Poly[[μ-(1-ammonio-ethane-1,1-di-yl)bis-(hydrogenphospho-nato)]diaquachloridodisodium]: a powder X-ray diffraction study.

The title compound, [Na(2)(C(2)H(8)NO(6)P(2))Cl(H(2)O)(2)](n), has a polymeric two-dimensional structure extending parallel to (001). The asymmetric unit contains two Na(+) cations located on a centre of symmetry and on a mirror plane, respectively, one half of a bis-phospho-nate anion (the entire anion is completed by mirror symmetry), one chloride anion on a mirror plane and one water mol-ecule in general positions. The two Na(+) cations exhibit distorted octa-hedral NaCl(2)O(4) coordination polyhedra, each consisting of two deprotonated O atoms of the bis-phospho-nate anion, of two water mol-ecules and of two chloride anions. Strong O-H⋯O hydrogen bonds between the -OH group and one of the free O atoms of the bis-phospho-nate anion connect adjacent layers along [100], supported by N-H⋯Cl inter-actions. Intra-layer O-H⋯O and N-H⋯O hydrogen bonds are also observed.

Related literature

For general ban class="Chemical">ckgrounpan>d to the use of organin class="Chemical">c diphospho­nic acids as chelating agents in metal extraction and as drugs to prevent calcification and to inhibit bone resorption, see: Matczak-Jon & Videnova-Adrabinska (2005 ▶); Tromelin et al. (1986 ▶); Szabo et al. (2002 ▶). For related structures, see: Bon et al. (2008 ▶); Maltezou et al. (2010 ▶). For standard bond lengths, see: Allen et al. (1987 ▶). For background and details of methods applied in data collection and Rietveld refinement, see: Thompson et al. (1987 ▶); Finger et al. (1994 ▶); Stephens (1999 ▶); Von Dreele (1997 ▶); Boultif & Louër (2004 ▶); Rodriguez-Carvajal (2001 ▶); Roisnel & Rodriguez-Carvajal (2001 ▶); Toby (2001 ▶). For the Le Bail method, see: Le Bail et al. (1988 ▶).

Experimental

Crystal data

[n class="Chemical">Na2(C2H8NO6P2)Cl(H2O)2]

M = 321.50

Monon class="Chemical">clinin class="Chemical">c,

a = 5.53806 (4) Å

b = 10.50365 (8) Å

n class="Chemical">c = 10.2096 (1) Å

β = 104.0764 (7)°

V = 576.06 (1) Å3

Z = 2

n class="Chemical">Cu Kα1 radiationpan>

λ = 1.5406 Å

μ = 6.62 mm−1

T = 298 K

Flat sheet, 8 × 8 mm

Data collection

STOE Transmission STADI P diffran class="Chemical">ctometer

Spen class="Chemical">cimen mounting: powder loaded between two Mylar foils

Data n class="Chemical">collen class="Chemical">ction mode: transmission

Sn class="Chemical">canpan> method: step

Absorption correction: for a cylinder mounted on the ϕ axis Absorption/surface roughness correction: function number 4 in GSAS (Larson & Von Dreele, 2004 ▶). Flat plate transmission absorption correction, terms = 0.51550 0.0000, correction is not refined. T min = 0.318, T max = 0.451

2θmin = 7.00°, 2θmax = 91.98°, 2θstep = 0.02°

Refinement

R p = 0.029

R wp = 0.038

R exp = 0.029

R(F 2) = 0.0257

χ2 = 1.769

4250 data points

109 parameters

10 restraints

n class="Disease">H atoms treated by a mixture of independent and n class="Chemical">constrained refinement

Data n class="Chemical">collection: WinXPOW (Stoe & Cie, 1999 ▶); cell refinement: GSAS (Larson & Von Dreele, 2004 ▶); data reduction: WinXPOW; program(s) used to solve structure: EXPO2009 (Altomare et al., 2009 ▶); program(s) used to refine structure: GSAS; molecular graphics: ORTEP-3 (Farrugia, 1997 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

n class="Chemical">Crystal strun class="Chemical">cture: contains datablock(s) global, I. DOI: 10.1107/S1600536812018077/wm2620sup1.cif

Rietveld powder data: n class="Chemical">contains datablon class="Chemical">ck(s) I. DOI: 10.1107/S1600536812018077/wm2620Isup2.rtv

Additional supplementary materials: n class="Chemical">crystallographin class="Chemical">c information; 3D view; checkCIF report

[Na2(C2H8NO6P2)Cl(H2O)2]	Dx = 1.854 Mg m−3
Mr = 321.50	Melting point: 623 K
Monoclinic, P21/m	Cu Kα1 radiation, λ = 1.5406 Å
Hall symbol: -P 2yb	µ = 6.62 mm−1
a = 5.53806 (4) Å	T = 298 K
b = 10.50365 (8) Å	Particle morphology: Fine powder
c = 10.2096 (1) Å	white
β = 104.0764 (7)°	flat sheet, 8 × 8 mm
V = 576.06 (1) Å3	Specimen preparation: Prepared at 298 K and 101.3 kPa
Z = 2

STOE Transmission STADI P diffractometer	Scan method: step
Radiation source: sealed X-ray tube	Absorption correction: for a cylinder mounted on the φ axis Absorption/surface roughness correction: function number 4 in GSAS (Larson & Von Dreele, 2004). Flat plate transmission absorption correction, terms = 0.51550 0.0000, correction is not refined.
Curved Ge(111) monochromator	Tmin = 0.318, Tmax = 0.451
Specimen mounting: powder loaded between two Mylar foils	2θmin = 7.00°, 2θmax = 91.98°, 2θstep = 0.02°
Data collection mode: transmission

Least-squares matrix: full	Profile function: CW Profile function number 4 with 21 terms Pseudovoigt profile coefficients as parameterized in Thompson et al. (1987) Asymmetry correction of Finger et al. (1994). Microstrain broadening by Stephens (1999). #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 11.529 #4(GP) = 0.000 #5(LX) = 0.000 #6(ptec) = 2.91 #7(trns) = 0.00 #8(shft) = -1.5788 #9(sfec) = 0.00 #10(S/L) = 0.0215 #11(H/L) = 0.0215 #12(eta) = 0.6000 #13(S400 ) = 2.1E-01 #14(S040 ) = 2.3E-02 #15(S004 ) = 1.2E-02 #16(S220 ) = 4.2E-02 #17(S202 ) = 4.6E-02 #18(S022 ) = 1.7E-03 #19(S301 ) = 8.7E-02 #20(S103 ) = -3.8E-05 #21(S121 ) = 2.8E-03 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.029	109 parameters
Rwp = 0.038	10 restraints
Rexp = 0.029	0 constraints
R(F2) = 0.0257	H atoms treated by a mixture of independent and constrained refinement
χ2 = 1.769	(Δ/σ)max = 0.08
4250 data points	Background function: GSAS Background function number 1 with 20 terms. Shifted Chebyshev function of 1st kind 1: 914.240 2: -1034.48 3: 577.328 4: -206.578 5: 31.4580 6: 15.1650 7: -17.0889 8: 0.311333 9: 15.3490 10: -12.5113 11: 3.19417 12: 9.78413 13: -11.5493 14: 7.63897 15: -0.448352 16: -4.70971 17: 6.05628 18: -4.89696 19: 6.60474 20: -2.48023
Excluded region(s): none	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 1.12753 h= 0.000 k= 0.000 l= 1.000 Prefered orientation correction range: Min= 0.69761, Max= 1.19727

Experimental. All chemical reagents and solvents were of commercial quality and used as received. NMR spectra were recorded on a Bruker Bio spin 400 spectrometer (400 MHz for 1H, 100 MHz for 13C, 162 MHz for 31P). Chemical shifts (δ) were expressed in p.p.m. relative to TMS as an internal standard. IR spectra were recorded on FTIR-JASCO 300E. Melting points were determined using a Stuart SMP3 melting point apparatus. The powder sample of compound (I) was slightly ground in a mortar, loaded into two foils of Mylar and fixed in the sample holder with a mask of suitable internal diameter (8.0 mm). X-ray powder diffraction patterns were obtained on a Stoe Stadi-P diffractometer with monochromatic Cu Kα1 radiation (λ = 1.5406 Å) selected using an incident-beam curved-crystal germanium Ge(111) monochromator, using the Stoe transmission geometry (horizontal set-up) with a linear position-sensitive detector (PSD). The pattern was scanned over the angular range 7–92° (2θ)The sample was ground lightly in a mortar, loaded between two Mylar foils and fixed in the sample holder with a mask of 8.0 mm internal diameter.

	x	y	z	Uiso*/Ueq
P1	0.1295 (3)	0.10112 (14)	0.1805 (2)	0.01656
Cl1	0.6926 (3)	0.25	0.5220 (2)	0.02613
Na1	0.5	0.0	0.5	0.03054
Na2	0.1724 (5)	0.25	0.5042 (3)	0.02699
O1	0.1724 (6)	0.0974 (3)	0.3308 (4)	0.0137 (11)*
O2	−0.1356 (6)	0.0911 (3)	0.0983 (4)	0.0137 (11)*
O3	0.2987 (8)	−0.0041 (4)	0.1397 (4)	0.0164 (11)*
O1w	0.2545 (8)	0.0669 (4)	0.6478 (5)	0.0326 (13)*
N1	0.5321 (15)	0.25	0.1977 (9)	0.022 (2)*
C1	0.2590 (13)	0.25	0.1280 (8)	0.009 (3)*
C2	0.2359 (11)	0.25	−0.0250 (6)	0.007 (2)*
H1c2	0.0613 (15)	0.25	−0.0726 (10)	0.009 (3)*
H2c2	0.315 (2)	0.1743 (6)	−0.0494 (10)	0.009 (3)*
H1n1	0.608 (7)	0.185 (3)	0.173 (5)	0.033 (3)*
H2n1	0.576 (11)	0.25	0.2855 (10)	0.033 (3)*
H3	0.252 (8)	−0.040 (3)	0.0666 (19)	0.0246 (17)*
H1w	0.132 (5)	0.021 (4)	0.639 (5)	0.0488 (19)*
H2w	0.337 (7)	0.077 (4)	0.7255 (17)	0.0488 (19)*

	U11	U22	U33	U12	U13	U23
P1	0.0136 (12)	0.0168 (12)	0.0188 (16)	−0.0016 (11)	0.0031 (12)	−0.0026 (13)
Cl1	0.0162 (17)	0.0362 (17)	0.024 (2)	0.0	0.0015 (16)	0.0
Na1	0.037 (3)	0.031 (3)	0.031 (3)	0.008 (2)	0.022 (3)	0.007 (3)
Na2	0.027 (2)	0.030 (2)	0.024 (3)	0.0	0.004 (2)	0.0

P1—O1	1.495 (4)	N1—H2n1	0.870 (14)
P1—O2	1.507 (4)	Na1—Cl1	2.8226 (7)
P1—O3	1.570 (4)	Na2—Cl1i	2.707 (3)
P1—C1	1.853 (4)	Na2—Cl1	2.842 (3)
C2—C1	1.537 (9)	Na1—O1	2.408 (3)
C2—H1c2	0.971 (11)	Na1—O1w	2.370 (5)
C2—H2c2	0.969 (9)	Na2—O1	2.389 (4)
N1—C1	1.507 (10)	Na2—O1w	2.394 (5)
N1—H1n1	0.87 (3)
O1—P1—O2	117.4 (2)	Cl1—Na1—O1w	86.43 (10)
O1—P1—O3	107.4 (2)	Cl1—Na1—O1wiii	93.57 (10)
O1—P1—C1	110.0 (3)	O1—Na2—O1ii	84.3 (2)
O2—P1—O3	111.5 (2)	O1—Na2—O1w	83.14 (14)
O2—P1—C1	106.9 (3)	O1—Na2—O1wii	163.5 (2)
O3—P1—C1	102.7 (3)	O1w—Na2—O1wii	106.9 (3)
P1—C1—P1ii	115.1 (4)	Cl1i—Na2—Cl1	172.72 (18)
P1—C1—N1	106.1 (4)	Cl1i—Na2—O1	103.11 (14)
P1—C1—C2	110.6 (3)	Cl1i—Na2—O1v	92.54 (2)
N1—C1—C2	107.8 (7)	Cl1i—Na2—O1w	90.14 (14)
C1—C2—H1c2	109.6 (4)	Cl1i—Na2—O1wv	90.02 (3)
C1—C2—H2c2	109.3 (4)	Na1—Cl1—Na1vi	136.97 (7)
H1c2—C2—H2c2	109.3 (5)	Na1—Cl1—Na2	68.74 (4)
H2c2—C2—H2c2ii	110.1 (11)	Na1—Cl1—Na2vii	110.65 (4)
C1—N1—H1n1	111 (4)	Na2—Cl1—Na2vii	172.72 (18)
C1—N1—H2n1	119 (4)	P1—O1—Na1	130.6 (2)
H1n1—N1—H1n1ii	103 (5)	P1—O1—Na2	135.7 (2)
H1n1—N1—H2n1	105 (4)	Na1—O1—Na2	83.63 (13)
O1—Na1—O1iii	180.0	Na1—O1w—Na2	84.34 (16)
O1—Na1—O1w	83.23 (13)	Na1—O1w—H1w	110 (4)
O1—Na1—O1wiii	96.77 (13)	Na1—O1w—H2w	113 (4)
O1w—Na1—O1wiii	180.0	Na2—O1w—H1w	112 (4)
Cl1—Na1—Cl1iv	180.0	Na2—O1w—H2w	118 (3)
Cl1—Na1—O1	82.29 (9)	H1w—O1w—H2w	116 (4)
Cl1—Na1—O1iii	97.71 (9)
Na2—Cl1—Na1—O1	43.53 (11)	Cl1—Na1—O1—Na2	−50.23 (10)
Na2—Cl1—Na1—O1W	−40.11 (13)	O1W—Na1—O1—P1	−174.5 (3)
Na1—Cl1—Na2—O1	−43.99 (9)	O1W—Na1—O1—Na2	37.07 (14)
Na1—Cl1—Na2—O1W	39.68 (12)	Cl1iv—Na1—O1—P1	−81.8 (2)
O2—P1—O1—Na1	142.2 (2)	O1Wiii—Na1—O1—P1	5.5 (3)
O2—P1—O1—Na2	−85.9 (3)	O1Wiii—Na1—O1—Na2	−142.93 (14)
O3—P1—O1—Na1	15.7 (3)	Cl1—Na1—O1W—Na2	45.75 (12)
O3—P1—O1—Na2	147.7 (3)	O1—Na1—O1W—Na2	−36.91 (13)
C1—P1—O1—Na1	−95.3 (3)	O1iii—Na1—O1W—Na2	143.09 (13)
C1—P1—O1—Na2	36.7 (4)	Cl1—Na2—O1—P1	−95.6 (3)
O1—P1—C1—N1	58.6 (5)	Cl1—Na2—O1—Na1	49.77 (8)
O1—P1—C1—C2	175.2 (4)	O1W—Na2—O1—P1	178.0 (3)
O1—P1—C1—P1ii	−58.5 (5)	O1W—Na2—O1—Na1	−36.65 (14)
O2—P1—C1—N1	−172.9 (4)	Cl1i—Na2—O1—P1	89.4 (3)
O2—P1—C1—C2	−56.3 (5)	O1ii—Na2—O1—P1	−12.7 (3)
O2—P1—C1—P1ii	70.0 (5)	O1ii—Na2—O1—Na1	132.66 (13)
O3—P1—C1—N1	−55.5 (5)	Cl1—Na2—O1W—Na1	−45.41 (11)
O3—P1—C1—C2	61.2 (5)	O1—Na2—O1W—Na1	37.27 (14)
O3—P1—C1—P1ii	−172.6 (4)	O1Wii—Na2—O1W—Na1	−129.37 (17)
Cl1—Na1—O1—P1	98.2 (2)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3···O2viii	0.82 (2)	1.74 (2)	2.547 (6)	170 (4)
O1W—H1W···O1ix	0.82 (3)	2.18 (4)	2.978 (6)	166 (5)
O1W—H2W···O3iii	0.82 (2)	2.28 (3)	2.942 (6)	138 (3)
N1—H1N1···O2vii	0.87 (3)	2.02 (4)	2.848 (8)	158 (3)
N1—H2N1···Cl1	0.87 (3)	2.34 (1)	3.213 (9)	180 (3)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H3⋯O2i	0.82 (2)	1.74 (2)	2.547 (6)	170 (4)
O1W—H1W⋯O1ii	0.82 (3)	2.18 (4)	2.978 (6)	166 (5)
O1W—H2W⋯O3iii	0.82 (2)	2.28 (3)	2.942 (6)	138 (3)
N1—H1N1⋯O2iv	0.87 (3)	2.02 (4)	2.848 (8)	158 (3)
N1—H2N1⋯Cl1	0.87 (3)	2.34 (1)	3.213 (9)	180 (3)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) .