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

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ISSN: 2056-9890

Di­aqua­tetra­kis­(1,3-di-4-pyridylpropane-κN)­manganese(II) bis­­(perchlorate) ses­qui­hydrate

aFaculty of Life Science and Chemical Engineering, Huaiyin Institute of Technology, Huaian 223003, People's Republic of China
*Correspondence e-mail: hyitshy@126.com

(Received 30 September 2011; accepted 8 October 2011; online 22 October 2011)

In the title complex, [Mn(C13H14N2)4(H2O)2](ClO4)2·1.5H2O, the MnII ion is coordinated by four N atoms from four different 1,3-di-4-pyridyl­propane mol­ecules and two O atoms from two coordinated water mol­ecules, leading to a distorted MnN4O2 octa­hedral geometry. Each 1,3-di-4-pyridyl­propane ligand displays a monodentate coordinating mode. In the crystal, there exist O—H⋯O, O—H⋯N and C—H⋯O hydrogen bonds. The perchlorate anions and the coordinated and lattice water mol­ecules play an important role in the formation of these hydrogen bonds. One of the two lattice water molecules shows half-occupancy.

Related literature

For a related structure, see: Zheng et al. (2007[Zheng, X., Niu, C., Wan, X. & Kou, C. (2007). Acta Cryst. E63, m2682-m2683.]).

[Scheme 1]

Experimental

Crystal data
  • [Mn(C13H14N2)4(H2O)2](ClO4)2·1.5H2O

  • Mr = 1108.94

  • Orthorhombic, P b c a

  • a = 19.0755 (10) Å

  • b = 15.9409 (9) Å

  • c = 37.533 (2) Å

  • V = 11412.9 (11) Å3

  • Z = 8

  • Mo Kα radiation

  • μ = 0.39 mm−1

  • T = 293 K

  • 0.30 × 0.30 × 0.10 mm

Data collection
  • Bruker APEXII CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.892, Tmax = 0.962

  • 61756 measured reflections

  • 10065 independent reflections

  • 6106 reflections with I > 2.σ(I)

  • Rint = 0.113

Refinement
  • R[F2 > 2σ(F2)] = 0.057

  • wR(F2) = 0.188

  • S = 1.01

  • 10065 reflections

  • 676 parameters

  • H-atom parameters constrained

  • Δρmax = 0.66 e Å−3

  • Δρmin = −0.47 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O3W—H3WA⋯N8i 0.92 1.86 2.753 (4) 162
O3W—H3W⋯N5ii 0.88 1.87 2.738 (4) 167
O2W—H2WA⋯O3Wiii 0.85 1.88 2.723 (3) 178
O2W—H2W⋯N7iv 0.86 1.98 2.844 (4) 174
O1W—H1W⋯N6v 0.81 2.08 2.824 (4) 153
O4W—H4W⋯O4 0.85 2.22 2.975 (9) 147
O1W—H1WA⋯O3W 0.80 1.91 2.684 (3) 163
O4W—H4WA⋯O6 0.85 2.43 3.035 (14) 129
C23—H23⋯O4iv 0.93 2.53 3.379 (6) 152
C28—H28⋯O5vi 0.93 2.43 3.255 (11) 148
C39—H39⋯O8 0.93 2.52 3.214 (9) 132
Symmetry codes: (i) [x-{\script{1\over 2}}, -y+{\script{3\over 2}}, -z]; (ii) [x+{\script{1\over 2}}, -y+{\script{3\over 2}}, -z]; (iii) [-x+{\script{1\over 2}}, y+{\script{1\over 2}}, z]; (iv) [-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]; (v) [-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]; (vi) [-x+{\script{3\over 2}}, y+{\script{1\over 2}}, z].

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, wisconsin, USA.]); cell refinement: SAINT (Bruker, 2008[Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, wisconsin, USA.]); data reduction: SAINT; 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: DIAMOND (Brandenburg, 2000[Brandenburg, K. (2000). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]).

Supporting information


Comment top

Flexible compounds, e.g., 1,3-di-4-pyridylpropane, are often used as ligands to synthesize complexes for their variable conformations. Herein, we report the crystal structure of thr title complex.

The asymmetric unit of the title complex consists of one manganese ion, four 1,3-di-4-pyridylpropane molecules, two coordinated water molecules, and sesqui crystallization water molecule. The Mn ion is coordinated by four N atoms from four different 1,3-di-4-pyridylpropane molecules and two O atoms from two coordinated water molecules, displaying a distorted MnN4O2 octahedral geometry (Fig. 1). Each 1,3-di-4-pyridylpropane displays a monodentate coordinating mode. In the crystal structure, there exist O—H···O, O—H···N and C—H···O hydrogen bonds (Table 1). Perchlorate anions and water molecules including coordinated water molecule and lattice water molecule, play very important roles in the formation of these hydrogen bonding interactions.

Related literature top

For a related structure, see: Zheng et al. (2007).

Experimental top

Reaction mixture of Mn(ClO4)2.6H2O (72.3 mg, 0.2 mmol), 1,3-di-4-pyridylpropane (39.6 mg, 0.2 mmol), 4-((1H-benzo[d]imidazol-1-yl)methyl)benzoic acid (50.4 mg, 0.2 mmol) and potassium hydroxide (11.2 mg, 0.2 mmol) in 12 ml H2O was sealed in a 16 ml Teflon-lined stainless steel container and heated to 373 K for 3 days. After cooling to room temperature, colorless block crystals of the title complex were obtained.

Refinement top

The hydrogen atoms bonded to C atoms were located in geometrically idealized positions and constrained to ride on their parent atoms, with C—H = 0.93–0.97 Å and Uiso(H) = 1.2Ueq(C). The hydrogen atoms of water molecules were located from difference Fourier maps and fixed at those positions with Uiso(H) = 1.2Ueq(O).

Computing details top

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT (Bruker, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2000); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. : The coordination environment of manganese ion in the title complex with the ellipsoids drawn at the 30% probability level. The hydrogen atoms are omitted for clarity.
Diaquatetrakis(1,3-di-4-pyridylpropane-κN)manganese(II) bis(perchlorate) sesquihydrate top
Crystal data top
[Mn(C13H14N2)4(H2O)2](ClO4)2·1.5H2OF(000) = 4648
Mr = 1108.94Dx = 1.291 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 8775 reflections
a = 19.0755 (10) Åθ = 2.3–22.1°
b = 15.9409 (9) ŵ = 0.39 mm1
c = 37.533 (2) ÅT = 293 K
V = 11412.9 (11) Å3Block, colorless
Z = 80.30 × 0.30 × 0.10 mm
Data collection top
Bruker APEXII CCD area-detector
diffractometer
10065 independent reflections
Radiation source: fine-focus sealed tube6106 reflections with I > 2.σ(I)
Graphite monochromatorRint = 0.113
ψ and ω scansθmax = 25.0°, θmin = 1.5°
Absorption correction: multi-scan
(SADBAS; Sheldrick, 1996)
h = 2221
Tmin = 0.892, Tmax = 0.962k = 1518
61756 measured reflectionsl = 4444
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)] = 0.057Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.188H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.1063P)2]
where P = (Fo2 + 2Fc2)/3
10065 reflections(Δ/σ)max < 0.001
676 parametersΔρmax = 0.66 e Å3
0 restraintsΔρmin = 0.47 e Å3
Crystal data top
[Mn(C13H14N2)4(H2O)2](ClO4)2·1.5H2OV = 11412.9 (11) Å3
Mr = 1108.94Z = 8
Orthorhombic, PbcaMo Kα radiation
a = 19.0755 (10) ŵ = 0.39 mm1
b = 15.9409 (9) ÅT = 293 K
c = 37.533 (2) Å0.30 × 0.30 × 0.10 mm
Data collection top
Bruker APEXII CCD area-detector
diffractometer
10065 independent reflections
Absorption correction: multi-scan
(SADBAS; Sheldrick, 1996)
6106 reflections with I > 2.σ(I)
Tmin = 0.892, Tmax = 0.962Rint = 0.113
61756 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0570 restraints
wR(F2) = 0.188H-atom parameters constrained
S = 1.01Δρmax = 0.66 e Å3
10065 reflectionsΔρmin = 0.47 e Å3
676 parameters
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
xyzUiso*/UeqOcc. (<1)
C10.14223 (18)1.0314 (2)0.10488 (10)0.0597 (10)
H10.16781.06940.09130.072*
C20.07095 (19)1.0255 (3)0.09937 (11)0.0655 (11)
H20.04961.05880.08220.079*
C30.03127 (18)0.9707 (2)0.11906 (9)0.0527 (9)
C40.06661 (19)0.9235 (2)0.14426 (10)0.0559 (9)
H40.04220.88590.15860.067*
C50.13743 (18)0.9323 (2)0.14805 (10)0.0547 (9)
H50.15990.89940.16510.066*
C60.04637 (19)0.9611 (3)0.11315 (11)0.0678 (11)
H6A0.06871.01550.11540.081*
H6B0.06560.92470.13140.081*
C70.06281 (19)0.9247 (2)0.07667 (11)0.0665 (11)
H7A0.04510.96230.05840.080*
H7B0.03890.87140.07410.080*
C80.1395 (2)0.9121 (3)0.07118 (12)0.0882 (15)
H8A0.16230.96640.07230.106*
H8B0.15730.87870.09080.106*
C90.16058 (19)0.8698 (2)0.03651 (10)0.0606 (10)
C100.1205 (2)0.8723 (3)0.00598 (12)0.0782 (13)
H100.07780.90050.00610.094*
C110.1432 (2)0.8335 (3)0.02461 (12)0.0821 (13)
H110.11450.83500.04460.099*
C120.2414 (2)0.7900 (3)0.00292 (12)0.0712 (11)
H120.28370.76100.00230.085*
C130.22126 (19)0.8261 (2)0.03454 (11)0.0637 (10)
H130.24940.82040.05460.076*
C140.24921 (19)1.0441 (2)0.21075 (9)0.0538 (9)
H140.21541.07330.19790.065*
C150.2552 (2)1.0593 (2)0.24677 (10)0.0580 (9)
H150.22621.09870.25760.070*
C160.30397 (19)1.0168 (2)0.26680 (9)0.0544 (9)
C170.3431 (2)0.9564 (2)0.24916 (9)0.0549 (9)
H170.37470.92340.26180.066*
C180.3351 (2)0.9453 (2)0.21296 (9)0.0531 (9)
H180.36280.90530.20160.064*
C190.3159 (2)1.0358 (3)0.30553 (9)0.0697 (11)
H19A0.33080.98520.31770.084*
H19B0.27221.05410.31620.084*
C200.3716 (2)1.1043 (3)0.31056 (10)0.0715 (12)
H20A0.35631.15450.29820.086*
H20B0.37491.11760.33570.086*
C210.4431 (2)1.0807 (3)0.29724 (10)0.0681 (11)
H21A0.44121.07660.27150.082*
H21B0.45461.02550.30640.082*
C220.5018 (2)1.1405 (2)0.30718 (10)0.0579 (9)
C230.5094 (2)1.1700 (2)0.34110 (10)0.0688 (11)
H230.47701.15540.35850.083*
C240.5653 (2)1.2215 (2)0.34953 (11)0.0688 (11)
H240.56981.23960.37300.083*
C250.6038 (2)1.2202 (3)0.29304 (12)0.0686 (11)
H250.63521.23820.27570.082*
C260.55031 (19)1.1674 (3)0.28279 (10)0.0644 (10)
H260.54711.15000.25920.077*
C270.45059 (19)1.0310 (2)0.15797 (10)0.0602 (10)
H270.42701.07350.16990.072*
C280.5213 (2)1.0201 (3)0.16459 (11)0.0676 (11)
H280.54401.05530.18060.081*
C290.55806 (19)0.9584 (3)0.14793 (11)0.0632 (11)
C300.5216 (2)0.9099 (3)0.12349 (11)0.0653 (11)
H300.54430.86760.11100.078*
C310.45089 (19)0.9250 (2)0.11788 (10)0.0574 (9)
H310.42750.89260.10100.069*
C320.6336 (2)0.9401 (3)0.15606 (12)0.0893 (15)
H32A0.65710.99160.16280.107*
H32B0.65640.91840.13490.107*
C330.6403 (2)0.8748 (4)0.18692 (14)0.126 (2)
H33A0.61920.82270.17890.151*
H33B0.68980.86380.19060.151*
C340.6109 (3)0.8954 (4)0.21972 (14)0.1048 (17)
H340.58600.94470.22360.126*
C350.6232 (2)0.8298 (3)0.24870 (10)0.0683 (11)
C360.5681 (2)0.7938 (2)0.26690 (11)0.0674 (11)
H360.52220.80530.26010.081*
C370.5809 (2)0.7406 (2)0.29507 (10)0.0597 (10)
H370.54280.71710.30680.072*
C380.6976 (2)0.7557 (2)0.28853 (10)0.0579 (10)
H380.74300.74330.29580.069*
C390.68936 (19)0.8087 (3)0.25999 (11)0.0680 (11)
H390.72850.83020.24830.082*
C400.3504 (2)1.0414 (2)0.05622 (10)0.0584 (9)
H400.37881.07470.07060.070*
C410.3601 (2)1.0443 (2)0.02028 (10)0.0649 (10)
H410.39461.07920.01090.078*
C420.3198 (2)0.9966 (2)0.00230 (9)0.0570 (10)
C430.2689 (2)0.9476 (2)0.01370 (10)0.0623 (10)
H430.23910.91520.00030.075*
C440.2621 (2)0.9468 (2)0.05040 (9)0.0560 (9)
H440.22820.91230.06050.067*
C450.3314 (3)0.9972 (3)0.04187 (9)0.0790 (13)
H45A0.33471.05480.05000.095*
H45B0.29140.97160.05350.095*
C460.3973 (2)0.9506 (2)0.05256 (11)0.0757 (12)
H46A0.40570.95980.07770.091*
H46B0.43670.97400.03960.091*
C470.3943 (2)0.8574 (2)0.04568 (11)0.0706 (11)
H47A0.35590.83340.05920.085*
H47B0.38500.84780.02060.085*
C480.46184 (19)0.8138 (2)0.05589 (10)0.0554 (9)
C490.5060 (2)0.7804 (2)0.03079 (10)0.0636 (10)
H490.49380.78230.00680.076*
C500.5681 (2)0.7442 (3)0.04085 (11)0.0697 (11)
H500.59660.72100.02330.084*
C510.5469 (2)0.7728 (2)0.09890 (11)0.0647 (10)
H510.56060.77090.12270.078*
C520.4838 (2)0.8086 (2)0.09083 (10)0.0660 (10)
H520.45550.82950.10900.079*
Cl10.58949 (8)0.70331 (11)0.06219 (3)0.1041 (5)
Cl20.86174 (6)0.74954 (9)0.18277 (3)0.0814 (4)
Mn10.29477 (3)0.98755 (3)0.132673 (12)0.04169 (17)
N10.17626 (15)0.98481 (17)0.12894 (7)0.0478 (7)
N20.28962 (14)0.98929 (16)0.19338 (7)0.0477 (7)
N30.41480 (15)0.98328 (17)0.13525 (7)0.0492 (7)
N40.30208 (15)0.99315 (16)0.07197 (7)0.0487 (7)
N50.20398 (19)0.7941 (2)0.02681 (9)0.0730 (9)
N60.61299 (18)1.24651 (18)0.32579 (10)0.0642 (9)
N70.64522 (17)0.72116 (18)0.30637 (8)0.0565 (8)
N80.58976 (18)0.7405 (2)0.07466 (9)0.0672 (9)
O10.6203 (5)0.6491 (4)0.03846 (15)0.266 (4)
O20.5196 (3)0.6942 (5)0.06484 (15)0.225 (3)
O30.6027 (2)0.7825 (3)0.04889 (12)0.1479 (16)
O40.6163 (3)0.6917 (5)0.09613 (11)0.230 (3)
O50.8830 (6)0.6780 (5)0.1902 (4)0.386 (7)
O60.8360 (5)0.7531 (9)0.1523 (2)0.402 (8)
O70.9184 (3)0.7981 (6)0.1854 (2)0.285 (4)
O80.8137 (4)0.7648 (5)0.2053 (2)0.283 (4)
O1W0.29594 (11)0.85152 (13)0.13508 (6)0.0529 (6)
H1W0.31010.81910.15010.063*
H1WA0.28370.82220.11890.063*
O2W0.29751 (12)1.12426 (13)0.13705 (5)0.0518 (6)
H2W0.31651.15580.15310.062*
H2WA0.28941.16210.12180.062*
O3W0.23088 (12)0.74826 (13)0.08930 (6)0.0526 (6)
H3W0.25670.74090.07000.063*
H3WA0.18480.76360.08580.063*
O4W0.7562 (4)0.6184 (6)0.1121 (2)0.130 (3)0.50
H4WA0.77190.66800.10960.156*0.50
H4W0.71370.61820.10550.156*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.048 (2)0.056 (2)0.075 (3)0.0006 (17)0.0087 (19)0.016 (2)
C20.052 (2)0.072 (3)0.072 (3)0.006 (2)0.013 (2)0.020 (2)
C30.049 (2)0.055 (2)0.055 (2)0.0003 (18)0.0047 (18)0.0070 (18)
C40.059 (2)0.051 (2)0.058 (2)0.0056 (18)0.0051 (19)0.0011 (18)
C50.052 (2)0.052 (2)0.060 (2)0.0007 (17)0.0087 (18)0.0110 (18)
C60.049 (2)0.085 (3)0.070 (2)0.006 (2)0.012 (2)0.007 (2)
C70.052 (2)0.061 (2)0.086 (3)0.0010 (19)0.018 (2)0.007 (2)
C80.058 (3)0.116 (4)0.090 (3)0.004 (2)0.016 (2)0.025 (3)
C90.054 (2)0.068 (3)0.060 (2)0.005 (2)0.0147 (19)0.004 (2)
C100.067 (3)0.091 (3)0.077 (3)0.021 (2)0.017 (2)0.015 (3)
C110.072 (3)0.111 (4)0.063 (3)0.004 (3)0.011 (2)0.024 (3)
C120.060 (2)0.077 (3)0.077 (3)0.004 (2)0.008 (2)0.007 (2)
C130.055 (2)0.066 (2)0.070 (3)0.001 (2)0.004 (2)0.007 (2)
C140.057 (2)0.054 (2)0.050 (2)0.0011 (18)0.0057 (18)0.0000 (18)
C150.059 (2)0.058 (2)0.056 (2)0.0079 (19)0.0057 (19)0.0087 (19)
C160.059 (2)0.061 (2)0.0433 (19)0.0275 (19)0.0027 (17)0.0038 (18)
C170.064 (2)0.049 (2)0.051 (2)0.0090 (18)0.0168 (19)0.0069 (18)
C180.069 (2)0.042 (2)0.048 (2)0.0008 (17)0.0135 (19)0.0002 (16)
C190.069 (3)0.096 (3)0.044 (2)0.030 (2)0.0012 (19)0.005 (2)
C200.073 (3)0.087 (3)0.055 (2)0.020 (2)0.007 (2)0.020 (2)
C210.073 (3)0.073 (3)0.059 (2)0.025 (2)0.001 (2)0.014 (2)
C220.064 (2)0.054 (2)0.056 (2)0.0164 (19)0.0099 (19)0.0044 (18)
C230.085 (3)0.065 (3)0.057 (2)0.028 (2)0.002 (2)0.007 (2)
C240.092 (3)0.057 (2)0.058 (2)0.018 (2)0.017 (2)0.007 (2)
C250.061 (2)0.072 (3)0.072 (3)0.014 (2)0.001 (2)0.001 (2)
C260.059 (2)0.077 (3)0.057 (2)0.017 (2)0.0062 (19)0.012 (2)
C270.059 (2)0.046 (2)0.076 (3)0.0040 (18)0.019 (2)0.0026 (19)
C280.066 (3)0.055 (2)0.081 (3)0.019 (2)0.024 (2)0.021 (2)
C290.048 (2)0.074 (3)0.068 (2)0.007 (2)0.005 (2)0.040 (2)
C300.059 (2)0.070 (3)0.066 (2)0.015 (2)0.009 (2)0.019 (2)
C310.056 (2)0.058 (2)0.059 (2)0.0009 (19)0.0041 (19)0.0006 (19)
C320.050 (2)0.125 (4)0.093 (3)0.004 (2)0.002 (2)0.060 (3)
C330.061 (3)0.216 (7)0.100 (4)0.051 (4)0.002 (3)0.071 (4)
C340.095 (4)0.125 (4)0.095 (4)0.037 (3)0.002 (3)0.040 (3)
C350.057 (2)0.080 (3)0.068 (2)0.000 (2)0.007 (2)0.029 (2)
C360.054 (2)0.071 (3)0.077 (3)0.002 (2)0.015 (2)0.016 (2)
C370.058 (2)0.061 (2)0.061 (2)0.0013 (19)0.0011 (19)0.0071 (19)
C380.052 (2)0.058 (2)0.064 (2)0.0068 (18)0.0157 (19)0.0024 (19)
C390.051 (2)0.082 (3)0.072 (3)0.001 (2)0.004 (2)0.023 (2)
C400.069 (2)0.047 (2)0.060 (2)0.0074 (19)0.003 (2)0.0025 (18)
C410.078 (3)0.054 (2)0.063 (2)0.005 (2)0.013 (2)0.005 (2)
C420.080 (3)0.046 (2)0.045 (2)0.018 (2)0.0022 (19)0.0020 (17)
C430.082 (3)0.053 (2)0.052 (2)0.003 (2)0.016 (2)0.0100 (19)
C440.070 (2)0.048 (2)0.050 (2)0.0076 (18)0.0087 (19)0.0004 (17)
C450.125 (4)0.063 (3)0.049 (2)0.031 (3)0.005 (2)0.0085 (19)
C460.109 (3)0.059 (2)0.060 (2)0.001 (2)0.024 (2)0.010 (2)
C470.077 (3)0.056 (2)0.079 (3)0.002 (2)0.017 (2)0.011 (2)
C480.065 (2)0.044 (2)0.057 (2)0.0059 (18)0.0084 (19)0.0027 (17)
C490.074 (3)0.071 (3)0.046 (2)0.009 (2)0.011 (2)0.0031 (19)
C500.066 (3)0.086 (3)0.058 (2)0.006 (2)0.003 (2)0.000 (2)
C510.077 (3)0.066 (3)0.051 (2)0.006 (2)0.009 (2)0.007 (2)
C520.077 (3)0.063 (3)0.058 (2)0.006 (2)0.002 (2)0.002 (2)
Cl10.1142 (11)0.1330 (12)0.0652 (8)0.0252 (9)0.0104 (7)0.0228 (8)
Cl20.0720 (8)0.1004 (9)0.0717 (7)0.0177 (7)0.0082 (6)0.0079 (6)
Mn10.0469 (3)0.0362 (3)0.0419 (3)0.0010 (2)0.0107 (2)0.0012 (2)
N10.0469 (16)0.0448 (16)0.0518 (17)0.0034 (14)0.0098 (14)0.0053 (14)
N20.0593 (18)0.0384 (15)0.0456 (15)0.0017 (14)0.0083 (14)0.0028 (13)
N30.0478 (16)0.0412 (16)0.0587 (18)0.0004 (14)0.0116 (14)0.0026 (14)
N40.0613 (18)0.0399 (16)0.0451 (16)0.0013 (14)0.0070 (14)0.0004 (13)
N50.070 (2)0.081 (2)0.069 (2)0.0043 (19)0.0157 (19)0.0024 (19)
N60.067 (2)0.0501 (19)0.075 (2)0.0130 (16)0.0197 (19)0.0016 (17)
N70.064 (2)0.0494 (18)0.0561 (18)0.0057 (15)0.0063 (16)0.0028 (15)
N80.067 (2)0.069 (2)0.066 (2)0.0103 (17)0.0092 (18)0.0078 (18)
O10.499 (13)0.146 (5)0.152 (5)0.097 (6)0.104 (6)0.003 (4)
O20.122 (4)0.342 (9)0.211 (6)0.116 (5)0.030 (4)0.133 (6)
O30.157 (4)0.136 (4)0.150 (4)0.051 (3)0.030 (3)0.022 (3)
O40.161 (5)0.443 (11)0.086 (3)0.041 (5)0.005 (3)0.073 (4)
O50.420 (15)0.138 (6)0.60 (2)0.134 (8)0.031 (12)0.032 (9)
O60.262 (9)0.78 (2)0.165 (6)0.151 (11)0.110 (7)0.125 (9)
O70.124 (4)0.351 (11)0.379 (11)0.081 (6)0.027 (5)0.110 (9)
O80.205 (6)0.350 (11)0.293 (9)0.006 (6)0.136 (6)0.104 (8)
O1W0.0661 (15)0.0344 (12)0.0582 (14)0.0003 (11)0.0221 (12)0.0011 (10)
O2W0.0750 (16)0.0336 (12)0.0469 (13)0.0014 (11)0.0150 (11)0.0014 (10)
O3W0.0577 (14)0.0523 (14)0.0479 (13)0.0098 (11)0.0016 (11)0.0021 (11)
O4W0.132 (6)0.141 (7)0.118 (6)0.020 (5)0.017 (5)0.014 (5)
Geometric parameters (Å, º) top
C1—N11.337 (4)C32—C331.563 (6)
C1—C21.379 (5)C32—H32A0.9700
C1—H10.9300C32—H32B0.9700
C2—C31.372 (5)C33—C341.392 (7)
C2—H20.9300C33—H33A0.9700
C3—C41.383 (5)C33—H33B0.9700
C3—C61.505 (5)C34—C351.527 (6)
C4—C51.366 (5)C34—H340.9300
C4—H40.9300C35—C391.372 (5)
C5—N11.328 (4)C35—C361.379 (5)
C5—H50.9300C36—C371.376 (5)
C6—C71.520 (5)C36—H360.9300
C6—H6A0.9700C37—N71.334 (5)
C6—H6B0.9700C37—H370.9300
C7—C81.491 (5)C38—N71.323 (5)
C7—H7A0.9700C38—C391.373 (5)
C7—H7B0.9700C38—H380.9300
C8—C91.520 (5)C39—H390.9300
C8—H8A0.9700C40—N41.338 (4)
C8—H8B0.9700C40—C411.363 (5)
C9—C131.353 (5)C40—H400.9300
C9—C101.378 (5)C41—C421.374 (5)
C10—C111.374 (6)C41—H410.9300
C10—H100.9300C42—C431.384 (5)
C11—N51.322 (5)C42—C451.502 (5)
C11—H110.9300C43—C441.383 (5)
C12—N51.326 (5)C43—H430.9300
C12—C131.374 (5)C44—N41.335 (4)
C12—H120.9300C44—H440.9300
C13—H130.9300C45—C461.513 (6)
C14—N21.335 (4)C45—H45A0.9700
C14—C151.379 (5)C45—H45B0.9700
C14—H140.9300C46—C471.509 (5)
C15—C161.375 (5)C46—H46A0.9700
C15—H150.9300C46—H46B0.9700
C16—C171.386 (5)C47—C481.514 (5)
C16—C191.502 (5)C47—H47A0.9700
C17—C181.378 (4)C47—H47B0.9700
C17—H170.9300C48—C491.371 (5)
C18—N21.336 (4)C48—C521.379 (5)
C18—H180.9300C49—C501.371 (5)
C19—C201.534 (5)C49—H490.9300
C19—H19A0.9700C50—N81.335 (5)
C19—H19B0.9700C50—H500.9300
C20—C211.500 (6)C51—N81.327 (5)
C20—H20A0.9700C51—C521.367 (5)
C20—H20B0.9700C51—H510.9300
C21—C221.518 (5)C52—H520.9300
C21—H21A0.9700Cl1—O21.344 (5)
C21—H21B0.9700Cl1—O11.373 (5)
C22—C231.365 (5)Cl1—O31.381 (4)
C22—C261.371 (5)Cl1—O41.385 (4)
C23—C241.381 (5)Cl2—O51.242 (7)
C23—H230.9300Cl2—O61.245 (6)
C24—N61.335 (5)Cl2—O81.271 (6)
C24—H240.9300Cl2—O71.334 (6)
C25—N61.311 (5)Mn1—O1W2.170 (2)
C25—C261.376 (5)Mn1—O2W2.186 (2)
C25—H250.9300Mn1—N12.265 (3)
C26—H260.9300Mn1—N22.281 (3)
C27—N31.331 (4)Mn1—N42.284 (3)
C27—C281.383 (5)Mn1—N32.293 (3)
C27—H270.9300O1W—H1W0.8104
C28—C291.359 (6)O1W—H1WA0.8011
C28—H280.9300O2W—H2W0.8636
C29—C301.387 (6)O2W—H2WA0.8457
C29—C321.502 (5)O3W—H3W0.8847
C30—C311.386 (5)O3W—H3WA0.9219
C30—H300.9300O4W—H4WA0.8497
C31—N31.327 (4)O4W—H4W0.8491
C31—H310.9300
N1—C1—C2122.8 (3)C34—C33—H33B107.9
N1—C1—H1118.6C32—C33—H33B107.9
C2—C1—H1118.6H33A—C33—H33B107.2
C3—C2—C1120.4 (3)C33—C34—C35114.0 (5)
C3—C2—H2119.8C33—C34—H34123.0
C1—C2—H2119.8C35—C34—H34123.0
C2—C3—C4116.5 (3)C39—C35—C36116.5 (3)
C2—C3—C6121.8 (3)C39—C35—C34121.9 (4)
C4—C3—C6121.7 (3)C36—C35—C34121.4 (4)
C5—C4—C3119.8 (3)C37—C36—C35120.1 (4)
C5—C4—H4120.1C37—C36—H36120.0
C3—C4—H4120.1C35—C36—H36120.0
N1—C5—C4124.0 (3)N7—C37—C36123.4 (4)
N1—C5—H5118.0N7—C37—H37118.3
C4—C5—H5118.0C36—C37—H37118.3
C3—C6—C7112.0 (3)N7—C38—C39124.4 (3)
C3—C6—H6A109.2N7—C38—H38117.8
C7—C6—H6A109.2C39—C38—H38117.8
C3—C6—H6B109.2C35—C39—C38119.8 (4)
C7—C6—H6B109.2C35—C39—H39120.1
H6A—C6—H6B107.9C38—C39—H39120.1
C8—C7—C6112.2 (3)N4—C40—C41123.5 (4)
C8—C7—H7A109.2N4—C40—H40118.3
C6—C7—H7A109.2C41—C40—H40118.3
C8—C7—H7B109.2C40—C41—C42121.0 (4)
C6—C7—H7B109.2C40—C41—H41119.5
H7A—C7—H7B107.9C42—C41—H41119.5
C7—C8—C9116.0 (4)C41—C42—C43116.0 (3)
C7—C8—H8A108.3C41—C42—C45121.6 (4)
C9—C8—H8A108.3C43—C42—C45122.4 (4)
C7—C8—H8B108.3C44—C43—C42120.2 (3)
C9—C8—H8B108.3C44—C43—H43119.9
H8A—C8—H8B107.4C42—C43—H43119.9
C13—C9—C10116.4 (4)N4—C44—C43123.1 (3)
C13—C9—C8120.1 (4)N4—C44—H44118.5
C10—C9—C8123.5 (4)C43—C44—H44118.5
C11—C10—C9120.5 (4)C42—C45—C46112.5 (3)
C11—C10—H10119.8C42—C45—H45A109.1
C9—C10—H10119.8C46—C45—H45A109.1
N5—C11—C10122.9 (4)C42—C45—H45B109.1
N5—C11—H11118.6C46—C45—H45B109.1
C10—C11—H11118.6H45A—C45—H45B107.8
N5—C12—C13123.8 (4)C47—C46—C45113.9 (3)
N5—C12—H12118.1C47—C46—H46A108.8
C13—C12—H12118.1C45—C46—H46A108.8
C9—C13—C12120.1 (4)C47—C46—H46B108.8
C9—C13—H13119.9C45—C46—H46B108.8
C12—C13—H13119.9H46A—C46—H46B107.7
N2—C14—C15123.1 (3)C46—C47—C48112.2 (3)
N2—C14—H14118.4C46—C47—H47A109.2
C15—C14—H14118.4C48—C47—H47A109.2
C16—C15—C14120.3 (4)C46—C47—H47B109.2
C16—C15—H15119.8C48—C47—H47B109.2
C14—C15—H15119.8H47A—C47—H47B107.9
C15—C16—C17116.5 (3)C49—C48—C52116.3 (4)
C15—C16—C19122.1 (4)C49—C48—C47121.8 (3)
C17—C16—C19121.4 (4)C52—C48—C47121.8 (4)
C18—C17—C16120.1 (3)C50—C49—C48120.4 (4)
C18—C17—H17120.0C50—C49—H49119.8
C16—C17—H17120.0C48—C49—H49119.8
N2—C18—C17123.1 (3)N8—C50—C49123.2 (4)
N2—C18—H18118.5N8—C50—H50118.4
C17—C18—H18118.5C49—C50—H50118.4
C16—C19—C20111.6 (3)N8—C51—C52123.5 (4)
C16—C19—H19A109.3N8—C51—H51118.2
C20—C19—H19A109.3C52—C51—H51118.2
C16—C19—H19B109.3C51—C52—C48120.2 (4)
C20—C19—H19B109.3C51—C52—H52119.9
H19A—C19—H19B108.0C48—C52—H52119.9
C21—C20—C19114.2 (4)O2—Cl1—O1113.8 (5)
C21—C20—H20A108.7O2—Cl1—O3107.9 (4)
C19—C20—H20A108.7O1—Cl1—O3105.3 (3)
C21—C20—H20B108.7O2—Cl1—O4106.5 (3)
C19—C20—H20B108.7O1—Cl1—O4110.8 (4)
H20A—C20—H20B107.6O3—Cl1—O4112.7 (4)
C20—C21—C22115.6 (3)O5—Cl2—O6112.1 (8)
C20—C21—H21A108.4O5—Cl2—O8105.2 (7)
C22—C21—H21A108.4O6—Cl2—O8108.5 (7)
C20—C21—H21B108.4O5—Cl2—O7104.6 (6)
C22—C21—H21B108.4O6—Cl2—O7111.2 (6)
H21A—C21—H21B107.4O8—Cl2—O7115.0 (6)
C23—C22—C26116.3 (3)O1W—Mn1—O2W173.02 (8)
C23—C22—C21121.6 (3)O1W—Mn1—N189.63 (9)
C26—C22—C21122.1 (3)O2W—Mn1—N192.74 (9)
C22—C23—C24120.0 (4)O1W—Mn1—N288.34 (9)
C22—C23—H23120.0O2W—Mn1—N285.05 (9)
C24—C23—H23120.0N1—Mn1—N291.08 (10)
N6—C24—C23123.4 (4)O1W—Mn1—N494.59 (9)
N6—C24—H24118.3O2W—Mn1—N491.98 (9)
C23—C24—H24118.3N1—Mn1—N490.00 (10)
N6—C25—C26123.9 (4)N2—Mn1—N4176.89 (10)
N6—C25—H25118.1O1W—Mn1—N387.61 (9)
C26—C25—H25118.1O2W—Mn1—N390.15 (9)
C22—C26—C25120.3 (4)N1—Mn1—N3176.97 (10)
C22—C26—H26119.8N2—Mn1—N390.08 (10)
C25—C26—H26119.8N4—Mn1—N388.98 (10)
N3—C27—C28122.9 (4)C5—N1—C1116.4 (3)
N3—C27—H27118.5C5—N1—Mn1122.4 (2)
C28—C27—H27118.5C1—N1—Mn1121.0 (2)
C29—C28—C27120.7 (4)C14—N2—C18116.7 (3)
C29—C28—H28119.6C14—N2—Mn1121.4 (2)
C27—C28—H28119.6C18—N2—Mn1121.0 (2)
C28—C29—C30116.7 (4)C31—N3—C27116.6 (3)
C28—C29—C32122.8 (4)C31—N3—Mn1121.2 (2)
C30—C29—C32120.5 (4)C27—N3—Mn1121.5 (2)
C31—C30—C29119.4 (4)C44—N4—C40116.3 (3)
C31—C30—H30120.3C44—N4—Mn1123.3 (2)
C29—C30—H30120.3C40—N4—Mn1120.4 (2)
N3—C31—C30123.5 (4)C11—N5—C12116.3 (4)
N3—C31—H31118.2C25—N6—C24116.0 (3)
C30—C31—H31118.2C38—N7—C37115.9 (3)
C29—C32—C33111.0 (3)C51—N8—C50116.4 (4)
C29—C32—H32A109.4Mn1—O1W—H1W132.0
C33—C32—H32A109.4Mn1—O1W—H1WA123.2
C29—C32—H32B109.4H1W—O1W—H1WA104.7
C33—C32—H32B109.4Mn1—O2W—H2W130.0
H32A—C32—H32B108.0Mn1—O2W—H2WA130.9
C34—C33—C32117.7 (5)H2W—O2W—H2WA97.7
C34—C33—H33A107.9H3W—O3W—H3WA116.6
C32—C33—H33A107.9H4WA—O4W—H4W108.0
N1—C1—C2—C30.5 (6)C46—C47—C48—C49110.6 (4)
C1—C2—C3—C40.4 (6)C46—C47—C48—C5266.5 (5)
C1—C2—C3—C6178.5 (4)C52—C48—C49—C500.1 (5)
C2—C3—C4—C50.9 (5)C47—C48—C49—C50177.4 (4)
C6—C3—C4—C5178.0 (3)C48—C49—C50—N81.3 (6)
C3—C4—C5—N10.6 (6)N8—C51—C52—C481.0 (6)
C2—C3—C6—C765.5 (5)C49—C48—C52—C511.0 (5)
C4—C3—C6—C7113.3 (4)C47—C48—C52—C51176.3 (4)
C3—C6—C7—C8177.8 (4)C4—C5—N1—C10.3 (5)
C6—C7—C8—C9175.6 (4)C4—C5—N1—Mn1173.9 (3)
C7—C8—C9—C13153.6 (4)C2—C1—N1—C50.9 (5)
C7—C8—C9—C1025.7 (6)C2—C1—N1—Mn1173.5 (3)
C13—C9—C10—C111.4 (6)O1W—Mn1—N1—C540.4 (3)
C8—C9—C10—C11179.2 (4)O2W—Mn1—N1—C5133.0 (3)
C9—C10—C11—N51.7 (7)N2—Mn1—N1—C547.9 (3)
C10—C9—C13—C122.5 (6)N3—Mn1—N1—C564.6 (19)
C8—C9—C13—C12178.0 (4)O1W—Mn1—N1—C1133.6 (3)
N5—C12—C13—C90.9 (7)O2W—Mn1—N1—C153.0 (3)
N2—C14—C15—C160.8 (5)N2—Mn1—N1—C1138.1 (3)
C14—C15—C16—C172.9 (5)N4—Mn1—N1—C139.0 (3)
C14—C15—C16—C19175.5 (3)C15—C14—N2—C183.3 (5)
C15—C16—C17—C184.0 (5)C15—C14—N2—Mn1166.0 (3)
C19—C16—C17—C18174.4 (3)C17—C18—N2—C142.2 (5)
C16—C17—C18—N21.5 (5)C17—C18—N2—Mn1167.2 (3)
C15—C16—C19—C2089.2 (4)O1W—Mn1—N2—C14140.1 (3)
C17—C16—C19—C2089.1 (5)O2W—Mn1—N2—C1442.2 (2)
C16—C19—C20—C2162.9 (5)N1—Mn1—N2—C1450.5 (3)
C19—C20—C21—C22170.3 (3)N3—Mn1—N2—C14132.3 (3)
C20—C21—C22—C2346.7 (6)O1W—Mn1—N2—C1851.0 (2)
C20—C21—C22—C26133.8 (4)O2W—Mn1—N2—C18126.7 (2)
C26—C22—C23—C242.3 (6)N1—Mn1—N2—C18140.6 (2)
C21—C22—C23—C24177.2 (4)N3—Mn1—N2—C1836.6 (2)
C22—C23—C24—N61.5 (6)C30—C31—N3—C272.9 (5)
C23—C22—C26—C251.0 (6)C30—C31—N3—Mn1167.8 (3)
C21—C22—C26—C25178.5 (4)C28—C27—N3—C312.1 (5)
N6—C25—C26—C221.3 (6)C28—C27—N3—Mn1168.6 (3)
N3—C27—C28—C290.4 (6)O1W—Mn1—N3—C3139.2 (3)
C27—C28—C29—C302.1 (5)O2W—Mn1—N3—C31147.4 (3)
C27—C28—C29—C32175.6 (3)N2—Mn1—N3—C31127.5 (3)
C28—C29—C30—C311.3 (5)N4—Mn1—N3—C3155.4 (3)
C32—C29—C30—C31176.5 (3)O1W—Mn1—N3—C27131.1 (3)
C29—C30—C31—N31.3 (6)O2W—Mn1—N3—C2742.3 (3)
C28—C29—C32—C3389.2 (6)N2—Mn1—N3—C2742.8 (3)
C30—C29—C32—C3388.4 (5)N4—Mn1—N3—C27134.2 (3)
C29—C32—C33—C3459.5 (7)C43—C44—N4—C400.3 (5)
C32—C33—C34—C35177.1 (4)C43—C44—N4—Mn1177.0 (3)
C33—C34—C35—C3961.5 (7)C41—C40—N4—C440.4 (5)
C33—C34—C35—C36123.9 (5)C41—C40—N4—Mn1176.4 (3)
C39—C35—C36—C370.9 (6)O1W—Mn1—N4—C4447.2 (3)
C34—C35—C36—C37174.0 (4)O2W—Mn1—N4—C44135.1 (3)
C35—C36—C37—N70.1 (6)N1—Mn1—N4—C4442.4 (3)
C36—C35—C39—C381.4 (6)N3—Mn1—N4—C44134.8 (3)
C34—C35—C39—C38173.5 (4)O1W—Mn1—N4—C40129.3 (3)
N7—C38—C39—C351.1 (7)O2W—Mn1—N4—C4048.3 (3)
N4—C40—C41—C420.0 (6)N2—Mn1—N4—C4031 (2)
C40—C41—C42—C431.1 (5)N3—Mn1—N4—C4041.8 (3)
C40—C41—C42—C45178.1 (4)C10—C11—N5—C123.3 (7)
C41—C42—C43—C441.8 (5)C13—C12—N5—C112.1 (6)
C45—C42—C43—C44177.4 (3)C26—C25—N6—C242.2 (6)
C42—C43—C44—N41.5 (6)C23—C24—N6—C250.8 (6)
C41—C42—C45—C4673.0 (5)C39—C38—N7—C370.0 (6)
C43—C42—C45—C46106.1 (5)C36—C37—N7—C380.6 (6)
C42—C45—C46—C4766.6 (5)C52—C51—N8—C500.2 (6)
C45—C46—C47—C48178.6 (4)C49—C50—N8—C511.3 (6)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3W—H3WA···N8i0.921.862.753 (4)162
O3W—H3W···N5ii0.881.872.738 (4)167
O2W—H2WA···O3Wiii0.851.882.723 (3)178
O2W—H2W···N7iv0.861.982.844 (4)174
O1W—H1W···N6v0.812.082.824 (4)153
O4W—H4W···O40.852.222.975 (9)147
O1W—H1WA···O3W0.801.912.684 (3)163
O4W—H4WA···O60.852.433.035 (14)129
C23—H23···O4iv0.932.533.379 (6)152
C28—H28···O5vi0.932.433.255 (11)148
C39—H39···O80.932.523.214 (9)132
Symmetry codes: (i) x1/2, y+3/2, z; (ii) x+1/2, y+3/2, z; (iii) x+1/2, y+1/2, z; (iv) x+1, y+1/2, z+1/2; (v) x+1, y1/2, z+1/2; (vi) x+3/2, y+1/2, z.

Experimental details

Crystal data
Chemical formula[Mn(C13H14N2)4(H2O)2](ClO4)2·1.5H2O
Mr1108.94
Crystal system, space groupOrthorhombic, Pbca
Temperature (K)293
a, b, c (Å)19.0755 (10), 15.9409 (9), 37.533 (2)
V3)11412.9 (11)
Z8
Radiation typeMo Kα
µ (mm1)0.39
Crystal size (mm)0.30 × 0.30 × 0.10
Data collection
DiffractometerBruker APEXII CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADBAS; Sheldrick, 1996)
Tmin, Tmax0.892, 0.962
No. of measured, independent and
observed [I > 2.σ(I)] reflections
61756, 10065, 6106
Rint0.113
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.057, 0.188, 1.01
No. of reflections10065
No. of parameters676
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.66, 0.47

Computer programs: APEX2 (Bruker, 2008), SAINT (Bruker, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2000), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3W—H3WA···N8i0.921.862.753 (4)162.1
O3W—H3W···N5ii0.881.872.738 (4)166.7
O2W—H2WA···O3Wiii0.851.882.723 (3)177.7
O2W—H2W···N7iv0.861.982.844 (4)174.1
O1W—H1W···N6v0.812.082.824 (4)153.3
O4W—H4W···O40.852.222.975 (9)147.4
O1W—H1WA···O3W0.801.912.684 (3)162.9
O4W—H4WA···O60.852.433.035 (14)128.7
C23—H23···O4iv0.932.533.379 (6)152.0
C28—H28···O5vi0.932.433.255 (11)148.0
C39—H39···O80.932.523.214 (9)132.0
Symmetry codes: (i) x1/2, y+3/2, z; (ii) x+1/2, y+3/2, z; (iii) x+1/2, y+1/2, z; (iv) x+1, y+1/2, z+1/2; (v) x+1, y1/2, z+1/2; (vi) x+3/2, y+1/2, z.
 

Acknowledgements

The authors gratefully acknowledge the Natural Science Foundation of Jiangsu Province of China (BK2008195) for financial support of this work.

References

First citationBrandenburg, K. (2000). DIAMOND. Crystal Impact GbR, Bonn, Germany.  Google Scholar
First citationBruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, wisconsin, USA.  Google Scholar
First citationSheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationZheng, X., Niu, C., Wan, X. & Kou, C. (2007). Acta Cryst. E63, m2682–m2683.  Web of Science CSD CrossRef IUCr Journals Google Scholar

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