catena-Poly­[[silver(I)-μ-1,4-di­amino­butane-κ²N:N′] hexa­fluoro­arsenate]

The title compound, {[Ag(C₄H₁₂N₂)](AsF₆)}_n, is a helical one-dimensional chain Ag^I complex. The Ag^I atom is coordinated by two N atoms from two 1,4-di­amino­butane ligands, in a nearly linear geometry. The crystal structure is a three-dimensional structure stabilized by N—H...F hydrogen bonds and weak Ag...F interactions.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.009 Å
• R factor = 0.042
• wR factor = 0.117
• Data-to-parameter ratio = 15.0

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low .......       0.94
PLAT242_ALERT_2_A Check Low    U(eq) as Compared to Neighbors ....        As1

Alert level C
WEIGH01_ALERT_1_C  Extra text has been found in the
            _refine_ls_weighting_scheme field. This should be in the
            _refine_ls_weighting_details field.
            Weighting scheme given as calc w = 1/[\s^2^(Fo^2^)+(0.0714P)^2^+0.904P
            Weighting scheme identified as calc
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.97
PLAT213_ALERT_2_C Atom F2      has ADP max/min Ratio .............       3.40 prolat
PLAT213_ALERT_2_C Atom F3      has ADP max/min Ratio .............       3.10 prolat
PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor ....       3.12
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          9
PLAT420_ALERT_2_C D-H Without Acceptor       N1     -   H1D    ...          ?
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          1
            N2  -AG1 -N1  -C1   -140.00  6.00   4.676   1.555   1.555   1.555

   2 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   8 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   5 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

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Computing details

Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1997); software used to prepare material for publication: SHELXTL.

catena-Poly[[silver(I)-µ-1,4-diaminobutane-κ²N:N'] hexafluoroarsenate]

Crystal data

[Ag(C4H12N2)](AsF6)	F(000) = 736
Mr = 384.95	Dx = 2.480 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 4450 reflections
a = 7.806 (2) Å	θ = 2.8–25.4°
b = 10.371 (2) Å	µ = 5.19 mm^−1
c = 13.234 (3) Å	T = 293 K
β = 105.74 (3)°	Block, colorless
V = 1031.2 (4) Å^3	0.38 × 0.32 × 0.20 mm
Z = 4

Data collection

Siemens SMART CCD area-detector diffractometer	2025 independent reflections
Radiation source: fine-focus sealed tube	1757 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.030
φ and ω scans	θmax = 26.0°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −9→9
Tmin = 0.155, Tmax = 0.366	k = −12→8
4479 measured reflections	l = −14→16

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)] = 0.042	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.117	H atoms treated by a mixture of independent and constrained refinement
S = 1.08	Calculated w = 1/[σ^2(Fo^2) + (0.0714P)^2 + 0.904P] where P = (Fo^2 + 2Fc^2)/3
2025 reflections	(Δ/σ)max = 0.001
135 parameters	Δρmax = 1.22 e Å^−3
0 restraints	Δρmin = −0.90 e Å^−3

Special details

Experimental. C, H and N elemental analyses were performed on a Perkin-Elmer elemental analyzer.

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
Ag1	0.02673 (6)	0.81308 (4)	0.63370 (3)	0.03993 (19)
As1	0.24632 (7)	0.84928 (6)	0.37684 (4)	0.0340 (2)
F1	0.1244 (9)	0.7787 (9)	0.2684 (5)	0.150 (4)
F2	0.3581 (11)	0.9251 (11)	0.4843 (5)	0.204 (6)
F3	0.2474 (8)	0.7193 (6)	0.4514 (6)	0.140 (3)
F4	0.4356 (7)	0.8061 (6)	0.3488 (5)	0.115 (3)
F5	0.2458 (8)	0.9844 (5)	0.3057 (5)	0.104 (2)
F6	0.0522 (6)	0.8927 (5)	0.4040 (5)	0.0861 (16)
N1	−0.2426 (6)	0.7491 (5)	0.5761 (4)	0.0413 (11)
H1C	−0.2878	0.7435	0.6317	0.050*
H1D	−0.3030	0.8121	0.5346	0.050*
H2C	−0.133 (10)	0.685 (7)	0.230 (6)	0.06 (2)*
N2	−0.2065 (7)	0.6210 (6)	0.1961 (5)	0.0469 (13)
H2D	−0.170 (9)	0.604 (7)	0.146 (6)	0.045 (19)*
C1	−0.2850 (8)	0.6274 (6)	0.5174 (5)	0.0395 (13)
H1A	−0.4116	0.6172	0.4916	0.080*
H1B	−0.2389	0.5564	0.5632	0.080*
C2	−0.2020 (7)	0.6269 (6)	0.4253 (5)	0.0379 (12)
H2A	−0.0750	0.6211	0.4518	0.080*
H2B	−0.2297	0.7067	0.3876	0.080*
C3	−0.2694 (8)	0.5163 (6)	0.3505 (5)	0.0412 (13)
H3A	−0.3952	0.5261	0.3203	0.080*
H3B	−0.2505	0.4373	0.3898	0.080*
C4	−0.1794 (8)	0.5072 (7)	0.2640 (5)	0.0475 (15)
H4A	−0.0541	0.4950	0.2943	0.080*
H4B	−0.2239	0.4327	0.2219	0.080*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ag1	0.0423 (3)	0.0427 (3)	0.0325 (3)	0.00143 (17)	0.0064 (2)	−0.00528 (17)
As1	0.0327 (3)	0.0383 (4)	0.0307 (3)	−0.0002 (2)	0.0083 (2)	0.0040 (2)
F1	0.144 (6)	0.232 (9)	0.093 (5)	−0.111 (6)	0.062 (4)	−0.103 (6)
F2	0.201 (8)	0.360 (14)	0.066 (4)	−0.208 (9)	0.060 (5)	−0.083 (6)
F3	0.123 (5)	0.121 (5)	0.223 (8)	0.069 (4)	0.125 (6)	0.125 (6)
F4	0.071 (3)	0.141 (6)	0.160 (6)	0.063 (3)	0.079 (4)	0.098 (5)
F5	0.118 (4)	0.073 (3)	0.154 (6)	0.027 (3)	0.092 (4)	0.057 (3)
F6	0.074 (3)	0.087 (3)	0.120 (4)	0.035 (3)	0.064 (3)	0.041 (3)
N1	0.041 (3)	0.046 (3)	0.037 (3)	0.003 (2)	0.010 (2)	−0.005 (2)
N2	0.041 (3)	0.066 (4)	0.034 (3)	−0.002 (3)	0.010 (2)	−0.003 (3)
C1	0.037 (3)	0.041 (3)	0.037 (3)	−0.001 (2)	0.006 (2)	0.000 (3)
C2	0.031 (3)	0.041 (3)	0.042 (3)	−0.003 (2)	0.010 (2)	−0.002 (3)
C3	0.046 (3)	0.040 (3)	0.033 (3)	−0.002 (2)	0.003 (2)	0.003 (2)
C4	0.049 (3)	0.051 (4)	0.040 (3)	0.008 (3)	0.007 (3)	−0.007 (3)

Geometric parameters (Å, º)

Ag1—N2^i	2.134 (6)	N2—H2C	0.91 (8)
Ag1—N1	2.138 (5)	N2—H2D	0.81 (7)
As1—F2	1.652 (6)	C1—C2	1.527 (8)
As1—F1	1.662 (5)	C1—H1A	0.9600
As1—F3	1.669 (5)	C1—H1B	0.9600
As1—F4	1.679 (4)	C2—C3	1.513 (8)
As1—F5	1.687 (5)	C2—H2A	0.9600
As1—F6	1.710 (4)	C2—H2B	0.9600
N1—C1	1.472 (8)	C3—C4	1.500 (9)
N1—H1C	0.9000	C3—H3A	0.9600
N1—H1D	0.9000	C3—H3B	0.9600
N2—C4	1.463 (9)	C4—H4A	0.9600
N2—Ag1^ii	2.134 (6)	C4—H4B	0.9600
N2^i—Ag1—N1	178.0 (2)	Ag1^ii—N2—H2D	106 (5)
F2—As1—F1	176.8 (5)	H2C—N2—H2D	104 (7)
F2—As1—F3	87.7 (5)	N1—C1—C2	109.9 (5)
F1—As1—F3	93.7 (5)	N1—C1—H1A	110.2
F2—As1—F4	91.5 (4)	C2—C1—H1A	109.6
F1—As1—F4	91.4 (4)	N1—C1—H1B	109.4
F3—As1—F4	93.0 (2)	C2—C1—H1B	109.6
F2—As1—F5	90.3 (5)	H1A—C1—H1B	108.2
F1—As1—F5	88.3 (4)	C3—C2—C1	112.2 (5)
F3—As1—F5	177.7 (4)	C3—C2—H2A	109.4
F4—As1—F5	88.1 (2)	C1—C2—H2A	109.2
F2—As1—F6	89.1 (4)	C3—C2—H2B	108.9
F1—As1—F6	88.0 (3)	C1—C2—H2B	109.1
F3—As1—F6	87.2 (2)	H2A—C2—H2B	108.0
F4—As1—F6	179.3 (3)	C4—C3—C2	113.3 (5)
F5—As1—F6	91.7 (2)	C4—C3—H3A	109.1
C1—N1—Ag1	120.8 (4)	C2—C3—H3A	109.1
C1—N1—H1C	107.1	C4—C3—H3B	108.9
Ag1—N1—H1C	107.1	C2—C3—H3B	108.5
C1—N1—H1D	107.1	H3A—C3—H3B	107.8
Ag1—N1—H1D	107.1	N2—C4—C3	113.5 (5)
H1C—N1—H1D	106.8	N2—C4—H4A	108.9
C4—N2—Ag1^ii	117.3 (4)	C3—C4—H4A	108.9
C4—N2—H2C	109 (5)	N2—C4—H4B	108.9
Ag1^ii—N2—H2C	112 (5)	C3—C4—H4B	108.8
C4—N2—H2D	108 (5)	H4A—C4—H4B	107.7
N2^i—Ag1—N1—C1	−140 (6)	C1—C2—C3—C4	−175.4 (5)
Ag1—N1—C1—C2	−53.7 (6)	Ag1^ii—N2—C4—C3	−50.6 (7)
N1—C1—C2—C3	−169.2 (5)	C2—C3—C4—N2	−61.6 (7)

Symmetry codes: (i) x+1/2, −y+3/2, z+1/2; (ii) x−1/2, −y+3/2, z−1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2C···F1	0.91 (8)	2.17 (8)	2.987 (8)	150 (7)
N1—H1C···F1^iii	0.90	2.11	3.012 (7)	175
N2—H2D···F2^ii	0.81 (7)	2.23 (7)	3.018 (8)	165 (6)

Symmetry codes: (ii) x−1/2, −y+3/2, z−1/2; (iii) x−1/2, −y+3/2, z+1/2.