Nitro-syltris(pyridine-2-thiol-ato-κN,S)molybdenum(II) dihydrate.

In the title compound, [Mo(C(5)H(4)NS)(3)(NO)]·2H(2)O, the Mo atom is coordinated by a nitrosyl ligand and three monoanionic N,S-bidentate ligands in a distorted MoN(4)S(3) penta-gonal-bipyramidal mol-ecular geometry. The pyridine N atom of one pyridine-2-thiol-ate (pyt) ligand is coordinated to the Mo atom in the trans position relative to the NO ligand [N(pyt)-Mo-N(NO) = 170.62 (19)°]. The compound has C(s) symmetry, with a mirror plane that includes one pyt ring and the NO group. The S-Mo-N(NO) and N(pyt)-Mo-N(NO) angles [97.24 (12) and 91.87 (8)°, respectively] are large relative to the ideal angles of 90°. In the crystal, the mol-ecules pack in a zigzag arrangement. The cavities between the mol-ecules are occupied by disordered water mol-ecules of crystallization.

Related literature

For the synthesis and chemistry of similar nitrosyl, pyridine­thilato, or pyrimidine­thiol­ato derivative complexes, see: Halpenny & Mascharak (2009 ▶); Rose et al. (2007 ▶); Cini et al. (2003 ▶); Maurya et al. (2006 ▶); Kunkely & Vogler (2003 ▶); Ford et al. (1998 ▶); Proust et al. (1994 ▶); Ardon & Cohen (1993 ▶); Calderon et al. (1969 ▶); Yonemura et al. (2006 ▶, 2001 ▶); Bucher et al. (2008 ▶).

Experimental

Crystal data

[Mo(C5H4NS)3(NO)]·2H2O

M = 492.44

Orthorhombic,

a = 15.7519 (16) Å

b = 14.8889 (14) Å

c = 9.0535 (12) Å

V = 2123.3 (4) Å3

Z = 4

Mo Kα radiation

μ = 0.93 mm−1

T = 296 K

0.45 × 0.40 × 0.25 mm

Data collection

Rigaku AFC-7S diffractometer

Absorption correction: ψ scan (North et al., 1968 ▶) T min = 0.727, T max = 0.792

3681 measured reflections

2540 independent reflections

2088 reflections with I > 2σ(I)

R int = 0.023

3 standard reflections every 150 reflections intensity decay: 1.3%

Refinement

R[F 2 > 2σ(F 2)] = 0.039

wR(F 2) = 0.126

S = 1.13

2540 reflections

144 parameters

H-atom parameters constrained

Δρmax = 1.14 e Å−3

Δρmin = −0.64 e Å−3

Data collection: WinAFC (Rigaku/MSC, 2000 ▶); cell refinement: WinAFC; data reduction: CrystalStructure (Rigaku/MSC, 2007 ▶); 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, 1997 ▶); software used to prepare material for publication: CrystalStructure.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809043712/su2152sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809043712/su2152Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Mo(C5H4NS)3(NO)]·2H2O	F(000) = 992.00
Mr = 492.44	Dx = 1.540 Mg m−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ac 2n	Cell parameters from 25 reflections
a = 15.7519 (16) Å	θ = 15.4–17.4°
b = 14.8889 (14) Å	µ = 0.93 mm−1
c = 9.0535 (12) Å	T = 296 K
V = 2123.3 (4) Å3	Prismatic, orange
Z = 4	0.45 × 0.40 × 0.25 mm

Rigaku AFC-7S diffractometer	Rint = 0.023
ω–2θ scans	θmax = 27.5°
Absorption correction: ψ scan (North et al., 1968)	h = 0→20
Tmin = 0.727, Tmax = 0.792	k = −10→19
3681 measured reflections	l = −11→6
2540 independent reflections	3 standard reflections every 150 reflections
2088 reflections with F2 > 2σ(F2)	intensity decay: −1.3%

Refinement on F2	H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.039	w = 1/[σ2(Fo2) + (0.0621P)2 + 2.5132P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.126	(Δ/σ)max = 0.002
S = 1.13	Δρmax = 1.14 e Å−3
2540 reflections	Δρmin = −0.64 e Å−3
144 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008)
0 restraints	Extinction coefficient: 0.0029 (5)

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles

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).

	x	y	z	Uiso*/Ueq	Occ. (<1)
Mo1	0.17875 (3)	0.25000	0.95698 (4)	0.0359 (1)
S1	0.07755 (7)	0.15176 (7)	1.10056 (12)	0.0512 (3)
S2	0.25067 (10)	0.25000	0.71312 (17)	0.0516 (4)
O1	0.3191 (3)	0.25000	1.1749 (5)	0.0667 (14)
N1	0.0907 (3)	0.25000	0.7658 (5)	0.0427 (12)
N2	0.1905 (2)	0.1024 (2)	0.9222 (3)	0.0427 (9)
N3	0.2627 (3)	0.25000	1.0881 (5)	0.0423 (12)
C1	0.1292 (2)	0.0662 (2)	1.0080 (4)	0.0420 (10)
C2	0.1159 (3)	−0.0257 (2)	1.0145 (4)	0.0520 (12)
C3	0.1680 (3)	−0.0801 (3)	0.9319 (5)	0.0627 (14)
C4	0.2315 (3)	−0.0437 (3)	0.8467 (5)	0.0653 (16)
C5	0.2415 (2)	0.0478 (3)	0.8434 (5)	0.0560 (12)
C6	0.1452 (4)	0.25000	0.6512 (6)	0.0477 (14)
C7	0.0065 (4)	0.25000	0.7415 (8)	0.0570 (17)
C8	−0.0257 (5)	0.25000	0.5987 (9)	0.077 (3)
C9	0.0308 (6)	0.25000	0.4820 (8)	0.080 (3)
C10	0.1160 (5)	0.25000	0.5066 (7)	0.066 (2)
O21	−0.0333 (11)	0.4696 (10)	0.609 (2)	0.258 (12)	0.500
O22	0.0678 (7)	0.5119 (9)	0.5891 (12)	0.128 (5)	0.500
H1	0.07300	−0.04980	1.07300	0.0630*
H2	0.16030	−0.14210	0.93360	0.0750*
H3	0.26730	−0.08070	0.79200	0.0780*
H4	0.28430	0.07260	0.78550	0.0670*
H5	−0.03070	0.25000	0.82130	0.0690*
H6	−0.08390	0.25000	0.58200	0.0920*
H7	0.01040	0.25000	0.38570	0.0960*
H8	0.15400	0.25000	0.42800	0.0790*
H9	−0.01120	0.48460	0.54280	0.3170*	0.500
H10	−0.05690	0.48240	0.65730	0.3170*	0.500
H11	0.02840	0.51090	0.60270	0.1900*	0.500
H12	0.08240	0.49480	0.49830	0.1900*	0.500

	U11	U22	U33	U12	U13	U23
Mo1	0.0365 (2)	0.0382 (2)	0.0330 (2)	0.0000	0.0017 (2)	0.0000
S1	0.0579 (5)	0.0446 (5)	0.0510 (5)	−0.0049 (4)	0.0178 (4)	−0.0019 (4)
S2	0.0495 (7)	0.0588 (8)	0.0464 (7)	0.0000	0.0145 (6)	0.0000
O1	0.066 (2)	0.074 (3)	0.060 (2)	0.0000	−0.025 (2)	0.0000
N1	0.045 (2)	0.049 (2)	0.034 (2)	0.0000	−0.0012 (18)	0.0000
N2	0.0440 (16)	0.0440 (17)	0.0401 (15)	0.0014 (13)	0.0003 (12)	−0.0030 (13)
N3	0.044 (2)	0.042 (2)	0.041 (2)	0.0000	−0.0001 (19)	0.0000
C1	0.0457 (19)	0.0416 (18)	0.0387 (17)	0.0002 (15)	−0.0037 (15)	−0.0016 (14)
C2	0.063 (2)	0.044 (2)	0.049 (2)	−0.0051 (19)	−0.0008 (19)	0.0026 (17)
C3	0.085 (3)	0.039 (2)	0.064 (2)	0.004 (2)	−0.011 (2)	−0.0020 (19)
C4	0.072 (3)	0.051 (2)	0.073 (3)	0.017 (2)	0.007 (2)	−0.008 (2)
C5	0.054 (2)	0.056 (2)	0.058 (2)	0.0076 (19)	0.0063 (19)	−0.004 (2)
C6	0.057 (3)	0.047 (2)	0.039 (2)	0.0000	0.005 (2)	0.0000
C7	0.047 (3)	0.068 (3)	0.056 (3)	0.0000	−0.003 (2)	0.0000
C8	0.070 (4)	0.099 (6)	0.061 (4)	0.0000	−0.023 (3)	0.0000
C9	0.095 (6)	0.103 (6)	0.043 (3)	0.0000	−0.019 (3)	0.0000
C10	0.084 (5)	0.079 (4)	0.034 (2)	0.0000	0.006 (3)	0.0000
O21	0.213 (18)	0.132 (13)	0.43 (3)	0.100 (12)	−0.21 (2)	−0.171 (17)
O22	0.104 (7)	0.164 (11)	0.117 (7)	0.009 (7)	−0.024 (6)	0.001 (8)

Mo1—S1	2.5240 (12)	N2—C5	1.347 (5)
Mo1—S2	2.4815 (16)	C1—C2	1.386 (4)
Mo1—N1	2.218 (5)	C2—C3	1.374 (6)
Mo1—N2	2.228 (3)	C3—C4	1.375 (7)
Mo1—N3	1.777 (5)	C4—C5	1.372 (6)
Mo1—S1i	2.5240 (12)	C6—C10	1.388 (9)
Mo1—N2i	2.228 (3)	C7—C8	1.389 (11)
S1—C1	1.728 (3)	C8—C9	1.381 (12)
S2—C6	1.753 (6)	C9—C10	1.360 (12)
O1—N3	1.186 (7)	C2—H1	0.9300
O21—O22	1.72 (2)	C3—H2	0.9300
O21—H10	0.6000	C4—H3	0.9300
O21—H9	0.7300	C5—H4	0.9300
O22—H12	0.8900	C7—H5	0.9300
O22—H11	0.6300	C8—H6	0.9300
N1—C6	1.347 (7)	C9—H7	0.9300
N1—C7	1.344 (8)	C10—H8	0.9300
N2—C1	1.351 (4)
S1—Mo1—S2	138.29 (3)	Mo1—N3—O1	179.6 (4)
S1—Mo1—N1	90.40 (10)	N2—C1—C2	121.8 (3)
S1—Mo1—N2	63.49 (8)	S1—C1—N2	108.7 (2)
S1—Mo1—N3	97.24 (12)	S1—C1—C2	129.5 (3)
S1—Mo1—S1i	70.83 (4)	C1—C2—C3	118.0 (4)
S1—Mo1—N2i	134.18 (8)	C2—C3—C4	120.5 (4)
S2—Mo1—N1	65.87 (13)	C3—C4—C5	119.2 (4)
S2—Mo1—N2	80.58 (7)	N2—C5—C4	121.3 (4)
S2—Mo1—N3	104.75 (15)	N1—C6—C10	121.0 (6)
S1i—Mo1—S2	138.29 (3)	S2—C6—N1	111.0 (4)
S2—Mo1—N2i	80.58 (7)	S2—C6—C10	128.0 (5)
N1—Mo1—N2	86.66 (8)	N1—C7—C8	120.8 (6)
N1—Mo1—N3	170.62 (19)	C7—C8—C9	118.5 (7)
S1i—Mo1—N1	90.40 (10)	C8—C9—C10	120.7 (7)
N1—Mo1—N2i	86.66 (8)	C6—C10—C9	118.8 (6)
N2—Mo1—N3	91.87 (8)	C1—C2—H1	121.00
S1i—Mo1—N2	134.18 (8)	C3—C2—H1	121.00
N2—Mo1—N2i	161.13 (11)	C2—C3—H2	120.00
S1i—Mo1—N3	97.24 (12)	C4—C3—H2	120.00
N2i—Mo1—N3	91.87 (8)	C5—C4—H3	120.00
S1i—Mo1—N2i	63.49 (8)	C3—C4—H3	120.00
Mo1—S1—C1	83.12 (11)	N2—C5—H4	119.00
Mo1—S2—C6	81.48 (19)	C4—C5—H4	119.00
H9—O21—H10	142.00	N1—C7—H5	120.00
H11—O22—H12	115.00	C8—C7—H5	120.00
Mo1—N1—C6	101.7 (4)	C7—C8—H6	121.00
C6—N1—C7	120.2 (5)	C9—C8—H6	121.00
Mo1—N1—C7	138.1 (4)	C8—C9—H7	120.00
Mo1—N2—C5	136.0 (3)	C10—C9—H7	120.00
C1—N2—C5	119.3 (3)	C9—C10—H8	121.00
Mo1—N2—C1	104.6 (2)	C6—C10—H8	121.00
S2—Mo1—S1—C1	32.54 (14)	Mo1—S1—C1—N2	1.4 (2)
N1—Mo1—S1—C1	85.19 (14)	Mo1—S1—C1—C2	−179.6 (4)
N2—Mo1—S1—C1	−0.87 (14)	Mo1—S2—C6—N1	0.00
N3—Mo1—S1—C1	−89.34 (15)	Mo1—S2—C6—C10	180.00
S1i—Mo1—S1—C1	175.48 (12)	Mo1—N1—C6—S2	0.00
N2i—Mo1—S1—C1	170.92 (16)	Mo1—N1—C6—C10	180.00
S1—Mo1—S2—C6	60.58 (6)	C7—N1—C6—S2	180.00
N1—Mo1—S2—C6	0.00	C7—N1—C6—C10	0.00
N2—Mo1—S2—C6	90.55 (8)	Mo1—N1—C7—C8	180.00
N3—Mo1—S2—C6	−180.00	C6—N1—C7—C8	0.00
S1—Mo1—N1—C6	−144.58 (2)	Mo1—N2—C1—S1	−1.6 (3)
S1—Mo1—N1—C7	35.42 (2)	Mo1—N2—C1—C2	179.3 (3)
S2—Mo1—N1—C6	0.00	C5—N2—C1—S1	177.5 (3)
S2—Mo1—N1—C7	180.00	C5—N2—C1—C2	−1.6 (5)
N2—Mo1—N1—C6	−81.17 (8)	Mo1—N2—C5—C4	179.9 (3)
N2—Mo1—N1—C7	98.83 (8)	C1—N2—C5—C4	1.1 (6)
S1—Mo1—N2—C1	1.14 (19)	S1—C1—C2—C3	−178.1 (3)
S1—Mo1—N2—C5	−177.8 (4)	N2—C1—C2—C3	0.8 (6)
S2—Mo1—N2—C1	−157.1 (2)	C1—C2—C3—C4	0.4 (6)
S2—Mo1—N2—C5	24.1 (3)	C2—C3—C4—C5	−0.9 (7)
N1—Mo1—N2—C1	−91.0 (2)	C3—C4—C5—N2	0.2 (7)
N1—Mo1—N2—C5	90.1 (4)	S2—C6—C10—C9	180.00
N3—Mo1—N2—C1	98.3 (3)	N1—C6—C10—C9	0.00
N3—Mo1—N2—C5	−80.6 (4)	N1—C7—C8—C9	0.00
S1i—Mo1—N2—C1	−3.7 (3)	C7—C8—C9—C10	0.00
S1i—Mo1—N2—C5	177.4 (3)	C8—C9—C10—C6	0.00

D—H···A	D—H	H···A	D···A	D—H···A
O21—H9···O22	0.73	1.37	1.72 (2)	106
C5—H4···S2	0.93	2.77	3.237 (5)	112

Mo1—S1	2.5240 (12)
Mo1—S2	2.4815 (16)
Mo1—N1	2.218 (5)
Mo1—N2	2.228 (3)
Mo1—N3	1.777 (5)

S1—Mo1—S2	138.29 (3)
S1—Mo1—N1	90.40 (10)
S1—Mo1—N3	97.24 (12)
S2—Mo1—N2	80.58 (7)
S1i—Mo1—S2	138.29 (3)
N1—Mo1—N2	86.66 (8)
N1—Mo1—N3	170.62 (19)
N2—Mo1—N3	91.87 (8)

Symmetry code: (i) .