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The title polymeric compound, {[MnHg(SCN)4(H2O)]·C4H8O2S}n, consists of slightly distorted MnN4O2 octahedra and HgS4 tetrahedra. Each MnII ion is bound to N atoms belonging to the thiocyanate (SCN) groups and to two O atoms of adjacent water ligands. The sulfolane molecule connects with the coordinated water molecule through hydrogen bonding. Each HgII atom is coordinated by four SCN S atoms. The two adjacent MnII atoms and two O atoms of bridging water molecules connect with one another and form a parallelogram. Each pair of MnII and HgII atoms is connected by an –SCN– bridge, forming an infinite three-dimensional structure.
Supporting information
CCDC reference: 620522
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (C-C) = 0.015 Å
- R factor = 0.036
- wR factor = 0.072
- Data-to-parameter ratio = 18.0
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for S2
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for S3
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Hg1
PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C6
PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C7
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for S5
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 15
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.16 Ratio
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
8 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
3 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
4 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: XSCANS (Siemens, 1996); cell refinement: XSCANS; data reduction: SHELXTL (Bruker, 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: WinGX (Farrugia, 1999).
Poly[[µ-aqua-tetra-µ-thiocyanato-manganese(II)mercury(II)] sulfolane solvate]
top
Crystal data top
[MnHg(NCS)4(H2O)]·C4H8O2S | F(000) = 1180 |
Mr = 626.03 | Dx = 2.299 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 39 reflections |
a = 8.6605 (9) Å | θ = 5.0–12.5° |
b = 17.1620 (18) Å | µ = 9.77 mm−1 |
c = 12.1745 (13) Å | T = 296 K |
β = 92.034 (9)° | Prism, colourless |
V = 1808.4 (3) Å3 | 0.20 × 0.10 × 0.10 mm |
Z = 4 | |
Data collection top
Bruker P4 diffractometer | 2500 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.029 |
Graphite monochromator | θmax = 26.5°, θmin = 2.1° |
ω scans | h = −10→1 |
Absorption correction: ψ scan (XSCANS; Siemens, 1996) | k = −21→1 |
Tmin = 0.315, Tmax = 0.376 | l = −15→15 |
4825 measured reflections | 3 standard reflections every 97 reflections |
3752 independent reflections | intensity decay: none |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.036 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.072 | w = 1/[σ2(Fo2) + (0.0266P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.98 | (Δ/σ)max = 0.001 |
3752 reflections | Δρmax = 1.11 e Å−3 |
209 parameters | Δρmin = −0.94 e Å−3 |
15 restraints | Extinction correction: SHELXTL (Bruker, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00342 (14) |
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 | Uiso*/Ueq | |
C1 | 0.8259 (9) | 0.2642 (5) | 0.5761 (6) | 0.037 (2) | |
C2 | 0.3419 (9) | 0.1879 (4) | 0.4232 (6) | 0.0313 (18) | |
C3 | 0.5292 (9) | 0.4269 (4) | 0.2615 (6) | 0.0336 (19) | |
C4 | 0.3687 (9) | 0.3655 (4) | 0.7460 (5) | 0.0298 (18) | |
C5 | 0.5020 (14) | 0.1332 (6) | 0.6884 (8) | 0.076 (4) | |
H5A | 0.5789 | 0.1517 | 0.6385 | 0.091* | |
H5B | 0.4003 | 0.1479 | 0.6595 | 0.091* | |
C6 | 0.5306 (19) | 0.1662 (7) | 0.8002 (9) | 0.124 (5) | |
H6A | 0.6372 | 0.1834 | 0.8077 | 0.149* | |
H6B | 0.4649 | 0.2114 | 0.8092 | 0.149* | |
C7 | 0.5004 (18) | 0.1096 (6) | 0.8868 (8) | 0.110 (5) | |
H7A | 0.4064 | 0.1244 | 0.9224 | 0.132* | |
H7B | 0.5844 | 0.1116 | 0.9416 | 0.132* | |
C8 | 0.4840 (13) | 0.0282 (6) | 0.8466 (7) | 0.065 (3) | |
H8A | 0.3815 | 0.0084 | 0.8600 | 0.078* | |
H8B | 0.5596 | −0.0054 | 0.8834 | 0.078* | |
N1 | 0.8844 (8) | 0.2105 (4) | 0.5410 (5) | 0.0446 (19) | |
N2 | 1.2290 (8) | 0.1632 (4) | 0.4564 (5) | 0.0402 (16) | |
N3 | 1.0540 (9) | 0.0905 (4) | 0.6736 (5) | 0.0423 (19) | |
N4 | 0.9272 (8) | 0.1140 (4) | 0.3261 (5) | 0.0394 (18) | |
O1 | 0.8417 (6) | 0.0098 (4) | 0.5114 (5) | 0.0314 (13) | |
O2 | 0.3954 (9) | −0.0065 (5) | 0.6443 (7) | 0.091 (3) | |
O3 | 0.6689 (7) | 0.0066 (4) | 0.6878 (5) | 0.067 (2) | |
S1 | 0.7453 (3) | 0.34179 (15) | 0.63208 (17) | 0.0462 (6) | |
S2 | 0.5024 (3) | 0.22395 (15) | 0.37626 (19) | 0.0577 (7) | |
S3 | 0.4915 (4) | 0.46071 (15) | 0.38531 (17) | 0.0649 (8) | |
S4 | 0.2770 (2) | 0.33364 (16) | 0.63267 (15) | 0.0470 (6) | |
S5 | 0.5151 (3) | 0.03230 (14) | 0.70517 (16) | 0.0384 (5) | |
Mn1 | 1.01482 (15) | 0.10850 (6) | 0.49682 (9) | 0.0276 (3) | |
Hg1 | 0.50509 (4) | 0.339533 (19) | 0.50594 (2) | 0.03523 (12) | |
H1A | 0.776 (10) | 0.016 (5) | 0.470 (7) | 0.03 (3)* | |
H1B | 0.783 (11) | 0.003 (5) | 0.559 (8) | 0.06 (3)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.033 (5) | 0.039 (5) | 0.039 (4) | −0.003 (4) | −0.001 (4) | 0.003 (4) |
C2 | 0.035 (5) | 0.029 (4) | 0.029 (4) | −0.003 (4) | 0.000 (4) | −0.005 (3) |
C3 | 0.043 (5) | 0.029 (4) | 0.028 (4) | −0.001 (4) | −0.007 (4) | 0.000 (3) |
C4 | 0.034 (4) | 0.034 (4) | 0.022 (3) | 0.007 (4) | 0.010 (3) | 0.004 (3) |
C5 | 0.102 (10) | 0.049 (7) | 0.076 (7) | −0.002 (7) | −0.010 (7) | 0.021 (6) |
C6 | 0.171 (10) | 0.083 (8) | 0.115 (8) | −0.019 (8) | −0.028 (8) | −0.013 (7) |
C7 | 0.166 (15) | 0.117 (12) | 0.049 (6) | −0.022 (12) | 0.025 (8) | −0.021 (8) |
C8 | 0.077 (8) | 0.074 (8) | 0.046 (5) | 0.022 (7) | 0.029 (5) | 0.017 (5) |
N1 | 0.053 (5) | 0.040 (5) | 0.041 (4) | 0.018 (4) | 0.001 (4) | 0.003 (4) |
N2 | 0.041 (4) | 0.042 (4) | 0.038 (3) | −0.012 (4) | 0.002 (3) | −0.001 (4) |
N3 | 0.059 (5) | 0.044 (5) | 0.025 (3) | 0.001 (4) | 0.000 (3) | −0.001 (3) |
N4 | 0.051 (5) | 0.040 (4) | 0.026 (3) | −0.009 (4) | 0.000 (3) | 0.007 (3) |
O1 | 0.028 (3) | 0.039 (4) | 0.027 (3) | 0.001 (3) | 0.002 (3) | 0.001 (3) |
O2 | 0.071 (5) | 0.085 (6) | 0.113 (6) | −0.005 (5) | −0.042 (5) | −0.025 (5) |
O3 | 0.047 (4) | 0.105 (6) | 0.050 (3) | 0.018 (5) | 0.017 (3) | −0.004 (4) |
S1 | 0.0424 (13) | 0.0474 (14) | 0.0480 (11) | 0.0106 (13) | −0.0088 (10) | −0.0206 (12) |
S2 | 0.0564 (16) | 0.0607 (17) | 0.0580 (14) | −0.0277 (15) | 0.0286 (12) | −0.0323 (13) |
S3 | 0.128 (2) | 0.0408 (13) | 0.0269 (10) | 0.0028 (16) | 0.0122 (13) | −0.0010 (10) |
S4 | 0.0367 (12) | 0.0744 (17) | 0.0300 (9) | −0.0109 (14) | 0.0035 (9) | −0.0087 (12) |
S5 | 0.0362 (12) | 0.0456 (12) | 0.0334 (10) | −0.0014 (11) | 0.0020 (9) | −0.0026 (9) |
Mn1 | 0.0328 (7) | 0.0270 (5) | 0.0230 (5) | −0.0023 (6) | 0.0021 (5) | 0.0011 (5) |
Hg1 | 0.04130 (19) | 0.03670 (17) | 0.02776 (16) | −0.0033 (2) | 0.00241 (11) | −0.00115 (17) |
Geometric parameters (Å, º) top
C1—N1 | 1.142 (10) | C8—H8B | 0.9700 |
C1—S1 | 1.661 (9) | N1—Mn1 | 2.161 (7) |
C2—N2i | 1.152 (9) | N2—C2iv | 1.152 (9) |
C2—S2 | 1.643 (8) | N2—Mn1 | 2.151 (7) |
C3—N3ii | 1.138 (9) | N3—C3v | 1.138 (9) |
C3—S3 | 1.658 (7) | N3—Mn1 | 2.189 (6) |
C4—N4iii | 1.139 (9) | N4—C4vi | 1.139 (9) |
C4—S4 | 1.659 (8) | N4—Mn1 | 2.190 (6) |
C5—C6 | 1.487 (9) | O1—Mn1 | 2.274 (6) |
C5—S5 | 1.747 (10) | O1—Mn1vii | 2.384 (6) |
C5—H5A | 0.9700 | O1—H1A | 0.75 (8) |
C5—H5B | 0.9700 | O1—H1B | 0.79 (10) |
C6—C7 | 1.465 (9) | O2—S5 | 1.419 (7) |
C6—H6A | 0.9700 | O3—S5 | 1.426 (6) |
C6—H6B | 0.9700 | S1—Hg1 | 2.542 (2) |
C7—C8 | 1.484 (9) | S2—Hg1 | 2.535 (2) |
C7—H7A | 0.9700 | S3—Hg1 | 2.546 (2) |
C7—H7B | 0.9700 | S4—Hg1 | 2.551 (2) |
C8—S5 | 1.754 (8) | Mn1—O1vii | 2.384 (6) |
C8—H8A | 0.9700 | | |
| | | |
N1—C1—S1 | 177.5 (8) | Mn1—O1—H1B | 127 (7) |
N2i—C2—S2 | 179.4 (8) | Mn1vii—O1—H1B | 105 (7) |
N3ii—C3—S3 | 174.7 (8) | H1A—O1—H1B | 91 (8) |
N4iii—C4—S4 | 177.3 (8) | C1—S1—Hg1 | 95.0 (3) |
C6—C5—S5 | 105.3 (7) | C2—S2—Hg1 | 93.8 (3) |
C6—C5—H5A | 110.7 | C3—S3—Hg1 | 103.4 (3) |
S5—C5—H5A | 110.7 | C4—S4—Hg1 | 97.6 (3) |
C6—C5—H5B | 110.7 | O2—S5—O3 | 116.5 (5) |
S5—C5—H5B | 110.7 | O2—S5—C5 | 111.2 (5) |
H5A—C5—H5B | 108.8 | O3—S5—C5 | 110.2 (5) |
C7—C6—C5 | 112.2 (9) | O2—S5—C8 | 111.1 (6) |
C7—C6—H6A | 109.2 | O3—S5—C8 | 108.1 (5) |
C5—C6—H6A | 109.2 | C5—S5—C8 | 98.2 (5) |
C7—C6—H6B | 109.2 | N2—Mn1—N1 | 99.5 (3) |
C5—C6—H6B | 109.2 | N2—Mn1—N3 | 100.5 (3) |
H6A—C6—H6B | 107.9 | N1—Mn1—N3 | 86.2 (2) |
C6—C7—C8 | 113.9 (9) | N2—Mn1—N4 | 92.1 (2) |
C6—C7—H7A | 108.8 | N1—Mn1—N4 | 92.0 (3) |
C8—C7—H7A | 108.8 | N3—Mn1—N4 | 167.4 (3) |
C6—C7—H7B | 108.8 | N2—Mn1—O1 | 156.8 (2) |
C8—C7—H7B | 108.8 | N1—Mn1—O1 | 103.4 (3) |
H7A—C7—H7B | 107.7 | N3—Mn1—O1 | 84.1 (2) |
C7—C8—S5 | 105.7 (7) | N4—Mn1—O1 | 84.2 (2) |
C7—C8—H8A | 110.6 | N2—Mn1—O1vii | 84.7 (2) |
S5—C8—H8A | 110.6 | N1—Mn1—O1vii | 167.9 (2) |
C7—C8—H8B | 110.6 | N3—Mn1—O1vii | 81.9 (2) |
S5—C8—H8B | 110.6 | N4—Mn1—O1vii | 99.2 (2) |
H8A—C8—H8B | 108.7 | O1—Mn1—O1vii | 73.4 (2) |
C1—N1—Mn1 | 171.6 (7) | S2—Hg1—S1 | 112.17 (8) |
C2iv—N2—Mn1 | 171.9 (6) | S2—Hg1—S3 | 106.30 (8) |
C3v—N3—Mn1 | 158.9 (7) | S1—Hg1—S3 | 110.86 (10) |
C4vi—N4—Mn1 | 162.8 (7) | S2—Hg1—S4 | 110.82 (8) |
Mn1—O1—Mn1vii | 106.6 (2) | S1—Hg1—S4 | 105.65 (7) |
Mn1—O1—H1A | 109 (6) | S3—Hg1—S4 | 111.12 (9) |
Mn1vii—O1—H1A | 118 (6) | | |
| | | |
S5—C5—C6—C7 | −21.9 (17) | C4vi—N4—Mn1—O1vii | −174 (2) |
C5—C6—C7—C8 | 13 (2) | Mn1vii—O1—Mn1—N2 | 19.7 (7) |
C6—C7—C8—S5 | 1.9 (17) | Mn1vii—O1—Mn1—N1 | −167.9 (2) |
C6—C5—S5—O2 | 136.9 (10) | Mn1vii—O1—Mn1—N3 | −83.2 (3) |
C6—C5—S5—O3 | −92.3 (10) | Mn1vii—O1—Mn1—N4 | 101.4 (3) |
C6—C5—S5—C8 | 20.5 (11) | Mn1vii—O1—Mn1—O1vii | 0.0 |
C7—C8—S5—O2 | −129.9 (9) | C2—S2—Hg1—S1 | 119.5 (3) |
C7—C8—S5—O3 | 101.1 (9) | C2—S2—Hg1—S3 | −119.2 (3) |
C7—C8—S5—C5 | −13.4 (10) | C2—S2—Hg1—S4 | 1.7 (3) |
C3v—N3—Mn1—N2 | 176.7 (19) | C1—S1—Hg1—S2 | 3.3 (3) |
C3v—N3—Mn1—N1 | 77.7 (19) | C1—S1—Hg1—S3 | −115.4 (3) |
C3v—N3—Mn1—N4 | −4 (3) | C1—S1—Hg1—S4 | 124.2 (3) |
C3v—N3—Mn1—O1 | −26.2 (19) | C3—S3—Hg1—S2 | −13.6 (3) |
C3v—N3—Mn1—O1vii | −100.3 (19) | C3—S3—Hg1—S1 | 108.5 (3) |
C4vi—N4—Mn1—N2 | −89 (2) | C3—S3—Hg1—S4 | −134.3 (3) |
C4vi—N4—Mn1—N1 | 11 (2) | C4—S4—Hg1—S2 | 141.2 (3) |
C4vi—N4—Mn1—N3 | 92 (3) | C4—S4—Hg1—S1 | 19.5 (3) |
C4vi—N4—Mn1—O1 | 114 (2) | C4—S4—Hg1—S3 | −100.8 (3) |
Symmetry codes: (i) x−1, y, z; (ii) x−1/2, −y+1/2, z−1/2; (iii) x−1/2, −y+1/2, z+1/2; (iv) x+1, y, z; (v) x+1/2, −y+1/2, z+1/2; (vi) x+1/2, −y+1/2, z−1/2; (vii) −x+2, −y, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···O2viii | 0.75 (8) | 2.01 (8) | 2.745 (9) | 168 (9) |
O1—H1B···O3 | 0.79 (10) | 1.88 (10) | 2.660 (8) | 166 (9) |
Symmetry code: (viii) −x+1, −y, −z+1. |
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