vii) -x+1, -y+1, -z+2.

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012 ) and ATOMS (Dowty, 1999 ); software used to prepare material for publication: SHELXL97.

Supporting information

CCDC reference: 1004306

Crystal structure: contains datablocks I, New_Global_Publ_Block. DOI: 10.1107/S1600536814011349/wm0004sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536814011349/wm0004Isup2.hkl

checkCIF report

Synthesis and crystallization top

0.91 g of V₂O₅ and 0.90 g of (CN₃H₆)₂CO₃ were added to 10 ml of a 0.1 M H₃AsO₄ solution and placed in a Teflon-lined hydrothermal vessel, which was heated to 423 K for 24 hours. After cooling to room temperature over several hours, solids were recovered by vacuum filtration to yield a few orange blocks of the title compound accompanied by an unidentified brown powder.

Refinement top

The H atoms were located in different maps (O—H) or geometrically placed (N—H) and refined as riding atoms with U_iso(H) = 1.2U_eq(carrier). The water-molecule H atoms could not be located in the present experiment. One of the water molecule O atoms is disordered over two adjacent sites in a 0.703 (17):0.297 (17) ratio.

Related literature top

For crystal structures containing the same type of anion accompanied by different counter-cations, see: Durif & Averbuch-Pouchot (1979); Nenoff et al. (1994); Bremner & Harrison (2002). The site symmetries of these anions include 1 (as seen for the title compound) as well as 2/m and mmm.

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012) and ATOMS (Dowty, 1999); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. The molecular structure of the (V₄As₆O₃₀H₆)^4- anion in the title compound showing 50% displacement ellipsoids. [Symmetry code: (i) –x, 1–y, 1–z.]
	Fig. 2. The packing of the title compound viewed down [100] with the anion shown in polyhedral representation (VO₆ octahedra orange, AsO₄ tetrahedra green). O—H···O hydrogen bonds within and between the anions are shown as yellow lines.

Tetraguanidinium [hexahydrogen hexaarsenato(V)tetravanadate(V)] tetrahydrate top

Crystal data top

(CH₆N₃)₄[H₆V₄As₆O₃₀]·4H₂O	Z = 1
M_r = 1447.71	F(000) = 704
Triclinic, P1	D_x = 2.244 Mg m⁻³
a = 10.0403 (5) Å	Mo Kα radiation, λ = 0.70173 Å
b = 11.0199 (6) Å	Cell parameters from 3266 reflections
c = 11.9806 (6) Å	θ = 2.3–27.5°
α = 114.892 (1)°	µ = 5.56 mm⁻¹
β = 94.696 (1)°	T = 293 K
γ = 111.751 (1)°	Block, orange
V = 1071.39 (10) Å³	0.30 × 0.20 × 0.20 mm

Data collection top

Bruker SMART CCD diffractometer	4909 independent reflections
Radiation source: fine-focus sealed tube	3655 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.035
ω scans	θ_max = 27.2°, θ_min = 1.9°
Absorption correction: multi-scan (SADABS; Bruker, 1999)	h = −13→13
T_min = 0.287, T_max = 0.403	k = −14→12
8711 measured reflections	l = −11→15

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.047	Hydrogen site location: mixed
wR(F²) = 0.129	H-atom parameters constrained
S = 0.99	w = 1/[σ²(F_o²) + (0.0766P)²] where P = (F_o² + 2F_c²)/3
4909 reflections	(Δ/σ)_max < 0.001
271 parameters	Δρ_max = 1.79 e Å⁻³
0 restraints	Δρ_min = −1.25 e Å⁻³

Crystal data top

(CH₆N₃)₄[H₆V₄As₆O₃₀]·4H₂O	γ = 111.751 (1)°
M_r = 1447.71	V = 1071.39 (10) Å³
Triclinic, P1	Z = 1
a = 10.0403 (5) Å	Mo Kα radiation
b = 11.0199 (6) Å	µ = 5.56 mm⁻¹
c = 11.9806 (6) Å	T = 293 K
α = 114.892 (1)°	0.30 × 0.20 × 0.20 mm
β = 94.696 (1)°

Data collection top

Bruker SMART CCD diffractometer	4909 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 1999)	3655 reflections with I > 2σ(I)
T_min = 0.287, T_max = 0.403	R_int = 0.035
8711 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.047	0 restraints
wR(F²) = 0.129	H-atom parameters constrained
S = 0.99	Δρ_max = 1.79 e Å⁻³
4909 reflections	Δρ_min = −1.25 e Å⁻³
271 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

	x	y	z	U_iso*/U_eq	Occ. (<1)
V1	0.26837 (10)	0.46285 (10)	0.57607 (9)	0.0176 (2)
V2	0.05032 (10)	0.50770 (11)	0.74922 (9)	0.0193 (2)
As1	0.26156 (6)	0.46227 (6)	0.30244 (6)	0.02044 (15)
As2	−0.08161 (6)	0.30204 (6)	0.44111 (5)	0.01626 (14)
As3	0.39072 (6)	0.77706 (6)	0.84192 (5)	0.01955 (15)
O1	0.3661 (5)	0.3738 (5)	0.5506 (4)	0.0282 (10)
O2	0.1882 (4)	0.4284 (4)	0.6880 (4)	0.0192 (8)
O3	0.1265 (4)	0.6002 (4)	0.6171 (4)	0.0194 (8)
O4	0.4243 (4)	0.6617 (4)	0.7138 (4)	0.0202 (8)
O5	0.0880 (4)	0.3108 (4)	0.4329 (4)	0.0198 (8)
O6	0.3215 (4)	0.5543 (4)	0.4605 (4)	0.0211 (8)
O7	−0.0827 (4)	0.6107 (5)	0.7760 (4)	0.0254 (9)
O8	0.0098 (5)	0.4435 (5)	0.8461 (4)	0.0328 (10)
O9	−0.1059 (4)	0.3374 (4)	0.5863 (4)	0.0216 (8)
O10	0.2301 (4)	0.7032 (4)	0.8748 (4)	0.0253 (9)
O11	0.3741 (5)	0.5860 (6)	0.2582 (5)	0.0389 (12)
O12	0.2976 (5)	0.3108 (5)	0.2403 (4)	0.0299 (10)
H12	0.4043	0.3389	0.2643	0.036*
O13	0.4138 (4)	0.9295 (4)	0.8315 (4)	0.0260 (9)
O14	0.5335 (5)	0.8266 (5)	0.9655 (4)	0.0319 (10)
H14	0.5560	0.9049	1.0518	0.038*
O15	−0.2016 (5)	0.1152 (4)	0.3450 (4)	0.0290 (10)
H15	−0.2710	0.1031	0.2766	0.035*
C1	0.6359 (8)	−0.0343 (7)	0.5654 (7)	0.0336 (15)
N1	0.5480 (7)	−0.1219 (6)	0.6055 (6)	0.0441 (16)
H1A	0.5002	−0.2169	0.5551	0.053*
H1B	0.5389	−0.0834	0.6818	0.053*
N2	0.6494 (8)	−0.0929 (7)	0.4497 (7)	0.0530 (19)
H2A	0.7044	−0.0363	0.4229	0.064*
H2B	0.6033	−0.1882	0.4001	0.064*
N3	0.7054 (8)	0.1105 (7)	0.6418 (7)	0.0510 (18)
H3A	0.7607	0.1680	0.6159	0.061*
H3B	0.6959	0.1482	0.7180	0.061*
C2	0.9422 (9)	0.0768 (8)	0.8896 (7)	0.0406 (17)
N4	0.8450 (8)	0.0292 (9)	0.9471 (8)	0.069 (2)
H4A	0.7854	−0.0646	0.9131	0.082*
H4B	0.8411	0.0919	1.0186	0.082*
N5	1.0309 (9)	0.2208 (7)	0.9432 (7)	0.061 (2)
H5A	1.0945	0.2540	0.9067	0.073*
H5B	1.0254	0.2818	1.0147	0.073*
N6	0.9483 (9)	−0.0180 (8)	0.7813 (7)	0.064 (2)
H6A	1.0112	0.0134	0.7435	0.076*
H6B	0.8894	−0.1120	0.7475	0.076*
O1W	0.7341 (7)	0.3408 (9)	0.9023 (6)	0.074 (2)
O2WA	0.2417 (12)	0.2587 (12)	0.7880 (10)	0.082 (4)*	0.703 (17)
O2WB	0.063 (5)	0.108 (5)	0.631 (5)	0.18 (2)*	0.297 (17)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
V1	0.0164 (4)	0.0168 (5)	0.0200 (5)	0.0099 (3)	0.0038 (4)	0.0073 (4)
V2	0.0180 (4)	0.0218 (5)	0.0200 (5)	0.0095 (4)	0.0055 (4)	0.0113 (4)
As1	0.0179 (3)	0.0225 (3)	0.0212 (3)	0.0109 (2)	0.0055 (2)	0.0093 (2)
As2	0.0159 (3)	0.0134 (3)	0.0203 (3)	0.0069 (2)	0.0036 (2)	0.0089 (2)
As3	0.0180 (3)	0.0178 (3)	0.0190 (3)	0.0090 (2)	0.0025 (2)	0.0055 (2)
O1	0.026 (2)	0.029 (2)	0.034 (2)	0.0197 (18)	0.0072 (18)	0.0131 (19)
O2	0.0200 (18)	0.0169 (19)	0.022 (2)	0.0090 (15)	0.0038 (15)	0.0109 (16)
O3	0.0208 (18)	0.0184 (19)	0.025 (2)	0.0113 (15)	0.0075 (16)	0.0136 (17)
O4	0.0168 (18)	0.0189 (19)	0.0205 (19)	0.0072 (15)	0.0075 (15)	0.0062 (16)
O5	0.0183 (18)	0.0166 (19)	0.022 (2)	0.0088 (15)	0.0058 (15)	0.0067 (16)
O6	0.0197 (18)	0.0189 (19)	0.020 (2)	0.0072 (15)	0.0042 (15)	0.0069 (16)
O7	0.0196 (19)	0.027 (2)	0.027 (2)	0.0131 (16)	0.0031 (17)	0.0086 (18)
O8	0.032 (2)	0.044 (3)	0.033 (2)	0.018 (2)	0.013 (2)	0.027 (2)
O9	0.0207 (19)	0.023 (2)	0.022 (2)	0.0098 (16)	0.0057 (16)	0.0120 (17)
O10	0.022 (2)	0.025 (2)	0.024 (2)	0.0098 (16)	0.0073 (17)	0.0076 (18)
O11	0.027 (2)	0.046 (3)	0.052 (3)	0.010 (2)	0.014 (2)	0.035 (3)
O12	0.022 (2)	0.026 (2)	0.037 (2)	0.0171 (17)	0.0060 (18)	0.0053 (19)
O13	0.027 (2)	0.019 (2)	0.027 (2)	0.0086 (16)	0.0018 (17)	0.0084 (17)
O14	0.030 (2)	0.031 (2)	0.023 (2)	0.0181 (19)	−0.0040 (18)	0.0021 (19)
O15	0.029 (2)	0.0147 (19)	0.034 (2)	0.0065 (16)	−0.0027 (18)	0.0091 (18)
C1	0.039 (4)	0.026 (3)	0.049 (4)	0.018 (3)	0.018 (3)	0.026 (3)
N1	0.059 (4)	0.024 (3)	0.050 (4)	0.012 (3)	0.024 (3)	0.024 (3)
N2	0.082 (5)	0.036 (4)	0.052 (4)	0.026 (3)	0.042 (4)	0.028 (3)
N3	0.066 (4)	0.032 (3)	0.049 (4)	0.011 (3)	0.027 (3)	0.023 (3)
C2	0.048 (4)	0.030 (4)	0.037 (4)	0.019 (3)	0.007 (3)	0.011 (3)
N4	0.057 (5)	0.051 (5)	0.078 (6)	0.017 (4)	0.028 (4)	0.018 (4)
N5	0.090 (6)	0.031 (4)	0.045 (4)	0.016 (4)	0.032 (4)	0.012 (3)
N6	0.096 (6)	0.036 (4)	0.050 (4)	0.030 (4)	0.031 (4)	0.012 (3)
O1W	0.062 (4)	0.101 (5)	0.049 (4)	0.019 (4)	0.003 (3)	0.047 (4)

Geometric parameters (Å, º) top

V1—O1	1.591 (4)	O3—As2ⁱ	1.671 (4)
V1—O2	1.723 (4)	O7—As1ⁱ	1.665 (4)
V1—O5	1.963 (4)	O12—H12	0.9769
V1—O4	1.992 (4)	O14—H14	0.9637
V1—O6	2.029 (4)	O15—H15	0.9600
V1—O3	2.376 (4)	C1—N2	1.304 (9)
V2—O8	1.603 (5)	C1—N3	1.309 (9)
V2—O2	1.934 (4)	C1—N1	1.330 (8)
V2—O9	2.006 (4)	N1—H1A	0.8600
V2—O7	2.015 (4)	N1—H1B	0.8600
V2—O10	2.027 (4)	N2—H2A	0.8600
V2—O3	2.260 (4)	N2—H2B	0.8600
As1—O6	1.649 (4)	N3—H3A	0.8600
As1—O7ⁱ	1.665 (4)	N3—H3B	0.8600
As1—O12	1.708 (4)	C2—N6	1.304 (9)
As1—O11	1.726 (5)	C2—N5	1.313 (9)
As2—O3ⁱ	1.671 (4)	C2—N4	1.318 (10)
As2—O9	1.675 (4)	N4—H4A	0.8600
As2—O5	1.683 (4)	N4—H4B	0.8600
As2—O15	1.719 (4)	N5—H5A	0.8600
As3—O13	1.669 (4)	N5—H5B	0.8600
As3—O10	1.679 (4)	N6—H6A	0.8600
As3—O4	1.687 (4)	N6—H6B	0.8600
As3—O14	1.714 (4)

O1—V1—O2	102.7 (2)	O13—As3—O4	109.0 (2)
O1—V1—O5	99.0 (2)	O10—As3—O4	117.33 (19)
O2—V1—O5	93.43 (17)	O13—As3—O14	108.5 (2)
O1—V1—O4	98.6 (2)	O10—As3—O14	107.1 (2)
O2—V1—O4	90.70 (17)	O4—As3—O14	101.8 (2)
O5—V1—O4	160.49 (18)	V1—O2—V2	119.8 (2)
O1—V1—O6	99.5 (2)	As2ⁱ—O3—V2	136.2 (2)
O2—V1—O6	157.65 (18)	As2ⁱ—O3—V1	137.1 (2)
O5—V1—O6	84.99 (16)	V2—O3—V1	86.10 (14)
O4—V1—O6	83.98 (16)	As3—O4—V1	124.0 (2)
O1—V1—O3	178.9 (2)	As2—O5—V1	121.6 (2)
O2—V1—O3	77.34 (16)	As1—O6—V1	125.2 (2)
O5—V1—O3	82.06 (15)	As1ⁱ—O7—V2	127.5 (2)
O4—V1—O3	80.26 (15)	As2—O9—V2	122.6 (2)
O6—V1—O3	80.37 (15)	As3—O10—V2	124.8 (2)
O8—V2—O2	99.5 (2)	As1—O12—H12	112.3
O8—V2—O9	100.3 (2)	As3—O14—H14	122.9
O2—V2—O9	87.28 (16)	As2—O15—H15	109.3
O8—V2—O7	96.9 (2)	N2—C1—N3	120.6 (6)
O2—V2—O7	163.55 (18)	N2—C1—N1	119.8 (6)
O9—V2—O7	88.82 (16)	N3—C1—N1	119.5 (7)
O8—V2—O10	97.8 (2)	C1—N1—H1A	120.0
O2—V2—O10	87.81 (16)	C1—N1—H1B	120.0
O9—V2—O10	161.83 (17)	H1A—N1—H1B	120.0
O7—V2—O10	90.97 (17)	C1—N2—H2A	120.0
O8—V2—O3	175.3 (2)	C1—N2—H2B	120.0
O2—V2—O3	76.60 (15)	H2A—N2—H2B	120.0
O9—V2—O3	82.29 (15)	C1—N3—H3A	120.0
O7—V2—O3	87.04 (16)	C1—N3—H3B	120.0
O10—V2—O3	79.55 (16)	H3A—N3—H3B	120.0
O6—As1—O7ⁱ	122.0 (2)	N6—C2—N5	121.2 (8)
O6—As1—O12	111.2 (2)	N6—C2—N4	120.1 (7)
O7ⁱ—As1—O12	102.3 (2)	N5—C2—N4	118.7 (7)
O6—As1—O11	103.8 (2)	C2—N4—H4A	120.0
O7ⁱ—As1—O11	110.7 (2)	C2—N4—H4B	120.0
O12—As1—O11	106.1 (2)	H4A—N4—H4B	120.0
O3ⁱ—As2—O9	114.15 (19)	C2—N5—H5A	120.0
O3ⁱ—As2—O5	112.86 (19)	C2—N5—H5B	120.0
O9—As2—O5	112.62 (19)	H5A—N5—H5B	120.0
O3ⁱ—As2—O15	108.9 (2)	C2—N6—H6A	120.0
O9—As2—O15	103.6 (2)	C2—N6—H6B	120.0
O5—As2—O15	103.63 (19)	H6A—N6—H6B	120.0
O13—As3—O10	112.3 (2)

O1—V1—O2—V2	−178.0 (2)	O3ⁱ—As2—O5—V1	92.3 (3)
O5—V1—O2—V2	−77.9 (2)	O9—As2—O5—V1	−38.8 (3)
O4—V1—O2—V2	83.0 (2)	O15—As2—O5—V1	−150.1 (3)
O6—V1—O2—V2	7.3 (6)	O1—V1—O5—As2	152.3 (3)
O3—V1—O2—V2	3.14 (19)	O2—V1—O5—As2	48.8 (3)
O8—V2—O2—V1	179.4 (2)	O4—V1—O5—As2	−53.1 (6)
O9—V2—O2—V1	79.4 (2)	O6—V1—O5—As2	−108.9 (3)
O7—V2—O2—V1	2.9 (7)	O3—V1—O5—As2	−27.9 (2)
O10—V2—O2—V1	−83.1 (2)	O7ⁱ—As1—O6—V1	67.3 (3)
O3—V2—O2—V1	−3.3 (2)	O12—As1—O6—V1	−53.5 (3)
O8—V2—O3—As2ⁱ	−152 (2)	O11—As1—O6—V1	−167.1 (3)
O2—V2—O3—As2ⁱ	173.8 (3)	O1—V1—O6—As1	73.3 (3)
O9—V2—O3—As2ⁱ	84.8 (3)	O2—V1—O6—As1	−111.9 (4)
O7—V2—O3—As2ⁱ	−4.4 (3)	O5—V1—O6—As1	−25.0 (3)
O10—V2—O3—As2ⁱ	−95.9 (3)	O4—V1—O6—As1	171.1 (3)
O8—V2—O3—V1	37 (3)	O3—V1—O6—As1	−107.8 (3)
O2—V2—O3—V1	2.09 (13)	O8—V2—O7—As1ⁱ	−88.3 (3)
O9—V2—O3—V1	−86.94 (14)	O2—V2—O7—As1ⁱ	88.2 (6)
O7—V2—O3—V1	−176.15 (14)	O9—V2—O7—As1ⁱ	12.0 (3)
O10—V2—O3—V1	92.32 (15)	O10—V2—O7—As1ⁱ	173.8 (3)
O1—V1—O3—As2ⁱ	91 (11)	O3—V2—O7—As1ⁱ	94.3 (3)
O2—V1—O3—As2ⁱ	−174.0 (3)	O3ⁱ—As2—O9—V2	−85.4 (3)
O5—V1—O3—As2ⁱ	−78.6 (3)	O5—As2—O9—V2	45.0 (3)
O4—V1—O3—As2ⁱ	93.1 (3)	O15—As2—O9—V2	156.3 (2)
O6—V1—O3—As2ⁱ	7.6 (3)	O8—V2—O9—As2	−153.2 (3)
O1—V1—O3—V2	−97 (10)	O2—V2—O9—As2	−54.0 (3)
O2—V1—O3—V2	−2.33 (14)	O7—V2—O9—As2	110.0 (3)
O5—V1—O3—V2	93.02 (15)	O10—V2—O9—As2	20.5 (7)
O4—V1—O3—V2	−95.27 (15)	O3—V2—O9—As2	22.8 (2)
O6—V1—O3—V2	179.25 (15)	O13—As3—O10—V2	109.2 (3)
O13—As3—O4—V1	−112.7 (3)	O4—As3—O10—V2	−18.1 (4)
O10—As3—O4—V1	16.3 (4)	O14—As3—O10—V2	−131.8 (3)
O14—As3—O4—V1	132.8 (3)	O8—V2—O10—As3	137.6 (3)
O1—V1—O4—As3	−142.3 (3)	O2—V2—O10—As3	38.3 (3)
O2—V1—O4—As3	−39.3 (3)	O9—V2—O10—As3	−36.1 (7)
O5—V1—O4—As3	63.0 (6)	O7—V2—O10—As3	−125.3 (3)
O6—V1—O4—As3	118.9 (3)	O3—V2—O10—As3	−38.5 (3)
O3—V1—O4—As3	37.7 (3)

Symmetry code: (i) −x, −y+1, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O12—H12···O4ⁱⁱ	0.98	1.72	2.678 (5)	165
O14—H14···O13ⁱⁱⁱ	0.96	1.66	2.579 (6)	158
O15—H15···O13ⁱ	0.96	1.67	2.619 (6)	170
N1—H1B···O13^iv	0.86	2.26	3.056 (8)	154
N1—H1A···O6^iv	0.86	2.18	3.007 (7)	160
N2—H2A···O15^v	0.86	2.20	3.042 (8)	167
N2—H2B···O11^iv	0.86	2.44	3.210 (8)	150
N2—H2B···O1^vi	0.86	2.47	3.040 (8)	125
N3—H3A···O9^v	0.86	2.05	2.895 (7)	169
N3—H3B···O1W	0.86	2.20	2.984 (10)	152
N4—H4A···O12^vi	0.86	2.30	3.089 (9)	152
N4—H4B···O10^vii	0.86	2.48	3.230 (9)	146
N5—H5A···O2WA^v	0.86	2.14	2.959 (13)	160
N5—H5B···O7^vii	0.86	2.19	2.963 (8)	150
N6—H6B···O12^vi	0.86	2.37	3.140 (9)	150
N6—H6B···O5^vi	0.86	2.45	3.022 (7)	125
N6—H6A···O2WB^v	0.86	2.01	2.78 (5)	148

Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) −x+1, −y+2, −z+2; (iv) x, y−1, z; (v) x+1, y, z; (vi) −x+1, −y, −z+1; (vii) −x+1, −y+1, −z+2.

Selected bond lengths (Å) top

V1—O1	1.591 (4)	V2—O8	1.603 (5)
V1—O2	1.723 (4)	V2—O2	1.934 (4)
V1—O5	1.963 (4)	V2—O9	2.006 (4)
V1—O4	1.992 (4)	V2—O7	2.015 (4)
V1—O6	2.029 (4)	V2—O10	2.027 (4)
V1—O3	2.376 (4)	V2—O3	2.260 (4)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O12—H12···O4ⁱ	0.98	1.72	2.678 (5)	165
O14—H14···O13ⁱⁱ	0.96	1.66	2.579 (6)	158
O15—H15···O13ⁱⁱⁱ	0.96	1.67	2.619 (6)	170
N1—H1B···O13^iv	0.86	2.26	3.056 (8)	154
N1—H1A···O6^iv	0.86	2.18	3.007 (7)	160
N2—H2A···O15^v	0.86	2.20	3.042 (8)	167
N2—H2B···O11^iv	0.86	2.44	3.210 (8)	150
N2—H2B···O1^vi	0.86	2.47	3.040 (8)	125
N3—H3A···O9^v	0.86	2.05	2.895 (7)	169
N3—H3B···O1W	0.86	2.20	2.984 (10)	152
N4—H4A···O12^vi	0.86	2.30	3.089 (9)	152
N4—H4B···O10^vii	0.86	2.48	3.230 (9)	146
N5—H5A···O2WA^v	0.86	2.14	2.959 (13)	160
N5—H5B···O7^vii	0.86	2.19	2.963 (8)	150
N6—H6B···O12^vi	0.86	2.37	3.140 (9)	150
N6—H6B···O5^vi	0.86	2.45	3.022 (7)	125
N6—H6A···O2WB^v	0.86	2.01	2.78 (5)	148

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y+2, −z+2; (iii) −x, −y+1, −z+1; (iv) x, y−1, z; (v) x+1, y, z; (vi) −x+1, −y, −z+1; (vii) −x+1, −y+1, −z+2.

References

Bremner, C. A. & Harrison, W. T. A. (2002). Acta Cryst. E58, m254–m256. Web of Science CSD CrossRef CAS IUCr Journals Google Scholar
Bruker (1999). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Dowty, E. (1999). ATOMS. Shape Software, Kingsport, Tennessee, USA. Google Scholar
Durif, A. & Averbuch-Pouchot, M. T. (1979). Acta Cryst. B35, 1441–1444. CrossRef CAS IUCr Journals Web of Science Google Scholar
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849–854. Web of Science CrossRef CAS IUCr Journals Google Scholar
Nenoff, T. M., Stucky, G. D. & Harrison, W. T. A. (1994). Z. Kristallogr. 209, 892–898. CrossRef CAS Web of Science Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar

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Volume 70| Part 9| September 2014| Pages m305-m306

doi:10.1107/S1600536814011349

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

Crystal structure of tetra­guanidinium [hexa­hydrogen hexa­arsenato(V)tetra­vanadate(V)] tetra­hydrate

1. Related literature

2. Experimental

2.1. Crystal data

2.2. Data collection

2.3. Refinement

Supporting information

References

metal-organic compounds

Crystal structure of tetraguanidinium [hexahydrogen hexaarsenato(V)tetravanadate(V)] tetrahydrate