Bis(1,10-phenanthroline-κ2N,N′)(sulfato-κ2O,O′)zinc(II) propane-1,3-diol solvate

Cui, J.-D.; Zhong, K.-L.; Liu, Y.-Y.

doi:10.1107/S1600536810014194

Bis(1,10-phenanthroline-κ²N,N′)(sulfato-κ²O,O′)zinc(II) propane-1,3-diol solvate

In the title compound, [Zn(SO₄)(C₁₂H₈N₂)₂]·C₃H₈O₂, the Zn²⁺ ion (site symmetry 2) is coordinated by two chelating 1,10-phenanthroline ligands and an O,O′-bidentate sulfate ion (S site symmetry 2), resulting in a distorted cis-ZnO₂N₄ octahedral geometry for the metal ion. The complete propane-1,3-diol molecule is generated by crystallographic twofold symmetry and two O—H

O hydrogen bonds are formed with the uncoordinated O atoms of the sulfate group.

Read article Similar articles

Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536810014194/hb5408sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536810014194/hb5408Isup2.hkl Contains datablock I

CCDC reference: 764025

checkCIF report

Key indicators

Single-crystal X-ray study
T = 223 K
Mean (C-C) = 0.005 Å
R factor = 0.044
wR factor = 0.104
Data-to-parameter ratio = 12.5

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Zn1    --  O1      ..       5.22 su
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         S1
PLAT910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) .....          3
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.595          5
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors of         C13

Alert level G
PLAT333_ALERT_2_G Check Large Av C6-Ring C-C Dist. C4     -C12           1.41 Ang.

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   5 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Comment top

The title compound, (I), was obtained unitentionally during an attempt to synthesize coordination polymers of Zn(II) with 1,10-phenanthroline as second ligand via a solvothermal reaction. It is isomorphous with the recently reported cobalt(II) structure (Zhong 2010a).

In this study, the structure of Zn^II complexe with bidentate-chelating sulfate ligand, viz. [ZnSO₄(phen)₂].C₃H₈O₂, has been characterized. each Zn^II metal ion is six-coordinated in a distorted octahedral manner by four N atoms from two chelating phen ligands and two O atoms from a bidentate-chelating sulfate ligand. The formula unit lies on a twofold rotation axis [symmetry code: -x, y, - z + 1/2] passes through the Zn^II and S atoms, and also through the central carbon of the propane-1,3-diol solvent molecule, in C/2c . Around the twofold axis two planar phen ligands are arranged in a propeller manner. Intermolecular O—H···O hydrogen bonds help to further stabilize the crystal structure(see Fig. 1). Selected coordination bond distances and angles in Table 1 and intermolecular hydrogen bond see Table 2.

We discuss the title complexe and compare it with the previously reported compound [ZnSO₄(C₁₀H₈N₂)₂].C₂H₆O₂, (II) (C₁₀H₈N₂ is 2,2'-bipyridine; Zhong, 2010b). In (I), the Zn^II metal ions has an octahedral coordinaiton environment is in good agreement with that observed in (II), The Zn—O bond distance [2.174 (2) Å] and the Zn—N bond distances [2.145 (3)-2.147 (3) Å] are close to those found in (II) [2.1811 (15)Å and 2.1287 (17)-2.1452 (17) Å; respectively]. The N—Zn—N angle [77.87 (10)°] and the O—Zn—O angle [65.58 (11)°] in (I) are also comparable with values reported in (II) [76.61 (7)° and 65.64 (8)° respectively], The dihedral angle (79.8°) between the two chelating NCCN groups is slightly less than that found in (II), 81.1 (1)°.

Related literature top

For related structures and background references, see: Zhong (2010a,b).

Experimental top

0.2 mmol phen, 0.1 mmol melamine, 0.1 mmol ZnO₄.7H₂O, 2.0 ml propane-1,3-diol and 1.0 ml water were mixed and placed in a thick Pyrex tube, which was sealed and heated to 413 K for 96 h. After cooling, colorless blocks of (I) were obtained.

Structure description top

For related structures and background references, see: Zhong (2010a,b).

Computing details top

Data collection: CrystalClear (Rigaku, 2007); cell refinement: CrystalClear (Rigaku, 2007); data reduction: CrystalClear (Rigaku, 2007); 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 (Sheldrick, 2008).

Figures top

Fig. 1. The molecular structure of (I) with displacement ellipsoids drawn at the 50% probability level. The dashed lines represent O—H···O interactions. Unlabeled atoms are related to the labelled atoms by the symmetry operator(-x, y, - z + 1/2).

Bis(1,10-phenanthroline-κ²N,N')(sulfato- κ²O,O')zinc(II) propane-1,3-diol solvate top

Crystal data top

[Zn(SO₄)(C₁₂H₈N₂)₂]·C₃H₈O₂	F(000) = 1232
M_r = 597.96	D_x = 1.555 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 4259 reflections
a = 18.330 (4) Å	θ = 3.2–27.5°
b = 12.406 (3) Å	µ = 1.10 mm⁻¹
c = 13.215 (3) Å	T = 223 K
β = 121.78 (3)°	Block, colourless
V = 2554.6 (13) Å³	0.25 × 0.20 × 0.12 mm
Z = 4

Data collection top

Rigaku Mercury CCD diffractometer	2241 independent reflections
Radiation source: fine-focus sealed tube	1932 reflections with I > 2σ(I)
Graphite Monochromator monochromator	R_int = 0.039
Detector resolution: 28.5714 pixels mm^-1	θ_max = 25.0°, θ_min = 3.2°
ω scans	h = −21→15
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	k = −14→13
T_min = 0.790, T_max = 1.000	l = −14→15
7464 measured reflections

Refinement top

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)] = 0.044	H-atom parameters constrained
wR(F²) = 0.104	w = 1/[σ²(F_o²) + (0.0559P)² + 1.7701P] where P = (F_o² + 2F_c²)/3
S = 1.08	(Δ/σ)_max < 0.001
2241 reflections	Δρ_max = 0.63 e Å⁻³
179 parameters	Δρ_min = −0.34 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: 0.0021 (4)

Crystal data top

[Zn(SO₄)(C₁₂H₈N₂)₂]·C₃H₈O₂	V = 2554.6 (13) Å³
M_r = 597.96	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 18.330 (4) Å	µ = 1.10 mm⁻¹
b = 12.406 (3) Å	T = 223 K
c = 13.215 (3) Å	0.25 × 0.20 × 0.12 mm
β = 121.78 (3)°

Data collection top

Rigaku Mercury CCD diffractometer	2241 independent reflections
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	1932 reflections with I > 2σ(I)
T_min = 0.790, T_max = 1.000	R_int = 0.039
7464 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.044	0 restraints
wR(F²) = 0.104	H-atom parameters constrained
S = 1.08	Δρ_max = 0.63 e Å⁻³
2241 reflections	Δρ_min = −0.34 e Å⁻³
179 parameters

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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
Zn1	0.0000	0.31613 (4)	0.2500	0.0275 (2)
S1	0.0000	0.53713 (8)	0.2500	0.0261 (3)
O2	0.05644 (17)	0.6038 (2)	0.2306 (2)	0.0501 (7)
O1	0.05155 (15)	0.46343 (17)	0.35278 (18)	0.0386 (6)
N1	0.08295 (17)	0.29637 (19)	0.1822 (2)	0.0279 (6)
N2	0.09735 (17)	0.21096 (19)	0.3797 (2)	0.0271 (6)
C9	0.1742 (2)	0.1058 (3)	0.5575 (3)	0.0365 (8)
H9A	0.1784	0.0812	0.6268	0.044*
C5	0.2775 (2)	0.1280 (3)	0.2899 (3)	0.0354 (8)
H5A	0.3165	0.1084	0.2684	0.042*
C1	0.0755 (2)	0.3403 (3)	0.0849 (3)	0.0347 (8)
H1A	0.0310	0.3887	0.0408	0.042*
C7	0.2267 (2)	0.1149 (2)	0.4258 (2)	0.0287 (7)
C2	0.1314 (2)	0.3164 (3)	0.0470 (3)	0.0370 (8)
H2A	0.1238	0.3479	−0.0218	0.044*
C4	0.2084 (2)	0.1990 (2)	0.2154 (3)	0.0302 (7)
C3	0.1975 (2)	0.2465 (3)	0.1113 (3)	0.0374 (8)
H3A	0.2353	0.2301	0.0867	0.045*
C6	0.2869 (2)	0.0887 (3)	0.3919 (3)	0.0348 (8)
H6A	0.3331	0.0440	0.4405	0.042*
C8	0.2340 (2)	0.0767 (2)	0.5317 (3)	0.0336 (8)
H8A	0.2794	0.0321	0.5831	0.040*
C12	0.14832 (19)	0.2268 (2)	0.2462 (2)	0.0249 (6)
C10	0.1065 (2)	0.1729 (3)	0.4796 (3)	0.0325 (7)
H10A	0.0660	0.1918	0.4985	0.039*
C11	0.15675 (19)	0.1826 (2)	0.3525 (2)	0.0246 (6)
O3	0.0629 (3)	0.8156 (2)	0.1807 (3)	0.0736 (10)
H3B	0.0462	0.7553	0.1845	0.110*
C14	0.0000	0.9448 (4)	0.2500	0.0615 (17)
C13	0.0766 (4)	0.8753 (4)	0.2756 (5)	0.0860 (17)
H13A	0.1258	0.9217	0.3005	0.103*
H13B	0.0905	0.8272	0.3412	0.103*
H14B	−0.0159	0.9906	0.1817	0.103*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zn1	0.0250 (3)	0.0253 (3)	0.0328 (3)	0.000	0.0157 (2)	0.000
S1	0.0229 (6)	0.0234 (5)	0.0330 (6)	0.000	0.0153 (5)	0.000
O2	0.0474 (16)	0.0435 (14)	0.0763 (18)	−0.0092 (13)	0.0442 (14)	0.0034 (13)
O1	0.0360 (14)	0.0343 (12)	0.0306 (12)	0.0007 (11)	0.0073 (10)	0.0020 (9)
N1	0.0247 (14)	0.0276 (13)	0.0297 (13)	0.0026 (11)	0.0133 (11)	0.0027 (10)
N2	0.0284 (15)	0.0251 (13)	0.0289 (13)	−0.0018 (11)	0.0160 (11)	−0.0031 (10)
C9	0.045 (2)	0.0368 (18)	0.0274 (16)	0.0002 (16)	0.0188 (15)	0.0027 (13)
C5	0.0276 (18)	0.0409 (19)	0.0379 (17)	0.0037 (15)	0.0175 (14)	−0.0052 (14)
C1	0.0340 (19)	0.0337 (18)	0.0326 (17)	−0.0015 (15)	0.0150 (14)	0.0038 (13)
C7	0.0282 (17)	0.0241 (15)	0.0268 (15)	−0.0022 (14)	0.0096 (13)	−0.0039 (12)
C2	0.044 (2)	0.0414 (18)	0.0292 (16)	−0.0030 (17)	0.0218 (15)	0.0013 (14)
C4	0.0275 (17)	0.0332 (17)	0.0303 (16)	−0.0019 (14)	0.0155 (14)	−0.0057 (12)
C3	0.037 (2)	0.047 (2)	0.0347 (17)	−0.0002 (17)	0.0231 (15)	−0.0012 (15)
C6	0.0260 (17)	0.0337 (17)	0.0347 (17)	0.0062 (15)	0.0091 (14)	−0.0053 (13)
C8	0.0318 (18)	0.0299 (17)	0.0280 (16)	0.0039 (15)	0.0080 (14)	0.0048 (12)
C12	0.0239 (16)	0.0236 (14)	0.0245 (14)	−0.0060 (13)	0.0110 (12)	−0.0051 (12)
C10	0.0377 (19)	0.0332 (17)	0.0318 (16)	−0.0006 (15)	0.0219 (15)	−0.0003 (13)
C11	0.0258 (16)	0.0211 (14)	0.0254 (14)	−0.0021 (13)	0.0124 (12)	−0.0042 (11)
O3	0.122 (3)	0.0507 (17)	0.089 (2)	−0.0088 (18)	0.084 (2)	−0.0004 (16)
C14	0.092 (5)	0.032 (3)	0.070 (4)	0.000	0.049 (4)	0.000
C13	0.084 (4)	0.086 (4)	0.084 (3)	−0.031 (3)	0.041 (3)	−0.005 (3)

Geometric parameters (Å, º) top

Zn1—N2ⁱ	2.145 (3)	C1—H1A	0.9300
Zn1—N2	2.145 (3)	C7—C11	1.407 (4)
Zn1—N1	2.147 (3)	C7—C8	1.415 (4)
Zn1—N1ⁱ	2.147 (3)	C7—C6	1.429 (5)
Zn1—O1	2.174 (2)	C2—C3	1.363 (5)
Zn1—O1ⁱ	2.174 (2)	C2—H2A	0.9300
S1—O2	1.449 (2)	C4—C12	1.403 (5)
S1—O2ⁱ	1.449 (2)	C4—C3	1.410 (4)
S1—O1ⁱ	1.491 (2)	C3—H3A	0.9300
S1—O1	1.491 (2)	C6—H6A	0.9300
N1—C1	1.335 (4)	C8—H8A	0.9300
N1—C12	1.352 (4)	C12—C11	1.439 (4)
N2—C10	1.327 (4)	C10—H10A	0.9300
N2—C11	1.360 (4)	O3—C13	1.361 (6)
C9—C8	1.357 (5)	O3—H3B	0.8200
C9—C10	1.395 (5)	C14—C13ⁱ	1.527 (7)
C9—H9A	0.9300	C14—C13	1.527 (7)
C5—C6	1.356 (5)	C14—H14B	0.9728
C5—C4	1.427 (5)	C13—H13A	0.9700
C5—H5A	0.9300	C13—H13B	0.9700
C1—C2	1.391 (5)

N2ⁱ—Zn1—N2	105.08 (13)	N1—C1—H1A	118.7
N2ⁱ—Zn1—N1	94.08 (10)	C2—C1—H1A	118.7
N2—Zn1—N1	77.87 (10)	C11—C7—C8	117.3 (3)
N2ⁱ—Zn1—N1ⁱ	77.87 (10)	C11—C7—C6	119.6 (3)
N2—Zn1—N1ⁱ	94.08 (10)	C8—C7—C6	123.1 (3)
N1—Zn1—N1ⁱ	166.89 (13)	C3—C2—C1	119.5 (3)
N2ⁱ—Zn1—O1	156.26 (9)	C3—C2—H2A	120.3
N2—Zn1—O1	96.15 (9)	C1—C2—H2A	120.3
N1—Zn1—O1	100.74 (9)	C12—C4—C3	116.7 (3)
N1ⁱ—Zn1—O1	90.32 (9)	C12—C4—C5	119.9 (3)
N2ⁱ—Zn1—O1ⁱ	96.15 (9)	C3—C4—C5	123.4 (3)
N2—Zn1—O1ⁱ	156.26 (9)	C2—C3—C4	119.9 (3)
N1—Zn1—O1ⁱ	90.32 (9)	C2—C3—H3A	120.1
N1ⁱ—Zn1—O1ⁱ	100.74 (9)	C4—C3—H3A	120.1
O1—Zn1—O1ⁱ	65.58 (11)	C5—C6—C7	121.0 (3)
O2—S1—O2ⁱ	110.4 (2)	C5—C6—H6A	119.5
O2—S1—O1ⁱ	110.96 (14)	C7—C6—H6A	119.5
O2ⁱ—S1—O1ⁱ	110.01 (15)	C9—C8—C7	119.4 (3)
O2—S1—O1	110.01 (14)	C9—C8—H8A	120.3
O2ⁱ—S1—O1	110.96 (14)	C7—C8—H8A	120.3
O1ⁱ—S1—O1	104.33 (18)	N1—C12—C4	123.2 (3)
O2—S1—Zn1	124.79 (11)	N1—C12—C11	117.2 (3)
O2ⁱ—S1—Zn1	124.79 (11)	C4—C12—C11	119.5 (3)
O1ⁱ—S1—Zn1	52.17 (9)	N2—C10—C9	123.0 (3)
O1—S1—Zn1	52.17 (9)	N2—C10—H10A	118.5
S1—O1—Zn1	95.04 (11)	C9—C10—H10A	118.5
C1—N1—C12	118.0 (3)	N2—C11—C7	122.6 (3)
C1—N1—Zn1	128.2 (2)	N2—C11—C12	118.1 (3)
C12—N1—Zn1	113.7 (2)	C7—C11—C12	119.3 (3)
C10—N2—C11	118.1 (3)	C13—O3—H3B	109.5
C10—N2—Zn1	128.9 (2)	C13ⁱ—C14—C13	111.2 (5)
C11—N2—Zn1	113.02 (19)	C13ⁱ—C14—H14B	109.5
C8—C9—C10	119.7 (3)	C13—C14—H14B	109.1
C8—C9—H9A	120.2	O3—C13—C14	113.7 (4)
C10—C9—H9A	120.2	O3—C13—H13A	108.8
C6—C5—C4	120.7 (3)	C14—C13—H13A	108.8
C6—C5—H5A	119.7	O3—C13—H13B	108.8
C4—C5—H5A	119.7	C14—C13—H13B	108.8
N1—C1—C2	122.6 (3)	H13A—C13—H13B	107.7

N2ⁱ—Zn1—S1—O2	−110.63 (16)	O1ⁱ—Zn1—N2—C10	114.9 (3)
N2—Zn1—S1—O2	69.37 (16)	S1—Zn1—N2—C10	87.6 (3)
N1—Zn1—S1—O2	−10.36 (14)	N2ⁱ—Zn1—N2—C11	88.39 (19)
N1ⁱ—Zn1—S1—O2	169.64 (14)	N1—Zn1—N2—C11	−2.61 (19)
O1—Zn1—S1—O2	89.31 (18)	N1ⁱ—Zn1—N2—C11	166.92 (19)
O1ⁱ—Zn1—S1—O2	−90.69 (18)	O1—Zn1—N2—C11	−102.3 (2)
N2ⁱ—Zn1—S1—O2ⁱ	69.37 (16)	O1ⁱ—Zn1—N2—C11	−64.3 (3)
N2—Zn1—S1—O2ⁱ	−110.63 (16)	S1—Zn1—N2—C11	−91.61 (19)
N1—Zn1—S1—O2ⁱ	169.64 (14)	C12—N1—C1—C2	0.6 (5)
N1ⁱ—Zn1—S1—O2ⁱ	−10.36 (14)	Zn1—N1—C1—C2	−176.5 (2)
O1—Zn1—S1—O2ⁱ	−90.69 (18)	N1—C1—C2—C3	−0.8 (5)
O1ⁱ—Zn1—S1—O2ⁱ	89.31 (18)	C6—C5—C4—C12	−1.4 (5)
N2ⁱ—Zn1—S1—O1ⁱ	−19.95 (15)	C6—C5—C4—C3	176.9 (3)
N2—Zn1—S1—O1ⁱ	160.05 (15)	C1—C2—C3—C4	0.1 (5)
N1—Zn1—S1—O1ⁱ	80.33 (14)	C12—C4—C3—C2	0.6 (5)
N1ⁱ—Zn1—S1—O1ⁱ	−99.67 (14)	C5—C4—C3—C2	−177.8 (3)
O1—Zn1—S1—O1ⁱ	180.0	C4—C5—C6—C7	1.7 (5)
N2ⁱ—Zn1—S1—O1	160.05 (15)	C11—C7—C6—C5	−0.2 (5)
N2—Zn1—S1—O1	−19.95 (15)	C8—C7—C6—C5	−179.5 (3)
N1—Zn1—S1—O1	−99.67 (14)	C10—C9—C8—C7	−0.1 (5)
N1ⁱ—Zn1—S1—O1	80.33 (14)	C11—C7—C8—C9	0.4 (4)
O1ⁱ—Zn1—S1—O1	180.0	C6—C7—C8—C9	179.7 (3)
O2—S1—O1—Zn1	−119.08 (14)	C1—N1—C12—C4	0.2 (4)
O2ⁱ—S1—O1—Zn1	118.43 (14)	Zn1—N1—C12—C4	177.7 (2)
O1ⁱ—S1—O1—Zn1	0.0	C1—N1—C12—C11	178.3 (3)
N2ⁱ—Zn1—O1—S1	−42.3 (3)	Zn1—N1—C12—C11	−4.2 (3)
N2—Zn1—O1—S1	164.20 (12)	C3—C4—C12—N1	−0.8 (4)
N1—Zn1—O1—S1	85.42 (13)	C5—C4—C12—N1	177.7 (3)
N1ⁱ—Zn1—O1—S1	−101.66 (13)	C3—C4—C12—C11	−178.9 (3)
O1ⁱ—Zn1—O1—S1	0.0	C5—C4—C12—C11	−0.4 (4)
N2ⁱ—Zn1—N1—C1	76.3 (3)	C11—N2—C10—C9	0.2 (5)
N2—Zn1—N1—C1	−179.1 (3)	Zn1—N2—C10—C9	−179.0 (2)
N1ⁱ—Zn1—N1—C1	127.8 (3)	C8—C9—C10—N2	−0.2 (5)
O1—Zn1—N1—C1	−85.1 (3)	C10—N2—C11—C7	0.2 (4)
O1ⁱ—Zn1—N1—C1	−19.9 (3)	Zn1—N2—C11—C7	179.5 (2)
S1—Zn1—N1—C1	−52.2 (3)	C10—N2—C11—C12	−178.0 (3)
N2ⁱ—Zn1—N1—C12	−100.9 (2)	Zn1—N2—C11—C12	1.3 (3)
N2—Zn1—N1—C12	3.66 (19)	C8—C7—C11—N2	−0.5 (4)
N1ⁱ—Zn1—N1—C12	−49.37 (19)	C6—C7—C11—N2	−179.8 (3)
O1—Zn1—N1—C12	97.7 (2)	C8—C7—C11—C12	177.7 (3)
O1ⁱ—Zn1—N1—C12	162.9 (2)	C6—C7—C11—C12	−1.7 (4)
S1—Zn1—N1—C12	130.63 (19)	N1—C12—C11—N2	2.0 (4)
N2ⁱ—Zn1—N2—C10	−92.4 (3)	C4—C12—C11—N2	−179.8 (3)
N1—Zn1—N2—C10	176.6 (3)	N1—C12—C11—C7	−176.3 (2)
N1ⁱ—Zn1—N2—C10	−13.9 (3)	C4—C12—C11—C7	1.9 (4)
O1—Zn1—N2—C10	76.9 (3)	C13ⁱ—C14—C13—O3	65.1 (3)

Symmetry code: (i) −x, y, −z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3B···O2	0.82	1.95	2.727 (4)	157

Experimental details

Crystal data
Chemical formula	[Zn(SO₄)(C₁₂H₈N₂)₂]·C₃H₈O₂
M_r	597.96
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	223
a, b, c (Å)	18.330 (4), 12.406 (3), 13.215 (3)
β (°)	121.78 (3)
V (Å³)	2554.6 (13)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.10
Crystal size (mm)	0.25 × 0.20 × 0.12

Data collection
Diffractometer	Rigaku Mercury CCD
Absorption correction	Multi-scan (REQAB; Jacobson, 1998)
T_min, T_max	0.790, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections	7464, 2241, 1932
R_int	0.039
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.044, 0.104, 1.08
No. of reflections	2241
No. of parameters	179
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.63, −0.34

Computer programs: CrystalClear (Rigaku, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected geometric parameters (Å, º) top

Zn1—N2	2.145 (3)	Zn1—O1	2.174 (2)
Zn1—N1	2.147 (3)

N2—Zn1—N1	77.87 (10)	O1—Zn1—O1ⁱ	65.58 (11)

Symmetry code: (i) −x, y, −z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3B···O2	0.82	1.95	2.727 (4)	157

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page