Download citation
Download citation
link to html
In the crystal structure of the title compound, (C2N2H10)2[Ni(HP2O7)2(H2O)2], each Ni cation is surrounded by two symmetry-related diphosphate anions and two symmetry-related water mol­ecules within a distorted octa­hedron. The octa­hedra are connected via O—H...O hydrogen bonding into layers. The ethyl­enediammonium cations are located in the inter­layer space and are connected by N—H...O hydrogen bonds to the anionic layers. The Ni cation and the two crystallographically independent ethyl­enediammonium cations are located on centres of inversion, whereas the diphosphate anion and the water mol­ecule are located in general positions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806004399/nc6053sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806004399/nc6053Isup2.hkl
Contains datablock I

CCDC reference: 601218

Key indicators

  • Single-crystal X-ray study
  • T = 301 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.032
  • wR factor = 0.089
  • Data-to-parameter ratio = 13.8

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 ... # 6 O1 -NI1 -O1 -P1 9.00 0.00 2.775 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 18 O3 -NI1 -O3 -P2 13.00 0.00 2.775 1.555 1.555 1.555
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 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 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2002); cell refinement: CrysAlis RED (Oxford Diffraction, 2002); 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.

bis(ethylenediammonium) diaquabis[hydrogendiphosphato(3-)]nickel(II) top
Crystal data top
(C2H10N2)2[Ni(HP2O7)2(H2O)2]Z = 1
Mr = 568.88F(000) = 294
Triclinic, P1Dx = 1.946 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.4898 (9) ÅCell parameters from 1929 reflections
b = 7.5517 (7) Åθ = 3.0–29.2°
c = 9.7780 (1) ŵ = 1.42 mm1
α = 103.876 (9)°T = 301 K
β = 111.190 (1)°Prism, pale green
γ = 97.711 (8)°0.18 × 0.10 × 0.06 mm
V = 485.48 (9) Å3
Data collection top
Oxford Xcalibur
diffractometer with Sapphire CCD area detector
1930 independent reflections
Radiation source: fine-focus sealed tube1662 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
Rotation method data acquisition using ω scansθmax = 26.4°, θmin = 4.1°
Absorption correction: analytical
(CrysAlis RED; Oxford Diffraction, 2002)
h = 99
Tmin = 0.785, Tmax = 0.920k = 99
3240 measured reflectionsl = 1112
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: inferred from neighbouring sites
wR(F2) = 0.089H atoms treated by a mixture of independent and constrained refinement
S = 1.03 w = 1/[σ2(Fo2) + (0.0576P)2]
where P = (Fo2 + 2Fc2)/3
1930 reflections(Δ/σ)max = 0.010
140 parametersΔρmax = 0.53 e Å3
3 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
Ni11.00001.00000.00000.01252 (15)
P11.22608 (10)0.71164 (9)0.14428 (8)0.01438 (18)
P21.29920 (9)0.77543 (9)0.18040 (7)0.01297 (17)
O11.0799 (3)0.8340 (2)0.1601 (2)0.0172 (4)
O21.3634 (3)0.7589 (3)0.0369 (2)0.0185 (4)
O31.1686 (3)0.9143 (2)0.17600 (19)0.0167 (4)
O41.1143 (3)0.4999 (3)0.2013 (2)0.0242 (5)
O51.3646 (3)0.7375 (3)0.2194 (2)0.0249 (5)
O61.4931 (3)0.8490 (3)0.3223 (2)0.0204 (4)
O71.1921 (3)0.5790 (3)0.1580 (2)0.0240 (5)
H71.10090.58480.18520.029*
O81.2352 (3)1.2237 (3)0.0447 (2)0.0210 (4)
H8A1.219 (4)1.334 (2)0.068 (3)0.025*
H8B1.3578 (18)1.232 (4)0.092 (3)0.025*
N10.8384 (3)0.8787 (3)0.2869 (2)0.0168 (5)
H1A0.86950.97180.25210.020*
H1C0.72200.87760.29210.020*
H1B0.83140.76950.22290.020*
N40.5620 (3)0.7615 (3)0.5911 (2)0.0196 (5)
H4A0.67750.84590.64370.024*
H4B0.49510.76300.65010.024*
H4C0.49280.78950.50710.024*
C20.9937 (4)0.9076 (4)0.4447 (3)0.0261 (7)
H2A1.12050.90810.43920.031*
H2B0.96150.80490.48200.031*
C30.5962 (4)0.5730 (4)0.5451 (3)0.0256 (6)
H3A0.67260.54290.63660.031*
H3B0.67160.57210.48270.031*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0119 (3)0.0121 (2)0.0139 (3)0.00482 (18)0.00507 (19)0.00399 (18)
P10.0149 (3)0.0141 (3)0.0159 (3)0.0051 (3)0.0083 (3)0.0038 (3)
P20.0122 (3)0.0124 (3)0.0149 (3)0.0041 (3)0.0052 (3)0.0052 (3)
O10.0190 (9)0.0175 (9)0.0163 (9)0.0083 (7)0.0075 (8)0.0049 (7)
O20.0163 (9)0.0239 (10)0.0170 (9)0.0062 (8)0.0079 (8)0.0067 (8)
O30.0181 (10)0.0183 (9)0.0171 (9)0.0101 (8)0.0082 (8)0.0067 (8)
O40.0278 (11)0.0125 (9)0.0308 (11)0.0039 (8)0.0144 (9)0.0011 (8)
O50.0237 (11)0.0340 (12)0.0236 (11)0.0075 (9)0.0154 (9)0.0108 (9)
O60.0158 (9)0.0267 (10)0.0180 (10)0.0058 (8)0.0052 (8)0.0084 (8)
O70.0231 (11)0.0186 (10)0.0364 (12)0.0045 (8)0.0180 (10)0.0100 (9)
O80.0148 (10)0.0152 (9)0.0303 (11)0.0029 (8)0.0080 (9)0.0045 (8)
N10.0131 (11)0.0169 (11)0.0208 (12)0.0024 (9)0.0101 (9)0.0020 (9)
N40.0261 (13)0.0151 (11)0.0164 (11)0.0029 (9)0.0090 (10)0.0037 (9)
C20.0265 (15)0.0266 (16)0.0265 (16)0.0086 (12)0.0122 (13)0.0075 (13)
C30.0263 (16)0.0206 (14)0.0277 (15)0.0069 (12)0.0085 (13)0.0071 (12)
Geometric parameters (Å, º) top
Ni1—O32.0389 (17)O8—H8B0.851 (10)
Ni1—O3i2.0389 (17)N1—C21.502 (4)
Ni1—O1i2.0780 (17)N1—H1A0.8900
Ni1—O12.0780 (17)N1—H1C0.8900
Ni1—O8i2.1070 (18)N1—H1B0.8900
Ni1—O82.1070 (18)N4—C31.472 (3)
P1—O51.4901 (19)N4—H4A0.8900
P1—O11.5144 (19)N4—H4B0.8900
P1—O41.5632 (19)N4—H4C0.8900
P1—O21.6141 (19)C2—C2ii1.515 (5)
P2—O71.5134 (19)C2—H2A0.9700
P2—O61.5163 (19)C2—H2B0.9700
P2—O31.5248 (18)C3—C3iii1.503 (5)
P2—O21.6230 (18)C3—H3A0.9700
O7—H70.8200C3—H3B0.9700
O8—H8A0.848 (10)
O3—Ni1—O3i180.0P2—O3—Ni1131.55 (10)
O3—Ni1—O1i86.68 (7)P2—O7—H7109.5
O3i—Ni1—O1i93.32 (7)Ni1—O8—H8A117.5 (18)
O3—Ni1—O193.32 (7)Ni1—O8—H8B126.7 (19)
O3i—Ni1—O186.68 (7)H8A—O8—H8B106.3 (15)
O1i—Ni1—O1180.00 (8)C2—N1—H1A109.5
O3—Ni1—O8i87.67 (8)C2—N1—H1C109.5
O3i—Ni1—O8i92.33 (8)H1A—N1—H1C109.5
O1i—Ni1—O8i88.94 (7)C2—N1—H1B109.5
O1—Ni1—O8i91.06 (7)H1A—N1—H1B109.5
O3—Ni1—O892.33 (8)H1C—N1—H1B109.5
O3i—Ni1—O887.67 (8)C3—N4—H4A109.5
O1i—Ni1—O891.06 (7)C3—N4—H4B109.5
O1—Ni1—O888.94 (7)H4A—N4—H4B109.5
O8i—Ni1—O8180.000 (1)C3—N4—H4C109.5
O5—P1—O1116.41 (11)H4A—N4—H4C109.5
O5—P1—O4109.98 (11)H4B—N4—H4C109.5
O1—P1—O4109.98 (11)N1—C2—C2ii110.1 (3)
O5—P1—O2105.77 (10)N1—C2—H2A109.6
O1—P1—O2108.27 (10)C2ii—C2—H2A109.6
O4—P1—O2105.81 (11)N1—C2—H2B109.6
O7—P2—O6113.18 (11)C2ii—C2—H2B109.6
O7—P2—O3112.79 (11)H2A—C2—H2B108.2
O6—P2—O3111.81 (10)N4—C3—C3iii110.8 (3)
O7—P2—O2106.21 (11)N4—C3—H3A109.5
O6—P2—O2104.25 (10)C3iii—C3—H3A109.5
O3—P2—O2107.93 (10)N4—C3—H3B109.5
P1—O1—Ni1132.24 (11)C3iii—C3—H3B109.5
P1—O2—P2129.18 (12)H3A—C3—H3B108.1
O5—P1—O1—Ni1131.40 (14)O7—P2—O2—P167.87 (18)
O4—P1—O1—Ni1102.69 (15)O6—P2—O2—P1172.34 (15)
O2—P1—O1—Ni112.48 (17)O3—P2—O2—P153.33 (18)
O3—Ni1—O1—P15.38 (15)O7—P2—O3—Ni193.67 (16)
O3i—Ni1—O1—P1174.62 (15)O6—P2—O3—Ni1137.43 (13)
O1i—Ni1—O1—P192 (100)O2—P2—O3—Ni123.35 (17)
O8i—Ni1—O1—P193.10 (15)O3i—Ni1—O3—P2132 (100)
O8—Ni1—O1—P186.90 (15)O1i—Ni1—O3—P2178.89 (15)
O5—P1—O2—P2173.42 (14)O1—Ni1—O3—P21.11 (15)
O1—P1—O2—P247.97 (18)O8i—Ni1—O3—P289.82 (15)
O4—P1—O2—P269.90 (17)O8—Ni1—O3—P290.18 (15)
Symmetry codes: (i) x+2, y+2, z; (ii) x+2, y+2, z+1; (iii) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7···O4iv0.821.732.501 (3)156
O8—H8A···O7v0.85 (1)1.92 (1)2.756 (3)169 (3)
O8—H8B···O5vi0.85 (1)1.95 (1)2.795 (3)174 (3)
N1—H1A···O1i0.891.962.846 (3)175
N1—H1C···O6vii0.891.842.718 (3)170
N1—H1B···O4iv0.892.102.888 (3)147
N4—H4A···O3ii0.892.042.816 (3)145
N4—H4B···O5viii0.891.892.779 (3)172
N4—H4C···O6vii0.891.962.748 (3)146
Symmetry codes: (i) x+2, y+2, z; (ii) x+2, y+2, z+1; (iv) x+2, y+1, z; (v) x, y+1, z; (vi) x+3, y+2, z; (vii) x1, y, z; (viii) x1, y, z+1.
 

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