1,4-Butane­di­ammonium chromate

The title compound, [NH₃(CH₂)₄NH₃]²⁺·CrO₄²⁻, is a new chromate associated with the diprotonated 1,4-butane­di­amine mol­ecule. The structure can be described as a succession of inorganic and organic layers parallel to the (010) plane. The structural cohesion is established by a three-dimensional network of N—H...O hydrogen bonds.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.024
• wR factor = 0.075
• Data-to-parameter ratio = 15.8

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

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Computing details

Data collection: CAD-4 EXPRESS (Duisenberg, 1992; Macíček & Yordanov, 1992); cell refinement: CAD-4 EXPRESS; data reduction: MolEN (Fair, 1990); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Johnson & Burnett, 1997) and DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.

1,4-Butanediammonium chromate

Crystal data

(C4H14N2)[CrO4]	F(000) = 864
Mr = 206.17	Dx = 1.555 Mg m^−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 25 reflections
a = 8.824 (1) Å	θ = 11–14°
b = 10.547 (1) Å	µ = 1.27 mm^−1
c = 18.928 (2) Å	T = 293 K
V = 1761.6 (3) Å^3	Prism, yellow
Z = 8	0.6 × 0.2 × 0.1 mm

Data collection

Enraf-Nonius CAD-4 diffractometer	1619 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.000
Graphite monochromator	θmax = 27.0°, θmin = 2.2°
ω/2θ scans	h = 0→11
Absorption correction: ψ scan (North et al., 1968)	k = 0→13
Tmin = 0.713, Tmax = 0.880	l = 0→24
1917 measured reflections	2 standard reflections every 120 min
1917 independent reflections	intensity decay: 0.4%

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.024	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.075	w = 1/[σ^2(Fo^2) + (0.0369P)^2 + 0.8354P] where P = (Fo^2 + 2Fc^2)/3
S = 1.08	(Δ/σ)max = 0.001
1917 reflections	Δρmax = 0.30 e Å^−3
121 parameters	Δρmin = −0.24 e Å^−3
2 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0152 (8)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Cr	0.38106 (3)	0.15583 (2)	0.374920 (13)	0.02322 (12)
O1	0.42959 (18)	0.00320 (13)	0.37758 (6)	0.0379 (3)
O2	0.42301 (16)	0.21736 (12)	0.29649 (7)	0.0356 (3)
O3	0.20027 (15)	0.17205 (15)	0.38673 (8)	0.0430 (4)
O4	0.46787 (15)	0.23625 (13)	0.43870 (7)	0.0363 (3)
N1	0.3392 (2)	−0.14491 (15)	0.25923 (8)	0.0325 (3)
H3	0.377 (2)	−0.1050 (19)	0.2921 (10)	0.036 (6)*
N2	0.21269 (18)	0.12106 (15)	−0.00876 (8)	0.0305 (3)
H6	0.171 (3)	0.089 (2)	−0.0450 (10)	0.047 (7)*
C1	0.2767 (2)	−0.06117 (19)	0.20293 (10)	0.0347 (4)
H11	0.2096	0.0009	0.2241	0.043 (6)*
H21	0.2178	−0.1117	0.1701	0.051 (7)*
C2	0.4016 (2)	0.00679 (18)	0.16302 (9)	0.0307 (4)
H12	0.4668	−0.0555	0.1407	0.050 (7)*
H22	0.4626	0.0549	0.1962	0.048 (6)*
C3	0.3395 (2)	0.09667 (17)	0.10647 (10)	0.0302 (4)
H13	0.2614	0.1495	0.1273	0.051 (7)*
H23	0.4205	0.1519	0.0905	0.039 (6)*
C4	0.2732 (2)	0.02730 (16)	0.04290 (9)	0.0297 (4)
H14	0.3512	−0.0238	0.0206	0.040 (6)*
H24	0.1925	−0.0287	0.0582	0.039 (6)*
H1	0.4128	−0.1881	0.2435	0.039 (6)*
H2	0.2685	−0.1964	0.2744	0.046 (6)*
H4	0.2803	0.1756	−0.0238	0.042 (6)*
H5	0.1383	0.1659	0.0116	0.047 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr	0.02408 (18)	0.02478 (17)	0.02081 (17)	−0.00101 (10)	0.00070 (10)	−0.00009 (10)
O1	0.0536 (8)	0.0274 (7)	0.0327 (7)	0.0040 (6)	0.0034 (6)	0.0012 (5)
O2	0.0434 (7)	0.0365 (7)	0.0271 (6)	−0.0022 (6)	0.0050 (6)	0.0048 (5)
O3	0.0255 (7)	0.0557 (9)	0.0479 (8)	−0.0044 (6)	0.0048 (6)	−0.0063 (7)
O4	0.0361 (7)	0.0390 (7)	0.0338 (7)	0.0052 (6)	−0.0108 (6)	−0.0097 (6)
N1	0.0376 (8)	0.0337 (8)	0.0262 (8)	−0.0008 (7)	0.0053 (7)	0.0006 (6)
N2	0.0344 (8)	0.0341 (8)	0.0229 (7)	−0.0026 (7)	0.0008 (6)	0.0018 (6)
C1	0.0331 (10)	0.0400 (10)	0.0311 (9)	−0.0010 (8)	−0.0001 (7)	0.0047 (8)
C2	0.0293 (8)	0.0344 (9)	0.0284 (8)	−0.0014 (7)	−0.0019 (7)	0.0024 (7)
C3	0.0309 (9)	0.0300 (9)	0.0296 (8)	−0.0033 (7)	−0.0017 (7)	0.0011 (7)
C4	0.0351 (9)	0.0281 (8)	0.0259 (8)	0.0006 (7)	0.0018 (7)	0.0011 (7)

Geometric parameters (Å, º)

Cr—O3	1.6199 (14)	C1—C2	1.516 (2)
Cr—O2	1.6620 (12)	C1—H11	0.9700
Cr—O4	1.6624 (12)	C1—H21	0.9700
Cr—O1	1.6666 (14)	C2—C3	1.531 (2)
N1—C1	1.490 (2)	C2—H12	0.9700
N1—H3	0.823 (15)	C2—H22	0.9700
N1—H1	0.8477	C3—C4	1.525 (2)
N1—H2	0.8754	C3—H13	0.9700
N2—C4	1.490 (2)	C3—H23	0.9700
N2—H6	0.850 (16)	C4—H14	0.9700
N2—H4	0.8767	C4—H24	0.9700
N2—H5	0.8956
O3—Cr—O2	107.54 (8)	N1—C1—H21	109.3
O3—Cr—O4	107.44 (7)	C2—C1—H21	109.3
O2—Cr—O4	110.30 (7)	H11—C1—H21	108.0
O3—Cr—O1	110.54 (8)	C1—C2—C3	112.39 (15)
O2—Cr—O1	110.30 (6)	C1—C2—H12	109.1
O4—Cr—O1	110.63 (7)	C3—C2—H12	109.1
C1—N1—H3	112.9 (16)	C1—C2—H22	109.1
C1—N1—H1	110.5	C3—C2—H22	109.1
H3—N1—H1	103.2	H12—C2—H22	107.9
C1—N1—H2	109.8	C4—C3—C2	113.06 (15)
H3—N1—H2	111.2	C4—C3—H13	109.0
H1—N1—H2	109.2	C2—C3—H13	109.0
C4—N2—H6	114.9 (16)	C4—C3—H23	109.0
C4—N2—H4	113.9	C2—C3—H23	109.0
H6—N2—H4	107.3	H13—C3—H23	107.8
C4—N2—H5	109.3	N2—C4—C3	109.68 (14)
H6—N2—H5	103.7	N2—C4—H14	109.7
H4—N2—H5	107.0	C3—C4—H14	109.7
N1—C1—C2	111.59 (15)	N2—C4—H24	109.7
N1—C1—H11	109.3	C3—C4—H24	109.7
C2—C1—H11	109.3	H14—C4—H24	108.2

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H6···O1^i	0.85 (2)	1.97 (2)	2.815 (2)	173 (2)
N1—H3···O1	0.82 (2)	2.03 (2)	2.845 (2)	169 (2)
N2—H5···O4^ii	0.90	1.92	2.811 (2)	171
N1—H2···O2^iii	0.88	1.96	2.822 (2)	166
N1—H2···O3^iii	0.88	2.55	3.110 (2)	122
N1—H1···O2^iv	0.85	1.91	2.761 (2)	177
N2—H4···O3^v	0.88	2.44	2.947 (2)	117
N2—H4···O4^v	0.88	2.03	2.885 (2)	166

Symmetry codes: (i) −x+1/2, −y, z−1/2; (ii) x−1/2, y, −z+1/2; (iii) −x+1/2, y−1/2, z; (iv) −x+1, y−1/2, −z+1/2; (v) x, −y+1/2, z−1/2.