Literature DB >> 21581192

catena-Poly[[di-μ-chlorido-bis-{[6-methoxy-2-(4-methyl-phenyl-iminio-methyl)phenolato-κO,O']cadmium(II)}]-di-μ(2)-thio-cyanato-κN:S;κS:N].

Hua-Qiong Li¹, Hui-Duo Xian, Jian-Feng Liu, Guo-Liang Zhao.

Abstract

The asymmetric unit of the title compound, [Cd(2)Cl(2)(NCS)(2)(C(15)H(15)NO(2))(2)](n), contains the Schiff base 2-[(4-methyl-phenyl-imino)meth-yl]-6-methoxy-phenol (HL) ligand, one thio-cyanate and one chloride ligand coordinated to a cadmium centre. The cadmium centers are linked to each other via two thio-cyanate and two chloride bridges alternately, resulting in centrosymmetric zigzag chains running parallel to the a axis. The Cd(II) coordination environment contains two Cl atoms, one thio-cyanate (SCN) S atom, one isothio-cyanate (NCS) N atom and two O atoms from the HL ligand. The Schiff base ligand is in the trans conformation.

Entities: CellLine Chemical Disease Gene

Year: 2008 PMID： 21581192 PMCID： PMC2959993 DOI： 10.1107/S1600536808038099

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

Related literature

For related literature regarding Schiff bases and their complexes, see: Mondal et al. (1999 ▶); Sen et al. (2006 ▶); Yi et al. (2004 ▶); Yu et al. (2007 ▶); Zhao et al. (2007 ▶); Zhou & Zhao (2007 ▶). For related structures, see: Ding et al. (2006 ▶); Suh et al. (2007 ▶).

Experimental

Crystal data

[Cd2Cl2(NCS)2(C15H15NO2)2] M = 447.23 Triclinic, a = 9.0485 (2) Å b = 9.7321 (2) Å c = 10.6676 (3) Å α = 71.518 (2)° β = 77.444 (2)° γ = 80.732 (2)° V = 865.32 (4) Å3 Z = 2 Mo Kα radiation μ = 1.55 mm−1 T = 296 (2) K 0.27 × 0.11 × 0.08 mm

Data collection

Bruker APEXII diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.82, T max = 0.882 13032 measured reflections 3940 independent reflections 3225 reflections with I > 2σ(I) R int = 0.029

Refinement

R[F 2 > 2σ(F 2)] = 0.032 wR(F 2) = 0.081 S = 1.01 3940 reflections 208 parameters H-atom parameters constrained Δρmax = 0.54 e Å−3 Δρmin = −0.52 e Å−3 Data collection: APEX2 (Bruker, 2006 ▶); cell refinement: SAINT (Bruker, 2006 ▶); 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: SHELXL97. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808038099/ez2146sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808038099/ez2146Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Cd₂Cl₂(NCS)₂(C₁₅H₁₅NO₂)₂]	Z = 2
M_r = 447.23	F₀₀₀ = 444
Triclinic, P1	D_x = 1.717 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation λ = 0.71073 Å
a = 9.0485 (2) Å	Cell parameters from 4749 reflections
b = 9.7321 (2) Å	θ = 2.1–27.4º
c = 10.6676 (3) Å	µ = 1.55 mm⁻¹
α = 71.518 (2)º	T = 296 (2) K
β = 77.444 (2)º	Block, red
γ = 80.732 (2)º	0.27 × 0.11 × 0.08 mm
V = 865.32 (4) Å³

Bruker APEXII diffractometer	3940 independent reflections
Radiation source: fine-focus sealed tube	3225 reflections with I > 2σ(I)
Monochromator: graphite	R_int = 0.029
T = 296(2) K	θ_max = 27.4º
ω scans	θ_min = 2.1º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)	h = −11→11
T_min = 0.82, T_max = 0.882	k = −12→12
13032 measured reflections	l = −13→13

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)] = 0.032	H-atom parameters constrained
wR(F²) = 0.081	w = 1/[σ²(F_o²) + (0.0453P)² + 0.1806P] where P = (F_o² + 2F_c²)/3
S = 1.01	(Δ/σ)_max < 0.001
3940 reflections	Δρ_max = 0.54 e Å⁻³
208 parameters	Δρ_min = −0.52 e Å⁻³
Primary atom site location: structure-invariant direct methods	Extinction correction: none

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
Cd1	0.16960 (2)	0.06238 (2)	0.54427 (2)	0.04022 (10)
Cl1	0.05869 (9)	0.10606 (10)	0.33628 (8)	0.0508 (2)
O1	−0.0129 (2)	0.2707 (2)	0.5970 (2)	0.0479 (5)
N1	0.2771 (3)	−0.0247 (3)	0.9681 (2)	0.0380 (5)
H1D	0.2767	−0.0267	0.8882	0.046*
C1	0.6806 (5)	−0.4746 (4)	1.2474 (5)	0.0786 (13)
H1A	0.6777	−0.4648	1.3347	0.118*
H1B	0.7825	−0.4685	1.1977	0.118*
H1C	0.6482	−0.5672	1.2569	0.118*
S1	0.64223 (10)	−0.27344 (10)	0.58734 (12)	0.0690 (3)
O2	0.1735 (2)	0.0798 (2)	0.7460 (2)	0.0448 (5)
C2	0.5752 (4)	−0.3537 (4)	1.1732 (4)	0.0549 (9)
N2	0.3597 (3)	−0.1180 (3)	0.5586 (3)	0.0555 (7)
C3	0.4944 (4)	−0.2504 (4)	1.2320 (4)	0.0538 (9)
H3A	0.5066	−0.2555	1.3178	0.065*
C4	0.3960 (4)	−0.1396 (4)	1.1679 (3)	0.0472 (8)
H4A	0.3428	−0.0712	1.2097	0.057*
C5	0.3782 (3)	−0.1326 (3)	1.0407 (3)	0.0385 (7)
C6	0.4605 (4)	−0.2321 (4)	0.9780 (4)	0.0541 (9)
H6A	0.4510	−0.2254	0.8911	0.065*
C7	0.5572 (4)	−0.3416 (4)	1.0452 (4)	0.0645 (10)
H7A	0.6116	−0.4091	1.0029	0.077*
C8	0.1852 (3)	0.0767 (3)	1.0080 (3)	0.0405 (7)
H8A	0.1835	0.0824	1.0937	0.049*
C9	0.0880 (3)	0.1784 (3)	0.9282 (3)	0.0373 (6)
C10	−0.0067 (4)	0.2857 (4)	0.9810 (3)	0.0543 (9)
H10A	−0.0047	0.2876	1.0673	0.065*
C11	−0.0998 (4)	0.3851 (4)	0.9058 (4)	0.0604 (10)
H11A	−0.1604	0.4560	0.9404	0.073*
C12	−0.1062 (3)	0.3829 (3)	0.7766 (3)	0.0464 (8)
H12A	−0.1718	0.4514	0.7267	0.056*
C13	−0.0171 (3)	0.2811 (3)	0.7232 (3)	0.0369 (6)
C14	0.0858 (3)	0.1752 (3)	0.7971 (3)	0.0334 (6)
C15	−0.1276 (4)	0.3549 (4)	0.5233 (3)	0.0516 (8)
H15A	−0.1801	0.4271	0.5654	0.077*
H15B	−0.1987	0.2921	0.5221	0.077*
H15C	−0.0812	0.4019	0.4330	0.077*
C16	0.4777 (4)	−0.1803 (3)	0.5696 (3)	0.0441 (7)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.03390 (14)	0.05451 (16)	0.03464 (15)	0.00929 (10)	−0.01210 (9)	−0.01906 (11)
Cl1	0.0445 (4)	0.0800 (6)	0.0284 (4)	−0.0077 (4)	−0.0083 (3)	−0.0144 (4)
O1	0.0485 (12)	0.0591 (13)	0.0372 (12)	0.0207 (10)	−0.0209 (10)	−0.0196 (10)
N1	0.0383 (13)	0.0445 (13)	0.0308 (14)	0.0031 (11)	−0.0115 (10)	−0.0104 (11)
C1	0.056 (2)	0.062 (2)	0.100 (3)	−0.0001 (19)	−0.035 (2)	0.012 (2)
S1	0.0392 (5)	0.0516 (5)	0.0980 (8)	0.0070 (4)	−0.0190 (5)	0.0023 (5)
O2	0.0492 (13)	0.0502 (12)	0.0392 (12)	0.0204 (10)	−0.0211 (10)	−0.0226 (10)
C2	0.0390 (18)	0.0470 (19)	0.068 (3)	−0.0045 (15)	−0.0191 (17)	0.0037 (17)
N2	0.0361 (15)	0.0505 (16)	0.076 (2)	0.0055 (13)	−0.0112 (14)	−0.0172 (15)
C3	0.052 (2)	0.063 (2)	0.040 (2)	−0.0058 (17)	−0.0179 (16)	0.0018 (16)
C4	0.0464 (18)	0.0571 (19)	0.0355 (18)	0.0009 (15)	−0.0106 (14)	−0.0105 (15)
C5	0.0341 (15)	0.0419 (16)	0.0375 (17)	−0.0010 (12)	−0.0119 (13)	−0.0066 (13)
C6	0.052 (2)	0.061 (2)	0.051 (2)	0.0156 (16)	−0.0234 (17)	−0.0204 (17)
C7	0.057 (2)	0.062 (2)	0.079 (3)	0.0174 (18)	−0.025 (2)	−0.030 (2)
C8	0.0395 (17)	0.0526 (18)	0.0284 (16)	−0.0012 (14)	−0.0054 (13)	−0.0125 (13)
C9	0.0336 (15)	0.0459 (16)	0.0314 (16)	0.0038 (13)	−0.0064 (12)	−0.0132 (13)
C10	0.056 (2)	0.069 (2)	0.0392 (19)	0.0146 (17)	−0.0108 (16)	−0.0249 (17)
C11	0.058 (2)	0.069 (2)	0.058 (2)	0.0254 (18)	−0.0117 (18)	−0.0367 (19)
C12	0.0386 (17)	0.0500 (18)	0.0453 (19)	0.0127 (14)	−0.0117 (14)	−0.0123 (15)
C13	0.0337 (15)	0.0425 (16)	0.0338 (16)	0.0011 (12)	−0.0088 (12)	−0.0106 (13)
C14	0.0290 (14)	0.0377 (15)	0.0323 (16)	0.0005 (11)	−0.0056 (11)	−0.0104 (12)
C15	0.0463 (19)	0.062 (2)	0.044 (2)	0.0107 (16)	−0.0222 (15)	−0.0110 (16)
C16	0.0392 (17)	0.0434 (17)	0.048 (2)	−0.0021 (14)	−0.0039 (14)	−0.0144 (14)

Cd1—O2	2.2191 (19)	C3—C4	1.383 (4)
Cd1—N2	2.244 (3)	C3—H3A	0.9300
Cd1—Cl1	2.5187 (8)	C4—C5	1.381 (4)
Cd1—O1	2.529 (2)	C4—H4A	0.9300
Cd1—Cl1ⁱ	2.6833 (9)	C5—C6	1.379 (4)
Cd1—S1ⁱⁱ	2.7107 (10)	C6—C7	1.380 (5)
Cl1—Cd1ⁱ	2.6833 (9)	C6—H6A	0.9300
O1—C13	1.373 (3)	C7—H7A	0.9300
O1—C15	1.428 (4)	C8—C9	1.410 (4)
N1—C8	1.303 (4)	C8—H8A	0.9300
N1—C5	1.421 (4)	C9—C14	1.413 (4)
N1—H1D	0.8600	C9—C10	1.420 (4)
C1—C2	1.515 (5)	C10—C11	1.352 (5)
C1—H1A	0.9600	C10—H10A	0.9300
C1—H1B	0.9600	C11—C12	1.400 (5)
C1—H1C	0.9600	C11—H11A	0.9300
S1—C16	1.629 (3)	C12—C13	1.362 (4)
S1—Cd1ⁱⁱ	2.7107 (10)	C12—H12A	0.9300
O2—C14	1.299 (3)	C13—C14	1.430 (4)
C2—C7	1.376 (5)	C15—H15A	0.9600
C2—C3	1.379 (5)	C15—H15B	0.9600
N2—C16	1.150 (4)	C15—H15C	0.9600

O2—Cd1—N2	92.93 (9)	C3—C4—H4A	120.7
O2—Cd1—Cl1	155.30 (6)	C6—C5—C4	120.3 (3)
N2—Cd1—Cl1	110.91 (8)	C6—C5—N1	117.0 (3)
O2—Cd1—O1	67.95 (7)	C4—C5—N1	122.7 (3)
N2—Cd1—O1	160.37 (10)	C5—C6—C7	119.4 (3)
Cl1—Cd1—O1	88.62 (5)	C5—C6—H6A	120.3
O2—Cd1—Cl1ⁱ	86.93 (6)	C7—C6—H6A	120.3
N2—Cd1—Cl1ⁱ	96.98 (7)	C2—C7—C6	121.8 (3)
Cl1—Cd1—Cl1ⁱ	83.92 (3)	C2—C7—H7A	119.1
O1—Cd1—Cl1ⁱ	86.77 (6)	C6—C7—H7A	119.1
O2—Cd1—S1ⁱⁱ	94.23 (6)	N1—C8—C9	123.5 (3)
N2—Cd1—S1ⁱⁱ	93.69 (8)	N1—C8—H8A	118.3
Cl1—Cd1—S1ⁱⁱ	90.71 (3)	C9—C8—H8A	118.3
O1—Cd1—S1ⁱⁱ	83.73 (6)	C8—C9—C14	120.8 (2)
Cl1ⁱ—Cd1—S1ⁱⁱ	169.20 (3)	C8—C9—C10	118.9 (3)
Cd1—Cl1—Cd1ⁱ	96.08 (3)	C14—C9—C10	120.3 (3)
C13—O1—C15	118.3 (2)	C11—C10—C9	119.9 (3)
C13—O1—Cd1	113.42 (16)	C11—C10—H10A	120.0
C15—O1—Cd1	126.96 (18)	C9—C10—H10A	120.0
C8—N1—C5	127.9 (3)	C10—C11—C12	121.0 (3)
C8—N1—H1D	116.1	C10—C11—H11A	119.5
C5—N1—H1D	116.1	C12—C11—H11A	119.5
C2—C1—H1A	109.5	C13—C12—C11	120.5 (3)
C2—C1—H1B	109.5	C13—C12—H12A	119.7
H1A—C1—H1B	109.5	C11—C12—H12A	119.7
C2—C1—H1C	109.5	C12—C13—O1	125.2 (3)
H1A—C1—H1C	109.5	C12—C13—C14	121.0 (3)
H1B—C1—H1C	109.5	O1—C13—C14	113.9 (2)
C16—S1—Cd1ⁱⁱ	100.35 (12)	O2—C14—C9	121.3 (3)
C14—O2—Cd1	123.29 (18)	O2—C14—C13	121.4 (3)
C7—C2—C3	117.5 (3)	C9—C14—C13	117.3 (2)
C7—C2—C1	121.8 (4)	O1—C15—H15A	109.5
C3—C2—C1	120.7 (4)	O1—C15—H15B	109.5
C16—N2—Cd1	160.6 (3)	H15A—C15—H15B	109.5
C2—C3—C4	122.3 (3)	O1—C15—H15C	109.5
C2—C3—H3A	118.8	H15A—C15—H15C	109.5
C4—C3—H3A	118.8	H15B—C15—H15C	109.5
C5—C4—C3	118.6 (3)	N2—C16—S1	178.1 (3)
C5—C4—H4A	120.7

O2—Cd1—Cl1—Cd1ⁱ	−68.87 (15)	C8—N1—C5—C6	177.7 (3)
N2—Cd1—Cl1—Cd1ⁱ	95.17 (8)	C8—N1—C5—C4	−2.6 (5)
O1—Cd1—Cl1—Cd1ⁱ	−86.90 (6)	C4—C5—C6—C7	2.1 (5)
Cl1ⁱ—Cd1—Cl1—Cd1ⁱ	0.0	N1—C5—C6—C7	−178.2 (3)
S1ⁱⁱ—Cd1—Cl1—Cd1ⁱ	−170.61 (3)	C3—C2—C7—C6	−0.9 (6)
O2—Cd1—O1—C13	−2.23 (18)	C1—C2—C7—C6	179.6 (3)
N2—Cd1—O1—C13	−16.0 (4)	C5—C6—C7—C2	−0.7 (6)
Cl1—Cd1—O1—C13	169.75 (19)	C5—N1—C8—C9	−179.5 (3)
Cl1ⁱ—Cd1—O1—C13	85.76 (19)	N1—C8—C9—C14	−0.1 (5)
S1ⁱⁱ—Cd1—O1—C13	−99.38 (19)	N1—C8—C9—C10	−179.3 (3)
O2—Cd1—O1—C15	−169.0 (3)	C8—C9—C10—C11	179.4 (3)
N2—Cd1—O1—C15	177.2 (3)	C14—C9—C10—C11	0.2 (5)
Cl1—Cd1—O1—C15	3.0 (2)	C9—C10—C11—C12	1.0 (6)
Cl1ⁱ—Cd1—O1—C15	−81.0 (2)	C10—C11—C12—C13	−0.8 (6)
S1ⁱⁱ—Cd1—O1—C15	93.8 (2)	C11—C12—C13—O1	−178.9 (3)
N2—Cd1—O2—C14	177.8 (2)	C11—C12—C13—C14	−0.6 (5)
Cl1—Cd1—O2—C14	−17.1 (3)	C15—O1—C13—C12	−11.6 (5)
O1—Cd1—O2—C14	2.4 (2)	Cd1—O1—C13—C12	−179.6 (3)
Cl1ⁱ—Cd1—O2—C14	−85.3 (2)	C15—O1—C13—C14	169.9 (3)
S1ⁱⁱ—Cd1—O2—C14	83.9 (2)	Cd1—O1—C13—C14	1.9 (3)
O2—Cd1—N2—C16	−59.5 (9)	Cd1—O2—C14—C9	177.4 (2)
Cl1—Cd1—N2—C16	127.1 (9)	Cd1—O2—C14—C13	−2.4 (4)
O1—Cd1—N2—C16	−46.8 (10)	C8—C9—C14—O2	−0.5 (4)
Cl1ⁱ—Cd1—N2—C16	−146.8 (9)	C10—C9—C14—O2	178.7 (3)
S1ⁱⁱ—Cd1—N2—C16	34.9 (9)	C8—C9—C14—C13	179.3 (3)
C7—C2—C3—C4	1.3 (5)	C10—C9—C14—C13	−1.4 (4)
C1—C2—C3—C4	−179.2 (3)	C12—C13—C14—O2	−178.5 (3)
C2—C3—C4—C5	0.1 (5)	O1—C13—C14—O2	0.0 (4)
C3—C4—C5—C6	−1.8 (5)	C12—C13—C14—C9	1.7 (4)
C3—C4—C5—N1	178.5 (3)	O1—C13—C14—C9	−179.8 (3)

4 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. Ligating properties of a potentially tetradentate Schiff base [(CH3)2NCH2CH2N=CHC6H3(OH)(OMe)] with zinc(II), cadmium(II), cobalt(II), cobalt(III) and manganese(III) ions: synthesis and structural studies.

Authors: Soma Sen; Pritha Talukder; Subrata K Dey; Samiran Mitra; Georgina Rosair; David L Hughes; Glenn P A Yap; Guillaume Pilet; V Gramlich; T Matsushita
Journal: Dalton Trans Date: 2006-01-06 Impact factor: 4.390

3. Synthesis of a series of 4-pyridyl-1,2,4-triazole-containing cadmium(II) luminescent complexes.

Authors: Bin Ding; Long Yi; Ying Wang; Peng Cheng; Dai-Zheng Liao; Shi-Ping Yan; Zong-Hui Jiang; Hai-Bin Song; Hong-Gen Wang
Journal: Dalton Trans Date: 2005-11-14 Impact factor: 4.390

4. Novel triazole-bridged cadmium coordination polymers varying from zero- to three-dimensionality.

Authors: Long Yi; Bin Ding; Bin Zhao; Peng Cheng; Dai-Zheng Liao; Shi-Ping Yan; Zong-Hui Jiang
Journal: Inorg Chem Date: 2004-01-12 Impact factor: 5.165

4 in total

17 in total

1. Tetra-kis(μ(2)-3,4-dimethoxy-phenyl-acetato)-κO,O':O';κO:O:O';κO:O';κO:O'-bis-[(3,4-dimethoxy-phenyl-acetato-κO,O')(1,10-phenanthroline-κN,N)thulium(III)].

Authors: Jia-Lu Liu; Hua-Qiong Li; Guo-Liang Zhao
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2009-12-04

2. Bis[6-meth-oxy-2-[(4-methyl-phen-yl)iminiometh-yl]phenolate-κO]tris-(nitrato-κO,O')ytterbium(III) monohydrate.

Authors: Jian-Feng Liu; Jia-Lu Liu; Guo-Liang Zhao
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2009-10-17

3. (Methanol-κO)bis-{2-meth-oxy-6-[(4-methyl-phen-yl)iminiometh-yl]phenolato-κO,O'}tris-(nitrato-κO,O')lanthanum(III).

Authors: Jia-Lu Liu; Hai-Ting Cai; Guo-Liang Zhao
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2010-09-30

4. Tris{2-meth-oxy-6-[(4-methyl-phen-yl)iminiometh-yl]phenolate-κO,O'}tris-(thio-cyanato-κN)europium(III).

Authors: Jian-Feng Liu; Jia-Lu Liu; Guo-Liang Zhao
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2009-11-21

5. Tris{2-meth-oxy-6-[(4-methyl-phen-yl)iminiometh-yl]phenolato-κO,O'}tris-(thio-cyanato-κN)praseodymium(III) monohydrate.

Authors: Jian-Feng Liu; Jia-Lu Liu; Guo-Liang Zhao
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2009-10-03

10. Tetra-kis[μ-2-(3,4-dimeth-oxy-phen-yl)acetato]-κO:O';κO,O':O;κO:O,O'-bis-{[2-(3,4-dimeth-oxy-phen-yl)acetato-κO,O'](1,10-phenanthroline-κN,N')samarium(III)}.

Authors: Jia-Lu Liu; Hua-Qiong Li; Guo-Liang Zhao
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2010-10-09