Bis(1,10-phenanthroline-κN,N')(sulfato-κO,O')cadmium(II) propane-1,3-diol solvate.

In the title compound, [Cd(SO(4))(C(12)H(8)N(2))(2)]·C(3)H(8)O(2), the Cd(II) atom 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 group. The two chelating NCCN groups subtend a dihedral angle of 82.21 (9)°. The Cd(II) ion, the S atom and the middle C atom of the propane-1,3-diol solvent mol-ecule are located on special positions, site symmetry 2. The solvate features a pair of O-H⋯O hydrogen bonds with the uncoordinated O atoms of the sulfate ion. The OH group of the propane-1,3-diol solvent is disordered over two positions of equal occupancy.

Related literature

For isostructural compounds, see: Cui et al. (2010 ▶); Ni et al. (2010 ▶); Zhong (2010a ▶). For the ethane-1,2-diol solvate of the title complex, see: Lu et al. (2006 ▶). For background to bidentate-chelating sulfate complexes, see: Zhong et al. (2006 ▶, 2010b ▶); Zhu et al. (2006 ▶). For the preparation, see: Zhong et al. (2010a ▶). For background to coordination polymers, see: Batten & Robson (1998 ▶); Eddaoudi et al. (2001 ▶); Li et al. (2003 ▶).

Experimental

Crystal data

[Cd(SO4)(C12H8N2)2]·C3H8O2

M = 644.98

Monoclinic,

a = 17.854 (4) Å

b = 12.520 (3) Å

c = 13.519 (3) Å

β = 123.01 (3)°

V = 2534.1 (13) Å3

Z = 4

Mo Kα radiation

μ = 1.00 mm−1

T = 223 K

0.40 × 0.30 × 0.20 mm

Data collection

Rigaku Mercury CCD diffractometer

Absorption correction: multi-scan (REQAB; Jacobson, 1998 ▶) T min = 0.691, T max = 0.826

8349 measured reflections

2880 independent reflections

2683 reflections with I > 2σ(I)

R int = 0.021

Refinement

R[F 2 > 2σ(F 2)] = 0.028

wR(F 2) = 0.072

S = 1.10

2880 reflections

178 parameters

3 restraints

H-atom parameters constrained

Δρmax = 0.75 e Å−3

Δρmin = −0.65 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.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810022518/bq2222sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810022518/bq2222Isup2.hkl

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

[Cd(SO4)(C12H8N2)2]·C3H8O2	F(000) = 1304
Mr = 644.98	Dx = 1.691 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 3776 reflections
a = 17.854 (4) Å	θ = 3.1–27.5°
b = 12.520 (3) Å	µ = 1.00 mm−1
c = 13.519 (3) Å	T = 223 K
β = 123.01 (3)°	Block, colorless
V = 2534.1 (13) Å3	0.40 × 0.30 × 0.20 mm
Z = 4

Rigaku Mercury CCD diffractometer	2880 independent reflections
Radiation source: fine-focus sealed tube	2683 reflections with I > 2σ(I)
graphite	Rint = 0.021
Detector resolution: 28.5714 pixels mm-1	θmax = 27.5°, θmin = 3.1°
ω scans	h = −19→23
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	k = −12→16
Tmin = 0.691, Tmax = 0.826	l = −17→12
8349 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)] = 0.028	H-atom parameters constrained
wR(F2) = 0.072	w = 1/[σ2(Fo2) + (0.0391P)2 + 2.1837P] where P = (Fo2 + 2Fc2)/3
S = 1.10	(Δ/σ)max < 0.001
2880 reflections	Δρmax = 0.75 e Å−3
178 parameters	Δρmin = −0.65 e Å−3
3 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: 0.0053 (3)

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)
Cd1	0.5000	0.174163 (16)	0.2500	0.02229 (10)
S1	0.5000	−0.06039 (5)	0.2500	0.01961 (16)
O1	0.51467 (11)	0.01117 (13)	0.34685 (14)	0.0300 (3)
O2	0.57895 (10)	−0.12744 (13)	0.29112 (15)	0.0306 (4)
N1	0.39140 (11)	0.29051 (15)	0.10875 (16)	0.0222 (4)
N2	0.40091 (11)	0.21462 (15)	0.30577 (17)	0.0234 (4)
C7	0.27252 (14)	0.31996 (16)	0.2610 (2)	0.0237 (4)
C9	0.34479 (16)	0.2062 (2)	0.4312 (2)	0.0306 (5)
H9A	0.3498	0.1780	0.4982	0.037*
C2	0.32079 (15)	0.39930 (19)	−0.0655 (2)	0.0295 (5)
H2A	0.3194	0.4232	−0.1316	0.035*
C8	0.27880 (15)	0.27765 (19)	0.3615 (2)	0.0290 (5)
H8A	0.2381	0.2983	0.3806	0.035*
C10	0.40478 (16)	0.17602 (17)	0.4000 (2)	0.0275 (5)
H10A	0.4493	0.1268	0.4472	0.033*
C6	0.20366 (14)	0.39348 (18)	0.1827 (2)	0.0282 (5)
H6A	0.1619	0.4159	0.1991	0.034*
C11	0.33584 (13)	0.28613 (16)	0.23634 (19)	0.0207 (4)
C5	0.19881 (15)	0.43057 (17)	0.0856 (2)	0.0272 (5)
H5A	0.1534	0.4777	0.0357	0.033*
C4	0.26246 (13)	0.39846 (17)	0.05810 (19)	0.0232 (4)
C3	0.25909 (15)	0.43470 (18)	−0.0429 (2)	0.0283 (5)
H3A	0.2150	0.4826	−0.0941	0.034*
C1	0.38597 (16)	0.32669 (17)	0.0124 (2)	0.0268 (5)
H1A	0.4274	0.3025	−0.0039	0.032*
C12	0.33059 (14)	0.32544 (15)	0.13234 (19)	0.0204 (4)
C14	0.5000	−0.4518 (3)	0.2500	0.0452 (10)
O3	0.55944 (17)	−0.32203 (16)	0.1763 (2)	0.0548 (6)
H3B	0.5502	−0.2607	0.1883	0.082*
C13'	0.5787 (6)	−0.3855 (7)	0.2714 (7)	0.084 (2)*	0.50
H13A	0.5986	−0.3401	0.3396	0.101*	0.50
H13B	0.6276	−0.4330	0.2897	0.101*	0.50
C13	0.4872 (3)	−0.3854 (4)	0.1485 (4)	0.0295 (10)*	0.50
H13E	0.4749	−0.4329	0.0846	0.035*	0.50
H13C	0.4354	−0.3400	0.1201	0.035*	0.50
H14A	0.4484	−0.4976	0.2216	0.035*

	U11	U22	U33	U12	U13	U23
Cd1	0.01994 (13)	0.02154 (14)	0.02924 (15)	0.000	0.01589 (10)	0.000
S1	0.0176 (3)	0.0208 (4)	0.0207 (4)	0.000	0.0106 (3)	0.000
O1	0.0381 (9)	0.0256 (7)	0.0242 (8)	0.0034 (7)	0.0156 (7)	−0.0016 (6)
O2	0.0249 (8)	0.0319 (9)	0.0366 (9)	0.0073 (6)	0.0178 (7)	0.0025 (7)
N1	0.0218 (9)	0.0223 (9)	0.0254 (9)	−0.0008 (7)	0.0147 (7)	−0.0011 (7)
N2	0.0227 (9)	0.0231 (9)	0.0274 (10)	0.0011 (7)	0.0155 (8)	0.0017 (7)
C7	0.0225 (10)	0.0246 (11)	0.0262 (11)	−0.0013 (7)	0.0147 (9)	−0.0048 (9)
C9	0.0363 (12)	0.0335 (12)	0.0301 (12)	0.0001 (10)	0.0234 (11)	0.0029 (10)
C2	0.0349 (12)	0.0303 (12)	0.0250 (11)	−0.0036 (10)	0.0174 (10)	0.0012 (10)
C8	0.0297 (11)	0.0317 (12)	0.0341 (13)	0.0002 (9)	0.0229 (10)	−0.0019 (10)
C10	0.0273 (11)	0.0278 (12)	0.0304 (12)	0.0026 (8)	0.0177 (10)	0.0051 (9)
C6	0.0236 (10)	0.0301 (12)	0.0332 (12)	0.0040 (8)	0.0170 (9)	−0.0054 (10)
C11	0.0198 (9)	0.0191 (10)	0.0247 (11)	−0.0017 (7)	0.0131 (8)	−0.0027 (8)
C5	0.0235 (10)	0.0252 (11)	0.0292 (12)	0.0045 (8)	0.0119 (9)	−0.0017 (9)
C4	0.0224 (10)	0.0204 (10)	0.0243 (10)	−0.0011 (8)	0.0112 (8)	−0.0030 (8)
C3	0.0271 (11)	0.0266 (12)	0.0257 (11)	0.0009 (8)	0.0107 (9)	0.0016 (9)
C1	0.0293 (11)	0.0276 (12)	0.0293 (12)	−0.0022 (8)	0.0196 (10)	−0.0023 (9)
C12	0.0189 (9)	0.0192 (10)	0.0231 (10)	−0.0022 (7)	0.0115 (8)	−0.0029 (8)
C14	0.050 (2)	0.0260 (19)	0.060 (3)	0.000	0.030 (2)	0.000
O3	0.0824 (17)	0.0422 (12)	0.0729 (16)	−0.0064 (10)	0.0636 (15)	−0.0086 (10)

Cd1—N2i	2.3255 (19)	C8—H8A	0.9300
Cd1—N2	2.3255 (19)	C10—H10A	0.9300
Cd1—N1i	2.344 (2)	C6—C5	1.351 (3)
Cd1—N1	2.3439 (19)	C6—H6A	0.9300
Cd1—O1i	2.3608 (17)	C11—C12	1.444 (3)
Cd1—O1	2.3608 (17)	C5—C4	1.432 (3)
Cd1—S1	2.9366 (10)	C5—H5A	0.9300
S1—O2i	1.4652 (16)	C4—C3	1.409 (3)
S1—O2	1.4652 (16)	C4—C12	1.412 (3)
S1—O1	1.4873 (17)	C3—H3A	0.9300
S1—O1i	1.4873 (17)	C1—H1A	0.9300
N1—C1	1.332 (3)	C14—C13i	1.512 (5)
N1—C12	1.360 (3)	C14—C13	1.512 (5)
N2—C10	1.328 (3)	C14—C13'	1.518 (9)
N2—C11	1.358 (3)	C14—C13'i	1.518 (9)
C7—C8	1.405 (3)	C14—H14A	0.9699
C7—C11	1.407 (3)	O3—C13	1.380 (5)
C7—C6	1.436 (3)	O3—C13'	1.385 (7)
C9—C8	1.367 (3)	O3—H3B	0.8200
C9—C10	1.400 (3)	C13'—H13A	0.9700
C9—H9A	0.9300	C13'—H13B	0.9700
C2—C3	1.367 (3)	C13—H13E	0.9700
C2—C1	1.398 (3)	C13—H13C	0.9700
C2—H2A	0.9300
N2i—Cd1—N2	154.84 (9)	N2—C10—C9	122.8 (2)
N2i—Cd1—N1i	72.00 (7)	N2—C10—H10A	118.6
N2—Cd1—N1i	92.19 (7)	C9—C10—H10A	118.6
N2i—Cd1—N1	92.19 (7)	C5—C6—C7	120.8 (2)
N2—Cd1—N1	72.00 (7)	C5—C6—H6A	119.6
N1i—Cd1—N1	103.15 (9)	C7—C6—H6A	119.6
N2i—Cd1—O1i	83.26 (6)	N2—C11—C7	122.0 (2)
N2—Cd1—O1i	119.60 (6)	N2—C11—C12	118.37 (18)
N1i—Cd1—O1i	141.41 (6)	C7—C11—C12	119.60 (19)
N1—Cd1—O1i	107.02 (6)	C6—C5—C4	121.1 (2)
N2i—Cd1—O1	119.60 (6)	C6—C5—H5A	119.5
N2—Cd1—O1	83.26 (6)	C4—C5—H5A	119.5
N1i—Cd1—O1	107.02 (6)	C3—C4—C12	117.6 (2)
N1—Cd1—O1	141.41 (6)	C3—C4—C5	122.7 (2)
O1i—Cd1—O1	60.38 (8)	C12—C4—C5	119.7 (2)
N2i—Cd1—S1	102.58 (5)	C2—C3—C4	119.9 (2)
N2—Cd1—S1	102.58 (5)	C2—C3—H3A	120.1
N1i—Cd1—S1	128.42 (5)	C4—C3—H3A	120.1
N1—Cd1—S1	128.42 (5)	N1—C1—C2	123.0 (2)
O1i—Cd1—S1	30.19 (4)	N1—C1—H1A	118.5
O1—Cd1—S1	30.19 (4)	C2—C1—H1A	118.5
O2i—S1—O2	110.10 (14)	N1—C12—C4	122.0 (2)
O2i—S1—O1	110.53 (10)	N1—C12—C11	118.83 (18)
O2—S1—O1	109.85 (10)	C4—C12—C11	119.14 (19)
O2i—S1—O1i	109.85 (10)	C13i—C14—C13	113.3 (4)
O2—S1—O1i	110.53 (10)	C13i—C14—C13'	82.0 (4)
O1—S1—O1i	105.92 (14)	C13—C14—C13'	62.5 (4)
O2i—S1—Cd1	124.95 (7)	C13i—C14—C13'i	62.5 (4)
O2—S1—Cd1	124.95 (7)	C13—C14—C13'i	82.0 (4)
O1—S1—Cd1	52.96 (7)	C13'—C14—C13'i	113.7 (8)
O1i—S1—Cd1	52.96 (7)	C13i—C14—H14A	109.0
S1—O1—Cd1	96.85 (8)	C13—C14—H14A	109.0
C1—N1—C12	118.56 (19)	C13'—C14—H14A	168.7
C1—N1—Cd1	126.53 (15)	C13'i—C14—H14A	70.5
C12—N1—Cd1	114.87 (14)	C13—O3—C13'	69.3 (4)
C10—N2—C11	118.73 (19)	C13—O3—H3B	109.5
C10—N2—Cd1	125.46 (15)	C13'—O3—H3B	109.2
C11—N2—Cd1	115.78 (14)	O3—C13'—C14	113.6 (6)
C8—C7—C11	117.7 (2)	O3—C13'—H13A	108.8
C8—C7—C6	122.7 (2)	C14—C13'—H13A	108.8
C11—C7—C6	119.6 (2)	O3—C13'—H13B	108.8
C8—C9—C10	118.8 (2)	C14—C13'—H13B	108.8
C8—C9—H9A	120.6	H13A—C13'—H13B	107.7
C10—C9—H9A	120.6	O3—C13—C14	114.3 (3)
C3—C2—C1	119.0 (2)	O3—C13—H13E	108.7
C3—C2—H2A	120.5	C14—C13—H13E	108.7
C1—C2—H2A	120.5	O3—C13—H13C	108.7
C9—C8—C7	119.9 (2)	C14—C13—H13C	108.7
C9—C8—H8A	120.1	H13E—C13—H13C	107.6
C7—C8—H8A	120.1
N2i—Cd1—S1—O2i	−140.99 (10)	N1—Cd1—N2—C11	−3.31 (14)
N2—Cd1—S1—O2i	39.01 (10)	O1i—Cd1—N2—C11	−103.06 (15)
N1i—Cd1—S1—O2i	142.14 (10)	O1—Cd1—N2—C11	−153.30 (15)
N1—Cd1—S1—O2i	−37.86 (10)	S1—Cd1—N2—C11	−129.96 (14)
O1i—Cd1—S1—O2i	−89.51 (12)	C10—C9—C8—C7	−0.4 (4)
O1—Cd1—S1—O2i	90.49 (12)	C11—C7—C8—C9	−0.1 (3)
N2i—Cd1—S1—O2	39.01 (10)	C6—C7—C8—C9	178.6 (2)
N2—Cd1—S1—O2	−140.99 (10)	C11—N2—C10—C9	−0.3 (3)
N1i—Cd1—S1—O2	−37.86 (10)	Cd1—N2—C10—C9	177.81 (17)
N1—Cd1—S1—O2	142.14 (10)	C8—C9—C10—N2	0.6 (4)
O1i—Cd1—S1—O2	90.49 (12)	C8—C7—C6—C5	−178.6 (2)
O1—Cd1—S1—O2	−89.51 (12)	C11—C7—C6—C5	0.0 (3)
N2i—Cd1—S1—O1	128.52 (9)	C10—N2—C11—C7	−0.3 (3)
N2—Cd1—S1—O1	−51.48 (9)	Cd1—N2—C11—C7	−178.50 (15)
N1i—Cd1—S1—O1	51.65 (10)	C10—N2—C11—C12	−178.31 (19)
N1—Cd1—S1—O1	−128.35 (10)	Cd1—N2—C11—C12	3.4 (2)
O1i—Cd1—S1—O1	180.0	C8—C7—C11—N2	0.4 (3)
N2i—Cd1—S1—O1i	−51.48 (9)	C6—C7—C11—N2	−178.3 (2)
N2—Cd1—S1—O1i	128.52 (9)	C8—C7—C11—C12	178.45 (19)
N1i—Cd1—S1—O1i	−128.35 (10)	C6—C7—C11—C12	−0.2 (3)
N1—Cd1—S1—O1i	51.65 (10)	C7—C6—C5—C4	−0.5 (3)
O1—Cd1—S1—O1i	180.0	C6—C5—C4—C3	179.4 (2)
O2i—S1—O1—Cd1	−118.93 (9)	C6—C5—C4—C12	1.1 (3)
O2—S1—O1—Cd1	119.38 (9)	C1—C2—C3—C4	0.5 (3)
O1i—S1—O1—Cd1	0.0	C12—C4—C3—C2	−0.3 (3)
N2i—Cd1—O1—S1	−61.43 (10)	C5—C4—C3—C2	−178.6 (2)
N2—Cd1—O1—S1	129.74 (9)	C12—N1—C1—C2	0.3 (3)
N1i—Cd1—O1—S1	−140.02 (8)	Cd1—N1—C1—C2	−177.53 (16)
N1—Cd1—O1—S1	80.06 (12)	C3—C2—C1—N1	−0.5 (3)
O1i—Cd1—O1—S1	0.0	C1—N1—C12—C4	0.0 (3)
N2i—Cd1—N1—C1	20.70 (18)	Cd1—N1—C12—C4	178.00 (15)
N2—Cd1—N1—C1	−179.26 (19)	C1—N1—C12—C11	179.70 (19)
N1i—Cd1—N1—C1	92.72 (18)	Cd1—N1—C12—C11	−2.3 (2)
O1i—Cd1—N1—C1	−62.92 (19)	C3—C4—C12—N1	0.1 (3)
O1—Cd1—N1—C1	−126.49 (17)	C5—C4—C12—N1	178.45 (19)
S1—Cd1—N1—C1	−87.28 (18)	C3—C4—C12—C11	−179.68 (19)
N2i—Cd1—N1—C12	−157.16 (14)	C5—C4—C12—C11	−1.3 (3)
N2—Cd1—N1—C12	2.88 (14)	N2—C11—C12—N1	−0.8 (3)
N1i—Cd1—N1—C12	−85.14 (14)	C7—C11—C12—N1	−178.89 (19)
O1i—Cd1—N1—C12	119.22 (14)	N2—C11—C12—C4	178.97 (19)
O1—Cd1—N1—C12	55.65 (18)	C7—C11—C12—C4	0.9 (3)
S1—Cd1—N1—C12	94.86 (14)	C13—O3—C13'—C14	−4.0 (5)
N2i—Cd1—N2—C10	−128.08 (18)	C13i—C14—C13'—O3	−117.7 (7)
N1i—Cd1—N2—C10	−78.30 (19)	C13—C14—C13'—O3	3.9 (5)
N1—Cd1—N2—C10	178.6 (2)	C13'i—C14—C13'—O3	−62.5 (5)
O1i—Cd1—N2—C10	78.82 (19)	C13'—O3—C13—C14	4.1 (5)
O1—Cd1—N2—C10	28.59 (18)	C13i—C14—C13—O3	62.8 (3)
S1—Cd1—N2—C10	51.92 (18)	C13'—C14—C13—O3	−3.9 (5)
N2i—Cd1—N2—C11	50.04 (14)	C13'i—C14—C13—O3	118.1 (4)
N1i—Cd1—N2—C11	99.81 (15)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3B···O2	0.82	2.05	2.806 (3)	153

Table 1

Selected bond lengths (Å)

Cd1—N2	2.3255 (19)
Cd1—N1	2.3439 (19)
Cd1—O1	2.3608 (17)
S1—O2	1.4652 (16)
S1—O1	1.4873 (17)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H3B⋯O2	0.82	2.05	2.806 (3)	153