(NH4)2[Ni(H2P2O7)2(H2O)2]

Essehli, R.; Lachkar, M.; Svoboda, I.; Fuess, H.; El Bali, B.

doi:10.1107/S1600536805008640

(NH₄)₂[Ni(H₂P₂O₇)₂(H₂O)₂]

R. Essehli, M. Lachkar, I. Svoboda, H. Fuess and B. El Bali

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.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805008640/wm6058sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536805008640/wm6058Isup2.hkl Contains datablock I

checkCIF report

Key indicators

Single-crystal X-ray study
T = 301 K
Mean (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
M_r = 482.74	F(000) = 246
Triclinic, P1	D_x = 2.137 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.0344 (9) Å	Cell parameters from 2066 reflections
b = 7.3214 (9) Å	θ = 3.0–29.8°
c = 7.792 (1) Å	µ = 1.81 mm⁻¹
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 tube	1409 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.027
ω scans	θ_max = 26.4°, θ_min = 4.1°
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2001)	h = −8→4
T_min = 0.632, T_max = 0.786	k = −9→9
2491 measured reflections	l = −9→9

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.033	Hydrogen site location: difference Fourier map
wR(F²) = 0.107	H-atom parameters constrained
S = 1.08	w = 1/[σ²(F_o²) + (0.0733P)² + 0.3934P] where P = (F_o² + 2F_c²)/3
1496 reflections	(Δ/σ)_max = 0.043
130 parameters	Δρ_max = 0.80 e Å⁻³
14 restraints	Δρ_min = −0.49 e Å⁻³

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

	x	y	z	U_iso*/U_eq
Ni1	0.0000	0.5000	0.0000	0.01619 (19)
P1	0.26016 (10)	0.21160 (10)	−0.25634 (10)	0.0164 (2)
P2	−0.15287 (10)	0.25971 (10)	−0.25832 (10)	0.0168 (2)
O1	0.2493 (3)	0.3609 (3)	−0.1412 (3)	0.0254 (5)
O2	0.4451 (3)	0.2364 (4)	−0.4361 (3)	0.0275 (5)
H2	0.555 (4)	0.281 (5)	−0.420 (6)	0.033*
O3	0.2459 (4)	0.0167 (3)	−0.1557 (3)	0.0318 (5)
O4	0.0844 (3)	0.2319 (3)	−0.3483 (3)	0.0238 (5)
O5	−0.1879 (3)	0.3820 (3)	−0.1112 (3)	0.0217 (4)
O6	−0.2250 (3)	0.3320 (3)	−0.4168 (3)	0.0249 (5)
O7	−0.2485 (4)	0.0649 (3)	−0.1698 (3)	0.0283 (5)
H7	−0.229 (6)	0.029 (6)	−0.061 (3)	0.034*
O8	0.0536 (4)	0.7156 (3)	−0.2159 (3)	0.0284 (5)
H81	0.112 (5)	0.809 (4)	−0.202 (4)	0.034*
H82	0.107 (5)	0.697 (5)	−0.326 (2)	0.034*
N1	−0.4186 (4)	0.7074 (4)	−0.2002 (4)	0.0297 (6)
H11	−0.544 (2)	0.681 (4)	−0.123 (3)	0.036*
H12	−0.413 (4)	0.699 (4)	−0.3154 (18)	0.036*
H13	−0.333 (4)	0.628 (4)	−0.167 (4)	0.036*
H14	−0.382 (5)	0.822 (2)	−0.194 (4)	0.036*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.0165 (3)	0.0172 (3)	0.0165 (3)	−0.00024 (19)	−0.0068 (2)	−0.0040 (2)
P1	0.0135 (4)	0.0206 (4)	0.0162 (4)	0.0004 (3)	−0.0060 (3)	−0.0039 (3)
P2	0.0141 (4)	0.0212 (4)	0.0173 (4)	−0.0005 (3)	−0.0078 (3)	−0.0038 (3)
O1	0.0223 (10)	0.0299 (12)	0.0286 (11)	0.0032 (8)	−0.0109 (9)	−0.0136 (9)
O2	0.0168 (10)	0.0472 (14)	0.0194 (11)	−0.0026 (9)	−0.0053 (8)	−0.0091 (9)
O3	0.0435 (14)	0.0243 (11)	0.0304 (13)	−0.0053 (10)	−0.0182 (11)	0.0028 (9)
O4	0.0141 (9)	0.0373 (12)	0.0236 (11)	0.0045 (8)	−0.0087 (8)	−0.0106 (9)
O5	0.0186 (9)	0.0247 (11)	0.0246 (11)	0.0020 (8)	−0.0088 (8)	−0.0091 (9)
O6	0.0182 (10)	0.0381 (12)	0.0206 (11)	−0.0003 (8)	−0.0114 (8)	0.0006 (9)
O7	0.0375 (12)	0.0224 (11)	0.0278 (12)	−0.0087 (9)	−0.0146 (10)	−0.0016 (9)
O8	0.0396 (13)	0.0248 (11)	0.0190 (11)	−0.0049 (9)	−0.0071 (9)	−0.0018 (9)
N1	0.0343 (15)	0.0302 (14)	0.0273 (15)	0.0049 (11)	−0.0137 (12)	−0.0049 (12)

Geometric parameters (Å, º) top

Ni1—O1ⁱ	2.069 (2)	P2—O5	1.510 (2)
Ni1—O1	2.069 (2)	P2—O7	1.559 (2)
Ni1—O5	2.070 (2)	P2—O4	1.604 (2)
Ni1—O5ⁱ	2.070 (2)	O2—H2	0.897 (10)
Ni1—O8	2.075 (2)	O7—H7	0.901 (10)
Ni1—O8ⁱ	2.075 (2)	O8—H81	0.846 (10)
P1—O1	1.499 (2)	O8—H82	0.847 (10)
P1—O3	1.513 (2)	N1—H11	0.895 (9)
P1—O2	1.560 (2)	N1—H12	0.896 (9)
P1—O4	1.613 (2)	N1—H13	0.896 (10)
P2—O6	1.504 (2)	N1—H14	0.899 (10)

O1ⁱ—Ni1—O1	180.0	O6—P2—O5	116.09 (13)
O1ⁱ—Ni1—O5	86.76 (8)	O6—P2—O7	109.50 (13)
O1—Ni1—O5	93.24 (8)	O5—P2—O7	109.52 (12)
O1ⁱ—Ni1—O5ⁱ	93.24 (8)	O6—P2—O4	105.22 (12)
O1—Ni1—O5ⁱ	86.76 (8)	O5—P2—O4	109.11 (11)
O5—Ni1—O5ⁱ	180.00 (9)	O7—P2—O4	106.95 (13)
O1ⁱ—Ni1—O8	88.33 (10)	P1—O1—Ni1	128.77 (13)
O1—Ni1—O8	91.67 (10)	P1—O2—H2	113 (3)
O5—Ni1—O8	87.95 (9)	P2—O4—P1	130.43 (14)
O5ⁱ—Ni1—O8	92.05 (9)	P2—O5—Ni1	133.64 (12)
O1ⁱ—Ni1—O8ⁱ	91.67 (10)	P2—O7—H7	111 (3)
O1—Ni1—O8ⁱ	88.33 (10)	Ni1—O8—H81	114 (3)
O5—Ni1—O8ⁱ	92.05 (9)	Ni1—O8—H82	121 (3)
O5ⁱ—Ni1—O8ⁱ	87.95 (9)	H81—O8—H82	107.5 (16)
O8—Ni1—O8ⁱ	180.00 (10)	H11—N1—H12	109.9 (14)
O1—P1—O3	115.06 (14)	H11—N1—H13	109.2 (14)
O1—P1—O2	112.58 (13)	H12—N1—H13	109.9 (14)
O3—P1—O2	111.15 (14)	H11—N1—H14	109.8 (14)
O1—P1—O4	111.07 (12)	H12—N1—H14	109.5 (14)
O3—P1—O4	107.19 (13)	H13—N1—H14	108 (3)
O2—P1—O4	98.40 (12)

O3—P1—O1—Ni1	−92.82 (19)	O1—P1—O4—P2	−49.3 (2)
O2—P1—O1—Ni1	138.44 (16)	O3—P1—O4—P2	77.2 (2)
O4—P1—O1—Ni1	29.2 (2)	O2—P1—O4—P2	−167.50 (19)
O1ⁱ—Ni1—O1—P1	3 (100)	O6—P2—O5—Ni1	−122.84 (17)
O5—Ni1—O1—P1	−7.41 (19)	O7—P2—O5—Ni1	112.55 (18)
O5ⁱ—Ni1—O1—P1	172.59 (19)	O4—P2—O5—Ni1	−4.2 (2)
O8—Ni1—O1—P1	−95.45 (19)	O1ⁱ—Ni1—O5—P2	173.11 (19)
O8ⁱ—Ni1—O1—P1	84.55 (19)	O1—Ni1—O5—P2	−6.89 (19)
O6—P2—O4—P1	161.55 (18)	O5ⁱ—Ni1—O5—P2	−44 (100)
O5—P2—O4—P1	36.3 (2)	O8—Ni1—O5—P2	84.67 (19)
O7—P2—O4—P1	−82.0 (2)	O8ⁱ—Ni1—O5—P2	−95.33 (19)

Symmetry code: (i) −x, −y+1, −z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O2—H2···O6ⁱⁱ	0.90 (1)	1.62 (1)	2.502 (3)	169 (4)
O7—H7···O3ⁱⁱⁱ	0.90 (1)	1.64 (1)	2.525 (3)	167 (4)
O8—H81···O3^iv	0.85 (1)	1.95 (1)	2.795 (3)	177 (3)
O8—H82···O6^v	0.85 (1)	1.94 (1)	2.789 (3)	177 (4)
N1—H11···O5^vi	0.90 (1)	2.16 (1)	3.038 (4)	167 (3)
N1—H12···O2^v	0.90 (1)	2.01 (1)	2.869 (4)	161 (3)
N1—H13···O5	0.90 (1)	2.10 (2)	2.966 (4)	162 (3)
N1—H14···O7^iv	0.90 (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, −z−1; (vi) −x−1, −y+1, −z.

Raman spectral data top

Raman bands (cm^-1)	Mode assignment
3310	OH stretching
3264	NH stretching
2531	NH₄⁺ combination modes
1684	OH₂ bending
1313	OH₂ bending
1448	NH₄⁺ bending
1162–1044	P—O stretching
966	asymmetric P—O—P stretching
906	asymmetric P—O—P stretching
755	symmetric P—O—P stretching
536–455	P—O bending modes and NH₄⁺ torsional oscillation

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