Poly[{μ₁₀-[(phosphono­meth­yl)imino­dimethyl­ene]diphospho­nato}dithallium(I)]

The title compound, [Tl₂(C₃H₁₀NO₉P₃)]_n, a Tl^I organic–inorganic hybrid complex, was synthesized by the reaction of nitrilo­tris(methyl­enephospho­nic acid) with thallium(I) nitrate. There are two types of Tl⁺ ions in the complex, with coordination numbers of eight and seven and with stereochemically active and inactive lone-pair electrons, respectively. In the crystal, the doubly deprotonated ligands form two-dimensional hydrogen-bonded layers through O—H...O hydrogen bonds. The NH group is involved in a trifurcated intra­molecular hydrogen bond. Coordination of the phospho­nate ligands to the Tl⁺ ions creates a three-dimensional structure.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](N-C) = 0.008 Å
• R factor = 0.025
• wR factor = 0.055
• Data-to-parameter ratio = 16.8

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       3.05 Ratio
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       4.00 Ratio

Alert level G
ABSTM02_ALERT_3_G  The ratio of expected to reported Tmax/Tmin(RR) is > 1.50
            Tmin and Tmax reported:      0.104     0.183
            Tmin and Tmax expected:      0.027     0.076
            RR =      1.616
            Please check that your absorption correction is appropriate.
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......         12
PLAT154_ALERT_1_G The su's on the Cell Angles are Equal  (x 10000)        100 Deg.
PLAT180_ALERT_4_G Check Cell Rounding: # of Values Ending with 0 =          3
PLAT764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.43 Ratio
PLAT793_ALERT_4_G The Model has Chirality at N1      (Verify) ....          S

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

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   3 ALERT type 3 Indicator that the structure quality may be low
   3 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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S1. Comment

Metal phosphonate complexes of the ligand nitrilotris(methylenephosphonic acid (H6L), giving two different types of 1:1 (M/L) metal phosphonate complexes, M[NH(CH₂PO₃H)₃(H₂O)₃](M = Mn, Co, Ni, Cu, Zn, Cd), with two-dimensional hydrogen-bonded layered structures, have been prepared previously by (Sharma et al., 2001).

In the structure of the title compound, synthesized by the reaction of the same ligand with thallium(I) nitrate, the nitrilotris(methylenephosphonate) (H4L^2-) group is doublely deprotonated and two different environments for the Thallium atoms are observed, as shown in Figs. 1 and 2. Eight O-atoms of five H4L^2- phosphonate ligands are coordinated to the Tl1 ion (Fig. 1), while seven oxygen atoms of five H4L^2- phosphonate ligands are coordinated to the Tl2 ion (Fig. 2).

The conformation of the doublely deprotonated nitrilotris(methylenephosphonate) ligand is illustrated in Fig. 3. The hydrogen atoms on atoms O1 and O2 are positionally disordered with relative occupancies of 0.5:0.5. Each H4L^2- dianion links to five Tl1 and five Tl2 ions (Fig. 4).

The doublely deprotonated H4L^2- ligand forms two-dimensional hydrogen bonded layers via O—H···O hydrogen bonds involving hydroxyl groups O1, O2, O6 and O7 (Table 1 and Fig. 5). Atoms O3, O5 and O8 do not contribute in this type of hydrogen bond, rather they coordinate only to the Tl⁺ions. The NH group is involved in a 4-centre trifurcated intramolecular hydrogen bond with O-atoms O3, O5 and O8 (Table 1). Coordination of the ligand to the metal ions in the interlayer space creates a three-dimensional structure (Fig. 6).

Related literature

For related metal phosphonate complexes of the same ligand, see: Sharma et al. (2001).

S2. Experimental

Thallium(I)nitrate (0.133 g, 0.5 mmol) was added in several portions to a solution of nitrilotris(methylenephosphonicacid) (H6L) (0.104 g, 0.35 mmol) in 12 ml of a deionized water-ethanol mixture (3:5). The solution was stirred for seven days and a white precipitate was obtained. This was filtered off and recrystallized from deionized water at rt. Colorless prism-like crystals of the title compound were obtained in 68% yield (based on the Tl atom). Elemental analysis for Tl₂(H₄L), C₃H₁₀NO₉P₃Tl₂:C, 5.06; H, 1.36; N, 2.03%. Calc.: C, 5.10; H, 1.41; N, 1.98%.

S3. Refinement

The NH and OH H-atoms were located in a difference electron-density map and were refined with distance restraints: O—H = 0.82 (2) and N—H = 0.86 (2) Å, with U_iso(H) = 1.2U_eq(N,O). The C-bound H atoms were positioned geometrically and refined using a riding model: C—H = 0.99 Å, with U_iso(H) = 1.2 times U_eq(C).

Computing details

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures

	Fig. 1. Environment of the Tl1 atom.
	Fig. 2. Environment of the Tl2 atom.
	Fig. 3. The conformation of the doubly deprotonated nitrilotris(methylenephosphonate) ligand.
	Fig. 4. Each H4L^2- dianion links to five Tl1 and five Tl2 ions.
	Fig. 5. Two-dimensional hydrogen-bonded layers formed via O—H···O hydrogen bonds involving hydroxyl groups.
	Fig. 6. The three-dimensional structure resulting from the coordination of the ligand to the metal ions in the interlayer space.
	Fig. 7. Reaction scheme.

Poly[{µ-[(phosphonomethyl)iminodimethylene]diphosphonato}dithallium(I)]

Crystal data

[Tl2(C3H10NO9P3)]	Z = 2
Mr = 705.77	F(000) = 628
Triclinic, P1	Dx = 3.691 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.9236 (6) Å	Cell parameters from 266 reflections
b = 8.0932 (6) Å	θ = 3–26°
c = 10.9136 (8) Å	µ = 25.76 mm^−1
α = 81.422 (1)°	T = 100 K
β = 79.023 (1)°	Prism, colorless
γ = 68.085 (1)°	0.16 × 0.14 × 0.10 mm
V = 635.06 (8) Å^3

Data collection

Bruker APEXII CCD area-detector diffractometer	2744 independent reflections
Radiation source: fine-focus sealed tube	2437 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.029
ω scans	θmax = 27.0°, θmin = 1.9°
Absorption correction: numerical (XPREP; Bruker, 2007)	h = −10→10
Tmin = 0.104, Tmax = 0.183	k = −10→10
6627 measured reflections	l = −13→13

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)] = 0.025	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.055	H-atom parameters constrained
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0225P)^2 + 1.104P] where P = (Fo^2 + 2Fc^2)/3
2744 reflections	(Δ/σ)max = 0.003
163 parameters	Δρmax = 1.72 e Å^−3
12 restraints	Δρmin = −1.83 e Å^−3

Special details

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	Occ. (<1)
Tl1	0.29076 (3)	−0.05875 (3)	0.25484 (2)	0.01064 (7)
Tl2	0.23248 (3)	0.24843 (3)	0.54672 (2)	0.01703 (8)
P1	0.7521 (3)	0.2462 (3)	0.42352 (16)	0.0201 (4)
P2	0.7554 (2)	−0.0669 (2)	0.10302 (14)	0.0090 (3)
P3	0.2557 (2)	0.4329 (2)	0.20298 (14)	0.0091 (3)
O1	0.6684 (8)	0.4387 (7)	0.4597 (5)	0.0331 (13)
H1O	0.5753	0.4894	0.5072	0.040*	0.50
O2	0.9424 (7)	0.1622 (8)	0.4631 (5)	0.0311 (12)
H2O	0.9828	0.0586	0.4936	0.037*	0.50
O3	0.6291 (6)	0.1391 (5)	0.4655 (4)	0.0119 (9)
O4	0.7469 (6)	−0.1263 (6)	−0.0199 (4)	0.0148 (9)
O5	0.6365 (6)	−0.1126 (6)	0.2173 (4)	0.0151 (9)
O6	0.9564 (6)	−0.1194 (5)	0.1274 (4)	0.0129 (9)
H6O	1.0047	−0.2157	0.1660	0.015*
O7	0.2360 (6)	0.4303 (6)	0.0624 (4)	0.0145 (9)
H7O	0.2418	0.3313	0.0485	0.017*
O8	0.2641 (6)	0.2594 (5)	0.2794 (4)	0.0108 (8)
O9	0.1203 (6)	0.6039 (6)	0.2530 (4)	0.0141 (9)
N1	0.6274 (7)	0.2583 (6)	0.2032 (4)	0.0086 (10)
H1N	0.5590	0.2094	0.2560	0.010*
C1	0.7944 (8)	0.2553 (8)	0.2523 (6)	0.0116 (12)
H1A	0.8225	0.3638	0.2177	0.014*
H1B	0.9018	0.1497	0.2251	0.014*
C2	0.6768 (8)	0.1763 (8)	0.0791 (5)	0.0089 (11)
H2A	0.7749	0.2130	0.0257	0.011*
H2B	0.5677	0.2209	0.0351	0.011*
C3	0.4836 (8)	0.4433 (8)	0.1986 (6)	0.0111 (12)
H3A	0.5140	0.5133	0.1209	0.013*
H3B	0.4828	0.5047	0.2708	0.013*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Tl1	0.00946 (12)	0.01138 (12)	0.01117 (12)	−0.00463 (9)	−0.00049 (9)	−0.00006 (9)
Tl2	0.01643 (14)	0.01862 (14)	0.00967 (13)	−0.00101 (10)	0.00066 (10)	0.00088 (10)
P1	0.0291 (10)	0.0340 (10)	0.0090 (8)	−0.0260 (9)	−0.0018 (7)	0.0005 (7)
P2	0.0088 (7)	0.0092 (7)	0.0072 (7)	−0.0023 (6)	0.0003 (6)	0.0001 (6)
P3	0.0081 (7)	0.0095 (7)	0.0080 (7)	−0.0021 (6)	0.0001 (6)	0.0003 (6)
O1	0.048 (3)	0.031 (2)	0.028 (2)	−0.026 (2)	0.006 (2)	−0.0084 (19)
O2	0.023 (2)	0.051 (3)	0.027 (2)	−0.0233 (19)	−0.0095 (18)	0.0074 (19)
O3	0.011 (2)	0.012 (2)	0.013 (2)	−0.0062 (17)	−0.0001 (18)	0.0018 (17)
O4	0.023 (2)	0.010 (2)	0.011 (2)	−0.0034 (18)	−0.0045 (19)	−0.0010 (17)
O5	0.010 (2)	0.020 (2)	0.011 (2)	−0.0038 (18)	0.0011 (18)	0.0028 (18)
O6	0.010 (2)	0.010 (2)	0.015 (2)	−0.0028 (17)	−0.0031 (18)	0.0090 (17)
O7	0.020 (2)	0.012 (2)	0.011 (2)	−0.0045 (19)	−0.0062 (19)	0.0013 (17)
O8	0.010 (2)	0.009 (2)	0.012 (2)	−0.0033 (17)	0.0013 (17)	−0.0001 (16)
O9	0.011 (2)	0.013 (2)	0.014 (2)	0.0010 (18)	−0.0017 (18)	−0.0027 (18)
N1	0.009 (2)	0.011 (2)	0.007 (2)	−0.005 (2)	0.0031 (19)	−0.0031 (19)
C1	0.009 (3)	0.016 (3)	0.014 (3)	−0.007 (2)	−0.001 (2)	−0.004 (2)
C2	0.006 (3)	0.011 (3)	0.007 (3)	−0.001 (2)	0.002 (2)	−0.001 (2)
C3	0.010 (3)	0.012 (3)	0.009 (3)	−0.003 (2)	0.004 (2)	−0.006 (2)

Geometric parameters (Å, º)

Tl1—O8	2.555 (4)	P3—C3	1.830 (6)
Tl1—O5	2.569 (4)	O1—Tl2^iii	2.906 (5)
Tl1—O4^i	2.778 (4)	O1—H1O	0.8200
Tl1—O3^ii	3.159 (4)	O2—Tl2^vi	2.965 (5)
Tl2—O5^ii	2.870 (4)	O2—H2O	0.8201
Tl2—O8	2.871 (4)	O3—Tl2^ii	2.926 (4)
Tl2—O1^iii	2.906 (5)	O3—Tl1^ii	3.159 (4)
Tl2—O3	2.922 (4)	O4—Tl1^i	2.778 (4)
Tl2—O3^ii	2.926 (4)	O5—Tl2^ii	2.870 (4)
Tl2—O2^iv	2.965 (5)	O6—H6O	0.8200
Tl2—O9^v	3.159 (4)	O7—H7O	0.8201
P1—O3	1.501 (4)	O9—Tl2^v	3.159 (4)
P1—O2	1.522 (5)	N1—C3	1.506 (7)
P1—O1	1.529 (6)	N1—C1	1.510 (7)
P1—C1	1.829 (6)	N1—C2	1.517 (7)
P2—O5	1.502 (5)	N1—H1N	0.8699
P2—O4	1.512 (4)	C1—H1A	0.9900
P2—O6	1.552 (4)	C1—H1B	0.9900
P2—C2	1.823 (6)	C2—H2A	0.9900
P3—O9	1.503 (4)	C2—H2B	0.9900
P3—O8	1.507 (4)	C3—H3A	0.9900
P3—O7	1.576 (4)	C3—H3B	0.9900
O8—Tl1—O5	82.65 (14)	O9—P3—O7	109.6 (2)
O8—Tl1—O4^i	73.72 (13)	O8—P3—O7	112.4 (2)
O5—Tl1—O4^i	90.64 (13)	O9—P3—C3	105.9 (3)
O8—Tl1—O3^ii	84.83 (12)	O8—P3—C3	104.2 (3)
O5—Tl1—O3^ii	80.14 (12)	O7—P3—C3	105.6 (3)
O4^i—Tl1—O3^ii	157.62 (11)	P1—O1—Tl2^iii	140.5 (3)
O8—Tl1—Tl2	42.43 (9)	P1—O1—H1O	131.2
O5—Tl1—Tl2	88.38 (10)	Tl2^iii—O1—H1O	87.0
O4^i—Tl1—Tl2	115.70 (8)	P1—O2—Tl2^vi	142.9 (3)
O3^ii—Tl1—Tl2	44.31 (7)	P1—O2—H2O	122.8
O5^ii—Tl2—O8	153.26 (12)	Tl2^vi—O2—H2O	91.4
O5^ii—Tl2—O1^iii	90.93 (14)	P1—O3—Tl2	131.5 (2)
O8—Tl2—O1^iii	94.48 (13)	P1—O3—Tl2^ii	121.5 (2)
O5^ii—Tl2—O3	79.76 (12)	Tl2—O3—Tl2^ii	106.77 (13)
O8—Tl2—O3	76.90 (12)	P1—O3—Tl1^ii	95.14 (19)
O1^iii—Tl2—O3	72.87 (14)	Tl2—O3—Tl1^ii	91.85 (11)
O5^ii—Tl2—O3^ii	76.88 (12)	Tl2^ii—O3—Tl1^ii	86.74 (11)
O8—Tl2—O3^ii	84.01 (11)	P2—O4—Tl1^i	130.9 (2)
O1^iii—Tl2—O3^ii	145.49 (14)	P2—O5—Tl1	130.2 (2)
O3—Tl2—O3^ii	73.23 (13)	P2—O5—Tl2^ii	122.6 (2)
O5^ii—Tl2—O2^iv	123.69 (14)	Tl1—O5—Tl2^ii	106.85 (15)
O8—Tl2—O2^iv	66.41 (13)	P2—O6—H6O	119.1
O1^iii—Tl2—O2^iv	137.28 (16)	P3—O7—H7O	111.0
O3—Tl2—O2^iv	132.04 (14)	P3—O8—Tl1	141.1 (2)
O3^ii—Tl2—O2^iv	73.22 (14)	P3—O8—Tl2	118.2 (2)
O5^ii—Tl2—O9^v	76.06 (12)	Tl1—O8—Tl2	100.67 (13)
O8—Tl2—O9^v	129.64 (11)	P3—O9—Tl2^v	141.9 (3)
O1^iii—Tl2—O9^v	92.73 (14)	C3—N1—C1	111.4 (4)
O3—Tl2—O9^v	151.59 (11)	C3—N1—C2	112.6 (4)
O3^ii—Tl2—O9^v	114.72 (11)	C1—N1—C2	112.4 (4)
O2^iv—Tl2—O9^v	74.91 (13)	C3—N1—H1N	95.5
O5^ii—Tl2—Tl1	125.55 (9)	C1—N1—H1N	113.9
O8—Tl2—Tl1	36.90 (8)	C2—N1—H1N	109.9
O1^iii—Tl2—Tl1	129.09 (10)	N1—C1—P1	110.2 (4)
O3—Tl2—Tl1	79.78 (8)	N1—C1—H1A	109.6
O3^ii—Tl2—Tl1	48.95 (8)	P1—C1—H1A	109.6
O2^iv—Tl2—Tl1	52.33 (11)	N1—C1—H1B	109.6
O9^v—Tl2—Tl1	126.82 (8)	P1—C1—H1B	109.6
O3—P1—O2	115.2 (3)	H1A—C1—H1B	108.1
O3—P1—O1	114.5 (3)	N1—C2—P2	110.9 (4)
O2—P1—O1	108.2 (3)	N1—C2—H2A	109.5
O3—P1—C1	106.0 (3)	P2—C2—H2A	109.5
O2—P1—C1	104.8 (3)	N1—C2—H2B	109.5
O1—P1—C1	107.4 (3)	P2—C2—H2B	109.5
O5—P2—O4	117.4 (3)	H2A—C2—H2B	108.1
O5—P2—O6	111.2 (2)	N1—C3—P3	110.7 (4)
O4—P2—O6	112.0 (3)	N1—C3—H3A	109.5
O5—P2—C2	106.8 (3)	P3—C3—H3A	109.5
O4—P2—C2	104.8 (3)	N1—C3—H3B	109.5
O6—P2—C2	103.2 (3)	P3—C3—H3B	109.5
O9—P3—O8	118.1 (3)	H3A—C3—H3B	108.1
O8—Tl1—Tl2—O5^ii	−151.22 (18)	O5—P2—O4—Tl1^i	132.5 (3)
O5—Tl1—Tl2—O5^ii	−70.36 (17)	O6—P2—O4—Tl1^i	−97.0 (3)
O4^i—Tl1—Tl2—O5^ii	−160.29 (15)	C2—P2—O4—Tl1^i	14.2 (4)
O3^ii—Tl1—Tl2—O5^ii	7.15 (15)	O4—P2—O5—Tl1	−51.5 (4)
O5—Tl1—Tl2—O8	80.86 (17)	O6—P2—O5—Tl1	177.6 (3)
O4^i—Tl1—Tl2—O8	−9.07 (17)	C2—P2—O5—Tl1	65.7 (4)
O3^ii—Tl1—Tl2—O8	158.37 (18)	O4—P2—O5—Tl2^ii	136.2 (3)
O8—Tl1—Tl2—O1^iii	−23.9 (2)	O6—P2—O5—Tl2^ii	5.3 (3)
O5—Tl1—Tl2—O1^iii	56.95 (18)	C2—P2—O5—Tl2^ii	−106.6 (3)
O4^i—Tl1—Tl2—O1^iii	−32.99 (19)	O8—Tl1—O5—P2	−77.8 (3)
O3^ii—Tl1—Tl2—O1^iii	134.46 (19)	O4^i—Tl1—O5—P2	−4.3 (3)
O8—Tl1—Tl2—O3	−81.77 (16)	O3^ii—Tl1—O5—P2	−163.8 (3)
O5—Tl1—Tl2—O3	−0.90 (12)	Tl2—Tl1—O5—P2	−120.0 (3)
O4^i—Tl1—Tl2—O3	−90.84 (13)	O8—Tl1—O5—Tl2^ii	95.39 (16)
O3^ii—Tl1—Tl2—O3	76.60 (15)	O4^i—Tl1—O5—Tl2^ii	168.88 (15)
O8—Tl1—Tl2—O3^ii	−158.37 (18)	O3^ii—Tl1—O5—Tl2^ii	9.39 (13)
O5—Tl1—Tl2—O3^ii	−77.51 (15)	Tl2—Tl1—O5—Tl2^ii	53.19 (12)
O4^i—Tl1—Tl2—O3^ii	−167.44 (15)	O9—P3—O8—Tl1	137.8 (3)
O8—Tl1—Tl2—O2^iv	100.75 (19)	O7—P3—O8—Tl1	8.7 (5)
O5—Tl1—Tl2—O2^iv	−178.39 (16)	C3—P3—O8—Tl1	−105.1 (4)
O4^i—Tl1—Tl2—O2^iv	91.67 (17)	O9—P3—O8—Tl2	−39.7 (3)
O3^ii—Tl1—Tl2—O2^iv	−100.88 (17)	O7—P3—O8—Tl2	−168.8 (2)
O8—Tl1—Tl2—O9^v	109.29 (17)	C3—P3—O8—Tl2	77.3 (3)
O5—Tl1—Tl2—O9^v	−169.85 (14)	O5—Tl1—O8—P3	86.5 (4)
O4^i—Tl1—Tl2—O9^v	100.22 (15)	O4^i—Tl1—O8—P3	−6.3 (4)
O3^ii—Tl1—Tl2—O9^v	−92.34 (15)	O3^ii—Tl1—O8—P3	167.2 (4)
O3—P1—O1—Tl2^iii	173.5 (4)	Tl2—Tl1—O8—P3	−177.8 (5)
O2—P1—O1—Tl2^iii	43.6 (5)	O5—Tl1—O8—Tl2	−95.68 (14)
C1—P1—O1—Tl2^iii	−69.0 (5)	O4^i—Tl1—O8—Tl2	171.49 (16)
O3—P1—O2—Tl2^vi	−143.4 (4)	O3^ii—Tl1—O8—Tl2	−14.98 (12)
O1—P1—O2—Tl2^vi	−13.9 (6)	O5^ii—Tl2—O8—P3	−121.0 (3)
C1—P1—O2—Tl2^vi	100.4 (5)	O1^iii—Tl2—O8—P3	−20.0 (3)
O2—P1—O3—Tl2	144.1 (3)	O3—Tl2—O8—P3	−91.2 (2)
O1—P1—O3—Tl2	17.7 (4)	O3^ii—Tl2—O8—P3	−165.3 (3)
C1—P1—O3—Tl2	−100.5 (3)	O2^iv—Tl2—O8—P3	120.4 (3)
O2—P1—O3—Tl2^ii	−42.3 (4)	O9^v—Tl2—O8—P3	77.3 (3)
O1—P1—O3—Tl2^ii	−168.6 (3)	Tl1—Tl2—O8—P3	178.4 (3)
C1—P1—O3—Tl2^ii	73.1 (3)	O5^ii—Tl2—O8—Tl1	60.5 (3)
O2—P1—O3—Tl1^ii	47.0 (3)	O1^iii—Tl2—O8—Tl1	161.60 (16)
O1—P1—O3—Tl1^ii	−79.3 (3)	O3—Tl2—O8—Tl1	90.36 (14)
C1—P1—O3—Tl1^ii	162.5 (2)	O3^ii—Tl2—O8—Tl1	16.23 (13)
O5^ii—Tl2—O3—P1	−106.4 (3)	O2^iv—Tl2—O8—Tl1	−58.05 (16)
O8—Tl2—O3—P1	86.7 (3)	O9^v—Tl2—O8—Tl1	−101.10 (16)
O1^iii—Tl2—O3—P1	−12.2 (3)	O8—P3—O9—Tl2^v	−15.8 (5)
O3^ii—Tl2—O3—P1	174.3 (4)	O7—P3—O9—Tl2^v	114.7 (4)
O2^iv—Tl2—O3—P1	127.0 (3)	C3—P3—O9—Tl2^v	−131.9 (4)
O9^v—Tl2—O3—P1	−74.5 (4)	C3—N1—C1—P1	80.8 (5)
Tl1—Tl2—O3—P1	124.3 (3)	C2—N1—C1—P1	−151.7 (4)
O5^ii—Tl2—O3—Tl2^ii	79.25 (14)	O3—P1—C1—N1	33.2 (5)
O8—Tl2—O3—Tl2^ii	−87.61 (13)	O2—P1—C1—N1	155.5 (4)
O1^iii—Tl2—O3—Tl2^ii	173.44 (17)	O1—P1—C1—N1	−89.7 (5)
O3^ii—Tl2—O3—Tl2^ii	0.0	C3—N1—C2—P2	−152.4 (4)
O2^iv—Tl2—O3—Tl2^ii	−47.3 (2)	C1—N1—C2—P2	80.8 (5)
O9^v—Tl2—O3—Tl2^ii	111.2 (2)	O5—P2—C2—N1	39.1 (4)
Tl1—Tl2—O3—Tl2^ii	−50.01 (10)	O4—P2—C2—N1	164.3 (4)
O5^ii—Tl2—O3—Tl1^ii	−7.90 (11)	O6—P2—C2—N1	−78.3 (4)
O8—Tl2—O3—Tl1^ii	−174.76 (12)	C1—N1—C3—P3	−156.6 (4)
O1^iii—Tl2—O3—Tl1^ii	86.28 (14)	C2—N1—C3—P3	76.0 (5)
O3^ii—Tl2—O3—Tl1^ii	−87.15 (13)	O9—P3—C3—N1	156.2 (4)
O2^iv—Tl2—O3—Tl1^ii	−134.49 (15)	O8—P3—C3—N1	31.0 (4)
O9^v—Tl2—O3—Tl1^ii	24.0 (3)	O7—P3—C3—N1	−87.6 (4)
Tl1—Tl2—O3—Tl1^ii	−137.17 (9)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1N···O3	0.87	2.39	2.882 (5)	116
N1—H1N···O5	0.87	2.53	2.957 (6)	111
N1—H1N···O8	0.87	2.19	2.837 (7)	131
O1—H1O···O1^iii	0.82	1.78	2.504 (8)	147
O2—H2O···O2^vii	0.82	1.68	2.497 (7)	171
O6—H6O···O9^viii	0.82	1.67	2.484 (6)	171
O7—H7O···O4^i	0.82	1.70	2.521 (6)	180

Symmetry codes: (i) −x+1, −y, −z; (iii) −x+1, −y+1, −z+1; (vii) −x+2, −y, −z+1; (viii) x+1, y−1, z.