Bis­(diethyl­di­thio­carbamato)(4,7-di­methyl-1,10-phenanthroline)­cadmium(II) aceto­nitrile solvate

An N₂S₄ donor set defines the coordination environment about the cadmium centre in the monomeric title complex, [Cd(dedtc)₂(4,7-Me₂phen)]·C₂H₃N or [Cd{S₂CN(CH₂CH₃)₂}₂(C₁₄H₁₂N₂)]·C₂H₃N. The disposition of the donor atoms is such as to define a polyhedron based on a trigonal prism.

Key indicators

• Single-crystal X-ray study
• T = 223 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.045
• wR factor = 0.105
• Data-to-parameter ratio = 27.7

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



PLAT_601  Alert C Structure Contains Solvent Accessible VOIDS of      31.00 A   3


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 1 Alert Level C = Please check

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Computing details

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SHELXTL (Bruker, 2000); program(s) used to solve structure: PATTY in DIRDIF92 (Beurskens et al., 1992); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

(I)

Crystal data

[Cd(C5H10NS2)2(C14H12N2)]·C2H3N	F(000) = 1352
Mr = 658.23	Dx = 1.396 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ybc	Cell parameters from 7229 reflections
a = 10.9451 (7) Å	θ = 2.4–30.0°
b = 10.0886 (6) Å	µ = 0.99 mm^−1
c = 28.4366 (17) Å	T = 223 K
β = 94.198 (1)°	Needle, pale yellow
V = 3131.6 (3) Å^3	0.55 × 0.08 × 0.08 mm
Z = 4

Data collection

Bruker SMART CCD diffractometer	9058 independent reflections
Radiation source: fine-focus sealed tube	7059 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.036
ω scans	θmax = 30.0°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Bruker, 2000)	h = −15→15
Tmin = 0.739, Tmax = 0.924	k = −13→14
25219 measured reflections	l = −29→39

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)] = 0.045	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.105	H-atom parameters constrained
S = 1.06	w = 1/[σ^2(Fo^2) + (0.0518P)^2 + 0.3208P] where P = (Fo^2 + 2Fc^2)/3
9058 reflections	(Δ/σ)max < 0.001
327 parameters	Δρmax = 1.27 e Å^−3
0 restraints	Δρmin = −0.39 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
Cd	0.209246 (17)	0.055993 (18)	0.381692 (6)	0.02906 (6)
S1	0.18936 (7)	−0.10176 (8)	0.30872 (3)	0.03940 (16)
S2	−0.02587 (6)	−0.00790 (8)	0.35664 (2)	0.03718 (16)
S3	0.31591 (7)	0.26857 (7)	0.34721 (3)	0.03747 (16)
S4	0.15161 (6)	0.27958 (7)	0.42552 (3)	0.03591 (15)
N1	−0.0398 (2)	−0.1606 (2)	0.27983 (8)	0.0377 (5)
N2	0.2453 (2)	0.4914 (2)	0.38633 (10)	0.0448 (6)
N3	0.21585 (19)	−0.0738 (2)	0.45277 (8)	0.0297 (4)
N4	0.4118 (2)	−0.0274 (2)	0.40355 (7)	0.0298 (4)
N5	0.6101 (5)	0.1238 (5)	0.27512 (19)	0.1218 (19)
C1	0.0333 (2)	−0.0971 (3)	0.31203 (9)	0.0304 (5)
C2	0.0082 (3)	−0.2366 (3)	0.24123 (11)	0.0501 (8)
H2A	0.0857	−0.2784	0.2524	0.060*
H2B	−0.0499	−0.3070	0.2314	0.060*
C3	0.0289 (4)	−0.1491 (4)	0.19928 (12)	0.0647 (11)
H3A	0.0605	−0.2022	0.1744	0.097*
H3B	0.0876	−0.0803	0.2087	0.097*
H3C	−0.0480	−0.1087	0.1878	0.097*
C4	−0.1741 (3)	−0.1545 (4)	0.27888 (11)	0.0483 (8)
H4A	−0.2080	−0.1487	0.2461	0.058*
H4B	−0.1981	−0.0742	0.2953	0.058*
C5	−0.2272 (4)	−0.2743 (4)	0.30194 (17)	0.0743 (12)
H5A	−0.3156	−0.2663	0.3008	0.111*
H5B	−0.1945	−0.2798	0.3345	0.111*
H5C	−0.2054	−0.3538	0.2853	0.111*
C6	0.2385 (2)	0.3603 (2)	0.38642 (9)	0.0315 (5)
C7	0.1800 (4)	0.5729 (3)	0.41929 (16)	0.0643 (11)
H7A	0.2264	0.6545	0.4262	0.077*
H7B	0.1753	0.5243	0.4490	0.077*
C8	0.0525 (4)	0.6082 (4)	0.40002 (19)	0.0814 (14)
H8A	0.0145	0.6650	0.4223	0.122*
H8B	0.0045	0.5280	0.3951	0.122*
H8C	0.0564	0.6545	0.3703	0.122*
C9	0.3169 (4)	0.5650 (3)	0.35282 (16)	0.0656 (11)
H9A	0.2778	0.6509	0.3458	0.079*
H9B	0.3177	0.5151	0.3233	0.079*
C10	0.4458 (4)	0.5869 (4)	0.3726 (2)	0.0953 (17)
H10A	0.4902	0.6369	0.3502	0.143*
H10B	0.4855	0.5020	0.3786	0.143*
H10C	0.4452	0.6361	0.4019	0.143*
C11	0.1182 (3)	−0.0979 (3)	0.47650 (11)	0.0411 (7)
H11	0.0415	−0.0668	0.4642	0.049*
C12	0.1248 (3)	−0.1674 (4)	0.51892 (11)	0.0495 (8)
H12	0.0530	−0.1817	0.5344	0.059*
C13	0.2335 (3)	−0.2152 (3)	0.53836 (11)	0.0447 (7)
C14	0.3389 (2)	−0.1924 (3)	0.51329 (9)	0.0335 (6)
C15	0.3253 (2)	−0.1206 (2)	0.47112 (8)	0.0266 (5)
C16	0.4308 (2)	−0.0978 (2)	0.44389 (8)	0.0259 (5)
C17	0.5073 (3)	−0.0085 (3)	0.37828 (10)	0.0364 (6)
H17	0.4958	0.0414	0.3504	0.044*
C18	0.6237 (3)	−0.0583 (3)	0.39075 (10)	0.0382 (6)
H18	0.6879	−0.0430	0.3712	0.046*
C19	0.6450 (2)	−0.1297 (3)	0.43158 (10)	0.0346 (6)
C20	0.5449 (2)	−0.1501 (3)	0.45999 (9)	0.0291 (5)
C21	0.5556 (3)	−0.2208 (3)	0.50364 (10)	0.0383 (6)
H21	0.6322	−0.2551	0.5148	0.046*
C22	0.4581 (3)	−0.2394 (3)	0.52906 (10)	0.0405 (7)
H22	0.4687	−0.2845	0.5580	0.049*
C23	0.2406 (4)	−0.2894 (4)	0.58441 (13)	0.0684 (11)
H23A	0.1599	−0.2931	0.5963	0.103*
H23B	0.2966	−0.2442	0.6071	0.103*
H23C	0.2698	−0.3787	0.5795	0.103*
C24	0.7687 (3)	−0.1870 (4)	0.44534 (12)	0.0499 (8)
H24A	0.8260	−0.1597	0.4227	0.075*
H24B	0.7633	−0.2829	0.4457	0.075*
H24C	0.7970	−0.1553	0.4765	0.075*
C25	0.5948 (4)	0.2325 (5)	0.27354 (17)	0.0771 (13)
C26	0.5714 (6)	0.3716 (5)	0.2716 (3)	0.133 (3)
H26A	0.5334	0.3946	0.2408	0.199*
H26B	0.6479	0.4196	0.2770	0.199*
H26C	0.5168	0.3954	0.2956	0.199*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cd	0.03002 (10)	0.02543 (10)	0.03156 (11)	0.00088 (7)	0.00117 (7)	0.00150 (7)
S1	0.0344 (3)	0.0431 (4)	0.0411 (4)	−0.0001 (3)	0.0060 (3)	−0.0097 (3)
S2	0.0351 (3)	0.0411 (4)	0.0356 (4)	0.0001 (3)	0.0044 (3)	−0.0086 (3)
S3	0.0425 (4)	0.0287 (3)	0.0422 (4)	0.0013 (3)	0.0101 (3)	0.0039 (3)
S4	0.0364 (3)	0.0347 (4)	0.0368 (4)	0.0020 (3)	0.0040 (3)	0.0005 (3)
N1	0.0392 (12)	0.0391 (13)	0.0351 (12)	−0.0053 (10)	0.0040 (10)	−0.0089 (10)
N2	0.0451 (14)	0.0245 (12)	0.0648 (18)	−0.0011 (10)	0.0050 (12)	−0.0020 (11)
N3	0.0295 (11)	0.0273 (11)	0.0326 (11)	0.0033 (8)	0.0058 (9)	0.0017 (8)
N4	0.0326 (11)	0.0298 (11)	0.0270 (11)	0.0016 (8)	0.0033 (9)	0.0030 (8)
N5	0.159 (5)	0.082 (3)	0.134 (4)	0.013 (3)	0.074 (4)	0.018 (3)
C1	0.0369 (14)	0.0269 (12)	0.0273 (12)	−0.0012 (10)	0.0018 (10)	0.0013 (9)
C2	0.056 (2)	0.0495 (19)	0.0452 (18)	−0.0107 (15)	0.0097 (15)	−0.0235 (14)
C3	0.074 (3)	0.085 (3)	0.0364 (18)	−0.022 (2)	0.0091 (17)	−0.0113 (17)
C4	0.0385 (16)	0.060 (2)	0.0447 (18)	−0.0019 (14)	−0.0056 (13)	−0.0140 (15)
C5	0.052 (2)	0.076 (3)	0.098 (3)	−0.019 (2)	0.020 (2)	−0.012 (2)
C6	0.0303 (12)	0.0243 (12)	0.0387 (15)	0.0006 (9)	−0.0063 (10)	−0.0001 (10)
C7	0.064 (2)	0.0314 (17)	0.098 (3)	−0.0008 (15)	0.011 (2)	−0.0241 (17)
C8	0.064 (3)	0.047 (2)	0.134 (4)	0.0165 (19)	0.018 (3)	−0.011 (2)
C9	0.069 (2)	0.0274 (16)	0.103 (3)	−0.0008 (15)	0.024 (2)	0.0144 (17)
C10	0.075 (3)	0.063 (3)	0.152 (5)	−0.035 (2)	0.037 (3)	−0.026 (3)
C11	0.0295 (13)	0.0441 (16)	0.0512 (18)	0.0047 (12)	0.0131 (12)	0.0047 (13)
C12	0.0402 (16)	0.060 (2)	0.0511 (19)	0.0024 (14)	0.0226 (14)	0.0138 (16)
C13	0.0479 (17)	0.0470 (18)	0.0409 (17)	−0.0008 (14)	0.0160 (13)	0.0114 (13)
C14	0.0371 (14)	0.0332 (14)	0.0307 (14)	−0.0013 (11)	0.0060 (11)	0.0032 (10)
C15	0.0287 (12)	0.0246 (12)	0.0269 (12)	0.0010 (9)	0.0052 (9)	−0.0021 (9)
C16	0.0298 (12)	0.0249 (11)	0.0232 (12)	−0.0008 (9)	0.0031 (9)	−0.0030 (9)
C17	0.0384 (14)	0.0411 (15)	0.0306 (14)	0.0033 (12)	0.0077 (11)	0.0059 (11)
C18	0.0333 (14)	0.0478 (17)	0.0346 (14)	0.0010 (12)	0.0105 (11)	0.0002 (12)
C19	0.0281 (12)	0.0393 (15)	0.0365 (14)	0.0003 (11)	0.0022 (10)	−0.0026 (11)
C20	0.0271 (12)	0.0303 (13)	0.0297 (13)	−0.0022 (10)	0.0009 (9)	−0.0022 (10)
C21	0.0330 (14)	0.0453 (16)	0.0354 (15)	0.0032 (12)	−0.0045 (11)	0.0066 (12)
C22	0.0423 (16)	0.0466 (17)	0.0321 (15)	0.0003 (13)	−0.0001 (12)	0.0131 (12)
C23	0.066 (2)	0.089 (3)	0.053 (2)	−0.002 (2)	0.0206 (18)	0.032 (2)
C24	0.0307 (14)	0.071 (2)	0.0483 (19)	0.0066 (14)	0.0058 (13)	0.0055 (16)
C25	0.077 (3)	0.079 (3)	0.080 (3)	0.001 (3)	0.042 (2)	0.011 (3)
C26	0.138 (5)	0.075 (4)	0.203 (7)	0.001 (3)	0.130 (5)	0.011 (4)

Geometric parameters (Å, º)

Cd—S1	2.6116 (7)	C8—H8C	0.9700
Cd—S2	2.6976 (7)	C9—C10	1.496 (6)
Cd—S3	2.6630 (7)	C9—H9A	0.9800
Cd—S4	2.6747 (7)	C9—H9B	0.9800
Cd—N3	2.405 (2)	C10—H10A	0.9700
Cd—N4	2.410 (2)	C10—H10B	0.9700
S1—C1	1.719 (3)	C10—H10C	0.9700
S2—C1	1.720 (3)	C11—C12	1.393 (4)
S4—C6	1.720 (3)	C11—H11	0.9400
S3—C6	1.720 (3)	C12—C13	1.363 (4)
N1—C1	1.335 (3)	C12—H12	0.9400
N1—C2	1.467 (4)	C13—C14	1.419 (4)
N1—C4	1.469 (4)	C13—C23	1.505 (4)
N2—C6	1.324 (4)	C14—C22	1.429 (4)
N2—C7	1.471 (4)	C14—C15	1.400 (3)
N2—C9	1.478 (4)	C15—C16	1.455 (3)
N3—C15	1.356 (3)	C16—C20	1.401 (3)
N3—C11	1.327 (3)	C17—C18	1.392 (4)
N4—C17	1.325 (3)	C17—H17	0.9400
N4—C16	1.353 (3)	C18—C19	1.372 (4)
N5—C25	1.110 (6)	C18—H18	0.9400
C2—C3	1.514 (5)	C19—C20	1.423 (4)
C2—H2A	0.9800	C19—C24	1.497 (4)
C2—H2B	0.9800	C20—C21	1.429 (4)
C3—H3A	0.9700	C21—C22	1.345 (4)
C3—H3B	0.9700	C21—H21	0.9400
C3—H3C	0.9700	C22—H22	0.9400
C4—C5	1.512 (5)	C23—H23A	0.9700
C4—H4A	0.9800	C23—H23B	0.9700
C4—H4B	0.9800	C23—H23C	0.9700
C5—H5A	0.9700	C24—H24A	0.9700
C5—H5B	0.9700	C24—H24B	0.9700
C5—H5C	0.9700	C24—H24C	0.9700
C7—C8	1.503 (6)	C25—C26	1.427 (7)
C7—H7A	0.9800	C26—H26A	0.9700
C7—H7B	0.9800	C26—H26B	0.9700
C8—H8A	0.9700	C26—H26C	0.9700
C8—H8B	0.9700
S1—Cd—S2	67.80 (2)	C7—C8—H8C	109.5
S1—Cd—S3	102.21 (2)	H8A—C8—H8C	109.5
S1—Cd—S4	151.09 (2)	H8B—C8—H8C	109.5
S1—Cd—N3	109.38 (5)	N2—C9—C10	111.2 (4)
S1—Cd—N4	90.79 (5)	N2—C9—H9A	109.4
S2—Cd—S3	122.05 (2)	C10—C9—H9A	109.4
S2—Cd—S4	94.11 (2)	N2—C9—H9B	109.4
S2—Cd—N3	93.52 (5)	C10—C9—H9B	109.4
S2—Cd—N4	145.75 (6)	H9A—C9—H9B	108.0
S3—Cd—S4	67.49 (2)	C9—C10—H10A	109.5
S3—Cd—N3	139.54 (5)	C9—C10—H10B	109.5
S3—Cd—N4	87.48 (5)	H10A—C10—H10B	109.5
S4—Cd—N3	93.50 (5)	C9—C10—H10C	109.5
S4—Cd—N4	114.71 (5)	H10A—C10—H10C	109.5
N3—Cd—N4	67.84 (7)	H10B—C10—H10C	109.5
Cd—S1—C1	88.00 (9)	N3—C11—C12	122.7 (3)
Cd—S2—C1	85.22 (9)	N3—C11—H11	118.6
Cd—S3—C6	86.83 (9)	C12—C11—H11	118.6
Cd—S4—C6	86.44 (9)	C13—C12—C11	121.2 (3)
C1—N1—C2	122.3 (3)	C13—C12—H12	119.4
C1—N1—C4	122.7 (2)	C11—C12—H12	119.4
C2—N1—C4	114.9 (2)	C12—C13—C14	117.2 (3)
C6—N2—C7	121.8 (3)	C12—C13—C23	121.1 (3)
C6—N2—C9	122.4 (3)	C14—C13—C23	121.7 (3)
C7—N2—C9	115.8 (3)	C22—C14—C15	118.6 (2)
C15—N3—C11	117.5 (2)	C22—C14—C13	123.1 (3)
C15—N3—Cd	118.97 (16)	C15—C14—C13	118.3 (3)
C11—N3—Cd	123.46 (18)	N3—C15—C16	117.0 (2)
C17—N4—C16	117.2 (2)	N3—C15—C14	123.1 (2)
C17—N4—Cd	123.88 (17)	C16—C15—C14	119.9 (2)
C16—N4—Cd	118.90 (16)	N4—C16—C15	117.1 (2)
S1—C1—S2	118.95 (15)	N4—C16—C20	123.6 (2)
S1—C1—N1	119.8 (2)	C15—C16—C20	119.3 (2)
S2—C1—N1	121.2 (2)	N4—C17—C18	123.6 (2)
C3—C2—N1	111.6 (3)	N4—C17—H17	118.2
C3—C2—H2A	109.3	C18—C17—H17	118.2
N1—C2—H2A	109.3	C19—C18—C17	120.1 (3)
C3—C2—H2B	109.3	C19—C18—H18	120.0
N1—C2—H2B	109.3	C17—C18—H18	120.0
H2A—C2—H2B	108.0	C18—C19—C20	117.8 (2)
C2—C3—H3A	109.5	C18—C19—C24	121.2 (3)
C2—C3—H3B	109.5	C20—C19—C24	121.0 (2)
H3A—C3—H3B	109.5	C19—C20—C16	117.7 (2)
C2—C3—H3C	109.5	C19—C20—C21	123.2 (2)
H3A—C3—H3C	109.5	C16—C20—C21	119.1 (2)
H3B—C3—H3C	109.5	C22—C21—C20	121.2 (3)
N1—C4—C5	112.0 (3)	C22—C21—H21	119.4
N1—C4—H4A	109.2	C20—C21—H21	119.4
C5—C4—H4A	109.2	C14—C22—C21	121.8 (3)
N1—C4—H4B	109.2	C14—C22—H22	119.1
C5—C4—H4B	109.2	C21—C22—H22	119.1
H4A—C4—H4B	107.9	C13—C23—H23A	109.5
C4—C5—H5A	109.5	C13—C23—H23B	109.5
C4—C5—H5B	109.5	H23A—C23—H23B	109.5
H5A—C5—H5B	109.5	C13—C23—H23C	109.5
C4—C5—H5C	109.5	H23A—C23—H23C	109.5
H5A—C5—H5C	109.5	H23B—C23—H23C	109.5
H5B—C5—H5C	109.5	C19—C24—H24A	109.5
S3—C6—S4	119.08 (15)	C19—C24—H24B	109.5
S3—C6—N2	120.4 (2)	H24A—C24—H24B	109.5
S4—C6—N2	120.5 (2)	C19—C24—H24C	109.5
N2—C7—C8	112.4 (3)	H24A—C24—H24C	109.5
N2—C7—H7A	109.1	H24B—C24—H24C	109.5
C8—C7—H7A	109.1	N5—C25—C26	178.3 (6)
N2—C7—H7B	109.1	C25—C26—H26A	109.5
C8—C7—H7B	109.1	C25—C26—H26B	109.5
H7A—C7—H7B	107.9	H26A—C26—H26B	109.5
C7—C8—H8A	109.5	C25—C26—H26C	109.5
C7—C8—H8B	109.5	H26A—C26—H26C	109.5
H8A—C8—H8B	109.5	H26B—C26—H26C	109.5