Tris­(ethyl­enedi­amine-κ²N,N′)­cadmium(II) bis­(1,2-dicyanoethylenedithiolato-κ²S,S′)­cuprate(II)

In the title complex, [Cd(C₂H₈N₂)₃][Cu(C₄N₂S₂)₂], the Cd^II atom has a distorted octahedral geometry. The Cu^II atom is in a distorted square-planar geometry. Both ions lie on twofold rotation axes. They are not connected covalently.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.034
• wR factor = 0.095
• Data-to-parameter ratio = 16.1

checkCIF/PLATON results

No syntax errors found





Alert level C
ABSTM02_ALERT_3_C  The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
            Tmin and Tmax reported:      0.426     0.821
            Tmin and Tmax expected:      0.373     0.814
            RR =      1.135
            Please check that your absorption correction is appropriate.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large .......       1.14
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       3.24
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent .....          ?
PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors  for         S2
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors  for        Cd1
PLAT371_ALERT_2_C Long   C(sp2)-C(sp1) Bond  C1     -   C2     ...       1.43 Ang.
PLAT371_ALERT_2_C Long   C(sp2)-C(sp1) Bond  C3     -   C4     ...       1.45 Ang.
PLAT420_ALERT_2_C D-H Without Acceptor       N5     -   H5B    ...          ?
PLAT480_ALERT_4_C Long H...A H-Bond Reported H5B    ..  N1      ..       2.70 Ang.

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
  12 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   6 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker,1997); cell refinement: SAINT (Bruker,1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

Tris(ethylenediamine-κ²N,N')cadmium(II) bis[2,3-dimercaptobutenedinitrile(2-)-κ²S,S']cuprate(II)

Crystal data

[Cd(C2H8N2)3][Cu(C4N2S2)2]	F(000) = 1276
Mr = 636.61	Dx = 1.691 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 13.490 (3) Å	Cell parameters from 3045 reflections
b = 12.103 (2) Å	θ = 2.3–25.0°
c = 15.620 (3) Å	µ = 2.06 mm^−1
β = 101.331 (3)°	T = 293 K
V = 2500.7 (9) Å^3	Block, blue
Z = 4	0.50 × 0.50 × 0.10 mm

Data collection

Bruker SMART CCD area-detector diffractometer	2206 independent reflections
Radiation source: fine-focus sealed tube	1828 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.033
φ and ω scans	θmax = 25.0°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −15→16
Tmin = 0.426, Tmax = 0.821	k = −14→14
6440 measured reflections	l = −18→12

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.034	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.095	H-atom parameters constrained
S = 1.00	w = 1/[σ^2(Fo^2) + (0.062P)^2] where P = (Fo^2 + 2Fc^2)/3
2206 reflections	(Δ/σ)max < 0.001
137 parameters	Δρmax = 1.20 e Å^−3
0 restraints	Δρmin = −0.37 e Å^−3

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cd1	0.5000	0.62243 (3)	0.7500	0.04570 (16)
Cu1	0.5000	0.06911 (5)	0.7500	0.0449 (2)
N1	0.1298 (3)	0.0263 (4)	0.5166 (3)	0.0885 (13)
N2	0.6704 (4)	0.1510 (4)	1.1014 (3)	0.0859 (14)
N3	0.4775 (3)	0.6758 (3)	0.6023 (2)	0.0608 (9)
H3A	0.5359	0.7024	0.5909	0.073*
H3B	0.4590	0.6170	0.5675	0.073*
N4	0.3465 (2)	0.7273 (3)	0.72292 (19)	0.0569 (9)
H4A	0.2991	0.6934	0.7468	0.068*
H4B	0.3573	0.7951	0.7466	0.068*
N5	0.3947 (3)	0.4642 (3)	0.7152 (3)	0.0815 (12)
H5A	0.3377	0.4733	0.7360	0.098*
H5B	0.3775	0.4571	0.6568	0.098*
S1	0.33395 (8)	0.02789 (9)	0.71373 (6)	0.0536 (3)
S2	0.49284 (9)	0.11388 (11)	0.88966 (7)	0.0638 (3)
C1	0.2093 (3)	0.0425 (4)	0.5553 (3)	0.0585 (11)
C2	0.3098 (3)	0.0594 (3)	0.6031 (2)	0.0489 (9)
C3	0.6463 (4)	0.1246 (4)	1.0306 (3)	0.0616 (11)
C4	0.6185 (3)	0.0954 (3)	0.9391 (2)	0.0502 (9)
C5	0.3983 (4)	0.7618 (4)	0.5849 (3)	0.0715 (13)
H5C	0.3738	0.7679	0.5224	0.086*
H5D	0.4272	0.8324	0.6059	0.086*
C6	0.3126 (3)	0.7359 (4)	0.6279 (3)	0.0652 (12)
H6A	0.2618	0.7934	0.6146	0.078*
H6B	0.2819	0.6666	0.6053	0.078*
C7	0.4451 (4)	0.3667 (4)	0.7515 (5)	0.101 (2)
H7A	0.4133	0.3030	0.7198	0.122*
H7B	0.4375	0.3597	0.8118	0.122*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cd1	0.0471 (3)	0.0436 (2)	0.0435 (3)	0.000	0.00175 (17)	0.000
Cu1	0.0448 (4)	0.0483 (4)	0.0394 (4)	0.000	0.0030 (3)	0.000
N1	0.059 (3)	0.123 (4)	0.076 (3)	−0.006 (3)	−0.004 (2)	−0.021 (3)
N2	0.093 (3)	0.109 (4)	0.049 (3)	0.014 (3)	−0.001 (2)	−0.017 (2)
N3	0.064 (2)	0.073 (2)	0.0456 (19)	−0.0114 (19)	0.0120 (17)	−0.0035 (17)
N4	0.062 (2)	0.059 (2)	0.0496 (19)	0.0086 (17)	0.0097 (16)	−0.0004 (15)
N5	0.056 (2)	0.062 (2)	0.124 (4)	−0.0037 (19)	0.011 (2)	−0.007 (2)
S1	0.0479 (6)	0.0708 (7)	0.0418 (6)	−0.0059 (5)	0.0084 (4)	0.0004 (5)
S2	0.0527 (7)	0.0932 (9)	0.0440 (6)	0.0145 (6)	0.0059 (5)	−0.0090 (5)
C1	0.053 (3)	0.075 (3)	0.046 (2)	0.001 (2)	0.007 (2)	−0.008 (2)
C2	0.048 (2)	0.051 (2)	0.045 (2)	−0.0013 (17)	0.0029 (17)	−0.0072 (16)
C3	0.062 (3)	0.071 (3)	0.047 (3)	0.008 (2)	0.000 (2)	−0.004 (2)
C4	0.053 (2)	0.055 (2)	0.039 (2)	0.0014 (19)	0.0007 (18)	−0.0005 (17)
C5	0.081 (3)	0.083 (3)	0.049 (2)	0.009 (3)	0.007 (2)	0.014 (2)
C6	0.064 (3)	0.074 (3)	0.052 (3)	0.012 (2)	−0.003 (2)	0.001 (2)
C7	0.063 (3)	0.049 (3)	0.191 (7)	−0.003 (2)	0.022 (4)	0.014 (3)

Geometric parameters (Å, º)

Cd1—N3^i	2.358 (3)	N5—C7	1.423 (6)
Cd1—N3	2.358 (3)	N5—H5A	0.900
Cd1—N5	2.382 (4)	N5—H5B	0.900
Cd1—N5^i	2.382 (4)	S1—C2	1.737 (4)
Cd1—N4^i	2.395 (3)	S2—C4	1.734 (4)
Cd1—N4	2.395 (3)	C1—C2	1.429 (6)
Cu1—S1	2.2559 (11)	C2—C4^i	1.345 (6)
Cu1—S1^i	2.2559 (11)	C3—C4	1.449 (6)
Cu1—S2^i	2.2682 (12)	C4—C2^i	1.345 (6)
Cu1—S2	2.2682 (12)	C5—C6	1.482 (6)
N1—C1	1.140 (5)	C5—H5C	0.970
N2—C3	1.135 (6)	C5—H5D	0.970
N3—C5	1.478 (6)	C6—H6A	0.970
N3—H3A	0.900	C6—H6B	0.970
N3—H3B	0.900	C7—C7^i	1.491 (11)
N4—C6	1.468 (4)	C7—H7A	0.970
N4—H4A	0.900	C7—H7B	0.970
N4—H4B	0.900
N3^i—Cd1—N3	148.20 (19)	C7—N5—H5A	109.4
N3^i—Cd1—N5	113.58 (15)	Cd1—N5—H5A	109.4
N3—Cd1—N5	92.31 (15)	C7—N5—H5B	109.4
N3^i—Cd1—N5^i	92.31 (15)	Cd1—N5—H5B	109.4
N3—Cd1—N5^i	113.58 (15)	H5A—N5—H5B	108.0
N5—Cd1—N5^i	73.02 (19)	C2—S1—Cu1	100.60 (14)
N3^i—Cd1—N4^i	75.02 (12)	C4—S2—Cu1	100.08 (14)
N3—Cd1—N4^i	88.17 (11)	N1—C1—C2	178.2 (5)
N5—Cd1—N4^i	157.27 (13)	C4^i—C2—C1	119.4 (4)
N5^i—Cd1—N4^i	85.97 (13)	C4^i—C2—S1	123.1 (3)
N3^i—Cd1—N4	88.17 (11)	C1—C2—S1	117.5 (3)
N3—Cd1—N4	75.02 (12)	N2—C3—C4	177.2 (6)
N5—Cd1—N4	85.97 (13)	C2^i—C4—C3	119.4 (4)
N5^i—Cd1—N4	157.27 (14)	C2^i—C4—S2	123.9 (3)
N4^i—Cd1—N4	115.99 (18)	C3—C4—S2	116.7 (3)
S1—Cu1—S1^i	154.45 (7)	N3—C5—C6	111.6 (4)
S1—Cu1—S2^i	92.24 (4)	N3—C5—H5C	109.3
S1^i—Cu1—S2^i	93.82 (4)	C6—C5—H5C	109.3
S1—Cu1—S2	93.81 (4)	N3—C5—H5D	109.3
S1^i—Cu1—S2	92.24 (4)	C6—C5—H5D	109.3
S2^i—Cu1—S2	152.36 (8)	H5C—C5—H5D	108.0
C5—N3—Cd1	108.8 (2)	N4—C6—C5	110.9 (4)
C5—N3—H3A	109.9	N4—C6—H6A	109.5
Cd1—N3—H3A	109.9	C5—C6—H6A	109.5
C5—N3—H3B	109.9	N4—C6—H6B	109.5
Cd1—N3—H3B	109.9	C5—C6—H6B	109.5
H3A—N3—H3B	108.3	H6A—C6—H6B	108.0
C6—N4—Cd1	107.6 (2)	N5—C7—C7^i	112.7 (4)
C6—N4—H4A	110.2	N5—C7—H7A	109.0
Cd1—N4—H4A	110.2	C7^i—C7—H7A	109.0
C6—N4—H4B	110.2	N5—C7—H7B	109.0
Cd1—N4—H4B	110.2	C7^i—C7—H7B	109.0
H4A—N4—H4B	108.5	H7A—C7—H7B	107.8
C7—N5—Cd1	111.0 (3)
N3—C5—C6—N4	59.7 (5)	N5—C7—C7^i—N5^i	51.9 (12)

Symmetry code: (i) −x+1, y, −z+3/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N3—H3A···N2^ii	0.90	2.52	3.343 (6)	152
N3—H3B···N1^iii	0.90	2.36	3.235 (6)	166
N4—H4A···S1^iv	0.90	2.84	3.698 (4)	161
N4—H4B···N2^v	0.90	2.56	3.162 (5)	125
N4—H4B···S1^vi	0.90	2.87	3.643 (4)	145
N5—H5A···S1^iv	0.90	2.67	3.563 (4)	172
N5—H5B···N1^iii	0.90	2.70	3.572 (6)	164

Symmetry codes: (ii) x, −y+1, z−1/2; (iii) −x+1/2, −y+1/2, −z+1; (iv) −x+1/2, y+1/2, −z+3/2; (v) −x+1, −y+1, −z+2; (vi) x, y+1, z.