Literature DB >> 21577466

Tetra-aqua-bis{2-[4-(3-pyrid-yl)pyrimidin-2-ylsulfan-yl]acetato}manganese(II) dihydrate.

Abstract

In the title compound, [Mn(C(11)H(8)N(3)O(n class="Chemical">2)S)(2)(H(2)O)(4)]·2H(2)O, the Mn(II) ion lies on an inversion centre and is coordinated by four water mol-ecules in equatorial positions and two N atoms from two 2-[4-(3-pyrid-yl)pyrimidin-2-ylsulfan-yl]acetate ligands in the axial positions. The water mol-ecules, including the uncoordinated water mol-ecules, and the acetate O atoms are involved in O-H⋯O and O-H⋯N hydrogen-bonding inter-actions, which link the components into layers parallel to the a (b + c) plane.

Entities: Chemical Disease Species

Year: 2009 PMID： 21577466 PMCID： PMC2970048 DOI： 10.1107/S1600536809033078

Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN： 1600-5368

Related literature

For hydro(solvo)thermal reactions between (heterocyclicthio)acetic acid and metal ions, see: Zhu et al. (2009 ▶); Hao et al. (2008 ▶); He et al. (2007 ▶). For a n class="Chemical">Cu(II) coordination compound with 4-(pyridin-4-yl)pyrimidine-2-sulfonate, see Li et al. (2009 ▶).

Experimental

Crystal data

[Mn(C11H8N3O2S)2(n class="Chemical">H2O)4]·2H2O M = 655.58 Triclinic, a = 8.459 (3) Å b = 9.240 (3) Å c = 9.360 (4) Å α = 87.396 (6)° β = 75.862 (5)° γ = 79.872 (5)° V = 698.4 (4) Å3 Z = 1 Mo Kα radiation μ = 0.69 mm−1 T = 298 K 0.14 × 0.12 × 0.10 mm

Data collection

Bruker APEXII CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.884, T max = 0.920 4518 measured reflections 3181 independent reflections 2443 reflections with I > 2σ(I) R int = 0.031

Refinement

R[F 2 > 2σ(F 2)] = 0.037 wR(F 2) = 0.094 S = 0.98 3181 reflections 187 parameters H-atom parameters constrained Δρmax = 0.49 e Å−3 Δρmin = −0.55 e Å−3 Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT-Plus (Bruker, 2007 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809033078/cv2600sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809033078/cv2600Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Mn(C₁₁H₈N₃O₂S)₂(H₂O)₄]·2H₂O	Z = 1
M_r = 655.58	F(000) = 339
Triclinic, P1	D_x = 1.559 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.459 (3) Å	Cell parameters from 3181 reflections
b = 9.240 (3) Å	θ = 2.2–28.1°
c = 9.360 (4) Å	µ = 0.69 mm⁻¹
α = 87.396 (6)°	T = 298 K
β = 75.862 (5)°	Block, colourless
γ = 79.872 (5)°	0.14 × 0.12 × 0.10 mm
V = 698.4 (4) Å³

Bruker APEXII CCD area-detector diffractometer	3181 independent reflections
Radiation source: fine-focus sealed tube	2443 reflections with I > 2σ(I)
graphite	R_int = 0.031
φ and ω scans	θ_max = 28.1°, θ_min = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 2001)	h = −10→10
T_min = 0.884, T_max = 0.920	k = −6→12
4518 measured reflections	l = −11→10

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.037	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.094	H-atom parameters constrained
S = 0.98	w = 1/[σ²(F_o²) + (0.0441P)²] where P = (F_o² + 2F_c²)/3
3181 reflections	(Δ/σ)_max < 0.001
187 parameters	Δρ_max = 0.49 e Å⁻³
0 restraints	Δρ_min = −0.55 e Å⁻³

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.

	x	y	z	U_iso*/U_eq
Mn1	0.0000	1.0000	0.5000	0.02786 (13)
S1	0.71353 (7)	0.62719 (6)	0.00440 (6)	0.03937 (16)
O1	0.12141 (17)	0.98576 (16)	0.26485 (16)	0.0383 (4)
O2	0.24139 (17)	1.03191 (17)	0.52792 (17)	0.0447 (4)
N2	0.49123 (19)	0.56249 (17)	0.24128 (18)	0.0291 (4)
O4	0.44775 (17)	0.95387 (16)	0.25780 (16)	0.0412 (4)
N1	0.6987 (2)	0.36606 (19)	0.1238 (2)	0.0379 (4)
C1	0.6227 (2)	0.5074 (2)	0.1385 (2)	0.0310 (4)
O3	0.71010 (18)	0.85073 (17)	0.23595 (17)	0.0455 (4)
C5	0.2749 (2)	0.5349 (2)	0.4544 (2)	0.0279 (4)
N3	0.0768 (2)	0.75451 (18)	0.53326 (19)	0.0335 (4)
C11	0.5782 (2)	0.8717 (2)	0.1953 (2)	0.0302 (4)
C4	0.4233 (2)	0.4687 (2)	0.3417 (2)	0.0295 (4)
C9	0.2097 (2)	0.6826 (2)	0.4396 (2)	0.0323 (5)
H9A	0.2621	0.7342	0.3595	0.039*
C10	0.5730 (3)	0.7975 (2)	0.0536 (2)	0.0342 (5)
H10A	0.5956	0.8662	−0.0272	0.041*
H10B	0.4614	0.7793	0.0633	0.041*
C6	0.1962 (3)	0.4588 (2)	0.5742 (2)	0.0354 (5)
H6A	0.2354	0.3600	0.5882	0.042*
C8	0.0031 (3)	0.6779 (2)	0.6484 (2)	0.0364 (5)
H8A	−0.0899	0.7256	0.7149	0.044*
C7	0.0596 (3)	0.5315 (2)	0.6721 (2)	0.0394 (5)
H7A	0.0058	0.4824	0.7534	0.047*
C2	0.6305 (3)	0.2757 (2)	0.2252 (3)	0.0415 (5)
H2C	0.6786	0.1769	0.2209	0.050*
C3	0.4920 (3)	0.3206 (2)	0.3369 (3)	0.0402 (5)
H3A	0.4466	0.2544	0.4060	0.048*
O5	1.0477 (2)	0.7838 (2)	0.1129 (2)	0.0871 (8)
H1	0.2712	1.0656	0.5985	0.105*
H2	0.2259	0.9808	0.2469	0.105*
H3	0.3309	1.0079	0.4625	0.105*
H4	0.0999	0.9300	0.2053	0.105*
H5	1.0980	0.7268	0.0413	0.105*
H6	0.9449	0.7871	0.1208	0.105*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mn1	0.0239 (2)	0.0266 (2)	0.0312 (3)	−0.00261 (17)	−0.00359 (17)	−0.00345 (17)
S1	0.0421 (3)	0.0381 (3)	0.0316 (3)	−0.0063 (2)	0.0042 (2)	−0.0080 (2)
O1	0.0354 (8)	0.0416 (9)	0.0347 (8)	−0.0006 (7)	−0.0053 (6)	−0.0082 (6)
O2	0.0289 (8)	0.0619 (11)	0.0447 (10)	−0.0092 (7)	−0.0080 (7)	−0.0149 (8)
N2	0.0291 (9)	0.0264 (9)	0.0310 (9)	−0.0038 (7)	−0.0055 (7)	−0.0033 (7)
O4	0.0305 (8)	0.0442 (9)	0.0447 (9)	−0.0013 (7)	−0.0023 (7)	−0.0141 (7)
N1	0.0360 (10)	0.0308 (10)	0.0452 (11)	0.0008 (8)	−0.0091 (8)	−0.0125 (8)
C1	0.0313 (11)	0.0301 (11)	0.0339 (12)	−0.0060 (8)	−0.0105 (9)	−0.0066 (8)
O3	0.0342 (8)	0.0558 (10)	0.0482 (10)	−0.0005 (7)	−0.0147 (7)	−0.0200 (8)
C5	0.0274 (10)	0.0260 (10)	0.0319 (11)	−0.0056 (8)	−0.0095 (8)	0.0004 (8)
N3	0.0293 (9)	0.0303 (9)	0.0371 (10)	−0.0036 (7)	−0.0019 (7)	−0.0008 (7)
C11	0.0309 (11)	0.0293 (11)	0.0301 (11)	−0.0086 (8)	−0.0039 (8)	−0.0006 (8)
C4	0.0304 (10)	0.0259 (10)	0.0344 (11)	−0.0039 (8)	−0.0125 (9)	−0.0017 (8)
C9	0.0314 (11)	0.0267 (10)	0.0361 (12)	−0.0048 (8)	−0.0035 (9)	0.0027 (8)
C10	0.0415 (12)	0.0325 (11)	0.0283 (11)	−0.0068 (9)	−0.0075 (9)	0.0003 (8)
C6	0.0428 (12)	0.0274 (11)	0.0374 (12)	−0.0076 (9)	−0.0121 (10)	0.0045 (9)
C8	0.0324 (11)	0.0390 (12)	0.0342 (12)	−0.0070 (9)	−0.0003 (9)	−0.0015 (9)
C7	0.0427 (13)	0.0403 (13)	0.0335 (12)	−0.0119 (10)	−0.0036 (10)	0.0084 (9)
C2	0.0462 (13)	0.0246 (11)	0.0512 (14)	0.0041 (10)	−0.0130 (11)	−0.0077 (10)
C3	0.0456 (13)	0.0253 (11)	0.0470 (14)	−0.0031 (9)	−0.0081 (11)	0.0008 (9)
O5	0.0420 (10)	0.1175 (19)	0.0989 (17)	−0.0176 (11)	0.0041 (11)	−0.0692 (14)

Mn1—O1	2.1889 (16)	C5—C9	1.393 (3)
Mn1—O1ⁱ	2.1889 (16)	C5—C4	1.485 (3)
Mn1—O2ⁱ	2.1919 (15)	N3—C9	1.335 (2)
Mn1—O2	2.1919 (15)	N3—C8	1.345 (3)
Mn1—N3ⁱ	2.2761 (18)	C11—C10	1.534 (3)
Mn1—N3	2.2761 (18)	C4—C3	1.388 (3)
S1—C1	1.759 (2)	C9—H9A	0.9300
S1—C10	1.800 (2)	C10—H10A	0.9700
O1—H2	0.8520	C10—H10B	0.9700
O1—H4	0.8477	C6—C7	1.375 (3)
O2—H1	0.8510	C6—H6A	0.9300
O2—H3	0.8511	C8—C7	1.380 (3)
N2—C1	1.320 (2)	C8—H8A	0.9300
N2—C4	1.342 (3)	C7—H7A	0.9300
O4—C11	1.252 (2)	C2—C3	1.382 (3)
N1—C2	1.327 (3)	C2—H2C	0.9300
N1—C1	1.347 (2)	C3—H3A	0.9300
O3—C11	1.246 (2)	O5—H5	0.8500
C5—C6	1.386 (3)	O5—H6	0.8501

O1—Mn1—O1ⁱ	180.000 (1)	C8—N3—Mn1	123.89 (14)
O1—Mn1—O2ⁱ	95.09 (6)	O3—C11—O4	125.43 (18)
O1ⁱ—Mn1—O2ⁱ	84.91 (6)	O3—C11—C10	118.76 (18)
O1—Mn1—O2	84.91 (6)	O4—C11—C10	115.76 (18)
O1ⁱ—Mn1—O2	95.09 (6)	N2—C4—C3	120.38 (18)
O2ⁱ—Mn1—O2	180.00 (8)	N2—C4—C5	115.60 (16)
O1—Mn1—N3ⁱ	87.81 (6)	C3—C4—C5	124.02 (18)
O1ⁱ—Mn1—N3ⁱ	92.19 (6)	N3—C9—C5	124.01 (18)
O2ⁱ—Mn1—N3ⁱ	88.48 (6)	N3—C9—H9A	118.0
O2—Mn1—N3ⁱ	91.52 (6)	C5—C9—H9A	118.0
O1—Mn1—N3	92.19 (6)	C11—C10—S1	116.57 (14)
O1ⁱ—Mn1—N3	87.81 (6)	C11—C10—H10A	108.1
O2ⁱ—Mn1—N3	91.52 (6)	S1—C10—H10A	108.1
O2—Mn1—N3	88.48 (6)	C11—C10—H10B	108.1
N3ⁱ—Mn1—N3	180.000 (1)	S1—C10—H10B	108.1
C1—S1—C10	101.21 (10)	H10A—C10—H10B	107.3
Mn1—O1—H2	113.5	C7—C6—C5	119.14 (19)
Mn1—O1—H4	123.8	C7—C6—H6A	120.4
H2—O1—H4	108.6	C5—C6—H6A	120.4
Mn1—O2—H1	132.6	N3—C8—C7	122.84 (19)
Mn1—O2—H3	122.8	N3—C8—H8A	118.6
H1—O2—H3	104.6	C7—C8—H8A	118.6
C1—N2—C4	117.31 (17)	C6—C7—C8	119.36 (19)
C2—N1—C1	114.58 (18)	C6—C7—H7A	120.3
N2—C1—N1	127.05 (19)	C8—C7—H7A	120.3
N2—C1—S1	118.41 (15)	N1—C2—C3	123.44 (19)
N1—C1—S1	114.55 (15)	N1—C2—H2C	118.3
C6—C5—C9	117.58 (18)	C3—C2—H2C	118.3
C6—C5—C4	124.11 (18)	C2—C3—C4	117.2 (2)
C9—C5—C4	118.31 (17)	C2—C3—H3A	121.4
C9—N3—C8	117.06 (18)	C4—C3—H3A	121.4
C9—N3—Mn1	118.88 (13)	H5—O5—H6	106.5

C4—N2—C1—N1	−0.9 (3)	C9—C5—C4—C3	−174.50 (19)
C4—N2—C1—S1	179.48 (14)	C8—N3—C9—C5	0.1 (3)
C2—N1—C1—N2	0.1 (3)	Mn1—N3—C9—C5	175.57 (15)
C2—N1—C1—S1	179.79 (15)	C6—C5—C9—N3	−0.1 (3)
C10—S1—C1—N2	−3.72 (17)	C4—C5—C9—N3	179.86 (18)
C10—S1—C1—N1	176.59 (14)	O3—C11—C10—S1	28.1 (3)
O1—Mn1—N3—C9	24.51 (15)	O4—C11—C10—S1	−154.45 (16)
O1ⁱ—Mn1—N3—C9	−155.49 (15)	C1—S1—C10—C11	71.70 (17)
O2ⁱ—Mn1—N3—C9	119.67 (15)	C9—C5—C6—C7	−0.2 (3)
O2—Mn1—N3—C9	−60.33 (15)	C4—C5—C6—C7	179.86 (19)
O1—Mn1—N3—C8	−160.35 (16)	C9—N3—C8—C7	0.2 (3)
O1ⁱ—Mn1—N3—C8	19.65 (16)	Mn1—N3—C8—C7	−175.02 (15)
O2ⁱ—Mn1—N3—C8	−65.20 (17)	C5—C6—C7—C8	0.5 (3)
O2—Mn1—N3—C8	114.80 (17)	N3—C8—C7—C6	−0.5 (3)
C1—N2—C4—C3	0.9 (3)	C1—N1—C2—C3	0.6 (3)
C1—N2—C4—C5	−179.45 (16)	N1—C2—C3—C4	−0.5 (3)
C6—C5—C4—N2	−174.15 (19)	N2—C4—C3—C2	−0.3 (3)
C9—C5—C4—N2	5.9 (3)	C5—C4—C3—C2	−179.9 (2)
C6—C5—C4—C3	5.5 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O2—H1···O3ⁱⁱ	0.85	1.82	2.655 (2)	168
O1—H2···O4	0.85	1.88	2.709 (2)	165
O2—H3···O4	0.85	1.97	2.743 (2)	150
O1—H4···O5ⁱⁱⁱ	0.85	1.81	2.642 (3)	167
O5—H5···N1^iv	0.85	2.09	2.888 (3)	155
O5—H6···O3	0.85	2.01	2.775 (3)	149

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2—H1⋯O3ⁱ	0.85	1.82	2.655 (2)	168
O1—H2⋯O4	0.85	1.88	2.709 (2)	165
O2—H3⋯O4	0.85	1.97	2.743 (2)	150
O1—H4⋯O5ⁱⁱ	0.85	1.81	2.642 (3)	167
O5—H5⋯N1ⁱⁱⁱ	0.85	2.09	2.888 (3)	155
O5—H6⋯O3	0.85	2.01	2.775 (3)	149

Symmetry codes: (i) ; (ii) ; (iii) .

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Authors: George M Sheldrick
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3. Cu6S4 cluster based twelve-connected face-centered cubic and Cu19I4S12 cluster based fourteen-connected body-centered cubic topological coordination polymers.

Authors: Zheng-Ming Hao; Rui-Qin Fang; Hai-Shun Wu; Xian-Ming Zhang
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