Diaqua-bis(1,10-phenanthroline)magnesium dichromate(VI) 1,10-phenanthroline disolvate.

In the title compound, [Mg(C(12)H(8)N(2))(2)(H(2)O)(2)][Cr(2)O(7)]·2C(12)H(8)N(2), the cation and anion are situated on a twofold rotation axis. The Mg(II) ion is coordinated by four N atoms from two 1,10-phenanthroline ligands and two O atoms from coordinated water mol-ecules in a distorted octa-hedral geometry. Inter-molecular O-H⋯N and O-H⋯O hydrogen bonds and π-π inter-actions between the aromatic rings [shortest centroid-centroid separation = 3.527 (2) Å] link the cations, anions and 1,10-phenanthroline solvent mol-ecules into a hydrogen-bonded cluster.

Related literature

For related magnesium–phenanthroline complexes, see: Zhu et al. (2008 ▶); Hao et al. (2008 ▶); Zhang (2004 ▶).

Experimental

Crystal data

[Mg(C12H8N2)2(H2O)2][Cr2O7]·2C12H8N2

M = 997.16

Monoclinic,

a = 16.761 (3) Å

b = 22.172 (4) Å

c = 13.996 (3) Å

β = 123.49 (3)°

V = 4338 (2) Å3

Z = 4

Mo Kα radiation

μ = 0.59 mm−1

T = 293 K

0.30 × 0.28 × 0.21 mm

Data collection

Bruker SMART CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.826, T max = 0.878

16762 measured reflections

3817 independent reflections

3068 reflections with I > 2σ(I)

R int = 0.020

Refinement

R[F 2 > 2σ(F 2)] = 0.051

wR(F 2) = 0.155

S = 1.06

3817 reflections

308 parameters

H-atom parameters constrained

Δρmax = 0.87 e Å−3

Δρmin = −0.46 e Å−3

Data collection: SMART (Bruker, 1998 ▶); cell refinement: SAINT (Bruker, 1999 ▶); data reduction: SAINT; 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 I, global. DOI: 10.1107/S1600536809030128/cv2597sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809030128/cv2597Isup2.hkl

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

[Mg(C12H8N2)2(H2O)2][Cr2O7]·2C12H8N2	F(000) = 2048
Mr = 997.16	Dx = 1.527 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 2800 reflections
a = 16.761 (3) Å	θ = 5.0–22.8°
b = 22.172 (4) Å	µ = 0.59 mm−1
c = 13.996 (3) Å	T = 293 K
β = 123.49 (3)°	Prism, yellow
V = 4338 (2) Å3	0.30 × 0.28 × 0.21 mm
Z = 4

Bruker SMART CCD area-detector diffractometer	3817 independent reflections
Radiation source: fine-focus sealed tube	3068 reflections with I > 2σ(I)
graphite	Rint = 0.020
φ and ω scans	θmax = 25.0°, θmin = 3.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −19→19
Tmin = 0.826, Tmax = 0.878	k = −26→26
16762 measured reflections	l = −16→15

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.051	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.155	H-atom parameters constrained
S = 1.06	w = 1/[σ2(Fo2) + (0.0878P)2 + 5.6611P] where P = (Fo2 + 2Fc2)/3
3817 reflections	(Δ/σ)max < 0.001
308 parameters	Δρmax = 0.87 e Å−3
0 restraints	Δρmin = −0.46 e Å−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
O4	0.5000	0.0547 (2)	0.2500	0.135 (2)
Mg1	0.5000	0.32609 (6)	0.2500	0.0429 (3)
C12	0.42272 (18)	0.41277 (11)	0.3486 (2)	0.0341 (6)
C4	0.36810 (18)	0.45551 (13)	0.3620 (2)	0.0387 (6)
N1	0.40575 (15)	0.39775 (10)	0.24512 (19)	0.0374 (5)
N2	0.55208 (16)	0.34161 (11)	0.4315 (2)	0.0427 (6)
C7	0.5222 (2)	0.39865 (14)	0.5573 (2)	0.0431 (7)
C11	0.50124 (18)	0.38299 (12)	0.4484 (2)	0.0367 (6)
O1W	0.60296 (19)	0.26585 (11)	0.2850 (2)	0.0743 (8)
C5	0.3893 (2)	0.46843 (14)	0.4739 (3)	0.0479 (7)
H5	0.3515	0.4957	0.4826	0.057*
C2	0.2783 (2)	0.46981 (15)	0.1593 (3)	0.0503 (7)
H2	0.2303	0.4890	0.0930	0.060*
C3	0.2941 (2)	0.48458 (14)	0.2624 (3)	0.0471 (7)
H3	0.2565	0.5136	0.2674	0.057*
C6	0.4639 (2)	0.44126 (15)	0.5673 (3)	0.0509 (8)
H6	0.4772	0.4507	0.6395	0.061*
C10	0.6264 (2)	0.31578 (16)	0.5247 (3)	0.0557 (8)
H10	0.6616	0.2871	0.5145	0.067*
C1	0.3345 (2)	0.42583 (14)	0.1536 (3)	0.0469 (7)
H1	0.3217	0.4155	0.0820	0.056*
C9	0.6539 (2)	0.32924 (18)	0.6350 (3)	0.0637 (10)
H9	0.7068	0.3104	0.6971	0.076*
C8	0.6026 (2)	0.37051 (17)	0.6519 (3)	0.0575 (9)
H8	0.6205	0.3801	0.7260	0.069*
H1B	0.5962	0.2278	0.2851	0.086*
H1A	0.6369	0.2686	0.2572	0.086*
C24	0.7163 (2)	0.30719 (14)	0.1147 (3)	0.0448 (7)
C16	0.7005 (2)	0.32042 (15)	0.0067 (3)	0.0496 (7)
C23	0.7918 (2)	0.33854 (14)	0.2156 (3)	0.0467 (7)
C19	0.8456 (2)	0.38268 (16)	0.2027 (3)	0.0513 (8)
N3	0.66308 (19)	0.26634 (13)	0.1282 (2)	0.0533 (7)
N4	0.8060 (2)	0.32422 (14)	0.3182 (2)	0.0577 (7)
C18	0.8266 (2)	0.39479 (17)	0.0912 (3)	0.0585 (9)
H18	0.8621	0.4241	0.0830	0.070*
C17	0.7583 (2)	0.36451 (18)	−0.0013 (3)	0.0590 (9)
H17	0.7486	0.3725	−0.0722	0.071*
C13	0.5949 (3)	0.23787 (17)	0.0359 (3)	0.0611 (9)
H13	0.5584	0.2097	0.0448	0.073*
C14	0.5743 (3)	0.24734 (17)	−0.0736 (3)	0.0641 (9)
H14	0.5252	0.2262	−0.1358	0.077*
C20	0.9162 (2)	0.41347 (18)	0.3012 (3)	0.0642 (10)
H20	0.9527	0.4434	0.2963	0.077*
C15	0.6273 (2)	0.28822 (17)	−0.0877 (3)	0.0601 (9)
H15	0.6151	0.2949	−0.1602	0.072*
C21	0.9307 (3)	0.3991 (2)	0.4040 (3)	0.0712 (11)
H21	0.9775	0.4188	0.4704	0.085*
C22	0.8749 (3)	0.35454 (19)	0.4088 (3)	0.0681 (10)
H22	0.8863	0.3452	0.4801	0.082*
Cr1	0.60986 (4)	0.08803 (3)	0.29232 (5)	0.0543 (2)
O2	0.69117 (19)	0.04355 (13)	0.3843 (2)	0.0739 (8)
O3	0.6203 (3)	0.09376 (18)	0.1873 (2)	0.1033 (11)
O1	0.6225 (2)	0.15268 (13)	0.3521 (3)	0.0874 (9)

	U11	U22	U33	U12	U13	U23
O4	0.069 (3)	0.058 (3)	0.271 (8)	0.000	0.090 (4)	0.000
Mg1	0.0517 (8)	0.0367 (8)	0.0523 (8)	0.000	0.0364 (7)	0.000
C12	0.0324 (13)	0.0281 (14)	0.0418 (14)	−0.0044 (10)	0.0205 (11)	−0.0012 (10)
C4	0.0358 (13)	0.0335 (15)	0.0485 (16)	−0.0045 (11)	0.0243 (13)	−0.0040 (11)
N1	0.0372 (12)	0.0352 (13)	0.0380 (12)	0.0007 (9)	0.0196 (10)	−0.0003 (9)
N2	0.0403 (12)	0.0390 (14)	0.0523 (14)	0.0048 (10)	0.0277 (11)	0.0096 (10)
C7	0.0438 (15)	0.0441 (17)	0.0387 (14)	−0.0092 (12)	0.0211 (13)	0.0024 (12)
C11	0.0356 (13)	0.0338 (14)	0.0411 (14)	−0.0048 (11)	0.0214 (12)	0.0042 (11)
O1W	0.105 (2)	0.0451 (14)	0.125 (2)	0.0226 (13)	0.0963 (19)	0.0224 (14)
C5	0.0520 (16)	0.0456 (18)	0.0575 (18)	−0.0037 (13)	0.0375 (15)	−0.0070 (14)
C2	0.0419 (15)	0.0481 (18)	0.0508 (17)	0.0093 (13)	0.0192 (14)	0.0080 (14)
C3	0.0395 (14)	0.0388 (17)	0.0640 (19)	0.0052 (12)	0.0292 (14)	0.0006 (13)
C6	0.0643 (19)	0.0529 (19)	0.0462 (16)	−0.0120 (15)	0.0373 (16)	−0.0081 (14)
C10	0.0470 (17)	0.054 (2)	0.064 (2)	0.0127 (14)	0.0293 (16)	0.0199 (15)
C1	0.0470 (16)	0.0472 (18)	0.0414 (15)	0.0003 (13)	0.0213 (14)	0.0005 (13)
C9	0.0467 (17)	0.071 (3)	0.0535 (19)	0.0029 (16)	0.0154 (16)	0.0253 (17)
C8	0.0597 (19)	0.061 (2)	0.0399 (16)	−0.0079 (16)	0.0198 (15)	0.0083 (14)
C24	0.0423 (15)	0.0439 (17)	0.0507 (16)	0.0145 (12)	0.0273 (14)	0.0063 (13)
C16	0.0462 (16)	0.0527 (19)	0.0503 (17)	0.0174 (14)	0.0268 (14)	0.0135 (14)
C23	0.0446 (16)	0.0453 (18)	0.0514 (16)	0.0152 (13)	0.0273 (14)	0.0078 (13)
C19	0.0370 (15)	0.055 (2)	0.0565 (18)	0.0120 (13)	0.0227 (14)	0.0077 (15)
N3	0.0573 (15)	0.0498 (16)	0.0617 (16)	0.0011 (12)	0.0384 (14)	0.0005 (12)
N4	0.0641 (17)	0.0592 (18)	0.0527 (15)	0.0123 (14)	0.0341 (14)	0.0042 (13)
C18	0.0449 (17)	0.064 (2)	0.068 (2)	0.0101 (15)	0.0322 (17)	0.0191 (17)
C17	0.0526 (18)	0.069 (2)	0.0556 (19)	0.0134 (16)	0.0302 (17)	0.0215 (17)
C13	0.062 (2)	0.051 (2)	0.075 (2)	−0.0018 (16)	0.0403 (19)	−0.0026 (17)
C14	0.060 (2)	0.055 (2)	0.064 (2)	0.0039 (16)	0.0255 (18)	−0.0025 (16)
C20	0.0405 (17)	0.066 (2)	0.074 (2)	0.0054 (15)	0.0244 (17)	0.0047 (18)
C15	0.060 (2)	0.062 (2)	0.0485 (17)	0.0138 (17)	0.0241 (16)	0.0055 (16)
C21	0.049 (2)	0.079 (3)	0.062 (2)	0.0107 (18)	0.0160 (18)	−0.0087 (19)
C22	0.071 (2)	0.075 (3)	0.055 (2)	0.015 (2)	0.0322 (19)	0.0016 (18)
Cr1	0.0481 (3)	0.0484 (4)	0.0652 (4)	0.0060 (2)	0.0305 (3)	0.0057 (2)
O2	0.0757 (17)	0.0743 (19)	0.0658 (15)	0.0237 (14)	0.0353 (14)	0.0140 (13)
O3	0.106 (3)	0.132 (3)	0.0579 (16)	0.020 (2)	0.0364 (17)	0.0151 (17)
O1	0.113 (2)	0.0484 (16)	0.114 (2)	−0.0003 (15)	0.071 (2)	0.0028 (15)

O4—Cr1	1.756 (2)	C9—C8	1.363 (5)
O4—Cr1i	1.756 (2)	C9—H9	0.9300
Mg1—O1Wi	2.017 (2)	C8—H8	0.9300
Mg1—O1W	2.017 (2)	C24—N3	1.355 (4)
Mg1—N2	2.210 (3)	C24—C16	1.414 (4)
Mg1—N2i	2.210 (3)	C24—C23	1.451 (4)
Mg1—N1	2.215 (2)	C16—C15	1.404 (5)
Mg1—N1i	2.215 (2)	C16—C17	1.424 (5)
C12—N1	1.354 (3)	C23—N4	1.357 (4)
C12—C4	1.401 (4)	C23—C19	1.408 (5)
C12—C11	1.446 (4)	C19—C20	1.403 (5)
C4—C3	1.410 (4)	C19—C18	1.434 (5)
C4—C5	1.431 (4)	N3—C13	1.321 (4)
N1—C1	1.329 (4)	N4—C22	1.333 (5)
N2—C10	1.337 (4)	C18—C17	1.342 (5)
N2—C11	1.359 (4)	C18—H18	0.9300
C7—C11	1.406 (4)	C17—H17	0.9300
C7—C8	1.410 (4)	C13—C14	1.387 (5)
C7—C6	1.421 (5)	C13—H13	0.9300
O1W—H1B	0.8517	C14—C15	1.359 (5)
O1W—H1A	0.8491	C14—H14	0.9300
C5—C6	1.353 (5)	C20—C21	1.358 (6)
C5—H5	0.9300	C20—H20	0.9300
C2—C3	1.356 (5)	C15—H15	0.9300
C2—C1	1.389 (4)	C21—C22	1.387 (6)
C2—H2	0.9300	C21—H21	0.9300
C3—H3	0.9300	C22—H22	0.9300
C6—H6	0.9300	Cr1—O3	1.578 (3)
C10—C9	1.378 (5)	Cr1—O2	1.597 (3)
C10—H10	0.9300	Cr1—O1	1.614 (3)
C1—H1	0.9300
Cr1—O4—Cr1i	130.3 (3)	N1—C1—H1	118.3
O1Wi—Mg1—O1W	97.08 (17)	C2—C1—H1	118.3
O1Wi—Mg1—N2	97.14 (10)	C8—C9—C10	119.2 (3)
O1W—Mg1—N2	94.70 (11)	C8—C9—H9	120.4
O1Wi—Mg1—N2i	94.70 (11)	C10—C9—H9	120.4
O1W—Mg1—N2i	97.14 (10)	C9—C8—C7	120.1 (3)
N2—Mg1—N2i	162.09 (14)	C9—C8—H8	120.0
O1Wi—Mg1—N1	88.13 (10)	C7—C8—H8	120.0
O1W—Mg1—N1	169.28 (11)	N3—C24—C16	122.5 (3)
N2—Mg1—N1	75.31 (9)	N3—C24—C23	118.2 (3)
N2i—Mg1—N1	91.73 (9)	C16—C24—C23	119.3 (3)
O1Wi—Mg1—N1i	169.28 (10)	C15—C16—C24	116.8 (3)
O1W—Mg1—N1i	88.13 (10)	C15—C16—C17	123.7 (3)
N2—Mg1—N1i	91.73 (9)	C24—C16—C17	119.5 (3)
N2i—Mg1—N1i	75.31 (9)	N4—C23—C19	123.2 (3)
N1—Mg1—N1i	88.32 (13)	N4—C23—C24	117.8 (3)
N1—C12—C4	122.9 (2)	C19—C23—C24	119.0 (3)
N1—C12—C11	117.6 (2)	C20—C19—C23	117.7 (3)
C4—C12—C11	119.5 (2)	C20—C19—C18	122.6 (3)
C12—C4—C3	117.3 (3)	C23—C19—C18	119.7 (3)
C12—C4—C5	119.8 (3)	C13—N3—C24	117.6 (3)
C3—C4—C5	122.9 (3)	C22—N4—C23	116.3 (3)
C1—N1—C12	117.6 (2)	C17—C18—C19	121.0 (3)
C1—N1—Mg1	127.7 (2)	C17—C18—H18	119.5
C12—N1—Mg1	114.72 (17)	C19—C18—H18	119.5
C10—N2—C11	117.1 (3)	C18—C17—C16	121.4 (3)
C10—N2—Mg1	128.2 (2)	C18—C17—H17	119.3
C11—N2—Mg1	114.65 (18)	C16—C17—H17	119.3
C11—C7—C8	116.6 (3)	N3—C13—C14	124.2 (3)
C11—C7—C6	119.8 (3)	N3—C13—H13	117.9
C8—C7—C6	123.7 (3)	C14—C13—H13	117.9
N2—C11—C7	123.3 (2)	C15—C14—C13	118.5 (3)
N2—C11—C12	117.7 (2)	C15—C14—H14	120.7
C7—C11—C12	119.0 (3)	C13—C14—H14	120.7
Mg1—O1W—H1B	124.0	C21—C20—C19	119.2 (4)
Mg1—O1W—H1A	122.7	C21—C20—H20	120.4
H1B—O1W—H1A	101.3	C19—C20—H20	120.4
C6—C5—C4	120.5 (3)	C14—C15—C16	120.3 (3)
C6—C5—H5	119.8	C14—C15—H15	119.9
C4—C5—H5	119.8	C16—C15—H15	119.9
C3—C2—C1	119.4 (3)	C20—C21—C22	119.2 (4)
C3—C2—H2	120.3	C20—C21—H21	120.4
C1—C2—H2	120.3	C22—C21—H21	120.4
C2—C3—C4	119.4 (3)	N4—C22—C21	124.4 (4)
C2—C3—H3	120.3	N4—C22—H22	117.8
C4—C3—H3	120.3	C21—C22—H22	117.8
C5—C6—C7	121.4 (3)	O3—Cr1—O2	108.43 (17)
C5—C6—H6	119.3	O3—Cr1—O1	111.17 (19)
C7—C6—H6	119.3	O2—Cr1—O1	108.75 (16)
N2—C10—C9	123.7 (3)	O3—Cr1—O4	110.76 (14)
N2—C10—H10	118.1	O2—Cr1—O4	106.38 (17)
C9—C10—H10	118.1	O1—Cr1—O4	111.18 (18)
N1—C1—C2	123.4 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1A···N3	0.85	2.08	2.876 (4)	156
O1W—H1B···O1	0.85	1.84	2.636 (4)	154

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1A⋯N3	0.85	2.08	2.876 (4)	156
O1W—H1B⋯O1	0.85	1.84	2.636 (4)	154