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The Co atom of the title compound, (NH4)2[Co(SCN)4]·4H2O, is located on a special position of site symmetry \overline 4, whereas all atoms of the SCN ligand lie on general positions. As a result, the anions possess crystallographic \overline 4 symmetry. The ammonium cations are located on a twofold rotation axis parallel to c. The four water mol­ecules occupy general positions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803025029/wm6002sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803025029/wm6002Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](N-C) = 0.008 Å
  • H-atom completeness 1%
  • R factor = 0.054
  • wR factor = 0.177
  • Data-to-parameter ratio = 20.0

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O1
Author Response: The H atoms could not be located.

Alert level B PLAT430_ALERT_2_B Short Inter D...A Contact N2 .. N2 = 2.68 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact N2 .. N2 = 2.68 Ang.
Alert level C CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_weight 391.33 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 4.00 48.04 H 1.01 0.00 0.00 Co 58.93 1.00 58.93 N 14.01 6.00 84.04 O 16.00 4.00 64.00 S 32.07 4.00 128.26 Calculated formula weight 383.28 PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.99 PLAT040_ALERT_1_C No H-atoms in this Carbon Containing Compound .. ? PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 391.33 PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.60
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C4 H8 Co1 N6 O4 S4 Atom count from _chemical_formula_moiety:C4 H16 Co1 N6 O4 S4 FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C4 H8 Co1 N6 O4 S4 Atom count from the _atom_site data: C4 Co1 N6 O4 S4 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C4 H8 Co N6 O4 S4 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 8.00 8.00 0.00 H 16.00 0.00 16.00 Co 2.00 2.00 0.00 N 12.00 12.00 0.00 O 8.00 8.00 0.00 S 8.00 8.00 0.00 REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 27.22 From the CIF: _reflns_number_total 882 Count of symmetry unique reflns 536 Completeness (_total/calc) 164.55% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 346 Fraction of Friedel pairs measured 0.646 Are heavy atom types Z>Si present yes
1 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 5 ALERT level G = General alerts; check 9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 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 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: PLATON (Spek, 1990).

Diammonium tetrathiocyanatocobaltate(II) tetrahydrate top
Crystal data top
(NH4)2[Co(SCN)4]·4H2ODx = 1.628 Mg m3
Mr = 391.33Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P421cCell parameters from 6680 reflections
Hall symbol: P -4 2nθ = 3.7–27.0°
a = 12.2050 (16) ŵ = 1.61 mm1
c = 5.3588 (7) ÅT = 100 K
V = 798.26 (18) Å3Plate, blue
Z = 20.37 × 0.13 × 0.04 mm
F(000) = 394
Data collection top
Stoe IPDS II two-circle
diffractometer
882 independent reflections
Radiation source: fine-focus sealed tube729 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.043
ω scansθmax = 27.2°, θmin = 4.2°
Absorption correction: multi-scan
(MULABS; Spek, 1990; Blessing, 1995)
h = 1513
Tmin = 0.587, Tmax = 0.938k = 1515
5438 measured reflectionsl = 66
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullH-atom parameters not refined
R[F2 > 2σ(F2)] = 0.054 w = 1/[σ2(Fo2) + (0.1367P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.177(Δ/σ)max < 0.001
S = 1.04Δρmax = 0.95 e Å3
882 reflectionsΔρmin = 0.37 e Å3
44 parametersAbsolute structure: Flack (1983), 351 Friedel pairs
0 restraintsAbsolute structure parameter: 0.02 (7)
Primary atom site location: structure-invariant direct methods
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
Co10.50000.50000.00000.0451 (4)
N10.5480 (4)0.3801 (4)0.2196 (9)0.0481 (11)
C10.5714 (5)0.3251 (5)0.3912 (12)0.0499 (13)
S10.60884 (16)0.24747 (17)0.6240 (3)0.0663 (6)
O10.7943 (3)0.3749 (3)0.9965 (10)0.0506 (9)
N20.00000.50000.961 (5)0.161 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0540 (6)0.0540 (6)0.0273 (6)0.0000.0000.000
N10.056 (3)0.054 (3)0.034 (2)0.006 (2)0.0010 (19)0.000 (2)
C10.053 (3)0.058 (3)0.039 (3)0.007 (3)0.005 (3)0.000 (3)
S10.0789 (11)0.0798 (12)0.0401 (8)0.0270 (9)0.0085 (8)0.0138 (8)
O10.058 (2)0.0379 (17)0.056 (2)0.0095 (15)0.005 (2)0.001 (2)
N20.093 (10)0.116 (12)0.27 (3)0.013 (7)0.0000.000
Geometric parameters (Å, º) top
Co1—N1i1.967 (5)Co1—N11.967 (5)
Co1—N1ii1.967 (5)N1—C11.174 (8)
Co1—N1iii1.967 (5)C1—S11.632 (7)
N1i—Co1—N1ii110.97 (15)N1ii—Co1—N1106.5 (3)
N1i—Co1—N1iii106.5 (3)N1iii—Co1—N1110.97 (15)
N1ii—Co1—N1iii110.97 (15)C1—N1—Co1165.1 (5)
N1i—Co1—N1110.97 (15)N1—C1—S1177.6 (6)
Symmetry codes: (i) y, x+1, z; (ii) x+1, y+1, z; (iii) y+1, x, z.
 

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