catena-Poly[[[bis­(methanol-κO)bis­(seleno­cyanato-κN)manganese(II)]-μ-1,2-bis­(pyridin-4-yl)ethane-κ2N:N′] 1,2-bis­(pyridin-4-yl)ethane monosolvate]

Wöhlert, S.; Jess, I.; Näther, C.

doi:10.1107/S1600536813007150

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 69| Part 4| April 2013| Page m223

doi:10.1107/S1600536813007150

Open

access

catena-Poly[[[bis(methanol-κO)bis(selenocyanato-κN)manganese(II)]-μ-1,2-bis(pyridin-4-yl)ethane-κ²N:N′] 1,2-bis(pyridin-4-yl)ethane monosolvate]

Susanne Wöhlert,^a ^* Inke Jess ^a and Christian Näther ^a

^aInstitut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Max-Eyth-Strasse 2, 24118 Kiel, Germany
^*Correspondence e-mail: swoehlert@ac.uni-kiel.de

(Received 13 March 2013; accepted 14 March 2013; online 20 March 2013)

The reaction of manganese selenocyanate with 1,2-bis(pyridin-4-yl)ethane (bpa) leads to the title compound, {[Mn(NCSe)₂(C₁₂H₁₂N₂)(CH₃OH)₂]·C₁₂H₁₂N₂}_n. The Mn^II cation is coordinated by two N-bonded selenocyanate anions, two bpa ligands and two O-bonded methanol molecules, within a slightly distorted octahedral geometry. The Mn^II cations and the non-coordinating N-donor ligands are located on centers of inversion while the coordinating N-donor co-ligands are located on a twofold rotation axis. In the crystal, the Mn^II cations are linked into chains along the c-axis direction by the bpa ligands. The chains are further connected via a non-coordinating bpa ligand into layers parallel to (3-10) via O—H⋯N hydrogen-bonding interactions.

Related literature

For background to this work and the structures of related compounds, see: Boeckmann & Näther (2010 , 2012 ), Wöhlert et al. (2012 ), Wöhlert & Näther (2012a ,b ).

Experimental

Crystal data

[Mn(NCSe)₂(C₁₂H₁₂N₂)(CH₄O)₂]·C₁₂H₁₂N₂
M_r = 697.46
Monoclinic, C 2/c
a = 19.184 (1) Å
b = 9.7854 (4) Å
c = 17.3468 (9) Å
β = 108.624 (4)°
V = 3085.9 (3) Å³
Z = 4
Mo Kα radiation
μ = 2.82 mm⁻¹
T = 293 K
0.14 × 0.11 × 0.06 mm

Data collection

Stoe IPDS-2 diffractometer
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008 ) T_min = 0.493, T_max = 0.748
10827 measured reflections
2998 independent reflections
2556 reflections with I > 2σ(I)
R_int = 0.032

Refinement

R[F² > 2σ(F²)] = 0.042
wR(F²) = 0.094
S = 1.06
2998 reflections
179 parameters
H-atom parameters constrained
Δρ_max = 0.56 e Å⁻³
Δρ_min = −0.58 e Å⁻³

Table 1
Selected bond lengths (Å)

Mn1—N1	2.180 (3)
Mn1—O1	2.211 (2)
Mn1—N10	2.322 (2)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1O1⋯N20	0.82	1.92	2.731 (3)	173

Data collection: X-AREA (Stoe & Cie, 2008); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011 ); software used to prepare material for publication: XCIF in SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536813007150/bt6898sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536813007150/bt6898Isup2.hkl

checkCIF report

Comment top

Recently, we have reported on the synthesis and characterization of thiocyanate coordination polymers with monodentate and bidentate neutral co-ligands like e.g. pyridine, pyridazine or 1,2-bis(pyridin-4-yl)ethylene (Boeckmann & Näther, 2010, 2012; Wöhlert & Näther, 2012a; Wöhlert & Näther, 2012b). Within this project we investigated the influence of the neutral co-ligand on the structural, thermal and magnetic properties of such compounds. In further work we also investigated the influence of the anionic ligand. In this context we have reported a new coordination polymer based on cobalt(II) selenocyanate and 1,2-bis(pyridin-4-yl)ethylene, in which the cobalt(II) cations are connected by the selenocyanato anions into chains that are further linked into layers by the neutral N-donor co-ligand (Wöhlert et al., 2012). In the present investigation we tried to prepare similar compounds with manganese(II) selenocyanate and 1,2-bis(pyridin-4-yl)ethane (bpa), which results in the formation of single-crystals of the title compound.

The asymmetric unit of the title compound [Mn(NCSe)₂(C₁₂H₁₂N₂)(CH₃OH)₂]_n^.nC₁₂H₁₂N₂ solvate consists of a manganese(II) cation and one non-coordinating bpa ligand which are located on a center of inversion, one coordinating bpa ligand on a 2-fold rotation axis and one selenocyanate anion and one methanol molecule in general positions (Fig. 1). In the crystal structure each manganese(II) cation is coordinated by two terminal N-bonded selenocyanate anions, two O-bonded methanol molecules and two N-bonded bpa ligands within slightly distorted octahedra. The MnN₄O₂ distances ranges from 2.180 (3) Å to 2.322 (2) Å with angles around the manganese(II) cation between 88.87 (9) ° to 91.13 (9) ° and of 180 ° (Tab. 1). The manganese(II) cations are linked by the bpa ligands into chains which elongate in the direction of the crystallographic c-axis (Fig. 2). These chains are further linked into layers parallel to the (3 -1 0) plane by non-coordinated bpa molecules via O–H–N hydrogen bonding (Fig. 3).

Related literature top

For background to this work and the structures of related compounds, see: Boeckmann & Näther (2010, 2012), Wöhlert et al. (2012), Wöhlert & Näther (2012a,b).

Experimental top

MnCl₂x2H₂O, KNCSe and 1,2-bis(pyridin-4-yl)ethane were obtained from Alfa Aesar. All chemicals were used without further purification. 0.15 mmol (24 mg) MnCl₂x2H₂O and 0.2 mmol (28 mg) KNCSe were reacted with 0.6 mmol (109 mg) 1,2-bis(pyridin-4-yl)ethane in 1 ml methanol. Light-red single crystals of the title compound were obtained after one week.

Computing details top

Data collection: X-AREA (Stoe & Cie, 2008); cell refinement: X-AREA (Stoe & Cie, 2008); data reduction: X-AREA (Stoe & Cie, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011); software used to prepare material for publication: XCIF in SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. The crystal structure of the title compound with labeling and displacement ellipsoids drawn at the 50% probability level. [Symmetry codes: (i) -x,+1, -y+2, -z+1; (ii) -x+1, y, -z + 3/2; (iii) -x+1/2, -y+1/2, -z+1.]
	Fig. 2. The crystal structure of the title compound with view along the b-axis (black = manganese, blue = nitrogen, orange = selenium, red = oxygen, grey = carbon, white = hydrogen).
	Fig. 3. The crystal structure of the title compound with O—H···N hydrogen bonds shown as dashed lines (black = manganese, blue = nitrogen, orange = selenium, red = oxygen, grey = carbon, white = hydrogen).

catena-Poly[[[bis(methanol-κO)bis(selenocyanato-κN)manganese(II)]-µ-1,2-bis(pyridin-4-yl)ethane-κ²N:N'] 1,2-bis(pyridin-4-yl)ethane monosolvate] top

Crystal data top

[Mn(NCSe)₂(C₁₂H₁₂N₂)(CH₄O)₂]·C₁₂H₁₂N₂	F(000) = 1404
M_r = 697.46	D_x = 1.501 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 10827 reflections
a = 19.184 (1) Å	θ = 2.2–26.0°
b = 9.7854 (4) Å	µ = 2.82 mm⁻¹
c = 17.3468 (9) Å	T = 293 K
β = 108.624 (4)°	Block, light-red
V = 3085.9 (3) Å³	0.14 × 0.11 × 0.06 mm
Z = 4

Data collection top

Stoe IPDS-2 diffractometer	2998 independent reflections
Radiation source: fine-focus sealed tube	2556 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.032
ω scan	θ_max = 26.0°, θ_min = 2.2°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	h = −23→23
T_min = 0.493, T_max = 0.748	k = −12→10
10827 measured reflections	l = −21→21

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)] = 0.042	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.094	H-atom parameters constrained
S = 1.06	w = 1/[σ²(F_o²) + (0.0346P)² + 5.6439P] where P = (F_o² + 2F_c²)/3
2998 reflections	(Δ/σ)_max = 0.001
179 parameters	Δρ_max = 0.56 e Å⁻³
0 restraints	Δρ_min = −0.58 e Å⁻³

Crystal data top

[Mn(NCSe)₂(C₁₂H₁₂N₂)(CH₄O)₂]·C₁₂H₁₂N₂	V = 3085.9 (3) Å³
M_r = 697.46	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 19.184 (1) Å	µ = 2.82 mm⁻¹
b = 9.7854 (4) Å	T = 293 K
c = 17.3468 (9) Å	0.14 × 0.11 × 0.06 mm
β = 108.624 (4)°

Data collection top

Stoe IPDS-2 diffractometer	2998 independent reflections
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	2556 reflections with I > 2σ(I)
T_min = 0.493, T_max = 0.748	R_int = 0.032
10827 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.042	0 restraints
wR(F²) = 0.094	H-atom parameters constrained
S = 1.06	Δρ_max = 0.56 e Å⁻³
2998 reflections	Δρ_min = −0.58 e Å⁻³
179 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
Mn1	0.5000	1.0000	0.5000	0.04285 (17)
N1	0.58695 (16)	0.8976 (3)	0.59516 (18)	0.0613 (7)
C1	0.63537 (18)	0.8574 (3)	0.64832 (19)	0.0490 (7)
Se1	0.71095 (2)	0.79679 (6)	0.72941 (2)	0.07953 (18)
N10	0.51948 (13)	1.1948 (3)	0.58050 (15)	0.0456 (6)
C10	0.48071 (18)	1.3084 (3)	0.55279 (19)	0.0519 (7)
H10	0.4496	1.3092	0.4992	0.062*
C11	0.48422 (19)	1.4238 (3)	0.59895 (19)	0.0538 (7)
H11	0.4558	1.4997	0.5765	0.065*
C12	0.52999 (17)	1.4274 (3)	0.67895 (18)	0.0479 (7)
C13	0.57134 (18)	1.3113 (3)	0.70726 (19)	0.0506 (7)
H13	0.6036	1.3087	0.7602	0.061*
C14	0.56489 (18)	1.1998 (3)	0.65745 (18)	0.0503 (7)
H14	0.5936	1.1235	0.6782	0.060*
C15	0.5318 (2)	1.5500 (3)	0.7320 (2)	0.0579 (8)
H15B	0.5292	1.6324	0.7002	0.070*
H15A	0.5782	1.5512	0.7761	0.070*
N20	0.34138 (14)	0.6923 (3)	0.51881 (16)	0.0499 (6)
C20	0.31374 (17)	0.6393 (3)	0.57385 (19)	0.0504 (7)
H20	0.3201	0.6876	0.6218	0.060*
C21	0.27652 (18)	0.5175 (3)	0.5634 (2)	0.0525 (8)
H21	0.2592	0.4845	0.6042	0.063*
C22	0.26479 (16)	0.4436 (3)	0.49260 (19)	0.0484 (7)
C23	0.29261 (19)	0.4991 (4)	0.4349 (2)	0.0556 (8)
H23	0.2864	0.4537	0.3861	0.067*
C24	0.32931 (18)	0.6210 (4)	0.4504 (2)	0.0556 (8)
H24	0.3470	0.6565	0.4105	0.067*
C25	0.22544 (19)	0.3082 (3)	0.4790 (2)	0.0594 (8)
H25B	0.2067	0.2898	0.4211	0.071*
H25A	0.1838	0.3135	0.4991	0.071*
O1	0.41951 (12)	0.9297 (2)	0.55852 (13)	0.0569 (6)
H1O1	0.3981	0.8571	0.5437	0.085*
C2	0.4253 (2)	0.9473 (4)	0.6411 (2)	0.0733 (11)
H2A	0.4674	0.8985	0.6747	0.110*
H2B	0.3817	0.9126	0.6502	0.110*
H2C	0.4305	1.0427	0.6546	0.110*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mn1	0.0432 (3)	0.0442 (3)	0.0405 (3)	−0.0021 (3)	0.0125 (3)	−0.0006 (3)
N1	0.0589 (17)	0.0628 (18)	0.0552 (16)	0.0070 (14)	0.0083 (14)	0.0008 (14)
C1	0.0547 (18)	0.0482 (17)	0.0464 (17)	−0.0017 (14)	0.0194 (15)	−0.0048 (13)
Se1	0.0631 (2)	0.1235 (4)	0.0473 (2)	0.0165 (2)	0.01114 (17)	0.0192 (2)
N10	0.0458 (13)	0.0472 (14)	0.0446 (13)	−0.0059 (11)	0.0153 (11)	−0.0015 (11)
C10	0.0552 (18)	0.0522 (18)	0.0444 (16)	0.0001 (15)	0.0105 (14)	−0.0015 (14)
C11	0.0618 (19)	0.0460 (18)	0.0528 (18)	0.0041 (15)	0.0171 (15)	0.0027 (14)
C12	0.0551 (17)	0.0460 (17)	0.0474 (16)	−0.0100 (14)	0.0231 (14)	−0.0007 (13)
C13	0.0529 (17)	0.0551 (19)	0.0411 (15)	−0.0065 (15)	0.0113 (13)	0.0002 (14)
C14	0.0531 (17)	0.0491 (17)	0.0471 (17)	0.0008 (14)	0.0139 (14)	0.0028 (14)
C15	0.078 (2)	0.0452 (17)	0.0534 (18)	−0.0115 (16)	0.0252 (17)	−0.0031 (15)
N20	0.0517 (14)	0.0441 (14)	0.0524 (15)	−0.0061 (12)	0.0144 (12)	0.0033 (11)
C20	0.0539 (18)	0.0471 (17)	0.0509 (17)	−0.0018 (14)	0.0179 (15)	−0.0029 (14)
C21	0.0586 (18)	0.0501 (19)	0.0542 (18)	−0.0050 (15)	0.0258 (15)	0.0060 (14)
C22	0.0445 (16)	0.0423 (15)	0.0574 (18)	−0.0046 (13)	0.0150 (14)	0.0021 (14)
C23	0.064 (2)	0.0557 (18)	0.0476 (17)	−0.0113 (17)	0.0184 (15)	−0.0044 (15)
C24	0.0605 (19)	0.058 (2)	0.0504 (17)	−0.0138 (16)	0.0208 (15)	0.0050 (15)
C25	0.0547 (19)	0.0495 (19)	0.073 (2)	−0.0122 (15)	0.0186 (17)	−0.0020 (16)
O1	0.0645 (14)	0.0578 (13)	0.0537 (12)	−0.0239 (11)	0.0262 (11)	−0.0092 (11)
C2	0.088 (3)	0.083 (3)	0.056 (2)	−0.030 (2)	0.032 (2)	−0.0117 (19)

Geometric parameters (Å, º) top

Mn1—N1ⁱ	2.180 (3)	C15—H15A	0.9700
Mn1—N1	2.180 (3)	N20—C24	1.331 (4)
Mn1—O1ⁱ	2.211 (2)	N20—C20	1.336 (4)
Mn1—O1	2.211 (2)	C20—C21	1.372 (4)
Mn1—N10ⁱ	2.322 (2)	C20—H20	0.9300
Mn1—N10	2.322 (2)	C21—C22	1.380 (5)
N1—C1	1.149 (4)	C21—H21	0.9300
C1—Se1	1.769 (3)	C22—C23	1.386 (4)
N10—C10	1.338 (4)	C22—C25	1.506 (4)
N10—C14	1.342 (4)	C23—C24	1.368 (5)
C10—C11	1.374 (4)	C23—H23	0.9300
C10—H10	0.9300	C24—H24	0.9300
C11—C12	1.386 (4)	C25—C25ⁱⁱⁱ	1.509 (7)
C11—H11	0.9300	C25—H25B	0.9700
C12—C13	1.383 (5)	C25—H25A	0.9700
C12—C15	1.506 (4)	O1—C2	1.412 (4)
C13—C14	1.372 (4)	O1—H1O1	0.8200
C13—H13	0.9300	C2—H2A	0.9600
C14—H14	0.9300	C2—H2B	0.9600
C15—C15ⁱⁱ	1.538 (7)	C2—H2C	0.9600
C15—H15B	0.9700

N1ⁱ—Mn1—N1	180.000 (1)	C12—C15—H15B	109.1
N1ⁱ—Mn1—O1ⁱ	89.25 (10)	C15ⁱⁱ—C15—H15B	109.1
N1—Mn1—O1ⁱ	90.75 (10)	C12—C15—H15A	109.1
N1ⁱ—Mn1—O1	90.75 (10)	C15ⁱⁱ—C15—H15A	109.1
N1—Mn1—O1	89.25 (10)	H15B—C15—H15A	107.9
O1ⁱ—Mn1—O1	180.0	C24—N20—C20	116.0 (3)
N1ⁱ—Mn1—N10ⁱ	89.13 (10)	N20—C20—C21	123.5 (3)
N1—Mn1—N10ⁱ	90.87 (10)	N20—C20—H20	118.3
O1ⁱ—Mn1—N10ⁱ	88.92 (8)	C21—C20—H20	118.3
O1—Mn1—N10ⁱ	91.08 (8)	C20—C21—C22	120.2 (3)
N1ⁱ—Mn1—N10	90.87 (10)	C20—C21—H21	119.9
N1—Mn1—N10	89.13 (10)	C22—C21—H21	119.9
O1ⁱ—Mn1—N10	91.08 (8)	C21—C22—C23	116.5 (3)
O1—Mn1—N10	88.92 (8)	C21—C22—C25	122.1 (3)
N10ⁱ—Mn1—N10	180.0	C23—C22—C25	121.4 (3)
C1—N1—Mn1	172.7 (3)	C24—C23—C22	119.5 (3)
N1—C1—Se1	179.0 (3)	C24—C23—H23	120.2
C10—N10—C14	115.9 (3)	C22—C23—H23	120.2
C10—N10—Mn1	120.1 (2)	N20—C24—C23	124.3 (3)
C14—N10—Mn1	123.9 (2)	N20—C24—H24	117.8
N10—C10—C11	123.7 (3)	C23—C24—H24	117.8
N10—C10—H10	118.1	C22—C25—C25ⁱⁱⁱ	112.6 (3)
C11—C10—H10	118.1	C22—C25—H25B	109.1
C10—C11—C12	120.1 (3)	C25ⁱⁱⁱ—C25—H25B	109.1
C10—C11—H11	119.9	C22—C25—H25A	109.1
C12—C11—H11	119.9	C25ⁱⁱⁱ—C25—H25A	109.1
C13—C12—C11	116.3 (3)	H25B—C25—H25A	107.8
C13—C12—C15	122.6 (3)	C2—O1—Mn1	126.0 (2)
C11—C12—C15	121.1 (3)	C2—O1—H1O1	107.0
C14—C13—C12	120.2 (3)	Mn1—O1—H1O1	118.7
C14—C13—H13	119.9	O1—C2—H2A	109.5
C12—C13—H13	119.9	O1—C2—H2B	109.5
N10—C14—C13	123.7 (3)	H2A—C2—H2B	109.5
N10—C14—H14	118.1	O1—C2—H2C	109.5
C13—C14—H14	118.1	H2A—C2—H2C	109.5
C12—C15—C15ⁱⁱ	112.4 (2)	H2B—C2—H2C	109.5

Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x+1, y, −z+3/2; (iii) −x+1/2, −y+1/2, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1O1···N20	0.82	1.92	2.731 (3)	173

Experimental details

Crystal data
Chemical formula	[Mn(NCSe)₂(C₁₂H₁₂N₂)(CH₄O)₂]·C₁₂H₁₂N₂
M_r	697.46
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	293
a, b, c (Å)	19.184 (1), 9.7854 (4), 17.3468 (9)
β (°)	108.624 (4)
V (Å³)	3085.9 (3)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	2.82
Crystal size (mm)	0.14 × 0.11 × 0.06

Data collection
Diffractometer	Stoe IPDS2 diffractometer
Absorption correction	Numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)
T_min, T_max	0.493, 0.748
No. of measured, independent and observed [I > 2σ(I)] reflections	10827, 2998, 2556
R_int	0.032
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.042, 0.094, 1.06
No. of reflections	2998
No. of parameters	179
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.56, −0.58

Computer programs: X-AREA (Stoe & Cie, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011), XCIF in SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

Mn1—N1	2.180 (3)	Mn1—N10	2.322 (2)
Mn1—O1	2.211 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1O1···N20	0.82	1.92	2.731 (3)	172.6

Acknowledgements

We gratefully acknowledge financial support by the DFG (project No. NA 720/3–1) and the State of Schleswig–Holstein. We thank Professor Dr Wolfgang Bensch for access to his experimental facility.

References

Boeckmann, J. & Näther, C. (2010). Dalton Trans. 39, 11019–11026. Web of Science CSD CrossRef CAS PubMed Google Scholar
Boeckmann, J. & Näther, C. (2012). Polyhedron, 31, 587–595. Web of Science CSD CrossRef CAS Google Scholar
Brandenburg, K. (2011). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Stoe & Cie (2008). X-AREA, X-RED32 and X-SHAPE. Stoe & Cie, Darmstadt, Germany. Google Scholar
Wöhlert, S. & Näther, C. (2012a). Z. Anorg. Allg. Chem. 638, 2262–2272. Google Scholar
Wöhlert, S. & Näther, C. (2012b). Z. Naturforsch. Teil B, 67, 41–50. Google Scholar
Wöhlert, S., Ruschewitz, U. & Näther, C. (2012). Cryst. Growth Des. 12, 2715–2718. Google Scholar

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.