Syntheses, Raman spectroscopy and crystal structures of alkali hexa­fluorido­rhenates(IV) revisited

Louis-Jean, J.; Mariappan Balasekaran, S.; Smith, D.; Salamat, A.; Pham, C.T.; Poineau, F.

doi:10.1107/S2056989018005297

Syntheses, Raman spectroscopy and crystal structures of alkali hexafluoridorhenates(IV) revisited

J. Louis-Jean, S. Mariappan Balasekaran, D. Smith, A. Salamat, C. T. Pham and F. Poineau

The A₂[ReF₆] (A = K, Rb, Cs) salts are isotypic and crystallize in the K₂[GeF₆] structure type.

Keywords: rhenium; fluorine; crystal structure; Raman spectroscopy; isotypism.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989018005297/wm5432sup1.cif Contains datablocks global, global_1, global_2, SMB_K2ReF6_1, SMB_Rb2ReF6_j, SMB_Cs2ReF6_1a
	Structure factor file (CIF format) https://doi.org/10.1107/S2056989018005297/wm5432SMB_K2ReF6_1sup2.hkl Contains datablock SMB_K2ReF6_1
	Structure factor file (CIF format) https://doi.org/10.1107/S2056989018005297/wm5432SMB_Cs2ReF6_1asup3.hkl Contains datablock SMB_Cs2ReF6_1a
	Structure factor file (CIF format) https://doi.org/10.1107/S2056989018005297/wm5432SMB_Rb2ReF6_jsup4.hkl Contains datablock SMB_Rb2ReF6_j
	Structure factor file (CIF format) https://doi.org/10.1107/S2056989018005297/wm5432SMB_ReF6_fsup5.hkl Contains datablock SMB_ReF6_f
	Portable Document Format (PDF) file https://doi.org/10.1107/S2056989018005297/wm5432sup6.pdf Hexafluororhenate(IV) - revisited
	Portable Document Format (PDF) file https://doi.org/10.1107/S2056989018005297/wm5432sup7.pdf Syntheses, Raman spectroscopy and crystal structures of alkali hexafluoridorhenates(IV) - revisited

CCDC references: 1834616; 1834615; 1834614

checkCIF report

Key indicators

Structure: SMB_K2ReF6_1

Single-crystal X-ray study
T = 100 K
Mean (e-F) = 0.003 Å
R factor = 0.016
wR factor = 0.041
Data-to-parameter ratio = 15.0

Structure: SMB_Rb2ReF6_j

Single-crystal X-ray study
T = 100 K
Mean (e-F) = 0.008 Å
R factor = 0.027
wR factor = 0.074
Data-to-parameter ratio = 9.6

Structure: SMB_Cs2ReF6_1a

Single-crystal X-ray study
T = 100 K
Mean (e-F) = 0.002 Å
R factor = 0.013
wR factor = 0.036
Data-to-parameter ratio = 16.8

checkCIF/PLATON results

No syntax errors found



Datablock: SMB_K2ReF6_1



Alert level C
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  1.42A   From Re1             1.76 eA-3
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  0.74A   From Re1             1.60 eA-3

Alert level G
PLAT152_ALERT_1_G The Supplied and Calc. Volume s.u. Differ by ...          2 Units
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd  1          6.42 Check
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd  2          0.17 Check
PLAT794_ALERT_5_G Tentative Bond Valency for Re1       (IV)      .       4.13 Info
PLAT961_ALERT_5_G Dataset Contains no Negative Intensities .......     Please Check

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   2 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   5 ALERT level G = General information/check it is not something unexpected

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 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
   2 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check




Datablock: SMB_Rb2ReF6_j



Alert level C
PLAT088_ALERT_3_C Poor Data / Parameter Ratio ....................       9.58 Note
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  0.81A   From Rb1             1.78 eA-3

Alert level G
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd  1          6.42 Check
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd  2          0.17 Check
PLAT794_ALERT_5_G Tentative Bond Valency for Re1       (IV)      .       4.17 Info
PLAT909_ALERT_3_G Percentage of I>2sig(I) Data at Theta(Max) Still       100% Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   2 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   4 ALERT level G = General information/check it is not something unexpected

   0 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
   2 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check




Datablock: SMB_Cs2ReF6_1a



Alert level B
PLAT972_ALERT_2_B Check Calcd Resid. Dens.  0.63A   From Re1            -2.57 eA-3

Alert level C
PLAT021_ALERT_4_C Ratio Unique / Expected Reflections too High ...      1.019
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.99A   From Cs1            -1.86 eA-3

Alert level G
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd  1          6.42 Check
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd  2          0.17 Check
PLAT794_ALERT_5_G Tentative Bond Valency for Re1       (IV)      .       4.00 Info
PLAT961_ALERT_5_G Dataset Contains no Negative Intensities .......     Please Check

   0 ALERT level A = Most likely a serious problem - resolve or explain
   1 ALERT level B = A potentially serious problem, consider carefully
   2 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   4 ALERT level G = General information/check it is not something unexpected

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 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
   3 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check

Computing details top

For all structures, data collection: APEX3 (Bruker, 2015); cell refinement: SAINT (Bruker, 2015); data reduction: SAINT (Bruker, 2015); program(s) used to solve structure: SHELXS (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 2007); software used to prepare material for publication: publCIF (Westrip, 2010).

Dipotassium hexafluoridorhenate(IV) (SMB_K2ReF6_1) top

Crystal data top

K₂[ReF₆]	D_x = 4.689 Mg m⁻³
M_r = 378.40	Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3m1	Cell parameters from 2236 reflections
a = 5.834 (2) Å	θ = 4.0–30.5°
c = 4.546 (2) Å	µ = 24.26 mm⁻¹
V = 134.00 (11) Å³	T = 100 K
Z = 1	Hexagonal, translucent colourless
F(000) = 167	0.10 × 0.07 × 0.04 mm

Data collection top

Bruker D8 QUEST diffractometer	180 independent reflections
Radiation source: sealed tube, Siemens KFFMo2K-90	180 reflections with I > 2σ(I)
Curved graphite monochromator	R_int = 0.054
Detector resolution: 8.3333 pixels mm^-1	θ_max = 30.5°, θ_min = 4.0°
φ and ω scans	h = −8→8
Absorption correction: multi-scan (SADABS; Bruker, 2015)	k = −8→8
T_min = 0.14, T_max = 0.44	l = −6→6
2148 measured reflections

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F² > 2σ(F²)] = 0.016	Secondary atom site location: difference Fourier map
wR(F²) = 0.041	w = 1/[σ²(F_o²) + (0.0194P)² + 0.517P] where P = (F_o² + 2F_c²)/3
S = 1.13	(Δ/σ)_max < 0.001
180 reflections	Δρ_max = 1.80 e Å⁻³
12 parameters	Δρ_min = −1.37 e Å⁻³

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Re1	0	0	0	0.00863 (14)
F1	0.3254 (6)	0.1627 (3)	0.2299 (6)	0.0137 (5)
K1	0.3333	0.6667	0.2955 (4)	0.0111 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Re1	0.00883 (16)	0.00883 (16)	0.0082 (2)	0.00441 (8)	0	0
F1	0.0119 (13)	0.0162 (10)	0.0117 (12)	0.0060 (6)	−0.0012 (10)	−0.0006 (5)
K1	0.0118 (5)	0.0118 (5)	0.0096 (6)	0.0059 (2)	0	0

Geometric parameters (Å, º) top

Re1—F1	1.948 (3)	F1—K1^viii	2.9325 (10)
Re1—F1ⁱ	1.948 (3)	F1—K1^vi	2.946 (3)
Re1—F1ⁱⁱ	1.948 (3)	K1—F1^xi	2.762 (3)
Re1—F1ⁱⁱⁱ	1.948 (3)	K1—F1^x	2.762 (3)
Re1—F1^iv	1.948 (3)	K1—F1^xii	2.762 (3)
Re1—F1^v	1.948 (3)	K1—F1^xiii	2.9325 (11)
Re1—K1ⁱ	3.6263 (13)	K1—F1^xiv	2.9325 (10)
Re1—K1^vi	3.6263 (13)	K1—F1^iv	2.9325 (11)
Re1—K1^vii	3.6263 (13)	K1—F1^xv	2.9325 (11)
Re1—K1	3.6263 (13)	K1—F1^xvi	2.9325 (11)
Re1—K1^viii	3.6263 (13)	K1—F1^xvii	2.946 (3)
Re1—K1^ix	3.6263 (13)	K1—F1ⁱⁱ	2.946 (3)
F1—K1^x	2.762 (3)	K1—F1^vi	2.946 (3)
F1—K1	2.9325 (11)

F1—Re1—F1ⁱ	180.0	K1—F1—K1^viii	168.22 (13)
F1—Re1—F1ⁱⁱ	86.08 (12)	Re1—F1—K1^vi	93.38 (11)
F1ⁱ—Re1—F1ⁱⁱ	93.92 (12)	K1^x—F1—K1^vi	105.55 (10)
F1—Re1—F1ⁱⁱⁱ	93.92 (12)	K1—F1—K1^vi	94.27 (6)
F1ⁱ—Re1—F1ⁱⁱⁱ	86.08 (12)	K1^viii—F1—K1^vi	94.27 (6)
F1ⁱⁱ—Re1—F1ⁱⁱⁱ	180.00 (19)	F1^xi—K1—F1^x	65.46 (11)
F1—Re1—F1^iv	93.92 (12)	F1^xi—K1—F1^xii	65.46 (11)
F1ⁱ—Re1—F1^iv	86.08 (12)	F1^x—K1—F1^xii	65.46 (11)
F1ⁱⁱ—Re1—F1^iv	86.08 (12)	F1^xi—K1—F1^xiii	62.44 (10)
F1ⁱⁱⁱ—Re1—F1^iv	93.92 (12)	F1^x—K1—F1^xiii	127.81 (6)
F1—Re1—F1^v	86.08 (12)	F1^xii—K1—F1^xiii	95.05 (6)
F1ⁱ—Re1—F1^v	93.92 (12)	F1^xi—K1—F1^xiv	62.44 (10)
F1ⁱⁱ—Re1—F1^v	93.92 (12)	F1^x—K1—F1^xiv	95.05 (6)
F1ⁱⁱⁱ—Re1—F1^v	86.08 (12)	F1^xii—K1—F1^xiv	127.81 (6)
F1^iv—Re1—F1^v	180.00 (7)	F1^xiii—K1—F1^xiv	58.10 (11)
F1—Re1—K1ⁱ	126.206 (14)	F1^xi—K1—F1^iv	95.05 (6)
F1ⁱ—Re1—K1ⁱ	53.794 (14)	F1^x—K1—F1^iv	127.81 (6)
F1ⁱⁱ—Re1—K1ⁱ	125.81 (9)	F1^xii—K1—F1^iv	62.44 (10)
F1ⁱⁱⁱ—Re1—K1ⁱ	54.19 (9)	F1^xiii—K1—F1^iv	61.22 (12)
F1^iv—Re1—K1ⁱ	126.205 (14)	F1^xiv—K1—F1^iv	118.98 (2)
F1^v—Re1—K1ⁱ	53.795 (14)	F1^xi—K1—F1^xv	95.05 (6)
F1—Re1—K1^vi	54.19 (9)	F1^x—K1—F1^xv	62.44 (10)
F1ⁱ—Re1—K1^vi	125.81 (9)	F1^xii—K1—F1^xv	127.81 (6)
F1ⁱⁱ—Re1—K1^vi	53.794 (14)	F1^xiii—K1—F1^xv	118.98 (2)
F1ⁱⁱⁱ—Re1—K1^vi	126.206 (14)	F1^xiv—K1—F1^xv	61.22 (12)
F1^iv—Re1—K1^vi	126.205 (14)	F1^iv—K1—F1^xv	168.22 (13)
F1^v—Re1—K1^vi	53.795 (14)	F1^xi—K1—F1^xvi	127.81 (6)
K1ⁱ—Re1—K1^vi	107.11 (3)	F1^x—K1—F1^xvi	62.44 (10)
F1—Re1—K1^vii	125.81 (9)	F1^xii—K1—F1^xvi	95.05 (6)
F1ⁱ—Re1—K1^vii	54.19 (9)	F1^xiii—K1—F1^xvi	168.22 (13)
F1ⁱⁱ—Re1—K1^vii	126.206 (14)	F1^xiv—K1—F1^xvi	118.98 (2)
F1ⁱⁱⁱ—Re1—K1^vii	53.794 (14)	F1^iv—K1—F1^xvi	118.98 (2)
F1^iv—Re1—K1^vii	53.795 (14)	F1^xv—K1—F1^xvi	58.10 (11)
F1^v—Re1—K1^vii	126.205 (14)	F1^xi—K1—F1	127.81 (6)
K1ⁱ—Re1—K1^vii	72.89 (3)	F1^x—K1—F1	95.05 (6)
K1^vi—Re1—K1^vii	180.0	F1^xii—K1—F1	62.44 (10)
F1—Re1—K1	53.794 (14)	F1^xiii—K1—F1	118.98 (2)
F1ⁱ—Re1—K1	126.206 (14)	F1^xiv—K1—F1	168.22 (13)
F1ⁱⁱ—Re1—K1	54.19 (9)	F1^iv—K1—F1	58.09 (11)
F1ⁱⁱⁱ—Re1—K1	125.81 (9)	F1^xv—K1—F1	118.98 (2)
F1^iv—Re1—K1	53.794 (14)	F1^xvi—K1—F1	61.22 (11)
F1^v—Re1—K1	126.206 (14)	F1^xi—K1—F1^xvii	105.55 (10)
K1ⁱ—Re1—K1	180.0	F1^x—K1—F1^xvii	144.70 (4)
K1^vi—Re1—K1	72.89 (3)	F1^xii—K1—F1^xvii	144.70 (4)
K1^vii—Re1—K1	107.11 (3)	F1^xiii—K1—F1^xvii	53.80 (10)
F1—Re1—K1^viii	53.795 (14)	F1^xiv—K1—F1^xvii	53.80 (10)
F1ⁱ—Re1—K1^viii	126.205 (14)	F1^iv—K1—F1^xvii	85.73 (6)
F1ⁱⁱ—Re1—K1^viii	126.206 (14)	F1^xv—K1—F1^xvii	85.73 (6)
F1ⁱⁱⁱ—Re1—K1^viii	53.794 (14)	F1^xvi—K1—F1^xvii	114.69 (6)
F1^iv—Re1—K1^viii	125.81 (9)	F1—K1—F1^xvii	114.69 (6)
F1^v—Re1—K1^viii	54.19 (9)	F1^xi—K1—F1ⁱⁱ	144.70 (4)
K1ⁱ—Re1—K1^viii	72.90 (3)	F1^x—K1—F1ⁱⁱ	144.70 (4)
K1^vi—Re1—K1^viii	72.90 (3)	F1^xii—K1—F1ⁱⁱ	105.55 (10)
K1^vii—Re1—K1^viii	107.10 (3)	F1^xiii—K1—F1ⁱⁱ	85.73 (6)
K1—Re1—K1^viii	107.10 (3)	F1^xiv—K1—F1ⁱⁱ	114.69 (6)
F1—Re1—K1^ix	126.205 (14)	F1^iv—K1—F1ⁱⁱ	53.80 (10)
F1ⁱ—Re1—K1^ix	53.795 (14)	F1^xv—K1—F1ⁱⁱ	114.69 (6)
F1ⁱⁱ—Re1—K1^ix	53.794 (14)	F1^xvi—K1—F1ⁱⁱ	85.73 (6)
F1ⁱⁱⁱ—Re1—K1^ix	126.206 (14)	F1—K1—F1ⁱⁱ	53.80 (10)
F1^iv—Re1—K1^ix	54.19 (9)	F1^xvii—K1—F1ⁱⁱ	60.91 (10)
F1^v—Re1—K1^ix	125.81 (9)	F1^xi—K1—F1^vi	144.70 (4)
K1ⁱ—Re1—K1^ix	107.10 (3)	F1^x—K1—F1^vi	105.55 (10)
K1^vi—Re1—K1^ix	107.10 (3)	F1^xii—K1—F1^vi	144.70 (4)
K1^vii—Re1—K1^ix	72.90 (3)	F1^xiii—K1—F1^vi	114.69 (6)
K1—Re1—K1^ix	72.90 (3)	F1^xiv—K1—F1^vi	85.73 (6)
K1^viii—Re1—K1^ix	180.0	F1^iv—K1—F1^vi	114.69 (6)
Re1—F1—K1^x	161.08 (14)	F1^xv—K1—F1^vi	53.80 (10)
Re1—F1—K1	93.79 (6)	F1^xvi—K1—F1^vi	53.80 (10)
K1^x—F1—K1	84.95 (6)	F1—K1—F1^vi	85.73 (6)
Re1—F1—K1^viii	93.79 (6)	F1^xvii—K1—F1^vi	60.91 (10)
K1^x—F1—K1^viii	84.95 (6)	F1ⁱⁱ—K1—F1^vi	60.91 (10)

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

Dirubidium hexafluoridorhenate(IV) (SMB_Rb2ReF6_j) top

Crystal data top

Rb₂[ReF₆]	D_x = 5.332 Mg m⁻³
M_r = 471.14	Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3m1	Cell parameters from 1612 reflections
a = 5.9926 (13) Å	θ = 3.9–28.3°
c = 4.7177 (10) Å	µ = 37.22 mm⁻¹
V = 146.72 (7) Å³	T = 100 K
Z = 1	Hexagonal plate, translucent colourless
F(000) = 203	0.08 × 0.07 × 0.04 mm

Data collection top

Bruker D8 QUEST diffractometer	115 independent reflections
Radiation source: sealed tube, Siemens KFFMo2K-90	111 reflections with I > 2σ(I)
Curved graphite monochromator	R_int = 0.073
Detector resolution: 8.3333 pixels mm^-1	θ_max = 24.9°, θ_min = 3.9°
φ and ω scans	h = −7→7
Absorption correction: numerical (SADABS; Bruker, 2015)	k = −7→7
T_min = 0.11, T_max = 0.30	l = −5→5
1526 measured reflections

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	Primary atom site location: heavy-atom method
R[F² > 2σ(F²)] = 0.027	Secondary atom site location: difference Fourier map
wR(F²) = 0.074	w = 1/[σ²(F_o²) + (0.0175P)² + 3.5548P] where P = (F_o² + 2F_c²)/3
S = 1.30	(Δ/σ)_max < 0.001
115 reflections	Δρ_max = 1.91 e Å⁻³
12 parameters	Δρ_min = −1.36 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Re1	0	0	0	0.0157 (5)
F1	0.3151 (14)	0.1576 (7)	0.2231 (15)	0.0151 (17)
Rb1	0.3333	0.6667	0.2971 (4)	0.0138 (6)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Re1	0.0133 (6)	0.0133 (6)	0.0205 (8)	0.0066 (3)	0	0
F1	0.015 (4)	0.017 (3)	0.012 (3)	0.0077 (19)	0.001 (3)	0.0007 (14)
Rb1	0.0131 (8)	0.0131 (8)	0.0152 (12)	0.0065 (4)	0	0

Geometric parameters (Å, º) top

Re1—F1ⁱ	1.945 (7)	F1—Rb1^viii	3.0181 (11)
Re1—F1ⁱⁱ	1.945 (7)	F1—Rb1^vi	3.058 (7)
Re1—F1ⁱⁱⁱ	1.945 (7)	Rb1—F1^xi	2.907 (7)
Re1—F1^iv	1.945 (7)	Rb1—F1^x	2.907 (7)
Re1—F1^v	1.945 (7)	Rb1—F1^xii	2.907 (7)
Re1—F1	1.945 (7)	Rb1—F1^xiii	3.0181 (11)
Re1—Rb1ⁱ	3.7330 (10)	Rb1—F1^xiv	3.0181 (11)
Re1—Rb1^vi	3.7330 (11)	Rb1—F1^v	3.0181 (11)
Re1—Rb1^vii	3.7330 (11)	Rb1—F1^xv	3.0181 (11)
Re1—Rb1	3.7330 (10)	Rb1—F1^xvi	3.0181 (11)
Re1—Rb1^viii	3.7330 (11)	Rb1—F1^xvii	3.058 (7)
Re1—Rb1^ix	3.7330 (11)	Rb1—F1ⁱⁱ	3.058 (7)
F1—Rb1^x	2.907 (7)	Rb1—F1^vi	3.058 (7)
F1—Rb1	3.0181 (11)

F1ⁱ—Re1—F1ⁱⁱ	93.5 (3)	Rb1—F1—Rb1^viii	166.2 (3)
F1ⁱ—Re1—F1ⁱⁱⁱ	86.5 (3)	Re1—F1—Rb1^vi	93.9 (2)
F1ⁱⁱ—Re1—F1ⁱⁱⁱ	180.0 (3)	Rb1^x—F1—Rb1^vi	104.5 (2)
F1ⁱ—Re1—F1^iv	93.5 (3)	Rb1—F1—Rb1^vi	94.26 (14)
F1ⁱⁱ—Re1—F1^iv	93.5 (3)	Rb1^viii—F1—Rb1^vi	94.26 (14)
F1ⁱⁱⁱ—Re1—F1^iv	86.5 (3)	F1^xi—Rb1—F1^x	65.8 (2)
F1ⁱ—Re1—F1^v	86.5 (3)	F1^xi—Rb1—F1^xii	65.8 (2)
F1ⁱⁱ—Re1—F1^v	86.5 (3)	F1^x—Rb1—F1^xii	65.8 (2)
F1ⁱⁱⁱ—Re1—F1^v	93.5 (3)	F1^xi—Rb1—F1^xiii	62.7 (2)
F1^iv—Re1—F1^v	180.0	F1^x—Rb1—F1^xiii	128.31 (8)
F1ⁱ—Re1—F1	180.0	F1^xii—Rb1—F1^xiii	96.30 (14)
F1ⁱⁱ—Re1—F1	86.5 (3)	F1^xi—Rb1—F1^xiv	62.7 (2)
F1ⁱⁱⁱ—Re1—F1	93.5 (3)	F1^x—Rb1—F1^xiv	96.30 (14)
F1^iv—Re1—F1	86.5 (3)	F1^xii—Rb1—F1^xiv	128.31 (8)
F1^v—Re1—F1	93.5 (3)	F1^xiii—Rb1—F1^xiv	56.0 (3)
F1ⁱ—Re1—Rb1ⁱ	53.64 (2)	F1^xi—Rb1—F1^v	96.30 (14)
F1ⁱⁱ—Re1—Rb1ⁱ	125.2 (2)	F1^x—Rb1—F1^v	128.31 (8)
F1ⁱⁱⁱ—Re1—Rb1ⁱ	54.8 (2)	F1^xii—Rb1—F1^v	62.7 (2)
F1^iv—Re1—Rb1ⁱ	53.64 (2)	F1^xiii—Rb1—F1^v	63.1 (3)
F1^v—Re1—Rb1ⁱ	126.36 (2)	F1^xiv—Rb1—F1^v	118.68 (6)
F1—Re1—Rb1ⁱ	126.36 (2)	F1^xi—Rb1—F1^xv	96.30 (14)
F1ⁱ—Re1—Rb1^vi	125.2 (2)	F1^x—Rb1—F1^xv	62.7 (2)
F1ⁱⁱ—Re1—Rb1^vi	53.64 (2)	F1^xii—Rb1—F1^xv	128.31 (8)
F1ⁱⁱⁱ—Re1—Rb1^vi	126.36 (2)	F1^xiii—Rb1—F1^xv	118.68 (5)
F1^iv—Re1—Rb1^vi	53.64 (2)	F1^xiv—Rb1—F1^xv	63.1 (3)
F1^v—Re1—Rb1^vi	126.36 (2)	F1^v—Rb1—F1^xv	166.2 (3)
F1—Re1—Rb1^vi	54.8 (2)	F1^xi—Rb1—F1^xvi	128.31 (8)
Rb1ⁱ—Re1—Rb1^vi	106.77 (3)	F1^x—Rb1—F1^xvi	62.7 (2)
F1ⁱ—Re1—Rb1^vii	54.8 (2)	F1^xii—Rb1—F1^xvi	96.30 (14)
F1ⁱⁱ—Re1—Rb1^vii	126.36 (2)	F1^xiii—Rb1—F1^xvi	166.2 (3)
F1ⁱⁱⁱ—Re1—Rb1^vii	53.64 (2)	F1^xiv—Rb1—F1^xvi	118.68 (6)
F1^iv—Re1—Rb1^vii	126.36 (2)	F1^v—Rb1—F1^xvi	118.68 (5)
F1^v—Re1—Rb1^vii	53.64 (2)	F1^xv—Rb1—F1^xvi	56.0 (3)
F1—Re1—Rb1^vii	125.2 (2)	F1^xi—Rb1—F1	128.31 (8)
Rb1ⁱ—Re1—Rb1^vii	73.23 (3)	F1^x—Rb1—F1	96.30 (14)
Rb1^vi—Re1—Rb1^vii	180.0	F1^xii—Rb1—F1	62.7 (2)
F1ⁱ—Re1—Rb1	126.36 (2)	F1^xiii—Rb1—F1	118.68 (6)
F1ⁱⁱ—Re1—Rb1	54.8 (2)	F1^xiv—Rb1—F1	166.2 (3)
F1ⁱⁱⁱ—Re1—Rb1	125.2 (2)	F1^v—Rb1—F1	56.0 (3)
F1^iv—Re1—Rb1	126.36 (2)	F1^xv—Rb1—F1	118.68 (5)
F1^v—Re1—Rb1	53.64 (2)	F1^xvi—Rb1—F1	63.1 (3)
F1—Re1—Rb1	53.64 (2)	F1^xi—Rb1—F1^xvii	104.5 (2)
Rb1ⁱ—Re1—Rb1	180.0	F1^x—Rb1—F1^xvii	144.30 (9)
Rb1^vi—Re1—Rb1	73.23 (3)	F1^xii—Rb1—F1^xvii	144.30 (9)
Rb1^vii—Re1—Rb1	106.77 (3)	F1^xiii—Rb1—F1^xvii	52.0 (2)
F1ⁱ—Re1—Rb1^viii	126.36 (2)	F1^xiv—Rb1—F1^xvii	52.0 (2)
F1ⁱⁱ—Re1—Rb1^viii	126.36 (2)	F1^v—Rb1—F1^xvii	85.74 (14)
F1ⁱⁱⁱ—Re1—Rb1^viii	53.64 (2)	F1^xv—Rb1—F1^xvii	85.74 (14)
F1^iv—Re1—Rb1^viii	54.8 (2)	F1^xvi—Rb1—F1^xvii	114.25 (9)
F1^v—Re1—Rb1^viii	125.2 (2)	F1—Rb1—F1^xvii	114.25 (9)
F1—Re1—Rb1^viii	53.64 (2)	F1^xi—Rb1—F1ⁱⁱ	144.30 (9)
Rb1ⁱ—Re1—Rb1^viii	73.23 (3)	F1^x—Rb1—F1ⁱⁱ	144.30 (9)
Rb1^vi—Re1—Rb1^viii	73.23 (3)	F1^xii—Rb1—F1ⁱⁱ	104.5 (2)
Rb1^vii—Re1—Rb1^viii	106.77 (3)	F1^xiii—Rb1—F1ⁱⁱ	85.74 (14)
Rb1—Re1—Rb1^viii	106.77 (3)	F1^xiv—Rb1—F1ⁱⁱ	114.25 (9)
F1ⁱ—Re1—Rb1^ix	53.64 (2)	F1^v—Rb1—F1ⁱⁱ	52.0 (2)
F1ⁱⁱ—Re1—Rb1^ix	53.64 (2)	F1^xv—Rb1—F1ⁱⁱ	114.25 (9)
F1ⁱⁱⁱ—Re1—Rb1^ix	126.36 (2)	F1^xvi—Rb1—F1ⁱⁱ	85.74 (14)
F1^iv—Re1—Rb1^ix	125.2 (2)	F1—Rb1—F1ⁱⁱ	52.0 (2)
F1^v—Re1—Rb1^ix	54.8 (2)	F1^xvii—Rb1—F1ⁱⁱ	62.2 (2)
F1—Re1—Rb1^ix	126.36 (2)	F1^xi—Rb1—F1^vi	144.30 (9)
Rb1ⁱ—Re1—Rb1^ix	106.77 (3)	F1^x—Rb1—F1^vi	104.5 (2)
Rb1^vi—Re1—Rb1^ix	106.77 (3)	F1^xii—Rb1—F1^vi	144.30 (9)
Rb1^vii—Re1—Rb1^ix	73.23 (3)	F1^xiii—Rb1—F1^vi	114.25 (9)
Rb1—Re1—Rb1^ix	73.23 (3)	F1^xiv—Rb1—F1^vi	85.74 (14)
Rb1^viii—Re1—Rb1^ix	180.0	F1^v—Rb1—F1^vi	114.25 (9)
Re1—F1—Rb1^x	161.6 (3)	F1^xv—Rb1—F1^vi	52.0 (2)
Re1—F1—Rb1	95.10 (14)	F1^xvi—Rb1—F1^vi	52.0 (2)
Rb1^x—F1—Rb1	83.70 (14)	F1—Rb1—F1^vi	85.74 (14)
Re1—F1—Rb1^viii	95.10 (14)	F1^xvii—Rb1—F1^vi	62.2 (2)
Rb1^x—F1—Rb1^viii	83.70 (14)	F1ⁱⁱ—Rb1—F1^vi	62.2 (2)

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

Dicaesium hexafluoridorhenate(IV) (SMB_Cs2ReF6_1a) top

Crystal data top

Cs₂[ReF₆]	D_x = 5.602 Mg m⁻³
M_r = 566.02	Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3m1	Cell parameters from 135 reflections
a = 6.268 (1) Å	θ = 3.8–32.6°
c = 4.931 (1) Å	µ = 28.83 mm⁻¹
V = 167.77 (6) Å³	T = 100 K
Z = 1	Hexagonal plate, clear colourless
F(000) = 239	0.25 × 0.12 × 0.11 mm

Data collection top

Bruker D8 QUEST diffractometer	218 independent reflections
Radiation source: sealed tube, Siemens KFFMo2K-90	218 reflections with I > 2σ(I)
Curved graphite monochromator	R_int = 0.040
Detector resolution: 8.3333 pixels mm^-1	θ_max = 30.4°, θ_min = 3.8°
φ and ω scans	h = −8→8
Absorption correction: multi-scan (SADABS; Bruker, 2015)	k = −8→8
T_min = 0.05, T_max = 0.15	l = −7→7
2683 measured reflections

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)] = 0.013	w = 1/[σ²(F_o²) + (0.0181P)² + 0.1419P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.036	(Δ/σ)_max < 0.001
S = 1.25	Δρ_max = 0.68 e Å⁻³
218 reflections	Δρ_min = −2.92 e Å⁻³
13 parameters	Extinction correction: SHELXL2014 (Sheldrick, 2015)
0 restraints	Extinction coefficient: 0.029 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Re1	0	0	0	0.00427 (15)
F1	0.3027 (3)	0.15135 (17)	0.2165 (4)	0.0092 (4)
Cs1	0.3333	0.6667	0.30027 (9)	0.00615 (14)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Re1	0.00483 (16)	0.00483 (16)	0.0032 (2)	0.00241 (8)	0	0
F1	0.0088 (8)	0.0107 (6)	0.0075 (9)	0.0044 (4)	−0.0023 (6)	−0.0012 (3)
Cs1	0.00661 (16)	0.00661 (16)	0.0052 (2)	0.00331 (8)	0	0

Geometric parameters (Å, º) top

Re1—F1ⁱ	1.9594 (18)	F1—Cs1^viii	3.1655 (6)
Re1—F1ⁱⁱ	1.9594 (18)	F1—Cs1^vi	3.224 (2)
Re1—F1ⁱⁱⁱ	1.9594 (18)	Cs1—F1^xi	3.0955 (19)
Re1—F1^iv	1.9594 (18)	Cs1—F1^x	3.0955 (19)
Re1—F1^v	1.9594 (18)	Cs1—F1^xii	3.0955 (19)
Re1—F1	1.9594 (18)	Cs1—F1^xiii	3.1655 (6)
Re1—Cs1ⁱ	3.9100 (6)	Cs1—F1^xiv	3.1655 (6)
Re1—Cs1^vi	3.9100 (6)	Cs1—F1ⁱⁱⁱ	3.1655 (6)
Re1—Cs1^vii	3.9100 (6)	Cs1—F1^xv	3.1655 (6)
Re1—Cs1	3.9100 (6)	Cs1—F1^xvi	3.1655 (6)
Re1—Cs1^viii	3.9100 (6)	Cs1—F1^xvii	3.224 (2)
Re1—Cs1^ix	3.9100 (6)	Cs1—F1^iv	3.224 (2)
F1—Cs1^x	3.0955 (19)	Cs1—F1^vi	3.224 (2)
F1—Cs1	3.1655 (6)

F1ⁱ—Re1—F1ⁱⁱ	93.14 (7)	Cs1—F1—Cs1^viii	163.82 (6)
F1ⁱ—Re1—F1ⁱⁱⁱ	86.86 (7)	Re1—F1—Cs1^vi	94.78 (7)
F1ⁱⁱ—Re1—F1ⁱⁱⁱ	180.00 (4)	Cs1^x—F1—Cs1^vi	102.55 (5)
F1ⁱ—Re1—F1^iv	93.14 (7)	Cs1—F1—Cs1^vi	94.07 (3)
F1ⁱⁱ—Re1—F1^iv	93.14 (7)	Cs1^viii—F1—Cs1^vi	94.07 (3)
F1ⁱⁱⁱ—Re1—F1^iv	86.86 (7)	F1^xi—Cs1—F1^x	67.11 (6)
F1ⁱ—Re1—F1^v	86.86 (7)	F1^xi—Cs1—F1^xii	67.11 (6)
F1ⁱⁱ—Re1—F1^v	86.86 (7)	F1^x—Cs1—F1^xii	67.11 (6)
F1ⁱⁱⁱ—Re1—F1^v	93.14 (7)	F1^xi—Cs1—F1^xiii	62.38 (6)
F1^iv—Re1—F1^v	180.00 (8)	F1^x—Cs1—F1^xiii	129.122 (17)
F1ⁱ—Re1—F1	180.0	F1^xii—Cs1—F1^xiii	97.70 (3)
F1ⁱⁱ—Re1—F1	86.86 (7)	F1^xi—Cs1—F1^xiv	62.38 (6)
F1ⁱⁱⁱ—Re1—F1	93.14 (7)	F1^x—Cs1—F1^xiv	97.70 (3)
F1^iv—Re1—F1	86.86 (7)	F1^xii—Cs1—F1^xiv	129.122 (17)
F1^v—Re1—F1	93.14 (7)	F1^xiii—Cs1—F1^xiv	53.43 (7)
F1ⁱ—Re1—Cs1ⁱ	53.533 (6)	F1^xi—Cs1—F1ⁱⁱⁱ	97.70 (3)
F1ⁱⁱ—Re1—Cs1ⁱ	53.533 (6)	F1^x—Cs1—F1ⁱⁱⁱ	129.122 (17)
F1ⁱⁱⁱ—Re1—Cs1ⁱ	126.467 (6)	F1^xii—Cs1—F1ⁱⁱⁱ	62.38 (6)
F1^iv—Re1—Cs1ⁱ	124.74 (6)	F1^xiii—Cs1—F1ⁱⁱⁱ	65.44 (7)
F1^v—Re1—Cs1ⁱ	55.26 (6)	F1^xiv—Cs1—F1ⁱⁱⁱ	118.323 (15)
F1—Re1—Cs1ⁱ	126.467 (6)	F1^xi—Cs1—F1^xv	97.70 (3)
F1ⁱ—Re1—Cs1^vi	124.74 (6)	F1^x—Cs1—F1^xv	62.38 (6)
F1ⁱⁱ—Re1—Cs1^vi	53.533 (6)	F1^xii—Cs1—F1^xv	129.122 (17)
F1ⁱⁱⁱ—Re1—Cs1^vi	126.467 (6)	F1^xiii—Cs1—F1^xv	118.323 (14)
F1^iv—Re1—Cs1^vi	53.532 (6)	F1^xiv—Cs1—F1^xv	65.44 (7)
F1^v—Re1—Cs1^vi	126.468 (6)	F1ⁱⁱⁱ—Cs1—F1^xv	163.82 (6)
F1—Re1—Cs1^vi	55.26 (6)	F1^xi—Cs1—F1	129.123 (17)
Cs1ⁱ—Re1—Cs1^vi	106.554 (9)	F1^x—Cs1—F1	97.70 (3)
F1ⁱ—Re1—Cs1^vii	55.26 (6)	F1^xii—Cs1—F1	62.38 (6)
F1ⁱⁱ—Re1—Cs1^vii	126.467 (6)	F1^xiii—Cs1—F1	118.323 (15)
F1ⁱⁱⁱ—Re1—Cs1^vii	53.533 (6)	F1^xiv—Cs1—F1	163.82 (6)
F1^iv—Re1—Cs1^vii	126.468 (6)	F1ⁱⁱⁱ—Cs1—F1	53.43 (7)
F1^v—Re1—Cs1^vii	53.532 (6)	F1^xv—Cs1—F1	118.323 (15)
F1—Re1—Cs1^vii	124.74 (6)	F1^xi—Cs1—F1^xvi	129.122 (17)
Cs1ⁱ—Re1—Cs1^vii	73.446 (9)	F1^x—Cs1—F1^xvi	62.38 (6)
Cs1^vi—Re1—Cs1^vii	180.0	F1^xii—Cs1—F1^xvi	97.70 (3)
F1ⁱ—Re1—Cs1	126.467 (6)	F1^xiii—Cs1—F1^xvi	163.82 (6)
F1ⁱⁱ—Re1—Cs1	126.467 (6)	F1^xiv—Cs1—F1^xvi	118.323 (15)
F1ⁱⁱⁱ—Re1—Cs1	53.533 (6)	F1ⁱⁱⁱ—Cs1—F1^xvi	118.323 (15)
F1^iv—Re1—Cs1	55.26 (6)	F1^xv—Cs1—F1^xvi	53.43 (7)
F1^v—Re1—Cs1	124.74 (6)	F1—Cs1—F1^xvi	65.44 (7)
F1—Re1—Cs1	53.533 (6)	F1^xi—Cs1—F1^xvii	102.55 (5)
Cs1ⁱ—Re1—Cs1	180.0	F1^x—Cs1—F1^xvii	143.51 (2)
Cs1^vi—Re1—Cs1	73.447 (8)	F1^xii—Cs1—F1^xvii	143.51 (2)
Cs1^vii—Re1—Cs1	106.553 (8)	F1^xiii—Cs1—F1^xvii	49.86 (5)
F1ⁱ—Re1—Cs1^viii	126.467 (6)	F1^xiv—Cs1—F1^xvii	49.86 (5)
F1ⁱⁱ—Re1—Cs1^viii	55.26 (6)	F1ⁱⁱⁱ—Cs1—F1^xvii	85.93 (3)
F1ⁱⁱⁱ—Re1—Cs1^viii	124.74 (6)	F1^xv—Cs1—F1^xvii	85.93 (3)
F1^iv—Re1—Cs1^viii	126.467 (6)	F1—Cs1—F1^xvii	113.96 (2)
F1^v—Re1—Cs1^viii	53.533 (6)	F1^xvi—Cs1—F1^xvii	113.96 (2)
F1—Re1—Cs1^viii	53.533 (6)	F1^xi—Cs1—F1^iv	143.51 (2)
Cs1ⁱ—Re1—Cs1^viii	73.447 (8)	F1^x—Cs1—F1^iv	143.51 (2)
Cs1^vi—Re1—Cs1^viii	73.447 (9)	F1^xii—Cs1—F1^iv	102.55 (5)
Cs1^vii—Re1—Cs1^viii	106.553 (9)	F1^xiii—Cs1—F1^iv	85.93 (3)
Cs1—Re1—Cs1^viii	106.553 (9)	F1^xiv—Cs1—F1^iv	113.96 (2)
F1ⁱ—Re1—Cs1^ix	53.533 (6)	F1ⁱⁱⁱ—Cs1—F1^iv	49.86 (5)
F1ⁱⁱ—Re1—Cs1^ix	124.74 (6)	F1^xv—Cs1—F1^iv	113.96 (2)
F1ⁱⁱⁱ—Re1—Cs1^ix	55.26 (6)	F1—Cs1—F1^iv	49.86 (5)
F1^iv—Re1—Cs1^ix	53.533 (6)	F1^xvi—Cs1—F1^iv	85.93 (3)
F1^v—Re1—Cs1^ix	126.467 (6)	F1^xvii—Cs1—F1^iv	64.10 (5)
F1—Re1—Cs1^ix	126.467 (6)	F1^xi—Cs1—F1^vi	143.51 (2)
Cs1ⁱ—Re1—Cs1^ix	106.553 (8)	F1^x—Cs1—F1^vi	102.55 (5)
Cs1^vi—Re1—Cs1^ix	106.553 (9)	F1^xii—Cs1—F1^vi	143.51 (2)
Cs1^vii—Re1—Cs1^ix	73.447 (9)	F1^xiii—Cs1—F1^vi	113.96 (2)
Cs1—Re1—Cs1^ix	73.447 (9)	F1^xiv—Cs1—F1^vi	85.93 (3)
Cs1^viii—Re1—Cs1^ix	180.0	F1ⁱⁱⁱ—Cs1—F1^vi	113.96 (2)
Re1—F1—Cs1^x	162.67 (9)	F1^xv—Cs1—F1^vi	49.86 (5)
Re1—F1—Cs1	96.61 (3)	F1—Cs1—F1^vi	85.93 (3)
Cs1^x—F1—Cs1	82.30 (3)	F1^xvi—Cs1—F1^vi	49.86 (5)
Re1—F1—Cs1^viii	96.61 (3)	F1^xvii—Cs1—F1^vi	64.10 (5)
Cs1^x—F1—Cs1^viii	82.30 (3)	F1^iv—Cs1—F1^vi	64.10 (5)

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

Structural details (Å, °) of the [ReF₆]^2- anion in this study and of the related anion in [TcF₆]^2- salts^a top

	M—F, M = Re	F—M—F, M = Re	M—F, M = Tc	F—M—F, M = Tc
K₂[MF₆]	1.948 (3)	86.08 (12), 93.92 (12), 180	1.928 (6)	86.93 (5), 93.07 (5), 180
Rb₂[MF₆]	1.945 (7)	86.5 (3), 93.5 (3), 180	1.933 (3)	87.2 (2), 92.8 (2), 180
Cs₂[MF₆]	1.9594 (18)	86.86 (7), 93.14 (7), 180	1.935 (5)	87.8 (2), 92.2 (2), 180

Note: (a) Balasekaran et al. (2013).

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Syntheses, Raman spectroscopy and crystal structures of alkali hexa­fluorido­rhenates(IV) revisited

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Syntheses, Raman spectroscopy and crystal structures of alkali hexafluoridorhenates(IV) revisited