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The title compound contains HPO3 pseudo-pyramids [dav(P—O) = 1.516 (2) Å], ZnO4 tetrahedra [dav(Zn—O) = 1.939 (2) Å], and trans-ZnO2(H2O)4 octahedra. These building units link together by way of Zn—O—P bridges [θav = 128.1°], resulting in a layered structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802008243/mg6009sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802008243/mg6009Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](P-O) = 0.002 Å
  • R factor = 0.026
  • wR factor = 0.074
  • Data-to-parameter ratio = 26.5

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
ABSTM_02 Alert C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.232 0.547 Tmin and Tmax expected: 0.183 0.503 RR = 1.167 Please check that your absorption correction is appropriate. PLAT_420 Alert C D-H Without Acceptor P(2) - H(2) ? PLAT_420 Alert C D-H Without Acceptor P(3) - H(3) ? General Notes
FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: H11 N1 O11 P3 Zn2.5 Atom count from _chemical_formula_moiety:H88 N20 O4 ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.919 Tmax scaled 0.503 Tmin scaled 0.213
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
3 Alert Level C = Please check

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SMART; data reduction: SMART; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

(I) top
Crystal data top
(NH4)2Zn5(HPO3)6·4H2OF(000) = 452
Mr = 457.43Dx = 2.469 Mg m3
Triclinic, P1Melting point: decomposes before melting K
a = 7.2263 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 9.7728 (4) ÅCell parameters from 3972 reflections
c = 10.2349 (5) Åθ = 2.5–32.4°
α = 63.409 (1)°µ = 5.29 mm1
β = 87.162 (1)°T = 293 K
γ = 72.969 (1)°Chunky plate, colourless
V = 615.18 (5) Å30.39 × 0.28 × 0.13 mm
Z = 2
Data collection top
Bruker SMART 1000 CCD
diffractometer
4274 independent reflections
Radiation source: fine-focus sealed tube3646 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.013
ω scansθmax = 32.5°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Bruker, 1999)
h = 109
Tmin = 0.232, Tmax = 0.547k = 1314
6425 measured reflectionsl = 1515
Refinement top
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-atom parameters constrained
wR(F2) = 0.074 w = 1/[σ2(Fo2) + (0.0457P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.001
4274 reflectionsΔρmax = 0.74 e Å3
161 parametersΔρmin = 0.64 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0101 (10)
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
N10.2216 (3)0.0432 (3)0.1527 (2)0.0323 (4)
H40.09010.06260.18320.039*
H50.31530.03890.19830.039*
H60.26530.05980.09470.039*
H70.23410.08880.08980.039*
Zn10.33591 (3)0.70373 (3)0.33542 (2)0.02207 (7)
Zn20.36418 (3)0.35646 (3)0.01856 (2)0.02207 (7)
Zn30.50000.00000.50000.02457 (8)
P10.76267 (7)0.49691 (6)0.34845 (5)0.02117 (10)
H10.93570.49530.38610.025*
P20.23711 (8)0.59235 (7)0.11813 (6)0.02365 (11)
H20.05740.65450.05500.028*
P30.24927 (7)0.06249 (6)0.20335 (5)0.01984 (10)
H30.10400.15870.23430.024*
O10.6177 (2)0.65059 (19)0.3397 (2)0.0319 (3)
O20.7265 (3)0.34607 (19)0.46569 (17)0.0351 (4)
O30.7754 (3)0.4894 (2)0.20445 (17)0.0364 (4)
O40.3106 (3)0.42325 (19)0.13484 (17)0.0324 (3)
O50.3533 (2)0.7013 (2)0.01944 (19)0.0323 (3)
O60.2266 (3)0.5857 (2)0.2685 (2)0.0414 (4)
O70.2957 (2)0.15858 (18)0.04834 (15)0.0265 (3)
O80.1819 (2)0.07397 (18)0.21001 (17)0.0274 (3)
O90.4199 (3)0.0023 (2)0.31444 (18)0.0340 (4)
O100.2921 (3)0.2245 (2)0.4567 (2)0.0510 (5)
H80.32680.27500.48480.061*
H90.27970.30580.35760.061*
O110.6953 (4)0.1300 (3)0.3727 (3)0.0661 (7)
H100.74170.18370.39450.079*
H110.61290.22080.26710.079*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0287 (9)0.0375 (11)0.0332 (10)0.0132 (8)0.0030 (7)0.0161 (9)
Zn10.02774 (13)0.01781 (11)0.01966 (11)0.00815 (9)0.00385 (9)0.00705 (9)
Zn20.02897 (13)0.01842 (12)0.01929 (11)0.01069 (9)0.00455 (9)0.00702 (9)
Zn30.03317 (19)0.02149 (16)0.02000 (15)0.00807 (13)0.00420 (13)0.00968 (13)
P10.0217 (2)0.0181 (2)0.0202 (2)0.00656 (18)0.00270 (17)0.00547 (18)
P20.0237 (2)0.0237 (2)0.0278 (2)0.0112 (2)0.00540 (19)0.0131 (2)
P30.0243 (2)0.0155 (2)0.0177 (2)0.00576 (17)0.00058 (17)0.00565 (17)
O10.0296 (8)0.0216 (7)0.0431 (9)0.0055 (6)0.0028 (7)0.0147 (7)
O20.0637 (12)0.0225 (8)0.0216 (7)0.0202 (8)0.0127 (7)0.0087 (6)
O30.0484 (10)0.0284 (8)0.0192 (7)0.0023 (7)0.0044 (7)0.0056 (6)
O40.0533 (10)0.0239 (8)0.0237 (7)0.0148 (7)0.0073 (7)0.0124 (6)
O50.0310 (8)0.0238 (8)0.0386 (9)0.0124 (6)0.0093 (7)0.0094 (7)
O60.0604 (12)0.0510 (11)0.0409 (9)0.0385 (10)0.0248 (9)0.0334 (9)
O70.0409 (9)0.0217 (7)0.0202 (6)0.0175 (6)0.0033 (6)0.0074 (6)
O80.0273 (7)0.0191 (7)0.0307 (7)0.0104 (6)0.0039 (6)0.0043 (6)
O90.0418 (9)0.0332 (9)0.0267 (7)0.0054 (7)0.0110 (7)0.0156 (7)
O100.0651 (13)0.0243 (9)0.0544 (12)0.0010 (9)0.0233 (10)0.0161 (9)
O110.111 (2)0.0719 (16)0.0597 (14)0.0694 (16)0.0384 (14)0.0449 (13)
Geometric parameters (Å, º) top
N1—H40.9525Zn3—O112.166 (2)
N1—H50.8048P1—O31.5050 (17)
N1—H60.8733P1—O21.5140 (16)
N1—H70.9526P1—O11.5260 (17)
Zn1—O61.9283 (16)P1—H11.3200
Zn1—O2i1.9325 (15)P2—O61.5104 (18)
Zn1—O11.9462 (17)P2—O41.5114 (16)
Zn1—O8ii1.9583 (15)P2—O51.5281 (16)
Zn2—O3iii1.9079 (16)P2—H21.3200
Zn2—O41.9365 (15)P3—O91.5079 (16)
Zn2—O71.9480 (14)P3—O71.5197 (15)
Zn2—O5iii1.9529 (17)P3—O81.5219 (15)
Zn3—O9iv2.0014 (14)P3—H31.3200
Zn3—O92.0014 (14)O10—H80.7717
Zn3—O102.1290 (19)O10—H90.9566
Zn3—O10iv2.1290 (19)O11—H100.8084
Zn3—O11iv2.166 (2)O11—H111.0981
H4—N1—H5128.6O3—P1—O2109.52 (10)
H4—N1—H6105.4O3—P1—O1113.71 (10)
H5—N1—H691.0O2—P1—O1113.08 (10)
H4—N1—H7113.4O3—P1—H1106.7
H5—N1—H7109.5O2—P1—H1106.7
H6—N1—H7102.7O1—P1—H1106.7
O6—Zn1—O2i108.41 (7)O6—P2—O4109.10 (10)
O6—Zn1—O1114.27 (8)O6—P2—O5112.87 (10)
O2i—Zn1—O1106.63 (8)O4—P2—O5113.41 (10)
O6—Zn1—O8ii102.07 (8)O6—P2—H2107.0
O2i—Zn1—O8ii107.23 (7)O4—P2—H2107.0
O1—Zn1—O8ii117.79 (7)O5—P2—H2107.0
O3iii—Zn2—O4114.23 (7)O9—P3—O7111.59 (10)
O3iii—Zn2—O7109.52 (7)O9—P3—O8111.91 (9)
O4—Zn2—O7106.65 (6)O7—P3—O8109.55 (8)
O3iii—Zn2—O5iii114.45 (8)O9—P3—H3107.9
O4—Zn2—O5iii104.69 (7)O7—P3—H3107.9
O7—Zn2—O5iii106.73 (7)O8—P3—H3107.9
O9iv—Zn3—O9180.0P1—O1—Zn1127.86 (10)
O9iv—Zn3—O1085.46 (7)P1—O2—Zn1i129.28 (10)
O9—Zn3—O1094.54 (7)P1—O3—Zn2iii128.74 (11)
O9iv—Zn3—O10iv94.54 (7)P2—O4—Zn2127.96 (10)
O9—Zn3—O10iv85.46 (7)P2—O5—Zn2iii126.35 (10)
O10—Zn3—O10iv180.0P2—O6—Zn1125.97 (10)
O9iv—Zn3—O11iv86.14 (8)P3—O7—Zn2124.65 (8)
O9—Zn3—O11iv93.86 (8)P3—O8—Zn1v119.29 (9)
O10—Zn3—O11iv91.57 (10)P3—O9—Zn3143.17 (12)
O10iv—Zn3—O11iv88.43 (10)Zn3—O10—H8114.5
O9iv—Zn3—O1193.86 (8)Zn3—O10—H9114.5
O9—Zn3—O1186.14 (8)H8—O10—H990.9
O10—Zn3—O1188.43 (10)Zn3—O11—H10125.1
O10iv—Zn3—O1191.57 (10)Zn3—O11—H11106.4
O11iv—Zn3—O11180.0 (2)H10—O11—H11101.0
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z; (iii) x+1, y+1, z; (iv) x+1, y, z+1; (v) x, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H4···O8vi0.951.962.904 (2)170
N1—H5···O9vii0.802.233.035 (3)174
N1—H6···O5v0.872.002.865 (3)173
N1—H7···O70.951.942.887 (2)172
O10—H8···O1i0.772.313.022 (3)154
O10—H9···O40.962.083.004 (3)162
O10—H9···O60.962.383.069 (3)129
O11—H10···O20.812.002.742 (2)153
O11—H11···O41.102.433.410 (3)148
Symmetry codes: (i) x+1, y+1, z+1; (v) x, y1, z; (vi) x, y, z; (vii) x+1, y, z.
 

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