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Di­ammonium nickel(II) di­hydrogendiphosphate(V) dihydrate is a member of the isotypic series (NH4)2T(H2P2O7)2·2H2O (T = Mn, Co or Zn). Isolated almost-regular NiO6 octahedra form a layered structure. The Raman spectrum shows bands characteristic of H2P2O7 groups.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805008640/wm6058sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805008640/wm6058Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 301 K
  • Mean [sigma](P-O) = 0.002 Å
  • R factor = 0.033
  • wR factor = 0.107
  • 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 ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 4 O1 -NI1 -O1 -P1 3.00100.00 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 -NI1 -O5 -P2 -44.00100.00 2.565 1.555 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.90(3), Rep 0.897(10) ...... 3.00 su-Rat O2 -H2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.90(3), Rep 0.901(10) ...... 3.00 su-Rat O7 -H7 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.846(10) ...... 3.00 su-Rat O8 -H81 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.898(19), Rep 0.895(9) ...... 2.11 su-Rat N1 -H11 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.90(3), Rep 0.896(10) ...... 3.00 su-Rat N1 -H13 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 110(3), Rep 109.9(14) ...... 2.14 su-Rat H12 -N1 -H13 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 110(3), Rep 109.8(14) ...... 2.14 su-Rat H11 -N1 -H14 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 110(3), Rep 109.5(14) ...... 2.14 su-Rat H12 -N1 -H14 1.555 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.90(3), Rep 0.897(10) ...... 3.00 su-Rat O2 -H2 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.90(3), Rep 0.901(10) ...... 3.00 su-Rat O7 -H7 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.846(10) ...... 3.00 su-Rat O8 -H81 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.898(19), Rep 0.895(9) ...... 2.11 su-Rat N1 -H11 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.90(3), Rep 0.896(10) ...... 3.00 su-Rat N1 -H13 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.61(3), Rep 1.615(13) ...... 2.31 su-Rat H2 -O6 1.555 1.655 PLAT736_ALERT_1_C H...A Calc 1.95(3), Rep 1.950(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 21 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 17 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 nickel(II) dihydrogendiphosphate(V) dihydrate top
Crystal data top
(NH4)2[Ni(H2P2O7)2(H2O)2]Z = 1
Mr = 482.74F(000) = 246
Triclinic, P1Dx = 2.137 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.0344 (9) ÅCell parameters from 2066 reflections
b = 7.3214 (9) Åθ = 3.0–29.8°
c = 7.792 (1) ŵ = 1.81 mm1
α = 81.53 (1)°T = 301 K
β = 70.91 (1)°Prism, light green
γ = 88.21 (1)°0.28 × 0.18 × 0.14 mm
V = 375.03 (8) Å3
Data collection top
Oxford Diffraction Xcalibur with Sapphire CCD detector
diffractometer
1496 independent reflections
Radiation source: fine-focus sealed tube1409 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
ω scansθmax = 26.4°, θmin = 4.1°
Absorption correction: analytical
(CrysAlis RED; Oxford Diffraction, 2001)
h = 84
Tmin = 0.632, Tmax = 0.786k = 99
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)] = 0.033Hydrogen site location: difference Fourier map
wR(F2) = 0.107H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.0733P)2 + 0.3934P]
where P = (Fo2 + 2Fc2)/3
1496 reflections(Δ/σ)max = 0.043
130 parametersΔρmax = 0.80 e Å3
14 restraintsΔρmin = 0.49 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
Ni10.00000.50000.00000.01619 (19)
P10.26016 (10)0.21160 (10)0.25634 (10)0.0164 (2)
P20.15287 (10)0.25971 (10)0.25832 (10)0.0168 (2)
O10.2493 (3)0.3609 (3)0.1412 (3)0.0254 (5)
O20.4451 (3)0.2364 (4)0.4361 (3)0.0275 (5)
H20.555 (4)0.281 (5)0.420 (6)0.033*
O30.2459 (4)0.0167 (3)0.1557 (3)0.0318 (5)
O40.0844 (3)0.2319 (3)0.3483 (3)0.0238 (5)
O50.1879 (3)0.3820 (3)0.1112 (3)0.0217 (4)
O60.2250 (3)0.3320 (3)0.4168 (3)0.0249 (5)
O70.2485 (4)0.0649 (3)0.1698 (3)0.0283 (5)
H70.229 (6)0.029 (6)0.061 (3)0.034*
O80.0536 (4)0.7156 (3)0.2159 (3)0.0284 (5)
H810.112 (5)0.809 (4)0.202 (4)0.034*
H820.107 (5)0.697 (5)0.326 (2)0.034*
N10.4186 (4)0.7074 (4)0.2002 (4)0.0297 (6)
H110.544 (2)0.681 (4)0.123 (3)0.036*
H120.413 (4)0.699 (4)0.3154 (18)0.036*
H130.333 (4)0.628 (4)0.167 (4)0.036*
H140.382 (5)0.822 (2)0.194 (4)0.036*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0165 (3)0.0172 (3)0.0165 (3)0.00024 (19)0.0068 (2)0.0040 (2)
P10.0135 (4)0.0206 (4)0.0162 (4)0.0004 (3)0.0060 (3)0.0039 (3)
P20.0141 (4)0.0212 (4)0.0173 (4)0.0005 (3)0.0078 (3)0.0038 (3)
O10.0223 (10)0.0299 (12)0.0286 (11)0.0032 (8)0.0109 (9)0.0136 (9)
O20.0168 (10)0.0472 (14)0.0194 (11)0.0026 (9)0.0053 (8)0.0091 (9)
O30.0435 (14)0.0243 (11)0.0304 (13)0.0053 (10)0.0182 (11)0.0028 (9)
O40.0141 (9)0.0373 (12)0.0236 (11)0.0045 (8)0.0087 (8)0.0106 (9)
O50.0186 (9)0.0247 (11)0.0246 (11)0.0020 (8)0.0088 (8)0.0091 (9)
O60.0182 (10)0.0381 (12)0.0206 (11)0.0003 (8)0.0114 (8)0.0006 (9)
O70.0375 (12)0.0224 (11)0.0278 (12)0.0087 (9)0.0146 (10)0.0016 (9)
O80.0396 (13)0.0248 (11)0.0190 (11)0.0049 (9)0.0071 (9)0.0018 (9)
N10.0343 (15)0.0302 (14)0.0273 (15)0.0049 (11)0.0137 (12)0.0049 (12)
Geometric parameters (Å, º) top
Ni1—O1i2.069 (2)P2—O51.510 (2)
Ni1—O12.069 (2)P2—O71.559 (2)
Ni1—O52.070 (2)P2—O41.604 (2)
Ni1—O5i2.070 (2)O2—H20.897 (10)
Ni1—O82.075 (2)O7—H70.901 (10)
Ni1—O8i2.075 (2)O8—H810.846 (10)
P1—O11.499 (2)O8—H820.847 (10)
P1—O31.513 (2)N1—H110.895 (9)
P1—O21.560 (2)N1—H120.896 (9)
P1—O41.613 (2)N1—H130.896 (10)
P2—O61.504 (2)N1—H140.899 (10)
O1i—Ni1—O1180.0O6—P2—O5116.09 (13)
O1i—Ni1—O586.76 (8)O6—P2—O7109.50 (13)
O1—Ni1—O593.24 (8)O5—P2—O7109.52 (12)
O1i—Ni1—O5i93.24 (8)O6—P2—O4105.22 (12)
O1—Ni1—O5i86.76 (8)O5—P2—O4109.11 (11)
O5—Ni1—O5i180.00 (9)O7—P2—O4106.95 (13)
O1i—Ni1—O888.33 (10)P1—O1—Ni1128.77 (13)
O1—Ni1—O891.67 (10)P1—O2—H2113 (3)
O5—Ni1—O887.95 (9)P2—O4—P1130.43 (14)
O5i—Ni1—O892.05 (9)P2—O5—Ni1133.64 (12)
O1i—Ni1—O8i91.67 (10)P2—O7—H7111 (3)
O1—Ni1—O8i88.33 (10)Ni1—O8—H81114 (3)
O5—Ni1—O8i92.05 (9)Ni1—O8—H82121 (3)
O5i—Ni1—O8i87.95 (9)H81—O8—H82107.5 (16)
O8—Ni1—O8i180.00 (10)H11—N1—H12109.9 (14)
O1—P1—O3115.06 (14)H11—N1—H13109.2 (14)
O1—P1—O2112.58 (13)H12—N1—H13109.9 (14)
O3—P1—O2111.15 (14)H11—N1—H14109.8 (14)
O1—P1—O4111.07 (12)H12—N1—H14109.5 (14)
O3—P1—O4107.19 (13)H13—N1—H14108 (3)
O2—P1—O498.40 (12)
O3—P1—O1—Ni192.82 (19)O1—P1—O4—P249.3 (2)
O2—P1—O1—Ni1138.44 (16)O3—P1—O4—P277.2 (2)
O4—P1—O1—Ni129.2 (2)O2—P1—O4—P2167.50 (19)
O1i—Ni1—O1—P13 (100)O6—P2—O5—Ni1122.84 (17)
O5—Ni1—O1—P17.41 (19)O7—P2—O5—Ni1112.55 (18)
O5i—Ni1—O1—P1172.59 (19)O4—P2—O5—Ni14.2 (2)
O8—Ni1—O1—P195.45 (19)O1i—Ni1—O5—P2173.11 (19)
O8i—Ni1—O1—P184.55 (19)O1—Ni1—O5—P26.89 (19)
O6—P2—O4—P1161.55 (18)O5i—Ni1—O5—P244 (100)
O5—P2—O4—P136.3 (2)O8—Ni1—O5—P284.67 (19)
O7—P2—O4—P182.0 (2)O8i—Ni1—O5—P295.33 (19)
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)1.62 (1)2.502 (3)169 (4)
O7—H7···O3iii0.90 (1)1.64 (1)2.525 (3)167 (4)
O8—H81···O3iv0.85 (1)1.95 (1)2.795 (3)177 (3)
O8—H82···O6v0.85 (1)1.94 (1)2.789 (3)177 (4)
N1—H11···O5vi0.90 (1)2.16 (1)3.038 (4)167 (3)
N1—H12···O2v0.90 (1)2.01 (1)2.869 (4)161 (3)
N1—H13···O50.90 (1)2.10 (2)2.966 (4)162 (3)
N1—H14···O7iv0.90 (1)2.10 (1)2.984 (4)169 (3)
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.
Raman spectral data top
Raman bands (cm-1)Mode assignment
3310OH stretching
3264NH stretching
2531NH4+ combination modes
1684OH2 bending
1313OH2 bending
1448NH4+ bending
1162–1044P—O stretching
966asymmetric P—O—P stretching
906asymmetric P—O—P stretching
755symmetric P—O—P stretching
536–455P—O bending modes and NH4+ torsional oscillation
 

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