Literature DB >> 21583314

Poly[[hemi-μ(4)-oxalato-hemi-μ(2)-oxalato-bis-(μ(3)-pyrazine-2-carboxyl-ato)erbium(III)silver(I)] monohydrate].

Ling-Zhi Zhao, Rui-Xia He, Qiu-Gui Zhong, Rong-Hua Zeng, Dong-Sheng Lu.

Abstract

The asymmetric unit of the title complex, {[AgEr(C(5)H(3)N(2)O(2))(2)(C(2)O(4))]·H(2)O}(n), contains one Er(III) atom, one Ag(I) atom, two n class="Chemical">pyrazine-2-carboxyl-ate (pyc) ligands, two half oxalate ligands (each lying on an inversion center) and one uncoordinated water mol-ecule. The Er(III) atom is coordinated by two O atoms and two N atoms from two pyc ligands, one O atom from a third pyc ligand and four O atoms from two oxalate ligands in a distorted monocapped square-anti-prismatic geometry. The Ag(I) atom is coordinated by two N atoms from two pyc ligands, one O atom from a third pyc ligand and one O atom from one oxalate ligand. The crystal structure exhibits a three-dimensional heterometallic polymeric network. O-H⋯O hydrogen bonding between the uncoordinated water mol-ecule and carboxyl-ate O atoms is observed.

Entities: Chemical Disease Species

Year: 2009 PMID： 21583314 PMCID： PMC2977120 DOI： 10.1107/S1600536809029742

Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN： 1600-5368

Related literature

For general background to lanthanide–transition heterometallic complexes, see: Deng et al. (2008 ▶); Wang et al. (2006 ▶); Zhou et al. (2006 ▶).

Experimental

Crystal data

[AgEr(C5H3N2O2)2(C2O4)]·H2O M = 627.35 Monoclinic, a = 10.0482 (6) Å b = 18.3968 (11) Å c = 8.0371 (5) Å β = 95.397 (1)° V = 1479.11 (16) Å3 Z = 4 Mo Kα radiation μ = 7.02 mm−1 T = 296 K 0.22 × 0.20 × 0.19 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.307, T max = 0.349 (expected range = 0.232–0.263) 7533 measured reflections 2649 independent reflections 2450 reflections with I > 2σ(I) R int = 0.019

Refinement

R[F 2 > 2σ(F 2)] = 0.021 wR(F 2) = 0.050 S = 1.04 2649 reflections 244 parameters 12 restraints H-atom parameters constrained Δρmax = 1.43 e Å−3 Δρmin = −1.14 e Å−3 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 Mercury (Macrae et al., 2006 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809029742/hy2207sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809029742/hy2207Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[AgEr(C₅H₃N₂O₂)₂(C₂O₄)]·H₂O	F(000) = 1180
M_r = 627.35	D_x = 2.817 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 5128 reflections
a = 10.0482 (6) Å	θ = 2.2–28.2°
b = 18.3968 (11) Å	µ = 7.02 mm⁻¹
c = 8.0371 (5) Å	T = 296 K
β = 95.397 (1)°	Block, colorless
V = 1479.11 (16) Å³	0.22 × 0.20 × 0.19 mm
Z = 4

Bruker APEXII CCD diffractometer	2649 independent reflections
Radiation source: fine-focus sealed tube	2450 reflections with I > 2σ(I)
graphite	R_int = 0.019
φ and ω scans	θ_max = 25.2°, θ_min = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −11→12
T_min = 0.307, T_max = 0.349	k = −22→19
7533 measured reflections	l = −9→5

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)] = 0.021	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.050	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.024P)² + 4.153P] where P = (F_o² + 2F_c²)/3
2649 reflections	(Δ/σ)_max = 0.001
244 parameters	Δρ_max = 1.43 e Å⁻³
12 restraints	Δρ_min = −1.14 e Å⁻³

	x	y	z	U_iso*/U_eq
Er1	0.364162 (17)	0.105359 (10)	0.24162 (2)	0.01442 (7)
Ag1	0.85087 (4)	0.42746 (2)	0.39306 (4)	0.03045 (11)
O1	0.2989 (3)	0.21768 (16)	0.3579 (4)	0.0242 (7)
O2	0.3493 (3)	0.32200 (16)	0.4921 (4)	0.0235 (7)
O3	−0.0813 (3)	0.0887 (2)	0.1736 (4)	0.0317 (8)
O4	0.1381 (3)	0.09487 (18)	0.1482 (4)	0.0250 (7)
O5	0.3318 (3)	0.01811 (16)	0.0110 (4)	0.0207 (6)
O7	0.5023 (3)	0.09455 (15)	0.4957 (4)	0.0199 (6)
N1	0.5506 (3)	0.20455 (19)	0.2760 (4)	0.0190 (8)
N2	0.7204 (4)	0.3245 (2)	0.3075 (5)	0.0289 (9)
N3	0.1969 (4)	0.09160 (19)	0.4735 (4)	0.0194 (8)
N4	−0.0028 (4)	0.0827 (2)	0.6909 (4)	0.0239 (8)
C1	0.3752 (4)	0.2695 (2)	0.4013 (5)	0.0193 (9)
C2	0.5118 (4)	0.2678 (2)	0.3374 (5)	0.0195 (9)
C3	0.5950 (4)	0.3270 (3)	0.3465 (6)	0.0259 (10)
H3	0.5621	0.3711	0.3818	0.031*
C4	0.7614 (5)	0.2604 (3)	0.2544 (6)	0.0287 (11)
H4	0.8491	0.2554	0.2282	0.034*
C5	0.6765 (4)	0.2009 (3)	0.2372 (6)	0.0255 (10)
H5	0.7082	0.1573	0.1976	0.031*
C6	0.0371 (4)	0.0914 (2)	0.2309 (5)	0.0185 (9)
C7	0.0668 (4)	0.0902 (2)	0.4181 (5)	0.0183 (9)
C8	−0.0327 (4)	0.0862 (3)	0.5258 (5)	0.0223 (10)
H8	−0.1219	0.0860	0.4824	0.027*
C9	0.1265 (4)	0.0855 (3)	0.7468 (5)	0.0267 (10)
H9	0.1508	0.0845	0.8614	0.032*
C10	0.2255 (4)	0.0900 (3)	0.6381 (6)	0.0269 (10)
H10	0.3145	0.0920	0.6818	0.032*
C11	0.4313 (4)	−0.0108 (2)	−0.0429 (5)	0.0164 (9)
C12	0.5388 (4)	0.0323 (2)	0.5434 (5)	0.0176 (9)
O1W	0.0424 (5)	0.2589 (3)	0.4885 (8)	0.0827 (16)
H1W	0.1096	0.2521	0.4314	0.124*
H2W	0.0662	0.2368	0.5816	0.124*
O6	0.4323 (3)	−0.05626 (16)	−0.1587 (4)	0.0212 (7)
O8	0.6284 (3)	0.01649 (16)	0.6555 (4)	0.0226 (7)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Er1	0.01594 (11)	0.01469 (11)	0.01268 (11)	0.00069 (7)	0.00162 (7)	−0.00034 (7)
Ag1	0.0286 (2)	0.0423 (2)	0.02146 (19)	−0.00868 (16)	0.00783 (14)	−0.00439 (16)
O1	0.0201 (15)	0.0210 (16)	0.0326 (18)	−0.0023 (13)	0.0074 (13)	−0.0060 (14)
O2	0.0281 (17)	0.0210 (16)	0.0212 (16)	0.0042 (13)	0.0014 (13)	−0.0076 (13)
O3	0.0201 (16)	0.059 (2)	0.0152 (16)	0.0027 (15)	−0.0017 (13)	−0.0041 (15)
O4	0.0199 (16)	0.042 (2)	0.0140 (15)	−0.0004 (13)	0.0046 (12)	0.0007 (14)
O5	0.0205 (15)	0.0238 (17)	0.0176 (15)	0.0042 (13)	0.0006 (12)	−0.0029 (13)
O7	0.0255 (16)	0.0166 (15)	0.0169 (15)	0.0009 (12)	−0.0013 (12)	0.0016 (12)
N1	0.0229 (19)	0.0172 (18)	0.0170 (18)	0.0012 (14)	0.0025 (14)	−0.0010 (15)
N2	0.027 (2)	0.028 (2)	0.032 (2)	−0.0040 (17)	0.0074 (17)	−0.0054 (18)
N3	0.0221 (19)	0.0197 (19)	0.0165 (19)	−0.0003 (15)	0.0029 (14)	0.0004 (15)
N4	0.025 (2)	0.032 (2)	0.0160 (19)	0.0015 (16)	0.0052 (15)	0.0012 (16)
C1	0.025 (2)	0.019 (2)	0.013 (2)	0.0028 (18)	0.0001 (17)	0.0025 (18)
C2	0.025 (2)	0.018 (2)	0.015 (2)	0.0029 (17)	0.0000 (17)	0.0000 (17)
C3	0.027 (2)	0.020 (2)	0.031 (3)	−0.0018 (19)	0.0060 (19)	−0.008 (2)
C4	0.020 (2)	0.031 (3)	0.035 (3)	−0.0030 (19)	0.006 (2)	−0.004 (2)
C5	0.022 (2)	0.026 (2)	0.028 (2)	0.0039 (19)	0.0025 (19)	−0.006 (2)
C6	0.021 (2)	0.018 (2)	0.016 (2)	0.0029 (17)	0.0032 (17)	0.0011 (17)
C7	0.020 (2)	0.018 (2)	0.017 (2)	−0.0001 (17)	0.0016 (17)	0.0000 (17)
C8	0.019 (2)	0.032 (3)	0.016 (2)	0.0006 (19)	0.0033 (17)	0.0000 (19)
C9	0.028 (3)	0.039 (3)	0.013 (2)	0.006 (2)	0.0032 (18)	0.004 (2)
C10	0.019 (2)	0.044 (3)	0.018 (2)	0.001 (2)	0.0023 (18)	0.000 (2)
C11	0.023 (2)	0.013 (2)	0.013 (2)	0.0026 (16)	0.0016 (17)	0.0050 (17)
C12	0.019 (2)	0.021 (2)	0.013 (2)	0.0000 (17)	0.0041 (16)	0.0021 (17)
O1W	0.053 (3)	0.067 (3)	0.130 (5)	−0.008 (2)	0.013 (3)	−0.020 (3)
O6	0.0200 (15)	0.0215 (16)	0.0224 (16)	−0.0006 (12)	0.0033 (12)	−0.0073 (13)
O8	0.0237 (16)	0.0220 (16)	0.0209 (16)	−0.0013 (13)	−0.0038 (13)	0.0024 (13)

Er1—O4	2.333 (3)	N3—C10	1.328 (6)
Er1—O7	2.367 (3)	N3—C7	1.341 (5)
Er1—O1	2.385 (3)	N4—C8	1.335 (5)
Er1—O6ⁱ	2.387 (3)	N4—C9	1.336 (6)
Er1—O8ⁱⁱ	2.388 (3)	C1—C2	1.510 (6)
Er1—O2ⁱⁱⁱ	2.403 (3)	C2—C3	1.370 (6)
Er1—O5	2.451 (3)	C3—H3	0.9300
Er1—N1	2.611 (4)	C4—C5	1.387 (7)
Er1—N3	2.636 (4)	C4—H4	0.9300
Ag1—N4^iv	2.299 (4)	C5—H5	0.9300
Ag1—O3^v	2.312 (3)	C6—C7	1.506 (6)
Ag1—N2	2.368 (4)	C7—C8	1.385 (6)
Ag1—O5^vi	2.648 (4)	C8—H8	0.9300
O1—C1	1.253 (5)	C9—C10	1.387 (6)
O2—C1	1.252 (5)	C9—H9	0.9300
O3—C6	1.236 (5)	C10—H10	0.9300
O4—C6	1.265 (5)	C11—O6	1.252 (5)
O5—C11	1.245 (5)	C11—C11ⁱ	1.537 (8)
O7—C12	1.252 (5)	C12—O8	1.247 (5)
N1—C5	1.332 (6)	C12—C12ⁱⁱ	1.549 (8)
N1—C2	1.337 (5)	O1W—H1W	0.86
N2—C3	1.328 (6)	O1W—H2W	0.86
N2—C4	1.332 (6)

O4—Er1—O7	138.16 (10)	C3—N2—C4	115.8 (4)
O4—Er1—O1	84.40 (11)	C3—N2—Ag1	114.5 (3)
O7—Er1—O1	83.98 (10)	C4—N2—Ag1	128.4 (3)
O4—Er1—O6ⁱ	135.46 (10)	C10—N3—C7	116.3 (4)
O7—Er1—O6ⁱ	76.17 (10)	C10—N3—Er1	127.9 (3)
O1—Er1—O6ⁱ	135.36 (10)	C7—N3—Er1	115.7 (3)
O4—Er1—O8ⁱⁱ	91.81 (11)	C8—N4—C9	117.0 (4)
O7—Er1—O8ⁱⁱ	68.02 (10)	C8—N4—Ag1^ix	127.4 (3)
O1—Er1—O8ⁱⁱ	132.72 (11)	C9—N4—Ag1^ix	115.6 (3)
O6ⁱ—Er1—O8ⁱⁱ	75.03 (10)	O2—C1—O1	126.4 (4)
O4—Er1—O2ⁱⁱⁱ	78.18 (10)	O2—C1—C2	117.4 (4)
O7—Er1—O2ⁱⁱⁱ	138.78 (10)	O1—C1—C2	116.2 (4)
O1—Er1—O2ⁱⁱⁱ	81.23 (11)	N1—C2—C3	120.9 (4)
O6ⁱ—Er1—O2ⁱⁱⁱ	87.99 (10)	N1—C2—C1	116.7 (4)
O8ⁱⁱ—Er1—O2ⁱⁱⁱ	143.95 (10)	C3—C2—C1	122.3 (4)
O4—Er1—O5	69.30 (10)	N2—C3—C2	123.2 (4)
O7—Er1—O5	128.53 (10)	N2—C3—H3	118.4
O1—Er1—O5	147.36 (10)	C2—C3—H3	118.4
O6ⁱ—Er1—O5	66.24 (9)	N2—C4—C5	121.7 (4)
O8ⁱⁱ—Er1—O5	69.19 (10)	N2—C4—H4	119.2
O2ⁱⁱⁱ—Er1—O5	74.90 (10)	C5—C4—H4	119.2
O4—Er1—N1	139.39 (11)	N1—C5—C4	121.7 (4)
O7—Er1—N1	67.09 (10)	N1—C5—H5	119.1
O1—Er1—N1	64.79 (10)	C4—C5—H5	119.1
O6ⁱ—Er1—N1	70.67 (10)	O3—C6—O4	126.7 (4)
O8ⁱⁱ—Er1—N1	128.36 (10)	O3—C6—C7	117.7 (4)
O2ⁱⁱⁱ—Er1—N1	71.78 (10)	O4—C6—C7	115.6 (4)
O5—Er1—N1	125.49 (10)	N3—C7—C8	122.2 (4)
O4—Er1—N3	63.46 (10)	N3—C7—C6	115.2 (4)
O7—Er1—N3	75.12 (11)	C8—C7—C6	122.6 (4)
O1—Er1—N3	65.75 (11)	N4—C8—C7	121.0 (4)
O6ⁱ—Er1—N3	141.34 (11)	N4—C8—H8	119.5
O8ⁱⁱ—Er1—N3	70.51 (11)	C7—C8—H8	119.5
O2ⁱⁱⁱ—Er1—N3	130.51 (11)	N4—C9—C10	121.6 (4)
O5—Er1—N3	115.07 (10)	N4—C9—H9	119.2
N1—Er1—N3	119.41 (11)	C10—C9—H9	119.2
N4^iv—Ag1—O3^v	121.94 (12)	N3—C10—C9	121.9 (4)
N4^iv—Ag1—N2	95.91 (13)	N3—C10—H10	119.0
O3^v—Ag1—N2	106.55 (13)	C9—C10—H10	119.0
C1—O1—Er1	125.8 (3)	O5—C11—O6	127.3 (4)
C1—O2—Er1^vii	156.2 (3)	O5—C11—C11ⁱ	116.8 (4)
C6—O3—Ag1^viii	123.6 (3)	O6—C11—C11ⁱ	115.9 (4)
C6—O4—Er1	129.8 (3)	O8—C12—O7	127.2 (4)
C11—O5—Er1	119.3 (3)	O8—C12—C12ⁱⁱ	116.4 (5)
C12—O7—Er1	118.2 (3)	O7—C12—C12ⁱⁱ	116.3 (4)
C5—N1—C2	116.5 (4)	H1W—O1W—H2W	103.0
C5—N1—Er1	128.9 (3)	C11—O6—Er1ⁱ	121.8 (3)
C2—N1—Er1	114.6 (3)	C12—O8—Er1ⁱⁱ	117.8 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1W···O1	0.86	2.14	2.971 (6)	162

Table 1

Selected bond lengths (Å)

Er1—O4	2.333 (3)
Er1—O7	2.367 (3)
Er1—O1	2.385 (3)
Er1—O6ⁱ	2.387 (3)
Er1—O8ⁱⁱ	2.388 (3)
Er1—O2ⁱⁱⁱ	2.403 (3)
Er1—O5	2.451 (3)
Er1—N1	2.611 (4)
Er1—N3	2.636 (4)
Ag1—N4^iv	2.299 (4)
Ag1—O3^v	2.312 (3)
Ag1—N2	2.368 (4)
Ag1—O5^vi	2.648 (4)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1W⋯O1	0.86	2.14	2.971 (6)	162

3 in total

Review 1. Lanthanide-transition metal coordination polymers based on multiple N- and O-donor ligands.

Authors: Youfu Zhou; Maochun Hong; Xintao Wu
Journal: Chem Commun (Camb) Date: 2005-11-22 Impact factor: 6.222

2. A short history of SHELX.

Authors: George M Sheldrick
Journal: Acta Crystallogr A Date: 2007-12-21 Impact factor: 2.290

3. A sodalite-like framework based on octacyanomolybdate and neodymium with guest methanol molecules and neodymium octahydrate ions.

Authors: Zhao-Xi Wang; Xiao-Fei Shen; Jun Wang; Peng Zhang; Yi-Zhi Li; Emmanuel N Nfor; You Song; Shin-ichi Ohkoshi; Kazuhito Hashimoto; Xiao-Zeng You
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3 in total