Diaqua­bis(1,10-phenanthroline)magnesium dichromate(VI) 1,10-phenanthroline disolvate

Liu, H.-X.; Dong, G.-Y.; Ma, Z.-H.; Cui, G.-H.

doi:10.1107/S1600536809030128

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 9| September 2009| Page m1026

doi:10.1107/S1600536809030128

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Diaquabis(1,10-phenanthroline)magnesium dichromate(VI) 1,10-phenanthroline disolvate

Hai-Xing Liu,^a Gui-Ying Dong,^b Zhi-Hong Ma ^c and Guang-Hua Cui ^b ^*

^aMicroscale Science Institute, College of Chemistry and Chemical Engineering, Weifang University, Weifang 261061, People's Republic of China, ^bCollege of Chemical Engineering and Biotechnology, Hebei Polytechnic University, Tangshan 063009, People's Republic of China, and ^cCollege of Basic Medicine, Hebei Medical University, Shijiazhuang 050017, People's Republic of China
^*Correspondence e-mail: tscghua@126.com

(Received 25 July 2009; accepted 29 July 2009; online 8 August 2009)

In the title compound, [Mg(C₁₂H₈N₂)₂(H₂O)₂][Cr₂O₇]·2C₁₂H₈N₂, 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 molecules in a distorted octahedral geometry. Intermolecular O—H⋯N and O—H⋯O hydrogen bonds and π–π interactions between the aromatic rings [shortest centroid–centroid separation = 3.527 (2) Å] link the cations, anions and 1,10-phenanthroline solvent molecules 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_r = 997.16
Monoclinic, C 2/c
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[F² > 2σ(F²)] = 0.051
wR(F²) = 0.155
S = 1.06
3817 reflections
308 parameters
H-atom parameters constrained
Δρ_max = 0.87 e Å⁻³
Δρ_min = −0.46 e Å⁻³

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

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.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809030128/cv2597sup1.cif

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

checkCIF report

Comment top

1,10-Phenanthroline (phen), which is the parent of an important class of chelating agents, has been widely used in the construction of supramolecular architectures. Some magnesium(II)-phenanthroline complexes have been synthesized and reported (Zhu et al., 2008; Hao et al. 2008; Zhang, 2004). As a continuation of these studies, we now report the crystal structure of the title complex (I).

X-ray structure analysis reveals that (I) is an ionic monomeric Mg^II complex (Fig. 1) with two solvent phen molecules. The Mg(II) ion is surrounded by four N atoms from the two phen ligands and two O atoms from two coordinated water molecules to form distorted MgN₄O₂ octahedron. The Mg—O(2.018 (2)–2.018 (3) Å) and Mg—N (2.211 (3)–2.215 (2) Å) bond lengths are normal.

In the crystal structure, intermolecular O—H···N and O—H···O hydrogen bonds (Table 1) and π–π interactions between the aromatic rings with the shortest centroid-centroid separation of 3.527 (2) Å, link cation, anion and two solvent 1,10-phenanthroline molecules into a hydrogen-bonded cluster (Fig. 1).

Related literature top

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

Experimental top

Magnesium chloride, potassium dichromate and 1,10-phenanthroline (molar ratio 1:1:4) were dissolved in water-ethanol mixture (1:1 v/v, 50 ml) and refluxed for 3 h. The resulting solution was allowed to stand at room temperature for a week and yellow crystals of (I) were obtained.

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT (Bruker, 1999); 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 (Sheldrick, 2008).

Figures top

Fig. 1. The hydrogen-bonded (dashed lines) cluster in (I) showing the atomic numbering and 30% probability displacement ellipsoids. Unlabelled atoms are related with the labelled ones by symmetry [-x + 1, y, 1/2 - z]. H atoms not involved in hydrogen-bonding are omitted for clarity.

Diaquabis(1,10-phenanthroline)magnesium(II) dichromate(VI) 1,10-phenanthroline disolvate top

Crystal data top

[Mg(C₁₂H₈N₂)₂(H₂O)₂][Cr₂O₇]·2C₁₂H₈N₂	F(000) = 2048
M_r = 997.16	D_x = 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

Data collection top

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

Refinement top

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(F_o²) + (0.0878P)² + 5.6611P] where P = (F_o² + 2F_c²)/3
3817 reflections	(Δ/σ)_max < 0.001
308 parameters	Δρ_max = 0.87 e Å⁻³
0 restraints	Δρ_min = −0.46 e Å⁻³

Crystal data top

[Mg(C₁₂H₈N₂)₂(H₂O)₂][Cr₂O₇]·2C₁₂H₈N₂	V = 4338 (2) Å³
M_r = 997.16	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 16.761 (3) Å	µ = 0.59 mm⁻¹
b = 22.172 (4) Å	T = 293 K
c = 13.996 (3) Å	0.30 × 0.28 × 0.21 mm
β = 123.49 (3)°

Data collection top

Bruker SMART CCD area-detector diffractometer	3817 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	3068 reflections with I > 2σ(I)
T_min = 0.826, T_max = 0.878	R_int = 0.020
16762 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.051	0 restraints
wR(F²) = 0.155	H-atom parameters constrained
S = 1.06	Δρ_max = 0.87 e Å⁻³
3817 reflections	Δρ_min = −0.46 e Å⁻³
308 parameters

Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º) top

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

Experimental details

Crystal data
Chemical formula	[Mg(C₁₂H₈N₂)₂(H₂O)₂][Cr₂O₇]·2C₁₂H₈N₂
M_r	997.16
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	293
a, b, c (Å)	16.761 (3), 22.172 (4), 13.996 (3)
β (°)	123.49 (3)
V (Å³)	4338 (2)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	0.59
Crystal size (mm)	0.30 × 0.28 × 0.21

Data collection
Diffractometer	Bruker SMART CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.826, 0.878
No. of measured, independent and observed [I > 2σ(I)] reflections	16762, 3817, 3068
R_int	0.020
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.051, 0.155, 1.06
No. of reflections	3817
No. of parameters	308
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.87, −0.46

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

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

Acknowledgements

The authors thank Weifang University and the Scientific Research Fund of Hebei Provincial Education Department (project No. 2006114) for financial support.

References

Bruker (1998). SMART. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruker (1999). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Hao, X.-M., Gu, C.-S., Song, W.-D. & Liu, J.-W. (2008). Acta Cryst. E64, m1052. Web of Science CSD CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Zhang, B.-S. (2004). Chin. J. Struct. Chem. 23, 1411–1415. CAS Google Scholar
Zhu, L., Huang, J., Han, S.-Y. & An, Z. (2008). Acta Cryst. E64, m683. Web of Science CSD CrossRef IUCr Journals Google Scholar

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Volume 65| Part 9| September 2009| Page m1026

doi:10.1107/S1600536809030128

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Di­aqua­bis­(1,10-phenanthroline)magnesium dichromate(VI) 1,10-phenanthroline disolvate

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Diaquabis(1,10-phenanthroline)magnesium dichromate(VI) 1,10-phenanthroline disolvate