Hemipotassium hemirubidium digallium(III) manganese(II) tris(phos­phate) dihydrate

Zhang, J.; Li, P.; Liu, Z.-H.; Ng, S.W.

doi:10.1107/S160053681101258X

inorganic compounds

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Volume 67| Part 5| May 2011| Page i30

doi:10.1107/S160053681101258X

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Hemipotassium hemirubidium digallium(III) manganese(II) tris(phosphate) dihydrate

Jing Zhang,^a Ping Li,^a Zhi-Hong Liu ^a and Seik Weng Ng ^b ^*

^aSchool of Chemistry and Materials Science, Shaanxi Normal University, Xi'an 710062, People's Republic of China, and ^bDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
^*Correspondence e-mail: seikweng@um.edu.my

(Received 29 March 2011; accepted 4 April 2011; online 13 April 2011)

The title manganese(II) substituted gallophosphate, K_0.5Rb_0.5[Ga₂Mn(PO₄)₃(H₂O)₂], features a three-dimensional network built of PO₄ tetrahedra, GaO₅ trigonal bipyramids and MnO₆ octahedra. The Rb^I and K^I ions, which are disordered with respect to each other in a 1:1 ratio, occupy sites within the channels of the framework. The Rb^I/K^I and Mn^II atoms occupy positions of 2 symmetry, as does one of the two P atoms. The Rb^I/K^I site is surrounded by six O atoms [2.996 (2)–3.178 (4) Å] in an irregularly-shaped coordination environment. O—H⋯O hydrogen bonds between the water molecules and phosphate O atoms consolidate the crystal packing.

Related literature

For isotypic NH₄[Ga₂Mn(PO₄)₃(H₂O)₂], see: Chippindale et al. (1998 ).

Experimental

Crystal data

K_0.5Rb_0.5[Ga₂Mn(PO₄)₃(H₂O)₂]
M_r = 577.61
Monoclinic, C 2/c
a = 13.5504 (12) Å
b = 10.2965 (9) Å
c = 8.9072 (8) Å
β = 108.527 (1)°
V = 1178.34 (18) Å³
Z = 4
Mo Kα radiation
μ = 8.31 mm⁻¹
T = 295 K
0.45 × 0.40 × 0.35 mm

Data collection

Bruker SMART APEX diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.118, T_max = 0.159
6267 measured reflections
1348 independent reflections
1239 reflections with I > 2σ(I)
R_int = 0.037

Refinement

R[F² > 2σ(F²)] = 0.023
wR(F²) = 0.065
S = 1.04
1348 reflections
103 parameters
2 restraints
H-atom parameters constrained
Δρ_max = 0.63 e Å⁻³
Δρ_min = −0.75 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1w—H1⋯O3ⁱ	0.84 (3)	1.97 (2)	2.790 (3)	166 (4)
O1w—H2⋯O6ⁱⁱ	0.84 (3)	2.10 (2)	2.913 (3)	165 (4)
Symmetry codes: (i) $[x-{\script{1\over 2}}, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (ii) -x, -y+1, -z.

Data collection: APEX2 (Bruker, 2005 ); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001 ); software used to prepare material for publication: publCIF (Westrip, 2010 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S160053681101258X/br2164sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S160053681101258X/br2164Isup2.hkl

checkCIF report

Comment top

Microporous aluminium phosphates are readily synthesized by using the hydrothermal route; studies on these compounds have led to improvements in the synthesis of the related gallophosphates. The structure of NH₄[Ga₂Mn(PO₄)₃(H₂O)₂] features PO₄ tetrahedra, GaO₅ trigonal bipyramids and MnO₆ octahedra that are linked together to form a three-dimensional network (Chippindale et al., 1998). The title compound has a similar structure (Fig. 1); however, the rubidium and potassium atoms that occupy the channels within the network rattle in the cavities, as noted from the irregular nature of the polyhedron surrounding the atoms. The coordination number is much higher when longer interactions are considered.

Related literature top

For isotypic NH₄[Ga₂Mn(PO₄)₃(H₂O)₂], see: Chippindale et al. (1998).

Experimental top

The compound was synthesized from a mixture of gallium oxide (0.037 g), boric acid (0.035 g), rubidium carbonate (0.023 g), potassium carbonate (0.138 g), manganese dichloride tetrahydrate (0.397 g), phosphoric acid (0.15 ml) and water (1.8 ml) (molar ratio of 2:5:1:10:20:20:1000). This mixture was sealed in 25 ml, Teflon-lined, stainless-steel Parr bomb. The bomb was heated at 468 K for 7 days. Colorless block-shaped crystals were isolated.

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

Fig. 1. Thermal ellipsoid plot (Barbour, 2001) of a portion of the polymeric structure of K_0.5Rb_0.5[Ga₂Mn(PO₄)₃(H₂O)₂] at the 70% probability level; hydrogen atoms are drawn as spheres of arbitrary radius. The potassium atoms are disordered with respect to the rubidium atoms in a 1:1 ratio. Symmetry codes: (i) x + 1/2, -y + 3/2, z + 1/2; (ii) -x + 1/2, -y + 3/2, -z + 1; (iii) -x + 1, y, -z + 3/2; (iv) -x + 1/2, y + 1/2, -z + 1/2; (v) x + 1/2, y + 1/2, z + 1; (vi) x, -y + 1, z + 1/2; (vii) -x + 1, -y + 1, -z + 1; (viii) x, -y + 1, z - 1/2; (ix) -x, y, -z + 1/2; (x) x - 1/2, -y + 1/2, z - 1/2.

Hemipotassium hemirubidium digallium(III) manganese(II) tris(phosphate) dihydrate top

Crystal data top

K_0.5Rb_0.5[Ga₂Mn(PO₄)₃(H₂O)₂]	F(000) = 1104
M_r = 577.61	D_x = 3.256 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 4099 reflections
a = 13.5504 (12) Å	θ = 2.5–28.6°
b = 10.2965 (9) Å	µ = 8.31 mm⁻¹
c = 8.9072 (8) Å	T = 295 K
β = 108.527 (1)°	Block, colorless
V = 1178.34 (18) Å³	0.45 × 0.40 × 0.35 mm
Z = 4

Data collection top

Bruker SMART APEX diffractometer	1348 independent reflections
Radiation source: fine-focus sealed tube	1239 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.037
ω scans	θ_max = 27.5°, θ_min = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −17→17
T_min = 0.118, T_max = 0.159	k = −13→13
6267 measured reflections	l = −11→11

Refinement top

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)] = 0.023	Hydrogen site location: difference Fourier map
wR(F²) = 0.065	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0391P)² + 2.8102P] where P = (F_o² + 2F_c²)/3
1348 reflections	(Δ/σ)_max = 0.001
103 parameters	Δρ_max = 0.63 e Å⁻³
2 restraints	Δρ_min = −0.75 e Å⁻³

Crystal data top

K_0.5Rb_0.5[Ga₂Mn(PO₄)₃(H₂O)₂]	V = 1178.34 (18) Å³
M_r = 577.61	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 13.5504 (12) Å	µ = 8.31 mm⁻¹
b = 10.2965 (9) Å	T = 295 K
c = 8.9072 (8) Å	0.45 × 0.40 × 0.35 mm
β = 108.527 (1)°

Data collection top

Bruker SMART APEX diffractometer	1348 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	1239 reflections with I > 2σ(I)
T_min = 0.118, T_max = 0.159	R_int = 0.037
6267 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.023	2 restraints
wR(F²) = 0.065	H-atom parameters constrained
S = 1.04	Δρ_max = 0.63 e Å⁻³
1348 reflections	Δρ_min = −0.75 e Å⁻³
103 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Rb1	0.5000	0.86132 (6)	0.7500	0.03306 (18)	0.50
Ga1	0.32950 (2)	0.57498 (3)	0.42741 (3)	0.01061 (11)
Mn1	0.0000	0.28198 (6)	0.2500	0.01443 (15)
K1	0.5000	0.86132 (6)	0.7500	0.03306 (18)	0.50
P1	0.5000	0.49997 (9)	0.7500	0.0106 (2)
P2	0.21012 (6)	0.37336 (7)	0.17422 (8)	0.01171 (16)
O1	0.44106 (16)	0.59068 (19)	0.6149 (2)	0.0150 (4)
O2	0.42851 (16)	0.40472 (19)	0.8014 (2)	0.0154 (4)
O3	0.29213 (16)	0.41300 (18)	0.3344 (2)	0.0146 (4)
O4	0.10038 (17)	0.3988 (2)	0.1749 (3)	0.0198 (4)
O5	0.23416 (16)	0.22845 (19)	0.1603 (2)	0.0156 (4)
O6	0.22740 (16)	0.45222 (19)	0.0373 (2)	0.0148 (4)
O1w	−0.11223 (19)	0.3043 (2)	0.0069 (3)	0.0263 (5)
H1	−0.146 (3)	0.237 (3)	−0.033 (5)	0.039*
H2	−0.154 (3)	0.366 (3)	−0.001 (5)	0.039*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Rb1	0.0418 (4)	0.0181 (3)	0.0425 (4)	0.000	0.0179 (3)	0.000
Ga1	0.01323 (18)	0.01036 (17)	0.00716 (17)	0.00043 (10)	0.00172 (12)	0.00000 (10)
Mn1	0.0166 (3)	0.0129 (3)	0.0145 (3)	0.000	0.0059 (2)	0.000
K1	0.0418 (4)	0.0181 (3)	0.0425 (4)	0.000	0.0179 (3)	0.000
P1	0.0127 (4)	0.0117 (4)	0.0067 (4)	0.000	0.0021 (3)	0.000
P2	0.0142 (4)	0.0121 (3)	0.0088 (3)	−0.0013 (3)	0.0036 (3)	−0.0006 (2)
O1	0.0181 (10)	0.0163 (10)	0.0072 (9)	−0.0007 (8)	−0.0010 (7)	0.0015 (7)
O2	0.0182 (10)	0.0134 (9)	0.0165 (10)	−0.0009 (8)	0.0081 (8)	0.0005 (8)
O3	0.0213 (11)	0.0110 (9)	0.0101 (9)	−0.0030 (8)	0.0028 (8)	−0.0027 (7)
O4	0.0176 (10)	0.0203 (10)	0.0232 (11)	0.0004 (8)	0.0088 (9)	0.0042 (9)
O5	0.0202 (10)	0.0115 (9)	0.0147 (9)	−0.0038 (8)	0.0048 (8)	−0.0038 (7)
O6	0.0196 (10)	0.0146 (9)	0.0118 (9)	0.0006 (8)	0.0072 (8)	0.0026 (7)
O1w	0.0286 (13)	0.0226 (11)	0.0204 (11)	0.0018 (10)	−0.0025 (9)	−0.0040 (9)

Geometric parameters (Å, º) top

Rb1—O1	3.040 (2)	Mn1—O2^ix	2.264 (2)
Rb1—O1ⁱ	3.040 (2)	Mn1—O2^x	2.264 (2)
Rb1—O4ⁱⁱ	3.613 (2)	Mn1—O4	2.079 (2)
Rb1—O4ⁱⁱⁱ	2.996 (2)	Mn1—O4^xi	2.079 (2)
Rb1—O4^iv	2.996 (2)	Mn1—O1w	2.228 (2)
Rb1—O5^v	3.555 (2)	Mn1—O1w^xi	2.228 (2)
Rb1—O5^vi	3.555 (2)	P1—O1	1.532 (2)
Rb1—O6^vii	3.451 (2)	P1—O1ⁱ	1.532 (2)
Rb1—O6ⁱⁱ	3.451 (2)	P1—O2	1.546 (2)
Rb1—O4^vii	3.613 (2)	P1—O2ⁱ	1.546 (2)
Rb1—O1wⁱⁱ	3.178 (3)	P2—O4	1.512 (2)
Rb1—O1w^vii	3.178 (3)	P2—O5	1.541 (2)
Ga1—O1	1.870 (2)	P2—O6	1.543 (2)
Ga1—O2^viii	2.015 (2)	P2—O3	1.558 (2)
Ga1—O3	1.860 (2)	O1w—H1	0.84 (3)
Ga1—O5ⁱⁱ	1.850 (2)	O1w—H2	0.84 (3)
Ga1—O6^vi	1.952 (2)

O4^iv—Rb1—O4ⁱⁱⁱ	68.95 (8)	O4ⁱⁱⁱ—Rb1—O4ⁱⁱ	95.69 (5)
O4^iv—Rb1—O1	138.43 (6)	O1—Rb1—O4ⁱⁱ	73.69 (5)
O4ⁱⁱⁱ—Rb1—O1	139.75 (6)	O1ⁱ—Rb1—O4ⁱⁱ	118.48 (5)
O4^iv—Rb1—O1ⁱ	139.75 (6)	O1wⁱⁱ—Rb1—O4ⁱⁱ	51.14 (5)
O4ⁱⁱⁱ—Rb1—O1ⁱ	138.43 (6)	O1w^vii—Rb1—O4ⁱⁱ	131.83 (5)
O1—Rb1—O1ⁱ	47.11 (7)	O6^vii—Rb1—O4ⁱⁱ	134.28 (5)
O4^iv—Rb1—O1wⁱⁱ	68.68 (6)	O6ⁱⁱ—Rb1—O4ⁱⁱ	40.88 (5)
O4ⁱⁱⁱ—Rb1—O1wⁱⁱ	131.90 (6)	O5^vi—Rb1—O4ⁱⁱ	77.00 (5)
O1—Rb1—O1wⁱⁱ	70.81 (6)	O5^v—Rb1—O4ⁱⁱ	106.30 (5)
O1ⁱ—Rb1—O1wⁱⁱ	89.44 (6)	O4^iv—Rb1—O4^vii	95.69 (5)
O4^iv—Rb1—O1w^vii	131.90 (6)	O4ⁱⁱⁱ—Rb1—O4^vii	74.01 (6)
O4ⁱⁱⁱ—Rb1—O1w^vii	68.68 (6)	O1—Rb1—O4^vii	118.48 (5)
O1—Rb1—O1w^vii	89.44 (6)	O1ⁱ—Rb1—O4^vii	73.69 (5)
O1ⁱ—Rb1—O1w^vii	70.81 (6)	O1wⁱⁱ—Rb1—O4^vii	131.83 (5)
O1wⁱⁱ—Rb1—O1w^vii	158.73 (9)	O1w^vii—Rb1—O4^vii	51.14 (5)
O4^iv—Rb1—O6^vii	65.17 (5)	O6^vii—Rb1—O4^vii	40.88 (5)
O4ⁱⁱⁱ—Rb1—O6^vii	88.43 (6)	O6ⁱⁱ—Rb1—O4^vii	134.28 (5)
O1—Rb1—O6^vii	127.06 (5)	O5^vi—Rb1—O4^vii	106.30 (5)
O1ⁱ—Rb1—O6^vii	83.95 (5)	O5^v—Rb1—O4^vii	77.00 (5)
O1wⁱⁱ—Rb1—O6^vii	93.74 (5)	O4ⁱⁱ—Rb1—O4^vii	167.72 (7)
O1w^vii—Rb1—O6^vii	92.00 (5)	O5ⁱⁱ—Ga1—O3	123.61 (9)
O4^iv—Rb1—O6ⁱⁱ	88.43 (6)	O5ⁱⁱ—Ga1—O1	116.06 (9)
O4ⁱⁱⁱ—Rb1—O6ⁱⁱ	65.17 (5)	O3—Ga1—O1	120.26 (9)
O1—Rb1—O6ⁱⁱ	83.95 (5)	O5ⁱⁱ—Ga1—O6^vi	91.40 (9)
O1ⁱ—Rb1—O6ⁱⁱ	127.06 (5)	O3—Ga1—O6^vi	87.64 (9)
O1wⁱⁱ—Rb1—O6ⁱⁱ	92.00 (5)	O1—Ga1—O6^vi	93.74 (9)
O1w^vii—Rb1—O6ⁱⁱ	93.74 (5)	O5ⁱⁱ—Ga1—O2^viii	88.85 (8)
O6^vii—Rb1—O6ⁱⁱ	148.53 (7)	O3—Ga1—O2^viii	88.85 (9)
O4^iv—Rb1—O5^vi	131.58 (5)	O1—Ga1—O2^viii	89.78 (9)
O4ⁱⁱⁱ—Rb1—O5^vi	76.41 (5)	O6^vi—Ga1—O2^viii	175.95 (8)
O1—Rb1—O5^vi	63.43 (5)	O4—Mn1—O4^xi	109.28 (12)
O1ⁱ—Rb1—O5^vi	88.32 (5)	O4—Mn1—O1w	86.67 (9)
O1wⁱⁱ—Rb1—O5^vi	118.20 (5)	O4^xi—Mn1—O1w	86.48 (9)
O1w^vii—Rb1—O5^vi	55.36 (5)	O4—Mn1—O1w^xi	86.48 (9)
O6^vii—Rb1—O5^vi	147.08 (4)	O4^xi—Mn1—O1w^xi	86.67 (9)
O6ⁱⁱ—Rb1—O5^vi	45.70 (4)	O1w—Mn1—O1w^xi	168.14 (13)
O4^iv—Rb1—O5^v	76.41 (5)	O4—Mn1—O2^x	157.23 (8)
O4ⁱⁱⁱ—Rb1—O5^v	131.58 (6)	O4^xi—Mn1—O2^x	93.49 (8)
O1—Rb1—O5^v	88.32 (5)	O1w—Mn1—O2^x	94.61 (8)
O1ⁱ—Rb1—O5^v	63.43 (5)	O1w^xi—Mn1—O2^x	95.46 (8)
O1wⁱⁱ—Rb1—O5^v	55.36 (5)	O4—Mn1—O2^ix	93.49 (8)
O1w^vii—Rb1—O5^v	118.20 (5)	O4^xi—Mn1—O2^ix	157.23 (8)
O6^vii—Rb1—O5^v	45.70 (4)	O1w—Mn1—O2^ix	95.46 (8)
O6ⁱⁱ—Rb1—O5^v	147.08 (4)	O1w^xi—Mn1—O2^ix	94.61 (8)
O5^vi—Rb1—O5^v	149.86 (6)	O2^x—Mn1—O2^ix	63.75 (10)
O4^iv—Rb1—O4ⁱⁱ	74.01 (6)

Symmetry codes: (i) −x+1, y, −z+3/2; (ii) −x+1/2, y+1/2, −z+1/2; (iii) −x+1/2, −y+3/2, −z+1; (iv) x+1/2, −y+3/2, z+1/2; (v) −x+1, −y+1, −z+1; (vi) x, −y+1, z+1/2; (vii) x+1/2, y+1/2, z+1; (viii) x, −y+1, z−1/2; (ix) −x+1/2, −y+1/2, −z+1; (x) x−1/2, −y+1/2, z−1/2; (xi) −x, y, −z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H1···O3^x	0.84 (3)	1.97 (2)	2.790 (3)	166 (4)
O1w—H2···O6^xii	0.84 (3)	2.10 (2)	2.913 (3)	165 (4)

Symmetry codes: (x) x−1/2, −y+1/2, z−1/2; (xii) −x, −y+1, −z.

Experimental details

Crystal data
Chemical formula	K_0.5Rb_0.5[Ga₂Mn(PO₄)₃(H₂O)₂]
M_r	577.61
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	295
a, b, c (Å)	13.5504 (12), 10.2965 (9), 8.9072 (8)
β (°)	108.527 (1)
V (Å³)	1178.34 (18)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	8.31
Crystal size (mm)	0.45 × 0.40 × 0.35

Data collection
Diffractometer	Bruker SMART APEX diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.118, 0.159
No. of measured, independent and observed [I > 2σ(I)] reflections	6267, 1348, 1239
R_int	0.037
(sin θ/λ)_max (Å⁻¹)	0.650

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.023, 0.065, 1.04
No. of reflections	1348
No. of parameters	103
No. of restraints	2
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.63, −0.75

Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2010).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H1···O3ⁱ	0.84 (3)	1.97 (2)	2.790 (3)	166 (4)
O1w—H2···O6ⁱⁱ	0.84 (3)	2.10 (2)	2.913 (3)	165 (4)

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

Acknowledgements

We thank Shaanxi Normal University and the University of Malaya for supporting this study.

References

Barbour, L. J. (2001). J. Supramol. Chem. 1, 189–191. CrossRef CAS Google Scholar
Bruker (2005). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Chippindale, A. M., Cowley, A. R. & Bond, A. D. (1998). Acta Cryst. C54, IUC9800061. CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Web of Science CrossRef CAS IUCr Journals Google Scholar

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Hemipotassium hemirubidium digallium(III) manganese(II) tris­(phos­phate) dihydrate

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

inorganic compounds

Hemipotassium hemirubidium digallium(III) manganese(II) tris(phosphate) dihydrate