Manganese mercury thio­cyanate (MMTC) glycol mono­methyl ether

In the title complex, [MnHg(NCS)₄(C₃H₈O₂)]_n, each Hg atom is tetrahedrally coordinated with four S atoms of the SCN^- ions, and each Mn atom is octahedrally coordinated with four N atoms of the SCN^- ions, one hydroxyl O atom and one ethereal O atom of the glycol mono­methyl ether mol­ecule. Each pair of Hg and Mn atoms is bridged by one SCN^- ion. A 24-membered Mn₃Hg₃(SCN)₆ ring is formed as the strucrural unit, with the six metal atoms in a chair-form hexagonal arrangement. The units are condensed and linked three-dimensionally in the crystal resulting in a diamond-like structure.

Computing details

Data collection: XSCANS (Bruker 1996); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXTL (Bruker, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL.

(I)

Crystal data

[MnHg(NCS)4(C3H8O2)]	Dx = 2.345 Mg m^−3
Mr = 563.94	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pca21	Cell parameters from 36 reflections
a = 16.2046 (16) Å	θ = 4.8–14.8°
b = 7.2974 (5) Å	µ = 10.91 mm^−1
c = 13.5090 (14) Å	T = 293 K
V = 1597.5 (3) Å^3	Prism, pale green
Z = 4	0.25 × 0.20 × 0.18 mm
F(000) = 1052

Data collection

Bruker P4 diffractometer	1779 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.047
Graphite monochromator	θmax = 28.0°, θmin = 2.5°
ω/2θ scans	h = −21→1
Absorption correction: ψ scans (XSCANS; Siemens, 1996)	k = −1→9
Tmin = 0.076, Tmax = 0.140	l = −17→1
2634 measured reflections	3 standard reflections every 97 reflections
2149 independent reflections	intensity decay: none

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.040	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.101	w = 1/[σ^2(Fo^2) + (0.059P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.04	(Δ/σ)max = 0.001
2149 reflections	Δρmax = 1.92 e Å^−3
173 parameters	Δρmin = −0.95 e Å^−3
1 restraint	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0044 (4)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Hg1	0.74555 (2)	0.36055 (6)	0.27674 (5)	0.05205 (18)
Mn1	0.46540 (10)	0.1386 (2)	0.5205 (2)	0.0401 (4)
S1	0.60068 (16)	0.4586 (5)	0.2391 (3)	0.0554 (7)
O1	0.4090 (5)	−0.0821 (11)	0.4263 (6)	0.055 (2)
H1A	0.3886	−0.0349	0.3770	0.066*
O2	0.5553 (5)	−0.0972 (10)	0.5246 (11)	0.056 (2)
N1	0.5284 (6)	0.2417 (15)	0.3874 (7)	0.053 (2)
N2	0.3691 (7)	0.3410 (14)	0.4957 (8)	0.059 (3)
N3	0.3876 (6)	0.0339 (15)	0.6429 (8)	0.062 (3)
N4	0.5503 (5)	0.2907 (14)	0.6137 (8)	0.049 (2)
C1	0.5589 (6)	0.3290 (14)	0.3260 (8)	0.042 (2)
C2	0.3211 (7)	0.4565 (16)	0.4856 (8)	0.046 (2)
C3	0.3300 (7)	0.0092 (15)	0.6872 (9)	0.048 (2)
C4	0.5891 (6)	0.3954 (14)	0.6563 (8)	0.042 (2)
C5	0.4697 (9)	−0.214 (2)	0.3969 (10)	0.070 (4)
H5A	0.5041	−0.1628	0.3450	0.084*
H5B	0.4426	−0.3223	0.3709	0.084*
C6	0.5205 (10)	−0.2635 (18)	0.4811 (12)	0.079 (4)
H6A	0.5646	−0.3444	0.4601	0.095*
H6B	0.4874	−0.3276	0.5300	0.095*
C7	0.6398 (7)	−0.0798 (18)	0.5074 (14)	0.075 (4)
H7A	0.6656	−0.1977	0.5133	0.113*
H7B	0.6632	0.0026	0.5551	0.113*
H7C	0.6487	−0.0325	0.4420	0.113*
S3	0.24565 (17)	−0.0155 (5)	0.7570 (3)	0.0631 (12)
S2	0.25328 (17)	0.6239 (5)	0.4751 (3)	0.0553 (8)
S4	0.64088 (17)	0.5579 (4)	0.7156 (2)	0.0485 (6)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Hg1	0.0366 (2)	0.0622 (3)	0.0574 (3)	−0.00611 (16)	0.0037 (3)	−0.0139 (3)
Mn1	0.0388 (8)	0.0376 (7)	0.0439 (8)	−0.0022 (6)	−0.0006 (8)	0.0009 (9)
S1	0.0425 (13)	0.0665 (18)	0.0571 (16)	0.0070 (13)	0.0049 (12)	0.0207 (15)
O1	0.053 (5)	0.054 (5)	0.059 (5)	0.001 (4)	−0.013 (4)	−0.004 (4)
O2	0.047 (4)	0.046 (4)	0.077 (5)	0.010 (3)	−0.005 (6)	−0.015 (6)
N1	0.049 (5)	0.060 (6)	0.050 (5)	−0.005 (5)	0.008 (4)	0.005 (5)
N2	0.058 (6)	0.060 (6)	0.059 (6)	0.003 (5)	0.010 (5)	0.016 (5)
N3	0.068 (6)	0.057 (6)	0.061 (7)	−0.010 (5)	0.014 (5)	0.012 (5)
N4	0.044 (4)	0.047 (5)	0.057 (6)	0.000 (4)	−0.009 (4)	−0.014 (5)
C1	0.032 (4)	0.049 (6)	0.046 (6)	0.009 (4)	0.003 (4)	0.000 (5)
C2	0.046 (5)	0.055 (7)	0.037 (5)	0.011 (5)	0.000 (5)	0.005 (5)
C3	0.052 (6)	0.039 (5)	0.053 (6)	0.000 (5)	0.005 (5)	0.014 (5)
C4	0.037 (4)	0.048 (6)	0.041 (5)	0.007 (4)	0.004 (4)	0.003 (5)
C5	0.093 (11)	0.060 (8)	0.058 (8)	−0.020 (8)	−0.006 (7)	−0.016 (7)
C6	0.111 (13)	0.034 (6)	0.092 (11)	−0.003 (7)	−0.013 (10)	0.001 (7)
C7	0.046 (6)	0.069 (8)	0.111 (13)	−0.004 (6)	0.013 (7)	0.011 (9)
S3	0.0594 (17)	0.0560 (16)	0.074 (3)	0.0067 (12)	0.0201 (16)	0.0162 (18)
S2	0.0575 (19)	0.064 (2)	0.0440 (17)	0.0210 (16)	0.0023 (12)	0.0045 (13)
S4	0.0495 (13)	0.0426 (14)	0.0533 (15)	0.0047 (11)	−0.0088 (12)	−0.0069 (13)

Geometric parameters (Å, º)

Hg1—S4^i	2.479 (3)	O2—C6	1.461 (16)
Hg1—S1	2.506 (3)	N1—C1	1.157 (13)
Hg1—S3^ii	2.536 (4)	N2—C2	1.155 (14)
Hg1—S2^iii	2.685 (4)	N3—C3	1.124 (13)
Mn1—N4	2.169 (9)	N4—C4	1.145 (13)
Mn1—N2	2.174 (11)	C2—S2	1.649 (11)
Mn1—N1	2.200 (10)	C3—S3	1.670 (11)
Mn1—N3	2.215 (10)	C4—S4	1.659 (11)
Mn1—O1	2.247 (8)	C5—C6	1.451 (18)
Mn1—O2	2.255 (7)	S3—Hg1^iv	2.536 (4)
S1—C1	1.652 (11)	S2—Hg1^v	2.685 (4)
O1—C5	1.432 (17)	S4—Hg1^vi	2.479 (3)
O2—C7	1.395 (14)
S4^i—Hg1—S1	117.52 (10)	O1—Mn1—O2	74.3 (3)
S4^i—Hg1—S3^ii	120.00 (10)	C1—S1—Hg1	94.4 (3)
S1—Hg1—S3^ii	108.35 (10)	C5—O1—Mn1	111.1 (7)
S4^i—Hg1—S2^iii	105.87 (10)	C7—O2—C6	112.8 (11)
S1—Hg1—S2^iii	103.53 (11)	C7—O2—Mn1	124.1 (8)
S3^ii—Hg1—S2^iii	98.31 (11)	C6—O2—Mn1	112.0 (8)
N4—Mn1—N2	101.4 (4)	C1—N1—Mn1	166.5 (9)
N4—Mn1—N1	90.3 (4)	C2—N2—Mn1	175.6 (11)
N2—Mn1—N1	88.6 (4)	C3—N3—Mn1	157.9 (10)
N4—Mn1—N3	96.0 (4)	C4—N4—Mn1	168.9 (9)
N2—Mn1—N3	86.6 (4)	N1—C1—S1	178.4 (10)
N1—Mn1—N3	172.7 (4)	N2—C2—S2	178.0 (12)
N4—Mn1—O1	162.4 (3)	N3—C3—S3	176.4 (12)
N2—Mn1—O1	96.2 (4)	N4—C4—S4	176.1 (10)
N1—Mn1—O1	88.4 (4)	O1—C5—C6	109.8 (11)
N3—Mn1—O1	86.7 (4)	C5—C6—O2	109.1 (11)
N4—Mn1—O2	88.1 (4)	C3—S3—Hg1^iv	96.9 (4)
N2—Mn1—O2	170.2 (4)	C2—S2—Hg1^v	98.5 (4)
N1—Mn1—O2	88.9 (4)	C4—S4—Hg1^vi	97.0 (3)
N3—Mn1—O2	94.9 (4)

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