Literature DB >> 21201341

Tetra-aqua-bis(2-oxo-1,2-dihydro-quinoline-4-carboxyl-ato-κO)nickel(II).

Gang Yuan¹, Jun-Sheng Qin, Zhong-Min Su, Kui-Zhan Shao, Yao-Mei Fu.

Abstract

In the title compound, [Ni(C(10)H(6)NO(3))(2)(H(2)O)(4)], the central Ni(II) atom is located on an inversion center and coordinated in a slightly distorted octa-hedral geometry by two O atoms from two 2-oxo-1,2-dihydro-quinoline-4-carboxyl-ate ligands and four water mol-ecules, all of which act as monodentate ligands. The crystal structure features an extensive network of inter-molecular hydrogen-bonding inter-actions (O-H⋯O and N-H⋯O) and offset face-to-face π-π stacking inter-actions [centroid-centroid distances = 3.525 (3) and 3.281 (5) Å].

Entities: CellLine Chemical Disease Species

Year: 2008 PMID： 21201341 PMCID： PMC2960272 DOI： 10.1107/S1600536807065671

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

Related literature

For related literature, see: Bai et al. (2007 ▶); Bu et al. (2005 ▶); Liu (2007 ▶); Pang et al. (2007 ▶); Wu et al. (2007 ▶); Xiong et al. (2000 ▶); Zhang et al. (2007 ▶).

Experimental

Crystal data

[Ni(C10H6NO3)2(H2O)4] M = 507.07 Triclinic, a = 7.105 (5) Å b = 8.507 (5) Å c = 9.216 (5) Å α = 108.723 (5)° β = 108.396 (5)° γ = 90.840 (5)° V = 496.4 (5) Å3 Z = 1 Mo Kα radiation μ = 1.04 mm−1 T = 293 (2) K 0.5 × 0.4 × 0.3 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.601, T max = 0.721 3041 measured reflections 2250 independent reflections 2064 reflections with I > 2σ(I) R int = 0.015

Refinement

R[F 2 > 2σ(F 2)] = 0.034 wR(F 2) = 0.121 S = 1.02 2250 reflections 151 parameters H-atom parameters constrained Δρmax = 0.40 e Å−3 Δρmin = −0.57 e Å−3 Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT (Bruker, 2004 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: SHELXTL-Plus (Siemens, 1990 ▶); software used to prepare material for publication: SHELXTL-Plus. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536807065671/hy2104sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536807065671/hy2104Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Ni(C₁₀H₆NO₃)₂(H₂O)₄]	Z = 1
M_r = 507.07	F₀₀₀ = 262
Triclinic, P1	D_x = 1.696 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation λ = 0.71069 Å
a = 7.105 (5) Å	Cell parameters from 2250 reflections
b = 8.507 (5) Å	θ = 1.3–26.0º
c = 9.216 (5) Å	µ = 1.04 mm⁻¹
α = 108.723 (5)º	T = 293 (2) K
β = 108.396 (5)º	Block, green
γ = 90.840 (5)º	0.5 × 0.4 × 0.3 mm
V = 496.4 (5) Å³

Bruker SMART APEXII CCD area-detector diffractometer	2250 independent reflections
Radiation source: fine-focus sealed tube	2064 reflections with I > 2σ(I)
Monochromator: graphite	R_int = 0.015
T = 293(2) K	θ_max = 28.3º
φ and ω scans	θ_min = 2.5º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)	h = −9→9
T_min = 0.601, T_max = 0.721	k = −8→11
3041 measured reflections	l = −12→7

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.034	H-atom parameters constrained
wR(F²) = 0.121	w = 1/[σ²(F_o²) + (0.0726P)² + 0.4272P] where P = (F_o² + 2F_c²)/3
S = 1.02	(Δ/σ)_max = 0.001
2250 reflections	Δρ_max = 0.40 e Å⁻³
151 parameters	Δρ_min = −0.57 e Å⁻³
Primary atom site location: structure-invariant direct methods	Extinction correction: none

	x	y	z	U_iso*/U_eq
Ni1	0.5000	1.0000	0.5000	0.02024 (16)
C1	0.6765 (4)	0.6477 (3)	−0.1760 (3)	0.0260 (5)
C2	0.6843 (4)	0.7807 (3)	−0.0285 (3)	0.0276 (6)
H2A	0.6609	0.8868	−0.0322	0.033*
C3	0.7249 (4)	0.7538 (3)	0.1145 (3)	0.0234 (5)
C4	0.7688 (4)	0.5932 (3)	0.1253 (3)	0.0241 (5)
C5	0.8169 (4)	0.5563 (4)	0.2709 (3)	0.0316 (6)
H5A	0.8186	0.6386	0.3666	0.038*
C6	0.8610 (5)	0.4004 (4)	0.2722 (4)	0.0363 (7)
H6A	0.8936	0.3779	0.3689	0.044*
C7	0.8573 (4)	0.2754 (4)	0.1295 (4)	0.0342 (6)
H7A	0.8882	0.1702	0.1320	0.041*
C8	0.8084 (4)	0.3057 (3)	−0.0152 (3)	0.0289 (6)
H8A	0.8052	0.2214	−0.1102	0.035*
C9	0.7636 (4)	0.4648 (3)	−0.0176 (3)	0.0233 (5)
C10	0.7168 (4)	0.8914 (3)	0.2641 (3)	0.0244 (5)
N1	0.7143 (3)	0.4972 (3)	−0.1615 (3)	0.0250 (5)
H1A	0.7072	0.4158	−0.2483	0.030*
O1	0.5726 (3)	0.8651 (3)	0.3072 (2)	0.0319 (5)
O2	0.8452 (3)	1.0169 (3)	0.3306 (3)	0.0337 (5)
O3	0.6381 (3)	0.6659 (3)	−0.3117 (2)	0.0342 (5)
O1W	0.2409 (3)	1.0448 (3)	0.3421 (3)	0.0331 (5)
H1	0.1249	1.0296	0.3471	0.050*
H2	0.2548	1.1369	0.3265	0.050*
O2W	0.3413 (3)	0.7783 (2)	0.4826 (2)	0.0274 (4)
H3	0.2601	0.8200	0.5308	0.041*
H4	0.4010	0.7217	0.5403	0.041*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.0210 (3)	0.0197 (2)	0.0201 (2)	0.00347 (17)	0.01005 (17)	0.00379 (17)
C1	0.0249 (13)	0.0306 (14)	0.0230 (12)	0.0038 (10)	0.0085 (10)	0.0095 (11)
C2	0.0327 (14)	0.0266 (13)	0.0272 (13)	0.0085 (11)	0.0138 (11)	0.0103 (11)
C3	0.0207 (12)	0.0268 (13)	0.0229 (12)	0.0038 (10)	0.0106 (10)	0.0056 (10)
C4	0.0230 (12)	0.0274 (13)	0.0232 (12)	0.0039 (10)	0.0097 (10)	0.0085 (10)
C5	0.0353 (15)	0.0379 (16)	0.0218 (12)	0.0064 (12)	0.0103 (11)	0.0100 (11)
C6	0.0383 (16)	0.0423 (17)	0.0331 (15)	0.0042 (13)	0.0087 (12)	0.0226 (13)
C7	0.0323 (15)	0.0287 (14)	0.0425 (16)	0.0034 (11)	0.0071 (12)	0.0189 (13)
C8	0.0274 (13)	0.0241 (13)	0.0306 (13)	0.0029 (10)	0.0074 (11)	0.0059 (11)
C9	0.0196 (12)	0.0261 (13)	0.0237 (11)	0.0026 (10)	0.0070 (9)	0.0081 (10)
C10	0.0254 (13)	0.0264 (13)	0.0230 (12)	0.0083 (10)	0.0117 (10)	0.0070 (10)
N1	0.0294 (12)	0.0237 (11)	0.0191 (10)	0.0037 (9)	0.0089 (9)	0.0031 (8)
O1	0.0308 (10)	0.0314 (11)	0.0293 (10)	−0.0013 (8)	0.0176 (8)	−0.0020 (8)
O2	0.0316 (11)	0.0295 (11)	0.0388 (11)	−0.0002 (8)	0.0197 (9)	0.0026 (9)
O3	0.0412 (12)	0.0395 (12)	0.0251 (9)	0.0082 (9)	0.0111 (9)	0.0154 (9)
O1W	0.0257 (10)	0.0366 (11)	0.0390 (11)	0.0058 (8)	0.0100 (8)	0.0165 (9)
O2W	0.0304 (10)	0.0278 (10)	0.0263 (9)	0.0055 (8)	0.0127 (8)	0.0094 (8)

Ni1—O1ⁱ	2.007 (2)	C5—H5A	0.9300
Ni1—O1	2.007 (2)	C6—C7	1.393 (5)
Ni1—O1W	2.083 (2)	C6—H6A	0.9300
Ni1—O1Wⁱ	2.083 (2)	C7—C8	1.377 (4)
Ni1—O2W	2.117 (2)	C7—H7A	0.9300
Ni1—O2Wⁱ	2.117 (2)	C8—C9	1.401 (4)
C1—O3	1.254 (3)	C8—H8A	0.9300
C1—N1	1.351 (4)	C9—N1	1.379 (3)
C1—C2	1.447 (4)	C10—O2	1.244 (3)
C2—C3	1.352 (4)	C10—O1	1.250 (3)
C2—H2A	0.9300	N1—H1A	0.8600
C3—C4	1.433 (4)	O1W—H1	0.8501
C3—C10	1.514 (3)	O1W—H2	0.8500
C4—C9	1.405 (4)	O2W—H3	0.8500
C4—C5	1.414 (4)	O2W—H4	0.8499
C5—C6	1.371 (4)

O1ⁱ—Ni1—O1	180.0	C6—C5—H5A	119.7
O1ⁱ—Ni1—O1W	90.69 (10)	C4—C5—H5A	119.7
O1—Ni1—O1W	89.31 (10)	C5—C6—C7	120.4 (3)
O1ⁱ—Ni1—O1Wⁱ	89.31 (9)	C5—C6—H6A	119.8
O1—Ni1—O1Wⁱ	90.69 (10)	C7—C6—H6A	119.8
O1W—Ni1—O1Wⁱ	180.000 (1)	C8—C7—C6	120.8 (3)
O1ⁱ—Ni1—O2W	91.65 (8)	C8—C7—H7A	119.6
O1—Ni1—O2W	88.35 (8)	C6—C7—H7A	119.6
O1W—Ni1—O2W	89.05 (9)	C7—C8—C9	119.2 (3)
O1Wⁱ—Ni1—O2W	90.95 (9)	C7—C8—H8A	120.4
O1ⁱ—Ni1—O2Wⁱ	88.35 (8)	C9—C8—H8A	120.4
O1—Ni1—O2Wⁱ	91.65 (8)	N1—C9—C8	120.0 (2)
O1W—Ni1—O2Wⁱ	90.95 (9)	N1—C9—C4	119.1 (2)
O1Wⁱ—Ni1—O2Wⁱ	89.05 (9)	C8—C9—C4	120.9 (2)
O2W—Ni1—O2Wⁱ	180.00 (10)	O2—C10—O1	126.3 (2)
O3—C1—N1	120.0 (2)	O2—C10—C3	119.9 (2)
O3—C1—C2	123.8 (3)	O1—C10—C3	113.8 (2)
N1—C1—C2	116.2 (2)	C1—N1—C9	124.7 (2)
C3—C2—C1	121.4 (3)	C1—N1—H1A	117.6
C3—C2—H2A	119.3	C9—N1—H1A	117.6
C1—C2—H2A	119.3	C10—O1—Ni1	129.97 (18)
C2—C3—C4	120.6 (2)	Ni1—O1W—H1	123.7
C2—C3—C10	120.3 (2)	Ni1—O1W—H2	113.0
C4—C3—C10	119.0 (2)	H1—O1W—H2	109.1
C9—C4—C5	118.1 (3)	Ni1—O2W—H3	100.1
C9—C4—C3	117.9 (2)	Ni1—O2W—H4	118.4
C5—C4—C3	124.0 (2)	H3—O2W—H4	101.2
C6—C5—C4	120.6 (3)

O3—C1—C2—C3	179.5 (3)	C5—C4—C9—C8	−1.2 (4)
N1—C1—C2—C3	−0.8 (4)	C3—C4—C9—C8	178.9 (2)
C1—C2—C3—C4	2.3 (4)	C2—C3—C10—O2	−69.5 (4)
C1—C2—C3—C10	−175.4 (2)	C4—C3—C10—O2	112.8 (3)
C2—C3—C4—C9	−1.4 (4)	C2—C3—C10—O1	109.5 (3)
C10—C3—C4—C9	176.2 (2)	C4—C3—C10—O1	−68.2 (3)
C2—C3—C4—C5	178.6 (3)	O3—C1—N1—C9	178.1 (2)
C10—C3—C4—C5	−3.7 (4)	C2—C1—N1—C9	−1.7 (4)
C9—C4—C5—C6	1.3 (4)	C8—C9—N1—C1	−177.2 (3)
C3—C4—C5—C6	−178.7 (3)	C4—C9—N1—C1	2.5 (4)
C4—C5—C6—C7	−0.6 (5)	O2—C10—O1—Ni1	−4.1 (4)
C5—C6—C7—C8	−0.3 (5)	C3—C10—O1—Ni1	176.92 (17)
C6—C7—C8—C9	0.5 (4)	O1W—Ni1—O1—C10	115.2 (3)
C7—C8—C9—N1	−180.0 (2)	O1Wⁱ—Ni1—O1—C10	−64.8 (3)
C7—C8—C9—C4	0.3 (4)	O2W—Ni1—O1—C10	−155.7 (3)
C5—C4—C9—N1	179.1 (2)	O2Wⁱ—Ni1—O1—C10	24.3 (3)
C3—C4—C9—N1	−0.9 (4)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···O2Wⁱⁱ	0.86	2.18	3.031 (3)	173
O1W—H1···O2ⁱⁱⁱ	0.85	1.94	2.783 (3)	169
O1W—H2···O3^iv	0.85	1.89	2.722 (3)	164
O2W—H3···O2ⁱ	0.85	1.90	2.709 (3)	158
O2W—H4···O3^v	0.85	1.98	2.767 (3)	154

Ni1—O1	2.007 (2)
Ni1—O1W	2.083 (2)
Ni1—O2W	2.117 (2)

O1—Ni1—O1W	89.31 (10)
O1—Ni1—O1Wⁱ	90.69 (10)
O1—Ni1—O2W	88.35 (8)
O1W—Ni1—O2W	89.05 (9)
O1Wⁱ—Ni1—O2W	90.95 (9)
O1—Ni1—O2Wⁱ	91.65 (8)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯O2Wⁱⁱ	0.86	2.18	3.031 (3)	173
O1W—H1⋯O2ⁱⁱⁱ	0.85	1.94	2.783 (3)	169
O1W—H2⋯O3^iv	0.85	1.89	2.722 (3)	164
O2W—H3⋯O2ⁱ	0.85	1.90	2.709 (3)	158
O2W—H4⋯O3^v	0.85	1.98	2.767 (3)	154

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

1 in total

1. Synthesis, structures, and magnetic properties of the copper(II), cobalt(II), and manganese(II) complexes with 9-acridinecarboxylate and 4-quinolinecarboxylate ligands.

Authors: Xian-He Bu; Ming-Liang Tong; Ya-Bo Xie; Jian-Rong Li; Ho-Chol Chang; Susumu Kitagawa; Joan Ribas
Journal: Inorg Chem Date: 2005-12-26 Impact factor: 5.165

1 in total