Download citation
Download citation
link to html
(NH4)2Zn(H2P2O7)2·2H2O is isostructural with its manganese homologue. Isolated almost-regular ZnO6 octahedra form a layered structure. The IR and Raman spectra show bands characteristic of H2P2O7 groups.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805004642/br6177sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805004642/br6177Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 301 K
  • Mean [sigma](P-O) = 0.002 Å
  • R factor = 0.032
  • wR factor = 0.090
  • Data-to-parameter ratio = 11.5

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 4 O1 -ZN1 -O1 -P1 52.00100.00 2.565 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 20 O5 -ZN1 -O5 -P2 -12.00100.00 2.565 1.555 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.90(3), Rep 0.896(10) ...... 3.00 su-Rat O2 -H2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.90(3), Rep 0.895(10) ...... 3.00 su-Rat O7 -H7 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.842(10) ...... 3.00 su-Rat O8 -H81 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.90(2), Rep 0.896(9) ...... 2.22 su-Rat N1 -H13 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.90(2), Rep 0.894(9) ...... 2.22 su-Rat N1 -H14 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.90(3), Rep 0.896(10) ...... 3.00 su-Rat O2 -H2 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.90(3), Rep 0.895(10) ...... 3.00 su-Rat O7 -H7 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.842(10) ...... 3.00 su-Rat O8 -H81 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.90(2), Rep 0.896(9) ...... 2.22 su-Rat N1 -H13 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.90(2), Rep 0.894(9) ...... 2.22 su-Rat N1 -H14 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.61(3), Rep 1.610(12) ...... 2.50 su-Rat H2 -O6 1.555 1.655 PLAT736_ALERT_1_C H...A Calc 1.95(3), Rep 1.948(10) ...... 3.00 su-Rat H81 -O3 1.555 1.565 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 H4 N
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 17 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 13 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2001); cell refinement: CrysAlis RED (Oxford Diffraction, 2001); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97.

diammonium zinc(II) dihydrogendiphosphate dihydrate top
Crystal data top
(NH4)2Zn(H2P2O7)2·2H2OZ = 1
Mr = 489.40F(000) = 248
Triclinic, P1Dx = 2.168 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.0074 (9) ÅCell parameters from 2048 reflections
b = 7.339 (1) Åθ = 2.8–29.8°
c = 7.796 (1) ŵ = 2.15 mm1
α = 81.240 (1)°T = 301 K
β = 71.080 (1)°Prism, colourless
γ = 88.150 (1)°0.26 × 0.18 × 0.08 mm
V = 374.78 (9) Å3
Data collection top
Oxford Diffraction Xcalibur with Sapphire CCD detector
diffractometer
1495 independent reflections
Radiation source: fine-focus sealed tube1402 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.036
Rotation method data acquisition using ω scansθmax = 26.4°, θmin = 4.1°
Absorption correction: analytical
(CrysAlis RED; Oxford Diffraction, 2003)
h = 88
Tmin = 0.605, Tmax = 0.847k = 96
2491 measured reflectionsl = 99
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)] = 0.032Hydrogen site location: difference Fourier map
wR(F2) = 0.090H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.0631P)2 + 0.1969P]
where P = (Fo2 + 2Fc2)/3
1495 reflections(Δ/σ)max = 0.001
130 parametersΔρmax = 0.78 e Å3
14 restraintsΔρmin = 0.72 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
Zn10.00000.50000.00000.01777 (16)
P10.25823 (9)0.21050 (8)0.25586 (8)0.01649 (18)
P20.15613 (9)0.25890 (8)0.25619 (8)0.01671 (18)
O10.2489 (3)0.3567 (3)0.1397 (3)0.0256 (4)
O20.4409 (3)0.2373 (3)0.4346 (2)0.0272 (4)
H20.552 (3)0.269 (5)0.412 (5)0.033*
O30.2456 (3)0.0158 (3)0.1574 (3)0.0321 (5)
O40.0814 (3)0.2336 (3)0.3463 (3)0.0237 (4)
O50.1912 (3)0.3815 (2)0.1113 (3)0.0217 (4)
O60.2283 (3)0.3292 (3)0.4143 (3)0.0263 (4)
O70.2490 (3)0.0646 (3)0.1662 (3)0.0279 (4)
H70.226 (6)0.022 (5)0.061 (3)0.033*
O80.0560 (3)0.7172 (3)0.2218 (3)0.0311 (5)
H810.118 (5)0.805 (4)0.204 (4)0.037*
H820.102 (5)0.705 (4)0.3338 (19)0.037*
N10.4171 (4)0.7101 (3)0.2020 (3)0.0292 (5)
H110.5452 (18)0.685 (3)0.131 (3)0.035*
H120.408 (4)0.715 (3)0.3199 (15)0.035*
H130.337 (3)0.622 (3)0.172 (3)0.035*
H140.379 (4)0.819 (3)0.184 (3)0.035*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0194 (2)0.0188 (2)0.0169 (2)0.00129 (15)0.00712 (17)0.00460 (15)
P10.0152 (3)0.0208 (3)0.0138 (3)0.0008 (2)0.0047 (2)0.0035 (2)
P20.0155 (3)0.0207 (3)0.0155 (3)0.0014 (2)0.0067 (2)0.0035 (2)
O10.0221 (9)0.0319 (10)0.0272 (10)0.0024 (7)0.0094 (8)0.0149 (8)
O20.0166 (9)0.0490 (12)0.0155 (9)0.0049 (8)0.0029 (7)0.0076 (8)
O30.0463 (12)0.0248 (9)0.0277 (11)0.0059 (8)0.0178 (10)0.0024 (8)
O40.0169 (8)0.0377 (10)0.0200 (9)0.0022 (7)0.0079 (7)0.0106 (8)
O50.0199 (8)0.0241 (8)0.0235 (9)0.0002 (7)0.0074 (7)0.0097 (7)
O60.0208 (9)0.0402 (10)0.0188 (9)0.0030 (8)0.0097 (8)0.0012 (8)
O70.0363 (11)0.0238 (9)0.0251 (10)0.0098 (8)0.0120 (9)0.0016 (8)
O80.0458 (13)0.0253 (9)0.0190 (9)0.0076 (8)0.0063 (9)0.0009 (7)
N10.0338 (13)0.0322 (12)0.0227 (12)0.0021 (10)0.0111 (10)0.0031 (10)
Geometric parameters (Å, º) top
Zn1—O1i2.0816 (18)P2—O51.5040 (17)
Zn1—O12.0816 (18)P2—O71.5521 (19)
Zn1—O5i2.0888 (17)P2—O41.5997 (19)
Zn1—O52.0888 (17)O2—H20.896 (10)
Zn1—O82.108 (2)O7—H70.895 (10)
Zn1—O8i2.108 (2)O8—H810.842 (10)
P1—O11.4930 (18)O8—H820.844 (10)
P1—O31.506 (2)N1—H110.896 (9)
P1—O21.5476 (18)N1—H120.897 (9)
P1—O41.6056 (19)N1—H130.896 (9)
P2—O61.4950 (19)N1—H140.894 (9)
O1i—Zn1—O1180.0O6—P2—O5116.10 (11)
O1i—Zn1—O5i92.85 (7)O6—P2—O7109.92 (11)
O1—Zn1—O5i87.15 (7)O5—P2—O7109.59 (11)
O1i—Zn1—O587.15 (7)O6—P2—O4104.82 (10)
O1—Zn1—O592.85 (7)O5—P2—O4108.97 (10)
O5i—Zn1—O5180.0O7—P2—O4106.97 (11)
O1i—Zn1—O888.23 (8)P1—O1—Zn1128.95 (11)
O1—Zn1—O891.77 (8)P1—O2—H2111 (2)
O5i—Zn1—O892.18 (8)P2—O4—P1130.82 (12)
O5—Zn1—O887.82 (8)P2—O5—Zn1133.31 (11)
O1i—Zn1—O8i91.77 (8)P2—O7—H7114 (2)
O1—Zn1—O8i88.23 (8)Zn1—O8—H81111 (2)
O5i—Zn1—O8i87.82 (8)Zn1—O8—H82125 (2)
O5—Zn1—O8i92.18 (8)H81—O8—H82108.8 (16)
O8—Zn1—O8i180.0H11—N1—H12109.0 (13)
O1—P1—O3114.88 (12)H11—N1—H13109.3 (14)
O1—P1—O2112.54 (11)H12—N1—H13110.0 (14)
O3—P1—O2111.10 (12)H11—N1—H14109.3 (14)
O1—P1—O4111.00 (10)H12—N1—H14109.9 (14)
O3—P1—O4107.63 (11)H13—N1—H14109 (3)
O2—P1—O498.36 (10)
O3—P1—O1—Zn194.77 (17)O1—P1—O4—P250.1 (2)
O2—P1—O1—Zn1136.75 (14)O3—P1—O4—P276.37 (18)
O4—P1—O1—Zn127.61 (18)O2—P1—O4—P2168.26 (16)
O1i—Zn1—O1—P152 (100)O6—P2—O5—Zn1123.32 (15)
O5i—Zn1—O1—P1174.21 (16)O7—P2—O5—Zn1111.43 (16)
O5—Zn1—O1—P15.79 (16)O4—P2—O5—Zn15.31 (18)
O8—Zn1—O1—P193.70 (16)O1i—Zn1—O5—P2173.00 (16)
O8i—Zn1—O1—P186.30 (16)O1—Zn1—O5—P27.00 (16)
O6—P2—O4—P1163.32 (16)O5i—Zn1—O5—P212 (100)
O5—P2—O4—P138.41 (19)O8—Zn1—O5—P284.66 (16)
O7—P2—O4—P179.99 (17)O8i—Zn1—O5—P295.34 (16)
Symmetry code: (i) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2—H2···O6ii0.90 (1)1.61 (1)2.495 (3)169 (4)
O7—H7···O3iii0.90 (1)1.64 (2)2.510 (3)162 (4)
O8—H81···O3iv0.84 (1)1.95 (1)2.788 (3)176 (3)
O8—H82···O6v0.84 (1)1.93 (1)2.770 (3)175 (4)
N1—H11···O5vi0.90 (1)2.18 (1)3.037 (3)161 (2)
N1—H12···O2v0.90 (1)1.98 (1)2.859 (3)167 (2)
N1—H13···O50.90 (1)2.08 (1)2.963 (3)169 (3)
N1—H14···O7iv0.89 (1)2.09 (1)2.977 (3)172 (2)
Symmetry codes: (ii) x+1, y, z; (iii) x, y, z; (iv) x, y+1, z; (v) x, y+1, z1; (vi) x1, y+1, z.
Brahim crystal Raman spectrum (cm-1) top
Raman frequencyMode assignment
3344.7OH stretching
3220NH stretching
2850NH4+ combination modes
1670OH2 bending
1340OH2 bending
1450NH4+ bending
1034.9-1192.4P—O stretching
970.6asymmetric P—O—P stretching
907.6asymmetric P—O—P stretching
748.2symmetric P—O—P stretching
473.6-578.5P—O bending modes and NH4+ torsional oscillation
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds