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The title structure, [Zn(C5H10Cl2O6P2)(H2O)3]n, consists of one-dimensional chains. The structure is best described as centrosymmetric monomeric units consisting of octahedral Zn atoms with two symmetrically chelating [Cl2C(PO3Et)2]2− ligands, connected into polymeric chains along the [110] direction by further octahedral Zn atoms.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805005957/lh6370sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805005957/lh6370Isup2.hkl
Contains datablock I

CCDC reference: 270472

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.020
  • wR factor = 0.053
  • Data-to-parameter ratio = 18.0

checkCIF/PLATON results

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Alert level C PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.20 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.08 Ratio
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Nonius, 1997); cell refinement: DENZO/SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO/SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXL97.

catena-Poly[diaquazinc(II)-µ-(diethyl dichloromethylenebisphosphonato)- κ3O,O':O''-tetraaquazinc(II)-µ-(diethyl dichloromethylenebisphosphonato)- κ3O:O',O''] top
Crystal data top
[Zn(C5H10Cl2O6P2)(H2O)3]Z = 2
Mr = 418.39F(000) = 424
Triclinic, P1Dx = 1.934 Mg m3
Dm = 1.90 (1) Mg m3
Dm measured by flotation in cyclohexane/bromoform
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.3809 (1) ÅCell parameters from 13591 reflections
b = 8.3383 (1) Åθ = 2.5–27.0°
c = 11.8498 (2) ŵ = 2.34 mm1
α = 94.659 (1)°T = 120 K
β = 97.724 (1)°Plate, colourless
γ = 93.244 (1)°0.20 × 0.15 × 0.08 mm
V = 718.60 (2) Å3
Data collection top
Nonius KappaCCD
diffractometer
3136 independent reflections
Radiation source: fine-focus sealed tube2852 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.037
φ scans and ω scans with κ offsetsθmax = 27.0°, θmin = 2.5°
Absorption correction: multi-scan
(XPREP in SHELXTL; Bruker, 1998)
h = 89
Tmin = 0.652, Tmax = 0.835k = 1010
13591 measured reflectionsl = 1515
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.020Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.053H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0245P)2 + 0.3604P]
where P = (Fo2 + 2Fc2)/3
3136 reflections(Δ/σ)max < 0.001
174 parametersΔρmax = 0.46 e Å3
0 restraintsΔρmin = 0.55 e Å3
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Zn10.00000.00000.50000.00638 (7)
Zn20.50000.50000.50000.00713 (7)
Cl10.22344 (6)0.29474 (5)0.14566 (3)0.01257 (10)
Cl20.09432 (5)0.08857 (5)0.17308 (4)0.01326 (10)
P10.27170 (5)0.02472 (5)0.29328 (4)0.00646 (9)
P20.07031 (5)0.31775 (5)0.36883 (4)0.00604 (9)
O10.23584 (16)0.10062 (14)0.61639 (10)0.0105 (2)
H1A0.31430.16940.59540.016*
H1B0.30590.03100.64280.016*
O20.42027 (16)0.54770 (15)0.66143 (10)0.0124 (2)
H2A0.46540.63930.69250.019*
H2B0.30680.55430.66540.019*
O30.44804 (16)0.73934 (14)0.46542 (10)0.0107 (2)
H3A0.47350.79230.53060.016*
H3B0.34600.77110.43660.016*
O110.18094 (15)0.05491 (14)0.38166 (10)0.0087 (2)
O120.46117 (15)0.10352 (14)0.32546 (10)0.0099 (2)
O130.26226 (16)0.10522 (14)0.18802 (10)0.0110 (2)
O210.04362 (15)0.21876 (14)0.43605 (10)0.0089 (2)
O220.24730 (15)0.39779 (14)0.42584 (10)0.0109 (2)
O230.05887 (15)0.44211 (14)0.31134 (10)0.0092 (2)
C10.1186 (2)0.1816 (2)0.24513 (14)0.0083 (3)
C110.3917 (3)0.1075 (2)0.10608 (16)0.0173 (4)
H11A0.51620.07070.14470.021*
H11B0.35580.03500.04600.021*
C120.38922 (18)0.27862 (18)0.05419 (18)0.0266 (5)
H12A0.42630.34890.11440.040*
H12B0.47460.28450.00240.040*
H12C0.26520.31390.01680.040*
C210.00929 (18)0.59655 (16)0.27487 (14)0.0104 (3)
H21A0.14090.59380.26680.013*
H21B0.00510.68610.33240.013*
C220.1006 (3)0.6211 (2)0.16188 (17)0.0198 (4)
H22A0.07950.53550.10440.030*
H22B0.06280.72610.13780.030*
H22C0.23120.61780.16990.030*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.00633 (13)0.00514 (13)0.00806 (14)0.00079 (9)0.00179 (10)0.00144 (10)
Zn20.00586 (13)0.00604 (14)0.00934 (14)0.00026 (9)0.00042 (10)0.00129 (10)
Cl10.0164 (2)0.0117 (2)0.0115 (2)0.00187 (16)0.00599 (16)0.00528 (16)
Cl20.01001 (19)0.0145 (2)0.0132 (2)0.00136 (15)0.00428 (15)0.00019 (16)
P10.0066 (2)0.0055 (2)0.0073 (2)0.00062 (15)0.00103 (15)0.00043 (15)
P20.00503 (19)0.0050 (2)0.0083 (2)0.00087 (15)0.00063 (15)0.00145 (16)
O10.0086 (6)0.0090 (6)0.0136 (6)0.0001 (4)0.0003 (5)0.0024 (5)
O20.0069 (6)0.0166 (6)0.0135 (6)0.0003 (5)0.0026 (5)0.0011 (5)
O30.0094 (6)0.0089 (6)0.0131 (6)0.0024 (4)0.0017 (5)0.0002 (5)
O110.0098 (6)0.0076 (6)0.0101 (6)0.0029 (4)0.0034 (5)0.0032 (5)
O120.0082 (6)0.0089 (6)0.0122 (6)0.0005 (4)0.0005 (5)0.0002 (5)
O130.0113 (6)0.0097 (6)0.0118 (6)0.0011 (5)0.0052 (5)0.0040 (5)
O210.0096 (6)0.0072 (6)0.0107 (6)0.0014 (4)0.0030 (5)0.0030 (5)
O220.0066 (5)0.0109 (6)0.0141 (6)0.0000 (4)0.0010 (5)0.0009 (5)
O230.0067 (5)0.0065 (6)0.0151 (6)0.0011 (4)0.0015 (5)0.0049 (5)
C10.0066 (7)0.0090 (8)0.0092 (8)0.0018 (6)0.0000 (6)0.0034 (6)
C110.0185 (9)0.0209 (10)0.0134 (9)0.0017 (7)0.0095 (7)0.0038 (8)
C120.0302 (11)0.0226 (11)0.0283 (11)0.0049 (9)0.0145 (9)0.0095 (9)
C210.0120 (8)0.0039 (8)0.0156 (9)0.0015 (6)0.0018 (7)0.0039 (7)
C220.0214 (10)0.0151 (10)0.0220 (10)0.0019 (7)0.0044 (8)0.0104 (8)
Geometric parameters (Å, º) top
Zn1—O21i2.0568 (11)P2—C11.8655 (17)
Zn1—O212.0568 (11)O1—H1A0.8657
Zn1—O112.1043 (11)O1—H1B0.8500
Zn1—O11i2.1043 (11)O2—H2A0.8500
Zn1—O12.1535 (12)O2—H2B0.8500
Zn1—O1i2.1535 (12)O3—H3A0.8500
Zn2—O22ii2.0580 (12)O3—H3B0.8500
Zn2—O222.0580 (12)O13—C111.451 (2)
Zn2—O2ii2.0902 (12)O23—C211.4744 (18)
Zn2—O22.0902 (12)C11—C121.505 (2)
Zn2—O3ii2.1154 (12)C11—H11A0.9900
Zn2—O32.1154 (12)C11—H11B0.9900
Cl1—C11.7947 (16)C12—H12A0.9800
Cl2—C11.7874 (17)C12—H12B0.9800
P1—O111.4959 (12)C12—H12C0.9800
P1—O121.4982 (12)C21—C221.505 (2)
P1—O131.5757 (12)C21—H21A0.9900
P1—C11.8517 (16)C21—H21B0.9900
P2—O221.4829 (12)C22—H22A0.9800
P2—O211.4937 (12)C22—H22B0.9800
P2—O231.5813 (11)C22—H22C0.9800
O21i—Zn1—O21180.0Zn1—O1—H1B114.2
O21i—Zn1—O1188.76 (4)H1A—O1—H1B101.2
O21—Zn1—O1191.24 (4)Zn2—O2—H2A111.2
O21i—Zn1—O11i91.24 (4)Zn2—O2—H2B118.0
O21—Zn1—O11i88.76 (4)H2A—O2—H2B101.9
O11—Zn1—O11i180.0Zn2—O3—H3A103.6
O21i—Zn1—O187.99 (4)Zn2—O3—H3B125.9
O21—Zn1—O192.01 (4)H3A—O3—H3B105.2
O11—Zn1—O187.27 (4)P1—O11—Zn1139.05 (7)
O11i—Zn1—O192.73 (4)C11—O13—P1124.27 (11)
O21i—Zn1—O1i92.01 (4)P2—O21—Zn1130.29 (7)
O21—Zn1—O1i87.99 (4)P2—O22—Zn2176.93 (8)
O11—Zn1—O1i92.73 (4)C21—O23—P2123.55 (9)
O11i—Zn1—O1i87.27 (4)Cl2—C1—Cl1108.03 (9)
O1—Zn1—O1i180.00 (4)Cl2—C1—P1109.76 (9)
O22ii—Zn2—O22180.00 (4)Cl1—C1—P1109.05 (8)
O22ii—Zn2—O2ii94.51 (5)Cl2—C1—P2108.30 (8)
O22—Zn2—O2ii85.49 (5)Cl1—C1—P2110.57 (9)
O22ii—Zn2—O285.49 (5)P1—C1—P2111.08 (8)
O22—Zn2—O294.51 (5)O13—C11—C12107.23 (15)
O2ii—Zn2—O2180.0O13—C11—H11A110.3
O22ii—Zn2—O3ii96.16 (5)C12—C11—H11A110.3
O22—Zn2—O3ii83.84 (5)O13—C11—H11B110.3
O2ii—Zn2—O3ii88.96 (5)C12—C11—H11B110.3
O2—Zn2—O3ii91.04 (5)H11A—C11—H11B108.5
O22ii—Zn2—O383.84 (5)C11—C12—H12A109.5
O22—Zn2—O396.16 (5)C11—C12—H12B109.5
O2ii—Zn2—O391.04 (5)H12A—C12—H12B109.5
O2—Zn2—O388.96 (5)C11—C12—H12C109.5
O3ii—Zn2—O3180.0H12A—C12—H12C109.5
O11—P1—O12119.22 (7)H12B—C12—H12C109.5
O11—P1—O13106.30 (7)O23—C21—C22107.80 (12)
O12—P1—O13111.32 (6)O23—C21—H21A110.1
O11—P1—C1105.42 (7)C22—C21—H21A110.1
O12—P1—C1107.72 (7)O23—C21—H21B110.1
O13—P1—C1105.99 (7)C22—C21—H21B110.1
O22—P2—O21119.18 (7)H21A—C21—H21B108.5
O22—P2—O23111.73 (7)C21—C22—H22A109.5
O21—P2—O23106.72 (6)C21—C22—H22B109.5
O22—P2—C1107.78 (7)H22A—C22—H22B109.5
O21—P2—C1106.61 (7)C21—C22—H22C109.5
O23—P2—C1103.63 (7)H22A—C22—H22C109.5
Zn1—O1—H1A121.2H22B—C22—H22C109.5
Symmetry codes: (i) x, y, z+1; (ii) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1B···O12iii0.852.112.9293 (16)161
O1—H1A···O3ii0.872.112.9377 (17)160
O2—H2A···Cl1ii0.852.793.3723 (13)128
O2—H2A···O12ii0.852.222.9749 (17)149
O2—H2B···O23iv0.851.892.7348 (16)174
O3—H3B···O11v0.852.042.8194 (16)153
O3—H3A···O12ii0.851.842.6895 (17)176
Symmetry codes: (ii) x+1, y+1, z+1; (iii) x+1, y, z+1; (iv) x, y+1, z+1; (v) x, y+1, z.
 

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