catena-Poly[[diaqua­zinc(II)]-μ-l-cystein­ato(2−)-κ4S:S,N,O-[di-μ-sulfido-bis­[oxido­molybdate(V)](Mo—Mo)]-μ-l-cysteinato(2−)-κ4S,N,O:S]

Shibahara, T.; Ogasahara, S.; Sakane, G.

doi:10.1107/S1600536808007757

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 5| May 2008| Pages m605-m606

doi:10.1107/S1600536808007757

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catena-Poly[[diaquazinc(II)]-μ-L-cysteinato(2−)-κ⁴S:S,N,O-[di-μ-sulfido-bis[oxidomolybdate(V)](Mo—Mo)]-μ-L-cysteinato(2−)-κ⁴S,N,O:S]

Takashi Shibahara,^a ^* Shinobu Ogasahara ^a and Genta Sakane ^a

^aDepartment of Chemistry, Okayama University of Science, Ridai-cho, Okayama 700-0005, Japan
^*Correspondence e-mail: shiba@chem.ous.ac.jp

(Received 6 March 2008; accepted 21 March 2008; online 2 April 2008)

The title compound, [Mo₂Zn(C₃H₅NO₂S)₂O₂S₂(H₂O)₂], forms a one-dimensional chain. The cysteine S atom of the dinuclear molybdenum complex anion coordinates to the zinc ion, which has a tetrahedral environment by the additional coordination of two water molecules. The one-dimensional chains are connected to each other by hydrogen bonds. The Zn—S(cysteine) distances [2.3599 (6) and 2.3072 (6) Å] are close to the value in ZnS (2.35 Å). The distances and angles within the complex are very close to those reported for the sodium and potassium di-μ-sulfide species.

Related literature

For related literature, see: Brown & Jeffreys (1973 ); Hong et al. (1983 ); Kay & Mitchell (1970 ); Knox & Prout (1969 ); Shibahara et al. (1987 ); Lee et al. (1989 ); Liu & Williams (1981 ); Xing et al. (1998 ).

Experimental

Crystal data

[Mo₂Zn(C₃H₅NO₂S)₂O₂S₂(H₂O)₂]
M_r = 627.69
Monoclinic, P 2₁
a = 8.6881 (11) Å
b = 10.3529 (8) Å
c = 9.8686 (11) Å
β = 108.2022 (14)°
V = 843.23 (16) Å³
Z = 2
Mo Kα radiation
μ = 3.40 mm⁻¹
T = 93.1 K
0.35 × 0.30 × 0.10 mm

Data collection

Rigaku Mercury diffractometer
Absorption correction: multi-scan (Jacobson, 1998 ) T_min = 0.382, T_max = 0.727
9357 measured reflections
4556 independent reflections
4549 reflections with F² > 2σ(F²)
R_int = 0.019

Refinement

R[F² > 2σ(F²)] = 0.019
wR(F²) = 0.049
S = 1.02
4556 reflections
209 parameters
15 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.47 e Å⁻³
Δρ_min = −0.94 e Å⁻³
Absolute structure: Flack (1983 ), with 2010 Friedel pairs
Flack parameter: 0.002 (7)

Table 1
Selected geometric parameters (Å, °)

Mo1—S1	2.3201 (6)
Mo1—S2	2.3378 (6)
Mo1—S3	2.5572 (6)
Mo1—Mo2	2.8354 (3)
Mo2—S2	2.3276 (6)
Mo2—S1	2.3368 (6)
Mo2—S4	2.5428 (6)
Zn1—O8	2.0052 (17)
Zn1—O7	2.0275 (19)
Zn1—S4ⁱ	2.3072 (6)
Zn1—S3	2.3599 (6)

O8—Zn1—O7	96.70 (7)
O8—Zn1—S4ⁱ	129.42 (5)
O7—Zn1—S4ⁱ	107.94 (6)
O8—Zn1—S3	93.73 (5)
O7—Zn1—S3	104.55 (6)
S4ⁱ—Zn1—S3	120.25 (2)
Symmetry code: (i) x-1, y, z.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H11⋯O3ⁱⁱ	0.84	2.03	2.832 (2)	161
O8—H13⋯O5ⁱⁱ	0.84	1.77	2.604 (2)	171
O8—H14⋯O4ⁱ	0.84	2.00	2.789 (2)	158
Symmetry codes: (i) x-1, y, z; (ii) $[-x, y+{\script{1\over 2}}, -z+2]$ .

Data collection: CrystalClear (Rigaku, 1999 ); cell refinement: CrystalClear; data reduction: CrystalStructure (Rigaku, 2007 ); program(s) used to solve structure: SIR97 (Altomare et al., 1999 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ); molecular graphics: CrystalStructure; software used to prepare material for publication: CrystalStructure.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808007757/wk2080sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808007757/wk2080Isup2.hkl

checkCIF report

Comment top

Molybdenum and L-cysteine are important components of many enzymes. X-ray structures of sulfur/oxygen-bridged dinuclear molybdenum complexes with L-cysteine ligands: Na₂[Mo₂(µ-S)₂O₂(cys)₂].4H₂O (Brown & Jeffreys, 1973; Hong et al., 1983); K₂[Mo₂S₂O₂(cys)₂].4H₂O.CH₃OH (Xing et al., 1998), Ca[Mo₂(µ-S)(µ-O)O₂(cys)₂].3H₂O (Shibahara et al., 1987), and Na₂[Mo₂O₄(cys)₂].5H₂O (Knox & Prout, 1969; Kay & Mitchell, 1970; Liu & Williams, 1981), have been reported, where alkaline or alkaline earth metals are counter cations, and the existence of metal-oxygen (cysteine oxygen) bonds has been reported. Seeking another crystal structure type, we used Zn²⁺ion, as the counter ion. The present structural study of the complex compound Zn[Mo₂O₂S₂(cys)₂].2H₂O (I) reveals the existence of Zn—S(cysteine sulfur) bonds, which result in polymerization; this type of Zn—S bond has been found in zinc finger proteins. The asymmetric unit of I is shown in Fig. 1 and a view of part of a one-dimensional polymeric chain of I is shown in Fig. 2. The zinc ion bridges the molybdenum complex anions: the coordination of the cysteine sulfur in the complex anion to the zinc ion results in the formation of one dimensional chains, where the zinc forms a tetrahedral structure by the additional coordination of two water molecules. The one dimensional chains are connected to each other by hydrogen bonds. Intra-chain hydrogen bonds also exist. The dimensions of the molybdenum complex and of the zinc tetrahedron are listed in Table 1, and the hydrogen bonds are listed in Table 2. The Zn—S(cysteine) distances (2.3599 (6), 2.3072 (6) Å) are close to that in ZnS (2.35 Å). The distances and angles within the complex are very close to those reported in the sodium and potassium salts in the di-µ-sulfide species.

Related literature top

For related literature, see: Brown & Jeffreys (1973); Hong et al. (1983); Kay & Mitchell (1970); Knox & Prout (1969); Shibahara et al. (1987); Lee et al. (1989); Liu & Williams (1981); Xing et al. (1998).

Experimental top

The title compound was prepared by the addition of ZnCl₂ to a diluted aqueous solution of Na₂[Mo₂O₂S₂(cys)₂].4H₂O. A crystal suitable for single-crystal X-ray diffraction was selected directly from the prepared sample.

Computing details top

Data collection: CrystalClear (Rigaku, 1999); cell refinement: CrystalClear (Rigaku, 1999); data reduction: CrystalStructure (Rigaku, 2007); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: CrystalStructure (Rigaku, 2007); software used to prepare material for publication: CrystalStructure (Rigaku, 2007).

Figures top

	Fig. 1. The asymmetric unit of I with atom labels and 50% probability displacement ellipsoids for non-H atoms.
	Fig. 2. A view of part of a one-dimensional polymeric chain with hydrogen bonds (dashed lines).

catena-Poly[[diaquazinc(II)]-µ-L-cysteinato(2-)-κ⁴S:S,N,O-[di-µ-sulfido- bis[oxidomolybdate(V)](Mo—Mo)]-µ-L-cysteinato(2-)-κ⁴S,N,O:S] top

Crystal data top

[Mo₂Zn(C₃H₅NO₂S)₂O₂S₂(H₂O)₂]	F(000) = 612.00
M_r = 627.69	D_x = 2.472 Mg m⁻³
Monoclinic, P2₁	Mo Kα radiation, λ = 0.71070 Å
Hall symbol: P 2yb	Cell parameters from 3004 reflections
a = 8.6881 (11) Å	θ = 5.5–30.0°
b = 10.3529 (8) Å	µ = 3.41 mm⁻¹
c = 9.8686 (11) Å	T = 93 K
β = 108.2022 (14)°	Platelet, orange
V = 843.23 (16) Å³	0.35 × 0.30 × 0.10 mm
Z = 2

Data collection top

Rigaku Mercury diffractometer	4549 reflections with F² > 2σ(F²)
Detector resolution: 14.63 pixels mm^-1	R_int = 0.019
ω scans	θ_max = 30.0°
Absorption correction: multi-scan (Jacobson, 1998)	h = −12→11
T_min = 0.382, T_max = 0.727	k = −14→14
9357 measured reflections	l = −13→13
4556 independent reflections

Refinement top

Refinement on F²	H atoms treated by a mixture of independent and constrained refinement
R[F² > 2σ(F²)] = 0.019	w = 1/[σ²(F_o²) + (0.0303P)² + 0.5406P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.049	(Δ/σ)_max = 0.001
S = 1.02	Δρ_max = 0.47 e Å⁻³
4556 reflections	Δρ_min = −0.94 e Å⁻³
209 parameters	Absolute structure: Flack (1983), with 2010 Friedel pairs
15 restraints	Absolute structure parameter: 0.002 (7)

Crystal data top

[Mo₂Zn(C₃H₅NO₂S)₂O₂S₂(H₂O)₂]	V = 843.23 (16) Å³
M_r = 627.69	Z = 2
Monoclinic, P2₁	Mo Kα radiation
a = 8.6881 (11) Å	µ = 3.41 mm⁻¹
b = 10.3529 (8) Å	T = 93 K
c = 9.8686 (11) Å	0.35 × 0.30 × 0.10 mm
β = 108.2022 (14)°

Data collection top

Rigaku Mercury diffractometer	4556 independent reflections
Absorption correction: multi-scan (Jacobson, 1998)	4549 reflections with F² > 2σ(F²)
T_min = 0.382, T_max = 0.727	R_int = 0.019
9357 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.019	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.049	Δρ_max = 0.47 e Å⁻³
S = 1.02	Δρ_min = −0.94 e Å⁻³
4556 reflections	Absolute structure: Flack (1983), with 2010 Friedel pairs
209 parameters	Absolute structure parameter: 0.002 (7)
15 restraints

Special details top

Geometry. ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY

Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F². R-factor (gt) are based on F. The threshold expression of F² > 2.0 σ>F²) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Mo1	−0.056910 (19)	0.591229 (16)	0.808774 (16)	0.00615 (4)
Mo2	0.113206 (19)	0.533750 (19)	0.613333 (16)	0.00647 (4)
Zn1	−0.46728 (3)	0.59442 (3)	0.84366 (3)	0.01008 (4)
S1	−0.07812 (7)	0.40574 (6)	0.67221 (6)	0.00917 (8)
S2	0.16158 (6)	0.70395 (5)	0.77534 (6)	0.00880 (8)
S3	−0.22984 (6)	0.46976 (5)	0.93439 (5)	0.00813 (8)
S4	0.39318 (6)	0.59322 (6)	0.60271 (5)	0.01009 (8)
O1	−0.2167 (2)	0.68209 (17)	0.71583 (17)	0.0104 (2)
O2	0.00101 (19)	0.60344 (18)	0.45909 (16)	0.0111 (2)
O3	0.2203 (2)	0.45050 (18)	1.21945 (17)	0.0125 (3)
O4	0.13324 (19)	0.49461 (16)	0.98677 (16)	0.0089 (2)
O5	0.4690 (2)	0.2383 (2)	0.7999 (2)	0.0217 (3)
O6	0.2865 (2)	0.39663 (18)	0.77426 (17)	0.0125 (3)
O7	−0.3954 (2)	0.77830 (18)	0.9006 (2)	0.0182 (3)
O8	−0.54704 (19)	0.55572 (18)	1.00931 (17)	0.0136 (3)
N1	−0.0163 (2)	0.70357 (19)	1.01408 (19)	0.0087 (3)
N2	0.1744 (2)	0.3658 (2)	0.4962 (2)	0.0102 (3)
C1	0.0084 (2)	0.6095 (2)	1.1320 (2)	0.0092 (3)
C2	0.1322 (2)	0.5110 (2)	1.1161 (2)	0.0083 (3)
C3	−0.1525 (2)	0.5421 (2)	1.1147 (2)	0.0099 (3)
C4	0.3455 (2)	0.3284 (2)	0.5675 (2)	0.0112 (3)
C5	0.3694 (2)	0.3165 (2)	0.7269 (2)	0.0116 (4)
C6	0.4534 (2)	0.4378 (2)	0.5447 (2)	0.0130 (4)
H1	0.0683	0.7596	1.0256	0.010*
H2	−0.1027	0.7551	1.0124	0.010*
H3	0.1090	0.2957	0.4919	0.012*
H4	0.1624	0.3890	0.4039	0.012*
H5	−0.2299	0.6042	1.1334	0.012*
H6	−0.1366	0.4727	1.1869	0.012*
H7	0.0460	0.6482	1.2291	0.011*
H8	0.4318	0.4416	0.4403	0.016*
H9	0.5706	0.4243	0.5928	0.016*
H10	0.3821	0.2458	0.5359	0.013*
H11	−0.3638	0.8290	0.8487	0.022*
H12	−0.4303	0.8035	0.9659	0.022*
H13	−0.5293	0.6197	1.0646	0.016*
H14	−0.6424	0.5281	0.9816	0.016*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.00760 (7)	0.00633 (8)	0.00567 (7)	0.00053 (6)	0.00374 (5)	0.00047 (6)
Mo2	0.00756 (7)	0.00729 (8)	0.00565 (7)	0.00067 (6)	0.00364 (5)	0.00022 (6)
Zn1	0.01030 (10)	0.01118 (12)	0.00928 (10)	0.00082 (10)	0.00382 (8)	−0.00105 (9)
S1	0.0114 (2)	0.0085 (2)	0.0091 (2)	−0.00148 (18)	0.00549 (17)	−0.00119 (17)
S2	0.0109 (2)	0.0077 (2)	0.0098 (2)	−0.00074 (18)	0.00601 (17)	−0.00107 (17)
S3	0.0087 (2)	0.0085 (2)	0.0086 (2)	−0.00003 (18)	0.00480 (16)	−0.00014 (17)
S4	0.0088 (2)	0.0127 (2)	0.0098 (2)	−0.0003 (2)	0.00436 (16)	0.00152 (19)
O1	0.0111 (6)	0.0117 (8)	0.0102 (6)	0.0024 (5)	0.0060 (5)	0.0015 (5)
O2	0.0113 (6)	0.0135 (8)	0.0097 (6)	0.0019 (6)	0.0048 (5)	0.0014 (6)
O3	0.0152 (7)	0.0123 (8)	0.0101 (6)	0.0030 (6)	0.0039 (5)	0.0014 (6)
O4	0.0102 (6)	0.0099 (7)	0.0074 (6)	0.0011 (5)	0.0041 (5)	0.0002 (5)
O5	0.0216 (8)	0.0185 (9)	0.0221 (8)	0.0064 (7)	0.0027 (7)	0.0083 (7)
O6	0.0166 (7)	0.0129 (8)	0.0087 (6)	0.0010 (6)	0.0049 (5)	−0.0004 (5)
O7	0.0217 (9)	0.0131 (8)	0.0250 (8)	−0.0031 (7)	0.0146 (7)	−0.0054 (7)
O8	0.0096 (6)	0.0217 (10)	0.0103 (6)	−0.0025 (5)	0.0045 (5)	−0.0045 (6)
N1	0.0111 (7)	0.0069 (8)	0.0096 (7)	0.0002 (6)	0.0053 (6)	0.0004 (6)
N2	0.0096 (7)	0.0125 (9)	0.0084 (7)	0.0010 (6)	0.0026 (6)	−0.0032 (6)
C1	0.0131 (8)	0.0086 (10)	0.0067 (7)	0.0002 (7)	0.0043 (6)	−0.0005 (7)
C2	0.0099 (8)	0.0060 (10)	0.0107 (8)	−0.0019 (6)	0.0058 (6)	−0.0008 (6)
C3	0.0118 (8)	0.0109 (9)	0.0088 (7)	−0.0005 (7)	0.0060 (6)	0.0001 (7)
C4	0.0114 (8)	0.0130 (10)	0.0088 (8)	0.0038 (7)	0.0024 (6)	−0.0032 (7)
C5	0.0126 (9)	0.0095 (10)	0.0124 (9)	−0.0007 (7)	0.0034 (7)	0.0003 (7)
C6	0.0117 (9)	0.0186 (11)	0.0099 (8)	0.0019 (7)	0.0052 (7)	−0.0024 (8)

Geometric parameters (Å, º) top

Mo1—O1	1.6905 (17)	O5—C5	1.238 (3)
Mo1—O4	2.2366 (16)	O6—C5	1.279 (3)
Mo1—N1	2.2662 (19)	O7—H11	0.837
Mo1—S1	2.3201 (6)	O7—H12	0.835
Mo1—S2	2.3378 (6)	O8—H13	0.841
Mo1—S3	2.5572 (6)	O8—H14	0.838
Mo1—Mo2	2.8354 (3)	N1—C1	1.481 (3)
Mo2—O2	1.6914 (16)	N1—H1	0.915
Mo2—N2	2.2419 (19)	N1—H2	0.917
Mo2—O6	2.3044 (18)	N2—C4	1.484 (3)
Mo2—S2	2.3276 (6)	N2—H3	0.914
Mo2—S1	2.3368 (6)	N2—H4	0.915
Mo2—S4	2.5428 (6)	C1—C3	1.523 (3)
Zn1—O8	2.0052 (17)	C1—C2	1.526 (3)
Zn1—O7	2.0275 (19)	C1—H7	0.995
Zn1—S4ⁱ	2.3072 (6)	C3—H5	0.989
Zn1—S3	2.3599 (6)	C3—H6	0.991
S3—C3	1.852 (2)	C4—C5	1.527 (3)
S4—C6	1.838 (3)	C4—C6	1.531 (4)
S4—Zn1ⁱⁱ	2.3072 (6)	C4—H10	0.996
O3—C2	1.237 (3)	C6—H8	0.989
O4—C2	1.290 (2)	C6—H9	0.989

O1—Mo1—O4	162.73 (7)	C6—S4—Zn1ⁱⁱ	102.50 (7)
O1—Mo1—N1	94.11 (7)	C6—S4—Mo2	99.79 (8)
O4—Mo1—N1	69.93 (6)	Zn1ⁱⁱ—S4—Mo2	99.22 (2)
O1—Mo1—S1	104.04 (6)	C2—O4—Mo1	119.10 (14)
O4—Mo1—S1	89.50 (4)	C5—O6—Mo2	117.99 (14)
N1—Mo1—S1	154.97 (5)	Zn1—O7—H11	123.4
O1—Mo1—S2	102.18 (6)	Zn1—O7—H12	110.6
O4—Mo1—S2	84.32 (4)	H11—O7—H12	122.9
N1—Mo1—S2	87.91 (5)	Zn1—O8—H13	109.3
S1—Mo1—S2	104.59 (2)	Zn1—O8—H14	111.1
O1—Mo1—S3	91.69 (6)	H13—O8—H14	116.3
O4—Mo1—S3	78.52 (4)	C1—N1—Mo1	107.99 (13)
N1—Mo1—S3	76.70 (5)	C1—N1—H1	113.9
S1—Mo1—S3	85.55 (2)	Mo1—N1—H1	109.3
S2—Mo1—S3	160.022 (19)	C1—N1—H2	108.3
O1—Mo1—Mo2	105.18 (6)	Mo1—N1—H2	112.6
O4—Mo1—Mo2	91.51 (4)	H1—N1—H2	104.8
N1—Mo1—Mo2	138.35 (5)	C4—N2—Mo2	108.76 (13)
S1—Mo1—Mo2	52.760 (15)	C4—N2—H3	109.3
S2—Mo1—Mo2	52.411 (14)	Mo2—N2—H3	113.3
S3—Mo1—Mo2	137.441 (15)	C4—N2—H4	109.0
O2—Mo2—N2	91.69 (8)	Mo2—N2—H4	109.8
O2—Mo2—O6	162.14 (7)	H3—N2—H4	106.6
N2—Mo2—O6	70.64 (6)	N1—C1—C3	108.11 (17)
O2—Mo2—S2	103.00 (6)	N1—C1—C2	107.01 (16)
N2—Mo2—S2	156.97 (5)	C3—C1—C2	109.49 (18)
O6—Mo2—S2	93.10 (5)	N1—C1—H7	114.5
O2—Mo2—S1	102.18 (6)	C3—C1—H7	107.9
N2—Mo2—S1	89.44 (5)	C2—C1—H7	109.8
O6—Mo2—S1	80.89 (5)	O3—C2—O4	123.7 (2)
S2—Mo2—S1	104.38 (2)	O3—C2—C1	121.88 (18)
O2—Mo2—S4	98.59 (6)	O4—C2—C1	114.38 (18)
N2—Mo2—S4	77.44 (5)	C1—C3—S3	109.75 (13)
O6—Mo2—S4	75.53 (5)	C1—C3—H5	109.6
S2—Mo2—S4	82.83 (2)	S3—C3—H5	112.2
S1—Mo2—S4	155.71 (2)	C1—C3—H6	109.6
O2—Mo2—Mo1	104.26 (5)	S3—C3—H6	109.0
N2—Mo2—Mo1	140.49 (5)	H5—C3—H6	106.7
O6—Mo2—Mo1	91.59 (4)	N2—C4—C5	107.66 (18)
S2—Mo2—Mo1	52.737 (15)	N2—C4—C6	107.82 (19)
S1—Mo2—Mo1	52.226 (15)	C5—C4—C6	108.60 (18)
S4—Mo2—Mo1	133.300 (15)	N2—C4—H10	116.5
O8—Zn1—O7	96.70 (7)	C5—C4—H10	107.4
O8—Zn1—S4ⁱ	129.42 (5)	C6—C4—H10	108.7
O7—Zn1—S4ⁱ	107.94 (6)	O5—C5—O6	125.6 (2)
O8—Zn1—S3	93.73 (5)	O5—C5—C4	119.9 (2)
O7—Zn1—S3	104.55 (6)	O6—C5—C4	114.4 (2)
S4ⁱ—Zn1—S3	120.25 (2)	C4—C6—S4	110.80 (15)
Mo1—S1—Mo2	75.014 (19)	C4—C6—H8	104.8
Mo2—S2—Mo1	74.853 (18)	S4—C6—H8	108.1
C3—S3—Zn1	98.94 (7)	C4—C6—H9	114.2
C3—S3—Mo1	100.08 (7)	S4—C6—H9	109.0
Zn1—S3—Mo1	97.09 (2)	H8—C6—H9	109.7

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H11···O3ⁱⁱⁱ	0.84	2.03	2.832 (2)	161
O7—H11···O4ⁱⁱⁱ	0.84	2.75	3.139 (2)	110
O7—H12···O5ⁱⁱⁱ	0.84	2.53	3.239 (3)	144
O7—H12···O6ⁱⁱⁱ	0.84	2.66	3.285 (2)	133
O7—H12···O8^iv	0.84	2.64	3.093 (2)	116
O8—H13···O5ⁱⁱⁱ	0.84	1.77	2.604 (2)	171
O8—H14···O4ⁱ	0.84	2.00	2.789 (2)	158
O8—H14···O6ⁱ	0.84	2.37	2.844 (2)	116
N1—H2···O4ⁱⁱⁱ	0.92	2.49	3.179 (2)	132
N1—H2···O7	0.92	2.45	3.224 (2)	143
N2—H3···O2^v	0.91	2.32	3.212 (2)	164
N2—H4···O1^v	0.92	2.56	2.934 (2)	105
N2—H4···O3^vi	0.92	2.13	3.011 (2)	161

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

Experimental details

Crystal data
Chemical formula	[Mo₂Zn(C₃H₅NO₂S)₂O₂S₂(H₂O)₂]
M_r	627.69
Crystal system, space group	Monoclinic, P2₁
Temperature (K)	93
a, b, c (Å)	8.6881 (11), 10.3529 (8), 9.8686 (11)
β (°)	108.2022 (14)
V (Å³)	843.23 (16)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	3.41
Crystal size (mm)	0.35 × 0.30 × 0.10

Data collection
Diffractometer	Rigaku Mercury diffractometer
Absorption correction	Multi-scan (Jacobson, 1998)
T_min, T_max	0.382, 0.727
No. of measured, independent and observed [F² > 2σ(F²)] reflections	9357, 4556, 4549
R_int	0.019
(sin θ/λ)_max (Å⁻¹)	0.704

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.019, 0.049, 1.02
No. of reflections	4556
No. of parameters	209
No. of restraints	15
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.47, −0.94
Absolute structure	Flack (1983), with 2010 Friedel pairs
Absolute structure parameter	0.002 (7)

Computer programs: CrystalClear (Rigaku, 1999), CrystalStructure (Rigaku, 2007), SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 2008), CrystalStructure (Rigaku, 2007).

Selected geometric parameters (Å, º) top

Mo1—S1	2.3201 (6)	Mo2—S4	2.5428 (6)
Mo1—S2	2.3378 (6)	Zn1—O8	2.0052 (17)
Mo1—S3	2.5572 (6)	Zn1—O7	2.0275 (19)
Mo1—Mo2	2.8354 (3)	Zn1—S4ⁱ	2.3072 (6)
Mo2—S2	2.3276 (6)	Zn1—S3	2.3599 (6)
Mo2—S1	2.3368 (6)

O8—Zn1—O7	96.70 (7)	O8—Zn1—S3	93.73 (5)
O8—Zn1—S4ⁱ	129.42 (5)	O7—Zn1—S3	104.55 (6)
O7—Zn1—S4ⁱ	107.94 (6)	S4ⁱ—Zn1—S3	120.25 (2)

Symmetry code: (i) x−1, y, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H11···O3ⁱⁱ	0.837	2.028	2.832 (2)	160.9
O8—H13···O5ⁱⁱ	0.841	1.770	2.604 (2)	170.9
O8—H14···O4ⁱ	0.838	1.996	2.789 (2)	157.7

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

Acknowledgements

This work was partly supported by a Special Grant for Cooperative Research administered by the Japan Private School Promotion Foundation.

References

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