Literature DB >> 21582697

catena-Poly[[[tetra-aqua-cobalt(II)]-μ-4,4'-bipyridine-κN:N'] 2-[4-(2-carboxyl-ato-eth-yl)phen-oxy]acetate].

Xi-Fang Wang, Chong-Bo Liu, De-He Huang, Zhi-Qiang Xiong.

Abstract

In the title complex, {[n class="Chemical">Co(C(10)H(8)N(2))(H(2)O)(4)](C(11)H(10)O(5))}(n), the unique Co(II) ion lies on an inversion center and is coordinated by two N atoms from two 4,4'-bipyridine ligands and four O atoms from four water mol-ecules in a slightly distorted octa-hedral coordination geometry. The 4,4'-bipyridine ligands bridge Co(II) ions into a one-dimensional chain structure. In the crystal structure, inter-molecular O-H⋯O hydrogen bonds link cations and anions into a three-dimensional network. The dianions are completely disordered about an inversion center.

Entities: Chemical Disease Species

Year: 2009 PMID： 21582697 PMCID： PMC2969250 DOI： 10.1107/S1600536809021552

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

Related literature

For background to assembly of high-dimensional supramolecular coordination n class="Chemical">polymers, see: Ye et al. (2005 ▶). For 3-(4-hydroxyphenyl)propanoic acid as a potential multidentate ligand and a good donor and acceptor of hydrogen bonds, see: Tan et al. (2007 ▶). 4,4′-Bipyridine is widely used as a spacer in the construction of supramolecular architectures, see: Tao et al. (2000 ▶); Cussen et al. (2002 ▶). For the analogous one-dimensional structure with a 3-carboxylatophenoxyacetate dianion, see: Zhao et al. (2005 ▶).

Experimental

Crystal data

[Co(C10n class="Species">H8N2)(H2O)4](C11H10O5) M = 509.37 Triclinic, a = 7.1311 (10) Å b = 7.6319 (10) Å c = 10.4978 (14) Å α = 91.930 (1)° β = 101.832 (1)° γ = 94.002 (1)° V = 557.15 (13) Å3 Z = 1 Mo Kα radiation μ = 0.83 mm−1 T = 291 K 0.50 × 0.41 × 0.21 mm

Data collection

Bruker SMART CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.674, T max = 0.845 4108 measured reflections 2036 independent reflections 2008 reflections with I > 2σ(I) R int = 0.011

Refinement

R[F 2 > 2σ(F 2)] = 0.036 wR(F 2) = 0.085 S = 1.06 2036 reflections 176 parameters 364 restraints H-atom parameters constrained Δρmax = 0.61 e Å−3 Δρmin = −0.63 e Å−3 Data collection: SMART (Bruker, 1998 ▶); cell refinement: SAINT (Bruker, 1998 ▶); 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. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809021552/lh2836sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809021552/lh2836Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Co(C₁₀H₈N₂)(H₂O)₄](C₁₁H₁₀O₅)	Z = 1
M_r = 509.37	F(000) = 265
Triclinic, P1	D_x = 1.518 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.1311 (10) Å	Cell parameters from 3868 reflections
b = 7.6319 (10) Å	θ = 2.7–28.2°
c = 10.4978 (14) Å	µ = 0.83 mm⁻¹
α = 91.930 (1)°	T = 291 K
β = 101.832 (1)°	Block, red
γ = 94.002 (1)°	0.50 × 0.41 × 0.21 mm
V = 557.15 (13) Å³

Bruker SMART CCD diffractometer	2036 independent reflections
Radiation source: fine-focus sealed tube	2008 reflections with I > 2σ(I)
graphite	R_int = 0.011
φ and ω scans	θ_max = 25.5°, θ_min = 2.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −8→8
T_min = 0.674, T_max = 0.845	k = −9→9
4108 measured reflections	l = −12→12

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) = 0.085	H-atom parameters constrained
S = 1.06	w = 1/[σ²(F_o²) + (0.0304P)² + 0.7695P] where P = (F_o² + 2F_c²)/3
2036 reflections	(Δ/σ)_max < 0.001
176 parameters	Δρ_max = 0.61 e Å⁻³
364 restraints	Δρ_min = −0.63 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	U_iso*/U_eq	Occ. (<1)
O3	0.7094 (13)	0.448 (3)	0.8766 (14)	0.0419 (15)	0.50
O4	0.522 (2)	0.2444 (14)	0.9494 (9)	0.0368 (16)	0.50
C8	0.3511 (11)	0.4124 (10)	0.6667 (8)	0.0635 (11)	0.50
H8A	0.4539	0.4806	0.6385	0.076*	0.50
H8B	0.3700	0.2890	0.6533	0.076*	0.50
C6	0.5492 (16)	0.370 (3)	0.879 (3)	0.0363 (9)	0.50
C7	0.3670 (11)	0.4520 (12)	0.8095 (7)	0.0522 (14)	0.50
H7A	0.2547	0.4010	0.8376	0.063*	0.50
H7B	0.3781	0.5780	0.8285	0.063*	0.50
C9	0.1644 (19)	0.451 (2)	0.5829 (11)	0.0583 (13)	0.50
C10	0.1182 (18)	0.3869 (16)	0.4541 (10)	0.0612 (15)	0.50
H10	0.1933	0.3074	0.4232	0.073*	0.50
C11	0.0411 (14)	0.5566 (15)	0.6274 (14)	0.0575 (17)	0.50
H11	0.0658	0.5913	0.7154	0.069*	0.50
O3'	0.7312 (13)	0.450 (3)	0.9043 (14)	0.0419 (15)	0.50
O4'	0.513 (2)	0.2290 (14)	0.9156 (9)	0.0368 (16)	0.50
C6'	0.5648 (17)	0.374 (3)	0.876 (3)	0.0363 (9)	0.50
C7'	0.4168 (11)	0.4553 (12)	0.7713 (8)	0.0522 (14)	0.50
H7'1	0.3503	0.5373	0.8153	0.063*	0.50
H7'2	0.4868	0.5234	0.7173	0.063*	0.50
O5	0.2825 (7)	0.3461 (6)	0.6915 (5)	0.0635 (11)	0.50
C9'	0.1435 (18)	0.435 (2)	0.5964 (11)	0.0583 (13)	0.50
C10'	0.1492 (18)	0.4241 (16)	0.4648 (9)	0.0612 (15)	0.50
H10'	0.2554	0.3795	0.4403	0.073*	0.50
C11'	−0.0013 (14)	0.5223 (14)	0.6328 (14)	0.0575 (17)	0.50
H11'	−0.0012	0.5453	0.7204	0.069*	0.50
Co1	0.0000	0.0000	0.0000	0.02210 (13)
O1	0.0283 (2)	0.2722 (2)	−0.01206 (18)	0.0396 (4)
H1W	−0.0701	0.3243	−0.0349	0.059*
H2W	0.1207	0.3397	0.0241	0.059*
O2	0.2400 (2)	−0.0305 (2)	−0.08486 (16)	0.0338 (4)
H3W	0.3136	0.0561	−0.0905	0.051*
H4W	0.2965	−0.1087	−0.0441	0.051*
N1	0.1824 (3)	0.0139 (3)	0.19142 (17)	0.0288 (4)
C1	0.3560 (3)	0.1002 (3)	0.2175 (2)	0.0341 (5)
H1	0.3934	0.1655	0.1524	0.041*
C2	0.4835 (3)	0.0981 (3)	0.3358 (2)	0.0356 (6)
H2	0.6033	0.1601	0.3483	0.043*
C3	0.4332 (3)	0.0036 (3)	0.4357 (2)	0.0285 (5)
C4	0.2514 (4)	−0.0850 (5)	0.4090 (3)	0.0557 (9)
H4	0.2096	−0.1502	0.4726	0.067*
C5	0.1325 (4)	−0.0761 (4)	0.2877 (3)	0.0532 (8)
H5	0.0114	−0.1361	0.2725	0.064*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
O3	0.0288 (17)	0.0355 (10)	0.050 (5)	−0.0043 (18)	−0.0169 (18)	0.009 (3)
O4	0.0306 (14)	0.0374 (17)	0.038 (4)	0.0015 (14)	−0.005 (3)	0.010 (3)
C8	0.053 (2)	0.056 (2)	0.067 (2)	0.0142 (17)	−0.0250 (18)	0.0040 (18)
C6	0.0301 (17)	0.0288 (13)	0.0428 (15)	0.0016 (14)	−0.0095 (18)	0.0037 (10)
C7	0.044 (3)	0.0434 (16)	0.059 (3)	0.006 (2)	−0.016 (2)	0.011 (2)
C9	0.044 (2)	0.058 (2)	0.065 (2)	0.0198 (19)	−0.0110 (16)	−0.0018 (17)
C10	0.042 (3)	0.063 (3)	0.072 (2)	0.020 (3)	−0.0052 (19)	−0.016 (2)
C11	0.047 (3)	0.063 (3)	0.059 (2)	0.010 (3)	0.001 (2)	−0.001 (2)
O3'	0.0288 (17)	0.0355 (10)	0.050 (5)	−0.0043 (18)	−0.0169 (18)	0.009 (3)
O4'	0.0306 (14)	0.0374 (17)	0.038 (4)	0.0015 (14)	−0.005 (3)	0.010 (3)
C6'	0.0301 (17)	0.0288 (13)	0.0428 (15)	0.0016 (14)	−0.0095 (18)	0.0037 (10)
C7'	0.044 (3)	0.0434 (16)	0.059 (3)	0.006 (2)	−0.016 (2)	0.011 (2)
O5	0.053 (2)	0.056 (2)	0.067 (2)	0.0142 (17)	−0.0250 (18)	0.0040 (18)
C9'	0.044 (2)	0.058 (2)	0.065 (2)	0.0198 (19)	−0.0110 (16)	−0.0018 (17)
C10'	0.042 (3)	0.063 (3)	0.072 (2)	0.020 (3)	−0.0052 (19)	−0.016 (2)
C11'	0.047 (3)	0.063 (3)	0.059 (2)	0.010 (3)	0.001 (2)	−0.001 (2)
Co1	0.0185 (2)	0.0246 (2)	0.0200 (2)	0.00069 (15)	−0.00368 (15)	0.00413 (15)
O1	0.0309 (9)	0.0260 (8)	0.0538 (11)	−0.0002 (7)	−0.0092 (8)	0.0043 (8)
O2	0.0249 (8)	0.0398 (9)	0.0356 (9)	0.0033 (7)	0.0029 (7)	0.0085 (7)
N1	0.0246 (9)	0.0354 (10)	0.0226 (9)	0.0004 (8)	−0.0041 (7)	0.0048 (8)
C1	0.0307 (12)	0.0427 (14)	0.0248 (11)	−0.0057 (10)	−0.0024 (9)	0.0090 (10)
C2	0.0279 (12)	0.0450 (14)	0.0281 (12)	−0.0084 (10)	−0.0052 (9)	0.0073 (10)
C3	0.0280 (11)	0.0307 (11)	0.0229 (11)	0.0029 (9)	−0.0044 (9)	0.0025 (9)
C4	0.0417 (15)	0.084 (2)	0.0310 (14)	−0.0249 (15)	−0.0109 (11)	0.0275 (14)
C5	0.0352 (14)	0.079 (2)	0.0348 (14)	−0.0234 (14)	−0.0105 (11)	0.0218 (14)

O3—C6	1.257 (6)	C10'—H10'	0.9300
O4—C6	1.257 (6)	C11'—C10'ⁱ	1.41 (2)
C8—C9	1.491 (13)	C11'—H11'	0.9300
C8—C7	1.499 (11)	Co1—O1ⁱⁱ	2.0840 (16)
C8—H8A	0.9700	Co1—O1	2.0840 (16)
C8—H8B	0.9700	Co1—O2ⁱⁱ	2.1083 (16)
C6—C7	1.540 (8)	Co1—O2	2.1083 (16)
C7—H7A	0.9700	Co1—N1	2.1530 (17)
C7—H7B	0.9700	Co1—N1ⁱⁱ	2.1531 (17)
C9—C11	1.375 (6)	O1—H1W	0.8271
C9—C10	1.387 (7)	O1—H2W	0.8245
C10—C11ⁱ	1.379 (19)	O2—H3W	0.8262
C10—H10	0.9300	O2—H4W	0.8251
C11—C10ⁱ	1.379 (19)	N1—C1	1.333 (3)
C11—H11	0.9300	N1—C5	1.334 (3)
O3'—C6'	1.258 (6)	C1—C2	1.382 (3)
O4'—C6'	1.255 (6)	C1—H1	0.9300
C6'—C7'	1.537 (7)	C2—C3	1.385 (3)
C7'—O5	1.352 (10)	C2—H2	0.9300
C7'—H7'1	0.9700	C3—C4	1.390 (3)
C7'—H7'2	0.9700	C3—C3ⁱⁱⁱ	1.489 (4)
O5—C9'	1.475 (13)	C4—C5	1.384 (3)
C9'—C11'	1.377 (6)	C4—H4	0.9300
C9'—C10'	1.391 (7)	C5—H5	0.9300
C10'—C11'ⁱ	1.41 (2)

C9—C8—C7	114.6 (7)	C9'—C11'—H11'	120.6
C9—C8—H8A	108.6	C10'ⁱ—C11'—H11'	120.6
C7—C8—H8A	108.6	O1ⁱⁱ—Co1—O1	180
C9—C8—H8B	108.6	O1ⁱⁱ—Co1—O2ⁱⁱ	91.66 (7)
C7—C8—H8B	108.6	O1—Co1—O2ⁱⁱ	88.34 (7)
H8A—C8—H8B	107.6	O1ⁱⁱ—Co1—O2	88.33 (7)
O3—C6—O4	125.4 (9)	O1—Co1—O2	91.66 (7)
O3—C6—C7	118.0 (7)	O2ⁱⁱ—Co1—O2	180
O4—C6—C7	115.7 (8)	O1ⁱⁱ—Co1—N1	88.07 (7)
C8—C7—C6	106.0 (13)	O1—Co1—N1	91.93 (7)
C8—C7—H7A	110.5	O2ⁱⁱ—Co1—N1	89.64 (7)
C6—C7—H7A	110.5	O2—Co1—N1	90.36 (7)
C8—C7—H7B	110.5	O1ⁱⁱ—Co1—N1ⁱⁱ	91.93 (7)
C6—C7—H7B	110.5	O1—Co1—N1ⁱⁱ	88.07 (7)
H7A—C7—H7B	108.7	O2ⁱⁱ—Co1—N1ⁱⁱ	90.36 (7)
C11—C9—C10	118.6 (7)	O2—Co1—N1ⁱⁱ	89.63 (7)
C11—C9—C8	121.7 (6)	N1—Co1—N1ⁱⁱ	180
C10—C9—C8	119.5 (5)	Co1—O1—H1W	118.4
C11ⁱ—C10—C9	119.0 (12)	Co1—O1—H2W	126.8
C11ⁱ—C10—H10	120.5	H1W—O1—H2W	112.0
C9—C10—H10	120.5	Co1—O2—H3W	119.7
C9—C11—C10ⁱ	122.2 (12)	Co1—O2—H4W	104.4
C9—C11—H11	118.9	H3W—O2—H4W	112.1
C10ⁱ—C11—H11	118.9	C1—N1—C5	116.50 (19)
O4'—C6'—O3'	125.8 (9)	C1—N1—Co1	122.27 (15)
O4'—C6'—C7'	116.6 (7)	C5—N1—Co1	121.02 (16)
O3'—C6'—C7'	117.2 (6)	N1—C1—C2	123.7 (2)
O5—C7'—C6'	118.2 (10)	N1—C1—H1	118.2
O5—C7'—H7'1	107.8	C2—C1—H1	118.2
C6'—C7'—H7'1	107.8	C1—C2—C3	120.1 (2)
O5—C7'—H7'2	107.8	C1—C2—H2	119.9
C6'—C7'—H7'2	107.8	C3—C2—H2	119.9
H7'1—C7'—H7'2	107.1	C2—C3—C4	116.2 (2)
C7'—O5—C9'	114.6 (8)	C2—C3—C3ⁱⁱⁱ	121.9 (3)
C11'—C9'—C10'	117.9 (7)	C4—C3—C3ⁱⁱⁱ	121.9 (3)
C11'—C9'—O5	121.8 (6)	C5—C4—C3	120.0 (2)
C10'—C9'—O5	120.2 (6)	C5—C4—H4	120.0
C9'—C10'—C11'ⁱ	122.8 (12)	C3—C4—H4	120.0
C9'—C10'—H10'	118.6	N1—C5—C4	123.5 (2)
C11'ⁱ—C10'—H10'	118.6	N1—C5—H5	118.2
C9'—C11'—C10'ⁱ	118.8 (12)	C4—C5—H5	118.2

C9—C8—C7—C6	168.9 (10)	O1—Co1—N1—C1	−51.9 (2)
O3—C6—C7—C8	76 (3)	O2ⁱⁱ—Co1—N1—C1	−140.20 (19)
O4—C6—C7—C8	−114 (2)	O2—Co1—N1—C1	39.80 (19)
C7—C8—C9—C11	17.1 (18)	N1ⁱⁱ—Co1—N1—C1	66 (3)
C7—C8—C9—C10	−167.0 (13)	O1ⁱⁱ—Co1—N1—C5	−46.4 (2)
C11—C9—C10—C11ⁱ	5(2)	O1—Co1—N1—C5	133.6 (2)
C8—C9—C10—C11ⁱ	−170.8 (13)	O2ⁱⁱ—Co1—N1—C5	45.3 (2)
C10—C9—C11—C10ⁱ	−5(2)	O2—Co1—N1—C5	−134.7 (2)
C8—C9—C11—C10ⁱ	170.5 (13)	N1ⁱⁱ—Co1—N1—C5	−109 (3)
O4'—C6'—C7'—O5	−27 (3)	C5—N1—C1—C2	1.0 (4)
O3'—C6'—C7'—O5	146 (2)	Co1—N1—C1—C2	−173.7 (2)
C6'—C7'—O5—C9'	178.6 (13)	N1—C1—C2—C3	−0.5 (4)
C7'—O5—C9'—C11'	−74.6 (15)	C1—C2—C3—C4	−0.2 (4)
C7'—O5—C9'—C10'	109.2 (15)	C1—C2—C3—C3ⁱⁱⁱ	179.5 (3)
C11'—C9'—C10'—C11'ⁱ	−8(2)	C2—C3—C4—C5	0.3 (5)
O5—C9'—C10'—C11'ⁱ	168.0 (12)	C3ⁱⁱⁱ—C3—C4—C5	−179.4 (3)
C10'—C9'—C11'—C10'ⁱ	8(2)	C1—N1—C5—C4	−0.9 (5)
O5—C9'—C11'—C10'ⁱ	−168.3 (12)	Co1—N1—C5—C4	173.9 (3)
O1ⁱⁱ—Co1—N1—C1	128.1 (2)	C3—C4—C5—N1	0.3 (6)

D—H···A	D—H	H···A	D···A	D—H···A
O2—H4W···O4'ⁱⁱⁱ	0.83	2.00	2.796 (10)	161
O2—H4W···O4ⁱⁱⁱ	0.83	1.86	2.667 (10)	165
O2—H3W···O4^iv	0.83	1.96	2.765 (14)	163
O2—H3W···O4'^iv	0.83	1.86	2.678 (14)	170
O1—H2W···O3^v	0.82	2.07	2.868 (16)	164
O1—H2W···O3'^v	0.82	1.90	2.691 (16)	161
O1—H1W···O3^vi	0.83	1.97	2.789 (13)	169
O1—H1W···O3'^vi	0.83	1.79	2.612 (14)	174

Co1—O1	2.0840 (16)
Co1—O2	2.1083 (16)
Co1—N1	2.1530 (17)

O1ⁱ—Co1—O1	180
O1—Co1—O2ⁱ	88.34 (7)
O1—Co1—O2	91.66 (7)
O2ⁱ—Co1—O2	180
O1—Co1—N1	91.93 (7)
O2—Co1—N1	90.36 (7)
O1—Co1—N1ⁱ	88.07 (7)
O2—Co1—N1ⁱ	89.63 (7)
N1—Co1—N1ⁱ	180

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2—H4W⋯O4′ⁱⁱ	0.83	2.00	2.796 (10)	161
O2—H4W⋯O4ⁱⁱ	0.83	1.86	2.667 (10)	165
O2—H3W⋯O4ⁱⁱⁱ	0.83	1.96	2.765 (14)	163
O2—H3W⋯O4′ⁱⁱⁱ	0.83	1.86	2.678 (14)	170
O1—H2W⋯O3^iv	0.82	2.07	2.868 (16)	164
O1—H2W⋯O3′^iv	0.82	1.90	2.691 (16)	161
O1—H1W⋯O3^v	0.83	1.97	2.789 (13)	169
O1—H1W⋯O3′^v	0.83	1.79	2.612 (14)	174

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

2 in total

1. Flexible sorption and transformation behavior in a microporous metal-organic framework.

Authors: Edmund J Cussen; John B Claridge; Matthew J Rosseinsky; Cameron J Kepert
Journal: J Am Chem Soc Date: 2002-08-14 Impact factor: 15.419

2. A short history of SHELX.

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

2 in total