Structure refinements of Na0.8Ti1.2Ga4.8O10: X-ray diffraction analysis for the sodium ion distribution in a one-dimensional tunnel-like space

Michiue, Y.; Sato, A.

doi:10.1107/S0108768104023328

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Structure refinements of Na_0.8Ti_1.2Ga_4.8O₁₀: X-ray diffraction analysis for the sodium ion distribution in a one-dimensional tunnel-like space

Y. Michiue and A. Sato

The structure of Na_0.8Ti_1.2Ga_4.8O₁₀ was determined by means of single-crystal X-ray diffraction at 173 and 123 K and reinvestigated at 299 K. The host structure containing one-dimensional tunnels was retained over the temperatures examined, while significant changes were observed in the probability density distribution of Na⁺ ions in the tunnel. The refinement based on the local structure model with the deviated Na⁺ ion neighboring the vacancy gave a similar result to that from the conventional model, but with reduced standard uncertainties of the structural parameters for the Na⁺ ions. The potential barrier for the Na⁺ ion hopping between adjacent cavities was estimated to be ca 30-40 meV from the joint probability density function of deviated Na⁺ ions.

Keywords: one-dimensional tunnel structure; Na distribution; probability density function; one-particle potential; ionic conduction.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768104023328/lc5009sup1.cif Contains datablocks global, 299K-model-III, 173K-model-III, 123K-model-III, 299K-model-I, 299K-model-II, 173K-model-I, 173K-model-II, 123K-model-I, 123K-model-II
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768104023328/lc5009299K-model-IIIsup2.hkl Contains datablock _299K-model-III
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768104023328/lc5009173K-model-IIIsup3.hkl Contains datablock 173K-model-III
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768104023328/lc5009123K-model-IIIsup4.hkl Contains datablock 123K-model-III
	Portable Document Format (PDF) file https://doi.org/10.1107/S0108768104023328/lc5009sup5.pdf Supplementary material

Computing details top

For all compounds, program(s) used to refine structure: (Jana2000; Petricek and Dusek, 2000); software used to prepare material for publication: (Jana2000; Petricek and Dusek, 2000).

Figures top

(299K-model-III) top

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	F(000) = 528
M_r = 570.5	D_x = 4.997 (1) Mg m⁻³
Monoclinic, C2/m	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -C 2y	Cell parameters from 967 reflections
a = 12.1008 (8) Å	θ = 3.8–51.6°
b = 3.0113 (2) Å	µ = 18.11 mm⁻¹
c = 10.4100 (6) Å	T = 299 K
β = 92.258 (4)°	Prism, colorless
V = 379.04 (4) Å³	0.24 × 0.16 × 0.10 mm
Z = 2

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	1785 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.060
ω scans	θ_max = 51.7°, θ_min = 2.0°
Absorption correction: analytical ?	h = −24→21
T_min = 0.074, T_max = 0.249	k = −6→5
5633 measured reflections	l = −22→22
2168 independent reflections

Refinement top

Refinement on F²	Weighting scheme based on measured s.u.'s w = 1/(σ²(I) + 0.0004I²)
R[F² > 2σ(F²)] = 0.028	(Δ/σ)_max = 0.007
wR(F²) = 0.069	Δρ_max = 2.88 e Å⁻³
S = 1.17	Δρ_min = −1.95 e Å⁻³
2168 reflections	Extinction correction: B-C type 2 (Becker & Coppens, 1974)
60 parameters	Extinction coefficient: 0.001741

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	V = 379.04 (4) Å³
M_r = 570.5	Z = 2
Monoclinic, C2/m	Mo Kα radiation
a = 12.1008 (8) Å	µ = 18.11 mm⁻¹
b = 3.0113 (2) Å	T = 299 K
c = 10.4100 (6) Å	0.24 × 0.16 × 0.10 mm
β = 92.258 (4)°

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	2168 independent reflections
Absorption correction: analytical ?	1785 reflections with I > 2σ(I)
T_min = 0.074, T_max = 0.249	R_int = 0.060
5633 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.028	60 parameters
wR(F²) = 0.069	Δρ_max = 2.88 e Å⁻³
S = 1.17	Δρ_min = −1.95 e Å⁻³
2168 reflections

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Na1	0	0	0.5	0.045 (4)	0.421 (19)
Na2	0	0.225 (11)	0.5	0.075 (9)	0.193 (6)
Ga1	0.063729 (18)	0	0.16343 (2)	0.00548 (4)
Ga2	0.323682 (18)	0	0.10155 (2)	0.00567 (5)
Ga	0.26463 (3)	0	0.62588 (3)	0.00758 (6)	0.404 (3)
Ti	0.26463 (3)	0	0.62588 (3)	0.00758 (6)	0.596 (3)
O1	0.16415 (12)	0	0.03184 (13)	0.0060 (3)
O2	0.13003 (13)	0	0.32496 (14)	0.0078 (3)
O3	0.20431 (13)	0	0.78848 (13)	0.0071 (3)
O4	0.32467 (13)	0	0.44561 (14)	0.0083 (3)
O5	0.48026 (12)	0	0.14288 (16)	0.0081 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.026 (4)	0.081 (10)	0.030 (3)	0	0.020 (3)	0
Na2	0.012 (4)	0.16 (2)	0.058 (8)	0	−0.006 (4)	0
Ga1	0.00490 (8)	0.00560 (8)	0.00592 (7)	0	−0.00006 (6)	0
Ga2	0.00476 (8)	0.00526 (8)	0.00693 (7)	0	−0.00074 (6)	0
Ga	0.01020 (12)	0.00705 (11)	0.00551 (8)	0	0.00043 (7)	0
Ti	0.01020 (12)	0.00705 (11)	0.00551 (8)	0	0.00043 (7)	0
O1	0.0049 (5)	0.0070 (5)	0.0062 (4)	0	0.0001 (3)	0
O2	0.0083 (5)	0.0087 (5)	0.0064 (4)	0	−0.0015 (4)	0
O3	0.0104 (6)	0.0057 (5)	0.0054 (4)	0	0.0017 (4)	0
O4	0.0084 (5)	0.0095 (6)	0.0070 (4)	0	−0.0002 (4)	0
O5	0.0048 (5)	0.0054 (5)	0.0138 (5)	0	−0.0016 (4)	0

Bond lengths (Å) top

Na1—O2	2.4539 (15)	Ga2—O1^vi	2.0574 (10)
Na1—O2ⁱ	2.4539 (15)	Ga2—O3^vii	1.9295 (9)
Na2—O4ⁱⁱ	2.327 (12)	Ga2—O3ⁱⁱⁱ	1.9295 (9)
Na2—O4ⁱⁱⁱ	2.327 (12)	Ga2—O5	1.9263 (15)
Ga1—O1	1.8666 (14)	Ga—O2^vii	2.0254 (10)
Ga1—O2	1.8344 (15)	Ga—O2ⁱⁱⁱ	2.0254 (10)
Ga1—O5^iv	1.8210 (8)	Ga—O3	1.8695 (15)
Ga1—O5ⁱⁱ	1.8210 (8)	Ga—O4	2.0389 (15)
Ga2—O1	2.0354 (14)	Ga—O4^vii	1.9812 (10)
Ga2—O1^v	2.0574 (10)	Ga—O4ⁱⁱⁱ	1.9812 (10)

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

(173K-model-III) top

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	F(000) = 528
M_r = 570.5	D_x = 5.010 (1) Mg m⁻³
Monoclinic, C2/m	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -C 2y	Cell parameters from 854 reflections
a = 12.0848 (12) Å	θ = 3.8–51.4°
b = 3.0101 (3) Å	µ = 18.16 mm⁻¹
c = 10.4014 (9) Å	T = 173 K
β = 92.187 (5)°	Prism, colorless
V = 378.09 (6) Å³	0.24 × 0.16 × 0.10 mm
Z = 2

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	1749 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.060
ω scans	θ_max = 51.6°, θ_min = 2.0°
Absorption correction: analytical ?	h = −24→21
T_min = 0.071, T_max = 0.250	k = −6→5
5581 measured reflections	l = −22→22
2159 independent reflections

Refinement top

Refinement on F²	Weighting scheme based on measured s.u.'s w = 1/(σ²(I) + 0.0004I²)
R[F² > 2σ(F²)] = 0.029	(Δ/σ)_max = 0.010
wR(F²) = 0.067	Δρ_max = 3.10 e Å⁻³
S = 1.06	Δρ_min = −2.21 e Å⁻³
2159 reflections	Extinction correction: B-C type 2 (Becker & Coppens, 1974)
60 parameters	Extinction coefficient: 0.002039

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	V = 378.09 (6) Å³
M_r = 570.5	Z = 2
Monoclinic, C2/m	Mo Kα radiation
a = 12.0848 (12) Å	µ = 18.16 mm⁻¹
b = 3.0101 (3) Å	T = 173 K
c = 10.4014 (9) Å	0.24 × 0.16 × 0.10 mm
β = 92.187 (5)°

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	2159 independent reflections
Absorption correction: analytical ?	1749 reflections with I > 2σ(I)
T_min = 0.071, T_max = 0.250	R_int = 0.060
5581 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.029	60 parameters
wR(F²) = 0.067	Δρ_max = 3.10 e Å⁻³
S = 1.06	Δρ_min = −2.21 e Å⁻³
2159 reflections

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Na1	0	0	0.5	0.037 (3)	0.433 (19)
Na2	0	0.223 (9)	0.5	0.050 (6)	0.189 (6)
Ga1	0.063739 (18)	0	0.16364 (2)	0.00414 (5)
Ga2	0.323600 (18)	0	0.10136 (2)	0.00433 (5)
Ga	0.26469 (3)	0	0.62574 (3)	0.00595 (6)	0.405 (3)
Ti	0.26469 (3)	0	0.62574 (3)	0.00595 (6)	0.595 (3)
O1	0.16412 (12)	0	0.03180 (14)	0.0049 (3)
O2	0.12989 (13)	0	0.32544 (14)	0.0063 (3)
O3	0.20427 (13)	0	0.78856 (15)	0.0059 (3)
O4	0.32473 (13)	0	0.44577 (15)	0.0068 (3)
O5	0.48034 (13)	0	0.14274 (16)	0.0063 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.022 (3)	0.064 (8)	0.028 (3)	0	0.018 (3)	0
Na2	0.011 (4)	0.108 (16)	0.029 (5)	0	−0.007 (3)	0
Ga1	0.00350 (8)	0.00442 (9)	0.00450 (7)	0	0.00002 (6)	0
Ga2	0.00339 (9)	0.00416 (8)	0.00538 (7)	0	−0.00066 (6)	0
Ga	0.00797 (12)	0.00557 (12)	0.00433 (9)	0	0.00034 (8)	0
Ti	0.00797 (12)	0.00557 (12)	0.00433 (9)	0	0.00034 (8)	0
O1	0.0040 (5)	0.0054 (5)	0.0052 (4)	0	0.0002 (4)	0
O2	0.0062 (5)	0.0076 (6)	0.0049 (4)	0	−0.0010 (4)	0
O3	0.0077 (6)	0.0052 (5)	0.0046 (4)	0	0.0007 (4)	0
O4	0.0071 (6)	0.0079 (6)	0.0054 (4)	0	0.0000 (4)	0
O5	0.0039 (5)	0.0044 (5)	0.0105 (5)	0	−0.0013 (4)	0

Bond lengths (Å) top

Na1—O2	2.4450 (16)	Ga2—O1^vi	2.0546 (10)
Na1—O2ⁱ	2.4450 (16)	Ga2—O3^vii	1.9285 (10)
Na2—O4ⁱⁱ	2.326 (9)	Ga2—O3ⁱⁱⁱ	1.9285 (10)
Na2—O4ⁱⁱⁱ	2.326 (9)	Ga2—O5	1.9264 (15)
Ga1—O1	1.8652 (15)	Ga—O2^vii	2.0240 (11)
Ga1—O2	1.8354 (15)	Ga—O2ⁱⁱⁱ	2.0240 (11)
Ga1—O5^iv	1.8198 (9)	Ga—O3	1.8697 (16)
Ga1—O5ⁱⁱ	1.8198 (9)	Ga—O4	2.0332 (16)
Ga2—O1	2.0326 (15)	Ga—O4^vii	1.9811 (10)
Ga2—O1^v	2.0546 (10)	Ga—O4ⁱⁱⁱ	1.9811 (10)

(123K-model-III) top

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	F(000) = 528
M_r = 570.5	D_x = 5.009 (1) Mg m⁻³
Monoclinic, C2/m	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -C 2y	Cell parameters from 871 reflections
a = 12.0828 (9) Å	θ = 3.9–51.4°
b = 3.0099 (3) Å	µ = 18.16 mm⁻¹
c = 10.4045 (7) Å	T = 123 K
β = 92.192 (4)°	Prism, colorless
V = 378.11 (5) Å³	0.24 × 0.16 × 0.10 mm
Z = 2

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	1752 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.059
ω scans	θ_max = 51.7°, θ_min = 2.0°
Absorption correction: analytical ?	h = −24→21
T_min = 0.073, T_max = 0.250	k = −6→5
5596 measured reflections	l = −22→22
2160 independent reflections

Refinement top

Refinement on F²	Weighting scheme based on measured s.u.'s w = 1/(σ²(I) + 0.0004I²)
R[F² > 2σ(F²)] = 0.028	(Δ/σ)_max = 0.008
wR(F²) = 0.065	Δρ_max = 2.92 e Å⁻³
S = 1.04	Δρ_min = −1.99 e Å⁻³
2160 reflections	Extinction correction: B-C type 2 (Becker & Coppens, 1974)
60 parameters	Extinction coefficient: 0.00195

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	V = 378.11 (5) Å³
M_r = 570.5	Z = 2
Monoclinic, C2/m	Mo Kα radiation
a = 12.0828 (9) Å	µ = 18.16 mm⁻¹
b = 3.0099 (3) Å	T = 123 K
c = 10.4045 (7) Å	0.24 × 0.16 × 0.10 mm
β = 92.192 (4)°

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	2160 independent reflections
Absorption correction: analytical ?	1752 reflections with I > 2σ(I)
T_min = 0.073, T_max = 0.250	R_int = 0.059
5596 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.028	60 parameters
wR(F²) = 0.065	Δρ_max = 2.92 e Å⁻³
S = 1.04	Δρ_min = −1.99 e Å⁻³
2160 reflections

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Na1	0	0	0.5	0.029 (2)	0.410 (18)
Na2	0	0.217 (7)	0.5	0.038 (4)	0.197 (6)
Ga1	0.063745 (18)	0	0.16375 (2)	0.00363 (5)
Ga2	0.323584 (18)	0	0.10129 (2)	0.00381 (5)
Ga	0.26467 (3)	0	0.62569 (3)	0.00534 (6)	0.402 (3)
Ti	0.26467 (3)	0	0.62569 (3)	0.00534 (6)	0.598 (3)
O1	0.16419 (12)	0	0.03201 (14)	0.0044 (3)
O2	0.12999 (13)	0	0.32565 (14)	0.0059 (3)
O3	0.20432 (13)	0	0.78878 (14)	0.0054 (3)
O4	0.32455 (13)	0	0.44570 (14)	0.0065 (3)
O5	0.48025 (12)	0	0.14286 (15)	0.0056 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.018 (3)	0.045 (6)	0.026 (3)	0	0.016 (2)	0
Na2	0.008 (3)	0.086 (11)	0.018 (3)	0	−0.001 (2)	0
Ga1	0.00310 (8)	0.00387 (9)	0.00392 (7)	0	0.00001 (6)	0
Ga2	0.00289 (8)	0.00370 (8)	0.00479 (7)	0	−0.00065 (6)	0
Ga	0.00708 (11)	0.00500 (11)	0.00395 (8)	0	0.00026 (7)	0
Ti	0.00708 (11)	0.00500 (11)	0.00395 (8)	0	0.00026 (7)	0
O1	0.0036 (5)	0.0049 (5)	0.0048 (4)	0	0.0001 (4)	0
O2	0.0063 (5)	0.0069 (6)	0.0044 (4)	0	−0.0003 (4)	0
O3	0.0077 (6)	0.0045 (5)	0.0041 (4)	0	0.0008 (4)	0
O4	0.0068 (6)	0.0072 (6)	0.0055 (4)	0	0.0001 (4)	0
O5	0.0035 (5)	0.0038 (5)	0.0092 (5)	0	−0.0011 (4)	0

Bond lengths (Å) top

Na1—O2	2.4445 (15)	Ga2—O1^vi	2.0557 (10)
Na1—O2ⁱ	2.4445 (15)	Ga2—O3^vii	1.9277 (9)
Na2—O4ⁱⁱ	2.334 (8)	Ga2—O3ⁱⁱⁱ	1.9277 (9)
Na2—O4ⁱⁱⁱ	2.334 (8)	Ga2—O5	1.9256 (15)
Ga1—O1	1.8652 (15)	Ga—O2^vii	2.0228 (10)
Ga1—O2	1.8372 (14)	Ga—O2ⁱⁱⁱ	2.0228 (10)
Ga1—O5^iv	1.8202 (8)	Ga—O3	1.8724 (15)
Ga1—O5ⁱⁱ	1.8202 (8)	Ga—O4	2.0332 (15)
Ga2—O1	2.0304 (14)	Ga—O4^vii	1.9793 (10)
Ga2—O1^v	2.0557 (10)	Ga—O4ⁱⁱⁱ	1.9793 (10)

(299K-model-I) top

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	F(000) = 528
M_r = 570.5	D_x = 4.997 (1) Mg m⁻³
Monoclinic, C2/m	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -C 2y	Cell parameters from 967 reflections
a = 12.1008 (8) Å	θ = 3.8–51.6°
b = 3.0113 (2) Å	µ = 18.11 mm⁻¹
c = 10.4100 (6) Å	T = 299 K
β = 92.258 (4)°	Prism, colorless
V = 379.04 (4) Å³	0.24 × 0.16 × 0.10 mm
Z = 2

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	1785 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.060
ω scans	θ_max = 51.7°, θ_min = 2.0°
Absorption correction: analytical ?	h = −24→21
T_min = 0.074, T_max = 0.249	k = −6→5
5633 measured reflections	l = −22→22
2168 independent reflections

Refinement top

Refinement on F²	Weighting scheme based on measured s.u.'s w = 1/(σ²(I) + 0.0004I²)
R[F² > 2σ(F²)] = 0.028	(Δ/σ)_max = 0.009
wR(F²) = 0.069	Δρ_max = 2.86 e Å⁻³
S = 1.18	Δρ_min = −1.95 e Å⁻³
2168 reflections	Extinction correction: B-C type 2 (Becker & Coppens, 1974)
60 parameters	Extinction coefficient: 0.001697

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	V = 379.04 (4) Å³
M_r = 570.5	Z = 2
Monoclinic, C2/m	Mo Kα radiation
a = 12.1008 (8) Å	µ = 18.11 mm⁻¹
b = 3.0113 (2) Å	T = 299 K
c = 10.4100 (6) Å	0.24 × 0.16 × 0.10 mm
β = 92.258 (4)°

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	2168 independent reflections
Absorption correction: analytical ?	1785 reflections with I > 2σ(I)
T_min = 0.074, T_max = 0.249	R_int = 0.060
5633 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.028	60 parameters
wR(F²) = 0.069	Δρ_max = 2.86 e Å⁻³
S = 1.18	Δρ_min = −1.95 e Å⁻³
2168 reflections

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Na1	0	0	0.5	0.1168	0.800 (6)
Ga1	0.063721 (18)	0	0.16342 (2)	0.00548 (5)
Ga2	0.323689 (18)	0	0.10155 (2)	0.00568 (5)
Ga	0.26463 (3)	0	0.62589 (3)	0.00755 (6)	0.400 (3)
Ti	0.26463 (3)	0	0.62589 (3)	0.00755 (6)	0.600 (3)
O1	0.16416 (12)	0	0.03187 (14)	0.0060 (3)
O2	0.13005 (13)	0	0.32495 (14)	0.0078 (3)
O3	0.20436 (13)	0	0.78849 (14)	0.0071 (3)
O4	0.32465 (13)	0	0.44564 (14)	0.0082 (3)
O5	0.48027 (12)	0	0.14294 (16)	0.0081 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.020832	0.291895	0.038548	0	0.01128	0
Ga1	0.00490 (8)	0.00561 (8)	0.00592 (7)	0	−0.00005 (6)	0
Ga2	0.00476 (9)	0.00526 (8)	0.00693 (7)	0	−0.00074 (6)	0
Ga	0.01014 (12)	0.00702 (11)	0.00549 (8)	0	0.00043 (7)	0
Ti	0.01014 (12)	0.00702 (11)	0.00549 (8)	0	0.00043 (7)	0
O1	0.0049 (5)	0.0071 (5)	0.0061 (4)	0	0.0001 (4)	0
O2	0.0083 (5)	0.0086 (6)	0.0064 (4)	0	−0.0015 (4)	0
O3	0.0105 (6)	0.0056 (5)	0.0053 (4)	0	0.0017 (4)	0
O4	0.0083 (5)	0.0094 (6)	0.0070 (4)	0	−0.0002 (4)	0
O5	0.0048 (5)	0.0055 (5)	0.0138 (5)	0	−0.0015 (4)	0

Bond lengths (Å) top

Na1—O2	2.4542 (15)	Ga2—O3^vi	1.9296 (9)
Na1—O2ⁱ	2.4542 (15)	Ga2—O3^vii	1.9296 (9)
Ga1—O1	1.8665 (15)	Ga2—O5	1.9265 (15)
Ga1—O2	1.8345 (15)	Ga—O2^vi	2.0253 (11)
Ga1—O5ⁱⁱ	1.8208 (8)	Ga—O2^vii	2.0253 (11)
Ga1—O5ⁱⁱⁱ	1.8208 (8)	Ga—O3	1.8694 (15)
Ga2—O1	2.0353 (14)	Ga—O4	2.0385 (15)
Ga2—O1^iv	2.0575 (10)	Ga—O4^vi	1.9812 (10)
Ga2—O1^v	2.0575 (10)	Ga—O4^vii	1.9812 (10)

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

(299K-model-II) top

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	F(000) = 528
M_r = 570.5	D_x = 4.997 (1) Mg m⁻³
Monoclinic, C2/m	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -C 2y	Cell parameters from 967 reflections
a = 12.1008 (8) Å	θ = 3.8–51.6°
b = 3.0113 (2) Å	µ = 18.11 mm⁻¹
c = 10.4100 (6) Å	T = 299 K
β = 92.258 (4)°	Prism, colorless
V = 379.04 (4) Å³	0.24 × 0.16 × 0.10 mm
Z = 2

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	1785 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.060
ω scans	θ_max = 51.7°, θ_min = 2.0°
Absorption correction: analytical ?	h = −24→21
T_min = 0.074, T_max = 0.249	k = −6→5
5633 measured reflections	l = −22→22
2168 independent reflections

Refinement top

Refinement on F²	Weighting scheme based on measured s.u.'s w = 1/(σ²(I) + 0.0004I²)
R[F² > 2σ(F²)] = 0.028	(Δ/σ)_max = 0.009
wR(F²) = 0.069	Δρ_max = 2.88 e Å⁻³
S = 1.17	Δρ_min = −1.96 e Å⁻³
2168 reflections	Extinction correction: B-C type 2 (Becker & Coppens, 1974)
61 parameters	Extinction coefficient: 0.001711

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	V = 379.04 (4) Å³
M_r = 570.5	Z = 2
Monoclinic, C2/m	Mo Kα radiation
a = 12.1008 (8) Å	µ = 18.11 mm⁻¹
b = 3.0113 (2) Å	T = 299 K
c = 10.4100 (6) Å	0.24 × 0.16 × 0.10 mm
β = 92.258 (4)°

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	2168 independent reflections
Absorption correction: analytical ?	1785 reflections with I > 2σ(I)
T_min = 0.074, T_max = 0.249	R_int = 0.060
5633 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.028	61 parameters
wR(F²) = 0.069	Δρ_max = 2.88 e Å⁻³
S = 1.17	Δρ_min = −1.96 e Å⁻³
2168 reflections

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Na1	0	0	0.5	0.060 (9)	0.59 (6)
Na2	0	0.30 (3)	0.5	0.059 (13)	0.11 (3)
Ga1	0.063729 (18)	0	0.16343 (2)	0.00548 (4)
Ga2	0.323681 (18)	0	0.10155 (2)	0.00567 (5)
Ga	0.26463 (3)	0	0.62588 (3)	0.00758 (6)	0.403 (3)
Ti	0.26463 (3)	0	0.62588 (3)	0.00758 (6)	0.597 (3)
O1	0.16414 (12)	0	0.03184 (13)	0.0060 (3)
O2	0.13003 (13)	0	0.32496 (14)	0.0078 (3)
O3	0.20430 (13)	0	0.78848 (13)	0.0071 (3)
O4	0.32467 (13)	0	0.44560 (14)	0.0083 (3)
O5	0.48026 (12)	0	0.14290 (16)	0.0081 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.022 (2)	0.13 (3)	0.033 (3)	0	0.016 (2)	0
Na2	0.012 (6)	0.09 (3)	0.075 (18)	0	−0.019 (10)	0
Ga1	0.00490 (8)	0.00560 (8)	0.00591 (7)	0	−0.00006 (6)	0
Ga2	0.00476 (8)	0.00526 (8)	0.00693 (7)	0	−0.00074 (6)	0
Ga	0.01019 (12)	0.00705 (11)	0.00550 (8)	0	0.00044 (7)	0
Ti	0.01019 (12)	0.00705 (11)	0.00550 (8)	0	0.00044 (7)	0
O1	0.0049 (5)	0.0070 (5)	0.0062 (4)	0	0.0001 (3)	0
O2	0.0083 (5)	0.0087 (5)	0.0064 (4)	0	−0.0015 (4)	0
O3	0.0104 (6)	0.0057 (5)	0.0054 (4)	0	0.0017 (4)	0
O4	0.0084 (5)	0.0095 (6)	0.0070 (4)	0	−0.0002 (4)	0
O5	0.0048 (5)	0.0054 (5)	0.0138 (5)	0	−0.0016 (4)	0

Bond lengths (Å) top

Na1—O2	2.4540 (15)	Ga2—O1^vi	2.0574 (10)
Na1—O2ⁱ	2.4540 (15)	Ga2—O3^vii	1.9295 (9)
Na2—O4ⁱⁱ	2.26 (2)	Ga2—O3ⁱⁱⁱ	1.9295 (9)
Na2—O4ⁱⁱⁱ	2.26 (2)	Ga2—O5	1.9264 (15)
Ga1—O1	1.8665 (14)	Ga—O2^vii	2.0254 (11)
Ga1—O2	1.8344 (15)	Ga—O2ⁱⁱⁱ	2.0254 (11)
Ga1—O5^iv	1.8209 (8)	Ga—O3	1.8695 (15)
Ga1—O5ⁱⁱ	1.8209 (8)	Ga—O4	2.0390 (15)
Ga2—O1	2.0355 (14)	Ga—O4^vii	1.9812 (10)
Ga2—O1^v	2.0574 (10)	Ga—O4ⁱⁱⁱ	1.9812 (10)

(173K-model-I) top

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	F(000) = 528
M_r = 570.5	D_x = 5.010 (1) Mg m⁻³
Monoclinic, C2/m	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -C 2y	Cell parameters from 854 reflections
a = 12.0848 (12) Å	θ = 3.8–51.4°
b = 3.0101 (3) Å	µ = 18.16 mm⁻¹
c = 10.4014 (9) Å	T = 173 K
β = 92.187 (5)°	Prism, colorless
V = 378.09 (6) Å³	0.24 × 0.16 × 0.10 mm
Z = 2

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	1749 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.060
ω scans	θ_max = 51.6°, θ_min = 2.0°
Absorption correction: analytical ?	h = −24→21
T_min = 0.071, T_max = 0.250	k = −6→5
5581 measured reflections	l = −22→22
2159 independent reflections

Refinement top

Refinement on F²	Weighting scheme based on measured s.u.'s w = 1/(σ²(I) + 0.0004I²)
R[F² > 2σ(F²)] = 0.030	(Δ/σ)_max = 0.009
wR(F²) = 0.068	Δρ_max = 3.09 e Å⁻³
S = 1.07	Δρ_min = −2.17 e Å⁻³
2159 reflections	Extinction correction: B-C type 2 (Becker & Coppens, 1974)
60 parameters	Extinction coefficient: 0.002006

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	V = 378.09 (6) Å³
M_r = 570.5	Z = 2
Monoclinic, C2/m	Mo Kα radiation
a = 12.0848 (12) Å	µ = 18.16 mm⁻¹
b = 3.0101 (3) Å	T = 173 K
c = 10.4014 (9) Å	0.24 × 0.16 × 0.10 mm
β = 92.187 (5)°

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	2159 independent reflections
Absorption correction: analytical ?	1749 reflections with I > 2σ(I)
T_min = 0.071, T_max = 0.250	R_int = 0.060
5581 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.030	60 parameters
wR(F²) = 0.068	Δρ_max = 3.09 e Å⁻³
S = 1.07	Δρ_min = −2.17 e Å⁻³
2159 reflections

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Na1	0	0	0.5	0.1085	0.808 (6)
Ga1	0.063737 (19)	0	0.16364 (2)	0.00414 (5)
Ga2	0.323601 (18)	0	0.10136 (2)	0.00433 (5)
Ga	0.26469 (3)	0	0.62574 (3)	0.00593 (6)	0.404 (3)
Ti	0.26469 (3)	0	0.62574 (3)	0.00593 (6)	0.596 (3)
O1	0.16412 (12)	0	0.03181 (14)	0.0049 (3)
O2	0.12991 (13)	0	0.32544 (15)	0.0062 (3)
O3	0.20429 (13)	0	0.78856 (15)	0.0058 (3)
O4	0.32471 (13)	0	0.44578 (15)	0.0068 (3)
O5	0.48034 (13)	0	0.14277 (17)	0.0063 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.017158	0.281274	0.027615	0	0.008105	0
Ga1	0.00349 (9)	0.00443 (9)	0.00450 (7)	0	0.00002 (6)	0
Ga2	0.00339 (9)	0.00415 (9)	0.00537 (7)	0	−0.00066 (6)	0
Ga	0.00794 (12)	0.00555 (12)	0.00432 (9)	0	0.00033 (8)	0
Ti	0.00794 (12)	0.00555 (12)	0.00432 (9)	0	0.00033 (8)	0
O1	0.0040 (5)	0.0055 (5)	0.0051 (4)	0	0.0002 (4)	0
O2	0.0062 (5)	0.0074 (6)	0.0050 (4)	0	−0.0010 (4)	0
O3	0.0078 (6)	0.0052 (5)	0.0046 (4)	0	0.0007 (4)	0
O4	0.0071 (6)	0.0079 (6)	0.0054 (5)	0	0.0000 (4)	0
O5	0.0039 (5)	0.0044 (5)	0.0105 (5)	0	−0.0013 (4)	0

Bond lengths (Å) top

Na1—O2	2.4452 (16)	Ga2—O3^vi	1.9285 (10)
Na1—O2ⁱ	2.4452 (16)	Ga2—O3^vii	1.9285 (10)
Ga1—O1	1.8651 (15)	Ga2—O5	1.9264 (15)
Ga1—O2	1.8355 (15)	Ga—O2^vi	2.0239 (11)
Ga1—O5ⁱⁱ	1.8197 (9)	Ga—O2^vii	2.0239 (11)
Ga1—O5ⁱⁱⁱ	1.8197 (9)	Ga—O3	1.8695 (16)
Ga2—O1	2.0326 (15)	Ga—O4	2.0331 (16)
Ga2—O1^iv	2.0547 (10)	Ga—O4^vi	1.9811 (10)
Ga2—O1^v	2.0547 (10)	Ga—O4^vii	1.9811 (10)

(173K-model-II) top

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	F(000) = 528
M_r = 570.5	D_x = 5.010 (1) Mg m⁻³
Monoclinic, C2/m	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -C 2y	Cell parameters from 854 reflections
a = 12.0848 (12) Å	θ = 3.8–51.4°
b = 3.0101 (3) Å	µ = 18.16 mm⁻¹
c = 10.4014 (9) Å	T = 173 K
β = 92.187 (5)°	Prism, colorless
V = 378.09 (6) Å³	0.24 × 0.16 × 0.10 mm
Z = 2

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	1749 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.060
ω scans	θ_max = 51.6°, θ_min = 2.0°
Absorption correction: analytical ?	h = −24→21
T_min = 0.071, T_max = 0.250	k = −6→5
5581 measured reflections	l = −22→22
2159 independent reflections

Refinement top

Refinement on F²	Weighting scheme based on measured s.u.'s w = 1/(σ²(I) + 0.0004I²)
R[F² > 2σ(F²)] = 0.029	(Δ/σ)_max = 0.009
wR(F²) = 0.067	Δρ_max = 3.17 e Å⁻³
S = 1.06	Δρ_min = −2.28 e Å⁻³
2159 reflections	Extinction correction: B-C type 2 (Becker & Coppens, 1974)
61 parameters	Extinction coefficient: 0.002061

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	V = 378.09 (6) Å³
M_r = 570.5	Z = 2
Monoclinic, C2/m	Mo Kα radiation
a = 12.0848 (12) Å	µ = 18.16 mm⁻¹
b = 3.0101 (3) Å	T = 173 K
c = 10.4014 (9) Å	0.24 × 0.16 × 0.10 mm
β = 92.187 (5)°

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	2159 independent reflections
Absorption correction: analytical ?	1749 reflections with I > 2σ(I)
T_min = 0.071, T_max = 0.250	R_int = 0.060
5581 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.029	61 parameters
wR(F²) = 0.067	Δρ_max = 3.17 e Å⁻³
S = 1.06	Δρ_min = −2.28 e Å⁻³
2159 reflections

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Na1	0	0	0.5	0.030 (7)	0.26 (10)
Na2	0	0.17 (3)	0.5	0.064 (12)	0.28 (5)
Ga1	0.063739 (18)	0	0.16364 (2)	0.00414 (5)
Ga2	0.323600 (18)	0	0.10137 (2)	0.00433 (5)
Ga	0.26469 (3)	0	0.62574 (3)	0.00596 (6)	0.406 (3)
Ti	0.26469 (3)	0	0.62574 (3)	0.00596 (6)	0.594 (3)
O1	0.16412 (12)	0	0.03180 (14)	0.0049 (3)
O2	0.12990 (13)	0	0.32545 (14)	0.0063 (3)
O3	0.20427 (13)	0	0.78856 (15)	0.0058 (3)
O4	0.32473 (13)	0	0.44577 (15)	0.0068 (3)
O5	0.48034 (13)	0	0.14273 (16)	0.0063 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.027 (8)	0.035 (16)	0.032 (7)	0	0.028 (10)	0
Na2	0.013 (3)	0.15 (4)	0.027 (4)	0	−0.003 (3)	0
Ga1	0.00350 (8)	0.00442 (9)	0.00450 (7)	0	0.00002 (6)	0
Ga2	0.00339 (9)	0.00416 (8)	0.00538 (7)	0	−0.00066 (6)	0
Ga	0.00798 (12)	0.00558 (12)	0.00433 (9)	0	0.00034 (8)	0
Ti	0.00798 (12)	0.00558 (12)	0.00433 (9)	0	0.00034 (8)	0
O1	0.0040 (5)	0.0054 (5)	0.0052 (4)	0	0.0002 (4)	0
O2	0.0062 (5)	0.0076 (6)	0.0049 (4)	0	−0.0010 (4)	0
O3	0.0077 (6)	0.0052 (5)	0.0046 (4)	0	0.0007 (4)	0
O4	0.0072 (6)	0.0079 (6)	0.0054 (4)	0	0.0000 (4)	0
O5	0.0039 (5)	0.0044 (5)	0.0105 (5)	0	−0.0013 (4)	0

Bond lengths (Å) top

Na1—O2	2.4450 (16)	Ga2—O1^v	2.0546 (10)
Na1—O2ⁱ	2.4450 (16)	Ga2—O1^vi	2.0546 (10)
Na2—O2	2.499 (19)	Ga2—O3^vii	1.9285 (10)
Na2—O2ⁱ	2.499 (19)	Ga2—O3ⁱⁱⁱ	1.9285 (10)
Na2—O4ⁱⁱ	2.39 (4)	Ga2—O5	1.9263 (15)
Na2—O4ⁱⁱⁱ	2.39 (4)	Ga—O2^vii	2.0240 (11)
Ga1—O1	1.8652 (15)	Ga—O2ⁱⁱⁱ	2.0240 (11)
Ga1—O2	1.8355 (15)	Ga—O3	1.8697 (16)
Ga1—O5^iv	1.8198 (9)	Ga—O4	2.0332 (16)
Ga1—O5ⁱⁱ	1.8198 (9)	Ga—O4^vii	1.9811 (10)
Ga2—O1	2.0326 (15)	Ga—O4ⁱⁱⁱ	1.9811 (10)

(123K-model-I) top

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	Z = 2
M_r = 570.5	F(000) = 528
Monoclinic, C2/m	D_x = 5.009 (1) Mg m⁻³
Hall symbol: -C 2y	Mo Kα radiation, λ = 0.71069 Å
a = 12.0828 (9) Å	Cell parameters from 871 reflections
b = 3.0099 (3) Å	µ = 18.16 mm⁻¹
c = 10.4045 (7) Å	T = 123 K
β = 92.192 (4)°	Prism, colorless
V = 378.11 (5) Å³	0.24 × 0.16 × 0.10 mm

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	1752 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.059
ω scans	θ_max = 51.7°, θ_min = 2.0°
Absorption correction: analytical ?	h = −24→21
T_min = 0.073, T_max = 0.250	k = −6→5
5596 measured reflections	l = −22→22
2160 independent reflections

Refinement top

Refinement on F²	Weighting scheme based on measured s.u.'s w = 1/(σ²(I) + 0.0004I²)
R[F² > 2σ(F²)] = 0.029	(Δ/σ)_max = 0.008
wR(F²) = 0.066	Δρ_max = 2.96 e Å⁻³
S = 1.05	Δρ_min = −1.93 e Å⁻³
2160 reflections	Extinction correction: B-C type 2 (Becker & Coppens, 1974)
60 parameters	Extinction coefficient: 0.001903

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	V = 378.11 (5) Å³
M_r = 570.5	Z = 2
Monoclinic, C2/m	Mo Kα radiation
a = 12.0828 (9) Å	µ = 18.16 mm⁻¹
b = 3.0099 (3) Å	T = 123 K
c = 10.4045 (7) Å	0.24 × 0.16 × 0.10 mm
β = 92.192 (4)°

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	2160 independent reflections
Absorption correction: analytical ?	1752 reflections with I > 2σ(I)
T_min = 0.073, T_max = 0.250	R_int = 0.059
5596 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.029	60 parameters
wR(F²) = 0.066	Δρ_max = 2.96 e Å⁻³
S = 1.05	Δρ_min = −1.93 e Å⁻³
2160 reflections

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Na1	0	0	0.5	0.103	0.802 (6)
Ga1	0.063744 (18)	0	0.16375 (2)	0.00363 (5)
Ga2	0.323584 (18)	0	0.10128 (2)	0.00381 (5)
Ga	0.26467 (3)	0	0.62570 (3)	0.00533 (6)	0.401 (3)
Ti	0.26467 (3)	0	0.62570 (3)	0.00533 (6)	0.599 (3)
O1	0.16418 (12)	0	0.03200 (14)	0.0044 (3)
O2	0.13001 (13)	0	0.32565 (14)	0.0059 (3)
O3	0.20431 (13)	0	0.78880 (14)	0.0054 (3)
O4	0.32454 (13)	0	0.44571 (15)	0.0065 (3)
O5	0.48026 (12)	0	0.14288 (16)	0.0055 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.013526	0.274117	0.021869	0	0.008462	0
Ga1	0.00310 (8)	0.00388 (9)	0.00391 (7)	0	0.00001 (6)	0
Ga2	0.00289 (9)	0.00369 (8)	0.00478 (7)	0	−0.00065 (6)	0
Ga	0.00705 (11)	0.00500 (11)	0.00394 (8)	0	0.00025 (7)	0
Ti	0.00705 (11)	0.00500 (11)	0.00394 (8)	0	0.00025 (7)	0
O1	0.0036 (5)	0.0049 (5)	0.0047 (4)	0	0.0001 (4)	0
O2	0.0063 (5)	0.0067 (6)	0.0045 (4)	0	−0.0003 (4)	0
O3	0.0078 (6)	0.0046 (5)	0.0041 (4)	0	0.0008 (4)	0
O4	0.0067 (6)	0.0073 (6)	0.0055 (4)	0	0.0001 (4)	0
O5	0.0036 (5)	0.0037 (5)	0.0092 (5)	0	−0.0010 (4)	0

Bond lengths (Å) top

Na1—O2	2.4446 (15)	Ga2—O3^vi	1.9277 (9)
Na1—O2ⁱ	2.4446 (15)	Ga2—O3^vii	1.9277 (9)
Ga1—O1	1.8652 (15)	Ga2—O5	1.9258 (15)
Ga1—O2	1.8373 (15)	Ga—O2^vi	2.0227 (10)
Ga1—O5ⁱⁱ	1.8201 (8)	Ga—O2^vii	2.0227 (10)
Ga1—O5ⁱⁱⁱ	1.8201 (8)	Ga—O3	1.8725 (15)
Ga2—O1	2.0305 (14)	Ga—O4	2.0332 (16)
Ga2—O1^iv	2.0556 (10)	Ga—O4^vi	1.9792 (10)
Ga2—O1^v	2.0556 (10)	Ga—O4^vii	1.9792 (10)

(123K-model-II) top

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	Z = 2
M_r = 570.5	F(000) = 528
Monoclinic, C2/m	D_x = 5.009 (1) Mg m⁻³
Hall symbol: -C 2y	Mo Kα radiation, λ = 0.71069 Å
a = 12.0828 (9) Å	Cell parameters from 871 reflections
b = 3.0099 (3) Å	µ = 18.16 mm⁻¹
c = 10.4045 (7) Å	T = 123 K
β = 92.192 (4)°	Prism, colorless
V = 378.11 (5) Å³	0.24 × 0.16 × 0.10 mm

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	1752 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.059
ω scans	θ_max = 51.7°, θ_min = 2.0°
Absorption correction: analytical ?	h = −24→21
T_min = 0.073, T_max = 0.250	k = −6→5
5596 measured reflections	l = −22→22
2160 independent reflections

Refinement top

Refinement on F²	Weighting scheme based on measured s.u.'s w = 1/(σ²(I) + 0.0004I²)
R[F² > 2σ(F²)] = 0.028	(Δ/σ)_max = 0.009
wR(F²) = 0.065	Δρ_max = 2.91 e Å⁻³
S = 1.04	Δρ_min = −1.99 e Å⁻³
2160 reflections	Extinction correction: B-C type 2 (Becker & Coppens, 1974)
61 parameters	Extinction coefficient: 0.001962

Crystal data top

Ga_4.8Na_0.8O₁₀Ti_1.2	V = 378.11 (5) Å³
M_r = 570.5	Z = 2
Monoclinic, C2/m	Mo Kα radiation
a = 12.0828 (9) Å	µ = 18.16 mm⁻¹
b = 3.0099 (3) Å	T = 123 K
c = 10.4045 (7) Å	0.24 × 0.16 × 0.10 mm
β = 92.192 (4)°

Data collection top

Bruker SMART APEX CCD areadetector diffractometer	2160 independent reflections
Absorption correction: analytical ?	1752 reflections with I > 2σ(I)
T_min = 0.073, T_max = 0.250	R_int = 0.059
5596 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.028	61 parameters
wR(F²) = 0.065	Δρ_max = 2.91 e Å⁻³
S = 1.04	Δρ_min = −1.99 e Å⁻³
2160 reflections

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Na1	0	0	0.5	0.027 (6)	0.34 (11)
Na2	0	0.20 (3)	0.5	0.044 (11)	0.23 (5)
Ga1	0.063745 (18)	0	0.16375 (2)	0.00363 (5)
Ga2	0.323584 (18)	0	0.10129 (2)	0.00381 (5)
Ga	0.26467 (3)	0	0.62569 (3)	0.00535 (6)	0.402 (3)
Ti	0.26467 (3)	0	0.62569 (3)	0.00535 (6)	0.598 (3)
O1	0.16419 (12)	0	0.03201 (14)	0.0044 (3)
O2	0.12999 (13)	0	0.32565 (14)	0.0059 (3)
O3	0.20431 (13)	0	0.78878 (14)	0.0054 (3)
O4	0.32455 (13)	0	0.44570 (14)	0.0065 (3)
O5	0.48025 (12)	0	0.14286 (15)	0.0056 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.019 (5)	0.034 (15)	0.028 (5)	0	0.019 (6)	0
Na2	0.009 (3)	0.11 (3)	0.018 (3)	0	0.000 (3)	0
Ga1	0.00310 (8)	0.00387 (9)	0.00392 (7)	0	0.00001 (6)	0
Ga2	0.00289 (8)	0.00370 (8)	0.00479 (7)	0	−0.00065 (6)	0
Ga	0.00708 (12)	0.00501 (11)	0.00396 (8)	0	0.00026 (7)	0
Ti	0.00708 (12)	0.00501 (11)	0.00396 (8)	0	0.00026 (7)	0
O1	0.0036 (5)	0.0049 (5)	0.0048 (4)	0	0.0001 (4)	0
O2	0.0063 (5)	0.0069 (6)	0.0044 (4)	0	−0.0003 (4)	0
O3	0.0077 (6)	0.0045 (5)	0.0041 (4)	0	0.0008 (4)	0
O4	0.0068 (6)	0.0072 (6)	0.0055 (4)	0	0.0001 (4)	0
O5	0.0035 (5)	0.0038 (5)	0.0092 (5)	0	−0.0011 (4)	0

Bond lengths (Å) top

Na1—O2	2.4445 (15)	Ga2—O1^vi	2.0557 (10)
Na1—O2ⁱ	2.4445 (15)	Ga2—O3^vii	1.9277 (9)
Na2—O4ⁱⁱ	2.36 (4)	Ga2—O3ⁱⁱⁱ	1.9277 (9)
Na2—O4ⁱⁱⁱ	2.36 (4)	Ga2—O5	1.9256 (15)
Ga1—O1	1.8652 (15)	Ga—O2^vii	2.0228 (10)
Ga1—O2	1.8372 (14)	Ga—O2ⁱⁱⁱ	2.0228 (10)
Ga1—O5^iv	1.8202 (8)	Ga—O3	1.8724 (15)
Ga1—O5ⁱⁱ	1.8202 (8)	Ga—O4	2.0332 (15)
Ga2—O1	2.0304 (14)	Ga—O4^vii	1.9793 (10)
Ga2—O1^v	2.0557 (10)	Ga—O4ⁱⁱⁱ	1.9793 (10)

Experimental details

	(299K-model-III)	(173K-model-III)	(123K-model-III)	(299K-model-I)
Crystal data
Chemical formula	Ga_4.8Na_0.8O₁₀Ti_1.2	Ga_4.8Na_0.8O₁₀Ti_1.2	Ga_4.8Na_0.8O₁₀Ti_1.2	Ga_4.8Na_0.8O₁₀Ti_1.2
M_r	570.5	570.5	570.5	570.5
Crystal system, space group	Monoclinic, C2/m	Monoclinic, C2/m	Monoclinic, C2/m	Monoclinic, C2/m
Temperature (K)	299	173	123	299
a, b, c (Å)	12.1008 (8), 3.0113 (2), 10.4100 (6)	12.0848 (12), 3.0101 (3), 10.4014 (9)	12.0828 (9), 3.0099 (3), 10.4045 (7)	12.1008 (8), 3.0113 (2), 10.4100 (6)
β (°)	92.258 (4)	92.187 (5)	92.192 (4)	92.258 (4)
V (Å³)	379.04 (4)	378.09 (6)	378.11 (5)	379.04 (4)
Z	2	2	2	2
Radiation type	Mo Kα	Mo Kα	Mo Kα	Mo Kα
µ (mm⁻¹)	18.11	18.16	18.16	18.11
Crystal size (mm)	0.24 × 0.16 × 0.10	0.24 × 0.16 × 0.10	0.24 × 0.16 × 0.10	0.24 × 0.16 × 0.10

Data collection
Diffractometer	Bruker SMART APEX CCD areadetector diffractometer	Bruker SMART APEX CCD areadetector diffractometer	Bruker SMART APEX CCD areadetector diffractometer	Bruker SMART APEX CCD areadetector diffractometer
Absorption correction	Analytical	Analytical	Analytical	Analytical
T_min, T_max	0.074, 0.249	0.071, 0.250	0.073, 0.250	0.074, 0.249
No. of measured, independent and observed [I > 2σ(I)] reflections	5633, 2168, 1785	5581, 2159, 1749	5596, 2160, 1752	5633, 2168, 1785
R_int	0.060	0.060	0.059	0.060
(sin θ/λ)_max (Å⁻¹)	1.104	1.102	1.104	1.104

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.028, 0.069, 1.17	0.029, 0.067, 1.06	0.028, 0.065, 1.04	0.028, 0.069, 1.18
No. of reflections	2168	2159	2160	2168
No. of parameters	60	60	60	60
No. of restraints	?	?	?	?
Δρ_max, Δρ_min (e Å⁻³)	2.88, −1.95	3.10, −2.21	2.92, −1.99	2.86, −1.95

	(299K-model-II)	(173K-model-I)	(173K-model-II)	(123K-model-I)
Crystal data
Chemical formula	Ga_4.8Na_0.8O₁₀Ti_1.2	Ga_4.8Na_0.8O₁₀Ti_1.2	Ga_4.8Na_0.8O₁₀Ti_1.2	Ga_4.8Na_0.8O₁₀Ti_1.2
M_r	570.5	570.5	570.5	570.5
Crystal system, space group	Monoclinic, C2/m	Monoclinic, C2/m	Monoclinic, C2/m	Monoclinic, C2/m
Temperature (K)	299	173	173	123
a, b, c (Å)	12.1008 (8), 3.0113 (2), 10.4100 (6)	12.0848 (12), 3.0101 (3), 10.4014 (9)	12.0848 (12), 3.0101 (3), 10.4014 (9)	12.0828 (9), 3.0099 (3), 10.4045 (7)
β (°)	92.258 (4)	92.187 (5)	92.187 (5)	92.192 (4)
V (Å³)	379.04 (4)	378.09 (6)	378.09 (6)	378.11 (5)
Z	2	2	2	2
Radiation type	Mo Kα	Mo Kα	Mo Kα	Mo Kα
µ (mm⁻¹)	18.11	18.16	18.16	18.16
Crystal size (mm)	0.24 × 0.16 × 0.10	0.24 × 0.16 × 0.10	0.24 × 0.16 × 0.10	0.24 × 0.16 × 0.10

Data collection
Diffractometer	Bruker SMART APEX CCD areadetector diffractometer	Bruker SMART APEX CCD areadetector diffractometer	Bruker SMART APEX CCD areadetector diffractometer	Bruker SMART APEX CCD areadetector diffractometer
Absorption correction	Analytical	Analytical	Analytical	Analytical
T_min, T_max	0.074, 0.249	0.071, 0.250	0.071, 0.250	0.073, 0.250
No. of measured, independent and observed [I > 2σ(I)] reflections	5633, 2168, 1785	5581, 2159, 1749	5581, 2159, 1749	5596, 2160, 1752
R_int	0.060	0.060	0.060	0.059
(sin θ/λ)_max (Å⁻¹)	1.104	1.102	1.102	1.104

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.028, 0.069, 1.17	0.030, 0.068, 1.07	0.029, 0.067, 1.06	0.029, 0.066, 1.05
No. of reflections	2168	2159	2159	2160
No. of parameters	61	60	61	60
No. of restraints	?	?	?	?
Δρ_max, Δρ_min (e Å⁻³)	2.88, −1.96	3.09, −2.17	3.17, −2.28	2.96, −1.93

	(123K-model-II)
Crystal data
Chemical formula	Ga_4.8Na_0.8O₁₀Ti_1.2
M_r	570.5
Crystal system, space group	Monoclinic, C2/m
Temperature (K)	123
a, b, c (Å)	12.0828 (9), 3.0099 (3), 10.4045 (7)
β (°)	92.192 (4)
V (Å³)	378.11 (5)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	18.16
Crystal size (mm)	0.24 × 0.16 × 0.10

Data collection
Diffractometer	Bruker SMART APEX CCD areadetector diffractometer
Absorption correction	Analytical
T_min, T_max	0.073, 0.250
No. of measured, independent and observed [I > 2σ(I)] reflections	5596, 2160, 1752
R_int	0.059
(sin θ/λ)_max (Å⁻¹)	1.104

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.028, 0.065, 1.04
No. of reflections	2160
No. of parameters	61
No. of restraints	?
Δρ_max, Δρ_min (e Å⁻³)	2.91, −1.99

Computer programs: (Jana2000; Petricek and Dusek, 2000).

Selected bond lengths (Å) for (299K-model-II) top

Ga—O4	2.0390 (15)	Ga—O4ⁱⁱ	1.9812 (10)
Ga—O4ⁱ	1.9812 (10)

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

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