Poly[[tetra-kis-(μ(2)-pyrazine N,N'-dioxide-κO:O')erbium(III)] tris-(perchlorate)].

The title three-dimensional coordination network, {[Er(C(4)H(4)N(2)O(2))(4)](ClO(4))(3)}(n), is isostructural to that of other lanthanides. The Er(+3 )cation lies on a fourfold roto-inversion axis. It is coordinated in a distorted square-anti-prismatic fashion by eight O atoms from bridging pyrazine N,N'-dioxide ligands. There are two unique pyrazine N,N'-dioxide ligands. One ring is located around an inversion center, and there is a a twofold rotation axis at the center of the other ring. There are also two unique perchlorate anions. One is centered on a twofold rotation axis and the other on a fourfold roto-inversion axis. The perchlorate anions are located in channels that run perpendicular to (001) and (110) and inter-act with the coordination network through C-H⋯O hydrogen bonds.

Related literature

For the isostructural La, Ce, Pr, Sm, Eu, Gd, Tb and Y coordination networks, see: Sun et al. (2004 ▶). For the isostructural Nd, Dy and Ho coordination networks, see: Quinn-Elmore et al. (2010a ▶,b ▶); Buchner et al. (2010 ▶), respectively. Detailed background to this study is described in the first article of this series by Quinn-Elmore et al. (2010a ▶).

Experimental

Crystal data

[Er(C4H4N2O2)4](ClO4)3

M = 913.98

Tetragonal,

a = 15.1777 (4) Å

c = 22.5094 (12) Å

V = 5185.3 (3) Å3

Z = 8

Mo Kα radiation

μ = 3.66 mm−1

T = 100 K

0.44 × 0.44 × 0.18 mm

Data collection

Bruker SMART APEX CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.725, T max = 1.000

27002 measured reflections

1997 independent reflections

1775 reflections with I > 2σ(I)

R int = 0.024

Refinement

R[F 2 > 2σ(F 2)] = 0.032

wR(F 2) = 0.092

S = 0.98

1997 reflections

110 parameters

H-atom parameters constrained

Δρmax = 3.41 e Å−3

Δρmin = −1.62 e Å−3

Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT-Plus (Bruker, 2007 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: X-SEED (Barbour, 2001 ▶); software used to prepare material for publication: X-SEED.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810031843/zl2301sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810031843/zl2301Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Er(C4H4N2O2)4](ClO4)3	Dx = 2.342 Mg m−3
Mr = 913.98	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I41/acd	Cell parameters from 13828 reflections
Hall symbol: -I 4bd 2c	θ = 2.6–30.6°
a = 15.1777 (4) Å	µ = 3.66 mm−1
c = 22.5094 (12) Å	T = 100 K
V = 5185.3 (3) Å3	Block, yellow
Z = 8	0.44 × 0.44 × 0.18 mm
F(000) = 3576

Bruker SMART APEX CCD diffractometer	1997 independent reflections
Radiation source: fine-focus sealed tube	1775 reflections with I > 2σ(I)
graphite	Rint = 0.024
ω scans	θmax = 30.6°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Bruker, 2001)	h = −21→21
Tmin = 0.725, Tmax = 1.000	k = −21→21
27002 measured reflections	l = −32→32

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)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.092	H-atom parameters constrained
S = 0.98	w = 1/[σ2(Fo2) + (0.0554P)2 + 37.1849P] where P = (Fo2 + 2Fc2)/3
1997 reflections	(Δ/σ)max = 0.001
110 parameters	Δρmax = 3.41 e Å−3
0 restraints	Δρmin = −1.62 e Å−3

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.

	x	y	z	Uiso*/Ueq
Er1	0.5000	0.2500	0.3750	0.00421 (10)
Cl1	0.5000	0.2500	0.1250	0.0105 (3)
Cl2	0.72764 (5)	−0.02236 (5)	0.1250	0.0251 (2)
O1	0.59052 (11)	0.21840 (12)	0.29594 (8)	0.0150 (3)
O2	0.53202 (12)	0.39323 (11)	0.34440 (8)	0.0146 (3)
O3	0.57685 (14)	0.24307 (14)	0.16232 (9)	0.0230 (4)
O4	0.6459 (3)	−0.0156 (4)	0.1512 (3)	0.116 (2)
O5	0.7922 (3)	−0.0078 (3)	0.1690 (3)	0.0919 (17)
N1	0.66916 (14)	0.23390 (14)	0.27491 (9)	0.0130 (4)
N2	0.52617 (14)	0.44427 (13)	0.29795 (9)	0.0120 (4)
C1	0.70908 (16)	0.17164 (16)	0.24123 (10)	0.0142 (4)
H1	0.6810	0.1164	0.2351	0.017*
C2	0.78967 (15)	0.18759 (16)	0.21586 (11)	0.0140 (4)
H2	0.8168	0.1438	0.1918	0.017*
C3	0.52531 (17)	0.41139 (15)	0.24210 (10)	0.0138 (4)
H3	0.5249	0.3494	0.2361	0.017*
C4	0.52504 (17)	0.46718 (15)	0.19415 (10)	0.0142 (4)
H4	0.5240	0.4436	0.1551	0.017*

	U11	U22	U33	U12	U13	U23
Er1	0.00435 (11)	0.00435 (11)	0.00392 (14)	−0.00025 (5)	0.000	0.000
Cl1	0.0123 (5)	0.0123 (5)	0.0067 (7)	0.000	0.000	0.000
Cl2	0.0235 (3)	0.0235 (3)	0.0283 (5)	−0.0089 (4)	0.0048 (2)	−0.0048 (2)
O1	0.0094 (7)	0.0220 (9)	0.0137 (7)	−0.0028 (6)	0.0040 (6)	−0.0033 (7)
O2	0.0220 (9)	0.0114 (7)	0.0105 (7)	−0.0015 (6)	−0.0032 (7)	0.0043 (6)
O3	0.0168 (9)	0.0376 (12)	0.0147 (9)	0.0044 (7)	−0.0043 (8)	−0.0022 (7)
O4	0.052 (3)	0.120 (4)	0.175 (5)	−0.003 (3)	0.075 (3)	0.000 (4)
O5	0.077 (3)	0.070 (3)	0.129 (5)	−0.002 (2)	−0.055 (3)	−0.029 (3)
N1	0.0110 (9)	0.0165 (9)	0.0113 (9)	−0.0011 (7)	0.0013 (7)	−0.0005 (8)
N2	0.0136 (9)	0.0107 (8)	0.0117 (9)	0.0001 (7)	−0.0016 (7)	0.0023 (7)
C1	0.0131 (10)	0.0149 (10)	0.0145 (10)	−0.0009 (8)	0.0016 (8)	−0.0019 (8)
C2	0.0122 (10)	0.0169 (11)	0.0128 (10)	−0.0003 (8)	0.0007 (8)	−0.0022 (8)
C3	0.0183 (11)	0.0105 (10)	0.0125 (10)	−0.0021 (8)	−0.0015 (9)	−0.0007 (8)
C4	0.0193 (11)	0.0115 (10)	0.0118 (10)	−0.0002 (8)	−0.0002 (9)	−0.0002 (8)

Er1—O1i	2.2989 (17)	Cl2—O5vi	1.410 (4)
Er1—O1ii	2.2989 (17)	O1—N1	1.305 (3)
Er1—O1	2.2989 (17)	O2—N2	1.304 (2)
Er1—O1iii	2.2989 (17)	N1—C1	1.354 (3)
Er1—O2i	2.3316 (17)	N1—C2vii	1.361 (3)
Er1—O2ii	2.3316 (17)	N2—C3	1.353 (3)
Er1—O2	2.3316 (17)	N2—C4viii	1.356 (3)
Er1—O2iii	2.3316 (17)	C1—C2	1.371 (3)
Cl1—O3	1.441 (2)	C1—H1	0.9500
Cl1—O3iv	1.441 (2)	C2—N1vii	1.361 (3)
Cl1—O3iii	1.441 (2)	C2—H2	0.9500
Cl1—O3v	1.441 (2)	C3—C4	1.372 (3)
Cl2—O4vi	1.377 (4)	C3—H3	0.9500
Cl2—O4	1.377 (4)	C4—N2viii	1.356 (3)
Cl2—O5	1.410 (4)	C4—H4	0.9500
O1i—Er1—O1ii	78.54 (9)	O3iv—Cl1—O3iii	109.86 (9)
O1i—Er1—O1	148.06 (9)	O3—Cl1—O3v	109.86 (9)
O1ii—Er1—O1	110.48 (9)	O3iv—Cl1—O3v	108.69 (17)
O1i—Er1—O1iii	110.48 (9)	O3iii—Cl1—O3v	109.86 (9)
O1ii—Er1—O1iii	148.06 (9)	O4vi—Cl2—O4	108.5 (5)
O1—Er1—O1iii	78.55 (9)	O4vi—Cl2—O5	113.0 (3)
O1i—Er1—O2i	80.86 (7)	O4—Cl2—O5	108.3 (4)
O1ii—Er1—O2i	72.63 (6)	O4vi—Cl2—O5vi	108.3 (4)
O1—Er1—O2i	73.44 (6)	O4—Cl2—O5vi	113.0 (3)
O1iii—Er1—O2i	137.94 (6)	O5—Cl2—O5vi	105.9 (5)
O1i—Er1—O2ii	72.63 (6)	N1—O1—Er1	142.15 (15)
O1ii—Er1—O2ii	80.86 (7)	N2—O2—Er1	140.93 (15)
O1—Er1—O2ii	137.94 (6)	O1—N1—C1	119.1 (2)
O1iii—Er1—O2ii	73.44 (6)	O1—N1—C2vii	121.5 (2)
O2i—Er1—O2ii	145.63 (8)	C1—N1—C2vii	119.4 (2)
O1i—Er1—O2	73.44 (6)	O2—N2—C3	121.8 (2)
O1ii—Er1—O2	137.94 (6)	O2—N2—C4viii	119.0 (2)
O1—Er1—O2	80.86 (7)	C3—N2—C4viii	119.2 (2)
O1iii—Er1—O2	72.63 (6)	N1—C1—C2	120.6 (2)
O2i—Er1—O2	72.46 (9)	N1—C1—H1	119.7
O2ii—Er1—O2	118.42 (9)	C2—C1—H1	119.7
O1i—Er1—O2iii	137.94 (6)	N1vii—C2—C1	120.0 (2)
O1ii—Er1—O2iii	73.44 (6)	N1vii—C2—H2	120.0
O1—Er1—O2iii	72.63 (6)	C1—C2—H2	120.0
O1iii—Er1—O2iii	80.87 (7)	N2—C3—C4	120.2 (2)
O2i—Er1—O2iii	118.42 (9)	N2—C3—H3	119.9
O2ii—Er1—O2iii	72.46 (9)	C4—C3—H3	119.9
O2—Er1—O2iii	145.64 (8)	N2viii—C4—C3	120.6 (2)
O3—Cl1—O3iv	109.86 (9)	N2viii—C4—H4	119.7
O3—Cl1—O3iii	108.69 (17)	C3—C4—H4	119.7

D—H···A	D—H	H···A	D···A	D—H···A
C2—H2···O2vii	0.95	2.50	3.266 (3)	138.
C2—H2···O5	0.95	2.39	3.147 (5)	137.
C3—H3···O1	0.95	2.60	3.321 (3)	133.
C3—H3···O3	0.95	2.45	3.219 (3)	138.
C4—H4···O3iv	0.95	2.35	3.218 (3)	152.

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C2—H2⋯O2i	0.95	2.50	3.266 (3)	138
C2—H2⋯O5	0.95	2.39	3.147 (5)	137
C3—H3⋯O1	0.95	2.60	3.321 (3)	133
C3—H3⋯O3	0.95	2.45	3.219 (3)	138
C4—H4⋯O3ii	0.95	2.35	3.218 (3)	152

Symmetry codes: (i) ; (ii) .