Disorder in crystals of dioxofluorotungstates, (NH₄)₂WO₂F₄ and Rb₂WO₂F₄

Dioxotetrafluorotungstates (NH₄)₂WO₂F₄ [(I) at 297 K and (II) at 133 K] and Rb₂WO₂F₄ (III) were synthesized in a single-crystal form and their structures were determined by X-ray diffraction. Two independent states of the cis-WO₂F₄ octahedron are characteristic of static and dynamic disorder in structure (I). Dynamically disordered W2 is displaced from the symmetry axis producing four possible orientations of anion that permits O and F atoms to be identified in separate orientations owing to the inherent differences between W-O and W-F bonding. After the phase transition at lower temperature (201 K), (I) transforms into the twin structure (II) with complete O/F ordering. Structure (III) is characterized by full O/F static disorder without any phase transitions at lower temperature.

Computing details

For all compounds, data collection: Bruker Smart v5.054 (Bruker, 1998); cell refinement: Bruker SAINT v6.02a (Bruker, 2000); data reduction: Bruker SAINT v6.02a (Bruker, 2000); program(s) used to solve structure: Bruker SHELXTL v5.1 (Bruker, 1998); program(s) used to refine structure: Bruker SHELXTL v5.1 (Bruker, 1998); molecular graphics: Bruker SHELXTL v5.1 (Bruker, 1998); software used to prepare material for publication: Bruker SHELXTL v5.1 (Bruker, 1998).

(I) ammonium dioxotetrafluorotungstate

Crystal data

(F4O2W)·2(H4N)	F(000) = 557
Mr = 327.93	Dx = 3.558 Mg m^−3
Orthorhombic, Cmcm	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2c 2	Cell parameters from 863 reflections
a = 5.9410 (4) Å	θ = 2.8–39.0°
b = 14.4206 (10) Å	µ = 18.77 mm^−1
c = 7.1456 (5) Å	T = 297 K
V = 612.18 (7) Å^3	Sphere, colorless
Z = 4	0.26 × 0.26 × 0.26 × 0.13 (radius) mm

Data collection

Bruker Smart 1000 CCD diffractometer	1012 independent reflections
Radiation source: fine-focus sealed tube	937 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.034
Detector resolution: 8.33 pixels mm^-1	θmax = 39.0°, θmin = 2.8°
ω scans	h = −10→9
Absorption correction: multi-scan SADABS v.2.03; Bruker 1999	k = −25→20
Tmin = 0.089, Tmax = 0.089	l = −12→12
8105 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.020	w = 1/[σ^2(Fo^2) + (0.0203P)^2 + 0.6776P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.045	(Δ/σ)max = 0.045
S = 1.13	Δρmax = 1.58 e Å^−3
1012 reflections	Δρmin = −1.52 e Å^−3
41 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0201 (3)

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	Occ. (<1)
W1	0.0000	0.10388 (3)	0.2500	0.00515 (10)	0.1431 (6)
W2	0.02077 (6)	0.109663 (14)	0.23099 (4)	0.01958 (7)	0.2142 (2)
N1	0.5000	0.27480 (19)	0.2500	0.0318 (5)
N2	0.0000	0.4420 (2)	0.2500	0.0308 (5)
F1	0.0000	0.24802 (14)	0.2500	0.0534 (7)
O1	0.0000	−0.01325 (15)	0.2500	0.0329 (5)
F2	0.22685 (19)	0.12096 (9)	0.06646 (15)	0.0364 (2)	0.75
O2	0.22685 (19)	0.12096 (9)	0.06646 (15)	0.0364 (2)	0.25

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
W1	0.0114 (2)	0.00007 (16)	0.00398 (16)	0.000	0.000	0.000
W2	0.01619 (14)	0.02899 (9)	0.01358 (13)	0.00032 (7)	0.00311 (10)	−0.00168 (6)
N1	0.0306 (11)	0.0266 (10)	0.0381 (11)	0.000	0.000	0.000
N2	0.0278 (10)	0.0334 (12)	0.0313 (10)	0.000	0.000	0.000
F1	0.0458 (12)	0.0179 (8)	0.097 (2)	0.000	0.000	0.000
O1	0.0383 (11)	0.0168 (8)	0.0435 (11)	0.000	0.000	0.000
F2	0.0265 (4)	0.0568 (6)	0.0260 (4)	−0.0044 (4)	0.0101 (3)	−0.0030 (4)
O2	0.0265 (4)	0.0568 (6)	0.0260 (4)	−0.0044 (4)	0.0101 (3)	−0.0030 (4)

Geometric parameters (Å, º)

W1—W2^i	0.2015 (4)	N1—F2^ix	3.046 (2)
W1—W2^ii	0.2015 (4)	N1—F2^x	3.046 (2)
W1—W2^iii	0.2015 (4)	N1—O1^xi	3.056 (4)
W1—O1	1.689 (2)	N2—F1	2.798 (3)
W1—O2^i	1.8966 (11)	N2—O2^xii	2.9278 (14)
W1—F2^i	1.8966 (11)	N2—O2^vii	2.9278 (14)
W1—O2^ii	1.8966 (11)	N2—F2^viii	2.9278 (14)
W1—F2^ii	1.8966 (11)	N2—O2^xiii	2.9278 (14)
W1—F1	2.079 (2)	N2—O1^xi	3.0397 (8)
W2—W2^i	0.2467 (7)	N2—O1^xiv	3.0397 (8)
W2—W2^ii	0.2717 (5)	N2—F2^xv	3.318 (3)
W2—W2^iii	0.3670 (6)	N2—F2^xvi	3.318 (3)
W2—O2	1.7052 (11)	N2—F2^xvii	3.318 (3)
W2—O1	1.782 (2)	F1—O2^i	2.6256 (19)
W2—F2^i	1.8902 (11)	F1—F2^i	2.6256 (19)
W2—F2^ii	1.9027 (11)	F1—F2	2.6256 (19)
W2—F1	2.004 (2)	F1—O2^iii	2.6256 (19)
W2—F2^iii	2.0701 (11)	O1—O2^ii	2.6986 (19)
N1—F1	2.9955 (5)	O1—F2^ii	2.6986 (19)
N1—F1^iv	2.9955 (5)	O1—O2^i	2.6986 (19)
N1—F2^v	3.0314 (18)	O1—O2^iii	2.6986 (19)
N1—F2^vi	3.0314 (18)	F2—O2^ii	2.623 (2)
N1—F2^vii	3.0314 (18)	F2—F2^ii	2.623 (2)
N1—F2^viii	3.0314 (18)	F2—O2^i	2.695 (2)
N1—F2	3.046 (2)	F2—F2^i	2.695 (2)
N1—F2^ii	3.046 (2)
O1—W1—O2^i	97.46 (4)	O1—W2—F2^ii	94.11 (4)
O1—W1—F2^i	97.46 (4)	O2^i—W2—F2^ii	165.14 (6)
O1—W1—O2^ii	97.46 (4)	F2^i—W2—F2^ii	165.14 (6)
F2^i—W1—O2^ii	165.08 (8)	F2—W2—F1	89.76 (5)
O1—W1—F2^ii	97.46 (4)	O1—W2—F1	168.84 (2)
O2^i—W1—F2^ii	165.08 (8)	O2^i—W2—F1	84.75 (4)
O1—W1—O2^iii	97.46 (4)	F2^i—W2—F1	84.75 (4)
O2^i—W1—O2^iii	87.50 (7)	O2^ii—W2—F1	84.42 (4)
F2^i—W1—O2^iii	87.50 (7)	F2^ii—W2—F1	84.42 (4)
O2^ii—W1—O2^iii	90.57 (7)	F1—W2—O2^iii	80.24 (4)
F2^ii—W1—O2^iii	90.57 (7)	F2—W2—O2^iii	169.98 (8)
O1—W1—F2^iii	97.46 (4)	O1—W2—O2^iii	88.61 (4)
O1—W1—F1	180.0	O1—W2—F2^i	94.55 (4)
O2^i—W1—F1	82.54 (4)	F2—W2—O1	101.38 (5)
F2^i—W1—F1	82.54 (4)	O2^i—W2—O2^iii	82.82 (7)
O2^ii—W1—F1	82.54 (4)	F2^i—W2—O2^iii	82.82 (7)
F2^ii—W1—F1	82.54 (4)	O2^ii—W2—O2^iii	85.34 (7)
F2—W2—O2^i	96.99 (7)	F2^ii—W2—O2^iii	85.34 (7)
O1—W2—O2^i	94.55 (4)	F2—W2—F2^iii	169.98 (8)
F2—W2—O2^ii	93.11 (8)	O1—W2—F2^iii	88.61 (4)
O1—W2—O2^ii	94.11 (4)	O2^i—W2—F2^iii	82.82 (7)
O2^i—W2—O2^ii	165.14 (6)	F2^i—W2—F2^iii	82.82 (7)
F2^i—W2—O2^ii	165.14 (6)	O2^ii—W2—F2^iii	85.34 (7)
F2—W2—F2^ii	93.11 (8)	F2^ii—W2—F2^iii	85.34 (7)

Symmetry codes: (i) −x, y, z; (ii) x, y, −z+1/2; (iii) −x, y, −z+1/2; (iv) x+1, y, z; (v) x+1/2, −y+1/2, z+1/2; (vi) x+1/2, −y+1/2, −z; (vii) −x+1/2, −y+1/2, −z; (viii) −x+1/2, −y+1/2, z+1/2; (ix) −x+1, y, z; (x) −x+1, y, −z+1/2; (xi) x+1/2, y+1/2, z; (xii) x−1/2, −y+1/2, −z; (xiii) x−1/2, −y+1/2, z+1/2; (xiv) x−1/2, y+1/2, z; (xv) −x+1/2, y+1/2, −z+1/2; (xvi) −x+1/2, y+1/2, z; (xvii) x−1/2, y+1/2, −z+1/2.

(II) ammonium dioxotetrafluorotungstate

Crystal data

(F4O2W)·2(H4N)	Z = 4
Mr = 327.93	F(000) = 592
Triclinic, P1	Dx = 3.645 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 5.9013 (4) Å	Cell parameters from 1019 reflections
b = 14.1993 (9) Å	θ = 1.4–39.4°
c = 7.7162 (5) Å	µ = 19.36 mm^−1
α = 90.022 (2)°	T = 133 K
β = 112.466 (2)°	Sphere, colorless
γ = 89.999 (2)°	0.26 × 0.26 × 0.25 × 0.13 (radius) mm
V = 597.50 (7) Å^3

Data collection

Bruker Smart 1000 CCD diffractometer	6355 independent reflections
Radiation source: fine-focus sealed tube	6066 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.035
Detector resolution: 8.33 pixels mm^-1	θmax = 39.4°, θmin = 1.4°
ω scans	h = −9→10
Absorption correction: multi-scan SADABS v.2.03; Bruker 1999	k = −25→25
Tmin = 0.086, Tmax = 0.086	l = −13→12
15611 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	H-atom parameters not defined
R[F^2 > 2σ(F^2)] = 0.039	w = 1/[σ^2(Fo^2) + (0.P)^2 + 17.957P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.092	(Δ/σ)max = 0.027
S = 1.06	Δρmax = 10.21 e Å^−3
6355 reflections	Δρmin = −7.78 e Å^−3
165 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.00027 (10)
Primary atom site location: structure-invariant direct methods

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
W1	0.62509 (3)	0.118066 (15)	0.21307 (2)	0.00468 (3)
W2	0.41301 (3)	0.382878 (15)	0.78691 (2)	0.00510 (3)
N1	0.7310 (8)	0.3639 (3)	0.4445 (6)	0.0081 (8)
N2	0.9588 (8)	0.1236 (4)	0.8872 (7)	0.0109 (8)
N3	0.2855 (8)	0.1360 (3)	0.5537 (7)	0.0081 (8)
N4	0.0741 (9)	0.3764 (4)	0.1145 (7)	0.0111 (8)
O1	0.5008 (7)	0.1123 (4)	−0.0296 (5)	0.0115 (7)
O2	0.8673 (7)	0.0355 (3)	0.2679 (6)	0.0105 (7)
O3	0.5313 (7)	0.3883 (3)	1.0289 (5)	0.0101 (6)
O4	0.5998 (6)	0.4641 (3)	0.7321 (5)	0.0082 (6)
F1	0.7293 (7)	0.1486 (3)	0.4929 (5)	0.0121 (7)
F2	0.8345 (6)	0.2233 (2)	0.2278 (5)	0.0087 (6)
F3	0.3709 (6)	0.2106 (2)	0.2138 (5)	0.0108 (6)
F4	0.4036 (6)	0.0316 (2)	0.2592 (5)	0.0118 (6)
F5	0.2371 (7)	0.3521 (3)	0.5071 (5)	0.0128 (7)
F6	0.1421 (6)	0.4678 (3)	0.7396 (5)	0.0119 (7)
F7	0.1562 (6)	0.2882 (2)	0.7857 (6)	0.0112 (7)
F8	0.6074 (6)	0.2770 (2)	0.7713 (5)	0.0095 (6)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
W1	0.00575 (5)	0.00573 (5)	0.00226 (5)	−0.00412 (6)	0.00118 (4)	−0.00104 (6)
W2	0.00601 (5)	0.00393 (5)	0.00440 (6)	0.00096 (6)	0.00091 (4)	−0.00117 (6)
N1	0.0101 (13)	0.0087 (16)	0.0063 (13)	−0.0008 (11)	0.0041 (11)	0.0001 (11)
N2	0.0106 (14)	0.0081 (16)	0.0121 (15)	0.0001 (15)	0.0022 (12)	0.0023 (15)
N3	0.0061 (13)	0.0077 (16)	0.0101 (15)	0.0009 (11)	0.0026 (11)	0.0003 (12)
N4	0.0112 (14)	0.0087 (17)	0.0124 (16)	0.0021 (15)	0.0035 (12)	0.0010 (15)
O1	0.0141 (12)	0.0160 (15)	0.0052 (11)	−0.0049 (15)	0.0045 (9)	−0.0039 (13)
O2	0.0102 (13)	0.0076 (13)	0.0136 (15)	−0.0008 (11)	0.0044 (11)	−0.0016 (12)
O3	0.0120 (12)	0.0091 (13)	0.0073 (12)	−0.0009 (13)	0.0016 (10)	−0.0041 (13)
O4	0.0091 (11)	0.0065 (12)	0.0118 (13)	0.0031 (10)	0.0071 (10)	−0.0009 (11)
F1	0.0125 (12)	0.0138 (13)	0.0077 (12)	−0.0007 (11)	0.0013 (10)	−0.0017 (11)
F2	0.0089 (10)	0.0051 (10)	0.0144 (12)	−0.0042 (9)	0.0068 (9)	−0.0026 (10)
F3	0.0116 (12)	0.0115 (13)	0.0098 (12)	0.0058 (10)	0.0045 (10)	0.0036 (10)
F4	0.0134 (11)	0.0089 (12)	0.0174 (13)	−0.0059 (10)	0.0107 (10)	−0.0034 (10)
F5	0.0168 (13)	0.0168 (14)	0.0031 (10)	−0.0015 (12)	0.0020 (10)	−0.0032 (10)
F6	0.0087 (11)	0.0093 (12)	0.0150 (14)	0.0041 (10)	0.0016 (11)	−0.0013 (11)
F7	0.0093 (11)	0.0087 (12)	0.0161 (14)	−0.0018 (10)	0.0053 (10)	0.0038 (11)
F8	0.0110 (11)	0.0051 (11)	0.0152 (13)	0.0028 (9)	0.0080 (10)	−0.0016 (10)

Geometric parameters (Å, º)

W1—O1	1.732 (3)	N3—F5	3.090 (6)
W1—O2	1.770 (4)	N3—O2^v	3.097 (6)
W1—F2	1.915 (3)	N3—F2^viii	3.136 (5)
W1—F4	1.923 (4)	N3—F1^viii	3.138 (6)
W1—F3	1.996 (4)	N4—F5	2.828 (6)
W1—F1	2.053 (4)	N4—F3	2.859 (6)
W2—O3	1.727 (4)	N4—F2^viii	2.904 (6)
W2—O4	1.755 (4)	N4—O4^iii	2.914 (6)
W2—F6	1.923 (4)	N4—F6^ix	2.981 (7)
W2—F8	1.923 (3)	N4—O3^x	3.018 (6)
W2—F7	2.024 (4)	N4—O3^ii	3.018 (7)
W2—F5	2.053 (3)	N4—F7^ii	3.030 (7)
N1—F2	2.816 (6)	N4—F8^x	3.319 (6)
N1—F5^i	2.842 (6)	N4—F6^ii	3.332 (7)
N1—O4	2.976 (6)	N4—O4^x	3.432 (6)
N1—O3^ii	2.984 (6)	N4—W2^x	3.752 (4)
N1—F6^i	3.004 (5)	O1—F3	2.676 (6)
N1—F6^iii	3.017 (6)	O1—F2	2.705 (5)
N1—F7^i	3.056 (5)	O1—O2	2.709 (5)
N1—F1	3.081 (6)	O1—F4	2.754 (6)
N1—F3	3.087 (5)	O2—F2	2.683 (5)
N1—O4^iii	3.099 (6)	O2—F1	2.708 (6)
N1—F8	3.134 (6)	O2—F4	2.712 (6)
N1—F5	3.136 (6)	O3—F7	2.696 (5)
N2—F1	2.840 (6)	O3—O4	2.697 (6)
N2—F7^i	2.852 (6)	O3—F8	2.708 (6)
N2—F8	2.903 (6)	O3—F6	2.759 (5)
N2—O2^iv	2.920 (7)	O4—F8	2.672 (5)
N2—F4^v	2.976 (6)	O4—F5	2.699 (5)
N2—O1^vi	3.011 (7)	O4—F6	2.724 (6)
N2—O1^vii	3.017 (6)	F1—F3	2.532 (5)
N2—F3^vii	3.018 (5)	F1—F2	2.583 (5)
N2—F2^vi	3.304 (7)	F1—F4	2.656 (5)
N3—F8	2.827 (5)	F2—F3	2.702 (5)
N3—F1	2.837 (6)	F3—F4	2.564 (5)
N3—O2^viii	2.971 (6)	F5—F7	2.541 (6)
N3—O1^vi	2.991 (6)	F5—F8	2.582 (5)
N3—F4	3.010 (6)	F5—F6	2.646 (6)
N3—F4^v	3.015 (6)	F6—F7	2.573 (5)
N3—F3	3.045 (7)	F7—F8	2.712 (5)
N3—F7	3.081 (6)
O1—W1—O2	101.4 (2)	O3—W2—F6	98.07 (18)
O1—W1—F2	95.62 (18)	O4—W2—F6	95.48 (17)
O2—W1—F2	93.36 (16)	O3—W2—F8	95.64 (18)
O1—W1—F4	97.64 (18)	O4—W2—F8	93.09 (17)
O2—W1—F4	94.40 (17)	F6—W2—F8	162.04 (15)
F2—W1—F4	163.00 (16)	O3—W2—F7	91.56 (18)
O1—W1—F3	91.48 (18)	O4—W2—F7	166.87 (17)
O2—W1—F3	167.00 (18)	F6—W2—F7	81.33 (15)
F2—W1—F3	87.39 (15)	F8—W2—F7	86.77 (16)
F4—W1—F3	81.69 (15)	O3—W2—F5	168.29 (18)
O1—W1—F1	168.51 (18)	O4—W2—F5	89.89 (17)
O2—W1—F1	89.88 (17)	F6—W2—F5	83.35 (16)
F2—W1—F1	81.15 (15)	F8—W2—F5	80.91 (16)
F4—W1—F1	83.76 (15)	F7—W2—F5	77.12 (16)
F3—W1—F1	77.40 (15)	O3—W2—O4	101.51 (19)

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

(III) rubidium tungsten oxide fluoride

Crystal data

(F4O2W)·2Rb	Dx = 5.059 Mg m^−3
Mr = 462.79	Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3m1	Cell parameters from 876 reflections
Hall symbol: -P 3 2"	θ = 3.9–31.4°
a = 6.0056 (3) Å	µ = 34.94 mm^−1
c = 4.8636 (5) Å	T = 297 K
V = 151.92 (2) Å^3	Plate, colorless
Z = 1	0.12 × 0.12 × 0.03 mm
F(000) = 200

Data collection

Bruker Smart 1000 CCD diffractometer	216 independent reflections
Radiation source: fine-focus sealed tube	208 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.035
Detector resolution: 8.33 pixels mm^-1	θmax = 31.4°, θmin = 3.9°
ω scans	h = −8→5
Absorption correction: integration SADABS v.2.03; Bruker 1999	k = −8→8
Tmin = 0.011, Tmax = 0.183	l = −6→7
1232 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.020	w = 1/[σ^2(Fo^2) + (0.013P)^2 + 0.656P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.047	(Δ/σ)max = 0.001
S = 1.01	Δρmax = 0.95 e Å^−3
216 reflections	Δρmin = −1.90 e Å^−3
13 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.169 (3)

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	Occ. (<1)
W	0.0000	0.0000	0.0000	0.02998 (8)
Rb	0.6667	0.3333	0.68686 (12)	0.02856 (12)
F	0.3003 (4)	0.1501 (2)	0.2177 (4)	0.0293 (5)	0.67
O	0.3003 (4)	0.1501 (2)	0.2177 (4)	0.0293 (5)	0.33

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
W	0.02882 (10)	0.02882 (10)	0.03229 (16)	0.01441 (5)	0.000	0.000
Rb	0.02559 (15)	0.02559 (15)	0.0345 (3)	0.01279 (8)	0.000	0.000
F	0.0223 (9)	0.0294 (7)	0.0339 (10)	0.0111 (5)	−0.0077 (8)	−0.0038 (4)
O	0.0223 (9)	0.0294 (7)	0.0339 (10)	0.0111 (5)	−0.0077 (8)	−0.0038 (4)

Geometric parameters (Å, º)

W—F^i	1.887 (2)	Rb—F^vi	3.0434 (4)
W—F	1.887 (2)	Rb—F^xv	3.0434 (4)
W—F^ii	1.887 (2)	Rb—F^xvi	3.0434 (4)
W—F^iii	1.887 (2)	Rb—F^xvii	3.0434 (4)
W—F^iv	1.887 (2)	Rb—F^viii	3.0434 (4)
W—F^v	1.887 (2)	Rb—O^xiv	3.0434 (4)
W—O^i	1.887 (2)	Rb—O^vi	3.0434 (4)
W—O	1.887 (2)	Rb—O^xv	3.0434 (4)
W—O^ii	1.887 (2)	Rb—O^xvi	3.0434 (4)
W—O^iii	1.887 (2)	Rb—O^xvii	3.0434 (4)
W—O^iv	1.887 (2)	Rb—O^viii	3.0434 (4)
W—O^v	1.887 (2)	Rb—F^xviii	3.209 (2)
W—Rb^vi	3.7871 (3)	Rb—F^xix	3.209 (2)
W—Rb^vii	3.7871 (3)	Rb—F^xx	3.209 (2)
W—Rb^viii	3.7871 (3)	Rb—O^xviii	3.209 (2)
W—Rb^ix	3.7871 (3)	Rb—O^xix	3.209 (2)
W—Rb^x	3.7871 (3)	Rb—O^xx	3.209 (2)
W—Rb^xi	3.7871 (3)	F—F^ii	2.631 (4)
Rb—F^xii	2.973 (2)	F—F^iv	2.631 (4)
Rb—F	2.973 (2)	F—F^iii	2.705 (4)
Rb—F^xiii	2.973 (2)	F—F^v	2.705 (4)
Rb—O^xii	2.973 (2)	F—Rb^vi	3.0434 (4)
Rb—O	2.973 (2)	F—Rb^viii	3.0434 (4)
Rb—O^xiii	2.973 (2)	F—F^xv	3.159 (4)
Rb—F^xiv	3.0434 (4)	F—F^xvii	3.159 (4)
F^i—W—F	180.00 (11)	F^ii—W—F^iv	91.59 (9)
F^i—W—F^ii	91.59 (9)	F^iii—W—F^iv	180.00 (3)
F—W—F^ii	88.41 (9)	F^i—W—F^v	88.41 (9)
F^i—W—F^iii	88.41 (9)	F—W—F^v	91.59 (9)
F—W—F^iii	91.59 (9)	F^ii—W—F^v	180.00 (12)
F^ii—W—F^iii	88.41 (9)	F^iii—W—F^v	91.59 (9)
F^i—W—F^iv	91.59 (9)	F^iv—W—F^v	88.41 (9)
F—W—F^iv	88.41 (9)

Symmetry codes: (i) −x, −y, −z; (ii) y, −x+y, −z; (iii) −x+y, −x, z; (iv) x−y, x, −z; (v) −y, x−y, z; (vi) −x+1, −y, −z+1; (vii) x−1, y, z−1; (viii) −x+1, −y+1, −z+1; (ix) x−1, y−1, z−1; (x) −x, −y, −z+1; (xi) x, y, z−1; (xii) −y+1, x−y, z; (xiii) −x+y+1, −x+1, z; (xiv) y+1, −x+y+1, −z+1; (xv) x−y, x, −z+1; (xvi) x−y+1, x, −z+1; (xvii) y, −x+y, −z+1; (xviii) −y+1, x−y, z+1; (xix) −x+y+1, −x+1, z+1; (xx) x, y, z+1.