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

Zhang, W.; Chen, Y.; Lei, T.; Li, Y.; Li, W.

doi:10.1107/S1600536811012360

metal-organic compounds

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ISSN: 2056-9890

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

doi:10.1107/S1600536811012360

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

Wenjun Zhang,^a Yanmei Chen,^a Tao Lei,^a Yahong Li ^a,^b ^* and Wu Li ^a

^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 Pr^III 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 Pr^III 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 ); 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

Crystal data

(C₃H₅N₂)₂[Pr₂(C₇H₃NO₄)₄(H₂O)₄]
M_r = 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 ) T_min = 0.652, T_max = 0.809
14917 measured reflections
3561 independent reflections
3468 reflections with I > 2σ(I)
R_int = 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
Δρ_max = 0.33 e Å⁻³
Δρ_min = −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	D⋯A	D—H⋯A
N4—H4⋯O2^iv	0.86	1.85	2.679 (3)	160
N3—H3A⋯O6^v	0.86	1.88	2.735 (3)	172
N3—H3A⋯O5^v	0.86	2.59	3.063 (3)	115
O9—H9A⋯O1^vi	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); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; 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.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811012360/jh2277sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811012360/jh2277Isup2.hkl

checkCIF report

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.

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

	Fig. 1. Molecular structure of 1 showing 50% probability displacement ellipsoids.
	Fig. 2. One-dimensional chain structure of 1 viewed down the b-axis
	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
M_r = 1152.48	F(000) = 568
Triclinic, P1	char
Hall symbol: -p 1	D_x = 1.887 Mg m⁻³
a = 9.5444 (19) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.667 (2) Å	Cell parameters from 3561 reflections
c = 11.222 (2) Å	θ = 2.6–25.5°
α = 64.63 (3)°	µ = 2.47 mm⁻¹
β = 79.50 (3)°	T = 293 K
γ = 87.50 (3)°	Block, light green
V = 1014.3 (3) Å³	0.19 × 0.16 × 0.09 mm

Data collection top

Bruker SMART CCD area-detector diffractometer	3561 independent reflections
Radiation source: fine-focus sealed tube	3468 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.020
ω scans	θ_max = 25.0°, θ_min = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2001)	h = −11→11
T_min = 0.652, T_max = 0.809	k = −12→12
14917 measured reflections	l = −13→13

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.015	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.043	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	w = 1/[σ²(F_o²) + (0.0271P)² + 0.5143P] where P = (F_o² + 2F_c²)/3
3561 reflections	(Δ/σ)_max = 0.068
305 parameters	Δρ_max = 0.33 e Å⁻³
0 restraints	Δρ_min = −0.45 e Å⁻³

Crystal data top

(C₃H₅N₂)₂[Pr₂(C₇H₃NO₄)₄(H₂O)₄]	γ = 87.50 (3)°
M_r = 1152.48	V = 1014.3 (3) Å³
Triclinic, P1	Z = 1
a = 9.5444 (19) Å	Mo Kα radiation
b = 10.667 (2) Å	µ = 2.47 mm⁻¹
c = 11.222 (2) Å	T = 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)
T_min = 0.652, T_max = 0.809	R_int = 0.020
14917 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.015	0 restraints
wR(F²) = 0.043	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	Δρ_max = 0.33 e Å⁻³
3561 reflections	Δρ_min = −0.45 e Å⁻³
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

	x	y	z	U_iso*/U_eq
Pr1	0.194718 (10)	0.107410 (10)	0.725374 (9)	0.01889 (5)
O1	0.17790 (15)	0.14537 (16)	0.92701 (14)	0.0277 (3)
N1	0.43859 (18)	0.13489 (18)	0.79437 (16)	0.0228 (4)
O4	0.94311 (15)	0.15185 (18)	0.73503 (16)	0.0337 (4)
N2	0.36969 (19)	0.25158 (18)	0.49260 (17)	0.0250 (4)
C5	0.5686 (2)	0.1198 (2)	0.7350 (2)	0.0252 (4)
H5	0.5761	0.0949	0.6642	0.030*
O9	0.0720 (2)	−0.1109 (2)	0.89507 (19)	0.0386 (4)
O5	0.19850 (19)	0.35430 (16)	0.63801 (16)	0.0379 (4)
O10	0.1175 (2)	0.0591 (2)	0.5508 (2)	0.0473 (5)
C7	0.8356 (2)	0.1232 (2)	0.7005 (2)	0.0263 (5)
O3	0.83952 (17)	0.0841 (2)	0.60974 (18)	0.0429 (4)
C1	0.4287 (2)	0.1698 (2)	0.89743 (19)	0.0205 (4)
C6	0.2795 (2)	0.1837 (2)	0.9634 (2)	0.0248 (4)
O6	0.2580 (2)	0.57179 (18)	0.49073 (19)	0.0560 (6)
C2	0.5464 (2)	0.1908 (2)	0.9421 (2)	0.0269 (5)
H2	0.5361	0.2152	1.0133	0.032*
C4	0.6928 (2)	0.1394 (2)	0.7731 (2)	0.0223 (4)
C8	0.3728 (2)	0.3897 (2)	0.4479 (2)	0.0291 (5)
O2	0.26769 (19)	0.2280 (2)	1.0488 (2)	0.0498 (5)
C13	0.2689 (3)	0.4449 (2)	0.5310 (2)	0.0325 (5)
C3	0.6802 (2)	0.1750 (2)	0.8796 (2)	0.0264 (4)
H3	0.7611	0.1882	0.9088	0.032*
C12	0.4576 (2)	0.1982 (2)	0.4206 (2)	0.0263 (4)
H12	0.4542	0.1025	0.4494	0.032*
N4	0.0958 (3)	0.3420 (3)	0.1892 (2)	0.0493 (6)
H4	0.1334	0.2930	0.1485	0.059*
C15	−0.0147 (3)	0.3044 (3)	0.2871 (3)	0.0434 (6)
H15	−0.0651	0.2196	0.3246	0.052*
C17	0.0534 (4)	0.5118 (3)	0.2475 (4)	0.0757 (12)
H17	0.0578	0.5961	0.2529	0.091*
N3	−0.0426 (3)	0.4050 (2)	0.3233 (2)	0.0471 (6)
H3A	−0.1110	0.4039	0.3854	0.056*
C16	0.1408 (4)	0.4721 (3)	0.1631 (4)	0.0760 (12)
H16	0.2177	0.5237	0.0987	0.091*
C11	0.5533 (2)	0.2772 (2)	0.3059 (2)	0.0262 (5)
C14	0.6545 (2)	0.2095 (2)	0.2339 (2)	0.0259 (4)
C10	0.5552 (3)	0.4201 (3)	0.2616 (3)	0.0439 (7)
H10	0.6176	0.4769	0.1845	0.053*
C9	0.4634 (3)	0.4765 (2)	0.3334 (3)	0.0460 (7)
H9	0.4624	0.5722	0.3051	0.055*
O8	0.7309 (2)	0.28565 (18)	0.12655 (17)	0.0446 (5)
O7	0.65553 (16)	0.07807 (15)	0.28965 (15)	0.0308 (3)
H9A	0.002 (4)	−0.129 (3)	0.946 (3)	0.041 (8)*
H10A	0.025 (4)	0.069 (3)	0.564 (3)	0.062 (10)*
H10B	0.149 (4)	0.034 (4)	0.501 (4)	0.066 (12)*
H9B	0.111 (4)	−0.174 (3)	0.904 (3)	0.047 (10)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pr1	0.01230 (7)	0.02507 (7)	0.02203 (7)	0.00136 (5)	0.00114 (5)	−0.01435 (5)
O1	0.0164 (7)	0.0434 (9)	0.0278 (7)	−0.0005 (6)	0.0028 (6)	−0.0218 (7)
N1	0.0155 (8)	0.0325 (9)	0.0258 (8)	0.0028 (7)	−0.0017 (7)	−0.0184 (7)
O4	0.0152 (8)	0.0515 (10)	0.0452 (9)	0.0058 (7)	−0.0054 (7)	−0.0313 (8)
N2	0.0237 (9)	0.0243 (9)	0.0255 (8)	0.0045 (7)	0.0023 (7)	−0.0122 (7)
C5	0.0183 (11)	0.0369 (12)	0.0272 (10)	0.0040 (9)	−0.0011 (8)	−0.0213 (9)
O9	0.0263 (9)	0.0326 (10)	0.0447 (10)	0.0001 (8)	0.0163 (8)	−0.0139 (8)
O5	0.0420 (10)	0.0259 (8)	0.0365 (9)	0.0040 (7)	0.0156 (7)	−0.0139 (7)
O10	0.0226 (10)	0.0907 (16)	0.0575 (12)	0.0071 (9)	−0.0061 (8)	−0.0598 (12)
C7	0.0170 (11)	0.0327 (11)	0.0320 (11)	0.0055 (9)	−0.0022 (9)	−0.0178 (9)
O3	0.0201 (8)	0.0775 (13)	0.0533 (10)	0.0061 (8)	−0.0017 (7)	−0.0512 (10)
C1	0.0184 (10)	0.0224 (9)	0.0210 (9)	0.0024 (8)	0.0003 (8)	−0.0113 (8)
C6	0.0210 (11)	0.0292 (11)	0.0259 (10)	0.0025 (9)	0.0015 (8)	−0.0157 (9)
O6	0.0734 (14)	0.0263 (9)	0.0484 (11)	0.0104 (9)	0.0250 (10)	−0.0122 (8)
C2	0.0255 (11)	0.0359 (12)	0.0248 (10)	0.0018 (9)	−0.0016 (9)	−0.0192 (9)
C4	0.0166 (10)	0.0255 (10)	0.0240 (10)	0.0028 (8)	−0.0013 (8)	−0.0111 (8)
C8	0.0301 (12)	0.0260 (11)	0.0286 (11)	0.0062 (9)	0.0020 (9)	−0.0126 (9)
O2	0.0279 (9)	0.0867 (14)	0.0640 (12)	0.0029 (9)	0.0032 (8)	−0.0643 (12)
C13	0.0342 (13)	0.0275 (12)	0.0332 (11)	0.0086 (10)	0.0041 (10)	−0.0155 (10)
C3	0.0187 (10)	0.0351 (11)	0.0300 (10)	0.0024 (9)	−0.0059 (8)	−0.0177 (9)
C12	0.0277 (11)	0.0218 (10)	0.0274 (10)	0.0045 (9)	0.0025 (9)	−0.0117 (9)
N4	0.0505 (14)	0.0556 (14)	0.0455 (13)	0.0149 (12)	0.0073 (11)	−0.0326 (11)
C15	0.0455 (16)	0.0406 (14)	0.0449 (14)	0.0077 (12)	0.0026 (12)	−0.0239 (12)
C17	0.080 (3)	0.0472 (18)	0.089 (3)	−0.0075 (17)	0.039 (2)	−0.0394 (18)
N3	0.0485 (14)	0.0444 (12)	0.0450 (12)	0.0069 (11)	0.0155 (11)	−0.0259 (10)
C16	0.074 (2)	0.0543 (19)	0.078 (2)	−0.0050 (17)	0.0407 (19)	−0.0288 (17)
C11	0.0247 (11)	0.0277 (11)	0.0249 (10)	0.0054 (9)	0.0004 (9)	−0.0122 (9)
C14	0.0209 (11)	0.0324 (11)	0.0271 (10)	0.0040 (9)	0.0000 (9)	−0.0172 (9)
C10	0.0512 (16)	0.0282 (12)	0.0367 (13)	0.0020 (11)	0.0191 (12)	−0.0099 (10)
C9	0.0570 (18)	0.0217 (11)	0.0423 (14)	0.0075 (11)	0.0175 (13)	−0.0089 (10)
O8	0.0481 (11)	0.0357 (9)	0.0361 (9)	0.0047 (8)	0.0184 (8)	−0.0128 (7)
O7	0.0261 (8)	0.0275 (8)	0.0378 (8)	0.0042 (6)	0.0054 (7)	−0.0176 (7)

Geometric parameters (Å, º) top

Pr1—O5	2.3835 (17)	O6—C13	1.236 (3)
Pr1—O4ⁱ	2.4193 (16)	C2—C3	1.380 (3)
Pr1—O7ⁱⁱ	2.4366 (16)	C2—H2	0.9300
Pr1—O1	2.4407 (15)	C4—C3	1.385 (3)
Pr1—O10	2.4643 (18)	C8—C9	1.379 (3)
Pr1—O9	2.459 (2)	C8—C13	1.511 (3)
Pr1—N1	2.6484 (18)	C3—H3	0.9300
Pr1—N2	2.677 (2)	C12—C11	1.382 (3)
O1—C6	1.263 (3)	C12—H12	0.9300
N1—C5	1.335 (3)	N4—C15	1.310 (4)
N1—C1	1.346 (3)	N4—C16	1.361 (4)
O4—C7	1.253 (3)	N4—H4	0.8600
O4—Pr1ⁱⁱⁱ	2.4193 (16)	C15—N3	1.303 (3)
N2—C8	1.337 (3)	C15—H15	0.9300
N2—C12	1.336 (3)	C17—C16	1.341 (4)
C5—C4	1.384 (3)	C17—N3	1.355 (4)
C5—H5	0.9300	C17—H17	0.9300
O9—H9A	0.77 (3)	N3—H3A	0.8600
O9—H9B	0.73 (3)	C16—H16	0.9300
O5—C13	1.263 (3)	C11—C10	1.386 (3)
O10—H10A	0.88 (4)	C11—C14	1.504 (3)
O10—H10B	0.73 (4)	C14—O8	1.240 (3)
C7—O3	1.249 (3)	C14—O7	1.267 (3)
C7—C4	1.499 (3)	C10—C9	1.376 (3)
C1—C2	1.373 (3)	C10—H10	0.9300
C1—C6	1.513 (3)	C9—H9	0.9300
C6—O2	1.224 (3)	O7—Pr1ⁱⁱ	2.4366 (16)

O5—Pr1—O4ⁱ	78.67 (7)	C2—C1—C6	121.25 (18)
O5—Pr1—O7ⁱⁱ	139.99 (6)	O2—C6—O1	125.8 (2)
O4ⁱ—Pr1—O7ⁱⁱ	135.10 (6)	O2—C6—C1	117.6 (2)
O5—Pr1—O1	77.58 (6)	O1—C6—C1	116.62 (17)
O4ⁱ—Pr1—O1	87.46 (6)	C1—C2—C3	119.03 (19)
O7ⁱⁱ—Pr1—O1	117.28 (6)	C1—C2—H2	120.5
O5—Pr1—O10	104.04 (8)	C3—C2—H2	120.5
O4ⁱ—Pr1—O10	72.69 (6)	C3—C4—C5	117.72 (19)
O7ⁱⁱ—Pr1—O10	75.16 (7)	C3—C4—C7	121.57 (19)
O1—Pr1—O10	159.11 (6)	C5—C4—C7	120.71 (18)
O5—Pr1—O9	145.52 (6)	N2—C8—C9	122.7 (2)
O4ⁱ—Pr1—O9	74.82 (7)	N2—C8—C13	115.37 (19)
O7ⁱⁱ—Pr1—O9	73.98 (6)	C9—C8—C13	121.9 (2)
O1—Pr1—O9	79.59 (6)	O6—C13—O5	125.2 (2)
O10—Pr1—O9	88.76 (8)	O6—C13—C8	119.1 (2)
O5—Pr1—N1	83.59 (7)	O5—C13—C8	115.67 (19)
O4ⁱ—Pr1—N1	148.64 (5)	C2—C3—C4	119.4 (2)
O7ⁱⁱ—Pr1—N1	73.00 (6)	C2—C3—H3	120.3
O1—Pr1—N1	63.42 (5)	C4—C3—H3	120.3
O10—Pr1—N1	137.32 (6)	N2—C12—C11	123.74 (19)
O9—Pr1—N1	108.60 (7)	N2—C12—H12	118.1
O5—Pr1—N2	62.40 (6)	C11—C12—H12	118.1
O4ⁱ—Pr1—N2	117.33 (6)	C15—N4—C16	108.2 (2)
O7ⁱⁱ—Pr1—N2	80.22 (6)	C15—N4—H4	125.9
O1—Pr1—N2	124.85 (5)	C16—N4—H4	125.9
O10—Pr1—N2	71.92 (7)	N3—C15—N4	109.0 (3)
O9—Pr1—N2	151.07 (6)	N3—C15—H15	125.5
N1—Pr1—N2	75.27 (6)	N4—C15—H15	125.5
C6—O1—Pr1	125.79 (12)	C16—C17—N3	106.5 (3)
C5—N1—C1	117.88 (18)	C16—C17—H17	126.8
C5—N1—Pr1	126.03 (13)	N3—C17—H17	126.8
C1—N1—Pr1	116.08 (13)	C15—N3—C17	109.1 (2)
C7—O4—Pr1ⁱⁱⁱ	140.65 (14)	C15—N3—H3A	125.4
C8—N2—C12	117.46 (18)	C17—N3—H3A	125.4
C8—N2—Pr1	116.34 (13)	C17—C16—N4	107.2 (3)
C12—N2—Pr1	126.14 (13)	C17—C16—H16	126.4
N1—C5—C4	123.45 (19)	N4—C16—H16	126.4
N1—C5—H5	118.3	C12—C11—C10	117.9 (2)
C4—C5—H5	118.3	C12—C11—C14	120.9 (2)
Pr1—O9—H9A	134 (2)	C10—C11—C14	121.2 (2)
Pr1—O9—H9B	115 (3)	O8—C14—O7	125.3 (2)
H9A—O9—H9B	111 (3)	O8—C14—C11	118.0 (2)
C13—O5—Pr1	130.05 (14)	O7—C14—C11	116.74 (18)
Pr1—O10—H10A	103 (2)	C9—C10—C11	119.0 (2)
Pr1—O10—H10B	137 (3)	C9—C10—H10	120.5
H10A—O10—H10B	119 (4)	C11—C10—H10	120.5
O3—C7—O4	124.8 (2)	C10—C9—C8	119.3 (2)
O3—C7—C4	118.38 (19)	C10—C9—H9	120.4
O4—C7—C4	116.84 (19)	C8—C9—H9	120.4
N1—C1—C2	122.48 (18)	C14—O7—Pr1ⁱⁱ	138.92 (13)
N1—C1—C6	116.26 (18)

Symmetry codes: (i) x−1, y, z; (ii) −x+1, −y, −z+1; (iii) x+1, y, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N4—H4···O2^iv	0.86	1.85	2.679 (3)	160
N3—H3A···O6^v	0.86	1.88	2.735 (3)	172
N3—H3A···O5^v	0.86	2.59	3.063 (3)	115
O9—H9A···O1^vi	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.

Experimental details

Crystal data
Chemical formula	(C₃H₅N₂)₂[Pr₂(C₇H₃NO₄)₄(H₂O)₄]
M_r	1152.48
Crystal system, space group	Triclinic, 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)
V (Å³)	1014.3 (3)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	2.47
Crystal size (mm)	0.19 × 0.16 × 0.09

Data collection
Diffractometer	Bruker SMART CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2001)
T_min, T_max	0.652, 0.809
No. of measured, independent and observed [I > 2σ(I)] reflections	14917, 3561, 3468
R_int	0.020
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.015, 0.043, 1.04
No. of reflections	3561
No. of parameters	305
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	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—O5	2.3835 (17)	Pr1—O10	2.4643 (18)
Pr1—O4ⁱ	2.4193 (16)	Pr1—O9	2.459 (2)
Pr1—O7ⁱⁱ	2.4366 (16)	Pr1—N1	2.6484 (18)
Pr1—O1	2.4407 (15)	Pr1—N2	2.677 (2)

O5—Pr1—O4ⁱ	78.67 (7)	O1—Pr1—N1	63.42 (5)
O5—Pr1—O7ⁱⁱ	139.99 (6)	O10—Pr1—N1	137.32 (6)
O4ⁱ—Pr1—O7ⁱⁱ	135.10 (6)	O9—Pr1—N1	108.60 (7)
O5—Pr1—O1	77.58 (6)	O5—Pr1—N2	62.40 (6)
O4ⁱ—Pr1—O1	87.46 (6)	O4ⁱ—Pr1—N2	117.33 (6)
O7ⁱⁱ—Pr1—O1	117.28 (6)	O7ⁱⁱ—Pr1—N2	80.22 (6)
O5—Pr1—O10	104.04 (8)	O1—Pr1—N2	124.85 (5)
O4ⁱ—Pr1—O10	72.69 (6)	O10—Pr1—N2	71.92 (7)
O7ⁱⁱ—Pr1—O10	75.16 (7)	O9—Pr1—N2	151.07 (6)
O1—Pr1—O10	159.11 (6)	N1—Pr1—N2	75.27 (6)
O5—Pr1—O9	145.52 (6)	C6—O1—Pr1	125.79 (12)
O4ⁱ—Pr1—O9	74.82 (7)	C5—N1—C1	117.88 (18)
O7ⁱⁱ—Pr1—O9	73.98 (6)	C5—N1—Pr1	126.03 (13)
O1—Pr1—O9	79.59 (6)	C1—N1—Pr1	116.08 (13)
O10—Pr1—O9	88.76 (8)	C7—O4—Pr1ⁱⁱⁱ	140.65 (14)
O5—Pr1—N1	83.59 (7)	C8—N2—Pr1	116.34 (13)
O4ⁱ—Pr1—N1	148.64 (5)	C12—N2—Pr1	126.14 (13)
O7ⁱⁱ—Pr1—N1	73.00 (6)

Symmetry codes: (i) x−1, y, z; (ii) −x+1, −y, −z+1; (iii) x+1, y, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N4—H4···O2^iv	0.86	1.85	2.679 (3)	160
N3—H3A···O6^v	0.86	1.88	2.735 (3)	172
N3—H3A···O5^v	0.86	2.59	3.063 (3)	115
O9—H9A···O1^vi	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.

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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ISSN: 2056-9890

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

doi:10.1107/S1600536811012360

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

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

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Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

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