Poly[diaqua-(μ(4)-carboxyl-atomethyl-phospho-nato)(μ(4)-carb-oxy-methyl-phospho-nato)penta-deca-methyl-penta-tin(IV)].

The central Sn(IV) atom of the penta-nuclear title complex, {[Sn(CH(3))(3)](3)O(2)C(CH(2))PO(3)[Sn(CH(3))(3)(H(2)O)](2)HO(2)C(CH(2))PO(3)}, is located on a twofold rotation axis; due to symmetry, the H atom of the carboxyl group of the anion is disordered with a site occupancy of 0.5. The central Sn(IV) atom is bonded to three methyl groups (one of which is disordered about the twofold rotation axis) and is symmetrically trans coordinated by two phospho-nate groups with Sn-O = 2.2665 (12) Å while the other SnMe(3) residues are asymmetrically trans coordinated with Sn-O = 2.1587 (12) and 2.3756 (13) Å for one residue and Sn-O = 2.1522 (12) and 2.4335 (12) Å for the other; the Sn-O distances involving two O atoms trans to carboxyl-ate are longer than those trans to phospho-nate groups. The Sn-C distances lie in a very narrow range [2.112 (2)-2.133 (3) Å]. The oxyanion behaves as a tetra-coordinating ligand. The bridging mode of the latter leads to the formation of layers parallel to (001) that are inter-connected by O-H⋯O and C-H⋯O hydrogen bonds.

Related literature

For applications of tin-based materials, see: Dutrecq et al. (1992 ▶); Basu Baul et al. (2011 ▶). For related structures, see: Zhang et al. (2010 ▶).

Experimental

Crystal data

[Sn5(CH3)15(C2H2O5P)(C2H3O5P)(H2O)2]

M = 1130.01

Monoclinic,

a = 11.6939 (2) Å

b = 13.1689 (3) Å

c = 25.9575 (5) Å

β = 95.40 (1)°

V = 3979.61 (14) Å3

Z = 4

Mo Kα radiation

μ = 3.22 mm−1

T = 150 K

0.32 × 0.15 × 0.15 mm

Data collection

Nonius KappaCCD diffractometer

Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997 ▶) T min = 0.426, T max = 0.644

15302 measured reflections

7932 independent reflections

7236 reflections with I > 2σ(I)

R int = 0.020

Refinement

R[F 2 > 2σ(F 2)] = 0.022

wR(F 2) = 0.054

S = 1.09

7932 reflections

182 parameters

H-atom parameters constrained

Δρmax = 1.14 e Å−3

Δρmin = −0.85 e Å−3

Data collection: COLLECT (Nonius, 2003 ▶); cell refinement: SCALEPACK (Otwinowski & Minor, 1997 ▶); data reduction: DENZO (Otwinowski & Minor, 1997 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 2012 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Click here for additional data file.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536813000676/pv2611sup1.cif

Click here for additional data file.

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813000676/pv2611Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Sn5(CH3)15(C2H2O5P)(C2H3O5P)(H2O)2]	F(000) = 2176
Mr = 1130.01	Dx = 1.886 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 34199 reflections
a = 11.6939 (2) Å	θ = 1.0–33.7°
b = 13.1689 (3) Å	µ = 3.22 mm−1
c = 25.9575 (5) Å	T = 150 K
β = 95.40 (1)°	Prism, colorless
V = 3979.61 (14) Å3	0.32 × 0.15 × 0.15 mm
Z = 4

Nonius KappaCCD diffractometer	7932 independent reflections
Radiation source: fine-focus sealed tube	7236 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.020
φ and ω scans with κ ofset	θmax = 33.8°, θmin = 2.3°
Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997)	h = −18→18
Tmin = 0.426, Tmax = 0.644	k = −20→20
15302 measured reflections	l = −40→40

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)] = 0.022	H-atom parameters constrained
wR(F2) = 0.054	w = 1/[σ2(Fo2) + (0.0207P)2 + 4.2723P] where P = (Fo2 + 2Fc2)/3
S = 1.09	(Δ/σ)max = 0.005
7932 reflections	Δρmax = 1.14 e Å−3
182 parameters	Δρmin = −0.85 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: 0.00041 (3)

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(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.

	x	y	z	Uiso*/Ueq	Occ. (<1)
Sn1	0.5000	0.755553 (11)	0.2500	0.01394 (4)
Sn3	0.657492 (10)	0.979143 (8)	0.093373 (4)	0.01521 (3)
Sn2	0.178461 (10)	0.935201 (8)	0.137009 (4)	0.01528 (3)
P1	0.43748 (3)	0.80781 (3)	0.118293 (15)	0.01189 (7)
O5	0.33357 (11)	0.57344 (9)	0.08457 (5)	0.0182 (2)
O4	0.24248 (11)	0.67603 (9)	0.02767 (5)	0.0180 (2)
O1	0.50422 (11)	0.75081 (9)	0.16291 (5)	0.0161 (2)
O3	0.49774 (11)	0.90382 (9)	0.10334 (5)	0.0186 (2)
C7	0.6528 (2)	0.94022 (17)	0.01376 (8)	0.0302 (4)
H7A	0.6136	0.9940	−0.0072	0.045*
H7B	0.6112	0.8761	0.0076	0.045*
H7C	0.7314	0.9326	0.0041	0.045*
O2	0.31351 (10)	0.82643 (9)	0.12850 (5)	0.0183 (2)
C9	0.43300 (13)	0.72417 (12)	0.06161 (6)	0.0139 (3)
H9A	0.4299	0.7663	0.0299	0.017*
H9B	0.5046	0.6836	0.0634	0.017*
C2	0.5000	0.9175 (2)	0.2500	0.0258 (5)
H2A	0.4976	0.9424	0.2143	0.039*	0.50
H2B	0.5699	0.9424	0.2698	0.039*	0.50
H2C	0.4325	0.9424	0.2658	0.039*	0.50
C8	0.33124 (13)	0.65301 (12)	0.05775 (6)	0.0135 (3)
C1	0.34603 (16)	0.66906 (15)	0.24300 (7)	0.0225 (3)
H1A	0.3063	0.6788	0.2084	0.034*
H1B	0.2962	0.6915	0.2691	0.034*
H1C	0.3645	0.5970	0.2482	0.034*
C4	0.28441 (19)	1.06554 (15)	0.13493 (10)	0.0303 (4)
H4A	0.2371	1.1245	0.1239	0.045*
H4B	0.3420	1.0543	0.1105	0.045*
H4C	0.3230	1.0781	0.1695	0.045*
C5	0.07938 (19)	0.89233 (17)	0.06770 (8)	0.0298 (4)
H5A	0.1051	0.8258	0.0564	0.045*
H5B	0.0891	0.9429	0.0408	0.045*
H5C	−0.0018	0.8885	0.0740	0.045*
C3	0.1385 (2)	0.86901 (18)	0.20725 (8)	0.0326 (5)
H3A	0.2046	0.8755	0.2332	0.049*
H3B	0.1204	0.7970	0.2016	0.049*
H3C	0.0721	0.9038	0.2195	0.049*
C6	0.59248 (18)	1.11584 (15)	0.12221 (9)	0.0284 (4)
H6A	0.5612	1.1025	0.1553	0.043*
H6B	0.5316	1.1424	0.0973	0.043*
H6C	0.6546	1.1658	0.1274	0.043*
O6	0.02501 (12)	1.04809 (10)	0.14945 (6)	0.0235 (3)
C10	0.76318 (18)	0.88614 (18)	0.14468 (9)	0.0339 (5)
H10A	0.8142	0.9290	0.1675	0.051*
H10B	0.8093	0.8413	0.1247	0.051*
H10C	0.7149	0.8451	0.1655	0.051*
H1O	−0.0374	1.0436	0.1273	0.050*
H2O	0.0350	1.1118	0.1539	0.050*
H1O4	0.2273	0.6343	0.0029	0.050*	0.50

	U11	U22	U33	U12	U13	U23
Sn1	0.01612 (7)	0.01318 (7)	0.01246 (7)	0.000	0.00108 (5)	0.000
Sn3	0.01622 (5)	0.01419 (5)	0.01498 (5)	−0.00358 (3)	0.00010 (4)	0.00139 (3)
Sn2	0.01507 (5)	0.01522 (5)	0.01564 (6)	0.00115 (3)	0.00182 (4)	−0.00054 (4)
P1	0.01177 (16)	0.01130 (16)	0.01267 (17)	−0.00176 (12)	0.00149 (13)	0.00042 (13)
O5	0.0157 (5)	0.0162 (5)	0.0220 (6)	−0.0029 (4)	−0.0018 (5)	0.0060 (4)
O4	0.0163 (5)	0.0181 (5)	0.0183 (5)	−0.0042 (4)	−0.0044 (4)	0.0046 (4)
O1	0.0189 (6)	0.0169 (5)	0.0123 (5)	0.0013 (4)	0.0005 (4)	0.0005 (4)
O3	0.0183 (6)	0.0140 (5)	0.0232 (6)	−0.0066 (4)	0.0010 (5)	0.0020 (4)
C7	0.0352 (11)	0.0341 (11)	0.0217 (9)	−0.0133 (8)	0.0055 (8)	−0.0054 (8)
O2	0.0134 (5)	0.0166 (5)	0.0258 (6)	0.0008 (4)	0.0063 (4)	−0.0011 (5)
C9	0.0130 (6)	0.0166 (7)	0.0123 (6)	−0.0039 (5)	0.0017 (5)	0.0001 (5)
C2	0.0419 (16)	0.0156 (10)	0.0194 (11)	0.000	0.0006 (11)	0.000
C8	0.0130 (6)	0.0135 (6)	0.0140 (6)	−0.0020 (5)	0.0013 (5)	0.0000 (5)
C1	0.0201 (8)	0.0262 (9)	0.0207 (8)	−0.0057 (6)	−0.0012 (6)	0.0045 (7)
C4	0.0254 (9)	0.0188 (8)	0.0481 (13)	−0.0023 (7)	0.0104 (9)	−0.0041 (8)
C5	0.0308 (10)	0.0330 (10)	0.0244 (9)	0.0088 (8)	−0.0042 (8)	−0.0088 (8)
C3	0.0387 (12)	0.0343 (11)	0.0269 (10)	0.0160 (9)	0.0150 (9)	0.0104 (8)
C6	0.0264 (9)	0.0196 (8)	0.0406 (11)	−0.0068 (7)	0.0110 (8)	−0.0071 (8)
O6	0.0195 (6)	0.0186 (6)	0.0308 (7)	0.0076 (5)	−0.0062 (5)	−0.0057 (5)
C10	0.0244 (9)	0.0344 (11)	0.0411 (12)	−0.0056 (8)	−0.0063 (9)	0.0204 (9)

Sn1—C1	2.124 (2)	C9—C8	1.511 (2)
Sn1—C1i	2.124 (2)	C9—H9A	0.9900
Sn1—C2	2.133 (3)	C9—H9B	0.9900
Sn1—O1i	2.2665 (12)	C2—H2A	0.9800
Sn1—O1	2.2665 (12)	C2—H2B	0.9800
Sn3—C6	2.118 (2)	C2—H2C	0.9800
Sn3—C10	2.119 (2)	C1—H1A	0.9800
Sn3—C7	2.125 (2)	C1—H1B	0.9800
Sn3—O3	2.1522 (12)	C1—H1C	0.9800
Sn3—O5ii	2.4335 (12)	C4—H4A	0.9800
Sn2—C3	2.112 (2)	C4—H4B	0.9800
Sn2—C4	2.120 (2)	C4—H4C	0.9800
Sn2—C5	2.123 (2)	C5—H5A	0.9800
Sn2—O2	2.1587 (12)	C5—H5B	0.9800
Sn2—O6	2.3756 (13)	C5—H5C	0.9800
P1—O3	1.5156 (12)	C3—H3A	0.9800
P1—O2	1.5180 (13)	C3—H3B	0.9800
P1—O1	1.5310 (12)	C3—H3C	0.9800
P1—C9	1.8348 (16)	C6—H6A	0.9800
O5—C8	1.2571 (19)	C6—H6B	0.9800
O5—Sn3iii	2.4335 (12)	C6—H6C	0.9800
O4—C8	1.2752 (19)	O6—H1O	0.8900
O4—H1O4	0.8500	O6—H2O	0.8500
C7—H7A	0.9800	C10—H10A	0.9800
C7—H7B	0.9800	C10—H10B	0.9800
C7—H7C	0.9800	C10—H10C	0.9800
C1—Sn1—C1i	115.13 (11)	P1—C9—H9B	109.0
C1—Sn1—C2	122.43 (6)	H9A—C9—H9B	107.8
C1i—Sn1—C2	122.43 (6)	Sn1—C2—H2A	109.5
C1—Sn1—O1i	88.44 (6)	Sn1—C2—H2B	109.5
C1i—Sn1—O1i	89.87 (6)	H2A—C2—H2B	109.5
C2—Sn1—O1i	91.58 (3)	Sn1—C2—H2C	109.5
C1—Sn1—O1	89.87 (6)	H2A—C2—H2C	109.5
C1i—Sn1—O1	88.44 (6)	H2B—C2—H2C	109.5
C2—Sn1—O1	91.58 (3)	O5—C8—O4	120.75 (14)
O1i—Sn1—O1	176.84 (6)	O5—C8—C9	120.30 (14)
C6—Sn3—C10	118.46 (10)	O4—C8—C9	118.94 (14)
C6—Sn3—C7	124.85 (9)	Sn1—C1—H1A	109.5
C10—Sn3—C7	115.59 (10)	Sn1—C1—H1B	109.5
C6—Sn3—O3	90.27 (6)	H1A—C1—H1B	109.5
C10—Sn3—O3	96.87 (7)	Sn1—C1—H1C	109.5
C7—Sn3—O3	93.58 (7)	H1A—C1—H1C	109.5
C6—Sn3—O5ii	86.24 (6)	H1B—C1—H1C	109.5
C10—Sn3—O5ii	84.57 (6)	Sn2—C4—H4A	109.5
C7—Sn3—O5ii	88.65 (7)	Sn2—C4—H4B	109.5
O3—Sn3—O5ii	176.51 (5)	H4A—C4—H4B	109.5
C3—Sn2—C4	122.21 (10)	Sn2—C4—H4C	109.5
C3—Sn2—C5	118.33 (10)	H4A—C4—H4C	109.5
C4—Sn2—C5	117.86 (10)	H4B—C4—H4C	109.5
C3—Sn2—O2	92.16 (7)	Sn2—C5—H5A	109.5
C4—Sn2—O2	95.72 (7)	Sn2—C5—H5B	109.5
C5—Sn2—O2	94.76 (7)	H5A—C5—H5B	109.5
C3—Sn2—O6	84.82 (7)	Sn2—C5—H5C	109.5
C4—Sn2—O6	86.99 (7)	H5A—C5—H5C	109.5
C5—Sn2—O6	85.56 (6)	H5B—C5—H5C	109.5
O2—Sn2—O6	176.72 (5)	Sn2—C3—H3A	109.5
O3—P1—O2	112.62 (7)	Sn2—C3—H3B	109.5
O3—P1—O1	112.74 (7)	H3A—C3—H3B	109.5
O2—P1—O1	111.98 (7)	Sn2—C3—H3C	109.5
O3—P1—C9	105.92 (7)	H3A—C3—H3C	109.5
O2—P1—C9	106.33 (7)	H3B—C3—H3C	109.5
O1—P1—C9	106.64 (7)	Sn3—C6—H6A	109.5
C8—O5—Sn3iii	120.20 (10)	Sn3—C6—H6B	109.5
C8—O4—H1O4	114.10	H6A—C6—H6B	109.5
P1—O1—Sn1	133.13 (7)	Sn3—C6—H6C	109.5
P1—O3—Sn3	147.67 (8)	H6A—C6—H6C	109.5
Sn3—C7—H7A	109.5	H6B—C6—H6C	109.5
Sn3—C7—H7B	109.5	Sn2—O6—H1O	117.00
H7A—C7—H7B	109.5	Sn2—O6—H2O	123.00
Sn3—C7—H7C	109.5	H1O—O6—H2O	104.00
H7A—C7—H7C	109.5	Sn3—C10—H10A	109.5
H7B—C7—H7C	109.5	Sn3—C10—H10B	109.5
P1—O2—Sn2	147.66 (8)	H10A—C10—H10B	109.5
C8—C9—P1	112.86 (11)	Sn3—C10—H10C	109.5
C8—C9—H9A	109.0	H10A—C10—H10C	109.5
P1—C9—H9A	109.0	H10B—C10—H10C	109.5
C8—C9—H9B	109.0
O3—P1—O1—Sn1	91.91 (11)	O1—P1—O2—Sn2	121.26 (15)
O2—P1—O1—Sn1	−36.34 (12)	C9—P1—O2—Sn2	−122.63 (15)
C9—P1—O1—Sn1	−152.26 (9)	C3—Sn2—O2—P1	−130.11 (17)
C1—Sn1—O1—P1	76.70 (11)	C4—Sn2—O2—P1	−7.43 (17)
C1i—Sn1—O1—P1	−168.15 (11)	C5—Sn2—O2—P1	111.23 (16)
C2—Sn1—O1—P1	−45.74 (10)	O3—P1—C9—C8	−151.17 (11)
O2—P1—O3—Sn3	164.46 (14)	O2—P1—C9—C8	−31.14 (13)
O1—P1—O3—Sn3	36.55 (17)	O1—P1—C9—C8	88.51 (12)
C9—P1—O3—Sn3	−79.71 (16)	Sn3iii—O5—C8—O4	−12.4 (2)
C6—Sn3—O3—P1	−142.37 (16)	Sn3iii—O5—C8—C9	166.22 (11)
C10—Sn3—O3—P1	−23.64 (17)	P1—C9—C8—O5	−80.06 (17)
C7—Sn3—O3—P1	92.69 (16)	P1—C9—C8—O4	98.60 (16)
O3—P1—O2—Sn2	−7.05 (18)

D—H···A	D—H	H···A	D···A	D—H···A
O6—H1O···O5iv	0.89	1.83	2.693 (2)	164
O6—H2O···O1iv	0.85	1.88	2.706 (2)	161
C9—H9A···O4v	0.99	2.51	3.227 (2)	129

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O6—H1O⋯O5i	0.89	1.83	2.693 (2)	164
O6—H2O⋯O1i	0.85	1.88	2.706 (2)	161
C9—H9A⋯O4ii	0.99	2.51	3.227 (2)	129

Symmetry codes: (i) ; (ii) .