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A new organic chromate, ethylenediammonium chromate, [NH3(CH2)2NH3][CrO4], has been isolated. Its structure is built up from organic cations and chromate anions, which pack in columns parallel to the a axis. The cohesion and stability of the ionic arragement result from a three-dimensional network of N—H...O hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804012747/dn6139sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804012747/dn6139Isup2.hkl
Contains datablock I

CCDC reference: 245109

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.023
  • wR factor = 0.067
  • Data-to-parameter ratio = 10.3

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT052_ALERT_1_A (Proper) Absorption Correction Method Missing .. ?
Alert level B PLAT057_ALERT_3_B Correction for Absorption Required RT(exp) ... 1.30
Alert level C PLAT034_ALERT_1_C No Flack Parameter Given. Z .GT. Si, NonCentro . ? PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C2 H10 N2
Alert level G REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 27.96 From the CIF: _reflns_number_total 1141 Count of symmetry unique reflns 1010 Completeness (_total/calc) 112.97% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 131 Fraction of Friedel pairs measured 0.130 Are heavy atom types Z>Si present yes
1 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 1 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: CAD-4 EXPRESS (Duisenberg, 1992; Macíček & Yordanov, 1992); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Johnson & Burnett, 1997) et DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.

ethylenediammonium chromate top
Crystal data top
(C2H10N2)[CrO4]F(000) = 368
Mr = 178.12Dx = 1.676 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 25 reflections
a = 6.6778 (13) Åθ = 10.2–15.1°
b = 8.9040 (17) ŵ = 1.57 mm1
c = 11.876 (2) ÅT = 293 K
V = 706.1 (2) Å3Prism, yellow
Z = 40.35 × 0.27 × 0.15 mm
Data collection top
Enraf-Nonius CAD-4
diffractometer
1076 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.046
Graphite monochromatorθmax = 28.0°, θmin = 2.9°
ω/2θ scansh = 18
Absorption correction: ψ scan
(North et al., 1968)
k = 011
Tmin = 0.607, Tmax = 0.790l = 015
1167 measured reflections2 standard reflections every 120 min
1141 independent reflections intensity decay: 1.0%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.023H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.067 w = 1/[σ2(Fo2) + (0.0364P)2 + 0.1776P]
where P = (Fo2 + 2Fc2)/3
S = 1.13(Δ/σ)max = 0.001
1141 reflectionsΔρmax = 0.29 e Å3
111 parametersΔρmin = 0.28 e Å3
2 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.034 (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
xyzUiso*/Ueq
Cr0.17097 (6)0.48771 (4)0.60978 (3)0.02252 (14)
O10.0566 (3)0.5515 (3)0.6077 (2)0.0413 (5)
O20.3272 (3)0.63750 (18)0.60783 (15)0.0269 (4)
O30.2139 (3)0.3897 (2)0.72717 (15)0.0337 (5)
O40.2161 (4)0.3827 (2)0.49964 (16)0.0381 (5)
N10.0498 (4)0.3830 (3)0.9090 (2)0.0262 (5)
N20.4612 (4)0.6425 (3)0.8120 (2)0.0297 (5)
C10.3386 (4)0.5036 (3)0.8198 (2)0.0286 (5)
H110.28580.47860.74610.046 (10)*
H120.42210.42080.84470.032 (9)*
C20.1668 (4)0.5251 (3)0.9020 (2)0.0272 (5)
H210.08110.60620.87660.038 (9)*
H220.21880.55120.97570.039 (9)*
H1A0.028 (6)0.377 (4)0.966 (3)0.036 (9)*
H1B0.132 (6)0.305 (4)0.911 (3)0.035 (9)*
H1C0.041 (5)0.371 (4)0.851 (3)0.034 (9)*
H2A0.378 (4)0.714 (3)0.809 (3)0.030 (8)*
H2B0.526 (6)0.649 (4)0.880 (3)0.044 (10)*
H2C0.533 (8)0.637 (6)0.750 (3)0.089 (17)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cr0.0236 (2)0.02180 (18)0.02219 (19)0.00060 (15)0.00038 (16)0.00056 (15)
O10.0248 (10)0.0463 (11)0.0529 (12)0.0033 (9)0.0011 (10)0.0029 (12)
O20.0281 (9)0.0235 (7)0.0293 (8)0.0018 (7)0.0002 (10)0.0012 (7)
O30.0428 (12)0.0315 (9)0.0266 (9)0.0045 (10)0.0041 (9)0.0065 (7)
O40.0491 (13)0.0357 (10)0.0294 (9)0.0023 (11)0.0001 (10)0.0086 (8)
N10.0265 (11)0.0243 (10)0.0279 (11)0.0013 (9)0.0022 (10)0.0002 (9)
N20.0284 (12)0.0267 (11)0.0340 (12)0.0026 (10)0.0054 (11)0.0022 (10)
C10.0296 (12)0.0266 (11)0.0295 (11)0.0041 (16)0.0017 (11)0.0019 (10)
C20.0278 (12)0.0245 (10)0.0293 (11)0.0033 (13)0.0036 (12)0.0017 (10)
Geometric parameters (Å, º) top
Cr—O11.623 (2)N2—H2A0.85 (3)
Cr—O41.636 (2)N2—H2B0.92 (4)
Cr—O31.670 (2)N2—H2C0.88 (2)
Cr—O21.693 (2)C1—C21.518 (4)
N1—C21.489 (3)C1—H110.9700
N1—H1A0.85 (4)C1—H120.9700
N1—H1B0.88 (4)C2—H210.9700
N1—H1C0.92 (4)C2—H220.9700
N2—C11.486 (3)
O1—Cr—O4111.1 (1)C1—N2—H2C108 (4)
O1—Cr—O3110.9 (1)H2A—N2—H2C111 (4)
O4—Cr—O3109.7 (1)H2B—N2—H2C119 (4)
O1—Cr—O2107.5 (1)N2—C1—C2110.6 (2)
O4—Cr—O2109.0 (1)N2—C1—H11109.5
O3—Cr—O2108.5 (1)C2—C1—H11109.5
C2—N1—H1A115 (2)N2—C1—H12109.5
C2—N1—H1B110 (2)C2—C1—H12109.5
H1A—N1—H1B108 (3)H11—C1—H12108.1
C2—N1—H1C114 (2)N1—C2—C1109.0 (2)
H1A—N1—H1C100 (3)N1—C2—H21109.9
H1B—N1—H1C110 (3)C1—C2—H21109.9
C1—N2—H2A105 (2)N1—C2—H22109.9
C1—N2—H2B105 (2)C1—C2—H22109.9
H2A—N2—H2B107 (3)H21—C2—H22108.3
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O2i0.86 (4)1.95 (4)2.796 (3)171 (4)
N2—H2A···O3ii0.85 (3)1.95 (3)2.789 (3)170 (4)
N1—H1B···O1iii0.89 (4)2.57 (4)3.046 (4)112 (3)
N1—H1B···O2iii0.89 (4)1.99 (4)2.873 (3)170 (4)
N2—H2B···O4iv0.92 (4)1.91 (4)2.813 (3)165 (3)
N1—H1C···O30.92 (3)1.88 (3)2.787 (3)167 (3)
N2—H2C···O2v0.92 (3)1.93 (4)2.807 (3)175 (3)
Symmetry codes: (i) x+1/2, y+1, z+1/2; (ii) x, y+1/2, z+3/2; (iii) x, y1/2, z+3/2; (iv) x1/2, y+1, z+1/2; (v) x1, y, z.
 

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