Literature DB >> 21522926

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

Hong Liu1, Hui Qin, Yun-Jie Zhang, Hong-Wei Yang, Jian Zhang.   

Abstract

The Zn(II) atom in the title compound, [Zn(SO(4))(C(12)H(8)N(2))(H(2)O)(3)], is coordinated by one O atom from a sulfate dianion, two N atoms from a 1,10-phenanthroline mol-ecule and three water O atoms in an octa-hedral geometry. An intra-molecular O-H⋯O hydrogen bond occurs. Inter-molecular O-H⋯O hydrogen bonds generate a layer structure parallel to (001). There are weak C-H⋯O inter-actions within the layers.

Entities:  

Year:  2011        PMID： 21522926      PMCID： PMC3051486          DOI： 10.1107/S1600536811003138

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For related structures, see: An et al. (2007 ▶); Dietz et al. (2009 ▶); Harvey et al. (2000 ▶); Hu et al. (2009 ▶); Zheng et al. (2002 ▶).

Experimental

Crystal data

[Zn(SO4)(C12H8N2)(H2O)3] M = 395.71 Orthorhombic, a = 8.0011 (4) Å b = 9.6006 (4) Å c = 19.1606 (9) Å V = 1471.83 (12) Å3 Z = 4 Mo Kα radiation μ = 1.85 mm−1 T = 296 K 0.25 × 0.16 × 0.14 mm

Data collection

Bruker APEXII diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.710, T max = 0.785 7397 measured reflections 2793 independent reflections 2667 reflections with I > 2σ(I) R int = 0.025

Refinement

R[F 2 > 2σ(F 2)] = 0.021 wR(F 2) = 0.050 S = 1.01 2793 reflections 208 parameters H-atom parameters constrained Δρmax = 0.29 e Å−3 Δρmin = −0.36 e Å−3 Absolute structure: Flack (1983 ▶), 1165 Friedel pairs Flack parameter: 0.005 (9) Data collection: APEX2 (Bruker, 2003 ▶); cell refinement: SAINT (Bruker, 2001 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg & Berndt, 1999 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811003138/ng5108sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536811003138/ng5108Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Zn(SO4)(C12H8N2)(H2O)3]F(000) = 808
Mr = 395.71Dx = 1.786 Mg m−3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 1025 reflections
a = 8.0011 (4) Åθ = 1.5–26.5°
b = 9.6006 (4) ŵ = 1.85 mm−1
c = 19.1606 (9) ÅT = 296 K
V = 1471.83 (12) Å3Block, colourless
Z = 40.25 × 0.16 × 0.14 mm
Bruker APEXII diffractometer2793 independent reflections
Radiation source: fine-focus sealed tube2667 reflections with I > 2σ(I)
graphiteRint = 0.025
ω and φ scansθmax = 26.0°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −9→9
Tmin = 0.710, Tmax = 0.785k = −11→11
7397 measured reflectionsl = −22→23
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.021H-atom parameters constrained
wR(F2) = 0.050w = 1/[σ2(Fo2) + (0.0161P)2 + 0.005P] where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max = 0.001
2793 reflectionsΔρmax = 0.29 e Å−3
208 parametersΔρmin = −0.36 e Å−3
0 restraintsAbsolute structure: Flack (1983), 1165 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.005 (9)
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.
xyzUiso*/Ueq
Zn0.35962 (3)0.46528 (2)0.682343 (13)0.02381 (7)
S0.75438 (7)0.43014 (5)0.72471 (3)0.02418 (13)
O10.59078 (18)0.36372 (14)0.70689 (8)0.0256 (4)
O20.8188 (2)0.50361 (18)0.66363 (10)0.0400 (5)
O30.7288 (2)0.52839 (19)0.78257 (9)0.0405 (4)
O40.8701 (2)0.31908 (16)0.74536 (10)0.0368 (4)
O50.13662 (19)0.58142 (15)0.67227 (9)0.0360 (4)
H510.03450.55160.67190.043*
H520.12590.65780.69610.043*
O60.3974 (2)0.57293 (15)0.77750 (9)0.0323 (4)
H610.37750.66430.78690.039*
H620.50030.55790.79080.039*
O70.2180 (2)0.31186 (16)0.73196 (10)0.0371 (4)
H710.23850.21400.73870.044*
H720.11560.31840.73920.044*
N10.4592 (2)0.62126 (19)0.61251 (10)0.0264 (4)
N20.3537 (3)0.35890 (18)0.58398 (10)0.0291 (4)
C10.3124 (3)0.2282 (3)0.57089 (15)0.0384 (6)
H10.27980.17200.60800.046*
C20.3153 (4)0.1707 (3)0.50423 (16)0.0489 (8)
H20.28820.07750.49750.059*
C30.3584 (4)0.2526 (3)0.44882 (16)0.0491 (7)
H30.35860.21590.40390.059*
C40.4539 (4)0.4834 (4)0.40547 (14)0.0534 (8)
H40.45500.45190.35960.064*
C50.5013 (4)0.6158 (4)0.41983 (16)0.0560 (8)
H50.53330.67400.38340.067*
C60.5501 (4)0.8055 (3)0.50634 (16)0.0513 (8)
H60.57990.86780.47130.062*
C70.5510 (4)0.8461 (3)0.57495 (17)0.0478 (7)
H70.58080.93660.58700.057*
C80.5069 (3)0.7504 (3)0.62626 (15)0.0356 (6)
H80.51120.77860.67270.043*
C90.4024 (3)0.3920 (3)0.45999 (14)0.0385 (6)
C100.5032 (4)0.6680 (3)0.48954 (14)0.0401 (6)
C110.4028 (3)0.4397 (2)0.52967 (12)0.0270 (5)
C120.4559 (3)0.5801 (2)0.54475 (13)0.0274 (5)
U11U22U33U12U13U23
Zn0.02190 (13)0.02351 (11)0.02601 (13)−0.00085 (10)−0.00003 (11)0.00258 (11)
S0.0178 (3)0.0195 (2)0.0353 (3)−0.00060 (19)−0.0031 (2)−0.0023 (2)
O10.0160 (7)0.0222 (7)0.0387 (10)−0.0020 (6)−0.0036 (7)−0.0028 (6)
O20.0267 (9)0.0472 (11)0.0462 (11)−0.0069 (7)0.0022 (7)0.0116 (8)
O30.0367 (9)0.0395 (9)0.0453 (11)0.0022 (9)−0.0069 (8)−0.0196 (9)
O40.0234 (8)0.0299 (8)0.0570 (11)0.0054 (7)−0.0058 (9)0.0058 (7)
O50.0207 (8)0.0286 (7)0.0589 (11)0.0011 (7)−0.0020 (9)0.0013 (8)
O60.0331 (9)0.0277 (8)0.0361 (9)0.0088 (6)−0.0016 (7)−0.0025 (7)
O70.0239 (9)0.0271 (8)0.0601 (12)−0.0002 (7)0.0102 (8)0.0125 (8)
N10.0217 (10)0.0288 (9)0.0288 (11)−0.0013 (8)0.0015 (8)0.0004 (8)
N20.0267 (10)0.0287 (8)0.0317 (10)−0.0010 (9)−0.0033 (10)−0.0012 (8)
C10.0392 (16)0.0324 (12)0.0436 (16)−0.0071 (11)−0.0047 (12)0.0014 (11)
C20.0497 (18)0.0393 (14)0.0578 (19)−0.0062 (13)−0.0099 (14)−0.0176 (13)
C30.0487 (17)0.0583 (16)0.0402 (16)−0.0022 (15)−0.0058 (15)−0.0209 (14)
C40.0595 (18)0.076 (2)0.0244 (14)−0.0044 (17)0.0069 (12)−0.0032 (14)
C50.068 (2)0.069 (2)0.0307 (16)−0.0089 (17)0.0116 (15)0.0113 (15)
C60.0566 (19)0.0457 (16)0.0515 (19)−0.0135 (14)0.0086 (15)0.0187 (14)
C70.0550 (18)0.0332 (13)0.0553 (19)−0.0153 (13)0.0078 (15)0.0037 (13)
C80.0347 (14)0.0338 (12)0.0383 (15)−0.0065 (11)0.0018 (12)−0.0044 (11)
C90.0332 (15)0.0476 (14)0.0347 (14)0.0019 (11)−0.0005 (11)−0.0067 (12)
C100.0385 (15)0.0482 (15)0.0338 (15)−0.0037 (13)0.0085 (12)0.0071 (12)
C110.0206 (11)0.0342 (12)0.0262 (12)0.0019 (9)0.0003 (9)−0.0021 (9)
C120.0221 (12)0.0324 (11)0.0277 (12)0.0007 (9)0.0014 (10)0.0009 (10)
Zn—O72.0874 (16)C1—C21.392 (4)
Zn—O52.1128 (15)C1—H10.9300
Zn—O62.1175 (16)C2—C31.365 (4)
Zn—O12.1431 (15)C2—H20.9300
Zn—N22.1442 (19)C3—C91.400 (4)
Zn—N12.1605 (19)C3—H30.9300
S—O21.4605 (18)C4—C51.355 (5)
S—O41.4663 (16)C4—C91.425 (4)
S—O31.4698 (18)C4—H40.9300
S—O11.4955 (15)C5—C101.427 (4)
O5—H510.8655C5—H50.9300
O5—H520.8678C6—C71.371 (4)
O6—H610.9094C6—C101.409 (4)
O6—H620.8738C6—H60.9300
O7—H710.9628C7—C81.392 (4)
O7—H720.8331C7—H70.9300
N1—C81.324 (3)C8—H80.9300
N1—C121.357 (3)C9—C111.412 (3)
N2—C11.322 (3)C10—C121.405 (3)
N2—C111.356 (3)C11—C121.442 (3)
O7—Zn—O587.46 (6)N2—C1—C2123.1 (3)
O7—Zn—O691.71 (7)N2—C1—H1118.4
O5—Zn—O686.66 (6)C2—C1—H1118.4
O7—Zn—O192.72 (6)C3—C2—C1119.3 (2)
O5—Zn—O1171.49 (6)C3—C2—H2120.3
O6—Zn—O184.83 (6)C1—C2—H2120.3
O7—Zn—N292.99 (7)C2—C3—C9119.7 (3)
O5—Zn—N298.77 (7)C2—C3—H3120.2
O6—Zn—N2172.97 (7)C9—C3—H3120.2
O1—Zn—N289.73 (7)C5—C4—C9120.7 (3)
O7—Zn—N1166.26 (7)C5—C4—H4119.7
O5—Zn—N183.64 (6)C9—C4—H4119.7
O6—Zn—N198.18 (7)C4—C5—C10121.5 (3)
O1—Zn—N197.64 (6)C4—C5—H5119.2
N2—Zn—N178.11 (7)C10—C5—H5119.2
O2—S—O4110.15 (10)C7—C6—C10119.2 (3)
O2—S—O3110.09 (11)C7—C6—H6120.4
O4—S—O3110.55 (11)C10—C6—H6120.4
O2—S—O1109.39 (10)C6—C7—C8119.2 (3)
O4—S—O1107.69 (9)C6—C7—H7120.4
O3—S—O1108.91 (10)C8—C7—H7120.4
S—O1—Zn127.69 (8)N1—C8—C7123.5 (3)
Zn—O5—H51128.6N1—C8—H8118.3
Zn—O5—H52118.8C7—C8—H8118.3
H51—O5—H52101.0C3—C9—C11117.1 (2)
Zn—O6—H61128.0C3—C9—C4123.3 (3)
Zn—O6—H62107.7C11—C9—C4119.5 (2)
H61—O6—H62105.5C12—C10—C6117.5 (2)
Zn—O7—H71131.1C12—C10—C5119.4 (3)
Zn—O7—H72123.8C6—C10—C5123.1 (3)
H71—O7—H72102.6N2—C11—C9122.6 (2)
C8—N1—C12118.0 (2)N2—C11—C12117.8 (2)
C8—N1—Zn129.22 (18)C9—C11—C12119.6 (2)
C12—N1—Zn112.53 (14)N1—C12—C10122.7 (2)
C1—N2—C11118.0 (2)N1—C12—C11118.0 (2)
C1—N2—Zn128.65 (18)C10—C12—C11119.3 (2)
C11—N2—Zn113.30 (14)
O2—S—O1—Zn−66.81 (14)C12—N1—C8—C71.1 (4)
O4—S—O1—Zn173.47 (11)Zn—N1—C8—C7−172.2 (2)
O3—S—O1—Zn53.56 (15)C6—C7—C8—N1−1.8 (5)
O7—Zn—O1—S−144.44 (12)C2—C3—C9—C111.3 (4)
O6—Zn—O1—S−52.97 (12)C2—C3—C9—C4178.0 (3)
N2—Zn—O1—S122.58 (13)C5—C4—C9—C3−177.4 (3)
N1—Zn—O1—S44.62 (13)C5—C4—C9—C11−0.8 (4)
O7—Zn—N1—C8127.7 (3)C7—C6—C10—C121.4 (4)
O5—Zn—N1—C877.8 (2)C7—C6—C10—C5−178.9 (3)
O6—Zn—N1—C8−7.9 (2)C4—C5—C10—C120.4 (5)
O1—Zn—N1—C8−93.7 (2)C4—C5—C10—C6−179.3 (3)
N2—Zn—N1—C8178.2 (2)C1—N2—C11—C93.6 (3)
O7—Zn—N1—C12−45.9 (4)Zn—N2—C11—C9−177.59 (18)
O5—Zn—N1—C12−95.77 (15)C1—N2—C11—C12−176.9 (2)
O6—Zn—N1—C12178.55 (15)Zn—N2—C11—C121.9 (3)
O1—Zn—N1—C1292.71 (15)C3—C9—C11—N2−3.9 (4)
N2—Zn—N1—C124.61 (15)C4—C9—C11—N2179.3 (2)
O7—Zn—N2—C1−15.4 (2)C3—C9—C11—C12176.6 (2)
O5—Zn—N2—C1−103.3 (2)C4—C9—C11—C12−0.2 (4)
O1—Zn—N2—C177.3 (2)C8—N1—C12—C101.0 (3)
N1—Zn—N2—C1175.2 (2)Zn—N1—C12—C10175.37 (19)
O7—Zn—N2—C11165.96 (15)C8—N1—C12—C11−179.6 (2)
O5—Zn—N2—C1178.08 (16)Zn—N1—C12—C11−5.2 (2)
O1—Zn—N2—C11−101.33 (16)C6—C10—C12—N1−2.2 (4)
N1—Zn—N2—C11−3.46 (15)C5—C10—C12—N1178.1 (3)
C11—N2—C1—C2−0.7 (4)C6—C10—C12—C11178.4 (3)
Zn—N2—C1—C2−179.3 (2)C5—C10—C12—C11−1.3 (4)
N2—C1—C2—C3−1.8 (5)N2—C11—C12—N12.3 (3)
C1—C2—C3—C91.4 (5)C9—C11—C12—N1−178.2 (2)
C9—C4—C5—C100.7 (5)N2—C11—C12—C10−178.2 (2)
C10—C6—C7—C80.4 (5)C9—C11—C12—C101.3 (3)
D—H···AD—HH···AD···AD—H···A
O5—H51···O2i0.871.792.655 (2)174
O5—H52···O4ii0.871.912.775 (2)172
O6—H61···O1ii0.911.932.809 (2)161
O6—H62···O30.871.862.688 (2)158
O7—H71···O3iii0.961.852.769 (3)160
O7—H72···O4i0.831.972.797 (2)173
C1—H1···O3iii0.932.513.416 (3)165
Table 1

Selected bond lengths (Å)

Zn—O72.0874 (16)
Zn—O52.1128 (15)
Zn—O62.1175 (16)
Zn—O12.1431 (15)
Zn—N22.1442 (19)
Zn—N12.1605 (19)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O5—H51⋯O2i0.871.792.655 (2)174
O5—H52⋯O4ii0.871.912.775 (2)172
O6—H61⋯O1ii0.911.932.809 (2)161
O6—H62⋯O30.871.862.688 (2)158
O7—H71⋯O3iii0.961.852.769 (3)160
O7—H72⋯O4i0.831.972.797 (2)173
C1—H1⋯O3iii0.932.513.416 (3)165

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

  2 in total

1.  Three new ZnII sulfate complexes

Authors: 
Journal:  Acta Crystallogr C       Date:  2000-07       Impact factor: 1.172

2.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290
  2 in total

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