In the crystal structure of the title compound, (C
2N
2H
10)
2[Ni(HP
2O
7)
2(H
2O)
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
CCDC reference: 601218
Key indicators
- Single-crystal X-ray study
- T = 301 K
- Mean (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
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 = 568.88 | F(000) = 294 |
Triclinic, P1 | Dx = 1.946 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.4898 (9) Å | Cell parameters from 1929 reflections |
b = 7.5517 (7) Å | θ = 3.0–29.2° |
c = 9.7780 (1) Å | µ = 1.42 mm−1 |
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 tube | 1662 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
Rotation method data acquisition using ω scans | θmax = 26.4°, θmin = 4.1° |
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2002) | h = −9→9 |
Tmin = 0.785, Tmax = 0.920 | k = −9→9 |
3240 measured reflections | l = −11→12 |
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: inferred from neighbouring sites |
wR(F2) = 0.089 | H 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 parameters | Δρmax = 0.53 e Å−3 |
3 restraints | Δρmin = −0.72 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 | Uiso*/Ueq | |
Ni1 | 1.0000 | 1.0000 | 0.0000 | 0.01252 (15) | |
P1 | 1.22608 (10) | 0.71164 (9) | −0.14428 (8) | 0.01438 (18) | |
P2 | 1.29920 (9) | 0.77543 (9) | 0.18040 (7) | 0.01297 (17) | |
O1 | 1.0799 (3) | 0.8340 (2) | −0.1601 (2) | 0.0172 (4) | |
O2 | 1.3634 (3) | 0.7589 (3) | 0.0369 (2) | 0.0185 (4) | |
O3 | 1.1686 (3) | 0.9143 (2) | 0.17600 (19) | 0.0167 (4) | |
O4 | 1.1143 (3) | 0.4999 (3) | −0.2013 (2) | 0.0242 (5) | |
O5 | 1.3646 (3) | 0.7375 (3) | −0.2194 (2) | 0.0249 (5) | |
O6 | 1.4931 (3) | 0.8490 (3) | 0.3223 (2) | 0.0204 (4) | |
O7 | 1.1921 (3) | 0.5790 (3) | 0.1580 (2) | 0.0240 (5) | |
H7 | 1.1009 | 0.5848 | 0.1852 | 0.029* | |
O8 | 1.2352 (3) | 1.2237 (3) | 0.0447 (2) | 0.0210 (4) | |
H8A | 1.219 (4) | 1.334 (2) | 0.068 (3) | 0.025* | |
H8B | 1.3578 (18) | 1.232 (4) | 0.092 (3) | 0.025* | |
N1 | 0.8384 (3) | 0.8787 (3) | 0.2869 (2) | 0.0168 (5) | |
H1A | 0.8695 | 0.9718 | 0.2521 | 0.020* | |
H1C | 0.7220 | 0.8776 | 0.2921 | 0.020* | |
H1B | 0.8314 | 0.7695 | 0.2229 | 0.020* | |
N4 | 0.5620 (3) | 0.7615 (3) | 0.5911 (2) | 0.0196 (5) | |
H4A | 0.6775 | 0.8459 | 0.6437 | 0.024* | |
H4B | 0.4951 | 0.7630 | 0.6501 | 0.024* | |
H4C | 0.4928 | 0.7895 | 0.5071 | 0.024* | |
C2 | 0.9937 (4) | 0.9076 (4) | 0.4447 (3) | 0.0261 (7) | |
H2A | 1.1205 | 0.9081 | 0.4392 | 0.031* | |
H2B | 0.9615 | 0.8049 | 0.4820 | 0.031* | |
C3 | 0.5962 (4) | 0.5730 (4) | 0.5451 (3) | 0.0256 (6) | |
H3A | 0.6726 | 0.5429 | 0.6366 | 0.031* | |
H3B | 0.6716 | 0.5721 | 0.4827 | 0.031* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0119 (3) | 0.0121 (2) | 0.0139 (3) | 0.00482 (18) | 0.00507 (19) | 0.00399 (18) |
P1 | 0.0149 (3) | 0.0141 (3) | 0.0159 (3) | 0.0051 (3) | 0.0083 (3) | 0.0038 (3) |
P2 | 0.0122 (3) | 0.0124 (3) | 0.0149 (3) | 0.0041 (3) | 0.0052 (3) | 0.0052 (3) |
O1 | 0.0190 (9) | 0.0175 (9) | 0.0163 (9) | 0.0083 (7) | 0.0075 (8) | 0.0049 (7) |
O2 | 0.0163 (9) | 0.0239 (10) | 0.0170 (9) | 0.0062 (8) | 0.0079 (8) | 0.0067 (8) |
O3 | 0.0181 (10) | 0.0183 (9) | 0.0171 (9) | 0.0101 (8) | 0.0082 (8) | 0.0067 (8) |
O4 | 0.0278 (11) | 0.0125 (9) | 0.0308 (11) | 0.0039 (8) | 0.0144 (9) | 0.0011 (8) |
O5 | 0.0237 (11) | 0.0340 (12) | 0.0236 (11) | 0.0075 (9) | 0.0154 (9) | 0.0108 (9) |
O6 | 0.0158 (9) | 0.0267 (10) | 0.0180 (10) | 0.0058 (8) | 0.0052 (8) | 0.0084 (8) |
O7 | 0.0231 (11) | 0.0186 (10) | 0.0364 (12) | 0.0045 (8) | 0.0180 (10) | 0.0100 (9) |
O8 | 0.0148 (10) | 0.0152 (9) | 0.0303 (11) | 0.0029 (8) | 0.0080 (9) | 0.0045 (8) |
N1 | 0.0131 (11) | 0.0169 (11) | 0.0208 (12) | 0.0024 (9) | 0.0101 (9) | 0.0020 (9) |
N4 | 0.0261 (13) | 0.0151 (11) | 0.0164 (11) | 0.0029 (9) | 0.0090 (10) | 0.0037 (9) |
C2 | 0.0265 (15) | 0.0266 (16) | 0.0265 (16) | 0.0086 (12) | 0.0122 (13) | 0.0075 (13) |
C3 | 0.0263 (16) | 0.0206 (14) | 0.0277 (15) | 0.0069 (12) | 0.0085 (13) | 0.0071 (12) |
Geometric parameters (Å, º) top
Ni1—O3 | 2.0389 (17) | O8—H8B | 0.851 (10) |
Ni1—O3i | 2.0389 (17) | N1—C2 | 1.502 (4) |
Ni1—O1i | 2.0780 (17) | N1—H1A | 0.8900 |
Ni1—O1 | 2.0780 (17) | N1—H1C | 0.8900 |
Ni1—O8i | 2.1070 (18) | N1—H1B | 0.8900 |
Ni1—O8 | 2.1070 (18) | N4—C3 | 1.472 (3) |
P1—O5 | 1.4901 (19) | N4—H4A | 0.8900 |
P1—O1 | 1.5144 (19) | N4—H4B | 0.8900 |
P1—O4 | 1.5632 (19) | N4—H4C | 0.8900 |
P1—O2 | 1.6141 (19) | C2—C2ii | 1.515 (5) |
P2—O7 | 1.5134 (19) | C2—H2A | 0.9700 |
P2—O6 | 1.5163 (19) | C2—H2B | 0.9700 |
P2—O3 | 1.5248 (18) | C3—C3iii | 1.503 (5) |
P2—O2 | 1.6230 (18) | C3—H3A | 0.9700 |
O7—H7 | 0.8200 | C3—H3B | 0.9700 |
O8—H8A | 0.848 (10) | | |
| | | |
O3—Ni1—O3i | 180.0 | P2—O3—Ni1 | 131.55 (10) |
O3—Ni1—O1i | 86.68 (7) | P2—O7—H7 | 109.5 |
O3i—Ni1—O1i | 93.32 (7) | Ni1—O8—H8A | 117.5 (18) |
O3—Ni1—O1 | 93.32 (7) | Ni1—O8—H8B | 126.7 (19) |
O3i—Ni1—O1 | 86.68 (7) | H8A—O8—H8B | 106.3 (15) |
O1i—Ni1—O1 | 180.00 (8) | C2—N1—H1A | 109.5 |
O3—Ni1—O8i | 87.67 (8) | C2—N1—H1C | 109.5 |
O3i—Ni1—O8i | 92.33 (8) | H1A—N1—H1C | 109.5 |
O1i—Ni1—O8i | 88.94 (7) | C2—N1—H1B | 109.5 |
O1—Ni1—O8i | 91.06 (7) | H1A—N1—H1B | 109.5 |
O3—Ni1—O8 | 92.33 (8) | H1C—N1—H1B | 109.5 |
O3i—Ni1—O8 | 87.67 (8) | C3—N4—H4A | 109.5 |
O1i—Ni1—O8 | 91.06 (7) | C3—N4—H4B | 109.5 |
O1—Ni1—O8 | 88.94 (7) | H4A—N4—H4B | 109.5 |
O8i—Ni1—O8 | 180.000 (1) | C3—N4—H4C | 109.5 |
O5—P1—O1 | 116.41 (11) | H4A—N4—H4C | 109.5 |
O5—P1—O4 | 109.98 (11) | H4B—N4—H4C | 109.5 |
O1—P1—O4 | 109.98 (11) | N1—C2—C2ii | 110.1 (3) |
O5—P1—O2 | 105.77 (10) | N1—C2—H2A | 109.6 |
O1—P1—O2 | 108.27 (10) | C2ii—C2—H2A | 109.6 |
O4—P1—O2 | 105.81 (11) | N1—C2—H2B | 109.6 |
O7—P2—O6 | 113.18 (11) | C2ii—C2—H2B | 109.6 |
O7—P2—O3 | 112.79 (11) | H2A—C2—H2B | 108.2 |
O6—P2—O3 | 111.81 (10) | N4—C3—C3iii | 110.8 (3) |
O7—P2—O2 | 106.21 (11) | N4—C3—H3A | 109.5 |
O6—P2—O2 | 104.25 (10) | C3iii—C3—H3A | 109.5 |
O3—P2—O2 | 107.93 (10) | N4—C3—H3B | 109.5 |
P1—O1—Ni1 | 132.24 (11) | C3iii—C3—H3B | 109.5 |
P1—O2—P2 | 129.18 (12) | H3A—C3—H3B | 108.1 |
| | | |
O5—P1—O1—Ni1 | −131.40 (14) | O7—P2—O2—P1 | 67.87 (18) |
O4—P1—O1—Ni1 | 102.69 (15) | O6—P2—O2—P1 | −172.34 (15) |
O2—P1—O1—Ni1 | −12.48 (17) | O3—P2—O2—P1 | −53.33 (18) |
O3—Ni1—O1—P1 | −5.38 (15) | O7—P2—O3—Ni1 | −93.67 (16) |
O3i—Ni1—O1—P1 | 174.62 (15) | O6—P2—O3—Ni1 | 137.43 (13) |
O1i—Ni1—O1—P1 | 92 (100) | O2—P2—O3—Ni1 | 23.35 (17) |
O8i—Ni1—O1—P1 | −93.10 (15) | O3i—Ni1—O3—P2 | −132 (100) |
O8—Ni1—O1—P1 | 86.90 (15) | O1i—Ni1—O3—P2 | 178.89 (15) |
O5—P1—O2—P2 | 173.42 (14) | O1—Ni1—O3—P2 | −1.11 (15) |
O1—P1—O2—P2 | 47.97 (18) | O8i—Ni1—O3—P2 | 89.82 (15) |
O4—P1—O2—P2 | −69.90 (17) | O8—Ni1—O3—P2 | −90.18 (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···A | D—H | H···A | D···A | D—H···A |
O7—H7···O4iv | 0.82 | 1.73 | 2.501 (3) | 156 |
O8—H8A···O7v | 0.85 (1) | 1.92 (1) | 2.756 (3) | 169 (3) |
O8—H8B···O5vi | 0.85 (1) | 1.95 (1) | 2.795 (3) | 174 (3) |
N1—H1A···O1i | 0.89 | 1.96 | 2.846 (3) | 175 |
N1—H1C···O6vii | 0.89 | 1.84 | 2.718 (3) | 170 |
N1—H1B···O4iv | 0.89 | 2.10 | 2.888 (3) | 147 |
N4—H4A···O3ii | 0.89 | 2.04 | 2.816 (3) | 145 |
N4—H4B···O5viii | 0.89 | 1.89 | 2.779 (3) | 172 |
N4—H4C···O6vii | 0.89 | 1.96 | 2.748 (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) x−1, y, z; (viii) x−1, y, z+1. |