catena-Poly[calcium-bis-[μ-N-(dimethyl-phosphino-yl)benzene-sulfonamidato]].

The crystal structure of the title calcium complex, [Ca(C(8)H(11)NO(5)PS)(2)](n), is composed of a polymeric chain, which is formed due to two bridging sulfonyl groups linking Ca(II) ions in a O-S-O-Ca manner. Thus, the coordination environment of the Ca(II) ions is composed of six O atoms belonging to the phosphoryl and sulfonyl groups of two chelate rings and two additional O atoms of two bridging sulfonyl groups. The coordination polyhedron of the central atom (2 symmetry) has a distorted octa-hedral geometry.

Related literature

For general background see: Wojtczak et al. (1996 ▶); Purdy et al. (1989 ▶); Oehr & Suhr (1988 ▶); Berry et al. (1988 ▶); Pietraszkiewicz et al. (2002 ▶); Anand (1996 ▶); Shannon (1976 ▶). For the synthesis of the ligand, see: Kirsanov (1952 ▶); Kirsanov & Shevchenko (1954 ▶). For theoretical S—O distances in the free non-coord­inated ligand, see: Moroz et al. (2009 ▶).

Experimental

Crystal data

[<span class="Chemical">Ca(C8H11NO5PS)2]

M = 568.50

Monoclinic,

a = 20.692 (2) Å

b = 5.675 (1) Å

c = 22.178 (3) Å

β = 115.26 (1)°

V = 2355.3 (6) Å3

Z = 4

Mo Kα radiation

μ = 0.63 mm−1

T = 293 K

0.40 × 0.20 × 0.10 mm

Data collection

Xcalibur’3 diffractometer

Absorption correction: multi-scan (CrysAlis <span class="Disease">RED; Oxford Diffraction, 2006 ▶) T min = 0.785, T max = 0.939

8999 measu<span class="Disease">red reflections

3280 independent reflections

2503 reflections with I > 2σ(I)

R int = 0.036

Refinement

R[F 2 > 2σ(F 2)] = 0.046

wR(F 2) = 0.139

S = 1.10

3280 reflections

152 parameters

H-atom parameters constrained

Δρmax = 1.28 e Å−3

Δρmin = −0.59 e Å−3

Data collection: CrysAlis CCD (Oxford Diffraction, 2006 ▶); cell refinement: CrysAlis RED (Oxford Diffraction, 2006 ▶); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809032875/bq2148sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809032875/bq2148Isup2.hkl

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

[Ca(C8H11NO5PS)2]	F(000) = 1176
Mr = 568.50	Dx = 1.603 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 6842 reflections
a = 20.692 (2) Å	θ = 3.6–27.5°
b = 5.675 (1) Å	µ = 0.63 mm−1
c = 22.178 (3) Å	T = 293 K
β = 115.26 (1)°	Block, colourless
V = 2355.3 (6) Å3	0.40 × 0.20 × 0.10 mm
Z = 4

Xcalibur'3 diffractometer	3280 independent reflections
Radiation source: Enhance (Mo) X-ray Source	2503 reflections with I > 2σ(I)
graphite	Rint = 0.036
Detector resolution: 16.1827 pixels mm-1	θmax = 30.0°, θmin = 3.6°
ω–scans	h = −25→29
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2006)	k = −7→7
Tmin = 0.785, Tmax = 0.939	l = −30→28
8999 measured reflections

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)] = 0.046	Hydrogen site location: difference Fourier map
wR(F2) = 0.139	H-atom parameters constrained
S = 1.10	w = 1/[σ2(Fo2) + (0.0886P)2] where P = (Fo2 + 2Fc2)/3
3280 reflections	(Δ/σ)max = 0.001
152 parameters	Δρmax = 1.28 e Å−3
0 restraints	Δρmin = −0.59 e Å−3

Experimental. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.

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.

	x	y	z	Uiso*/Ueq
Ca1	0.0000	0.11798 (9)	0.7500	0.02738 (15)
P1	−0.08497 (3)	0.40618 (9)	0.59729 (3)	0.03320 (16)
S1	0.11429 (2)	0.61596 (8)	0.80223 (2)	0.02767 (15)
N1	0.10168 (11)	0.6246 (3)	0.86566 (10)	0.0398 (4)
O1	0.08963 (8)	0.4015 (2)	0.76256 (7)	0.0361 (3)
O2	0.08568 (8)	−0.1711 (3)	0.76345 (8)	0.0407 (4)
O3	−0.03860 (8)	0.2157 (3)	0.63913 (7)	0.0386 (3)
O4	−0.05382 (10)	0.5213 (3)	0.55067 (8)	0.0476 (4)
O5	−0.15878 (8)	0.3097 (3)	0.54554 (8)	0.0506 (4)
C1	0.20763 (10)	0.6308 (3)	0.82721 (10)	0.0299 (4)
C2	0.24528 (12)	0.8183 (4)	0.86721 (13)	0.0457 (5)
H2	0.2221	0.9313	0.8812	0.055*
C3	0.31817 (13)	0.8330 (5)	0.88576 (15)	0.0565 (7)
H3	0.3441	0.9571	0.9126	0.068*
C4	0.35270 (13)	0.6668 (5)	0.86510 (14)	0.0518 (6)
H4	0.4015	0.6799	0.8774	0.062*
C5	0.31461 (12)	0.4795 (5)	0.82586 (12)	0.0488 (6)
H5	0.3379	0.3667	0.8119	0.059*
C6	0.24168 (12)	0.4602 (4)	0.80730 (11)	0.0397 (5)
H6	0.2161	0.3333	0.7817	0.048*
C7	0.00791 (16)	0.6710 (5)	0.57917 (17)	0.0597 (7)
H7C	−0.0048	0.8154	0.5940	0.090*
H7B	0.0251	0.7052	0.5462	0.090*
H7A	0.0446	0.5927	0.6164	0.090*
C8	−0.16248 (17)	0.0968 (5)	0.50864 (15)	0.0606 (8)
H8C	−0.2108	0.0719	0.4763	0.091*
H8B	−0.1472	−0.0345	0.5388	0.091*
H8A	−0.1319	0.1115	0.4863	0.091*

	U11	U22	U33	U12	U13	U23
Ca1	0.0234 (2)	0.0265 (3)	0.0295 (3)	0.000	0.0087 (2)	0.000
P1	0.0313 (3)	0.0385 (3)	0.0308 (3)	0.00411 (19)	0.0142 (2)	0.0013 (2)
S1	0.0241 (2)	0.0263 (2)	0.0343 (3)	−0.00034 (15)	0.01395 (19)	0.00146 (16)
N1	0.0460 (10)	0.0390 (10)	0.0458 (11)	−0.0092 (8)	0.0305 (9)	−0.0062 (8)
O1	0.0359 (7)	0.0375 (8)	0.0371 (8)	−0.0088 (6)	0.0176 (6)	−0.0062 (6)
O2	0.0320 (7)	0.0384 (8)	0.0543 (9)	0.0098 (6)	0.0210 (7)	0.0140 (7)
O3	0.0413 (8)	0.0406 (8)	0.0311 (7)	0.0107 (6)	0.0126 (6)	−0.0017 (6)
O4	0.0515 (9)	0.0581 (10)	0.0415 (8)	0.0041 (8)	0.0280 (7)	0.0036 (8)
O5	0.0340 (8)	0.0555 (10)	0.0503 (10)	0.0032 (7)	0.0065 (7)	−0.0052 (8)
C1	0.0257 (8)	0.0337 (9)	0.0300 (9)	0.0009 (7)	0.0115 (7)	0.0019 (7)
C2	0.0365 (11)	0.0409 (11)	0.0571 (14)	−0.0054 (9)	0.0174 (10)	−0.0132 (10)
C3	0.0370 (11)	0.0575 (15)	0.0651 (16)	−0.0168 (11)	0.0124 (11)	−0.0087 (13)
C4	0.0285 (10)	0.0703 (16)	0.0541 (14)	0.0023 (11)	0.0153 (10)	0.0073 (13)
C5	0.0360 (11)	0.0663 (16)	0.0472 (13)	0.0121 (11)	0.0206 (10)	0.0021 (12)
C6	0.0334 (10)	0.0450 (11)	0.0389 (11)	0.0060 (9)	0.0136 (8)	−0.0042 (9)
C7	0.0610 (16)	0.0568 (15)	0.082 (2)	−0.0038 (13)	0.0498 (16)	−0.0032 (15)
C8	0.0541 (15)	0.0649 (18)	0.0486 (15)	−0.0044 (12)	0.0084 (12)	−0.0119 (12)

Ca1—O3i	2.3055 (15)	O5—C8	1.443 (3)
Ca1—O3	2.3055 (15)	C1—C6	1.377 (3)
Ca1—O2i	2.3392 (15)	C1—C2	1.391 (3)
Ca1—O2	2.3392 (15)	C2—C3	1.386 (3)
Ca1—O1	2.3802 (14)	C2—H2	0.9300
Ca1—O1i	2.3802 (14)	C3—C4	1.375 (4)
Ca1—P1i	3.4863 (6)	C3—H3	0.9300
Ca1—P1	3.4863 (6)	C4—C5	1.387 (4)
P1—O3	1.4801 (15)	C4—H4	0.9300
P1—O5	1.5664 (17)	C5—C6	1.389 (3)
P1—O4	1.5748 (17)	C5—H5	0.9300
P1—N1i	1.6043 (19)	C6—H6	0.9300
S1—O2ii	1.4547 (15)	C7—H7C	0.9600
S1—O1	1.4603 (14)	C7—H7B	0.9600
S1—N1	1.5370 (19)	C7—H7A	0.9600
S1—C1	1.7695 (19)	C8—H8C	0.9600
N1—P1i	1.6043 (19)	C8—H8B	0.9600
O2—S1iii	1.4547 (15)	C8—H8A	0.9600
O4—C7	1.437 (4)
O3i—Ca1—O3	152.17 (8)	O1—S1—N1	115.20 (9)
O3i—Ca1—O2i	101.74 (5)	O2ii—S1—C1	105.07 (9)
O3—Ca1—O2i	97.69 (6)	O1—S1—C1	106.42 (9)
O3i—Ca1—O2	97.69 (6)	N1—S1—C1	107.50 (11)
O3—Ca1—O2	101.74 (5)	S1—N1—P1i	127.01 (12)
O2i—Ca1—O2	90.94 (8)	S1—O1—Ca1	133.51 (9)
O3i—Ca1—O1	79.32 (5)	S1iii—O2—Ca1	138.86 (9)
O3—Ca1—O1	81.97 (6)	P1—O3—Ca1	132.93 (9)
O2i—Ca1—O1	177.86 (5)	C7—O4—P1	119.51 (17)
O2—Ca1—O1	87.07 (5)	C8—O5—P1	120.50 (17)
O3i—Ca1—O1i	81.97 (6)	C6—C1—C2	121.22 (19)
O3—Ca1—O1i	79.32 (5)	C6—C1—S1	120.38 (15)
O2i—Ca1—O1i	87.07 (5)	C2—C1—S1	118.40 (15)
O2—Ca1—O1i	177.86 (5)	C3—C2—C1	118.5 (2)
O1—Ca1—O1i	94.93 (8)	C1—C2—H2	120.6
O3i—Ca1—P1i	18.11 (4)	C3—C2—H2	120.6
O3—Ca1—P1i	136.46 (4)	C4—C3—C2	121.0 (2)
O2i—Ca1—P1i	119.57 (4)	C4—C3—H3	119.7
O2—Ca1—P1i	99.47 (4)	C2—C3—H3	119.7
O1—Ca1—P1i	61.60 (4)	C3—C4—C5	119.9 (2)
O1i—Ca1—P1i	80.87 (4)	C3—C4—H4	120.0
O3i—Ca1—P1	136.46 (4)	C5—C4—H4	120.0
O3—Ca1—P1	18.11 (4)	C4—C5—C6	120.1 (2)
O2i—Ca1—P1	99.47 (4)	C4—C5—H5	119.9
O2—Ca1—P1	119.57 (4)	C6—C5—H5	119.9
O1—Ca1—P1	80.87 (4)	C1—C6—C5	119.3 (2)
O1i—Ca1—P1	61.60 (4)	C1—C6—H6	120.4
P1i—Ca1—P1	124.04 (2)	C5—C6—H6	120.4
O3—P1—O5	111.87 (10)	O4—C7—H7C	109.5
O3—P1—O4	112.15 (10)	O4—C7—H7B	109.5
O5—P1—O4	102.01 (10)	H7C—C7—H7B	109.5
O3—P1—N1i	117.84 (9)	O4—C7—H7A	109.5
O5—P1—N1i	106.83 (10)	H7C—C7—H7A	109.5
O4—P1—N1i	104.71 (10)	H7B—C7—H7A	109.5
O3—P1—Ca1	28.96 (6)	O5—C8—H8C	109.5
O5—P1—Ca1	118.53 (8)	O5—C8—H8B	109.5
O4—P1—Ca1	130.87 (7)	H8C—C8—H8B	109.5
N1i—P1—Ca1	89.68 (7)	O5—C8—H8A	109.5
O2ii—S1—O1	112.75 (9)	H8C—C8—H8A	109.5
O2ii—S1—N1	109.23 (10)	H8B—C8—H8A	109.5
O3i—Ca1—P1—O3	155.86 (11)	P1—Ca1—O1—S1	106.66 (12)
O2i—Ca1—P1—O3	−85.79 (14)	O3i—Ca1—O2—S1iii	52.16 (15)
O2—Ca1—P1—O3	10.74 (14)	O3—Ca1—O2—S1iii	−147.87 (15)
O1—Ca1—P1—O3	92.07 (14)	O2i—Ca1—O2—S1iii	−49.81 (12)
O1i—Ca1—P1—O3	−167.21 (14)	O1—Ca1—O2—S1iii	130.96 (15)
P1i—Ca1—P1—O3	138.45 (14)	P1i—Ca1—O2—S1iii	70.39 (15)
O3i—Ca1—P1—O5	−120.27 (10)	P1—Ca1—O2—S1iii	−151.26 (13)
O3—Ca1—P1—O5	83.87 (16)	O5—P1—O3—Ca1	−109.73 (13)
O2i—Ca1—P1—O5	−1.92 (9)	O4—P1—O3—Ca1	136.34 (13)
O2—Ca1—P1—O5	94.62 (9)	N1i—P1—O3—Ca1	14.66 (17)
O1—Ca1—P1—O5	175.94 (9)	O3i—Ca1—O3—P1	−37.12 (12)
O1i—Ca1—P1—O5	−83.34 (9)	O2i—Ca1—O3—P1	96.95 (13)
P1i—Ca1—P1—O5	−137.68 (8)	O2—Ca1—O3—P1	−170.47 (13)
O3i—Ca1—P1—O4	98.13 (11)	O1—Ca1—O3—P1	−85.18 (13)
O3—Ca1—P1—O4	−57.74 (17)	O1i—Ca1—O3—P1	11.43 (13)
O2i—Ca1—P1—O4	−143.52 (10)	P1i—Ca1—O3—P1	−52.92 (16)
O2—Ca1—P1—O4	−46.99 (11)	O3—P1—O4—C7	−72.2 (2)
O1—Ca1—P1—O4	34.34 (10)	O5—P1—O4—C7	167.92 (19)
O1i—Ca1—P1—O4	135.05 (11)	N1i—P1—O4—C7	56.7 (2)
P1i—Ca1—P1—O4	80.71 (10)	Ca1—P1—O4—C7	−46.0 (2)
O3i—Ca1—P1—N1i	−11.21 (9)	O3—P1—O5—C8	−43.3 (2)
O3—Ca1—P1—N1i	−167.07 (15)	O4—P1—O5—C8	76.7 (2)
O2i—Ca1—P1—N1i	107.14 (8)	N1i—P1—O5—C8	−173.7 (2)
O2—Ca1—P1—N1i	−156.32 (9)	Ca1—P1—O5—C8	−74.6 (2)
O1—Ca1—P1—N1i	−75.00 (8)	O2ii—S1—C1—C6	−118.55 (18)
O1i—Ca1—P1—N1i	25.72 (9)	O1—S1—C1—C6	1.2 (2)
P1i—Ca1—P1—N1i	−28.62 (7)	N1—S1—C1—C6	125.18 (18)
O2ii—S1—N1—P1i	145.87 (15)	O2ii—S1—C1—C2	61.4 (2)
O1—S1—N1—P1i	17.8 (2)	O1—S1—C1—C2	−178.77 (18)
C1—S1—N1—P1i	−100.63 (16)	N1—S1—C1—C2	−54.8 (2)
O2ii—S1—O1—Ca1	−100.86 (13)	C6—C1—C2—C3	1.3 (4)
N1—S1—O1—Ca1	25.45 (16)	S1—C1—C2—C3	−178.7 (2)
C1—S1—O1—Ca1	144.47 (12)	C1—C2—C3—C4	0.2 (4)
O3i—Ca1—O1—S1	−34.37 (12)	C2—C3—C4—C5	−0.9 (5)
O3—Ca1—O1—S1	124.94 (13)	C3—C4—C5—C6	0.2 (4)
O2—Ca1—O1—S1	−132.76 (13)	C2—C1—C6—C5	−1.9 (3)
O1i—Ca1—O1—S1	46.48 (10)	S1—C1—C6—C5	178.06 (18)
P1i—Ca1—O1—S1	−30.35 (10)	C4—C5—C6—C1	1.2 (4)

Ca1—O3	2.3055 (15)
Ca1—O2	2.3392 (15)
Ca1—O1	2.3802 (14)

O3i—Ca1—O3	152.17 (8)
O3—Ca1—O1	81.97 (6)
O2i—Ca1—O1	177.86 (5)

Symmetry code: (i) .