Literature DB >> 22199522

catena-Poly[[[triaqua-copper(II)]-μ-2,2'-bipyridine-3,3'-dicarboxyl-ato-κN,N':O] monohydrate].

Qihui Wu¹, Fuxiang Wang, Nanqing Jiang, Li Cao, Qinhe Pan.

Abstract

The title compound, {[Cu(C(12)H(6)N(2)O(4))(H(2)O)(3)]·H(2)O}(n), was synthesized under hydro-thermal conditions. The Cu(2+) ion is six-coordinated by three water O atoms, and two N atoms and one O atom of the 2,2'-bipyridine-3,3'-dicarboxyl-ate bridging ligand in a sligthly distorted octa-hedral environment. The 2,2-bipyridine-3,3'-dicarboxyl-ate bridges link the Cu(2+) ions into chains along the b-axis direction. These chains are further linked by O-H⋯O hydrogen bonds involving the water solvent mol-ecules, forming a three-dimensional framework.

Entities: CellLine Chemical Disease Species

Year: 2011 PMID： 22199522 PMCID： PMC3238631 DOI： 10.1107/S1600536811046423

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

Related literature

For potential applications of coordination polymers in drug delivery, shape-selective sorption/separation and catalysis, see: Chen & Tong (2007 ▶); Zeng et al. (2009 ▶). Their structures vary from one-dimensional to three-dimensional architectures, see: Du & Bu (2009 ▶); Qiu & Zhu (2009 ▶). For our recent research on the synthesis of coordination polymers, see: Pan et al. (2010a ▶,b ▶,c ▶, 2011 ▶).

Experimental

Crystal data

[Cu(C12H6N2O4)(H2O)3]·H2O M = 377.79 Monoclinic, a = 9.950 (4) Å b = 9.161 (4) Å c = 15.974 (7) Å β = 96.848 (8)° V = 1445.7 (10) Å3 Z = 4 Mo Kα radiation μ = 1.56 mm−1 T = 296 K 0.30 × 0.18 × 0.15 mm

Data collection

Bruker APEXII CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2005 ▶) T min = 0.722, T max = 0.792 10263 measured reflections 3585 independent reflections 2268 reflections with I > 2σ(I) R int = 0.062

Refinement

R[F 2 > 2σ(F 2)] = 0.054 wR(F 2) = 0.153 S = 1.08 3585 reflections 208 parameters H-atom parameters constrained Δρmax = 1.02 e Å−3 Δρmin = −1.13 e Å−3 Data collection: APEX2 (Bruker, 2005 ▶); cell refinement: SAINT (Bruker, 2005 ▶); 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 datablock(s) I, global. DOI: 10.1107/S1600536811046423/yk2027sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811046423/yk2027Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Cu(C₁₂H₆N₂O₄)(H₂O)₃]·H₂O	Z = 4
M_r = 377.79	F(000) = 772
Monoclinic, P2₁/n	D_x = 1.736 Mg m⁻³
Hall symbol: -P 2yn	Mo Kα radiation, λ = 0.71073 Å
a = 9.950 (4) Å	θ = 1.0–28.4°
b = 9.161 (4) Å	µ = 1.56 mm⁻¹
c = 15.974 (7) Å	T = 296 K
β = 96.848 (8)°	Rod-like, blue
V = 1445.7 (10) Å³	0.3 × 0.18 × 0.15 mm

Bruker APEXII CCD area-detector diffractometer	3585 independent reflections
Radiation source: fine-focus sealed tube	2268 reflections with I > 2σ(I)
graphite	R_int = 0.062
Detector resolution: 5.00 pixels mm^-1	θ_max = 28.4°, θ_min = 2.3°
phi and ω scans	h = −10→13
Absorption correction: multi-scan (SADABS; Bruker, 2005)	k = −12→12
T_min = 0.722, T_max = 0.792	l = −21→21
10263 measured reflections

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)] = 0.054	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.153	H-atom parameters constrained
S = 1.08	w = 1/[σ²(F_o²) + (0.0663P)² + 0.4177P] where P = (F_o² + 2F_c²)/3
3585 reflections	(Δ/σ)_max < 0.001
208 parameters	Δρ_max = 1.02 e Å⁻³
0 restraints	Δρ_min = −1.13 e Å⁻³

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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	−0.03139 (5)	0.32126 (5)	0.24233 (3)	0.02945 (18)
O1	0.5391 (3)	0.5386 (4)	0.1205 (3)	0.0636 (12)
O2	0.4238 (3)	0.6377 (3)	0.21712 (17)	0.0274 (6)
O3	0.4864 (3)	0.2420 (4)	0.2535 (2)	0.0508 (9)
O4	0.6054 (3)	0.4033 (3)	0.3363 (2)	0.0453 (9)
O5	−0.1561 (3)	0.1917 (3)	0.1632 (2)	0.0487 (9)
H5A	−0.2390	0.2119	0.1489	0.058*
H5	−0.1267	0.1045	0.1642	0.058*
O6	−0.1426 (3)	0.5059 (3)	0.19990 (19)	0.0373 (7)
H6A	−0.1026	0.5863	0.2126	0.045*
H6	−0.2252	0.5142	0.1795	0.045*
O7	−0.1432 (3)	0.3074 (3)	0.3421 (2)	0.0375 (7)
H7A	−0.2269	0.3278	0.3398	0.045*
H7	−0.1294	0.2276	0.3689	0.045*
N1	0.1256 (3)	0.4331 (3)	0.31322 (19)	0.0232 (7)
N2	0.1029 (3)	0.3501 (3)	0.1547 (2)	0.0243 (7)
C1	0.0730 (4)	0.3334 (5)	0.0718 (3)	0.0346 (10)
H1	−0.0109	0.2945	0.0514	0.042*
C2	0.1597 (5)	0.3706 (6)	0.0152 (3)	0.0438 (12)
H2	0.1373	0.3541	−0.0422	0.053*
C3	0.2821 (5)	0.4335 (5)	0.0460 (3)	0.0399 (11)
H3	0.3430	0.4599	0.0088	0.048*
C4	0.3149 (4)	0.4575 (4)	0.1313 (2)	0.0264 (8)
C5	0.2231 (4)	0.4074 (4)	0.1854 (2)	0.0225 (8)
C6	0.2437 (4)	0.4159 (4)	0.2795 (2)	0.0230 (8)
C7	0.3662 (4)	0.4059 (4)	0.3308 (2)	0.0261 (9)
C8	0.3664 (4)	0.4325 (5)	0.4164 (3)	0.0370 (10)
H8	0.4477	0.4297	0.4517	0.044*
C9	0.2479 (5)	0.4629 (6)	0.4497 (3)	0.0420 (11)
H9	0.2483	0.4865	0.5063	0.050*
C10	0.1292 (4)	0.4572 (5)	0.3962 (3)	0.0336 (10)
H10	0.0479	0.4707	0.4186	0.040*
C11	0.4367 (4)	0.5507 (5)	0.1593 (3)	0.0335 (10)
C12	0.4963 (4)	0.3469 (4)	0.3029 (3)	0.0304 (9)
O1W	0.5895 (3)	0.2368 (4)	0.0943 (3)	0.0610 (11)
H1WA	0.5835	0.3265	0.0808	0.073*
H1W	0.5492	0.2392	0.1383	0.073*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.0221 (3)	0.0281 (3)	0.0382 (3)	−0.0002 (2)	0.0039 (2)	0.0025 (2)
O1	0.054 (2)	0.065 (2)	0.082 (3)	−0.0323 (19)	0.051 (2)	−0.039 (2)
O2	0.0259 (14)	0.0270 (14)	0.0306 (15)	−0.0058 (12)	0.0086 (11)	−0.0046 (12)
O3	0.0329 (17)	0.044 (2)	0.076 (3)	0.0054 (15)	0.0063 (17)	−0.0190 (19)
O4	0.0202 (15)	0.0339 (17)	0.079 (3)	0.0038 (13)	−0.0036 (15)	−0.0010 (17)
O5	0.0301 (17)	0.0296 (17)	0.081 (3)	−0.0008 (13)	−0.0178 (16)	−0.0044 (16)
O6	0.0261 (15)	0.0325 (16)	0.0517 (19)	0.0042 (12)	−0.0018 (13)	0.0067 (14)
O7	0.0219 (14)	0.0347 (17)	0.058 (2)	0.0061 (12)	0.0150 (13)	0.0121 (14)
N1	0.0223 (16)	0.0232 (16)	0.0243 (17)	0.0012 (13)	0.0033 (13)	0.0001 (13)
N2	0.0232 (16)	0.0259 (17)	0.0237 (17)	−0.0036 (13)	0.0018 (13)	−0.0011 (13)
C1	0.034 (2)	0.038 (2)	0.031 (2)	−0.0079 (19)	0.0003 (18)	−0.0036 (19)
C2	0.057 (3)	0.049 (3)	0.026 (2)	−0.006 (2)	0.002 (2)	−0.006 (2)
C3	0.049 (3)	0.043 (3)	0.030 (2)	−0.008 (2)	0.016 (2)	−0.003 (2)
C4	0.027 (2)	0.026 (2)	0.028 (2)	−0.0050 (16)	0.0089 (16)	−0.0048 (16)
C5	0.0226 (18)	0.0193 (18)	0.026 (2)	0.0027 (15)	0.0040 (15)	−0.0014 (15)
C6	0.0201 (18)	0.0187 (18)	0.030 (2)	−0.0027 (15)	0.0026 (15)	−0.0003 (15)
C7	0.0236 (19)	0.0221 (19)	0.031 (2)	−0.0005 (15)	−0.0016 (16)	−0.0004 (16)
C8	0.033 (2)	0.040 (3)	0.034 (2)	−0.003 (2)	−0.0097 (19)	−0.001 (2)
C9	0.045 (3)	0.060 (3)	0.021 (2)	−0.007 (2)	0.0029 (19)	−0.003 (2)
C10	0.034 (2)	0.038 (2)	0.031 (2)	−0.0007 (19)	0.0101 (18)	−0.0053 (19)
C11	0.030 (2)	0.032 (2)	0.040 (3)	−0.0075 (18)	0.0146 (18)	−0.0015 (19)
C12	0.0213 (19)	0.025 (2)	0.044 (3)	0.0033 (16)	0.0005 (17)	0.0032 (18)
O1W	0.040 (2)	0.056 (2)	0.086 (3)	0.0137 (18)	0.0043 (19)	−0.014 (2)

Cu1—O5	2.043 (3)	N2—C5	1.344 (5)
Cu1—O7	2.053 (3)	C1—C2	1.365 (6)
Cu1—O2ⁱ	2.056 (3)	C1—H1	0.9300
Cu1—N2	2.064 (3)	C2—C3	1.383 (6)
Cu1—N1	2.085 (3)	C2—H2	0.9300
Cu1—O6	2.090 (3)	C3—C4	1.380 (6)
O1—C11	1.259 (5)	C3—H3	0.9300
O2—C11	1.239 (5)	C4—C5	1.408 (5)
O2—Cu1ⁱⁱ	2.056 (3)	C4—C11	1.506 (5)
O3—C12	1.241 (5)	C5—C6	1.495 (5)
O4—C12	1.261 (5)	C6—C7	1.388 (5)
O5—H5A	0.8500	C7—C8	1.389 (6)
O5—H5	0.8500	C7—C12	1.518 (5)
O6—H6A	0.8501	C8—C9	1.379 (6)
O6—H6	0.8509	C8—H8	0.9300
O7—H7A	0.8500	C9—C10	1.373 (6)
O7—H7	0.8499	C9—H9	0.9300
N1—C10	1.341 (5)	C10—H10	0.9300
N1—C6	1.359 (5)	O1W—H1WA	0.8500
N2—C1	1.332 (5)	O1W—H1W	0.8500

O5—Cu1—O7	95.69 (14)	C1—C2—C3	117.9 (4)
O5—Cu1—O2ⁱ	88.56 (12)	C1—C2—H2	121.1
O7—Cu1—O2ⁱ	90.86 (11)	C3—C2—H2	121.1
O5—Cu1—N2	92.82 (14)	C4—C3—C2	120.8 (4)
O7—Cu1—N2	171.37 (12)	C4—C3—H3	119.6
O2ⁱ—Cu1—N2	87.91 (12)	C2—C3—H3	119.6
O5—Cu1—N1	169.05 (13)	C3—C4—C5	117.4 (4)
O7—Cu1—N1	92.80 (12)	C3—C4—C11	118.1 (4)
O2ⁱ—Cu1—N1	84.41 (12)	C5—C4—C11	124.1 (3)
N2—Cu1—N1	78.58 (12)	N2—C5—C4	121.2 (3)
O5—Cu1—O6	90.61 (12)	N2—C5—C6	113.4 (3)
O7—Cu1—O6	89.24 (11)	C4—C5—C6	125.4 (3)
O2ⁱ—Cu1—O6	179.16 (12)	N1—C6—C7	121.0 (4)
N2—Cu1—O6	92.12 (12)	N1—C6—C5	112.5 (3)
N1—Cu1—O6	96.42 (12)	C7—C6—C5	126.5 (3)
C11—O2—Cu1ⁱⁱ	131.7 (3)	C6—C7—C8	117.8 (4)
Cu1—O5—H5A	122.6	C6—C7—C12	124.8 (4)
Cu1—O5—H5	110.6	C8—C7—C12	116.7 (4)
H5A—O5—H5	122.0	C9—C8—C7	121.0 (4)
Cu1—O6—H6A	114.2	C9—C8—H8	119.5
Cu1—O6—H6	130.3	C7—C8—H8	119.5
H6A—O6—H6	114.7	C10—C9—C8	117.7 (4)
Cu1—O7—H7A	124.9	C10—C9—H9	121.2
Cu1—O7—H7	111.9	C8—C9—H9	121.2
H7A—O7—H7	108.0	N1—C10—C9	122.8 (4)
C10—N1—C6	119.2 (3)	N1—C10—H10	118.6
C10—N1—Cu1	123.3 (3)	C9—C10—H10	118.6
C6—N1—Cu1	110.8 (2)	O2—C11—O1	125.8 (4)
C1—N2—C5	119.4 (3)	O2—C11—C4	115.8 (3)
C1—N2—Cu1	125.1 (3)	O1—C11—C4	118.3 (4)
C5—N2—Cu1	115.0 (2)	O3—C12—O4	125.9 (4)
N2—C1—C2	123.1 (4)	O3—C12—C7	117.1 (4)
N2—C1—H1	118.4	O4—C12—C7	116.8 (4)
C2—C1—H1	118.4	H1WA—O1W—H1W	99.2

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5A···O1Wⁱⁱⁱ	0.85	1.84	2.669 (5)	167.
O5—H5···O4ⁱ	0.85	1.86	2.689 (4)	167.
O6—H6A···O3ⁱⁱ	0.85	1.88	2.715 (5)	169.
O6—H6···O1ⁱⁱⁱ	0.85	2.43	3.282 (5)	180.
O7—H7A···O4ⁱⁱⁱ	0.85	1.80	2.642 (4)	170.
O7—H7···O1ⁱ	0.85	1.95	2.711 (4)	149.
O1W—H1WA···O1	0.85	2.11	2.850 (5)	146.
O1W—H1W···O3	0.85	2.01	2.854 (6)	170.

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5A⋯O1Wⁱ	0.85	1.84	2.669 (5)	167
O5—H5⋯O4ⁱⁱ	0.85	1.86	2.689 (4)	167
O6—H6A⋯O3ⁱⁱⁱ	0.85	1.88	2.715 (5)	169
O6—H6⋯O1ⁱ	0.85	2.43	3.282 (5)	180
O7—H7A⋯O4ⁱ	0.85	1.80	2.642 (4)	170
O7—H7⋯O1ⁱⁱ	0.85	1.95	2.711 (4)	149
O1W—H1WA⋯O1	0.85	2.11	2.850 (5)	146
O1W—H1W⋯O3	0.85	2.01	2.854 (6)	170

Symmetry codes: (i) ; (ii) ; (iii) .

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