Issue contents
Download PDF of article
Download CIF
3D view
Navigation
Highlighting
Dictionary of Crystallography reference
IUPAC Gold Book reference
more ...
Download citation
FormatBIBTeX
EndNote
RefMan
Refer
Medline
CIF
SGML
Plain Text
share
Previous article
Next article
Previous article
Issue contents
Download PDF of article
Download CIF
3D view
Navigation
Highlighting
Dictionary of Crystallography reference
IUPAC Gold Book reference
more ...
Download citation
FormatBIBTeX
EndNote
RefMan
Refer
Medline
CIF
SGML
Plain Text
share
Next article

metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 66| Part 9| September 2010| Pages m1115-m1116
https://doi.org/10.1107/S1600536810031909

Di-μ-sulfato-κ4O:O′-bis­­[di­aqua­(1H-imidazo[4,5-f][1,10]phenanthroline)manganese(II)] dihydrate

Ming-Xing Yang,a,b Shen Lin,a,b* Li-Juan Chena,b and Xiao-Hua Chena

aCollege of Chemistry and Materials Science, Fujian Normal University, Fuzhou, Fujian 350007, People's Republic of China, and bState Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002, People's Republic of China
*Correspondence e-mail: shenlin@fjnu.edu.cn

(Received 29 July 2010; accepted 9 August 2010; online 18 August 2010)

In the title centrosymmetric dinuclear compound, [Mn2(SO4)2(C13H8N4)2(H2O)4]·2H2O, the MnII atom is octa­hedrally 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 mol­ecules and the uncoodinated water mol­ecules are connected by O—H⋯O, O—H⋯N and N—H⋯O hydrogen bonds into a three-dimensional network. A π–π stacking inter­action 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.

Related literature

For general background to the crystal engineering of functional materials, see: Aoyama (1998[Aoyama, Y. (1998). Top. Curr. Chem. 198, 131-162.]); Bassani et al. (2000[Bassani, D. M., Darcos, V., Mahony, S. & Desvergne, J. P. (2000). J. Am. Chem. Soc. 122, 8795-8796.]); Kahn (2000[Kahn, O. (2000). Acc. Chem. Res. 33, 647-657.]); Matsuda et al. (2005[Matsuda, R., Kitaura, R., Kitagawa, S., Kubota, Y., Belosludov, R. V., Kobayashi, T. C., Sakamoto, H., Chiba, T., Takata, M., Kawazoe, Y. & Mita, Y. (2005). Nature (London), 436, 238-241.]); Miller (2000[Miller, J. S. (2000). Inorg. Chem. 39, 4392-4408.]); Rowsell et al. (2004[Rowsell, J. L. C., Millward, A. R., Park, K. S. & Yaghi, O. M. (2004). J. Am. Chem. Soc. 126, 5666-5667.]). For related structures, see: Gong et al. (2009[Gong, Y., Zhou, Y., Li, J., Wu, X. & Qin, J. (2009). Acta Cryst. E65, m844-m845.]); Wang et al. (2008[Wang, H., Liu, J.-Q., Zhang, Y.-N., Wang, Y.-Y., Wen, G.-L., Guo, C.-Y. & Shi, Q.-Z. (2008). Inorg. Chem. Commun. 11, 129-133.]); Wu et al. (1997[Wu, J.-Z., Ye, B.-H., Wang, L., Ji, L.-N., Zhou, J.-Y., Li, R.-H. & Zhou, Z.-Y. (1997). J. Chem. Soc. Dalton Trans. pp. 1395-1401.]); Yang et al. (2010[Yang, M.-X., Lin, S., Zheng, S.-N., Chen, X.-H. & Chen, L.-J. (2010). Inorg. Chem. Commun. 13, 1043-1046.]); Yu (2009[Yu, J. (2009). Acta Cryst. E65, m618.]); Zeng et al. (2009[Zeng, W., She, J.-H., Wang, C.-J. & Fang, Y. (2009). Acta Cryst. E65, m42-m43.]).

[Scheme 1]

Experimental

Crystal data

  • [Mn2(SO4)2(C13H8N4)2(H2O)4]·2H2O

  • Mr = 850.58

  • Monoclinic, P 21 /c

  • 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[Rigaku (2002). CrystalClear. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.432, Tmax = 1.000

  • 11099 measured reflections

  • 3544 independent reflections

  • 3251 reflections with I > 2σ(I)

  • Rint = 0.024
Refinement

  • R[F2 > 2σ(F2)] = 0.030

  • wR(F2) = 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

Table 1
Selected bond lengths (Å)

Mn1—O1 2.1366 (17)
Mn1—O3i 2.1641 (16)
Mn1—O5 2.2590 (16)
Mn1—O6 2.1751 (17)
Mn1—N1 2.2718 (19)
Mn1—N2 2.2715 (19)
Symmetry code: (i) -x, -y+1, -z.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O5—H1⋯O2i 0.85 (1) 1.95 (1) 2.789 (2) 165 (3)
O5—H2⋯N4ii 0.86 (3) 1.99 (3) 2.824 (2) 164 (3)
O6—H3⋯O7iii 0.84 (1) 1.80 (1) 2.644 (3) 172 (3)
O6—H4⋯O2 0.84 (2) 1.97 (1) 2.745 (2) 154 (2)
O7—H5⋯O2iv 0.85 (1) 1.98 (1) 2.828 (3) 171 (3)
O7—H6⋯O4 0.84 (1) 2.04 (2) 2.833 (3) 157 (3)
N3—H3B⋯O4v 0.86 2.04 2.890 (2) 167
Symmetry codes: (i) -x, -y+1, -z; (ii) -x+1, -y+2, -z; (iii) x, y+1, z; (iv) [-x, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]; (v) [-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}].

Data collection: CrystalClear (Rigaku, 2002[Rigaku (2002). CrystalClear. Rigaku Corporation, Tokyo, Japan.]); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]) and DIAMOND (Brandenburg, 1999[Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536810031909/hy2338sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810031909/hy2338Isup2.hkl

checkCIF report


Comment top

An important aspect of crystal engineering is to understand and attempt to control the manner in which molecules are arranged in crystal lattices through the use of noncovalent interactions such as electrostatic interactions, hydrogen bonding, dispersion and induction forces, and π-π stacking interactions. These materials have attracted much interest due to their strong potential for a variety of applications including gas storage (Matsuda et al., 2005; Rowsell et al., 2004), catalytic properties (Aoyama, 1998; Bassani et al., 2000) and magnetism (Kahn, 2000; Miller, 2000). One approach to forming networks of discrete transition metal complexes is to use a chelating ligand that has additional interactional functionality attached to its backbone, such as additional coordination sites or hydrogen bonding groups, or extended π systems. 1H-Imidazo[5,f][1,10]phenanthroline (ip) has been used to form metal complexes with novel supramolecular architectures due to their excellent coordinating ability, large conjugated systems and strong hydrogen bonding donor and acceptor groups (Gong et al., 2009; Wang et al., 2008; Wu et al., 1997; Yang et al., 2010; Yu, 2009; Zeng et al., 2009). In the present paper,we hydrothermally synthesized a new coordination complex constructed from MnSO4 and ip.

The title dimeric complex is generated by an inversion center (Fig. 1). The MnII atom is six-coordinated by two N atoms from one ip ligand, two O atoms from water molecules and two O atoms from two sulfate anions in a distorted octahedral geometry (Table 1). The equatorial plane is defined by N2, O6, O1 and O5 and the axial coordination sites are occupied by N1 and O3i atoms [symmetry code: (i) -x, 1-y, -z]. The sulfate anion acts as a bidentate bridging ligand connecting two MnII ions, thus generating a binuclear complex. The hydrogen bonds play a key role in the structural stability (Table 2). The uncoordinated water molecule is a hydrogen bond acceptor from the coordinated water, and a hydrogen bond donor to two O atoms of two sulfate anions in two neighboring complex molecules. So each free water is hydrogen bonded to three different complex molecules. The ip ligand is a hydrogen bond donor through the imidazolyl NH group to a sulfate O atom of an adjacent complex molecule and a hydrogen bond acceptor from the coordinated water molecule (O5) of another adjacent complex molecule through the other imidazolyl N atom, forming a three-dimensional network structure, as illustrated in Fig. 2. There is also a π–π stacking interaction between the pyridyl ring of the ip ligand and the benzene ring of the neighboring ip ligand, with a centroid–centroid distance of 3.579 (2) Å.

Related literature top

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 top

The ip ligand was synthesized according to literature (Wu et al., 1997). A mixture of MnSO4, ip and H2O in a molar ratio of 1:1:556 was stirred for an hour, then sealed in an 18 ml Teflon-lined stainless steel reactor and heated for 3 d at 433 K and autogeneous pressure. After allowing the reaction mixture to cool down to room temperature, yellow crystals were collected, washed with water and dried at room temperature.

Refinement top

C- and N-bound H atoms were positioned geometrically and refined as riding atoms, with C—H = 0.93 and N—H = 0.86 Å and Uiso(H) = 1.2Ueq(C,N). The water H atoms were located in a difference Fourier map and refined isotropically, with restraints of O—H = 0.84 (1) and H···H = 1.44 (1) Å.

Structure description top

An important aspect of crystal engineering is to understand and attempt to control the manner in which molecules are arranged in crystal lattices through the use of noncovalent interactions such as electrostatic interactions, hydrogen bonding, dispersion and induction forces, and π-π stacking interactions. These materials have attracted much interest due to their strong potential for a variety of applications including gas storage (Matsuda et al., 2005; Rowsell et al., 2004), catalytic properties (Aoyama, 1998; Bassani et al., 2000) and magnetism (Kahn, 2000; Miller, 2000). One approach to forming networks of discrete transition metal complexes is to use a chelating ligand that has additional interactional functionality attached to its backbone, such as additional coordination sites or hydrogen bonding groups, or extended π systems. 1H-Imidazo[5,f][1,10]phenanthroline (ip) has been used to form metal complexes with novel supramolecular architectures due to their excellent coordinating ability, large conjugated systems and strong hydrogen bonding donor and acceptor groups (Gong et al., 2009; Wang et al., 2008; Wu et al., 1997; Yang et al., 2010; Yu, 2009; Zeng et al., 2009). In the present paper,we hydrothermally synthesized a new coordination complex constructed from MnSO4 and ip.

The title dimeric complex is generated by an inversion center (Fig. 1). The MnII atom is six-coordinated by two N atoms from one ip ligand, two O atoms from water molecules and two O atoms from two sulfate anions in a distorted octahedral geometry (Table 1). The equatorial plane is defined by N2, O6, O1 and O5 and the axial coordination sites are occupied by N1 and O3i atoms [symmetry code: (i) -x, 1-y, -z]. The sulfate anion acts as a bidentate bridging ligand connecting two MnII ions, thus generating a binuclear complex. The hydrogen bonds play a key role in the structural stability (Table 2). The uncoordinated water molecule is a hydrogen bond acceptor from the coordinated water, and a hydrogen bond donor to two O atoms of two sulfate anions in two neighboring complex molecules. So each free water is hydrogen bonded to three different complex molecules. The ip ligand is a hydrogen bond donor through the imidazolyl NH group to a sulfate O atom of an adjacent complex molecule and a hydrogen bond acceptor from the coordinated water molecule (O5) of another adjacent complex molecule through the other imidazolyl N atom, forming a three-dimensional network structure, as illustrated in Fig. 2. There is also a π–π stacking interaction between the pyridyl ring of the ip ligand and the benzene ring of the neighboring ip ligand, with a centroid–centroid distance of 3.579 (2) Å.

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).

Computing details top

Data collection: CrystalClear (Rigaku, 2002); cell refinement: CrystalClear (Rigaku, 2002); data reduction: CrystalClear (Rigaku, 2002); 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 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. Molecular structure of the title compound. H atoms have been omitted for clarity. [Symmetry code: (A) -x, 1-y, -z.]
[Figure 2] Fig. 2. The three-dimensional hydrogen bonding network in the title compound.
Di-µ-sulfato-κ4O:O'- bis[diaqua(1H-imidazo-[4,5-f][1,10]phenanthroline)manganese(II)] dihydrate top
Crystal data top
[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
Data collection top
Rigaku Mercury CCD
diffractometer		3544 independent reflections
Radiation source: fine-focus sealed tube3251 reflections with I > 2σ(I)
Graphite monochromatorRint = 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 top
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 = 1.05 w = 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
Crystal data top
[Mn2(SO4)2(C13H8N4)2(H2O)4]·2H2OV = 1615.2 (18) Å3
Mr = 850.58Z = 2
Monoclinic, P21/cMo Kα radiation
a = 10.467 (7) ŵ = 1.00 mm−1
b = 9.171 (6) ÅT = 293 K
c = 17.025 (11) Å1.00 × 0.80 × 0.60 mm
β = 98.758 (12)°
Data collection top
Rigaku Mercury CCD
diffractometer		3544 independent reflections
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2002)		3251 reflections with I > 2σ(I)
Tmin = 0.432, Tmax = 1.000Rint = 0.024
11099 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0309 restraints
wR(F2) = 0.082H atoms treated by a mixture of independent and constrained refinement
S = 1.05Δρmax = 0.30 e Å−3
3544 reflectionsΔρmin = −0.39 e Å−3
259 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
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*
Atomic displacement parameters (Å2) top
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)
Geometric parameters (Å, º) top
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)
Symmetry code: (i) −x, −y+1, −z.
Hydrogen-bond geometry (Å, º) top
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) −x, −y+1, −z; (ii) −x+1, −y+2, −z; (iii) x, y+1, z; (iv) −x, y−1/2, −z+1/2; (v) −x+1, y+1/2, −z+1/2.

Experimental details

Crystal data
Chemical formula[Mn2(SO4)2(C13H8N4)2(H2O)4]·2H2O
Mr850.58
Crystal system, space groupMonoclinic, P21/c
Temperature (K)293
a, b, c (Å)10.467 (7), 9.171 (6), 17.025 (11)
β (°) 98.758 (12)
V (Å3)1615.2 (18)
Z2
Radiation typeMo Kα
µ (mm−1)1.00
Crystal size (mm)1.00 × 0.80 × 0.60
Data collection
DiffractometerRigaku Mercury CCD
Absorption correctionMulti-scan
(CrystalClear; Rigaku, 2002)
Tmin, Tmax0.432, 1.000
No. of measured, independent and
observed [I > 2σ(I)] reflections		11099, 3544, 3251
Rint0.024
(sin θ/λ)max (Å−1)0.647
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.030, 0.082, 1.05
No. of reflections3544
No. of parameters259
No. of restraints9
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3)0.30, −0.39

Computer programs: CrystalClear (Rigaku, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top
Mn1—O12.1366 (17)Mn1—O62.1751 (17)
Mn1—O3i2.1641 (16)Mn1—N12.2718 (19)
Mn1—O52.2590 (16)Mn1—N22.2715 (19)
Symmetry code: (i) −x, −y+1, −z.
Hydrogen-bond geometry (Å, º) top
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) −x, −y+1, −z; (ii) −x+1, −y+2, −z; (iii) x, y+1, z; (iv) −x, y−1/2, −z+1/2; (v) −x+1, y+1/2, −z+1/2.
 

Acknowledgements

This work was supported by the National Natural Science Foundation of China (grant No. 20771024), the Natural Science Foundation of Fujian Province (grant No. 2008 J0142) and the Key Project Fund of Science and Technology of Fujian Province (grant No. 2008I0013).

References

First citationAoyama, Y. (1998). Top. Curr. Chem. 198, 131–162.  CrossRef CAS Google Scholar
 First citationBassani, D. M., Darcos, V., Mahony, S. & Desvergne, J. P. (2000). J. Am. Chem. Soc. 122, 8795–8796.  Web of Science CrossRef CAS Google Scholar
 First citationBrandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.  Google Scholar
 First citationGong, Y., Zhou, Y., Li, J., Wu, X. & Qin, J. (2009). Acta Cryst. E65, m844–m845.  Web of Science CSD CrossRef IUCr Journals Google Scholar
 First citationKahn, O. (2000). Acc. Chem. Res. 33, 647–657.  Web of Science CrossRef PubMed CAS Google Scholar
 First citationMatsuda, R., Kitaura, R., Kitagawa, S., Kubota, Y., Belosludov, R. V., Kobayashi, T. C., Sakamoto, H., Chiba, T., Takata, M., Kawazoe, Y. & Mita, Y. (2005). Nature (London), 436, 238–241.  Web of Science CrossRef PubMed CAS Google Scholar
 First citationMiller, J. S. (2000). Inorg. Chem. 39, 4392–4408.  Web of Science CrossRef CAS Google Scholar
 First citationRigaku (2002). CrystalClear. Rigaku Corporation, Tokyo, Japan.  Google Scholar
 First citationRowsell, J. L. C., Millward, A. R., Park, K. S. & Yaghi, O. M. (2004). J. Am. Chem. Soc. 126, 5666–5667.  Web of Science CSD CrossRef PubMed CAS Google Scholar
 First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
 First citationWang, H., Liu, J.-Q., Zhang, Y.-N., Wang, Y.-Y., Wen, G.-L., Guo, C.-Y. & Shi, Q.-Z. (2008). Inorg. Chem. Commun. 11, 129–133.  Web of Science CSD CrossRef CAS Google Scholar
 First citationWu, J.-Z., Ye, B.-H., Wang, L., Ji, L.-N., Zhou, J.-Y., Li, R.-H. & Zhou, Z.-Y. (1997). J. Chem. Soc. Dalton Trans. pp. 1395–1401.  CSD CrossRef Web of Science Google Scholar
 First citationYang, M.-X., Lin, S., Zheng, S.-N., Chen, X.-H. & Chen, L.-J. (2010). Inorg. Chem. Commun. 13, 1043–1046.  Web of Science CSD CrossRef CAS Google Scholar
 First citationYu, J. (2009). Acta Cryst. E65, m618.  Web of Science CSD CrossRef IUCr Journals Google Scholar
 First citationZeng, W., She, J.-H., Wang, C.-J. & Fang, Y. (2009). Acta Cryst. E65, m42–m43.  Web of Science CrossRef IUCr Journals Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 66| Part 9| September 2010| Pages m1115-m1116
https://doi.org/10.1107/S1600536810031909
Follow Acta Cryst. E
Sign up for e-alerts
E-alerts
Follow Acta Cryst. on Twitter
Twitter
Follow us on facebook
Facebook
Sign up for RSS feeds
RSS