The structure of the title complex, (C4N2H14)[MoS4], consists of tetrahedral tetrathiomolybdate dianions connected to butane-1,4-diammonium dications, (1,4-bnH2)2+, via hydrogen bonding. The compound contains two crystallographically independent butane-1,4-diammonium dications in the asymmetric unit, both of which are located around centres of inversion. The anions are located in general positions.
Supporting information
CCDC reference: 289824
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.004 Å
- R factor = 0.026
- wR factor = 0.074
- Data-to-parameter ratio = 34.0
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C3
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 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
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: DIF4 (Stoe & Cie, 1998); cell refinement: DIF4; data reduction: REDU4 (Stoe & Cie, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1998); software used to prepare material for publication: CIFTAB in SHELXTL.
butane-1,4-diammonium tetrathiomolybdate(VI)
top
Crystal data top
(C4H14N2)[MoS4] | Z = 2 |
Mr = 314.35 | F(000) = 316 |
Triclinic, P1 | Dx = 1.747 Mg m−3 |
a = 7.1447 (11) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.2159 (12) Å | Cell parameters from 104 reflections |
c = 10.5031 (19) Å | θ = 15–18.5° |
α = 79.558 (10)° | µ = 1.75 mm−1 |
β = 81.561 (13)° | T = 293 K |
γ = 83.701 (12)° | Block, red |
V = 597.57 (17) Å3 | 0.12 × 0.09 × 0.07 mm |
Data collection top
Stoe AED-II four-circle diffractometer | 2852 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.027 |
Graphite monochromator | θmax = 30.0°, θmin = 2.9° |
ω/2θ scans | h = 0→10 |
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1998) | k = −11→11 |
Tmin = 0.824, Tmax = 0.887 | l = −14→14 |
3726 measured reflections | 4 standard reflections every 120 min |
3467 independent reflections | intensity decay: none |
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)] = 0.027 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.074 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0377P)2 + 0.2604P] where P = (Fo2 + 2Fc2)/3 |
3467 reflections | (Δ/σ)max = 0.001 |
102 parameters | Δρmax = 0.71 e Å−3 |
0 restraints | Δρmin = −0.65 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 | |
Mo | 0.78466 (3) | 0.46745 (2) | 0.76883 (2) | 0.03517 (7) | |
S1 | 1.02927 (9) | 0.34404 (9) | 0.66472 (7) | 0.04668 (15) | |
S2 | 0.81558 (11) | 0.73567 (8) | 0.73775 (7) | 0.04939 (16) | |
S3 | 0.76759 (10) | 0.36931 (8) | 0.97671 (7) | 0.04692 (15) | |
S4 | 0.53026 (10) | 0.42320 (11) | 0.69362 (8) | 0.05565 (18) | |
N1 | 0.7553 (3) | 0.7381 (3) | 1.0547 (2) | 0.0471 (5) | |
H1A | 0.6747 | 0.6832 | 1.1160 | 0.071* | |
H1B | 0.8735 | 0.6955 | 1.0638 | 0.071* | |
H1C | 0.7291 | 0.7290 | 0.9762 | 0.071* | |
C1 | 0.7362 (4) | 0.9161 (3) | 1.0685 (3) | 0.0525 (7) | |
H1D | 0.8177 | 0.9770 | 0.9980 | 0.063* | |
H1E | 0.7779 | 0.9266 | 1.1502 | 0.063* | |
C2 | 0.5329 (4) | 0.9917 (3) | 1.0658 (3) | 0.0433 (5) | |
H2A | 0.4499 | 0.9229 | 1.1297 | 0.052* | |
H2B | 0.5224 | 1.1007 | 1.0908 | 0.052* | |
N2 | 0.7677 (4) | 0.2874 (3) | 0.4312 (3) | 0.0558 (6) | |
H2C | 0.6854 | 0.3654 | 0.3954 | 0.084* | |
H2D | 0.8835 | 0.3001 | 0.3881 | 0.084* | |
H2E | 0.7677 | 0.2966 | 0.5143 | 0.084* | |
C3 | 0.7122 (5) | 0.1222 (4) | 0.4242 (4) | 0.0702 (10) | |
H3A | 0.8116 | 0.0388 | 0.4519 | 0.084* | |
H3B | 0.7008 | 0.1169 | 0.3341 | 0.084* | |
C4 | 0.5298 (4) | 0.0828 (3) | 0.5064 (3) | 0.0502 (6) | |
H4A | 0.4314 | 0.1689 | 0.4814 | 0.060* | |
H4B | 0.5429 | 0.0828 | 0.5970 | 0.060* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mo | 0.03135 (10) | 0.03155 (10) | 0.04152 (11) | −0.00230 (7) | −0.00552 (7) | −0.00286 (7) |
S1 | 0.0369 (3) | 0.0496 (3) | 0.0535 (4) | 0.0048 (3) | −0.0066 (3) | −0.0131 (3) |
S2 | 0.0592 (4) | 0.0325 (3) | 0.0518 (4) | −0.0045 (3) | 0.0020 (3) | −0.0018 (3) |
S3 | 0.0539 (4) | 0.0400 (3) | 0.0439 (3) | −0.0068 (3) | −0.0052 (3) | 0.0014 (2) |
S4 | 0.0359 (3) | 0.0686 (5) | 0.0627 (4) | −0.0063 (3) | −0.0102 (3) | −0.0076 (4) |
N1 | 0.0470 (12) | 0.0407 (11) | 0.0528 (12) | 0.0110 (9) | −0.0144 (10) | −0.0077 (9) |
C1 | 0.0454 (14) | 0.0405 (13) | 0.0768 (19) | 0.0026 (10) | −0.0263 (13) | −0.0125 (13) |
C2 | 0.0429 (12) | 0.0324 (11) | 0.0541 (15) | 0.0033 (9) | −0.0079 (11) | −0.0084 (10) |
N2 | 0.0542 (14) | 0.0524 (13) | 0.0619 (15) | −0.0210 (11) | 0.0010 (11) | −0.0101 (11) |
C3 | 0.0589 (19) | 0.0572 (18) | 0.097 (3) | −0.0234 (15) | 0.0158 (18) | −0.0296 (18) |
C4 | 0.0479 (14) | 0.0428 (13) | 0.0620 (16) | −0.0128 (11) | −0.0069 (12) | −0.0095 (12) |
Geometric parameters (Å, º) top
Mo—S1 | 2.1749 (8) | C2—H2A | 0.9700 |
Mo—S4 | 2.1750 (8) | C2—H2B | 0.9700 |
Mo—S3 | 2.1765 (8) | N2—C3 | 1.472 (4) |
Mo—S2 | 2.1992 (7) | N2—H2C | 0.8900 |
N1—C1 | 1.485 (3) | N2—H2D | 0.8900 |
N1—H1A | 0.8900 | N2—H2E | 0.8900 |
N1—H1B | 0.8900 | C3—C4 | 1.486 (4) |
N1—H1C | 0.8900 | C3—H3A | 0.9700 |
C1—C2 | 1.518 (3) | C3—H3B | 0.9700 |
C1—H1D | 0.9700 | C4—C4ii | 1.504 (5) |
C1—H1E | 0.9700 | C4—H4A | 0.9700 |
C2—C2i | 1.503 (5) | C4—H4B | 0.9700 |
| | | |
S1—Mo—S4 | 108.56 (3) | C2i—C2—H2B | 109.0 |
S1—Mo—S3 | 109.58 (3) | C1—C2—H2B | 109.0 |
S4—Mo—S3 | 110.28 (3) | H2A—C2—H2B | 107.8 |
S1—Mo—S2 | 109.41 (3) | C3—N2—H2C | 109.5 |
S4—Mo—S2 | 109.87 (3) | C3—N2—H2D | 109.5 |
S3—Mo—S2 | 109.14 (3) | H2C—N2—H2D | 109.5 |
C1—N1—H1A | 109.5 | C3—N2—H2E | 109.5 |
C1—N1—H1B | 109.5 | H2C—N2—H2E | 109.5 |
H1A—N1—H1B | 109.5 | H2D—N2—H2E | 109.5 |
C1—N1—H1C | 109.5 | N2—C3—C4 | 113.0 (3) |
H1A—N1—H1C | 109.5 | N2—C3—H3A | 109.0 |
H1B—N1—H1C | 109.5 | C4—C3—H3A | 109.0 |
N1—C1—C2 | 111.8 (2) | N2—C3—H3B | 109.0 |
N1—C1—H1D | 109.2 | C4—C3—H3B | 109.0 |
C2—C1—H1D | 109.2 | H3A—C3—H3B | 107.8 |
N1—C1—H1E | 109.2 | C3—C4—C4ii | 112.5 (3) |
C2—C1—H1E | 109.2 | C3—C4—H4A | 109.1 |
H1D—C1—H1E | 107.9 | C4ii—C4—H4A | 109.1 |
C2i—C2—C1 | 113.0 (3) | C3—C4—H4B | 109.1 |
C2i—C2—H2A | 109.0 | C4ii—C4—H4B | 109.1 |
C1—C2—H2A | 109.0 | H4A—C4—H4B | 107.8 |
Symmetry codes: (i) −x+1, −y+2, −z+2; (ii) −x+1, −y, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···S4iii | 0.89 | 2.39 | 3.263 (3) | 168 |
N1—H1B···S3iv | 0.89 | 2.55 | 3.410 (2) | 163 |
N1—H1C···S2 | 0.89 | 2.48 | 3.297 (3) | 153 |
N2—H2C···S4v | 0.89 | 2.35 | 3.238 (3) | 178 |
N2—H2D···S2vi | 0.89 | 2.37 | 3.240 (3) | 165 |
N2—H2E···S4 | 0.89 | 2.63 | 3.324 (3) | 136 |
N2—H2E···S1 | 0.89 | 2.72 | 3.417 (3) | 136 |
Symmetry codes: (iii) −x+1, −y+1, −z+2; (iv) −x+2, −y+1, −z+2; (v) −x+1, −y+1, −z+1; (vi) −x+2, −y+1, −z+1. |