Diaquatetramethanolcobalt(II) sulfate

In the title compound, [Co(CH₃OH)₄(H₂O)₂]SO₄, the Co^II atom and S atom lie on special positions on a twofold rotation axis. The Co^II ion is six-coordinated by four O atoms of methanol mol­ecules and two water mol­ecules in a distorted octa­hedral geometry. The cations and anions are linked by hydrogen bonds into a three-dimensional supra­molecular network.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](S-O) = 0.002 Å
• R factor = 0.026
• wR factor = 0.079
• Data-to-parameter ratio = 18.0

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Co1
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         S1
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          2

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

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Diaquatetraethanolcobalt(II) sulfate

Crystal data

[Co(CH4O)4(H2O)2]SO4	Dx = 1.542 Mg m^−3
Mr = 319.19	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3c	Cell parameters from 15909 reflections
Hall symbol: -R 3 2"c	θ = 3.2–27.5°
a = 15.656 (2) Å	µ = 1.43 mm^−1
c = 29.144 (6) Å	T = 295 K
V = 6186.8 (17) Å^3	Prism, orange
Z = 18	0.32 × 0.25 × 0.18 mm
F(000) = 3006

Data collection

Rigaku R-AXIS RAPID diffractometer	1583 independent reflections
Radiation source: fine-focus sealed tube	1383 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.020
Detector resolution: 10 pixels mm^-1	θmax = 27.5°, θmin = 3.2°
ω scans	h = −20→19
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −17→20
Tmin = 0.657, Tmax = 0.783	l = −37→37
18840 measured reflections

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)] = 0.026	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.079	H atoms treated by a mixture of independent and constrained refinement
S = 1.08	w = 1/[σ^2(Fo^2) + (0.0486P)^2 + 4.4049P] where P = (Fo^2 + 2Fc^2)/3
1583 reflections	(Δ/σ)max < 0.001
88 parameters	Δρmax = 0.30 e Å^−3
5 restraints	Δρmin = −0.36 e Å^−3

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

	x	y	z	Uiso*/Ueq
Co1	0.339420 (18)	0.3333	0.0833	0.03261 (13)
S1	0.02523 (4)	0.3333	0.0833	0.02996 (15)
O1	0.44246 (9)	0.34726 (10)	0.03377 (4)	0.0461 (3)
O2	0.26321 (10)	0.18372 (11)	0.06918 (6)	0.0593 (4)
O3	0.10905 (9)	0.39292 (9)	0.05269 (4)	0.0406 (3)
O4	−0.06168 (9)	0.26858 (10)	0.05582 (4)	0.0516 (3)
O1W	0.25588 (11)	0.35362 (13)	0.03469 (4)	0.0570 (4)
C1	0.54615 (15)	0.4107 (2)	0.03263 (8)	0.0723 (7)
C2	0.16039 (17)	0.12499 (19)	0.06291 (10)	0.0809 (8)
H1	0.4186 (17)	0.3243 (16)	0.0078 (5)	0.069*
H2	0.284 (2)	0.1443 (18)	0.0668 (9)	0.089*
H1A	0.5624	0.4619	0.0104	0.108*
H1B	0.5774	0.3735	0.0243	0.108*
H1C	0.5688	0.4397	0.0624	0.108*
H2A	0.1308	0.1659	0.0643	0.121*
H2B	0.1332	0.0759	0.0866	0.121*
H2C	0.1472	0.0932	0.0335	0.121*
H1W1	0.2579 (19)	0.344 (2)	0.0065 (4)	0.085*
H1W2	0.2062 (14)	0.358 (2)	0.0410 (7)	0.085*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.03453 (16)	0.0423 (2)	0.02355 (19)	0.02117 (10)	−0.00208 (5)	−0.00417 (11)
S1	0.0340 (2)	0.0368 (3)	0.0201 (3)	0.01839 (14)	0.00121 (9)	0.00241 (18)
O1	0.0407 (6)	0.0653 (8)	0.0274 (6)	0.0228 (6)	0.0002 (5)	−0.0091 (5)
O2	0.0436 (7)	0.0447 (7)	0.0887 (12)	0.0214 (6)	−0.0103 (7)	−0.0160 (7)
O3	0.0388 (6)	0.0517 (7)	0.0307 (6)	0.0222 (5)	0.0069 (5)	0.0110 (5)
O4	0.0432 (7)	0.0578 (8)	0.0334 (6)	0.0098 (6)	−0.0085 (5)	0.0057 (6)
O1W	0.0659 (9)	0.1066 (12)	0.0261 (6)	0.0639 (9)	−0.0039 (6)	−0.0042 (7)
C1	0.0435 (11)	0.0927 (18)	0.0597 (13)	0.0184 (12)	0.0038 (10)	−0.0171 (13)
C2	0.0482 (12)	0.0597 (14)	0.121 (2)	0.0168 (11)	−0.0246 (14)	−0.0195 (14)

Geometric parameters (Å, º)

Co1—O1	2.0940 (12)	O1—H1	0.842 (10)
Co1—O2	2.0703 (15)	O2—C2	1.411 (3)
Co1—O1W	2.0584 (13)	O2—H2	0.83 (3)
Co1—O1^i	2.0940 (12)	O1W—H1W1	0.839 (13)
Co1—O2^i	2.0702 (15)	O1W—H1W2	0.84 (3)
Co1—O1W^i	2.0583 (13)	C1—H1A	0.9600
S1—O3	1.4716 (12)	C1—H1B	0.9600
S1—O4	1.4638 (12)	C1—H1C	0.9600
S1—O3^i	1.4716 (12)	C2—H2A	0.9600
S1—O4^i	1.4637 (12)	C2—H2B	0.9600
O1—C1	1.418 (2)	C2—H2C	0.9600
O1—Co1—O1^i	88.16 (7)	O1—C1—H1C	109.5
O2—Co1—O1	87.62 (6)	O2—C2—H2A	109.5
O2^i—Co1—O1	93.25 (6)	O2—C2—H2B	109.5
O2^i—Co1—O2	178.79 (8)	O2—C2—H2C	109.5
O1W—Co1—O1	91.42 (5)	O3—S1—O3^i	109.83 (10)
O1W^i—Co1—O1	177.48 (6)	O4^i—S1—O4	108.64 (13)
O1W—Co1—O2	89.21 (7)	O4^i—S1—O3	109.78 (7)
O1W^i—Co1—O2	89.93 (6)	O4—S1—O3	109.40 (7)
O2—Co1—O1^i	93.25 (6)	O4^i—S1—O3^i	109.40 (7)
O2^i—Co1—O1^i	87.62 (6)	O4—S1—O3^i	109.78 (7)
O1W^i—Co1—O1^i	91.42 (5)	C1—O1—Co1	129.92 (12)
O1W—Co1—O1^i	177.49 (6)	C1—O1—H1	112.7 (17)
O1W^i—Co1—O2^i	89.21 (6)	C2—O2—Co1	125.98 (15)
O1W—Co1—O2^i	89.93 (6)	C2—O2—H2	104 (2)
O1W^i—Co1—O1W	89.11 (8)	H1A—C1—H1B	109.5
Co1—O1W—H1W1	124.1 (17)	H1A—C1—H1C	109.5
Co1—O1W—H1W2	123.4 (16)	H1B—C1—H1C	109.5
Co1—O2—H2	130 (2)	H2A—C2—H2B	109.5
Co1—O1—H1	115.0 (17)	H2A—C2—H2C	109.5
O1—C1—H1A	109.5	H2B—C2—H2C	109.5
O1—C1—H1B	109.5	H1W1—O1W—H1W2	110.7 (15)
O1W—Co1—O1—C1	126.2 (2)	O1W^i—Co1—O2—C2	45.6 (2)
O2^i—Co1—O1—C1	36.2 (2)	O1W—Co1—O2—C2	−43.5 (2)
O2—Co1—O1—C1	−144.6 (2)	O1—Co1—O2—C2	−135.0 (2)
O1^i—Co1—O1—C1	−51.29 (18)	O1^i—Co1—O2—C2	137.0 (2)

Symmetry code: (i) x−y+1/3, −y+2/3, −z+1/6.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1W1···O4^ii	0.84 (1)	1.85 (1)	2.6839 (18)	176 (3)
O1W—H1W2···O3	0.84 (3)	1.89 (3)	2.7117 (17)	170 (3)
O1—H1···O3^ii	0.84 (3)	1.85 (3)	2.6770 (16)	168 (2)
O2—H2···O4^iii	0.83 (3)	1.83 (3)	2.629 (2)	174 (3)

Symmetry codes: (ii) y, −x+y, −z; (iii) −x+y, −x, z.