Bis(1,10-phenanthroline-κ(2) N,N')(sulfato-κ(2) O,O')cobalt(II) propane-1,2-diol monosolvate.

In the title compound, [Co(SO4)(C12H8N2)2]·C3H8O2, the Co(II) atom (site symmetry 2) has a distorted octa-hedral coordination composed of four N atoms from two chelating 1,10-phenanthroline ligands and two O atoms from an O,O'-bidentate sulfate ligand, in which the S atom has site symmetry 2. The dihedral angle between the two chelating N2C2 groups is 84.46 (15)°. The complex and solvent mol-ecules are connected through O-H⋯O hydrogen bonds. The solvent mol-ecule is equally disordered over two positions and is also located on a twofold axis.

Related literature

The title complex has been reported with other solvant mol­ecules. In the case of ethane-1,2-diol, see: Zhong et al. (2006 ▶); for n class="Chemical">propane-1,3-diol, see: Zhong (2010 ▶); for butane-2,3-diol, see: Wang & Zhong (2011 ▶). For crystal engineering aspects of coordination framework structures, see: Batten & Robson (1998 ▶); Robin & Fromm (2006 ▶).

Experimental

Crystal data

[Co(SO4)(C12H8N2)2]·n class="Chemical">C3H8O2

M = 591.49

Monoclinic,

a = 18.117 (4) Å

b = 12.987 (3) Å

c = 12.881 (3) Å

β = 121.46 (3)°

V = 2585.2 (13) Å3

Z = 4

Mo Kα radiation

μ = 0.80 mm−1

T = 223 K

0.35 × 0.34 × 0.25 mm

Data collection

Rigaku Mercury CCD diffractometer

Absorption correction: multi-scan (REQAB; Jacobson, 1998 ▶) T min = 0.373, T max = 1.000

11477 measured reflections

2284 independent reflections

1465 reflections with I > 2/s(I)

R int = 0.100

Refinement

R[F 2 > 2σ(F 2)] = 0.052

wR(F 2) = 0.129

S = 0.95

2284 reflections

193 parameters

38 restraints

H-atom parameters constrained

Δρmax = 0.37 e Å−3

Δρmin = −0.39 e Å−3

Data collection: CrystalClear (Rigaku, 2007 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP in SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Click here for additional data file.

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812049616/vn2062sup1.cif

Click here for additional data file.

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812049616/vn2062Isup2.hkl

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

[Co(SO4)(C12H8N2)2]·C3H8O2	F(000) = 1220
Mr = 591.49	Dx = 1.520 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 5104 reflections
a = 18.117 (4) Å	θ = 3.1–25.4°
b = 12.987 (3) Å	µ = 0.80 mm−1
c = 12.881 (3) Å	T = 223 K
β = 121.46 (3)°	Block, red
V = 2585.2 (13) Å3	0.35 × 0.34 × 0.25 mm
Z = 4

Rigaku Mercury CCD diffractometer	2284 independent reflections
Radiation source: fine-focus sealed tube	1465 reflections with I > 2/s(I)
Graphite Monochromator monochromator	Rint = 0.100
Detector resolution: 28.5714 pixels mm-1	θmax = 25.0°, θmin = 3.1°
ω scans	h = −20→21
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	k = −14→15
Tmin = 0.373, Tmax = 1.000	l = −15→15
11477 measured reflections

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.052	H-atom parameters constrained
wR(F2) = 0.129	w = 1/[σ2(Fo2) + (0.0385P)2] where P = (Fo2 + 2Fc2)/3
S = 0.95	(Δ/σ)max = 0.001
2284 reflections	Δρmax = 0.37 e Å−3
193 parameters	Δρmin = −0.39 e Å−3
38 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0060 (5)

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	Occ. (<1)
Co1	0.0000	0.32137 (6)	0.2500	0.0348 (3)
S1	0.0000	0.52899 (11)	0.2500	0.0344 (4)
O1	0.0533 (2)	0.4578 (2)	0.3537 (3)	0.0495 (9)
O2	−0.0552 (2)	0.5929 (2)	0.2742 (3)	0.0604 (10)
O3	−0.0492 (7)	0.7963 (6)	0.3204 (8)	0.071 (3)	0.50
H3	−0.0428	0.7424	0.2931	0.106*	0.50
O3'	−0.0869 (6)	0.7996 (6)	0.2438 (10)	0.097 (4)	0.50
H3'	−0.0613	0.7472	0.2804	0.145*	0.50
N1	0.0830 (2)	0.3000 (3)	0.1814 (3)	0.0379 (9)
N2	0.0959 (2)	0.2178 (2)	0.3803 (3)	0.0363 (9)
C1	0.0774 (3)	0.3442 (4)	0.0841 (4)	0.0459 (12)
H1A	0.0340	0.3924	0.0406	0.055*
C2	0.1339 (3)	0.3208 (4)	0.0454 (5)	0.0537 (14)
H2A	0.1284	0.3535	−0.0225	0.064*
C3	0.1977 (3)	0.2495 (4)	0.1074 (5)	0.0555 (14)
H3A	0.2354	0.2331	0.0814	0.067*
C4	0.2061 (3)	0.2012 (3)	0.2104 (4)	0.0419 (12)
C5	0.2732 (3)	0.1286 (4)	0.2841 (5)	0.0538 (14)
H5A	0.3117	0.1082	0.2608	0.065*
C6	0.2814 (3)	0.0902 (4)	0.3853 (5)	0.0493 (13)
H6A	0.3258	0.0440	0.4320	0.059*
C7	0.2225 (3)	0.1189 (3)	0.4240 (4)	0.0402 (11)
C8	0.2298 (3)	0.0829 (3)	0.5312 (4)	0.0506 (13)
H8A	0.2738	0.0375	0.5816	0.061*
C9	0.1723 (3)	0.1150 (4)	0.5605 (4)	0.0546 (14)
H9A	0.1767	0.0924	0.6320	0.065*
C10	0.1062 (3)	0.1819 (3)	0.4833 (4)	0.0468 (13)
H10A	0.0671	0.2026	0.5053	0.056*
C11	0.1546 (3)	0.1866 (3)	0.3517 (4)	0.0320 (10)
C12	0.1473 (3)	0.2300 (3)	0.2447 (4)	0.0341 (11)
C13	−0.0288 (6)	0.8772 (5)	0.2729 (9)	0.139 (3)	0.50
H13	−0.0837	0.8822	0.1948	0.167*	0.50
C13'	−0.0288 (6)	0.8772 (5)	0.2729 (9)	0.139 (3)	0.50
H13A	0.0069	0.8799	0.3610	0.167*	0.50
H13B	−0.0613	0.9411	0.2467	0.167*	0.50
C14	−0.0305 (12)	0.9804 (8)	0.3222 (18)	0.168 (9)	0.50
H14A	0.0001	1.0290	0.3021	0.252*	0.50
H14B	−0.0032	0.9762	0.4091	0.252*	0.50
H14C	−0.0894	1.0025	0.2872	0.252*	0.50

	U11	U22	U33	U12	U13	U23
Co1	0.0323 (5)	0.0367 (5)	0.0407 (6)	0.000	0.0228 (5)	0.000
S1	0.0282 (9)	0.0352 (9)	0.0424 (10)	0.000	0.0203 (8)	0.000
O1	0.048 (2)	0.0428 (18)	0.038 (2)	−0.0012 (15)	0.0091 (17)	0.0020 (15)
O2	0.060 (2)	0.049 (2)	0.095 (3)	0.0103 (17)	0.056 (2)	−0.0082 (19)
O3	0.111 (7)	0.050 (5)	0.077 (6)	0.005 (4)	0.068 (5)	−0.001 (4)
O3'	0.110 (7)	0.067 (6)	0.126 (8)	0.026 (5)	0.070 (6)	0.023 (6)
N1	0.038 (2)	0.042 (2)	0.041 (2)	0.0010 (17)	0.026 (2)	0.0036 (18)
N2	0.041 (2)	0.036 (2)	0.042 (2)	−0.0010 (17)	0.029 (2)	0.0011 (17)
C1	0.041 (3)	0.056 (3)	0.044 (3)	0.003 (2)	0.024 (3)	0.007 (2)
C2	0.054 (3)	0.070 (4)	0.046 (3)	0.003 (3)	0.033 (3)	0.008 (3)
C3	0.050 (3)	0.080 (4)	0.052 (3)	0.004 (3)	0.038 (3)	−0.003 (3)
C4	0.036 (3)	0.057 (3)	0.036 (3)	0.004 (2)	0.021 (2)	−0.002 (2)
C5	0.044 (3)	0.073 (4)	0.050 (3)	0.018 (3)	0.028 (3)	−0.001 (3)
C6	0.037 (3)	0.059 (3)	0.047 (3)	0.015 (2)	0.018 (3)	0.001 (3)
C7	0.036 (3)	0.042 (3)	0.038 (3)	0.005 (2)	0.017 (2)	0.002 (2)
C8	0.046 (3)	0.049 (3)	0.047 (3)	0.007 (2)	0.018 (3)	0.006 (2)
C9	0.063 (4)	0.059 (3)	0.046 (3)	0.005 (3)	0.031 (3)	0.015 (3)
C10	0.056 (3)	0.050 (3)	0.049 (3)	0.003 (2)	0.038 (3)	0.005 (2)
C11	0.033 (3)	0.031 (2)	0.034 (3)	−0.0038 (19)	0.019 (2)	−0.0020 (19)
C12	0.027 (3)	0.041 (3)	0.034 (3)	−0.001 (2)	0.015 (2)	−0.002 (2)
C13	0.195 (9)	0.076 (5)	0.215 (9)	0.002 (5)	0.155 (7)	−0.006 (6)
C13'	0.195 (9)	0.076 (5)	0.215 (9)	0.002 (5)	0.155 (7)	−0.006 (6)
C14	0.20 (2)	0.069 (10)	0.32 (3)	−0.029 (11)	0.19 (2)	−0.032 (14)

Co1—O1	2.124 (3)	C3—C4	1.402 (6)
Co1—O1i	2.124 (3)	C3—H3A	0.9300
Co1—N1	2.123 (3)	C4—C12	1.400 (6)
Co1—N1i	2.123 (3)	C4—C5	1.437 (6)
Co1—N2i	2.145 (4)	C5—C6	1.330 (6)
Co1—N2	2.145 (4)	C5—H5A	0.9300
Co1—S1	2.6964 (18)	C6—C7	1.442 (6)
S1—O2i	1.453 (3)	C6—H6A	0.9300
S1—O2	1.453 (3)	C7—C11	1.399 (6)
S1—O1i	1.492 (3)	C7—C8	1.397 (6)
S1—O1	1.492 (3)	C8—C9	1.346 (6)
O3—C13	1.361 (4)	C8—H8A	0.9300
O3—H3	0.8200	C9—C10	1.391 (6)
O3'—H3'	0.8200	C9—H9A	0.9300
N1—C1	1.333 (5)	C10—H10A	0.9300
N1—C12	1.363 (5)	C11—C12	1.430 (6)
N2—C10	1.324 (5)	C13—C13i	1.443 (7)
N2—C11	1.356 (5)	C13—C14	1.489 (9)
C1—C2	1.386 (6)	C13—H13	0.9800
C1—H1A	0.9300	C14—H14A	0.9600
C2—C3	1.366 (6)	C14—H14B	0.9600
C2—H2A	0.9300	C14—H14C	0.9600
O1—Co1—O1i	66.91 (16)	C1—C2—H2A	120.2
O1—Co1—N1	100.51 (13)	C2—C3—C4	119.9 (4)
O1i—Co1—N1	92.02 (13)	C2—C3—H3A	120.1
O1—Co1—N1i	92.02 (13)	C4—C3—H3A	120.1
O1i—Co1—N1i	100.51 (13)	C12—C4—C3	117.0 (4)
N1—Co1—N1i	165.01 (18)	C12—C4—C5	119.2 (4)
O1—Co1—N2i	158.77 (12)	C3—C4—C5	123.8 (4)
O1i—Co1—N2i	96.57 (12)	C6—C5—C4	121.1 (4)
N1—Co1—N2i	93.03 (13)	C6—C5—H5A	119.5
N1i—Co1—N2i	77.50 (13)	C4—C5—H5A	119.5
O1—Co1—N2	96.57 (12)	C5—C6—C7	121.2 (4)
O1i—Co1—N2	158.77 (12)	C5—C6—H6A	119.4
N1—Co1—N2	77.50 (13)	C7—C6—H6A	119.4
N1i—Co1—N2	93.03 (13)	C11—C7—C8	117.7 (4)
N2i—Co1—N2	102.31 (18)	C11—C7—C6	119.0 (4)
O1—Co1—S1	33.45 (8)	C8—C7—C6	123.3 (4)
O1i—Co1—S1	33.45 (8)	C9—C8—C7	119.0 (4)
N1—Co1—S1	97.50 (9)	C9—C8—H8A	120.5
N1i—Co1—S1	97.50 (9)	C7—C8—H8A	120.5
N2i—Co1—S1	128.85 (9)	C8—C9—C10	119.7 (5)
N2—Co1—S1	128.85 (9)	C8—C9—H9A	120.1
O2i—S1—O2	110.3 (3)	C10—C9—H9A	120.1
O2i—S1—O1i	111.01 (19)	N2—C10—C9	123.8 (4)
O2—S1—O1i	110.46 (19)	N2—C10—H10A	118.1
O2i—S1—O1	110.46 (19)	C9—C10—H10A	118.1
O2—S1—O1	111.01 (19)	N2—C11—C7	123.3 (4)
O1i—S1—O1	103.4 (2)	N2—C11—C12	116.9 (4)
O2i—S1—Co1	124.83 (13)	C7—C11—C12	119.7 (4)
O2—S1—Co1	124.83 (13)	N1—C12—C4	122.9 (4)
O1i—S1—Co1	51.70 (12)	N1—C12—C11	117.4 (4)
O1—S1—Co1	51.70 (12)	C4—C12—C11	119.8 (4)
S1—O1—Co1	94.85 (16)	O3—C13—C13i	127.5 (5)
C13—O3—H3	109.5	O3—C13—C14	115.6 (8)
C1—N1—C12	118.1 (4)	C13i—C13—C14	110.8 (7)
C1—N1—Co1	127.8 (3)	O3—C13—H13	98.3
C12—N1—Co1	114.1 (3)	C13i—C13—H13	98.3
C10—N2—C11	116.5 (4)	C14—C13—H13	98.3
C10—N2—Co1	129.7 (3)	C13—C14—H14A	109.5
C11—N2—Co1	113.9 (3)	C13—C14—H14B	109.5
N1—C1—C2	122.4 (4)	H14A—C14—H14B	109.5
N1—C1—H1A	118.8	C13—C14—H14C	109.5
C2—C1—H1A	118.8	H14A—C14—H14C	109.5
C3—C2—C1	119.7 (5)	H14B—C14—H14C	109.5
C3—C2—H2A	120.2
O1—Co1—S1—O2i	89.6 (2)	N2i—Co1—N2—C10	−94.6 (4)
O1i—Co1—S1—O2i	−90.4 (2)	S1—Co1—N2—C10	85.4 (4)
N1—Co1—S1—O2i	−8.1 (2)	O1—Co1—N2—C11	−103.3 (3)
N1i—Co1—S1—O2i	171.9 (2)	O1i—Co1—N2—C11	−65.9 (5)
N2i—Co1—S1—O2i	−108.2 (2)	N1—Co1—N2—C11	−4.0 (3)
N2—Co1—S1—O2i	71.8 (2)	N1i—Co1—N2—C11	164.3 (3)
O1—Co1—S1—O2	−90.4 (2)	N2i—Co1—N2—C11	86.4 (3)
O1i—Co1—S1—O2	89.6 (2)	S1—Co1—N2—C11	−93.6 (3)
N1—Co1—S1—O2	171.9 (2)	C12—N1—C1—C2	0.4 (7)
N1i—Co1—S1—O2	−8.1 (2)	Co1—N1—C1—C2	−177.4 (3)
N2i—Co1—S1—O2	71.8 (2)	N1—C1—C2—C3	0.5 (8)
N2—Co1—S1—O2	−108.2 (2)	C1—C2—C3—C4	−0.6 (8)
O1—Co1—S1—O1i	180.0	C2—C3—C4—C12	−0.3 (7)
N1—Co1—S1—O1i	82.27 (19)	C2—C3—C4—C5	−177.3 (5)
N1i—Co1—S1—O1i	−97.73 (19)	C12—C4—C5—C6	−1.3 (7)
N2i—Co1—S1—O1i	−17.8 (2)	C3—C4—C5—C6	175.6 (5)
N2—Co1—S1—O1i	162.2 (2)	C4—C5—C6—C7	0.8 (8)
O1i—Co1—S1—O1	180.0	C5—C6—C7—C11	1.5 (7)
N1—Co1—S1—O1	−97.73 (19)	C5—C6—C7—C8	−178.2 (5)
N1i—Co1—S1—O1	82.27 (19)	C11—C7—C8—C9	−0.4 (7)
N2i—Co1—S1—O1	162.2 (2)	C6—C7—C8—C9	179.2 (4)
N2—Co1—S1—O1	−17.8 (2)	C7—C8—C9—C10	0.8 (7)
O2i—S1—O1—Co1	−118.82 (17)	C11—N2—C10—C9	−0.6 (7)
O2—S1—O1—Co1	118.44 (18)	Co1—N2—C10—C9	−179.5 (3)
O1i—S1—O1—Co1	0.0	C8—C9—C10—N2	−0.4 (8)
O1i—Co1—O1—S1	0.0	C10—N2—C11—C7	1.0 (6)
N1—Co1—O1—S1	87.70 (17)	Co1—N2—C11—C7	−179.9 (3)
N1i—Co1—O1—S1	−100.56 (16)	C10—N2—C11—C12	−176.1 (4)
N2i—Co1—O1—S1	−41.1 (4)	Co1—N2—C11—C12	3.0 (5)
N2—Co1—O1—S1	166.15 (15)	C8—C7—C11—N2	−0.6 (7)
O1—Co1—N1—C1	−83.2 (4)	C6—C7—C11—N2	179.8 (4)
O1i—Co1—N1—C1	−16.3 (4)	C8—C7—C11—C12	176.5 (4)
N1i—Co1—N1—C1	130.6 (4)	C6—C7—C11—C12	−3.1 (6)
N2i—Co1—N1—C1	80.4 (4)	C1—N1—C12—C4	−1.4 (6)
N2—Co1—N1—C1	−177.6 (4)	Co1—N1—C12—C4	176.7 (3)
S1—Co1—N1—C1	−49.4 (4)	C1—N1—C12—C11	177.4 (4)
O1—Co1—N1—C12	99.0 (3)	Co1—N1—C12—C11	−4.5 (5)
O1i—Co1—N1—C12	165.9 (3)	C3—C4—C12—N1	1.3 (7)
N1i—Co1—N1—C12	−47.3 (3)	C5—C4—C12—N1	178.4 (4)
N2i—Co1—N1—C12	−97.5 (3)	C3—C4—C12—C11	−177.5 (4)
N2—Co1—N1—C12	4.5 (3)	C5—C4—C12—C11	−0.4 (6)
S1—Co1—N1—C12	132.7 (3)	N2—C11—C12—N1	1.0 (6)
O1—Co1—N2—C10	75.6 (4)	C7—C11—C12—N1	−176.3 (4)
O1i—Co1—N2—C10	113.1 (5)	N2—C11—C12—C4	179.9 (4)
N1—Co1—N2—C10	175.0 (4)	C7—C11—C12—C4	2.6 (6)
N1i—Co1—N2—C10	−16.8 (4)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3···O2	0.82	1.95	2.698 (9)	150
O3′—H3′···O2	0.82	2.01	2.730 (10)	146

Table 1

Selected bond lengths (Å)

Co1—O1	2.124 (3)
Co1—N1	2.123 (3)
Co1—N2	2.145 (4)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H3⋯O2	0.82	1.95	2.698 (9)	150
O3′—H3′⋯O2	0.82	2.01	2.730 (10)	146