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Acta Crystallogr Sect E Struct Rep Online. 2008 September 1; 64(Pt 9): m1158.
Published online 2008 August 13. doi:  10.1107/S1600536808025622
PMCID: PMC2960719

Tetra­aqua­(1,10-phenanthroline)zinc(II) 3,6-dicarboxy­bicyclo­[2.2.2]oct-7-ene-2,5-dicarboxyl­ate

Abstract

In the title compound, [Zn(C12H8N2)(H2O)4](C12H10O8), each ZnII atom is six-coordinated by two N atoms from one phenanthroline mol­ecule and by four O atoms from four water mol­ecules in a distorted octa­hedral environment. In the crystal structure, ions are linked by O—H(...)O hydrogen bonds.

Related literature

For related literature, see: Ma et al. (2003 [triangle]); Hu (2008 [triangle]).

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Object name is e-64-m1158-scheme1.jpg

Experimental

Crystal data

  • [Zn(C12H8N2)(H2O)4](C12H10O8)
  • M r = 599.84
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-m1158-efi1.jpg
  • a = 7.4550 (2) Å
  • b = 13.5991 (4) Å
  • c = 22.9833 (7) Å
  • β = 91.555 (1)°
  • V = 2329.22 (12) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 1.13 mm−1
  • T = 293 (2) K
  • 0.33 × 0.22 × 0.19 mm

Data collection

  • Bruker APEX CCD area-detector diffractometer
  • Absorption correction: multi-scan (SAINT; Bruker, 1998 [triangle]) T min = 0.687, T max = 0.805
  • 14301 measured reflections
  • 5626 independent reflections
  • 3854 reflections with I > 2σ(I)
  • R int = 0.048

Refinement

  • R[F 2 > 2σ(F 2)] = 0.046
  • wR(F 2) = 0.122
  • S = 0.96
  • 5626 reflections
  • 382 parameters
  • 12 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.50 e Å−3
  • Δρmin = −0.59 e Å−3

Data collection: SMART (Bruker, 1998 [triangle]); cell refinement: SAINT (Bruker, 1998 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808025622/bt2766sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808025622/bt2766Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

The authors thank Beihua University for supporting this work.

supplementary crystallographic information

Comment

Recently, complexes with poly(carboxylic acids) have been investigated in the area of solid state and material science (Ma et al., 2003). I selected bicyclo[2.2.2]oct-7-ene-2,3,5,6-tetracarboxylic acid (H4L) as a poly(carboxylic acid) ligand and phenanthroline (phen) as a secondary ligand, generating a new complex, [Zn(phen)(H2O)4].[H2L], which is reported here.

In the title compound, [Zn(phen)(H2O)4].[H2L], each ZnII atom is six-coordinated by two N atoms from one phen molecule, and four O atoms from four water molecules in a distorted octahedral environment. Each H2L2- acts as a counter-anion. In the crystal, the molecules are linked by O—H···O hydrogen bonds.

Experimental

A mixture of H4L (0.5 mmol), phen (0.5 mmol), NaOH (1 mmol) and ZnCl2.6H2O (0.5 mmol) was suspended in 12 ml of deionized water and sealed in a 20-ml Teflon-lined autoclave. Upon heating at 140°C for one week, the autoclave was slowly cooled to room temperature. The crystals were collected, washed with deionized water and dried.

Refinement

All H atoms on C atoms were positioned geometrically (C—H = 0.93 Å) and refined as riding, with Uiso(H)=1.2Ueq(carrier). The water H-atoms were located in a difference Fourier map, and were refined with distance restraints of O–H = 0.85±0.01 Å; their displacement parameters were set to 1.2Ueq(O).

Figures

Fig. 1.
The structure of the title compound, showing the atomic numbering scheme. Displacement ellipsoids are drawn at the 30% probability level.

Crystal data

[Zn(C12H8N2)(H2O)4](C12H10O8)F000 = 1240
Mr = 599.84Dx = 1.711 Mg m3
Monoclinic, P21/cMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 5626 reflections
a = 7.4550 (2) Åθ = 1.1–28.3º
b = 13.5991 (4) ŵ = 1.13 mm1
c = 22.9833 (7) ÅT = 293 (2) K
β = 91.5550 (10)ºBlock, colorless
V = 2329.22 (12) Å30.33 × 0.22 × 0.19 mm
Z = 4

Data collection

Bruker APEX CCD area-detector diffractometer5626 independent reflections
Radiation source: fine-focus sealed tube3854 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.048
T = 293(2) Kθmax = 28.3º
[var phi] and ω scansθmin = 1.7º
Absorption correction: multi-scan(SAINT; Bruker, 1998)h = −9→8
Tmin = 0.687, Tmax = 0.805k = −14→18
14301 measured reflectionsl = −29→30

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.046H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.122  w = 1/[σ2(Fo2) + (0.0613P)2] where P = (Fo2 + 2Fc2)/3
S = 0.96(Δ/σ)max < 0.001
5626 reflectionsΔρmax = 0.50 e Å3
382 parametersΔρmin = −0.59 e Å3
12 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods

Special details

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)

xyzUiso*/Ueq
C1−0.2556 (4)0.2855 (2)0.61401 (12)0.0348 (7)
H1−0.25290.22640.63440.042*
C2−0.2659 (4)0.3745 (3)0.64532 (13)0.0414 (8)
H2−0.27080.37340.68570.050*
C4−0.2686 (5)0.4609 (3)0.61680 (15)0.0459 (9)
H4−0.27560.51940.63760.055*
C5−0.2610 (5)0.4632 (2)0.55588 (14)0.0399 (8)
C6−0.2629 (6)0.5510 (2)0.52184 (18)0.0570 (10)
H6−0.26280.61170.54050.068*
C7−0.2648 (6)0.5479 (2)0.46388 (18)0.0554 (10)
H7−0.26920.60640.44300.067*
C8−0.2603 (5)0.4564 (2)0.43289 (15)0.0385 (8)
C9−0.2666 (4)0.4472 (2)0.37212 (14)0.0409 (8)
H9−0.27270.50320.34890.049*
C10−0.2639 (4)0.3579 (2)0.34720 (13)0.0377 (8)
H10−0.26940.35230.30690.045*
C11−0.2527 (4)0.2731 (2)0.38191 (12)0.0307 (7)
H11−0.25020.21180.36410.037*
C12−0.2538 (4)0.3703 (2)0.52783 (12)0.0272 (6)
C13−0.2518 (4)0.3674 (2)0.46512 (12)0.0271 (6)
C140.1068 (4)0.06219 (19)0.70078 (12)0.0268 (6)
C150.2475 (4)0.12469 (19)0.73318 (11)0.0220 (6)
H150.32950.08080.75480.026*
C160.3605 (4)0.19231 (18)0.69329 (10)0.0206 (5)
H160.48690.17840.70270.025*
C170.3320 (4)0.1720 (2)0.62817 (11)0.0252 (6)
C180.3279 (3)0.30060 (18)0.70964 (10)0.0187 (5)
H180.38940.34450.68290.022*
C190.1500 (4)0.19201 (18)0.77770 (11)0.0209 (5)
H190.07440.15240.80290.025*
C200.0380 (4)0.26442 (19)0.74361 (11)0.0243 (6)
H20−0.08570.26920.74690.029*
C0210.2081 (4)0.3018 (2)0.86562 (11)0.0234 (6)
C210.1303 (4)0.32112 (19)0.70833 (11)0.0245 (6)
H210.07730.36930.68490.029*
C220.4016 (4)0.31473 (18)0.77246 (11)0.0211 (5)
H220.52460.28920.77320.025*
C230.4151 (4)0.4227 (2)0.79029 (11)0.0262 (6)
C250.2936 (4)0.24790 (18)0.81443 (10)0.0216 (6)
H250.37710.19900.83090.026*
N1−0.2458 (3)0.27831 (16)0.43985 (9)0.0246 (5)
N2−0.2495 (3)0.28378 (17)0.55612 (9)0.0255 (5)
O10.2699 (3)0.23710 (15)0.59560 (8)0.0417 (6)
O20.3860 (3)0.08866 (14)0.60983 (8)0.0348 (5)
O1W−0.4920 (3)0.13197 (19)0.49279 (10)0.0375 (5)
O30.1019 (3)−0.02720 (15)0.72076 (9)0.0469 (6)
H30.0255−0.05870.70240.070*
O2W−0.1668 (4)0.06205 (18)0.43708 (11)0.0422 (6)
O40.0122 (3)0.09170 (16)0.66157 (10)0.0473 (6)
O3W−0.2116 (4)0.0585 (2)0.56396 (12)0.0490 (6)
O50.3699 (3)0.49114 (14)0.76039 (9)0.0399 (5)
O4W0.0517 (3)0.17941 (19)0.50606 (9)0.0401 (6)
O60.4927 (3)0.42964 (15)0.84189 (8)0.0374 (5)
H6A0.49950.48770.85140.056*
O70.2531 (3)0.27139 (14)0.91541 (8)0.0336 (5)
O80.0968 (3)0.36877 (15)0.85579 (8)0.0371 (5)
Zn1−0.22063 (5)0.16487 (2)0.499735 (13)0.02916 (12)
HW22−0.223 (4)0.013 (2)0.4325 (16)0.063 (13)*
HW410.113 (5)0.198 (3)0.5355 (10)0.095*
HW21−0.092 (4)0.069 (3)0.4124 (14)0.074 (15)*
HW420.109 (4)0.195 (2)0.4781 (9)0.037 (10)*
HW12−0.551 (4)0.168 (2)0.4714 (11)0.043 (11)*
HW11−0.551 (5)0.118 (3)0.5214 (12)0.079 (15)*
HW31−0.282 (6)0.057 (3)0.5893 (17)0.119*
HW32−0.195 (6)0.009 (2)0.5475 (17)0.083 (18)*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
C10.0317 (17)0.049 (2)0.0242 (14)0.0001 (14)0.0003 (12)−0.0013 (14)
C20.0318 (18)0.067 (2)0.0255 (15)0.0106 (16)−0.0019 (13)−0.0162 (16)
C40.043 (2)0.049 (2)0.0447 (19)0.0084 (16)−0.0065 (16)−0.0268 (17)
C50.045 (2)0.0296 (17)0.0447 (19)0.0040 (14)−0.0066 (15)−0.0126 (15)
C60.079 (3)0.0198 (17)0.072 (3)0.0021 (16)−0.007 (2)−0.0094 (18)
C70.074 (3)0.0221 (18)0.070 (3)0.0012 (17)−0.004 (2)0.0069 (17)
C80.044 (2)0.0230 (16)0.0478 (19)−0.0010 (13)−0.0031 (15)0.0094 (14)
C90.041 (2)0.0408 (19)0.0404 (18)−0.0060 (15)−0.0033 (15)0.0234 (15)
C100.0336 (18)0.054 (2)0.0251 (15)0.0009 (14)0.0010 (13)0.0107 (15)
C110.0318 (16)0.0369 (17)0.0235 (14)0.0024 (13)−0.0001 (12)0.0001 (13)
C120.0309 (16)0.0223 (14)0.0283 (15)−0.0003 (11)−0.0022 (12)−0.0038 (12)
C130.0319 (16)0.0208 (14)0.0283 (14)−0.0005 (11)−0.0027 (12)0.0022 (12)
C140.0353 (17)0.0180 (14)0.0273 (14)−0.0034 (11)0.0054 (13)−0.0008 (11)
C150.0283 (15)0.0176 (13)0.0201 (13)−0.0006 (10)0.0004 (11)0.0004 (10)
C160.0236 (14)0.0201 (13)0.0180 (12)0.0012 (10)0.0012 (11)0.0023 (10)
C170.0331 (16)0.0264 (15)0.0161 (12)−0.0042 (12)−0.0006 (11)−0.0004 (11)
C180.0241 (14)0.0152 (12)0.0167 (12)−0.0037 (10)0.0017 (10)0.0019 (10)
C190.0234 (14)0.0178 (13)0.0218 (13)−0.0028 (10)0.0054 (11)0.0012 (10)
C200.0220 (14)0.0252 (14)0.0255 (14)0.0014 (11)−0.0029 (11)−0.0002 (11)
C0210.0296 (15)0.0219 (14)0.0188 (13)−0.0019 (11)0.0028 (11)−0.0009 (11)
C210.0279 (15)0.0220 (14)0.0233 (13)0.0030 (11)−0.0051 (11)0.0010 (11)
C220.0233 (14)0.0196 (13)0.0203 (13)0.0002 (10)−0.0001 (11)0.0007 (10)
C230.0341 (16)0.0241 (15)0.0204 (13)−0.0099 (12)0.0031 (12)−0.0014 (11)
C250.0248 (14)0.0187 (13)0.0213 (13)0.0027 (10)0.0006 (11)0.0001 (11)
N10.0286 (13)0.0241 (12)0.0212 (11)0.0011 (10)−0.0006 (9)0.0011 (10)
N20.0282 (13)0.0278 (13)0.0203 (11)0.0000 (10)−0.0019 (9)−0.0015 (10)
O10.0729 (17)0.0249 (11)0.0264 (10)−0.0026 (10)−0.0152 (11)0.0063 (9)
O20.0529 (14)0.0266 (11)0.0248 (10)0.0048 (9)−0.0025 (10)−0.0068 (9)
O1W0.0282 (12)0.0574 (16)0.0270 (12)−0.0047 (11)0.0014 (10)0.0052 (11)
O30.0640 (17)0.0305 (12)0.0454 (13)−0.0204 (11)−0.0111 (12)0.0083 (10)
O2W0.0487 (16)0.0325 (14)0.0457 (14)−0.0005 (11)0.0034 (12)−0.0171 (11)
O40.0527 (15)0.0370 (13)0.0507 (14)−0.0078 (11)−0.0267 (12)0.0000 (11)
O3W0.0611 (18)0.0372 (15)0.0482 (15)−0.0090 (12)−0.0082 (13)0.0157 (13)
O50.0610 (16)0.0250 (11)0.0330 (11)−0.0052 (10)−0.0117 (10)0.0037 (9)
O4W0.0259 (12)0.0736 (18)0.0208 (10)−0.0078 (11)0.0007 (9)0.0006 (11)
O60.0551 (15)0.0235 (11)0.0328 (11)−0.0068 (9)−0.0142 (10)−0.0010 (9)
O70.0495 (14)0.0329 (12)0.0184 (9)0.0085 (10)0.0031 (9)0.0025 (8)
O80.0507 (14)0.0341 (12)0.0267 (11)0.0174 (10)0.0063 (10)0.0014 (9)
Zn10.0328 (2)0.0265 (2)0.0280 (2)0.00085 (14)−0.00117 (14)0.00085 (14)

Geometric parameters (Å, °)

C1—N21.333 (3)C18—C211.499 (4)
C1—C21.410 (4)C18—C221.543 (3)
C1—H10.9300C18—H180.9800
C2—C41.346 (5)C19—C201.498 (4)
C2—H20.9300C19—C251.545 (4)
C4—C51.403 (5)C19—H190.9800
C4—H40.9300C20—C211.325 (4)
C5—C121.420 (4)C20—H200.9300
C5—C61.428 (5)C021—O81.248 (3)
C6—C71.333 (6)C021—O71.254 (3)
C6—H60.9300C021—C251.539 (3)
C7—C81.434 (5)C21—H210.9300
C7—H70.9300C22—C231.526 (3)
C8—C91.402 (4)C22—C251.564 (3)
C8—C131.419 (4)C22—H220.9800
C9—C101.343 (4)C23—O51.200 (3)
C9—H90.9300C23—O61.309 (3)
C10—C111.403 (4)C25—H250.9800
C10—H100.9300N1—Zn12.073 (2)
C11—N11.333 (3)N2—Zn12.087 (2)
C11—H110.9300O1W—Zn12.074 (2)
C12—N21.344 (3)O1W—HW120.816 (17)
C12—C131.442 (4)O1W—HW110.826 (18)
C13—N11.345 (3)O3—H30.8200
C14—O41.198 (3)O2W—Zn12.055 (2)
C14—O31.300 (3)O2W—HW220.799 (17)
C14—C151.528 (4)O2W—HW210.809 (17)
C15—C161.561 (3)O3W—Zn12.067 (2)
C15—C191.567 (3)O3W—HW310.80 (4)
C15—H150.9800O3W—HW320.784 (18)
C16—C171.531 (3)O4W—Zn12.041 (2)
C16—C181.541 (3)O4W—HW410.845 (18)
C16—H160.9800O4W—HW420.811 (17)
C17—O11.240 (3)O6—H6A0.8200
C17—O21.279 (3)
N2—C1—C2121.9 (3)C20—C19—H19110.4
N2—C1—H1119.1C25—C19—H19110.4
C2—C1—H1119.1C15—C19—H19110.4
C4—C2—C1120.0 (3)C21—C20—C19114.3 (2)
C4—C2—H2120.0C21—C20—H20122.9
C1—C2—H2120.0C19—C20—H20122.9
C2—C4—C5120.3 (3)O8—C021—O7124.5 (2)
C2—C4—H4119.8O8—C021—C25119.8 (2)
C5—C4—H4119.8O7—C021—C25115.7 (2)
C4—C5—C12115.9 (3)C20—C21—C18113.9 (2)
C4—C5—C6124.4 (3)C20—C21—H21123.0
C12—C5—C6119.7 (3)C18—C21—H21123.0
C7—C6—C5121.4 (3)C23—C22—C18113.0 (2)
C7—C6—H6119.3C23—C22—C25115.1 (2)
C5—C6—H6119.3C18—C22—C25109.2 (2)
C6—C7—C8121.7 (3)C23—C22—H22106.3
C6—C7—H7119.2C18—C22—H22106.3
C8—C7—H7119.2C25—C22—H22106.3
C9—C8—C13116.4 (3)O5—C23—O6124.9 (3)
C9—C8—C7124.9 (3)O5—C23—C22125.2 (2)
C13—C8—C7118.8 (3)O6—C23—C22109.7 (2)
C10—C9—C8120.3 (3)C021—C25—C19110.9 (2)
C10—C9—H9119.8C021—C25—C22115.2 (2)
C8—C9—H9119.8C19—C25—C22108.0 (2)
C9—C10—C11120.1 (3)C021—C25—H25107.5
C9—C10—H10119.9C19—C25—H25107.5
C11—C10—H10119.9C22—C25—H25107.5
N1—C11—C10121.6 (3)C11—N1—C13118.6 (2)
N1—C11—H11119.2C11—N1—Zn1128.64 (19)
C10—C11—H11119.2C13—N1—Zn1112.79 (17)
N2—C12—C5124.0 (3)C1—N2—C12117.8 (3)
N2—C12—C13117.4 (2)C1—N2—Zn1129.8 (2)
C5—C12—C13118.6 (3)C12—N2—Zn1112.28 (17)
N1—C13—C8123.0 (3)Zn1—O1W—HW12115 (2)
N1—C13—C12117.2 (2)Zn1—O1W—HW11122 (3)
C8—C13—C12119.8 (3)HW12—O1W—HW11109 (3)
O4—C14—O3123.8 (3)C14—O3—H3109.5
O4—C14—C15124.2 (2)Zn1—O2W—HW22124 (3)
O3—C14—C15111.9 (2)Zn1—O2W—HW21124 (3)
C14—C15—C16114.5 (2)HW22—O2W—HW21112 (3)
C14—C15—C19108.6 (2)Zn1—O3W—HW31122 (4)
C16—C15—C19107.85 (19)Zn1—O3W—HW32105 (3)
C14—C15—H15108.6HW31—O3W—HW32117 (3)
C16—C15—H15108.6Zn1—O4W—HW41127 (3)
C19—C15—H15108.6Zn1—O4W—HW42121 (2)
C17—C16—C18113.1 (2)HW41—O4W—HW42106 (3)
C17—C16—C15113.9 (2)C23—O6—H6A109.5
C18—C16—C15109.2 (2)O4W—Zn1—O2W84.42 (10)
C17—C16—H16106.7O4W—Zn1—O3W90.23 (10)
C18—C16—H16106.7O2W—Zn1—O3W91.20 (12)
C15—C16—H16106.7O4W—Zn1—N192.69 (9)
O1—C17—O2123.3 (2)O2W—Zn1—N193.26 (10)
O1—C17—C16120.1 (2)O3W—Zn1—N1174.89 (11)
O2—C17—C16116.4 (2)O4W—Zn1—O1W173.09 (10)
C21—C18—C16109.5 (2)O2W—Zn1—O1W90.46 (10)
C21—C18—C22108.7 (2)O3W—Zn1—O1W85.22 (10)
C16—C18—C22107.0 (2)N1—Zn1—O1W92.24 (9)
C21—C18—H18110.5O4W—Zn1—N290.00 (9)
C16—C18—H18110.5O2W—Zn1—N2171.08 (10)
C22—C18—H18110.5O3W—Zn1—N295.79 (11)
C20—C19—C25109.3 (2)N1—Zn1—N280.02 (9)
C20—C19—C15107.7 (2)O1W—Zn1—N295.62 (9)
C25—C19—C15108.5 (2)

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O3—H3···O8i0.821.882.674 (3)163
O6—H6A···O2ii0.821.842.583 (3)151
O2W—HW22···O2iii0.799 (17)2.06 (2)2.818 (3)158 (4)
O4W—HW41···O10.845 (18)1.86 (2)2.705 (3)174 (4)
O2W—HW21···O8iv0.809 (17)2.121 (18)2.904 (3)163 (4)
O4W—HW42···O7iv0.811 (17)1.876 (17)2.686 (3)177 (3)
O1W—HW12···O7v0.816 (17)2.09 (2)2.884 (3)165 (3)
O1W—HW11···O2vi0.826 (18)2.13 (2)2.923 (3)160 (4)
O3W—HW31···O2vi0.80 (4)2.57 (4)3.233 (4)142 (5)

Symmetry codes: (i) −x, y−1/2, −z+3/2; (ii) −x+1, y+1/2, −z+3/2; (iii) −x, −y, −z+1; (iv) x, −y+1/2, z−1/2; (v) x−1, −y+1/2, z−1/2; (vi) x−1, y, z.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BT2766).

References

  • Bruker (1998). SMART and SAINT Bruker AXS Inc., Madison, Wisconsin, USA.
  • Hu, T. (2008). Acta Cryst. E64, o1021. [PMC free article] [PubMed]
  • Ma, J.-F., Yang, J., Zheng, G.-L., Li, L. & Liu, J.-F. (2003). Inorg. Chem.42, 7531–7534. [PubMed]
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]

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