Poly[penta­aqua­tetra­kis(μ2-nicotinato-κ2N:O)(perchlorato-κO)lanthanum(III)disilver(I)]

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

doi:10.1107/S1600536809026130

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 8| August 2009| Pages m896-m897

doi:10.1107/S1600536809026130

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Poly[pentaaquatetrakis(μ₂-nicotinato-κ²N:O)(perchlorato-κO)lanthanum(III)disilver(I)]

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

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

(Received 13 May 2009; accepted 5 July 2009; online 11 July 2009)

In the title complex, [Ag₂La(C₆H₄NO₂)₄(ClO₄)(H₂O)₅]_n, the La^III atom, lying on a twofold rotation axis, is eight-coordinated by four O atoms from four nicotinate (nic) ligands and four water molecules in a distorted square-antiprismatic coordination geometry. The Ag^I atom is coordinated in an almost linear fashion by two pyridyl N atoms of two nic ligands. The linear coordination is augmented by weak interactions with one O atom from a half-occupied ClO₄⁻ anion and a water molecule lying on a twofold axis. Two Ag(nic)₂ units connect two La atoms, forming a cyclic unit. These units are further extended into an infinite zigzag chain. The chains are bridged by the disordered perchlorate ions via weak Ag—O [2.678 (2) Å] interactions. O—H⋯O hydrogen bonds, weak Ag⋯Ag [3.3340 (15) Å] interactions and π–π interactions between the pyridyl rings [centroid–centroid distance = 3.656 (2) Å] lead to a three-dimensional network.

Related literature

For related structures see: Evans & Lin (2001 ); Luo et al. (2004 ).

Experimental

Crystal data

[Ag₂La(C₆H₄NO₂)₄(ClO₄)(H₂O)₅]
M_r = 1032.59
Orthorhombic, C m c a
a = 35.140 (5) Å
b = 12.3371 (16) Å
c = 15.046 (2) Å
V = 6522.8 (15) Å³
Z = 8
Mo Kα radiation
μ = 2.64 mm⁻¹
T = 298 K
0.30 × 0.25 × 0.22 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.465, T_max = 0.567
15911 measured reflections
2999 independent reflections
2251 reflections with I > 2σ(I)
R_int = 0.067

Refinement

R[F² > 2σ(F²)] = 0.049
wR(F²) = 0.090
S = 1.95
2999 reflections
212 parameters
48 restraints
H-atom parameters constrained
Δρ_max = 1.90 e Å⁻³
Δρ_min = −0.97 e Å⁻³

Table 1
Selected bond lengths (Å)

La1—O1	2.511 (5)
La1—O3ⁱ	2.401 (4)
La1—O1W	2.498 (5)
La1—O2W	2.494 (4)
Ag1—N1	2.175 (6)
Ag1—N2	2.161 (6)
Ag1—O6	2.681 (2)
Ag1—O3W	2.877 (6)
Ag1—Ag1ⁱⁱ	3.3352 (14)
Symmetry codes: (i) $[x, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (ii) x, -y+1, -z+1.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1W⋯O2ⁱⁱⁱ	0.86	1.85	2.667 (6)	159
O1W—H2W⋯O4ⁱⁱ	0.84	1.80	2.611 (7)	161
O2W—H3W⋯O2^iv	0.84	1.92	2.738 (7)	165
O2W—H4W⋯O2^v	0.84	1.89	2.693 (7)	161
O3W—H5W⋯O1W^vi	0.82	2.11	2.883 (5)	157
Symmetry codes: (ii) x, -y+1, -z+1; (iii) $[-x+{\script{1\over 2}}, y, -z+{\script{1\over 2}}]$ ; (iv) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, z]$ ; (v) x, -y+2, -z+1; (vi) $[x, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ .

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) and DIAMOND (Brandenburg, 1999 ); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809026130/hy2200sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809026130/hy2200Isup2.hkl

checkCIF report

Comment top

In the structural investigation of nictinate complexes, it has been found that nictinate functions as a multidentate ligand with versatile binding and coordination modes (Evans & Lin, 2001; Luo et al., 2004). In this paper, we report the crystal structure of the title compound, a new La^III complex, resulted from the hydrothermal treatment of La₂O₃, AgNO₃, perchloric acid and nicotinic acid in water.

As depicted in Fig. 1, the La^III atom, lying on a twofold rotation axis, is surrounded by four O atoms from four nic ligands and four water molecules in a distorted square-antiprismatic coordination geometry. The Ag^I atom is coordinated in an almost linear fashion by two pyridyl N atoms of two nic ligands. The linear coordination is augmented by weak interactions with one O atom from a half-occupied ClO₄^- anion and a water molecule lying on a twofold rotation axis. The two pyridyl rings of the nic ligands coordinating to the Ag atom are alomost coplanar and have a dihedral angle of 1.74 (2)°. Two Ag(nic)₂ units connect two La atoms, forming a cyclic unit. These cycles are further extended into an infinite zigzag chain. The chains are bridged by disordered perchlorate ions via the weak Ag—O [2.678 (2) Å] interactions into a two-dimensional wavelike layer in the b axis direction (Fig. 2). Finally, the layers are further self-assembled into a three-dimensional supramolecular network (Fig. 3) via O—H···O hydrogen bonds involving the coordinated water molecules and carboxylate O atoms from the nic ligands (Table 1), weak Ag···Ag [3.3340 (15) Å] interactions and π–π stacking interactions between the pyridyl rings [centroid–centroid distance = 3.656 (2) Å].

Related literature top

For related structures see: Evans & Lin (2001); Luo et al. (2004).

Experimental top

A mixture of La₂O₃ (0.162 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 crystals obtained were washed with water and dried in air (yield 46% based on La).

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) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. The asymetric unit of the title compound. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry codes: (i) 1/2 - x, y, 1/2 - z; (ii) x, 1 - y, 1 - z; (iii) x, 3/2 - y, -1/2 + z; (iv) 1/2 - x, 3/2 - y, 1 - z.]
	Fig. 2. View of the two-dimensional wavelike layer of the title compound. Dashed lines denote weak Ag···O interactions.
	Fig. 3. View of the three-dimensional network via hydrogen bonds, weak Ag···O, Ag···Ag, and π–π interactions (dashed lines).

Poly[pentaaquatetrakis(µ₂-nicotinato-κ²N:O)(perchlorato- κO)lanthanum(III)disilver(I)] top

Crystal data top

[Ag₂La(C₆H₄NO₂)₄(ClO₄)(H₂O)₅]	F(000) = 4016
M_r = 1032.59	D_x = 2.103 Mg m⁻³
Orthorhombic, Cmca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2bc 2	Cell parameters from 3600 reflections
a = 35.140 (5) Å	θ = 1.4–28°
b = 12.3371 (16) Å	µ = 2.64 mm⁻¹
c = 15.046 (2) Å	T = 298 K
V = 6522.8 (15) Å³	Block, colorless
Z = 8	0.30 × 0.25 × 0.22 mm

Data collection top

Bruker APEXII CCD diffractometer	2999 independent reflections
Radiation source: fine-focus sealed tube	2251 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.067
ϕ and ω scans	θ_max = 25.2°, θ_min = 2.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −42→41
T_min = 0.465, T_max = 0.567	k = −14→11
15911 measured reflections	l = −18→15

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)] = 0.049	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.090	H-atom parameters constrained
S = 1.95	w = 1/[σ²(F_o²)] where P = (F_o² + 2F_c²)/3
2999 reflections	(Δ/σ)_max = 0.008
212 parameters	Δρ_max = 1.90 e Å⁻³
48 restraints	Δρ_min = −0.97 e Å⁻³

Crystal data top

[Ag₂La(C₆H₄NO₂)₄(ClO₄)(H₂O)₅]	V = 6522.8 (15) Å³
M_r = 1032.59	Z = 8
Orthorhombic, Cmca	Mo Kα radiation
a = 35.140 (5) Å	µ = 2.64 mm⁻¹
b = 12.3371 (16) Å	T = 298 K
c = 15.046 (2) Å	0.30 × 0.25 × 0.22 mm

Data collection top

Bruker APEXII CCD diffractometer	2999 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	2251 reflections with I > 2σ(I)
T_min = 0.465, T_max = 0.567	R_int = 0.067
15911 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.049	48 restraints
wR(F²) = 0.090	H-atom parameters constrained
S = 1.95	Δρ_max = 1.90 e Å⁻³
2999 reflections	Δρ_min = −0.97 e Å⁻³
212 parameters

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
La1	0.2500	1.08273 (5)	0.2500	0.02358 (16)
Ag1	0.389767 (18)	0.60965 (6)	0.56481 (4)	0.0465 (2)
C1	0.3039 (2)	0.9196 (6)	0.3991 (4)	0.0299 (18)
C2	0.34312 (19)	0.8866 (6)	0.4214 (5)	0.0318 (18)
C3	0.3495 (2)	0.7964 (6)	0.4729 (4)	0.0331 (19)
H3	0.3287	0.7591	0.4956	0.040*
C4	0.4138 (2)	0.8140 (8)	0.4627 (5)	0.053 (3)
H4	0.4380	0.7896	0.4770	0.064*
C5	0.4097 (2)	0.9060 (8)	0.4114 (7)	0.071 (3)
H5	0.4311	0.9430	0.3913	0.085*
C6	0.3744 (2)	0.9422 (7)	0.3905 (5)	0.048 (2)
H6	0.3714	1.0039	0.3557	0.057*
C7	0.4322 (2)	0.4349 (7)	0.6693 (6)	0.054 (3)
H7	0.4534	0.4729	0.6489	0.065*
C8	0.3685 (2)	0.4135 (6)	0.6768 (5)	0.0313 (18)
H8	0.3444	0.4376	0.6605	0.038*
C9	0.37074 (19)	0.3248 (6)	0.7314 (4)	0.0288 (18)
C10	0.4064 (2)	0.2925 (7)	0.7546 (6)	0.060 (3)
H10	0.4098	0.2331	0.7919	0.072*
C11	0.4374 (2)	0.3480 (8)	0.7226 (7)	0.078 (4)
H11	0.4619	0.3257	0.7375	0.094*
C12	0.3359 (2)	0.2677 (6)	0.7620 (5)	0.0292 (17)
N1	0.38410 (17)	0.7606 (5)	0.4913 (4)	0.0369 (16)
N2	0.39810 (17)	0.4670 (5)	0.6458 (4)	0.0375 (16)
O1	0.30034 (13)	0.9960 (4)	0.3448 (3)	0.0366 (13)
O2	0.27688 (13)	0.8707 (4)	0.4351 (3)	0.0331 (13)
O3	0.30462 (12)	0.3020 (4)	0.7338 (3)	0.0328 (12)
O4	0.33989 (13)	0.1890 (5)	0.8112 (3)	0.0432 (15)
O1W	0.28251 (13)	0.9406 (4)	0.1593 (3)	0.0373 (14)
H1W	0.2679	0.9115	0.1204	0.056*
H2W	0.2983	0.8959	0.1795	0.056*
O2W	0.24825 (13)	1.1647 (4)	0.4015 (3)	0.0478 (14)
H3W	0.2385	1.2269	0.4029	0.072*
H4W	0.2620	1.1535	0.4461	0.072*
O3W	0.32305 (14)	0.5000	0.5000	0.074 (3)
H5W	0.3086	0.5297	0.5356	0.111*
Cl1	0.5030 (4)	0.6862 (4)	0.5923 (4)	0.0816 (15)	0.50
O5	0.5071 (4)	0.8007 (6)	0.5862 (9)	0.118 (3)	0.50
O6	0.4640 (3)	0.6544 (14)	0.5835 (10)	0.118 (3)	0.50
O7	0.5133 (4)	0.6545 (12)	0.6849 (7)	0.118 (3)	0.50
O8	0.5275 (4)	0.6292 (12)	0.5351 (9)	0.118 (3)	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
La1	0.0267 (3)	0.0230 (3)	0.0210 (3)	0.000	−0.0014 (3)	0.000
Ag1	0.0542 (4)	0.0386 (4)	0.0466 (4)	0.0050 (4)	−0.0029 (3)	0.0150 (3)
C1	0.043 (4)	0.027 (5)	0.020 (4)	0.006 (4)	−0.007 (4)	−0.007 (3)
C2	0.034 (4)	0.032 (5)	0.028 (4)	−0.004 (4)	−0.004 (4)	−0.004 (4)
C3	0.032 (4)	0.036 (5)	0.030 (4)	0.005 (4)	0.000 (4)	0.010 (4)
C4	0.038 (5)	0.061 (8)	0.060 (6)	−0.003 (5)	−0.004 (4)	0.024 (5)
C5	0.033 (5)	0.075 (9)	0.105 (9)	−0.004 (5)	−0.001 (5)	0.049 (7)
C6	0.044 (5)	0.052 (7)	0.047 (5)	−0.006 (4)	−0.011 (4)	0.029 (4)
C7	0.033 (5)	0.051 (7)	0.078 (7)	−0.004 (4)	−0.002 (5)	0.026 (5)
C8	0.029 (4)	0.037 (5)	0.028 (4)	0.002 (4)	−0.001 (3)	−0.004 (4)
C9	0.033 (4)	0.028 (5)	0.025 (5)	0.003 (4)	−0.006 (3)	−0.001 (4)
C10	0.039 (5)	0.055 (6)	0.087 (7)	−0.002 (4)	−0.007 (5)	0.040 (6)
C11	0.027 (5)	0.069 (8)	0.139 (10)	−0.003 (5)	−0.007 (5)	0.059 (7)
C12	0.035 (4)	0.025 (5)	0.027 (5)	−0.003 (3)	0.004 (4)	−0.010 (4)
N1	0.037 (4)	0.037 (5)	0.037 (4)	0.002 (4)	−0.004 (3)	0.011 (3)
N2	0.040 (4)	0.033 (4)	0.040 (4)	0.004 (3)	0.004 (3)	0.008 (3)
O1	0.041 (3)	0.031 (4)	0.038 (3)	0.006 (2)	−0.005 (3)	0.013 (3)
O2	0.037 (3)	0.036 (4)	0.027 (3)	−0.002 (2)	0.001 (2)	0.005 (2)
O3	0.027 (3)	0.033 (3)	0.038 (3)	0.007 (2)	−0.004 (2)	−0.002 (2)
O4	0.037 (3)	0.038 (4)	0.054 (4)	−0.004 (3)	−0.007 (3)	0.021 (3)
O1W	0.039 (3)	0.034 (4)	0.039 (3)	0.007 (2)	−0.010 (2)	−0.009 (2)
O2W	0.073 (3)	0.046 (4)	0.025 (3)	0.026 (3)	−0.017 (3)	−0.009 (2)
O3W	0.050 (5)	0.123 (10)	0.048 (6)	0.000	0.000	−0.011 (5)
Cl1	0.044 (3)	0.069 (3)	0.132 (4)	0.015 (5)	0.044 (5)	0.014 (3)
O5	0.075 (5)	0.108 (7)	0.172 (8)	0.003 (5)	0.005 (5)	0.035 (6)
O6	0.075 (5)	0.108 (7)	0.172 (8)	0.003 (5)	0.005 (5)	0.035 (6)
O7	0.075 (5)	0.108 (7)	0.172 (8)	0.003 (5)	0.005 (5)	0.035 (6)
O8	0.075 (5)	0.108 (7)	0.172 (8)	0.003 (5)	0.005 (5)	0.035 (6)

Geometric parameters (Å, º) top

La1—O1	2.511 (5)	C7—C11	1.352 (11)
La1—O3ⁱ	2.401 (4)	C7—H7	0.9300
La1—O1W	2.498 (5)	C8—N2	1.317 (8)
La1—O2W	2.494 (4)	C8—C9	1.371 (10)
Ag1—N1	2.175 (6)	C8—H8	0.9300
Ag1—N2	2.161 (6)	C9—C10	1.360 (9)
Ag1—O6	2.681 (2)	C9—C12	1.484 (10)
Ag1—O3W	2.877 (6)	C10—C11	1.375 (11)
Ag1—Ag1ⁱⁱ	3.3352 (14)	C10—H10	0.9300
C1—O1	1.254 (8)	C11—H11	0.9300
C1—O2	1.249 (8)	C12—O4	1.230 (8)
C1—C2	1.475 (9)	C12—O3	1.253 (8)
C2—C6	1.378 (10)	O3—La1ⁱⁱⁱ	2.401 (4)
C2—C3	1.373 (10)	O1W—H1W	0.8564
C3—N1	1.324 (8)	O1W—H2W	0.8388
C3—H3	0.9300	O2W—H3W	0.8404
C4—N1	1.306 (9)	O2W—H4W	0.8395
C4—C5	1.379 (11)	O3W—H5W	0.8241
C4—H4	0.9300	Cl1—O8	1.4076
C5—C6	1.354 (10)	Cl1—O5	1.4226
C5—H5	0.9300	Cl1—O6	1.4309
C6—H6	0.9300	Cl1—O7	1.4925
C7—N2	1.312 (9)

O3ⁱⁱⁱ—La1—O3ⁱ	107.4 (2)	N1—C4—H4	119.5
O3ⁱⁱⁱ—La1—O2W^iv	82.65 (16)	C5—C4—H4	119.5
O3ⁱ—La1—O2W^iv	69.35 (15)	C4—C5—C6	119.8 (8)
O3ⁱⁱⁱ—La1—O2W	69.35 (15)	C4—C5—H5	120.1
O3ⁱ—La1—O2W	82.65 (16)	C6—C5—H5	120.1
O2W^iv—La1—O2W	132.1 (2)	C2—C6—C5	119.2 (8)
O3ⁱⁱⁱ—La1—O1W	146.78 (15)	C2—C6—H6	120.4
O3ⁱ—La1—O1W	89.71 (15)	C5—C6—H6	120.4
O2W^iv—La1—O1W	76.96 (16)	N2—C7—C11	121.5 (8)
O2W—La1—O1W	142.66 (15)	N2—C7—H7	119.2
O3ⁱⁱⁱ—La1—O1W^iv	89.71 (15)	C11—C7—H7	119.2
O3ⁱ—La1—O1W^iv	146.78 (15)	N2—C8—C9	124.5 (7)
O2W^iv—La1—O1W^iv	142.66 (15)	N2—C8—H8	117.8
O2W—La1—O1W^iv	76.96 (16)	C9—C8—H8	117.8
O1W—La1—O1W^iv	90.8 (2)	C10—C9—C8	116.2 (7)
O3ⁱⁱⁱ—La1—O1^iv	75.34 (16)	C10—C9—C12	122.7 (7)
O3ⁱ—La1—O1^iv	139.26 (15)	C8—C9—C12	121.1 (6)
O2W^iv—La1—O1^iv	70.81 (16)	C9—C10—C11	119.7 (8)
O2W—La1—O1^iv	132.40 (16)	C9—C10—H10	120.2
O1W—La1—O1^iv	73.32 (16)	C11—C10—H10	120.2
O1W^iv—La1—O1^iv	71.89 (16)	C7—C11—C10	119.7 (8)
O3ⁱⁱⁱ—La1—O1	139.26 (15)	C7—C11—H11	120.1
O3ⁱ—La1—O1	75.34 (16)	C10—C11—H11	120.1
O2W^iv—La1—O1	132.40 (16)	O4—C12—O3	124.7 (7)
O2W—La1—O1	70.81 (16)	O4—C12—C9	117.9 (7)
O1W—La1—O1	71.89 (16)	O3—C12—C9	117.4 (7)
O1W^iv—La1—O1	73.32 (16)	C4—N1—C3	119.7 (7)
O1^iv—La1—O1	129.6 (2)	C4—N1—Ag1	121.8 (5)
N2—Ag1—N1	175.3 (2)	C3—N1—Ag1	118.5 (5)
N2—Ag1—Ag1ⁱⁱ	70.66 (16)	C7—N2—C8	118.4 (7)
N1—Ag1—Ag1ⁱⁱ	113.42 (17)	C7—N2—Ag1	121.4 (5)
O6—Ag1—N2	88.67 (6)	C8—N2—Ag1	120.0 (5)
O6—Ag1—N1	88.06 (7)	C1—O1—La1	139.5 (5)
O3W—Ag1—N1	98.95 (17)	C12—O3—La1ⁱⁱⁱ	150.2 (5)
O3W—Ag1—N2	85.33 (16)	La1—O1W—H1W	113.1
O3W—Ag1—O6	157.70 (7)	La1—O1W—H2W	124.4
O1—C1—O2	124.7 (7)	H1W—O1W—H2W	111.6
O1—C1—C2	116.7 (7)	La1—O2W—H3W	113.8
O2—C1—C2	118.6 (7)	La1—O2W—H4W	130.5
C6—C2—C3	117.6 (7)	H3W—O2W—H4W	111.4
C6—C2—C1	122.1 (7)	O8—Cl1—O5	113.3
C3—C2—C1	120.3 (7)	O8—Cl1—O6	113.1
N1—C3—C2	122.5 (7)	O5—Cl1—O6	111.3
N1—C3—H3	118.7	O8—Cl1—O7	106.8
C2—C3—H3	118.7	O5—Cl1—O7	107.2
N1—C4—C5	121.1 (8)	O6—Cl1—O7	104.5

Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) x, −y+1, −z+1; (iii) −x+1/2, −y+3/2, −z+1; (iv) −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^iv	0.86	1.85	2.667 (6)	159
O1W—H2W···O4ⁱⁱ	0.84	1.80	2.611 (7)	161
O2W—H3W···O2^v	0.84	1.92	2.738 (7)	165
O2W—H4W···O2^vi	0.84	1.89	2.693 (7)	161
O3W—H5W···O1W^vii	0.82	2.11	2.883 (5)	157

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

Experimental details

Crystal data
Chemical formula	[Ag₂La(C₆H₄NO₂)₄(ClO₄)(H₂O)₅]
M_r	1032.59
Crystal system, space group	Orthorhombic, Cmca
Temperature (K)	298
a, b, c (Å)	35.140 (5), 12.3371 (16), 15.046 (2)
V (Å³)	6522.8 (15)
Z	8
Radiation type	Mo Kα
µ (mm⁻¹)	2.64
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	0.465, 0.567
No. of measured, independent and observed [I > 2σ(I)] reflections	15911, 2999, 2251
R_int	0.067
(sin θ/λ)_max (Å⁻¹)	0.599

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.049, 0.090, 1.95
No. of reflections	2999
No. of parameters	212
No. of restraints	48
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.90, −0.97

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

La1—O1	2.511 (5)	Ag1—N2	2.161 (6)
La1—O3ⁱ	2.401 (4)	Ag1—O6	2.681 (2)
La1—O1W	2.498 (5)	Ag1—O3W	2.877 (6)
La1—O2W	2.494 (4)	Ag1—Ag1ⁱⁱ	3.3352 (14)
Ag1—N1	2.175 (6)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1W···O2ⁱⁱⁱ	0.86	1.85	2.667 (6)	159
O1W—H2W···O4ⁱⁱ	0.84	1.80	2.611 (7)	161
O2W—H3W···O2^iv	0.84	1.92	2.738 (7)	165
O2W—H4W···O2^v	0.84	1.89	2.693 (7)	161
O3W—H5W···O1W^vi	0.82	2.11	2.883 (5)	157

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

Acknowledgements

The authors acknowledge Guang Dong Ocean University for support of this work.

References

Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
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