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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 64| Part 2| February 2008| Pages m419-m420

(μ-6-Oxido-4-oxo-1,2-di­hydro­pyrimidine-5-carboxyl­ato-κ4O5,O6:O2,N3)bis­­[aquabis­(4-oxido-2-oxo-1,2-di­hydro­pyrimidin-3-ium-5-carboxyl­ato-κ2O4,O5)­(1,10-phenanthroline-κ2N,N′)neodymium(III)] hexa­hydrate

aCollege of Chemistry and Chemical Engineering, Guangxi Normal University, Gulin 541004, People's Republic of China, and bDepartment of Chemistry, University of Malaya, 50603, Kuala Lumpur, Malaysia
*Correspondence e-mail: seikweng@um.edu.my

(Received 7 January 2008; accepted 15 January 2008; online 25 January 2008)

The water-coordinated neodymium(III) atom in the centrosymmetric title compound, [Nd2(C5H2N2O4)(C5H3N2O4)4(C12H8N2)2(H2O)2]·6H2O is chelated by a 1,10-phenanthroline heterocycle and two 2,4-dihydroxy­pyrimidine-5-carboxyl­ate dianions. Two tris-chelated water-coordinated units are bridged by a 2,4-dihydroxy­pyrimidine-5-carboxyl­ate dianion, which is disordered about a center of inversion. The metal center has a monocapped square-anti­prismatic coordination.

Related literature

The title neodymium compound is isostructural with the praseodymium analog (Sun & Jin, 2004[Sun, C.-Y. & Jin, L. P. (2004). Polyhedron, 23, 2085-2093.]). For a related structure, see: Xing et al. (2008[Xing, H.-H., Chen, Z.-L. & Ng, S. W. (2008). Acta Cryst. E64, m418.]).

[Scheme 1]

Experimental

Crystal data
  • [Nd2(C5H2N2O4)(C5H3N2O4)4(C12H8N2)2(H2O)2]·6H2O

  • Mr = 1567.48

  • Triclinic, [P \overline 1]

  • a = 10.1980 (7) Å

  • b = 12.8896 (9) Å

  • c = 13.3383 (9) Å

  • α = 118.711 (1)°

  • β = 90.010 (1)°

  • γ = 108.612 (1)°

  • V = 1432.25 (17) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 1.90 mm−1

  • T = 295 (2) K

  • 0.10 × 0.04 × 0.02 mm

Data collection
  • Bruker APEXII diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.724, Tmax = 0.963

  • 12405 measured reflections

  • 6377 independent reflections

  • 5349 reflections with I > 2σ(I)

  • Rint = 0.039

Refinement
  • R[F2 > 2σ(F2)] = 0.054

  • wR(F2) = 0.136

  • S = 1.04

  • 6377 reflections

  • 454 parameters

  • 84 restraints

  • H-atom parameters constrained

  • Δρmax = 1.23 e Å−3

  • Δρmin = −0.90 e Å−3

Table 1
Selected geometric parameters (Å, °)

Nd1—O2 2.526 (4)
Nd1—O3 2.502 (9)
Nd1—O5 2.392 (4)
Nd1—O6 2.575 (4)
Nd1—O9 2.341 (4)
Nd1—O10 2.526 (4)
Nd1—O1W 2.475 (4)
Nd1—N7 2.638 (5)
Nd1—N8 2.725 (5)
O2—Nd1—O3 67.5 (2)
O2—Nd1—O5 71.6 (1)
O2—Nd1—O6 123.5 (1)
O2—Nd1—O9 127.7 (1)
O2—Nd1—O10 71.8 (1)
O2—Nd1—O1W 136.6 (2)
O2—Nd1—N7 70.6 (2)
O2—Nd1—N8 111.7 (2)
O3—Nd1—O5 138.7 (2)
O3—Nd1—O6 133.6 (3)
O3—Nd1—O9 68.6 (3)
O3—Nd1—O10 76.5 (3)
O3—Nd1—O1W 138.2 (3)
O3—Nd1—N7 87.9 (3)
O3—Nd1—N8 65.6 (3)
O5—Nd1—O6 67.9 (1)
O5—Nd1—O9 139.7 (2)
O5—Nd1—O10 85.9 (1)
O5—Nd1—O1W 78.2 (2)
O5—Nd1—N7 83.8 (2)
O5—Nd1—N8 138.8 (2)
O6—Nd1—O9 72.6 (1)
O6—Nd1—O10 67.7 (1)
O6—Nd1—O1W 69.0 (1)
O6—Nd1—N7 138.2 (2)
O6—Nd1—N8 124.8 (2)
O9—Nd1—O10 71.5 (1)
O9—Nd1—O1W 95.5 (2)
O9—Nd1—N7 133.8 (2)
O9—Nd1—N8 72.8 (2)
O10—Nd1—O1W 136.7 (2)
O10—Nd1—N7 142.5 (2)
O10—Nd1—N8 135.1 (2)
O1W—Nd1—N7 75.78 (16)
O1W—Nd1—N8 72.93 (16)
N7—Nd1—N8 61.14 (16)

Data collection: APEX2 (Bruker, 2006[Bruker (2006). APEX2 and SAINT. Bruker AXS Inc., Madison, Winconsin, USA.]); cell refinement: SAINT (Bruker, 2006[Bruker (2006). APEX2 and SAINT. Bruker AXS Inc., Madison, Winconsin, USA.]); data reduction: SAINT; method used to solve structure: atomic coordinates taken from the Pr analog (Sun & Jin, 2004[Sun, C.-Y. & Jin, L. P. (2004). Polyhedron, 23, 2085-2093.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: X-SEED (Barbour, 2001[Barbour, L. J. (2001). J. Supramol. Chem., 1, 189-191.]); software used to prepare material for publication: publCIF (Westrip, 2008[Westrip, S. P. (2008). publCIF. In preparation.]).

Supporting information


Comment top

The 1,10-phenanthroline-chelated rare-earth compound, Pr2(C12H8N2)2(C5H2N2O4)(C5H3N2O4)4(H2O)2.3H2O, represents the first example of dinculear lanthanum derivatives of 2,4-dihydroxpyrimidine-5-carboxylic acid (Sun & Jin, 2004). The present neodymium compound is isostructural with the praseodymium analog.

Related literature top

The title neodymium compound is isostructural with the praesodymium analog (Sun & Jin, 2004). For a related structure, see: Xing et al. (2008).

Experimental top

2,4-Dihydroxypyrimidine-5-carboxylic acid (0.044 g, 0.25 mmol), neodymium trichloride hexahydrate (0.090 g, 0.25 mmol), 1,10-phenanthroline (0.050 g, 0.25 mmol), sodium hydroxide (0.010 g, 0.25 mmol) and water (15 ml) was sealed in a 25-ml, Teflon-lined, stainless-steel Parr bomb. The bomb was heated to 383 K for 120 h. It was then cooled over 48 h to give lilac crystals in 70% yield. CH&N elemental analysis. Found (Calculated) for C49H46N14O28Nd2: C 37.37, H 3.07, N 12.62% (37.54, 2.96, 12.51%).

Refinement top

The bridging dianion is disordered about a center of inversion; all atoms were assigned only half site-occupancy except for O2, which had full site occupancy. The pyrimidine ring was refined as a rigid hexagon of 1.39 Å sides.

Carbon-bound H atoms were generated geometrically, and were included in the refinements in the riding model approximation, as well the nitrogen-bound ones. For the water molecules, only those on the coordinated water were were placed in chemically sensible positions on the basis of hydrogen bonding interactions. TWo of the lattice water molecules are each disordered over two positions. The displacement parameters of the two components were restrained to be equal. The H atoms bound to the lattice water molecules could not be located. The final difference Fourier map had a large peak near Nd1.

Computing details top

Data collection: APEX2 (Bruker, 2006); cell refinement: SAINT (Bruker, 2006); data reduction: SAINT (Bruker, 2006); program(s) used to solve structure: atomic coordinates taken from the Pr analog (Sun & Jin, 2004); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2008).

Figures top
[Figure 1] Fig. 1. Displacement ellipsoid plot of Nd2(C12H8N2)2(C5H2N2O4)(C5H3N2O4)4(H2O)2 .6H2O drawn at the 50% probability level. Unlabelled atoms are related to labelled atoms by the symmetry operation (1 - x, 1 - y, 1 - z). Lattice water molecules have been omitted for clarity. Only one disorder component is shown.
[Figure 2] Fig. 2. Geometry of Nd.
(µ-6-Oxido-4-oxo-1,2-dihydropyrimidine-5-carboxylato- κ4O5,O6:O2,N3)bis[aquabis(4-oxido- 2-oxo-1,2-dihydropyrimidin-3-ium-5-carboxylato- κ2O4,O5)(1,10-phenanthroline- κ2N,N')neodymium(III)] hexahydrate top
Crystal data top
[Nd2(C5H2N2O4)(C5H3N2O4)4(C12H8N2)2(H2O)2]·6H2OZ = 1
Mr = 1567.48F(000) = 782
Triclinic, P1Dx = 1.817 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.1980 (7) ÅCell parameters from 2901 reflections
b = 12.8896 (9) Åθ = 2.3–22.7°
c = 13.3383 (9) ŵ = 1.90 mm1
α = 118.711 (1)°T = 295 K
β = 90.010 (1)°Prism, lilac
γ = 108.612 (1)°0.10 × 0.04 × 0.02 mm
V = 1432.25 (17) Å3
Data collection top
Bruker APEXII
diffractometer
6377 independent reflections
Radiation source: fine-focus sealed tube5349 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.039
ϕ and ω scansθmax = 27.5°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1313
Tmin = 0.724, Tmax = 0.963k = 1616
12405 measured reflectionsl = 1717
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)] = 0.054Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.136H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0735P)2 + 0.4633P]
where P = (Fo2 + 2Fc2)/3
6377 reflections(Δ/σ)max = 0.001
454 parametersΔρmax = 1.23 e Å3
84 restraintsΔρmin = 0.90 e Å3
Crystal data top
[Nd2(C5H2N2O4)(C5H3N2O4)4(C12H8N2)2(H2O)2]·6H2Oγ = 108.612 (1)°
Mr = 1567.48V = 1432.25 (17) Å3
Triclinic, P1Z = 1
a = 10.1980 (7) ÅMo Kα radiation
b = 12.8896 (9) ŵ = 1.90 mm1
c = 13.3383 (9) ÅT = 295 K
α = 118.711 (1)°0.10 × 0.04 × 0.02 mm
β = 90.010 (1)°
Data collection top
Bruker APEXII
diffractometer
6377 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
5349 reflections with I > 2σ(I)
Tmin = 0.724, Tmax = 0.963Rint = 0.039
12405 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.05484 restraints
wR(F2) = 0.136H-atom parameters constrained
S = 1.04Δρmax = 1.23 e Å3
6377 reflectionsΔρmin = 0.90 e Å3
454 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Nd10.26520 (3)0.27712 (3)0.14686 (3)0.02555 (12)
O40.2306 (5)0.1369 (4)0.0511 (5)0.0486 (12)
O50.2203 (5)0.0542 (4)0.0456 (4)0.0400 (11)
O60.3131 (5)0.1959 (4)0.0621 (4)0.0349 (10)
O70.6565 (7)0.1207 (7)0.2689 (7)0.090 (2)
O80.5206 (5)0.6553 (4)0.2061 (5)0.0490 (13)
O90.3726 (4)0.4550 (4)0.1277 (4)0.0370 (10)
O100.5209 (4)0.3057 (4)0.1378 (4)0.0334 (9)
O110.9276 (5)0.3690 (5)0.0047 (5)0.0535 (14)
O1W0.0466 (5)0.1916 (4)0.0068 (4)0.0442 (11)
H1W10.03050.15570.02120.066*
H1W20.03890.25260.00130.066*
O2W0.0203 (12)0.1690 (10)0.2139 (10)0.156 (4)
O3W0.212 (2)0.192 (2)0.3809 (18)0.149 (5)0.50
O4W0.483 (2)0.789 (2)0.4468 (18)0.155 (5)0.50
O3'0.144 (2)0.0260 (19)0.5588 (18)0.149 (5)0.50
O4'0.418 (2)0.918 (2)0.4944 (18)0.155 (5)0.50
N30.5421 (7)0.0189 (6)0.2106 (6)0.0512 (16)
H3N0.59120.06540.24330.061*
N40.4768 (6)0.1499 (5)0.1699 (5)0.0415 (13)
H4N0.48300.21240.17970.050*
N50.8306 (5)0.5190 (5)0.0582 (5)0.0373 (13)
H5N0.89860.56470.04160.045*
N60.7237 (5)0.3425 (5)0.0743 (5)0.0325 (11)
H6N0.72510.27360.06890.039*
N70.0616 (5)0.2175 (5)0.2535 (5)0.0359 (12)
N80.1220 (6)0.4365 (5)0.2479 (5)0.0404 (13)
C60.2655 (6)0.0264 (6)0.0300 (5)0.0302 (13)
C70.3654 (6)0.0150 (5)0.0962 (5)0.0282 (12)
C80.3800 (6)0.1251 (5)0.1048 (5)0.0291 (12)
C90.5642 (8)0.0857 (8)0.2206 (7)0.053 (2)
C100.4462 (7)0.0521 (6)0.1512 (6)0.0386 (15)
H100.43560.12490.14820.046*
C110.4953 (7)0.5402 (6)0.1568 (5)0.0319 (13)
C120.6137 (6)0.4941 (5)0.1250 (5)0.0300 (13)
C130.6123 (6)0.3775 (5)0.1135 (5)0.0279 (12)
C140.8335 (6)0.4081 (6)0.0429 (6)0.0379 (15)
C150.7258 (6)0.5607 (6)0.0983 (5)0.0338 (14)
H150.73030.63830.10810.041*
C160.0321 (8)0.1146 (7)0.2595 (6)0.0479 (17)
H160.08520.06400.22600.057*
C170.0746 (8)0.0765 (8)0.3131 (7)0.058 (2)
H170.09150.00240.31540.069*
C180.1540 (8)0.1494 (9)0.3626 (7)0.061 (2)
H180.22550.12510.39890.073*
C190.1288 (7)0.2575 (8)0.3586 (6)0.0489 (18)
C200.0184 (6)0.2911 (7)0.3026 (5)0.0382 (15)
C210.2097 (8)0.3371 (10)0.4055 (7)0.067 (3)
H210.28340.31490.44100.080*
C220.1824 (8)0.4419 (9)0.3998 (7)0.062 (2)
H220.23820.49060.42990.074*
C230.0688 (8)0.4805 (8)0.3481 (6)0.0499 (18)
C240.0120 (7)0.4047 (6)0.2980 (5)0.0376 (15)
C250.0328 (9)0.5927 (8)0.3471 (7)0.059 (2)
H250.08490.64470.37890.071*
C260.0792 (9)0.6270 (8)0.2994 (7)0.059 (2)
H260.10580.70360.30050.071*
C270.1537 (8)0.5466 (7)0.2491 (7)0.0483 (18)
H270.22840.57000.21490.058*
O10.3919 (11)0.1911 (9)0.4221 (9)0.059 (3)0.50
O20.3542 (4)0.2234 (4)0.2860 (4)0.0383 (10)
O30.3932 (12)0.4700 (9)0.3390 (8)0.042 (3)0.50
C10.3988 (6)0.2642 (7)0.3854 (7)0.034 (3)0.50
C20.4626 (9)0.4027 (5)0.4640 (6)0.021 (3)0.50
C30.4558 (9)0.4923 (6)0.4366 (5)0.032 (3)0.50
N20.5211 (9)0.6211 (6)0.5170 (6)0.028 (3)0.50
H2N0.51690.67660.50010.034*0.50
C40.5931 (8)0.6601 (5)0.6250 (6)0.033 (3)0.50
N10.5999 (9)0.5705 (8)0.6524 (5)0.033 (3)0.50
C50.5346 (9)0.4417 (7)0.5719 (7)0.040 (3)0.50
H50.53910.38170.59030.048*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nd10.02497 (18)0.02326 (18)0.03442 (19)0.01369 (13)0.01123 (12)0.01601 (14)
O40.057 (3)0.030 (2)0.071 (3)0.022 (2)0.022 (3)0.030 (3)
O50.051 (3)0.025 (2)0.047 (3)0.015 (2)0.021 (2)0.019 (2)
O60.048 (3)0.033 (2)0.041 (2)0.027 (2)0.019 (2)0.023 (2)
O70.103 (5)0.095 (5)0.133 (6)0.066 (4)0.085 (5)0.084 (5)
O80.059 (3)0.028 (2)0.074 (3)0.024 (2)0.031 (3)0.031 (2)
O90.038 (2)0.035 (2)0.057 (3)0.026 (2)0.021 (2)0.030 (2)
O100.030 (2)0.032 (2)0.052 (3)0.0154 (18)0.0149 (19)0.029 (2)
O110.038 (3)0.046 (3)0.100 (4)0.025 (2)0.036 (3)0.048 (3)
O1W0.035 (2)0.046 (3)0.058 (3)0.021 (2)0.011 (2)0.026 (2)
O2W0.174 (8)0.147 (7)0.156 (7)0.074 (6)0.026 (6)0.075 (6)
O3W0.195 (10)0.126 (8)0.143 (8)0.064 (7)0.005 (7)0.077 (7)
O4W0.177 (10)0.163 (9)0.127 (8)0.035 (7)0.036 (7)0.092 (7)
O3'0.195 (10)0.126 (8)0.143 (8)0.064 (7)0.005 (7)0.077 (7)
O4'0.177 (10)0.163 (9)0.127 (8)0.035 (7)0.036 (7)0.092 (7)
N30.063 (4)0.052 (4)0.070 (4)0.042 (3)0.036 (3)0.041 (3)
N40.051 (3)0.037 (3)0.057 (4)0.025 (3)0.027 (3)0.034 (3)
N50.029 (3)0.035 (3)0.064 (4)0.012 (2)0.016 (3)0.036 (3)
N60.028 (3)0.027 (3)0.053 (3)0.011 (2)0.012 (2)0.027 (3)
N70.033 (3)0.040 (3)0.040 (3)0.016 (2)0.010 (2)0.023 (3)
N80.038 (3)0.044 (3)0.045 (3)0.025 (3)0.015 (3)0.021 (3)
C60.029 (3)0.028 (3)0.037 (3)0.012 (2)0.005 (2)0.018 (3)
C70.030 (3)0.024 (3)0.031 (3)0.013 (2)0.003 (2)0.013 (3)
C80.031 (3)0.023 (3)0.032 (3)0.011 (2)0.007 (2)0.013 (3)
C90.057 (5)0.060 (5)0.067 (5)0.037 (4)0.037 (4)0.040 (4)
C100.046 (4)0.035 (3)0.046 (4)0.021 (3)0.012 (3)0.024 (3)
C110.041 (4)0.033 (3)0.038 (3)0.020 (3)0.016 (3)0.026 (3)
C120.033 (3)0.027 (3)0.036 (3)0.012 (3)0.009 (3)0.019 (3)
C130.023 (3)0.027 (3)0.035 (3)0.009 (2)0.005 (2)0.017 (3)
C140.027 (3)0.034 (3)0.061 (4)0.012 (3)0.011 (3)0.030 (3)
C150.037 (3)0.023 (3)0.045 (4)0.010 (3)0.006 (3)0.020 (3)
C160.043 (4)0.049 (4)0.053 (4)0.017 (3)0.014 (3)0.027 (4)
C170.050 (5)0.060 (5)0.063 (5)0.010 (4)0.014 (4)0.038 (4)
C180.043 (4)0.077 (6)0.057 (5)0.013 (4)0.018 (4)0.036 (5)
C190.036 (4)0.064 (5)0.035 (4)0.014 (4)0.011 (3)0.019 (4)
C200.028 (3)0.054 (4)0.030 (3)0.020 (3)0.010 (3)0.016 (3)
C210.041 (4)0.104 (8)0.054 (5)0.037 (5)0.031 (4)0.032 (5)
C220.048 (5)0.086 (7)0.061 (5)0.044 (5)0.026 (4)0.031 (5)
C230.047 (4)0.058 (5)0.041 (4)0.031 (4)0.009 (3)0.015 (4)
C240.035 (3)0.047 (4)0.032 (3)0.027 (3)0.010 (3)0.014 (3)
C250.063 (5)0.063 (5)0.051 (5)0.047 (4)0.016 (4)0.014 (4)
C260.065 (5)0.050 (5)0.070 (5)0.039 (4)0.014 (4)0.025 (4)
C270.053 (4)0.040 (4)0.064 (5)0.030 (4)0.022 (4)0.027 (4)
O10.076 (6)0.042 (5)0.057 (6)0.020 (5)0.013 (5)0.025 (4)
O20.036 (2)0.028 (2)0.048 (3)0.0158 (19)0.010 (2)0.015 (2)
O30.050 (6)0.027 (5)0.046 (5)0.017 (4)0.006 (4)0.015 (4)
C10.040 (6)0.024 (5)0.046 (6)0.014 (5)0.011 (5)0.022 (5)
C20.028 (5)0.023 (5)0.029 (6)0.017 (4)0.009 (4)0.022 (5)
C30.030 (6)0.033 (6)0.029 (6)0.014 (5)0.014 (4)0.011 (5)
N20.040 (5)0.027 (5)0.030 (5)0.021 (4)0.002 (4)0.018 (4)
C40.024 (5)0.038 (6)0.035 (6)0.017 (5)0.012 (4)0.014 (5)
N10.039 (6)0.029 (6)0.034 (6)0.021 (5)0.004 (4)0.013 (5)
C50.041 (6)0.043 (7)0.037 (6)0.019 (5)0.016 (5)0.018 (5)
Geometric parameters (Å, º) top
Nd1—O22.526 (4)C10—H100.93
Nd1—O32.502 (9)C11—C121.485 (8)
Nd1—O52.392 (4)C12—C151.355 (8)
Nd1—O62.575 (4)C12—C131.431 (8)
Nd1—O92.341 (4)C15—H150.93
Nd1—O102.526 (4)C16—C171.391 (10)
Nd1—O1W2.475 (4)C16—H160.93
Nd1—N1i2.478 (6)C17—C181.366 (11)
Nd1—N72.638 (5)C17—H170.93
Nd1—N82.725 (5)C18—C191.361 (11)
O4—C61.234 (7)C18—H180.93
O5—C61.268 (7)C19—C201.419 (9)
O6—C81.233 (7)C19—C211.431 (11)
O7—C91.229 (8)C20—C241.427 (9)
O8—C111.232 (7)C21—C221.330 (12)
O9—C111.279 (7)C21—H210.93
O10—C131.252 (7)C22—C231.424 (11)
O11—C141.222 (7)C22—H220.93
O1W—H1W10.85C23—C251.381 (11)
O1W—H1W20.85C23—C241.402 (9)
N3—C101.351 (8)C25—C261.361 (12)
N3—C91.366 (9)C25—H250.93
N3—H3N0.86C26—C271.391 (9)
N4—C91.367 (8)C26—H260.93
N4—C81.378 (7)C27—H270.93
N4—H4N0.86O1—C11.238 (8)
N5—C151.345 (8)O2—C11.191 (8)
N5—C141.354 (7)O3—C31.307 (8)
N5—H5N0.86C1—C21.473 (8)
N6—C131.368 (7)C2—C31.39
N6—C141.371 (7)C2—C51.39
N6—H6N0.86C3—N21.39
N7—C161.305 (9)N2—C41.39
N7—C201.375 (8)N2—H2N0.86
N8—C271.343 (9)C4—N11.39
N8—C241.358 (8)N1—C51.39
C6—C71.487 (8)N1—Nd1i2.478 (6)
C7—C101.346 (8)C5—H50.93
C7—C81.438 (8)
O2—Nd1—O367.5 (2)O7—C9—N4122.9 (7)
O2—Nd1—O571.6 (1)N3—C9—N4114.1 (6)
O2—Nd1—O6123.5 (1)C7—C10—N3123.2 (6)
O2—Nd1—O9127.7 (1)C7—C10—H10118.4
O2—Nd1—O1071.8 (1)N3—C10—H10118.4
O2—Nd1—O1W136.6 (2)O8—C11—O9124.9 (6)
O2—Nd1—N770.6 (2)O8—C11—C12118.8 (6)
O2—Nd1—N8111.7 (2)O9—C11—C12116.3 (5)
O3—Nd1—O5138.7 (2)C15—C12—C13117.4 (5)
O3—Nd1—O6133.6 (3)C15—C12—C11119.2 (5)
O3—Nd1—O968.6 (3)C13—C12—C11123.3 (5)
O3—Nd1—O1076.5 (3)O10—C13—N6116.8 (5)
O3—Nd1—O1W138.2 (3)O10—C13—C12126.6 (5)
O3—Nd1—N787.9 (3)N6—C13—C12116.6 (5)
O3—Nd1—N865.6 (3)O11—C14—N5122.8 (6)
O5—Nd1—O667.9 (1)O11—C14—N6122.0 (6)
O5—Nd1—O9139.7 (2)N5—C14—N6115.2 (5)
O5—Nd1—O1085.9 (1)N5—C15—C12122.7 (5)
O5—Nd1—O1W78.2 (2)N5—C15—H15118.7
O5—Nd1—N783.8 (2)C12—C15—H15118.7
O5—Nd1—N8138.8 (2)N7—C16—C17123.6 (7)
O6—Nd1—O972.6 (1)N7—C16—H16118.2
O6—Nd1—O1067.7 (1)C17—C16—H16118.2
O6—Nd1—O1W69.0 (1)C18—C17—C16119.1 (8)
O6—Nd1—N7138.2 (2)C18—C17—H17120.5
O6—Nd1—N8124.8 (2)C16—C17—H17120.5
O9—Nd1—O1071.5 (1)C19—C18—C17120.1 (7)
O9—Nd1—O1W95.5 (2)C19—C18—H18120.0
O9—Nd1—N7133.8 (2)C17—C18—H18120.0
O9—Nd1—N872.8 (2)C18—C19—C20118.1 (7)
O10—Nd1—O1W136.7 (2)C18—C19—C21123.4 (7)
O10—Nd1—N7142.5 (2)C20—C19—C21118.5 (8)
O10—Nd1—N8135.1 (2)N7—C20—C19121.5 (7)
O1W—Nd1—N775.78 (16)N7—C20—C24119.0 (6)
O1W—Nd1—N872.93 (16)C19—C20—C24119.5 (6)
N7—Nd1—N861.14 (16)C22—C21—C19121.9 (7)
O9—Nd1—N1i80.8 (3)C22—C21—H21119.1
O5—Nd1—N1i124.7 (3)C19—C21—H21119.1
O1W—Nd1—N1i147.5 (3)C21—C22—C23120.8 (7)
N1i—Nd1—O314.1 (3)C21—C22—H22119.6
N1i—Nd1—O1073.0 (3)C23—C22—H22119.6
N1i—Nd1—O253.4 (2)C25—C23—C24118.0 (7)
N1i—Nd1—O6137.7 (4)C25—C23—C22122.0 (7)
N1i—Nd1—N783.6 (4)C24—C23—C22119.9 (8)
N1i—Nd1—N875.1 (3)N8—C24—C23122.7 (7)
C6—O5—Nd1140.6 (4)N8—C24—C20117.9 (5)
C8—O6—Nd1123.2 (4)C23—C24—C20119.4 (6)
C11—O9—Nd1137.2 (4)C26—C25—C23119.8 (7)
C13—O10—Nd1130.2 (4)C26—C25—H25120.1
Nd1—O1W—H1W1117.9C23—C25—H25120.1
Nd1—O1W—H1W2107.8C25—C26—C27119.5 (8)
H1W1—O1W—H1W2107.7C25—C26—H26120.2
C10—N3—C9122.5 (6)C27—C26—H26120.2
C10—N3—H3N118.7N8—C27—C26122.6 (7)
C9—N3—H3N118.7N8—C27—H27118.7
C9—N4—C8126.9 (6)C26—C27—H27118.7
C9—N4—H4N116.5C1—O2—Nd1143.9 (5)
C8—N4—H4N116.5C3—O3—Nd1135.9 (6)
C15—N5—C14122.6 (5)O2—C1—O1120.4 (8)
C15—N5—H5N118.7O2—C1—C2119.1 (7)
C14—N5—H5N118.7O1—C1—C2120.5 (8)
C13—N6—C14125.4 (5)C3—C2—C5120.0
C13—N6—H6N117.3C3—C2—C1124.7 (6)
C14—N6—H6N117.3C5—C2—C1115.3 (6)
C16—N7—C20117.7 (6)O3—C3—N2113.1 (6)
C16—N7—Nd1120.3 (4)O3—C3—C2126.9 (6)
C20—N7—Nd1121.9 (4)N2—C3—C2120.0
C27—N8—C24117.3 (6)C4—N2—C3120.0
C27—N8—Nd1122.7 (4)C4—N2—H2N120.0
C24—N8—Nd1119.9 (4)C3—N2—H2N120.0
O4—C6—O5123.3 (6)N2—C4—N1120.0
O4—C6—C7118.8 (5)N2—C4—Nd1i175.4 (3)
O5—C6—C7117.9 (5)N1—C4—Nd1i55.6 (3)
C10—C7—C8117.7 (6)C5—N1—C4120.0
C10—C7—C6119.6 (5)C5—N1—Nd1i143.1 (4)
C8—C7—C6122.7 (5)C4—N1—Nd1i96.8 (4)
O6—C8—N4118.1 (5)N1—C5—C2120.0
O6—C8—C7126.6 (5)N1—C5—H5120.0
N4—C8—C7115.3 (5)C2—C5—H5120.0
O7—C9—N3123.0 (7)
O9—Nd1—O5—C621.5 (8)C9—N3—C10—C70.6 (11)
O1W—Nd1—O5—C6106.0 (7)Nd1—O9—C11—O8131.1 (6)
N1i—Nd1—O5—C699.5 (8)Nd1—O9—C11—C1250.7 (8)
O3—Nd1—O5—C697.6 (8)O8—C11—C12—C1530.9 (9)
O10—Nd1—O5—C633.4 (6)O9—C11—C12—C15147.5 (6)
O2—Nd1—O5—C6105.6 (7)O8—C11—C12—C13153.3 (6)
O6—Nd1—O5—C634.1 (6)O9—C11—C12—C1328.4 (9)
N7—Nd1—O5—C6177.3 (7)Nd1—O10—C13—N6156.8 (4)
N8—Nd1—O5—C6152.1 (6)Nd1—O10—C13—C1224.7 (9)
C4i—Nd1—O5—C6104.4 (7)C14—N6—C13—O10179.7 (6)
O9—Nd1—O6—C8125.4 (5)C14—N6—C13—C121.7 (9)
O5—Nd1—O6—C846.1 (4)C15—C12—C13—O10177.3 (6)
O1W—Nd1—O6—C8131.5 (5)C11—C12—C13—O106.8 (10)
N1i—Nd1—O6—C871.6 (6)C15—C12—C13—N61.2 (8)
O3—Nd1—O6—C890.9 (5)C11—C12—C13—N6174.7 (5)
O10—Nd1—O6—C848.7 (4)C15—N5—C14—O11178.8 (7)
O2—Nd1—O6—C81.2 (5)C15—N5—C14—N61.8 (10)
N7—Nd1—O6—C897.0 (5)C13—N6—C14—O11177.5 (6)
N8—Nd1—O6—C8179.0 (4)C13—N6—C14—N53.1 (10)
C4i—Nd1—O6—C830.3 (6)C14—N5—C15—C121.0 (10)
O5—Nd1—O9—C1189.4 (6)C13—C12—C15—N52.5 (9)
O1W—Nd1—O9—C11167.6 (6)C11—C12—C15—N5173.6 (6)
N1i—Nd1—O9—C1145.0 (6)C20—N7—C16—C170.5 (10)
O3—Nd1—O9—C1152.3 (6)Nd1—N7—C16—C17179.3 (6)
O10—Nd1—O9—C1130.0 (6)N7—C16—C17—C180.2 (12)
O2—Nd1—O9—C1117.6 (6)C16—C17—C18—C190.2 (12)
O6—Nd1—O9—C11101.6 (6)C17—C18—C19—C200.2 (11)
N7—Nd1—O9—C11116.9 (6)C17—C18—C19—C21178.3 (8)
N8—Nd1—O9—C11122.2 (6)C16—N7—C20—C190.5 (9)
C4i—Nd1—O9—C1133.9 (6)Nd1—N7—C20—C19179.3 (5)
O9—Nd1—O10—C1310.0 (5)C16—N7—C20—C24179.6 (6)
O5—Nd1—O10—C13136.0 (5)Nd1—N7—C20—C241.6 (8)
O1W—Nd1—O10—C1368.0 (6)C18—C19—C20—N70.1 (10)
N1i—Nd1—O10—C1395.8 (6)C21—C19—C20—N7178.7 (6)
O3—Nd1—O10—C1381.7 (5)C18—C19—C20—C24179.3 (7)
O2—Nd1—O10—C13152.0 (5)C21—C19—C20—C242.2 (10)
O6—Nd1—O10—C1368.3 (5)C18—C19—C21—C22179.8 (8)
N7—Nd1—O10—C13149.7 (5)C20—C19—C21—C221.3 (12)
N8—Nd1—O10—C1349.2 (6)C19—C21—C22—C231.2 (13)
C4i—Nd1—O10—C13124.7 (5)C21—C22—C23—C25176.1 (8)
O9—Nd1—N7—C16173.0 (5)C21—C22—C23—C242.8 (12)
O5—Nd1—N7—C1623.8 (5)C27—N8—C24—C231.0 (10)
O1W—Nd1—N7—C16103.2 (5)Nd1—N8—C24—C23177.9 (5)
N1i—Nd1—N7—C16102.2 (6)C27—N8—C24—C20176.9 (6)
O3—Nd1—N7—C16115.7 (5)Nd1—N8—C24—C204.2 (8)
O10—Nd1—N7—C1651.2 (6)C25—C23—C24—N80.8 (10)
O2—Nd1—N7—C1648.8 (5)C22—C23—C24—N8179.7 (7)
O6—Nd1—N7—C1670.1 (6)C25—C23—C24—C20177.1 (7)
N8—Nd1—N7—C16178.7 (6)C22—C23—C24—C201.8 (10)
C4i—Nd1—N7—C1675.8 (5)N7—C20—C24—N81.8 (9)
O9—Nd1—N7—C208.2 (6)C19—C20—C24—N8177.3 (6)
O5—Nd1—N7—C20155.0 (5)N7—C20—C24—C23179.8 (6)
O1W—Nd1—N7—C2075.6 (5)C19—C20—C24—C230.6 (9)
N1i—Nd1—N7—C2079.0 (5)C24—C23—C25—C260.7 (11)
O3—Nd1—N7—C2065.6 (5)C22—C23—C25—C26178.2 (8)
O10—Nd1—N7—C20130.0 (4)C23—C25—C26—C271.9 (12)
O2—Nd1—N7—C20132.4 (5)C24—N8—C27—C260.3 (11)
O6—Nd1—N7—C20108.7 (5)Nd1—N8—C27—C26179.2 (6)
N8—Nd1—N7—C202.5 (4)C25—C26—C27—N81.8 (12)
C4i—Nd1—N7—C20105.4 (5)O9—Nd1—O2—C150.4 (6)
O9—Nd1—N8—C272.1 (5)O5—Nd1—O2—C1170.3 (6)
O5—Nd1—N8—C27147.0 (5)O1W—Nd1—O2—C1122.0 (6)
O1W—Nd1—N8—C2799.4 (6)N1i—Nd1—O2—C116.0 (8)
N1i—Nd1—N8—C2786.9 (6)O3—Nd1—O2—C115.5 (6)
O3—Nd1—N8—C2775.9 (6)O10—Nd1—O2—C198.0 (6)
O10—Nd1—N8—C2740.9 (6)O6—Nd1—O2—C1143.8 (6)
O2—Nd1—N8—C27126.6 (5)N7—Nd1—O2—C180.5 (6)
O6—Nd1—N8—C2751.4 (6)N8—Nd1—O2—C134.2 (6)
N7—Nd1—N8—C27177.7 (6)C4i—Nd1—O2—C112.6 (9)
C4i—Nd1—N8—C27108.0 (6)O9—Nd1—O3—C3151.4 (14)
O9—Nd1—N8—C24179.1 (5)O5—Nd1—O3—C38.8 (16)
O5—Nd1—N8—C2431.9 (6)O1W—Nd1—O3—C3135.1 (11)
O1W—Nd1—N8—C2479.4 (5)N1i—Nd1—O3—C32 (2)
N1i—Nd1—N8—C2494.3 (6)O10—Nd1—O3—C376.2 (13)
O3—Nd1—N8—C24105.3 (5)O2—Nd1—O3—C30.5 (12)
O10—Nd1—N8—C24140.3 (4)O6—Nd1—O3—C3116.0 (12)
O2—Nd1—N8—C2454.6 (5)N7—Nd1—O3—C369.4 (13)
O6—Nd1—N8—C24127.4 (4)N8—Nd1—O3—C3128.4 (14)
N7—Nd1—N8—C243.4 (4)C4i—Nd1—O3—C31.4 (13)
C4i—Nd1—N8—C2473.2 (5)Nd1—O2—C1—O1158.2 (7)
Nd1—O5—C6—O4168.0 (5)Nd1—O2—C1—C221.9 (7)
Nd1—O5—C6—C712.1 (9)O2—C1—C2—C310.7 (6)
O4—C6—C7—C1019.2 (9)O1—C1—C2—C3169.4 (6)
O5—C6—C7—C10160.9 (6)O2—C1—C2—C5168.7 (5)
O4—C6—C7—C8160.7 (6)O1—C1—C2—C511.2 (5)
O5—C6—C7—C819.2 (8)Nd1—O3—C3—N2175.8 (8)
Nd1—O6—C8—N4137.4 (5)Nd1—O3—C3—C23.7 (18)
Nd1—O6—C8—C744.3 (8)C5—C2—C3—O3179.5 (12)
C9—N4—C8—O6177.5 (7)C1—C2—C3—O30.1 (11)
C9—N4—C8—C74.0 (10)C5—C2—C3—N20.0
C10—C7—C8—O6178.5 (6)C1—C2—C3—N2179.4 (6)
C6—C7—C8—O61.3 (9)O3—C3—N2—C4179.6 (11)
C10—C7—C8—N40.2 (8)C2—C3—N2—C40.0
C6—C7—C8—N4179.7 (5)C3—N2—C4—N10.0
C10—N3—C9—O7175.9 (8)N2—C4—N1—C50.0
C10—N3—C9—N42.7 (11)N2—C4—N1—Nd1i178.2 (5)
C8—N4—C9—O7173.4 (8)C4—N1—C5—C20.0
C8—N4—C9—N35.2 (11)Nd1i—N1—C5—C2177.1 (8)
C8—C7—C10—N31.9 (10)C3—C2—C5—N10.0
C6—C7—C10—N3178.2 (6)C1—C2—C5—N1179.4 (6)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N3—H3N···O1ii0.862.192.877 (13)136
N3—H3N···O2ii0.862.102.883 (7)152
N4—H4N···O8iii0.861.912.768 (7)175
N5—H5N···O11iv0.861.952.786 (7)164
N6—H6N···O4ii0.861.862.709 (6)167
O1W—H1W1···O4v0.852.042.822 (7)153
O1W—H1W2···O11vi0.852.142.921 (6)153
Symmetry codes: (ii) x+1, y, z; (iii) x+1, y+1, z; (iv) x+2, y+1, z; (v) x, y, z; (vi) x1, y, z.

Experimental details

Crystal data
Chemical formula[Nd2(C5H2N2O4)(C5H3N2O4)4(C12H8N2)2(H2O)2]·6H2O
Mr1567.48
Crystal system, space groupTriclinic, P1
Temperature (K)295
a, b, c (Å)10.1980 (7), 12.8896 (9), 13.3383 (9)
α, β, γ (°)118.711 (1), 90.010 (1), 108.612 (1)
V3)1432.25 (17)
Z1
Radiation typeMo Kα
µ (mm1)1.90
Crystal size (mm)0.10 × 0.04 × 0.02
Data collection
DiffractometerBruker APEXII
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.724, 0.963
No. of measured, independent and
observed [I > 2σ(I)] reflections
12405, 6377, 5349
Rint0.039
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.054, 0.136, 1.04
No. of reflections6377
No. of parameters454
No. of restraints84
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.23, 0.90

Computer programs: APEX2 (Bruker, 2006), SAINT (Bruker, 2006), atomic coordinates taken from the Pr analog (Sun & Jin, 2004), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2008).

Selected geometric parameters (Å, º) top
Nd1—O22.526 (4)Nd1—O102.526 (4)
Nd1—O32.502 (9)Nd1—O1W2.475 (4)
Nd1—O52.392 (4)Nd1—N72.638 (5)
Nd1—O62.575 (4)Nd1—N82.725 (5)
Nd1—O92.341 (4)
O2—Nd1—O367.5 (2)O5—Nd1—O1W78.2 (2)
O2—Nd1—O571.6 (1)O5—Nd1—N783.8 (2)
O2—Nd1—O6123.5 (1)O5—Nd1—N8138.8 (2)
O2—Nd1—O9127.7 (1)O6—Nd1—O972.6 (1)
O2—Nd1—O1071.8 (1)O6—Nd1—O1067.7 (1)
O2—Nd1—O1W136.6 (2)O6—Nd1—O1W69.0 (1)
O2—Nd1—N770.6 (2)O6—Nd1—N7138.2 (2)
O2—Nd1—N8111.7 (2)O6—Nd1—N8124.8 (2)
O3—Nd1—O5138.7 (2)O9—Nd1—O1071.5 (1)
O3—Nd1—O6133.6 (3)O9—Nd1—O1W95.5 (2)
O3—Nd1—O968.6 (3)O9—Nd1—N7133.8 (2)
O3—Nd1—O1076.5 (3)O9—Nd1—N872.8 (2)
O3—Nd1—O1W138.2 (3)O10—Nd1—O1W136.7 (2)
O3—Nd1—N787.9 (3)O10—Nd1—N7142.5 (2)
O3—Nd1—N865.6 (3)O10—Nd1—N8135.1 (2)
O5—Nd1—O667.9 (1)O1W—Nd1—N775.78 (16)
O5—Nd1—O9139.7 (2)O1W—Nd1—N872.93 (16)
O5—Nd1—O1085.9 (1)N7—Nd1—N861.14 (16)
 

Acknowledgements

The authors thank the Scientifc Research Foundation of Guangxi Normal University, the Science Foundation of Guangxi (grant No. 0542021) and the University of Malaya for supporting this study.

References

First citationBarbour, L. J. (2001). J. Supramol. Chem., 1, 189–191.  CrossRef CAS Google Scholar
First citationBruker (2006). APEX2 and SAINT. Bruker AXS Inc., Madison, Winconsin, 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 citationSun, C.-Y. & Jin, L. P. (2004). Polyhedron, 23, 2085–2093.  Web of Science CSD CrossRef CAS Google Scholar
First citationWestrip, S. P. (2008). publCIF. In preparation.  Google Scholar
First citationXing, H.-H., Chen, Z.-L. & Ng, S. W. (2008). Acta Cryst. E64, m418.  Web of Science CSD CrossRef IUCr Journals Google Scholar

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ISSN: 2056-9890
Volume 64| Part 2| February 2008| Pages m419-m420
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