Literature DB >> 21582682

catena-Poly[[[tetra-aqua-zinc(II)]-μ-4,4'-bipyridine-κN:N'] benzene-1,4-di-carboxyl-ate].

Ming-Bo Ruan, Jian-Cheng Deng, Zhi-Gang Li, Jing-Wei Xu.

Abstract

In the title compound, {[Zn(C(10)n class="Species">H(8)N(2))(H(2)O)(4)](C(8)H(4)O(4))}(n), the Zn(II) atoms, lying on a twofold rotation axis, are bridged by 4,4'-bipyridine ligands, resulting in a linear chain along the b axis. In the chain, the Zn(II) atom adopts a slightly distorted octa-hedral coordination geometry involving four water mol-ecules at the equatorial positions. The noncoordinated benzene-1,4-dicarboxyl-ate anion, which is also located on a twofold rotation axis, bridges adjacent chains through O-H⋯O hydrogen bonds, forming a three-dimensional supra-molecular network.

Entities: Chemical Disease Species

Year: 2009 PMID： 21582682 PMCID： PMC2969229 DOI： 10.1107/S1600536809019412

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

Related literature

For background information on hydrothermal reactions, see: Yaghi et al. (2003 ▶). For hydrogen-bond graph-set motifs, see: Bernstein et al. (1995 ▶).

Experimental

Crystal data

[Zn(C10H8N2)(H2O)4](C8H4O4) M = 457.75 Monoclinic, a = 6.9861 (12) Å b = 11.3436 (19) Å c = 11.3219 (19) Å β = 101.209 (3)° V = 880.1 (3) Å3 Z = 2 Mo Kα radiation μ = 1.45 mm−1 T = 186 K 0.21 × 0.18 × 0.12 mm

Data collection

Bruker APEX CCD area-detector diffractometer Absorption correction: multi-scan (; Sheldrick, 1996 ▶) T min = 0.751, T max = 0.845 4812 measured reflections 1735 independent reflections 1465 reflections with I > 2σ(I) R int = 0.035

Refinement

R[F 2 > 2σ(F 2)] = 0.042 wR(F 2) = 0.108 S = 1.08 1735 reflections 136 parameters H-atom parameters constrained Δρmax = 0.64 e Å−3 Δρmin = −0.27 e Å−3 Data collection: SMART (Bruker, 1998 ▶); cell refinement: SAINT-Plus (Bruker, 2003 ▶); data reduction: SAINT-Plus; 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/S1600536809019412/is2415sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809019412/is2415Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Zn(C₁₀H₈N₂)(H₂O)₄](C₈H₄O₄)	F(000) = 472
M_r = 457.75	D_x = 1.727 Mg m⁻³
Monoclinic, P2/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yac	Cell parameters from 1213 reflections
a = 6.9861 (12) Å	θ = 2.3–24.8°
b = 11.3436 (19) Å	µ = 1.45 mm⁻¹
c = 11.3219 (19) Å	T = 186 K
β = 101.209 (3)°	Block, colorless
V = 880.1 (3) Å³	0.21 × 0.18 × 0.12 mm
Z = 2

Bruker APEX CCD area-detector diffractometer	1735 independent reflections
Radiation source: fine-focus sealed tube	1465 reflections with I > 2σ(I)
graphite	R_int = 0.035
φ and ω scans	θ_max = 26.0°, θ_min = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −8→4
T_min = 0.751, T_max = 0.845	k = −14→12
4812 measured reflections	l = −12→13

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)] = 0.042	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.108	H-atom parameters constrained
S = 1.08	w = 1/[σ²(F_o²) + (0.0572P)² + 0.2035P] where P = (F_o² + 2F_c²)/3
1735 reflections	(Δ/σ)_max = 0.001
136 parameters	Δρ_max = 0.64 e Å⁻³
0 restraints	Δρ_min = −0.27 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
Zn1	0.7500	0.60167 (4)	0.7500	0.0231 (2)
N1	0.7500	0.7908 (3)	0.7500	0.0219 (8)
N2	0.7500	1.4169 (3)	0.7500	0.0233 (8)
O1	0.8792 (3)	0.61311 (19)	0.59227 (19)	0.0310 (6)
H1AA	0.8253	0.6201	0.5164	0.037*
H1AB	0.9941	0.6430	0.6054	0.037*
O2	1.0343 (3)	0.59315 (16)	0.8530 (2)	0.0272 (5)
H2AA	1.1223	0.6455	0.8544	0.033*
H2AB	1.1024	0.5339	0.8452	0.033*
O3	0.2410 (4)	0.38845 (18)	0.8474 (2)	0.0329 (6)
O4	0.2079 (3)	−0.22784 (18)	0.64951 (18)	0.0285 (5)
C1	0.8163 (4)	0.8531 (3)	0.8503 (3)	0.0231 (7)
H1A	0.8638	0.8121	0.9211	0.028*
C2	0.8179 (4)	0.9744 (3)	0.8544 (3)	0.0227 (7)
H2A	0.8642	1.0131	0.9267	0.027*
C3	0.7500	1.0391 (4)	0.7500	0.0192 (9)
C4	0.7500	1.1695 (3)	0.7500	0.0177 (9)
C5	0.7615 (5)	1.2339 (3)	0.8561 (3)	0.0223 (7)
H5	0.7694	1.1949	0.9292	0.027*
C6	0.7612 (5)	1.3551 (3)	0.8525 (3)	0.0255 (7)
H6	0.7691	1.3963	0.9243	0.031*
C7	0.2500	0.3377 (4)	0.7500	0.0245 (10)
C8	0.2500	0.2043 (4)	0.7500	0.0201 (9)
C9	0.1895 (4)	0.1414 (3)	0.6432 (3)	0.0225 (7)
H9	0.1501	0.1818	0.5711	0.027*
C10	0.1878 (4)	0.0195 (3)	0.6440 (3)	0.0225 (7)
H10	0.1442	−0.0210	0.5724	0.027*
C11	0.2500	−0.0438 (4)	0.7500	0.0200 (9)
C12	0.2500	−0.1761 (4)	0.7500	0.0244 (10)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zn1	0.0313 (4)	0.0149 (3)	0.0225 (3)	0.000	0.0040 (2)	0.000
N1	0.027 (2)	0.0174 (18)	0.0222 (19)	0.000	0.0068 (15)	0.000
N2	0.028 (2)	0.0169 (18)	0.0242 (19)	0.000	0.0038 (16)	0.000
O1	0.0362 (14)	0.0349 (13)	0.0221 (12)	−0.0073 (10)	0.0066 (10)	−0.0017 (9)
O2	0.0287 (13)	0.0174 (11)	0.0339 (13)	−0.0010 (9)	0.0017 (10)	−0.0001 (9)
O3	0.0464 (16)	0.0256 (12)	0.0253 (13)	0.0101 (10)	0.0036 (11)	−0.0026 (9)
O4	0.0399 (14)	0.0217 (12)	0.0236 (12)	0.0017 (10)	0.0057 (10)	−0.0039 (9)
C1	0.0257 (18)	0.0225 (15)	0.0208 (15)	0.0014 (13)	0.0037 (13)	0.0027 (12)
C2	0.0265 (19)	0.0234 (16)	0.0179 (16)	−0.0005 (13)	0.0034 (13)	−0.0030 (12)
C3	0.018 (2)	0.019 (2)	0.023 (2)	0.000	0.0075 (18)	0.000
C4	0.012 (2)	0.018 (2)	0.023 (2)	0.000	0.0030 (17)	0.000
C5	0.0253 (17)	0.0227 (16)	0.0186 (15)	−0.0007 (13)	0.0032 (13)	0.0014 (12)
C6	0.033 (2)	0.0228 (15)	0.0202 (16)	−0.0001 (14)	0.0046 (14)	−0.0012 (12)
C7	0.025 (3)	0.022 (2)	0.024 (2)	0.000	−0.0009 (19)	0.000
C8	0.017 (2)	0.021 (2)	0.023 (2)	0.000	0.0079 (18)	0.000
C9	0.0266 (19)	0.0230 (15)	0.0181 (15)	0.0028 (13)	0.0047 (13)	0.0030 (12)
C10	0.0215 (18)	0.0267 (16)	0.0195 (16)	0.0009 (13)	0.0040 (13)	−0.0017 (12)
C11	0.018 (2)	0.020 (2)	0.023 (2)	0.000	0.0089 (18)	0.000
C12	0.023 (2)	0.022 (2)	0.029 (2)	0.000	0.006 (2)	0.000

Zn1—N2ⁱ	2.096 (3)	C3—C2ⁱⁱ	1.394 (3)
Zn1—O2ⁱⁱ	2.101 (2)	C3—C4	1.479 (6)
Zn1—O2	2.101 (2)	C4—C5	1.395 (3)
Zn1—N1	2.145 (3)	C4—C5ⁱⁱ	1.395 (3)
Zn1—O1	2.156 (2)	C5—C6	1.376 (4)
Zn1—O1ⁱⁱ	2.156 (2)	C5—H5	0.9300
N1—C1	1.342 (3)	C6—H6	0.9300
N2—C6	1.344 (3)	C7—O3ⁱⁱⁱ	1.256 (3)
O1—H1AA	0.8719	C7—C8	1.513 (6)
O1—H1AB	0.8571	C8—C9	1.397 (3)
O2—H2AA	0.8525	C8—C9ⁱⁱⁱ	1.397 (3)
O2—H2AB	0.8379	C9—C10	1.383 (4)
O3—C7	1.256 (3)	C9—H9	0.9300
O4—C12	1.263 (3)	C10—C11	1.394 (3)
C1—C2	1.377 (4)	C10—H10	0.9300
C1—H1A	0.9300	C11—C10ⁱⁱⁱ	1.394 (4)
C2—C3	1.394 (3)	C11—C12	1.500 (6)
C2—H2A	0.9300	C12—O4ⁱⁱⁱ	1.263 (3)

N2ⁱ—Zn1—O2ⁱⁱ	87.36 (5)	C3—C2—H2A	120.0
N2ⁱ—Zn1—O2	87.36 (5)	C2ⁱⁱ—C3—C2	116.4 (4)
O2ⁱⁱ—Zn1—O2	174.73 (10)	C2ⁱⁱ—C3—C4	121.79 (19)
N2ⁱ—Zn1—N1	180.000 (1)	C2—C3—C4	121.79 (19)
O2ⁱⁱ—Zn1—N1	92.64 (5)	C5—C4—C5ⁱⁱ	116.8 (4)
O2—Zn1—N1	92.64 (5)	C5—C4—C3	121.58 (18)
N2ⁱ—Zn1—O1	93.45 (6)	C5ⁱⁱ—C4—C3	121.58 (18)
O2ⁱⁱ—Zn1—O1	92.63 (9)	C6—C5—C4	119.9 (3)
O2—Zn1—O1	87.69 (9)	C6—C5—H5	120.1
N1—Zn1—O1	86.55 (6)	C4—C5—H5	120.1
N2ⁱ—Zn1—O1ⁱⁱ	93.45 (6)	N2—C6—C5	123.1 (3)
O2ⁱⁱ—Zn1—O1ⁱⁱ	87.69 (9)	N2—C6—H6	118.4
O2—Zn1—O1ⁱⁱ	92.63 (9)	C5—C6—H6	118.4
N1—Zn1—O1ⁱⁱ	86.55 (6)	O3—C7—O3ⁱⁱⁱ	125.5 (4)
O1—Zn1—O1ⁱⁱ	173.10 (12)	O3—C7—C8	117.3 (2)
C1—N1—C1ⁱⁱ	116.4 (4)	O3ⁱⁱⁱ—C7—C8	117.3 (2)
C1—N1—Zn1	121.81 (18)	C9—C8—C9ⁱⁱⁱ	118.5 (4)
C1ⁱⁱ—N1—Zn1	121.81 (18)	C9—C8—C7	120.73 (19)
C6ⁱⁱ—N2—C6	117.2 (4)	C9ⁱⁱⁱ—C8—C7	120.73 (19)
C6ⁱⁱ—N2—Zn1^iv	121.42 (18)	C10—C9—C8	120.5 (3)
C6—N2—Zn1^iv	121.42 (18)	C10—C9—H9	119.8
Zn1—O1—H1AA	130.6	C8—C9—H9	119.8
Zn1—O1—H1AB	114.1	C9—C10—C11	121.3 (3)
H1AA—O1—H1AB	110.2	C9—C10—H10	119.4
Zn1—O2—H2AA	125.3	C11—C10—H10	119.4
Zn1—O2—H2AB	118.2	C10ⁱⁱⁱ—C11—C10	117.9 (4)
H2AA—O2—H2AB	98.0	C10ⁱⁱⁱ—C11—C12	121.03 (19)
N1—C1—C2	123.7 (3)	C10—C11—C12	121.03 (19)
N1—C1—H1A	118.2	O4—C12—O4ⁱⁱⁱ	124.6 (4)
C2—C1—H1A	118.2	O4—C12—C11	117.7 (2)
C1—C2—C3	119.9 (3)	O4ⁱⁱⁱ—C12—C11	117.7 (2)
C1—C2—H2A	120.0

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1AA···O3^v	0.87	1.89	2.753 (3)	169
O1—H1AB···O4^vi	0.86	2.08	2.893 (3)	157
O2—H2AA···O4^vii	0.85	1.87	2.718 (3)	173
O2—H2AB···O3^viii	0.84	1.91	2.742 (3)	171

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1AA⋯O3ⁱ	0.87	1.89	2.753 (3)	169
O1—H1AB⋯O4ⁱⁱ	0.86	2.08	2.893 (3)	157
O2—H2AA⋯O4ⁱⁱⁱ	0.85	1.87	2.718 (3)	173
O2—H2AB⋯O3^iv	0.84	1.91	2.742 (3)	171

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

2 in total

1. Reticular synthesis and the design of new materials.

Authors: Omar M Yaghi; Michael O'Keeffe; Nathan W Ockwig; Hee K Chae; Mohamed Eddaoudi; Jaheon Kim
Journal: Nature Date: 2003-06-12 Impact factor: 49.962

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

1 in total

1. Crystal structure of catena-poly[[[trans-bis(aceto-nitrile-κN)diaquacobalt(II)]-μ-pyrazine-κ(2) N:N'] dinitrate].

Authors: Chen Liu; Ashley C Felts; Annaliese E Thuijs; Aaron Useche; Khalil A Abboud
Journal: Acta Crystallogr E Crystallogr Commun Date: 2016-01-13

1 in total