Literature DB >> 21578657

Poly[[diaqua-(μ(4)-1H-benzimidazole-5,6-dicarboxyl-ato)strontium] monohydrate].

Wen-Dong Song, Hao Wang, Juan-Hua Liu, Xiao-Tian Ma, Seik Weng Ng.   

Abstract

Each of the carboxyl-ate -CO(2) fragments of the dianion ligand in the title compound, {[Sr(C(9)H(4)N(2)O(4))(H(2)O)(2)]·H(2)O}(n), chelates to a Sr(II) atom and at the same time, one of the two O atoms coordinates to a third Sr(II) atom. The μ(4)-bridging mode of the dianion generates a square-grid layer motif; adjacent layers are connected by O-H⋯O, O-H⋯N and N-H⋯O hydrogen bonds, forming a three-dimensional network. The eight-coordinate Sr atom exists in a distorted square-anti-prismatic geometry. The crystal studied was a non-merohedral twin with a minor twin component of 24%.

Entities:  

Year:  2009        PMID： 21578657      PMCID： PMC2971846          DOI： 10.1107/S1600536809048284

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


Related literature

For the crystal structures of other metal salts of dicarboxylic acid, see: Gao et al. (2008 ▶); Lo et al. (2007 ▶); Song et al. (2009a ▶,b ▶). For the treated of diffraction data of twinned crystals, see: Spek (2009 ▶).

Experimental

Crystal data

[Sr(C9H4N2O4)(H2O)2]·H2O M = 345.81 Triclinic, a = 6.909 (1) Å b = 7.093 (1) Å c = 13.037 (2) Å α = 80.860 (5)° β = 83.974 (5)° γ = 71.795 (4)° V = 598.2 (2) Å3 Z = 2 Mo Kα radiation μ = 4.54 mm−1 T = 293 K 0.31 × 0.24 × 0.20 mm

Data collection

Rigaku R-AXIS RAPID IP diffractometer Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.334, T max = 0.464 5799 measured reflections 2695 independent reflections 2339 reflections with I > 2σ(I) R int = 0.075

Refinement

R[F 2 > 2σ(F 2)] = 0.076 wR(F 2) = 0.214 S = 1.05 2695 reflections 173 parameters H-atom parameters constrained Δρmax = 2.69 e Å−3 Δρmin = −2.12 e Å−3 Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalClear (Rigaku/MSC, 2002 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: OLEX (Dolomanov et al., 2003 ▶) and X-SEED (Barbour, 2001 ▶); software used to prepare material for publication: publCIF (Westrip, 2009 ▶). Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809048284/xu2672sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809048284/xu2672Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Sr(C9H4N2O4)(H2O)2]·H2OZ = 2
Mr = 345.81F(000) = 344
Triclinic, P1Dx = 1.920 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.909 (1) ÅCell parameters from 5129 reflections
b = 7.093 (1) Åθ = 3.1–27.5°
c = 13.037 (2) ŵ = 4.54 mm−1
α = 80.860 (5)°T = 293 K
β = 83.974 (5)°Block, colorless
γ = 71.795 (4)°0.31 × 0.24 × 0.20 mm
V = 598.2 (2) Å3
Rigaku R-AXIS RAPID IP diffractometer2695 independent reflections
Radiation source: fine-focus sealed tube2339 reflections with I > 2σ(I)
graphiteRint = 0.075
ω scanθmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)h = −8→8
Tmin = 0.334, Tmax = 0.464k = −9→9
5799 measured reflectionsl = −16→16
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.076Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.214H-atom parameters constrained
S = 1.05w = 1/[σ2(Fo2) + (0.1352P)2 + 1.3937P] where P = (Fo2 + 2Fc2)/3
2695 reflections(Δ/σ)max = 0.001
173 parametersΔρmax = 2.69 e Å−3
0 restraintsΔρmin = −2.12 e Å−3
xyzUiso*/Ueq
Sr10.25457 (8)0.25734 (8)0.46107 (4)0.0207 (3)
O10.4011 (8)0.3453 (8)0.6171 (5)0.0353 (13)
O20.1154 (7)0.5758 (7)0.5744 (4)0.0261 (10)
O30.3642 (7)0.8869 (7)0.5721 (4)0.0268 (10)
O40.0729 (8)1.0928 (8)0.6225 (5)0.0401 (14)
O1w0.2542 (8)0.5682 (8)0.3316 (4)0.0327 (12)
H110.35960.60020.33700.049*
H120.15020.66310.34430.049*
O2w0.2942 (10)0.0310 (10)0.3189 (6)0.0502 (17)
H210.30870.09530.26020.075*
H220.1896−0.00640.32130.075*
O3w0.3469 (12)0.0350 (11)1.0913 (6)0.0594 (19)
H3w10.31650.14851.05550.089*
H3w20.4687−0.02481.07400.089*
N10.2543 (11)0.4413 (11)1.0195 (5)0.0378 (16)
N20.1892 (12)0.7679 (11)1.0241 (5)0.0387 (16)
H2N0.16400.88301.04800.046*
C10.2549 (10)0.4986 (9)0.6338 (5)0.0198 (12)
C20.2500 (9)0.5836 (9)0.7336 (5)0.0192 (12)
C30.2665 (11)0.4524 (10)0.8249 (6)0.0254 (14)
H30.29160.31600.82390.031*
C40.2448 (11)0.5298 (11)0.9184 (6)0.0281 (15)
C50.2019 (11)0.7366 (11)0.9214 (6)0.0276 (14)
C60.1836 (11)0.8687 (10)0.8295 (6)0.0267 (14)
H60.15501.00550.83080.032*
C70.2086 (9)0.7926 (9)0.7361 (5)0.0190 (12)
C80.2165 (9)0.9307 (9)0.6363 (5)0.0216 (13)
C100.2225 (14)0.5909 (14)1.0781 (6)0.042 (2)
H100.22430.56921.15030.051*
U11U22U33U12U13U23
Sr10.0175 (4)0.0190 (4)0.0219 (4)−0.0002 (2)−0.0012 (2)−0.0025 (3)
O10.027 (3)0.032 (3)0.042 (3)0.008 (2)−0.010 (2)−0.017 (2)
O20.022 (2)0.028 (2)0.026 (3)−0.0030 (18)−0.0043 (19)−0.007 (2)
O30.020 (2)0.026 (2)0.029 (3)−0.0029 (18)0.0065 (19)−0.002 (2)
O40.030 (3)0.026 (3)0.045 (3)0.011 (2)0.010 (2)0.005 (2)
O1w0.026 (3)0.030 (3)0.039 (3)−0.006 (2)0.004 (2)−0.004 (2)
O2w0.047 (4)0.051 (4)0.057 (4)−0.009 (3)−0.012 (3)−0.024 (3)
O3w0.066 (5)0.045 (4)0.066 (5)−0.016 (3)−0.013 (4)0.001 (4)
N10.049 (4)0.045 (4)0.020 (3)−0.018 (3)−0.005 (3)0.000 (3)
N20.055 (4)0.039 (4)0.024 (3)−0.011 (3)0.000 (3)−0.017 (3)
C10.018 (3)0.020 (3)0.022 (3)−0.004 (2)0.000 (2)−0.005 (2)
C20.014 (3)0.019 (3)0.022 (3)−0.001 (2)−0.002 (2)−0.005 (2)
C30.032 (4)0.020 (3)0.027 (4)−0.009 (2)−0.002 (3)−0.005 (3)
C40.035 (4)0.030 (4)0.021 (4)−0.012 (3)−0.005 (3)−0.001 (3)
C50.033 (4)0.027 (3)0.025 (4)−0.011 (3)−0.003 (3)−0.005 (3)
C60.034 (4)0.019 (3)0.026 (4)−0.007 (3)0.000 (3)−0.004 (3)
C70.020 (3)0.015 (3)0.021 (3)−0.004 (2)0.002 (2)−0.003 (2)
C80.016 (3)0.021 (3)0.025 (3)0.000 (2)−0.001 (2)−0.008 (3)
C100.049 (5)0.058 (5)0.018 (4)−0.013 (4)−0.006 (3)0.000 (3)
Sr1—O12.604 (5)O2w—H220.8400
Sr1—O22.760 (5)O3w—H3w10.8400
Sr1—O2i2.516 (5)O3w—H3w20.8400
Sr1—O3ii2.711 (5)N1—C101.354 (11)
Sr1—O3iii2.528 (5)N1—C41.366 (9)
Sr1—O4ii2.635 (6)N2—C101.302 (11)
Sr1—O1w2.554 (5)N2—C51.381 (9)
Sr1—O2w2.579 (6)N2—H2N0.8800
O1—C11.262 (8)C1—C21.511 (9)
O2—C11.233 (8)C2—C31.382 (10)
O2—Sr1i2.516 (5)C2—C71.424 (8)
O3—C81.242 (8)C3—C41.390 (10)
O3—Sr1iii2.528 (5)C3—H30.9300
O3—Sr1iv2.711 (5)C4—C51.409 (9)
O4—C81.264 (8)C5—C61.390 (10)
O4—Sr1iv2.635 (6)C6—C71.383 (9)
O1w—H110.8400C6—H60.9300
O1w—H120.8400C7—C81.506 (9)
O2w—H210.8400C10—H100.9300
O2i—Sr1—O3iii159.81 (17)Sr1—O1w—H12109.5
O2i—Sr1—O1w75.51 (17)H11—O1w—H12109.5
O3iii—Sr1—O1w90.53 (16)Sr1—O2w—H21109.5
O2i—Sr1—O2w90.93 (18)Sr1—O2w—H22109.5
O3iii—Sr1—O2w75.39 (19)H21—O2w—H22109.5
O1w—Sr1—O2w94.2 (2)H3w1—O3w—H3w2107.1
O2i—Sr1—O1118.96 (15)C10—N1—C4106.1 (7)
O3iii—Sr1—O177.00 (17)C10—N2—C5105.4 (7)
O1w—Sr1—O198.63 (19)C10—N2—H2N127.3
O2w—Sr1—O1149.54 (18)C5—N2—H2N127.3
O2i—Sr1—O4ii78.71 (17)O2—C1—O1122.9 (6)
O3iii—Sr1—O4ii118.75 (16)O2—C1—C2119.6 (6)
O1w—Sr1—O4ii148.09 (16)O1—C1—C2117.4 (6)
O2w—Sr1—O4ii104.7 (2)C3—C2—C7120.5 (6)
O1—Sr1—O4ii77.8 (2)C3—C2—C1117.0 (5)
O2i—Sr1—O3ii118.90 (16)C7—C2—C1122.2 (6)
O3iii—Sr1—O3ii73.35 (17)C2—C3—C4118.1 (6)
O1w—Sr1—O3ii163.41 (16)C2—C3—H3120.9
O2w—Sr1—O3ii78.2 (2)C4—C3—H3120.9
O1—Sr1—O3ii81.86 (17)N1—C4—C3132.1 (7)
O4ii—Sr1—O3ii48.37 (14)N1—C4—C5106.2 (6)
O2i—Sr1—O272.84 (17)C3—C4—C5121.7 (7)
O3iii—Sr1—O2117.87 (16)N2—C5—C6131.4 (7)
O1w—Sr1—O274.33 (16)N2—C5—C4108.4 (6)
O2w—Sr1—O2161.91 (19)C6—C5—C4120.1 (7)
O1—Sr1—O248.13 (14)C7—C6—C5118.6 (6)
O4ii—Sr1—O280.35 (17)C7—C6—H6120.7
O3ii—Sr1—O2116.38 (15)C5—C6—H6120.7
O1—Sr1—C8ii76.73 (18)C6—C7—C2121.0 (6)
C1—O1—Sr197.5 (4)C6—C7—C8118.7 (5)
C1—O2—Sr1i152.2 (5)C2—C7—C8119.9 (6)
C1—O2—Sr190.8 (4)O3—C8—O4122.0 (7)
Sr1i—O2—Sr1107.16 (17)O3—C8—C7120.0 (5)
C8—O3—Sr1iii148.1 (5)O4—C8—C7117.9 (6)
C8—O3—Sr1iv92.8 (4)N2—C10—N1113.9 (7)
Sr1iii—O3—Sr1iv106.65 (17)N2—C10—H10123.0
C8—O4—Sr1iv95.9 (4)N1—C10—H10123.0
Sr1—O1w—H11109.5
O2i—Sr1—O1—C1−13.7 (5)C1—C2—C3—C4−174.6 (6)
O3iii—Sr1—O1—C1153.0 (5)C10—N1—C4—C3179.6 (8)
O1w—Sr1—O1—C164.5 (5)C10—N1—C4—C5−1.3 (9)
O2w—Sr1—O1—C1178.4 (4)C2—C3—C4—N1−179.4 (8)
O4ii—Sr1—O1—C1−83.2 (4)C2—C3—C4—C51.6 (10)
O3ii—Sr1—O1—C1−132.3 (5)C10—N2—C5—C6−178.7 (9)
O2—Sr1—O1—C14.7 (4)C10—N2—C5—C40.0 (9)
O2i—Sr1—O2—C1158.5 (5)N1—C4—C5—N20.8 (9)
O3iii—Sr1—O2—C1−40.1 (4)C3—C4—C5—N2−180.0 (7)
O1w—Sr1—O2—C1−122.2 (4)N1—C4—C5—C6179.7 (7)
O2w—Sr1—O2—C1−174.5 (6)C3—C4—C5—C6−1.1 (11)
O1—Sr1—O2—C1−4.8 (4)N2—C5—C6—C7178.5 (8)
O4ii—Sr1—O2—C177.4 (4)C4—C5—C6—C7−0.1 (11)
O3ii—Sr1—O2—C144.2 (4)C5—C6—C7—C20.7 (10)
O2i—Sr1—O2—Sr1i0.0C5—C6—C7—C8−172.0 (6)
O3iii—Sr1—O2—Sr1i161.42 (17)C3—C2—C7—C6−0.2 (9)
O1w—Sr1—O2—Sr1i79.3 (2)C1—C2—C7—C6173.1 (6)
O2w—Sr1—O2—Sr1i27.0 (7)C3—C2—C7—C8172.4 (6)
O1—Sr1—O2—Sr1i−163.2 (3)C1—C2—C7—C8−14.3 (9)
O4ii—Sr1—O2—Sr1i−81.1 (2)Sr1iii—O3—C8—O4138.1 (7)
O3ii—Sr1—O2—Sr1i−114.29 (18)Sr1iv—O3—C8—O49.6 (7)
Sr1i—O2—C1—O1139.9 (8)Sr1iii—O3—C8—C7−39.6 (12)
Sr1—O2—C1—O18.8 (7)Sr1iv—O3—C8—C7−168.1 (5)
Sr1i—O2—C1—C2−37.6 (12)Sr1iv—O4—C8—O3−9.9 (7)
Sr1—O2—C1—C2−168.8 (5)Sr1iv—O4—C8—C7167.8 (5)
Sr1—O1—C1—O2−9.4 (8)C6—C7—C8—O3125.0 (7)
Sr1—O1—C1—C2168.3 (5)C2—C7—C8—O3−47.8 (9)
O2—C1—C2—C3125.8 (7)C6—C7—C8—O4−52.8 (9)
O1—C1—C2—C3−51.9 (9)C2—C7—C8—O4134.4 (7)
O2—C1—C2—C7−47.7 (9)C5—N2—C10—N1−0.9 (10)
O1—C1—C2—C7134.6 (7)C4—N1—C10—N21.4 (10)
C7—C2—C3—C4−0.9 (9)
D—H···AD—HH···AD···AD—H···A
O1w—H11···O1iii0.841.982.81 (1)167
O1w—H12···O4v0.842.002.83 (1)173
O2w—H21···O3wvi0.842.282.95 (1)136
O2w—H22···O4i0.842.122.93 (1)162
O3w—H3w1···N10.841.972.78 (1)160
O3w—H3w2···O3wvii0.842.393.01 (2)132
N2—H2n···O3wiv0.882.072.75 (1)134
Table 1

Selected bond lengths (Å)

Sr1—O12.604 (5)
Sr1—O22.760 (5)
Sr1—O2i 2.516 (5)
Sr1—O3ii 2.711 (5)
Sr1—O3iii 2.528 (5)
Sr1—O4ii 2.635 (6)
Sr1—O1w 2.554 (5)
Sr1—O2w 2.579 (6)

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

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A D⋯A D—H⋯A
O1w—H11⋯O1iii 0.841.982.81 (1)167
O1w—H12⋯O4iv 0.842.002.83 (1)173
O2w—H21⋯O3w v 0.842.282.95 (1)136
O2w—H22⋯O4i 0.842.122.93 (1)162
O3w—H3w1⋯N10.841.972.78 (1)160
O3w—H3w2⋯O3w vi 0.842.393.01 (2)132
N2—H2n⋯O3w vii 0.882.072.75 (1)134

Symmetry codes: (i) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) .

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4.  Penta-aqua-(1H-benzimidazole-5,6-dicarboxyl-ato-κN)nickel(II) penta-hydrate.

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Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-05-23

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