Literature DB >> 21580481

Poly[(dimethyl-formamide)(μ(4)-2,2'-sulfanediyldibenzoato)nickel(II)].

Abstract

The title centrosymmetric dinuclear Ni(II) complex, [Ni(C(14)H(8)O(4)S)(C(3)H(7)NO)](n), was prepared via reaction of Ni(NO(3))(2)·6H(2)O and thio-salicylic acid, with H(2)O and dimethyl-formamide (DMF) as the mixed solvent. The central Ni(II) ion is five-coordinated by five O atoms from DMF and from the carboxyl-ate groups of the organic ligand. The symmetry-related coordination polyhedra inter-link into centrosymmetric dimeric units and these, in turn, are linked into infinite chains propagating parallel to [100].

Entities: Chemical Disease Gene Species

Year: 2010 PMID： 21580481 PMCID： PMC2983770 DOI： 10.1107/S1600536810007749

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

Related literature

For high-dimensional coordination polymers, see: Li et al. (2009 ▶, 2010 ▶).

Experimental

Crystal data

[Ni(C14H8O4S)(C3H7NO)] M = 808.12 Triclinic, a = 8.5196 (2) Å b = 10.5240 (2) Å c = 11.0138 (3) Å α = 67.241 (1)° β = 79.0410 (11)° γ = 71.796 (1)° V = 862.33 (3) Å3 Z = 1 Mo Kα radiation μ = 1.27 mm−1 T = 298 K 0.30 × 0.25 × 0.19 mm

Data collection

Bruker APEXII area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 2004 ▶) T min = 0.701, T max = 0.794 11190 measured reflections 3350 independent reflections 2553 reflections with I > 2σ(I) R int = 0.035

Refinement

R[F 2 > 2σ(F 2)] = 0.036 wR(F 2) = 0.079 S = 1.01 3350 reflections 228 parameters H-atom parameters constrained Δρmax = 0.44 e Å−3 Δρmin = −0.35 e Å−3 Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT (Bruker, 2004 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP in SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810007749/bg2334sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810007749/bg2334Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Ni(C₁₄H₈O₄S)(C₃H₇NO)]	Z = 1
M_r = 808.12	F(000) = 416
Triclinic, P1	D_x = 1.556 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.5196 (2) Å	Cell parameters from 2701 reflections
b = 10.5240 (2) Å	θ = 2.4–22.3°
c = 11.0138 (3) Å	µ = 1.27 mm⁻¹
α = 67.241 (1)°	T = 298 K
β = 79.0410 (11)°	Block, green
γ = 71.796 (1)°	0.30 × 0.25 × 0.19 mm
V = 862.33 (3) Å³

Bruker APEXII area-detector diffractometer	3350 independent reflections
Radiation source: fine-focus sealed tube	2553 reflections with I > 2σ(I)
graphite	R_int = 0.035
φ and ω scan	θ_max = 26.0°, θ_min = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	h = −9→10
T_min = 0.701, T_max = 0.794	k = −12→12
11190 measured reflections	l = −13→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)] = 0.036	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.079	H-atom parameters constrained
S = 1.01	w = 1/[σ²(F_o²) + (0.0295P)² + 0.4P] where P = (F_o² + 2F_c²)/3
3350 reflections	(Δ/σ)_max = 0.001
228 parameters	Δρ_max = 0.44 e Å⁻³
0 restraints	Δρ_min = −0.34 e Å⁻³

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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
Ni1	0.37381 (4)	0.57945 (3)	0.55076 (3)	0.03249 (12)
S1	−0.02998 (9)	0.75102 (9)	0.29878 (7)	0.0481 (2)
O1	0.2572 (2)	0.5904 (2)	0.40641 (19)	0.0499 (5)
O2	0.4743 (3)	0.4593 (2)	0.3200 (2)	0.0551 (6)
O3	−0.3145 (3)	0.5998 (2)	0.33626 (19)	0.0501 (5)
O4	−0.5286 (2)	0.7322 (2)	0.4242 (2)	0.0521 (5)
O5	0.1675 (3)	0.7125 (2)	0.6255 (2)	0.0547 (6)
N1	−0.1056 (3)	0.8241 (3)	0.6247 (3)	0.0535 (7)
C1	0.3275 (4)	0.5360 (3)	0.3199 (3)	0.0417 (7)
C2	0.2315 (3)	0.5674 (3)	0.2057 (3)	0.0381 (6)
C3	0.3089 (4)	0.5029 (3)	0.1132 (3)	0.0501 (8)
H3	0.4126	0.4380	0.1281	0.060*
C4	0.2369 (4)	0.5317 (4)	0.0004 (3)	0.0561 (8)
H4	0.2922	0.4894	−0.0614	0.067*
C5	0.0810 (4)	0.6248 (3)	−0.0189 (3)	0.0553 (8)
H5	0.0308	0.6456	−0.0948	0.066*
C6	−0.0010 (4)	0.6872 (3)	0.0722 (3)	0.0494 (8)
H6	−0.1072	0.7477	0.0582	0.059*
C7	0.0723 (3)	0.6616 (3)	0.1858 (3)	0.0411 (7)
C8	−0.2076 (4)	0.8749 (3)	0.2161 (3)	0.0429 (7)
C9	−0.1898 (4)	1.0066 (3)	0.1271 (3)	0.0571 (9)
H9	−0.0855	1.0235	0.1077	0.069*
C10	−0.3225 (5)	1.1122 (4)	0.0670 (3)	0.0665 (10)
H10	−0.3077	1.1993	0.0069	0.080*
C11	−0.4766 (4)	1.0887 (3)	0.0962 (3)	0.0620 (9)
H11	−0.5668	1.1595	0.0550	0.074*
C12	−0.4984 (4)	0.9601 (3)	0.1866 (3)	0.0529 (8)
H12	−0.6039	0.9455	0.2069	0.063*
C13	−0.3648 (3)	0.8520 (3)	0.2478 (3)	0.0388 (7)
C14	−0.4029 (4)	0.7160 (3)	0.3450 (3)	0.0399 (7)
C15	0.0244 (4)	0.7207 (3)	0.6097 (3)	0.0472 (7)
H15	0.0070	0.6507	0.5859	0.057*
C16	−0.2706 (4)	0.8325 (4)	0.5980 (4)	0.0821 (12)
H16A	−0.2647	0.7545	0.5709	0.123*
H16B	−0.3115	0.9213	0.5289	0.123*
H16C	−0.3440	0.8271	0.6765	0.123*
C17	−0.0867 (4)	0.9353 (4)	0.6631 (4)	0.0730 (11)
H17A	0.0279	0.9356	0.6498	0.110*
H17B	−0.1239	0.9177	0.7546	0.110*
H17C	−0.1515	1.0264	0.6103	0.110*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.0266 (2)	0.0328 (2)	0.0312 (2)	−0.00384 (15)	−0.00182 (14)	−0.00739 (15)
S1	0.0385 (5)	0.0590 (5)	0.0440 (4)	−0.0096 (4)	−0.0055 (3)	−0.0165 (4)
O1	0.0380 (12)	0.0645 (14)	0.0418 (12)	−0.0035 (11)	−0.0075 (9)	−0.0189 (11)
O2	0.0390 (13)	0.0620 (14)	0.0583 (14)	0.0012 (11)	−0.0136 (10)	−0.0217 (11)
O3	0.0488 (13)	0.0383 (12)	0.0507 (13)	−0.0109 (10)	0.0077 (10)	−0.0083 (10)
O4	0.0458 (13)	0.0440 (12)	0.0561 (13)	−0.0135 (10)	0.0116 (11)	−0.0125 (10)
O5	0.0396 (13)	0.0615 (14)	0.0619 (14)	−0.0011 (11)	−0.0042 (11)	−0.0302 (12)
N1	0.0392 (16)	0.0548 (17)	0.0596 (17)	−0.0016 (13)	−0.0001 (13)	−0.0230 (14)
C1	0.0382 (18)	0.0402 (17)	0.0422 (17)	−0.0145 (15)	−0.0034 (14)	−0.0062 (14)
C2	0.0373 (17)	0.0401 (16)	0.0344 (15)	−0.0146 (14)	−0.0054 (12)	−0.0058 (13)
C3	0.0479 (19)	0.0488 (19)	0.0492 (19)	−0.0120 (16)	−0.0056 (15)	−0.0124 (16)
C4	0.059 (2)	0.066 (2)	0.0479 (19)	−0.0171 (19)	−0.0054 (16)	−0.0247 (17)
C5	0.064 (2)	0.061 (2)	0.0452 (18)	−0.0191 (19)	−0.0137 (16)	−0.0157 (17)
C6	0.0444 (19)	0.056 (2)	0.0467 (18)	−0.0127 (16)	−0.0133 (15)	−0.0122 (16)
C7	0.0380 (17)	0.0432 (17)	0.0398 (16)	−0.0177 (14)	−0.0025 (13)	−0.0068 (13)
C8	0.0430 (18)	0.0410 (17)	0.0387 (16)	−0.0096 (14)	−0.0039 (13)	−0.0084 (14)
C9	0.056 (2)	0.055 (2)	0.055 (2)	−0.0266 (18)	0.0023 (17)	−0.0072 (17)
C10	0.075 (3)	0.044 (2)	0.060 (2)	−0.018 (2)	−0.001 (2)	0.0035 (17)
C11	0.059 (2)	0.0440 (19)	0.057 (2)	0.0006 (17)	−0.0058 (18)	−0.0013 (16)
C12	0.0407 (19)	0.0497 (19)	0.055 (2)	−0.0071 (16)	−0.0006 (15)	−0.0090 (16)
C13	0.0368 (17)	0.0370 (16)	0.0371 (16)	−0.0094 (14)	0.0002 (13)	−0.0088 (13)
C14	0.0338 (17)	0.0419 (18)	0.0397 (16)	−0.0105 (14)	−0.0036 (13)	−0.0090 (14)
C15	0.048 (2)	0.0482 (19)	0.0381 (17)	−0.0065 (16)	0.0032 (15)	−0.0155 (15)
C16	0.045 (2)	0.111 (3)	0.092 (3)	−0.013 (2)	−0.004 (2)	−0.044 (3)
C17	0.060 (2)	0.064 (2)	0.094 (3)	−0.0011 (19)	0.003 (2)	−0.042 (2)

Ni1—O2ⁱ	1.947 (2)	C5—C6	1.373 (4)
Ni1—O4ⁱⁱ	1.9695 (19)	C5—H5	0.9300
Ni1—O3ⁱⁱⁱ	1.9751 (19)	C6—C7	1.400 (4)
Ni1—O1	1.9790 (19)	C6—H6	0.9300
Ni1—O5	2.129 (2)	C8—C9	1.389 (4)
Ni1—Ni1ⁱ	2.6374 (6)	C8—C13	1.390 (4)
S1—C7	1.781 (3)	C9—C10	1.371 (4)
S1—C8	1.786 (3)	C9—H9	0.9300
O1—C1	1.259 (3)	C10—C11	1.368 (5)
O2—C1	1.258 (3)	C10—H10	0.9300
O3—C14	1.249 (3)	C11—C12	1.379 (4)
O4—C14	1.258 (3)	C11—H11	0.9300
O5—C15	1.236 (3)	C12—C13	1.391 (4)
N1—C15	1.325 (4)	C12—H12	0.9300
N1—C17	1.450 (4)	C13—C14	1.507 (4)
N1—C16	1.460 (4)	C15—H15	0.9300
C1—C2	1.504 (4)	C16—H16A	0.9600
C2—C3	1.391 (4)	C16—H16B	0.9600
C2—C7	1.405 (4)	C16—H16C	0.9600
C3—C4	1.375 (4)	C17—H17A	0.9600
C3—H3	0.9300	C17—H17B	0.9600
C4—C5	1.379 (4)	C17—H17C	0.9600
C4—H4	0.9300

O2ⁱ—Ni1—O4ⁱⁱ	90.48 (9)	C7—C6—H6	119.4
O2ⁱ—Ni1—O3ⁱⁱⁱ	88.17 (9)	C6—C7—C2	118.1 (3)
O4ⁱⁱ—Ni1—O3ⁱⁱⁱ	168.24 (8)	C6—C7—S1	120.9 (2)
O2ⁱ—Ni1—O1	168.07 (8)	C2—C7—S1	121.0 (2)
O4ⁱⁱ—Ni1—O1	89.02 (9)	C9—C8—C13	118.9 (3)
O3ⁱⁱⁱ—Ni1—O1	89.89 (8)	C9—C8—S1	117.6 (2)
O2ⁱ—Ni1—O5	97.16 (8)	C13—C8—S1	123.1 (2)
O4ⁱⁱ—Ni1—O5	97.19 (8)	C10—C9—C8	121.5 (3)
O3ⁱⁱⁱ—Ni1—O5	94.56 (8)	C10—C9—H9	119.2
O1—Ni1—O5	94.73 (8)	C8—C9—H9	119.2
O2ⁱ—Ni1—Ni1ⁱ	84.58 (6)	C11—C10—C9	119.6 (3)
O4ⁱⁱ—Ni1—Ni1ⁱ	81.54 (6)	C11—C10—H10	120.2
O3ⁱⁱⁱ—Ni1—Ni1ⁱ	86.70 (6)	C9—C10—H10	120.2
O1—Ni1—Ni1ⁱ	83.56 (6)	C10—C11—C12	120.1 (3)
O5—Ni1—Ni1ⁱ	177.88 (6)	C10—C11—H11	120.0
C7—S1—C8	102.75 (13)	C12—C11—H11	120.0
C1—O1—Ni1	123.11 (19)	C11—C12—C13	120.9 (3)
C1—O2—Ni1ⁱ	123.63 (19)	C11—C12—H12	119.6
C14—O3—Ni1ⁱⁱⁱ	119.78 (18)	C13—C12—H12	119.6
C14—O4—Ni1^iv	125.92 (19)	C8—C13—C12	119.0 (3)
C15—O5—Ni1	120.6 (2)	C8—C13—C14	124.6 (3)
C15—N1—C17	120.9 (3)	C12—C13—C14	116.4 (2)
C15—N1—C16	120.9 (3)	O3—C14—O4	126.0 (3)
C17—N1—C16	118.2 (3)	O3—C14—C13	118.5 (2)
O2—C1—O1	124.9 (3)	O4—C14—C13	115.4 (3)
O2—C1—C2	117.1 (3)	O5—C15—N1	123.4 (3)
O1—C1—C2	118.0 (3)	O5—C15—H15	118.3
C3—C2—C7	119.1 (3)	N1—C15—H15	118.3
C3—C2—C1	117.4 (3)	N1—C16—H16A	109.5
C7—C2—C1	123.5 (3)	N1—C16—H16B	109.5
C4—C3—C2	122.1 (3)	H16A—C16—H16B	109.5
C4—C3—H3	118.9	N1—C16—H16C	109.5
C2—C3—H3	118.9	H16A—C16—H16C	109.5
C3—C4—C5	118.5 (3)	H16B—C16—H16C	109.5
C3—C4—H4	120.7	N1—C17—H17A	109.5
C5—C4—H4	120.7	N1—C17—H17B	109.5
C6—C5—C4	120.9 (3)	H17A—C17—H17B	109.5
C6—C5—H5	119.6	N1—C17—H17C	109.5
C4—C5—H5	119.6	H17A—C17—H17C	109.5
C5—C6—C7	121.2 (3)	H17B—C17—H17C	109.5
C5—C6—H6	119.4

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. Poly[[(μ-1H-benzimidazole-5,6-dicarboxyl-ato)zinc(II)] monohydrate].

Authors: Zhao-Yang Li; Jing-Wei Dai; Shan-Tang Yue
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2009-06-13

2 in total