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The quaternary vanadium thio­phosphate CsVP2S7 (caesium vanadium diphospho­rus heptasulfide) was synthesized by reacting a mixture of Cs2S3, V, P4S3 and S. The crystal structure is composed of VS6 octahedra, which are linked by bitetrahedral [P2S7] groups to form two-dimensional anionic [VP2S7]- layers. The layers are stacked perpendicular to the crystallographic c axis and are separated by the Cs+ ions. The VS6 octahedra, the [P2S7] groups and the Cs+ ions are located in special positions. CsVP2S7 is isostructural to KVP2S7 and RbVP2S7.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804031150/wm6043sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804031150/wm6043Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](S-P) = 0.004 Å
  • R factor = 0.046
  • wR factor = 0.100
  • Data-to-parameter ratio = 23.2

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT035_ALERT_1_A No _chemical_absolute_configuration info given . ?
Author Response: The compound is not chiral. Therefore, only the absolute structure is needed. This was determined and is in agreement with the selected setting.

Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.37 PLAT199_ALERT_1_C Check the Reported cell_measurement_temperature 293 PLAT200_ALERT_1_C Check the Reported cell_ambient_temperature .... 293
Alert level G 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 27.03 From the CIF: _reflns_number_total 1205 Count of symmetry unique reflns 638 Completeness (_total/calc) 188.87% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 567 Fraction of Friedel pairs measured 0.889 Are heavy atom types Z>Si present yes
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 3 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

Computing details top

Data collection: DIF4 (Stoe & Cie, 1992); cell refinement: DIF4; data reduction: REDU4 (Stoe & Cie, 1992); 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: CIFTAB in SHELXTL (Bruker, 1998).

Caesium vanadium diphosphorus heptasulfide top
Crystal data top
CsVP2S7F(000) = 440
Mr = 470.21Dx = 2.864 Mg m3
Monoclinic, C2Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2yCell parameters from 68 reflections
a = 8.6010 (17) Åθ = 10–15°
b = 9.5176 (19) ŵ = 5.77 mm1
c = 6.7287 (13) ÅT = 293 K
β = 98.17 (3)°Plate, green
V = 545.23 (19) Å30.15 × 0.05 × 0.05 mm
Z = 2
Data collection top
Philips PW1100 4-circle-
diffractometer
979 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.044
Graphite monochromatorθmax = 27.0°, θmin = 3.1°
ω/θ scansh = 010
Absorption correction: numerical
X-SHAPE and X-RED (Stoe & Cie, 1998)
k = 1212
Tmin = 0.701, Tmax = 0.738l = 88
1280 measured reflections3 standard reflections every 120 min
1205 independent reflections intensity decay: none
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.046 w = 1/[σ2(Fo2) + (0.0566P)2P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.100(Δ/σ)max < 0.001
S = 1.01Δρmax = 1.49 e Å3
1205 reflectionsΔρmin = 0.63 e Å3
52 parametersAbsolute structure: Flack (1983)
1 restraintAbsolute structure parameter: 0.03 (4)
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
P10.3030 (3)0.6425 (3)0.4194 (4)0.0169 (5)
S10.1582 (2)0.5244 (3)0.2257 (3)0.0214 (6)
S20.1928 (3)0.6633 (3)0.6648 (4)0.0235 (6)
S30.3703 (3)0.8139 (3)0.2801 (4)0.0252 (6)
S40.50000.5068 (4)0.50000.0175 (7)
V10.00000.4975 (2)0.50000.0167 (5)
Cs10.50000.39532 (12)0.00000.0370 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
P10.0134 (11)0.0173 (14)0.0202 (11)0.0010 (9)0.0027 (9)0.0009 (10)
S10.0153 (11)0.0275 (15)0.0214 (12)0.0070 (11)0.0023 (9)0.0025 (11)
S20.0214 (12)0.0228 (15)0.0284 (12)0.0062 (10)0.0109 (10)0.0090 (11)
S30.0254 (13)0.0223 (14)0.0255 (13)0.0077 (11)0.0044 (10)0.0067 (11)
S40.0171 (15)0.0133 (18)0.0219 (16)0.0000.0015 (11)0.000
V10.0134 (10)0.0162 (13)0.0211 (11)0.0000.0048 (8)0.000
Cs10.0264 (5)0.0629 (8)0.0216 (5)0.0000.0029 (4)0.000
Geometric parameters (Å, º) top
P1—S32.008 (4)S4—Cs1iii3.5277 (13)
P1—S12.013 (3)V1—S2vi2.439 (3)
P1—S22.027 (4)V1—S3vii2.453 (3)
P1—S42.138 (3)V1—S3viii2.453 (3)
P1—Cs14.211 (3)V1—S1vi2.457 (2)
S1—V12.457 (2)Cs1—S4ix3.5277 (13)
S1—Cs13.705 (2)Cs1—S3x3.548 (3)
S1—Cs1i4.004 (3)Cs1—S3xi3.548 (3)
S2—V12.439 (3)Cs1—S1xii3.705 (2)
S2—Cs1ii3.711 (3)Cs1—S2xiii3.711 (3)
S2—Cs1iii4.108 (3)Cs1—S2viii3.711 (3)
S3—V1iv2.453 (3)Cs1—S1x4.004 (3)
S3—Cs1i3.548 (3)Cs1—S1xi4.004 (3)
S4—P1v2.138 (3)Cs1—S2v4.108 (3)
S4—Cs13.5277 (13)Cs1—S2ix4.108 (3)
S3—P1—S1110.13 (15)S4—Cs1—S153.26 (4)
S3—P1—S2120.02 (16)S4ix—Cs1—S1113.50 (5)
S1—P1—S2105.32 (14)S3x—Cs1—S165.52 (6)
S3—P1—S4109.79 (15)S3xi—Cs1—S1124.00 (6)
S1—P1—S4102.84 (15)S1xii—Cs1—S1141.26 (9)
S2—P1—S4107.33 (14)S4—Cs1—S2xiii144.98 (6)
S3—P1—Cs188.33 (12)S4ix—Cs1—S2xiii62.54 (6)
S1—P1—Cs161.64 (9)S3x—Cs1—S2xiii89.55 (6)
S2—P1—Cs1151.62 (12)S3xi—Cs1—S2xiii75.41 (6)
S4—P1—Cs156.81 (6)S1xii—Cs1—S2xiii59.95 (6)
P1—S1—V185.96 (11)S1—Cs1—S2xiii153.56 (6)
P1—S1—Cs189.81 (10)S4—Cs1—S2viii62.54 (6)
V1—S1—Cs1146.05 (10)S4ix—Cs1—S2viii144.98 (6)
P1—S1—Cs1i84.21 (11)S3x—Cs1—S2viii75.41 (6)
V1—S1—Cs1i100.51 (9)S3xi—Cs1—S2viii89.55 (6)
Cs1—S1—Cs1i112.55 (6)S1xii—Cs1—S2viii153.56 (6)
P1—S2—V186.14 (12)S1—Cs1—S2viii59.95 (6)
P1—S2—Cs1ii148.66 (13)S2xiii—Cs1—S2viii106.97 (9)
V1—S2—Cs1ii109.13 (8)S4—Cs1—S1x125.51 (7)
P1—S2—Cs1iii92.75 (11)S4ix—Cs1—S1x87.10 (6)
V1—S2—Cs1iii100.99 (9)S3x—Cs1—S1x51.32 (5)
Cs1ii—S2—Cs1iii110.11 (7)S3xi—Cs1—S1x103.88 (6)
P1—S3—V1iv115.70 (13)S1xii—Cs1—S1x112.55 (6)
P1—S3—Cs1i97.41 (11)S1—Cs1—S1x101.61 (4)
V1iv—S3—Cs1i117.51 (10)S2xiii—Cs1—S1x53.27 (5)
P1v—S4—P1105.7 (2)S2viii—Cs1—S1x63.18 (6)
P1v—S4—Cs1108.42 (7)S4—Cs1—S1xi87.10 (6)
P1—S4—Cs192.71 (7)S4ix—Cs1—S1xi125.51 (7)
P1v—S4—Cs1iii92.71 (7)S3x—Cs1—S1xi103.88 (6)
P1—S4—Cs1iii108.42 (7)S3xi—Cs1—S1xi51.32 (5)
Cs1—S4—Cs1iii144.99 (12)S1xii—Cs1—S1xi101.61 (4)
S2—V1—S2vi99.35 (16)S1—Cs1—S1xi112.55 (6)
S2—V1—S3vii163.10 (9)S2xiii—Cs1—S1xi63.18 (6)
S2vi—V1—S3vii87.99 (9)S2viii—Cs1—S1xi53.27 (5)
S2—V1—S3viii87.99 (9)S1x—Cs1—S1xi56.32 (7)
S2vi—V1—S3viii163.10 (9)S4—Cs1—S2v51.46 (5)
S3vii—V1—S3viii89.17 (14)S4ix—Cs1—S2v104.46 (6)
S2—V1—S182.00 (9)S3x—Cs1—S2v152.36 (6)
S2vi—V1—S190.23 (9)S3xi—Cs1—S2v52.07 (6)
S3vii—V1—S182.78 (9)S1xii—Cs1—S2v62.18 (5)
S3viii—V1—S1105.93 (10)S1—Cs1—S2v93.15 (5)
S2—V1—S1vi90.23 (9)S2xiii—Cs1—S2v113.26 (3)
S2vi—V1—S1vi82.00 (9)S2viii—Cs1—S2v110.11 (7)
S3vii—V1—S1vi105.93 (10)S1x—Cs1—S2v155.91 (5)
S3viii—V1—S1vi82.78 (9)S1xi—Cs1—S2v100.47 (5)
S1—V1—S1vi168.01 (17)S4—Cs1—S2ix104.46 (6)
S4—Cs1—S4ix144.99 (12)S4ix—Cs1—S2ix51.46 (5)
S4—Cs1—S3x116.79 (5)S3x—Cs1—S2ix52.07 (6)
S4ix—Cs1—S3x71.38 (5)S3xi—Cs1—S2ix152.36 (6)
S4—Cs1—S3xi71.38 (5)S1xii—Cs1—S2ix93.15 (5)
S4ix—Cs1—S3xi116.79 (5)S1—Cs1—S2ix62.18 (5)
S3x—Cs1—S3xi154.77 (9)S2xiii—Cs1—S2ix110.11 (7)
S4—Cs1—S1xii113.50 (5)S2viii—Cs1—S2ix113.26 (3)
S4ix—Cs1—S1xii53.26 (4)S1x—Cs1—S2ix100.47 (5)
S3x—Cs1—S1xii124.00 (6)S1xi—Cs1—S2ix155.91 (5)
S3xi—Cs1—S1xii65.52 (6)S2v—Cs1—S2ix103.25 (8)
Symmetry codes: (i) x1/2, y+1/2, z; (ii) x1/2, y+1/2, z+1; (iii) x, y, z+1; (iv) x+1/2, y+1/2, z; (v) x+1, y, z+1; (vi) x, y, z+1; (vii) x1/2, y1/2, z; (viii) x+1/2, y1/2, z+1; (ix) x, y, z1; (x) x+1/2, y1/2, z; (xi) x+1/2, y1/2, z; (xii) x+1, y, z; (xiii) x+1/2, y1/2, z1.
 

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