Literature DB >> 21200612

Decaaqua-dioxidobis[μ(3)-N-(phospho-n-atometh-yl)imino-diacetato]-dizinc(II)-divanadium(IV) dihydrate.

Luís Cunha-Silva, Fa-Nian Shi, Jacek Klinowski, Tito Trindade, João Rocha, Filipe A Almeida Paz.   

Abstract

The title compound, [Zn(2)V(2)(C(5)H(6)NO(7)P)(2)O(2)(H(2)O)(10)]·2H(2)O, contains a [V(2)O(2)(pmida)(2)](4-) dimeric anionic unit [where H(4)pmida is N-(phosphono-meth-yl)imino-diacetic acid] lying on a centre of symmetry which is exo-coordinated via the two deprotonated phospho-nate groups to two Zn(2+) cations, with the coordination environment of Zn completed by five water mol-ecules. The crystal packing is mediated by an extensive network of strong and highly directional O-H⋯O hydrogen bonds involving the water mol-ecules (coordinated and uncoordinated) and the functional groups of pmida(4-), leading to a three-dimensional supra-molecular network.

Entities:  

Year:  2007        PMID: 21200612      PMCID: PMC2914926          DOI: 10.1107/S1600536807062253

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


Related literature

For related literature, see: Cunha-Silva, Mafra et al. (2007 ▶); Cunha-Silva, Shi et al. (2007 ▶); Shi et al. (2007 ▶); Mafra et al. (2006 ▶); Shi, Paz, Girginova, Amaral et al. (2006 ▶); Shi, Paz, Girginova, Rocha et al. (2006 ▶); Shi, Almeida Paz, Trindade & Rocha (2006 ▶); Paz, Rocha, Klinowski et al. (2005 ▶); Almeida Paz, Shi, Mafra et al. (2005 ▶); Almeida Paz, Shi, Trindade et al. (2005 ▶); Shi et al. (2005 ▶); Paz et al. (2004 ▶).

Experimental

Crystal data

[Zn2V2(C5H6NO7P)2O2(H2O)10]·2H2O M = 926.97 Monoclinic, a = 10.0161 (5) Å b = 14.8811 (7) Å c = 10.8298 (5) Å β = 111.147 (2)° V = 1505.48 (12) Å3 Z = 2 Mo Kα radiation μ = 2.40 mm−1 T = 293 (2) K 0.22 × 0.14 × 0.10 mm

Data collection

Bruker Kappa APEXII diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1998 ▶) T min = 0.621, T max = 0.796 95509 measured reflections 4040 independent reflections 3765 reflections with I > 2σ(I) R int = 0.028

Refinement

R[F 2 > 2σ(F 2)] = 0.027 wR(F 2) = 0.077 S = 1.04 4040 reflections 238 parameters 15 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 1.06 e Å−3 Δρmin = −0.87 e Å−3 Data collection: APEX2 (Bruker, 2006 ▶); cell refinement: APEX2; data reduction: SAINT (Bruker, 2005 ▶); program(s) used to solve structure: SHELXTL (Bruker 2001 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Brandenburg, 2006 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807062253/bg2149sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536807062253/bg2149Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Zn2V2(C5H6NO7P)2O2(H2O)10]·2H2OF000 = 940
Mr = 926.97Dx = 2.045 Mg m3
Monoclinic, P21/cMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 9009 reflections
a = 10.0161 (5) Åθ = 2.6–37.6º
b = 14.8811 (7) ŵ = 2.40 mm1
c = 10.8298 (5) ÅT = 293 (2) K
β = 111.147 (2)ºPrism, blue
V = 1505.48 (12) Å30.22 × 0.14 × 0.10 mm
Z = 2
Bruker X8 APEXII Kappa CCD diffractometer4040 independent reflections
Radiation source: fine-focus sealed tube3765 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.028
T = 293(2) Kθmax = 29.1º
Thin–slice ω and φ scansθmin = 3.6º
Absorption correction: multi-scan(SADABS; Sheldrick, 1998)h = −13→13
Tmin = 0.621, Tmax = 0.796k = −20→20
95509 measured reflectionsl = −14→14
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.077  w = 1/[σ2(Fo2) + (0.038P)2 + 2.056P] where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.002
4040 reflectionsΔρmax = 1.06 e Å3
238 parametersΔρmin = −0.87 e Å3
15 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods
Experimental. See dedicated section in the main paper
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
Zn10.47946 (2)0.566124 (16)0.26276 (2)0.02202 (7)
V11.01192 (3)0.52639 (2)0.74230 (3)0.01679 (8)
P10.81721 (5)0.55866 (3)0.44467 (5)0.01775 (10)
N10.98913 (17)0.66771 (11)0.63798 (15)0.0188 (3)
O50.85567 (14)0.49988 (10)0.57024 (13)0.0223 (3)
O70.66854 (14)0.59666 (10)0.40459 (14)0.0242 (3)
O41.16206 (16)0.60558 (10)0.87361 (13)0.0252 (3)
C50.9481 (2)0.65025 (13)0.49415 (17)0.0199 (3)
H5A1.03230.63400.47470.024*
H5B0.90720.70410.44460.024*
O60.83989 (15)0.50552 (10)0.33263 (14)0.0249 (3)
O20.86146 (16)0.59104 (10)0.79428 (16)0.0275 (3)
C41.1990 (2)0.68247 (13)0.84317 (19)0.0229 (4)
C10.8075 (2)0.66657 (14)0.7474 (2)0.0239 (4)
O81.0159 (2)0.43890 (11)0.83081 (18)0.0348 (4)
C31.1313 (2)0.71027 (15)0.69835 (19)0.0263 (4)
H3A1.12130.77510.69220.032*
H3B1.19240.69200.65090.032*
C20.8762 (2)0.71885 (14)0.6657 (2)0.0266 (4)
H2A0.80270.73590.58240.032*
H2B0.91760.77360.71250.032*
O31.28796 (19)0.73187 (12)0.92367 (16)0.0371 (4)
O10.70218 (18)0.69941 (11)0.76509 (19)0.0360 (4)
O1W0.5041 (2)0.43314 (11)0.32805 (19)0.0392 (4)
H1W0.440 (3)0.390 (2)0.288 (3)0.059*
H2W0.528 (4)0.419 (2)0.414 (2)0.059*
O2W0.36824 (16)0.59655 (11)0.39610 (15)0.0266 (3)
H3W0.348 (3)0.6535 (14)0.402 (3)0.040*
H4W0.298 (3)0.5638 (17)0.401 (3)0.040*
O3W0.28954 (18)0.52927 (14)0.11685 (17)0.0409 (4)
H5W0.238 (4)0.560 (2)0.045 (3)0.061*
H6W0.234 (4)0.491 (2)0.136 (3)0.061*
O4W0.45023 (17)0.69926 (11)0.19464 (16)0.0304 (3)
H7W0.397 (3)0.706 (2)0.113 (2)0.046*
H8W0.531 (3)0.727 (2)0.205 (3)0.046*
O5W0.58091 (19)0.53840 (17)0.12317 (18)0.0446 (5)
H9W0.666 (3)0.513 (2)0.170 (3)0.067*
H10W0.598 (4)0.574 (2)0.068 (3)0.067*
O6W0.5884 (6)0.6734 (4)−0.0345 (5)0.1474 (18)
U11U22U33U12U13U23
Zn10.01727 (12)0.02490 (13)0.01985 (12)−0.00060 (8)0.00183 (8)0.00210 (8)
V10.01574 (14)0.01789 (15)0.01586 (14)0.00001 (10)0.00464 (11)0.00076 (10)
P10.01270 (19)0.0220 (2)0.0165 (2)−0.00024 (16)0.00279 (16)−0.00184 (16)
N10.0182 (7)0.0201 (7)0.0165 (7)−0.0029 (6)0.0045 (5)−0.0002 (5)
O50.0185 (6)0.0238 (6)0.0206 (6)−0.0037 (5)0.0023 (5)0.0009 (5)
O70.0142 (6)0.0304 (7)0.0239 (6)0.0025 (5)0.0018 (5)−0.0048 (6)
O40.0279 (7)0.0252 (7)0.0171 (6)−0.0049 (6)0.0017 (5)0.0016 (5)
C50.0195 (8)0.0232 (8)0.0152 (7)−0.0024 (7)0.0041 (6)0.0014 (6)
O60.0177 (6)0.0331 (7)0.0233 (6)−0.0002 (5)0.0067 (5)−0.0079 (6)
O20.0287 (7)0.0247 (7)0.0357 (8)0.0029 (6)0.0196 (6)0.0039 (6)
C40.0210 (8)0.0251 (9)0.0190 (8)−0.0035 (7)0.0026 (7)0.0003 (7)
C10.0227 (9)0.0225 (9)0.0270 (9)−0.0022 (7)0.0094 (7)−0.0053 (7)
O80.0410 (9)0.0272 (8)0.0383 (9)0.0017 (7)0.0169 (7)0.0086 (7)
C30.0248 (9)0.0288 (10)0.0202 (8)−0.0110 (8)0.0021 (7)0.0036 (7)
C20.0337 (10)0.0189 (8)0.0299 (10)0.0036 (8)0.0148 (8)0.0009 (7)
O30.0405 (9)0.0334 (8)0.0242 (7)−0.0151 (7)−0.0043 (7)0.0007 (6)
O10.0305 (8)0.0297 (8)0.0538 (10)0.0047 (6)0.0226 (8)−0.0033 (7)
O1W0.0428 (10)0.0270 (8)0.0340 (9)−0.0057 (7)−0.0029 (7)0.0044 (7)
O2W0.0235 (7)0.0261 (7)0.0316 (7)−0.0003 (6)0.0117 (6)0.0027 (6)
O3W0.0269 (8)0.0578 (12)0.0266 (8)−0.0179 (8)−0.0040 (6)0.0167 (8)
O4W0.0274 (7)0.0287 (8)0.0303 (8)−0.0041 (6)0.0046 (6)0.0066 (6)
O5W0.0281 (8)0.0761 (14)0.0268 (8)0.0078 (9)0.0064 (7)−0.0058 (9)
O6W0.163 (4)0.159 (5)0.143 (4)−0.009 (4)0.083 (4)0.009 (3)
Zn1—O72.0133 (14)C5—H5B0.9700
Zn1—O3W2.0609 (16)O6—V1i1.9890 (14)
Zn1—O1W2.0860 (17)O2—C11.271 (3)
Zn1—O4W2.0974 (16)C4—O31.238 (2)
Zn1—O5W2.1440 (18)C4—C31.524 (3)
Zn1—O2W2.1660 (15)C1—O11.239 (3)
V1—O81.6086 (16)C1—C21.517 (3)
V1—O6i1.9890 (14)C3—H3A0.9700
V1—O51.9932 (14)C3—H3B0.9700
V1—O22.0312 (15)C2—H2A0.9700
V1—O42.0321 (14)C2—H2B0.9700
V1—N12.3590 (16)O1W—H1W0.90 (2)
P1—O71.5030 (14)O1W—H2W0.90 (2)
P1—O61.5324 (15)O2W—H3W0.88 (2)
P1—O51.5443 (14)O2W—H4W0.87 (2)
P1—C51.8323 (19)O3W—H5W0.89 (2)
N1—C31.478 (2)O3W—H6W0.88 (2)
N1—C21.481 (3)O4W—H7W0.86 (2)
N1—C51.484 (2)O4W—H8W0.88 (2)
O4—C41.282 (2)O5W—H9W0.90 (2)
C5—H5A0.9700O5W—H10W0.86 (2)
O7—Zn1—O3W177.43 (8)P1—O7—Zn1134.17 (9)
O7—Zn1—O1W89.53 (7)C4—O4—V1123.17 (12)
O3W—Zn1—O1W88.34 (7)N1—C5—P1109.58 (12)
O7—Zn1—O4W91.64 (6)N1—C5—H5A109.8
O3W—Zn1—O4W90.49 (7)P1—C5—H5A109.8
O1W—Zn1—O4W178.81 (7)N1—C5—H5B109.8
O7—Zn1—O5W91.53 (6)P1—C5—H5B109.8
O3W—Zn1—O5W87.09 (8)H5A—C5—H5B108.2
O1W—Zn1—O5W91.61 (9)P1—O6—V1i142.36 (9)
O4W—Zn1—O5W88.58 (8)C1—O2—V1123.99 (13)
O7—Zn1—O2W90.73 (6)O3—C4—O4123.37 (18)
O3W—Zn1—O2W90.71 (7)O3—C4—C3120.23 (18)
O1W—Zn1—O2W89.93 (7)O4—C4—C3116.37 (16)
O4W—Zn1—O2W89.83 (6)O1—C1—O2123.4 (2)
O5W—Zn1—O2W177.27 (7)O1—C1—C2118.61 (19)
O8—V1—O6i100.84 (8)O2—C1—C2118.02 (17)
O8—V1—O5103.84 (8)N1—C3—C4109.82 (15)
O6i—V1—O591.21 (6)N1—C3—H3A109.7
O8—V1—O294.57 (8)C4—C3—H3A109.7
O6i—V1—O2164.50 (7)N1—C3—H3B109.7
O5—V1—O286.67 (6)C4—C3—H3B109.7
O8—V1—O4101.49 (8)H3A—C3—H3B108.2
O6i—V1—O487.20 (6)N1—C2—C1113.27 (16)
O5—V1—O4154.45 (6)N1—C2—H2A108.9
O2—V1—O488.12 (6)C1—C2—H2A108.9
O8—V1—N1169.79 (8)N1—C2—H2B108.9
O6i—V1—N188.57 (6)C1—C2—H2B108.9
O5—V1—N179.69 (6)H2A—C2—H2B107.7
O2—V1—N175.95 (6)Zn1—O1W—H1W122 (2)
O4—V1—N174.78 (6)Zn1—O1W—H2W121 (2)
O7—P1—O6112.33 (8)H1W—O1W—H2W103 (3)
O7—P1—O5111.96 (8)Zn1—O2W—H3W115.9 (19)
O6—P1—O5110.11 (9)Zn1—O2W—H4W123 (2)
O7—P1—C5109.55 (9)H3W—O2W—H4W109 (2)
O6—P1—C5108.69 (8)Zn1—O3W—H5W128 (2)
O5—P1—C5103.82 (8)Zn1—O3W—H6W119 (2)
C3—N1—C2111.98 (16)H5W—O3W—H6W109 (3)
C3—N1—C5113.40 (15)Zn1—O4W—H7W115 (2)
C2—N1—C5111.14 (15)Zn1—O4W—H8W113 (2)
C3—N1—V1105.00 (11)H7W—O4W—H8W106 (3)
C2—N1—V1108.06 (11)Zn1—O5W—H9W106 (2)
C5—N1—V1106.80 (11)Zn1—O5W—H10W130 (3)
P1—O5—V1124.99 (8)H9W—O5W—H10W105 (3)
O8—V1—N1—C395.2 (5)O5—V1—O4—C4−10.3 (3)
O6i—V1—N1—C3−62.07 (12)O2—V1—O4—C4−88.53 (16)
O5—V1—N1—C3−153.56 (13)N1—V1—O4—C4−12.59 (15)
O2—V1—N1—C3117.32 (13)C3—N1—C5—P1155.80 (14)
O4—V1—N1—C325.42 (12)C2—N1—C5—P1−77.01 (17)
O8—V1—N1—C2−24.5 (5)V1—N1—C5—P140.64 (13)
O6i—V1—N1—C2178.27 (13)O7—P1—C5—N189.70 (14)
O5—V1—N1—C286.78 (13)O6—P1—C5—N1−147.23 (12)
O2—V1—N1—C2−2.35 (12)O5—P1—C5—N1−30.04 (15)
O4—V1—N1—C2−94.24 (13)O7—P1—O6—V1i147.90 (15)
O8—V1—N1—C5−144.1 (4)O5—P1—O6—V1i−86.60 (17)
O6i—V1—N1—C558.62 (11)C5—P1—O6—V1i26.51 (19)
O5—V1—N1—C5−32.88 (11)O8—V1—O2—C1−176.55 (17)
O2—V1—N1—C5−122.00 (12)O6i—V1—O2—C19.6 (4)
O4—V1—N1—C5146.11 (12)O5—V1—O2—C1−72.91 (17)
O7—P1—O5—V1−116.85 (10)O4—V1—O2—C182.07 (17)
O6—P1—O5—V1117.44 (10)N1—V1—O2—C17.29 (16)
C5—P1—O5—V11.24 (12)V1—O4—C4—O3178.20 (17)
O8—V1—O5—P1−173.68 (11)V1—O4—C4—C3−4.0 (3)
O6i—V1—O5—P1−72.20 (11)V1—O2—C1—O1169.44 (16)
O2—V1—O5—P192.43 (11)V1—O2—C1—C2−10.6 (3)
O4—V1—O5—P113.8 (2)C2—N1—C3—C483.0 (2)
N1—V1—O5—P116.12 (10)C5—N1—C3—C4−150.29 (17)
O6—P1—O7—Zn121.40 (16)V1—N1—C3—C4−34.07 (19)
O5—P1—O7—Zn1−103.09 (13)O3—C4—C3—N1−153.7 (2)
C5—P1—O7—Zn1142.29 (12)O4—C4—C3—N128.5 (3)
O1W—Zn1—O7—P152.88 (14)C3—N1—C2—C1−116.61 (19)
O4W—Zn1—O7—P1−127.34 (14)C5—N1—C2—C1115.43 (18)
O5W—Zn1—O7—P1−38.72 (15)V1—N1—C2—C1−1.4 (2)
O2W—Zn1—O7—P1142.81 (13)O1—C1—C2—N1−172.84 (19)
O8—V1—O4—C4177.18 (16)O2—C1—C2—N17.2 (3)
O6i—V1—O4—C476.69 (16)
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O1ii0.90 (2)1.88 (2)2.770 (2)169 (3)
O1W—H2W···O2Wii0.90 (2)1.95 (2)2.828 (2)164 (3)
O2W—H3W···O3iii0.88 (2)1.85 (2)2.725 (2)172 (3)
O2W—H4W···O5ii0.87 (2)1.93 (2)2.795 (2)173 (3)
O3W—H6W···O2ii0.88 (2)1.87 (2)2.733 (2)171 (3)
O3W—H5W···O4iv0.89 (2)1.86 (2)2.726 (2)164 (4)
O4W—H7W···O3iv0.86 (2)1.98 (2)2.837 (2)174 (3)
O4W—H8W···O1v0.88 (2)1.94 (2)2.799 (2)167 (3)
O5W—H9W···O60.90 (2)1.98 (3)2.805 (2)150 (4)
O5W—H10W···O6W0.86 (2)1.84 (3)2.656 (6)159 (4)
Table 1

Selected bond lengths (Å)

Zn1—O72.0133 (14)
Zn1—O3W2.0609 (16)
Zn1—O1W2.0860 (17)
Zn1—O4W2.0974 (16)
Zn1—O5W2.1440 (18)
Zn1—O2W2.1660 (15)
V1—O81.6086 (16)
V1—O6i1.9890 (14)
V1—O51.9932 (14)
V1—O22.0312 (15)
V1—O42.0321 (14)
V1—N12.3590 (16)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
O1W—H1W⋯O1ii0.90 (2)1.88 (2)2.770 (2)169 (3)
O1W—H2W⋯O2Wii0.90 (2)1.95 (2)2.828 (2)164 (3)
O2W—H3W⋯O3iii0.88 (2)1.85 (2)2.725 (2)172 (3)
O2W—H4W⋯O5ii0.87 (2)1.93 (2)2.795 (2)173 (3)
O3W—H6W⋯O2ii0.88 (2)1.87 (2)2.733 (2)171 (3)
O3W—H5W⋯O4iv0.89 (2)1.86 (2)2.726 (2)164 (4)
O4W—H7W⋯O3iv0.86 (2)1.98 (2)2.837 (2)174 (3)
O4W—H8W⋯O1v0.88 (2)1.94 (2)2.799 (2)167 (3)
O5W—H9W⋯O60.90 (2)1.98 (3)2.805 (2)150 (4)
O5W—H10W⋯O6W0.86 (2)1.84 (3)2.656 (6)159 (4)

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

  1 in total

1.  X-ray diffraction and solid-state NMR studies of a germanium binuclear complex.

Authors:  Luís Mafra; Filipe A Almeida Paz; Fa-Nian Shi; João Rocha; Tito Trindade; Christian Fernandez; Anna Makal; Krzysztof Wozniak; Jacek Klinowski
Journal:  Chemistry       Date:  2005-12-23       Impact factor: 5.236

  1 in total

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