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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 67| Part 5| May 2011| Pages m569-m570

catena-Poly[diimidazolium [bis­­(μ-pyridine-2,5-di­carboxyl­ato)bis­­[di­aqua­praseodymate(III)]]-bis­­(μ-pyridine-2,5-di­carboxyl­ato)]

aQinghai Institute of Salt Lakes, Chinese Academy of Sciences, Xining 810008, People's Republic of China, and bKey Laboratory of Organic Synthesis of Jiangsu Province, College of Chemistry and Chemical Engineering, Soochow University, Suzhou 215123, People's Republic of China
*Correspondence e-mail: liyahong@suda.edu.cn

(Received 24 March 2011; accepted 3 April 2011; online 13 April 2011)

The title compound {(C3H5N2)2[Pr2(C7H3NO4)4(H2O)4]}n, has a chain structure featuring a dimeric unit consisting of two PrIII atoms within a dodecahedral environment. Each of the metal cations is coordinated by two N atoms and two O atoms from two pyridine-2,5-dicarboxyl­ate ligands, two O atoms from another two pyridine-2,5-dicarboxyl­ate ligands and two water O atoms. The PrIII ions are bridged by two ligands along the c axis, forming the dimeric unit, and these are connected by four ligands along the b axis, forming a chain. N—H⋯O and O—H⋯O hydrogen bonds are found in the structure.

Related literature

For praseodymium complexes with pyridine-dicarboxylate ligands, see: Chen et al. (2011[Chen, Y., She, S., Zheng, L., Hu, B., Chen, W., Xu, B., Chen, Z., Zhou, F. & Li, Y. (2011). Polyhedron. doi:10.1016/j.poly.2011.02.017.]); Zhao et al. (2009[Zhao, X.-Q., Zuo, Y., Gao, D.-L., Zhao, B., Shi, W. & Cheng, P. (2009). Cryst. Growth Des. 9, 3948-3957.]); Song et al. (2006[Song, Y.-S., Yan, B. & Weng, L.-H. (2006). Inorg. Chem. Commun. 9, 567-570.]); Chi et al. (2009[Chi, Y.-X., Niu, S.-Y. & Jin, J. (2009). Inorg. Chim. Acta, 362, 3821-3828.]). For complexes with similar structures, see: Li, Zhang et al. (2009[Li, S., Zhang, F.-L., Wang, S.-B. & Bai, H.-L. (2009). Acta Cryst. E65, m410.]); Li, Chen et al. (2009[Li, S., Chen, Y., He, H.-M. & Ma, Y.-F. (2009). Acta Cryst. E65, m411.]); Huang et al. (2009[Huang, Y.-G., Jiang, F.-L., Yuan, D.-Q., Wu, M.-Y., Gao, Q., Wei, W. & Hong, M.-C. (2009). J. Solid State Chem. 182, 215-222.]); Zhang et al. (2005[Zhang, X., Huang, D., Chen, C., Liu, Q., Liao, D. & Li, L. (2005). Inorg. Chem. Commun. 8, 22-26.], 2007[Zhang, F., Yu, B., Wang, X.-Q., Shen, G.-Q. & Shen, D.-Z. (2007). Acta Cryst. E63, m2069-m2070.]).

[Scheme 1]

Experimental

Crystal data
  • (C3H5N2)2[Pr2(C7H3NO4)4(H2O)4]

  • Mr = 1152.48

  • Triclinic, [P \overline 1]

  • a = 9.5444 (19) Å

  • b = 10.667 (2) Å

  • c = 11.222 (2) Å

  • α = 64.63 (3)°

  • β = 79.50 (3)°

  • γ = 87.50 (3)°

  • V = 1014.3 (3) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 2.47 mm−1

  • T = 293 K

  • 0.19 × 0.16 × 0.09 mm

Data collection
  • Bruker SMART CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2001[Bruker (2001). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.652, Tmax = 0.809

  • 14917 measured reflections

  • 3561 independent reflections

  • 3468 reflections with I > 2σ(I)

  • Rint = 0.020

Refinement
  • R[F2 > 2σ(F2)] = 0.015

  • wR(F2) = 0.043

  • S = 1.04

  • 3561 reflections

  • 305 parameters

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 0.33 e Å−3

  • Δρmin = −0.45 e Å−3

Table 1
Selected geometric parameters (Å, °)

Pr1—O5 2.3835 (17)
Pr1—O4i 2.4193 (16)
Pr1—O7ii 2.4366 (16)
Pr1—O1 2.4407 (15)
Pr1—O10 2.4643 (18)
Pr1—O9 2.459 (2)
Pr1—N1 2.6484 (18)
Pr1—N2 2.677 (2)
Symmetry codes: (i) x-1, y, z; (ii) -x+1, -y, -z+1.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
N4—H4⋯O2iv 0.86 1.85 2.679 (3) 160
N3—H3A⋯O6v 0.86 1.88 2.735 (3) 172
N3—H3A⋯O5v 0.86 2.59 3.063 (3) 115
O9—H9A⋯O1vi 0.77 (3) 1.98 (3) 2.743 (3) 172 (3)
O10—H10A⋯O3i 0.88 (4) 1.77 (4) 2.645 (3) 173 (3)
O10—H10A⋯O4i 0.88 (4) 2.44 (3) 2.894 (3) 113 (3)
O10—H10B⋯O3ii 0.73 (4) 2.10 (4) 2.789 (3) 157 (4)
O9—H9B⋯O8ii 0.73 (3) 1.96 (4) 2.644 (3) 157 (3)
Symmetry codes: (i) x-1, y, z; (ii) -x+1, -y, -z+1; (iv) x, y, z-1; (v) -x, -y+1, -z+1; (vi) -x, -y, -z+2.

Data collection: SMART (Bruker, 2001[Bruker (2001). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2001[Bruker (2001). SMART, SAINT and SADABS. 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: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

Pyridine-dicarboxylic acids as multidentate ligands containing N– and O– donors, have been widely used in preparing many kinds of coordination complexes especially in complexes containing rare earth metals (Chen et al. 2011, Zhao et al. 2009). Many complexes based on pyridine-2,5-dicarboxylic acid have been prepared (Li, Zhang et al. 2009, Li, Chen et al. 2009, Huang et al. 2009, Zhang et al. 2007, Zhang et al. 2005), but no complex containing Pr elememt, except two 3 d-4f complexes (Song et al. 2006, Chi et al. 2009) was reported. The reaction of pyridine-2,5-dicarboxylic acid with praseodymium salt under hydrothermal conditions results in the formation of a complex formulated as {(C3N2H5)[(C7H3NO4)2Pr(H2O)2]}n, and the complex has been structurally characterized by elemental analysis and X-ray diffraction. The structure of 1 viewed down the b-axis was presented in Fig. 2. Hydrogen banding packing diagram of 1 view down the b-axis was shown in Fig. 3. Selected band lengthes and angles were summarized inTable 1. The distances of the hydrogen bands were listed in Table 2.

Related literature top

For the use of pyridine-dicarboxylic acids ligands in praseodymium complexes, see: Chen et al. (2011); Zhao et al. (2009); Song et al. (2006); Chi et al. (2009). For complexes with similar structures, see: Li, Zhang et al. (2009); Li, Chen et al. (2009); Huang et al. (2009); Zhang et al. (2005, 2007).

Experimental top

The compound 1 was synthesized by solvothermal reaction. A mixture of pyridine-2,5-dicarboxylic acid (0.0334 g, 0.2 mmol), Pr(NO3)3.6H2O (0.0230 g, 0.05 mmol), imidazole (0.0361 g, 0.53 mmol) and water (3 ml) was sealed in a 7 ml glass tube and heated to 120 oC for 96 h. After cooling to room temperature, light green crystals were obtained.

Refinement top

Hydroxy H atoms were placed in calculated positions with O—H = 0.85 Å, and torsion angles were refined, Water H atoms were placed through fourier electronic density, Uiso(H) = 1.5 Ueq(O). Other H atoms were placed in calculated positions with C—H = 0.93 (aromatic and imidazole), N—H = 0.86 (imidazole)and refined in riding mode, with Uiso(H) = 1.2 Ueq(C or N).

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); 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 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. Molecular structure of 1 showing 50% probability displacement ellipsoids.
[Figure 2] Fig. 2. One-dimensional chain structure of 1 viewed down the b-axis
[Figure 3] Fig. 3. Hydrogen bonding packing diagram of 1 viewed down the b-axis.
catena-Poly[diimidazolium [bis(µ-pyridine-2,5-dicarboxylato)bis[diaquapraseodymate(III)]]-bis(µ- pyridine-2,5-dicarboxylato)] top
Crystal data top
(C3H5N2)2[Pr2(C7H3NO4)4(H2O)4]Z = 1
Mr = 1152.48F(000) = 568
Triclinic, P1char
Hall symbol: -p 1Dx = 1.887 Mg m3
a = 9.5444 (19) ÅMo Kα radiation, λ = 0.71073 Å
b = 10.667 (2) ÅCell parameters from 3561 reflections
c = 11.222 (2) Åθ = 2.6–25.5°
α = 64.63 (3)°µ = 2.47 mm1
β = 79.50 (3)°T = 293 K
γ = 87.50 (3)°Block, light green
V = 1014.3 (3) Å30.19 × 0.16 × 0.09 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
3561 independent reflections
Radiation source: fine-focus sealed tube3468 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
ω scansθmax = 25.0°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 1111
Tmin = 0.652, Tmax = 0.809k = 1212
14917 measured reflectionsl = 1313
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)] = 0.015Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.043H atoms treated by a mixture of independent and constrained refinement
S = 1.04 w = 1/[σ2(Fo2) + (0.0271P)2 + 0.5143P]
where P = (Fo2 + 2Fc2)/3
3561 reflections(Δ/σ)max = 0.068
305 parametersΔρmax = 0.33 e Å3
0 restraintsΔρmin = 0.45 e Å3
Crystal data top
(C3H5N2)2[Pr2(C7H3NO4)4(H2O)4]γ = 87.50 (3)°
Mr = 1152.48V = 1014.3 (3) Å3
Triclinic, P1Z = 1
a = 9.5444 (19) ÅMo Kα radiation
b = 10.667 (2) ŵ = 2.47 mm1
c = 11.222 (2) ÅT = 293 K
α = 64.63 (3)°0.19 × 0.16 × 0.09 mm
β = 79.50 (3)°
Data collection top
Bruker SMART CCD area-detector
diffractometer
3561 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
3468 reflections with I > 2σ(I)
Tmin = 0.652, Tmax = 0.809Rint = 0.020
14917 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0150 restraints
wR(F2) = 0.043H atoms treated by a mixture of independent and constrained refinement
S = 1.04Δρmax = 0.33 e Å3
3561 reflectionsΔρmin = 0.45 e Å3
305 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*/Ueq
Pr10.194718 (10)0.107410 (10)0.725374 (9)0.01889 (5)
O10.17790 (15)0.14537 (16)0.92701 (14)0.0277 (3)
N10.43859 (18)0.13489 (18)0.79437 (16)0.0228 (4)
O40.94311 (15)0.15185 (18)0.73503 (16)0.0337 (4)
N20.36969 (19)0.25158 (18)0.49260 (17)0.0250 (4)
C50.5686 (2)0.1198 (2)0.7350 (2)0.0252 (4)
H50.57610.09490.66420.030*
O90.0720 (2)0.1109 (2)0.89507 (19)0.0386 (4)
O50.19850 (19)0.35430 (16)0.63801 (16)0.0379 (4)
O100.1175 (2)0.0591 (2)0.5508 (2)0.0473 (5)
C70.8356 (2)0.1232 (2)0.7005 (2)0.0263 (5)
O30.83952 (17)0.0841 (2)0.60974 (18)0.0429 (4)
C10.4287 (2)0.1698 (2)0.89743 (19)0.0205 (4)
C60.2795 (2)0.1837 (2)0.9634 (2)0.0248 (4)
O60.2580 (2)0.57179 (18)0.49073 (19)0.0560 (6)
C20.5464 (2)0.1908 (2)0.9421 (2)0.0269 (5)
H20.53610.21521.01330.032*
C40.6928 (2)0.1394 (2)0.7731 (2)0.0223 (4)
C80.3728 (2)0.3897 (2)0.4479 (2)0.0291 (5)
O20.26769 (19)0.2280 (2)1.0488 (2)0.0498 (5)
C130.2689 (3)0.4449 (2)0.5310 (2)0.0325 (5)
C30.6802 (2)0.1750 (2)0.8796 (2)0.0264 (4)
H30.76110.18820.90880.032*
C120.4576 (2)0.1982 (2)0.4206 (2)0.0263 (4)
H120.45420.10250.44940.032*
N40.0958 (3)0.3420 (3)0.1892 (2)0.0493 (6)
H40.13340.29300.14850.059*
C150.0147 (3)0.3044 (3)0.2871 (3)0.0434 (6)
H150.06510.21960.32460.052*
C170.0534 (4)0.5118 (3)0.2475 (4)0.0757 (12)
H170.05780.59610.25290.091*
N30.0426 (3)0.4050 (2)0.3233 (2)0.0471 (6)
H3A0.11100.40390.38540.056*
C160.1408 (4)0.4721 (3)0.1631 (4)0.0760 (12)
H160.21770.52370.09870.091*
C110.5533 (2)0.2772 (2)0.3059 (2)0.0262 (5)
C140.6545 (2)0.2095 (2)0.2339 (2)0.0259 (4)
C100.5552 (3)0.4201 (3)0.2616 (3)0.0439 (7)
H100.61760.47690.18450.053*
C90.4634 (3)0.4765 (2)0.3334 (3)0.0460 (7)
H90.46240.57220.30510.055*
O80.7309 (2)0.28565 (18)0.12655 (17)0.0446 (5)
O70.65553 (16)0.07807 (15)0.28965 (15)0.0308 (3)
H9A0.002 (4)0.129 (3)0.946 (3)0.041 (8)*
H10A0.025 (4)0.069 (3)0.564 (3)0.062 (10)*
H10B0.149 (4)0.034 (4)0.501 (4)0.066 (12)*
H9B0.111 (4)0.174 (3)0.904 (3)0.047 (10)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pr10.01230 (7)0.02507 (7)0.02203 (7)0.00136 (5)0.00114 (5)0.01435 (5)
O10.0164 (7)0.0434 (9)0.0278 (7)0.0005 (6)0.0028 (6)0.0218 (7)
N10.0155 (8)0.0325 (9)0.0258 (8)0.0028 (7)0.0017 (7)0.0184 (7)
O40.0152 (8)0.0515 (10)0.0452 (9)0.0058 (7)0.0054 (7)0.0313 (8)
N20.0237 (9)0.0243 (9)0.0255 (8)0.0045 (7)0.0023 (7)0.0122 (7)
C50.0183 (11)0.0369 (12)0.0272 (10)0.0040 (9)0.0011 (8)0.0213 (9)
O90.0263 (9)0.0326 (10)0.0447 (10)0.0001 (8)0.0163 (8)0.0139 (8)
O50.0420 (10)0.0259 (8)0.0365 (9)0.0040 (7)0.0156 (7)0.0139 (7)
O100.0226 (10)0.0907 (16)0.0575 (12)0.0071 (9)0.0061 (8)0.0598 (12)
C70.0170 (11)0.0327 (11)0.0320 (11)0.0055 (9)0.0022 (9)0.0178 (9)
O30.0201 (8)0.0775 (13)0.0533 (10)0.0061 (8)0.0017 (7)0.0512 (10)
C10.0184 (10)0.0224 (9)0.0210 (9)0.0024 (8)0.0003 (8)0.0113 (8)
C60.0210 (11)0.0292 (11)0.0259 (10)0.0025 (9)0.0015 (8)0.0157 (9)
O60.0734 (14)0.0263 (9)0.0484 (11)0.0104 (9)0.0250 (10)0.0122 (8)
C20.0255 (11)0.0359 (12)0.0248 (10)0.0018 (9)0.0016 (9)0.0192 (9)
C40.0166 (10)0.0255 (10)0.0240 (10)0.0028 (8)0.0013 (8)0.0111 (8)
C80.0301 (12)0.0260 (11)0.0286 (11)0.0062 (9)0.0020 (9)0.0126 (9)
O20.0279 (9)0.0867 (14)0.0640 (12)0.0029 (9)0.0032 (8)0.0643 (12)
C130.0342 (13)0.0275 (12)0.0332 (11)0.0086 (10)0.0041 (10)0.0155 (10)
C30.0187 (10)0.0351 (11)0.0300 (10)0.0024 (9)0.0059 (8)0.0177 (9)
C120.0277 (11)0.0218 (10)0.0274 (10)0.0045 (9)0.0025 (9)0.0117 (9)
N40.0505 (14)0.0556 (14)0.0455 (13)0.0149 (12)0.0073 (11)0.0326 (11)
C150.0455 (16)0.0406 (14)0.0449 (14)0.0077 (12)0.0026 (12)0.0239 (12)
C170.080 (3)0.0472 (18)0.089 (3)0.0075 (17)0.039 (2)0.0394 (18)
N30.0485 (14)0.0444 (12)0.0450 (12)0.0069 (11)0.0155 (11)0.0259 (10)
C160.074 (2)0.0543 (19)0.078 (2)0.0050 (17)0.0407 (19)0.0288 (17)
C110.0247 (11)0.0277 (11)0.0249 (10)0.0054 (9)0.0004 (9)0.0122 (9)
C140.0209 (11)0.0324 (11)0.0271 (10)0.0040 (9)0.0000 (9)0.0172 (9)
C100.0512 (16)0.0282 (12)0.0367 (13)0.0020 (11)0.0191 (12)0.0099 (10)
C90.0570 (18)0.0217 (11)0.0423 (14)0.0075 (11)0.0175 (13)0.0089 (10)
O80.0481 (11)0.0357 (9)0.0361 (9)0.0047 (8)0.0184 (8)0.0128 (7)
O70.0261 (8)0.0275 (8)0.0378 (8)0.0042 (6)0.0054 (7)0.0176 (7)
Geometric parameters (Å, º) top
Pr1—O52.3835 (17)O6—C131.236 (3)
Pr1—O4i2.4193 (16)C2—C31.380 (3)
Pr1—O7ii2.4366 (16)C2—H20.9300
Pr1—O12.4407 (15)C4—C31.385 (3)
Pr1—O102.4643 (18)C8—C91.379 (3)
Pr1—O92.459 (2)C8—C131.511 (3)
Pr1—N12.6484 (18)C3—H30.9300
Pr1—N22.677 (2)C12—C111.382 (3)
O1—C61.263 (3)C12—H120.9300
N1—C51.335 (3)N4—C151.310 (4)
N1—C11.346 (3)N4—C161.361 (4)
O4—C71.253 (3)N4—H40.8600
O4—Pr1iii2.4193 (16)C15—N31.303 (3)
N2—C81.337 (3)C15—H150.9300
N2—C121.336 (3)C17—C161.341 (4)
C5—C41.384 (3)C17—N31.355 (4)
C5—H50.9300C17—H170.9300
O9—H9A0.77 (3)N3—H3A0.8600
O9—H9B0.73 (3)C16—H160.9300
O5—C131.263 (3)C11—C101.386 (3)
O10—H10A0.88 (4)C11—C141.504 (3)
O10—H10B0.73 (4)C14—O81.240 (3)
C7—O31.249 (3)C14—O71.267 (3)
C7—C41.499 (3)C10—C91.376 (3)
C1—C21.373 (3)C10—H100.9300
C1—C61.513 (3)C9—H90.9300
C6—O21.224 (3)O7—Pr1ii2.4366 (16)
O5—Pr1—O4i78.67 (7)C2—C1—C6121.25 (18)
O5—Pr1—O7ii139.99 (6)O2—C6—O1125.8 (2)
O4i—Pr1—O7ii135.10 (6)O2—C6—C1117.6 (2)
O5—Pr1—O177.58 (6)O1—C6—C1116.62 (17)
O4i—Pr1—O187.46 (6)C1—C2—C3119.03 (19)
O7ii—Pr1—O1117.28 (6)C1—C2—H2120.5
O5—Pr1—O10104.04 (8)C3—C2—H2120.5
O4i—Pr1—O1072.69 (6)C3—C4—C5117.72 (19)
O7ii—Pr1—O1075.16 (7)C3—C4—C7121.57 (19)
O1—Pr1—O10159.11 (6)C5—C4—C7120.71 (18)
O5—Pr1—O9145.52 (6)N2—C8—C9122.7 (2)
O4i—Pr1—O974.82 (7)N2—C8—C13115.37 (19)
O7ii—Pr1—O973.98 (6)C9—C8—C13121.9 (2)
O1—Pr1—O979.59 (6)O6—C13—O5125.2 (2)
O10—Pr1—O988.76 (8)O6—C13—C8119.1 (2)
O5—Pr1—N183.59 (7)O5—C13—C8115.67 (19)
O4i—Pr1—N1148.64 (5)C2—C3—C4119.4 (2)
O7ii—Pr1—N173.00 (6)C2—C3—H3120.3
O1—Pr1—N163.42 (5)C4—C3—H3120.3
O10—Pr1—N1137.32 (6)N2—C12—C11123.74 (19)
O9—Pr1—N1108.60 (7)N2—C12—H12118.1
O5—Pr1—N262.40 (6)C11—C12—H12118.1
O4i—Pr1—N2117.33 (6)C15—N4—C16108.2 (2)
O7ii—Pr1—N280.22 (6)C15—N4—H4125.9
O1—Pr1—N2124.85 (5)C16—N4—H4125.9
O10—Pr1—N271.92 (7)N3—C15—N4109.0 (3)
O9—Pr1—N2151.07 (6)N3—C15—H15125.5
N1—Pr1—N275.27 (6)N4—C15—H15125.5
C6—O1—Pr1125.79 (12)C16—C17—N3106.5 (3)
C5—N1—C1117.88 (18)C16—C17—H17126.8
C5—N1—Pr1126.03 (13)N3—C17—H17126.8
C1—N1—Pr1116.08 (13)C15—N3—C17109.1 (2)
C7—O4—Pr1iii140.65 (14)C15—N3—H3A125.4
C8—N2—C12117.46 (18)C17—N3—H3A125.4
C8—N2—Pr1116.34 (13)C17—C16—N4107.2 (3)
C12—N2—Pr1126.14 (13)C17—C16—H16126.4
N1—C5—C4123.45 (19)N4—C16—H16126.4
N1—C5—H5118.3C12—C11—C10117.9 (2)
C4—C5—H5118.3C12—C11—C14120.9 (2)
Pr1—O9—H9A134 (2)C10—C11—C14121.2 (2)
Pr1—O9—H9B115 (3)O8—C14—O7125.3 (2)
H9A—O9—H9B111 (3)O8—C14—C11118.0 (2)
C13—O5—Pr1130.05 (14)O7—C14—C11116.74 (18)
Pr1—O10—H10A103 (2)C9—C10—C11119.0 (2)
Pr1—O10—H10B137 (3)C9—C10—H10120.5
H10A—O10—H10B119 (4)C11—C10—H10120.5
O3—C7—O4124.8 (2)C10—C9—C8119.3 (2)
O3—C7—C4118.38 (19)C10—C9—H9120.4
O4—C7—C4116.84 (19)C8—C9—H9120.4
N1—C1—C2122.48 (18)C14—O7—Pr1ii138.92 (13)
N1—C1—C6116.26 (18)
Symmetry codes: (i) x1, y, z; (ii) x+1, y, z+1; (iii) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N4—H4···O2iv0.861.852.679 (3)160
N3—H3A···O6v0.861.882.735 (3)172
N3—H3A···O5v0.862.593.063 (3)115
O9—H9A···O1vi0.77 (3)1.98 (3)2.743 (3)172 (3)
O10—H10A···O3i0.88 (4)1.77 (4)2.645 (3)173 (3)
O10—H10A···O4i0.88 (4)2.44 (3)2.894 (3)113 (3)
O10—H10B···O3ii0.73 (4)2.10 (4)2.789 (3)157 (4)
O9—H9B···O8ii0.73 (3)1.96 (4)2.644 (3)157 (3)
Symmetry codes: (i) x1, y, z; (ii) x+1, y, z+1; (iv) x, y, z1; (v) x, y+1, z+1; (vi) x, y, z+2.

Experimental details

Crystal data
Chemical formula(C3H5N2)2[Pr2(C7H3NO4)4(H2O)4]
Mr1152.48
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)9.5444 (19), 10.667 (2), 11.222 (2)
α, β, γ (°)64.63 (3), 79.50 (3), 87.50 (3)
V3)1014.3 (3)
Z1
Radiation typeMo Kα
µ (mm1)2.47
Crystal size (mm)0.19 × 0.16 × 0.09
Data collection
DiffractometerBruker SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2001)
Tmin, Tmax0.652, 0.809
No. of measured, independent and
observed [I > 2σ(I)] reflections
14917, 3561, 3468
Rint0.020
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.015, 0.043, 1.04
No. of reflections3561
No. of parameters305
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.33, 0.45

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected geometric parameters (Å, º) top
Pr1—O52.3835 (17)Pr1—O102.4643 (18)
Pr1—O4i2.4193 (16)Pr1—O92.459 (2)
Pr1—O7ii2.4366 (16)Pr1—N12.6484 (18)
Pr1—O12.4407 (15)Pr1—N22.677 (2)
O5—Pr1—O4i78.67 (7)O1—Pr1—N163.42 (5)
O5—Pr1—O7ii139.99 (6)O10—Pr1—N1137.32 (6)
O4i—Pr1—O7ii135.10 (6)O9—Pr1—N1108.60 (7)
O5—Pr1—O177.58 (6)O5—Pr1—N262.40 (6)
O4i—Pr1—O187.46 (6)O4i—Pr1—N2117.33 (6)
O7ii—Pr1—O1117.28 (6)O7ii—Pr1—N280.22 (6)
O5—Pr1—O10104.04 (8)O1—Pr1—N2124.85 (5)
O4i—Pr1—O1072.69 (6)O10—Pr1—N271.92 (7)
O7ii—Pr1—O1075.16 (7)O9—Pr1—N2151.07 (6)
O1—Pr1—O10159.11 (6)N1—Pr1—N275.27 (6)
O5—Pr1—O9145.52 (6)C6—O1—Pr1125.79 (12)
O4i—Pr1—O974.82 (7)C5—N1—C1117.88 (18)
O7ii—Pr1—O973.98 (6)C5—N1—Pr1126.03 (13)
O1—Pr1—O979.59 (6)C1—N1—Pr1116.08 (13)
O10—Pr1—O988.76 (8)C7—O4—Pr1iii140.65 (14)
O5—Pr1—N183.59 (7)C8—N2—Pr1116.34 (13)
O4i—Pr1—N1148.64 (5)C12—N2—Pr1126.14 (13)
O7ii—Pr1—N173.00 (6)
Symmetry codes: (i) x1, y, z; (ii) x+1, y, z+1; (iii) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N4—H4···O2iv0.861.852.679 (3)160
N3—H3A···O6v0.861.882.735 (3)172
N3—H3A···O5v0.862.593.063 (3)115
O9—H9A···O1vi0.77 (3)1.98 (3)2.743 (3)172 (3)
O10—H10A···O3i0.88 (4)1.77 (4)2.645 (3)173 (3)
O10—H10A···O4i0.88 (4)2.44 (3)2.894 (3)113 (3)
O10—H10B···O3ii0.73 (4)2.10 (4)2.789 (3)157 (4)
O9—H9B···O8ii0.73 (3)1.96 (4)2.644 (3)157 (3)
Symmetry codes: (i) x1, y, z; (ii) x+1, y, z+1; (iv) x, y, z1; (v) x, y+1, z+1; (vi) x, y, z+2.
 

Acknowledgements

The authors thank the Natural Science Foundation of China (20872105), the Qinglan Project of Jiangsu Province (Bu109805) and the Natural Science Foundation of Qinghai Province (2006-G-105).

References

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Volume 67| Part 5| May 2011| Pages m569-m570
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