catena-Poly[[μ3-hydroxido-tetra-μ2-pyrid­azine-1:2κ4N:N′;1:3κ2N:N′;2:3κ2N:N′-tetrakis(selenocyanato)-1κN,2κN,3κ2N-trizinc(II)]-μ-cyanido-1:2′κ2C:N]

Reinert, T.; Boeckmann, J.; Jess, I.; Näther, C.

doi:10.1107/S1600536810029107

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 8| August 2010| Pages m1018-m1019

https://doi.org/10.1107/S1600536810029107

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catena-Poly[[μ₃-hydroxido-tetra-μ₂-pyridazine-1:2κ⁴N:N′;1:3κ²N:N′;2:3κ²N:N′-tetrakis(selenocyanato)-1κN,2κN,3κ²N-trizinc(II)]-μ-cyanido-1:2′κ²C:N]

Thorben Reinert,^a Jan Boeckmann,^a Inke Jess ^a and Christian Näther ^a ^*

^aInstitut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Max-Eyth-Str. 2, 24098 Kiel, Germany
^*Correspondence e-mail: cnaether@ac.uni-kiel.de

(Received 19 July 2010; accepted 21 July 2010; online 24 July 2010)

In the crystal structure of the title compound, [Zn₃(NCSe)₄(OH)(CN)(C₄H₄N₂)₄]_n one of the two crystallographically independent zinc(II) cations is coordinated by two terminal N-bonded selenocyanato anions and two N atoms of two symmetry-related pyridazine ligands in a trigonal-bipyramidal geometry, while the other zinc(II) cation is coordinated by one terminal N-bonded selenocyanato anion, one μ-1,2-cyanido anion and three N atoms of three crystallographically independent pyridazine ligands in a slightly distorted octahedral coordination geometry. The zinc(II) atoms are further connected via a μ₃-hydroxido anion into trinuclear building blocks. The formula unit consists of three zinc cations, four selenocyanato anions, one μ₃-hydroxido anion, four pyridazine molecules as well as one cyanido anion. The asymmetric unit contains half of a formula unit. One of the zinc atoms, two selenocyanato anions, two pyridazine ligands and the μ₃-hydroxido anion are located on a crystallographic mirror plane, whereas the cyanido anion is located on a twofold rotation axis. Therefore, this anion is disordered due to symmetry. The cyanido anions connect the metal centres into polymeric zigzag chains propagating along the a axis.

Related literature

For related μ₃-hydroxo Zn coordination, see: Alexiou et al. (2005 ); Jana et al. (2006 ). For general background to inorganic–organic coordination polymers based on zinc(II) halides or pseudohalides and N-donor ligands, see: Näther et al. (2007 ); Bhosekar et al. (2006 ).

Experimental

Crystal data

[Zn₃(CNSe)₄(OH)(CN)(C₄H₄N₂)₄]
M_r = 979.43
Orthorhombic, A m a 2
a = 15.6156 (12) Å
b = 22.6489 (16) Å
c = 8.6626 (5) Å
V = 3063.8 (4) Å³
Z = 4
Mo Kα radiation
μ = 7.12 mm⁻¹
T = 170 K
0.16 × 0.12 × 0.06 mm

Data collection

STOE IPDS-1 diffractometer
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe, 2008 ) T_min = 0.196, T_max = 0.503
22283 measured reflections
3752 independent reflections
3588 reflections with I > 2σ(I)
R_int = 0.049

Refinement

R[F² > 2σ(F²)] = 0.024
wR(F²) = 0.058
S = 1.03
3752 reflections
206 parameters
1 restraint
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.42 e Å⁻³
Δρ_min = −0.65 e Å⁻³
Absolute structure: Flack (1983 ), 1747 Friedel pairs
Flack parameter: −0.012 (10)

Table 1
Selected bond lengths (Å)

Zn1—N1	1.985 (5)
Zn1—O1	1.997 (3)
Zn1—N2	2.015 (4)
Zn1—N11	2.214 (3)
Zn2—N3	2.092 (3)
Zn2—O1	2.1254 (19)
Zn2—N41	2.141 (3)
Zn2—N31	2.174 (3)
Zn2—N21	2.227 (3)
Zn2—N12	2.247 (3)

Data collection: X-AREA (Stoe, 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, 2010 ); software used to prepare material for publication: XCIF in SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536810029107/bt5302sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810029107/bt5302Isup2.hkl

checkCIF report

Comment top

Recently, we have investigated inorganic organic coordination polymers based on zinc(II) halides or pseudohalides and N-donor ligands (Näther et al., 2007; Bhosekar et al., 2006). In our ongoing investigation on the synthesis, structures and properties of such compounds based on diamagnetic transition metals, pseudo-halides and N-donor ligands, we have reacted zinc(II) dinitrate, potassium selenocyanate and pyridazine in water. In this reaction single crystals were obtained by accident, which were identified as the title compound by single-crystal X-ray diffraction.

The title compound of composition [Zn₃(NCSe)₄(OH^-)(CN^-)(pyridazine)₄]_n (Fig. 1) represents a polymeric chain, in which trinuclear building units built up of three zinc(II) cations centered by a µ₃-hydroxido anion are connected by µ-1,2-cyanido anions. One of the three zinc cations is coordinated by two selenocyanato anions, two N atoms of two pyridazine ligands and one µ₃-hydroxido anion in a distorted trigonal bipyramidal coordination environment. The other two zinc(II) cations, are each coordinated by one selenocyanato, one µ-1,2-cyanido and one µ₃-hydroxido anion and three N atoms of three pyridazine ligands in a slightly distorted octahedral coordination geometry. The Zn—N_pyridazine distances range between 2.174 (3) Å and 2.247 (3) Å, whereas the Zn—N_{selenocyanato} distances of the terminally N-bonded selenocyanato anions range between 1.985 (5) Å and 2.092 (3) Å. The angles around the trigonally bipyramidally coordinated metal centre range between 113.64 (18) - 130.90 (17)° and 177.39 (16)° (Tab. 1), whereas the angles around the octahedrally coordinated metal centres range between 83.09 (12) - 93.64 (12) and 178.62 (10)° (Tab. 1). The µ₃-hydroxido anion coordination of the metal centres is not unusual and is similar to that found in related structures (Alexiou et al., 2005; Jana et al., 2006). The shortest Zn···Zn distances of the trinuclear metal centre amount to 3.4450 (5), whereas the shortest intrachain and interchain Zn···Zn distances amount to 5.2687 (5) and 9.0482 (6), respectively (Fig. 3).

Related literature top

For related µ₃-hydroxido Zn coordination, see: Alexiou et al. (2005); Jana et al. (2006). For general background to inorganic–organic coordination polymers based on zinc(II) halides or pseudohalides and N-donor ligands, see: Näther et al. (2007); Bhosekar et al. (2006).

Experimental top

Zn(NO₃)₂ x 6H₂O was obtained from Merck, KNCSe and pyridazine were obtained from Alfa Aesar. 1 mmol (128 mg) Zn(NO₃)₂ x 6H₂O, 2 mmol (288 mg) KNCSe, 2 mmol (160 mg) pyridazine and 3 ml water were reacted in a closed snap-vail without stirring. After the mixture has been standing for several days in the dark at room temperature light-yellow needle like single crystals of the title compound were obtained in a mixture with unknown phases.

Structure description top

Computing details top

Data collection: X-AREA (Stoe, 2008); cell refinement: X-AREA (Stoe, 2008); data reduction: X-AREA (Stoe, 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, 2010); software used to prepare material for publication: XCIF in SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. : Crystal structure of the discrete title compound with labelling and displacement ellipsoids drawn at the 50% probability level. Symmetry codes: i: -x + 3/2, y, z; ii: -x + 1, -y + 1, z.
	Fig. 2. : Crystal structure of the title compound with view onto the polymeric chain along the crystallographic c-axis.
	Fig. 3. : Crystal structure of the title compound with topview onto the crystallographic ab-plane.

catena-Poly[[µ₃-hydroxido-tetra-µ₂-pyridazine- 1:2κ⁴N:N';1:3κ²N:N'; 2:3κ²N:N'-tetrakis(selenocyanato)- 1κN,2κN,3κ²N- trizinc(II)]-µ-cyanido-1:2'κ²C:N] top

Crystal data top

[Zn₃(CNSe)₄(OH)(CN)(C₄H₄N₂)₄]	F(000) = 1872
M_r = 979.43	D_x = 2.123 Mg m⁻³
Orthorhombic, Ama2	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: A 2 -2a	Cell parameters from 8001 reflections
a = 15.6156 (12) Å	θ = 2.5–28.1°
b = 22.6489 (16) Å	µ = 7.12 mm⁻¹
c = 8.6626 (5) Å	T = 170 K
V = 3063.8 (4) Å³	Needle, light-yellow
Z = 4	0.16 × 0.12 × 0.06 mm

Data collection top

STOE IPDS-1 diffractometer	3752 independent reflections
Radiation source: fine-focus sealed tube	3588 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.049
Phi scans	θ_max = 28.1°, θ_min = 2.5°
Absorption correction: numerical (X-SHAPE and X-RED32 ;Stoe, 2008)	h = −20→20
T_min = 0.196, T_max = 0.503	k = −29→29
22283 measured reflections	l = −11→11

Refinement top

Refinement on F²	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F² > 2σ(F²)] = 0.024	w = 1/[σ²(F_o²) + (0.0346P)² + 4.6032P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.058	(Δ/σ)_max = 0.002
S = 1.03	Δρ_max = 0.42 e Å⁻³
3752 reflections	Δρ_min = −0.65 e Å⁻³
206 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
1 restraint	Extinction coefficient: 0.00122 (10)
Primary atom site location: structure-invariant direct methods	Absolute structure: Flack (1983), 1747 Friedel pairs
Secondary atom site location: difference Fourier map	Absolute structure parameter: −0.012 (10)

Crystal data top

[Zn₃(CNSe)₄(OH)(CN)(C₄H₄N₂)₄]	V = 3063.8 (4) Å³
M_r = 979.43	Z = 4
Orthorhombic, Ama2	Mo Kα radiation
a = 15.6156 (12) Å	µ = 7.12 mm⁻¹
b = 22.6489 (16) Å	T = 170 K
c = 8.6626 (5) Å	0.16 × 0.12 × 0.06 mm

Data collection top

STOE IPDS-1 diffractometer	3752 independent reflections
Absorption correction: numerical (X-SHAPE and X-RED32 ;Stoe, 2008)	3588 reflections with I > 2σ(I)
T_min = 0.196, T_max = 0.503	R_int = 0.049
22283 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.024	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.058	Δρ_max = 0.42 e Å⁻³
S = 1.03	Δρ_min = −0.65 e Å⁻³
3752 reflections	Absolute structure: Flack (1983), 1747 Friedel pairs
206 parameters	Absolute structure parameter: −0.012 (10)
1 restraint

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)
Zn1	0.7500	0.69593 (2)	0.31561 (6)	0.01454 (11)
Zn2	0.63959 (2)	0.565314 (15)	0.35942 (4)	0.01401 (9)
O1	0.7500	0.61613 (13)	0.4136 (4)	0.0124 (6)
H1	0.7500	0.619 (4)	0.500 (12)	0.05 (3)*
Se1	0.7500	0.70340 (2)	−0.25158 (6)	0.02447 (12)
C1	0.7500	0.6962 (2)	−0.0473 (6)	0.0211 (10)
N1	0.7500	0.6936 (2)	0.0866 (6)	0.0283 (10)
Se2	0.7500	0.89017 (2)	0.57363 (7)	0.02695 (13)
C2	0.7500	0.8214 (2)	0.4730 (6)	0.0180 (9)
N2	0.7500	0.77724 (17)	0.4100 (5)	0.0209 (9)
Se3	0.45849 (2)	0.591502 (15)	0.83059 (4)	0.02298 (9)
C3	0.5344 (2)	0.58566 (15)	0.6754 (4)	0.0198 (7)
N3	0.58164 (18)	0.58100 (13)	0.5733 (4)	0.0210 (6)
N11	0.60825 (17)	0.69737 (12)	0.3112 (4)	0.0203 (6)
N12	0.56988 (17)	0.64629 (12)	0.2776 (3)	0.0161 (5)
C11	0.4879 (2)	0.64663 (16)	0.2356 (5)	0.0244 (7)
H11	0.4619	0.6103	0.2074	0.029*
C12	0.4386 (2)	0.69777 (17)	0.2312 (6)	0.0334 (10)
H12	0.3799	0.6964	0.2026	0.040*
C13	0.4770 (2)	0.74982 (17)	0.2690 (7)	0.0410 (12)
H13	0.4463	0.7860	0.2689	0.049*
C14	0.5641 (2)	0.74755 (16)	0.3081 (6)	0.0339 (10)
H14	0.5927	0.7833	0.3334	0.041*
N21	0.70660 (17)	0.48500 (12)	0.4454 (3)	0.0160 (5)
C21	0.6652 (2)	0.43725 (16)	0.4926 (5)	0.0242 (7)
H21	0.6043	0.4381	0.4938	0.029*
C22	0.7066 (2)	0.38574 (17)	0.5405 (5)	0.0302 (8)
H22	0.6751	0.3519	0.5720	0.036*
N31	0.70651 (16)	0.55138 (11)	0.1423 (3)	0.0140 (5)
C31	0.6645 (2)	0.54118 (15)	0.0115 (4)	0.0198 (6)
H31	0.6037	0.5408	0.0133	0.024*
C32	0.7064 (2)	0.53091 (16)	−0.1289 (4)	0.0222 (7)
H32	0.6750	0.5242	−0.2211	0.027*
N41	0.53181 (18)	0.51316 (13)	0.2907 (4)	0.0168 (6)	0.50
C41	0.53181 (18)	0.51316 (13)	0.2907 (4)	0.0168 (6)	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zn1	0.0139 (2)	0.0139 (2)	0.0157 (3)	0.000	0.000	0.00062 (18)
Zn2	0.00941 (14)	0.01595 (16)	0.01666 (19)	−0.00099 (12)	0.00125 (13)	−0.00029 (13)
O1	0.0098 (13)	0.0144 (14)	0.0130 (17)	0.000	0.000	0.0006 (12)
Se1	0.0252 (2)	0.0320 (3)	0.0162 (3)	0.000	0.000	−0.00013 (19)
C1	0.016 (2)	0.020 (2)	0.026 (3)	0.000	0.000	0.0012 (19)
N1	0.026 (2)	0.037 (3)	0.021 (3)	0.000	0.000	−0.0007 (19)
Se2	0.0326 (3)	0.0148 (2)	0.0334 (3)	0.000	0.000	−0.0050 (2)
C2	0.015 (2)	0.021 (2)	0.017 (2)	0.000	0.000	0.0075 (18)
N2	0.0187 (19)	0.0137 (18)	0.030 (2)	0.000	0.000	−0.0081 (17)
Se3	0.02313 (16)	0.02491 (16)	0.02089 (19)	0.00440 (12)	0.00737 (13)	0.00093 (13)
C3	0.0202 (16)	0.0189 (16)	0.0204 (19)	−0.0006 (12)	−0.0082 (13)	−0.0005 (12)
N3	0.0187 (13)	0.0253 (14)	0.0190 (15)	0.0008 (11)	0.0058 (11)	0.0006 (11)
N11	0.0139 (12)	0.0160 (12)	0.0309 (17)	0.0008 (9)	−0.0026 (11)	0.0011 (11)
N12	0.0154 (12)	0.0156 (12)	0.0172 (15)	−0.0007 (10)	−0.0005 (9)	0.0008 (10)
C11	0.0198 (16)	0.0213 (16)	0.032 (2)	−0.0004 (13)	−0.0060 (14)	−0.0014 (14)
C12	0.0176 (15)	0.0245 (19)	0.058 (3)	0.0035 (14)	−0.0155 (17)	0.0010 (18)
C13	0.0191 (18)	0.0224 (18)	0.081 (4)	0.0023 (14)	−0.018 (2)	−0.003 (2)
C14	0.0172 (16)	0.0157 (15)	0.069 (3)	0.0037 (12)	−0.0092 (17)	−0.0025 (17)
N21	0.0128 (13)	0.0180 (13)	0.0174 (16)	0.0004 (10)	0.0005 (10)	0.0028 (10)
C21	0.0179 (15)	0.0276 (18)	0.027 (2)	−0.0052 (13)	0.0014 (14)	0.0071 (14)
C22	0.0307 (19)	0.0229 (17)	0.037 (2)	−0.0041 (15)	−0.0013 (17)	0.0107 (16)
N31	0.0092 (12)	0.0165 (13)	0.0162 (14)	0.0003 (10)	0.0006 (10)	0.0003 (9)
C31	0.0162 (14)	0.0232 (16)	0.0199 (18)	0.0004 (12)	−0.0038 (13)	0.0023 (12)
C32	0.0266 (17)	0.0265 (16)	0.0133 (17)	−0.0002 (13)	−0.0041 (13)	−0.0006 (12)
N41	0.0131 (12)	0.0169 (13)	0.0203 (17)	0.0001 (10)	−0.0031 (11)	−0.0012 (11)
C41	0.0131 (12)	0.0169 (13)	0.0203 (17)	0.0001 (10)	−0.0031 (11)	−0.0012 (11)

Geometric parameters (Å, º) top

Zn1—N1	1.985 (5)	C11—C12	1.392 (5)
Zn1—O1	1.997 (3)	C11—H11	0.9500
Zn1—N2	2.015 (4)	C12—C13	1.363 (5)
Zn1—N11ⁱ	2.214 (3)	C12—H12	0.9500
Zn1—N11	2.214 (3)	C13—C14	1.402 (5)
Zn2—N3	2.092 (3)	C13—H13	0.9500
Zn2—O1	2.1254 (19)	C14—H14	0.9500
Zn2—N41	2.141 (3)	N21—C21	1.325 (4)
Zn2—N31	2.174 (3)	N21—N21ⁱ	1.355 (5)
Zn2—N21	2.227 (3)	C21—C22	1.398 (5)
Zn2—N12	2.247 (3)	C21—H21	0.9500
O1—Zn2ⁱ	2.1254 (19)	C22—C22ⁱ	1.355 (8)
O1—H1	0.75 (10)	C22—H22	0.9500
Se1—C1	1.777 (5)	N31—C31	1.330 (4)
C1—N1	1.161 (7)	N31—N31ⁱ	1.358 (5)
Se2—C2	1.784 (5)	C31—C32	1.400 (5)
C2—N2	1.140 (7)	C31—H31	0.9500
Se3—C3	1.797 (4)	C32—C32ⁱ	1.363 (7)
C3—N3	1.157 (5)	C32—H32	0.9500
N11—C14	1.330 (4)	N41—C41ⁱⁱ	1.159 (6)
N11—N12	1.335 (4)	N41—N41ⁱⁱ	1.159 (6)
N12—C11	1.331 (4)

N1—Zn1—O1	113.64 (18)	C14—N11—Zn1	122.1 (2)
N1—Zn1—N2	115.5 (2)	N12—N11—Zn1	116.09 (19)
O1—Zn1—N2	130.90 (17)	C11—N12—N11	119.1 (3)
N1—Zn1—N11ⁱ	89.03 (9)	C11—N12—Zn2	123.8 (2)
O1—Zn1—N11ⁱ	91.19 (7)	N11—N12—Zn2	114.92 (19)
N2—Zn1—N11ⁱ	89.64 (7)	N12—C11—C12	123.0 (3)
N1—Zn1—N11	89.03 (9)	N12—C11—H11	118.5
O1—Zn1—N11	91.19 (7)	C12—C11—H11	118.5
N2—Zn1—N11	89.64 (7)	C13—C12—C11	118.0 (3)
N11ⁱ—Zn1—N11	177.39 (16)	C13—C12—H12	121.0
N3—Zn2—O1	93.64 (12)	C11—C12—H12	121.0
N3—Zn2—N41	89.99 (12)	C12—C13—C14	117.0 (3)
O1—Zn2—N41	176.37 (13)	C12—C13—H13	121.5
N3—Zn2—N31	176.69 (11)	C14—C13—H13	121.5
O1—Zn2—N31	83.09 (12)	N11—C14—C13	122.6 (3)
N41—Zn2—N31	93.28 (11)	N11—C14—H14	118.7
N3—Zn2—N21	92.62 (11)	C13—C14—H14	118.7
O1—Zn2—N21	89.28 (10)	C21—N21—N21ⁱ	119.2 (2)
N41—Zn2—N21	90.67 (11)	C21—N21—Zn2	122.7 (2)
N31—Zn2—N21	86.85 (10)	N21ⁱ—N21—Zn2	118.03 (7)
N3—Zn2—N12	86.05 (11)	N21—C21—C22	123.2 (3)
O1—Zn2—N12	91.18 (10)	N21—C21—H21	118.4
N41—Zn2—N12	88.96 (11)	C22—C21—H21	118.4
N31—Zn2—N12	94.50 (10)	C22ⁱ—C22—C21	117.6 (2)
N21—Zn2—N12	178.62 (10)	C22ⁱ—C22—H22	121.2
Zn1—O1—Zn2	113.35 (11)	C21—C22—H22	121.2
Zn1—O1—Zn2ⁱ	113.35 (11)	C31—N31—N31ⁱ	119.55 (18)
Zn2—O1—Zn2ⁱ	108.42 (14)	C31—N31—Zn2	121.7 (2)
Zn1—O1—H1	110 (6)	N31ⁱ—N31—Zn2	118.72 (7)
Zn2—O1—H1	106 (3)	N31—C31—C32	122.6 (3)
Zn2ⁱ—O1—H1	106 (3)	N31—C31—H31	118.7
N1—C1—Se1	177.7 (5)	C32—C31—H31	118.7
C1—N1—Zn1	175.6 (5)	C32ⁱ—C32—C31	117.84 (19)
N2—C2—Se2	179.4 (4)	C32ⁱ—C32—H32	121.1
C2—N2—Zn1	175.3 (4)	C31—C32—H32	121.1
N3—C3—Se3	178.2 (3)	C41ⁱⁱ—N41—N41ⁱⁱ	0.0 (4)
C3—N3—Zn2	165.6 (3)	C41ⁱⁱ—N41—Zn2	163.36 (12)
C14—N11—N12	120.3 (3)	N41ⁱⁱ—N41—Zn2	163.36 (12)

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

Experimental details

Crystal data
Chemical formula	[Zn₃(CNSe)₄(OH)(CN)(C₄H₄N₂)₄]
M_r	979.43
Crystal system, space group	Orthorhombic, Ama2
Temperature (K)	170
a, b, c (Å)	15.6156 (12), 22.6489 (16), 8.6626 (5)
V (Å³)	3063.8 (4)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	7.12
Crystal size (mm)	0.16 × 0.12 × 0.06

Data collection
Diffractometer	STOE IPDS1
Absorption correction	Numerical (X-SHAPE and X-RED32 ;Stoe, 2008)
T_min, T_max	0.196, 0.503
No. of measured, independent and observed [I > 2σ(I)] reflections	22283, 3752, 3588
R_int	0.049
(sin θ/λ)_max (Å⁻¹)	0.663

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.024, 0.058, 1.03
No. of reflections	3752
No. of parameters	206
No. of restraints	1
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.42, −0.65
Absolute structure	Flack (1983), 1747 Friedel pairs
Absolute structure parameter	−0.012 (10)

Computer programs: X-AREA (Stoe, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2010), XCIF in SHELXTL (Sheldrick, 2008).

Selected geometric parameters (Å, º) top

Zn1—N1	1.985 (5)	Zn2—O1	2.1254 (19)
Zn1—O1	1.997 (3)	Zn2—N41	2.141 (3)
Zn1—N2	2.015 (4)	Zn2—N31	2.174 (3)
Zn1—N11	2.214 (3)	Zn2—N21	2.227 (3)
Zn2—N3	2.092 (3)	Zn2—N12	2.247 (3)

N1—Zn1—O1	113.64 (18)	N3—Zn2—N21	92.62 (11)
N1—Zn1—N2	115.5 (2)	O1—Zn2—N21	89.28 (10)
O1—Zn1—N2	130.90 (17)	N41—Zn2—N21	90.67 (11)
N1—Zn1—N11ⁱ	89.03 (9)	N31—Zn2—N21	86.85 (10)
O1—Zn1—N11ⁱ	91.19 (7)	N3—Zn2—N12	86.05 (11)
N2—Zn1—N11ⁱ	89.64 (7)	O1—Zn2—N12	91.18 (10)
N1—Zn1—N11	89.03 (9)	N41—Zn2—N12	88.96 (11)
O1—Zn1—N11	91.19 (7)	N31—Zn2—N12	94.50 (10)
N2—Zn1—N11	89.64 (7)	N21—Zn2—N12	178.62 (10)
N11ⁱ—Zn1—N11	177.39 (16)	Zn1—O1—Zn2	113.35 (11)
N3—Zn2—O1	93.64 (12)	Zn1—O1—Zn2ⁱ	113.35 (11)
N3—Zn2—N41	89.99 (12)	Zn2—O1—Zn2ⁱ	108.42 (14)
O1—Zn2—N41	176.37 (13)	C21—N21—Zn2	122.7 (2)
N3—Zn2—N31	176.69 (11)	C31—N31—Zn2	121.7 (2)
O1—Zn2—N31	83.09 (12)	N41ⁱⁱ—N41—Zn2	163.36 (12)
N41—Zn2—N31	93.28 (11)

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

Acknowledgements

We gratefully acknowledge financial support by the State of Schleswig-Holstein and the Deutsche Forschungsgemeinschaft (Project 720/3–1). We thank Professor Dr Wolfgang Bensch for access to his experimental facility.

References

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