Crystal structure of [Ag(NH₃)₃]₂[Ag(NH₃)₂]₂[SnF₆]F₂, a compound showing argentophilic inter­actions

The structure of [Ag(NH₃)₃]₂[Ag(NH₃)₂]₂[SnF₆]F₂ contains linear diammine silver(I) and T-shaped triammine silver(I) cations which show short Ag...Ag distances in the range of argentophilic inter­actions.

Key indicators

• Single-crystal X-ray study
• T = 123 K
• Mean [sigma](Ag-N) = 0.002 Å
• R factor = 0.020
• wR factor = 0.046
• Data-to-parameter ratio = 34.3

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT934_ALERT_3_B Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          4 Check

Alert level C
PLAT420_ALERT_2_C D-H Without Acceptor       N3     --  H3B    ...     Please Check
PLAT480_ALERT_4_C Long H...A H-Bond Reported H2A    ..  F3      ..       2.56 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H3A    ..  F1      ..       2.57 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H3B    ..  F3      ..       2.61 Ang.
PLAT906_ALERT_3_C Large K value in the Analysis of Variance ......      4.117 Check
PLAT976_ALERT_2_C Check Calcd Residual Density  0.56A From      N2      -0.58 eA-3
PLAT976_ALERT_2_C Check Calcd Residual Density  0.65A From      N4      -0.51 eA-3
PLAT976_ALERT_2_C Check Calcd Residual Density  0.65A From      N3      -0.48 eA-3

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:   H30 Ag4 F8 N10 Sn1
            Atom count from _chemical_formula_moiety:H30 Ag4 F8 N8 Sn1
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          1 Info
PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          3 Note
              F
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min)           1 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        320 Note

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

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   4 ALERT type 2 Indicator that the structure model may be wrong or deficient
   3 ALERT type 3 Indicator that the structure quality may be low
   5 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check

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Computing details

Data collection: CrysAlis CCD (Oxford Diffraction, 2008); cell refinement: CrysAlis RED (Oxford Diffraction, 2008); data reduction: CrysAlis RED (Oxford Diffraction, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2016 (Sheldrick, 2015) and SHELXLE (Hübschle et al., 2011); molecular graphics: DIAMOND (Brandenburg, 2012); software used to prepare material for publication: publCIF (Westrip, 2010).

Bis[triamminesilver(I)] bis[diamminesilver(I)] hexafluoridostannate(IV) difluoride

Crystal data

[Ag(NH3)3]2[Ag(NH3)2]2[SnF6]F2	F(000) = 820
Mr = 872.51	Dx = 2.815 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 7.3274 (2) Å	Cell parameters from 16653 reflections
b = 19.4495 (4) Å	θ = 2.8–39.1°
c = 7.8579 (3) Å	µ = 5.01 mm^−1
β = 113.205 (4)°	T = 123 K
V = 1029.27 (6) Å^3	Block, colorless
Z = 2	0.20 × 0.05 × 0.05 mm

Data collection

Oxford-Diffraction Xcalibur3 diffractometer	5731 independent reflections
Radiation source: Enhance (Mo) X-ray Source	4330 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.030
Detector resolution: 16.0238 pixels mm^-1	θmax = 39.2°, θmin = 3.0°
phi– and ω–rotation scans	h = −12→13
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2008)	k = −34→30
Tmin = 0.602, Tmax = 1.000	l = −13→13
30418 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.020	All H-atom parameters refined
wR(F^2) = 0.046	w = 1/[σ^2(Fo^2) + (0.0215P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.99	(Δ/σ)max = 0.002
5731 reflections	Δρmax = 1.04 e Å^−3
167 parameters	Δρmin = −0.93 e Å^−3
0 restraints	Extinction correction: SHELXL2016 (Sheldrick, 2015), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00277 (14)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
SN1	0.500000	0.000000	0.500000	0.01140 (3)
F1	0.71015 (17)	0.04893 (6)	0.45645 (18)	0.0254 (3)
F2	0.31983 (17)	0.07728 (6)	0.39037 (17)	0.0232 (2)
F3	0.58561 (19)	0.04104 (7)	0.74794 (16)	0.0274 (3)
AG1	0.16018 (2)	0.12778 (2)	0.95234 (2)	0.01661 (3)
N1	−0.1364 (2)	0.16467 (9)	0.8813 (2)	0.0179 (3)
H1A	−0.170 (4)	0.1789 (14)	0.968 (4)	0.029 (7)*
H1B	−0.171 (4)	0.2005 (14)	0.805 (4)	0.028 (7)*
H1C	−0.222 (5)	0.1286 (19)	0.805 (5)	0.070 (11)*
N2	0.4708 (2)	0.10144 (9)	1.0373 (2)	0.0175 (3)
H2A	0.509 (4)	0.0701 (13)	1.131 (3)	0.021 (6)*
H2B	0.485 (4)	0.0811 (15)	0.935 (4)	0.041 (8)*
H2C	0.557 (5)	0.1316 (16)	1.084 (4)	0.044 (9)*
N3	0.0911 (3)	0.00306 (10)	0.8291 (3)	0.0277 (4)
H3A	−0.031 (5)	−0.0050 (15)	0.751 (5)	0.046 (9)*
H3B	0.149 (5)	−0.0181 (16)	0.920 (5)	0.043 (9)*
H3C	0.133 (5)	−0.0059 (15)	0.737 (4)	0.043 (9)*
AG2	0.23394 (2)	0.22258 (2)	0.67497 (2)	0.01676 (3)
N4	0.0292 (3)	0.15407 (9)	0.4859 (2)	0.0196 (3)
H4A	0.111 (4)	0.1257 (14)	0.459 (4)	0.033 (7)*
H4B	−0.052 (4)	0.1757 (14)	0.396 (4)	0.034 (7)*
H4C	−0.034 (4)	0.1288 (15)	0.520 (4)	0.033 (8)*
N5	0.4733 (2)	0.28292 (9)	0.8539 (2)	0.0167 (3)
H5A	0.543 (4)	0.2617 (14)	0.973 (4)	0.033 (7)*
H5B	0.562 (4)	0.2883 (12)	0.793 (3)	0.020 (6)*
H5C	0.439 (5)	0.3248 (17)	0.891 (4)	0.052 (9)*
F4	0.74284 (16)	0.21290 (6)	1.16824 (14)	0.0177 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
SN1	0.01283 (6)	0.01077 (7)	0.01170 (7)	−0.00057 (5)	0.00600 (5)	−0.00041 (5)
F1	0.0194 (5)	0.0291 (7)	0.0314 (6)	−0.0056 (5)	0.0139 (5)	0.0066 (5)
F2	0.0207 (5)	0.0175 (5)	0.0319 (6)	0.0053 (4)	0.0110 (5)	0.0065 (5)
F3	0.0329 (6)	0.0314 (7)	0.0179 (5)	−0.0038 (5)	0.0098 (5)	−0.0095 (5)
AG1	0.01565 (5)	0.01867 (7)	0.01611 (6)	0.00126 (5)	0.00689 (4)	0.00184 (5)
N1	0.0179 (7)	0.0166 (7)	0.0183 (7)	0.0021 (6)	0.0061 (6)	0.0005 (6)
N2	0.0175 (6)	0.0178 (7)	0.0160 (7)	0.0000 (6)	0.0053 (5)	−0.0007 (6)
N3	0.0206 (8)	0.0236 (9)	0.0346 (10)	0.0001 (7)	0.0063 (8)	−0.0068 (8)
AG2	0.01614 (6)	0.01801 (7)	0.01510 (6)	−0.00111 (5)	0.00505 (4)	0.00066 (4)
N4	0.0184 (7)	0.0174 (8)	0.0194 (7)	−0.0010 (6)	0.0035 (6)	0.0012 (6)
N5	0.0169 (6)	0.0173 (7)	0.0161 (7)	0.0003 (5)	0.0066 (5)	0.0011 (5)
F4	0.0176 (5)	0.0200 (5)	0.0143 (5)	−0.0003 (4)	0.0051 (4)	−0.0015 (4)

Geometric parameters (Å, º)

Sn1—F1^i	1.9518 (11)	N2—H2A	0.91 (3)
Sn1—F1	1.9518 (11)	N2—H2B	0.94 (3)
Sn1—F2	1.9617 (11)	N2—H2C	0.83 (3)
Sn1—F2^i	1.9617 (11)	N3—H3A	0.88 (3)
Sn1—F3^i	1.9655 (11)	N3—H3B	0.79 (3)
Sn1—F3	1.9656 (11)	N3—H3C	0.91 (3)
Ag1—N1	2.1434 (16)	Ag2—N4	2.1160 (16)
Ag1—N2	2.1662 (16)	Ag2—N5	2.1183 (16)
Ag1—N3	2.5870 (19)	N4—H4A	0.90 (3)
Ag1—Ag2	3.0611 (2)	N4—H4B	0.84 (3)
Ag1—Ag2^ii	3.3283 (2)	N4—H4C	0.79 (3)
N1—H1A	0.85 (3)	N5—H5A	0.96 (3)
N1—H1B	0.89 (3)	N5—H5B	0.95 (3)
N1—H1C	0.98 (4)	N5—H5C	0.93 (3)
F1^i—Sn1—F1	180.0	Ag1—N2—H2A	110.8 (15)
F1^i—Sn1—F2	90.56 (5)	Ag1—N2—H2B	107.2 (17)
F1—Sn1—F2	89.44 (5)	H2A—N2—H2B	108 (2)
F1^i—Sn1—F2^i	89.44 (5)	Ag1—N2—H2C	119 (2)
F1—Sn1—F2^i	90.56 (5)	H2A—N2—H2C	100 (2)
F2—Sn1—F2^i	180.0	H2B—N2—H2C	111 (3)
F1^i—Sn1—F3^i	90.58 (6)	Ag1—N3—H3A	115 (2)
F1—Sn1—F3^i	89.42 (6)	Ag1—N3—H3B	101 (2)
F2—Sn1—F3^i	88.80 (5)	H3A—N3—H3B	126 (3)
F2^i—Sn1—F3^i	91.19 (5)	Ag1—N3—H3C	113.7 (19)
F1^i—Sn1—F3	89.42 (6)	H3A—N3—H3C	89 (3)
F1—Sn1—F3	90.58 (6)	H3B—N3—H3C	113 (3)
F2—Sn1—F3	91.19 (5)	N4—Ag2—N5	170.93 (7)
F2^i—Sn1—F3	88.81 (5)	N4—Ag2—Ag1	81.11 (5)
F3^i—Sn1—F3	180.0	N5—Ag2—Ag1	101.15 (5)
N1—Ag1—N2	173.74 (7)	N4—Ag2—Ag1^iii	104.96 (5)
N1—Ag1—N3	100.82 (6)	N5—Ag2—Ag1^iii	77.58 (4)
N2—Ag1—N3	85.44 (6)	Ag1—Ag2—Ag1^iii	149.685 (7)
N1—Ag1—Ag2	93.35 (5)	Ag2—N4—H4A	101.3 (17)
N2—Ag1—Ag2	84.44 (5)	Ag2—N4—H4B	110.4 (19)
N3—Ag1—Ag2	111.20 (6)	H4A—N4—H4B	115 (3)
N1—Ag1—Ag2^ii	77.42 (5)	Ag2—N4—H4C	120 (2)
N2—Ag1—Ag2^ii	96.40 (5)	H4A—N4—H4C	104 (3)
N3—Ag1—Ag2^ii	169.75 (6)	H4B—N4—H4C	107 (3)
Ag2—Ag1—Ag2^ii	79.041 (4)	Ag2—N5—H5A	113.0 (16)
Ag1—N1—H1A	118.6 (17)	Ag2—N5—H5B	106.2 (14)
Ag1—N1—H1B	115.3 (18)	H5A—N5—H5B	109 (2)
H1A—N1—H1B	101 (2)	Ag2—N5—H5C	115.7 (19)
Ag1—N1—H1C	105 (2)	H5A—N5—H5C	100 (2)
H1A—N1—H1C	114 (3)	H5B—N5—H5C	112 (2)
H1B—N1—H1C	102 (3)

Symmetry codes: (i) −x+1, −y, −z+1; (ii) x, −y+1/2, z+1/2; (iii) x, −y+1/2, z−1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···F4^iv	0.85 (3)	2.03 (3)	2.884 (2)	178 (2)
N1—H1B···F4^v	0.89 (3)	1.96 (3)	2.844 (2)	171 (3)
N1—H1C···F3^iv	0.98 (4)	2.14 (4)	3.057 (2)	156 (3)
N2—H2A···F1^vi	0.91 (3)	2.43 (3)	3.227 (2)	146 (2)
N2—H2A···F3^vii	0.91 (3)	2.56 (3)	3.354 (2)	145.4 (19)
N2—H2B···F3	0.94 (3)	2.04 (3)	2.961 (2)	167 (3)
N2—H2C···F4	0.83 (3)	2.02 (3)	2.849 (2)	172 (3)
N3—H3A···F1^iv	0.88 (3)	2.57 (3)	3.274 (2)	138 (3)
N3—H3A···F2^viii	0.88 (3)	2.42 (3)	3.223 (2)	153 (3)
N3—H3B···F3^vii	0.79 (3)	2.61 (3)	3.345 (3)	157 (3)
N3—H3C···F1^i	0.91 (3)	2.39 (3)	3.279 (3)	167 (3)
N4—H4A···F2	0.90 (3)	2.04 (3)	2.930 (2)	170 (2)
N4—H4B···F4^ix	0.84 (3)	1.97 (3)	2.7955 (19)	171 (3)
N4—H4C···F1^iv	0.79 (3)	2.33 (3)	3.045 (2)	151 (3)
N5—H5A···F4	0.96 (3)	1.90 (3)	2.8305 (19)	160 (3)
N5—H5B···F4^iii	0.95 (3)	1.93 (3)	2.882 (2)	173 (2)
N5—H5C···F2^ii	0.93 (3)	2.09 (3)	2.999 (2)	163 (3)

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