mer-Triaqua-(1,10-phenanthroline-κN,N')(sulfato-κO)magnesium(II).

In the title compound, [Mg(SO(4))(C(12)H(8)N(2))(H(2)O)(3)], the Mg(II) centre exhibits a slightly distorted octa-hedral coordination environment defined by two N atoms from a 1,10-phenanthroline mol-ecule, one O atom from a sulfate dianion and three meridionally arranged O atoms from coordinated water mol-ecules. The crystal structure involves intra- and intermolecular O-H⋯O hydrogen bonds.

Related literature

For copper(II), zinc(II) and cadmium(II) complexes of phenanthroline, see: Xu et al. (2003 ▶); Zhang et al. (1999 ▶).

Experimental

Crystal data

[Mg(SO4)(C12H8N2)(H2O)3]

M = 354.62

Monoclinic,

a = 11.968 (2) Å

b = 10.025 (2) Å

c = 13.798 (3) Å

β = 113.53 (3)°

V = 1517.8 (6) Å3

Z = 4

Mo Kα radiation

μ = 0.29 mm−1

T = 295 (2) K

0.36 × 0.28 × 0.20 mm

Data collection

Rigaku R-AXIS RAPID diffractometer

Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.902, T max = 0.944

14532 measured reflections

3454 independent reflections

2941 reflections with I > 2σ(I)

R int = 0.023

Refinement

R[F 2 > 2σ(F 2)] = 0.033

wR(F 2) = 0.098

S = 1.07

3454 reflections

226 parameters

9 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.39 e Å−3

Δρmin = −0.30 e Å−3

Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 ▶); 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: SHELXL97.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808009938/im2060sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808009938/im2060Isup2.hkl

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

[Mg(SO4)(C12H8N2)(H2O)3]	F000 = 736
Mr = 354.62	Dx = 1.552 Mg m−3
Monoclinic, P21/c	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 11791 reflections
a = 11.968 (2) Å	θ = 3.0–27.5º
b = 10.025 (2) Å	µ = 0.29 mm−1
c = 13.798 (3) Å	T = 295 (2) K
β = 113.53 (3)º	Prism, colorless
V = 1517.8 (6) Å3	0.36 × 0.28 × 0.20 mm
Z = 4

Rigaku R-AXIS RAPID diffractometer	3454 independent reflections
Radiation source: fine-focus sealed tube	2941 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.023
Detector resolution: 10.000 pixels mm-1	θmax = 27.5º
T = 295(2) K	θmin = 3.0º
ω scans	h = −15→15
Absorption correction: multi-scan(ABSCOR; Higashi, 1995)	k = −12→13
Tmin = 0.902, Tmax = 0.944	l = −17→17
14532 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)] = 0.033	H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.098	w = 1/[σ2(Fo2) + (0.059P)2 + 0.2998P] where P = (Fo2 + 2Fc2)/3
S = 1.07	(Δ/σ)max = 0.001
3454 reflections	Δρmax = 0.39 e Å−3
226 parameters	Δρmin = −0.30 e Å−3
9 restraints	Extinction correction: none
Primary atom site location: structure-invariant direct methods

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
Mg1	0.13726 (4)	0.25963 (5)	0.47420 (4)	0.02612 (13)
S1	−0.06777 (3)	0.22093 (3)	0.57725 (3)	0.02562 (11)
O1	−0.17699 (10)	0.15328 (13)	0.50549 (11)	0.0455 (3)
O1W	0.19239 (10)	0.09656 (11)	0.57638 (9)	0.0334 (2)
O2	0.01644 (11)	0.12166 (11)	0.65134 (9)	0.0366 (3)
O2W	0.08603 (12)	0.40809 (11)	0.36365 (9)	0.0391 (3)
O3	−0.09964 (11)	0.32153 (11)	0.63949 (9)	0.0384 (3)
O3W	0.06431 (12)	0.13366 (12)	0.34794 (9)	0.0446 (3)
O4	−0.00451 (10)	0.28537 (12)	0.51813 (9)	0.0382 (3)
N1	0.32491 (12)	0.24769 (13)	0.47706 (11)	0.0356 (3)
N2	0.24343 (11)	0.41322 (12)	0.58883 (10)	0.0298 (3)
C1	0.36509 (19)	0.1648 (2)	0.42311 (17)	0.0524 (5)
H1	0.3098	0.1075	0.3744	0.063*
C2	0.4875 (2)	0.1602 (2)	0.4366 (2)	0.0659 (6)
H2	0.5124	0.0993	0.3983	0.079*
C3	0.56924 (19)	0.2443 (2)	0.5052 (2)	0.0598 (6)
H3	0.6504	0.2424	0.5138	0.072*
C4	0.53087 (15)	0.3344 (2)	0.56323 (15)	0.0440 (4)
C5	0.61079 (16)	0.4266 (2)	0.63750 (18)	0.0583 (6)
H5	0.6930	0.4274	0.6495	0.070*
C6	0.56954 (18)	0.5119 (2)	0.69028 (16)	0.0587 (6)
H6	0.6237	0.5711	0.7381	0.070*
C7	0.44359 (16)	0.51409 (19)	0.67458 (13)	0.0443 (4)
C8	0.3943 (2)	0.6039 (2)	0.72430 (16)	0.0599 (6)
H8	0.4441	0.6679	0.7702	0.072*
C9	0.2739 (2)	0.5983 (2)	0.70592 (16)	0.0574 (5)
H9	0.2405	0.6589	0.7379	0.069*
C10	0.20141 (16)	0.50001 (17)	0.63810 (13)	0.0407 (4)
H10	0.1196	0.4955	0.6271	0.049*
C11	0.40669 (13)	0.33127 (16)	0.54670 (12)	0.0324 (3)
C12	0.36302 (13)	0.42130 (15)	0.60482 (11)	0.0311 (3)
H2W1	0.0974 (17)	0.4912 (10)	0.3757 (13)	0.047*
H3W1	0.0497 (17)	0.0531 (11)	0.3577 (14)	0.047*
H1W1	0.1920 (16)	0.0180 (12)	0.5506 (14)	0.047*
H2W2	0.0668 (18)	0.3949 (17)	0.2979 (8)	0.047*
H1W2	0.1422 (15)	0.0933 (18)	0.6067 (14)	0.047*
H3W2	0.0186 (15)	0.1583 (17)	0.2863 (9)	0.047*

	U11	U22	U33	U12	U13	U23
Mg1	0.0285 (3)	0.0215 (2)	0.0276 (3)	−0.00238 (18)	0.0104 (2)	−0.00030 (17)
S1	0.03023 (19)	0.01845 (18)	0.03043 (19)	−0.00086 (12)	0.01448 (15)	−0.00115 (12)
O1	0.0335 (6)	0.0388 (7)	0.0627 (8)	−0.0073 (5)	0.0177 (6)	−0.0200 (6)
O1W	0.0371 (6)	0.0265 (5)	0.0364 (6)	0.0044 (4)	0.0145 (5)	0.0030 (4)
O2	0.0492 (6)	0.0277 (6)	0.0367 (6)	0.0085 (5)	0.0212 (5)	0.0088 (4)
O2W	0.0656 (8)	0.0205 (5)	0.0299 (5)	−0.0014 (5)	0.0177 (5)	0.0015 (4)
O3	0.0519 (7)	0.0244 (5)	0.0410 (6)	0.0034 (5)	0.0206 (5)	−0.0070 (4)
O3W	0.0656 (8)	0.0230 (6)	0.0317 (6)	−0.0114 (5)	0.0054 (6)	−0.0001 (4)
O4	0.0349 (5)	0.0378 (6)	0.0470 (7)	0.0080 (5)	0.0216 (5)	0.0181 (5)
N1	0.0396 (7)	0.0303 (7)	0.0425 (8)	0.0008 (5)	0.0223 (7)	−0.0016 (5)
N2	0.0311 (6)	0.0278 (6)	0.0303 (6)	−0.0003 (5)	0.0121 (5)	−0.0022 (5)
C1	0.0600 (12)	0.0448 (11)	0.0648 (12)	0.0045 (9)	0.0380 (10)	−0.0088 (9)
C2	0.0752 (15)	0.0628 (14)	0.0839 (16)	0.0239 (12)	0.0573 (14)	0.0053 (12)
C3	0.0444 (11)	0.0698 (14)	0.0799 (16)	0.0211 (10)	0.0403 (12)	0.0285 (12)
C4	0.0306 (8)	0.0519 (11)	0.0512 (10)	0.0054 (7)	0.0182 (8)	0.0233 (8)
C5	0.0272 (8)	0.0749 (15)	0.0629 (12)	−0.0076 (9)	0.0076 (9)	0.0273 (11)
C6	0.0416 (9)	0.0677 (14)	0.0484 (10)	−0.0247 (10)	−0.0015 (9)	0.0075 (10)
C7	0.0443 (9)	0.0438 (10)	0.0339 (8)	−0.0147 (8)	0.0041 (7)	0.0006 (7)
C8	0.0755 (14)	0.0480 (12)	0.0442 (10)	−0.0217 (10)	0.0114 (10)	−0.0191 (9)
C9	0.0798 (15)	0.0431 (11)	0.0507 (11)	−0.0004 (10)	0.0276 (11)	−0.0178 (9)
C10	0.0481 (9)	0.0356 (9)	0.0394 (8)	0.0042 (7)	0.0186 (7)	−0.0049 (7)
C11	0.0291 (7)	0.0323 (8)	0.0364 (8)	0.0009 (6)	0.0137 (6)	0.0103 (6)
C12	0.0313 (7)	0.0298 (7)	0.0283 (7)	−0.0041 (6)	0.0078 (6)	0.0036 (6)

Mg1—O4	2.0333 (13)	C1—C2	1.403 (3)
Mg1—O2W	2.0423 (12)	C1—H1	0.9300
Mg1—O3W	2.0439 (13)	C2—C3	1.350 (3)
Mg1—O1W	2.0864 (12)	C2—H2	0.9300
Mg1—N2	2.2096 (14)	C3—C4	1.401 (3)
Mg1—N1	2.2335 (15)	C3—H3	0.9300
S1—O1	1.4545 (12)	C4—C11	1.411 (2)
S1—O4	1.4659 (11)	C4—C5	1.427 (3)
S1—O3	1.4702 (11)	C5—C6	1.339 (3)
S1—O2	1.4929 (12)	C5—H5	0.9300
O1W—H1W1	0.864 (9)	C6—C7	1.435 (3)
O1W—H1W2	0.859 (19)	C6—H6	0.9300
O2W—H2W1	0.850 (9)	C7—C8	1.397 (3)
O2W—H2W2	0.852 (9)	C7—C12	1.407 (2)
O3W—H3W1	0.848 (9)	C8—C9	1.361 (3)
O3W—H3W2	0.843 (9)	C8—H8	0.9300
N1—C1	1.327 (2)	C9—C10	1.397 (3)
N1—C11	1.354 (2)	C9—H9	0.9300
N2—C10	1.321 (2)	C10—H10	0.9300
N2—C12	1.3607 (19)	C11—C12	1.437 (2)
O4—Mg1—O2W	95.32 (5)	N1—C1—C2	122.7 (2)
O4—Mg1—O3W	102.08 (6)	N1—C1—H1	118.7
O2W—Mg1—O3W	85.12 (5)	C2—C1—H1	118.7
O4—Mg1—O1W	88.53 (5)	C3—C2—C1	119.86 (19)
O2W—Mg1—O1W	174.49 (5)	C3—C2—H2	120.1
O3W—Mg1—O1W	90.23 (5)	C1—C2—H2	120.1
O4—Mg1—N2	90.46 (5)	C2—C3—C4	119.51 (17)
O2W—Mg1—N2	86.69 (5)	C2—C3—H3	120.2
O3W—Mg1—N2	165.60 (6)	C4—C3—H3	120.2
O1W—Mg1—N2	97.24 (5)	C3—C4—C11	117.25 (18)
O4—Mg1—N1	162.63 (6)	C3—C4—C5	123.33 (18)
O2W—Mg1—N1	92.99 (6)	C11—C4—C5	119.42 (19)
O3W—Mg1—N1	93.80 (6)	C6—C5—C4	121.16 (17)
O1W—Mg1—N1	84.35 (5)	C6—C5—H5	119.4
N2—Mg1—N1	74.81 (5)	C4—C5—H5	119.4
O1—S1—O4	110.49 (8)	C5—C6—C7	121.38 (18)
O1—S1—O3	110.20 (7)	C5—C6—H6	119.3
O4—S1—O3	109.56 (7)	C7—C6—H6	119.3
O1—S1—O2	109.44 (8)	C8—C7—C12	116.99 (17)
O4—S1—O2	108.51 (6)	C8—C7—C6	124.00 (18)
O3—S1—O2	108.60 (7)	C12—C7—C6	119.01 (18)
Mg1—O1W—H1W1	119.2 (13)	C9—C8—C7	120.31 (17)
Mg1—O1W—H1W2	105.4 (13)	C9—C8—H8	119.8
H1W1—O1W—H1W2	106.0 (12)	C7—C8—H8	119.8
Mg1—O2W—H2W1	126.3 (12)	C8—C9—C10	118.85 (18)
Mg1—O2W—H2W2	123.7 (12)	C8—C9—H9	120.6
H2W1—O2W—H2W2	108.3 (13)	C10—C9—H9	120.6
Mg1—O3W—H3W1	119.9 (12)	N2—C10—C9	123.16 (17)
Mg1—O3W—H3W2	124.3 (13)	N2—C10—H10	118.4
H3W1—O3W—H3W2	110.3 (13)	C9—C10—H10	118.4
S1—O4—Mg1	141.98 (7)	N1—C11—C4	123.02 (16)
C1—N1—C11	117.67 (15)	N1—C11—C12	117.63 (13)
C1—N1—Mg1	127.63 (13)	C4—C11—C12	119.34 (16)
C11—N1—Mg1	114.61 (10)	N2—C12—C7	122.64 (15)
C10—N2—C12	117.98 (14)	N2—C12—C11	117.74 (13)
C10—N2—Mg1	126.81 (11)	C7—C12—C11	119.62 (15)
C12—N2—Mg1	115.12 (10)
O1—S1—O4—Mg1	−99.19 (14)	C2—C3—C4—C5	179.9 (2)
O3—S1—O4—Mg1	139.21 (13)	C3—C4—C5—C6	179.20 (19)
O2—S1—O4—Mg1	20.79 (15)	C11—C4—C5—C6	−1.3 (3)
O2W—Mg1—O4—S1	166.33 (13)	C4—C5—C6—C7	0.1 (3)
O3W—Mg1—O4—S1	80.20 (14)	C5—C6—C7—C8	−177.5 (2)
O1W—Mg1—O4—S1	−9.73 (14)	C5—C6—C7—C12	2.2 (3)
N2—Mg1—O4—S1	−106.96 (14)	C12—C7—C8—C9	1.0 (3)
N1—Mg1—O4—S1	−75.4 (2)	C6—C7—C8—C9	−179.3 (2)
O4—Mg1—N1—C1	146.11 (19)	C7—C8—C9—C10	1.1 (3)
O2W—Mg1—N1—C1	−95.33 (16)	C12—N2—C10—C9	−0.5 (2)
O3W—Mg1—N1—C1	−10.02 (16)	Mg1—N2—C10—C9	−176.88 (14)
O1W—Mg1—N1—C1	79.84 (16)	C8—C9—C10—N2	−1.4 (3)
N2—Mg1—N1—C1	178.93 (17)	C1—N1—C11—C4	0.5 (2)
O4—Mg1—N1—C11	−30.2 (2)	Mg1—N1—C11—C4	177.26 (12)
O2W—Mg1—N1—C11	88.34 (11)	C1—N1—C11—C12	179.79 (16)
O3W—Mg1—N1—C11	173.64 (11)	Mg1—N1—C11—C12	−3.49 (17)
O1W—Mg1—N1—C11	−96.50 (11)	C3—C4—C11—N1	−1.1 (2)
N2—Mg1—N1—C11	2.60 (10)	C5—C4—C11—N1	179.40 (15)
O4—Mg1—N2—C10	−14.19 (14)	C3—C4—C11—C12	179.68 (15)
O2W—Mg1—N2—C10	81.12 (14)	C5—C4—C11—C12	0.2 (2)
O3W—Mg1—N2—C10	136.5 (2)	C10—N2—C12—C7	2.7 (2)
O1W—Mg1—N2—C10	−102.77 (13)	Mg1—N2—C12—C7	179.56 (12)
N1—Mg1—N2—C10	175.12 (14)	C10—N2—C12—C11	−176.75 (14)
O4—Mg1—N2—C12	169.30 (10)	Mg1—N2—C12—C11	0.08 (17)
O2W—Mg1—N2—C12	−95.39 (11)	C8—C7—C12—N2	−3.0 (2)
O3W—Mg1—N2—C12	−40.0 (3)	C6—C7—C12—N2	177.28 (15)
O1W—Mg1—N2—C12	80.72 (11)	C8—C7—C12—C11	176.47 (16)
N1—Mg1—N2—C12	−1.39 (10)	C6—C7—C12—C11	−3.3 (2)
C11—N1—C1—C2	0.7 (3)	N1—C11—C12—N2	2.3 (2)
Mg1—N1—C1—C2	−175.54 (16)	C4—C11—C12—N2	−178.38 (14)
N1—C1—C2—C3	−1.4 (3)	N1—C11—C12—C7	−177.16 (14)
C1—C2—C3—C4	0.8 (3)	C4—C11—C12—C7	2.1 (2)
C2—C3—C4—C11	0.4 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O2W—H2W1···O3i	0.850 (9)	1.891 (11)	2.7170 (17)	163.8 (16)
O3W—H3W1···O2ii	0.848 (9)	1.906 (10)	2.7375 (17)	166.2 (17)
O1W—H1W1···O1ii	0.864 (9)	1.862 (10)	2.7235 (17)	174.8 (17)
O2W—H2W2···O2iii	0.852 (9)	1.873 (10)	2.7232 (17)	175.4 (19)
O1W—H1W2···O2	0.859 (19)	1.862 (19)	2.7030 (17)	166.0 (19)
O3W—H3W2···O3iii	0.843 (9)	1.965 (10)	2.7961 (19)	168.5 (17)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2W—H2W1⋯O3i	0.850 (9)	1.891 (11)	2.7170 (17)	163.8 (16)
O3W—H3W1⋯O2ii	0.848 (9)	1.906 (10)	2.7375 (17)	166.2 (17)
O1W—H1W1⋯O1ii	0.864 (9)	1.862 (10)	2.7235 (17)	174.8 (17)
O2W—H2W2⋯O2iii	0.852 (9)	1.873 (10)	2.7232 (17)	175.4 (19)
O1W—H1W2⋯O2	0.859 (19)	1.862 (19)	2.7030 (17)	166.0 (19)
O3W—H3W2⋯O3iii	0.843 (9)	1.965 (10)	2.7961 (19)	168.5 (17)

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