A three-dimensional tin(II) phosphon­atobenzene­sulfonate with Sn4O12 clusters. Corrigendum

Maniam, P.; Stock, N.

doi:10.1107/S0108270111016076

addenda and errata

STRUCTURAL

CHEMISTRY

ISSN: 2053-2296

Volume 67| Part 6| June 2011| Page e14

https://doi.org/10.1107/S0108270111016076

A three-dimensional tin(II) phosphonatobenzenesulfonate with Sn₄O₁₂ clusters. Corrigendum

Palanikumar Maniam ^a and Norbert Stock ^a ^*

^aInstitut für Anorganische Chemie, Christian-Albrechts-Universität zu Kiel, Max-Eyth-Strasse 2, 24118 Kiel, Germany

^*Correspondence e-mail: [email protected]

(Received 15 April 2011; accepted 27 April 2011; online 5 May 2011)

An error in the scattering factors in the paper by Maniam & Stock [Acta Cryst. (2011), C67, m73–m76] is corrected.

In the paper by Maniam & Stock (2011), the S and P atoms were inadvertently refined using the scattering factors of the other element. A corrected CIF and structure factors are now available. Minor changes in the geometric parameters reported in the paper have occurred as a consequence, but all of the conclusions about the structure remain unchanged.

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S0108270111016076/jz9200sup1.cif

Structure factors: contains datablock pm1. DOI: https://doi.org/10.1107/S0108270111016076/jz9200Isup2.hkl

Computing details top

Data collection: X-AREA (Stoe & Cie, 2008); cell refinement: X-AREA (Stoe & Cie, 2008); data reduction: X-AREA (Stoe & Cie, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2010); software used to prepare material for publication: XCIF in SHELXTL (Sheldrick, 2008).

Poly[µ-hydroxido-(µ7–4-phosphonatobenzenesulfonato)ditin(II)] top

Crystal data top

[Sn₂(C₆H₄O₆PS)(OH)]	Z = 2
M_r = 489.56	F(000) = 456
Triclinic, P1	D_x = 2.847 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.0045 (14) Å	Cell parameters from 1556 reflections
b = 8.487 (2) Å	θ = 1.9–28.2°
c = 10.0570 (17) Å	µ = 4.72 mm⁻¹
α = 81.10 (2)°	T = 293 K
β = 86.17 (2)°	Plate, colourless
γ = 75.25 (3)°	0.14 × 0.10 × 0.07 mm
V = 571.0 (2) Å³

Data collection top

Stoe IPDS-1 diffractometer	2550 independent reflections
Radiation source: fine-focus sealed tube	2146 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.048
φ scans	θ_max = 28.1°, θ_min = 2.5°
Absorption correction: numerical (XRED rev 1.19 and X-SHAPE rev 1.06)	h = −9→9
T_min = 0.380, T_max = 0.581	k = −11→11
6691 measured reflections	l = −13→13

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.025	H-atom parameters constrained
wR(F²) = 0.066	w = 1/[σ²(F_o²) + (0.0397P)²] where P = (F_o² + 2F_c²)/3
S = 1.02	(Δ/σ)_max = 0.001
2550 reflections	Δρ_max = 0.79 e Å⁻³
155 parameters	Δρ_min = −1.08 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0121 (9)

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

	x	y	z	U_iso*/U_eq
Sn1	−0.18614 (4)	0.83666 (3)	0.57934 (2)	0.01832 (10)
Sn2	−0.35359 (4)	0.61742 (3)	0.35282 (2)	0.01956 (10)
P1	0.12971 (14)	0.57551 (11)	0.34654 (8)	0.01184 (19)
S1	0.37171 (15)	0.93625 (12)	−0.21627 (8)	0.0192 (2)
O1	−0.0710 (4)	0.6751 (3)	0.3976 (2)	0.0150 (5)
O2	0.1080 (4)	0.4085 (3)	0.3189 (2)	0.0178 (5)
O3	0.2898 (4)	0.5661 (3)	0.4465 (2)	0.0173 (5)
O4	0.2573 (5)	0.9067 (4)	−0.3215 (3)	0.0323 (7)
O5	0.5823 (5)	0.8540 (4)	−0.2319 (3)	0.0270 (7)
O6	0.3415 (5)	1.1096 (4)	−0.2013 (3)	0.0290 (7)
O7	−0.4330 (4)	0.7917 (3)	0.4877 (2)	0.0164 (5)
H7	−0.5508	0.8395	0.5044	0.025*
C1	0.1893 (6)	0.6797 (4)	0.1859 (3)	0.0158 (7)
C2	0.2372 (10)	0.5963 (6)	0.0754 (4)	0.0482 (16)
H2	0.2351	0.4861	0.0837	0.058*
C3	0.2879 (12)	0.6763 (6)	−0.0469 (5)	0.057 (2)
H3	0.3180	0.6203	−0.1211	0.069*
C4	0.2942 (6)	0.8397 (5)	−0.0594 (3)	0.0213 (8)
C5	0.2430 (7)	0.9258 (5)	0.0479 (4)	0.0253 (9)
H5	0.2455	1.0359	0.0389	0.030*
C6	0.1875 (7)	0.8459 (5)	0.1701 (4)	0.0260 (9)
H6	0.1487	0.9044	0.2423	0.031*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Sn1	0.02088 (18)	0.01538 (14)	0.01944 (15)	−0.00646 (11)	−0.00125 (10)	−0.00118 (9)
Sn2	0.01846 (18)	0.02484 (16)	0.01551 (14)	−0.00269 (12)	−0.00038 (9)	−0.00787 (10)
P1	0.0122 (5)	0.0145 (4)	0.0075 (4)	−0.0030 (4)	0.0025 (3)	0.0007 (3)
S1	0.0209 (5)	0.0235 (5)	0.0096 (4)	−0.0031 (4)	0.0045 (3)	0.0022 (3)
O1	0.0129 (14)	0.0192 (12)	0.0121 (11)	−0.0036 (11)	0.0035 (9)	−0.0019 (9)
O2	0.0247 (17)	0.0140 (12)	0.0138 (11)	−0.0049 (11)	−0.0020 (10)	0.0012 (9)
O3	0.0147 (15)	0.0226 (13)	0.0135 (11)	−0.0051 (11)	−0.0016 (9)	0.0020 (10)
O4	0.032 (2)	0.050 (2)	0.0148 (13)	−0.0133 (16)	−0.0001 (11)	0.0001 (13)
O5	0.0213 (18)	0.0370 (17)	0.0170 (13)	0.0009 (14)	0.0059 (11)	−0.0030 (12)
O6	0.039 (2)	0.0227 (15)	0.0184 (13)	−0.0017 (14)	0.0080 (12)	0.0043 (11)
O7	0.0104 (15)	0.0216 (13)	0.0161 (11)	−0.0012 (11)	0.0031 (9)	−0.0049 (9)
C1	0.017 (2)	0.0190 (17)	0.0106 (14)	−0.0047 (15)	0.0027 (12)	0.0000 (13)
C2	0.103 (5)	0.022 (2)	0.021 (2)	−0.023 (3)	0.026 (2)	−0.0072 (17)
C3	0.126 (6)	0.027 (2)	0.020 (2)	−0.025 (3)	0.032 (3)	−0.0093 (18)
C4	0.024 (2)	0.0267 (19)	0.0105 (15)	−0.0062 (17)	0.0060 (14)	0.0015 (14)
C5	0.041 (3)	0.0223 (19)	0.0143 (17)	−0.0131 (19)	0.0088 (16)	−0.0033 (14)
C6	0.046 (3)	0.0216 (19)	0.0125 (16)	−0.0136 (19)	0.0103 (16)	−0.0051 (14)

Geometric parameters (Å, º) top

Sn1—O1	2.427 (3)	S1—C4	1.780 (3)
Sn1—O2ⁱ	2.124 (2)	O2—Sn1ⁱ	2.124 (2)
Sn1—O5ⁱⁱ	2.410 (3)	O3—Sn2ⁱ	2.344 (2)
Sn1—O7	2.155 (3)	O5—Sn1^v	2.410 (3)
Sn2—O1	2.246 (3)	O7—H7	0.8400
Sn2—O3ⁱ	2.344 (2)	C1—C2	1.386 (5)
Sn2—O3ⁱⁱⁱ	2.726 (3)	C1—C6	1.391 (5)
Sn2—O6^iv	2.586 (3)	C2—C3	1.381 (6)
Sn2—O7	2.108 (3)	C2—H2	0.9300
P1—O1	1.545 (3)	C3—C4	1.384 (6)
P1—O2	1.532 (3)	C3—H3	0.9300
P1—O3	1.535 (3)	C4—C5	1.373 (6)
P1—C1	1.795 (3)	C5—C6	1.391 (5)
S1—O4	1.460 (4)	C5—H5	0.9300
S1—O5	1.472 (3)	C6—H6	0.9300
S1—O6	1.462 (4)

O2ⁱ—Sn1—O7	91.85 (10)	P1—O1—Sn1	136.42 (15)
O2ⁱ—Sn1—O5ⁱⁱ	78.75 (11)	Sn2—O1—Sn1	99.92 (10)
O7—Sn1—O5ⁱⁱ	80.68 (10)	P1—O2—Sn1ⁱ	135.22 (15)
O2ⁱ—Sn1—O1	76.93 (9)	P1—O3—Sn2ⁱ	126.01 (14)
O7—Sn1—O1	69.83 (10)	S1—O5—Sn1^v	133.80 (16)
O5ⁱⁱ—Sn1—O1	140.72 (10)	Sn2—O7—Sn1	114.23 (12)
O1—Sn2—O3ⁱ	83.17 (9)	Sn2—O7—H7	122.9
O3ⁱ—Sn2—O3ⁱⁱⁱ	74.26 (8)	Sn1—O7—H7	122.9
O3ⁱⁱⁱ—Sn2—O6^iv	119.16 (10)	C2—C1—C6	118.8 (3)
O6^iv—Sn2—O1	73.59 (10)	C2—C1—P1	120.6 (3)
O7—Sn2—O1	74.32 (9)	C6—C1—P1	120.5 (3)
O6^iv—Sn2—O3ⁱ	152.18 (9)	C3—C2—C1	120.2 (4)
O1—Sn2—O3ⁱⁱⁱ	147.71 (10)	C3—C2—H2	119.9
O2—P1—O3	114.80 (16)	C1—C2—H2	119.9
O2—P1—O1	109.26 (16)	C2—C3—C4	120.2 (4)
O3—P1—O1	109.44 (15)	C2—C3—H3	119.9
O2—P1—C1	105.37 (16)	C4—C3—H3	119.9
O3—P1—C1	109.46 (16)	C5—C4—C3	120.6 (3)
O1—P1—C1	108.27 (16)	C5—C4—S1	120.4 (3)
O4—S1—O6	114.6 (2)	C3—C4—S1	119.1 (3)
O4—S1—O5	110.96 (19)	C4—C5—C6	119.1 (4)
O6—S1—O5	112.1 (2)	C4—C5—H5	120.5
O4—S1—C4	107.95 (19)	C6—C5—H5	120.5
O6—S1—C4	105.61 (18)	C1—C6—C5	121.0 (4)
O5—S1—C4	104.99 (19)	C1—C6—H6	119.5
P1—O1—Sn2	120.56 (15)	C5—C6—H6	119.5

O2—P1—O1—Sn2	−22.08 (19)	O3ⁱ—Sn2—O7—Sn1	73.83 (12)
O3—P1—O1—Sn2	−148.56 (14)	O2ⁱ—Sn1—O7—Sn2	−64.68 (13)
C1—P1—O1—Sn2	92.19 (18)	O5ⁱⁱ—Sn1—O7—Sn2	−142.96 (13)
O2—P1—O1—Sn1	133.51 (19)	O1—Sn1—O7—Sn2	10.67 (10)
O3—P1—O1—Sn1	7.0 (2)	O2—P1—C1—C2	−10.4 (5)
C1—P1—O1—Sn1	−112.2 (2)	O3—P1—C1—C2	113.5 (4)
O7—Sn2—O1—P1	172.42 (17)	O1—P1—C1—C2	−127.2 (4)
O3ⁱ—Sn2—O1—P1	88.70 (16)	O2—P1—C1—C6	169.4 (4)
O7—Sn2—O1—Sn1	9.22 (9)	O3—P1—C1—C6	−66.7 (4)
O3ⁱ—Sn2—O1—Sn1	−74.49 (10)	O1—P1—C1—C6	52.6 (4)
O2ⁱ—Sn1—O1—P1	−71.2 (2)	C6—C1—C2—C3	1.9 (9)
O7—Sn1—O1—P1	−168.1 (2)	P1—C1—C2—C3	−178.3 (5)
O5ⁱⁱ—Sn1—O1—P1	−124.3 (2)	C1—C2—C3—C4	1.0 (11)
O2ⁱ—Sn1—O1—Sn2	87.68 (11)	C2—C3—C4—C5	−2.5 (10)
O7—Sn1—O1—Sn2	−9.25 (9)	C2—C3—C4—S1	177.0 (5)
O5ⁱⁱ—Sn1—O1—Sn2	34.56 (19)	O4—S1—C4—C5	−129.6 (4)
O3—P1—O2—Sn1ⁱ	20.6 (3)	O6—S1—C4—C5	−6.6 (4)
O1—P1—O2—Sn1ⁱ	−102.7 (2)	O5—S1—C4—C5	112.0 (4)
C1—P1—O2—Sn1ⁱ	141.1 (2)	O4—S1—C4—C3	51.0 (5)
O2—P1—O3—Sn2ⁱ	−42.0 (2)	O6—S1—C4—C3	174.0 (5)
O1—P1—O3—Sn2ⁱ	81.3 (2)	O5—S1—C4—C3	−67.4 (5)
C1—P1—O3—Sn2ⁱ	−160.22 (18)	C3—C4—C5—C6	0.9 (8)
O4—S1—O5—Sn1^v	46.6 (3)	S1—C4—C5—C6	−178.5 (4)
O6—S1—O5—Sn1^v	−82.9 (3)	C2—C1—C6—C5	−3.5 (7)
C4—S1—O5—Sn1^v	163.0 (2)	P1—C1—C6—C5	176.7 (4)
O1—Sn2—O7—Sn1	−11.25 (10)	C4—C5—C6—C1	2.0 (7)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7···O4ⁱⁱ	0.84	2.19	2.878 (4)	139

Symmetry code: (ii) x−1, y, z+1.

References

Maniam, P. & Stock, N. (2011). Acta Cryst. C67, m73–m76. Web of Science CSD CrossRef IUCr Journals Google Scholar

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STRUCTURAL

CHEMISTRY

ISSN: 2053-2296

Volume 67| Part 6| June 2011| Page e14

https://doi.org/10.1107/S0108270111016076

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