Literature DB >> 22904749

Poly[[bis-(μ-3-amino-5-carb-oxy-benzoato-κ(2)N:O(1))diaqua-zinc] dihydrate].

Kou-Lin Zhang, Ting-Ting Qiu, Seik Weng Ng.

Abstract

The Zn(II) atom in the title polymeric compound, {[Zn(C(8)H(6)NO(4))(2)(H(2)O)(2)]·2H(2)O}(n), lies on a center of inversion and is coordinated by two amine N atoms and two carboxyl-ate O atoms from two 3-amino-5-carb-oxy-benzoate anions along with two water mol-ecules in a distorted octa-hedral geometry. The bridging nature of the anion generates a layer motif parallel to (100). Hydrogen bonds of the N-H⋯O and O-H⋯O types exist in the structure. One H atom of the coordinated water mol-ecule and one H atom of the solvent water mol-ecule are each disordered over two positions in a 1:1 ratio.

Entities: Chemical Disease Gene

Year: 2012 PMID： 22904749 PMCID： PMC3414142 DOI： 10.1107/S1600536812031789

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

Related literature

For catena-poly[(5-aminoisophthalato)aquazinc], see: Wu et al. (2002 ▶).

Experimental

Crystal data

[Zn(C8H6NO4)2(H2O)2]·2H2O M = 497.71 Monoclinic, a = 14.2209 (10) Å b = 11.2252 (8) Å c = 12.7139 (9) Å β = 113.286 (1)° V = 1864.2 (2) Å3 Z = 4 Mo Kα radiation μ = 1.39 mm−1 T = 293 K 0.30 × 0.26 × 0.18 mm

Data collection

Bruker SMART APEX diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.680, T max = 0.788 8005 measured reflections 2130 independent reflections 1843 reflections with I > 2σ(I) R int = 0.018

Refinement

R[F 2 > 2σ(F 2)] = 0.034 wR(F 2) = 0.098 S = 1.07 2130 reflections 144 parameters H-atom parameters constrained Δρmax = 0.37 e Å−3 Δρmin = −0.37 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: OLEX (Dolomanov et al., 2003 ▶) and X-SEED (Barbour, 2001 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶). Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812031789/xu5588sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812031789/xu5588Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Zn(C₈H₆NO₄)₂(H₂O)₂]·2H₂O	F(000) = 1024
M_r = 497.71	D_x = 1.773 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 4815 reflections
a = 14.2209 (10) Å	θ = 2.4–28.2°
b = 11.2252 (8) Å	µ = 1.39 mm⁻¹
c = 12.7139 (9) Å	T = 293 K
β = 113.286 (1)°	Prism, light brown
V = 1864.2 (2) Å³	0.30 × 0.26 × 0.18 mm
Z = 4

Bruker SMART APEX diffractometer	2130 independent reflections
Radiation source: fine-focus sealed tube	1843 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.018
ω scans	θ_max = 27.5°, θ_min = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −18→15
T_min = 0.680, T_max = 0.788	k = −14→14
8005 measured reflections	l = −16→16

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)] = 0.034	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.098	H-atom parameters constrained
S = 1.07	w = 1/[σ²(F_o²) + (0.0506P)² + 3.2779P] where P = (F_o² + 2F_c²)/3
2130 reflections	(Δ/σ)_max = 0.001
144 parameters	Δρ_max = 0.37 e Å⁻³
0 restraints	Δρ_min = −0.37 e Å⁻³

	x	y	z	U_iso*/U_eq	Occ. (<1)
Zn1	0.2500	0.2500	0.0000	0.02950 (14)
O1	0.20751 (15)	0.32463 (16)	0.12770 (14)	0.0412 (4)
O2	0.1529 (2)	0.1571 (2)	0.1754 (2)	0.0655 (7)
O3	0.09628 (17)	0.14472 (16)	0.53610 (16)	0.0436 (4)
H1	0.0885	0.1154	0.5929	0.065*
O4	0.07472 (15)	0.31377 (16)	0.61500 (15)	0.0408 (4)
O1W	0.35790 (16)	0.38916 (19)	0.03707 (18)	0.0531 (5)
H2	0.3743	0.3994	−0.0189	0.080*
H3	0.4102	0.3714	0.0953	0.080*	0.50
H3'	0.3322	0.4522	0.0496	0.080*	0.50
O2W	0.0898 (2)	−0.04635 (18)	0.22475 (18)	0.0594 (6)
H4	0.1052	0.0229	0.2118	0.089*
H5	0.0334	−0.0439	0.2320	0.089*	0.50
H5'	0.1397	−0.0755	0.2797	0.089*	0.50
N1	0.12864 (15)	0.64309 (17)	0.36983 (16)	0.0312 (4)
H6	0.0705	0.6633	0.3742	0.037*
H7	0.1250	0.6675	0.3025	0.037*
C1	0.1718 (2)	0.2655 (2)	0.1878 (2)	0.0349 (5)
C2	0.15207 (17)	0.3304 (2)	0.28176 (18)	0.0291 (4)
C3	0.15228 (17)	0.4538 (2)	0.28397 (18)	0.0294 (5)
H3A	0.1667	0.4963	0.2293	0.035*
C4	0.13087 (16)	0.5152 (2)	0.36787 (17)	0.0274 (4)
C5	0.11166 (17)	0.4506 (2)	0.45058 (18)	0.0295 (5)
H5A	0.0982	0.4904	0.5073	0.035*
C6	0.11247 (17)	0.3261 (2)	0.44894 (17)	0.0277 (4)
C7	0.13167 (19)	0.2662 (2)	0.3638 (2)	0.0302 (5)
H7A	0.1309	0.1834	0.3618	0.036*
C8	0.09264 (19)	0.2626 (2)	0.54063 (19)	0.0309 (5)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zn1	0.0412 (2)	0.0297 (2)	0.0248 (2)	−0.00028 (15)	0.02079 (16)	−0.00161 (13)
O1	0.0631 (12)	0.0436 (10)	0.0312 (9)	0.0127 (9)	0.0339 (8)	0.0038 (7)
O2	0.121 (2)	0.0466 (12)	0.0583 (13)	−0.0156 (13)	0.0664 (14)	−0.0190 (10)
O3	0.0725 (13)	0.0354 (9)	0.0375 (9)	0.0045 (9)	0.0374 (9)	0.0025 (7)
O4	0.0639 (12)	0.0404 (10)	0.0321 (9)	−0.0022 (9)	0.0340 (8)	−0.0024 (7)
O1W	0.0501 (11)	0.0531 (12)	0.0538 (12)	−0.0046 (9)	0.0181 (9)	−0.0207 (10)
O2W	0.1023 (18)	0.0426 (11)	0.0469 (11)	0.0111 (11)	0.0441 (12)	0.0074 (9)
N1	0.0419 (11)	0.0334 (10)	0.0242 (9)	0.0046 (8)	0.0194 (8)	0.0030 (7)
C1	0.0436 (13)	0.0414 (14)	0.0258 (11)	0.0043 (10)	0.0203 (10)	−0.0048 (9)
C2	0.0323 (11)	0.0388 (12)	0.0199 (9)	0.0037 (9)	0.0142 (8)	−0.0027 (8)
C3	0.0324 (11)	0.0394 (12)	0.0203 (9)	0.0035 (9)	0.0148 (8)	0.0011 (8)
C4	0.0290 (10)	0.0343 (11)	0.0208 (9)	0.0016 (9)	0.0118 (8)	−0.0011 (8)
C5	0.0340 (11)	0.0367 (12)	0.0227 (10)	0.0037 (9)	0.0165 (9)	−0.0024 (8)
C6	0.0295 (11)	0.0366 (11)	0.0200 (9)	0.0015 (9)	0.0129 (8)	0.0000 (8)
C7	0.0376 (12)	0.0323 (11)	0.0256 (10)	0.0033 (9)	0.0178 (9)	−0.0022 (8)
C8	0.0356 (11)	0.0380 (12)	0.0233 (10)	0.0028 (9)	0.0160 (9)	0.0013 (8)

Zn1—O1W	2.108 (2)	O2W—H5'	0.8407
Zn1—O1Wⁱ	2.108 (2)	N1—C4	1.436 (3)
Zn1—O1	2.1163 (16)	N1—Zn1^iv	2.214 (2)
Zn1—O1ⁱ	2.1163 (16)	N1—H6	0.8800
Zn1—N1ⁱⁱ	2.214 (2)	N1—H7	0.8800
Zn1—N1ⁱⁱⁱ	2.214 (2)	C1—C2	1.517 (3)
O1—C1	1.261 (3)	C2—C7	1.390 (3)
O2—C1	1.243 (3)	C2—C3	1.386 (3)
O3—C8	1.326 (3)	C3—C4	1.401 (3)
O3—H1	0.8400	C3—H3A	0.9300
O4—C8	1.217 (3)	C4—C5	1.390 (3)
O1W—H2	0.8400	C5—C6	1.398 (3)
O1W—H3	0.8400	C5—H5A	0.9300
O1W—H3'	0.8400	C6—C7	1.390 (3)
O2W—H4	0.8408	C6—C8	1.486 (3)
O2W—H5	0.8425	C7—H7A	0.9300

O1W—Zn1—O1Wⁱ	180.00 (9)	Zn1^iv—N1—H6	106.7
O1W—Zn1—O1	86.47 (8)	C4—N1—H7	106.7
O1Wⁱ—Zn1—O1	93.53 (8)	Zn1^iv—N1—H7	106.7
O1W—Zn1—O1ⁱ	93.53 (8)	H6—N1—H7	106.6
O1Wⁱ—Zn1—O1ⁱ	86.47 (8)	O2—C1—O1	123.9 (2)
O1—Zn1—O1ⁱ	180.00 (8)	O2—C1—C2	118.2 (2)
O1W—Zn1—N1ⁱⁱ	92.80 (8)	O1—C1—C2	117.9 (2)
O1Wⁱ—Zn1—N1ⁱⁱ	87.20 (8)	C7—C2—C3	120.2 (2)
O1—Zn1—N1ⁱⁱ	89.10 (7)	C7—C2—C1	120.1 (2)
O1ⁱ—Zn1—N1ⁱⁱ	90.90 (7)	C3—C2—C1	119.8 (2)
O1W—Zn1—N1ⁱⁱⁱ	87.20 (8)	C2—C3—C4	120.5 (2)
O1Wⁱ—Zn1—N1ⁱⁱⁱ	92.80 (8)	C2—C3—H3A	119.7
O1—Zn1—N1ⁱⁱⁱ	90.90 (7)	C4—C3—H3A	119.7
O1ⁱ—Zn1—N1ⁱⁱⁱ	89.10 (7)	C5—C4—C3	119.1 (2)
N1ⁱⁱ—Zn1—N1ⁱⁱⁱ	180.00 (18)	C5—C4—N1	119.72 (19)
C1—O1—Zn1	124.19 (16)	C3—C4—N1	121.18 (19)
C8—O3—H1	109.5	C4—C5—C6	120.31 (19)
Zn1—O1W—H2	109.5	C4—C5—H5A	119.8
Zn1—O1W—H3	109.5	C6—C5—H5A	119.8
H2—O1W—H3	109.5	C7—C6—C5	120.1 (2)
Zn1—O1W—H3'	109.5	C7—C6—C8	122.4 (2)
H2—O1W—H3'	109.5	C5—C6—C8	117.58 (19)
H3—O1W—H3'	109.5	C2—C7—C6	119.8 (2)
H4—O2W—H5	108.9	C2—C7—H7A	120.1
H4—O2W—H5'	108.8	C6—C7—H7A	120.1
H5—O2W—H5'	116.7	O4—C8—O3	121.9 (2)
C4—N1—Zn1^iv	122.60 (14)	O4—C8—C6	123.1 (2)
C4—N1—H6	106.7	O3—C8—C6	114.96 (19)

O1W—Zn1—O1—C1	−150.9 (2)	Zn1^iv—N1—C4—C5	72.4 (2)
O1Wⁱ—Zn1—O1—C1	29.1 (2)	Zn1^iv—N1—C4—C3	−107.5 (2)
N1ⁱⁱ—Zn1—O1—C1	116.2 (2)	C3—C4—C5—C6	−0.8 (3)
N1ⁱⁱⁱ—Zn1—O1—C1	−63.8 (2)	N1—C4—C5—C6	179.3 (2)
Zn1—O1—C1—O2	−3.4 (4)	C4—C5—C6—C7	−0.6 (3)
Zn1—O1—C1—C2	175.68 (15)	C4—C5—C6—C8	179.3 (2)
O2—C1—C2—C7	11.5 (4)	C3—C2—C7—C6	−0.7 (3)
O1—C1—C2—C7	−167.7 (2)	C1—C2—C7—C6	−179.2 (2)
O2—C1—C2—C3	−167.1 (3)	C5—C6—C7—C2	1.3 (3)
O1—C1—C2—C3	13.8 (3)	C8—C6—C7—C2	−178.5 (2)
C7—C2—C3—C4	−0.7 (3)	C7—C6—C8—O4	−179.2 (2)
C1—C2—C3—C4	177.9 (2)	C5—C6—C8—O4	1.0 (3)
C2—C3—C4—C5	1.4 (3)	C7—C6—C8—O3	1.0 (3)
C2—C3—C4—N1	−178.7 (2)	C5—C6—C8—O3	−178.8 (2)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H1···O2W^v	0.84	1.84	2.675 (3)	172
O1W—H2···O2ⁱ	0.84	1.97	2.695 (3)	143
O2W—H4···O2	0.84	1.79	2.619 (3)	170
O2W—H5···O2W^vi	0.84	2.03	2.869 (5)	171
O2W—H5′···O1ⁱⁱⁱ	0.84	2.31	3.106 (3)	158
O2W—H5′···O1Wⁱⁱⁱ	0.84	2.35	2.910 (3)	125
N1—H6···O4^vii	0.88	2.14	3.013 (3)	172
N1—H7···O4ⁱⁱ	0.88	2.21	3.059 (2)	161

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H1⋯O2W ⁱ	0.84	1.84	2.675 (3)	172
O1W—H2⋯O2ⁱⁱ	0.84	1.97	2.695 (3)	143
O2W—H4⋯O2	0.84	1.79	2.619 (3)	170
O2W—H5⋯O2W ⁱⁱⁱ	0.84	2.03	2.869 (5)	171
O2W—H5′⋯O1^iv	0.84	2.31	3.106 (3)	158
O2W—H5′⋯O1W ^iv	0.84	2.35	2.910 (3)	125
N1—H6⋯O4^v	0.88	2.14	3.013 (3)	172
N1—H7⋯O4^vi	0.88	2.21	3.059 (2)	161

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

2 in total

1. A short history of SHELX.

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

2. Hydrothermal synthesis, structures, and magnetic properties of three novel 5-aminoisophthalic acid ligand bridged transition metal cation polymers.

Authors: Chuan-De Wu; Can-Zhong Lu; Wen-Bin Yang; Hong-Hui Zhuang; Jin-Shun Huang
Journal: Inorg Chem Date: 2002-06-17 Impact factor: 5.165

2 in total