catena-Poly[[[tetra­aqua­praseo­dym­ium(III)]-di-μ-nicotinato-κ2O:N;κ2O:N-disilver(I)-di-μ-nicotinato-κ2N:O;κ2N:O] perchlorate monohydrate]

Guan, B.; Zhang, C.-H.; Song, W.-D.

doi:10.1107/S1600536809001718

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 2| February 2009| Pages m208-m209

doi:10.1107/S1600536809001718

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catena-Poly[[[tetraaquapraseodymium(III)]-di-μ-nicotinato-κ²O:N;κ²O:N-disilver(I)-di-μ-nicotinato-κ²N:O;κ²N:O] perchlorate monohydrate]

Biao Guan,^a Chao-Hua Zhang ^b and Wen-Dong Song ^c ^*

^aLaboratory and Facility Management Division, Guangdong Ocean University, Zhanjiang 524088, People's Republic of China, ^bSchool of Food Science and Technology, Guangdong Ocean University, Zhanjiang 524088, People's Republic of China, and ^cCollege of Science, Guangdong Ocean University, Zhanjiang 524088, People's Republic of China
^*Correspondence e-mail: songwd60@126.com

(Received 28 December 2008; accepted 14 January 2009; online 17 January 2009)

In the title compound, {[Ag₂Pr(C₆H₄NO₂)₄(H₂O)₄]ClO₄·H₂O}_n, the Pr^III atom, lying on a twofold rotation axis, has a distorted square-antiprismatic coordination geometry, defined by four O atoms from four nicotinate (nic) ligands and four water molecules. The Ag^I atom is coordinated in an almost linear fashion by two pyridyl N atoms from two nicotinate ligands. The linear coordination is augmented by weak interactions with three O atoms from one perchlorate anion, one uncoordinated water molecule and one carboxylate group. Two Pr atoms link two {Ag(nic)₂}⁺ units into a ring, which is further extended into an infinite zigzag chain by sharing the Pr atoms. These chains are further connected into a three-dimensional network via weak Ag⋯O interactions, O—H⋯O hydrogen bonds, Ag⋯Ag interactions [3.357 (2) Å] and π–π interactions between the pyridyl rings [centroid–centroid distance = 3.685 (4) Å].

Related literature

For general background, see: Cheng et al. (2007a ,b ); Luo et al. (2006 , 2007 ).

Experimental

Crystal data

[Ag₂Pr(C₆H₄NO₂)₄(H₂O)₄]ClO₄·H₂O
M_r = 1034.59
Orthorhombic, C m c a
a = 35.396 (3) Å
b = 12.3733 (10) Å
c = 15.2324 (13) Å
V = 6671.2 (10) Å³
Z = 8
Mo Kα radiation
μ = 2.76 mm⁻¹
T = 273 (2) K
0.30 × 0.25 × 0.22 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.453, T_max = 0.552
16336 measured reflections
3065 independent reflections
2478 reflections with I > 2σ(I)
R_int = 0.049

Refinement

R[F² > 2σ(F²)] = 0.036
wR(F²) = 0.097
S = 1.06
3065 reflections
227 parameters
27 restraints
H-atom parameters constrained
Δρ_max = 1.56 e Å⁻³
Δρ_min = −0.87 e Å⁻³

Table 1
Selected bond lengths (Å)

Pr1—O3ⁱ	2.390 (14)
Pr1—O1W	2.477 (14)
Pr1—O2W	2.495 (14)
Pr1—O1	2.504 (13)
Ag1—N2	2.165 (18)
Ag1—N1	2.175 (18)
Ag1—O4ⁱⁱ	2.777 (16)
Ag1—O5	2.81 (3)
Ag1—O3W	2.90 (2)
Symmetry codes: (i) $[-x+{\script{1\over 2}}, -y+{\script{3\over 2}}, -z+1]$ ; (ii) $[x, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]$ .

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1W⋯O2ⁱⁱⁱ	0.88	1.79	2.67 (2)	179
O1W—H2W⋯O4^iv	0.97	1.68	2.63 (2)	163
O2W—H3W⋯O2^v	1.00	1.77	2.77 (2)	176
O2W—H4W⋯O2^vi	0.83	1.95	2.76 (2)	162
O3W—H5W⋯O1W^vii	0.82	2.15	2.91 (2)	157
Symmetry codes: (iii) $[-x+{\script{1\over 2}}, y, -z+{\script{1\over 2}}]$ ; (iv) x, -y+1, -z+1; (v) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, z]$ ; (vi) x, -y+2, -z+1; (vii) $[x, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

Data collection: APEX2 (Bruker, 2007 ); cell refinement: SAINT (Bruker, 2007); 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/S1600536809001718/hy2177sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809001718/hy2177Isup2.hkl

checkCIF report

Comment top

Nicotinic acid is a multifunctional bridging ligand possessing of O and N donors, which can thus be utilized to construct lanthanide–transition heterometallic complexes, via carboxylate O atoms binding to lanthanides and N atoms binding to transition metal ions such as Ag^I or Cu^I (Cheng et al., 2007a,b; Luo et al., 2006, 2007). On the basis of above considerations, we chose nicotinic acid, Pr^III and Ag^I metal ions as building blocks. A new one-dimensional 4 d–4f coordination polymer was obtained from the hydrothermal treatment of Pr₆O₁₁, AgNO₃, perchloric acid and nicotinic acid in water.

In the title compound (Fig. 1), the Pr^III atom, lying on a twofold rotation axis, has a distorted square-antiprismatic coordination geometry, defined by four O atoms from four nicotinate (nic) ligands and four water molecules. The perchlorate anion lies on a mirror plane and the uncoordinated water molecule lies on a twofold rotation axis. The Ag^I atom is coordinated in an almost linear fashion by two pyridyl N atoms from two nic ligands. The linear coordination are augmented by weak Ag···O interactions with one O atom from the ClO₄^- anion, one O atom from the uncoordinated water molecule and one carboxylate O atom from the nic ligand (Table 1). The Ag atom also exhibits an argentophilic interaction, with an Ag···Ag distance of 3.357 (1) Å. The pyridyl rings of the nic ligands coordinating to the Ag atom are almost coplanar and have a dihedral angle of 1.74 (2)°. Two Pr atoms link two Ag(nic)₂⁺ units into a ring, which are further extended into an infinite zigzag chain by sharing the common Pr atoms (Fig. 2). These chains are further connected into a three-dimensional network via the weak Ag···O interactions, O—H···O hydrogen bonds (Table 2), weak Ag···Ag interactions and π–π interactions occurring between the pyridyl rings of neighboring nic ligands [centroid–centroid distance = 3.685 (4) Å].

Related literature top

For general background, see: Cheng et al. (2007a,b); Luo et al. (2006, 2007).

Experimental top

A mixture of Pr₆O₁₁ (0.170 g, 0.5 mmol), AgNO₃ (0.169 g, 1 mmol), nicotinic acid (0.123 g, 1 mmol), HClO₄ (0.12 ml) and H₂O (10 ml) was placed in a 23 ml Teflon-lined reactor, which was heated to 433 K for 3 d and then cooled to room temperature at a rate of 10 K h^-1. The pale-purple plate crystals obtained were washed with water and dried in air (yield 46% based on Pr).

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); 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. The asymmetric unit of the title compound, extended to show the Pr and Ag coordination environments. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry codes: (i) 1/2 - x, 3/2 - y, 1 - z; (ii) x, 1/2 + y, 3/2 - z; (iii) 1/2 - x, y, 1/2 - z; (viii) x, 3/2 - y, -1/2 + z; (ix) -x, y, z.]
	Fig. 2. View of the zigzag chain in the title compound.

catena-Poly[[[tetraaquapraseodymium(III)]-di-µ-nicotinato- κ²O:N;κ²O:N-disilver(I)-di-µ-nicotinato- κ²N:O;κ²N:O] perchlorate monohydrate] top

Crystal data top

[Ag₂Pr(C₆H₄NO₂)₄(H₂O)₄]ClO₄·H₂O	F(000) = 4032
M_r = 1034.59	D_x = 2.060 Mg m⁻³
Orthorhombic, Cmca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2bc 2	Cell parameters from 3121 reflections
a = 35.396 (3) Å	θ = 1.4–28°
b = 12.3733 (10) Å	µ = 2.76 mm⁻¹
c = 15.2324 (13) Å	T = 273 K
V = 6671.2 (10) Å³	Plate, pale purple
Z = 8	0.30 × 0.25 × 0.22 mm

Data collection top

Bruker APEXII CCD diffractometer	3065 independent reflections
Radiation source: fine-focus sealed tube	2478 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.049
ϕ and ω scans	θ_max = 25.2°, θ_min = 2.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −28→42
T_min = 0.453, T_max = 0.552	k = −13→14
16336 measured reflections	l = −18→18

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)] = 0.036	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.097	H-atom parameters constrained
S = 1.06	w = 1/[σ²(F_o²) + (0.0479P)² + 31.5675P] where P = (F_o² + 2F_c²)/3
3065 reflections	(Δ/σ)_max < 0.001
227 parameters	Δρ_max = 1.56 e Å⁻³
27 restraints	Δρ_min = −0.87 e Å⁻³

Crystal data top

[Ag₂Pr(C₆H₄NO₂)₄(H₂O)₄]ClO₄·H₂O	V = 6671.2 (10) Å³
M_r = 1034.59	Z = 8
Orthorhombic, Cmca	Mo Kα radiation
a = 35.396 (3) Å	µ = 2.76 mm⁻¹
b = 12.3733 (10) Å	T = 273 K
c = 15.2324 (13) Å	0.30 × 0.25 × 0.22 mm

Data collection top

Bruker APEXII CCD diffractometer	3065 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	2478 reflections with I > 2σ(I)
T_min = 0.453, T_max = 0.552	R_int = 0.049
16336 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.036	27 restraints
wR(F²) = 0.097	H-atom parameters constrained
S = 1.06	w = 1/[σ²(F_o²) + (0.0479P)² + 31.5675P] where P = (F_o² + 2F_c²)/3
3065 reflections	Δρ_max = 1.56 e Å⁻³
227 parameters	Δρ_min = −0.87 e Å⁻³

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Pr1	0.2500	1.08315 (12)	0.2500	0.0216 (5)
Ag1	0.11088 (6)	0.60988 (15)	0.56463 (12)	0.0439 (6)
C2	0.1570 (6)	0.8876 (17)	0.4208 (13)	0.031 (5)
C6	0.1963 (6)	0.9230 (16)	0.3979 (13)	0.027 (4)
C3	0.1260 (7)	0.943 (2)	0.3901 (17)	0.048 (6)
H3	0.1292	1.0038	0.3555	0.058*
C1	0.1508 (6)	0.7976 (18)	0.4725 (13)	0.033 (5)
H1	0.1716	0.7607	0.4945	0.040*
C4	0.0904 (8)	0.908 (2)	0.411 (2)	0.067 (9)
H4	0.0692	0.9439	0.3899	0.081*
C5	0.0867 (7)	0.816 (2)	0.4631 (18)	0.054 (7)
H5	0.0625	0.7927	0.4782	0.065*
N1	0.1163 (5)	0.7608 (15)	0.4925 (12)	0.040 (5)
O1	0.2002 (4)	0.9976 (12)	0.3439 (9)	0.035 (3)
O2	0.2235 (4)	0.8725 (12)	0.4344 (9)	0.033 (3)
N2	0.1025 (5)	0.4681 (15)	0.6456 (12)	0.037 (4)
C7	0.1323 (6)	0.4144 (16)	0.6770 (14)	0.032 (5)
H7	0.1563	0.4385	0.6610	0.038*
C11	0.0685 (8)	0.434 (2)	0.669 (2)	0.057 (8)
H11	0.0474	0.4718	0.6489	0.069*
Cl1	0.0000	0.6849 (10)	0.5898 (10)	0.080 (4)
O7	0.0000	0.803 (3)	0.588 (4)	0.150 (19)
O6	0.0000	0.647 (5)	0.685 (4)	0.25 (4)
C8	0.1300 (6)	0.3255 (16)	0.7316 (13)	0.030 (5)
C9	0.0945 (7)	0.292 (2)	0.7558 (19)	0.057 (8)
H9	0.0914	0.2344	0.7941	0.069*
C10	0.0631 (8)	0.346 (3)	0.723 (3)	0.082 (12)
H10	0.0388	0.3232	0.7362	0.098*
C12	0.1652 (6)	0.2676 (16)	0.7619 (13)	0.028 (4)
O3	0.1962 (4)	0.3019 (12)	0.7341 (9)	0.032 (3)
O4	0.1611 (4)	0.1878 (13)	0.8104 (11)	0.044 (4)
O1W	0.2180 (4)	0.9435 (12)	0.1603 (9)	0.035 (4)
H1W	0.2373	0.9195	0.1295	0.053*
H2W	0.1996	0.8918	0.1807	0.053*
O2W	0.2515 (5)	1.1653 (13)	0.3996 (10)	0.046 (4)
H3W	0.2615	1.2394	0.4110	0.069*
H4W	0.2454	1.1409	0.4486	0.069*
O3W	0.1776 (8)	0.5000	0.5000	0.080 (10)
H5W	0.1920	0.5010	0.4583	0.120*
O5	0.0324 (9)	0.643 (3)	0.565 (3)	0.19 (2)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pr1	0.0227 (9)	0.0223 (8)	0.0199 (8)	0.000	0.0012 (6)	0.000
Ag1	0.0482 (12)	0.0376 (11)	0.0458 (11)	−0.0044 (9)	0.0028 (8)	0.0151 (8)
C2	0.035 (12)	0.033 (11)	0.024 (10)	0.001 (10)	0.006 (9)	0.001 (9)
C6	0.032 (12)	0.025 (10)	0.023 (10)	0.000 (9)	0.005 (9)	−0.004 (8)
C3	0.038 (14)	0.051 (15)	0.054 (15)	0.000 (12)	0.009 (12)	0.023 (12)
C1	0.034 (12)	0.038 (12)	0.028 (10)	−0.003 (10)	0.003 (9)	0.004 (10)
C4	0.035 (15)	0.07 (2)	0.09 (2)	0.003 (14)	0.004 (15)	0.043 (17)
C5	0.034 (14)	0.060 (17)	0.069 (18)	−0.005 (13)	0.012 (12)	0.023 (14)
N1	0.039 (11)	0.040 (11)	0.040 (10)	−0.002 (9)	0.006 (8)	0.014 (9)
O1	0.034 (8)	0.032 (8)	0.037 (8)	0.000 (7)	0.005 (6)	0.013 (7)
O2	0.029 (8)	0.038 (8)	0.031 (8)	0.000 (7)	0.000 (6)	0.005 (7)
N2	0.034 (11)	0.033 (10)	0.045 (11)	0.000 (8)	0.002 (8)	0.010 (8)
C7	0.030 (12)	0.028 (11)	0.037 (12)	−0.006 (9)	0.001 (9)	0.001 (9)
C11	0.037 (15)	0.054 (17)	0.08 (2)	0.006 (12)	0.003 (13)	0.029 (15)
Cl1	0.040 (6)	0.070 (8)	0.130 (11)	0.000	0.000	0.009 (7)
O7	0.17 (5)	0.09 (3)	0.19 (5)	0.000	0.000	0.04 (3)
O6	0.45 (13)	0.14 (5)	0.15 (6)	0.000	0.000	0.02 (4)
C8	0.030 (12)	0.024 (11)	0.036 (12)	−0.002 (9)	0.004 (9)	0.001 (9)
C9	0.034 (14)	0.054 (16)	0.08 (2)	−0.002 (12)	0.005 (13)	0.042 (15)
C10	0.029 (15)	0.08 (2)	0.13 (3)	0.000 (15)	0.004 (17)	0.06 (2)
C12	0.026 (11)	0.028 (11)	0.031 (11)	0.000 (9)	0.003 (8)	−0.005 (9)
O3	0.027 (8)	0.031 (8)	0.037 (8)	−0.005 (6)	0.002 (6)	−0.005 (6)
O4	0.031 (9)	0.044 (10)	0.056 (10)	0.005 (7)	0.007 (7)	0.023 (8)
O1W	0.029 (8)	0.035 (8)	0.041 (9)	−0.006 (6)	0.006 (7)	−0.009 (7)
O2W	0.071 (12)	0.044 (10)	0.024 (8)	−0.021 (9)	0.013 (8)	−0.010 (7)
O3W	0.047 (16)	0.15 (3)	0.040 (14)	0.000	0.000	−0.002 (17)
O5	0.07 (2)	0.14 (3)	0.35 (6)	0.04 (2)	0.07 (3)	0.12 (3)

Geometric parameters (Å, º) top

Pr1—O3ⁱ	2.390 (14)	N2—C11	1.32 (3)
Pr1—O1W	2.477 (14)	N2—C7	1.34 (3)
Pr1—O2W	2.495 (14)	C7—C8	1.38 (3)
Pr1—O1	2.504 (13)	C7—H7	0.9300
Ag1—N2	2.165 (18)	C11—C10	1.37 (4)
Ag1—N1	2.175 (18)	C11—H11	0.9300
Ag1—O4ⁱⁱ	2.777 (16)	Cl1—O5^iv	1.31 (3)
Ag1—O5	2.81 (3)	Cl1—O5	1.31 (3)
Ag1—O3W	2.90 (2)	Cl1—O7	1.46 (4)
Ag1—Ag1ⁱⁱⁱ	3.357 (2)	Cl1—O6	1.52 (5)
C2—C3	1.37 (3)	C8—C9	1.37 (3)
C2—C1	1.38 (3)	C8—C12	1.51 (3)
C2—C6	1.50 (3)	C9—C10	1.39 (4)
C6—O1	1.24 (2)	C9—H9	0.9300
C6—O2	1.27 (3)	C10—H10	0.9300
C3—C4	1.37 (4)	C12—O4	1.24 (2)
C3—H3	0.9300	C12—O3	1.25 (2)
C1—N1	1.34 (3)	O1W—H1W	0.88
C1—H1	0.9300	O1W—H2W	0.97
C4—C5	1.39 (4)	O2W—H3W	1.00
C4—H4	0.9300	O2W—H4W	0.83
C5—N1	1.33 (3)	O3W—H5W	0.82
C5—H5	0.9300

O3ⁱ—Pr1—O3^v	106.9 (7)	C3—C4—H4	120.8
O3ⁱ—Pr1—O1W	146.7 (5)	C5—C4—H4	120.8
O3^v—Pr1—O1W	89.7 (5)	N1—C5—C4	123 (2)
O3ⁱ—Pr1—O1W^vi	89.7 (5)	N1—C5—H5	118.7
O3^v—Pr1—O1W^vi	146.7 (5)	C4—C5—H5	118.7
O1W—Pr1—O1W^vi	91.5 (7)	C5—N1—C1	118 (2)
O3ⁱ—Pr1—O2W	69.4 (5)	C5—N1—Ag1	122.9 (16)
O3^v—Pr1—O2W	82.3 (5)	C1—N1—Ag1	119.1 (15)
O1W—Pr1—O2W	142.9 (5)	C6—O1—Pr1	140.4 (13)
O1W^vi—Pr1—O2W	76.7 (5)	C11—N2—C7	118 (2)
O3ⁱ—Pr1—O2W^vi	82.3 (5)	C11—N2—Ag1	122.3 (16)
O3^v—Pr1—O2W^vi	69.4 (5)	C7—N2—Ag1	119.9 (14)
O1W—Pr1—O2W^vi	76.7 (5)	N2—C7—C8	124 (2)
O1W^vi—Pr1—O2W^vi	142.9 (5)	N2—C7—H7	117.8
O2W—Pr1—O2W^vi	131.9 (7)	C8—C7—H7	117.8
O3ⁱ—Pr1—O1	139.0 (5)	N2—C11—C10	123 (2)
O3^v—Pr1—O1	75.5 (5)	N2—C11—H11	118.7
O1W—Pr1—O1	72.5 (5)	C10—C11—H11	118.7
O1W^vi—Pr1—O1	73.2 (5)	O5^iv—Cl1—O5	122 (4)
O2W—Pr1—O1	70.5 (5)	O5^iv—Cl1—O7	113.2 (18)
O2W^vi—Pr1—O1	132.8 (5)	O5—Cl1—O7	113.2 (18)
O3ⁱ—Pr1—O1^vi	75.5 (5)	O5^iv—Cl1—O6	98 (2)
O3^v—Pr1—O1^vi	139.0 (5)	O5—Cl1—O6	98 (2)
O1W—Pr1—O1^vi	73.2 (5)	O7—Cl1—O6	109 (3)
O1W^vi—Pr1—O1^vi	72.5 (5)	C9—C8—C7	117 (2)
O2W—Pr1—O1^vi	132.8 (5)	C9—C8—C12	122.1 (19)
O2W^vi—Pr1—O1^vi	70.5 (5)	C7—C8—C12	120.9 (19)
O1—Pr1—O1^vi	129.9 (7)	C8—C9—C10	119 (2)
N2—Ag1—N1	174.6 (7)	C8—C9—H9	120.3
N2—Ag1—Ag1ⁱⁱⁱ	71.2 (5)	C10—C9—H9	120.3
N1—Ag1—Ag1ⁱⁱⁱ	113.5 (5)	C11—C10—C9	119 (3)
C3—C2—C1	118 (2)	C11—C10—H10	120.5
C3—C2—C6	121.2 (19)	C9—C10—H10	120.5
C1—C2—C6	121 (2)	O4—C12—O3	124.9 (19)
O1—C6—O2	124.6 (19)	O4—C12—C8	117.7 (18)
O1—C6—C2	118.3 (19)	O3—C12—C8	117.4 (18)
O2—C6—C2	117.1 (17)	C12—O3—Pr1ⁱ	150.2 (13)
C4—C3—C2	120 (2)	Pr1—O1W—H1W	100.1
C4—C3—H3	119.9	Pr1—O1W—H2W	126.4
C2—C3—H3	119.9	H1W—O1W—H2W	118.2
N1—C1—C2	123 (2)	Pr1—O2W—H3W	122.7
N1—C1—H1	118.3	Pr1—O2W—H4W	131.7
C2—C1—H1	118.3	H3W—O2W—H4W	105.6
C3—C4—C5	118 (3)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1W···O2^vi	0.88	1.79	2.67 (2)	179
O1W—H2W···O4ⁱⁱⁱ	0.97	1.68	2.63 (2)	163
O2W—H3W···O2^vii	1.00	1.77	2.77 (2)	176
O2W—H4W···O2^viii	0.83	1.95	2.76 (2)	162
O3W—H5W···O1W^ix	0.82	2.15	2.91 (2)	157

Symmetry codes: (iii) x, −y+1, −z+1; (vi) −x+1/2, y, −z+1/2; (vii) −x+1/2, y+1/2, z; (viii) x, −y+2, −z+1; (ix) x, y−1/2, −z+1/2.

Experimental details

Crystal data
Chemical formula	[Ag₂Pr(C₆H₄NO₂)₄(H₂O)₄]ClO₄·H₂O
M_r	1034.59
Crystal system, space group	Orthorhombic, Cmca
Temperature (K)	273
a, b, c (Å)	35.396 (3), 12.3733 (10), 15.2324 (13)
V (Å³)	6671.2 (10)
Z	8
Radiation type	Mo Kα
µ (mm⁻¹)	2.76
Crystal size (mm)	0.30 × 0.25 × 0.22

Data collection
Diffractometer	Bruker APEXII CCD diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.453, 0.552
No. of measured, independent and observed [I > 2σ(I)] reflections	16336, 3065, 2478
R_int	0.049
(sin θ/λ)_max (Å⁻¹)	0.599

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.036, 0.097, 1.06
No. of reflections	3065
No. of parameters	227
No. of restraints	27
H-atom treatment	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.0479P)² + 31.5675P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	1.56, −0.87

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

Pr1—O3ⁱ	2.390 (14)	Ag1—N1	2.175 (18)
Pr1—O1W	2.477 (14)	Ag1—O4ⁱⁱ	2.777 (16)
Pr1—O2W	2.495 (14)	Ag1—O5	2.81 (3)
Pr1—O1	2.504 (13)	Ag1—O3W	2.90 (2)
Ag1—N2	2.165 (18)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1W···O2ⁱⁱⁱ	0.88	1.79	2.67 (2)	179
O1W—H2W···O4^iv	0.97	1.68	2.63 (2)	163
O2W—H3W···O2^v	1.00	1.77	2.77 (2)	176
O2W—H4W···O2^vi	0.83	1.95	2.76 (2)	162
O3W—H5W···O1W^vii	0.82	2.15	2.91 (2)	157

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

Acknowledgements

The authors acknowledge Guangdong Ocean University for supporting this work.

References

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