Tetra-aqua-(1,10-phenanthroline-κN,N')cadmium(II) sulfate dihydrate.

In the title mononuclear complex, [Cd(C(12)H(8)N(2))(H(2)O)(4)]SO(4)·2H(2)O, the coordination geometry around the Cd(II) atom is a distorted octa-hedron, with two aqua ligands occupying the axial positions. Inter-molecular O-H⋯O hydrogen bonds lead to the formation of a two-dimensional layer structure parallel to (001). The layers are connected by π-π inter-actions between the pyridyl and benzene rings of the phenanthroline ligands [centroid-centroid distances = 3.591 (1) and 3.610 (1) Å].

Related literature

For general backgound to supra­molecular structures with coordination frameworks, see: Bie et al. (2006 ▶); Huang et al. (2010 ▶); Wu et al. (2009 ▶). For related structures, see: Li et al. (2003 ▶); Zheng & Lin (2003 ▶).

Experimental

Crystal data

[Cd(C12n class="Species">H8N2)(H2O)4]SO4·2H2O

M = 496.78

Orthorhombic,

a = 8.8398 (9) Å

b = 18.6996 (19) Å

c = 22.349 (2) Å

V = 3694.3 (6) Å3

Z = 8

Mo Kα radiation

μ = 1.35 mm−1

T = 298 K

0.41 × 0.30 × 0.27 mm

Data collection

Bruker APEX CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.622, T max = 0.695

17188 measured reflections

3266 independent reflections

2789 reflections with I > 2σ(I)

R int = 0.045

Refinement

R[F 2 > 2σ(F 2)] = 0.033

wR(F 2) = 0.065

S = 1.16

3266 reflections

236 parameters

H-atom parameters constrained

Δρmax = 0.52 e Å−3

Δρmin = −0.46 e Å−3

Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT-Plus (Bruker, 2007 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810028175/hy2328sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810028175/hy2328Isup2.hkl

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

[Cd(C12H8N2)(H2O)4]SO4·2H2O	F(000) = 2000.0
Mr = 496.78	Dx = 1.786 Mg m−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 8439 reflections
a = 8.8398 (9) Å	θ = 2.2–28.1°
b = 18.6996 (19) Å	µ = 1.35 mm−1
c = 22.349 (2) Å	T = 298 K
V = 3694.3 (6) Å3	Block, yellow
Z = 8	0.41 × 0.30 × 0.27 mm

Bruker APEX CCD diffractometer	3266 independent reflections
Radiation source: fine-focus sealed tube	2789 reflections with I > 2σ(I)
graphite	Rint = 0.045
φ and ω scans	θmax = 25.0°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 2001)	h = −10→7
Tmin = 0.622, Tmax = 0.695	k = −22→22
17188 measured reflections	l = −22→26

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)] = 0.033	H-atom parameters constrained
wR(F2) = 0.065	w = 1/[σ2(Fo2) + (0.0047P)2 + 7.3452P] where P = (Fo2 + 2Fc2)/3
S = 1.16	(Δ/σ)max = 0.001
3266 reflections	Δρmax = 0.52 e Å−3
236 parameters	Δρmin = −0.46 e Å−3
0 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: 0.00446 (16)

	x	y	z	Uiso*/Ueq
Cd1	0.63465 (3)	0.587420 (13)	0.411381 (11)	0.03164 (12)
N1	0.7363 (4)	0.52699 (16)	0.33033 (14)	0.0367 (7)
N2	0.5467 (4)	0.64254 (17)	0.32424 (14)	0.0379 (8)
O1	0.4794 (3)	0.49034 (13)	0.42568 (12)	0.0433 (7)
H1A	0.5121	0.4505	0.4127	0.052*
H1B	0.4110	0.4828	0.4516	0.052*
O2	0.7916 (3)	0.68309 (13)	0.42330 (11)	0.0392 (6)
H2A	0.7508	0.7241	0.4202	0.047*
H2B	0.8638	0.6858	0.4483	0.047*
O3	0.4697 (3)	0.64814 (14)	0.46954 (13)	0.0505 (8)
H3A	0.4856	0.6921	0.4769	0.061*
H3B	0.3776	0.6393	0.4775	0.061*
O4	0.7684 (3)	0.53557 (13)	0.48847 (12)	0.0433 (7)
H4A	0.7885	0.4911	0.4880	0.052*
H4B	0.8429	0.5579	0.5037	0.052*
O5	0.8325 (3)	0.31356 (13)	0.41435 (12)	0.0445 (7)
O6	1.0491 (3)	0.38259 (15)	0.44410 (13)	0.0500 (8)
O7	0.8156 (3)	0.39447 (14)	0.49742 (14)	0.0517 (8)
O8	0.9605 (3)	0.28672 (13)	0.50624 (13)	0.0489 (8)
O9	0.9479 (3)	0.86732 (14)	0.37107 (13)	0.0499 (8)
H9A	0.8684	0.8471	0.3842	0.060*
H9B	1.0241	0.8436	0.3830	0.060*
O10	0.7963 (3)	0.20834 (17)	0.59585 (14)	0.0601 (8)
H10A	0.8254	0.2339	0.5666	0.072*
H10B	0.7303	0.1791	0.5829	0.072*
S1	0.91417 (11)	0.34438 (4)	0.46528 (4)	0.0313 (2)
C1	0.8259 (5)	0.4706 (2)	0.3331 (2)	0.0528 (12)
H1	0.8577	0.4545	0.3704	0.063*
C2	0.8748 (6)	0.4343 (3)	0.2817 (3)	0.0679 (15)
H2	0.9362	0.3941	0.2850	0.082*
C3	0.8315 (6)	0.4584 (3)	0.2274 (3)	0.0711 (16)
H3	0.8640	0.4348	0.1931	0.085*
C4	0.7386 (5)	0.5184 (3)	0.22216 (19)	0.0513 (12)
C5	0.6928 (4)	0.5516 (2)	0.27550 (16)	0.0370 (9)
C6	0.5959 (4)	0.6128 (2)	0.27248 (16)	0.0361 (9)
C7	0.5517 (5)	0.6411 (3)	0.21632 (18)	0.0500 (12)
C8	0.4601 (6)	0.7016 (3)	0.2162 (2)	0.0628 (14)
H8	0.4307	0.7218	0.1800	0.075*
C9	0.4140 (6)	0.7310 (3)	0.2677 (2)	0.0643 (14)
H9	0.3534	0.7716	0.2676	0.077*
C10	0.4585 (5)	0.6996 (2)	0.3217 (2)	0.0508 (11)
H10	0.4246	0.7197	0.3574	0.061*
C11	0.6927 (6)	0.5484 (3)	0.1662 (2)	0.0679 (15)
H11	0.7245	0.5269	0.1308	0.081*
C12	0.6042 (6)	0.6069 (3)	0.1636 (2)	0.0663 (15)
H12	0.5770	0.6254	0.1265	0.080*

	U11	U22	U33	U12	U13	U23
Cd1	0.03948 (18)	0.02569 (15)	0.02976 (16)	0.00082 (12)	0.00038 (12)	−0.00058 (12)
N1	0.0370 (18)	0.0301 (17)	0.0429 (19)	−0.0027 (15)	0.0088 (15)	−0.0022 (14)
N2	0.040 (2)	0.0347 (18)	0.0389 (18)	−0.0004 (15)	−0.0040 (16)	0.0039 (14)
O1	0.0472 (17)	0.0317 (14)	0.0510 (17)	−0.0061 (13)	0.0075 (14)	−0.0014 (12)
O2	0.0394 (15)	0.0253 (13)	0.0530 (17)	0.0024 (12)	−0.0097 (13)	−0.0017 (12)
O3	0.0479 (18)	0.0342 (15)	0.069 (2)	−0.0064 (13)	0.0238 (15)	−0.0175 (14)
O4	0.0484 (17)	0.0236 (13)	0.0579 (17)	0.0007 (12)	−0.0196 (14)	0.0005 (12)
O5	0.0478 (17)	0.0312 (14)	0.0545 (17)	−0.0085 (13)	−0.0188 (14)	0.0023 (13)
O6	0.0409 (17)	0.0461 (17)	0.0632 (19)	−0.0136 (14)	0.0002 (15)	−0.0023 (14)
O7	0.0480 (18)	0.0301 (15)	0.077 (2)	0.0033 (13)	0.0094 (16)	−0.0063 (14)
O8	0.0584 (19)	0.0302 (15)	0.0580 (18)	0.0041 (13)	−0.0206 (15)	0.0032 (13)
O9	0.0431 (17)	0.0403 (16)	0.066 (2)	0.0016 (14)	0.0109 (15)	0.0069 (14)
O10	0.0499 (19)	0.061 (2)	0.070 (2)	0.0017 (16)	−0.0032 (17)	−0.0018 (16)
S1	0.0291 (5)	0.0196 (4)	0.0451 (5)	−0.0003 (4)	−0.0060 (4)	−0.0012 (4)
C1	0.050 (3)	0.041 (2)	0.067 (3)	0.003 (2)	0.015 (2)	0.000 (2)
C2	0.062 (3)	0.052 (3)	0.090 (4)	0.009 (3)	0.026 (3)	−0.018 (3)
C3	0.067 (4)	0.077 (4)	0.069 (4)	−0.006 (3)	0.026 (3)	−0.027 (3)
C4	0.046 (3)	0.062 (3)	0.046 (3)	−0.015 (2)	0.016 (2)	−0.013 (2)
C5	0.032 (2)	0.045 (2)	0.035 (2)	−0.0137 (18)	0.0064 (17)	−0.0060 (17)
C6	0.032 (2)	0.043 (2)	0.034 (2)	−0.0137 (18)	0.0001 (17)	0.0022 (17)
C7	0.044 (3)	0.068 (3)	0.038 (2)	−0.023 (2)	−0.004 (2)	0.007 (2)
C8	0.056 (3)	0.073 (3)	0.060 (3)	−0.014 (3)	−0.019 (3)	0.026 (3)
C9	0.061 (3)	0.058 (3)	0.074 (4)	−0.003 (3)	−0.020 (3)	0.015 (3)
C10	0.051 (3)	0.045 (3)	0.056 (3)	0.003 (2)	−0.008 (2)	0.004 (2)
C11	0.066 (3)	0.101 (4)	0.036 (3)	−0.019 (3)	0.013 (2)	−0.013 (3)
C12	0.062 (3)	0.101 (4)	0.036 (3)	−0.020 (3)	−0.001 (2)	0.007 (3)

Cd1—O3	2.260 (3)	O9—H9B	0.8500
Cd1—O2	2.280 (2)	O10—H10A	0.8500
Cd1—O1	2.298 (3)	O10—H10B	0.8500
Cd1—O4	2.304 (2)	C1—C2	1.403 (6)
Cd1—N1	2.317 (3)	C1—H1	0.9300
Cd1—N2	2.337 (3)	C2—C3	1.350 (7)
N1—C1	1.320 (5)	C2—H2	0.9300
N1—C5	1.364 (5)	C3—C4	1.396 (7)
N2—C10	1.323 (5)	C3—H3	0.9300
N2—C6	1.355 (5)	C4—C5	1.403 (5)
O1—H1A	0.8500	C4—C11	1.429 (7)
O1—H1B	0.8499	C5—C6	1.432 (6)
O2—H2A	0.8499	C6—C7	1.417 (5)
O2—H2B	0.8500	C7—C8	1.392 (7)
O3—H3A	0.8500	C7—C12	1.418 (7)
O3—H3B	0.8500	C8—C9	1.340 (7)
O4—H4A	0.8500	C8—H8	0.9300
O4—H4B	0.8500	C9—C10	1.398 (6)
O5—S1	1.466 (3)	C9—H9	0.9300
O6—S1	1.469 (3)	C10—H10	0.9300
O7—S1	1.467 (3)	C11—C12	1.347 (7)
O8—S1	1.473 (3)	C11—H11	0.9300
O9—H9A	0.8500	C12—H12	0.9300
O3—Cd1—O2	86.06 (9)	O7—S1—O8	109.16 (18)
O3—Cd1—O1	86.08 (10)	O6—S1—O8	109.31 (18)
O2—Cd1—O1	165.28 (9)	N1—C1—C2	122.2 (5)
O3—Cd1—O4	96.46 (11)	N1—C1—H1	118.9
O2—Cd1—O4	86.02 (9)	C2—C1—H1	118.9
O1—Cd1—O4	82.52 (9)	C3—C2—C1	119.1 (5)
O3—Cd1—N1	160.98 (12)	C3—C2—H2	120.4
O2—Cd1—N1	103.77 (10)	C1—C2—H2	120.4
O1—Cd1—N1	87.42 (10)	C2—C3—C4	120.8 (5)
O4—Cd1—N1	100.39 (10)	C2—C3—H3	119.6
O3—Cd1—N2	92.46 (11)	C4—C3—H3	119.6
O2—Cd1—N2	87.35 (10)	C3—C4—C5	116.9 (4)
O1—Cd1—N2	105.41 (10)	C3—C4—C11	123.8 (5)
O4—Cd1—N2	168.48 (11)	C5—C4—C11	119.3 (5)
N1—Cd1—N2	72.09 (11)	N1—C5—C4	122.2 (4)
C1—N1—C5	118.7 (4)	N1—C5—C6	118.7 (3)
C1—N1—Cd1	125.8 (3)	C4—C5—C6	119.0 (4)
C5—N1—Cd1	115.4 (2)	N2—C6—C7	120.9 (4)
C10—N2—C6	119.0 (3)	N2—C6—C5	118.7 (3)
C10—N2—Cd1	126.0 (3)	C7—C6—C5	120.4 (4)
C6—N2—Cd1	115.0 (2)	C8—C7—C6	117.8 (4)
Cd1—O1—H1A	116.2	C8—C7—C12	123.7 (5)
Cd1—O1—H1B	130.6	C6—C7—C12	118.5 (5)
H1A—O1—H1B	109.3	C9—C8—C7	120.5 (4)
Cd1—O2—H2A	116.1	C9—C8—H8	119.7
Cd1—O2—H2B	125.5	C7—C8—H8	119.7
H2A—O2—H2B	108.6	C8—C9—C10	119.0 (5)
Cd1—O3—H3A	119.4	C8—C9—H9	120.5
Cd1—O3—H3B	129.9	C10—C9—H9	120.5
H3A—O3—H3B	107.8	N2—C10—C9	122.7 (5)
Cd1—O4—H4A	120.7	N2—C10—H10	118.6
Cd1—O4—H4B	119.3	C9—C10—H10	118.6
H4A—O4—H4B	108.8	C12—C11—C4	121.4 (5)
H9A—O9—H9B	108.3	C12—C11—H11	119.3
H10A—O10—H10B	107.9	C4—C11—H11	119.3
O5—S1—O7	109.79 (17)	C11—C12—C7	121.3 (5)
O5—S1—O6	109.95 (17)	C11—C12—H12	119.3
O7—S1—O6	109.24 (17)	C7—C12—H12	119.3
O5—S1—O8	109.38 (15)
O3—Cd1—N1—C1	−141.9 (4)	Cd1—N1—C5—C6	2.5 (4)
O2—Cd1—N1—C1	98.5 (3)	C3—C4—C5—N1	0.1 (6)
O1—Cd1—N1—C1	−71.8 (3)	C11—C4—C5—N1	−178.0 (4)
O4—Cd1—N1—C1	10.1 (3)	C3—C4—C5—C6	−179.2 (4)
N2—Cd1—N1—C1	−178.9 (3)	C11—C4—C5—C6	2.7 (6)
O3—Cd1—N1—C5	35.5 (5)	C10—N2—C6—C7	−1.2 (6)
O2—Cd1—N1—C5	−84.1 (3)	Cd1—N2—C6—C7	−179.7 (3)
O1—Cd1—N1—C5	105.6 (3)	C10—N2—C6—C5	179.2 (3)
O4—Cd1—N1—C5	−172.5 (2)	Cd1—N2—C6—C5	0.7 (4)
N2—Cd1—N1—C5	−1.5 (2)	N1—C5—C6—N2	−2.2 (5)
O3—Cd1—N2—C10	13.4 (3)	C4—C5—C6—N2	177.1 (4)
O2—Cd1—N2—C10	−72.6 (3)	N1—C5—C6—C7	178.2 (3)
O1—Cd1—N2—C10	100.0 (3)	C4—C5—C6—C7	−2.5 (5)
O4—Cd1—N2—C10	−127.4 (5)	N2—C6—C7—C8	1.9 (6)
N1—Cd1—N2—C10	−178.0 (4)	C5—C6—C7—C8	−178.6 (4)
O3—Cd1—N2—C6	−168.3 (3)	N2—C6—C7—C12	−178.8 (4)
O2—Cd1—N2—C6	105.8 (3)	C5—C6—C7—C12	0.7 (6)
O1—Cd1—N2—C6	−81.6 (3)	C6—C7—C8—C9	−1.0 (7)
O4—Cd1—N2—C6	50.9 (6)	C12—C7—C8—C9	179.7 (5)
N1—Cd1—N2—C6	0.4 (2)	C7—C8—C9—C10	−0.4 (7)
C5—N1—C1—C2	−1.6 (6)	C6—N2—C10—C9	−0.3 (6)
Cd1—N1—C1—C2	175.7 (3)	Cd1—N2—C10—C9	178.0 (3)
N1—C1—C2—C3	1.4 (8)	C8—C9—C10—N2	1.2 (7)
C1—C2—C3—C4	−0.4 (8)	C3—C4—C11—C12	−179.2 (5)
C2—C3—C4—C5	−0.3 (7)	C5—C4—C11—C12	−1.2 (7)
C2—C3—C4—C11	177.8 (5)	C4—C11—C12—C7	−0.6 (8)
C1—N1—C5—C4	0.8 (6)	C8—C7—C12—C11	−180.0 (5)
Cd1—N1—C5—C4	−176.8 (3)	C6—C7—C12—C11	0.8 (7)
C1—N1—C5—C6	−179.9 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···O9i	0.85	1.85	2.682 (4)	167
O1—H1B···O4ii	0.85	2.10	2.952 (4)	176
O2—H2A···O5iii	0.85	1.83	2.682 (3)	178
O2—H2B···O8iv	0.85	1.93	2.757 (4)	165
O3—H3A···O8iii	0.85	1.95	2.787 (4)	170
O3—H3B···O7ii	0.85	1.90	2.746 (4)	170
O4—H4A···O7	0.85	1.84	2.679 (4)	171
O4—H4B···O6iv	0.85	1.87	2.686 (4)	159
O9—H9A···O5iii	0.85	2.00	2.844 (4)	172
O9—H9B···O10iv	0.85	1.92	2.768 (4)	176
O10—H10A···O8	0.85	2.05	2.875 (4)	162
O10—H10B···O6v	0.85	2.06	2.909 (4)	172

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯O9i	0.85	1.85	2.682 (4)	167
O1—H1B⋯O4ii	0.85	2.10	2.952 (4)	176
O2—H2A⋯O5iii	0.85	1.83	2.682 (3)	178
O2—H2B⋯O8iv	0.85	1.93	2.757 (4)	165
O3—H3A⋯O8iii	0.85	1.95	2.787 (4)	170
O3—H3B⋯O7ii	0.85	1.90	2.746 (4)	170
O4—H4A⋯O7	0.85	1.84	2.679 (4)	171
O4—H4B⋯O6iv	0.85	1.87	2.686 (4)	159
O9—H9A⋯O5iii	0.85	2.00	2.844 (4)	172
O9—H9B⋯O10iv	0.85	1.92	2.768 (4)	176
O10—H10A⋯O8	0.85	2.05	2.875 (4)	162
O10—H10B⋯O6v	0.85	2.06	2.909 (4)	172

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .