catena-Poly[[nickel(II)-μ(3)-1,1-dicyano-ethene-2,2-dithiol-ato-κS,S':N:N'-bis-[(15-crown-5)magnesium(II)]-μ(3)-1,1-dicyano-ethene-2,2-dithiol-ato-κN:N':S,S'] dichloride].

The reaction of MgCl(2), NiCl(2), and Na(2)(i-mnt) (i-mnt is 1,1-dicyano-thene-2,2-dithiol-ate) with 15-crown-5 (15-C-5) leads to an infinite chain polymer, {[NiMg(2)(C(4)N(2)S(2))(2)(C(10)H(20)O(5))(2)]Cl(2)}(n) or {[Mg(15-C-5)](2)[Ni(i-mnt)(2)]Cl(2)}(n), which consists of two [Mg(15-C-5)](2+) complex cations, one [Ni(i-mnt)(2)](2-) complex anion and two Cl(-) ions per formula unit. In the [Ni(i-mnt)(2)](2-) complex anion, Ni(2+) is located on a crystallographic mirror plane with a slightly distorted square-planar coordination by four S atoms. In the [Mg(15-C-5)](2+) complex cations, the Mg and one O atom of the crown lie on mirror planes and the Mg atoms are in sevenfold coordination environments of five O atoms from the crown and two N atoms from two i-mnt anions. The bridging of the two complexes via the Mg-N bonds leads to the formation of one-dimensional chains along the a axis.

Related literature

For studies on crown ether complexes of alkaline earth n class="Chemical">metals, see: Junk & Steed (1999 ▶). For comparative data on Ni–S bonds, see: Gao et al. (2005 ▶). For comparative data on Mg–O bonds, see: Chadwick et al. (1999 ▶).

Experimental

Crystal data

[NiMg2(C4N2S2)2(C10H20O5)2]Cl2

M = 899.11

Orthorhombic,

a = 13.6227 (16) Å

b = 20.591 (3) Å

c = 15.148 (2) Å

V = 4249 (1) Å3

Z = 4

Mo Kα radiation

μ = 0.86 mm−1

T = 298 (2) K

0.41 × 0.32 × 0.30 mm

Data collection

Bruker SMART CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.719, T max = 0.783

10632 measured reflections

1979 independent reflections

1651 reflections with I > 2σ(I)

R int = 0.033

Refinement

R[F 2 > 2σ(F 2)] = 0.065

wR(F 2) = 0.192

S = 1.06

1979 reflections

242 parameters

1 restraint

H-atom parameters constrained

Δρmax = 0.92 e Å−3

Δρmin = −0.47 e Å−3

Absolute structure: Flack (1983 ▶), 1979 Friedel pairs

Flack parameter: 0.02 (5)

Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1997 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a ▶); molecular graphics: SHELXTL (Sheldrick, 1997b ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807065622/sq2001sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536807065622/sq2001Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[NiMg2(C4N2S2)2(C10H20O5)2]Cl2	F000 = 1864
Mr = 899.11	Dx = 1.406 Mg m−3
Orthorhombic, Cmc21	Mo Kα radiation λ = 0.71073 Å
Hall symbol: C 2c -2	Cell parameters from 4296 reflections
a = 13.6227 (16) Å	θ = 2.2–24.9º
b = 20.591 (3) Å	µ = 0.86 mm−1
c = 15.148 (2) Å	T = 298 (2) K
V = 4249 (1) Å3	Block, brown
Z = 4	0.41 × 0.32 × 0.30 mm

Bruker SMART CCD area-detector diffractometer	1979 independent reflections
Radiation source: fine-focus sealed tube	1651 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.033
T = 298(2) K	θmax = 25.0º
φ and ω scans	θmin = 2.4º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)	h = −16→16
Tmin = 0.719, Tmax = 0.783	k = −24→23
10632 measured reflections	l = −9→18

Refinement on F2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.065	w = 1/[σ2(Fo2) + (0.1309P)2 + 12.7693P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.192	(Δ/σ)max = 0.001
S = 1.06	Δρmax = 0.92 e Å−3
1979 reflections	Δρmin = −0.46 e Å−3
242 parameters	Extinction correction: none
1 restraint	Absolute structure: Flack (1983)
Primary atom site location: structure-invariant direct methods	Flack parameter: 0.02 (5)
Secondary atom site location: difference Fourier map

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	Uiso*/Ueq
Ni1	0.0000	0.12793 (7)	0.9803 (2)	0.0492 (4)
Mg1	0.5000	0.3176 (3)	1.0866 (4)	0.0713 (14)
Mg2	0.5000	−0.0308 (2)	0.8135 (3)	0.0565 (11)
N1	0.3850 (8)	0.2476 (5)	0.9910 (9)	0.093 (4)
N2	0.3863 (6)	0.0587 (5)	0.8547 (8)	0.074 (3)
O1	0.5000	0.4399 (6)	1.1122 (9)	0.084 (3)
O2	0.3268 (7)	0.3721 (4)	1.1116 (7)	0.084 (2)
O3	0.3963 (10)	0.2655 (6)	1.2030 (8)	0.112 (4)
O4	0.5000	−0.0908 (6)	0.9581 (9)	0.109 (5)
O5	0.6412 (9)	−0.1054 (5)	0.8323 (8)	0.103 (3)
O6	0.5988 (12)	−0.0446 (7)	0.6826 (9)	0.131 (4)
Cl1	0.0000	0.9064 (4)	0.8312 (9)	0.159 (4)
Cl2	0.0000	0.2859 (4)	0.2265 (8)	0.149 (3)
S1	0.12480 (17)	0.18894 (12)	1.02320 (19)	0.0571 (6)
S2	0.12522 (16)	0.07215 (11)	0.9274 (2)	0.0564 (6)
C1	0.4140 (11)	0.4707 (7)	1.1444 (12)	0.095 (4)
H1A	0.4158	0.5167	1.1309	0.114*
H1B	0.4095	0.4655	1.2079	0.114*
C2	0.3302 (12)	0.4407 (6)	1.1020 (12)	0.098 (4)
H2A	0.2706	0.4591	1.1265	0.118*
H2B	0.3316	0.4512	1.0395	0.118*
C3	0.2781 (12)	0.3557 (9)	1.1909 (12)	0.100 (4)
H3A	0.2084	0.3647	1.1863	0.120*
H3B	0.3047	0.3803	1.2401	0.120*
C4	0.2959 (14)	0.2843 (9)	1.2035 (13)	0.108 (5)
H4A	0.2670	0.2712	1.2592	0.129*
H4B	0.2620	0.2609	1.1569	0.129*
C5	0.4508 (14)	0.2588 (10)	1.2820 (11)	0.116 (6)
H5A	0.4301	0.2936	1.3210	0.140*
H5B	0.4301	0.2185	1.3093	0.140*
C6	0.589 (2)	−0.1249 (9)	0.9749 (16)	0.132 (7)
H6A	0.5784	−0.1707	0.9635	0.159*
H6B	0.6055	−0.1202	1.0368	0.159*
C7	0.674 (2)	−0.1019 (10)	0.9200 (15)	0.130 (7)
H7A	0.6922	−0.0577	0.9353	0.156*
H7B	0.7311	−0.1297	0.9287	0.156*
C8	0.7145 (16)	−0.0869 (10)	0.7714 (16)	0.123 (6)
H8A	0.7715	−0.1148	0.7775	0.147*
H8B	0.7347	−0.0425	0.7823	0.147*
C9	0.6722 (17)	−0.0931 (10)	0.6793 (15)	0.127 (7)
H9A	0.7209	−0.0838	0.6343	0.152*
H9B	0.6445	−0.1358	0.6691	0.152*
C10	0.552 (2)	−0.0474 (13)	0.600 (2)	0.172 (11)
H10A	0.5743	−0.0863	0.5698	0.206*
H10B	0.5743	−0.0105	0.5652	0.206*
C11	0.1961 (6)	0.1356 (4)	0.9620 (6)	0.051 (2)
C12	0.2935 (7)	0.1459 (4)	0.9403 (7)	0.0521 (19)
C13	0.3435 (7)	0.2023 (5)	0.9693 (8)	0.061 (2)
C14	0.3456 (7)	0.0975 (5)	0.8923 (8)	0.057 (2)

	U11	U22	U33	U12	U13	U23
Ni1	0.0437 (7)	0.0506 (8)	0.0532 (8)	0.000	0.000	−0.0009 (7)
Mg1	0.077 (3)	0.067 (3)	0.069 (3)	0.000	0.000	−0.006 (3)
Mg2	0.057 (2)	0.058 (2)	0.055 (2)	0.000	0.000	−0.009 (2)
N1	0.075 (6)	0.090 (7)	0.116 (9)	−0.019 (5)	0.025 (6)	−0.051 (7)
N2	0.044 (4)	0.075 (6)	0.104 (7)	0.008 (4)	0.006 (5)	−0.033 (6)
O1	0.080 (8)	0.071 (7)	0.101 (9)	0.000	0.000	−0.023 (6)
O2	0.078 (5)	0.086 (5)	0.089 (6)	0.005 (4)	0.003 (5)	−0.012 (5)
O3	0.121 (9)	0.138 (9)	0.077 (6)	0.016 (7)	0.026 (6)	0.007 (6)
O4	0.185 (16)	0.072 (7)	0.069 (8)	0.000	0.000	0.007 (6)
O5	0.126 (9)	0.080 (6)	0.103 (8)	0.020 (6)	−0.031 (7)	−0.013 (6)
O6	0.173 (12)	0.117 (9)	0.103 (9)	0.033 (9)	0.043 (9)	0.004 (7)
Cl1	0.130 (6)	0.122 (5)	0.225 (11)	0.000	0.000	0.018 (7)
Cl2	0.115 (5)	0.136 (5)	0.197 (9)	0.000	0.000	0.046 (6)
S1	0.0443 (12)	0.0618 (13)	0.0652 (14)	0.0027 (9)	0.0003 (11)	−0.0202 (12)
S2	0.0471 (12)	0.0464 (11)	0.0757 (15)	0.0005 (8)	0.0012 (12)	−0.0051 (11)
C1	0.092 (9)	0.084 (8)	0.108 (11)	0.010 (7)	−0.009 (9)	−0.006 (8)
C2	0.096 (10)	0.081 (8)	0.117 (11)	0.016 (7)	−0.011 (9)	−0.009 (8)
C3	0.085 (9)	0.116 (12)	0.100 (11)	−0.005 (8)	0.004 (8)	−0.006 (9)
C4	0.103 (11)	0.120 (12)	0.101 (11)	−0.014 (9)	0.026 (9)	−0.002 (10)
C5	0.132 (13)	0.136 (14)	0.081 (9)	−0.036 (10)	0.006 (9)	0.012 (9)
C6	0.21 (2)	0.098 (11)	0.085 (9)	0.031 (14)	−0.032 (16)	0.003 (9)
C7	0.161 (19)	0.104 (12)	0.126 (16)	0.037 (12)	−0.043 (15)	−0.029 (12)
C8	0.121 (15)	0.108 (12)	0.140 (16)	0.038 (11)	0.015 (14)	−0.022 (12)
C9	0.138 (16)	0.110 (13)	0.132 (16)	0.022 (12)	0.044 (14)	−0.013 (11)
C10	0.20 (3)	0.18 (2)	0.135 (18)	0.064 (19)	0.041 (18)	−0.006 (17)
C11	0.046 (4)	0.052 (4)	0.055 (6)	0.007 (4)	−0.005 (4)	0.001 (4)
C12	0.052 (5)	0.049 (4)	0.055 (5)	0.006 (4)	−0.002 (4)	−0.005 (4)
C13	0.053 (5)	0.062 (5)	0.066 (6)	−0.002 (4)	0.004 (5)	−0.017 (5)
C14	0.048 (5)	0.052 (5)	0.072 (6)	0.000 (4)	−0.003 (5)	−0.006 (5)

Ni1—S2i	2.207 (3)	O6—C10	1.41 (3)
Ni1—S2	2.207 (3)	O6—C9	1.41 (2)
Ni1—S1	2.212 (3)	S1—C11	1.734 (9)
Ni1—S1i	2.212 (3)	S2—C11	1.708 (9)
Mg1—O3	2.502 (13)	C1—C2	1.45 (2)
Mg1—O3ii	2.502 (13)	C1—H1A	0.9700
Mg1—O1	2.548 (13)	C1—H1B	0.9700
Mg1—N1	2.575 (12)	C2—H2A	0.9700
Mg1—N1ii	2.575 (12)	C2—H2B	0.9700
Mg1—O2ii	2.640 (10)	C3—C4	1.50 (2)
Mg1—O2	2.640 (10)	C3—H3A	0.9700
Mg2—O6ii	2.414 (12)	C3—H3B	0.9700
Mg2—O6	2.414 (12)	C4—H4A	0.9700
Mg2—O5ii	2.478 (11)	C4—H4B	0.9700
Mg2—O5	2.478 (11)	C5—H5A	0.9700
Mg2—N2ii	2.487 (10)	C5—H5B	0.9700
Mg2—N2	2.487 (9)	C6—C7	1.51 (3)
Mg2—O4	2.514 (14)	C6—H6A	0.9700
N1—C13	1.140 (13)	C6—H6B	0.9700
N2—C14	1.128 (13)	C7—H7A	0.9700
O1—C1ii	1.418 (16)	C7—H7B	0.9700
O1—C1	1.418 (16)	C8—C9	1.51 (3)
O2—C3	1.41 (2)	C8—H8A	0.9700
O2—C2	1.420 (15)	C8—H8B	0.9700
O3—C5	1.41 (2)	C9—H9A	0.9700
O3—C4	1.42 (2)	C9—H9B	0.9700
O4—C6	1.42 (2)	C10—H10A	0.9700
O4—C6ii	1.42 (2)	C10—H10B	0.9700
O5—C7	1.40 (2)	C11—C12	1.383 (13)
O5—C8	1.41 (2)
S2i—Ni1—S2	101.24 (16)	C11—S2—Ni1	85.8 (3)
S2i—Ni1—S1	175.2 (2)	O1—C1—C2	108.0 (12)
S2—Ni1—S1	78.94 (8)	O1—C1—H1A	110.1
S2i—Ni1—S1i	78.94 (8)	C2—C1—H1A	110.1
S2—Ni1—S1i	175.2 (2)	O1—C1—H1B	110.1
S1—Ni1—S1i	100.48 (15)	C2—C1—H1B	110.1
O3—Mg1—O3ii	68.8 (6)	H1A—C1—H1B	108.4
O3—Mg1—O1	108.5 (4)	O2—C2—C1	113.8 (12)
O3ii—Mg1—O1	108.5 (4)	O2—C2—H2A	108.8
O3—Mg1—N1	79.2 (4)	C1—C2—H2A	108.8
O3ii—Mg1—N1	120.0 (5)	O2—C2—H2B	108.8
O1—Mg1—N1	129.7 (4)	C1—C2—H2B	108.8
O3—Mg1—N1ii	120.0 (5)	H2A—C2—H2B	107.7
O3ii—Mg1—N1ii	79.2 (4)	O2—C3—C4	105.4 (13)
O1—Mg1—N1ii	129.7 (4)	O2—C3—H3A	110.7
N1—Mg1—N1ii	74.9 (5)	C4—C3—H3A	110.7
O3—Mg1—O2ii	125.9 (4)	O2—C3—H3B	110.7
O3ii—Mg1—O2ii	64.9 (4)	C4—C3—H3B	110.7
O1—Mg1—O2ii	63.8 (2)	H3A—C3—H3B	108.8
N1—Mg1—O2ii	149.6 (4)	O3—C4—C3	114.9 (14)
N1ii—Mg1—O2ii	77.0 (3)	O3—C4—H4A	108.5
O3—Mg1—O2	64.9 (4)	C3—C4—H4A	108.5
O3ii—Mg1—O2	125.9 (4)	O3—C4—H4B	108.5
O1—Mg1—O2	63.8 (2)	C3—C4—H4B	108.5
N1—Mg1—O2	77.0 (3)	H4A—C4—H4B	107.5
N1ii—Mg1—O2	149.6 (4)	C5ii—C5—O3	121.6 (8)
O2ii—Mg1—O2	126.7 (4)	C5ii—C5—H5A	106.9
O6ii—Mg2—O6	67.8 (9)	O3—C5—H5A	106.9
O6ii—Mg2—O5ii	65.7 (5)	C5ii—C5—H5B	106.9
O6—Mg2—O5ii	117.0 (5)	O3—C5—H5B	106.9
O6ii—Mg2—O5	117.0 (5)	H5A—C5—H5B	106.7
O6—Mg2—O5	65.7 (5)	O4—C6—C7	113.9 (16)
O5ii—Mg2—O5	101.9 (6)	O4—C6—H6A	108.8
O6ii—Mg2—N2ii	129.8 (5)	C7—C6—H6A	108.8
O6—Mg2—N2ii	86.9 (5)	O4—C6—H6B	108.8
O5ii—Mg2—N2ii	156.1 (4)	C7—C6—H6B	108.8
O5—Mg2—N2ii	87.0 (3)	H6A—C6—H6B	107.7
O6ii—Mg2—N2	86.9 (5)	O5—C7—C6	104.8 (19)
O6—Mg2—N2	129.8 (5)	O5—C7—H7A	110.8
O5ii—Mg2—N2	87.0 (3)	C6—C7—H7A	110.8
O5—Mg2—N2	156.1 (4)	O5—C7—H7B	110.8
N2ii—Mg2—N2	77.0 (4)	C6—C7—H7B	110.8
O6ii—Mg2—O4	131.1 (4)	H7A—C7—H7B	108.9
O6—Mg2—O4	131.1 (4)	O5—C8—C9	108.1 (17)
O5ii—Mg2—O4	66.1 (4)	O5—C8—H8A	110.1
O5—Mg2—O4	66.1 (4)	C9—C8—H8A	110.1
N2ii—Mg2—O4	98.4 (4)	O5—C8—H8B	110.1
N2—Mg2—O4	98.4 (4)	C9—C8—H8B	110.1
C13—N1—Mg1	157.3 (12)	H8A—C8—H8B	108.4
C14—N2—Mg2	163.5 (10)	O6—C9—C8	100.3 (15)
C1ii—O1—C1	111.5 (14)	O6—C9—H9A	111.7
C1ii—O1—Mg1	119.6 (7)	C8—C9—H9A	111.7
C1—O1—Mg1	119.6 (8)	O6—C9—H9B	111.7
C3—O2—C2	109.9 (13)	C8—C9—H9B	111.7
C3—O2—Mg1	116.1 (9)	H9A—C9—H9B	109.5
C2—O2—Mg1	112.2 (9)	O6—C10—C10ii	116.9 (12)
C5—O3—C4	121.8 (13)	O6—C10—H10A	108.1
C5—O3—Mg1	110.0 (10)	C10ii—C10—H10A	108.1
C4—O3—Mg1	115.4 (10)	O6—C10—H10B	108.1
C6—O4—C6ii	117 (2)	C10ii—C10—H10B	108.1
C6—O4—Mg2	113.4 (13)	H10A—C10—H10B	107.3
C6ii—O4—Mg2	113.4 (13)	C12—C11—S2	125.9 (7)
C7—O5—C8	112.1 (18)	C12—C11—S1	124.6 (7)
C7—O5—Mg2	109.1 (11)	S2—C11—S1	109.4 (5)
C8—O5—Mg2	107.9 (10)	C11—C12—C13	120.9 (8)
C10—O6—C9	105.1 (16)	C11—C12—C14	119.5 (8)
C10—O6—Mg2	119.0 (14)	C13—C12—C14	119.5 (8)
C9—O6—Mg2	120.5 (12)	N1—C13—C12	178.5 (12)
C11—S1—Ni1	85.1 (3)	N2—C14—C12	179.3 (13)