Literature DB >> 21200658

catena-Poly[[aqua-dipyridine-copper(II)]-μ-fumarato].

Dong Xie¹, Junwei Ye, Yuan Lin, Guiling Ning.

Abstract

The title compound, [Cu(C(4)H(2)O(4))(C(5)H(5)N)(2)(H(2)O)](n), is a one-dimensional coordination polymer based on pyridine and fumarate ligands. Each Cu(II) cation is coordinated by two carboxyl-ate O atoms belonging to two fumarate anions, two N atoms from two pyridine mol-ecules and one water mol-ecule, in a square-based pyramidal geometry. Each fumarate anion bridges two Cu(II) cations through the two carboxyl-ate groups in a bis-monodentate fashion to form a one-dimensional polymeric chain along the c axis. Neighbouring chains are linked together to form a two-dimensional network parallel to the ac plane via hydrogen bonding inter-actions between uncoordinated carboxyl-ate O atoms and coordinated water mol-ecules of adjecent chains.

Entities: Chemical Disease Gene Species

Year: 2007 PMID： 21200658 PMCID： PMC2914965 DOI： 10.1107/S1600536807063738

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

Related literature

For related literature, see: Barthelet et al. (2002 ▶); Che et al. (2006 ▶); Dalai et al. (2002 ▶); Rao et al. (2004 ▶); Yaghi et al. (1998 ▶).

Experimental

Crystal data

[Cu(C4H2O4)(C5H5N)2(H2O)] M = 353.81 Orthorhombic, a = 5.6238 (6) Å b = 15.3174 (16) Å c = 17.4404 (16) Å V = 1502.4 (3) Å3 Z = 4 Mo Kα radiation μ = 1.48 mm−1 T = 273 (2) K 0.32 × 0.32 × 0.22 mm

Data collection

Bruker SMART CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.648, T max = 0.732 9106 measured reflections 3330 independent reflections 2520 reflections with I > 2σ(I) R int = 0.034

Refinement

R[F 2 > 2σ(F 2)] = 0.046 wR(F 2) = 0.116 S = 1.02 3330 reflections 199 parameters H-atom parameters constrained Δρmax = 0.70 e Å−3 Δρmin = −0.33 e Å−3 Absolute structure: Flack (1983 ▶), 1347 Friedel pairs Flack parameter: 0.50 (2) Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1997 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 1997 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536807063738/ci2529sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536807063738/ci2529Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Cu(C₄H₂O₄)(C₅H₅N)₂(H₂O)]	F₀₀₀ = 724
M_r = 353.81	D_x = 1.564 Mg m⁻³
Orthorhombic, P2₁2₁2₁	Mo Kα radiation λ = 0.71073 Å
Hall symbol: P 2ac 2ab	Cell parameters from 2169 reflections
a = 5.6238 (6) Å	θ = 2.3–27.5º
b = 15.3174 (16) Å	µ = 1.48 mm⁻¹
c = 17.4404 (16) Å	T = 273 (2) K
V = 1502.4 (3) Å³	Block, blue
Z = 4	0.32 × 0.32 × 0.22 mm

Bruker SMART CCD area-detector diffractometer	3330 independent reflections
Radiation source: fine-focus sealed tube	2520 reflections with I > 2σ(I)
Monochromator: graphite	R_int = 0.034
Detector resolution: Bruker SMART CCD area-detector pixels mm^-1	θ_max = 27.5º
T = 273(2) K	θ_min = 2.3º
φ and ω scans	h = −7→7
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)	k = −18→19
T_min = 0.648, T_max = 0.732	l = −22→22
9106 measured reflections

Refinement on F²	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F² > 2σ(F²)] = 0.046	w = 1/[σ²(F_o²) + (0.0579P)² + 0.6209P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.116	(Δ/σ)_max = 0.001
S = 1.03	Δρ_max = 0.70 e Å⁻³
3330 reflections	Δρ_min = −0.32 e Å⁻³
199 parameters	Extinction correction: none
Primary atom site location: structure-invariant direct methods	Absolute structure: Flack (1983), with 1347 Friedel pairs
Secondary atom site location: difference Fourier map	Flack parameter: 0.50 (2)

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	U_iso*/U_eq
Cu1	0.25711 (11)	0.97944 (3)	0.87637 (2)	0.03127 (15)
O1	0.2678 (6)	0.9836 (2)	0.76609 (13)	0.0420 (7)
O2	−0.1160 (6)	0.9684 (3)	0.74117 (16)	0.0595 (10)
O3	0.6212 (6)	0.9782 (3)	0.50624 (16)	0.0573 (9)
O4	0.2510 (6)	1.02406 (18)	0.48704 (12)	0.0404 (6)
O5	0.6495 (5)	0.9721 (2)	0.87740 (15)	0.0526 (8)
H5B	0.7218	0.9792	0.8313	0.063*
H5A	0.7522	0.9928	0.9109	0.063*
N1	0.2274 (7)	0.8475 (2)	0.87281 (18)	0.0414 (8)
N2	0.2434 (7)	1.1119 (2)	0.87979 (17)	0.0411 (7)
C1	0.0911 (8)	0.9761 (3)	0.7220 (2)	0.0338 (9)
C2	0.1466 (8)	0.9824 (3)	0.6380 (2)	0.0356 (10)
H2	0.0221	0.9820	0.6030	0.043*
C3	0.3656 (9)	0.9883 (3)	0.6126 (2)	0.0345 (10)
H3	0.4903	0.9872	0.6476	0.041*
C4	0.4217 (9)	0.9968 (2)	0.5281 (2)	0.0320 (11)
C5	0.0718 (10)	0.8032 (4)	0.9141 (3)	0.0586 (14)
H5	−0.0377	0.8337	0.9438	0.070*
C6	0.0664 (13)	0.7118 (4)	0.9146 (4)	0.083 (2)
H6	−0.0454	0.6822	0.9440	0.100*
C7	0.2251 (13)	0.6674 (4)	0.8719 (4)	0.087 (2)
H7	0.2249	0.6067	0.8716	0.105*
C8	0.3846 (13)	0.7123 (4)	0.8294 (4)	0.086 (2)
H8	0.4958	0.6827	0.7998	0.103*
C9	0.3818 (11)	0.8019 (4)	0.8303 (3)	0.0606 (14)
H9	0.4911	0.8320	0.8003	0.073*
C10	0.0860 (10)	1.1570 (3)	0.8377 (3)	0.0581 (15)
H10	−0.0264	1.1269	0.8088	0.070*
C11	0.0874 (12)	1.2476 (4)	0.8363 (4)	0.080 (2)
H11	−0.0234	1.2776	0.8067	0.095*
C12	0.2507 (12)	1.2924 (3)	0.8781 (3)	0.0804 (17)
H12	0.2544	1.3530	0.8771	0.096*
C13	0.4077 (11)	1.2468 (4)	0.9211 (4)	0.0752 (19)
H13	0.5201	1.2761	0.9505	0.090*
C14	0.4004 (9)	1.1567 (3)	0.9211 (3)	0.0538 (13)
H14	0.5091	1.1262	0.9511	0.065*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.0335 (2)	0.0455 (3)	0.01487 (19)	0.0008 (4)	−0.0003 (2)	−0.0007 (2)
O1	0.0401 (18)	0.0715 (17)	0.0145 (11)	−0.003 (2)	−0.0026 (13)	0.0035 (12)
O2	0.039 (2)	0.115 (3)	0.0241 (14)	−0.006 (2)	0.0066 (13)	−0.0059 (19)
O3	0.0350 (19)	0.108 (3)	0.0286 (15)	0.009 (2)	0.0072 (13)	0.0122 (18)
O4	0.0478 (18)	0.0552 (15)	0.0180 (11)	0.010 (3)	0.0002 (15)	0.0010 (12)
O5	0.0291 (14)	0.101 (3)	0.0279 (15)	−0.0031 (16)	−0.0005 (12)	−0.013 (2)
N1	0.046 (2)	0.0493 (19)	0.0295 (16)	0.001 (2)	−0.002 (2)	−0.0013 (15)
N2	0.0424 (18)	0.0470 (19)	0.0340 (16)	−0.007 (2)	−0.001 (3)	0.0016 (15)
C1	0.034 (2)	0.047 (2)	0.0204 (17)	0.001 (2)	0.0036 (15)	−0.005 (2)
C2	0.033 (2)	0.050 (2)	0.023 (2)	0.004 (2)	−0.0031 (16)	−0.003 (2)
C3	0.041 (2)	0.042 (3)	0.020 (2)	−0.0003 (19)	−0.0036 (16)	0.0008 (17)
C4	0.033 (3)	0.041 (3)	0.0226 (19)	−0.0061 (16)	−0.0010 (16)	0.0006 (15)
C5	0.060 (4)	0.053 (3)	0.063 (3)	−0.001 (3)	0.000 (3)	0.000 (3)
C6	0.078 (5)	0.065 (4)	0.107 (5)	−0.016 (4)	−0.013 (4)	0.020 (4)
C7	0.067 (4)	0.047 (3)	0.147 (7)	0.005 (3)	−0.043 (6)	−0.008 (4)
C8	0.072 (5)	0.063 (4)	0.122 (6)	0.015 (4)	−0.014 (4)	−0.037 (4)
C9	0.058 (4)	0.056 (3)	0.068 (4)	0.003 (3)	−0.002 (3)	−0.015 (3)
C10	0.070 (4)	0.045 (3)	0.059 (3)	−0.001 (3)	−0.018 (3)	0.005 (2)
C11	0.085 (5)	0.052 (4)	0.102 (5)	0.010 (3)	−0.031 (4)	0.007 (3)
C12	0.082 (4)	0.046 (3)	0.114 (5)	−0.008 (4)	−0.008 (6)	0.001 (3)
C13	0.070 (4)	0.050 (3)	0.106 (5)	−0.010 (3)	−0.027 (4)	−0.015 (3)
C14	0.045 (3)	0.057 (3)	0.059 (3)	−0.006 (2)	−0.014 (2)	−0.002 (3)

Cu1—O1	1.925 (2)	C3—H3	0.93
Cu1—O4ⁱ	1.931 (2)	C5—C6	1.400 (8)
Cu1—N2	2.031 (3)	C5—H5	0.93
Cu1—N1	2.030 (4)	C6—C7	1.347 (9)
Cu1—O5	2.210 (3)	C6—H6	0.93
O1—C1	1.262 (5)	C7—C8	1.351 (9)
O2—C1	1.218 (5)	C7—H7	0.93
O3—C4	1.219 (5)	C8—C9	1.372 (8)
O4—C4	1.268 (5)	C8—H8	0.93
O4—Cu1ⁱⁱ	1.931 (2)	C9—H9	0.93
O5—H5B	0.91	C10—C11	1.388 (8)
O5—H5A	0.88	C10—H10	0.93
N1—C5	1.321 (6)	C11—C12	1.358 (8)
N1—C9	1.338 (6)	C11—H11	0.93
N2—C14	1.330 (6)	C12—C13	1.352 (8)
N2—C10	1.342 (6)	C12—H12	0.93
C1—C2	1.501 (5)	C13—C14	1.381 (7)
C2—C3	1.312 (6)	C13—H13	0.93
C2—H2	0.93	C14—H14	0.93
C3—C4	1.513 (5)

O1—Cu1—O4ⁱ	179.45 (15)	O4—C4—C3	114.9 (4)
O1—Cu1—N2	89.83 (13)	N1—C5—C6	122.1 (6)
O4ⁱ—Cu1—N2	89.86 (12)	N1—C5—H5	119.0
O1—Cu1—N1	90.30 (13)	C6—C5—H5	119.0
O4ⁱ—Cu1—N1	90.06 (12)	C7—C6—C5	119.2 (7)
N2—Cu1—N1	173.11 (17)	C7—C6—H6	120.4
O1—Cu1—O5	88.78 (12)	C5—C6—H6	120.4
O4ⁱ—Cu1—O5	90.80 (12)	C6—C7—C8	119.0 (6)
N2—Cu1—O5	95.07 (15)	C6—C7—H7	120.5
N1—Cu1—O5	91.82 (15)	C8—C7—H7	120.5
C1—O1—Cu1	125.5 (3)	C7—C8—C9	119.7 (7)
C4—O4—Cu1ⁱⁱ	124.9 (3)	C7—C8—H8	120.1
Cu1—O5—H5B	115.7	C9—C8—H8	120.1
Cu1—O5—H5A	130.0	N1—C9—C8	122.4 (6)
H5B—O5—H5A	104.5	N1—C9—H9	118.8
C5—N1—C9	117.6 (5)	C8—C9—H9	118.8
C5—N1—Cu1	123.3 (3)	N2—C10—C11	121.4 (5)
C9—N1—Cu1	118.9 (4)	N2—C10—H10	119.3
C14—N2—C10	117.9 (4)	C11—C10—H10	119.3
C14—N2—Cu1	120.4 (3)	C12—C11—C10	120.0 (6)
C10—N2—Cu1	121.6 (3)	C12—C11—H11	120.0
O2—C1—O1	126.5 (4)	C10—C11—H11	120.0
O2—C1—C2	118.2 (4)	C13—C12—C11	118.6 (6)
O1—C1—C2	115.2 (4)	C13—C12—H12	120.7
C3—C2—C1	122.0 (4)	C11—C12—H12	120.7
C3—C2—H2	119.0	C12—C13—C14	119.8 (5)
C1—C2—H2	119.0	C12—C13—H13	120.1
C2—C3—C4	122.1 (4)	C14—C13—H13	120.1
C2—C3—H3	119.0	N2—C14—C13	122.4 (5)
C4—C3—H3	119.0	N2—C14—H14	118.8
O3—C4—O4	126.7 (4)	C13—C14—H14	118.8
O3—C4—C3	118.4 (4)

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5B···O2ⁱⁱⁱ	0.91	1.82	2.718 (4)	167
O5—H5A···O3^iv	0.88	1.86	2.700 (4)	158

Cu1—O1	1.925 (2)
Cu1—O4ⁱ	1.931 (2)
Cu1—N2	2.031 (3)
Cu1—N1	2.030 (4)
Cu1—O5	2.210 (3)

O1—Cu1—O4ⁱ	179.45 (15)
O1—Cu1—N2	89.83 (13)
O4ⁱ—Cu1—N2	89.86 (12)
O1—Cu1—N1	90.30 (13)
O4ⁱ—Cu1—N1	90.06 (12)
N2—Cu1—N1	173.11 (17)
O1—Cu1—O5	88.78 (12)
O4ⁱ—Cu1—O5	90.80 (12)
N2—Cu1—O5	95.07 (15)
N1—Cu1—O5	91.82 (15)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5B⋯O2ⁱⁱ	0.91	1.82	2.718 (4)	167
O5—H5A⋯O3ⁱⁱⁱ	0.88	1.86	2.700 (4)	158

Symmetry codes: (ii) ; (iii) .

1 in total

1. A breathing hybrid organic-inorganic solid with very large pores and high magnetic characteristics.

Authors: Karin Barthelet; Jérôme Marrot; Didier Riou; Gérard Férey
Journal: Angew Chem Int Ed Engl Date: 2002-01-18 Impact factor: 15.336

1 in total