Literature DB >> 21588521

Di-μ-sulfato-κO:O'-bis-[diaqua-(1H-imidazo[4,5-f][1,10]phenanthroline)manganese(II)] dihydrate.

Ming-Xing Yang, Shen Lin, Li-Juan Chen, Xiao-Hua Chen.   

Abstract

In the title centrosymmetric dinuclear compound, [Mn(2)(SO(4))(2)(C(13)n class="Species">H(8)N(4))(2)(H(2)O)(4)]·2H(2)O, the Mn(II) atom is octa-hedrally coordinated by two N atoms from a 1H-imidazo[4,5-f][1,10]phenanthroline (ip) ligand, two O atoms belonging to two bridging sulfate anions and two water O atoms. In the crystal structure, the complex mol-ecules and the uncoodinated water mol-ecules are connected by O-H⋯O, O-H⋯N and N-H⋯O hydrogen bonds into a three-dimensional network. A π-π stacking inter-action between the pyridyl ring of the ip ligand and the benzene ring of the neighboring ligand [centroid-centroid distance = 3.579 (2) Å] is also observed.

Entities:  

Year:  2010        PMID： 21588521      PMCID： PMC3007874          DOI： 10.1107/S1600536810031909

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


Related literature

For general background to the crystal engineering of functional materials, see: Aoyama (1998 ▶); Bassani et al. (2000 ▶); Kahn (2000 ▶); Matsuda et al. (2005 ▶); Miller (2000 ▶); Rowsell et al. (2004 ▶). For related structures, see: Gong et al. (2009 ▶); Wang et al. (2008 ▶); Wu et al. (1997 ▶); Yang et al. (2010 ▶); Yu (2009 ▶); Zeng et al. (2009 ▶).

Experimental

Crystal data

[Mn2(SO4)2(C13H8N4)2(n class="Chemical">H2O)4]·2H2O M = 850.58 Monoclinic, a = 10.467 (7) Å b = 9.171 (6) Å c = 17.025 (11) Å β = 98.758 (12)° V = 1615.2 (18) Å3 Z = 2 Mo Kα radiation μ = 1.00 mm−1 T = 293 K 1.00 × 0.80 × 0.60 mm

Data collection

Rigaku Mercury CCD diffractometer Absorption correction: multi-scan (CrystalClear; Rigaku, 2002 ▶) T min = 0.432, T max = 1.000 11099 measured reflections 3544 independent reflections 3251 reflections with I > 2σ(I) R int = 0.024

Refinement

R[F 2 > 2σ(F 2)] = 0.030 wR(F 2) = 0.082 S = 1.05 3544 reflections 259 parameters 9 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.30 e Å−3 Δρmin = −0.39 e Å−3 Data collection: CrystalClear (Rigaku, 2002 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶) and DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810031909/hy2338sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810031909/hy2338Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Mn2(SO4)2(C13H8N4)2(H2O)4]·2H2OF(000) = 868
Mr = 850.58Dx = 1.749 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 4851 reflections
a = 10.467 (7) Åθ = 3.3–27.4°
b = 9.171 (6) ŵ = 1.00 mm−1
c = 17.025 (11) ÅT = 293 K
β = 98.758 (12)°Prism, yellow
V = 1615.2 (18) Å31.00 × 0.80 × 0.60 mm
Z = 2
Rigaku Mercury CCD diffractometer3544 independent reflections
Radiation source: fine-focus sealed tube3251 reflections with I > 2σ(I)
graphiteRint = 0.024
Detector resolution: 14.6306 pixels mm-1θmax = 27.4°, θmin = 2.5°
ω scanh = −13→13
Absorption correction: multi-scan (CrystalClear; Rigaku, 2002)k = −11→11
Tmin = 0.432, Tmax = 1.000l = −21→21
11099 measured reflections
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.082H atoms treated by a mixture of independent and constrained refinement
S = 1.05w = 1/[σ2(Fo2) + (0.0437P)2 + 0.5623P] where P = (Fo2 + 2Fc2)/3
3544 reflections(Δ/σ)max = 0.001
259 parametersΔρmax = 0.30 e Å−3
9 restraintsΔρmin = −0.39 e Å−3
xyzUiso*/Ueq
Mn10.18299 (2)0.67998 (3)0.039544 (16)0.02452 (10)
S10.03061 (4)0.40185 (4)0.11921 (2)0.02399 (11)
O10.13383 (12)0.47205 (14)0.08303 (9)0.0374 (3)
O2−0.06301 (12)0.51435 (14)0.13804 (8)0.0316 (3)
O3−0.03679 (12)0.29274 (14)0.06387 (8)0.0311 (3)
O40.08663 (14)0.32790 (15)0.19348 (9)0.0400 (3)
O50.29524 (13)0.55706 (16)−0.04252 (8)0.0339 (3)
H10.2295 (19)0.519 (3)−0.0712 (14)0.074 (9)*
H20.329 (3)0.626 (3)−0.0665 (16)0.096 (12)*
O60.05988 (16)0.77338 (17)0.11855 (10)0.0484 (4)
H30.065 (2)0.8546 (15)0.1421 (14)0.059 (8)*
H40.012 (2)0.7107 (19)0.1349 (14)0.056 (8)*
O70.0949 (3)0.01928 (19)0.20000 (11)0.0714 (6)
H50.090 (3)0.008 (3)0.2492 (7)0.076 (10)*
H60.088 (3)0.1066 (16)0.1844 (15)0.084 (10)*
N10.37913 (14)0.68351 (15)0.11788 (9)0.0257 (3)
N20.25995 (13)0.91094 (15)0.03511 (9)0.0252 (3)
N30.74601 (14)1.01809 (18)0.20156 (9)0.0321 (3)
H3B0.80550.96780.22970.039*
N40.64434 (15)1.21029 (17)0.13915 (10)0.0338 (4)
C10.43732 (18)0.56818 (19)0.15534 (11)0.0303 (4)
H1A0.39300.48000.15220.036*
C20.56195 (18)0.5734 (2)0.19914 (12)0.0333 (4)
H2B0.59930.49010.22400.040*
C30.62820 (17)0.7031 (2)0.20480 (12)0.0314 (4)
H3C0.71050.70930.23430.038*
C40.56986 (15)0.82664 (18)0.16534 (10)0.0239 (3)
C50.62700 (15)0.96855 (19)0.16508 (10)0.0257 (4)
C60.56533 (16)1.08776 (18)0.12661 (10)0.0253 (3)
C70.43740 (15)1.07578 (18)0.08161 (10)0.0236 (3)
C80.36759 (18)1.19078 (18)0.04063 (12)0.0302 (4)
H8A0.40321.28380.04140.036*
C90.24595 (18)1.1648 (2)−0.00075 (12)0.0337 (4)
H9A0.19771.2403−0.02690.040*
C100.19618 (16)1.0231 (2)−0.00289 (11)0.0306 (4)
H10A0.11501.0060−0.03210.037*
C110.37862 (15)0.93635 (17)0.07832 (10)0.0220 (3)
C120.44406 (15)0.81270 (17)0.12160 (10)0.0222 (3)
C130.75016 (19)1.1614 (2)0.18408 (12)0.0370 (4)
H13A0.82091.22050.20200.044*
U11U22U33U12U13U23
Mn10.02168 (14)0.02247 (15)0.02823 (17)−0.00592 (9)−0.00001 (11)−0.00163 (10)
S10.0223 (2)0.0203 (2)0.0272 (2)−0.00508 (14)−0.00289 (16)0.00196 (15)
O10.0317 (7)0.0248 (6)0.0578 (9)−0.0043 (5)0.0138 (6)0.0050 (6)
O20.0289 (6)0.0270 (6)0.0384 (7)−0.0024 (5)0.0037 (5)−0.0046 (5)
O30.0290 (6)0.0253 (6)0.0354 (8)−0.0023 (5)−0.0067 (5)−0.0044 (5)
O40.0475 (8)0.0336 (7)0.0330 (8)−0.0034 (6)−0.0129 (6)0.0068 (6)
O50.0305 (7)0.0349 (7)0.0361 (8)−0.0022 (5)0.0040 (6)−0.0011 (6)
O60.0599 (9)0.0302 (8)0.0626 (10)−0.0153 (7)0.0334 (8)−0.0142 (7)
O70.1428 (19)0.0306 (9)0.0456 (11)−0.0169 (10)0.0295 (12)−0.0072 (7)
N10.0253 (7)0.0215 (7)0.0292 (8)−0.0046 (5)0.0008 (6)0.0003 (5)
N20.0209 (6)0.0247 (7)0.0287 (8)−0.0030 (5)0.0000 (6)0.0014 (6)
N30.0235 (7)0.0369 (9)0.0323 (9)−0.0062 (6)−0.0073 (6)0.0023 (7)
N40.0326 (8)0.0295 (8)0.0376 (9)−0.0113 (6)−0.0004 (7)0.0004 (7)
C10.0348 (9)0.0221 (8)0.0330 (10)−0.0035 (7)0.0026 (8)0.0010 (7)
C20.0363 (9)0.0266 (9)0.0352 (11)0.0049 (7)0.0002 (8)0.0060 (7)
C30.0244 (8)0.0342 (10)0.0335 (10)0.0018 (7)−0.0023 (7)0.0032 (8)
C40.0217 (7)0.0251 (8)0.0240 (9)−0.0023 (6)0.0006 (6)−0.0010 (6)
C50.0200 (7)0.0293 (9)0.0263 (9)−0.0046 (6)−0.0011 (6)−0.0012 (7)
C60.0253 (8)0.0234 (8)0.0266 (9)−0.0068 (6)0.0022 (7)−0.0018 (6)
C70.0241 (8)0.0224 (8)0.0241 (8)−0.0032 (6)0.0032 (7)−0.0012 (6)
C80.0327 (9)0.0207 (8)0.0364 (11)−0.0025 (6)0.0029 (8)0.0005 (7)
C90.0319 (9)0.0278 (9)0.0393 (11)0.0050 (7)−0.0019 (8)0.0064 (8)
C100.0218 (8)0.0316 (9)0.0362 (10)0.0006 (7)−0.0023 (7)0.0042 (8)
C110.0196 (7)0.0220 (8)0.0240 (9)−0.0025 (6)0.0024 (6)−0.0007 (6)
C120.0214 (7)0.0216 (8)0.0232 (9)−0.0030 (6)0.0019 (6)−0.0008 (6)
C130.0318 (9)0.0387 (11)0.0380 (11)−0.0177 (8)−0.0029 (8)−0.0020 (8)
Mn1—O12.1366 (17)N3—H3B0.8600
Mn1—O3i2.1641 (16)N4—C131.325 (3)
Mn1—O52.2590 (16)N4—C61.392 (2)
Mn1—O62.1751 (17)C1—C21.401 (3)
Mn1—N12.2718 (19)C1—H1A0.9300
Mn1—N22.2715 (19)C2—C31.373 (3)
S1—O11.4711 (14)C2—H2B0.9300
S1—O41.4753 (16)C3—C41.408 (2)
S1—O31.4779 (14)C3—H3C0.9300
S1—O21.4910 (14)C4—C121.416 (2)
O3—Mn1i2.1641 (16)C4—C51.433 (2)
O5—H10.85 (1)C5—C61.383 (2)
O5—H20.86 (3)C6—C71.442 (2)
O6—H30.84 (1)C7—C81.406 (2)
O6—H40.84 (2)C7—C111.416 (2)
O7—H50.85 (1)C8—C91.379 (3)
O7—H60.84 (1)C8—H8A0.9300
N1—C11.333 (2)C9—C101.398 (3)
N1—C121.363 (2)C9—H9A0.9300
N2—C101.338 (2)C10—H10A0.9300
N2—C111.364 (2)C11—C121.464 (2)
N3—C131.350 (3)C13—H13A0.9300
N3—C51.381 (2)
O1—Mn1—O3i101.97 (6)N1—C1—C2123.22 (16)
O1—Mn1—O686.60 (7)N1—C1—H1A118.4
O3i—Mn1—O692.60 (8)C2—C1—H1A118.4
O1—Mn1—O586.81 (6)C3—C2—C1119.08 (17)
O3i—Mn1—O585.67 (7)C3—C2—H2B120.5
O6—Mn1—O5172.68 (5)C1—C2—H2B120.5
O1—Mn1—N2161.64 (6)C2—C3—C4119.07 (17)
O3i—Mn1—N294.33 (5)C2—C3—H3C120.5
O6—Mn1—N284.25 (6)C4—C3—H3C120.5
O5—Mn1—N2102.96 (6)C3—C4—C12118.63 (15)
O1—Mn1—N193.04 (6)C3—C4—C5125.55 (16)
O3i—Mn1—N1160.02 (5)C12—C4—C5115.82 (15)
O6—Mn1—N1101.47 (8)N3—C5—C6106.07 (15)
O5—Mn1—N182.04 (7)N3—C5—C4130.22 (16)
N2—Mn1—N173.31 (5)C6—C5—C4123.70 (15)
O1—S1—O4109.79 (9)C5—C6—N4110.00 (16)
O1—S1—O3109.82 (9)C5—C6—C7121.34 (15)
O4—S1—O3108.90 (9)N4—C6—C7128.66 (16)
O1—S1—O2109.62 (9)C8—C7—C11117.88 (16)
O4—S1—O2108.80 (9)C8—C7—C6125.22 (15)
O3—S1—O2109.88 (8)C11—C7—C6116.90 (15)
S1—O1—Mn1140.06 (8)C9—C8—C7119.55 (16)
S1—O3—Mn1i130.55 (8)C9—C8—H8A120.2
Mn1—O5—H196 (2)C7—C8—H8A120.2
Mn1—O5—H2102 (2)C8—C9—C10119.05 (16)
H1—O5—H2112.2 (16)C8—C9—H9A120.5
Mn1—O6—H3129.9 (16)C10—C9—H9A120.5
Mn1—O6—H4112.2 (16)N2—C10—C9123.04 (17)
H3—O6—H4116.3 (16)N2—C10—H10A118.5
H5—O7—H6114.1 (16)C9—C10—H10A118.5
C1—N1—C12118.64 (15)N2—C11—C7122.01 (15)
C1—N1—Mn1125.14 (11)N2—C11—C12117.19 (14)
C12—N1—Mn1116.06 (11)C7—C11—C12120.81 (15)
C10—N2—C11118.41 (15)N1—C12—C4121.34 (15)
C10—N2—Mn1125.42 (12)N1—C12—C11117.28 (15)
C11—N2—Mn1116.10 (11)C4—C12—C11121.39 (14)
C13—N3—C5106.16 (15)N4—C13—N3113.86 (16)
C13—N3—H3B126.9N4—C13—H13A123.1
C5—N3—H3B126.9N3—C13—H13A123.1
C13—N4—C6103.91 (16)
D—H···AD—HH···AD···AD—H···A
O5—H1···O2i0.85 (1)1.95 (1)2.789 (2)165 (3)
O5—H2···N4ii0.86 (3)1.99 (3)2.824 (2)164 (3)
O6—H3···O7iii0.84 (1)1.80 (1)2.644 (3)172 (3)
O6—H4···O20.84 (2)1.97 (1)2.745 (2)154 (2)
O7—H5···O2iv0.85 (1)1.98 (1)2.828 (3)171 (3)
O7—H6···O40.84 (1)2.04 (2)2.833 (3)157 (3)
N3—H3B···O4v0.862.042.890 (2)167
Table 1

Selected bond lengths (Å)

Mn1—O12.1366 (17)
Mn1—O3i2.1641 (16)
Mn1—O52.2590 (16)
Mn1—O62.1751 (17)
Mn1—N12.2718 (19)
Mn1—N22.2715 (19)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O5—H1⋯O2i0.85 (1)1.95 (1)2.789 (2)165 (3)
O5—H2⋯N4ii0.86 (3)1.99 (3)2.824 (2)164 (3)
O6—H3⋯O7iii0.84 (1)1.80 (1)2.644 (3)172 (3)
O6—H4⋯O20.84 (2)1.97 (1)2.745 (2)154 (2)
O7—H5⋯O2iv0.85 (1)1.98 (1)2.828 (3)171 (3)
O7—H6⋯O40.84 (1)2.04 (2)2.833 (3)157 (3)
N3—H3B⋯O4v0.862.042.890 (2)167

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

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4.  Di-μ-sulfato-κO:O'-bis-[diaqua-(1H-imidazo[4,5-f][1,10]phenanthroline-κN,N)cobalt(II)] dihydrate.

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7.  Di-μ-sulfato-bis-[diaqua-(1H-imidazo[4,5-f][1,10]phenanthroline)nickel(II)] dihydrate.

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