Crystal structure of hexa­kis­(dimethyl sulfoxide-κO)cobalt(II) bis­[tri­chlorido­(quinoline-κN)cobaltate(II)]

Anhydrous cobalt(II) chloride reacts with quinoline (C₉H₇N) in dimethyl sulfoxide (Me₂SO) to form the novel complex salt [Co^II(Me₂SO)₆][Co^IICl₃quinoline]₂. The compound comprises an octa­hedral homoleptic Me₂SO-solvated cobalt(II) cation and a tetra­hedral cobaltate(II) anion attached to three chloro ligands and one quinoline moiety.

Key indicators

• Single-crystal X-ray study
• T = 230 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.045
• wR factor = 0.116
• Data-to-parameter ratio = 30.1

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT230_ALERT_2_B Hirshfeld Test Diff for   C1       --C2        .       10.0 s.u.
PLAT230_ALERT_2_B Hirshfeld Test Diff for   C5       --C6        .       17.5 s.u.
PLAT230_ALERT_2_B Hirshfeld Test Diff for   C6       --C7        .        8.2 s.u.

Alert level C
PLAT230_ALERT_2_C Hirshfeld Test Diff for   N        --C9        .        7.0 s.u.
PLAT241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of         C2 Check
PLAT241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of         C5 Check
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of         S2 Check
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        Co1 Check
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of         C6 Check
PLAT341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.00633 Ang.
PLAT905_ALERT_3_C Negative K value in the Analysis of Variance ...     -1.340 Report
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Info

Alert level G
PLAT154_ALERT_1_G The s.u.'s on the Cell Angles are Equal ..(Note)      0.002 Degree
PLAT794_ALERT_5_G Tentative Bond Valency for Co2       (II)      .       2.05 Info
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         44 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   3 ALERT level B = A potentially serious problem, consider carefully
   9 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   3 ALERT level G = General information/check it is not something unexpected

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  10 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
   1 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check

---

Computing details

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT (Bruker, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Hexakis(dimethyl sulfoxide-κO)cobalt(II) bis[trichlorido(quinoline-κN)cobaltate(II)]

Crystal data

[Co(C2H6OS)6][CoCl3(C9H7N)]2	Z = 1
Mr = 1116.57	F(000) = 571
Triclinic, P1	Dx = 1.515 Mg m^−3
a = 8.3182 (13) Å	Mo Kα radiation, λ = 0.71073 Å
b = 9.6130 (15) Å	Cell parameters from 7471 reflections
c = 15.595 (2) Å	θ = 2.4–30.1°
α = 81.767 (2)°	µ = 1.63 mm^−1
β = 82.776 (2)°	T = 230 K
γ = 87.183 (2)°	Block, blue
V = 1223.7 (3) Å^3	0.39 × 0.12 × 0.05 mm

Data collection

Bruker APEXII CCD diffractometer	4839 reflections with I > 2σ(I)
φ and ω scans	Rint = 0.035
Absorption correction: multi-scan (SADABS; Bruker, 2008)	θmax = 30.5°, θmin = 1.3°
Tmin = 0.626, Tmax = 0.746	h = −11→11
19375 measured reflections	k = −13→13
7447 independent reflections	l = −22→22

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.045	H-atom parameters constrained
wR(F^2) = 0.116	w = 1/[σ^2(Fo^2) + (0.0457P)^2 + 0.7087P] where P = (Fo^2 + 2Fc^2)/3
S = 1.02	(Δ/σ)max < 0.001
7447 reflections	Δρmax = 0.77 e Å^−3
247 parameters	Δρmin = −0.46 e Å^−3

Special details

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.

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

	x	y	z	Uiso*/Ueq
Co1	0.56334 (6)	0.57989 (4)	0.70199 (3)	0.04816 (13)
Co2	0.0000	0.0000	1.0000	0.02575 (11)
Cl1	0.56412 (18)	0.34385 (10)	0.71205 (7)	0.0874 (4)
Cl2	0.81055 (11)	0.65246 (10)	0.64138 (7)	0.0647 (2)
Cl3	0.48261 (13)	0.64884 (10)	0.83322 (6)	0.0659 (3)
N	0.3997 (3)	0.6584 (3)	0.61758 (17)	0.0502 (6)
S1	−0.13554 (8)	0.28530 (7)	0.90892 (5)	0.04024 (17)
S2	−0.09070 (8)	−0.10708 (7)	0.82809 (5)	0.03584 (16)
S3	0.31946 (7)	0.11911 (7)	0.89997 (4)	0.03205 (15)
O1	−0.0198 (2)	0.22294 (17)	0.97373 (12)	0.0334 (4)
O2	−0.0073 (2)	0.00114 (19)	0.86695 (12)	0.0366 (4)
O3	0.2483 (2)	0.01632 (18)	0.97778 (12)	0.0340 (4)
C1	0.3345 (5)	0.5732 (4)	0.5722 (3)	0.0657 (10)
H1A	0.3652	0.4773	0.5809	0.079*
C2	0.2274 (6)	0.6144 (7)	0.5145 (3)	0.0948 (17)
H2A	0.1791	0.5472	0.4885	0.114*
C3	0.1909 (5)	0.7490 (7)	0.4948 (3)	0.0865 (15)
H3A	0.1210	0.7776	0.4522	0.104*
C4	0.2547 (4)	0.8511 (5)	0.5364 (2)	0.0667 (11)
C5	0.2245 (6)	1.0016 (6)	0.5210 (3)	0.0875 (15)
H5A	0.1511	1.0396	0.4821	0.105*
C6	0.2971 (4)	1.0822 (5)	0.5601 (2)	0.0621 (10)
H6A	0.2807	1.1796	0.5447	0.074*
C7	0.3967 (5)	1.0394 (4)	0.6224 (3)	0.0706 (11)
H7A	0.4403	1.1045	0.6519	0.085*
C8	0.4309 (4)	0.8990 (4)	0.6405 (2)	0.0610 (9)
H8A	0.5021	0.8674	0.6820	0.073*
C9	0.3626 (4)	0.8004 (4)	0.5987 (2)	0.0534 (8)
C11	−0.0084 (5)	0.3546 (4)	0.8131 (2)	0.0638 (10)
H11A	−0.0742	0.4082	0.7720	0.096*
H11B	0.0482	0.2779	0.7866	0.096*
H11C	0.0699	0.4154	0.8286	0.096*
C12	−0.2066 (4)	0.4461 (3)	0.9459 (3)	0.0588 (9)
H12A	−0.2738	0.4975	0.9047	0.088*
H12B	−0.1149	0.5020	0.9504	0.088*
H12C	−0.2699	0.4266	1.0026	0.088*
C21	0.0638 (5)	−0.2325 (4)	0.8012 (2)	0.0618 (9)
H21A	0.0252	−0.2929	0.7638	0.093*
H21B	0.0920	−0.2890	0.8542	0.093*
H21C	0.1587	−0.1844	0.7708	0.093*
C22	−0.1126 (5)	−0.0229 (4)	0.7210 (2)	0.0601 (9)
H22A	−0.1599	−0.0871	0.6892	0.090*
H22B	−0.0071	0.0041	0.6910	0.090*
H22C	−0.1828	0.0602	0.7242	0.090*
C31	0.3992 (4)	0.2550 (3)	0.9467 (2)	0.0536 (8)
H31A	0.4504	0.3230	0.9006	0.080*
H31B	0.4788	0.2149	0.9844	0.080*
H31C	0.3121	0.3012	0.9805	0.080*
C32	0.5044 (3)	0.0349 (3)	0.8624 (2)	0.0442 (7)
H32A	0.5610	0.0958	0.8142	0.066*
H32B	0.4817	−0.0527	0.8429	0.066*
H32C	0.5715	0.0156	0.9095	0.066*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0638 (3)	0.0365 (2)	0.0456 (3)	−0.00097 (19)	−0.0139 (2)	−0.00423 (18)
Co2	0.0226 (2)	0.0228 (2)	0.0314 (3)	−0.00025 (17)	−0.00292 (18)	−0.00259 (18)
Cl1	0.1588 (12)	0.0370 (5)	0.0626 (6)	−0.0162 (6)	−0.0005 (6)	−0.0004 (4)
Cl2	0.0591 (5)	0.0601 (5)	0.0769 (6)	−0.0037 (4)	−0.0140 (4)	−0.0104 (4)
Cl3	0.0886 (7)	0.0612 (5)	0.0506 (5)	0.0280 (5)	−0.0216 (4)	−0.0151 (4)
N	0.0579 (16)	0.0548 (17)	0.0405 (14)	−0.0099 (13)	−0.0111 (12)	−0.0073 (12)
S1	0.0376 (4)	0.0294 (3)	0.0545 (4)	0.0028 (3)	−0.0158 (3)	−0.0006 (3)
S2	0.0322 (3)	0.0401 (4)	0.0366 (4)	−0.0029 (3)	−0.0049 (3)	−0.0090 (3)
S3	0.0250 (3)	0.0296 (3)	0.0396 (4)	−0.0002 (2)	−0.0032 (3)	0.0012 (3)
O1	0.0318 (9)	0.0231 (8)	0.0447 (11)	0.0014 (7)	−0.0088 (8)	0.0001 (7)
O2	0.0448 (11)	0.0338 (10)	0.0317 (10)	−0.0067 (8)	−0.0041 (8)	−0.0049 (8)
O3	0.0232 (8)	0.0339 (10)	0.0420 (10)	−0.0012 (7)	−0.0027 (7)	0.0039 (8)
C1	0.061 (2)	0.066 (2)	0.079 (3)	−0.0140 (18)	−0.024 (2)	−0.022 (2)
C2	0.082 (3)	0.143 (5)	0.074 (3)	−0.030 (3)	−0.008 (2)	−0.056 (3)
C3	0.069 (3)	0.147 (5)	0.050 (2)	−0.008 (3)	−0.023 (2)	−0.023 (3)
C4	0.051 (2)	0.112 (3)	0.0344 (18)	−0.003 (2)	−0.0007 (15)	−0.0031 (19)
C5	0.078 (3)	0.110 (4)	0.059 (3)	0.031 (3)	−0.009 (2)	0.030 (3)
C6	0.056 (2)	0.083 (3)	0.0409 (19)	−0.0063 (19)	−0.0049 (16)	0.0146 (18)
C7	0.074 (3)	0.057 (2)	0.077 (3)	−0.0079 (19)	−0.005 (2)	0.000 (2)
C8	0.062 (2)	0.061 (2)	0.059 (2)	−0.0091 (17)	−0.0185 (17)	0.0077 (17)
C9	0.0495 (18)	0.073 (2)	0.0360 (17)	−0.0071 (16)	−0.0040 (14)	−0.0008 (16)
C11	0.078 (2)	0.053 (2)	0.054 (2)	0.0094 (18)	−0.0079 (18)	0.0151 (16)
C12	0.0554 (19)	0.0396 (17)	0.083 (3)	0.0199 (15)	−0.0223 (18)	−0.0105 (17)
C21	0.074 (2)	0.0475 (19)	0.068 (2)	0.0225 (17)	−0.0182 (19)	−0.0216 (17)
C22	0.082 (3)	0.060 (2)	0.0423 (18)	0.0125 (18)	−0.0244 (17)	−0.0116 (16)
C31	0.065 (2)	0.0356 (16)	0.060 (2)	−0.0148 (15)	0.0069 (16)	−0.0121 (15)
C32	0.0398 (15)	0.0405 (16)	0.0468 (17)	0.0067 (12)	0.0089 (13)	−0.0023 (13)

Geometric parameters (Å, º)

Co1—N	2.054 (3)	C4—C5	1.446 (6)
Co1—Cl1	2.2517 (10)	C5—C6	1.269 (6)
Co1—Cl2	2.2521 (11)	C5—H5A	0.9400
Co1—Cl3	2.2534 (10)	C6—C7	1.362 (5)
Co2—O3	2.0606 (17)	C6—H6A	0.9400
Co2—O3^i	2.0607 (17)	C7—C8	1.362 (5)
Co2—O2^i	2.0818 (18)	C7—H7A	0.9400
Co2—O2	2.0819 (18)	C8—C9	1.404 (5)
Co2—O1^i	2.1258 (17)	C8—H8A	0.9400
Co2—O1	2.1258 (17)	C11—H11A	0.9700
N—C1	1.331 (4)	C11—H11B	0.9700
N—C9	1.383 (4)	C11—H11C	0.9700
S1—O1	1.5236 (18)	C12—H12A	0.9700
S1—C12	1.775 (3)	C12—H12B	0.9700
S1—C11	1.784 (4)	C12—H12C	0.9700
S2—O2	1.5127 (19)	C21—H21A	0.9700
S2—C21	1.772 (3)	C21—H21B	0.9700
S2—C22	1.776 (3)	C21—H21C	0.9700
S3—O3	1.5273 (19)	C22—H22A	0.9700
S3—C32	1.775 (3)	C22—H22B	0.9700
S3—C31	1.776 (3)	C22—H22C	0.9700
C1—C2	1.351 (6)	C31—H31A	0.9700
C1—H1A	0.9400	C31—H31B	0.9700
C2—C3	1.316 (7)	C31—H31C	0.9700
C2—H2A	0.9400	C32—H32A	0.9700
C3—C4	1.410 (6)	C32—H32B	0.9700
C3—H3A	0.9400	C32—H32C	0.9700
C4—C9	1.424 (5)
N—Co1—Cl1	107.09 (9)	C4—C5—H5A	120.0
N—Co1—Cl2	107.76 (8)	C5—C6—C7	125.4 (4)
Cl1—Co1—Cl2	108.21 (5)	C5—C6—H6A	117.3
N—Co1—Cl3	108.80 (8)	C7—C6—H6A	117.3
Cl1—Co1—Cl3	110.46 (4)	C6—C7—C8	117.8 (4)
Cl2—Co1—Cl3	114.26 (4)	C6—C7—H7A	121.1
O3—Co2—O3^i	180.0	C8—C7—H7A	121.1
O3—Co2—O2^i	90.17 (7)	C7—C8—C9	121.6 (4)
O3^i—Co2—O2^i	89.83 (7)	C7—C8—H8A	119.2
O3—Co2—O2	89.83 (7)	C9—C8—H8A	119.2
O3^i—Co2—O2	90.17 (7)	N—C9—C8	120.7 (3)
O2^i—Co2—O2	180.00 (10)	N—C9—C4	121.2 (3)
O3—Co2—O1^i	91.82 (7)	C8—C9—C4	118.0 (4)
O3^i—Co2—O1^i	88.19 (7)	S1—C11—H11A	109.5
O2^i—Co2—O1^i	86.29 (7)	S1—C11—H11B	109.5
O2—Co2—O1^i	93.71 (7)	H11A—C11—H11B	109.5
O3—Co2—O1	88.18 (7)	S1—C11—H11C	109.5
O3^i—Co2—O1	91.81 (7)	H11A—C11—H11C	109.5
O2^i—Co2—O1	93.71 (7)	H11B—C11—H11C	109.5
O2—Co2—O1	86.29 (7)	S1—C12—H12A	109.5
O1^i—Co2—O1	180.000 (19)	S1—C12—H12B	109.5
C1—N—C9	116.5 (3)	H12A—C12—H12B	109.5
C1—N—Co1	120.2 (3)	S1—C12—H12C	109.5
C9—N—Co1	123.0 (2)	H12A—C12—H12C	109.5
O1—S1—C12	103.99 (14)	H12B—C12—H12C	109.5
O1—S1—C11	105.22 (15)	S2—C21—H21A	109.5
C12—S1—C11	98.78 (18)	S2—C21—H21B	109.5
O2—S2—C21	105.12 (15)	H21A—C21—H21B	109.5
O2—S2—C22	103.28 (15)	S2—C21—H21C	109.5
C21—S2—C22	98.54 (18)	H21A—C21—H21C	109.5
O3—S3—C32	103.92 (12)	H21B—C21—H21C	109.5
O3—S3—C31	104.93 (13)	S2—C22—H22A	109.5
C32—S3—C31	98.99 (16)	S2—C22—H22B	109.5
S1—O1—Co2	117.12 (10)	H22A—C22—H22B	109.5
S2—O2—Co2	124.52 (11)	S2—C22—H22C	109.5
S3—O3—Co2	118.17 (10)	H22A—C22—H22C	109.5
N—C1—C2	124.9 (4)	H22B—C22—H22C	109.5
N—C1—H1A	117.6	S3—C31—H31A	109.5
C2—C1—H1A	117.6	S3—C31—H31B	109.5
C3—C2—C1	119.7 (4)	H31A—C31—H31B	109.5
C3—C2—H2A	120.2	S3—C31—H31C	109.5
C1—C2—H2A	120.2	H31A—C31—H31C	109.5
C2—C3—C4	121.2 (4)	H31B—C31—H31C	109.5
C2—C3—H3A	119.4	S3—C32—H32A	109.5
C4—C3—H3A	119.4	S3—C32—H32B	109.5
C3—C4—C9	116.3 (4)	H32A—C32—H32B	109.5
C3—C4—C5	126.7 (4)	S3—C32—H32C	109.5
C9—C4—C5	117.0 (4)	H32A—C32—H32C	109.5
C6—C5—C4	120.0 (4)	H32B—C32—H32C	109.5
C6—C5—H5A	120.0
C12—S1—O1—Co2	148.84 (16)	C4—C5—C6—C7	−5.0 (7)
C11—S1—O1—Co2	−107.81 (16)	C5—C6—C7—C8	4.8 (6)
C21—S2—O2—Co2	−95.18 (18)	C6—C7—C8—C9	−1.9 (6)
C22—S2—O2—Co2	162.00 (16)	C1—N—C9—C8	−177.3 (3)
C32—S3—O3—Co2	−145.35 (14)	Co1—N—C9—C8	−3.1 (4)
C31—S3—O3—Co2	111.19 (15)	C1—N—C9—C4	2.5 (5)
C9—N—C1—C2	−4.9 (6)	Co1—N—C9—C4	176.7 (2)
Co1—N—C1—C2	−179.3 (4)	C7—C8—C9—N	179.6 (3)
N—C1—C2—C3	5.5 (7)	C7—C8—C9—C4	−0.3 (5)
C1—C2—C3—C4	−3.5 (8)	C3—C4—C9—N	−0.9 (5)
C2—C3—C4—C9	1.4 (6)	C5—C4—C9—N	−179.7 (3)
C2—C3—C4—C5	−180.0 (4)	C3—C4—C9—C8	178.9 (3)
C3—C4—C5—C6	−176.3 (4)	C5—C4—C9—C8	0.2 (5)
C9—C4—C5—C6	2.3 (6)

Symmetry code: (i) −x, −y, −z+2.