Literature DB >> 21202200

Poly[[diaqua-bis[μ-(2,4-dichloro-phen-oxy)acetato]calcium(II)] monohydrate].

Wen-Dong Song, Xiang-Hu Huang, Jian-Bin Yan, De-Yun Ma.   

Abstract

In the title coordination polymer, {[Ca(C(8)H(5)Cl(2)O(3))(2)(H(2)O)(2)]·H(2)O}(n), the Ca(II) atom is eight-coordinated by six O atoms from four different (2,4-dichloro-phen-oxy)acetate ligands and two water mol-ecules, and displays a distorted square-anti-prismatic coordination geometry. The compound forms an infinite zigzag chain through connection of the metal centers by (2,4-dichlorphen-oxy)acetate ligands and hydrogen bonding of coordinated and inter-stitial water mol-ecules. These chains are further hydrogen bonded with neighboring chains, forming a supra-molecular network.

Entities:  

Year:  2008        PMID： 21202200      PMCID： PMC2961213          DOI： 10.1107/S1600536808009379

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


Related literature

For related literature, see: Song et al. (2006 ▶); Hao et al. (2006 ▶).

Experimental

Crystal data

[Ca(C8H5Cl2O3)2(H2O)2]·H2O M = 534.17 Monoclinic, a = 17.8354 (7) Å b = 6.8077 (3) Å c = 18.5276 (8) Å β = 101.297 (3)° V = 2206.00 (16) Å3 Z = 4 Mo Kα radiation μ = 0.81 mm−1 T = 296 (2) K 0.30 × 0.26 × 0.23 mm

Data collection

Bruker APEXII area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.790, T max = 0.840 15522 measured reflections 5049 independent reflections 2962 reflections with I > 2σ(I) R int = 0.047

Refinement

R[F 2 > 2σ(F 2)] = 0.050 wR(F 2) = 0.158 S = 1.00 5049 reflections 289 parameters 9 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.55 e Å−3 Δρmin = −0.60 e Å−3 Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT (Bruker, 2004 ▶); data reduction: SAINT; 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. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808009379/zl2102sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808009379/zl2102Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ca(C8H5Cl2O3)2(H2O)2]·H2OF000 = 1088
Mr = 534.17Dx = 1.608 Mg m−3
Monoclinic, P21/cMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 5837 reflections
a = 17.8354 (7) Åθ = 2.8–27.9º
b = 6.8077 (3) ŵ = 0.81 mm−1
c = 18.5276 (8) ÅT = 296 (2) K
β = 101.297 (3)ºBlock, colorless
V = 2206.00 (16) Å30.30 × 0.26 × 0.23 mm
Z = 4
Bruker APEXII area-detector diffractometer5049 independent reflections
Radiation source: fine-focus sealed tube2962 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.047
T = 296(2) Kθmax = 27.5º
φ and ω scansθmin = 1.2º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)h = −22→23
Tmin = 0.790, Tmax = 0.840k = −8→8
15522 measured reflectionsl = −23→24
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.050H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.158  w = 1/[σ2(Fo2) + (0.0794P)2] where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max < 0.001
5049 reflectionsΔρmax = 0.55 e Å−3
289 parametersΔρmin = −0.60 e Å−3
9 restraintsExtinction 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.
xyzUiso*/Ueq
C10.10806 (18)0.6762 (5)0.41264 (16)0.0380 (7)
C20.18125 (18)0.6618 (5)0.46951 (19)0.0450 (8)
H2A0.17070.60230.51400.054*
H2B0.21750.57900.45100.054*
C30.28244 (17)0.8609 (6)0.53280 (18)0.0448 (9)
C40.3216 (2)1.0370 (6)0.5327 (2)0.0570 (10)
C50.3898 (2)1.0689 (7)0.5798 (3)0.0700 (13)
H50.41561.18740.57910.084*
C60.4196 (2)0.9231 (7)0.6281 (2)0.0621 (11)
C70.3831 (2)0.7454 (7)0.6279 (2)0.0622 (11)
H70.40460.64630.66000.075*
C80.31519 (19)0.7145 (6)0.5804 (2)0.0555 (10)
H80.29080.59370.58010.067*
C9−0.24793 (17)1.0577 (5)0.26633 (18)0.0408 (8)
C10−0.2516 (2)1.2253 (6)0.2240 (2)0.0529 (10)
H10−0.21561.32430.23730.063*
C11−0.3083 (2)1.2475 (7)0.1617 (2)0.0632 (11)
H11−0.31121.36220.13400.076*
C12−0.3600 (2)1.1003 (8)0.1412 (2)0.0655 (12)
C13−0.3568 (2)0.9291 (7)0.1815 (2)0.0638 (12)
H13−0.39190.82890.16680.077*
C14−0.30089 (18)0.9088 (6)0.2439 (2)0.0481 (9)
C15−0.13933 (18)1.1724 (5)0.35198 (17)0.0400 (8)
H15A−0.11351.14850.40230.048*
H15B−0.16371.30010.35020.048*
C16−0.08085 (15)1.1739 (5)0.30233 (15)0.0290 (6)
Ca1−0.02416 (3)0.67481 (9)0.29818 (3)0.03103 (18)
Cl10.28379 (8)1.21602 (17)0.46954 (10)0.1105 (6)
Cl20.50445 (6)0.9670 (2)0.69082 (8)0.1050 (5)
Cl3−0.43126 (7)1.1255 (3)0.06300 (7)0.1062 (5)
Cl4−0.29530 (6)0.69273 (16)0.29402 (7)0.0722 (3)
O10.07745 (13)0.5164 (3)0.39084 (12)0.0501 (6)
O20.08134 (12)0.8394 (3)0.38986 (12)0.0456 (6)
O30.21318 (13)0.8512 (4)0.48578 (14)0.0531 (7)
O4−0.06060 (11)1.0138 (3)0.27914 (11)0.0369 (5)
O5−0.05492 (12)1.3347 (3)0.28650 (12)0.0387 (5)
O6−0.19623 (11)1.0256 (3)0.33051 (12)0.0427 (6)
O1W−0.10329 (14)0.6837 (4)0.38884 (13)0.0494 (6)
H2W−0.1418 (13)0.750 (5)0.3754 (18)0.074*
H1W−0.0840 (18)0.731 (5)0.4291 (12)0.074*
O2W−0.12281 (14)0.6700 (4)0.18973 (12)0.0480 (6)
H3W−0.123 (2)0.766 (3)0.1629 (15)0.072*
H4W−0.122 (2)0.577 (3)0.1615 (14)0.072*
O3W0.0390 (2)0.1918 (4)0.47185 (15)0.0702 (8)
H5W0.047 (3)0.286 (3)0.444 (2)0.105*
H6W0.049 (3)0.084 (3)0.453 (2)0.105*
U11U22U33U12U13U23
C10.0464 (17)0.033 (2)0.0330 (15)−0.0011 (16)0.0041 (13)0.0020 (17)
C20.0487 (18)0.035 (2)0.0459 (17)0.0030 (16)−0.0045 (14)−0.0007 (18)
C30.0376 (16)0.045 (2)0.0480 (18)0.0036 (16)−0.0011 (14)−0.0061 (18)
C40.051 (2)0.038 (2)0.075 (2)0.0067 (18)−0.0046 (18)−0.008 (2)
C50.047 (2)0.053 (3)0.103 (3)−0.003 (2)−0.005 (2)−0.016 (3)
C60.0421 (19)0.069 (3)0.068 (2)0.007 (2)−0.0073 (17)−0.020 (3)
C70.056 (2)0.070 (3)0.055 (2)0.013 (2)−0.0043 (18)0.003 (2)
C80.0472 (19)0.059 (3)0.056 (2)−0.0014 (19)−0.0016 (16)0.005 (2)
C90.0363 (15)0.039 (2)0.0495 (18)0.0025 (15)0.0130 (14)−0.0018 (18)
C100.0451 (18)0.045 (2)0.067 (2)0.0010 (18)0.0072 (17)0.009 (2)
C110.051 (2)0.067 (3)0.070 (3)0.010 (2)0.0087 (19)0.017 (2)
C120.044 (2)0.083 (3)0.067 (2)0.002 (2)0.0049 (18)0.000 (3)
C130.050 (2)0.075 (3)0.066 (2)−0.015 (2)0.0083 (18)−0.014 (3)
C140.0439 (18)0.045 (2)0.058 (2)−0.0077 (17)0.0157 (16)−0.007 (2)
C150.0465 (17)0.0297 (19)0.0453 (17)−0.0031 (15)0.0128 (14)−0.0073 (17)
C160.0321 (13)0.0212 (17)0.0317 (14)−0.0017 (13)0.0012 (11)−0.0023 (15)
Ca10.0361 (3)0.0204 (3)0.0360 (3)−0.0013 (3)0.0055 (2)−0.0010 (3)
Cl10.0981 (9)0.0400 (7)0.1650 (15)−0.0089 (7)−0.0439 (10)0.0245 (8)
Cl20.0585 (6)0.1143 (12)0.1209 (11)0.0061 (7)−0.0348 (6)−0.0308 (10)
Cl30.0697 (7)0.1599 (15)0.0775 (8)0.0059 (8)−0.0140 (6)0.0030 (9)
Cl40.0734 (6)0.0479 (7)0.0945 (8)−0.0211 (5)0.0145 (6)0.0040 (6)
O10.0637 (14)0.0287 (14)0.0493 (13)−0.0065 (12)−0.0102 (11)−0.0002 (12)
O20.0485 (12)0.0296 (14)0.0523 (13)−0.0008 (11)−0.0060 (10)0.0041 (12)
O30.0491 (13)0.0330 (14)0.0660 (15)0.0001 (11)−0.0159 (11)0.0012 (13)
O40.0465 (11)0.0192 (12)0.0479 (12)0.0012 (10)0.0163 (10)−0.0007 (11)
O50.0455 (11)0.0198 (12)0.0528 (13)−0.0056 (10)0.0143 (10)−0.0036 (11)
O60.0399 (11)0.0360 (14)0.0535 (13)−0.0074 (11)0.0121 (10)0.0018 (12)
O1W0.0600 (15)0.0416 (16)0.0490 (13)0.0065 (13)0.0161 (11)0.0002 (13)
O2W0.0533 (13)0.0359 (15)0.0495 (13)0.0035 (13)−0.0031 (11)−0.0039 (12)
O3W0.109 (2)0.0463 (18)0.0554 (16)−0.0093 (19)0.0159 (15)−0.0003 (15)
C1—O11.248 (4)C14—Cl41.732 (4)
C1—O21.250 (4)C15—O61.424 (4)
C1—C21.512 (4)C15—C161.520 (4)
C2—O31.417 (4)C15—H15A0.9700
C2—H2A0.9700C15—H15B0.9700
C2—H2B0.9700C16—O51.246 (3)
C3—O31.367 (4)C16—O41.251 (3)
C3—C81.382 (5)C16—Ca1i2.888 (3)
C3—C41.387 (5)Ca1—O5ii2.379 (2)
C4—C51.370 (5)Ca1—O1W2.397 (2)
C4—Cl11.732 (4)Ca1—O2W2.398 (2)
C5—C61.370 (6)Ca1—O42.405 (2)
C5—H50.9300Ca1—O12.485 (2)
C6—C71.373 (6)Ca1—O4iii2.527 (2)
C6—Cl21.745 (4)Ca1—O22.536 (2)
C7—C81.367 (5)Ca1—O5iii2.550 (2)
C7—H70.9300Ca1—C16iii2.888 (3)
C8—H80.9300Ca1—Ca1iii4.0148 (6)
C9—O61.372 (4)Ca1—Ca1i4.0148 (6)
C9—C101.379 (5)O4—Ca1i2.527 (2)
C9—C141.392 (5)O5—Ca1iv2.379 (2)
C10—C111.386 (5)O5—Ca1i2.550 (2)
C10—H100.9300O1W—H2W0.818 (10)
C11—C121.364 (6)O1W—H1W0.823 (10)
C11—H110.9300O2W—H3W0.822 (10)
C12—C131.379 (6)O2W—H4W0.823 (10)
C12—Cl31.739 (4)O3W—H5W0.850 (10)
C13—C141.379 (5)O3W—H6W0.848 (10)
C13—H130.9300
O1—C1—O2123.5 (3)O2W—Ca1—O1152.75 (8)
O1—C1—C2115.6 (3)O4—Ca1—O1131.10 (8)
O2—C1—C2120.9 (3)O5ii—Ca1—O4iii71.29 (7)
O3—C2—C1110.2 (3)O1W—Ca1—O4iii155.21 (8)
O3—C2—H2A109.6O2W—Ca1—O4iii86.63 (8)
C1—C2—H2A109.6O4—Ca1—O4iii120.50 (6)
O3—C2—H2B109.6O1—Ca1—O4iii76.53 (8)
C1—C2—H2B109.6O5ii—Ca1—O2128.21 (8)
H2A—C2—H2B108.1O1W—Ca1—O288.91 (8)
O3—C3—C8126.0 (3)O2W—Ca1—O2153.37 (8)
O3—C3—C4115.7 (3)O4—Ca1—O279.51 (7)
C8—C3—C4118.3 (3)O1—Ca1—O251.97 (7)
C5—C4—C3121.4 (4)O4iii—Ca1—O297.10 (7)
C5—C4—Cl1119.9 (3)O5ii—Ca1—O5iii120.33 (6)
C3—C4—Cl1118.7 (3)O1W—Ca1—O5iii153.23 (8)
C4—C5—C6118.9 (4)O2W—Ca1—O5iii83.90 (8)
C4—C5—H5120.6O4—Ca1—O5iii70.50 (7)
C6—C5—H5120.6O1—Ca1—O5iii101.18 (8)
C5—C6—C7120.9 (3)O4iii—Ca1—O5iii51.11 (7)
C5—C6—Cl2119.0 (4)O2—Ca1—O5iii78.24 (7)
C7—C6—Cl2120.1 (3)O5ii—Ca1—C16iii96.11 (8)
C8—C7—C6119.8 (4)O1W—Ca1—C16iii175.59 (8)
C8—C7—H7120.1O2W—Ca1—C16iii85.51 (8)
C6—C7—H7120.1O4—Ca1—C16iii95.63 (8)
C7—C8—C3120.7 (4)O1—Ca1—C16iii88.12 (8)
C7—C8—H8119.7O4iii—Ca1—C16iii25.61 (7)
C3—C8—H8119.7O2—Ca1—C16iii86.73 (8)
O6—C9—C10125.0 (3)O5iii—Ca1—C16iii25.52 (7)
O6—C9—C14116.4 (3)O5ii—Ca1—Ca1iii36.91 (5)
C10—C9—C14118.6 (3)O1W—Ca1—Ca1iii122.70 (6)
C9—C10—C11120.6 (4)O2W—Ca1—Ca1iii78.57 (6)
C9—C10—H10119.7O4—Ca1—Ca1iii145.47 (6)
C11—C10—H10119.7O1—Ca1—Ca1iii75.42 (6)
C12—C11—C10119.6 (4)O4iii—Ca1—Ca1iii34.50 (5)
C12—C11—H11120.2O2—Ca1—Ca1iii118.48 (6)
C10—C11—H11120.2O5iii—Ca1—Ca1iii84.01 (5)
C11—C12—C13121.1 (4)C16iii—Ca1—Ca1iii59.25 (7)
C11—C12—Cl3120.2 (4)O5ii—Ca1—Ca1i148.24 (6)
C13—C12—Cl3118.7 (3)O1W—Ca1—Ca1i119.82 (6)
C14—C13—C12119.0 (4)O2W—Ca1—Ca1i79.94 (6)
C14—C13—H13120.5O4—Ca1—Ca1i36.54 (5)
C12—C13—H13120.5O1—Ca1—Ca1i118.95 (6)
C13—C14—C9121.0 (4)O4iii—Ca1—Ca1i84.92 (5)
C13—C14—Cl4119.4 (3)O2—Ca1—Ca1i74.18 (5)
C9—C14—Cl4119.6 (3)O5iii—Ca1—Ca1i34.07 (5)
O6—C15—C16111.8 (2)C16iii—Ca1—Ca1i59.49 (7)
O6—C15—H15A109.3Ca1iii—Ca1—Ca1i115.95 (3)
C16—C15—H15A109.3C1—O1—Ca193.37 (19)
O6—C15—H15B109.3C1—O2—Ca190.98 (19)
C16—C15—H15B109.3C3—O3—C2117.1 (3)
H15A—C15—H15B107.9C16—O4—Ca1150.93 (19)
O5—C16—O4122.7 (3)C16—O4—Ca1i93.54 (17)
O5—C16—C15118.6 (3)Ca1—O4—Ca1i108.96 (8)
O4—C16—C15118.7 (3)C16—O5—Ca1iv157.43 (19)
O5—C16—Ca1i61.88 (15)C16—O5—Ca1i92.60 (17)
O4—C16—Ca1i60.85 (14)Ca1iv—O5—Ca1i109.02 (8)
C15—C16—Ca1i177.18 (19)C9—O6—C15116.8 (3)
O5ii—Ca1—O1W86.07 (8)Ca1—O1W—H2W112 (3)
O5ii—Ca1—O2W78.00 (8)Ca1—O1W—H1W117 (3)
O1W—Ca1—O2W98.71 (9)H2W—O1W—H1W103.9 (16)
O5ii—Ca1—O4150.41 (8)Ca1—O2W—H3W114 (3)
O1W—Ca1—O484.21 (8)Ca1—O2W—H4W116 (3)
O2W—Ca1—O475.96 (8)H3W—O2W—H4W103.2 (16)
O5ii—Ca1—O176.38 (8)H5W—O3W—H6W109.8 (17)
O1W—Ca1—O188.67 (8)
D—H···AD—HH···AD···AD—H···A
O3W—H6W···O2ii0.848 (10)2.176 (14)3.013 (4)169 (3)
O2W—H4W···O2iii0.823 (10)2.079 (16)2.866 (3)160 (4)
O2W—H3W···O1i0.822 (10)2.205 (18)2.986 (4)159 (4)
O1W—H1W···O3Wv0.823 (10)1.927 (11)2.745 (4)173 (4)
O3W—H5W···O10.850 (10)1.986 (12)2.830 (4)172 (5)
O1W—H2W···Cl40.818 (10)2.88 (2)3.530 (3)138 (3)
O1W—H2W···O60.818 (10)2.20 (2)2.938 (3)150 (4)
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O3W—H6W⋯O2i0.848 (10)2.176 (14)3.013 (4)169 (3)
O2W—H4W⋯O2ii0.823 (10)2.079 (16)2.866 (3)160 (4)
O2W—H3W⋯O1iii0.822 (10)2.205 (18)2.986 (4)159 (4)
O1W—H1W⋯O3Wiv0.823 (10)1.927 (11)2.745 (4)173 (4)
O3W—H5W⋯O10.850 (10)1.986 (12)2.830 (4)172 (5)
O1W—H2W⋯Cl40.818 (10)2.88 (2)3.530 (3)138 (3)
O1W—H2W⋯O60.818 (10)2.20 (2)2.938 (3)150 (4)

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

  1 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290
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1.  Crystal structures of the potassium and rubidium salts of (3,5-di-chloro-phen-oxy)acetic acid: two isotypic coordination polymers.

Authors:  Graham Smith
Journal:  Acta Crystallogr E Crystallogr Commun       Date:  2015-09-17
  1 in total

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